Structural Variation, Magnetism and Single-source Deposition of Lanthanide-containing Polyoxotitanates
Muller, Rosa; Georghiades, Olivia; Bocarsly, Joshua D.; Sayed, Farheen N.; Riesgo-González, Victor; Bond, Andrew David; Grey, Clare P.; Wright, Dominic S.; Dalton Transactions  (2023) –; doi:10.1039/D3DT02553E

data_7713965
_publ_section_title
;
 Structural Variation, Magnetism and Single-source Deposition of
 Lanthanide-containing Polyoxotitanates
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02553E
_journal_year                    2023
_chemical_formula_moiety         'C36 H92 Cl2 Gd2 O20 Ti4'
_chemical_formula_sum            'C36 H92 Cl2 Gd2 O20 Ti4'
_chemical_formula_weight         1422.09
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2023-07-22 deposited with the CCDC.	2023-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.454(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9414(5)
_cell_length_b                   18.8718(8)
_cell_length_c                   12.7327(5)
_cell_measurement_reflns_used    9000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      66.46
_cell_measurement_theta_min      4.69
_cell_volume                     2866.8(2)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_collection       'APEX4 (Bruker, 2021)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-III'
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            49395
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.797
_diffrn_reflns_theta_max         66.797
_diffrn_reflns_theta_min         4.686
_diffrn_source                   'Incoatec I\mS Cu microsource'
_exptl_absorpt_coefficient_mu    20.613
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       block
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         5049
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0183
_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^)+(0.0215P)^2^+1.8308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0440
_refine_ls_wR_factor_ref         0.0448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4807
_reflns_number_total             5049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02553e2.cif
_cod_data_source_block           Ti4Gd2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7713965
_cambridge_user_name             'Rosa Mueller'
_cambridge_user_crsid            rm2055
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             RM93A
_cambridge_data_id               DW_B2_0373
_shelx_estimated_absorpt_t_min   0.232
_shelx_estimated_absorpt_t_max   0.289
_shelx_res_checksum              6399