A self-hydrosilylation of phosphanylhydrosilylalkynes promoted by B(C6F5)3? An experimental and mechanistic study
Huang, Yanting; Wang, Xiaoping; Li, Yan; Yang, Ming-Chung; Su, Ming-Der; Zhu, Hongping; Chemical Communications  (2019) –; doi:10.1039/C8CC09022J

data_7122862
_publ_section_title
;
 A self-hydrosilylation of phosphanylhydrosilylalkynes promoted by
 B(C6F5)3? An experimental and mechanistic study
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC09022J
_journal_year                    2019
_chemical_formula_sum            'C75 H44 B2 F30 N0 O P2 Si2'
_chemical_formula_weight         1670.84
_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
'H-atoms at the P atom are disclosed by difmap and the others are geometrically included'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-12-04 deposited with the CCDC.
2019-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                80.938(6)
_cell_angle_beta                 87.066(7)
_cell_angle_gamma                89.252(8)
_cell_formula_units_Z            2
_cell_length_a                   11.0069(12)
_cell_length_b                   11.1895(10)
_cell_length_c                   29.9621(15)
_cell_measurement_reflns_used    3836
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      62.0630
_cell_measurement_theta_min      4.0020
_cell_volume                     3639.3(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1020
_diffrn_reflns_av_unetI/netI     0.1374
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            21959
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        62.646
_diffrn_reflns_theta_max         62.646
_diffrn_reflns_theta_min         2.991
_exptl_absorpt_coefficient_mu    1.967
_exptl_absorpt_correction_T_max  0.7437
_exptl_absorpt_correction_T_min  0.5219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.869
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.233
_refine_ls_hydrogen_treatment
'all are isotropically refined where the geometrically included H-atoms are constrained'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1079
_refine_ls_number_reflns         11277
_refine_ls_number_restraints     987
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.1695
_refine_ls_R_factor_gt           0.1258
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3365
_refine_ls_wR_factor_ref         0.4107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6326
_reflns_number_total             11277
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc09022j2.cif
_cod_data_source_block           hyt-170628
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7122862
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.522
_shelx_estimated_absorpt_t_max   0.744
_shelx_res_checksum              56188