#------------------------------------------------------------------------------ #$Date: 2012-03-26 00:42:28 +0200 (Mon, 26 Mar 2012) $ #$Revision: 47583 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/15/4001511.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_4001511 loop_ _publ_author_name 'Wei, Xiaolan' 'Carroll, Patrick J.' 'Sneddon, Larry G.' _publ_section_title ; Ruthenium-Catalyzed Ring-Opening Polymerization Syntheses of Poly(organodecaboranes):  New Single-Source Boron-Carbide Precursors ; _journal_issue 5 _journal_name_full 'Chemistry of Materials' _journal_page_first 1113 _journal_volume 18 _journal_year 2006 _chemical_formula_sum 'C6 H22 B10' _chemical_formula_weight 202.34 _space_group_IT_number 29 _symmetry_cell_setting orthorhombic _symmetry_Int_Tables_number 29 _symmetry_space_group_name_Hall 'P 2c -2ac' _symmetry_space_group_name_H-M 'P c a 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 10.969(4) _cell_length_b 21.912(8) _cell_length_c 10.902(4) _cell_measurement_temperature 143(1) _cell_volume 2620.3(17) _computing_data_collection 'CrystalClear (Rigaku, 1999)' _computing_data_reduction 'CrystalClear (Rigaku, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SIR97 (Altomare, 1999)' _diffrn_ambient_temperature 143(1) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device 'CCD Area Detector' _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method 'phi and omega rotations' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'rotating anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.1102 _diffrn_reflns_av_sigmaI/netI 0.1364 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 8440 _diffrn_reflns_theta_full 25.35 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_min 2.63 _exptl_absorpt_coefficient_mu 0.045 _exptl_absorpt_correction_type none _exptl_crystal_density_diffrn 1.026 _exptl_crystal_F_000 864 _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.464 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.101 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 290 _refine_ls_number_reflns 3830 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.1600 _refine_ls_R_factor_gt 0.1290 _refine_ls_shift/su_max 0.045 _refine_ls_shift/su_mean 0.005 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1802P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2905 _refine_ls_wR_factor_ref 0.3198 _reflns_number_gt 2439 _reflns_number_total 3830 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file cm0524603si20051104_125740.cif _[local]_cod_data_source_block UP3250 _[local]_cod_cif_authors_sg_H-M 'P c a 21 ' _cod_original_cell_volume 2620.4(16) _cod_database_code 4001511 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' '-x, -y, z+1/2' 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 B1 B 0.3429(6) 0.0989(3) 0.1163(7) 0.0399(16) Uani 1 1 d . B2 B 0.4083(6) 0.1610(3) 0.1961(8) 0.0429(18) Uani 1 1 d . B3 B 0.4766(6) 0.0874(3) 0.2069(8) 0.0405(18) Uani 1 1 d . B4 B 0.3710(6) 0.0259(3) 0.1837(7) 0.0397(17) Uani 1 1 d . B5 B 0.2468(5) 0.1485(3) 0.1988(7) 0.0348(16) Uani 1 1 d . B6 B 0.3259(6) 0.1802(3) 0.3275(7) 0.0390(16) Uani 1 1 d . B7 B 0.4601(6) 0.1312(3) 0.3401(8) 0.0448(18) Uani 1 1 d . B8 B 0.4365(6) 0.0430(3) 0.3307(8) 0.0434(18) Uani 1 1 d . B9 B 0.2814(6) 0.0151(3) 0.3132(8) 0.0453(19) Uani 1 1 d . B10 B 0.2219(6) 0.0593(3) 0.1894(8) 0.0447(19) Uani 1 1 d . C1 C 0.3016(5) 0.2427(2) 0.3905(7) 0.0414(15) Uani 1 1 d . H1A H 0.2424 0.2348 0.4559 0.055 Uiso 1 1 calc R C2 C 0.4152(5) 0.2701(2) 0.4537(6) 0.0409(15) Uani 1 1 d . H2A H 0.4385 0.2441 0.5218 0.054 Uiso 1 1 calc R H2B H 0.4823 0.2706 0.3957 0.054 Uiso 1 1 calc R C3 C 0.3951(6) 0.3326(3) 0.4996(7) 0.0512(17) Uani 1 1 d . H3A H 0.4501 0.3489 0.5557 0.068 Uiso 1 1 calc R C4 C 0.3002(6) 0.3670(3) 0.4635(7) 0.0511(18) Uani 1 1 d . H4A H 0.2926 0.4059 0.4969 0.068 Uiso 1 1 calc R C5 C 0.2085(6) 0.3474(3) 0.3754(8) 0.061(2) Uani 1 1 d . H5A H 0.1957 0.3796 0.3159 0.080 Uiso 1 1 calc R H5B H 0.1321 0.3406 0.4181 0.080 Uiso 1 1 calc R C6 C 0.2443(6) 0.2891(2) 0.3081(7) 0.0492(17) Uani 1 1 d . H6A H 0.1722 0.2715 0.2707 0.065 Uiso 1 1 calc R H6B H 0.3010 0.2992 0.2430 0.065 Uiso 1 1 calc R C1' C 0.2809(7) 0.7406(3) 0.2601(8) 0.060(2) Uani 1 1 d . H1A' H 0.2239 0.7552 0.3227 0.080 Uiso 1 1 calc R C2' C 0.4053(7) 0.7400(3) 0.3216(10) 0.079(3) Uani 1 1 d . H2A' H 0.4025 0.7148 0.3946 0.105 Uiso 1 1 calc R H2B' H 0.4654 0.7229 0.2661 0.105 Uiso 1 1 calc R C3' C 0.4408(8) 0.8039(3) 0.3555(8) 0.072(2) Uani 1 1 d . H3A' H 0.4837 0.8104 0.4279 0.096 Uiso 1 1 calc R C4' C 0.4125(5) 0.8528(3) 0.2842(10) 0.068(2) Uani 1 1 d . H4B' H 0.4475 0.8906 0.3004 0.090 Uiso 1 1 calc R C5' C 0.3284(8) 0.8461(3) 0.1836(11) 0.086(3) Uani 1 1 d . H5A' H 0.3703 0.8593 0.1098 0.114 Uiso 1 1 calc R H5B' H 0.2621 0.8746 0.1973 0.114 Uiso 1 1 calc R C6' C 0.2738(6) 0.7862(3) 0.1573(8) 0.0557(19) Uani 1 1 d . H6A' H 0.3140 0.7691 0.0859 0.074 Uiso 1 1 calc R H6B' H 0.1887 0.7923 0.1363 0.074 Uiso 1 1 calc R B1' B 0.1077(5) 0.5877(3) 0.0714(7) 0.0325(16) Uani 1 1 d . B2' B 0.2414(6) 0.6319(3) 0.0941(7) 0.0349(16) Uani 1 1 d . B3' B 0.2469(5) 0.5525(3) 0.1222(6) 0.0308(14) Uani 1 1 d . B4' B 0.1023(5) 0.5220(3) 0.1649(7) 0.0327(15) Uani 1 1 d . B5' B 0.0964(6) 0.6577(3) 0.1443(7) 0.0394(17) Uani 1 1 d . B6' B 0.2363(6) 0.6745(3) 0.2257(7) 0.0414(18) Uani 1 1 d . B7' B 0.3156(6) 0.6023(3) 0.2256(7) 0.0363(16) Uani 1 1 d . B8' B 0.2218(5) 0.5298(3) 0.2740(7) 0.0358(17) Uani 1 1 d . B9' B 0.0651(6) 0.5404(3) 0.3146(8) 0.0420(18) Uani 1 1 d . B10' B 0.0029(5) 0.5846(3) 0.1906(7) 0.0388(16) Uani 1 1 d . H1 H 0.3280 0.1014 0.0253 0.060 Uiso 1 1 d . H2 H 0.4500 0.1977 0.1532 0.060 Uiso 1 1 d . H3 H 0.5652 0.0832 0.1817 0.060 Uiso 1 1 d . H4 H 0.3941 -0.0118 0.1323 0.060 Uiso 1 1 d . H5 H 0.1756 0.1751 0.1615 0.060 Uiso 1 1 d . H7 H 0.5358 0.1465 0.3951 0.060 Uiso 1 1 d . H8 H 0.4947 0.0129 0.3867 0.060 Uiso 1 1 d . H9 H 0.2396 -0.0267 0.3580 0.060 Uiso 1 1 d . H10 H 0.1361 0.0435 0.1449 0.060 Uiso 1 1 d . H56 H 0.2193 0.1492 0.3151 0.060 Uiso 1 1 d . H67 H 0.3591 0.1447 0.3989 0.060 Uiso 1 1 d . H89 H 0.3385 0.0465 0.4067 0.060 Uiso 1 1 d . H910 H 0.1898 0.0544 0.3072 0.060 Uiso 1 1 d . H1' H 0.0698 0.5854 -0.0183 0.060 Uiso 1 1 d . H2' H 0.2905 0.6500 0.0142 0.060 Uiso 1 1 d . H3' H 0.3081 0.5242 0.0821 0.060 Uiso 1 1 d . H4' H 0.0711 0.4789 0.1323 0.060 Uiso 1 1 d . H5' H 0.0441 0.6950 0.0976 0.060 Uiso 1 1 d . H7' H 0.4051 0.6039 0.2518 0.060 Uiso 1 1 d . H8' H 0.2716 0.4948 0.3277 0.060 Uiso 1 1 d . H9' H 0.0084 0.5188 0.3884 0.060 Uiso 1 1 d . H10' H -0.0956 0.5867 0.1801 0.060 Uiso 1 1 d . H56' H 0.1348 0.6745 0.2447 0.060 Uiso 1 1 d . H67' H 0.2627 0.6362 0.3109 0.060 Uiso 1 1 d . H89' H 0.1649 0.5588 0.3686 0.060 Uiso 1 1 d . H910' H 0.0190 0.6003 0.3051 0.060 Uiso 1 1 d . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.031(3) 0.045(4) 0.043(4) 0.001(3) -0.001(3) -0.006(3) B2 0.037(4) 0.036(4) 0.056(5) -0.001(3) 0.003(4) -0.005(3) B3 0.023(3) 0.042(4) 0.056(5) -0.002(3) -0.002(3) -0.002(3) B4 0.036(3) 0.035(3) 0.048(5) -0.006(3) 0.002(4) -0.001(3) B5 0.025(3) 0.038(3) 0.042(4) -0.001(3) -0.005(3) 0.001(3) B6 0.029(3) 0.042(3) 0.046(4) 0.014(4) -0.013(3) -0.005(3) B7 0.027(3) 0.048(4) 0.059(5) -0.004(4) -0.008(4) 0.004(3) B8 0.027(3) 0.043(4) 0.060(5) 0.000(4) 0.006(3) 0.003(3) B9 0.035(3) 0.038(3) 0.063(5) -0.001(4) 0.011(4) -0.004(3) B10 0.029(3) 0.050(4) 0.055(5) -0.006(4) 0.009(3) -0.004(3) C1 0.042(3) 0.037(3) 0.045(4) -0.004(3) 0.000(3) -0.005(3) C2 0.029(3) 0.044(3) 0.050(4) -0.002(3) 0.000(3) -0.009(3) C3 0.053(4) 0.049(4) 0.051(4) 0.007(3) -0.007(3) -0.014(3) C4 0.057(4) 0.046(4) 0.050(4) -0.001(3) 0.012(4) -0.005(3) C5 0.048(4) 0.046(4) 0.087(6) -0.008(4) -0.018(4) 0.002(3) C6 0.049(3) 0.043(3) 0.056(5) 0.003(3) -0.003(3) -0.002(3) C1' 0.067(5) 0.045(4) 0.069(5) -0.002(4) -0.021(4) -0.003(3) C2' 0.060(5) 0.073(5) 0.103(7) 0.011(5) -0.017(5) -0.018(4) C3' 0.071(5) 0.067(5) 0.080(6) 0.002(5) -0.009(5) -0.038(4) C4' 0.028(3) 0.055(4) 0.120(8) -0.013(5) 0.010(4) -0.002(3) C5' 0.078(5) 0.055(5) 0.125(9) 0.012(5) -0.020(6) -0.001(4) C6' 0.052(4) 0.037(3) 0.079(5) 0.009(4) -0.013(4) 0.003(3) B1' 0.024(3) 0.036(3) 0.038(4) -0.005(3) -0.005(3) 0.000(3) B2' 0.024(3) 0.046(3) 0.034(4) -0.004(3) 0.002(3) -0.003(3) B3' 0.024(3) 0.046(3) 0.023(3) -0.001(3) 0.004(3) 0.002(3) B4' 0.025(3) 0.034(3) 0.039(4) -0.007(3) 0.003(3) -0.001(3) B5' 0.034(3) 0.042(4) 0.042(5) -0.002(3) -0.008(3) -0.001(3) B6' 0.047(4) 0.036(3) 0.042(5) -0.001(3) -0.011(4) 0.004(3) B7' 0.031(3) 0.039(3) 0.039(4) -0.005(3) -0.005(3) -0.008(3) B8' 0.024(3) 0.044(4) 0.039(4) 0.004(3) 0.010(3) 0.007(3) B9' 0.027(3) 0.048(4) 0.051(5) 0.001(4) 0.016(3) 0.002(3) B10' 0.024(3) 0.052(4) 0.040(4) -0.001(3) 0.007(3) 0.007(3) 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle B5 B1 B2 61.1(4) B5 B1 B10 67.9(4) B2 B1 B10 117.3(6) B5 B1 B3 107.2(5) B2 B1 B3 60.2(4) B10 B1 B3 107.3(5) B5 B1 B4 116.5(5) B2 B1 B4 114.7(5) B10 B1 B4 60.4(4) B3 B1 B4 60.3(4) B6 B2 B1 112.2(5) B6 B2 B3 112.4(6) B1 B2 B3 60.4(4) B6 B2 B7 62.2(4) B1 B2 B7 106.2(5) B3 B2 B7 58.6(4) B6 B2 B5 60.8(4) B1 B2 B5 59.3(4) B3 B2 B5 105.9(4) B7 B2 B5 104.0(5) B8 B3 B7 68.4(5) B8 B3 B2 117.1(5) B7 B3 B2 61.0(4) B8 B3 B1 107.7(5) B7 B3 B1 107.2(5) B2 B3 B1 59.4(4) B8 B3 B4 61.4(4) B7 B3 B4 117.6(5) B2 B3 B4 113.6(5) B1 B3 B4 59.9(4) B9 B4 B1 111.0(5) B9 B4 B10 60.7(4) B1 B4 B10 59.4(4) B9 B4 B3 110.6(5) B1 B4 B3 59.8(4) B10 B4 B3 106.1(5) B9 B4 B8 61.9(4) B1 B4 B8 104.3(5) B10 B4 B8 104.4(5) B3 B4 B8 57.2(4) B1 B5 B6 110.5(5) B1 B5 B2 59.7(4) B6 B5 B2 58.3(4) B1 B5 B10 56.4(3) B6 B5 B10 119.4(5) B2 B5 B10 106.7(4) C1 B6 B2 131.5(5) C1 B6 B5 127.2(5) B2 B6 B5 60.9(4) C1 B6 B7 128.5(5) B2 B6 B7 60.2(4) B5 B6 B7 102.8(5) B3 B7 B2 60.4(4) B3 B7 B6 110.1(5) B2 B7 B6 57.7(4) B3 B7 B8 55.1(4) B2 B7 B8 105.9(5) B6 B7 B8 118.1(4) B3 B8 B4 61.3(4) B3 B8 B9 110.3(6) B4 B8 B9 57.4(4) B3 B8 B7 56.5(4) B4 B8 B7 107.9(5) B9 B8 B7 117.5(4) B4 B9 B10 61.2(4) B4 B9 B8 60.7(4) B10 B9 B8 103.9(5) B1 B10 B9 109.3(5) B1 B10 B4 60.1(4) B9 B10 B4 58.1(4) B1 B10 B5 55.7(4) B9 B10 B5 116.5(5) B4 B10 B5 106.3(4) C6 C1 C2 110.0(5) C6 C1 B6 113.9(6) C2 C1 B6 113.7(5) C3 C2 C1 113.1(5) C4 C3 C2 122.5(6) C3 C4 C5 124.2(6) C4 C5 C6 112.8(6) C1 C6 C5 112.9(6) C6' C1' C2' 112.3(6) C6' C1' B6' 114.7(6) C2' C1' B6' 112.2(5) C3' C2' C1' 109.6(6) C4' C3' C2' 122.4(8) C3' C4' C5' 120.1(7) C4' C5' C6' 120.0(7) C5' C6' C1' 115.3(7) B5' B1' B10' 69.1(4) B5' B1' B4' 117.0(5) B10' B1' B4' 60.8(4) B5' B1' B2' 60.8(4) B10' B1' B2' 117.7(5) B4' B1' B2' 113.1(5) B5' B1' B3' 107.4(4) B10' B1' B3' 108.3(5) B4' B1' B3' 60.1(3) B2' B1' B3' 59.3(3) B6' B2' B3' 113.1(5) B6' B2' B7' 62.4(4) B3' B2' B7' 58.9(4) B6' B2' B5' 62.5(4) B3' B2' B5' 106.9(4) B7' B2' B5' 106.2(5) B6' B2' B1' 112.8(5) B3' B2' B1' 61.0(3) B7' B2' B1' 107.0(5) B5' B2' B1' 58.4(4) B7' B3' B8' 68.5(4) B7' B3' B2' 60.7(4) B8' B3' B2' 116.0(5) B7' B3' B4' 116.8(5) B8' B3' B4' 60.4(4) B2' B3' B4' 112.6(4) B7' B3' B1' 107.4(4) B8' B3' B1' 106.2(4) B2' B3' B1' 59.7(3) B4' B3' B1' 59.1(3) B9' B4' B1' 111.3(5) B9' B4' B10' 61.7(4) B1' B4' B10' 58.8(4) B9' B4' B8' 61.3(4) B1' B4' B8' 106.5(4) B10' B4' B8' 105.9(5) B9' B4' B3' 111.7(5) B1' B4' B3' 60.9(3) B10' B4' B3' 107.4(4) B8' B4' B3' 58.9(3) B1' B5' B2' 60.8(4) B1' B5' B6' 110.1(4) B2' B5' B6' 57.0(4) B1' B5' B10' 55.5(4) B2' B5' B10' 106.7(4) B6' B5' B10' 118.8(5) C1' B6' B2' 133.7(6) C1' B6' B7' 131.0(5) B2' B6' B7' 60.4(4) C1' B6' B5' 124.6(5) B2' B6' B5' 60.4(4) B7' B6' B5' 103.3(5) B3' B7' B2' 60.4(4) B3' B7' B6' 109.9(5) B2' B7' B6' 57.2(4) B3' B7' B8' 56.0(3) B2' B7' B8' 105.8(4) B6' B7' B8' 117.1(5) B3' B8' B4' 60.7(4) B3' B8' B9' 110.4(5) B4' B8' B9' 58.0(4) B3' B8' B7' 55.5(3) B4' B8' B7' 106.5(5) B9' B8' B7' 117.7(4) B4' B9' B8' 60.6(4) B4' B9' B10' 60.3(4) B8' B9' B10' 104.3(5) B1' B10' B4' 60.4(4) B1' B10' B9' 109.5(4) B4' B10' B9' 58.0(4) B1' B10' B5' 55.3(4) B4' B10' B5' 105.6(4) B9' B10' B5' 115.7(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance B1 B5 1.761(10) B1 B2 1.768(10) B1 B10 1.775(9) B1 B3 1.786(10) B1 B4 1.787(10) B2 B6 1.745(11) B2 B3 1.783(9) B2 B7 1.792(12) B2 B5 1.793(9) B3 B8 1.720(11) B3 B7 1.750(11) B3 B4 1.795(9) B4 B9 1.736(11) B4 B10 1.793(9) B4 B8 1.797(11) B5 B6 1.790(10) B5 B10 1.976(9) B6 C1 1.555(9) B6 B7 1.827(9) B7 B8 1.952(10) B8 B9 1.818(9) B9 B10 1.784(11) C1 C6 1.495(9) C1 C2 1.545(8) C2 C3 1.475(9) C3 C4 1.344(10) C4 C5 1.456(10) C5 C6 1.524(9) C1' C6' 1.504(10) C1' C2' 1.520(10) C1' B6' 1.573(9) C2' C3' 1.499(11) C3' C4' 1.359(11) C4' C5' 1.440(13) C5' C6' 1.471(10) B1' B5' 1.732(9) B1' B10' 1.736(10) B1' B4' 1.764(10) B1' B2' 1.775(9) B1' B3' 1.797(8) B2' B6' 1.712(10) B2' B3' 1.768(9) B2' B7' 1.773(10) B2' B5' 1.774(9) B3' B7' 1.741(9) B3' B8' 1.750(9) B3' B4' 1.783(8) B4' B9' 1.730(11) B4' B10' 1.773(9) B4' B8' 1.778(9) B5' B6' 1.811(9) B5' B10' 1.968(9) B6' B7' 1.806(9) B7' B8' 1.965(9) B8' B9' 1.790(8) B9' B10' 1.797(10)