Structural and vibrational properties of lanthanide Lindqvist polyoxometalate complexes.
Subintoro, Primadi J.; Carter, Korey P.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 9526–9539; doi:10.1039/d4dt00786g

data_7716059
_publ_section_title
;
 Structural and vibrational properties of lanthanide Lindqvist
 polyoxometalate complexes.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9526
_journal_page_last               9539
_journal_paper_doi               10.1039/d4dt00786g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'Ce Na9 O63.5 W10, 0.5(O)'
_chemical_formula_sum            'Ce Na9 O64 W10'
_chemical_formula_weight         3209.53
_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_primary     direct
_audit_creation_date             2023-12-20
_audit_creation_method
;FinalCif V134 by Daniel Kratzert, Freiburg 2024, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2024-02-29 deposited with the CCDC.	2024-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                101.615(2)
_cell_angle_beta                 98.179(2)
_cell_angle_gamma                101.864(2)
_cell_formula_units_Z            2
_cell_length_a                   12.8331(6)
_cell_length_b                   12.9660(6)
_cell_length_c                   20.1117(10)
_cell_measurement_reflns_used    9106
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.33
_cell_volume                     3148.5(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture Duo'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0969
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            129983
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.565
_diffrn_reflns_theta_min         2.123
_exptl_absorpt_coefficient_mu    19.071
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_correction_T_min  0.1524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.'
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.385
_exptl_crystal_description       plank
_exptl_crystal_F_000             2818
_exptl_crystal_preparation
'Sodium tungstate in aqueous media was acidified with Nitric acid followed by addition of Cerium Chloride solution'
_exptl_crystal_recrystallization_method 'Slow evaporation from water'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.668
_refine_diff_density_min         -3.372
_refine_diff_density_rms         0.593
_refine_ls_extinction_coef       0.00147(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         19235
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+87.1717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1264
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17254
_reflns_number_total             19235
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00786g2.cif
_cod_data_source_block           Complex_2
_cod_depositor_comments
'Adding full bibliography for 7716058--7716071.cif.'
_cod_database_code               7716059
_olex2_exptl_crystal_mounting_method 'Mitegen Mount'
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O62A) \\sim Ueq, Uanis(O29) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O57) \\sim Ueq, Uanis(O13) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O60) \\sim Ueq, Uanis(O62C) \\sim Ueq, Uanis(Na1) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.002
2. Others
 Fixed Sof: Na9B(0.5) Na9A(0.5) O57(0.5) O59(0.5) O61A(0.6) O62C(0.5) Na1(0.5)
 Na3(0.5) O62B(0.5) O62A(0.5) O61B(0.4) O67(0.5)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.115
_shelx_estimated_absorpt_t_max   0.251
_shelx_res_checksum              67871