Synthesis and catalytic activity of N-heterocyclic silylene (NHSi) cobalt hydride for Kumada coupling reactions.
Qi, Xinghao; Sun, Hongjian; Li, Xiaoyan; Fuhr, Olaf; Fenske, Dieter; Dalton transactions (Cambridge, England : 2003) 47 (2018) 2581–2588; doi:10.1039/c7dt04155a

data_7045317
_publ_section_title
;
 Synthesis and catalytic activity of N-heterocyclic silylene (NHSi) cobalt
 hydride for Kumada coupling reactions.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2581
_journal_page_last               2588
_journal_paper_doi               10.1039/c7dt04155a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C51 H63 Cl2 Co N4 P3 Si2, C4 H10 O'
_chemical_formula_sum            'C55 H73 Cl2 Co N4 O P3 Si2'
_chemical_formula_weight         1085.09
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-02-29
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2017-07-07 deposited with the CCDC.
2018-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                98.767(9)
_cell_angle_beta                 101.053(8)
_cell_angle_gamma                103.860(8)
_cell_formula_units_Z            4
_cell_length_a                   13.9845(14)
_cell_length_b                   17.415(2)
_cell_length_c                   24.858(3)
_cell_measurement_reflns_used    23126
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      1.97
_cell_volume                     5642.3(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            56456
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.358
_diffrn_reflns_theta_min         1.544
_diffrn_source                   'Bruker rotating anode'
_diffrn_source_current           120
_diffrn_source_power             6.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  0.9302
_exptl_absorpt_correction_T_min  0.7772
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       needle
_exptl_crystal_F_000             2292
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.263
_refine_diff_density_min         -1.369
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.0051(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1196
_refine_ls_number_reflns         30063
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1409
_refine_ls_R_factor_gt           0.0838
_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^)+(0.1640P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2208
_refine_ls_wR_factor_ref         0.2695
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15183
_reflns_number_total             30063
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04155a2.cif
_cod_data_source_block           sun18
_cod_depositor_comments
'Adding full bibliography for 7045316--7045318.cif.'
_cod_original_cell_volume        5642.2(11)
_cod_database_code               7045317
_shelxl_version_number           2013-4
_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. Restrained distances
 C103-C104
 1.54 with sigma of 0.02
 C109-C110
 1.54 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C20(H20A,H20B), C64(H64A,H64B), C71(H71A,H71B), C109(H10W,
 H10X), C103(H10M,H10N), C107(H10Y,H), C105(H10R,H10S)
3.b Me refined with riding coordinates:
 C104(H10J,H10K,H10L), C108(H10T,H10U,H10V), C106(H10O,H10P,H10Q), C110(H11A,
 H11B,H11C)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C53(H53), C54(H54), C55(H55),
  C56(H56), C57(H57), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63),
 C66(H66), C67(H67), C68(H68), C69(H69), C73(H73), C74(H74), C75(H75), C76(H76),
  C77(H77), C79(H79), C80(H80), C81(H81), C82(H82), C83(H83), C91(H91),
 C92(H92), C93(H93), C94(H94), C95(H95)
3.d Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,
 H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C84(H84A,H84B,H84C),
 C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C97(H97A,H97B,
 H97C), C98(H98A,H98B,H98C), C99(H99A,H99B,H99C), C100(H10A,H10B,H10C),
 C101(H10D,H10E,H10F), C102(H10G,H10H,H10I)
;
_olex2_submission_special_instructions 'No special instructions were received'