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_4113712
_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
' C100 H98 Mo4 N12 O16, (C6 H14), (C6 H4 Cl2)'
_chemical_formula_sum            'C112 H116 Cl2 Mo4 N12 O16'
_chemical_formula_weight         2340.83
_chemical_name_systematic
; Bis(dimolybdenum(II)(N,N'-di-p-anisylformamidinate)3)
(\m-deca-trans,trans,trans,trans-2,4,6,8-tetraene-1,10-dioate) 
mono(C~6~H~14~) mono(C~6~H~4~Cl~2~) disolvate
;
_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                98.0810(10)
_cell_angle_beta                 105.7150(10)
_cell_angle_gamma                104.3500(10)
_cell_formula_units_Z            1
_cell_length_a                   12.6901(10)
_cell_length_b                   15.0798(12)
_cell_length_c                   15.4836(12)
_cell_measurement_reflns_used    5961
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.47
_cell_volume                     2693.9(4)
_computing_cell_refinement       'SAINT V. 6.22'
_computing_data_collection       'SMART V. 5.618'
_computing_data_reduction        'SAINT V. 6.22'
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0605
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15943
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.77
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_T_max  0.9841
_exptl_absorpt_correction_T_min  0.8282
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       plate
_exptl_crystal_F_000             1202
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.261
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         9379
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.206
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+2.7802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1464
_refine_ls_wR_factor_ref         0.1703
_reflns_number_gt                6530
_reflns_number_total             9379
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ja029101isi20030123_021228_19.cif
_cod_data_source_block           xl
_cod_database_code               4113712