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_4310809
_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_moiety
'(C32 H16 N4), 4(C10 H8 N2), 2(Os Cl2), 14(H2 O)'
_chemical_formula_sum            'C72 H76 Cl4 N12 O14 Os2'
_chemical_formula_weight         1855.65
_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                102.0240(7)
_cell_angle_beta                 97.4120(7)
_cell_angle_gamma                95.6780(14)
_cell_formula_units_Z            1
_cell_length_a                   9.6320(2)
_cell_length_b                   12.7620(2)
_cell_length_c                   16.0470(3)
_cell_measurement_reflns_used    7701
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.32
_cell_volume                     1896.99(6)
_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 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. Phi & Omega scan'
_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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15826
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    3.557
_exptl_absorpt_correction_T_max  0.6175
_exptl_absorpt_correction_T_min  0.4150
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelpiped
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.243
_refine_diff_density_min         -1.712
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         8687
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.171
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+3.4567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0877
_reflns_number_gt                7701
_reflns_number_total             8687
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0354062si20040209_095757_3.cif
_cod_data_source_block           mk106
_cod_database_code               4310809