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_7047773
_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 Na5 O83 Sb2 W19.89 Zn2.11, 4(C12 H10.25 N4)'
_chemical_formula_sum            'C48 H53 N16 Na5 O83 Sb2 W19.89 Zn2.11'
_chemical_formula_weight         6335.22
_chemical_name_common            '(2, 3-DAP)-di-zinc-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     heavy
_audit_creation_date             2017-08-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375)
;
_audit_update_record
;
2018-07-03 deposited with the CCDC.
2018-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                92.665(3)
_cell_angle_beta                 93.300(3)
_cell_angle_gamma                115.147(3)
_cell_formula_units_Z            1
_cell_length_a                   12.6796(7)
_cell_length_b                   14.1057(7)
_cell_length_c                   20.5025(11)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      30.522
_cell_measurement_theta_min      2.559
_cell_volume                     3303.7(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8 APEX'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            65919
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         2.115
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              'Incoatec IuS'
_exptl_absorpt_coefficient_mu    18.120
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1163 before and 0.0645 after correction. 
The Ratio of minimum to maximum transmission is 0.6031. 
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.184
_exptl_crystal_description       plate
_exptl_crystal_F_000             2809
_exptl_crystal_recrystallization_method 'Evaporation from water buffer'
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.724
_refine_diff_density_min         -1.822
_refine_diff_density_rms         0.322
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         12045
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0329P)^2^+128.4466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0956
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10072
_reflns_number_total             12045
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02787k2.cif
_cod_data_source_block           et046_0m_a
_cod_depositor_comments
'Adding full bibliography for 7047772--7047776.cif.'
_cod_database_code               7047773