Fluorinated cobalt catalysts and their use in forming narrowly dispersed polyethylene waxes of high linearity and incorporating vinyl functionality
Zhang, Qiuyue; Li, Zilong; Han, Mingyang; Xiang, Junfeng; Solan, Gregory A.; Ma, Yanping; Liang, Tongling; Sun, Wen-Hua; Catalysis Science & Technology 11 (2021) 656–670; doi:10.1039/D0CY01917H

data_1559567
_publ_section_title
;
 Fluorinated cobalt catalysts and their use in forming narrowly dispersed
 polyethylene waxes of high linearity and incorporating vinyl
 functionality
;
_journal_issue                   2
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              656
_journal_page_last               670
_journal_paper_doi               10.1039/D0CY01917H
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C49 H38 Cl2 Co F5 N3'
_chemical_formula_sum            'C49 H38 Cl2 Co F5 N3'
_chemical_formula_weight         893.65
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-02-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-08-18 deposited with the CCDC.	2020-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                97.115(3)
_cell_angle_beta                 92.063(4)
_cell_angle_gamma                98.641(4)
_cell_formula_units_Z            2
_cell_length_a                   11.8773(6)
_cell_length_b                   12.8721(5)
_cell_length_c                   14.5308(6)
_cell_measurement_reflns_used    7061
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      28.0380
_cell_measurement_theta_min      3.5260
_cell_volume                     2176.04(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.872
_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      5.00  32.00   0.50   12.00    --    5.00  45.00 120.00   54
  2  \w   -104.00 -46.00   0.50   12.00    --  -15.10  45.00  90.00  116
  3  \w   -103.00  -9.00   0.50   12.00    --  -15.10  45.00 150.00  188
  4  \w   -104.00  62.00   0.50   12.00    --  -15.10  45.00  30.00  332
  5  \w    -48.00 -21.00   0.50   12.00    --  -15.10  45.00 -19.23   54
  6  \w     18.00  64.00   0.50   12.00    --  -15.10  45.00 -19.23   92
  7  \w    -29.00  74.00   0.50   12.00    --  -15.10  45.00  90.00  206
  8  \w     -7.00  24.00   0.50   12.00    --  -15.10  45.00 150.00   62
  9  \w   -103.00 -49.00   0.50   12.00    --  -15.10  45.00 169.97  108
 10  \w     20.00  74.00   0.50   12.00    --  -15.10  45.00 179.70  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0162110000
_diffrn_orient_matrix_UB_12      -0.0389990000
_diffrn_orient_matrix_UB_13      0.0295054000
_diffrn_orient_matrix_UB_21      0.0560050000
_diffrn_orient_matrix_UB_22      0.0095314000
_diffrn_orient_matrix_UB_23      0.0211128000
_diffrn_orient_matrix_UB_31      -0.0161465000
_diffrn_orient_matrix_UB_32      0.0393556000
_diffrn_orient_matrix_UB_33      0.0333329000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_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            35166
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.862
_diffrn_reflns_theta_min         3.437
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45i (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       block
_exptl_crystal_F_000             918
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.251
_exptl_crystal_size_min          0.123
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         11961
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0557P)^2^+1.3076P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1438
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7274
_reflns_number_total             11961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cy01917h2.cif
_cod_data_source_block           Co1
_cod_depositor_comments
'Adding full bibliography for 1559567--1559568.cif.'
_cod_database_code               1559567
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_usercomment     'C H N Co Cl F'
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C37(H37), C24(H24)
2.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C20(H20), C5(H5), C6(H6), C4(H4), C36(H36), C45(H45), C35(H35),
 C43(H43), C32(H32), C42(H42), C46(H46), C30(H30), C39(H39), C49(H49), C14(H14),
  C13(H13), C26(H26), C12(H12), C29(H29), C48(H48), C40(H40), C33(H33), C27(H27)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              51727
_shelx_fab_checksum              54603
_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 1.258
_oxdiff_exptl_absorpt_empirical_full_min 0.856