Polyunsaturated Dicarboxylate Tethers Connecting Dimolybdenum Redox and Chromophoric Centers: Syntheses, Structures, and Electrochemistry
F. Albert Cotton; James P. Donahue; Carlos A. Murillo; Journal of the American Chemical Society 125 (2003) 5436–5450; doi:10.1021/ja029101i

data_4113704
_publ_section_title
;
 Polyunsaturated Dicarboxylate Tethers Connecting Dimolybdenum Redox and
 Chromophoric Centers: Syntheses, Structures, and Electrochemistry
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5436
_journal_page_last               5450
_journal_paper_doi               10.1021/ja029101i
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety
;
[Mo2 (H3 C O C6 H4 N)2 C H)3 (O2 C C C H)] . (C H2 Cl2)0.5 .
(C6 H14)0.5
;
_chemical_formula_sum            'C51.5 H54 Cl Mo2 N6 O8'
_chemical_formula_weight         1112.34
_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                101.04(3)
_cell_angle_beta                 90.23(3)
_cell_angle_gamma                93.04(3)
_cell_formula_units_Z            4
_cell_length_a                   10.527(2)
_cell_length_b                   19.057(4)
_cell_length_c                   25.424(5)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.1
_cell_volume                     4998.4(18)
_computing_cell_refinement       'MADNES (Nonius, 1989)'
_computing_data_collection       'MADNES (Nonius, 1989)'
_computing_data_reduction        'PROCOR (Kabsch, 1988)'
_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 0.899
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  '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  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            22364
_diffrn_reflns_theta_full        22.74
_diffrn_reflns_theta_max         22.74
_diffrn_reflns_theta_min         2.27
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_description       wedge
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.289
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1185
_refine_ls_number_reflns         12107
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0712
_refine_ls_shift/su_max          0.070
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0654P)^2^+42.9322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1673
_refine_ls_wR_factor_ref         0.1908
_reflns_number_gt                9607
_reflns_number_total             12107
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ja029101isi20030123_021228_11.cif
_cod_data_source_block           xl
_cod_original_cell_volume        4998.4(17)
_cod_original_formula_sum        'C51.50 H54 Cl Mo2 N6 O8'
_cod_database_code               4113704