Aminolysis of bis[bis(trimethylsilyl)amido]-manganese, -iron, and -cobalt for the synthesis of mono- and bis-silylene complexes.
He, Zhiyuan; Xue, Xiaolian; Liu, Yilan; Yu, Na; Krogman, Jeremy P.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 12586–12591; doi:10.1039/d0dt00570c

data_7705160
_publ_section_title
;
 Aminolysis of bis[bis(trimethylsilyl)amido]-manganese, -iron, and -cobalt
 for the synthesis of mono- and bis-silylene complexes.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12586
_journal_page_last               12591
_journal_paper_doi               10.1039/d0dt00570c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'C36 H52 Cl2 Co N4 Si2, 0.5(Cl6 Co2), 2(C6 H6)'
_chemical_formula_sum            'C48 H64 Cl5 Co2 N4 Si2'
_chemical_formula_weight         1048.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-14 deposited with the CCDC.	2020-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.706(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.502(2)
_cell_length_b                   13.2285(9)
_cell_length_c                   18.1814(15)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.369
_cell_measurement_theta_min      2.530
_cell_volume                     5643.2(7)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      149.99
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36261
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         2.309
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.900
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0866 before and 0.0599 after correction. The Ratio of minimum to maximum transmission is 0.3768. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             2188
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Benzene'
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.151
_refine_diff_density_max         2.130
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         5730
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1451P)^2^+14.0619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2220
_refine_ls_wR_factor_ref         0.2481
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4111
_reflns_number_total             5730
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00570c2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7705159--7705168.cif.'
_cod_original_cell_volume        5643.3(8)
_cod_database_code               7705160
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.876
_shelx_estimated_absorpt_t_min   0.819
_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. Rigid body (RIGU) restrains
 C26, H26, C27, H27, C28, H28, C29, H29, C30, H30, C31, H31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C26A, H26A, C27A, H27A, C28A, H28A, C29A, H29A, C30A, H30A, C31A, H31A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C29A)=Sof(H29A)=Sof(C28A)=Sof(H28A)=Sof(C27A)=Sof(H27A)=Sof(C26A)=
 Sof(H26A)=Sof(C31A)=Sof(H31A)=Sof(C30A)=Sof(H30A)=1-FVAR(1)
 Sof(C26)=Sof(H26)=Sof(C31)=Sof(H31)=Sof(C30)=Sof(H30)=Sof(C29)=Sof(H29)=
 Sof(C28)=Sof(H28)=Sof(C27)=Sof(H27)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C23(H23), C24(H24), C25(H25)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C26(H26), C31(H31), C30(H30), C29(H29), C28(H28), C27(H27),
  C29A(H29A), C28A(H28A), C27A(H27A), C26A(H26A), C31A(H31A), C30A(H30A)
4.c Fitted hexagon refined as free rotating group:
 C26(C31,C30,C29,C28,C27), C29A(C28A,C27A,C26A,C31A,C30A)
4.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              42045
_shelx_fab_checksum              64913
_olex2_submission_special_instructions 'No special instructions were received'