# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Ghosh, Ashutosh' _publ_contact_author_email 'ghosh 59@yahoo.com' _publ_section_title ; Two unusual mixed-valent trinuclear CuII2CuI complexes containing copper(I) tribromide dianion as bridging ligand: Identification of an unprecedented doubly hydrogen-bonded water dimer ; _publ_author_name A.Ghosh data_1 _database_code_depnum_ccdc_archive 'CCDC 793723' #TrackingRef '1-2.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H32 Br5 Cu3 N4 O2, 2(H2 O)' _chemical_formula_sum 'C22 H36 Br5 Cu3 N4 O4' _chemical_formula_weight 1010.72 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_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.979(10) _cell_length_b 10.157(4) _cell_length_c 15.902(7) _cell_angle_alpha 90.00 _cell_angle_beta 118.944(4) _cell_angle_gamma 90.00 _cell_volume 3248(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2239 _cell_measurement_theta_min 2.03 _cell_measurement_theta_max 23.03 _exptl_crystal_description plate _exptl_crystal_colour 'deep brown' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.067 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 8.131 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.307 _exptl_absorpt_correction_T_max 0.375 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _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 6068 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 23.03 _reflns_number_total 2239 _reflns_number_gt 1508 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for windows (Farrugia, 1997)' _computing_publication_material 'Platon99 (Spek, 1999)' _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^)+(0.1234P)^2^+13.6695P] 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 nonref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2239 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.2024 _refine_ls_wR_factor_gt 0.1790 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Br4 Br 0.19908(8) 0.9554(2) 0.27629(12) 0.0989(7) Uani 1 1 d . . . Br1 Br 0.53508(9) 1.09392(14) 0.39815(9) 0.0790(6) Uani 1 1 d . . . Br2 Br 0.5000 1.4398(2) 0.2500 0.1146(10) Uani 1 2 d S . . Cu1 Cu 0.53266(6) 0.83447(14) 0.35947(9) 0.0429(5) Uani 1 1 d . . . Cu2 Cu 0.5000 1.2088(3) 0.2500 0.0741(8) Uani 1 2 d S . . O1 O 0.4455(3) 0.8486(8) 0.2442(5) 0.0481(19) Uani 1 1 d . . . N2 N 0.6208(5) 0.7704(11) 0.4708(6) 0.060(3) Uani 1 1 d . . . C4 C 0.2789(6) 0.9238(16) 0.2681(9) 0.067(4) Uani 1 1 d . . . C5 C 0.3209(5) 0.8280(12) 0.3224(8) 0.044(3) Uani 1 1 d . . . H5 H 0.3127 0.7800 0.3654 0.053 Uiso 1 1 calc R . . C6 C 0.3763(5) 0.8031(11) 0.3126(7) 0.040(3) Uani 1 1 d . . . C7 C 0.4249(6) 0.6988(11) 0.3731(9) 0.052(3) Uani 1 1 d . . . H7A H 0.4095 0.6569 0.4136 0.062 Uiso 1 1 calc R . . H7B H 0.4282 0.6321 0.3320 0.062 Uiso 1 1 calc R . . N1 N 0.4913(4) 0.7597(9) 0.4340(6) 0.045(2) Uani 1 1 d . . . H1 H 0.4856 0.8272 0.4669 0.054 Uiso 1 1 calc R . . C1 C 0.3898(5) 0.8747(12) 0.2520(8) 0.051(3) Uani 1 1 d . . . C2 C 0.3497(7) 0.9804(15) 0.2021(10) 0.071(4) Uani 1 1 d . . . H2 H 0.3609 1.0337 0.1645 0.086 Uiso 1 1 calc R . . C3 C 0.2930(7) 1.0059(16) 0.2090(10) 0.076(4) Uani 1 1 d . . . H3 H 0.2649 1.0754 0.1755 0.092 Uiso 1 1 calc R . . C8 C 0.5393(6) 0.6684(13) 0.5051(10) 0.068(4) Uani 1 1 d . . . H8A H 0.5394 0.5858 0.4744 0.081 Uiso 1 1 calc R . . H8B H 0.5275 0.6506 0.5548 0.081 Uiso 1 1 calc R . . C9 C 0.6063(7) 0.7304(16) 0.5478(9) 0.078(4) Uani 1 1 d . . . H9A H 0.6076 0.8068 0.5853 0.094 Uiso 1 1 calc R . . H9B H 0.6397 0.6683 0.5903 0.094 Uiso 1 1 calc R . . C10 C 0.6765(7) 0.8643(17) 0.5160(10) 0.092(5) Uani 1 1 d . . . H10A H 0.6886 0.8939 0.4692 0.138 Uiso 1 1 calc R . . H10B H 0.7140 0.8218 0.5680 0.138 Uiso 1 1 calc R . . H10C H 0.6633 0.9384 0.5403 0.138 Uiso 1 1 calc R . . C11 C 0.6439(7) 0.6586(15) 0.4354(11) 0.084(4) Uani 1 1 d . . . H11A H 0.6529 0.6884 0.3856 0.126 Uiso 1 1 calc R . . H11B H 0.6100 0.5920 0.4101 0.126 Uiso 1 1 calc R . . H11C H 0.6837 0.6225 0.4873 0.126 Uiso 1 1 calc R . . O2W O 0.3146(16) 0.689(2) 0.5274(15) 0.43(3) Uani 1 1 d . . . H1W2 H 0.2913 0.7279 0.5484 0.515 Uiso 1 1 d R . . H2W2 H 0.3665 0.7063 0.5833 0.515 Uiso 1 1 d 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 Br4 0.0585(10) 0.1444(18) 0.0921(12) -0.0257(11) 0.0352(9) 0.0158(10) Br1 0.1417(15) 0.0524(9) 0.0626(9) -0.0058(6) 0.0651(10) 0.0002(9) Br2 0.172(3) 0.0508(15) 0.0961(18) 0.000 0.0447(18) 0.000 Cu1 0.0405(8) 0.0541(10) 0.0372(8) 0.0009(6) 0.0213(6) 0.0011(7) Cu2 0.0909(18) 0.0674(17) 0.0751(16) 0.000 0.0490(14) 0.000 O1 0.041(4) 0.068(5) 0.037(4) 0.008(4) 0.020(3) 0.013(4) N2 0.044(6) 0.084(8) 0.045(6) 0.000(5) 0.017(5) -0.001(6) C4 0.042(7) 0.097(11) 0.058(8) -0.033(8) 0.021(6) 0.000(8) C5 0.029(6) 0.056(8) 0.047(6) 0.000(5) 0.018(5) 0.001(6) C6 0.032(6) 0.050(7) 0.037(6) 0.002(5) 0.015(5) 0.000(5) C7 0.051(7) 0.041(7) 0.084(8) 0.000(6) 0.049(7) -0.004(6) N1 0.049(6) 0.046(6) 0.046(5) 0.002(4) 0.028(5) 0.008(5) C1 0.032(6) 0.071(9) 0.038(6) -0.002(6) 0.008(5) 0.013(6) C2 0.059(9) 0.089(11) 0.073(9) 0.013(8) 0.038(8) 0.016(8) C3 0.062(9) 0.097(12) 0.064(9) 0.019(8) 0.026(7) 0.036(8) C8 0.062(9) 0.056(9) 0.084(10) 0.039(7) 0.035(7) 0.027(7) C9 0.062(9) 0.109(13) 0.058(8) 0.029(8) 0.024(7) 0.027(9) C10 0.062(9) 0.116(14) 0.067(10) -0.018(9) 0.008(8) -0.013(9) C11 0.069(10) 0.087(12) 0.080(10) -0.006(9) 0.024(8) 0.027(9) O2W 0.63(6) 0.21(2) 0.139(17) 0.059(14) -0.06(2) -0.23(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 Br4 C4 1.928(12) . ? Br1 Cu2 2.392(2) . ? Br1 Cu1 2.701(2) . ? Br2 Cu2 2.346(4) . ? Cu1 O1 1.947(6) 2_655 ? Cu1 O1 1.959(7) . ? Cu1 N1 1.994(8) . ? Cu1 N2 2.047(9) . ? Cu1 Cu1 3.052(3) 2_655 ? Cu2 Br1 2.392(2) 2_655 ? O1 C1 1.371(12) . ? O1 Cu1 1.947(6) 2_655 ? N2 C9 1.473(15) . ? N2 C10 1.475(17) . ? N2 C11 1.476(16) . ? C4 C5 1.348(18) . ? C4 C3 1.406(19) . ? C5 C6 1.378(13) . ? C5 H5 0.9300 . ? C6 C1 1.358(15) . ? C6 C7 1.502(15) . ? C7 N1 1.490(14) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? N1 C8 1.465(14) . ? N1 H1 0.9100 . ? C1 C2 1.387(17) . ? C2 C3 1.386(17) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C8 C9 1.488(18) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? O2W H1W2 0.8512 . ? O2W H2W2 1.1025 . ? 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 Cu2 Br1 Cu1 106.96(8) . . ? O1 Cu1 O1 76.6(3) 2_655 . ? O1 Cu1 N1 157.5(4) 2_655 . ? O1 Cu1 N1 91.1(3) . . ? O1 Cu1 N2 101.7(3) 2_655 . ? O1 Cu1 N2 165.5(4) . . ? N1 Cu1 N2 85.5(4) . . ? O1 Cu1 Br1 97.8(2) 2_655 . ? O1 Cu1 Br1 92.3(2) . . ? N1 Cu1 Br1 101.5(3) . . ? N2 Cu1 Br1 102.1(3) . . ? O1 Cu1 Cu1 38.8(2) 2_655 2_655 ? O1 Cu1 Cu1 38.46(19) . 2_655 ? N1 Cu1 Cu1 124.4(3) . 2_655 ? N2 Cu1 Cu1 136.2(3) . 2_655 ? Br1 Cu1 Cu1 101.79(4) . 2_655 ? Br2 Cu2 Br1 119.19(7) . 2_655 ? Br2 Cu2 Br1 119.19(7) . . ? Br1 Cu2 Br1 121.62(13) 2_655 . ? C1 O1 Cu1 136.5(6) . 2_655 ? C1 O1 Cu1 120.4(6) . . ? Cu1 O1 Cu1 102.8(3) 2_655 . ? C9 N2 C10 105.4(11) . . ? C9 N2 C11 111.9(12) . . ? C10 N2 C11 107.3(11) . . ? C9 N2 Cu1 106.2(7) . . ? C10 N2 Cu1 118.6(9) . . ? C11 N2 Cu1 107.6(7) . . ? C5 C4 C3 122.2(11) . . ? C5 C4 Br4 119.1(11) . . ? C3 C4 Br4 118.7(11) . . ? C4 C5 C6 118.2(11) . . ? C4 C5 H5 120.9 . . ? C6 C5 H5 120.9 . . ? C1 C6 C5 121.5(10) . . ? C1 C6 C7 118.5(9) . . ? C5 C6 C7 119.9(9) . . ? N1 C7 C6 109.6(9) . . ? N1 C7 H7A 109.8 . . ? C6 C7 H7A 109.8 . . ? N1 C7 H7B 109.8 . . ? C6 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? C8 N1 C7 113.1(9) . . ? C8 N1 Cu1 107.6(7) . . ? C7 N1 Cu1 113.9(6) . . ? C8 N1 H1 107.3 . . ? C7 N1 H1 107.3 . . ? Cu1 N1 H1 107.3 . . ? C6 C1 O1 120.3(10) . . ? C6 C1 C2 120.3(10) . . ? O1 C1 C2 119.2(11) . . ? C3 C2 C1 119.2(13) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 118.1(13) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? N1 C8 C9 108.1(10) . . ? N1 C8 H8A 110.1 . . ? C9 C8 H8A 110.1 . . ? N1 C8 H8B 110.1 . . ? C9 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? N2 C9 C8 109.7(11) . . ? N2 C9 H9A 109.7 . . ? C8 C9 H9A 109.7 . . ? N2 C9 H9B 109.7 . . ? C8 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? N2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? H1W2 O2W H2W2 104.7 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 23.03 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.193 _refine_diff_density_min -1.208 _refine_diff_density_rms 0.160 data_2 _database_code_depnum_ccdc_archive 'CCDC 793724' #TrackingRef '1-2.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H38 Br3 Cu3 N4 O2, 2(C H4 O)' _chemical_formula_sum 'C26 H46 Br3 Cu3 N4 O4' _chemical_formula_weight 909.02 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_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.267(3) _cell_length_b 11.0415(16) _cell_length_c 15.727(2) _cell_angle_alpha 90.00 _cell_angle_beta 122.907(2) _cell_angle_gamma 90.00 _cell_volume 3392.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3359 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 26.22 _exptl_crystal_description plate _exptl_crystal_colour 'deep brown' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.780 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 5.433 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.436 _exptl_absorpt_correction_T_max 0.521 _exptl_absorpt_process_details ? _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 ? _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 12417 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 26.22 _reflns_number_total 3359 _reflns_number_gt 1873 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for windows (Farrugia, 1997)' _computing_publication_material 'Platon99 (Spek, 1999)' _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^)+(0.1385P)^2^+8.8251P] 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 nonref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3359 _refine_ls_number_parameters 192 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1291 _refine_ls_R_factor_gt 0.0712 _refine_ls_wR_factor_ref 0.2423 _refine_ls_wR_factor_gt 0.2055 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.46424(6) 0.92620(10) 0.09580(8) 0.0795(4) Uani 1 1 d . . . Cu1 Cu 0.46709(5) 1.16305(10) 0.13570(8) 0.0572(4) Uani 1 1 d . . . Cu2 Cu 0.5000 0.8234(2) 0.2500 0.1019(7) Uani 1 2 d S . . Br2 Br 0.5000 0.6042(6) 0.2500 0.141(3) Uani 0.60 2 d SP . . Br2A Br 0.4512(8) 0.6305(10) 0.2170(12) 0.166(6) Uani 0.20 1 d P . . O1 O 0.5570(3) 1.1546(5) 0.2637(4) 0.0606(15) Uani 1 1 d . . . N1 N 0.5112(4) 1.2283(7) 0.0654(5) 0.0618(19) Uani 1 1 d . . . H1 H 0.5172 1.1643 0.0345 0.074 Uiso 1 1 calc R . . N2 N 0.3766(4) 1.2258(8) 0.0141(6) 0.077(2) Uani 1 1 d . . . C6 C 0.6275(5) 1.1844(10) 0.1989(7) 0.069(3) Uani 1 1 d . . . C10 C 0.3942(6) 1.2530(12) -0.0635(8) 0.096(4) Uani 1 1 d . . . H10A H 0.3945 1.1782 -0.0957 0.115 Uiso 1 1 calc R . . H10B H 0.3595 1.3057 -0.1155 0.115 Uiso 1 1 calc R . . C9 C 0.4613(6) 1.3115(12) -0.0166(10) 0.096(4) Uani 1 1 d . . . H9A H 0.4609 1.3895 0.0114 0.115 Uiso 1 1 calc R . . H9B H 0.4734 1.3236 -0.0661 0.115 Uiso 1 1 calc R . . C1 C 0.6112(4) 1.1199(9) 0.2599(7) 0.065(2) Uani 1 1 d . . . C3 C 0.7060(5) 0.9868(12) 0.3104(9) 0.088(3) Uani 1 1 d . . . H3 H 0.7323 0.9201 0.3467 0.106 Uiso 1 1 calc R . . C2 C 0.6514(5) 1.0197(11) 0.3157(8) 0.082(3) Uani 1 1 d . . . H2 H 0.6408 0.9761 0.3561 0.099 Uiso 1 1 calc R . . C4 C 0.7218(5) 1.0508(15) 0.2524(11) 0.107(5) Uani 1 1 d . . . H4 H 0.7598 1.0285 0.2510 0.129 Uiso 1 1 calc R . . C12 C 0.3563(7) 1.3334(12) 0.0442(10) 0.111(5) Uani 1 1 d . . . H12A H 0.3463 1.3122 0.0941 0.166 Uiso 1 1 calc R . . H12B H 0.3162 1.3678 -0.0138 0.166 Uiso 1 1 calc R . . H12C H 0.3928 1.3915 0.0724 0.166 Uiso 1 1 calc R . . C5 C 0.6843(5) 1.1451(12) 0.1974(9) 0.083(3) Uani 1 1 d . . . H5 H 0.6959 1.1858 0.1571 0.100 Uiso 1 1 calc R . . C7 C 0.5797(5) 1.2849(10) 0.1324(9) 0.080(3) Uani 1 1 d . . . H7 H 0.5759 1.3422 0.1767 0.096 Uiso 1 1 calc R . . C11 C 0.3188(5) 1.1430(14) -0.0318(9) 0.111(5) Uani 1 1 d . . . H11A H 0.3302 1.0713 -0.0540 0.166 Uiso 1 1 calc R . . H11B H 0.2799 1.1816 -0.0887 0.166 Uiso 1 1 calc R . . H11C H 0.3080 1.1215 0.0171 0.166 Uiso 1 1 calc R . . C8 C 0.6122(13) 1.3519(19) 0.085(2) 0.217(12) Uani 1 1 d . . . H8A H 0.5822 1.4156 0.0421 0.326 Uiso 1 1 calc R . . H8B H 0.6198 1.2965 0.0447 0.326 Uiso 1 1 calc R . . H8C H 0.6551 1.3860 0.1368 0.326 Uiso 1 1 calc R . . O2 O 0.3189(17) 0.576(2) 0.1981(14) 0.56(4) Uani 1 1 d D . . H1O2 H 0.3429 0.6125 0.2554 0.666 Uiso 1 1 d RD . . C13 C 0.3128(8) 0.6375(16) 0.1092(17) 0.142(6) Uani 1 1 d D . . H13A H 0.3091 0.7234 0.1145 0.213 Uiso 1 1 calc R . . H13B H 0.2728 0.6083 0.0481 0.213 Uiso 1 1 calc R . . H13C H 0.3527 0.6201 0.1077 0.213 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.1003(8) 0.0694(7) 0.0708(7) -0.0066(5) 0.0478(6) 0.0039(5) Cu1 0.0527(6) 0.0644(7) 0.0530(7) 0.0056(5) 0.0278(5) 0.0091(5) Cu2 0.1103(16) 0.1022(17) 0.0911(15) 0.000 0.0534(13) 0.000 Br2 0.159(6) 0.078(3) 0.143(4) 0.000 0.055(5) 0.000 Br2A 0.280(19) 0.082(7) 0.197(15) -0.077(8) 0.170(15) -0.085(10) O1 0.047(3) 0.076(4) 0.057(4) 0.003(3) 0.027(3) 0.006(3) N1 0.073(5) 0.059(5) 0.066(5) 0.013(4) 0.045(4) 0.012(4) N2 0.053(4) 0.104(7) 0.058(5) 0.008(5) 0.021(4) 0.028(4) C6 0.062(5) 0.082(7) 0.071(6) -0.023(5) 0.041(5) -0.017(5) C10 0.100(8) 0.123(10) 0.062(6) 0.031(6) 0.043(6) 0.051(8) C9 0.101(9) 0.104(9) 0.104(9) 0.054(7) 0.069(8) 0.041(7) C1 0.050(5) 0.078(6) 0.059(6) -0.011(5) 0.025(4) -0.004(4) C3 0.045(5) 0.122(10) 0.087(8) -0.007(7) 0.029(6) 0.016(6) C2 0.064(6) 0.094(8) 0.074(7) 0.000(6) 0.028(5) 0.009(6) C4 0.039(5) 0.166(14) 0.098(9) -0.056(9) 0.025(6) 0.000(7) C12 0.137(11) 0.107(10) 0.092(9) 0.035(7) 0.065(9) 0.061(8) C5 0.062(6) 0.115(10) 0.074(7) -0.010(6) 0.038(6) -0.017(6) C7 0.092(8) 0.060(6) 0.108(8) 0.002(6) 0.067(7) -0.007(6) C11 0.063(7) 0.172(14) 0.068(7) 0.012(8) 0.017(6) 0.022(8) C8 0.23(2) 0.142(18) 0.33(4) 0.059(19) 0.18(3) 0.000(16) O2 0.70(7) 0.29(3) 0.169(19) -0.13(2) -0.09(3) 0.16(3) C13 0.102(10) 0.148(15) 0.19(2) -0.026(13) 0.087(12) -0.018(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Cu2 2.3809(16) . ? Br1 Cu1 2.6818(16) . ? Cu1 O1 1.948(6) 2_655 ? Cu1 O1 1.965(6) . ? Cu1 N1 2.007(7) . ? Cu1 N2 2.048(7) . ? Cu1 Cu1 3.048(2) 2_655 ? Cu2 Br2A 2.335(10) . ? Cu2 Br2A 2.335(10) 2_655 ? Cu2 Br1 2.3809(16) 2_655 ? Cu2 Br2 2.420(7) . ? Br2 Br2A 1.000(17) 2_655 ? Br2 Br2A 1.000(17) . ? Br2A Br2A 1.91(3) 2_655 ? O1 C1 1.349(10) . ? O1 Cu1 1.948(6) 2_655 ? N1 C7 1.488(12) . ? N1 C9 1.492(12) . ? N1 H1 0.9100 . ? N2 C12 1.451(14) . ? N2 C11 1.454(15) . ? N2 C10 1.514(13) . ? C6 C5 1.401(14) . ? C6 C1 1.404(14) . ? C6 C7 1.516(15) . ? C10 C9 1.465(17) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C1 C2 1.405(14) . ? C3 C4 1.353(19) . ? C3 C2 1.368(14) . ? C3 H3 0.9300 . ? C2 H2 0.9300 . ? C4 C5 1.332(18) . ? C4 H4 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C5 H5 0.9300 . ? C7 C8 1.52(2) . ? C7 H7 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? O2 C13 1.488(19) . ? O2 H1O2 0.8580 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? 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 Cu2 Br1 Cu1 106.01(7) . . ? O1 Cu1 O1 77.4(2) 2_655 . ? O1 Cu1 N1 157.5(3) 2_655 . ? O1 Cu1 N1 90.1(3) . . ? O1 Cu1 N2 99.9(3) 2_655 . ? O1 Cu1 N2 162.7(3) . . ? N1 Cu1 N2 86.4(3) . . ? O1 Cu1 Br1 99.33(18) 2_655 . ? O1 Cu1 Br1 94.05(18) . . ? N1 Cu1 Br1 100.1(2) . . ? N2 Cu1 Br1 103.2(3) . . ? O1 Cu1 Cu1 39.05(16) 2_655 2_655 ? O1 Cu1 Cu1 38.64(16) . 2_655 ? N1 Cu1 Cu1 124.8(2) . 2_655 ? N2 Cu1 Cu1 134.8(2) . 2_655 ? Br1 Cu1 Cu1 102.05(3) . 2_655 ? Br2A Cu2 Br2A 48.4(9) . 2_655 ? Br2A Cu2 Br1 121.3(4) . 2_655 ? Br2A Cu2 Br1 110.4(4) 2_655 2_655 ? Br2A Cu2 Br1 110.4(4) . . ? Br2A Cu2 Br1 121.3(4) 2_655 . ? Br1 Cu2 Br1 123.08(11) 2_655 . ? Br2A Cu2 Br2 24.2(4) . . ? Br2A Cu2 Br2 24.2(4) 2_655 . ? Br1 Cu2 Br2 118.46(6) 2_655 . ? Br1 Cu2 Br2 118.46(6) . . ? Br2A Br2 Br2A 146.3(18) 2_655 . ? Br2A Br2 Cu2 73.1(9) 2_655 . ? Br2A Br2 Cu2 73.1(9) . . ? Br2 Br2A Br2A 16.9(9) . 2_655 ? Br2 Br2A Cu2 82.7(9) . . ? Br2A Br2A Cu2 65.8(4) 2_655 . ? C1 O1 Cu1 137.5(6) . 2_655 ? C1 O1 Cu1 118.0(5) . . ? Cu1 O1 Cu1 102.3(2) 2_655 . ? C7 N1 C9 112.6(9) . . ? C7 N1 Cu1 115.6(6) . . ? C9 N1 Cu1 107.8(6) . . ? C7 N1 H1 106.8 . . ? C9 N1 H1 106.8 . . ? Cu1 N1 H1 106.8 . . ? C12 N2 C11 107.4(9) . . ? C12 N2 C10 112.3(10) . . ? C11 N2 C10 108.0(9) . . ? C12 N2 Cu1 108.9(7) . . ? C11 N2 Cu1 117.1(7) . . ? C10 N2 Cu1 103.3(6) . . ? C5 C6 C1 117.5(10) . . ? C5 C6 C7 124.1(10) . . ? C1 C6 C7 118.2(8) . . ? C9 C10 N2 111.2(9) . . ? C9 C10 H10A 109.4 . . ? N2 C10 H10A 109.4 . . ? C9 C10 H10B 109.4 . . ? N2 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C10 C9 N1 106.3(9) . . ? C10 C9 H9A 110.5 . . ? N1 C9 H9A 110.5 . . ? C10 C9 H9B 110.5 . . ? N1 C9 H9B 110.5 . . ? H9A C9 H9B 108.7 . . ? O1 C1 C6 119.5(9) . . ? O1 C1 C2 121.1(9) . . ? C6 C1 C2 119.4(9) . . ? C4 C3 C2 120.3(12) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C2 C1 119.7(11) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C5 C4 C3 121.6(10) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C4 C5 C6 121.5(11) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? N1 C7 C6 106.4(8) . . ? N1 C7 C8 118.9(13) . . ? C6 C7 C8 108.7(12) . . ? N1 C7 H7 107.4 . . ? C6 C7 H7 107.4 . . ? C8 C7 H7 107.4 . . ? N2 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C13 O2 H1O2 116.9 . . ? O2 C13 H13A 109.5 . . ? O2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.22 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.875 _refine_diff_density_min -1.276 _refine_diff_density_rms 0.132