#------------------------------------------------------------------------------
#$Date: 2021-11-15 10:07:04 +0200 (Mon, 15 Nov 2021) $
#$Revision: 270642 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/52/1565204.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_1565204
loop_
_publ_author_name
'Yokley, Timothy W.'
'Schley, Nathan D.'
'Brewster, Timothy P.'
_publ_section_title
;
 Rhodium and iridium NNO-Scorpionate complexes: synthesis, structure, and
 reactivity with aluminum alkyls
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119529
_journal_paper_doi               10.1016/j.ica.2020.119529
_journal_volume                  506
_journal_year                    2020
_chemical_formula_moiety
'C20 H28 Ir N4 O2, 2.5(C H2 Cl2), C32 H12 B F24'
_chemical_formula_sum            'C54.5 H45 B Cl5 F24 Ir N4 O2'
_chemical_formula_weight         1624.20
_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   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                108.581(3)
_cell_angle_beta                 92.978(2)
_cell_angle_gamma                103.244(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7123(3)
_cell_length_b                   12.9256(4)
_cell_length_c                   20.2507(5)
_cell_measurement_reflns_used    23662
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.5110
_cell_measurement_theta_min      3.1870
_cell_volume                     3041.86(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1506
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -50.00  44.00   1.00   10.00    --   17.65 -77.00 150.00   94
  2  ω     -9.00  85.00   1.00   10.00    --   17.65  77.00-150.00   94
  3  ω      1.00  85.00   1.00   10.00    --   17.65  57.00  90.00   84
  4  ω    -50.00  34.00   1.00   10.00    --   17.65 -57.00 -90.00   84
  5  ω     -9.00  85.00   1.00   10.00    --   17.65  77.00   0.00   94
  6  ω    -85.00 -35.00   1.00   10.00    --  -17.73 148.00  15.00   50
  7  ω    -71.00 -22.00   1.00   10.00    --  -17.73 124.00-148.00   49
  8  ω     -1.00  87.00   1.00   10.00    --   17.65  38.00 -60.00   88
  9  ω      1.00  85.00   1.00   10.00    --   17.65  57.00-180.00   84
 10  ω     35.00  78.00   1.00   10.00    --   17.65 178.00 -30.00   43
 11  ω     35.00  90.00   1.00   10.00    --   17.65 178.00 120.00   55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0130383000
_diffrn_orient_matrix_UB_12      -0.0287752000
_diffrn_orient_matrix_UB_13      -0.0367862000
_diffrn_orient_matrix_UB_21      -0.0503861000
_diffrn_orient_matrix_UB_22      -0.0315235000
_diffrn_orient_matrix_UB_23      0.0052877000
_diffrn_orient_matrix_UB_31      -0.0252649000
_diffrn_orient_matrix_UB_32      0.0420941000
_diffrn_orient_matrix_UB_33      -0.0031267000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            57450
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.005
_diffrn_reflns_theta_min         2.246
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.533
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.173
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_description       block
_exptl_crystal_F_000             1598
_exptl_crystal_size_max          0.535
_exptl_crystal_size_mid          0.345
_exptl_crystal_size_min          0.122
_refine_diff_density_max         1.631
_refine_diff_density_min         -1.896
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         15839
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0422
_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/[σ²(Fo²)+(0.0404P)²+3.9113P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.0976
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                14141
_reflns_number_total             15839
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            tj08.cif
_cod_data_source_block           tj08
_cod_original_cell_volume        3041.86(15)
_cod_original_formula_sum        'C54.50 H45 B Cl5 F24 Ir N4 O2'
_cod_database_code               1565204
_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.
;
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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. Rigid body (RIGU) restrains
 F4, F4A, F5, F5A, F6, F6A, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F19, F19A, F20, F20A, F21, F21A, C51
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(2)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(2)
 Fixed Sof: C55(0.5) H55A(0.5) H55B(0.5)
4.a Ternary CH refined with riding coordinates:
 C2(H2), C13(H13), C14(H14), C17(H17), C18(H18)
4.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C15(H15A,H15B), C16(H16A,H16B), C19(H19A,H19B), C20(H20A,H20B),
 C54(H54A,H54B), C55(H55A,H55B), C53(H53A,H53B)
4.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C22(H22), C24(H24), C26(H26), C30(H30), C32(H32), C34(H34), C38(H38),
 C40(H40), C42(H42), C46(H46), C48(H48), C50(H50)
4.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_olex2_date_sample_data_collection 2019-02-09
_olex2_exptl_crystal_mounting_method 'mounted in a polyimide loop'
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.061
_oxdiff_exptl_absorpt_empirical_full_min 0.356
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 1.00463(2) 0.66296(2) 0.27194(2) 0.01523(5) Uani 1 1 d . . . . .
O1 O 0.90423(19) 0.5622(2) 0.17173(12) 0.0175(5) Uani 1 1 d . . . . .
O2 O 0.8944(2) 0.4849(2) 0.05565(13) 0.0217(5) Uani 1 1 d . . . . .
N1 N 1.0753(2) 0.7712(2) 0.22050(16) 0.0180(6) Uani 1 1 d . . . . .
N2 N 1.0881(2) 0.7230(2) 0.15116(16) 0.0186(6) Uani 1 1 d . . . . .
N3 N 1.1251(2) 0.5829(2) 0.23157(15) 0.0163(6) Uani 1 1 d . . . . .
N4 N 1.1305(2) 0.5585(2) 0.16072(15) 0.0174(6) Uani 1 1 d . . . . .
C1 C 0.9432(3) 0.5435(3) 0.11413(18) 0.0172(7) Uani 1 1 d . . . . .
C2 C 1.0652(3) 0.6010(3) 0.11973(19) 0.0179(7) Uani 1 1 d . . . . .
H2 H 1.085979 0.582815 0.072238 0.021 Uiso 1 1 calc R . . . .
C3 C 1.1369(3) 0.8037(3) 0.1249(2) 0.0284(9) Uani 1 1 d . . . . .
C4 C 1.1562(4) 0.9044(3) 0.1790(2) 0.0302(9) Uani 1 1 d . . . . .
H4A H 1.118368 0.954007 0.166287 0.036 Uiso 1 1 calc R . . . .
H4B H 1.233689 0.941338 0.189091 0.036 Uiso 1 1 calc R . . . .
C5 C 1.1188(3) 0.8822(3) 0.2374(2) 0.0245(8) Uani 1 1 d . . . . .
C6 C 1.1552(5) 0.7774(4) 0.0498(2) 0.0446(13) Uani 1 1 d . . . . .
H6A H 1.192288 0.718364 0.037176 0.067 Uiso 1 1 calc GR . . . .
H6B H 1.198889 0.843795 0.043413 0.067 Uiso 1 1 calc GR . . . .
H6C H 1.086260 0.752949 0.020382 0.067 Uiso 1 1 calc GR . . . .
C7 C 1.1247(3) 0.9648(3) 0.3089(2) 0.0291(9) Uani 1 1 d . . . . .
H7A H 1.056680 0.985044 0.313777 0.044 Uiso 1 1 calc GR . . . .
H7B H 1.182466 1.031223 0.315541 0.044 Uiso 1 1 calc GR . . . .
H7C H 1.138721 0.931535 0.343456 0.044 Uiso 1 1 calc GR . . . .
C8 C 1.2175(3) 0.5166(3) 0.1431(2) 0.0257(8) Uani 1 1 d . . . . .
C9 C 1.2678(3) 0.5142(4) 0.2036(2) 0.0289(9) Uani 1 1 d . . . . .
H9 H 1.329488 0.488306 0.207783 0.035 Uiso 1 1 calc R . . . .
C10 C 1.2101(3) 0.5573(3) 0.2577(2) 0.0216(7) Uani 1 1 d . . . . .
C11 C 1.2434(4) 0.4820(5) 0.0698(2) 0.0388(11) Uani 1 1 d . . . . .
H11A H 1.180171 0.430162 0.038900 0.058 Uiso 1 1 calc GR . . . .
H11B H 1.302020 0.446000 0.067211 0.058 Uiso 1 1 calc GR . . . .
H11C H 1.264863 0.547510 0.056050 0.058 Uiso 1 1 calc GR . . . .
C12 C 1.2404(3) 0.5799(4) 0.3339(2) 0.0272(8) Uani 1 1 d . . . . .
H12A H 1.212840 0.641118 0.361116 0.041 Uiso 1 1 calc GR . . . .
H12B H 1.318333 0.599645 0.344793 0.041 Uiso 1 1 calc GR . . . .
H12C H 1.209410 0.513362 0.345029 0.041 Uiso 1 1 calc GR . . . .
C13 C 0.8592(3) 0.7278(3) 0.2843(2) 0.0201(7) Uani 1 1 d . . . . .
H13 H 0.854360 0.779660 0.258696 0.024 Uiso 1 1 calc R . . . .
C14 C 0.9257(3) 0.7778(3) 0.3483(2) 0.0236(8) Uani 1 1 d . . . . .
H14 H 0.960505 0.858366 0.359178 0.028 Uiso 1 1 calc R . . . .
C15 C 0.9029(3) 0.7440(3) 0.4129(2) 0.0257(8) Uani 1 1 d . . . . .
H15A H 0.825245 0.711083 0.409408 0.031 Uiso 1 1 calc R . . . .
H15B H 0.923538 0.811118 0.454655 0.031 Uiso 1 1 calc R . . . .
C16 C 0.9649(3) 0.6591(3) 0.42082(19) 0.0253(8) Uani 1 1 d . . . . .
H16A H 1.036951 0.700051 0.446401 0.030 Uiso 1 1 calc R . . . .
H16B H 0.926844 0.617049 0.448350 0.030 Uiso 1 1 calc R . . . .
C17 C 0.9766(3) 0.5770(3) 0.35119(19) 0.0220(8) Uani 1 1 d . . . . .
H17 H 1.028242 0.532450 0.354412 0.026 Uiso 1 1 calc R . . . .
C18 C 0.8940(3) 0.5241(3) 0.29400(19) 0.0208(7) Uani 1 1 d . . . . .
H18 H 0.899089 0.449093 0.264779 0.025 Uiso 1 1 calc R . . . .
C19 C 0.7777(3) 0.5357(3) 0.2945(2) 0.0235(8) Uani 1 1 d . . . . .
H19A H 0.759731 0.550535 0.342070 0.028 Uiso 1 1 calc R . . . .
H19B H 0.728473 0.464565 0.265049 0.028 Uiso 1 1 calc R . . . .
C20 C 0.7591(3) 0.6298(3) 0.2686(2) 0.0231(8) Uani 1 1 d . . . . .
H20A H 0.736407 0.598611 0.218246 0.028 Uiso 1 1 calc R . . . .
H20B H 0.700328 0.657529 0.290582 0.028 Uiso 1 1 calc R . . . .
Cl3 Cl -0.13821(13) -0.03145(10) 0.20063(6) 0.0525(3) Uani 1 1 d . . . . .
Cl4 Cl -0.17582(13) -0.25584(10) 0.09844(6) 0.0512(3) Uani 1 1 d . . . . .
C54 C -0.1661(5) -0.1141(4) 0.1111(2) 0.0471(13) Uani 1 1 d . . . . .
H54A H -0.234119 -0.107040 0.091208 0.057 Uiso 1 1 calc R . . . .
H54B H -0.108593 -0.086229 0.086613 0.057 Uiso 1 1 calc R . . . .
Cl5 Cl 0.5949(2) -0.0407(2) -0.01948(12) 0.1042(8) Uani 1 1 d . . . . .
C55 C 0.4667(9) -0.0594(13) -0.0179(6) 0.076(5) Uani 0.5 1 d . . P A 1
H55A H 0.445186 -0.116901 0.003612 0.091 Uiso 0.5 1 calc R . P A 1
H55B H 0.433240 -0.093330 -0.066541 0.091 Uiso 0.5 1 calc R . P A 1
Cl1 Cl 0.26474(15) 0.01561(19) 0.65327(8) 0.0831(6) Uani 1 1 d . . . . .
Cl2 Cl 0.13480(12) -0.03787(13) 0.51923(9) 0.0654(4) Uani 1 1 d . . . . .
C53 C 0.2665(4) 0.0003(5) 0.5650(3) 0.0478(12) Uani 1 1 d . . . . .
H53A H 0.303805 -0.057129 0.543619 0.057 Uiso 1 1 calc R . . . .
H53B H 0.307183 0.070947 0.561166 0.057 Uiso 1 1 calc R . . . .
F1 F 0.4722(3) -0.1145(4) 0.4072(2) 0.0963(16) Uani 1 1 d . . . . .
F2 F 0.3058(2) -0.1367(3) 0.38025(19) 0.0654(10) Uani 1 1 d . . . . .
F3 F 0.4007(5) 0.0238(3) 0.44263(19) 0.119(2) Uani 1 1 d . . . . .
F4 F 0.4756(15) -0.2767(7) 0.1514(7) 0.103(6) Uani 0.62(2) 1 d . U P B 1
F4A F 0.5666(11) -0.2039(19) 0.1381(11) 0.107(9) Uani 0.38(2) 1 d . U P B 2
F5 F 0.5606(7) -0.1485(7) 0.1150(5) 0.072(3) Uani 0.62(2) 1 d . U P B 1
F5A F 0.452(2) -0.1645(11) 0.0792(7) 0.081(6) Uani 0.38(2) 1 d . U P B 2
F6 F 0.3917(9) -0.2100(12) 0.0896(6) 0.099(6) Uani 0.62(2) 1 d . U P B 1
F6A F 0.4006(14) -0.2837(9) 0.1268(7) 0.072(5) Uani 0.38(2) 1 d . U P B 2
F7 F 0.85984(18) 0.2297(2) 0.20611(13) 0.0331(6) Uani 1 1 d . . . . .
F8 F 0.89077(19) 0.2963(2) 0.12296(15) 0.0381(6) Uani 1 1 d . . . . .
F9 F 0.7994(2) 0.1247(2) 0.09887(14) 0.0372(6) Uani 1 1 d . . . . .
F10 F 0.6409(2) 0.4918(3) 0.06229(19) 0.0635(10) Uani 1 1 d . . . . .
F11 F 0.4812(3) 0.3765(2) 0.03117(14) 0.0499(8) Uani 1 1 d . . . . .
F12 F 0.5148(2) 0.5165(2) 0.12581(13) 0.0368(6) Uani 1 1 d . . . . .
F13 F 0.8448(2) 0.4537(2) 0.51697(13) 0.0403(7) Uani 1 1 d . . . . .
F14 F 0.8504(2) 0.3314(3) 0.41794(14) 0.0565(9) Uani 1 1 d . . . . .
F15 F 0.7508(2) 0.2834(2) 0.49024(15) 0.0431(7) Uani 1 1 d . . . . .
F16 F 0.6104(3) 0.6950(2) 0.51366(15) 0.0541(9) Uani 1 1 d . . . . .
F17 F 0.6007(3) 0.6933(2) 0.40806(16) 0.0529(9) Uani 1 1 d . . . . .
F18 F 0.45834(19) 0.6311(2) 0.44816(14) 0.0342(6) Uani 1 1 d . . . . .
F19 F 0.1607(6) 0.0646(9) 0.0497(4) 0.074(3) Uani 0.721(17) 1 d . U P C 1
F19A F 0.1948(10) 0.180(2) 0.0511(6) 0.060(6) Uani 0.279(17) 1 d . U P C 2
F20 F 0.1362(10) 0.2276(5) 0.0658(3) 0.094(4) Uani 0.721(17) 1 d . U P C 1
F20A F 0.0442(19) 0.172(3) 0.0777(7) 0.084(9) Uani 0.279(17) 1 d . U P C 2
F21 F 0.0177(4) 0.1043(7) 0.0848(3) 0.0527(19) Uani 0.721(17) 1 d . U P C 1
F21A F 0.109(3) 0.0386(13) 0.0619(10) 0.097(9) Uani 0.279(17) 1 d . U P C 2
F22 F 0.0612(3) 0.3557(2) 0.35508(17) 0.0540(9) Uani 1 1 d . . . . .
F23 F 0.00594(19) 0.1800(2) 0.33514(13) 0.0340(6) Uani 1 1 d . . . . .
F24 F 0.1475(2) 0.2762(3) 0.40863(13) 0.0521(8) Uani 1 1 d . . . . .
C21 C 0.4615(3) 0.1031(3) 0.26421(19) 0.0180(7) Uani 1 1 d . . . . .
C22 C 0.4389(3) 0.0739(3) 0.3239(2) 0.0234(8) Uani 1 1 d . . . . .
H22 H 0.432598 0.129862 0.364754 0.028 Uiso 1 1 calc R . . . .
C23 C 0.4254(3) -0.0358(4) 0.3242(2) 0.0313(9) Uani 1 1 d . . . . .
C24 C 0.4349(4) -0.1206(4) 0.2647(3) 0.0369(11) Uani 1 1 d . . . . .
H24 H 0.426501 -0.193921 0.264851 0.044 Uiso 1 1 calc R . . . .
C25 C 0.4570(4) -0.0952(3) 0.2051(3) 0.0337(10) Uani 1 1 d . . . . .
C26 C 0.4697(3) 0.0152(3) 0.2050(2) 0.0245(8) Uani 1 1 d . . . . .
H26 H 0.483964 0.030365 0.163940 0.029 Uiso 1 1 calc R . . . .
C27 C 0.4025(4) -0.0636(4) 0.3887(3) 0.0449(13) Uani 1 1 d . . . . .
C28 C 0.4708(5) -0.1844(4) 0.1403(3) 0.0501(12) Uani 1 1 d . U . . .
C29 C 0.5430(3) 0.2613(3) 0.20517(17) 0.0144(6) Uani 1 1 d . . . . .
C30 C 0.6407(3) 0.2302(3) 0.19507(18) 0.0165(7) Uani 1 1 d . . . . .
H30 H 0.659419 0.183966 0.218193 0.020 Uiso 1 1 calc R . . . .
C31 C 0.7111(3) 0.2658(3) 0.15169(18) 0.0174(7) Uani 1 1 d . . . . .
C32 C 0.6875(3) 0.3347(3) 0.11572(19) 0.0183(7) Uani 1 1 d . . . . .
H32 H 0.734735 0.359004 0.086934 0.022 Uiso 1 1 calc R . . . .
C33 C 0.5902(3) 0.3658(3) 0.12469(18) 0.0168(7) Uani 1 1 d . . . . .
C34 C 0.5211(3) 0.3311(3) 0.16893(17) 0.0155(7) Uani 1 1 d . . . . .
H34 H 0.457658 0.355429 0.174581 0.019 Uiso 1 1 calc R . . . .
C35 C 0.8145(3) 0.2297(3) 0.1448(2) 0.0227(8) Uani 1 1 d . . . . .
C36 C 0.5582(3) 0.4376(4) 0.0860(2) 0.0248(8) Uani 1 1 d . . . . .
C37 C 0.5348(3) 0.3266(3) 0.33820(17) 0.0150(6) Uani 1 1 d . . . . .
C38 C 0.6243(3) 0.3092(3) 0.37276(17) 0.0168(7) Uani 1 1 d . . . . .
H38 H 0.639720 0.239135 0.356398 0.020 Uiso 1 1 calc R . . . .
C39 C 0.6904(3) 0.3933(3) 0.43067(18) 0.0184(7) Uani 1 1 d . . . . .
C40 C 0.6708(3) 0.4987(3) 0.45717(18) 0.0189(7) Uani 1 1 d . . . . .
H40 H 0.714812 0.554707 0.496155 0.023 Uiso 1 1 calc R . . . .
C41 C 0.5830(3) 0.5180(3) 0.42352(18) 0.0177(7) Uani 1 1 d . . . . .
C42 C 0.5174(3) 0.4344(3) 0.36513(18) 0.0170(7) Uani 1 1 d . . . . .
H42 H 0.460226 0.450646 0.343263 0.020 Uiso 1 1 calc R . . . .
C43 C 0.7846(3) 0.3669(3) 0.46368(19) 0.0247(8) Uani 1 1 d . . . . .
C44 C 0.5634(3) 0.6335(3) 0.4484(2) 0.0226(8) Uani 1 1 d . . . . .
C45 C 0.3423(3) 0.2331(3) 0.24893(18) 0.0157(7) Uani 1 1 d . . . . .
C46 C 0.2882(3) 0.1963(3) 0.18040(18) 0.0158(7) Uani 1 1 d . . . . .
H46 H 0.327979 0.178994 0.142943 0.019 Uiso 1 1 calc R . . . .
C47 C 0.1773(3) 0.1848(3) 0.16622(19) 0.0185(7) Uani 1 1 d . . . . .
C48 C 0.1144(3) 0.2070(3) 0.21996(19) 0.0205(7) Uani 1 1 d . . . . .
H48 H 0.039988 0.198586 0.210448 0.025 Uiso 1 1 calc R . . . .
C49 C 0.1652(3) 0.2421(3) 0.28864(19) 0.0191(7) Uani 1 1 d . . . . .
C50 C 0.2765(3) 0.2558(3) 0.30294(18) 0.0160(7) Uani 1 1 d . . . . .
H50 H 0.308485 0.280707 0.349493 0.019 Uiso 1 1 calc R . . . .
C51 C 0.1250(3) 0.1452(4) 0.0913(2) 0.0280(8) Uani 1 1 d . U . . .
C52 C 0.0964(3) 0.2635(3) 0.3467(2) 0.0236(8) Uani 1 1 d . . . . .
B1 B 0.4694(3) 0.2316(3) 0.2643(2) 0.0146(7) Uani 1 1 d . . . . .
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-11 16 -9 0.1170
-1 -17 12 0.1140
14 7 -7 0.1828
17 -10 3 0.2074
1 -1 27 0.0608
-1 1 -27 0.0608
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
O1 Ir1 C13 78.87(12) . .
O1 Ir1 C14 115.08(12) . .
O1 Ir1 C17 111.45(12) . .
O1 Ir1 C18 75.59(12) . .
N1 Ir1 O1 85.93(10) . .
N1 Ir1 N3 81.49(11) . .
N1 Ir1 C13 93.48(13) . .
N1 Ir1 C14 99.21(13) . .
N1 Ir1 C17 161.76(13) . .
N1 Ir1 C18 161.31(13) . .
N3 Ir1 O1 86.16(10) . .
N3 Ir1 C13 164.53(13) . .
N3 Ir1 C14 158.77(13) . .
N3 Ir1 C17 93.76(12) . .
N3 Ir1 C18 99.74(13) . .
C13 Ir1 C14 36.41(14) . .
C13 Ir1 C17 95.31(14) . .
C13 Ir1 C18 80.41(14) . .
C17 Ir1 C14 78.92(14) . .
C18 Ir1 C14 86.37(14) . .
C18 Ir1 C17 36.82(14) . .
C1 O1 Ir1 122.1(2) . .
N2 N1 Ir1 117.2(2) . .
C5 N1 Ir1 136.6(3) . .
C5 N1 N2 106.1(3) . .
N1 N2 C2 119.9(3) . .
C3 N2 N1 110.6(3) . .
C3 N2 C2 128.8(3) . .
N4 N3 Ir1 116.6(2) . .
C10 N3 Ir1 136.6(2) . .
C10 N3 N4 106.4(3) . .
N3 N4 C2 120.1(3) . .
C8 N4 N3 110.3(3) . .
C8 N4 C2 127.9(3) . .
O1 C1 C2 115.4(3) . .
O2 C1 O1 126.9(3) . .
O2 C1 C2 117.8(3) . .
N2 C2 C1 111.6(3) . .
N2 C2 H2 108.4 . .
N4 C2 N2 109.6(3) . .
N4 C2 C1 110.4(3) . .
N4 C2 H2 108.4 . .
C1 C2 H2 108.4 . .
N2 C3 C4 106.0(3) . .
N2 C3 C6 122.6(4) . .
C4 C3 C6 131.2(4) . .
C3 C4 H4A 110.1 . .
C3 C4 H4B 110.1 . .
C3 C4 C5 107.9(4) . .
H4A C4 H4B 108.4 . .
C5 C4 H4A 110.1 . .
C5 C4 H4B 110.1 . .
N1 C5 C4 109.3(4) . .
N1 C5 C7 123.3(3) . .
C4 C5 C7 127.4(4) . .
C3 C6 H6A 109.5 . .
C3 C6 H6B 109.5 . .
C3 C6 H6C 109.5 . .
H6A C6 H6B 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C5 C7 H7A 109.5 . .
C5 C7 H7B 109.5 . .
C5 C7 H7C 109.5 . .
H7A C7 H7B 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
N4 C8 C9 106.4(3) . .
N4 C8 C11 122.3(3) . .
C9 C8 C11 131.2(4) . .
C8 C9 H9 126.2 . .
C8 C9 C10 107.6(3) . .
C10 C9 H9 126.2 . .
N3 C10 C9 109.3(3) . .
N3 C10 C12 124.0(3) . .
C9 C10 C12 126.6(3) . .
C8 C11 H11A 109.5 . .
C8 C11 H11B 109.5 . .
C8 C11 H11C 109.5 . .
H11A C11 H11B 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C10 C12 H12A 109.5 . .
C10 C12 H12B 109.5 . .
C10 C12 H12C 109.5 . .
H12A C12 H12B 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
Ir1 C13 H13 114.1 . .
C14 C13 Ir1 73.4(2) . .
C14 C13 H13 114.1 . .
C14 C13 C20 124.5(3) . .
C20 C13 Ir1 109.2(2) . .
C20 C13 H13 114.1 . .
Ir1 C14 H14 114.1 . .
C13 C14 Ir1 70.2(2) . .
C13 C14 H14 114.1 . .
C13 C14 C15 123.5(3) . .
C15 C14 Ir1 113.3(2) . .
C15 C14 H14 114.1 . .
C14 C15 H15A 109.1 . .
C14 C15 H15B 109.1 . .
C14 C15 C16 112.5(3) . .
H15A C15 H15B 107.8 . .
C16 C15 H15A 109.1 . .
C16 C15 H15B 109.1 . .
C15 C16 H16A 109.0 . .
C15 C16 H16B 109.0 . .
H16A C16 H16B 107.8 . .
C17 C16 C15 113.0(3) . .
C17 C16 H16A 109.0 . .
C17 C16 H16B 109.0 . .
Ir1 C17 H17 114.2 . .
C16 C17 Ir1 110.6(2) . .
C16 C17 H17 114.2 . .
C18 C17 Ir1 70.4(2) . .
C18 C17 C16 124.9(3) . .
C18 C17 H17 114.2 . .
Ir1 C18 H18 113.4 . .
C17 C18 Ir1 72.7(2) . .
C17 C18 H18 113.4 . .
C17 C18 C19 124.7(3) . .
C19 C18 Ir1 112.4(2) . .
C19 C18 H18 113.4 . .
C18 C19 H19A 108.9 . .
C18 C19 H19B 108.9 . .
C18 C19 C20 113.5(3) . .
H19A C19 H19B 107.7 . .
C20 C19 H19A 108.9 . .
C20 C19 H19B 108.9 . .
C13 C20 C19 113.3(3) . .
C13 C20 H20A 108.9 . .
C13 C20 H20B 108.9 . .
C19 C20 H20A 108.9 . .
C19 C20 H20B 108.9 . .
H20A C20 H20B 107.7 . .
Cl3 C54 H54A 109.3 . .
Cl3 C54 H54B 109.3 . .
Cl4 C54 Cl3 111.6(3) . .
Cl4 C54 H54A 109.3 . .
Cl4 C54 H54B 109.3 . .
H54A C54 H54B 108.0 . .
C55 Cl5 C55 54.5(8) . 2_655
Cl5 C55 Cl5 125.5(8) . 2_655
Cl5 C55 H55A 106.0 2_655 .
Cl5 C55 H55A 106.0 . .
Cl5 C55 H55B 106.0 2_655 .
Cl5 C55 H55B 106.0 . .
H55A C55 H55B 106.3 . .
Cl1 C53 Cl2 112.2(3) . .
Cl1 C53 H53A 109.2 . .
Cl1 C53 H53B 109.2 . .
Cl2 C53 H53A 109.2 . .
Cl2 C53 H53B 109.2 . .
H53A C53 H53B 107.9 . .
C22 C21 B1 120.9(3) . .
C26 C21 C22 115.8(3) . .
C26 C21 B1 123.1(3) . .
C21 C22 H22 118.9 . .
C23 C22 C21 122.2(4) . .
C23 C22 H22 118.9 . .
C22 C23 C27 120.8(4) . .
C24 C23 C22 120.4(4) . .
C24 C23 C27 118.8(4) . .
C23 C24 H24 120.5 . .
C25 C24 C23 119.0(4) . .
C25 C24 H24 120.5 . .
C24 C25 C26 120.4(4) . .
C24 C25 C28 120.4(4) . .
C26 C25 C28 119.2(4) . .
C21 C26 C25 122.2(4) . .
C21 C26 H26 118.9 . .
C25 C26 H26 118.9 . .
F1 C27 F2 103.7(4) . .
F1 C27 C23 112.7(5) . .
F2 C27 C23 112.7(4) . .
F3 C27 F1 108.4(5) . .
F3 C27 F2 105.2(5) . .
F3 C27 C23 113.5(4) . .
F4 C28 F5 108.1(7) . .
F4 C28 F6 107.9(8) . .
F4 C28 C25 112.5(6) . .
F4A C28 F5A 103.2(12) . .
F4A C28 F6A 105.9(10) . .
F4A C28 C25 116.2(8) . .
F5 C28 C25 111.0(5) . .
F5A C28 C25 114.9(6) . .
F6 C28 F5 105.1(8) . .
F6 C28 C25 111.8(5) . .
F6A C28 F5A 100.9(9) . .
F6A C28 C25 114.0(8) . .
C30 C29 B1 121.2(3) . .
C34 C29 C30 115.3(3) . .
C34 C29 B1 122.9(3) . .
C29 C30 H30 118.8 . .
C31 C30 C29 122.4(3) . .
C31 C30 H30 118.8 . .
C30 C31 C35 118.8(3) . .
C32 C31 C30 121.4(3) . .
C32 C31 C35 119.8(3) . .
C31 C32 H32 121.5 . .
C33 C32 C31 117.0(3) . .
C33 C32 H32 121.5 . .
C32 C33 C34 121.2(3) . .
C32 C33 C36 119.8(3) . .
C34 C33 C36 119.0(3) . .
C29 C34 H34 118.7 . .
C33 C34 C29 122.6(3) . .
C33 C34 H34 118.7 . .
F7 C35 C31 112.0(3) . .
F8 C35 F7 106.0(3) . .
F8 C35 F9 106.1(3) . .
F8 C35 C31 113.4(3) . .
F9 C35 F7 106.4(3) . .
F9 C35 C31 112.4(3) . .
F10 C36 F11 107.8(3) . .
F10 C36 F12 106.2(3) . .
F10 C36 C33 113.5(3) . .
F11 C36 C33 111.6(3) . .
F12 C36 F11 104.9(3) . .
F12 C36 C33 112.4(3) . .
C38 C37 B1 120.2(3) . .
C42 C37 C38 115.8(3) . .
C42 C37 B1 123.3(3) . .
C37 C38 H38 119.0 . .
C39 C38 C37 122.0(3) . .
C39 C38 H38 119.0 . .
C38 C39 C43 118.1(3) . .
C40 C39 C38 121.3(3) . .
C40 C39 C43 120.6(3) . .
C39 C40 H40 121.2 . .
C39 C40 C41 117.7(3) . .
C41 C40 H40 121.2 . .
C40 C41 C42 121.2(3) . .
C40 C41 C44 118.9(3) . .
C42 C41 C44 119.8(3) . .
C37 C42 H42 119.0 . .
C41 C42 C37 122.1(3) . .
C41 C42 H42 119.0 . .
F13 C43 F15 105.5(3) . .
F13 C43 C39 113.5(3) . .
F14 C43 F13 107.6(3) . .
F14 C43 F15 105.8(3) . .
F14 C43 C39 112.4(3) . .
F15 C43 C39 111.6(3) . .
F16 C44 F17 106.4(3) . .
F16 C44 C41 113.4(3) . .
F17 C44 C41 112.0(3) . .
F18 C44 F16 105.7(3) . .
F18 C44 F17 105.6(3) . .
F18 C44 C41 113.1(3) . .
C46 C45 C50 115.6(3) . .
C46 C45 B1 121.5(3) . .
C50 C45 B1 122.3(3) . .
C45 C46 H46 118.8 . .
C47 C46 C45 122.4(3) . .
C47 C46 H46 118.8 . .
C46 C47 C51 119.3(3) . .
C48 C47 C46 120.9(3) . .
C48 C47 C51 119.8(3) . .
C47 C48 H48 120.9 . .
C47 C48 C49 118.2(3) . .
C49 C48 H48 120.9 . .
C48 C49 C52 118.1(3) . .
C50 C49 C48 121.0(3) . .
C50 C49 C52 121.0(3) . .
C45 C50 H50 119.1 . .
C49 C50 C45 121.9(3) . .
C49 C50 H50 119.1 . .
F19 C51 F20 109.0(6) . .
F19 C51 F21 105.8(5) . .
F19 C51 C47 113.2(4) . .
F19A C51 C47 110.9(6) . .
F20 C51 F21 103.8(5) . .
F20 C51 C47 112.4(4) . .
F20A C51 F19A 104.2(12) . .
F20A C51 F21A 109.2(16) . .
F20A C51 C47 119.3(8) . .
F21 C51 C47 112.0(4) . .
F21A C51 F19A 99.3(13) . .
F21A C51 C47 111.8(9) . .
F22 C52 F23 104.8(3) . .
F22 C52 C49 112.6(3) . .
F23 C52 C49 112.8(3) . .
F24 C52 F22 106.6(3) . .
F24 C52 F23 105.9(3) . .
F24 C52 C49 113.5(3) . .
C21 B1 C29 111.8(3) . .
C37 B1 C21 111.4(3) . .
C37 B1 C29 103.2(3) . .
C45 B1 C21 104.0(3) . .
C45 B1 C29 112.7(3) . .
C45 B1 C37 113.9(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ir1 O1 2.175(2) .
Ir1 N1 2.073(3) .
Ir1 N3 2.098(3) .
Ir1 C13 2.192(3) .
Ir1 C14 2.232(4) .
Ir1 C17 2.225(4) .
Ir1 C18 2.195(4) .
O1 C1 1.265(4) .
O2 C1 1.224(4) .
N1 N2 1.378(4) .
N1 C5 1.336(5) .
N2 C2 1.452(4) .
N2 C3 1.359(5) .
N3 N4 1.376(4) .
N3 C10 1.331(5) .
N4 C2 1.451(4) .
N4 C8 1.355(5) .
C1 C2 1.540(5) .
C2 H2 0.9800 .
C3 C4 1.368(6) .
C3 C6 1.493(6) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C4 C5 1.387(6) .
C5 C7 1.485(6) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 C9 1.365(5) .
C8 C11 1.484(6) .
C9 H9 0.9300 .
C9 C10 1.390(5) .
C10 C12 1.489(5) .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 H13 0.9800 .
C13 C14 1.382(5) .
C13 C20 1.513(5) .
C14 H14 0.9800 .
C14 C15 1.529(5) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C15 C16 1.532(5) .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C16 C17 1.508(5) .
C17 H17 0.9800 .
C17 C18 1.396(5) .
C18 H18 0.9800 .
C18 C19 1.521(5) .
C19 H19A 0.9700 .
C19 H19B 0.9700 .
C19 C20 1.528(5) .
C20 H20A 0.9700 .
C20 H20B 0.9700 .
Cl3 C54 1.755(5) .
Cl4 C54 1.742(5) .
C54 H54A 0.9700 .
C54 H54B 0.9700 .
Cl5 C55 1.595(11) .
Cl5 C55 1.662(14) 2_655
C55 H55A 0.9700 .
C55 H55B 0.9700 .
Cl1 C53 1.736(5) .
Cl2 C53 1.754(5) .
C53 H53A 0.9700 .
C53 H53B 0.9700 .
F1 C27 1.323(6) .
F2 C27 1.333(5) .
F3 C27 1.303(7) .
F4 C28 1.297(9) .
F4A C28 1.299(13) .
F5 C28 1.324(9) .
F5A C28 1.363(14) .
F6 C28 1.303(10) .
F6A C28 1.321(11) .
F7 C35 1.342(4) .
F8 C35 1.334(4) .
F9 C35 1.342(5) .
F10 C36 1.324(4) .
F11 C36 1.338(5) .
F12 C36 1.333(5) .
F13 C43 1.326(4) .
F14 C43 1.324(5) .
F15 C43 1.349(5) .
F16 C44 1.329(4) .
F17 C44 1.329(5) .
F18 C44 1.328(4) .
F19 C51 1.302(7) .
F19A C51 1.334(12) .
F20 C51 1.308(6) .
F20A C51 1.205(12) .
F21 C51 1.329(6) .
F21A C51 1.277(17) .
F22 C52 1.332(5) .
F23 C52 1.336(4) .
F24 C52 1.326(5) .
C21 C22 1.401(5) .
C21 C26 1.392(5) .
C21 B1 1.642(5) .
C22 H22 0.9300 .
C22 C23 1.391(6) .
C23 C24 1.379(7) .
C23 C27 1.487(6) .
C24 H24 0.9300 .
C24 C25 1.374(7) .
C25 C26 1.400(5) .
C25 C28 1.495(7) .
C26 H26 0.9300 .
C29 C30 1.396(5) .
C29 C34 1.395(5) .
C29 B1 1.643(5) .
C30 H30 0.9300 .
C30 C31 1.391(5) .
C31 C32 1.389(5) .
C31 C35 1.490(5) .
C32 H32 0.9300 .
C32 C33 1.389(5) .
C33 C34 1.390(5) .
C33 C36 1.499(5) .
C34 H34 0.9300 .
C37 C38 1.403(5) .
C37 C42 1.399(5) .
C37 B1 1.635(5) .
C38 H38 0.9300 .
C38 C39 1.389(5) .
C39 C40 1.382(5) .
C39 C43 1.498(5) .
C40 H40 0.9300 .
C40 C41 1.389(5) .
C41 C42 1.390(5) .
C41 C44 1.499(5) .
C42 H42 0.9300 .
C45 C46 1.398(5) .
C45 C50 1.409(5) .
C45 B1 1.634(5) .
C46 H46 0.9300 .
C46 C47 1.388(5) .
C47 C48 1.379(5) .
C47 C51 1.500(5) .
C48 H48 0.9300 .
C48 C49 1.388(5) .
C49 C50 1.387(5) .
C49 C52 1.494(5) .
C50 H50 0.9300 .
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-11.0000 15.9999 -9.0001 0.0141 0.0023 0.9796
-1.0000 -16.9999 12.0005 0.0608 0.6497 -0.7279
14.0000 7.0000 -7.0006 -0.1264 -0.9631 -0.0372
17.0000 -9.9999 2.9998 -0.0443 -0.5255 -0.8598
1.0000 -1.0000 26.9987 -0.9774 0.1239 -0.1518
-1.0000 1.0000 -26.9987 0.9774 -0.1239 0.1518
