Discrete unusual mixed-bridged trinuclear CoIII2CoII and pentanuclear NiII coordination complexes supported by a phenolate-based ligand: theoretical and experimental magneto-structural study
Richa,; Rathnam, Muni; Kumar, Akhilesh; Verma, Indresh; Kłak, Julia; Cano, Joan; Mota, Antonio J.; Rajput, Amit; Arora, Himanshu; New Journal of Chemistry 45 (2021) 6053–6066; doi:10.1039/D1NJ00228G

data_7060424
_publ_section_title
;
 Discrete unusual mixed-bridged trinuclear CoIII2CoII and pentanuclear
 NiII coordination complexes supported by a phenolate-based ligand:
 theoretical and experimental magneto-structural study
;
_journal_issue                   13
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6053
_journal_page_last               6066
_journal_paper_doi               10.1039/D1NJ00228G
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         '2(C32 H36 Co3 N16 O6)'
_chemical_formula_sum            'C64 H72 Co6 N32 O12'
_chemical_formula_weight         1835.11
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-02-14 deposited with the CCDC.	2021-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6157(8)
_cell_length_b                   15.3792(6)
_cell_length_c                   28.2430(9)
_cell_measurement_reflns_used    6425
_cell_measurement_temperature    100
_cell_measurement_theta_max      65.7970
_cell_measurement_theta_min      3.6570
_cell_volume                     8520.2(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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    -51.00  64.00   1.00    4.00    --   25.65 -57.00  90.00  115
  2  \w      1.00  82.00   1.00    4.00    --   25.65 -99.00  60.00   81
  3  \w    -13.00 102.00   1.00    4.00    --   25.65  57.00 120.00  115
  4  \w    100.00 153.00   1.00   16.00    --   66.82 111.00 -30.00   53
  5  \w    100.00 153.00   1.00   16.00    --   66.82 111.00 150.00   53
  6  \w    100.00 153.00   1.00   16.00    --   66.82 111.00   0.00   53
  7  \w    100.00 153.00   1.00   16.00    --   66.82 111.00 -60.00   53
  8  \w     27.00 145.00   1.00   16.00    --   66.82  61.00  90.00  118
  9  \w    100.00 153.00   1.00   16.00    --   66.82 111.00-120.00   53
 10  \w     34.00 109.00   1.00   16.00    --   66.82 -94.00 120.00   75
 11  \w    123.00 164.00   1.00   32.00    --  108.00  77.00 -58.53   41
 12  \w     56.00  99.00   1.00   32.00    --  108.00  43.00 -90.00   43
 13  \w    103.00 129.00   1.00   32.00    --  108.00  43.00 -90.00   26
 14  \w     21.00 113.00   1.00   32.00    --  108.00-104.00   0.00   92
 15  \w     32.00  58.00   1.00   32.00    --  108.00  28.00-131.67   26
 16  \w    143.00 171.00   1.00   32.00    --  108.00 104.00  90.00   28
 17  \w    101.00 176.00   1.00   32.00    --  108.00 104.00  30.00   75
 18  \w     74.00 107.00   1.00   32.00    --  108.00-104.00 120.00   33
 19  \w     78.00 111.00   1.00   32.00    --  108.00 -98.00-155.17   33
 20  \w    129.00 157.00   1.00   32.00    --  108.00 104.00  60.00   28
 21  \w     42.00 106.00   1.00   32.00    --  108.00-104.00-150.00   64
 22  \w    119.00 145.00   1.00   32.00    --  108.00 -65.00-120.00   26
 23  \w     61.00  96.00   1.00   32.00    --  108.00 -65.00-120.00   35
 24  \w    100.00 133.00   1.00   32.00    --  108.00  28.00-131.67   33
 25  \w    143.00 176.00   1.00   32.00    --  108.00  65.00-150.00   33
 26  \w     86.00 166.00   1.00   32.00    --  108.00 138.00 -90.00   80
 27  \w    102.00 131.00   1.00   32.00    --  108.00 104.00  90.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            30490
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        66.087
_diffrn_reflns_theta_max         66.087
_diffrn_reflns_theta_min         3.652
_exptl_absorpt_coefficient_mu    9.548
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull brownish brown'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3752
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         7373
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0840P)^2^+0.6749P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4717
_reflns_number_total             7373
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00228g2.cif
_cod_data_source_block           l11nhcon3
_cod_depositor_comments
'Adding full bibliography for 7060423--7060424.cif.'
_cod_database_code               7060424
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.832
_shelx_estimated_absorpt_t_min   0.598
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N2(H2), N10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C23(H23A,H23B), C24(H24A,H24B), C9(H9A,H9B), C8(H8A,H8B),
 C25(H25A,H25B)
2.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C28(H28), C5(H5), C30(H30), C27(H27), C14(H14), C13(H13), C29(H29),
 C21(H21), C19(H19), C2(H2A), C11(H11), C20(H20), C12(H12), C4(H4), C3(H3)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C32(H32A,H32B,H32C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              35570
_shelx_hkl_checksum              6137
_shelx_fab_checksum              5871
_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
;