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_4127549
_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         'C27 H53 B Co I P3, C24 H48 Na O6'
_chemical_formula_sum            'C51 H101 B Co I Na O6 P3'
_chemical_formula_weight         1122.85
_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             2019-03-04
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90.509(6)
_cell_angle_beta                 91.262(7)
_cell_angle_gamma                98.341(6)
_cell_formula_units_Z            2
_cell_length_a                   11.4364(13)
_cell_length_b                   15.6713(18)
_cell_length_c                   16.661(2)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    104
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.20
_cell_volume                     2953.5(6)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      104.57
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51913
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.399
_diffrn_reflns_theta_min         1.223
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.944
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6311
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0952 before and 0.0607 after correction. The Ratio of minimum to maximum transmission is 0.8469. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'clear pinkish blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       needle
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.597
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         10677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0633
_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^)+(0.0403P)^2^+17.9134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1489
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8795
_reflns_number_total             10677
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04265_si_002.cif
_cod_data_source_block           rh_3_1_0m
_cod_database_code               4127549
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H48C(0.5) H48D(0.5) H48A(0.5) H48B(0.5) H50A(0.5) H50B(0.5)
 H50C(0.5) H50D(0.5) C49A(0.5) H49A(0.5) H49B(0.5) C49(0.5) H49C(0.5) H49D(0.5)
3.a Ternary CH refined with riding coordinates:
 C16(H16), C13(H13), C25(H25), C10(H10), C19(H19), C22(H22)
3.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C41(H41A,H41B), C32(H32A,H32B), C47(H47A,H47B), C31(H31A,
 H31B), C30(H30A,H30B), C35(H35A,H35B), C42(H42A,H42B), C28(H28A,H28B),
 C36(H36A,H36B), C33(H33A,H33B), C45(H45A,H45B), C51(H51A,H51B), C44(H44A,H44B),
  C2(H2A,H2B), C39(H39A,H39B), C43(H43A,H43B), C46(H46A,H46B), C29(H29A,H29B),
 C34(H34A,H34B), C40(H40A,H40B), C1(H1A,H1B), C3(H3A,H3B), C38(H38A,H38B),
 C48(H48C,H48D), C48(H48A,H48B), C50(H50A,H50B), C50(H50C,H50D), C49A(H49A,
 H49B), C49(H49C,H49D)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C6(H6), C9(H9), C8(H8)
3.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C18(H18A,H18B,H18C), C12(H12A,H12B,
 H12C), C11(H11A,H11B,H11C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C15(H15A,
 H15B,H15C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C),
 C27(H27A,H27B,H27C)
;
_olex2_diffrn_ambient_temperature_device '100 K'
_olex2_exptl_crystal_mounting_method
'Crystal suspended in Paratone N oil and mounted on a Cryoloop.'
_olex2_submission_original_sample_id RH-3-1
_olex2_submission_special_instructions 'No special instructions were received'