Sterically and Electronically Modified Aryliminopyridyl-Nickel Bromide Precatalysts for an Access to Branched Polyethylene with Vinyl/Vinylene End Groups
Zada, Muhammad; Vignesh, Arumugam; Guo, Liwei; Zhang, Randi; Zhang, Wenjuan; Ma, Yanping; Sun, Yang; Sun, Wen-Hua; ACS Omega  (2020) –; doi:10.1021/acsomega.0c01208

data_4517619
_publ_section_title
;
 Sterically and Electronically Modified Aryliminopyridyl-Nickel Bromide
 Precatalysts for an Access to Branched Polyethylene with Vinyl/Vinylene
 End Groups
;
_journal_name_full               'ACS Omega'
_journal_paper_doi               10.1021/acsomega.0c01208
_journal_year                    2020
_chemical_formula_moiety         'C90 H80 Br N4 Ni, Br'
_chemical_formula_sum            'C90 H80 Br2 N4 Ni'
_chemical_formula_weight         1436.11
_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             2018-12-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.329(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4100(4)
_cell_length_b                   38.9819(12)
_cell_length_c                   18.2057(7)
_cell_measurement_reflns_used    13512
_cell_measurement_temperature    170.01(10)
_cell_measurement_theta_max      24.5030
_cell_measurement_theta_min      3.4080
_cell_volume                     8031.4(5)
_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_temperature      170.01(10)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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   -103.00  73.00   0.50   15.00    --  -14.80  45.00  60.00  352
  2  \w    -63.00 -12.00   0.50   15.00    --  -14.80  45.00   0.00  102
  3  \w    -31.00  21.00   0.50   15.00    --  -14.80  45.00 120.00  104
  4  \w     26.00  74.00   0.50   15.00    --  -14.80  45.00 120.00   96
  5  \w   -100.00 -25.00   0.50   15.00    --  -14.80  45.00  90.00  150
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0807
_diffrn_reflns_av_unetI/netI     0.0915
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            77553
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         3.416
_exptl_absorpt_coefficient_mu    1.282
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50595
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       plate
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.085
_refine_diff_density_max         1.312
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     878
_refine_ls_number_reflns         18415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1336
_refine_ls_R_factor_gt           0.0859
_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^)+(0.0662P)^2^+23.3529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1759
_refine_ls_wR_factor_ref         0.1933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12186
_reflns_number_total             18415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c01208_si_002.cif
_cod_data_source_block           Ni2
_cod_database_code               4517619
_shelx_shelxl_version_number     2016/6
_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), C31A(H31A), C16A(H16A), C31(H31)
2.b Secondary CH2 refined with riding coordinates:
 C39A(H39A,H39B), C14(H14A,H14B), C38A(H38A,H38B), C14A(H14C,H14D), C39(H39C,
 H39D), C23A(H23A,H23B), C24A(H24A,H24B), C24(H24C,H24D), C23(H23C,H23D),
 C38(H38C,H38D)
2.c Aromatic/amide H refined with riding coordinates:
 C12A(H12A), C1(H1), C33A(H33A), C12(H12), C18(H18), C10A(H10A), C4(H4),
 C2(H2), C10(H10), C18A(H18A), C21A(H21A), C36A(H36A), C34A(H34A), C4A(H4A),
 C1A(H1A), C43A(H43A), C3(H3), C29A(H29A), C21(H21), C41A(H41A), C42A(H42A),
 C19(H19), C44A(H44A), C35A(H35A), C29(H29), C20A(H20A), C33(H33), C19A(H19A),
 C27A(H27A), C26A(H26A), C44(H44), C20(H20), C2A(H2A), C3A(H3A), C28A(H28A),
 C26(H26), C28(H28), C41(H41), C36(H36), C27(H27), C35(H35), C34(H34), C43(H43),
  C42(H42)
2.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C7A(H7AA,H7AB,H7AC), C15A(H15A,H15B,H15C), C15(H15D,H15E,H15F)
;
_shelx_res_checksum              5862
_shelx_hkl_checksum              77442
_shelx_fab_checksum              91057
_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
;