Self-assembly of Schiff base anions and the trapping of HO−, O2− and Piv− bridges in a family of Ni3Ln4 complexes: synthesis, structures and magnetic properties
Biswas, Mousumi; Mavromagoulos, Athanasios; Murrie, Mark; Ray, Debashis; New Journal of Chemistry 47 (2023) 14868–14875; doi:10.1039/D3NJ01092A

data_7062592
_publ_section_title
;
 Self-assembly of Schiff base anions and the trapping of HO&#x2212;,
 O2&#x2212; and Piv&#x2212; bridges in a family of Ni3Ln4 complexes:
 synthesis, structures and magnetic properties
;
_journal_issue                   31
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14868
_journal_page_last               14875
_journal_paper_doi               10.1039/D3NJ01092A
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety
'C77.494 H97.482 N3 Ni3 O30.494 Tb4, 0.506(C1 H3 O1), 2H, 9[H2O]'
_chemical_formula_sum            'C78 H119 N3 Ni3 O40 Tb4'
_chemical_formula_weight         2550.55
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-07-05
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-07-07 deposited with the CCDC.	2023-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   20.046(4)
_cell_length_b                   20.046(4)
_cell_length_c                   15.420(3)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.047
_cell_measurement_theta_min      2.421
_cell_volume                     5366.2(18)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5-beta (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            57521
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.095
_diffrn_reflns_theta_max         25.095
_diffrn_reflns_theta_min         2.346
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.192
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       needle
_exptl_crystal_F_000             2540
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         6343
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0082P)^2^+7.9932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0510
_refine_ls_wR_factor_ref         0.0544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5605
_reflns_number_total             6343
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj01092a2.cif
_cod_data_source_block           complex_2
_cod_depositor_comments
'Adding full bibliography for 7062591--7062593.cif.'
_cod_original_cell_volume        5366(2)
_cod_database_code               7062592
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C17-C18 \\sim C17-C18A
 with sigma of 0.02
 C18-C20 \\sim C18-C19 \\sim C20-C19 \\sim C20A-C18A \\sim C20A-C19A \\sim
C18A-C19A
 with sigma of 0.04
 C17-C20 \\sim C17-C20A
 with sigma of 0.02
 C17-C19 \\sim C17-C19A
 with sigma of 0.02
 C17-C16 \\sim C17-C18 \\sim C17-C20 \\sim C17-C19 \\sim C17-C20A \\sim
C17-C18A \\sim C17-C19A
 with sigma of 0.02
 Ni1-O11 \\sim Ni1-O11A
 with sigma of 0.02
 O11-C26 \\sim O11A-C26A
 with sigma of 0.02
 Ni1-C26 \\sim Ni1-C26A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C18A) \\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C20A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C26) = Uanis(C26A)
Uanis(O11) = Uanis(O11A)
4. Rigid body (RIGU) restrains
 C18, C19, C20, C17, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C20A, C19A, C18A, C17, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(O11A)=1-FVAR(1)
 Sof(O11)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
 Fixed Sof: C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C20(0.5) H20A(0.5)
 H20B(0.5) H20C(0.5) C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5) C20A(0.5) H20D(0.5)
 H20E(0.5) H20F(0.5) C18A(0.5) H18D(0.5) H18E(0.5) H18F(0.5) C19A(0.5)
 H19D(0.5) H19E(0.5) H19F(0.5)
6.a Ternary CH refined with riding coordinates:
 O9(H9)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C13(H13), C10(H10), C3(H3), C12(H12), C5(H5), C11(H11), C4(H4)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C23(H23A,H23B,
 H23C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C),
 C20A(H20D,H20E,H20F), C18A(H18D,H18E,H18F), C19A(H19D,H19E,H19F), C26(H26A,
 H26B,H26C), C26A(H26D,H26E,H26F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 187 electrons were 
found in a volume of 1220\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 9[H2O] per 
Formula Unit which account for 180 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              61061
_shelx_fab_checksum              43439
_olex2_submission_special_instructions 'No special instructions were received'