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_4514361
_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         'C38 H36 Br2 N2 Ni'
_chemical_formula_sum            'C38 H36 Br2 N2 Ni'
_chemical_formula_weight         739.22
_chemical_name_systematic
;
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-10-17
_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                 109.503(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.579(2)
_cell_length_b                   14.443(2)
_cell_length_c                   18.148(3)
_cell_measurement_reflns_used    5662
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.909
_cell_measurement_theta_min      2.162
_cell_volume                     3355.0(9)
_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      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0772
_diffrn_reflns_av_unetI/netI     0.1005
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16888
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        27.05
_diffrn_reflns_theta_max         27.05
_diffrn_reflns_theta_min         1.845
_exptl_absorpt_coefficient_mu    2.989
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.543276
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0999 before and 0.0636 after correction.
The Ratio of minimum to maximum transmission is 0.5433.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.152
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         7296
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.1393
_refine_ls_R_factor_gt           0.0966
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+45.3052P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2194
_refine_ls_wR_factor_ref         0.2339
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4662
_reflns_number_total             7296
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b03282_si_004.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4514359--4514361.cif.'
_cod_original_cell_volume        3355.2(9)
_cod_database_code               4514361
_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
2. Restrained distances
 H11A-H1C_$1
 2.2 with sigma of 0.02
 H11B-H7
 2.2 with sigma of 0.02
 C7-C8 \\sim C8-C7A
 with sigma of 0.02
 C5-C4 \\sim C4-C5A
 with sigma of 0.02
 C1-C3 \\sim C3-C1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C1, C1A, C3, C4, C5, C5A, C6, C6A, C7, C7A, C8, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=1-FVAR(1)
 Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(H3B)=1-FVAR(2)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(H3A)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C3(H3A), C3(H3B), C10(H10)
6.b Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C5A(H5A), C6(H6), C6A(H6A), C7(H7), C7A(H7A), C15(H15), C16(H16),
 C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
  C28(H28), C29(H29), C30(H30), C31(H31), C34(H34), C35(H35), C36(H36),
 C37(H37), C38(H38)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              81285
_shelx_hkl_checksum              33416
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'