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_7703768
_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         'C78 H64 Br4 N4 Ni2 O2'
_chemical_formula_sum            'C78 H64 Br4 N4 Ni2 O2'
_chemical_formula_weight         1526.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                96.0490(10)
_cell_angle_beta                 91.8800(10)
_cell_angle_gamma                107.2170(10)
_cell_formula_units_Z            1
_cell_length_a                   9.5838(6)
_cell_length_b                   13.0175(9)
_cell_length_c                   13.8929(9)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.479
_cell_measurement_theta_min      2.344
_cell_volume                     1642.61(19)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'bruker apex ccd'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47034
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.521
_diffrn_reflns_theta_min         2.344
_exptl_absorpt_coefficient_mu    3.057
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1408 before and 0.0830 after correction.
The Ratio of minimum to maximum transmission is 0.6699.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       block
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.0046(6)
_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   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         7505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0319P)^2^+1.0684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0756
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6506
_reflns_number_total             7505
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00505c2.cif
_cod_data_source_block           Ni1
_cod_depositor_comments
'Adding full bibliography for 7703768--7703771.cif.'
_cod_database_code               7703768
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.515
_shelx_estimated_absorpt_t_min   0.461
_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:
 C00D(H00D), C00F(H00F)
2.b Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00E(H00E), C00G(H00G), C00L(H00L), C00M(H00M), C00N(H00N),
 C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T),
 C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y), C00Z(H00Z),
 C010(H010), C012(H012), C013(H013), C014(H014), C015(H015), C016(H016),
 C017(H017), C018(H018), C019(H019)
2.c Idealised Me refined as rotating group:
 C011(H01A,H01B,H01C)
;
_shelx_res_checksum              78379
_olex2_submission_special_instructions 'No special instructions were received'