Bright orange/red-emitting rhodium(iii) and iridium(iii) complexes: tridentate N^C^N-cyclometallating ligands lead to high luminescence efficiencies.
Gildea, Louise F.; Batsanov, Andrei S.; Williams, J. A. Gareth; Dalton transactions (Cambridge, England : 2003) 42 (2013) 10388–10393; doi:10.1039/c3dt51211h

data_7021584
_publ_section_title
;
 Bright orange/red-emitting rhodium(iii) and iridium(iii) complexes:
 tridentate N^C^N-cyclometallating ligands lead to high luminescence
 efficiencies.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10388
_journal_page_last               10393
_journal_paper_doi               10.1039/c3dt51211h
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C35 H23 Cl Ir N3, 1.67(C H4 O), 0.67(H2 O)'
_chemical_formula_sum            'C36.67 H31 Cl Ir N3 O2.33'
_chemical_formula_weight         778.63
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_Hall           'I -2y'
_space_group_name_H-M_alt        'I 1 m 1'
_symmetry_space_group_name_Hall  'I -2y'
_symmetry_space_group_name_H-M   'I 1 m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-05-04
_audit_creation_method
;
  Olex2 1.2-alpha
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.476(13)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   10.6873(11)
_cell_length_b                   32.019(4)
_cell_length_c                   14.1789(19)
_cell_measurement_reflns_used    5305
_cell_measurement_temperature    120
_cell_measurement_theta_max      24.948
_cell_measurement_theta_min      2.497
_cell_volume                     4697.9(10)
_computing_cell_refinement       'SAINT v7.46A (Bruker, 2008)'
_computing_data_collection       'SMART v5.630 (Bruker, 2003)'
_computing_data_reduction        'SAINT v7.46A (Bruker, 2008)'
_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.
;
_computing_structure_refinement
;
SHELXL-2013/2, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122
;
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1000 area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.1076
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13063
_diffrn_reflns_point_group_measured_fraction_full 0.921
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        24.988
_diffrn_reflns_theta_max         24.988
_diffrn_reflns_theta_min         1.614
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.75
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.388
_exptl_absorpt_correction_T_max  0.4285
_exptl_absorpt_correction_T_min  0.2916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.1031 before and 0.0732 after correction.
The Ratio of minimum to maximum transmission is 0.6805.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2308
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.268
_refine_diff_density_min         -1.245
_refine_diff_density_rms         0.168
_refine_ls_abs_structure_details
;
 Flack x determined using 2363 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61), Hooft y=0.022(13).
;
_refine_ls_abs_structure_Flack   0.032(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         7756
_refine_ls_number_restraints     381
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0326P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1080
_reflns_Friedel_coverage         0.839
_reflns_Friedel_fraction_full    0.842
_reflns_Friedel_fraction_max     0.842
_reflns_number_gt                6214
_reflns_number_total             7756
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt51211h.txt
_cod_data_source_block           2b
_cod_database_code               7021584
_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, All O(H) groups
2. Restrained distances
 C4-H4 = C6-H6 = C9-H9 = C18-H18
 0.96 with sigma of 0.02
3. Others
 Fixed Sof: O3(0.5) C62(0.5) H62A(0.5) H62B(0.5) H62C(0.5)
4.a Riding coordinates:
 C5(H5), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C19(H19), C20(H20),
 C21(H21), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C32(H32),
  C33(H33), C34(H34), C35(H35), C38(H38), C42(H42), C43(H43), C44(H44),
 C45(H45), C47(H47), C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C56(H56),
  C57(H57), C58(H58), C59(H59), C60(H60A,H60B,H60C), O2(H2), C61(H61A,H61B,
 H61C), C62(H62A,H62B,H62C)
4.b Aromatic/amide H refined with riding coordinates:
 C39(H39)
;
_shelxl_version_number           2013-2