# Copyright The Royal Society of Chemistry, 1998 data_global #================================================================= # SUBMISSION DETAILS _publ_contact_author ; Dr. Michael Ward School of Chemistry University of Bristol Cantock's Close BS8 1TS Bristol UK ; _publ_contact_author_phone '0117 9287655' _publ_contact_author_fax '0117 9290509' _publ_contact_author_email mike.ward@bristol.ac.uk _publ_contact_letter ; This CIF file contains details of the six crystal structures in the paper 'Synthesis and coordination chemistry of the tetradentate chelating ligand 1,3-bis[3-(2-pyridyl)pyrazol-1-yl]propane', by K. L. V. Mann, J. C. Jeffery, J. A. McCleverty and M. D. Ward submitted to Dalton Transactions for publication. ; #================================================================= data_/sun/sad _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C50 H64 Cl4 Fe2 N16 O20' _chemical_formula_weight 1462.67 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.714(6) _cell_length_b 11.095(2) _cell_length_c 14.910(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.03(2) _cell_angle_gamma 90.00 _cell_volume 3164.0(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method ? _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 0.712 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13083 _diffrn_reflns_av_R_equivalents 0.1080 _diffrn_reflns_av_sigmaI/netI 0.0874 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2786 _reflns_number_observed 1729 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 12 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+7.3203P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2774 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1178 _refine_ls_R_factor_obs 0.0597 _refine_ls_wR_factor_all 0.1171 _refine_ls_wR_factor_obs 0.0964 _refine_ls_goodness_of_fit_all 1.043 _refine_ls_goodness_of_fit_obs 1.124 _refine_ls_restrained_S_all 1.050 _refine_ls_restrained_S_obs 1.124 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.5000 0.48033(8) 0.2500 0.0246(3) Uani 1 d S . N11 N 0.5455(2) 0.3655(3) 0.1554(2) 0.0287(9) Uani 1 d . . C12 C 0.5802(2) 0.4304(4) 0.1040(3) 0.0265(11) Uani 1 d . . C13 C 0.6239(3) 0.3771(5) 0.0546(3) 0.0386(13) Uani 1 d . . H13 H 0.6481(3) 0.4251(5) 0.0198(3) 0.046 Uiso 1 calc R . C14 C 0.6312(3) 0.2539(5) 0.0571(3) 0.0432(14) Uani 1 d . . H14 H 0.6609(3) 0.2155(5) 0.0243(3) 0.052 Uiso 1 calc R . C15 C 0.5951(3) 0.1872(5) 0.1076(3) 0.0402(13) Uani 1 d . . H15 H 0.5991(3) 0.1018(5) 0.1094(3) 0.048 Uiso 1 calc R . C16 C 0.5529(3) 0.2451(4) 0.1559(3) 0.0366(12) Uani 1 d . . H16 H 0.5282(3) 0.1979(4) 0.1907(3) 0.044 Uiso 1 calc R . N21 N 0.5231(2) 0.6022(3) 0.1498(2) 0.0256(9) Uani 1 d . . N22 N 0.5167(2) 0.7219(3) 0.1305(2) 0.0286(9) Uani 1 d . . C23 C 0.5561(2) 0.7543(5) 0.0727(3) 0.0357(12) Uani 1 d . . H23 H 0.5598(2) 0.8332(5) 0.0495(3) 0.043 Uiso 1 calc R . C24 C 0.5898(3) 0.6542(4) 0.0530(3) 0.0356(13) Uani 1 d . . H24 H 0.6218(3) 0.6490(4) 0.0147(3) 0.043 Uiso 1 calc R . C25 C 0.5670(2) 0.5607(4) 0.1013(3) 0.0274(11) Uani 1 d . . C3 C 0.4662(2) 0.7952(4) 0.1652(3) 0.0334(12) Uani 1 d . . H3A H 0.4309(2) 0.7412(4) 0.1810(3) 0.040 Uiso 1 calc R . H3B H 0.4416(2) 0.8498(4) 0.1154(3) 0.040 Uiso 1 calc R . C4 C 0.5000 0.8701(6) 0.2500 0.039(2) Uani 1 d S . H4A H 0.4639 0.9228(6) 0.2655 0.047 Uiso 0.50 calc PR . H4B H 0.5361 0.9228(6) 0.2345 0.047 Uiso 0.50 calc PR . O200 O 0.39781(15) 0.4793(3) 0.1685(2) 0.0326(8) Uani 1 d . . C201 C 0.3475(2) 0.4106(4) 0.1683(3) 0.0291(11) Uani 1 d . . H201 H 0.3532(2) 0.3276(4) 0.1562(3) 0.035 Uiso 1 calc R . N202 N 0.2880(2) 0.4441(3) 0.1833(3) 0.0286(9) Uani 1 d . . C203 C 0.2765(3) 0.5699(5) 0.2028(4) 0.058(2) Uani 1 d . . H20A H 0.2464(16) 0.5747(5) 0.2462(19) 0.087 Uiso 1 calc R . H20B H 0.2540(17) 0.6113(9) 0.1453(6) 0.087 Uiso 1 calc R . H20C H 0.3215(3) 0.6085(10) 0.2302(23) 0.087 Uiso 1 calc R . C204 C 0.2301(3) 0.3600(5) 0.1787(4) 0.0456(14) Uani 1 d . . H20D H 0.1891(5) 0.3877(16) 0.1320(15) 0.068 Uiso 1 calc R . H20E H 0.2188(11) 0.3564(21) 0.2392(7) 0.068 Uiso 1 calc R . H20F H 0.2437(6) 0.2797(8) 0.1620(21) 0.068 Uiso 1 calc R . Cl1 Cl 0.32830(7) 0.03667(11) 0.08800(9) 0.0401(4) Uani 1 d . . O1 O 0.3614(2) 0.0859(4) 0.1758(3) 0.0786(14) Uani 1 d . . O2 O 0.2700(2) 0.1102(4) 0.0459(3) 0.088(2) Uani 1 d . . O3 O 0.3767(2) 0.0301(3) 0.0306(3) 0.0600(11) Uani 1 d . . O4 O 0.3053(2) -0.0830(3) 0.1021(3) 0.0733(13) Uani 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 Fe1 0.0264(5) 0.0253(5) 0.0231(5) 0.000 0.0081(4) 0.000 N11 0.032(2) 0.031(2) 0.021(2) -0.002(2) 0.001(2) 0.004(2) C12 0.024(3) 0.040(3) 0.013(2) 0.000(2) -0.002(2) 0.004(2) C13 0.038(3) 0.050(3) 0.029(3) -0.002(3) 0.011(2) 0.006(3) C14 0.035(3) 0.065(4) 0.029(3) -0.008(3) 0.007(3) 0.018(3) C15 0.051(3) 0.037(3) 0.029(3) -0.005(2) 0.003(3) 0.015(3) C16 0.046(3) 0.036(3) 0.027(3) -0.001(2) 0.006(2) 0.006(2) N21 0.030(2) 0.022(2) 0.024(2) 0.003(2) 0.004(2) -0.001(2) N22 0.031(2) 0.025(2) 0.028(2) 0.001(2) 0.004(2) -0.004(2) C23 0.040(3) 0.038(3) 0.028(3) 0.008(2) 0.005(2) -0.011(2) C24 0.044(3) 0.043(3) 0.023(3) -0.002(2) 0.013(2) -0.012(3) C25 0.024(3) 0.036(3) 0.021(3) 0.001(2) 0.003(2) -0.001(2) C3 0.037(3) 0.027(3) 0.035(3) 0.005(2) 0.006(2) 0.003(2) C4 0.050(5) 0.025(4) 0.044(5) 0.000 0.012(4) 0.000 O200 0.025(2) 0.040(2) 0.032(2) 0.006(2) 0.0052(14) -0.001(2) C201 0.034(3) 0.031(3) 0.021(3) -0.002(2) 0.005(2) 0.003(2) N202 0.022(2) 0.032(2) 0.030(2) 0.001(2) 0.003(2) -0.002(2) C203 0.041(3) 0.045(3) 0.090(5) -0.009(3) 0.020(3) 0.008(3) C204 0.040(3) 0.057(4) 0.040(3) 0.003(3) 0.011(3) -0.016(3) Cl1 0.0486(8) 0.0384(8) 0.0345(7) -0.0019(6) 0.0126(6) 0.0126(6) O1 0.091(3) 0.087(3) 0.047(3) -0.027(2) -0.003(2) 0.010(3) O2 0.088(3) 0.107(4) 0.067(3) 0.007(3) 0.015(3) 0.068(3) O3 0.078(3) 0.050(2) 0.069(3) 0.016(2) 0.050(2) 0.011(2) O4 0.081(3) 0.052(3) 0.103(4) -0.007(3) 0.054(3) -0.013(2) _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 Fe1 O200 2.085(3) 2_655 ? Fe1 O200 2.085(3) . ? Fe1 N21 2.144(4) 2_655 ? Fe1 N21 2.144(4) . ? Fe1 N11 2.242(4) 2_655 ? Fe1 N11 2.242(4) . ? N11 C16 1.344(5) . ? N11 C12 1.353(5) . ? C12 C13 1.392(6) . ? C12 C25 1.468(6) . ? C13 C14 1.375(7) . ? C14 C15 1.372(7) . ? C15 C16 1.383(6) . ? N21 C25 1.336(5) . ? N21 N22 1.359(5) . ? N22 C23 1.342(5) . ? N22 C3 1.472(5) . ? C23 C24 1.362(6) . ? C24 C25 1.398(6) . ? C3 C4 1.525(5) . ? C4 C3 1.525(5) 2_655 ? O200 C201 1.249(5) . ? C201 N202 1.300(5) . ? N202 C203 1.455(6) . ? N202 C204 1.463(5) . ? Cl1 O1 1.422(4) . ? Cl1 O2 1.425(4) . ? Cl1 O3 1.430(3) . ? Cl1 O4 1.434(4) . ? 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 O200 Fe1 O200 179.4(2) 2_655 . ? O200 Fe1 N21 86.35(13) 2_655 2_655 ? O200 Fe1 N21 94.04(13) . 2_655 ? O200 Fe1 N21 94.04(13) 2_655 . ? O200 Fe1 N21 86.35(13) . . ? N21 Fe1 N21 101.8(2) 2_655 . ? O200 Fe1 N11 96.19(12) 2_655 2_655 ? O200 Fe1 N11 83.46(12) . 2_655 ? N21 Fe1 N11 74.65(13) 2_655 2_655 ? N21 Fe1 N11 168.91(13) . 2_655 ? O200 Fe1 N11 83.45(12) 2_655 . ? O200 Fe1 N11 96.19(12) . . ? N21 Fe1 N11 168.91(13) 2_655 . ? N21 Fe1 N11 74.65(13) . . ? N11 Fe1 N11 110.8(2) 2_655 . ? C16 N11 C12 117.5(4) . . ? C16 N11 Fe1 128.4(3) . . ? C12 N11 Fe1 112.9(3) . . ? N11 C12 C13 122.5(4) . . ? N11 C12 C25 115.3(4) . . ? C13 C12 C25 122.2(4) . . ? C14 C13 C12 118.9(5) . . ? C15 C14 C13 119.1(5) . . ? C14 C15 C16 119.5(5) . . ? N11 C16 C15 122.5(5) . . ? C25 N21 N22 105.2(3) . . ? C25 N21 Fe1 115.8(3) . . ? N22 N21 Fe1 137.7(3) . . ? C23 N22 N21 111.0(4) . . ? C23 N22 C3 128.6(4) . . ? N21 N22 C3 120.1(4) . . ? N22 C23 C24 108.0(4) . . ? C23 C24 C25 105.1(4) . . ? N21 C25 C24 110.7(4) . . ? N21 C25 C12 117.3(4) . . ? C24 C25 C12 131.9(4) . . ? N22 C3 C4 113.3(3) . . ? C3 C4 C3 113.9(5) . 2_655 ? C201 O200 Fe1 131.2(3) . . ? O200 C201 N202 125.0(4) . . ? C201 N202 C203 120.0(4) . . ? C201 N202 C204 122.4(4) . . ? C203 N202 C204 117.6(4) . . ? O1 Cl1 O2 109.1(3) . . ? O1 Cl1 O3 110.2(3) . . ? O2 Cl1 O3 110.5(2) . . ? O1 Cl1 O4 108.1(3) . . ? O2 Cl1 O4 110.2(3) . . ? O3 Cl1 O4 108.7(2) . . ? _refine_diff_density_max 0.413 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.081 #=END data_/jade/sad _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C19 H18 B2 Cu F8 N6' _chemical_formula_weight 567.55 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 '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 'P 2(1) /n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.398(2) _cell_length_b 7.294(2) _cell_length_c 21.622(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.285(14) _cell_angle_gamma 90.00 _cell_volume 2179.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.730 _exptl_crystal_density_method ? _exptl_crystal_F_000 1140 _exptl_absorpt_coefficient_mu 1.092 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13248 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4966 _reflns_number_observed 3510 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+0.7956P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4966 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_obs 0.0413 _refine_ls_wR_factor_all 0.1035 _refine_ls_wR_factor_obs 0.0906 _refine_ls_goodness_of_fit_all 1.011 _refine_ls_goodness_of_fit_obs 1.067 _refine_ls_restrained_S_all 1.011 _refine_ls_restrained_S_obs 1.067 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.31792(2) 0.20910(5) 0.06209(2) 0.02070(11) Uani 1 d . . N11 N 0.4585(2) 0.2860(3) 0.08851(11) 0.0202(5) Uani 1 d . . C12 C 0.5022(2) 0.2742(4) 0.04080(13) 0.0199(6) Uani 1 d . . C13 C 0.5985(2) 0.3216(4) 0.05008(15) 0.0254(7) Uani 1 d . . H13 H 0.6275(2) 0.3133(4) 0.01573(15) 0.031 Uiso 1 calc R . C14 C 0.6518(2) 0.3817(4) 0.11069(15) 0.0273(7) Uani 1 d . . H14 H 0.7187(2) 0.4089(4) 0.11901(15) 0.033 Uiso 1 calc R . C15 C 0.6060(2) 0.4013(4) 0.15885(15) 0.0269(7) Uani 1 d . . H15 H 0.6405(2) 0.4463(4) 0.20015(15) 0.032 Uiso 1 calc R . C16 C 0.5097(2) 0.3545(4) 0.14576(14) 0.0243(6) Uani 1 d . . H16 H 0.4781(2) 0.3713(4) 0.17848(14) 0.029 Uiso 1 calc R . N21 N 0.3484(2) 0.1665(3) -0.02030(10) 0.0198(5) Uani 1 d . . N22 N 0.3034(2) 0.1037(3) -0.08025(11) 0.0220(5) Uani 1 d . . C23 C 0.3646(2) 0.1073(4) -0.11724(14) 0.0255(7) Uani 1 d . . H23 H 0.3497(2) 0.0700(4) -0.16102(14) 0.031 Uiso 1 calc R . C24 C 0.4525(2) 0.1742(4) -0.08090(14) 0.0258(7) Uani 1 d . . H24 H 0.5094(2) 0.1929(4) -0.09409(14) 0.031 Uiso 1 calc R . C25 C 0.4393(2) 0.2082(4) -0.02054(13) 0.0201(6) Uani 1 d . . C3 C 0.2053(2) 0.0274(4) -0.09643(14) 0.0250(6) Uani 1 d . . H3A H 0.1937(2) -0.0255(4) -0.05710(14) 0.030 Uiso 1 calc R . H3B H 0.2001(2) -0.0730(4) -0.12802(14) 0.030 Uiso 1 calc R . C4 C 0.1276(2) 0.1704(4) -0.12449(14) 0.0286(7) Uani 1 d . . H4A H 0.1383(2) 0.2198(4) -0.16459(14) 0.034 Uiso 1 calc R . H4B H 0.0636(2) 0.1094(4) -0.13617(14) 0.034 Uiso 1 calc R . C5 C 0.1252(2) 0.3298(4) -0.07940(13) 0.0253(7) Uani 1 d . . H5A H 0.1885(2) 0.3932(4) -0.06855(13) 0.030 Uiso 1 calc R . H5B H 0.0753(2) 0.4185(4) -0.10222(13) 0.030 Uiso 1 calc R . N61 N 0.1755(2) 0.2299(3) 0.03407(11) 0.0195(5) Uani 1 d . . N62 N 0.1045(2) 0.2738(3) -0.01981(11) 0.0222(5) Uani 1 d . . C63 C 0.0178(2) 0.2728(4) -0.00743(15) 0.0269(7) Uani 1 d . . H63 H -0.0429(2) 0.2978(4) -0.03758(15) 0.032 Uiso 1 calc R . C64 C 0.0326(2) 0.2294(4) 0.0563(2) 0.0268(7) Uani 1 d . . H64 H -0.0148(2) 0.2189(4) 0.0791(2) 0.032 Uiso 1 calc R . C65 C 0.1322(2) 0.2040(4) 0.08048(13) 0.0195(6) Uani 1 d . . N71 N 0.2912(2) 0.1567(3) 0.14675(11) 0.0189(5) Uani 1 d . . C72 C 0.1961(2) 0.1595(4) 0.14427(13) 0.0204(6) Uani 1 d . . C73 C 0.1640(2) 0.1224(4) 0.19755(14) 0.0247(6) Uani 1 d . . H73 H 0.0968(2) 0.1258(4) 0.19443(14) 0.030 Uiso 1 calc R . C74 C 0.2308(2) 0.0805(4) 0.25534(14) 0.0310(7) Uani 1 d . . H74 H 0.2106(2) 0.0592(4) 0.29292(14) 0.037 Uiso 1 calc R . C75 C 0.3276(2) 0.0701(4) 0.25774(14) 0.0297(7) Uani 1 d . . H75 H 0.3747(2) 0.0383(4) 0.29670(14) 0.036 Uiso 1 calc R . C76 C 0.3548(2) 0.1065(4) 0.20273(13) 0.0249(7) Uani 1 d . . H76 H 0.4212(2) 0.0958(4) 0.20434(13) 0.030 Uiso 1 calc R . B1 B 0.9176(3) 0.3154(5) 0.2296(2) 0.0257(8) Uani 1 d . . F1 F 0.9156(2) 0.4975(3) 0.24743(11) 0.0613(7) Uani 1 d . . F2 F 0.99344(15) 0.2296(4) 0.27261(11) 0.0619(7) Uani 1 d . . F3 F 0.9293(2) 0.3080(3) 0.16863(9) 0.0490(6) Uani 1 d . . F4 F 0.83039(13) 0.2334(3) 0.22967(9) 0.0413(5) Uani 1 d . . B2 B 0.2527(2) 0.7041(5) 0.0658(2) 0.0228(7) Uani 1 d . . F5 F 0.31046(13) 0.5547(3) 0.08895(10) 0.0414(5) Uani 1 d . . F6 F 0.19663(13) 0.6698(3) 0.00294(8) 0.0357(5) Uani 1 d . . F7 F 0.19258(13) 0.7404(3) 0.10458(8) 0.0377(5) Uani 1 d . . F8 F 0.31146(13) 0.8562(2) 0.06495(9) 0.0338(4) Uani 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 Cu1 0.0176(2) 0.0300(2) 0.0146(2) -0.0006(2) 0.00458(12) 0.0016(2) N11 0.0184(11) 0.0210(13) 0.0209(12) -0.0007(10) 0.0049(9) 0.0026(10) C12 0.0223(14) 0.0134(14) 0.0239(14) 0.0033(11) 0.0066(12) 0.0047(12) C13 0.025(2) 0.022(2) 0.033(2) 0.0056(12) 0.0131(13) 0.0005(13) C14 0.020(2) 0.020(2) 0.041(2) 0.0058(13) 0.0064(14) -0.0010(12) C15 0.023(2) 0.022(2) 0.030(2) -0.0033(13) -0.0017(13) -0.0010(13) C16 0.0234(15) 0.026(2) 0.0226(15) -0.0040(12) 0.0053(12) 0.0020(13) N21 0.0229(12) 0.0217(14) 0.0145(11) -0.0006(9) 0.0046(10) 0.0012(10) N22 0.0291(13) 0.0212(13) 0.0152(12) -0.0009(9) 0.0052(10) 0.0015(11) C23 0.041(2) 0.023(2) 0.0155(14) 0.0012(11) 0.0118(13) 0.0058(14) C24 0.033(2) 0.026(2) 0.0223(15) 0.0038(12) 0.0149(13) 0.0081(13) C25 0.0247(14) 0.0164(14) 0.0202(14) 0.0018(12) 0.0079(11) 0.0039(12) C3 0.029(2) 0.021(2) 0.0221(15) -0.0016(12) 0.0022(12) -0.0040(13) C4 0.030(2) 0.031(2) 0.0203(15) 0.0022(12) 0.0010(13) -0.0009(14) C5 0.028(2) 0.024(2) 0.0200(14) 0.0061(11) 0.0013(12) 0.0007(13) N61 0.0182(11) 0.0198(13) 0.0189(11) 0.0014(9) 0.0027(9) 0.0014(10) N62 0.0201(12) 0.0223(13) 0.0219(12) 0.0032(10) 0.0020(10) 0.0029(10) C63 0.0184(14) 0.028(2) 0.033(2) 0.0010(13) 0.0039(12) 0.0001(13) C64 0.0198(14) 0.027(2) 0.035(2) -0.0004(13) 0.0104(13) 0.0022(13) C65 0.0193(13) 0.0171(14) 0.0236(14) -0.0012(12) 0.0086(11) 0.0005(12) N71 0.0220(12) 0.0164(13) 0.0184(12) 0.0003(9) 0.0060(10) 0.0022(10) C72 0.0269(15) 0.0146(14) 0.0211(14) -0.0027(11) 0.0092(12) 0.0018(12) C73 0.029(2) 0.022(2) 0.027(2) -0.0024(12) 0.0140(13) -0.0040(13) C74 0.050(2) 0.025(2) 0.021(2) -0.0006(13) 0.0158(15) -0.007(2) C75 0.042(2) 0.024(2) 0.0203(15) 0.0041(12) 0.0042(14) 0.0007(14) C76 0.027(2) 0.024(2) 0.0214(15) 0.0006(12) 0.0016(12) 0.0027(13) B1 0.029(2) 0.032(2) 0.017(2) 0.0005(14) 0.0073(14) -0.001(2) F1 0.072(2) 0.0450(15) 0.072(2) -0.0217(12) 0.0286(13) -0.0095(12) F2 0.0338(12) 0.092(2) 0.0566(14) 0.0376(13) 0.0080(10) 0.0085(12) F3 0.0649(15) 0.062(2) 0.0267(10) 0.0013(10) 0.0238(10) -0.0069(12) F4 0.0308(10) 0.0597(15) 0.0323(10) 0.0025(9) 0.0073(8) -0.0119(9) B2 0.024(2) 0.024(2) 0.021(2) 0.0008(14) 0.0062(13) -0.0013(15) F5 0.0352(11) 0.0227(11) 0.0600(13) 0.0020(9) 0.0029(9) 0.0071(8) F6 0.0387(11) 0.0414(13) 0.0255(9) -0.0055(8) 0.0065(8) -0.0038(9) F7 0.0301(10) 0.0572(15) 0.0284(10) 0.0015(9) 0.0128(8) 0.0034(9) F8 0.0393(11) 0.0226(10) 0.0427(11) -0.0051(8) 0.0169(9) -0.0044(8) _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 N61 1.975(2) . ? Cu1 N21 1.975(2) . ? Cu1 N71 2.010(2) . ? Cu1 N11 2.022(2) . ? N11 C16 1.347(4) . ? N11 C12 1.353(3) . ? C12 C13 1.389(4) . ? C12 C25 1.462(4) . ? C13 C14 1.390(4) . ? C14 C15 1.386(4) . ? C15 C16 1.379(4) . ? N21 C25 1.345(3) . ? N21 N22 1.356(3) . ? N22 C23 1.346(4) . ? N22 C3 1.466(4) . ? C23 C24 1.378(4) . ? C24 C25 1.392(4) . ? C3 C4 1.526(4) . ? C4 C5 1.524(4) . ? C5 N62 1.460(4) . ? N61 C65 1.335(3) . ? N61 N62 1.355(3) . ? N62 C63 1.348(4) . ? C63 C64 1.371(4) . ? C64 C65 1.394(4) . ? C65 C72 1.464(4) . ? N71 C76 1.348(3) . ? N71 C72 1.355(4) . ? C72 C73 1.383(4) . ? C73 C74 1.381(4) . ? C74 C75 1.382(4) . ? C75 C76 1.378(4) . ? B1 F2 1.371(4) . ? B1 F3 1.377(4) . ? B1 F1 1.385(4) . ? B1 F4 1.392(4) . ? B2 F5 1.377(4) . ? B2 F7 1.389(4) . ? B2 F6 1.395(4) . ? B2 F8 1.399(4) . ? 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 N61 Cu1 N21 102.12(9) . . ? N61 Cu1 N71 81.16(9) . . ? N21 Cu1 N71 159.93(9) . . ? N61 Cu1 N11 159.47(10) . . ? N21 Cu1 N11 80.81(9) . . ? N71 Cu1 N11 103.16(9) . . ? C16 N11 C12 118.2(2) . . ? C16 N11 Cu1 127.5(2) . . ? C12 N11 Cu1 114.2(2) . . ? N11 C12 C13 122.2(3) . . ? N11 C12 C25 114.3(2) . . ? C13 C12 C25 123.5(3) . . ? C12 C13 C14 118.6(3) . . ? C15 C14 C13 119.2(3) . . ? C16 C15 C14 118.8(3) . . ? N11 C16 C15 122.7(3) . . ? C25 N21 N22 106.1(2) . . ? C25 N21 Cu1 115.5(2) . . ? N22 N21 Cu1 138.4(2) . . ? C23 N22 N21 110.1(2) . . ? C23 N22 C3 127.8(2) . . ? N21 N22 C3 121.8(2) . . ? N22 C23 C24 108.5(2) . . ? C23 C24 C25 104.7(3) . . ? N21 C25 C24 110.6(3) . . ? N21 C25 C12 115.2(2) . . ? C24 C25 C12 134.2(3) . . ? N22 C3 C4 112.7(2) . . ? C5 C4 C3 114.4(2) . . ? N62 C5 C4 113.5(2) . . ? C65 N61 N62 106.4(2) . . ? C65 N61 Cu1 115.0(2) . . ? N62 N61 Cu1 138.6(2) . . ? C63 N62 N61 110.2(2) . . ? C63 N62 C5 127.3(2) . . ? N61 N62 C5 122.3(2) . . ? N62 C63 C64 108.0(3) . . ? C63 C64 C65 105.1(3) . . ? N61 C65 C64 110.3(2) . . ? N61 C65 C72 116.0(2) . . ? C64 C65 C72 133.7(3) . . ? C76 N71 C72 117.7(2) . . ? C76 N71 Cu1 127.9(2) . . ? C72 N71 Cu1 114.2(2) . . ? N71 C72 C73 122.3(3) . . ? N71 C72 C65 113.7(2) . . ? C73 C72 C65 124.0(3) . . ? C74 C73 C72 119.1(3) . . ? C73 C74 C75 119.1(3) . . ? C76 C75 C74 119.0(3) . . ? N71 C76 C75 122.8(3) . . ? F2 B1 F3 110.1(3) . . ? F2 B1 F1 108.9(3) . . ? F3 B1 F1 108.8(3) . . ? F2 B1 F4 110.5(3) . . ? F3 B1 F4 109.7(3) . . ? F1 B1 F4 108.8(3) . . ? F5 B2 F7 110.3(3) . . ? F5 B2 F6 109.8(3) . . ? F7 B2 F6 109.5(2) . . ? F5 B2 F8 109.0(2) . . ? F7 B2 F8 109.7(3) . . ? F6 B2 F8 108.4(2) . . ? _refine_diff_density_max 0.688 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.080 #=END data_sad _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C58 H61 Cl4 N18 O22.50 Zn3' _chemical_formula_weight 1708.16 _chemical_melting_point ? _chemical_compound_source ? 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' 'Zn' 'Zn' 0.2839 1.4301 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'Pa-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' '-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 23.981(4) _cell_length_b 23.981(5) _cell_length_c 23.981(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13790.7(46) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.645 _exptl_crystal_density_method ? _exptl_crystal_F_000 6984 _exptl_absorpt_coefficient_mu 1.281 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54976 _diffrn_reflns_av_R_equivalents 0.1461 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 22.48 _reflns_number_total 3022 _reflns_number_observed 2226 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+76.0600P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3017 _refine_ls_number_parameters 318 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0903 _refine_ls_R_factor_obs 0.0592 _refine_ls_wR_factor_all 0.1414 _refine_ls_wR_factor_obs 0.1193 _refine_ls_goodness_of_fit_all 1.088 _refine_ls_goodness_of_fit_obs 1.096 _refine_ls_restrained_S_all 1.092 _refine_ls_restrained_S_obs 1.094 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn1 Zn 0.80087(3) 0.23057(3) 0.10663(3) 0.0405(3) Uani 1 d . . N11 N 0.8601(2) 0.1677(2) 0.0916(2) 0.0438(15) Uani 1 d . . C12 C 0.8553(3) 0.1221(3) 0.1249(3) 0.043(2) Uani 1 d . . C13 C 0.8949(3) 0.0809(3) 0.1253(3) 0.057(2) Uani 1 d . . H13 H 0.8909(3) 0.0497(3) 0.1493(3) 0.068 Uiso 1 calc R . C14 C 0.9400(4) 0.0852(4) 0.0911(4) 0.073(3) Uani 1 d . . H14 H 0.9675(4) 0.0567(4) 0.0907(4) 0.088 Uiso 1 calc R . C15 C 0.9457(4) 0.1313(4) 0.0568(4) 0.071(3) Uani 1 d . . H15 H 0.9772(4) 0.1352(4) 0.0331(4) 0.085 Uiso 1 calc R . C16 C 0.9042(3) 0.1717(3) 0.0580(3) 0.052(2) Uani 1 d . . H16 H 0.9073(3) 0.2032(3) 0.0341(3) 0.063 Uiso 1 calc R . N21 N 0.7700(2) 0.1635(2) 0.1548(2) 0.0438(15) Uani 1 d . . N22 N 0.7276(2) 0.1531(2) 0.1901(3) 0.048(2) Uani 1 d . . C23 C 0.7355(3) 0.1043(3) 0.2168(3) 0.051(2) Uani 1 d . . H23 H 0.7108(3) 0.0882(3) 0.2432(3) 0.061 Uiso 1 calc R . C24 C 0.7851(3) 0.0820(3) 0.1992(3) 0.047(2) Uani 1 d . . H24 H 0.8020(3) 0.0481(3) 0.2109(3) 0.057 Uiso 1 calc R . C25 C 0.8054(3) 0.1206(3) 0.1601(3) 0.043(2) Uani 1 d . . C3 C 0.6793(3) 0.1904(3) 0.1901(3) 0.050(2) Uani 1 d . . H3A H 0.6920(3) 0.2290(3) 0.1828(3) 0.061 Uiso 1 calc R . H3B H 0.6616(3) 0.1896(3) 0.2274(3) 0.061 Uiso 1 calc R . C4 C 0.6365(3) 0.1737(3) 0.1463(4) 0.059(2) Uani 1 d . . H4A H 0.6202(3) 0.1374(3) 0.1572(4) 0.071 Uiso 1 calc R . H4B H 0.6060(3) 0.2016(3) 0.1466(4) 0.071 Uiso 1 calc R . C5 C 0.6587(3) 0.1689(3) 0.0870(3) 0.059(2) Uani 1 d . . H5A H 0.6919(3) 0.1444(3) 0.0874(3) 0.070 Uiso 1 calc R . H5B H 0.6300(3) 0.1505(3) 0.0637(3) 0.070 Uiso 1 calc R . N61 N 0.7256(2) 0.2433(2) 0.0639(2) 0.046(2) Uani 1 d . . N62 N 0.6739(3) 0.2218(3) 0.0608(3) 0.055(2) Uani 1 d . . C63 C 0.6411(3) 0.2535(4) 0.0283(3) 0.070(3) Uani 1 d . . H63 H 0.6030(3) 0.2466(4) 0.0198(3) 0.084 Uiso 1 calc R . C64 C 0.6722(3) 0.2976(4) 0.0095(3) 0.067(3) Uani 1 d . . H64 H 0.6605(3) 0.3269(4) -0.0144(3) 0.081 Uiso 1 calc R . C65 C 0.7245(3) 0.2904(3) 0.0329(3) 0.048(2) Uani 1 d . . N71 N 0.8207(3) 0.2980(2) 0.0516(2) 0.0452(15) Uani 1 d . . C72 C 0.7759(3) 0.3216(3) 0.0266(3) 0.049(2) Uani 1 d . . C73 C 0.7813(4) 0.3709(3) -0.0030(3) 0.058(2) Uani 1 d . . H73 H 0.7494(4) 0.3874(3) -0.0198(3) 0.069 Uiso 1 calc R . C74 C 0.8316(4) 0.3959(3) -0.0082(3) 0.066(2) Uani 1 d . . H74 H 0.8354(4) 0.4297(3) -0.0285(3) 0.079 Uiso 1 calc R . C75 C 0.8774(4) 0.3714(4) 0.0164(3) 0.062(2) Uani 1 d . . H75 H 0.9134(4) 0.3876(4) 0.0127(3) 0.074 Uiso 1 calc R . C76 C 0.8701(3) 0.3229(3) 0.0467(3) 0.051(2) Uani 1 d . . H76 H 0.9014(3) 0.3067(3) 0.0648(3) 0.062 Uiso 1 calc R . Cl1 Cl 0.63567(8) 0.36433(8) -0.13567(8) 0.0442(8) Uani 1 d S . O1 O 0.6032(4) 0.3968(4) -0.1032(4) 0.194(9) Uani 1 d S . O2 O 0.6145(4) 0.3116(3) -0.1266(4) 0.135(4) Uani 1 d . . Cl2 Cl 0.74251(10) 0.05763(8) 0.01362(8) 0.0578(6) Uani 1 d . . O5 O 0.6939(4) 0.0431(5) -0.0125(4) 0.162(4) Uani 1 d . . O6 O 0.7529(4) 0.1118(3) 0.0003(3) 0.137(4) Uani 1 d . . O7 O 0.7822(4) 0.0208(4) -0.0085(3) 0.149(4) Uani 1 d . . O8 O 0.7355(3) 0.0511(2) 0.0716(2) 0.088(2) Uani 1 d . . C111 C 0.8089(3) 0.3089(3) 0.1911(3) 0.036(3) Uani 1 d S . O9 O 0.8347(2) 0.2656(2) 0.1735(2) 0.0414(12) Uani 1 d . . O11 O 0.5793(8) 0.0624(9) -0.0186(8) 0.343(11) Uani 1 d U . O10 O 0.5000 0.0000 0.0000 0.366(27) Uani 1 d SU . 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 0.0385(5) 0.0374(5) 0.0456(5) -0.0036(4) -0.0046(4) 0.0031(4) N11 0.040(4) 0.047(4) 0.045(4) -0.007(3) 0.000(3) 0.002(3) C12 0.049(5) 0.030(4) 0.049(5) -0.007(4) -0.012(4) 0.003(4) C13 0.056(5) 0.052(5) 0.062(5) 0.007(4) 0.004(4) 0.012(4) C14 0.076(7) 0.062(6) 0.081(7) 0.002(5) 0.003(5) 0.030(5) C15 0.063(6) 0.083(7) 0.067(6) -0.005(5) 0.014(5) 0.020(5) C16 0.054(5) 0.049(5) 0.053(5) -0.002(4) 0.000(4) 0.009(4) N21 0.040(4) 0.032(3) 0.059(4) -0.003(3) 0.001(3) -0.001(3) N22 0.048(4) 0.037(4) 0.058(4) -0.001(3) 0.001(3) -0.009(3) C23 0.064(6) 0.032(4) 0.058(5) -0.003(4) 0.003(4) -0.005(4) C24 0.056(5) 0.037(4) 0.048(5) -0.004(4) -0.008(4) -0.003(4) C25 0.040(4) 0.043(4) 0.045(4) -0.008(4) -0.006(4) -0.004(4) C3 0.046(5) 0.041(4) 0.064(5) -0.006(4) 0.008(4) 0.000(4) C4 0.035(4) 0.054(5) 0.088(7) -0.004(5) 0.003(4) -0.006(4) C5 0.037(4) 0.059(5) 0.080(6) -0.020(5) -0.010(4) -0.008(4) N61 0.040(4) 0.045(4) 0.052(4) -0.014(3) -0.006(3) 0.005(3) N62 0.040(4) 0.072(5) 0.054(4) -0.013(4) -0.001(3) 0.005(4) C63 0.038(5) 0.122(8) 0.051(5) 0.004(6) -0.012(4) 0.013(6) C64 0.052(5) 0.104(8) 0.046(5) 0.011(5) -0.003(4) 0.025(5) C65 0.058(5) 0.057(5) 0.029(4) -0.005(4) 0.001(4) 0.017(4) N71 0.050(4) 0.041(4) 0.044(4) -0.007(3) 0.001(3) 0.001(3) C72 0.064(5) 0.052(5) 0.032(4) -0.010(4) -0.003(4) 0.014(4) C73 0.092(7) 0.042(5) 0.040(5) -0.006(4) -0.013(4) 0.012(5) C74 0.102(8) 0.041(5) 0.054(5) 0.003(4) -0.002(5) -0.013(5) C75 0.066(6) 0.066(6) 0.053(5) -0.006(5) 0.003(5) -0.008(5) C76 0.062(6) 0.046(5) 0.047(5) 0.004(4) 0.001(4) -0.001(4) Cl1 0.0442(8) 0.0442(8) 0.0442(8) 0.0058(9) -0.0058(9) -0.0058(9) O1 0.194(9) 0.194(9) 0.194(9) -0.063(7) 0.063(7) 0.063(7) O2 0.184(8) 0.074(5) 0.149(7) 0.042(5) -0.095(7) -0.060(5) Cl2 0.086(2) 0.0505(12) 0.0373(11) 0.0033(9) 0.0069(11) 0.0105(11) O5 0.143(8) 0.244(12) 0.100(7) -0.042(7) -0.016(6) -0.051(8) O6 0.219(9) 0.064(5) 0.126(6) 0.032(4) 0.094(7) 0.013(5) O7 0.238(10) 0.148(7) 0.061(4) 0.023(5) 0.036(5) 0.132(7) O8 0.145(6) 0.076(4) 0.042(3) 0.008(3) 0.024(4) 0.011(4) C111 0.036(3) 0.036(3) 0.036(3) 0.004(3) 0.004(3) -0.004(3) O9 0.045(3) 0.035(3) 0.044(3) -0.005(2) -0.007(2) 0.004(2) O11 0.383(25) 0.389(28) 0.256(18) -0.019(18) -0.070(20) 0.152(20) O10 0.366(27) 0.366(27) 0.366(27) -0.089(33) 0.089(33) -0.089(33) _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 O9 1.984(4) . ? Zn1 N61 2.098(6) . ? Zn1 N11 2.102(6) . ? Zn1 N21 2.115(6) . ? Zn1 N71 2.141(6) . ? N11 C16 1.333(9) . ? N11 C12 1.360(9) . ? C12 C13 1.371(10) . ? C12 C25 1.464(10) . ? C13 C14 1.362(11) . ? C14 C15 1.383(12) . ? C15 C16 1.391(11) . ? N21 C25 1.338(8) . ? N21 N22 1.345(8) . ? N22 C23 1.345(9) . ? N22 C3 1.464(9) . ? C23 C24 1.372(10) . ? C24 C25 1.405(10) . ? C3 C4 1.523(10) . ? C4 C5 1.523(11) . ? C5 N62 1.464(10) . ? N61 N62 1.345(8) . ? N61 C65 1.352(9) . ? N62 C63 1.342(10) . ? C63 C64 1.370(12) . ? C64 C65 1.383(10) . ? C65 C72 1.451(10) . ? N71 C76 1.330(9) . ? N71 C72 1.356(9) . ? C72 C73 1.385(10) . ? C73 C74 1.353(11) . ? C74 C75 1.378(11) . ? C75 C76 1.382(10) . ? Cl1 O1 1.348(15) . ? Cl1 O2 1.379(6) . ? Cl1 O2 1.379(6) 7_564 ? Cl1 O2 1.379(6) 10_655 ? Cl2 O6 1.361(7) . ? Cl2 O5 1.369(9) . ? Cl2 O7 1.404(7) . ? Cl2 O8 1.409(5) . ? C111 O9 1.280(4) . ? C111 O9 1.280(4) 8_645 ? C111 O9 1.280(4) 11_556 ? 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 O9 Zn1 N61 133.2(2) . . ? O9 Zn1 N11 99.6(2) . . ? N61 Zn1 N11 127.0(2) . . ? O9 Zn1 N21 91.3(2) . . ? N61 Zn1 N21 94.4(2) . . ? N11 Zn1 N21 77.6(2) . . ? O9 Zn1 N71 95.0(2) . . ? N61 Zn1 N71 77.3(2) . . ? N11 Zn1 N71 106.6(2) . . ? N21 Zn1 N71 171.7(2) . . ? C16 N11 C12 118.8(6) . . ? C16 N11 Zn1 126.0(5) . . ? C12 N11 Zn1 114.7(5) . . ? N11 C12 C13 121.6(7) . . ? N11 C12 C25 115.3(6) . . ? C13 C12 C25 123.0(7) . . ? C14 C13 C12 119.5(8) . . ? C13 C14 C15 119.8(8) . . ? C14 C15 C16 118.3(8) . . ? N11 C16 C15 122.0(8) . . ? C25 N21 N22 106.1(6) . . ? C25 N21 Zn1 114.4(5) . . ? N22 N21 Zn1 138.5(5) . . ? N21 N22 C23 110.8(6) . . ? N21 N22 C3 119.0(6) . . ? C23 N22 C3 129.8(6) . . ? N22 C23 C24 108.3(7) . . ? C23 C24 C25 104.3(7) . . ? N21 C25 C24 110.5(6) . . ? N21 C25 C12 116.4(6) . . ? C24 C25 C12 133.1(7) . . ? N22 C3 C4 111.9(6) . . ? C5 C4 C3 115.4(6) . . ? N62 C5 C4 115.0(6) . . ? N62 N61 C65 105.7(6) . . ? N62 N61 Zn1 139.9(5) . . ? C65 N61 Zn1 114.0(5) . . ? C63 N62 N61 110.9(7) . . ? C63 N62 C5 126.5(7) . . ? N61 N62 C5 122.5(6) . . ? N62 C63 C64 107.9(7) . . ? C63 C64 C65 105.4(8) . . ? N61 C65 C64 110.2(8) . . ? N61 C65 C72 118.1(7) . . ? C64 C65 C72 131.5(8) . . ? C76 N71 C72 118.6(7) . . ? C76 N71 Zn1 126.2(5) . . ? C72 N71 Zn1 114.3(5) . . ? N71 C72 C73 120.6(8) . . ? N71 C72 C65 114.3(7) . . ? C73 C72 C65 125.0(8) . . ? C74 C73 C72 120.5(8) . . ? C73 C74 C75 118.9(8) . . ? C74 C75 C76 118.8(8) . . ? N71 C76 C75 122.5(8) . . ? O1 Cl1 O2 103.0(5) . . ? O1 Cl1 O2 103.0(5) . 7_564 ? O2 Cl1 O2 115.1(3) . 7_564 ? O1 Cl1 O2 103.0(5) . 10_655 ? O2 Cl1 O2 115.1(3) . 10_655 ? O2 Cl1 O2 115.1(3) 7_564 10_655 ? O6 Cl2 O5 107.0(7) . . ? O6 Cl2 O7 112.9(5) . . ? O5 Cl2 O7 104.1(6) . . ? O6 Cl2 O8 111.0(4) . . ? O5 Cl2 O8 108.8(5) . . ? O7 Cl2 O8 112.6(4) . . ? O9 C111 O9 120.000(1) . 8_645 ? O9 C111 O9 120.000(2) . 11_556 ? O9 C111 O9 120.000(1) 8_645 11_556 ? C111 O9 Zn1 114.3(3) . . ? _refine_diff_density_max 0.623 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.073 #=END data_/moon/j _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C21 H21 Ag N8 O3' _chemical_formula_weight 541.33 _chemical_melting_point ? _chemical_compound_source ? 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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 2(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 6.9549(12) _cell_length_b 15.977(3) _cell_length_c 19.698(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2188.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method ? _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.963 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14087 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4970 _reflns_number_observed 3994 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0263P)^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 ? _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 0.01(2) _refine_ls_number_reflns 4970 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0493 _refine_ls_R_factor_obs 0.0315 _refine_ls_wR_factor_all 0.0606 _refine_ls_wR_factor_obs 0.0552 _refine_ls_goodness_of_fit_all 0.949 _refine_ls_goodness_of_fit_obs 0.971 _refine_ls_restrained_S_all 0.949 _refine_ls_restrained_S_obs 0.971 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ag1 Ag 0.38123(4) 0.27727(2) 0.025238(12) 0.03175(7) Uani 1 d . . N11 N 0.4061(4) 0.2232(2) 0.13152(12) 0.0229(6) Uani 1 d . . C12 C 0.3623(5) 0.2738(2) 0.18449(14) 0.0215(6) Uani 1 d . . C13 C 0.3602(5) 0.2451(2) 0.25084(15) 0.0275(8) Uani 1 d . . H13 H 0.3317(5) 0.2823(2) 0.28710(15) 0.033 Uiso 1 calc R . C14 C 0.4001(6) 0.1618(2) 0.2638(2) 0.0314(8) Uani 1 d . . H14 H 0.3982(6) 0.1409(2) 0.3089(2) 0.038 Uiso 1 calc R . C15 C 0.4424(5) 0.1098(2) 0.2102(2) 0.0311(8) Uani 1 d . . H15 H 0.4709(5) 0.0523(2) 0.2177(2) 0.037 Uiso 1 calc R . C16 C 0.4428(4) 0.1424(2) 0.1449(2) 0.0251(8) Uani 1 d . . H16 H 0.4703(4) 0.1059(2) 0.1081(2) 0.030 Uiso 1 calc R . N21 N 0.2808(4) 0.38192(15) 0.10344(13) 0.0218(6) Uani 1 d . . N22 N 0.2407(4) 0.4649(2) 0.10485(13) 0.0257(6) Uani 1 d . . C23 C 0.2495(5) 0.4953(2) 0.1683(2) 0.0302(8) Uani 1 d . . H23 H 0.2272(5) 0.5516(2) 0.1815(2) 0.036 Uiso 1 calc R . C24 C 0.2962(5) 0.4307(2) 0.2103(2) 0.0283(8) Uani 1 d . . H24 H 0.3124(5) 0.4326(2) 0.2582(2) 0.034 Uiso 1 calc R . C25 C 0.3151(4) 0.3608(2) 0.1679(2) 0.0215(7) Uani 1 d . . C3 C 0.1910(5) 0.5101(2) 0.04238(15) 0.0300(8) Uani 1 d . . H3A H 0.0725(5) 0.5431(2) 0.05007(15) 0.036 Uiso 1 calc R . H3B H 0.1646(5) 0.4692(2) 0.00578(15) 0.036 Uiso 1 calc R . C4 C 0.3523(5) 0.5688(2) 0.0198(2) 0.0368(8) Uani 1 d . . H4A H 0.3053(5) 0.6034(2) -0.0185(2) 0.044 Uiso 1 calc R . H4B H 0.3838(5) 0.6071(2) 0.0577(2) 0.044 Uiso 1 calc R . C5 C 0.5331(5) 0.5244(2) -0.0020(2) 0.0372(9) Uani 1 d . . H5A H 0.6345(5) 0.5664(2) -0.0110(2) 0.045 Uiso 1 calc R . H5B H 0.5780(5) 0.4881(2) 0.0355(2) 0.045 Uiso 1 calc R . N61 N 0.4744(4) 0.3898(2) -0.05727(13) 0.0278(6) Uani 1 d . . N62 N 0.5059(4) 0.4734(2) -0.06268(14) 0.0308(7) Uani 1 d . . C63 C 0.4935(5) 0.4991(3) -0.1275(2) 0.0388(9) Uani 1 d . . H63 H 0.5085(5) 0.5550(3) -0.1432(2) 0.047 Uiso 1 calc R . C64 C 0.4556(5) 0.4309(2) -0.1664(2) 0.0387(9) Uani 1 d . . H64 H 0.4417(5) 0.4290(2) -0.2144(2) 0.046 Uiso 1 calc R . C65 C 0.4413(5) 0.3637(2) -0.1207(2) 0.0296(8) Uani 1 d . . N71 N 0.3642(4) 0.2255(2) -0.07937(12) 0.0276(5) Uani 1 d . . C72 C 0.3948(5) 0.2751(3) -0.13366(14) 0.0279(7) Uani 1 d . . C73 C 0.3774(6) 0.2445(2) -0.1996(2) 0.0369(10) Uani 1 d . . H73 H 0.3972(6) 0.2803(2) -0.2374(2) 0.044 Uiso 1 calc R . C74 C 0.3307(5) 0.1613(3) -0.2090(2) 0.0442(11) Uani 1 d . . H74 H 0.3164(5) 0.1395(3) -0.2536(2) 0.053 Uiso 1 calc R . C75 C 0.3052(5) 0.1105(3) -0.1540(2) 0.0436(10) Uani 1 d . . H75 H 0.2760(5) 0.0529(3) -0.1597(2) 0.052 Uiso 1 calc R . C76 C 0.3226(5) 0.1446(2) -0.0898(2) 0.0335(8) Uani 1 d . . H76 H 0.3042(5) 0.1093(2) -0.0516(2) 0.040 Uiso 1 calc R . N100 N -0.0567(4) 0.7049(2) 0.11517(14) 0.0340(8) Uani 1 d . . O101 O -0.1707(4) 0.6538(2) 0.08819(13) 0.0525(8) Uani 1 d . . O102 O 0.0804(4) 0.6777(2) 0.14946(12) 0.0471(7) Uani 1 d . . O103 O -0.0777(4) 0.7816(2) 0.10742(13) 0.0539(7) Uani 1 d . . N200 N 0.4804(5) -0.0650(2) 0.1175(2) 0.0577(10) Uani 1 d . . C201 C 0.4584(5) -0.1302(2) 0.0977(2) 0.0339(8) Uani 1 d . . C202 C 0.4289(5) -0.2146(2) 0.0729(2) 0.0386(9) Uani 1 d . . H20A H 0.5524(7) -0.2440(5) 0.0714(10) 0.058 Uiso 1 calc R . H20B H 0.3734(29) -0.2125(2) 0.0272(5) 0.058 Uiso 1 calc R . H20C H 0.3409(25) -0.2443(5) 0.1034(6) 0.058 Uiso 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 Ag1 0.04690(15) 0.02761(11) 0.02073(10) -0.00033(12) 0.00066(13) -0.00089(14) N11 0.0197(15) 0.0248(12) 0.0243(12) -0.0035(13) -0.0022(11) 0.002(2) C12 0.015(2) 0.0219(14) 0.028(2) -0.0036(14) -0.0006(14) 0.000(2) C13 0.026(2) 0.031(2) 0.025(2) -0.0020(12) 0.001(2) 0.0000(15) C14 0.033(2) 0.033(2) 0.028(2) 0.0064(14) 0.001(2) -0.001(2) C15 0.033(2) 0.023(2) 0.037(2) 0.0065(15) 0.000(2) 0.0038(15) C16 0.027(2) 0.022(2) 0.026(2) -0.0028(13) -0.0009(14) 0.0026(14) N21 0.025(2) 0.0158(13) 0.0251(14) -0.0017(11) 0.0006(11) -0.0012(11) N22 0.031(2) 0.0170(14) 0.029(2) -0.0004(11) 0.0001(13) 0.0011(12) C23 0.042(2) 0.021(2) 0.028(2) -0.0052(14) 0.003(2) -0.001(2) C24 0.036(2) 0.025(2) 0.024(2) -0.0042(14) 0.0011(15) -0.0023(15) C25 0.020(2) 0.022(2) 0.022(2) -0.0038(13) 0.0034(13) -0.0030(13) C3 0.037(2) 0.024(2) 0.029(2) 0.0037(13) -0.0016(14) 0.0062(15) C4 0.055(3) 0.0196(14) 0.035(2) 0.0032(15) -0.004(2) 0.000(2) C5 0.035(2) 0.036(2) 0.040(2) 0.007(2) 0.000(2) -0.008(2) N61 0.025(2) 0.032(2) 0.0265(15) 0.0044(12) 0.0025(12) 0.0027(13) N62 0.028(2) 0.031(2) 0.033(2) 0.0083(13) 0.0039(13) -0.0022(13) C63 0.032(2) 0.047(2) 0.037(2) 0.016(2) 0.002(2) -0.001(2) C64 0.034(2) 0.054(2) 0.028(2) 0.015(2) 0.001(2) 0.003(2) C65 0.020(2) 0.043(2) 0.025(2) 0.0047(15) 0.0028(14) 0.006(2) N71 0.0262(15) 0.0290(13) 0.0277(13) -0.0035(15) 0.0012(13) 0.000(2) C72 0.017(2) 0.046(2) 0.0214(15) 0.002(2) 0.0033(14) 0.004(2) C73 0.025(2) 0.059(3) 0.027(2) -0.002(2) 0.003(2) 0.011(2) C74 0.029(2) 0.074(3) 0.029(2) -0.022(2) -0.003(2) 0.005(2) C75 0.028(2) 0.049(2) 0.053(3) -0.016(2) -0.001(2) -0.002(2) C76 0.027(2) 0.039(2) 0.035(2) -0.005(2) -0.001(2) 0.001(2) N100 0.036(2) 0.041(2) 0.025(2) 0.0010(13) 0.0070(13) 0.0081(15) O101 0.049(2) 0.062(2) 0.046(2) -0.0117(14) 0.0047(14) -0.0042(15) O102 0.054(2) 0.050(2) 0.0375(14) -0.0007(12) -0.0112(13) 0.0238(14) O103 0.057(2) 0.0352(14) 0.070(2) 0.0113(14) 0.0050(14) 0.014(2) N200 0.063(3) 0.036(2) 0.074(3) -0.014(2) -0.001(2) 0.005(2) C201 0.034(2) 0.034(2) 0.033(2) 0.003(2) 0.000(2) 0.008(2) C202 0.041(2) 0.033(2) 0.043(2) -0.004(2) -0.005(2) 0.001(2) _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 Ag1 N71 2.223(2) . ? Ag1 N11 2.271(3) . ? Ag1 N21 2.378(2) . ? Ag1 N61 2.508(3) . ? N11 C16 1.343(4) . ? N11 C12 1.354(4) . ? C12 C13 1.385(4) . ? C12 C25 1.466(5) . ? C13 C14 1.384(4) . ? C14 C15 1.376(4) . ? C15 C16 1.387(4) . ? N21 C25 1.335(4) . ? N21 N22 1.355(3) . ? N22 C23 1.342(4) . ? N22 C3 1.468(4) . ? C23 C24 1.363(4) . ? C24 C25 1.400(4) . ? C3 C4 1.528(5) . ? C4 C5 1.507(5) . ? C5 N62 1.459(4) . ? N61 C65 1.338(4) . ? N61 N62 1.357(4) . ? N62 C63 1.345(4) . ? C63 C64 1.359(5) . ? C64 C65 1.404(5) . ? C65 C72 1.475(5) . ? N71 C76 1.340(4) . ? N71 C72 1.348(4) . ? C72 C73 1.392(4) . ? C73 C74 1.381(5) . ? C74 C75 1.366(6) . ? C75 C76 1.382(5) . ? N100 O103 1.243(4) . ? N100 O102 1.246(3) . ? N100 O101 1.257(4) . ? N200 C201 1.124(4) . ? C201 C202 1.447(5) . ? 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 N71 Ag1 N11 135.79(9) . . ? N71 Ag1 N21 147.80(10) . . ? N11 Ag1 N21 72.10(9) . . ? N71 Ag1 N61 71.33(10) . . ? N11 Ag1 N61 148.21(10) . . ? N21 Ag1 N61 89.53(9) . . ? C16 N11 C12 117.7(3) . . ? C16 N11 Ag1 124.2(2) . . ? C12 N11 Ag1 117.8(2) . . ? N11 C12 C13 122.2(3) . . ? N11 C12 C25 116.4(3) . . ? C13 C12 C25 121.4(3) . . ? C14 C13 C12 119.3(3) . . ? C15 C14 C13 118.9(3) . . ? C14 C15 C16 119.0(3) . . ? N11 C16 C15 122.9(3) . . ? C25 N21 N22 105.3(2) . . ? C25 N21 Ag1 112.7(2) . . ? N22 N21 Ag1 139.6(2) . . ? C23 N22 N21 111.3(3) . . ? C23 N22 C3 127.8(3) . . ? N21 N22 C3 120.8(2) . . ? N22 C23 C24 107.7(3) . . ? C23 C24 C25 105.2(3) . . ? N21 C25 C24 110.5(3) . . ? N21 C25 C12 119.4(3) . . ? C24 C25 C12 130.1(3) . . ? N22 C3 C4 111.9(3) . . ? C5 C4 C3 114.0(3) . . ? N62 C5 C4 112.9(3) . . ? C65 N61 N62 105.1(3) . . ? C65 N61 Ag1 109.8(2) . . ? N62 N61 Ag1 142.9(2) . . ? C63 N62 N61 111.5(3) . . ? C63 N62 C5 127.9(3) . . ? N61 N62 C5 120.4(3) . . ? N62 C63 C64 107.6(3) . . ? C63 C64 C65 105.4(3) . . ? N61 C65 C64 110.5(3) . . ? N61 C65 C72 119.8(3) . . ? C64 C65 C72 129.7(3) . . ? C76 N71 C72 118.6(3) . . ? C76 N71 Ag1 120.8(2) . . ? C72 N71 Ag1 120.5(3) . . ? N71 C72 C73 121.3(4) . . ? N71 C72 C65 117.5(3) . . ? C73 C72 C65 121.1(3) . . ? C74 C73 C72 119.0(3) . . ? C75 C74 C73 119.6(3) . . ? C74 C75 C76 118.7(4) . . ? N71 C76 C75 122.7(4) . . ? O103 N100 O102 120.0(3) . . ? O103 N100 O101 121.0(3) . . ? O102 N100 O101 119.0(3) . . ? N200 C201 C202 179.3(4) . . ? _refine_diff_density_max 0.346 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.079 #=END data_/glass/sad _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C76 H72 Ag4 Cl4 N24 O16' _chemical_formula_weight 2150.86 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2(1) /n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.0405(10) _cell_length_b 21.604(6) _cell_length_c 26.427(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.570(11) _cell_angle_gamma 90.00 _cell_volume 4011.8(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.781 _exptl_crystal_density_method ? _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 1.180 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24520 _diffrn_reflns_av_R_equivalents 0.0776 _diffrn_reflns_av_sigmaI/netI 0.1110 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9024 _reflns_number_observed 3967 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0549P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9024 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1710 _refine_ls_R_factor_obs 0.0620 _refine_ls_wR_factor_all 0.1585 _refine_ls_wR_factor_obs 0.1178 _refine_ls_goodness_of_fit_all 0.985 _refine_ls_goodness_of_fit_obs 1.146 _refine_ls_restrained_S_all 0.985 _refine_ls_restrained_S_obs 1.146 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ag1 Ag 0.61544(9) 0.74570(2) 0.11506(2) 0.0403(2) Uani 1 d . . Ag2 Ag 0.12803(9) 0.75092(3) 0.13899(2) 0.0403(2) Uani 1 d . . C10 C 0.4293(10) 0.7080(3) -0.0256(2) 0.034(2) Uani 1 d . . C11 C 0.5750(11) 0.7332(3) -0.0608(2) 0.040(2) Uani 1 d . . N11 N 0.1258(8) 0.8482(3) 0.1090(2) 0.0314(14) Uani 1 d . . C12 C 0.7519(11) 0.7623(3) -0.0348(3) 0.041(2) Uani 1 d . . C12 C 0.0829(9) 0.8956(3) 0.1399(3) 0.031(2) Uani 1 d . . C16 C 0.1501(9) 0.8620(3) 0.0609(2) 0.032(2) Uani 1 d . . H16 H 0.1753(9) 0.8288(3) 0.0387(2) 0.039 Uiso 1 calc R . C13 C 0.0648(10) 0.9559(4) 0.1222(3) 0.041(2) Uani 1 d . . H13 H 0.0324(10) 0.9882(4) 0.1445(3) 0.049 Uiso 1 calc R . C14 C 0.0939(10) 0.9686(4) 0.0727(3) 0.046(2) Uani 1 d . . H14 H 0.0813(10) 1.0098(4) 0.0603(3) 0.055 Uiso 1 calc R . C15 C 0.1415(11) 0.9215(3) 0.0406(3) 0.042(2) Uani 1 d . . H15 H 0.1672(11) 0.9293(3) 0.0063(3) 0.050 Uiso 1 calc R . N21 N 0.0353(8) 0.8203(3) 0.2069(2) 0.0351(14) Uani 1 d . . N22 N 0.0133(8) 0.8221(3) 0.2579(2) 0.0344(14) Uani 1 d . . C23 C 0.0153(11) 0.8810(3) 0.2748(3) 0.045(2) Uani 1 d . . H23 H 0.0010(11) 0.8937(3) 0.3088(3) 0.054 Uiso 1 calc R . C24 C 0.0414(10) 0.9190(3) 0.2349(3) 0.040(2) Uani 1 d . . H24 H 0.0489(10) 0.9629(3) 0.2352(3) 0.048 Uiso 1 calc R . C25 C 0.0548(9) 0.8797(3) 0.1930(3) 0.032(2) Uani 1 d . . C30 C -0.0097(11) 0.7642(3) 0.2870(3) 0.042(2) Uani 1 d . . C40 C 0.1736(11) 0.7444(3) 0.3155(2) 0.042(2) Uani 1 d . . C50 C 0.3300(10) 0.7242(3) 0.2821(2) 0.035(2) Uani 1 d . . N61 N 0.2364(8) 0.6743(2) 0.2005(2) 0.0308(14) Uani 1 d . . N62 N 0.2741(8) 0.6692(3) 0.2512(2) 0.0304(13) Uani 1 d . . C63 C 0.2563(10) 0.6098(3) 0.2669(3) 0.039(2) Uani 1 d . . H63 H 0.2742(10) 0.5952(3) 0.3007(3) 0.046 Uiso 1 calc R . C64 C 0.2079(10) 0.5748(3) 0.2250(3) 0.035(2) Uani 1 d . . H64 H 0.1860(10) 0.5315(3) 0.2236(3) 0.042 Uiso 1 calc R . C65 C 0.1976(9) 0.6169(3) 0.1844(2) 0.0248(15) Uani 1 d . . N71 N 0.1130(8) 0.6559(3) 0.1012(2) 0.0291(13) Uani 1 d . . C72 C 0.1550(9) 0.6061(3) 0.1300(2) 0.029(2) Uani 1 d . . C73 C 0.1600(9) 0.5480(3) 0.1087(2) 0.032(2) Uani 1 d . . H73 H 0.1847(9) 0.5129(3) 0.1297(2) 0.038 Uiso 1 calc R . C74 C 0.1298(10) 0.5407(3) 0.0576(3) 0.037(2) Uani 1 d . . H74 H 0.1342(10) 0.5006(3) 0.0430(3) 0.044 Uiso 1 calc R . C75 C 0.0932(10) 0.5913(4) 0.0276(3) 0.043(2) Uani 1 d . . H75 H 0.0742(10) 0.5876(4) -0.0081(3) 0.051 Uiso 1 calc R . C76 C 0.0848(9) 0.6476(3) 0.0511(2) 0.035(2) Uani 1 d . . H76 H 0.0572(9) 0.6829(3) 0.0306(2) 0.042 Uiso 1 calc R . N81 N 0.6620(8) 0.6532(2) 0.1555(2) 0.0290(13) Uani 1 d . . C82 C 0.6536(9) 0.6012(3) 0.1266(2) 0.028(2) Uani 1 d . . C83 C 0.6849(10) 0.5430(3) 0.1485(2) 0.033(2) Uani 1 d . . H83 H 0.6818(10) 0.5069(3) 0.1280(2) 0.039 Uiso 1 calc R . C84 C 0.7202(10) 0.5383(3) 0.2001(3) 0.040(2) Uani 1 d . . H84 H 0.7432(10) 0.4989(3) 0.2152(3) 0.049 Uiso 1 calc R . C85 C 0.7223(10) 0.5904(4) 0.2297(3) 0.041(2) Uani 1 d . . H85 H 0.7422(10) 0.5878(4) 0.2655(3) 0.049 Uiso 1 calc R . C86 C 0.6940(9) 0.6476(3) 0.2053(2) 0.034(2) Uani 1 d . . H86 H 0.6979(9) 0.6841(3) 0.2254(2) 0.041 Uiso 1 calc R . N91 N 0.5432(8) 0.6636(3) 0.0555(2) 0.0279(13) Uani 1 d . . N92 N 0.5104(7) 0.6572(2) 0.0050(2) 0.0271(13) Uani 1 d . . C93 C 0.5536(10) 0.5992(3) -0.0097(2) 0.034(2) Uani 1 d . . H93 H 0.5424(10) 0.5837(3) -0.0434(2) 0.040 Uiso 1 calc R . C94 C 0.6157(9) 0.5672(3) 0.0322(2) 0.030(2) Uani 1 d . . H94 H 0.6564(9) 0.5253(3) 0.0338(2) 0.036 Uiso 1 calc R . C95 C 0.6073(9) 0.6086(3) 0.0726(2) 0.0241(15) Uani 1 d . . N131 N 0.7083(8) 0.8189(3) -0.0068(2) 0.0360(15) Uani 1 d . . N132 N 0.6825(8) 0.8164(2) 0.0437(2) 0.0303(13) Uani 1 d . . C133 C 0.6842(10) 0.8759(3) -0.0255(3) 0.043(2) Uani 1 d . . H133 H 0.6951(10) 0.8880(3) -0.0598(3) 0.051 Uiso 1 calc R . C134 C 0.6406(10) 0.9140(4) 0.0140(3) 0.041(2) Uani 1 d . . H134 H 0.6155(10) 0.9572(4) 0.0128(3) 0.049 Uiso 1 calc R . C135 C 0.6412(10) 0.8752(3) 0.0564(3) 0.032(2) Uani 1 d . . N141 N 0.5892(8) 0.8431(3) 0.1425(2) 0.0337(14) Uani 1 d . . C142 C 0.6028(9) 0.8899(3) 0.1090(3) 0.031(2) Uani 1 d . . C143 C 0.5795(10) 0.9506(3) 0.1239(3) 0.038(2) Uani 1 d . . H143 H 0.5846(10) 0.9831(3) 0.0998(3) 0.046 Uiso 1 calc R . C144 C 0.5484(10) 0.9640(3) 0.1740(3) 0.045(2) Uani 1 d . . H144 H 0.5359(10) 1.0056(3) 0.1848(3) 0.054 Uiso 1 calc R . C145 C 0.5360(11) 0.9160(4) 0.2079(3) 0.046(2) Uani 1 d . . H145 H 0.5124(11) 0.9239(4) 0.2423(3) 0.056 Uiso 1 calc R . C146 C 0.5585(10) 0.8554(3) 0.1909(3) 0.034(2) Uani 1 d . . Cl2 Cl 0.8270(3) 0.13393(8) 0.10761(7) 0.0399(5) Uani 1 d . . Cl1 Cl 0.9367(3) 0.37649(9) 0.13271(7) 0.0427(5) Uani 1 d . . O1 O 1.0655(12) 0.3630(4) 0.0966(3) 0.135(4) Uani 1 d . . O2 O 1.0119(11) 0.4235(3) 0.1652(2) 0.095(2) Uani 1 d . . O3 O 0.9075(11) 0.3251(3) 0.1637(4) 0.126(3) Uani 1 d . . O4 O 0.7644(9) 0.3985(3) 0.1094(2) 0.091(2) Uani 1 d . . O5 O 0.7516(11) 0.0771(3) 0.0884(3) 0.106(3) Uani 1 d . . O6 O 1.0219(9) 0.1239(3) 0.1227(2) 0.078(2) Uani 1 d . . O7 O 0.7303(11) 0.1576(4) 0.1478(2) 0.107(3) Uani 1 d . . O8 O 0.8163(8) 0.1768(3) 0.0663(2) 0.065(2) Uani 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 Ag1 0.0595(5) 0.0258(3) 0.0356(3) 0.0021(3) 0.0042(3) 0.0016(3) Ag2 0.0565(4) 0.0298(3) 0.0346(3) -0.0015(2) 0.0036(3) 0.0007(3) C10 0.040(5) 0.032(4) 0.031(4) 0.006(3) 0.006(3) 0.006(3) C11 0.050(5) 0.044(5) 0.026(4) 0.007(3) 0.008(4) 0.007(4) N11 0.023(3) 0.034(3) 0.036(3) -0.003(3) 0.001(3) -0.003(3) C12 0.038(5) 0.045(5) 0.042(4) 0.001(4) 0.012(4) 0.006(4) C12 0.018(4) 0.032(4) 0.044(4) -0.002(3) -0.005(3) 0.001(3) C16 0.020(4) 0.044(5) 0.034(4) 0.000(3) -0.004(3) 0.007(3) C13 0.021(4) 0.042(5) 0.059(5) -0.001(4) -0.004(4) 0.004(3) C14 0.030(5) 0.042(5) 0.063(6) 0.009(4) -0.013(4) -0.004(4) C15 0.038(5) 0.040(5) 0.048(5) 0.010(4) 0.001(4) 0.003(4) N21 0.027(3) 0.039(4) 0.040(4) -0.010(3) 0.002(3) 0.001(3) N22 0.030(4) 0.032(4) 0.042(4) -0.011(3) 0.008(3) -0.002(3) C23 0.045(5) 0.045(5) 0.045(5) -0.021(4) 0.013(4) -0.007(4) C24 0.040(5) 0.026(4) 0.055(5) -0.007(4) 0.011(4) -0.006(3) C25 0.016(4) 0.031(4) 0.048(4) -0.013(3) -0.001(3) -0.001(3) C30 0.051(5) 0.035(5) 0.041(4) -0.001(3) 0.016(4) -0.008(4) C40 0.043(5) 0.058(5) 0.027(3) -0.002(4) 0.006(3) -0.007(4) C50 0.044(5) 0.028(4) 0.033(4) -0.010(3) 0.010(3) -0.012(3) N61 0.036(4) 0.032(3) 0.024(3) 0.000(2) 0.007(3) -0.009(3) N62 0.031(3) 0.034(3) 0.026(3) 0.005(2) 0.005(3) -0.002(3) C63 0.038(5) 0.041(5) 0.037(4) 0.015(3) 0.008(4) 0.005(4) C64 0.033(4) 0.031(4) 0.042(4) 0.000(3) 0.003(3) -0.003(3) C65 0.020(4) 0.032(4) 0.022(3) 0.004(3) 0.004(3) 0.002(3) N71 0.028(3) 0.033(3) 0.027(3) -0.003(2) 0.005(3) -0.006(3) C72 0.024(4) 0.032(4) 0.031(4) -0.004(3) 0.008(3) 0.000(3) C73 0.020(4) 0.036(4) 0.039(4) -0.001(3) -0.002(3) -0.004(3) C74 0.032(4) 0.036(4) 0.043(4) -0.016(4) 0.004(4) -0.010(4) C75 0.032(5) 0.061(6) 0.034(4) -0.019(4) 0.001(4) -0.016(4) C76 0.027(4) 0.052(5) 0.025(4) 0.006(3) -0.005(3) -0.007(4) N81 0.025(3) 0.027(3) 0.035(3) 0.000(3) 0.002(3) -0.003(3) C82 0.022(4) 0.031(4) 0.033(4) 0.000(3) 0.005(3) -0.001(3) C83 0.041(5) 0.029(4) 0.029(4) 0.001(3) 0.006(3) 0.003(3) C84 0.037(5) 0.037(5) 0.048(5) 0.010(4) 0.007(4) 0.004(4) C85 0.028(4) 0.064(6) 0.029(4) 0.014(4) -0.001(3) 0.006(4) C86 0.023(4) 0.047(5) 0.032(4) 0.001(3) -0.001(3) 0.001(3) N91 0.027(3) 0.035(3) 0.022(3) 0.001(2) 0.004(2) -0.008(3) N92 0.024(3) 0.029(3) 0.029(3) 0.003(2) 0.003(2) -0.002(3) C93 0.037(4) 0.039(4) 0.026(4) -0.004(3) 0.008(3) 0.002(3) C94 0.028(4) 0.024(4) 0.039(4) -0.004(3) 0.010(3) 0.001(3) C95 0.022(4) 0.019(3) 0.032(4) 0.003(3) 0.004(3) -0.002(3) N131 0.034(4) 0.035(4) 0.041(4) 0.014(3) 0.011(3) 0.004(3) N132 0.029(3) 0.027(3) 0.036(3) 0.007(3) 0.006(3) -0.002(3) C133 0.042(5) 0.041(5) 0.045(4) 0.023(4) 0.002(4) -0.001(4) C134 0.035(5) 0.040(5) 0.049(5) 0.012(4) 0.007(4) -0.005(4) C135 0.026(4) 0.030(4) 0.039(4) 0.008(3) 0.006(3) -0.008(3) N141 0.030(4) 0.030(3) 0.040(4) 0.006(3) 0.000(3) -0.004(3) C142 0.021(4) 0.026(4) 0.044(4) 0.001(3) -0.002(3) -0.003(3) C143 0.033(5) 0.030(4) 0.051(5) 0.004(3) -0.007(4) -0.008(3) C144 0.032(5) 0.030(4) 0.070(6) -0.005(4) -0.011(4) -0.001(3) C145 0.033(5) 0.062(6) 0.043(5) -0.009(4) 0.001(4) -0.015(4) C146 0.024(4) 0.034(4) 0.043(4) -0.005(3) -0.001(3) -0.009(3) Cl2 0.0440(12) 0.0349(10) 0.0404(10) 0.0042(8) -0.0004(9) 0.0046(9) Cl1 0.0461(13) 0.0371(11) 0.0442(11) 0.0018(9) -0.0014(10) 0.0090(9) O1 0.142(8) 0.194(9) 0.073(5) 0.015(5) 0.043(5) 0.100(7) O2 0.111(6) 0.080(5) 0.088(5) -0.008(4) -0.040(4) -0.022(4) O3 0.089(6) 0.055(5) 0.236(10) 0.064(6) 0.031(6) 0.009(4) O4 0.085(5) 0.074(5) 0.108(5) -0.041(4) -0.054(4) 0.042(4) O5 0.107(6) 0.043(4) 0.164(7) 0.012(4) -0.010(5) -0.034(4) O6 0.060(4) 0.123(6) 0.049(4) -0.007(3) -0.016(3) 0.031(4) O7 0.114(6) 0.143(7) 0.069(4) 0.021(4) 0.049(4) 0.054(6) O8 0.066(4) 0.057(4) 0.073(4) 0.029(3) 0.008(3) 0.009(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 Ag1 N141 2.237(6) . ? Ag1 N81 2.281(5) . ? Ag1 N91 2.405(5) . ? Ag1 N132 2.495(5) . ? Ag2 N11 2.246(6) . ? Ag2 N71 2.281(5) . ? Ag2 N61 2.411(5) . ? Ag2 N21 2.457(5) . ? C10 N92 1.459(8) . ? C10 C11 1.526(9) . ? C11 C12 1.520(11) . ? N11 C16 1.326(8) . ? N11 C12 1.356(8) . ? C12 N131 1.472(9) . ? C12 C13 1.387(9) . ? C12 C25 1.470(9) . ? C16 C15 1.394(9) . ? C13 C14 1.366(10) . ? C14 C15 1.379(10) . ? N21 C25 1.343(8) . ? N21 N22 1.366(7) . ? N22 C23 1.347(8) . ? N22 C30 1.484(9) . ? C23 C24 1.358(10) . ? C24 C25 1.404(9) . ? C30 C40 1.515(11) . ? C40 C50 1.517(9) . ? C50 N62 1.481(8) . ? N61 C65 1.333(8) . ? N61 N62 1.355(7) . ? N62 C63 1.355(8) . ? C63 C64 1.365(9) . ? C64 C65 1.404(9) . ? C65 C72 1.468(8) . ? N71 C76 1.339(7) . ? N71 C72 1.342(8) . ? C72 C73 1.376(9) . ? C73 C74 1.364(9) . ? C74 C75 1.365(10) . ? C75 C76 1.368(9) . ? N81 C86 1.326(8) . ? N81 C82 1.358(8) . ? C82 C83 1.396(9) . ? C82 C95 1.451(8) . ? C83 C84 1.373(9) . ? C84 C85 1.369(10) . ? C85 C86 1.403(10) . ? N91 C95 1.340(8) . ? N91 N92 1.345(7) . ? N92 C93 1.352(8) . ? C93 C94 1.356(9) . ? C94 C95 1.397(8) . ? N131 C133 1.333(8) . ? N131 N132 1.358(7) . ? N132 C135 1.351(8) . ? C133 C134 1.381(10) . ? C134 C135 1.397(9) . ? C135 C142 1.469(9) . ? N141 C146 1.338(8) . ? N141 C142 1.351(8) . ? C142 C143 1.380(9) . ? C143 C144 1.388(10) . ? C144 C145 1.376(10) . ? C145 C146 1.396(10) . ? Cl2 O7 1.394(6) . ? Cl2 O6 1.422(6) . ? Cl2 O5 1.419(7) . ? Cl2 O8 1.431(5) . ? Cl1 O1 1.388(7) . ? Cl1 O3 1.403(7) . ? Cl1 O4 1.409(6) . ? Cl1 O2 1.412(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 N141 Ag1 N81 133.2(2) . . ? N141 Ag1 N91 152.5(2) . . ? N81 Ag1 N91 71.3(2) . . ? N141 Ag1 N132 72.1(2) . . ? N81 Ag1 N132 149.6(2) . . ? N91 Ag1 N132 89.9(2) . . ? N11 Ag2 N71 133.5(2) . . ? N11 Ag2 N61 151.1(2) . . ? N71 Ag2 N61 71.4(2) . . ? N11 Ag2 N21 72.0(2) . . ? N71 Ag2 N21 149.4(2) . . ? N61 Ag2 N21 90.8(2) . . ? N92 C10 C11 110.6(6) . . ? C12 C11 C10 115.8(6) . . ? C16 N11 C12 117.0(6) . . ? C16 N11 Ag2 123.4(5) . . ? C12 N11 Ag2 119.4(4) . . ? N131 C12 C11 112.4(6) . . ? N11 C12 C13 121.7(7) . . ? N11 C12 C25 116.5(6) . . ? C13 C12 C25 121.8(6) . . ? N11 C16 C15 124.9(7) . . ? C14 C13 C12 119.7(7) . . ? C13 C14 C15 120.0(7) . . ? C14 C15 C16 116.6(7) . . ? C25 N21 N22 105.2(5) . . ? C25 N21 Ag2 110.3(4) . . ? N22 N21 Ag2 142.1(4) . . ? C23 N22 N21 110.8(6) . . ? C23 N22 C30 128.5(6) . . ? N21 N22 C30 120.7(5) . . ? N22 C23 C24 108.2(6) . . ? C23 C24 C25 105.4(7) . . ? N21 C25 C24 110.5(6) . . ? N21 C25 C12 120.4(6) . . ? C24 C25 C12 129.1(7) . . ? N22 C30 C40 112.3(6) . . ? C30 C40 C50 114.8(6) . . ? N62 C50 C40 112.0(6) . . ? C65 N61 N62 105.3(5) . . ? C65 N61 Ag2 111.9(4) . . ? N62 N61 Ag2 139.2(4) . . ? C63 N62 N61 111.2(5) . . ? C63 N62 C50 128.1(6) . . ? N61 N62 C50 120.6(5) . . ? N62 C63 C64 107.4(6) . . ? C63 C64 C65 105.0(6) . . ? N61 C65 C64 111.0(6) . . ? N61 C65 C72 119.1(6) . . ? C64 C65 C72 130.0(6) . . ? C76 N71 C72 117.8(6) . . ? C76 N71 Ag2 123.7(5) . . ? C72 N71 Ag2 118.1(4) . . ? N71 C72 C73 120.6(6) . . ? N71 C72 C65 116.9(6) . . ? C73 C72 C65 122.5(6) . . ? C74 C73 C72 120.4(7) . . ? C73 C74 C75 119.6(7) . . ? C74 C75 C76 117.4(7) . . ? N71 C76 C75 124.1(7) . . ? C86 N81 C82 118.9(6) . . ? C86 N81 Ag1 123.7(5) . . ? C82 N81 Ag1 117.4(4) . . ? N81 C82 C83 120.6(6) . . ? N81 C82 C95 117.4(6) . . ? C83 C82 C95 121.9(6) . . ? C84 C83 C82 119.5(6) . . ? C85 C84 C83 120.1(7) . . ? C84 C85 C86 117.7(7) . . ? N81 C86 C85 123.1(7) . . ? C95 N91 N92 106.1(5) . . ? C95 N91 Ag1 112.2(4) . . ? N92 N91 Ag1 137.8(4) . . ? N91 N92 C93 110.7(5) . . ? N91 N92 C10 120.7(5) . . ? C93 N92 C10 128.6(5) . . ? N92 C93 C94 107.7(6) . . ? C93 C94 C95 105.7(6) . . ? N91 C95 C94 109.8(6) . . ? N91 C95 C82 118.8(6) . . ? C94 C95 C82 131.4(6) . . ? C133 N131 N132 112.3(6) . . ? C133 N131 C12 127.2(6) . . ? N132 N131 C12 120.4(5) . . ? C135 N132 N131 104.5(5) . . ? C135 N132 Ag1 109.6(4) . . ? N131 N132 Ag1 144.1(4) . . ? N131 C133 C134 107.4(6) . . ? C133 C134 C135 104.9(7) . . ? N132 C135 C134 110.9(6) . . ? N132 C135 C142 119.6(6) . . ? C134 C135 C142 129.6(7) . . ? C146 N141 C142 120.0(6) . . ? C146 N141 Ag1 121.2(4) . . ? C142 N141 Ag1 118.8(5) . . ? N141 C142 C143 120.7(7) . . ? N141 C142 C135 118.9(6) . . ? C143 C142 C135 120.4(6) . . ? C142 C143 C144 119.9(7) . . ? C145 C144 C143 118.9(7) . . ? C144 C145 C146 119.0(7) . . ? N141 C146 C145 121.4(7) . . ? O7 Cl2 O6 110.5(4) . . ? O7 Cl2 O5 113.6(5) . . ? O6 Cl2 O5 107.6(4) . . ? O7 Cl2 O8 109.8(4) . . ? O6 Cl2 O8 108.5(4) . . ? O5 Cl2 O8 106.6(4) . . ? O1 Cl1 O3 111.1(5) . . ? O1 Cl1 O4 110.6(5) . . ? O3 Cl1 O4 111.6(5) . . ? O1 Cl1 O2 109.5(5) . . ? O3 Cl1 O2 106.1(5) . . ? O4 Cl1 O2 107.7(4) . . ? _refine_diff_density_max 0.751 _refine_diff_density_min -0.785 _refine_diff_density_rms 0.114 #=END data_sad _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C19 H18 N8 O6 Pb' _chemical_formula_weight 661.60 _chemical_melting_point ? _chemical_compound_source ? 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' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2(1) /n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.2539(8) _cell_length_b 10.8331(14) _cell_length_c 16.792(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.471(8) _cell_angle_gamma 90.00 _cell_volume 2204.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.993 _exptl_crystal_density_method ? _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 7.707 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13713 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5025 _reflns_number_observed 4191 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0192P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5025 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0243 _refine_ls_R_factor_obs 0.0177 _refine_ls_wR_factor_all 0.0402 _refine_ls_wR_factor_obs 0.0392 _refine_ls_goodness_of_fit_all 0.948 _refine_ls_goodness_of_fit_obs 1.020 _refine_ls_restrained_S_all 0.948 _refine_ls_restrained_S_obs 1.020 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pb Pb 0.135110(9) 1.098105(9) -0.059163(6) 0.01775(4) Uani 1 d . . N11 N 0.2874(2) 0.9459(2) 0.0196(2) 0.0275(6) Uani 1 d . . C12 C 0.3685(3) 0.9033(3) -0.0198(2) 0.0300(7) Uani 1 d . . C13 C 0.4420(3) 0.8127(3) 0.0129(2) 0.0412(9) Uani 1 d . . H13 H 0.4978(3) 0.7830(3) -0.0159(2) 0.049 Uiso 1 calc R . C14 C 0.4322(3) 0.7673(3) 0.0876(3) 0.0509(11) Uani 1 d . . H14 H 0.4813(3) 0.7047(3) 0.1107(3) 0.061 Uiso 1 calc R . C15 C 0.3523(3) 0.8109(4) 0.1294(2) 0.0463(10) Uani 1 d . . H15 H 0.3462(3) 0.7813(4) 0.1819(2) 0.056 Uiso 1 calc R . C16 C 0.2809(3) 0.8997(3) 0.0926(2) 0.0377(8) Uani 1 d . . H16 H 0.2243(3) 0.9294(3) 0.1206(2) 0.045 Uiso 1 calc R . N21 N 0.3077(2) 1.0475(2) -0.1290(2) 0.0229(6) Uani 1 d . . N22 N 0.3424(2) 1.0809(2) -0.1987(2) 0.0279(6) Uani 1 d . . C23 C 0.4301(3) 1.0138(4) -0.2120(2) 0.0436(10) Uani 1 d . . H23 H 0.4668(3) 1.0189(4) -0.2580(2) 0.052 Uiso 1 calc R . C24 C 0.4572(3) 0.9370(3) -0.1477(3) 0.0435(10) Uani 1 d . . H24 H 0.5170(3) 0.8806(3) -0.1387(3) 0.052 Uiso 1 calc R . C25 C 0.3774(3) 0.9597(3) -0.0979(2) 0.0265(7) Uani 1 d . . C30 C 0.2839(3) 1.1719(3) -0.2530(2) 0.0293(8) Uani 1 d . . H30A H 0.3379(3) 1.2276(3) -0.2730(2) 0.035 Uiso 1 calc R . H30B H 0.2360(3) 1.2225(3) -0.2232(2) 0.035 Uiso 1 calc R . C31 C 0.2134(3) 1.1093(3) -0.3244(2) 0.0308(8) Uani 1 d . . H31A H 0.1795(3) 1.1738(3) -0.3619(2) 0.037 Uiso 1 calc R . H31B H 0.2621(3) 1.0588(3) -0.3535(2) 0.037 Uiso 1 calc R . C32 C 0.1223(3) 1.0271(3) -0.3010(2) 0.0279(7) Uani 1 d . . H32A H 0.0956(3) 0.9714(3) -0.3465(2) 0.033 Uiso 1 calc R . H32B H 0.1529(3) 0.9752(3) -0.2545(2) 0.033 Uiso 1 calc R . N41 N 0.0344(2) 1.1564(2) -0.20788(14) 0.0209(5) Uani 1 d . . N42 N 0.0293(2) 1.0986(2) -0.28002(15) 0.0251(6) Uani 1 d . . C43 C -0.0637(3) 1.1277(3) -0.3291(2) 0.0302(8) Uani 1 d . . H43 H -0.0841(3) 1.0992(3) -0.3827(2) 0.036 Uiso 1 calc R . C44 C -0.1233(3) 1.2050(3) -0.2887(2) 0.0290(7) Uani 1 d . . H44 H -0.1934(3) 1.2402(3) -0.3075(2) 0.035 Uiso 1 calc R . C45 C -0.0594(2) 1.2216(3) -0.2136(2) 0.0212(6) Uani 1 d . . N51 N -0.0325(2) 1.2690(2) -0.07211(15) 0.0248(6) Uani 1 d . . C52 C -0.0834(2) 1.2991(3) -0.1466(2) 0.0230(6) Uani 1 d . . C53 C -0.1545(3) 1.3988(3) -0.1594(2) 0.0347(8) Uani 1 d . . H53 H -0.1878(3) 1.4195(3) -0.2124(2) 0.042 Uiso 1 calc R . C54 C -0.1766(3) 1.4678(3) -0.0946(2) 0.0407(9) Uani 1 d . . H54 H -0.2243(3) 1.5373(3) -0.1024(2) 0.049 Uiso 1 calc R . C55 C -0.1285(3) 1.4342(3) -0.0187(2) 0.0394(9) Uani 1 d . . H55 H -0.1446(3) 1.4778(3) 0.0273(2) 0.047 Uiso 1 calc R . C56 C -0.0564(3) 1.3359(3) -0.0104(2) 0.0321(8) Uani 1 d . . H56 H -0.0218(3) 1.3147(3) 0.0422(2) 0.039 Uiso 1 calc R . N100 N 0.2860(2) 1.3247(2) -0.03224(15) 0.0203(5) Uani 1 d . . O101 O 0.2816(2) 1.2470(2) 0.02296(13) 0.0399(6) Uani 1 d . . O102 O 0.2183(2) 1.3178(2) -0.09488(12) 0.0294(5) Uani 1 d . . O103 O 0.3577(2) 1.4072(2) -0.02315(13) 0.0317(5) Uani 1 d . . N200 N -0.0176(3) 0.8728(2) -0.1367(2) 0.0339(7) Uani 1 d . . O201 O -0.0735(3) 0.7985(3) -0.1769(2) 0.0822(11) Uani 1 d . . O202 O -0.0560(2) 0.9448(2) -0.08837(14) 0.0367(6) Uani 1 d . . O203 O 0.0850(2) 0.8797(2) -0.1391(2) 0.0428(7) Uani 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 Pb 0.01664(6) 0.01799(5) 0.01889(6) 0.00000(5) 0.00349(4) 0.00261(5) N11 0.0188(14) 0.0228(13) 0.041(2) 0.0090(12) 0.0038(12) 0.0029(11) C12 0.022(2) 0.0194(15) 0.047(2) -0.001(2) -0.0007(14) 0.0006(14) C13 0.029(2) 0.027(2) 0.064(3) -0.002(2) -0.004(2) 0.011(2) C14 0.036(2) 0.033(2) 0.076(3) 0.019(2) -0.015(2) 0.010(2) C15 0.032(2) 0.046(2) 0.056(3) 0.025(2) -0.008(2) -0.001(2) C16 0.025(2) 0.040(2) 0.047(2) 0.016(2) 0.002(2) -0.002(2) N21 0.0200(13) 0.0207(12) 0.0294(15) -0.0023(11) 0.0086(11) -0.0013(11) N22 0.0261(15) 0.032(2) 0.0277(15) -0.0058(12) 0.0113(12) -0.0032(12) C23 0.038(2) 0.055(2) 0.042(2) -0.008(2) 0.022(2) 0.008(2) C24 0.023(2) 0.047(2) 0.061(3) -0.016(2) 0.010(2) 0.007(2) C25 0.020(2) 0.022(2) 0.038(2) -0.0067(14) 0.0059(14) 0.0022(13) C30 0.035(2) 0.026(2) 0.030(2) -0.0012(14) 0.013(2) -0.0054(14) C31 0.040(2) 0.032(2) 0.024(2) -0.0061(15) 0.0140(15) -0.004(2) C32 0.038(2) 0.023(2) 0.024(2) -0.0092(13) 0.0089(14) -0.0020(14) N41 0.0267(14) 0.0228(13) 0.0129(12) -0.0041(10) 0.0019(10) -0.0016(11) N42 0.0300(15) 0.0260(13) 0.0190(13) -0.0026(12) 0.0031(11) -0.0053(12) C43 0.032(2) 0.038(2) 0.018(2) 0.0004(13) -0.0060(14) -0.0148(15) C44 0.024(2) 0.036(2) 0.025(2) 0.0050(15) -0.0039(13) -0.0047(15) C45 0.020(2) 0.0226(15) 0.021(2) 0.0059(13) 0.0016(12) -0.0030(13) N51 0.0285(15) 0.0239(14) 0.0219(14) 0.0011(11) 0.0032(11) 0.0054(11) C52 0.0167(15) 0.026(2) 0.026(2) 0.0039(14) 0.0039(12) -0.0007(13) C53 0.026(2) 0.041(2) 0.036(2) 0.011(2) 0.0013(14) 0.013(2) C54 0.035(2) 0.040(2) 0.048(2) 0.002(2) 0.009(2) 0.020(2) C55 0.044(2) 0.037(2) 0.041(2) -0.003(2) 0.019(2) 0.014(2) C56 0.044(2) 0.029(2) 0.025(2) 0.0003(14) 0.009(2) 0.007(2) N100 0.0239(14) 0.0194(13) 0.0184(13) -0.0011(10) 0.0062(11) 0.0041(11) O101 0.058(2) 0.0382(14) 0.0213(12) 0.0084(11) -0.0024(11) -0.0177(12) O102 0.0342(13) 0.0294(12) 0.0219(12) 0.0006(10) -0.0048(10) 0.0011(10) O103 0.0338(13) 0.0319(12) 0.0283(12) 0.0034(11) 0.0011(10) -0.0077(11) N200 0.051(2) 0.027(2) 0.025(2) 0.0036(12) 0.0074(14) -0.0064(14) O201 0.102(3) 0.076(2) 0.061(2) -0.024(2) -0.009(2) -0.042(2) O202 0.0356(14) 0.0431(14) 0.0347(14) 0.0018(11) 0.0163(11) 0.0023(11) O203 0.052(2) 0.0299(13) 0.054(2) -0.0013(12) 0.0325(14) 0.0046(12) _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 Pb N21 2.623(2) . ? Pb O101 2.644(2) . ? Pb N11 2.688(3) . ? Pb O102 2.692(2) . ? Pb N41 2.693(2) . ? Pb O203 2.745(2) . ? Pb N51 2.749(2) . ? Pb O202 2.854(2) . ? N11 C16 1.337(4) . ? N11 C12 1.353(4) . ? C12 C13 1.389(5) . ? C12 C25 1.466(5) . ? C13 C14 1.369(5) . ? C14 C15 1.370(5) . ? C15 C16 1.384(5) . ? N21 C25 1.332(4) . ? N21 N22 1.352(3) . ? N22 C23 1.343(4) . ? N22 C30 1.457(4) . ? C23 C24 1.365(5) . ? C24 C25 1.398(4) . ? C30 C31 1.529(4) . ? C31 C32 1.524(4) . ? C32 N42 1.464(4) . ? N41 C45 1.340(4) . ? N41 N42 1.357(3) . ? N42 C43 1.342(4) . ? C43 C44 1.357(5) . ? C44 C45 1.395(4) . ? C45 C52 1.468(4) . ? N51 C56 1.332(4) . ? N51 C52 1.354(4) . ? C52 C53 1.384(4) . ? C53 C54 1.380(5) . ? C54 C55 1.373(5) . ? C55 C56 1.377(5) . ? N100 O102 1.242(3) . ? N100 O103 1.246(3) . ? N100 O101 1.260(3) . ? N200 O201 1.198(4) . ? N200 O202 1.266(3) . ? N200 O203 1.267(4) . ? 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 N21 Pb O101 80.26(8) . . ? N21 Pb N11 62.91(8) . . ? O101 Pb N11 75.46(8) . . ? N21 Pb O102 74.23(7) . . ? O101 Pb O102 47.68(6) . . ? N11 Pb O102 113.18(7) . . ? N21 Pb N41 85.63(8) . . ? O101 Pb N41 121.59(7) . . ? N11 Pb N41 142.21(8) . . ? O102 Pb N41 73.92(7) . . ? N21 Pb O203 74.81(7) . . ? O101 Pb O203 150.04(8) . . ? N11 Pb O203 78.51(8) . . ? O102 Pb O203 135.89(7) . . ? N41 Pb O203 73.11(8) . . ? N21 Pb N51 138.37(7) . . ? O101 Pb N51 94.14(8) . . ? N11 Pb N51 155.29(8) . . ? O102 Pb N51 71.95(7) . . ? N41 Pb N51 62.21(7) . . ? O203 Pb N51 115.53(8) . . ? N21 Pb O202 119.79(7) . . ? O101 Pb O202 157.08(7) . . ? N11 Pb O202 102.73(7) . . ? O102 Pb O202 143.56(7) . . ? N41 Pb O202 74.01(7) . . ? O203 Pb O202 45.23(7) . . ? N51 Pb O202 78.09(7) . . ? C16 N11 C12 117.9(3) . . ? C16 N11 Pb 123.3(2) . . ? C12 N11 Pb 118.4(2) . . ? N11 C12 C13 121.9(3) . . ? N11 C12 C25 116.8(3) . . ? C13 C12 C25 121.2(3) . . ? C14 C13 C12 118.4(3) . . ? C13 C14 C15 120.8(3) . . ? C14 C15 C16 117.6(4) . . ? N11 C16 C15 123.4(3) . . ? C25 N21 N22 105.4(2) . . ? C25 N21 Pb 119.1(2) . . ? N22 N21 Pb 135.1(2) . . ? C23 N22 N21 111.1(3) . . ? C23 N22 C30 126.5(3) . . ? N21 N22 C30 122.3(2) . . ? N22 C23 C24 107.8(3) . . ? C23 C24 C25 104.8(3) . . ? N21 C25 C24 110.8(3) . . ? N21 C25 C12 121.4(3) . . ? C24 C25 C12 127.7(3) . . ? N22 C30 C31 111.0(3) . . ? C32 C31 C30 114.1(3) . . ? N42 C32 C31 112.2(2) . . ? C45 N41 N42 104.7(2) . . ? C45 N41 Pb 117.5(2) . . ? N42 N41 Pb 132.4(2) . . ? C43 N42 N41 111.3(3) . . ? C43 N42 C32 126.6(3) . . ? N41 N42 C32 121.6(3) . . ? N42 C43 C44 108.0(3) . . ? C43 C44 C45 105.0(3) . . ? N41 C45 C44 111.0(3) . . ? N41 C45 C52 120.9(3) . . ? C44 C45 C52 128.1(3) . . ? C56 N51 C52 117.6(3) . . ? C56 N51 Pb 123.5(2) . . ? C52 N51 Pb 118.2(2) . . ? N51 C52 C53 121.7(3) . . ? N51 C52 C45 116.9(3) . . ? C53 C52 C45 121.3(3) . . ? C54 C53 C52 119.5(3) . . ? C55 C54 C53 118.8(3) . . ? C54 C55 C56 118.7(3) . . ? N51 C56 C55 123.6(3) . . ? O102 N100 O103 121.2(2) . . ? O102 N100 O101 119.2(3) . . ? O103 N100 O101 119.7(3) . . ? N100 O101 Pb 97.1(2) . . ? N100 O102 Pb 95.3(2) . . ? O201 N200 O202 122.6(3) . . ? O201 N200 O203 120.6(3) . . ? O202 N200 O203 116.7(3) . . ? N200 O202 Pb 95.5(2) . . ? N200 O203 Pb 100.7(2) . . ? _refine_diff_density_max 0.955 _refine_diff_density_min -0.993 _refine_diff_density_rms 0.097 #=END