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

data_4319218
_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[trans-O2CCHCHCO2]4.(4.5toluene)(1.4CH2Cl2)'
_chemical_formula_sum            'C168.9 H166.8 Cl2.8 Mo8 N16 O32'
_chemical_formula_weight         3799.56
_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                62.78(1)
_cell_angle_beta                 73.09(2)
_cell_angle_gamma                77.68(2)
_cell_formula_units_Z            1
_cell_length_a                   16.922(1)
_cell_length_b                   17.570(6)
_cell_length_c                   18.129(8)
_cell_measurement_reflns_used    241
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      8.2
_cell_volume                     4565(3)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_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      273(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device       'Nonius FAST area detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_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  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20496
_diffrn_reflns_theta_full        22.54
_diffrn_reflns_theta_max         22.54
_diffrn_reflns_theta_min         1.90
_diffrn_standards_number         'None (area detector data)'
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.713
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1932
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.456
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     951
_refine_ls_number_reflns         11173
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_obs          0.0650
_refine_ls_shift/esd_max         0.015
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0743P)^2^+29.2787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1790
_refine_ls_wR_factor_obs         0.1657
_reflns_number_total             11173
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001016t_2.cif
_cod_data_source_block           cmpd_2
_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.

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

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0743P)^2^+29.2787P] 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^)+(0.0743P)^2^+29.2787P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C168.90 H166.80 Cl2.80 Mo8 N16 O32'
_cod_database_code               4319218
_reflns_number_obs               9546