Surface-grafted lanthanoid complexes of the tungstosilicate polyanion [SiW~12~O~40~]^4{-^}: a synthetic, structural and computational investigation
Derakhshanrad, Shadi; Mirzaei, Masoud; Najafi, Atefeh; Ritchie, Chris; Bauzá, Antonio; Frontera, Antonio; Mague, Joel T.; Acta Crystallographica Section C 74 (2018) –; doi:10.1107/S2053229618009580

data_2021262
_publ_section_title
;
 Surface-grafted lanthanoid complexes of the tungstosilicate polyanion
 [SiW~12~O~40~]^4{-^}: a synthetic, structural and computational
 investigation
;
_journal_coeditor_code           JR3020
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229618009580
_journal_volume                  74
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_iupac
'[Na Pr (C7 H3 N O5)3 (H2 O)13 (Si W12 O40)], 12H2 O'
_chemical_formula_moiety         'C21 H35 N3 Na O68 Pr3 Si W12, 9(H2 O), 3O'
_chemical_formula_sum            'C21 H53 N3 Na O80 Pr3 Si W12'
_chemical_formula_weight         4307.67
_chemical_name_systematic
;
Sodium aqua
tris[tetraaqua(\m-4-hydroxypyridine-2,6-dicarboxylato)praseodymium(III)]
silicododecatungstate dodecahydrate
;
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3'
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   18.119(3)
_cell_length_b                   18.119(3)
_cell_length_c                   21.078(3)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1241
_cell_measurement_theta_min      2.2480
_cell_volume                     5992.8(16)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2016)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2016) and <i>CELL_NOW</i>
(Sheldrick, 2008)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg & Putz, 2012)
;
_computing_publication_material
;
<i>SHELXTL</i> (Bruker, 2016)
;
_computing_structure_refinement
;
<i>SHELXL2018</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0849
_diffrn_reflns_av_unetI/netI     0.1276
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            74256
_diffrn_reflns_theta_full        29.150
_diffrn_reflns_theta_max         29.172
_diffrn_reflns_theta_min         1.618
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    19.138
_exptl_absorpt_correction_T_max  0.22
_exptl_absorpt_correction_T_min  0.09
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>TWINABS</i>; Sheldrick, 2009)
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    3.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             5790
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.115
_refine_diff_density_max         1.965
_refine_diff_density_min         -2.070
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2688 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.006(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         7142
_refine_ls_number_restraints     241
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0314P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0652
_reflns_number_gt                6106
_reflns_number_total             7142
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jr3020sup1.cif
_cod_data_source_block           jtm570b_4_a
_cod_original_cell_volume        5993(2)
_cod_database_code               2021262
_shelx_estimated_absorpt_t_min   0.092
_shelx_estimated_absorpt_t_max   0.217
_shelx_hkl_checksum              91485
_shelx_res_checksum              77992
_cod_database_fobs_code 2021262