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_4127553
_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         'C34 H63 B Co N2 P3, C7 H8'
_chemical_formula_sum            'C41 H71 B Co N2 P3'
_chemical_formula_weight         754.64
_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   geom
_audit_creation_date             2019-02-26
_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                 97.246(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6934(6)
_cell_length_b                   16.3703(7)
_cell_length_c                   18.7873(8)
_cell_measurement_reflns_used    9673
_cell_measurement_temperature    98.15
_cell_measurement_theta_max      29.12
_cell_measurement_theta_min      2.55
_cell_volume                     4177.8(3)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      98.15
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0675
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            67322
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        29.070
_diffrn_reflns_theta_max         29.158
_diffrn_reflns_theta_min         1.698
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_T_max  0.8749
_exptl_absorpt_correction_T_min  0.7900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1354 before and 0.0686 after correction.
The Ratio of minimum to maximum transmission is 0.9030.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         10430
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+2.0888P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0930
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8779
_reflns_number_total             10430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04265_si_002.cif
_cod_data_source_block           rh_4_17_075_BP3CoDMAP
_cod_database_code               4127553
_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. Uiso/Uaniso restraints and constraints
C40A \\sim C39A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C35A \\sim C36A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C41A \\sim C36 \\sim C37A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C41A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C35A) \\sim Ueq, Uanis(C40A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C37A) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C35A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C39A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: C39(0.8) H39(0.8) C40(0.8) H40(0.8) C36(0.8) H36(0.8) C35(0.8)
 C38(0.8) H38(0.8) C41(0.8) H41A(0.8) H41B(0.8) H41C(0.8) C37(0.8) H37(0.8)
 C41A(0.2) H41D(0.2) H41E(0.2) H41F(0.2) C35A(0.2) C40A(0.2) H40A(0.2)
 C39A(0.2) H39A(0.2) C38A(0.2) H38A(0.2) C37A(0.2) H37A(0.2) C36A(0.2) H36A(0.2)
4.a Ternary CH refined with riding coordinates:
 C25(H25), C22(H22), C13(H13), C10(H10), C16(H16), C19(H19)
4.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C1(H1A,H1B), C2(H2A,H2B)
4.c Aromatic/amide H refined with riding coordinates:
 C32(H32), C28(H28), C29(H29), C31(H31), C5(H5), C9(H9), C6(H6), C8(H8),
 C7(H7), C39(H39), C40(H40), C36(H36), C38(H38), C37(H37), C40A(H40A),
 C39A(H39A), C38A(H38A), C37A(H37A), C36A(H36A)
4.d Fitted hexagon refined as free rotating group:
 C35A(C40A,C39A,C38A,C37A,C36A)
4.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C26(H26A,H26B,H26C), C11(H11A,H11B,H11C), C27(H27A,H27B,
 H27C), C33(H33A,H33B,H33C), C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C23(H23A,
 H23B,H23C), C24(H24A,H24B,H24C), C20(H20A,H20B,H20C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C34(H34A,H34B,H34C), C41(H41A,H41B,
 H41C), C41A(H41D,H41E,H41F)
;
_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_special_instructions 'No special instructions were received'