Exploring fluoride effects in sterically enhanced cobalt ethylene polymerisation catalysts; a combined experimental and DFT study.
Li, Zilong; Ma, Yanping; Liu, Tian; Zhang, Qiuyue; Solan, Gregory A.; Liang, Tongling; Sun, Wen-Hua; RSC advances 13 (2022) 14–24; doi:10.1039/d2ra05806e

data_7246023
_publ_section_title
;
 Exploring fluoride effects in sterically enhanced cobalt ethylene
 polymerisation catalysts; a combined experimental and DFT study.
;
_journal_issue                   1
_journal_name_full               'RSC advances'
_journal_page_first              14
_journal_page_last               24
_journal_paper_doi               10.1039/d2ra05806e
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C52 H47 Cl2 Co F2 N3, C H2 Cl2'
_chemical_formula_sum            'C53 H49 Cl4 Co F2 N3'
_chemical_formula_weight         966.68
_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             2021-07-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-08-16 deposited with the CCDC.	2022-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 127.0490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.2166(3)
_cell_length_b                   14.6821(2)
_cell_length_c                   16.4823(2)
_cell_measurement_reflns_used    12900
_cell_measurement_temperature    169.97(11)
_cell_measurement_theta_max      75.2990
_cell_measurement_theta_min      3.7320
_cell_volume                     4677.22(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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      169.97(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.952
_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    -81.00  -4.00   0.50    0.13    --  -47.20 113.00-163.00  154
  2  \w     50.00  75.00   0.50    0.13    --   47.20-113.00 105.00   50
  3  \w   -117.00 -91.00   0.50    0.52    --  -99.00-113.00 105.00   52
  4  \w   -106.00 -26.00   0.50    0.52    --  -99.00 113.00-163.00  160
  5  \w     73.00 106.00   0.50    0.52    --  103.25-113.00 105.00   66
  6  \w     87.00 165.00   0.50    0.52    --  103.25 113.00-163.00  156
  7  \w   -108.00 -74.00   0.50    0.13    --  -47.20-125.00-180.00   68
  8  \w   -120.00 -75.00   0.50    0.13    --  -47.20-125.00 -90.00   90
  9  \w    -40.00  26.00   0.50    0.13    --  -47.20  38.00  90.00  132
 10  \w   -108.00 -79.00   0.50    0.13    --  -47.20-125.00   0.00   58
 11  \w    -10.00  30.00   0.50    0.13    --   47.20 -19.00 -30.00   80
 12  \w    -59.00 -27.00   0.50    0.52    --  -99.00  61.00  60.00   64
 13  \w    -58.00 -27.00   0.50    0.52    --  -99.00  77.00-150.00   62
 14  \w    -65.00 -26.00   0.50    0.52    --  -99.00  61.00  30.00   78
 15  \w   -167.00-142.00   0.50    0.52    --  -99.00 -45.00 -60.00   50
 16  \w   -135.00 -90.00   0.50    0.52    --  -99.00 -45.00 -60.00   90
 17  \w    -56.00 -30.00   0.50    0.52    --  -99.00  61.00   0.00   52
 18  \w    -99.00 -72.00   0.50    0.52    --  -99.00  77.00-150.00   54
 19  \w    -68.00 -42.00   0.50    0.52    --  -99.00  61.00-150.00   52
 20  \w     96.00 122.00   0.50    0.52    --  103.25  45.00   0.00   52
 21  \w     39.00  75.00   0.50    0.52    --  103.25 -61.00 150.00   72
 22  \w     33.00 104.00   0.50    0.52    --  103.25 -94.00 120.00  142
 23  \w    133.00 163.00   0.50    0.52    --  103.25  30.00-180.00   60
 24  \w     44.00  73.00   0.50    0.52    --  103.25 -61.00  90.00   58
 25  \w    138.00 169.00   0.50    0.52    --  103.25  45.00   0.00   62
 26  \w     91.00 128.00   0.50    0.52    --  103.25  30.00-180.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0431407000
_diffrn_orient_matrix_UB_12      -0.0901115000
_diffrn_orient_matrix_UB_13      -0.0215479000
_diffrn_orient_matrix_UB_21      -0.0529616000
_diffrn_orient_matrix_UB_22      0.0503137000
_diffrn_orient_matrix_UB_23      -0.0577594000
_diffrn_orient_matrix_UB_31      0.0644495000
_diffrn_orient_matrix_UB_32      -0.0190124000
_diffrn_orient_matrix_UB_33      -0.0505141000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16345
_diffrn_reflns_point_group_measured_fraction_full 0.651
_diffrn_reflns_point_group_measured_fraction_max 0.617
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.357
_diffrn_reflns_theta_min         3.781
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.360
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       block
_exptl_crystal_F_000             2004
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.376
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.008(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         5983
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0772P)^2^+2.6124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.295
_reflns_Friedel_fraction_full    0.306
_reflns_Friedel_fraction_max     0.281
_reflns_number_gt                5816
_reflns_number_total             5983
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra05806e2.cif
_cod_data_source_block           Co5
_cod_depositor_comments
'Adding full bibliography for 7246022--7246023.cif.'
_cod_original_cell_volume        4677.22(11)
_cod_database_code               7246023
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N F Co Cl'
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Ternary CH refined with riding coordinates:
 C29(H29), C16(H16)
2.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C48(H48A,H48B), C01R(H01A,H01B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C14(H14), C5(H5), C24(H24), C46(H46), C28(H28), C18(H18), C25(H25),
 C21(H21), C20(H20), C22(H22), C31(H31), C27(H27), C44(H44), C19(H19), C6(H6),
 C35(H35), C26(H26), C32(H32), C33(H33), C37(H37), C41(H41), C34(H34), C40(H40),
  C38(H38), C39(H39)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C52(H52A,H52B,H52C), C50(H50A,H50B,H50C),
 C49(H49A,H49B,H49C)
;
_shelx_res_checksum              4586
_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 1.440
_oxdiff_exptl_absorpt_empirical_full_min 0.747