Crystal structure of hexasodium tetraserinolium paratungstate B decahydrate, [Na~6~{(CH~2~OH)~2~CHNH~3~}~4~][W~12~O~40~(OH)~2~]·10H~2~O
Sifaki, Kleanthi; Gumerova, Nadiia I.; Giester, Gerald; Rompel, Annette; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S2056989022000457

data_2244016
_publ_section_title
;
 Crystal structure of hexasodium tetraserinolium paratungstate B
 decahydrate,
 [Na~6~{(CH~2~OH)~2~CHNH~3~}~4~][W~12~O~40~(OH)~2~]&#x00B7;10H~2~O
;
_journal_coeditor_code           WM5630
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022000457
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac
'[Na6 (C3 H10 N1 O2)4] [W12 O40 (O H)2] , 10 H2 O'
_chemical_formula_moiety         'C12 H56 N4 Na6 O60 W12'
_chemical_formula_sum            'C12 H62 N4 Na6 O60 W12'
_chemical_formula_weight         3566.79
_chemical_name_common            'Sodium-serinol paratungstate B'
_chemical_name_systematic
;Hexasodium tetraserinolium
di-\m~3~-hydroxido-tetra-\m~3~-oxido-octadeca-\m-oxido-octadecaoxidododecatungstate decahydrate
;
_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_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_cell_angle_alpha                73.180(2)
_cell_angle_beta                 65.308(2)
_cell_angle_gamma                64.345(2)
_cell_formula_units_Z            1
_cell_length_a                   12.0541(8)
_cell_length_b                   12.0821(8)
_cell_length_c                   12.7050(8)
_cell_measurement_reflns_used    9742
_cell_measurement_temperature    200.15
_cell_measurement_theta_max      33.14
_cell_measurement_theta_min      2.17
_cell_volume                     1502.07(17)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015)
;
_computing_structure_solution
;
<i>olex2.solve</i> (Bourhis <i>et al.</i>,  2015)
;
_diffrn_ambient_temperature      200.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            39702
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.169
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.042
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.2452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    3.943
_exptl_crystal_description       block
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.052
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.986
_refine_diff_density_min         -1.615
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.247
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         5490
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.247
_refine_ls_R_factor_all          0.0176
_refine_ls_R_factor_gt           0.0171
_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^)+(0.0095P)^2^+5.2022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0422
_refine_ls_wR_factor_ref         0.0425
_reflns_number_gt                5404
_reflns_number_total             5490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5630sup1.cif
_cod_data_source_block           I
_cod_database_code               2244016
_shelx_estimated_absorpt_t_min   0.029
_shelx_estimated_absorpt_t_max   0.031
_shelx_hkl_checksum              23958
_shelx_res_checksum              13885
_cod_database_fobs_code 2244016