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_4101882
_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_sum            'C30 H138 K9 Mo23 N5 O113 S24'
_chemical_formula_weight         5705.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_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                 92.5880(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.0140(2)
_cell_length_b                   27.2308(5)
_cell_length_c                   19.7247(3)
_cell_measurement_reflns_used    149801
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.34
_cell_measurement_theta_min      2.03
_cell_volume                     9665.8(3)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 512x512
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            222028
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         0.75
_exptl_absorpt_coefficient_mu    1.974
_exptl_absorpt_correction_T_max  0.7696
_exptl_absorpt_correction_T_min  0.5367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, V2.10)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.960
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             5556
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.579
_refine_diff_density_min         -2.602
_refine_diff_density_rms         0.246
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.20(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1888
_refine_ls_number_reflns         51875
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1405
_refine_ls_wR_factor_ref         0.1474
_reflns_number_gt                43437
_reflns_number_total             51875
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja909762p_si_001.cif
_cod_data_source_block           1
_cod_database_code               4101882