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_4319322
_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            'C41 H87 Cl5 Mo3 N25 Ni O34.5 S4'
_chemical_formula_weight         2134.38
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.53(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.819(21)
_cell_length_b                   14.956(9)
_cell_length_c                   24.148(12)
_cell_measurement_reflns_used    12
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     7512(10)
_computing_cell_refinement       'SIEMENS SHELXTL Plus'
_computing_data_collection       'SIEMENS SHELXTL Plus'
_computing_data_reduction        'SIEMENS SHELXTL Plus'
_computing_molecular_graphics    SHELXLTL-Plus
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'SYNTEX P21 4-circle diffractometer'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2073
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5639
_diffrn_reflns_theta_max         18.54
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 120
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    1.130
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark_green
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_description       prism
_exptl_crystal_F_000             4348
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.758
_refine_ls_goodness_of_fit_obs   1.172
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         5639
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.763
_refine_ls_restrained_S_obs      1.182
_refine_ls_R_factor_all          0.1128
_refine_ls_R_factor_obs          0.0548
_refine_ls_shift/esd_max         0.059
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1423
_refine_ls_wR_factor_obs         0.1285
_reflns_number_observed          2289
_reflns_number_total             5639
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic001034a_2.cif
_cod_data_source_block           vf455
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7511.6(96)
_cod_original_formula_sum        'C41 H87 Cl5 Mo3 N25 Ni O34.50 S4'
_cod_database_code               4319322