Nickel complexes based on BIAN ligands: transformation and catalysis on ethylene polymerization.
Xu, Shuyun; Chen, Xuemeng; Luo, Gen; Gao, Wei; Dalton transactions (Cambridge, England : 2003) 50 (2021) 7356–7363; doi:10.1039/d1dt00649e

data_7707157
_publ_section_title
;
 Nickel complexes based on BIAN ligands: transformation and catalysis on
 ethylene polymerization.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7356
_journal_page_last               7363
_journal_paper_doi               10.1039/d1dt00649e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C72 H80 N4 Ni2 O2'
_chemical_formula_sum            'C72 H80 N4 Ni2 O2'
_chemical_formula_weight         1150.82
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2021-03-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-08 deposited with the CCDC.	2021-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.498(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2628(9)
_cell_length_b                   29.492(2)
_cell_length_c                   19.3880(14)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.47
_cell_volume                     7403.8(9)
_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    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      239.98
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39284
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.098
_diffrn_reflns_theta_max         25.098
_diffrn_reflns_theta_min         2.334
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5723
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.032
_exptl_crystal_description       block
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         13037
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0654P)^2^+3.9790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1411
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9364
_reflns_number_total             13037
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00649e1.cif
_cod_data_source_block           Complex_3b
_cod_depositor_comments
'Adding full bibliography for 7707155--7707157.cif.'
_cod_original_cell_volume        7403.9(9)
_cod_database_code               7707157
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.912
_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
Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C22, C24, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C58(H58), C22(H22), C70(H70), C19(H19), C55(H55), C34(H34), C67(H67), C31(H31)
4.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C10(H10), C39(H39), C15(H15), C17(H17), C16(H16), C8(H8), C40(H40),
 C46(H46), C53(H53), C27(H27), C44(H44), C3(H3), C9(H9), C29(H29), C51(H51),
 C52(H52), C45(H45), C5(H5), C65(H65), C4(H4), C28(H28), C63(H63), C64(H64)
4.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C60(H60A,H60B,H60C), C68(H68A,H68B,
 H68C), C23(H23A,H23B,H23C), C69(H69A,H69B,H69C), C24(H24A,H24B,H24C), C36(H36A,
 H36B,H36C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C32(H32A,H32B,H32C),
 C35(H35A,H35B,H35C), C72(H72A,H72B,H72C), C33(H33A,H33B,H33C), C71(H71A,H71B,
 H71C), C59(H59A,H59B,H59C)
;
_shelx_res_checksum              57225
_shelx_hkl_checksum              43984
_shelx_fab_checksum              12139
_olex2_submission_special_instructions 'No special instructions were received'