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_7045318
_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         'C36 H64 Cl3 Co N4 P2 Si2, C5 H12'
_chemical_formula_sum            'C41 H76 Cl3 Co N4 P2 Si2'
_chemical_formula_weight         908.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2017-05-19 deposited with the CCDC.
2018-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.406(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8468(3)
_cell_length_b                   19.5827(5)
_cell_length_c                   18.5459(4)
_cell_measurement_reflns_used    17211
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      65.85
_cell_measurement_theta_min      4.91
_cell_volume                     4891.8(2)
_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      150.15
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            DECTRIS
_diffrn_measured_fraction_theta_full 0.901
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device       '4-circle goniometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '2.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'secondary plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0853
_diffrn_reflns_Laue_measured_fraction_full 0.901
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            22857
_diffrn_reflns_point_group_measured_fraction_full 0.901
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         65.192
_diffrn_reflns_theta_min         4.903
_diffrn_source                   'Cu Genix 3D'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_target            Cu
_diffrn_source_type              'microfocus sealed X-ray tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.581
_exptl_absorpt_correction_T_max  0.7714
_exptl_absorpt_correction_T_min  0.5008
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.875
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         7980
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.880
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0522P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1097
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4999
_reflns_number_total             7980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04155a2.cif
_cod_data_source_block           sun19
_cod_depositor_comments
'Adding full bibliography for 7045316--7045318.cif.'
_cod_database_code               7045318
_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
 C40A-C39A = C41A-C40A
 1.54 with sigma of 0.02
 C38A-C37A
 1.54 with sigma of 0.02
 C40B-C41B
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C37A \\sim C38A \\sim C39A \\sim C40A \\sim C41A: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.03
C37B \\sim C38B \\sim C39B \\sim C40B \\sim C41B: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.03
4. Others
 Fixed Sof: C37B(0.5) H37A(0.5) H37B(0.5) H37C(0.5) C38A(0.5) H38C(0.5)
 H38D(0.5) C40B(0.5) H40A(0.5) H40B(0.5) C41B(0.5) H41A(0.5) H41B(0.5)
 H41C(0.5) C37A(0.5) H37D(0.5) H37E(0.5) H37F(0.5) C40A(0.5) H40C(0.5)
 H40D(0.5) C41A(0.5) H41D(0.5) H41E(0.5) H41F(0.5) C39B(0.5) H39A(0.5)
 H39B(0.5) C39A(0.5) H39C(0.5) H39D(0.5) C38B(0.5) H38A(0.5) H38B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C38A(H38C,H38D), C40B(H40A,H40B), C40A(H40C,H40D), C39B(H39A,H39B), C39A(H39C,
 H39D), C38B(H38A,H38B)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C22(H22), C23(H23), C24(H24),
 C25(H25), C26(H26)
5.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C),
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37B(H37A,H37B,
 H37C), C41B(H41A,H41B,H41C), C37A(H37D,H37E,H37F), C41A(H41D,H41E,H41F)
;
_olex2_submission_special_instructions 'No special instructions were received'