Pseudo-octahedral nickel(ii) complexes of strongly absorbing benzannulated pincer-type amido ligands: ligand-based redox and non-Aufbau electronic behaviour
Braun, Jason D.; Lozada, Issiah B.; Shepit, Michael; van Lierop, Johan; Herbert, David E.; RSC Advances 11 (2021) 3547–3555; doi:10.1039/D0RA10761A

data_7242150
_publ_section_title
;
 Pseudo-octahedral nickel(ii) complexes of strongly absorbing
 benzannulated pincer-type amido ligands: ligand-based redox and
 non-Aufbau electronic behaviour
;
_journal_issue                   6
_journal_name_full               'RSC Advances'
_journal_page_first              3547
_journal_page_last               3555
_journal_paper_doi               10.1039/D0RA10761A
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C46 H26 F6 N6 Ni, 2(C5 H12)'
_chemical_formula_sum            'C56 H50 F6 N6 Ni'
_chemical_formula_weight         979.73
_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             2020-01-16
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-13 deposited with the CCDC.	2021-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                113.683(2)
_cell_angle_beta                 90.763(2)
_cell_angle_gamma                113.819(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9342(6)
_cell_length_b                   14.6616(7)
_cell_length_c                   16.6289(8)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.57
_cell_volume                     2383.5(2)
_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      150.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            68060
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.529
_diffrn_reflns_theta_min         2.570
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.476
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0834 before and 0.0723 after correction.
The Ratio of minimum to maximum transmission is 0.8305.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       block
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         10937
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0350P)^2^+3.1118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1191
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8721
_reflns_number_total             10937
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra10761a2.cif
_cod_data_source_block           (CF3L)2Ni
_cod_database_code               7242150
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.882
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(F1B)=Sof(F2B)=Sof(F3B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C53(H53A,H53B), C54(H54A,
 H54B), C55(H55A,H55B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C13(H13), C15(H15),
 C16(H16), C17(H17), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27),
  C28(H28), C29(H29), C34(H34), C36(H36), C38(H38), C39(H39), C40(H40),
 C44(H44), C45(H45), C46(H46)
3.c Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C56(H56A,H56B,
 H56C)
;
_shelx_res_checksum              85373
_olex2_submission_special_instructions 'No special instructions were received'