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_4319371
_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 C B10 H10 C C O2)
 . (C H2 Cl2)2.9
;
_chemical_formula_structural
;
 [Mo2(DAniF)3]2(mu-O2CCB10H10CCO2).2.9(CH2Cl2)
;
_chemical_formula_sum            'C96.9 H105.8 B10 Cl5.8 Mo4 N12 O16'
_chemical_formula_weight         2392.01
_chemical_melting_point          ?
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.760(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.7180(10)
_cell_length_b                   17.7860(10)
_cell_length_c                   20.059(2)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.1
_cell_volume                     5601.2(7)
_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  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20861
_diffrn_reflns_theta_max         22.57
_diffrn_reflns_theta_min         2.33
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_meas      ?
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.111
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.081
_refine_ls_goodness_of_fit_obs   1.018
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         7227
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.134
_refine_ls_restrained_S_obs      1.018
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_obs          0.0772
_refine_ls_shift/esd_max         -0.717
_refine_ls_shift/esd_mean        0.028
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1076P)^2^+38.6517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2412
_refine_ls_wR_factor_obs         0.1904
_reflns_number_observed          5701
_reflns_number_total             7289
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000934o_05.cif
_cod_data_source_block           '[Mo2(DAniF)3]2(mu-O2CCB10H10CCO2).2.9(CH2Cl2)'
_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 (115 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 (142
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
(83 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^)+(0.1076P)^2^+38.6517P] 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^)+(0.1076P)^2^+38.6517P] 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        'C96.90 H105.80 B10 Cl5.80 Mo4 N12 O16'
_cod_database_code               4319371