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_4115327
_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         'C26 H22 As2'
_chemical_formula_sum            'C26 H22 As2'
_chemical_formula_weight         484.28
_chemical_name_common            DPAENE-ligand
_chemical_name_systematic
; 
DPAENE-ligand 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 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                 117.1651(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.5920(4)
_cell_length_b                   5.6160(2)
_cell_length_c                   17.0320(6)
_cell_measurement_reflns_used    539
_cell_measurement_temperature    130(2)
_cell_volume                     1071.59(6)
_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    SIR97
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0535
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            4081
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    3.127
_exptl_absorpt_correction_T_max  0.7054
_exptl_absorpt_correction_T_min  0.2182
_exptl_absorpt_correction_type   DENZO2000
_exptl_absorpt_process_details   'numerical, using redundancy'
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       prism
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    'H atoms riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         4081
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0378P)^2^+0.8532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0872
_reflns_number_gt                3759
_reflns_number_total             4081
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0176705-2_s2_1.cif
_cod_data_source_block           DPAENEligand
_cod_database_code               4115327