Ligand steric effects on α-diimine nickel catalyzed ethylene and 1-hexene polymerization
Sun, Jinlong; Wang, Fuzhou; Li, Weimin; Chen, Min; RSC Advances 7 (2017) 55051–; doi:10.1039/C7RA11783C

data_7229654
_publ_section_title
;
 Ligand steric effects on \a-diimine nickel catalyzed ethylene and
 1-hexene polymerization
;
_journal_issue                   87
_journal_name_full               'RSC Advances'
_journal_page_first              55051
_journal_paper_doi               10.1039/C7RA11783C
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         '2(C25 H26 Br N Ni0.5)'
_chemical_formula_sum            'C50 H52 Br2 N2 Ni'
_chemical_formula_weight         899.47
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2ya'
_space_group_name_H-M_alt        'P 1 2/a 1'
_symmetry_space_group_name_Hall  '-P 2ya'
_symmetry_space_group_name_H-M   'P 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-04-26
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_audit_update_record
;
2016-03-14 deposited with the CCDC.
2017-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 114.281(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.4157(8)
_cell_length_b                   8.5771(3)
_cell_length_c                   24.0509(8)
_cell_measurement_reflns_used    4526
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.6660
_cell_measurement_theta_min      3.6980
_cell_volume                     4215.0(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.9452
_diffrn_measured_fraction_theta_max 0.9329
_diffrn_measurement_details
;
  1 omega  -22.00   14.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   60.0000 36

  2 omega  -79.00  -36.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000 -150.0000 43

  3 omega  -82.00  -45.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000 -180.0000 37

  4 omega   16.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   60.0000 54

  5 omega -128.00  -82.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -58.0000  -99.0000 -180.0000 46

  6 omega -108.00  -81.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -58.0000  -99.0000  -90.0000 27

  7 omega  -93.00  -11.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -58.0000  125.0000    0.0000 82

  8 omega  -40.00   14.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -58.0000   38.0000  -60.0000 54

  9 omega -130.00  -79.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  178.0000 -180.0000 51

 10 omega  -32.00    5.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000   50.0000 -180.0000 37

 11 omega  -46.00   -7.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000   38.0000   60.0000 39

 12 omega   45.00   75.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      116.0000  -25.0000  150.0000 30

 13 omega   76.00  116.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      116.0000 -113.0000   64.0000 40

 14 omega   74.00  100.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      116.0000 -111.0000  -60.0000 26

 15 omega   50.00  104.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      116.0000  -50.0000  120.0000 54

 16 omega  100.00  175.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      116.0000  111.0000 -150.0000 75

 17 omega   50.00  103.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      116.0000  -50.0000   60.0000 53

 18 omega  116.00  145.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      116.0000  178.0000  -90.0000 29

 19 omega  111.00  172.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      116.0000   63.0000   30.0000 61

 20 omega   57.00   83.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      116.0000  178.0000  -90.0000 26

 21 omega   44.00  116.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      116.0000 -111.0000  -90.0000 72

 22 omega   44.00   74.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      116.0000  -38.0000  -30.0000 30

 23 omega   42.00   67.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      116.0000  -25.0000  -90.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0104061000
_diffrn_orient_matrix_UB_12      0.1680419000
_diffrn_orient_matrix_UB_13      -0.0247362000
_diffrn_orient_matrix_UB_21      -0.0428925000
_diffrn_orient_matrix_UB_22      -0.0616225000
_diffrn_orient_matrix_UB_23      -0.0643087000
_diffrn_orient_matrix_UB_31      -0.0611464000
_diffrn_orient_matrix_UB_32      0.0145730000
_diffrn_orient_matrix_UB_33      0.0137287000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            14743
_diffrn_reflns_theta_full        72.61
_diffrn_reflns_theta_max         72.61
_diffrn_reflns_theta_min         3.95
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.154
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.244
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.260
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7775
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.260
_refine_ls_R_factor_all          0.1146
_refine_ls_R_factor_gt           0.0823
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+19.0153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1875
_refine_ls_wR_factor_ref         0.2022
_reflns_number_gt                4193
_reflns_number_total             7775
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ra11783c2.cif
_cod_data_source_block           wangfzh03_0421
_cod_original_cell_volume        4215.0(2)
_cod_database_code               7229654
_reflns_odcompleteness_completeness 94.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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:
 C7(H7), C15(H15), C31(H31), C40(H40)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C1A(H1A), C2(H2), C3(H3), C5(H5), C10(H10), C12(H12), C18(H18),
 C19(H19), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27), C28(H28),
  C29(H29), C34(H34), C36(H36), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C24(H24A,H24B,
 H24C), C32(H32A,H32B,H32C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C49(H49A,
 H49B,H49C)
;