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_7047775
_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
'O72 Sb2 W17.5 Zn6, 14(H2 O), 4(C12 H11 N4), 8.6(O), 2(C4 H12 N), 0.5(C24 H1'
_chemical_formula_sum            'C68 H109 N22 O94 Sb2 W18 Zn6'
_chemical_formula_weight         6683.79
_chemical_name_common            Hexa-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
_audit_creation_date             2017-08-17
_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                94.425(4)
_cell_angle_beta                 109.140(3)
_cell_angle_gamma                104.946(4)
_cell_formula_units_Z            1
_cell_length_a                   12.4792(8)
_cell_length_b                   17.4813(13)
_cell_length_c                   17.6938(11)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.240
_cell_measurement_theta_min      2.344
_cell_volume                     3467.5(4)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'APEX 2 v2011.2-0'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0849
_diffrn_reflns_av_unetI/netI     0.0714
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            56012
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.344
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              'Incoatec IuS'
_exptl_absorpt_coefficient_mu    16.367
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.4281
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1584 before and 0.0624 after correction.
The Ratio of minimum to maximum transmission is 0.5739.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.201
_exptl_crystal_description       plate
_exptl_crystal_F_000             3037
_exptl_crystal_recrystallization_method 'Evaporation in aqueous solution'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.096
_refine_diff_density_min         -1.887
_refine_diff_density_rms         0.327
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         12509
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.325
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0432P)^2^+53.8347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1124
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9612
_reflns_number_total             12509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02787k2.cif
_cod_data_source_block           elta076_p-1
_cod_depositor_comments
'Adding full bibliography for 7047772--7047776.cif.'
_cod_database_code               7047775
_shelx_estimated_absorpt_t_max   0.639
_shelx_estimated_absorpt_t_min   0.208