Blue Phosphorescent Zwitterionic Iridium(III) Complexes Featuring Weakly Coordinating nido-Carborane-Based Ligands.
Axtell, Jonathan C.; Kirlikovali, Kent O.; Djurovich, Peter I.; Jung, Dahee; Nguyen, Vinh T.; Munekiyo, Brian; Royappa, A. Timothy; Rheingold, Arnold L.; Spokoyny, Alexander M.; Journal of the American Chemical Society 138 (2016) 15758–15765; doi:10.1021/jacs.6b10232

data_4131149
_publ_section_title
;
 Blue Phosphorescent Zwitterionic Iridium(III) Complexes Featuring Weakly
 Coordinating nido-Carborane-Based Ligands.
;
_journal_issue                   48
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15758
_journal_page_last               15765
_journal_paper_doi               10.1021/jacs.6b10232
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C30 H33 B9 Ir N3, 0.25(C H2 Cl2)'
_chemical_formula_sum            'C30.25 H33.5 B9 Cl0.5 Ir N3'
_chemical_formula_weight         746.31
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-02-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                77.255(5)
_cell_angle_beta                 82.784(5)
_cell_angle_gamma                83.833(5)
_cell_formula_units_Z            4
_cell_length_a                   12.823(2)
_cell_length_b                   13.237(2)
_cell_length_c                   18.560(3)
_cell_measurement_reflns_used    9059
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.508
_cell_measurement_theta_min      2.263
_cell_volume                     3038.0(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            97521
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_min         1.131
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.467
_exptl_absorpt_correction_T_max  0.0949
_exptl_absorpt_correction_T_min  0.0557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0911 before and 0.0786 after correction.
The Ratio of minimum to maximum transmission is 0.5869.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       block
_exptl_crystal_F_000             1466
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     884
_refine_ls_number_reflns         13937
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0230
_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^)+(0.0210P)^2^+2.3392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0591
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12401
_reflns_number_total             13937
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b10232_si_002.cif
_cod_data_source_block           2b
_cod_original_cell_volume        3038.2(9)
_cod_original_formula_sum        'C30.25 H33.50 B9 Cl0.50 Ir N3'
_cod_database_code               4131149
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: Cl1(0.5) C31(0.5) H31A(0.5) H31B(0.5) Cl2(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B)
3.b Aromatic/amide H refined with riding coordinates:
 C24A(H24A), C10(H10), C7A(H7A), C19(H19), C29A(H29A), C6A(H6A), C5A(H5A),
 C16(H16), C19A(H19A), C7(H7), C17(H17), C5(H5), C18(H18), C13A(H13A), C8(H8),
 C6(H6), C18A(H18A), C27A(H27A), C22(H22), C11A(H11A), C12A(H12A), C17A(H17A),
 C30A(H30A), C21A(H21A), C22A(H22A), C8A(H8A), C16A(H16A), C21(H21), C11(H11),
 C13(H13), C24(H24), C28A(H28A), C23(H23), C12(H12), C30(H30), C10A(H10A),
 C27(H27), C28(H28), C23A(H23A), C29(H29)
3.c Idealised Me refined as rotating group:
 C1(H1B,H1C,H1D), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              14147
_shelx_hkl_checksum              34636
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id KK-2-020
_olex2_submission_special_instructions 'No special instructions were received'