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_4319374
_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 H2 C H2 C O2)
 . (C H2 Cl2)2 . (C6 H14)2 . (H2 O)0.5
;
_chemical_formula_structural
;
 [Mo2(DAniF)3]2(mu-O2CCH2CH2CO2).2(CH2Cl2).2(C6H14).0.5(H2O)
;
_chemical_formula_sum            'C108 H127 Cl4 Mo4 N12 O16.5'
_chemical_formula_weight         2382.78
_chemical_melting_point          ?
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 104.360(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.792(2)
_cell_length_b                   19.467(2)
_cell_length_c                   31.665(3)
_cell_measurement_reflns_used    584
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      24.8
_cell_measurement_theta_min      2.3
_cell_volume                     10624.7(19)
_computing_cell_refinement       'SAINT V. 4.035'
_computing_data_collection       'SMART V. 4.043'
_computing_data_reduction        'SAINT V. 4.035'
_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       'Bruker SMART 1000'
_diffrn_measurement_method       omega-scans
_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  0.0614
_diffrn_reflns_av_sigmaI/netI    0.0737
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            53888
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.20
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       yellow
_exptl_crystal_F_000             4908
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.013
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.063
_refine_ls_goodness_of_fit_obs   1.139
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1314
_refine_ls_number_reflns         18574
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.083
_refine_ls_restrained_S_obs      1.138
_refine_ls_R_factor_all          0.1191
_refine_ls_R_factor_obs          0.0693
_refine_ls_shift/esd_max         3.343
_refine_ls_shift/esd_mean        0.023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0878P)^2^+25.7193P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2021
_refine_ls_wR_factor_obs         0.1660
_reflns_number_observed          11742
_reflns_number_total             18637
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000934o_08.cif
_cod_data_source_block
'[Mo2(DAniF)3]2(mu-O2CCH2CH2CO2).2(CH2Cl2).2(C6H14).0.5(H2O)'
_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 (96 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 (308
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 (50 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
(163 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^)+(0.0878P)^2^+25.7193P] 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^)+(0.0878P)^2^+25.7193P] 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        10624.7(17)
_cod_original_formula_sum        'C108 H127 Cl4 Mo4 N12 O16.50'
_cod_database_code               4319374