High-yielding and Facile Synthesis of Organosilicon Compounds containing m-Carboranylmethyl Group
Han, Xiaojie; Fei, Huafeng; Liu, Bozheng; Tan, Yongxia; Zhang, Xuezhong; Xie, Zemin; Zhang, Zhijie; RSC Adv.  (2015) –; doi:10.1039/C5RA13344K

data_7222016
_publ_section_title
;
 High-yielding and Facile Synthesis of Organosilicon Compounds containing
 m-Carboranylmethyl Group
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA13344K
_journal_year                    2015
_chemical_formula_moiety         'C22 H40 B10 O2 Si2'
_chemical_formula_sum            'C22 H40 B10 O2 Si2'
_chemical_formula_weight         500.82
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-06-03 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.830(7)
_cell_length_b                   12.211(2)
_cell_length_c                   6.5889(13)
_cell_measurement_reflns_used    5931
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4805
_cell_measurement_theta_min      2.0184
_cell_volume                     2882.8(9)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2014)'
_computing_structure_solution
;
'SHELXT (Sheldrick, 2014)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
scan:
    Number of images: 270
               Slice: -76.2500 - 58.7500
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 50.0415
              2theta: -20.0084
scan:
    Number of images: 240
               Slice: -95.0000 - 25.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 270.0000
                 XTD: 50.0415
              2theta: -20.0084
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0219
_diffrn_orient_matrix_UB_12      0.1360
_diffrn_orient_matrix_UB_13      0.0636
_diffrn_orient_matrix_UB_21      0.0426
_diffrn_orient_matrix_UB_22      0.0239
_diffrn_orient_matrix_UB_23      -0.0657
_diffrn_orient_matrix_UB_31      -0.0235
_diffrn_orient_matrix_UB_32      0.0093
_diffrn_orient_matrix_UB_33      -0.0118
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_laue_measured_fraction_full 0.992
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            13946
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         2.018
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.63
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.162
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 2245 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         6316
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+1.1555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1019
_reflns_Friedel_coverage         0.769
_reflns_friedel_fraction_full    0.937
_reflns_friedel_fraction_max     0.910
_reflns_number_gt                5998
_reflns_number_total             6316
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra13344k2.cif
_cod_data_source_block           a
_cod_original_cell_volume        2882.9(10)
_cod_database_code               7222016
_audit_block_doi                 10.5517/cc1j4n2d
_diffrn_number_total             3792
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C17(H17), C18(H18), C20(H20), C21(H21)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C22(H22A,H22B,H22C)
2.d Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3A), B4(H4A), B5(H5), B6(H6A), B7(H7A), B8(H8), B9(H9),
 B10(H10)
;
_shelx_res_checksum              10161
_shelx_hkl_checksum              98880
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'