Mononuclear and Dinuclear Complexes of Dibenzoeilatin: Synthesis, Structure, and Electrochemical and Photophysical Properties
Sheba D. Bergman; Israel Goldberg; Andrea Barbieri; Francesco Barigelletti; Moshe Kol; Inorganic Chemistry 43 (2004) 2355–2367; doi:10.1021/ic0354062

data_4310807
_publ_section_title
;
 Mononuclear and Dinuclear Complexes of Dibenzoeilatin: Synthesis,
 Structure, and Electrochemical and Photophysical Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2355
_journal_page_last               2367
_journal_paper_doi               10.1021/ic0354062
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C66.5 H50 F12 N10 Os P2'
_chemical_formula_weight         1469.30
_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                79.2050(4)
_cell_angle_beta                 77.5380(4)
_cell_angle_gamma                63.5320(6)
_cell_formula_units_Z            2
_cell_length_a                   13.68300(10)
_cell_length_b                   14.16800(10)
_cell_length_c                   17.4750(2)
_cell_measurement_reflns_used    12001
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      29.91
_cell_measurement_theta_min      1.77
_cell_volume                     2945.04(5)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        Denzo
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    DIRDIF-96
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean '56 microns'
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. Phi & 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  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30257
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    2.311
_exptl_absorpt_correction_T_max  0.8367
_exptl_absorpt_correction_T_min  0.5440
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing (1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin needles'
_exptl_crystal_F_000             1466
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.468
_refine_diff_density_min         -1.317
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         13603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.357
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+13.4542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1046
_reflns_number_gt                12001
_reflns_number_total             13603
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0354062si20040209_095757_1.cif
_cod_data_source_block           mk83
_cod_original_cell_volume        2945.05(5)
_cod_original_formula_sum        'C66.50 H50 F12 N10 Os P2'
_cod_database_code               4310807