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_4320813
_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     (NH4)3.20K0.80H3O[Mo3O4(HCO2)8]HCO2.H2O
_chemical_formula_sum            'C9 H26.8 K0.8 Mo3 N3.2 O24'
_chemical_formula_weight         883.06
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                106.817(7)
_cell_angle_beta                 91.651(9)
_cell_angle_gamma                88.340(9)
_cell_formula_units_Z            2
_cell_length_a                   11.011(2)
_cell_length_b                   13.310(2)
_cell_length_c                   9.993(1)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    294
_cell_measurement_theta_max      14.3
_cell_measurement_theta_min      10.1
_cell_volume                     1401.0(4)
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5370
_diffrn_reflns_reduction_process 5161
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.6
_diffrn_standards_decay_%        11
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.507
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   'integration, DATAP,KRYSTAL(Hazell,1995)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    2.093
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             872.80
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.81(9)
_refine_diff_density_min         -0.87(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   0.887
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    20
_refine_ls_number_parameters     451
_refine_ls_number_reflns         3972
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.026
_refine_ls_shift/esd_max         0.121
_refine_ls_shift/esd_mean        0.006
_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         0.034
_reflns_number_observed          3972
_reflns_number_total             4926
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            ic9906656_2.cif
_cod_data_source_block           compound(1)
_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 
;
_cod_original_cell_volume        1401.0(3)
_cod_original_formula_sum        'C9 H26.80 K0.80 Mo3 N3.20 O24'
_cod_database_code               4320813