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_4131148
_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         'C29 H27 B9 F4 Ir N3, C H2 Cl2'
_chemical_formula_sum            'C30 H29 B9 Cl2 F4 Ir N3'
_chemical_formula_weight         868.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2016-06-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.385(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2061(13)
_cell_length_b                   12.6835(9)
_cell_length_c                   16.3956(10)
_cell_measurement_reflns_used    5521
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.600
_cell_measurement_theta_min      2.361
_cell_volume                     3367.2(4)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15163
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         25.77
_diffrn_reflns_theta_min         2.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.175
_exptl_absorpt_correction_T_max  0.490342
_exptl_absorpt_correction_T_min  0.372821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1355 before and 0.0461 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1565 before and 0.0516 after correction.
 The Ratio of minimum to maximum transmission is 0.76.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 45863 reflections, Rint = 0.0705
 (18030 with I > 3sig(I), Rint = 0.0468)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.7121
_exptl_crystal_description       plate
_exptl_crystal_F_000             1684.7262
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.0904
_refine_diff_density_min         -1.5028
_refine_diff_density_rms         0.2401
_refine_ls_d_res_high            0.8173
_refine_ls_d_res_low             10.0288
_refine_ls_goodness_of_fit_ref   1.0784
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    53
_refine_ls_number_parameters     450
_refine_ls_number_reflns         9536
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0784
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+32.1278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1195
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              19
_reflns_limit_h_min              -19
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                7985
_reflns_number_total             9536
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja6b10232_si_002.cif
_cod_data_source_block           spok19
_cod_database_code               4131148
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5873(14) 0.4127(14)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C30(H30a,H30b)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C11(H11), C15(H15), C16(H16),
 C17(H17), C18(H18), C20(H20), C22(H22), C26(H26), C27(H27), C28(H28), C29(H29)
3.c Boron cage BH refined with riding coordinates:
 C1(H1), B2(H2a), B3(H3), B4(H4a), B5(H5a), B6(H6a), B7(H7a), B8(H8), B9(H9a)
;
_olex2_submission_original_sample_id JCA-I-268
_olex2_submission_special_instructions 'No special instructions were received'