#------------------------------------------------------------------------------ #$Date: 2014-02-06 11:48:57 +0200 (Thu, 06 Feb 2014) $ #$Revision: 100534 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/33/46/4334664.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_4334664 loop_ _publ_author_name 'William Levason' 'David Pugh' 'Gillian Reid' _publ_contact_author_address ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; _publ_contact_author_email wxl@soton.ac.uk _publ_contact_author_fax '023 8059 3781' _publ_contact_author_name 'Professor William Levason' _publ_contact_author_phone '023 8059 3792' _publ_section_title ; Phosphine and Diphosphine Complexes of Silicon(IV) Halides ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 5185 _journal_page_last 5193 _journal_paper_doi 10.1021/ic400077z _journal_volume 52 _journal_year 2013 _chemical_formula_moiety 'C10 H24 Br4 P2 Si' _chemical_formula_sum 'C10 H24 Br4 P2 Si' _chemical_formula_weight 553.96 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 15 _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 104.902(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.353(3) _cell_length_b 11.954(4) _cell_length_c 17.285(6) _cell_measurement_reflns_used 2566 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 31.2 _cell_measurement_theta_min 2.8 _cell_volume 1867.6(11) _computing_cell_refinement ; CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011) ; _computing_data_collection ; CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011) ; _computing_data_reduction ; CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011) ; _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 100(2) _diffrn_detector CCD _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device ; AFC12 (Right): Kappa 3 circle ; _diffrn_measurement_device_type ; Rigaku Saturn724+ (2x2 bin mode) ; _diffrn_measurement_method 'profile data from \w-scans' _diffrn_measurement_specimen_support Mitegen _diffrn_radiation_monochromator Confocal _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0149 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 3781 _diffrn_reflns_theta_full 25.02 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_min 3.30 _diffrn_source 'Rotating Anode' _diffrn_source_current 55.0 _diffrn_source_power 2.5 _diffrn_source_voltage 45.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 8.837 _exptl_absorpt_correction_T_max 0.7774 _exptl_absorpt_correction_T_min 0.5767 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.970 _exptl_crystal_description block _exptl_crystal_F_000 1072 _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.396 _refine_diff_density_min -0.262 _refine_diff_density_rms 0.067 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 80 _refine_ls_number_reflns 1635 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.984 _refine_ls_R_factor_all 0.0181 _refine_ls_R_factor_gt 0.0158 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.006 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0192P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0357 _reflns_number_gt 1493 _reflns_number_total 1635 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ic400077z_si_002_07.cif _[local]_cod_data_source_block Compound_6 _cod_original_cell_volume 1867.5(11) _cod_database_code 4334664 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_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 C1 C 0.4569(2) 0.17150(18) 0.56027(13) 0.0183(5) Uani 1 1 d . H1A H 0.5010 0.1099 0.5359 0.022 Uiso 1 1 calc R H1B H 0.3514 0.1532 0.5543 0.022 Uiso 1 1 calc R C2 C 0.4666(3) 0.27934(18) 0.51489(15) 0.0305(6) Uani 1 1 d . H2A H 0.4216 0.3406 0.5380 0.046 Uiso 1 1 calc R H2B H 0.4139 0.2699 0.4584 0.046 Uiso 1 1 calc R H2C H 0.5707 0.2969 0.5190 0.046 Uiso 1 1 calc R C3 C 0.74265(19) 0.21001(16) 0.66984(13) 0.0165(5) Uani 1 1 d . H3A H 0.7463 0.2808 0.6407 0.020 Uiso 1 1 calc R H3B H 0.7974 0.2221 0.7264 0.020 Uiso 1 1 calc R C4 C 0.8224(2) 0.11865(17) 0.63413(15) 0.0246(6) Uani 1 1 d . H4A H 0.8233 0.0488 0.6639 0.037 Uiso 1 1 calc R H4B H 0.9244 0.1422 0.6379 0.037 Uiso 1 1 calc R H4C H 0.7704 0.1067 0.5778 0.037 Uiso 1 1 calc R C5 C 0.4805(2) 0.30501(16) 0.70399(12) 0.0161(5) Uani 1 1 d . H5A H 0.5239 0.3719 0.6851 0.019 Uiso 1 1 calc R H5B H 0.3717 0.3088 0.6827 0.019 Uiso 1 1 calc R Si1 Si 0.5000 0.03442(6) 0.7500 0.01165(18) Uani 1 2 d S P1 P 0.55018(5) 0.17934(4) 0.66627(3) 0.01254(13) Uani 1 1 d . Br1 Br 0.245882(19) 0.041566(15) 0.672152(13) 0.01513(7) Uani 1 1 d . Br2 Br 0.55500(2) -0.100300(16) 0.661253(13) 0.01513(7) Uani 1 1 d . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0179(11) 0.0213(12) 0.0153(13) 0.0011(10) 0.0036(10) -0.0015(10) C2 0.0440(15) 0.0261(13) 0.0199(16) 0.0061(11) 0.0051(12) 0.0006(12) C3 0.0110(10) 0.0181(11) 0.0220(14) 0.0015(10) 0.0068(10) -0.0030(9) C4 0.0206(11) 0.0217(12) 0.0368(17) -0.0005(11) 0.0170(12) -0.0001(10) C5 0.0142(10) 0.0113(10) 0.0246(14) 0.0029(9) 0.0080(10) 0.0001(9) Si1 0.0096(4) 0.0112(4) 0.0140(5) 0.000 0.0028(3) 0.000 P1 0.0112(3) 0.0115(3) 0.0153(4) 0.0007(2) 0.0042(2) -0.0004(2) Br1 0.00970(11) 0.01552(12) 0.01895(14) 0.00097(9) 0.00149(9) -0.00122(8) Br2 0.01598(12) 0.01234(12) 0.01762(14) -0.00223(9) 0.00531(9) 0.00025(8) 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' Si Si 0.0817 0.0704 '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' Br Br -0.2901 2.4595 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 C2 C1 P1 113.48(16) . . C2 C1 H1A 108.9 . . P1 C1 H1A 108.9 . . C2 C1 H1B 108.9 . . P1 C1 H1B 108.9 . . H1A C1 H1B 107.7 . . C1 C2 H2A 109.5 . . C1 C2 H2B 109.5 . . H2A C2 H2B 109.5 . . C1 C2 H2C 109.5 . . H2A C2 H2C 109.5 . . H2B C2 H2C 109.5 . . C4 C3 P1 114.85(14) . . C4 C3 H3A 108.6 . . P1 C3 H3A 108.6 . . C4 C3 H3B 108.6 . . P1 C3 H3B 108.6 . . H3A C3 H3B 107.5 . . C3 C4 H4A 109.5 . . C3 C4 H4B 109.5 . . H4A C4 H4B 109.5 . . C3 C4 H4C 109.5 . . H4A C4 H4C 109.5 . . H4B C4 H4C 109.5 . . C5 C5 P1 110.99(10) 2_656 . C5 C5 H5A 109.4 2_656 . P1 C5 H5A 109.4 . . C5 C5 H5B 109.4 2_656 . P1 C5 H5B 109.4 . . H5A C5 H5B 108.0 . . Br2 Si1 Br2 94.39(4) . 2_656 Br2 Si1 P1 176.09(3) . 2_656 Br2 Si1 P1 89.51(3) 2_656 2_656 Br2 Si1 P1 89.51(3) . . Br2 Si1 P1 176.09(3) 2_656 . P1 Si1 P1 86.59(4) 2_656 . Br2 Si1 Br1 92.20(2) . 2_656 Br2 Si1 Br1 90.56(2) 2_656 2_656 P1 Si1 Br1 87.43(2) 2_656 2_656 P1 Si1 Br1 89.62(2) . 2_656 Br2 Si1 Br1 90.56(2) . . Br2 Si1 Br1 92.20(2) 2_656 . P1 Si1 Br1 89.62(2) 2_656 . P1 Si1 Br1 87.43(2) . . Br1 Si1 Br1 175.94(4) 2_656 . C1 P1 C3 104.97(10) . . C1 P1 C5 106.25(10) . . C3 P1 C5 105.25(9) . . C1 P1 Si1 117.18(7) . . C3 P1 Si1 118.25(7) . . C5 P1 Si1 103.75(7) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 C2 1.524(3) . C1 P1 1.818(2) . C1 H1A 0.9900 . C1 H1B 0.9900 . C2 H2A 0.9800 . C2 H2B 0.9800 . C2 H2C 0.9800 . C3 C4 1.539(3) . C3 P1 1.8225(18) . C3 H3A 0.9900 . C3 H3B 0.9900 . C4 H4A 0.9800 . C4 H4B 0.9800 . C4 H4C 0.9800 . C5 C5 1.538(4) 2_656 C5 P1 1.824(2) . C5 H5A 0.9900 . C5 H5B 0.9900 . Si1 Br2 2.3701(8) . Si1 Br2 2.3701(7) 2_656 Si1 P1 2.3802(9) 2_656 Si1 P1 2.3802(9) . Si1 Br1 2.4128(7) 2_656 Si1 Br1 2.4128(8) . 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 C2 C1 P1 C3 -59.85(17) . C2 C1 P1 C5 51.34(17) . C2 C1 P1 Si1 166.67(13) . C4 C3 P1 C1 -63.37(18) . C4 C3 P1 C5 -175.28(16) . C4 C3 P1 Si1 69.50(18) . C5 C5 P1 C1 165.32(15) 2_656 C5 C5 P1 C3 -83.68(17) 2_656 C5 C5 P1 Si1 41.19(17) 2_656 Br2 Si1 P1 C1 51.34(8) . P1 Si1 P1 C1 -129.01(8) 2_656 Br1 Si1 P1 C1 143.55(8) 2_656 Br1 Si1 P1 C1 -39.24(8) . Br2 Si1 P1 C3 -75.92(8) . P1 Si1 P1 C3 103.72(8) 2_656 Br1 Si1 P1 C3 16.28(8) 2_656 Br1 Si1 P1 C3 -166.50(8) . Br2 Si1 P1 C5 168.05(7) . P1 Si1 P1 C5 -12.30(6) 2_656 Br1 Si1 P1 C5 -99.75(7) 2_656 Br1 Si1 P1 C5 77.47(7) .