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_7047774
_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
'Cd2 Cl Mn2 Na6 O89.5 Sb2 W18, 4(H2 O), 2(C4 H12 N)'
_chemical_formula_sum            'C8 H32 Cd2 Cl Mn2 N2 Na6 O93.5 Sb2 W18'
_chemical_formula_weight         5713.22
_chemical_name_common            Krebs-Cadmium-tungstoantimonate
_chemical_name_systematic
'Di-cadmium-di-manganese octadecatungstoantimonate'
_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_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-15 deposited with the CCDC.
2018-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                70.120(2)
_cell_angle_beta                 83.879(2)
_cell_angle_gamma                65.614(2)
_cell_formula_units_Z            1
_cell_length_a                   12.3753(7)
_cell_length_b                   13.6520(8)
_cell_length_c                   17.0910(10)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      30.119
_cell_measurement_theta_min      2.54
_cell_volume                     2471.2(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX 3'
_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)'
_diffrn_ambient_temperature      101.85
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42040
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.249
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              'Incoatec IuS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.216
_exptl_absorpt_correction_T_max  0.0082
_exptl_absorpt_correction_T_min  0.0003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1194 before and 0.0588 after correction. 
The Ratio of minimum to maximum transmission is 0.0366. 
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.839
_exptl_crystal_description       block
_exptl_crystal_F_000             2505
_exptl_crystal_recrystallization_method
'Evaporation of aqueous buffer solution'
_exptl_crystal_size_max          0.451
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.042
_refine_diff_density_max         3.967
_refine_diff_density_min         -1.826
_refine_diff_density_rms         0.656
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         8983
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0652
_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^)+(0.1280P)^2^+11.0744P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1693
_refine_ls_wR_factor_ref         0.1780
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7844
_reflns_number_total             8983
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02787k2.cif
_cod_data_source_block           mo_eltacd6_p-1_a_final
_cod_depositor_comments
'Adding full bibliography for 7047772--7047776.cif.'
_cod_original_formula_sum        'C8 H32 Cd2 Cl Mn2 N2 Na6 O93.50 Sb2 W18'
_cod_database_code               7047774
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.456
_shelx_estimated_absorpt_t_min   0.036