Dinitrogen silylation catalyzed by silylene cobalt(I) and silylene iron(I) chlorides.
Fan, Qingqing; Li, Qingshuang; Sun, Hongjian; Li, Xiaoyan; Dalton transactions (Cambridge, England : 2003) 53 (2024) 16261–16270; doi:10.1039/d4dt02057j

data_7717003
_publ_section_title
;
 Dinitrogen silylation catalyzed by silylene cobalt(I) and silylene
 iron(I) chlorides.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16261
_journal_page_last               16270
_journal_paper_doi               10.1039/d4dt02057j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C44 H80 Cl3 Co N4 P2 Si2'
_chemical_formula_sum            'C44 H80 Cl3 Co N4 P2 Si2'
_chemical_formula_weight         948.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-06-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-06-28 deposited with the CCDC.	2024-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.3210(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.4451(2)
_cell_length_b                   10.29200(10)
_cell_length_c                   25.0566(3)
_cell_measurement_reflns_used    21194
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.1510
_cell_measurement_theta_min      3.6960
_cell_volume                     5249.99(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -105.00 -23.00   0.50    0.50    --  -91.75  77.00   0.00  164
  2  \w    -56.00 -20.00   0.50    0.50    --  -91.75  57.00 -30.00   72
  3  \w    -64.00 -24.00   0.50    0.50    --  -91.75  57.00   0.00   80
  4  \w    -45.00 -20.00   0.50    0.50    --  -91.75  57.00  30.00   50
  5  \w    -66.00 -31.00   0.50    0.50    --  -91.75  57.00  60.00   70
  6  \w    -61.00 -19.00   0.50    0.50    --  -91.75  57.00-120.00   84
  7  \w    -66.00 -22.00   0.50    0.50    --  -91.75  57.00 -60.00   88
  8  \w   -121.00 -37.00   0.50    0.10    --  -48.42 -36.00  77.00  168
  9  \w   -121.00 -74.00   0.50    0.10    --  -48.42-125.00  30.00   94
 10  \w   -122.00 -95.00   0.50    0.50    --  -91.75 -36.00  77.00   54
 11  \w     55.00  80.00   0.50    0.10    --   48.42  36.00-126.00   50
 12  \w    113.00 141.00   0.50    0.50    --  106.65  36.00-126.00   56
 13  \w     92.00 173.00   0.50    0.50    --  106.65  57.00-120.00  162
 14  \w    129.00 170.00   0.50    0.50    --  106.65  38.00 -30.00   82
 15  \w     51.00 104.00   0.50    0.50    --  106.65 -77.00 120.00  106
 16  \w     34.00  66.00   0.50    0.50    --  106.65 -57.00 150.00   64
 17  \w     40.00  66.00   0.50    0.50    --  106.65 -57.00 120.00   52
 18  \w     37.00  63.00   0.50    0.50    --  106.65 -57.00  90.00   52
 19  \w     47.00 104.00   0.50    0.50    --  106.65 -77.00  60.00  114
 20  \w    -11.00  36.00   0.50    0.10    --   48.42 -36.00  77.00   94
 21  \w     34.00  66.00   0.50    0.50    --  106.65 -57.00-180.00   64
 22  \w     52.00  78.00   0.50    0.50    --  106.65-125.00 -30.00   52
 23  \w     86.00 111.00   0.50    0.50    --  106.65-125.00 -30.00   50
 24  \w    -39.00 -10.00   0.50    0.10    --  -48.42  36.00-126.00   58
 25  \w    -43.00  23.00   0.50    0.10    --  -48.42  38.00 -90.00  132
 26  \w    -24.00  26.00   0.50    0.10    --  -48.42  19.00  30.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            39439
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.424
_diffrn_reflns_theta_min         3.668
_exptl_absorpt_coefficient_mu    5.221
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         10368
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0475P)^2^+3.3138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0973
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9403
_reflns_number_total             10368
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02057j2.cif
_cod_data_source_block           231108b_auto
_cod_depositor_comments
'Adding full bibliography for 7717003--7717006.cif.'
_cod_original_cell_volume        5249.98(10)
_cod_database_code               7717003
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.745
_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
 C4-C3 \\sim C4-C3A \\sim C4-C2 \\sim C4-C2A \\sim C4-C1 \\sim C4-C1A
 with sigma of 0.02
 C3A-C1A \\sim C3A-C2A \\sim C2A-C1A
 with sigma of 0.02
 C3-C2 \\sim C3-C1 \\sim C2-C1
 with sigma of 0.02
 C5-C1 \\sim C5-C3 \\sim C5-C2
 with sigma of 0.02
 C5-C1A \\sim C5-C2A \\sim C5-C3A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C3, C2, C1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C1A, C3A, C2A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Others
 Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C36(H36), C39(H39), C37(H37), C40(H40), C9(H9), C6(H6), C7(H7), C10(H10)
5.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C42(H42A,H42B,H42C), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C24(H24A,H24B,H24C), C21(H21A,H21B,H21C), C13(H13A,
 H13B,H13C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C27(H27A,H27B,H27C),
 C31(H31A,H31B,H31C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C30(H30A,H30B,
 H30C), C22(H22A,H22B,H22C), C32(H32A,H32B,H32C), C14(H14A,H14B,H14C), C12(H12A,
 H12B,H12C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C), C2(H2A,H2B,H2C), C1(H1A,
 H1B,H1C), C3(H3A,H3B,H3C), C2A(H2AA,H2AB,H2AC), C1A(H1AA,H1AB,H1AC), C3A(H3AA,
 H3AB,H3AC)
;
_shelx_res_checksum              93819
_shelx_hkl_checksum              50913
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;