Synthesis and properties of [PCP] pincer silylene cobalt(i) complexes
Li, Yonghui; Fan, Qingqing; Yang, Haiquan; Xie, Shangqing; Huang, Wei; Li, Xiaoyan; Sun, Hongjian; Fuhr, Olaf; Fenske, Dieter; New Journal of Chemistry 45 (2021) 19950–19956; doi:10.1039/D1NJ02982G

data_7060980
_publ_section_title
;
 Synthesis and properties of [PCP] pincer silylene cobalt(i) complexes
;
_journal_issue                   42
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19950
_journal_page_last               19956
_journal_paper_doi               10.1039/D1NJ02982G
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C43 H48 Cl1.007 Co N2 O3 P2 Si'
_chemical_formula_sum            'C43 H48 Cl Co N2 O3 P2 Si'
_chemical_formula_weight         825.24
_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
_audit_creation_date             2021-09-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-16 deposited with the CCDC.	2021-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.7760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7134(2)
_cell_length_b                   12.4172(2)
_cell_length_c                   22.7388(3)
_cell_measurement_reflns_used    10511
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      75.6560
_cell_measurement_theta_min      2.6130
_cell_volume                     4718.63(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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    -80.00  24.00   1.00    0.30    --  -48.45  96.00  43.00  104
  2  \w      9.00  46.00   1.00    0.30    --   48.45 -96.00 -65.00   37
  3  \w   -120.00 -33.00   1.00    0.30    --  -48.45 -57.00 -60.00   87
  4  \w   -159.00 -81.00   1.00    3.00    --  -86.25 -96.00 -65.00   78
  5  \w    -72.00 -47.00   1.00    3.00    --  -86.25  96.00  43.00   25
  6  \w     67.00 109.00   1.00    3.00    --  106.49 -96.00 -65.00   42
  7  \w    105.00 178.00   1.00    3.00    --  106.49  96.00  43.00   73
  8  \w     36.00  89.00   1.00    3.00    --  106.49 -57.00  60.00   53
  9  \w     96.00 121.00   1.00    3.00    --  106.49 -57.00  60.00   25
 10  \w     86.00 178.00   1.00    3.00    --  106.49  77.00 120.00   92
 11  \w     34.00 117.00   1.00    3.00    --  106.49-125.00 -90.00   83
 12  \w     94.00 178.00   1.00    3.00    --  106.49 125.00 150.00   84
;
_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  0.0423
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25008
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        66.596
_diffrn_reflns_theta_max         66.596
_diffrn_reflns_theta_min         2.644
_exptl_absorpt_coefficient_mu    4.537
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       needle
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         8225
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0934P)^2^+2.2768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1554
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6664
_reflns_number_total             8225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj02982g2.cif
_cod_data_source_block           191009c
_cod_depositor_comments
'Adding full bibliography for 7060978--7060981.cif.'
_cod_database_code               7060980
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.660
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Cl1B \\sim Cl1A \\sim Cl1C: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004 within 2A
Uanis(Cl1B) \\sim Ueq, Uanis(Cl1A) \\sim Ueq, Uanis(Cl1C) \\sim Ueq: with sigma
of 0.002 and sigma for terminal atoms of 0.004
3. Others
 1*[Sof(Cl1A)]+1*[Sof(Cl1B)]+1*[Sof(Cl1C)]=1 with esd of 0.001
4.a Ternary CH refined with riding coordinates:
 C30(H30)
4.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C31(H31A,H31B)
4.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C18(H18), C19(H19), C20(H20),
 C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C33(H33),
  C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41),
 C42(H42), C43(H43)
4.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              54183
_shelx_fab_checksum              72994
_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
;