Supramolecular Assemblies Based on Cucurbituril Adducts of Hydrogen-Bonded Cubane-Type Molybdenum-Nickel Sulfide Aqua Complexes
Vladimir P. Fedin; Volker Gramlich; Michael Wörle; Thomas Weber; Inorganic Chemistry 40 (2001) 1074–1077; doi:10.1021/ic001034a

data_4319321
_publ_contact_author
;
 Weber, Thomas
 Laboratory for Technical Chemistry,
 Universit\"atstr. 6
 CH-8092 Z\"urich,
 Switzerland
;
_publ_contact_author_email       thomas.weber@tech.chem.ethz.ch
_publ_contact_author_fax         41(1)6321162
_publ_contact_author_phone       41(1)6323043
_publ_section_title
;
 Supramolecular Assemblies Based on Cucurbituril Adducts of
 Hydrogen-Bonded Cubane-Type Molybdenum-Nickel Sulfide Aqua Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1074
_journal_page_last               1077
_journal_paper_doi               10.1021/ic001034a
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C36 H76 Cl4 Mo3 N24 Ni O32 S4'
_chemical_formula_weight         1973.78
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 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                 103.35(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.579(3)
_cell_length_b                   14.405(2)
_cell_length_c                   24.407(4)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      46.6
_cell_measurement_theta_min      3
_cell_volume                     7040(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SMART PLATFORM, CCD Detector'
_diffrn_measurement_method       '\w 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  0.0965
_diffrn_reflns_av_sigmaI/netI    0.1029
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19703
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    1.158
_exptl_absorpt_correction_T_max  0.9131
_exptl_absorpt_correction_T_min  0.6673
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Program Sadabs, G. Sheldrick, 1997, G\"ottingen'
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.862
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4008
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.387
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         7389
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0803
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1253P)^2^+74.9989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2057
_refine_ls_wR_factor_ref         0.2237
_reflns_number_gt                5901
_reflns_number_total             7389
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001034a_1.cif
_cod_data_source_block           1
_cod_original_cell_volume        7039.9(18)
_cod_database_code               4319321