A novel polyoxo(thio)molybdenum(V) sulfite compound: Synthesis and crystal structure of {[Mo2V(�-S)2O2]6(�3-SO3)4(�-SO3)12}20? anion
Miras, Haralampos N.; Derek Woollins, J.; Slawin, Alexandra M.; Raptis, Raphael; Baran, Peter; Kabanos, Themistoklis A.; Dalton Transactions  (2003) 3668–; doi:10.1039/b309473c

data_7013513
_publ_section_title
;
 A novel polyoxo(thio)molybdenum(V) sulfite compound: Synthesis and
 crystal structure of
 {[Mo2V(&#xFFFD;-S)2O2]6(&#xFFFD;3-SO3)4(&#xFFFD;-SO3)12}20? anion
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              3668
_journal_paper_doi               10.1039/b309473c
_journal_year                    2003
_chemical_formula_moiety
'[N H4]14.K6.[Mo12 O60 S28].[H2 O]2.5.[C H4 O]2'
_chemical_formula_sum            'C2 H69 K6 Mo12 N14 O64.5 S28'
_chemical_formula_weight         3605.27
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.260(4)
_cell_length_b                   23.199(3)
_cell_length_c                   16.6631(19)
_cell_measurement_reflns_used    142
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      168
_cell_measurement_theta_min      12
_cell_volume                     11698(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      125(2)
_diffrn_detector_area_resol_mean 0.9
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1445
_diffrn_reflns_av_sigmaI/netI    0.1432
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            49929
_diffrn_reflns_theta_full        23.35
_diffrn_reflns_theta_max         23.35
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    2.039
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.779237
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.047
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7044
_exptl_crystal_size_max          .1
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .05
_refine_diff_density_max         2.032
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.210
_refine_ls_extinction_coef       0.00031(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         8619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.916
_refine_ls_R_factor_all          0.1263
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0954P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1566
_refine_ls_wR_factor_ref         0.1769
_reflns_number_gt                4649
_reflns_number_total             8619
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b309473c.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        11697(2)
_cod_original_sg_symbol_H-M      Pnma
_cod_original_formula_sum        'C2 H69 K6 Mo12 N14 O64.50 S28'
_cod_database_code               7013513