#============================================================================== data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 9 _journal_issue 3 _journal_year 2018 _journal_page_first 178 _journal_page_last 181 #=============================================================================== # SUBMISSION DETAILS _publ_requested_journal 'Eur.J.Chem.' # Name of author for correspondence _publ_contact_author_name 'Dr. Leslaw Sieron' _publ_contact_author_email 'leslaw.sieron@p.lodz.pl' _publ_contact_author_address ; Institute of General and Ecological Chemistry Lodz University of Technology Zeromskiego 116, 90-924 Lodz Poland ; #=============================================================================== # AUTHOR LIST loop_ _publ_author_name 'L.Sieron' 'A.Czylkowska' 'B.Rogalewicz' #=============================================================================== data_gd #=============================================================================== _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ; catena-(tris(\m~2~-Dibromoacetato-O,O')-(4,4'-bipyridine-N)-aqua-gadolinium(iii)) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H13 Br6 Gd N2 O7' _chemical_formula_sum 'C16 H13 Br6 Gd N2 O7' _chemical_formula_weight 981.99 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' 'Br' 'Br' -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Gd' 'Gd' -8.8380 11.9157 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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, -y, -z' _cell_length_a 9.7368(4) _cell_length_b 11.5416(4) _cell_length_c 11.7634(4) _cell_angle_alpha 104.2750(10) _cell_angle_beta 94.060(2) _cell_angle_gamma 92.6900(10) _cell_volume 1275.08(8) _cell_formula_units_Z 2 _cell_measurement_temperature 90 _cell_measurement_reflns_used 8706 _cell_measurement_theta_min 3.89 _cell_measurement_theta_max 72.36 _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.558 _exptl_crystal_F_000 906 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_absorpt_coefficient_mu 28.190 _shelx_estimated_absorpt_T_min 0.165 _shelx_estimated_absorpt_T_max 0.211 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.15 _exptl_absorpt_correction_T_max 0.23 _exptl_absorpt_process_details SADABS _exptl_absorpt_special_details ? _diffrn_ambient_temperature 90 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_probe 'x-ray' _diffrn_radiation_type 'CuK\a' _diffrn_radiation_source '30W microsource with MonoCap capillary' _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_reflns_number 8399 _diffrn_reflns_av_unetI/netI 0.0639 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.891 _diffrn_reflns_theta_max 66.590 _diffrn_reflns_theta_full 66.590 _diffrn_measured_fraction_theta_max 0.888 _diffrn_measured_fraction_theta_full 0.888 _diffrn_reflns_Laue_measured_fraction_max 0.888 _diffrn_reflns_Laue_measured_fraction_full 0.888 _diffrn_reflns_point_group_measured_fraction_max 0.888 _diffrn_reflns_point_group_measured_fraction_full 0.888 _reflns_number_total 4006 _reflns_number_gt 3834 _reflns_threshold_expression 'I > 2\s(I)' _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_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _refine_special_details ? _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^)+(0.0605P)^2^+12.6846P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary difmap _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_extinction_coef 0.00057(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4006 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1396 _refine_ls_wR_factor_gt 0.1386 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 2.091 _refine_diff_density_min -2.675 _refine_diff_density_rms 0.215 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 Gd1 Gd 0.22787(5) 0.47800(5) 0.47932(4) 0.01327(19) Uani 1 1 d . . . . . N1 N 0.2811(8) 0.3069(7) 0.2938(7) 0.0195(18) Uani 1 1 d . . . . . N2 N 0.3188(11) -0.1873(9) -0.1978(8) 0.036(2) Uani 1 1 d . . . . . O1 O 0.4186(7) 0.3756(6) 0.5265(5) 0.0190(10) Uani 1 1 d . . . . . O2 O 0.6227(6) 0.4298(6) 0.6295(5) 0.0178(14) Uani 1 1 d . . . . . O3 O 0.1566(7) 0.4789(6) 0.6697(6) 0.0190(10) Uani 1 1 d . . . . . O4 O -0.0667(7) 0.5197(7) 0.6783(7) 0.0292(17) Uani 1 1 d . . . . . O5 O 0.1270(8) 0.6581(7) 0.5276(8) 0.0315(18) Uani 1 1 d . . . . . O6 O -0.0937(7) 0.7017(7) 0.5299(6) 0.0259(16) Uani 1 1 d . . . . . O7 O 0.3811(6) 0.6114(6) 0.6317(6) 0.0200(15) Uani 1 1 d . . . . . H71 H 0.451102 0.620136 0.595993 0.030 Uiso 1 1 d R U . . . H72 H 0.351872 0.671225 0.677535 0.030 Uiso 1 1 d R U . . . Br1 Br 0.38223(14) 0.16385(12) 0.63989(11) 0.0394(3) Uani 1 1 d . . . . . Br2 Br 0.56873(13) 0.34248(13) 0.84718(10) 0.0380(3) Uani 1 1 d . . . . . Br3 Br -0.00779(19) 0.27451(13) 0.78789(12) 0.0552(5) Uani 1 1 d . . . . . Br4 Br 0.20463(11) 0.48350(11) 0.93198(9) 0.0278(3) Uani 1 1 d . . . . . Br5 Br 0.04767(11) 0.95830(10) 0.68360(10) 0.0293(3) Uani 1 1 d . . . . . Br6 Br 0.24979(12) 0.88250(11) 0.47859(10) 0.0348(3) Uani 1 1 d . . . . . C1 C 0.5034(9) 0.3832(8) 0.6142(7) 0.0131(13) Uani 1 1 d . . . . . C2 C 0.4448(11) 0.3305(10) 0.7088(8) 0.027(2) Uani 1 1 d . . . . . H2 H 0.362073 0.374851 0.734585 0.033 Uiso 1 1 calc R U . . . C3 C 0.0471(9) 0.4872(8) 0.7142(7) 0.0131(13) Uani 1 1 d . . . . . C4 C 0.0347(11) 0.4451(10) 0.8302(9) 0.029(2) Uani 1 1 d . . . . . H4 H -0.042040 0.485566 0.872970 0.034 Uiso 1 1 calc R U . . . C5 C 0.0332(10) 0.7238(9) 0.5301(8) 0.022(2) Uani 1 1 d . . . . . C6 C 0.0674(10) 0.8585(9) 0.5281(9) 0.023(2) Uani 1 1 d . . . . . H6 H -0.001834 0.880263 0.471246 0.027 Uiso 1 1 calc R U . . . C7 C 0.2854(10) 0.1939(8) 0.3054(8) 0.019(2) Uani 1 1 d . . . . . H7 H 0.285019 0.180452 0.381916 0.023 Uiso 1 1 calc R U . . . C8 C 0.2904(11) 0.0954(9) 0.2089(9) 0.024(2) Uani 1 1 d . . . . . H8 H 0.294394 0.016830 0.220051 0.029 Uiso 1 1 calc R U . . . C9 C 0.2362(15) -0.1027(11) -0.0099(11) 0.043(3) Uani 1 1 d . . . . . H9 H 0.185608 -0.114666 0.052915 0.051 Uiso 1 1 calc R U . . . C10 C 0.2521(16) -0.1966(11) -0.1062(11) 0.043(3) Uani 1 1 d . . . . . H10 H 0.212015 -0.273298 -0.106476 0.052 Uiso 1 1 calc R U . . . C11 C 0.3721(11) -0.0776(11) -0.1947(10) 0.032(3) Uani 1 1 d . . . . . H11 H 0.418609 -0.067557 -0.260358 0.038 Uiso 1 1 calc R U . . . C12 C 0.3644(11) 0.0212(10) -0.1038(8) 0.026(2) Uani 1 1 d . . . . . H12 H 0.405427 0.096552 -0.106918 0.031 Uiso 1 1 calc R U . . . C13 C 0.2967(12) 0.0106(9) -0.0076(9) 0.026(2) Uani 1 1 d . . . . . C14 C 0.2895(10) 0.1139(9) 0.0983(9) 0.022(2) Uani 1 1 d . . . . . C15 C 0.2870(11) 0.2288(10) 0.0853(10) 0.028(2) Uani 1 1 d . . . . . H15 H 0.289264 0.244071 0.009634 0.034 Uiso 1 1 calc R U . . . C16 C 0.2811(10) 0.3226(9) 0.1850(8) 0.021(2) Uani 1 1 d . . . . . H16 H 0.276969 0.401706 0.175188 0.025 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 Gd1 0.0173(3) 0.0142(3) 0.0080(3) 0.0008(2) 0.0042(2) 0.0035(2) N1 0.031(4) 0.020(4) 0.006(4) 0.000(3) 0.000(3) 0.005(3) N2 0.064(7) 0.025(5) 0.017(5) 0.000(4) 0.006(4) 0.013(5) O1 0.027(2) 0.022(3) 0.008(2) 0.003(2) 0.0072(19) 0.007(2) O2 0.020(3) 0.022(4) 0.009(3) 0.000(3) -0.002(2) -0.002(3) O3 0.027(2) 0.022(3) 0.008(2) 0.003(2) 0.0072(19) 0.007(2) O4 0.020(3) 0.039(5) 0.030(4) 0.012(4) -0.001(3) 0.002(3) O5 0.035(4) 0.021(4) 0.044(5) 0.012(4) 0.019(4) 0.018(3) O6 0.023(4) 0.027(4) 0.027(4) 0.006(3) 0.003(3) -0.004(3) O7 0.020(3) 0.024(4) 0.014(3) -0.001(3) 0.005(3) 0.000(3) Br1 0.0548(8) 0.0354(7) 0.0287(6) 0.0155(6) -0.0043(5) -0.0191(6) Br2 0.0435(7) 0.0547(8) 0.0166(5) 0.0166(6) -0.0085(5) -0.0143(6) Br3 0.0967(12) 0.0385(8) 0.0285(7) 0.0146(6) -0.0077(7) -0.0293(8) Br4 0.0333(6) 0.0382(7) 0.0117(5) 0.0071(5) -0.0010(4) 0.0013(5) Br5 0.0332(6) 0.0204(6) 0.0291(6) -0.0043(5) 0.0031(4) 0.0032(4) Br6 0.0370(6) 0.0385(7) 0.0264(6) 0.0056(5) 0.0057(5) -0.0148(5) C1 0.024(3) 0.010(3) 0.005(3) -0.002(3) 0.003(2) 0.004(2) C2 0.030(5) 0.038(6) 0.009(4) 0.001(5) -0.008(4) -0.005(5) C3 0.024(3) 0.010(3) 0.005(3) -0.002(3) 0.003(2) 0.004(2) C4 0.036(6) 0.034(6) 0.014(5) 0.003(5) 0.004(4) -0.004(5) C5 0.025(5) 0.023(5) 0.011(4) -0.008(4) 0.002(4) -0.008(4) C6 0.028(5) 0.024(6) 0.020(5) 0.012(5) 0.007(4) -0.002(4) C7 0.032(5) 0.014(5) 0.010(4) -0.001(4) 0.007(4) 0.007(4) C8 0.039(6) 0.015(5) 0.021(5) 0.006(4) 0.012(4) 0.008(4) C9 0.076(9) 0.027(7) 0.022(6) -0.003(5) 0.021(6) 0.000(6) C10 0.079(10) 0.024(6) 0.030(7) 0.009(6) 0.015(7) 0.000(6) C11 0.035(6) 0.041(7) 0.020(6) 0.007(5) 0.002(5) 0.016(5) C12 0.031(5) 0.027(6) 0.011(5) -0.009(4) 0.005(4) 0.000(4) C13 0.045(6) 0.020(6) 0.011(5) -0.002(4) 0.006(4) 0.009(5) C14 0.032(5) 0.015(5) 0.015(5) -0.006(4) 0.006(4) 0.004(4) C15 0.038(6) 0.033(6) 0.015(5) 0.006(5) 0.008(4) 0.006(5) C16 0.033(5) 0.014(5) 0.012(5) -0.003(4) 0.003(4) 0.003(4) _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 Gd1 O5 2.301(7) . ? Gd1 O4 2.349(7) 2_566 ? Gd1 O1 2.353(7) . ? Gd1 O6 2.374(7) 2_566 ? Gd1 O2 2.383(7) 2_666 ? Gd1 O3 2.389(6) . ? Gd1 O7 2.420(6) . ? Gd1 N1 2.657(7) . ? N1 C16 1.336(13) . ? N1 C7 1.348(13) . ? N2 C10 1.320(15) . ? N2 C11 1.337(16) . ? O1 C1 1.258(11) . ? O2 C1 1.239(11) . ? O3 C3 1.218(11) . ? O4 C3 1.264(11) . ? O5 C5 1.212(13) . ? O6 C5 1.250(12) . ? O7 H71 0.8400 . ? O7 H72 0.8400 . ? Br1 C2 1.944(11) . ? Br2 C2 1.929(10) . ? Br3 C4 1.925(12) . ? Br4 C4 1.938(11) . ? Br5 C6 1.934(10) . ? Br6 C6 1.936(10) . ? C1 C2 1.524(14) . ? C2 H2 1.0000 . ? C3 C4 1.568(14) . ? C4 H4 1.0000 . ? C5 C6 1.580(15) . ? C6 H6 1.0000 . ? C7 C8 1.400(13) . ? C7 H7 0.9500 . ? C8 C14 1.369(15) . ? C8 H8 0.9500 . ? C9 C10 1.385(16) . ? C9 C13 1.402(17) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.367(14) . ? C11 H11 0.9500 . ? C12 C13 1.377(15) . ? C12 H12 0.9500 . ? C13 C14 1.504(12) . ? C14 C15 1.374(16) . ? C15 C16 1.393(14) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? 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 O5 Gd1 O4 73.0(3) . 2_566 ? O5 Gd1 O1 143.6(3) . . ? O4 Gd1 O1 141.1(2) 2_566 . ? O5 Gd1 O6 119.2(3) . 2_566 ? O4 Gd1 O6 80.6(3) 2_566 2_566 ? O1 Gd1 O6 86.0(2) . 2_566 ? O5 Gd1 O2 86.6(3) . 2_666 ? O4 Gd1 O2 82.4(2) 2_566 2_666 ? O1 Gd1 O2 86.8(2) . 2_666 ? O6 Gd1 O2 142.6(2) 2_566 2_666 ? O5 Gd1 O3 78.7(3) . . ? O4 Gd1 O3 121.3(2) 2_566 . ? O1 Gd1 O3 87.1(2) . . ? O6 Gd1 O3 70.2(2) 2_566 . ? O2 Gd1 O3 145.8(2) 2_666 . ? O5 Gd1 O7 73.2(3) . . ? O4 Gd1 O7 141.1(3) 2_566 . ? O1 Gd1 O7 70.4(2) . . ? O6 Gd1 O7 133.6(2) 2_566 . ? O2 Gd1 O7 77.0(2) 2_666 . ? O3 Gd1 O7 69.3(2) . . ? O5 Gd1 N1 141.3(3) . . ? O4 Gd1 N1 71.6(3) 2_566 . ? O1 Gd1 N1 69.5(2) . . ? O6 Gd1 N1 69.4(3) 2_566 . ? O2 Gd1 N1 73.7(2) 2_666 . ? O3 Gd1 N1 134.2(3) . . ? O7 Gd1 N1 130.9(2) . . ? C16 N1 C7 117.3(8) . . ? C16 N1 Gd1 123.4(6) . . ? C7 N1 Gd1 118.4(6) . . ? C10 N2 C11 115.7(10) . . ? C1 O1 Gd1 136.9(5) . . ? C1 O2 Gd1 136.6(6) . 2_666 ? C3 O3 Gd1 135.0(6) . . ? C3 O4 Gd1 148.9(6) . 2_566 ? C5 O5 Gd1 155.2(7) . . ? C5 O6 Gd1 132.2(7) . 2_566 ? Gd1 O7 H71 102.4 . . ? Gd1 O7 H72 121.0 . . ? H71 O7 H72 119.5 . . ? O2 C1 O1 126.6(9) . . ? O2 C1 C2 120.1(8) . . ? O1 C1 C2 113.2(8) . . ? C1 C2 Br2 115.2(7) . . ? C1 C2 Br1 109.1(6) . . ? Br2 C2 Br1 109.8(6) . . ? C1 C2 H2 107.5 . . ? Br2 C2 H2 107.5 . . ? Br1 C2 H2 107.5 . . ? O3 C3 O4 130.0(9) . . ? O3 C3 C4 118.5(8) . . ? O4 C3 C4 111.4(8) . . ? C3 C4 Br3 108.3(6) . . ? C3 C4 Br4 111.3(7) . . ? Br3 C4 Br4 109.8(6) . . ? C3 C4 H4 109.2 . . ? Br3 C4 H4 109.2 . . ? Br4 C4 H4 109.2 . . ? O5 C5 O6 129.9(10) . . ? O5 C5 C6 118.8(9) . . ? O6 C5 C6 111.3(9) . . ? C5 C6 Br5 108.0(7) . . ? C5 C6 Br6 111.9(7) . . ? Br5 C6 Br6 111.6(5) . . ? C5 C6 H6 108.4 . . ? Br5 C6 H6 108.4 . . ? Br6 C6 H6 108.4 . . ? N1 C7 C8 122.4(9) . . ? N1 C7 H7 118.8 . . ? C8 C7 H7 118.8 . . ? C14 C8 C7 119.1(10) . . ? C14 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C10 C9 C13 118.1(11) . . ? C10 C9 H9 120.9 . . ? C13 C9 H9 120.9 . . ? N2 C10 C9 124.8(12) . . ? N2 C10 H10 117.6 . . ? C9 C10 H10 117.6 . . ? N2 C11 C12 124.6(11) . . ? N2 C11 H11 117.7 . . ? C12 C11 H11 117.7 . . ? C11 C12 C13 119.5(11) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C12 C13 C9 117.2(9) . . ? C12 C13 C14 122.6(10) . . ? C9 C13 C14 120.2(10) . . ? C8 C14 C15 119.1(9) . . ? C8 C14 C13 120.8(10) . . ? C15 C14 C13 120.1(10) . . ? C14 C15 C16 118.8(10) . . ? C14 C15 H15 120.6 . . ? C16 C15 H15 120.6 . . ? N1 C16 C15 123.3(10) . . ? N1 C16 H16 118.4 . . ? C15 C16 H16 118.4 . . ? _shelx_res_file ; TITL gd in P-1 gd.res created by SHELXL-2018/3 at 22:34:55 on 18-May-2018 CELL 1.54178 9.7368 11.5416 11.7634 104.275 94.060 92.690 ZERR 2.000 0.0004 0.0004 0.0004 0.001 0.002 0.001 LATT 1 SFAC C H N O Br Gd UNIT 32 26 4 14 12 2 L.S. 75 SHEL 100 0.84 ACTA BOND $H FMAP 2 PLAN 20 SIZE 0.08 0.1 0.1 EADP O1 O3 EADP C1 C3 TEMP -183 WGHT 0.060500 12.684600 EXTI 0.000573 FVAR 0.29807 GD1 6 0.227872 0.478004 0.479319 11.00000 0.01731 0.01419 = 0.00799 0.00083 0.00424 0.00346 N1 3 0.281080 0.306944 0.293845 11.00000 0.03061 0.02036 = 0.00597 0.00013 0.00038 0.00510 N2 3 0.318850 -0.187337 -0.197790 11.00000 0.06411 0.02460 = 0.01664 0.00023 0.00650 0.01308 O1 4 0.418592 0.375556 0.526483 11.00000 0.02741 0.02234 = 0.00836 0.00326 0.00724 0.00729 O2 4 0.622746 0.429792 0.629529 11.00000 0.01966 0.02206 = 0.00875 -0.00036 -0.00212 -0.00207 O3 4 0.156573 0.478858 0.669658 11.00000 0.02741 0.02234 = 0.00836 0.00326 0.00724 0.00729 O4 4 -0.066697 0.519697 0.678282 11.00000 0.01993 0.03876 = 0.03048 0.01220 -0.00099 0.00229 O5 4 0.127008 0.658085 0.527626 11.00000 0.03469 0.02142 = 0.04444 0.01225 0.01881 0.01780 O6 4 -0.093694 0.701690 0.529881 11.00000 0.02334 0.02671 = 0.02698 0.00646 0.00317 -0.00441 O7 4 0.381148 0.611381 0.631700 11.00000 0.01978 0.02382 = 0.01356 -0.00114 0.00479 0.00010 AFIX 3 H71 2 0.451102 0.620136 0.595993 11.00000 -1.50000 H72 2 0.351872 0.671225 0.677535 11.00000 -1.50000 AFIX 0 BR1 5 0.382232 0.163852 0.639886 11.00000 0.05478 0.03539 = 0.02874 0.01553 -0.00428 -0.01907 BR2 5 0.568727 0.342475 0.847179 11.00000 0.04345 0.05465 = 0.01663 0.01664 -0.00852 -0.01433 BR3 5 -0.007793 0.274514 0.787895 11.00000 0.09671 0.03850 = 0.02846 0.01455 -0.00775 -0.02934 BR4 5 0.204629 0.483500 0.931979 11.00000 0.03329 0.03817 = 0.01172 0.00708 -0.00099 0.00129 BR5 5 0.047668 0.958304 0.683597 11.00000 0.03317 0.02038 = 0.02910 -0.00427 0.00306 0.00325 BR6 5 0.249792 0.882497 0.478595 11.00000 0.03701 0.03847 = 0.02644 0.00564 0.00570 -0.01479 C1 1 0.503438 0.383157 0.614243 11.00000 0.02366 0.00966 = 0.00478 -0.00153 0.00282 0.00392 C2 1 0.444825 0.330510 0.708780 11.00000 0.02986 0.03795 = 0.00876 0.00070 -0.00773 -0.00479 AFIX 13 H2 2 0.362073 0.374851 0.734585 11.00000 -1.20000 AFIX 0 C3 1 0.047088 0.487199 0.714195 11.00000 0.02366 0.00966 = 0.00478 -0.00153 0.00282 0.00392 C4 1 0.034698 0.445059 0.830200 11.00000 0.03572 0.03412 = 0.01371 0.00282 0.00411 -0.00402 AFIX 13 H4 2 -0.042040 0.485566 0.872970 11.00000 -1.20000 AFIX 0 C5 1 0.033247 0.723846 0.530091 11.00000 0.02494 0.02348 = 0.01084 -0.00779 0.00243 -0.00781 C6 1 0.067400 0.858504 0.528121 11.00000 0.02788 0.02428 = 0.02017 0.01177 0.00654 -0.00156 AFIX 13 H6 2 -0.001834 0.880263 0.471246 11.00000 -1.20000 AFIX 0 C7 1 0.285393 0.193853 0.305430 11.00000 0.03164 0.01418 = 0.01004 -0.00069 0.00695 0.00684 AFIX 43 H7 2 0.285019 0.180452 0.381916 11.00000 -1.20000 AFIX 0 C8 1 0.290402 0.095421 0.208929 11.00000 0.03881 0.01516 = 0.02074 0.00643 0.01228 0.00805 AFIX 43 H8 2 0.294394 0.016830 0.220051 11.00000 -1.20000 AFIX 0 C9 1 0.236165 -0.102657 -0.009866 11.00000 0.07647 0.02710 = 0.02197 -0.00286 0.02089 0.00036 AFIX 43 H9 2 0.185608 -0.114666 0.052915 11.00000 -1.20000 AFIX 0 C10 1 0.252090 -0.196580 -0.106243 11.00000 0.07870 0.02368 = 0.02985 0.00878 0.01524 -0.00050 AFIX 43 H10 2 0.212015 -0.273298 -0.106476 11.00000 -1.20000 AFIX 0 C11 1 0.372146 -0.077568 -0.194732 11.00000 0.03528 0.04112 = 0.02016 0.00667 0.00226 0.01613 AFIX 43 H11 2 0.418609 -0.067557 -0.260358 11.00000 -1.20000 AFIX 0 C12 1 0.364425 0.021195 -0.103785 11.00000 0.03145 0.02718 = 0.01104 -0.00916 0.00536 0.00012 AFIX 43 H12 2 0.405427 0.096552 -0.106918 11.00000 -1.20000 AFIX 0 C13 1 0.296748 0.010634 -0.007559 11.00000 0.04503 0.02003 = 0.01089 -0.00183 0.00620 0.00876 C14 1 0.289472 0.113869 0.098268 11.00000 0.03171 0.01490 = 0.01529 -0.00627 0.00624 0.00447 C15 1 0.287008 0.228817 0.085258 11.00000 0.03784 0.03323 = 0.01498 0.00568 0.00757 0.00642 AFIX 43 H15 2 0.289264 0.244071 0.009634 11.00000 -1.20000 AFIX 0 C16 1 0.281138 0.322646 0.185020 11.00000 0.03307 0.01438 = 0.01164 -0.00344 0.00260 0.00343 AFIX 43 H16 2 0.276969 0.401706 0.175188 11.00000 -1.20000 AFIX 0 HKLF 4 REM gd in P-1 REM wR2 = 0.1396, GooF = S = 1.096, Restrained GooF = 1.096 for all data REM R1 = 0.0527 for 3834 Fo > 4sig(Fo) and 0.0539 for all 4006 data REM 278 parameters refined using 0 restraints END WGHT 0.0605 12.6757 REM Highest difference peak 2.091, deepest hole -2.675, 1-sigma level 0.215 Q1 1 0.2499 0.4057 0.4504 11.00000 0.05 2.09 Q2 1 0.5996 0.2762 0.8237 11.00000 0.05 1.55 Q3 1 0.1854 0.4827 0.5751 11.00000 0.05 1.31 Q4 1 0.0698 0.2753 0.7896 11.00000 0.05 1.24 Q5 1 0.3713 0.0991 0.6389 11.00000 0.05 1.02 Q6 1 0.2087 0.4633 0.4149 11.00000 0.05 0.98 Q7 1 -0.0324 0.2224 0.7897 11.00000 0.05 0.95 Q8 1 0.2715 0.4704 0.9043 11.00000 0.05 0.93 Q9 1 0.1880 0.5865 0.5294 11.00000 0.05 0.91 Q10 1 0.0942 0.9213 0.6456 11.00000 0.05 0.89 Q11 1 0.2507 0.8083 0.4602 11.00000 0.05 0.83 Q12 1 0.0047 1.0430 0.6996 11.00000 0.05 0.80 Q13 1 0.1228 0.4261 0.4412 11.00000 0.05 0.79 Q14 1 0.4489 0.6443 0.6427 11.00000 0.05 0.71 Q15 1 0.2680 0.8823 0.3931 11.00000 0.05 0.71 Q16 1 -0.0058 0.9570 0.7874 11.00000 0.05 0.70 Q17 1 0.0955 0.4912 0.6384 11.00000 0.05 0.68 Q18 1 0.4462 0.3823 0.4960 11.00000 0.05 0.67 Q19 1 0.2045 0.9509 0.5932 11.00000 0.05 0.66 Q20 1 0.1323 -0.0782 -0.0584 11.00000 0.05 0.66 ; _shelx_res_checksum 25422 _shelx_hkl_file ; -1 0 0 164.00 14.29 -1 0 0 156.64 12.73 -2 0 0 579.69 44.11 2 0 0 555.57 42.89 2 0 0 571.25 46.73 -3 0 0 774.04 60.01 3 0 0 820.11 64.33 3 0 0 717.28 58.03 -4 0 0 1647.50 126.64 4 0 0 1653.39 131.66 -5 0 0 2030.89 143.84 -5 0 0 1798.74 145.67 -5 0 0 1908.93 145.35 5 0 0 1921.72 143.52 5 0 0 1800.86 151.40 -6 0 0 1119.64 93.98 -6 0 0 1172.76 92.20 -6 0 0 1209.96 94.92 6 0 0 1193.49 91.90 6 0 0 1254.95 101.94 -7 0 0 241.15 23.86 -7 0 0 258.40 22.30 7 0 0 185.43 34.61 7 0 0 230.75 21.31 -8 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