Ni(ii) complexes of a new tetradentate NN′N′′O picolinoyl-1,2-phenylenediamide-phenolate redox-active ligand at different redox levels
Mukhopadhyay, Narottam; Sengupta, Arunava; Vijay, Aswin Kottapurath; Lloret, Francesc; Mukherjee, Rabindranath; Dalton Transactions  (2022) –; doi:10.1039/D2DT01043G

data_7710384
_publ_section_title
;
 Ni(ii) complexes of a new tetradentate NN&#x2032;N&#x2032;&#x2032;O
 picolinoyl-1,2-phenylenediamide-phenolate redox-active ligand at
 different redox levels
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01043G
_journal_year                    2022
_chemical_formula_moiety         'F6 Sb, C26 H28 N3 Ni O2, 0.5[CH2Cl2]'
_chemical_formula_sum            'C26.5 H29 Cl F6 N3 Ni O2 Sb'
_chemical_formula_weight         751.44
_chemical_name_common            2
_chemical_name_systematic        '[Ni(L2)](SbF6)'
_chemical_properties_physical    Moisture-sensitive
_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             2022-03-25
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-03-25 deposited with the CCDC.	2022-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                67.728(3)
_cell_angle_beta                 81.980(3)
_cell_angle_gamma                86.088(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0860(7)
_cell_length_b                   12.2357(10)
_cell_length_c                   15.7588(13)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.025
_cell_measurement_theta_min      2.752
_cell_volume                     1428.5(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.9580
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0290
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11027
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.752
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.767
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5611
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1610 before and 0.0643 after correction.
The Ratio of minimum to maximum transmission is 0.7524.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             750
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.746
_exptl_transmission_factor_min   0.561
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         5039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0133P)^2^+0.9465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0597
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4526
_reflns_number_total             5039
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01043g2.cif
_cod_data_source_block           Complex2
_cod_original_formula_sum        'C26.50 H29 Cl F6 N3 Ni O2 Sb'
_cod_database_code               7710384
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.719
_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 Aromatic/amide H refined with riding coordinates:
 C10(H10), C16(H16), C11(H11), C1(H1), C4(H4), C9(H9), C8(H8), C14(H14),
 C3(H3), C2(H2)
2.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C22(H22A,H22B,H22C), C20(H20A,H20B,H20C), C19(H19A,H19B,
 H19C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 45 electrons were 
found in a volume of 144\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.5[CH2Cl2] per Formula Unit 
which account for 42 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              50409
_shelx_hkl_checksum              21105
_shelx_fab_checksum              67084
_olex2_submission_special_instructions 'No special instructions were received'