Activations of all Bonds to Silicon (Si-H, Si-C) in a Silane with Extrusion of [CoSiCo] Silicide Cores.
Handford, Rex C.; Smith, Patrick W.; Tilley, T. Don; Journal of the American Chemical Society 141 (2019) 8769–8772; doi:10.1021/jacs.9b04265

data_4127550
_publ_section_title
;
 Activations of all Bonds to Silicon (Si-H, Si-C) in a Silane with
 Extrusion of [CoSiCo] Silicide Cores.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8769
_journal_page_last               8772
_journal_paper_doi               10.1021/jacs.9b04265
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C53 H101 B2 Co2 P5 Si2'
_chemical_formula_sum            'C53 H101 B2 Co2 P5 Si2'
_chemical_formula_weight         1088.84
_chemical_name_systematic        '[[BP2iPr](PhSiH2)CoH2]Si[H2Co[BP3iPr]]'
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-15
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                95.2960(10)
_cell_angle_beta                 96.8830(10)
_cell_angle_gamma                107.2870(10)
_cell_formula_units_Z            2
_cell_length_a                   11.5244(4)
_cell_length_b                   12.7658(4)
_cell_length_c                   21.2150(7)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.89
_cell_measurement_theta_min      2.30
_cell_volume                     2931.59(17)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker-Nonius APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device
'Bruker-Nonius APEXII CCD area detector and D8 diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    '0.2 mm sinlge-pinhole'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0681
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            54155
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        31.915
_diffrn_reflns_theta_max         31.915
_diffrn_reflns_theta_min         1.729
_diffrn_source                   synchrotron
_diffrn_source_type              'Bend magnet, Station 11.3.1, ALS, LBNL'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 - Bruker AXS, Madison WI'
_exptl_crystal_colour            'clear orangish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       prism
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.048
_exptl_crystal_size_mid          0.037
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         18653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0397P)^2^+1.8746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1152
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13886
_reflns_number_total             18653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04265_si_002.cif
_cod_data_source_block           rh_2_132
_cod_database_code               4127550
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Others
 Fixed Sof: H44D(0.5) H44E(0.5) H44F(0.5) H44A(0.5) H44B(0.5) H44C(0.5)
 C42A(0.5) H42A(0.5) C43A(0.5) H43A(0.5) H43B(0.5) H43C(0.5) C43(0.5) H43D(0.5)
 H43E(0.5) H43F(0.5) C42(0.5) H42(0.5)
3.a Ternary CH refined with riding coordinates:
 C48(H48), C36(H36), C9(H9), C15(H15), C51(H51), C12(H12), C39(H39), C18(H18),
 C45(H45), C42A(H42A), C42(H42)
3.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C1(H1A,H1B), C2(H2C,H2D), C29(H29A,H29B), C28(H28A,H28B)
3.c Aromatic/amide H refined with riding coordinates:
 C35(H35), C34(H34), C4(H4), C33(H33), C6(H6), C31(H31), C32(H32), C5(H5),
 C26(H26), C22(H22), C7(H7), C8(H8), C24(H24), C25(H25), C23(H23)
3.d Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C37(H37A,H37B,H37C), C49(H49A,H49B,H49C), C11(H11A,H11B,
 H11C), C53(H53A,H53B,H53C), C52(H52A,H52B,H52C), C13(H13A,H13B,H13C), C38(H38A,
 H38B,H38C), C16(H16A,H16B,H16C), C10(H10A,H10B,H10C), C17(H17A,H17B,H17C),
 C14(H14A,H14B,H14C), C44(H44D,H44E,H44F), C44(H44A,H44B,H44C), C41(H41A,H41B,
 H41C), C20(H20A,H20B,H20C), C40(H40A,H40B,H40C), C46(H46A,H46B,H46C), C47(H47A,
 H47B,H47C), C19(H19A,H19B,H19C), C43A(H43A,H43B,H43C), C43(H43D,H43E,H43F)
;
_olex2_exptl_crystal_mounting_method
'Suspended in Paratone N oil and mounted on a Cryoloop'
_olex2_submission_original_sample_id RH-2-132
_olex2_submission_special_instructions 'No special instructions were received'