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_7703769
_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         'C84 H60 Br4 N4 Ni2 O2'
_chemical_formula_sum            'C84 H60 Br4 N4 Ni2 O2'
_chemical_formula_weight         1594.42
_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                 109.8600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.9201(2)
_cell_length_b                   22.8955(5)
_cell_length_c                   14.1583(3)
_cell_measurement_reflns_used    8519
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      59.053
_cell_measurement_theta_min      4.719
_cell_volume                     3329.34(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      173.0
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'bruker apex ccd'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14606
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        59.053
_diffrn_reflns_theta_max         59.053
_diffrn_reflns_theta_min         4.719
_exptl_absorpt_coefficient_mu    3.941
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.4366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       needle
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.842
_refine_diff_density_min         -1.583
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.00020(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         4747
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0676P)^2^+5.4143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1371
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3982
_reflns_number_total             4747
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00505c2.cif
_cod_data_source_block           Ni4
_cod_depositor_comments
'Adding full bibliography for 7703768--7703771.cif.'
_cod_database_code               7703769
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.827
_shelx_estimated_absorpt_t_min   0.384
_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.a Ternary CH refined with riding coordinates:
 C16(H16), C14(H14), C15(H15), C17(H17)
2.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C4(H4), C26(H26), C38(H38), C31(H31), C3(H3), C27(H27), C34(H34),
 C19(H19), C39(H39), C29(H29), C2(H2), C1(H1), C22(H22), C28(H28), C32(H32),
 C20(H20), C21(H21), C33(H33), C40(H40)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              9654
_olex2_submission_special_instructions 'No special instructions were received'