Preparation, Structure, and Properties of the Corner-Shared Double Cubes [Mo6HgQ8(H2O)18]8+ (Q = S, Se) and Tungsten Analogues
Vladimir P. Fedin; Maxim Sokolov; Gert J. Lamprecht; Rita Hernandez-Molina; Mi-Sook Seo; Alexander V. Virovets; William Clegg; A. Geoffrey Sykes; Inorganic Chemistry 40 (2001) 6598–6603; doi:10.1021/ic010362n

data_4320689
_publ_contact_author
;
         Prof. A. Geoffrey Sykes FRS
         Department of Chemistry,
         The University of Newcastle upon Tyne,
         Newcastle upon Tyne NE1 7RU, UK
;
_publ_contact_author_email       a.g.sykes@ncl.ac.uk
_publ_contact_author_fax         '44 191 2611182'
_publ_contact_author_phone       '44 191 2226700'
_publ_section_title
;
 Preparation, Structure, and Properties of the Corner-Shared Double Cubes
 [Mo6HgQ8(H2O)18]8+ (Q = S, Se) and Tungsten Analogues
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6598
_journal_page_last               6603
_journal_paper_doi               10.1021/ic010362n
_journal_volume                  40
_journal_year                    2001
_chemical_formula_structural
'(Hg Mo6 S8 Cl4 (H2 O)14) (C36 H36 N24 O12) Cl4 . 14(H2 O)'
_chemical_formula_sum            'C36 H92 Cl8 Hg Mo6 N24 O40 S8'
_chemical_formula_weight         2817.65
_chemical_name_common            none
_chemical_name_systematic
;
Bis(heptaaquadichloro-tetrakis(mu3-sulphido)-
trimolybdenium)-mercury(0) tetrachloride cucurbituril adduct
tetradecahydrate.
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 102.1280(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.7750(10)
_cell_length_b                   18.2980(10)
_cell_length_c                   15.2680(10)
_cell_measurement_reflns_used    6462
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.1
_cell_measurement_theta_min      2.3
_cell_volume                     4581.9(5)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0644
_diffrn_reflns_av_sigmaI/netI    0.1117
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18445
_diffrn_reflns_theta_full        28.59
_diffrn_reflns_theta_max         28.59
_diffrn_reflns_theta_min         1.36
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.974
_exptl_absorpt_correction_T_max  0.8015
_exptl_absorpt_correction_T_min  0.6461
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    2.042
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.087
_refine_diff_density_min         -1.280
_refine_diff_density_rms         0.173
_refine_ls_extinction_coef       0.00029(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   0.957
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5645
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1197
_reflns_number_gt                3399
_reflns_number_total             5645
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010362n_1.cif
_cod_data_source_block           compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4320689