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_7703771
_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         'C40 H34 Br2 N2 Ni O'
_chemical_formula_sum            'C40 H34 Br2 N2 Ni O'
_chemical_formula_weight         777.22
_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             2020-02-11
_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                 105.2580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7994(7)
_cell_length_b                   20.1287(14)
_cell_length_c                   16.4169(11)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.399
_cell_measurement_theta_min      2.397
_cell_volume                     3442.9(4)
_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)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'bruker apex ccd'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            56091
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.513
_diffrn_reflns_theta_min         2.398
_exptl_absorpt_coefficient_mu    2.919
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1226 before and 0.0608 after correction.
The Ratio of minimum to maximum transmission is 0.4037.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         7885
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0313P)^2^+2.8052P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6291
_reflns_number_total             7885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00505c2.cif
_cod_data_source_block           Ni3
_cod_depositor_comments
'Adding full bibliography for 7703768--7703771.cif.'
_cod_database_code               7703771
_shelx_shelxl_version_number     2016/6
_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:
 C12(H12), C41(H41)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C13(H13), C25(H25), C29(H29), C35(H35), C37(H37), C42(H42), C43(H43),
 C45(H45), C46(H46), C50(H50), C53(H53), C55(H55), C56(H56), C59(H59), C63(H63),
  C65(H65), C68(H68), C69(H69), C70(H70), C72(H72), C73(H73), C81(H81),
 C83(H83), C85(H85), C86(H86)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C75(H75A,H75B,H75C)
;
_shelx_res_checksum              94587
_olex2_submission_special_instructions 'No special instructions were received'