data_leeds _journal_coden_Cambridge 440 _audit_creation_method SHELXL-97 _publ_contact_author_name ' Michaele J. Hardie' _publ_contact_author_address ; School of Chemistry University of Leeds Woodhouse Lane Leeds LS2 9JT UNITED KINGDOM ; _publ_contact_author_email ' m.j.hardie@leeds.ac.uk ' _publ_contact_author_fax ' 44 - 113 - 343 6565' loop_ _publ_author_name _publ_author_address ' Andreas Franken' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; ' Neil J. Bullen' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; ' Tomas Jelinek' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; ' Mark Thornton-Pett' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; ' Simon J. Teat' ; Daresbury Laboratory Daresbury, Warrington WA4 4AD UK ; ' William Clegg' ; Daresbury Laboratory Daresbury, Warrington WA4 4AD UK ; ' John D. Kennedy' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; ' Michaele J. Hardie ' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Structural chemistry of halogenated monocarbaboranes: the eextended structures of Cs[1-HC9H4Br5], Cs[1-HCB11H5Cl6] and Cs[1-HCB11H5Br6] ; data_complex_1a _database_code_depnum_ccdc_archive 'CCDC 248036' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'caesium penta-bromo-monocarbadecaborane' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C H5 B9 Br5 Cs' _chemical_formula_weight 646.80 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' B B 0.0013 0.0007 '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' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4/nmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x, z' '-x+1/2, -y+1/2, z' 'y, -x+1/2, z' '-x+1/2, y, z' 'y, x, z' 'x, -y+1/2, z' '-y+1/2, -x+1/2, z' '-x, -y, -z' 'y-1/2, -x, -z' 'x-1/2, y-1/2, -z' '-y, x-1/2, -z' 'x-1/2, -y, -z' '-y, -x, -z' '-x, y-1/2, -z' 'y-1/2, x-1/2, -z' _cell_length_a 8.3873(6) _cell_length_b 8.3873(6) _cell_length_c 10.5853(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 744.64(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3951 _cell_measurement_theta_min 6.00 _cell_measurement_theta_max 58.00 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.885 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 572 _exptl_absorpt_coefficient_mu 15.861 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1436 _exptl_absorpt_correction_T_max 0.5695 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.68830 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Siemens SMART area-detector diffractometer' _diffrn_measurement_method 'area detector \w-exposures' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3515 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 26.00 _reflns_number_total 493 _reflns_number_gt 481 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'local programs' _computing_data_reduction 'SMART (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _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^)+(0.0860P)^2^+0.2068P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 493 _refine_ls_number_parameters 34 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1222 _refine_ls_wR_factor_gt 0.1211 _refine_ls_goodness_of_fit_ref 1.241 _refine_ls_restrained_S_all 1.241 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 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 Cs1 Cs 0.2500 0.7500 0.5000 0.0265(4) Uani 1 8 d S . . C1 C 0.2500 0.2500 1.0236(7) 0.0188(16) Uani 1 8 d S . . H1 H 0.2500 0.2500 1.108(9) 0.03(2) Uiso 1 8 d S . . B2 B 0.4065(5) 0.2500 0.9372(4) 0.0186(9) Uani 1 2 d S . . H2 H 0.539(7) 0.2500 0.979(4) 0.024(12) Uiso 1 2 d S . . B6 B 0.3597(3) 0.3597(3) 0.7941(4) 0.0157(8) Uani 1 2 d S . . Br6 Br 0.51334(6) 0.51334(6) 0.72524(6) 0.0218(3) Uani 1 2 d S . . B10 B 0.2500 0.2500 0.6921(7) 0.0148(15) Uiso 1 8 d S . . Br10 Br 0.2500 0.2500 0.50937(8) 0.0217(4) Uani 1 8 d S . . 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 Cs1 0.0290(4) 0.0290(4) 0.0214(5) 0.000 0.000 0.000 C1 0.025(2) 0.025(2) 0.006(3) 0.000 0.000 0.000 B2 0.0184(18) 0.0204(19) 0.0170(19) 0.000 -0.0026(14) 0.000 B6 0.0149(11) 0.0149(11) 0.018(2) -0.0012(9) -0.0012(9) -0.0003(15) Br6 0.0197(4) 0.0197(4) 0.0259(5) 0.00154(11) 0.00154(11) -0.00658(15) Br10 0.0276(5) 0.0276(5) 0.0100(6) 0.000 0.000 0.000 _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 Cs1 Br6 3.8083(4) . ? Cs1 Br10 4.1948(3) . ? C1 B2 1.600(6) . ? B2 B6 1.816(5) . ? B2 B2 1.857(6) 2 ? B6 B10 1.690(6) . ? B6 B6 1.840(6) 2 ? B6 Br6 1.963(4) . ? B10 Br10 1.935(8) . ? 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 Br6 Cs1 Br6 62.827(19) 4_565 . ? Br6 Cs1 Br6 113.077(8) 10_566 . ? Br6 Cs1 Br6 77.725(16) . 9_666 ? Br6 Cs1 Br6 175.24(2) . 11_566 ? Br6 Cs1 Br6 102.478(16) . 3_565 ? Br6 Cs1 Br6 113.077(8) . 12_666 ? Br6 Cs1 Br6 70.897(19) . 2 ? Br6 Cs1 Br10 126.485(16) . 9_566 ? Br6 Cs1 Br10 120.415(16) . 1_565 ? Br6 Cs1 Br10 55.598(10) . 9_666 ? Br6 Cs1 Br10 57.597(9) . . ? Br10 Cs1 Br10 90.032(1) 9_566 . ? Br10 Cs1 Br10 177.29(2) 1_565 . ? B2 C1 B2 110.3(5) 3 . ? B2 C1 B2 70.9(3) 2 . ? C1 B2 B6 107.4(3) . . ? B6 B2 B6 60.9(2) 4 . ? B6 B2 B2 101.85(16) . 4 ? C1 B2 B2 54.53(13) . 2 ? B6 B2 B2 59.25(13) . 2 ? B2 B2 B2 90.000(1) 4 2 ? B10 B6 B2 112.0(3) . . ? B2 B6 B2 61.5(3) 2 . ? B10 B6 B6 57.02(13) . 2 ? B2 B6 B6 102.50(16) . 2 ? B2 B6 B6 59.55(12) . 4 ? B6 B6 B6 90.000(1) 2 4 ? B10 B6 Br6 118.5(3) . . ? B2 B6 Br6 120.0(2) . . ? B6 B6 Br6 131.04(4) 2 . ? B6 Br6 Cs1 101.17(7) . . ? Cs1 Br6 Cs1 102.275(16) 9_666 . ? B6 B10 B6 66.0(3) . 2 ? B6 B10 B6 100.7(5) . 3 ? B6 B10 B6 66.0(3) 2 3 ? B6 B10 Br10 129.7(2) . . ? B10 Br10 Cs1 91.355(12) . . ? Cs1 Br10 Cs1 89.968(1) 9_566 . ? Cs1 Br10 Cs1 177.29(2) 1_545 . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max '5.329 (0.3 A from Br6)' _refine_diff_density_min -3.398 _refine_diff_density_rms 0.628 #===END #complex 2a data_complex_2a _database_code_depnum_ccdc_archive 'CCDC 248037' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'caesium hexa-chloro-monocarbadodecaborane' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C H6 B11 Cl6 Cs' _chemical_formula_weight 482.58 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 14.5462(2) _cell_length_b 8.8913(2) _cell_length_c 12.2784(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.0100(10) _cell_angle_gamma 90.00 _cell_volume 1576.15(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.034 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 3.334 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5144 _exptl_absorpt_correction_T_max 0.8510 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 CCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23927 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3089 _reflns_number_gt 2849 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius)' _computing_cell_refinement DENZO _computing_data_reduction 'DENZO, SCALEPACK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour)' _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. Cs(2) shows a symmetry induced disorder and is refined at 50% occupancy. ; _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^)+(0.0408P)^2^+4.4038P] 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 3089 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.1019 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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 Cs1 Cs 1.0000 -0.21310(6) 0.2500 0.05926(17) Uani 1 2 d S . . C1 C 0.7427(3) 0.2983(5) 0.1722(3) 0.0342(9) Uani 1 1 d . . . H1 H 0.7359 0.3200 0.0817 0.041 Uiso 1 1 calc R . . Cs2 Cs 0.55410(4) 0.75630(6) 0.18738(5) 0.04648(17) Uani 0.50 1 d P . . B2 B 0.6456(3) 0.3192(5) 0.2356(4) 0.0321(9) Uani 1 1 d . . . H2 H 0.5758 0.3533 0.1942 0.039 Uiso 1 1 calc R . . B3 B 0.6932(3) 0.1391(5) 0.2141(4) 0.0328(9) Uani 1 1 d . . . H3 H 0.6542 0.0546 0.1587 0.039 Uiso 1 1 calc R . . B4 B 0.8155(3) 0.1588(5) 0.2211(4) 0.0325(9) Uani 1 1 d . . . H4 H 0.8570 0.0873 0.1700 0.039 Uiso 1 1 calc R . . B5 B 0.8439(3) 0.3511(5) 0.2479(4) 0.0318(9) Uani 1 1 d . . . H5 H 0.9040 0.4060 0.2146 0.038 Uiso 1 1 calc R . . B6 B 0.7390(3) 0.4499(5) 0.2569(4) 0.0331(9) Uani 1 1 d . . . H6 H 0.7302 0.5697 0.2294 0.040 Uiso 1 1 calc R . . Cl7 Cl 0.61918(7) 0.49520(11) 0.44907(9) 0.0390(2) Uani 1 1 d . . . B7 B 0.6879(3) 0.3789(5) 0.3703(4) 0.0280(8) Uani 1 1 d . . . Cl8 Cl 0.56449(6) 0.09566(11) 0.39869(8) 0.0365(2) Uani 1 1 d . . . B8 B 0.6597(3) 0.1852(5) 0.3439(3) 0.0266(8) Uani 1 1 d . . . Cl9 Cl 0.77996(7) -0.10781(10) 0.37601(9) 0.0405(2) Uani 1 1 d . . . B9 B 0.7657(3) 0.0857(5) 0.3349(4) 0.0299(9) Uani 1 1 d . . . Cl10 Cl 0.97036(6) 0.16145(11) 0.42201(8) 0.0350(2) Uani 1 1 d . . . B10 B 0.8586(3) 0.2174(5) 0.3557(3) 0.0270(8) Uani 1 1 d . . . Cl11 Cl 0.87498(6) 0.53552(10) 0.46390(8) 0.0354(2) Uani 1 1 d . . . B11 B 0.8114(3) 0.3989(5) 0.3780(3) 0.0274(8) Uani 1 1 d . . . Cl12 Cl 0.77476(7) 0.20009(11) 0.57719(7) 0.0340(2) Uani 1 1 d . . . B12 B 0.7627(3) 0.2350(4) 0.4322(3) 0.0249(8) 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 Cs1 0.0399(3) 0.0705(3) 0.0652(3) 0.000 -0.0028(2) 0.000 C1 0.035(2) 0.038(2) 0.0279(19) 0.0035(16) -0.0015(16) -0.0058(17) Cs2 0.0438(3) 0.0356(3) 0.0580(4) 0.0012(2) -0.0021(3) 0.0006(2) B2 0.031(2) 0.032(2) 0.031(2) 0.0024(17) -0.0034(17) -0.0014(17) B3 0.032(2) 0.032(2) 0.033(2) -0.0046(18) 0.0001(18) -0.0038(18) B4 0.033(2) 0.034(2) 0.031(2) -0.0039(18) 0.0027(17) -0.0035(18) B5 0.032(2) 0.032(2) 0.030(2) 0.0038(17) -0.0005(17) -0.0047(17) B6 0.033(2) 0.029(2) 0.035(2) 0.0075(18) -0.0054(18) -0.0028(17) Cl7 0.0326(5) 0.0327(5) 0.0502(6) -0.0108(4) -0.0007(4) 0.0067(4) B7 0.028(2) 0.0222(19) 0.032(2) 0.0014(16) -0.0033(16) 0.0015(15) Cl8 0.0287(5) 0.0353(5) 0.0452(5) 0.0039(4) 0.0037(4) -0.0060(4) B8 0.0250(19) 0.0247(19) 0.029(2) 0.0006(16) -0.0001(16) -0.0023(15) Cl9 0.0441(6) 0.0212(4) 0.0566(6) 0.0012(4) 0.0077(5) 0.0019(4) B9 0.028(2) 0.0222(19) 0.039(2) -0.0019(17) 0.0005(17) -0.0003(16) Cl10 0.0270(4) 0.0346(5) 0.0425(5) 0.0022(4) 0.0001(4) 0.0043(4) B10 0.027(2) 0.0246(19) 0.029(2) -0.0002(16) 0.0013(16) -0.0009(15) Cl11 0.0326(5) 0.0282(5) 0.0434(5) -0.0079(4) -0.0031(4) -0.0035(4) B11 0.029(2) 0.0222(19) 0.030(2) 0.0005(16) -0.0014(16) -0.0005(15) Cl12 0.0347(5) 0.0402(5) 0.0263(4) 0.0061(4) 0.0007(4) 0.0026(4) B12 0.0259(19) 0.0211(18) 0.0276(19) -0.0003(15) 0.0027(16) -0.0003(15) _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 Cs1 Cl12 3.6815(9) 3_756 ? Cs1 Cl12 3.6815(9) 4 ? Cs1 Cl9 3.8372(11) . ? Cs1 Cl9 3.8372(11) 2_755 ? Cs1 Cl10 3.9949(11) . ? Cs1 Cl10 3.9949(11) 2_755 ? Cs1 Cl10 4.0238(10) 3_756 ? Cs1 Cl10 4.0238(10) 4 ? Cs1 Cl11 4.0455(11) 1_545 ? Cs1 Cl11 4.0455(11) 2_745 ? C1 B4 1.693(6) . ? C1 B3 1.696(6) . ? C1 B2 1.704(6) . ? C1 B6 1.707(6) . ? C1 B5 1.708(6) . ? C1 H1 1.1200 . ? Cs2 Cs2 2.3307(13) 2_655 ? Cs2 Cl8 3.5709(11) 2_665 ? Cs2 Cl12 3.6529(11) 4_565 ? Cs2 Cl7 3.6767(11) 2_655 ? Cs2 Cl8 3.8015(12) 4_565 ? Cs2 B6 3.850(5) . ? Cs2 Cl7 3.8904(13) 4_565 ? Cs2 B3 3.953(4) 1_565 ? Cs2 Cl9 3.9700(12) 1_565 ? Cs2 Cl8 3.9702(12) 1_565 ? Cs2 Cl7 3.9833(12) . ? B2 B7 1.775(6) . ? B2 B3 1.777(6) . ? B2 B8 1.779(6) . ? B2 B6 1.782(6) . ? B2 H2 1.1200 . ? B3 B8 1.770(6) . ? B3 B9 1.777(6) . ? B3 B4 1.780(6) . ? B3 Cs2 3.953(4) 1_545 ? B3 H3 1.1200 . ? B4 B9 1.773(6) . ? B4 B10 1.773(6) . ? B4 B5 1.781(6) . ? B4 H4 1.1200 . ? B5 B11 1.773(6) . ? B5 B10 1.774(6) . ? B5 B6 1.776(6) . ? B5 H5 1.1200 . ? B6 B7 1.773(6) . ? B6 B11 1.774(6) . ? B6 H6 1.1200 . ? Cl7 B7 1.800(4) . ? Cl7 Cs2 3.6767(11) 2_655 ? Cl7 Cs2 3.8904(13) 4_566 ? B7 B12 1.788(6) . ? B7 B8 1.791(6) . ? B7 B11 1.795(6) . ? Cl8 B8 1.798(4) . ? Cl8 Cs2 3.5709(11) 2_645 ? Cl8 Cs2 3.8015(12) 4_566 ? Cl8 Cs2 3.9702(12) 1_545 ? B8 B9 1.793(6) . ? B8 B12 1.794(6) . ? Cl9 B9 1.798(4) . ? Cl9 Cs2 3.9700(12) 1_545 ? B9 B10 1.782(6) . ? B9 B12 1.791(6) . ? Cl10 B10 1.797(4) . ? Cl10 Cs1 4.0238(10) 3_756 ? B10 B12 1.782(6) . ? B10 B11 1.788(6) . ? Cl11 B11 1.791(4) . ? Cl11 Cs1 4.0455(11) 1_565 ? B11 B12 1.784(6) . ? Cl12 B12 1.794(4) . ? Cl12 Cs2 3.6529(11) 4_566 ? Cl12 Cs1 3.6815(9) 3_756 ? 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 Cl12 Cs1 Cl12 176.40(3) 3_756 4 ? Cl12 Cs1 Cl9 119.17(2) 3_756 . ? Cl12 Cs1 Cl9 59.82(2) 4 . ? Cl12 Cs1 Cl9 59.82(2) 3_756 2_755 ? Cl12 Cs1 Cl9 119.17(2) 4 2_755 ? Cl9 Cs1 Cl9 151.76(3) . 2_755 ? Cl12 Cs1 Cl10 79.34(2) 3_756 . ? Cl12 Cs1 Cl10 97.62(2) 4 . ? Cl9 Cs1 Cl10 55.55(2) . . ? Cl9 Cs1 Cl10 99.15(2) 2_755 . ? Cl12 Cs1 Cl10 97.62(2) 3_756 2_755 ? Cl12 Cs1 Cl10 79.34(2) 4 2_755 ? Cl9 Cs1 Cl10 99.15(2) . 2_755 ? Cl9 Cs1 Cl10 55.55(2) 2_755 2_755 ? Cl10 Cs1 Cl10 67.06(3) . 2_755 ? Cl12 Cs1 Cl10 55.977(19) 3_756 3_756 ? Cl12 Cs1 Cl10 123.529(19) 4 3_756 ? Cl9 Cs1 Cl10 63.98(2) . 3_756 ? Cl9 Cs1 Cl10 112.52(2) 2_755 3_756 ? Cl10 Cs1 Cl10 51.76(2) . 3_756 ? Cl10 Cs1 Cl10 115.384(17) 2_755 3_756 ? Cl12 Cs1 Cl10 123.529(19) 3_756 4 ? Cl12 Cs1 Cl10 55.977(19) 4 4 ? Cl9 Cs1 Cl10 112.52(2) . 4 ? Cl9 Cs1 Cl10 63.98(2) 2_755 4 ? Cl10 Cs1 Cl10 115.384(17) . 4 ? Cl10 Cs1 Cl10 51.76(2) 2_755 4 ? Cl10 Cs1 Cl10 166.89(3) 3_756 4 ? Cl12 Cs1 Cl11 94.71(2) 3_756 1_545 ? Cl12 Cs1 Cl11 87.28(2) 4 1_545 ? Cl9 Cs1 Cl11 53.83(2) . 1_545 ? Cl9 Cs1 Cl11 149.29(2) 2_755 1_545 ? Cl10 Cs1 Cl11 91.791(19) . 1_545 ? Cl10 Cs1 Cl11 152.85(2) 2_755 1_545 ? Cl10 Cs1 Cl11 54.201(19) 3_756 1_545 ? Cl10 Cs1 Cl11 135.32(2) 4 1_545 ? Cl12 Cs1 Cl11 87.28(2) 3_756 2_745 ? Cl12 Cs1 Cl11 94.71(2) 4 2_745 ? Cl9 Cs1 Cl11 149.29(2) . 2_745 ? Cl9 Cs1 Cl11 53.83(2) 2_755 2_745 ? Cl10 Cs1 Cl11 152.85(2) . 2_745 ? Cl10 Cs1 Cl11 91.791(19) 2_755 2_745 ? Cl10 Cs1 Cl11 135.32(2) 3_756 2_745 ? Cl10 Cs1 Cl11 54.201(19) 4 2_745 ? Cl11 Cs1 Cl11 112.93(3) 1_545 2_745 ? B4 C1 B3 63.3(3) . . ? B4 C1 B2 115.8(3) . . ? B3 C1 B2 63.0(3) . . ? B4 C1 B6 115.3(3) . . ? B3 C1 B6 115.3(3) . . ? B2 C1 B6 63.0(3) . . ? B4 C1 B5 63.2(3) . . ? B3 C1 B5 115.7(3) . . ? B2 C1 B5 115.4(3) . . ? B6 C1 B5 62.7(3) . . ? B4 C1 H1 117.0 . . ? B3 C1 H1 117.1 . . ? B2 C1 H1 117.2 . . ? B6 C1 H1 117.6 . . ? B5 C1 H1 117.3 . . ? Cs2 Cs2 Cl8 81.64(2) 2_655 2_665 ? Cs2 Cs2 Cl12 159.88(4) 2_655 4_565 ? Cl8 Cs2 Cl12 102.43(3) 2_665 4_565 ? Cs2 Cs2 Cl7 79.64(3) 2_655 2_655 ? Cl8 Cs2 Cl7 96.84(3) 2_665 2_655 ? Cl12 Cs2 Cl7 118.86(3) 4_565 2_655 ? Cs2 Cs2 Cl8 136.23(3) 2_655 4_565 ? Cl8 Cs2 Cl8 60.28(3) 2_665 4_565 ? Cl12 Cs2 Cl8 58.74(2) 4_565 4_565 ? Cl7 Cs2 Cl8 84.08(3) 2_655 4_565 ? Cs2 Cs2 B6 111.31(7) 2_655 . ? Cl8 Cs2 B6 164.29(7) 2_665 . ? Cl12 Cs2 B6 62.33(7) 4_565 . ? Cl7 Cs2 B6 94.33(7) 2_655 . ? Cl8 Cs2 B6 110.21(7) 4_565 . ? Cs2 Cs2 Cl7 137.91(2) 2_655 4_565 ? Cl8 Cs2 Cl7 114.59(3) 2_665 4_565 ? Cl12 Cs2 Cl7 58.46(2) 4_565 4_565 ? Cl7 Cs2 Cl7 60.69(3) 2_655 4_565 ? Cl8 Cs2 Cl7 57.09(2) 4_565 4_565 ? B6 Cs2 Cl7 62.12(7) . 4_565 ? Cs2 Cs2 B3 108.98(7) 2_655 1_565 ? Cl8 Cs2 B3 61.36(7) 2_665 1_565 ? Cl12 Cs2 B3 58.36(7) 4_565 1_565 ? Cl7 Cs2 B3 153.76(7) 2_655 1_565 ? Cl8 Cs2 B3 72.60(7) 4_565 1_565 ? B6 Cs2 B3 104.74(9) . 1_565 ? Cl7 Cs2 B3 112.85(7) 4_565 1_565 ? Cs2 Cs2 Cl9 101.10(3) 2_655 1_565 ? Cl8 Cs2 Cl9 104.54(2) 2_665 1_565 ? Cl12 Cs2 Cl9 58.78(2) 4_565 1_565 ? Cl7 Cs2 Cl9 158.51(3) 2_655 1_565 ? Cl8 Cs2 Cl9 108.32(3) 4_565 1_565 ? B6 Cs2 Cl9 65.18(7) . 1_565 ? Cl7 Cs2 Cl9 110.71(3) 4_565 1_565 ? B3 Cs2 Cl9 46.44(7) 1_565 1_565 ? Cs2 Cs2 Cl8 62.86(2) 2_655 1_565 ? Cl8 Cs2 Cl8 61.95(3) 2_665 1_565 ? Cl12 Cs2 Cl8 101.32(2) 4_565 1_565 ? Cl7 Cs2 Cl8 138.33(3) 2_655 1_565 ? Cl8 Cs2 Cl8 110.092(16) 4_565 1_565 ? B6 Cs2 Cl8 115.03(7) . 1_565 ? Cl7 Cs2 Cl8 159.23(3) 4_565 1_565 ? B3 Cs2 Cl8 46.61(7) 1_565 1_565 ? Cl9 Cs2 Cl8 54.88(2) 1_565 1_565 ? Cs2 Cs2 Cl7 65.23(3) 2_655 . ? Cl8 Cs2 Cl7 142.17(3) 2_665 . ? Cl12 Cs2 Cl7 103.15(2) 4_565 . ? Cl7 Cs2 Cl7 94.69(3) 2_655 . ? Cl8 Cs2 Cl7 157.12(3) 4_565 . ? B6 Cs2 Cl7 47.00(7) . . ? Cl7 Cs2 Cl7 102.474(15) 4_565 . ? B3 Cs2 Cl7 111.48(7) 1_565 . ? Cl9 Cs2 Cl7 66.95(2) 1_565 . ? Cl8 Cs2 Cl7 85.96(2) 1_565 . ? C1 B2 B7 104.3(3) . . ? C1 B2 B3 58.3(2) . . ? B7 B2 B3 108.1(3) . . ? C1 B2 B8 104.0(3) . . ? B7 B2 B8 60.5(2) . . ? B3 B2 B8 59.7(2) . . ? C1 B2 B6 58.6(2) . . ? B7 B2 B6 59.8(2) . . ? B3 B2 B6 107.8(3) . . ? B8 B2 B6 108.1(3) . . ? C1 B2 H2 125.3 . . ? B7 B2 H2 122.3 . . ? B3 B2 H2 121.6 . . ? B8 B2 H2 122.4 . . ? B6 B2 H2 121.5 . . ? C1 B3 B8 104.7(3) . . ? C1 B3 B2 58.7(3) . . ? B8 B3 B2 60.2(2) . . ? C1 B3 B9 104.2(3) . . ? B8 B3 B9 60.7(2) . . ? B2 B3 B9 108.6(3) . . ? C1 B3 B4 58.2(2) . . ? B8 B3 B4 108.5(3) . . ? B2 B3 B4 108.0(3) . . ? B9 B3 B4 59.8(2) . . ? C1 B3 Cs2 157.7(3) . 1_545 ? B8 B3 Cs2 94.6(2) . 1_545 ? B2 B3 Cs2 125.7(2) . 1_545 ? B9 B3 Cs2 94.9(2) . 1_545 ? B4 B3 Cs2 125.9(2) . 1_545 ? C1 B3 H3 125.3 . . ? B8 B3 H3 121.9 . . ? B2 B3 H3 121.2 . . ? B9 B3 H3 122.2 . . ? B4 B3 H3 121.6 . . ? Cs2 B3 H3 32.4 1_545 . ? C1 B4 B9 104.5(3) . . ? C1 B4 B10 104.5(3) . . ? B9 B4 B10 60.3(2) . . ? C1 B4 B3 58.4(2) . . ? B9 B4 B3 60.0(2) . . ? B10 B4 B3 108.2(3) . . ? C1 B4 B5 58.8(2) . . ? B9 B4 B5 108.3(3) . . ? B10 B4 B5 59.9(2) . . ? B3 B4 B5 108.1(3) . . ? C1 B4 H4 125.0 . . ? B9 B4 H4 122.2 . . ? B10 B4 H4 122.3 . . ? B3 B4 H4 121.5 . . ? B5 B4 H4 121.3 . . ? C1 B5 B11 104.4(3) . . ? C1 B5 B10 103.8(3) . . ? B11 B5 B10 60.6(2) . . ? C1 B5 B6 58.6(2) . . ? B11 B5 B6 60.0(2) . . ? B10 B5 B6 108.1(3) . . ? C1 B5 B4 58.0(2) . . ? B11 B5 B4 108.3(3) . . ? B10 B5 B4 59.9(2) . . ? B6 B5 B4 107.7(3) . . ? C1 B5 H5 125.5 . . ? B11 B5 H5 122.0 . . ? B10 B5 H5 122.4 . . ? B6 B5 H5 121.5 . . ? B4 B5 H5 121.6 . . ? C1 B6 B7 104.2(3) . . ? C1 B6 B11 104.4(3) . . ? B7 B6 B11 60.8(2) . . ? C1 B6 B5 58.7(2) . . ? B7 B6 B5 108.6(3) . . ? B11 B6 B5 59.9(2) . . ? C1 B6 B2 58.4(2) . . ? B7 B6 B2 59.9(2) . . ? B11 B6 B2 108.7(3) . . ? B5 B6 B2 108.3(3) . . ? C1 B6 Cs2 119.8(2) . . ? B7 B6 Cs2 94.5(2) . . ? B11 B6 Cs2 133.9(3) . . ? B5 B6 Cs2 156.7(3) . . ? B2 B6 Cs2 86.0(2) . . ? C1 B6 H6 125.3 . . ? B7 B6 H6 122.1 . . ? B11 B6 H6 122.0 . . ? B5 B6 H6 121.2 . . ? B2 B6 H6 121.3 . . ? Cs2 B6 H6 37.8 . . ? B7 Cl7 Cs2 120.86(14) . 2_655 ? B7 Cl7 Cs2 106.02(14) . 4_566 ? Cs2 Cl7 Cs2 119.31(3) 2_655 4_566 ? B7 Cl7 Cs2 89.68(14) . . ? Cs2 Cl7 Cs2 35.14(2) 2_655 . ? Cs2 Cl7 Cs2 152.38(3) 4_566 . ? B6 B7 B2 60.3(2) . . ? B6 B7 B12 107.3(3) . . ? B2 B7 B12 107.8(3) . . ? B6 B7 B8 108.0(3) . . ? B2 B7 B8 59.9(2) . . ? B12 B7 B8 60.2(2) . . ? B6 B7 B11 59.6(2) . . ? B2 B7 B11 108.0(3) . . ? B12 B7 B11 59.7(2) . . ? B8 B7 B11 108.1(3) . . ? B6 B7 Cl7 122.1(3) . . ? B2 B7 Cl7 121.4(3) . . ? B12 B7 Cl7 122.1(3) . . ? B8 B7 Cl7 121.3(3) . . ? B11 B7 Cl7 122.2(3) . . ? B8 Cl8 Cs2 129.05(14) . 2_645 ? B8 Cl8 Cs2 108.40(14) . 4_566 ? Cs2 Cl8 Cs2 119.72(3) 2_645 4_566 ? B8 Cl8 Cs2 93.55(14) . 1_545 ? Cs2 Cl8 Cs2 35.51(2) 2_645 1_545 ? Cs2 Cl8 Cs2 150.44(3) 4_566 1_545 ? B3 B8 B2 60.1(2) . . ? B3 B8 B7 107.7(3) . . ? B2 B8 B7 59.6(2) . . ? B3 B8 B9 59.8(2) . . ? B2 B8 B9 107.8(3) . . ? B7 B8 B9 107.8(3) . . ? B3 B8 B12 107.5(3) . . ? B2 B8 B12 107.4(3) . . ? B7 B8 B12 59.8(2) . . ? B9 B8 B12 59.9(2) . . ? B3 B8 Cl8 122.9(3) . . ? B2 B8 Cl8 123.6(3) . . ? B7 B8 Cl8 121.9(3) . . ? B9 B8 Cl8 120.8(3) . . ? B12 B8 Cl8 120.5(3) . . ? B9 Cl9 Cs1 101.13(15) . . ? B9 Cl9 Cs2 93.94(14) . 1_545 ? Cs1 Cl9 Cs2 111.23(3) . 1_545 ? B4 B9 B3 60.2(3) . . ? B4 B9 B10 59.8(2) . . ? B3 B9 B10 107.9(3) . . ? B4 B9 B12 107.5(3) . . ? B3 B9 B12 107.4(3) . . ? B10 B9 B12 59.8(2) . . ? B4 B9 B8 107.8(3) . . ? B3 B9 B8 59.5(2) . . ? B10 B9 B8 108.0(3) . . ? B12 B9 B8 60.1(2) . . ? B4 B9 Cl9 121.9(3) . . ? B3 B9 Cl9 121.8(3) . . ? B10 B9 Cl9 121.9(3) . . ? B12 B9 Cl9 122.2(3) . . ? B8 B9 Cl9 121.7(3) . . ? B10 Cl10 Cs1 98.12(14) . . ? B10 Cl10 Cs1 113.72(14) . 3_756 ? Cs1 Cl10 Cs1 128.24(2) . 3_756 ? B4 B10 B5 60.3(2) . . ? B4 B10 B12 107.9(3) . . ? B5 B10 B12 107.7(3) . . ? B4 B10 B9 59.8(2) . . ? B5 B10 B9 108.2(3) . . ? B12 B10 B9 60.3(2) . . ? B4 B10 B11 108.0(3) . . ? B5 B10 B11 59.7(2) . . ? B12 B10 B11 60.0(2) . . ? B9 B10 B11 108.4(3) . . ? B4 B10 Cl10 122.6(3) . . ? B5 B10 Cl10 122.9(3) . . ? B12 B10 Cl10 120.6(3) . . ? B9 B10 Cl10 120.8(3) . . ? B11 B10 Cl10 121.6(3) . . ? B11 Cl11 Cs1 103.50(14) . 1_565 ? B5 B11 B6 60.1(3) . . ? B5 B11 B12 107.6(3) . . ? B6 B11 B12 107.4(3) . . ? B5 B11 B10 59.7(2) . . ? B6 B11 B10 107.6(3) . . ? B12 B11 B10 59.8(2) . . ? B5 B11 Cl11 121.2(3) . . ? B6 B11 Cl11 122.1(3) . . ? B12 B11 Cl11 122.3(3) . . ? B10 B11 Cl11 121.4(3) . . ? B5 B11 B7 107.7(3) . . ? B6 B11 B7 59.6(2) . . ? B12 B11 B7 59.9(2) . . ? B10 B11 B7 107.7(3) . . ? Cl11 B11 B7 122.7(3) . . ? B12 Cl12 Cs2 111.40(14) . 4_566 ? B12 Cl12 Cs1 122.60(14) . 3_756 ? Cs2 Cl12 Cs1 122.93(3) 4_566 3_756 ? B10 B12 B11 60.2(2) . . ? B10 B12 B7 108.3(3) . . ? B11 B12 B7 60.4(2) . . ? B10 B12 B9 59.8(2) . . ? B11 B12 B9 108.2(3) . . ? B7 B12 B9 108.1(3) . . ? B10 B12 Cl12 121.3(3) . . ? B11 B12 Cl12 121.1(3) . . ? B7 B12 Cl12 121.8(3) . . ? B9 B12 Cl12 121.8(3) . . ? B10 B12 B8 108.0(3) . . ? B11 B12 B8 108.4(3) . . ? B7 B12 B8 60.0(2) . . ? B9 B12 B8 60.0(2) . . ? Cl12 B12 B8 122.0(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max ' 2.089 (1.16 from Cs2)' _refine_diff_density_min -0.893 _refine_diff_density_rms 0.108 #===END data_complex_3a _database_code_depnum_ccdc_archive 'CCDC 248038' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'caesium hexa-bromo-monocarbadodecaborane' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C H6 B11 Br6 Cs' _chemical_formula_weight 749.34 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' B B 0.0013 0.0007 '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' Cs Cs -0.3680 2.1192 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 15.0967(3) _cell_length_b 9.2460(2) _cell_length_c 12.5568(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.1120(10) _cell_angle_gamma 90.00 _cell_volume 1739.24(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.862 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 15.885 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1732 _exptl_absorpt_correction_T_max 0.2516 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 CCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18141 _diffrn_reflns_av_R_equivalents 0.0864 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3414 _reflns_number_gt 2976 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius)' _computing_cell_refinement DENZO _computing_data_reduction 'DENZO, SCALEPACK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour)' _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^)+(0.0445P)^2^+7.4685P] 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 3414 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 Cs1 Cs 0.5000 0.20645(10) 0.7500 0.0549(2) Uani 1 2 d S . . Cs2 Cs -0.06234(5) -0.24524(9) 0.30852(7) 0.0329(2) Uani 0.50 1 d P . . Br7 Br 0.06389(4) 0.09245(7) 0.40134(5) 0.03034(17) Uani 1 1 d . . . Br8 Br 0.28166(4) -0.11001(6) 0.37562(5) 0.02769(16) Uani 1 1 d . . . Br9 Br 0.47254(4) 0.16354(7) 0.41623(5) 0.02735(16) Uani 1 1 d . . . Br10 Br 0.37542(4) 0.53891(6) 0.45901(5) 0.02726(16) Uani 1 1 d . . . Br11 Br 0.11694(4) 0.49584(7) 0.44848(5) 0.02875(17) Uani 1 1 d . . . Br12 Br 0.27754(4) 0.20121(6) 0.58045(5) 0.02433(15) Uani 1 1 d . . . C1 C 0.2400(4) 0.2956(6) 0.1709(5) 0.0245(12) Uani 1 1 d . . . H1 H 0.2324 0.3162 0.0823 0.029 Uiso 1 1 calc R . . B2 B 0.1468(4) 0.3148(7) 0.2350(6) 0.0245(14) Uani 1 1 d . . . H2 H 0.0786 0.3461 0.1965 0.029 Uiso 1 1 calc R . . B3 B 0.1936(4) 0.1413(7) 0.2128(5) 0.0215(13) Uani 1 1 d . . . H3 H 0.1562 0.0597 0.1587 0.026 Uiso 1 1 calc R . . B4 B 0.3107(5) 0.1609(7) 0.2189(5) 0.0235(14) Uani 1 1 d . . . H4 H 0.3501 0.0912 0.1689 0.028 Uiso 1 1 calc R . . B5 B 0.3378(4) 0.3470(7) 0.2431(5) 0.0226(13) Uani 1 1 d . . . H5 H 0.3952 0.3997 0.2095 0.027 Uiso 1 1 calc R . . B6 B 0.2364(5) 0.4426(7) 0.2516(5) 0.0248(14) Uani 1 1 d . . . H6 H 0.2272 0.5571 0.2232 0.030 Uiso 1 1 calc R . . B7 B 0.1631(4) 0.1860(7) 0.3413(5) 0.0208(13) Uani 1 1 d . . . B8 B 0.2650(4) 0.0919(7) 0.3313(5) 0.0209(13) Uani 1 1 d . . . B9 B 0.3540(4) 0.2196(7) 0.3492(5) 0.0205(13) Uani 1 1 d . . . B10 B 0.3078(4) 0.3937(7) 0.3707(6) 0.0232(14) Uani 1 1 d . . . B11 B 0.1892(4) 0.3741(7) 0.3651(5) 0.0214(13) Uani 1 1 d . . . B12 B 0.2625(4) 0.2362(7) 0.4264(5) 0.0208(13) 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 Cs1 0.0321(3) 0.0831(6) 0.0480(4) 0.000 -0.0009(3) 0.000 Cs2 0.0304(4) 0.0333(4) 0.0359(5) -0.0029(3) 0.0068(3) -0.0015(3) Br7 0.0238(3) 0.0341(3) 0.0332(4) 0.0035(3) 0.0038(3) -0.0058(2) Br8 0.0343(3) 0.0185(3) 0.0305(3) 0.0012(2) 0.0047(3) 0.0012(2) Br9 0.0208(3) 0.0301(3) 0.0304(3) 0.0004(2) 0.0004(2) 0.0032(2) Br10 0.0283(3) 0.0231(3) 0.0294(3) -0.0045(2) -0.0005(3) -0.0033(2) Br11 0.0258(3) 0.0278(3) 0.0324(4) -0.0060(2) 0.0024(3) 0.0058(2) Br12 0.0272(3) 0.0286(3) 0.0170(3) 0.0035(2) 0.0019(2) 0.0015(2) C1 0.026(3) 0.029(3) 0.018(3) 0.001(2) 0.001(2) -0.002(2) B2 0.024(3) 0.027(3) 0.021(3) 0.003(3) -0.002(3) 0.004(3) B3 0.022(3) 0.024(3) 0.018(3) 0.000(2) 0.002(3) 0.002(3) B4 0.031(4) 0.027(3) 0.013(3) -0.002(2) 0.004(3) -0.003(3) B5 0.026(3) 0.028(3) 0.014(3) 0.002(3) 0.003(3) -0.004(3) B6 0.029(4) 0.024(3) 0.020(3) 0.002(3) -0.001(3) 0.001(3) B7 0.019(3) 0.022(3) 0.020(3) 0.001(2) 0.000(3) 0.002(2) B8 0.022(3) 0.022(3) 0.019(3) -0.002(2) 0.004(3) 0.000(2) B9 0.022(3) 0.023(3) 0.017(3) 0.003(2) 0.006(3) 0.003(2) B10 0.024(3) 0.020(3) 0.025(4) -0.001(3) 0.000(3) 0.001(2) B11 0.025(3) 0.020(3) 0.020(3) 0.001(2) 0.003(3) -0.001(2) B12 0.022(3) 0.023(3) 0.018(3) -0.003(2) 0.006(3) 0.000(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 Cs1 Br12 3.7475(6) . ? Cs1 Br12 3.7475(6) 2_656 ? Cs1 Br8 3.9288(6) 3_656 ? Cs1 Br8 3.9288(6) 4_556 ? Cs1 Br9 4.0553(10) 3_656 ? Cs1 Br9 4.0553(10) 4_556 ? Cs1 Br10 4.1461(8) 3_666 ? Cs1 Br10 4.1461(8) 4_566 ? Cs1 Br9 4.1791(6) . ? Cs1 Br9 4.1791(6) 2_656 ? Cs2 Cs2 2.5274(16) 2 ? Cs2 Br12 3.7129(10) 3_556 ? Cs2 Br7 3.7668(10) . ? Cs2 Br11 3.8688(10) 1_545 ? Cs2 Br7 3.9103(11) 3_556 ? Cs2 B6 3.913(7) 2_545 ? Cs2 Br8 3.9971(10) 2 ? Cs2 Br11 3.9976(11) 3_556 ? Cs2 Br11 4.0207(11) 2_545 ? Cs2 Br7 4.0839(11) 2 ? Br7 B7 1.959(7) . ? Br7 Cs2 3.9103(11) 3_556 ? Br7 Cs2 4.0839(11) 2 ? Br8 B8 1.955(6) . ? Br8 Cs1 3.9288(6) 3_656 ? Br8 Cs2 3.9971(10) 2 ? Br9 B9 1.951(6) . ? Br9 Cs1 4.0553(10) 3_656 ? Br10 B10 1.948(7) . ? Br10 Cs1 4.1461(8) 3_666 ? Br11 B11 1.959(7) . ? Br11 Cs2 3.8688(10) 1_565 ? Br11 Cs2 3.9976(11) 3_556 ? Br11 Cs2 4.0207(11) 2_565 ? Br12 B12 1.947(7) . ? Br12 Cs2 3.7129(10) 3_556 ? C1 B6 1.700(9) . ? C1 B3 1.700(9) . ? C1 B4 1.702(9) . ? C1 B5 1.703(9) . ? C1 B2 1.714(9) . ? B2 B11 1.767(9) . ? B2 B7 1.782(9) . ? B2 B3 1.788(9) . ? B2 B6 1.789(9) . ? B3 B4 1.769(9) . ? B3 B7 1.782(9) . ? B3 B8 1.786(9) . ? B4 B8 1.765(9) . ? B4 B9 1.771(9) . ? B4 B5 1.786(9) . ? B5 B10 1.771(9) . ? B5 B9 1.772(9) . ? B5 B6 1.783(9) . ? B6 B11 1.787(9) . ? B6 B10 1.790(9) . ? B6 Cs2 3.913(7) 2_565 ? B7 B8 1.786(9) . ? B7 B12 1.793(9) . ? B7 B11 1.800(9) . ? B8 B9 1.782(9) . ? B8 B12 1.794(9) . ? B9 B10 1.787(9) . ? B9 B12 1.789(9) . ? B10 B12 1.787(9) . ? B10 B11 1.792(9) . ? B11 B12 1.797(9) . ? 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 Br12 Cs1 Br12 178.52(3) . 2_656 ? Br12 Cs1 Br8 120.423(14) . 3_656 ? Br12 Cs1 Br8 59.186(13) 2_656 3_656 ? Br12 Cs1 Br8 59.186(13) . 4_556 ? Br12 Cs1 Br8 120.423(14) 2_656 4_556 ? Br8 Cs1 Br8 153.76(3) 3_656 4_556 ? Br12 Cs1 Br9 80.690(16) . 3_656 ? Br12 Cs1 Br9 98.047(18) 2_656 3_656 ? Br8 Cs1 Br9 57.152(14) 3_656 3_656 ? Br8 Cs1 Br9 99.18(2) 4_556 3_656 ? Br12 Cs1 Br9 98.047(18) . 4_556 ? Br12 Cs1 Br9 80.690(16) 2_656 4_556 ? Br8 Cs1 Br9 99.18(2) 3_656 4_556 ? Br8 Cs1 Br9 57.152(14) 4_556 4_556 ? Br9 Cs1 Br9 64.96(2) 3_656 4_556 ? Br12 Cs1 Br10 95.311(15) . 3_666 ? Br12 Cs1 Br10 85.533(14) 2_656 3_666 ? Br8 Cs1 Br10 53.550(12) 3_656 3_666 ? Br8 Cs1 Br10 148.417(19) 4_556 3_666 ? Br9 Cs1 Br10 94.010(13) 3_656 3_666 ? Br9 Cs1 Br10 152.638(18) 4_556 3_666 ? Br12 Cs1 Br10 85.533(14) . 4_566 ? Br12 Cs1 Br10 95.311(15) 2_656 4_566 ? Br8 Cs1 Br10 148.42(2) 3_656 4_566 ? Br8 Cs1 Br10 53.550(12) 4_556 4_566 ? Br9 Cs1 Br10 152.638(18) 3_656 4_566 ? Br9 Cs1 Br10 94.010(13) 4_556 4_566 ? Br10 Cs1 Br10 110.80(3) 3_666 4_566 ? Br12 Cs1 Br9 57.205(12) . . ? Br12 Cs1 Br9 122.628(12) 2_656 . ? Br8 Cs1 Br9 63.883(12) 3_656 . ? Br8 Cs1 Br9 113.398(14) 4_556 . ? Br9 Cs1 Br9 53.665(16) 3_656 . ? Br9 Cs1 Br9 115.62(2) 4_556 . ? Br10 Cs1 Br9 54.236(12) 3_666 . ? Br10 Cs1 Br9 133.811(18) 4_566 . ? Br12 Cs1 Br9 122.628(12) . 2_656 ? Br12 Cs1 Br9 57.205(12) 2_656 2_656 ? Br8 Cs1 Br9 113.398(14) 3_656 2_656 ? Br8 Cs1 Br9 63.883(12) 4_556 2_656 ? Br9 Cs1 Br9 115.62(2) 3_656 2_656 ? Br9 Cs1 Br9 53.665(16) 4_556 2_656 ? Br10 Cs1 Br9 133.811(18) 3_666 2_656 ? Br10 Cs1 Br9 54.236(12) 4_566 2_656 ? Br9 Cs1 Br9 169.10(3) . 2_656 ? Cs2 Cs2 Br12 165.38(5) 2 3_556 ? Cs2 Cs2 Br7 78.19(2) 2 . ? Br12 Cs2 Br7 103.04(2) 3_556 . ? Cs2 Cs2 Br11 74.61(3) 2 1_545 ? Br12 Cs2 Br11 119.52(3) 3_556 1_545 ? Br7 Cs2 Br11 94.23(2) . 1_545 ? Cs2 Cs2 Br7 129.24(4) 2 3_556 ? Br12 Cs2 Br7 60.269(17) 3_556 3_556 ? Br7 Cs2 Br7 58.22(2) . 3_556 ? Br11 Cs2 Br7 83.39(2) 1_545 3_556 ? Cs2 Cs2 B6 114.74(11) 2 2_545 ? Br12 Cs2 B6 63.60(10) 3_556 2_545 ? Br7 Cs2 B6 166.64(11) . 2_545 ? Br11 Cs2 B6 92.67(10) 1_545 2_545 ? Br7 Cs2 B6 111.39(10) 3_556 2_545 ? Cs2 Cs2 Br8 106.67(4) 2 2 ? Br12 Cs2 Br8 58.819(17) 3_556 2 ? Br7 Cs2 Br8 105.71(2) . 2 ? Br11 Cs2 Br8 159.91(3) 1_545 2 ? Br7 Cs2 Br8 109.02(2) 3_556 2 ? B6 Cs2 Br8 68.33(10) 2_545 2 ? Cs2 Cs2 Br11 133.05(3) 2 3_556 ? Br12 Cs2 Br11 60.280(17) 3_556 3_556 ? Br7 Cs2 Br11 112.86(3) . 3_556 ? Br11 Cs2 Br11 59.56(2) 1_545 3_556 ? Br7 Cs2 Br11 58.176(17) 3_556 3_556 ? B6 Cs2 Br11 61.49(10) 2_545 3_556 ? Br8 Cs2 Br11 112.86(2) 2 3_556 ? Cs2 Cs2 Br11 68.08(3) 2 2_545 ? Br12 Cs2 Br11 105.35(2) 3_556 2_545 ? Br7 Cs2 Br11 141.95(3) . 2_545 ? Br11 Cs2 Br11 93.36(2) 1_545 2_545 ? Br7 Cs2 Br11 159.82(3) 3_556 2_545 ? B6 Cs2 Br11 48.71(10) 2_545 2_545 ? Br8 Cs2 Br11 69.459(18) 2 2_545 ? Br11 Cs2 Br11 103.083(19) 3_556 2_545 ? Cs2 Cs2 Br7 64.53(2) 2 2 ? Br12 Cs2 Br7 102.89(2) 3_556 2 ? Br7 Cs2 Br7 61.85(2) . 2 ? Br11 Cs2 Br7 135.56(2) 1_545 2 ? Br7 Cs2 Br7 108.95(2) 3_556 2 ? B6 Cs2 Br7 119.30(10) 2_545 2 ? Br8 Cs2 Br7 56.593(17) 2 2 ? Br11 Cs2 Br7 161.87(3) 3_556 2 ? Br11 Cs2 Br7 87.31(2) 2_545 2 ? B7 Br7 Cs2 128.94(19) . . ? B7 Br7 Cs2 107.0(2) . 3_556 ? Cs2 Br7 Cs2 121.78(2) . 3_556 ? B7 Br7 Cs2 91.89(19) . 2 ? Cs2 Br7 Cs2 37.28(2) . 2 ? Cs2 Br7 Cs2 151.31(2) 3_556 2 ? B8 Br8 Cs1 100.78(19) . 3_656 ? B8 Br8 Cs2 93.78(19) . 2 ? Cs1 Br8 Cs2 111.89(2) 3_656 2 ? B9 Br9 Cs1 98.57(19) . 3_656 ? B9 Br9 Cs1 112.27(19) . . ? Cs1 Br9 Cs1 126.335(16) 3_656 . ? B10 Br10 Cs1 106.1(2) . 3_666 ? B11 Br11 Cs2 121.2(2) . 1_565 ? B11 Br11 Cs2 104.84(19) . 3_556 ? Cs2 Br11 Cs2 120.44(2) 1_565 3_556 ? B11 Br11 Cs2 89.17(19) . 2_565 ? Cs2 Br11 Cs2 37.31(2) 1_565 2_565 ? Cs2 Br11 Cs2 156.43(3) 3_556 2_565 ? B12 Br12 Cs2 110.82(19) . 3_556 ? B12 Br12 Cs1 123.24(19) . . ? Cs2 Br12 Cs1 123.33(2) 3_556 . ? B6 C1 B3 116.2(5) . . ? B6 C1 B4 116.0(5) . . ? B3 C1 B4 62.7(4) . . ? B6 C1 B5 63.2(4) . . ? B3 C1 B5 115.6(5) . . ? B4 C1 B5 63.3(4) . . ? B6 C1 B2 63.2(4) . . ? B3 C1 B2 63.2(4) . . ? B4 C1 B2 115.1(5) . . ? B5 C1 B2 115.4(5) . . ? C1 B2 B11 104.0(5) . . ? C1 B2 B7 103.8(4) . . ? B11 B2 B7 61.0(4) . . ? C1 B2 B3 58.0(4) . . ? B11 B2 B3 108.5(5) . . ? B7 B2 B3 59.9(4) . . ? C1 B2 B6 58.0(4) . . ? B11 B2 B6 60.3(4) . . ? B7 B2 B6 108.8(5) . . ? B3 B2 B6 107.6(5) . . ? C1 B3 B4 58.7(4) . . ? C1 B3 B7 104.4(5) . . ? B4 B3 B7 107.8(5) . . ? C1 B3 B8 104.1(4) . . ? B4 B3 B8 59.6(4) . . ? B7 B3 B8 60.1(4) . . ? C1 B3 B2 58.8(4) . . ? B4 B3 B2 108.3(5) . . ? B7 B3 B2 59.9(4) . . ? B8 B3 B2 108.0(5) . . ? C1 B4 B8 104.9(5) . . ? C1 B4 B3 58.6(4) . . ? B8 B4 B3 60.7(4) . . ? C1 B4 B9 104.3(5) . . ? B8 B4 B9 60.5(4) . . ? B3 B4 B9 108.9(5) . . ? C1 B4 B5 58.4(4) . . ? B8 B4 B5 108.4(5) . . ? B3 B4 B5 108.2(5) . . ? B9 B4 B5 59.8(4) . . ? C1 B5 B10 104.3(5) . . ? C1 B5 B9 104.2(4) . . ? B10 B5 B9 60.6(4) . . ? C1 B5 B6 58.3(4) . . ? B10 B5 B6 60.5(4) . . ? B9 B5 B6 108.9(5) . . ? C1 B5 B4 58.3(4) . . ? B10 B5 B4 108.1(5) . . ? B9 B5 B4 59.7(4) . . ? B6 B5 B4 107.9(5) . . ? C1 B6 B5 58.5(4) . . ? C1 B6 B11 103.7(5) . . ? B5 B6 B11 107.6(5) . . ? C1 B6 B2 58.8(4) . . ? B5 B6 B2 108.0(5) . . ? B11 B6 B2 59.2(4) . . ? C1 B6 B10 103.6(5) . . ? B5 B6 B10 59.4(4) . . ? B11 B6 B10 60.1(4) . . ? B2 B6 B10 107.4(5) . . ? C1 B6 Cs2 123.0(4) . 2_565 ? B5 B6 Cs2 156.3(4) . 2_565 ? B11 B6 Cs2 95.2(3) . 2_565 ? B2 B6 Cs2 89.1(3) . 2_565 ? B10 B6 Cs2 131.9(4) . 2_565 ? B3 B7 B2 60.2(4) . . ? B3 B7 B8 60.1(4) . . ? B2 B7 B8 108.2(5) . . ? B3 B7 B12 107.9(4) . . ? B2 B7 B12 107.5(5) . . ? B8 B7 B12 60.2(4) . . ? B3 B7 B11 107.4(5) . . ? B2 B7 B11 59.1(4) . . ? B8 B7 B11 108.0(4) . . ? B12 B7 B11 60.0(4) . . ? B3 B7 Br7 122.8(4) . . ? B2 B7 Br7 122.8(4) . . ? B8 B7 Br7 121.2(4) . . ? B12 B7 Br7 120.6(4) . . ? B11 B7 Br7 121.7(4) . . ? B4 B8 B9 59.9(4) . . ? B4 B8 B3 59.8(4) . . ? B9 B8 B3 107.7(5) . . ? B4 B8 B7 107.8(5) . . ? B9 B8 B7 108.1(4) . . ? B3 B8 B7 59.8(4) . . ? B4 B8 B12 107.8(4) . . ? B9 B8 B12 60.0(3) . . ? B3 B8 B12 107.7(4) . . ? B7 B8 B12 60.1(4) . . ? B4 B8 Br8 121.6(4) . . ? B9 B8 Br8 121.9(4) . . ? B3 B8 Br8 121.6(4) . . ? B7 B8 Br8 121.8(4) . . ? B12 B8 Br8 122.2(4) . . ? B4 B9 B5 60.5(4) . . ? B4 B9 B8 59.6(4) . . ? B5 B9 B8 108.3(5) . . ? B4 B9 B10 108.0(5) . . ? B5 B9 B10 59.7(4) . . ? B8 B9 B10 108.3(4) . . ? B4 B9 B12 107.8(5) . . ? B5 B9 B12 107.8(4) . . ? B8 B9 B12 60.3(4) . . ? B10 B9 B12 60.0(4) . . ? B4 B9 Br9 122.1(4) . . ? B5 B9 Br9 122.3(4) . . ? B8 B9 Br9 121.0(4) . . ? B10 B9 Br9 121.9(4) . . ? B12 B9 Br9 121.2(4) . . ? B5 B10 B12 108.0(4) . . ? B5 B10 B9 59.7(4) . . ? B12 B10 B9 60.1(3) . . ? B5 B10 B6 60.1(4) . . ? B12 B10 B6 108.2(5) . . ? B9 B10 B6 107.9(5) . . ? B5 B10 B11 107.8(5) . . ? B12 B10 B11 60.3(4) . . ? B9 B10 B11 108.0(4) . . ? B6 B10 B11 59.8(4) . . ? B5 B10 Br10 120.5(4) . . ? B12 B10 Br10 122.5(4) . . ? B9 B10 Br10 121.3(4) . . ? B6 B10 Br10 121.4(4) . . ? B11 B10 Br10 122.8(4) . . ? B2 B11 B6 60.5(4) . . ? B2 B11 B10 108.3(5) . . ? B6 B11 B10 60.0(4) . . ? B2 B11 B12 108.0(5) . . ? B6 B11 B12 107.9(5) . . ? B10 B11 B12 59.7(4) . . ? B2 B11 B7 59.9(4) . . ? B6 B11 B7 108.1(5) . . ? B10 B11 B7 107.5(4) . . ? B12 B11 B7 59.8(4) . . ? B2 B11 Br11 120.7(4) . . ? B6 B11 Br11 121.8(4) . . ? B10 B11 Br11 122.8(4) . . ? B12 B11 Br11 122.2(4) . . ? B7 B11 Br11 121.2(4) . . ? B10 B12 B9 60.0(4) . . ? B10 B12 B7 108.1(5) . . ? B9 B12 B7 107.5(4) . . ? B10 B12 B8 107.8(4) . . ? B9 B12 B8 59.6(4) . . ? B7 B12 B8 59.7(4) . . ? B10 B12 B11 60.0(4) . . ? B9 B12 B11 107.8(4) . . ? B7 B12 B11 60.2(4) . . ? B8 B12 B11 107.8(4) . . ? B10 B12 Br12 121.4(4) . . ? B9 B12 Br12 121.4(4) . . ? B7 B12 Br12 122.3(4) . . ? B8 B12 Br12 121.9(4) . . ? B11 B12 Br12 122.2(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max '1.677 (0.84 A from Cs1)' _refine_diff_density_min -1.937 _refine_diff_density_rms 0.205