Mixed Valency in Hydrogen Bonded 'Dimers of Dimers'
Luke A. Wilkinson; Laura McNeill; Anthony J. H. M. Meijer; Nathan J. Patmore; Journal of the American Chemical Society 135 (2013) 1723–1726; doi:10.1021/ja312176x

data_4119307
_publ_section_title
;
 Mixed Valency in Hydrogen Bonded 'Dimers of Dimers'
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1723
_journal_page_last               1726
_journal_paper_doi               10.1021/ja312176x
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C56 H84 Mo2 N2 O10 S2, 2(C2 H6 O S)'
_chemical_formula_sum            'C60 H96 Mo2 N2 O12 S4'
_chemical_formula_weight         1357.51
_chemical_name_systematic
;
 ?
;
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                96.497(2)
_cell_angle_beta                 107.341(2)
_cell_angle_gamma                103.535(2)
_cell_formula_units_Z            2
_cell_length_a                   13.5032(4)
_cell_length_b                   14.9415(5)
_cell_length_c                   17.9245(6)
_cell_measurement_reflns_used    6797
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      2.352
_cell_volume                     3290.33(19)
_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    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.981
_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  0.0628
_diffrn_reflns_av_sigmaI/netI    0.0789
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34287
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.566
_exptl_absorpt_correction_T_max  0.9508
_exptl_absorpt_correction_T_min  0.8266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       block
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.209
_refine_diff_density_min         -1.930
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         11518
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.0674
_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^)+(0.0781P)^2^+21.0551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1625
_refine_ls_wR_factor_ref         0.2072
_reflns_number_gt                7049
_reflns_number_total             11518
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja312176x_si_002_1.cif
_cod_data_source_block           2(DMSO)2.2DMSO
_cod_original_cell_volume        3290.33(18)
_cod_database_code               4119307