Capture of the [Mo~3~S~4~]^4+^ Cluster within a {Mo~18~} Macrocycle Yielding a Supramolecular Assembly Stabilized by a Dynamic H-Bond Network
Sylvain Duval; Sébastien Floquet; Corine Simonnet-Jégat; Jérôme Marrot; Rosa Ngo Biboum; Bineta Keita; Louis Nadjo; Mohamed Haouas; Francis Taulelle; Emmanuel Cadot; Journal of the American Chemical Society 132 (2010) 2069–2077; doi:10.1021/ja909762p

data_4101883
_publ_contact_author
;
      Pr E. Cadot
      Institut Lavoisier de Versailles, UMR CNRS 8180
      Universit\'e de Versailles 
      45 Avenue des Etats Unis
      78035 Versailles
      France
;
_publ_contact_author_email       emmanuel.cadot@chimie.uvsq.fr
_publ_contact_author_fax         '(33) 01 39 25 43 81'
_publ_contact_author_phone       '(33) 01 39 25 43 73'
_publ_section_title
;
 Capture of the [Mo~3~S~4~]^4+^ Cluster within a {Mo~18~} Macrocycle
 Yielding a Supramolecular Assembly Stabilized by a Dynamic H-Bond Network
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2069
_journal_page_last               2077
_journal_paper_doi               10.1021/ja909762p
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C24 H56 K2 Mo4 N4 Na2 O42 S4'
_chemical_formula_sum            'C24 H56 K2 Mo4 N4 Na2 O42 S4'
_chemical_formula_weight         1708.91
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.4851(12)
_cell_length_b                   20.4851(12)
_cell_length_c                   29.203(2)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.98
_cell_measurement_theta_min      1.41
_cell_volume                     12254.7(13)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    Diamond
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0788
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            91285
_diffrn_reflns_theta_full        30.38
_diffrn_reflns_theta_max         30.38
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    1.189
_exptl_absorpt_correction_T_max  0.8903
_exptl_absorpt_correction_T_min  0.6477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick,V2.10)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             6848
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.930
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.266
_refine_ls_extinction_coef       0.00027(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    geom
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         9178
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1200
_refine_ls_R_factor_gt           0.0691
_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^)+(0.1267P)^2^+53.5034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2074
_refine_ls_wR_factor_ref         0.2486
_reflns_number_gt                5677
_reflns_number_total             9178
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja909762p_si_002.cif
_cod_data_source_block           3
_cod_original_cell_volume        12254.6(14)
_cod_original_sg_symbol_Hall     '-P 4/a 2ac  '
_cod_original_sg_symbol_H-M      'P 4/n c c '
_cod_database_code               4101883