A combined stopped-flow, electrospray ionization mass spectrometry and (31)P NMR study on the acetic acid-mediated fragmentation of the hydroxo-chalcogenide cluster [W(3)Se(4)(OH)(3)(dmpe)(3)](+) (dmpe = 1,2-bis(dimethylphosphanyl)ethane) to yield the dinuclear [W(2)Se(2)(mu-Se)(2)(mu-CH(3)CO(2))(dmpe)(2)](+) complex.
Algarra, Andrés G; Basallote, Manuel G.; Esther Castillo, C.; Corao, Carolina; Llusar, Rosa; Jesús Fernández-Trujillo, M; Vicent, Cristian; Dalton transactions (Cambridge, England : 2003)  (2006) 5725–5733; doi:10.1039/b611274a

data_7007837
_publ_section_title
;
 A combined stopped-flow, electrospray ionization mass spectrometry and
 (31)P NMR study on the acetic acid-mediated fragmentation of the
 hydroxo-chalcogenide cluster [W(3)Se(4)(OH)(3)(dmpe)(3)](+) (dmpe =
 1,2-bis(dimethylphosphanyl)ethane) to yield the dinuclear
 [W(2)Se(2)(mu-Se)(2)(mu-CH(3)CO(2))(dmpe)(2)](+) complex.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5725
_journal_page_last               5733
_journal_paper_doi               10.1039/b611274a
_journal_year                    2006
_chemical_formula_sum            'C14 H35 F6 O2 P5 Se4 W2'
_chemical_formula_weight         1187.81
_chemical_name_common            (W2Se4(dmpe)2(CH3CO2))PF6
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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                 91.892(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.446(5)
_cell_length_b                   12.795(7)
_cell_length_c                   14.728(8)
_cell_measurement_temperature    293(2)
_cell_volume                     1590.7(15)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1017
_diffrn_reflns_av_sigmaI/netI    0.2389
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7512
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    12.100
_exptl_absorpt_correction_type   'Bruker SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.309
_refine_diff_density_min         -1.173
_refine_diff_density_rms         0.292
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.41(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         5150
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1822
_refine_ls_R_factor_gt           0.0803
_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^)+(0.0770P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.2051
_reflns_number_gt                2565
_reflns_number_total             5150
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b611274a.txt
_cod_data_source_block           '[W2Se4(dmpe)2(CH3CO2)]PF6'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        1590.8(15)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7007837
_ratio_of_minimum_to_maximum_apparent_transmission 0.650835