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_4517620
_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         'C43 H37 Br2 F N2 Ni O'
_chemical_formula_sum            'C43 H37 Br2 F N2 Ni O'
_chemical_formula_weight         835.27
_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   mixed
_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                 92.195(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6936(4)
_cell_length_b                   18.8357(5)
_cell_length_c                   14.8346(7)
_cell_measurement_reflns_used    14134
_cell_measurement_temperature    170.01(10)
_cell_measurement_theta_max      28.3440
_cell_measurement_theta_min      3.5760
_cell_volume                     4381.9(3)
_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      170.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.898
_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     56.00  82.00   0.50   13.00    --    5.00  45.00   0.00   52
  2  \w   -101.00  71.00   0.50   13.00    --  -14.80  45.00 150.00  344
  3  \w   -104.00 -66.00   0.50   13.00    --  -14.80  45.00 120.00   76
  4  \w      4.00  54.00   0.50   13.00    --  -14.80  45.00 120.00  100
  5  \w    -32.00  73.00   0.50   13.00    --  -14.80  45.00   0.00  210
  6  \w    -81.00 -55.00   0.50   13.00    --  -14.80  45.00   0.00   52
;
_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      0.0044846000
_diffrn_orient_matrix_UB_12      0.0078979000
_diffrn_orient_matrix_UB_13      0.0467235000
_diffrn_orient_matrix_UB_21      -0.0142768000
_diffrn_orient_matrix_UB_22      0.0351573000
_diffrn_orient_matrix_UB_23      -0.0087209000
_diffrn_orient_matrix_UB_31      -0.0426524000
_diffrn_orient_matrix_UB_32      -0.0108926000
_diffrn_orient_matrix_UB_33      0.0059029000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46334
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.625
_diffrn_reflns_theta_min         3.495
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.301
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54379
_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    1.266
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.901
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         12143
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0579P)^2^+5.0062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1496
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7254
_reflns_number_total             12143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c01208_si_002.cif
_cod_data_source_block           Ni5
_cod_database_code               4517620
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H N Ni F Br'
_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, All O(H,H) groups
2.a Rotating group:
 O1(H1A,H1B)
2.b Ternary CH refined with riding coordinates:
 C29(H29), C14(H14)
2.c Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C21(H21A,H21B), C37(H37A,H37B), C36(H36A,H36B)
2.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C27(H27), C42(H42), C31(H31), C40(H40), C39(H39),
 C41(H41), C4(H4), C16(H16), C1(H1), C24(H24), C19(H19), C25(H25), C26(H26),
 C32(H32), C34(H34), C18(H18), C3(H3), C33(H33), C17(H17), C2(H2)
2.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              14744
_shelx_hkl_checksum              43999
_shelx_fab_checksum              75527
_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 3.933
_oxdiff_exptl_absorpt_empirical_full_min 0.403