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_7047776
_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 W18 Zn6, 4(C4 H12 N)'
_chemical_formula_sum            'C16 H48 N4 O72 Sb2 W18 Zn6'
_chemical_formula_weight         5393.60
_chemical_name_common            (TMA)4Hexa-zinc-18-tungstoantimonate
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 95.440(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.5029(12)
_cell_length_b                   23.1699(12)
_cell_length_c                   18.1162(11)
_cell_measurement_reflns_used    9097
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.994
_cell_measurement_theta_min      2.697
_cell_volume                     6060.2(7)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_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)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2444
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            151418
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.876
_diffrn_reflns_theta_min         2.083
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.674
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.1335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction. 
wR2(int) was 0.1811 before and 0.1090 after correction. 
The Ratio of minimum to maximum transmission is 0.1790. 
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.956
_exptl_crystal_description       block
_exptl_crystal_F_000             4724
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         3.336
_refine_diff_density_min         -6.817
_refine_diff_density_rms         0.681
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         7386
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0753
_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^)+(0.1346P)^2^+178.2807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1982
_refine_ls_wR_factor_ref         0.2026
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6705
_reflns_number_total             7386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02787k2.cif
_cod_data_source_block           elta076_c2m
_cod_depositor_comments
'Adding full bibliography for 7047772--7047776.cif.'
_cod_database_code               7047776
_shelx_estimated_absorpt_t_max   0.094
_shelx_estimated_absorpt_t_min   0.071