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_4113969
_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         'C94 H92 Mo4 N14 O14 , 4(C H2 Cl2)'
_chemical_formula_sum            'C98 H100 Cl8 Mo4 N14 O14'
_chemical_formula_weight         2365.28
_chemical_name_common
;
 [Mo2(DAniF)3]2(mu-2,3-dioxypyrazinate),4(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                71.936(2)
_cell_angle_beta                 83.479(2)
_cell_angle_gamma                71.188(2)
_cell_formula_units_Z            1
_cell_length_a                   12.4674(13)
_cell_length_b                   14.6201(15)
_cell_length_c                   15.2751(16)
_cell_measurement_reflns_used    5057
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.21
_cell_volume                     2505.3(5)
_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 (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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Bruker SMART 1000'
_diffrn_measurement_device_type  'area detector'
_diffrn_measurement_method       omega-scan
_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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10620
_diffrn_reflns_theta_full        22.54
_diffrn_reflns_theta_max         22.54
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.772
_exptl_absorpt_correction_T_max  0.9401
_exptl_absorpt_correction_T_min  0.7740
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       needle
_exptl_crystal_F_000             1202
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.121
_refine_diff_density_min         -0.960
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         6515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0870P)^2^+7.1666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1551
_reflns_number_gt                5166
_reflns_number_total             6515
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0358044si20030425_064324_3.cif
_cod_data_source_block
'[Mo2(DAniF)3]2(mu-2,3-dioxy-1,4-pyrazinate),4(CH2Cl2)'
_cod_database_code               4113969