The Simplest Supramolecular Complexes Containing Pairs of Mo2(formamidinate)3 Units Linked with Various Dicarboxylates: Preparative Methods, Structures, and Electrochemistry
F. Albert Cotton; James P. Donahue; Chun Lin; Carlos A. Murillo; Inorganic Chemistry 40 (2001) 1234–1244; doi:10.1021/ic000934o

data_4319370
_publ_section_title
;
 The Simplest Supramolecular Complexes Containing Pairs of
 Mo2(formamidinate)3 Units Linked with Various Dicarboxylates: Preparative
 Methods, Structures, and Electrochemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1234
_journal_page_last               1244
_journal_paper_doi               10.1021/ic000934o
_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 (O2 C C6 F4 C O2)
 . (C H2 Cl2)2 . (C6 H14)
;
_chemical_formula_structural
;
 [Mo2(DAniF)3]2(mu-O2CC6F4CO2).2(CH2Cl2).(C6H14)
;
_chemical_formula_sum            'C106 H108 Cl4 F4 Mo4 N12 O16'
_chemical_formula_weight         2407.60
_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                76.650(10)
_cell_angle_beta                 79.610(10)
_cell_angle_gamma                87.630(10)
_cell_formula_units_Z            1
_cell_length_a                   9.7910(10)
_cell_length_b                   15.756(2)
_cell_length_c                   18.090(3)
_cell_measurement_reflns_used    225
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.1
_cell_volume                     2670.8(6)
_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  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13257
_diffrn_reflns_theta_max         22.53
_diffrn_reflns_theta_min         2.23
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.057
_refine_ls_goodness_of_fit_obs   1.057
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         6661
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.079
_refine_ls_restrained_S_obs      1.059
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_obs          0.0676
_refine_ls_shift/esd_max         0.260
_refine_ls_shift/esd_mean        0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0860P)^2^+17.0794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1875
_refine_ls_wR_factor_obs         0.1667
_reflns_number_observed          5555
_reflns_number_total             6668
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000934o_04.cif
_cod_data_source_block
'[Mo2(DAniF)3]2(mu-O2CC6F4CO2).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 (55 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 (75
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 (30 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
(62 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^)+(0.0860P)^2^+17.0794P] 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^)+(0.0860P)^2^+17.0794P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4319370