Effects of silylene ligands on the catalytic activity of [PSiP] pincer cobalt(ii) chloride for N2 silylation
Zhang, Min; Dong, Yanhong; Li, Qingshuang; Li, Xiaoyan; Sun, Hongjian; New Journal of Chemistry 48 (2024) 7334–7339; doi:10.1039/D4NJ00883A

data_7063100
_publ_section_title
;
 Effects of silylene ligands on the catalytic activity of [PSiP] pincer
 cobalt(ii) chloride for N2 silylation
;
_journal_issue                   16
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7334
_journal_page_last               7339
_journal_paper_doi               10.1039/D4NJ00883A
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C52 H54 Cl2 Co N2 P2 Si2'
_chemical_formula_sum            'C52 H54 Cl2 Co N2 P2 Si2'
_chemical_formula_weight         954.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-03-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-03-11 deposited with the CCDC.	2024-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.3770(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8498(2)
_cell_length_b                   16.2943(2)
_cell_length_c                   18.5455(2)
_cell_measurement_reflns_used    17638
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.2900
_cell_measurement_theta_min      3.8920
_cell_volume                     4738.49(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_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.974
_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   -119.00 -39.00   1.00    1.20    --  -48.67 -61.00  99.00   80
  2  \w    -60.00  18.00   1.00    1.20    --  -48.67  61.00-122.00   78
  3  \w    -16.00  59.00   1.00    1.20    --   48.67 -61.00  99.00   75
  4  \w     35.00  99.00   1.00    1.20    --   48.67  61.00-122.00   64
  5  \w    -52.00 -26.00   1.00    4.10    --  -91.75  61.00-122.00   26
  6  \w   -152.00 -81.00   1.00    4.10    --  -91.75 -61.00  99.00   71
  7  \w    116.00 172.00   1.00    4.10    --  106.65  61.00-122.00   56
  8  \w     34.00  70.00   1.00    4.10    --  106.65 -61.00  99.00   36
  9  \w    -33.00  -7.00   1.00    1.20    --  -48.67  57.00 150.00   26
 10  \w   -120.00 -86.00   1.00    1.20    --  -48.67-125.00  30.00   34
 11  \w   -119.00 -73.00   1.00    1.20    --  -48.67-125.00-180.00   46
 12  \w     -2.00  24.00   1.00    1.20    --  -48.67  57.00 150.00   26
 13  \w     38.00  90.00   1.00    1.20    --   48.67-125.00 -30.00   52
 14  \w   -119.00 -93.00   1.00    4.10    --  -91.75 -99.00-180.00   26
 15  \w    -56.00 -20.00   1.00    4.10    --  -91.75  77.00  60.00   36
 16  \w    -66.00 -24.00   1.00    4.10    --  -91.75  57.00   0.00   42
 17  \w    -86.00 -20.00   1.00    4.10    --  -91.75  77.00-150.00   66
 18  \w    -64.00 -20.00   1.00    4.10    --  -91.75  57.00  60.00   44
 19  \w   -102.00 -64.00   1.00    4.10    --  -91.75  77.00  60.00   38
 20  \w     35.00  65.00   1.00    4.10    --  106.65 -57.00 -90.00   30
 21  \w     41.00 101.00   1.00    4.10    --  106.65 -77.00  60.00   60
 22  \w     96.00 121.00   1.00    4.10    --  106.65 125.00-120.00   25
 23  \w    130.00 158.00   1.00    4.10    --  106.65  38.00   0.00   28
 24  \w     98.00 124.00   1.00    4.10    --  106.65  38.00   0.00   26
 25  \w     61.00  94.00   1.00    4.10    --  106.65 -99.00-150.00   33
 26  \w     66.00  92.00   1.00    4.10    --  106.65 -99.00 -60.00   26
 27  \w    144.00 169.00   1.00    4.10    --  106.65   0.00  30.00   25
 28  \w     39.00  65.00   1.00    4.10    --  106.65 -57.00-120.00   26
 29  \w     41.00 107.00   1.00    4.10    --  106.65   0.00  30.00   66
 30  \w     59.00 111.00   1.00    4.10    --  106.65-125.00-150.00   52
 31  \w     64.00  99.00   1.00    4.10    --  106.65 -99.00   0.00   35
 32  \w     40.00 117.00   1.00    4.10    --  106.65-132.00 -77.51   77
 33  \w     96.00 140.00   1.00    4.10    --  106.65  19.00-150.00   44
 34  \w    143.00 177.00   1.00    4.10    --  106.65  19.00-150.00   34
 35  \w     79.00 106.00   1.00    4.10    --  106.65 -99.00  60.00   27
 36  \w     43.00 111.00   1.00    4.10    --  106.65-125.00  90.00   68
 37  \w     40.00 105.00   1.00    4.10    --  106.65 -99.00 -90.00   65
 38  \w     71.00 103.00   1.00    4.10    --  106.65 -99.00-180.00   32
 39  \w     39.00  64.00   1.00    4.10    --  106.65 -57.00 -30.00   25
 40  \w    148.00 174.00   1.00    4.10    --  106.65 125.00-120.00   26
 41  \w     39.00  98.00   1.00    4.10    --  106.65 -99.00 -30.00   59
 42  \w     97.00 160.00   1.00    4.10    --  106.65  57.00 150.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0488955000
_diffrn_orient_matrix_UB_12      -0.0554740000
_diffrn_orient_matrix_UB_13      -0.0592568000
_diffrn_orient_matrix_UB_21      -0.0844401000
_diffrn_orient_matrix_UB_22      0.0409545000
_diffrn_orient_matrix_UB_23      0.0119631000
_diffrn_orient_matrix_UB_31      0.0115655000
_diffrn_orient_matrix_UB_32      0.0647277000
_diffrn_orient_matrix_UB_33      -0.0582474000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30338
_diffrn_reflns_point_group_measured_fraction_full 0.893
_diffrn_reflns_point_group_measured_fraction_max 0.846
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.726
_diffrn_reflns_theta_min         3.912
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.287
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79238
_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    1.339
_exptl_crystal_description       block
_exptl_crystal_F_000             1996
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 3136 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.027(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         8452
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0286P)^2^+2.1306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0626
_reflns_Friedel_coverage         0.737
_reflns_Friedel_fraction_full    0.787
_reflns_Friedel_fraction_max     0.719
_reflns_number_gt                8104
_reflns_number_total             8452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj00883a2.cif
_cod_data_source_block           230407e-1_auto
_cod_depositor_comments          'Adding full bibliography for 7063100.cif.'
_cod_database_code               7063100
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CSiNPCoCl
_shelx_estimated_absorpt_t_max   0.778
_shelx_estimated_absorpt_t_min   0.620
_reflns_odcompleteness_completeness 88.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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), C5(H5), C4(H4), C14(H14), C21(H21), C28(H28), C38(H38), C22(H22),
 C27(H27), C29(H29), C10(H10), C2(H2), C23(H23), C12(H12), C36(H36), C8(H8),
 C43(H43), C41(H41), C24(H24), C37(H37), C3(H3), C42(H42), C11(H11), C9(H9),
 C30(H30), C40(H40), C31(H31), C33(H33), C35(H35), C15(H15), C16(H16), C17(H17),
  C34(H34)
2.b Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C46(H46A,H46B,H46C), C51(H51A,H51B,H51C), C45(H45A,H45B,
 H45C), C50(H50A,H50B,H50C), C19(H19A,H19B,H19C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              22483
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.431
_oxdiff_exptl_absorpt_empirical_full_min 0.764