Synthesis of the novel [W3PdS4H3(dmpe)3(CO)]+ cubane cluster and kinetic studies on the substitution of coordinated hydrides in acidic media.
Algarra, Andrés G; Basallote, Manuel G.; Feliz, Marta; Fernandez-Trujillo, M Jesús; Guillamón, Eva; Llusar, Rosa; Vicent, Cristian; Inorganic chemistry 45 (2006) 5576–5584; doi:10.1021/ic052184u

data_4350203
_publ_section_title
;
 Synthesis of the novel [W3PdS4H3(dmpe)3(CO)]+ cubane cluster and kinetic
 studies on the substitution of coordinated hydrides in acidic media.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5576
_journal_page_last               5584
_journal_paper_doi               10.1021/ic052184u
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C43 H71 B O P6 Pd S4 W3'
_chemical_formula_weight         1586.82
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 134.204(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.037(3)
_cell_length_b                   21.782(2)
_cell_length_c                   22.351(2)
_cell_measurement_temperature    293(2)
_cell_volume                     11181.0(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0928
_diffrn_reflns_av_sigmaI/netI    0.1223
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            38487
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    6.820
_exptl_absorpt_correction_type   'Bruker SADABS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.885
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6112
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.624
_refine_diff_density_min         -1.384
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         12821
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1197
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0255P)^2^+104.1158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1162
_reflns_number_gt                7305
_reflns_number_total             12821
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic052184usi20051223_032929.cif
_cod_data_source_block           '[W3PdS4H3(dmpe)3(CO)]BPh4'
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        11181.1(18)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4350203
_ratio_of_minimum_to_maximum_apparent_transmission 0.739167