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_4127552
_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         'C54 H99 B2 Co2 N2 P5 Si'
_chemical_formula_sum            'C54 H99 B2 Co2 N2 P5 Si'
_chemical_formula_weight         1098.77
_chemical_name_systematic        {[BP2]Co(dmap)}Si{H2Co[BP3[)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-10-07
_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                   12.1123(6)
_cell_length_b                   21.5468(11)
_cell_length_c                   22.5752(11)
_cell_measurement_reflns_used    698
_cell_measurement_temperature    100
_cell_measurement_theta_max      10.49
_cell_measurement_theta_min      2.53
_cell_volume                     5891.7(5)
_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      100
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker-Nonius APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0696
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            90354
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.541
_diffrn_reflns_theta_max         27.541
_diffrn_reflns_theta_min         1.340
_diffrn_source                   synchrotron
_diffrn_source_type              'Bend magnet, Station 11.3.1, ALS, LBNL'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.802
_exptl_absorpt_correction_T_max  100
_exptl_absorpt_correction_T_min  100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 - Bruker AXS, Madison WI'
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       block
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.408(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         12603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0509P)^2^+2.1815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0988
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                10996
_reflns_number_total             12603
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04265_si_002.cif
_cod_data_source_block           rh2_174_0m
_cod_database_code               4127552
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.976
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.592(14)
 0.408(14)
2. 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
3. Uiso/Uaniso restraints and constraints
Uanis(Si0A) = Uanis(Si2)
4. Others
 Fixed Sof: HJ(0.5) HK(0.5) HL(0.5) H6AA(0.5) HM(0.5) HN(0.5) H7AA(0.5)
 HO(0.5) HP(0.5) HQ(0.5) HR(0.5) HS(0.5) C1(0.5) H1(0.5) C3(0.5) H3A(0.5)
 H3B(0.5) H3C(0.5) C4(0.5) H4(0.5) C01T(0.5) H0BA(0.5) HX(0.5) HY(0.5)
 C01U(0.5) H1BA(0.5) HZ(0.5) H2BA(0.5) C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5)
 C6(0.5) H6(0.5) C7(0.5) H7(0.5) C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5) C9(0.5)
 H9A(0.5) H9B(0.5) H9C(0.5) H10A(0.5) H10(0.5) C11B(0.5) H11A(0.5) H11B(0.5)
 H11C(0.5) C11A(0.5) H11D(0.5) H11E(0.5) H11F(0.5) Si0A(0.4) Si2(0.6)
5.a Ternary CH refined with riding coordinates:
 C00H(H00H), C00K(H00K), C00N(H00N), C00R(H00S), C00Z(H1AA), C011(H011),
 C01D(H01Y), C1(H1), C4(H4), C6(H6), C7(H7), C10(H10A), C10(H10)
5.b Secondary CH2 refined with riding coordinates:
 C00D(H00A,H00C), C00F(H00D,H00F), C010(H01A,H01B), C012(H01C,H01D), C015(H01H,
 H01I)
5.c Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00E(H00E), C00J(H00J), C00L(H00L), C00P(H00P), C00S(H00T),
 C00U(H00X), C00V(H00Y), C00W(H00Z), C00X(H00), C00Y(H0AA), C014(H014),
 C01E(H01Z)
5.d Idealised Me refined as rotating group:
 C00O(H00G,H00I,H00M), C00Q(H00O,H00Q,H00R), C00T(H00U,H00V,H00W), C013(H01E,
 H01F,H01G), C016(H01J,H01K,H01L), C017(H01M,H01N,H01O), C019(H01P,H01Q,H01R),
 C01A(H01S,H01T,H01U), C01C(H01V,H01W,H01X), C01F(H01,H,HA), C01G(H2AA,HB,HC),
 C01H(H3AA,HD,HE), C01I(H4AA,HF,HG), C01K(H5AA,HH,HI), C01L(HJ,HK,HL),
 C01L(H6AA,HM,HN), C01M(H7AA,HO,HP), C01M(HQ,HR,HS), C01N(H8AA,HT,HU),
 C01P(H9AA,HV,HW), C3(H3A,H3B,H3C), C01T(H0BA,HX,HY), C01U(H1BA,HZ,H2BA),
 C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11B(H11A,H11B,H11C),
 C11A(H11D,H11E,H11F)
;
_olex2_exptl_crystal_mounting_method
'Crystal suspended in Paratone N oil and mounted on a Cryoloop.'
_olex2_submission_original_sample_id RH_2_174_0m
_olex2_submission_special_instructions 'No special instructions were received'