Synthesis of Polyethylenes with Controlled Branching with α-Diimine Nickel Catalysts and Revisiting Formation of Long-Chain Branching
Pei, Lixia; Liu, Fengshou; Liao, Heng; Gao, Jie; Zhong, Liu; Gao, Haiyang; Wu, Qing; ACS Catalysis 8 (2018) 1104–; doi:10.1021/acscatal.7b03282

data_4514360
_publ_section_title
;
 Synthesis of Polyethylenes with Controlled Branching with \a-Diimine
 Nickel Catalysts and Revisiting Formation of Long-Chain Branching
;
_journal_issue                   2
_journal_name_full               'ACS Catalysis'
_journal_page_first              1104
_journal_paper_doi               10.1021/acscatal.7b03282
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C48 H36 Br2 N2 Ni, 4(C H2 Cl2)'
_chemical_formula_sum            'C52 H44 Br2 Cl8 N2 Ni'
_chemical_formula_weight         1199.02
_space_group_crystal_system      orthorhombic
_space_group_IT_number           45
_space_group_name_Hall           'I 2 -2c'
_space_group_name_H-M_alt        'I b a 2'
_symmetry_space_group_name_Hall  'I 2 -2c'
_symmetry_space_group_name_H-M   'I b a 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-10-15
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.752(6)
_cell_length_b                   10.970(3)
_cell_length_c                   22.093(5)
_cell_measurement_reflns_used    5144
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      24.97
_cell_measurement_theta_min      2.47
_cell_volume                     5999(3)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            13046
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         1.843
_exptl_absorpt_coefficient_mu    2.044
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.511050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0864 before and 0.0441 after correction.
The Ratio of minimum to maximum transmission is 0.5111.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.042(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         4181
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0471P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0890
_reflns_Friedel_coverage         0.945
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                3323
_reflns_number_total             4181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b03282_si_002.cif
_cod_data_source_block           1_sq
_cod_depositor_comments
'Adding full bibliography for 4514359--4514361.cif.'
_cod_original_cell_volume        5999(2)
_cod_database_code               4514360
_shelx_estimated_absorpt_t_max   0.619
_shelx_estimated_absorpt_t_min   0.440
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.958(17) 0.042(17)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B)
3.b Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C12(H12), C14(H14),
 C23(H23), C24(H24), C25(H25)
;
_shelx_res_checksum              43497
_shelx_hkl_checksum              8382
_shelx_fab_checksum              16625
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'