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_7716067
_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         'Na9 Nd O67 W10, 0.5(O)'
_chemical_formula_sum            'Na9 Nd O67.5 W10'
_chemical_formula_weight         3269.65
_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                98.160(2)
_cell_angle_beta                 102.820(2)
_cell_angle_gamma                101.538(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7722(5)
_cell_length_b                   13.0343(6)
_cell_length_c                   19.6802(8)
_cell_measurement_reflns_used    9541
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      33.102
_cell_measurement_theta_min      2.441
_cell_volume                     3070.0(2)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Venture Duo'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1081
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            185380
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.041
_exptl_absorpt_coefficient_mu    19.670
_exptl_absorpt_correction_T_max  0.2694
_exptl_absorpt_correction_T_min  0.1176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1586 before and 0.0958 after correction.
The Ratio of minimum to maximum transmission is 0.4365.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.537
_exptl_crystal_description       plate
_exptl_crystal_F_000             2878
_exptl_crystal_preparation
'Sodium Tungstate in aqueous media was acidified with Nitric acid. Neodymium Nitrate solution was then added into the tungstate solution.'
_exptl_crystal_recrystallization_method 'Slow evaporation from water'
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.051
_refine_diff_density_max         2.223
_refine_diff_density_min         -4.654
_refine_diff_density_rms         0.374
_refine_ls_extinction_coef       0.00046(3)
_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   1.041
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     878
_refine_ls_number_reflns         15235
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0371P)^2^+35.2102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12889
_reflns_number_total             15235
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00786g2.cif
_cod_data_source_block           Complex_4
_cod_depositor_comments
'Adding full bibliography for 7716058--7716071.cif.'
_cod_original_formula_sum        'Na9 Nd O67.50 W10'
_cod_database_code               7716067
_olex2_exptl_crystal_mounting_method 'Mitegen mount'
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O66B) \\sim Ueq, Uanis(O66A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O19) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
2. Others
 Fixed Sof: O45A(0.666667) Na8B(0.5) Na11(0.25) Na8A(0.25) Na10(0.5)
 Na9A(0.25) Na9B(0.25) O60B(0.5) O60A(0.5) O66A(0.75) O64A(0.5) O64B(0.5)
 O41A(0.5) O41B(0.5) O67(0.5) O45B(0.333333) O66B(0.25)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.101
_shelx_estimated_absorpt_t_max   0.434
_shelx_res_checksum              54484