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_7705167
_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         'C42 H82 Cl4 Mn2 N6 Si6'
_chemical_formula_sum            'C42 H82 Cl4 Mn2 N6 Si6'
_chemical_formula_weight         1091.35
_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             2019-10-15
_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                 106.756(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.052(3)
_cell_length_b                   13.466(2)
_cell_length_c                   16.318(2)
_cell_measurement_reflns_used    3227
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.724
_cell_volume                     2956.7(9)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0943
_diffrn_reflns_av_unetI/netI     0.1195
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19446
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         2.267
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0774 before and 0.0592 after correction. The Ratio of minimum to maximum transmission is 0.3659. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       block
_exptl_crystal_F_000             1156
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Diethyl Ether'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.436
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         5774
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1238
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0919P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.1937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3395
_reflns_number_total             5774
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00570c2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7705159--7705168.cif.'
_cod_original_cell_volume        2956.9(9)
_cod_database_code               7705167
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.888
_shelx_estimated_absorpt_t_min   0.827
_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
 C131-C133 \\sim C131-C132 \\sim C133-C132 \\sim C14-C13 \\sim C14-C15 \\sim
C13-C15
 with sigma of 0.04
 C12-N2 \\sim C12-C131 \\sim C12-C133 \\sim C12-C132 \\sim C12-C14 \\sim
C12-C13 \\sim C12-C15
 with sigma of 0.02
3. Others
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C13)=Sof(H13J)=Sof(H13K)=Sof(H13L)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=1-FVAR(1)
 Sof(C131)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C133)=Sof(H13D)=Sof(H13E)=
 Sof(H13F)=Sof(C132)=Sof(H13G)=Sof(H13H)=Sof(H13I)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C6(H6), C5(H5), C4(H4)
4.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C10(H10A,H10B,
 H10C), C17(H17A,H17B,H17C), C9(H9A,H9B,H9C), C19(H19A,H19B,H19C), C11(H11A,
 H11B,H11C), C18(H18A,H18B,H18C), C131(H13A,H13B,H13C), C133(H13D,H13E,H13F),
 C132(H13G,H13H,H13I), C14(H14A,H14B,H14C), C13(H13J,H13K,H13L), C15(H15A,H15B,
 H15C)
;
_olex2_submission_special_instructions 'No special instructions were received'