#============================================================================== data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 12 _journal_issue 1 _journal_year 2021 _journal_page_first 52 _journal_page_last 55 #============================================================================== data_180524RAL_MW_HERO_100K_0m_a _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H22 N O4, Cl, 3(H2 O)' _chemical_formula_sum 'C19 H28 Cl N O7' _chemical_formula_weight 417.87 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' 'Cl' 'Cl' 0.3639 0.7018 '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' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.9367(2) _cell_length_b 13.0374(3) _cell_length_c 21.9856(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1988.30(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6849 _cell_measurement_theta_min 3.94 _cell_measurement_theta_max 68.63 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_F_000 888 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.209 _exptl_crystal_size_mid 0.121 _exptl_crystal_size_min 0.101 _exptl_absorpt_coefficient_mu 2.066 _shelx_estimated_absorpt_T_min 0.672 _shelx_estimated_absorpt_T_max 0.819 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.710 _exptl_absorpt_correction_T_max 0.849 _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_special_details ; 'crystal mounted on a Cryoloop using Paratone-N' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD Apex-II area-detector' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18382 _diffrn_reflns_av_unetI/netI 0.0456 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 4.021 _diffrn_reflns_theta_max 69.116 _diffrn_reflns_theta_full 67.679 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.983 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.972 _diffrn_reflns_point_group_measured_fraction_full 0.989 _reflns_number_total 3594 _reflns_number_gt 3181 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.707 _reflns_Friedel_fraction_max 0.956 _reflns_Friedel_fraction_full 0.978 _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. ; _computing_data_collection 'APEX 2 (Bruker, 2006)' _computing_cell_refinement 'APEX 2' _computing_data_reduction 'SAINT (Bruker, 2005)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'SHELXTL' _computing_publication_material 'SHELXTL' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+0.5682P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 1178 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.05(1) _chemical_absolute_configuration syn _refine_ls_number_reflns 3594 _refine_ls_number_parameters 271 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1026 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Cl1 Cl 0.68328(13) 0.17730(8) 0.56361(4) 0.0333(2) Uani 1 1 d . . . . . O1 O 0.2719(3) 0.64493(19) 0.62321(11) 0.0223(6) Uani 1 1 d . . . . . O3 O 0.6164(4) 0.72658(18) 0.59501(11) 0.0232(6) Uani 1 1 d . . . . . O4 O 0.0742(4) 0.7593(2) 0.72481(12) 0.0258(6) Uani 1 1 d . . . . . H4 H 0.086803 0.781471 0.689151 0.039 Uiso 1 1 calc R U . . . O6 O 0.3225(2) 0.11132(12) 0.49215(12) 0.0405(7) Uani 1 1 d D . . . . H22 H 0.309900 0.170500 0.478000 0.061 Uiso 1 1 d D U . . . H23 H 0.433700 0.119800 0.507500 0.061 Uiso 1 1 d D U . . . N1 N 0.3913(4) 0.2546(2) 0.65886(14) 0.0219(7) Uani 1 1 d D . . . . H3 H 0.464(4) 0.238(3) 0.6276(10) 0.026 Uiso 1 1 d D U . . . O2 O 0.5096(5) 0.7260(2) 0.49872(14) 0.0445(8) Uani 1 1 d . . . . . O5 O 0.1199(6) 0.8523(2) 0.62102(15) 0.0529(9) Uani 1 1 d D . . . . H20 H 0.081(8) 0.907(2) 0.605(2) 0.079 Uiso 1 1 d D U . . . H21 H 0.096(9) 0.806(3) 0.5954(16) 0.079 Uiso 1 1 d D U . . . C13 C 0.2360(5) 0.6094(3) 0.68097(15) 0.0195(8) Uani 1 1 d . . . . . C14 C 0.1472(5) 0.6622(3) 0.72837(16) 0.0194(8) Uani 1 1 d . . . . . C6 C 0.5749(5) 0.4150(3) 0.64755(16) 0.0200(8) Uani 1 1 d . . . . . H6 H 0.627545 0.382116 0.609974 0.024 Uiso 1 1 calc R U . . . C5 C 0.5197(5) 0.3297(3) 0.69314(16) 0.0224(7) Uani 1 1 d . . . . . H5 H 0.640649 0.292480 0.704326 0.027 Uiso 1 1 calc R U . . . C11 C 0.3079(5) 0.4626(3) 0.74510(16) 0.0208(7) Uani 1 1 d . . . . . C12 C 0.3033(5) 0.5111(3) 0.68916(16) 0.0185(7) Uani 1 1 d . . . . . C2 C 0.3871(5) 0.4720(3) 0.63077(15) 0.0188(8) Uani 1 1 d . . . . . C15 C 0.1382(5) 0.6105(3) 0.78391(17) 0.0232(8) Uani 1 1 d . . . . . H15 H 0.074230 0.642656 0.817014 0.028 Uiso 1 1 calc R U . . . C3 C 0.2507(6) 0.3977(3) 0.59826(16) 0.0219(8) Uani 1 1 d . . . . . H3A H 0.128034 0.433322 0.589147 0.026 Uiso 1 1 calc R U . . . H3B H 0.309164 0.376543 0.559144 0.026 Uiso 1 1 calc R U . . . C7 C 0.7223(5) 0.4893(3) 0.67150(17) 0.0250(8) Uani 1 1 d . . . . . H7 H 0.805412 0.469418 0.703754 0.030 Uiso 1 1 calc R U . . . C1 C 0.4065(5) 0.5729(3) 0.59450(17) 0.0215(8) Uani 1 1 d . . . . . H1 H 0.365163 0.560572 0.551536 0.026 Uiso 1 1 calc R U . . . C10 C 0.4267(6) 0.3671(3) 0.75210(17) 0.0268(8) Uani 1 1 d . . . . . H10A H 0.343489 0.311865 0.768402 0.032 Uiso 1 1 calc R U . . . H10B H 0.529471 0.380272 0.782344 0.032 Uiso 1 1 calc R U . . . C16 C 0.2181(5) 0.5147(3) 0.79284(16) 0.0236(8) Uani 1 1 d . . . . . H16 H 0.211996 0.483906 0.831938 0.028 Uiso 1 1 calc R U . . . C17 C 0.3498(5) 0.1585(3) 0.69316(19) 0.0303(9) Uani 1 1 d . . . . . H17A H 0.260502 0.173427 0.726538 0.045 Uiso 1 1 calc R U . . . H17B H 0.470218 0.130819 0.709750 0.045 Uiso 1 1 calc R U . . . H17C H 0.291539 0.107976 0.665742 0.045 Uiso 1 1 calc R U . . . C4 C 0.2085(5) 0.3027(3) 0.63611(16) 0.0221(8) Uani 1 1 d . . . . . H4A H 0.126330 0.321808 0.671136 0.027 Uiso 1 1 calc R U . . . H4B H 0.136895 0.252404 0.611097 0.027 Uiso 1 1 calc R U . . . C18 C 0.5608(6) 0.7732(3) 0.54333(18) 0.0306(9) Uani 1 1 d . . . . . C9 C 0.6140(6) 0.6154(3) 0.59461(17) 0.0230(8) Uani 1 1 d . . . . . H13 H 0.678797 0.591733 0.556477 0.028 Uiso 1 1 calc R U . . . C8 C 0.7365(5) 0.5823(3) 0.64774(17) 0.0243(8) Uani 1 1 d . . . . . H8 H 0.826230 0.629386 0.664610 0.029 Uiso 1 1 calc R U . . . C19 C 0.5729(7) 0.8867(3) 0.5484(2) 0.0381(11) Uani 1 1 d . . . . . H19A H 0.536155 0.917864 0.509531 0.057 Uiso 1 1 calc R U . . . H19B H 0.705209 0.906561 0.558607 0.057 Uiso 1 1 calc R U . . . H19C H 0.485189 0.910402 0.580385 0.057 Uiso 1 1 calc R U . . . O7 O 0.0562(5) 0.0457(2) 0.57573(17) 0.0492(9) Uani 1 1 d D . . . . H24 H -0.043(4) 0.077(4) 0.563(2) 0.074 Uiso 1 1 d D U . . . H25 H 0.118(6) 0.065(4) 0.5448(13) 0.074 Uiso 1 1 d D 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 Cl1 0.0335(5) 0.0389(5) 0.0274(4) -0.0009(5) 0.0037(4) 0.0067(5) O1 0.0202(12) 0.0237(13) 0.0229(12) 0.0025(10) 0.0027(10) 0.0033(11) O3 0.0287(14) 0.0206(13) 0.0203(13) 0.0004(11) -0.0002(11) -0.0044(11) O4 0.0245(13) 0.0235(14) 0.0296(14) -0.0021(11) 0.0015(12) 0.0060(12) O6 0.0322(15) 0.0493(19) 0.0401(16) 0.0112(14) -0.0016(14) 0.0039(15) N1 0.0195(15) 0.0200(16) 0.0264(16) 0.0010(14) 0.0042(13) 0.0002(13) O2 0.063(2) 0.0418(19) 0.0290(15) 0.0044(15) -0.0084(15) -0.0180(16) O5 0.086(3) 0.0314(17) 0.0409(18) 0.0030(15) 0.0097(19) 0.0123(19) C13 0.0159(16) 0.0229(18) 0.0197(17) 0.0004(15) -0.0017(14) -0.0010(14) C14 0.0130(15) 0.0218(19) 0.0234(17) -0.0037(16) -0.0027(13) -0.0006(15) C6 0.0149(16) 0.0206(18) 0.0246(18) -0.0034(16) 0.0031(14) 0.0026(15) C5 0.0194(16) 0.0244(18) 0.0235(17) 0.0019(17) 0.0002(14) 0.0006(17) C11 0.0181(17) 0.0238(18) 0.0204(17) -0.0004(15) -0.0002(15) 0.0004(16) C12 0.0128(15) 0.0217(18) 0.0209(17) -0.0040(15) -0.0019(15) 0.0005(16) C2 0.0152(16) 0.0233(19) 0.0178(17) -0.0022(15) -0.0005(14) 0.0014(15) C15 0.0158(16) 0.031(2) 0.0230(18) -0.0066(16) -0.0017(14) 0.0030(16) C3 0.0239(18) 0.0205(17) 0.0212(18) -0.0022(16) -0.0009(15) -0.0013(15) C7 0.0179(17) 0.029(2) 0.0283(19) -0.0017(17) -0.0021(15) 0.0054(17) C1 0.0220(18) 0.0209(18) 0.0217(18) -0.0025(16) -0.0019(15) 0.0010(16) C10 0.0286(19) 0.028(2) 0.0236(19) 0.0034(17) -0.0028(16) 0.0050(18) C16 0.0212(18) 0.030(2) 0.0195(17) -0.0028(16) -0.0017(14) 0.0003(17) C17 0.0223(19) 0.023(2) 0.045(2) 0.0090(19) 0.0025(17) 0.0020(17) C4 0.0184(17) 0.0210(19) 0.0269(18) -0.0008(15) 0.0005(15) 0.0012(16) C18 0.033(2) 0.034(2) 0.025(2) 0.0043(18) 0.0023(18) -0.008(2) C9 0.0256(19) 0.0215(18) 0.0220(19) -0.0028(17) 0.0060(16) 0.0005(16) C8 0.0173(17) 0.027(2) 0.0285(19) -0.0048(17) -0.0004(15) -0.0004(16) C19 0.045(3) 0.031(2) 0.038(2) 0.011(2) -0.004(2) -0.008(2) O7 0.0464(19) 0.0365(18) 0.065(2) 0.0066(17) 0.0255(18) 0.0075(16) _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 O1 C13 1.375(4) . ? O1 C1 1.467(4) . ? O3 C18 1.345(5) . ? O3 C9 1.450(4) . ? O4 C14 1.366(4) . ? O4 H4 0.8400 . ? O6 H22 0.8366 . ? O6 H23 0.8489 . ? N1 C17 1.491(5) . ? N1 C4 1.500(5) . ? N1 C5 1.523(5) . ? N1 H3 0.8800(14) . ? O2 C18 1.211(5) . ? O5 H20 0.8402(14) . ? O5 H21 0.8400(15) . ? C13 C12 1.376(5) . ? C13 C14 1.392(5) . ? C14 C15 1.396(5) . ? C6 C7 1.503(5) . ? C6 C2 1.544(5) . ? C6 C5 1.546(5) . ? C6 H6 1.0000 . ? C5 C10 1.528(5) . ? C5 H5 1.0000 . ? C11 C12 1.384(5) . ? C11 C16 1.397(5) . ? C11 C10 1.500(5) . ? C12 C2 1.498(5) . ? C2 C3 1.532(5) . ? C2 C1 1.543(5) . ? C15 C16 1.380(5) . ? C15 H15 0.9500 . ? C3 C4 1.520(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C7 C8 1.324(5) . ? C7 H7 0.9500 . ? C1 C9 1.542(5) . ? C1 H1 1.0000 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C18 C19 1.486(6) . ? C9 C8 1.508(5) . ? C9 H13 1.0000 . ? C8 H8 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? O7 H24 0.8399(14) . ? O7 H25 0.8399(14) . ? 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 C13 O1 C1 107.3(3) . . ? C18 O3 C9 116.3(3) . . ? C14 O4 H4 109.5 . . ? H22 O6 H23 97.1 . . ? C17 N1 C4 110.9(3) . . ? C17 N1 C5 113.8(3) . . ? C4 N1 C5 113.0(3) . . ? C17 N1 H3 107(3) . . ? C4 N1 H3 109(2) . . ? C5 N1 H3 102(3) . . ? H20 O5 H21 105(5) . . ? O1 C13 C12 111.9(3) . . ? O1 C13 C14 127.2(3) . . ? C12 C13 C14 120.8(3) . . ? O4 C14 C13 125.4(3) . . ? O4 C14 C15 118.8(3) . . ? C13 C14 C15 115.8(3) . . ? C7 C6 C2 110.3(3) . . ? C7 C6 C5 113.9(3) . . ? C2 C6 C5 107.0(3) . . ? C7 C6 H6 108.5 . . ? C2 C6 H6 108.5 . . ? C5 C6 H6 108.5 . . ? N1 C5 C10 112.2(3) . . ? N1 C5 C6 106.6(3) . . ? C10 C5 C6 115.1(3) . . ? N1 C5 H5 107.5 . . ? C10 C5 H5 107.5 . . ? C6 C5 H5 107.5 . . ? C12 C11 C16 115.8(3) . . ? C12 C11 C10 118.9(3) . . ? C16 C11 C10 124.9(3) . . ? C13 C12 C11 123.4(3) . . ? C13 C12 C2 109.6(3) . . ? C11 C12 C2 126.7(3) . . ? C12 C2 C3 112.0(3) . . ? C12 C2 C1 100.8(3) . . ? C3 C2 C1 110.6(3) . . ? C12 C2 C6 106.6(3) . . ? C3 C2 C6 109.1(3) . . ? C1 C2 C6 117.4(3) . . ? C16 C15 C14 122.9(3) . . ? C16 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? C4 C3 C2 112.3(3) . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3B 109.2 . . ? C2 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C8 C7 C6 120.1(3) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? O1 C1 C9 111.3(3) . . ? O1 C1 C2 105.5(3) . . ? C9 C1 C2 112.7(3) . . ? O1 C1 H1 109.1 . . ? C9 C1 H1 109.1 . . ? C2 C1 H1 109.1 . . ? C11 C10 C5 114.2(3) . . ? C11 C10 H10A 108.7 . . ? C5 C10 H10A 108.7 . . ? C11 C10 H10B 108.7 . . ? C5 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C15 C16 C11 120.8(3) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? N1 C17 H17A 109.5 . . ? N1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N1 C4 C3 111.1(3) . . ? N1 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? N1 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? O2 C18 O3 122.6(4) . . ? O2 C18 C19 125.6(4) . . ? O3 C18 C19 111.7(4) . . ? O3 C9 C8 106.0(3) . . ? O3 C9 C1 111.7(3) . . ? C8 C9 C1 115.1(3) . . ? O3 C9 H13 107.9 . . ? C8 C9 H13 107.9 . . ? C1 C9 H13 107.9 . . ? C7 C8 C9 121.7(3) . . ? C7 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? H24 O7 H25 90(5) . . ? _refine_diff_density_max 0.498 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.049 _shelx_res_file ; TITL 180524RAL_MW_HERO_100K_0m_a.res in P2(1)2(1)2(1) 180524RAL_MW_HERO_100K_0m_a.res created by SHELXL-2018/3 at 14:29:38 on 08-Jan-2021 CELL 1.54178 6.9367 13.0374 21.9856 90.000 90.000 90.000 ZERR 4.000 0.0002 0.0003 0.0006 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H Cl N O UNIT 76 112 4 4 28 OMIT 0 3 4 OMIT 0 1 1 L.S. 50 ACTA BOND $H FMAP 2 PLAN 8 SIZE 0.101 0.121 0.209 DFIX 0.84 .001 O7 H24 O7 H25 O5 H20 O5 H21 O6 H22 O6 H23 DFIX 0.88 .001 N1 H3 TEMP -173.140 WGHT 0.052100 0.568200 FVAR 0.79229 CL1 3 0.683283 0.177300 0.563607 11.00000 0.03351 0.03889 = 0.02736 -0.00093 0.00371 0.00669 O1 5 0.271896 0.644932 0.623210 11.00000 0.02017 0.02374 = 0.02289 0.00247 0.00273 0.00330 O3 5 0.616371 0.726583 0.595011 11.00000 0.02871 0.02063 = 0.02030 0.00038 -0.00020 -0.00435 O4 5 0.074215 0.759338 0.724812 11.00000 0.02446 0.02348 = 0.02957 -0.00211 0.00146 0.00596 AFIX 147 H4 2 0.086803 0.781471 0.689151 11.00000 -1.50000 AFIX 0 O6 5 0.322544 0.111315 0.492150 11.00000 0.03223 0.04929 = 0.04005 0.01117 -0.00164 0.00394 AFIX 1 H22 2 0.309900 0.170500 0.478000 11.00000 -1.50000 H23 2 0.433700 0.119800 0.507500 11.00000 -1.50000 AFIX 0 N1 4 0.391266 0.254640 0.658862 11.00000 0.01946 0.01997 = 0.02641 0.00101 0.00417 0.00016 H3 2 0.464167 0.237882 0.627648 11.00000 -1.20000 O2 5 0.509588 0.726031 0.498719 11.00000 0.06266 0.04182 = 0.02898 0.00444 -0.00840 -0.01796 O5 5 0.119891 0.852279 0.621016 11.00000 0.08638 0.03140 = 0.04093 0.00295 0.00971 0.01233 H20 2 0.081427 0.906999 0.604889 11.00000 -1.50000 H21 2 0.096481 0.806128 0.595398 11.00000 -1.50000 C13 1 0.235964 0.609418 0.680972 11.00000 0.01593 0.02287 = 0.01972 0.00037 -0.00167 -0.00096 C14 1 0.147241 0.662215 0.728371 11.00000 0.01304 0.02183 = 0.02344 -0.00365 -0.00273 -0.00058 C6 1 0.574890 0.415035 0.647548 11.00000 0.01492 0.02064 = 0.02456 -0.00343 0.00310 0.00258 AFIX 13 H6 2 0.627545 0.382116 0.609974 11.00000 -1.20000 AFIX 0 C5 1 0.519678 0.329696 0.693144 11.00000 0.01935 0.02438 = 0.02352 0.00194 0.00020 0.00056 AFIX 13 H5 2 0.640649 0.292480 0.704326 11.00000 -1.20000 AFIX 0 C11 1 0.307914 0.462564 0.745104 11.00000 0.01813 0.02377 = 0.02043 -0.00043 -0.00015 0.00041 C12 1 0.303250 0.511085 0.689158 11.00000 0.01282 0.02169 = 0.02090 -0.00397 -0.00188 0.00046 C2 1 0.387141 0.472049 0.630771 11.00000 0.01519 0.02329 = 0.01778 -0.00221 -0.00054 0.00139 C15 1 0.138212 0.610501 0.783908 11.00000 0.01578 0.03079 = 0.02298 -0.00662 -0.00170 0.00296 AFIX 43 H15 2 0.074230 0.642656 0.817014 11.00000 -1.20000 AFIX 0 C3 1 0.250675 0.397658 0.598263 11.00000 0.02394 0.02051 = 0.02116 -0.00220 -0.00086 -0.00132 AFIX 23 H3A 2 0.128034 0.433322 0.589147 11.00000 -1.20000 H3B 2 0.309164 0.376543 0.559144 11.00000 -1.20000 AFIX 0 C7 1 0.722277 0.489275 0.671498 11.00000 0.01788 0.02872 = 0.02834 -0.00165 -0.00208 0.00539 AFIX 43 H7 2 0.805412 0.469418 0.703754 11.00000 -1.20000 AFIX 0 C1 1 0.406489 0.572869 0.594497 11.00000 0.02203 0.02095 = 0.02165 -0.00247 -0.00185 0.00097 AFIX 13 H1 2 0.365163 0.560572 0.551536 11.00000 -1.20000 AFIX 0 C10 1 0.426652 0.367119 0.752105 11.00000 0.02856 0.02841 = 0.02356 0.00337 -0.00284 0.00504 AFIX 23 H10A 2 0.343489 0.311865 0.768402 11.00000 -1.20000 H10B 2 0.529471 0.380272 0.782344 11.00000 -1.20000 AFIX 0 C16 1 0.218121 0.514742 0.792835 11.00000 0.02125 0.03012 = 0.01945 -0.00277 -0.00175 0.00033 AFIX 43 H16 2 0.211996 0.483906 0.831938 11.00000 -1.20000 AFIX 0 C17 1 0.349831 0.158476 0.693162 11.00000 0.02234 0.02332 = 0.04521 0.00899 0.00254 0.00198 AFIX 137 H17A 2 0.260502 0.173427 0.726538 11.00000 -1.50000 H17B 2 0.470218 0.130819 0.709750 11.00000 -1.50000 H17C 2 0.291539 0.107976 0.665742 11.00000 -1.50000 AFIX 0 C4 1 0.208544 0.302743 0.636108 11.00000 0.01838 0.02101 = 0.02693 -0.00081 0.00050 0.00115 AFIX 23 H4A 2 0.126330 0.321808 0.671136 11.00000 -1.20000 H4B 2 0.136895 0.252404 0.611097 11.00000 -1.20000 AFIX 0 C18 1 0.560838 0.773161 0.543329 11.00000 0.03324 0.03376 = 0.02475 0.00432 0.00226 -0.00772 C9 1 0.613951 0.615354 0.594608 11.00000 0.02559 0.02147 = 0.02204 -0.00279 0.00595 0.00054 AFIX 13 H13 2 0.678797 0.591733 0.556477 11.00000 -1.20000 AFIX 0 C8 1 0.736482 0.582268 0.647740 11.00000 0.01734 0.02700 = 0.02850 -0.00480 -0.00038 -0.00035 AFIX 43 H8 2 0.826230 0.629386 0.664610 11.00000 -1.20000 AFIX 0 C19 1 0.572873 0.886663 0.548394 11.00000 0.04511 0.03070 = 0.03850 0.01086 -0.00382 -0.00800 AFIX 137 H19A 2 0.536155 0.917864 0.509531 11.00000 -1.50000 H19B 2 0.705209 0.906561 0.558607 11.00000 -1.50000 H19C 2 0.485189 0.910402 0.580385 11.00000 -1.50000 AFIX 0 O7 5 0.056211 0.045716 0.575730 11.00000 0.04635 0.03652 = 0.06467 0.00659 0.02550 0.00746 H24 2 -0.042515 0.076528 0.563271 11.00000 -1.50000 H25 2 0.117584 0.064916 0.544828 11.00000 -1.50000 HKLF 4 REM 180524RAL_MW_HERO_100K_0m_a.res in P2(1)2(1)2(1) REM wR2 = 0.102581, GooF = S = 1.03722, Restrained GooF = 1.04920 for all data REM R1 = 0.041358 for 3181 Fo > 4sig(Fo) and 0.048907 for all 3594 data REM 271 parameters refined using 7 restraints END WGHT 0.0521 0.5682 REM Highest difference peak 0.498, deepest hole -0.440, 1-sigma level 0.049 Q1 1 0.2720 0.1154 0.4841 11.00000 0.05 0.50 Q2 1 0.1142 0.8046 0.6579 11.00000 0.05 0.24 Q3 1 0.0390 0.0032 0.5890 11.00000 0.05 0.21 Q4 1 0.3242 0.6408 0.5708 11.00000 0.05 0.21 Q5 1 0.7041 0.1470 0.5144 11.00000 0.05 0.19 Q6 1 0.6346 0.1944 0.5212 11.00000 0.05 0.19 Q7 1 0.0510 0.0045 0.5421 11.00000 0.05 0.18 Q8 1 0.0499 0.7803 0.6311 11.00000 0.05 0.18 ; _shelx_res_checksum 47411 _shelx_hkl_file ; -1 0 0 4.20 3.10 -1 0 0 3.70 2.50 1 0 0 3.10 3.90 1 0 0 4.20 4.40 -1 0 0 3.00 4.10 1 0 0 2.50 3.90 -1 0 0 -0.20 3.20 2 0 0 4015.40 205.78 2 0 0 4325.97 208.38 -2 0 0 4350.46 204.48 -2 0 0 3927.51 206.28 -2 0 0 4404.26 203.48 -2 0 0 4129.89 200.88 3 0 0 4.70 8.70 3 0 0 8.90 8.40 -3 0 0 2.90 6.30 3 0 0 5.70 5.60 -3 0 0 2.10 5.80 -4 0 0 305.97 28.00 4 0 0 297.67 24.60 4 0 0 298.07 32.40 -4 0 0 303.87 29.30 4 0 0 263.77 34.50 5 0 0 -4.90 8.40 -5 0 0 -1.80 7.60 5 0 0 0.80 12.30 6 0 0 216.68 32.60 6 0 0 249.58 29.50 6 0 0 218.88 25.40 -6 0 0 229.98 24.80 6 0 0 288.67 33.10 7 0 0 4.60 9.00 7 0 0 -0.80 14.10 -7 0 0 11.10 11.30 7 0 0 4.40 12.70 8 0 0 19.60 15.90 8 0 0 27.20 8.80 8 0 0 7.60 13.50 0 -1 0 2.20 2.00 0 1 0 2.20 2.30 0 -1 0 3.60 1.00 0 -1 0 2.50 2.10 0 1 0 2.10 1.90 0 1 0 4.10 2.20 0 1 0 2.00 1.20 0 -1 0 3.10 1.20 0 1 0 2.60 1.00 -1 -1 0 4220.88 196.18 1 1 0 4217.88 198.68 -1 1 0 4167.38 200.98 -1 -1 0 4192.68 197.58 1 1 0 3799.22 197.48 -1 1 0 4004.80 196.88 1 -1 0 4142.79 200.48 1 -1 0 4093.39 197.98 -1 1 0 4239.18 196.68 1 1 0 4175.48 197.58 -1 1 0 4110.09 196.88 -2 1 0 9539.75 448.66 2 1 0 9755.92 451.95 2 1 0 9454.25 451.75 2 -1 0 9534.55 451.05 -2 -1 0 8952.90 444.26 -2 1 0 9092.09 447.46 -2 -1 0 9787.62 449.95 2 1 0 8406.06 451.25 -2 1 0 9656.53 448.66 2 -1 0 9276.27 454.95 -2 1 0 9999.00 455.15 -2 -1 0 9619.04 447.76 3 -1 0 893.71 57.09 -3 -1 0 883.01 54.69 3 1 0 905.51 49.40 -3 1 0 948.51 53.99 3 1 0 928.21 59.79 3 -1 0 899.21 50.59 -3 1 0 894.41 51.59 -3 -1 0 916.11 52.79 3 -1 0 935.01 62.49 3 1 0 892.41 57.79 -3 1 0 921.31 54.29 -4 -1 0 1617.74 95.29 4 -1 0 1652.93 88.99 -4 1 0 1654.33 94.49 4 -1 0 1656.63 106.29 -4 1 0 1677.53 93.99 4 -1 0 1750.12 100.29 4 1 0 1622.94 102.89 4 1 0 1602.64 98.99 -4 -1 0 1593.04 91.69 4 1 0 1635.94 87.69 -5 1 0 16.60 9.60 5 1 0 6.40 13.70 5 1 0 27.40 11.50 5 -1 0 14.60 14.90 5 -1 0 25.90 11.90 -5 -1 0 12.60 9.40 6 -1 0 763.02 54.99 6 1 0 796.52 54.29 -6 -1 0 800.22 64.79 -6 1 0 737.03 50.29 6 1 0 762.02 57.69 6 -1 0 782.72 58.29 6 -1 0 723.33 55.89 6 -1 0 740.63 49.00 6 1 0 705.03 55.29 7 -1 0 8.80 16.10 7 -1 0 -2.50 9.10 7 1 0 -4.10 9.80 7 1 0 23.80 20.40 -7 1 0 -11.10 9.40 7 -1 0 18.50 14.60 7 1 0 35.60 17.10 7 1 0 20.00 15.80 8 -1 0 -6.50 13.20 8 1 0 -3.10 7.00 8 -1 0 5.30 7.30 8 1 0 18.20 13.80 8 1 0 0.20 13.30 0 2 0 1392.16 68.09 0 2 0 1453.65 68.79 0 -2 0 1440.96 68.09 0 2 0 1398.96 70.89 0 -2 0 1444.36 71.29 0 2 0 1505.65 72.29 0 -2 0 1381.56 71.29 0 2 0 1429.26 71.89 0 -2 0 1423.66 68.69 1 2 0 79.59 9.50 1 2 0 80.89 11.20 -1 -2 0 74.99 7.00 1 -2 0 76.79 10.50 1 2 0 77.79 7.70 -1 2 0 73.79 9.60 -1 -2 0 78.99 9.20 1 -2 0 82.69 12.80 -1 2 0 73.29 7.00 -1 2 0 90.59 8.90 1 2 0 83.59 9.40 -1 2 0 82.69 13.10 2 2 0 3121.09 150.48 2 2 0 2941.01 148.09 2 -2 0 2942.81 154.08 -2 -2 0 2984.60 144.19 -2 2 0 2889.61 144.99 -2 2 0 2941.21 153.48 -2 2 0 2949.80 145.99 2 2 0 2848.22 148.19 -2 2 0 2814.52 146.19 -2 -2 0 2930.71 147.29 2 -2 0 3115.49 148.79 -3 -2 0 4172.58 209.68 3 2 0 4189.28 205.88 -3 2 0 4333.67 212.48 -3 -2 0 4238.38 213.78 -3 2 0 4193.68 211.28 3 -2 0 4191.78 223.18 -3 2 0 4241.58 211.88 3 -2 0 4180.08 208.98 3 -2 0 4578.34 216.88 3 2 0 4430.66 218.08 3 2 0 4242.08 217.68 4 2 0 664.13 52.49 4 -2 0 659.83 42.20 -4 2 0 582.44 44.30 4 2 0 602.84 51.89 4 2 0 673.43 40.10 -4 2 0 668.63 46.70 4 -2 0 648.74 57.29 -4 -2 0 604.74 42.90 4 -2 0 651.83 50.89 -4 -2 0 611.74 47.00 5 2 0 521.95 51.19 5 -2 0 472.85 41.20 5 -2 0 465.65 48.40 5 -2 0 472.55 39.60 5 2 0 418.46 40.60 5 2 0 502.25 37.50 -5 2 0 481.35 36.60 5 2 0 517.65 42.50 6 -2 0 122.59 18.90 6 2 0 120.49 23.00 6 -2 0 120.39 24.90 6 2 0 158.38 24.70 6 2 0 146.99 27.00 -6 2 0 127.79 20.80 7 -2 0 10.90 13.40 -7 2 0 -2.50 9.90 7 2 0 8.90 14.60 7 -2 0 -1.90 7.90 7 2 0 1.90 9.70 7 2 0 -0.60 13.80 8 2 0 7.00 12.40 8 2 0 6.30 13.30 8 -2 0 -5.40 12.90 8 2 0 6.30 7.50 0 3 0 2.50 3.10 0 3 0 4.50 5.70 0 3 0 1.20 4.70 0 3 0 2.20 6.10 0 -3 0 2.10 5.20 -1 3 0 560.44 37.30 1 -3 0 531.25 36.10 1 3 0 546.65 31.90 -1 3 0 540.65 33.50 1 3 0 517.15 29.90 1 3 0 508.45 34.20 1 3 0 523.35 31.80 -1 3 0 540.05 30.60 1 -3 0 520.65 33.30 -1 -3 0 530.85 30.50 -1 -3 0 545.55 27.80 -1 3 0 532.15 27.70 -2 -3 0 93.89 13.10 2 3 0 71.69 12.20 -2 3 0 92.59 14.00 -2 3 0 92.89 12.80 2 3 0 88.29 13.30 -2 3 0 85.79 10.20 2 -3 0 86.89 13.80 -2 -3 0 80.09 9.50 2 -3 0 96.79 18.90 2 3 0 101.29 15.60 -2 3 0 103.59 19.50 -3 3 0 1079.29 61.19 -3 -3 0 1058.09 64.29 3 -3 0 1102.09 74.89 3 3 0 1102.79 67.59 -3 -3 0 1059.99 59.69 3 -3 0 1073.39 60.19 -3 3 0 1112.79 63.89 3 3 0 1039.00 55.89 3 3 0 1141.19 69.39 3 -3 0 1055.59 66.29 -3 3 0 1109.69 64.59 4 -3 0 3391.46 174.68 -4 3 0 3235.58 169.08 4 3 0 3170.88 159.78 4 3 0 3191.38 176.48 4 -3 0 2886.11 178.28 -4 -3 0 3189.28 170.78 4 3 0 3313.07 177.48 -5 3 0 190.68 23.40 5 -3 0 205.38 29.30 5 -3 0 172.88 33.10 5 3 0 191.48 34.70 5 -3 0 221.68 22.50 5 3 0 209.18 29.00 5 3 0 252.87 30.90 5 3 0 204.48 23.40 6 3 0 31.60 14.50 6 -3 0 47.10 17.60 6 3 0 90.19 23.30 6 3 0 51.09 18.60 6 -3 0 52.29 12.90 -6 3 0 46.80 14.70 7 3 0 13.90 11.40 -7 3 0 24.80 12.50 7 3 0 42.60 17.80 7 -3 0 34.70 10.90 7 3 0 24.10 16.20 7 -3 0 23.40 15.70 8 3 0 19.80 8.90 8 3 0 25.10 13.90 8 3 0 6.40 13.10 0 -4 0 1788.62 95.79 0 4 0 1769.92 96.79 0 4 0 2058.79 98.69 0 4 0 1773.02 90.19 0 4 0 1880.31 95.39 -1 4 0 3109.09 147.59 1 4 0 2976.50 150.08 -1 -4 0 2948.10 143.59 1 4 0 2819.22 147.69 1 -4 0 3098.59 151.88 1 -4 0 3034.00 155.08 -1 -4 0 3095.19 147.49 -1 -4 0 3016.20 151.28 1 4 0 2854.21 149.99 -1 4 0 3111.49 156.78 -1 4 0 3173.68 151.98 -1 -4 0 2962.60 144.59 2 4 0 1524.55 82.99 -2 4 0 1519.05 92.29 2 -4 0 1564.44 84.89 -2 4 0 1528.95 84.49 -2 4 0 1548.25 81.39 2 4 0 1585.24 87.19 -2 -4 0 1553.34 82.09 -2 -4 0 1423.16 76.29 3 4 0 1188.48 64.29 3 4 0 1267.77 76.29 3 -4 0 1228.18 76.29 3 4 0 1331.77 80.99 -3 -4 0 1278.17 74.29 -3 4 0 1297.27 73.19 -3 4 0 1295.07 75.49 4 4 0 5.90 12.10 4 4 0 6.10 12.10 -4 4 0 -4.50 8.90 -4 -4 0 -2.10 8.50 4 4 0 8.70 7.00 -4 4 0 1.50 10.10 4 -4 0 0.20 10.20 5 4 0 231.08 32.10 5 4 0 278.87 47.50 5 -4 0 218.68 38.50 -5 4 0 292.27 27.20 5 4 0 299.77 27.00 5 -4 0 254.07 23.80 5 4 0 262.77 33.80 5 -4 0 288.57 32.30 6 -4 0 12.50 9.70 6 4 0 24.30 17.50 -6 4 0 34.50 13.50 6 4 0 16.40 13.70 6 -4 0 23.60 15.20 6 4 0 16.60 15.60 7 4 0 162.38 26.90 7 4 0 146.29 26.30 -7 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10.90 0 3 25 -2.40 15.30 -1 3 25 38.40 18.90 1 -3 25 35.50 12.90 -1 3 -25 43.20 11.20 1 3 25 51.09 13.60 -1 -3 25 14.50 12.40 2 -3 25 11.40 11.10 -2 3 -25 10.50 7.70 -2 -3 25 17.40 10.60 2 3 25 7.80 8.30 0 -4 25 9.00 11.80 0 4 25 17.30 10.90 1 -4 25 203.48 22.60 -1 -4 25 153.68 20.10 -1 4 -25 184.48 20.00 1 4 25 181.28 21.00 0 0 26 131.39 18.90 -1 0 -26 50.29 11.60 1 0 26 48.80 13.70 0 -1 26 -2.40 11.40 1 -1 26 124.09 17.30 -1 -1 -26 139.29 16.80 -1 -1 26 140.09 20.90 -1 1 -26 134.39 16.10 0 -2 26 40.10 13.30 1 -2 26 31.90 12.40 1 2 26 23.90 14.70 -1 -2 26 33.40 14.10 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 76593