data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_section_title ;Isomorphic polysupermolecules assembled from mixvalent Cu-triazolate sheets, benzene-1,3,5-tricarboxylates and halides ; _publ_contact_author_name 'Ye-Gao Yin' _publ_contact_author_email ygyin@stu.edu.cn loop_ _publ_author_name 'Zhi-Ling Zhang' 'Ying Chen' 'Ye-Gao Yin' 'You-Bang Ding' 'Dan Li' # Attachment 'date_cu1' data_data_cu1 _database_code_depnum_ccdc_archive 'CCDC 702860' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H11 Br Cu6 N12 O6' _chemical_formula_sum 'C17 H11 Br Cu6 N12 O6' _chemical_formula_weight 940.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I 4/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 20.3711(5) _cell_length_b 20.3711(5) _cell_length_c 13.7711(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5714.8(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.490 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.184 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3632.0 _exptl_absorpt_coefficient_mu 5.839 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.339 _exptl_absorpt_correction_T_max 0.496 _exptl_absorpt_process_details '(SADABS; Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17794 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3419 _reflns_number_gt 2588 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SMART _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0558P)^2^+4.3037P] 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 3402 _refine_ls_number_parameters 198 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.1206 _refine_ls_wR_factor_gt 0.0963 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.182 _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 Br1 Br 0.0000 0.0000 0.0000 0.0379(4) Uani 1 8 d S . . Br2 Br 0.0000 0.0000 0.25034(9) 0.0366(2) Uani 1 4 d S . . Br3 Br 0.5000 0.5000 0.0000 0.0392(4) Uani 1 8 d S . . Cu1 Cu 0.01634(4) 0.11757(5) 0.12555(6) 0.0583(3) Uani 1 1 d . . . Cu2 Cu 0.28272(5) 0.21734(5) 0.12290(4) 0.05069(19) Uani 1 1 d . . . Cu3 Cu 0.51526(4) 0.38291(6) 0.12822(6) 0.0608(3) Uani 1 1 d . . . O1 O 0.36681(18) 0.1367(2) 0.08034(18) 0.0394(6) Uani 1 1 d . . . O2 O 0.57392(18) 0.1264(2) 0.2576(2) 0.0593(10) Uani 1 1 d . . . O3 O 0.6682(2) 0.1259(4) 0.1841(3) 0.120(2) Uani 1 1 d U . . N1 N 0.1092(3) 0.1241(3) 0.1283(3) 0.0405(13) Uani 1 1 d . . . N2 N 0.2111(3) 0.1593(3) 0.1269(3) 0.0432(14) Uani 1 1 d . . . N3 N 0.1496(3) 0.0706(3) 0.1250(3) 0.0396(14) Uani 1 1 d . . . N4 N 0.3382(3) 0.2906(3) 0.1268(3) 0.0410(14) Uani 1 1 d . . . N5 N 0.4279(3) 0.3515(3) 0.1292(3) 0.0432(15) Uani 1 1 d . . . N6 N 0.3756(3) 0.3924(3) 0.1273(3) 0.0418(13) Uani 1 1 d . . . C1 C 0.3950(3) 0.1325(2) 0.0000 0.0350(14) Uani 1 2 d SD . . C2 C 0.4702(3) 0.12960(19) 0.0000 0.0339(14) Uani 1 2 d SD . . C3 C 0.5053(2) 0.12833(17) 0.0866(3) 0.0382(10) Uani 1 1 d D . . H3 H 0.4827 0.1291 0.1453 0.046 Uiso 1 1 calc R . . C4 C 0.5724(2) 0.1260(2) 0.0870(4) 0.0495(13) Uani 1 1 d D . . C5 C 0.6062(4) 0.1245(4) 0.0000 0.055(2) Uani 1 2 d SD . . H5 H 0.6518 0.1226 0.0000 0.066 Uiso 1 2 calc SR . . C6 C 0.6116(3) 0.1244(3) 0.1805(3) 0.0647(19) Uani 1 1 d D . . C7 C 0.1474(4) 0.1756(4) 0.1296(4) 0.0436(19) Uani 1 1 d . . . H7 H 0.1322 0.2186 0.1322 0.052 Uiso 1 1 calc R . . C8 C 0.2084(4) 0.0938(4) 0.1253(4) 0.0453(17) Uani 1 1 d . . . H8 H 0.2456 0.0673 0.1245 0.054 Uiso 1 1 calc R . . C9 C 0.4042(4) 0.2906(3) 0.1278(4) 0.0420(17) Uani 1 1 d . . . H9 H 0.4299 0.2529 0.1274 0.050 Uiso 1 1 calc R . . C10 C 0.3232(4) 0.3539(3) 0.1268(4) 0.0398(17) Uani 1 1 d . . . H10B H 0.2803 0.3697 0.1264 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0351(6) 0.0351(6) 0.0433(8) 0.000 0.000 0.000 Br2 0.0329(3) 0.0329(3) 0.0438(4) 0.000 0.000 0.000 Br3 0.0368(6) 0.0368(6) 0.0438(8) 0.000 0.000 0.000 Cu1 0.0193(5) 0.0415(6) 0.1141(7) 0.0028(5) 0.0035(3) 0.0044(5) Cu2 0.0357(6) 0.0360(6) 0.0804(4) -0.0008(3) 0.0009(3) -0.0204(2) Cu3 0.0200(5) 0.0415(6) 0.1209(8) -0.0051(5) -0.0005(4) -0.0040(5) O1 0.0312(19) 0.054(2) 0.0329(13) 0.0061(18) 0.0046(17) 0.0091(12) O2 0.047(2) 0.089(3) 0.0417(19) 0.0007(18) -0.0085(16) 0.003(2) O3 0.044(2) 0.254(7) 0.061(3) 0.002(3) -0.011(2) -0.019(4) N1 0.020(3) 0.029(3) 0.072(3) -0.003(2) 0.006(2) -0.007(3) N2 0.023(3) 0.033(3) 0.073(3) -0.005(2) 0.007(2) -0.007(3) N3 0.016(3) 0.020(3) 0.082(4) -0.004(2) 0.0014(19) -0.004(2) N4 0.024(3) 0.031(3) 0.068(3) -0.001(2) 0.002(2) -0.011(3) N5 0.024(3) 0.029(3) 0.077(4) -0.005(2) 0.000(2) 0.003(3) N6 0.022(3) 0.025(3) 0.079(3) 0.002(2) -0.002(2) 0.001(3) C1 0.034(3) 0.027(3) 0.044(3) 0.000 0.000 -0.003(3) C2 0.022(3) 0.043(4) 0.037(3) 0.000 0.000 -0.005(3) C3 0.032(2) 0.049(3) 0.034(2) 0.002(2) -0.0001(18) 0.002(2) C4 0.030(2) 0.074(4) 0.044(3) 0.004(3) -0.007(2) -0.005(3) C5 0.043(4) 0.086(7) 0.037(3) 0.000 0.000 0.001(5) C6 0.040(3) 0.121(6) 0.033(2) 0.005(3) -0.005(2) -0.028(3) C7 0.045(5) 0.020(3) 0.066(4) -0.002(2) 0.010(3) -0.004(3) C8 0.029(4) 0.025(4) 0.082(4) -0.007(3) 0.005(3) 0.001(3) C9 0.037(4) 0.013(3) 0.076(4) -0.003(2) 0.004(3) -0.004(3) C10 0.022(3) 0.018(3) 0.079(4) 0.002(2) -0.003(2) -0.002(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 Br1 Cu1 2.9726(10) . ? Cu1 N3 1.887(5) 3 ? Cu1 N1 1.898(6) . ? Cu2 N4 1.873(7) . ? Cu2 N2 1.879(7) . ? Cu3 N6 1.887(6) 3_655 ? Cu3 N5 1.890(6) . ? O1 C1 1.249(4) . ? O2 C6 1.311(6) . ? O3 C6 1.154(7) . ? N1 C7 1.307(9) . ? N1 N3 1.366(8) . ? N2 C8 1.335(10) . ? N2 C7 1.340(10) . ? N3 C8 1.289(10) . ? N3 Cu1 1.887(5) 4 ? N4 C10 1.325(9) . ? N4 C9 1.344(10) . ? N5 C9 1.332(9) . ? N5 N6 1.353(7) . ? N6 C10 1.325(9) . ? N6 Cu3 1.887(6) 4_565 ? C1 O1 1.249(4) 10 ? C1 C2 1.534(8) . ? C2 C3 1.391(5) . ? C2 C3 1.391(5) 10 ? C3 C4 1.368(6) . ? C3 H3 0.9300 . ? C4 C5 1.382(7) . ? C4 C6 1.516(7) . ? C5 C4 1.382(6) 10 ? C5 H5 0.9300 . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 H10B 0.9300 . ? 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 N3 Cu1 N1 155.7(2) 3 . ? N3 Cu1 Br1 99.84(16) 3 . ? N1 Cu1 Br1 100.36(17) . . ? N4 Cu2 N2 165.76(16) . . ? N6 Cu3 N5 155.7(2) 3_655 . ? C7 N1 N3 106.5(5) . . ? C7 N1 Cu1 130.6(6) . . ? N3 N1 Cu1 122.9(4) . . ? C8 N2 C7 102.1(7) . . ? C8 N2 Cu2 131.3(6) . . ? C7 N2 Cu2 126.6(6) . . ? C8 N3 N1 105.5(5) . . ? C8 N3 Cu1 131.7(5) . 4 ? N1 N3 Cu1 122.8(4) . 4 ? C10 N4 C9 103.3(6) . . ? C10 N4 Cu2 129.5(5) . . ? C9 N4 Cu2 127.1(6) . . ? C9 N5 N6 106.6(5) . . ? C9 N5 Cu3 131.1(5) . . ? N6 N5 Cu3 122.3(5) . . ? C10 N6 N5 105.7(5) . . ? C10 N6 Cu3 130.8(5) . 4_565 ? N5 N6 Cu3 123.4(5) . 4_565 ? O1 C1 O1 124.7(6) 10 . ? O1 C1 C2 117.5(3) 10 . ? O1 C1 C2 117.5(3) . . ? C3 C2 C3 118.1(6) . 10 ? C3 C2 C1 121.0(3) . . ? C3 C2 C1 121.0(3) 10 . ? C4 C3 C2 121.1(5) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 119.7(5) . . ? C3 C4 C6 122.0(5) . . ? C5 C4 C6 118.3(5) . . ? C4 C5 C4 120.1(7) 10 . ? C4 C5 H5 119.9 10 . ? C4 C5 H5 119.9 . . ? O3 C6 O2 123.3(5) . . ? O3 C6 C4 124.2(5) . . ? O2 C6 C4 112.3(5) . . ? N1 C7 N2 112.1(7) . . ? N1 C7 H7 124.0 . . ? N2 C7 H7 124.0 . . ? N3 C8 N2 113.8(7) . . ? N3 C8 H8 123.1 . . ? N2 C8 H8 123.1 . . ? N5 C9 N4 111.4(7) . . ? N5 C9 H9 124.3 . . ? N4 C9 H9 124.3 . . ? N6 C10 N4 113.0(7) . . ? N6 C10 H10B 123.5 . . ? N4 C10 H10B 123.5 . . ? 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 N3 Cu1 N1 C7 -1.9(8) 3 . . . ? Br1 Cu1 N1 C7 144.1(5) . . . . ? N3 Cu1 N1 N3 -178.9(5) 3 . . . ? Br1 Cu1 N1 N3 -33.0(4) . . . . ? N4 Cu2 N2 C8 -169.3(6) . . . . ? N4 Cu2 N2 C7 12.7(9) . . . . ? C7 N1 N3 C8 0.4(6) . . . . ? Cu1 N1 N3 C8 178.1(3) . . . . ? C7 N1 N3 Cu1 178.2(4) . . . 4 ? Cu1 N1 N3 Cu1 -4.1(5) . . . 4 ? N2 Cu2 N4 C10 -14.8(9) . . . . ? N2 Cu2 N4 C9 167.1(6) . . . . ? N6 Cu3 N5 C9 -1.5(8) 3_655 . . . ? N6 Cu3 N5 N6 -178.4(5) 3_655 . . . ? C9 N5 N6 C10 1.2(5) . . . . ? Cu3 N5 N6 C10 178.8(4) . . . . ? C9 N5 N6 Cu3 -180.0(3) . . . 4_565 ? Cu3 N5 N6 Cu3 -2.4(5) . . . 4_565 ? O1 C1 C2 C3 176.6(4) 10 . . . ? O1 C1 C2 C3 3.2(5) . . . . ? O1 C1 C2 C3 -3.2(5) 10 . . 10 ? O1 C1 C2 C3 -176.6(4) . . . 10 ? C3 C2 C3 C4 0.1(6) 10 . . . ? C1 C2 C3 C4 -179.7(2) . . . . ? C2 C3 C4 C5 -0.4(5) . . . . ? C2 C3 C4 C6 -179.8(3) . . . . ? C3 C4 C5 C4 0.6(9) . . . 10 ? C6 C4 C5 C4 -180.0(5) . . . 10 ? C3 C4 C6 O3 -175.7(6) . . . . ? C5 C4 C6 O3 4.9(9) . . . . ? C3 C4 C6 O2 -1.0(7) . . . . ? C5 C4 C6 O2 179.6(6) . . . . ? N3 N1 C7 N2 0.3(6) . . . . ? Cu1 N1 C7 N2 -177.1(4) . . . . ? C8 N2 C7 N1 -0.9(6) . . . . ? Cu2 N2 C7 N1 177.6(4) . . . . ? N1 N3 C8 N2 -1.1(7) . . . . ? Cu1 N3 C8 N2 -178.6(4) 4 . . . ? C7 N2 C8 N3 1.2(7) . . . . ? Cu2 N2 C8 N3 -177.1(3) . . . . ? N6 N5 C9 N4 -1.1(6) . . . . ? Cu3 N5 C9 N4 -178.5(4) . . . . ? C10 N4 C9 N5 0.6(6) . . . . ? Cu2 N4 C9 N5 179.1(3) . . . . ? N5 N6 C10 N4 -0.9(6) . . . . ? Cu3 N6 C10 N4 -179.6(4) 4_565 . . . ? C9 N4 C10 N6 0.2(6) . . . . ? Cu2 N4 C10 N6 -178.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.943 _refine_diff_density_min -1.310 _refine_diff_density_rms 0.325 # Attachment 'data_cu2' data_data_cu2 _database_code_depnum_ccdc_archive 'CCDC 702861' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H11 Cl Cu6 N12 O6' _chemical_formula_sum 'C17 H11 Cl Cu6 N12 O6' _chemical_formula_weight 896.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4/ncc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y, x, z-1/2' _cell_length_a 20.321(2) _cell_length_b 20.321 _cell_length_c 13.6990(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5656.9(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 25.000 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.104 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3488 _exptl_absorpt_coefficient_mu 4.581 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.387 _exptl_absorpt_correction_T_max 0.551 _exptl_absorpt_process_details '(SADABS; Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 27321 _diffrn_reflns_av_R_equivalents 0.0728 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2498 _reflns_number_gt 1408 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SMART _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0991P)^2^+4.7487P] 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 2497 _refine_ls_number_parameters 247 _refine_ls_number_restraints 105 _refine_ls_R_factor_all 0.1112 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1954 _refine_ls_wR_factor_gt 0.1533 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.63266(5) 0.73511(5) 0.08204(11) 0.0704(5) Uani 1 1 d . . . Cu2 Cu 0.46931(6) 0.96885(6) 0.12761(9) 0.0690(5) Uani 1 1 d . . . Cu3 Cu 0.36721(5) 1.23534(5) 0.16431(11) 0.0706(5) Uani 1 1 d . . . Cl1 Cl 0.7500 0.7500 -0.0015(4) 0.0503(10) Uani 1 4 d S . . Cl2 Cl 0.2500 1.2500 0.2507(4) 0.0521(10) Uani 1 4 d S . . N1 N 0.6014(3) 0.8220(3) 0.0902(6) 0.0528(18) Uani 1 1 d . . . N2 N 0.6427(3) 0.8747(3) 0.0913(6) 0.0558(19) Uani 1 1 d . . . N3 N 0.5403(3) 0.9109(3) 0.1078(5) 0.0552(19) Uani 1 1 d . . . N4 N 0.4126(3) 1.0414(3) 0.1372(6) 0.062(2) Uani 1 1 d . . . N5 N 0.3761(3) 1.1431(3) 0.1553(5) 0.0518(18) Uani 1 1 d . . . N6 N 0.3229(3) 1.1021(3) 0.1560(6) 0.0507(18) Uani 1 1 d . . . C1 C 0.5419(4) 0.8464(4) 0.1020(7) 0.064(3) Uani 1 1 d . . . H1 H 0.5043 0.8203 0.1059 0.076 Uiso 1 1 calc R . . C2 C 0.6055(4) 0.9271(5) 0.1005(6) 0.056(2) Uani 1 1 d . . . H2 H 0.6214 0.9700 0.1020 0.067 Uiso 1 1 calc R . . C3 C 0.4275(4) 1.1032(4) 0.1440(7) 0.059(3) Uani 1 1 d . . . H3 H 0.4706 1.1185 0.1413 0.071 Uiso 1 1 calc R . . C4 C 0.3474(4) 1.0419(4) 0.1463(7) 0.058(2) Uani 1 1 d . . . H4 H 0.3217 1.0040 0.1460 0.070 Uiso 1 1 calc R . . O1 O 0.3852(18) 0.8853(17) 0.1730(19) 0.038(7) Uani 0.50 1 d PDU A -1 O2 O 0.381(2) 0.892(2) 0.336(2) 0.059(10) Uani 0.50 1 d PDU A -1 O3 O 0.1747(5) 0.8793(6) 0.5064(9) 0.072(3) Uani 0.50 1 d PDU A -1 O4 O 0.0805(6) 0.8719(10) 0.4294(12) 0.107(5) Uani 0.50 1 d PDU A -1 O5 O 0.0842(6) 0.8761(10) 0.0607(12) 0.108(5) Uani 0.50 1 d PDU A -1 O6 O 0.1797(5) 0.8758(5) -0.0123(8) 0.058(3) Uani 0.50 1 d PDU A -1 C5 C 0.2815(3) 0.8800(3) 0.2505(8) 0.043(3) Uani 0.50 1 d PGDU A -1 C6 C 0.2463(4) 0.8789(5) 0.3374(6) 0.043(4) Uani 0.50 1 d PGDU A -1 H6 H 0.2684 0.8802 0.3968 0.052 Uiso 0.50 1 calc PR A -1 C7 C 0.1779(4) 0.8760(5) 0.3356(7) 0.060(5) Uani 0.50 1 d PGDU A -1 C8 C 0.1449(3) 0.8741(4) 0.2469(9) 0.057(5) Uani 0.50 1 d PGDU A -1 H8 H 0.0991 0.8721 0.2457 0.069 Uiso 0.50 1 calc PR A -1 C9 C 0.1801(5) 0.8751(5) 0.1599(7) 0.050(4) Uani 0.50 1 d PGDU A -1 C10 C 0.2484(4) 0.8781(5) 0.1617(6) 0.051(4) Uani 0.50 1 d PGDU A -1 H10 H 0.2720 0.8788 0.1035 0.061 Uiso 0.50 1 calc PR A -1 C11 C 0.3562(4) 0.8834(5) 0.2533(16) 0.037(4) Uani 0.50 1 d PDU A -1 C12 C 0.1413(6) 0.8750(9) 0.4299(9) 0.061(6) Uani 0.50 1 d PDU A -1 C13 C 0.1455(6) 0.8731(8) 0.0638(8) 0.060(6) Uani 0.50 1 d PDU A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0524(7) 0.0282(5) 0.1306(12) 0.0007(7) 0.0068(7) 0.0052(5) Cu2 0.0458(7) 0.0463(7) 0.1148(11) 0.0004(6) 0.0061(6) 0.0240(5) Cu3 0.0518(8) 0.0271(5) 0.1329(12) 0.0044(7) -0.0030(7) -0.0046(5) Cl1 0.0444(14) 0.0444(14) 0.062(3) 0.000 0.000 0.000 Cl2 0.0456(15) 0.0456(15) 0.065(3) 0.000 0.000 0.000 N1 0.028(3) 0.031(3) 0.100(6) 0.003(4) 0.008(3) 0.003(3) N2 0.035(4) 0.034(4) 0.098(6) -0.009(4) -0.001(4) 0.002(3) N3 0.036(4) 0.043(4) 0.087(6) 0.000(4) 0.004(3) 0.009(3) N4 0.034(4) 0.042(4) 0.111(7) 0.008(4) 0.005(4) 0.016(3) N5 0.029(4) 0.033(4) 0.094(6) 0.001(4) 0.002(4) 0.007(3) N6 0.025(3) 0.028(3) 0.099(5) 0.001(3) 0.003(3) 0.003(3) C1 0.022(4) 0.047(5) 0.122(8) 0.000(5) 0.015(4) -0.003(4) C2 0.024(4) 0.053(5) 0.091(7) -0.005(5) 0.007(4) 0.008(4) C3 0.018(4) 0.051(6) 0.109(8) 0.010(5) -0.001(4) 0.002(4) C4 0.038(5) 0.031(4) 0.106(7) 0.003(4) 0.010(5) -0.003(4) O1 0.040(10) 0.035(9) 0.039(9) -0.001(7) 0.001(6) -0.005(6) O2 0.057(12) 0.056(12) 0.065(12) -0.001(8) 0.006(8) -0.005(8) O3 0.057(6) 0.097(7) 0.060(6) -0.001(6) 0.004(6) -0.005(6) O4 0.069(8) 0.155(10) 0.096(9) 0.004(8) 0.012(7) -0.007(8) O5 0.072(8) 0.157(10) 0.096(9) 0.001(8) -0.008(7) 0.002(8) O6 0.046(5) 0.075(6) 0.052(6) -0.005(6) 0.001(5) -0.003(5) C5 0.036(7) 0.043(7) 0.048(7) 0.005(6) -0.002(6) -0.006(6) C6 0.036(7) 0.040(7) 0.053(8) -0.001(7) 0.003(6) -0.005(5) C7 0.057(8) 0.064(8) 0.058(8) 0.000(7) 0.008(7) -0.007(7) C8 0.040(8) 0.073(9) 0.059(7) 0.005(8) 0.000(8) -0.002(7) C9 0.050(7) 0.048(7) 0.053(8) 0.001(7) -0.003(7) 0.006(6) C10 0.049(8) 0.056(8) 0.048(8) 0.000(7) 0.003(6) 0.001(6) C11 0.037(7) 0.026(6) 0.048(7) -0.005(7) 0.001(7) 0.003(5) C12 0.042(8) 0.074(10) 0.068(10) 0.006(8) 0.015(7) 0.014(8) C13 0.051(9) 0.063(10) 0.067(10) -0.008(8) -0.008(7) 0.002(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.880(6) . ? Cu1 N2 1.888(6) 3_655 ? Cu1 Cl1 2.662(3) . ? Cu2 N4 1.876(7) . ? Cu2 N3 1.882(7) . ? Cu2 O2 2.43(5) 7_455 ? Cu3 N5 1.887(6) . ? Cu3 N6 1.889(6) 3_665 ? Cu3 Cl2 2.677(3) . ? Cl1 Cu1 2.662(2) 2_665 ? Cl1 Cu1 2.662(2) 3_655 ? Cl1 Cu1 2.662(2) 4_565 ? Cl2 Cu3 2.677(3) 4_465 ? Cl2 Cu3 2.677(3) 2_575 ? Cl2 Cu3 2.677(3) 3_665 ? N1 C1 1.317(9) . ? N1 N2 1.362(8) . ? N2 C2 1.312(10) . ? N2 Cu1 1.888(6) 4_565 ? N3 C1 1.314(10) . ? N3 C2 1.368(10) . ? N4 C3 1.296(11) . ? N4 C4 1.331(10) . ? N5 C3 1.331(10) . ? N5 N6 1.366(8) . ? N6 C4 1.327(9) . ? N6 Cu3 1.889(6) 4_465 ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? O1 C11 1.248(10) . ? O2 C11 1.248(10) . ? O2 Cu2 2.43(5) 7_455 ? O3 C12 1.252(9) . ? O4 C12 1.237(9) . ? O5 C13 1.249(9) . ? O6 C13 1.253(9) . ? C5 C6 1.3900 . ? C5 C10 1.3900 . ? C5 C11 1.520(9) . ? C6 C7 1.3900 . ? C6 H6 0.9300 . ? C7 C8 1.3900 . ? C7 C12 1.490(9) . ? C8 C9 1.3900 . ? C8 H8 0.9300 . ? C9 C10 1.3900 . ? C9 C13 1.493(9) . ? C10 H10 0.9300 . ? 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 N1 Cu1 N2 154.6(3) . 3_655 ? N1 Cu1 Cl1 102.82(19) . . ? N2 Cu1 Cl1 102.3(2) 3_655 . ? N4 Cu2 N3 166.6(3) . . ? N4 Cu2 O2 99.5(9) . 7_455 ? N3 Cu2 O2 93.8(9) . 7_455 ? N5 Cu3 N6 154.2(3) . 3_665 ? N5 Cu3 Cl2 103.0(2) . . ? N6 Cu3 Cl2 102.5(2) 3_665 . ? Cu1 Cl1 Cu1 79.35(8) 2_665 3_655 ? Cu1 Cl1 Cu1 79.35(8) 2_665 4_565 ? Cu1 Cl1 Cu1 129.1(2) 3_655 4_565 ? Cu1 Cl1 Cu1 129.1(2) 2_665 . ? Cu1 Cl1 Cu1 79.35(8) 3_655 . ? Cu1 Cl1 Cu1 79.35(8) 4_565 . ? Cu3 Cl2 Cu3 78.71(8) 4_465 . ? Cu3 Cl2 Cu3 78.71(8) 4_465 2_575 ? Cu3 Cl2 Cu3 127.5(2) . 2_575 ? Cu3 Cl2 Cu3 127.5(2) 4_465 3_665 ? Cu3 Cl2 Cu3 78.71(8) . 3_665 ? Cu3 Cl2 Cu3 78.71(8) 2_575 3_665 ? C1 N1 N2 105.5(6) . . ? C1 N1 Cu1 132.2(5) . . ? N2 N1 Cu1 122.1(5) . . ? C2 N2 N1 106.5(6) . . ? C2 N2 Cu1 130.1(6) . 4_565 ? N1 N2 Cu1 123.3(5) . 4_565 ? C1 N3 C2 102.3(7) . . ? C1 N3 Cu2 130.7(6) . . ? C2 N3 Cu2 127.0(6) . . ? C3 N4 C4 102.6(7) . . ? C3 N4 Cu2 128.5(6) . . ? C4 N4 Cu2 128.6(6) . . ? C3 N5 N6 104.5(6) . . ? C3 N5 Cu3 133.4(6) . . ? N6 N5 Cu3 122.0(5) . . ? C4 N6 N5 105.4(6) . . ? C4 N6 Cu3 131.6(5) . 4_465 ? N5 N6 Cu3 123.0(5) . 4_465 ? N3 C1 N1 114.0(7) . . ? N3 C1 H1 123.0 . . ? N1 C1 H1 123.0 . . ? N2 C2 N3 111.7(8) . . ? N2 C2 H2 124.2 . . ? N3 C2 H2 124.2 . . ? N4 C3 N5 114.5(8) . . ? N4 C3 H3 122.7 . . ? N5 C3 H3 122.7 . . ? N6 C4 N4 113.0(7) . . ? N6 C4 H4 123.5 . . ? N4 C4 H4 123.5 . . ? C11 O2 Cu2 125(3) . 7_455 ? C6 C5 C10 120.0 . . ? C6 C5 C11 119.6(11) . . ? C10 C5 C11 120.4(11) . . ? C7 C6 C5 120.0 . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C8 C7 C6 120.0 . . ? C8 C7 C12 121.0(9) . . ? C6 C7 C12 119.0(9) . . ? C9 C8 C7 120.0 . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 120.0 . . ? C8 C9 C13 120.9(9) . . ? C10 C9 C13 119.1(9) . . ? C9 C10 C5 120.0 . . ? C9 C10 H10 120.0 . . ? C5 C10 H10 120.0 . . ? O1 C11 O2 127.0(16) . . ? O1 C11 C5 117(2) . . ? O2 C11 C5 116(2) . . ? O4 C12 O3 123.3(13) . . ? O4 C12 C7 119.6(12) . . ? O3 C12 C7 117.0(11) . . ? O5 C13 O6 121.5(13) . . ? O5 C13 C9 119.8(12) . . ? O6 C13 C9 118.2(11) . . ? 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 N1 Cu1 Cl1 Cu1 92.3(2) . . . 2_665 ? N2 Cu1 Cl1 Cu1 -91.6(3) 3_655 . . 2_665 ? N1 Cu1 Cl1 Cu1 159.1(2) . . . 3_655 ? N2 Cu1 Cl1 Cu1 -24.9(3) 3_655 . . 3_655 ? N1 Cu1 Cl1 Cu1 25.6(3) . . . 4_565 ? N2 Cu1 Cl1 Cu1 -158.3(3) 3_655 . . 4_565 ? N5 Cu3 Cl2 Cu3 -26.1(3) . . . 4_465 ? N6 Cu3 Cl2 Cu3 158.5(2) 3_665 . . 4_465 ? N5 Cu3 Cl2 Cu3 -92.2(2) . . . 2_575 ? N6 Cu3 Cl2 Cu3 92.3(2) 3_665 . . 2_575 ? N5 Cu3 Cl2 Cu3 -158.4(2) . . . 3_665 ? N6 Cu3 Cl2 Cu3 26.2(3) 3_665 . . 3_665 ? N2 Cu1 N1 C1 -9.9(14) 3_655 . . . ? Cl1 Cu1 N1 C1 161.1(9) . . . . ? N2 Cu1 N1 N2 165.0(10) 3_655 . . . ? Cl1 Cu1 N1 N2 -24.0(7) . . . . ? C1 N1 N2 C2 -1.9(10) . . . . ? Cu1 N1 N2 C2 -178.0(6) . . . . ? C1 N1 N2 Cu1 177.5(6) . . . 4_565 ? Cu1 N1 N2 Cu1 1.4(10) . . . 4_565 ? N4 Cu2 N3 C1 -164.6(13) . . . . ? O2 Cu2 N3 C1 8.9(12) 7_455 . . . ? N4 Cu2 N3 C2 19.0(19) . . . . ? O2 Cu2 N3 C2 -167.5(11) 7_455 . . . ? N3 Cu2 N4 C3 -21(2) . . . . ? O2 Cu2 N4 C3 165.1(12) 7_455 . . . ? N3 Cu2 N4 C4 164.4(12) . . . . ? O2 Cu2 N4 C4 -9.0(12) 7_455 . . . ? N6 Cu3 N5 C3 10.3(14) 3_665 . . . ? Cl2 Cu3 N5 C3 -159.5(9) . . . . ? N6 Cu3 N5 N6 -167.0(9) 3_665 . . . ? Cl2 Cu3 N5 N6 23.2(7) . . . . ? C3 N5 N6 C4 0.7(10) . . . . ? Cu3 N5 N6 C4 178.6(6) . . . . ? C3 N5 N6 Cu3 -177.1(6) . . . 4_465 ? Cu3 N5 N6 Cu3 0.9(10) . . . 4_465 ? C2 N3 C1 N1 -1.2(11) . . . . ? Cu2 N3 C1 N1 -178.2(6) . . . . ? N2 N1 C1 N3 2.0(11) . . . . ? Cu1 N1 C1 N3 177.5(6) . . . . ? N1 N2 C2 N3 1.3(11) . . . . ? Cu1 N2 C2 N3 -178.1(6) 4_565 . . . ? C1 N3 C2 N2 -0.2(11) . . . . ? Cu2 N3 C2 N2 177.1(6) . . . . ? C4 N4 C3 N5 -1.1(11) . . . . ? Cu2 N4 C3 N5 -176.4(6) . . . . ? N6 N5 C3 N4 0.2(11) . . . . ? Cu3 N5 C3 N4 -177.3(7) . . . . ? N5 N6 C4 N4 -1.5(11) . . . . ? Cu3 N6 C4 N4 176.0(6) 4_465 . . . ? C3 N4 C4 N6 1.6(11) . . . . ? Cu2 N4 C4 N6 176.8(6) . . . . ? C10 C5 C6 C7 0.0 . . . . ? C11 C5 C6 C7 179.9(3) . . . . ? C5 C6 C7 C8 0.0 . . . . ? C5 C6 C7 C12 -180.0(3) . . . . ? C6 C7 C8 C9 0.0 . . . . ? C12 C7 C8 C9 180.0(3) . . . . ? C7 C8 C9 C10 0.0 . . . . ? C7 C8 C9 C13 180.0(3) . . . . ? C8 C9 C10 C5 0.0 . . . . ? C13 C9 C10 C5 180.0(3) . . . . ? C6 C5 C10 C9 0.0 . . . . ? C11 C5 C10 C9 -179.9(3) . . . . ? Cu2 O2 C11 O1 36(5) 7_455 . . . ? Cu2 O2 C11 C5 -134.7(18) 7_455 . . . ? C6 C5 C11 O1 -178.8(19) . . . . ? C10 C5 C11 O1 1.0(19) . . . . ? C6 C5 C11 O2 -7(3) . . . . ? C10 C5 C11 O2 173(2) . . . . ? C8 C7 C12 O4 0.5(18) . . . . ? C6 C7 C12 O4 -179.5(17) . . . . ? C8 C7 C12 O3 -177.4(14) . . . . ? C6 C7 C12 O3 2.5(15) . . . . ? C8 C9 C13 O5 6.1(17) . . . . ? C10 C9 C13 O5 -173.9(17) . . . . ? C8 C9 C13 O6 178.3(13) . . . . ? C10 C9 C13 O6 -1.7(14) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.066 _refine_diff_density_min -0.738 _refine_diff_density_rms 0.286