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_7709758
_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            'C84.5 H147 Cl5 Mo5 N3 O22 Y'
_chemical_formula_weight         2302.90
_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   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                100.93(3)
_cell_angle_beta                 102.94(3)
_cell_angle_gamma                101.77(3)
_cell_formula_units_Z            2
_cell_length_a                   13.449(3)
_cell_length_b                   14.984(3)
_cell_length_c                   27.024(5)
_cell_measurement_reflns_used    8928
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.99
_cell_measurement_theta_min      1.62
_cell_volume                     5036(2)
_computing_cell_refinement
;
X-Area Recipe 1.36.0.0 (STOE, 2020)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.170.0 (STOE, 2020)
;
_computing_data_reduction
;
X-Area Integrate 1.78.3.0 (STOE, 2020)
X-Area X-Red 1.65.2.0 (STOE, 2020) 
;
_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 5.81
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_av_unetI/netI     0.0848
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            92044
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.280
_diffrn_source                   'Genix Mo'
_exptl_absorpt_coefficient_mu    1.371
_exptl_absorpt_correction_T_max  0.9432
_exptl_absorpt_correction_T_min  0.7589
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2370
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.289
_refine_diff_density_min         -1.688
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1099
_refine_ls_number_reflns         17716
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1266
_refine_ls_R_factor_gt           0.0794
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1414P)^2^+3.1387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2056
_refine_ls_wR_factor_ref         0.2388
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11169
_reflns_number_total             17716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00769j2.cif
_cod_data_source_block           y_a
_cod_original_formula_sum        'C84.50 H147 Cl5 Mo5 N3 O22 Y'
_cod_database_code               7709758
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.752
_shelx_estimated_absorpt_t_max   0.935
_shelx_res_checksum              64716