Supramolecular Squares with Mo24+ Corners
F. Albert Cotton; Chun Lin; Carlos A. Murillo; Inorganic Chemistry 40 (2001) 478–484; doi:10.1021/ic001016t

data_4319220
_publ_section_title
;
 Supramolecular Squares with Mo24+ Corners
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              478
_journal_page_last               484
_journal_paper_doi               10.1021/ic001016t
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety
'[Mo2(DAniF)2]4(O2CPhPhCO2)4(0.1CH2Cl2)(0.5CH3CN)'
_chemical_formula_sum            'C177.1 H153.7 Cl0.2 Mo8 N16.5 O32'
_chemical_formula_weight         3799.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                61.909(2)
_cell_angle_beta                 81.464(2)
_cell_angle_gamma                84.454(2)
_cell_formula_units_Z            2
_cell_length_a                   12.394(1)
_cell_length_b                   28.572(2)
_cell_length_c                   30.336(3)
_cell_measurement_reflns_used    3557
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      22.45
_cell_measurement_theta_min      2.19
_cell_volume                     9367.8(14)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XP (Siemens, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART area detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2181
_diffrn_reflns_av_sigmaI/netI    0.4523
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            42921
_diffrn_reflns_theta_full        22.55
_diffrn_reflns_theta_max         22.55
_diffrn_reflns_theta_min         1.66
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3854
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.282
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1046
_refine_ls_number_reflns         24467
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.3454
_refine_ls_R_factor_gt           0.1274
_refine_ls_shift/su_max          0.021
_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          0.2210
_refine_ls_wR_factor_ref         0.3063
_reflns_number_gt                6862
_reflns_number_total             24467
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001016t_4.cif
_cod_data_source_block           cmpd_4
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_geom_angle_publ_flag' value 'Y' changed to 'y'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (80
times).

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (36 times).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'C177.10 H153.70 Cl0.20 Mo8 N16.50 O32'
_cod_database_code               4319220