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_7222017
_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         'C8 H28 B10 O2 Si2'
_chemical_formula_sum            'C8 H28 B10 O2 Si2'
_chemical_formula_weight         320.58
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_audit_update_record
;
2015-06-03 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                108.715(3)
_cell_angle_beta                 96.432(4)
_cell_angle_gamma                94.360(3)
_cell_formula_units_Z            2
_cell_length_a                   7.1014(18)
_cell_length_b                   11.404(3)
_cell_length_c                   12.182(4)
_cell_measurement_reflns_used    3235
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4837
_cell_measurement_theta_min      1.8989
_cell_volume                     921.9(5)
_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  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2013)'
_computing_structure_solution
;
'SHELXS (Sheldrick, 2013)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_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      -0.1129
_diffrn_orient_matrix_UB_12      0.0835
_diffrn_orient_matrix_UB_13      0.0257
_diffrn_orient_matrix_UB_21      -0.0283
_diffrn_orient_matrix_UB_22      -0.0432
_diffrn_orient_matrix_UB_23      0.0776
_diffrn_orient_matrix_UB_31      0.0313
_diffrn_orient_matrix_UB_32      0.0423
_diffrn_orient_matrix_UB_33      0.0700
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_laue_measured_fraction_full 0.991
_diffrn_reflns_laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11082
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_min         2.907
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_description       block
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         4193
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+0.3862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1084
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4067
_reflns_number_total             4193
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra13344k2.cif
_cod_data_source_block           sa3795
_cod_original_cell_volume        921.9(4)
_cod_database_code               7222017
_audit_block_doi                 10.5517/cc1j4n3f
_shelxl_version_number           2013-4
_diffrn_number_total             4196
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C6(H6A,H6B)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
2.d Boron cage BH refined with riding coordinates:
 B1(H1D), B2(H2D), B3(H3), B4(H4), B5(H5), B6(H6), B7(H7), B8(H8), B9(H9),
 B10(H10)
;
_shelx_res_checksum              82230
_shelx_hkl_checksum              81203