New synthetic pathways to the preparation of near-blue emitting heteroleptic Ir(III)N6 coordinated compounds with microsecond lifetimes
Suraj Soman; Jennifer C. Manton; Jane L. Inglis; Yvonne Halpin; Brendan Twamley; Edwin Otten; Wesley R. Browne; Luisa De Cola; Johannes G. Vos; Mary T. Pryce; Chem.Commun. 50 (2014) 6461–; doi:10.1039/C4CC02249A

data_7113962
_publ_section_title
;
 New synthetic pathways to the preparation of near-blue emitting
 heteroleptic Ir(III)N6 coordinated compounds with microsecond lifetimes
;
_journal_name_full               Chem.Commun.
_journal_page_first              6461
_journal_paper_doi               10.1039/C4CC02249A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety
'C37 H33 Ir N8, 0.2(C14 H16), 2(C F3 O3 S), H2 O'
_chemical_formula_sum            'C41.8 H38.2 F6 Ir N8 O7 S2'
_chemical_formula_weight         1134.92
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.157(3)
_cell_angle_beta                 75.969(3)
_cell_angle_gamma                71.057(3)
_cell_formula_units_Z            2
_cell_length_a                   12.0363(11)
_cell_length_b                   13.4312(13)
_cell_length_c                   15.4313(14)
_cell_measurement_reflns_used    9800
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.308
_cell_measurement_theta_min      5.615
_cell_volume                     2253.8(4)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2007)'
_computing_molecular_graphics
;
 PLATON (Spek, 2003)
 PLUTO (Meetsma, 2008)
;
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution
;
 DIRDIF-08 (Beurskens et al., 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            63885
_diffrn_reflns_theta_full        27.26
_diffrn_reflns_theta_max         27.26
_diffrn_reflns_theta_min         2.76
_diffrn_source                   'fine-focus sealed Siemens tube'
_diffrn_source_type
;Bruker
SMART APEX CCD
diffractometer
;
_exptl_absorpt_coefficient_mu    3.138
_exptl_absorpt_correction_T_max  0.8589
_exptl_absorpt_correction_T_min  0.6337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         5.529
_refine_diff_density_min         -1.635
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         10001
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0622P)^2^+12.3180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1262
_reflns_number_gt                8862
_reflns_number_total             10001
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c4cc02249a2.cif
_cod_data_source_block           eoir
_cod_original_formula_sum        'C41.80 H38.20 F6 Ir N8 O7 S2'
_cod_database_code               7113962