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_7717006
_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 Fe N4 P2 Si2'
_chemical_formula_sum            'C44 H80 Cl3 Fe N4 P2 Si2'
_chemical_formula_weight         945.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 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                 111.412(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.6307(4)
_cell_length_b                   10.3205(2)
_cell_length_c                   24.7701(5)
_cell_measurement_reflns_used    9827
_cell_measurement_temperature    173.01(18)
_cell_measurement_theta_max      76.3030
_cell_measurement_theta_min      3.8100
_cell_volume                     5148.01(19)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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     73.00 103.00   0.50    0.20    --  106.65 -77.00-180.00   60
  2  \w     75.00 103.00   0.50    0.20    --  106.65 -99.00-150.00   56
  3  \w     42.00  90.00   0.50    0.20    --  106.65 -99.00 -60.00   96
  4  \w     34.00  63.00   0.50    0.20    --  106.65 -57.00   0.00   58
  5  \w     34.00  66.00   0.50    0.20    --  106.65 -57.00  30.00   64
  6  \w     49.00  94.00   0.50    0.20    --  106.65 -99.00  60.00   90
  7  \w     66.00  98.00   0.50    0.20    --  106.65 -77.00  60.00   64
  8  \w     34.00  59.00   0.50    0.20    --  106.65 -57.00  90.00   50
  9  \w     34.00  65.00   0.50    0.20    --  106.65 -57.00  60.00   62
 10  \w     55.00 117.00   0.50    0.07    --   48.42  32.00 164.00  124
 11  \w     94.00 171.00   0.50    0.20    --  106.65  32.00 164.00  154
 12  \w      2.00  37.00   0.50    0.07    --   48.42 -32.00   5.00   70
 13  \w     -5.00  24.00   0.50    0.07    --  -48.42  32.00 164.00   58
 14  \w    -37.00  -8.00   0.50    0.07    --  -48.42  32.00 164.00   58
 15  \w    -25.00  25.00   0.50    0.07    --  -48.42  19.00 -30.00  100
 16  \w    -66.00 -32.00   0.50    0.20    --  -91.75  57.00 -30.00   68
 17  \w    -66.00 -29.00   0.50    0.20    --  -91.75  57.00-120.00   74
 18  \w    -64.00 -20.00   0.50    0.20    --  -91.75  57.00-150.00   88
 19  \w    -62.00 -24.00   0.50    0.20    --  -91.75  57.00-180.00   76
 20  \w   -148.00 -78.00   0.50    0.20    --  -91.75 -57.00-120.00  140
 21  \w   -104.00 -74.00   0.50    0.07    --  -48.42-125.00 -60.00   60
 22  \w   -111.00 -75.00   0.50    0.07    --  -48.42-125.00 -30.00   72
 23  \w   -104.00 -79.00   0.50    0.20    --  -91.75 -32.00   5.00   50
 24  \w   -122.00 -42.00   0.50    0.07    --  -48.42 -32.00   5.00  160
 25  \w   -159.00-103.00   0.50    0.20    --  -91.75 -99.00 150.00  112
;
_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  0.0605
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            17284
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.594
_diffrn_reflns_theta_max         66.594
_diffrn_reflns_theta_min         3.834
_exptl_absorpt_coefficient_mu    5.060
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49896
_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    1.220
_exptl_crystal_description       block
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.373
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0994P)^2^+15.8662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1657
_refine_ls_wR_factor_ref         0.1710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3998
_reflns_number_total             4515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02057j2.cif
_cod_data_source_block           231124a_auto
_cod_depositor_comments
'Adding full bibliography for 7717003--7717006.cif.'
_cod_original_cell_volume        5148.01(18)
_cod_database_code               7717006
_shelx_shelxl_version_number     2018/3
_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:
 C6(H6), C8(H8), C9(H9), C7(H7)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C2(H2A,H2B,H2C), C16(H16A,H16B,H16C), C22(H22A,H22B,
 H22C), C3(H3A,H3B,H3C), C12(H12A,H12B,H12C), C1(H1A,H1B,H1C), C21(H21A,H21B,
 H21C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C14(H14A,H14B,H14C), C13(H13A,
 H13B,H13C)
;
_shelx_res_checksum              20015
_shelx_hkl_checksum              4170
_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
;