Rhenium-Based Molecular Rectangles as Frameworks for Ligand-Centered Mixed Valency and Optical Electron Transfer
Peter H. Dinolfo; Mary Elizabeth Williams; Charlotte L. Stern; Joseph T. Hupp; Journal of the American Chemical Society 126 (2004) 12989–13001; doi:10.1021/ja0473182

data_4113028
_publ_section_title
;
 Rhenium-Based Molecular Rectangles as Frameworks for Ligand-Centered
 Mixed Valency and Optical Electron Transfer
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12989
_journal_page_last               13001
_journal_paper_doi               10.1021/ja0473182
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety
'Re4 C60 H32 N12 O12, 3(C4 H8 O), C3 H6 O0.75'
_chemical_formula_sum            'C75 H62 N12 O15.75 Re4'
_chemical_formula_weight         2128.194
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.262(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.3741(10)
_cell_length_b                   48.753(4)
_cell_length_c                   24.198(2)
_cell_measurement_temperature    153(2)
_cell_volume                     14574(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_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  0.2095
_diffrn_reflns_av_sigmaI/netI    0.2201
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       64
_diffrn_reflns_limit_k_min       -63
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            134544
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         0.94
_exptl_absorpt_coefficient_mu    6.699
_exptl_absorpt_correction_T_max  0.7601
_exptl_absorpt_correction_T_min  0.5169
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_description       block
_exptl_crystal_F_000             8176
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.044
_refine_diff_density_max         2.772
_refine_diff_density_min         -2.034
_refine_diff_density_rms         0.281
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1945
_refine_ls_number_reflns         34953
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.1801
_refine_ls_R_factor_gt           0.0783
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1490
_reflns_number_gt                17392
_reflns_number_total             34953
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0473182si20040521_054757.cif
_cod_data_source_block           rectangle_1
_cod_original_cell_volume        14575(2)
_cod_database_code               4113028