Bis(arylimidazole) Iridium Picolinate Emitters and Preferential Dipole Orientation in Films.
Huckaba, Aron J.; Senes, Alessia; Aghazada, Sadig; Babaei, Azin; Meskers, Stefan C. J.; Zimmermann, Iwan; Schouwink, Pascal; Gasilova, Natalia; Janssen, René A J; Bolink, Henk J.; Nazeeruddin, Mohammad Khaja; ACS omega 3 (2018) 2673–2682; doi:10.1021/acsomega.8b00137

data_4516188
_publ_section_title
;
 Bis(arylimidazole) Iridium Picolinate Emitters and Preferential Dipole
 Orientation in Films.
;
_journal_issue                   3
_journal_name_full               'ACS omega'
_journal_page_first              2673
_journal_page_last               2682
_journal_paper_doi               10.1021/acsomega.8b00137
_journal_volume                  3
_journal_year                    2018
_chemical_formula_moiety
'C54 H58 Ir N5 O2, C54 H62 Ir N5 O2, 1.79(H2 O)'
_chemical_formula_sum            'C112 H124 Ir2 N10 O4'
_chemical_formula_weight         2058.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-11-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.641(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.0272(6)
_cell_length_b                   29.178(2)
_cell_length_c                   18.4176(14)
_cell_measurement_reflns_used    1150
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      3.0
_cell_volume                     4782.6(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      130.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            121437
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.330
_diffrn_reflns_theta_min         2.243
_exptl_absorpt_coefficient_mu    2.839
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear yellowish'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       needle
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   0.6489
_exptl_transmission_factor_min   0.2901
_refine_diff_density_max         2.451
_refine_diff_density_min         -3.863
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.520(14)
_refine_ls_extinction_coef       0.00033(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.249
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         23681
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.249
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+33.5265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.963
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                22731
_reflns_number_total             23681
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b00137_si_004.cif
_cod_data_source_block           C56H62N5O2Ir1
_cod_original_cell_volume        4782.5(6)
_cod_database_code               4516188
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.675
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.480(14)
 0.520(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C2) = Uanis(C113) = Uanis(C95)
Uanis(C73) = Uanis(C1AA) = Uanis(C0AA)
Uanis(C54) = Uanis(C55) = Uanis(C64) = Uanis(C66) = Uanis(C83) = Uanis(C109)
Uanis(C31) = Uanis(C32) = Uanis(C59) = Uanis(C89) = Uanis(C97) = Uanis(C103)
Uanis(C47) = Uanis(C56) = Uanis(C71) = Uanis(C77) = Uanis(C101) = Uanis(C149) =
Uanis(C67) = Uanis(C80) = Uanis(C96) = Uanis(N100) = Uanis(C125) = Uanis(C127)
= Uanis(C36) = Uanis(C41) = Uanis(C43) = Uanis(C45) = Uanis(C49) = Uanis(C62) =
Uanis(C76)
Uanis(C105) = Uanis(C120) = Uanis(C158) = Uanis(C82) = Uanis(C3AA) =
Uanis(C2AA) = Uanis(C3) = Uanis(C123) = Uanis(C4AA) = Uanis(C39) = Uanis(C129)
= Uanis(C137) = Uanis(C33) = Uanis(C106) = Uanis(C152) = Uanis(C21) =
Uanis(C104) = Uanis(C119)
Uanis(C67) = Uanis(C80) = Uanis(C96) = Uanis(N100) = Uanis(C125) = Uanis(C127)
Uanis(N8) = Uanis(N12) = Uanis(C16) = Uanis(C28) = Uanis(C42) = Uanis(N6) =
Uanis(N10) = Uanis(C22) = Uanis(C29) = Uanis(C50)
Uanis(N7) = Uanis(C14) = Uanis(N15) = Uanis(C20) = Uanis(C60)
Uanis(C57) = Uanis(N65) = Uanis(C81) = Uanis(C124) = Uanis(C130) = Uanis(C141)
Uanis(C11) = Uanis(C46) = Uanis(C48) = Uanis(C61) = Uanis(C72) = Uanis(C84) =
Uanis(C27) = Uanis(C35) = Uanis(C43) = Uanis(C88) = Uanis(C92) = Uanis(C93)
Uanis(C23) = Uanis(O26) = Uanis(O115)
Uanis(C98) = Uanis(C111) = Uanis(C114) = Uanis(C73) = Uanis(C1AA) = Uanis(C0AA)
Uanis(C23) = Uanis(O26) = Uanis(O115) = Uanis(C67) = Uanis(C80) = Uanis(C96) =
Uanis(N100) = Uanis(C125) = Uanis(C127)
Uanis(O24) = Uanis(C30) = Uanis(O7)
Uanis(C13) = Uanis(C38) = Uanis(C53) = Uanis(C58) = Uanis(C63) = Uanis(C74) =
Uanis(N5) = Uanis(N9) = Uanis(C17) = Uanis(C18) = Uanis(C51)
Uanis(C44) = Uanis(C79) = Uanis(C132) = Uanis(C37) = Uanis(C69) = Uanis(C108) =
Uanis(C19) = Uanis(C90) = Uanis(C5AA)
Uanis(C25) = Uanis(C34) = Uanis(C52) = Uanis(C70) = Uanis(C78) = Uanis(C94)
4. Others
 Sof(O1)=Sof(H1A)=Sof(H1B)=FVAR(1)
5.a Free rotating group:
 O1(H1A,H1B), O2(H2A,H2B)
5.b Ternary CH refined with riding coordinates:
 C2(H2), C19(H19), C21(H21), C33(H33), C37(H37), C39(H39), C44(H44), C73(H73),
 C82(H82), C105(H105), C111(H111)
5.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C16(H16), C17(H17), C22(H22), C38(H38), C42(H42), C43(H43),
 C45(H45), C46(H46), C50(H50), C51(H51), C52(H52), C53(H53), C55(H55), C56(H56),
  C57(H57), C130(H130), C124(H124), C141(H141), C59(H59), C60(H60), C61(H61),
 C62(H62), C63(H63), C64(H64), C72(H72), C74(H74), C78(H78), C80(H80), C84(H84),
  C88(H88), C89(H89), C92(H92), C93(H93), C96(H96), C97(H97), C103(H103),
 C125(H125), C127(H127), C149(H149)
5.d Fitted hexagon refined as free rotating group:
 C57(C130,C81,N65,C124,C141)
5.e Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C69(H69A,H69B,H69C), C79(H79A,H79B,H79C), C90(H90A,H90B,
 H90C), C95(H95A,H95B,H95C), C98(H98A,H98B,H98C), C104(H10D,H10E,H10F),
 C106(H10G,H10H,H10I), C108(H10A,H10B,H10C), C113(H11A,H11B,H11C), C114(H11D,
 H11E,H11F), C119(H11G,H11H,H11I), C120(H12A,H12B,H12C), C129(H12D,H12E,H12F),
 C132(H13A,H13B,H13C), C137(H13D,H13E,H13F), C152(H15A,H15B,H15C), C158(H15D,
 H15E,H15F), C1AA(H1AA,H1AB,H1AC), C3AA(H3AA,H3AB,H3AC), C0AA(H0AA,H0AB,H0AC),
 C2AA(H2AA,H2AB,H2AC), C5AA(H5AA,H5AB,H5AC)
;
_shelx_res_checksum              74037
_shelx_hkl_checksum              91743
_olex2_submission_special_instructions 'No special instructions were received'