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_7705163
_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         'C30 H46 Br0.84 Cl3.16 Mn N4 Si2'
_chemical_formula_sum            'C30 H46 Br0.84 Cl3.16 Mn N4 Si2'
_chemical_formula_weight         752.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-30
_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                77.080(4)
_cell_angle_beta                 79.212(4)
_cell_angle_gamma                73.855(4)
_cell_formula_units_Z            2
_cell_length_a                   10.5954(9)
_cell_length_b                   10.9184(8)
_cell_length_c                   17.2222(14)
_cell_measurement_reflns_used    6237
_cell_measurement_temperature    150.03
_cell_measurement_theta_max      26.433
_cell_measurement_theta_min      2.449
_cell_volume                     1848.6(3)
_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      150.03
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0814
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35332
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         2.443
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.583
_exptl_absorpt_correction_T_max  0.0277
_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 0.0768 before and 0.0595 after correction. The Ratio of minimum to maximum transmission is 0.3755. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Diethyl Ether'
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7211
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0372P)^2^+1.5811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.1096
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4630
_reflns_number_total             7211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00570c2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7705159--7705168.cif.'
_cod_database_code               7705163
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.845
_shelx_estimated_absorpt_t_min   0.623
_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. Restrained distances
 C11-C28 \\sim C11-C33
 with sigma of 0.02
 C11-C29 \\sim C11-C32
 with sigma of 0.02
 C11-C30 \\sim C11-C31
 with sigma of 0.02
3. Others
 Sof(Br1)=1-FVAR(1)
 Sof(Cl1)=FVAR(1)
 Sof(Br2)=1-FVAR(2)
 Sof(Cl2)=FVAR(2)
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=1-FVAR(3)
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(3)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C12(H12), C13(H13), C15(H15), C17(H17), C18(H18), C21(H21), C24(H24),
 C25(H25), C26(H26)
4.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              33126
_olex2_submission_special_instructions 'No special instructions were received'