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_7716061
_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 O63.4 Pr W10, 1.75(O)'
_chemical_formula_sum            'Na9 O65.15 Pr W10'
_chemical_formula_weight         3228.72
_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             2024-02-07
_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                101.581(2)
_cell_angle_beta                 98.253(2)
_cell_angle_gamma                101.755(2)
_cell_formula_units_Z            2
_cell_length_a                   12.8137(6)
_cell_length_b                   12.9517(7)
_cell_length_c                   20.0978(12)
_cell_measurement_reflns_used    9394
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      32.931
_cell_measurement_theta_min      2.350
_cell_volume                     3139.3(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 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0878
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            234155
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.241
_diffrn_reflns_theta_min         2.039
_exptl_absorpt_coefficient_mu    19.180
_exptl_absorpt_correction_T_max  0.2694
_exptl_absorpt_correction_T_min  0.1389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1404 before and 0.0808 after correction.
The Ratio of minimum to maximum transmission is 0.5156.
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    3.416
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             2838
_exptl_crystal_preparation
'Sodium Tungstate in aqueous media was acidified with Nitric acid, followed by addition of Praseodymium Nitrate solution'
_exptl_crystal_recrystallization_method 'Slow evaporation from water'
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.083
_refine_diff_density_max         3.995
_refine_diff_density_min         -5.382
_refine_diff_density_rms         0.424
_refine_ls_extinction_coef       0.00034(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   1.115
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     893
_refine_ls_number_reflns         23994
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0338P)^2^+79.9484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1181
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18931
_reflns_number_total             23994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00786g2.cif
_cod_data_source_block           Complex_3
_cod_depositor_comments
'Adding full bibliography for 7716058--7716071.cif.'
_cod_database_code               7716061
_olex2_exptl_crystal_mounting_method 'Mitegen mount'
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O49B) \\sim Ueq, Uanis(O48A) \\sim Ueq, Uanis(O48B) \\sim Ueq, Uanis(O37)
\\sim Ueq, Uanis(O36) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
2. Others
 Fixed Sof: O61B(0.5) O62B(0.5) O68(0.5) O64(0.5) Na2B(0.5) Na2A(0.5)
 O50(0.75) O47(0.4) O49B(0.5) O61A(0.5) O62A(0.5) O48B(0.25) O48A(0.25)
 Na3B(0.26) O70(0.5) Na3A(0.34) Na9(0.4) O37(0.25) O69(0.25) O49A(0.5) O51(0.5)
 O52A(0.5) O71A(0.666667) O52B(0.5) O71B(0.333333)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.138
_shelx_estimated_absorpt_t_max   0.299
_shelx_res_checksum              33176