#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/1/1100849.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100849 _chemical_formula_sum 'C20 H35 B4 Cl3 Ru2' _chemical_formula_weight 627.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.5503(4) _cell_length_b 13.9118(5) _cell_length_c 17.6855(7) _cell_angle_alpha 90.00 _cell_angle_beta 105.0630(10) _cell_angle_gamma 90.00 _cell_volume 2506.58(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8780 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 28.29 _exptl_crystal_description rectangular _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 1.531 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9141 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26582 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 28.31 _reflns_number_total 6228 _reflns_number_gt 5712 _reflns_threshold_expression >2sigma(I) _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^)+(0.0312P)^2^+1.8061P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, except difmap for M-H' _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6228 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0256 _refine_ls_R_factor_gt 0.0228 _refine_ls_wR_factor_ref 0.0589 _refine_ls_wR_factor_gt 0.0575 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.465532(14) 0.394409(11) 0.270331(8) 0.01292(5) Uani 1 1 d . . . Cl1 Cl 0.20009(5) 0.50750(4) 0.12306(3) 0.02264(10) Uani 1 1 d . . . C1 C 0.34484(19) 0.44528(15) 0.34647(11) 0.0191(4) Uani 1 1 d . . . B1 B 0.3627(2) 0.45712(15) 0.15531(13) 0.0153(4) Uani 1 1 d . . . H1 H 0.4377 0.4978 0.2176 0.018 Uiso 1 1 d R . . Ru2 Ru 0.602636(14) 0.315078(11) 0.163249(8) 0.01293(5) Uani 1 1 d . . . H5 H 0.6190 0.3990 0.2430 0.016 Uiso 1 1 d R . . Cl2 Cl 0.38099(5) 0.40164(4) -0.01695(3) 0.02031(10) Uani 1 1 d . . . C2 C 0.34945(19) 0.34279(15) 0.34871(11) 0.0184(4) Uani 1 1 d . . . B2 B 0.4486(2) 0.40628(15) 0.08815(12) 0.0155(4) Uani 1 1 d . . . H3 H 0.5670 0.4187 0.1106 0.019 Uiso 1 1 d R . . H2 H 0.4264 0.4949 0.1073 0.019 Uiso 1 1 d R . . Cl3 Cl 0.24154(4) 0.25963(3) 0.10786(3) 0.01892(10) Uani 1 1 d . . . B3 B 0.3883(2) 0.33335(15) 0.15090(12) 0.0142(4) Uani 1 1 d . . . C3 C 0.4844(2) 0.31376(15) 0.38155(11) 0.0188(4) Uani 1 1 d . . . B4 B 0.4840(2) 0.26005(16) 0.22732(13) 0.0157(4) Uani 1 1 d . . . H4 H 0.4388 0.1556 0.2535 0.019 Uiso 1 1 d R . . C4 C 0.56166(19) 0.40018(15) 0.39931(11) 0.0191(4) Uani 1 1 d . . . C5 C 0.4777(2) 0.48057(15) 0.37831(11) 0.0197(4) Uani 1 1 d . . . C6 C 0.2226(2) 0.50477(17) 0.32371(13) 0.0251(4) Uani 1 1 d . . . H6A H 0.1898 0.5164 0.3699 0.030 Uiso 1 1 calc R . . H6B H 0.1557 0.4705 0.2840 0.030 Uiso 1 1 calc R . . H6C H 0.2422 0.5663 0.3023 0.030 Uiso 1 1 calc R . . C7 C 0.2321(2) 0.27822(16) 0.32226(12) 0.0227(4) Uani 1 1 d . . . H7A H 0.1956 0.2642 0.3667 0.027 Uiso 1 1 calc R . . H7B H 0.2586 0.2181 0.3019 0.027 Uiso 1 1 calc R . . H7C H 0.1654 0.3103 0.2809 0.027 Uiso 1 1 calc R . . C8 C 0.5323(2) 0.21436(16) 0.40618(13) 0.0250(4) Uani 1 1 d . . . H8A H 0.5268 0.2028 0.4599 0.030 Uiso 1 1 calc R . . H8B H 0.6236 0.2079 0.4037 0.030 Uiso 1 1 calc R . . H8C H 0.4776 0.1674 0.3710 0.030 Uiso 1 1 calc R . . C9 C 0.7060(2) 0.40344(17) 0.43908(12) 0.0241(4) Uani 1 1 d . . . H9A H 0.7187 0.4059 0.4959 0.029 Uiso 1 1 calc R . . H9B H 0.7447 0.4608 0.4219 0.029 Uiso 1 1 calc R . . H9C H 0.7486 0.3458 0.4253 0.029 Uiso 1 1 calc R . . C10 C 0.5164(2) 0.58383(16) 0.39257(13) 0.0252(4) Uani 1 1 d . . . H10A H 0.5125 0.6022 0.4454 0.030 Uiso 1 1 calc R . . H10B H 0.4560 0.6242 0.3540 0.030 Uiso 1 1 calc R . . H10C H 0.6060 0.5927 0.3876 0.030 Uiso 1 1 calc R . . C21 C 0.6511(2) 0.19185(15) 0.09737(14) 0.0241(4) Uani 1 1 d . . . C22 C 0.7227(2) 0.27379(16) 0.08391(12) 0.0209(4) Uani 1 1 d . . . C23 C 0.81049(19) 0.30301(15) 0.15699(12) 0.0186(4) Uani 1 1 d . . . C24 C 0.79170(19) 0.23902(16) 0.21548(12) 0.0211(4) Uani 1 1 d . . . C25 C 0.6942(2) 0.16982(15) 0.17926(14) 0.0235(4) Uani 1 1 d . . . C26 C 0.5536(3) 0.1361(2) 0.03537(18) 0.0411(7) Uani 1 1 d . . . H26A H 0.5994 0.0850 0.0149 0.049 Uiso 1 1 calc R . . H26B H 0.5110 0.1794 -0.0073 0.049 Uiso 1 1 calc R . . H26C H 0.4872 0.1076 0.0583 0.049 Uiso 1 1 calc R . . C27 C 0.7170(3) 0.3200(2) 0.00630(14) 0.0353(6) Uani 1 1 d . . . H27A H 0.7804 0.2888 -0.0175 0.042 Uiso 1 1 calc R . . H27B H 0.7383 0.3884 0.0141 0.042 Uiso 1 1 calc R . . H27C H 0.6284 0.3128 -0.0283 0.042 Uiso 1 1 calc R . . C28 C 0.9117(2) 0.38068(17) 0.16604(16) 0.0306(5) Uani 1 1 d . . . H28A H 0.9940 0.3531 0.1601 0.037 Uiso 1 1 calc R . . H28B H 0.9265 0.4098 0.2181 0.037 Uiso 1 1 calc R . . H28C H 0.8808 0.4300 0.1259 0.037 Uiso 1 1 calc R . . C29 C 0.8683(2) 0.2370(2) 0.29979(14) 0.0351(6) Uani 1 1 d . . . H29A H 0.9475 0.1979 0.3052 0.042 Uiso 1 1 calc R . . H29B H 0.8141 0.2092 0.3316 0.042 Uiso 1 1 calc R . . H29C H 0.8934 0.3027 0.3176 0.042 Uiso 1 1 calc R . . C30 C 0.6616(3) 0.08028(18) 0.21762(19) 0.0403(7) Uani 1 1 d . . . H30A H 0.7236 0.0293 0.2136 0.048 Uiso 1 1 calc R . . H30B H 0.5722 0.0597 0.1914 0.048 Uiso 1 1 calc R . . H30C H 0.6679 0.0934 0.2729 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01261(8) 0.01407(8) 0.01186(8) -0.00005(5) 0.00279(5) -0.00193(5) Cl1 0.0197(2) 0.0218(2) 0.0266(3) 0.00432(19) 0.00635(19) 0.00553(18) C1 0.0175(9) 0.0256(10) 0.0155(9) -0.0029(8) 0.0068(7) -0.0025(8) B1 0.0149(10) 0.0136(10) 0.0174(10) 0.0017(8) 0.0040(8) 0.0014(8) Ru2 0.01245(8) 0.01306(8) 0.01316(8) 0.00118(5) 0.00311(6) 0.00011(5) Cl2 0.0229(2) 0.0231(2) 0.0137(2) 0.00194(17) 0.00258(18) -0.00125(18) C2 0.0169(9) 0.0246(10) 0.0141(9) 0.0008(8) 0.0047(7) -0.0041(8) B2 0.0164(10) 0.0159(10) 0.0140(9) 0.0003(8) 0.0037(8) 0.0001(8) Cl3 0.0170(2) 0.0192(2) 0.0182(2) -0.00051(17) 0.00043(17) -0.00506(17) B3 0.0129(9) 0.0148(9) 0.0146(9) 0.0004(8) 0.0030(8) -0.0018(8) C3 0.0180(9) 0.0259(10) 0.0119(9) 0.0025(7) 0.0027(7) -0.0042(8) B4 0.0132(9) 0.0169(10) 0.0157(10) -0.0001(8) 0.0014(8) 0.0007(8) C4 0.0160(9) 0.0291(11) 0.0115(9) -0.0007(8) 0.0025(7) -0.0060(8) C5 0.0214(10) 0.0244(10) 0.0149(9) -0.0052(8) 0.0074(7) -0.0070(8) C6 0.0201(10) 0.0297(11) 0.0272(11) -0.0061(9) 0.0093(9) 0.0011(8) C7 0.0183(10) 0.0285(11) 0.0205(10) 0.0023(8) 0.0036(8) -0.0072(8) C8 0.0235(10) 0.0282(11) 0.0207(10) 0.0092(9) 0.0010(8) -0.0042(9) C9 0.0193(10) 0.0335(12) 0.0166(10) 0.0023(8) -0.0003(8) -0.0075(9) C10 0.0252(11) 0.0258(11) 0.0260(11) -0.0098(9) 0.0093(9) -0.0063(9) C21 0.0180(10) 0.0198(10) 0.0326(12) -0.0061(9) 0.0032(9) 0.0048(8) C22 0.0213(10) 0.0234(10) 0.0188(10) -0.0007(8) 0.0065(8) 0.0067(8) C23 0.0150(9) 0.0205(10) 0.0221(10) -0.0025(8) 0.0077(8) 0.0014(7) C24 0.0163(9) 0.0267(11) 0.0204(10) 0.0025(8) 0.0046(8) 0.0066(8) C25 0.0178(10) 0.0182(10) 0.0365(12) 0.0066(9) 0.0110(9) 0.0069(8) C26 0.0288(12) 0.0311(13) 0.0555(17) -0.0223(12) -0.0034(12) 0.0060(10) C27 0.0417(14) 0.0464(15) 0.0217(11) 0.0063(10) 0.0151(10) 0.0176(12) C28 0.0226(11) 0.0276(12) 0.0450(14) -0.0069(10) 0.0147(10) -0.0057(9) C29 0.0229(11) 0.0582(17) 0.0220(11) 0.0051(11) 0.0021(9) 0.0122(11) C30 0.0314(13) 0.0236(12) 0.071(2) 0.0184(12) 0.0221(13) 0.0098(10)