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_4518531
_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         'C53 H50 Cl2 Co F N3, C H2 Cl2'
_chemical_formula_sum            'C54 H52 Cl4 Co F N3'
_chemical_formula_weight         962.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.065(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1335(3)
_cell_length_b                   29.5446(6)
_cell_length_c                   16.6587(4)
_cell_measurement_reflns_used    16636
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      30.4490
_cell_measurement_theta_min      3.6490
_cell_volume                     4792.7(2)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.8797
_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    -82.00  47.00   0.50   15.00    --  -15.00  45.00 150.00  258
  2  \w    -64.00 -33.00   0.50   15.00    --  -15.00  45.00  90.00   62
  3  \w     -7.00  19.00   0.50   15.00    --  -15.00  45.00  90.00   52
  4  \w   -104.00  56.00   0.50   15.00    --  -15.00  45.00 120.00  320
;
_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      0.0447794000
_diffrn_orient_matrix_UB_12      0.0035721000
_diffrn_orient_matrix_UB_13      0.0405596000
_diffrn_orient_matrix_UB_21      0.0498687000
_diffrn_orient_matrix_UB_22      -0.0141282000
_diffrn_orient_matrix_UB_23      -0.0099623000
_diffrn_orient_matrix_UB_31      0.0286472000
_diffrn_orient_matrix_UB_32      0.0190682000
_diffrn_orient_matrix_UB_33      -0.0147846000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43296
_diffrn_reflns_theta_full        30.8046
_diffrn_reflns_theta_max         30.80
_diffrn_reflns_theta_min         3.46
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67872
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.3342
_exptl_crystal_description       block
_exptl_crystal_F_000             2008.4303
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.218
_exptl_crystal_size_min          0.145
_refine_diff_density_max         0.9547
_refine_diff_density_min         -0.9403
_refine_diff_density_rms         0.0696
_refine_ls_d_res_high            0.6939
_refine_ls_d_res_low             5.8848
_refine_ls_goodness_of_fit_ref   1.0217
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    91
_refine_ls_number_parameters     574
_refine_ls_number_reflns         13219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0217
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+2.4644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1054
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -13
_reflns_limit_k_max              42
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              -9
_reflns_number_gt                10693
_reflns_number_total             13219
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ao0c05916_si_002.cif
_cod_data_source_block           Co3
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               4518531
_chemical_oxdiff_formula         'C H N Co Cl F'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.82
_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), C51(H51), C48(H48)
2.b Secondary CH2 refined with riding coordinates:
 C54(H54a,H54b)
2.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C22(H22), C35(H35), C31(H31), C24(H24), C6(H6), C37(H37),
 C46(H46), C21(H21), C41(H41), C44(H44), C4(H4), C34(H34), C28(H28), C5(H5),
 C18(H18), C32(H32), C45(H45), C27(H27), C20(H20), C39(H39), C40(H40), C38(H38),
  C33(H33), C25(H25), C19(H19), C26(H26)
2.d Idealised Me refined as rotating group:
 C9(H9a,H9b,H9c), C1(H1a,H1b,H1c), C49(H49a,H49b,H49c), C50(H50a,H50b,H50c),
 C52(H52a,H52b,H52c), C53(H53a,H53b,H53c)
;
_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 1.501
_oxdiff_exptl_absorpt_empirical_full_min 0.567