Synthesis, Reactivity, and Kinetics of Substitution in W3PdSe4 Cuboidal Clusters. A Reexamination of the Kinetics of Substitution of the Related W3S4 Cluster with Thiocyanate
Andrés G. Algarra; Maxim N. Sokolov; Javier González-Platas; María Jesús Fernández-Trujillo; Manuel G. Basallote; Rita Hernández-Molina; Inorganic Chemistry 48 (2009) 3639–3649; doi:10.1021/ic802150x

data_4301957
_publ_section_title
;
Synthesis, Reactivity, and Kinetics of Substitution in W3PdSe4 Cuboidal
Clusters. A Reexamination of the Kinetics of Substitution of the Related
W3S4 Cluster with Thiocyanate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3639
_journal_page_last               3649
_journal_paper_doi               10.1021/ic802150x
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'O18 Pd2 Se8 W6, 8(C7 H7 O3 S), 18(O)'
_chemical_formula_sum            'C56 H128 O60 Pd2 S8 Se8 W6'
_chemical_formula_weight         3965.64
_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                77.862(5)
_cell_angle_beta                 84.503(5)
_cell_angle_gamma                82.573(5)
_cell_formula_units_Z            1
_cell_length_a                   11.7366(9)
_cell_length_b                   15.0088(14)
_cell_length_c                   16.4770(16)
_cell_measurement_temperature    293(2)
_cell_volume                     2806.7(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Altomare et al., 2005)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0857
_diffrn_reflns_av_sigmaI/netI    0.1338
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50096
_diffrn_reflns_theta_full        28.67
_diffrn_reflns_theta_max         28.67
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    9.268
_exptl_absorpt_correction_T_max  0.523
_exptl_absorpt_correction_T_min  0.312
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.817
_refine_diff_density_min         -2.926
_refine_diff_density_rms         0.609
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         13819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1457
_reflns_number_gt                9106
_reflns_number_total             13819
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802150x_si_002.cif
_cod_data_source_block           w3se4pd
_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_database_code               4301957