Tetranuclear {Ln<sup>III</sup>}<sub>4</sub> complexes possessing homometallic <i>O-capped</i> structural subunits: study of magnetic and photoluminescent properties.
Halder, Purbashree; Barman, Nandini; Tarannum, Ibtesham; Mukhopadhyay, Subrata; Schwarz, Björn; Singh, Saurabh Kumar; Goura, Joydeb; Dalton transactions (Cambridge, England : 2003) 54 (2025) 13879–13893; doi:10.1039/d4dt02976c

data_7719558
_publ_section_title
;
 Tetranuclear {Ln<sup>III</sup>}<sub>4</sub> complexes possessing
 homometallic <i>O-capped</i> structural subunits: study of magnetic and
 photoluminescent properties.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13879
_journal_page_last               13893
_journal_paper_doi               10.1039/d4dt02976c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C62 H92 Er4 N4 O22'
_chemical_formula_sum            'C62 H92 Er4 N4 O22'
_chemical_formula_weight         1914.43
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-02
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-22 deposited with the CCDC.	2025-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 128.970(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.351(2)
_cell_length_b                   13.7014(9)
_cell_length_c                   22.6638(18)
_cell_measurement_reflns_used    5516
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.92
_cell_measurement_theta_min      2.41
_cell_volume                     7327.5(9)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0987
_diffrn_reflns_av_unetI/netI     0.0811
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28744
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.355
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.605
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0861 before and 0.0625 after correction.
The Ratio of minimum to maximum transmission is 0.7886.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_description       block
_exptl_crystal_F_000             3760
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.667
_refine_diff_density_min         -0.948
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         6441
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0219P)^2^+8.8458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0732
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4939
_reflns_number_total             6441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02976c2.cif
_cod_data_source_block           Compound_5
_cod_original_cell_volume        7327.4(10)
_cod_database_code               7719558
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.770
_shelx_estimated_absorpt_t_min   0.608
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O3-H3
 0.87 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C16) \\sim Ueq, Uanis(C29) \\sim Ueq: with sigma of 0.04 and sigma for
terminal atoms of 0.002
Uanis(C26) = Uanis(C23)
Uanis(C24) = Uanis(C23)
Uanis(C29) = Uanis(C28)
Uanis(C13) = Uanis(C16)
Uanis(C14) = Uanis(C13)
Uanis(C25) = Uanis(C23)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3A), C2(H2A), C1(H1), C4(H4), C11(H11), C9(H9), C8(H8), C10(H10)
4.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C15(H15A,H15B,H15C), C29(H29A,H29B,
 H29C), C21(H21A,H21B,H21C), C31(H31A,H31B,H31C), C16(H16A,H16B,H16C), C30(H30A,
 H30B,H30C), C14(H14A,H14B,H14C), C26(H26A,H26B,H26C), C24(H24A,H24B,H24C),
 C25(H25A,H25B,H25C)
4.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              64259
_shelx_hkl_checksum              5548
_olex2_submission_special_instructions 'No special instructions were received'