Preparation and Properties of the Full Series of Cuboidal Clusters [MoxW4-xSe4(H2O)12]n+ (n= 4-6) and Their Derivatives
M. Sokolov; P. Esparza; R. Hernandez-Molina; J. G. Platas; A. Mederos; J. A. Gavin; R. Llusar; C. Vicent; Inorganic Chemistry 44 (2005) 1132–1141; doi:10.1021/ic049298a

data_4308622
_publ_contact_author_address
;
Departament de Ci\`encies Experimentals, Universitat Jaume I 
Campus de Riu Sec, Box 224, Castell\'o, Spain
;
_publ_contact_author_email       llusar@exp.uji.es
_publ_contact_author_name        'Professor Rosa Llusar'
_publ_section_title
;
Preparation and Properties of the Full Series of Cuboidal Clusters
[MoxW4-xSe4(H2O)12]n+ (n= 4-6) and Their Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1132
_journal_page_last               1141
_journal_paper_doi               10.1021/ic049298a
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C24 H60 Mo4 O12 P6 S12 Se4'
_chemical_formula_weight         1810.86
_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_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.204(5)
_cell_angle_beta                 87.584(5)
_cell_angle_gamma                84.193(5)
_cell_formula_units_Z            2
_cell_length_a                   13.3753(10)
_cell_length_b                   13.899(2)
_cell_length_c                   16.467(3)
_cell_measurement_temperature    150(2)
_cell_volume                     2899.6(7)
_computing_cell_refinement       'HKL Scalepck (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius BV, 1997-2000)'
_computing_data_reduction        'HKL Denzo and Scalepack)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  kappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            56936
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    4.000
_exptl_absorpt_correction_T_max  0.712
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.074
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.868
_refine_diff_density_min         -2.359
_refine_diff_density_rms         0.517
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         13331
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0708P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1315
_reflns_number_gt                10754
_reflns_number_total             13331
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049298asi20040601_102124_4.cif
_cod_data_source_block           '[Mo4Se4(dtp)6]'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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        2899.5(7)
_cod_database_code               4308622