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_7710386
_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 H31 N3 O2'
_chemical_formula_sum            'C26 H31 N3 O2'
_chemical_formula_weight         417.54
_chemical_name_common            LIGAND
_chemical_name_systematic        H3L
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-03-30
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-03-30 deposited with the CCDC.	2022-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.531(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8121(5)
_cell_length_b                   9.6447(4)
_cell_length_c                   18.5196(7)
_cell_measurement_reflns_used    4127
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      26.3250
_cell_measurement_theta_min      2.3520
_cell_volume                     2263.13(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      6.00 100.00   1.00   21.00    --   25.18  57.00  60.00   94
  2  \w    -20.00  98.00   1.00   21.00    --   25.18  19.00  30.00  118
  3  \w     10.00  63.00   1.00   21.00    --   25.18 -99.00 -60.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0153607000
_diffrn_orient_matrix_UB_12      -0.0006184000
_diffrn_orient_matrix_UB_13      0.0352658000
_diffrn_orient_matrix_UB_21      -0.0535508000
_diffrn_orient_matrix_UB_22      0.0068310000
_diffrn_orient_matrix_UB_23      -0.0159300000
_diffrn_orient_matrix_UB_31      -0.0048508000
_diffrn_orient_matrix_UB_32      -0.0732724000
_diffrn_orient_matrix_UB_33      -0.0018469000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7644
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.022
_diffrn_reflns_theta_max         25.022
_diffrn_reflns_theta_min         2.387
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeOH, CH2Cl2'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   1.000
_exptl_transmission_factor_min   0.890
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         3977
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+1.6597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1083
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3417
_reflns_number_total             3977
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01043g2.cif
_cod_data_source_block           H3L2
_cod_original_cell_volume        2263.14(16)
_cod_database_code               7710386
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O'
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.981
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O1A-C14
 1.37 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(O1A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: O1(0.9) H1(0.9) H14A(0.1) H14(0.9) O1A(0.1) H1A(0.1)
5.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C18(H14A), C16(H16), C14(H14), C11(H11), C8(H8), C10(H10),
 C9(H9), C4(H4), C3(H3A), C1(H5), C2(H2A)
5.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C21(H21A,H21B,H21C), C19(H19A,H19B,H19C)
5.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O1A(H1A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              36442
_shelx_hkl_checksum              87937
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.191
_oxdiff_exptl_absorpt_empirical_full_min 0.903