High molecular weight PE elastomers through 4,4-difluorobenzhydryl substitution in symmetrical α-diimino-nickel ethylene polymerization catalysts
Zheng, Yuting; Jiang, Shu; Liu, Ming; Yu, Zhixin; Ma, Yanping; Solan, Gregory A.; Zhang, Wenjuan; Liang, Tongling; Sun, Wen-Hua; RSC Advances 12 (2022) 24037–24049; doi:10.1039/D2RA04321A

data_7245419
_publ_section_title
;
 High molecular weight PE elastomers through 4,4-difluorobenzhydryl
 substitution in symmetrical \a-diimino-nickel ethylene polymerization
 catalysts
;
_journal_issue                   37
_journal_name_full               'RSC Advances'
_journal_page_first              24037
_journal_page_last               24049
_journal_paper_doi               10.1039/D2RA04321A
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C74 H60 Br2 F8 N2 Ni'
_chemical_formula_sum            'C74 H60 Br2 F8 N2 Ni'
_chemical_formula_weight         1347.77
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-12-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-03-24 deposited with the CCDC.	2022-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.635(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8443(4)
_cell_length_b                   36.4718(12)
_cell_length_c                   16.3540(7)
_cell_measurement_reflns_used    9090
_cell_measurement_temperature    169.99(12)
_cell_measurement_theta_max      74.4830
_cell_measurement_theta_min      4.5610
_cell_volume                     6197.5(4)
_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      169.99(12)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.947
_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    -22.00  28.00   0.50    0.60    --  -46.95  19.00 -60.00  100
  2  \w     -4.00  22.00   0.50    0.60    --  -46.95  85.00  48.00   52
  3  \w    -56.00 -27.00   0.50    8.00    --  -99.00  61.00 -90.00   58
  4  \w    -63.00 -38.00   0.50    8.00    --  -99.00  61.00-120.00   50
  5  \w    -68.00 -43.00   0.50    8.00    --  -99.00  61.00-150.00   50
  6  \w    -22.00  28.00   0.50    0.60    --  -46.95  19.00-180.00  100
  7  \w    -13.00  14.00   0.50    0.60    --   46.95 -85.00 -69.00   54
  8  \w     24.00  62.00   0.50    0.60    --   46.95 -85.00 -69.00   76
  9  \w     32.00 101.00   0.50    8.00    --  103.25-125.00 -90.00  138
 10  \w     32.00  62.00   0.50    8.00    --  103.25 -61.00-120.00   60
 11  \w     32.00 129.00   0.50    8.00    --  103.25 -85.00 -69.00  194
 12  \w     91.00 167.00   0.50    8.00    --  103.25  30.00   0.00  152
 13  \w    128.00 156.00   0.50    8.00    --  103.25  61.00 -30.00   56
 14  \w    103.00 128.00   0.50    8.00    --  103.25  85.00  48.00   50
 15  \w     96.00 123.00   0.50    8.00    --  103.25  61.00 -30.00   54
 16  \w     34.00  72.00   0.50    8.00    --  103.25 -61.00 120.00   76
 17  \w     32.00  70.00   0.50    8.00    --  103.25 -94.00  60.00   76
 18  \w    -26.00  29.00   0.50    0.60    --   46.95 -19.00   0.00  110
 19  \w    -72.00 -14.00   0.50    0.60    --  -46.95  85.00  48.00  116
 20  \w    -59.00 -34.00   0.50    8.00    --  -99.00  61.00 -30.00   50
 21  \w    -68.00 -30.00   0.50    8.00    --  -99.00  61.00  30.00   76
 22  \w    -65.00 -31.00   0.50    8.00    --  -99.00  61.00 150.00   68
 23  \w   -104.00 -77.00   0.50    8.00    --  -99.00  85.00  48.00   54
 24  \w   -112.00 -26.00   0.50    8.00    --  -99.00 125.00  60.00  172
 25  \w   -168.00-126.00   0.50    8.00    --  -99.00 -45.00   0.00   84
 26  \w   -156.00 -85.00   0.50    8.00    --  -99.00 -85.00 -69.00  142
 27  \w   -117.00 -91.00   0.50    0.60    --  -46.95-125.00  60.00   52
 28  \w   -118.00 -75.00   0.50    0.60    --  -46.95-125.00  90.00   86
;
_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      0.0363729000
_diffrn_orient_matrix_UB_12      -0.0368635000
_diffrn_orient_matrix_UB_13      -0.0326893000
_diffrn_orient_matrix_UB_21      -0.0996737000
_diffrn_orient_matrix_UB_22      0.0067555000
_diffrn_orient_matrix_UB_23      -0.0870661000
_diffrn_orient_matrix_UB_31      0.1035612000
_diffrn_orient_matrix_UB_32      0.0194590000
_diffrn_orient_matrix_UB_33      -0.0319880000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1023
_diffrn_reflns_av_unetI/netI     0.0706
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46177
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.662
_diffrn_reflns_theta_min         2.423
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.542
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54450
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       block
_exptl_crystal_F_000             2752
_refine_diff_density_max         3.391
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         12209
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1634
_refine_ls_R_factor_gt           0.1343
_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^)+(0.1987P)^2^+104.6350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3939
_refine_ls_wR_factor_ref         0.4189
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8462
_reflns_number_total             12209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra04321a2.cif
_cod_data_source_block           Ni1
_cod_database_code               7245419
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     'C H N O Ni Br F'
_reflns_odcompleteness_completeness 99.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C27(H27), C47(H47), C12(H12), C62(H62), C7(H7), C42(H42)
2.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C64(H64), C25(H25), C45(H45), C10(H10), C60(H60), C52(H52),
 C39(H39), C33(H33), C53(H53), C36(H36), C35(H35), C59(H59), C30(H30), C65(H65),
  C49(H49), C68(H68), C50(H50), C24(H24), C38(H38), C74(H74), C18(H18),
 C71(H71), C55(H55), C58(H58), C32(H32), C20(H20), C14(H14), C70(H70), C67(H67),
  C23(H23), C17(H17), C15(H15), C56(H56), C21(H21), C73(H73)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C44(H44A,H44B,H44C), C8(H8A,H8B,H8C),
 C43(H43A,H43B,H43C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              80625
_shelx_fab_checksum              74921
_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 1.794
_oxdiff_exptl_absorpt_empirical_full_min 0.479