Cyclic Polyamidato Dianions as Bridges between Mo24+ Units: Synthesis, Crystal Structures, Electrochemistry, Absorption Spectra, and Electronic Structures
F. A. Cotton; James P. Donahue; Carlos A. Murillo; Lisa M. Pérez; Rongmin Yu; Journal of the American Chemical Society 125 (2003) 8900–8910; doi:10.1021/ja0358044

data_4113971
_publ_section_title
;
 Cyclic Polyamidato Dianions as Bridges between Mo24+ Units: Synthesis,
 Crystal Structures, Electrochemistry, Absorption Spectra, and Electronic
 Structures
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8900
_journal_page_last               8910
_journal_paper_doi               10.1021/ja0358044
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety
;
 [[(H3 C O C6 H4 N)2 C H]3 Mo2]2 (O C N C (C N) C (C N) N C O) , 2(C H2 Cl2)
 , (C6 H14)
;
_chemical_formula_sum            'C102 H104 Cl4 Mo4 N16 O15'
_chemical_formula_weight         2319.57
_chemical_name_common
;
 [Mo2(DAniF)3]2(mu-2,3-dicyano-5,6-dioxypyrazinate),2(CH2Cl2),Et2O
;
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.131(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.581(3)
_cell_length_b                   17.679(3)
_cell_length_c                   18.365(3)
_cell_measurement_reflns_used    5776
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      22.55
_cell_measurement_theta_min      2.25
_cell_volume                     5054.5(15)
_computing_cell_refinement       'SAINT V. 6.02'
_computing_data_collection       'SMART V. 5.059'
_computing_data_reduction        'SAINT V. 6.02'
_computing_molecular_graphics    'SHELXTL (Siemens, 1996)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Bruker SMART 1000'
_diffrn_measurement_device_type  'area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20452
_diffrn_reflns_theta_full        22.56
_diffrn_reflns_theta_max         22.56
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_T_max  0.9188
_exptl_absorpt_correction_T_min  0.7244
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       block
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.049
_refine_diff_density_min         -1.086
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         6625
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+43.3463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1547
_refine_ls_wR_factor_ref         0.1668
_reflns_number_gt                5343
_reflns_number_total             6625
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ja0358044si20030425_064324_5.cif
_cod_data_source_block
'[Mo2(DAniF)3]2(mu-2,3-dicyano-5,6-dioxypyrazinate),2(CH2Cl2),Et2O'
_cod_original_cell_volume        5054.8(16)
_cod_database_code               4113971