Systematic studies on dibenzhydryl and pentiptycenyl substituted pyridine-imine nickel(ii) mediated ethylene polymerization.
Wang, Chaoqun; Zhang, Yuxing; Mu, Hongliang; Jian, Zhongbao; Dalton transactions (Cambridge, England : 2003) 49 (2020) 4824–4833; doi:10.1039/d0dt00505c

data_7703770
_publ_section_title
;
 Systematic studies on dibenzhydryl and pentiptycenyl substituted
 pyridine-imine nickel(ii) mediated ethylene polymerization.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4824
_journal_page_last               4833
_journal_paper_doi               10.1039/d0dt00505c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C82 H56 Br4 N4 Ni2 O2'
_chemical_formula_sum            'C82 H56 Br4 N4 Ni2 O2'
_chemical_formula_weight         1566.36
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-02-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2020-02-11 deposited with the CCDC.	2020-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.612(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.6818(17)
_cell_length_b                   16.776(2)
_cell_length_c                   22.885(3)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.492
_cell_measurement_theta_min      2.428
_cell_volume                     4339.8(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'bruker apex ccd'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2275
_diffrn_reflns_av_unetI/netI     0.1255
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            26588
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.428
_exptl_absorpt_coefficient_mu    2.316
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.380
_refine_diff_density_min         -2.160
_refine_diff_density_rms         0.176
_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     425
_refine_ls_number_reflns         7623
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0806
_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^)+(0.1082P)^2^+26.1756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2202
_refine_ls_wR_factor_ref         0.2325
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5737
_reflns_number_total             7623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00505c2.cif
_cod_data_source_block           Ni2
_cod_depositor_comments
'Adding full bibliography for 7703768--7703771.cif.'
_cod_original_cell_volume        4339.9(10)
_cod_database_code               7703770
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.618
_shelx_estimated_absorpt_t_min   0.543
_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. Uiso/Uaniso restraints and constraints
C7: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C23: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.014
Uanis(C20) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Ni1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C13(H13), C14(H14), C39(H39), C40(H40)
3.b Aromatic/amide H refined with riding coordinates:
 C35(H35), C24(H24), C19(H19), C20(H20), C6(H6), C1(H1), C18(H18), C4(H4),
 C21(H21), C30(H30), C38(H38), C25(H25), C33(H33), C27(H27), C3(H3), C26(H26),
 C2(H2), C31(H31), C36(H36), C32(H32), C37(H37)
3.c Idealised Me refined as rotating group:
 C01G(H01A,H01B,H01C)
;
_shelx_res_checksum              60589
_shelx_fab_checksum              80784
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'