#------------------------------------------------------------------------------ #$Date: 2016-02-20 16:35:30 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176787 $ #$URL: svn://www.crystallography.net/cod/cif/2/21/43/2214328.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2214328 loop_ _publ_author_name 'Fang-Fang Su' 'Jian-Min Dou' 'Da-Cheng Li' 'Da-Qi Wang' _publ_section_title ; 1,2-Bis(dicyclohexylphosphino)-1,2-dicarba-closo-dodecaborane ; _journal_coeditor_code LH2435 _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o3335 _journal_page_last o3335 _journal_paper_doi 10.1107/S1600536807030553 _journal_volume 63 _journal_year 2007 _chemical_formula_iupac 'C26 H54 B10 P2' _chemical_formula_moiety 'C26 H54 B10 P2' _chemical_formula_sum 'C26 H54 B10 P2' _chemical_formula_weight 536.73 _chemical_name_systematic ; 1,2-Bis(dicyclohexylphosphino)-1,2-dicarba-closo-dodecaborane ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 103.196(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 21.507(2) _cell_length_b 10.0350(14) _cell_length_c 15.2976(18) _cell_measurement_reflns_used 1912 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 26.820 _cell_measurement_theta_min 2.251 _cell_volume 3214.4(7) _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_collection 'SMART (Bruker, 1998)' _computing_data_reduction SAINT _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997b)' _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997a)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997a)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.969 _diffrn_measured_fraction_theta_max 0.969 _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method '\f and \w' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0814 _diffrn_reflns_av_sigmaI/netI 0.0906 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 6226 _diffrn_reflns_theta_full 25.01 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_min 2.25 _exptl_absorpt_coefficient_mu 0.152 _exptl_absorpt_correction_T_max 0.9335 _exptl_absorpt_correction_T_min 0.9172 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.109 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1160 _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.57 _exptl_crystal_size_min 0.46 _refine_diff_density_max 0.841 _refine_diff_density_min -0.263 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 172 _refine_ls_number_reflns 2743 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.002 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0631 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.095P)^2^+4.2002P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1571 _refine_ls_wR_factor_ref 0.1967 _reflns_number_gt 1814 _reflns_number_total 2743 _reflns_threshold_expression I>2\s(I) _cod_data_source_file lh2435.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2214328 _cod_database_fobs_code 2214328 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy P P1 0.42512(4) 0.27894(9) 0.24958(6) 0.0338(3) Uani d . 1 B B1 0.43839(18) 0.5863(4) 0.2987(3) 0.0430(10) Uani d . 1 H H1 0.3976 0.5852 0.3308 0.052 Uiso calc R 1 B B2 0.42621(18) 0.5876(4) 0.1819(3) 0.0449(10) Uani d . 1 H H2 0.3780 0.5879 0.1379 0.054 Uiso calc R 1 B B3 0.49093(16) 0.4982(4) 0.1542(3) 0.0369(9) Uani d . 1 H H3 0.4852 0.4392 0.0923 0.044 Uiso calc R 1 B B4 0.4907(2) 0.6734(4) 0.1540(3) 0.0507(11) Uani d . 1 H H4 0.4848 0.7297 0.0909 0.061 Uiso calc R 1 B B5 0.4581(2) 0.7292(4) 0.2444(3) 0.0533(12) Uani d . 1 H H5 0.4310 0.8228 0.2410 0.064 Uiso calc R 1 C C1 0.45992(3) 0.4513(3) 0.2439(2) 0.0322(7) Uani d D 1 C C2 0.34879(14) 0.3209(4) 0.2810(2) 0.0376(8) Uani d . 1 H H2A 0.3332 0.4063 0.2534 0.045 Uiso calc R 1 C C3 0.29691(16) 0.2158(4) 0.2520(2) 0.0491(10) Uani d . 1 H H3A 0.2880 0.2056 0.1872 0.059 Uiso calc R 1 H H3B 0.3121 0.1308 0.2788 0.059 Uiso calc R 1 C C4 0.23611(17) 0.2539(5) 0.2798(3) 0.0585(12) Uani d . 1 H H4A 0.2048 0.1837 0.2621 0.070 Uiso calc R 1 H H4B 0.2189 0.3346 0.2485 0.070 Uiso calc R 1 C C5 0.24694(19) 0.2765(5) 0.3802(3) 0.0596(11) Uani d . 1 H H5A 0.2079 0.3091 0.3943 0.071 Uiso calc R 1 H H5B 0.2581 0.1928 0.4116 0.071 Uiso calc R 1 C C6 0.30009(18) 0.3768(4) 0.4113(3) 0.0579(11) Uani d . 1 H H6A 0.3089 0.3847 0.4762 0.070 Uiso calc R 1 H H6B 0.2866 0.4634 0.3858 0.070 Uiso calc R 1 C C7 0.36042(16) 0.3344(4) 0.3831(2) 0.0469(9) Uani d . 1 H H7A 0.3750 0.2497 0.4110 0.056 Uiso calc R 1 H H7B 0.3937 0.3998 0.4040 0.056 Uiso calc R 1 C C8 0.40569(16) 0.2213(4) 0.1319(2) 0.0411(8) Uani d . 1 H H8 0.4456 0.2351 0.1124 0.049 Uiso calc R 1 C C9 0.35584(16) 0.2903(4) 0.0595(2) 0.0421(9) Uani d . 1 H H9A 0.3146 0.2842 0.0749 0.050 Uiso calc R 1 H H9B 0.3667 0.3839 0.0579 0.050 Uiso calc R 1 C C10 0.3510(3) 0.2312(5) -0.0312(3) 0.0753(14) Uani d . 1 H H10A 0.3147 0.2705 -0.0727 0.090 Uiso calc R 1 H H10B 0.3891 0.2541 -0.0518 0.090 Uiso calc R 1 C C11 0.3436(3) 0.0868(6) -0.0332(3) 0.104(2) Uani d . 1 H H11A 0.3444 0.0544 -0.0927 0.124 Uiso calc R 1 H H11B 0.3024 0.0642 -0.0216 0.124 Uiso calc R 1 C C12 0.3957(3) 0.0175(5) 0.0354(3) 0.0798(15) Uani d . 1 H H12A 0.4366 0.0311 0.0203 0.096 Uiso calc R 1 H H12B 0.3873 -0.0775 0.0346 0.096 Uiso calc R 1 C C13 0.3979(2) 0.0735(4) 0.1297(3) 0.0677(12) Uani d . 1 H H13A 0.3588 0.0504 0.1475 0.081 Uiso calc R 1 H H13B 0.4333 0.0333 0.1725 0.081 Uiso calc R 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 P1 0.0271(4) 0.0393(5) 0.0346(5) -0.0027(3) 0.0062(3) 0.0053(4) B1 0.0341(19) 0.043(2) 0.055(3) 0.0033(16) 0.0179(17) -0.006(2) B2 0.0306(19) 0.047(2) 0.059(3) 0.0054(17) 0.0147(17) 0.013(2) B3 0.0304(17) 0.043(2) 0.040(2) 0.0035(16) 0.0118(15) 0.0096(17) B4 0.045(2) 0.041(2) 0.070(3) 0.0025(19) 0.022(2) 0.015(2) B5 0.046(2) 0.040(2) 0.079(4) 0.0055(19) 0.026(2) 0.001(2) C1 0.0214(15) 0.0375(18) 0.0391(19) -0.0004(13) 0.0103(12) 0.0026(14) C2 0.0266(15) 0.052(2) 0.0353(19) -0.0063(14) 0.0096(13) 0.0050(16) C3 0.0410(19) 0.069(3) 0.040(2) -0.0186(18) 0.0134(15) 0.0007(18) C4 0.0346(19) 0.093(3) 0.051(3) -0.0203(19) 0.0150(17) -0.003(2) C5 0.048(2) 0.081(3) 0.058(3) -0.015(2) 0.0298(18) -0.003(2) C6 0.059(2) 0.075(3) 0.046(2) -0.016(2) 0.0254(18) -0.008(2) C7 0.0398(18) 0.062(2) 0.038(2) -0.0123(17) 0.0089(15) 0.0043(18) C8 0.0354(17) 0.048(2) 0.040(2) 0.0072(15) 0.0083(14) 0.0042(16) C9 0.0398(18) 0.049(2) 0.036(2) -0.0035(16) 0.0053(14) 0.0078(16) C10 0.091(3) 0.082(3) 0.047(3) 0.007(3) 0.003(2) -0.003(2) C11 0.157(6) 0.081(4) 0.055(3) -0.005(4) -0.013(3) -0.018(3) C12 0.111(4) 0.056(3) 0.066(3) 0.007(3) 0.007(3) -0.015(2) C13 0.076(3) 0.054(3) 0.071(3) -0.004(2) 0.012(2) -0.003(2) 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' P P 0.1023 0.0942 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle C8 P1 C2 . . 107.84(15) C8 P1 C1 . . 104.18(15) C2 P1 C1 . . 100.73(13) C1 B1 B2 . . 59.9(2) C1 B1 B5 . . 107.0(3) B2 B1 B5 . . 60.4(2) C1 B1 B4 . 2_655 106.8(2) B2 B1 B4 . 2_655 109.3(3) B5 B1 B4 . 2_655 60.7(3) C1 B1 B3 . 2_655 59.93(19) B2 B1 B3 . 2_655 109.6(3) B5 B1 B3 . 2_655 108.9(3) B4 B1 B3 2_655 2_655 59.8(2) C1 B1 H1 . . 122.9 B2 B1 H1 . . 120.6 B5 B1 H1 . . 121.5 B4 B1 H1 2_655 . 121.7 B3 B1 H1 2_655 . 121.0 C1 B2 B1 . . 59.1(2) C1 B2 B5 . . 106.1(3) B1 B2 B5 . . 60.1(2) C1 B2 B4 . . 105.3(2) B1 B2 B4 . . 108.0(3) B5 B2 B4 . . 60.5(3) C1 B2 B3 . . 58.67(19) B1 B2 B3 . . 107.2(3) B5 B2 B3 . . 107.8(3) B4 B2 B3 . . 59.3(2) C1 B2 H2 . . 123.9 B1 B2 H2 . . 121.7 B5 B2 H2 . . 121.7 B4 B2 H2 . . 122.3 B3 B2 H2 . . 122.3 C1 B3 C1 . 2_655 58.54(13) C1 B3 B4 . . 105.9(3) C1 B3 B4 2_655 . 105.9(3) C1 B3 B1 . 2_655 105.4(3) C1 B3 B1 2_655 2_655 58.6(2) B4 B3 B1 . 2_655 60.1(2) C1 B3 B2 . . 59.0(2) C1 B3 B2 2_655 . 105.7(3) B4 B3 B2 . . 59.8(2) B1 B3 B2 2_655 . 107.3(3) C1 B3 H3 . . 123.5 C1 B3 H3 2_655 . 123.5 B4 B3 H3 . . 122.4 B1 B3 H3 2_655 . 122.5 B2 B3 H3 . . 122.3 B3 B4 B1 . 2_655 60.1(2) B3 B4 B2 . . 60.9(2) B1 B4 B2 2_655 . 108.2(3) B3 B4 B5 . 2_655 108.2(3) B1 B4 B5 2_655 2_655 59.5(2) B2 B4 B5 . 2_655 107.8(3) B3 B4 B5 . . 108.3(3) B1 B4 B5 2_655 . 107.1(3) B2 B4 B5 . . 59.6(3) B5 B4 B5 2_655 . 59.7(3) B3 B4 H4 . . 121.1 B1 B4 H4 2_655 . 122.1 B2 B4 H4 . . 121.5 B5 B4 H4 2_655 . 122.0 B5 B4 H4 . . 122.2 B1 B5 B2 . . 59.5(2) B1 B5 B5 . 2_655 107.7(3) B2 B5 B5 . 2_655 108.3(3) B1 B5 B4 . 2_655 59.8(2) B2 B5 B4 . 2_655 107.9(3) B5 B5 B4 2_655 2_655 60.2(3) B1 B5 B4 . . 106.9(3) B2 B5 B4 . . 59.8(2) B5 B5 B4 2_655 . 60.1(3) B4 B5 B4 2_655 . 107.8(3) B1 B5 H5 . . 122.4 B2 B5 H5 . . 121.7 B5 B5 H5 2_655 . 121.4 B4 B5 H5 2_655 . 121.7 B4 B5 H5 . . 122.1 C1 C1 B1 2_655 . 109.19(19) C1 C1 B3 2_655 . 61.16(19) B1 C1 B3 . . 111.8(3) C1 C1 B2 2_655 . 110.50(19) B1 C1 B2 . . 61.0(2) B3 C1 B2 . . 62.4(2) C1 C1 B3 2_655 2_655 60.30(19) B1 C1 B3 . 2_655 61.5(2) B3 C1 B3 . 2_655 112.0(2) B2 C1 B3 . 2_655 111.8(3) C1 C1 P1 2_655 . 113.48(5) B1 C1 P1 . . 123.10(18) B3 C1 P1 . . 121.0(2) B2 C1 P1 . . 128.88(17) B3 C1 P1 2_655 . 111.8(2) C3 C2 C7 . . 107.3(3) C3 C2 P1 . . 113.4(3) C7 C2 P1 . . 109.6(2) C3 C2 H2A . . 108.8 C7 C2 H2A . . 108.8 P1 C2 H2A . . 108.8 C4 C3 C2 . . 111.4(3) C4 C3 H3A . . 109.4 C2 C3 H3A . . 109.4 C4 C3 H3B . . 109.4 C2 C3 H3B . . 109.4 H3A C3 H3B . . 108.0 C3 C4 C5 . . 112.3(3) C3 C4 H4A . . 109.1 C5 C4 H4A . . 109.1 C3 C4 H4B . . 109.1 C5 C4 H4B . . 109.1 H4A C4 H4B . . 107.9 C6 C5 C4 . . 110.4(3) C6 C5 H5A . . 109.6 C4 C5 H5A . . 109.6 C6 C5 H5B . . 109.6 C4 C5 H5B . . 109.6 H5A C5 H5B . . 108.1 C5 C6 C7 . . 110.9(3) C5 C6 H6A . . 109.5 C7 C6 H6A . . 109.5 C5 C6 H6B . . 109.5 C7 C6 H6B . . 109.5 H6A C6 H6B . . 108.1 C6 C7 C2 . . 111.3(3) C6 C7 H7A . . 109.4 C2 C7 H7A . . 109.4 C6 C7 H7B . . 109.4 C2 C7 H7B . . 109.4 H7A C7 H7B . . 108.0 C13 C8 C9 . . 112.3(3) C13 C8 P1 . . 109.4(3) C9 C8 P1 . . 122.2(3) C13 C8 H8 . . 103.6 C9 C8 H8 . . 103.6 P1 C8 H8 . . 103.6 C10 C9 C8 . . 112.7(3) C10 C9 H9A . . 109.1 C8 C9 H9A . . 109.1 C10 C9 H9B . . 109.1 C8 C9 H9B . . 109.1 H9A C9 H9B . . 107.8 C11 C10 C9 . . 113.5(4) C11 C10 H10A . . 108.9 C9 C10 H10A . . 108.9 C11 C10 H10B . . 108.9 C9 C10 H10B . . 108.9 H10A C10 H10B . . 107.7 C10 C11 C12 . . 112.5(4) C10 C11 H11A . . 109.1 C12 C11 H11A . . 109.1 C10 C11 H11B . . 109.1 C12 C11 H11B . . 109.1 H11A C11 H11B . . 107.8 C11 C12 C13 . . 110.0(4) C11 C12 H12A . . 109.7 C13 C12 H12A . . 109.7 C11 C12 H12B . . 109.7 C13 C12 H12B . . 109.7 H12A C12 H12B . . 108.2 C8 C13 C12 . . 111.3(4) C8 C13 H13A . . 109.4 C12 C13 H13A . . 109.4 C8 C13 H13B . . 109.4 C12 C13 H13B . . 109.4 H13A C13 H13B . . 108.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance P1 C8 . 1.845(4) P1 C2 . 1.861(3) P1 C1 . 1.894(3) B1 C1 . 1.712(5) B1 B2 . 1.747(6) B1 B5 . 1.757(6) B1 B4 2_655 1.762(6) B1 B3 2_655 1.764(5) B1 H1 . 1.1000 B2 C1 . 1.727(5) B2 B5 . 1.762(6) B2 B4 . 1.766(6) B2 B3 . 1.786(5) B2 H2 . 1.1000 B3 C1 . 1.722(5) B3 C1 2_655 1.737(5) B3 B4 . 1.758(6) B3 B1 2_655 1.764(5) B3 H3 . 1.1000 B4 B1 2_655 1.762(6) B4 B5 2_655 1.778(7) B4 B5 . 1.779(7) B4 H4 . 1.1000 B5 B5 2_655 1.771(8) B5 B4 2_655 1.778(7) B5 H5 . 1.1000 C1 C1 2_655 1.6911(10) C1 B3 2_655 1.737(5) C2 C3 . 1.526(5) C2 C7 . 1.530(5) C2 H2A . 0.9800 C3 C4 . 1.514(5) C3 H3A . 0.9700 C3 H3B . 0.9700 C4 C5 . 1.517(6) C4 H4A . 0.9700 C4 H4B . 0.9700 C5 C6 . 1.516(5) C5 H5A . 0.9700 C5 H5B . 0.9700 C6 C7 . 1.519(5) C6 H6A . 0.9700 C6 H6B . 0.9700 C7 H7A . 0.9700 C7 H7B . 0.9700 C8 C13 . 1.493(6) C8 C9 . 1.521(5) C8 H8 . 0.9800 C9 C10 . 1.491(6) C9 H9A . 0.9700 C9 H9B . 0.9700 C10 C11 . 1.458(7) C10 H10A . 0.9700 C10 H10B . 0.9700 C11 C12 . 1.517(7) C11 H11A . 0.9700 C11 H11B . 0.9700 C12 C13 . 1.539(6) C12 H12A . 0.9700 C12 H12B . 0.9700 C13 H13A . 0.9700 C13 H13B . 0.9700