Varying Electronic Structures of Diosmium Complexes from Noninnocently Behaving Anthraquinone-Derived Bis-chelate Ligands.
Mandal, Abhishek; Grupp, Anita; Schwederski, Brigitte; Kaim, Wolfgang; Lahiri, Goutam Kumar; Inorganic chemistry 54 (2015) 7936–7944; doi:10.1021/acs.inorgchem.5b01017

data_4346227
_publ_section_title
;
 Varying Electronic Structures of Diosmium Complexes from Noninnocently
 Behaving Anthraquinone-Derived Bis-chelate Ligands.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7936
_journal_page_last               7944
_journal_paper_doi               10.1021/acs.inorgchem.5b01017
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C58 H46 Cl2 N12 O10 Os2'
_chemical_formula_weight         1522.37
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                100.196(3)
_cell_angle_beta                 110.811(2)
_cell_angle_gamma                98.421(3)
_cell_formula_units_Z            2
_cell_length_a                   13.639(4)
_cell_length_b                   13.862(4)
_cell_length_c                   17.859(5)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2
_cell_measurement_theta_min      3.0
_cell_volume                     3024.9(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29119
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    4.351
_exptl_absorpt_correction_T_max  0.7803
_exptl_absorpt_correction_T_min  0.4344
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.761
_refine_diff_density_min         -1.675
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         10629
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+22.6338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1160
_reflns_number_gt                9205
_reflns_number_total             10629
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01017_si_001.cif
_cod_data_source_block           '[3](ClO4)3'
_cod_database_code               4346227