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_4127551
_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         'C40 H71 B Co N2 P3 Si, C4 H8 O'
_chemical_formula_sum            'C44 H79 B Co N2 O P3 Si'
_chemical_formula_weight         842.83
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-11-26
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.4030(10)
_cell_length_b                   10.1831(5)
_cell_length_c                   21.2625(10)
_cell_measurement_reflns_used    9503
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.47
_cell_volume                     4634.1(4)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0716
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            67769
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         27.950
_diffrn_reflns_theta_min         1.951
_diffrn_source                   'Advanced Light Source, station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6373
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1780 before and 0.0744 after correction.
The Ratio of minimum to maximum transmission is 0.8547.
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    1.208
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details
;
 Flack x determined using 4489 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         10289
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0450P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0797
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                9835
_reflns_number_total             10289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04265_si_002.cif
_cod_data_source_block           rh_3_186b
_cod_database_code               4127551
_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
2.a Ternary CH refined with riding coordinates:
 C19(H19), C22(H22), C25(H25), C10(H10), C16(H16), C13(H13)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1A,H1B), C3(H3A,H3B), C42(H42B,H42A), C44(H44A,H44B),
 C41(H41B,H41A), C43(H43A,H43B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C34(H34), C9(H9), C38(H38), C37(H37), C29(H29), C33(H33),
 C30(H30), C35(H35), C7(H7), C31(H31), C32(H32), C8(H8)
2.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C21(H21A,H21B,
 H21C), C20(H20A,H20B,H20C), C39(H39A,H39B,H39C), C11(H11A,H11B,H11C), C15(H15A,
 H15B,H15C), C40(H40A,H40B,H40C), C12(H12A,H12B,H12C), C24(H24A,H24B,H24C),
 C17(H17A,H17B,H17C), C14(H14A,H14B,H14C), C18(H18A,H18B,H18C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'Crystal suspended in Paratone N oil and mounted on a Cryoloop.'
_olex2_submission_original_sample_id RH-3-186-B
_olex2_submission_special_instructions 'No special instructions were received'