Enhancing Ethylene Polymerization of <i>NNN</i>-Cobalt(II) Precatalysts Adorned with a Fluoro-substituent.
Bariashir, Chantsalnyam; Zhang, Randi; Vignesh, Arumugam; Ma, Yanping; Liang, Tongling; Sun, Wen-Hua; ACS omega 6 (2021) 4448–4460; doi:10.1021/acsomega.0c05916

data_4518532
_publ_section_title
;
 Enhancing Ethylene Polymerization of <i>NNN</i>-Cobalt(II) Precatalysts
 Adorned with a Fluoro-substituent.
;
_journal_issue                   6
_journal_name_full               'ACS omega'
_journal_page_first              4448
_journal_page_last               4460
_journal_paper_doi               10.1021/acsomega.0c05916
_journal_volume                  6
_journal_year                    2021
_chemical_formula_moiety         'C50 H44 Cl2 Co F N3'
_chemical_formula_sum            'C50 H44 Cl2 Co F N3'
_chemical_formula_weight         835.71
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-12-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.466(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.7565(16)
_cell_length_b                   14.1649(9)
_cell_length_c                   16.2888(10)
_cell_measurement_reflns_used    5739
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      28.8220
_cell_measurement_theta_min      3.8950
_cell_volume                     4671.7(6)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.835
_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    -10.00  16.22   0.38   15.00    --  -14.80  45.00   0.00   69
  2  \w     45.00  71.22   0.38   15.00    --  -14.80  45.00   0.00   69
  3  \w   -104.00  57.12   0.38   15.00    --  -14.80  45.00 120.00  424
;
_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      -0.0266686000
_diffrn_orient_matrix_UB_12      0.0176485000
_diffrn_orient_matrix_UB_13      -0.0368192000
_diffrn_orient_matrix_UB_21      -0.0221160000
_diffrn_orient_matrix_UB_22      -0.0295305000
_diffrn_orient_matrix_UB_23      0.0110786000
_diffrn_orient_matrix_UB_31      -0.0052202000
_diffrn_orient_matrix_UB_32      0.0364133000
_diffrn_orient_matrix_UB_33      0.0265821000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0986
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.835
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25518
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.835
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.758
_diffrn_reflns_theta_min         3.476
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18159
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       block
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         12183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0846P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1525
_refine_ls_wR_factor_ref         0.1724
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7097
_reflns_number_total             12183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c05916_si_002.cif
_cod_data_source_block           Co4
_cod_database_code               4518532
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_usercomment     'C H N Ni Br'
_reflns_odcompleteness_completeness 97.99
_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:
 C16(H16), C29(H29)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C12(H12), C4(H4), C6(H6), C5(H5), C18(H18), C28(H28), C24(H24),
 C22(H22), C46(H46), C44(H44), C41(H41), C26(H26), C21(H21), C27(H27), C25(H25),
  C31(H31), C20(H20), C19(H19), C37(H37), C35(H35), C40(H40), C39(H39),
 C38(H38), C33(H33), C32(H32), C34(H34)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C1(H1A,H1B,H1C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C),
 C50(H50A,H50B,H50C)
;
_shelx_res_checksum              34926
_shelx_hkl_checksum              7585
_shelx_fab_checksum              3408
_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 2.562
_oxdiff_exptl_absorpt_empirical_full_min 0.448