Synthesis of the first Zn<sub>6</sub>-hexagon sandwich-tungstoantimonate via rearrangement of a non-lacunary Krebs-type polyoxotungstate.
Tanuhadi, Elias; Roller, Alexander; Giester, Gerald; Kampatsikas, Ioannis; Rompel, Annette; Dalton transactions (Cambridge, England : 2003) 47 (2018) 15651–15655; doi:10.1039/c8dt02787k

data_7047772
_publ_section_title
;
 Synthesis of the first Zn<sub>6</sub>-hexagon sandwich-tungstoantimonate
 via rearrangement of a non-lacunary Krebs-type polyoxotungstate.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15651
_journal_page_last               15655
_journal_paper_doi               10.1039/c8dt02787k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'H12 K4 Mn3 O74.5 Sb2 W19, 5.6(H2 O), 4(C12 H11 N4)'
_chemical_formula_sum            'C48 H67.2 K4 Mn3 N16 O80.1 Sb2 W19'
_chemical_formula_weight         6207.84
_chemical_name_common            '(2, 3-DAP)-tri-manganese-18-tungstoantimonate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-08-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2018-07-03 deposited with the CCDC.
2018-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                108.55(3)
_cell_angle_beta                 91.90(3)
_cell_angle_gamma                99.07(3)
_cell_formula_units_Z            1
_cell_length_a                   12.116(2)
_cell_length_b                   14.374(3)
_cell_length_c                   21.414(4)
_cell_measurement_temperature    200
_cell_volume                     3477.6(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Nonius Kappa'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_av_unetI/netI     0.0980
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            37980
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.064
_diffrn_reflns_theta_min         2.075
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              'Incoatec IuS'
_exptl_absorpt_coefficient_mu    16.489
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.964
_exptl_crystal_description       plate
_exptl_crystal_F_000             2767
_exptl_crystal_recrystallization_method
'Evaporation from aqueous buffer solution'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.181
_refine_diff_density_min         -2.688
_refine_diff_density_rms         0.337
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     800
_refine_ls_number_reflns         20123
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0553
_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^)+(0.0702P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1451
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12262
_reflns_number_total             20123
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02787k2.cif
_cod_data_source_block           rot
_cod_depositor_comments
'Adding full bibliography for 7047772--7047776.cif.'
_cod_original_formula_sum        'C48 H67.20 K4 Mn3 N16 O80.10 Sb2 W19'
_cod_database_code               7047772
_shelx_estimated_absorpt_t_max   0.493
_shelx_estimated_absorpt_t_min   0.493