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_4113703
_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 Cl (H3 C C N)] . (C H2 Cl2)0.5
;
_chemical_formula_sum            'C47.5 H49 Cl2 Mo2 N7 O6'
_chemical_formula_weight         1076.72
_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                78.960(3)
_cell_angle_beta                 72.683(3)
_cell_angle_gamma                72.767(3)
_cell_formula_units_Z            2
_cell_length_a                   11.4243(19)
_cell_length_b                   12.827(2)
_cell_length_c                   18.004(3)
_cell_measurement_reflns_used    5545
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.482
_cell_measurement_theta_min      2.385
_cell_volume                     2390.1(7)
_computing_cell_refinement       'SAINT V. 6.02'
_computing_data_collection       'SMART V. 5.059'
_computing_data_reduction        'SAINT 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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10791
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.99
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.692
_exptl_absorpt_correction_T_max  0.807
_exptl_absorpt_correction_T_min  0.601
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       block
_exptl_crystal_F_000             1098
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.43
_refine_diff_density_max         1.479
_refine_diff_density_min         -1.179
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         6157
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+8.4039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1316
_reflns_number_gt                5335
_reflns_number_total             6157
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja029101isi20030123_021228_10.cif
_cod_data_source_block           xl
_cod_original_formula_sum        'C47.50 H49 Cl2 Mo2 N7 O6'
_cod_database_code               4113703