Synthesis and Structure of Cuboctahedral and Anticuboctahedral Cages Containing 12 Quadruply Bonded Dimolybdenum Units
Ke, Yanxiong; Collins, David J.; Zhou, Hong-Cai; Inorganic Chemistry 44 (2005) 4154–4156; doi:10.1021/ic050460z

data_4331524
_publ_section_title
;
 Synthesis and Structure of Cuboctahedral and Anticuboctahedral Cages
 Containing 12 Quadruply Bonded Dimolybdenum Units
;
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4154
_journal_page_last               4156
_journal_paper_doi               10.1021/ic050460z
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'Mo2 2(C12 H12 O4) (C5 H5 N)'
_chemical_formula_sum            'C29 H29 Mo2 N O8'
_chemical_formula_weight         711.41
_chemical_melting_point          ?
_chemical_name_common            none
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_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            24
_cell_length_a                   28.8679(10)
_cell_length_b                   28.8679(10)
_cell_length_c                   42.999(3)
_cell_measurement_reflns_used    8643
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.17
_cell_volume                     35833(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0659
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            102073
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         0.85
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.444
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.638
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadas
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    0.791
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8592
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.38
_refine_diff_density_max         1.888
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         16740
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0659
_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^)+(0.1238P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1782
_refine_ls_wR_factor_ref         0.1923
_reflns_number_gt                11843
_reflns_number_total             16740
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050460zsup1.cif
_cod_data_source_block           xamd357s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Tetragonal' changed to 'tetragonal' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

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_original_sg_symbol_H-M      I4/m
_cod_database_code               4331524