# 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 _publ_contact_author_name 'Molcanov, Kresimir' _publ_contact_author_email kmolcano@irb.hr _publ_section_title ; Stabilisation of tetrabromo- and tetrachlorosemiquinone (bromanil and chloranil) anion radicals in crystals ; loop_ _publ_author_name K.Molcanov B.Kojic-Prodic D.Babic D.Zilic B.Rakvin #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-05-18 at 16:29:05 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\program files\wingx\files\cifdoc.dat # CIF files read : br4q-1 br4q-1-teh struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_Br4Q _database_code_depnum_ccdc_archive 'CCDC 815385' _audit_creation_date 2009-05-18T16:29:05-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C6 Br4 O2' _chemical_formula_sum 'C6 Br4 O2' _chemical_formula_weight 423.68 #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.0589(3) _cell_length_b 6.1970(2) _cell_length_c 8.6426(3) _cell_angle_alpha 90 _cell_angle_beta 105.932(3) _cell_angle_gamma 90 _cell_volume 466.54(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1403 _cell_measurement_theta_min 5.0653 _cell_measurement_theta_max 75.9014 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'dark yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 3.016 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 20.726 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1670 _exptl_absorpt_correction_T_max 0.4360 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54179 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_measurement_device_type 'Oxford Xcalibur Nova' _diffrn_measurement_method ; CCD detector ; _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4323 _diffrn_radiation_probe x-ray _diffrn_reflns_number 2308 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 5.08 _diffrn_reflns_theta_max 75.00 _diffrn_reflns_theta_full 75.93 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measured_fraction_theta_full 0.991 _reflns_number_total 954 _reflns_number_gt 867 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.0495P)^2^+0.6025P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 954 _refine_ls_number_parameters 55 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0949 _refine_ls_goodness_of_fit_ref 1.09 _refine_ls_restrained_S_all 1.09 _refine_ls_shift/su_max 0 _refine_diff_density_max 0.606 _refine_diff_density_min -0.475 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.018 0.009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.676 1.281 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.049 0.032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly C1 C -0.1471(4) 0.0877(7) 0.9200(4) 0.0454(8) Uani 1 d . . . C2 C -0.0041(4) 0.1950(7) 0.9077(5) 0.0448(9) Uani 1 d . . . C3 C 0.1426(4) 0.0904(7) 0.9939(4) 0.0450(8) Uani 1 d . . . Br1 Br 0.31973(6) 0.22629(10) 0.96780(7) 0.0666(2) Uani 1 d . . . Br2 Br -0.33039(6) 0.22159(10) 0.80313(6) 0.0648(2) Uani 1 d . . . O1 O -0.0067(4) 0.3611(6) 0.8341(4) 0.0681(9) Uani 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 C1 0.0463(18) 0.052(2) 0.0357(16) -0.0007(15) 0.0085(14) 0.0064(16) C2 0.055(2) 0.044(2) 0.0358(16) 0.0021(14) 0.0126(15) 0.0028(16) C3 0.0466(18) 0.050(2) 0.0385(16) -0.0032(16) 0.0126(14) -0.0012(16) Br1 0.0542(3) 0.0767(4) 0.0706(4) -0.0013(2) 0.0200(3) -0.0185(2) Br2 0.0531(3) 0.0761(4) 0.0602(3) 0.0076(2) 0.0075(2) 0.0211(2) O1 0.078(2) 0.061(2) 0.0664(18) 0.0256(17) 0.0209(16) 0.0039(16) #------------------ MOLECULAR GEOMETRY --------------------------------------# _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 C1 C3 1.326(6) 3_557 ? C2 C1 1.485(6) . ? C2 C3 1.483(5) . ? C2 O1 1.207(6) . ? C3 C1 1.326(6) 3_557 ? Br1 C3 1.879(4) . ? Br2 C1 1.883(4) . ? 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 C1 C3 C2 122.1(4) 3_557 . ? C1 C3 Br1 123.0(3) 3_557 . ? C2 C1 Br2 115.0(3) . . ? C2 C3 Br1 114.9(3) . . ? C3 C1 C2 121.3(3) 3_557 . ? C3 C2 C1 116.6(4) . . ? C3 C1 Br2 123.7(3) 3_557 . ? O1 C2 C1 121.9(4) . . ? O1 C2 C3 121.5(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 C1 -1.1(6) . . . 3_557 ? C1 C2 C3 Br1 177.7(3) . . . . ? C3 C2 C1 C3 1.1(6) . . . 3_557 ? C3 C2 C1 Br2 -178.1(3) . . . . ? O1 C2 C1 C3 -177.5(4) . . . 3_557 ? O1 C2 C1 Br2 3.3(6) . . . . ? O1 C2 C3 C1 177.5(4) . . . 3_557 ? O1 C2 C3 Br1 -3.7(6) . . . . ? #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-04-18 at 13:52:50 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\program files\wingx\files\cifdoc.dat # CIF files read : new kbr4q-1-teh struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_KBr4QxMe2CO _database_code_depnum_ccdc_archive 'CCDC 815386' _audit_creation_date 2011-04-18T13:52:50-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C9 Br4 K1 O3 H6' _chemical_formula_sum 'C9 Br4 K1 O3 H6' _chemical_formula_weight 520.86 #------------------ UNIT CELL INFORMATION -----------------------------------# _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 7.5940(2) _cell_length_b 10.6229(4) _cell_length_c 16.9280(5) _cell_angle_alpha 91.426(3) _cell_angle_beta 91.085(3) _cell_angle_gamma 100.728(3) _cell_volume 1340.92(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9366 _cell_measurement_theta_min 2.6077 _cell_measurement_theta_max 76.1102 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 2.58 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 17.399 _exptl_absorpt_correction_T_min 0.1570 _exptl_absorpt_correction_T_max 0.8400 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54179 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_measurement_device_type 'Oxford Xcalibur Nova' _diffrn_measurement_method ; CCD detector ; _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4323 _diffrn_reflns_number 13053 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 76.34 _diffrn_reflns_theta_full 76.34 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measured_fraction_theta_full 0.975 _reflns_number_total 5485 _reflns_number_gt 4898 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.1036P)^2^+66.5373P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5485 _refine_ls_number_parameters 305 _refine_ls_number_restraints 18 _refine_ls_R_factor_gt 0.0787 _refine_ls_wR_factor_ref 0.233 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0 _refine_diff_density_max 4.776 _refine_diff_density_min -1.423 _refine_special_details ; Due to extremely small size of the crystals (which are also unstable) data quality was relatively poor, resulting with high R factor and residual electron density. Anisotropic displacement ellipsoids of atoms C3B, C4B and O2B were restrained (using the command ISOR in SHELXL) to prevent unrealistic elongation. ; #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly C1A C 0.6759(16) 0.4138(12) 0.0719(8) 0.018(2) Uani 1 d . . . C1B C 0.7667(16) 0.4166(13) 0.4286(7) 0.016(2) Uani 1 d . . . C2A C 0.7954(16) 0.5371(13) 0.0585(7) 0.017(2) Uani 1 d . . . C2B C 0.7168(15) 0.5419(12) 0.4403(7) 0.016(2) Uani 1 d . . . C3A C 0.8105(17) 0.5885(11) -0.0138(7) 0.016(2) Uani 1 d . . . C3B C 0.7336(16) 0.6078(12) 0.5126(7) 0.016(2) Uani 1 d U . . C4A C 0.7118(16) 0.5311(12) -0.0835(7) 0.016(2) Uani 1 d . . . C4B C 0.8034(16) 0.5535(13) 0.5833(8) 0.019(2) Uani 1 d U . . C5A C 0.6083(16) 0.4037(12) -0.0690(8) 0.019(3) Uani 1 d . . . C5B C 0.8384(17) 0.4222(14) 0.5704(7) 0.021(3) Uani 1 d . . . C6A C 0.5918(16) 0.3510(12) 0.0017(8) 0.017(2) Uani 1 d . . . C6B C 0.8202(16) 0.3626(12) 0.4992(8) 0.018(2) Uani 1 d . . . C7A C 1.1030(19) 0.0295(13) 0.1696(9) 0.024(3) Uani 1 d . . . C7B C 0.647(2) 0.0227(13) 0.3125(8) 0.024(3) Uani 1 d . . . C8A C 1.241(2) -0.0491(15) 0.1516(10) 0.033(3) Uani 1 d . . . C8B C 0.806(2) -0.0350(14) 0.3316(11) 0.032(3) Uani 1 d . . . C9A C 0.9193(18) -0.0155(13) 0.1329(8) 0.023(3) Uani 1 d . . . C9B C 0.477(2) -0.0338(15) 0.3533(9) 0.032(3) Uani 1 d . . . Br1A Br 0.93438(17) 0.60974(13) 0.14703(8) 0.0194(3) Uani 1 d . . . Br1B Br 0.61396(18) 0.60616(13) 0.35107(8) 0.0211(3) Uani 1 d . . . Br2A Br 0.97840(17) 0.73993(12) -0.03145(8) 0.0192(3) Uani 1 d . . . Br2B Br 0.65885(18) 0.76412(13) 0.52876(8) 0.0226(3) Uani 1 d . . . Br3A Br 0.51249(18) 0.31200(13) -0.16391(8) 0.0203(3) Uani 1 d . . . Br3B Br 0.89070(18) 0.34578(14) 0.66456(8) 0.0225(3) Uani 1 d . . . Br4A Br 0.47680(18) 0.17819(13) 0.01554(8) 0.0212(3) Uani 1 d . . . Br4B Br 0.84703(18) 0.18919(13) 0.48780(8) 0.0214(3) Uani 1 d . . . O1A O 0.6630(12) 0.3661(9) 0.1403(5) 0.0196(18) Uani 1 d . . . O1B O 0.7500(12) 0.3608(9) 0.3620(5) 0.0172(17) Uani 1 d . . . O2A O 0.7277(13) 0.5797(9) -0.1510(5) 0.0208(19) Uani 1 d . . . O2B O 0.8187(12) 0.6129(10) 0.6477(6) 0.0240(18) Uani 1 d U . . O3A O 1.1363(13) 0.1263(9) 0.2128(6) 0.023(2) Uani 1 d . . . O3B O 0.6535(13) 0.1120(10) 0.2696(6) 0.026(2) Uani 1 d . . . K1A K 0.9444(3) 0.3239(2) 0.23472(15) 0.0163(5) Uani 1 d . . . K1B K 0.4436(3) 0.3086(3) 0.26085(15) 0.0168(5) Uani 1 d . . . H8A H 1.2017 -0.1347 0.1694 0.049 Uiso 1 calc R . . H8B H 1.2586 -0.0516 0.0956 0.049 Uiso 1 calc R . . H8C H 1.352 -0.0118 0.1782 0.049 Uiso 1 calc R . . H8D H 0.907 0.0068 0.3027 0.048 Uiso 1 calc R . . H8E H 0.7807 -0.1247 0.3172 0.048 Uiso 1 calc R . . H8F H 0.8333 -0.0246 0.3873 0.048 Uiso 1 calc R . . H9A H 0.9274 -0.0168 0.0764 0.035 Uiso 1 calc R . . H9B H 0.8716 -0.1002 0.1501 0.035 Uiso 1 calc R . . H9C H 0.8418 0.0418 0.1489 0.035 Uiso 1 calc R . . H9D H 0.4452 -0.1235 0.3395 0.048 Uiso 1 calc R . . H9E H 0.496 -0.023 0.4095 0.048 Uiso 1 calc R . . H9F H 0.3827 0.0089 0.3368 0.048 Uiso 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 C1A 0.014(5) 0.018(6) 0.022(7) 0.003(5) -0.005(5) 0.004(4) C1B 0.013(5) 0.026(6) 0.009(6) -0.003(5) -0.003(4) 0.000(5) C2A 0.012(5) 0.026(6) 0.014(6) -0.003(5) -0.001(4) 0.006(5) C2B 0.009(5) 0.025(6) 0.013(6) 0.000(5) 0.003(4) 0.000(4) C3A 0.021(6) 0.016(6) 0.012(6) 0.004(4) -0.001(5) 0.007(5) C3B 0.012(5) 0.023(6) 0.010(5) -0.004(4) -0.006(4) -0.001(4) C4A 0.012(5) 0.024(6) 0.012(6) 0.001(5) 0.002(4) 0.002(5) C4B 0.011(5) 0.024(6) 0.02 -0.004(5) -0.003(5) 0.000(5) C5A 0.013(5) 0.013(6) 0.031(7) 0.003(5) 0.007(5) 0.004(4) C5B 0.017(6) 0.035(7) 0.009(6) 0.001(5) -0.002(5) -0.004(5) C6A 0.013(5) 0.018(6) 0.021(6) 0.005(5) 0.006(5) 0.002(4) C6B 0.013(5) 0.018(6) 0.021(6) 0.000(5) 0.003(5) -0.001(4) C7A 0.023(7) 0.016(6) 0.031(8) 0.002(5) 0.007(6) -0.001(5) C7B 0.032(7) 0.020(6) 0.019(7) 0.000(5) 0.002(5) 0.005(5) C8A 0.035(8) 0.028(8) 0.036(9) -0.008(6) -0.002(7) 0.008(6) C8B 0.024(7) 0.022(7) 0.052(10) 0.004(6) 0.015(7) 0.008(6) C9A 0.021(6) 0.022(6) 0.024(7) -0.012(5) 0.002(5) -0.003(5) C9B 0.038(8) 0.029(8) 0.027(8) 0.004(6) 0.007(6) -0.004(6) Br1A 0.0200(6) 0.0252(7) 0.0127(6) -0.0038(5) -0.0052(5) 0.0044(5) Br1B 0.0200(6) 0.0259(7) 0.0168(7) 0.0036(5) -0.0040(5) 0.0030(5) Br2A 0.0187(6) 0.0201(6) 0.0182(6) 0.0013(5) 0.0006(5) 0.0015(5) Br2B 0.0214(7) 0.0240(7) 0.0227(7) -0.0032(5) 0.0010(5) 0.0058(5) Br3A 0.0222(6) 0.0254(7) 0.0132(6) -0.0051(5) -0.0044(5) 0.0051(5) Br3B 0.0207(6) 0.0331(7) 0.0128(6) 0.0041(5) -0.0036(5) 0.0023(5) Br4A 0.0206(6) 0.0195(6) 0.0229(7) 0.0013(5) -0.0003(5) 0.0016(5) Br4B 0.0204(6) 0.0224(7) 0.0209(7) -0.0009(5) -0.0015(5) 0.0030(5) O1A 0.018(4) 0.028(5) 0.013(4) 0.004(4) -0.003(3) 0.007(4) O1B 0.018(4) 0.025(4) 0.007(4) -0.003(3) -0.006(3) 0.001(3) O2A 0.025(5) 0.021(4) 0.016(4) 0.003(3) -0.002(4) 0.004(4) O2B 0.019(4) 0.030(5) 0.02 -0.010(4) -0.010(4) 0.001(4) O3A 0.022(5) 0.020(5) 0.025(5) -0.003(4) -0.002(4) 0.001(4) O3B 0.027(5) 0.026(5) 0.026(5) -0.001(4) -0.001(4) 0.006(4) K1A 0.0166(12) 0.0213(12) 0.0106(12) -0.0020(9) -0.0017(9) 0.0034(9) K1B 0.0172(12) 0.0226(13) 0.0101(11) 0.0001(9) 0.0001(9) 0.0029(10) #------------------ MOLECULAR GEOMETRY --------------------------------------# _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 C1A C2A 1.474(18) . ? C1A C6A 1.427(18) . ? C1B C6B 1.423(18) . ? C2A C3A 1.351(17) . ? C2A Br1A 1.880(12) . ? C2B C3B 1.386(17) . ? C2B C1B 1.461(18) . ? C3A Br2A 1.891(12) . ? C3B C4B 1.473(18) . ? C4A C3A 1.443(17) . ? C4A O2A 1.265(15) . ? C4B O2B 1.238(16) . ? C5A C4A 1.462(17) . ? C5A Br3A 1.916(14) . ? C5B C4B 1.48(2) . ? C6A C5A 1.333(19) . ? C6A Br4A 1.903(12) . ? C6B C5B 1.340(19) . ? C7A C8A 1.49(2) . ? C7A C9A 1.505(19) . ? C7B C8B 1.48(2) . ? C7B C9B 1.51(2) . ? C8A H8C 0.96 . ? C8A H8B 0.96 . ? C8A H8A 0.96 . ? C8B H8D 0.96 . ? C8B H8E 0.96 . ? C8B H8F 0.96 . ? C9A H9C 0.96 . ? C9A H9B 0.96 . ? C9A H9A 0.96 . ? C9B H9D 0.96 . ? C9B H9E 0.96 . ? C9B H9F 0.96 . ? Br1A K1A 3.426(3) . ? Br1B C2B 1.888(13) . ? Br1B K1B 3.487(3) . ? Br2A K1A 3.571(3) 2_765 ? Br2B C3B 1.868(13) . ? Br2B K1B 3.729(3) 2_666 ? Br3B C5B 1.876(13) . ? Br3B K1A 3.844(3) 2_766 ? Br4B C6B 1.896(13) . ? O1A C1A 1.273(16) . ? O1A K1A 2.755(9) . ? O1A K1B 2.670(9) . ? O1B C1B 1.252(15) . ? O1B K1A 2.697(9) . ? O1B K1B 2.825(9) . ? O2A K1A 2.918(10) 2_765 ? O2A K1B 2.674(9) 2_665 ? O2B K1A 2.646(9) 2_766 ? O2B K1B 2.781(10) 2_666 ? O3A C7A 1.232(17) . ? O3A K1A 2.790(10) . ? O3A K1B 2.832(10) 1_655 ? O3B C7B 1.204(17) . ? O3B K1A 2.926(10) . ? O3B K1B 2.858(10) . ? K1A Br2A 3.571(3) 2_765 ? K1A Br3B 3.844(3) 2_766 ? K1A O2A 2.918(10) 2_765 ? K1A O2B 2.646(9) 2_766 ? K1A K1B 3.842(4) 1_655 ? K1B Br2B 3.729(3) 2_666 ? K1B O2A 2.674(9) 2_665 ? K1B O2B 2.781(10) 2_666 ? K1B O3A 2.832(10) 1_455 ? 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 C1A C2A Br1A 115.1(9) . . ? C1A C6A Br4A 114.1(9) . . ? C1A O1A K1A 125.8(8) . . ? C1A O1A K1B 144.1(8) . . ? C1B C2B Br1B 115.4(9) . . ? C1B C6B Br4B 114.5(10) . . ? C1B O1B K1A 140.6(8) . . ? C1B O1B K1B 128.2(8) . . ? C2A C3A C4A 124.2(12) . . ? C2A C3A Br2A 120.8(10) . . ? C2A Br1A K1A 95.4(4) . . ? C2B Br1B K1B 96.2(4) . . ? C2B C3B C4B 121.1(12) . . ? C2B C3B Br2B 123.1(10) . . ? C3A C2A C1A 121.6(12) . . ? C3A C2A Br1A 123.2(10) . . ? C3A C4A C5A 112.2(11) . . ? C3A Br2A K1A 97.5(4) . 2_765 ? C3B C2B C1B 123.2(11) . . ? C3B C2B Br1B 121.3(10) . . ? C3B C4B C5B 114.0(11) . . ? C3B Br2B K1B 91.6(4) . 2_666 ? C4A C3A Br2A 114.9(9) . . ? C4A C5A Br3A 113.2(9) . . ? C4A O2A K1A 128.4(8) . 2_765 ? C4A O2A K1B 143.4(8) . 2_665 ? C4B C3B Br2B 115.7(9) . . ? C4B C5B Br3B 112.8(9) . . ? C4B O2B K1A 139.4(9) . 2_766 ? C4B O2B K1B 129.5(8) . 2_666 ? C5A C6A C1A 123.0(12) . . ? C5A C6A Br4A 122.5(10) . . ? C5B C6B C1B 124.8(13) . . ? C5B C6B Br4B 120.6(10) . . ? C5B Br3B K1A 91.1(4) . 2_766 ? C6A C1A C2A 114.2(11) . . ? C6A C5A C4A 124.3(13) . . ? C6A C5A Br3A 122.4(10) . . ? C6B C1B C2B 114.1(11) . . ? C6B C5B C4B 122.5(12) . . ? C6B C5B Br3B 124.5(11) . . ? C7A C8A H8A 109.5 . . ? C7A C8A H8B 109.5 . . ? C7A C8A H8C 109.5 . . ? C7A C9A H9A 109.5 . . ? C7A C9A H9B 109.5 . . ? C7A C9A H9C 109.5 . . ? C7A O3A K1A 130.1(9) . . ? C7A O3A K1B 136.9(9) . 1_655 ? C7B C8B H8D 109.5 . . ? C7B C8B H8E 109.5 . . ? C7B C8B H8F 109.5 . . ? C7B C9B H9D 109.5 . . ? C7B C9B H9E 109.5 . . ? C7B C9B H9F 109.5 . . ? C7B O3B K1A 131.7(9) . . ? C7B O3B K1B 131.9(9) . . ? C8A C7A C9A 116.8(12) . . ? C8B C7B C9B 115.7(13) . . ? Br1A K1A Br2A 76.24(6) . 2_765 ? Br1A K1A Br3B 55.76(5) . 2_766 ? Br2A K1A Br3B 122.35(8) 2_765 2_766 ? Br1B K1B Br2B 79.72(6) . 2_666 ? O1A C1A C2A 121.0(11) . . ? O1A C1A C6A 124.6(12) . . ? O1A K1A O3A 125.6(3) . . ? O1A K1A O2A 106.8(3) . 2_765 ? O1A K1A Br1A 56.7(2) . . ? O1A K1A O3B 76.2(3) . . ? O1B K1A O2A 144.6(3) . 2_765 ? O1A K1A Br3B 102.6(2) . 2_766 ? O1A K1A Br2A 69.1(2) . 2_765 ? O1A K1B O3A 110.9(3) . 1_455 ? O1A K1B O2A 71.8(3) . 2_665 ? O1A K1B O2B 145.4(3) . 2_666 ? O1A K1B O1B 87.6(3) . . ? O1A K1B O3B 78.7(3) . . ? O1A K1B Br2B 154.0(2) . 2_666 ? O1A K1B Br1B 90.1(2) . . ? O1B C1B C2B 121.0(11) . . ? O1B C1B C6B 124.7(12) . . ? O1B K1A Br1A 97.7(2) . . ? O1B K1A Br3B 68.1(2) . 2_766 ? O1B K1A Br2A 156.4(2) . 2_765 ? O1B K1A O3B 64.3(3) . . ? O1B K1A O3A 125.9(3) . . ? O1B K1A O1A 88.5(3) . . ? O1B K1B Br1B 55.26(19) . . ? O1B K1B Br2B 66.92(19) . 2_666 ? O1B K1B O3A 145.7(3) . 1_455 ? O1B K1B O3B 63.7(3) . . ? O2A C4A C3A 123.7(11) . . ? O2A C4A C5A 123.7(12) . . ? O2A K1A Br1A 67.39(19) 2_765 . ? O2A K1A O3B 149.6(3) 2_765 . ? O2A K1A Br2A 54.27(19) 2_765 2_765 ? O2A K1A Br3B 77.31(19) 2_765 2_766 ? O2A K1B O2B 79.9(3) 2_665 2_666 ? O2A K1B O1B 140.6(3) 2_665 . ? O2B K1B O1B 102.8(3) 2_666 . ? O2A K1B O3B 138.5(3) 2_665 . ? O2A K1B O3A 73.7(3) 2_665 1_455 ? O2A K1B Br1B 90.7(2) 2_665 . ? O2A K1B Br2B 131.6(2) 2_665 2_666 ? O2B C4B C3B 120.8(12) . . ? O2B C4B C5B 125.1(12) . . ? O2B K1A O1B 74.7(3) 2_766 . ? O2B K1A O3A 81.7(3) 2_766 . ? O2B K1A O2A 77.9(3) 2_766 2_765 ? O2B K1A O3B 113.7(3) 2_766 . ? O2B K1A Br1A 103.6(2) 2_766 . ? O3B K1A Br2A 102.0(2) . 2_765 ? O2B K1A O1A 152.6(3) 2_766 . ? O2B K1A Br3B 51.2(2) 2_766 2_766 ? O2B K1A Br2A 128.7(2) 2_766 2_765 ? O2B K1B O3A 78.7(3) 2_666 1_455 ? O2B K1B O3B 135.6(3) 2_666 . ? O2B K1B Br1B 70.3(2) 2_666 . ? O2B K1B Br2B 52.1(2) 2_666 2_666 ? O3A C7A C8A 121.9(13) . . ? O3A C7A C9A 121.3(12) . . ? O3A K1A O2A 70.7(3) . 2_765 ? O3A K1A O3B 82.9(3) . . ? O3A K1A Br1A 135.3(2) . . ? O3A K1A Br2A 67.1(2) . 2_765 ? O3A K1A Br3B 127.7(2) . 2_766 ? O3A K1B Br1B 147.4(2) 1_455 . ? O3A K1B Br2B 89.5(2) 1_455 2_666 ? O3A K1B O3B 90.9(3) 1_455 . ? O3B C7B C8B 122.9(13) . . ? O3B C7B C9B 121.3(14) . . ? O3B K1A Br1A 130.5(2) . . ? O3B K1A Br3B 132.4(2) . 2_766 ? O3B K1B K1A 136.5(2) . 1_455 ? O3B K1B Br1B 118.3(2) . . ? K1A O1B K1B 87.3(2) . . ? K1A O2B K1B 90.1(3) 2_766 2_666 ? K1A O3A K1B 86.2(3) . 1_655 ? K1B O1A K1A 89.3(3) . . ? K1B O2A K1A 86.7(3) 2_665 2_765 ? K1B O3B K1A 82.4(3) . . ? H8B C8A H8A 109.5 . . ? H8C C8A H8B 109.5 . . ? H8C C8A H8A 109.5 . . ? H8D C8B H8E 109.5 . . ? H8D C8B H8F 109.5 . . ? H8E C8B H8F 109.5 . . ? H9B C9A H9A 109.5 . . ? H9C C9A H9B 109.5 . . ? H9C C9A H9A 109.5 . . ? H9E C9B H9D 109.5 . . ? H9F C9B H9E 109.5 . . ? H9F C9B H9D 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1A C2A C3A C4A 1.2(19) . . . . ? C1A C2A C3A Br2A -175.0(9) . . . . ? C1A C2A Br1A K1A 27.4(9) . . . . ? C1A C6A C5A C4A -1(2) . . . . ? C1A C6A C5A Br3A 174.2(9) . . . . ? C1A O1A K1A O3A -75.3(11) . . . . ? C1A O1A K1A O2A 2.7(11) . . . 2_765 ? C1A O1A K1A Br2A -37.1(10) . . . 2_765 ? C1A O1A K1A Br3B 83.0(10) . . . 2_766 ? C1A O1A K1A O2B 98.8(11) . . . 2_766 ? C1A O1A K1A O1B 150.2(10) . . . . ? C1A O1A K1B O2A -1.9(14) . . . 2_665 ? C1A O1A K1B O2B -38.7(17) . . . 2_666 ? C1A O1A K1B O1B -147.8(15) . . . . ? C1A O1A K1B O3A 61.8(15) . . . 1_455 ? C1A O1A K1B O3B 148.5(15) . . . . ? C1A O1A K1B Br1B -92.6(14) . . . . ? C1A O1A K1B Br2B -158.8(12) . . . 2_666 ? C1B C2B C3B C4B -0.3(18) . . . . ? C1B C2B C3B Br2B -176.8(9) . . . . ? C1B C6B C5B C4B 0(2) . . . . ? C1B C6B C5B Br3B 174.8(10) . . . . ? C1B O1B K1A O2B 21.5(13) . . . 2_766 ? C1B O1B K1A O1A -136.6(13) . . . . ? C1B O1B K1A O3A 89.1(13) . . . . ? C1B O1B K1A O2A -19.1(15) . . . 2_765 ? C1B O1B K1A O3B 147.9(14) . . . . ? C1B O1B K1A Br1A -80.6(13) . . . . ? C1B O1B K1A Br2A -153.8(11) . . . 2_765 ? C1B O1B K1A Br3B -32.4(13) . . . 2_766 ? C1B O1B K1B O1A 140.6(10) . . . . ? C1B O1B K1B O2A 83.6(11) . . . 2_665 ? C1B O1B K1B O2B -6.0(11) . . . 2_666 ? C1B O1B K1B O3A -94.5(11) . . . 1_455 ? C1B O1B K1B O3B -140.8(11) . . . . ? C1B O1B K1B Br1B 48.8(10) . . . . ? C1B O1B K1B Br2B -44.6(10) . . . 2_666 ? C2A C1A C6A C5A -5.0(18) . . . . ? C2A C1A C6A Br4A 168.1(8) . . . . ? C2A C3A Br2A K1A 150.9(10) . . . 2_765 ? C2A Br1A K1A O2B 170.5(4) . . . 2_766 ? C2A Br1A K1A O1B -113.4(4) . . . . ? C2A Br1A K1A O1A -30.4(4) . . . . ? C2A Br1A K1A O3A 78.5(5) . . . . ? C2A Br1A K1A O2A 100.1(4) . . . 2_765 ? C2A Br1A K1A O3B -50.7(5) . . . . ? C2A Br1A K1A Br2A 43.4(4) . . . 2_765 ? C2A Br1A K1A Br3B -170.2(4) . . . 2_766 ? C2B C1B C6B C5B -5.0(18) . . . . ? C2B C1B C6B Br4B 170.1(8) . . . . ? C2B C3B C4B O2B 179.8(12) . . . . ? C2B C3B C4B C5B -4.4(16) . . . . ? C2B Br1B K1B O1A -115.4(4) . . . . ? C2B Br1B K1B O2A 172.8(4) . . . 2_665 ? C2B Br1B K1B O2B 93.8(4) . . . 2_666 ? C2B Br1B K1B O1B -28.5(4) . . . . ? C2B Br1B K1B O3A 113.0(5) . . . 1_455 ? C2B Br1B K1B O3B -38.2(4) . . . . ? C2B Br1B K1B Br2B 40.5(4) . . . 2_666 ? C3A C2A Br1A K1A -148.5(10) . . . . ? C3A C4A O2A K1A 49.0(16) . . . 2_765 ? C3A C4A O2A K1B -111.2(14) . . . 2_665 ? C3B C2B C1B O1B -179.7(11) . . . . ? C3B C2B C1B C6B 5.0(17) . . . . ? C3B C4B O2B K1A -133.8(11) . . . 2_766 ? C5B C4B O2B K1A 51(2) . . . 2_766 ? C3B C4B O2B K1B 61.6(16) . . . 2_666 ? C4A C3A Br2A K1A -25.6(9) . . . 2_765 ? C5A C4A C3A C2A -6.5(17) . . . . ? C5A C4A C3A Br2A 169.9(8) . . . . ? C5A C4A O2A K1B 76.4(18) . . . 2_665 ? C5A C4A O2A K1A -123.4(11) . . . 2_765 ? C5B C4B O2B K1B -113.7(13) . . . 2_666 ? C6A C1A C2A C3A 4.8(17) . . . . ? C6A C1A C2A Br1A -171.2(9) . . . . ? C6A C5A C4A O2A 179.4(12) . . . . ? C6A C5A C4A C3A 6.3(17) . . . . ? C6B C5B C4B O2B -179.8(13) . . . . ? C6B C5B C4B C3B 4.6(18) . . . . ? C7A O3A K1A O2B 170.2(12) . . . 2_766 ? C7A O3A K1A O1B 105.9(11) . . . . ? C7A O3A K1A O1A -12.5(13) . . . . ? C7A O3A K1A O2A -109.8(12) . . . 2_765 ? C7A O3A K1A O3B 54.9(11) . . . . ? C7A O3A K1A Br1A -88.7(11) . . . . ? C7A O3A K1A Br2A -51.3(11) . . . 2_765 ? C7A O3A K1A Br3B -165.4(10) . . . 2_766 ? C7B O3B K1A O2B -28.5(13) . . . 2_766 ? C7B O3B K1A O1B -86.4(12) . . . . ? C7B O3B K1A O1A 178.6(13) . . . . ? C7B O3B K1A O3A 49.2(12) . . . . ? C7B O3B K1A O2A 78.7(14) . . . 2_765 ? C7B O3B K1A Br1A -164.1(11) . . . . ? C7B O3B K1A Br2A 113.9(12) . . . 2_765 ? C7B O3B K1A Br3B -86.9(12) . . . 2_766 ? C7B O3B K1B O1A -177.7(13) . . . . ? C7B O3B K1B O2A -132.6(12) . . . 2_665 ? C7B O3B K1B O2B 8.2(14) . . . 2_666 ? C7B O3B K1B O1B 89.5(13) . . . . ? C7B O3B K1B O3A -66.6(13) . . . 1_455 ? C7B O3B K1B Br1B 98.4(12) . . . . ? C7B O3B K1B Br2B 22.8(12) . . . 2_666 ? Br1A C2A C3A C4A 176.8(9) . . . . ? Br1A C2A C3A Br2A 0.6(15) . . . . ? Br1B C2B C1B O1B 3.7(15) . . . . ? Br1B C2B C1B C6B -171.6(8) . . . . ? Br1B C2B C3B C4B 176.1(9) . . . . ? Br1B C2B C3B Br2B -0.3(14) . . . . ? Br2B C3B C4B O2B -3.6(16) . . . . ? Br2B C3B C4B C5B 172.3(9) . . . . ? Br3A C5A C4A O2A 4.2(16) . . . . ? Br3A C5A C4A C3A -169.0(8) . . . . ? Br3B C5B C4B O2B 5.0(17) . . . . ? Br3B C5B C4B C3B -170.6(9) . . . . ? Br4A C6A C5A C4A -173.2(9) . . . . ? Br4A C6A C5A Br3A 1.6(15) . . . . ? Br4B C6B C5B Br3B 0.0(16) . . . . ? Br4B C6B C5B C4B -174.6(9) . . . . ? O1A C1A C2A C3A 179.9(12) . . . . ? O1A C1A C2A Br1A 4.0(16) . . . . ? O1A C1A C6A C5A -179.9(12) . . . . ? O1A C1A C6A Br4A -6.8(16) . . . . ? O1B C1B C6B C5B 179.9(12) . . . . ? O1B C1B C6B Br4B -5.0(16) . . . . ? O2A C4A C3A C2A -179.6(12) . . . . ? O2A C4A C3A Br2A -3.3(16) . . . . ? O3A K1B K1A K1B -98.8(5) 1_455 . . 1_655 ? K1B Br1B C2B C3B -150.5(9) . . . . ? K1B Br1B C2B C1B 26.3(9) . . . . ? K1A Br3B C5B C6B 160.0(11) 2_766 . . . ? K1A Br3B C5B C4B -24.9(9) 2_766 . . . ? K1A O1A C1A C6A 121.4(11) . . . . ? K1A O1A K1B Br2B 9.1(7) . . . 2_666 ? K1A O1A C1A C2A -53.2(15) . . . . ? K1A O3A C7A C9A -15.2(19) . . . . ? K1A O3A C7A C8A 165.3(10) . . . . ? K1A O3B C7B C9B 148.2(11) . . . . ? K1A O1B C1B C6B -87.6(16) . . . . ? K1A O1B C1B C2B 97.6(14) . . . . ? K1A O3B K1B K1A 162.17(17) . . . 1_455 ? K1A O3B C7B C8B -29(2) . . . . ? K1B Br2B C3B C2B 149.6(10) 2_666 . . . ? K1B Br2B C3B C4B -27.0(9) 2_666 . . . ? K1B O1A C1A C6A -73.5(19) . . . . ? K1B O1A C1A C2A 111.9(14) . . . . ? K1B O1B C1B C6B 122.8(11) . . . . ? K1B O1B C1B C2B -52.0(15) . . . . ? K1B O3A C7A C8A 25(2) 1_655 . . . ? K1B O3A C7A C9A -155.8(10) 1_655 . . . ? K1B O3A K1A O1B -99.8(3) 1_655 . . . ? K1B O3B C7B C8B -153.2(11) . . . . ? K1B O3B C7B C9B 24(2) . . . . ? #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-05-08 at 16:31:07 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\program files\wingx\files\cifdoc.dat # CIF files read : kca-100 kca-100-teh struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_KCl4QxMe2CO _database_code_depnum_ccdc_archive 'CCDC 815387' _audit_creation_date 2009-05-08T16:31:07-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C9 H6 Cl4 K O3' _chemical_formula_sum 'C9 H6 Cl4 K O3' _chemical_formula_weight 343.04 #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.46550(10) _cell_length_b 16.7229(2) _cell_length_c 7.45740(10) _cell_angle_alpha 90 _cell_angle_beta 102.8920(10) _cell_angle_gamma 90 _cell_volume 1272.25(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4860 _cell_measurement_theta_min 4.3238 _cell_measurement_theta_max 76.1068 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.791 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 11.345 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1980 _exptl_absorpt_correction_T_max 0.6350 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.11 (release 31-10-2007 CrysAlis171 .NET) (compiled Oct 31 2007,17:16:07) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_measurement_device_type 'Oxford Xcalibur Nova' _diffrn_measurement_method ; CCD detector ; _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4323 _diffrn_radiation_probe x-ray _diffrn_reflns_number 6336 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 4.33 _diffrn_reflns_theta_max 75 _diffrn_reflns_theta_full 76.33 _diffrn_measured_fraction_theta_max 0.974 _diffrn_measured_fraction_theta_full 0.991 _reflns_number_total 2601 _reflns_number_gt 2400 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.0754P)^2^+0.0582P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2601 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0962 _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_restrained_S_all 1.04 _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.555 _refine_diff_density_min -0.364 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly C1 C 0.96568(18) 0.08569(11) 0.7794(2) 0.0228(4) Uani 1 d . . . C2 C 0.90802(18) 0.01433(11) 0.6814(2) 0.0235(4) Uani 1 d . . . C3 C 0.96861(18) -0.05818(11) 0.7041(2) 0.0236(4) Uani 1 d . . . C4 C 1.09647(18) -0.07063(11) 0.8266(2) 0.0228(3) Uani 1 d . . . C5 C 1.15721(18) 0.00162(12) 0.9154(3) 0.0234(4) Uani 1 d . . . C6 C 1.09600(18) 0.07419(11) 0.8935(2) 0.0235(4) Uani 1 d . . . C7 C 0.51794(19) 0.17352(13) 0.5926(3) 0.0305(4) Uani 1 d . . . C8 C 0.4454(3) 0.15050(19) 0.7370(4) 0.0445(6) Uani 1 d . . . C9 C 0.4694(2) 0.13846(17) 0.4042(3) 0.0419(5) Uani 1 d . . . Cl1 Cl 0.76142(4) 0.02830(3) 0.52547(6) 0.03009(15) Uani 1 d . . . Cl2 Cl 0.90209(5) -0.14065(3) 0.57932(7) 0.03052(15) Uani 1 d . . . Cl3 Cl 1.31724(4) -0.00842(3) 1.03498(6) 0.03170(15) Uani 1 d . . . Cl4 Cl 1.17432(5) 0.16002(3) 0.98857(7) 0.03097(15) Uani 1 d . . . O1 O 0.91023(14) 0.15223(8) 0.75666(19) 0.0280(3) Uani 1 d . . . O2 O 1.15234(14) -0.13671(8) 0.84475(19) 0.0278(3) Uani 1 d . . . O3 O 0.61132(14) 0.21834(9) 0.6271(2) 0.0326(3) Uani 1 d . . . K1 K 0.81189(4) 0.23520(2) 0.43634(5) 0.02259(13) Uani 1 d . . . H8A H 0.365(5) 0.178(3) 0.714(6) 0.077(12) Uiso 1 d . . . H8B H 0.426(4) 0.098(3) 0.736(5) 0.067(11) Uiso 1 d . . . H8C H 0.493(3) 0.167(2) 0.854(5) 0.046(8) Uiso 1 d . . . H9A H 0.378(3) 0.1512(19) 0.364(5) 0.048(8) Uiso 1 d . . . H9B H 0.475(4) 0.076(2) 0.414(5) 0.057(9) Uiso 1 d . . . H9C H 0.516(3) 0.157(2) 0.316(5) 0.047(8) Uiso 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 C1 0.0308(9) 0.0189(8) 0.0207(8) 0.0021(6) 0.0101(7) 0.0029(7) C2 0.0274(8) 0.0220(9) 0.0216(9) 0.0025(6) 0.0066(7) 0.0017(6) C3 0.0302(9) 0.0183(8) 0.0247(8) -0.0015(7) 0.0111(7) -0.0014(7) C4 0.0312(9) 0.0175(8) 0.0214(8) 0.0013(6) 0.0097(7) 0.0026(7) C5 0.0277(8) 0.0219(9) 0.0216(8) 0.0018(6) 0.0072(7) 0.0022(7) C6 0.0318(9) 0.0173(8) 0.0230(8) 0.0008(6) 0.0092(7) -0.0002(7) C7 0.0250(8) 0.0319(10) 0.0334(10) 0.0024(8) 0.0040(7) -0.0005(7) C8 0.0403(12) 0.0537(15) 0.0411(13) 0.0015(11) 0.0126(10) -0.0121(11) C9 0.0347(11) 0.0509(15) 0.0380(12) -0.0036(10) 0.0038(9) -0.0135(10) Cl1 0.0283(2) 0.0321(3) 0.0287(3) 0.00215(17) 0.00394(17) 0.00237(17) Cl2 0.0356(2) 0.0224(2) 0.0350(3) -0.00722(17) 0.01087(19) -0.00446(16) Cl3 0.0279(2) 0.0324(3) 0.0333(3) 0.00147(18) 0.00366(18) 0.00434(17) Cl4 0.0395(3) 0.0192(2) 0.0343(3) -0.00278(16) 0.00839(19) -0.00408(16) O1 0.0372(7) 0.0203(7) 0.0280(7) 0.0036(5) 0.0103(5) 0.0077(5) O2 0.0394(7) 0.0171(6) 0.0293(7) 0.0025(5) 0.0131(6) 0.0073(5) O3 0.0287(7) 0.0334(8) 0.0354(8) -0.0022(6) 0.0063(6) -0.0052(6) K1 0.0282(2) 0.0179(2) 0.0224(2) -0.00018(12) 0.00710(15) -0.00035(13) #------------------ MOLECULAR GEOMETRY --------------------------------------# _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 C1 C2 1.458(3) . ? C1 C6 1.450(3) . ? C3 C2 1.361(3) . ? C3 C4 1.457(3) . ? C3 Cl2 1.7215(18) . ? C4 O2 1.243(2) . ? C5 C6 1.365(3) . ? C5 C4 1.454(3) . ? C7 C8 1.499(3) . ? C7 C9 1.503(3) . ? C7 O3 1.213(3) . ? C8 H8A 0.94(5) . ? C8 H8B 0.90(5) . ? C8 H8C 0.94(4) . ? C9 H9A 0.96(3) . ? C9 H9B 1.04(4) . ? C9 H9C 0.95(3) . ? Cl1 C2 1.7219(19) . ? Cl2 K1 3.4103(6) 3_756 ? Cl3 C5 1.7210(19) . ? Cl4 C6 1.7249(19) . ? O1 C1 1.249(2) . ? O1 K1 2.6484(14) 4_566 ? O2 K1 2.6686(14) 2_746 ? O2 K1 2.7562(14) 3_756 ? O3 K1 2.8581(15) 4_566 ? K1 Cl1 3.5845(6) . ? K1 Cl2 3.4103(6) 3_756 ? K1 O1 2.6484(14) 4_565 ? K1 O1 2.7556(14) . ? K1 O2 2.6686(14) 2_756 ? K1 O2 2.7562(14) 3_756 ? K1 O3 2.8000(15) . ? K1 O3 2.8581(15) 4_565 ? 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 C1 C2 Cl1 115.74(13) . . ? C1 C6 Cl4 115.42(14) . . ? C1 O1 K1 141.79(12) . 4_566 ? C1 O1 K1 129.71(12) . . ? C2 C3 C4 122.85(17) . . ? C2 C3 Cl2 121.69(15) . . ? C2 Cl1 K1 96.33(6) . . ? C3 C2 C1 122.52(16) . . ? C3 C2 Cl1 121.66(15) . . ? C3 Cl2 K1 97.92(6) . 3_756 ? C4 C3 Cl2 115.37(14) . . ? C4 C5 Cl3 115.53(14) . . ? C4 O2 K1 141.12(12) . 2_746 ? C4 O2 K1 126.05(12) . 3_756 ? C5 C4 C3 114.44(16) . . ? C5 C6 C1 122.89(17) . . ? C5 C6 Cl4 121.56(15) . . ? C6 C1 C2 114.55(16) . . ? C6 C5 C4 122.57(17) . . ? C6 C5 Cl3 121.68(15) . . ? C7 O3 K1 127.92(14) . . ? C7 O3 K1 138.67(14) . 4_566 ? C7 C8 H8A 108(3) . . ? C7 C8 H8B 113(2) . . ? C7 C8 H8C 110(2) . . ? C7 C9 H9A 108(2) . . ? C7 C9 H9B 108.9(19) . . ? C7 C9 H9C 114(2) . . ? C8 C7 C9 116.87(19) . . ? Cl2 K1 Cl1 74.074(12) 3_756 . ? O1 C1 C6 123.06(17) . . ? O1 C1 C2 122.23(17) . . ? O1 K1 O1 133.18(6) 4_565 . ? O1 K1 O2 73.84(4) 4_565 2_756 ? O1 K1 O2 84.60(4) 4_565 3_756 ? O1 K1 O2 105.70(4) . 3_756 ? O1 K1 O3 138.46(5) 4_565 . ? O1 K1 O3 71.72(4) . . ? O1 K1 O3 154.35(5) . 4_565 ? O1 K1 O3 72.35(4) 4_565 4_565 ? O1 K1 Cl1 52.79(3) . . ? O1 K1 Cl1 150.45(3) 4_565 . ? O1 K1 Cl2 82.48(3) 4_565 3_756 ? O1 K1 Cl2 68.61(3) . 3_756 ? O2 C4 C5 122.79(17) . . ? O2 C4 C3 122.63(17) . . ? O2 K1 O1 84.24(4) 2_756 . ? O2 K1 O2 157.01(5) 2_756 3_756 ? O2 K1 O3 77.81(4) 2_756 . ? O2 K1 O3 124.79(5) 3_756 . ? O2 K1 O3 104.66(5) 2_756 4_565 ? O2 K1 O3 75.44(4) 3_756 4_565 ? O2 K1 Cl1 67.35(3) 3_756 . ? O2 K1 Cl2 112.87(3) 2_756 3_756 ? O2 K1 Cl2 55.09(3) 3_756 3_756 ? O3 C7 C8 121.3(2) . . ? O3 C7 C9 121.83(19) . . ? O3 K1 O3 86.47(4) . 4_565 ? O2 K1 Cl1 131.89(3) 2_756 . ? O3 K1 Cl1 69.54(3) . . ? O3 K1 Cl1 107.46(3) 4_565 . ? O3 K1 Cl2 137.22(4) . 3_756 ? O3 K1 Cl2 126.20(3) 4_565 3_756 ? K1 O1 K1 88.20(4) 4_566 . ? K1 O2 K1 87.78(4) 2_746 3_756 ? K1 O3 K1 83.32(4) . 4_566 ? H8B C8 H8A 106(4) . . ? H8C C8 H8A 107(3) . . ? H8C C8 H8B 112(3) . . ? H9A C9 H9B 106(3) . . ? H9A C9 H9C 109(3) . . ? H9C C9 H9B 110(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 C1 C6 C5 -3.3(2) . . . . ? C2 C1 C6 Cl4 172.44(12) . . . . ? C2 C3 C4 C5 -3.0(2) . . . . ? C2 C3 C4 O2 -178.89(17) . . . . ? C2 C3 Cl2 K1 149.28(14) . . . 3_756 ? C3 C4 O2 K1 -96.8(2) . . . 2_746 ? C3 C4 O2 K1 49.0(2) . . . 3_756 ? C4 C3 C2 C1 -0.6(3) . . . . ? C4 C3 C2 Cl1 176.07(13) . . . . ? C4 C3 Cl2 K1 -27.43(13) . . . 3_756 ? C4 C5 C6 C1 -0.3(3) . . . . ? C4 C5 C6 Cl4 -175.79(13) . . . . ? C5 C4 O2 K1 87.7(2) . . . 2_746 ? C5 C4 O2 K1 -126.52(16) . . . 3_756 ? C6 C1 C2 C3 3.8(2) . . . . ? C6 C1 C2 Cl1 -173.08(13) . . . . ? C6 C5 C4 O2 179.30(17) . . . . ? C6 C5 C4 C3 3.5(2) . . . . ? C8 C7 O3 K1 158.74(17) . . . . ? C8 C7 O3 K1 27.2(3) . . . 4_566 ? C9 C7 O3 K1 -152.74(17) . . . 4_566 ? C9 C7 O3 K1 -21.2(3) . . . . ? Cl1 K1 O1 C1 47.28(15) . . . . ? Cl1 K1 O3 C7 -48.72(17) . . . . ? Cl1 K1 O1 K1 -127.38(5) . . . 4_566 ? Cl1 K1 O3 K1 101.42(3) . . . 4_566 ? Cl2 C3 C2 C1 -177.05(13) . . . . ? Cl2 C3 C2 Cl1 -0.4(2) . . . . ? Cl2 C3 C4 C5 173.63(12) . . . . ? Cl2 C3 C4 O2 -2.2(2) . . . . ? Cl2 K1 O1 C1 -38.55(15) 3_756 . . . ? Cl2 K1 O1 K1 146.78(4) 3_756 . . 4_566 ? Cl2 K1 O3 C7 -82.19(18) 3_756 . . . ? Cl2 K1 O3 K1 67.95(5) 3_756 . . 4_566 ? Cl2 K1 Cl1 C2 45.82(6) 3_756 . . . ? Cl3 C5 C4 C3 -171.25(13) . . . . ? Cl3 C5 C4 O2 4.6(2) . . . . ? Cl3 C5 C6 C1 174.12(13) . . . . ? Cl3 C5 C6 Cl4 -1.4(2) . . . . ? O1 C1 C2 C3 179.25(17) . . . . ? O1 C1 C2 Cl1 2.4(2) . . . . ? O1 C1 C6 C5 -178.79(17) . . . . ? O1 C1 C6 Cl4 -3.0(2) . . . . ? O1 K1 O1 C1 -94.47(14) 4_565 . . . ? O1 K1 O1 K1 90.86(7) 4_565 . . 4_566 ? O1 K1 O1 K1 90.86(7) 4_565 . . 4_566 ? O1 K1 O3 K1 45.23(4) . . . 4_566 ? O1 K1 O3 K1 -90.32(7) 4_565 . . 4_566 ? O1 K1 O3 C7 119.54(17) 4_565 . . . ? O1 K1 O3 C7 -104.91(18) . . . . ? O1 K1 Cl1 C2 -29.14(7) . . . . ? O1 K1 Cl1 C2 84.62(9) 4_565 . . . ? O2 K1 O1 C1 -155.89(16) 2_756 . . . ? O2 K1 O1 C1 2.98(17) 3_756 . . . ? O2 K1 O1 K1 29.45(4) 2_756 . . 4_566 ? O2 K1 O1 K1 -171.68(4) 3_756 . . 4_566 ? O2 K1 O3 C7 167.20(18) 2_756 . . . ? O2 K1 O3 K1 -42.66(4) 2_756 . . 4_566 ? O2 K1 O3 K1 141.98(4) 3_756 . . 4_566 ? O2 K1 O3 C7 -8.16(19) 3_756 . . . ? O2 K1 Cl1 C2 -60.86(8) 2_756 . . . ? O2 K1 Cl1 C2 104.10(7) 3_756 . . . ? O3 K1 O1 C1 125.08(16) . . . . ? O3 K1 O1 C1 91.96(18) 4_565 . . . ? O3 K1 O1 K1 -49.58(4) . . . 4_566 ? O3 K1 O1 K1 -82.71(11) 4_565 . . 4_566 ? O3 K1 O3 C7 61.38(16) 4_565 . . . ? O3 K1 O3 K1 -148.48(6) 4_565 . . 4_566 ? O3 K1 Cl1 C2 -111.26(7) . . . . ? O3 K1 Cl1 C2 169.47(7) 4_565 . . . ? K1 K1 O1 C1 -19.87(19) 4_565 . . . ? K1 K1 O1 C1 174.67(18) 4_566 . . . ? K1 O1 C1 C2 118.82(19) 4_566 . . . ? K1 O1 C1 C2 -52.5(2) . . . . ? K1 O1 C1 C6 -66.1(3) 4_566 . . . ? K1 O1 C1 C6 122.57(16) . . . . ? K1 Cl1 C2 C3 -151.16(14) . . . . ? K1 Cl1 C2 C1 25.70(13) . . . . ? #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-05-11 at 10:48:22 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\program files\wingx\files\cifdoc.dat # CIF files read : exp_713 exp713teh struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_NaBr4Q _database_code_depnum_ccdc_archive 'CCDC 815388' _audit_creation_date 2009-05-11T10:48:22-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C6 Br4 Na1 O2' _chemical_formula_sum 'C6 Br4 Na O2' _chemical_formula_weight 446.67 #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.1909(3) _cell_length_b 3.6689(3) _cell_length_c 15.5125(6) _cell_angle_alpha 90 _cell_angle_beta 97.712(3) _cell_angle_gamma 90 _cell_volume 461.96(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1589 _cell_measurement_theta_min 2.8658 _cell_measurement_theta_max 75.8036 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 3.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 406 _exptl_absorpt_coefficient_mu 21.425 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0858 _exptl_absorpt_correction_T_max 0.8036 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.11 (release 31-10-2007 CrysAlis171 .NET) (compiled Oct 31 2007,17:16:07) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54179 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_measurement_device_type 'Oxford Xcalibur Nova' _diffrn_measurement_method ; CCD detector ; _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4323 _diffrn_radiation_probe x-ray _diffrn_reflns_number 2253 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 5.76 _diffrn_reflns_theta_max 75.95 _diffrn_reflns_theta_full 75.95 _diffrn_measured_fraction_theta_max 0.967 _diffrn_measured_fraction_theta_full 0.967 _reflns_number_total 939 _reflns_number_gt 784 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.1527P)^2^+29.5980P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 939 _refine_ls_number_parameters 61 _refine_ls_number_restraints 6 _refine_ls_R_factor_gt 0.072 _refine_ls_wR_factor_ref 0.2649 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0 _refine_diff_density_max 3.789 _refine_diff_density_min -2.57 _refine_special_details ; Due to extremely small size of the crystals (which are also unstable) data quality was relatively poor, resulting with high R factor and residual electron density. Anisotropic displacement ellipsoid of atom C3 was restrained (using the command ISOR in SHELXL) to prevent unrealistic elongation. ; #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.018 0.009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.676 1.281 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.135 0.124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.049 0.032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly C1 C 0.6740(17) 0.495(6) -0.0141(9) 0.026(4) Uani 1 d . . . C2 C 0.6200(17) 0.351(4) 0.0658(9) 0.018(3) Uani 1 d . . . C3 C 0.4590(16) 0.367(4) 0.0782(9) 0.015(3) Uani 1 d U . . Br1 Br 0.78973(17) 0.1841(4) 0.14791(9) 0.0177(6) Uani 1 d . . . Br2 Br 0.39207(17) 0.2025(5) 0.18443(10) 0.0193(6) Uani 1 d . . . O1 O 0.8204(12) 0.496(4) -0.0286(7) 0.024(2) Uani 1 d . . . Na1 Na 1 0 0 0.034(2) Uani 1 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 C1 0.005(6) 0.057(12) 0.015(6) -0.007(7) 0.002(5) 0.007(7) C2 0.010(6) 0.024(7) 0.017(6) -0.012(6) -0.004(5) -0.005(5) C3 0.007(6) 0.023(7) 0.014(6) 0.000(5) 0.000(4) -0.006(5) Br1 0.0106(9) 0.0203(11) 0.0218(9) -0.0014(6) 0.0003(6) 0.0012(5) Br2 0.0145(9) 0.0212(10) 0.0232(9) 0.0000(6) 0.0059(6) 0.0000(5) O1 0.008(5) 0.043(7) 0.023(5) -0.008(5) 0.004(4) -0.006(5) Na1 0.023(5) 0.036(6) 0.046(6) -0.007(5) 0.020(4) -0.003(4) #------------------ MOLECULAR GEOMETRY --------------------------------------# _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 C1 C3 1.46(2) 3_665 ? C1 O1 1.249(17) . ? C2 C1 1.47(2) . ? C3 C1 1.46(2) 3_665 ? C3 C2 1.36(2) . ? Br1 C2 1.859(15) . ? Br2 C3 1.902(14) . ? Br1 Na1 3.1222(14) . ? O1 Na1 2.366(12) 1_565 ? Na1 O1 2.345(13) 3_755 ? Na1 O1 2.345(13) . ? Na1 O1 2.366(12) 3_765 ? Na1 O1 2.366(12) 1_545 ? Na1 Br1 3.1222(14) 3_755 ? 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 C1 C2 Br1 114.5(10) . . ? C1 C3 Br2 115.1(10) 3_665 . ? C1 O1 Na1 123.7(13) . . ? C1 O1 Na1 123.9(12) . 1_565 ? C2 C3 C1 124.4(14) . 3_665 ? C2 C3 Br2 120.5(11) . . ? C2 Br1 Na1 90.2(5) . . ? C3 C1 C2 114.7(12) 3_665 . ? C3 C2 C1 120.9(13) . . ? C3 C2 Br1 124.5(12) . . ? Br1 Na1 Br1 180 . 3_755 ? O1 C1 C3 121.4(15) . 3_665 ? O1 C1 C2 123.9(14) . . ? O1 Na1 O1 180 3_755 . ? O1 Na1 O1 102.3(4) 3_755 3_765 ? O1 Na1 O1 77.7(4) . 3_765 ? O1 Na1 O1 77.7(4) 3_755 1_545 ? O1 Na1 O1 102.3(4) . 1_545 ? O1 Na1 O1 180 3_765 1_545 ? O1 Na1 Br1 115.0(3) 3_755 . ? O1 Na1 Br1 65.0(3) . . ? O1 Na1 Br1 94.8(2) 3_765 . ? O1 Na1 Br1 85.2(2) 1_545 . ? O1 Na1 Br1 65.0(3) 3_755 3_755 ? O1 Na1 Br1 115.0(3) . 3_755 ? O1 Na1 Br1 85.2(2) 3_765 3_755 ? O1 Na1 Br1 94.8(2) 1_545 3_755 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C3 C2 C1 3(3) 3_665 . . . ? C1 C3 C2 Br1 178.6(13) 3_665 . . . ? C2 C1 O1 Na1 -95(2) . . . 1_565 ? C2 Br1 Na1 O1 -149.0(5) . . . 3_755 ? C2 Br1 Na1 O1 31.0(5) . . . . ? C2 Br1 Na1 O1 105.1(5) . . . 3_765 ? C2 Br1 Na1 O1 -74.9(5) . . . 1_545 ? C2 Br1 Na1 Br1 8E1(10) . . . 3_755 ? C2 C1 O1 Na1 44(2) . . . . ? C3 C1 O1 Na1 86.1(17) 3_665 . . 1_565 ? C3 C1 O1 Na1 -134.7(15) 3_665 . . . ? C3 C2 C1 O1 178.2(17) . . . . ? C3 C2 C1 C3 -3(3) . . . 3_665 ? Br1 C2 C1 O1 2(2) . . . . ? Br1 C2 C1 C3 -178.8(12) . . . 3_665 ? Br2 C3 C2 C1 -176.8(12) . . . . ? Br2 C3 C2 Br1 -1.2(19) . . . . ? Br1 Na1 O1 C1 -45.0(11) . . . . ? Br1 Na1 O1 C1 135.0(11) 3_755 . . . ? Br1 Na1 O1 Na1 101.3(4) . . . 1_565 ? Br1 Na1 O1 Na1 -78.7(4) 3_755 . . 1_565 ? O1 Na1 O1 C1 -7E1(10) 3_755 . . . ? O1 Na1 O1 C1 -146.3(13) 3_765 . . . ? O1 Na1 O1 C1 33.7(13) 1_545 . . . ? O1 Na1 O1 Na1 8E1(10) 3_755 . . 1_565 ? O1 Na1 O1 Na1 0 3_765 . . 1_565 ? O1 Na1 O1 Na1 180 1_545 . . 1_565 ? Na1 Br1 C2 C3 156.0(13) . . . . ? Na1 Br1 C2 C1 -28.1(12) . . . . ? #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-09-16 at 11:15:53 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\program files\wingx\files\cifdoc.dat # CIF files read : rbbr4q-2 rbbr4q-2-teh #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_RbBr4Q-293K _database_code_depnum_ccdc_archive 'CCDC 815389' _audit_creation_date 2009-09-16T11:15:53-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_sum 'C6 Br4 O2 Rb' _chemical_formula_weight 509.17 _chemical_absolute_configuration unk #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 4.33820(10) _cell_length_b 13.8640(2) _cell_length_c 17.4665(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1050.52(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2265 _cell_measurement_theta_min 2.5259 _cell_measurement_theta_max 75.7743 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 3.219 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 24.044 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.18836 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_reflns_number 3488 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.07 _diffrn_reflns_theta_max 75.84 _diffrn_reflns_theta_full 75.84 _diffrn_measured_fraction_theta_max 0.974 _diffrn_measured_fraction_theta_full 0.974 _reflns_number_total 1920 _reflns_number_gt 1771 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.0934P)^2^+0.4994P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_number_reflns 1920 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.045 _refine_ls_wR_factor_ref 0.1241 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.43(8) _refine_diff_density_max 1.378 _refine_diff_density_min -0.6 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.4688 1.6079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly C1 C 0.756(2) 0.5404(6) 0.3101(4) 0.0392(16) Uani 1 d . . . C2 C 0.911(2) 0.4537(6) 0.3330(4) 0.0398(16) Uani 1 d . . . C3 C 0.906(2) 0.4222(6) 0.4070(4) 0.0392(15) Uani 1 d . . . C4 C 0.748(2) 0.4726(7) 0.4673(4) 0.0422(17) Uani 1 d . . . C5 C 0.598(2) 0.5604(6) 0.4438(4) 0.0395(16) Uani 1 d . . . C6 C 0.6035(19) 0.5924(6) 0.3709(4) 0.0398(15) Uani 1 d . . . Br1 Br 1.1069(3) 0.38288(8) 0.25477(5) 0.0565(3) Uani 1 d . . . Br2 Br 1.1221(3) 0.30988(7) 0.43713(5) 0.0529(3) Uani 1 d . . . Br3 Br 0.3865(3) 0.62764(8) 0.52256(5) 0.0566(3) Uani 1 d . . . Br4 Br 0.3994(3) 0.70726(8) 0.34149(6) 0.0563(3) Uani 1 d . . . O1 O 0.7576(17) 0.5715(6) 0.2422(3) 0.0517(16) Uani 1 d . . . O2 O 0.7461(18) 0.4414(5) 0.5351(3) 0.0498(14) Uani 1 d . . . Rb1 Rb 0.2616(2) 0.59623(8) 0.13909(4) 0.0537(3) Uani 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 C1 0.040(3) 0.051(4) 0.026(3) 0.003(3) -0.014(4) -0.001(4) C2 0.039(4) 0.053(4) 0.027(3) 0.004(3) -0.004(3) -0.007(4) C3 0.043(4) 0.047(4) 0.028(3) -0.002(3) -0.003(4) 0.000(4) C4 0.039(3) 0.062(5) 0.026(3) 0.005(3) -0.002(4) -0.007(4) C5 0.043(4) 0.046(4) 0.030(3) -0.005(3) -0.002(4) -0.004(4) C6 0.036(3) 0.048(4) 0.036(3) 0.004(3) -0.003(3) -0.005(4) Br1 0.0662(6) 0.0670(6) 0.0363(4) -0.0094(4) 0.0094(5) -0.0005(6) Br2 0.0560(5) 0.0544(5) 0.0483(4) 0.0103(4) 0.0000(4) 0.0025(5) Br3 0.0683(6) 0.0646(6) 0.0370(4) -0.0085(4) 0.0106(5) -0.0030(6) Br4 0.0588(5) 0.0576(5) 0.0524(5) 0.0119(4) 0.0018(5) 0.0075(5) O1 0.049(3) 0.084(5) 0.022(2) 0.011(2) 0.002(3) 0.002(4) O2 0.047(3) 0.073(4) 0.030(2) 0.012(3) 0.001(3) 0.002(3) Rb1 0.0449(4) 0.0890(6) 0.0272(3) 0.0064(4) 0.0001(4) 0.0022(4) #------------------ MOLECULAR GEOMETRY --------------------------------------# _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 C1 C6 1.444(12) . ? C2 C1 1.432(12) . ? C2 C3 1.363(10) . ? C4 C3 1.437(12) . ? C4 C5 1.442(13) . ? C5 C6 1.349(10) . ? Br1 C2 1.886(8) . ? Br1 Rb1 3.6445(14) 1_655 ? Br2 C3 1.893(8) . ? Br2 Rb1 3.6494(15) 3_645 ? Br2 Rb1 3.7937(13) 2_665 ? Br3 C5 1.897(8) . ? Br3 Rb1 3.7668(15) 2_565 ? Br4 C6 1.893(8) . ? O1 C1 1.263(9) . ? O1 Rb1 2.853(7) 1_655 ? O2 C4 1.261(9) . ? O2 Rb1 2.852(7) 2_665 ? O2 Rb1 2.902(7) 2_565 ? Rb1 Br1 3.6445(14) 1_455 ? Rb1 Br2 3.6494(15) 3_655 ? Rb1 Br2 3.7937(13) 2_664 ? Rb1 Br3 3.7668(15) 2_564 ? Rb1 Br4 3.9020(14) . ? Rb1 O1 2.826(7) . ? Rb1 O1 2.853(7) 1_455 ? Rb1 O2 2.852(7) 2_664 ? Rb1 O2 2.902(7) 2_564 ? 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 C1 C2 Br1 116.5(6) . . ? C1 C6 Br4 115.8(5) . . ? C1 O1 Rb1 129.6(7) . . ? C1 O1 Rb1 129.6(7) . 1_655 ? C2 C1 C6 115.4(7) . . ? C2 C3 C4 123.1(8) . . ? C2 C3 Br2 121.3(7) . . ? C2 Br1 Rb1 93.6(2) . 1_655 ? C3 C2 C1 121.7(8) . . ? C3 C2 Br1 121.8(7) . . ? C3 C4 C5 114.7(7) . . ? C3 Br2 Rb1 109.9(3) . 3_645 ? C3 Br2 Rb1 92.4(2) . 2_665 ? C4 C3 Br2 115.6(6) . . ? C4 C5 Br3 115.3(6) . . ? C4 O2 Rb1 131.0(7) . 2_665 ? C4 O2 Rb1 130.9(7) . 2_565 ? C5 C6 C1 122.6(8) . . ? C5 C6 Br4 121.6(7) . . ? C5 Br3 Rb1 94.0(3) . 2_565 ? C6 C5 C4 122.5(8) . . ? C6 C5 Br3 122.2(7) . . ? C6 Br4 Rb1 89.2(2) . . ? Br1 Rb1 Br2 140.99(4) 1_455 3_655 ? Br1 Rb1 Br2 144.93(3) 1_455 2_664 ? Br1 Rb1 Br3 66.38(3) 1_455 2_564 ? Br1 Rb1 Br4 81.15(2) 1_455 . ? Br2 Rb1 Br2 56.15(2) 3_655 2_664 ? Br2 Rb1 Br3 113.20(3) 3_655 2_564 ? Br2 Rb1 Br4 94.60(3) 3_655 . ? Br2 Rb1 Br4 133.37(4) 2_664 . ? Br3 Rb1 Br2 78.64(2) 2_564 2_664 ? Br3 Rb1 Br4 147.22(3) 2_564 . ? O1 C1 C2 123.1(9) . . ? O1 C1 C6 121.5(8) . . ? O2 C4 C3 121.7(9) . . ? O2 C4 C5 123.6(9) . . ? O1 Rb1 Br1 53.94(15) 1_455 1_455 ? O1 Rb1 Br1 71.85(15) . 1_455 ? O1 Rb1 Br2 136.87(13) 1_455 2_664 ? O1 Rb1 Br2 132.70(16) . 3_655 ? O1 Rb1 Br2 88.75(14) 1_455 3_655 ? O1 Rb1 Br2 122.19(13) . 2_664 ? O1 Rb1 Br3 111.97(16) . 2_564 ? O1 Rb1 Br3 96.38(16) 1_455 2_564 ? O1 Rb1 Br4 49.77(14) . . ? O1 Rb1 Br4 65.99(14) 1_455 . ? O1 Rb1 O1 99.61(15) . 1_455 ? O1 Rb1 O2 79.25(17) . 2_664 ? O1 Rb1 O2 162.7(2) . 2_564 ? O1 Rb1 O2 77.98(17) 1_455 2_564 ? O2 Rb1 Br1 110.03(15) 2_664 1_455 ? O2 Rb1 Br1 93.51(14) 2_564 1_455 ? O2 Rb1 Br2 64.63(14) 2_564 3_655 ? O2 Rb1 Br2 65.21(13) 2_564 2_664 ? O2 Rb1 Br2 104.94(14) 2_664 3_655 ? O2 Rb1 Br2 51.02(14) 2_664 2_664 ? O2 Rb1 Br3 68.45(14) 2_664 2_564 ? O2 Rb1 Br3 51.98(14) 2_564 2_564 ? O2 Rb1 Br4 122.32(14) 2_664 . ? O2 Rb1 Br4 138.96(13) 2_564 . ? O2 Rb1 O1 162.5(2) 2_664 1_455 ? O2 Rb1 O2 97.85(16) 2_664 2_564 ? Rb1 Rb1 Rb1 180 1_655 1_455 ? Rb1 Br2 Rb1 132.72(3) 3_645 2_665 ? Rb1 O1 Rb1 99.61(15) . 1_655 ? Rb1 O2 Rb1 97.85(16) 2_665 2_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 C4 0.0(14) . . . . ? C1 C2 C3 Br2 -177.9(7) . . . . ? C2 C1 C6 Br4 179.9(6) . . . . ? C2 C1 C6 C5 -1.9(12) . . . . ? C3 C2 C1 C6 1.4(12) . . . . ? C3 C4 C5 C6 0.3(13) . . . . ? C3 C4 C5 Br3 179.7(6) . . . . ? C3 C2 C1 O1 179.8(9) . . . . ? C4 C5 C6 C1 1.2(14) . . . . ? C4 C5 C6 Br4 179.3(7) . . . . ? C5 C4 C3 C2 -0.8(13) . . . . ? C5 C4 C3 Br2 177.1(6) . . . . ? Br1 C2 C1 C6 179.0(6) . . . . ? Br1 C2 C1 O1 -2.6(13) . . . . ? Br1 C2 C3 Br2 4.6(11) . . . . ? Br1 C2 C3 C4 -177.5(7) . . . . ? Br1 Rb1 Br4 C6 40.7(3) 1_455 . . . ? Br1 Rb1 O1 C1 -34.9(8) 1_455 . . . ? Br1 Rb1 O1 Rb1 133.1(2) 1_455 . . 1_655 ? Br2 Rb1 Br4 C6 -178.4(3) 3_655 . . . ? Br2 Rb1 Br4 C6 -132.2(3) 2_664 . . . ? Br2 Rb1 O1 C1 109.2(8) 3_655 . . . ? Br2 Rb1 O1 C1 -179.2(7) 2_664 . . . ? Br2 Rb1 O1 Rb1 -82.8(2) 3_655 . . 1_655 ? Br2 Rb1 O1 Rb1 -11.1(3) 2_664 . . 1_655 ? Br3 C5 C6 C1 -178.3(6) . . . . ? Br3 C5 C6 Br4 -0.2(11) . . . . ? Br3 Rb1 Br4 C6 32.9(3) 2_564 . . . ? Br3 Rb1 O1 C1 -89.0(8) 2_564 . . . ? Br3 Rb1 O1 Rb1 79.1(2) 2_564 . . 1_655 ? Br4 Rb1 O1 C1 58.8(7) . . . . ? Br4 Rb1 O1 Rb1 -133.1(3) . . . 1_655 ? O1 C1 C6 C5 179.6(9) . . . . ? O1 C1 C6 Br4 1.4(12) . . . . ? O1 Rb1 Br4 C6 -33.0(3) . . . . ? O1 Rb1 Br4 C6 95.0(3) 1_455 . . . ? O1 Rb1 O1 C1 11.9(9) 1_455 . . . ? O1 Rb1 O1 Rb1 180 1_455 . . 1_655 ? O2 C4 C3 C2 179.5(9) . . . . ? O2 C4 C3 Br2 -2.5(12) . . . . ? O2 C4 C5 C6 179.9(9) . . . . ? O2 C4 C5 Br3 -0.6(13) . . . . ? O2 Rb1 Br4 C6 -67.5(3) 2_664 . . . ? O2 Rb1 Br4 C6 125.8(3) 2_564 . . . ? O2 Rb1 O1 C1 -150.3(8) 2_664 . . . ? O2 Rb1 O1 C1 -68.5(10) 2_564 . . . ? O2 Rb1 O1 Rb1 17.7(2) 2_664 . . 1_655 ? O2 Rb1 O1 Rb1 99.6(6) 2_564 . . 1_655 ? Rb1 Br1 C2 C1 29.5(7) 1_655 . . . ? Rb1 Br1 C2 C3 -152.8(7) 1_655 . . . ? Rb1 Br2 C3 C2 -71.4(8) 3_645 . . . ? Rb1 Br2 C3 C2 151.0(7) 2_665 . . . ? Rb1 Br2 C3 C4 110.6(6) 3_645 . . . ? Rb1 Br2 C3 C4 -27.0(7) 2_665 . . . ? Rb1 Br3 C5 C6 152.3(7) 2_565 . . . ? Rb1 Br3 C5 C4 -27.2(7) 2_565 . . . ? Rb1 Br4 C6 C5 -149.0(7) . . . . ? Rb1 Br4 C6 C1 29.2(6) . . . . ? Rb1 O1 C1 C2 116.4(9) . . . . ? Rb1 O1 C1 C2 -48.3(13) 1_655 . . . ? Rb1 O1 C1 C6 -65.3(11) . . . . ? Rb1 O1 C1 C6 130.0(8) 1_655 . . . ? Rb1 O2 C4 C3 59.8(12) 2_665 . . . ? Rb1 O2 C4 C3 -127.2(8) 2_565 . . . ? Rb1 O2 C4 C5 -119.8(9) 2_665 . . . ? Rb1 O2 C4 C5 53.2(13) 2_565 . . . ? #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-05-11 at 10:44:10 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\program files\wingx\files\cifdoc.dat # CIF files read : rbbr4q-1 rbbr4q-1 struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_RbBr4Q-100K _database_code_depnum_ccdc_archive 'CCDC 815390' _audit_creation_date 2009-05-11T10:44:10-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C6 Br4 O2 Rb1' _chemical_formula_sum 'C6 Br4 O2 Rb' _chemical_formula_weight 509.17 _chemical_absolute_configuration unk #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 4.33400(10) _cell_length_b 13.5784(3) _cell_length_c 17.4009(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1024.02(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3956 _cell_measurement_theta_min 2.5396 _cell_measurement_theta_max 76.0029 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 3.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 24.666 _exptl_absorpt_correction_T_min 0.10845 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54179 _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_measurement_device_type 'Oxford Xcalibur Nova' _diffrn_measurement_method ; CCD detector ; _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4323 _diffrn_reflns_number 5013 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.89 _diffrn_reflns_theta_max 66.12 _diffrn_reflns_theta_full 66.12 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measured_fraction_theta_full 0.985 _reflns_number_total 2041 _reflns_number_gt 1953 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.0764P)^2^+2.1726P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2041 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.043 _refine_ls_wR_factor_ref 0.1115 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.51(7) _refine_diff_density_max 1.359 _refine_diff_density_min -0.917 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.4688 1.6079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly C1 C 0.760(2) 0.5460(6) 0.3091(4) 0.0214(15) Uani 1 d . . . C2 C 0.916(2) 0.4562(6) 0.3331(5) 0.0230(17) Uani 1 d . . . C3 C 0.914(2) 0.4241(6) 0.4077(5) 0.0228(16) Uani 1 d . . . C4 C 0.745(2) 0.4724(7) 0.4694(4) 0.0262(17) Uani 1 d . . . C5 C 0.590(2) 0.5627(6) 0.4451(4) 0.0216(16) Uani 1 d . . . C6 C 0.5951(19) 0.5957(6) 0.3719(4) 0.0188(14) Uani 1 d . . . Br1 Br 1.1188(2) 0.38590(7) 0.25510(4) 0.0266(2) Uani 1 d . . . Br2 Br 1.1303(3) 0.30975(6) 0.43771(4) 0.0256(2) Uani 1 d . . . Br3 Br 0.3706(3) 0.62895(6) 0.52323(4) 0.0263(2) Uani 1 d . . . Br4 Br 0.3891(2) 0.71255(6) 0.34183(5) 0.0266(2) Uani 1 d . . . O1 O 0.7596(17) 0.5758(5) 0.2423(3) 0.0263(12) Uani 1 d . . . O2 O 0.7409(17) 0.4412(4) 0.5359(3) 0.0244(12) Uani 1 d . . . Rb1 Rb 0.2638(2) 0.59907(7) 0.13900(4) 0.0264(2) Uani 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 C1 0.024(4) 0.030(4) 0.009(3) 0.005(3) -0.001(3) -0.002(4) C2 0.020(4) 0.028(4) 0.021(3) -0.002(3) 0.000(3) -0.004(3) C3 0.017(4) 0.024(4) 0.027(4) 0.003(3) -0.002(3) -0.006(3) C4 0.025(4) 0.036(5) 0.017(3) 0.002(3) -0.004(4) -0.007(4) C5 0.027(4) 0.028(4) 0.010(3) -0.005(3) 0.000(3) -0.003(3) C6 0.017(4) 0.024(4) 0.015(3) -0.003(3) -0.003(3) -0.003(3) Br1 0.0334(5) 0.0310(5) 0.0153(3) -0.0041(3) 0.0032(3) -0.0007(4) Br2 0.0306(4) 0.0269(4) 0.0194(4) 0.0036(3) -0.0001(3) 0.0005(4) Br3 0.0339(5) 0.0297(4) 0.0153(4) -0.0021(3) 0.0036(4) -0.0017(4) Br4 0.0305(4) 0.0281(4) 0.0213(4) 0.0042(3) 0.0014(3) 0.0023(4) O1 0.028(3) 0.037(3) 0.014(2) 0.004(2) -0.002(2) -0.007(3) O2 0.032(3) 0.029(3) 0.012(2) 0.007(2) 0.003(2) 0.000(3) Rb1 0.0265(4) 0.0407(4) 0.0121(3) 0.0024(3) 0.0004(3) 0.0017(4) #------------------ MOLECULAR GEOMETRY --------------------------------------# _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 C1 C6 1.470(11) . ? C1 Rb1 3.749(8) 1_655 ? C2 C1 1.456(12) . ? C2 C3 1.369(11) . ? C4 C3 1.457(13) . ? C4 C5 1.460(14) . ? C5 C6 1.349(10) . ? Br1 C2 1.877(8) . ? Br1 Rb1 3.5854(12) 1_655 ? Br2 C3 1.887(9) . ? Br2 Rb1 3.5893(13) 4_645 ? Br2 Rb1 3.7432(11) 2_665 ? Br3 C5 1.887(8) . ? Br3 Rb1 3.7396(12) 2_565 ? Br4 C6 1.895(8) . ? O1 C1 1.231(9) . ? O1 Rb1 2.847(7) 1_655 ? O2 C4 1.233(10) . ? O2 Rb1 2.850(7) 2_665 ? O2 Rb1 2.881(7) 2_565 ? Rb1 Br1 3.5854(12) 1_455 ? Rb1 Br2 3.5893(13) 4_655 ? Rb1 Br3 3.7396(12) 2_564 ? Rb1 Br4 3.8893(11) . ? Rb1 O1 2.819(7) . ? Rb1 O1 2.847(7) 1_455 ? Rb1 O2 2.850(7) 2_664 ? Rb1 O2 2.881(7) 2_564 ? 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 C1 C2 Br1 115.9(6) . . ? C1 C6 Br4 114.1(5) . . ? C1 O1 Rb1 129.8(6) . . ? C1 O1 Rb1 129.2(6) . 1_655 ? C2 C3 C4 124.0(8) . . ? C2 C3 Br2 121.4(7) . . ? C2 C1 C6 113.4(7) . . ? C2 C1 Rb1 131.2(5) . . ? C2 C1 Rb1 96.7(5) . 1_655 ? C2 Br1 Rb1 94.5(3) . 1_655 ? C3 C2 C1 122.3(8) . . ? C3 C2 Br1 121.8(7) . . ? C3 C4 C5 113.3(7) . . ? C3 Br2 Rb1 108.5(3) . 4_645 ? C3 Br2 Rb1 92.7(3) . 2_665 ? C3 Br2 Rb1 143.2(3) . 4_745 ? C4 C3 Br2 114.6(6) . . ? C4 C5 Br3 115.0(6) . . ? C4 O2 Rb1 130.3(7) . 2_665 ? C4 O2 Rb1 131.3(7) . 2_565 ? C5 C6 C1 123.9(8) . . ? C5 C6 Br4 122.0(6) . . ? C5 Br3 Rb1 94.1(3) . 2_565 ? C6 Br4 Rb1 89.1(2) . . ? C6 C1 Rb1 102.8(5) . . ? C6 C1 Rb1 141.4(5) . 1_655 ? C6 C5 C4 123.0(8) . . ? C6 C5 Br3 122.0(7) . . ? Br1 Rb1 C1 59.84(13) 1_455 . ? Br1 Rb1 Br2 140.31(4) 1_455 4_655 ? Br1 Rb1 Br2 149.06(3) 1_455 4_755 ? Br1 Rb1 Br2 144.66(3) 1_455 2_664 ? Br1 Rb1 Br2 144.66(3) 1_455 2_664 ? Br1 Rb1 Br3 66.91(2) 1_455 2_564 ? Br1 Rb1 Br4 80.38(2) 1_455 . ? Br2 Rb1 Br2 56.41(2) 4_655 2_664 ? Br2 Rb1 Br2 52.20(2) 2_664 4_755 ? Br2 Rb1 Br2 68.17(2) 4_655 4_755 ? Br2 Rb1 Br3 112.67(3) 4_655 2_564 ? Br2 Rb1 Br4 95.06(3) 4_655 . ? Br2 Rb1 Br4 134.51(3) 2_664 . ? Br3 Rb1 Br2 77.81(2) 2_564 2_664 ? Br3 Rb1 Br2 120.09(3) 2_564 4_755 ? Br3 Rb1 Br4 147.00(3) 2_564 . ? Br4 Rb1 Br2 85.97(3) . 4_755 ? O1 C1 C2 123.1(8) . . ? O1 C1 C6 123.4(8) . . ? O1 C1 Rb1 36.1(5) . 1_655 ? O1 C1 Rb1 35.5(5) . . ? O1 Rb1 Br1 71.56(13) . 1_455 ? O1 Rb1 Br1 54.54(14) 1_455 1_455 ? O1 Rb1 Br2 133.58(14) . 4_655 ? O1 Rb1 Br2 87.60(14) 1_455 4_655 ? O1 Rb1 Br2 78.35(13) . 4_755 ? O1 Rb1 Br2 140.67(13) 1_455 4_755 ? O1 Rb1 Br2 122.71(13) . 2_664 ? O1 Rb1 Br2 136.19(13) 1_455 2_664 ? O1 Rb1 Br3 111.67(14) . 2_564 ? O1 Rb1 Br3 97.38(13) 1_455 2_564 ? O1 Rb1 Br4 50.17(13) . . ? O1 Rb1 Br4 65.05(12) 1_455 . ? O1 Rb1 O1 99.78(17) . 1_455 ? O1 Rb1 O2 78.80(17) . 2_664 ? O1 Rb1 O2 162.55(18) 1_455 2_664 ? O1 Rb1 O2 162.60(18) . 2_564 ? O1 Rb1 O2 77.83(17) 1_455 2_564 ? O2 C4 C3 122.9(10) . . ? O2 C4 C5 123.7(9) . . ? O2 Rb1 Br1 109.38(13) 2_664 1_455 ? O2 Rb1 Br1 93.69(12) 2_564 1_455 ? O2 Rb1 Br2 51.85(12) 2_664 2_664 ? O2 Rb1 Br2 64.74(13) 2_564 2_664 ? O2 Rb1 Br2 56.46(13) 2_664 4_755 ? O2 Rb1 Br2 114.55(13) 2_564 4_755 ? O2 Rb1 Br2 106.10(12) 2_664 4_655 ? O2 Rb1 Br2 63.80(12) 2_564 4_655 ? O2 Rb1 Br3 67.63(13) 2_664 2_564 ? O2 Rb1 Br3 52.35(12) 2_564 2_564 ? O2 Rb1 Br4 122.82(13) 2_664 . ? O2 Rb1 Br4 138.25(13) 2_564 . ? O2 Rb1 O2 98.26(15) 2_664 2_564 ? Rb1 C1 Rb1 70.84(12) . 1_655 ? Rb1 Br2 Rb1 68.17(2) 4_645 4_745 ? Rb1 Br2 Rb1 117.14(3) 2_665 4_745 ? Rb1 O1 Rb1 99.78(17) . 1_655 ? Rb1 O2 Rb1 98.26(15) 2_665 2_565 ? Rb1 Br2 Rb1 132.06(3) 4_645 2_665 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 C4 3.4(14) . . . . ? C1 C2 C3 Br2 -178.0(7) . . . . ? C1 Rb1 C1 O1 -170.5(7) 1_455 . . . ? C1 Rb1 C1 C2 98.1(8) 1_455 . . . ? C1 Rb1 C1 C6 -39.6(5) 1_455 . . . ? C1 Rb1 O1 C1 9.0(6) 1_455 . . . ? C1 Rb1 Br4 C6 -15.6(3) . . . . ? C1 Rb1 Br4 C6 82.2(3) 1_455 . . . ? C1 Rb1 O1 Rb1 168.0(9) . . . 1_655 ? C1 Rb1 O1 Rb1 177.0(2) 1_455 . . 1_655 ? C1 Rb1 C1 Rb1 180 1_455 . . 1_655 ? C2 C1 C6 C5 0.5(12) . . . . ? C2 C1 C6 Br4 -179.9(6) . . . . ? C3 C2 C1 O1 180 . . . . ? C3 C2 C1 C6 -1.7(12) . . . . ? C3 C2 C1 Rb1 -136.1(7) . . . . ? C3 C2 C1 Rb1 153.6(7) . . . 1_655 ? C3 C4 C5 C6 2.2(13) . . . . ? C3 C4 C5 Br3 -179.3(6) . . . . ? C4 C5 C6 C1 -0.9(14) . . . . ? C4 C5 C6 Br4 179.5(7) . . . . ? C5 C4 C3 C2 -3.4(13) . . . . ? C5 C4 C3 Br2 177.8(6) . . . . ? Br1 C2 C1 O1 -0.6(12) . . . . ? Br1 C2 C1 C6 177.6(6) . . . . ? Br1 C2 C1 Rb1 43.3(10) . . . . ? Br1 C2 C1 Rb1 -27.1(6) . . . 1_655 ? Br1 C2 C3 C4 -175.9(7) . . . . ? Br1 C2 C3 Br2 2.7(10) . . . . ? Br1 Rb1 C1 C2 49.2(7) 1_455 . . . ? Br1 Rb1 C1 C6 -88.5(5) 1_455 . . . ? Br1 Rb1 C1 Rb1 131.16(16) 1_455 . . 1_655 ? Br1 Rb1 O1 Rb1 132.69(19) 1_455 . . 1_655 ? Br1 Rb1 C1 O1 140.6(8) 1_455 . . . ? Br1 Rb1 Br4 C6 40.3(2) 1_455 . . . ? Br1 Rb1 O1 C1 -35.3(7) 1_455 . . . ? Rb1 Br3 C5 C6 152.1(7) 2_565 . . . ? Rb1 Br3 C5 C4 -26.4(7) 2_565 . . . ? Br2 Rb1 C1 C2 -177.9(7) 4_655 . . . ? Br2 Rb1 C1 C2 -90.4(8) 2_664 . . . ? Br2 Rb1 C1 C2 -118.8(8) 4_755 . . . ? Br2 Rb1 C1 C6 44.4(6) 4_655 . . . ? Br2 Rb1 C1 C6 103.5(5) 4_755 . . . ? Br2 Rb1 C1 C6 131.9(4) 2_664 . . . ? Br2 Rb1 C1 Rb1 -95.98(17) 4_655 . . 1_655 ? Br2 Rb1 C1 Rb1 -8.5(2) 2_664 . . 1_655 ? Br2 Rb1 C1 Rb1 -36.88(10) 4_755 . . 1_655 ? Br2 Rb1 C1 O1 -27.4(7) 4_755 . . . ? Br2 Rb1 C1 O1 -86.5(8) 4_655 . . . ? Br2 Rb1 C1 O1 1.0(8) 2_664 . . . ? Br2 Rb1 Br4 C6 -179.5(2) 4_655 . . . ? Br2 Rb1 Br4 C6 -133.2(3) 2_664 . . . ? Br2 Rb1 Br4 C6 -111.8(2) 4_755 . . . ? Br2 Rb1 O1 C1 108.0(7) 4_655 . . . ? Br2 Rb1 O1 C1 -179.2(7) 2_664 . . . ? Br2 Rb1 O1 C1 152.0(8) 4_755 . . . ? Br2 Rb1 O1 Rb1 -83.9(2) 4_655 . . 1_655 ? Br2 Rb1 O1 Rb1 -11.2(2) 2_664 . . 1_655 ? Br2 Rb1 O1 Rb1 -40.01(14) 4_755 . . 1_655 ? Br3 C5 C6 C1 -179.4(7) . . . . ? Br3 C5 C6 Br4 1.1(11) . . . . ? Br3 Rb1 C1 Rb1 86.23(11) 2_564 . . 1_655 ? Br3 Rb1 C1 O1 95.7(7) 2_564 . . . ? Br3 Rb1 C1 C2 4.3(8) 2_564 . . . ? Br3 Rb1 C1 C6 -133.4(5) 2_564 . . . ? Br3 Rb1 Br4 C6 32.7(3) 2_564 . . . ? Br3 Rb1 O1 C1 -90.1(7) 2_564 . . . ? Br3 Rb1 O1 Rb1 77.95(17) 2_564 . . 1_655 ? Br4 Rb1 C1 C2 158.5(9) . . . . ? Br4 Rb1 C1 C6 20.8(4) . . . . ? Br4 Rb1 C1 Rb1 -119.6(2) . . . 1_655 ? Br4 Rb1 C1 O1 -110.1(8) . . . . ? Br4 Rb1 O1 C1 57.5(7) . . . . ? Br4 Rb1 O1 Rb1 -134.5(2) . . . 1_655 ? O1 C1 C6 C5 178.8(9) . . . . ? O1 C1 C6 Br4 -1.6(12) . . . . ? O1 Rb1 C1 O1 -168.1(8) 1_455 . . . ? O1 Rb1 C1 C2 -91.4(11) . . . . ? O1 Rb1 C1 C2 100.5(8) 1_455 . . . ? O1 Rb1 C1 C6 130.9(10) . . . . ? O1 Rb1 C1 C6 -37.3(5) 1_455 . . . ? O1 Rb1 C1 Rb1 -9.5(7) . . . 1_655 ? O1 Rb1 C1 Rb1 -177.62(17) 1_455 . . 1_655 ? O1 Rb1 Br4 C6 -33.6(3) . . . . ? O1 Rb1 Br4 C6 95.6(3) 1_455 . . . ? O1 Rb1 O1 C1 12.0(9) 1_455 . . . ? O1 Rb1 O1 Rb1 180 1_455 . . 1_655 ? O2 C4 C3 C2 178.5(9) . . . . ? O2 C4 C5 C6 -179.8(9) . . . . ? O2 C4 C3 Br2 -0.2(13) . . . . ? O2 C4 C5 Br3 -1.2(13) . . . . ? O2 Rb1 C1 C2 -62.3(8) 2_664 . . . ? O2 Rb1 C1 C2 50.0(10) 2_564 . . . ? O2 Rb1 C1 C6 160.0(5) 2_664 . . . ? O2 Rb1 C1 C6 -87.7(6) 2_564 . . . ? O2 Rb1 C1 Rb1 19.60(15) 2_664 . . 1_655 ? O2 Rb1 C1 Rb1 131.9(4) 2_564 . . 1_655 ? O2 Rb1 C1 O1 29.1(8) 2_664 . . . ? O2 Rb1 C1 O1 141.4(7) 2_564 . . . ? O2 Rb1 Br4 C6 -66.6(3) 2_664 . . . ? O2 Rb1 Br4 C6 125.0(3) 2_564 . . . ? O2 Rb1 O1 C1 -150.3(8) 2_664 . . . ? O2 Rb1 O1 C1 -68.5(10) 2_564 . . . ? O2 Rb1 O1 Rb1 17.69(18) 2_664 . . 1_655 ? O2 Rb1 O1 Rb1 99.5(6) 2_564 . . 1_655 ? Rb1 C1 C6 C5 147.0(7) . . . . ? Rb1 C1 C6 C5 -137.7(8) 1_655 . . . ? Rb1 C1 C6 Br4 -33.4(6) . . . . ? Rb1 C1 C6 Br4 41.9(11) 1_655 . . . ? Rb1 Br1 C2 C3 -152.4(7) 1_655 . . . ? Rb1 Br1 C2 C1 28.3(7) 1_655 . . . ? Rb1 Br2 C3 C2 -71.2(7) 4_645 . . . ? Rb1 Br2 C3 C2 152.5(7) 2_665 . . . ? Rb1 Br2 C3 C2 6.8(10) 4_745 . . . ? Rb1 Br2 C3 C4 107.6(6) 4_645 . . . ? Rb1 Br2 C3 C4 -28.7(6) 2_665 . . . ? Rb1 Br2 C3 C4 -174.4(5) 4_745 . . . ? Rb1 Br4 C6 C5 -149.4(7) . . . . ? Rb1 Br4 C6 C1 31.0(6) . . . . ? Rb1 O1 C1 C2 116.0(9) . . . . ? Rb1 O1 C1 C2 -48.6(12) 1_655 . . . ? Rb1 O1 C1 C6 -62.1(11) . . . . ? Rb1 O1 C1 C6 133.2(8) 1_655 . . . ? Rb1 O1 C1 Rb1 -164.7(11) 1_655 . . . ? Rb1 O1 C1 Rb1 164.7(11) . . . 1_655 ? Rb1 O2 C4 C3 56.4(12) 2_665 . . . ? Rb1 O2 C4 C3 -129.1(8) 2_565 . . . ? Rb1 O2 C4 C5 -121.5(10) 2_665 . . . ? Rb1 O2 C4 C5 53.0(13) 2_565 . . . ? #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-05-11 at 10:40:16 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\program files\wingx\files\cifdoc.dat # CIF files read : rbcl4q-2 rbcl4q-2-teh struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_RbCl4QxMe2CO _database_code_depnum_ccdc_archive 'CCDC 815391' _audit_creation_date 2009-05-11T10:40:16-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C9 H6 Cl4 O3 Rb1' _chemical_formula_sum 'C9 H6 Cl4 O3 Rb' _chemical_formula_weight 389.41 #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.47490(10) _cell_length_b 16.96000(10) _cell_length_c 7.66630(10) _cell_angle_alpha 90 _cell_angle_beta 103.2670(10) _cell_angle_gamma 90 _cell_volume 1325.60(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5638 _cell_measurement_theta_min 2.6014 _cell_measurement_theta_max 76.0348 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.951 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 12.518 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1303 _exptl_absorpt_correction_T_max 0.2200 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.11 (release 31-10-2007 CrysAlis171 .NET) (compiled Oct 31 2007,17:16:07) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54179 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_measurement_device_type 'Oxford Xcalibur Nova' _diffrn_measurement_method ; CCD detector ; _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4323 _diffrn_radiation_probe x-ray _diffrn_reflns_number 7000 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 4.34 _diffrn_reflns_theta_max 75.0 _diffrn_reflns_theta_full 76.15 _diffrn_measured_fraction_theta_max 0.977 _diffrn_measured_fraction_theta_full 0.988 _reflns_number_total 2704 _reflns_number_gt 2519 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.0665P)^2^+0.4237P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2704 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0898 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.98 _refine_diff_density_min -1.075 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.4688 1.6079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly C1 C 0.9645(2) 0.08530(15) 0.7850(3) 0.0157(5) Uani 1 d . . . C2 C 0.9116(2) 0.01540(15) 0.6849(3) 0.0149(5) Uani 1 d . . . C3 C 0.9745(2) -0.05570(14) 0.7068(3) 0.0143(4) Uani 1 d . . . C4 C 1.1017(2) -0.06676(15) 0.8316(3) 0.0145(4) Uani 1 d . . . C5 C 1.1583(2) 0.00409(14) 0.9226(3) 0.0148(4) Uani 1 d . . . C6 C 1.0945(2) 0.07534(14) 0.9019(3) 0.0146(4) Uani 1 d . . . C7 C 0.5009(2) 0.17281(17) 0.5985(4) 0.0218(5) Uani 1 d . . . C8 C 0.4304(3) 0.1475(2) 0.7390(4) 0.0339(7) Uani 1 d . . . C9 C 0.4566(3) 0.1372(2) 0.4162(4) 0.0304(6) Uani 1 d . . . Cl1 Cl 0.76636(5) 0.02818(4) 0.52781(8) 0.01906(15) Uani 1 d . . . Cl2 Cl 0.91243(6) -0.13667(3) 0.58019(8) 0.01900(15) Uani 1 d . . . Cl3 Cl 1.31661(5) -0.00448(4) 1.04710(8) 0.02047(15) Uani 1 d . . . Cl4 Cl 1.16741(6) 0.16019(3) 1.00094(8) 0.02048(15) Uani 1 d . . . O1 O 0.90684(18) 0.15033(11) 0.7642(2) 0.0185(4) Uani 1 d . . . O2 O 1.15945(17) -0.13163(10) 0.8489(2) 0.0176(4) Uani 1 d . . . O3 O 0.58950(19) 0.22128(13) 0.6319(3) 0.0241(4) Uani 1 d . . . Rb1 Rb 0.80078(2) 0.232840(12) 0.43798(3) 0.01334(11) Uani 1 d . . . H8A H 0.4672 0.1742 0.8495 0.051 Uiso 1 calc R . . H8B H 0.4397 0.0916 0.7568 0.051 Uiso 1 calc R . . H8C H 0.339 0.1606 0.7005 0.051 Uiso 1 calc R . . H9A H 0.5087 0.1578 0.3387 0.046 Uiso 1 calc R . . H9B H 0.3661 0.15 0.3684 0.046 Uiso 1 calc R . . H9C H 0.4667 0.081 0.4245 0.046 Uiso 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 C1 0.0202(11) 0.0122(11) 0.0167(11) 0.0019(9) 0.0085(9) 0.0025(8) C2 0.0172(10) 0.0128(11) 0.0155(11) 0.0022(9) 0.0055(9) 0.0017(8) C3 0.0181(10) 0.0112(11) 0.0142(11) -0.0005(9) 0.0052(9) 0.0003(8) C4 0.0206(11) 0.0105(11) 0.0134(11) 0.0023(8) 0.0058(9) 0.0025(8) C5 0.0178(11) 0.0130(11) 0.0145(11) 0.0025(9) 0.0052(9) 0.0007(8) C6 0.0195(11) 0.0102(11) 0.0148(11) 0.0006(8) 0.0052(9) 0.0003(8) C7 0.0162(11) 0.0249(13) 0.0236(13) 0.0026(11) 0.0028(9) -0.0024(9) C9 0.0267(13) 0.0388(17) 0.0251(14) -0.0051(13) 0.0045(11) -0.0140(12) C8 0.0302(14) 0.0465(19) 0.0258(14) 0.0003(14) 0.0082(12) -0.0139(13) Cl1 0.0166(3) 0.0190(3) 0.0203(3) 0.0024(2) 0.0015(2) 0.00190(19) Cl3 0.0165(3) 0.0210(3) 0.0224(3) 0.0010(2) 0.0013(2) 0.0026(2) Cl2 0.0208(3) 0.0132(3) 0.0232(3) -0.0049(2) 0.0055(2) -0.00199(19) Cl4 0.0266(3) 0.0116(3) 0.0232(3) -0.0020(2) 0.0054(2) -0.0033(2) O1 0.0264(8) 0.0112(8) 0.0186(8) 0.0019(7) 0.0064(7) 0.0067(7) O2 0.0242(8) 0.0108(8) 0.0191(8) 0.0028(7) 0.0075(7) 0.0058(6) O3 0.0179(9) 0.0287(10) 0.0254(10) -0.0016(8) 0.0048(7) -0.0059(7) Rb1 0.01672(16) 0.00953(16) 0.01392(16) 0.00039(7) 0.00380(10) 0.00014(7) #------------------ MOLECULAR GEOMETRY --------------------------------------# _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 C1 C2 1.451(4) . ? C1 C6 1.458(3) . ? C3 C2 1.366(3) . ? C3 C4 1.464(3) . ? C3 Cl2 1.721(2) . ? C4 O2 1.248(3) . ? C5 C4 1.447(3) . ? C5 C6 1.372(3) . ? C7 O3 1.222(3) . ? C7 C8 1.502(4) . ? C7 C9 1.495(4) . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 0.96 . ? Cl1 C2 1.724(2) . ? Cl2 Rb1 3.4491(6) 3_756 ? Cl3 C5 1.719(2) . ? Cl4 C6 1.722(3) . ? O1 C1 1.250(3) . ? O1 Rb1 2.7593(18) 4_566 ? O2 Rb1 2.7956(18) 2_746 ? O2 Rb1 2.8941(18) 3_756 ? O3 Rb1 2.937(2) 4_566 ? Rb1 Cl2 3.4491(6) 3_756 ? Rb1 O1 2.7593(18) 4_565 ? Rb1 O1 2.8587(18) . ? Rb1 O2 2.7956(18) 2_756 ? Rb1 O2 2.8941(18) 3_756 ? Rb1 O3 2.937(2) 4_565 ? Rb1 O3 2.942(2) . ? 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 C1 C2 Cl1 115.81(18) . . ? C1 C6 Cl4 115.56(18) . . ? C1 O1 Rb1 143.93(16) . 4_566 ? C1 O1 Rb1 128.53(16) . . ? C2 C1 C6 114.8(2) . . ? C2 C3 C4 122.3(2) . . ? C2 C3 Cl2 121.77(19) . . ? C2 Cl1 Rb1 98.33(9) . . ? C3 C2 C1 122.8(2) . . ? C3 C2 Cl1 121.3(2) . . ? C3 Cl2 Rb1 100.40(8) . 3_756 ? C4 C3 Cl2 115.84(18) . . ? C4 C5 Cl3 115.72(18) . . ? C4 O2 Rb1 142.22(15) . 2_746 ? C4 O2 Rb1 126.40(15) . 3_756 ? C5 C4 C3 114.8(2) . . ? C5 C6 C1 122.3(2) . . ? C5 C6 Cl4 121.98(19) . . ? C6 C5 C4 122.7(2) . . ? C6 C5 Cl3 121.4(2) . . ? C7 O3 Rb1 137.92(19) . 4_566 ? C7 O3 Rb1 124.19(18) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? C9 C7 C8 117.2(2) . . ? Cl1 Rb1 Rb1 111.058(12) . 4_565 ? Cl1 Rb1 Rb1 86.123(11) . 4_566 ? Cl2 Rb1 Cl1 71.078(13) 3_756 . ? Cl2 Rb1 Rb1 107.971(11) 3_756 4_566 ? Cl2 Rb1 Rb1 80.413(11) 3_756 4_565 ? O1 C1 C2 122.6(2) . . ? O1 C1 C6 122.4(2) . . ? O1 Rb1 O1 130.93(7) 4_565 . ? O1 Rb1 O2 70.69(5) 4_565 2_756 ? O1 Rb1 O2 85.12(5) 4_565 3_756 ? O1 Rb1 O2 106.24(5) . 3_756 ? O1 Rb1 O3 74.76(6) 4_565 4_565 ? O1 Rb1 O3 154.02(6) . 4_565 ? O1 Rb1 O3 136.44(6) 4_565 . ? O1 Rb1 O3 73.24(6) . . ? O1 Rb1 Cl1 149.34(4) 4_565 . ? O1 Rb1 Cl1 52.55(4) . . ? O1 Rb1 Cl2 82.48(4) 4_565 3_756 ? O1 Rb1 Cl2 68.69(4) . 3_756 ? O2 C4 C5 123.1(2) . . ? O2 C4 C3 121.9(2) . . ? O2 Rb1 O1 85.13(5) 2_756 . ? O2 Rb1 O2 154.65(6) 2_756 3_756 ? O2 Rb1 O3 103.48(6) 2_756 4_565 ? O2 Rb1 O3 76.32(5) 3_756 4_565 ? O2 Rb1 O3 77.75(5) 2_756 . ? O2 Rb1 O3 126.91(6) 3_756 . ? O2 Rb1 Cl1 133.96(4) 2_756 . ? O2 Rb1 Cl1 66.97(4) 3_756 . ? O2 Rb1 Cl2 113.46(4) 2_756 3_756 ? O2 Rb1 Cl2 53.86(4) 3_756 3_756 ? O3 C7 C9 121.7(3) . . ? O3 C7 C8 121.1(3) . . ? O3 Rb1 O3 84.55(5) 4_565 . ? O3 Rb1 Cl1 108.69(5) 4_565 . ? O3 Rb1 Cl1 73.56(4) . . ? O3 Rb1 Cl2 138.77(4) . 3_756 ? O3 Rb1 Cl2 126.63(4) 4_565 3_756 ? Rb1 O1 Rb1 87.26(5) 4_566 . ? Rb1 O2 Rb1 85.89(5) 2_746 3_756 ? Rb1 O3 Rb1 82.52(5) 4_566 . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 C1 C6 Cl4 172.45(17) . . . . ? C2 C1 C6 C5 -3.5(3) . . . . ? C2 C3 C4 O2 -178.9(2) . . . . ? C2 C3 C4 C5 -3.0(3) . . . . ? C2 C3 Cl2 Rb1 149.07(19) . . . 3_756 ? C3 C4 O2 Rb1 47.0(3) . . . 3_756 ? C3 C4 O2 Rb1 -96.7(3) . . . 2_746 ? C4 C3 C2 C1 -0.9(4) . . . . ? C4 C3 C2 Cl1 176.25(18) . . . . ? C4 C3 Cl2 Rb1 -27.69(18) . . . 3_756 ? C4 C5 C6 C1 -0.5(4) . . . . ? C4 C5 C6 Cl4 -176.09(18) . . . . ? C5 C4 O2 Rb1 -128.6(2) . . . 3_756 ? C5 C4 O2 Rb1 87.7(3) . . . 2_746 ? C6 C1 C2 C3 4.1(3) . . . . ? C6 C1 C2 Cl1 -173.20(17) . . . . ? C6 C5 C4 O2 179.5(2) . . . . ? C6 C5 C4 C3 3.7(3) . . . . ? C8 C7 O3 Rb1 33.9(4) . . . 4_566 ? C8 C7 O3 Rb1 155.0(2) . . . . ? C9 C7 O3 Rb1 -147.2(2) . . . 4_566 ? C9 C7 O3 Rb1 -26.0(4) . . . . ? Cl1 Rb1 O1 C1 45.44(19) . . . . ? Cl1 Rb1 O3 C7 -45.1(2) . . . . ? Cl1 Rb1 O3 Rb1 99.52(4) . . . 4_566 ? Cl1 Rb1 O1 Rb1 -129.63(6) . . . 4_566 ? Cl2 C3 C2 C1 -177.49(18) . . . . ? Cl2 C3 C2 Cl1 -0.3(3) . . . . ? Cl2 C3 C4 C5 173.74(17) . . . . ? Cl2 C3 C4 O2 -2.1(3) . . . . ? Cl2 Rb1 O1 C1 -36.53(19) 3_756 . . . ? Cl2 Rb1 O1 Rb1 148.40(5) 3_756 . . 4_566 ? Cl2 Rb1 O3 C7 -77.0(2) 3_756 . . . ? Cl2 Rb1 O3 Rb1 67.69(7) 3_756 . . 4_566 ? Cl2 Rb1 Cl1 C2 48.39(8) 3_756 . . . ? Cl3 C5 C4 O2 4.0(3) . . . . ? Cl3 C5 C4 C3 -171.78(16) . . . . ? Cl3 C5 C6 C1 174.76(18) . . . . ? Cl3 C5 C6 Cl4 -0.9(3) . . . . ? O1 C1 C2 C3 179.8(2) . . . . ? O1 C1 C2 Cl1 2.5(3) . . . . ? O1 C1 C6 C5 -179.1(2) . . . . ? O1 C1 C6 Cl4 -3.2(3) . . . . ? O1 Rb1 Cl1 C2 80.22(11) 4_565 . . . ? O1 Rb1 Cl1 C2 -28.82(9) . . . . ? O1 Rb1 O1 C1 -94.92(18) 4_565 . . . ? O1 Rb1 O1 Rb1 90.01(9) 4_565 . . 4_566 ? O1 Rb1 O3 C7 127.3(2) 4_565 . . . ? O1 Rb1 O3 C7 -100.2(2) . . . . ? O1 Rb1 O3 Rb1 -88.05(8) 4_565 . . 4_566 ? O1 Rb1 O3 Rb1 44.50(5) . . . 4_566 ? O2 Rb1 O1 C1 -154.0(2) 2_756 . . . ? O2 Rb1 O1 C1 2.9(2) 3_756 . . . ? O2 Rb1 O1 Rb1 30.88(5) 2_756 . . 4_566 ? O2 Rb1 O1 Rb1 -172.22(5) 3_756 . . 4_566 ? O2 Rb1 O3 C7 171.3(2) 2_756 . . . ? O2 Rb1 O3 C7 -2.2(2) 3_756 . . . ? O2 Rb1 O3 Rb1 142.49(5) 3_756 . . 4_566 ? O2 Rb1 O3 Rb1 -44.05(5) 2_756 . . 4_566 ? O2 Rb1 Cl1 C2 -56.33(10) 2_756 . . . ? O2 Rb1 Cl1 C2 106.27(9) 3_756 . . . ? O3 Rb1 O1 C1 94.9(2) 4_565 . . . ? O3 Rb1 O1 C1 127.3(2) . . . . ? O3 Rb1 O1 Rb1 -80.19(13) 4_565 . . 4_566 ? O3 Rb1 O1 Rb1 -47.78(5) . . . 4_566 ? O3 Rb1 O3 C7 66.19(19) 4_565 . . . ? O3 Rb1 O3 Rb1 -149.14(9) 4_565 . . 4_566 ? O3 Rb1 Cl1 C2 171.74(9) 4_565 . . . ? O3 Rb1 Cl1 C2 -110.04(9) . . . . ? Rb1 Cl1 C2 C3 -150.99(19) . . . . ? Rb1 Cl1 C2 C1 26.39(18) . . . . ? Rb1 O1 C1 C2 121.5(3) 4_566 . . . ? Rb1 O1 C1 C2 -50.1(3) . . . . ? Rb1 O1 C1 C6 -63.1(4) 4_566 . . . ? Rb1 O1 C1 C6 125.2(2) . . . . ?