Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Ren-Gen Xiong' _publ_contact_author_address ; Southeast University Ordered Matter Science Research Center JiangNin Nanjing JiangSu 211189 CHINA ; _publ_contact_author_email XIONGRG@NJU.EDU.CN _publ_section_title ; Ferroelectric Metal-organic Coordination Polymer with a High Dielectric Constant ; loop_ _publ_author_name 'Ren-Gen Xiong.' 'Da-Wei Fu.' 'Qiong Ye.' 'Heng-Yun Ye.' # Attachment '1.cif' data_123 _database_code_depnum_ccdc_archive 'CCDC 297353' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H30 Br Cu3 N6 O2' _chemical_formula_weight 789.14 _chemical_absolute_configuration rm loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 21.5698(15) _cell_length_b 19.2120(13) _cell_length_c 8.8873(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.125(2) _cell_angle_gamma 90.00 _cell_volume 3538.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1596 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 26.41 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 2.951 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.680 _exptl_absorpt_correction_T_max 0.712 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14182 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.1710 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 33.44 _reflns_number_total 10602 _reflns_number_gt 3216 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(2) _refine_ls_number_reflns 10602 _refine_ls_number_parameters 388 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2514 _refine_ls_R_factor_gt 0.0830 _refine_ls_wR_factor_ref 0.2696 _refine_ls_wR_factor_gt 0.1932 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.953 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.40903(7) 0.15521(7) 0.84107(16) 0.0703(4) Uani 1 1 d . . . Cu2 Cu 0.23318(9) 0.32570(8) 0.7666(2) 0.0907(5) Uani 1 1 d . . . Br1 Br 0.36272(11) 0.03133(10) 0.8174(2) 0.1279(7) Uani 1 1 d . . . Cu3 Cu 0.32830(9) -0.09230(10) 0.7782(2) 0.0995(6) Uani 1 1 d . . . O1 O 0.6598(4) 0.0413(4) 0.5673(9) 0.071(2) Uani 1 1 d . . . H1A H 0.6906 0.0345 0.5319 0.106 Uiso 1 1 calc R . . C2 C 0.7265(6) 0.1130(6) 0.8751(12) 0.068(3) Uani 1 1 d . . . H2A H 0.7044 0.1413 0.9345 0.082 Uiso 1 1 calc R . . H2B H 0.7098 0.0659 0.8712 0.082 Uiso 1 1 calc R . . C3 C 0.5950(5) 0.1276(6) 0.6576(13) 0.060(3) Uani 1 1 d . . . N2 N 0.7774(4) 0.1299(4) 0.6623(9) 0.0502(19) Uani 1 1 d . . . C5 C 0.7651(5) 0.1391(5) 0.4868(12) 0.062(3) Uani 1 1 d . . . H5A H 0.7482 0.1855 0.4580 0.075 Uiso 1 1 calc R . . H5B H 0.7324 0.1060 0.4333 0.075 Uiso 1 1 calc R . . C6 C 0.6537(5) 0.1136(5) 0.5916(12) 0.055(3) Uani 1 1 d . . . H6A H 0.6470 0.1380 0.4915 0.067 Uiso 1 1 calc R . . O2 O 0.5916(4) 0.3805(4) 0.5786(12) 0.087(3) Uani 1 1 d . . . C8 C 0.8030(5) 0.0581(5) 0.7106(10) 0.050(2) Uani 1 1 d . . . H8A H 0.8376 0.0472 0.6644 0.059 Uiso 1 1 calc R . . H8B H 0.7690 0.0239 0.6744 0.059 Uiso 1 1 calc R . . C9 C 0.8904(6) 0.0491(6) 0.3319(11) 0.061(3) Uani 1 1 d . . . H9A H 0.8993 0.0042 0.3051 0.074 Uiso 1 1 calc R . . C10 C 0.7129(5) 0.1421(5) 0.7063(11) 0.056(2) Uani 1 1 d . . . H10A H 0.7070 0.1925 0.7121 0.068 Uiso 1 1 calc R . . C11 C 0.5750(5) 0.3207(6) 0.6376(13) 0.068(3) Uani 1 1 d . . . C12 C 0.8257(5) 0.1288(6) 0.4296(13) 0.059(3) Uani 1 1 d . . . C13 C 0.7971(6) 0.1128(6) 0.9546(13) 0.066(3) Uani 1 1 d . . . H13A H 0.8034 0.1062 1.0672 0.079 Uiso 1 1 calc R . . C14 C 0.9187(6) 0.1713(8) 0.3618(15) 0.087(4) Uani 1 1 d . . . H14A H 0.9458 0.2073 0.3500 0.104 Uiso 1 1 calc R . . C15 C 0.5251(5) 0.2021(5) 0.7484(13) 0.060(3) Uani 1 1 d . . . C16 C 0.5968(6) 0.2545(6) 0.6138(14) 0.071(3) Uani 1 1 d . . . H16A H 0.6274 0.2495 0.5586 0.085 Uiso 1 1 calc R . . N1 N 0.4945(4) 0.1472(5) 0.7960(10) 0.066(2) Uani 1 1 d . . . C18 C 0.8377(5) 0.0634(5) 0.3812(11) 0.055(2) Uani 1 1 d . . . H18A H 0.8087 0.0277 0.3824 0.066 Uiso 1 1 calc R . . C19 C 0.8168(7) -0.0166(6) 0.9430(13) 0.074(3) Uani 1 1 d . . . H19A H 0.7750 -0.0278 0.9437 0.089 Uiso 1 1 calc R . . C20 C 0.5731(5) 0.1952(5) 0.6723(12) 0.051(2) Uani 1 1 d . . . C21 C 0.5286(6) 0.3253(7) 0.7234(15) 0.077(3) Uani 1 1 d . . . H21A H 0.5160 0.3696 0.7453 0.092 Uiso 1 1 calc R . . C22 C 0.8291(5) 0.0557(5) 0.8966(11) 0.058(3) Uani 1 1 d . . . H22A H 0.8757 0.0641 0.9273 0.070 Uiso 1 1 calc R . . C23 C 0.9288(6) 0.1025(8) 0.3236(15) 0.082(4) Uani 1 1 d . . . C24 C 0.5156(6) 0.0853(7) 0.7763(15) 0.070(3) Uani 1 1 d . . . H24A H 0.4956 0.0472 0.8075 0.085 Uiso 1 1 calc R . . C25 C 0.5663(5) 0.0726(6) 0.7118(15) 0.068(3) Uani 1 1 d . . . H25A H 0.5807 0.0273 0.7052 0.082 Uiso 1 1 calc R . . C27 C 0.8249(5) 0.1820(5) 0.7564(14) 0.064(3) Uani 1 1 d . . . H27A H 0.8132 0.2283 0.7144 0.077 Uiso 1 1 calc R . . H27B H 0.8677 0.1716 0.7475 0.077 Uiso 1 1 calc R . . C29 C 0.5027(5) 0.2730(6) 0.7734(13) 0.065(3) Uani 1 1 d . . . H29A H 0.4707 0.2795 0.8238 0.078 Uiso 1 1 calc R . . C30 C 0.8649(6) 0.1829(6) 0.4194(15) 0.075(3) Uani 1 1 d . . . H30A H 0.8563 0.2273 0.4502 0.090 Uiso 1 1 calc R . . C31 C 0.8257(6) 0.1805(5) 0.9301(13) 0.065(3) Uani 1 1 d . . . H31A H 0.8695 0.1844 0.9971 0.078 Uiso 1 1 calc R . . H31B H 0.8004 0.2187 0.9536 0.078 Uiso 1 1 calc R . . C32 C 0.8600(9) -0.0646(8) 0.9821(19) 0.113(5) Uani 1 1 d . . . H32A H 0.9024 -0.0553 0.9828 0.135 Uiso 1 1 calc R . . H32B H 0.8488 -0.1085 1.0098 0.135 Uiso 1 1 calc R . . C49 C 0.6356(8) 0.3780(7) 0.500(2) 0.117(6) Uani 1 1 d . . . H49A H 0.6430 0.4240 0.4663 0.175 Uiso 1 1 calc R . . H49B H 0.6205 0.3485 0.4097 0.175 Uiso 1 1 calc R . . H49C H 0.6752 0.3596 0.5660 0.175 Uiso 1 1 calc R . . C40 C 0.9916(7) 0.0893(9) 0.273(2) 0.104(5) Uani 1 1 d . . . N3 N 1.0328(7) 0.0841(10) 0.231(2) 0.154(7) Uani 1 1 d . . . N4 N 0.3019(6) 0.2630(6) 0.8134(15) 0.088(3) Uani 1 1 d . . . C41 C 0.3431(8) 0.2238(8) 0.8329(14) 0.083(4) Uani 1 1 d . . . N5 N 0.2045(7) 0.3569(7) 0.558(2) 0.112(4) Uani 1 1 d . . . N6 N 0.1965(7) 0.3523(6) 0.9336(18) 0.109(4) Uani 1 1 d . . . C43 C 0.1889(8) 0.3751(8) 0.436(2) 0.088(4) Uani 1 1 d . . . C44 C 0.1836(8) 0.3709(7) 1.0409(19) 0.097(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0661(8) 0.0914(10) 0.0585(8) -0.0017(7) 0.0259(7) -0.0002(7) Cu2 0.1075(13) 0.0788(10) 0.0965(13) -0.0138(9) 0.0459(11) 0.0024(9) Br1 0.1458(16) 0.1316(14) 0.1106(13) 0.0081(9) 0.0428(12) -0.0131(10) Cu3 0.1022(13) 0.1203(13) 0.0859(12) 0.0025(10) 0.0428(11) -0.0062(10) O1 0.067(5) 0.077(5) 0.073(5) -0.002(4) 0.027(4) 0.007(4) C2 0.082(9) 0.086(8) 0.040(6) -0.001(5) 0.022(7) 0.013(6) C3 0.059(7) 0.074(7) 0.053(6) 0.001(5) 0.025(6) 0.005(5) N2 0.061(5) 0.050(5) 0.045(5) 0.009(3) 0.022(4) 0.005(3) C5 0.066(7) 0.068(7) 0.052(6) 0.012(5) 0.015(6) 0.012(5) C6 0.058(7) 0.061(7) 0.046(6) -0.001(4) 0.012(6) 0.004(5) O2 0.089(6) 0.067(5) 0.122(8) -0.007(5) 0.056(6) -0.011(4) C8 0.058(6) 0.056(6) 0.036(5) -0.001(4) 0.015(5) 0.005(4) C9 0.069(8) 0.073(7) 0.042(6) -0.010(5) 0.015(6) 0.001(6) C10 0.051(6) 0.070(7) 0.048(6) 0.005(5) 0.014(5) 0.014(5) C11 0.056(7) 0.083(8) 0.062(7) -0.009(6) 0.013(6) -0.003(6) C12 0.045(6) 0.080(7) 0.055(7) 0.008(5) 0.018(6) 0.013(5) C13 0.064(8) 0.084(8) 0.044(6) -0.013(5) 0.006(6) 0.018(6) C14 0.068(8) 0.140(13) 0.059(8) 0.006(7) 0.027(7) -0.019(7) C15 0.058(7) 0.066(7) 0.061(7) 0.005(5) 0.025(6) -0.005(5) C16 0.068(8) 0.089(9) 0.060(8) 0.005(6) 0.027(7) 0.016(6) N1 0.056(5) 0.085(6) 0.058(5) 0.008(5) 0.017(5) 0.017(5) C18 0.047(6) 0.072(7) 0.038(6) -0.001(4) -0.001(5) 0.005(5) C19 0.105(10) 0.055(7) 0.056(7) 0.010(5) 0.011(7) 0.005(6) C20 0.045(6) 0.065(6) 0.042(6) 0.000(4) 0.009(5) 0.004(4) C21 0.076(8) 0.070(7) 0.087(9) -0.022(6) 0.027(7) -0.006(6) C22 0.053(6) 0.078(7) 0.036(5) 0.011(5) -0.003(5) -0.006(5) C23 0.061(8) 0.133(12) 0.056(8) -0.013(7) 0.022(7) 0.030(8) C24 0.055(7) 0.088(9) 0.073(8) 0.020(6) 0.026(7) 0.005(6) C25 0.061(7) 0.068(7) 0.080(9) 0.000(6) 0.027(7) 0.009(5) C27 0.059(7) 0.054(6) 0.070(8) 0.015(5) 0.001(6) 0.002(4) C29 0.058(7) 0.082(8) 0.061(7) -0.020(6) 0.026(6) -0.006(5) C30 0.085(9) 0.072(8) 0.074(9) 0.003(6) 0.031(8) 0.009(6) C31 0.079(8) 0.056(6) 0.054(7) -0.006(4) 0.006(6) -0.012(5) C32 0.118(13) 0.091(11) 0.105(13) 0.030(8) -0.008(11) -0.018(9) C49 0.129(13) 0.087(10) 0.159(17) -0.019(9) 0.081(13) -0.039(9) C40 0.055(9) 0.159(14) 0.088(11) -0.029(9) 0.002(9) -0.005(8) N3 0.058(8) 0.28(2) 0.135(14) -0.088(12) 0.042(10) -0.010(9) N4 0.083(8) 0.092(8) 0.100(10) -0.007(6) 0.042(7) 0.004(6) C41 0.109(11) 0.104(11) 0.045(7) -0.012(6) 0.034(8) -0.027(9) N5 0.112(11) 0.086(8) 0.146(15) -0.007(8) 0.049(11) 0.024(7) N6 0.138(11) 0.081(8) 0.123(12) -0.010(7) 0.060(10) -0.004(7) C43 0.097(11) 0.085(9) 0.084(11) 0.000(8) 0.029(10) 0.030(7) C44 0.147(13) 0.058(7) 0.109(12) -0.009(7) 0.075(11) 0.000(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 C41 1.925(19) . ? Cu1 N1 1.998(8) . ? Cu1 Br1 2.567(2) . ? Cu2 N4 1.866(13) . ? Cu2 N5 1.883(18) . ? Cu2 N6 1.936(14) . ? Br1 Cu3 2.484(3) . ? Cu3 C44 1.839(15) 4_547 ? Cu3 C43 1.935(17) 4_546 ? O1 C6 1.419(12) . ? O1 H1A 0.8200 . ? C2 C13 1.491(16) . ? C2 C10 1.551(14) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C25 1.377(14) . ? C3 C20 1.401(14) . ? C3 C6 1.561(13) . ? N2 C8 1.504(11) . ? N2 C27 1.508(13) . ? N2 C5 1.518(12) . ? N2 C10 1.563(11) . ? C5 C12 1.541(13) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C10 1.499(14) . ? C6 H6A 0.9800 . ? O2 C49 1.328(15) . ? O2 C11 1.352(13) . ? C8 C22 1.592(13) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C23 1.334(18) . ? C9 C18 1.354(14) . ? C9 H9A 0.9300 . ? C10 H10A 0.9800 . ? C11 C16 1.393(15) . ? C11 C21 1.419(15) . ? C12 C30 1.359(15) . ? C12 C18 1.375(14) . ? C13 C22 1.465(14) . ? C13 C31 1.481(15) . ? C13 H13A 0.9800 . ? C14 C23 1.397(19) . ? C14 C30 1.409(16) . ? C14 H14A 0.9300 . ? C15 N1 1.373(13) . ? C15 C20 1.392(13) . ? C15 C29 1.482(14) . ? C16 C20 1.405(15) . ? C16 H16A 0.9300 . ? N1 C24 1.303(14) . ? C18 H18A 0.9300 . ? C19 C32 1.286(19) . ? C19 C22 1.493(14) . ? C19 H19A 0.9300 . ? C21 C29 1.288(15) . ? C21 H21A 0.9300 . ? C22 H22A 0.9800 . ? C23 C40 1.56(2) . ? C24 C25 1.389(15) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C27 C31 1.540(15) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9300 . ? C32 H32B 0.9300 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C40 N3 1.057(17) . ? N4 C41 1.141(16) . ? N5 C43 1.102(18) . ? N6 C44 1.123(16) . ? C43 Cu3 1.935(17) 4_556 ? C44 Cu3 1.839(15) 4_557 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C41 Cu1 N1 139.3(5) . . ? C41 Cu1 Br1 111.4(4) . . ? N1 Cu1 Br1 105.8(3) . . ? N4 Cu2 N5 116.6(5) . . ? N4 Cu2 N6 118.0(6) . . ? N5 Cu2 N6 125.4(6) . . ? Cu3 Br1 Cu1 172.90(10) . . ? C44 Cu3 C43 134.3(6) 4_547 4_546 ? C44 Cu3 Br1 110.7(4) 4_547 . ? C43 Cu3 Br1 114.6(4) 4_546 . ? C6 O1 H1A 109.5 . . ? C13 C2 C10 110.6(9) . . ? C13 C2 H2A 109.5 . . ? C10 C2 H2A 109.5 . . ? C13 C2 H2B 109.5 . . ? C10 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C25 C3 C20 119.0(9) . . ? C25 C3 C6 119.3(9) . . ? C20 C3 C6 121.5(8) . . ? C8 N2 C27 108.2(8) . . ? C8 N2 C5 110.2(7) . . ? C27 N2 C5 113.0(7) . . ? C8 N2 C10 110.4(6) . . ? C27 N2 C10 106.0(7) . . ? C5 N2 C10 109.1(7) . . ? N2 C5 C12 113.7(8) . . ? N2 C5 H5A 108.8 . . ? C12 C5 H5A 108.8 . . ? N2 C5 H5B 108.8 . . ? C12 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? O1 C6 C10 111.4(8) . . ? O1 C6 C3 110.2(8) . . ? C10 C6 C3 108.0(8) . . ? O1 C6 H6A 109.1 . . ? C10 C6 H6A 109.1 . . ? C3 C6 H6A 109.1 . . ? C49 O2 C11 118.7(10) . . ? N2 C8 C22 108.6(7) . . ? N2 C8 H8A 110.0 . . ? C22 C8 H8A 110.0 . . ? N2 C8 H8B 110.0 . . ? C22 C8 H8B 110.0 . . ? H8A C8 H8B 108.3 . . ? C23 C9 C18 117.0(10) . . ? C23 C9 H9A 121.5 . . ? C18 C9 H9A 121.5 . . ? C6 C10 C2 115.0(9) . . ? C6 C10 N2 115.0(7) . . ? C2 C10 N2 104.2(8) . . ? C6 C10 H10A 107.4 . . ? C2 C10 H10A 107.4 . . ? N2 C10 H10A 107.4 . . ? O2 C11 C16 125.4(9) . . ? O2 C11 C21 117.3(10) . . ? C16 C11 C21 117.2(11) . . ? C30 C12 C18 120.2(9) . . ? C30 C12 C5 121.6(10) . . ? C18 C12 C5 118.1(9) . . ? C22 C13 C2 110.7(9) . . ? C22 C13 C31 110.6(9) . . ? C2 C13 C31 109.9(10) . . ? C22 C13 H13A 108.5 . . ? C2 C13 H13A 108.5 . . ? C31 C13 H13A 108.5 . . ? C23 C14 C30 116.0(12) . . ? C23 C14 H14A 122.0 . . ? C30 C14 H14A 122.0 . . ? N1 C15 C20 124.3(9) . . ? N1 C15 C29 117.0(9) . . ? C20 C15 C29 118.6(9) . . ? C11 C16 C20 120.7(10) . . ? C11 C16 H16A 119.7 . . ? C20 C16 H16A 119.7 . . ? C24 N1 C15 116.3(9) . . ? C24 N1 Cu1 118.3(8) . . ? C15 N1 Cu1 123.5(7) . . ? C9 C18 C12 122.2(10) . . ? C9 C18 H18A 118.9 . . ? C12 C18 H18A 118.9 . . ? C32 C19 C22 124.8(14) . . ? C32 C19 H19A 117.6 . . ? C22 C19 H19A 117.6 . . ? C15 C20 C3 116.6(9) . . ? C15 C20 C16 119.9(9) . . ? C3 C20 C16 123.5(9) . . ? C29 C21 C11 125.1(11) . . ? C29 C21 H21A 117.4 . . ? C11 C21 H21A 117.4 . . ? C13 C22 C19 117.6(9) . . ? C13 C22 C8 106.2(8) . . ? C19 C22 C8 106.0(8) . . ? C13 C22 H22A 108.9 . . ? C19 C22 H22A 108.9 . . ? C8 C22 H22A 108.9 . . ? C9 C23 C14 124.9(11) . . ? C9 C23 C40 119.6(12) . . ? C14 C23 C40 115.5(13) . . ? N1 C24 C25 124.1(11) . . ? N1 C24 H24A 117.9 . . ? C25 C24 H24A 117.9 . . ? C3 C25 C24 119.4(10) . . ? C3 C25 H25A 120.3 . . ? C24 C25 H25A 120.3 . . ? N2 C27 C31 111.1(8) . . ? N2 C27 H27A 109.4 . . ? C31 C27 H27A 109.4 . . ? N2 C27 H27B 109.4 . . ? C31 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C21 C29 C15 118.3(10) . . ? C21 C29 H29A 120.9 . . ? C15 C29 H29A 120.9 . . ? C12 C30 C14 119.6(12) . . ? C12 C30 H30A 120.2 . . ? C14 C30 H30A 120.2 . . ? C13 C31 C27 105.9(8) . . ? C13 C31 H31A 110.5 . . ? C27 C31 H31A 110.5 . . ? C13 C31 H31B 110.5 . . ? C27 C31 H31B 110.5 . . ? H31A C31 H31B 108.7 . . ? C19 C32 H32A 120.0 . . ? C19 C32 H32B 120.0 . . ? H32A C32 H32B 120.0 . . ? O2 C49 H49A 109.5 . . ? O2 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? O2 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N3 C40 C23 175(2) . . ? C41 N4 Cu2 176.0(12) . . ? N4 C41 Cu1 173.5(12) . . ? C43 N5 Cu2 178.7(15) . . ? C44 N6 Cu2 170.4(15) . . ? N5 C43 Cu3 173.5(16) . 4_556 ? N6 C44 Cu3 172.9(15) . 4_557 ? _diffrn_measured_fraction_theta_max 0.896 _diffrn_reflns_theta_full 33.44 _diffrn_measured_fraction_theta_full 0.896 _refine_diff_density_max 0.862 _refine_diff_density_min -0.680 _refine_diff_density_rms 0.130 # Attachment '2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 297354' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H28 Br1.50 Cu2.50 N5 O' _chemical_formula_weight 741.28 _chemical_absolute_configuration rm loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 30.762(10) _cell_length_b 8.711(3) _cell_length_c 10.642(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.471(6) _cell_angle_gamma 90.00 _cell_volume 2761.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1256 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 26.22 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.783 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 4.119 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.680 _exptl_absorpt_correction_T_max 0.781 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6895 _diffrn_reflns_av_R_equivalents 0.0893 _diffrn_reflns_av_sigmaI/netI 0.1098 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 24.83 _reflns_number_total 4439 _reflns_number_gt 3145 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1286P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_number_reflns 4439 _refine_ls_number_parameters 353 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0989 _refine_ls_R_factor_gt 0.0779 _refine_ls_wR_factor_ref 0.2073 _refine_ls_wR_factor_gt 0.1955 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu3 Cu 0.41744(5) -0.0374(2) 0.46016(15) 0.0517(5) Uani 1 1 d . . . Cu2 Cu 0.27714(6) -0.09768(18) 0.11285(16) 0.0507(5) Uani 1 1 d . . . Br2 Br 0.43817(4) -0.35816(16) 0.55438(14) 0.0519(4) Uani 1 1 d . . . N2 N 0.3836(3) 0.4045(11) 1.1607(8) 0.0280(19) Uani 1 1 d . . . N3 N 0.3389(3) -0.0840(11) 0.2237(10) 0.039(2) Uani 1 1 d . . . C27 C 0.3201(3) 0.3909(13) 1.2786(11) 0.028(2) Uani 1 1 d . . . N1 N 0.3989(3) 0.0791(13) 0.6128(10) 0.039(2) Uani 1 1 d . . . C26 C 0.2888(3) 0.4141(13) 1.5018(10) 0.030(2) Uani 1 1 d . . . C25 C 0.3965(4) 0.3324(14) 1.0427(10) 0.034(3) Uani 1 1 d . . . H25A H 0.3992 0.2215 1.0584 0.041 Uiso 1 1 calc R . . C24 C 0.3707(4) -0.0713(14) 0.3109(11) 0.038(3) Uani 1 1 d . . . C23 C 0.3712(4) 0.0218(13) 0.6807(11) 0.030(3) Uani 1 1 d . . . C22 C 0.2933(4) 0.5437(14) 1.4336(12) 0.038(3) Uani 1 1 d . . . H22A H 0.2855 0.6388 1.4614 0.045 Uiso 1 1 calc R . . C21 C 0.3001(4) 0.2711(13) 1.4581(12) 0.036(3) Uani 1 1 d . . . H21A H 0.2973 0.1827 1.5044 0.044 Uiso 1 1 calc R . . C20 C 0.2724(4) 0.4202(15) 1.6172(11) 0.038(3) Uani 1 1 d . . . C19 C 0.4663(4) 0.4603(18) 1.1714(13) 0.051(4) Uani 1 1 d . . . H19A H 0.4978 0.4805 1.1734 0.061 Uiso 1 1 calc R . . C18 C 0.3594(4) 0.1065(13) 0.7826(11) 0.034(3) Uani 1 1 d . . . C17 C 0.3354(4) 0.3735(15) 1.1547(11) 0.037(3) Uani 1 1 d . . . H17A H 0.3287 0.2694 1.1235 0.044 Uiso 1 1 calc R . . H17B H 0.3173 0.4416 1.0903 0.044 Uiso 1 1 calc R . . C16 C 0.4147(4) 0.3330(14) 1.2829(11) 0.035(3) Uani 1 1 d . . . H16A H 0.4096 0.3824 1.3597 0.042 Uiso 1 1 calc R . . H16B H 0.4078 0.2247 1.2870 0.042 Uiso 1 1 calc R . . C15 C 0.3919(4) 0.5760(13) 1.1681(12) 0.039(3) Uani 1 1 d . . . H15A H 0.3818 0.6180 1.2403 0.047 Uiso 1 1 calc R . . H15B H 0.3746 0.6240 1.0892 0.047 Uiso 1 1 calc R . . C14 C 0.3617(5) 0.3554(14) 0.9103(12) 0.042(3) Uani 1 1 d . . . H14A H 0.3317 0.3256 0.9176 0.050 Uiso 1 1 calc R . . N4 N 0.2596(4) 0.4172(14) 1.7088(11) 0.051(3) Uani 1 1 d . . . C13 C 0.3149(4) 0.2609(14) 1.3517(12) 0.037(3) Uani 1 1 d . . . H13A H 0.3220 0.1648 1.3245 0.045 Uiso 1 1 calc R . . C12 C 0.4426(4) 0.3901(17) 1.0411(12) 0.044(3) Uani 1 1 d . . . H12A H 0.4399 0.4666 0.9734 0.053 Uiso 1 1 calc R . . H12B H 0.4604 0.3056 1.0216 0.053 Uiso 1 1 calc R . . C11 C 0.3747(4) 0.2624(14) 0.8075(11) 0.037(3) Uani 1 1 d . . . C10 C 0.4137(4) 0.217(2) 0.6398(13) 0.054(4) Uani 1 1 d . . . H10A H 0.4337 0.2550 0.5950 0.065 Uiso 1 1 calc R . . C9 C 0.3521(4) -0.1244(14) 0.6471(12) 0.039(3) Uani 1 1 d . . . H9A H 0.3597 -0.1799 0.5809 0.047 Uiso 1 1 calc R . . O1 O 0.3624(4) 0.5160(10) 0.8795(9) 0.068(3) Uani 1 1 d . . . H1A H 0.3444 0.5327 0.8098 0.102 Uiso 1 1 calc R . . C8 C 0.3094(4) 0.5338(14) 1.3221(12) 0.039(3) Uani 1 1 d . . . H8A H 0.3130 0.6224 1.2769 0.047 Uiso 1 1 calc R . . C7 C 0.4636(4) 0.3521(16) 1.2801(13) 0.047(3) Uani 1 1 d . . . H7A H 0.4807 0.3931 1.3623 0.057 Uiso 1 1 calc R . . H7B H 0.4762 0.2533 1.2665 0.057 Uiso 1 1 calc R . . C6 C 0.4421(5) 0.6142(17) 1.1858(14) 0.055(4) Uani 1 1 d . . . H6A H 0.4540 0.6527 1.2742 0.066 Uiso 1 1 calc R . . C5 C 0.4015(5) 0.3171(16) 0.7351(12) 0.048(3) Uani 1 1 d . . . H5A H 0.4121 0.4175 0.7459 0.057 Uiso 1 1 calc R . . C4 C 0.3294(5) 0.0381(17) 0.8483(13) 0.055(4) Uani 1 1 d . . . H4A H 0.3216 0.0900 0.9158 0.066 Uiso 1 1 calc R . . C3 C 0.3227(5) -0.1855(16) 0.7105(13) 0.048(3) Uani 1 1 d . . . H3A H 0.3099 -0.2808 0.6851 0.057 Uiso 1 1 calc R . . C2 C 0.3115(5) -0.1092(18) 0.8109(14) 0.057(4) Uani 1 1 d . . . H2A H 0.2921 -0.1546 0.8544 0.069 Uiso 1 1 calc R . . Br1 Br 0.5000 0.0266(9) 0.5000 0.277(5) Uani 1 2 d S . . N5 N 0.2510(4) 0.1041(14) 0.0274(10) 0.039(3) Uani 1 1 d . . . C1 C 0.2426(4) 0.2036(16) -0.0233(13) 0.029(3) Uani 1 1 d . . . Cu1 Cu 0.5000 -0.2450(3) 0.5000 0.0594(7) Uani 1 2 d S . . C28 C 0.4497(7) 0.735(2) 1.092(2) 0.094(7) Uani 1 1 d D . . H28A H 0.4437 0.7127 1.0037 0.113 Uiso 1 1 calc R . . C29 C 0.4654(16) 0.879(3) 1.136(5) 0.25(3) Uani 1 1 d D . . H29A H 0.4714 0.9017 1.2238 0.303 Uiso 1 1 calc R . . H29B H 0.4700 0.9528 1.0774 0.303 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu3 0.0350(9) 0.0806(13) 0.0372(9) -0.0169(8) 0.0046(7) 0.0008(8) Cu2 0.0520(10) 0.0349(8) 0.0518(10) -0.0002(8) -0.0123(8) -0.0010(7) Br2 0.0485(8) 0.0530(8) 0.0563(9) 0.0084(7) 0.0170(6) 0.0057(7) N2 0.029(5) 0.024(4) 0.031(5) -0.005(4) 0.006(4) 0.001(4) N3 0.040(6) 0.021(5) 0.055(6) -0.010(5) 0.010(5) 0.002(4) C27 0.025(6) 0.022(5) 0.037(6) -0.008(5) 0.008(5) 0.005(5) N1 0.037(6) 0.046(6) 0.037(6) -0.016(5) 0.014(5) -0.018(5) C26 0.029(6) 0.029(6) 0.032(6) -0.003(5) 0.006(5) -0.002(5) C25 0.042(7) 0.040(7) 0.023(6) -0.006(5) 0.014(5) 0.005(5) C24 0.031(6) 0.044(8) 0.037(7) -0.004(6) 0.005(5) 0.005(5) C23 0.025(6) 0.039(7) 0.028(6) -0.010(5) 0.009(5) 0.003(5) C22 0.044(7) 0.031(7) 0.040(7) -0.016(6) 0.016(6) 0.001(5) C21 0.040(7) 0.025(6) 0.050(8) 0.003(6) 0.022(6) 0.008(5) C20 0.037(7) 0.047(8) 0.030(6) -0.008(6) 0.008(5) 0.001(6) C19 0.028(6) 0.078(10) 0.046(8) -0.013(7) 0.006(6) -0.013(7) C18 0.033(6) 0.042(8) 0.029(6) -0.002(5) 0.014(5) -0.005(5) C17 0.028(6) 0.047(8) 0.033(6) -0.008(5) 0.005(5) -0.001(5) C16 0.034(7) 0.041(7) 0.030(6) 0.002(6) 0.007(5) 0.000(5) C15 0.055(8) 0.027(6) 0.035(7) -0.009(5) 0.012(6) -0.006(6) C14 0.055(8) 0.037(7) 0.033(7) -0.009(5) 0.013(6) 0.000(6) N4 0.056(7) 0.051(7) 0.051(7) -0.001(6) 0.022(6) -0.003(5) C13 0.042(7) 0.026(6) 0.051(8) -0.001(6) 0.024(6) 0.007(5) C12 0.040(7) 0.054(8) 0.044(7) -0.018(6) 0.021(6) -0.012(6) C11 0.046(7) 0.040(7) 0.024(6) -0.008(5) 0.009(5) 0.004(6) C10 0.039(7) 0.093(12) 0.037(7) -0.006(8) 0.021(6) -0.013(8) C9 0.036(7) 0.041(8) 0.042(7) -0.019(6) 0.012(5) 0.003(5) O1 0.122(9) 0.032(5) 0.037(5) -0.004(4) -0.002(6) 0.025(5) C8 0.052(8) 0.028(6) 0.040(7) 0.004(5) 0.014(6) 0.011(5) C7 0.027(7) 0.064(9) 0.047(8) 0.003(7) -0.001(6) 0.006(6) C6 0.053(8) 0.061(10) 0.051(8) -0.008(7) 0.015(7) -0.024(7) C5 0.070(10) 0.047(8) 0.028(6) -0.021(6) 0.016(6) -0.023(7) C4 0.066(10) 0.062(10) 0.049(8) -0.024(7) 0.035(8) -0.023(7) C3 0.062(9) 0.038(7) 0.043(7) -0.004(6) 0.010(7) -0.012(6) C2 0.066(10) 0.058(9) 0.058(9) -0.013(8) 0.035(7) -0.028(8) Br1 0.520(16) 0.134(5) 0.195(6) 0.000 0.125(8) 0.000 N5 0.053(7) 0.045(8) 0.021(5) -0.010(5) 0.013(5) -0.026(6) C1 0.021(6) 0.028(6) 0.035(7) -0.014(6) 0.002(5) -0.003(5) Cu1 0.0542(15) 0.0796(19) 0.0443(14) 0.000 0.0123(11) 0.000 C28 0.120(15) 0.076(13) 0.116(15) -0.036(12) 0.086(13) -0.058(12) C29 0.39(7) 0.09(2) 0.37(6) -0.03(3) 0.27(6) -0.04(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu3 C24 1.880(12) . ? Cu3 N1 2.112(10) . ? Cu3 Br1 2.530(2) . ? Cu3 Cu1 3.059(3) . ? Cu2 N3 1.973(10) . ? Cu2 C1 1.996(16) 4_545 ? Cu2 N5 2.049(14) . ? Cu2 N4 2.444(12) 4_547 ? Br2 Cu1 2.3398(19) . ? N2 C17 1.493(14) . ? N2 C15 1.515(16) . ? N2 C16 1.541(14) . ? N2 C25 1.542(13) . ? N3 C24 1.174(14) . ? C27 C8 1.396(16) . ? C27 C13 1.405(17) . ? C27 C17 1.514(15) . ? N1 C10 1.290(19) . ? N1 C23 1.343(15) . ? C26 C22 1.368(17) . ? C26 C21 1.404(16) . ? C26 C20 1.440(16) . ? C25 C12 1.508(17) . ? C25 C14 1.555(17) . ? C25 H25A 0.9800 . ? C23 C9 1.411(17) . ? C23 C18 1.432(15) . ? C22 C8 1.398(16) . ? C22 H22A 0.9300 . ? C21 C13 1.323(16) . ? C21 H21A 0.9300 . ? C20 N4 1.139(15) . ? C19 C7 1.51(2) . ? C19 C12 1.524(17) . ? C19 C6 1.56(2) . ? C19 H19A 0.9800 . ? C18 C4 1.420(16) . ? C18 C11 1.440(17) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C16 C7 1.520(16) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C15 C6 1.542(17) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C14 O1 1.439(17) . ? C14 C11 1.493(16) . ? C14 H14A 0.9800 . ? N4 Cu2 2.444(12) 4_557 ? C13 H13A 0.9300 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C11 C5 1.349(17) . ? C10 C5 1.458(19) . ? C10 H10A 0.9300 . ? C9 C3 1.366(18) . ? C9 H9A 0.9300 . ? O1 H1A 0.8200 . ? C8 H8A 0.9300 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C6 C28 1.51(2) . ? C6 H6A 0.9800 . ? C5 H5A 0.9300 . ? C4 C2 1.41(2) . ? C4 H4A 0.9300 . ? C3 C2 1.373(19) . ? C3 H3A 0.9300 . ? C2 H2A 0.9300 . ? Br1 Cu1 2.366(8) . ? Br1 Cu3 2.530(2) 2_656 ? N5 C1 1.019(13) . ? C1 Cu2 1.996(16) 4 ? Cu1 Br2 2.3398(19) 2_656 ? Cu1 Cu3 3.059(3) 2_656 ? C28 C29 1.381(10) . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? C29 H29B 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C24 Cu3 N1 115.4(4) . . ? C24 Cu3 Br1 134.4(4) . . ? N1 Cu3 Br1 102.6(3) . . ? C24 Cu3 Cu1 117.2(4) . . ? N1 Cu3 Cu1 123.5(3) . . ? Br1 Cu3 Cu1 48.97(17) . . ? N3 Cu2 C1 118.1(4) . 4_545 ? N3 Cu2 N5 115.2(4) . . ? C1 Cu2 N5 119.6(4) 4_545 . ? N3 Cu2 N4 95.5(4) . 4_547 ? C1 Cu2 N4 105.8(5) 4_545 4_547 ? N5 Cu2 N4 95.3(4) . 4_547 ? C17 N2 C15 109.5(8) . . ? C17 N2 C16 111.3(9) . . ? C15 N2 C16 107.0(9) . . ? C17 N2 C25 110.3(8) . . ? C15 N2 C25 111.7(9) . . ? C16 N2 C25 106.9(8) . . ? C24 N3 Cu2 165.1(10) . . ? C8 C27 C13 117.8(10) . . ? C8 C27 C17 121.9(11) . . ? C13 C27 C17 120.3(10) . . ? C10 N1 C23 117.6(11) . . ? C10 N1 Cu3 118.0(9) . . ? C23 N1 Cu3 124.4(8) . . ? C22 C26 C21 119.3(10) . . ? C22 C26 C20 121.7(11) . . ? C21 C26 C20 119.0(11) . . ? C12 C25 N2 107.9(9) . . ? C12 C25 C14 112.5(10) . . ? N2 C25 C14 115.2(9) . . ? C12 C25 H25A 106.9 . . ? N2 C25 H25A 106.9 . . ? C14 C25 H25A 106.9 . . ? N3 C24 Cu3 173.3(10) . . ? N1 C23 C9 118.6(10) . . ? N1 C23 C18 122.1(10) . . ? C9 C23 C18 119.3(10) . . ? C26 C22 C8 120.2(11) . . ? C26 C22 H22A 119.9 . . ? C8 C22 H22A 119.9 . . ? C13 C21 C26 120.6(11) . . ? C13 C21 H21A 119.7 . . ? C26 C21 H21A 119.7 . . ? N4 C20 C26 176.6(14) . . ? C7 C19 C12 109.9(12) . . ? C7 C19 C6 110.0(11) . . ? C12 C19 C6 107.6(11) . . ? C7 C19 H19A 109.8 . . ? C12 C19 H19A 109.8 . . ? C6 C19 H19A 109.8 . . ? C4 C18 C23 118.4(11) . . ? C4 C18 C11 121.8(11) . . ? C23 C18 C11 119.5(10) . . ? N2 C17 C27 117.8(9) . . ? N2 C17 H17A 107.8 . . ? C27 C17 H17A 107.8 . . ? N2 C17 H17B 107.8 . . ? C27 C17 H17B 107.8 . . ? H17A C17 H17B 107.2 . . ? C7 C16 N2 110.3(9) . . ? C7 C16 H16A 109.6 . . ? N2 C16 H16A 109.6 . . ? C7 C16 H16B 109.6 . . ? N2 C16 H16B 109.6 . . ? H16A C16 H16B 108.1 . . ? N2 C15 C6 111.7(10) . . ? N2 C15 H15A 109.3 . . ? C6 C15 H15A 109.3 . . ? N2 C15 H15B 109.3 . . ? C6 C15 H15B 109.3 . . ? H15A C15 H15B 107.9 . . ? O1 C14 C11 109.8(11) . . ? O1 C14 C25 106.6(10) . . ? C11 C14 C25 110.2(10) . . ? O1 C14 H14A 110.1 . . ? C11 C14 H14A 110.1 . . ? C25 C14 H14A 110.1 . . ? C20 N4 Cu2 172.7(10) . 4_557 ? C21 C13 C27 122.1(11) . . ? C21 C13 H13A 119.0 . . ? C27 C13 H13A 119.0 . . ? C25 C12 C19 111.2(10) . . ? C25 C12 H12A 109.4 . . ? C19 C12 H12A 109.4 . . ? C25 C12 H12B 109.4 . . ? C19 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C5 C11 C18 116.5(11) . . ? C5 C11 C14 122.7(12) . . ? C18 C11 C14 120.8(11) . . ? N1 C10 C5 125.0(12) . . ? N1 C10 H10A 117.5 . . ? C5 C10 H10A 117.5 . . ? C3 C9 C23 120.7(11) . . ? C3 C9 H9A 119.6 . . ? C23 C9 H9A 119.6 . . ? C14 O1 H1A 109.5 . . ? C27 C8 C22 120.0(11) . . ? C27 C8 H8A 120.0 . . ? C22 C8 H8A 120.0 . . ? C19 C7 C16 109.2(10) . . ? C19 C7 H7A 109.8 . . ? C16 C7 H7A 109.8 . . ? C19 C7 H7B 109.8 . . ? C16 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? C28 C6 C15 112.6(14) . . ? C28 C6 C19 112.2(13) . . ? C15 C6 C19 106.9(10) . . ? C28 C6 H6A 108.3 . . ? C15 C6 H6A 108.3 . . ? C19 C6 H6A 108.3 . . ? C11 C5 C10 119.1(12) . . ? C11 C5 H5A 120.4 . . ? C10 C5 H5A 120.4 . . ? C2 C4 C18 119.8(12) . . ? C2 C4 H4A 120.1 . . ? C18 C4 H4A 120.1 . . ? C9 C3 C2 121.5(12) . . ? C9 C3 H3A 119.3 . . ? C2 C3 H3A 119.3 . . ? C3 C2 C4 120.2(12) . . ? C3 C2 H2A 119.9 . . ? C4 C2 H2A 119.9 . . ? Cu1 Br1 Cu3 77.26(17) . . ? Cu1 Br1 Cu3 77.26(17) . 2_656 ? Cu3 Br1 Cu3 154.5(3) . 2_656 ? C1 N5 Cu2 169.6(11) . . ? N5 C1 Cu2 175.2(12) . 4 ? Br2 Cu1 Br2 130.16(15) . 2_656 ? Br2 Cu1 Br1 114.92(7) . . ? Br2 Cu1 Br1 114.92(7) 2_656 . ? Br2 Cu1 Cu3 65.50(6) . . ? Br2 Cu1 Cu3 155.88(7) 2_656 . ? Br1 Cu1 Cu3 53.78(6) . . ? Br2 Cu1 Cu3 155.88(7) . 2_656 ? Br2 Cu1 Cu3 65.50(6) 2_656 2_656 ? Br1 Cu1 Cu3 53.78(6) . 2_656 ? Cu3 Cu1 Cu3 107.55(11) . 2_656 ? C29 C28 C6 120(3) . . ? C29 C28 H28A 119.8 . . ? C6 C28 H28A 119.8 . . ? C28 C29 H29A 120.0 . . ? C28 C29 H29B 120.0 . . ? H29A C29 H29B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 24.83 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.030 _refine_diff_density_min -1.517 _refine_diff_density_rms 0.201