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_7705165
_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 H48 Cl4 N4 Si2, C7 H8'
_chemical_formula_sum            'C43 H56 Cl4 N4 Si2'
_chemical_formula_weight         826.89
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-07-26 deposited with the CCDC.	2020-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.199(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9514(9)
_cell_length_b                   19.3184(16)
_cell_length_c                   19.1714(17)
_cell_measurement_reflns_used    9383
_cell_measurement_temperature    150.02
_cell_measurement_theta_max      25.529
_cell_measurement_theta_min      2.361
_cell_volume                     4425.4(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.02
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.1131
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            146405
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.442
_diffrn_reflns_theta_min         2.252
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6934
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.969
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         9066
_refine_ls_number_restraints     459
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.1360
_refine_ls_R_factor_gt           0.0989
_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^)+(0.0512P)^2^+11.3538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1858
_refine_ls_wR_factor_ref         0.2012
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6557
_reflns_number_total             9066
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00570c2.cif
_cod_data_source_block           10
_cod_depositor_comments
'Adding full bibliography for 7705159--7705168.cif.'
_cod_database_code               7705165
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.932
_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
 Si2-Cl3 \\sim Si2-Cl4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
4. Others
 1*[Sof(Si2)+Sof(Cl4)+Sof(Cl3)]+1*[Sof(Si2A)+Sof(Cl4A)+Sof(Cl3A)]+1*[Sof(Si2B)+
 Sof(Cl4B)+Sof(Cl3B)]=1 with esd of 0.0001
 1*[Sof(Cl1)]+1*[Sof(Cl1A)]+1*[Sof(Cl1B)]=1 with esd of 0.0001
 Sof(Si2)=Sof(Cl4)=Sof(Cl3)=FVAR(1)
 Sof(Si2A)=Sof(Cl4A)=Sof(Cl3A)=FVAR(5)
 Sof(Si2B)=Sof(Cl4B)=Sof(Cl3B)=FVAR(6)
5.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C20(H20), C17(H17), C18(H18), C11(H11), C14(H14), C13(H13),
 C12(H12), C26(H26), C23(H23), C24(H24), C25(H25), C017(H017), C018(H018),
 C01B(H01B), C01C(H01C), C01E(H01E)
5.b Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C),
 C4(H4A,H4B,H4C), C30(H30A,H30B,H30C), C2(H2A,H2B,H2C), C32(H32A,H32B,H32C),
 C9(H9A,H9B,H9C), C3(H3A,H3B,H3C), C34(H34A,H34B,H34C), C31(H31A,H31B,H31C),
 C01I(H01A,H01D,H01F)
;
_shelx_res_checksum              90910
_olex2_submission_special_instructions 'No special instructions were received'