A HPLC-ICP-AES technique for the screening of [XW11NbO40]n− aqueous solutions
Shmakova, Alexandra A.; Akhmetova, Maria M.; Volchek, Victoria V.; Romanova, Tamara E.; Korolkov, Ilya; Sheven, Dmitri G.; Adonin, Sergey A.; Abramov, Pavel A.; Sokolov, Maxim N.; New Journal of Chemistry 42 (2018) 7940–; doi:10.1039/C7NJ04702A

data_7057085
_publ_section_title
;
 A HPLC-ICP-AES technique for the screening of [XW11NbO40]n&#x2212;
 aqueous solutions
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7940
_journal_paper_doi               10.1039/C7NJ04702A
_journal_volume                  42
_journal_year                    2018
_chemical_formula_sum            'C36 H84 Co2 N12 O52 P W12'
_chemical_formula_weight         3872.18
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-03-01 deposited with the CCDC.
2018-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   15.8751(6)
_cell_length_b                   15.8751(6)
_cell_length_c                   31.9698(14)
_cell_measurement_reflns_used    2417
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      29.0750
_cell_measurement_theta_min      3.8190
_cell_volume                     6977.6(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'ShelXle (H\"ubschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.830
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.830
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            6745
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.556
_diffrn_reflns_theta_min         3.514
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    15.221
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.765
_exptl_crystal_description       plate
_exptl_crystal_F_000             5271
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.060
_refine_diff_density_max         3.509
_refine_diff_density_min         -4.374
_refine_diff_density_rms         0.370
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.23(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4974
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0706P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1247
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.830
_reflns_number_gt                4549
_reflns_number_total             4974
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c7nj04702a2.cif
_cod_data_source_block           1_b_sq
_cod_depositor_comments
'Adding full bibliography for 7057085--7057086.cif.'
_cod_original_cell_volume        6977.6(6)
_cod_database_code               7057085
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.135
_shelx_estimated_absorpt_t_max   0.462
_shelx_res_checksum              20737
_shelx_fab_checksum              58080