High-performance polyethylene elastomers using a hybrid steric approach in α-diimine nickel precatalysts
Saeed, Hassan; Mahmood, Qaiser; Yuan, Rongyan; Wang, Yizhou; Zou, Song; Tahir, Kainat Fatima; Ma, Yanping; Liang, Tongling; Sun, Wen-Hua; Polymer Chemistry 15 (2024) 1437–1452; doi:10.1039/D4PY00061G

data_1571185
_publ_section_title
;
 High-performance polyethylene elastomers using a hybrid steric approach
 in \a-diimine nickel precatalysts
;
_journal_issue                   14
_journal_name_full               'Polymer Chemistry'
_journal_page_first              1437
_journal_page_last               1452
_journal_paper_doi               10.1039/D4PY00061G
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C100 H100 Br2 N2 Ni'
_chemical_formula_sum            'C100 H100 Br2 N2 Ni'
_chemical_formula_weight         1548.34
_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             2024-01-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-01-18 deposited with the CCDC.	2024-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.380(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.8212(18)
_cell_length_b                   10.4943(4)
_cell_length_c                   30.215(2)
_cell_measurement_reflns_used    12735
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      22.8650
_cell_measurement_theta_min      1.5240
_cell_volume                     8040.4(10)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.859
_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   -100.00  76.70   0.38   12.90    --  -10.70  45.00  90.00  465
  2  \w   -100.00  77.08   0.38   12.90    --  -10.70  45.00   0.00  466
;
_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      0.0176858000
_diffrn_orient_matrix_UB_12      0.0497467000
_diffrn_orient_matrix_UB_13      0.0136502000
_diffrn_orient_matrix_UB_21      -0.0047783000
_diffrn_orient_matrix_UB_22      -0.0114137000
_diffrn_orient_matrix_UB_23      0.0206412000
_diffrn_orient_matrix_UB_31      0.0211884000
_diffrn_orient_matrix_UB_32      -0.0441972000
_diffrn_orient_matrix_UB_33      0.0100382000
_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  0.1511
_diffrn_reflns_av_unetI/netI     0.1744
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.859
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            81936
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.028
_diffrn_reflns_theta_min         1.532
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.285
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.687
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       block
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.204
_refine_diff_density_min         -1.321
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1001
_refine_ls_number_reflns         22073
_refine_ls_number_restraints     234
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.2209
_refine_ls_R_factor_gt           0.1353
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+44.6599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2532
_refine_ls_wR_factor_ref         0.2861
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12572
_reflns_number_total             25703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4py00061g2.cif
_cod_data_source_block           mx11312c
_cod_depositor_comments
'Adding full bibliography for 1571184--1571186.cif.'
_cod_original_cell_volume        8040.6(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1571185
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNNiBr
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C95-C106 = C106-C105 = C105-C104 = C97-C104 = C97-C96 = C96-C95
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C39 \\sim C35 \\sim C94 \\sim C38 \\sim C48 \\sim C19 \\sim C106 \\sim C105
\\sim C96 \\sim C95 \\sim C104 \\sim C97: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 1.7A
Uanis(C39) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C106) \\sim Ueq,
Uanis(C105) \\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C104)
\\sim Ueq, Uanis(C97) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Others
 Sof(H93A)=Sof(C106)=Sof(H106)=Sof(C105)=Sof(H105)=Sof(C96)=Sof(H96)=Sof(C95)=
 Sof(C104)=Sof(H104)=Sof(C97)=Sof(H97)=1-FVAR(1)
 Sof(H93)=Sof(C39)=Sof(C35)=Sof(H35)=Sof(C94)=Sof(H94)=Sof(C38)=Sof(H38)=
 Sof(C48)=Sof(H48)=Sof(C19)=Sof(H19)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C22(H22), C81(H81), C93(H93), C93(H93A), C54(H54), C68(H68), C55(H55)
5.b Secondary CH2 refined with riding coordinates:
 C82(H82A,H82B), C84(H84A,H84B), C5(H5A,H5B), C92(H92A,H92B), C6(H6A,H6B),
 C85(H85A,H85B), C83(H83A,H83B), C15(H15A,H15B), C14(H14A,H14B), C86(H86A,H86B),
  C13(H13A,H13B), C87(H87A,H87B), C11(H11A,H11B), C7(H7A,H7B), C91(H91A,H91B),
 C8(H8A,H8B), C9(H9A,H9B), C12(H12A,H12B), C10(H10A,H10B), C88(H88A,H88B),
 C90(H90A,H90B), C89(H89A,H89B)
5.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C21(H21), C47(H47), C52(H52), C28(H28), C41(H41), C50(H50),
 C103(H103), C61(H61), C24(H24), C63(H63), C42(H42), C60(H60), C67(H67),
 C45(H45), C43(H43), C27(H27), C34(H34), C70(H70), C66(H66), C99(H99), C57(H57),
  C46(H46), C74(H74), C26(H26), C25(H25), C73(H73), C64(H64), C102(H102),
 C58(H58), C65(H65), C71(H71), C59(H59), C72(H72), C100(H100), C80(H80),
 C101(H101), C76(H76), C30(H30), C33(H33), C78(H78), C79(H79), C77(H77),
 C31(H31), C32(H32), C35(H35), C94(H94), C38(H38), C48(H48), C19(H19),
 C106(H106), C105(H105), C96(H96), C104(H104), C97(H97)
;
_shelx_res_checksum              51107
_shelx_hkl_checksum              97201
_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 5.194
_oxdiff_exptl_absorpt_empirical_full_min 0.420