A facile color-tuning strategy for constructing a library of Ir(iii) complexes with fine-tuned phosphorescence from bluish green to red using a synergetic substituent effect of -OCH3 and -CN at only the C-ring of C/Ν ligand
Yan Jiao; Ming Li; Ning Wang; Tao Lu; Liang Zhou; Yan Huang; Zhiyun Lu; Daibing Luo; Xuemei Pu; Journal of Materials Chemistry C 4 (2016) 4269–4277; doi:10.1039/C6TC00153J

data_7234727
_publ_section_title
;
 A facile color-tuning strategy for constructing a library of Ir(iii)
 complexes with fine-tuned phosphorescence from bluish green to red using
 a synergetic substituent effect of -OCH3 and -CN at only the C-ring of
 C/\N ligand
;
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              4269
_journal_page_last               4277
_journal_paper_doi               10.1039/C6TC00153J
_journal_volume                  4
_journal_year                    2016
_chemical_formula_moiety         'C45 H31 Ir N6 O2'
_chemical_formula_sum            'C45 H31 Ir N6 O2'
_chemical_formula_weight         879.96
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90.118(3)
_cell_angle_beta                 97.538(3)
_cell_angle_gamma                95.431(2)
_cell_formula_units_Z            4
_cell_length_a                   13.2010(4)
_cell_length_b                   15.9948(4)
_cell_length_c                   19.2170(7)
_cell_measurement_reflns_used    7129
_cell_measurement_temperature    143.00(10)
_cell_measurement_theta_max      23.4470
_cell_measurement_theta_min      3.1500
_cell_volume                     4004.1(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      143.00(10)
_diffrn_detector_area_resol_mean 16.0874
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -35.00    5.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3611   57.0000  -30.0000 40

  2 omega  -23.00    4.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3611  -99.0000    0.0000 27

  3 omega  -23.00   24.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3611  -99.0000  -60.0000 47

  4 omega  -39.00   49.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3611   57.0000 -150.0000 88

  5 omega   36.00   93.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1580  178.0000  -30.0000 57

  6 omega    0.00   45.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1580   57.0000 -180.0000 45

  7 omega   -1.00   88.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1580   57.0000   90.0000 89

  8 omega  -25.00   84.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1580   19.0000   30.0000 109
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0039885000
_diffrn_orient_matrix_UB_12      0.0031905000
_diffrn_orient_matrix_UB_13      0.0363413000
_diffrn_orient_matrix_UB_21      -0.0481819000
_diffrn_orient_matrix_UB_22      0.0163871000
_diffrn_orient_matrix_UB_23      -0.0080533000
_diffrn_orient_matrix_UB_31      -0.0250468000
_diffrn_orient_matrix_UB_32      -0.0413039000
_diffrn_orient_matrix_UB_33      -0.0009771000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_unetI/netI     0.1175
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38944
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.811
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.379
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.912
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     876
_refine_ls_number_reflns         16322
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.1133
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0557P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1430
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9905
_reflns_number_total             16322
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            J-Mater-Chem-C-2016-4-4269.cif
_cod_data_source_block           130924_s2_lm
_cod_database_code               7234727
_shelx_estimated_absorpt_t_max   0.551
_shelx_estimated_absorpt_t_min   0.431
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C85B-C90B
 1.4 with sigma of 0.02
 C90B-C89B
 1.4 with sigma of 0.02
 C89B-C88B
 1.4 with sigma of 0.02
 C88B-C87B
 1.4 with sigma of 0.02
 C87B-C86B
 1.4 with sigma of 0.02
 C85B-C86B
 1.4 with sigma of 0.02
 C90B-C88B
 2.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C90A) = Uanis(C60) = Uanis(C90B)
Uanis(C89A) = Uanis(C61) = Uanis(C89B)
Uanis(C88A) = Uanis(C86A) = Uanis(C88B) = Uanis(C25) = Uanis(C86B)
Uanis(C87B) = Uanis(C85A) = Uanis(C87A) = Uanis(C59) = Uanis(C85B)
Uanis(O1) = Uanis(O2) = Uanis(O3) = Uanis(O4)
Uanis(C46) = Uanis(C48) = Uanis(C49) = Uanis(C50) = Uanis(C47) = Uanis(C1) =
Uanis(C2) = Uanis(C3) = Uanis(C5) = Uanis(C4)
4. Others
 Sof(C85B)=Sof(C86B)=Sof(H86B)=Sof(C87B)=Sof(H87B)=Sof(C88B)=Sof(H88B)=
 Sof(C89B)=Sof(H89B)=Sof(C90B)=Sof(H90B)=1-FVAR(1)
 Sof(C85A)=Sof(C90A)=Sof(H90A)=Sof(C89A)=Sof(H89A)=Sof(C88A)=Sof(H88A)=
 Sof(C87A)=Sof(H87A)=Sof(C86A)=Sof(H86A)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C20(H20), C22(H22), C23(H23), C27(H27), C28(H28), C29(H29),
  C30(H30), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40),
 C42(H42), C43(H43), C47(H47), C52(H52), C53(H53), C54(H54), C55(H55), C59(H59),
  C60(H60), C61(H61), C62(H62), C63(H63), C65(H65), C67(H67), C68(H68),
 C72(H72), C73(H73), C74(H74), C75(H75), C79(H79), C81(H81), C82(H82),
 C90A(H90A), C89A(H89A), C88A(H88A), C87A(H87A), C86A(H86A), C86B(H86B),
 C87B(H87B), C88B(H88B), C89B(H89B), C90B(H90B)
5.b Fitted hexagon refined as free rotating group:
 C85A(C90A,C89A,C88A,C87A,C86A)
5.c Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C5(H5a,H5b,H5c), C49(H49a,H49b,H49c), C50(H50a,H50b,H50c)
;
_shelx_res_checksum              51859
_shelx_hkl_checksum              2286