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_7246022
_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         'C51 H45 Cl2 Co F2 N3, C H2 Cl2'
_chemical_formula_sum            'C52 H47 Cl4 Co F2 N3'
_chemical_formula_weight         952.65
_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
_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                 125.0950(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.8272(3)
_cell_length_b                   14.5493(2)
_cell_length_c                   16.0514(2)
_cell_measurement_reflns_used    12151
_cell_measurement_temperature    170.00(11)
_cell_measurement_theta_max      74.5360
_cell_measurement_theta_min      3.7570
_cell_volume                     4552.89(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      170.00(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.965
_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    -48.00  24.00   0.50    0.06    --  -47.20  46.00-125.00  144
  2  \w    -77.00 -52.00   0.50    0.06    --  -47.20 -46.00  85.00   50
  3  \w     56.00 102.00   0.50    0.06    --   47.20  46.00-125.00   92
  4  \w    -18.00  48.00   0.50    0.06    --   47.20 -46.00  85.00  132
  5  \w   -127.00-102.00   0.50    0.26    --  -99.00 -46.00  85.00   50
  6  \w     91.00 168.00   0.50    0.26    --  103.25  46.00-125.00  154
  7  \w    -22.00  26.00   0.50    0.06    --  -47.20  19.00 -30.00   96
  8  \w   -120.00 -75.00   0.50    0.06    --  -47.20-125.00-180.00   90
  9  \w    -20.00   6.00   0.50    0.06    --   47.20 -19.00 -90.00   52
 10  \w    -62.00 -29.00   0.50    0.26    --  -99.00  61.00 -90.00   66
 11  \w    -60.00 -26.00   0.50    0.26    --  -99.00  61.00  90.00   68
 12  \w    -88.00 -31.00   0.50    0.26    --  -99.00  77.00-180.00  114
 13  \w    -64.00 -26.00   0.50    0.26    --  -99.00  61.00  60.00   76
 14  \w    -67.00 -32.00   0.50    0.26    --  -99.00  61.00 150.00   70
 15  \w     44.00  75.00   0.50    0.26    --  103.25 -61.00 -60.00   62
 16  \w     34.00  60.00   0.50    0.26    --  103.25 -77.00 -60.00   52
 17  \w     38.00 100.00   0.50    0.26    --  103.25 -94.00-150.00  124
 18  \w     80.00 106.00   0.50    0.26    --  103.25 -77.00 -60.00   52
 19  \w     91.00 133.00   0.50    0.26    --  103.25  15.00 150.00   84
 20  \w    142.00 167.00   0.50    0.26    --  103.25  15.00 150.00   50
 21  \w     43.00  72.00   0.50    0.26    --  103.25 -61.00 -30.00   58
 22  \w     99.00 130.00   0.50    0.26    --  103.25  45.00-180.00   62
 23  \w     46.00 109.00   0.50    0.26    --  103.25 -77.00  30.00  126
 24  \w     84.00 109.00   0.50    0.26    --  103.25 -77.00-180.00   50
 25  \w     44.00  70.00   0.50    0.26    --  103.25 -77.00-180.00   52
 26  \w     92.00 168.00   0.50    0.26    --  103.25  30.00 -30.00  152
;
_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      0.0517765000
_diffrn_orient_matrix_UB_12      0.0565546000
_diffrn_orient_matrix_UB_13      0.0589355000
_diffrn_orient_matrix_UB_21      0.0561822000
_diffrn_orient_matrix_UB_22      -0.0207244000
_diffrn_orient_matrix_UB_23      -0.0566118000
_diffrn_orient_matrix_UB_31      -0.0202447000
_diffrn_orient_matrix_UB_32      0.0870700000
_diffrn_orient_matrix_UB_33      -0.0516328000
_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  0.0351
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16783
_diffrn_reflns_point_group_measured_fraction_full 0.851
_diffrn_reflns_point_group_measured_fraction_max 0.800
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.288
_diffrn_reflns_theta_min         3.791
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.498
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67003
_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    1.390
_exptl_crystal_description       block
_exptl_crystal_F_000             1972
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.658
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Flack x determined using 2687 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.017(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         7537
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0988P)^2^+6.0571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1403
_refine_ls_wR_factor_ref         0.1416
_reflns_Friedel_coverage         0.657
_reflns_Friedel_fraction_full    0.703
_reflns_Friedel_fraction_max     0.635
_reflns_number_gt                7275
_reflns_number_total             7537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra05806e2.cif
_cod_data_source_block           Co2
_cod_depositor_comments
'Adding full bibliography for 7246022--7246023.cif.'
_cod_original_cell_volume        4552.89(11)
_cod_database_code               7246022
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N F Co Cl'
_shelx_estimated_absorpt_t_max   0.771
_shelx_estimated_absorpt_t_min   0.493
_reflns_odcompleteness_completeness 99.93
_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:
 C16(H16), C29(H29)
2.b Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C50(H50A,H50B), C01P(H01A,H01B)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C4(H4), C24(H24), C6(H6), C31(H31), C5(H5), C35(H35), C32(H32),
 C27(H27), C28(H28), C18(H18), C25(H25), C21(H21), C20(H20), C46(H46), C22(H22),
  C44(H44), C26(H26), C33(H33), C19(H19), C45(H45), C34(H34), C37(H37),
 C41(H41), C38(H38), C40(H40), C39(H39)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              39636
_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 1.716
_oxdiff_exptl_absorpt_empirical_full_min 0.729