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_7710387
_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         'C26 H28 N3 Ni O2, C10 H10 Co, C6 H6'
_chemical_formula_sum            'C42 H44 Co N3 Ni O2'
_chemical_formula_weight         740.44
_chemical_name_common            3
_chemical_name_systematic        '[Co(AE\<z5-C5H5)2][Ni(L2)]'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive,Oxygen-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
;
2022-04-04 deposited with the CCDC.	2022-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                85.954(2)
_cell_angle_beta                 81.575(3)
_cell_angle_gamma                89.811(3)
_cell_formula_units_Z            4
_cell_length_a                   10.6611(9)
_cell_length_b                   17.4758(15)
_cell_length_c                   19.0544(17)
_cell_measurement_reflns_used    9435
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.027
_cell_measurement_theta_min      2.388
_cell_volume                     3502.9(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0487
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43863
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.388
_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    1.052
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6412
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.2050 before and 0.0597 after correction.
The Ratio of minimum to maximum transmission is 0.8599.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic brownish red'
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_recrystallization_method Layering
_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   0.641
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.061
_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     895
_refine_ls_number_reflns         12386
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0231P)^2^+2.7197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10284
_reflns_number_total             12386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01043g2.cif
_cod_data_source_block           Complex3
_cod_database_code               7710387
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.817
_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:
 C36(H36), C16(H16), C40(H40), C42(H42), C60(H60), C14(H14), C27(H27),
 C29(H29), C61(H61), C63(H63), C64(H64), C2(H2), C62(H62), C11(H11), C10(H10),
 C37(H37), C28(H28), C68(H68), C1(H1), C58(H58), C8(H8), C35(H35), C59(H59),
 C67(H67), C34(H34), C53(H53), C9(H9), C30(H30), C3(H3), C72(H72), C57(H57),
 C4(H4), C66(H66), C65(H65), C74(H74), C71(H71), C73(H73), C69(H69), C54(H54),
 C70(H70), C76(H76), C75(H75), C82(H82), C56(H56), C81(H81), C78(H78), C77(H77),
  C83(H83), C80(H80), C55(H55), C84(H84), C79(H79)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C50(H50A,H50B,H50C), C22(H22A,H22B,H22C), C21(H21A,H21B,
 H21C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C51(H51A,H51B,H51C), C52(H52A,
 H52B,H52C), C47(H47A,H47B,H47C), C24(H24A,H24B,H24C), C46(H46A,H46B,H46C),
 C48(H48A,H48B,H48C)
;
_shelx_res_checksum              79388
_shelx_hkl_checksum              52796
_olex2_submission_special_instructions 'No special instructions were received'