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_4131147
_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 H29 B9 F4 Ir N3'
_chemical_formula_sum            'C30 H29 B9 F4 Ir N3'
_chemical_formula_weight         797.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-02-25
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.951(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.6207(17)
_cell_length_b                   10.4388(6)
_cell_length_c                   15.9363(9)
_cell_measurement_reflns_used    3253
_cell_measurement_temperature    100
_cell_measurement_theta_max      22.613
_cell_measurement_theta_min      2.400
_cell_volume                     6257.6(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (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_detector_area_resol_mean 8.0
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_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  0.0664
_diffrn_reflns_av_unetI/netI     0.0786
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19818
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.693
_diffrn_reflns_theta_max         25.693
_diffrn_reflns_theta_min         2.390
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.320
_exptl_absorpt_correction_T_max  0.2594
_exptl_absorpt_correction_T_min  0.1689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0987 before and 0.0523 after correction.
The Ratio of minimum to maximum transmission is 0.6511.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_description       plate
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.287
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         5917
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0239P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4348
_reflns_number_total             5917
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b10232_si_002.cif
_cod_data_source_block           2a
_cod_database_code               4131147
_shelx_estimated_absorpt_t_max   0.583
_shelx_estimated_absorpt_t_min   0.330
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B3-H3A
 1.1 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C19(H19), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26)
3.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C)
3.c Boron cage BH refined with riding coordinates:
 B4(H4A), B5(H5), B6(H6), B7(H7), B8(H8A), B9(H9)
;
_shelx_res_checksum              82407
_shelx_hkl_checksum              40177
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id JCA-I-251_EtOH
_olex2_submission_special_instructions 'No special instructions were received'