Hybrid lanthanide double-deckers based on calixarene and polyoxometalate units
Jiao, Yushu; Sanz, Sergio; Izarova, Natalya V.; van Leusen, Jan; Sarwar, Sidra; Dalgarno, Scott; Brechin, Euan K.; Kögerler, Paul; Dalton Transactions  (2022) –; doi:10.1039/D2DT00769J

data_7709759
_publ_section_title
;
 Hybrid lanthanide double-deckers based on calixarene and polyoxometalate
 units
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00769J
_journal_year                    2022
_chemical_formula_sum            'C83 H144 Cl2 Gd Mo5 N3 O22'
_chemical_formula_weight         2243.85
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-01-19 deposited with the CCDC.	2022-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.345(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   67.2987(15)
_cell_length_b                   12.5266(2)
_cell_length_c                   23.4455(4)
_cell_measurement_reflns_used    18285
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2930
_cell_measurement_theta_min      3.4680
_cell_volume                     19231.4(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4623
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       80
_diffrn_reflns_limit_h_min       -78
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            84378
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.182
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.434
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             9176
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.533
_refine_diff_density_min         -1.500
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1045
_refine_ls_number_reflns         16931
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0363P)^2^+72.3114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.1039
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12688
_reflns_number_total             16931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00769j2.cif
_cod_data_source_block           gd_a
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7709759
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.762
_shelx_estimated_absorpt_t_max   0.958
_shelx_res_checksum              4181