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_7061390
_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         'C17 H36 F4 Fe N P4'
_chemical_formula_sum            'C17 H36 F4 Fe N P4'
_chemical_formula_weight         510.20
_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             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                 98.2920(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9999(2)
_cell_length_b                   10.1154(2)
_cell_length_c                   26.2786(5)
_cell_measurement_reflns_used    6370
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      75.3340
_cell_measurement_theta_min      3.3830
_cell_volume                     2367.33(8)
_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      172.99(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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     92.00 174.00   1.00    0.26    --  106.49  56.00 -50.00   82
  2  \w     94.00 178.00   1.00    0.26    --  106.49  38.00  30.00   84
  3  \w     39.00 117.00   1.00    0.10    --   48.45  56.00 -50.00   78
  4  \w    -21.00  51.00   1.00    0.10    --   48.45 -56.00 167.00   72
  5  \w     34.00  66.00   1.00    0.26    --  106.49 -57.00  30.00   32
  6  \w     35.00  64.00   1.00    0.26    --  106.49 -56.00 167.00   29
  7  \w     39.00  65.00   1.00    0.26    --  106.49 -57.00   0.00   26
  8  \w     34.00 101.00   1.00    0.26    --  106.49 -77.00 -90.00   67
  9  \w     34.00  65.00   1.00    0.26    --  106.49 -57.00-150.00   31
 10  \w     39.00 105.00   1.00    0.26    --  106.49 -99.00   0.00   66
 11  \w     34.00 105.00   1.00    0.26    --  106.49 -99.00-180.00   71
 12  \w    -62.00  22.00   1.00    0.10    --  -48.45  56.00 -50.00   84
 13  \w    -66.00 -19.00   1.00    0.26    --  -86.25  57.00-180.00   47
 14  \w    -56.00 -16.00   1.00    0.26    --  -86.25  56.00 -50.00   40
 15  \w    -43.00 -15.00   1.00    0.26    --  -86.25  38.00 150.00   28
 16  \w    -70.00 -34.00   1.00    0.10    --  -48.45 -56.00 167.00   36
 17  \w   -102.00 -75.00   1.00    0.26    --  -86.25 -56.00 167.00   27
 18  \w   -120.00 -82.00   1.00    0.10    --  -48.45 -56.00 167.00   38
 19  \w   -119.00 -74.00   1.00    0.10    --  -48.45-125.00 -60.00   45
;
_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  0.0527
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            15188
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.046
_diffrn_reflns_theta_max         67.046
_diffrn_reflns_theta_min         3.399
_exptl_absorpt_coefficient_mu    7.981
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44551
_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            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       block
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         4177
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0618P)^2^+2.0066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1108
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3798
_reflns_number_total             4177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj06133j2.cif
_cod_data_source_block           201216d
_cod_depositor_comments
'Adding full bibliography for 7061389--7061390.cif.'
_cod_original_cell_volume        2367.33(9)
_cod_database_code               7061390
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.741
_shelx_estimated_absorpt_t_min   0.646
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F5-C18 \\sim F5A-C18A
 with sigma of 0.02
 C18-C5 \\sim C18A-C5A
 with sigma of 0.04
 F3-C3 \\sim F3A-C3A
 with sigma of 0.02
 F1-C5 \\sim F1A-C5A
 with sigma of 0.04
 Fe1-C1 \\sim Fe1-C1A
 with sigma of 0.02
 F1-C4 \\sim F1A-C4A
 with sigma of 0.02
 F4-C5 \\sim F4A-C5A
 with sigma of 0.02
 C4-C3 \\sim C4A-C3A
 with sigma of 0.02
 C4-C1 \\sim C4A-C1A
 with sigma of 0.04
 C1-N2 \\sim C1A-N2A
 with sigma of 0.04
 C1-C18 \\sim C1A-C18A
 with sigma of 0.02
 C1-C5 \\sim C1A-C5A
 with sigma of 0.02
 C5-C3 \\sim C5A-C3A
 with sigma of 0.04
 N2-C18 \\sim N2A-C18A
 with sigma of 0.02
 N2-C3 \\sim N2A-C3A
 with sigma of 0.02
 C4-C5 \\sim C4A-C5A
 with sigma of 0.02
 F1-C3 \\sim F1A-C3A
 with sigma of 0.04
 C4-N2 \\sim C4A-N2A
 with sigma of 0.04
 Fe1-C18 \\sim Fe1-C18A
 with sigma of 0.04
 Fe1-C5 \\sim Fe1-C5A
 with sigma of 0.04
 F4-C4 \\sim F4A-C4A
 with sigma of 0.04
 C18-C3 \\sim C18A-C3A
 with sigma of 0.04
 F4-C1 \\sim F4A-C1A
 with sigma of 0.04
 F5-C1 \\sim F5A-C1A
 with sigma of 0.04
 F5-N2 \\sim F5A-N2A
 with sigma of 0.04
 F3-C4 \\sim F3A-C4A
 with sigma of 0.04
 F3-N2 \\sim F3A-N2A
 with sigma of 0.04
3. Rigid bond restraints
 N2, C3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
F3A \\sim F4A \\sim C5A \\sim C4A \\sim C1A \\sim F1A \\sim C3A \\sim C18A
\\sim N2A \\sim F5A: within 2A with sigma of 0.001 and sigma for terminal atoms
of 0.002 within 2A
Uanis(N2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 N2, F4, C5, C4, C1, F1, C3, C18, F3, F5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(F4A)=Sof(F5A)=Sof(F3A)=Sof(F1A)=Sof(C4A)=Sof(C1A)=Sof(N2A)=Sof(C18A)=
 Sof(C5A)=Sof(C3A)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F3)=Sof(F1)=Sof(C4)=Sof(C1)=Sof(N2)=Sof(C18)=Sof(C5)=
 Sof(C3)=FVAR(1)
7.a Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C15(H15A,H15B,H15C), C8(H8A,H8B,H8C), C6(H6A,H6B,H6C),
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C17(H17A,H17B,H17C),
 C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C14(H14A,H14B,H14C), C13(H13A,H13B,
 H13C)
;
_shelx_res_checksum              76078
_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
;