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_4113972
_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 Mo2]2 (O C N (C H) N C O (C H))
;
_chemical_formula_structural
;
 [Mo2(DAniF)3]2(mu-4,6-dioxypyrimidinate)
;
_chemical_formula_sum            'C94 H92 Mo4 N14 O14'
_chemical_formula_weight         2025.58
_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                 90.717(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.613(2)
_cell_length_b                   24.806(4)
_cell_length_c                   33.840(2)
_cell_measurement_reflns_used    248
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.1
_cell_volume                     8908(2)
_computing_cell_refinement       'MADNES (Enraf-Nonius, 1989)'
_computing_data_collection       'MADNES (Enraf-Nonius, 1989)'
_computing_data_reduction        'PROCOR (Kabsch, 1988)'
_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       'Enraf-Nonius FAST area detector'
_diffrn_measurement_method       'ellipsoid-mask fitting'
_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  0.0704
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            35898
_diffrn_reflns_theta_max         22.53
_diffrn_reflns_theta_min         1.98
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.9404
_exptl_absorpt_correction_T_min  0.7888
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             4136
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.102
_refine_ls_goodness_of_fit_obs   1.076
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1094
_refine_ls_number_reflns         11400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.148
_refine_ls_restrained_S_obs      1.076
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_obs          0.0524
_refine_ls_shift/esd_max         -0.023
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+40.4575P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1430
_refine_ls_wR_factor_obs         0.1176
_reflns_number_observed          9030
_reflns_number_total             11461
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja0358044si20030425_064324_6.cif
_cod_data_source_block           '[Mo2(DAniF)3]2(mu-4,6-dioxypyrimidinate)(2)'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+40.4575P] 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^)+(0.0420P)^2^+40.4575P] 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        8908.6(21)
_cod_database_code               4113972