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_7705162
_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         'C60 H120 Cl2 Fe2 N8 Si10'
_chemical_formula_sum            'C60 H120 Cl2 Fe2 N8 Si10'
_chemical_formula_weight         1417.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-26 deposited with the CCDC.	2020-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.4720(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   37.0728(13)
_cell_length_b                   13.2937(5)
_cell_length_c                   17.4231(6)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      74.52
_cell_measurement_theta_min      5.08
_cell_volume                     8044.4(5)
_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      149.87
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0679
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18524
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.238
_diffrn_reflns_theta_min         2.544
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.223
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.4917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1079 before and 0.0628 after correction.
The Ratio of minimum to maximum transmission is 0.6523.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       block
_exptl_crystal_F_000             3048
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         7108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+3.0977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6272
_reflns_number_total             7108
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00570c2.cif
_cod_data_source_block           11
_cod_depositor_comments
'Adding full bibliography for 7705159--7705168.cif.'
_cod_database_code               7705162
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.573
_shelx_estimated_absorpt_t_min   0.421
_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 Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C8(H8), C5(H5), C7(H7), C6(H6)
2.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C24(H24A,H24B,H24C), C16(H16A,H16B,H16C), C23(H23A,H23B,
 H23C), C13(H13A,H13B,H13C), C19(H19A,H19B,H19C), C14(H14A,H14B,H14C), C20(H20A,
 H20B,H20C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C17(H17A,H17B,H17C),
 C00Z(H00A,H00B,H00C), C28(H28A,H28B,H28C), C26(H26A,H26B,H26C), C012(H01A,H01B,
 H01C), C22(H22A,H22B,H22C), C12(H12A,H12B,H12C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              5077
_olex2_submission_special_instructions 'No special instructions were received'