A further step towards tuning the properties of metal-chalcogenide nanocapsules by replacing skeletal oxide by sulphide ligands.
Schäffer, Christian; Todea, Ana Maria; Bögge, Hartmut; Floquet, Sébastien; Cadot, Emmanuel; Korenev, Vladimir S.; Fedin, Vladimir P.; Gouzerh, Pierre; Müller, Achim; Dalton transactions (Cambridge, England : 2003) 42 (2013) 330–333; doi:10.1039/c2dt32247a

data_7020868
_publ_section_title
;
 A further step towards tuning the properties of metal-chalcogenide
 nanocapsules by replacing skeletal oxide by sulphide ligands.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              330
_journal_page_last               333
_journal_paper_doi               10.1039/c2dt32247a
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C68 H1012 Mo60 N68 Na4 O764 S60 W72'
_chemical_formula_weight         36022.62
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   notdet
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   32.6869(18)
_cell_length_b                   32.6869(18)
_cell_length_c                   73.762(4)
_cell_measurement_reflns_used    9085
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.20
_cell_volume                     68251(6)
_computing_cell_refinement       'APEX2 v2009.11-0 (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 v2009.11-0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_molecular_graphics    'DIAMOND 2.1 (Crystal Impact, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device       'Bruker KAPPA APEX II X8 PROSPECTOR ULTRA'
_diffrn_measurement_device_type  'four circle diffractometer'
_diffrn_measurement_method       'omega- and phi-scans'
_diffrn_radiation_monochromator  'graphite monochromator '
_diffrn_radiation_source         'fine focus sealed tube '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0580
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       95
_diffrn_reflns_limit_l_min       -95
_diffrn_reflns_number            184856
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.106
_exptl_absorpt_correction_T_max  0.1867
_exptl_absorpt_correction_T_min  0.1260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Bruker AXS, 2008)'
_exptl_crystal_colour            reddish
_exptl_crystal_density_diffrn    2.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             50580
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.134
_refine_diff_density_min         -2.127
_refine_diff_density_rms         0.285
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1255
_refine_ls_number_reflns         34131
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+3446.9529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1591
_reflns_number_gt                25014
_reflns_number_total             34131
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32247a.txt
_cod_data_source_block           m1894
_cod_original_cell_volume        68251(7)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7020868