Bis(tetraphenylphosphonium) octa-μ~3~-chloro-hexakis(trifluoromethanesulfonato)-<i>octahedro</i>-hexamolybdate dichloromethane/diethyl ether solvate
Peay, Miya; Updegraff III, James; Gray, Thomas G.; Acta Crystallographica Section E 62 (2006) m2895–m2897; doi:10.1107/S1600536806040517

data_2211225
_publ_section_title
;Bis(tetraphenylphosphonium)
 octa-\m~3~-chloro-hexakis(trifluoromethanesulfonato)-<i>octahedro</i>-hexamolybdate
 dichloromethane/diethyl ether solvate
;
_journal_coeditor_code           WM2040
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2895
_journal_page_last               m2897
_journal_paper_doi               10.1107/S1600536806040517
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac
;
(C24 H20 P)2 [Mo6 Cl8 (C F3 O3 S)6], C4 H10 O, C H2 Cl2
;
_chemical_formula_moiety
;
2C24 H20 P +, C6 Cl8 F18 Mo6 O18 S6 2-, C4 H10 O, C H2 Cl2
;
_chemical_formula_sum            'C59 H52 Cl8 F18 Mo6 O19 P2 S6'
_chemical_formula_weight         2432.40
_chemical_name_systematic
;
Bis(tetraphenylphosphonium) [octa(\m^3^-chloro)hexakis
(trifluoromethanesulfonato)-<i>octahedro</i>-hexamolybdate]
dichloromethane/diethylether solvate
;
_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
_cell_angle_alpha                74.640(2)
_cell_angle_beta                 75.367(2)
_cell_angle_gamma                74.263(2)
_cell_formula_units_Z            1
_cell_length_a                   11.8710(4)
_cell_length_b                   13.8264(5)
_cell_length_c                   14.0267(5)
_cell_measurement_reflns_used    5957
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.88
_cell_measurement_theta_min      3.12
_cell_volume                     2095.87(13)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2004)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX2 CCD'
_diffrn_measurement_method       '\f and \w 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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24669
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.57
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.412
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS in SAINT-Plus; Bruker, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular chunk'
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.402
_refine_diff_density_min         -1.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         9451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0615P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0972
_reflns_number_gt                7868
_reflns_number_total             9451
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm2040.cif
_cod_data_source_block           I
_cod_database_code               2211225
_cod_database_fobs_code          2211225