# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Bin Zhang' _publ_contact_author_email zhangbin@iccas.ac.cn _publ_section_title ; Solvent-Mediated Crystal-to-Crystal Transformation within CoBr2(1,4-dioxane)m(H2O)n Family (m = 2, 3; n = 0, 2, 4) from 2D to 1D, and 0D ; loop_ _publ_author_name 'Bin Zhang' 'Zhiming Duan' 'Yan Zhang' 'Daoben Zhu' # Attachment '- CCDC820394.cif' data_802394 _database_code_depnum_ccdc_archive 'CCDC 802394' #TrackingRef '- CCDC820394.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H16 Br2 Co O4' _chemical_formula_weight 394.96 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 4(1)/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 10.0681(3) _cell_length_b 10.0681(3) _cell_length_c 23.3960(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2371.57(14) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 5810 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 8.178 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.259 _exptl_absorpt_correction_T_max 0.718 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method CCD _diffrn_reflns_number 24605 _diffrn_reflns_av_R_equivalents 0.1424 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 4.05 _diffrn_reflns_theta_max 27.47 _reflns_number_total 1354 _reflns_number_gt 723 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0684P)^2^+1.9481P] 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 SHELXL _refine_ls_extinction_coef 0.0015(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1354 _refine_ls_number_parameters 71 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1328 _refine_ls_wR_factor_gt 0.1179 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 Co1 Co 0.0000 0.7500 0.11674(4) 0.0160(3) Uani 1 2 d S . . Br1 Br 0.0000 0.7500 0.22620(4) 0.0257(3) Uani 1 2 d S . . Br2 Br 0.0000 0.7500 0.00807(3) 0.0207(3) Uani 1 2 d S . . O1 O -0.1581(4) 0.6047(4) 0.1188(4) 0.0244(13) Uani 1 1 d . . . O2 O -0.3457(4) 0.3977(4) 0.1330(3) 0.0205(14) Uani 1 1 d . . . C1 C -0.2788(7) 0.6229(7) 0.1519(3) 0.0323(18) Uani 1 1 d . . . H1A H -0.3491 0.6561 0.1274 0.039 Uiso 1 1 calc R . . H1B H -0.2636 0.6872 0.1820 0.039 Uiso 1 1 calc R . . C2 C -0.3196(8) 0.4909(7) 0.1776(3) 0.0341(19) Uani 1 1 d . . . H2A H -0.2491 0.4577 0.2020 0.041 Uiso 1 1 calc R . . H2B H -0.3985 0.5026 0.2008 0.041 Uiso 1 1 calc R . . C3 C -0.2235(7) 0.3770(7) 0.1006(3) 0.0302(18) Uani 1 1 d . . . H3A H -0.2381 0.3119 0.0707 0.036 Uiso 1 1 calc R . . H3B H -0.1540 0.3443 0.1257 0.036 Uiso 1 1 calc R . . C4 C -0.1825(8) 0.5084(7) 0.0747(3) 0.0344(19) Uani 1 1 d . . . H4A H -0.1028 0.4963 0.0520 0.041 Uiso 1 1 calc R . . H4B H -0.2523 0.5404 0.0496 0.041 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 Co1 0.0137(6) 0.0136(5) 0.0205(6) 0.000 0.000 0.0004(4) Br1 0.0272(7) 0.0270(7) 0.0230(5) 0.000 0.000 0.0007(6) Br2 0.0207(6) 0.0195(6) 0.0218(5) 0.000 0.000 0.0020(5) O1 0.021(2) 0.024(2) 0.028(4) -0.003(3) 0.010(3) -0.0068(17) O2 0.018(2) 0.021(2) 0.023(4) -0.003(2) 0.003(2) -0.0063(16) C1 0.027(4) 0.027(4) 0.043(5) -0.003(3) 0.002(3) 0.000(3) C2 0.048(5) 0.039(5) 0.015(4) 0.000(3) 0.005(3) -0.022(4) C3 0.027(4) 0.028(4) 0.035(4) -0.010(3) 0.010(3) -0.002(3) C4 0.030(5) 0.033(4) 0.040(5) -0.004(3) 0.008(3) -0.009(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 Co1 O2 2.151(4) 12_676 ? Co1 O2 2.151(4) 15 ? Co1 O1 2.162(4) 6_464 ? Co1 O1 2.162(4) . ? Co1 Br2 2.5425(12) . ? Co1 Br1 2.5608(13) . ? O1 C4 1.437(10) . ? O1 C1 1.453(9) . ? O2 C2 1.428(9) . ? O2 C3 1.459(8) . ? O2 Co1 2.151(4) 15_455 ? C1 C2 1.515(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.513(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? 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 O2 Co1 O2 179.7(4) 12_676 15 ? O2 Co1 O1 91.14(16) 12_676 6_464 ? O2 Co1 O1 88.85(16) 15 6_464 ? O2 Co1 O1 88.85(16) 12_676 . ? O2 Co1 O1 91.14(16) 15 . ? O1 Co1 O1 177.5(5) 6_464 . ? O2 Co1 Br2 90.2(2) 12_676 . ? O2 Co1 Br2 90.2(2) 15 . ? O1 Co1 Br2 91.3(2) 6_464 . ? O1 Co1 Br2 91.3(2) . . ? O2 Co1 Br1 89.8(2) 12_676 . ? O2 Co1 Br1 89.8(2) 15 . ? O1 Co1 Br1 88.7(2) 6_464 . ? O1 Co1 Br1 88.7(2) . . ? Br2 Co1 Br1 180.0 . . ? C4 O1 C1 108.9(5) . . ? C4 O1 Co1 124.5(5) . . ? C1 O1 Co1 122.9(4) . . ? C2 O2 C3 108.5(5) . . ? C2 O2 Co1 125.8(5) . 15_455 ? C3 O2 Co1 120.8(4) . 15_455 ? O1 C1 C2 109.1(5) . . ? O1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? O1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? O2 C2 C1 109.6(6) . . ? O2 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? O2 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? O2 C3 C4 108.3(5) . . ? O2 C3 H3A 110.0 . . ? C4 C3 H3A 110.0 . . ? O2 C3 H3B 110.0 . . ? C4 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? O1 C4 C3 110.4(6) . . ? O1 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? O1 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C4 H4A Br2 0.97 3.03 3.728(7) 129.7 9_565 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.694 _refine_diff_density_min -0.779 _refine_diff_density_rms 0.172 # Attachment '- CCDC802395.cif' data_802395 _database_code_depnum_ccdc_archive 'CCDC 802395' #TrackingRef '- CCDC802395.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H20 Br2 Co O6' _chemical_formula_weight 430.99 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' O O 0.0106 0.0060 '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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.8213(15) _cell_length_b 6.9778(18) _cell_length_c 10.275(3) _cell_angle_alpha 99.636(3) _cell_angle_beta 101.641(3) _cell_angle_gamma 112.746(2) _cell_volume 362.80(16) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1615 _cell_measurement_theta_min 3.2896 _cell_measurement_theta_max 30.9874 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.973 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 213 _exptl_absorpt_coefficient_mu 6.700 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.2055 _exptl_absorpt_correction_T_max 0.3237 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device ; Saturn724+ (2x2 bin mode) ; _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 5941 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 30.99 _reflns_number_total 2283 _reflns_number_gt 2206 _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 _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0149P)^2^+0.3731P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0141(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2283 _refine_ls_number_parameters 86 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0298 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0609 _refine_ls_wR_factor_gt 0.0602 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _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 Co1 Co 0.0000 0.0000 0.0000 0.01389(10) Uani 1 2 d S . . Br1 Br -0.10000(4) 0.17890(3) 0.20829(2) 0.01842(8) Uani 1 1 d . . . O1 O 0.3052(3) 0.3010(2) 0.00232(16) 0.0186(3) Uani 1 1 d . . . O2 O -0.2596(4) 0.0650(3) -0.40012(18) 0.0294(4) Uani 1 1 d . . . O3 O 0.2664(3) -0.0563(3) 0.13366(18) 0.0202(3) Uani 1 1 d . . . H1 H 0.419(7) -0.006(5) 0.137(3) 0.030 Uiso 1 1 d . . . H2 H 0.266(7) -0.050(5) 0.208(3) 0.030 Uiso 1 1 d . . . C1 C 0.2772(4) 0.3909(4) -0.1134(2) 0.0194(4) Uani 1 1 d . . . H1A H 0.1835 0.4812 -0.1001 0.023 Uiso 1 1 calc R . . H1B H 0.1730 0.2726 -0.1993 0.023 Uiso 1 1 calc R . . C2 C 0.4596(4) 0.4741(4) 0.1268(2) 0.0193(4) Uani 1 1 d . . . H2A H 0.4814 0.4133 0.2064 0.023 Uiso 1 1 calc R . . H2B H 0.3688 0.5658 0.1439 0.023 Uiso 1 1 calc R . . C3 C -0.3733(6) -0.1333(5) -0.5062(3) 0.0322(6) Uani 1 1 d . . . H3A H -0.3240 -0.2403 -0.4715 0.039 Uiso 1 1 calc R . . H3B H -0.3064 -0.1094 -0.5862 0.039 Uiso 1 1 calc R . . C4 C -0.3344(6) 0.2197(4) -0.4489(3) 0.0301(5) Uani 1 1 d . . . H4A H -0.2666 0.2511 -0.5277 0.036 Uiso 1 1 calc R . . H4B H -0.2578 0.3560 -0.3744 0.036 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 Co1 0.01142(18) 0.01278(18) 0.0161(2) 0.00522(15) 0.00422(14) 0.00326(14) Br1 0.01650(11) 0.01834(12) 0.02024(13) 0.00477(8) 0.00701(8) 0.00680(8) O1 0.0180(7) 0.0146(7) 0.0168(7) 0.0057(6) 0.0038(6) 0.0006(6) O2 0.0290(9) 0.0344(10) 0.0198(9) 0.0047(8) 0.0013(7) 0.0126(8) O3 0.0141(7) 0.0272(8) 0.0193(8) 0.0098(7) 0.0050(6) 0.0076(6) C1 0.0164(9) 0.0176(10) 0.0194(10) 0.0086(8) 0.0025(8) 0.0025(8) C2 0.0182(10) 0.0168(10) 0.0170(10) 0.0045(8) 0.0051(8) 0.0015(8) C3 0.0384(15) 0.0353(14) 0.0240(13) 0.0048(11) 0.0058(11) 0.0203(12) C4 0.0355(14) 0.0255(12) 0.0207(12) 0.0043(10) 0.0062(10) 0.0062(11) _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 Co1 O3 2.0587(17) 2 ? Co1 O3 2.0587(17) . ? Co1 O1 2.1564(15) . ? Co1 O1 2.1564(15) 2 ? Co1 Br1 2.5783(5) . ? Co1 Br1 2.5783(5) 2 ? O1 C2 1.443(3) . ? O1 C1 1.444(3) . ? O2 C3 1.427(3) . ? O2 C4 1.436(3) . ? O3 H1 0.81(4) . ? O3 H2 0.75(3) . ? C1 C2 1.506(3) 2_665 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C1 1.506(3) 2_665 ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.506(4) 2_454 ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C3 1.506(4) 2_454 ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? 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 O3 Co1 O3 180.00(10) 2 . ? O3 Co1 O1 89.90(7) 2 . ? O3 Co1 O1 90.10(7) . . ? O3 Co1 O1 90.10(7) 2 2 ? O3 Co1 O1 89.90(7) . 2 ? O1 Co1 O1 180.00(9) . 2 ? O3 Co1 Br1 90.58(5) 2 . ? O3 Co1 Br1 89.42(5) . . ? O1 Co1 Br1 92.77(5) . . ? O1 Co1 Br1 87.23(5) 2 . ? O3 Co1 Br1 89.42(5) 2 2 ? O3 Co1 Br1 90.58(5) . 2 ? O1 Co1 Br1 87.23(5) . 2 ? O1 Co1 Br1 92.77(5) 2 2 ? Br1 Co1 Br1 180.000(9) . 2 ? C2 O1 C1 109.29(16) . . ? C2 O1 Co1 122.83(12) . . ? C1 O1 Co1 119.71(12) . . ? C3 O2 C4 109.91(19) . . ? Co1 O3 H1 122(2) . . ? Co1 O3 H2 121(3) . . ? H1 O3 H2 104(3) . . ? O1 C1 C2 110.37(18) . 2_665 ? O1 C1 H1A 109.6 . . ? C2 C1 H1A 109.6 2_665 . ? O1 C1 H1B 109.6 . . ? C2 C1 H1B 109.6 2_665 . ? H1A C1 H1B 108.1 . . ? O1 C2 C1 110.23(18) . 2_665 ? O1 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 2_665 . ? O1 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 2_665 . ? H2A C2 H2B 108.1 . . ? O2 C3 C4 110.3(2) . 2_454 ? O2 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 2_454 . ? O2 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 2_454 . ? H3A C3 H3B 108.1 . . ? O2 C4 C3 110.3(2) . 2_454 ? O2 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 2_454 . ? O2 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 2_454 . ? H4A C4 H4B 108.1 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H1 Br1 0.81(4) 2.47(4) 3.2621(19) 166(3) 1_655 O3 H2 O2 0.75(3) 2.01(3) 2.757(3) 174(3) 2 C1 H1A Br1 0.99 2.94 3.741(2) 138.5 2_565 C4 H4B Br1 0.99 3.04 3.990(3) 160.1 2_565 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 30.99 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.871 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.104 # Attachment '- CCDC802396.cif' data_802396 _database_code_depnum_ccdc_archive 'CCDC 802396' #TrackingRef '- CCDC802396.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H24 Br2 Co O8' _chemical_formula_weight 467.02 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 'C 2/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 23.4355(4) _cell_length_b 25.8418(6) _cell_length_c 11.7298(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.1090(10) _cell_angle_gamma 90.00 _cell_volume 6533.7(2) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15347 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 25.028 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.899 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3728 _exptl_absorpt_coefficient_mu 5.969 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.226 _exptl_absorpt_correction_T_max 0.469 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42739 _diffrn_reflns_av_R_equivalents 0.1059 _diffrn_reflns_av_sigmaI/netI 0.0637 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 25.09 _reflns_number_total 5777 _reflns_number_gt 2632 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0375P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5777 _refine_ls_number_parameters 392 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.1052 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.1012 _refine_ls_wR_factor_gt 0.0830 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.912 _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 0.18755(3) 0.06042(3) 0.89299(6) 0.02398(19) Uani 1 1 d . . . Br2 Br 0.43110(3) 0.31719(3) 0.38042(6) 0.02425(19) Uani 1 1 d . . . Br3 Br 0.32210(3) 0.06464(3) 0.62641(6) 0.02354(19) Uani 1 1 d . . . Br4 Br 0.43532(3) 0.19241(3) 0.88875(6) 0.0240(2) Uani 1 1 d . . . Co1 Co 0.25578(3) 0.06289(5) 0.76169(6) 0.0185(3) Uani 1 1 d . . . Co2 Co 0.5000 0.31788(6) 0.2500 0.0195(3) Uani 1 2 d SD . . Co3 Co 0.5000 0.19369(5) 0.7500 0.0191(3) Uani 1 2 d S . . O1 O 0.31415(19) 0.11859(19) 0.8758(4) 0.0273(12) Uani 1 1 d D . . O2 O 0.2004(2) 0.00614(17) 0.6483(4) 0.0240(12) Uani 1 1 d D . . O3 O 0.1997(2) 0.11957(17) 0.6503(4) 0.0252(11) Uani 1 1 d D . . O4 O 0.3112(2) 0.00641(18) 0.8774(4) 0.0273(12) Uani 1 1 d D . . O5 O 0.4423(2) 0.26227(17) 0.1345(4) 0.0279(12) Uani 1 1 d D . . O6 O 0.4432(2) 0.37509(17) 0.1405(4) 0.0266(12) Uani 1 1 d D . . O7 O 0.4444(2) 0.25136(18) 0.6366(4) 0.0292(13) Uani 1 1 d D . . O8 O 0.4425(2) 0.13696(19) 0.6373(4) 0.0263(12) Uani 1 1 d D . . O11 O 0.3949(2) 0.13813(19) 0.3811(4) 0.0449(14) Uani 1 1 d . . . O12 O 0.3551(2) 0.11647(19) 0.1295(4) 0.0472(14) Uani 1 1 d . . . O13 O 0.0108(2) 0.0405(2) -0.0655(4) 0.0510(14) Uani 1 1 d . . . O14 O 0.2393(2) 0.20768(19) 0.5648(4) 0.0439(13) Uani 1 1 d . . . O15 O 0.0953(2) 0.16524(18) 0.2723(4) 0.0467(14) Uani 1 1 d . . . O16 O 0.1618(2) 0.08255(19) 0.2307(4) 0.0481(14) Uani 1 1 d . . . O17 O 0.3138(2) 0.26104(19) 1.0396(4) 0.0444(14) Uani 1 1 d . . . O18 O 0.4379(2) 0.0116(2) 0.9623(5) 0.0520(15) Uani 1 1 d . . . H11 H 0.335(2) 0.109(2) 0.960(2) 0.078 Uiso 1 1 d D . . H12 H 0.344(2) 0.134(3) 0.852(5) 0.078 Uiso 1 1 d D . . H21 H 0.172(2) -0.017(2) 0.663(5) 0.078 Uiso 1 1 d D . . H22 H 0.206(3) -0.007(2) 0.577(4) 0.078 Uiso 1 1 d D . . H31 H 0.1650(18) 0.135(2) 0.660(6) 0.078 Uiso 1 1 d D . . H32 H 0.226(2) 0.1467(16) 0.648(6) 0.078 Uiso 1 1 d D . . H41 H 0.3531(13) 0.017(3) 0.913(5) 0.078 Uiso 1 1 d D . . H42 H 0.302(3) -0.012(2) 0.938(4) 0.078 Uiso 1 1 d D . . H51 H 0.447(3) 0.2339(16) 0.187(5) 0.078 Uiso 1 1 d D . . H52 H 0.454(3) 0.250(2) 0.068(4) 0.078 Uiso 1 1 d D . . H62 H 0.4614(16) 0.3999(14) 0.110(5) 0.078 Uiso 1 1 d D . . H71 H 0.448(3) 0.2805(16) 0.688(5) 0.078 Uiso 1 1 d D . . H72 H 0.457(3) 0.262(2) 0.573(4) 0.078 Uiso 1 1 d D . . H81 H 0.410(2) 0.124(3) 0.658(5) 0.078 Uiso 1 1 d D . . H82 H 0.425(2) 0.140(3) 0.5495(19) 0.078 Uiso 1 1 d D . . C1 C 0.4158(3) 0.1680(3) 0.3034(6) 0.041(2) Uani 1 1 d . . . H1A H 0.4576 0.1803 0.3505 0.049 Uiso 1 1 calc R . . H1B H 0.3891 0.1978 0.2721 0.049 Uiso 1 1 calc R . . C2 C 0.4150(3) 0.1351(3) 0.1970(6) 0.048(2) Uani 1 1 d . . . H2A H 0.4288 0.1555 0.1431 0.058 Uiso 1 1 calc R . . H2B H 0.4434 0.1063 0.2283 0.058 Uiso 1 1 calc R . . C3 C 0.3350(3) 0.0876(3) 0.2099(7) 0.048(2) Uani 1 1 d . . . H3A H 0.3620 0.0580 0.2421 0.058 Uiso 1 1 calc R . . H3B H 0.2933 0.0748 0.1639 0.058 Uiso 1 1 calc R . . C4 C 0.3356(3) 0.1196(3) 0.3122(6) 0.042(2) Uani 1 1 d . . . H4A H 0.3074 0.1485 0.2800 0.050 Uiso 1 1 calc R . . H4B H 0.3212 0.0994 0.3655 0.050 Uiso 1 1 calc R . . C5 C 0.2982(3) 0.2162(3) 0.5562(7) 0.054(2) Uani 1 1 d . . . H5A H 0.3182 0.1832 0.5573 0.065 Uiso 1 1 calc R . . H5B H 0.3249 0.2362 0.6270 0.065 Uiso 1 1 calc R . . C6 C 0.2893(4) 0.2443(3) 0.4400(7) 0.041(2) Uani 1 1 d . . . H6A H 0.3292 0.2495 0.4350 0.050 Uiso 1 1 calc R . . H6B H 0.2638 0.2236 0.3694 0.050 Uiso 1 1 calc R . . C7 C 0.0439(4) -0.0056(3) -0.0472(8) 0.048(2) Uani 1 1 d . . . H7A H 0.0849 0.0015 -0.0457 0.058 Uiso 1 1 calc R . . H7B H 0.0229 -0.0287 -0.1162 0.058 Uiso 1 1 calc R . . C8 C -0.0502(3) 0.0312(3) -0.0691(6) 0.043(2) Uani 1 1 d . . . H8A H -0.0734 0.0093 -0.1392 0.052 Uiso 1 1 calc R . . H8B H -0.0724 0.0636 -0.0779 0.052 Uiso 1 1 calc R . . C9 C 0.1560(4) 0.1300(3) 0.1704(6) 0.043(2) Uani 1 1 d . . . H9A H 0.1577 0.1245 0.0900 0.051 Uiso 1 1 calc R . . H9B H 0.1904 0.1522 0.2184 0.051 Uiso 1 1 calc R . . C10 C 0.0980(3) 0.1551(3) 0.1540(6) 0.042(2) Uani 1 1 d . . . H10A H 0.0946 0.1874 0.1096 0.050 Uiso 1 1 calc R . . H10B H 0.0636 0.1332 0.1050 0.050 Uiso 1 1 calc R . . C11 C 0.1607(4) 0.0916(3) 0.3496(6) 0.052(2) Uani 1 1 d . . . H11A H 0.1958 0.1131 0.3984 0.063 Uiso 1 1 calc R . . H11B H 0.1642 0.0590 0.3927 0.063 Uiso 1 1 calc R . . C12 C 0.1017(4) 0.1179(3) 0.3362(7) 0.053(3) Uani 1 1 d . . . H12A H 0.0668 0.0956 0.2910 0.064 Uiso 1 1 calc R . . H12B H 0.1015 0.1243 0.4175 0.064 Uiso 1 1 calc R . . C13 C 0.2782(4) 0.2454(3) 0.9191(6) 0.041(2) Uani 1 1 d . . . H13A H 0.3044 0.2271 0.8859 0.049 Uiso 1 1 calc R . . H13B H 0.2617 0.2757 0.8680 0.049 Uiso 1 1 calc R . . C14 C 0.2269(3) 0.2118(3) 0.9127(7) 0.050(2) Uani 1 1 d . . . H14A H 0.2431 0.1808 0.9612 0.060 Uiso 1 1 calc R . . H14B H 0.2035 0.2016 0.8274 0.060 Uiso 1 1 calc R . . C15 C 0.4716(4) -0.0094(4) 1.0802(7) 0.052(3) Uani 1 1 d . . . H15A H 0.4444 -0.0304 1.1058 0.063 Uiso 1 1 calc R . . H15B H 0.4881 0.0183 1.1400 0.063 Uiso 1 1 calc R . . C16 C 0.4772(4) 0.0414(3) 0.9239(7) 0.050(2) Uani 1 1 d . . . H16A H 0.4940 0.0700 0.9810 0.060 Uiso 1 1 calc R . . H16B H 0.4537 0.0557 0.8423 0.060 Uiso 1 1 calc R . . H61 H 0.415(2) 0.3899(17) 0.169(4) 0.075 Uiso 1 1 d 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 Br1 0.0228(4) 0.0306(4) 0.0227(3) 0.0013(4) 0.0134(3) 0.0007(4) Br2 0.0230(4) 0.0306(4) 0.0232(4) 0.0020(4) 0.0134(3) 0.0019(4) Br3 0.0241(4) 0.0288(4) 0.0225(3) -0.0007(4) 0.0143(3) -0.0013(4) Br4 0.0254(4) 0.0288(4) 0.0222(3) -0.0023(3) 0.0140(3) -0.0026(4) Co1 0.0182(6) 0.0220(6) 0.0160(5) 0.0001(4) 0.0074(4) -0.0005(4) Co2 0.0196(7) 0.0205(8) 0.0197(6) 0.000 0.0091(6) 0.000 Co3 0.0189(7) 0.0209(8) 0.0177(6) 0.000 0.0073(6) 0.000 O1 0.026(3) 0.039(3) 0.018(2) -0.001(2) 0.010(2) -0.006(2) O2 0.024(3) 0.025(3) 0.025(2) -0.009(2) 0.012(2) -0.010(2) O3 0.019(2) 0.030(3) 0.027(2) 0.006(2) 0.009(2) 0.005(2) O4 0.023(3) 0.031(3) 0.031(3) 0.012(2) 0.013(2) 0.004(2) O5 0.033(3) 0.027(3) 0.024(3) -0.002(2) 0.011(2) -0.004(2) O6 0.030(3) 0.021(3) 0.034(3) 0.013(2) 0.019(2) 0.009(2) O7 0.036(3) 0.033(3) 0.022(3) 0.003(2) 0.015(2) 0.009(2) O8 0.029(3) 0.031(3) 0.025(2) -0.007(2) 0.017(2) -0.009(2) O11 0.049(3) 0.057(4) 0.021(2) -0.001(2) 0.006(2) -0.019(3) O12 0.057(4) 0.061(4) 0.022(2) -0.004(3) 0.014(2) -0.019(3) O13 0.039(3) 0.049(3) 0.067(3) 0.028(3) 0.023(3) 0.006(3) O14 0.039(3) 0.035(3) 0.064(3) 0.025(3) 0.027(3) 0.004(3) O15 0.068(4) 0.035(3) 0.040(3) 0.003(3) 0.024(3) 0.021(3) O16 0.068(4) 0.040(3) 0.039(3) 0.004(3) 0.024(3) 0.025(3) O17 0.022(3) 0.063(4) 0.044(3) -0.024(3) 0.009(2) -0.006(3) O18 0.024(3) 0.061(4) 0.067(4) 0.024(3) 0.015(3) 0.005(3) C1 0.046(5) 0.034(4) 0.034(4) -0.008(4) 0.006(4) -0.028(4) C2 0.032(4) 0.073(6) 0.042(4) 0.017(5) 0.018(4) -0.014(5) C3 0.049(5) 0.042(5) 0.061(5) -0.014(4) 0.030(4) -0.029(4) C4 0.043(5) 0.058(6) 0.029(4) 0.008(4) 0.019(4) -0.005(5) C5 0.030(5) 0.059(6) 0.073(6) 0.025(5) 0.021(4) 0.023(4) C6 0.040(5) 0.045(5) 0.046(5) 0.006(4) 0.024(4) -0.009(4) C7 0.036(5) 0.025(4) 0.095(7) -0.001(5) 0.038(5) 0.006(4) C8 0.032(5) 0.043(5) 0.050(5) 0.018(4) 0.010(4) 0.018(4) C9 0.054(5) 0.040(5) 0.041(5) -0.009(4) 0.026(4) -0.003(5) C10 0.042(4) 0.058(5) 0.019(4) 0.018(4) 0.004(3) 0.014(4) C11 0.075(6) 0.043(5) 0.033(4) 0.009(4) 0.015(4) 0.028(5) C12 0.095(7) 0.047(5) 0.037(5) 0.001(4) 0.048(5) 0.001(5) C13 0.043(5) 0.054(5) 0.033(4) -0.001(4) 0.023(4) 0.018(4) C14 0.047(5) 0.048(5) 0.054(5) -0.039(4) 0.018(4) -0.023(5) C15 0.040(5) 0.078(7) 0.038(4) 0.018(5) 0.014(4) -0.015(5) C16 0.056(6) 0.047(5) 0.041(4) 0.018(4) 0.013(4) -0.008(5) _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 Co1 2.6204(9) . ? Br2 Co2 2.6243(6) . ? Br3 Co1 2.6213(9) . ? Br4 Co3 2.6238(6) . ? Co1 O3 2.058(5) . ? Co1 O2 2.061(4) . ? Co1 O4 2.068(4) . ? Co1 O1 2.073(5) . ? Co2 O6 2.066(4) 2_655 ? Co2 O6 2.066(4) . ? Co2 O5 2.071(5) . ? Co2 O5 2.071(5) 2_655 ? Co2 Br2 2.6243(6) 2_655 ? Co3 O8 2.077(5) . ? Co3 O8 2.077(4) 2_656 ? Co3 O7 2.080(5) 2_656 ? Co3 O7 2.080(5) . ? Co3 Br4 2.6238(6) 2_656 ? O1 H11 0.946(19) . ? O1 H12 0.943(19) . ? O2 H21 0.950(19) . ? O2 H22 0.956(19) . ? O3 H31 0.949(19) . ? O3 H32 0.943(19) . ? O4 H41 0.941(19) . ? O4 H42 0.946(19) . ? O5 H51 0.939(19) . ? O5 H52 0.970(19) . ? O6 H62 0.920(18) . ? O6 H61 0.929(18) . ? O7 H71 0.949(19) . ? O7 H72 0.938(19) . ? O8 H81 0.953(19) . ? O8 H82 0.950(19) . ? O11 C4 1.390(8) . ? O11 C1 1.420(7) . ? O12 C2 1.399(8) . ? O12 C3 1.422(7) . ? O13 C7 1.391(8) . ? O13 C8 1.435(7) . ? O14 C6 1.400(8) 7_556 ? O14 C5 1.441(7) . ? O15 C12 1.411(8) . ? O15 C10 1.438(7) . ? O16 C9 1.395(8) . ? O16 C11 1.424(7) . ? O17 C13 1.390(8) . ? O17 C14 1.461(7) 7_557 ? O18 C15 1.404(8) . ? O18 C16 1.404(7) . ? C1 C2 1.504(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.453(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.485(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O14 1.400(8) 7_556 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.471(9) 5 ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C7 1.471(9) 5 ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.449(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.493(10) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.461(9) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 O17 1.461(7) 7_557 ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.473(10) 5_657 ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C15 1.473(10) 5_657 ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? 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 O3 Co1 O2 90.75(17) . . ? O3 Co1 O4 178.37(18) . . ? O2 Co1 O4 89.8(2) . . ? O3 Co1 O1 90.6(2) . . ? O2 Co1 O1 178.01(19) . . ? O4 Co1 O1 88.91(18) . . ? O3 Co1 Br1 90.29(12) . . ? O2 Co1 Br1 89.27(12) . . ? O4 Co1 Br1 88.16(12) . . ? O1 Co1 Br1 92.16(11) . . ? O3 Co1 Br3 89.22(12) . . ? O2 Co1 Br3 89.66(12) . . ? O4 Co1 Br3 92.34(12) . . ? O1 Co1 Br3 88.92(11) . . ? Br1 Co1 Br3 178.82(5) . . ? O6 Co2 O6 88.6(3) 2_655 . ? O6 Co2 O5 177.85(19) 2_655 . ? O6 Co2 O5 89.65(16) . . ? O6 Co2 O5 89.65(16) 2_655 2_655 ? O6 Co2 O5 177.85(19) . 2_655 ? O5 Co2 O5 92.1(3) . 2_655 ? O6 Co2 Br2 92.10(11) 2_655 . ? O6 Co2 Br2 88.45(11) . . ? O5 Co2 Br2 89.08(12) . . ? O5 Co2 Br2 90.38(12) 2_655 . ? O6 Co2 Br2 88.45(11) 2_655 2_655 ? O6 Co2 Br2 92.10(11) . 2_655 ? O5 Co2 Br2 90.38(12) . 2_655 ? O5 Co2 Br2 89.08(12) 2_655 2_655 ? Br2 Co2 Br2 179.22(8) . 2_655 ? O8 Co3 O8 90.2(3) . 2_656 ? O8 Co3 O7 178.52(19) . 2_656 ? O8 Co3 O7 90.67(17) 2_656 2_656 ? O8 Co3 O7 90.67(17) . . ? O8 Co3 O7 178.52(19) 2_656 . ? O7 Co3 O7 88.5(3) 2_656 . ? O8 Co3 Br4 89.88(11) . . ? O8 Co3 Br4 89.10(11) 2_656 . ? O7 Co3 Br4 88.94(12) 2_656 . ? O7 Co3 Br4 92.09(12) . . ? O8 Co3 Br4 89.10(11) . 2_656 ? O8 Co3 Br4 89.88(11) 2_656 2_656 ? O7 Co3 Br4 92.09(12) 2_656 2_656 ? O7 Co3 Br4 88.94(12) . 2_656 ? Br4 Co3 Br4 178.55(7) . 2_656 ? Co1 O1 H11 116(4) . . ? Co1 O1 H12 119(4) . . ? H11 O1 H12 106(3) . . ? Co1 O2 H21 129(3) . . ? Co1 O2 H22 124(4) . . ? H21 O2 H22 106(3) . . ? Co1 O3 H31 125(4) . . ? Co1 O3 H32 106(4) . . ? H31 O3 H32 108(3) . . ? Co1 O4 H41 112(4) . . ? Co1 O4 H42 125(4) . . ? H41 O4 H42 108(3) . . ? Co2 O5 H51 104(4) . . ? Co2 O5 H52 116(4) . . ? H51 O5 H52 106(3) . . ? Co2 O6 H62 117.2(19) . . ? Co2 O6 H61 116.3(18) . . ? H62 O6 H61 111(2) . . ? Co3 O7 H71 106(4) . . ? Co3 O7 H72 114(4) . . ? H71 O7 H72 108(3) . . ? Co3 O8 H81 118(4) . . ? Co3 O8 H82 122(4) . . ? H81 O8 H82 105(3) . . ? C4 O11 C1 109.5(5) . . ? C2 O12 C3 109.1(5) . . ? C7 O13 C8 110.5(6) . . ? C6 O14 C5 108.5(6) 7_556 . ? C12 O15 C10 108.6(5) . . ? C9 O16 C11 108.5(5) . . ? C13 O17 C14 107.9(5) . 7_557 ? C15 O18 C16 110.0(6) . . ? O11 C1 C2 109.4(6) . . ? O11 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? O11 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? O12 C2 C1 110.3(6) . . ? O12 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 . . ? O12 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? O12 C3 C4 110.6(6) . . ? O12 C3 H3A 109.5 . . ? C4 C3 H3A 109.5 . . ? O12 C3 H3B 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? O11 C4 C3 111.1(6) . . ? O11 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? O11 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? O14 C5 C6 110.2(6) . . ? O14 C5 H5A 109.6 . . ? C6 C5 H5A 109.6 . . ? O14 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? O14 C6 C5 111.3(6) 7_556 . ? O14 C6 H6A 109.4 7_556 . ? C5 C6 H6A 109.4 . . ? O14 C6 H6B 109.4 7_556 . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? O13 C7 C8 112.0(6) . 5 ? O13 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 5 . ? O13 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 5 . ? H7A C7 H7B 107.9 . . ? O13 C8 C7 108.2(6) . 5 ? O13 C8 H8A 110.1 . . ? C7 C8 H8A 110.1 5 . ? O13 C8 H8B 110.1 . . ? C7 C8 H8B 110.1 5 . ? H8A C8 H8B 108.4 . . ? O16 C9 C10 111.2(6) . . ? O16 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? O16 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? O15 C10 C9 110.4(5) . . ? O15 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? O15 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? O16 C11 C12 110.0(6) . . ? O16 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? O16 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? O15 C12 C11 110.6(6) . . ? O15 C12 H12A 109.5 . . ? C11 C12 H12A 109.5 . . ? O15 C12 H12B 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? O17 C13 C14 112.2(6) . . ? O17 C13 H13A 109.2 . . ? C14 C13 H13A 109.2 . . ? O17 C13 H13B 109.2 . . ? C14 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C13 C14 O17 110.1(6) . 7_557 ? C13 C14 H14A 109.6 . . ? O17 C14 H14A 109.6 7_557 . ? C13 C14 H14B 109.6 . . ? O17 C14 H14B 109.6 7_557 . ? H14A C14 H14B 108.2 . . ? O18 C15 C16 109.6(6) . 5_657 ? O18 C15 H15A 109.8 . . ? C16 C15 H15A 109.8 5_657 . ? O18 C15 H15B 109.8 . . ? C16 C15 H15B 109.8 5_657 . ? H15A C15 H15B 108.2 . . ? O18 C16 C15 110.3(6) . 5_657 ? O18 C16 H16A 109.6 . . ? C15 C16 H16A 109.6 5_657 . ? O18 C16 H16B 109.6 . . ? C15 C16 H16B 109.6 5_657 . ? H16A C16 H16B 108.1 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H11 O12 0.946(19) 1.86(3) 2.745(6) 154(6) 1_556 O1 H12 Br4 0.943(19) 2.51(4) 3.375(4) 153(5) . O2 H21 O16 0.950(19) 1.94(4) 2.774(6) 146(6) 6_556 O2 H22 Br1 0.956(19) 2.45(3) 3.363(4) 159(5) 6 O3 H31 Br2 0.949(19) 2.45(3) 3.365(4) 162(6) 7_556 O3 H32 O14 0.943(19) 1.94(4) 2.790(6) 148(6) . O4 H41 O18 0.941(19) 1.84(3) 2.740(6) 158(6) . O4 H42 Br3 0.946(19) 2.48(3) 3.373(4) 158(5) 6_556 O6 H61 Br1 0.929(18) 2.57(2) 3.372(4) 145(3) 7_556 O5 H52 Br4 0.970(19) 2.47(4) 3.350(4) 150(6) 1_554 O6 H62 O13 0.920(18) 1.82(2) 2.728(6) 167(4) 7 O7 H71 O15 0.949(19) 1.90(4) 2.727(6) 145(6) 7_556 O7 H72 Br2 0.938(19) 2.54(4) 3.359(4) 146(6) . O8 H81 Br4 0.953(19) 3.09(6) 3.343(4) 97(4) . O5 H52 Br4 0.970(19) 2.47(4) 3.350(4) 150(6) 1_554 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.500 _refine_diff_density_min -1.077 _refine_diff_density_rms 0.117 # Attachment '- CCDC802397.cif' data_802397 _database_code_depnum_ccdc_archive 'CCDC 802397' #TrackingRef '- CCDC802397.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H24 Br2 Co O8' _chemical_formula_weight 467.02 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 9.1728(3) _cell_length_b 9.1728(3) _cell_length_c 19.5503(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1644.97(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10336 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485? _exptl_crystal_description dimonaiod _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_diffrn 1.886 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 932 _exptl_absorpt_coefficient_mu 5.928 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.105 _exptl_absorpt_correction_T_max 0.226 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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 KappaCCD _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 10060 _diffrn_reflns_av_R_equivalents 0.0910 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 27.50 _reflns_number_total 940 _reflns_number_gt 662 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0515P)^2^+8.1672P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0065(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 940 _refine_ls_number_parameters 51 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1239 _refine_ls_wR_factor_gt 0.1132 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 Co1 Co 0.5000 0.2500 0.3750 0.0464(4) Uani 1 4 d S . . Br1 Br 0.5000 0.2500 0.50893(3) 0.0512(3) Uani 1 2 d S . . O1 O 0.5013(6) 0.0237(5) 0.3759(2) 0.0640(12) Uani 1 1 d . . . H1 H 0.516(8) -0.037(8) 0.429(4) 0.096 Uiso 1 1 d . . . H2 H 0.458(11) 0.036(11) 0.396(5) 0.096 Uiso 1 1 d . . . O2 O 0.2917(10) -0.1297(9) 0.2812(6) 0.173(4) Uani 1 1 d . . . C1 C 0.2528(9) -0.2515(13) 0.3181(4) 0.103(3) Uani 1 1 d . . . H1A H 0.2953 -0.2475 0.3635 0.124 Uiso 1 1 calc R . . H1B H 0.1476 -0.2563 0.3227 0.124 Uiso 1 1 calc R . . C2 C 0.2008(10) -0.1371(9) 0.2136(5) 0.098(3) Uani 1 1 d . . . H2A H 0.0978 -0.1469 0.2237 0.118 Uiso 1 1 calc R . . H2B H 0.2154 -0.0497 0.1865 0.118 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 Co1 0.0564(5) 0.0564(5) 0.0264(6) 0.000 0.000 0.000 Br1 0.0565(5) 0.0724(6) 0.0245(4) 0.000 0.000 -0.0001(4) O1 0.096(4) 0.061(2) 0.0349(18) 0.0005(19) 0.000(2) 0.002(2) O2 0.192(8) 0.114(6) 0.213(9) -0.098(6) 0.076(7) -0.084(6) C1 0.076(5) 0.185(11) 0.047(4) 0.004(6) -0.025(4) -0.004(6) C2 0.115(7) 0.068(5) 0.111(7) 0.051(5) 0.025(6) 0.042(5) _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 Co1 O1 2.076(5) 11_666 ? Co1 O1 2.076(5) . ? Co1 O1 2.076(5) 6_554 ? Co1 O1 2.076(5) 16_656 ? Co1 Br1 2.6184(6) . ? Co1 Br1 2.6184(6) 11_666 ? Co1 H2 2.04(10) . ? O1 H1 1.19(8) . ? O1 H2 0.57(9) . ? O2 C1 1.377(11) . ? O2 C2 1.563(12) . ? C1 C2 1.268(11) 13_545 ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C1 1.268(11) 13_545 ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? 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 Co1 O1 90.004(2) 11_666 . ? O1 Co1 O1 90.004(2) 11_666 6_554 ? O1 Co1 O1 179.1(2) . 6_554 ? O1 Co1 O1 179.1(2) 11_666 16_656 ? O1 Co1 O1 90.004(2) . 16_656 ? O1 Co1 O1 90.004(2) 6_554 16_656 ? O1 Co1 Br1 90.46(11) 11_666 . ? O1 Co1 Br1 89.54(11) . . ? O1 Co1 Br1 89.54(11) 6_554 . ? O1 Co1 Br1 90.46(11) 16_656 . ? O1 Co1 Br1 89.54(11) 11_666 11_666 ? O1 Co1 Br1 90.46(11) . 11_666 ? O1 Co1 Br1 90.46(11) 6_554 11_666 ? O1 Co1 Br1 89.54(11) 16_656 11_666 ? Br1 Co1 Br1 180.0 . 11_666 ? O1 Co1 H2 79(3) 11_666 . ? O1 Co1 H2 16(3) . . ? O1 Co1 H2 163(3) 6_554 . ? O1 Co1 H2 101(3) 16_656 . ? Br1 Co1 H2 78(3) . . ? Br1 Co1 H2 102(3) 11_666 . ? Co1 O1 H1 119(4) . . ? Co1 O1 H2 79(10) . . ? H1 O1 H2 64(10) . . ? C1 O2 C2 105.6(6) . . ? C2 C1 O2 108.1(7) 13_545 . ? C2 C1 H1A 110.1 13_545 . ? O2 C1 H1A 110.1 . . ? C2 C1 H1B 110.1 13_545 . ? O2 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? C1 C2 O2 105.6(6) 13_545 . ? C1 C2 H2A 110.6 13_545 . ? O2 C2 H2A 110.6 . . ? C1 C2 H2B 110.6 13_545 . ? O2 C2 H2B 110.6 . . ? H2A C2 H2B 108.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 Br1 1.19(8) 2.30(8) 3.373(5) 149(5) 9_656 O1 H2 Br1 0.57(9) 2.98(10) 3.328(4) 123(12) . O1 H1 Br1 1.19(8) 2.30(8) 3.373(5) 149(5) 9_656 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.683 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.101 # Attachment '- CCDC802398.cif' data_802398 _database_code_depnum_ccdc_archive 'CCDC 802398' #TrackingRef '- CCDC802398.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H32 Br2 Co O10' _chemical_formula_weight 555.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.4597(16) _cell_length_b 9.033(2) _cell_length_c 9.738(3) _cell_angle_alpha 105.540(4) _cell_angle_beta 98.341(3) _cell_angle_gamma 92.690(3) _cell_volume 539.4(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2242 _cell_measurement_theta_min 2.3409 _cell_measurement_theta_max 30.4866 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 281 _exptl_absorpt_coefficient_mu 4.541 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0858 _exptl_absorpt_correction_T_max 0.2806 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 8706 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 30.49 _reflns_number_total 3260 _reflns_number_gt 3019 _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 _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0193P)^2^+0.3116P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3260 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0683 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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 Co1 Co 0.5000 0.5000 0.5000 0.02096(10) Uani 1 2 d S . . Br2 Br 0.83887(3) 0.61917(3) 0.68927(2) 0.02753(7) Uani 1 1 d . . . O1 O 0.3243(3) 0.6197(2) 0.64276(19) 0.0311(4) Uani 1 1 d . . . O2 O 0.4797(3) 0.31540(19) 0.58983(18) 0.0276(4) Uani 1 1 d . . . O3 O 0.8517(3) 0.8870(2) 0.4028(2) 0.0360(4) Uani 1 1 d . . . O4 O 0.4381(3) 0.88048(19) 0.87175(18) 0.0337(4) Uani 1 1 d . . . O5 O 0.4821(3) 0.63049(19) 1.11432(17) 0.0329(4) Uani 1 1 d . . . C1 C 1.0706(4) 0.8644(3) 0.4207(3) 0.0362(6) Uani 1 1 d . . . H1A H 1.1365 0.9003 0.3483 0.043 Uiso 1 1 calc R . . H1B H 1.0883 0.7531 0.4048 0.043 Uiso 1 1 calc R . . C2 C 0.8238(4) 1.0483(3) 0.4307(3) 0.0347(6) Uani 1 1 d . . . H2A H 0.6719 1.0627 0.4205 0.042 Uiso 1 1 calc R . . H2B H 0.8832 1.0895 0.3588 0.042 Uiso 1 1 calc R . . C3 C 0.6192(4) 0.9856(3) 0.8894(3) 0.0360(6) Uani 1 1 d . . . H3A H 0.5786 1.0731 0.8513 0.043 Uiso 1 1 calc R . . H3B H 0.7243 0.9325 0.8340 0.043 Uiso 1 1 calc R . . C4 C 0.2862(4) 0.9550(3) 0.9533(3) 0.0373(6) Uani 1 1 d . . . H4A H 0.1627 0.8810 0.9418 0.045 Uiso 1 1 calc R . . H4B H 0.2383 1.0419 0.9166 0.045 Uiso 1 1 calc R . . C5 C 0.6958(4) 0.4428(3) 0.9913(3) 0.0351(5) Uani 1 1 d . . . H5A H 0.8244 0.4317 0.9465 0.042 Uiso 1 1 calc R . . H5B H 0.7117 0.3921 1.0702 0.042 Uiso 1 1 calc R . . C6 C 0.6706(4) 0.6107(3) 1.0523(3) 0.0347(6) Uani 1 1 d . . . H6A H 0.7932 0.6590 1.1273 0.042 Uiso 1 1 calc R . . H6B H 0.6652 0.6629 0.9747 0.042 Uiso 1 1 calc R . . H1 H 0.365(5) 0.694(4) 0.713(3) 0.052 Uiso 1 1 d . . . H2 H 0.200(5) 0.608(4) 0.642(4) 0.052 Uiso 1 1 d . . . H3 H 0.368(5) 0.258(4) 0.572(3) 0.052 Uiso 1 1 d . . . H4 H 0.503(5) 0.342(4) 0.673(4) 0.052 Uiso 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 Co1 0.0195(2) 0.0204(2) 0.02061(19) 0.00098(15) 0.00502(15) 0.00054(15) Br2 0.02020(12) 0.03157(13) 0.02564(12) -0.00007(9) 0.00343(8) -0.00126(9) O1 0.0208(8) 0.0335(9) 0.0292(9) -0.0094(7) 0.0080(7) -0.0005(7) O2 0.0298(9) 0.0247(8) 0.0261(8) 0.0047(7) 0.0034(7) -0.0022(7) O3 0.0312(9) 0.0274(9) 0.0433(10) 0.0067(7) -0.0054(8) -0.0061(7) O4 0.0377(10) 0.0249(8) 0.0304(9) -0.0042(7) 0.0021(7) 0.0015(7) O5 0.0403(10) 0.0300(9) 0.0242(8) 0.0020(7) 0.0035(7) -0.0002(8) C1 0.0374(14) 0.0296(13) 0.0385(14) 0.0058(10) 0.0031(11) 0.0039(11) C2 0.0295(13) 0.0319(13) 0.0406(14) 0.0112(11) -0.0038(11) 0.0024(10) C3 0.0453(15) 0.0268(12) 0.0339(13) 0.0017(10) 0.0120(11) 0.0032(11) C4 0.0342(14) 0.0264(12) 0.0417(14) -0.0047(10) 0.0019(11) 0.0024(10) C5 0.0338(13) 0.0383(14) 0.0309(12) 0.0080(10) 0.0014(10) 0.0031(11) C6 0.0361(14) 0.0340(13) 0.0297(12) 0.0041(10) 0.0033(10) -0.0053(11) _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 Co1 O1 2.0391(17) . ? Co1 O1 2.0391(17) 2_666 ? Co1 O2 2.0873(17) 2_666 ? Co1 O2 2.0873(17) . ? Co1 Br2 2.6254(5) 2_666 ? Co1 Br2 2.6254(5) . ? O1 H1 0.82(3) . ? O1 H2 0.80(3) . ? O2 H3 0.84(3) . ? O2 H4 0.77(3) . ? O3 C1 1.430(3) . ? O3 C2 1.434(3) . ? O4 C4 1.431(3) . ? O4 C3 1.431(3) . ? O5 C5 1.428(3) 2_667 ? O5 C6 1.433(3) . ? C1 C2 1.494(3) 2_776 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C1 1.494(3) 2_776 ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.505(4) 2_677 ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C3 1.505(4) 2_677 ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 O5 1.428(3) 2_667 ? C5 C6 1.499(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? 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 Co1 O1 180.0 . 2_666 ? O1 Co1 O2 90.24(8) . 2_666 ? O1 Co1 O2 89.76(8) 2_666 2_666 ? O1 Co1 O2 89.76(8) . . ? O1 Co1 O2 90.24(8) 2_666 . ? O2 Co1 O2 180.00(4) 2_666 . ? O1 Co1 Br2 91.23(5) . 2_666 ? O1 Co1 Br2 88.77(5) 2_666 2_666 ? O2 Co1 Br2 89.62(5) 2_666 2_666 ? O2 Co1 Br2 90.38(5) . 2_666 ? O1 Co1 Br2 88.77(5) . . ? O1 Co1 Br2 91.23(5) 2_666 . ? O2 Co1 Br2 90.38(5) 2_666 . ? O2 Co1 Br2 89.62(5) . . ? Br2 Co1 Br2 180.0 2_666 . ? Co1 O1 H1 127(2) . . ? Co1 O1 H2 129(2) . . ? H1 O1 H2 104(3) . . ? Co1 O2 H3 121(2) . . ? Co1 O2 H4 112(2) . . ? H3 O2 H4 103(3) . . ? C1 O3 C2 110.18(19) . . ? C4 O4 C3 110.23(19) . . ? C5 O5 C6 110.21(18) 2_667 . ? O3 C1 C2 110.2(2) . 2_776 ? O3 C1 H1A 109.6 . . ? C2 C1 H1A 109.6 2_776 . ? O3 C1 H1B 109.6 . . ? C2 C1 H1B 109.6 2_776 . ? H1A C1 H1B 108.1 . . ? O3 C2 C1 111.0(2) . 2_776 ? O3 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 2_776 . ? O3 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 2_776 . ? H2A C2 H2B 108.0 . . ? O4 C3 C4 110.1(2) . 2_677 ? O4 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 2_677 . ? O4 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 2_677 . ? H3A C3 H3B 108.1 . . ? O4 C4 C3 110.1(2) . 2_677 ? O4 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 2_677 . ? O4 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 2_677 . ? H4A C4 H4B 108.2 . . ? O5 C5 C6 110.6(2) 2_667 . ? O5 C5 H5A 109.5 2_667 . ? C6 C5 H5A 109.5 . . ? O5 C5 H5B 109.5 2_667 . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? O5 C6 C5 110.8(2) . . ? O5 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? O5 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H2 Br2 0.80(3) 2.45(3) 3.2323(19) 167(3) 1_455 O1 H1 O4 0.82(3) 1.94(3) 2.758(2) 175(3) . O2 H3 O3 0.84(3) 1.97(3) 2.771(3) 160(3) 2_666 O2 H4 O5 0.77(3) 2.00(3) 2.762(2) 167(3) 2_667 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.49 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.403 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.084