Preparation and Crystal Structures of Formato Complexes of the [M^IV^~3~O~4~]^4+^ and [M^IV^~3~S~4~]^4+^ (M = Mo,W) Clusters. Convenient Precursors to the Corresponding Aqua Complexes
Michael Brorson; Alan Hazell; Claus J. H. Jacobsen; Iver Schmidt; Jørgen Villadsen; Inorganic Chemistry 39 (2000) 1346–1350; doi:10.1021/ic9906656

data_4320812
_publ_contact_author
;
Michael Brorson
Haldor Tops\/oe Research Laboratories
Nym\/ollevej 55
DK-2800 Lyngby
Denmark
;
_publ_section_title
;
 Preparation and Crystal Structures of Formato Complexes of the
 [M^IV^~3~O~4~]^4+^ and [M^IV^~3~S~4~]^4+^ (M = Mo,W) Clusters. Convenient
 Precursors to the Corresponding Aqua Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1346
_journal_page_last               1350
_journal_paper_doi               10.1021/ic9906656
_journal_volume                  39
_journal_year                    2000
_chemical_formula_structural     K6[W3S4(HCO2)9]HCO2.2.27H2O.0.73CH3OH
_chemical_formula_sum            'C10.73 H17.46 K6 O23 S4 W3'
_chemical_formula_weight         1428.920
_chemical_name_systematic        ?
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90
_cell_angle_beta                 118.94(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.605(6)
_cell_length_b                   14.458(7)
_cell_length_c                   13.627(5)
_cell_measurement_radiation      'Mo K\a'
_cell_measurement_reflns_used    30
_cell_measurement_temperature    294
_cell_measurement_theta_max      14.4
_cell_measurement_theta_min      10.1
_cell_measurement_wavelength     0.71073
_cell_volume                     3380(2)
_computing_cell_refinement       MAD
_computing_data_collection       'MAD (Allibon, 1995)'
_computing_data_reduction        'KRYSTAL (Hazell, 1995)'
_computing_molecular_graphics
;                                  
      ORTEP-III (Burnett & Johnson, 1996), KRYSTAL                    
;
_computing_publication_material  KRYSTAL
_computing_structure_refinement  'modified ORFLS(1962), KRYSTAL'
_computing_structure_solution
;                                  
      SIR92 (Altomare et al., 1994) KRYSTAL                           
;
_diffrn_ambient_temperature      294
_diffrn_measurement_device       'Huber four-circle diffractometer'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           'Ag K\a'
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4989
_diffrn_reflns_reduction_process 4794
_diffrn_reflns_theta_max         22.5
_diffrn_reflns_theta_min         1.3
_diffrn_standards_decay_%        8
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    6.121
_exptl_absorpt_correction_T_max  0.513
_exptl_absorpt_correction_T_min  0.326
_exptl_absorpt_correction_type   integration,DATAP,KRYSTAL(Hazell,1995)
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.807
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2663.360
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.9(2)
_refine_diff_density_min         -1.9(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.224
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    2
_refine_ls_number_parameters     234
_refine_ls_number_reflns         2656
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.046
_refine_ls_shift/esd_max         0.037
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.055
_reflns_number_observed          2656
_reflns_number_total             4664
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            ic9906656_1.cif
_cod_data_source_block           compound(2)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '
1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^' was changed to 'calc'. New
tag '_refine_ls_weighting_details' was created. The value of the new
tag was set to 'w = 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constrained' was replaced with
the value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

'_atom_site_thermal_displace_type' value 'Uij' was replaced with the
value 'Uani' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'
(29 times).

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        3381(2)
_cod_original_sg_symbol_Hall     '-C 2y '
_cod_database_code               4320812