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_4113970
_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 H)4 C N C O),3(C H2 Cl2)
;
_chemical_formula_sum            'C101 H100 Cl6 Mo4 N14 O14'
_chemical_formula_weight         2330.41
_chemical_name_common
;
 [Mo2(DAniF)3]2(mu-2,3-dioxyquinoxalinate),3(CH2Cl2)
;
_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-97
_cell_angle_alpha                72.6680(10)
_cell_angle_beta                 84.6780(10)
_cell_angle_gamma                72.6560(10)
_cell_formula_units_Z            1
_cell_length_a                   12.5325(8)
_cell_length_b                   14.3280(9)
_cell_length_c                   15.3801(10)
_cell_measurement_reflns_used    9755
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.36
_cell_volume                     2516.4(3)
_computing_cell_refinement       'SMART V. 6.02'
_computing_data_collection       'SMART V. 5.059'
_computing_data_reduction        'SMART V. 6.02'
_computing_molecular_graphics    'SHELXTL V. 5.03 (Siemens, 1994)'
_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 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0137
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13055
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.12
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  0.7877
_exptl_absorpt_correction_T_min  0.6341
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       block
_exptl_crystal_F_000             1186
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.131
_refine_diff_density_min         -1.039
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         8667
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+9.2222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1435
_reflns_number_gt                7858
_reflns_number_total             8667
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ja0358044si20030425_064324_4.cif
_cod_data_source_block
'[Mo2(DAniF)3]2(mu-2,3-dioxyquinoxalinate),3(CH2Cl2)'
_cod_database_code               4113970