Synthesis, structure, and magnetic properties of diamagnetic Co(iii) ion-based heterometallic CoIII–LnIII (Ln = Dy, Tb, Ho, Er) complexes
Barman, Nandini; Halder, Purbashree; Mukhopadhyay, Subrata; Schwarz, Björn; Colacio, Enrique; Rana, Rajanikanta; Rajaraman, Gopalan; Goura, Joydeb; New Journal of Chemistry 48 (2024) 15735–15746; doi:10.1039/D4NJ02058H

data_7063309
_publ_section_title
;
 Synthesis, structure, and magnetic properties of diamagnetic Co(iii)
 ion-based heterometallic CoIII--LnIII (Ln = Dy, Tb, Ho, Er) complexes
;
_journal_issue                   36
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15735
_journal_page_last               15746
_journal_paper_doi               10.1039/D4NJ02058H
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C38 H58 Co Ho N2 O12'
_chemical_formula_sum            'C38 H58 Co Ho N2 O12'
_chemical_formula_weight         958.72
_chemical_name_systematic        Monoclinic
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-27
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-27 deposited with the CCDC.	2024-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.197(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1250(10)
_cell_length_b                   10.6664(10)
_cell_length_c                   25.1229(18)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.495
_cell_measurement_theta_min      2.324
_cell_volume                     4127.9(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_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  0.0394
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            32055
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.604
_diffrn_source_current           45.0
_diffrn_source_power             2.25
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.366
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0673 before and 0.0477 after correction. The Ratio of minimum to maximum transmission is 0.8636. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       block
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.443
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.226
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0235
_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^)+22.0093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0544
_refine_ls_wR_factor_ref         0.0549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3505
_reflns_number_total             3638
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02058h2.cif
_cod_data_source_block           Compound_3
_cod_depositor_comments
'Adding full bibliography for 7063306--7063309.cif.'
_cod_database_code               7063309
_shelx_shelxl_version_number     2016/4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C7(H7), C4(H4), C2(H2)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C18(H18A,H18B,H18C), C13(H13A,H13B,H13C), C12(H12A,H12B,
 H12C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C)
2.d Idealised tetrahedral OH refined as rotating group:
 O6(H6)
;
_shelx_res_checksum              13198
_shelx_hkl_checksum              46569
_olex2_submission_special_instructions 'No special instructions were received'