Synthesis of aryl cobalt and iron complexes and their catalytic activity on hydrosilylation of alkenes
Huang, Wei; Lu, Jiahui; Fan, Qingqing; Li, Xiaoyan; Hinz, Alexander; Sun, Hongjian; New Journal of Chemistry 46 (2022) 7512–7521; doi:10.1039/D1NJ06133J

data_7061389
_publ_section_title
;
 Synthesis of aryl cobalt and iron complexes and their catalytic activity
 on hydrosilylation of alkenes
;
_journal_issue                   16
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7512
_journal_page_last               7521
_journal_paper_doi               10.1039/D1NJ06133J
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C14 H27 Cl Co F4 N P3'
_chemical_formula_sum            'C14 H27 Cl Co F4 N P3'
_chemical_formula_weight         472.65
_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
_audit_creation_date             2022-01-13
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.12.21 svn.raa29eb21 for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2022-02-25 deposited with the CCDC.	2022-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.586(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2381(2)
_cell_length_b                   15.2301(4)
_cell_length_c                   15.7220(4)
_cell_measurement_reflns_used    4664
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      75.1320
_cell_measurement_theta_min      5.7190
_cell_volume                     2120.00(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.00(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     95.00 176.00   1.00    0.40    --  106.49 125.00  30.00   81
  2  \w    104.00 161.00   1.00    0.40    --  106.49 120.00-177.00   57
  3  \w     80.00 105.00   1.00    0.40    --  106.49 -77.00-180.00   25
  4  \w     35.00  62.00   1.00    0.40    --  106.49 -77.00-180.00   27
  5  \w     38.00  66.00   1.00    0.40    --  106.49 -57.00 -90.00   28
  6  \w     34.00  65.00   1.00    0.40    --  106.49 -57.00  60.00   31
  7  \w     34.00  66.00   1.00    0.40    --  106.49 -57.00 120.00   32
  8  \w     36.00 104.00   1.00    0.40    --  106.49 -99.00 120.00   68
  9  \w     75.00 108.00   1.00    0.40    --  106.49-120.00  98.00   33
 10  \w     38.00  63.00   1.00    0.13    --   48.45-120.00  98.00   25
 11  \w     61.00  88.00   1.00    0.40    --  106.49-155.00 -58.00   27
 12  \w    106.00 132.00   1.00    0.40    --  106.49-155.00 -58.00   26
 13  \w     58.00  84.00   1.00    0.13    --   48.45-155.00 -58.00   26
 14  \w    -42.00 -14.00   1.00    0.40    --  -86.25  38.00 150.00   28
 15  \w    -39.00  -9.00   1.00    0.13    --  -48.45 120.00-177.00   30
 16  \w    -81.00 -23.00   1.00    0.40    --  -86.25 120.00-177.00   58
 17  \w    -43.00 -13.00   1.00    0.40    --  -86.25  38.00   0.00   30
 18  \w    -43.00 -17.00   1.00    0.40    --  -86.25  38.00  30.00   26
 19  \w   -157.00 -73.00   1.00    0.40    --  -86.25 -19.00 -90.00   84
 20  \w   -142.00-117.00   1.00    0.40    --  -86.25-120.00  98.00   25
 21  \w   -119.00 -53.00   1.00    0.13    --  -48.45-155.00 -58.00   66
 22  \w   -127.00 -59.00   1.00    0.40    --  -86.25-155.00 -58.00   68
 23  \w   -120.00 -28.00   1.00    0.13    --  -48.45 -77.00-150.00   92
;
_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_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6948
_diffrn_reflns_point_group_measured_fraction_full 0.642
_diffrn_reflns_point_group_measured_fraction_max 0.642
_diffrn_reflns_theta_full        67.074
_diffrn_reflns_theta_max         67.074
_diffrn_reflns_theta_min         5.780
_exptl_absorpt_coefficient_mu    9.947
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       block
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.002(4)
_refine_ls_extinction_coef       0.00049(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         2431
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0486P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0760
_reflns_Friedel_coverage         0.299
_reflns_Friedel_fraction_full    0.297
_reflns_Friedel_fraction_max     0.297
_reflns_number_gt                2353
_reflns_number_total             2431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj06133j2.cif
_cod_data_source_block           201216f
_cod_depositor_comments
'Adding full bibliography for 7061389--7061390.cif.'
_cod_original_cell_volume        2119.99(9)
_cod_database_code               7061389
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.692
_shelx_estimated_absorpt_t_min   0.587
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Co1-C5 \\sim Co1-C5A
 with sigma of 0.02
 N1-C5 \\sim N1A-C5A
 with sigma of 0.04
 F4-C4 \\sim F4A-C4A
 with sigma of 0.02
 C4-C1 \\sim C4A-C1A
 with sigma of 0.04
 F1-C1 \\sim F1A-C1A
 with sigma of 0.02
 N1-C2 \\sim N1A-C2A
 with sigma of 0.02
 N1-C1 \\sim N1A-C1A
 with sigma of 0.02
 N1-C3 \\sim N1A-C3A
 with sigma of 0.04
 C5-C4 \\sim C5A-C4A
 with sigma of 0.02
 F3-C2 \\sim F3A-C2A
 with sigma of 0.04
 C5-C1 \\sim C5A-C1A
 with sigma of 0.02
 C2-C1 \\sim C2A-C1A
 with sigma of 0.04
 F3-C3 \\sim F3A-C3A
 with sigma of 0.02
 C2-F2 \\sim C2A-F2A
 with sigma of 0.02
 N1-F2 \\sim N1A-F2A
 with sigma of 0.04
 C2-C3 \\sim C2A-C3A
 with sigma of 0.02
 C5-C3 \\sim C5A-C3A
 with sigma of 0.04
 F3-C4 \\sim F3A-C4A
 with sigma of 0.04
 C2-C4 \\sim C2A-C4A
 with sigma of 0.04
 C4-C3 \\sim C4A-C3A
 with sigma of 0.02
 F2-C3 \\sim F2A-C3A
 with sigma of 0.04
 Co1-C4 \\sim Co1-C4A
 with sigma of 0.04
 Co1-C1 \\sim Co1-C1A
 with sigma of 0.04
 F4-C5 \\sim F4A-C5A
 with sigma of 0.04
 F4-C3 \\sim F4A-C3A
 with sigma of 0.04
 F1-N1 \\sim F1A-N1A
 with sigma of 0.04
 F1-C5 \\sim F1A-C5A
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 N1, F4, C4, C5, C3, C1, F3, C2, F1, F2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(N1A)=Sof(F4A)=Sof(C4A)=Sof(C5A)=Sof(C3A)=Sof(C1A)=Sof(F3A)=Sof(C2A)=
 Sof(F1A)=Sof(F2A)=1-FVAR(1)
 Sof(F4)=Sof(F1)=Sof(N1)=Sof(C5)=Sof(F3)=Sof(C2)=Sof(F2)=Sof(C4)=Sof(C3)=
 Sof(C1)=FVAR(1)
5.a Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C),
 C13(H13A,H13B,H13C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C7(H7A,H7B,H7C),
  C10(H10A,H10B,H10C)
;
_shelx_res_checksum              61572
_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
;