(Me2NH2)10[H2-Dodecatungstate] polymorphs: dodecatungstate cages embedded in a variable dimethylammonium cation + water of crystallization matrix
Lendvay, György; Majzik, Eszter; Bereczki, Laura; Domján, Attila; Trif, László; Sajó, István E.; Franguelli, Fernanda Paiva; Farkas, Attila; Klébert, Szilvia; Bombicz, Petra; Németh, Csaba; Szilágyi, Imre Miklós; Kótai, László; RSC Advances 11 (2021) 3713–3724; doi:10.1039/D0RA09997J

data_7242146
_publ_section_title
;
 (Me2NH2)10[H2-Dodecatungstate] polymorphs: dodecatungstate cages embedded
 in a variable dimethylammonium cation + water of crystallization matrix
;
_journal_issue                   6
_journal_name_full               'RSC Advances'
_journal_page_first              3713
_journal_page_last               3724
_journal_paper_doi               10.1039/D0RA09997J
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'O42 W12, 10(C2 H8 N), 11(O)'
_chemical_formula_sum            'C20 H80 N10 O53 W12'
_chemical_formula_weight         3515.14
_chemical_name_common
;
dimethylammonium paratungstate B.11 hydrate
;
_chemical_name_systematic
;
decakis(dimethylammonium) dihydrododecatungstate(10-).11 hydrate
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-12-17 deposited with the CCDC.	2020-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.344(6)
_cell_angle_beta                 105.743(7)
_cell_angle_gamma                112.051(8)
_cell_formula_units_Z            2
_cell_length_a                   13.5917(3)
_cell_length_b                   16.6057(4)
_cell_length_c                   18.6449(4)
_cell_measurement_reflns_used    149683
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30.490
_cell_measurement_theta_min      3.015
_cell_volume                     3726.5(3)
_computing_cell_refinement
;
RAPID-AUTO (Rigaku Corp., Tokyo, Japan, 2015)
;
_computing_data_collection
;
RAPID-AUTO (Rigaku Corp., Tokyo, Japan, 2015)
;
_computing_data_reduction
;
RAPID-AUTO (Rigaku Corp., Tokyo, Japan, 2015)
;
_computing_molecular_graphics
;
Spek, A.L. (2003). J.Appl.Cryst. 36,7-13.
;
_computing_publication_material
;
C. F. Macrae, J. Appl. Cryst., 41, 466-470, 2008
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
;
L. Palatinus, G. Chapuis 2007 J. Appl. Cryst., Vol. 40, pp. 786-790.
;
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  RAXIS-RAPID
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1837
_diffrn_reflns_av_unetI/netI     0.1079
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            199047
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.491
_diffrn_reflns_theta_min         3.015
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    18.538
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.998
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
  NUMABS, Numerical Absorption correction Program (T.Higashi, 2011)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.133
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3164
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   0.999224
_exptl_transmission_factor_min   0.998108
_refine_diff_density_max         4.215
_refine_diff_density_min         -4.202
_refine_diff_density_rms         0.478
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     876
_refine_ls_number_reflns         22666
_refine_ls_number_restraints     663
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0687
_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^)+(0.0571P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1387
_refine_ls_wR_factor_ref         0.1505
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17352
_reflns_number_total             22666
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra09997j2.cif
_cod_data_source_block           shelx_CCDC1
_cod_database_code               7242146
_shelx_res_checksum              68356