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_4113968
_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_compound_source        synthesized
_chemical_formula_moiety
;
 [[(H3 C O C6 H4 N)2 C H]3 (C O N C O N H (C H)2) Mo2],(C H2 Cl2),(C6 H14)
;
_chemical_formula_structural     '[Mo2(DAniF)3(uracilate)].(CH2Cl2).(C6H14)'
_chemical_formula_sum            'C56 H64 Cl2 Mo2 N8 O8'
_chemical_formula_weight         1239.93
_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                64.9400(10)
_cell_angle_beta                 87.2070(10)
_cell_angle_gamma                86.7980(10)
_cell_formula_units_Z            2
_cell_length_a                   11.0140(8)
_cell_length_b                   15.3541(11)
_cell_length_c                   17.8103(12)
_cell_measurement_reflns_used    5297
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.75
_cell_measurement_theta_min      2.303
_cell_volume                     2723.1(3)
_computing_cell_refinement       'SAINT 6.28A 2001'
_computing_data_collection       'SMART 5.618 2000'
_computing_data_reduction        'SAINT 6.28A 2001'
_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 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device       'Bruker SMART 1000'
_diffrn_measurement_device_type  'area detector'
_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  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19064
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.21
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.7239
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.385
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.618
_refine_diff_density_min         -1.399
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     672
_refine_ls_number_reflns         11955
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          5.103
_refine_ls_shift/su_mean         0.041
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+4.5189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1217
_refine_ls_wR_factor_ref         0.1328
_reflns_number_gt                9660
_reflns_number_total             11955
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ja0358044si20030425_064324_2.cif
_cod_data_source_block           '[Mo2(DAniF)3(uracilate)].(CH2Cl2).(C6H14)'
_cod_database_code               4113968