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_2021261
_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 syn
_chemical_formula_iupac
'[Dy Na (C14 H6 N2 O4)3 (H2 O)9 (Si W12 O40)], 12H2 O'
_chemical_formula_moiety         'C42 H18 Dy3 N6 Na1 O61.5 Si1 W12, 12(O)'
_chemical_formula_sum            'C42 H18 Dy3 N6 Na O73.5 Si W12'
_chemical_formula_weight         4527.40
_chemical_name_systematic
;
Sodium tris[triaqua(\m-1,10-phenanthroline-2,9-dicarboxylato)dysprosium(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   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   20.3334(3)
_cell_length_b                   20.3334(3)
_cell_length_c                   18.7836(3)
_cell_measurement_reflns_used    11603
_cell_measurement_temperature    130.00(10)
_cell_measurement_theta_max      76.7970
_cell_measurement_theta_min      4.3290
_cell_volume                     6725.58(18)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      130.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16672
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.058
_diffrn_reflns_theta_min         3.440
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    41.928
_exptl_absorpt_correction_T_max  0.369
_exptl_absorpt_correction_T_min  0.097
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.353
_exptl_crystal_description       block
_exptl_crystal_F_000             6033
_exptl_crystal_size_max          0.066
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.031
_refine_diff_density_max         1.533
_refine_diff_density_min         -1.890
_refine_ls_abs_structure_details
;
Classical Flack method preferred over Parsons because s.u. lower
;
_refine_ls_abs_structure_Flack   0.013(7)
_refine_ls_extinction_coef       0.000018(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         5475
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0696P)^2^+182.8632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.0976
_reflns_number_gt                5450
_reflns_number_total             5475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jr3020sup1.cif
_cod_data_source_block           d23_4
_cod_original_cell_volume        6725.60(19)
_cod_original_formula_sum        'C42 H18 Dy3 N6 Na O73.50 Si W12'
_cod_database_code               2021261
_shelx_estimated_absorpt_t_min   0.168
_shelx_estimated_absorpt_t_max   0.356