Bulky yet flexible substituents in insertion polymerization with α-diimine nickel and palladium systems
Guo, Lihua; Sun, Wenting; Li, Shuaikang; Xu, Guoyong; Dai, Shengyu; Polymer Chemistry 10 (2019) 4866–; doi:10.1039/C9PY00857H

data_1552149
_publ_section_title
;
 Bulky yet flexible substituents in insertion polymerization with
 \a-diimine nickel and palladium systems
;
_journal_issue                   35
_journal_name_full               'Polymer Chemistry'
_journal_page_first              4866
_journal_paper_doi               10.1039/C9PY00857H
_journal_volume                  10
_journal_year                    2019
_chemical_formula_moiety         'C44 H56 Br2 N2 Ni'
_chemical_formula_sum            'C44 H56 Br2 N2 Ni'
_chemical_formula_weight         831.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-13 deposited with the CCDC.    2019-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                89.688(5)
_cell_angle_beta                 82.245(6)
_cell_angle_gamma                88.268(5)
_cell_formula_units_Z            4
_cell_length_a                   11.341(2)
_cell_length_b                   17.349(3)
_cell_length_c                   20.734(3)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.252
_cell_measurement_theta_min      2.301
_cell_volume                     4040.4(12)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0940
_diffrn_reflns_av_unetI/netI     0.0957
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            65679
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.503
_diffrn_reflns_theta_min         2.131
_exptl_absorpt_coefficient_mu    2.490
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1078 before and 0.0666 after correction. The Ratio of minimum to maximum transmission is 0.6653. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     899
_refine_ls_number_reflns         16457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0614P)^2^+1.2080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1409
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10205
_reflns_number_total             16457
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9py00857h2.cif
_cod_data_source_block           22019211ni_0m
_cod_depositor_comments
'Adding full bibliography for 1552149--1552150.cif.'
_cod_original_cell_volume        4040.6(12)
_cod_database_code               1552149
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.826
_shelx_estimated_absorpt_t_min   0.663
_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.a Ternary CH refined with riding coordinates:
 C3(H3), C11(H11), C35(H35), C40(H40), C47(H47), C56(H56), C75(H75), C84(H84)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C12(H12A,H12B), C14(H14A,H14B), C36(H36A,H36B),
 C38(H38A,H38B), C41(H41A,H41B), C43(H43A,H43B), C46(H46A,H46B), C48(H48A,H48B),
  C57(H57A,H57B), C59(H59A,H59B), C76(H76A,H76B), C78(H78A,H78B), C85(H85A,
 H85B), C87(H87A,H87B)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25),
 C26(H26), C31(H31), C32(H32), C33(H33), C51(H51), C52(H52), C53(H53), C63(H63),
  C64(H64), C65(H65), C68(H68), C69(H69), C70(H70), C80(H80), C81(H81), C82(H82)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C),
 C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C42(H42A,H42B,H42C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C49(H49A,H49B,H49C), C58(H58A,H58B,H58C), C60(H60A,
 H60B,H60C), C77(H77A,H77B,H77C), C79(H79A,H79B,H79C), C86(H86A,H86B,H86C),
 C88(H88A,H88B,H88C)
;
_olex2_submission_special_instructions 'No special instructions were received'