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_7717005
_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         'C38 H68 Cl3 Fe N4 P2 Si2'
_chemical_formula_sum            'C38 H68 Cl3 Fe N4 P2 Si2'
_chemical_formula_weight         861.28
_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                 92.5530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6644(2)
_cell_length_b                   20.2740(3)
_cell_length_c                   16.7641(2)
_cell_measurement_reflns_used    18494
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      75.7720
_cell_measurement_theta_min      3.2470
_cell_volume                     4639.58(11)
_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 0.996
_diffrn_measured_fraction_theta_max 0.945
_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    -27.00  17.00   0.50    0.10    --  -48.42  19.00 150.00   88
  2  \w    -65.00 -38.00   0.50    0.50    --  -91.75  57.00  90.00   54
  3  \w    -60.00 -25.00   0.50    0.50    --  -91.75  57.00 -30.00   70
  4  \w    -22.00   4.00   0.50    0.10    --  -48.42  19.00-180.00   52
  5  \w    -54.00 -26.00   0.50    0.50    --  -91.75  57.00-120.00   56
  6  \w   -152.00 -85.00   0.50    0.50    --  -91.75 -38.00   0.00  134
  7  \w   -160.00-112.00   0.50    0.50    --  -91.75 -85.00 -55.00   96
  8  \w   -120.00 -74.00   0.50    0.10    --  -48.42-125.00  30.00   92
  9  \w   -120.00 -74.00   0.50    0.10    --  -48.42-125.00  90.00   92
 10  \w   -165.00 -83.00   0.50    0.50    --  -91.75 -38.00 -30.00  164
 11  \w    -69.00 -44.00   0.50    0.50    --  -91.75  85.00  64.00   50
 12  \w    -75.00  24.00   0.50    0.10    --  -48.42  85.00  64.00  198
 13  \w     36.00  62.00   0.50    0.50    --  106.65 -77.00-150.00   52
 14  \w     36.00  61.00   0.50    0.50    --  106.65 -57.00-150.00   50
 15  \w     65.00 105.00   0.50    0.50    --  106.65 -77.00-150.00   80
 16  \w     37.00  66.00   0.50    0.50    --  106.65 -57.00 -30.00   58
 17  \w     37.00  63.00   0.50    0.50    --  106.65 -57.00   0.00   52
 18  \w     36.00  62.00   0.50    0.50    --  106.65 -57.00  90.00   52
 19  \w     34.00  93.00   0.50    0.10    --   48.42-125.00  60.00  118
 20  \w     46.00  71.00   0.50    0.10    --   48.42 -85.00 -55.00   50
 21  \w      4.00  40.00   0.50    0.10    --   48.42 -85.00 -55.00   72
 22  \w     57.00 128.00   0.50    0.50    --  106.65 -85.00 -55.00  142
 23  \w    104.00 176.00   0.50    0.50    --  106.65  38.00-180.00  144
 24  \w     94.00 167.00   0.50    0.50    --  106.65  57.00  30.00  146
 25  \w    104.00 168.00   0.50    0.50    --  106.65  85.00  64.00  128
;
_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  0.0495
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36306
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.555
_diffrn_reflns_theta_min         3.237
_exptl_absorpt_coefficient_mu    5.567
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64284
_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    1.233
_exptl_crystal_description       block
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.502
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         9217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+7.1359P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1381
_refine_ls_wR_factor_ref         0.1439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7937
_reflns_number_total             9217
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02057j2.cif
_cod_data_source_block           231208f_auto
_cod_depositor_comments
'Adding full bibliography for 7717003--7717006.cif.'
_cod_database_code               7717005
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.768
_shelx_estimated_absorpt_t_min   0.634
_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:
 C33(H33), C6(H6), C5(H5), C3(H3), C34(H34), C4(H4), C36(H36), C35(H35)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C20(H20A,H20B,H20C), C17(H17A,H17B,H17C), C11(H11A,H11B,H11C), C19(H19A,
 H19B,H19C), C1(H1A,H1B,H1C), C23(H23A,H23B,H23C), C15(H15A,H15B,H15C), C9(H9A,
 H9B,H9C), C13(H13A,H13B,H13C), C12(H12A,H12B,H12C), C27(H27A,H27B,H27C),
 C26(H26A,H26B,H26C), C14(H14A,H14B,H14C), C29(H29A,H29B,H29C), C38(H38A,H38B,
 H38C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              14227
_shelx_hkl_checksum              95678
_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
;