A two-coordinate Ni(I) silyl complex: CO2 insertion and oxidatively-induced silyl migrations
Witzke, Ryan J.; Tilley, T. Don; Chemical Communications  (2019) –; doi:10.1039/C9CC03128F

data_7123412
_publ_section_title
;
 A two-coordinate Ni(I) silyl complex: CO2 insertion and
 oxidatively-induced silyl migrations
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03128F
_journal_year                    2019
_chemical_formula_moiety         'C36 H63 N2 Ni Si4'
_chemical_formula_sum            'C36 H63 N2 Ni Si4'
_chemical_formula_weight         694.95
_chemical_name_common            RJW_3_034
_chemical_name_systematic        IPrNiSi(SiMe3)3
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-27 deposited with the CCDC.    2019-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.886(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9291(11)
_cell_length_b                   18.3739(18)
_cell_length_c                   21.345(2)
_cell_measurement_reflns_used    8559
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.67
_cell_measurement_theta_min      2.18
_cell_volume                     4245.8(7)
_computing_cell_refinement       'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX2 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.34A Bruker-AXS, Madison WI'
_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      99.98
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2168
_diffrn_reflns_av_unetI/netI     0.1183
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            115097
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.886
_diffrn_reflns_theta_min         1.468
_diffrn_source                   'microfocus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  0.9801
_exptl_absorpt_correction_T_min  0.7331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_description       plate
_exptl_crystal_F_000             1508
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.798
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         8175
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1583
_refine_ls_R_factor_gt           0.0849
_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^)+(0.0916P)^2^+11.7991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1931
_refine_ls_wR_factor_ref         0.2283
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4923
_reflns_number_total             8175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03128f2.cif
_cod_data_source_block           rjw_3_034_0m
_cod_original_cell_volume        4245.7(7)
_cod_database_code               7123412
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.943
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C22(H22), C13(H13), C25(H25), C10(H10)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C8(H8), C6(H6), C7(H7), C18(H18), C20(H20), C19(H19)
2.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C35(H35A,H35B,H35C), C34(H34A,H34B,H34C), C14(H14A,H14B,
 H14C), C28(H28A,H28B,H28C), C15(H15A,H15B,H15C), C12(H12A,H12B,H12C), C29(H29A,
 H29B,H29C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C),
 C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C11(H11A,H11B,H11C), C27(H27A,H27B,
 H27C), C23(H23A,H23B,H23C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              3594
_olex2_submission_special_instructions 'No special instructions were received'