Polynuclear osmium–dioxolene complexes: comparison of electrochemical and spectroelectrochemical properties with those of their ruthenium analogues
Barthram, Anita M.; Reeves, Zöe R.; Jeffery, John C.; Ward, Michael D.; Journal of the Chemical Society, Dalton Transactions  (2000) 3162–; doi:10.1039/b004858p

data_7009964
_publ_section_title
;
 Polynuclear osmium--dioxolene complexes: comparison of electrochemical
 and spectroelectrochemical properties with those of their ruthenium
 analogues
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3162
_journal_paper_doi               10.1039/b004858p
_journal_year                    2000
_chemical_formula_sum            'C26 H20 F6 N4 O2 Os P'
_chemical_formula_weight         755.63
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                90.000(11)
_cell_angle_beta                 104.011(10)
_cell_angle_gamma                90.000(14)
_cell_formula_units_Z            4
_cell_length_a                   11.8056(14)
_cell_length_b                   14.869(3)
_cell_length_c                   14.909(3)
_cell_measurement_temperature    173(2)
_cell_volume                     2539.2(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Siemens SMART Area Detector'
_diffrn_measurement_method       '\w rotation with narrow frames (0.3 degrees)'
_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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8036
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    5.163
_exptl_absorpt_correction_T_max  0.60
_exptl_absorpt_correction_T_min  0.08
_exptl_absorpt_correction_type   'Empirical, pseudo-azimuthal scan (SADABS)'
_exptl_crystal_colour            'dark green '
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0224
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0549
_reflns_number_gt                2647
_reflns_number_total             2910
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004858p.txt
_cod_data_source_block           sad
_cod_original_cell_volume        2539.3(7)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7009964