Chiral [Mo3S4H3(diphosphine)3]+ Hydrido Clusters and Study of the Effect of the Metal Atom on the Kinetics of the Acid-Assisted Substitution of the Coordinated Hydride: Mo vs W
Andrés G. Algarra; Manuel G. Basallote; M. Jesús Fernández-Trujillo; Marta Feliz; Eva Guillamón; Rosa Llusar; Ivan Sorribes; Cristian Vicent; Inorganic Chemistry 49 (2010) 5935–5942; doi:10.1021/ic100381u

data_4315909
_publ_contact_author             'Rosa Llusar'
_publ_contact_author_address
;
 Departament de Qu\'imica F\'isica i Anal\'itica, Universitat Jaume I,  
 Av. Sos Baynat s/n,  12071 Castell\'o de la Plana, Spain.
;
_publ_contact_author_email       llusar@exp.uji.es
_publ_contact_author_phone       '+34 964 728086'
_publ_section_title
;
 Chiral [Mo3S4H3(diphosphine)3]+ Hydrido Clusters and Study of the Effect
 of the Metal Atom on the Kinetics of the Acid-Assisted Substitution of
 the Coordinated Hydride: Mo vs W
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5935
_journal_page_last               5942
_journal_paper_doi               10.1021/ic100381u
_journal_volume                  49
_journal_year                    2010
_chemical_absolute_configuration syn
_chemical_formula_sum            'C42.5 H85 Br4 Cl P6 S4 W3'
_chemical_formula_weight         1816.81
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 98.248(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.0152(9)
_cell_length_b                   19.7370(15)
_cell_length_c                   15.0015(12)
_cell_measurement_reflns_used    7390
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.03
_cell_measurement_theta_min      2.28
_cell_volume                     3520.7(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0544
_diffrn_reflns_av_sigmaI/netI    0.1036
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19168
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    7.476
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.574947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1746
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.943
_refine_diff_density_min         -1.502
_refine_diff_density_rms         0.263
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.023(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         11606
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0564
_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^)+(0.1019P)^2^+10.8804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1684
_reflns_number_gt                9128
_reflns_number_total             11606
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100381u_si_001_2.cif
_cod_data_source_block           '[3]Br0.5CH2Cl2'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'C42.50 H85 Br4 Cl P6 S4 W3'
_cod_database_code               4315909