Syntheses, Structures, and Comparison of the Photophysical Properties of Cyclometalated Iridium Complexes Containing the Isomeric 1- and 2-(2'-pyridyl)pyrene Ligands
Robert M. Edkins; Katharina Fucke; Michael J. G. Peach; Andrew G. Crawford; Todd B. Marder; Andrew Beeby; Inorganic Chemistry 52 (2013) 9842–9860; doi:10.1021/ic400819f

data_4335815
_publ_section_title
;
 Syntheses, Structures, and Comparison of the Photophysical Properties of
 Cyclometalated Iridium Complexes Containing the Isomeric 1- and
 2-(2'-pyridyl)pyrene Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9842
_journal_page_last               9860
_journal_paper_doi               10.1021/ic400819f
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C21 H13 N'
_chemical_formula_sum            'C21 H13 N'
_chemical_formula_weight         279.32
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
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  (compiled Feb 15 2011 20:38:53, GUI svn.r3494)
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
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;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
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;
  1 omega  -89.00  -61.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.0928  179.0000 -150.0000 28

  2 omega  -95.00  -61.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.0928  179.0000   60.0000 34

  3 omega  -85.00  -35.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.0928    0.0000   60.0000 50
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
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_diffrn_orient_matrix_UB_22      -0.0287384000
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_diffrn_orient_matrix_UB_31      -0.1221435000
_diffrn_orient_matrix_UB_32      0.0137647000
_diffrn_orient_matrix_UB_33      -0.0285528000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0528
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_diffrn_reflns_limit_h_min       -5
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_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9403
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.06
_diffrn_source                   'Enhance (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whitish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whitish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       prism
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.2464
_exptl_crystal_size_mid          0.0586
_exptl_crystal_size_min          0.0477
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.907
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         2637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.907
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0487P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                1628
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400819f_si_002_1.cif
_cod_data_source_block           2-pypyrH
_cod_original_cell_volume        1341.3(3)
_cod_database_code               4335815
_chemical_oxdiff_formula         'C20 H20 N5 O5'
_reflns_odcompleteness_completeness 66.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32