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_7060423
_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         'C64 H72 N14 Ni5 O12, 2(C2 H3 N)'
_chemical_formula_sum            'C68 H78 N16 Ni5 O12'
_chemical_formula_weight         1605.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-02-12
_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                 105.300(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.3768(7)
_cell_length_b                   11.2447(3)
_cell_length_c                   30.5394(14)
_cell_measurement_reflns_used    11002
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.4100
_cell_measurement_theta_min      2.0720
_cell_volume                     7080.7(5)
_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 0.995
_diffrn_measured_fraction_theta_max 0.900
_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    -11.00 103.00   1.00   80.00    --   26.72  57.00 -30.00  114
  2  \w    -49.00  65.00   1.00   80.00    --   26.72 -57.00  90.00  114
  3  \w   -119.00 -86.00   1.00   80.00    --  -23.50 178.00-150.00   33
  4  \w    -57.00 114.00   1.00   80.00    --   26.72  19.00-150.00  171
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            21158
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.648
_diffrn_reflns_theta_min         1.939
_exptl_absorpt_coefficient_mu    1.377
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74233
_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 greenish green'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       block
_exptl_crystal_F_000             3336
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         7442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0373P)^2^+8.8047P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0884
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6339
_reflns_number_total             7442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00228g2.cif
_cod_data_source_block           l11nhnin3
_cod_depositor_comments
'Adding full bibliography for 7060423--7060424.cif.'
_cod_database_code               7060423
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.947
_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), N7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C7(H7A,H7B), C21(H21A,H21B), C9(H9A,H9B), C23(H23A,H23B),
 C22(H22A,H22B)
2.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C28(H28), C11(H11), C2(H2A), C5(H5), C12(H12), C17(H17), C13(H13),
 C14(H14), C25(H25), C19(H19), C27(H27), C3(H3), C4(H4), C26(H26), C18(H18)
2.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              75406
_shelx_hkl_checksum              82945
_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
;