Octahedral lanthanide clusters containing a central PO43- anion: structures, luminescent, magnetic and relaxometric properties
Qu, Yi-Ping; Huang, Xin-Da; Xu, Kui; Bao, Song-Song; Zheng, Li-Min; Dalton Transactions  (2023) –; doi:10.1039/D3DT01542D

data_7713361
_publ_section_title
;
 Octahedral lanthanide clusters containing a central PO43- anion:
 structures, luminescent, magnetic and relaxometric properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01542D
_journal_year                    2023
_chemical_formula_moiety         'C130 H114 Gd6 N6 O34 P9 [+ solvent]'
_chemical_formula_sum            'C130 H114 Gd6 N6 O34 P9'
_chemical_formula_weight         3526.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-05-17 deposited with the CCDC.	2023-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                86.674(2)
_cell_angle_beta                 76.792(2)
_cell_angle_gamma                89.442(2)
_cell_formula_units_Z            2
_cell_length_a                   15.2645(7)
_cell_length_b                   15.4068(7)
_cell_length_c                   29.8145(13)
_cell_measurement_reflns_used    9813
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      53.991
_cell_measurement_theta_min      2.624
_cell_volume                     6814.7(5)
_computing_cell_refinement       'APEX 3'
_computing_data_collection       'APEX 3'
_computing_data_reduction        "'APEX 3"
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 4K
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 with Metal Jet'
_diffrn_measurement_method       CCD
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0858
_diffrn_reflns_av_unetI/netI     0.0766
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            87398
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        52.981
_diffrn_reflns_theta_max         52.981
_diffrn_reflns_theta_min         2.587
_exptl_absorpt_coefficient_mu    16.104
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.4810
_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            'light yellow'
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_description       block
_exptl_crystal_F_000             3454
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.703
_refine_diff_density_min         -1.806
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1658
_refine_ls_number_reflns         24067
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0541P)^2^+10.8559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1246
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18116
_reflns_number_total             24067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01542d2.cif
_cod_data_source_block           Gd6
_cod_database_code               7713361
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.296
_shelx_estimated_absorpt_t_max   0.296
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              58503
_shelx_fab_checksum              72154