Metal‒organic frameworks based on polynuclear lanthanide complexes and octahedral rhenium clusters
Litvinova, Yulia M.; Gayfulin, Yakov M.; van Leusen, Jan; Samsonenko, Denis G.; Lazarenko, Vladimir A.; Zubavichus, Yan V.; Kögerler, Paul; Mironov, Yuri V.; Inorganic Chemistry Frontiers 6 (2019) 1518–; doi:10.1039/C9QI00339H

data_4350019
_publ_section_title
;
 Metal--organic frameworks based on polynuclear lanthanide complexes and
 octahedral rhenium clusters
;
_journal_issue                   6
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1518
_journal_paper_doi               10.1039/C9QI00339H
_journal_volume                  6
_journal_year                    2019
_chemical_formula_sum            'C30 H44 N10 O24 Re6 S8 Tb4'
_chemical_formula_weight         2938.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-03-20 deposited with the CCDC.	2019-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.930(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.6022(7)
_cell_length_b                   12.3896(3)
_cell_length_c                   23.5464(7)
_cell_measurement_reflns_used    22317
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      3.42
_cell_volume                     6158.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'ShelXle (H\"ubschle, 2011)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            52272
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.541
_diffrn_reflns_theta_min         3.251
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    16.614
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25313
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.169
_exptl_crystal_description       stick
_exptl_crystal_F_000             5296
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.070
_refine_diff_density_max         2.256
_refine_diff_density_min         -2.062
_refine_diff_density_rms         0.260
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         14100
_refine_ls_number_restraints     785
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+53.1300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0743
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12531
_reflns_number_total             14100
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9qi00339h2.cif
_cod_data_source_block           lit74Tb
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4350019
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.050
_shelx_estimated_absorpt_t_max   0.389
_shelx_res_checksum              84333
_shelx_hkl_checksum              55949