μ~2~-Acetato-κ^2^<i>O</i>:<i>O</i>'-(4,4'-bipyridyl-κ<i>N</i>)tris(diethyl dithiophosphato-κ^2^<i>S</i>,<i>S</i>')-μ~3~-sulfido-tri-μ~2~-sulfido-trimolybdenum(IV) diethyl ether monosolvate
Kawamoto, Keisuke; Kinoshita, Isamu; Acta Crystallographica Section E 70 (2014) m240–m241; doi:10.1107/S1600536814012501

data_2239634
_publ_section_title
;
 \m~2~-Acetato-\k^2^<i>O</i>:<i>O</i>'-(4,4'-bipyridyl-\k<i>N</i>)tris(diethyl
 dithiophosphato-\k^2^<i>S</i>,<i>S</i>')-\m~3~-sulfido-tri-\m~2~-sulfido-trimolybdenum(IV)
 diethyl ether monosolvate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m240
_journal_page_last               m241
_journal_paper_doi               10.1107/S1600536814012501
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac
'[Mo3 (C2 H3 O2) (C4 H10 O2 P S2)3 S4 (C10 H8 N2)], C4 H10 O'
_chemical_formula_moiety         'C24 H41 Mo3 N2 O8 P3 S10, C4 H10 O'
_chemical_formula_sum            'C28 H51 Mo3 N2 O9 P3 S10'
_chemical_formula_weight         1261.06
_chemical_name_systematic
;\m~2~-Acetato-\k^2^<i>O</i>:<i>O</i>'-(4,4'-bipyridyl-\k<i>N</i>)tris(diethyl
dithiophosphato-\k^2^<i>S</i>,<i>S</i>')-\m~3~-sulfido-tri-\m~2~-sulfido-trimolybdenum(V) diethyl ether solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 107.7183(16)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   13.1573(16)
_cell_length_b                   27.647(3)
_cell_length_c                   14.2153(17)
_cell_measurement_reflns_used    12390
_cell_measurement_temperature    153
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.04
_cell_volume                     4925.7(10)
_computing_cell_refinement       'CrystalClear (Rigaku, 2010)'
_computing_data_collection       'CrystalClear (Rigaku, 2010)'
_computing_data_reduction        'CrystalClear (Rigaku, 2010)'
_computing_molecular_graphics    'CrystalStructure (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1994)'
_diffrn_ambient_temperature      153
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            40597
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.317
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>REQAB</i>; Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2544.00
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.730
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     506
_refine_ls_number_reflns         11260
_refine_ls_number_restraints     1
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0350P)^2^+9.5598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0945
_reflns_number_gt                9267
_reflns_number_total             11260
_reflns_threshold_expression     F^2^>2\s(F^2^)
_cod_data_source_file            cv5459sup1.cf
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2239634.cif.'
_cod_original_cell_volume        4925.6(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2239634
_cod_database_fobs_code          2239634