# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global #TrackingRef '1-SJK-R3(875819).CIF' _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year 2012 _journal_volume 41 _journal_page_first 13441 loop_ _publ_contact_author_name 'Prof Jie Zhang' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences Fuzhou, Fujian, 350002, CHINA ; _publ_contact_author_email Zhangjie@fjirsm.ac.cn loop_ _publ_author_name 'Jian-Ke Sun.' 'Peng Wang.' 'Cheng Chen.' 'Xue-Jun Zhou.' 'Li-Ming Wu.' 'Yong-Fan Zhang.' 'Jie Zhang.' data_1 _database_code_depnum_ccdc_archive 'CCDC 875819' #TrackingRef '1-SJK-R3(875819).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H22 Br2 Cd N2 O5' _chemical_formula_sum 'C26 H22 Br2 Cd N2 O5' _chemical_formula_weight 714.68 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' Cd Cd -0.8075 1.2024 '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/c 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 19.058(8) _cell_length_b 8.910(3) _cell_length_c 16.588(7) _cell_angle_alpha 90.00 _cell_angle_beta 121.379(4) _cell_angle_gamma 90.00 _cell_volume 2404.8(17) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 3480 _cell_measurement_theta_min 2.1415 _cell_measurement_theta_max 27.5476 _exptl_crystal_description plate _exptl_crystal_colour 'yellowish white' _exptl_crystal_size_max 0.2800 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.0800 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.974 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 4.274 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8933 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; The data set was collected on Rigaku Saturn 724+ MicroMax 007 CCD diffractometer with equipment liquid nitrogen device, which could maintain the temperature at around 123 K ; _diffrn_ambient_temperature 123(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 Saturn724+ _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0 _diffrn_reflns_number 9194 _diffrn_reflns_av_R_equivalents 0.1118 _diffrn_reflns_av_sigmaI/netI 0.1315 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2747 _reflns_number_gt 1898 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _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^)+(0.1001P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2747 _refine_ls_number_parameters 168 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1807 _refine_ls_wR_factor_gt 0.1651 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 Cd1 Cd 0.0000 0.34222(7) 0.2500 0.0365(3) Uani 1 2 d S . . Br1 Br 0.04886(4) 0.52505(10) 0.16497(5) 0.0602(3) Uani 1 1 d D . . O1 O -0.1221(2) 0.2430(5) 0.1176(3) 0.0335(9) Uani 1 1 d . . . O1W O 0.029(3) 0.709(4) 0.012(2) 0.269(16) Uani 0.50 1 d PDU . . O2 O -0.0051(2) 0.1305(5) 0.1551(3) 0.0415(10) Uani 1 1 d . . . N1 N -0.1893(3) -0.0778(5) -0.1604(3) 0.0335(11) Uani 1 1 d . . . C1 C -0.0812(4) 0.1496(7) 0.1035(4) 0.0355(14) Uani 1 1 d . . . C2 C -0.1239(3) 0.0582(6) 0.0121(4) 0.0291(12) Uani 1 1 d . . . C3 C -0.0833(3) -0.0561(8) -0.0025(4) 0.0384(14) Uani 1 1 d . . . H3 H -0.0318 -0.0906 0.0479 0.046 Uiso 1 1 calc R . . C4 C -0.2032(3) 0.0944(7) -0.0596(4) 0.0294(12) Uani 1 1 d . . . H4 H -0.2349 0.1665 -0.0501 0.035 Uiso 1 1 calc R . . C5 C -0.1172(3) -0.1199(7) -0.0899(4) 0.0361(13) Uani 1 1 d . . . H5 H -0.0880 -0.1967 -0.0999 0.043 Uiso 1 1 calc R . . C6 C -0.2343(4) 0.0222(6) -0.1451(4) 0.0327(12) Uani 1 1 d . . . H6 H -0.2890 0.0433 -0.1945 0.039 Uiso 1 1 calc R . . C7 C -0.2221(5) -0.1360(7) -0.2582(4) 0.0413(15) Uani 1 1 d . . . H7A H -0.2760 -0.1843 -0.2807 0.050 Uiso 1 1 calc R . . H7B H -0.1843 -0.2137 -0.2567 0.050 Uiso 1 1 calc R . . C8 C -0.2325(4) -0.0127(7) -0.3280(4) 0.0335(13) Uani 1 1 d . . . C9 C -0.3021(4) -0.0026(7) -0.4137(4) 0.0339(13) Uani 1 1 d . . . H9 H -0.3470 -0.0662 -0.4273 0.041 Uiso 1 1 calc R . . C10 C -0.1671(4) 0.0865(7) -0.3058(4) 0.0378(13) Uani 1 1 d . . . H10 H -0.1180 0.0826 -0.2455 0.045 Uiso 1 1 calc R . . C11 C -0.3107(3) 0.0972(7) -0.4829(4) 0.0310(12) Uani 1 1 d . . . H11 H -0.3598 0.0976 -0.5432 0.037 Uiso 1 1 calc R . . C12 C -0.1752(4) 0.1901(7) -0.3730(4) 0.0348(13) Uani 1 1 d . . . H12 H -0.1314 0.2577 -0.3574 0.042 Uiso 1 1 calc R . . C13 C -0.2465(3) 0.1976(6) -0.4633(4) 0.0278(12) 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 Cd1 0.0209(3) 0.0646(5) 0.0219(3) 0.000 0.0096(3) 0.000 Br1 0.0401(5) 0.0944(7) 0.0440(5) 0.0021(4) 0.0205(4) -0.0140(3) O1 0.0243(18) 0.050(3) 0.0241(19) -0.0003(18) 0.0109(16) -0.0012(17) O1W 0.27(2) 0.30(2) 0.29(2) -0.004(17) 0.179(18) 0.017(17) O2 0.022(2) 0.069(3) 0.028(2) -0.0062(19) 0.0093(17) -0.0024(18) N1 0.041(3) 0.033(3) 0.034(3) -0.001(2) 0.025(2) -0.009(2) C1 0.028(3) 0.056(4) 0.025(3) 0.009(2) 0.016(2) -0.004(2) C2 0.027(3) 0.039(3) 0.026(3) 0.000(2) 0.017(2) -0.007(2) C3 0.020(3) 0.061(4) 0.035(3) 0.000(3) 0.015(2) -0.005(2) C4 0.031(3) 0.034(3) 0.027(3) 0.007(2) 0.017(2) -0.001(2) C5 0.027(3) 0.048(4) 0.039(3) -0.006(3) 0.020(3) -0.004(2) C6 0.032(3) 0.033(3) 0.029(3) 0.002(2) 0.013(3) -0.005(2) C7 0.054(4) 0.041(4) 0.030(3) -0.005(3) 0.023(3) -0.009(3) C8 0.042(3) 0.036(3) 0.030(3) -0.009(2) 0.024(3) -0.006(2) C9 0.035(3) 0.036(3) 0.036(3) -0.004(2) 0.022(3) -0.006(2) C10 0.041(3) 0.045(4) 0.031(3) -0.003(3) 0.021(3) -0.007(3) C11 0.033(3) 0.036(3) 0.028(3) -0.004(2) 0.018(2) 0.000(2) C12 0.042(3) 0.039(3) 0.032(3) -0.011(2) 0.024(3) -0.010(3) C13 0.029(3) 0.034(3) 0.028(3) -0.008(2) 0.019(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.387(4) . ? Cd1 O1 2.387(4) 2 ? Cd1 O2 2.426(4) . ? Cd1 O2 2.426(4) 2 ? Cd1 Br1 2.6226(10) . ? Cd1 Br1 2.6226(10) 2 ? Cd1 C1 2.708(6) . ? Cd1 C1 2.707(6) 2 ? O1 C1 1.243(7) . ? O2 C1 1.254(7) . ? N1 C5 1.312(8) . ? N1 C6 1.351(7) . ? N1 C7 1.496(8) . ? C1 C2 1.529(8) . ? C2 C3 1.375(8) . ? C2 C4 1.390(8) . ? C3 C5 1.366(8) . ? C3 H3 0.9500 . ? C4 C6 1.378(8) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.533(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.351(8) . ? C8 C10 1.411(8) . ? C9 C11 1.392(8) . ? C9 H9 0.9500 . ? C10 C12 1.393(9) . ? C10 H10 0.9500 . ? C11 C13 1.411(8) . ? C11 H11 0.9500 . ? C12 C13 1.405(8) . ? C12 H12 0.9500 . ? C13 C13 1.485(11) 7_454 ? 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 O1 Cd1 O1 136.5(2) . 2 ? O1 Cd1 O2 54.86(14) . . ? O1 Cd1 O2 89.98(14) 2 . ? O1 Cd1 O2 89.98(14) . 2 ? O1 Cd1 O2 54.86(14) 2 2 ? O2 Cd1 O2 77.9(2) . 2 ? O1 Cd1 Br1 100.63(10) . . ? O1 Cd1 Br1 106.00(10) 2 . ? O2 Cd1 Br1 92.27(11) . . ? O2 Cd1 Br1 157.86(10) 2 . ? O1 Cd1 Br1 106.00(10) . 2 ? O1 Cd1 Br1 100.63(10) 2 2 ? O2 Cd1 Br1 157.86(10) . 2 ? O2 Cd1 Br1 92.27(11) 2 2 ? Br1 Cd1 Br1 103.21(5) . 2 ? O1 Cd1 C1 27.32(15) . . ? O1 Cd1 C1 114.77(16) 2 . ? O2 Cd1 C1 27.58(16) . . ? O2 Cd1 C1 84.30(15) 2 . ? Br1 Cd1 C1 96.20(11) . . ? Br1 Cd1 C1 132.79(13) 2 . ? O1 Cd1 C1 114.77(16) . 2 ? O1 Cd1 C1 27.32(15) 2 2 ? O2 Cd1 C1 84.30(15) . 2 ? O2 Cd1 C1 27.58(16) 2 2 ? Br1 Cd1 C1 132.79(13) . 2 ? Br1 Cd1 C1 96.20(11) 2 2 ? C1 Cd1 C1 101.3(2) . 2 ? C1 O1 Cd1 90.8(3) . . ? C1 O2 Cd1 88.8(4) . . ? C5 N1 C6 119.6(5) . . ? C5 N1 C7 121.3(5) . . ? C6 N1 C7 119.0(5) . . ? O1 C1 O2 125.3(6) . . ? O1 C1 C2 118.8(5) . . ? O2 C1 C2 115.7(5) . . ? O1 C1 Cd1 61.8(3) . . ? O2 C1 Cd1 63.6(3) . . ? C2 C1 Cd1 171.0(4) . . ? C3 C2 C4 118.8(5) . . ? C3 C2 C1 120.8(5) . . ? C4 C2 C1 120.3(5) . . ? C5 C3 C2 119.8(6) . . ? C5 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C6 C4 C2 117.8(5) . . ? C6 C4 H4 121.1 . . ? C2 C4 H4 121.1 . . ? N1 C5 C3 121.6(6) . . ? N1 C5 H5 119.2 . . ? C3 C5 H5 119.2 . . ? N1 C6 C4 121.7(5) . . ? N1 C6 H6 119.1 . . ? C4 C6 H6 119.1 . . ? N1 C7 C8 112.8(5) . . ? N1 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? N1 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C9 C8 C10 118.9(6) . . ? C9 C8 C7 120.8(5) . . ? C10 C8 C7 120.2(6) . . ? C8 C9 C11 122.7(5) . . ? C8 C9 H9 118.7 . . ? C11 C9 H9 118.7 . . ? C12 C10 C8 119.4(6) . . ? C12 C10 H10 120.3 . . ? C8 C10 H10 120.3 . . ? C9 C11 C13 119.9(5) . . ? C9 C11 H11 120.0 . . ? C13 C11 H11 120.0 . . ? C10 C12 C13 121.8(5) . . ? C10 C12 H12 119.1 . . ? C13 C12 H12 119.1 . . ? C12 C13 C11 117.2(5) . . ? C12 C13 C13 121.9(6) . 7_454 ? C11 C13 C13 120.9(6) . 7_454 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.603 _refine_diff_density_min -1.509 _refine_diff_density_rms 0.165 data_2 _database_code_depnum_ccdc_archive 'CCDC 875820' #TrackingRef '- 2-SJK-R.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H28 Br2 Cd N2 O8' _chemical_formula_sum 'C26 H28 Br2 Cd N2 O8' _chemical_formula_weight 768.72 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' Cd Cd -0.8075 1.2024 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.368(2) _cell_length_b 9.5792(11) _cell_length_c 19.184(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.300(7) _cell_angle_gamma 90.00 _cell_volume 2762.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2630 _cell_measurement_theta_min 2.0999 _cell_measurement_theta_max 27.4333 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 3.735 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4917 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _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 'Rigaku SCXmini' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0 _diffrn_reflns_number 21087 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6325 _reflns_number_gt 5089 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _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^)+(0.0600P)^2^+1.5000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6325 _refine_ls_number_parameters 371 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1217 _refine_ls_wR_factor_gt 0.1116 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.006 _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 Cd1 Cd 0.308946(16) 0.27439(3) 0.531080(16) 0.03676(11) Uani 1 1 d . . . Br1 Br 0.23244(3) 0.10478(5) 0.59600(3) 0.05339(14) Uani 1 1 d . . . Br2 Br 0.38786(3) 0.10953(5) 0.46940(2) 0.04474(13) Uani 1 1 d . . . O1 O 0.19981(18) 0.4447(4) 0.4923(2) 0.0583(9) Uani 1 1 d . . . O2 O 0.1663(2) 0.2712(4) 0.4105(2) 0.0655(10) Uani 1 1 d . . . O3 O -1.0709(2) 0.1730(4) 0.14886(19) 0.0564(8) Uani 1 1 d . . . O4 O -1.07985(18) 0.0410(3) 0.05261(17) 0.0504(8) Uani 1 1 d . . . N1 N -0.28447(18) 0.4830(3) 0.28868(18) 0.0338(7) Uani 1 1 d . . . N2 N -0.60987(18) 0.0051(3) 0.28756(17) 0.0314(6) Uani 1 1 d . . . C1 C 0.1456(3) 0.3808(5) 0.4352(3) 0.0439(10) Uani 1 1 d . . . C2 C 0.0524(2) 0.4370(4) 0.3958(2) 0.0377(8) Uani 1 1 d . . . C3 C 0.0244(2) 0.5519(4) 0.4253(2) 0.0409(9) Uani 1 1 d . . . H3 H 0.0641 0.5972 0.4682 0.049 Uiso 1 1 calc R . . C4 C -0.0072(2) 0.3731(4) 0.3307(2) 0.0423(9) Uani 1 1 d . . . H4 H 0.0114 0.2971 0.3105 0.051 Uiso 1 1 calc R . . C5 C -0.0629(2) 0.5987(4) 0.3905(2) 0.0386(9) Uani 1 1 d . . . H5 H -0.0817 0.6744 0.4106 0.046 Uiso 1 1 calc R . . C6 C -0.0933(3) 0.4201(4) 0.2955(2) 0.0419(9) Uani 1 1 d . . . H6 H -0.1323 0.3767 0.2516 0.050 Uiso 1 1 calc R . . C7 C -0.1219(2) 0.5330(4) 0.3260(2) 0.0333(8) Uani 1 1 d . . . C8 C -0.2166(2) 0.5866(4) 0.2866(3) 0.0417(9) Uani 1 1 d . . . H8A H -0.2228 0.6723 0.3110 0.050 Uiso 1 1 calc R . . H8B H -0.2280 0.6082 0.2342 0.050 Uiso 1 1 calc R . . C9 C -0.2701(3) 0.4049(5) 0.3497(2) 0.0438(10) Uani 1 1 d . . . H9 H -0.2169 0.4144 0.3919 0.053 Uiso 1 1 calc R . . C10 C -0.3621(2) 0.4750(4) 0.2276(2) 0.0378(8) Uani 1 1 d . . . H10 H -0.3720 0.5319 0.1858 0.045 Uiso 1 1 calc R . . C11 C -0.3323(2) 0.3105(5) 0.3517(2) 0.0431(9) Uani 1 1 d . . . H11 H -0.3207 0.2560 0.3947 0.052 Uiso 1 1 calc R . . C12 C -0.4264(2) 0.3835(4) 0.2271(2) 0.0379(9) Uani 1 1 d . . . H12 H -0.4800 0.3791 0.1849 0.045 Uiso 1 1 calc R . . C13 C -0.4129(2) 0.2967(4) 0.2889(2) 0.0328(8) Uani 1 1 d . . . C14 C -0.4817(2) 0.1940(4) 0.2888(2) 0.0327(8) Uani 1 1 d . . . C15 C -0.4617(2) 0.0882(4) 0.3425(2) 0.0413(9) Uani 1 1 d . . . H15 H -0.4041 0.0794 0.3793 0.050 Uiso 1 1 calc R . . C16 C -0.5678(2) 0.2001(4) 0.2333(2) 0.0361(8) Uani 1 1 d . . . H16 H -0.5831 0.2675 0.1953 0.043 Uiso 1 1 calc R . . C17 C -0.5268(2) -0.0034(4) 0.3415(2) 0.0387(9) Uani 1 1 d . . . H17 H -0.5133 -0.0722 0.3785 0.046 Uiso 1 1 calc R . . C18 C -0.6301(2) 0.1052(4) 0.2350(2) 0.0380(9) Uani 1 1 d . . . H18 H -0.6880 0.1110 0.1986 0.046 Uiso 1 1 calc R . . C19 C -0.6764(2) -0.1014(4) 0.2895(3) 0.0405(9) Uani 1 1 d . . . H19A H -0.6659 -0.1883 0.2685 0.049 Uiso 1 1 calc R . . H19B H -0.6672 -0.1185 0.3419 0.049 Uiso 1 1 calc R . . C20 C -0.7712(2) -0.0580(4) 0.2462(2) 0.0342(8) Uani 1 1 d . . . C21 C -0.8158(2) -0.0957(4) 0.1708(2) 0.0402(9) Uani 1 1 d . . . H21 H -0.7875 -0.1515 0.1475 0.048 Uiso 1 1 calc R . . C22 C -0.8156(2) 0.0200(4) 0.2816(2) 0.0363(8) Uani 1 1 d . . . H22 H -0.7869 0.0435 0.3326 0.044 Uiso 1 1 calc R . . C23 C -0.9027(2) -0.0508(4) 0.1296(2) 0.0403(9) Uani 1 1 d . . . H23 H -0.9316 -0.0744 0.0787 0.048 Uiso 1 1 calc R . . C24 C -0.9026(2) 0.0626(4) 0.2407(2) 0.0362(8) Uani 1 1 d . . . H24 H -0.9320 0.1143 0.2648 0.043 Uiso 1 1 calc R . . C25 C -0.9462(2) 0.0292(4) 0.1649(2) 0.0329(8) Uani 1 1 d . . . C26 C -1.0388(2) 0.0847(4) 0.1194(2) 0.0406(9) Uani 1 1 d . . . O1W O -0.0936(9) 0.1821(11) 0.4282(6) 0.128(5) Uani 0.690(19) 1 d PU . . O2W O -0.4064(3) 0.2704(4) 0.5123(3) 0.1067(19) Uani 1 1 d . . . H2A H -0.4547 0.2327 0.5023 0.160 Uiso 1 1 d R . . H2B H -0.4055 0.3479 0.4944 0.160 Uiso 1 1 d R . . O3W O -0.2276(3) 0.2802(5) 0.5587(3) 0.1058(17) Uani 1 1 d . . . H3A H -0.2743 0.2930 0.5641 0.159 Uiso 1 1 d R . . H3B H -0.2296 0.2140 0.5310 0.159 Uiso 1 1 d R . . O4W O -0.1087(6) 0.0760(12) 0.5715(5) 0.094(3) Uani 0.690(19) 1 d PU . . O1WB O -0.026(2) 0.116(3) 0.4538(14) 0.137(10) Uani 0.310(19) 1 d PU . . O4WB O -0.089(2) 0.002(4) 0.5792(16) 0.138(10) Uani 0.310(19) 1 d PU . . 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 Cd1 0.02675(16) 0.04233(18) 0.03786(18) -0.00332(12) 0.00921(12) 0.00078(10) Br1 0.0463(3) 0.0651(3) 0.0504(3) 0.0000(2) 0.0209(2) -0.0120(2) Br2 0.0417(2) 0.0489(3) 0.0406(2) -0.00136(18) 0.01312(17) 0.01270(17) O1 0.0285(14) 0.065(2) 0.064(2) 0.0010(18) -0.0005(13) 0.0025(14) O2 0.0430(18) 0.085(3) 0.062(2) -0.0033(19) 0.0135(15) 0.0242(17) O3 0.0484(18) 0.063(2) 0.055(2) 0.0068(17) 0.0180(14) 0.0237(16) O4 0.0343(14) 0.0586(19) 0.0470(18) 0.0072(15) 0.0039(12) 0.0045(13) N1 0.0246(14) 0.0403(16) 0.0361(17) -0.0007(14) 0.0117(12) 0.0007(12) N2 0.0238(14) 0.0347(15) 0.0325(16) 0.0009(13) 0.0077(11) 0.0039(12) C1 0.0299(19) 0.057(3) 0.046(2) 0.012(2) 0.0160(17) 0.0075(18) C2 0.0251(17) 0.049(2) 0.038(2) 0.0063(18) 0.0112(14) 0.0018(16) C3 0.0307(18) 0.048(2) 0.040(2) -0.0018(18) 0.0094(15) -0.0019(16) C4 0.036(2) 0.046(2) 0.045(2) -0.0036(18) 0.0158(17) 0.0078(17) C5 0.0342(19) 0.039(2) 0.044(2) -0.0050(17) 0.0160(16) -0.0016(15) C6 0.0324(19) 0.047(2) 0.041(2) -0.0087(18) 0.0090(16) -0.0025(17) C7 0.0222(16) 0.040(2) 0.0348(19) 0.0027(16) 0.0076(13) -0.0002(14) C8 0.0284(18) 0.037(2) 0.058(3) 0.0062(19) 0.0148(17) -0.0013(15) C9 0.0302(19) 0.062(3) 0.033(2) -0.0001(19) 0.0062(15) -0.0061(17) C10 0.0275(17) 0.044(2) 0.038(2) 0.0036(17) 0.0085(14) 0.0060(16) C11 0.0320(19) 0.061(3) 0.033(2) 0.0044(19) 0.0086(15) -0.0040(18) C12 0.0215(17) 0.049(2) 0.037(2) 0.0017(17) 0.0048(14) 0.0045(15) C13 0.0237(16) 0.041(2) 0.0331(19) -0.0024(15) 0.0111(13) 0.0032(14) C14 0.0244(17) 0.0379(19) 0.0336(19) -0.0041(16) 0.0092(14) 0.0044(14) C15 0.0240(17) 0.054(2) 0.039(2) 0.0070(19) 0.0050(15) 0.0045(16) C16 0.0260(17) 0.0372(19) 0.039(2) 0.0016(16) 0.0067(15) 0.0012(14) C17 0.0284(18) 0.045(2) 0.037(2) 0.0118(18) 0.0077(15) 0.0058(16) C18 0.0249(17) 0.040(2) 0.041(2) 0.0032(16) 0.0044(15) 0.0041(14) C19 0.0332(19) 0.0298(19) 0.051(3) 0.0032(16) 0.0093(17) -0.0002(14) C20 0.0285(17) 0.0296(17) 0.042(2) 0.0011(16) 0.0118(15) -0.0042(14) C21 0.034(2) 0.047(2) 0.042(2) -0.0048(18) 0.0167(16) 0.0022(16) C22 0.0348(18) 0.0358(19) 0.034(2) -0.0052(16) 0.0097(14) -0.0054(15) C23 0.0332(19) 0.051(2) 0.033(2) -0.0028(18) 0.0093(15) -0.0021(17) C24 0.0350(19) 0.0322(18) 0.043(2) -0.0006(17) 0.0168(16) 0.0001(15) C25 0.0279(17) 0.0287(17) 0.042(2) 0.0026(15) 0.0135(14) -0.0021(13) C26 0.0301(19) 0.044(2) 0.045(2) 0.0135(19) 0.0117(16) 0.0024(16) O1W 0.172(9) 0.107(6) 0.115(6) -0.007(5) 0.068(6) -0.045(6) O2W 0.065(3) 0.058(2) 0.175(6) 0.003(3) 0.024(3) -0.003(2) O3W 0.080(3) 0.113(4) 0.104(4) 0.006(3) 0.016(3) -0.025(3) O4W 0.080(4) 0.109(6) 0.080(5) -0.039(4) 0.019(3) -0.023(4) O1WB 0.140(13) 0.138(13) 0.134(12) 0.004(8) 0.054(9) -0.020(9) O4WB 0.142(12) 0.139(13) 0.123(12) 0.001(9) 0.041(8) -0.044(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.314(3) . ? Cd1 O3 2.390(3) 4_766 ? Cd1 O4 2.453(3) 4_766 ? Cd1 O2 2.556(3) . ? Cd1 Br2 2.6022(5) . ? Cd1 Br1 2.6443(6) . ? Cd1 C26 2.751(4) 4_766 ? O1 C1 1.262(6) . ? O2 C1 1.253(5) . ? O3 C26 1.244(5) . ? O3 Cd1 2.390(3) 4_465 ? O4 C26 1.260(5) . ? O4 Cd1 2.453(3) 4_465 ? N1 C9 1.330(5) . ? N1 C10 1.347(4) . ? N1 C8 1.501(5) . ? N2 C18 1.334(5) . ? N2 C17 1.347(4) . ? N2 C19 1.503(5) . ? C1 C2 1.509(5) . ? C2 C4 1.386(6) . ? C2 C3 1.395(6) . ? C3 C5 1.391(5) . ? C3 H3 0.9300 . ? C4 C6 1.376(5) . ? C4 H4 0.9300 . ? C5 C7 1.383(5) . ? C5 H5 0.9300 . ? C6 C7 1.396(5) . ? C6 H6 0.9300 . ? C7 C8 1.520(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C11 1.373(6) . ? C9 H9 0.9300 . ? C10 C12 1.367(5) . ? C10 H10 0.9300 . ? C11 C13 1.398(5) . ? C11 H11 0.9300 . ? C12 C13 1.392(5) . ? C12 H12 0.9300 . ? C13 C14 1.493(5) . ? C14 C15 1.390(6) . ? C14 C16 1.392(5) . ? C15 C17 1.374(6) . ? C15 H15 0.9300 . ? C16 C18 1.377(5) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.500(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.385(6) . ? C20 C22 1.392(5) . ? C21 C23 1.395(5) . ? C21 H21 0.9300 . ? C22 C24 1.389(5) . ? C22 H22 0.9300 . ? C23 C25 1.390(5) . ? C23 H23 0.9300 . ? C24 C25 1.381(5) . ? C24 H24 0.9300 . ? C25 C26 1.514(5) . ? C26 Cd1 2.751(4) 4_465 ? O1W O1WB 1.20(3) . ? O2W H2A 0.8203 . ? O2W H2B 0.8199 . ? O3W H3A 0.8200 . ? O3W H3B 0.8201 . ? O4W O4WB 0.76(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O3 113.40(12) . 4_766 ? O1 Cd1 O4 88.45(11) . 4_766 ? O3 Cd1 O4 53.87(11) 4_766 4_766 ? O1 Cd1 O2 53.48(11) . . ? O3 Cd1 O2 166.87(12) 4_766 . ? O4 Cd1 O2 120.84(12) 4_766 . ? O1 Cd1 Br2 137.79(9) . . ? O3 Cd1 Br2 100.78(9) 4_766 . ? O4 Cd1 Br2 92.60(8) 4_766 . ? O2 Cd1 Br2 91.22(8) . . ? O1 Cd1 Br1 97.77(9) . . ? O3 Cd1 Br1 92.88(8) 4_766 . ? O4 Cd1 Br1 145.26(8) 4_766 . ? O2 Cd1 Br1 89.17(9) . . ? Br2 Cd1 Br1 104.72(2) . . ? O1 Cd1 C26 104.37(12) . 4_766 ? O3 Cd1 C26 26.84(12) 4_766 4_766 ? O4 Cd1 C26 27.26(12) 4_766 4_766 ? O2 Cd1 C26 147.61(13) . 4_766 ? Br2 Cd1 C26 94.95(8) . 4_766 ? Br1 Cd1 C26 119.60(10) . 4_766 ? C1 O1 Cd1 97.2(3) . . ? C1 O2 Cd1 86.2(3) . . ? C26 O3 Cd1 93.0(3) . 4_465 ? C26 O4 Cd1 89.6(2) . 4_465 ? C9 N1 C10 120.7(3) . . ? C9 N1 C8 121.4(3) . . ? C10 N1 C8 117.9(3) . . ? C18 N2 C17 119.8(3) . . ? C18 N2 C19 122.7(3) . . ? C17 N2 C19 117.5(3) . . ? O2 C1 O1 122.2(4) . . ? O2 C1 C2 118.7(4) . . ? O1 C1 C2 119.1(4) . . ? C4 C2 C3 119.1(3) . . ? C4 C2 C1 120.4(4) . . ? C3 C2 C1 120.5(4) . . ? C5 C3 C2 120.0(4) . . ? C5 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C6 C4 C2 121.2(4) . . ? C6 C4 H4 119.4 . . ? C2 C4 H4 119.4 . . ? C7 C5 C3 120.3(4) . . ? C7 C5 H5 119.9 . . ? C3 C5 H5 119.9 . . ? C4 C6 C7 119.7(4) . . ? C4 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C5 C7 C6 119.7(3) . . ? C5 C7 C8 120.3(4) . . ? C6 C7 C8 119.9(3) . . ? N1 C8 C7 112.5(3) . . ? N1 C8 H8A 109.1 . . ? C7 C8 H8A 109.1 . . ? N1 C8 H8B 109.1 . . ? C7 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? N1 C9 C11 121.4(4) . . ? N1 C9 H9 119.3 . . ? C11 C9 H9 119.3 . . ? N1 C10 C12 120.1(4) . . ? N1 C10 H10 119.9 . . ? C12 C10 H10 119.9 . . ? C9 C11 C13 119.7(4) . . ? C9 C11 H11 120.1 . . ? C13 C11 H11 120.1 . . ? C10 C12 C13 121.0(3) . . ? C10 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C12 C13 C11 117.0(3) . . ? C12 C13 C14 121.8(3) . . ? C11 C13 C14 121.2(4) . . ? C15 C14 C16 117.9(3) . . ? C15 C14 C13 121.5(3) . . ? C16 C14 C13 120.5(4) . . ? C17 C15 C14 120.0(3) . . ? C17 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C18 C16 C14 119.3(4) . . ? C18 C16 H16 120.3 . . ? C14 C16 H16 120.3 . . ? N2 C17 C15 121.0(4) . . ? N2 C17 H17 119.5 . . ? C15 C17 H17 119.5 . . ? N2 C18 C16 121.8(3) . . ? N2 C18 H18 119.1 . . ? C16 C18 H18 119.1 . . ? C20 C19 N2 113.6(3) . . ? C20 C19 H19A 108.9 . . ? N2 C19 H19A 108.9 . . ? C20 C19 H19B 108.9 . . ? N2 C19 H19B 108.9 . . ? H19A C19 H19B 107.7 . . ? C21 C20 C22 119.2(3) . . ? C21 C20 C19 120.5(4) . . ? C22 C20 C19 120.2(4) . . ? C20 C21 C23 120.6(4) . . ? C20 C21 H21 119.7 . . ? C23 C21 H21 119.7 . . ? C24 C22 C20 119.9(4) . . ? C24 C22 H22 120.0 . . ? C20 C22 H22 120.0 . . ? C25 C23 C21 119.9(4) . . ? C25 C23 H23 120.1 . . ? C21 C23 H23 120.1 . . ? C25 C24 C22 121.0(4) . . ? C25 C24 H24 119.5 . . ? C22 C24 H24 119.5 . . ? C24 C25 C23 119.3(3) . . ? C24 C25 C26 120.6(4) . . ? C23 C25 C26 120.1(4) . . ? O3 C26 O4 122.5(4) . . ? O3 C26 C25 118.9(4) . . ? O4 C26 C25 118.6(4) . . ? O3 C26 Cd1 60.2(2) . 4_465 ? O4 C26 Cd1 63.1(2) . 4_465 ? C25 C26 Cd1 169.6(3) . 4_465 ? H2A O2W H2B 118.4 . . ? H3A O3W H3B 113.3 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.788 _refine_diff_density_min -1.000 _refine_diff_density_rms 0.111