Divalent Osmium Complexes: Synthesis, Characterization, Strong Red Phosphorescence, and Electrophosphorescence
Brenden Carlsen; Gregory D. Phelan; Werner Kaminsky; Larry R. Dalton; Xuezhong Jiang; Sen Liu; Alex K-Y. Jen; Journal of the American Chemical Society 124 (2002) 14162–14172; doi:10.1021/ja0176705

data_4115329
_publ_contact_author
;
    Larry R. Dalton
    Department of Chemistry, Box 351700
    University of Washington
    Seattle, WA 98195
    USA
;
_publ_contact_author_email       dalton@chem.washington.edu
_publ_section_title
;
 Divalent Osmium Complexes: Synthesis, Characterization, Strong Red
 Phosphorescence, and Electrophosphorescence
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14162
_journal_page_last               14172
_journal_paper_doi               10.1021/ja0176705
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         'C45 H33 As Br2 Cl3 N2 O3 Os0.50 S'
_chemical_formula_sum            'C45 H33 As Br2 Cl3 N2 O3 Os0.5 S'
_chemical_formula_weight         1117.98
_chemical_name_common            Comple12
_chemical_name_systematic
; 
Comple12
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5150(2)
_cell_length_b                   26.0710(3)
_cell_length_c                   11.1480(7)
_cell_measurement_reflns_used    903
_cell_measurement_temperature    130(2)
_cell_volume                     4218.6(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w 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  0.061
_diffrn_reflns_av_sigmaI/netI    0.0984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8380
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         4.09
_exptl_absorpt_coefficient_mu    4.481
_exptl_absorpt_correction_T_max  0.6628
_exptl_absorpt_correction_T_min  0.4127
_exptl_absorpt_correction_type   Denzo2000
_exptl_absorpt_process_details   'numerical, using redundancy'
_exptl_crystal_colour            'Dark Red'
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2196
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.379
_refine_diff_density_min         -1.132
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.016(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    'H atoms riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         8380
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0666P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                6225
_reflns_number_total             8380
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0176705-2_s2_3.cif
_cod_data_source_block           Comple12
_cod_original_formula_sum        'C45 H33 As Br2 Cl3 N2 O3 Os0.50 S'
_cod_database_code               4115329