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_4127554
_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         'C33 H61 B Co P3 Si'
_chemical_formula_sum            'C33 H61 B Co P3 Si'
_chemical_formula_weight         648.55
_chemical_name_systematic        '[BP2]Co(SiHPhCH2PiPr2)H2'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-08
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.360(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2110(6)
_cell_length_b                   19.7623(10)
_cell_length_c                   13.6214(7)
_cell_measurement_reflns_used    9148
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.46
_cell_measurement_theta_min      2.23
_cell_volume                     3555.3(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.42
_diffrn_detector_type            'Bruker-Nonius APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device
'Bruker-Nonius APEXII CCD area detector and D8 diffractometer'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless 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  0.0497
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            60857
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        30.405
_diffrn_reflns_theta_max         30.494
_diffrn_reflns_theta_min         1.862
_diffrn_source                   'Advanced Light Source, station 11.3.1'
_diffrn_source_type              'Bend magnet, Station 11.3.1, ALS, LBNL'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6447
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016) was used for absorption correction. wR2(int) was 0.1240 before and 0.0578 after correction. The Ratio of minimum to maximum transmission is 0.8641. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         10028
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0273P)^2^+2.4469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0842
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7951
_reflns_number_total             10028
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04265_si_002.cif
_cod_data_source_block           rh_3_27
_cod_database_code               4127554
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.972
_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
2.a Ternary CH refined with riding coordinates:
 C007(H007), C009(H009), C00B(H00D), C00D(H00G), C00H(H00I), C00J(H00M)
2.b Secondary CH2 refined with riding coordinates:
 C00C(H00E,H00F), C7(H7A,H7B), C00N(H00T,H00U)
2.c Aromatic/amide H refined with riding coordinates:
 C00E(H00H), C6(H6), C2(H6AA), C00P(H00Y), C00R(H00), C3(H5AA), C5(H5), C4(H4),
  C00W(H1AA), C00Z(H4AA)
2.d Idealised Me refined as rotating group:
 C00A(H00A,H00B,H00C), C00I(H00J,H00K,H00L), C00L(H00N,H00O,H00P), C00M(H00Q,
 H00R,H00S), C00O(H00V,H00W,H00X), C00Q(H00Z,H,HA), C00V(H0AA,HB,HC), C00X(H2AA,
 HD,HE), C00Y(H3AA,HF,HG), C010(H01A,H01B,H01C), C011(H01D,H01E,H01F),
 C012(H01G,H01H,H01I)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'