# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data__synCu2(bpypz)2Br2 _database_code_depnum_ccdc_archive 'CCDC 704681' #TrackingRef 'synCu2(bpypz)2Br2.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C26 H18 Br2 Cu2 N8 ' _chemical_formula_moiety 'C26 H18 Br2 Cu2 N8 ' _chemical_formula_weight 729.38 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 9.105(14) _cell_length_b 12.40(2) _cell_length_c 12.57(2) _cell_angle_alpha 100.78(4) _cell_angle_beta 96.00(3) _cell_angle_gamma 94.43(4) _cell_volume 1379(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 2262 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 200.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716.00 _exptl_absorpt_coefficient_mu 4.478 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.425 _exptl_absorpt_correction_T_max 0.639 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 343 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 13228 _diffrn_reflns_av_R_equivalents 0.183 _diffrn_reflns_theta_max 27.64 _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.64 _diffrn_measured_fraction_theta_full 0.975 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6263 _reflns_number_gt 1655 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.3495 _refine_ls_wR_factor_ref 0.6973 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 6263 _refine_ls_number_parameters 174 _refine_ls_goodness_of_fit_ref 1.476 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 2.7380 _refine_diff_density_max 4.84 _refine_diff_density_min -2.20 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Br Br -0.290 2.459 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Br(1) Br 0.2029(4) 0.3865(3) 0.8729(3) 0.105(2) Uani 1.00 1 d . . . Br(2) Br 0.4035(5) 0.0058(3) 0.6753(4) 0.111(2) Uani 1.00 1 d . . . Cu(1) Cu 0.0292(5) 0.2220(3) 0.9134(4) 0.103(2) Uani 1.00 1 d . . . Cu(2) Cu 0.1781(5) -0.0555(4) 0.7710(4) 0.108(2) Uani 1.00 1 d . . . N(1) N 0.053(3) 0.276(3) 1.086(2) 0.097(10) Uiso 1.00 1 d . . . N(2) N 0.155(4) 0.117(3) 0.966(3) 0.121(12) Uiso 1.00 1 d . . . N(3) N 0.206(3) 0.013(2) 0.942(2) 0.095(10) Uiso 1.00 1 d . . . N(4) N 0.289(3) -0.160(2) 0.849(2) 0.085(9) Uiso 1.00 1 d . . . N(5) N -0.163(3) 0.273(2) 0.862(2) 0.096(10) Uiso 1.00 1 d . . . N(6) N -0.039(3) 0.116(2) 0.786(2) 0.090(9) Uiso 1.00 1 d . . . N(7) N 0.008(3) 0.031(2) 0.731(2) 0.080(8) Uiso 1.00 1 d . . . N(8) N 0.066(4) -0.167(3) 0.618(3) 0.116(11) Uiso 1.00 1 d . . . C(1) C 0.018(7) 0.361(6) 1.135(6) 0.18(2) Uiso 1.00 1 d . . . C(2) C 0.043(3) 0.431(2) 1.233(2) 0.059(8) Uiso 1.00 1 d . . . C(3) C 0.153(6) 0.373(5) 1.291(4) 0.15(2) Uiso 1.00 1 d . . . C(4) C 0.214(5) 0.256(4) 1.269(4) 0.140(18) Uiso 1.00 1 d . . . C(5) C 0.160(3) 0.234(2) 1.143(2) 0.067(9) Uiso 1.00 1 d . . . C(6) C 0.209(3) 0.125(2) 1.076(2) 0.054(8) Uiso 1.00 1 d . . . C(7) C 0.291(4) 0.042(3) 1.105(3) 0.105(13) Uiso 1.00 1 d . . . C(8) C 0.2917(18) -0.0078(13) 1.0006(14) 0.000(3) Uiso 1.00 1 d . . . C(9) C 0.349(3) -0.129(2) 0.955(2) 0.060(8) Uiso 1.00 1 d . . . C(10) C 0.434(3) -0.170(2) 1.041(2) 0.060(8) Uiso 1.00 1 d . . . C(11) C 0.526(6) -0.256(5) 0.982(4) 0.16(2) Uiso 1.00 1 d . . . C(12) C 0.430(5) -0.322(4) 0.873(3) 0.110(14) Uiso 1.00 1 d . . . C(13) C 0.352(4) -0.234(4) 0.838(3) 0.107(14) Uiso 1.00 1 d . . . C(14) C -0.209(4) 0.384(3) 0.855(3) 0.084(11) Uiso 1.00 1 d . . . C(15) C -0.340(4) 0.428(3) 0.829(3) 0.093(12) Uiso 1.00 1 d . . . C(16) C -0.444(5) 0.355(4) 0.744(4) 0.127(16) Uiso 1.00 1 d . . . C(17) C -0.355(4) 0.271(3) 0.702(3) 0.098(13) Uiso 1.00 1 d . . . C(18) C -0.226(7) 0.234(5) 0.750(5) 0.16(2) Uiso 1.00 1 d . . . C(19) C -0.147(4) 0.132(3) 0.714(3) 0.091(12) Uiso 1.00 1 d . . . C(20) C -0.205(5) 0.064(4) 0.631(4) 0.115(15) Uiso 1.00 1 d . . . C(21) C -0.0852(18) -0.0170(12) 0.6487(13) 0.000(3) Uiso 1.00 1 d . . . C(22) C -0.073(4) -0.133(3) 0.570(3) 0.090(11) Uiso 1.00 1 d . . . C(23) C -0.139(4) -0.168(3) 0.457(3) 0.083(11) Uiso 1.00 1 d . . . C(24) C -0.054(6) -0.270(5) 0.442(4) 0.145(19) Uiso 1.00 1 d . . . C(25) C 0.068(4) -0.324(3) 0.497(3) 0.096(12) Uiso 1.00 1 d . . . C(26) C 0.165(6) -0.250(5) 0.590(5) 0.16(2) Uiso 1.00 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.106(3) 0.065(2) 0.119(3) 0.027(2) -0.003(2) -0.040(2) Br(2) 0.102(3) 0.093(3) 0.118(3) 0.026(2) -0.006(2) -0.030(2) Cu(1) 0.101(3) 0.061(3) 0.125(4) 0.034(2) -0.003(3) -0.035(2) Cu(2) 0.102(4) 0.072(3) 0.127(4) 0.039(2) -0.005(3) -0.040(3) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Br(1) Cu(1) 2.642(6) yes . . Br(2) Cu(2) 2.618(7) yes . . Cu(1) N(1) 2.12(3) yes . . Cu(1) N(2) 1.95(4) yes . . Cu(1) N(5) 2.00(3) yes . . Cu(1) N(6) 1.89(2) yes . . Cu(2) N(3) 2.13(3) yes . . Cu(2) N(4) 2.03(3) yes . . Cu(2) N(7) 2.03(3) yes . . Cu(2) N(8) 2.24(3) yes . . N(1) C(1) 1.20(8) yes . . N(1) C(5) 1.34(5) yes . . N(2) N(3) 1.41(5) yes . . N(2) C(6) 1.41(5) yes . . N(3) C(8) 1.09(3) yes . . N(4) C(9) 1.37(4) yes . . N(4) C(13) 1.11(6) yes . . N(5) C(14) 1.49(5) yes . . N(5) C(18) 1.43(6) yes . . N(6) N(7) 1.27(4) yes . . N(6) C(19) 1.32(5) yes . . N(7) C(21) 1.29(3) yes . . N(8) C(22) 1.47(5) yes . . N(8) C(26) 1.45(7) yes . . C(1) C(2) 1.36(7) yes . . C(2) C(3) 1.49(7) yes . . C(3) C(4) 1.57(8) yes . . C(4) C(5) 1.57(6) yes . . C(5) C(6) 1.59(4) yes . . C(6) C(7) 1.39(5) yes . . C(7) C(8) 1.34(4) yes . . C(8) C(9) 1.65(3) yes . . C(9) C(10) 1.45(4) yes . . C(9) C(13) 1.77(5) yes . . C(10) C(11) 1.54(7) yes . . C(11) C(12) 1.59(7) yes . . C(12) C(13) 1.45(7) yes . . C(14) C(15) 1.38(5) yes . . C(15) C(16) 1.46(5) yes . . C(16) C(17) 1.43(7) yes . . C(17) C(18) 1.42(8) yes . . C(18) C(19) 1.52(8) yes . . C(19) C(20) 1.25(5) yes . . C(20) C(21) 1.57(5) yes . . C(21) C(22) 1.61(4) yes . . C(22) C(23) 1.46(5) yes . . C(23) C(24) 1.53(7) yes . . C(24) C(25) 1.52(7) yes . . C(25) C(26) 1.50(6) yes . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Br(1) Cu(1) N(1) 96.3(10) yes . . . Br(1) Cu(1) N(2) 108.1(11) yes . . . Br(1) Cu(1) N(5) 96.9(10) yes . . . Br(1) Cu(1) N(6) 112.3(11) yes . . . N(1) Cu(1) N(2) 77.0(15) yes . . . N(1) Cu(1) N(5) 104.3(14) yes . . . N(1) Cu(1) N(6) 151.1(15) yes . . . N(2) Cu(1) N(5) 154.7(15) yes . . . N(2) Cu(1) N(6) 89.8(15) yes . . . N(5) Cu(1) N(6) 77.2(14) yes . . . Br(2) Cu(2) N(3) 112.1(9) yes . . . Br(2) Cu(2) N(4) 94.9(9) yes . . . Br(2) Cu(2) N(7) 107.6(9) yes . . . Br(2) Cu(2) N(8) 93.1(10) yes . . . N(3) Cu(2) N(4) 72.0(13) yes . . . N(3) Cu(2) N(7) 96.5(12) yes . . . N(3) Cu(2) N(8) 154.5(14) yes . . . N(4) Cu(2) N(7) 157.4(13) yes . . . N(4) Cu(2) N(8) 103.0(13) yes . . . N(7) Cu(2) N(8) 78.8(13) yes . . . Cu(1) N(1) C(1) 127(4) yes . . . Cu(1) N(1) C(5) 116(2) yes . . . C(1) N(1) C(5) 112(4) yes . . . Cu(1) N(2) N(3) 146(2) yes . . . Cu(1) N(2) C(6) 124(2) yes . . . N(3) N(2) C(6) 89(3) yes . . . Cu(2) N(3) N(2) 113(2) yes . . . Cu(2) N(3) C(8) 124(2) yes . . . N(2) N(3) C(8) 118(2) yes . . . Cu(2) N(4) C(9) 122(2) yes . . . Cu(2) N(4) C(13) 145(3) yes . . . C(9) N(4) C(13) 91(3) yes . . . Cu(1) N(5) C(14) 132(2) yes . . . Cu(1) N(5) C(18) 119(3) yes . . . C(14) N(5) C(18) 89(3) yes . . . Cu(1) N(6) N(7) 137(2) yes . . . Cu(1) N(6) C(19) 122(2) yes . . . N(7) N(6) C(19) 99(3) yes . . . Cu(2) N(7) N(6) 130(2) yes . . . Cu(2) N(7) C(21) 116(2) yes . . . N(6) N(7) C(21) 113(2) yes . . . Cu(2) N(8) C(22) 116(2) yes . . . Cu(2) N(8) C(26) 106(3) yes . . . C(22) N(8) C(26) 137(3) yes . . . N(1) C(1) C(2) 143(6) yes . . . C(1) C(2) C(3) 100(4) yes . . . C(2) C(3) C(4) 136(4) yes . . . C(3) C(4) C(5) 94(4) yes . . . N(1) C(5) C(4) 131(3) yes . . . N(1) C(5) C(6) 112(2) yes . . . C(4) C(5) C(6) 114(3) yes . . . N(2) C(6) C(5) 108(2) yes . . . N(2) C(6) C(7) 119(3) yes . . . C(5) C(6) C(7) 133(3) yes . . . C(6) C(7) C(8) 93(3) yes . . . N(3) C(8) C(7) 116(3) yes . . . N(3) C(8) C(9) 111(2) yes . . . C(7) C(8) C(9) 127(2) yes . . . N(4) C(9) C(8) 106(2) yes . . . N(4) C(9) C(10) 142(3) yes . . . N(4) C(9) C(13) 39(2) yes . . . C(8) C(9) C(10) 112(2) yes . . . C(8) C(9) C(13) 144(2) yes . . . C(10) C(9) C(13) 103(2) yes . . . C(9) C(10) C(11) 106(3) yes . . . C(10) C(11) C(12) 109(4) yes . . . C(11) C(12) C(13) 101(4) yes . . . N(4) C(13) C(9) 50(2) yes . . . N(4) C(13) C(12) 156(5) yes . . . C(9) C(13) C(12) 108(3) yes . . . N(5) C(14) C(15) 136(3) yes . . . C(14) C(15) C(16) 114(3) yes . . . C(15) C(16) C(17) 103(4) yes . . . C(16) C(17) C(18) 131(4) yes . . . N(5) C(18) C(17) 124(5) yes . . . N(5) C(18) C(19) 104(4) yes . . . C(17) C(18) C(19) 131(4) yes . . . N(6) C(19) C(18) 115(3) yes . . . N(6) C(19) C(20) 126(4) yes . . . C(18) C(19) C(20) 118(4) yes . . . C(19) C(20) C(21) 91(3) yes . . . N(7) C(21) C(20) 108(2) yes . . . N(7) C(21) C(22) 127(2) yes . . . C(20) C(21) C(22) 126(2) yes . . . N(8) C(22) C(21) 102(2) yes . . . N(8) C(22) C(23) 126(3) yes . . . C(21) C(22) C(23) 126(3) yes . . . C(22) C(23) C(24) 92(3) yes . . . C(23) C(24) C(25) 142(4) yes . . . C(24) C(25) C(26) 115(4) yes . . . N(8) C(26) C(25) 99(4) yes . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Br(1) Cu(1) N(1) C(1) 62(4) ? . . . . Br(1) Cu(1) N(1) C(5) -93(2) ? . . . . Br(1) Cu(1) N(2) N(3) -109(5) ? . . . . Br(1) Cu(1) N(2) C(6) 88(3) ? . . . . Br(1) Cu(1) N(5) C(14) -27(3) ? . . . . Br(1) Cu(1) N(5) C(18) 92(3) ? . . . . Br(1) Cu(1) N(6) N(7) 84(4) ? . . . . Br(1) Cu(1) N(6) C(19) -77(3) ? . . . . N(1) Cu(1) N(2) N(3) 158(5) ? . . . . N(1) Cu(1) N(2) C(6) -4(3) ? . . . . N(2) Cu(1) N(1) C(1) 169(5) ? . . . . N(2) Cu(1) N(1) C(5) 14(2) ? . . . . N(1) Cu(1) N(5) C(14) 72(3) ? . . . . N(1) Cu(1) N(5) C(18) -170(3) ? . . . . N(5) Cu(1) N(1) C(1) -37(5) ? . . . . N(5) Cu(1) N(1) C(5) 168(2) ? . . . . N(1) Cu(1) N(6) N(7) -87(5) ? . . . . N(1) Cu(1) N(6) C(19) 112(4) ? . . . . N(6) Cu(1) N(1) C(1) -127(5) ? . . . . N(6) Cu(1) N(1) C(5) 79(4) ? . . . . N(2) Cu(1) N(5) C(14) 161(3) ? . . . . N(2) Cu(1) N(5) C(18) -80(5) ? . . . . N(5) Cu(1) N(2) N(3) 62(7) ? . . . . N(5) Cu(1) N(2) C(6) -100(4) ? . . . . N(2) Cu(1) N(6) N(7) -25(4) ? . . . . N(2) Cu(1) N(6) C(19) 173(3) ? . . . . N(6) Cu(1) N(2) N(3) 4(5) ? . . . . N(6) Cu(1) N(2) C(6) -158(3) ? . . . . N(5) Cu(1) N(6) N(7) 177(4) ? . . . . N(5) Cu(1) N(6) C(19) 15(3) ? . . . . N(6) Cu(1) N(5) C(14) -138(3) ? . . . . N(6) Cu(1) N(5) C(18) -19(3) ? . . . . Br(2) Cu(2) N(3) N(2) 87(2) ? . . . . Br(2) Cu(2) N(3) C(8) -66(3) ? . . . . Br(2) Cu(2) N(4) C(9) 99(2) ? . . . . Br(2) Cu(2) N(4) C(13) -58(5) ? . . . . Br(2) Cu(2) N(7) N(6) -102(3) ? . . . . Br(2) Cu(2) N(7) C(21) 95(2) ? . . . . Br(2) Cu(2) N(8) C(22) -112(3) ? . . . . Br(2) Cu(2) N(8) C(26) 63(3) ? . . . . N(3) Cu(2) N(4) C(9) -13(2) ? . . . . N(3) Cu(2) N(4) C(13) -170(6) ? . . . . N(4) Cu(2) N(3) N(2) 175(2) ? . . . . N(4) Cu(2) N(3) C(8) 22(2) ? . . . . N(3) Cu(2) N(7) N(6) 14(3) ? . . . . N(3) Cu(2) N(7) C(21) -149(2) ? . . . . N(7) Cu(2) N(3) N(2) -25(2) ? . . . . N(7) Cu(2) N(3) C(8) -178(3) ? . . . . N(3) Cu(2) N(8) C(22) 76(4) ? . . . . N(3) Cu(2) N(8) C(26) -109(4) ? . . . . N(8) Cu(2) N(3) N(2) -102(4) ? . . . . N(8) Cu(2) N(3) C(8) 105(4) ? . . . . N(4) Cu(2) N(7) N(6) 72(4) ? . . . . N(4) Cu(2) N(7) C(21) -92(3) ? . . . . N(7) Cu(2) N(4) C(9) -75(4) ? . . . . N(7) Cu(2) N(4) C(13) 128(5) ? . . . . N(4) Cu(2) N(8) C(22) 152(3) ? . . . . N(4) Cu(2) N(8) C(26) -33(3) ? . . . . N(8) Cu(2) N(4) C(9) -167(2) ? . . . . N(8) Cu(2) N(4) C(13) 36(6) ? . . . . N(7) Cu(2) N(8) C(22) -5(3) ? . . . . N(7) Cu(2) N(8) C(26) 170(3) ? . . . . N(8) Cu(2) N(7) N(6) 169(3) ? . . . . N(8) Cu(2) N(7) C(21) 5(2) ? . . . . Cu(1) N(1) C(1) C(2) -160(8) ? . . . . Cu(1) N(1) C(5) C(4) 178(3) ? . . . . Cu(1) N(1) C(5) C(6) -20(3) ? . . . . C(1) N(1) C(5) C(4) 20(7) ? . . . . C(1) N(1) C(5) C(6) -178(4) ? . . . . C(5) N(1) C(1) C(2) -4(11) ? . . . . Cu(1) N(2) N(3) Cu(2) 19(6) ? . . . . Cu(1) N(2) N(3) C(8) 175(3) ? . . . . Cu(1) N(2) C(6) C(5) -4(4) ? . . . . Cu(1) N(2) C(6) C(7) 176(2) ? . . . . N(3) N(2) C(6) C(5) -175(2) ? . . . . N(3) N(2) C(6) C(7) 6(4) ? . . . . C(6) N(2) N(3) Cu(2) -175(2) ? . . . . C(6) N(2) N(3) C(8) -20(4) ? . . . . Cu(2) N(3) C(8) C(7) -179.3(18) ? . . . . Cu(2) N(3) C(8) C(9) -23(3) ? . . . . N(2) N(3) C(8) C(7) 29(4) ? . . . . N(2) N(3) C(8) C(9) -175(3) ? . . . . Cu(2) N(4) C(9) C(8) 7(3) ? . . . . Cu(2) N(4) C(9) C(10) -179(2) ? . . . . Cu(2) N(4) C(9) C(13) -167(4) ? . . . . Cu(2) N(4) C(13) C(9) 161(6) ? . . . . Cu(2) N(4) C(13) C(12) -174(7) ? . . . . C(9) N(4) C(13) C(12) 25(11) ? . . . . C(13) N(4) C(9) C(8) 174(3) ? . . . . C(13) N(4) C(9) C(10) -12(6) ? . . . . Cu(1) N(5) C(14) C(15) -174(3) ? . . . . Cu(1) N(5) C(18) C(17) -175(4) ? . . . . Cu(1) N(5) C(18) C(19) 19(5) ? . . . . C(14) N(5) C(18) C(17) -35(6) ? . . . . C(14) N(5) C(18) C(19) 158(4) ? . . . . C(18) N(5) C(14) C(15) 57(6) ? . . . . Cu(1) N(6) N(7) Cu(2) 15(6) ? . . . . Cu(1) N(6) N(7) C(21) 179(2) ? . . . . Cu(1) N(6) C(19) C(18) -9(5) ? . . . . Cu(1) N(6) C(19) C(20) -176(4) ? . . . . N(7) N(6) C(19) C(18) -176(4) ? . . . . N(7) N(6) C(19) C(20) 17(6) ? . . . . C(19) N(6) N(7) Cu(2) 179(2) ? . . . . C(19) N(6) N(7) C(21) -17(4) ? . . . . Cu(2) N(7) C(21) C(20) -179.6(19) ? . . . . Cu(2) N(7) C(21) C(22) -5(3) ? . . . . N(6) N(7) C(21) C(20) 14(4) ? . . . . N(6) N(7) C(21) C(22) -172(3) ? . . . . Cu(2) N(8) C(22) C(21) 4(3) ? . . . . Cu(2) N(8) C(22) C(23) 158(3) ? . . . . Cu(2) N(8) C(26) C(25) 173(3) ? . . . . C(22) N(8) C(26) C(25) -13(8) ? . . . . C(26) N(8) C(22) C(21) -169(5) ? . . . . C(26) N(8) C(22) C(23) -15(8) ? . . . . N(1) C(1) C(2) C(3) 0(11) ? . . . . C(1) C(2) C(3) C(4) -11(8) ? . . . . C(2) C(3) C(4) C(5) 19(7) ? . . . . C(3) C(4) C(5) N(1) -23(5) ? . . . . C(3) C(4) C(5) C(6) 175(3) ? . . . . N(1) C(5) C(6) N(2) 15(4) ? . . . . N(1) C(5) C(6) C(7) -165(4) ? . . . . C(4) C(5) C(6) N(2) -179(3) ? . . . . C(4) C(5) C(6) C(7) 0(5) ? . . . . N(2) C(6) C(7) C(8) 5(4) ? . . . . C(5) C(6) C(7) C(8) -174(3) ? . . . . C(6) C(7) C(8) N(3) -19(3) ? . . . . C(6) C(7) C(8) C(9) -171(2) ? . . . . N(3) C(8) C(9) N(4) 10(3) ? . . . . N(3) C(8) C(9) C(10) -166(3) ? . . . . N(3) C(8) C(9) C(13) 16(5) ? . . . . C(7) C(8) C(9) N(4) 162(3) ? . . . . C(7) C(8) C(9) C(10) -13(4) ? . . . . C(7) C(8) C(9) C(13) 168(4) ? . . . . N(4) C(9) C(10) C(11) 27(6) ? . . . . N(4) C(9) C(13) C(12) -170(5) ? . . . . C(8) C(9) C(10) C(11) -159(3) ? . . . . C(8) C(9) C(13) N(4) -9(5) ? . . . . C(8) C(9) C(13) C(12) -179(3) ? . . . . C(10) C(9) C(13) N(4) 173(3) ? . . . . C(10) C(9) C(13) C(12) 3(4) ? . . . . C(13) C(9) C(10) C(11) 20(3) ? . . . . C(9) C(10) C(11) C(12) -37(5) ? . . . . C(10) C(11) C(12) C(13) 37(5) ? . . . . C(11) C(12) C(13) N(4) -43(12) ? . . . . C(11) C(12) C(13) C(9) -23(4) ? . . . . N(5) C(14) C(15) C(16) -35(7) ? . . . . C(14) C(15) C(16) C(17) -12(5) ? . . . . C(15) C(16) C(17) C(18) 24(7) ? . . . . C(16) C(17) C(18) N(5) 5(10) ? . . . . C(16) C(17) C(18) C(19) 168(5) ? . . . . N(5) C(18) C(19) N(6) -7(6) ? . . . . N(5) C(18) C(19) C(20) 161(4) ? . . . . C(17) C(18) C(19) N(6) -172(5) ? . . . . C(17) C(18) C(19) C(20) -4(9) ? . . . . N(6) C(19) C(20) C(21) -8(6) ? . . . . C(18) C(19) C(20) C(21) -175(4) ? . . . . C(19) C(20) C(21) N(7) -4(4) ? . . . . C(19) C(20) C(21) C(22) -178(3) ? . . . . N(7) C(21) C(22) N(8) 1(3) ? . . . . N(7) C(21) C(22) C(23) -154(3) ? . . . . C(20) C(21) C(22) N(8) 174(3) ? . . . . C(20) C(21) C(22) C(23) 20(5) ? . . . . N(8) C(22) C(23) C(24) 22(5) ? . . . . C(21) C(22) C(23) C(24) 171(3) ? . . . . C(22) C(23) C(24) C(25) -9(8) ? . . . . C(23) C(24) C(25) C(26) -16(10) ? . . . . C(24) C(25) C(26) N(8) 22(6) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Br(1) C(11) 3.58(6) ? . 2_657 N(1) N(4) 3.57(4) ? . 2_557 N(2) C(11) 3.19(6) ? . 2_657 N(4) N(1) 3.57(4) ? . 2_557 N(5) C(10) 3.15(4) ? . 2_557 N(6) C(7) 3.46(6) ? . 2_557 N(7) C(23) 3.41(5) ? . 2_556 N(8) C(3) 3.55(7) ? . 2_557 N(8) C(4) 3.27(7) ? . 2_557 C(1) C(14) 3.46(8) ? . 2_567 C(2) C(14) 3.09(5) ? . 2_567 C(2) C(15) 3.35(5) ? . 2_567 C(3) N(8) 3.55(7) ? . 2_557 C(3) C(15) 3.54(8) ? . 2_567 C(4) N(8) 3.27(7) ? . 2_557 C(4) C(21) 3.49(6) ? . 2_557 C(4) C(22) 3.08(7) ? . 2_557 C(5) C(11) 3.41(7) ? . 2_657 C(6) C(11) 3.03(7) ? . 2_657 C(7) N(6) 3.46(6) ? . 2_557 C(7) C(9) 3.57(5) ? . 2_657 C(7) C(11) 3.43(8) ? . 2_657 C(8) C(9) 3.51(3) ? . 2_657 C(8) C(10) 3.35(3) ? . 2_657 C(8) C(11) 3.51(6) ? . 2_657 C(9) C(7) 3.57(5) ? . 2_657 C(9) C(8) 3.51(3) ? . 2_657 C(10) N(5) 3.15(4) ? . 2_557 C(10) C(8) 3.35(3) ? . 2_657 C(10) C(18) 3.56(7) ? . 2_557 C(11) Br(1) 3.58(6) ? . 2_657 C(11) N(2) 3.19(6) ? . 2_657 C(11) C(5) 3.41(7) ? . 2_657 C(11) C(6) 3.03(7) ? . 2_657 C(11) C(7) 3.43(8) ? . 2_657 C(11) C(8) 3.51(6) ? . 2_657 C(14) C(1) 3.46(8) ? . 2_567 C(14) C(2) 3.09(5) ? . 2_567 C(15) C(2) 3.35(5) ? . 2_567 C(15) C(3) 3.54(8) ? . 2_567 C(18) C(10) 3.56(7) ? . 2_557 C(19) C(24) 3.42(8) ? . 2_556 C(21) C(4) 3.49(6) ? . 2_557 C(21) C(23) 3.49(4) ? . 2_556 C(22) C(4) 3.08(7) ? . 2_557 C(23) N(7) 3.41(5) ? . 2_556 C(23) C(21) 3.49(4) ? . 2_556 C(24) C(19) 3.42(8) ? . 2_556 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data__Cu2(bpypz)2Br2(H2O)3 _database_code_depnum_ccdc_archive 'CCDC 704683' #TrackingRef 'Cu2(bpypz)2Br2(H2O)3.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C26 H24 Br2 Cu2 N8 O3 ' _chemical_formula_moiety 'C26 H24 Br2 Cu2 N8 O3 ' _chemical_formula_weight 783.43 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 9.900(4) _cell_length_b 11.605(4) _cell_length_c 12.558(5) _cell_angle_alpha 104.791(10) _cell_angle_beta 89.286(9) _cell_angle_gamma 97.093(10) _cell_volume 1384.0(10) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3608 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 200 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.880 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776.00 _exptl_absorpt_coefficient_mu 4.478 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.355 _exptl_absorpt_correction_T_max 0.639 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 200 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 13606 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.981 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6225 _reflns_number_gt 4847 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0941 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 6225 _refine_ls_number_parameters 393 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0423P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.91 _refine_diff_density_min -0.71 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Br Br -0.290 2.459 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Br(1) Br 0.4365(2) 0.1581(2) 0.81763(19) 0.0392(5) Uani 0.25 1 d P . . Br(2) Br 0.08207(3) 0.33896(3) 0.63234(3) 0.02934(10) Uani 1.00 1 d . . . Br(3) Br -0.0717(2) 0.07370(18) 0.93627(13) 0.0461(3) Uani 0.50 1 d P . . Br(4) Br 0.5941(3) 0.0331(4) 0.9196(4) 0.0436(8) Uani 0.25 1 d P . . Cu(1) Cu 0.58869(4) 0.30925(3) 0.71512(3) 0.02458(11) Uani 1.00 1 d . . . Cu(2) Cu 0.31079(4) 0.45452(3) 0.57502(3) 0.02498(11) Uani 1.00 1 d . . . O(2) O 0.1622(3) 0.1631(2) 0.7861(2) 0.0764(10) Uani 1.00 1 d . . . O(1) O 0.4521(6) 0.1881(5) 0.7894(5) 0.0547(17) Uani 0.75 1 d P . . O(3) O -0.0439(12) 0.0980(10) 0.9349(10) 0.048(4) Uiso 0.50 1 d P . . O(4) O 0.6023(10) 0.0323(9) 0.9038(9) 0.068(3) Uani 0.75 1 d P . . N(1) N 0.6913(2) 0.3887(2) 0.8648(2) 0.0292(6) Uani 1.00 1 d . . . N(2) N 0.5093(2) 0.4596(2) 0.7593(2) 0.0258(5) Uani 1.00 1 d . . . N(3) N 0.4177(2) 0.5076(2) 0.7129(2) 0.0255(5) Uani 1.00 1 d . . . N(4) N 0.2476(2) 0.6218(2) 0.6389(2) 0.0268(5) Uani 1.00 1 d . . . N(5) N 0.6957(2) 0.1687(2) 0.6340(2) 0.0273(5) Uani 1.00 1 d . . . N(6) N 0.5097(2) 0.2734(2) 0.5668(2) 0.0265(5) Uani 1.00 1 d . . . N(7) N 0.4168(2) 0.3207(2) 0.5210(2) 0.0275(5) Uani 1.00 1 d . . . N(8) N 0.2540(2) 0.4033(2) 0.4067(2) 0.0291(6) Uani 1.00 1 d . . . C(1) C 0.7823(3) 0.3450(3) 0.9170(3) 0.0401(8) Uani 1.00 1 d . . . C(2) C 0.8437(3) 0.4086(3) 1.0167(3) 0.0400(8) Uani 1.00 1 d . . . C(3) C 0.8115(3) 0.5212(3) 1.0654(2) 0.0365(8) Uani 1.00 1 d . . . C(4) C 0.7152(3) 0.5671(3) 1.0144(2) 0.0319(7) Uani 1.00 1 d . . . C(5) C 0.6562(3) 0.4993(2) 0.9147(2) 0.0258(6) Uani 1.00 1 d . . . C(6) C 0.5536(3) 0.5382(2) 0.8552(2) 0.0259(6) Uani 1.00 1 d . . . C(7) C 0.4873(3) 0.6404(2) 0.8709(2) 0.0277(7) Uani 1.00 1 d . . . C(8) C 0.4024(3) 0.6163(2) 0.7790(2) 0.0253(6) Uani 1.00 1 d . . . C(9) C 0.3039(3) 0.6805(2) 0.7396(2) 0.0257(6) Uani 1.00 1 d . . . C(10) C 0.2679(3) 0.7900(3) 0.7989(2) 0.0344(7) Uani 1.00 1 d . . . C(11) C 0.1735(3) 0.8441(3) 0.7539(3) 0.0390(8) Uani 1.00 1 d . . . C(12) C 0.1163(3) 0.7850(3) 0.6523(3) 0.0383(8) Uani 1.00 1 d . . . C(13) C 0.1546(3) 0.6750(3) 0.5983(3) 0.0342(7) Uani 1.00 1 d . . . C(14) C 0.7934(3) 0.1197(3) 0.6731(3) 0.0386(8) Uani 1.00 1 d . . . C(15) C 0.8488(3) 0.0204(3) 0.6112(3) 0.0383(8) Uani 1.00 1 d . . . C(16) C 0.8038(3) -0.0309(3) 0.5053(3) 0.0346(8) Uani 1.00 1 d . . . C(17) C 0.7037(3) 0.0188(2) 0.4631(2) 0.0295(7) Uani 1.00 1 d . . . C(18) C 0.6519(2) 0.1182(2) 0.5285(2) 0.0239(6) Uani 1.00 1 d . . . C(19) C 0.5474(3) 0.1785(2) 0.4906(2) 0.0240(6) Uani 1.00 1 d . . . C(20) C 0.4777(3) 0.1643(2) 0.3925(2) 0.0263(6) Uani 1.00 1 d . . . C(21) C 0.3960(3) 0.2561(2) 0.4155(2) 0.0248(6) Uani 1.00 1 d . . . C(22) C 0.2976(3) 0.2975(2) 0.3530(2) 0.0270(6) Uani 1.00 1 d . . . C(23) C 0.2503(3) 0.2359(3) 0.2482(2) 0.0340(7) Uani 1.00 1 d . . . C(24) C 0.1596(3) 0.2834(3) 0.1944(2) 0.0370(8) Uani 1.00 1 d . . . C(25) C 0.1192(3) 0.3929(3) 0.2465(3) 0.0388(8) Uani 1.00 1 d . . . C(26) C 0.1679(3) 0.4495(3) 0.3519(3) 0.0378(8) Uani 1.00 1 d . . . H(1) H 0.8057 0.2670 0.8841 0.048 Uiso 1.00 1 c R . . H(2) H 0.9077 0.3744 1.0511 0.048 Uiso 1.00 1 c R . . H(3) H 0.8544 0.5669 1.1328 0.044 Uiso 1.00 1 c R . . H(4) H 0.6897 0.6443 1.0474 0.038 Uiso 1.00 1 c R . . H(5) H 0.4979 0.7103 0.9307 0.033 Uiso 1.00 1 c R . . H(6) H 0.3073 0.8276 0.8697 0.041 Uiso 1.00 1 c R . . H(7) H 0.1490 0.9201 0.7923 0.047 Uiso 1.00 1 c R . . H(8) H 0.0510 0.8197 0.6197 0.046 Uiso 1.00 1 c R . . H(9) H 0.1130 0.6349 0.5287 0.041 Uiso 1.00 1 c R . . H(10) H 0.8262 0.1546 0.7465 0.046 Uiso 1.00 1 c R . . H(11) H 0.9176 -0.0119 0.6423 0.046 Uiso 1.00 1 c R . . H(12) H 0.8405 -0.0991 0.4618 0.042 Uiso 1.00 1 c R . . H(13) H 0.6705 -0.0149 0.3897 0.035 Uiso 1.00 1 c R . . H(14) H 0.4842 0.1053 0.3250 0.032 Uiso 1.00 1 c R . . H(15) H 0.2804 0.1610 0.2134 0.041 Uiso 1.00 1 c R . . H(16) H 0.1255 0.2414 0.1228 0.044 Uiso 1.00 1 c R . . H(17) H 0.0589 0.4291 0.2105 0.047 Uiso 1.00 1 c R . . H(18) H 0.1390 0.5247 0.3874 0.045 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.0423(10) 0.0379(11) 0.0364(11) 0.0027(8) 0.0015(8) 0.0087(8) Br(2) 0.02846(18) 0.02896(18) 0.03401(19) 0.00612(13) -0.00168(13) 0.01295(14) Br(3) 0.0543(8) 0.0519(7) 0.0405(6) 0.0203(7) 0.0033(5) 0.0205(5) Br(4) 0.0340(12) 0.057(2) 0.0352(11) 0.0066(11) 0.0008(9) 0.0041(10) Cu(1) 0.0258(2) 0.0257(2) 0.0231(2) 0.00923(15) -0.00251(15) 0.00479(16) Cu(2) 0.0261(2) 0.0255(2) 0.0253(2) 0.00956(15) -0.00190(15) 0.00710(16) O(2) 0.115(2) 0.055(2) 0.068(2) 0.0166(18) -0.0213(19) 0.0281(17) O(1) 0.045(2) 0.062(3) 0.073(4) 0.006(2) 0.010(2) 0.046(2) O(4) 0.090(5) 0.027(4) 0.084(6) 0.014(3) 0.031(3) 0.005(3) N(1) 0.0302(14) 0.0299(14) 0.0285(15) 0.0056(11) -0.0046(11) 0.0083(12) N(2) 0.0262(13) 0.0258(13) 0.0253(14) 0.0091(10) -0.0024(10) 0.0034(11) N(3) 0.0254(13) 0.0252(13) 0.0266(14) 0.0077(10) -0.0018(10) 0.0055(11) N(4) 0.0267(13) 0.0236(13) 0.0326(15) 0.0073(10) 0.0019(11) 0.0099(11) N(5) 0.0256(13) 0.0310(14) 0.0282(14) 0.0117(11) 0.0021(11) 0.0089(12) N(6) 0.0304(14) 0.0263(14) 0.0246(14) 0.0112(11) -0.0017(11) 0.0061(11) N(7) 0.0291(14) 0.0307(14) 0.0245(14) 0.0119(11) -0.0011(11) 0.0063(11) N(8) 0.0271(14) 0.0365(15) 0.0264(14) 0.0072(11) 0.0005(11) 0.0117(12) C(1) 0.049(2) 0.039(2) 0.034(2) 0.0164(16) -0.0104(16) 0.0059(16) C(2) 0.0355(19) 0.050(2) 0.036(2) 0.0092(16) -0.0118(15) 0.0112(17) C(3) 0.0360(19) 0.044(2) 0.0284(18) 0.0017(15) -0.0040(14) 0.0089(16) C(4) 0.0327(18) 0.0343(18) 0.0278(18) 0.0057(14) -0.0037(13) 0.0051(14) C(5) 0.0279(16) 0.0266(16) 0.0225(16) 0.0006(12) 0.0011(12) 0.0071(13) C(6) 0.0250(16) 0.0271(16) 0.0254(16) 0.0035(12) 0.0008(12) 0.0065(13) C(7) 0.0299(17) 0.0252(16) 0.0264(17) 0.0063(13) 0.0014(13) 0.0022(13) C(8) 0.0231(15) 0.0246(16) 0.0288(17) 0.0051(12) 0.0041(12) 0.0074(13) C(9) 0.0245(15) 0.0228(15) 0.0320(17) 0.0047(12) 0.0046(13) 0.0104(13) C(10) 0.0374(19) 0.0287(17) 0.037(2) 0.0089(14) 0.0052(15) 0.0056(15) C(11) 0.041(2) 0.0272(18) 0.055(2) 0.0180(15) 0.0120(17) 0.0156(17) C(12) 0.0367(19) 0.036(2) 0.051(2) 0.0168(15) 0.0059(16) 0.0205(18) C(13) 0.0339(18) 0.0365(19) 0.037(2) 0.0122(15) -0.0006(15) 0.0151(16) C(14) 0.040(2) 0.044(2) 0.035(2) 0.0219(16) -0.0053(15) 0.0062(16) C(15) 0.0343(19) 0.041(2) 0.044(2) 0.0194(16) -0.0004(16) 0.0117(17) C(16) 0.0346(18) 0.0280(17) 0.044(2) 0.0147(14) 0.0140(15) 0.0103(16) C(17) 0.0374(18) 0.0284(17) 0.0256(17) 0.0106(14) 0.0048(13) 0.0093(14) C(18) 0.0235(15) 0.0234(15) 0.0267(16) 0.0041(12) 0.0079(12) 0.0099(13) C(19) 0.0261(15) 0.0237(15) 0.0238(16) 0.0057(12) 0.0047(12) 0.0076(13) C(20) 0.0300(16) 0.0276(16) 0.0222(16) 0.0067(13) 0.0042(12) 0.0064(13) C(21) 0.0259(15) 0.0274(16) 0.0219(16) 0.0028(12) 0.0008(12) 0.0080(13) C(22) 0.0247(15) 0.0345(17) 0.0259(17) 0.0048(13) 0.0035(12) 0.0150(14) C(23) 0.0362(19) 0.039(2) 0.0274(18) 0.0058(15) 0.0014(14) 0.0094(15) C(24) 0.0348(19) 0.052(2) 0.0262(18) 0.0046(16) -0.0036(14) 0.0146(16) C(25) 0.0314(18) 0.057(2) 0.034(2) 0.0092(16) -0.0046(15) 0.0202(18) C(26) 0.0374(19) 0.046(2) 0.036(2) 0.0180(16) -0.0024(15) 0.0163(17) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Br(1) Cu(1) 2.730(2) yes . . Br(1) O(1) 0.564(7) yes . . Br(2) Cu(2) 2.6733(4) yes . . Br(3) O(3) 0.373(12) yes . . Br(4) O(4) 0.212(12) yes . . Cu(1) O(1) 2.201(6) yes . . Cu(1) N(1) 2.085(2) yes . . Cu(1) N(2) 1.950(2) yes . . Cu(1) N(5) 2.091(2) yes . . Cu(1) N(6) 1.953(2) yes . . Cu(2) N(3) 1.958(2) yes . . Cu(2) N(4) 2.073(2) yes . . Cu(2) N(7) 1.955(2) yes . . Cu(2) N(8) 2.108(2) yes . . N(1) C(1) 1.340(5) yes . . N(1) C(5) 1.362(4) yes . . N(2) N(3) 1.333(3) yes . . N(2) C(6) 1.352(3) yes . . N(3) C(8) 1.347(3) yes . . N(4) C(9) 1.362(3) yes . . N(4) C(13) 1.342(4) yes . . N(5) C(14) 1.338(4) yes . . N(5) C(18) 1.356(3) yes . . N(6) N(7) 1.334(4) yes . . N(6) C(19) 1.349(3) yes . . N(7) C(21) 1.350(3) yes . . N(8) C(22) 1.360(4) yes . . N(8) C(26) 1.342(5) yes . . C(1) C(2) 1.386(4) yes . . C(2) C(3) 1.368(5) yes . . C(3) C(4) 1.385(5) yes . . C(4) C(5) 1.389(4) yes . . C(5) C(6) 1.448(4) yes . . C(6) C(7) 1.396(4) yes . . C(7) C(8) 1.385(4) yes . . C(8) C(9) 1.459(4) yes . . C(9) C(10) 1.385(4) yes . . C(10) C(11) 1.388(5) yes . . C(11) C(12) 1.376(5) yes . . C(12) C(13) 1.380(4) yes . . C(14) C(15) 1.387(4) yes . . C(15) C(16) 1.366(4) yes . . C(16) C(17) 1.381(5) yes . . C(17) C(18) 1.385(4) yes . . C(18) C(19) 1.467(4) yes . . C(19) C(20) 1.383(4) yes . . C(20) C(21) 1.386(4) yes . . C(21) C(22) 1.458(4) yes . . C(22) C(23) 1.384(4) yes . . C(23) C(24) 1.375(5) yes . . C(24) C(25) 1.378(5) yes . . C(25) C(26) 1.381(4) yes . . C(1) H(1) 0.950 no . . C(2) H(2) 0.950 no . . C(3) H(3) 0.950 no . . C(4) H(4) 0.950 no . . C(7) H(5) 0.950 no . . C(10) H(6) 0.950 no . . C(11) H(7) 0.950 no . . C(12) H(8) 0.950 no . . C(13) H(9) 0.950 no . . C(14) H(10) 0.950 no . . C(15) H(11) 0.950 no . . C(16) H(12) 0.950 no . . C(17) H(13) 0.950 no . . C(20) H(14) 0.950 no . . C(23) H(15) 0.950 no . . C(24) H(16) 0.950 no . . C(25) H(17) 0.950 no . . C(26) H(18) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cu(1) Br(1) O(1) 18.2(6) yes . . . Br(1) Cu(1) O(1) 4.60(18) yes . . . Br(1) Cu(1) N(1) 88.16(9) yes . . . Br(1) Cu(1) N(2) 104.74(9) yes . . . Br(1) Cu(1) N(5) 90.05(9) yes . . . Br(1) Cu(1) N(6) 105.35(9) yes . . . O(1) Cu(1) N(1) 91.90(17) yes . . . O(1) Cu(1) N(2) 102.82(18) yes . . . O(1) Cu(1) N(5) 91.56(17) yes . . . O(1) Cu(1) N(6) 101.37(17) yes . . . N(1) Cu(1) N(2) 79.45(10) yes . . . N(1) Cu(1) N(5) 106.32(10) yes . . . N(1) Cu(1) N(6) 165.48(11) yes . . . N(2) Cu(1) N(5) 164.43(11) yes . . . N(2) Cu(1) N(6) 91.73(10) yes . . . N(5) Cu(1) N(6) 79.46(10) yes . . . Br(2) Cu(2) N(3) 103.12(7) yes . . . Br(2) Cu(2) N(4) 92.90(7) yes . . . Br(2) Cu(2) N(7) 100.61(7) yes . . . Br(2) Cu(2) N(8) 92.74(7) yes . . . N(3) Cu(2) N(4) 79.64(10) yes . . . N(3) Cu(2) N(7) 91.37(10) yes . . . N(3) Cu(2) N(8) 162.86(10) yes . . . N(4) Cu(2) N(7) 165.21(9) yes . . . N(4) Cu(2) N(8) 106.34(11) yes . . . N(7) Cu(2) N(8) 79.19(10) yes . . . Br(1) O(1) Cu(1) 157.2(8) yes . . . Cu(1) N(1) C(1) 129.0(2) yes . . . Cu(1) N(1) C(5) 113.3(2) yes . . . C(1) N(1) C(5) 117.7(2) yes . . . Cu(1) N(2) N(3) 133.58(17) yes . . . Cu(1) N(2) C(6) 117.9(2) yes . . . N(3) N(2) C(6) 108.5(2) yes . . . Cu(2) N(3) N(2) 133.92(18) yes . . . Cu(2) N(3) C(8) 117.6(2) yes . . . N(2) N(3) C(8) 108.5(2) yes . . . Cu(2) N(4) C(9) 113.7(2) yes . . . Cu(2) N(4) C(13) 129.1(2) yes . . . C(9) N(4) C(13) 117.1(2) yes . . . Cu(1) N(5) C(14) 129.3(2) yes . . . Cu(1) N(5) C(18) 113.3(2) yes . . . C(14) N(5) C(18) 117.4(2) yes . . . Cu(1) N(6) N(7) 133.57(18) yes . . . Cu(1) N(6) C(19) 118.0(2) yes . . . N(7) N(6) C(19) 108.3(2) yes . . . Cu(2) N(7) N(6) 133.92(18) yes . . . Cu(2) N(7) C(21) 117.9(2) yes . . . N(6) N(7) C(21) 108.2(2) yes . . . Cu(2) N(8) C(22) 112.3(2) yes . . . Cu(2) N(8) C(26) 129.5(2) yes . . . C(22) N(8) C(26) 117.4(2) yes . . . N(1) C(1) C(2) 122.8(3) yes . . . C(1) C(2) C(3) 119.5(3) yes . . . C(2) C(3) C(4) 118.7(3) yes . . . C(3) C(4) C(5) 119.5(3) yes . . . N(1) C(5) C(4) 121.7(3) yes . . . N(1) C(5) C(6) 114.3(2) yes . . . C(4) C(5) C(6) 124.0(2) yes . . . N(2) C(6) C(5) 115.0(2) yes . . . N(2) C(6) C(7) 109.2(2) yes . . . C(5) C(6) C(7) 135.7(2) yes . . . C(6) C(7) C(8) 103.9(2) yes . . . N(3) C(8) C(7) 109.9(2) yes . . . N(3) C(8) C(9) 115.1(2) yes . . . C(7) C(8) C(9) 135.0(2) yes . . . N(4) C(9) C(8) 113.9(2) yes . . . N(4) C(9) C(10) 122.4(3) yes . . . C(8) C(9) C(10) 123.7(2) yes . . . C(9) C(10) C(11) 119.3(3) yes . . . C(10) C(11) C(12) 118.4(3) yes . . . C(11) C(12) C(13) 119.4(3) yes . . . N(4) C(13) C(12) 123.3(3) yes . . . N(5) C(14) C(15) 122.8(3) yes . . . C(14) C(15) C(16) 119.7(3) yes . . . C(15) C(16) C(17) 118.4(3) yes . . . C(16) C(17) C(18) 119.6(2) yes . . . N(5) C(18) C(17) 122.2(3) yes . . . N(5) C(18) C(19) 114.2(2) yes . . . C(17) C(18) C(19) 123.6(2) yes . . . N(6) C(19) C(18) 114.7(2) yes . . . N(6) C(19) C(20) 109.9(2) yes . . . C(18) C(19) C(20) 135.4(2) yes . . . C(19) C(20) C(21) 103.8(2) yes . . . N(7) C(21) C(20) 109.8(2) yes . . . N(7) C(21) C(22) 115.0(2) yes . . . C(20) C(21) C(22) 135.1(2) yes . . . N(8) C(22) C(21) 114.3(2) yes . . . N(8) C(22) C(23) 121.8(3) yes . . . C(21) C(22) C(23) 123.9(2) yes . . . C(22) C(23) C(24) 119.9(3) yes . . . C(23) C(24) C(25) 118.6(3) yes . . . C(24) C(25) C(26) 119.0(3) yes . . . N(8) C(26) C(25) 123.2(3) yes . . . N(1) C(1) H(1) 118.6 no . . . C(2) C(1) H(1) 118.6 no . . . C(1) C(2) H(2) 120.2 no . . . C(3) C(2) H(2) 120.2 no . . . C(2) C(3) H(3) 120.7 no . . . C(4) C(3) H(3) 120.7 no . . . C(3) C(4) H(4) 120.3 no . . . C(5) C(4) H(4) 120.3 no . . . C(6) C(7) H(5) 128.1 no . . . C(8) C(7) H(5) 128.1 no . . . C(9) C(10) H(6) 120.3 no . . . C(11) C(10) H(6) 120.3 no . . . C(10) C(11) H(7) 120.8 no . . . C(12) C(11) H(7) 120.8 no . . . C(11) C(12) H(8) 120.3 no . . . C(13) C(12) H(8) 120.3 no . . . N(4) C(13) H(9) 118.3 no . . . C(12) C(13) H(9) 118.3 no . . . N(5) C(14) H(10) 118.6 no . . . C(15) C(14) H(10) 118.6 no . . . C(14) C(15) H(11) 120.2 no . . . C(16) C(15) H(11) 120.2 no . . . C(15) C(16) H(12) 120.8 no . . . C(17) C(16) H(12) 120.8 no . . . C(16) C(17) H(13) 120.2 no . . . C(18) C(17) H(13) 120.2 no . . . C(19) C(20) H(14) 128.1 no . . . C(21) C(20) H(14) 128.1 no . . . C(22) C(23) H(15) 120.1 no . . . C(24) C(23) H(15) 120.1 no . . . C(23) C(24) H(16) 120.7 no . . . C(25) C(24) H(16) 120.7 no . . . C(24) C(25) H(17) 120.5 no . . . C(26) C(25) H(17) 120.5 no . . . N(8) C(26) H(18) 118.4 no . . . C(25) C(26) H(18) 118.4 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(1) Br(1) Cu(1) N(1) 144.5(19) ? . . . . O(1) Br(1) Cu(1) N(2) 65.9(19) ? . . . . O(1) Br(1) Cu(1) N(5) -109.2(19) ? . . . . O(1) Br(1) Cu(1) N(6) -30.1(19) ? . . . . Br(1) Cu(1) N(1) C(1) 72.3(3) ? . . . . Br(1) Cu(1) N(1) C(5) -106.4(2) ? . . . . Br(1) Cu(1) N(2) N(3) -95.9(2) ? . . . . Br(1) Cu(1) N(2) C(6) 86.0(2) ? . . . . Br(1) Cu(1) N(5) C(14) -75.9(2) ? . . . . Br(1) Cu(1) N(5) C(18) 100.3(2) ? . . . . Br(1) Cu(1) N(6) N(7) 94.3(2) ? . . . . Br(1) Cu(1) N(6) C(19) -82.1(2) ? . . . . O(1) Cu(1) N(1) C(1) 75.0(3) ? . . . . O(1) Cu(1) N(1) C(5) -103.7(2) ? . . . . N(1) Cu(1) O(1) Br(1) -35.5(19) ? . . . . O(1) Cu(1) N(2) N(3) -91.6(3) ? . . . . O(1) Cu(1) N(2) C(6) 90.4(2) ? . . . . N(2) Cu(1) O(1) Br(1) -115.1(19) ? . . . . O(1) Cu(1) N(5) C(14) -80.2(3) ? . . . . O(1) Cu(1) N(5) C(18) 95.9(2) ? . . . . N(5) Cu(1) O(1) Br(1) 70.9(19) ? . . . . O(1) Cu(1) N(6) N(7) 92.0(3) ? . . . . O(1) Cu(1) N(6) C(19) -84.5(2) ? . . . . N(6) Cu(1) O(1) Br(1) 150.4(19) ? . . . . N(1) Cu(1) N(2) N(3) 178.8(2) ? . . . . N(1) Cu(1) N(2) C(6) 0.8(2) ? . . . . N(2) Cu(1) N(1) C(1) 177.7(3) ? . . . . N(2) Cu(1) N(1) C(5) -1.0(2) ? . . . . N(1) Cu(1) N(5) C(14) 12.2(3) ? . . . . N(1) Cu(1) N(5) C(18) -171.6(2) ? . . . . N(5) Cu(1) N(1) C(1) -17.2(3) ? . . . . N(5) Cu(1) N(1) C(5) 164.1(2) ? . . . . N(1) Cu(1) N(6) N(7) -63.6(5) ? . . . . N(1) Cu(1) N(6) C(19) 119.9(4) ? . . . . N(6) Cu(1) N(1) C(1) -128.9(4) ? . . . . N(6) Cu(1) N(1) C(5) 52.4(5) ? . . . . N(2) Cu(1) N(5) C(14) 122.1(4) ? . . . . N(2) Cu(1) N(5) C(18) -61.7(4) ? . . . . N(5) Cu(1) N(2) N(3) 65.5(4) ? . . . . N(5) Cu(1) N(2) C(6) -112.6(3) ? . . . . N(2) Cu(1) N(6) N(7) -11.5(2) ? . . . . N(2) Cu(1) N(6) C(19) 172.1(2) ? . . . . N(6) Cu(1) N(2) N(3) 10.5(2) ? . . . . N(6) Cu(1) N(2) C(6) -167.6(2) ? . . . . N(5) Cu(1) N(6) N(7) -178.5(2) ? . . . . N(5) Cu(1) N(6) C(19) 5.0(2) ? . . . . N(6) Cu(1) N(5) C(14) 178.5(3) ? . . . . N(6) Cu(1) N(5) C(18) -5.3(2) ? . . . . Br(2) Cu(2) N(3) N(2) 90.9(2) ? . . . . Br(2) Cu(2) N(3) C(8) -90.3(2) ? . . . . Br(2) Cu(2) N(4) C(9) 100.9(2) ? . . . . Br(2) Cu(2) N(4) C(13) -74.5(2) ? . . . . Br(2) Cu(2) N(7) N(6) -94.3(2) ? . . . . Br(2) Cu(2) N(7) C(21) 84.4(2) ? . . . . Br(2) Cu(2) N(8) C(22) -90.1(2) ? . . . . Br(2) Cu(2) N(8) C(26) 79.3(2) ? . . . . N(3) Cu(2) N(4) C(9) -1.9(2) ? . . . . N(3) Cu(2) N(4) C(13) -177.3(3) ? . . . . N(4) Cu(2) N(3) N(2) -178.5(2) ? . . . . N(4) Cu(2) N(3) C(8) 0.3(2) ? . . . . N(3) Cu(2) N(7) N(6) 9.3(2) ? . . . . N(3) Cu(2) N(7) C(21) -172.0(2) ? . . . . N(7) Cu(2) N(3) N(2) -10.3(2) ? . . . . N(7) Cu(2) N(3) C(8) 168.4(2) ? . . . . N(3) Cu(2) N(8) C(22) 67.7(4) ? . . . . N(3) Cu(2) N(8) C(26) -122.8(4) ? . . . . N(8) Cu(2) N(3) N(2) -66.3(5) ? . . . . N(8) Cu(2) N(3) C(8) 112.5(3) ? . . . . N(4) Cu(2) N(7) N(6) 61.4(6) ? . . . . N(4) Cu(2) N(7) C(21) -119.9(4) ? . . . . N(7) Cu(2) N(4) C(9) -55.2(5) ? . . . . N(7) Cu(2) N(4) C(13) 129.3(4) ? . . . . N(4) Cu(2) N(8) C(22) 176.1(2) ? . . . . N(4) Cu(2) N(8) C(26) -14.5(3) ? . . . . N(8) Cu(2) N(4) C(9) -165.4(2) ? . . . . N(8) Cu(2) N(4) C(13) 19.2(3) ? . . . . N(7) Cu(2) N(8) C(22) 10.2(2) ? . . . . N(7) Cu(2) N(8) C(26) 179.6(3) ? . . . . N(8) Cu(2) N(7) N(6) 174.9(2) ? . . . . N(8) Cu(2) N(7) C(21) -6.4(2) ? . . . . Cu(1) N(1) C(1) C(2) 179.6(2) ? . . . . Cu(1) N(1) C(5) C(4) -179.1(2) ? . . . . Cu(1) N(1) C(5) C(6) 1.1(3) ? . . . . C(1) N(1) C(5) C(4) 2.1(4) ? . . . . C(1) N(1) C(5) C(6) -177.8(2) ? . . . . C(5) N(1) C(1) C(2) -1.8(5) ? . . . . Cu(1) N(2) N(3) Cu(2) 0.3(4) ? . . . . Cu(1) N(2) N(3) C(8) -178.6(2) ? . . . . Cu(1) N(2) C(6) C(5) -0.5(3) ? . . . . Cu(1) N(2) C(6) C(7) 178.7(2) ? . . . . N(3) N(2) C(6) C(5) -179.0(2) ? . . . . N(3) N(2) C(6) C(7) 0.2(3) ? . . . . C(6) N(2) N(3) Cu(2) 178.4(2) ? . . . . C(6) N(2) N(3) C(8) -0.4(3) ? . . . . Cu(2) N(3) C(8) C(7) -178.6(2) ? . . . . Cu(2) N(3) C(8) C(9) 1.3(3) ? . . . . N(2) N(3) C(8) C(7) 0.5(3) ? . . . . N(2) N(3) C(8) C(9) -179.6(2) ? . . . . Cu(2) N(4) C(9) C(8) 3.0(3) ? . . . . Cu(2) N(4) C(9) C(10) -175.8(2) ? . . . . Cu(2) N(4) C(13) C(12) 176.4(2) ? . . . . C(9) N(4) C(13) C(12) 1.1(5) ? . . . . C(13) N(4) C(9) C(8) 179.1(2) ? . . . . C(13) N(4) C(9) C(10) 0.3(4) ? . . . . Cu(1) N(5) C(14) C(15) 175.2(2) ? . . . . Cu(1) N(5) C(18) C(17) -175.8(2) ? . . . . Cu(1) N(5) C(18) C(19) 4.9(3) ? . . . . C(14) N(5) C(18) C(17) 0.9(4) ? . . . . C(14) N(5) C(18) C(19) -178.5(2) ? . . . . C(18) N(5) C(14) C(15) -0.8(5) ? . . . . Cu(1) N(6) N(7) Cu(2) 1.8(4) ? . . . . Cu(1) N(6) N(7) C(21) -177.0(2) ? . . . . Cu(1) N(6) C(19) C(18) -3.8(3) ? . . . . Cu(1) N(6) C(19) C(20) 177.7(2) ? . . . . N(7) N(6) C(19) C(18) 178.9(2) ? . . . . N(7) N(6) C(19) C(20) 0.3(3) ? . . . . C(19) N(6) N(7) Cu(2) 178.5(2) ? . . . . C(19) N(6) N(7) C(21) -0.3(3) ? . . . . Cu(2) N(7) C(21) C(20) -178.9(2) ? . . . . Cu(2) N(7) C(21) C(22) 1.7(3) ? . . . . N(6) N(7) C(21) C(20) 0.1(3) ? . . . . N(6) N(7) C(21) C(22) -179.3(2) ? . . . . Cu(2) N(8) C(22) C(21) -12.2(3) ? . . . . Cu(2) N(8) C(22) C(23) 167.5(2) ? . . . . Cu(2) N(8) C(26) C(25) -166.8(2) ? . . . . C(22) N(8) C(26) C(25) 2.2(5) ? . . . . C(26) N(8) C(22) C(21) 177.0(2) ? . . . . C(26) N(8) C(22) C(23) -3.3(4) ? . . . . N(1) C(1) C(2) C(3) -0.1(4) ? . . . . C(1) C(2) C(3) C(4) 1.7(5) ? . . . . C(2) C(3) C(4) C(5) -1.4(5) ? . . . . C(3) C(4) C(5) N(1) -0.6(5) ? . . . . C(3) C(4) C(5) C(6) 179.3(3) ? . . . . N(1) C(5) C(6) N(2) -0.5(4) ? . . . . N(1) C(5) C(6) C(7) -179.3(3) ? . . . . C(4) C(5) C(6) N(2) 179.7(3) ? . . . . C(4) C(5) C(6) C(7) 0.8(6) ? . . . . N(2) C(6) C(7) C(8) 0.1(2) ? . . . . C(5) C(6) C(7) C(8) 179.0(3) ? . . . . C(6) C(7) C(8) N(3) -0.3(3) ? . . . . C(6) C(7) C(8) C(9) 179.8(3) ? . . . . N(3) C(8) C(9) N(4) -2.9(4) ? . . . . N(3) C(8) C(9) C(10) 175.9(3) ? . . . . C(7) C(8) C(9) N(4) 177.0(3) ? . . . . C(7) C(8) C(9) C(10) -4.2(5) ? . . . . N(4) C(9) C(10) C(11) -1.6(5) ? . . . . C(8) C(9) C(10) C(11) 179.7(3) ? . . . . C(9) C(10) C(11) C(12) 1.6(5) ? . . . . C(10) C(11) C(12) C(13) -0.4(5) ? . . . . C(11) C(12) C(13) N(4) -1.0(5) ? . . . . N(5) C(14) C(15) C(16) 0.4(5) ? . . . . C(14) C(15) C(16) C(17) 0.1(4) ? . . . . C(15) C(16) C(17) C(18) -0.1(3) ? . . . . C(16) C(17) C(18) N(5) -0.4(4) ? . . . . C(16) C(17) C(18) C(19) 178.9(3) ? . . . . N(5) C(18) C(19) N(6) -1.0(3) ? . . . . N(5) C(18) C(19) C(20) 177.0(3) ? . . . . C(17) C(18) C(19) N(6) 179.7(2) ? . . . . C(17) C(18) C(19) C(20) -2.3(5) ? . . . . N(6) C(19) C(20) C(21) -0.3(3) ? . . . . C(18) C(19) C(20) C(21) -178.3(3) ? . . . . C(19) C(20) C(21) N(7) 0.1(3) ? . . . . C(19) C(20) C(21) C(22) 179.3(3) ? . . . . N(7) C(21) C(22) N(8) 7.4(4) ? . . . . N(7) C(21) C(22) C(23) -172.2(3) ? . . . . C(20) C(21) C(22) N(8) -171.7(3) ? . . . . C(20) C(21) C(22) C(23) 8.6(5) ? . . . . N(8) C(22) C(23) C(24) 1.9(5) ? . . . . C(21) C(22) C(23) C(24) -178.5(3) ? . . . . C(22) C(23) C(24) C(25) 0.8(5) ? . . . . C(23) C(24) C(25) C(26) -1.9(5) ? . . . . C(24) C(25) C(26) N(8) 0.4(5) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Br(1) Br(4) 2.782(6) ? . . Br(1) O(2) 2.759(4) ? . . Br(1) O(4) 2.729(12) ? . . Br(2) O(2) 3.313(3) ? . . Br(3) Br(3) 3.091(3) ? . 2_557 Br(3) Br(4) 3.286(4) ? . 1_455 Br(3) O(2) 3.208(4) ? . . Br(3) O(3) 3.186(14) ? . 2_557 Br(3) O(4) 3.219(10) ? . 1_455 Br(4) Br(1) 2.782(6) ? . . Br(4) Br(3) 3.286(4) ? . 1_655 Br(4) Br(4) 2.912(6) ? . 2_657 Br(4) O(1) 3.173(9) ? . . Br(4) O(3) 3.568(12) ? . 1_655 Br(4) O(4) 3.108(12) ? . 2_657 O(2) Br(1) 2.759(4) ? . . O(2) Br(2) 3.313(3) ? . . O(2) Br(3) 3.208(4) ? . . O(2) O(1) 2.848(7) ? . . O(2) O(3) 2.910(13) ? . . O(2) C(4) 3.562(4) ? . 2_667 O(1) Br(4) 3.173(9) ? . . O(1) O(2) 2.848(7) ? . . O(1) O(4) 3.097(14) ? . . O(3) Br(3) 3.186(14) ? . 2_557 O(3) Br(4) 3.568(12) ? . 1_455 O(3) O(2) 2.910(13) ? . . O(3) O(3) 3.32(2) ? . 2_557 O(3) O(4) 3.497(15) ? . 1_455 O(3) C(1) 3.575(13) ? . 1_455 O(4) Br(1) 2.729(12) ? . . O(4) Br(3) 3.219(10) ? . 1_655 O(4) Br(4) 3.108(12) ? . 2_657 O(4) O(1) 3.097(14) ? . . O(4) O(3) 3.497(15) ? . 1_655 O(4) O(4) 3.305(15) ? . 2_657 N(1) C(25) 3.530(4) ? . 2_666 N(4) C(19) 3.579(4) ? . 2_666 N(4) C(20) 3.539(3) ? . 2_666 C(1) O(3) 3.575(13) ? . 1_655 C(2) C(7) 3.590(4) ? . 2_667 C(2) C(8) 3.556(4) ? . 2_667 C(3) C(7) 3.499(4) ? . 2_667 C(3) C(8) 3.392(5) ? . 2_667 C(4) O(2) 3.562(4) ? . 2_667 C(4) C(6) 3.371(4) ? . 2_667 C(4) C(7) 3.521(4) ? . 2_667 C(5) C(24) 3.483(5) ? . 2_666 C(5) C(25) 3.332(5) ? . 2_666 C(6) C(4) 3.371(4) ? . 2_667 C(6) C(23) 3.570(4) ? . 2_666 C(6) C(24) 3.450(4) ? . 2_666 C(6) C(25) 3.541(4) ? . 2_666 C(7) C(2) 3.590(4) ? . 2_667 C(7) C(3) 3.499(4) ? . 2_667 C(7) C(4) 3.521(4) ? . 2_667 C(7) C(23) 3.335(4) ? . 2_666 C(8) C(2) 3.556(4) ? . 2_667 C(8) C(3) 3.392(5) ? . 2_667 C(8) C(22) 3.544(4) ? . 2_666 C(9) C(20) 3.338(4) ? . 2_666 C(10) C(20) 3.546(4) ? . 2_666 C(11) C(24) 3.566(4) ? . 2_566 C(12) C(17) 3.328(5) ? . 2_666 C(12) C(18) 3.496(5) ? . 2_666 C(12) C(24) 3.451(5) ? . 2_566 C(12) C(25) 3.376(5) ? . 2_566 C(13) C(18) 3.564(4) ? . 2_666 C(13) C(19) 3.534(4) ? . 2_666 C(13) C(25) 3.449(5) ? . 2_566 C(13) C(26) 3.456(4) ? . 2_566 C(16) C(20) 3.416(4) ? . 2_656 C(16) C(21) 3.425(4) ? . 2_656 C(17) C(12) 3.328(5) ? . 2_666 C(17) C(19) 3.317(4) ? . 2_656 C(17) C(20) 3.460(4) ? . 2_656 C(18) C(12) 3.496(5) ? . 2_666 C(18) C(13) 3.564(4) ? . 2_666 C(19) N(4) 3.579(4) ? . 2_666 C(19) C(13) 3.534(4) ? . 2_666 C(19) C(17) 3.317(4) ? . 2_656 C(20) N(4) 3.539(3) ? . 2_666 C(20) C(9) 3.338(4) ? . 2_666 C(20) C(10) 3.546(4) ? . 2_666 C(20) C(16) 3.416(4) ? . 2_656 C(20) C(17) 3.460(4) ? . 2_656 C(21) C(16) 3.425(4) ? . 2_656 C(22) C(8) 3.544(4) ? . 2_666 C(23) C(6) 3.570(4) ? . 2_666 C(23) C(7) 3.335(4) ? . 2_666 C(24) C(5) 3.483(5) ? . 2_666 C(24) C(6) 3.450(4) ? . 2_666 C(24) C(11) 3.566(4) ? . 2_566 C(24) C(12) 3.451(5) ? . 2_566 C(25) N(1) 3.530(4) ? . 2_666 C(25) C(5) 3.332(5) ? . 2_666 C(25) C(6) 3.541(4) ? . 2_666 C(25) C(12) 3.376(5) ? . 2_566 C(25) C(13) 3.449(5) ? . 2_566 C(26) C(13) 3.456(4) ? . 2_566 Br(1) H(4) 2.891 ? . 2_667 Br(1) H(5) 3.175 ? . 2_667 Br(1) H(13) 2.844 ? . 2_656 Br(1) H(14) 3.307 ? . 2_656 Br(2) H(3) 2.919 ? . 2_667 Br(2) H(8) 3.417 ? . 2_566 Br(2) H(9) 2.910 ? . 2_566 Br(2) H(12) 2.925 ? . 2_656 Br(2) H(17) 3.352 ? . 2_566 Br(2) H(18) 2.903 ? . 2_566 Br(3) H(1) 2.894 ? . 1_455 Br(3) H(2) 3.449 ? . 1_455 Br(3) H(6) 3.432 ? . 2_567 Br(3) H(7) 3.231 ? . 1_545 Br(3) H(7) 3.469 ? . 2_567 Br(3) H(10) 3.003 ? . 1_455 Br(3) H(11) 3.568 ? . 1_455 Br(3) H(15) 3.364 ? . 2_556 Br(3) H(16) 3.152 ? . 1_556 Br(3) H(16) 3.515 ? . 2_556 Br(4) H(1) 3.339 ? . . Br(4) H(5) 3.317 ? . 2_667 Br(4) H(6) 3.428 ? . 1_545 Br(4) H(6) 2.838 ? . 2_667 Br(4) H(10) 3.555 ? . . Br(4) H(14) 3.139 ? . 2_656 Br(4) H(15) 2.851 ? . 2_656 Cu(1) H(18) 3.540 ? . 2_666 O(2) H(3) 3.062 ? . 2_667 O(2) H(4) 2.898 ? . 2_667 O(2) H(7) 2.827 ? . 1_545 O(2) H(10) 3.355 ? . 1_455 O(2) H(11) 3.204 ? . 1_455 O(2) H(12) 3.010 ? . 2_656 O(2) H(13) 3.041 ? . 2_656 O(1) H(4) 2.919 ? . 2_667 O(1) H(5) 3.431 ? . 2_667 O(1) H(13) 2.780 ? . 2_656 O(1) H(14) 3.473 ? . 2_656 O(3) H(1) 2.802 ? . 1_455 O(3) H(2) 3.258 ? . 1_455 O(3) H(6) 3.589 ? . 2_567 O(3) H(7) 3.181 ? . 1_545 O(3) H(10) 2.960 ? . 1_455 O(3) H(11) 3.577 ? . 1_455 O(3) H(16) 2.925 ? . 1_556 O(4) H(1) 3.242 ? . . O(4) H(5) 3.426 ? . 2_667 O(4) H(6) 3.486 ? . 1_545 O(4) H(6) 2.979 ? . 2_667 O(4) H(10) 3.373 ? . . O(4) H(14) 2.987 ? . 2_656 O(4) H(15) 2.731 ? . 2_656 N(1) H(5) 3.504 ? . 2_667 N(1) H(17) 3.340 ? . 2_666 N(2) H(4) 3.466 ? . 2_667 N(3) H(3) 3.451 ? . 2_667 N(6) H(13) 3.461 ? . 2_656 N(7) H(12) 3.436 ? . 2_656 C(1) H(5) 3.438 ? . 2_667 C(2) H(2) 3.555 ? . 2_767 C(2) H(3) 3.530 ? . 2_767 C(2) H(6) 3.566 ? . 2_667 C(2) H(17) 3.198 ? . 1_656 C(3) H(2) 3.363 ? . 2_767 C(3) H(17) 3.495 ? . 1_656 C(4) H(16) 3.379 ? . 2_666 C(4) H(17) 3.587 ? . 2_666 C(5) H(17) 3.332 ? . 2_666 C(6) H(4) 3.431 ? . 2_667 C(7) H(15) 3.405 ? . 2_666 C(8) H(3) 3.466 ? . 2_667 C(9) H(2) 3.477 ? . 2_667 C(9) H(14) 3.308 ? . 2_666 C(10) H(2) 3.337 ? . 2_667 C(10) H(14) 3.172 ? . 2_666 C(11) H(13) 3.250 ? . 2_666 C(11) H(14) 3.540 ? . 2_666 C(11) H(16) 3.477 ? . 2_566 C(12) H(11) 3.277 ? . 1_465 C(12) H(13) 3.338 ? . 2_666 C(13) H(17) 3.524 ? . 2_566 C(13) H(18) 3.520 ? . 2_566 C(14) H(14) 3.554 ? . 2_656 C(15) H(8) 3.275 ? . 1_645 C(15) H(12) 3.287 ? . 2_756 C(15) H(15) 3.542 ? . 2_656 C(16) H(8) 3.402 ? . 2_666 C(16) H(11) 3.361 ? . 2_756 C(17) H(8) 3.209 ? . 2_666 C(18) H(8) 3.558 ? . 2_666 C(18) H(13) 3.505 ? . 2_656 C(19) H(13) 3.300 ? . 2_656 C(21) H(12) 3.386 ? . 2_656 C(22) H(8) 3.596 ? . 2_566 C(23) H(5) 3.441 ? . 2_666 C(23) H(8) 3.467 ? . 2_566 C(23) H(11) 3.481 ? . 2_656 C(24) H(2) 3.508 ? . 1_454 C(24) H(8) 3.452 ? . 2_566 C(25) H(2) 3.194 ? . 1_454 C(25) H(8) 3.574 ? . 2_566 C(26) H(9) 3.304 ? . 2_566 H(1) Br(3) 2.894 ? . 1_655 H(1) Br(4) 3.339 ? . . H(1) O(3) 2.802 ? . 1_655 H(1) O(4) 3.242 ? . . H(2) Br(3) 3.449 ? . 1_655 H(2) O(3) 3.258 ? . 1_655 H(2) C(2) 3.555 ? . 2_767 H(2) C(3) 3.363 ? . 2_767 H(2) C(9) 3.477 ? . 2_667 H(2) C(10) 3.337 ? . 2_667 H(2) C(24) 3.508 ? . 1_656 H(2) C(25) 3.194 ? . 1_656 H(2) H(3) 3.408 ? . 2_767 H(2) H(6) 3.304 ? . 2_667 H(2) H(16) 3.069 ? . 1_656 H(2) H(17) 2.417 ? . 1_656 H(3) Br(2) 2.919 ? . 2_667 H(3) O(2) 3.062 ? . 2_667 H(3) N(3) 3.451 ? . 2_667 H(3) C(2) 3.530 ? . 2_767 H(3) C(8) 3.466 ? . 2_667 H(3) H(2) 3.408 ? . 2_767 H(3) H(17) 3.042 ? . 1_656 H(4) Br(1) 2.891 ? . 2_667 H(4) O(2) 2.898 ? . 2_667 H(4) O(1) 2.919 ? . 2_667 H(4) N(2) 3.466 ? . 2_667 H(4) C(6) 3.431 ? . 2_667 H(4) H(16) 3.229 ? . 2_666 H(5) Br(1) 3.175 ? . 2_667 H(5) Br(4) 3.317 ? . 2_667 H(5) O(1) 3.431 ? . 2_667 H(5) O(4) 3.426 ? . 2_667 H(5) N(1) 3.504 ? . 2_667 H(5) C(1) 3.438 ? . 2_667 H(5) C(23) 3.441 ? . 2_666 H(5) H(15) 3.286 ? . 2_666 H(6) Br(3) 3.432 ? . 2_567 H(6) Br(4) 3.428 ? . 1_565 H(6) Br(4) 2.838 ? . 2_667 H(6) O(3) 3.589 ? . 2_567 H(6) O(4) 3.486 ? . 1_565 H(6) O(4) 2.979 ? . 2_667 H(6) C(2) 3.566 ? . 2_667 H(6) H(2) 3.304 ? . 2_667 H(6) H(14) 3.362 ? . 2_666 H(7) Br(3) 3.231 ? . 1_565 H(7) Br(3) 3.469 ? . 2_567 H(7) O(2) 2.827 ? . 1_565 H(7) O(3) 3.181 ? . 1_565 H(7) H(11) 3.275 ? . 1_465 H(7) H(13) 3.212 ? . 2_666 H(7) H(16) 3.425 ? . 2_566 H(8) Br(2) 3.417 ? . 2_566 H(8) C(15) 3.275 ? . 1_465 H(8) C(16) 3.402 ? . 2_666 H(8) C(17) 3.209 ? . 2_666 H(8) C(18) 3.558 ? . 2_666 H(8) C(22) 3.596 ? . 2_566 H(8) C(23) 3.467 ? . 2_566 H(8) C(24) 3.452 ? . 2_566 H(8) C(25) 3.574 ? . 2_566 H(8) H(11) 2.447 ? . 1_465 H(8) H(12) 3.272 ? . 1_465 H(8) H(13) 3.366 ? . 2_666 H(9) Br(2) 2.910 ? . 2_566 H(9) C(26) 3.304 ? . 2_566 H(9) H(9) 3.534 ? . 2_566 H(9) H(18) 3.249 ? . 2_566 H(10) Br(3) 3.003 ? . 1_655 H(10) Br(4) 3.555 ? . . H(10) O(2) 3.355 ? . 1_655 H(10) O(3) 2.960 ? . 1_655 H(10) O(4) 3.373 ? . . H(11) Br(3) 3.568 ? . 1_655 H(11) O(2) 3.204 ? . 1_655 H(11) O(3) 3.577 ? . 1_655 H(11) C(12) 3.277 ? . 1_645 H(11) C(16) 3.361 ? . 2_756 H(11) C(23) 3.481 ? . 2_656 H(11) H(7) 3.275 ? . 1_645 H(11) H(8) 2.447 ? . 1_645 H(11) H(12) 3.021 ? . 2_756 H(11) H(15) 3.285 ? . 2_656 H(12) Br(2) 2.925 ? . 2_656 H(12) O(2) 3.010 ? . 2_656 H(12) N(7) 3.436 ? . 2_656 H(12) C(15) 3.287 ? . 2_756 H(12) C(21) 3.386 ? . 2_656 H(12) H(8) 3.272 ? . 1_645 H(12) H(11) 3.021 ? . 2_756 H(13) Br(1) 2.844 ? . 2_656 H(13) O(2) 3.041 ? . 2_656 H(13) O(1) 2.780 ? . 2_656 H(13) N(6) 3.461 ? . 2_656 H(13) C(11) 3.250 ? . 2_666 H(13) C(12) 3.338 ? . 2_666 H(13) C(18) 3.505 ? . 2_656 H(13) C(19) 3.300 ? . 2_656 H(13) H(7) 3.212 ? . 2_666 H(13) H(8) 3.366 ? . 2_666 H(14) Br(1) 3.307 ? . 2_656 H(14) Br(4) 3.139 ? . 2_656 H(14) O(1) 3.473 ? . 2_656 H(14) O(4) 2.987 ? . 2_656 H(14) C(9) 3.308 ? . 2_666 H(14) C(10) 3.172 ? . 2_666 H(14) C(11) 3.540 ? . 2_666 H(14) C(14) 3.554 ? . 2_656 H(14) H(6) 3.362 ? . 2_666 H(15) Br(3) 3.364 ? . 2_556 H(15) Br(4) 2.851 ? . 2_656 H(15) O(4) 2.731 ? . 2_656 H(15) C(7) 3.405 ? . 2_666 H(15) C(15) 3.542 ? . 2_656 H(15) H(5) 3.286 ? . 2_666 H(15) H(11) 3.285 ? . 2_656 H(16) Br(3) 3.152 ? . 1_554 H(16) Br(3) 3.515 ? . 2_556 H(16) O(3) 2.925 ? . 1_554 H(16) C(4) 3.379 ? . 2_666 H(16) C(11) 3.477 ? . 2_566 H(16) H(2) 3.069 ? . 1_454 H(16) H(4) 3.229 ? . 2_666 H(16) H(7) 3.425 ? . 2_566 H(17) Br(2) 3.352 ? . 2_566 H(17) N(1) 3.340 ? . 2_666 H(17) C(2) 3.198 ? . 1_454 H(17) C(3) 3.495 ? . 1_454 H(17) C(4) 3.587 ? . 2_666 H(17) C(5) 3.332 ? . 2_666 H(17) C(13) 3.524 ? . 2_566 H(17) H(2) 2.417 ? . 1_454 H(17) H(3) 3.042 ? . 1_454 H(18) Br(2) 2.903 ? . 2_566 H(18) Cu(1) 3.540 ? . 2_666 H(18) C(13) 3.520 ? . 2_566 H(18) H(9) 3.249 ? . 2_566 data__Cu2(bpypz)2Br2(H2O)2 _database_code_depnum_ccdc_archive 'CCDC 704684' #TrackingRef 'Cu2(bpypz)2Br2(H2O)2.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C26 H22 Br2 Cu2 N8 O2 ' _chemical_formula_moiety 'C26 H22 Br2 Cu2 N8 O2 ' _chemical_formula_weight 765.41 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 10.17(5) _cell_length_b 11.52(6) _cell_length_c 11.77(5) _cell_angle_alpha 77.82(6) _cell_angle_beta 86.94(6) _cell_angle_gamma 85.43(8) _cell_volume 1342(11) _cell_formula_units_Z 2 _cell_measurement_reflns_used 123 _cell_measurement_theta_min 12.6 _cell_measurement_theta_max 26.7 _cell_measurement_temperature 200.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756.00 _exptl_absorpt_coefficient_mu 4.612 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.649 _exptl_absorpt_correction_T_max 0.871 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 323 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 12759 _diffrn_reflns_av_R_equivalents 0.179 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6073 _reflns_number_gt 2096 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.1718 _refine_ls_wR_factor_ref 0.4726 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 6073 _refine_ls_number_parameters 326 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 2.43 _refine_diff_density_min -1.37 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Br Br -0.290 2.459 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Br(1) Br 0.5813(2) 0.1509(2) 0.1459(2) 0.0534(7) Uani 1.00 1 d . . . Br(2) Br 0.9454(2) 0.3481(2) 0.3432(2) 0.0722(9) Uani 1.00 1 d . . . Cu(1) Cu 0.8081(2) 0.0639(2) 0.0690(2) 0.0479(8) Uani 1.00 1 d . . . Cu(2) Cu 1.0841(2) 0.2111(2) 0.2151(2) 0.0503(8) Uani 1.00 1 d . . . O(1) O 0.613(2) 0.337(2) 0.324(2) 0.112(9) Uiso 0.75 1 d P . . O(2) O 0.444(2) 0.430(2) 0.433(2) 0.102(8) Uiso 0.75 1 d P . . O(3) O 0.164(3) 0.479(3) 0.466(3) 0.095(11) Uiso 0.50 1 d P . . N(1) N 0.7509(15) -0.1038(14) 0.1202(16) 0.048(4) Uani 1.00 1 d . . . N(2) N 0.9133(15) 0.0101(14) 0.2102(15) 0.044(4) Uani 1.00 1 d . . . N(3) N 1.0062(17) 0.0565(14) 0.2527(14) 0.048(4) Uani 1.00 1 d . . . N(4) N 1.1900(18) 0.1244(17) 0.3561(17) 0.060(4) Uiso 1.00 1 d . . . N(5) N 0.7559(16) 0.1199(18) -0.1014(16) 0.058(5) Uani 1.00 1 d . . . N(6) N 0.9114(16) 0.1992(16) 0.0194(15) 0.050(4) Uani 1.00 1 d . . . N(7) N 1.0022(16) 0.2486(16) 0.0640(13) 0.046(4) Uani 1.00 1 d . . . N(8) N 1.1947(17) 0.3497(18) 0.1290(15) 0.058(5) Uani 1.00 1 d . . . C(1) C 0.6549(16) -0.1576(17) 0.081(2) 0.068(8) Uani 1.00 1 d . . . C(2) C 0.619(2) -0.274(2) 0.132(2) 0.054(5) Uiso 1.00 1 d . . . C(3) C 0.667(2) -0.332(2) 0.237(2) 0.064(6) Uani 1.00 1 d . . . C(4) C 0.770(2) -0.279(2) 0.289(2) 0.058(6) Uani 1.00 1 d . . . C(5) C 0.8008(19) -0.1670(17) 0.226(2) 0.048(5) Uani 1.00 1 d . . . C(6) C 0.9002(18) -0.1005(19) 0.2694(19) 0.049(5) Uani 1.00 1 d . . . C(7) C 0.990(2) -0.133(2) 0.360(2) 0.063(6) Uani 1.00 1 d . . . C(8) C 1.049(2) -0.0201(18) 0.345(2) 0.059(6) Uani 1.00 1 d . . . C(9) C 1.157(2) 0.0148(18) 0.4101(19) 0.046(5) Uani 1.00 1 d . . . C(10) C 1.2134(18) -0.0518(17) 0.5032(18) 0.040(4) Uiso 1.00 1 d . . . C(11) C 1.311(2) -0.014(2) 0.553(2) 0.073(7) Uiso 1.00 1 d . . . C(12) C 1.348(2) 0.103(2) 0.503(2) 0.074(8) Uani 1.00 1 d . . . C(13) C 1.285(2) 0.171(2) 0.413(2) 0.076(7) Uiso 1.00 1 d . . . C(14) C 0.656(2) 0.074(2) -0.159(2) 0.064(6) Uiso 1.00 1 d . . . C(15) C 0.620(2) 0.141(3) -0.277(2) 0.097(12) Uani 1.00 1 d . . . C(16) C 0.668(2) 0.231(2) -0.328(2) 0.069(7) Uani 1.00 1 d . . . C(17) C 0.767(2) 0.285(2) -0.274(2) 0.077(9) Uani 1.00 1 d . . . C(18) C 0.799(2) 0.224(2) -0.160(2) 0.051(5) Uani 1.00 1 d . . . C(19) C 0.8972(18) 0.2652(18) -0.091(2) 0.047(5) Uani 1.00 1 d . . . C(20) C 0.986(2) 0.3540(19) -0.117(2) 0.059(6) Uani 1.00 1 d . . . C(21) C 1.047(2) 0.340(2) -0.014(2) 0.058(6) Uani 1.00 1 d . . . C(22) C 1.159(2) 0.401(2) 0.026(2) 0.054(5) Uani 1.00 1 d . . . C(23) C 1.209(2) 0.496(2) -0.049(2) 0.063(6) Uani 1.00 1 d . . . C(24) C 1.313(2) 0.549(2) -0.005(2) 0.071(8) Uani 1.00 1 d . . . C(25) C 1.354(2) 0.494(3) 0.112(2) 0.083(9) Uani 1.00 1 d . . . C(26) C 1.281(3) 0.404(2) 0.182(2) 0.089(9) Uani 1.00 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.0473(12) 0.0599(14) 0.0566(15) -0.0086(10) -0.0155(11) -0.0154(12) Br(2) 0.0680(16) 0.0773(19) 0.0735(19) -0.0039(13) -0.0119(14) -0.0190(15) Cu(1) 0.0438(14) 0.0526(16) 0.0494(17) -0.0102(11) -0.0161(12) -0.0090(13) Cu(2) 0.0465(14) 0.0561(17) 0.0512(17) -0.0132(12) -0.0183(13) -0.0104(14) N(1) 0.036(8) 0.036(9) 0.073(13) -0.000(7) -0.014(9) -0.008(9) N(2) 0.042(9) 0.045(10) 0.051(11) -0.003(8) 0.012(8) -0.027(9) N(3) 0.074(11) 0.028(8) 0.041(10) 0.005(8) -0.026(9) -0.006(8) N(5) 0.048(10) 0.076(14) 0.054(12) -0.003(9) -0.025(9) -0.013(11) N(6) 0.054(10) 0.055(11) 0.041(11) -0.006(8) -0.008(9) -0.006(9) N(7) 0.058(10) 0.060(11) 0.019(8) -0.027(9) -0.016(8) 0.009(8) N(8) 0.061(11) 0.083(14) 0.030(10) -0.025(10) -0.015(9) -0.001(10) C(1) 0.016(8) 0.023(10) 0.17(2) 0.006(7) -0.012(12) -0.026(14) C(3) 0.050(13) 0.087(18) 0.048(14) -0.015(12) 0.020(12) 0.001(14) C(4) 0.051(12) 0.067(16) 0.059(15) -0.020(11) -0.002(12) -0.016(14) C(5) 0.052(12) 0.033(11) 0.066(15) 0.027(9) -0.024(11) -0.029(11) C(6) 0.043(11) 0.053(14) 0.055(14) -0.023(10) -0.016(10) -0.013(12) C(7) 0.042(11) 0.090(18) 0.062(16) -0.028(12) -0.008(11) -0.019(14) C(8) 0.057(13) 0.029(11) 0.089(19) -0.008(10) -0.030(13) -0.002(12) C(9) 0.046(11) 0.041(12) 0.045(13) 0.004(9) -0.000(10) 0.003(10) C(12) 0.074(15) 0.10(2) 0.070(17) -0.029(14) -0.031(14) -0.041(16) C(15) 0.045(13) 0.22(3) 0.053(17) -0.059(19) 0.003(13) -0.07(2) C(16) 0.033(12) 0.11(2) 0.065(17) -0.011(13) -0.018(12) -0.021(17) C(17) 0.053(13) 0.081(18) 0.12(2) 0.009(12) -0.032(15) -0.059(19) C(18) 0.059(13) 0.050(14) 0.047(13) -0.017(11) -0.010(11) -0.012(12) C(19) 0.032(10) 0.041(12) 0.063(15) -0.008(9) 0.007(10) 0.004(12) C(20) 0.056(13) 0.043(13) 0.079(18) 0.009(10) -0.018(13) -0.014(13) C(21) 0.048(12) 0.085(18) 0.053(14) -0.023(12) -0.021(11) -0.028(14) C(22) 0.040(11) 0.059(15) 0.058(16) 0.002(11) -0.003(11) -0.000(13) C(23) 0.072(15) 0.057(15) 0.058(16) 0.008(12) -0.005(13) -0.010(14) C(24) 0.061(14) 0.049(14) 0.11(2) 0.006(11) 0.011(15) -0.048(16) C(25) 0.083(18) 0.13(2) 0.052(16) -0.009(18) -0.028(15) -0.035(18) C(26) 0.12(2) 0.10(2) 0.052(16) -0.051(19) -0.030(16) 0.009(16) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Br(1) Cu(1) 2.633(3) yes . . Br(2) Cu(2) 2.679(4) yes . . Cu(1) N(1) 2.020(16) yes . . Cu(1) N(2) 1.985(17) yes . . Cu(1) N(5) 2.057(18) yes . . Cu(1) N(6) 1.920(18) yes . . Cu(2) N(3) 1.962(16) yes . . Cu(2) N(4) 2.056(19) yes . . Cu(2) N(7) 1.954(15) yes . . Cu(2) N(8) 2.078(19) yes . . N(1) C(1) 1.35(2) yes . . N(1) C(5) 1.40(2) yes . . N(2) N(3) 1.29(2) yes . . N(2) C(6) 1.33(2) yes . . N(3) C(8) 1.32(2) yes . . N(4) C(9) 1.35(2) yes . . N(4) C(13) 1.41(3) yes . . N(5) C(14) 1.44(3) yes . . N(5) C(18) 1.34(2) yes . . N(6) N(7) 1.31(2) yes . . N(6) C(19) 1.36(2) yes . . N(7) C(21) 1.34(2) yes . . N(8) C(22) 1.29(2) yes . . N(8) C(26) 1.36(4) yes . . C(1) C(2) 1.42(2) yes . . C(2) C(3) 1.37(3) yes . . C(3) C(4) 1.46(3) yes . . C(4) C(5) 1.40(2) yes . . C(5) C(6) 1.49(3) yes . . C(6) C(7) 1.41(3) yes . . C(7) C(8) 1.45(3) yes . . C(8) C(9) 1.50(3) yes . . C(9) C(10) 1.33(2) yes . . C(10) C(11) 1.33(3) yes . . C(11) C(12) 1.42(3) yes . . C(12) C(13) 1.34(3) yes . . C(14) C(15) 1.48(3) yes . . C(15) C(16) 1.21(4) yes . . C(16) C(17) 1.46(4) yes . . C(17) C(18) 1.41(3) yes . . C(18) C(19) 1.49(3) yes . . C(19) C(20) 1.39(3) yes . . C(20) C(21) 1.36(3) yes . . C(21) C(22) 1.53(3) yes . . C(22) C(23) 1.37(3) yes . . C(23) C(24) 1.44(4) yes . . C(24) C(25) 1.45(3) yes . . C(25) C(26) 1.41(4) yes . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Br(1) Cu(1) N(1) 90.9(4) yes . . . Br(1) Cu(1) N(2) 104.5(4) yes . . . Br(1) Cu(1) N(5) 91.9(5) yes . . . Br(1) Cu(1) N(6) 104.8(5) yes . . . N(1) Cu(1) N(2) 80.4(7) yes . . . N(1) Cu(1) N(5) 106.0(8) yes . . . N(1) Cu(1) N(6) 163.5(6) yes . . . N(2) Cu(1) N(5) 162.4(6) yes . . . N(2) Cu(1) N(6) 90.7(7) yes . . . N(5) Cu(1) N(6) 78.7(7) yes . . . Br(2) Cu(2) N(3) 105.9(5) yes . . . Br(2) Cu(2) N(4) 91.6(5) yes . . . Br(2) Cu(2) N(7) 105.1(5) yes . . . Br(2) Cu(2) N(8) 93.0(5) yes . . . N(3) Cu(2) N(4) 78.4(7) yes . . . N(3) Cu(2) N(7) 90.6(7) yes . . . N(3) Cu(2) N(8) 160.4(7) yes . . . N(4) Cu(2) N(7) 162.1(8) yes . . . N(4) Cu(2) N(8) 106.4(7) yes . . . N(7) Cu(2) N(8) 79.6(7) yes . . . Cu(1) N(1) C(1) 130.4(14) yes . . . Cu(1) N(1) C(5) 115.0(14) yes . . . C(1) N(1) C(5) 113.4(17) yes . . . Cu(1) N(2) N(3) 132.8(12) yes . . . Cu(1) N(2) C(6) 116.8(15) yes . . . N(3) N(2) C(6) 109.9(16) yes . . . Cu(2) N(3) N(2) 134.6(12) yes . . . Cu(2) N(3) C(8) 117.1(15) yes . . . N(2) N(3) C(8) 108.2(16) yes . . . Cu(2) N(4) C(9) 118.1(15) yes . . . Cu(2) N(4) C(13) 127.4(15) yes . . . C(9) N(4) C(13) 114.0(19) yes . . . Cu(1) N(5) C(14) 127.1(14) yes . . . Cu(1) N(5) C(18) 117.4(16) yes . . . C(14) N(5) C(18) 114.2(18) yes . . . Cu(1) N(6) N(7) 136.3(13) yes . . . Cu(1) N(6) C(19) 118.4(15) yes . . . N(7) N(6) C(19) 105.3(16) yes . . . Cu(2) N(7) N(6) 132.8(12) yes . . . Cu(2) N(7) C(21) 116.7(15) yes . . . N(6) N(7) C(21) 110.4(16) yes . . . Cu(2) N(8) C(22) 116.2(16) yes . . . Cu(2) N(8) C(26) 124.3(15) yes . . . C(22) N(8) C(26) 118(2) yes . . . N(1) C(1) C(2) 124(2) yes . . . C(1) C(2) C(3) 120(2) yes . . . C(2) C(3) C(4) 120(2) yes . . . C(3) C(4) C(5) 113(2) yes . . . N(1) C(5) C(4) 129(2) yes . . . N(1) C(5) C(6) 111.7(16) yes . . . C(4) C(5) C(6) 119.8(19) yes . . . N(2) C(6) C(5) 115.5(18) yes . . . N(2) C(6) C(7) 112(2) yes . . . C(5) C(6) C(7) 133(2) yes . . . C(6) C(7) C(8) 98.1(19) yes . . . N(3) C(8) C(7) 112(2) yes . . . N(3) C(8) C(9) 117.9(18) yes . . . C(7) C(8) C(9) 129.9(19) yes . . . N(4) C(9) C(8) 108.4(17) yes . . . N(4) C(9) C(10) 126(2) yes . . . C(8) C(9) C(10) 125.9(19) yes . . . C(9) C(10) C(11) 121(2) yes . . . C(10) C(11) C(12) 116(2) yes . . . C(11) C(12) C(13) 122(2) yes . . . N(4) C(13) C(12) 120(2) yes . . . N(5) C(14) C(15) 117(2) yes . . . C(14) C(15) C(16) 125(3) yes . . . C(15) C(16) C(17) 121(2) yes . . . C(16) C(17) C(18) 115(2) yes . . . N(5) C(18) C(17) 128(2) yes . . . N(5) C(18) C(19) 109.7(18) yes . . . C(17) C(18) C(19) 122(2) yes . . . N(6) C(19) C(18) 115.0(17) yes . . . N(6) C(19) C(20) 112(2) yes . . . C(18) C(19) C(20) 133(2) yes . . . C(19) C(20) C(21) 102(2) yes . . . N(7) C(21) C(20) 111(2) yes . . . N(7) C(21) C(22) 115.1(19) yes . . . C(20) C(21) C(22) 134(2) yes . . . N(8) C(22) C(21) 112.2(19) yes . . . N(8) C(22) C(23) 130(2) yes . . . C(21) C(22) C(23) 118(2) yes . . . C(22) C(23) C(24) 115(2) yes . . . C(23) C(24) C(25) 116(2) yes . . . C(24) C(25) C(26) 120(2) yes . . . N(8) C(26) C(25) 118(2) yes . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Br(1) Cu(1) N(1) C(1) 66(2) ? . . . . Br(1) Cu(1) N(1) C(5) -100.1(13) ? . . . . Br(1) Cu(1) N(2) N(3) -100.5(17) ? . . . . Br(1) Cu(1) N(2) C(6) 88.2(14) ? . . . . Br(1) Cu(1) N(5) C(14) -68.8(18) ? . . . . Br(1) Cu(1) N(5) C(18) 97.0(15) ? . . . . Br(1) Cu(1) N(6) N(7) 97(2) ? . . . . Br(1) Cu(1) N(6) C(19) -85.5(15) ? . . . . N(1) Cu(1) N(2) N(3) 171.0(19) ? . . . . N(1) Cu(1) N(2) C(6) -0.2(11) ? . . . . N(2) Cu(1) N(1) C(1) 171(2) ? . . . . N(2) Cu(1) N(1) C(5) 4.4(14) ? . . . . N(1) Cu(1) N(5) C(14) 23(2) ? . . . . N(1) Cu(1) N(5) C(18) -171.5(15) ? . . . . N(5) Cu(1) N(1) C(1) -26(2) ? . . . . N(5) Cu(1) N(1) C(5) 167.6(13) ? . . . . N(1) Cu(1) N(6) N(7) -65(4) ? . . . . N(1) Cu(1) N(6) C(19) 112(2) ? . . . . N(6) Cu(1) N(1) C(1) -131(2) ? . . . . N(6) Cu(1) N(1) C(5) 63(3) ? . . . . N(2) Cu(1) N(5) C(14) 132(2) ? . . . . N(2) Cu(1) N(5) C(18) -62(3) ? . . . . N(5) Cu(1) N(2) N(3) 58(3) ? . . . . N(5) Cu(1) N(2) C(6) -114(2) ? . . . . N(2) Cu(1) N(6) N(7) -8(2) ? . . . . N(2) Cu(1) N(6) C(19) 169.3(15) ? . . . . N(6) Cu(1) N(2) N(3) 5.0(19) ? . . . . N(6) Cu(1) N(2) C(6) -166.2(15) ? . . . . N(5) Cu(1) N(6) N(7) -174(2) ? . . . . N(5) Cu(1) N(6) C(19) 3.5(15) ? . . . . N(6) Cu(1) N(5) C(14) -174(2) ? . . . . N(6) Cu(1) N(5) C(18) -7.8(15) ? . . . . Br(2) Cu(2) N(3) N(2) 90.8(19) ? . . . . Br(2) Cu(2) N(3) C(8) -85.0(16) ? . . . . Br(2) Cu(2) N(4) C(9) 102.4(16) ? . . . . Br(2) Cu(2) N(4) C(13) -69(2) ? . . . . Br(2) Cu(2) N(7) N(6) -94.9(18) ? . . . . Br(2) Cu(2) N(7) C(21) 87.4(15) ? . . . . Br(2) Cu(2) N(8) C(22) -100.5(17) ? . . . . Br(2) Cu(2) N(8) C(26) 65(2) ? . . . . N(3) Cu(2) N(4) C(9) -3.6(16) ? . . . . N(3) Cu(2) N(4) C(13) -175(2) ? . . . . N(4) Cu(2) N(3) N(2) 179.1(18) ? . . . . N(4) Cu(2) N(3) C(8) 3.4(16) ? . . . . N(3) Cu(2) N(7) N(6) 11.8(19) ? . . . . N(3) Cu(2) N(7) C(21) -165.9(16) ? . . . . N(7) Cu(2) N(3) N(2) -15.1(19) ? . . . . N(7) Cu(2) N(3) C(8) 169.1(16) ? . . . . N(3) Cu(2) N(8) C(22) 65(2) ? . . . . N(3) Cu(2) N(8) C(26) -129(2) ? . . . . N(8) Cu(2) N(3) N(2) -74(2) ? . . . . N(8) Cu(2) N(3) C(8) 110(2) ? . . . . N(4) Cu(2) N(7) N(6) 64(3) ? . . . . N(4) Cu(2) N(7) C(21) -114(2) ? . . . . N(7) Cu(2) N(4) C(9) -57(3) ? . . . . N(7) Cu(2) N(4) C(13) 131(2) ? . . . . N(4) Cu(2) N(8) C(22) 167.0(17) ? . . . . N(4) Cu(2) N(8) C(26) -27(2) ? . . . . N(8) Cu(2) N(4) C(9) -164.0(16) ? . . . . N(8) Cu(2) N(4) C(13) 24(2) ? . . . . N(7) Cu(2) N(8) C(22) 4.3(17) ? . . . . N(7) Cu(2) N(8) C(26) 170(2) ? . . . . N(8) Cu(2) N(7) N(6) 174.8(19) ? . . . . N(8) Cu(2) N(7) C(21) -2.9(16) ? . . . . Cu(1) N(1) C(1) C(2) -174.9(17) ? . . . . Cu(1) N(1) C(5) C(4) 173.3(18) ? . . . . Cu(1) N(1) C(5) C(6) -7(2) ? . . . . C(1) N(1) C(5) C(4) 5(3) ? . . . . C(1) N(1) C(5) C(6) -176.1(18) ? . . . . C(5) N(1) C(1) C(2) -8(3) ? . . . . Cu(1) N(2) N(3) Cu(2) 8(3) ? . . . . Cu(1) N(2) N(3) C(8) -175.9(16) ? . . . . Cu(1) N(2) C(6) C(5) -4(2) ? . . . . Cu(1) N(2) C(6) C(7) 173.8(14) ? . . . . N(3) N(2) C(6) C(5) -177.0(17) ? . . . . N(3) N(2) C(6) C(7) 1(2) ? . . . . C(6) N(2) N(3) Cu(2) 179.7(11) ? . . . . C(6) N(2) N(3) C(8) -4(2) ? . . . . Cu(2) N(3) C(8) C(7) -176.9(15) ? . . . . Cu(2) N(3) C(8) C(9) -3(2) ? . . . . N(2) N(3) C(8) C(7) 6(2) ? . . . . N(2) N(3) C(8) C(9) -179.7(13) ? . . . . Cu(2) N(4) C(9) C(8) 3(2) ? . . . . Cu(2) N(4) C(9) C(10) -178.6(18) ? . . . . Cu(2) N(4) C(13) C(12) -178.5(19) ? . . . . C(9) N(4) C(13) C(12) 10(3) ? . . . . C(13) N(4) C(9) C(8) 176(2) ? . . . . C(13) N(4) C(9) C(10) -6(3) ? . . . . Cu(1) N(5) C(14) C(15) 170.2(19) ? . . . . Cu(1) N(5) C(18) C(17) -174.2(19) ? . . . . Cu(1) N(5) C(18) C(19) 10(2) ? . . . . C(14) N(5) C(18) C(17) -7(3) ? . . . . C(14) N(5) C(18) C(19) 177.3(18) ? . . . . C(18) N(5) C(14) C(15) 4(3) ? . . . . Cu(1) N(6) N(7) Cu(2) -1(3) ? . . . . Cu(1) N(6) N(7) C(21) 176.4(17) ? . . . . Cu(1) N(6) C(19) C(18) 0.7(19) ? . . . . Cu(1) N(6) C(19) C(20) -175.1(15) ? . . . . N(7) N(6) C(19) C(18) 178.9(17) ? . . . . N(7) N(6) C(19) C(20) 3(2) ? . . . . C(19) N(6) N(7) Cu(2) -179.2(15) ? . . . . C(19) N(6) N(7) C(21) -1(2) ? . . . . Cu(2) N(7) C(21) C(20) 177.4(15) ? . . . . Cu(2) N(7) C(21) C(22) 1(2) ? . . . . N(6) N(7) C(21) C(20) -1(2) ? . . . . N(6) N(7) C(21) C(22) -176.7(18) ? . . . . Cu(2) N(8) C(22) C(21) -5(2) ? . . . . Cu(2) N(8) C(22) C(23) 178(2) ? . . . . Cu(2) N(8) C(26) C(25) 178(2) ? . . . . C(22) N(8) C(26) C(25) -17(3) ? . . . . C(26) N(8) C(22) C(21) -171(2) ? . . . . C(26) N(8) C(22) C(23) 11(4) ? . . . . N(1) C(1) C(2) C(3) 11(3) ? . . . . C(1) C(2) C(3) C(4) -9(3) ? . . . . C(2) C(3) C(4) C(5) 5(3) ? . . . . C(3) C(4) C(5) N(1) -3(3) ? . . . . C(3) C(4) C(5) C(6) 178(2) ? . . . . N(1) C(5) C(6) N(2) 7(2) ? . . . . N(1) C(5) C(6) C(7) -170(2) ? . . . . C(4) C(5) C(6) N(2) -173(2) ? . . . . C(4) C(5) C(6) C(7) 10(3) ? . . . . N(2) C(6) C(7) C(8) 3(2) ? . . . . C(5) C(6) C(7) C(8) 180(2) ? . . . . C(6) C(7) C(8) N(3) -5(2) ? . . . . C(6) C(7) C(8) C(9) -179(2) ? . . . . N(3) C(8) C(9) N(4) -0(2) ? . . . . N(3) C(8) C(9) C(10) -179(2) ? . . . . C(7) C(8) C(9) N(4) 173(2) ? . . . . C(7) C(8) C(9) C(10) -6(4) ? . . . . N(4) C(9) C(10) C(11) 0(2) ? . . . . C(8) C(9) C(10) C(11) 179(2) ? . . . . C(9) C(10) C(11) C(12) 1(3) ? . . . . C(10) C(11) C(12) C(13) 3(4) ? . . . . C(11) C(12) C(13) N(4) -8(4) ? . . . . N(5) C(14) C(15) C(16) -0(4) ? . . . . C(14) C(15) C(16) C(17) -2(4) ? . . . . C(15) C(16) C(17) C(18) -0(3) ? . . . . C(16) C(17) C(18) N(5) 5(3) ? . . . . C(16) C(17) C(18) C(19) -179.5(18) ? . . . . N(5) C(18) C(19) N(6) -7(2) ? . . . . N(5) C(18) C(19) C(20) 168(2) ? . . . . C(17) C(18) C(19) N(6) 177(2) ? . . . . C(17) C(18) C(19) C(20) -8(3) ? . . . . N(6) C(19) C(20) C(21) -4(2) ? . . . . C(18) C(19) C(20) C(21) -178(2) ? . . . . C(19) C(20) C(21) N(7) 3(2) ? . . . . C(19) C(20) C(21) C(22) 177(2) ? . . . . N(7) C(21) C(22) N(8) 2(2) ? . . . . N(7) C(21) C(22) C(23) -179.7(15) ? . . . . C(20) C(21) C(22) N(8) -173(2) ? . . . . C(20) C(21) C(22) C(23) 6(4) ? . . . . N(8) C(22) C(23) C(24) -3(4) ? . . . . C(21) C(22) C(23) C(24) 179(2) ? . . . . C(22) C(23) C(24) C(25) 1(3) ? . . . . C(23) C(24) C(25) C(26) -8(4) ? . . . . C(24) C(25) C(26) N(8) 16(4) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Br(1) O(1) 3.34(3) ? . . Br(2) O(1) 3.42(2) ? . . Br(2) O(3) 3.34(4) ? . 1_655 Br(2) O(3) 3.39(4) ? . 2_666 O(1) Br(1) 3.34(3) ? . . O(1) Br(2) 3.42(2) ? . . O(1) O(2) 2.41(4) ? . . O(2) O(1) 2.41(4) ? . . O(2) O(2) 2.82(4) ? . 2_666 O(2) O(3) 2.88(4) ? . . O(2) C(13) 3.56(4) ? . 1_455 O(2) C(26) 3.54(4) ? . 1_455 O(3) Br(2) 3.34(4) ? . 1_455 O(3) Br(2) 3.39(4) ? . 2_666 O(3) O(2) 2.88(4) ? . . O(3) O(3) 3.41(5) ? . 2_566 O(3) C(4) 3.35(4) ? . 2_656 O(3) C(17) 3.24(4) ? . 2_665 N(2) C(11) 3.51(3) ? . 2_756 N(3) C(10) 3.54(2) ? . 2_756 N(6) C(24) 3.53(2) ? . 2_765 N(7) C(23) 3.48(3) ? . 2_765 C(1) C(14) 3.36(3) ? . 2_655 C(1) C(15) 3.54(3) ? . 2_655 C(2) C(14) 3.52(3) ? . 2_655 C(2) C(15) 3.35(3) ? . 2_655 C(2) C(22) 3.30(3) ? . 2_755 C(2) C(23) 3.27(3) ? . 2_755 C(3) C(15) 3.58(4) ? . 2_655 C(3) C(23) 3.34(3) ? . 2_755 C(4) O(3) 3.35(4) ? . 2_656 C(4) C(20) 3.30(3) ? . 2_755 C(5) C(19) 3.59(2) ? . 2_755 C(5) C(20) 3.33(3) ? . 2_755 C(6) C(10) 3.59(3) ? . 2_756 C(6) C(11) 3.30(3) ? . 2_756 C(6) C(12) 3.58(3) ? . 2_756 C(6) C(18) 3.56(3) ? . 2_755 C(6) C(19) 3.59(3) ? . 2_755 C(7) C(9) 3.49(3) ? . 2_756 C(7) C(10) 3.43(3) ? . 2_756 C(7) C(11) 3.58(3) ? . 2_756 C(7) C(16) 3.60(3) ? . 2_755 C(7) C(17) 3.17(3) ? . 2_755 C(7) C(18) 3.38(3) ? . 2_755 C(8) C(9) 3.48(3) ? . 2_756 C(8) C(10) 3.28(3) ? . 2_756 C(9) C(7) 3.49(3) ? . 2_756 C(9) C(8) 3.48(3) ? . 2_756 C(9) C(15) 3.32(4) ? . 2_755 C(9) C(16) 3.51(3) ? . 2_755 C(10) N(3) 3.54(2) ? . 2_756 C(10) C(6) 3.59(3) ? . 2_756 C(10) C(7) 3.43(3) ? . 2_756 C(10) C(8) 3.28(3) ? . 2_756 C(10) C(15) 3.38(3) ? . 2_755 C(10) C(16) 3.33(3) ? . 2_755 C(11) N(2) 3.51(3) ? . 2_756 C(11) C(6) 3.30(3) ? . 2_756 C(11) C(7) 3.58(3) ? . 2_756 C(12) C(6) 3.58(3) ? . 2_756 C(13) O(2) 3.56(4) ? . 1_655 C(14) C(1) 3.36(3) ? . 2_655 C(14) C(2) 3.52(3) ? . 2_655 C(15) C(1) 3.54(3) ? . 2_655 C(15) C(2) 3.35(3) ? . 2_655 C(15) C(3) 3.58(4) ? . 2_655 C(15) C(9) 3.32(4) ? . 2_755 C(15) C(10) 3.38(3) ? . 2_755 C(16) C(7) 3.60(3) ? . 2_755 C(16) C(9) 3.51(3) ? . 2_755 C(16) C(10) 3.33(3) ? . 2_755 C(17) O(3) 3.24(4) ? . 2_665 C(17) C(7) 3.17(3) ? . 2_755 C(17) C(25) 3.59(4) ? . 2_765 C(18) C(6) 3.56(3) ? . 2_755 C(18) C(7) 3.38(3) ? . 2_755 C(19) C(5) 3.59(2) ? . 2_755 C(19) C(6) 3.59(3) ? . 2_755 C(19) C(23) 3.56(3) ? . 2_765 C(19) C(24) 3.23(3) ? . 2_765 C(19) C(25) 3.60(3) ? . 2_765 C(20) C(4) 3.30(3) ? . 2_755 C(20) C(5) 3.33(3) ? . 2_755 C(20) C(22) 3.42(3) ? . 2_765 C(20) C(23) 3.34(3) ? . 2_765 C(20) C(24) 3.50(3) ? . 2_765 C(21) C(22) 3.48(3) ? . 2_765 C(21) C(23) 3.23(3) ? . 2_765 C(22) C(2) 3.30(3) ? . 2_755 C(22) C(20) 3.42(3) ? . 2_765 C(22) C(21) 3.48(3) ? . 2_765 C(23) N(7) 3.48(3) ? . 2_765 C(23) C(2) 3.27(3) ? . 2_755 C(23) C(3) 3.34(3) ? . 2_755 C(23) C(19) 3.56(3) ? . 2_765 C(23) C(20) 3.34(3) ? . 2_765 C(23) C(21) 3.23(3) ? . 2_765 C(24) N(6) 3.53(2) ? . 2_765 C(24) C(19) 3.23(3) ? . 2_765 C(24) C(20) 3.50(3) ? . 2_765 C(24) C(25) 3.59(3) ? . 2_865 C(25) C(17) 3.59(4) ? . 2_765 C(25) C(19) 3.60(3) ? . 2_765 C(25) C(24) 3.59(3) ? . 2_865 C(26) O(2) 3.54(4) ? . 1_655 data__antiCu2(bpypz)2Br2 _database_code_depnum_ccdc_archive 'CCDC 704685' #TrackingRef 'antiCu2(bpypz)2Br2.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C26 H18 Br2 Cu2 N8 ' _chemical_formula_moiety 'C26 H18 Br2 Cu2 N8 ' _chemical_formula_weight 729.38 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 6.382(2) _cell_length_b 10.275(4) _cell_length_c 18.954(7) _cell_angle_alpha 90.0000 _cell_angle_beta 93.034(4) _cell_angle_gamma 90.0000 _cell_volume 1241.2(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3296 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 200.1 #------------------------------------------------------------------------------ _exptl_crystal_description column _exptl_crystal_colour green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.951 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716.00 _exptl_absorpt_coefficient_mu 4.977 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.556 _exptl_absorpt_correction_T_max 0.608 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 11428 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.986 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2813 _reflns_number_gt 2427 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0609 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2813 _refine_ls_number_parameters 173 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0356P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.53 _refine_diff_density_min -0.50 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Br Br -0.290 2.459 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Br(1) Br 0.44215(3) 0.25951(2) 0.134837(11) 0.02418(7) Uani 1.00 1 d . . . Cu(1) Cu 0.25885(4) 0.08837(2) 0.047106(12) 0.01714(7) Uani 1.00 1 d . . . N(1) N 0.0593(2) 0.22680(16) -0.00164(9) 0.0198(3) Uani 1.00 1 d . . . N(2) N 0.3964(2) 0.11555(16) -0.04154(8) 0.0187(3) Uani 1.00 1 d . . . N(3) N 0.5679(2) 0.06498(16) -0.06877(9) 0.0183(3) Uani 1.00 1 d . . . N(4) N 0.8997(2) -0.00865(16) -0.13148(9) 0.0191(3) Uani 1.00 1 d . . . C(1) C -0.1169(3) 0.2802(2) 0.02082(12) 0.0270(5) Uani 1.00 1 d . . . C(2) C -0.2257(3) 0.3791(2) -0.01458(13) 0.0284(5) Uani 1.00 1 d . . . C(3) C -0.1485(3) 0.4277(2) -0.07500(12) 0.0267(5) Uani 1.00 1 d . . . C(4) C 0.0340(3) 0.3757(2) -0.09932(12) 0.0248(4) Uani 1.00 1 d . . . C(5) C 0.1337(3) 0.27533(18) -0.06195(11) 0.0181(4) Uani 1.00 1 d . . . C(6) C 0.3240(3) 0.21209(19) -0.08405(11) 0.0183(4) Uani 1.00 1 d . . . C(7) C 0.4502(3) 0.22400(19) -0.14140(11) 0.0208(4) Uani 1.00 1 d . . . C(8) C 0.6019(3) 0.1283(2) -0.12907(10) 0.0183(4) Uani 1.00 1 d . . . C(9) C 0.7874(3) 0.08678(19) -0.16481(11) 0.0182(4) Uani 1.00 1 d . . . C(10) C 0.8471(3) 0.1422(2) -0.22756(11) 0.0249(4) Uani 1.00 1 d . . . C(11) C 1.0303(3) 0.1008(2) -0.25617(12) 0.0275(5) Uani 1.00 1 d . . . C(12) C 1.1464(3) 0.0048(2) -0.22207(12) 0.0278(5) Uani 1.00 1 d . . . C(13) C 1.0767(3) -0.0478(2) -0.16104(12) 0.0260(4) Uani 1.00 1 d . . . H(1) H -0.1700 0.2483 0.0634 0.032 Uiso 1.00 1 c R . . H(2) H -0.3518 0.4125 0.0028 0.034 Uiso 1.00 1 c R . . H(3) H -0.2192 0.4964 -0.1000 0.032 Uiso 1.00 1 c R . . H(4) H 0.0905 0.4084 -0.1412 0.030 Uiso 1.00 1 c R . . H(5) H 0.4361 0.2833 -0.1798 0.025 Uiso 1.00 1 c R . . H(6) H 0.7631 0.2077 -0.2504 0.030 Uiso 1.00 1 c R . . H(7) H 1.0753 0.1381 -0.2987 0.033 Uiso 1.00 1 c R . . H(8) H 1.2734 -0.0248 -0.2406 0.033 Uiso 1.00 1 c R . . H(9) H 1.1572 -0.1151 -0.1385 0.031 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.01947(14) 0.02767(12) 0.02535(13) 0.00269(8) 0.00067(9) -0.00712(8) Cu(1) 0.01750(15) 0.01892(13) 0.01528(13) 0.00470(9) 0.00337(10) 0.00132(9) N(1) 0.0183(10) 0.0226(8) 0.0184(8) 0.0047(6) 0.0008(7) -0.0007(6) N(2) 0.0188(9) 0.0219(8) 0.0157(8) 0.0057(6) 0.0033(7) 0.0007(6) N(3) 0.0178(9) 0.0214(8) 0.0162(8) 0.0044(6) 0.0050(7) 0.0005(6) N(4) 0.0182(9) 0.0201(8) 0.0192(8) 0.0003(6) 0.0030(7) 0.0005(6) C(1) 0.0218(12) 0.0337(11) 0.0260(11) 0.0059(9) 0.0050(9) 0.0015(9) C(2) 0.0210(12) 0.0293(11) 0.0350(13) 0.0077(9) 0.0010(10) -0.0031(9) C(3) 0.0231(12) 0.0239(10) 0.0326(12) 0.0079(9) -0.0052(10) 0.0026(9) C(4) 0.0265(13) 0.0245(10) 0.0231(11) 0.0039(9) -0.0013(9) 0.0032(8) C(5) 0.0161(11) 0.0179(9) 0.0198(10) 0.0011(7) -0.0027(8) -0.0023(7) C(6) 0.0194(11) 0.0172(8) 0.0182(9) 0.0022(7) 0.0002(8) 0.0011(7) C(7) 0.0235(12) 0.0215(9) 0.0175(10) 0.0016(8) 0.0016(8) 0.0037(8) C(8) 0.0196(11) 0.0209(9) 0.0147(9) 0.0014(8) 0.0024(8) 0.0011(7) C(9) 0.0177(11) 0.0192(9) 0.0177(9) -0.0019(7) 0.0007(8) -0.0017(7) C(10) 0.0265(13) 0.0276(10) 0.0209(10) -0.0008(9) 0.0032(9) 0.0027(8) C(11) 0.0294(13) 0.0328(11) 0.0211(10) -0.0057(9) 0.0089(9) -0.0007(9) C(12) 0.0235(12) 0.0309(11) 0.0299(12) -0.0021(9) 0.0107(10) -0.0059(9) C(13) 0.0211(12) 0.0277(11) 0.0296(11) 0.0043(9) 0.0046(9) 0.0009(9) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Br(1) Cu(1) 2.6495(2) yes . . Cu(1) N(1) 2.0914(16) yes . . Cu(1) N(2) 1.9564(16) yes . . Cu(1) N(3) 1.9560(16) yes . 3_655 Cu(1) N(4) 2.1034(17) yes . 3_655 N(1) C(1) 1.341(2) yes . . N(1) C(5) 1.356(2) yes . . N(2) N(3) 1.340(2) yes . . N(2) C(6) 1.344(2) yes . . N(3) C(8) 1.343(2) yes . . N(4) C(9) 1.351(2) yes . . N(4) C(13) 1.349(2) yes . . C(1) C(2) 1.384(3) yes . . C(2) C(3) 1.365(3) yes . . C(3) C(4) 1.383(3) yes . . C(4) C(5) 1.387(2) yes . . C(5) C(6) 1.458(2) yes . . C(6) C(7) 1.392(3) yes . . C(7) C(8) 1.391(2) yes . . C(8) C(9) 1.459(3) yes . . C(9) C(10) 1.390(2) yes . . C(10) C(11) 1.382(3) yes . . C(11) C(12) 1.375(3) yes . . C(12) C(13) 1.372(3) yes . . C(1) H(1) 0.950(2) no . . C(2) H(2) 0.950(2) no . . C(3) H(3) 0.950(2) no . . C(4) H(4) 0.950(2) no . . C(7) H(5) 0.950(2) no . . C(10) H(6) 0.950 no . . C(11) H(7) 0.950 no . . C(12) H(8) 0.950 no . . C(13) H(9) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Br(1) Cu(1) N(1) 93.68(4) yes . . . Br(1) Cu(1) N(2) 103.94(4) yes . . . Br(1) Cu(1) N(3) 100.19(4) yes . . 3_655 Br(1) Cu(1) N(4) 89.75(4) yes . . 3_655 N(1) Cu(1) N(2) 79.27(6) yes . . . N(1) Cu(1) N(3) 164.76(6) yes . . 3_655 N(1) Cu(1) N(4) 107.13(6) yes . . 3_655 N(2) Cu(1) N(3) 91.20(7) yes . . 3_655 N(2) Cu(1) N(4) 164.66(6) yes . . 3_655 N(3) Cu(1) N(4) 79.40(6) yes 3_655 . 3_655 Cu(1) N(1) C(1) 129.74(14) yes . . . Cu(1) N(1) C(5) 112.97(13) yes . . . C(1) N(1) C(5) 117.03(17) yes . . . Cu(1) N(2) N(3) 133.50(12) yes . . . Cu(1) N(2) C(6) 117.68(13) yes . . . N(3) N(2) C(6) 108.49(16) yes . . . Cu(1) N(3) N(2) 134.11(13) yes 3_655 . . Cu(1) N(3) C(8) 117.01(14) yes 3_655 . . N(2) N(3) C(8) 108.18(16) yes . . . Cu(1) N(4) C(9) 111.92(13) yes 3_655 . . Cu(1) N(4) C(13) 130.33(14) yes 3_655 . . C(9) N(4) C(13) 117.21(18) yes . . . N(1) C(1) C(2) 123.7(2) yes . . . C(1) C(2) C(3) 118.8(2) yes . . . C(2) C(3) C(4) 119.1(2) yes . . . C(3) C(4) C(5) 119.3(2) yes . . . N(1) C(5) C(4) 122.17(19) yes . . . N(1) C(5) C(6) 114.36(17) yes . . . C(4) C(5) C(6) 123.46(19) yes . . . N(2) C(6) C(5) 114.93(18) yes . . . N(2) C(6) C(7) 109.77(18) yes . . . C(5) C(6) C(7) 135.26(18) yes . . . C(6) C(7) C(8) 103.47(17) yes . . . N(3) C(8) C(7) 110.08(18) yes . . . N(3) C(8) C(9) 115.15(17) yes . . . C(7) C(8) C(9) 134.72(18) yes . . . N(4) C(9) C(8) 114.75(17) yes . . . N(4) C(9) C(10) 122.33(19) yes . . . C(8) C(9) C(10) 122.91(18) yes . . . C(9) C(10) C(11) 119.04(19) yes . . . C(10) C(11) C(12) 118.9(2) yes . . . C(11) C(12) C(13) 119.2(2) yes . . . N(4) C(13) C(12) 123.3(2) yes . . . N(1) C(1) H(1) 118.2(2) no . . . C(2) C(1) H(1) 118.2(2) no . . . C(1) C(2) H(2) 120.6(2) no . . . C(3) C(2) H(2) 120.6(2) no . . . C(2) C(3) H(3) 120.5(2) no . . . C(4) C(3) H(3) 120.5(2) no . . . C(3) C(4) H(4) 120.4(2) no . . . C(5) C(4) H(4) 120.4(2) no . . . C(6) C(7) H(5) 128.3(2) no . . . C(8) C(7) H(5) 128.3(2) no . . . C(9) C(10) H(6) 120.5 no . . . C(11) C(10) H(6) 120.5 no . . . C(10) C(11) H(7) 120.6 no . . . C(12) C(11) H(7) 120.6 no . . . C(11) C(12) H(8) 120.4 no . . . C(13) C(12) H(8) 120.4 no . . . N(4) C(13) H(9) 118.4 no . . . C(12) C(13) H(9) 118.3 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Br(1) Cu(1) N(1) C(1) -77.82(18) ? . . . . Br(1) Cu(1) N(1) C(5) 96.08(13) ? . . . . Br(1) Cu(1) N(2) N(3) 89.24(17) ? . . . . Br(1) Cu(1) N(2) C(6) -83.37(14) ? . . . . Br(1) Cu(1) N(3) N(2) -92.70(17) ? . . 3_655 3_655 Br(1) Cu(1) N(3) C(8) 76.34(14) ? . . 3_655 3_655 Br(1) Cu(1) N(4) C(9) -89.02(13) ? . . 3_655 3_655 Br(1) Cu(1) N(4) C(13) 82.17(18) ? . . 3_655 3_655 N(1) Cu(1) N(2) N(3) -179.60(18) ? . . . . N(1) Cu(1) N(2) C(6) 7.79(14) ? . . . . N(2) Cu(1) N(1) C(1) 178.67(19) ? . . . . N(2) Cu(1) N(1) C(5) -7.43(13) ? . . . . N(1) Cu(1) N(3) N(2) 62.5(3) ? . . 3_655 3_655 N(1) Cu(1) N(3) C(8) -128.4(2) ? . . 3_655 3_655 N(3) Cu(1) N(1) C(1) 126.6(2) ? 3_655 . . . N(3) Cu(1) N(1) C(5) -59.5(3) ? 3_655 . . . N(1) Cu(1) N(4) C(9) 177.21(13) ? . . 3_655 3_655 N(1) Cu(1) N(4) C(13) -11.60(19) ? . . 3_655 3_655 N(4) Cu(1) N(1) C(1) 13.05(19) ? 3_655 . . . N(4) Cu(1) N(1) C(5) -173.06(13) ? 3_655 . . . N(2) Cu(1) N(3) N(2) 11.69(18) ? . . 3_655 3_655 N(2) Cu(1) N(3) C(8) -179.26(15) ? . . 3_655 3_655 N(3) Cu(1) N(2) N(3) -11.58(17) ? 3_655 . . . N(3) Cu(1) N(2) C(6) 175.82(14) ? 3_655 . . . N(2) Cu(1) N(4) C(9) 64.4(3) ? . . 3_655 3_655 N(2) Cu(1) N(4) C(13) -124.4(2) ? . . 3_655 3_655 N(4) Cu(1) N(2) N(3) -63.3(3) ? 3_655 . . . N(4) Cu(1) N(2) C(6) 124.0(2) ? 3_655 . . . N(3) Cu(1) N(4) C(9) 11.40(13) ? 3_655 . 3_655 3_655 N(3) Cu(1) N(4) C(13) -177.41(19) ? 3_655 . 3_655 3_655 N(4) Cu(1) N(3) N(2) 179.49(18) ? 3_655 . 3_655 3_655 N(4) Cu(1) N(3) C(8) -11.46(14) ? 3_655 . 3_655 3_655 Cu(1) N(1) C(1) C(2) 174.71(16) ? . . . . Cu(1) N(1) C(5) C(4) -174.68(15) ? . . . . Cu(1) N(1) C(5) C(6) 6.0(2) ? . . . . C(1) N(1) C(5) C(4) 0.1(2) ? . . . . C(1) N(1) C(5) C(6) -179.24(18) ? . . . . C(5) N(1) C(1) C(2) 1.0(3) ? . . . . Cu(1) N(2) N(3) Cu(1) 16.2(2) ? . . . 3_655 Cu(1) N(2) N(3) C(8) -174.04(14) ? . . . . Cu(1) N(2) C(6) C(5) -6.9(2) ? . . . . Cu(1) N(2) C(6) C(7) 175.19(13) ? . . . . N(3) N(2) C(6) C(5) 178.79(16) ? . . . . N(3) N(2) C(6) C(7) 0.8(2) ? . . . . C(6) N(2) N(3) Cu(1) -170.68(14) ? . . . 3_655 C(6) N(2) N(3) C(8) -0.9(2) ? . . . . Cu(1) N(3) C(8) C(7) 172.45(13) ? 3_655 . . . Cu(1) N(3) C(8) C(9) -9.7(2) ? 3_655 . . . N(2) N(3) C(8) C(7) 0.7(2) ? . . . . N(2) N(3) C(8) C(9) 178.59(16) ? . . . . Cu(1) N(4) C(9) C(8) 9.7(2) ? 3_655 . . . Cu(1) N(4) C(9) C(10) -171.45(16) ? 3_655 . . . Cu(1) N(4) C(13) C(12) 171.16(16) ? 3_655 . . . C(9) N(4) C(13) C(12) 0.3(3) ? . . . . C(13) N(4) C(9) C(8) -177.86(18) ? . . . . C(13) N(4) C(9) C(10) 1.0(2) ? . . . . N(1) C(1) C(2) C(3) -1.5(3) ? . . . . C(1) C(2) C(3) C(4) 0.8(3) ? . . . . C(2) C(3) C(4) C(5) 0.2(3) ? . . . . C(3) C(4) C(5) N(1) -0.6(3) ? . . . . C(3) C(4) C(5) C(6) 178.58(19) ? . . . . N(1) C(5) C(6) N(2) 0.1(2) ? . . . . N(1) C(5) C(6) C(7) 177.4(2) ? . . . . C(4) C(5) C(6) N(2) -179.18(19) ? . . . . C(4) C(5) C(6) C(7) -1.9(3) ? . . . . N(2) C(6) C(7) C(8) -0.4(2) ? . . . . C(5) C(6) C(7) C(8) -177.8(2) ? . . . . C(6) C(7) C(8) N(3) -0.2(2) ? . . . . C(6) C(7) C(8) C(9) -177.5(2) ? . . . . N(3) C(8) C(9) N(4) -0.7(2) ? . . . . N(3) C(8) C(9) C(10) -179.60(19) ? . . . . C(7) C(8) C(9) N(4) 176.5(2) ? . . . . C(7) C(8) C(9) C(10) -2.4(3) ? . . . . N(4) C(9) C(10) C(11) -1.6(3) ? . . . . C(8) C(9) C(10) C(11) 177.18(19) ? . . . . C(9) C(10) C(11) C(12) 0.8(3) ? . . . . C(10) C(11) C(12) C(13) 0.4(3) ? . . . . C(11) C(12) C(13) N(4) -1.1(3) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 N(1) N(4) 3.561(2) ? . 1_455 N(2) C(13) 3.409(2) ? . 1_455 N(3) C(1) 3.385(2) ? . 1_655 N(4) N(1) 3.561(2) ? . 1_655 N(4) C(5) 3.503(2) ? . 1_655 C(1) N(3) 3.385(2) ? . 1_455 C(1) C(3) 3.570(3) ? . 3_565 C(2) C(3) 3.478(3) ? . 3_565 C(2) C(4) 3.497(3) ? . 3_565 C(2) C(6) 3.541(3) ? . 1_455 C(2) C(7) 3.474(3) ? . 1_455 C(2) C(8) 3.508(3) ? . 1_455 C(3) C(1) 3.570(3) ? . 3_565 C(3) C(2) 3.478(3) ? . 3_565 C(3) C(7) 3.491(3) ? . 1_455 C(3) C(8) 3.589(2) ? . 1_455 C(4) C(2) 3.497(3) ? . 3_565 C(4) C(9) 3.553(2) ? . 1_455 C(4) C(10) 3.575(3) ? . 1_455 C(4) C(11) 3.592(3) ? . 2_654 C(5) N(4) 3.503(2) ? . 1_455 C(5) C(9) 3.462(2) ? . 1_455 C(6) C(2) 3.541(3) ? . 1_655 C(6) C(12) 3.514(3) ? . 1_455 C(6) C(13) 3.392(2) ? . 1_455 C(7) C(2) 3.474(3) ? . 1_655 C(7) C(3) 3.491(3) ? . 1_655 C(7) C(11) 3.592(3) ? . 1_455 C(7) C(12) 3.295(3) ? . 1_455 C(8) C(2) 3.508(3) ? . 1_655 C(8) C(3) 3.589(2) ? . 1_655 C(8) C(12) 3.553(3) ? . 1_455 C(9) C(4) 3.553(2) ? . 1_655 C(9) C(5) 3.462(2) ? . 1_655 C(10) C(4) 3.575(3) ? . 1_655 C(11) C(4) 3.592(3) ? . 2_644 C(11) C(7) 3.592(3) ? . 1_655 C(12) C(6) 3.514(3) ? . 1_655 C(12) C(7) 3.295(3) ? . 1_655 C(12) C(8) 3.553(3) ? . 1_655 C(13) N(2) 3.409(2) ? . 1_655 C(13) C(6) 3.392(2) ? . 1_655 Br(1) H(1) 2.8860(2) ? . 1_655 Br(1) H(2) 3.2874(2) ? . 1_655 Br(1) H(3) 2.9419(2) ? . 3_565 Br(1) H(5) 3.5432(2) ? . 4_555 Br(1) H(6) 2.927 ? . 4_555 Br(1) H(7) 2.914 ? . 4_455 Br(1) H(8) 3.569 ? . 3_755 Br(1) H(9) 2.954 ? . 3_755 N(1) H(3) 3.5543(16) ? . 3_565 N(2) H(1) 3.5911(16) ? . 1_655 N(2) H(2) 3.5292(16) ? . 1_655 N(2) H(9) 3.320 ? . 1_455 N(3) H(1) 3.4902(16) ? . 1_655 N(3) H(9) 3.416 ? . 1_455 C(1) H(3) 3.432(2) ? . 3_565 C(2) H(2) 3.460(2) ? . 3_465 C(3) H(5) 3.552(2) ? . 1_455 C(3) H(7) 3.277 ? . 2_654 C(3) H(8) 3.578 ? . 2_654 C(4) H(2) 3.435(2) ? . 3_565 C(4) H(7) 3.369 ? . 2_654 C(6) H(2) 3.297(2) ? . 1_655 C(7) H(2) 3.529(2) ? . 1_655 C(7) H(3) 3.567(2) ? . 1_655 C(7) H(8) 3.334 ? . 1_455 C(8) H(8) 3.297 ? . 1_455 C(10) H(4) 3.508(2) ? . 1_655 C(10) H(4) 3.496(2) ? . 2_644 C(10) H(8) 3.551 ? . 2_754 C(10) H(9) 3.558 ? . 2_754 C(11) H(3) 3.223(2) ? . 2_644 C(11) H(4) 2.851(2) ? . 2_644 C(11) H(5) 3.453(2) ? . 1_655 C(12) H(3) 3.430(2) ? . 2_644 C(12) H(4) 3.093(2) ? . 2_644 C(12) H(5) 3.478(2) ? . 1_655 C(12) H(6) 3.156 ? . 2_744 C(13) H(6) 3.218 ? . 2_744 C(13) H(7) 3.445 ? . 2_744 H(1) Br(1) 2.8860(2) ? . 1_455 H(1) N(2) 3.5911(16) ? . 1_455 H(1) N(3) 3.4902(16) ? . 1_455 H(1) H(7) 3.196 ? . 4_455 H(2) Br(1) 3.2874(2) ? . 1_455 H(2) N(2) 3.5292(16) ? . 1_455 H(2) C(2) 3.460(2) ? . 3_465 H(2) C(4) 3.435(2) ? . 3_565 H(2) C(6) 3.297(2) ? . 1_455 H(2) C(7) 3.529(2) ? . 1_455 H(2) H(2) 2.609 ? . 3_465 H(2) H(3) 3.507 ? . 3_465 H(2) H(4) 3.547 ? . 3_565 H(3) Br(1) 2.9419(2) ? . 3_565 H(3) N(1) 3.5543(16) ? . 3_565 H(3) C(1) 3.432(2) ? . 3_565 H(3) C(7) 3.567(2) ? . 1_455 H(3) C(11) 3.223(2) ? . 2_654 H(3) C(12) 3.430(2) ? . 2_654 H(3) H(2) 3.507 ? . 3_465 H(3) H(5) 3.401 ? . 1_455 H(3) H(7) 2.615 ? . 2_654 H(3) H(8) 3.032 ? . 2_654 H(4) C(10) 3.508(2) ? . 1_455 H(4) C(10) 3.496(2) ? . 2_654 H(4) C(11) 2.851(2) ? . 2_654 H(4) C(12) 3.093(2) ? . 2_654 H(4) H(2) 3.547 ? . 3_565 H(4) H(6) 3.528 ? . 1_455 H(4) H(7) 2.804 ? . 2_654 H(4) H(8) 3.215 ? . 2_654 H(5) Br(1) 3.5432(2) ? . 4_554 H(5) C(3) 3.552(2) ? . 1_655 H(5) C(11) 3.453(2) ? . 1_455 H(5) C(12) 3.478(2) ? . 1_455 H(5) H(3) 3.401 ? . 1_655 H(5) H(7) 3.473 ? . 1_455 H(5) H(8) 3.508 ? . 1_455 H(5) H(8) 3.146 ? . 2_754 H(6) Br(1) 2.927 ? . 4_554 H(6) C(12) 3.156 ? . 2_754 H(6) C(13) 3.218 ? . 2_754 H(6) H(4) 3.528 ? . 1_655 H(6) H(8) 2.763 ? . 2_754 H(6) H(9) 2.850 ? . 2_754 H(7) Br(1) 2.914 ? . 4_654 H(7) C(3) 3.277 ? . 2_644 H(7) C(4) 3.369 ? . 2_644 H(7) C(13) 3.445 ? . 2_754 H(7) H(1) 3.196 ? . 4_654 H(7) H(3) 2.615 ? . 2_644 H(7) H(4) 2.804 ? . 2_644 H(7) H(5) 3.473 ? . 1_655 H(7) H(9) 3.141 ? . 2_754 H(8) Br(1) 3.569 ? . 3_755 H(8) C(3) 3.578 ? . 2_644 H(8) C(7) 3.334 ? . 1_655 H(8) C(8) 3.297 ? . 1_655 H(8) C(10) 3.551 ? . 2_744 H(8) H(3) 3.032 ? . 2_644 H(8) H(4) 3.215 ? . 2_644 H(8) H(5) 3.508 ? . 1_655 H(8) H(5) 3.146 ? . 2_744 H(8) H(6) 2.763 ? . 2_744 H(9) Br(1) 2.954 ? . 3_755 H(9) N(2) 3.320 ? . 1_655 H(9) N(3) 3.416 ? . 1_655 H(9) C(10) 3.558 ? . 2_744 H(9) H(6) 2.850 ? . 2_744 H(9) H(7) 3.141 ? . 2_744