#------------------------------------------------------------------------------
#$Date: 2021-08-18 02:03:37 +0300 (Wed, 18 Aug 2021) $
#$Revision: 268110 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/80/7708066.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7708066
loop_
_publ_author_name
'Takimoto, Kazuyoshi'
'Watanabe, Yutaka'
'Yoshida, Jun'
'Sato, Hisako'
_publ_section_title
;
 Five-Coordinate Iridium(III) Complex with ΔΛ Chirality
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT01960K
_journal_year                    2021
_chemical_formula_moiety
'C46 H40 Ir N4, Cl, 1.31(C H4 O), C0.69 H3.07 O0.69'
_chemical_formula_sum            'C48 H48.31 Cl Ir N4 O2'
_chemical_formula_weight         940.86
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-27 deposited with the CCDC.	2021-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.488(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3729(4)
_cell_length_b                   16.0231(3)
_cell_length_c                   17.1143(4)
_cell_measurement_reflns_used    35563
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.1160
_cell_measurement_theta_min      1.7560
_cell_volume                     4081.56(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00  90.00  360
  3  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00 180.00  360
  4  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00 270.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0399883000
_diffrn_orient_matrix_UB_12      -0.0233200000
_diffrn_orient_matrix_UB_13      -0.0146633000
_diffrn_orient_matrix_UB_21      -0.0255415000
_diffrn_orient_matrix_UB_22      0.0373098000
_diffrn_orient_matrix_UB_23      -0.0039609000
_diffrn_orient_matrix_UB_31      0.0044439000
_diffrn_orient_matrix_UB_32      0.0048332000
_diffrn_orient_matrix_UB_33      -0.0400185000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            68718
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.768
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.381
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83313
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       block
_exptl_crystal_F_000             1897
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.166
_refine_diff_density_min         -2.012
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         9849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0256P)²+9.0291P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8091
_reflns_number_total             9849
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt01960k2.cif
_cod_data_source_block           takimoto_autored
_cod_database_code               7708066
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         Ir1Cl1N4C46H40
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.729
_reflns_odcompleteness_completeness 94.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.06
_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, All O(H) groups
2. Others
 Sof(O3)=Sof(H3)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=1-FVAR(1)
 Sof(O2)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C31(H31A,H31B), C32(H32A,
 H32B), C33(H33A,H33B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C21(H21),
 C22(H22), C23(H23), C25(H25), C26(H26), C28(H28), C29(H29), C35(H35), C36(H36),
  C37(H37), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44)
3.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C34(H34A,H34B,H34C), C47(H47A,H47B,H47C), C48(H48A,H48B,
 H48C), C49(H49A,H49B,H49C)
3.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.225
_oxdiff_exptl_absorpt_empirical_full_min 0.895
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.28049(2) 0.64989(2) 0.64859(2) 0.01355(5) Uani 1 1 d . . . . .
N1 N 0.4175(2) 0.6750(2) 0.6568(2) 0.0173(8) Uani 1 1 d . . . . .
N2 N 0.1463(2) 0.6459(2) 0.6567(2) 0.0180(7) Uani 1 1 d . . . . .
N3 N 0.2668(2) 0.5164(2) 0.6279(2) 0.0178(8) Uani 1 1 d . . . . .
N4 N 0.2699(2) 0.6383(2) 0.52047(19) 0.0155(7) Uani 1 1 d . . . . .
C1 C 0.4323(3) 0.7601(3) 0.6501(2) 0.0201(10) Uani 1 1 d . . . . .
C2 C 0.3577(3) 0.8136(3) 0.6471(2) 0.0216(10) Uani 1 1 d . . . . .
C3 C 0.2771(3) 0.7756(3) 0.6516(3) 0.0190(9) Uani 1 1 d . . . . .
C4 C 0.2052(3) 0.8296(3) 0.6517(3) 0.0245(11) Uani 1 1 d . . . . .
H4 H 0.150199 0.807476 0.654619 0.029 Uiso 1 1 calc R . . . .
C5 C 0.2152(4) 0.9165(3) 0.6475(3) 0.0306(12) Uani 1 1 d . . . . .
H5 H 0.166362 0.950692 0.647954 0.037 Uiso 1 1 calc R . . . .
C6 C 0.2946(4) 0.9525(3) 0.6429(3) 0.0330(13) Uani 1 1 d . . . . .
H6 H 0.299251 1.010241 0.640093 0.040 Uiso 1 1 calc R . . . .
C7 C 0.3694(4) 0.9017(3) 0.6423(3) 0.0274(12) Uani 1 1 d . . . . .
C8 C 0.4535(4) 0.9330(3) 0.6360(3) 0.0331(13) Uani 1 1 d . . . . .
H8 H 0.460242 0.990025 0.629415 0.040 Uiso 1 1 calc R . . . .
C9 C 0.5243(4) 0.8818(4) 0.6395(3) 0.0357(14) Uani 1 1 d . . . . .
H9 H 0.578847 0.904325 0.635580 0.043 Uiso 1 1 calc R . . . .
C10 C 0.5169(3) 0.7934(3) 0.6491(3) 0.0264(11) Uani 1 1 d . . . . .
C11 C 0.5898(4) 0.7380(4) 0.6613(3) 0.0361(13) Uani 1 1 d . . . . .
H11 H 0.646923 0.757285 0.661650 0.043 Uiso 1 1 calc R . . . .
C12 C 0.5755(3) 0.6559(4) 0.6726(3) 0.0340(12) Uani 1 1 d . . . . .
H12 H 0.624224 0.619525 0.682572 0.041 Uiso 1 1 calc R . . . .
C13 C 0.4893(3) 0.6236(3) 0.6697(3) 0.0232(10) Uani 1 1 d . . . . .
C14 C 0.4811(3) 0.5323(3) 0.6817(3) 0.0235(10) Uani 1 1 d . . . . .
H14A H 0.424213 0.521427 0.694669 0.028 Uiso 1 1 calc R . . . .
H14B H 0.528622 0.514907 0.727557 0.028 Uiso 1 1 calc R . . . .
C15 C 0.4862(3) 0.4790(3) 0.6080(3) 0.0235(10) Uani 1 1 d . . . . .
H15A H 0.434702 0.491552 0.563685 0.028 Uiso 1 1 calc R . . . .
H15B H 0.539906 0.493935 0.591237 0.028 Uiso 1 1 calc R . . . .
C16 C 0.4878(3) 0.3859(3) 0.6254(3) 0.0270(11) Uani 1 1 d . . . . .
H16A H 0.436649 0.371711 0.646499 0.032 Uiso 1 1 calc R . . . .
H16B H 0.541927 0.372512 0.666502 0.032 Uiso 1 1 calc R . . . .
C17 C 0.4848(3) 0.3335(3) 0.5502(3) 0.0344(13) Uani 1 1 d . . . . .
H17A H 0.427151 0.339708 0.512745 0.052 Uiso 1 1 calc GR . . . .
H17B H 0.494459 0.275868 0.565175 0.052 Uiso 1 1 calc GR . . . .
H17C H 0.530915 0.352008 0.525370 0.052 Uiso 1 1 calc GR . . . .
C18 C 0.1400(3) 0.6298(3) 0.7351(3) 0.0199(10) Uani 1 1 d . . . . .
C19 C 0.2235(3) 0.6209(3) 0.7940(2) 0.0178(9) Uani 1 1 d . . . . .
C20 C 0.3034(3) 0.6353(3) 0.7688(2) 0.0172(9) Uani 1 1 d . . . . .
C21 C 0.3843(3) 0.6288(3) 0.8275(2) 0.0194(10) Uani 1 1 d . . . . .
H21 H 0.438233 0.638904 0.813833 0.023 Uiso 1 1 calc R . . . .
C22 C 0.3848(3) 0.6068(3) 0.9080(3) 0.0232(10) Uani 1 1 d . . . . .
H22 H 0.439409 0.602497 0.946370 0.028 Uiso 1 1 calc R . . . .
C23 C 0.3067(3) 0.5917(3) 0.9304(3) 0.0259(11) Uani 1 1 d . . . . .
H23 H 0.309156 0.574899 0.982948 0.031 Uiso 1 1 calc R . . . .
C24 C 0.2223(3) 0.6015(3) 0.8746(3) 0.0221(10) Uani 1 1 d . . . . .
C25 C 0.1378(3) 0.5950(3) 0.8948(3) 0.0293(11) Uani 1 1 d . . . . .
H25 H 0.136773 0.581494 0.947446 0.035 Uiso 1 1 calc R . . . .
C26 C 0.0594(3) 0.6079(3) 0.8392(3) 0.0312(12) Uani 1 1 d . . . . .
H26 H 0.005527 0.604983 0.854520 0.037 Uiso 1 1 calc R . . . .
C27 C 0.0583(3) 0.6262(3) 0.7564(3) 0.0265(11) Uani 1 1 d . . . . .
C28 C -0.0210(3) 0.6434(4) 0.6971(3) 0.0378(13) Uani 1 1 d . . . . .
H28 H -0.076764 0.641970 0.709071 0.045 Uiso 1 1 calc R . . . .
C29 C -0.0135(3) 0.6623(4) 0.6206(3) 0.0345(13) Uani 1 1 d . . . . .
H29 H -0.065262 0.674533 0.580853 0.041 Uiso 1 1 calc R . . . .
C30 C 0.0697(3) 0.6639(3) 0.6006(3) 0.0234(10) Uani 1 1 d . . . . .
C31 C 0.0690(3) 0.6894(3) 0.5159(3) 0.0224(10) Uani 1 1 d . . . . .
H31A H 0.129450 0.705296 0.514366 0.027 Uiso 1 1 calc R . . . .
H31B H 0.030940 0.738185 0.501579 0.027 Uiso 1 1 calc R . . . .
C32 C 0.0354(3) 0.6207(3) 0.4526(3) 0.0271(11) Uani 1 1 d . . . . .
H32A H 0.078360 0.575167 0.461316 0.033 Uiso 1 1 calc R . . . .
H32B H -0.021423 0.598941 0.458667 0.033 Uiso 1 1 calc R . . . .
C33 C 0.0232(3) 0.6550(4) 0.3672(3) 0.0355(12) Uani 1 1 d . . . . .
H33A H -0.024319 0.696436 0.356757 0.043 Uiso 1 1 calc R . . . .
H33B H 0.078233 0.682487 0.363298 0.043 Uiso 1 1 calc R . . . .
C34 C 0.0000(4) 0.5866(4) 0.3032(3) 0.0542(18) Uani 1 1 d . . . . .
H34A H -0.008990 0.611030 0.250580 0.081 Uiso 1 1 calc GR . . . .
H34B H -0.054063 0.558825 0.307272 0.081 Uiso 1 1 calc GR . . . .
H34C H 0.048274 0.547037 0.311623 0.081 Uiso 1 1 calc GR . . . .
C35 C 0.2586(3) 0.4573(3) 0.6810(3) 0.0236(10) Uani 1 1 d . . . . .
H35 H 0.264738 0.472379 0.734530 0.028 Uiso 1 1 calc R . . . .
C36 C 0.2410(3) 0.3734(3) 0.6589(3) 0.0267(11) Uani 1 1 d . . . . .
H36 H 0.234585 0.334204 0.697118 0.032 Uiso 1 1 calc R . . . .
C37 C 0.2332(3) 0.3500(3) 0.5806(3) 0.0295(11) Uani 1 1 d . . . . .
H37 H 0.222168 0.294562 0.565337 0.035 Uiso 1 1 calc R . . . .
C38 C 0.2422(3) 0.4103(3) 0.5231(3) 0.0206(10) Uani 1 1 d . . . . .
C39 C 0.2366(3) 0.3919(3) 0.4400(3) 0.0260(11) Uani 1 1 d . . . . .
H39 H 0.227772 0.336990 0.422121 0.031 Uiso 1 1 calc R . . . .
C40 C 0.2439(3) 0.4521(3) 0.3871(3) 0.0269(11) Uani 1 1 d . . . . .
H40 H 0.239817 0.438050 0.333558 0.032 Uiso 1 1 calc R . . . .
C41 C 0.2578(3) 0.5376(3) 0.4120(2) 0.0190(9) Uani 1 1 d . . . . .
C42 C 0.2679(3) 0.6035(3) 0.3599(3) 0.0231(10) Uani 1 1 d . . . . .
H42 H 0.266474 0.592695 0.306219 0.028 Uiso 1 1 calc R . . . .
C43 C 0.2797(3) 0.6827(3) 0.3892(3) 0.0252(10) Uani 1 1 d . . . . .
H43 H 0.287838 0.726247 0.355800 0.030 Uiso 1 1 calc R . . . .
C44 C 0.2795(3) 0.6988(3) 0.4700(3) 0.0213(10) Uani 1 1 d . . . . .
H44 H 0.286422 0.753462 0.488722 0.026 Uiso 1 1 calc R . . . .
C45 C 0.2610(3) 0.5581(3) 0.4931(2) 0.0163(9) Uani 1 1 d . . . . .
C46 C 0.2561(3) 0.4938(3) 0.5496(3) 0.0173(9) Uani 1 1 d . . . . .
Cl1 Cl 0.19578(9) 1.15607(8) 0.68690(8) 0.0375(3) Uani 1 1 d . . . . .
O1 O 0.1116(3) 1.1719(3) 0.5028(3) 0.0646(14) Uani 1 1 d . . . . .
H1 H 0.131088 1.169052 0.551903 0.097 Uiso 1 1 calc GR . . . .
C47 C 0.0612(6) 1.1014(4) 0.4752(5) 0.079(3) Uani 1 1 d . . . . .
H47A H 0.081549 1.055991 0.511849 0.119 Uiso 1 1 calc GR . . . .
H47B H 0.068204 1.086856 0.422705 0.119 Uiso 1 1 calc GR . . . .
H47C H -0.000934 1.112413 0.471996 0.119 Uiso 1 1 calc GR . . . .
O2 O 0.3786(3) 1.1543(3) 0.6212(3) 0.0261(12) Uani 0.690(6) 1 d . . P A 1
H2 H 0.336673 1.166584 0.640669 0.039 Uiso 1 1 calc GR . . A 1
C48 C 0.3453(5) 1.1409(5) 0.5357(5) 0.040(2) Uani 0.690(6) 1 d . . P A 1
H48A H 0.303649 1.095202 0.526462 0.060 Uiso 0.690(6) 1 calc GR . P A 1
H48B H 0.394645 1.128185 0.512644 0.060 Uiso 0.690(6) 1 calc GR . P A 1
H48C H 0.315565 1.190466 0.511018 0.060 Uiso 0.690(6) 1 calc GR . P A 1
O3 O 0.1998(7) 0.2997(9) 0.8444(8) 0.052(4) Uani 0.310(6) 1 d . . P A 2
H3 H 0.152241 0.325490 0.833955 0.078 Uiso 0.310(6) 1 calc GR . P A 2
C49 C 0.2649(13) 0.3283(12) 0.9429(10) 0.042(5) Uani 0.310(6) 1 d . . P A 2
H49A H 0.226006 0.350786 0.973613 0.064 Uiso 0.310(6) 1 calc GR . P A 2
H49B H 0.308535 0.369618 0.938046 0.064 Uiso 0.310(6) 1 calc GR . P A 2
H49C H 0.295145 0.279942 0.969764 0.064 Uiso 0.310(6) 1 calc GR . P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ir1 N3 104.65(13) . . ?
N1 Ir1 N4 84.57(13) . . ?
N2 Ir1 N1 168.16(14) . . ?
N2 Ir1 N3 85.66(14) . . ?
N2 Ir1 N4 103.75(13) . . ?
N4 Ir1 N3 76.74(13) . . ?
C3 Ir1 N1 80.79(17) . . ?
C3 Ir1 N2 89.79(17) . . ?
C3 Ir1 N3 170.81(16) . . ?
C3 Ir1 N4 96.66(15) . . ?
C20 Ir1 N1 92.15(15) . . ?
C20 Ir1 N2 81.50(16) . . ?
C20 Ir1 N3 92.13(15) . . ?
C20 Ir1 N4 167.13(15) . . ?
C20 Ir1 C3 95.09(17) . . ?
C1 N1 Ir1 111.2(3) . . ?
C13 N1 Ir1 130.9(3) . . ?
C13 N1 C1 117.8(4) . . ?
C18 N2 Ir1 112.1(3) . . ?
C30 N2 Ir1 129.8(3) . . ?
C30 N2 C18 117.8(4) . . ?
C35 N3 Ir1 127.5(3) . . ?
C35 N3 C46 118.1(4) . . ?
C46 N3 Ir1 114.0(3) . . ?
C44 N4 Ir1 127.1(3) . . ?
C44 N4 C45 118.7(4) . . ?
C45 N4 Ir1 113.9(3) . . ?
N1 C1 C2 116.5(4) . . ?
N1 C1 C10 122.9(4) . . ?
C10 C1 C2 120.6(4) . . ?
C1 C2 C7 119.1(5) . . ?
C3 C2 C1 116.9(4) . . ?
C3 C2 C7 124.0(5) . . ?
C2 C3 Ir1 113.8(3) . . ?
C2 C3 C4 116.1(4) . . ?
C4 C3 Ir1 129.9(4) . . ?
C3 C4 H4 119.5 . . ?
C3 C4 C5 121.0(5) . . ?
C5 C4 H4 119.5 . . ?
C4 C5 H5 119.0 . . ?
C6 C5 C4 122.0(5) . . ?
C6 C5 H5 119.0 . . ?
C5 C6 H6 120.1 . . ?
C5 C6 C7 119.8(5) . . ?
C7 C6 H6 120.1 . . ?
C6 C7 C2 117.1(5) . . ?
C6 C7 C8 123.8(5) . . ?
C8 C7 C2 119.0(5) . . ?
C7 C8 H8 119.3 . . ?
C9 C8 C7 121.5(5) . . ?
C9 C8 H8 119.3 . . ?
C8 C9 H9 119.4 . . ?
C8 C9 C10 121.2(5) . . ?
C10 C9 H9 119.4 . . ?
C1 C10 C9 118.4(5) . . ?
C11 C10 C1 117.6(5) . . ?
C11 C10 C9 124.0(5) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 C10 118.9(5) . . ?
C12 C11 H11 120.5 . . ?
C11 C12 H12 118.8 . . ?
C11 C12 C13 122.3(5) . . ?
C13 C12 H12 118.8 . . ?
N1 C13 C12 120.2(5) . . ?
N1 C13 C14 121.9(4) . . ?
C12 C13 C14 117.9(4) . . ?
C13 C14 H14A 108.7 . . ?
C13 C14 H14B 108.7 . . ?
C13 C14 C15 114.1(4) . . ?
H14A C14 H14B 107.6 . . ?
C15 C14 H14A 108.7 . . ?
C15 C14 H14B 108.7 . . ?
C14 C15 H15A 109.1 . . ?
C14 C15 H15B 109.1 . . ?
H15A C15 H15B 107.8 . . ?
C16 C15 C14 112.6(4) . . ?
C16 C15 H15A 109.1 . . ?
C16 C15 H15B 109.1 . . ?
C15 C16 H16A 109.2 . . ?
C15 C16 H16B 109.2 . . ?
C15 C16 C17 112.2(4) . . ?
H16A C16 H16B 107.9 . . ?
C17 C16 H16A 109.2 . . ?
C17 C16 H16B 109.2 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 C19 115.5(4) . . ?
C27 C18 N2 123.0(4) . . ?
C27 C18 C19 121.5(4) . . ?
C20 C19 C18 117.6(4) . . ?
C24 C19 C18 118.7(4) . . ?
C24 C19 C20 123.6(4) . . ?
C19 C20 Ir1 112.7(3) . . ?
C21 C20 Ir1 129.9(3) . . ?
C21 C20 C19 117.0(4) . . ?
C20 C21 H21 119.8 . . ?
C20 C21 C22 120.3(4) . . ?
C22 C21 H21 119.8 . . ?
C21 C22 H22 119.2 . . ?
C23 C22 C21 121.5(4) . . ?
C23 C22 H22 119.2 . . ?
C22 C23 H23 119.6 . . ?
C22 C23 C24 120.7(4) . . ?
C24 C23 H23 119.6 . . ?
C19 C24 C25 119.0(4) . . ?
C23 C24 C19 116.7(4) . . ?
C23 C24 C25 124.3(4) . . ?
C24 C25 H25 119.3 . . ?
C26 C25 C24 121.5(4) . . ?
C26 C25 H25 119.3 . . ?
C25 C26 H26 119.6 . . ?
C25 C26 C27 120.7(4) . . ?
C27 C26 H26 119.6 . . ?
C18 C27 C26 118.4(4) . . ?
C18 C27 C28 118.7(4) . . ?
C28 C27 C26 122.9(4) . . ?
C27 C28 H28 121.1 . . ?
C29 C28 C27 117.7(4) . . ?
C29 C28 H28 121.1 . . ?
C28 C29 H29 118.8 . . ?
C28 C29 C30 122.4(4) . . ?
C30 C29 H29 118.8 . . ?
N2 C30 C29 120.4(4) . . ?
N2 C30 C31 122.6(4) . . ?
C29 C30 C31 116.9(4) . . ?
C30 C31 H31A 108.8 . . ?
C30 C31 H31B 108.8 . . ?
C30 C31 C32 113.8(4) . . ?
H31A C31 H31B 107.7 . . ?
C32 C31 H31A 108.8 . . ?
C32 C31 H31B 108.8 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 108.1 . . ?
C33 C32 C31 110.8(4) . . ?
C33 C32 H32A 109.5 . . ?
C33 C32 H32B 109.5 . . ?
C32 C33 H33A 109.2 . . ?
C32 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?
C34 C33 C32 112.2(5) . . ?
C34 C33 H33A 109.2 . . ?
C34 C33 H33B 109.2 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N3 C35 H35 118.7 . . ?
N3 C35 C36 122.6(4) . . ?
C36 C35 H35 118.7 . . ?
C35 C36 H36 120.3 . . ?
C37 C36 C35 119.3(5) . . ?
C37 C36 H36 120.3 . . ?
C36 C37 H37 120.1 . . ?
C36 C37 C38 119.8(5) . . ?
C38 C37 H37 120.1 . . ?
C37 C38 C39 124.0(4) . . ?
C37 C38 C46 117.3(4) . . ?
C46 C38 C39 118.7(4) . . ?
C38 C39 H39 119.2 . . ?
C40 C39 C38 121.7(4) . . ?
C40 C39 H39 119.2 . . ?
C39 C40 H40 119.5 . . ?
C39 C40 C41 121.0(4) . . ?
C41 C40 H40 119.5 . . ?
C42 C41 C40 123.8(4) . . ?
C45 C41 C40 118.6(4) . . ?
C45 C41 C42 117.5(4) . . ?
C41 C42 H42 120.3 . . ?
C43 C42 C41 119.3(4) . . ?
C43 C42 H42 120.3 . . ?
C42 C43 H43 120.0 . . ?
C42 C43 C44 120.0(4) . . ?
C44 C43 H43 120.0 . . ?
N4 C44 C43 122.2(4) . . ?
N4 C44 H44 118.9 . . ?
C43 C44 H44 118.9 . . ?
N4 C45 C41 122.2(4) . . ?
N4 C45 C46 117.7(4) . . ?
C41 C45 C46 120.1(4) . . ?
N3 C46 C38 122.8(4) . . ?
N3 C46 C45 117.5(4) . . ?
C38 C46 C45 119.7(4) . . ?
C47 O1 H1 109.5 . . ?
O1 C47 H47A 109.5 . . ?
O1 C47 H47B 109.5 . . ?
O1 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C48 O2 H2 109.5 . . ?
O2 C48 H48A 109.5 . . ?
O2 C48 H48B 109.5 . . ?
O2 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C49 O3 H3 109.5 . . ?
O3 C49 H49A 109.5 . . ?
O3 C49 H49B 109.5 . . ?
O3 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 N1 2.114(4) . ?
Ir1 N2 2.103(3) . ?
Ir1 N3 2.170(4) . ?
Ir1 N4 2.166(3) . ?
Ir1 C3 2.016(4) . ?
Ir1 C20 2.013(4) . ?
N1 C1 1.391(6) . ?
N1 C13 1.352(6) . ?
N2 C18 1.393(5) . ?
N2 C30 1.352(5) . ?
N3 C35 1.340(5) . ?
N3 C46 1.357(5) . ?
N4 C44 1.331(5) . ?
N4 C45 1.363(5) . ?
C1 C2 1.423(7) . ?
C1 C10 1.410(6) . ?
C2 C3 1.401(6) . ?
C2 C7 1.427(6) . ?
C3 C4 1.403(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.405(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.371(7) . ?
C6 H6 0.9300 . ?
C6 C7 1.410(7) . ?
C7 C8 1.416(7) . ?
C8 H8 0.9300 . ?
C8 C9 1.353(8) . ?
C9 H9 0.9300 . ?
C9 C10 1.433(7) . ?
C10 C11 1.404(8) . ?
C11 H11 0.9300 . ?
C11 C12 1.356(8) . ?
C12 H12 0.9300 . ?
C12 C13 1.412(7) . ?
C13 C14 1.487(7) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.541(6) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.520(7) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.528(7) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.427(6) . ?
C18 C27 1.392(6) . ?
C19 C20 1.419(6) . ?
C19 C24 1.418(6) . ?
C20 C21 1.393(6) . ?
C21 H21 0.9300 . ?
C21 C22 1.421(6) . ?
C22 H22 0.9300 . ?
C22 C23 1.371(7) . ?
C23 H23 0.9300 . ?
C23 C24 1.414(7) . ?
C24 C25 1.429(6) . ?
C25 H25 0.9300 . ?
C25 C26 1.352(7) . ?
C26 H26 0.9300 . ?
C26 C27 1.444(6) . ?
C27 C28 1.405(7) . ?
C28 H28 0.9300 . ?
C28 C29 1.376(7) . ?
C29 H29 0.9300 . ?
C29 C30 1.405(6) . ?
C30 C31 1.502(6) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.542(6) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.529(7) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.527(7) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35 0.9300 . ?
C35 C36 1.403(6) . ?
C36 H36 0.9300 . ?
C36 C37 1.368(7) . ?
C37 H37 0.9300 . ?
C37 C38 1.409(7) . ?
C38 C39 1.435(6) . ?
C38 C46 1.412(6) . ?
C39 H39 0.9300 . ?
C39 C40 1.346(7) . ?
C40 H40 0.9300 . ?
C40 C41 1.435(7) . ?
C41 C42 1.414(6) . ?
C41 C45 1.414(5) . ?
C42 H42 0.9300 . ?
C42 C43 1.360(7) . ?
C43 H43 0.9300 . ?
C43 C44 1.407(6) . ?
C44 H44 0.9300 . ?
C45 C46 1.429(6) . ?
O1 H1 0.8200 . ?
O1 C47 1.384(8) . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
O2 H2 0.8200 . ?
O2 C48 1.440(9) . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
O3 H3 0.8200 . ?
O3 C49 1.79(2) . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
