# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Yang, Xiu-Li' 'Xie, Ming-Hua' 'Zou, Chao' 'Wu, Chuan-De' _publ_contact_author_name 'Wu, Chuan-De' _publ_contact_author_email cdwu@zju.edu.cn _publ_section_title ; Syntheses, crystal structures and optical properties of six homochiral coordination networks based on phenyl acid-amino acids ; # Attachment '- New.cif' data_New1 _database_code_depnum_ccdc_archive 'CCDC 821192' #TrackingRef '- New.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H36 N2 O10 Zn' _chemical_formula_weight 601.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 21.960(5) _cell_length_b 5.8873(13) _cell_length_c 10.731(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.46(2) _cell_angle_gamma 90.00 _cell_volume 1354.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2916 _cell_measurement_theta_min 3.80 _cell_measurement_theta_max 25.68 _exptl_crystal_description bloc _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.966 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.870 _exptl_absorpt_correction_T_max 0.953 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2916 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.1080 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.80 _diffrn_reflns_theta_max 25.68 _reflns_number_total 1866 _reflns_number_gt 1264 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.045(19) _refine_ls_number_reflns 1866 _refine_ls_number_parameters 177 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.0710 _refine_ls_wR_factor_gt 0.0666 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.923 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 0.21293(15) 1.0000 0.0367(3) Uani 1 2 d S . . O1 O 0.35291(15) 1.4915(6) 0.7217(3) 0.0416(10) Uani 1 1 d . . . O2 O 0.27360(17) 1.3725(7) 0.5770(4) 0.0521(11) Uani 1 1 d . . . H2B H 0.2385 1.3091 0.5530 0.062 Uiso 1 1 d . . . O3 O 0.07884(15) 0.3315(6) 0.9681(4) 0.0446(11) Uani 1 1 d . . . O4 O 0.01424(16) 0.5746(6) 0.8547(4) 0.0516(12) Uani 1 1 d . . . O5 O -0.03431(14) -0.0052(7) 0.8630(4) 0.0609(13) Uani 1 1 d . . . H5A H -0.0713 -0.0142 0.8180 0.073 Uiso 1 1 d . . . H5B H -0.0108 -0.1153 0.8529 0.073 Uiso 1 1 d . . . N1 N 0.30185(18) 0.9325(7) 0.6666(4) 0.0297(11) Uani 1 1 d . . . H1D H 0.3226 0.8038 0.6682 0.036 Uiso 1 1 d . . . C1 C 0.4274(2) 1.2351(18) 0.5312(6) 0.082(2) Uani 1 1 d . . . H1A H 0.4424 1.2170 0.4541 0.124 Uiso 1 1 calc R . . H1B H 0.4609 1.2098 0.6036 0.124 Uiso 1 1 calc R . . H1C H 0.4115 1.3864 0.5348 0.124 Uiso 1 1 calc R . . C2 C 0.3757(3) 1.0650(11) 0.5329(6) 0.0572(18) Uani 1 1 d . . . H2A H 0.3414 1.1002 0.4605 0.069 Uiso 1 1 calc R . . C3 C 0.3966(4) 0.8269(12) 0.5148(7) 0.105(3) Uani 1 1 d . . . H3A H 0.4098 0.8166 0.4354 0.157 Uiso 1 1 calc R . . H3B H 0.3626 0.7238 0.5138 0.157 Uiso 1 1 calc R . . H3C H 0.4307 0.7880 0.5837 0.157 Uiso 1 1 calc R . . C4 C 0.3515(3) 1.1048(11) 0.6562(6) 0.0340(15) Uani 1 1 d . . . H4A H 0.3862 1.0924 0.7307 0.041 Uiso 1 1 calc R . . C5 C 0.3232(3) 1.3464(13) 0.6505(6) 0.0378(15) Uani 1 1 d . . . C6 C 0.2832(2) 0.9707(10) 0.7899(5) 0.0436(16) Uani 1 1 d . . . H6A H 0.2749 1.1313 0.7978 0.052 Uiso 1 1 calc R . . H6B H 0.3179 0.9306 0.8587 0.052 Uiso 1 1 calc R . . C7 C 0.2263(3) 0.8379(12) 0.8065(5) 0.0369(16) Uani 1 1 d . . . C8 C 0.1685(3) 0.9355(9) 0.7774(5) 0.0428(16) Uani 1 1 d . . . H8A H 0.1637 1.0777 0.7388 0.051 Uiso 1 1 calc R . . C9 C 0.1174(3) 0.8271(12) 0.8041(6) 0.0437(18) Uani 1 1 d . . . H9A H 0.0787 0.8979 0.7839 0.052 Uiso 1 1 calc R . . C10 C 0.1226(3) 0.6117(11) 0.8614(5) 0.0313(15) Uani 1 1 d . . . C11 C 0.1806(2) 0.5149(9) 0.8878(5) 0.0318(13) Uani 1 1 d . . . H11A H 0.1855 0.3721 0.9257 0.038 Uiso 1 1 calc R . . C12 C 0.2323(3) 0.6227(10) 0.8599(5) 0.0361(16) Uani 1 1 d . . . H12A H 0.2709 0.5506 0.8771 0.043 Uiso 1 1 calc R . . C13 C 0.0674(2) 0.4999(10) 0.8951(5) 0.0358(14) Uani 1 1 d . . . 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 Zn1 0.0265(5) 0.0366(6) 0.0464(7) 0.000 0.0067(5) 0.000 O1 0.037(2) 0.029(3) 0.054(3) -0.009(2) -0.001(2) 0.002(2) O2 0.036(2) 0.048(3) 0.058(3) 0.000(2) -0.022(2) -0.0006(18) O3 0.039(2) 0.035(3) 0.063(3) 0.012(2) 0.020(2) -0.0039(18) O4 0.034(2) 0.048(3) 0.072(3) -0.002(2) 0.011(2) 0.0093(19) O5 0.032(2) 0.058(3) 0.079(3) -0.034(2) -0.019(2) 0.019(2) N1 0.033(2) 0.021(3) 0.035(3) -0.001(2) 0.007(2) -0.006(2) C1 0.064(4) 0.100(6) 0.094(5) -0.003(6) 0.043(4) -0.016(5) C2 0.052(4) 0.058(5) 0.068(5) -0.008(4) 0.029(4) -0.006(3) C3 0.155(7) 0.060(6) 0.125(7) -0.025(5) 0.090(7) -0.016(5) C4 0.033(3) 0.037(4) 0.030(3) -0.004(3) 0.002(3) -0.005(3) C5 0.037(3) 0.035(4) 0.038(4) 0.008(3) 0.001(3) -0.006(3) C6 0.064(4) 0.036(4) 0.035(4) -0.008(3) 0.020(3) -0.016(3) C7 0.038(4) 0.038(4) 0.036(4) -0.004(3) 0.009(3) -0.010(3) C8 0.063(4) 0.028(4) 0.039(4) 0.010(3) 0.015(3) -0.001(3) C9 0.036(3) 0.046(4) 0.050(5) 0.000(4) 0.011(3) 0.010(3) C10 0.042(4) 0.027(4) 0.028(4) -0.005(3) 0.015(3) -0.004(3) C11 0.040(3) 0.028(3) 0.030(3) 0.001(3) 0.012(3) 0.003(3) C12 0.032(3) 0.040(4) 0.037(4) -0.006(3) 0.009(3) -0.005(3) C13 0.041(3) 0.036(4) 0.034(4) -0.009(3) 0.016(3) -0.008(3) _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 Zn1 O3 1.964(3) . ? Zn1 O3 1.964(3) 2_557 ? Zn1 O5 1.975(4) . ? Zn1 O5 1.975(4) 2_557 ? O1 C5 1.235(7) . ? O2 C5 1.208(6) . ? O3 C13 1.255(6) . ? O4 C13 1.235(6) . ? N1 C6 1.484(6) . ? N1 C4 1.511(6) . ? C1 C2 1.517(9) . ? C2 C3 1.501(8) . ? C2 C4 1.547(7) . ? C4 C5 1.549(7) . ? C6 C7 1.516(7) . ? C7 C8 1.366(7) . ? C7 C12 1.385(7) . ? C8 C9 1.374(7) . ? C9 C10 1.403(7) . ? C10 C11 1.368(7) . ? C10 C13 1.491(7) . ? C11 C12 1.389(6) . ? 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 O3 Zn1 O3 138.4(2) . 2_557 ? O3 Zn1 O5 108.09(16) . . ? O3 Zn1 O5 98.73(15) 2_557 . ? O3 Zn1 O5 98.73(15) . 2_557 ? O3 Zn1 O5 108.09(16) 2_557 2_557 ? O5 Zn1 O5 98.9(2) . 2_557 ? C13 O3 Zn1 108.9(3) . . ? C6 N1 C4 107.9(4) . . ? C3 C2 C1 111.4(6) . . ? C3 C2 C4 115.0(6) . . ? C1 C2 C4 107.8(5) . . ? N1 C4 C2 110.3(5) . . ? N1 C4 C5 109.2(5) . . ? C2 C4 C5 108.3(5) . . ? O2 C5 O1 126.7(7) . . ? O2 C5 C4 116.2(6) . . ? O1 C5 C4 117.1(5) . . ? N1 C6 C7 114.8(4) . . ? C8 C7 C12 118.8(6) . . ? C8 C7 C6 120.3(6) . . ? C12 C7 C6 120.8(6) . . ? C7 C8 C9 121.1(6) . . ? C8 C9 C10 121.3(6) . . ? C11 C10 C9 116.8(6) . . ? C11 C10 C13 122.4(6) . . ? C9 C10 C13 120.8(6) . . ? C10 C11 C12 122.2(6) . . ? C7 C12 C11 119.8(6) . . ? O4 C13 O3 123.2(5) . . ? O4 C13 C10 120.9(6) . . ? O3 C13 C10 115.9(5) . . ? 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 O5 H5A O1 0.85 1.76 2.610(5) 175.1 3_435 O5 H5B O4 0.85 1.91 2.702(5) 155.7 1_545 N1 H1D O1 0.88 2.00 2.839(5) 159.2 1_545 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.294 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.063 #===END data_New2 _database_code_depnum_ccdc_archive 'CCDC 821193' #TrackingRef '- New.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H36 Cu2 N2 O11' _chemical_formula_weight 679.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 21.574(3) _cell_length_b 5.9897(3) _cell_length_c 14.1692(18) _cell_angle_alpha 90.00 _cell_angle_beta 127.501(19) _cell_angle_gamma 90.00 _cell_volume 1452.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3288 _cell_measurement_theta_min 3.60 _cell_measurement_theta_max 25.05 _exptl_crystal_description bloc _exptl_crystal_colour blue _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 1.525 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.713 _exptl_absorpt_correction_T_max 0.899 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3288 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0494 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 25.05 _reflns_number_total 2078 _reflns_number_gt 1805 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.006(17) _refine_ls_number_reflns 2078 _refine_ls_number_parameters 186 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0667 _refine_ls_wR_factor_gt 0.0651 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.10014(3) -0.42684(7) -0.20945(4) 0.02462(14) Uani 1 1 d . . . O1 O -0.12412(17) -0.0694(5) -0.0670(3) 0.0306(7) Uani 1 1 d . . . O2 O -0.18207(16) -0.3540(4) -0.1937(3) 0.0329(8) Uani 1 1 d . . . O3 O -0.59829(17) 0.3689(4) -0.2626(3) 0.0302(7) Uani 1 1 d . . . O4 O -0.56302(17) 0.5592(6) -0.3568(2) 0.0389(7) Uani 1 1 d . . . O5 O -0.1061(2) -0.7383(5) -0.1776(4) 0.0567(12) Uani 1 1 d . . . H5B H -0.1275 -0.8343 -0.1570 0.068 Uiso 1 1 d . . . H5A H -0.0879 -0.7996 -0.1867 0.068 Uiso 1 1 d . . . O6 O 0.0000 -0.3153(6) 0.0000 0.0282(10) Uani 1 2 d S . . H6B H 0.0351 -0.2369 0.0052 0.042 Uiso 1 1 d . . . N1 N -0.53296(19) -0.0037(5) -0.2601(3) 0.0209(8) Uani 1 1 d . . . H11B H -0.5470 -0.1405 -0.2954 0.025 Uiso 1 1 calc R . . C1 C -0.1819(2) -0.1902(6) -0.1386(4) 0.0231(9) Uani 1 1 d . . . C2 C -0.2570(2) -0.1355(6) -0.1576(3) 0.0222(9) Uani 1 1 d . . . C3 C -0.3183(3) -0.2862(7) -0.2117(4) 0.0360(12) Uani 1 1 d . . . H3A H -0.3165 -0.4158 -0.2460 0.043 Uiso 1 1 calc R . . C4 C -0.3826(3) -0.2427(7) -0.2145(5) 0.0405(12) Uani 1 1 d . . . H4A H -0.4230 -0.3461 -0.2492 0.049 Uiso 1 1 calc R . . C5 C -0.3876(3) -0.0508(7) -0.1670(4) 0.0294(11) Uani 1 1 d . . . C6 C -0.3283(2) 0.1027(9) -0.1188(4) 0.0326(11) Uani 1 1 d . . . H6A H -0.3320 0.2372 -0.0897 0.039 Uiso 1 1 calc R . . C7 C -0.2632(2) 0.0595(10) -0.1131(3) 0.0291(9) Uani 1 1 d . . . H7A H -0.2230 0.1639 -0.0787 0.035 Uiso 1 1 calc R . . C8 C -0.4506(2) -0.0118(7) -0.1510(4) 0.0346(12) Uani 1 1 d . . . H8A H -0.4464 -0.1295 -0.1003 0.041 Uiso 1 1 calc R . . H8B H -0.4391 0.1280 -0.1087 0.041 Uiso 1 1 calc R . . C9 C -0.5707(2) 0.3844(7) -0.3208(4) 0.0261(10) Uani 1 1 d . . . C10 C -0.5475(2) 0.1658(6) -0.3473(4) 0.0224(9) Uani 1 1 d . . . H10A H -0.4987 0.1906 -0.3366 0.027 Uiso 1 1 calc R . . C11 C -0.6100(3) 0.0839(11) -0.4759(3) 0.0419(10) Uani 1 1 d . . . H11A H -0.5900 -0.0542 -0.4856 0.050 Uiso 1 1 calc R . . C12 C -0.6212(5) 0.2471(11) -0.5654(6) 0.111(3) Uani 1 1 d . . . H12A H -0.5716 0.2801 -0.5477 0.166 Uiso 1 1 calc R . . H12B H -0.6438 0.3821 -0.5621 0.166 Uiso 1 1 calc R . . H12C H -0.6554 0.1837 -0.6436 0.166 Uiso 1 1 calc R . . C13 C -0.6873(3) 0.0267(12) -0.5011(5) 0.085(2) Uani 1 1 d . . . H13A H -0.6786 -0.0791 -0.4433 0.127 Uiso 1 1 calc R . . H13B H -0.7219 -0.0368 -0.5793 0.127 Uiso 1 1 calc R . . H13C H -0.7102 0.1597 -0.4968 0.127 Uiso 1 1 calc R . . 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 Cu1 0.0273(2) 0.0202(2) 0.0393(3) 0.0000(3) 0.0269(2) 0.0024(3) O1 0.0255(18) 0.0354(17) 0.0383(19) -0.0022(15) 0.0232(16) -0.0011(14) O2 0.0286(17) 0.034(2) 0.050(2) -0.0059(13) 0.0314(17) 0.0013(11) O3 0.0468(19) 0.0202(15) 0.042(2) 0.0011(13) 0.0368(17) 0.0068(13) O4 0.067(2) 0.0159(14) 0.0513(18) 0.0010(19) 0.0447(17) -0.001(2) O5 0.107(3) 0.0174(16) 0.109(3) 0.0016(17) 0.099(3) 0.0026(16) O6 0.020(2) 0.037(2) 0.034(3) 0.000 0.019(2) 0.000 N1 0.0178(18) 0.0197(17) 0.025(2) -0.0016(13) 0.0130(16) 0.0020(12) C1 0.025(2) 0.025(2) 0.031(3) 0.008(2) 0.023(2) 0.0068(19) C2 0.023(2) 0.026(2) 0.025(2) 0.0076(18) 0.019(2) 0.0094(18) C3 0.030(3) 0.037(3) 0.049(3) -0.014(2) 0.029(3) -0.002(2) C4 0.031(3) 0.040(3) 0.057(4) -0.011(2) 0.031(3) -0.005(2) C5 0.021(2) 0.044(3) 0.024(3) 0.002(2) 0.014(2) 0.0097(19) C6 0.031(2) 0.039(3) 0.029(2) -0.005(2) 0.019(2) 0.012(2) C7 0.025(2) 0.032(2) 0.031(2) -0.002(3) 0.0175(18) -0.001(3) C8 0.021(2) 0.059(3) 0.027(3) 0.005(2) 0.016(2) 0.0146(19) C9 0.022(2) 0.027(2) 0.023(3) -0.0043(19) 0.010(2) -0.0026(19) C10 0.023(2) 0.0208(19) 0.031(3) 0.0006(18) 0.020(2) 0.0006(16) C11 0.060(3) 0.031(2) 0.028(2) 0.000(3) 0.023(2) 0.006(3) C12 0.188(9) 0.072(5) 0.051(5) -0.002(3) 0.061(6) -0.013(5) C13 0.045(4) 0.097(6) 0.053(4) -0.020(4) 0.000(3) -0.001(3) _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 Cu1 O3 1.935(3) 3_545 ? Cu1 O5 1.942(3) . ? Cu1 O2 1.961(3) . ? Cu1 N1 2.024(3) 3_545 ? Cu1 O6 2.4728(13) . ? O1 C1 1.252(5) . ? O2 C1 1.252(5) . ? O3 C9 1.280(5) . ? O3 Cu1 1.935(3) 3_455 ? O4 C9 1.219(6) . ? N1 C10 1.477(5) . ? N1 C8 1.485(5) . ? N1 Cu1 2.024(3) 3_455 ? C1 C2 1.508(5) . ? C2 C7 1.371(7) . ? C2 C3 1.385(6) . ? C3 C4 1.387(6) . ? C4 C5 1.369(6) . ? C5 C6 1.373(6) . ? C5 C8 1.526(6) . ? C6 C7 1.381(5) . ? C9 C10 1.528(6) . ? C10 C11 1.546(6) . ? C11 C12 1.499(8) . ? C11 C13 1.516(7) . ? 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 O3 Cu1 O5 171.86(15) 3_545 . ? O3 Cu1 O2 94.27(11) 3_545 . ? O5 Cu1 O2 89.76(13) . . ? O3 Cu1 N1 83.17(12) 3_545 3_545 ? O5 Cu1 N1 91.52(12) . 3_545 ? O2 Cu1 N1 168.81(14) . 3_545 ? O3 Cu1 O6 90.57(12) 3_545 . ? O5 Cu1 O6 96.54(15) . . ? O2 Cu1 O6 89.59(10) . . ? N1 Cu1 O6 101.31(10) 3_545 . ? C1 O2 Cu1 125.8(3) . . ? C9 O3 Cu1 116.4(3) . 3_455 ? C10 N1 C8 113.8(3) . . ? C10 N1 Cu1 107.9(2) . 3_455 ? C8 N1 Cu1 107.4(2) . 3_455 ? O1 C1 O2 125.5(4) . . ? O1 C1 C2 116.8(4) . . ? O2 C1 C2 117.7(4) . . ? C7 C2 C3 118.8(4) . . ? C7 C2 C1 119.8(3) . . ? C3 C2 C1 121.2(4) . . ? C2 C3 C4 119.7(4) . . ? C5 C4 C3 121.4(4) . . ? C4 C5 C6 118.6(4) . . ? C4 C5 C8 123.1(4) . . ? C6 C5 C8 117.9(4) . . ? C5 C6 C7 120.7(5) . . ? C2 C7 C6 120.8(5) . . ? N1 C8 C5 117.3(4) . . ? O4 C9 O3 124.5(4) . . ? O4 C9 C10 119.0(4) . . ? O3 C9 C10 116.5(4) . . ? N1 C10 C9 108.5(3) . . ? N1 C10 C11 110.9(3) . . ? C9 C10 C11 112.4(4) . . ? C12 C11 C13 111.1(5) . . ? C12 C11 C10 111.5(5) . . ? C13 C11 C10 113.2(4) . . ? 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 O5 H5B O1 0.89 1.87 2.699(4) 153.7 1_545 O5 H5A O3 0.61 2.20 2.695(4) 139.8 3_535 O6 H6B O1 0.86 1.85 2.673(3) 161.7 2 N1 H11B O4 0.91 1.94 2.841(5) 172.8 1_545 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.318 _refine_diff_density_min -0.233 _refine_diff_density_rms 0.060 #===END data_New3 _database_code_depnum_ccdc_archive 'CCDC 821194' #TrackingRef '- New.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H30 N2 O8 Zn2' _chemical_formula_weight 629.26 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' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_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 6.65340(10) _cell_length_b 18.9600(3) _cell_length_c 22.5591(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2845.80(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10549 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 67.06 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 2.490 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.861 _exptl_absorpt_correction_T_max 0.905 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10549 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 67.06 _reflns_number_total 4568 _reflns_number_gt 3956 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+0.0361P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.19(4) _refine_ls_number_reflns 4568 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0833 _refine_ls_wR_factor_gt 0.0791 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.79778(7) 0.48997(2) 0.138155(16) 0.05259(13) Uani 1 1 d . . . Zn2 Zn 0.29258(7) 0.50780(3) 0.092286(16) 0.05752(14) Uani 1 1 d . . . O1 O 0.9241(6) 0.58481(19) 0.15018(16) 0.0892(9) Uani 1 1 d . . . O2 O 1.2176(7) 0.60724(17) 0.10831(13) 0.0865(10) Uani 1 1 d . . . O3 O 0.9520(4) 0.94600(15) 0.40105(11) 0.0620(6) Uani 1 1 d . . . O4 O 0.7470(6) 0.8557(2) 0.40207(18) 0.0987(11) Uani 1 1 d . . . O5 O 0.6300(5) 0.5174(2) 0.21031(11) 0.0828(9) Uani 1 1 d . . . O6 O 0.3207(5) 0.4919(2) 0.18391(11) 0.0940(11) Uani 1 1 d . . . O7 O -0.0947(4) 0.49270(16) 0.57465(9) 0.0606(6) Uani 1 1 d . . . O8 O -0.3245(5) 0.4667(2) 0.50732(13) 0.0864(10) Uani 1 1 d . . . N1 N 1.1872(6) 0.88444(17) 0.32295(14) 0.0676(8) Uani 1 1 d . . . H11B H 1.3141 0.8676 0.3177 0.081 Uiso 1 1 calc R . . N2 N 0.2020(5) 0.48679(17) 0.49692(11) 0.0607(7) Uani 1 1 d . . . H22A H 0.3088 0.4602 0.4854 0.073 Uiso 1 1 calc R . . C1 C 1.0700(8) 0.6232(2) 0.13986(18) 0.0704(11) Uani 1 1 d . . . C2 C 1.0720(7) 0.6934(2) 0.17009(18) 0.0680(10) Uani 1 1 d . . . C3 C 0.9047(8) 0.7177(3) 0.1993(2) 0.0776(12) Uani 1 1 d . . . H3A H 0.7880 0.6907 0.1993 0.093 Uiso 1 1 calc R . . C4 C 0.9069(8) 0.7812(3) 0.2286(2) 0.0806(12) Uani 1 1 d . . . H4A H 0.7917 0.7968 0.2479 0.097 Uiso 1 1 calc R . . C5 C 1.0777(8) 0.8217(2) 0.22969(18) 0.0733(11) Uani 1 1 d . . . C6 C 1.2458(8) 0.7977(3) 0.2003(2) 0.0829(14) Uani 1 1 d . . . H6A H 1.3626 0.8246 0.2005 0.100 Uiso 1 1 calc R . . C7 C 1.2429(7) 0.7342(3) 0.17070(19) 0.0794(13) Uani 1 1 d . . . H7A H 1.3574 0.7188 0.1510 0.095 Uiso 1 1 calc R . . C8 C 1.0853(9) 0.8899(2) 0.26412(18) 0.0750(11) Uani 1 1 d . . . H8A H 1.1548 0.9250 0.2405 0.090 Uiso 1 1 calc R . . H8B H 0.9489 0.9065 0.2703 0.090 Uiso 1 1 calc R . . C9 C 0.9089(8) 0.8812(2) 0.39106(17) 0.0667(11) Uani 1 1 d . . . C10 C 1.0777(8) 0.8379(2) 0.36378(19) 0.0721(10) Uani 1 1 d . . . H10A H 1.0180 0.7993 0.3408 0.087 Uiso 1 1 calc R . . C11 C 1.2212(11) 0.8059(3) 0.4098(2) 0.0984(16) Uani 1 1 d . . . H11A H 1.3059 0.8441 0.4252 0.118 Uiso 1 1 calc R . . C12 C 1.1153(17) 0.7753(6) 0.4593(5) 0.179(5) Uani 1 1 d . . . H12A H 1.2104 0.7572 0.4874 0.268 Uiso 1 1 calc R . . H12B H 1.0311 0.7376 0.4455 0.268 Uiso 1 1 calc R . . H12C H 1.0337 0.8107 0.4779 0.268 Uiso 1 1 calc R . . C13 C 1.3582(12) 0.7518(4) 0.3807(4) 0.122(2) Uani 1 1 d . . . H13A H 1.4504 0.7336 0.4097 0.183 Uiso 1 1 calc R . . H13B H 1.4320 0.7738 0.3492 0.183 Uiso 1 1 calc R . . H13C H 1.2786 0.7140 0.3650 0.183 Uiso 1 1 calc R . . C14 C 0.4471(6) 0.5111(2) 0.22064(14) 0.0607(9) Uani 1 1 d . . . C15 C 0.3818(7) 0.5262(2) 0.28334(15) 0.0626(10) Uani 1 1 d . . . C16 C 0.1881(7) 0.5422(2) 0.29740(16) 0.0682(10) Uani 1 1 d . . . H16A H 0.0920 0.5452 0.2676 0.082 Uiso 1 1 calc R . . C17 C 0.1324(7) 0.5542(2) 0.35606(17) 0.0679(10) Uani 1 1 d . . . H17A H 0.0003 0.5662 0.3648 0.082 Uiso 1 1 calc R . . C18 C 0.2712(7) 0.5484(2) 0.40144(14) 0.0641(10) Uani 1 1 d . . . C19 C 0.4667(7) 0.5334(3) 0.38637(18) 0.0837(15) Uani 1 1 d . . . H19A H 0.5634 0.5303 0.4160 0.100 Uiso 1 1 calc R . . C20 C 0.5221(7) 0.5228(3) 0.32815(17) 0.0824(15) Uani 1 1 d . . . H20A H 0.6558 0.5134 0.3190 0.099 Uiso 1 1 calc R . . C21 C 0.2182(8) 0.5558(2) 0.46625(14) 0.0654(9) Uani 1 1 d . . . H21A H 0.3203 0.5840 0.4857 0.078 Uiso 1 1 calc R . . H21B H 0.0913 0.5806 0.4697 0.078 Uiso 1 1 calc R . . C22 C -0.1510(6) 0.4705(2) 0.52260(16) 0.0613(10) Uani 1 1 d . . . C23 C 0.0194(6) 0.4479(2) 0.48115(15) 0.0602(9) Uani 1 1 d . . . H23A H -0.0182 0.4615 0.4407 0.072 Uiso 1 1 calc R . . C24 C 0.2028(13) 0.3472(3) 0.4334(3) 0.119(2) Uani 1 1 d . . . H24A H 0.2256 0.2973 0.4345 0.179 Uiso 1 1 calc R . . H24B H 0.3274 0.3715 0.4399 0.179 Uiso 1 1 calc R . . H24C H 0.1493 0.3602 0.3954 0.179 Uiso 1 1 calc R . . C25 C 0.0534(10) 0.3675(3) 0.4818(2) 0.0830(13) Uani 1 1 d . . . H25A H 0.1121 0.3548 0.5201 0.100 Uiso 1 1 calc R . . C26 C -0.1406(14) 0.3265(4) 0.4744(4) 0.132(3) Uani 1 1 d . . . H26A H -0.1124 0.2769 0.4755 0.197 Uiso 1 1 calc R . . H26B H -0.2011 0.3383 0.4371 0.197 Uiso 1 1 calc R . . H26C H -0.2312 0.3384 0.5060 0.197 Uiso 1 1 calc R . . 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 Zn1 0.0522(2) 0.0661(3) 0.03948(19) 0.00164(17) 0.00015(18) 0.0016(3) Zn2 0.0550(2) 0.0794(3) 0.03820(19) -0.00573(19) 0.00439(18) -0.0035(3) O1 0.079(2) 0.081(2) 0.107(2) -0.0301(17) 0.0071(19) -0.0095(19) O2 0.109(3) 0.0772(18) 0.0734(17) -0.0202(13) 0.034(2) -0.004(2) O3 0.0691(16) 0.0627(17) 0.0543(13) -0.0026(11) 0.0031(12) 0.0026(13) O4 0.087(3) 0.098(2) 0.111(3) -0.0165(19) 0.025(2) -0.019(2) O5 0.0737(18) 0.131(3) 0.0442(12) -0.0059(15) 0.0038(12) 0.0148(19) O6 0.086(2) 0.157(3) 0.0392(11) 0.0005(16) 0.0012(13) -0.033(3) O7 0.0573(13) 0.0841(17) 0.0405(10) -0.0035(11) -0.0009(10) 0.0001(15) O8 0.0616(18) 0.136(3) 0.0622(16) -0.0132(16) -0.0112(14) 0.0012(19) N1 0.076(2) 0.0676(19) 0.0593(16) -0.0085(13) 0.0057(18) 0.0040(19) N2 0.0633(16) 0.0780(18) 0.0407(11) 0.0005(12) 0.0006(13) 0.003(2) C1 0.080(3) 0.075(3) 0.056(2) -0.0106(18) 0.002(2) -0.005(2) C2 0.074(3) 0.073(3) 0.057(2) -0.0093(18) 0.008(2) 0.000(2) C3 0.068(3) 0.086(3) 0.079(3) -0.018(2) 0.001(2) -0.007(2) C4 0.074(3) 0.088(3) 0.080(3) -0.021(2) 0.010(2) 0.006(3) C5 0.088(3) 0.079(3) 0.052(2) -0.0082(17) 0.006(2) 0.002(3) C6 0.091(4) 0.085(3) 0.073(2) -0.020(2) 0.014(2) -0.013(3) C7 0.075(3) 0.090(3) 0.073(2) -0.020(2) 0.018(2) -0.002(2) C8 0.094(3) 0.072(3) 0.059(2) -0.0145(18) -0.003(2) 0.004(3) C9 0.074(3) 0.071(3) 0.055(2) 0.0012(17) 0.006(2) -0.001(2) C10 0.090(3) 0.064(2) 0.062(2) -0.0026(18) 0.000(2) 0.001(2) C11 0.124(5) 0.089(3) 0.082(3) 0.004(2) -0.007(3) 0.018(4) C12 0.170(9) 0.212(10) 0.154(7) 0.092(7) 0.029(7) 0.058(8) C13 0.122(5) 0.102(4) 0.142(5) 0.000(4) -0.016(4) 0.031(4) C14 0.066(2) 0.072(2) 0.0440(16) 0.0024(16) 0.0014(16) -0.005(2) C15 0.067(2) 0.079(3) 0.0421(16) 0.0056(16) 0.0019(16) 0.000(2) C16 0.070(3) 0.091(3) 0.0446(16) 0.0061(16) -0.0055(18) -0.002(2) C17 0.067(2) 0.089(3) 0.0483(18) 0.0051(18) 0.0042(17) 0.007(2) C18 0.072(3) 0.077(2) 0.0438(16) 0.0023(15) 0.0041(17) -0.003(2) C19 0.069(3) 0.136(5) 0.0471(19) 0.003(2) -0.0091(19) 0.002(3) C20 0.067(2) 0.133(5) 0.0476(19) 0.000(2) 0.0022(17) 0.008(3) C21 0.077(3) 0.076(2) 0.0435(16) 0.0024(14) 0.0034(19) -0.002(2) C22 0.065(2) 0.076(3) 0.0440(16) 0.0001(15) -0.0041(15) 0.0016(18) C23 0.067(2) 0.072(3) 0.0411(16) 0.0005(16) -0.0080(16) 0.0004(19) C24 0.136(5) 0.100(4) 0.122(4) -0.031(3) 0.015(5) 0.018(5) C25 0.108(4) 0.079(3) 0.062(2) -0.007(2) -0.011(2) 0.008(3) C26 0.150(7) 0.090(4) 0.155(6) -0.024(4) 0.004(5) -0.032(5) _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 Zn1 O7 1.996(2) 2_564 ? Zn1 O1 2.003(3) . ? Zn1 O5 2.041(3) . ? Zn1 O3 2.061(3) 3_745 ? Zn1 N1 2.187(3) 3_745 ? Zn2 O2 1.984(3) 1_455 ? Zn2 O3 2.011(3) 3_645 ? Zn2 O7 2.049(3) 2_564 ? Zn2 O6 2.097(3) . ? Zn2 N2 2.154(3) 2_564 ? O1 C1 1.236(6) . ? O2 C1 1.250(6) . ? O2 Zn2 1.984(3) 1_655 ? O3 C9 1.282(5) . ? O3 Zn2 2.011(3) 3_655 ? O3 Zn1 2.061(3) 3_755 ? O4 C9 1.206(6) . ? O5 C14 1.245(5) . ? O6 C14 1.235(5) . ? O7 C22 1.302(4) . ? O7 Zn1 1.996(2) 2_565 ? O7 Zn2 2.049(3) 2_565 ? O8 C22 1.207(5) . ? N1 C10 1.469(6) . ? N1 C8 1.494(6) . ? N1 Zn1 2.187(3) 3_755 ? N2 C23 1.465(5) . ? N2 C21 1.483(5) . ? N2 Zn2 2.154(3) 2_565 ? C1 C2 1.495(6) . ? C2 C3 1.373(7) . ? C2 C7 1.375(7) . ? C3 C4 1.373(7) . ? C4 C5 1.373(7) . ? C5 C6 1.378(7) . ? C5 C8 1.508(6) . ? C6 C7 1.376(7) . ? C9 C10 1.522(7) . ? C10 C11 1.535(8) . ? C11 C12 1.442(11) . ? C11 C13 1.521(9) . ? C14 C15 1.507(5) . ? C15 C16 1.362(6) . ? C15 C20 1.378(6) . ? C16 C17 1.393(6) . ? C17 C18 1.383(6) . ? C18 C19 1.374(7) . ? C18 C21 1.510(5) . ? C19 C20 1.379(6) . ? C22 C23 1.530(6) . ? C23 C25 1.542(7) . ? C24 C25 1.525(9) . ? C25 C26 1.515(10) . ? 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 O7 Zn1 O1 103.50(15) 2_564 . ? O7 Zn1 O5 99.23(11) 2_564 . ? O1 Zn1 O5 83.85(15) . . ? O7 Zn1 O3 107.77(10) 2_564 3_745 ? O1 Zn1 O3 94.72(13) . 3_745 ? O5 Zn1 O3 152.49(11) . 3_745 ? O7 Zn1 N1 117.99(14) 2_564 3_745 ? O1 Zn1 N1 138.39(16) . 3_745 ? O5 Zn1 N1 86.44(14) . 3_745 ? O3 Zn1 N1 76.42(12) 3_745 3_745 ? O2 Zn2 O3 109.67(15) 1_455 3_645 ? O2 Zn2 O7 106.65(15) 1_455 2_564 ? O3 Zn2 O7 143.68(12) 3_645 2_564 ? O2 Zn2 O6 88.80(16) 1_455 . ? O3 Zn2 O6 85.12(12) 3_645 . ? O7 Zn2 O6 95.92(11) 2_564 . ? O2 Zn2 N2 98.11(13) 1_455 2_564 ? O3 Zn2 N2 96.66(12) 3_645 2_564 ? O7 Zn2 N2 77.87(11) 2_564 2_564 ? O6 Zn2 N2 171.78(15) . 2_564 ? C1 O1 Zn1 146.4(3) . . ? C1 O2 Zn2 122.2(3) . 1_655 ? C9 O3 Zn2 113.0(3) . 3_655 ? C9 O3 Zn1 119.5(3) . 3_755 ? Zn2 O3 Zn1 116.75(14) 3_655 3_755 ? C14 O5 Zn1 131.3(3) . . ? C14 O6 Zn2 132.8(3) . . ? C22 O7 Zn1 120.4(2) . 2_565 ? C22 O7 Zn2 117.1(2) . 2_565 ? Zn1 O7 Zn2 121.68(10) 2_565 2_565 ? C10 N1 C8 111.9(4) . . ? C10 N1 Zn1 108.7(2) . 3_755 ? C8 N1 Zn1 108.3(3) . 3_755 ? C23 N2 C21 113.0(3) . . ? C23 N2 Zn2 106.3(2) . 2_565 ? C21 N2 Zn2 115.0(2) . 2_565 ? O1 C1 O2 125.5(4) . . ? O1 C1 C2 116.5(4) . . ? O2 C1 C2 118.0(4) . . ? C3 C2 C7 118.5(4) . . ? C3 C2 C1 120.7(4) . . ? C7 C2 C1 120.8(4) . . ? C2 C3 C4 121.1(5) . . ? C5 C4 C3 120.5(5) . . ? C4 C5 C6 118.6(4) . . ? C4 C5 C8 121.1(5) . . ? C6 C5 C8 120.3(5) . . ? C7 C6 C5 120.8(5) . . ? C2 C7 C6 120.5(4) . . ? N1 C8 C5 114.4(4) . . ? O4 C9 O3 123.2(5) . . ? O4 C9 C10 121.8(4) . . ? O3 C9 C10 115.0(4) . . ? N1 C10 C9 107.2(4) . . ? N1 C10 C11 110.7(4) . . ? C9 C10 C11 113.5(4) . . ? C12 C11 C13 110.8(6) . . ? C12 C11 C10 112.3(7) . . ? C13 C11 C10 110.3(5) . . ? O6 C14 O5 124.6(3) . . ? O6 C14 C15 119.3(4) . . ? O5 C14 C15 116.1(3) . . ? C16 C15 C20 118.7(3) . . ? C16 C15 C14 122.3(4) . . ? C20 C15 C14 119.0(4) . . ? C15 C16 C17 120.6(4) . . ? C18 C17 C16 120.9(4) . . ? C19 C18 C17 117.7(3) . . ? C19 C18 C21 118.7(4) . . ? C17 C18 C21 123.6(4) . . ? C18 C19 C20 121.3(4) . . ? C15 C20 C19 120.7(4) . . ? N2 C21 C18 112.8(3) . . ? O8 C22 O7 123.5(4) . . ? O8 C22 C23 121.2(3) . . ? O7 C22 C23 115.4(3) . . ? N2 C23 C22 109.0(3) . . ? N2 C23 C25 112.0(4) . . ? C22 C23 C25 112.3(4) . . ? C26 C25 C24 110.3(5) . . ? C26 C25 C23 112.4(5) . . ? C24 C25 C23 109.8(5) . . ? 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 N2 H22A O8 0.91 2.49 3.182(5) 132.8 1_655 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 67.06 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.439 _refine_diff_density_min -0.186 _refine_diff_density_rms 0.055 #===END data_New4 _database_code_depnum_ccdc_archive 'CCDC 821195' #TrackingRef '- New.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H19 Cu N O9' _chemical_formula_weight 372.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 21.5285(10) _cell_length_b 5.9677(3) _cell_length_c 11.6873(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.289(5) _cell_angle_gamma 90.00 _cell_volume 1485.85(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3531 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 26.37 _exptl_crystal_description bloc _exptl_crystal_colour blue _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 1.516 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.804 _exptl_absorpt_correction_T_max 0.913 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3531 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0938 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 26.37 _reflns_number_total 2478 _reflns_number_gt 1856 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0082P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.036(18) _refine_ls_number_reflns 2478 _refine_ls_number_parameters 204 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0538 _refine_ls_wR_factor_gt 0.0512 _refine_ls_goodness_of_fit_ref 0.876 _refine_ls_restrained_S_all 0.876 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.42518(2) 0.11341(11) 0.24443(4) 0.02276(13) Uani 1 1 d . . . O1 O 0.06260(14) 0.8112(6) 0.3296(3) 0.0482(10) Uani 1 1 d . . . O2 O 0.01231(13) 0.5185(5) 0.2428(2) 0.0293(8) Uani 1 1 d . . . O3 O 0.39501(14) -0.1922(5) 0.2007(2) 0.0274(8) Uani 1 1 d . . . O4 O 0.31300(13) -0.3648(7) 0.0995(2) 0.0397(8) Uani 1 1 d . . . O5 O 0.40413(14) 0.1487(8) 0.0238(2) 0.0428(10) Uani 1 1 d . . . H5A H 0.4119 0.2408 -0.0429 0.051 Uiso 1 1 d . . . O6 O 0.44707(14) 0.4266(5) 0.2906(3) 0.0317(9) Uani 1 1 d . . . H6B H 0.4274 0.5193 0.2435 0.038 Uiso 1 1 d . . . H6C H 0.4867 0.4111 0.3086 0.038 Uiso 1 1 d . . . O7 O 0.43635(15) 0.0230(5) 0.4420(2) 0.0415(10) Uani 1 1 d . . . H7B H 0.4191 -0.0936 0.4640 0.050 Uiso 1 1 d . . . H7C H 0.4189 0.1329 0.4750 0.050 Uiso 1 1 d . . . O101 O 0.39035(14) 0.5984(9) 0.4826(2) 0.0549(9) Uani 1 1 d . . . H10A H 0.4083 0.5151 0.4375 0.066 Uiso 1 1 d . . . H10B H 0.4125 0.5326 0.5388 0.066 Uiso 1 1 d . . . O102 O 0.5000 -0.1432(10) 0.0000 0.0575(19) Uani 1 2 d S . . H10C H 0.5035 -0.1009 0.0702 0.069 Uiso 1 1 d . . . O103 O 0.4854(5) 0.4248(14) -0.0454(6) 0.064(3) Uani 0.50 1 d P . . N1 N 0.33338(14) 0.1851(5) 0.2087(3) 0.0191(9) Uani 1 1 d . . . H1A H 0.3286 0.3307 0.1860 0.023 Uiso 1 1 calc R . . C1 C 0.06148(16) 0.6173(13) 0.2871(3) 0.0245(9) Uani 1 1 d . . . C2 C 0.1231(2) 0.4957(8) 0.2898(3) 0.0227(11) Uani 1 1 d . . . C3 C 0.17771(16) 0.5892(11) 0.3432(3) 0.0260(11) Uani 1 1 d . . . H3A H 0.1770 0.7310 0.3759 0.031 Uiso 1 1 calc R . . C4 C 0.2339(2) 0.4753(8) 0.3490(3) 0.0296(12) Uani 1 1 d . . . H4A H 0.2705 0.5402 0.3868 0.036 Uiso 1 1 calc R . . C5 C 0.23633(19) 0.2671(8) 0.2997(3) 0.0238(11) Uani 1 1 d . . . C6 C 0.18098(18) 0.1713(7) 0.2453(3) 0.0268(13) Uani 1 1 d . . . H6A H 0.1822 0.0308 0.2114 0.032 Uiso 1 1 calc R . . C7 C 0.12446(19) 0.2808(8) 0.2408(3) 0.0260(11) Uani 1 1 d . . . H7A H 0.0876 0.2135 0.2058 0.031 Uiso 1 1 calc R . . C8 C 0.29901(17) 0.1464(11) 0.3080(3) 0.0282(12) Uani 1 1 d . . . H8A H 0.3253 0.1942 0.3782 0.034 Uiso 1 1 calc R . . H8B H 0.2918 -0.0133 0.3146 0.034 Uiso 1 1 calc R . . C9 C 0.31311(19) 0.0374(6) 0.1085(3) 0.0231(11) Uani 1 1 d . . . H9A H 0.2672 0.0287 0.0949 0.028 Uiso 1 1 calc R . . C10 C 0.3405(2) -0.1953(8) 0.1372(4) 0.0268(11) Uani 1 1 d . . . C11 C 0.33673(17) 0.1263(12) 0.0018(3) 0.0325(10) Uani 1 1 d . . . H11A H 0.3250 0.0245 -0.0624 0.039 Uiso 1 1 calc R . . H11B H 0.3178 0.2709 -0.0188 0.039 Uiso 1 1 calc R . . 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 Cu1 0.0133(2) 0.0204(3) 0.0341(2) -0.0029(4) 0.00208(18) 0.0030(4) O1 0.0190(19) 0.035(2) 0.087(3) -0.024(2) -0.0044(18) 0.0082(17) O2 0.0144(16) 0.027(2) 0.0451(18) -0.0067(16) 0.0015(14) 0.0021(15) O3 0.0187(17) 0.0168(19) 0.0436(19) -0.0014(16) -0.0052(15) 0.0055(15) O4 0.0352(16) 0.0194(19) 0.0592(17) -0.008(2) -0.0108(14) -0.004(2) O5 0.0331(16) 0.054(3) 0.0436(15) 0.006(2) 0.0149(13) 0.005(2) O6 0.0170(17) 0.024(2) 0.051(2) -0.0034(16) -0.0047(15) 0.0047(15) O7 0.043(2) 0.041(3) 0.0420(18) -0.0006(16) 0.0117(16) 0.0027(17) O101 0.067(2) 0.049(2) 0.0486(16) -0.009(3) 0.0076(16) 0.002(3) O102 0.078(5) 0.042(4) 0.049(4) 0.000 -0.002(3) 0.000 O103 0.077(8) 0.053(6) 0.064(7) 0.009(4) 0.021(6) -0.002(5) N1 0.0126(18) 0.014(2) 0.0305(19) 0.0058(15) 0.0024(15) 0.0067(15) C1 0.020(2) 0.026(2) 0.027(2) 0.005(4) 0.0023(16) 0.009(4) C2 0.018(2) 0.026(3) 0.025(2) 0.002(2) 0.005(2) 0.007(2) C3 0.017(2) 0.024(3) 0.035(2) -0.007(3) -0.0003(17) -0.003(3) C4 0.016(2) 0.036(3) 0.034(3) -0.007(2) -0.004(2) 0.006(2) C5 0.011(2) 0.033(3) 0.028(2) -0.001(2) 0.0040(19) 0.006(2) C6 0.021(2) 0.021(3) 0.038(2) -0.004(2) 0.004(2) 0.005(2) C7 0.012(2) 0.036(3) 0.029(3) 0.003(2) 0.000(2) -0.002(2) C8 0.020(2) 0.033(4) 0.031(2) -0.002(3) 0.0026(17) 0.011(3) C9 0.013(2) 0.021(3) 0.033(2) -0.005(2) -0.0039(19) 0.0001(19) C10 0.026(3) 0.024(3) 0.029(3) 0.001(2) -0.001(2) 0.005(2) C11 0.026(2) 0.036(3) 0.036(2) -0.006(4) 0.0058(18) 0.005(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 Cu1 O2 1.962(3) 3_545 ? Cu1 O3 1.978(3) . ? Cu1 O6 1.983(3) . ? Cu1 N1 2.006(3) . ? Cu1 O7 2.349(3) . ? Cu1 O5 2.561(3) . ? O1 C1 1.258(8) . ? O2 C1 1.256(5) . ? O2 Cu1 1.962(3) 3_455 ? O3 C10 1.294(4) . ? O4 C10 1.222(6) . ? O5 C11 1.443(4) . ? O103 O103 1.153(13) 2_655 ? N1 C9 1.480(4) . ? N1 C8 1.482(5) . ? C1 C2 1.508(6) . ? C2 C3 1.368(5) . ? C2 C7 1.407(6) . ? C3 C4 1.380(6) . ? C4 C5 1.374(6) . ? C5 C6 1.390(5) . ? C5 C8 1.520(6) . ? C6 C7 1.375(5) . ? C9 C11 1.510(6) . ? C9 C10 1.527(6) . ? 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 O2 Cu1 O3 90.58(12) 3_545 . ? O2 Cu1 O6 94.86(12) 3_545 . ? O3 Cu1 O6 174.50(14) . . ? O2 Cu1 N1 166.88(12) 3_545 . ? O3 Cu1 N1 82.30(12) . . ? O6 Cu1 N1 92.52(12) . . ? O2 Cu1 O7 88.91(11) 3_545 . ? O3 Cu1 O7 91.47(11) . . ? O6 Cu1 O7 87.84(12) . . ? N1 Cu1 O7 102.22(13) . . ? O2 Cu1 O5 92.55(11) 3_545 . ? O3 Cu1 O5 79.15(14) . . ? O6 Cu1 O5 101.36(14) . . ? N1 Cu1 O5 75.34(11) . . ? O7 Cu1 O5 170.52(14) . . ? C1 O2 Cu1 127.6(3) . 3_455 ? C10 O3 Cu1 113.4(3) . . ? C11 O5 Cu1 101.5(2) . . ? C9 N1 C8 113.8(3) . . ? C9 N1 Cu1 101.9(2) . . ? C8 N1 Cu1 113.1(2) . . ? O2 C1 O1 124.1(4) . . ? O2 C1 C2 118.0(6) . . ? O1 C1 C2 117.9(4) . . ? C3 C2 C7 119.3(4) . . ? C3 C2 C1 120.6(5) . . ? C7 C2 C1 120.0(4) . . ? C2 C3 C4 120.8(5) . . ? C5 C4 C3 120.7(4) . . ? C4 C5 C6 118.8(4) . . ? C4 C5 C8 119.3(4) . . ? C6 C5 C8 121.9(4) . . ? C7 C6 C5 121.2(4) . . ? C6 C7 C2 119.2(4) . . ? N1 C8 C5 114.5(3) . . ? N1 C9 C11 110.4(4) . . ? N1 C9 C10 107.9(3) . . ? C11 C9 C10 109.6(4) . . ? O4 C10 O3 124.8(4) . . ? O4 C10 C9 121.4(4) . . ? O3 C10 C9 113.7(4) . . ? O5 C11 C9 109.6(3) . . ? 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 O5 H5A O103 0.99 1.93 2.615(10) 124.1 . O6 H6B O3 0.85 1.90 2.682(3) 153.1 1_565 O6 H6C O1 0.85 1.72 2.558(4) 165.0 3_545 O7 H7B O101 0.85 1.96 2.786(6) 164.5 1_545 O101 H10A O6 0.86 2.08 2.893(4) 157.7 . O101 H10B O1 0.85 2.04 2.853(5) 159.9 4_546 O102 H10C O2 0.85 2.12 2.972(3) 177.6 3_545 N1 H1A O4 0.91 2.08 2.979(5) 168.0 1_565 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.308 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.070 #===END data_New5 _database_code_depnum_ccdc_archive 'CCDC 821196' #TrackingRef '- New.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H11 N O5 Zn' _chemical_formula_weight 302.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.3240(8) _cell_length_b 6.4377(4) _cell_length_c 11.3504(8) _cell_angle_alpha 90.00 _cell_angle_beta 101.988(9) _cell_angle_gamma 90.00 _cell_volume 594.97(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2326 _cell_measurement_theta_min 3.67 _cell_measurement_theta_max 25.05 _exptl_crystal_description bloc _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 308 _exptl_absorpt_coefficient_mu 2.076 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.503 _exptl_absorpt_correction_T_max 0.830 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2326 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0857 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.67 _diffrn_reflns_theta_max 25.05 _reflns_number_total 1774 _reflns_number_gt 1300 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(3) _refine_ls_number_reflns 1774 _refine_ls_number_parameters 163 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0724 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1018 _refine_ls_wR_factor_gt 0.0969 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn -0.00003(10) 0.76868(14) 0.83226(7) 0.0322(3) Uani 1 1 d . . . O1 O 0.2280(7) 0.5412(11) 0.7637(5) 0.0572(18) Uani 1 1 d . . . O2 O 0.0215(7) 0.7227(11) 0.6680(5) 0.046(2) Uani 1 1 d . . . O3 O 0.0164(7) 0.0557(8) 0.0395(4) 0.0347(14) Uani 1 1 d . . . O4 O 0.1559(6) -0.0198(8) -0.0978(4) 0.0347(13) Uani 1 1 d . . . O5 O 0.4541(7) -0.0265(8) 0.1410(5) 0.0426(15) Uani 1 1 d . . . H5A H 0.5477 -0.0432 0.1805 0.051 Uiso 1 1 d . . . N1 N 0.2433(7) 0.3007(12) 0.1660(5) 0.0257(17) Uani 1 1 d . . . H1A H 0.2950 0.2038 0.2190 0.031 Uiso 1 1 calc R . . C1 C 0.1530(10) 0.6208(13) 0.6696(7) 0.032(2) Uani 1 1 d . . . C2 C 0.2090(10) 0.6002(12) 0.5520(7) 0.032(2) Uani 1 1 d . . . C3 C 0.3302(10) 0.4608(15) 0.5411(7) 0.043(2) Uani 1 1 d . . . H3A H 0.3827 0.3832 0.6070 0.051 Uiso 1 1 calc R . . C4 C 0.3724(11) 0.4385(15) 0.4303(8) 0.047(2) Uani 1 1 d . . . H4A H 0.4549 0.3453 0.4224 0.057 Uiso 1 1 calc R . . C5 C 0.2947(10) 0.5515(12) 0.3302(7) 0.033(2) Uani 1 1 d . . . C6 C 0.1767(11) 0.6943(11) 0.3459(7) 0.047(3) Uani 1 1 d . . . H6A H 0.1270 0.7786 0.2822 0.056 Uiso 1 1 calc R . . C7 C 0.1334(11) 0.7111(12) 0.4550(7) 0.046(3) Uani 1 1 d . . . H7A H 0.0493 0.8017 0.4630 0.055 Uiso 1 1 calc R . . C8 C 0.3264(10) 0.5032(12) 0.2087(7) 0.037(2) Uani 1 1 d . . . H8A H 0.4437 0.4920 0.2127 0.044 Uiso 1 1 calc R . . H8B H 0.2836 0.6135 0.1527 0.044 Uiso 1 1 calc R . . C9 C 0.1387(9) 0.0803(11) -0.0047(6) 0.0248(18) Uani 1 1 d . . . C10 C 0.2716(8) 0.2337(14) 0.0478(6) 0.022(2) Uani 1 1 d . . . H10A H 0.2629 0.3549 -0.0055 0.027 Uiso 1 1 calc R . . C11 C 0.4397(9) 0.1397(11) 0.0595(6) 0.0283(19) Uani 1 1 d . . . H11A H 0.4545 0.0906 -0.0183 0.034 Uiso 1 1 calc R . . H11B H 0.5233 0.2431 0.0885 0.034 Uiso 1 1 calc R . . 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 Zn1 0.0411(5) 0.0309(4) 0.0268(4) -0.0018(7) 0.0125(4) -0.0029(7) O1 0.042(4) 0.087(5) 0.043(4) 0.002(4) 0.010(3) 0.003(4) O2 0.047(4) 0.062(7) 0.031(3) -0.013(3) 0.010(3) 0.003(4) O3 0.036(3) 0.033(3) 0.037(3) -0.010(3) 0.010(3) -0.008(3) O4 0.038(4) 0.038(3) 0.028(3) -0.004(3) 0.006(3) -0.009(3) O5 0.053(4) 0.023(3) 0.051(4) 0.019(3) 0.009(3) 0.002(3) N1 0.033(3) 0.025(5) 0.019(3) -0.010(3) 0.004(3) 0.003(4) C1 0.018(5) 0.044(5) 0.032(5) -0.006(4) 0.003(4) -0.007(4) C2 0.024(5) 0.039(5) 0.031(5) -0.017(4) 0.004(4) -0.006(4) C3 0.035(6) 0.064(6) 0.029(5) -0.012(4) 0.005(4) 0.019(5) C4 0.042(6) 0.057(6) 0.044(6) -0.023(5) 0.011(5) 0.008(5) C5 0.037(5) 0.024(4) 0.037(5) -0.018(4) 0.007(4) -0.021(4) C6 0.082(7) 0.027(5) 0.036(5) -0.007(3) 0.024(5) 0.029(4) C7 0.061(6) 0.046(7) 0.032(4) -0.008(4) 0.015(4) 0.026(5) C8 0.044(5) 0.035(5) 0.031(5) -0.013(4) 0.005(4) -0.022(4) C9 0.029(5) 0.031(5) 0.016(4) -0.002(4) 0.009(4) 0.011(4) C10 0.024(4) 0.020(6) 0.025(3) 0.004(3) 0.010(3) -0.008(4) C11 0.029(5) 0.029(4) 0.028(4) -0.002(4) 0.008(4) -0.007(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 Zn1 O2 1.932(5) . ? Zn1 O4 1.934(5) 1_566 ? Zn1 O3 2.025(5) 2_556 ? Zn1 N1 2.040(5) 2_556 ? O1 C1 1.231(9) . ? O2 C1 1.273(9) . ? O3 C9 1.235(8) . ? O3 Zn1 2.025(5) 2_546 ? O4 C9 1.271(8) . ? O4 Zn1 1.934(5) 1_544 ? O5 C11 1.403(8) . ? N1 C10 1.475(7) . ? N1 C8 1.508(10) . ? N1 Zn1 2.040(5) 2_546 ? C1 C2 1.509(10) . ? C2 C7 1.352(10) . ? C2 C3 1.374(11) . ? C3 C4 1.382(10) . ? C4 C5 1.390(12) . ? C5 C6 1.383(10) . ? C5 C8 1.491(10) . ? C6 C7 1.364(10) . ? C9 C10 1.510(10) . ? C10 C11 1.505(9) . ? 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 O2 Zn1 O4 108.3(2) . 1_566 ? O2 Zn1 O3 128.6(3) . 2_556 ? O4 Zn1 O3 108.7(2) 1_566 2_556 ? O2 Zn1 N1 108.4(2) . 2_556 ? O4 Zn1 N1 120.5(3) 1_566 2_556 ? O3 Zn1 N1 81.1(2) 2_556 2_556 ? C1 O2 Zn1 108.5(5) . . ? C9 O3 Zn1 112.9(5) . 2_546 ? C9 O4 Zn1 121.1(5) . 1_544 ? C10 N1 C8 113.3(6) . . ? C10 N1 Zn1 109.0(4) . 2_546 ? C8 N1 Zn1 118.3(5) . 2_546 ? O1 C1 O2 120.4(8) . . ? O1 C1 C2 122.4(8) . . ? O2 C1 C2 117.1(8) . . ? C7 C2 C3 119.8(7) . . ? C7 C2 C1 119.8(7) . . ? C3 C2 C1 120.3(8) . . ? C2 C3 C4 118.7(8) . . ? C3 C4 C5 121.7(8) . . ? C6 C5 C4 117.7(7) . . ? C6 C5 C8 121.7(8) . . ? C4 C5 C8 120.3(8) . . ? C7 C6 C5 119.9(8) . . ? C2 C7 C6 122.1(7) . . ? C5 C8 N1 108.7(6) . . ? O3 C9 O4 121.2(7) . . ? O3 C9 C10 121.5(6) . . ? O4 C9 C10 117.3(6) . . ? N1 C10 C11 111.0(6) . . ? N1 C10 C9 107.9(5) . . ? C11 C10 C9 111.3(6) . . ? O5 C11 C10 108.4(6) . . ? 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 O5 H5A O1 0.82 1.92 2.678(8) 152.8 2_646 N1 H1A O5 0.91 2.29 2.793(9) 114.9 . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.598 _refine_diff_density_min -0.624 _refine_diff_density_rms 0.096 #===END data_New6 _database_code_depnum_ccdc_archive 'CCDC 821197' #TrackingRef '- New.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H46 Cd3 Cl N4 Na O23' _chemical_formula_weight 1298.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M P2(1)3 loop_ _symmetry_equiv_pos_as_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' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' _cell_length_a 17.01460(10) _cell_length_b 17.01460(10) _cell_length_c 17.01460(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4925.67(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7138 _cell_measurement_theta_min 3.39 _cell_measurement_theta_max 26.01 _exptl_crystal_description bloc _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2584 _exptl_absorpt_coefficient_mu 1.429 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.681 _exptl_absorpt_correction_T_max 0.796 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7138 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0796 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 26.01 _reflns_number_total 3222 _reflns_number_gt 2291 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.037 0.037 0.037 317 41 ' ' 2 -0.038 0.537 0.463 317 41 ' ' 3 0.169 0.669 0.831 25 9 ' ' 4 0.462 0.963 0.537 317 41 ' ' 5 0.331 0.331 0.331 25 9 ' ' 6 0.537 0.463 -0.037 317 41 ' ' 7 0.669 0.831 0.169 25 9 ' ' 8 0.830 0.169 0.669 25 9 ' ' _platon_squeeze_details ; ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(4) _refine_ls_number_reflns 3222 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0847 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd -0.09052(3) -1.08533(3) -0.33828(3) 0.03706(14) Uani 1 1 d . . . Na1 Na -0.00496(13) -0.99504(13) -0.49504(13) 0.0360(10) Uani 1 3 d S . . Cl1 Cl -0.18787(9) -1.18787(9) -0.18787(9) 0.0361(6) Uani 1 3 d S . . O1 O 0.0048(4) -0.7965(3) -0.2903(4) 0.0783(19) Uani 1 1 d . . . H11A H -0.0364 -0.7607 -0.2918 0.094 Uiso 1 1 calc R . . O2 O 0.3353(4) -1.1719(4) -0.0302(3) 0.0860(18) Uani 1 1 d . . . O3 O 0.3795(3) -1.0580(3) 0.0033(3) 0.0641(15) Uani 1 1 d . . . O4 O -0.1152(2) -1.1644(3) -0.2303(3) 0.0487(12) Uani 1 1 d . . . O5 O -0.0281(3) -1.0071(3) -0.2521(3) 0.0579(14) Uani 1 1 d . . . O6 O 0.0102(3) -0.9561(3) -0.3631(3) 0.0418(11) Uani 1 1 d . . . O7 O -0.2381(3) -1.2381(3) -0.2381(3) 0.065(3) Uani 1 3 d S . . N1 N 0.1392(3) -0.8916(3) -0.2960(3) 0.0398(14) Uani 1 1 d . . . H1D H 0.1705 -0.8570 -0.2660 0.048 Uiso 1 1 d . . . C1 C 0.1906(5) -0.9578(5) -0.3132(5) 0.060(2) Uani 1 1 d . . . H1A H 0.2318 -0.9402 -0.3485 0.072 Uiso 1 1 calc R . . H1B H 0.1604 -0.9977 -0.3404 0.072 Uiso 1 1 calc R . . C2 C 0.0324(5) -0.8368(5) -0.2185(5) 0.063(2) Uani 1 1 d . . . H2A H -0.0117 -0.8496 -0.1846 0.076 Uiso 1 1 calc R . . H2B H 0.0686 -0.8036 -0.1896 0.076 Uiso 1 1 calc R . . C3 C 0.0730(3) -0.9106(4) -0.2460(3) 0.0377(15) Uani 1 1 d . . . H3A H 0.0922 -0.9395 -0.2000 0.045 Uiso 1 1 calc R . . C4 C 0.3410(4) -1.0991(5) -0.0404(4) 0.053(2) Uani 1 1 d . . . C5 C 0.0156(4) -0.9626(4) -0.2906(4) 0.0353(16) Uani 1 1 d . . . C6 C 0.2286(4) -0.9948(4) -0.2413(4) 0.0459(18) Uani 1 1 d . . . C7 C 0.2707(5) -0.9495(5) -0.1880(5) 0.071(3) Uani 1 1 d . . . H7A H 0.2736 -0.8953 -0.1944 0.085 Uiso 1 1 calc R . . C8 C 0.2194(4) -1.0777(5) -0.2265(4) 0.064(2) Uani 1 1 d . . . H8A H 0.1884 -1.1079 -0.2599 0.077 Uiso 1 1 calc R . . C9 C 0.3083(5) -0.9854(5) -0.1252(5) 0.070(3) Uani 1 1 d . . . H9A H 0.3393 -0.9555 -0.0916 0.084 Uiso 1 1 calc R . . C10 C 0.2562(5) -1.1126(4) -0.1636(5) 0.061(2) Uani 1 1 d . . . H10A H 0.2515 -1.1666 -0.1560 0.074 Uiso 1 1 calc R . . C11 C 0.3000(4) -1.0680(4) -0.1117(4) 0.0486(18) Uani 1 1 d . . . 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 Cd1 0.0372(3) 0.0375(3) 0.0365(3) 0.0015(2) -0.0014(2) -0.0057(2) Na1 0.0360(10) 0.0360(10) 0.0360(10) -0.0013(11) 0.0013(11) 0.0013(11) Cl1 0.0361(6) 0.0361(6) 0.0361(6) 0.0037(7) 0.0037(7) 0.0037(7) O1 0.073(4) 0.047(3) 0.115(5) -0.012(3) 0.027(4) 0.006(3) O2 0.076(4) 0.115(5) 0.067(4) 0.049(4) -0.023(3) 0.001(4) O3 0.052(3) 0.091(4) 0.050(3) -0.003(3) -0.019(3) 0.004(3) O4 0.038(3) 0.058(3) 0.050(3) 0.016(3) 0.018(2) 0.008(2) O5 0.074(4) 0.051(3) 0.048(3) 0.003(3) -0.006(3) -0.021(3) O6 0.040(3) 0.049(3) 0.036(3) -0.002(2) -0.007(2) -0.001(2) O7 0.065(3) 0.065(3) 0.065(3) -0.011(3) -0.011(3) -0.011(3) N1 0.047(4) 0.037(4) 0.036(3) 0.010(2) -0.011(3) -0.003(3) C1 0.066(5) 0.058(5) 0.056(5) 0.014(4) -0.004(4) -0.003(4) C2 0.077(6) 0.049(5) 0.062(5) -0.007(4) 0.006(4) -0.005(5) C3 0.044(4) 0.042(4) 0.026(3) 0.007(3) -0.003(3) -0.007(3) C4 0.039(4) 0.071(6) 0.048(5) 0.032(4) 0.010(4) 0.004(4) C5 0.042(4) 0.027(4) 0.037(4) 0.002(3) -0.003(3) -0.004(3) C6 0.035(4) 0.052(5) 0.051(4) 0.017(4) -0.010(3) -0.001(3) C7 0.077(6) 0.048(5) 0.088(7) 0.016(4) -0.033(5) -0.017(4) C8 0.067(5) 0.070(6) 0.055(5) -0.001(5) -0.029(4) -0.013(5) C9 0.064(6) 0.078(6) 0.068(6) 0.002(5) -0.039(4) -0.022(5) C10 0.091(6) 0.039(4) 0.054(5) 0.019(4) -0.026(5) -0.017(4) C11 0.037(4) 0.064(5) 0.045(5) 0.015(4) -0.005(3) -0.001(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 Cd1 O5 2.247(5) . ? Cd1 O4 2.315(4) . ? Cd1 N1 2.321(5) 7_445 ? Cd1 O3 2.383(5) 8_533 ? Cd1 O2 2.463(5) 8_533 ? Cd1 O6 2.505(4) 7_445 ? Cd1 O1 2.548(5) 7_445 ? Cd1 Na1 3.4050(18) . ? Na1 O3 2.318(6) 8_533 ? Na1 O3 2.318(6) 2_534 ? Na1 O3 2.318(6) 9_644 ? Na1 O6 2.356(5) 10_444 ? Na1 O6 2.356(5) 7_445 ? Na1 O6 2.356(5) . ? Na1 Cd1 3.4049(18) 10_444 ? Na1 Cd1 3.4050(18) 7_445 ? Cl1 O7 1.480(9) . ? Cl1 O4 1.486(4) . ? Cl1 O4 1.486(4) 9_645 ? Cl1 O4 1.486(4) 5_546 ? O1 C2 1.477(10) . ? O1 Cd1 2.548(5) 10_444 ? O2 C4 1.255(10) . ? O2 Cd1 2.463(5) 11_635 ? O3 C4 1.213(9) . ? O3 Na1 2.318(6) 2_535 ? O3 Cd1 2.383(5) 11_635 ? O5 C5 1.248(7) . ? O6 C5 1.241(7) . ? O6 Cd1 2.504(4) 10_444 ? N1 C3 1.449(8) . ? N1 C1 1.456(9) . ? N1 Cd1 2.321(5) 10_444 ? C1 C6 1.520(10) . ? C2 C3 1.508(10) . ? C3 C5 1.521(8) . ? C4 C11 1.496(9) . ? C6 C7 1.388(10) . ? C6 C8 1.442(10) . ? C7 C9 1.387(10) . ? C8 C10 1.374(9) . ? C9 C11 1.431(10) . ? C10 C11 1.384(9) . ? 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 Cd1 O4 84.97(18) . . ? O5 Cd1 N1 151.9(2) . 7_445 ? O4 Cd1 N1 85.95(17) . 7_445 ? O5 Cd1 O3 109.7(2) . 8_533 ? O4 Cd1 O3 123.71(17) . 8_533 ? N1 Cd1 O3 97.44(19) 7_445 8_533 ? O5 Cd1 O2 83.4(2) . 8_533 ? O4 Cd1 O2 77.13(19) . 8_533 ? N1 Cd1 O2 120.3(2) 7_445 8_533 ? O3 Cd1 O2 52.79(19) 8_533 8_533 ? O5 Cd1 O6 111.66(16) . 7_445 ? O4 Cd1 O6 150.92(15) . 7_445 ? N1 Cd1 O6 68.08(15) 7_445 7_445 ? O3 Cd1 O6 74.44(17) 8_533 7_445 ? O2 Cd1 O6 126.78(19) 8_533 7_445 ? O5 Cd1 O1 82.9(2) . 7_445 ? O4 Cd1 O1 86.93(16) . 7_445 ? N1 Cd1 O1 70.1(2) 7_445 7_445 ? O3 Cd1 O1 146.86(18) 8_533 7_445 ? O2 Cd1 O1 159.8(2) 8_533 7_445 ? O6 Cd1 O1 72.42(16) 7_445 7_445 ? O5 Cd1 Na1 92.39(13) . . ? O4 Cd1 Na1 164.01(11) . . ? N1 Cd1 Na1 103.16(12) 7_445 . ? O3 Cd1 Na1 42.83(14) 8_533 . ? O2 Cd1 Na1 86.90(16) 8_533 . ? O6 Cd1 Na1 43.77(11) 7_445 . ? O1 Cd1 Na1 108.43(14) 7_445 . ? O3 Na1 O3 110.61(15) 8_533 2_534 ? O3 Na1 O3 110.61(15) 8_533 9_644 ? O3 Na1 O3 110.61(15) 2_534 9_644 ? O3 Na1 O6 157.5(2) 8_533 10_444 ? O3 Na1 O6 83.50(18) 2_534 10_444 ? O3 Na1 O6 78.53(16) 9_644 10_444 ? O3 Na1 O6 78.53(16) 8_533 7_445 ? O3 Na1 O6 157.5(2) 2_534 7_445 ? O3 Na1 O6 83.51(18) 9_644 7_445 ? O6 Na1 O6 82.36(19) 10_444 7_445 ? O3 Na1 O6 83.51(18) 8_533 . ? O3 Na1 O6 78.53(16) 2_534 . ? O3 Na1 O6 157.5(2) 9_644 . ? O6 Na1 O6 82.36(19) 10_444 . ? O6 Na1 O6 82.36(19) 7_445 . ? O3 Na1 Cd1 123.34(14) 8_533 10_444 ? O3 Na1 Cd1 44.34(13) 2_534 10_444 ? O3 Na1 Cd1 125.39(13) 9_644 10_444 ? O6 Na1 Cd1 55.05(12) 10_444 10_444 ? O6 Na1 Cd1 113.31(17) 7_445 10_444 ? O6 Na1 Cd1 47.34(11) . 10_444 ? O3 Na1 Cd1 125.39(13) 8_533 7_445 ? O3 Na1 Cd1 123.33(14) 2_534 7_445 ? O3 Na1 Cd1 44.34(13) 9_644 7_445 ? O6 Na1 Cd1 47.34(11) 10_444 7_445 ? O6 Na1 Cd1 55.05(12) 7_445 7_445 ? O6 Na1 Cd1 113.31(17) . 7_445 ? Cd1 Na1 Cd1 102.20(7) 10_444 7_445 ? O3 Na1 Cd1 44.34(13) 8_533 . ? O3 Na1 Cd1 125.39(13) 2_534 . ? O3 Na1 Cd1 123.33(14) 9_644 . ? O6 Na1 Cd1 113.31(17) 10_444 . ? O6 Na1 Cd1 47.34(11) 7_445 . ? O6 Na1 Cd1 55.06(12) . . ? Cd1 Na1 Cd1 102.20(7) 10_444 . ? Cd1 Na1 Cd1 102.20(7) 7_445 . ? O7 Cl1 O4 110.8(2) . . ? O7 Cl1 O4 110.8(2) . 9_645 ? O4 Cl1 O4 108.1(2) . 9_645 ? O7 Cl1 O4 110.8(2) . 5_546 ? O4 Cl1 O4 108.1(2) . 5_546 ? O4 Cl1 O4 108.1(2) 9_645 5_546 ? C2 O1 Cd1 111.0(4) . 10_444 ? C4 O2 Cd1 90.3(5) . 11_635 ? C4 O3 Na1 136.8(5) . 2_535 ? C4 O3 Cd1 95.2(5) . 11_635 ? Na1 O3 Cd1 92.8(2) 2_535 11_635 ? Cl1 O4 Cd1 133.9(2) . . ? C5 O5 Cd1 107.4(4) . . ? C5 O6 Na1 158.4(4) . . ? C5 O6 Cd1 110.3(4) . 10_444 ? Na1 O6 Cd1 88.89(15) . 10_444 ? C3 N1 C1 114.3(5) . . ? C3 N1 Cd1 105.6(4) . 10_444 ? C1 N1 Cd1 111.9(4) . 10_444 ? N1 C1 C6 114.5(6) . . ? O1 C2 C3 106.0(6) . . ? N1 C3 C2 110.6(6) . . ? N1 C3 C5 109.6(5) . . ? C2 C3 C5 110.1(6) . . ? O3 C4 O2 121.7(7) . . ? O3 C4 C11 123.0(8) . . ? O2 C4 C11 115.3(8) . . ? O6 C5 O5 122.1(6) . . ? O6 C5 C3 119.5(6) . . ? O5 C5 C3 118.3(6) . . ? C7 C6 C8 119.0(6) . . ? C7 C6 C1 121.0(7) . . ? C8 C6 C1 120.0(6) . . ? C9 C7 C6 119.8(7) . . ? C10 C8 C6 120.6(7) . . ? C7 C9 C11 120.7(7) . . ? C8 C10 C11 120.4(6) . . ? C10 C11 C9 119.3(6) . . ? C10 C11 C4 125.1(7) . . ? C9 C11 C4 115.6(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 O1 H11A O2 0.93 2.62 3.073(9) 110.9 5_546 N1 H1D O7 0.94 2.33 3.160(5) 146.7 3_554 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.454 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.083 #===END