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_4514359
_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         'C92 H64 Br4 N4 Ni2, 2(C H2 Cl2)'
_chemical_formula_sum            'C94 H68 Br4 Cl4 N4 Ni2'
_chemical_formula_weight         1832.38
_chemical_name_systematic
;
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-07-03
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.06.29 svn.r3433 for OlexSys, GUI svn.r5356)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.981(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.4354(14)
_cell_length_b                   18.923(2)
_cell_length_c                   18.566(2)
_cell_measurement_reflns_used    6245
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.458
_cell_measurement_theta_min      2.152
_cell_volume                     3978.6(8)
_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)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.979
_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  0.0460
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23363
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.147
_diffrn_reflns_theta_min         2.096
_exptl_absorpt_coefficient_mu    2.667
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.721807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) was 0.0777 before and 0.0307 after correction. The Ratio of minimum to maximum transmission is 0.7218. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.658
_refine_diff_density_min         -1.010
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         8641
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0587P)^2^+9.3846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1371
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5593
_reflns_number_total             8641
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b03282_si_003.cif
_cod_data_source_block           01231m
_cod_depositor_comments
'Adding full bibliography for 4514359--4514361.cif.'
_cod_database_code               4514359
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid body (RIGU) restrains
 Cl1, Cl2, C47
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34),
 C35(H35), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45)
;
_shelx_res_checksum              74458
_shelx_hkl_checksum              15377
_olex2_submission_special_instructions 'No special instructions were received'