Quadridentate Bridging EO~4~^2-^ (E = S, Mo, W) Ligands and Their Role as Electronic Bridges
F. Albert Cotton; James P. Donahue; Carlos A. Murillo; Inorganic Chemistry 40 (2001) 2229–2233; doi:10.1021/ic0012470

data_4319630
_publ_section_title
;
 Quadridentate Bridging EO~4~^2-^ (E = S, Mo, W) Ligands and Their Role as
 Electronic Bridges
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2229
_journal_page_last               2233
_journal_paper_doi               10.1021/ic0012470
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety
;
 [[(H3 C O C6 H4 N)2 C H]3 Mo2]2 (S O4) . (C H2 Cl2)2 . (C6 H14)
;
_chemical_formula_structural
;
 [Mo2(DAniF)3]2(mu-SO4).2(CH2Cl2).C6H14
;
_chemical_formula_sum            'C98 H108 Cl4 Mo4 N12 O16 S'
_chemical_formula_weight         2267.58
_chemical_melting_point          ?
_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
_cell_angle_alpha                87.83(2)
_cell_angle_beta                 79.721(14)
_cell_angle_gamma                69.758(14)
_cell_formula_units_Z            2
_cell_length_a                   15.224(4)
_cell_length_b                   17.860(6)
_cell_length_c                   20.030(5)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.1
_cell_volume                     5026(3)
_computing_cell_refinement       'MADNES (Enraf-Nonius, 1989)'
_computing_data_collection       'MADNES (Enraf-Nonius, 1989)'
_computing_data_reduction        'PROCOR (Kabsch, 1988)'
_computing_molecular_graphics    'SHELXTL V.5 (Siemens, 1994)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Enraf-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  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24881
_diffrn_reflns_theta_max         22.57
_diffrn_reflns_theta_min         2.30
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.443
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.109
_refine_ls_goodness_of_fit_obs   1.093
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1212
_refine_ls_number_reflns         12608
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_restrained_S_obs      1.093
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_obs          0.0698
_refine_ls_shift/esd_max         2.353
_refine_ls_shift/esd_mean        0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0648P)^2^+45.2013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1905
_refine_ls_wR_factor_obs         0.1671
_reflns_number_observed          10579
_reflns_number_total             12661
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0012470_2.cif
_cod_data_source_block           '[Mo2(DAniF)3]2(mu-SO4).2(CH2Cl2).C6H14'
_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.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_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 (92 times).

'_geom_angle_publ_flag' value 'N'
changed to 'n' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (263
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 (46 times).

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

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^)+(0.0648P)^2^+45.2013P] 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^)+(0.0648P)^2^+45.2013P] 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        5026.0(24)
_cod_database_code               4319630