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_4115328
_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         C70H54As2N4Os1*2C7H7SO*H2O
_chemical_formula_sum            'C84 H70 As2 N4 O7 Os S2'
_chemical_formula_weight         1651.60
_chemical_name_common            Complex3
_chemical_name_systematic
; 
 Complex3 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                90.00
_cell_angle_beta                 99.055(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.329(5)
_cell_length_b                   17.240(10)
_cell_length_c                   22.048(9)
_cell_measurement_reflns_used    1355
_cell_measurement_temperature    130(2)
_cell_volume                     6880(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        DENZO2000
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    DIRDIFF
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.892
_diffrn_measured_fraction_theta_max 0.892
_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  0.1580
_diffrn_reflns_av_sigmaI/netI    0.2920
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11576
_diffrn_reflns_theta_full        21.49
_diffrn_reflns_theta_max         21.49
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    2.931
_exptl_absorpt_correction_T_max  0.8918
_exptl_absorpt_correction_T_min  0.5648
_exptl_absorpt_correction_type   DENZO2000
_exptl_absorpt_process_details   'numerical, using redundancy'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       plate
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.218
_refine_diff_density_min         -1.355
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.896
_refine_ls_hydrogen_treatment    'H atoms riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     909
_refine_ls_number_reflns         7042
_refine_ls_number_restraints     207
_refine_ls_restrained_S_all      0.890
_refine_ls_R_factor_all          0.1780
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0840
_reflns_number_gt                3442
_reflns_number_total             7042
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0176705-2_s2_2.cif
_cod_data_source_block           Complex3
_cod_database_code               4115328