#============================================================================= data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 15 _journal_issue 1 _journal_year 2024 _journal_page_first 1 _journal_page_last 16 #============================================================================= data_exp_291 _audit_creation_date 2023-08-11 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _shelx_SHELXL_version_number '2018/3' loop_ _audit_author_name _audit_author_email ; lata_panicker@yahoo.com ; _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name 'Panicker, L.' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic '4-Carboxyanilinium dihydrogen phosphate monohydrate' _chemical_formula_moiety 'H2 O4 P, H2 O, C7 H8 N O2' _chemical_formula_sum 'C7 H12 N O7 P' _chemical_formula_weight 253.15 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5238(2) _cell_length_b 8.9068(2) _cell_length_c 14.4976(4) _cell_angle_alpha 106.456(2) _cell_angle_beta 90.195(2) _cell_angle_gamma 92.811(2) _cell_volume 1054.13(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 14552 _cell_measurement_temperature 293 _cell_measurement_theta_max 73.0620 _cell_measurement_theta_min 5.1810 _shelx_estimated_absorpt_T_max 0.626 _shelx_estimated_absorpt_T_min 0.306 _exptl_absorpt_coefficient_mu 2.587 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.18975 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear light brown' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary brown _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 528 _exptl_crystal_preparation ? _exptl_crystal_recrystallization_method ? _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1018 _diffrn_reflns_av_unetI/netI 0.0521 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.982 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 18182 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.982 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.198 _diffrn_reflns_theta_min 3.179 _diffrn_ambient_temperature 293 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 4.1600 _diffrn_detector_type Titan _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -31.00 75.00 1.00 1.00 -- 43.29 -77.00 90.00 106 2 \w -26.00 69.00 1.00 1.00 -- 43.29 -57.00-150.00 95 3 \w 18.00 113.00 1.00 1.00 -- 43.29 57.00 0.00 95 4 \w 29.00 134.00 1.00 1.00 -- 102.90 -77.00-150.00 105 5 \w 29.00 122.00 1.00 1.00 -- 102.90-126.00 30.00 93 6 \w 72.00 158.00 1.00 1.00 -- 102.90 126.00 0.00 86 7 \w 29.00 134.00 1.00 1.00 -- 102.90 -77.00 30.00 105 8 \w 20.00 110.00 1.00 1.00 -- 102.90 -95.00-150.00 90 9 \w 20.00 110.00 1.00 1.00 -- 102.90 -95.00 150.00 90 10 \w 78.00 158.00 1.00 1.00 -- 102.90 45.00 -60.00 80 11 \w 30.00 129.00 1.00 1.00 -- 102.90 -30.00-150.00 99 12 \w 30.00 129.00 1.00 1.00 -- 102.90 -30.00 -30.00 99 13 \w 78.00 158.00 1.00 1.00 -- 102.90 45.00-180.00 80 14 \w 12.00 118.00 1.00 1.00 -- 43.29 77.00-120.00 106 15 \w 18.00 113.00 1.00 1.00 -- 43.29 57.00 150.00 95 16 \w 18.00 113.00 1.00 1.00 -- 43.29 57.00 90.00 95 17 \w 78.00 158.00 1.00 1.00 -- 102.90 45.00-120.00 80 18 \w 71.00 158.00 1.00 1.00 -- 102.90 77.00-120.00 87 19 \w 76.00 158.00 1.00 1.00 -- 102.90 61.00 60.00 82 20 \w 78.00 158.00 1.00 1.00 -- 102.90 45.00 120.00 80 21 \w 76.00 158.00 1.00 1.00 -- 102.90 61.00 30.00 82 22 \w 71.00 158.00 1.00 1.00 -- 102.90 77.00 120.00 87 23 \w 71.00 158.00 1.00 1.00 -- 102.90 77.00-180.00 87 24 \w 71.00 158.00 1.00 1.00 -- 102.90 77.00 -60.00 87 25 \w 78.00 158.00 1.00 1.00 -- 102.90 45.00 0.00 80 26 \w 72.00 117.00 1.00 1.00 -- 43.29 126.00 120.00 45 27 \w 12.00 118.00 1.00 1.00 -- 43.29 77.00 -30.00 106 28 \w 12.00 118.00 1.00 1.00 -- 43.29 77.00 150.00 106 29 \w 76.00 158.00 1.00 1.00 -- 102.90 61.00 0.00 82 30 \w 71.00 158.00 1.00 1.00 -- 102.90 77.00 60.00 87 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset, Titan' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.1445911000 _diffrn_orient_matrix_UB_12 0.1133520000 _diffrn_orient_matrix_UB_13 0.0059996000 _diffrn_orient_matrix_UB_21 -0.1053539000 _diffrn_orient_matrix_UB_22 0.1206400000 _diffrn_orient_matrix_UB_23 -0.0232997000 _diffrn_orient_matrix_UB_31 -0.0273643000 _diffrn_orient_matrix_UB_32 0.0722020000 _diffrn_orient_matrix_UB_33 0.1081768000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3839 _reflns_number_total 4149 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _refine_diff_density_max 0.664 _refine_diff_density_min -0.430 _refine_diff_density_rms 0.106 _refine_ls_extinction_coef 0.046(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 304 _refine_ls_number_reflns 4149 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0584 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1308P)^2^+0.1535P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1647 _refine_ls_wR_factor_ref 0.1712 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H,H,H) groups At 1.5 times of: All O(H) groups, All O(H,H) groups 2.a Free rotating group: O7(H7B,H7C), O7A(H7AA,H7AB) 2.b Aromatic/amide H refined with riding coordinates: C7(H7), C4(H4), C6(H6), C3A(H3A), C6A(H6A), C3(H3), C4A(H4A), C7A(H7A) 2.c Idealised Me refined as rotating group: N1(H1A,H1B,H1C), N1A(H1AA,H1AB,H1AC) 2.d Idealised tetrahedral OH refined as rotating group: O5A(H5A), O5(H5), O4(H4B), O2(H2), O4A(H4AA), O2A(H2A) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P1A P 1.17380(5) 0.26679(5) 0.86592(3) 0.0252(2) Uani 1 1 d . . . . . P1 P 0.32735(5) 0.77865(5) 0.86329(3) 0.0242(2) Uani 1 1 d . . . . . O6A O 1.10517(17) 0.15033(16) 0.91450(10) 0.0300(3) Uani 1 1 d . . . . . O7 O 0.90250(17) 0.76036(17) 0.89035(10) 0.0312(3) Uani 1 1 d G . . . . H7B H 0.913901 0.786419 0.951148 0.047 Uiso 1 1 d G U . . . H7C H 0.995589 0.751095 0.869098 0.047 Uiso 1 1 d G U . . . O6 O 0.38666(16) 0.66147(15) 0.91079(10) 0.0292(3) Uani 1 1 d . . . . . O5A O 1.2258(2) 0.41731(17) 0.94892(10) 0.0372(4) Uani 1 1 d . . . . . H5A H 1.275785 0.479202 0.926339 0.056 Uiso 1 1 calc R U . . . O5 O 0.2828(2) 0.92423(17) 0.94714(10) 0.0373(4) Uani 1 1 d . . . . . H5 H 0.232189 0.982659 0.925257 0.056 Uiso 1 1 calc R U . . . O7A O 0.59369(16) 0.25469(17) 0.89372(10) 0.0304(3) Uani 1 1 d G . . . . H7AA H 0.589959 0.270872 0.954309 0.046 Uiso 1 1 d G U . . . H7AB H 0.497995 0.240788 0.874891 0.046 Uiso 1 1 d G U . . . O3A O 1.30933(17) 0.21023(19) 0.80104(10) 0.0347(4) Uani 1 1 d . . . . . O3 O 0.18922(16) 0.72012(18) 0.79532(10) 0.0330(4) Uani 1 1 d . . . . . O4 O 0.46816(18) 0.83485(19) 0.80946(11) 0.0376(4) Uani 1 1 d . . . . . H4B H 0.452043 0.802526 0.751217 0.056 Uiso 1 1 calc R U . . . O2 O 0.80101(18) 0.3841(2) 0.38798(11) 0.0401(4) Uani 1 1 d . . . . . H2 H 0.796005 0.348153 0.329283 0.060 Uiso 1 1 calc R U . . . O4A O 1.03886(19) 0.3144(2) 0.80754(11) 0.0383(4) Uani 1 1 d . . . . . H4AA H 1.060430 0.290193 0.750299 0.057 Uiso 1 1 calc R U . . . O1 O 0.5651(2) 0.2587(2) 0.37928(11) 0.0431(4) Uani 1 1 d . . . . . O2A O 0.71061(19) -0.0791(2) 0.38147(11) 0.0391(4) Uani 1 1 d . . . . . H2A H 0.710883 -0.118451 0.323038 0.059 Uiso 1 1 calc R U . . . N1 N 0.6661(2) 0.52441(19) 0.83599(12) 0.0273(4) Uani 1 1 d . . . . . H1A H 0.663625 0.439079 0.856439 0.033 Uiso 1 1 calc R U . . . H1B H 0.581215 0.577934 0.856040 0.033 Uiso 1 1 calc R U . . . H1C H 0.751901 0.584260 0.859482 0.033 Uiso 1 1 calc R U . . . O1A O 0.9054(2) -0.2388(2) 0.37850(11) 0.0473(5) Uani 1 1 d . . . . . N1A N 0.80966(19) 0.02443(19) 0.83247(11) 0.0272(4) Uani 1 1 d . . . . . H1AA H 0.801895 -0.063463 0.850191 0.033 Uiso 1 1 calc R U . . . H1AB H 0.727913 0.081833 0.854337 0.033 Uiso 1 1 calc R U . . . H1AC H 0.898159 0.078586 0.856785 0.033 Uiso 1 1 calc R U . . . C5 C 0.6687(2) 0.4786(2) 0.73134(14) 0.0242(4) Uani 1 1 d . . . . . C1 C 0.6755(2) 0.3375(2) 0.42557(15) 0.0285(4) Uani 1 1 d . . . . . C2 C 0.6748(2) 0.3891(2) 0.53266(14) 0.0266(4) Uani 1 1 d . . . . . C2A C 0.8134(2) -0.0929(2) 0.52950(14) 0.0268(4) Uani 1 1 d . . . . . C5A C 0.8113(2) -0.0145(2) 0.72756(14) 0.0251(4) Uani 1 1 d . . . . . C7 C 0.5364(2) 0.3706(2) 0.58003(15) 0.0313(4) Uani 1 1 d . . . . . H7 H 0.446083 0.327002 0.544379 0.038 Uiso 1 1 calc R U . . . C4 C 0.8071(2) 0.4968(3) 0.68578(15) 0.0319(5) Uani 1 1 d . . . . . H4 H 0.897925 0.537859 0.721659 0.038 Uiso 1 1 calc R U . . . C6 C 0.5317(2) 0.4161(2) 0.67932(15) 0.0314(4) Uani 1 1 d . . . . . H6 H 0.438779 0.405113 0.710751 0.038 Uiso 1 1 calc R U . . . C1A C 0.8150(2) -0.1436(2) 0.42216(14) 0.0296(4) Uani 1 1 d . . . . . C3A C 0.6991(2) 0.0003(3) 0.57972(15) 0.0331(5) Uani 1 1 d . . . . . H3A H 0.623349 0.037269 0.546571 0.040 Uiso 1 1 calc R U . . . C6A C 0.9293(3) -0.1044(3) 0.67889(16) 0.0363(5) Uani 1 1 d . . . . . H6A H 1.007235 -0.137666 0.712458 0.044 Uiso 1 1 calc R U . . . C3 C 0.8099(2) 0.4537(3) 0.58640(15) 0.0329(5) Uani 1 1 d . . . . . H3 H 0.902395 0.467959 0.555323 0.040 Uiso 1 1 calc R U . . . C4A C 0.6968(2) 0.0387(3) 0.67907(15) 0.0321(5) Uani 1 1 d . . . . . H4A H 0.618756 0.099840 0.712815 0.039 Uiso 1 1 calc R U . . . C7A C 0.9293(3) -0.1440(3) 0.57971(15) 0.0354(5) Uani 1 1 d . . . . . H7A H 1.007416 -0.205208 0.546129 0.043 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1A 0.0307(3) 0.0306(3) 0.0148(3) 0.0078(2) -0.0008(2) -0.0020(2) P1 0.0297(3) 0.0293(3) 0.0142(3) 0.0071(2) 0.0001(2) 0.00252(19) O6A 0.0387(8) 0.0318(7) 0.0209(7) 0.0104(6) 0.0004(5) -0.0032(5) O7 0.0327(7) 0.0415(8) 0.0186(7) 0.0076(6) 0.0019(5) -0.0004(6) O6 0.0372(7) 0.0311(7) 0.0208(7) 0.0091(6) 0.0006(5) 0.0053(5) O5A 0.0543(9) 0.0348(8) 0.0200(7) 0.0065(6) -0.0007(6) -0.0126(6) O5 0.0555(10) 0.0366(8) 0.0199(8) 0.0057(6) -0.0006(6) 0.0159(7) O7A 0.0310(7) 0.0427(8) 0.0177(7) 0.0088(6) -0.0013(5) 0.0028(6) O3A 0.0316(7) 0.0552(9) 0.0165(7) 0.0088(6) 0.0001(6) 0.0012(6) O3 0.0295(7) 0.0517(9) 0.0165(7) 0.0075(6) -0.0003(5) 0.0022(6) O4 0.0394(8) 0.0535(9) 0.0205(7) 0.0138(7) -0.0003(6) -0.0114(7) O2 0.0367(8) 0.0638(10) 0.0167(7) 0.0076(7) 0.0029(6) -0.0040(7) O4A 0.0426(8) 0.0536(9) 0.0211(8) 0.0129(7) 0.0002(6) 0.0113(7) O1 0.0510(9) 0.0549(10) 0.0198(8) 0.0079(7) -0.0018(6) -0.0152(7) O2A 0.0440(9) 0.0551(10) 0.0179(8) 0.0086(7) -0.0043(6) 0.0112(7) N1 0.0345(8) 0.0311(8) 0.0169(8) 0.0078(6) 0.0007(6) 0.0025(6) O1A 0.0648(11) 0.0589(10) 0.0191(8) 0.0088(7) 0.0016(7) 0.0260(8) N1A 0.0331(8) 0.0311(8) 0.0170(9) 0.0065(6) -0.0006(6) -0.0001(6) C5 0.0320(9) 0.0255(8) 0.0159(9) 0.0070(7) 0.0001(7) 0.0030(7) C1 0.0352(10) 0.0306(9) 0.0211(10) 0.0095(8) 0.0008(8) 0.0024(7) C2 0.0341(10) 0.0285(9) 0.0179(10) 0.0077(7) 0.0010(7) 0.0023(7) C2A 0.0339(9) 0.0289(9) 0.0173(10) 0.0067(7) -0.0015(7) -0.0011(7) C5A 0.0310(9) 0.0269(8) 0.0172(9) 0.0067(7) -0.0016(7) -0.0036(7) C7 0.0338(10) 0.0373(10) 0.0228(10) 0.0096(8) -0.0025(8) -0.0056(7) C4 0.0283(9) 0.0436(11) 0.0204(10) 0.0039(8) -0.0001(7) 0.0004(8) C6 0.0323(10) 0.0394(10) 0.0223(10) 0.0096(8) 0.0025(8) -0.0046(7) C1A 0.0372(10) 0.0332(10) 0.0193(10) 0.0090(8) -0.0022(8) -0.0002(8) C3A 0.0339(10) 0.0419(11) 0.0230(11) 0.0076(9) -0.0062(8) 0.0066(8) C6A 0.0440(11) 0.0445(11) 0.0225(10) 0.0109(8) -0.0013(8) 0.0144(9) C3 0.0288(9) 0.0471(11) 0.0204(10) 0.0061(8) 0.0052(8) -0.0015(8) C4A 0.0324(10) 0.0397(10) 0.0226(10) 0.0050(8) -0.0010(8) 0.0077(8) C7A 0.0429(11) 0.0426(11) 0.0217(10) 0.0083(9) 0.0030(8) 0.0153(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1A O6A 1.5072(13) . ? P1A O5A 1.5703(15) . ? P1A O3A 1.5063(15) . ? P1A O4A 1.5695(15) . ? P1 O6 1.5086(13) . ? P1 O5 1.5689(15) . ? P1 O3 1.5066(14) . ? P1 O4 1.5712(15) . ? O7 H7B 0.8495 . ? O7 H7C 0.8515 . ? O5A H5A 0.8200 . ? O5 H5 0.8200 . ? O7A H7AA 0.8499 . ? O7A H7AB 0.8512 . ? O4 H4B 0.8200 . ? O2 H2 0.8200 . ? O2 C1 1.305(3) . ? O4A H4AA 0.8200 . ? O1 C1 1.221(3) . ? O2A H2A 0.8200 . ? O2A C1A 1.307(2) . ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? N1 C5 1.456(2) . ? O1A C1A 1.215(3) . ? N1A H1AA 0.8900 . ? N1A H1AB 0.8900 . ? N1A H1AC 0.8900 . ? N1A C5A 1.461(2) . ? C5 C4 1.379(3) . ? C5 C6 1.391(3) . ? C1 C2 1.489(3) . ? C2 C7 1.393(3) . ? C2 C3 1.393(3) . ? C2A C1A 1.493(3) . ? C2A C3A 1.382(3) . ? C2A C7A 1.393(3) . ? C5A C6A 1.383(3) . ? C5A C4A 1.379(3) . ? C7 H7 0.9300 . ? C7 C6 1.382(3) . ? C4 H4 0.9300 . ? C4 C3 1.383(3) . ? C6 H6 0.9300 . ? C3A H3A 0.9300 . ? C3A C4A 1.383(3) . ? C6A H6A 0.9300 . ? C6A C7A 1.380(3) . ? C3 H3 0.9300 . ? C4A H4A 0.9300 . ? C7A H7A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6A P1A O5A 106.05(8) . . ? O6A P1A O4A 108.27(9) . . ? O3A P1A O6A 114.79(9) . . ? O3A P1A O5A 110.65(9) . . ? O3A P1A O4A 109.95(8) . . ? O4A P1A O5A 106.77(9) . . ? O6 P1 O5 106.05(8) . . ? O6 P1 O4 108.04(9) . . ? O5 P1 O4 106.83(9) . . ? O3 P1 O6 115.04(9) . . ? O3 P1 O5 110.21(9) . . ? O3 P1 O4 110.27(8) . . ? H7B O7 H7C 104.7 . . ? P1A O5A H5A 109.5 . . ? P1 O5 H5 109.5 . . ? H7AA O7A H7AB 104.6 . . ? P1 O4 H4B 109.5 . . ? C1 O2 H2 109.5 . . ? P1A O4A H4AA 109.5 . . ? C1A O2A H2A 109.5 . . ? H1A N1 H1B 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C5 N1 H1A 109.5 . . ? C5 N1 H1B 109.5 . . ? C5 N1 H1C 109.5 . . ? H1AA N1A H1AB 109.5 . . ? H1AA N1A H1AC 109.5 . . ? H1AB N1A H1AC 109.5 . . ? C5A N1A H1AA 109.5 . . ? C5A N1A H1AB 109.5 . . ? C5A N1A H1AC 109.5 . . ? C4 C5 N1 119.37(17) . . ? C4 C5 C6 121.33(18) . . ? C6 C5 N1 119.29(17) . . ? O2 C1 C2 114.40(17) . . ? O1 C1 O2 124.58(19) . . ? O1 C1 C2 121.02(19) . . ? C7 C2 C1 119.21(17) . . ? C3 C2 C1 121.42(18) . . ? C3 C2 C7 119.36(18) . . ? C3A C2A C1A 121.89(18) . . ? C3A C2A C7A 119.56(18) . . ? C7A C2A C1A 118.54(18) . . ? C6A C5A N1A 118.78(17) . . ? C4A C5A N1A 119.90(18) . . ? C4A C5A C6A 121.32(19) . . ? C2 C7 H7 119.6 . . ? C6 C7 C2 120.81(18) . . ? C6 C7 H7 119.6 . . ? C5 C4 H4 120.2 . . ? C5 C4 C3 119.53(18) . . ? C3 C4 H4 120.2 . . ? C5 C6 H6 120.6 . . ? C7 C6 C5 118.71(18) . . ? C7 C6 H6 120.6 . . ? O2A C1A C2A 114.17(18) . . ? O1A C1A O2A 124.39(19) . . ? O1A C1A C2A 121.43(18) . . ? C2A C3A H3A 119.8 . . ? C2A C3A C4A 120.32(18) . . ? C4A C3A H3A 119.8 . . ? C5A C6A H6A 120.5 . . ? C7A C6A C5A 118.90(19) . . ? C7A C6A H6A 120.5 . . ? C2 C3 H3 119.9 . . ? C4 C3 C2 120.23(18) . . ? C4 C3 H3 119.9 . . ? C5A C4A C3A 119.34(19) . . ? C5A C4A H4A 120.3 . . ? C3A C4A H4A 120.3 . . ? C2A C7A H7A 119.7 . . ? C6A C7A C2A 120.53(19) . . ? C6A C7A H7A 119.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O7 H7B O6A 0.85 1.88 2.7153(19) 168.3 2_767 yes O7 H7C O3 0.85 1.96 2.798(2) 168.7 1_655 yes O5A H5A O6 0.82 1.91 2.703(2) 163.4 1_655 yes O5 H5 O6A 0.82 1.93 2.722(2) 162.7 1_465 yes O7A H7AA O6 0.85 1.88 2.7209(19) 168.4 2_667 yes O7A H7AB O3A 0.85 1.89 2.7238(19) 164.6 1_455 yes O4 H4B O1 0.82 1.82 2.635(2) 174.2 2_666 yes O2 H2 O3 0.82 1.74 2.558(2) 172.6 2_666 yes O4A H4AA O1A 0.82 1.82 2.639(2) 176.1 2_756 yes O2A H2A O3A 0.82 1.76 2.573(2) 173.9 2_756 yes N1 H1A O7A 0.89 1.94 2.802(2) 163.4 . yes N1 H1B O6 0.89 1.93 2.809(2) 168.8 . yes N1 H1C O7 0.89 1.93 2.781(2) 160.5 . yes N1A H1AA O7 0.89 2.05 2.856(2) 151.0 1_545 yes N1A H1AB O7A 0.89 1.92 2.781(2) 162.4 . yes N1A H1AC O6A 0.89 1.95 2.822(2) 166.5 . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C7 168.67(18) . . . . ? O2 C1 C2 C3 -12.1(3) . . . . ? O1 C1 C2 C7 -11.0(3) . . . . ? O1 C1 C2 C3 168.2(2) . . . . ? N1 C5 C4 C3 -179.85(18) . . . . ? N1 C5 C6 C7 -178.92(17) . . . . ? N1A C5A C6A C7A 178.71(19) . . . . ? N1A C5A C4A C3A -179.58(18) . . . . ? C5 C4 C3 C2 -1.4(3) . . . . ? C1 C2 C7 C6 179.53(19) . . . . ? C1 C2 C3 C4 -178.27(19) . . . . ? C2 C7 C6 C5 -1.1(3) . . . . ? C2A C3A C4A C5A 1.2(3) . . . . ? C5A C6A C7A C2A 0.6(3) . . . . ? C7 C2 C3 C4 0.9(3) . . . . ? C4 C5 C6 C7 0.6(3) . . . . ? C6 C5 C4 C3 0.6(3) . . . . ? C1A C2A C3A C4A 176.81(19) . . . . ? C1A C2A C7A C6A -177.7(2) . . . . ? C3A C2A C1A O2A 7.0(3) . . . . ? C3A C2A C1A O1A -172.0(2) . . . . ? C3A C2A C7A C6A 1.1(3) . . . . ? C6A C5A C4A C3A 0.5(3) . . . . ? C3 C2 C7 C6 0.3(3) . . . . ? C4A C5A C6A C7A -1.4(3) . . . . ? C7A C2A C1A O2A -174.26(18) . . . . ? C7A C2A C1A O1A 6.8(3) . . . . ? C7A C2A C3A C4A -2.0(3) . . . . ? _shelx_res_file ; TITL exp_291_a.res in P-1 exp_291.res created by SHELXL-2018/3 at 20:19:06 on 11-Aug-2023 REM Old TITL exp_291 in P-1 REM SHELXT solution in P-1 REM R1 0.191, Rweak 0.011, Alpha 0.072, Orientation as input REM Formula found by SHELXT: C14 N O15 Cl2 CELL 1.54184 8.5238 8.9068 14.4976 106.456 90.195 92.811 ZERR 4 0.0002 0.0002 0.0004 0.002 0.002 0.002 LATT 1 SFAC C H N O P UNIT 28 48 4 28 4 EQIV $1 2-X,1-Y,2-Z EQIV $2 1+X,+Y,+Z EQIV $3 -1+X,1+Y,+Z EQIV $4 1-X,1-Y,2-Z EQIV $5 -1+X,+Y,+Z EQIV $6 1-X,1-Y,1-Z EQIV $7 2-X,-Y,1-Z EQIV $8 +X,-1+Y,+Z L.S. 4 0 0 PLAN 5 SIZE 0.2 0.4 0.6 TEMP 19.85 CONF HTAB O7 O6A_$1 HTAB O7 O3_$2 HTAB O5A O6_$2 HTAB O5 O6A_$3 HTAB O7A O6_$4 HTAB O7A O3A_$5 HTAB O4 O1_$6 HTAB O2 O3_$6 HTAB O4A O1A_$7 HTAB O2A O3A_$7 HTAB N1 O7 HTAB N1 O6 HTAB N1 O7A HTAB N1A O6A HTAB N1A O7_$8 HTAB N1A O7A BOND $H list 4 MORE -1 fmap 2 53 acta OMIT 2 1 0 OMIT -1 -2 1 OMIT 2 -1 0 OMIT -6 -2 14 OMIT -1 -2 17 OMIT -2 3 4 OMIT 1 -3 2 OMIT 2 3 4 OMIT -4 1 10 OMIT 4 1 10 OMIT -3 -1 3 OMIT 1 2 0 OMIT -2 4 5 OMIT 2 1 4 OMIT 1 0 1 OMIT 0 2 1 OMIT 1 0 2 OMIT 0 2 3 REM REM REM WGHT 0.130800 0.153500 EXTI 0.045702 FVAR 1.11359 P1A 5 1.173797 0.266794 0.865920 11.00000 0.03065 0.03062 = 0.01480 0.00780 -0.00083 -0.00199 P1 5 0.327353 0.778652 0.863289 11.00000 0.02975 0.02934 = 0.01417 0.00706 0.00007 0.00252 O6A 4 1.105168 0.150329 0.914502 11.00000 0.03872 0.03180 = 0.02090 0.01044 0.00043 -0.00321 AFIX 6 O7 4 0.902499 0.760362 0.890348 11.00000 0.03269 0.04148 = 0.01861 0.00764 0.00188 -0.00040 H7B 2 0.913901 0.786419 0.951148 11.00000 -1.50000 H7C 2 0.995589 0.751095 0.869098 11.00000 -1.50000 AFIX 0 O6 4 0.386659 0.661468 0.910791 11.00000 0.03720 0.03110 = 0.02075 0.00910 0.00058 0.00532 O5A 4 1.225841 0.417310 0.948915 11.00000 0.05434 0.03478 = 0.02000 0.00646 -0.00073 -0.01255 AFIX 147 H5A 2 1.275785 0.479202 0.926339 11.00000 -1.50000 AFIX 0 O5 4 0.282825 0.924228 0.947138 11.00000 0.05547 0.03659 = 0.01986 0.00571 -0.00062 0.01594 AFIX 147 H5 2 0.232189 0.982659 0.925257 11.00000 -1.50000 AFIX 6 O7A 4 0.593686 0.254687 0.893719 11.00000 0.03097 0.04267 = 0.01771 0.00875 -0.00127 0.00284 H7AA 2 0.589959 0.270872 0.954309 11.00000 -1.50000 H7AB 2 0.497995 0.240788 0.874891 11.00000 -1.50000 AFIX 0 O3A 4 1.309326 0.210231 0.801040 11.00000 0.03158 0.05518 = 0.01649 0.00885 0.00012 0.00116 O3 4 0.189220 0.720120 0.795325 11.00000 0.02947 0.05170 = 0.01648 0.00746 -0.00030 0.00224 O4 4 0.468157 0.834852 0.809463 11.00000 0.03936 0.05354 = 0.02048 0.01377 -0.00030 -0.01140 AFIX 147 H4B 2 0.452043 0.802526 0.751217 11.00000 -1.50000 AFIX 0 O2 4 0.801007 0.384089 0.387976 11.00000 0.03669 0.06381 = 0.01671 0.00759 0.00290 -0.00404 AFIX 147 H2 2 0.796005 0.348153 0.329283 11.00000 -1.50000 AFIX 0 O4A 4 1.038865 0.314370 0.807535 11.00000 0.04259 0.05361 = 0.02107 0.01293 0.00023 0.01130 AFIX 147 H4AA 2 1.060430 0.290193 0.750299 11.00000 -1.50000 AFIX 0 O1 4 0.565128 0.258747 0.379282 11.00000 0.05102 0.05494 = 0.01977 0.00789 -0.00178 -0.01522 O2A 4 0.710607 -0.079069 0.381469 11.00000 0.04401 0.05514 = 0.01785 0.00861 -0.00425 0.01118 AFIX 147 H2A 2 0.710883 -0.118451 0.323038 11.00000 -1.50000 AFIX 0 N1 3 0.666108 0.524413 0.835994 11.00000 0.03451 0.03110 = 0.01688 0.00781 0.00067 0.00249 AFIX 137 H1A 2 0.663625 0.439079 0.856439 11.00000 -1.20000 H1B 2 0.581215 0.577934 0.856040 11.00000 -1.20000 H1C 2 0.751901 0.584260 0.859482 11.00000 -1.20000 AFIX 0 O1A 4 0.905355 -0.238820 0.378497 11.00000 0.06482 0.05894 = 0.01909 0.00875 0.00158 0.02604 N1A 3 0.809663 0.024426 0.832474 11.00000 0.03307 0.03113 = 0.01704 0.00650 -0.00064 -0.00011 AFIX 137 H1AA 2 0.801895 -0.063463 0.850191 11.00000 -1.20000 H1AB 2 0.727913 0.081833 0.854337 11.00000 -1.20000 H1AC 2 0.898159 0.078586 0.856785 11.00000 -1.20000 AFIX 0 C5 1 0.668699 0.478560 0.731344 11.00000 0.03198 0.02550 = 0.01590 0.00699 0.00009 0.00298 C1 1 0.675472 0.337526 0.425572 11.00000 0.03525 0.03064 = 0.02109 0.00953 0.00080 0.00243 C2 1 0.674821 0.389145 0.532662 11.00000 0.03407 0.02847 = 0.01795 0.00771 0.00104 0.00235 C2A 1 0.813392 -0.092862 0.529498 11.00000 0.03392 0.02892 = 0.01728 0.00672 -0.00150 -0.00109 C5A 1 0.811342 -0.014456 0.727557 11.00000 0.03102 0.02695 = 0.01716 0.00665 -0.00160 -0.00364 C7 1 0.536416 0.370564 0.580028 11.00000 0.03377 0.03734 = 0.02278 0.00957 -0.00252 -0.00560 AFIX 43 H7 2 0.446083 0.327002 0.544379 11.00000 -1.20000 AFIX 0 C4 1 0.807123 0.496839 0.685783 11.00000 0.02829 0.04360 = 0.02043 0.00395 -0.00007 0.00043 AFIX 43 H4 2 0.897925 0.537859 0.721659 11.00000 -1.20000 AFIX 0 C6 1 0.531728 0.416067 0.679322 11.00000 0.03227 0.03936 = 0.02235 0.00960 0.00251 -0.00457 AFIX 43 H6 2 0.438779 0.405113 0.710751 11.00000 -1.20000 AFIX 0 C1A 1 0.814971 -0.143645 0.422155 11.00000 0.03719 0.03315 = 0.01930 0.00898 -0.00221 -0.00022 C3A 1 0.699093 0.000267 0.579720 11.00000 0.03391 0.04192 = 0.02305 0.00762 -0.00622 0.00665 AFIX 43 H3A 2 0.623349 0.037269 0.546571 11.00000 -1.20000 AFIX 0 C6A 1 0.929279 -0.104401 0.678893 11.00000 0.04397 0.04446 = 0.02252 0.01089 -0.00134 0.01445 AFIX 43 H6A 2 1.007235 -0.137666 0.712458 11.00000 -1.20000 AFIX 0 C3 1 0.809943 0.453749 0.586395 11.00000 0.02883 0.04705 = 0.02043 0.00609 0.00516 -0.00149 AFIX 43 H3 2 0.902395 0.467959 0.555323 11.00000 -1.20000 AFIX 0 C4A 1 0.696786 0.038726 0.679066 11.00000 0.03242 0.03968 = 0.02256 0.00504 -0.00098 0.00766 AFIX 43 H4A 2 0.618756 0.099840 0.712815 11.00000 -1.20000 AFIX 0 C7A 1 0.929342 -0.143955 0.579712 11.00000 0.04285 0.04256 = 0.02170 0.00826 0.00301 0.01532 AFIX 43 H7A 2 1.007416 -0.205208 0.546129 11.00000 -1.20000 AFIX 0 HKLF 4 REM exp_291_a.res in P-1 REM wR2 = 0.1712, GooF = S = 1.061, Restrained GooF = 1.061 for all data REM R1 = 0.0584 for 3839 Fo > 4sig(Fo) and 0.0624 for all 4149 data REM 304 parameters refined using 0 restraints END WGHT 0.1308 0.1535 REM Highest difference peak 0.664, deepest hole -0.430, 1-sigma level 0.106 Q1 1 1.0845 0.1823 0.8606 11.00000 0.05 0.66 Q2 1 1.1313 0.1345 0.8449 11.00000 0.05 0.66 Q3 1 0.2118 0.7369 0.8605 11.00000 0.05 0.63 Q4 1 1.1636 0.2808 0.9359 11.00000 0.05 0.62 Q5 1 0.4330 0.8598 0.8744 11.00000 0.05 0.60 ; _shelx_res_checksum 26880 _shelx_hkl_file ; 0 0 1 108.29 1.76 0 0 1 102.92 1.68 0 0 2 331.80 4.26 0 0 2 305.34 4.23 0 0 3 2355.38 14.10 0 0 3 1854.10 12.80 0 0 5 261.93 6.50 0 0 5 259.20 6.24 0 0 6 736.59 11.76 0 0 6 712.34 12.10 0 0 7 840.35 14.03 0 0 7 806.45 14.37 0 0 8 384.69 10.54 0 0 -8 314.89 9.09 0 0 9 250.78 8.13 0 0 -9 263.70 9.15 0 0 -10 433.75 13.58 0 0 10 372.08 10.77 0 0 -10 381.46 11.68 0 0 10 378.80 11.24 0 0 10 471.12 14.21 0 0 10 380.36 12.32 0 0 10 391.37 12.17 0 0 -10 331.66 9.40 0 0 10 409.30 11.24 0 0 11 455.40 12.69 0 0 11 463.07 13.27 0 0 11 439.25 14.28 0 0 12 614.35 15.76 0 0 12 598.46 17.67 0 0 12 620.35 16.21 0 0 13 53.58 5.08 0 0 13 53.57 4.98 0 0 13 51.44 5.57 0 0 13 55.23 5.11 0 0 14 5.10 2.17 0 0 14 9.14 2.72 0 0 14 6.73 2.63 0 0 15 706.96 16.78 0 0 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1351.88 42.70 0 -6 4 1657.17 37.75 0 -6 4 1753.46 30.14 0 -6 4 1710.49 33.14 0 6 -4 1520.02 26.08 0 6 -4 1692.41 42.82 0 6 -4 1603.53 32.56 0 -6 3 250.57 12.27 0 6 -3 210.74 12.44 0 6 -3 237.82 10.44 0 -6 3 254.04 11.26 0 6 -3 233.90 12.21 0 6 -3 246.88 15.18 0 -6 3 277.32 10.92 0 -6 3 258.31 14.79 0 6 -3 243.35 16.17 0 -6 2 42.07 9.13 0 -6 2 74.01 8.07 0 6 -2 58.96 6.69 0 6 -2 71.04 8.74 0 6 -2 82.18 6.10 0 6 -2 84.66 8.34 0 6 -2 67.34 6.61 0 6 -2 78.11 8.75 0 -6 2 88.16 5.89 0 6 -1 13.93 3.14 0 -6 1 15.49 2.42 0 -6 1 9.58 4.76 0 6 -1 15.66 4.11 0 6 -1 15.59 3.74 0 6 -1 12.91 3.81 0 -6 1 12.14 3.46 0 -6 0 495.16 20.51 0 6 0 484.91 22.36 0 6 0 505.49 18.23 0 6 0 497.81 22.19 0 6 1 356.53 15.49 0 6 1 496.65 19.93 0 -6 -1 329.23 16.72 0 -6 -1 190.38 20.31 0 6 1 331.20 18.70 0 6 1 334.35 18.54 0 6 2 1076.43 33.91 0 -6 -2 973.88 28.63 0 6 2 992.47 32.56 0 6 2 1090.90 27.87 0 6 3 285.50 17.70 0 6 3 308.69 15.29 0 -6 -3 250.22 14.39 0 6 4 200.54 15.08 0 6 4 225.44 13.46 0 6 4 201.34 12.35 0 6 5 272.96 17.39 0 6 5 278.52 14.79 0 6 5 279.37 15.05 0 6 6 25.00 4.59 0 -6 -6 21.75 4.17 0 6 6 23.70 5.81 0 -6 -7 430.76 16.37 0 6 7 523.91 20.28 0 6 8 1296.05 19.94 0 6 8 1215.96 30.00 0 6 9 221.18 7.83 0 6 9 180.60 11.00 0 6 10 2.21 1.05 0 6 10 2.66 1.55 0 -7 16 15.84 2.68 0 7 -16 22.44 4.12 0 -7 15 3.81 1.70 0 7 -15 4.51 2.56 0 -7 14 15.21 2.79 0 -7 14 5.61 2.08 0 7 -14 10.73 3.38 0 -7 14 4.91 2.60 0 7 -14 11.12 3.91 0 7 -13 285.17 14.83 0 7 -13 278.93 17.63 0 7 -12 102.77 9.11 0 -7 12 133.89 7.85 0 -7 12 47.87 5.85 0 -7 12 48.34 6.85 0 7 -12 95.83 10.75 0 7 -11 3.54 2.16 0 -7 11 5.01 1.81 0 -7 11 2.71 1.69 0 -7 11 7.56 2.83 0 7 -11 6.45 3.47 0 -7 10 59.88 7.22 0 7 -10 60.57 6.87 0 -7 10 82.59 6.02 0 -7 10 30.42 5.74 0 -7 10 25.70 4.41 0 7 -10 58.65 8.47 0 -7 9 28.75 4.68 0 7 -9 68.61 8.81 0 -7 9 89.49 8.64 0 -7 9 47.13 7.17 0 7 -9 78.12 7.80 0 7 -9 73.36 6.85 0 -7 9 67.74 7.37 0 -7 9 87.68 6.16 0 -7 8 41.31 5.61 0 7 -8 88.66 9.97 0 -7 8 108.00 9.06 0 -7 8 50.48 8.32 0 7 -8 75.72 6.95 0 -7 8 93.11 8.34 0 7 -8 87.00 7.94 0 -7 8 103.18 6.38 0 -7 8 71.68 8.72 0 7 -7 19.90 5.74 0 -7 7 27.39 6.49 0 7 -7 19.08 3.70 0 -7 7 21.46 5.21 0 -7 7 15.14 4.89 0 7 -7 16.20 3.74 0 -7 7 10.60 3.64 0 7 -7 22.63 5.05 0 -7 7 25.35 4.26 0 -7 7 22.86 4.28 0 7 -7 13.87 2.93 0 -7 6 224.24 11.56 0 7 -6 221.72 12.53 0 7 -6 208.00 14.18 0 -7 6 216.77 11.80 0 -7 6 195.90 14.07 0 7 -6 196.19 10.54 0 7 -6 239.32 16.25 0 -7 6 176.06 15.69 0 7 -6 202.17 11.23 0 -7 6 188.31 11.57 0 -7 6 219.53 13.53 0 7 -6 227.93 17.27 0 -7 5 63.95 6.29 0 7 -5 68.03 8.45 0 -7 5 51.76 7.33 0 7 -5 53.95 8.60 0 -7 5 61.92 5.89 0 7 -5 49.18 6.82 0 -7 5 63.60 7.07 0 -7 5 54.38 9.32 0 7 -5 61.24 6.35 0 7 -5 55.33 5.64 0 -7 5 55.20 7.96 0 7 -5 55.29 6.27 0 -7 5 66.69 6.93 0 7 -4 25.97 3.79 0 -7 4 28.27 3.86 0 -7 4 28.72 6.38 0 -7 4 27.06 5.49 0 7 -4 23.64 4.06 0 -7 4 19.13 4.69 0 7 -4 18.96 4.55 0 -7 4 30.22 4.61 0 7 -4 28.61 5.76 0 -7 4 25.70 3.92 0 7 -4 19.86 4.67 0 -7 4 14.80 5.72 0 7 -4 23.26 5.40 0 -7 4 42.62 5.81 0 7 -3 93.16 10.22 0 7 -3 88.21 7.91 0 -7 3 92.26 12.23 0 7 -3 104.21 9.82 0 7 -3 77.42 8.33 0 -7 3 99.76 10.93 0 -7 3 91.61 7.02 0 -7 3 68.27 11.68 0 7 -3 83.80 10.44 0 -7 3 90.80 9.38 0 -7 3 87.33 7.71 0 -7 2 65.63 6.34 0 7 -2 71.47 9.46 0 -7 2 38.37 9.14 0 7 -2 68.21 6.98 0 7 -2 95.51 9.26 0 7 -2 65.65 7.76 0 -7 2 81.42 8.86 0 -7 2 67.09 5.85 0 7 -2 73.46 9.07 0 7 -1 -0.21 1.22 0 -7 1 -1.15 2.95 0 7 -1 2.06 1.57 0 7 -1 -1.89 2.34 0 -7 1 2.69 1.98 0 7 -1 -4.58 2.78 0 7 0 6.04 4.02 0 7 0 7.76 3.92 0 -7 0 9.12 3.15 0 -7 0 3.51 4.42 0 7 0 8.88 3.11 0 7 0 14.88 3.59 0 7 1 1.36 3.21 0 7 1 0.91 2.09 0 7 1 4.54 1.98 0 -7 -1 0.60 4.42 0 -7 -1 5.03 3.15 0 7 1 2.95 3.37 0 -7 -2 96.54 9.02 0 7 2 96.82 11.39 0 7 2 124.25 9.88 0 7 2 101.72 8.52 0 7 3 48.51 6.13 0 7 3 44.76 7.48 0 7 3 59.08 6.90 0 -7 -3 46.42 6.06 0 7 4 30.33 4.99 0 7 4 20.41 5.39 0 -7 -4 24.17 4.25 0 7 4 31.33 4.88 0 -7 -5 15.22 3.18 0 7 5 12.13 3.05 0 7 5 14.80 4.47 0 -7 -6 0.84 0.99 0 7 6 -0.35 1.43 0 7 6 -0.49 1.50 0 7 7 8.27 2.77 0 7 8 53.13 5.55 0 7 9 3.91 1.45 0 -7 -9 4.16 1.92 0 8 -15 14.80 3.34 0 -8 15 9.74 1.96 0 -8 14 3.67 1.34 0 8 -14 6.51 2.81 0 8 -14 2.40 2.20 0 -8 14 2.41 1.53 0 -8 14 -0.31 0.88 0 -8 13 7.46 2.27 0 -8 13 12.44 2.13 0 8 -13 10.60 3.13 0 8 -13 8.56 3.61 0 -8 12 229.50 11.78 0 -8 12 212.03 13.40 0 8 -12 321.51 18.28 0 8 -12 315.23 14.31 0 -8 12 403.40 11.59 0 8 -11 80.41 9.68 0 -8 11 97.72 5.79 0 8 -11 72.33 7.16 0 -8 11 48.85 6.81 0 -8 11 58.32 6.18 0 8 -10 191.71 14.59 0 -8 10 154.30 10.27 0 -8 10 148.29 12.05 0 8 -10 177.72 11.10 0 8 -9 88.69 9.95 0 8 -9 87.81 7.77 0 -8 9 90.90 8.17 0 -8 9 82.21 7.77 0 -8 9 80.93 9.16 0 -8 8 301.23 18.45 0 8 -8 242.07 12.61 0 -8 8 263.06 13.79 0 8 -8 250.34 16.46 0 -8 8 283.04 13.99 0 8 -8 294.86 13.59 0 -8 8 256.15 16.23 0 -8 7 109.27 8.88 0 -8 7 96.17 10.14 0 -8 7 120.84 12.04 0 8 -7 100.90 8.13 0 8 -7 95.81 10.05 0 -8 7 100.49 8.20 0 8 -7 112.01 8.71 0 8 -6 477.11 22.02 0 -8 6 572.93 24.15 0 -8 6 610.73 20.65 0 8 -6 543.87 25.31 0 8 -6 515.10 26.97 0 -8 6 597.06 28.33 0 8 -6 544.33 17.82 0 -8 6 519.69 17.93 0 -8 6 493.65 20.18 0 8 -6 525.19 19.01 0 -8 5 4.04 1.93 0 8 -5 8.85 2.76 0 -8 5 10.15 3.09 0 8 -5 5.04 3.63 0 -8 5 10.46 3.28 0 -8 5 5.42 2.88 0 8 -5 7.17 3.46 0 -8 5 -0.18 2.65 0 -8 5 5.26 2.71 0 8 -5 5.41 2.79 0 -8 4 674.90 19.14 0 8 -4 681.50 22.11 0 -8 4 644.53 21.06 0 8 -4 671.13 30.43 0 -8 4 893.56 24.74 0 -8 4 755.41 26.87 0 -8 4 824.43 34.74 0 8 -4 653.51 24.89 0 -8 4 946.22 30.97 0 8 -4 707.12 29.08 0 8 -3 1138.39 28.42 0 8 -3 1141.94 37.08 0 -8 3 1234.96 33.91 0 -8 3 1066.43 23.08 0 8 -3 1073.40 38.15 0 -8 3 1027.70 25.32 0 8 -3 1149.13 32.54 0 -8 3 1296.79 43.56 0 8 -2 743.01 23.03 0 -8 2 874.05 30.89 0 -8 2 814.20 34.60 0 8 -2 698.48 20.39 0 8 -2 739.92 25.85 0 8 -2 733.86 29.58 0 -8 2 782.16 26.37 0 8 -2 690.94 30.33 0 -8 1 421.32 24.60 0 8 -1 381.64 15.43 0 8 -1 407.92 17.12 0 -8 1 424.19 18.87 0 8 -1 380.51 22.21 0 -8 1 400.68 20.97 0 -8 0 438.51 18.75 0 8 0 390.64 22.27 0 8 0 414.10 16.21 0 8 0 436.92 17.70 0 8 1 94.55 10.93 0 8 1 104.57 8.28 0 -8 -1 103.12 8.97 0 8 1 116.25 9.19 0 8 2 539.31 24.98 0 8 2 534.45 18.68 0 -8 -2 530.59 18.90 0 -8 -3 268.39 12.71 0 8 3 326.93 14.84 0 8 3 297.25 13.89 0 8 3 292.41 17.76 0 8 4 49.08 7.01 0 -8 -4 50.05 5.19 0 8 4 58.32 6.13 0 -8 -5 212.20 9.28 0 8 5 242.64 14.33 0 8 5 258.97 12.19 0 8 6 577.14 16.83 0 8 7 330.77 11.59 0 -8 -7 271.46 11.91 0 8 8 111.39 5.80 0 -9 14 78.59 4.62 0 -9 13 8.79 1.87 0 9 -13 9.36 2.37 0 9 -13 9.38 3.27 0 9 -12 71.78 5.68 0 9 -12 80.18 8.19 0 -9 12 76.26 6.90 0 -9 12 83.76 6.11 0 9 -11 5.14 2.93 0 9 -11 7.39 2.44 0 -9 11 6.21 2.02 0 -9 11 6.49 2.41 0 9 -10 39.41 4.55 0 -9 10 41.42 5.80 0 -9 10 39.03 4.66 0 9 -10 43.61 6.55 0 9 -9 9.86 2.63 0 -9 9 6.89 2.15 0 -9 9 6.33 2.91 0 9 -9 4.02 2.73 0 9 -8 1.71 2.35 0 9 -8 1.92 1.61 0 -9 8 -0.41 1.47 0 -9 8 2.33 1.73 0 -9 8 6.55 2.27 0 -9 8 2.03 2.13 0 9 -7 80.68 6.80 0 -9 7 90.73 8.98 0 -9 7 100.18 7.86 0 9 -7 81.95 8.89 0 -9 7 107.17 10.39 0 -9 7 83.70 6.67 0 -9 6 92.26 10.13 0 9 -6 70.23 6.47 0 -9 6 82.31 7.19 0 -9 6 64.26 5.70 0 -9 6 74.21 8.19 0 9 -6 67.09 9.40 0 9 -6 65.11 7.84 0 -9 5 3.64 2.72 0 -9 5 3.43 2.26 0 -9 5 8.14 2.07 0 9 -5 4.18 2.39 0 9 -5 7.54 2.50 0 -9 5 7.17 2.97 0 9 -4 3.73 3.31 0 9 -4 12.17 3.65 0 -9 4 11.05 2.36 0 -9 4 12.23 3.08 0 -9 4 10.67 2.98 0 -9 4 10.61 3.33 0 -9 4 6.64 3.39 0 9 -4 6.61 2.49 0 -9 3 116.71 8.15 0 -9 3 95.85 10.71 0 9 -3 83.17 7.26 0 9 -3 92.88 8.63 0 -9 3 111.52 9.48 0 -9 3 87.68 8.26 0 9 -3 68.80 9.37 0 -9 2 11.92 4.15 0 9 -2 8.51 2.02 0 -9 2 17.51 3.37 0 -9 2 9.75 3.03 0 -9 2 7.77 2.61 0 9 -2 7.96 2.46 0 9 -2 7.71 3.51 0 9 -1 6.25 2.08 0 -9 1 3.28 2.03 0 -9 1 5.20 2.37 0 9 -1 3.08 2.82 0 9 -1 4.24 1.99 0 -9 1 2.39 2.26 0 -9 0 -0.21 1.95 0 9 0 1.03 1.00 0 9 0 2.94 1.94 0 9 0 1.85 2.63 0 -9 0 3.08 2.22 0 9 1 9.63 3.79 0 -9 -1 13.57 2.99 0 -9 -1 15.31 3.70 0 9 1 13.48 2.96 0 9 1 14.26 2.85 0 -9 -1 10.50 3.45 0 -9 -2 14.72 3.28 0 -9 -2 18.02 3.00 0 9 2 18.05 3.08 0 9 2 21.86 3.49 0 -9 -2 17.89 4.02 0 9 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25.82 3 -5 12 1230.90 22.45 3 -5 13 214.49 9.82 3 -5 13 130.31 14.04 -3 5 -13 123.63 9.53 3 -5 13 91.54 9.08 3 -5 13 176.42 8.74 3 -5 14 37.24 7.72 -3 5 -14 47.33 5.65 3 -5 14 51.13 4.94 -3 5 -15 138.85 14.17 3 -5 15 134.19 7.68 3 -5 16 116.65 6.91 -3 5 -16 56.75 7.62 -3 4 12 37.77 3.74 -3 4 12 28.70 4.44 -3 4 11 2.96 1.98 -3 4 11 4.11 2.27 -3 4 10 -0.69 1.40 -3 4 10 4.88 2.56 -3 4 9 1.26 1.89 -3 4 9 3.48 2.14 -3 4 8 1423.47 24.36 -3 4 8 1360.98 32.38 3 -4 -7 30.29 9.62 -3 4 7 18.09 4.54 -3 4 7 34.84 3.87 -3 4 7 28.83 4.92 3 -4 -6 49.64 11.27 -3 4 6 42.69 6.14 3 -4 -6 41.72 7.17 -3 4 6 65.23 6.66 -3 4 5 70.47 6.32 -3 4 5 58.74 6.84 3 -4 -5 46.18 7.59 3 -4 -5 42.82 11.45 -3 4 5 83.19 5.45 -3 4 5 67.55 6.46 -3 4 4 398.26 14.74 -3 4 4 400.17 18.82 -3 4 4 358.29 14.13 3 -4 -4 250.38 17.35 -3 4 4 358.33 16.16 3 -4 -4 248.72 23.90 -3 4 3 4.47 2.10 3 -4 -3 6.72 2.87 -3 4 3 8.49 2.19 3 -4 -2 979.28 33.22 -3 4 2 1248.14 27.74 -3 4 1 91.27 7.28 3 -4 -1 50.73 7.45 -3 4 0 36.71 4.51 -3 4 0 39.59 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283.51 21.77 4 -6 7 286.53 17.19 -4 6 -7 273.24 13.15 4 -6 8 205.95 15.36 4 -6 8 202.05 12.47 -4 6 -8 174.29 10.68 4 -6 8 208.85 15.72 -4 6 -8 189.45 11.04 -4 6 -8 224.90 15.09 4 -6 8 189.91 13.91 4 -6 9 3.23 3.00 4 -6 9 3.51 2.11 4 -6 9 2.86 2.64 -4 6 -9 4.37 2.30 -4 6 -9 4.38 2.60 4 -6 9 2.97 2.34 4 -6 10 16.11 4.40 4 -6 10 18.51 5.84 4 -6 10 17.93 5.17 -4 6 -10 18.59 3.74 -4 6 -10 24.59 5.05 4 -6 11 90.28 11.20 4 -6 11 69.83 9.20 -4 6 -11 81.53 7.27 4 -6 11 57.85 7.39 4 -6 12 90.90 11.59 4 -6 12 71.20 9.08 -4 6 -12 87.22 7.32 4 -6 13 109.47 12.46 -4 6 -13 105.31 7.47 4 -6 14 -0.06 2.12 -4 6 -14 0.88 2.47 -4 6 -14 2.47 1.62 4 -6 15 19.31 4.75 -4 6 -15 -2.89 1.36 -4 5 11 229.59 10.70 -4 5 10 5.03 1.98 -4 5 9 55.56 6.20 -4 5 8 329.35 15.47 -4 5 7 2.27 1.63 -4 5 6 29.19 4.73 -4 5 5 759.54 23.12 -4 5 5 803.24 26.79 -4 5 5 984.50 23.56 4 -5 -5 372.44 39.63 4 -5 -5 544.43 27.20 4 -5 -5 499.00 39.21 -4 5 5 778.79 30.12 -4 5 4 107.76 8.12 -4 5 4 103.48 9.31 4 -5 -4 65.24 9.48 4 -5 -4 46.36 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1.91 -5 -7 9 3.46 1.81 5 7 -9 3.21 3.09 -5 -7 9 6.93 2.71 -5 -7 8 11.13 3.51 5 7 -8 10.71 3.77 -5 -7 8 9.46 2.30 -5 -7 8 7.09 2.47 5 7 -8 10.31 3.90 -5 -7 7 5.29 2.94 5 7 -7 5.97 3.22 -5 -7 7 7.26 1.93 -5 -7 7 3.33 2.01 5 7 -7 3.62 2.68 5 7 -6 84.14 8.80 -5 -7 6 104.36 8.61 5 7 -6 85.27 10.74 -5 -7 6 99.12 9.70 5 7 -5 17.62 5.00 5 7 -5 16.19 4.52 -5 -7 5 20.40 4.04 5 7 -5 23.45 6.07 -5 -7 5 19.99 4.68 5 7 -4 325.57 17.02 5 7 -4 283.68 14.09 -5 -7 4 350.39 15.72 5 7 -4 295.33 19.98 -5 -7 4 340.35 17.83 5 7 -3 140.77 10.94 -5 -7 3 184.96 11.51 -5 -7 3 164.46 10.72 5 7 -3 137.43 13.56 -5 -7 3 169.56 12.46 5 7 -2 75.56 7.84 -5 -7 2 75.72 7.61 -5 -7 2 68.01 6.90 5 7 -2 52.53 8.37 -5 -7 2 65.12 7.59 5 7 -1 147.53 10.52 -5 -7 1 166.68 11.19 -5 -7 1 136.05 9.40 5 7 -1 125.83 12.37 -5 -7 1 136.71 10.53 5 7 0 151.79 10.15 -5 -7 0 152.25 10.68 -5 -7 0 129.44 8.88 5 7 0 129.83 12.14 -5 -7 0 126.27 9.80 5 7 1 53.72 5.67 -5 -7 -1 56.88 6.57 -5 -7 -1 46.23 5.12 5 7 1 43.67 6.90 -5 -7 -1 45.81 5.67 -5 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2.83 1.19 5 9 -6 2.39 1.82 -5 -9 6 2.54 1.63 5 9 -5 49.83 4.38 -5 -9 5 45.27 3.85 5 9 -5 45.99 5.56 -5 -9 5 45.05 4.42 5 9 -4 159.99 7.64 -5 -9 4 156.07 6.97 5 9 -4 154.70 9.91 -5 -9 4 146.72 7.66 -5 -9 3 1.67 1.22 5 9 -3 1.74 1.63 5 9 -3 2.27 1.25 -5 -9 3 1.44 0.96 5 9 -3 1.60 1.97 -5 -9 2 2.57 1.26 5 9 -2 1.88 1.49 5 9 -2 3.46 1.27 -5 -9 2 -1.59 0.74 -5 -9 2 2.18 0.99 5 9 -2 3.45 1.94 -5 -9 1 1.86 1.07 5 9 -1 -1.51 1.58 -5 -9 1 -0.26 0.76 5 9 -1 -0.88 1.86 5 9 0 0.22 0.76 5 9 0 1.14 1.35 6 -9 0 8.42 3.01 -6 9 -1 86.73 7.81 6 -9 1 73.69 8.54 6 -9 1 76.98 4.39 -6 9 -2 7.46 2.88 6 -9 2 2.07 2.72 -6 9 -2 4.95 1.00 6 -9 2 3.95 1.40 -6 9 -3 4.50 2.70 6 -9 3 2.74 2.76 6 -9 3 3.82 1.21 -6 9 -3 3.57 0.98 6 -9 3 3.31 1.30 6 -9 4 20.21 2.82 -6 9 -4 22.74 2.10 6 -9 4 24.06 3.03 -6 9 -4 23.01 4.70 6 -9 5 67.12 5.09 -6 9 -5 65.65 3.51 6 -9 5 73.87 5.13 -6 9 -5 76.86 8.19 -6 9 -6 11.15 3.68 6 -9 6 13.47 2.56 -6 9 -6 10.79 1.51 6 -9 6 10.69 2.20 6 -9 7 115.27 6.70 -6 9 -7 106.91 4.37 6 -9 7 124.59 6.47 6 -9 8 2.19 1.04 6 -9 8 3.96 1.63 -6 9 -8 2.58 0.83 6 -8 -3 7.52 3.24 -6 8 2 13.67 3.53 6 -8 -2 11.28 4.50 6 -8 -2 10.49 1.82 6 -8 -1 39.81 7.55 -6 8 1 45.45 3.19 6 -8 -1 45.73 3.99 -6 8 1 42.05 6.22 6 -8 0 36.70 7.66 -6 8 0 52.99 3.74 6 -8 0 51.43 4.61 -6 8 0 53.35 7.44 6 -8 1 58.71 9.95 6 -8 1 63.60 5.20 -6 8 -1 71.44 4.58 6 -8 1 71.71 5.77 -6 8 -1 58.17 8.28 6 -8 2 80.92 11.78 6 -8 2 95.57 7.00 -6 8 -2 94.59 5.25 -6 8 -2 94.68 10.46 6 -8 2 103.84 7.23 -6 8 -3 21.64 5.67 6 -8 3 17.53 6.23 6 -8 3 19.60 3.46 -6 8 -3 19.76 2.55 -6 8 -3 17.84 3.54 6 -8 3 18.37 3.43 6 -8 4 44.21 8.80 6 -8 4 41.02 5.04 -6 8 -4 47.17 3.84 -6 8 -4 45.97 5.63 6 -8 4 46.34 5.28 -6 8 -4 44.33 7.48 6 -8 5 227.67 18.80 6 -8 5 212.13 11.61 -6 8 -5 212.01 7.98 -6 8 -5 200.57 11.44 6 -8 5 216.29 11.06 -6 8 -5 201.19 16.04 6 -8 6 246.00 11.82 6 -8 6 234.55 12.28 -6 8 -6 209.01 7.85 -6 8 -6 235.35 12.17 -6 8 -6 235.58 17.21 -6 8 -7 3.61 3.45 6 -8 7 4.44 2.08 -6 8 -7 6.80 1.61 -6 8 -7 7.79 2.57 6 -8 7 8.06 2.55 6 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2.37 6 -7 4 5.52 2.48 -6 7 -5 11.57 4.97 6 -7 5 9.69 4.94 6 -7 5 11.73 3.48 -6 7 -5 17.60 2.76 -6 7 -5 10.36 3.37 6 -7 5 9.85 3.06 -6 7 -6 9.39 4.53 6 -7 6 5.20 2.36 6 -7 6 8.45 4.25 -6 7 -6 9.25 3.08 6 -7 6 7.22 3.04 -6 7 -6 8.55 2.05 -6 7 -6 7.78 3.03 6 -7 6 6.52 2.60 -6 7 -7 10.34 5.29 6 -7 7 12.20 3.53 6 -7 7 2.51 3.01 -6 7 -7 16.03 3.80 6 -7 7 10.84 3.40 -6 7 -7 14.98 2.58 -6 7 -7 10.39 3.36 6 -7 7 12.74 3.48 -6 7 -8 8.72 4.76 6 -7 8 9.49 3.42 -6 7 -8 14.11 3.79 6 -7 8 15.80 3.97 -6 7 -8 11.47 2.23 -6 7 -8 11.62 2.92 6 -7 8 15.61 3.70 6 -7 9 29.43 5.18 -6 7 -9 31.56 5.03 6 -7 9 24.66 4.68 -6 7 -9 30.77 3.30 -6 7 -9 32.29 4.86 6 -7 9 33.05 4.94 6 -7 10 399.67 19.03 -6 7 -10 453.81 17.74 6 -7 10 439.22 18.19 -6 7 -10 426.15 11.08 6 -7 10 433.80 16.15 6 -7 11 56.05 7.13 -6 7 -11 70.26 6.86 6 -7 11 63.33 6.63 -6 7 -11 64.14 3.94 6 -7 11 60.11 5.84 6 -7 12 196.99 12.30 -6 7 -12 234.93 11.40 6 -7 12 211.72 9.94 -6 6 8 265.88 10.01 -6 6 7 138.81 7.91 6 -6 -6 7.91 3.80 -6 6 6 7.76 2.11 6 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-9 37.94 2.43 9 -2 9 34.69 4.42 -9 1 8 34.83 2.55 9 -1 -8 28.95 5.57 9 -1 -7 -1.99 1.48 -9 1 7 1.18 0.76 9 -1 -7 -1.91 2.67 -9 1 7 0.18 1.12 9 -1 -6 193.58 11.49 -9 1 6 223.29 7.54 9 -1 -5 246.34 13.88 -9 1 5 283.03 8.87 -9 1 4 54.59 3.83 9 -1 -4 47.66 6.74 -9 1 4 50.61 3.98 -9 1 3 103.59 5.48 9 -1 -3 89.31 9.25 -9 1 3 117.90 8.60 9 -1 -3 78.58 9.35 -9 1 3 106.61 5.79 -9 1 2 133.38 6.38 9 -1 -2 109.55 10.48 -9 1 2 151.82 10.11 9 -1 -2 109.44 11.74 -9 1 2 139.84 6.63 -9 1 1 79.39 4.98 9 -1 -1 70.50 8.71 -9 1 1 81.46 7.46 9 -1 -1 68.62 9.78 -9 1 1 81.77 5.08 -9 1 0 184.57 7.56 9 -1 0 180.79 13.62 -9 1 0 192.14 11.59 -9 1 0 205.08 7.89 -9 1 -1 677.30 14.16 9 -1 1 708.02 26.75 9 -1 1 653.97 30.58 -9 1 -2 66.15 4.44 9 -1 2 63.62 7.51 9 -1 2 68.15 8.32 -9 1 -2 66.57 6.73 9 -1 2 67.41 10.27 -9 1 -3 12.04 2.02 9 -1 3 18.85 4.31 9 -1 3 14.19 3.78 9 -1 3 10.56 4.76 -9 1 -3 12.61 3.09 -9 1 -4 138.08 6.17 9 -1 4 126.73 10.75 9 -1 4 156.92 11.34 -9 1 -4 140.79 9.20 9 -1 4 127.85 13.36 -9 1 -5 443.42 10.71 9 -1 5 486.90 18.80 -9 1 -5 444.48 15.60 9 -1 5 435.24 23.77 -9 1 -6 213.25 7.14 9 -1 6 243.88 12.14 -9 1 -6 217.52 10.24 9 -1 6 217.54 16.04 -9 1 -7 103.64 4.77 9 -1 7 91.62 8.46 -9 1 -7 99.19 6.43 9 -1 7 114.68 11.01 -9 1 -7 88.50 6.90 -9 1 -8 241.85 6.61 9 -1 8 232.34 12.24 -9 1 -8 243.83 8.80 -9 1 -8 226.37 10.26 -9 1 -9 258.04 6.05 9 -1 9 252.03 11.33 -9 0 8 21.42 2.00 9 0 -8 15.57 4.29 9 0 -7 22.03 3.38 -9 0 7 19.90 2.11 9 0 -7 16.47 5.26 -9 0 6 82.14 4.55 9 0 -6 65.11 6.54 -9 0 6 80.07 4.45 9 0 -6 61.00 9.37 -9 0 5 26.16 2.88 9 0 -5 23.49 4.29 -9 0 5 26.86 2.67 9 0 -5 20.33 5.96 -9 0 4 28.01 3.07 9 0 -4 18.30 4.21 -9 0 4 26.17 2.72 9 0 -4 15.49 5.16 -9 0 3 3.65 1.33 9 0 -3 2.50 2.01 9 0 -3 1.64 2.65 -9 0 3 1.72 1.81 -9 0 3 1.79 0.95 9 0 -3 -3.46 3.53 -9 0 2 2.65 1.23 9 0 -2 0.02 1.95 9 0 -2 0.34 2.19 -9 0 2 0.30 1.89 -9 0 2 1.36 1.04 -9 0 1 0.87 0.92 9 0 -1 0.33 2.04 9 0 -1 -0.13 3.02 -9 0 1 1.47 1.51 -9 0 1 3.41 1.21 9 0 -1 2.46 3.73 -9 0 0 11.05 2.04 9 0 0 7.81 3.40 9 0 0 6.71 3.77 -9 0 0 11.31 3.10 -9 0 0 15.02 2.05 9 0 0 10.10 5.41 -9 0 -1 0.92 1.04 9 0 1 2.88 2.12 9 0 1 -1.69 2.40 9 0 1 1.08 3.21 -9 0 -1 -0.22 1.88 -9 0 -1 1.17 0.66 9 0 1 -3.71 2.58 -9 0 -2 -1.10 1.43 9 0 2 0.05 2.52 9 0 2 -3.00 2.58 9 0 2 0.11 3.56 -9 0 -2 1.76 1.54 -9 0 -3 27.60 2.91 9 0 3 27.27 5.29 9 0 3 34.12 5.44 -9 0 -3 31.24 4.47 9 0 3 27.30 6.34 -9 0 -4 16.32 3.16 -9 0 -4 19.39 2.46 9 0 4 25.98 4.63 9 0 4 17.08 4.09 -9 0 -4 20.44 3.48 9 0 4 20.61 5.55 9 0 4 24.68 3.12 -9 0 -5 29.74 2.87 9 0 5 31.40 5.41 9 0 5 33.21 4.88 -9 0 -5 29.74 3.84 9 0 5 31.45 6.44 9 0 5 38.09 3.60 -9 0 -5 28.90 4.35 -9 0 -6 56.31 3.61 9 0 6 50.01 6.40 9 0 6 59.74 5.96 -9 0 -6 54.15 4.78 9 0 6 53.47 7.90 -9 0 -6 52.91 5.67 -9 0 -7 81.70 4.01 9 0 7 77.79 7.35 9 0 7 94.94 6.57 -9 0 -7 80.77 5.19 9 0 7 94.81 9.53 -9 0 -7 80.80 6.55 -9 0 -8 0.87 1.15 -9 0 -8 -0.39 0.76 9 0 8 -0.36 1.89 9 1 -9 308.96 13.06 9 1 -8 39.73 5.48 -9 -1 8 56.23 2.91 9 1 -8 55.78 7.64 -9 -1 7 145.54 5.10 9 1 -7 131.17 12.61 -9 -1 6 103.36 5.53 9 1 -6 89.53 6.96 -9 -1 6 103.68 4.55 9 1 -6 85.23 10.89 9 1 -5 363.94 15.20 -9 -1 5 388.68 9.00 9 1 -5 341.71 22.39 -9 -1 4 98.65 5.84 9 1 -4 85.65 7.87 9 1 -4 81.05 11.37 -9 -1 3 40.40 3.87 9 1 -3 30.79 5.20 -9 -1 3 42.36 5.63 9 1 -3 25.78 6.56 -9 -1 2 222.28 8.81 9 1 -2 197.95 12.57 9 1 -2 188.81 14.54 9 1 -2 181.82 16.70 -9 -1 1 122.67 6.53 9 1 -1 113.99 9.87 -9 -1 1 140.55 9.78 9 1 -1 103.48 11.29 9 1 -1 99.79 12.51 -9 -1 0 37.04 3.59 9 1 0 39.63 5.74 9 1 0 35.62 5.63 -9 -1 0 42.55 5.35 9 1 0 32.01 6.81 9 1 0 29.41 7.24 -9 -1 -1 0.72 1.01 9 1 1 1.22 1.67 9 1 1 -1.07 1.75 9 1 1 3.35 3.27 -9 -1 -1 0.77 1.77 9 1 1 -0.13 2.46 -9 -1 -2 237.37 8.26 9 1 2 252.12 14.57 9 1 2 238.18 13.72 -9 -1 -2 254.05 12.03 9 1 2 234.96 17.23 -9 -1 -3 138.98 6.11 9 1 3 156.31 11.52 9 1 3 143.18 10.15 -9 -1 -3 146.96 8.79 9 1 3 146.64 13.50 -9 -1 -3 151.98 9.56 -9 -1 -4 1.85 1.79 -9 -1 -4 1.44 0.95 9 1 4 2.14 1.87 9 1 4 0.37 1.87 9 1 4 -0.95 2.28 -9 -1 -4 1.83 1.19 9 1 4 1.85 1.04 -9 -1 -5 127.10 5.26 9 1 5 138.37 10.25 9 1 5 145.66 9.21 -9 -1 -5 140.61 7.39 9 1 5 145.97 12.64 9 1 5 167.39 7.28 -9 -1 -5 128.37 8.47 -9 -1 -6 74.05 3.73 9 1 6 77.49 7.25 9 1 6 84.46 6.55 9 1 6 96.35 5.15 -9 -1 -6 80.95 6.42 -9 -1 -7 82.77 3.54 9 1 7 90.70 7.18 9 1 7 102.08 6.35 9 1 7 82.50 4.24 -9 -1 -7 90.78 6.28 9 1 8 42.65 4.32 9 2 -8 74.88 6.85 9 2 -8 111.22 10.06 9 2 -7 23.21 4.06 9 2 -7 40.58 6.75 -9 -2 6 1.90 0.98 9 2 -6 3.01 1.75 9 2 -6 4.57 3.20 -9 -2 5 70.09 4.80 9 2 -5 65.27 5.74 9 2 -5 65.41 9.40 -9 -2 4 104.23 5.91 9 2 -4 84.72 6.98 9 2 -4 84.23 10.78 -9 -2 3 40.89 3.77 9 2 -3 37.77 5.03 9 2 -3 32.87 7.13 -9 -2 2 3.19 1.28 9 2 -2 4.12 1.91 9 2 -2 8.59 3.18 -9 -2 2 2.81 2.09 9 2 -2 4.52 3.04 -9 -2 1 163.81 7.26 9 2 -1 144.05 9.86 -9 -2 1 172.21 10.27 9 2 -1 149.93 12.83 9 2 -1 145.83 13.77 -9 -2 0 99.88 5.54 9 2 0 124.37 9.56 9 2 0 98.67 8.14 -9 -2 0 105.16 7.77 9 2 0 83.29 9.83 9 2 0 94.81 10.66 -9 -2 -1 114.78 5.71 9 2 1 137.17 10.12 9 2 1 115.20 8.63 -9 -2 -1 115.89 7.88 9 2 1 110.70 11.36 9 2 1 4.90 2.19 -9 -2 -1 30.35 4.03 -9 -2 -2 17.50 2.22 9 2 2 22.95 4.32 9 2 2 17.34 3.48 -9 -2 -2 16.90 3.07 9 2 2 17.37 4.94 -9 -2 -2 18.66 3.27 -9 -2 -3 48.84 3.40 9 2 3 59.70 6.69 9 2 3 56.20 5.82 -9 -2 -3 53.86 4.78 9 2 3 56.03 7.93 9 2 3 61.60 4.64 -9 -2 -3 59.83 5.81 -9 -2 -4 4.59 1.80 -9 -2 -4 4.47 1.12 9 2 4 4.05 1.54 9 2 4 4.22 2.12 -9 -2 -4 5.56 1.54 9 2 4 6.50 1.57 -9 -2 -5 8.07 2.18 -9 -2 -5 5.77 1.06 9 2 5 6.68 1.90 9 2 5 8.16 2.68 9 2 5 7.26 1.64 -9 -2 -6 10.03 1.22 9 2 6 12.68 2.48 9 2 6 11.09 2.68 9 2 6 14.41 1.93 -9 -2 -6 13.64 2.56 9 2 7 -0.52 1.33 9 3 -8 51.78 4.97 9 3 -8 82.18 8.12 9 3 -7 0.73 0.71 9 3 -7 -1.09 2.51 -9 -3 6 210.28 7.39 9 3 -6 3.19 1.48 9 3 -6 196.61 14.18 -9 -3 5 102.29 5.42 -9 -3 5 89.84 4.42 9 3 -5 104.67 10.81 -9 -3 4 18.94 2.40 -9 -3 4 13.43 1.92 9 3 -4 14.62 4.00 -9 -3 3 4.29 1.37 9 3 -3 3.37 1.54 9 3 -3 2.53 2.51 -9 -3 2 180.16 7.13 9 3 -2 165.57 8.94 9 3 -2 180.44 14.20 -9 -3 1 765.62 14.14 9 3 -1 759.41 19.65 9 3 -1 788.51 28.55 -9 -3 0 67.35 4.09 9 3 0 71.80 6.11 9 3 0 76.78 8.35 -9 -3 -1 4.44 1.92 -9 -3 -1 4.06 1.22 9 3 1 3.09 2.16 9 3 1 4.73 2.04 9 3 1 5.05 2.27 -9 -3 -2 448.11 9.37 9 3 2 601.33 18.96 9 3 2 466.87 14.88 9 3 2 528.22 12.49 -9 -3 -2 542.61 15.78 -9 -3 -3 264.04 6.63 9 3 3 367.85 14.23 9 3 3 298.92 11.47 9 3 3 321.45 9.25 -9 -3 -3 318.85 11.82 9 3 4 93.95 6.83 9 3 4 77.24 5.55 9 3 4 82.41 4.43 -9 -3 -4 84.07 5.77 -9 -3 -5 0.52 1.01 9 3 5 0.86 1.08 9 3 5 1.46 0.95 9 3 5 0.80 0.77 9 4 -7 111.13 8.88 -9 -4 6 4.32 0.93 9 4 -6 5.60 2.92 -9 -4 5 10.87 1.66 -9 -4 5 8.27 1.42 9 4 -5 6.49 2.98 -9 -4 4 46.90 3.25 -9 -4 4 43.25 3.13 9 4 -4 46.05 6.51 -9 -4 3 2.52 0.95 9 4 -3 1.25 2.46 -9 -4 2 51.11 3.28 9 4 -2 52.96 6.68 -9 -4 1 36.98 2.67 9 4 -1 32.81 3.41 9 4 -1 41.10 5.69 -9 -4 0 15.18 1.67 9 4 0 14.38 2.38 9 4 0 14.68 2.01 -9 -4 0 15.44 2.46 -9 -4 -1 -0.77 0.86 -9 -4 -1 -0.57 0.54 9 4 1 -0.02 0.87 9 4 1 0.40 0.68 -9 -4 -2 1.42 0.97 9 4 2 1.34 1.19 9 4 2 0.99 0.78 9 4 3 45.83 3.68 9 4 3 43.49 2.82 -9 -4 -3 45.49 3.76 -9 -5 5 277.50 6.33 9 5 -5 460.29 15.90 -9 -5 4 9.92 1.35 9 5 -4 17.66 3.36 -9 -5 3 37.34 2.53 9 5 -3 57.05 5.78 9 5 -2 105.39 7.33 10 -4 1 16.85 3.56 -10 4 -1 12.57 1.34 10 -4 2 6.02 2.55 -10 4 -2 4.24 0.85 10 -4 3 3.59 1.87 10 -3 -3 1.04 1.10 10 -3 -2 13.85 2.80 -10 3 2 11.01 1.31 10 -3 -2 11.76 2.98 10 -3 -1 168.28 8.93 10 -3 -1 149.59 9.65 -10 3 1 154.78 4.81 10 -3 0 147.95 8.58 10 -3 0 131.66 9.83 -10 3 0 123.75 4.43 10 -3 1 109.28 7.27 10 -3 1 97.32 8.87 -10 3 -1 87.03 3.71 10 -3 2 42.53 4.30 -10 3 -2 49.32 3.90 10 -3 2 42.15 6.07 -10 3 -2 33.01 2.29 -10 3 -3 110.41 5.84 10 -3 3 97.48 8.87 -10 3 -4 316.78 9.66 10 -3 4 298.90 14.63 -10 3 -5 0.52 0.86 10 -2 -4 2.42 1.49 -10 2 4 0.86 0.51 10 -2 -4 0.91 1.94 10 -2 -3 19.75 3.31 -10 2 3 18.86 1.72 10 -2 -3 17.55 4.49 10 -2 -2 0.86 1.56 -10 2 2 0.39 0.51 10 -2 -2 0.78 2.17 10 -2 -1 8.45 2.47 10 -2 -1 6.13 2.44 -10 2 1 5.32 1.79 -10 2 1 6.15 1.12 10 -2 -1 10.22 3.02 10 -2 0 20.55 3.58 -10 2 0 23.00 3.03 10 -2 0 17.89 4.07 -10 2 0 19.24 1.86 10 -2 1 140.06 8.77 -10 2 -1 139.22 7.22 10 -2 1 126.50 10.47 -10 2 -2 -1.05 0.42 10 -2 2 0.21 1.27 10 -2 2 0.86 1.99 -10 2 -2 -0.81 1.00 -10 2 -2 0.75 0.52 -10 2 -3 0.41 0.31 10 -2 3 5.08 1.90 10 -2 3 4.44 2.38 -10 2 -3 4.11 1.48 -10 2 -3 3.26 0.71 -10 2 -4 58.08 2.77 10 -2 4 64.20 5.03 -10 2 -4 65.79 4.82 10 -2 4 64.55 7.36 -10 2 -5 16.47 2.35 10 -2 5 15.96 3.54 10 -1 -5 38.92 5.54 10 -1 -4 240.88 10.22 -10 1 4 215.12 5.35 10 -1 -4 228.83 14.31 10 -1 -3 91.55 6.81 -10 1 3 78.20 3.37 10 -1 -3 76.11 8.59 10 -1 -2 116.38 8.00 10 -1 -2 99.33 8.07 -10 1 2 103.26 3.98 10 -1 -2 110.00 10.30 -10 1 1 8.64 1.28 10 -1 -1 7.07 2.36 10 -1 -1 9.19 3.07 -10 1 1 9.64 2.24 -10 1 1 6.92 1.09 10 -1 -1 8.15 2.83 -10 1 0 22.12 2.05 10 -1 0 20.27 3.58 -10 1 0 23.10 3.23 10 -1 0 17.32 4.28 -10 1 0 16.77 1.64 -10 1 -1 0.85 0.57 10 -1 1 1.93 1.46 10 -1 1 1.76 2.20 -10 1 -1 0.82 1.03 -10 1 -2 4.30 0.95 10 -1 2 6.05 1.97 10 -1 2 3.17 2.40 -10 1 -2 4.68 1.55 -10 1 -3 1.48 0.74 10 -1 3 2.55 1.44 10 -1 3 3.48 2.69 -10 1 -3 2.22 1.23 -10 1 -4 125.22 4.34 10 -1 4 147.88 7.79 -10 1 -4 139.45 6.95 10 -1 4 139.60 10.53 -10 1 -5 73.48 3.15 -10 1 -5 87.53 5.09 10 -1 5 88.94 8.03 10 0 -5 2.67 2.34 -10 0 4 21.67 1.84 10 0 -4 24.18 3.29 10 0 -4 21.18 4.85 -10 0 3 0.44 0.51 10 0 -3 1.14 1.00 10 0 -3 -0.75 1.39 -10 0 2 56.44 3.38 10 0 -2 54.65 5.32 10 0 -2 49.74 6.98 -10 0 1 4.85 1.12 10 0 -1 5.62 2.01 10 0 -1 6.47 2.83 -10 0 1 5.56 1.82 10 0 -1 7.75 2.94 -10 0 0 256.58 7.26 10 0 0 248.46 11.40 -10 0 0 282.20 10.86 10 0 0 246.35 13.95 -10 0 -1 1.46 0.78 10 0 1 1.15 1.13 10 0 1 0.19 1.37 -10 0 -1 3.41 1.31 -10 0 -2 20.70 2.04 10 0 2 21.06 3.34 -10 0 -2 22.89 3.06 10 0 2 16.83 3.97 -10 0 -3 3.91 0.99 10 0 3 5.81 1.84 10 0 3 3.44 2.04 -10 0 -3 5.27 1.63 10 0 3 -0.89 0.56 -10 0 -4 24.00 1.99 10 0 4 26.10 3.30 -10 0 -4 22.38 2.72 10 0 4 27.38 4.94 -10 0 -5 4.06 0.82 10 1 -5 31.02 5.03 -10 -1 4 103.44 4.33 10 1 -4 94.23 5.46 10 1 -4 103.76 9.35 -10 -1 3 59.45 3.44 10 1 -3 57.33 4.83 10 1 -3 51.58 6.88 -10 -1 2 9.67 1.49 10 1 -2 10.14 2.18 10 1 -2 8.74 3.19 -10 -1 1 4.42 1.11 10 1 -1 3.25 1.64 10 1 -1 6.92 2.80 10 1 -1 6.04 2.99 -10 -1 0 299.25 7.75 10 1 0 301.61 11.65 10 1 0 319.82 15.00 -10 -1 -1 18.57 1.92 10 1 1 16.91 2.87 -10 -1 -1 19.96 2.84 10 1 1 22.70 4.25 -10 -1 -2 53.96 3.10 10 1 2 55.52 4.89 -10 -1 -2 58.62 4.42 10 1 2 60.24 6.84 10 1 2 63.18 3.67 -10 -1 -3 102.27 3.98 10 1 3 113.21 6.55 -10 -1 -3 112.54 5.67 10 1 3 108.01 4.47 -10 -1 -4 170.00 4.73 10 1 4 190.63 7.72 10 2 -5 12.21 3.25 -10 -2 4 21.41 2.00 10 2 -4 20.46 4.10 -10 -2 3 10.03 1.44 10 2 -3 11.78 3.52 -10 -2 2 0.68 0.71 10 2 -2 -0.86 0.97 10 2 -2 -0.44 2.18 -10 -2 1 270.52 6.97 10 2 -1 262.46 9.36 -10 -2 0 56.35 3.15 10 2 0 53.10 4.36 -10 -2 -1 0.33 0.59 10 2 1 -0.08 1.05 10 2 1 1.02 0.66 -10 -2 -2 0.95 0.57 10 2 2 1.33 1.09 10 2 2 0.23 0.57 10 3 -1 78.37 3.54 0 0 0 0.00 0.00 TITL exp_291 in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 8.523835 8.906782 14.497603 106.4561 90.1947 92.8107 ZERR 5.00 0.000201 0.000203 0.000409 0.0022 0.0021 0.0019 LATT 1 SFAC C H N O UNIT 55.00 50.00 5.00 5.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 41300 _database_code_depnum_ccdc_archive '0000 0001 5448' _olex2_submission_original_sample_id 4-CAH2PO4.H2O _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 5.151 _oxdiff_exptl_absorpt_empirical_full_min 0.307