# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Mike Ward' _publ_contact_author_email M.D.WARD@SHEFFIELD.AC.UK _publ_section_title ; Hierarchical Self-Assembly of Heteronuclear Co-ordination Networks ; loop_ _publ_author_name 'Mike Ward' 'Hazel E Fenton' 'Ian Tidmarsh' # Attachment 'mixed_metal_networks.cif' data_imw1200p21c _database_code_depnum_ccdc_archive 'CCDC 758085' #TrackingRef 'mixed_metal_networks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H12 N4' _chemical_formula_weight 260.30 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.804(2) _cell_length_b 10.805(3) _cell_length_c 12.268(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.515(9) _cell_angle_gamma 90.00 _cell_volume 1281.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9752 _exptl_absorpt_correction_T_max 0.9752 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22007 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0138 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 26.37 _reflns_number_total 2627 _reflns_number_gt 2395 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0417P)^2^+0.5070P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2627 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0849 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _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 N11 N -0.24336(10) 0.12758(9) 0.53273(8) 0.0247(2) Uani 1 1 d . . . C12 C -0.10536(11) 0.12577(10) 0.56099(8) 0.0189(2) Uani 1 1 d . . . C13 C -0.01745(12) 0.17868(10) 0.49551(9) 0.0209(2) Uani 1 1 d . . . H13 H 0.0800 0.1754 0.5178 0.025 Uiso 1 1 calc R . . C14 C -0.07398(12) 0.23604(10) 0.39760(9) 0.0226(2) Uani 1 1 d . . . H14 H -0.0160 0.2729 0.3518 0.027 Uiso 1 1 calc R . . C15 C -0.21636(12) 0.23890(10) 0.36734(9) 0.0235(2) Uani 1 1 d . . . H15 H -0.2584 0.2777 0.3007 0.028 Uiso 1 1 calc R . . C16 C -0.29550(12) 0.18361(11) 0.43690(10) 0.0259(3) Uani 1 1 d . . . H16 H -0.3932 0.1852 0.4157 0.031 Uiso 1 1 calc R . . N21 N 0.10337(10) -0.00493(8) 0.79611(7) 0.0209(2) Uani 1 1 d . . . N22 N 0.08771(10) 0.06177(8) 0.70160(7) 0.0206(2) Uani 1 1 d . . . C23 C -0.04881(11) 0.06300(10) 0.66563(9) 0.0194(2) Uani 1 1 d . . . C24 C -0.12018(12) -0.00278(10) 0.73783(9) 0.0217(2) Uani 1 1 d . . . H24 H -0.2171 -0.0154 0.7309 0.026 Uiso 1 1 calc R . . C25 C -0.01895(12) -0.04454(11) 0.82025(9) 0.0228(2) Uani 1 1 d . . . H25 H -0.0323 -0.0924 0.8826 0.027 Uiso 1 1 calc R . . C26 C 0.24104(12) -0.02328(10) 0.85984(9) 0.0232(3) Uani 1 1 d . . . H26A H 0.3069 -0.0382 0.8082 0.028 Uiso 1 1 calc R . . H26B H 0.2400 -0.0982 0.9062 0.028 Uiso 1 1 calc R . . C31 C 0.29213(11) 0.08544(10) 0.93384(9) 0.0197(2) Uani 1 1 d . . . C32 C 0.28952(11) 0.20597(10) 0.89197(9) 0.0206(2) Uani 1 1 d . . . H32 H 0.2527 0.2206 0.8165 0.025 Uiso 1 1 calc R . . C33 C 0.33995(11) 0.30413(10) 0.95929(9) 0.0209(2) Uani 1 1 d . . . H33 H 0.3366 0.3859 0.9306 0.025 Uiso 1 1 calc R . . C34 C 0.39596(11) 0.28159(10) 1.07016(9) 0.0200(2) Uani 1 1 d . . . C35 C 0.39910(12) 0.16220(11) 1.11292(9) 0.0239(3) Uani 1 1 d . . . H35 H 0.4367 0.1474 1.1882 0.029 Uiso 1 1 calc R . . C36 C 0.34698(12) 0.06495(11) 1.04472(9) 0.0235(2) Uani 1 1 d . . . H36 H 0.3486 -0.0166 1.0739 0.028 Uiso 1 1 calc R . . C37 C 0.45307(12) 0.38126(11) 1.14161(9) 0.0229(2) Uani 1 1 d . . . N38 N 0.50059(11) 0.45813(10) 1.20035(9) 0.0311(3) 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 N11 0.0217(5) 0.0262(5) 0.0259(5) 0.0007(4) 0.0032(4) -0.0016(4) C12 0.0218(6) 0.0149(5) 0.0197(5) -0.0040(4) 0.0026(4) -0.0007(4) C13 0.0198(5) 0.0190(5) 0.0237(5) -0.0022(4) 0.0030(4) -0.0002(4) C14 0.0267(6) 0.0180(5) 0.0238(5) 0.0000(4) 0.0062(4) -0.0007(4) C15 0.0282(6) 0.0182(5) 0.0226(5) -0.0006(4) 0.0000(4) 0.0015(5) C16 0.0202(6) 0.0266(6) 0.0294(6) 0.0002(5) -0.0007(4) 0.0002(5) N21 0.0254(5) 0.0174(5) 0.0190(5) -0.0003(3) 0.0007(4) -0.0012(4) N22 0.0249(5) 0.0175(5) 0.0186(4) 0.0001(3) 0.0016(4) -0.0008(4) C23 0.0220(5) 0.0161(5) 0.0200(5) -0.0045(4) 0.0032(4) -0.0016(4) C24 0.0242(6) 0.0195(5) 0.0216(5) -0.0035(4) 0.0043(4) -0.0044(4) C25 0.0299(6) 0.0180(5) 0.0209(5) -0.0012(4) 0.0052(4) -0.0041(5) C26 0.0258(6) 0.0189(6) 0.0234(5) 0.0001(4) -0.0006(4) 0.0018(4) C31 0.0176(5) 0.0199(5) 0.0214(5) 0.0002(4) 0.0028(4) 0.0011(4) C32 0.0198(5) 0.0226(6) 0.0184(5) 0.0029(4) 0.0000(4) 0.0016(4) C33 0.0195(5) 0.0188(5) 0.0238(5) 0.0032(4) 0.0022(4) 0.0005(4) C34 0.0170(5) 0.0211(6) 0.0216(5) -0.0018(4) 0.0026(4) 0.0001(4) C35 0.0268(6) 0.0251(6) 0.0186(5) 0.0022(4) 0.0002(4) 0.0019(5) C36 0.0288(6) 0.0182(6) 0.0227(5) 0.0042(4) 0.0020(4) 0.0012(5) C37 0.0212(6) 0.0236(6) 0.0235(5) 0.0008(5) 0.0024(4) 0.0020(5) N38 0.0300(6) 0.0304(6) 0.0320(5) -0.0078(5) 0.0019(4) -0.0030(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 N11 C12 1.3401(15) . ? N11 C16 1.3458(15) . ? C12 C13 1.3942(16) . ? C12 C23 1.4764(15) . ? C13 C14 1.3834(16) . ? C13 H13 0.9500 . ? C14 C15 1.3842(17) . ? C14 H14 0.9500 . ? C15 C16 1.3805(17) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? N21 C25 1.3514(15) . ? N21 N22 1.3522(13) . ? N21 C26 1.4572(15) . ? N22 C23 1.3382(15) . ? C23 C24 1.4086(16) . ? C24 C25 1.3708(16) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.5180(15) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C31 C36 1.3952(15) . ? C31 C32 1.3987(16) . ? C32 C33 1.3842(16) . ? C32 H32 0.9500 . ? C33 C34 1.4014(15) . ? C33 H33 0.9500 . ? C34 C35 1.3910(16) . ? C34 C37 1.4420(16) . ? C35 C36 1.3870(16) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 N38 1.1468(16) . ? 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 C12 N11 C16 117.00(10) . . ? N11 C12 C13 122.60(10) . . ? N11 C12 C23 116.72(10) . . ? C13 C12 C23 120.68(10) . . ? C14 C13 C12 119.14(10) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 118.97(11) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C16 C15 C14 118.00(11) . . ? C16 C15 H15 121.0 . . ? C14 C15 H15 121.0 . . ? N11 C16 C15 124.30(11) . . ? N11 C16 H16 117.9 . . ? C15 C16 H16 117.9 . . ? C25 N21 N22 112.18(9) . . ? C25 N21 C26 128.03(10) . . ? N22 N21 C26 119.76(9) . . ? C23 N22 N21 104.70(9) . . ? N22 C23 C24 111.18(10) . . ? N22 C23 C12 120.17(10) . . ? C24 C23 C12 128.63(10) . . ? C25 C24 C23 104.80(10) . . ? C25 C24 H24 127.6 . . ? C23 C24 H24 127.6 . . ? N21 C25 C24 107.13(10) . . ? N21 C25 H25 126.4 . . ? C24 C25 H25 126.4 . . ? N21 C26 C31 113.60(9) . . ? N21 C26 H26A 108.8 . . ? C31 C26 H26A 108.8 . . ? N21 C26 H26B 108.8 . . ? C31 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? C36 C31 C32 119.11(10) . . ? C36 C31 C26 119.75(10) . . ? C32 C31 C26 121.11(10) . . ? C33 C32 C31 120.75(10) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 119.34(10) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? C35 C34 C33 120.52(10) . . ? C35 C34 C37 118.76(10) . . ? C33 C34 C37 120.71(10) . . ? C36 C35 C34 119.48(10) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C35 C36 C31 120.80(11) . . ? C35 C36 H36 119.6 . . ? C31 C36 H36 119.6 . . ? N38 C37 C34 178.08(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 N11 C12 C13 -0.09(16) . . . . ? C16 N11 C12 C23 -179.37(10) . . . . ? N11 C12 C13 C14 0.32(16) . . . . ? C23 C12 C13 C14 179.57(10) . . . . ? C12 C13 C14 C15 -0.18(16) . . . . ? C13 C14 C15 C16 -0.15(16) . . . . ? C12 N11 C16 C15 -0.28(18) . . . . ? C14 C15 C16 N11 0.40(18) . . . . ? C25 N21 N22 C23 -0.33(12) . . . . ? C26 N21 N22 C23 -178.73(9) . . . . ? N21 N22 C23 C24 0.24(12) . . . . ? N21 N22 C23 C12 -178.45(9) . . . . ? N11 C12 C23 N22 -177.28(9) . . . . ? C13 C12 C23 N22 3.43(15) . . . . ? N11 C12 C23 C24 4.29(17) . . . . ? C13 C12 C23 C24 -175.01(11) . . . . ? N22 C23 C24 C25 -0.07(12) . . . . ? C12 C23 C24 C25 178.48(10) . . . . ? N22 N21 C25 C24 0.30(13) . . . . ? C26 N21 C25 C24 178.53(10) . . . . ? C23 C24 C25 N21 -0.13(12) . . . . ? C25 N21 C26 C31 -96.71(13) . . . . ? N22 N21 C26 C31 81.41(12) . . . . ? N21 C26 C31 C36 130.77(11) . . . . ? N21 C26 C31 C32 -51.38(14) . . . . ? C36 C31 C32 C33 -0.28(17) . . . . ? C26 C31 C32 C33 -178.14(10) . . . . ? C31 C32 C33 C34 0.94(16) . . . . ? C32 C33 C34 C35 -0.99(16) . . . . ? C32 C33 C34 C37 178.15(10) . . . . ? C33 C34 C35 C36 0.38(17) . . . . ? C37 C34 C35 C36 -178.78(10) . . . . ? C34 C35 C36 C31 0.30(18) . . . . ? C32 C31 C36 C35 -0.35(17) . . . . ? C26 C31 C36 C35 177.54(11) . . . . ? C35 C34 C37 N38 20(4) . . . . ? C33 C34 C37 N38 -159(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.236 _refine_diff_density_min -0.205 _refine_diff_density_rms 0.037 #===END data_imw1209p21c _database_code_depnum_ccdc_archive 'CCDC 758086' #TrackingRef 'mixed_metal_networks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H14 N4' _chemical_formula_weight 310.35 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.2760(5) _cell_length_b 13.4222(9) _cell_length_c 15.4417(10) _cell_angle_alpha 90.00 _cell_angle_beta 89.253(4) _cell_angle_gamma 90.00 _cell_volume 1507.91(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8655 _cell_measurement_theta_min 2.639 _cell_measurement_theta_max 27.351 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9671 _exptl_absorpt_correction_T_max 0.9834 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23919 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0184 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3070 _reflns_number_gt 2662 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The data was solved by direct methods. Data processing was conducted to a resolution of 0.8 angstroms as the data was only complete to this resolution. 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^)+(0.0369P)^2^+1.1581P] 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_number_reflns 3070 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1086 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 N11 N 0.0167(2) 1.03882(11) 0.10840(9) 0.0275(3) Uani 1 1 d . . . C12 C -0.0641(2) 0.94969(12) 0.12157(10) 0.0233(3) Uani 1 1 d . . . C13 C -0.2523(2) 0.93540(13) 0.11274(10) 0.0257(4) Uani 1 1 d . . . H13 H -0.3052 0.8716 0.1224 0.031 Uiso 1 1 calc R . . C14 C -0.3615(2) 1.01505(14) 0.08980(11) 0.0297(4) Uani 1 1 d . . . H14 H -0.4905 1.0071 0.0842 0.036 Uiso 1 1 calc R . . C15 C -0.2796(3) 1.10640(14) 0.07515(12) 0.0315(4) Uani 1 1 d . . . H15 H -0.3506 1.1625 0.0586 0.038 Uiso 1 1 calc R . . C16 C -0.0926(3) 1.11419(13) 0.08507(12) 0.0310(4) Uani 1 1 d . . . H16 H -0.0372 1.1772 0.0747 0.037 Uiso 1 1 calc R . . N21 N 0.14529(19) 0.72114(10) 0.17793(9) 0.0237(3) Uani 1 1 d . . . N22 N 0.00104(19) 0.77347(10) 0.14729(8) 0.0236(3) Uani 1 1 d . . . C23 C 0.0581(2) 0.86848(12) 0.14859(10) 0.0231(3) Uani 1 1 d . . . C24 C 0.2379(2) 0.87622(13) 0.18007(11) 0.0265(4) Uani 1 1 d . . . H24 H 0.3084 0.9351 0.1875 0.032 Uiso 1 1 calc R . . C25 C 0.2892(2) 0.78021(13) 0.19768(11) 0.0267(4) Uani 1 1 d . . . H25 H 0.4042 0.7591 0.2196 0.032 Uiso 1 1 calc R . . C26 C 0.1421(2) 0.61307(12) 0.17730(10) 0.0240(3) Uani 1 1 d . . . H26A H 0.0172 0.5901 0.1939 0.029 Uiso 1 1 calc R . . H26B H 0.2283 0.5881 0.2213 0.029 Uiso 1 1 calc R . . C31 C 0.1940(2) 0.56834(12) 0.08969(10) 0.0213(3) Uani 1 1 d . . . C32 C 0.2093(2) 0.62607(12) 0.01672(11) 0.0237(3) Uani 1 1 d . . . H32 H 0.1855 0.6955 0.0206 0.028 Uiso 1 1 calc R . . C33 C 0.2596(2) 0.58440(12) -0.06377(10) 0.0234(3) Uani 1 1 d . . . H33 H 0.2693 0.6255 -0.1137 0.028 Uiso 1 1 calc R . . C34 C 0.2945(2) 0.48404(12) -0.07000(10) 0.0214(3) Uani 1 1 d . . . C35 C 0.2786(2) 0.42042(12) 0.00385(10) 0.0210(3) Uani 1 1 d . . . C36 C 0.2275(2) 0.46367(12) 0.08456(10) 0.0210(3) Uani 1 1 d . . . C41 C 0.3117(2) 0.31662(12) -0.00123(11) 0.0249(4) Uani 1 1 d . . . H41 H 0.3456 0.2875 -0.0552 0.030 Uiso 1 1 calc R . . C42 C 0.2953(2) 0.25781(13) 0.07092(12) 0.0276(4) Uani 1 1 d . . . H42 H 0.3173 0.1882 0.0667 0.033 Uiso 1 1 calc R . . C43 C 0.2459(2) 0.30004(13) 0.15114(11) 0.0278(4) Uani 1 1 d . . . H43 H 0.2360 0.2590 0.2011 0.033 Uiso 1 1 calc R . . C44 C 0.2122(2) 0.39995(13) 0.15767(10) 0.0253(4) Uani 1 1 d . . . H44 H 0.1779 0.4273 0.2123 0.030 Uiso 1 1 calc R . . C51 C 0.3511(2) 0.44158(12) -0.15176(11) 0.0237(3) Uani 1 1 d . . . N52 N 0.3961(2) 0.40687(11) -0.21703(9) 0.0286(3) 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 N11 0.0288(8) 0.0257(8) 0.0281(7) 0.0016(6) 0.0021(6) -0.0020(6) C12 0.0288(9) 0.0244(8) 0.0167(7) -0.0039(6) 0.0037(6) -0.0014(7) C13 0.0308(9) 0.0260(8) 0.0203(8) -0.0010(6) 0.0009(7) -0.0052(7) C14 0.0267(9) 0.0372(10) 0.0253(8) 0.0012(7) -0.0006(7) -0.0032(7) C15 0.0321(10) 0.0312(9) 0.0312(9) 0.0072(7) 0.0000(7) 0.0026(8) C16 0.0330(10) 0.0253(9) 0.0346(9) 0.0041(7) 0.0005(8) -0.0028(7) N21 0.0245(7) 0.0241(7) 0.0224(7) -0.0035(5) 0.0009(5) 0.0001(6) N22 0.0248(7) 0.0249(7) 0.0210(7) -0.0028(5) 0.0020(5) 0.0007(6) C23 0.0270(9) 0.0240(8) 0.0180(7) -0.0037(6) 0.0044(6) -0.0014(6) C24 0.0272(9) 0.0265(9) 0.0258(8) -0.0062(7) 0.0022(7) -0.0031(7) C25 0.0235(8) 0.0313(9) 0.0254(8) -0.0056(7) -0.0002(7) -0.0005(7) C26 0.0259(8) 0.0231(8) 0.0230(8) -0.0011(6) 0.0013(6) -0.0001(6) C31 0.0182(8) 0.0237(8) 0.0221(8) -0.0013(6) -0.0002(6) -0.0013(6) C32 0.0250(8) 0.0200(8) 0.0261(8) -0.0007(6) 0.0006(6) 0.0007(6) C33 0.0238(8) 0.0244(8) 0.0220(8) 0.0033(6) 0.0004(6) -0.0010(6) C34 0.0187(8) 0.0238(8) 0.0218(8) -0.0024(6) -0.0003(6) -0.0015(6) C35 0.0175(8) 0.0225(8) 0.0230(8) -0.0010(6) -0.0019(6) -0.0027(6) C36 0.0188(8) 0.0218(8) 0.0223(8) -0.0011(6) -0.0012(6) -0.0017(6) C41 0.0226(8) 0.0236(8) 0.0284(8) -0.0040(7) -0.0003(7) -0.0012(6) C42 0.0247(9) 0.0208(8) 0.0373(10) 0.0011(7) -0.0011(7) -0.0010(7) C43 0.0299(9) 0.0259(9) 0.0278(9) 0.0070(7) -0.0005(7) -0.0026(7) C44 0.0286(9) 0.0263(8) 0.0209(8) 0.0007(6) 0.0008(6) -0.0011(7) C51 0.0226(8) 0.0234(8) 0.0252(8) 0.0026(7) -0.0019(6) -0.0014(6) N52 0.0327(8) 0.0294(8) 0.0238(7) -0.0022(6) 0.0005(6) 0.0018(6) _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 N11 C16 1.339(2) . ? N11 C12 1.347(2) . ? C12 C13 1.392(2) . ? C12 C23 1.471(2) . ? C13 C14 1.381(3) . ? C13 H13 0.9500 . ? C14 C15 1.381(3) . ? C14 H14 0.9500 . ? C15 C16 1.375(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? N21 C25 1.351(2) . ? N21 N22 1.3534(19) . ? N21 C26 1.451(2) . ? N22 C23 1.341(2) . ? C23 C24 1.405(2) . ? C24 C25 1.370(2) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.523(2) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C31 C32 1.371(2) . ? C31 C36 1.428(2) . ? C32 C33 1.407(2) . ? C32 H32 0.9500 . ? C33 C34 1.374(2) . ? C33 H33 0.9500 . ? C34 C35 1.428(2) . ? C34 C51 1.441(2) . ? C35 C41 1.416(2) . ? C35 C36 1.420(2) . ? C36 C44 1.419(2) . ? C41 C42 1.369(2) . ? C41 H41 0.9500 . ? C42 C43 1.405(2) . ? C42 H42 0.9500 . ? C43 C44 1.367(2) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C51 N52 1.154(2) . ? 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 C16 N11 C12 116.90(15) . . ? N11 C12 C13 122.37(16) . . ? N11 C12 C23 115.92(15) . . ? C13 C12 C23 121.68(15) . . ? C14 C13 C12 119.25(16) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 118.77(17) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? C16 C15 C14 118.34(17) . . ? C16 C15 H15 120.8 . . ? C14 C15 H15 120.8 . . ? N11 C16 C15 124.35(17) . . ? N11 C16 H16 117.8 . . ? C15 C16 H16 117.8 . . ? C25 N21 N22 112.40(14) . . ? C25 N21 C26 126.92(15) . . ? N22 N21 C26 120.25(13) . . ? C23 N22 N21 104.26(13) . . ? N22 C23 C24 111.43(15) . . ? N22 C23 C12 120.79(15) . . ? C24 C23 C12 127.76(15) . . ? C25 C24 C23 104.85(15) . . ? C25 C24 H24 127.6 . . ? C23 C24 H24 127.6 . . ? N21 C25 C24 107.06(15) . . ? N21 C25 H25 126.5 . . ? C24 C25 H25 126.5 . . ? N21 C26 C31 113.34(13) . . ? N21 C26 H26A 108.9 . . ? C31 C26 H26A 108.9 . . ? N21 C26 H26B 108.9 . . ? C31 C26 H26B 108.9 . . ? H26A C26 H26B 107.7 . . ? C32 C31 C36 119.90(14) . . ? C32 C31 C26 121.59(14) . . ? C36 C31 C26 118.50(14) . . ? C31 C32 C33 121.25(15) . . ? C31 C32 H32 119.4 . . ? C33 C32 H32 119.4 . . ? C34 C33 C32 119.82(15) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 121.16(14) . . ? C33 C34 C51 119.99(15) . . ? C35 C34 C51 118.84(14) . . ? C41 C35 C36 119.56(15) . . ? C41 C35 C34 122.16(15) . . ? C36 C35 C34 118.28(14) . . ? C44 C36 C35 117.95(14) . . ? C44 C36 C31 122.49(14) . . ? C35 C36 C31 119.57(14) . . ? C42 C41 C35 120.61(15) . . ? C42 C41 H41 119.7 . . ? C35 C41 H41 119.7 . . ? C41 C42 C43 120.23(16) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C44 C43 C42 120.30(15) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C43 C44 C36 121.35(15) . . ? C43 C44 H44 119.3 . . ? C36 C44 H44 119.3 . . ? N52 C51 C34 179.49(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 N11 C12 C13 -0.8(2) . . . . ? C16 N11 C12 C23 -178.98(14) . . . . ? N11 C12 C13 C14 -0.1(2) . . . . ? C23 C12 C13 C14 177.98(15) . . . . ? C12 C13 C14 C15 0.9(2) . . . . ? C13 C14 C15 C16 -0.7(3) . . . . ? C12 N11 C16 C15 1.0(3) . . . . ? C14 C15 C16 N11 -0.2(3) . . . . ? C25 N21 N22 C23 -0.27(17) . . . . ? C26 N21 N22 C23 -173.34(13) . . . . ? N21 N22 C23 C24 -0.07(17) . . . . ? N21 N22 C23 C12 -178.46(13) . . . . ? N11 C12 C23 N22 -166.99(14) . . . . ? C13 C12 C23 N22 14.8(2) . . . . ? N11 C12 C23 C24 14.9(2) . . . . ? C13 C12 C23 C24 -163.29(16) . . . . ? N22 C23 C24 C25 0.37(19) . . . . ? C12 C23 C24 C25 178.61(15) . . . . ? N22 N21 C25 C24 0.51(19) . . . . ? C26 N21 C25 C24 173.02(15) . . . . ? C23 C24 C25 N21 -0.51(18) . . . . ? C25 N21 C26 C31 -90.75(19) . . . . ? N22 N21 C26 C31 81.23(18) . . . . ? N21 C26 C31 C32 -10.8(2) . . . . ? N21 C26 C31 C36 169.09(14) . . . . ? C36 C31 C32 C33 -0.7(2) . . . . ? C26 C31 C32 C33 179.21(15) . . . . ? C31 C32 C33 C34 -0.1(2) . . . . ? C32 C33 C34 C35 0.7(2) . . . . ? C32 C33 C34 C51 -178.22(15) . . . . ? C33 C34 C35 C41 179.20(15) . . . . ? C51 C34 C35 C41 -1.8(2) . . . . ? C33 C34 C35 C36 -0.6(2) . . . . ? C51 C34 C35 C36 178.33(14) . . . . ? C41 C35 C36 C44 0.2(2) . . . . ? C34 C35 C36 C44 -179.95(14) . . . . ? C41 C35 C36 C31 -179.95(15) . . . . ? C34 C35 C36 C31 -0.1(2) . . . . ? C32 C31 C36 C44 -179.41(15) . . . . ? C26 C31 C36 C44 0.7(2) . . . . ? C32 C31 C36 C35 0.7(2) . . . . ? C26 C31 C36 C35 -179.13(14) . . . . ? C36 C35 C41 C42 -0.2(2) . . . . ? C34 C35 C41 C42 179.99(15) . . . . ? C35 C41 C42 C43 -0.2(2) . . . . ? C41 C42 C43 C44 0.6(3) . . . . ? C42 C43 C44 C36 -0.6(3) . . . . ? C35 C36 C44 C43 0.2(2) . . . . ? C31 C36 C44 C43 -179.66(16) . . . . ? C33 C34 C51 N52 -162(21) . . . . ? C35 C34 C51 N52 19(21) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.254 _refine_diff_density_min -0.199 _refine_diff_density_rms 0.045 #===END data_imw1182P21c _database_code_depnum_ccdc_archive 'CCDC 758087' #TrackingRef 'mixed_metal_networks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H12 Ag N5 O3' _chemical_formula_weight 430.18 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' Ag Ag -0.8971 1.1015 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.6667(5) _cell_length_b 8.6020(5) _cell_length_c 21.8779(14) _cell_angle_alpha 90.00 _cell_angle_beta 96.882(3) _cell_angle_gamma 90.00 _cell_volume 1619.27(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8948 _cell_measurement_theta_min 2.547 _cell_measurement_theta_max 27.516 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.765 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 1.271 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6303 _exptl_absorpt_correction_T_max 0.7851 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16408 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.52 _reflns_number_total 3716 _reflns_number_gt 3335 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The data was solved by direct methods. All hydrogen atoms were added in calculated positions. 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^)+(0.0326P)^2^+1.8428P] 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_number_reflns 3716 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0752 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.001 _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 Ag1 Ag 0.35275(2) 0.91895(2) 0.302590(10) 0.03256(8) Uani 1 1 d . . . N11 N 0.3674(2) 1.0785(2) 0.38959(11) 0.0301(5) Uani 1 1 d . . . C12 C 0.2384(3) 1.0864(3) 0.41820(11) 0.0232(5) Uani 1 1 d . . . C13 C 0.2330(3) 1.1690(3) 0.47252(11) 0.0295(5) Uani 1 1 d . . . H13 H 0.1397 1.1741 0.4912 0.035 Uiso 1 1 calc R . . C14 C 0.3665(4) 1.2439(4) 0.49885(13) 0.0430(7) Uani 1 1 d . . . H14 H 0.3668 1.2996 0.5364 0.052 Uiso 1 1 calc R . . C15 C 0.4985(4) 1.2359(4) 0.46959(17) 0.0518(8) Uani 1 1 d . . . H15 H 0.5912 1.2868 0.4865 0.062 Uiso 1 1 calc R . . C16 C 0.4943(3) 1.1534(4) 0.41560(16) 0.0448(7) Uani 1 1 d . . . H16 H 0.5858 1.1493 0.3957 0.054 Uiso 1 1 calc R . . N21 N -0.0308(2) 0.8476(2) 0.32652(9) 0.0206(4) Uani 1 1 d . . . N22 N 0.1129(2) 0.9077(2) 0.34147(9) 0.0205(4) Uani 1 1 d . . . C23 C 0.1001(3) 1.0030(2) 0.38882(10) 0.0201(4) Uani 1 1 d . . . C24 C -0.0527(3) 1.0049(3) 0.40384(11) 0.0231(4) Uani 1 1 d . . . H24 H -0.0921 1.0633 0.4354 0.028 Uiso 1 1 calc R . . C25 C -0.1329(3) 0.9041(3) 0.36295(11) 0.0248(5) Uani 1 1 d . . . H25 H -0.2401 0.8788 0.3607 0.030 Uiso 1 1 calc R . . C26 C -0.0598(3) 0.7409(2) 0.27408(11) 0.0232(4) Uani 1 1 d . . . H26A H -0.1565 0.6818 0.2774 0.028 Uiso 1 1 calc R . . H26B H 0.0269 0.6657 0.2751 0.028 Uiso 1 1 calc R . . C31 C -0.0751(3) 0.8282(2) 0.21366(10) 0.0199(4) Uani 1 1 d . . . C32 C 0.0534(3) 0.8454(2) 0.18197(10) 0.0206(4) Uani 1 1 d . . . H32 H 0.1487 0.7963 0.1970 0.025 Uiso 1 1 calc R . . C33 C 0.0439(3) 0.9336(2) 0.12855(10) 0.0212(4) Uani 1 1 d . . . H33 H 0.1321 0.9459 0.1071 0.025 Uiso 1 1 calc R . . C34 C -0.0966(3) 1.0039(3) 0.10685(10) 0.0216(4) Uani 1 1 d . . . C35 C -0.2280(3) 0.9850(3) 0.13766(11) 0.0240(5) Uani 1 1 d . . . H35 H -0.3238 1.0324 0.1222 0.029 Uiso 1 1 calc R . . C36 C -0.2169(3) 0.8964(3) 0.19092(11) 0.0233(5) Uani 1 1 d . . . H36 H -0.3055 0.8819 0.2120 0.028 Uiso 1 1 calc R . . C37 C -0.1074(3) 1.1008(3) 0.05273(11) 0.0247(5) Uani 1 1 d . . . N38 N -0.1178(2) 1.1797(3) 0.00995(9) 0.0301(5) Uani 1 1 d . . . O1 O 0.5338(2) 0.7106(2) 0.34262(10) 0.0422(5) Uani 1 1 d . . . O2 O 0.4510(3) 0.6629(3) 0.24705(10) 0.0449(5) Uani 1 1 d . . . O3 O 0.3812(2) 1.0093(2) 0.20284(9) 0.0367(4) Uani 1 1 d . . . N1 N 0.5345(2) 0.6281(2) 0.29532(11) 0.0294(5) 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 Ag1 0.03026(12) 0.03171(12) 0.03826(13) -0.00234(8) 0.01458(8) 0.00335(8) N11 0.0223(10) 0.0295(11) 0.0382(12) -0.0014(9) 0.0027(9) 0.0002(8) C12 0.0234(11) 0.0198(10) 0.0259(11) 0.0047(9) 0.0010(9) 0.0016(8) C13 0.0323(13) 0.0321(13) 0.0237(12) 0.0006(10) 0.0020(10) -0.0007(10) C14 0.0449(16) 0.0482(17) 0.0327(15) -0.0069(13) -0.0089(12) -0.0050(14) C15 0.0297(14) 0.059(2) 0.063(2) -0.0154(17) -0.0109(14) -0.0079(14) C16 0.0229(13) 0.0506(18) 0.060(2) -0.0108(15) 0.0023(12) -0.0037(12) N21 0.0235(9) 0.0160(8) 0.0232(9) 0.0018(7) 0.0065(7) -0.0031(7) N22 0.0226(9) 0.0163(8) 0.0231(9) 0.0040(7) 0.0052(7) 0.0000(7) C23 0.0244(11) 0.0153(9) 0.0211(11) 0.0053(8) 0.0045(8) 0.0003(8) C24 0.0268(11) 0.0204(10) 0.0235(11) 0.0013(9) 0.0091(9) -0.0003(9) C25 0.0249(11) 0.0235(11) 0.0274(12) 0.0025(9) 0.0092(9) -0.0032(9) C26 0.0302(12) 0.0134(9) 0.0266(12) 0.0006(8) 0.0064(9) -0.0023(9) C31 0.0265(11) 0.0116(9) 0.0221(11) -0.0030(8) 0.0051(8) -0.0021(8) C32 0.0233(11) 0.0164(10) 0.0220(11) -0.0049(8) 0.0028(8) 0.0007(8) C33 0.0238(11) 0.0211(10) 0.0195(10) -0.0062(8) 0.0063(8) -0.0010(8) C34 0.0277(11) 0.0198(10) 0.0178(10) -0.0048(8) 0.0046(9) 0.0003(9) C35 0.0243(11) 0.0226(11) 0.0251(11) -0.0031(9) 0.0035(9) 0.0047(9) C36 0.0241(11) 0.0197(10) 0.0272(12) -0.0022(8) 0.0077(9) 0.0000(8) C37 0.0265(11) 0.0257(11) 0.0223(11) -0.0055(9) 0.0044(9) 0.0036(9) N38 0.0329(11) 0.0351(11) 0.0229(10) 0.0021(9) 0.0064(8) 0.0055(9) O1 0.0316(10) 0.0368(10) 0.0601(13) -0.0219(10) 0.0133(9) -0.0052(8) O2 0.0482(12) 0.0454(12) 0.0445(12) 0.0152(10) 0.0198(10) 0.0176(10) O3 0.0337(10) 0.0313(10) 0.0460(11) 0.0024(8) 0.0081(8) -0.0111(8) N1 0.0222(10) 0.0219(10) 0.0475(14) -0.0023(9) 0.0176(9) -0.0042(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 Ag1 N11 2.337(2) . ? Ag1 N22 2.3401(19) . ? Ag1 O3 2.357(2) . ? Ag1 O1 2.472(2) . ? N11 C16 1.341(3) . ? N11 C12 1.347(3) . ? C12 C13 1.390(3) . ? C12 C23 1.476(3) . ? C13 C14 1.388(4) . ? C13 H13 0.9500 . ? C14 C15 1.378(5) . ? C14 H14 0.9500 . ? C15 C16 1.375(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? N21 C25 1.351(3) . ? N21 N22 1.352(3) . ? N21 C26 1.467(3) . ? N22 C23 1.336(3) . ? C23 C24 1.402(3) . ? C24 C25 1.374(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.512(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C31 C32 1.389(3) . ? C31 C36 1.398(3) . ? C32 C33 1.388(3) . ? C32 H32 0.9500 . ? C33 C34 1.391(3) . ? C33 H33 0.9500 . ? C34 C35 1.401(3) . ? C34 C37 1.442(3) . ? C35 C36 1.386(3) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 N38 1.151(3) . ? O1 N1 1.255(3) . ? O2 N1 1.243(3) . ? O3 N1 1.254(3) 2_655 ? N1 O3 1.254(3) 2_645 ? 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 N11 Ag1 N22 72.07(7) . . ? N11 Ag1 O3 123.97(7) . . ? N22 Ag1 O3 123.10(7) . . ? N11 Ag1 O1 99.61(7) . . ? N22 Ag1 O1 113.27(7) . . ? O3 Ag1 O1 115.77(7) . . ? C16 N11 C12 117.6(2) . . ? C16 N11 Ag1 126.11(19) . . ? C12 N11 Ag1 116.16(16) . . ? N11 C12 C13 122.5(2) . . ? N11 C12 C23 116.7(2) . . ? C13 C12 C23 120.8(2) . . ? C14 C13 C12 118.7(3) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C15 C14 C13 118.8(3) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C16 C15 C14 119.1(3) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? N11 C16 C15 123.3(3) . . ? N11 C16 H16 118.4 . . ? C15 C16 H16 118.4 . . ? C25 N21 N22 111.69(18) . . ? C25 N21 C26 128.6(2) . . ? N22 N21 C26 119.68(18) . . ? C23 N22 N21 105.22(18) . . ? C23 N22 Ag1 114.62(14) . . ? N21 N22 Ag1 139.49(14) . . ? N22 C23 C24 111.0(2) . . ? N22 C23 C12 119.8(2) . . ? C24 C23 C12 129.2(2) . . ? C25 C24 C23 105.0(2) . . ? C25 C24 H24 127.5 . . ? C23 C24 H24 127.5 . . ? N21 C25 C24 107.2(2) . . ? N21 C25 H25 126.4 . . ? C24 C25 H25 126.4 . . ? N21 C26 C31 111.21(17) . . ? N21 C26 H26A 109.4 . . ? C31 C26 H26A 109.4 . . ? N21 C26 H26B 109.4 . . ? C31 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C32 C31 C36 120.1(2) . . ? C32 C31 C26 119.8(2) . . ? C36 C31 C26 120.0(2) . . ? C33 C32 C31 120.5(2) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 119.1(2) . . ? C32 C33 H33 120.4 . . ? C34 C33 H33 120.4 . . ? C33 C34 C35 120.9(2) . . ? C33 C34 C37 120.0(2) . . ? C35 C34 C37 119.1(2) . . ? C36 C35 C34 119.3(2) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C35 C36 C31 120.0(2) . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? N38 C37 C34 178.9(3) . . ? N1 O1 Ag1 100.56(17) . . ? N1 O3 Ag1 111.36(16) 2_655 . ? O2 N1 O3 120.1(2) . 2_645 ? O2 N1 O1 120.3(2) . . ? O3 N1 O1 119.6(2) 2_645 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N22 Ag1 N11 C16 175.1(3) . . . . ? O3 Ag1 N11 C16 -66.6(3) . . . . ? O1 Ag1 N11 C16 63.7(2) . . . . ? N22 Ag1 N11 C12 -0.08(16) . . . . ? O3 Ag1 N11 C12 118.21(17) . . . . ? O1 Ag1 N11 C12 -111.57(17) . . . . ? C16 N11 C12 C13 0.4(4) . . . . ? Ag1 N11 C12 C13 176.05(18) . . . . ? C16 N11 C12 C23 -180.0(2) . . . . ? Ag1 N11 C12 C23 -4.3(3) . . . . ? N11 C12 C13 C14 -1.2(4) . . . . ? C23 C12 C13 C14 179.2(2) . . . . ? C12 C13 C14 C15 1.2(4) . . . . ? C13 C14 C15 C16 -0.4(5) . . . . ? C12 N11 C16 C15 0.4(5) . . . . ? Ag1 N11 C16 C15 -174.8(3) . . . . ? C14 C15 C16 N11 -0.4(6) . . . . ? C25 N21 N22 C23 0.6(2) . . . . ? C26 N21 N22 C23 177.79(18) . . . . ? C25 N21 N22 Ag1 -168.87(17) . . . . ? C26 N21 N22 Ag1 8.3(3) . . . . ? N11 Ag1 N22 C23 4.84(15) . . . . ? O3 Ag1 N22 C23 -114.50(15) . . . . ? O1 Ag1 N22 C23 97.81(15) . . . . ? N11 Ag1 N22 N21 173.6(2) . . . . ? O3 Ag1 N22 N21 54.3(2) . . . . ? O1 Ag1 N22 N21 -93.4(2) . . . . ? N21 N22 C23 C24 -0.6(2) . . . . ? Ag1 N22 C23 C24 171.91(14) . . . . ? N21 N22 C23 C12 178.43(18) . . . . ? Ag1 N22 C23 C12 -9.1(2) . . . . ? N11 C12 C23 N22 9.2(3) . . . . ? C13 C12 C23 N22 -171.1(2) . . . . ? N11 C12 C23 C24 -172.0(2) . . . . ? C13 C12 C23 C24 7.7(4) . . . . ? N22 C23 C24 C25 0.4(3) . . . . ? C12 C23 C24 C25 -178.5(2) . . . . ? N22 N21 C25 C24 -0.4(3) . . . . ? C26 N21 C25 C24 -177.3(2) . . . . ? C23 C24 C25 N21 0.0(2) . . . . ? C25 N21 C26 C31 99.2(3) . . . . ? N22 N21 C26 C31 -77.5(2) . . . . ? N21 C26 C31 C32 95.1(2) . . . . ? N21 C26 C31 C36 -82.6(2) . . . . ? C36 C31 C32 C33 1.9(3) . . . . ? C26 C31 C32 C33 -175.81(19) . . . . ? C31 C32 C33 C34 -0.5(3) . . . . ? C32 C33 C34 C35 -0.9(3) . . . . ? C32 C33 C34 C37 177.7(2) . . . . ? C33 C34 C35 C36 0.8(3) . . . . ? C37 C34 C35 C36 -177.8(2) . . . . ? C34 C35 C36 C31 0.6(3) . . . . ? C32 C31 C36 C35 -1.9(3) . . . . ? C26 C31 C36 C35 175.7(2) . . . . ? C33 C34 C37 N38 -146(15) . . . . ? C35 C34 C37 N38 32(15) . . . . ? N11 Ag1 O1 N1 -176.34(14) . . . . ? N22 Ag1 O1 N1 109.15(14) . . . . ? O3 Ag1 O1 N1 -41.03(16) . . . . ? N11 Ag1 O3 N1 27.90(19) . . . 2_655 ? N22 Ag1 O3 N1 117.67(15) . . . 2_655 ? O1 Ag1 O3 N1 -95.38(16) . . . 2_655 ? Ag1 O1 N1 O2 -2.5(2) . . . . ? Ag1 O1 N1 O3 178.30(18) . . . 2_645 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.192 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.074 #===END data_imw1202p21c _database_code_depnum_ccdc_archive 'CCDC 758088' #TrackingRef 'mixed_metal_networks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H28 Ag2 N10 O6' _chemical_formula_weight 960.46 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.5051(4) _cell_length_b 18.8729(9) _cell_length_c 12.8752(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.361(3) _cell_angle_gamma 90.00 _cell_volume 1812.45(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9874 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 26.43 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.760 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 1.146 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5980 _exptl_absorpt_correction_T_max 0.9886 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29358 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 26.36 _reflns_number_total 3713 _reflns_number_gt 3179 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The data was solved by direct methods. Data processing was conducted to a resolution of 0.8 angstroms as the data was only complete to this resolution. The oxygen atoms of the nitrate anion (O1 > O3) beneffited from the application of displacement restraints to their isotropic and anisotropic thermal parameters. 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^)+(0.0244P)^2^+2.0264P] 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_number_reflns 3713 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0597 _refine_ls_wR_factor_gt 0.0550 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.001 _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 Ag1 Ag 0.28910(2) 0.491034(9) 0.285610(14) 0.02311(7) Uani 1 1 d . . . N11 N 0.2612(2) 0.46236(10) 0.46181(15) 0.0197(4) Uani 1 1 d . . . C12 C 0.2448(3) 0.51751(12) 0.52651(17) 0.0172(4) Uani 1 1 d . . . C13 C 0.1915(3) 0.50839(13) 0.62599(18) 0.0217(5) Uani 1 1 d . . . H13 H 0.1803 0.5480 0.6704 0.026 Uiso 1 1 calc R . . C14 C 0.1551(3) 0.44059(13) 0.65879(19) 0.0242(5) Uani 1 1 d . . . H14 H 0.1188 0.4330 0.7263 0.029 Uiso 1 1 calc R . . C15 C 0.1720(3) 0.38421(13) 0.59281(19) 0.0249(5) Uani 1 1 d . . . H15 H 0.1470 0.3373 0.6137 0.030 Uiso 1 1 calc R . . C16 C 0.2263(3) 0.39729(12) 0.49550(19) 0.0227(5) Uani 1 1 d . . . H16 H 0.2394 0.3582 0.4504 0.027 Uiso 1 1 calc R . . N21 N 0.3527(2) 0.66192(9) 0.37024(14) 0.0179(4) Uani 1 1 d . . . N22 N 0.3294(2) 0.59238(9) 0.38730(14) 0.0164(4) Uani 1 1 d . . . C23 C 0.2840(3) 0.58754(12) 0.48506(17) 0.0163(4) Uani 1 1 d . . . C24 C 0.2800(3) 0.65518(12) 0.53054(18) 0.0211(5) Uani 1 1 d . . . H24 H 0.2523 0.6666 0.5988 0.025 Uiso 1 1 calc R . . C25 C 0.3246(3) 0.70120(12) 0.45500(18) 0.0212(5) Uani 1 1 d . . . H25 H 0.3341 0.7513 0.4610 0.025 Uiso 1 1 calc R . . C26 C 0.4173(3) 0.68525(12) 0.27265(17) 0.0186(4) Uani 1 1 d . . . H26A H 0.5442 0.6709 0.2726 0.022 Uiso 1 1 calc R . . H26B H 0.4118 0.7376 0.2687 0.022 Uiso 1 1 calc R . . C31 C 0.3084(3) 0.65431(11) 0.17767(17) 0.0170(4) Uani 1 1 d . . . C32 C 0.3867(3) 0.60573(12) 0.11769(18) 0.0191(5) Uani 1 1 d . . . H32 H 0.5071 0.5916 0.1377 0.023 Uiso 1 1 calc R . . C33 C 0.2929(3) 0.57652(12) 0.02735(18) 0.0213(5) Uani 1 1 d . . . H33 H 0.3499 0.5434 -0.0137 0.026 Uiso 1 1 calc R . . C34 C 0.1185(3) 0.59613(12) -0.00123(17) 0.0197(5) Uani 1 1 d . . . C35 C 0.0291(3) 0.64559(12) 0.05887(17) 0.0185(4) Uani 1 1 d . . . C36 C 0.1264(3) 0.67541(11) 0.14941(17) 0.0166(4) Uani 1 1 d . . . C37 C -0.0224(3) 0.43410(13) 0.09355(18) 0.0228(5) Uani 1 1 d . . . N38 N 0.0592(3) 0.45865(12) 0.16502(16) 0.0275(5) Uani 1 1 d . . . C41 C -0.1520(3) 0.66616(13) 0.03112(19) 0.0236(5) Uani 1 1 d . . . H41 H -0.2180 0.6466 -0.0294 0.028 Uiso 1 1 calc R . . C42 C -0.2317(3) 0.71388(13) 0.0911(2) 0.0275(5) Uani 1 1 d . . . H42 H -0.3534 0.7267 0.0724 0.033 Uiso 1 1 calc R . . C43 C -0.1359(3) 0.74414(13) 0.17996(19) 0.0242(5) Uani 1 1 d . . . H43 H -0.1929 0.7775 0.2205 0.029 Uiso 1 1 calc R . . C44 C 0.0392(3) 0.72583(12) 0.20851(18) 0.0200(5) Uani 1 1 d . . . H44 H 0.1031 0.7470 0.2684 0.024 Uiso 1 1 calc R . . O1 O 0.6763(2) 0.35377(9) 0.18789(15) 0.0305(4) Uani 1 1 d . . . O2 O 0.4229(3) 0.35655(10) 0.25205(18) 0.0421(5) Uani 1 1 d . . . O3 O 0.5220(2) 0.45129(8) 0.18466(13) 0.0263(4) Uani 1 1 d . . . N1 N 0.5396(2) 0.38642(10) 0.20719(15) 0.0199(4) 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 Ag1 0.03011(11) 0.02286(10) 0.01668(10) -0.00565(7) 0.00403(7) 0.00152(7) N11 0.0201(9) 0.0210(10) 0.0177(10) -0.0014(8) -0.0001(7) 0.0016(8) C12 0.0125(10) 0.0222(11) 0.0163(11) -0.0003(8) -0.0015(8) 0.0012(8) C13 0.0189(11) 0.0289(12) 0.0174(11) -0.0031(9) 0.0022(9) 0.0021(9) C14 0.0196(11) 0.0343(13) 0.0192(12) 0.0054(10) 0.0044(9) 0.0006(10) C15 0.0213(12) 0.0247(13) 0.0279(13) 0.0072(10) -0.0012(10) -0.0014(9) C16 0.0245(12) 0.0189(11) 0.0237(12) -0.0002(9) -0.0006(10) 0.0011(9) N21 0.0199(9) 0.0171(9) 0.0160(10) -0.0010(7) -0.0006(7) -0.0013(7) N22 0.0167(9) 0.0169(9) 0.0154(9) -0.0015(7) 0.0011(7) -0.0007(7) C23 0.0140(10) 0.0214(11) 0.0131(11) -0.0026(8) -0.0008(8) 0.0010(8) C24 0.0245(11) 0.0229(12) 0.0160(11) -0.0054(9) 0.0022(9) 0.0025(9) C25 0.0241(12) 0.0177(11) 0.0209(12) -0.0062(9) -0.0011(9) 0.0008(9) C26 0.0182(11) 0.0192(11) 0.0183(11) 0.0023(9) 0.0018(9) -0.0022(8) C31 0.0169(10) 0.0173(11) 0.0173(11) 0.0035(8) 0.0036(8) -0.0022(8) C32 0.0166(10) 0.0199(11) 0.0210(12) 0.0026(9) 0.0038(9) 0.0001(8) C33 0.0255(12) 0.0205(11) 0.0189(12) -0.0006(9) 0.0068(9) -0.0006(9) C34 0.0240(11) 0.0209(12) 0.0143(11) 0.0023(8) 0.0028(9) -0.0057(9) C35 0.0187(11) 0.0206(11) 0.0161(11) 0.0051(9) 0.0021(9) -0.0030(9) C36 0.0191(11) 0.0152(10) 0.0162(11) 0.0052(8) 0.0050(8) -0.0005(8) C37 0.0239(12) 0.0250(12) 0.0202(12) 0.0022(9) 0.0063(10) -0.0036(9) N38 0.0271(11) 0.0336(12) 0.0220(11) -0.0019(9) 0.0032(9) -0.0045(9) C41 0.0195(11) 0.0262(13) 0.0244(13) 0.0048(10) -0.0008(9) -0.0031(9) C42 0.0168(11) 0.0286(13) 0.0369(15) 0.0106(11) 0.0019(10) 0.0033(9) C43 0.0231(12) 0.0217(12) 0.0294(13) 0.0065(10) 0.0099(10) 0.0053(9) C44 0.0227(11) 0.0183(11) 0.0198(12) 0.0036(9) 0.0064(9) 0.0004(9) O1 0.0317(10) 0.0242(9) 0.0384(11) 0.0047(8) 0.0170(8) 0.0083(7) O2 0.0317(10) 0.0304(10) 0.0685(15) 0.0147(10) 0.0244(10) -0.0011(8) O3 0.0344(9) 0.0180(9) 0.0285(9) 0.0034(7) 0.0121(7) 0.0046(7) N1 0.0215(10) 0.0209(10) 0.0175(10) -0.0001(7) 0.0031(8) -0.0003(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 Ag1 N38 2.273(2) . ? Ag1 N22 2.3187(18) . ? Ag1 N11 2.3641(19) . ? Ag1 O3 2.4106(16) . ? N11 C16 1.338(3) . ? N11 C12 1.347(3) . ? C12 C13 1.394(3) . ? C12 C23 1.467(3) . ? C13 C14 1.384(3) . ? C13 H13 0.9500 . ? C14 C15 1.376(4) . ? C14 H14 0.9500 . ? C15 C16 1.382(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? N21 N22 1.345(3) . ? N21 C25 1.355(3) . ? N21 C26 1.464(3) . ? N22 C23 1.343(3) . ? C23 C24 1.406(3) . ? C24 C25 1.373(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.511(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C31 C32 1.372(3) . ? C31 C36 1.431(3) . ? C32 C33 1.404(3) . ? C32 H32 0.9500 . ? C33 C34 1.371(3) . ? C33 H33 0.9500 . ? C34 C35 1.427(3) . ? C34 C37 1.438(3) 3_565 ? C35 C41 1.421(3) . ? C35 C36 1.421(3) . ? C36 C44 1.423(3) . ? C37 N38 1.146(3) . ? C37 C34 1.438(3) 3_565 ? C41 C42 1.366(4) . ? C41 H41 0.9500 . ? C42 C43 1.404(4) . ? C42 H42 0.9500 . ? C43 C44 1.369(3) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? O1 N1 1.246(2) . ? O2 N1 1.237(3) . ? O3 N1 1.262(2) . ? 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 N38 Ag1 N22 130.48(7) . . ? N38 Ag1 N11 116.91(7) . . ? N22 Ag1 N11 70.54(6) . . ? N38 Ag1 O3 95.10(7) . . ? N22 Ag1 O3 120.27(6) . . ? N11 Ag1 O3 126.36(6) . . ? C16 N11 C12 118.3(2) . . ? C16 N11 Ag1 124.23(15) . . ? C12 N11 Ag1 116.13(15) . . ? N11 C12 C13 121.9(2) . . ? N11 C12 C23 115.80(19) . . ? C13 C12 C23 122.3(2) . . ? C14 C13 C12 118.7(2) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C15 C14 C13 119.5(2) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 118.6(2) . . ? C14 C15 H15 120.7 . . ? C16 C15 H15 120.7 . . ? N11 C16 C15 123.1(2) . . ? N11 C16 H16 118.5 . . ? C15 C16 H16 118.5 . . ? N22 N21 C25 111.58(18) . . ? N22 N21 C26 119.66(17) . . ? C25 N21 C26 128.51(19) . . ? C23 N22 N21 105.68(17) . . ? C23 N22 Ag1 116.25(14) . . ? N21 N22 Ag1 136.37(14) . . ? N22 C23 C24 110.36(19) . . ? N22 C23 C12 118.95(19) . . ? C24 C23 C12 130.7(2) . . ? C25 C24 C23 105.1(2) . . ? C25 C24 H24 127.4 . . ? C23 C24 H24 127.4 . . ? N21 C25 C24 107.2(2) . . ? N21 C25 H25 126.4 . . ? C24 C25 H25 126.4 . . ? N21 C26 C31 112.18(17) . . ? N21 C26 H26A 109.2 . . ? C31 C26 H26A 109.2 . . ? N21 C26 H26B 109.2 . . ? C31 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C32 C31 C36 119.9(2) . . ? C32 C31 C26 119.1(2) . . ? C36 C31 C26 120.93(19) . . ? C31 C32 C33 121.5(2) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? C34 C33 C32 119.5(2) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C33 C34 C35 121.6(2) . . ? C33 C34 C37 119.4(2) . 3_565 ? C35 C34 C37 119.0(2) . 3_565 ? C41 C35 C36 119.2(2) . . ? C41 C35 C34 122.5(2) . . ? C36 C35 C34 118.3(2) . . ? C35 C36 C44 118.6(2) . . ? C35 C36 C31 119.2(2) . . ? C44 C36 C31 122.2(2) . . ? N38 C37 C34 177.5(2) . 3_565 ? C37 N38 Ag1 162.8(2) . . ? C42 C41 C35 120.3(2) . . ? C42 C41 H41 119.9 . . ? C35 C41 H41 119.9 . . ? C41 C42 C43 120.8(2) . . ? C41 C42 H42 119.6 . . ? C43 C42 H42 119.6 . . ? C44 C43 C42 120.4(2) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C43 C44 C36 120.7(2) . . ? C43 C44 H44 119.7 . . ? C36 C44 H44 119.7 . . ? N1 O3 Ag1 103.98(12) . . ? O2 N1 O1 120.6(2) . . ? O2 N1 O3 119.23(19) . . ? O1 N1 O3 120.11(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N38 Ag1 N11 C16 53.3(2) . . . . ? N22 Ag1 N11 C16 179.62(19) . . . . ? O3 Ag1 N11 C16 -66.6(2) . . . . ? N38 Ag1 N11 C12 -113.27(16) . . . . ? N22 Ag1 N11 C12 13.09(14) . . . . ? O3 Ag1 N11 C12 126.90(14) . . . . ? C16 N11 C12 C13 -0.6(3) . . . . ? Ag1 N11 C12 C13 166.79(16) . . . . ? C16 N11 C12 C23 -179.74(19) . . . . ? Ag1 N11 C12 C23 -12.4(2) . . . . ? N11 C12 C13 C14 0.2(3) . . . . ? C23 C12 C13 C14 179.3(2) . . . . ? C12 C13 C14 C15 -0.1(3) . . . . ? C13 C14 C15 C16 0.4(3) . . . . ? C12 N11 C16 C15 0.9(3) . . . . ? Ag1 N11 C16 C15 -165.37(17) . . . . ? C14 C15 C16 N11 -0.8(4) . . . . ? C25 N21 N22 C23 0.5(2) . . . . ? C26 N21 N22 C23 175.22(18) . . . . ? C25 N21 N22 Ag1 164.30(16) . . . . ? C26 N21 N22 Ag1 -21.0(3) . . . . ? N38 Ag1 N22 C23 96.94(16) . . . . ? N11 Ag1 N22 C23 -12.30(14) . . . . ? O3 Ag1 N22 C23 -133.76(14) . . . . ? N38 Ag1 N22 N21 -65.6(2) . . . . ? N11 Ag1 N22 N21 -174.9(2) . . . . ? O3 Ag1 N22 N21 63.7(2) . . . . ? N21 N22 C23 C24 -0.5(2) . . . . ? Ag1 N22 C23 C24 -168.04(14) . . . . ? N21 N22 C23 C12 178.50(18) . . . . ? Ag1 N22 C23 C12 10.9(2) . . . . ? N11 C12 C23 N22 1.2(3) . . . . ? C13 C12 C23 N22 -178.0(2) . . . . ? N11 C12 C23 C24 179.8(2) . . . . ? C13 C12 C23 C24 0.7(4) . . . . ? N22 C23 C24 C25 0.2(3) . . . . ? C12 C23 C24 C25 -178.6(2) . . . . ? N22 N21 C25 C24 -0.4(3) . . . . ? C26 N21 C25 C24 -174.5(2) . . . . ? C23 C24 C25 N21 0.1(2) . . . . ? N22 N21 C26 C31 51.6(3) . . . . ? C25 N21 C26 C31 -134.7(2) . . . . ? N21 C26 C31 C32 -111.9(2) . . . . ? N21 C26 C31 C36 68.6(3) . . . . ? C36 C31 C32 C33 0.9(3) . . . . ? C26 C31 C32 C33 -178.6(2) . . . . ? C31 C32 C33 C34 -0.8(3) . . . . ? C32 C33 C34 C35 -0.2(3) . . . . ? C32 C33 C34 C37 -179.7(2) . . . 3_565 ? C33 C34 C35 C41 -179.4(2) . . . . ? C37 C34 C35 C41 0.1(3) 3_565 . . . ? C33 C34 C35 C36 0.9(3) . . . . ? C37 C34 C35 C36 -179.5(2) 3_565 . . . ? C41 C35 C36 C44 -0.9(3) . . . . ? C34 C35 C36 C44 178.76(19) . . . . ? C41 C35 C36 C31 179.6(2) . . . . ? C34 C35 C36 C31 -0.8(3) . . . . ? C32 C31 C36 C35 -0.1(3) . . . . ? C26 C31 C36 C35 179.36(19) . . . . ? C32 C31 C36 C44 -179.6(2) . . . . ? C26 C31 C36 C44 -0.1(3) . . . . ? C34 C37 N38 Ag1 -36(7) 3_565 . . . ? N22 Ag1 N38 C37 148.7(7) . . . . ? N11 Ag1 N38 C37 -124.6(7) . . . . ? O3 Ag1 N38 C37 10.9(7) . . . . ? C36 C35 C41 C42 -0.2(3) . . . . ? C34 C35 C41 C42 -179.8(2) . . . . ? C35 C41 C42 C43 0.9(4) . . . . ? C41 C42 C43 C44 -0.5(4) . . . . ? C42 C43 C44 C36 -0.6(3) . . . . ? C35 C36 C44 C43 1.3(3) . . . . ? C31 C36 C44 C43 -179.2(2) . . . . ? N38 Ag1 O3 N1 -85.66(14) . . . . ? N22 Ag1 O3 N1 130.57(13) . . . . ? N11 Ag1 O3 N1 43.39(16) . . . . ? Ag1 O3 N1 O2 14.2(2) . . . . ? Ag1 O3 N1 O1 -163.08(17) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.142 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.068 #===END data_imw1243p21c _database_code_depnum_ccdc_archive 'CCDC 758089' #TrackingRef 'mixed_metal_networks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H14 Ag B F4 N4' _chemical_formula_weight 505.03 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' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.55750(10) _cell_length_b 18.7864(3) _cell_length_c 13.2436(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.8550(10) _cell_angle_gamma 90.00 _cell_volume 1879.32(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9907 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 27.46 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 1.126 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4306 _exptl_absorpt_correction_T_max 0.6029 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26130 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0123 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4304 _reflns_number_gt 4160 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The data was solved by direct methods. 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^)+(0.0240P)^2^+1.3435P] 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_number_reflns 4304 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0229 _refine_ls_R_factor_gt 0.0219 _refine_ls_wR_factor_ref 0.0562 _refine_ls_wR_factor_gt 0.0556 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 0.002 _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 Ag1 Ag 0.218344(18) 0.511100(7) 0.786195(9) 0.02815(5) Uani 1 1 d . . . N11 N 0.2232(2) 0.53967(8) 0.95709(11) 0.0269(3) Uani 1 1 d . . . C12 C 0.2402(2) 0.48450(9) 1.02116(12) 0.0217(3) Uani 1 1 d . . . C13 C 0.2250(3) 0.49296(10) 1.12499(13) 0.0284(4) Uani 1 1 d . . . H13 H 0.2357 0.4532 1.1691 0.034 Uiso 1 1 calc R . . C14 C 0.1939(3) 0.56034(11) 1.16277(14) 0.0321(4) Uani 1 1 d . . . H14 H 0.1825 0.5673 1.2333 0.038 Uiso 1 1 calc R . . C15 C 0.1797(3) 0.61701(10) 1.09755(15) 0.0347(4) Uani 1 1 d . . . H15 H 0.1598 0.6638 1.1221 0.042 Uiso 1 1 calc R . . C16 C 0.1949(3) 0.60443(10) 0.99539(15) 0.0355(4) Uani 1 1 d . . . H16 H 0.1849 0.6436 0.9502 0.043 Uiso 1 1 calc R . . N21 N 0.33799(18) 0.34241(7) 0.85747(10) 0.0216(3) Uani 1 1 d . . . N22 N 0.30938(18) 0.41174(7) 0.87663(10) 0.0205(3) Uani 1 1 d . . . C23 C 0.2771(2) 0.41505(9) 0.97557(12) 0.0217(3) Uani 1 1 d . . . C24 C 0.2866(3) 0.34724(9) 1.01930(13) 0.0280(4) Uani 1 1 d . . . H24 H 0.2689 0.3351 1.0879 0.034 Uiso 1 1 calc R . . C25 C 0.3267(2) 0.30216(9) 0.94199(13) 0.0280(4) Uani 1 1 d . . . H25 H 0.3434 0.2521 0.9467 0.034 Uiso 1 1 calc R . . C26 C 0.4027(2) 0.32041(9) 0.75943(12) 0.0224(3) Uani 1 1 d . . . H26A H 0.4031 0.2678 0.7560 0.027 Uiso 1 1 calc R . . H26B H 0.5265 0.3369 0.7537 0.027 Uiso 1 1 calc R . . C31 C 0.2933(2) 0.34915(8) 0.67106(11) 0.0197(3) Uani 1 1 d . . . C32 C 0.3673(2) 0.39785(9) 0.60802(13) 0.0242(3) Uani 1 1 d . . . H32 H 0.4843 0.4143 0.6225 0.029 Uiso 1 1 calc R . . C33 C 0.2738(2) 0.42404(9) 0.52225(13) 0.0264(3) Uani 1 1 d . . . H33 H 0.3276 0.4575 0.4791 0.032 Uiso 1 1 calc R . . C34 C 0.1043(2) 0.40091(9) 0.50147(12) 0.0242(3) Uani 1 1 d . . . C35 C 0.0195(2) 0.35123(9) 0.56550(12) 0.0215(3) Uani 1 1 d . . . C36 C 0.1169(2) 0.32448(8) 0.65107(11) 0.0190(3) Uani 1 1 d . . . C37 C -0.0097(2) 0.57240(9) 0.58710(13) 0.0273(3) Uani 1 1 d . . . N38 N 0.0666(2) 0.55052(9) 0.65605(11) 0.0318(3) Uani 1 1 d . . . C41 C -0.1562(2) 0.32744(10) 0.54567(13) 0.0279(4) Uani 1 1 d . . . H41 H -0.2220 0.3453 0.4888 0.033 Uiso 1 1 calc R . . C42 C -0.2312(2) 0.27888(10) 0.60801(14) 0.0305(4) Uani 1 1 d . . . H42 H -0.3495 0.2636 0.5945 0.037 Uiso 1 1 calc R . . C43 C -0.1355(2) 0.25122(9) 0.69199(13) 0.0277(3) Uani 1 1 d . . . H43 H -0.1889 0.2171 0.7343 0.033 Uiso 1 1 calc R . . C44 C 0.0343(2) 0.27332(9) 0.71287(12) 0.0226(3) Uani 1 1 d . . . H44 H 0.0980 0.2541 0.7696 0.027 Uiso 1 1 calc R . . B11 B 0.5233(3) 0.62307(10) 0.70025(15) 0.0252(4) Uani 1 1 d . . . F12 F 0.44553(18) 0.66495(7) 0.62536(10) 0.0486(3) Uani 1 1 d . . . F13 F 0.51072(17) 0.55131(6) 0.67529(9) 0.0419(3) Uani 1 1 d . . . F14 F 0.43842(15) 0.63419(7) 0.79024(9) 0.0388(3) Uani 1 1 d . . . F15 F 0.70035(14) 0.64230(6) 0.71229(8) 0.0313(2) 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 Ag1 0.03614(9) 0.02939(8) 0.01868(8) 0.00798(5) -0.00275(5) 0.00098(5) N11 0.0373(8) 0.0223(7) 0.0211(7) 0.0017(5) -0.0005(6) 0.0014(6) C12 0.0213(7) 0.0238(8) 0.0199(8) 0.0017(6) -0.0025(6) -0.0014(6) C13 0.0335(9) 0.0317(9) 0.0200(8) 0.0017(6) -0.0011(7) 0.0004(7) C14 0.0349(9) 0.0387(10) 0.0227(8) -0.0066(7) 0.0005(7) -0.0007(8) C15 0.0421(10) 0.0291(9) 0.0328(10) -0.0074(7) 0.0008(8) 0.0039(8) C16 0.0511(12) 0.0247(9) 0.0304(9) 0.0017(7) 0.0003(8) 0.0047(8) N21 0.0264(7) 0.0202(6) 0.0181(6) 0.0019(5) -0.0040(5) 0.0016(5) N22 0.0226(6) 0.0209(6) 0.0177(6) 0.0007(5) -0.0027(5) 0.0005(5) C23 0.0230(7) 0.0244(8) 0.0173(7) 0.0022(6) -0.0032(6) -0.0009(6) C24 0.0400(10) 0.0257(8) 0.0181(8) 0.0046(6) -0.0035(7) -0.0004(7) C25 0.0396(10) 0.0212(8) 0.0227(8) 0.0048(6) -0.0061(7) 0.0009(7) C26 0.0221(7) 0.0253(8) 0.0196(7) -0.0015(6) -0.0035(6) 0.0030(6) C31 0.0218(7) 0.0206(7) 0.0165(7) -0.0022(6) -0.0001(6) 0.0034(6) C32 0.0227(8) 0.0261(8) 0.0240(8) -0.0012(6) 0.0015(6) -0.0006(6) C33 0.0330(9) 0.0251(8) 0.0214(8) 0.0029(6) 0.0059(7) 0.0014(7) C34 0.0304(8) 0.0263(8) 0.0160(7) -0.0002(6) -0.0002(6) 0.0087(6) C35 0.0238(8) 0.0239(8) 0.0166(7) -0.0035(6) -0.0008(6) 0.0053(6) C36 0.0205(7) 0.0198(7) 0.0166(7) -0.0035(5) -0.0002(5) 0.0033(6) C37 0.0342(9) 0.0278(8) 0.0201(8) 0.0004(6) 0.0022(7) 0.0076(7) N38 0.0382(8) 0.0348(8) 0.0222(7) 0.0049(6) 0.0001(6) 0.0099(7) C41 0.0248(8) 0.0335(9) 0.0249(8) -0.0052(7) -0.0066(6) 0.0058(7) C42 0.0207(8) 0.0356(9) 0.0350(9) -0.0096(8) -0.0020(7) -0.0011(7) C43 0.0275(8) 0.0270(8) 0.0287(9) -0.0041(7) 0.0044(7) -0.0035(7) C44 0.0256(8) 0.0228(8) 0.0193(7) -0.0011(6) 0.0003(6) 0.0013(6) B11 0.0268(9) 0.0238(9) 0.0247(9) 0.0008(7) -0.0012(7) -0.0019(7) F12 0.0477(7) 0.0511(8) 0.0453(7) 0.0190(6) -0.0243(6) -0.0124(6) F13 0.0550(7) 0.0270(6) 0.0446(7) -0.0089(5) 0.0161(6) -0.0138(5) F14 0.0360(6) 0.0466(7) 0.0342(6) -0.0060(5) 0.0086(5) 0.0059(5) F15 0.0260(5) 0.0313(5) 0.0363(6) 0.0013(4) -0.0011(4) -0.0023(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 Ag1 N38 2.1693(15) . ? Ag1 N22 2.3106(13) . ? Ag1 N11 2.3252(14) . ? N11 C16 1.338(2) . ? N11 C12 1.343(2) . ? C12 C13 1.393(2) . ? C12 C23 1.468(2) . ? C13 C14 1.384(3) . ? C13 H13 0.9500 . ? C14 C15 1.373(3) . ? C14 H14 0.9500 . ? C15 C16 1.382(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? N21 N22 1.3458(19) . ? N21 C25 1.356(2) . ? N21 C26 1.462(2) . ? N22 C23 1.342(2) . ? C23 C24 1.400(2) . ? C24 C25 1.370(2) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.511(2) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C31 C32 1.370(2) . ? C31 C36 1.428(2) . ? C32 C33 1.407(2) . ? C32 H32 0.9500 . ? C33 C34 1.372(3) . ? C33 H33 0.9500 . ? C34 C35 1.427(2) . ? C34 C37 1.444(2) 3_566 ? C35 C41 1.418(2) . ? C35 C36 1.423(2) . ? C36 C44 1.420(2) . ? C37 N38 1.141(2) . ? C37 C34 1.444(2) 3_566 ? C41 C42 1.366(3) . ? C41 H41 0.9500 . ? C42 C43 1.406(3) . ? C42 H42 0.9500 . ? C43 C44 1.369(2) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? B11 F12 1.382(2) . ? B11 F14 1.387(2) . ? B11 F15 1.390(2) . ? B11 F13 1.390(2) . ? 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 N38 Ag1 N22 145.94(6) . . ? N38 Ag1 N11 133.30(6) . . ? N22 Ag1 N11 71.75(5) . . ? C16 N11 C12 118.39(15) . . ? C16 N11 Ag1 125.54(12) . . ? C12 N11 Ag1 115.78(11) . . ? N11 C12 C13 121.76(16) . . ? N11 C12 C23 116.20(14) . . ? C13 C12 C23 122.03(15) . . ? C14 C13 C12 118.80(17) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C15 C14 C13 119.51(17) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 118.43(18) . . ? C14 C15 H15 120.8 . . ? C16 C15 H15 120.8 . . ? N11 C16 C15 123.09(18) . . ? N11 C16 H16 118.5 . . ? C15 C16 H16 118.5 . . ? N22 N21 C25 111.67(14) . . ? N22 N21 C26 120.10(13) . . ? C25 N21 C26 127.40(14) . . ? C23 N22 N21 105.33(13) . . ? C23 N22 Ag1 114.09(10) . . ? N21 N22 Ag1 136.98(10) . . ? N22 C23 C24 110.69(15) . . ? N22 C23 C12 119.06(14) . . ? C24 C23 C12 130.25(15) . . ? C25 C24 C23 105.23(15) . . ? C25 C24 H24 127.4 . . ? C23 C24 H24 127.4 . . ? N21 C25 C24 107.08(15) . . ? N21 C25 H25 126.5 . . ? C24 C25 H25 126.5 . . ? N21 C26 C31 113.34(13) . . ? N21 C26 H26A 108.9 . . ? C31 C26 H26A 108.9 . . ? N21 C26 H26B 108.9 . . ? C31 C26 H26B 108.9 . . ? H26A C26 H26B 107.7 . . ? C32 C31 C36 120.06(14) . . ? C32 C31 C26 119.11(14) . . ? C36 C31 C26 120.80(14) . . ? C31 C32 C33 121.40(16) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? C34 C33 C32 119.51(15) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C33 C34 C35 121.51(15) . . ? C33 C34 C37 119.19(16) . 3_566 ? C35 C34 C37 119.31(16) . 3_566 ? C41 C35 C36 119.58(15) . . ? C41 C35 C34 122.17(15) . . ? C36 C35 C34 118.24(15) . . ? C44 C36 C35 118.18(14) . . ? C44 C36 C31 122.55(14) . . ? C35 C36 C31 119.27(14) . . ? N38 C37 C34 178.81(19) . 3_566 ? C37 N38 Ag1 178.25(17) . . ? C42 C41 C35 120.22(16) . . ? C42 C41 H41 119.9 . . ? C35 C41 H41 119.9 . . ? C41 C42 C43 120.79(16) . . ? C41 C42 H42 119.6 . . ? C43 C42 H42 119.6 . . ? C44 C43 C42 120.17(16) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C36 121.05(15) . . ? C43 C44 H44 119.5 . . ? C36 C44 H44 119.5 . . ? F12 B11 F14 109.45(16) . . ? F12 B11 F15 108.64(15) . . ? F14 B11 F15 109.42(15) . . ? F12 B11 F13 110.92(16) . . ? F14 B11 F13 108.68(15) . . ? F15 B11 F13 109.71(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N38 Ag1 N11 C16 -33.4(2) . . . . ? N22 Ag1 N11 C16 174.01(18) . . . . ? N38 Ag1 N11 C12 140.32(12) . . . . ? N22 Ag1 N11 C12 -12.29(12) . . . . ? C16 N11 C12 C13 1.5(3) . . . . ? Ag1 N11 C12 C13 -172.62(13) . . . . ? C16 N11 C12 C23 -177.97(16) . . . . ? Ag1 N11 C12 C23 7.87(19) . . . . ? N11 C12 C13 C14 -0.9(3) . . . . ? C23 C12 C13 C14 178.58(16) . . . . ? C12 C13 C14 C15 -0.3(3) . . . . ? C13 C14 C15 C16 0.8(3) . . . . ? C12 N11 C16 C15 -1.0(3) . . . . ? Ag1 N11 C16 C15 172.51(15) . . . . ? C14 C15 C16 N11 -0.1(3) . . . . ? C25 N21 N22 C23 -0.75(18) . . . . ? C26 N21 N22 C23 -171.10(13) . . . . ? C25 N21 N22 Ag1 -156.81(13) . . . . ? C26 N21 N22 Ag1 32.8(2) . . . . ? N38 Ag1 N22 C23 -127.84(12) . . . . ? N11 Ag1 N22 C23 15.46(11) . . . . ? N38 Ag1 N22 N21 26.8(2) . . . . ? N11 Ag1 N22 N21 170.08(16) . . . . ? N21 N22 C23 C24 0.38(18) . . . . ? Ag1 N22 C23 C24 162.73(11) . . . . ? N21 N22 C23 C12 179.98(14) . . . . ? Ag1 N22 C23 C12 -17.67(18) . . . . ? N11 C12 C23 N22 6.7(2) . . . . ? C13 C12 C23 N22 -172.76(16) . . . . ? N11 C12 C23 C24 -173.74(17) . . . . ? C13 C12 C23 C24 6.7(3) . . . . ? N22 C23 C24 C25 0.1(2) . . . . ? C12 C23 C24 C25 -179.43(17) . . . . ? N22 N21 C25 C24 0.8(2) . . . . ? C26 N21 C25 C24 170.32(16) . . . . ? C23 C24 C25 N21 -0.6(2) . . . . ? N22 N21 C26 C31 -52.30(19) . . . . ? C25 N21 C26 C31 139.01(17) . . . . ? N21 C26 C31 C32 113.10(17) . . . . ? N21 C26 C31 C36 -68.91(19) . . . . ? C36 C31 C32 C33 -0.7(2) . . . . ? C26 C31 C32 C33 177.29(15) . . . . ? C31 C32 C33 C34 0.5(3) . . . . ? C32 C33 C34 C35 0.6(3) . . . . ? C32 C33 C34 C37 -179.53(15) . . . 3_566 ? C33 C34 C35 C41 179.26(16) . . . . ? C37 C34 C35 C41 -0.6(2) 3_566 . . . ? C33 C34 C35 C36 -1.5(2) . . . . ? C37 C34 C35 C36 178.61(14) 3_566 . . . ? C41 C35 C36 C44 1.2(2) . . . . ? C34 C35 C36 C44 -178.00(14) . . . . ? C41 C35 C36 C31 -179.46(14) . . . . ? C34 C35 C36 C31 1.3(2) . . . . ? C32 C31 C36 C44 179.06(15) . . . . ? C26 C31 C36 C44 1.1(2) . . . . ? C32 C31 C36 C35 -0.2(2) . . . . ? C26 C31 C36 C35 -178.21(14) . . . . ? C34 C37 N38 Ag1 84(13) 3_566 . . . ? N22 Ag1 N38 C37 -136(5) . . . . ? N11 Ag1 N38 C37 95(5) . . . . ? C36 C35 C41 C42 -0.3(2) . . . . ? C34 C35 C41 C42 178.85(16) . . . . ? C35 C41 C42 C43 -0.6(3) . . . . ? C41 C42 C43 C44 0.6(3) . . . . ? C42 C43 C44 C36 0.3(3) . . . . ? C35 C36 C44 C43 -1.2(2) . . . . ? C31 C36 C44 C43 179.49(15) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.457 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.074 #===END data_imw1257p-1 _database_code_depnum_ccdc_archive 'CCDC 758090' #TrackingRef 'mixed_metal_networks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H42 B2 F8 N12 Zn' _chemical_formula_weight 1170.05 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0620(3) _cell_length_b 12.9944(3) _cell_length_c 19.4624(5) _cell_angle_alpha 87.222(2) _cell_angle_beta 87.857(2) _cell_angle_gamma 65.088(2) _cell_volume 2762.94(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5503 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 23.20 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1196 _exptl_absorpt_coefficient_mu 0.524 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8802 _exptl_absorpt_correction_T_max 0.9495 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35377 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0756 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12643 _reflns_number_gt 7856 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The data was solved by direct methods. Data processing was conducted to a resolution of 0.77 angstroms as the data was only complete to this resolution. The structure contains two disordered tetrafluoroborate anions. The anion B11 > F15 is disordered over three sites (25:33:42). The anion B21 > F25 displays rotational disorder about the B21 F22 bond (53:47). The anions have benefited from the application of geometric and displacement restraints. The disordered residues have been left isotropic due to their fluxional nature. The residual electron density is associated with the disordered anions, further spliting could have been attempted but this was not done as it was felt that doing so would not add any further chemical information. The terminal cyano groups (C151 > N152, C251 > N252 and C351 > N352 had higher than average therimal and anisotropic thermal perameters. Displacement restraints were employed to bring these parameters in line with the average. 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^)+(0.1511P)^2^+1.5109P] 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_number_reflns 12643 _refine_ls_number_parameters 754 _refine_ls_number_restraints 120 _refine_ls_R_factor_all 0.1243 _refine_ls_R_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.2564 _refine_ls_wR_factor_gt 0.2245 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.064 _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 0.78935(5) 0.79717(4) 0.68618(3) 0.02740(17) Uani 1 1 d . . . N111 N 0.9105(3) 0.6475(3) 0.74152(19) 0.0295(8) Uani 1 1 d . . . C112 C 0.9239(4) 0.6586(4) 0.8088(2) 0.0322(10) Uani 1 1 d . . . C113 C 1.0055(5) 0.5705(4) 0.8497(3) 0.0424(12) Uani 1 1 d . . . H113 H 1.0164 0.5814 0.8964 0.051 Uiso 1 1 calc R . . C114 C 1.0705(5) 0.4661(4) 0.8203(3) 0.0449(13) Uani 1 1 d . . . H114 H 1.1260 0.4036 0.8470 0.054 Uiso 1 1 calc R . . C115 C 1.0538(5) 0.4543(4) 0.7528(3) 0.0420(12) Uani 1 1 d . . . H115 H 1.0968 0.3831 0.7322 0.050 Uiso 1 1 calc R . . C116 C 0.9740(4) 0.5463(4) 0.7144(3) 0.0358(11) Uani 1 1 d . . . H116 H 0.9641 0.5372 0.6672 0.043 Uiso 1 1 calc R . . N121 N 0.7033(4) 0.9384(3) 0.8332(2) 0.0337(9) Uani 1 1 d . . . N122 N 0.7630(3) 0.8479(3) 0.79441(19) 0.0314(8) Uani 1 1 d . . . C123 C 0.8450(4) 0.7701(4) 0.8363(2) 0.0316(10) Uani 1 1 d . . . C124 C 0.8401(5) 0.8112(4) 0.9018(3) 0.0421(12) Uani 1 1 d . . . H124 H 0.8894 0.7730 0.9401 0.051 Uiso 1 1 calc R . . C125 C 0.7479(5) 0.9195(4) 0.8987(3) 0.0420(12) Uani 1 1 d . . . H125 H 0.7204 0.9712 0.9350 0.050 Uiso 1 1 calc R . . C126 C 0.6122(4) 1.0440(4) 0.8048(3) 0.0372(11) Uani 1 1 d . . . H12A H 0.5532 1.0841 0.8417 0.045 Uiso 1 1 calc R . . H12B H 0.5667 1.0269 0.7691 0.045 Uiso 1 1 calc R . . C131 C 0.6669(4) 1.1218(4) 0.7733(2) 0.0321(10) Uani 1 1 d . . . C132 C 0.7839(5) 1.1040(4) 0.7865(3) 0.0398(11) Uani 1 1 d . . . H132 H 0.8311 1.0430 0.8170 0.048 Uiso 1 1 calc R . . C133 C 0.8357(5) 1.1735(4) 0.7562(3) 0.0432(12) Uani 1 1 d . . . H133 H 0.9175 1.1596 0.7660 0.052 Uiso 1 1 calc R . . C134 C 0.7688(5) 1.2611(4) 0.7127(3) 0.0375(11) Uani 1 1 d . . . C135 C 0.6455(5) 1.2859(4) 0.6975(2) 0.0353(11) Uani 1 1 d . . . C136 C 0.5932(4) 1.2143(4) 0.7293(2) 0.0331(10) Uani 1 1 d . . . C141 C 0.5752(6) 1.3746(4) 0.6523(3) 0.0461(13) Uani 1 1 d . . . H141 H 0.6106 1.4200 0.6294 0.055 Uiso 1 1 calc R . . C142 C 0.4562(6) 1.3968(5) 0.6408(3) 0.0563(15) Uani 1 1 d . . . H142 H 0.4097 1.4576 0.6100 0.068 Uiso 1 1 calc R . . C143 C 0.4024(5) 1.3314(4) 0.6735(3) 0.0514(14) Uani 1 1 d . . . H143 H 0.3187 1.3494 0.6662 0.062 Uiso 1 1 calc R . . C144 C 0.4695(5) 1.2411(4) 0.7162(3) 0.0440(12) Uani 1 1 d . . . H144 H 0.4322 1.1959 0.7374 0.053 Uiso 1 1 calc R . . C151 C 0.8228(5) 1.3334(4) 0.6815(3) 0.0439(13) Uani 1 1 d . . . N152 N 0.8625(5) 1.3928(4) 0.6580(3) 0.0587(14) Uani 1 1 d . . . N211 N 0.6810(3) 0.9554(3) 0.6338(2) 0.0309(8) Uani 1 1 d . . . C212 C 0.7461(5) 1.0111(4) 0.6054(2) 0.0332(10) Uani 1 1 d . . . C213 C 0.6942(5) 1.1019(4) 0.5583(3) 0.0442(13) Uani 1 1 d . . . H213 H 0.7411 1.1393 0.5383 0.053 Uiso 1 1 calc R . . C214 C 0.5727(5) 1.1368(4) 0.5411(3) 0.0522(14) Uani 1 1 d . . . H214 H 0.5350 1.1988 0.5093 0.063 Uiso 1 1 calc R . . C215 C 0.5080(5) 1.0807(4) 0.5706(3) 0.0506(14) Uani 1 1 d . . . H215 H 0.4248 1.1036 0.5593 0.061 Uiso 1 1 calc R . . C216 C 0.5634(4) 0.9916(4) 0.6164(3) 0.0371(11) Uani 1 1 d . . . H216 H 0.5170 0.9540 0.6366 0.045 Uiso 1 1 calc R . . N221 N 1.0427(4) 0.8486(3) 0.6690(2) 0.0359(9) Uani 1 1 d . . . N222 N 0.9219(3) 0.8718(3) 0.66430(19) 0.0295(8) Uani 1 1 d . . . C223 C 0.8738(4) 0.9666(4) 0.6244(2) 0.0329(10) Uani 1 1 d . . . C224 C 0.9644(5) 1.0044(4) 0.6046(3) 0.0434(12) Uani 1 1 d . . . H224 H 0.9545 1.0695 0.5766 0.052 Uiso 1 1 calc R . . C225 C 1.0680(5) 0.9285(4) 0.6338(3) 0.0445(13) Uani 1 1 d . . . H225 H 1.1457 0.9308 0.6303 0.053 Uiso 1 1 calc R . . C226 C 1.1270(4) 0.7509(4) 0.7076(3) 0.0353(10) Uani 1 1 d . . . H22A H 1.2059 0.7193 0.6819 0.042 Uiso 1 1 calc R . . H22B H 1.0948 0.6922 0.7101 0.042 Uiso 1 1 calc R . . C231 C 1.1511(5) 0.7722(4) 0.7796(2) 0.0359(11) Uani 1 1 d . . . C232 C 1.0880(6) 0.8763(5) 0.8073(3) 0.0530(14) Uani 1 1 d . . . H232 H 1.0279 0.9357 0.7810 0.064 Uiso 1 1 calc R . . C233 C 1.1115(8) 0.8957(6) 0.8746(3) 0.069(2) Uani 1 1 d . . . H233 H 1.0666 0.9683 0.8932 0.083 Uiso 1 1 calc R . . C234 C 1.1979(7) 0.8120(5) 0.9137(3) 0.0578(17) Uani 1 1 d . . . C235 C 1.2683(5) 0.7042(5) 0.8855(3) 0.0448(13) Uani 1 1 d . . . C236 C 1.2421(5) 0.6840(4) 0.8185(2) 0.0348(11) Uani 1 1 d . . . C241 C 1.3625(7) 0.6183(6) 0.9228(3) 0.0596(17) Uani 1 1 d . . . H241 H 1.3792 0.6327 0.9678 0.072 Uiso 1 1 calc R . . C242 C 1.4311(6) 0.5140(6) 0.8956(3) 0.0621(17) Uani 1 1 d . . . H242 H 1.4954 0.4574 0.9212 0.074 Uiso 1 1 calc R . . C243 C 1.4042(5) 0.4922(5) 0.8289(3) 0.0526(14) Uani 1 1 d . . . H243 H 1.4497 0.4199 0.8100 0.063 Uiso 1 1 calc R . . C244 C 1.3132(5) 0.5748(4) 0.7917(3) 0.0379(11) Uani 1 1 d . . . H244 H 1.2971 0.5590 0.7469 0.046 Uiso 1 1 calc R . . C251 C 1.2177(9) 0.8334(7) 0.9830(4) 0.080(2) Uani 1 1 d . . . N252 N 1.2346(10) 0.8502(7) 1.0380(3) 0.120(3) Uani 1 1 d . . . N311 N 0.8295(3) 0.7192(3) 0.58581(18) 0.0275(8) Uani 1 1 d . . . C312 C 0.7517(4) 0.6757(4) 0.5664(2) 0.0306(10) Uani 1 1 d . . . C313 C 0.7650(5) 0.6229(4) 0.5049(3) 0.0413(12) Uani 1 1 d . . . H313 H 0.7095 0.5926 0.4927 0.050 Uiso 1 1 calc R . . C314 C 0.8618(5) 0.6152(5) 0.4610(3) 0.0488(13) Uani 1 1 d . . . H314 H 0.8741 0.5786 0.4185 0.059 Uiso 1 1 calc R . . C315 C 0.9393(5) 0.6612(5) 0.4800(3) 0.0482(13) Uani 1 1 d . . . H315 H 1.0049 0.6580 0.4504 0.058 Uiso 1 1 calc R . . C316 C 0.9208(4) 0.7119(4) 0.5426(2) 0.0359(10) Uani 1 1 d . . . H316 H 0.9753 0.7429 0.5555 0.043 Uiso 1 1 calc R . . N321 N 0.5458(3) 0.7382(3) 0.7085(2) 0.0331(9) Uani 1 1 d . . . N322 N 0.6482(3) 0.7351(3) 0.67545(19) 0.0285(8) Uani 1 1 d . . . C323 C 0.6526(4) 0.6871(3) 0.6156(2) 0.0283(9) Uani 1 1 d . . . C324 C 0.5549(4) 0.6578(4) 0.6106(3) 0.0370(11) Uani 1 1 d . . . H324 H 0.5377 0.6219 0.5736 0.044 Uiso 1 1 calc R . . C325 C 0.4892(4) 0.6918(4) 0.6704(3) 0.0370(11) Uani 1 1 d . . . H325 H 0.4162 0.6841 0.6829 0.044 Uiso 1 1 calc R . . C326 C 0.5227(4) 0.7676(4) 0.7803(3) 0.0380(11) Uani 1 1 d . . . H32A H 0.4366 0.7838 0.7924 0.046 Uiso 1 1 calc R . . H32B H 0.5341 0.8377 0.7868 0.046 Uiso 1 1 calc R . . C331 C 0.6052(4) 0.6752(4) 0.8281(2) 0.0343(10) Uani 1 1 d . . . C332 C 0.6772(4) 0.5696(4) 0.8052(2) 0.0344(10) Uani 1 1 d . . . H332 H 0.6728 0.5536 0.7586 0.041 Uiso 1 1 calc R . . C333 C 0.7570(5) 0.4846(4) 0.8490(3) 0.0399(11) Uani 1 1 d . . . H333 H 0.8049 0.4112 0.8322 0.048 Uiso 1 1 calc R . . C334 C 0.7667(5) 0.5064(5) 0.9157(3) 0.0440(12) Uani 1 1 d . . . C335 C 0.6921(5) 0.6156(5) 0.9432(3) 0.0428(12) Uani 1 1 d . . . C336 C 0.6093(5) 0.6995(4) 0.8988(3) 0.0392(11) Uani 1 1 d . . . C341 C 0.7007(7) 0.6408(6) 1.0124(3) 0.0596(16) Uani 1 1 d . . . H341 H 0.7579 0.5846 1.0418 0.072 Uiso 1 1 calc R . . C342 C 0.6286(7) 0.7439(7) 1.0371(4) 0.073(2) Uani 1 1 d . . . H342 H 0.6352 0.7600 1.0835 0.088 Uiso 1 1 calc R . . C343 C 0.5438(7) 0.8268(6) 0.9935(4) 0.069(2) Uani 1 1 d . . . H343 H 0.4926 0.8987 1.0112 0.083 Uiso 1 1 calc R . . C344 C 0.5330(6) 0.8072(5) 0.9264(3) 0.0511(14) Uani 1 1 d . . . H344 H 0.4749 0.8649 0.8981 0.061 Uiso 1 1 calc R . . C351 C 0.8566(6) 0.4208(5) 0.9591(3) 0.0575(15) Uani 1 1 d . . . N352 N 0.9310(6) 0.3539(5) 0.9931(3) 0.0772(17) Uani 1 1 d . . . B11X B 0.2435(7) 0.1069(6) 0.8370(5) 0.0793(15) Uiso 0.362(9) 1 d PDU A 1 F12X F 0.3319(9) 0.0157(7) 0.8044(7) 0.0821(17) Uiso 0.362(9) 1 d PDU A 1 F13X F 0.2649(11) 0.2022(7) 0.8232(6) 0.0728(19) Uiso 0.362(9) 1 d PDU A 1 F14X F 0.2473(11) 0.0839(10) 0.9070(5) 0.079(2) Uiso 0.362(9) 1 d PDU A 1 F15X F 0.1298(8) 0.1260(10) 0.8134(6) 0.0861(18) Uiso 0.362(9) 1 d PDU A 1 B11Y B 0.2661(12) 0.0962(9) 0.8147(8) 0.0804(15) Uiso 0.225(9) 1 d PDU B 2 F12Y F 0.1559(13) 0.0982(16) 0.7962(10) 0.0841(19) Uiso 0.225(9) 1 d PDU B 2 F13Y F 0.2595(19) 0.2049(11) 0.8097(10) 0.074(2) Uiso 0.225(9) 1 d PDU B 2 F14Y F 0.3577(14) 0.0275(15) 0.7713(11) 0.0846(18) Uiso 0.225(9) 1 d PDU B 2 F15Y F 0.2914(18) 0.0543(15) 0.8816(9) 0.0791(19) Uiso 0.225(9) 1 d PDU B 2 B11Z B 0.2575(5) 0.0766(5) 0.7103(3) 0.0843(18) Uiso 0.413(4) 1 d PDU C 3 F12Z F 0.1544(7) 0.0787(7) 0.7446(4) 0.0909(19) Uiso 0.413(4) 1 d PDU C 3 F13Z F 0.3546(7) 0.0365(8) 0.7546(4) 0.0867(17) Uiso 0.413(4) 1 d PDU C 3 F14Z F 0.2364(9) 0.1851(5) 0.6868(4) 0.100(3) Uiso 0.413(4) 1 d PDU C 3 F15Z F 0.2847(6) 0.0065(5) 0.6552(3) 0.0526(18) Uiso 0.413(4) 1 d PDU C 3 B21 B 0.2496(2) 0.65638(19) 0.53256(13) 0.0378(9) Uiso 1 1 d DU . . F22 F 0.1948(2) 0.60496(19) 0.57760(12) 0.0383(6) Uiso 1 1 d DU D . F23X F 0.2823(11) 0.7283(9) 0.5687(2) 0.0398(14) Uiso 0.50(3) 1 d PDU D 1 F24X F 0.3557(8) 0.5743(4) 0.5054(7) 0.0491(15) Uiso 0.50(3) 1 d PDU D 1 F25X F 0.1691(6) 0.7179(10) 0.4820(4) 0.0392(14) Uiso 0.50(3) 1 d PDU D 1 F23Y F 0.3077(11) 0.7064(10) 0.5697(2) 0.0429(15) Uiso 0.50(3) 1 d PDU D 2 F24Y F 0.3323(11) 0.5749(4) 0.4905(6) 0.0470(15) Uiso 0.50(3) 1 d PDU D 2 F25Y F 0.1598(4) 0.7393(8) 0.4930(5) 0.0381(14) Uiso 0.50(3) 1 d PDU D 2 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 0.0277(3) 0.0254(3) 0.0313(3) 0.00527(19) -0.0048(2) -0.0136(2) N111 0.031(2) 0.0267(18) 0.034(2) 0.0029(15) -0.0038(16) -0.0154(16) C112 0.034(2) 0.029(2) 0.037(3) 0.0069(19) -0.009(2) -0.0164(19) C113 0.054(3) 0.033(2) 0.042(3) 0.009(2) -0.017(2) -0.020(2) C114 0.043(3) 0.031(2) 0.055(3) 0.010(2) -0.017(3) -0.010(2) C115 0.040(3) 0.028(2) 0.056(3) -0.002(2) -0.006(2) -0.012(2) C116 0.036(3) 0.028(2) 0.044(3) 0.001(2) -0.005(2) -0.014(2) N121 0.042(2) 0.0267(18) 0.033(2) 0.0029(16) -0.0003(18) -0.0157(17) N122 0.032(2) 0.0294(19) 0.034(2) 0.0008(16) 0.0018(17) -0.0147(16) C123 0.039(3) 0.029(2) 0.029(2) 0.0068(18) -0.004(2) -0.018(2) C124 0.054(3) 0.039(3) 0.036(3) 0.006(2) -0.010(2) -0.022(2) C125 0.059(3) 0.039(3) 0.031(3) -0.001(2) -0.002(2) -0.024(3) C126 0.037(3) 0.027(2) 0.047(3) 0.002(2) 0.001(2) -0.013(2) C131 0.039(3) 0.025(2) 0.034(3) -0.0017(18) 0.001(2) -0.0152(19) C132 0.042(3) 0.029(2) 0.046(3) 0.005(2) -0.005(2) -0.013(2) C133 0.035(3) 0.043(3) 0.053(3) -0.004(2) 0.000(2) -0.018(2) C134 0.048(3) 0.029(2) 0.040(3) -0.009(2) 0.012(2) -0.021(2) C135 0.049(3) 0.028(2) 0.031(3) -0.0052(19) 0.002(2) -0.018(2) C136 0.037(3) 0.025(2) 0.036(3) -0.0048(18) 0.003(2) -0.0110(19) C141 0.067(4) 0.027(2) 0.043(3) 0.001(2) -0.002(3) -0.019(2) C142 0.069(4) 0.036(3) 0.057(4) 0.010(3) -0.020(3) -0.015(3) C143 0.041(3) 0.037(3) 0.068(4) 0.002(3) -0.016(3) -0.008(2) C144 0.041(3) 0.035(3) 0.056(3) -0.001(2) -0.006(2) -0.015(2) C151 0.061(3) 0.042(3) 0.039(3) -0.012(2) 0.013(3) -0.032(3) N152 0.084(4) 0.059(3) 0.052(3) -0.008(2) 0.014(3) -0.049(3) N211 0.033(2) 0.0272(18) 0.033(2) 0.0030(15) -0.0038(16) -0.0131(16) C212 0.045(3) 0.025(2) 0.030(2) 0.0030(18) -0.001(2) -0.015(2) C213 0.062(4) 0.030(2) 0.038(3) 0.011(2) -0.003(3) -0.018(2) C214 0.056(4) 0.037(3) 0.055(4) 0.020(2) -0.014(3) -0.011(3) C215 0.045(3) 0.039(3) 0.061(4) 0.011(3) -0.019(3) -0.010(2) C216 0.033(3) 0.027(2) 0.048(3) 0.006(2) -0.008(2) -0.010(2) N221 0.038(2) 0.040(2) 0.039(2) 0.0045(18) -0.0067(18) -0.0256(19) N222 0.031(2) 0.0317(19) 0.032(2) 0.0003(15) -0.0019(16) -0.0186(16) C223 0.042(3) 0.030(2) 0.033(2) 0.0005(19) -0.002(2) -0.022(2) C224 0.053(3) 0.042(3) 0.047(3) 0.008(2) 0.000(3) -0.032(3) C225 0.044(3) 0.049(3) 0.055(3) 0.004(2) -0.003(3) -0.034(3) C226 0.029(2) 0.041(3) 0.043(3) -0.003(2) -0.005(2) -0.020(2) C231 0.041(3) 0.041(3) 0.037(3) -0.004(2) 0.005(2) -0.028(2) C232 0.068(4) 0.045(3) 0.049(3) -0.004(3) 0.002(3) -0.026(3) C233 0.112(6) 0.053(4) 0.049(4) -0.020(3) 0.020(4) -0.042(4) C234 0.099(5) 0.060(4) 0.035(3) -0.007(3) 0.000(3) -0.052(4) C235 0.066(4) 0.055(3) 0.033(3) 0.004(2) -0.002(3) -0.045(3) C236 0.046(3) 0.040(3) 0.030(2) 0.000(2) 0.000(2) -0.030(2) C241 0.084(5) 0.083(5) 0.035(3) 0.013(3) -0.016(3) -0.059(4) C242 0.061(4) 0.077(4) 0.051(4) 0.023(3) -0.014(3) -0.033(4) C243 0.049(3) 0.055(3) 0.052(4) 0.006(3) -0.004(3) -0.021(3) C244 0.041(3) 0.043(3) 0.034(3) 0.002(2) 0.000(2) -0.022(2) C251 0.137(7) 0.085(5) 0.046(4) -0.012(3) 0.005(4) -0.075(5) N252 0.229(10) 0.140(7) 0.040(4) -0.023(4) 0.002(5) -0.125(7) N311 0.0261(18) 0.0286(18) 0.030(2) 0.0020(15) -0.0045(15) -0.0136(15) C312 0.028(2) 0.025(2) 0.036(3) 0.0040(18) -0.0095(19) -0.0083(18) C313 0.034(3) 0.048(3) 0.045(3) -0.007(2) -0.009(2) -0.018(2) C314 0.044(3) 0.062(3) 0.040(3) -0.015(3) 0.001(2) -0.021(3) C315 0.039(3) 0.070(4) 0.037(3) -0.010(3) 0.002(2) -0.024(3) C316 0.030(2) 0.046(3) 0.033(3) -0.003(2) -0.001(2) -0.017(2) N321 0.028(2) 0.0328(19) 0.040(2) 0.0102(17) -0.0020(17) -0.0154(16) N322 0.0257(19) 0.0270(17) 0.034(2) 0.0071(15) -0.0026(16) -0.0134(15) C323 0.026(2) 0.0234(19) 0.037(2) 0.0097(18) -0.0115(18) -0.0116(17) C324 0.039(3) 0.033(2) 0.046(3) 0.016(2) -0.016(2) -0.022(2) C325 0.028(2) 0.041(3) 0.048(3) 0.018(2) -0.012(2) -0.021(2) C326 0.035(3) 0.032(2) 0.047(3) 0.001(2) 0.006(2) -0.014(2) C331 0.037(3) 0.037(2) 0.035(3) 0.002(2) 0.005(2) -0.022(2) C332 0.041(3) 0.031(2) 0.032(3) 0.0026(19) -0.003(2) -0.016(2) C333 0.046(3) 0.036(2) 0.036(3) 0.005(2) -0.008(2) -0.015(2) C334 0.047(3) 0.049(3) 0.037(3) 0.006(2) -0.004(2) -0.022(3) C335 0.053(3) 0.051(3) 0.033(3) 0.000(2) 0.002(2) -0.031(3) C336 0.042(3) 0.041(3) 0.043(3) -0.005(2) 0.009(2) -0.026(2) C341 0.079(4) 0.073(4) 0.033(3) -0.005(3) 0.001(3) -0.037(4) C342 0.092(5) 0.089(5) 0.048(4) -0.020(4) 0.018(4) -0.047(5) C343 0.083(5) 0.063(4) 0.065(5) -0.026(4) 0.033(4) -0.036(4) C344 0.055(3) 0.048(3) 0.055(4) -0.014(3) 0.020(3) -0.026(3) C351 0.072(4) 0.064(4) 0.037(3) 0.005(3) -0.007(3) -0.028(3) N352 0.087(4) 0.078(4) 0.054(3) 0.021(3) -0.028(3) -0.022(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 N111 2.145(4) . ? Zn1 N211 2.146(4) . ? Zn1 N311 2.187(4) . ? Zn1 N322 2.189(3) . ? Zn1 N122 2.209(4) . ? Zn1 N222 2.212(3) . ? N111 C116 1.335(6) . ? N111 C112 1.347(6) . ? C112 C113 1.392(6) . ? C112 C123 1.472(6) . ? C113 C114 1.388(7) . ? C113 H113 0.9500 . ? C114 C115 1.362(7) . ? C114 H114 0.9500 . ? C115 C116 1.383(7) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? N121 N122 1.342(5) . ? N121 C125 1.374(6) . ? N121 C126 1.448(6) . ? N122 C123 1.342(6) . ? C123 C124 1.396(7) . ? C124 C125 1.378(7) . ? C124 H124 0.9500 . ? C125 H125 0.9500 . ? C126 C131 1.518(6) . ? C126 H12A 0.9900 . ? C126 H12B 0.9900 . ? C131 C132 1.362(7) . ? C131 C136 1.423(6) . ? C132 C133 1.397(7) . ? C132 H132 0.9500 . ? C133 C134 1.360(7) . ? C133 H133 0.9500 . ? C134 C135 1.422(7) . ? C134 C151 1.450(6) . ? C135 C141 1.399(7) . ? C135 C136 1.433(6) . ? C136 C144 1.413(7) . ? C141 C142 1.364(8) . ? C141 H141 0.9500 . ? C142 C143 1.390(8) . ? C142 H142 0.9500 . ? C143 C144 1.371(7) . ? C143 H143 0.9500 . ? C144 H144 0.9500 . ? C151 N152 1.139(6) . ? N211 C216 1.344(6) . ? N211 C212 1.362(6) . ? C212 C213 1.393(6) . ? C212 C223 1.455(7) . ? C213 C214 1.388(8) . ? C213 H213 0.9500 . ? C214 C215 1.370(8) . ? C214 H214 0.9500 . ? C215 C216 1.369(7) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? N221 C225 1.350(6) . ? N221 N222 1.364(5) . ? N221 C226 1.445(6) . ? N222 C223 1.339(6) . ? C223 C224 1.409(6) . ? C224 C225 1.349(8) . ? C224 H224 0.9500 . ? C225 H225 0.9500 . ? C226 C231 1.503(7) . ? C226 H22A 0.9900 . ? C226 H22B 0.9900 . ? C231 C232 1.368(7) . ? C231 C236 1.418(7) . ? C232 C233 1.406(9) . ? C232 H232 0.9500 . ? C233 C234 1.368(10) . ? C233 H233 0.9500 . ? C234 C235 1.422(8) . ? C234 C251 1.438(9) . ? C235 C241 1.407(8) . ? C235 C236 1.416(7) . ? C236 C244 1.426(7) . ? C241 C242 1.376(9) . ? C241 H241 0.9500 . ? C242 C243 1.421(9) . ? C242 H242 0.9500 . ? C243 C244 1.369(7) . ? C243 H243 0.9500 . ? C244 H244 0.9500 . ? C251 N252 1.145(9) . ? N311 C316 1.333(6) . ? N311 C312 1.356(6) . ? C312 C313 1.379(7) . ? C312 C323 1.465(6) . ? C313 C314 1.391(7) . ? C313 H313 0.9500 . ? C314 C315 1.373(8) . ? C314 H314 0.9500 . ? C315 C316 1.380(7) . ? C315 H315 0.9500 . ? C316 H316 0.9500 . ? N321 C325 1.345(6) . ? N321 N322 1.357(5) . ? N321 C326 1.453(6) . ? N322 C323 1.337(6) . ? C323 C324 1.390(6) . ? C324 C325 1.366(7) . ? C324 H324 0.9500 . ? C325 H325 0.9500 . ? C326 C331 1.501(7) . ? C326 H32A 0.9900 . ? C326 H32B 0.9900 . ? C331 C332 1.364(6) . ? C331 C336 1.432(7) . ? C332 C333 1.396(7) . ? C332 H332 0.9500 . ? C333 C334 1.361(7) . ? C333 H333 0.9500 . ? C334 C335 1.439(8) . ? C334 C351 1.444(8) . ? C335 C336 1.411(7) . ? C335 C341 1.419(8) . ? C336 C344 1.431(7) . ? C341 C342 1.353(9) . ? C341 H341 0.9500 . ? C342 C343 1.406(10) . ? C342 H342 0.9500 . ? C343 C344 1.363(9) . ? C343 H343 0.9500 . ? C344 H344 0.9500 . ? C351 N352 1.154(8) . ? B11X F12X 1.380(2) . ? B11X F13X 1.380(2) . ? B11X F15X 1.380(2) . ? B11X F14X 1.380(2) . ? B11Y F13Y 1.380(2) . ? B11Y F15Y 1.380(2) . ? B11Y F14Y 1.380(2) . ? B11Y F12Y 1.380(2) . ? B11Z F15Z 1.379(2) . ? B11Z F12Z 1.380(2) . ? B11Z F14Z 1.380(2) . ? B11Z F13Z 1.380(2) . ? B21 F25X 1.376(2) . ? B21 F23Y 1.380(2) . ? B21 F24X 1.381(2) . ? B21 F23X 1.385(2) . ? B21 F24Y 1.386(2) . ? B21 F22 1.3870(19) . ? B21 F25Y 1.387(2) . ? 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 N111 Zn1 N211 173.73(14) . . ? N111 Zn1 N311 94.93(14) . . ? N211 Zn1 N311 87.74(14) . . ? N111 Zn1 N322 94.24(13) . . ? N211 Zn1 N322 91.92(13) . . ? N311 Zn1 N322 75.86(13) . . ? N111 Zn1 N122 76.25(14) . . ? N211 Zn1 N122 101.28(14) . . ? N311 Zn1 N122 170.87(13) . . ? N322 Zn1 N122 102.13(14) . . ? N111 Zn1 N222 97.15(14) . . ? N211 Zn1 N222 77.11(14) . . ? N311 Zn1 N222 90.67(13) . . ? N322 Zn1 N222 163.06(14) . . ? N122 Zn1 N222 92.75(13) . . ? C116 N111 C112 118.3(4) . . ? C116 N111 Zn1 125.3(3) . . ? C112 N111 Zn1 116.4(3) . . ? N111 C112 C113 122.4(4) . . ? N111 C112 C123 115.4(4) . . ? C113 C112 C123 122.2(4) . . ? C114 C113 C112 118.1(5) . . ? C114 C113 H113 120.9 . . ? C112 C113 H113 120.9 . . ? C115 C114 C113 119.2(5) . . ? C115 C114 H114 120.4 . . ? C113 C114 H114 120.4 . . ? C114 C115 C116 119.8(5) . . ? C114 C115 H115 120.1 . . ? C116 C115 H115 120.1 . . ? N111 C116 C115 122.1(5) . . ? N111 C116 H116 118.9 . . ? C115 C116 H116 118.9 . . ? N122 N121 C125 111.4(4) . . ? N122 N121 C126 122.0(4) . . ? C125 N121 C126 126.4(4) . . ? C123 N122 N121 105.3(4) . . ? C123 N122 Zn1 112.5(3) . . ? N121 N122 Zn1 141.3(3) . . ? N122 C123 C124 111.7(4) . . ? N122 C123 C112 118.4(4) . . ? C124 C123 C112 129.9(4) . . ? C125 C124 C123 104.7(4) . . ? C125 C124 H124 127.7 . . ? C123 C124 H124 127.7 . . ? N121 C125 C124 107.0(4) . . ? N121 C125 H125 126.5 . . ? C124 C125 H125 126.5 . . ? N121 C126 C131 113.0(4) . . ? N121 C126 H12A 109.0 . . ? C131 C126 H12A 109.0 . . ? N121 C126 H12B 109.0 . . ? C131 C126 H12B 109.0 . . ? H12A C126 H12B 107.8 . . ? C132 C131 C136 120.4(4) . . ? C132 C131 C126 121.1(4) . . ? C136 C131 C126 118.5(4) . . ? C131 C132 C133 121.3(5) . . ? C131 C132 H132 119.3 . . ? C133 C132 H132 119.3 . . ? C134 C133 C132 119.8(5) . . ? C134 C133 H133 120.1 . . ? C132 C133 H133 120.1 . . ? C133 C134 C135 121.8(4) . . ? C133 C134 C151 119.6(5) . . ? C135 C134 C151 118.5(5) . . ? C141 C135 C134 123.0(4) . . ? C141 C135 C136 119.3(5) . . ? C134 C135 C136 117.8(4) . . ? C144 C136 C131 123.3(4) . . ? C144 C136 C135 117.8(4) . . ? C131 C136 C135 118.8(4) . . ? C142 C141 C135 120.8(5) . . ? C142 C141 H141 119.6 . . ? C135 C141 H141 119.6 . . ? C141 C142 C143 120.7(5) . . ? C141 C142 H142 119.7 . . ? C143 C142 H142 119.7 . . ? C144 C143 C142 120.3(5) . . ? C144 C143 H143 119.8 . . ? C142 C143 H143 119.8 . . ? C143 C144 C136 121.0(5) . . ? C143 C144 H144 119.5 . . ? C136 C144 H144 119.5 . . ? N152 C151 C134 177.9(6) . . ? C216 N211 C212 118.2(4) . . ? C216 N211 Zn1 126.0(3) . . ? C212 N211 Zn1 114.6(3) . . ? N211 C212 C213 121.6(5) . . ? N211 C212 C223 116.1(4) . . ? C213 C212 C223 122.3(4) . . ? C214 C213 C212 118.7(5) . . ? C214 C213 H213 120.6 . . ? C212 C213 H213 120.6 . . ? C215 C214 C213 119.1(5) . . ? C215 C214 H214 120.5 . . ? C213 C214 H214 120.5 . . ? C216 C215 C214 119.9(5) . . ? C216 C215 H215 120.1 . . ? C214 C215 H215 120.1 . . ? N211 C216 C215 122.5(5) . . ? N211 C216 H216 118.8 . . ? C215 C216 H216 118.8 . . ? C225 N221 N222 110.5(4) . . ? C225 N221 C226 127.1(4) . . ? N222 N221 C226 122.3(3) . . ? C223 N222 N221 105.4(3) . . ? C223 N222 Zn1 111.6(3) . . ? N221 N222 Zn1 142.2(3) . . ? N222 C223 C224 110.2(4) . . ? N222 C223 C212 119.6(4) . . ? C224 C223 C212 130.1(4) . . ? C225 C224 C223 105.4(4) . . ? C225 C224 H224 127.3 . . ? C223 C224 H224 127.3 . . ? C224 C225 N221 108.4(4) . . ? C224 C225 H225 125.8 . . ? N221 C225 H225 125.8 . . ? N221 C226 C231 115.8(4) . . ? N221 C226 H22A 108.3 . . ? C231 C226 H22A 108.3 . . ? N221 C226 H22B 108.3 . . ? C231 C226 H22B 108.3 . . ? H22A C226 H22B 107.4 . . ? C232 C231 C236 119.8(5) . . ? C232 C231 C226 120.8(5) . . ? C236 C231 C226 119.4(4) . . ? C231 C232 C233 120.4(6) . . ? C231 C232 H232 119.8 . . ? C233 C232 H232 119.8 . . ? C234 C233 C232 121.2(6) . . ? C234 C233 H233 119.4 . . ? C232 C233 H233 119.4 . . ? C233 C234 C235 119.8(5) . . ? C233 C234 C251 120.0(6) . . ? C235 C234 C251 120.2(6) . . ? C241 C235 C236 119.9(5) . . ? C241 C235 C234 121.3(5) . . ? C236 C235 C234 118.8(5) . . ? C235 C236 C231 119.9(5) . . ? C235 C236 C244 117.6(5) . . ? C231 C236 C244 122.4(4) . . ? C242 C241 C235 121.5(5) . . ? C242 C241 H241 119.2 . . ? C235 C241 H241 119.2 . . ? C241 C242 C243 119.0(6) . . ? C241 C242 H242 120.5 . . ? C243 C242 H242 120.5 . . ? C244 C243 C242 120.3(6) . . ? C244 C243 H243 119.8 . . ? C242 C243 H243 119.8 . . ? C243 C244 C236 121.6(5) . . ? C243 C244 H244 119.2 . . ? C236 C244 H244 119.2 . . ? N252 C251 C234 179.4(10) . . ? C316 N311 C312 118.0(4) . . ? C316 N311 Zn1 126.5(3) . . ? C312 N311 Zn1 115.5(3) . . ? N311 C312 C313 122.6(4) . . ? N311 C312 C323 115.5(4) . . ? C313 C312 C323 121.9(4) . . ? C312 C313 C314 118.4(5) . . ? C312 C313 H313 120.8 . . ? C314 C313 H313 120.8 . . ? C315 C314 C313 119.1(5) . . ? C315 C314 H314 120.4 . . ? C313 C314 H314 120.4 . . ? C314 C315 C316 119.3(5) . . ? C314 C315 H315 120.4 . . ? C316 C315 H315 120.4 . . ? N311 C316 C315 122.7(5) . . ? N311 C316 H316 118.7 . . ? C315 C316 H316 118.7 . . ? C325 N321 N322 110.6(4) . . ? C325 N321 C326 127.8(4) . . ? N322 N321 C326 120.5(4) . . ? C323 N322 N321 105.4(3) . . ? C323 N322 Zn1 114.5(3) . . ? N321 N322 Zn1 139.8(3) . . ? N322 C323 C324 111.0(4) . . ? N322 C323 C312 118.6(4) . . ? C324 C323 C312 130.4(4) . . ? C325 C324 C323 104.9(4) . . ? C325 C324 H324 127.6 . . ? C323 C324 H324 127.6 . . ? N321 C325 C324 108.2(4) . . ? N321 C325 H325 125.9 . . ? C324 C325 H325 125.9 . . ? N321 C326 C331 112.7(4) . . ? N321 C326 H32A 109.0 . . ? C331 C326 H32A 109.0 . . ? N321 C326 H32B 109.0 . . ? C331 C326 H32B 109.0 . . ? H32A C326 H32B 107.8 . . ? C332 C331 C336 119.8(4) . . ? C332 C331 C326 121.2(4) . . ? C336 C331 C326 119.0(4) . . ? C331 C332 C333 121.3(5) . . ? C331 C332 H332 119.3 . . ? C333 C332 H332 119.3 . . ? C334 C333 C332 120.3(5) . . ? C334 C333 H333 119.8 . . ? C332 C333 H333 119.8 . . ? C333 C334 C335 121.0(5) . . ? C333 C334 C351 119.9(5) . . ? C335 C334 C351 119.1(5) . . ? C336 C335 C341 119.9(5) . . ? C336 C335 C334 117.9(5) . . ? C341 C335 C334 122.2(5) . . ? C335 C336 C344 118.0(5) . . ? C335 C336 C331 119.6(5) . . ? C344 C336 C331 122.4(5) . . ? C342 C341 C335 121.0(6) . . ? C342 C341 H341 119.5 . . ? C335 C341 H341 119.5 . . ? C341 C342 C343 119.3(6) . . ? C341 C342 H342 120.3 . . ? C343 C342 H342 120.3 . . ? C344 C343 C342 121.9(6) . . ? C344 C343 H343 119.0 . . ? C342 C343 H343 119.0 . . ? C343 C344 C336 119.9(6) . . ? C343 C344 H344 120.1 . . ? C336 C344 H344 120.1 . . ? N352 C351 C334 177.8(7) . . ? F12X B11X F13X 109.44(16) . . ? F12X B11X F15X 109.51(16) . . ? F13X B11X F15X 109.48(16) . . ? F12X B11X F14X 109.46(16) . . ? F13X B11X F14X 109.49(16) . . ? F15X B11X F14X 109.45(16) . . ? F13Y B11Y F15Y 109.48(16) . . ? F13Y B11Y F14Y 109.46(16) . . ? F15Y B11Y F14Y 109.43(16) . . ? F13Y B11Y F12Y 109.47(16) . . ? F15Y B11Y F12Y 109.54(16) . . ? F14Y B11Y F12Y 109.45(16) . . ? F15Z B11Z F12Z 109.63(16) . . ? F15Z B11Z F14Z 109.47(16) . . ? F12Z B11Z F14Z 109.41(15) . . ? F15Z B11Z F13Z 109.44(15) . . ? F12Z B11Z F13Z 109.46(16) . . ? F14Z B11Z F13Z 109.42(16) . . ? F25X B21 F23Y 120.3(4) . . ? F25X B21 F24X 111.8(4) . . ? F23Y B21 F24X 95.3(5) . . ? F25X B21 F23X 109.4(4) . . ? F23Y B21 F23X 13.3(5) . . ? F24X B21 F23X 107.4(5) . . ? F25X B21 F24Y 96.9(4) . . ? F23Y B21 F24Y 110.8(5) . . ? F24X B21 F24Y 17.0(5) . . ? F23X B21 F24Y 121.9(4) . . ? F25X B21 F22 109.80(19) . . ? F23Y B21 F22 109.31(19) . . ? F24X B21 F22 109.30(19) . . ? F23X B21 F22 109.07(19) . . ? F24Y B21 F22 108.85(19) . . ? F25X B21 F25Y 14.0(5) . . ? F23Y B21 F25Y 109.2(4) . . ? F24X B21 F25Y 123.7(4) . . ? F23X B21 F25Y 97.4(4) . . ? F24Y B21 F25Y 109.9(4) . . ? F22 B21 F25Y 108.74(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N211 Zn1 N111 C116 -119.1(13) . . . . ? N311 Zn1 N111 C116 -4.2(4) . . . . ? N322 Zn1 N111 C116 72.0(4) . . . . ? N122 Zn1 N111 C116 173.4(4) . . . . ? N222 Zn1 N111 C116 -95.5(4) . . . . ? N211 Zn1 N111 C112 59.8(14) . . . . ? N311 Zn1 N111 C112 174.7(3) . . . . ? N322 Zn1 N111 C112 -109.2(3) . . . . ? N122 Zn1 N111 C112 -7.7(3) . . . . ? N222 Zn1 N111 C112 83.4(3) . . . . ? C116 N111 C112 C113 3.2(6) . . . . ? Zn1 N111 C112 C113 -175.7(4) . . . . ? C116 N111 C112 C123 -176.0(4) . . . . ? Zn1 N111 C112 C123 5.0(5) . . . . ? N111 C112 C113 C114 -3.2(7) . . . . ? C123 C112 C113 C114 176.0(4) . . . . ? C112 C113 C114 C115 1.1(8) . . . . ? C113 C114 C115 C116 0.9(8) . . . . ? C112 N111 C116 C115 -1.1(7) . . . . ? Zn1 N111 C116 C115 177.7(3) . . . . ? C114 C115 C116 N111 -0.9(7) . . . . ? C125 N121 N122 C123 1.0(5) . . . . ? C126 N121 N122 C123 175.6(4) . . . . ? C125 N121 N122 Zn1 -166.3(4) . . . . ? C126 N121 N122 Zn1 8.4(7) . . . . ? N111 Zn1 N122 C123 9.3(3) . . . . ? N211 Zn1 N122 C123 -164.8(3) . . . . ? N311 Zn1 N122 C123 24.5(10) . . . . ? N322 Zn1 N122 C123 100.7(3) . . . . ? N222 Zn1 N122 C123 -87.4(3) . . . . ? N111 Zn1 N122 N121 175.9(5) . . . . ? N211 Zn1 N122 N121 1.9(5) . . . . ? N311 Zn1 N122 N121 -168.9(7) . . . . ? N322 Zn1 N122 N121 -92.6(5) . . . . ? N222 Zn1 N122 N121 79.2(5) . . . . ? N121 N122 C123 C124 -1.2(5) . . . . ? Zn1 N122 C123 C124 170.1(3) . . . . ? N121 N122 C123 C112 178.6(4) . . . . ? Zn1 N122 C123 C112 -10.0(5) . . . . ? N111 C112 C123 N122 3.7(6) . . . . ? C113 C112 C123 N122 -175.5(4) . . . . ? N111 C112 C123 C124 -176.5(4) . . . . ? C113 C112 C123 C124 4.3(8) . . . . ? N122 C123 C124 C125 1.0(5) . . . . ? C112 C123 C124 C125 -178.8(5) . . . . ? N122 N121 C125 C124 -0.3(6) . . . . ? C126 N121 C125 C124 -174.7(4) . . . . ? C123 C124 C125 N121 -0.4(5) . . . . ? N122 N121 C126 C131 -85.9(5) . . . . ? C125 N121 C126 C131 87.9(6) . . . . ? N121 C126 C131 C132 -15.1(7) . . . . ? N121 C126 C131 C136 164.9(4) . . . . ? C136 C131 C132 C133 -1.7(8) . . . . ? C126 C131 C132 C133 178.3(5) . . . . ? C131 C132 C133 C134 0.2(8) . . . . ? C132 C133 C134 C135 1.0(8) . . . . ? C132 C133 C134 C151 179.8(5) . . . . ? C133 C134 C135 C141 -179.2(5) . . . . ? C151 C134 C135 C141 1.9(7) . . . . ? C133 C134 C135 C136 -0.5(7) . . . . ? C151 C134 C135 C136 -179.4(4) . . . . ? C132 C131 C136 C144 -176.6(5) . . . . ? C126 C131 C136 C144 3.4(7) . . . . ? C132 C131 C136 C135 2.1(7) . . . . ? C126 C131 C136 C135 -177.9(4) . . . . ? C141 C135 C136 C144 -3.4(7) . . . . ? C134 C135 C136 C144 177.8(4) . . . . ? C141 C135 C136 C131 177.8(4) . . . . ? C134 C135 C136 C131 -1.0(6) . . . . ? C134 C135 C141 C142 -178.3(5) . . . . ? C136 C135 C141 C142 3.0(7) . . . . ? C135 C141 C142 C143 -0.2(9) . . . . ? C141 C142 C143 C144 -2.2(9) . . . . ? C142 C143 C144 C136 1.6(9) . . . . ? C131 C136 C144 C143 179.9(5) . . . . ? C135 C136 C144 C143 1.1(7) . . . . ? C133 C134 C151 N152 -117(18) . . . . ? C135 C134 C151 N152 62(18) . . . . ? N111 Zn1 N211 C216 -159.6(12) . . . . ? N311 Zn1 N211 C216 85.1(4) . . . . ? N322 Zn1 N211 C216 9.4(4) . . . . ? N122 Zn1 N211 C216 -93.4(4) . . . . ? N222 Zn1 N211 C216 176.3(4) . . . . ? N111 Zn1 N211 C212 33.5(15) . . . . ? N311 Zn1 N211 C212 -81.8(3) . . . . ? N322 Zn1 N211 C212 -157.6(3) . . . . ? N122 Zn1 N211 C212 99.6(3) . . . . ? N222 Zn1 N211 C212 9.4(3) . . . . ? C216 N211 C212 C213 -1.3(7) . . . . ? Zn1 N211 C212 C213 166.8(4) . . . . ? C216 N211 C212 C223 -178.4(4) . . . . ? Zn1 N211 C212 C223 -10.3(5) . . . . ? N211 C212 C213 C214 0.9(8) . . . . ? C223 C212 C213 C214 177.8(5) . . . . ? C212 C213 C214 C215 -0.3(8) . . . . ? C213 C214 C215 C216 0.1(9) . . . . ? C212 N211 C216 C215 1.0(7) . . . . ? Zn1 N211 C216 C215 -165.5(4) . . . . ? C214 C215 C216 N211 -0.5(9) . . . . ? C225 N221 N222 C223 1.1(5) . . . . ? C226 N221 N222 C223 -179.3(4) . . . . ? C225 N221 N222 Zn1 169.1(4) . . . . ? C226 N221 N222 Zn1 -11.4(7) . . . . ? N111 Zn1 N222 C223 175.6(3) . . . . ? N211 Zn1 N222 C223 -7.0(3) . . . . ? N311 Zn1 N222 C223 80.5(3) . . . . ? N322 Zn1 N222 C223 43.7(6) . . . . ? N122 Zn1 N222 C223 -108.0(3) . . . . ? N111 Zn1 N222 N221 8.1(5) . . . . ? N211 Zn1 N222 N221 -174.5(5) . . . . ? N311 Zn1 N222 N221 -87.0(5) . . . . ? N322 Zn1 N222 N221 -123.8(5) . . . . ? N122 Zn1 N222 N221 84.6(5) . . . . ? N221 N222 C223 C224 -0.9(5) . . . . ? Zn1 N222 C223 C224 -172.9(3) . . . . ? N221 N222 C223 C212 176.1(4) . . . . ? Zn1 N222 C223 C212 4.1(5) . . . . ? N211 C212 C223 N222 4.1(6) . . . . ? C213 C212 C223 N222 -173.0(4) . . . . ? N211 C212 C223 C224 -179.6(5) . . . . ? C213 C212 C223 C224 3.3(8) . . . . ? N222 C223 C224 C225 0.3(6) . . . . ? C212 C223 C224 C225 -176.3(5) . . . . ? C223 C224 C225 N221 0.4(6) . . . . ? N222 N221 C225 C224 -1.0(6) . . . . ? C226 N221 C225 C224 179.5(5) . . . . ? C225 N221 C226 C231 82.7(6) . . . . ? N222 N221 C226 C231 -96.7(5) . . . . ? N221 C226 C231 C232 5.3(6) . . . . ? N221 C226 C231 C236 -173.5(4) . . . . ? C236 C231 C232 C233 -0.9(8) . . . . ? C226 C231 C232 C233 -179.7(5) . . . . ? C231 C232 C233 C234 0.3(10) . . . . ? C232 C233 C234 C235 2.0(10) . . . . ? C232 C233 C234 C251 -178.3(6) . . . . ? C233 C234 C235 C241 176.4(6) . . . . ? C251 C234 C235 C241 -3.4(9) . . . . ? C233 C234 C235 C236 -3.6(8) . . . . ? C251 C234 C235 C236 176.7(5) . . . . ? C241 C235 C236 C231 -177.0(5) . . . . ? C234 C235 C236 C231 3.0(7) . . . . ? C241 C235 C236 C244 0.6(7) . . . . ? C234 C235 C236 C244 -179.4(5) . . . . ? C232 C231 C236 C235 -0.8(7) . . . . ? C226 C231 C236 C235 178.0(4) . . . . ? C232 C231 C236 C244 -178.2(5) . . . . ? C226 C231 C236 C244 0.6(6) . . . . ? C236 C235 C241 C242 0.2(8) . . . . ? C234 C235 C241 C242 -179.8(6) . . . . ? C235 C241 C242 C243 -1.2(9) . . . . ? C241 C242 C243 C244 1.4(9) . . . . ? C242 C243 C244 C236 -0.7(8) . . . . ? C235 C236 C244 C243 -0.4(7) . . . . ? C231 C236 C244 C243 177.1(5) . . . . ? C233 C234 C251 N252 -120(75) . . . . ? C235 C234 C251 N252 60(76) . . . . ? N111 Zn1 N311 C316 -86.3(4) . . . . ? N211 Zn1 N311 C316 88.0(4) . . . . ? N322 Zn1 N311 C316 -179.4(4) . . . . ? N122 Zn1 N311 C316 -101.1(9) . . . . ? N222 Zn1 N311 C316 10.9(4) . . . . ? N111 Zn1 N311 C312 94.4(3) . . . . ? N211 Zn1 N311 C312 -91.3(3) . . . . ? N322 Zn1 N311 C312 1.3(3) . . . . ? N122 Zn1 N311 C312 79.6(9) . . . . ? N222 Zn1 N311 C312 -168.3(3) . . . . ? C316 N311 C312 C313 1.2(6) . . . . ? Zn1 N311 C312 C313 -179.5(3) . . . . ? C316 N311 C312 C323 -179.5(4) . . . . ? Zn1 N311 C312 C323 -0.1(5) . . . . ? N311 C312 C313 C314 -0.5(7) . . . . ? C323 C312 C313 C314 -179.8(5) . . . . ? C312 C313 C314 C315 -0.7(8) . . . . ? C313 C314 C315 C316 1.2(9) . . . . ? C312 N311 C316 C315 -0.7(7) . . . . ? Zn1 N311 C316 C315 -179.9(4) . . . . ? C314 C315 C316 N311 -0.5(8) . . . . ? C325 N321 N322 C323 0.9(5) . . . . ? C326 N321 N322 C323 169.6(4) . . . . ? C325 N321 N322 Zn1 173.0(3) . . . . ? C326 N321 N322 Zn1 -18.2(6) . . . . ? N111 Zn1 N322 C323 -96.4(3) . . . . ? N211 Zn1 N322 C323 84.8(3) . . . . ? N311 Zn1 N322 C323 -2.4(3) . . . . ? N122 Zn1 N322 C323 -173.2(3) . . . . ? N222 Zn1 N322 C323 35.8(6) . . . . ? N111 Zn1 N322 N321 91.9(4) . . . . ? N211 Zn1 N322 N321 -86.9(4) . . . . ? N311 Zn1 N322 N321 -174.1(4) . . . . ? N122 Zn1 N322 N321 15.1(4) . . . . ? N222 Zn1 N322 N321 -135.9(5) . . . . ? N321 N322 C323 C324 -1.0(4) . . . . ? Zn1 N322 C323 C324 -175.5(3) . . . . ? N321 N322 C323 C312 177.6(3) . . . . ? Zn1 N322 C323 C312 3.2(5) . . . . ? N311 C312 C323 N322 -2.1(6) . . . . ? C313 C312 C323 N322 177.3(4) . . . . ? N311 C312 C323 C324 176.2(4) . . . . ? C313 C312 C323 C324 -4.4(7) . . . . ? N322 C323 C324 C325 0.8(5) . . . . ? C312 C323 C324 C325 -177.6(4) . . . . ? N322 N321 C325 C324 -0.4(5) . . . . ? C326 N321 C325 C324 -168.1(4) . . . . ? C323 C324 C325 N321 -0.2(5) . . . . ? C325 N321 C326 C331 94.3(5) . . . . ? N322 N321 C326 C331 -72.3(5) . . . . ? N321 C326 C331 C332 -10.7(6) . . . . ? N321 C326 C331 C336 168.4(4) . . . . ? C336 C331 C332 C333 -1.3(7) . . . . ? C326 C331 C332 C333 177.8(4) . . . . ? C331 C332 C333 C334 -1.5(7) . . . . ? C332 C333 C334 C335 2.3(8) . . . . ? C332 C333 C334 C351 -175.1(5) . . . . ? C333 C334 C335 C336 -0.4(7) . . . . ? C351 C334 C335 C336 176.9(5) . . . . ? C333 C334 C335 C341 -179.7(5) . . . . ? C351 C334 C335 C341 -2.3(8) . . . . ? C341 C335 C336 C344 -2.1(7) . . . . ? C334 C335 C336 C344 178.6(4) . . . . ? C341 C335 C336 C331 177.0(5) . . . . ? C334 C335 C336 C331 -2.2(7) . . . . ? C332 C331 C336 C335 3.1(7) . . . . ? C326 C331 C336 C335 -176.0(4) . . . . ? C332 C331 C336 C344 -177.8(5) . . . . ? C326 C331 C336 C344 3.2(7) . . . . ? C336 C335 C341 C342 1.4(9) . . . . ? C334 C335 C341 C342 -179.4(6) . . . . ? C335 C341 C342 C343 0.2(10) . . . . ? C341 C342 C343 C344 -0.9(10) . . . . ? C342 C343 C344 C336 0.1(9) . . . . ? C335 C336 C344 C343 1.4(8) . . . . ? C331 C336 C344 C343 -177.7(5) . . . . ? C333 C334 C351 N352 93(19) . . . . ? C335 C334 C351 N352 -84(19) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.467 _refine_diff_density_min -0.772 _refine_diff_density_rms 0.109 #===END data_imw1258p-1 _database_code_depnum_ccdc_archive 'CCDC 758091' #TrackingRef 'mixed_metal_networks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H42 B2 Co F8 N12' _chemical_formula_weight 1163.61 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8250(5) _cell_length_b 12.9746(5) _cell_length_c 19.4176(7) _cell_angle_alpha 88.251(2) _cell_angle_beta 88.655(2) _cell_angle_gamma 64.931(2) _cell_volume 2697.06(18) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9926 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 27.41 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1190 _exptl_absorpt_coefficient_mu 0.399 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8566 _exptl_absorpt_correction_T_max 0.9611 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43280 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 27.58 _reflns_number_total 12403 _reflns_number_gt 9842 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The data was solved by direct methods. Data processing was conducted to a resolution of 0.77 angstroms as the data was only complete to this resolution. The structure contains a disordered tetrafluoroborate anion split over two sites (42:58). The disordered anion have benefited from the application of geometric and displacement restraints. The disordered residue has been left isotropic due to its fluxional nature. 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^)+(0.0860P)^2^+5.0363P] 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_number_reflns 12403 _refine_ls_number_parameters 744 _refine_ls_number_restraints 90 _refine_ls_R_factor_all 0.0783 _refine_ls_R_factor_gt 0.0602 _refine_ls_wR_factor_ref 0.1802 _refine_ls_wR_factor_gt 0.1659 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _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 Co1 Co 0.78577(3) 0.80374(3) 0.688885(18) 0.01535(11) Uani 1 1 d . . . N111 N 0.9102(2) 0.6523(2) 0.74322(13) 0.0267(5) Uani 1 1 d . . . C112 C 0.9236(3) 0.6633(3) 0.81087(16) 0.0275(6) Uani 1 1 d . . . C113 C 1.0024(3) 0.5732(3) 0.85198(18) 0.0351(7) Uani 1 1 d . . . H113 H 1.0119 0.5832 0.8994 0.042 Uiso 1 1 calc R . . C114 C 1.0672(3) 0.4678(3) 0.8219(2) 0.0391(8) Uani 1 1 d . . . H114 H 1.1215 0.4045 0.8488 0.047 Uiso 1 1 calc R . . C115 C 1.0521(3) 0.4558(3) 0.75318(19) 0.0357(7) Uani 1 1 d . . . H115 H 1.0949 0.3843 0.7320 0.043 Uiso 1 1 calc R . . C116 C 0.9733(3) 0.5500(3) 0.71547(18) 0.0306(7) Uani 1 1 d . . . H116 H 0.9636 0.5419 0.6678 0.037 Uiso 1 1 calc R . . N121 N 0.7074(3) 0.9474(2) 0.83555(14) 0.0301(6) Uani 1 1 d . . . N122 N 0.7642(2) 0.8547(2) 0.79664(13) 0.0266(5) Uani 1 1 d . . . C124 C 0.8443(3) 0.8193(3) 0.90383(17) 0.0339(7) Uani 1 1 d . . . H124 H 0.8938 0.7813 0.9425 0.041 Uiso 1 1 calc R . . C125 C 0.7539(3) 0.9286(3) 0.89991(17) 0.0353(7) Uani 1 1 d . . . H125 H 0.7284 0.9818 0.9360 0.042 Uiso 1 1 calc R . . C126 C 0.6143(3) 1.0531(3) 0.80631(17) 0.0306(7) Uani 1 1 d . . . H12A H 0.5555 1.0960 0.8432 0.037 Uiso 1 1 calc R . . H12B H 0.5660 1.0350 0.7714 0.037 Uiso 1 1 calc R . . C131 C 0.6712(3) 1.1274(3) 0.77296(16) 0.0270(6) Uani 1 1 d . . . C132 C 0.7906(3) 1.1111(3) 0.78683(17) 0.0322(7) Uani 1 1 d . . . H132 H 0.8392 1.0515 0.8179 0.039 Uiso 1 1 calc R . . C133 C 0.8428(3) 1.1804(3) 0.75620(18) 0.0354(7) Uani 1 1 d . . . H133 H 0.9258 1.1679 0.7666 0.042 Uiso 1 1 calc R . . C134 C 0.7739(3) 1.2662(3) 0.71128(17) 0.0331(7) Uani 1 1 d . . . C135 C 0.6478(3) 1.2885(3) 0.69583(16) 0.0311(7) Uani 1 1 d . . . C136 C 0.5955(3) 1.2185(3) 0.72807(16) 0.0286(6) Uani 1 1 d . . . C141 C 0.5744(4) 1.3768(3) 0.64993(18) 0.0394(8) Uani 1 1 d . . . H141 H 0.6097 1.4226 0.6275 0.047 Uiso 1 1 calc R . . C142 C 0.4542(4) 1.3973(3) 0.63726(19) 0.0441(9) Uani 1 1 d . . . H142 H 0.4062 1.4570 0.6062 0.053 Uiso 1 1 calc R . . C143 C 0.4010(4) 1.3304(3) 0.6700(2) 0.0429(9) Uani 1 1 d . . . H143 H 0.3162 1.3465 0.6617 0.051 Uiso 1 1 calc R . . C144 C 0.4697(3) 1.2420(3) 0.71379(18) 0.0356(7) Uani 1 1 d . . . H144 H 0.4328 1.1962 0.7347 0.043 Uiso 1 1 calc R . . C151 C 0.8267(4) 1.3376(3) 0.67941(19) 0.0416(9) Uani 1 1 d . . . N152 N 0.8662(4) 1.3970(3) 0.65461(17) 0.0543(9) Uani 1 1 d . . . N211 N 0.6725(3) 0.9612(2) 0.63671(13) 0.0284(5) Uani 1 1 d . . . C123 C 0.8478(3) 0.7762(3) 0.83835(16) 0.0278(6) Uani 1 1 d . . . C212 C 0.7373(3) 1.0156(3) 0.60697(16) 0.0294(7) Uani 1 1 d . . . C213 C 0.6839(4) 1.1039(3) 0.55899(18) 0.0380(8) Uani 1 1 d . . . H213 H 0.7312 1.1408 0.5387 0.046 Uiso 1 1 calc R . . C214 C 0.5611(4) 1.1369(3) 0.54141(19) 0.0448(9) Uani 1 1 d . . . H214 H 0.5230 1.1961 0.5081 0.054 Uiso 1 1 calc R . . C215 C 0.4933(4) 1.0828(3) 0.5728(2) 0.0428(9) Uani 1 1 d . . . H215 H 0.4080 1.1054 0.5621 0.051 Uiso 1 1 calc R . . C216 C 0.5522(3) 0.9962(3) 0.61973(18) 0.0338(7) Uani 1 1 d . . . H216 H 0.5059 0.9593 0.6411 0.041 Uiso 1 1 calc R . . N221 N 1.0383(3) 0.8593(3) 0.67504(15) 0.0342(6) Uani 1 1 d . . . N222 N 0.9180(2) 0.8786(2) 0.66647(13) 0.0279(5) Uani 1 1 d . . . C223 C 0.8683(3) 0.9734(3) 0.62681(16) 0.0302(7) Uani 1 1 d . . . C224 C 0.9572(4) 1.0152(3) 0.6108(2) 0.0407(8) Uani 1 1 d . . . H224 H 0.9459 1.0812 0.5839 0.049 Uiso 1 1 calc R . . C225 C 1.0636(4) 0.9406(3) 0.6420(2) 0.0452(9) Uani 1 1 d . . . H225 H 1.1419 0.9449 0.6408 0.054 Uiso 1 1 calc R . . C226 C 1.1261(3) 0.7572(3) 0.70995(17) 0.0322(7) Uani 1 1 d . . . H22A H 1.2041 0.7254 0.6822 0.039 Uiso 1 1 calc R . . H22B H 1.0909 0.7002 0.7116 0.039 Uiso 1 1 calc R . . C231 C 1.1584(3) 0.7738(3) 0.78259(17) 0.0316(7) Uani 1 1 d . . . C232 C 1.1061(4) 0.8771(3) 0.8135(2) 0.0423(8) Uani 1 1 d . . . H232 H 1.0476 0.9412 0.7889 0.051 Uiso 1 1 calc R . . C233 C 1.1376(4) 0.8901(4) 0.8816(2) 0.0515(10) Uani 1 1 d . . . H233 H 1.0997 0.9624 0.9024 0.062 Uiso 1 1 calc R . . C234 C 1.2219(4) 0.7993(4) 0.91737(19) 0.0449(9) Uani 1 1 d . . . C235 C 1.2829(4) 0.6907(3) 0.88662(17) 0.0378(8) Uani 1 1 d . . . C236 C 1.2493(3) 0.6777(3) 0.81892(16) 0.0308(7) Uani 1 1 d . . . C241 C 1.3757(4) 0.5962(4) 0.92169(18) 0.0441(9) Uani 1 1 d . . . H241 H 1.3977 0.6048 0.9672 0.053 Uiso 1 1 calc R . . C242 C 1.4332(4) 0.4941(4) 0.8914(2) 0.0455(9) Uani 1 1 d . . . H242 H 1.4957 0.4319 0.9154 0.055 Uiso 1 1 calc R . . C243 C 1.4005(4) 0.4801(3) 0.82451(19) 0.0417(8) Uani 1 1 d . . . H243 H 1.4411 0.4083 0.8034 0.050 Uiso 1 1 calc R . . C244 C 1.3103(3) 0.5693(3) 0.78935(17) 0.0335(7) Uani 1 1 d . . . H244 H 1.2884 0.5579 0.7444 0.040 Uiso 1 1 calc R . . C251 C 1.2521(5) 0.8117(4) 0.9871(2) 0.0573(12) Uani 1 1 d . . . N252 N 1.2789(5) 0.8190(4) 1.0432(2) 0.0794(14) Uani 1 1 d . . . N311 N 0.8218(2) 0.7238(2) 0.58869(13) 0.0268(5) Uani 1 1 d . . . C312 C 0.7440(3) 0.6773(3) 0.57143(16) 0.0285(6) Uani 1 1 d . . . C313 C 0.7581(3) 0.6195(3) 0.51067(18) 0.0363(8) Uani 1 1 d . . . H313 H 0.7033 0.5858 0.5002 0.044 Uiso 1 1 calc R . . C314 C 0.8531(3) 0.6119(3) 0.4659(2) 0.0434(9) Uani 1 1 d . . . H314 H 0.8649 0.5723 0.4240 0.052 Uiso 1 1 calc R . . C315 C 0.9311(3) 0.6618(3) 0.48183(19) 0.0418(8) Uani 1 1 d . . . H315 H 0.9958 0.6589 0.4509 0.050 Uiso 1 1 calc R . . C316 C 0.9128(3) 0.7164(3) 0.54413(17) 0.0320(7) Uani 1 1 d . . . H316 H 0.9671 0.7501 0.5556 0.038 Uiso 1 1 calc R . . N321 N 0.5369(2) 0.7490(2) 0.71402(14) 0.0310(6) Uani 1 1 d . . . N322 N 0.6414(2) 0.7424(2) 0.68087(13) 0.0274(5) Uani 1 1 d . . . C323 C 0.6437(3) 0.6922(3) 0.62133(16) 0.0280(6) Uani 1 1 d . . . C324 C 0.5414(3) 0.6656(3) 0.61673(18) 0.0360(8) Uani 1 1 d . . . H324 H 0.5215 0.6298 0.5799 0.043 Uiso 1 1 calc R . . C325 C 0.4762(3) 0.7026(3) 0.67696(19) 0.0381(8) Uani 1 1 d . . . H325 H 0.4013 0.6966 0.6903 0.046 Uiso 1 1 calc R . . C326 C 0.5160(3) 0.7799(3) 0.78632(17) 0.0338(7) Uani 1 1 d . . . H32A H 0.4275 0.8003 0.7988 0.041 Uiso 1 1 calc R . . H32B H 0.5328 0.8474 0.7933 0.041 Uiso 1 1 calc R . . C331 C 0.5992(3) 0.6832(3) 0.83275(17) 0.0309(7) Uani 1 1 d . . . C332 C 0.6647(3) 0.5759(3) 0.80777(17) 0.0335(7) Uani 1 1 d . . . H332 H 0.6541 0.5616 0.7612 0.040 Uiso 1 1 calc R . . C333 C 0.7470(3) 0.4869(3) 0.84961(18) 0.0361(7) Uani 1 1 d . . . H333 H 0.7906 0.4129 0.8317 0.043 Uiso 1 1 calc R . . C334 C 0.7642(3) 0.5074(3) 0.91632(17) 0.0350(7) Uani 1 1 d . . . C335 C 0.6979(3) 0.6169(3) 0.94561(17) 0.0347(7) Uani 1 1 d . . . C336 C 0.6116(3) 0.7056(3) 0.90313(17) 0.0330(7) Uani 1 1 d . . . C341 C 0.5435(4) 0.8132(3) 0.93285(19) 0.0404(8) Uani 1 1 d . . . H341 H 0.4841 0.8735 0.9061 0.048 Uiso 1 1 calc R . . C342 C 0.5627(4) 0.8311(4) 1.0001(2) 0.0522(10) Uani 1 1 d . . . H342 H 0.5159 0.9037 1.0193 0.063 Uiso 1 1 calc R . . C343 C 0.6493(5) 0.7450(4) 1.0405(2) 0.0530(11) Uani 1 1 d . . . H343 H 0.6625 0.7594 1.0867 0.064 Uiso 1 1 calc R . . C344 C 0.7153(4) 0.6399(4) 1.01414(19) 0.0443(9) Uani 1 1 d . . . H344 H 0.7739 0.5812 1.0422 0.053 Uiso 1 1 calc R . . C351 C 0.8559(4) 0.4179(3) 0.95685(19) 0.0424(8) Uani 1 1 d . . . N352 N 0.9316(4) 0.3464(3) 0.98823(19) 0.0598(10) Uani 1 1 d . . . B11X B 0.2530(4) 0.0845(4) 0.7527(2) 0.0765(12) Uiso 0.416(3) 1 d PDU A 1 F12X F 0.1401(5) 0.1067(6) 0.7849(3) 0.0789(15) Uiso 0.416(3) 1 d PDU A 1 F13X F 0.2874(6) -0.0106(4) 0.7128(3) 0.0779(16) Uiso 0.416(3) 1 d PDU A 1 F14X F 0.2417(6) 0.1767(4) 0.7113(3) 0.0813(19) Uiso 0.416(3) 1 d PDU A 1 F15X F 0.3431(5) 0.0650(5) 0.8016(3) 0.0772(13) Uiso 0.416(3) 1 d PDU A 1 B11Y B 0.2670(3) 0.0945(3) 0.80050(18) 0.0740(11) Uiso 0.584(3) 1 d PDU A 2 F12Y F 0.1490(3) 0.0980(5) 0.7980(3) 0.0811(13) Uiso 0.584(3) 1 d PDU A 2 F13Y F 0.3365(4) 0.0382(4) 0.74408(19) 0.0815(12) Uiso 0.584(3) 1 d PDU A 2 F14Y F 0.2581(4) 0.2041(3) 0.8003(2) 0.0664(12) Uiso 0.584(3) 1 d PDU A 2 F15Y F 0.3251(4) 0.0376(4) 0.86000(19) 0.0806(13) Uiso 0.584(3) 1 d PDU A 2 B21 B 0.2451(4) 0.6665(4) 0.5326(2) 0.0357(5) Uani 1 1 d U . . F22 F 0.19098(19) 0.61311(17) 0.57788(10) 0.0366(4) Uani 1 1 d U . . F23 F 0.3502(2) 0.5845(2) 0.50199(12) 0.0550(6) Uani 1 1 d U . . F24 F 0.2794(2) 0.7382(2) 0.57028(11) 0.0440(5) Uani 1 1 d U . . F25 F 0.1595(2) 0.73094(19) 0.48350(11) 0.0417(5) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01542(18) 0.01448(18) 0.01669(17) 0.00359(12) -0.00313(12) -0.00697(13) N111 0.0253(13) 0.0251(13) 0.0312(13) 0.0038(10) -0.0037(10) -0.0121(11) C112 0.0264(15) 0.0263(15) 0.0314(15) 0.0055(12) -0.0044(12) -0.0131(13) C113 0.0371(18) 0.0319(17) 0.0352(17) 0.0054(13) -0.0106(14) -0.0136(15) C114 0.0355(18) 0.0300(17) 0.047(2) 0.0077(15) -0.0120(15) -0.0090(15) C115 0.0332(17) 0.0271(16) 0.0455(19) 0.0001(14) -0.0051(14) -0.0113(14) C116 0.0297(16) 0.0263(15) 0.0369(17) 0.0012(13) -0.0027(13) -0.0129(13) N121 0.0342(14) 0.0257(13) 0.0287(13) 0.0017(10) 0.0011(11) -0.0112(11) N122 0.0281(13) 0.0220(12) 0.0287(13) 0.0033(10) -0.0001(10) -0.0099(10) C124 0.0387(18) 0.0334(17) 0.0298(16) 0.0063(13) -0.0059(13) -0.0156(15) C125 0.044(2) 0.0338(17) 0.0275(16) 0.0006(13) -0.0016(14) -0.0158(15) C126 0.0294(16) 0.0274(16) 0.0327(16) 0.0026(12) 0.0010(13) -0.0102(13) C131 0.0284(15) 0.0235(14) 0.0270(14) -0.0022(11) 0.0024(12) -0.0091(12) C132 0.0308(17) 0.0281(16) 0.0336(16) 0.0009(13) -0.0004(13) -0.0085(13) C133 0.0301(17) 0.0356(18) 0.0430(19) -0.0066(14) 0.0023(14) -0.0162(14) C134 0.0425(19) 0.0282(16) 0.0324(16) -0.0070(13) 0.0084(14) -0.0184(15) C135 0.0407(18) 0.0255(15) 0.0267(15) -0.0033(12) 0.0024(13) -0.0137(14) C136 0.0330(16) 0.0223(14) 0.0278(15) -0.0024(11) 0.0021(12) -0.0091(13) C141 0.062(2) 0.0264(16) 0.0306(17) 0.0015(13) -0.0012(16) -0.0192(16) C142 0.059(2) 0.0275(17) 0.0391(19) 0.0045(14) -0.0155(17) -0.0108(17) C143 0.039(2) 0.0362(19) 0.047(2) -0.0012(16) -0.0129(16) -0.0087(16) C144 0.0349(18) 0.0287(17) 0.0399(18) -0.0003(14) -0.0039(14) -0.0100(14) C151 0.058(2) 0.043(2) 0.0351(18) -0.0113(15) 0.0106(16) -0.0316(19) N152 0.083(3) 0.062(2) 0.0415(18) -0.0092(16) 0.0109(18) -0.055(2) N211 0.0346(14) 0.0246(13) 0.0260(12) 0.0022(10) -0.0035(10) -0.0126(11) C123 0.0291(16) 0.0279(15) 0.0276(15) 0.0050(12) -0.0036(12) -0.0135(13) C212 0.0399(18) 0.0240(15) 0.0257(14) -0.0004(12) -0.0003(13) -0.0150(13) C213 0.053(2) 0.0289(17) 0.0315(17) 0.0040(13) -0.0022(15) -0.0163(16) C214 0.057(2) 0.0304(18) 0.0383(19) 0.0105(15) -0.0126(17) -0.0106(17) C215 0.042(2) 0.0317(18) 0.046(2) 0.0044(15) -0.0128(16) -0.0074(16) C216 0.0344(18) 0.0271(16) 0.0368(17) 0.0016(13) -0.0066(14) -0.0098(14) N221 0.0329(15) 0.0356(15) 0.0398(15) 0.0025(12) -0.0011(12) -0.0202(13) N222 0.0293(13) 0.0297(13) 0.0277(13) 0.0001(10) -0.0016(10) -0.0156(11) C223 0.0403(18) 0.0263(15) 0.0275(15) 0.0016(12) 0.0020(13) -0.0177(14) C224 0.048(2) 0.0356(19) 0.045(2) 0.0033(15) 0.0037(16) -0.0244(17) C225 0.042(2) 0.044(2) 0.059(2) 0.0050(18) 0.0032(18) -0.0277(18) C226 0.0285(16) 0.0338(17) 0.0371(17) -0.0017(13) -0.0017(13) -0.0155(14) C231 0.0328(17) 0.0363(17) 0.0328(16) -0.0030(13) 0.0054(13) -0.0216(14) C232 0.047(2) 0.0357(19) 0.047(2) -0.0055(16) 0.0050(17) -0.0192(17) C233 0.071(3) 0.040(2) 0.049(2) -0.0182(18) 0.013(2) -0.029(2) C234 0.068(3) 0.048(2) 0.0334(18) -0.0080(16) 0.0084(17) -0.039(2) C235 0.050(2) 0.047(2) 0.0296(16) -0.0024(14) 0.0050(15) -0.0330(18) C236 0.0346(17) 0.0361(17) 0.0303(16) -0.0011(13) 0.0034(13) -0.0233(15) C241 0.059(2) 0.060(2) 0.0271(16) 0.0046(16) -0.0052(16) -0.038(2) C242 0.048(2) 0.052(2) 0.0374(19) 0.0100(17) -0.0081(16) -0.0230(19) C243 0.043(2) 0.041(2) 0.0392(19) -0.0015(15) -0.0005(15) -0.0157(17) C244 0.0371(18) 0.0374(18) 0.0283(16) -0.0025(13) 0.0009(13) -0.0180(15) C251 0.092(4) 0.061(3) 0.038(2) -0.0142(19) 0.010(2) -0.051(3) N252 0.139(4) 0.084(3) 0.041(2) -0.019(2) 0.009(2) -0.071(3) N311 0.0244(13) 0.0260(13) 0.0295(13) 0.0018(10) -0.0036(10) -0.0103(10) C312 0.0259(15) 0.0240(15) 0.0333(16) 0.0039(12) -0.0098(12) -0.0080(12) C313 0.0318(17) 0.0352(18) 0.0401(18) -0.0047(14) -0.0115(14) -0.0115(14) C314 0.0355(19) 0.050(2) 0.0388(19) -0.0142(16) -0.0047(15) -0.0114(17) C315 0.0317(18) 0.054(2) 0.0356(18) -0.0079(16) 0.0007(14) -0.0136(17) C316 0.0257(15) 0.0368(18) 0.0324(16) -0.0021(13) -0.0005(12) -0.0122(14) N321 0.0246(13) 0.0346(15) 0.0349(14) 0.0127(11) -0.0055(11) -0.0142(11) N322 0.0237(12) 0.0272(13) 0.0322(13) 0.0068(10) -0.0034(10) -0.0119(11) C323 0.0263(15) 0.0244(15) 0.0332(16) 0.0077(12) -0.0090(12) -0.0107(12) C324 0.0396(19) 0.0363(18) 0.0394(18) 0.0137(14) -0.0163(15) -0.0232(15) C325 0.0314(17) 0.046(2) 0.0441(19) 0.0190(16) -0.0121(14) -0.0236(16) C326 0.0282(16) 0.0355(18) 0.0374(17) 0.0084(14) 0.0021(13) -0.0139(14) C331 0.0277(16) 0.0318(17) 0.0344(16) 0.0072(13) -0.0010(13) -0.0143(13) C332 0.0390(18) 0.0328(17) 0.0299(16) 0.0056(13) -0.0075(13) -0.0165(15) C333 0.0422(19) 0.0294(17) 0.0339(17) 0.0038(13) -0.0057(14) -0.0127(15) C334 0.0360(18) 0.0348(18) 0.0326(16) 0.0069(13) -0.0050(14) -0.0138(15) C335 0.0372(18) 0.0393(19) 0.0314(16) 0.0042(14) 0.0018(13) -0.0202(15) C336 0.0335(17) 0.0342(17) 0.0329(16) 0.0047(13) 0.0034(13) -0.0163(14) C341 0.0397(19) 0.0374(19) 0.0405(19) 0.0023(15) 0.0097(15) -0.0136(16) C342 0.063(3) 0.044(2) 0.046(2) -0.0078(18) 0.0174(19) -0.019(2) C343 0.070(3) 0.055(3) 0.0327(19) -0.0051(17) 0.0056(18) -0.026(2) C344 0.051(2) 0.049(2) 0.0321(18) 0.0010(16) -0.0020(16) -0.0213(19) C351 0.049(2) 0.043(2) 0.0336(18) 0.0046(15) -0.0092(16) -0.0171(18) N352 0.064(2) 0.053(2) 0.049(2) 0.0111(17) -0.0229(18) -0.0104(19) B21 0.0359(12) 0.0427(13) 0.0318(12) 0.0047(9) -0.0032(9) -0.0201(9) F22 0.0377(10) 0.0397(10) 0.0339(9) 0.0040(8) -0.0005(8) -0.0183(8) F23 0.0499(12) 0.0528(13) 0.0475(12) 0.0069(10) 0.0138(9) -0.0086(10) F24 0.0454(11) 0.0610(13) 0.0380(10) 0.0039(9) -0.0074(8) -0.0345(10) F25 0.0441(11) 0.0468(11) 0.0402(10) 0.0108(8) -0.0146(8) -0.0251(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N211 2.148(3) . ? Co1 N111 2.153(3) . ? Co1 N322 2.177(3) . ? Co1 N311 2.180(3) . ? Co1 N122 2.190(3) . ? Co1 N222 2.192(3) . ? N111 C116 1.339(4) . ? N111 C112 1.346(4) . ? C112 C113 1.388(4) . ? C112 C123 1.465(4) . ? C113 C114 1.392(5) . ? C113 H113 0.9500 . ? C114 C115 1.373(5) . ? C114 H114 0.9500 . ? C115 C116 1.382(5) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? N121 N122 1.347(4) . ? N121 C125 1.351(4) . ? N121 C126 1.455(4) . ? N122 C123 1.344(4) . ? C124 C125 1.368(5) . ? C124 C123 1.398(5) . ? C124 H124 0.9500 . ? C125 H125 0.9500 . ? C126 C131 1.514(4) . ? C126 H12A 0.9900 . ? C126 H12B 0.9900 . ? C131 C132 1.368(5) . ? C131 C136 1.427(4) . ? C132 C133 1.402(5) . ? C132 H132 0.9500 . ? C133 C134 1.368(5) . ? C133 H133 0.9500 . ? C134 C135 1.430(5) . ? C134 C151 1.437(5) . ? C135 C141 1.411(5) . ? C135 C136 1.423(5) . ? C136 C144 1.420(5) . ? C141 C142 1.358(6) . ? C141 H141 0.9500 . ? C142 C143 1.401(6) . ? C142 H142 0.9500 . ? C143 C144 1.373(5) . ? C143 H143 0.9500 . ? C144 H144 0.9500 . ? C151 N152 1.147(5) . ? N211 C216 1.343(4) . ? N211 C212 1.353(4) . ? C212 C213 1.388(5) . ? C212 C223 1.465(5) . ? C213 C214 1.377(6) . ? C213 H213 0.9500 . ? C214 C215 1.391(6) . ? C214 H214 0.9500 . ? C215 C216 1.372(5) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? N221 N222 1.349(4) . ? N221 C225 1.353(5) . ? N221 C226 1.451(4) . ? N222 C223 1.343(4) . ? C223 C224 1.397(5) . ? C224 C225 1.363(6) . ? C224 H224 0.9500 . ? C225 H225 0.9500 . ? C226 C231 1.515(5) . ? C226 H22A 0.9900 . ? C226 H22B 0.9900 . ? C231 C232 1.366(5) . ? C231 C236 1.433(5) . ? C232 C233 1.417(6) . ? C232 H232 0.9500 . ? C233 C234 1.360(6) . ? C233 H233 0.9500 . ? C234 C235 1.425(5) . ? C234 C251 1.440(6) . ? C235 C236 1.417(5) . ? C235 C241 1.420(6) . ? C236 C244 1.414(5) . ? C241 C242 1.352(6) . ? C241 H241 0.9500 . ? C242 C243 1.403(5) . ? C242 H242 0.9500 . ? C243 C244 1.372(5) . ? C243 H243 0.9500 . ? C244 H244 0.9500 . ? C251 N252 1.159(6) . ? N311 C316 1.338(4) . ? N311 C312 1.350(4) . ? C312 C313 1.386(5) . ? C312 C323 1.465(5) . ? C313 C314 1.377(5) . ? C313 H313 0.9500 . ? C314 C315 1.378(5) . ? C314 H314 0.9500 . ? C315 C316 1.386(5) . ? C315 H315 0.9500 . ? C316 H316 0.9500 . ? N321 C325 1.347(5) . ? N321 N322 1.351(4) . ? N321 C326 1.458(4) . ? N322 C323 1.339(4) . ? C323 C324 1.396(4) . ? C324 C325 1.368(5) . ? C324 H324 0.9500 . ? C325 H325 0.9500 . ? C326 C331 1.510(4) . ? C326 H32A 0.9900 . ? C326 H32B 0.9900 . ? C331 C332 1.372(5) . ? C331 C336 1.430(5) . ? C332 C333 1.403(5) . ? C332 H332 0.9500 . ? C333 C334 1.367(5) . ? C333 H333 0.9500 . ? C334 C335 1.428(5) . ? C334 C351 1.436(5) . ? C335 C344 1.411(5) . ? C335 C336 1.425(5) . ? C336 C341 1.416(5) . ? C341 C342 1.374(6) . ? C341 H341 0.9500 . ? C342 C343 1.388(6) . ? C342 H342 0.9500 . ? C343 C344 1.362(6) . ? C343 H343 0.9500 . ? C344 H344 0.9500 . ? C351 N352 1.149(5) . ? B11X F12X 1.379(2) . ? B11X F14X 1.381(2) . ? B11X F13X 1.381(2) . ? B11X F15X 1.381(2) . ? B11Y F12Y 1.379(2) . ? B11Y F14Y 1.380(2) . ? B11Y F13Y 1.381(2) . ? B11Y F15Y 1.381(2) . ? B21 F25 1.383(4) . ? B21 F23 1.384(5) . ? B21 F24 1.393(5) . ? B21 F22 1.404(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 N211 Co1 N111 175.05(10) . . ? N211 Co1 N322 91.80(10) . . ? N111 Co1 N322 93.08(10) . . ? N211 Co1 N311 87.55(10) . . ? N111 Co1 N311 94.42(10) . . ? N322 Co1 N311 76.16(10) . . ? N211 Co1 N122 101.95(10) . . ? N111 Co1 N122 76.26(10) . . ? N322 Co1 N122 101.43(10) . . ? N311 Co1 N122 170.33(9) . . ? N211 Co1 N222 77.09(10) . . ? N111 Co1 N222 98.30(10) . . ? N322 Co1 N222 163.85(10) . . ? N311 Co1 N222 91.50(10) . . ? N122 Co1 N222 92.41(10) . . ? C116 N111 C112 118.4(3) . . ? C116 N111 Co1 125.6(2) . . ? C112 N111 Co1 116.0(2) . . ? N111 C112 C113 122.2(3) . . ? N111 C112 C123 115.5(3) . . ? C113 C112 C123 122.3(3) . . ? C112 C113 C114 118.3(3) . . ? C112 C113 H113 120.8 . . ? C114 C113 H113 120.8 . . ? C115 C114 C113 119.6(3) . . ? C115 C114 H114 120.2 . . ? C113 C114 H114 120.2 . . ? C114 C115 C116 118.6(3) . . ? C114 C115 H115 120.7 . . ? C116 C115 H115 120.7 . . ? N111 C116 C115 122.9(3) . . ? N111 C116 H116 118.6 . . ? C115 C116 H116 118.6 . . ? N122 N121 C125 111.3(3) . . ? N122 N121 C126 121.0(3) . . ? C125 N121 C126 127.6(3) . . ? C123 N122 N121 105.1(2) . . ? C123 N122 Co1 113.0(2) . . ? N121 N122 Co1 140.7(2) . . ? C125 C124 C123 104.7(3) . . ? C125 C124 H124 127.7 . . ? C123 C124 H124 127.7 . . ? N121 C125 C124 107.8(3) . . ? N121 C125 H125 126.1 . . ? C124 C125 H125 126.1 . . ? N121 C126 C131 112.8(3) . . ? N121 C126 H12A 109.0 . . ? C131 C126 H12A 109.0 . . ? N121 C126 H12B 109.0 . . ? C131 C126 H12B 109.0 . . ? H12A C126 H12B 107.8 . . ? C132 C131 C136 120.1(3) . . ? C132 C131 C126 121.5(3) . . ? C136 C131 C126 118.3(3) . . ? C131 C132 C133 121.4(3) . . ? C131 C132 H132 119.3 . . ? C133 C132 H132 119.3 . . ? C134 C133 C132 119.8(3) . . ? C134 C133 H133 120.1 . . ? C132 C133 H133 120.1 . . ? C133 C134 C135 121.2(3) . . ? C133 C134 C151 120.2(3) . . ? C135 C134 C151 118.5(3) . . ? C141 C135 C136 119.2(3) . . ? C141 C135 C134 122.4(3) . . ? C136 C135 C134 118.3(3) . . ? C144 C136 C135 118.4(3) . . ? C144 C136 C131 122.6(3) . . ? C135 C136 C131 119.0(3) . . ? C142 C141 C135 121.1(3) . . ? C142 C141 H141 119.5 . . ? C135 C141 H141 119.5 . . ? C141 C142 C143 120.1(3) . . ? C141 C142 H142 120.0 . . ? C143 C142 H142 120.0 . . ? C144 C143 C142 120.9(4) . . ? C144 C143 H143 119.6 . . ? C142 C143 H143 119.6 . . ? C143 C144 C136 120.3(4) . . ? C143 C144 H144 119.9 . . ? C136 C144 H144 119.9 . . ? N152 C151 C134 178.2(4) . . ? C216 N211 C212 118.2(3) . . ? C216 N211 Co1 125.8(2) . . ? C212 N211 Co1 114.5(2) . . ? N122 C123 C124 111.0(3) . . ? N122 C123 C112 118.2(3) . . ? C124 C123 C112 130.7(3) . . ? N211 C212 C213 122.1(3) . . ? N211 C212 C223 116.0(3) . . ? C213 C212 C223 121.9(3) . . ? C214 C213 C212 118.7(4) . . ? C214 C213 H213 120.7 . . ? C212 C213 H213 120.7 . . ? C213 C214 C215 119.5(3) . . ? C213 C214 H214 120.3 . . ? C215 C214 H214 120.3 . . ? C216 C215 C214 118.6(4) . . ? C216 C215 H215 120.7 . . ? C214 C215 H215 120.7 . . ? N211 C216 C215 123.0(4) . . ? N211 C216 H216 118.5 . . ? C215 C216 H216 118.5 . . ? N222 N221 C225 110.8(3) . . ? N222 N221 C226 121.7(3) . . ? C225 N221 C226 127.2(3) . . ? C223 N222 N221 105.5(3) . . ? C223 N222 Co1 112.4(2) . . ? N221 N222 Co1 141.9(2) . . ? N222 C223 C224 110.7(3) . . ? N222 C223 C212 118.6(3) . . ? C224 C223 C212 130.7(3) . . ? C225 C224 C223 105.0(3) . . ? C225 C224 H224 127.5 . . ? C223 C224 H224 127.5 . . ? N221 C225 C224 108.0(3) . . ? N221 C225 H225 126.0 . . ? C224 C225 H225 126.0 . . ? N221 C226 C231 115.2(3) . . ? N221 C226 H22A 108.5 . . ? C231 C226 H22A 108.5 . . ? N221 C226 H22B 108.5 . . ? C231 C226 H22B 108.5 . . ? H22A C226 H22B 107.5 . . ? C232 C231 C236 119.5(3) . . ? C232 C231 C226 122.3(3) . . ? C236 C231 C226 118.2(3) . . ? C231 C232 C233 121.1(4) . . ? C231 C232 H232 119.5 . . ? C233 C232 H232 119.5 . . ? C234 C233 C232 120.2(4) . . ? C234 C233 H233 119.9 . . ? C232 C233 H233 119.9 . . ? C233 C234 C235 121.0(3) . . ? C233 C234 C251 120.3(4) . . ? C235 C234 C251 118.7(4) . . ? C236 C235 C241 119.5(3) . . ? C236 C235 C234 118.5(4) . . ? C241 C235 C234 122.0(3) . . ? C244 C236 C235 117.7(3) . . ? C244 C236 C231 122.6(3) . . ? C235 C236 C231 119.6(3) . . ? C242 C241 C235 121.1(3) . . ? C242 C241 H241 119.4 . . ? C235 C241 H241 119.4 . . ? C241 C242 C243 119.9(4) . . ? C241 C242 H242 120.0 . . ? C243 C242 H242 120.0 . . ? C244 C243 C242 120.6(4) . . ? C244 C243 H243 119.7 . . ? C242 C243 H243 119.7 . . ? C243 C244 C236 121.1(3) . . ? C243 C244 H244 119.4 . . ? C236 C244 H244 119.4 . . ? N252 C251 C234 178.3(6) . . ? C316 N311 C312 118.2(3) . . ? C316 N311 Co1 126.3(2) . . ? C312 N311 Co1 115.5(2) . . ? N311 C312 C313 122.3(3) . . ? N311 C312 C323 115.4(3) . . ? C313 C312 C323 122.4(3) . . ? C314 C313 C312 118.5(3) . . ? C314 C313 H313 120.7 . . ? C312 C313 H313 120.7 . . ? C313 C314 C315 119.9(3) . . ? C313 C314 H314 120.1 . . ? C315 C314 H314 120.1 . . ? C314 C315 C316 118.3(3) . . ? C314 C315 H315 120.8 . . ? C316 C315 H315 120.8 . . ? N311 C316 C315 122.7(3) . . ? N311 C316 H316 118.6 . . ? C315 C316 H316 118.6 . . ? C325 N321 N322 111.2(3) . . ? C325 N321 C326 127.1(3) . . ? N322 N321 C326 120.3(3) . . ? C323 N322 N321 105.2(3) . . ? C323 N322 Co1 114.1(2) . . ? N321 N322 Co1 140.1(2) . . ? N322 C323 C324 111.1(3) . . ? N322 C323 C312 118.7(3) . . ? C324 C323 C312 130.2(3) . . ? C325 C324 C323 104.7(3) . . ? C325 C324 H324 127.6 . . ? C323 C324 H324 127.6 . . ? N321 C325 C324 107.8(3) . . ? N321 C325 H325 126.1 . . ? C324 C325 H325 126.1 . . ? N321 C326 C331 111.4(3) . . ? N321 C326 H32A 109.4 . . ? C331 C326 H32A 109.4 . . ? N321 C326 H32B 109.4 . . ? C331 C326 H32B 109.4 . . ? H32A C326 H32B 108.0 . . ? C332 C331 C336 120.1(3) . . ? C332 C331 C326 120.9(3) . . ? C336 C331 C326 118.9(3) . . ? C331 C332 C333 121.3(3) . . ? C331 C332 H332 119.3 . . ? C333 C332 H332 119.3 . . ? C334 C333 C332 119.6(3) . . ? C334 C333 H333 120.2 . . ? C332 C333 H333 120.2 . . ? C333 C334 C335 121.8(3) . . ? C333 C334 C351 118.9(3) . . ? C335 C334 C351 119.2(3) . . ? C344 C335 C336 119.5(3) . . ? C344 C335 C334 122.6(3) . . ? C336 C335 C334 118.0(3) . . ? C341 C336 C335 117.9(3) . . ? C341 C336 C331 123.0(3) . . ? C335 C336 C331 119.1(3) . . ? C342 C341 C336 120.5(4) . . ? C342 C341 H341 119.7 . . ? C336 C341 H341 119.7 . . ? C341 C342 C343 121.2(4) . . ? C341 C342 H342 119.4 . . ? C343 C342 H342 119.4 . . ? C344 C343 C342 120.0(4) . . ? C344 C343 H343 120.0 . . ? C342 C343 H343 120.0 . . ? C343 C344 C335 120.9(4) . . ? C343 C344 H344 119.6 . . ? C335 C344 H344 119.6 . . ? N352 C351 C334 178.3(5) . . ? F12X B11X F14X 109.48(16) . . ? F12X B11X F13X 109.49(16) . . ? F14X B11X F13X 109.43(15) . . ? F12X B11X F15X 109.55(16) . . ? F14X B11X F15X 109.54(16) . . ? F13X B11X F15X 109.33(15) . . ? F12Y B11Y F14Y 109.48(15) . . ? F12Y B11Y F13Y 109.81(15) . . ? F14Y B11Y F13Y 109.51(15) . . ? F12Y B11Y F15Y 109.48(15) . . ? F14Y B11Y F15Y 109.36(15) . . ? F13Y B11Y F15Y 109.19(15) . . ? F25 B21 F23 110.8(3) . . ? F25 B21 F24 108.8(3) . . ? F23 B21 F24 109.3(3) . . ? F25 B21 F22 110.0(3) . . ? F23 B21 F22 109.2(3) . . ? F24 B21 F22 108.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N211 Co1 N111 C116 -116.9(11) . . . . ? N322 Co1 N111 C116 72.7(3) . . . . ? N311 Co1 N111 C116 -3.6(3) . . . . ? N122 Co1 N111 C116 173.7(3) . . . . ? N222 Co1 N111 C116 -95.8(3) . . . . ? N211 Co1 N111 C112 63.5(12) . . . . ? N322 Co1 N111 C112 -106.8(2) . . . . ? N311 Co1 N111 C112 176.8(2) . . . . ? N122 Co1 N111 C112 -5.8(2) . . . . ? N222 Co1 N111 C112 84.6(2) . . . . ? C116 N111 C112 C113 1.5(5) . . . . ? Co1 N111 C112 C113 -178.9(3) . . . . ? C116 N111 C112 C123 -177.5(3) . . . . ? Co1 N111 C112 C123 2.1(3) . . . . ? N111 C112 C113 C114 -1.4(5) . . . . ? C123 C112 C113 C114 177.5(3) . . . . ? C112 C113 C114 C115 0.2(5) . . . . ? C113 C114 C115 C116 0.7(5) . . . . ? C112 N111 C116 C115 -0.5(5) . . . . ? Co1 N111 C116 C115 180.0(2) . . . . ? C114 C115 C116 N111 -0.6(5) . . . . ? C125 N121 N122 C123 0.4(4) . . . . ? C126 N121 N122 C123 176.7(3) . . . . ? C125 N121 N122 Co1 -165.7(3) . . . . ? C126 N121 N122 Co1 10.7(5) . . . . ? N211 Co1 N122 C123 -166.4(2) . . . . ? N111 Co1 N122 C123 8.8(2) . . . . ? N322 Co1 N122 C123 99.2(2) . . . . ? N311 Co1 N122 C123 24.7(7) . . . . ? N222 Co1 N122 C123 -89.1(2) . . . . ? N211 Co1 N122 N121 -1.1(3) . . . . ? N111 Co1 N122 N121 174.2(3) . . . . ? N322 Co1 N122 N121 -95.4(3) . . . . ? N311 Co1 N122 N121 -170.0(5) . . . . ? N222 Co1 N122 N121 76.2(3) . . . . ? N122 N121 C125 C124 -0.3(4) . . . . ? C126 N121 C125 C124 -176.4(3) . . . . ? C123 C124 C125 N121 0.2(4) . . . . ? N122 N121 C126 C131 -86.4(4) . . . . ? C125 N121 C126 C131 89.3(4) . . . . ? N121 C126 C131 C132 -17.4(4) . . . . ? N121 C126 C131 C136 164.8(3) . . . . ? C136 C131 C132 C133 -1.9(5) . . . . ? C126 C131 C132 C133 -179.6(3) . . . . ? C131 C132 C133 C134 -0.2(5) . . . . ? C132 C133 C134 C135 1.4(5) . . . . ? C132 C133 C134 C151 -179.8(3) . . . . ? C133 C134 C135 C141 179.7(3) . . . . ? C151 C134 C135 C141 0.8(5) . . . . ? C133 C134 C135 C136 -0.4(5) . . . . ? C151 C134 C135 C136 -179.3(3) . . . . ? C141 C135 C136 C144 -1.4(4) . . . . ? C134 C135 C136 C144 178.8(3) . . . . ? C141 C135 C136 C131 178.3(3) . . . . ? C134 C135 C136 C131 -1.6(4) . . . . ? C132 C131 C136 C144 -177.7(3) . . . . ? C126 C131 C136 C144 0.1(4) . . . . ? C132 C131 C136 C135 2.7(4) . . . . ? C126 C131 C136 C135 -179.5(3) . . . . ? C136 C135 C141 C142 1.4(5) . . . . ? C134 C135 C141 C142 -178.7(3) . . . . ? C135 C141 C142 C143 0.0(5) . . . . ? C141 C142 C143 C144 -1.6(6) . . . . ? C142 C143 C144 C136 1.6(6) . . . . ? C135 C136 C144 C143 -0.1(5) . . . . ? C131 C136 C144 C143 -179.7(3) . . . . ? C133 C134 C151 N152 -125(15) . . . . ? C135 C134 C151 N152 54(15) . . . . ? N111 Co1 N211 C216 -162.3(11) . . . . ? N322 Co1 N211 C216 8.0(3) . . . . ? N311 Co1 N211 C216 84.1(3) . . . . ? N122 Co1 N211 C216 -94.0(3) . . . . ? N222 Co1 N211 C216 176.2(3) . . . . ? N111 Co1 N211 C212 32.0(13) . . . . ? N322 Co1 N211 C212 -157.7(2) . . . . ? N311 Co1 N211 C212 -81.6(2) . . . . ? N122 Co1 N211 C212 100.3(2) . . . . ? N222 Co1 N211 C212 10.5(2) . . . . ? N121 N122 C123 C124 -0.2(4) . . . . ? Co1 N122 C123 C124 170.2(2) . . . . ? N121 N122 C123 C112 178.7(3) . . . . ? Co1 N122 C123 C112 -10.9(4) . . . . ? C125 C124 C123 N122 0.0(4) . . . . ? C125 C124 C123 C112 -178.7(3) . . . . ? N111 C112 C123 N122 6.1(4) . . . . ? C113 C112 C123 N122 -172.8(3) . . . . ? N111 C112 C123 C124 -175.2(3) . . . . ? C113 C112 C123 C124 5.8(6) . . . . ? C216 N211 C212 C213 -1.3(5) . . . . ? Co1 N211 C212 C213 165.6(3) . . . . ? C216 N211 C212 C223 -179.5(3) . . . . ? Co1 N211 C212 C223 -12.6(3) . . . . ? N211 C212 C213 C214 0.1(5) . . . . ? C223 C212 C213 C214 178.2(3) . . . . ? C212 C213 C214 C215 1.2(5) . . . . ? C213 C214 C215 C216 -1.3(6) . . . . ? C212 N211 C216 C215 1.2(5) . . . . ? Co1 N211 C216 C215 -164.0(3) . . . . ? C214 C215 C216 N211 0.0(6) . . . . ? C225 N221 N222 C223 0.5(4) . . . . ? C226 N221 N222 C223 -174.0(3) . . . . ? C225 N221 N222 Co1 174.9(3) . . . . ? C226 N221 N222 Co1 0.4(5) . . . . ? N211 Co1 N222 C223 -6.7(2) . . . . ? N111 Co1 N222 C223 175.1(2) . . . . ? N322 Co1 N222 C223 40.7(5) . . . . ? N311 Co1 N222 C223 80.4(2) . . . . ? N122 Co1 N222 C223 -108.5(2) . . . . ? N211 Co1 N222 N221 179.0(4) . . . . ? N111 Co1 N222 N221 0.9(4) . . . . ? N322 Co1 N222 N221 -133.5(4) . . . . ? N311 Co1 N222 N221 -93.8(3) . . . . ? N122 Co1 N222 N221 77.3(3) . . . . ? N221 N222 C223 C224 -0.6(4) . . . . ? Co1 N222 C223 C224 -176.9(2) . . . . ? N221 N222 C223 C212 178.8(3) . . . . ? Co1 N222 C223 C212 2.5(4) . . . . ? N211 C212 C223 N222 6.8(4) . . . . ? C213 C212 C223 N222 -171.4(3) . . . . ? N211 C212 C223 C224 -174.0(3) . . . . ? C213 C212 C223 C224 7.9(6) . . . . ? N222 C223 C224 C225 0.6(4) . . . . ? C212 C223 C224 C225 -178.7(3) . . . . ? N222 N221 C225 C224 -0.1(4) . . . . ? C226 N221 C225 C224 174.0(3) . . . . ? C223 C224 C225 N221 -0.3(4) . . . . ? N222 N221 C226 C231 -104.6(3) . . . . ? C225 N221 C226 C231 81.9(4) . . . . ? N221 C226 C231 C232 1.6(5) . . . . ? N221 C226 C231 C236 -177.0(3) . . . . ? C236 C231 C232 C233 -1.7(5) . . . . ? C226 C231 C232 C233 179.7(3) . . . . ? C231 C232 C233 C234 0.5(6) . . . . ? C232 C233 C234 C235 1.9(6) . . . . ? C232 C233 C234 C251 -178.6(4) . . . . ? C233 C234 C235 C236 -3.0(6) . . . . ? C251 C234 C235 C236 177.5(3) . . . . ? C233 C234 C235 C241 176.8(4) . . . . ? C251 C234 C235 C241 -2.6(6) . . . . ? C241 C235 C236 C244 0.4(5) . . . . ? C234 C235 C236 C244 -179.7(3) . . . . ? C241 C235 C236 C231 -178.1(3) . . . . ? C234 C235 C236 C231 1.8(5) . . . . ? C232 C231 C236 C244 -177.9(3) . . . . ? C226 C231 C236 C244 0.7(5) . . . . ? C232 C231 C236 C235 0.6(5) . . . . ? C226 C231 C236 C235 179.2(3) . . . . ? C236 C235 C241 C242 0.5(6) . . . . ? C234 C235 C241 C242 -179.4(4) . . . . ? C235 C241 C242 C243 -0.6(6) . . . . ? C241 C242 C243 C244 -0.1(6) . . . . ? C242 C243 C244 C236 1.0(6) . . . . ? C235 C236 C244 C243 -1.1(5) . . . . ? C231 C236 C244 C243 177.3(3) . . . . ? C233 C234 C251 N252 -169(17) . . . . ? C235 C234 C251 N252 11(18) . . . . ? N211 Co1 N311 C316 87.4(3) . . . . ? N111 Co1 N311 C316 -88.0(3) . . . . ? N322 Co1 N311 C316 179.9(3) . . . . ? N122 Co1 N311 C316 -103.5(6) . . . . ? N222 Co1 N311 C316 10.4(3) . . . . ? N211 Co1 N311 C312 -93.0(2) . . . . ? N111 Co1 N311 C312 91.5(2) . . . . ? N322 Co1 N311 C312 -0.6(2) . . . . ? N122 Co1 N311 C312 76.1(6) . . . . ? N222 Co1 N311 C312 -170.0(2) . . . . ? C316 N311 C312 C313 2.2(5) . . . . ? Co1 N311 C312 C313 -177.4(2) . . . . ? C316 N311 C312 C323 -177.7(3) . . . . ? Co1 N311 C312 C323 2.6(3) . . . . ? N311 C312 C313 C314 -1.6(5) . . . . ? C323 C312 C313 C314 178.4(3) . . . . ? C312 C313 C314 C315 -0.4(6) . . . . ? C313 C314 C315 C316 1.5(6) . . . . ? C312 N311 C316 C315 -1.0(5) . . . . ? Co1 N311 C316 C315 178.6(3) . . . . ? C314 C315 C316 N311 -0.9(6) . . . . ? C325 N321 N322 C323 1.0(3) . . . . ? C326 N321 N322 C323 168.5(3) . . . . ? C325 N321 N322 Co1 171.3(3) . . . . ? C326 N321 N322 Co1 -21.1(5) . . . . ? N211 Co1 N322 C323 85.2(2) . . . . ? N111 Co1 N322 C323 -95.6(2) . . . . ? N311 Co1 N322 C323 -1.8(2) . . . . ? N122 Co1 N322 C323 -172.2(2) . . . . ? N222 Co1 N322 C323 39.3(5) . . . . ? N211 Co1 N322 N321 -84.5(3) . . . . ? N111 Co1 N322 N321 94.6(3) . . . . ? N311 Co1 N322 N321 -171.6(3) . . . . ? N122 Co1 N322 N321 18.0(3) . . . . ? N222 Co1 N322 N321 -130.5(4) . . . . ? N321 N322 C323 C324 -0.6(3) . . . . ? Co1 N322 C323 C324 -173.9(2) . . . . ? N321 N322 C323 C312 177.1(3) . . . . ? Co1 N322 C323 C312 3.9(3) . . . . ? N311 C312 C323 N322 -4.4(4) . . . . ? C313 C312 C323 N322 175.6(3) . . . . ? N311 C312 C323 C324 172.8(3) . . . . ? C313 C312 C323 C324 -7.2(5) . . . . ? N322 C323 C324 C325 0.0(4) . . . . ? C312 C323 C324 C325 -177.4(3) . . . . ? N322 N321 C325 C324 -1.0(4) . . . . ? C326 N321 C325 C324 -167.5(3) . . . . ? C323 C324 C325 N321 0.6(4) . . . . ? C325 N321 C326 C331 91.6(4) . . . . ? N322 N321 C326 C331 -73.8(4) . . . . ? N321 C326 C331 C332 -11.9(4) . . . . ? N321 C326 C331 C336 166.4(3) . . . . ? C336 C331 C332 C333 -1.5(5) . . . . ? C326 C331 C332 C333 176.7(3) . . . . ? C331 C332 C333 C334 -1.1(5) . . . . ? C332 C333 C334 C335 1.7(6) . . . . ? C332 C333 C334 C351 -175.2(3) . . . . ? C333 C334 C335 C344 -179.4(4) . . . . ? C351 C334 C335 C344 -2.5(5) . . . . ? C333 C334 C335 C336 0.2(5) . . . . ? C351 C334 C335 C336 177.1(3) . . . . ? C344 C335 C336 C341 -2.1(5) . . . . ? C334 C335 C336 C341 178.3(3) . . . . ? C344 C335 C336 C331 176.9(3) . . . . ? C334 C335 C336 C331 -2.7(5) . . . . ? C332 C331 C336 C341 -177.7(3) . . . . ? C326 C331 C336 C341 4.0(5) . . . . ? C332 C331 C336 C335 3.4(5) . . . . ? C326 C331 C336 C335 -174.9(3) . . . . ? C335 C336 C341 C342 1.4(5) . . . . ? C331 C336 C341 C342 -177.5(4) . . . . ? C336 C341 C342 C343 0.3(6) . . . . ? C341 C342 C343 C344 -1.3(7) . . . . ? C342 C343 C344 C335 0.5(7) . . . . ? C336 C335 C344 C343 1.2(6) . . . . ? C334 C335 C344 C343 -179.3(4) . . . . ? C333 C334 C351 N352 69(15) . . . . ? C335 C334 C351 N352 -108(15) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.488 _refine_diff_density_min -1.258 _refine_diff_density_rms 0.092 #===END data_imw1294p-1 _database_code_depnum_ccdc_archive 'CCDC 758092' #TrackingRef 'mixed_metal_networks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H42 B2 F8 N12 Ni' _chemical_formula_weight 1163.39 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0001(3) _cell_length_b 13.0392(3) _cell_length_c 19.2770(5) _cell_angle_alpha 87.1780(10) _cell_angle_beta 87.2000(10) _cell_angle_gamma 64.8680(10) _cell_volume 2726.14(12) _cell_formula_units_Z 2 _cell_measurement_temperature 135(2) _cell_measurement_reflns_used 9765 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.40 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 0.436 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8803 _exptl_absorpt_correction_T_max 0.8803 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 135(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50263 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12433 _reflns_number_gt 10298 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The data was solved by Paterson methods. Data processing was conducted to a resolution of 0.77 angstroms as the data was only complete to this resolution. The structure contains two disordered tetrafluoroborate anions. The anion B11 > F15 displays rotational disorder about the B11 F12 bond (49:51). The anion B21 > F25/B31 > F35 is disordered in the first instance over two sites (40:60 respectively). Part B21 > F25 is further disordered with F21 > F25 being disordered over three sites, pivoting at the boron atom (0.188:0.132:0.08) and B31 > F35 displaying rotational disorder along the B31 F32 bond (0.47:0.13). The disordered residue have benefited from the application of geometric and displacement restraints. The disordered residues have been left isotropic due to their fluxional nature. 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^)+(0.1392P)^2^+4.2310P] 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_number_reflns 12433 _refine_ls_number_parameters 775 _refine_ls_number_restraints 192 _refine_ls_R_factor_all 0.0820 _refine_ls_R_factor_gt 0.0693 _refine_ls_wR_factor_ref 0.2208 _refine_ls_wR_factor_gt 0.2056 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _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 Ni1 Ni 0.78518(3) 0.80028(3) 0.684832(19) 0.02059(13) Uani 1 1 d . . . N111 N 0.9050(2) 0.6515(2) 0.73655(14) 0.0240(5) Uani 1 1 d . . . C112 C 0.9207(3) 0.6616(3) 0.80436(16) 0.0252(6) Uani 1 1 d . . . C113 C 1.0029(3) 0.5728(3) 0.84445(18) 0.0324(7) Uani 1 1 d . . . H113 H 1.0144 0.5829 0.8916 0.039 Uiso 1 1 calc R . . C114 C 1.0677(3) 0.4690(3) 0.8140(2) 0.0372(8) Uani 1 1 d . . . H114 H 1.1250 0.4068 0.8401 0.045 Uiso 1 1 calc R . . C115 C 1.0485(3) 0.4568(3) 0.7458(2) 0.0338(7) Uani 1 1 d . . . H115 H 1.0901 0.3855 0.7246 0.041 Uiso 1 1 calc R . . C116 C 0.9675(3) 0.5501(3) 0.70838(18) 0.0284(6) Uani 1 1 d . . . H116 H 0.9558 0.5418 0.6609 0.034 Uiso 1 1 calc R . . N121 N 0.6988(3) 0.9405(2) 0.83000(14) 0.0272(5) Uani 1 1 d . . . N122 N 0.7603(2) 0.8496(2) 0.79021(13) 0.0238(5) Uani 1 1 d . . . C123 C 0.8424(3) 0.7724(3) 0.83238(16) 0.0255(6) Uani 1 1 d . . . C124 C 0.8351(3) 0.8139(3) 0.89868(17) 0.0321(7) Uani 1 1 d . . . H124 H 0.8833 0.7758 0.9375 0.039 Uiso 1 1 calc R . . C125 C 0.7430(3) 0.9215(3) 0.89538(17) 0.0328(7) Uani 1 1 d . . . H125 H 0.7150 0.9735 0.9320 0.039 Uiso 1 1 calc R . . C126 C 0.6059(3) 1.0451(3) 0.80147(17) 0.0279(6) Uani 1 1 d . . . H12A H 0.5439 1.0834 0.8385 0.033 Uiso 1 1 calc R . . H12B H 0.5634 1.0270 0.7644 0.033 Uiso 1 1 calc R . . C131 C 0.6587(3) 1.1254(3) 0.77168(16) 0.0259(6) Uani 1 1 d . . . C132 C 0.7761(3) 1.1088(3) 0.78496(19) 0.0326(7) Uani 1 1 d . . . H132 H 0.8243 1.0476 0.8150 0.039 Uiso 1 1 calc R . . C133 C 0.8269(3) 1.1805(3) 0.7551(2) 0.0360(8) Uani 1 1 d . . . H133 H 0.9085 1.1677 0.7651 0.043 Uiso 1 1 calc R . . C134 C 0.7586(3) 1.2682(3) 0.71175(18) 0.0313(7) Uani 1 1 d . . . C135 C 0.6342(3) 1.2913(3) 0.69709(17) 0.0292(7) Uani 1 1 d . . . C136 C 0.5829(3) 1.2193(3) 0.72881(16) 0.0271(6) Uani 1 1 d . . . C141 C 0.5620(4) 1.3822(3) 0.65276(19) 0.0377(8) Uani 1 1 d . . . H141 H 0.5965 1.4293 0.6308 0.045 Uiso 1 1 calc R . . C142 C 0.4431(4) 1.4029(3) 0.6412(2) 0.0436(9) Uani 1 1 d . . . H142 H 0.3954 1.4640 0.6109 0.052 Uiso 1 1 calc R . . C143 C 0.3903(4) 1.3342(3) 0.6739(2) 0.0421(9) Uani 1 1 d . . . H143 H 0.3067 1.3505 0.6665 0.051 Uiso 1 1 calc R . . C144 C 0.4587(3) 1.2444(3) 0.71626(19) 0.0331(7) Uani 1 1 d . . . H144 H 0.4224 1.1982 0.7376 0.040 Uiso 1 1 calc R . . C151 C 0.8115(4) 1.3411(3) 0.6802(2) 0.0379(8) Uani 1 1 d . . . N152 N 0.8511(4) 1.4006(3) 0.65669(19) 0.0515(9) Uani 1 1 d . . . N211 N 0.6733(2) 0.9534(2) 0.63412(13) 0.0246(5) Uani 1 1 d . . . C212 C 0.7353(3) 1.0115(3) 0.60571(16) 0.0263(6) Uani 1 1 d . . . C213 C 0.6809(4) 1.1040(3) 0.56024(18) 0.0342(7) Uani 1 1 d . . . H213 H 0.7263 1.1433 0.5406 0.041 Uiso 1 1 calc R . . C214 C 0.5590(4) 1.1374(3) 0.5442(2) 0.0411(9) Uani 1 1 d . . . H214 H 0.5199 1.2000 0.5130 0.049 Uiso 1 1 calc R . . C215 C 0.4946(4) 1.0798(3) 0.5735(2) 0.0390(8) Uani 1 1 d . . . H215 H 0.4106 1.1023 0.5634 0.047 Uiso 1 1 calc R . . C216 C 0.5551(3) 0.9879(3) 0.61807(18) 0.0305(7) Uani 1 1 d . . . H216 H 0.5109 0.9477 0.6381 0.037 Uiso 1 1 calc R . . N221 N 1.0337(3) 0.8487(2) 0.66742(14) 0.0284(6) Uani 1 1 d . . . N222 N 0.9124(2) 0.8726(2) 0.66379(13) 0.0239(5) Uani 1 1 d . . . C223 C 0.8644(3) 0.9675(3) 0.62374(16) 0.0259(6) Uani 1 1 d . . . C224 C 0.9547(4) 1.0053(3) 0.60236(19) 0.0347(7) Uani 1 1 d . . . H224 H 0.9446 1.0701 0.5740 0.042 Uiso 1 1 calc R . . C225 C 1.0599(4) 0.9282(3) 0.63139(19) 0.0369(8) Uani 1 1 d . . . H225 H 1.1384 0.9298 0.6271 0.044 Uiso 1 1 calc R . . C226 C 1.1199(3) 0.7515(3) 0.70571(17) 0.0280(6) Uani 1 1 d . . . H22A H 1.1997 0.7209 0.6794 0.034 Uiso 1 1 calc R . . H22B H 1.0890 0.6921 0.7087 0.034 Uiso 1 1 calc R . . C231 C 1.1416(3) 0.7762(3) 0.77855(17) 0.0278(6) Uani 1 1 d . . . C232 C 1.0751(4) 0.8803(3) 0.8058(2) 0.0395(8) Uani 1 1 d . . . H232 H 1.0153 0.9383 0.7784 0.047 Uiso 1 1 calc R . . C233 C 1.0936(5) 0.9030(4) 0.8736(2) 0.0480(10) Uani 1 1 d . . . H233 H 1.0449 0.9754 0.8920 0.058 Uiso 1 1 calc R . . C234 C 1.1812(4) 0.8216(4) 0.9134(2) 0.0427(9) Uani 1 1 d . . . C235 C 1.2570(4) 0.7128(3) 0.88622(18) 0.0340(7) Uani 1 1 d . . . C236 C 1.2348(3) 0.6891(3) 0.81813(16) 0.0280(6) Uani 1 1 d . . . C241 C 1.3531(4) 0.6291(4) 0.92450(19) 0.0432(9) Uani 1 1 d . . . H241 H 1.3689 0.6447 0.9697 0.052 Uiso 1 1 calc R . . C242 C 1.4232(4) 0.5260(4) 0.8969(2) 0.0462(9) Uani 1 1 d . . . H242 H 1.4883 0.4709 0.9229 0.055 Uiso 1 1 calc R . . C243 C 1.4002(4) 0.5006(3) 0.8305(2) 0.0424(9) Uani 1 1 d . . . H243 H 1.4485 0.4280 0.8123 0.051 Uiso 1 1 calc R . . C244 C 1.3079(3) 0.5807(3) 0.79209(18) 0.0323(7) Uani 1 1 d . . . H244 H 1.2930 0.5628 0.7473 0.039 Uiso 1 1 calc R . . C251 C 1.1979(5) 0.8463(4) 0.9825(2) 0.0578(12) Uani 1 1 d . . . N252 N 1.2108(6) 0.8660(5) 1.0385(2) 0.0846(17) Uani 1 1 d . . . N311 N 0.8248(2) 0.7269(2) 0.58654(13) 0.0233(5) Uani 1 1 d . . . C312 C 0.7494(3) 0.6800(3) 0.56848(17) 0.0259(6) Uani 1 1 d . . . C313 C 0.7653(3) 0.6246(3) 0.50692(19) 0.0360(8) Uani 1 1 d . . . H313 H 0.7111 0.5923 0.4957 0.043 Uiso 1 1 calc R . . C314 C 0.8606(4) 0.6173(4) 0.4625(2) 0.0463(10) Uani 1 1 d . . . H314 H 0.8740 0.5789 0.4202 0.056 Uiso 1 1 calc R . . C315 C 0.9376(4) 0.6663(4) 0.4796(2) 0.0448(10) Uani 1 1 d . . . H315 H 1.0035 0.6629 0.4490 0.054 Uiso 1 1 calc R . . C316 C 0.9166(3) 0.7199(3) 0.54201(18) 0.0315(7) Uani 1 1 d . . . H316 H 0.9695 0.7533 0.5538 0.038 Uiso 1 1 calc R . . N321 N 0.5455(2) 0.7442(2) 0.71421(15) 0.0286(6) Uani 1 1 d . . . N322 N 0.6485(2) 0.7393(2) 0.67980(14) 0.0248(5) Uani 1 1 d . . . C323 C 0.6506(3) 0.6919(3) 0.61915(17) 0.0255(6) Uani 1 1 d . . . C324 C 0.5498(3) 0.6657(3) 0.61513(19) 0.0323(7) Uani 1 1 d . . . H324 H 0.5303 0.6317 0.5779 0.039 Uiso 1 1 calc R . . C325 C 0.4854(3) 0.6997(3) 0.6765(2) 0.0356(8) Uani 1 1 d . . . H325 H 0.4114 0.6933 0.6903 0.043 Uiso 1 1 calc R . . C326 C 0.5243(3) 0.7725(3) 0.78720(18) 0.0326(7) Uani 1 1 d . . . H32A H 0.4373 0.7911 0.8006 0.039 Uiso 1 1 calc R . . H32B H 0.5389 0.8406 0.7939 0.039 Uiso 1 1 calc R . . C331 C 0.6069(3) 0.6771(3) 0.83375(17) 0.0291(7) Uani 1 1 d . . . C332 C 0.6784(3) 0.5716(3) 0.80816(18) 0.0304(7) Uani 1 1 d . . . H332 H 0.6724 0.5574 0.7609 0.036 Uiso 1 1 calc R . . C333 C 0.7600(3) 0.4849(3) 0.85100(18) 0.0328(7) Uani 1 1 d . . . H333 H 0.8078 0.4121 0.8329 0.039 Uiso 1 1 calc R . . C334 C 0.7710(3) 0.5046(3) 0.91885(18) 0.0341(7) Uani 1 1 d . . . C335 C 0.6970(4) 0.6116(3) 0.94824(18) 0.0357(7) Uani 1 1 d . . . C336 C 0.6125(3) 0.6984(3) 0.90518(18) 0.0324(7) Uani 1 1 d . . . C341 C 0.7063(4) 0.6333(4) 1.0183(2) 0.0484(10) Uani 1 1 d . . . H341 H 0.7635 0.5757 1.0471 0.058 Uiso 1 1 calc R . . C342 C 0.6333(5) 0.7370(5) 1.0449(2) 0.0612(13) Uani 1 1 d . . . H342 H 0.6399 0.7514 1.0920 0.073 Uiso 1 1 calc R . . C343 C 0.5496(5) 0.8210(4) 1.0028(2) 0.0559(12) Uani 1 1 d . . . H343 H 0.4993 0.8924 1.0220 0.067 Uiso 1 1 calc R . . C344 C 0.5372(4) 0.8045(3) 0.9349(2) 0.0434(9) Uani 1 1 d . . . H344 H 0.4786 0.8636 0.9075 0.052 Uiso 1 1 calc R . . C351 C 0.8635(4) 0.4178(4) 0.9601(2) 0.0428(9) Uani 1 1 d . . . N352 N 0.9393(4) 0.3506(4) 0.9923(2) 0.0607(11) Uani 1 1 d . . . B11 B 0.24788(16) 0.65732(14) 0.53078(9) 0.0321(7) Uiso 1 1 d DU . . F12 F 0.18779(15) 0.60879(14) 0.57500(8) 0.0329(4) Uiso 1 1 d DU A . F13X F 0.3502(6) 0.5725(2) 0.4998(4) 0.0416(11) Uiso 0.55(3) 1 d PDU A 1 F14X F 0.1696(4) 0.7248(6) 0.4802(3) 0.0354(10) Uiso 0.55(3) 1 d PDU A 1 F15X F 0.2867(8) 0.7235(7) 0.56918(14) 0.0354(10) Uiso 0.55(3) 1 d PDU A 1 F13Y F 0.3291(8) 0.5757(3) 0.4875(4) 0.0426(12) Uiso 0.45(3) 1 d PDU A 2 F14Y F 0.1613(3) 0.7434(6) 0.4913(4) 0.0318(11) Uiso 0.45(3) 1 d PDU A 2 F15Y F 0.3105(8) 0.7008(9) 0.56913(16) 0.0376(12) Uiso 0.45(3) 1 d PDU A 2 B21 B 0.2442(6) 0.1020(5) 0.8297(3) 0.0575(12) Uiso 0.40 1 d PDU . . F22X F 0.2466(14) 0.2066(7) 0.8198(8) 0.0562(19) Uiso 0.19 1 d PDU B 1 F23X F 0.1271(8) 0.1134(13) 0.8177(8) 0.0631(16) Uiso 0.19 1 d PDU B 1 F24X F 0.3312(10) 0.0334(10) 0.7825(6) 0.0573(16) Uiso 0.19 1 d PDU B 1 F25X F 0.2890(12) 0.0566(10) 0.8941(4) 0.0491(17) Uiso 0.19 1 d PDU B 1 F22Y F 0.2662(18) 0.1954(11) 0.8108(10) 0.056(2) Uiso 0.13 1 d PDU B 2 F23Y F 0.1484(12) 0.1051(16) 0.7914(9) 0.0608(17) Uiso 0.13 1 d PDU B 2 F24Y F 0.3481(11) 0.0050(9) 0.8147(9) 0.0571(15) Uiso 0.13 1 d PDU B 2 F25Y F 0.2174(16) 0.1059(15) 0.9004(4) 0.0500(18) Uiso 0.13 1 d PDU B 2 F22Z F 0.251(2) 0.1869(16) 0.7866(11) 0.0582(19) Uiso 0.08 1 d PDU B 3 F23Z F 0.256(2) 0.0104(14) 0.7920(12) 0.0608(14) Uiso 0.08 1 d PDU B 3 F24Z F 0.3357(17) 0.0638(19) 0.8778(10) 0.0461(19) Uiso 0.08 1 d PDU B 3 F25Z F 0.1308(12) 0.144(2) 0.8641(12) 0.0601(19) Uiso 0.08 1 d PDU B 3 B31 B 0.2440(3) 0.0799(3) 0.70792(16) 0.0584(12) Uiso 0.60 1 d PDU . . F32 F 0.1429(3) 0.0787(4) 0.7448(2) 0.0696(11) Uiso 0.60 1 d PDU C . F33X F 0.2209(4) 0.1897(3) 0.6870(2) 0.0674(14) Uiso 0.47 1 d PDU C 1 F34X F 0.2686(4) 0.0137(4) 0.65020(19) 0.0517(12) Uiso 0.47 1 d PDU C 1 F35X F 0.3456(3) 0.0364(4) 0.7499(2) 0.0547(11) Uiso 0.47 1 d PDU C 1 F33Y F 0.2427(9) 0.1861(5) 0.7113(6) 0.061(2) Uiso 0.13 1 d PDU C 2 F34Y F 0.2390(8) 0.0564(12) 0.6394(2) 0.050(2) Uiso 0.13 1 d PDU C 2 F35Y F 0.3503(3) -0.0001(9) 0.7363(5) 0.0573(16) Uiso 0.13 1 d PDU C 2 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 Ni1 0.0203(2) 0.0198(2) 0.0230(2) 0.00223(14) -0.00295(14) -0.00985(15) N111 0.0217(12) 0.0219(12) 0.0295(13) 0.0013(10) -0.0025(10) -0.0104(10) C112 0.0252(15) 0.0230(14) 0.0292(15) 0.0030(11) -0.0030(12) -0.0121(12) C113 0.0360(18) 0.0287(16) 0.0325(17) 0.0057(13) -0.0094(14) -0.0135(14) C114 0.0355(18) 0.0260(16) 0.045(2) 0.0075(14) -0.0130(15) -0.0082(14) C115 0.0286(16) 0.0243(15) 0.0449(19) -0.0013(14) -0.0028(14) -0.0075(13) C116 0.0279(16) 0.0259(15) 0.0329(16) -0.0013(12) -0.0020(13) -0.0128(13) N121 0.0317(14) 0.0215(12) 0.0268(13) -0.0003(10) 0.0007(11) -0.0101(11) N122 0.0265(13) 0.0200(12) 0.0247(12) 0.0010(9) -0.0018(10) -0.0096(10) C123 0.0272(15) 0.0234(14) 0.0272(15) 0.0043(11) -0.0030(12) -0.0123(12) C124 0.0403(19) 0.0318(17) 0.0245(15) 0.0035(12) -0.0053(13) -0.0156(15) C125 0.0430(19) 0.0297(16) 0.0252(15) -0.0025(12) -0.0020(14) -0.0147(15) C126 0.0268(15) 0.0231(14) 0.0309(16) -0.0002(12) 0.0017(12) -0.0083(12) C131 0.0274(15) 0.0214(14) 0.0270(15) -0.0018(11) -0.0001(12) -0.0085(12) C132 0.0292(16) 0.0268(16) 0.0404(18) 0.0017(13) -0.0054(14) -0.0105(13) C133 0.0297(17) 0.0348(18) 0.045(2) -0.0043(15) -0.0002(15) -0.0149(15) C134 0.0346(17) 0.0261(15) 0.0362(17) -0.0063(13) 0.0066(14) -0.0161(14) C135 0.0360(17) 0.0236(15) 0.0281(15) -0.0052(12) 0.0028(13) -0.0125(13) C136 0.0300(16) 0.0217(14) 0.0274(15) -0.0024(11) -0.0004(12) -0.0087(12) C141 0.052(2) 0.0246(16) 0.0357(18) 0.0016(13) -0.0022(16) -0.0158(16) C142 0.051(2) 0.0288(18) 0.044(2) 0.0064(15) -0.0138(18) -0.0102(16) C143 0.0342(19) 0.0346(19) 0.051(2) 0.0011(16) -0.0124(16) -0.0077(15) C144 0.0305(17) 0.0264(16) 0.0419(19) -0.0003(13) -0.0027(14) -0.0114(13) C151 0.047(2) 0.0375(19) 0.0375(18) -0.0111(15) 0.0092(16) -0.0259(17) N152 0.074(3) 0.056(2) 0.0443(19) -0.0090(16) 0.0104(18) -0.047(2) N211 0.0267(13) 0.0229(12) 0.0251(12) 0.0001(10) -0.0030(10) -0.0113(10) C212 0.0325(16) 0.0226(14) 0.0239(14) 0.0011(11) -0.0028(12) -0.0117(12) C213 0.044(2) 0.0264(16) 0.0320(17) 0.0071(13) -0.0051(14) -0.0155(15) C214 0.045(2) 0.0295(17) 0.040(2) 0.0116(15) -0.0127(16) -0.0071(16) C215 0.0341(18) 0.0314(18) 0.044(2) 0.0062(15) -0.0131(15) -0.0058(15) C216 0.0283(16) 0.0247(15) 0.0352(17) 0.0016(13) -0.0061(13) -0.0079(13) N221 0.0283(14) 0.0351(14) 0.0286(13) 0.0011(11) -0.0034(11) -0.0198(12) N222 0.0254(13) 0.0264(12) 0.0240(12) -0.0002(10) -0.0022(10) -0.0149(11) C223 0.0331(16) 0.0244(14) 0.0246(14) 0.0012(11) -0.0029(12) -0.0163(13) C224 0.043(2) 0.0351(18) 0.0353(18) 0.0044(14) -0.0006(15) -0.0260(16) C225 0.0377(19) 0.044(2) 0.0401(19) 0.0046(15) -0.0022(15) -0.0284(17) C226 0.0251(15) 0.0333(16) 0.0299(16) -0.0025(12) -0.0030(12) -0.0162(13) C231 0.0283(16) 0.0325(16) 0.0288(15) -0.0021(12) 0.0000(12) -0.0190(13) C232 0.045(2) 0.0332(18) 0.0378(19) -0.0034(14) -0.0038(16) -0.0131(16) C233 0.067(3) 0.036(2) 0.041(2) -0.0114(16) 0.0001(19) -0.020(2) C234 0.062(3) 0.046(2) 0.0308(18) -0.0083(15) -0.0001(17) -0.032(2) C235 0.043(2) 0.0399(19) 0.0284(16) 0.0016(14) -0.0012(14) -0.0267(16) C236 0.0298(16) 0.0331(16) 0.0281(15) 0.0008(12) -0.0007(12) -0.0203(14) C241 0.055(2) 0.056(2) 0.0288(17) 0.0090(16) -0.0118(16) -0.033(2) C242 0.042(2) 0.052(2) 0.041(2) 0.0142(18) -0.0110(17) -0.0177(19) C243 0.038(2) 0.038(2) 0.044(2) 0.0025(16) 0.0011(16) -0.0106(16) C244 0.0332(17) 0.0341(17) 0.0316(17) 0.0010(13) -0.0001(13) -0.0165(14) C251 0.091(4) 0.055(3) 0.040(2) -0.0088(19) -0.004(2) -0.041(3) N252 0.147(5) 0.084(3) 0.041(2) -0.013(2) -0.015(3) -0.063(4) N311 0.0203(12) 0.0242(12) 0.0253(12) 0.0014(9) -0.0047(9) -0.0091(10) C312 0.0229(14) 0.0211(14) 0.0322(16) 0.0020(11) -0.0096(12) -0.0073(12) C313 0.0310(17) 0.0357(18) 0.0401(19) -0.0081(15) -0.0102(14) -0.0113(14) C314 0.037(2) 0.063(3) 0.039(2) -0.0219(18) -0.0023(16) -0.0176(19) C315 0.0306(18) 0.071(3) 0.0335(19) -0.0177(18) 0.0044(15) -0.0206(19) C316 0.0246(15) 0.0384(18) 0.0321(17) -0.0074(13) -0.0013(13) -0.0131(14) N321 0.0214(12) 0.0301(14) 0.0351(14) 0.0099(11) -0.0032(11) -0.0127(11) N322 0.0197(12) 0.0233(12) 0.0314(13) 0.0052(10) -0.0018(10) -0.0096(10) C323 0.0241(14) 0.0217(14) 0.0318(15) 0.0084(11) -0.0102(12) -0.0108(12) C324 0.0331(17) 0.0316(16) 0.0391(18) 0.0120(13) -0.0152(14) -0.0201(14) C325 0.0284(17) 0.0403(19) 0.045(2) 0.0169(15) -0.0127(14) -0.0216(15) C326 0.0268(16) 0.0310(16) 0.0383(18) 0.0041(14) 0.0039(13) -0.0115(13) C331 0.0261(15) 0.0299(16) 0.0328(16) 0.0036(13) 0.0029(12) -0.0142(13) C332 0.0335(17) 0.0291(16) 0.0284(16) 0.0026(12) -0.0029(13) -0.0134(14) C333 0.0365(18) 0.0282(16) 0.0310(17) 0.0029(13) -0.0014(14) -0.0116(14) C334 0.0349(18) 0.0353(18) 0.0305(17) 0.0095(14) -0.0044(14) -0.0142(15) C335 0.0403(19) 0.0419(19) 0.0284(16) -0.0005(14) 0.0040(14) -0.0213(16) C336 0.0314(17) 0.0342(17) 0.0349(17) -0.0008(13) 0.0079(14) -0.0180(14) C341 0.054(3) 0.059(3) 0.0314(19) -0.0024(17) -0.0022(17) -0.023(2) C342 0.077(3) 0.069(3) 0.035(2) -0.015(2) 0.009(2) -0.028(3) C343 0.061(3) 0.052(3) 0.051(3) -0.019(2) 0.021(2) -0.021(2) C344 0.043(2) 0.038(2) 0.046(2) -0.0062(16) 0.0135(17) -0.0155(17) C351 0.048(2) 0.047(2) 0.0316(18) 0.0038(16) -0.0071(16) -0.0179(19) N352 0.063(3) 0.060(2) 0.048(2) 0.0129(18) -0.0200(19) -0.015(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 Ni1 N211 2.099(3) . ? Ni1 N111 2.099(3) . ? Ni1 N311 2.106(3) . ? Ni1 N322 2.113(3) . ? Ni1 N222 2.123(2) . ? Ni1 N122 2.129(3) . ? N111 C116 1.339(4) . ? N111 C112 1.350(4) . ? C112 C113 1.388(4) . ? C112 C123 1.462(4) . ? C113 C114 1.386(5) . ? C113 H113 0.9500 . ? C114 C115 1.375(5) . ? C114 H114 0.9500 . ? C115 C116 1.387(5) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? N121 N122 1.352(4) . ? N121 C125 1.361(4) . ? N121 C126 1.449(4) . ? N122 C123 1.341(4) . ? C123 C124 1.396(5) . ? C124 C125 1.369(5) . ? C124 H124 0.9500 . ? C125 H125 0.9500 . ? C126 C131 1.515(4) . ? C126 H12A 0.9900 . ? C126 H12B 0.9900 . ? C131 C132 1.367(5) . ? C131 C136 1.427(4) . ? C132 C133 1.404(5) . ? C132 H132 0.9500 . ? C133 C134 1.362(5) . ? C133 H133 0.9500 . ? C134 C135 1.432(5) . ? C134 C151 1.446(5) . ? C135 C141 1.409(5) . ? C135 C136 1.425(4) . ? C136 C144 1.415(5) . ? C141 C142 1.363(6) . ? C141 H141 0.9500 . ? C142 C143 1.410(6) . ? C142 H142 0.9500 . ? C143 C144 1.366(5) . ? C143 H143 0.9500 . ? C144 H144 0.9500 . ? C151 N152 1.137(5) . ? N211 C216 1.340(4) . ? N211 C212 1.351(4) . ? C212 C213 1.390(4) . ? C212 C223 1.459(5) . ? C213 C214 1.384(5) . ? C213 H213 0.9500 . ? C214 C215 1.374(6) . ? C214 H214 0.9500 . ? C215 C216 1.386(5) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? N221 C225 1.356(4) . ? N221 N222 1.358(4) . ? N221 C226 1.446(4) . ? N222 C223 1.342(4) . ? C223 C224 1.406(4) . ? C224 C225 1.361(5) . ? C224 H224 0.9500 . ? C225 H225 0.9500 . ? C226 C231 1.514(4) . ? C226 H22A 0.9900 . ? C226 H22B 0.9900 . ? C231 C232 1.366(5) . ? C231 C236 1.428(5) . ? C232 C233 1.403(5) . ? C232 H232 0.9500 . ? C233 C234 1.368(6) . ? C233 H233 0.9500 . ? C234 C251 1.429(5) . ? C234 C235 1.431(6) . ? C235 C241 1.414(5) . ? C235 C236 1.426(5) . ? C236 C244 1.412(5) . ? C241 C242 1.365(6) . ? C241 H241 0.9500 . ? C242 C243 1.406(6) . ? C242 H242 0.9500 . ? C243 C244 1.375(5) . ? C243 H243 0.9500 . ? C244 H244 0.9500 . ? C251 N252 1.153(6) . ? N311 C316 1.338(4) . ? N311 C312 1.354(4) . ? C312 C313 1.383(5) . ? C312 C323 1.459(5) . ? C313 C314 1.367(6) . ? C313 H313 0.9500 . ? C314 C315 1.387(6) . ? C314 H314 0.9500 . ? C315 C316 1.379(5) . ? C315 H315 0.9500 . ? C316 H316 0.9500 . ? N321 N322 1.353(4) . ? N321 C325 1.354(5) . ? N321 C326 1.455(5) . ? N322 C323 1.343(4) . ? C323 C324 1.396(4) . ? C324 C325 1.366(6) . ? C324 H324 0.9500 . ? C325 H325 0.9500 . ? C326 C331 1.505(5) . ? C326 H32A 0.9900 . ? C326 H32B 0.9900 . ? C331 C332 1.376(5) . ? C331 C336 1.428(5) . ? C332 C333 1.402(5) . ? C332 H332 0.9500 . ? C333 C334 1.369(5) . ? C333 H333 0.9500 . ? C334 C335 1.426(5) . ? C334 C351 1.441(5) . ? C335 C341 1.413(5) . ? C335 C336 1.419(5) . ? C336 C344 1.423(5) . ? C341 C342 1.370(7) . ? C341 H341 0.9500 . ? C342 C343 1.386(7) . ? C342 H342 0.9500 . ? C343 C344 1.363(6) . ? C343 H343 0.9500 . ? C344 H344 0.9500 . ? C351 N352 1.142(5) . ? B11 F15Y 1.3747(19) . ? B11 F13Y 1.3811(19) . ? B11 F14X 1.3817(19) . ? B11 F14Y 1.3858(19) . ? B11 F12 1.3862(14) . ? B11 F13X 1.3883(19) . ? B11 F15X 1.3957(19) . ? B21 F23X 1.379(2) . ? B21 F24Y 1.379(2) . ? B21 F22Z 1.379(2) . ? B21 F25X 1.379(2) . ? B21 F24Z 1.380(2) . ? B21 F23Z 1.380(2) . ? B21 F22Y 1.381(2) . ? B21 F22X 1.381(2) . ? B21 F25Z 1.381(2) . ? B21 F23Y 1.382(2) . ? B21 F24X 1.383(2) . ? B21 F25Y 1.383(2) . ? B31 F35Y 1.377(2) . ? B31 F34Y 1.380(2) . ? B31 F33X 1.381(2) . ? B31 F32 1.3814(15) . ? B31 F33Y 1.383(2) . ? B31 F34X 1.385(2) . ? B31 F35X 1.388(2) . ? 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 N211 Ni1 N111 176.41(10) . . ? N211 Ni1 N311 87.23(10) . . ? N111 Ni1 N311 93.90(10) . . ? N211 Ni1 N322 91.49(10) . . ? N111 Ni1 N322 92.08(10) . . ? N311 Ni1 N322 78.34(10) . . ? N211 Ni1 N222 78.94(10) . . ? N111 Ni1 N222 97.62(10) . . ? N311 Ni1 N222 90.74(10) . . ? N322 Ni1 N222 165.88(10) . . ? N211 Ni1 N122 101.25(10) . . ? N111 Ni1 N122 77.69(10) . . ? N311 Ni1 N122 171.48(10) . . ? N322 Ni1 N122 100.38(10) . . ? N222 Ni1 N122 91.73(10) . . ? C116 N111 C112 118.1(3) . . ? C116 N111 Ni1 126.2(2) . . ? C112 N111 Ni1 115.6(2) . . ? N111 C112 C113 122.5(3) . . ? N111 C112 C123 114.7(3) . . ? C113 C112 C123 122.8(3) . . ? C114 C113 C112 118.4(3) . . ? C114 C113 H113 120.8 . . ? C112 C113 H113 120.8 . . ? C115 C114 C113 119.4(3) . . ? C115 C114 H114 120.3 . . ? C113 C114 H114 120.3 . . ? C114 C115 C116 118.9(3) . . ? C114 C115 H115 120.5 . . ? C116 C115 H115 120.5 . . ? N111 C116 C115 122.5(3) . . ? N111 C116 H116 118.7 . . ? C115 C116 H116 118.7 . . ? N122 N121 C125 111.2(3) . . ? N122 N121 C126 121.6(3) . . ? C125 N121 C126 127.1(3) . . ? C123 N122 N121 104.9(2) . . ? C123 N122 Ni1 113.1(2) . . ? N121 N122 Ni1 141.3(2) . . ? N122 C123 C124 111.6(3) . . ? N122 C123 C112 117.8(3) . . ? C124 C123 C112 130.6(3) . . ? C125 C124 C123 104.7(3) . . ? C125 C124 H124 127.6 . . ? C123 C124 H124 127.6 . . ? N121 C125 C124 107.6(3) . . ? N121 C125 H125 126.2 . . ? C124 C125 H125 126.2 . . ? N121 C126 C131 113.0(3) . . ? N121 C126 H12A 109.0 . . ? C131 C126 H12A 109.0 . . ? N121 C126 H12B 109.0 . . ? C131 C126 H12B 109.0 . . ? H12A C126 H12B 107.8 . . ? C132 C131 C136 120.3(3) . . ? C132 C131 C126 121.3(3) . . ? C136 C131 C126 118.4(3) . . ? C131 C132 C133 121.3(3) . . ? C131 C132 H132 119.3 . . ? C133 C132 H132 119.3 . . ? C134 C133 C132 119.8(3) . . ? C134 C133 H133 120.1 . . ? C132 C133 H133 120.1 . . ? C133 C134 C135 121.4(3) . . ? C133 C134 C151 119.8(3) . . ? C135 C134 C151 118.8(3) . . ? C141 C135 C136 119.6(3) . . ? C141 C135 C134 122.1(3) . . ? C136 C135 C134 118.3(3) . . ? C144 C136 C135 118.3(3) . . ? C144 C136 C131 122.9(3) . . ? C135 C136 C131 118.8(3) . . ? C142 C141 C135 120.5(3) . . ? C142 C141 H141 119.8 . . ? C135 C141 H141 119.8 . . ? C141 C142 C143 120.4(3) . . ? C141 C142 H142 119.8 . . ? C143 C142 H142 119.8 . . ? C144 C143 C142 120.4(4) . . ? C144 C143 H143 119.8 . . ? C142 C143 H143 119.8 . . ? C143 C144 C136 120.9(3) . . ? C143 C144 H144 119.6 . . ? C136 C144 H144 119.6 . . ? N152 C151 C134 178.2(4) . . ? C216 N211 C212 118.2(3) . . ? C216 N211 Ni1 126.7(2) . . ? C212 N211 Ni1 114.1(2) . . ? N211 C212 C213 122.2(3) . . ? N211 C212 C223 115.4(3) . . ? C213 C212 C223 122.4(3) . . ? C214 C213 C212 118.4(3) . . ? C214 C213 H213 120.8 . . ? C212 C213 H213 120.8 . . ? C215 C214 C213 119.9(3) . . ? C215 C214 H214 120.1 . . ? C213 C214 H214 120.1 . . ? C214 C215 C216 118.4(3) . . ? C214 C215 H215 120.8 . . ? C216 C215 H215 120.8 . . ? N211 C216 C215 122.9(3) . . ? N211 C216 H216 118.6 . . ? C215 C216 H216 118.6 . . ? C225 N221 N222 110.7(3) . . ? C225 N221 C226 126.2(3) . . ? N222 N221 C226 123.1(3) . . ? C223 N222 N221 105.2(2) . . ? C223 N222 Ni1 112.0(2) . . ? N221 N222 Ni1 141.8(2) . . ? N222 C223 C224 111.1(3) . . ? N222 C223 C212 118.7(3) . . ? C224 C223 C212 130.1(3) . . ? C225 C224 C223 104.6(3) . . ? C225 C224 H224 127.7 . . ? C223 C224 H224 127.7 . . ? N221 C225 C224 108.4(3) . . ? N221 C225 H225 125.8 . . ? C224 C225 H225 125.8 . . ? N221 C226 C231 114.4(3) . . ? N221 C226 H22A 108.7 . . ? C231 C226 H22A 108.7 . . ? N221 C226 H22B 108.7 . . ? C231 C226 H22B 108.7 . . ? H22A C226 H22B 107.6 . . ? C232 C231 C236 120.2(3) . . ? C232 C231 C226 120.8(3) . . ? C236 C231 C226 118.9(3) . . ? C231 C232 C233 121.1(4) . . ? C231 C232 H232 119.5 . . ? C233 C232 H232 119.5 . . ? C234 C233 C232 120.5(4) . . ? C234 C233 H233 119.8 . . ? C232 C233 H233 119.8 . . ? C233 C234 C251 119.5(4) . . ? C233 C234 C235 120.6(3) . . ? C251 C234 C235 119.8(4) . . ? C241 C235 C236 119.4(3) . . ? C241 C235 C234 122.1(3) . . ? C236 C235 C234 118.5(3) . . ? C244 C236 C235 118.3(3) . . ? C244 C236 C231 122.7(3) . . ? C235 C236 C231 119.0(3) . . ? C242 C241 C235 120.4(3) . . ? C242 C241 H241 119.8 . . ? C235 C241 H241 119.8 . . ? C241 C242 C243 120.7(4) . . ? C241 C242 H242 119.6 . . ? C243 C242 H242 119.6 . . ? C244 C243 C242 120.0(4) . . ? C244 C243 H243 120.0 . . ? C242 C243 H243 120.0 . . ? C243 C244 C236 121.1(3) . . ? C243 C244 H244 119.5 . . ? C236 C244 H244 119.5 . . ? N252 C251 C234 179.5(6) . . ? C316 N311 C312 117.9(3) . . ? C316 N311 Ni1 127.1(2) . . ? C312 N311 Ni1 115.0(2) . . ? N311 C312 C313 122.6(3) . . ? N311 C312 C323 114.9(3) . . ? C313 C312 C323 122.6(3) . . ? C314 C313 C312 118.6(3) . . ? C314 C313 H313 120.7 . . ? C312 C313 H313 120.7 . . ? C313 C314 C315 119.6(3) . . ? C313 C314 H314 120.2 . . ? C315 C314 H314 120.2 . . ? C316 C315 C314 118.6(4) . . ? C316 C315 H315 120.7 . . ? C314 C315 H315 120.7 . . ? N311 C316 C315 122.7(3) . . ? N311 C316 H316 118.7 . . ? C315 C316 H316 118.7 . . ? N322 N321 C325 111.0(3) . . ? N322 N321 C326 120.3(3) . . ? C325 N321 C326 127.5(3) . . ? C323 N322 N321 105.1(3) . . ? C323 N322 Ni1 113.4(2) . . ? N321 N322 Ni1 140.7(2) . . ? N322 C323 C324 111.1(3) . . ? N322 C323 C312 118.1(3) . . ? C324 C323 C312 130.7(3) . . ? C325 C324 C323 104.9(3) . . ? C325 C324 H324 127.6 . . ? C323 C324 H324 127.6 . . ? N321 C325 C324 107.9(3) . . ? N321 C325 H325 126.1 . . ? C324 C325 H325 126.1 . . ? N321 C326 C331 112.2(3) . . ? N321 C326 H32A 109.2 . . ? C331 C326 H32A 109.2 . . ? N321 C326 H32B 109.2 . . ? C331 C326 H32B 109.2 . . ? H32A C326 H32B 107.9 . . ? C332 C331 C336 120.1(3) . . ? C332 C331 C326 121.1(3) . . ? C336 C331 C326 118.8(3) . . ? C331 C332 C333 120.8(3) . . ? C331 C332 H332 119.6 . . ? C333 C332 H332 119.6 . . ? C334 C333 C332 120.3(3) . . ? C334 C333 H333 119.9 . . ? C332 C333 H333 119.9 . . ? C333 C334 C335 121.1(3) . . ? C333 C334 C351 119.4(3) . . ? C335 C334 C351 119.4(3) . . ? C341 C335 C336 119.6(4) . . ? C341 C335 C334 121.9(4) . . ? C336 C335 C334 118.4(3) . . ? C335 C336 C344 118.4(3) . . ? C335 C336 C331 119.3(3) . . ? C344 C336 C331 122.4(3) . . ? C342 C341 C335 120.3(4) . . ? C342 C341 H341 119.8 . . ? C335 C341 H341 119.8 . . ? C341 C342 C343 119.8(4) . . ? C341 C342 H342 120.1 . . ? C343 C342 H342 120.1 . . ? C344 C343 C342 122.2(4) . . ? C344 C343 H343 118.9 . . ? C342 C343 H343 118.9 . . ? C343 C344 C336 119.7(4) . . ? C343 C344 H344 120.2 . . ? C336 C344 H344 120.2 . . ? N352 C351 C334 177.8(5) . . ? F15Y B11 F13Y 110.05(14) . . ? F15Y B11 F14X 119.6(2) . . ? F13Y B11 F14X 97.3(3) . . ? F15Y B11 F14Y 109.77(14) . . ? F13Y B11 F14Y 109.48(14) . . ? F14X B11 F14Y 12.9(3) . . ? F15Y B11 F12 109.63(14) . . ? F13Y B11 F12 109.09(14) . . ? F14X B11 F12 110.27(14) . . ? F14Y B11 F12 108.81(14) . . ? F15Y B11 F13X 97.1(3) . . ? F13Y B11 F13X 14.3(3) . . ? F14X B11 F13X 109.78(14) . . ? F14Y B11 F13X 121.2(2) . . ? F12 B11 F13X 109.48(13) . . ? F15Y B11 F15X 12.9(3) . . ? F13Y B11 F15X 121.0(2) . . ? F14X B11 F15X 109.27(14) . . ? F14Y B11 F15X 98.4(3) . . ? F12 B11 F15X 109.14(13) . . ? F13X B11 F15X 108.88(14) . . ? F23X B21 F24Y 122.5(11) . . ? F23X B21 F22Z 101.5(12) . . ? F24Y B21 F22Z 106.2(14) . . ? F23X B21 F25X 115.5(7) . . ? F24Y B21 F25X 76.1(8) . . ? F22Z B21 F25X 134.6(12) . . ? F23X B21 F24Z 143.5(11) . . ? F24Y B21 F24Z 62.8(12) . . ? F22Z B21 F24Z 111.7(9) . . ? F25X B21 F24Z 28.0(10) . . ? F23X B21 F23Z 72.7(12) . . ? F24Y B21 F23Z 50.6(13) . . ? F22Z B21 F23Z 110.9(9) . . ? F25X B21 F23Z 104.8(12) . . ? F24Z B21 F23Z 107.6(9) . . ? F23X B21 F22Y 115.2(12) . . ? F24Y B21 F22Y 109.1(8) . . ? F22Z B21 F22Y 22.6(13) . . ? F25X B21 F22Y 112.5(11) . . ? F24Z B21 F22Y 92.6(13) . . ? F23Z B21 F22Y 130.8(14) . . ? F23X B21 F22X 108.7(7) . . ? F24Y B21 F22X 119.8(11) . . ? F22Z B21 F22X 29.1(12) . . ? F25X B21 F22X 109.7(8) . . ? F24Z B21 F22X 94.1(12) . . ? F23Z B21 F22X 139.9(12) . . ? F22Y B21 F22X 11.5(12) . . ? F23X B21 F25Z 42.8(11) . . ? F24Y B21 F25Z 144.4(13) . . ? F22Z B21 F25Z 108.7(9) . . ? F25X B21 F25Z 84.4(11) . . ? F24Z B21 F25Z 109.2(9) . . ? F23Z B21 F25Z 108.7(9) . . ? F22Y B21 F25Z 105.8(14) . . ? F22X B21 F25Z 94.6(12) . . ? F23X B21 F23Y 23.1(9) . . ? F24Y B21 F23Y 108.8(8) . . ? F22Z B21 F23Y 89.2(13) . . ? F25X B21 F23Y 134.0(10) . . ? F24Z B21 F23Y 158.8(13) . . ? F23Z B21 F23Y 58.9(13) . . ? F22Y B21 F23Y 108.6(8) . . ? F22X B21 F23Y 106.6(12) . . ? F25Z B21 F23Y 65.2(13) . . ? F23X B21 F24X 112.7(7) . . ? F24Y B21 F24X 29.4(8) . . ? F22Z B21 F24X 82.4(12) . . ? F25X B21 F24X 105.0(7) . . ? F24Z B21 F24X 87.3(12) . . ? F23Z B21 F24X 45.5(12) . . ? F22Y B21 F24X 93.3(10) . . ? F22X B21 F24X 104.7(7) . . ? F25Z B21 F24X 153.7(12) . . ? F23Y B21 F24X 91.9(9) . . ? F23X B21 F25Y 89.6(9) . . ? F24Y B21 F25Y 110.2(8) . . ? F22Z B21 F25Y 127.5(13) . . ? F25X B21 F25Y 35.1(7) . . ? F24Z B21 F25Y 58.2(12) . . ? F23Z B21 F25Y 121.3(13) . . ? F22Y B21 F25Y 107.6(8) . . ? F22X B21 F25Y 98.8(10) . . ? F25Z B21 F25Y 50.9(12) . . ? F23Y B21 F25Y 112.4(8) . . ? F24X B21 F25Y 139.5(8) . . ? F35Y B31 F34Y 109.73(15) . . ? F35Y B31 F33X 127.0(4) . . ? F34Y B31 F33X 88.7(6) . . ? F35Y B31 F32 109.63(15) . . ? F34Y B31 F32 109.45(15) . . ? F33X B31 F32 109.75(15) . . ? F35Y B31 F33Y 109.52(15) . . ? F34Y B31 F33Y 109.34(15) . . ? F33X B31 F33Y 22.4(6) . . ? F32 B31 F33Y 109.16(15) . . ? F35Y B31 F34X 88.7(5) . . ? F34Y B31 F34X 23.2(6) . . ? F33X B31 F34X 109.60(15) . . ? F32 B31 F34X 109.67(15) . . ? F33Y B31 F34X 127.7(4) . . ? F35Y B31 F35X 22.4(6) . . ? F34Y B31 F35X 127.6(4) . . ? F33X B31 F35X 109.33(15) . . ? F32 B31 F35X 109.46(15) . . ? F33Y B31 F35X 89.3(6) . . ? F34X B31 F35X 109.01(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N211 Ni1 N111 C116 -113.8(16) . . . . ? N311 Ni1 N111 C116 -5.5(3) . . . . ? N322 Ni1 N111 C116 72.9(3) . . . . ? N222 Ni1 N111 C116 -96.8(3) . . . . ? N122 Ni1 N111 C116 173.1(3) . . . . ? N211 Ni1 N111 C112 65.0(17) . . . . ? N311 Ni1 N111 C112 173.2(2) . . . . ? N322 Ni1 N111 C112 -108.3(2) . . . . ? N222 Ni1 N111 C112 82.0(2) . . . . ? N122 Ni1 N111 C112 -8.1(2) . . . . ? C116 N111 C112 C113 3.1(4) . . . . ? Ni1 N111 C112 C113 -175.8(2) . . . . ? C116 N111 C112 C123 -175.6(3) . . . . ? Ni1 N111 C112 C123 5.5(3) . . . . ? N111 C112 C113 C114 -2.3(5) . . . . ? C123 C112 C113 C114 176.3(3) . . . . ? C112 C113 C114 C115 -0.4(5) . . . . ? C113 C114 C115 C116 2.1(5) . . . . ? C112 N111 C116 C115 -1.2(5) . . . . ? Ni1 N111 C116 C115 177.5(2) . . . . ? C114 C115 C116 N111 -1.4(5) . . . . ? C125 N121 N122 C123 1.2(3) . . . . ? C126 N121 N122 C123 176.5(3) . . . . ? C125 N121 N122 Ni1 -167.5(3) . . . . ? C126 N121 N122 Ni1 7.8(5) . . . . ? N211 Ni1 N122 C123 -166.9(2) . . . . ? N111 Ni1 N122 C123 9.6(2) . . . . ? N311 Ni1 N122 C123 19.0(8) . . . . ? N322 Ni1 N122 C123 99.5(2) . . . . ? N222 Ni1 N122 C123 -87.8(2) . . . . ? N211 Ni1 N122 N121 1.2(3) . . . . ? N111 Ni1 N122 N121 177.7(3) . . . . ? N311 Ni1 N122 N121 -173.0(5) . . . . ? N322 Ni1 N122 N121 -92.5(3) . . . . ? N222 Ni1 N122 N121 80.2(3) . . . . ? N121 N122 C123 C124 -0.9(3) . . . . ? Ni1 N122 C123 C124 171.5(2) . . . . ? N121 N122 C123 C112 177.7(3) . . . . ? Ni1 N122 C123 C112 -10.0(3) . . . . ? N111 C112 C123 N122 3.2(4) . . . . ? C113 C112 C123 N122 -175.5(3) . . . . ? N111 C112 C123 C124 -178.6(3) . . . . ? C113 C112 C123 C124 2.7(5) . . . . ? N122 C123 C124 C125 0.2(4) . . . . ? C112 C123 C124 C125 -178.1(3) . . . . ? N122 N121 C125 C124 -1.0(4) . . . . ? C126 N121 C125 C124 -176.0(3) . . . . ? C123 C124 C125 N121 0.5(4) . . . . ? N122 N121 C126 C131 -88.4(3) . . . . ? C125 N121 C126 C131 86.1(4) . . . . ? N121 C126 C131 C132 -13.2(4) . . . . ? N121 C126 C131 C136 166.5(3) . . . . ? C136 C131 C132 C133 -2.4(5) . . . . ? C126 C131 C132 C133 177.3(3) . . . . ? C131 C132 C133 C134 -0.2(6) . . . . ? C132 C133 C134 C135 1.6(5) . . . . ? C132 C133 C134 C151 -179.2(3) . . . . ? C133 C134 C135 C141 179.6(3) . . . . ? C151 C134 C135 C141 0.3(5) . . . . ? C133 C134 C135 C136 -0.4(5) . . . . ? C151 C134 C135 C136 -179.6(3) . . . . ? C141 C135 C136 C144 -2.1(5) . . . . ? C134 C135 C136 C144 177.8(3) . . . . ? C141 C135 C136 C131 177.9(3) . . . . ? C134 C135 C136 C131 -2.2(4) . . . . ? C132 C131 C136 C144 -176.5(3) . . . . ? C126 C131 C136 C144 3.8(5) . . . . ? C132 C131 C136 C135 3.6(5) . . . . ? C126 C131 C136 C135 -176.2(3) . . . . ? C136 C135 C141 C142 1.3(5) . . . . ? C134 C135 C141 C142 -178.6(3) . . . . ? C135 C141 C142 C143 0.5(6) . . . . ? C141 C142 C143 C144 -1.6(6) . . . . ? C142 C143 C144 C136 0.8(6) . . . . ? C135 C136 C144 C143 1.1(5) . . . . ? C131 C136 C144 C143 -178.9(3) . . . . ? C133 C134 C151 N152 -105(16) . . . . ? C135 C134 C151 N152 74(16) . . . . ? N111 Ni1 N211 C216 -165.7(15) . . . . ? N311 Ni1 N211 C216 85.9(3) . . . . ? N322 Ni1 N211 C216 7.6(3) . . . . ? N222 Ni1 N211 C216 177.1(3) . . . . ? N122 Ni1 N211 C216 -93.3(3) . . . . ? N111 Ni1 N211 C212 25.8(17) . . . . ? N311 Ni1 N211 C212 -82.6(2) . . . . ? N322 Ni1 N211 C212 -160.8(2) . . . . ? N222 Ni1 N211 C212 8.7(2) . . . . ? N122 Ni1 N211 C212 98.3(2) . . . . ? C216 N211 C212 C213 -0.8(5) . . . . ? Ni1 N211 C212 C213 168.7(3) . . . . ? C216 N211 C212 C223 -178.3(3) . . . . ? Ni1 N211 C212 C223 -8.8(3) . . . . ? N211 C212 C213 C214 0.4(5) . . . . ? C223 C212 C213 C214 177.7(3) . . . . ? C212 C213 C214 C215 0.4(6) . . . . ? C213 C214 C215 C216 -0.8(6) . . . . ? C212 N211 C216 C215 0.4(5) . . . . ? Ni1 N211 C216 C215 -167.6(3) . . . . ? C214 C215 C216 N211 0.4(6) . . . . ? C225 N221 N222 C223 1.0(4) . . . . ? C226 N221 N222 C223 -179.6(3) . . . . ? C225 N221 N222 Ni1 167.5(3) . . . . ? C226 N221 N222 Ni1 -13.2(5) . . . . ? N211 Ni1 N222 C223 -7.1(2) . . . . ? N111 Ni1 N222 C223 173.9(2) . . . . ? N311 Ni1 N222 C223 79.9(2) . . . . ? N322 Ni1 N222 C223 40.9(5) . . . . ? N122 Ni1 N222 C223 -108.2(2) . . . . ? N211 Ni1 N222 N221 -173.0(3) . . . . ? N111 Ni1 N222 N221 8.1(3) . . . . ? N311 Ni1 N222 N221 -86.0(3) . . . . ? N322 Ni1 N222 N221 -124.9(4) . . . . ? N122 Ni1 N222 N221 85.9(3) . . . . ? N221 N222 C223 C224 -0.7(4) . . . . ? Ni1 N222 C223 C224 -171.7(2) . . . . ? N221 N222 C223 C212 175.9(3) . . . . ? Ni1 N222 C223 C212 4.9(3) . . . . ? N211 C212 C223 N222 2.6(4) . . . . ? C213 C212 C223 N222 -174.9(3) . . . . ? N211 C212 C223 C224 178.4(3) . . . . ? C213 C212 C223 C224 0.9(5) . . . . ? N222 C223 C224 C225 0.2(4) . . . . ? C212 C223 C224 C225 -175.9(3) . . . . ? N222 N221 C225 C224 -1.0(4) . . . . ? C226 N221 C225 C224 179.7(3) . . . . ? C223 C224 C225 N221 0.5(4) . . . . ? C225 N221 C226 C231 83.5(4) . . . . ? N222 N221 C226 C231 -95.8(3) . . . . ? N221 C226 C231 C232 5.5(4) . . . . ? N221 C226 C231 C236 -173.4(3) . . . . ? C236 C231 C232 C233 -2.2(6) . . . . ? C226 C231 C232 C233 179.0(4) . . . . ? C231 C232 C233 C234 1.6(7) . . . . ? C232 C233 C234 C251 -179.6(4) . . . . ? C232 C233 C234 C235 1.2(7) . . . . ? C233 C234 C235 C241 176.3(4) . . . . ? C251 C234 C235 C241 -3.0(6) . . . . ? C233 C234 C235 C236 -3.3(6) . . . . ? C251 C234 C235 C236 177.5(4) . . . . ? C241 C235 C236 C244 1.9(5) . . . . ? C234 C235 C236 C244 -178.5(3) . . . . ? C241 C235 C236 C231 -176.9(3) . . . . ? C234 C235 C236 C231 2.7(5) . . . . ? C232 C231 C236 C244 -178.8(3) . . . . ? C226 C231 C236 C244 0.1(5) . . . . ? C232 C231 C236 C235 0.0(5) . . . . ? C226 C231 C236 C235 178.8(3) . . . . ? C236 C235 C241 C242 -0.7(6) . . . . ? C234 C235 C241 C242 179.8(4) . . . . ? C235 C241 C242 C243 -0.9(6) . . . . ? C241 C242 C243 C244 1.3(6) . . . . ? C242 C243 C244 C236 0.0(6) . . . . ? C235 C236 C244 C243 -1.5(5) . . . . ? C231 C236 C244 C243 177.2(3) . . . . ? C233 C234 C251 N252 89(98) . . . . ? C235 C234 C251 N252 -91(98) . . . . ? N211 Ni1 N311 C316 89.9(3) . . . . ? N111 Ni1 N311 C316 -86.7(3) . . . . ? N322 Ni1 N311 C316 -178.1(3) . . . . ? N222 Ni1 N311 C316 11.0(3) . . . . ? N122 Ni1 N311 C316 -95.9(7) . . . . ? N211 Ni1 N311 C312 -91.8(2) . . . . ? N111 Ni1 N311 C312 91.6(2) . . . . ? N322 Ni1 N311 C312 0.3(2) . . . . ? N222 Ni1 N311 C312 -170.7(2) . . . . ? N122 Ni1 N311 C312 82.5(7) . . . . ? C316 N311 C312 C313 1.0(5) . . . . ? Ni1 N311 C312 C313 -177.5(3) . . . . ? C316 N311 C312 C323 -179.4(3) . . . . ? Ni1 N311 C312 C323 2.1(3) . . . . ? N311 C312 C313 C314 -0.2(5) . . . . ? C323 C312 C313 C314 -179.8(3) . . . . ? C312 C313 C314 C315 -0.7(6) . . . . ? C313 C314 C315 C316 0.9(7) . . . . ? C312 N311 C316 C315 -0.8(5) . . . . ? Ni1 N311 C316 C315 177.5(3) . . . . ? C314 C315 C316 N311 -0.2(6) . . . . ? C325 N321 N322 C323 0.8(3) . . . . ? C326 N321 N322 C323 169.1(3) . . . . ? C325 N321 N322 Ni1 169.3(3) . . . . ? C326 N321 N322 Ni1 -22.3(5) . . . . ? N211 Ni1 N322 C323 84.0(2) . . . . ? N111 Ni1 N322 C323 -96.4(2) . . . . ? N311 Ni1 N322 C323 -2.8(2) . . . . ? N222 Ni1 N322 C323 37.1(5) . . . . ? N122 Ni1 N322 C323 -174.2(2) . . . . ? N211 Ni1 N322 N321 -83.9(3) . . . . ? N111 Ni1 N322 N321 95.6(3) . . . . ? N311 Ni1 N322 N321 -170.8(3) . . . . ? N222 Ni1 N322 N321 -130.8(4) . . . . ? N122 Ni1 N322 N321 17.8(3) . . . . ? N321 N322 C323 C324 -0.5(3) . . . . ? Ni1 N322 C323 C324 -172.7(2) . . . . ? N321 N322 C323 C312 177.1(2) . . . . ? Ni1 N322 C323 C312 4.9(3) . . . . ? N311 C312 C323 N322 -4.8(4) . . . . ? C313 C312 C323 N322 174.9(3) . . . . ? N311 C312 C323 C324 172.3(3) . . . . ? C313 C312 C323 C324 -8.1(5) . . . . ? N322 C323 C324 C325 0.1(4) . . . . ? C312 C323 C324 C325 -177.1(3) . . . . ? N322 N321 C325 C324 -0.7(4) . . . . ? C326 N321 C325 C324 -168.1(3) . . . . ? C323 C324 C325 N321 0.4(4) . . . . ? N322 N321 C326 C331 -73.0(4) . . . . ? C325 N321 C326 C331 93.3(4) . . . . ? N321 C326 C331 C332 -9.1(4) . . . . ? N321 C326 C331 C336 169.3(3) . . . . ? C336 C331 C332 C333 -1.8(5) . . . . ? C326 C331 C332 C333 176.5(3) . . . . ? C331 C332 C333 C334 -1.0(5) . . . . ? C332 C333 C334 C335 2.4(5) . . . . ? C332 C333 C334 C351 -174.2(3) . . . . ? C333 C334 C335 C341 179.5(4) . . . . ? C351 C334 C335 C341 -3.9(6) . . . . ? C333 C334 C335 C336 -0.9(5) . . . . ? C351 C334 C335 C336 175.7(3) . . . . ? C341 C335 C336 C344 -1.4(5) . . . . ? C334 C335 C336 C344 178.9(3) . . . . ? C341 C335 C336 C331 177.7(3) . . . . ? C334 C335 C336 C331 -1.9(5) . . . . ? C332 C331 C336 C335 3.3(5) . . . . ? C326 C331 C336 C335 -175.1(3) . . . . ? C332 C331 C336 C344 -177.6(3) . . . . ? C326 C331 C336 C344 4.0(5) . . . . ? C336 C335 C341 C342 0.7(6) . . . . ? C334 C335 C341 C342 -179.6(4) . . . . ? C335 C341 C342 C343 0.1(8) . . . . ? C341 C342 C343 C344 -0.3(8) . . . . ? C342 C343 C344 C336 -0.5(7) . . . . ? C335 C336 C344 C343 1.3(6) . . . . ? C331 C336 C344 C343 -177.8(4) . . . . ? C333 C334 C351 N352 93(13) . . . . ? C335 C334 C351 N352 -84(13) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.345 _refine_diff_density_min -1.158 _refine_diff_density_rms 0.117 #===END data_imw1299p213 _database_code_depnum_ccdc_archive 'CCDC 758093' #TrackingRef 'mixed_metal_networks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H45 Ag B3 F12 N13 Ni O2' _chemical_formula_weight 1419.11 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' Ag Ag -0.8971 1.1015 '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' F F 0.0171 0.0103 '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' Ni Ni 0.3393 1.1124 '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' H H 0.0000 0.0000 '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+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' 'z, x, y' '-z+1/2, -x, y+1/2' 'z+1/2, -x+1/2, -y' '-z, x+1/2, -y+1/2' 'y, z, x' 'y+1/2, -z+1/2, -x' '-y, z+1/2, -x+1/2' '-y+1/2, -z, x+1/2' _cell_length_a 23.0065(2) _cell_length_b 23.0065(2) _cell_length_c 23.0065(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12177.32(18) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9844 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 21.14 _exptl_crystal_description Block _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5728 _exptl_absorpt_coefficient_mu 0.724 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8688 _exptl_absorpt_correction_T_max 0.9311 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 170762 _diffrn_reflns_av_R_equivalents 0.0764 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 27.46 _reflns_number_total 9317 _reflns_number_gt 7327 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure is of {[Ag4{Co(L)3}4](BF4)12}n.4MeNO2 The data was solved by direct methods. Hydrogen atoms were included in calculated positions. Attempts to obtain a better data set were hampered by the weakly diffracting nature of the crystals, presumably due to the large number of voids present in the structure and lattice and the high disorder arising from a combination of fluxional counter- ions solvent molecules. Due to the weakness of the data all five and six-membered rings have benefitted from geometric restraints. The tertrafluoroborate counter-ion B21 F22 > F25 displays rotational disorder through the B21 - F22 (80:20) bond. Geometric and global displacement restraints have been applied to boron and fluorine atoms to improve the model. The structure also contains a disordered nitromethane (O11, O12, N13, C14; 33% occupancy in each of two closely-spaced sites) that has also benefitted from the application of geometric and displacement restraints. All disordered residues have been left isotropic. A Platon SQUEEZE function was used to eliminate a void containing disordered counter-ions and solvent molecules. These could not be satisfactorily modelled and were therefore omitted from the refinement. Only two thirds of the required counter-ions could be found from the data. 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 0.096 -0.097 0.404 180 105 ' ' 2 -0.097 0.403 0.096 180 104 ' ' 3 0.096 0.404 0.596 69 41 ' ' 4 0.403 0.096 0.904 180 105 ' ' 5 0.404 0.596 0.096 69 41 ' ' 6 0.596 0.596 0.596 180 104 ' ' 7 0.596 0.096 0.404 69 41 ' ' 8 0.904 0.904 0.904 69 41 ' ' _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^)+(0.2000P)^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 0.09(4) _refine_ls_number_reflns 9317 _refine_ls_number_parameters 461 _refine_ls_number_restraints 98 _refine_ls_R_factor_all 0.1290 _refine_ls_R_factor_gt 0.1145 _refine_ls_wR_factor_ref 0.3330 _refine_ls_wR_factor_gt 0.3214 _refine_ls_goodness_of_fit_ref 1.339 _refine_ls_restrained_S_all 1.365 _refine_ls_shift/su_max 0.003 _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 Ag11 Ag 0.48961(4) 0.51039(4) 1.01039(4) 0.0521(4) Uani 1 3 d S . . Ni11 Ni 0.61095(4) 0.88905(4) 1.11095(4) 0.0325(4) Uani 1 3 d S . . N111 N 0.70171(15) 0.8985(2) 1.1137(2) 0.0379(14) Uani 1 1 d G . . C112 C 0.7283(2) 0.9025(2) 1.05957(17) 0.0399(18) Uani 1 1 d G . . C113 C 0.7883(2) 0.9085(3) 1.0558(2) 0.047(2) Uani 1 1 d G . . H113 H 0.8065 0.9113 1.0188 0.057 Uiso 1 1 calc R . . C114 C 0.82172(15) 0.9104(3) 1.1061(3) 0.058(3) Uani 1 1 d G . . H114 H 0.8627 0.9145 1.1034 0.069 Uiso 1 1 calc R . . C115 C 0.7951(2) 0.9063(3) 1.1602(2) 0.057(3) Uani 1 1 d G . . H115 H 0.8180 0.9076 1.1945 0.068 Uiso 1 1 calc R . . C116 C 0.7351(2) 0.9004(3) 1.16397(17) 0.046(2) Uani 1 1 d G . . H116 H 0.7170 0.8976 1.2009 0.055 Uiso 1 1 calc R . . N121 N 0.6045(2) 0.8982(2) 0.9662(2) 0.0453(17) Uani 1 1 d G . . N122 N 0.6319(2) 0.8952(2) 1.02146(16) 0.0369(14) Uani 1 1 d G . . C123 C 0.69267(19) 0.9018(3) 1.0130(2) 0.0401(18) Uani 1 1 d G . . C124 C 0.7028(2) 0.9089(3) 0.9525(3) 0.065(3) Uani 1 1 d G . . H124 H 0.7396 0.9142 0.9345 0.078 Uiso 1 1 calc R . . C125 C 0.6483(3) 0.9066(3) 0.92361(16) 0.048(2) Uani 1 1 d G . . H125 H 0.6423 0.9101 0.8829 0.057 Uiso 1 1 calc R . . C126 C 0.5464(4) 0.8843(4) 0.9585(4) 0.046(2) Uani 1 1 d . . . H12A H 0.5318 0.9043 0.9233 0.056 Uiso 1 1 calc R . . H12B H 0.5239 0.8988 0.9922 0.056 Uiso 1 1 calc R . . C131 C 0.5356(2) 0.81742(15) 0.9519(2) 0.0412(19) Uani 1 1 d G . . C132 C 0.58248(16) 0.7795(2) 0.9545(2) 0.0394(18) Uani 1 1 d G . . H132 H 0.6208 0.7943 0.9588 0.047 Uiso 1 1 calc R . . C133 C 0.5734(2) 0.71985(19) 0.9507(3) 0.047(2) Uani 1 1 d G . . H133 H 0.6054 0.6939 0.9525 0.056 Uiso 1 1 calc R . . C134 C 0.5173(2) 0.69821(15) 0.9444(3) 0.054(2) Uani 1 1 d G . . C135 C 0.47038(18) 0.7362(2) 0.9418(2) 0.044(2) Uani 1 1 d GD . . C136 C 0.47950(17) 0.7958(2) 0.9456(2) 0.0437(19) Uani 1 1 d GD . . C141 C 0.4153(2) 0.7126(2) 0.9338(5) 0.066(3) Uani 1 1 d D . . H141 H 0.4108 0.6718 0.9296 0.079 Uiso 1 1 calc R . . C142 C 0.36694(19) 0.7487(3) 0.9318(6) 0.071(3) Uani 1 1 d D . . H142 H 0.3287 0.7332 0.9310 0.086 Uiso 1 1 calc R . . C143 C 0.37659(18) 0.8083(3) 0.9311(4) 0.063(3) Uani 1 1 d D . . H143 H 0.3448 0.8337 0.9239 0.076 Uiso 1 1 calc R . . C144 C 0.4315(2) 0.83215(18) 0.9407(4) 0.055(3) Uani 1 1 d D . . H144 H 0.4361 0.8731 0.9438 0.065 Uiso 1 1 calc R . . C151 C 0.5112(6) 0.6376(6) 0.9479(5) 0.069(3) Uani 1 1 d . . . N152 N 0.5040(5) 0.5836(4) 0.9497(5) 0.071(3) Uani 1 1 d . . . Ag21 Ag 0.75736(6) 0.75736(6) 0.75736(6) 0.0773(5) Uani 1 3 d S . . Ni21 Ni 0.61829(4) 0.38171(4) 0.88171(4) 0.0320(4) Uani 1 3 d S . . N211 N 0.6122(2) 0.3681(2) 0.97231(16) 0.0431(16) Uani 1 1 d G . . C212 C 0.6653(2) 0.3624(2) 1.0006(2) 0.042(2) Uani 1 1 d G . . C213 C 0.6668(3) 0.3501(3) 1.0597(2) 0.053(2) Uani 1 1 d G . . H213 H 0.7031 0.3462 1.0791 0.064 Uiso 1 1 calc R . . C214 C 0.6153(3) 0.3434(3) 1.09056(16) 0.064(3) Uani 1 1 d G . . H214 H 0.6163 0.3350 1.1310 0.077 Uiso 1 1 calc R . . C215 C 0.5622(3) 0.3491(3) 1.0623(2) 0.067(3) Uani 1 1 d G . . H215 H 0.5270 0.3445 1.0833 0.080 Uiso 1 1 calc R . . C216 C 0.5607(2) 0.3614(3) 1.0031(2) 0.053(2) Uani 1 1 d G . . H216 H 0.5244 0.3653 0.9838 0.064 Uiso 1 1 calc R . . N221 N 0.7624(2) 0.3722(2) 0.88015(19) 0.0461(18) Uani 1 1 d G . . N222 N 0.70622(16) 0.3718(2) 0.90568(19) 0.0349(14) Uani 1 1 d G . . C223 C 0.7130(2) 0.3653(3) 0.96667(18) 0.0416(19) Uani 1 1 d G . . C224 C 0.7734(3) 0.3616(3) 0.9788(2) 0.052(2) Uani 1 1 d G . . H224 H 0.7904 0.3570 1.0162 0.062 Uiso 1 1 calc R . . C225 C 0.80395(16) 0.3658(3) 0.9254(3) 0.052(2) Uani 1 1 d G . . H225 H 0.8450 0.3647 0.9207 0.063 Uiso 1 1 calc R . . C226 C 0.7736(3) 0.3865(4) 0.8233(4) 0.0425(19) Uani 1 1 d . . . H22A H 0.7407 0.3727 0.7992 0.051 Uiso 1 1 calc R . . H22B H 0.8087 0.3649 0.8107 0.051 Uiso 1 1 calc R . . C231 C 0.7831(2) 0.45004(17) 0.8104(2) 0.044(2) Uani 1 1 d G . . C232 C 0.7864(2) 0.4888(2) 0.85662(15) 0.0445(19) Uani 1 1 d G . . H232 H 0.7835 0.4750 0.8954 0.053 Uiso 1 1 calc R . . C233 C 0.7941(2) 0.5478(2) 0.8461(2) 0.048(2) Uani 1 1 d G . . H233 H 0.7963 0.5743 0.8777 0.058 Uiso 1 1 calc R . . C234 C 0.7984(2) 0.56804(17) 0.7893(2) 0.050(2) Uani 1 1 d G . . C235 C 0.7951(2) 0.5293(2) 0.74310(17) 0.049(2) Uani 1 1 d GD . . C236 C 0.7875(2) 0.4703(2) 0.75363(18) 0.051(2) Uani 1 1 d GD . . C241 C 0.7937(5) 0.5502(2) 0.68644(19) 0.063(3) Uani 1 1 d D . . H241 H 0.7944 0.5909 0.6795 0.075 Uiso 1 1 calc R . . C242 C 0.7912(5) 0.5117(4) 0.6400(2) 0.072(3) Uani 1 1 d D . . H242 H 0.7921 0.5258 0.6012 0.087 Uiso 1 1 calc R . . C243 C 0.7874(5) 0.4523(4) 0.65052(17) 0.067(3) Uani 1 1 d D . . H243 H 0.7851 0.4259 0.6189 0.081 Uiso 1 1 calc R . . C244 C 0.7868(4) 0.4314(2) 0.7074(2) 0.061(3) Uani 1 1 d D . . H244 H 0.7860 0.3908 0.7145 0.073 Uiso 1 1 calc R . . C251 C 0.8058(6) 0.6290(6) 0.7838(7) 0.076(4) Uani 1 1 d . . . N252 N 0.8127(6) 0.6790(4) 0.7780(6) 0.091(4) Uani 1 1 d . . . B11 B 0.7588(2) 0.2412(2) 0.7412(2) 0.0678(15) Uani 1 3 d SDU . . F12 F 0.7326(3) 0.2344(3) 0.6877(2) 0.0689(14) Uani 1 1 d DU . . F13 F 0.7241(2) 0.2759(2) 0.7759(2) 0.0683(15) Uani 1 3 d SDU . . B21 B 0.5586(3) 0.0152(3) 0.7990(3) 0.1062(18) Uiso 1 1 d DU . . F22 F 0.5509(4) 0.0647(3) 0.8318(4) 0.1072(18) Uiso 1 1 d DU A . F23X F 0.6057(4) 0.0225(4) 0.7625(4) 0.1074(18) Uiso 0.795(10) 1 d PDU A 1 F24X F 0.5685(5) -0.0315(3) 0.8352(4) 0.1077(18) Uiso 0.795(10) 1 d PDU A 1 F25X F 0.5094(3) 0.0050(4) 0.7662(4) 0.1062(18) Uiso 0.795(10) 1 d PDU A 1 F23Y F 0.6082(8) -0.0133(8) 0.8169(10) 0.1071(18) Uiso 0.205(10) 1 d PDU A 2 F24Y F 0.5112(7) -0.0210(7) 0.8060(11) 0.1069(18) Uiso 0.205(10) 1 d PDU A 2 F25Y F 0.5639(14) 0.0301(5) 0.7411(3) 0.1068(18) Uiso 0.205(10) 1 d PDU A 2 O11X O 0.8021(9) 0.7403(16) 0.9340(14) 0.17(2) Uiso 0.33 1 d PD B 1 O12X O 0.7397(10) 0.7668(10) 0.9958(8) 0.073(5) Uiso 0.33 1 d PDU B 1 N13X N 0.7489(7) 0.7368(7) 0.9499(7) 0.043(5) Uiso 0.33 1 d PDU B 1 C14X C 0.7050(12) 0.7032(15) 0.9200(14) 0.081(11) Uiso 0.33 1 d PD B 1 H14A H 0.6919 0.7245 0.8854 0.122 Uiso 0.33 1 calc PR B 1 H14B H 0.6719 0.6967 0.9460 0.122 Uiso 0.33 1 calc PR B 1 H14C H 0.7213 0.6657 0.9081 0.122 Uiso 0.33 1 calc PR B 1 O11Y O 0.7205(9) 0.7350(10) 0.9673(9) 0.074(5) Uiso 0.33 1 d PDU C 2 O12Y O 0.7751(12) 0.6738(8) 0.9140(13) 0.098(9) Uiso 0.33 1 d PD C 2 N13Y N 0.7633(7) 0.7262(7) 0.9315(7) 0.053(6) Uiso 0.33 1 d PDU C 2 C14Y C 0.7983(15) 0.7754(11) 0.9107(18) 0.099(15) Uiso 0.33 1 d PD C 2 H14D H 0.8305 0.7609 0.8870 0.149 Uiso 0.33 1 calc PR C 2 H14E H 0.8137 0.7970 0.9441 0.149 Uiso 0.33 1 calc PR C 2 H14F H 0.7739 0.8013 0.8872 0.149 Uiso 0.33 1 calc PR C 2 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 Ag11 0.0521(4) 0.0521(4) 0.0521(4) 0.0052(3) -0.0052(3) -0.0052(3) Ni11 0.0325(4) 0.0325(4) 0.0325(4) -0.0003(4) 0.0003(4) -0.0003(4) N111 0.031(3) 0.038(3) 0.045(4) -0.003(3) -0.002(3) 0.002(3) C112 0.040(4) 0.034(4) 0.046(5) -0.010(3) 0.003(3) 0.000(3) C113 0.051(5) 0.029(4) 0.062(6) -0.008(4) 0.014(4) -0.002(4) C114 0.041(5) 0.034(4) 0.098(9) -0.009(5) 0.007(5) -0.001(4) C115 0.043(5) 0.066(6) 0.061(6) -0.012(5) -0.007(4) 0.011(4) C116 0.036(4) 0.054(5) 0.049(5) 0.010(4) -0.009(4) 0.007(4) N121 0.064(5) 0.030(3) 0.042(4) 0.005(3) 0.002(3) -0.007(3) N122 0.049(4) 0.033(3) 0.029(3) -0.007(2) 0.002(3) -0.004(3) C123 0.051(5) 0.032(4) 0.037(4) -0.010(3) 0.008(4) -0.001(3) C124 0.102(9) 0.030(4) 0.063(6) -0.004(4) 0.047(6) -0.020(5) C125 0.074(6) 0.035(4) 0.034(4) -0.003(3) -0.001(4) -0.005(4) C126 0.073(6) 0.032(4) 0.035(4) -0.003(3) -0.014(4) -0.009(4) C131 0.064(6) 0.033(4) 0.026(4) -0.010(3) 0.008(4) -0.001(4) C132 0.056(5) 0.031(4) 0.031(4) 0.000(3) 0.010(3) -0.008(3) C133 0.067(6) 0.034(4) 0.040(4) -0.002(3) 0.010(4) 0.001(4) C134 0.080(7) 0.044(5) 0.039(5) -0.002(4) 0.002(5) -0.012(5) C135 0.063(6) 0.044(5) 0.024(4) -0.001(3) 0.001(3) -0.010(4) C136 0.051(5) 0.050(5) 0.030(4) 0.005(3) -0.002(3) -0.005(4) C141 0.094(9) 0.033(5) 0.070(7) 0.011(5) -0.007(6) -0.007(5) C142 0.051(6) 0.080(8) 0.083(8) 0.005(6) 0.014(6) -0.021(6) C143 0.069(7) 0.075(7) 0.045(5) 0.010(5) -0.006(5) 0.005(6) C144 0.069(6) 0.067(6) 0.027(4) 0.003(4) -0.009(4) -0.017(5) C151 0.072(7) 0.074(8) 0.062(7) 0.005(5) -0.021(6) -0.001(6) N152 0.088(8) 0.037(4) 0.088(7) -0.001(4) 0.023(6) -0.007(4) Ag21 0.0773(5) 0.0773(5) 0.0773(5) 0.0144(6) 0.0144(6) 0.0144(6) Ni21 0.0320(4) 0.0320(4) 0.0320(4) 0.0024(4) -0.0024(4) -0.0024(4) N211 0.057(4) 0.029(3) 0.043(4) -0.004(3) 0.011(3) -0.011(3) C212 0.070(6) 0.026(4) 0.031(4) 0.000(3) -0.008(4) -0.003(3) C213 0.076(7) 0.040(5) 0.044(5) -0.003(4) -0.008(5) -0.004(5) C214 0.108(10) 0.044(5) 0.040(5) -0.007(4) -0.002(6) 0.007(6) C215 0.092(9) 0.073(7) 0.035(5) -0.019(5) 0.024(5) -0.022(6) C216 0.068(6) 0.041(5) 0.050(6) -0.003(4) 0.008(4) -0.007(4) N221 0.026(3) 0.039(3) 0.074(5) 0.001(3) -0.016(3) 0.001(3) N222 0.041(4) 0.029(3) 0.034(3) 0.000(2) 0.000(3) -0.003(3) C223 0.054(5) 0.028(4) 0.042(4) 0.004(3) -0.015(4) -0.002(3) C224 0.056(6) 0.046(5) 0.053(5) 0.009(4) -0.025(4) 0.006(4) C225 0.050(5) 0.039(5) 0.068(6) -0.002(4) -0.031(5) 0.000(4) C226 0.031(4) 0.035(4) 0.062(5) -0.003(4) 0.000(3) 0.010(3) C231 0.024(4) 0.054(5) 0.055(5) 0.005(4) -0.009(3) 0.001(3) C232 0.033(4) 0.047(5) 0.054(5) -0.006(4) 0.011(4) -0.007(4) C233 0.030(4) 0.043(5) 0.070(6) -0.012(4) -0.003(4) 0.000(3) C234 0.024(4) 0.049(5) 0.079(7) 0.016(5) -0.005(4) 0.004(3) C235 0.026(4) 0.071(6) 0.049(5) 0.001(4) 0.008(3) 0.008(4) C236 0.026(4) 0.065(6) 0.064(6) 0.020(5) 0.007(4) 0.024(4) C241 0.042(5) 0.076(7) 0.070(7) 0.021(6) -0.004(5) 0.002(5) C242 0.060(7) 0.105(10) 0.051(6) 0.003(6) 0.000(5) 0.018(7) C243 0.059(6) 0.092(9) 0.052(6) -0.003(6) -0.003(5) 0.014(6) C244 0.049(6) 0.065(7) 0.070(7) -0.001(5) 0.007(5) 0.030(5) C251 0.075(8) 0.061(7) 0.091(9) -0.002(6) -0.033(7) 0.004(6) N252 0.115(10) 0.033(5) 0.126(11) 0.011(5) -0.016(8) -0.009(5) B11 0.0678(15) 0.0678(15) 0.0678(15) -0.0057(15) 0.0057(15) 0.0057(15) F12 0.0693(17) 0.0693(16) 0.0683(16) -0.0054(16) 0.0050(16) 0.0053(17) F13 0.0683(15) 0.0683(15) 0.0683(15) -0.0059(15) 0.0059(15) 0.0059(15) _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 Ag11 N152 2.214(10) 11_646 ? Ag11 N152 2.214(10) . ? Ag11 N152 2.214(10) 6_665 ? Ni11 N111 2.100(4) 7_467 ? Ni11 N111 2.100(4) . ? Ni11 N111 2.100(4) 12_675 ? Ni11 N122 2.119(4) . ? Ni11 N122 2.119(8) 7_467 ? Ni11 N122 2.119(9) 12_675 ? N111 C112 1.3900 . ? N111 C116 1.3900 . ? C112 C123 1.349(6) . ? C112 C113 1.3900 . ? C113 C114 1.3900 . ? C113 H113 0.9500 . ? C114 C115 1.3900 . ? C114 H114 0.9500 . ? C115 C116 1.3900 . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? N121 C126 1.387(11) . ? N121 C125 1.4200 . ? N121 N122 1.4200 . ? N122 C123 1.4200 . ? C123 C124 1.4200 . ? C124 C125 1.4200 . ? C124 H124 0.9500 . ? C125 H125 0.9500 . ? C126 C131 1.565(9) . ? C126 H12A 0.9900 . ? C126 H12B 0.9900 . ? C131 C132 1.3900 . ? C131 C136 1.3900 . ? C132 C133 1.3900 . ? C132 H132 0.9500 . ? C133 C134 1.3900 . ? C133 H133 0.9500 . ? C134 C135 1.3900 . ? C134 C151 1.403(13) . ? C135 C141 1.3900(10) . ? C135 C136 1.3900 . ? C136 C144 1.3905(10) . ? C141 C142 1.3899(10) . ? C141 H141 0.9500 . ? C142 C143 1.3901(11) . ? C142 H142 0.9500 . ? C143 C144 1.394(3) . ? C143 H143 0.9500 . ? C144 H144 0.9500 . ? C151 N152 1.254(15) . ? Ag21 N252 2.258(11) 5 ? Ag21 N252 2.258(11) . ? Ag21 N252 2.258(11) 9 ? Ni21 N222 2.109(9) 6_665 ? Ni21 N222 2.109(4) . ? Ni21 N222 2.109(8) 11_646 ? Ni21 N211 2.112(4) . ? Ni21 N211 2.112(4) 11_646 ? Ni21 N211 2.112(4) 6_665 ? N211 C212 1.3900 . ? N211 C216 1.3900 . ? C212 C223 1.349(6) . ? C212 C213 1.3900 . ? C213 C214 1.3900 . ? C213 H213 0.9500 . ? C214 C215 1.3900 . ? C214 H214 0.9500 . ? C215 C216 1.3900 . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? N221 C226 1.374(10) . ? N221 N222 1.4200 . ? N221 C225 1.4200 . ? N222 C223 1.4200 . ? C223 C224 1.4200 . ? C224 C225 1.4200 . ? C224 H224 0.9500 . ? C225 H225 0.9500 . ? C226 C231 1.507(10) . ? C226 H22A 0.9900 . ? C226 H22B 0.9900 . ? C231 C232 1.3900 . ? C231 C236 1.3900 . ? C232 C233 1.3900 . ? C232 H232 0.9500 . ? C233 C234 1.3900 . ? C233 H233 0.9500 . ? C234 C235 1.3900 . ? C234 C251 1.418(14) . ? C235 C236 1.3900 . ? C235 C241 1.3902(10) . ? C236 C244 1.3902(10) . ? C241 C242 1.3901(10) . ? C241 H241 0.9500 . ? C242 C243 1.3899(10) . ? C242 H242 0.9500 . ? C243 C244 1.393(3) . ? C243 H243 0.9500 . ? C244 H244 0.9500 . ? C251 N252 1.169(16) . ? B11 F13 1.380(2) . ? B11 F12 1.381(2) 11_646 ? B11 F12 1.381(2) . ? B11 F12 1.381(2) 6_665 ? B21 F24X 1.379(2) . ? B21 F25X 1.380(2) . ? B21 F23Y 1.380(2) . ? B21 F22 1.380(2) . ? B21 F25Y 1.380(2) . ? B21 F24Y 1.380(2) . ? B21 F23X 1.381(2) . ? O11X N13X 1.2794(18) . ? O12X N13X 1.2795(18) . ? N13X C14X 1.4465(18) . ? C14X H14A 0.9800 . ? C14X H14B 0.9800 . ? C14X H14C 0.9800 . ? O11Y N13Y 1.299(2) . ? O12Y N13Y 1.300(2) . ? N13Y C14Y 1.470(2) . ? C14Y H14D 0.9800 . ? C14Y H14E 0.9800 . ? C14Y H14F 0.9800 . ? 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 N152 Ag11 N152 119.988(10) 11_646 . ? N152 Ag11 N152 119.988(10) 11_646 6_665 ? N152 Ag11 N152 119.988(10) . 6_665 ? N111 Ni11 N111 94.4(2) 7_467 . ? N111 Ni11 N111 94.4(2) 7_467 12_675 ? N111 Ni11 N111 94.4(2) . 12_675 ? N111 Ni11 N122 87.7(2) 7_467 . ? N111 Ni11 N122 78.23(19) . . ? N111 Ni11 N122 172.5(2) 12_675 . ? N111 Ni11 N122 78.2(4) 7_467 7_467 ? N111 Ni11 N122 172.5(4) . 7_467 ? N111 Ni11 N122 87.7(5) 12_675 7_467 ? N122 Ni11 N122 99.8(5) . 7_467 ? N111 Ni11 N122 172.5(4) 7_467 12_675 ? N111 Ni11 N122 87.7(4) . 12_675 ? N111 Ni11 N122 78.2(4) 12_675 12_675 ? N122 Ni11 N122 99.8(4) . 12_675 ? N122 Ni11 N122 99.8(5) 7_467 12_675 ? C112 N111 C116 120.0 . . ? C112 N111 Ni11 114.7(3) . . ? C116 N111 Ni11 125.3(3) . . ? C123 C112 N111 116.3(4) . . ? C123 C112 C113 123.7(4) . . ? N111 C112 C113 120.0 . . ? C114 C113 C112 120.0 . . ? C114 C113 H113 120.0 . . ? C112 C113 H113 120.0 . . ? C113 C114 C115 120.0 . . ? C113 C114 H114 120.0 . . ? C115 C114 H114 120.0 . . ? C116 C115 C114 120.0 . . ? C116 C115 H115 120.0 . . ? C114 C115 H115 120.0 . . ? C115 C116 N111 120.0 . . ? C115 C116 H116 120.0 . . ? N111 C116 H116 120.0 . . ? C126 N121 C125 128.9(5) . . ? C126 N121 N122 122.1(5) . . ? C125 N121 N122 108.0 . . ? C123 N122 N121 108.0 . . ? C123 N122 Ni11 111.4(3) . . ? N121 N122 Ni11 140.5(3) . . ? C112 C123 C124 132.6(4) . . ? C112 C123 N122 119.4(4) . . ? C124 C123 N122 108.0 . . ? C123 C124 C125 108.0 . . ? C123 C124 H124 126.0 . . ? C125 C124 H124 126.0 . . ? N121 C125 C124 108.0 . . ? N121 C125 H125 126.0 . . ? C124 C125 H125 126.0 . . ? N121 C126 C131 113.1(7) . . ? N121 C126 H12A 109.0 . . ? C131 C126 H12A 109.0 . . ? N121 C126 H12B 109.0 . . ? C131 C126 H12B 109.0 . . ? H12A C126 H12B 107.8 . . ? C132 C131 C136 120.0 . . ? C132 C131 C126 119.3(5) . . ? C136 C131 C126 120.6(5) . . ? C133 C132 C131 120.0 . . ? C133 C132 H132 120.0 . . ? C131 C132 H132 120.0 . . ? C134 C133 C132 120.0 . . ? C134 C133 H133 120.0 . . ? C132 C133 H133 120.0 . . ? C133 C134 C135 120.0 . . ? C133 C134 C151 116.2(6) . . ? C135 C134 C151 123.3(7) . . ? C141 C135 C136 122.1(3) . . ? C141 C135 C134 117.9(3) . . ? C136 C135 C134 120.0 . . ? C135 C136 C131 120.0 . . ? C135 C136 C144 117.9(3) . . ? C131 C136 C144 122.0(3) . . ? C142 C141 C135 120.06(13) . . ? C142 C141 H141 120.0 . . ? C135 C141 H141 120.0 . . ? C141 C142 C143 117.5(4) . . ? C141 C142 H142 121.2 . . ? C143 C142 H142 121.2 . . ? C142 C143 C144 122.1(4) . . ? C142 C143 H143 119.0 . . ? C144 C143 H143 119.0 . . ? C136 C144 C143 119.74(16) . . ? C136 C144 H144 120.1 . . ? C143 C144 H144 120.1 . . ? N152 C151 C134 177.6(13) . . ? C151 N152 Ag11 142.6(10) . . ? N252 Ag21 N252 119.980(16) 5 . ? N252 Ag21 N252 119.980(15) 5 9 ? N252 Ag21 N252 119.980(15) . 9 ? N222 Ni21 N222 100.1(4) 6_665 . ? N222 Ni21 N222 100.1(4) 6_665 11_646 ? N222 Ni21 N222 100.1(5) . 11_646 ? N222 Ni21 N211 86.9(4) 6_665 . ? N222 Ni21 N211 77.85(19) . . ? N222 Ni21 N211 172.9(3) 11_646 . ? N222 Ni21 N211 172.9(4) 6_665 11_646 ? N222 Ni21 N211 86.9(2) . 11_646 ? N222 Ni21 N211 77.9(3) 11_646 11_646 ? N211 Ni21 N211 95.2(2) . 11_646 ? N222 Ni21 N211 77.9(4) 6_665 6_665 ? N222 Ni21 N211 172.92(19) . 6_665 ? N222 Ni21 N211 86.9(5) 11_646 6_665 ? N211 Ni21 N211 95.2(2) . 6_665 ? N211 Ni21 N211 95.2(2) 11_646 6_665 ? C212 N211 C216 120.0 . . ? C212 N211 Ni21 114.7(3) . . ? C216 N211 Ni21 125.2(3) . . ? C223 C212 N211 116.1(4) . . ? C223 C212 C213 123.7(4) . . ? N211 C212 C213 120.0 . . ? C214 C213 C212 120.0 . . ? C214 C213 H213 120.0 . . ? C212 C213 H213 120.0 . . ? C215 C214 C213 120.0 . . ? C215 C214 H214 120.0 . . ? C213 C214 H214 120.0 . . ? C216 C215 C214 120.0 . . ? C216 C215 H215 120.0 . . ? C214 C215 H215 120.0 . . ? C215 C216 N211 120.0 . . ? C215 C216 H216 120.0 . . ? N211 C216 H216 120.0 . . ? C226 N221 N222 124.5(5) . . ? C226 N221 C225 126.6(5) . . ? N222 N221 C225 108.0 . . ? N221 N222 C223 108.0 . . ? N221 N222 Ni21 139.9(3) . . ? C223 N222 Ni21 112.1(3) . . ? C212 C223 C224 132.8(4) . . ? C212 C223 N222 119.2(4) . . ? C224 C223 N222 108.0 . . ? C223 C224 C225 108.0 . . ? C223 C224 H224 126.0 . . ? C225 C224 H224 126.0 . . ? C224 C225 N221 108.0 . . ? C224 C225 H225 126.0 . . ? N221 C225 H225 126.0 . . ? N221 C226 C231 116.5(7) . . ? N221 C226 H22A 108.2 . . ? C231 C226 H22A 108.2 . . ? N221 C226 H22B 108.2 . . ? C231 C226 H22B 108.2 . . ? H22A C226 H22B 107.3 . . ? C232 C231 C236 120.0 . . ? C232 C231 C226 118.7(5) . . ? C236 C231 C226 121.3(5) . . ? C231 C232 C233 120.0 . . ? C231 C232 H232 120.0 . . ? C233 C232 H232 120.0 . . ? C234 C233 C232 120.0 . . ? C234 C233 H233 120.0 . . ? C232 C233 H233 120.0 . . ? C233 C234 C235 120.0 . . ? C233 C234 C251 115.0(7) . . ? C235 C234 C251 125.0(7) . . ? C234 C235 C236 120.0 . . ? C234 C235 C241 119.7(4) . . ? C236 C235 C241 120.0(4) . . ? C235 C236 C231 120.0 . . ? C235 C236 C244 119.7(4) . . ? C231 C236 C244 120.2(4) . . ? C242 C241 C235 120.01(13) . . ? C242 C241 H241 120.0 . . ? C235 C241 H241 120.0 . . ? C243 C242 C241 119.7(4) . . ? C243 C242 H242 120.1 . . ? C241 C242 H242 120.1 . . ? C242 C243 C244 120.2(4) . . ? C242 C243 H243 119.9 . . ? C244 C243 H243 119.9 . . ? C236 C244 C243 119.81(16) . . ? C236 C244 H244 120.1 . . ? C243 C244 H244 120.1 . . ? N252 C251 C234 178.3(19) . . ? C251 N252 Ag21 137.2(12) . . ? F13 B11 F12 109.2(5) . 11_646 ? F13 B11 F12 109.2(5) . . ? F12 B11 F12 109.7(5) 11_646 . ? F13 B11 F12 109.2(5) . 6_665 ? F12 B11 F12 109.7(5) 11_646 6_665 ? F12 B11 F12 109.7(5) . 6_665 ? F24X B21 F25X 109.54(16) . . ? F24X B21 F23Y 46.6(12) . . ? F25X B21 F23Y 139.7(4) . . ? F24X B21 F22 109.49(16) . . ? F25X B21 F22 109.53(16) . . ? F23Y B21 F22 109.51(16) . . ? F24X B21 F25Y 139.7(4) . . ? F25X B21 F25Y 65.7(12) . . ? F23Y B21 F25Y 109.46(16) . . ? F22 B21 F25Y 109.48(16) . . ? F24X B21 F24Y 65.9(12) . . ? F25X B21 F24Y 46.7(12) . . ? F23Y B21 F24Y 109.47(16) . . ? F22 B21 F24Y 109.46(16) . . ? F25Y B21 F24Y 109.46(16) . . ? F24X B21 F23X 109.46(16) . . ? F25X B21 F23X 109.42(16) . . ? F23Y B21 F23X 65.8(12) . . ? F22 B21 F23X 109.38(16) . . ? F25Y B21 F23X 46.7(12) . . ? F24Y B21 F23X 139.9(4) . . ? O11X N13X O12X 111.19(19) . . ? O11X N13X C14X 124.4(2) . . ? O12X N13X C14X 124.4(2) . . ? N13X C14X H14A 109.5 . . ? N13X C14X H14B 109.5 . . ? H14A C14X H14B 109.5 . . ? N13X C14X H14C 109.5 . . ? H14A C14X H14C 109.5 . . ? H14B C14X H14C 109.5 . . ? O11Y N13Y O12Y 119.9(4) . . ? O11Y N13Y C14Y 120.1(3) . . ? O12Y N13Y C14Y 120.0(3) . . ? N13Y C14Y H14D 109.5 . . ? N13Y C14Y H14E 109.5 . . ? H14D C14Y H14E 109.5 . . ? N13Y C14Y H14F 109.5 . . ? H14D C14Y H14F 109.5 . . ? H14E C14Y H14F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N111 Ni11 N111 C112 85.5(4) 7_467 . . . ? N111 Ni11 N111 C112 -179.7(3) 12_675 . . . ? N122 Ni11 N111 C112 -1.2(3) . . . . ? N122 Ni11 N111 C112 75(4) 7_467 . . . ? N122 Ni11 N111 C112 -101.7(5) 12_675 . . . ? N111 Ni11 N111 C116 -94.0(3) 7_467 . . . ? N111 Ni11 N111 C116 0.7(4) 12_675 . . . ? N122 Ni11 N111 C116 179.3(4) . . . . ? N122 Ni11 N111 C116 -105(4) 7_467 . . . ? N122 Ni11 N111 C116 78.7(5) 12_675 . . . ? C116 N111 C112 C123 -178.4(6) . . . . ? Ni11 N111 C112 C123 2.1(5) . . . . ? C116 N111 C112 C113 0.0 . . . . ? Ni11 N111 C112 C113 -179.6(4) . . . . ? C123 C112 C113 C114 178.3(6) . . . . ? N111 C112 C113 C114 0.0 . . . . ? C112 C113 C114 C115 0.0 . . . . ? C113 C114 C115 C116 0.0 . . . . ? C114 C115 C116 N111 0.0 . . . . ? C112 N111 C116 C115 0.0 . . . . ? Ni11 N111 C116 C115 179.5(4) . . . . ? C126 N121 N122 C123 169.7(7) . . . . ? C125 N121 N122 C123 0.0 . . . . ? C126 N121 N122 Ni11 -14.9(8) . . . . ? C125 N121 N122 Ni11 175.3(6) . . . . ? N111 Ni11 N122 C123 -94.8(3) 7_467 . . . ? N111 Ni11 N122 C123 0.2(3) . . . . ? N111 Ni11 N122 C123 11.1(17) 12_675 . . . ? N122 Ni11 N122 C123 -172.4(4) 7_467 . . . ? N122 Ni11 N122 C123 85.7(6) 12_675 . . . ? N111 Ni11 N122 N121 90.0(5) 7_467 . . . ? N111 Ni11 N122 N121 -175.1(5) . . . . ? N111 Ni11 N122 N121 -164.1(14) 12_675 . . . ? N122 Ni11 N122 N121 12.3(6) 7_467 . . . ? N122 Ni11 N122 N121 -89.6(2) 12_675 . . . ? N111 C112 C123 C124 175.1(4) . . . . ? C113 C112 C123 C124 -3.2(8) . . . . ? N111 C112 C123 N122 -2.0(6) . . . . ? C113 C112 C123 N122 179.7(4) . . . . ? N121 N122 C123 C112 177.8(6) . . . . ? Ni11 N122 C123 C112 0.9(5) . . . . ? N121 N122 C123 C124 0.0 . . . . ? Ni11 N122 C123 C124 -176.8(4) . . . . ? C112 C123 C124 C125 -177.3(7) . . . . ? N122 C123 C124 C125 0.0 . . . . ? C126 N121 C125 C124 -168.8(7) . . . . ? N122 N121 C125 C124 0.0 . . . . ? C123 C124 C125 N121 0.0 . . . . ? C125 N121 C126 C131 84.7(8) . . . . ? N122 N121 C126 C131 -82.7(8) . . . . ? N121 C126 C131 C132 0.3(8) . . . . ? N121 C126 C131 C136 178.0(5) . . . . ? C136 C131 C132 C133 0.0 . . . . ? C126 C131 C132 C133 177.8(6) . . . . ? C131 C132 C133 C134 0.0 . . . . ? C132 C133 C134 C135 0.0 . . . . ? C132 C133 C134 C151 -172.7(7) . . . . ? C133 C134 C135 C141 178.2(7) . . . . ? C151 C134 C135 C141 -9.7(9) . . . . ? C133 C134 C135 C136 0.0 . . . . ? C151 C134 C135 C136 172.1(8) . . . . ? C141 C135 C136 C131 -178.1(8) . . . . ? C134 C135 C136 C131 0.0 . . . . ? C141 C135 C136 C144 -0.4(9) . . . . ? C134 C135 C136 C144 177.7(6) . . . . ? C132 C131 C136 C135 0.0 . . . . ? C126 C131 C136 C135 -177.8(6) . . . . ? C132 C131 C136 C144 -177.6(6) . . . . ? C126 C131 C136 C144 4.6(7) . . . . ? C136 C135 C141 C142 -2.8(14) . . . . ? C134 C135 C141 C142 179.0(9) . . . . ? C135 C141 C142 C143 7.5(17) . . . . ? C141 C142 C143 C144 -9.4(17) . . . . ? C135 C136 C144 C143 -1.2(10) . . . . ? C131 C136 C144 C143 176.4(7) . . . . ? C142 C143 C144 C136 6.3(15) . . . . ? C133 C134 C151 N152 -153(35) . . . . ? C135 C134 C151 N152 34(35) . . . . ? C134 C151 N152 Ag11 -121(34) . . . . ? N152 Ag11 N152 C151 128.2(15) 11_646 . . . ? N152 Ag11 N152 C151 -54.0(19) 6_665 . . . ? N222 Ni21 N211 C212 103.6(5) 6_665 . . . ? N222 Ni21 N211 C212 2.5(3) . . . . ? N222 Ni21 N211 C212 -71(4) 11_646 . . . ? N211 Ni21 N211 C212 -83.2(4) 11_646 . . . ? N211 Ni21 N211 C212 -178.9(3) 6_665 . . . ? N222 Ni21 N211 C216 -72.7(5) 6_665 . . . ? N222 Ni21 N211 C216 -173.7(4) . . . . ? N222 Ni21 N211 C216 112(4) 11_646 . . . ? N211 Ni21 N211 C216 100.6(3) 11_646 . . . ? N211 Ni21 N211 C216 4.8(4) 6_665 . . . ? C216 N211 C212 C223 175.2(6) . . . . ? Ni21 N211 C212 C223 -1.2(5) . . . . ? C216 N211 C212 C213 0.0 . . . . ? Ni21 N211 C212 C213 -176.4(3) . . . . ? C223 C212 C213 C214 -174.8(6) . . . . ? N211 C212 C213 C214 0.0 . . . . ? C212 C213 C214 C215 0.0 . . . . ? C213 C214 C215 C216 0.0 . . . . ? C214 C215 C216 N211 0.0 . . . . ? C212 N211 C216 C215 0.0 . . . . ? Ni21 N211 C216 C215 176.0(4) . . . . ? C226 N221 N222 C223 -169.6(7) . . . . ? C225 N221 N222 C223 0.0 . . . . ? C226 N221 N222 Ni21 6.6(8) . . . . ? C225 N221 N222 Ni21 176.3(6) . . . . ? N222 Ni21 N222 N221 95.87(19) 6_665 . . . ? N222 Ni21 N222 N221 -6.4(6) 11_646 . . . ? N211 Ni21 N222 N221 -179.5(5) . . . . ? N211 Ni21 N222 N221 -83.5(5) 11_646 . . . ? N211 Ni21 N222 N221 168.5(16) 6_665 . . . ? N222 Ni21 N222 C223 -87.9(6) 6_665 . . . ? N222 Ni21 N222 C223 169.8(4) 11_646 . . . ? N211 Ni21 N222 C223 -3.3(3) . . . . ? N211 Ni21 N222 C223 92.7(3) 11_646 . . . ? N211 Ni21 N222 C223 -15.3(19) 6_665 . . . ? N211 C212 C223 C224 179.9(4) . . . . ? C213 C212 C223 C224 -5.0(8) . . . . ? N211 C212 C223 N222 -1.9(7) . . . . ? C213 C212 C223 N222 173.1(4) . . . . ? N221 N222 C223 C212 -178.6(6) . . . . ? Ni21 N222 C223 C212 4.0(6) . . . . ? N221 N222 C223 C224 0.0 . . . . ? Ni21 N222 C223 C224 -177.4(4) . . . . ? C212 C223 C224 C225 178.3(7) . . . . ? N222 C223 C224 C225 0.0 . . . . ? C223 C224 C225 N221 0.0 . . . . ? C226 N221 C225 C224 169.4(7) . . . . ? N222 N221 C225 C224 0.0 . . . . ? N222 N221 C226 C231 87.3(8) . . . . ? C225 N221 C226 C231 -80.4(8) . . . . ? N221 C226 C231 C232 7.0(8) . . . . ? N221 C226 C231 C236 -171.8(5) . . . . ? C236 C231 C232 C233 0.0 . . . . ? C226 C231 C232 C233 -178.8(6) . . . . ? C231 C232 C233 C234 0.0 . . . . ? C232 C233 C234 C235 0.0 . . . . ? C232 C233 C234 C251 179.7(8) . . . . ? C233 C234 C235 C236 0.0 . . . . ? C251 C234 C235 C236 -179.7(8) . . . . ? C233 C234 C235 C241 173.7(7) . . . . ? C251 C234 C235 C241 -6.0(9) . . . . ? C234 C235 C236 C231 0.0 . . . . ? C241 C235 C236 C231 -173.6(7) . . . . ? C234 C235 C236 C244 -177.1(7) . . . . ? C241 C235 C236 C244 9.3(8) . . . . ? C232 C231 C236 C235 0.0 . . . . ? C226 C231 C236 C235 178.8(6) . . . . ? C232 C231 C236 C244 177.1(7) . . . . ? C226 C231 C236 C244 -4.2(7) . . . . ? C234 C235 C241 C242 179.1(8) . . . . ? C236 C235 C241 C242 -7.2(12) . . . . ? C235 C241 C242 C243 3.0(17) . . . . ? C241 C242 C243 C244 -0.9(18) . . . . ? C235 C236 C244 C243 -7.1(12) . . . . ? C231 C236 C244 C243 175.8(8) . . . . ? C242 C243 C244 C236 2.9(17) . . . . ? C233 C234 C251 N252 152(49) . . . . ? C235 C234 C251 N252 -29(50) . . . . ? C234 C251 N252 Ag21 110(49) . . . . ? N252 Ag21 N252 C251 -121.6(18) 5 . . . ? N252 Ag21 N252 C251 56(2) 9 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 5.085 _refine_diff_density_min -0.800 _refine_diff_density_rms 0.189 #===END data_platon _database_code_depnum_ccdc_archive 'CCDC 758094' #TrackingRef 'mixed_metal_networks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H42 Ag B3 Co F12 N12' _chemical_formula_weight 1358.29 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' Co Co 0.3494 0.9721 '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 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 23.0538(10) _cell_length_b 23.0538(10) _cell_length_c 23.0538(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12252.6(9) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7024 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 17.77 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5464 _exptl_absorpt_coefficient_mu 0.676 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8766 _exptl_absorpt_correction_T_max 0.8766 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 102046 _diffrn_reflns_av_R_equivalents 0.1095 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 22.49 _reflns_number_total 5346 _reflns_number_gt 4677 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure is a {[AgCo(L)3](BF4)3}n polymer. The data was solved by direct methods. Hydrogen atoms were included in calculated positions. Data processing was carried out to 45 2theta as the data was only complete to this resolution. Attempts to obtain a better data set were hampered by the weakly diffracting nature of the crystals, presumably due to the large number of voids present in the structure and lattice and the high disorder arising from a combination of fluxional counter-ions solvent molecules. Due to the weakness of the data all six-membered rings have benefitted from geometric restraints. Global displacement restraints have been employed to inprove the model. The occupany of the tertrafluoroborate counter-ions B11 F12 > F15 and B31 F32 > F35 has been reducted to half to bring their thermal parameters in line with those of the other residues. These have been left isotropic. A Platon SQUEEZE function was used to eliminate a void containing disordered counter-ions and solvent molecules. These could not be satisfacturaly modeled and were therefore omitted from the refinement. Only half the required counter-ions could be found from the data. 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 -0.086 -0.086 0.914 326 119 ' ' 2 0.086 0.414 0.586 326 116 ' ' 3 0.206 0.206 0.206 97 23 ' ' 4 0.294 0.794 0.706 97 24 ' ' 5 0.414 0.586 0.086 326 116 ' ' 6 0.586 0.086 0.414 326 118 ' ' 7 0.706 0.294 0.794 97 25 ' ' 8 0.794 0.706 0.294 97 24 ' ' _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^)+(0.2000P)^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 0.10(7) _refine_ls_number_reflns 5346 _refine_ls_number_parameters 435 _refine_ls_number_restraints 449 _refine_ls_R_factor_all 0.1335 _refine_ls_R_factor_gt 0.1259 _refine_ls_wR_factor_ref 0.3570 _refine_ls_wR_factor_gt 0.3498 _refine_ls_goodness_of_fit_ref 1.560 _refine_ls_restrained_S_all 1.509 _refine_ls_shift/su_max 0.001 _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 Ag11 Ag 1.00679(8) 0.49321(8) 1.50679(8) 0.0766(8) Uani 1 3 d S . . Co11 Co 1.12978(7) 0.87022(7) 1.37022(7) 0.0350(8) Uani 1 3 d S . . N111 N 1.1165(4) 0.8658(4) 1.2770(2) 0.0513(14) Uani 1 1 d GU . . C112 C 1.1108(4) 0.9186(3) 1.2485(3) 0.0515(14) Uani 1 1 d GU . . C113 C 1.0980(4) 0.9198(3) 1.1896(3) 0.0519(15) Uani 1 1 d GU . . H113 H 1.0941 0.9559 1.1701 0.062 Uiso 1 1 calc R . . C114 C 1.0908(4) 0.8683(4) 1.1592(2) 0.0521(15) Uani 1 1 d GU . . H114 H 1.0821 0.8691 1.1190 0.063 Uiso 1 1 calc R . . C115 C 1.0965(4) 0.8154(3) 1.1877(3) 0.0520(15) Uani 1 1 d GU . . H115 H 1.0916 0.7802 1.1670 0.062 Uiso 1 1 calc R . . C116 C 1.1094(4) 0.8142(3) 1.2466(3) 0.0517(15) Uani 1 1 d GU . . H116 H 1.1133 0.7781 1.2661 0.062 Uiso 1 1 calc R . . N121 N 1.1346(5) 0.8766(5) 1.5145(5) 0.0483(11) Uani 1 1 d U . . N122 N 1.1562(5) 0.8791(5) 1.4598(5) 0.0474(13) Uani 1 1 d U . . C123 C 1.1136(6) 0.9690(7) 1.2856(6) 0.0513(16) Uani 1 1 d U . . C124 C 1.2271(7) 0.8896(6) 1.5285(6) 0.0484(14) Uani 1 1 d U . . H124 H 1.2639 0.8936 1.5466 0.058 Uiso 1 1 calc R . . C125 C 1.1741(7) 0.8858(6) 1.5539(6) 0.0486(13) Uani 1 1 d U . . H125 H 1.1669 0.8892 1.5944 0.058 Uiso 1 1 calc R . . C126 C 1.0741(7) 0.8634(6) 1.5249(6) 0.0490(11) Uani 1 1 d U . . H12A H 1.0512 0.8771 1.4912 0.059 Uiso 1 1 calc R . . H12B H 1.0611 0.8857 1.5592 0.059 Uiso 1 1 calc R . . C131 C 1.0606(3) 0.8011(2) 1.5347(4) 0.0500(10) Uani 1 1 d GU . . C132 C 1.1063(2) 0.7620(3) 1.5378(4) 0.0504(11) Uani 1 1 d GU . . H132 H 1.1452 0.7755 1.5359 0.061 Uiso 1 1 calc R . . C133 C 1.0952(3) 0.7030(3) 1.5438(4) 0.0513(11) Uani 1 1 d GU . . H133 H 1.1265 0.6763 1.5459 0.062 Uiso 1 1 calc R . . C134 C 1.0383(3) 0.6832(2) 1.5466(4) 0.0522(11) Uani 1 1 d GU . . C135 C 0.9926(2) 0.7223(3) 1.5435(4) 0.0519(11) Uani 1 1 d GDU . . C136 C 1.0037(3) 0.7813(3) 1.5375(4) 0.0512(11) Uani 1 1 d GDU . . C141 C 0.9360(3) 0.7016(3) 1.5462(6) 0.0525(12) Uani 1 1 d DU . . H141 H 0.9291 0.6615 1.5523 0.063 Uiso 1 1 calc R . . C142 C 0.8896(3) 0.7396(4) 1.5399(6) 0.0529(12) Uani 1 1 d DU . . H142 H 0.8510 0.7254 1.5377 0.063 Uiso 1 1 calc R . . C143 C 0.9007(3) 0.7988(4) 1.5369(6) 0.0528(12) Uani 1 1 d DU . . H143 H 0.8693 0.8252 1.5332 0.063 Uiso 1 1 calc R . . C144 C 0.9576(3) 0.8201(2) 1.5392(6) 0.0520(12) Uani 1 1 d DU . . H144 H 0.9645 0.8606 1.5419 0.062 Uiso 1 1 calc R . . C151 C 1.0326(7) 0.6202(7) 1.5529(7) 0.0538(12) Uani 1 1 d U . . N152 N 1.0283(6) 0.5709(5) 1.5578(5) 0.0548(14) Uani 1 1 d U . . Ag21 Ag 1.24084(5) 0.25916(5) 0.74084(5) 0.0528(6) Uani 1 3 d S . . Co21 Co 0.86161(7) 0.13839(7) 0.63839(7) 0.0349(8) Uani 1 3 d S . . N211 N 0.9535(2) 0.1368(3) 0.6474(4) 0.0485(13) Uani 1 1 d GU . . C212 C 0.9807(3) 0.1906(3) 0.6495(4) 0.0486(13) Uani 1 1 d GU . . C213 C 1.0405(3) 0.1940(3) 0.6561(4) 0.0489(14) Uani 1 1 d GU . . H213 H 1.0590 0.2307 0.6575 0.059 Uiso 1 1 calc R . . C214 C 1.0732(2) 0.1435(4) 0.6607(4) 0.0492(14) Uani 1 1 d GU . . H214 H 1.1141 0.1458 0.6653 0.059 Uiso 1 1 calc R . . C215 C 1.0460(3) 0.0897(3) 0.6586(4) 0.0493(14) Uani 1 1 d GU . . H215 H 1.0683 0.0552 0.6617 0.059 Uiso 1 1 calc R . . C216 C 0.9862(3) 0.0864(3) 0.6520(4) 0.0490(14) Uani 1 1 d GU . . H216 H 0.9676 0.0496 0.6505 0.059 Uiso 1 1 calc R . . N221 N 0.8527(5) 0.1401(6) 0.7833(5) 0.0505(12) Uani 1 1 d U . . N222 N 0.8548(5) 0.1150(6) 0.7288(5) 0.0502(14) Uani 1 1 d U . . C223 C 0.9414(6) 0.2391(6) 0.6524(6) 0.0486(14) Uani 1 1 d U . . C224 C 0.9534(7) 0.2978(6) 0.6571(6) 0.0490(15) Uani 1 1 d U . . H224 H 0.9906 0.3152 0.6605 0.059 Uiso 1 1 calc R . . C225 C 0.8440(6) 0.0966(7) 0.8244(6) 0.0502(14) Uani 1 1 d U . . H225 H 0.8396 0.1023 0.8650 0.060 Uiso 1 1 calc R . . C226 C 0.8677(6) 0.2023(7) 0.7897(6) 0.0512(12) Uani 1 1 d U . . H22A H 0.8466 0.2184 0.8234 0.061 Uiso 1 1 calc R . . H22B H 0.8546 0.2234 0.7547 0.061 Uiso 1 1 calc R . . C231 C 0.9341(3) 0.2128(3) 0.7982(4) 0.0518(11) Uani 1 1 d GU . . C232 C 0.9719(3) 0.1659(3) 0.7959(4) 0.0520(12) Uani 1 1 d GU . . H232 H 0.9570 0.1277 0.7921 0.062 Uiso 1 1 calc R . . C233 C 1.0314(3) 0.1750(3) 0.7992(4) 0.0528(12) Uani 1 1 d GU . . H233 H 1.0572 0.1429 0.7976 0.063 Uiso 1 1 calc R . . C234 C 1.0531(2) 0.2310(4) 0.8047(4) 0.0534(11) Uani 1 1 d GU . . C235 C 1.0153(3) 0.2779(3) 0.8070(4) 0.0531(11) Uani 1 1 d GDU . . C236 C 0.9558(3) 0.2688(3) 0.8038(4) 0.0526(11) Uani 1 1 d GDU . . C241 C 1.0381(3) 0.3334(3) 0.8125(6) 0.0535(12) Uani 1 1 d DU . . H241 H 1.0789 0.3388 0.8154 0.064 Uiso 1 1 calc R . . C242 C 1.0013(4) 0.3812(3) 0.8139(6) 0.0538(12) Uani 1 1 d DU . . H242 H 1.0164 0.4195 0.8129 0.065 Uiso 1 1 calc R . . C243 C 0.9419(4) 0.3715(3) 0.8168(6) 0.0537(12) Uani 1 1 d DU . . H243 H 0.9165 0.4029 0.8251 0.064 Uiso 1 1 calc R . . C244 C 0.9188(2) 0.3163(3) 0.8078(6) 0.0531(12) Uani 1 1 d DU . . H244 H 0.8781 0.3112 0.8044 0.064 Uiso 1 1 calc R . . C251 C 1.1138(6) 0.2377(7) 0.8007(6) 0.0545(13) Uani 1 1 d U . . N252 N 1.1661(5) 0.2426(6) 0.7999(5) 0.0554(14) Uani 1 1 d U . . B11 B 0.8090(4) 0.4490(6) 0.7646(5) 0.057(3) Uiso 0.50 1 d PDU . . F12 F 0.8551(7) 0.4865(7) 0.7721(6) 0.067(3) Uiso 0.50 1 d PDU . . F13 F 0.8197(8) 0.4099(6) 0.7206(7) 0.066(3) Uiso 0.50 1 d PDU . . F14 F 0.7992(6) 0.4166(7) 0.8140(6) 0.061(3) Uiso 0.50 1 d PDU . . F15 F 0.7621(6) 0.4840(6) 0.7521(6) 0.054(3) Uiso 0.50 1 d PDU . . B21 B -0.0090(2) 1.0090(2) 0.5090(2) 0.062(3) Uiso 1 3 d SDU . . F22 F -0.0149(4) 0.9842(3) 0.5632(3) 0.076(2) Uiso 1 1 d DU . . F23 F 0.0255(2) 0.9745(2) 0.4745(2) 0.063(3) Uiso 1 3 d SDU . . B31 B 0.9165(4) 0.5835(4) 1.4165(4) 0.062(5) Uiso 0.50 3 d SPDU . . F32 F 0.9295(8) 0.5326(5) 1.3879(5) 0.068(4) Uiso 0.50 1 d PDU . . F33 F 0.8819(4) 0.6181(4) 1.3819(4) 0.070(5) Uiso 0.50 3 d SPDU . . 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 Ag11 0.0766(8) 0.0766(8) 0.0766(8) -0.0168(8) 0.0168(8) -0.0168(8) Co11 0.0350(8) 0.0350(8) 0.0350(8) 0.0024(8) -0.0024(8) -0.0024(8) N111 0.040(3) 0.074(4) 0.040(3) -0.006(2) 0.013(3) -0.010(3) C112 0.040(3) 0.074(4) 0.040(3) -0.006(2) 0.012(3) -0.009(3) C113 0.040(3) 0.075(4) 0.040(3) -0.006(2) 0.012(3) -0.009(3) C114 0.040(3) 0.076(4) 0.040(3) -0.007(2) 0.012(3) -0.009(3) C115 0.040(3) 0.075(4) 0.041(3) -0.007(3) 0.012(3) -0.009(3) C116 0.040(3) 0.075(4) 0.040(3) -0.007(3) 0.012(3) -0.009(3) N121 0.058(2) 0.045(2) 0.042(2) 0.002(2) -0.007(2) -0.003(2) N122 0.057(3) 0.044(3) 0.042(2) 0.002(3) -0.007(2) -0.003(2) C123 0.040(3) 0.074(4) 0.040(3) -0.006(3) 0.013(3) -0.010(3) C124 0.058(3) 0.045(3) 0.042(3) 0.002(3) -0.008(2) -0.003(3) C125 0.059(3) 0.045(3) 0.042(3) 0.002(2) -0.007(2) -0.003(2) C126 0.059(2) 0.046(2) 0.042(2) 0.000(2) -0.005(2) -0.003(2) C131 0.060(2) 0.047(2) 0.043(2) -0.001(2) -0.003(2) -0.0032(18) C132 0.061(2) 0.047(2) 0.044(2) -0.001(2) -0.003(2) -0.0027(19) C133 0.062(2) 0.047(2) 0.045(2) -0.001(2) -0.004(2) -0.003(2) C134 0.062(2) 0.048(2) 0.046(2) -0.002(2) -0.003(2) -0.0038(19) C135 0.061(2) 0.048(2) 0.046(2) -0.002(2) -0.002(2) -0.0041(19) C136 0.060(2) 0.048(2) 0.045(2) -0.002(2) -0.003(2) -0.0038(18) C141 0.062(2) 0.050(2) 0.046(2) -0.003(2) -0.002(2) -0.005(2) C142 0.061(2) 0.051(2) 0.047(2) -0.003(2) -0.001(2) -0.004(2) C143 0.061(2) 0.051(2) 0.047(2) -0.003(2) -0.001(2) -0.004(2) C144 0.061(2) 0.049(2) 0.046(2) -0.003(2) -0.002(2) -0.003(2) C151 0.064(3) 0.048(2) 0.049(3) -0.002(2) -0.003(2) -0.004(2) N152 0.065(3) 0.048(2) 0.051(3) -0.002(3) -0.004(3) -0.005(3) Ag21 0.0528(6) 0.0528(6) 0.0528(6) -0.0035(5) 0.0035(5) -0.0035(5) Co21 0.0349(8) 0.0349(8) 0.0349(8) -0.0025(7) 0.0025(7) 0.0025(7) N211 0.046(3) 0.053(3) 0.046(3) 0.007(3) -0.006(2) -0.004(2) C212 0.047(3) 0.053(3) 0.046(3) 0.007(3) -0.006(2) -0.004(2) C213 0.047(3) 0.054(3) 0.046(3) 0.007(3) -0.005(3) -0.004(2) C214 0.047(3) 0.054(3) 0.047(3) 0.007(3) -0.005(3) -0.004(2) C215 0.047(3) 0.054(3) 0.047(3) 0.007(3) -0.005(3) -0.003(2) C216 0.047(3) 0.053(3) 0.047(3) 0.006(3) -0.005(3) -0.003(2) N221 0.043(2) 0.068(3) 0.040(2) 0.001(2) 0.002(2) -0.009(2) N222 0.043(3) 0.068(3) 0.040(3) 0.001(2) 0.002(3) -0.008(3) C223 0.048(3) 0.053(3) 0.045(3) 0.008(3) -0.007(3) -0.004(2) C224 0.048(3) 0.053(3) 0.046(3) 0.007(3) -0.008(3) -0.005(3) C225 0.043(3) 0.068(3) 0.040(3) 0.001(2) 0.002(3) -0.009(3) C226 0.044(2) 0.068(3) 0.041(2) 0.000(2) 0.002(2) -0.009(2) C231 0.045(2) 0.069(3) 0.042(2) 0.001(2) 0.002(2) -0.0098(19) C232 0.045(2) 0.069(3) 0.042(2) 0.002(2) 0.002(2) -0.010(2) C233 0.045(2) 0.070(3) 0.043(2) 0.002(2) 0.002(2) -0.010(2) C234 0.046(2) 0.070(3) 0.044(2) 0.001(2) 0.002(2) -0.0103(19) C235 0.046(2) 0.069(3) 0.044(2) 0.001(2) 0.003(2) -0.0104(19) C236 0.046(2) 0.069(3) 0.043(2) 0.001(2) 0.003(2) -0.0098(19) C241 0.047(2) 0.069(3) 0.044(2) 0.001(2) 0.003(2) -0.011(2) C242 0.048(2) 0.069(3) 0.045(3) 0.002(2) 0.003(2) -0.010(2) C243 0.048(2) 0.069(3) 0.044(3) 0.001(2) 0.003(2) -0.010(2) C244 0.047(2) 0.069(3) 0.043(2) 0.001(2) 0.003(2) -0.009(2) C251 0.046(2) 0.071(3) 0.046(3) 0.001(2) 0.002(2) -0.010(2) N252 0.047(2) 0.072(3) 0.047(3) 0.001(3) 0.002(3) -0.010(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 Ag11 N152 2.200(12) . ? Ag11 N152 2.200(12) 12_675 ? Ag11 N152 2.200(12) 6_467 ? Co11 N122 2.162(11) . ? Co11 N122 2.162(12) 7_775 ? Co11 N122 2.162(11) 10_747 ? Co11 N111 2.172(6) . ? Co11 N111 2.172(6) 7_775 ? Co11 N111 2.172(6) 10_747 ? N111 C112 1.3900 . ? N111 C116 1.3900 . ? C112 C113 1.3900 . ? C112 C123 1.444(17) . ? C113 C114 1.3900 . ? C113 H113 0.9500 . ? C114 C115 1.3900 . ? C114 H114 0.9500 . ? C115 C116 1.3900 . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? N121 C125 1.305(18) . ? N121 N122 1.356(16) . ? N121 C126 1.448(19) . ? N122 C123 1.370(19) 7_775 ? C123 N122 1.370(18) 10_747 ? C123 C124 1.40(2) 10_747 ? C124 C125 1.36(2) . ? C124 C123 1.40(2) 7_775 ? C124 H124 0.9500 . ? C125 H125 0.9500 . ? C126 C131 1.487(15) . ? C126 H12A 0.9900 . ? C126 H12B 0.9900 . ? C131 C132 1.3900 . ? C131 C136 1.3900 . ? C132 C133 1.3900 . ? C132 H132 0.9500 . ? C133 C134 1.3900 . ? C133 H133 0.9500 . ? C134 C135 1.3900 . ? C134 C151 1.465(16) . ? C135 C136 1.3900 . ? C135 C141 1.3900(10) . ? C136 C144 1.3900(10) . ? C141 C142 1.3900(10) . ? C141 H141 0.9500 . ? C142 C143 1.3900(10) . ? C142 H142 0.9500 . ? C143 C144 1.400(4) . ? C143 H143 0.9500 . ? C144 H144 0.9500 . ? C151 N152 1.146(18) . ? Ag21 N252 2.229(12) 6_566 ? Ag21 N252 2.229(12) 12_664 ? Ag21 N252 2.229(12) . ? Co21 N211 2.129(6) 7_665 ? Co21 N211 2.129(6) . ? Co21 N211 2.129(6) 10_646 ? Co21 N222 2.158(12) 10_646 ? Co21 N222 2.158(12) 7_665 ? Co21 N222 2.158(12) . ? N211 C212 1.3900 . ? N211 C216 1.3900 . ? C212 C213 1.3900 . ? C212 C223 1.439(16) . ? C213 C214 1.3900 . ? C213 H213 0.9500 . ? C214 C215 1.3900 . ? C214 H214 0.9500 . ? C215 C216 1.3900 . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? N221 N222 1.386(17) . ? N221 C225 1.395(19) . ? N221 C226 1.48(2) . ? N222 C223 1.331(19) 7_665 ? C223 N222 1.331(19) 10_646 ? C223 C224 1.39(2) . ? C224 C225 1.31(2) 10_646 ? C224 H224 0.9500 . ? C225 C224 1.31(2) 7_665 ? C225 H225 0.9500 . ? C226 C231 1.561(15) . ? C226 H22A 0.9900 . ? C226 H22B 0.9900 . ? C231 C232 1.3900 . ? C231 C236 1.3900 . ? C232 C233 1.3900 . ? C232 H232 0.9500 . ? C233 C234 1.3900 . ? C233 H233 0.9500 . ? C234 C235 1.3900 . ? C234 C251 1.410(16) . ? C235 C236 1.3900 . ? C235 C241 1.3902(10) . ? C236 C244 1.3902(10) . ? C241 C242 1.3900(10) . ? C241 H241 0.9500 . ? C242 C243 1.3900(10) . ? C242 H242 0.9500 . ? C243 C244 1.394(3) . ? C243 H243 0.9500 . ? C244 H244 0.9500 . ? C251 N252 1.213(18) . ? B11 F13 1.380(2) . ? B11 F15 1.380(2) . ? B11 F14 1.380(2) . ? B11 F12 1.380(2) . ? B21 F23 1.380(2) . ? B21 F22 1.3812(19) 10_655 ? B21 F22 1.3812(19) 7_564 ? B21 F22 1.3812(19) . ? B31 F32 1.380(2) 12_675 ? B31 F32 1.380(2) . ? B31 F32 1.380(2) 6_467 ? B31 F33 1.380(2) . ? 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 N152 Ag11 N152 119.90(4) . 12_675 ? N152 Ag11 N152 119.90(4) . 6_467 ? N152 Ag11 N152 119.90(4) 12_675 6_467 ? N122 Co11 N122 101.8(4) . 7_775 ? N122 Co11 N122 101.8(4) . 10_747 ? N122 Co11 N122 101.8(4) 7_775 10_747 ? N122 Co11 N111 171.2(4) . . ? N122 Co11 N111 86.9(4) 7_775 . ? N122 Co11 N111 75.7(4) 10_747 . ? N122 Co11 N111 75.7(4) . 7_775 ? N122 Co11 N111 171.2(4) 7_775 7_775 ? N122 Co11 N111 86.9(4) 10_747 7_775 ? N111 Co11 N111 95.7(3) . 7_775 ? N122 Co11 N111 86.9(4) . 10_747 ? N122 Co11 N111 75.7(4) 7_775 10_747 ? N122 Co11 N111 171.2(4) 10_747 10_747 ? N111 Co11 N111 95.7(3) . 10_747 ? N111 Co11 N111 95.7(3) 7_775 10_747 ? C112 N111 C116 120.0 . . ? C112 N111 Co11 116.1(4) . . ? C116 N111 Co11 123.7(4) . . ? C113 C112 N111 120.0 . . ? C113 C112 C123 124.8(8) . . ? N111 C112 C123 114.9(8) . . ? C112 C113 C114 120.0 . . ? C112 C113 H113 120.0 . . ? C114 C113 H113 120.0 . . ? C115 C114 C113 120.0 . . ? C115 C114 H114 120.0 . . ? C113 C114 H114 120.0 . . ? C114 C115 C116 120.0 . . ? C114 C115 H115 120.0 . . ? C116 C115 H115 120.0 . . ? C115 C116 N111 120.0 . . ? C115 C116 H116 120.0 . . ? N111 C116 H116 120.0 . . ? C125 N121 N122 112.7(12) . . ? C125 N121 C126 126.3(12) . . ? N122 N121 C126 121.1(11) . . ? N121 N122 C123 102.7(12) . 7_775 ? N121 N122 Co11 141.3(9) . . ? C123 N122 Co11 115.9(10) 7_775 . ? N122 C123 C124 111.3(13) 10_747 10_747 ? N122 C123 C112 117.4(13) 10_747 . ? C124 C123 C112 131.4(13) 10_747 . ? C125 C124 C123 103.4(13) . 7_775 ? C125 C124 H124 128.3 . . ? C123 C124 H124 128.3 7_775 . ? N121 C125 C124 109.7(13) . . ? N121 C125 H125 125.1 . . ? C124 C125 H125 125.1 . . ? N121 C126 C131 115.4(11) . . ? N121 C126 H12A 108.4 . . ? C131 C126 H12A 108.4 . . ? N121 C126 H12B 108.4 . . ? C131 C126 H12B 108.4 . . ? H12A C126 H12B 107.5 . . ? C132 C131 C136 120.0 . . ? C132 C131 C126 118.4(8) . . ? C136 C131 C126 121.5(8) . . ? C131 C132 C133 120.0 . . ? C131 C132 H132 120.0 . . ? C133 C132 H132 120.0 . . ? C134 C133 C132 120.0 . . ? C134 C133 H133 120.0 . . ? C132 C133 H133 120.0 . . ? C133 C134 C135 120.0 . . ? C133 C134 C151 114.5(8) . . ? C135 C134 C151 125.5(8) . . ? C134 C135 C136 120.0 . . ? C134 C135 C141 119.1(5) . . ? C136 C135 C141 120.9(5) . . ? C144 C136 C135 119.0(5) . . ? C144 C136 C131 120.8(5) . . ? C135 C136 C131 120.0 . . ? C142 C141 C135 120.04(13) . . ? C142 C141 H141 120.0 . . ? C135 C141 H141 120.0 . . ? C141 C142 C143 118.8(5) . . ? C141 C142 H142 120.6 . . ? C143 C142 H142 120.6 . . ? C142 C143 C144 121.0(5) . . ? C142 C143 H143 119.5 . . ? C144 C143 H143 119.5 . . ? C136 C144 C143 119.3(2) . . ? C136 C144 H144 120.3 . . ? C143 C144 H144 120.3 . . ? N152 C151 C134 180(2) . . ? C151 N152 Ag11 140.7(12) . . ? N252 Ag21 N252 119.997(6) 6_566 12_664 ? N252 Ag21 N252 119.997(7) 6_566 . ? N252 Ag21 N252 119.997(7) 12_664 . ? N211 Co21 N211 94.7(3) 7_665 . ? N211 Co21 N211 94.7(3) 7_665 10_646 ? N211 Co21 N211 94.7(3) . 10_646 ? N211 Co21 N222 170.5(4) 7_665 10_646 ? N211 Co21 N222 76.1(4) . 10_646 ? N211 Co21 N222 88.5(4) 10_646 10_646 ? N211 Co21 N222 88.5(4) 7_665 7_665 ? N211 Co21 N222 170.5(4) . 7_665 ? N211 Co21 N222 76.1(4) 10_646 7_665 ? N222 Co21 N222 100.9(4) 10_646 7_665 ? N211 Co21 N222 76.1(4) 7_665 . ? N211 Co21 N222 88.5(4) . . ? N211 Co21 N222 170.5(4) 10_646 . ? N222 Co21 N222 100.9(4) 10_646 . ? N222 Co21 N222 100.9(4) 7_665 . ? C212 N211 C216 120.0 . . ? C212 N211 Co21 115.9(4) . . ? C216 N211 Co21 124.1(4) . . ? N211 C212 C213 120.0 . . ? N211 C212 C223 114.2(8) . . ? C213 C212 C223 125.2(8) . . ? C214 C213 C212 120.0 . . ? C214 C213 H213 120.0 . . ? C212 C213 H213 120.0 . . ? C213 C214 C215 120.0 . . ? C213 C214 H214 120.0 . . ? C215 C214 H214 120.0 . . ? C216 C215 C214 120.0 . . ? C216 C215 H215 120.0 . . ? C214 C215 H215 120.0 . . ? C215 C216 N211 120.0 . . ? C215 C216 H216 120.0 . . ? N211 C216 H216 120.0 . . ? N222 N221 C225 108.7(12) . . ? N222 N221 C226 119.1(11) . . ? C225 N221 C226 131.5(12) . . ? C223 N222 N221 104.0(11) 7_665 . ? C223 N222 Co21 115.2(10) 7_665 . ? N221 N222 Co21 140.7(10) . . ? N222 C223 C224 112.3(13) 10_646 . ? N222 C223 C212 118.0(12) 10_646 . ? C224 C223 C212 129.5(13) . . ? C225 C224 C223 106.3(14) 10_646 . ? C225 C224 H224 126.8 10_646 . ? C223 C224 H224 126.8 . . ? C224 C225 N221 108.6(14) 7_665 . ? C224 C225 H225 125.7 7_665 . ? N221 C225 H225 125.7 . . ? N221 C226 C231 113.1(12) . . ? N221 C226 H22A 109.0 . . ? C231 C226 H22A 109.0 . . ? N221 C226 H22B 109.0 . . ? C231 C226 H22B 109.0 . . ? H22A C226 H22B 107.8 . . ? C232 C231 C236 120.0 . . ? C232 C231 C226 119.2(8) . . ? C236 C231 C226 120.6(8) . . ? C231 C232 C233 120.0 . . ? C231 C232 H232 120.0 . . ? C233 C232 H232 120.0 . . ? C234 C233 C232 120.0 . . ? C234 C233 H233 120.0 . . ? C232 C233 H233 120.0 . . ? C233 C234 C235 120.0 . . ? C233 C234 C251 116.9(9) . . ? C235 C234 C251 122.6(9) . . ? C234 C235 C236 120.0 . . ? C234 C235 C241 118.9(5) . . ? C236 C235 C241 121.1(5) . . ? C235 C236 C231 120.0 . . ? C235 C236 C244 118.8(5) . . ? C231 C236 C244 121.1(5) . . ? C242 C241 C235 120.01(13) . . ? C242 C241 H241 120.0 . . ? C235 C241 H241 120.0 . . ? C243 C242 C241 118.4(5) . . ? C243 C242 H242 120.8 . . ? C241 C242 H242 120.8 . . ? C242 C243 C244 120.9(5) . . ? C242 C243 H243 119.5 . . ? C244 C243 H243 119.5 . . ? C236 C244 C243 119.73(18) . . ? C236 C244 H244 120.1 . . ? C243 C244 H244 120.1 . . ? N252 C251 C234 177.0(15) . . ? C251 N252 Ag21 142.6(11) . . ? F13 B11 F15 111.6(13) . . ? F13 B11 F14 106.4(14) . . ? F15 B11 F14 111.2(6) . . ? F13 B11 F12 111.2(6) . . ? F15 B11 F12 105.3(14) . . ? F14 B11 F12 111.2(6) . . ? F23 B21 F22 109.8(2) . 10_655 ? F23 B21 F22 109.8(2) . 7_564 ? F22 B21 F22 109.1(2) 10_655 7_564 ? F23 B21 F22 109.8(2) . . ? F22 B21 F22 109.1(2) 10_655 . ? F22 B21 F22 109.1(2) 7_564 . ? F32 B31 F32 109.0(2) 12_675 . ? F32 B31 F32 109.0(2) 12_675 6_467 ? F32 B31 F32 109.0(2) . 6_467 ? F32 B31 F33 109.9(2) 12_675 . ? F32 B31 F33 109.9(2) . . ? F32 B31 F33 109.9(2) 6_467 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N122 Co11 N111 C112 -73(3) . . . . ? N122 Co11 N111 C112 104.5(5) 7_775 . . . ? N122 Co11 N111 C112 1.5(5) 10_747 . . . ? N111 Co11 N111 C112 -83.8(6) 7_775 . . . ? N111 Co11 N111 C112 179.8(5) 10_747 . . . ? N122 Co11 N111 C116 112(3) . . . . ? N122 Co11 N111 C116 -70.6(6) 7_775 . . . ? N122 Co11 N111 C116 -173.6(6) 10_747 . . . ? N111 Co11 N111 C116 101.1(4) 7_775 . . . ? N111 Co11 N111 C116 4.7(6) 10_747 . . . ? C116 N111 C112 C113 0.0 . . . . ? Co11 N111 C112 C113 -175.3(5) . . . . ? C116 N111 C112 C123 174.2(9) . . . . ? Co11 N111 C112 C123 -1.0(9) . . . . ? N111 C112 C113 C114 0.0 . . . . ? C123 C112 C113 C114 -173.6(10) . . . . ? C112 C113 C114 C115 0.0 . . . . ? C113 C114 C115 C116 0.0 . . . . ? C114 C115 C116 N111 0.0 . . . . ? C112 N111 C116 C115 0.0 . . . . ? Co11 N111 C116 C115 174.9(6) . . . . ? C125 N121 N122 C123 4.6(15) . . . 7_775 ? C126 N121 N122 C123 -174.0(12) . . . 7_775 ? C125 N121 N122 Co11 179.3(11) . . . . ? C126 N121 N122 Co11 1(2) . . . . ? N122 Co11 N122 N121 -4.7(15) 7_775 . . . ? N122 Co11 N122 N121 100.2(11) 10_747 . . . ? N111 Co11 N122 N121 173(2) . . . . ? N111 Co11 N122 N121 -176.1(14) 7_775 . . . ? N111 Co11 N122 N121 -79.4(14) 10_747 . . . ? N122 Co11 N122 C123 169.6(9) 7_775 . . 7_775 ? N122 Co11 N122 C123 -85.5(12) 10_747 . . 7_775 ? N111 Co11 N122 C123 -13(3) . . . 7_775 ? N111 Co11 N122 C123 -1.8(9) 7_775 . . 7_775 ? N111 Co11 N122 C123 94.9(10) 10_747 . . 7_775 ? C113 C112 C123 N122 173.4(9) . . . 10_747 ? N111 C112 C123 N122 -0.6(15) . . . 10_747 ? C113 C112 C123 C124 -6.9(19) . . . 10_747 ? N111 C112 C123 C124 179.1(13) . . . 10_747 ? N122 N121 C125 C124 -6.0(16) . . . . ? C126 N121 C125 C124 172.5(13) . . . . ? C123 C124 C125 N121 4.6(16) 7_775 . . . ? C125 N121 C126 C131 -85.6(17) . . . . ? N122 N121 C126 C131 92.9(14) . . . . ? N121 C126 C131 C132 5.1(14) . . . . ? N121 C126 C131 C136 -171.4(9) . . . . ? C136 C131 C132 C133 0.0 . . . . ? C126 C131 C132 C133 -176.5(10) . . . . ? C131 C132 C133 C134 0.0 . . . . ? C132 C133 C134 C135 0.0 . . . . ? C132 C133 C134 C151 179.9(10) . . . . ? C133 C134 C135 C136 0.0 . . . . ? C151 C134 C135 C136 -179.9(11) . . . . ? C133 C134 C135 C141 179.7(11) . . . . ? C151 C134 C135 C141 -0.2(12) . . . . ? C134 C135 C136 C144 -174.8(11) . . . . ? C141 C135 C136 C144 5.4(13) . . . . ? C134 C135 C136 C131 0.0 . . . . ? C141 C135 C136 C131 -179.7(11) . . . . ? C132 C131 C136 C144 174.7(11) . . . . ? C126 C131 C136 C144 -8.8(12) . . . . ? C132 C131 C136 C135 0.0 . . . . ? C126 C131 C136 C135 176.4(10) . . . . ? C134 C135 C141 C142 -176.4(11) . . . . ? C136 C135 C141 C142 3.3(17) . . . . ? C135 C141 C142 C143 -6(2) . . . . ? C141 C142 C143 C144 1(2) . . . . ? C135 C136 C144 C143 -10.8(17) . . . . ? C131 C136 C144 C143 174.4(10) . . . . ? C142 C143 C144 C136 8(2) . . . . ? C133 C134 C151 N152 26(100) . . . . ? C135 C134 C151 N152 -154(100) . . . . ? C134 C151 N152 Ag11 -130(100) . . . . ? N152 Ag11 N152 C151 -115.7(19) 12_675 . . . ? N152 Ag11 N152 C151 58(2) 6_467 . . . ? N211 Co21 N211 C212 179.0(4) 7_665 . . . ? N211 Co21 N211 C212 83.9(6) 10_646 . . . ? N222 Co21 N211 C212 -3.4(5) 10_646 . . . ? N222 Co21 N211 C212 70(3) 7_665 . . . ? N222 Co21 N211 C212 -105.1(6) . . . . ? N211 Co21 N211 C216 -2.0(6) 7_665 . . . ? N211 Co21 N211 C216 -97.1(4) 10_646 . . . ? N222 Co21 N211 C216 175.6(6) 10_646 . . . ? N222 Co21 N211 C216 -111(2) 7_665 . . . ? N222 Co21 N211 C216 74.0(6) . . . . ? C216 N211 C212 C213 0.0 . . . . ? Co21 N211 C212 C213 179.1(6) . . . . ? C216 N211 C212 C223 -171.8(10) . . . . ? Co21 N211 C212 C223 7.3(9) . . . . ? N211 C212 C213 C214 0.0 . . . . ? C223 C212 C213 C214 170.8(11) . . . . ? C212 C213 C214 C215 0.0 . . . . ? C213 C214 C215 C216 0.0 . . . . ? C214 C215 C216 N211 0.0 . . . . ? C212 N211 C216 C215 0.0 . . . . ? Co21 N211 C216 C215 -179.0(6) . . . . ? C225 N221 N222 C223 -0.2(14) . . . 7_665 ? C226 N221 N222 C223 171.1(12) . . . 7_665 ? C225 N221 N222 Co21 176.0(11) . . . . ? C226 N221 N222 Co21 -13(2) . . . . ? N211 Co21 N222 C223 -1.2(9) 7_665 . . 7_665 ? N211 Co21 N222 C223 -96.4(10) . . . 7_665 ? N211 Co21 N222 C223 14(3) 10_646 . . 7_665 ? N222 Co21 N222 C223 -172.0(9) 10_646 . . 7_665 ? N222 Co21 N222 C223 84.5(12) 7_665 . . 7_665 ? N211 Co21 N222 N221 -177.1(15) 7_665 . . . ? N211 Co21 N222 N221 87.7(14) . . . . ? N211 Co21 N222 N221 -162.4(19) 10_646 . . . ? N222 Co21 N222 N221 12.1(15) 10_646 . . . ? N222 Co21 N222 N221 -91.4(11) 7_665 . . . ? N211 C212 C223 N222 -8.6(15) . . . 10_646 ? C213 C212 C223 N222 -179.9(9) . . . 10_646 ? N211 C212 C223 C224 177.3(13) . . . . ? C213 C212 C223 C224 6(2) . . . . ? N222 C223 C224 C225 3.4(18) 10_646 . . 10_646 ? C212 C223 C224 C225 177.8(13) . . . 10_646 ? N222 N221 C225 C224 2.3(16) . . . 7_665 ? C226 N221 C225 C224 -167.6(14) . . . 7_665 ? N222 N221 C226 C231 -86.7(14) . . . . ? C225 N221 C226 C231 82.3(18) . . . . ? N221 C226 C231 C232 3.5(14) . . . . ? N221 C226 C231 C236 178.8(8) . . . . ? C236 C231 C232 C233 0.0 . . . . ? C226 C231 C232 C233 175.3(10) . . . . ? C231 C232 C233 C234 0.0 . . . . ? C232 C233 C234 C235 0.0 . . . . ? C232 C233 C234 C251 -172.5(10) . . . . ? C233 C234 C235 C236 0.0 . . . . ? C251 C234 C235 C236 172.1(11) . . . . ? C233 C234 C235 C241 -179.9(11) . . . . ? C251 C234 C235 C241 -7.8(12) . . . . ? C234 C235 C236 C231 0.0 . . . . ? C241 C235 C236 C231 179.9(11) . . . . ? C234 C235 C236 C244 178.3(11) . . . . ? C241 C235 C236 C244 -1.8(13) . . . . ? C232 C231 C236 C235 0.0 . . . . ? C226 C231 C236 C235 -175.2(10) . . . . ? C232 C231 C236 C244 -178.2(11) . . . . ? C226 C231 C236 C244 6.6(12) . . . . ? C234 C235 C241 C242 178.9(11) . . . . ? C236 C235 C241 C242 -1.1(17) . . . . ? C235 C241 C242 C243 8(2) . . . . ? C241 C242 C243 C244 -12(2) . . . . ? C235 C236 C244 C243 -2.1(17) . . . . ? C231 C236 C244 C243 176.1(10) . . . . ? C242 C243 C244 C236 9(2) . . . . ? C233 C234 C251 N252 -79(33) . . . . ? C235 C234 C251 N252 109(33) . . . . ? C234 C251 N252 Ag21 170(32) . . . . ? N252 Ag21 N252 C251 122.2(19) 6_566 . . . ? N252 Ag21 N252 C251 -59(2) 12_664 . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 5.727 _refine_diff_density_min -1.286 _refine_diff_density_rms 0.192 #===END data_imw1310r-3 _database_code_depnum_ccdc_archive 'CCDC 758095' #TrackingRef 'mixed_metal_networks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H36 Ag B3 F12 N12 Ni' _chemical_formula_weight 1207.90 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' Ni Ni 0.3393 1.1124 '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 Hexagonal _symmetry_space_group_name_H-M 'R-3 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 17.8044(4) _cell_length_b 17.8044(4) _cell_length_c 37.1701(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10204.2(4) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6763 _cell_measurement_theta_min 2.289 _cell_measurement_theta_max 23.900 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3636 _exptl_absorpt_coefficient_mu 0.634 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8837 _exptl_absorpt_correction_T_max 0.9109 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33761 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5210 _reflns_number_gt 4031 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure is a {[AgNi(L)3](BF4)3}n polymer. The data was solved by direct methods. Hydrogen atoms were included in calculated positions. Attempts to obtain a better data set were hampered by the weakly diffracting nature of the crystals, presumably due to the large number of voids present in the structure and lattice and the high disorder arising from a combination of fluxional counter- ions solvent molecules. The tertrafluoroborate counter-ion B11 F12 > F15 is fully disordered over two sites (44:56) and has benefitted from the application of geometric and displacement restraints. A Platon SQUEEZE function was used to eliminate voids containing disordered solvent molecules. These could not be satisfactorily modelled and were therefore omitted from the refinement. The electron count per void is high but this is not surprising given the size of the voids present. 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 -0.021 0.462 0.000 1100 252 ' ' 2 -0.007 -0.004 0.333 1106 252 ' ' 3 -0.041 0.866 0.667 1105 253 ' ' _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^)+(0.2000P)^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_number_reflns 5210 _refine_ls_number_parameters 278 _refine_ls_number_restraints 228 _refine_ls_R_factor_all 0.1240 _refine_ls_R_factor_gt 0.1087 _refine_ls_wR_factor_ref 0.3515 _refine_ls_wR_factor_gt 0.3365 _refine_ls_goodness_of_fit_ref 1.451 _refine_ls_restrained_S_all 1.457 _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 Ag1 Ag 0.3333 0.6667 0.11735(4) 0.0718(5) Uani 1 3 d S . . Ni1 Ni 0.0000 1.0000 0.11457(3) 0.0232(3) Uani 1 3 d S . . N11 N 0.0697(3) 1.1129(3) 0.08329(11) 0.0301(9) Uani 1 1 d . . . C12 C 0.0575(3) 1.1782(3) 0.09214(13) 0.0324(10) Uani 1 1 d . . . C13 C 0.0925(4) 1.2547(4) 0.07196(15) 0.0422(13) Uani 1 1 d . . . H13 H 0.0832 1.3007 0.0790 0.051 Uiso 1 1 calc R . . C14 C 0.1410(5) 1.2625(4) 0.04150(17) 0.0533(16) Uani 1 1 d . . . H14 H 0.1648 1.3134 0.0271 0.064 Uiso 1 1 calc R . . C15 C 0.1538(4) 1.1939(4) 0.03261(17) 0.0504(15) Uani 1 1 d . . . H15 H 0.1860 1.1970 0.0117 0.060 Uiso 1 1 calc R . . C16 C 0.1195(4) 1.1215(4) 0.05429(13) 0.0374(12) Uani 1 1 d . . . H16 H 0.1310 1.0762 0.0487 0.045 Uiso 1 1 calc R . . N21 N -0.0970(3) 0.8400(3) 0.17163(12) 0.0336(9) Uani 1 1 d . . . N22 N -0.0903(2) 0.8862(2) 0.14154(11) 0.0278(8) Uani 1 1 d . . . C23 C -0.1660(3) 0.8416(3) 0.12464(14) 0.0308(10) Uani 1 1 d . . . C24 C -0.2213(3) 0.7666(3) 0.14425(15) 0.0360(11) Uani 1 1 d . . . H24 H -0.2792 0.7243 0.1383 0.043 Uiso 1 1 calc R . . C25 C -0.1759(4) 0.7668(4) 0.17299(17) 0.0429(13) Uani 1 1 d . . . H25 H -0.1955 0.7234 0.1911 0.051 Uiso 1 1 calc R . . C26 C -0.0232(4) 0.8585(4) 0.19359(14) 0.0375(12) Uani 1 1 d . . . H26A H -0.0437 0.8347 0.2180 0.045 Uiso 1 1 calc R . . H26B H 0.0139 0.9222 0.1959 0.045 Uiso 1 1 calc R . . C31 C 0.0304(4) 0.8223(3) 0.17932(15) 0.0375(12) Uani 1 1 d . . . C32 C 0.0110(4) 0.7775(4) 0.14700(15) 0.0389(12) Uani 1 1 d . . . H32 H -0.0375 0.7689 0.1331 0.047 Uiso 1 1 calc R . . C33 C 0.0641(4) 0.7448(4) 0.13502(19) 0.0441(13) Uani 1 1 d . . . H33 H 0.0523 0.7147 0.1128 0.053 Uiso 1 1 calc R . . C34 C 0.1326(4) 0.7566(4) 0.1556(2) 0.0538(17) Uani 1 1 d . . . C35 C 0.1511(4) 0.7994(5) 0.1892(2) 0.0595(18) Uani 1 1 d . . . H35 H 0.1984 0.8059 0.2033 0.071 Uiso 1 1 calc R . . C36 C 0.0994(4) 0.8317(5) 0.20120(19) 0.0541(16) Uani 1 1 d . . . H36 H 0.1101 0.8599 0.2239 0.065 Uiso 1 1 calc R . . C41 C 0.1881(4) 0.7243(5) 0.1418(3) 0.0618(19) Uani 1 1 d . . . N42 N 0.2300(5) 0.6982(5) 0.1315(3) 0.081(2) Uani 1 1 d . . . B11X B 0.3606(6) 0.1727(8) 0.0552(2) 0.0984(16) Uani 0.442(7) 1 d PDU A 1 F12X F 0.3705(9) 0.2355(8) 0.0307(3) 0.1017(18) Uani 0.442(7) 1 d PDU A 1 F13X F 0.3437(9) 0.1917(11) 0.0892(3) 0.1021(19) Uani 0.442(7) 1 d PDU A 1 F14X F 0.2947(9) 0.0931(9) 0.0435(5) 0.0987(19) Uani 0.442(7) 1 d PDU A 1 F15X F 0.4372(7) 0.1711(10) 0.0567(3) 0.1013(16) Uani 0.442(7) 1 d PDU A 1 B11Y B 0.3554(5) 0.1635(6) 0.0570(2) 0.0978(15) Uani 0.558(7) 1 d PDU A 2 F12Y F 0.4108(6) 0.2112(8) 0.0295(2) 0.1033(18) Uani 0.558(7) 1 d PDU A 2 F13Y F 0.3386(8) 0.2177(8) 0.0779(3) 0.1010(17) Uani 0.558(7) 1 d PDU A 2 F14Y F 0.3881(7) 0.1219(7) 0.0777(2) 0.1015(17) Uani 0.558(7) 1 d PDU A 2 F15Y F 0.2793(7) 0.0986(8) 0.0423(4) 0.0973(19) Uani 0.558(7) 1 d PDU A 2 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 0.0388(4) 0.0388(4) 0.1378(11) 0.000 0.000 0.0194(2) Ni1 0.0224(4) 0.0224(4) 0.0247(5) 0.000 0.000 0.0112(2) N11 0.028(2) 0.029(2) 0.030(2) 0.0070(15) 0.0007(15) 0.0124(17) C12 0.029(2) 0.029(2) 0.033(2) 0.0008(19) -0.0080(19) 0.011(2) C13 0.053(3) 0.032(3) 0.039(3) 0.006(2) 0.002(2) 0.019(2) C14 0.066(4) 0.040(3) 0.046(3) 0.015(3) 0.009(3) 0.021(3) C15 0.057(4) 0.049(3) 0.041(3) 0.014(3) 0.016(3) 0.023(3) C16 0.042(3) 0.041(3) 0.027(2) 0.007(2) 0.008(2) 0.020(2) N21 0.031(2) 0.032(2) 0.036(2) 0.0068(17) 0.0053(17) 0.0147(18) N22 0.0220(18) 0.0225(18) 0.036(2) 0.0039(15) -0.0003(15) 0.0091(15) C23 0.026(2) 0.026(2) 0.038(3) -0.0038(18) 0.0020(18) 0.0106(19) C24 0.029(2) 0.025(2) 0.046(3) 0.005(2) 0.007(2) 0.008(2) C25 0.037(3) 0.030(3) 0.055(3) 0.012(2) 0.014(2) 0.012(2) C26 0.042(3) 0.032(3) 0.034(3) 0.008(2) -0.001(2) 0.015(2) C31 0.034(3) 0.030(2) 0.044(3) 0.013(2) 0.003(2) 0.013(2) C32 0.037(3) 0.037(3) 0.047(3) 0.015(2) 0.003(2) 0.022(2) C33 0.036(3) 0.033(3) 0.066(4) 0.010(2) 0.003(3) 0.019(2) C34 0.040(3) 0.039(3) 0.085(5) 0.021(3) 0.009(3) 0.022(3) C35 0.039(3) 0.064(4) 0.077(5) 0.017(4) -0.007(3) 0.026(3) C36 0.043(3) 0.059(4) 0.057(4) 0.011(3) -0.011(3) 0.023(3) C41 0.036(3) 0.045(4) 0.108(6) 0.017(4) 0.004(3) 0.023(3) N42 0.051(4) 0.054(4) 0.148(7) 0.017(4) -0.002(4) 0.034(3) B11X 0.084(3) 0.138(4) 0.062(2) -0.018(2) -0.019(2) 0.048(2) F12X 0.087(3) 0.138(4) 0.068(3) -0.015(2) -0.018(2) 0.047(3) F13X 0.089(3) 0.140(4) 0.063(3) -0.019(2) -0.017(2) 0.046(3) F14X 0.085(3) 0.137(4) 0.062(3) -0.017(2) -0.019(2) 0.047(3) F15X 0.085(3) 0.140(4) 0.067(3) -0.016(2) -0.017(2) 0.048(3) B11Y 0.084(3) 0.138(4) 0.062(2) -0.017(2) -0.0190(19) 0.048(2) F12Y 0.087(3) 0.140(4) 0.069(2) -0.015(2) -0.015(2) 0.046(3) F13Y 0.089(3) 0.138(4) 0.065(3) -0.019(2) -0.018(2) 0.049(3) F14Y 0.086(3) 0.140(4) 0.068(3) -0.014(2) -0.020(2) 0.048(3) F15Y 0.084(3) 0.137(4) 0.061(2) -0.017(2) -0.019(2) 0.048(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 N42 2.239(7) . ? Ag1 N42 2.239(7) 3_565 ? Ag1 N42 2.239(7) 2_665 ? Ni1 N22 2.107(4) 2_675 ? Ni1 N22 2.107(4) . ? Ni1 N22 2.107(4) 3_465 ? Ni1 N11 2.107(4) 2_675 ? Ni1 N11 2.107(4) 3_465 ? Ni1 N11 2.107(4) . ? N11 C12 1.327(7) . ? N11 C16 1.355(6) . ? C12 C13 1.399(7) . ? C12 C23 1.450(7) 3_465 ? C13 C14 1.388(9) . ? C13 H13 0.9500 . ? C14 C15 1.389(10) . ? C14 H14 0.9500 . ? C15 C16 1.378(8) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? N21 C25 1.358(7) . ? N21 N22 1.358(6) . ? N21 C26 1.439(7) . ? N22 C23 1.331(6) . ? C23 C24 1.403(7) . ? C23 C12 1.450(7) 2_675 ? C24 C25 1.338(9) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.491(8) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C31 C32 1.387(8) . ? C31 C36 1.411(8) . ? C32 C33 1.407(8) . ? C32 H32 0.9500 . ? C33 C34 1.364(9) . ? C33 H33 0.9500 . ? C34 C35 1.413(11) . ? C34 C41 1.461(10) . ? C35 C36 1.380(11) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C41 N42 1.126(10) . ? B11X F15X 1.3804(15) . ? B11X F14X 1.381(2) . ? B11X F13X 1.381(2) . ? B11X F12X 1.382(2) . ? B11Y F12Y 1.381(2) . ? B11Y F15Y 1.3811(15) . ? B11Y F14Y 1.381(2) . ? B11Y F13Y 1.382(2) . ? 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 N42 Ag1 N42 114.67(18) . 3_565 ? N42 Ag1 N42 114.67(18) . 2_665 ? N42 Ag1 N42 114.67(18) 3_565 2_665 ? N22 Ni1 N22 99.22(14) 2_675 . ? N22 Ni1 N22 99.22(14) 2_675 3_465 ? N22 Ni1 N22 99.22(14) . 3_465 ? N22 Ni1 N11 169.31(15) 2_675 2_675 ? N22 Ni1 N11 77.39(16) . 2_675 ? N22 Ni1 N11 91.36(16) 3_465 2_675 ? N22 Ni1 N11 77.39(16) 2_675 3_465 ? N22 Ni1 N11 91.36(16) . 3_465 ? N22 Ni1 N11 169.31(16) 3_465 3_465 ? N11 Ni1 N11 92.47(16) 2_675 3_465 ? N22 Ni1 N11 91.36(16) 2_675 . ? N22 Ni1 N11 169.31(15) . . ? N22 Ni1 N11 77.39(16) 3_465 . ? N11 Ni1 N11 92.47(16) 2_675 . ? N11 Ni1 N11 92.47(16) 3_465 . ? C12 N11 C16 118.9(4) . . ? C12 N11 Ni1 115.0(3) . . ? C16 N11 Ni1 125.9(4) . . ? N11 C12 C13 122.1(5) . . ? N11 C12 C23 115.5(4) . 3_465 ? C13 C12 C23 122.3(5) . 3_465 ? C14 C13 C12 119.1(6) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 118.2(5) . . ? C13 C14 H14 120.9 . . ? C15 C14 H14 120.9 . . ? C16 C15 C14 119.5(6) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? N11 C16 C15 122.0(5) . . ? N11 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? C25 N21 N22 110.3(4) . . ? C25 N21 C26 126.0(5) . . ? N22 N21 C26 122.3(4) . . ? C23 N22 N21 105.7(4) . . ? C23 N22 Ni1 114.0(3) . . ? N21 N22 Ni1 140.2(3) . . ? N22 C23 C24 110.0(5) . . ? N22 C23 C12 117.3(4) . 2_675 ? C24 C23 C12 132.6(5) . 2_675 ? C25 C24 C23 106.1(5) . . ? C25 C24 H24 127.0 . . ? C23 C24 H24 127.0 . . ? C24 C25 N21 107.8(5) . . ? C24 C25 H25 126.1 . . ? N21 C25 H25 126.1 . . ? N21 C26 C31 114.1(5) . . ? N21 C26 H26A 108.7 . . ? C31 C26 H26A 108.7 . . ? N21 C26 H26B 108.7 . . ? C31 C26 H26B 108.7 . . ? H26A C26 H26B 107.6 . . ? C32 C31 C36 121.3(6) . . ? C32 C31 C26 121.8(5) . . ? C36 C31 C26 116.8(6) . . ? C31 C32 C33 119.1(5) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C34 C33 C32 119.5(6) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C33 C34 C35 121.8(6) . . ? C33 C34 C41 118.1(7) . . ? C35 C34 C41 120.1(7) . . ? C36 C35 C34 119.1(6) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C35 C36 C31 119.0(7) . . ? C35 C36 H36 120.5 . . ? C31 C36 H36 120.5 . . ? N42 C41 C34 178.9(9) . . ? C41 N42 Ag1 169.0(8) . . ? F15X B11X F14X 109.5(8) . . ? F15X B11X F13X 107.7(8) . . ? F14X B11X F13X 111.1(8) . . ? F15X B11X F12X 108.4(8) . . ? F14X B11X F12X 108.9(8) . . ? F13X B11X F12X 111.1(8) . . ? F12Y B11Y F15Y 108.7(7) . . ? F12Y B11Y F14Y 112.3(7) . . ? F15Y B11Y F14Y 105.8(7) . . ? F12Y B11Y F13Y 109.0(7) . . ? F15Y B11Y F13Y 110.1(7) . . ? F14Y B11Y F13Y 110.9(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N22 Ni1 N11 C12 -106.7(4) 2_675 . . . ? N22 Ni1 N11 C12 65.0(10) . . . . ? N22 Ni1 N11 C12 -7.5(3) 3_465 . . . ? N11 Ni1 N11 C12 83.3(4) 2_675 . . . ? N11 Ni1 N11 C12 175.9(3) 3_465 . . . ? N22 Ni1 N11 C16 78.1(4) 2_675 . . . ? N22 Ni1 N11 C16 -110.3(9) . . . . ? N22 Ni1 N11 C16 177.2(4) 3_465 . . . ? N11 Ni1 N11 C16 -92.0(3) 2_675 . . . ? N11 Ni1 N11 C16 0.6(4) 3_465 . . . ? C16 N11 C12 C13 1.7(7) . . . . ? Ni1 N11 C12 C13 -173.9(4) . . . . ? C16 N11 C12 C23 -176.6(4) . . . 3_465 ? Ni1 N11 C12 C23 7.7(5) . . . 3_465 ? N11 C12 C13 C14 0.5(9) . . . . ? C23 C12 C13 C14 178.8(6) 3_465 . . . ? C12 C13 C14 C15 -0.9(10) . . . . ? C13 C14 C15 C16 -0.9(10) . . . . ? C12 N11 C16 C15 -3.6(8) . . . . ? Ni1 N11 C16 C15 171.5(5) . . . . ? C14 C15 C16 N11 3.2(10) . . . . ? C25 N21 N22 C23 0.9(6) . . . . ? C26 N21 N22 C23 168.3(5) . . . . ? C25 N21 N22 Ni1 -177.8(4) . . . . ? C26 N21 N22 Ni1 -10.4(8) . . . . ? N22 Ni1 N22 C23 -163.6(3) 2_675 . . . ? N22 Ni1 N22 C23 95.4(4) 3_465 . . . ? N11 Ni1 N22 C23 6.1(3) 2_675 . . . ? N11 Ni1 N22 C23 -86.1(4) 3_465 . . . ? N11 Ni1 N22 C23 24.9(11) . . . . ? N22 Ni1 N22 N21 15.0(5) 2_675 . . . ? N22 Ni1 N22 N21 -86.0(4) 3_465 . . . ? N11 Ni1 N22 N21 -175.3(5) 2_675 . . . ? N11 Ni1 N22 N21 92.4(5) 3_465 . . . ? N11 Ni1 N22 N21 -156.6(8) . . . . ? N21 N22 C23 C24 0.2(5) . . . . ? Ni1 N22 C23 C24 179.2(3) . . . . ? N21 N22 C23 C12 176.8(4) . . . 2_675 ? Ni1 N22 C23 C12 -4.1(6) . . . 2_675 ? N22 C23 C24 C25 -1.1(6) . . . . ? C12 C23 C24 C25 -177.1(5) 2_675 . . . ? C23 C24 C25 N21 1.6(6) . . . . ? N22 N21 C25 C24 -1.6(6) . . . . ? C26 N21 C25 C24 -168.4(5) . . . . ? C25 N21 C26 C31 85.2(6) . . . . ? N22 N21 C26 C31 -80.2(6) . . . . ? N21 C26 C31 C32 2.1(7) . . . . ? N21 C26 C31 C36 -174.6(5) . . . . ? C36 C31 C32 C33 -3.4(8) . . . . ? C26 C31 C32 C33 -179.9(5) . . . . ? C31 C32 C33 C34 1.0(8) . . . . ? C32 C33 C34 C35 1.3(9) . . . . ? C32 C33 C34 C41 -178.1(5) . . . . ? C33 C34 C35 C36 -1.3(10) . . . . ? C41 C34 C35 C36 178.1(6) . . . . ? C34 C35 C36 C31 -1.0(10) . . . . ? C32 C31 C36 C35 3.4(9) . . . . ? C26 C31 C36 C35 -179.9(6) . . . . ? C33 C34 C41 N42 -91(62) . . . . ? C35 C34 C41 N42 89(62) . . . . ? C34 C41 N42 Ag1 -116(60) . . . . ? N42 Ag1 N42 C41 -14(4) 3_565 . . . ? N42 Ag1 N42 C41 121(4) 2_665 . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.824 _refine_diff_density_min -1.373 _refine_diff_density_rms 0.166 #===END data_imw1190p21n _database_code_depnum_ccdc_archive 'CCDC 758096' #TrackingRef 'mixed_metal_networks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H12 Ag B F4 N4' _chemical_formula_weight 454.98 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' 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 'P2(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 8.2337(3) _cell_length_b 16.3732(6) _cell_length_c 12.5880(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.866(2) _cell_angle_gamma 90.00 _cell_volume 1632.36(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9931 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 30.00 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.851 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 1.285 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7395 _exptl_absorpt_correction_T_max 0.8307 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26881 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3338 _reflns_number_gt 2815 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The data was solved using direct methods. Data processing was carried out to a resolution of 0.8 angstromas as the data was only complete to this resolution. The structure contains a disordered BF4 anion. The atoms F2 > F4 have been modelled as being disordered over two sites (70:30). The model has benefited from the application of geometric and displacement restraints. The data suggested that further splitting may have been required, however as doing so would not have added any further chemical information no further action was thought necessary. 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^)+(0.0544P)^2^+6.1674P] 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_number_reflns 3338 _refine_ls_number_parameters 263 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1130 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.121 _refine_ls_shift/su_max 0.002 _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 Ag1 Ag 0.18784(4) 1.02875(2) 1.00373(3) 0.03217(15) Uani 1 1 d . . . N111 N 0.3985(5) 0.9539(2) 1.1101(3) 0.0247(8) Uani 1 1 d . . . C112 C 0.4638(5) 0.8954(2) 1.0583(4) 0.0219(8) Uani 1 1 d . . . C113 C 0.6051(5) 0.8497(3) 1.1130(4) 0.0276(9) Uani 1 1 d . . . H113 H 0.6477 0.8080 1.0755 0.033 Uiso 1 1 calc R . . C114 C 0.6820(6) 0.8665(3) 1.2233(4) 0.0349(11) Uani 1 1 d . . . H114 H 0.7797 0.8372 1.2622 0.042 Uiso 1 1 calc R . . C115 C 0.6155(7) 0.9260(3) 1.2757(4) 0.0367(11) Uani 1 1 d . . . H115 H 0.6667 0.9384 1.3511 0.044 Uiso 1 1 calc R . . C116 C 0.4725(7) 0.9676(3) 1.2172(4) 0.0334(11) Uani 1 1 d . . . H116 H 0.4251 1.0075 1.2547 0.040 Uiso 1 1 calc R . . N121 N 0.2016(5) 0.9060(2) 0.7850(3) 0.0255(8) Uani 1 1 d . . . N122 N 0.2422(4) 0.9256(2) 0.8930(3) 0.0228(7) Uani 1 1 d . . . C123 C 0.3821(5) 0.8832(2) 0.9401(3) 0.0224(8) Uani 1 1 d . . . C124 C 0.4311(6) 0.8356(3) 0.8617(4) 0.0277(9) Uani 1 1 d . . . H124 H 0.5256 0.8000 0.8737 0.033 Uiso 1 1 calc R . . C125 C 0.3122(6) 0.8517(3) 0.7635(4) 0.0298(10) Uani 1 1 d . . . H125 H 0.3085 0.8288 0.6935 0.036 Uiso 1 1 calc R . . C126 C 0.0447(6) 0.9378(3) 0.7108(4) 0.0310(10) Uani 1 1 d . . . H12A H 0.0672 0.9575 0.6418 0.037 Uiso 1 1 calc R . . H12B H 0.0048 0.9848 0.7464 0.037 Uiso 1 1 calc R . . C131 C -0.0920(5) 0.8728(3) 0.6831(4) 0.0247(9) Uani 1 1 d . . . C132 C -0.2244(7) 0.8840(3) 0.5894(4) 0.0392(12) Uani 1 1 d . . . H132 H -0.2321 0.9331 0.5481 0.047 Uiso 1 1 calc R . . C133 C -0.0876(7) 0.8041(3) 0.7468(4) 0.0345(11) Uani 1 1 d . . . H133 H -0.0008 0.7981 0.8138 0.041 Uiso 1 1 calc R . . N211 N 0.0315(5) 1.1317(2) 0.9584(4) 0.0317(9) Uani 1 1 d . . . C212 C -0.0532(6) 1.1864(3) 0.9242(4) 0.0295(10) Uani 1 1 d . . . C213 C -0.1667(5) 1.2526(3) 0.8842(4) 0.0273(9) Uani 1 1 d . . . C214 C -0.2913(6) 1.2437(3) 0.7860(4) 0.0340(11) Uani 1 1 d . . . H214 H -0.2939 1.1966 0.7414 0.041 Uiso 1 1 calc R . . C215 C -0.1543(7) 1.3241(3) 0.9444(5) 0.0434(13) Uani 1 1 d . . . H215 H -0.0630 1.3320 1.0086 0.052 Uiso 1 1 calc R . . B1 B 0.8158(4) 0.12014(16) 0.5567(2) 0.0312(11) Uani 1 1 d D . . F1 F 0.7521(4) 0.19759(16) 0.5288(2) 0.0462(8) Uani 1 1 d D A . F2X F 0.7312(8) 0.0654(2) 0.4771(4) 0.0580(17) Uani 0.711(6) 1 d PDU A 1 F3X F 0.9856(4) 0.1191(3) 0.5623(4) 0.0557(12) Uani 0.711(6) 1 d PDU A 1 F4X F 0.7947(8) 0.0968(2) 0.6568(3) 0.0545(12) Uani 0.711(6) 1 d PDU A 1 F2Y F 0.7874(19) 0.0725(3) 0.4630(4) 0.060(3) Uani 0.289(6) 1 d PDU A 2 F3Y F 0.9470(12) 0.1245(4) 0.6525(7) 0.0598(15) Uani 0.289(6) 1 d PDU A 2 F4Y F 0.7156(13) 0.0803(4) 0.6126(11) 0.0541(19) Uani 0.289(6) 1 d PDU A 2 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 0.0262(2) 0.0212(2) 0.0530(3) 0.00123(15) 0.01733(16) 0.00325(13) N111 0.0266(18) 0.0201(17) 0.0289(19) -0.0007(14) 0.0100(15) -0.0056(14) C112 0.0210(19) 0.0179(19) 0.028(2) 0.0002(16) 0.0083(17) -0.0050(15) C113 0.025(2) 0.021(2) 0.033(2) 0.0036(18) 0.0030(18) -0.0028(17) C114 0.033(2) 0.029(2) 0.035(3) 0.006(2) -0.002(2) -0.008(2) C115 0.045(3) 0.036(3) 0.024(2) 0.001(2) 0.001(2) -0.017(2) C116 0.046(3) 0.025(2) 0.033(2) -0.0058(19) 0.017(2) -0.012(2) N121 0.0284(18) 0.0189(17) 0.0258(18) 0.0013(14) 0.0016(15) -0.0001(14) N122 0.0230(17) 0.0173(17) 0.0265(18) 0.0011(14) 0.0037(14) -0.0022(13) C123 0.023(2) 0.0159(19) 0.027(2) 0.0034(16) 0.0052(17) -0.0021(15) C124 0.029(2) 0.019(2) 0.035(2) 0.0009(17) 0.0078(19) 0.0015(17) C125 0.041(3) 0.022(2) 0.026(2) -0.0011(17) 0.008(2) -0.0012(19) C126 0.032(2) 0.023(2) 0.031(2) 0.0052(18) -0.0027(19) -0.0034(18) C131 0.027(2) 0.021(2) 0.026(2) 0.0025(17) 0.0081(18) 0.0001(17) C132 0.037(3) 0.030(2) 0.042(3) 0.015(2) -0.003(2) -0.007(2) C133 0.045(3) 0.031(3) 0.025(2) 0.0065(19) 0.006(2) -0.004(2) N211 0.0258(19) 0.0233(19) 0.049(2) -0.0028(17) 0.0150(18) -0.0001(16) C212 0.025(2) 0.025(2) 0.042(3) -0.004(2) 0.014(2) -0.0030(18) C213 0.022(2) 0.023(2) 0.040(2) -0.0014(18) 0.0133(19) 0.0009(17) C214 0.041(3) 0.029(2) 0.033(2) -0.007(2) 0.012(2) 0.004(2) C215 0.037(3) 0.035(3) 0.048(3) -0.010(2) -0.006(2) 0.006(2) B1 0.034(3) 0.028(3) 0.029(3) 0.000(2) 0.005(2) 0.001(2) F1 0.0397(16) 0.0242(14) 0.067(2) 0.0089(14) 0.0016(15) -0.0010(12) F2X 0.109(5) 0.032(2) 0.046(2) -0.0028(18) 0.043(3) -0.024(2) F3X 0.042(2) 0.062(3) 0.062(3) -0.005(2) 0.013(2) 0.004(2) F4X 0.085(3) 0.043(2) 0.042(2) -0.0065(19) 0.028(2) -0.002(2) F2Y 0.119(6) 0.032(3) 0.046(3) 0.001(3) 0.051(4) -0.025(4) F3Y 0.065(3) 0.056(3) 0.056(3) -0.004(3) 0.012(3) 0.002(3) F4Y 0.089(4) 0.039(3) 0.045(4) -0.007(3) 0.036(3) -0.015(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 N211 2.103(4) . ? Ag1 N111 2.243(4) . ? Ag1 N122 2.311(4) . ? Ag1 Ag1 3.2101(7) 3_577 ? N111 C116 1.337(6) . ? N111 C112 1.351(6) . ? C112 C113 1.397(6) . ? C112 C123 1.470(6) . ? C113 C114 1.387(7) . ? C113 H113 0.9500 . ? C114 C115 1.371(8) . ? C114 H114 0.9500 . ? C115 C116 1.385(8) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? N121 N122 1.346(5) . ? N121 C125 1.353(6) . ? N121 C126 1.467(6) . ? N122 C123 1.337(5) . ? C123 C124 1.400(6) . ? C124 C125 1.376(7) . ? C124 H124 0.9500 . ? C125 H125 0.9500 . ? C126 C131 1.518(6) . ? C126 H12A 0.9900 . ? C126 H12B 0.9900 . ? C131 C133 1.376(6) . ? C131 C132 1.382(7) . ? C132 C215 1.381(7) 2_446 ? C132 H132 0.9500 . ? C133 C214 1.385(7) 2_446 ? C133 H133 0.9500 . ? N211 C212 1.144(6) . ? C212 C213 1.431(6) . ? C213 C214 1.382(7) . ? C213 C215 1.383(7) . ? C214 C133 1.385(7) 2_456 ? C214 H214 0.9500 . ? C215 C132 1.381(7) 2_456 ? C215 H215 0.9500 . ? B1 F4X 1.373(2) . ? B1 F2Y 1.379(3) . ? B1 F1 1.380(2) . ? B1 F3X 1.381(2) . ? B1 F2X 1.382(2) . ? B1 F3Y 1.384(3) . ? B1 F4Y 1.385(3) . ? 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 N211 Ag1 N111 156.29(15) . . ? N211 Ag1 N122 128.87(15) . . ? N111 Ag1 N122 73.47(13) . . ? N211 Ag1 Ag1 73.36(11) . 3_577 ? N111 Ag1 Ag1 116.03(9) . 3_577 ? N122 Ag1 Ag1 96.44(9) . 3_577 ? C116 N111 C112 118.3(4) . . ? C116 N111 Ag1 125.1(3) . . ? C112 N111 Ag1 116.3(3) . . ? N111 C112 C113 122.0(4) . . ? N111 C112 C123 117.0(4) . . ? C113 C112 C123 121.0(4) . . ? C114 C113 C112 118.6(5) . . ? C114 C113 H113 120.7 . . ? C112 C113 H113 120.7 . . ? C115 C114 C113 119.3(5) . . ? C115 C114 H114 120.4 . . ? C113 C114 H114 120.4 . . ? C114 C115 C116 119.2(4) . . ? C114 C115 H115 120.4 . . ? C116 C115 H115 120.4 . . ? N111 C116 C115 122.7(5) . . ? N111 C116 H116 118.7 . . ? C115 C116 H116 118.7 . . ? N122 N121 C125 111.3(4) . . ? N122 N121 C126 119.4(4) . . ? C125 N121 C126 129.0(4) . . ? C123 N122 N121 105.7(3) . . ? C123 N122 Ag1 113.4(3) . . ? N121 N122 Ag1 138.4(3) . . ? N122 C123 C124 110.8(4) . . ? N122 C123 C112 118.6(4) . . ? C124 C123 C112 130.5(4) . . ? C125 C124 C123 104.8(4) . . ? C125 C124 H124 127.6 . . ? C123 C124 H124 127.6 . . ? N121 C125 C124 107.4(4) . . ? N121 C125 H125 126.3 . . ? C124 C125 H125 126.3 . . ? N121 C126 C131 111.5(4) . . ? N121 C126 H12A 109.3 . . ? C131 C126 H12A 109.3 . . ? N121 C126 H12B 109.3 . . ? C131 C126 H12B 109.3 . . ? H12A C126 H12B 108.0 . . ? C133 C131 C132 119.6(4) . . ? C133 C131 C126 122.6(4) . . ? C132 C131 C126 117.8(4) . . ? C215 C132 C131 120.3(5) 2_446 . ? C215 C132 H132 119.9 2_446 . ? C131 C132 H132 119.9 . . ? C131 C133 C214 120.6(4) . 2_446 ? C131 C133 H133 119.7 . . ? C214 C133 H133 119.7 2_446 . ? C212 N211 Ag1 173.8(4) . . ? N211 C212 C213 176.6(5) . . ? C214 C213 C215 120.4(4) . . ? C214 C213 C212 119.2(4) . . ? C215 C213 C212 120.4(4) . . ? C213 C214 C133 119.3(4) . 2_456 ? C213 C214 H214 120.4 . . ? C133 C214 H214 120.4 2_456 . ? C132 C215 C213 119.6(5) 2_456 . ? C132 C215 H215 120.2 2_456 . ? C213 C215 H215 120.2 . . ? F4X B1 F2Y 126.4(6) . . ? F4X B1 F1 110.8(2) . . ? F2Y B1 F1 109.7(2) . . ? F4X B1 F3X 109.3(4) . . ? F2Y B1 F3X 88.2(7) . . ? F1 B1 F3X 109.47(19) . . ? F4X B1 F2X 108.6(4) . . ? F2Y B1 F2X 23.1(7) . . ? F1 B1 F2X 109.3(2) . . ? F3X B1 F2X 109.3(4) . . ? F4X B1 F3Y 58.6(6) . . ? F2Y B1 F3Y 133.1(7) . . ? F1 B1 F3Y 109.1(2) . . ? F3X B1 F3Y 54.4(6) . . ? F2X B1 F3Y 141.6(4) . . ? F4X B1 F4Y 32.8(5) . . ? F2Y B1 F4Y 100.6(8) . . ? F1 B1 F4Y 109.0(2) . . ? F3X B1 F4Y 134.7(5) . . ? F2X B1 F4Y 79.1(6) . . ? F3Y B1 F4Y 90.7(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N211 Ag1 N111 C116 18.9(6) . . . . ? N122 Ag1 N111 C116 -178.9(4) . . . . ? Ag1 Ag1 N111 C116 -89.7(4) 3_577 . . . ? N211 Ag1 N111 C112 -154.9(3) . . . . ? N122 Ag1 N111 C112 7.3(3) . . . . ? Ag1 Ag1 N111 C112 96.5(3) 3_577 . . . ? C116 N111 C112 C113 -0.2(6) . . . . ? Ag1 N111 C112 C113 174.0(3) . . . . ? C116 N111 C112 C123 -178.6(4) . . . . ? Ag1 N111 C112 C123 -4.3(5) . . . . ? N111 C112 C113 C114 -1.4(6) . . . . ? C123 C112 C113 C114 176.9(4) . . . . ? C112 C113 C114 C115 1.3(7) . . . . ? C113 C114 C115 C116 0.3(7) . . . . ? C112 N111 C116 C115 1.9(7) . . . . ? Ag1 N111 C116 C115 -171.8(3) . . . . ? C114 C115 C116 N111 -1.9(7) . . . . ? C125 N121 N122 C123 0.5(5) . . . . ? C126 N121 N122 C123 175.2(4) . . . . ? C125 N121 N122 Ag1 160.2(3) . . . . ? C126 N121 N122 Ag1 -25.1(6) . . . . ? N211 Ag1 N122 C123 161.2(3) . . . . ? N111 Ag1 N122 C123 -9.7(3) . . . . ? Ag1 Ag1 N122 C123 -125.0(3) 3_577 . . . ? N211 Ag1 N122 N121 2.6(5) . . . . ? N111 Ag1 N122 N121 -168.3(4) . . . . ? Ag1 Ag1 N122 N121 76.4(4) 3_577 . . . ? N121 N122 C123 C124 -0.4(5) . . . . ? Ag1 N122 C123 C124 -165.8(3) . . . . ? N121 N122 C123 C112 176.5(3) . . . . ? Ag1 N122 C123 C112 11.1(5) . . . . ? N111 C112 C123 N122 -4.9(6) . . . . ? C113 C112 C123 N122 176.7(4) . . . . ? N111 C112 C123 C124 171.2(4) . . . . ? C113 C112 C123 C124 -7.1(7) . . . . ? N122 C123 C124 C125 0.1(5) . . . . ? C112 C123 C124 C125 -176.3(4) . . . . ? N122 N121 C125 C124 -0.5(5) . . . . ? C126 N121 C125 C124 -174.6(4) . . . . ? C123 C124 C125 N121 0.3(5) . . . . ? N122 N121 C126 C131 -103.1(4) . . . . ? C125 N121 C126 C131 70.6(6) . . . . ? N121 C126 C131 C133 20.0(7) . . . . ? N121 C126 C131 C132 -159.6(5) . . . . ? C133 C131 C132 C215 -4.4(8) . . . 2_446 ? C126 C131 C132 C215 175.2(5) . . . 2_446 ? C132 C131 C133 C214 4.2(8) . . . 2_446 ? C126 C131 C133 C214 -175.3(5) . . . 2_446 ? N111 Ag1 N211 C212 142(3) . . . . ? N122 Ag1 N211 C212 -16(3) . . . . ? Ag1 Ag1 N211 C212 -101(3) 3_577 . . . ? Ag1 N211 C212 C213 122(8) . . . . ? N211 C212 C213 C214 -83(9) . . . . ? N211 C212 C213 C215 96(9) . . . . ? C215 C213 C214 C133 -5.5(8) . . . 2_456 ? C212 C213 C214 C133 173.0(5) . . . 2_456 ? C214 C213 C215 C132 5.3(9) . . . 2_456 ? C212 C213 C215 C132 -173.2(5) . . . 2_456 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.631 _refine_diff_density_min -1.425 _refine_diff_density_rms 0.114 #===END