# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
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#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
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#  except for the purpose of generating routine backup copies
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data_1-prime
#==============================================================================
_audit_creation_date             14-05-02
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 045np12
_chemical_name_systematic        .
_chemical_melting_point          'not measured'

_refine_special_details          
;
The structure was found to be twinned by rotation about the direct a-axis.
However, as the space group was non-centrosymmetric, the possibility that 
both components were racemic twins ('conglomerates') needed to be considered.

An attempt was made to treat the crystal as a four-component twin with the 
following twin laws:
1(Identity)

2(Inversion)                 (h') (-1      0      0) (h)
                             (k')=(0      -1      0).(k)
                             (l') (0       0     -1) (l) 

3(Rotation about a)          (h') (1       0      0) (h)
                             (k')=(0      -1      0).(k)
                             (l') (-0.235  0     -1) (l) 

4(Reflection about (1 0 0))  (h') (-1      0      0) (h)
                             (k')=(0       1      0).(k)
                             (l') (0.235   0      1) (l)

(Component 2 is distinguishable from the primary component only as a result
of anomalous scattering, and similarly components 3 and 4 are distinguishable 
as a result of anomalous scattering,) 

Refinement of the relative contributions of the four components was unstable 
due to the small amount of minor twin component.  For this reason, the only 
scale factors for components 1, 2 and 3 were refined which converged readily
to give 0.540(12), 0.411(12) and 0.0498(15) respectively.
         

Note that the Flack or Rogers parameters conventionally used as measures of 
correctness of absolute structure are inappropriate in this context.

The largest residual electron density peaks are close to the heavy 
element (Ir).
;


_cell_length_a                   9.0172(3)
_cell_length_b                   15.0295(6)
_cell_length_c                   12.2995(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.9522(17)
_cell_angle_gamma                90
_cell_volume                     1660.66(11)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1 '
_symmetry_space_group_name_Hall  'P 2yb'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y+1/2,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ir -1.4442 7.9887 27.3049 1.5928 16.7296 8.8655 15.6115 0.4179 5.8338 45.0011
11.4722 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C40 H46 Ir1 N4 
# Dc =      1.55 Fooo =    782.00 Mu =     40.55 M =    775.05
# Found Formula = C40 H46 Ir1 N4 
# Dc =      1.55 FOOO =    782.00 Mu =     40.55 M =    775.05

_chemical_formula_sum            'C40 H46 Ir1 N4'
_chemical_formula_moiety         'C40 H46 Ir1 N4'
_chemical_compound_source        .
_chemical_formula_weight         775.05


_cell_measurement_reflns_used    3727
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       lath
_exptl_crystal_colour            red
_exptl_crystal_size_min          0.02
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_max          0.24

_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             782
_exptl_absorpt_coefficient_mu    4.055

# Sheldrick geometric approximatio 0.78 0.92 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_T_max  0.92
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            15631
_reflns_number_total             7051
_diffrn_reflns_av_R_equivalents  0.090
# Number of reflections without Friedels Law is 7051 
# Number of reflections with Friedels Law is 3917 
# Theoretical number of reflections is about 3811 


_diffrn_reflns_theta_min         5.149
_diffrn_reflns_theta_max         27.489
_diffrn_measured_fraction_theta_max 0.990

_diffrn_reflns_theta_full        26.939
_diffrn_measured_fraction_theta_full 0.991


_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       15
_reflns_limit_h_min              -11
_reflns_limit_h_max              11
_reflns_limit_k_min              -18
_reflns_limit_k_max              19
_reflns_limit_l_min              0
_reflns_limit_l_max              15

_oxford_diffrn_Wilson_B_factor   2.12
_oxford_diffrn_Wilson_scale      82.33

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -5.76
_refine_diff_density_max         6.96


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         7050
_refine_ls_number_restraints     1
_refine_ls_number_parameters     408
_oxford_refine_ls_R_factor_ref   0.0877
_refine_ls_wR_factor_ref         0.0946
_refine_ls_goodness_of_fit_ref   0.9235
_refine_ls_shift/su_max          0.0003711
_refine_ls_shift/su_mean         0.0000168


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        7050
_refine_ls_R_factor_all          0.0877
_refine_ls_wR_factor_all         0.0946

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5113
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_gt          0.0832

# The Flack parameter was determined before Friedel pairs were merged 
_refine_ls_abs_structure_Flack   0.437(14)
_refine_ls_abs_structure_details 'Flack (1983), 7051 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.00P)² + 4.21P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ir1 Ir 0.26515(3) 0.50006(14) 0.28473(2) 0.0255 1.0000 Uani . . . . . .
C2 C 0.2210(13) 0.6288(8) 0.2760(8) 0.0277 1.0000 Uani . . . . . .
N3 N 0.2620(16) 0.6746(11) 0.3679(13) 0.0293 1.0000 Uani . . . . . .
C4 C 0.2623(18) 0.7724(12) 0.3789(15) 0.0290 1.0000 Uani . . . . . .
C5 C 0.2795(14) 0.8163(15) 0.2684(12) 0.0351 1.0000 Uani . . . . . .
C6 C 0.1567(12) 0.7793(7) 0.1877(9) 0.0392 1.0000 Uani . . . . . .
N7 N 0.1621(8) 0.6816(5) 0.1896(6) 0.0304 1.0000 Uani . . . . . .
C8 C 0.0960(10) 0.6369(6) 0.0941(7) 0.0283 1.0000 Uani . . . . . .
C9 C -0.0585(11) 0.6211(7) 0.0834(8) 0.0364 1.0000 Uani . . . . . .
C10 C -0.1197(14) 0.5788(8) -0.0075(10) 0.0523 1.0000 Uani . . . . . .
C11 C -0.0330(18) 0.5558(9) -0.0908(10) 0.0662 1.0000 Uani . . . . . .
C12 C 0.1147(16) 0.5770(8) -0.0836(8) 0.0519 1.0000 Uani . . . . . .
C13 C 0.176(2) 0.6190(10) 0.0076(14) 0.0365 1.0000 Uani . . . . . .
C14 C 0.347(2) 0.6356(14) 0.0209(19) 0.0586 1.0000 Uani . . . . . .
C15 C -0.1535(11) 0.6467(8) 0.1739(9) 0.0509 1.0000 Uani . . . . . .
C16 C 0.3329(10) 0.6227(7) 0.4536(8) 0.0294 1.0000 Uani . . . . . .
C17 C 0.2847(12) 0.6267(7) 0.5574(8) 0.0325 1.0000 Uani . . . . . .
C18 C 0.3577(11) 0.5745(7) 0.6394(9) 0.0423 1.0000 Uani . . . . . .
C19 C 0.4770(10) 0.5203(10) 0.6192(9) 0.0488 1.0000 Uani . . . . . .
C20 C 0.5234(9) 0.5153(11) 0.5169(8) 0.0399 1.0000 Uani . . . . . .
C21 C 0.4555(10) 0.5677(6) 0.4289(8) 0.0314 1.0000 Uani . . . . . .
C22 C 0.4864(10) 0.5551(7) 0.3135(8) 0.0358 1.0000 Uani . . . . . .
C23 C 0.1479(13) 0.6769(9) 0.5794(11) 0.0414 1.0000 Uani . . . . . .
C24 C 0.3028(13) 0.3689(9) 0.2981(9) 0.0296 1.0000 Uani . . . . . .
N25 N 0.2539(16) 0.3223(12) 0.3851(13) 0.0295 1.0000 Uani . . . . . .
C26 C 0.257(2) 0.2246(12) 0.4000(17) 0.0376 1.0000 Uani . . . . . .
C27 C 0.2308(16) 0.1834(13) 0.2887(12) 0.0348 1.0000 Uani . . . . . .
C28 C 0.3486(12) 0.2162(7) 0.2190(9) 0.0390 1.0000 Uani . . . . . .
N29 N 0.3560(8) 0.3147(5) 0.2229(6) 0.0282 1.0000 Uani . . . . . .
C30 C 0.4260(10) 0.3521(7) 0.1330(8) 0.0312 1.0000 Uani . . . . . .
C31 C 0.3433(18) 0.3647(12) 0.0314(15) 0.0361 1.0000 Uani . . . . . .
C32 C 0.1830(19) 0.3497(10) 0.0208(15) 0.0433 1.0000 Uani . . . . . .
C33 C 0.4166(13) 0.4007(7) -0.0513(9) 0.0423 1.0000 Uani . . . . . .
C34 C 0.5677(12) 0.4178(8) -0.0384(9) 0.0481 1.0000 Uani . . . . . .
C35 C 0.6486(12) 0.3996(7) 0.0586(9) 0.0422 1.0000 Uani . . . . . .
C36 C 0.5791(11) 0.3657(7) 0.1463(8) 0.0357 1.0000 Uani . . . . . .
C37 C 0.6696(12) 0.3418(8) 0.2502(9) 0.0472 1.0000 Uani . . . . . .
C38 C 0.1648(10) 0.3734(6) 0.4570(7) 0.0251 1.0000 Uani . . . . . .
C39 C 0.1892(15) 0.3617(8) 0.5708(10) 0.0306 1.0000 Uani . . . . . .
C40 C 0.3148(11) 0.3066(8) 0.6240(8) 0.0451 1.0000 Uani . . . . . .
C41 C 0.0926(11) 0.4064(7) 0.6373(9) 0.0425 1.0000 Uani . . . . . .
C42 C -0.0183(11) 0.4614(7) 0.5914(9) 0.0447 1.0000 Uani . . . . . .
C43 C -0.0390(10) 0.4737(7) 0.4793(8) 0.0437 1.0000 Uani . . . . . .
C44 C 0.0515(10) 0.4322(7) 0.4089(8) 0.0326 1.0000 Uani . . . . . .
C45 C 0.0479(10) 0.4522(7) 0.2921(8) 0.0408 1.0000 Uani . . . . . .
H11 H 0.3337 0.5025 0.1615 0.0390 1.0000 Uiso R . . . . .
H41 H 0.1698 0.7929 0.4055 0.0358 1.0000 Uiso R . . . . .
H42 H 0.3463 0.7893 0.4300 0.0359 1.0000 Uiso R . . . . .
H51 H 0.2713 0.8804 0.2733 0.0379 1.0000 Uiso R . . . . .
H52 H 0.3769 0.7999 0.2446 0.0380 1.0000 Uiso R . . . . .
H61 H 0.1709 0.7999 0.1144 0.0427 1.0000 Uiso R . . . . .
H62 H 0.0599 0.7993 0.2088 0.0431 1.0000 Uiso R . . . . .
H101 H -0.2207 0.5653 -0.0145 0.0631 1.0000 Uiso R . . . . .
H111 H -0.0744 0.5247 -0.1521 0.0771 1.0000 Uiso R . . . . .
H121 H 0.1721 0.5639 -0.1412 0.0622 1.0000 Uiso R . . . . .
H141 H 0.3928 0.6066 -0.0367 0.0930 1.0000 Uiso R . . . . .
H142 H 0.3875 0.6126 0.0899 0.0928 1.0000 Uiso R . . . . .
H143 H 0.3657 0.6981 0.0183 0.0928 1.0000 Uiso R . . . . .
H153 H -0.2407 0.6093 0.1732 0.0773 1.0000 Uiso R . . . . .
H152 H -0.1840 0.7076 0.1645 0.0771 1.0000 Uiso R . . . . .
H151 H -0.0936 0.6408 0.2428 0.0768 1.0000 Uiso R . . . . .
H181 H 0.3234 0.5758 0.7087 0.0530 1.0000 Uiso R . . . . .
H191 H 0.5267 0.4881 0.6762 0.0601 1.0000 Uiso R . . . . .
H201 H 0.6006 0.4765 0.5037 0.0511 1.0000 Uiso R . . . . .
H221 H 0.5609 0.5107 0.3000 0.0423 1.0000 Uiso R . . . . .
H222 H 0.4984 0.6094 0.2732 0.0429 1.0000 Uiso R . . . . .
H231 H 0.1117 0.6563 0.6463 0.0651 1.0000 Uiso R . . . . .
H232 H 0.0718 0.6672 0.5206 0.0648 1.0000 Uiso R . . . . .
H233 H 0.1703 0.7392 0.5850 0.0648 1.0000 Uiso R . . . . .
H261 H 0.2772 0.1951 0.4651 0.0495 1.0000 Uiso R . . . . .
H271 H 0.2362 0.1191 0.2957 0.0390 1.0000 Uiso R . . . . .
H272 H 0.1328 0.2007 0.2568 0.0389 1.0000 Uiso R . . . . .
H281 H 0.3239 0.1975 0.1439 0.0478 1.0000 Uiso R . . . . .
H282 H 0.4446 0.1913 0.2463 0.0480 1.0000 Uiso R . . . . .
H323 H 0.1435 0.3680 -0.0511 0.0698 1.0000 Uiso R . . . . .
H322 H 0.1601 0.2878 0.0313 0.0700 1.0000 Uiso R . . . . .
H321 H 0.1387 0.3851 0.0742 0.0701 1.0000 Uiso R . . . . .
H331 H 0.3619 0.4150 -0.1169 0.0520 1.0000 Uiso R . . . . .
H341 H 0.6146 0.4421 -0.0963 0.0568 1.0000 Uiso R . . . . .
H351 H 0.7512 0.4098 0.0655 0.0520 1.0000 Uiso R . . . . .
H373 H 0.7653 0.3703 0.2537 0.0689 1.0000 Uiso R . . . . .
H372 H 0.6837 0.2784 0.2521 0.0688 1.0000 Uiso R . . . . .
H371 H 0.6191 0.3596 0.3123 0.0690 1.0000 Uiso R . . . . .
H401 H 0.3366 0.3248 0.6989 0.0660 1.0000 Uiso R . . . . .
H402 H 0.2878 0.2446 0.6220 0.0661 1.0000 Uiso R . . . . .
H403 H 0.4027 0.3150 0.5855 0.0661 1.0000 Uiso R . . . . .
H411 H 0.1040 0.3993 0.7129 0.0510 1.0000 Uiso R . . . . .
H421 H -0.0814 0.4909 0.6363 0.0550 1.0000 Uiso R . . . . .
H431 H -0.1166 0.5100 0.4509 0.0500 1.0000 Uiso R . . . . .
H451 H 0.0272 0.4009 0.2469 0.0418 1.0000 Uiso R . . . . .
H452 H -0.0208 0.4997 0.2729 0.0418 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.11261(3)

loop_
_oxford_twin_element_scale_factors
0.540(12)
0.0498(15)
0.411(12)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ir1 . C2 . 1.976(12) yes
Ir1 . C21 . 2.569(10) yes
Ir1 . C22 . 2.161(9) yes
Ir1 . C24 . 2.005(14) yes
Ir1 . C45 . 2.096(10) yes
Ir1 . H11 . 1.686 no
C2 . N3 . 1.348(19) yes
C2 . N7 . 1.395(14) yes
N3 . C4 . 1.47(2) yes
N3 . C16 . 1.418(18) yes
C4 . C5 . 1.53(2) yes
C4 . H41 . 0.972 no
C4 . H42 . 0.976 no
C5 . C6 . 1.527(18) yes
C5 . H51 . 0.969 no
C5 . H52 . 0.981 no
C6 . N7 . 1.468(13) yes
C6 . H61 . 0.972 no
C6 . H62 . 0.979 no
N7 . C8 . 1.437(12) yes
C8 . C9 . 1.408(13) yes
C8 . C13 . 1.363(18) yes
C9 . C10 . 1.360(15) yes
C9 . C15 . 1.512(14) yes
C10 . C11 . 1.386(17) yes
C10 . H101 . 0.930 no
C11 . C12 . 1.365(18) yes
C11 . H111 . 0.937 no
C12 . C13 . 1.36(2) yes
C12 . H121 . 0.934 no
C13 . C14 . 1.55(2) yes
C14 . H141 . 0.956 no
C14 . H142 . 0.960 no
C14 . H143 . 0.956 no
C15 . H153 . 0.967 no
C15 . H152 . 0.960 no
C15 . H151 . 0.969 no
C16 . C17 . 1.385(13) yes
C16 . C21 . 1.434(13) yes
C17 . C18 . 1.397(15) yes
C17 . C23 . 1.491(13) yes
C18 . C19 . 1.388(15) yes
C18 . H181 . 0.932 no
C19 . C20 . 1.362(13) yes
C19 . H191 . 0.934 no
C20 . C21 . 1.432(15) yes
C20 . H201 . 0.933 no
C21 . C22 . 1.482(13) yes
C22 . H221 . 0.972 no
C22 . H222 . 0.965 no
C23 . H231 . 0.962 no
C23 . H232 . 0.964 no
C23 . H233 . 0.959 no
C24 . N25 . 1.382(18) yes
C24 . N29 . 1.350(13) yes
N25 . C26 . 1.48(2) yes
N25 . C38 . 1.463(18) yes
C26 . C27 . 1.50(2) yes
C26 . H261 . 0.919 no
C27 . C28 . 1.505(15) yes
C27 . H271 . 0.971 no
C27 . H272 . 0.972 no
C28 . N29 . 1.482(13) yes
C28 . H281 . 0.973 no
C28 . H282 . 0.976 no
N29 . C30 . 1.435(11) yes
C30 . C31 . 1.41(2) yes
C30 . C36 . 1.392(13) yes
C31 . C32 . 1.46(2) yes
C31 . C33 . 1.372(19) yes
C32 . H323 . 0.965 no
C32 . H322 . 0.964 no
C32 . H321 . 0.959 no
C33 . C34 . 1.382(14) yes
C33 . H331 . 0.933 no
C34 . C35 . 1.371(14) yes
C34 . H341 . 0.933 no
C35 . C36 . 1.389(14) yes
C35 . H351 . 0.934 no
C36 . C37 . 1.500(14) yes
C37 . H373 . 0.962 no
C37 . H372 . 0.961 no
C37 . H371 . 0.961 no
C38 . C39 . 1.409(14) yes
C38 . C44 . 1.438(13) yes
C39 . C40 . 1.506(15) yes
C39 . C41 . 1.416(16) yes
C40 . H401 . 0.965 no
C40 . H402 . 0.964 no
C40 . H403 . 0.966 no
C41 . C42 . 1.379(14) yes
C41 . H411 . 0.932 no
C42 . C43 . 1.388(14) yes
C42 . H421 . 0.937 no
C43 . C44 . 1.388(12) yes
C43 . H431 . 0.930 no
C44 . C45 . 1.465(13) yes
C45 . H451 . 0.959 no
C45 . H452 . 0.961 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . Ir1 . C21 . 76.7(4) yes
C2 . Ir1 . C22 . 79.2(4) yes
C21 . Ir1 . C22 . 35.2(3) yes
C2 . Ir1 . C24 . 177.5(4) yes
C21 . Ir1 . C24 . 103.5(4) yes
C22 . Ir1 . C24 . 102.5(4) yes
C2 . Ir1 . C45 . 98.8(4) yes
C21 . Ir1 . C45 . 132.6(3) yes
C22 . Ir1 . C45 . 167.8(4) yes
C24 . Ir1 . C45 . 79.1(4) yes
C2 . Ir1 . H11 . 91.0 no
C21 . Ir1 . H11 . 109.7 no
C22 . Ir1 . H11 . 74.6 no
C24 . Ir1 . H11 . 91.3 no
C45 . Ir1 . H11 . 117.6 no
Ir1 . C2 . N3 . 114.5(10) yes
Ir1 . C2 . N7 . 131.3(8) yes
N3 . C2 . N7 . 114.0(12) yes
C2 . N3 . C4 . 125.7(15) yes
C2 . N3 . C16 . 114.5(13) yes
C4 . N3 . C16 . 118.9(14) yes
N3 . C4 . C5 . 110.3(15) yes
N3 . C4 . H41 . 110.6 no
C5 . C4 . H41 . 108.5 no
N3 . C4 . H42 . 108.3 no
C5 . C4 . H42 . 109.0 no
H41 . C4 . H42 . 110.0 no
C4 . C5 . C6 . 107.3(13) yes
C4 . C5 . H51 . 111.1 no
C6 . C5 . H51 . 110.4 no
C4 . C5 . H52 . 108.6 no
C6 . C5 . H52 . 109.4 no
H51 . C5 . H52 . 110.1 no
C5 . C6 . N7 . 109.4(11) yes
C5 . C6 . H61 . 109.9 no
N7 . C6 . H61 . 109.1 no
C5 . C6 . H62 . 109.2 no
N7 . C6 . H62 . 109.3 no
H61 . C6 . H62 . 109.8 no
C6 . N7 . C2 . 126.3(9) yes
C6 . N7 . C8 . 116.3(8) yes
C2 . N7 . C8 . 117.4(8) yes
N7 . C8 . C9 . 119.5(8) yes
N7 . C8 . C13 . 121.3(10) yes
C9 . C8 . C13 . 118.7(11) yes
C8 . C9 . C10 . 118.9(10) yes
C8 . C9 . C15 . 120.5(9) yes
C10 . C9 . C15 . 120.6(10) yes
C9 . C10 . C11 . 120.6(11) yes
C9 . C10 . H101 . 120.2 no
C11 . C10 . H101 . 119.2 no
C10 . C11 . C12 . 120.2(11) yes
C10 . C11 . H111 . 120.6 no
C12 . C11 . H111 . 119.1 no
C11 . C12 . C13 . 119.1(12) yes
C11 . C12 . H121 . 120.2 no
C13 . C12 . H121 . 120.7 no
C8 . C13 . C12 . 121.9(14) yes
C8 . C13 . C14 . 118.3(14) yes
C12 . C13 . C14 . 119.3(15) yes
C13 . C14 . H141 . 109.8 no
C13 . C14 . H142 . 109.6 no
H141 . C14 . H142 . 109.6 no
C13 . C14 . H143 . 109.4 no
H141 . C14 . H143 . 109.4 no
H142 . C14 . H143 . 109.1 no
C9 . C15 . H153 . 110.9 no
C9 . C15 . H152 . 109.2 no
H153 . C15 . H152 . 109.3 no
C9 . C15 . H151 . 108.2 no
H153 . C15 . H151 . 110.2 no
H152 . C15 . H151 . 109.0 no
N3 . C16 . C17 . 120.2(10) yes
N3 . C16 . C21 . 117.8(10) yes
C17 . C16 . C21 . 121.9(10) yes
C16 . C17 . C18 . 118.4(10) yes
C16 . C17 . C23 . 121.3(11) yes
C18 . C17 . C23 . 119.9(10) yes
C17 . C18 . C19 . 121.6(10) yes
C17 . C18 . H181 . 118.4 no
C19 . C18 . H181 . 119.9 no
C18 . C19 . C20 . 120.1(12) yes
C18 . C19 . H191 . 120.0 no
C20 . C19 . H191 . 119.9 no
C19 . C20 . C21 . 121.5(12) yes
C19 . C20 . H201 . 119.3 no
C21 . C20 . H201 . 119.3 no
C16 . C21 . C20 . 116.4(9) yes
C16 . C21 . Ir1 . 83.8(5) yes
C20 . C21 . Ir1 . 121.4(8) yes
C16 . C21 . C22 . 119.2(9) yes
C20 . C21 . C22 . 123.4(9) yes
Ir1 . C21 . C22 . 57.2(5) yes
Ir1 . C22 . C21 . 87.6(5) yes
Ir1 . C22 . H221 . 110.5 no
C21 . C22 . H221 . 116.2 no
Ir1 . C22 . H222 . 112.5 no
C21 . C22 . H222 . 115.1 no
H221 . C22 . H222 . 112.5 no
C17 . C23 . H231 . 109.8 no
C17 . C23 . H232 . 109.5 no
H231 . C23 . H232 . 108.7 no
C17 . C23 . H233 . 109.5 no
H231 . C23 . H233 . 109.8 no
H232 . C23 . H233 . 109.5 no
Ir1 . C24 . N25 . 119.9(10) yes
Ir1 . C24 . N29 . 127.2(8) yes
N25 . C24 . N29 . 112.4(13) yes
C24 . N25 . C26 . 126.6(16) yes
C24 . N25 . C38 . 115.5(14) yes
C26 . N25 . C38 . 116.7(14) yes
N25 . C26 . C27 . 107.2(16) yes
N25 . C26 . H261 . 125.9 no
C27 . C26 . H261 . 126.8 no
C26 . C27 . C28 . 108.9(13) yes
C26 . C27 . H271 . 109.1 no
C28 . C27 . H271 . 110.1 no
C26 . C27 . H272 . 108.8 no
C28 . C27 . H272 . 110.1 no
H271 . C27 . H272 . 109.9 no
C27 . C28 . N29 . 109.9(11) yes
C27 . C28 . H281 . 109.3 no
N29 . C28 . H281 . 109.1 no
C27 . C28 . H282 . 109.0 no
N29 . C28 . H282 . 109.7 no
H281 . C28 . H282 . 109.8 no
C28 . N29 . C24 . 127.4(9) yes
C28 . N29 . C30 . 112.8(8) yes
C24 . N29 . C30 . 119.8(8) yes
N29 . C30 . C31 . 120.1(10) yes
N29 . C30 . C36 . 117.7(9) yes
C31 . C30 . C36 . 121.8(10) yes
C30 . C31 . C32 . 120.2(14) yes
C30 . C31 . C33 . 117.3(12) yes
C32 . C31 . C33 . 122.2(15) yes
C31 . C32 . H323 . 108.8 no
C31 . C32 . H322 . 111.1 no
H323 . C32 . H322 . 109.3 no
C31 . C32 . H321 . 108.8 no
H323 . C32 . H321 . 109.1 no
H322 . C32 . H321 . 109.7 no
C31 . C33 . C34 . 121.4(12) yes
C31 . C33 . H331 . 118.6 no
C34 . C33 . H331 . 119.9 no
C33 . C34 . C35 . 120.5(10) yes
C33 . C34 . H341 . 119.4 no
C35 . C34 . H341 . 120.0 no
C34 . C35 . C36 . 120.5(10) yes
C34 . C35 . H351 . 119.6 no
C36 . C35 . H351 . 119.9 no
C30 . C36 . C35 . 118.2(10) yes
C30 . C36 . C37 . 121.7(9) yes
C35 . C36 . C37 . 120.1(9) yes
C36 . C37 . H373 . 110.6 no
C36 . C37 . H372 . 108.6 no
H373 . C37 . H372 . 108.9 no
C36 . C37 . H371 . 110.6 no
H373 . C37 . H371 . 109.0 no
H372 . C37 . H371 . 109.1 no
N25 . C38 . C39 . 119.2(10) yes
N25 . C38 . C44 . 118.8(10) yes
C39 . C38 . C44 . 122.0(9) yes
C38 . C39 . C40 . 123.2(10) yes
C38 . C39 . C41 . 117.6(11) yes
C40 . C39 . C41 . 119.1(10) yes
C39 . C40 . H401 . 110.1 no
C39 . C40 . H402 . 110.0 no
H401 . C40 . H402 . 109.1 no
C39 . C40 . H403 . 109.4 no
H401 . C40 . H403 . 108.9 no
H402 . C40 . H403 . 109.2 no
C39 . C41 . C42 . 120.5(10) yes
C39 . C41 . H411 . 120.1 no
C42 . C41 . H411 . 119.4 no
C41 . C42 . C43 . 121.2(9) yes
C41 . C42 . H421 . 119.8 no
C43 . C42 . H421 . 119.0 no
C42 . C43 . C44 . 121.6(9) yes
C42 . C43 . H431 . 118.9 no
C44 . C43 . H431 . 119.5 no
C38 . C44 . C43 . 117.0(9) yes
C38 . C44 . C45 . 118.9(8) yes
C43 . C44 . C45 . 123.7(9) yes
C44 . C45 . Ir1 . 99.9(6) yes
C44 . C45 . H451 . 113.0 no
Ir1 . C45 . H451 . 112.7 no
C44 . C45 . H452 . 110.6 no
Ir1 . C45 . H452 . 108.6 no
H451 . C45 . H452 . 111.4 no
_database_code_depnum_ccdc_archive 'CCDC 1002300'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2.OEt2
#==============================================================================
_audit_creation_date             14-05-02
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 004npir11
_chemical_name_systematic        .
_chemical_melting_point          'not measured'

_cell_length_a                   17.3193(2)
_cell_length_b                   18.8464(2)
_cell_length_c                   15.1207(1)
_cell_angle_alpha                90
_cell_angle_beta                 96.00
_cell_angle_gamma                90
_cell_volume                     4908.44(8)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1 '
_symmetry_space_group_name_Hall  '-P 2ybc '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ir -1.4442 7.9887 27.3049 1.5928 16.7296 8.8655 15.6115 0.4179 5.8338 45.0011
11.4722 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C54 H76 Cl1 Ir1 N4 O1 
# Dc =      1.39 Fooo =   2120.00 Mu =     28.16 M =   1024.90
# Found Formula = C54 H76 Cl1 Ir1 N4 O1 
# Dc =      1.39 FOOO =   2120.00 Mu =     28.16 M =   1024.90

_chemical_formula_sum            'C54 H76 Cl1 Ir1 N4 O1'
_chemical_formula_moiety         'C54 H76 Cl1 Ir1 N4 O1'
_chemical_compound_source        .
_chemical_formula_weight         1024.90


_cell_measurement_reflns_used    11413
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.140
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.240

_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2120
_exptl_absorpt_coefficient_mu    2.816

# Sheldrick geometric approximatio 0.57 0.67 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_T_max  0.67
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            69693
_reflns_number_total             11168
_diffrn_reflns_av_R_equivalents  0.050
# Number of reflections without Friedels Law is 21917 
# Number of reflections with Friedels Law is 11168 
# Theoretical number of reflections is about 11238 


_diffrn_reflns_theta_min         5.098
_diffrn_reflns_theta_max         27.466
_diffrn_measured_fraction_theta_max 0.992

_diffrn_reflns_theta_full        26.917
_diffrn_measured_fraction_theta_full 0.993


_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_reflns_limit_h_min              0
_reflns_limit_h_max              22
_reflns_limit_k_min              -24
_reflns_limit_k_max              0
_reflns_limit_l_min              -19
_reflns_limit_l_max              19

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.54
_refine_diff_density_max         3.01


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         11166
_refine_ls_number_restraints     0
_refine_ls_number_parameters     550
_oxford_refine_ls_R_factor_ref   0.0659
_refine_ls_wR_factor_ref         0.0745
_refine_ls_goodness_of_fit_ref   0.9719
_refine_ls_shift/su_max          0.0008328
_refine_ls_shift/su_mean         0.0000189


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        11167
_refine_ls_R_factor_all          0.0659
_refine_ls_wR_factor_all         0.0745

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                8087
_refine_ls_R_factor_gt           0.0356
_refine_ls_wR_factor_gt          0.0566

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 2.86 2.56 0.630 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ir1 Ir 0.309089(11) 0.427136(10) 0.733999(12) 0.0196 1.0000 Uani . . . . . .
Cl2 Cl 0.36250(7) 0.43849(6) 0.59683(7) 0.0297 1.0000 Uani . . . . . .
C55 C 0.2286(3) 0.3908(3) 0.8217(3) 0.0279 1.0000 Uani . . . . . .
C56 C 0.2940(3) 0.4225(3) 0.8719(3) 0.0247 1.0000 Uani . . . . . .
C58 C 0.2845(3) 0.4881(3) 0.9268(3) 0.0312 1.0000 Uani . . . . . .
C51 C 0.2578(4) 0.4727(3) 1.0189(4) 0.0395 1.0000 Uani . . . . . .
C57 C 0.1475(3) 0.4188(3) 0.8181(3) 0.0319 1.0000 Uani . . . . . .
C54 C 0.3094(3) 0.5373(2) 0.7348(4) 0.0234 1.0000 Uani . . . . . .
N9 N 0.2508(2) 0.5857(2) 0.7305(3) 0.0263 1.0000 Uani . . . . . .
C53 C 0.2766(3) 0.6584(3) 0.7108(4) 0.0348 1.0000 Uani . . . . . .
C11 C 0.3630(3) 0.6535(3) 0.7408(4) 0.0350 1.0000 Uani . . . . . .
N12 N 0.3762(2) 0.5760(3) 0.7336(3) 0.0255 1.0000 Uani . . . . . .
C52 C 0.4538(3) 0.5564(2) 0.7187(3) 0.0258 1.0000 Uani . . . . . .
C14 C 0.5066(3) 0.5303(3) 0.7871(3) 0.0264 1.0000 Uani . . . . . .
C15 C 0.4820(3) 0.5118(3) 0.8774(3) 0.0372 1.0000 Uani . . . . . .
C16 C 0.5840(3) 0.5219(3) 0.7720(4) 0.0318 1.0000 Uani . . . . . .
C17 C 0.6094(3) 0.5388(3) 0.6905(4) 0.0345 1.0000 Uani . . . . . .
C18 C 0.5554(3) 0.5633(3) 0.6231(3) 0.0360 1.0000 Uani . . . . . .
C19 C 0.4785(3) 0.5726(3) 0.6352(3) 0.0305 1.0000 Uani . . . . . .
C20 C 0.4237(4) 0.6003(3) 0.5590(4) 0.0444 1.0000 Uani . . . . . .
C21 C 0.1687(3) 0.5737(3) 0.7211(3) 0.0272 1.0000 Uani . . . . . .
C22 C 0.1245(3) 0.6008(3) 0.7859(4) 0.0309 1.0000 Uani . . . . . .
C23 C 0.1328(3) 0.5414(3) 0.6441(3) 0.0313 1.0000 Uani . . . . . .
C24 C 0.1776(4) 0.5199(3) 0.5687(4) 0.0399 1.0000 Uani . . . . . .
C25 C 0.0534(3) 0.5297(3) 0.6390(4) 0.0352 1.0000 Uani . . . . . .
C26 C 0.0086(3) 0.5503(3) 0.7054(4) 0.0388 1.0000 Uani . . . . . .
C27 C -0.0770(4) 0.5323(3) 0.6999(5) 0.0513 1.0000 Uani . . . . . .
C28 C 0.3230(3) 0.3204(2) 0.7107(3) 0.0240 1.0000 Uani . . . . . .
N29 N 0.3892(2) 0.2841(2) 0.7265(3) 0.0244 1.0000 Uani . . . . . .
C30 C 0.4553(3) 0.3021(3) 0.7892(3) 0.0246 1.0000 Uani . . . . . .
C31 C 0.4526(3) 0.2831(3) 0.8785(3) 0.0280 1.0000 Uani . . . . . .
C32 C 0.3825(3) 0.2473(3) 0.9097(4) 0.0357 1.0000 Uani . . . . . .
C33 C 0.5185(3) 0.2938(3) 0.9379(3) 0.0310 1.0000 Uani . . . . . .
C34 C 0.5863(3) 0.3213(3) 0.9097(4) 0.0328 1.0000 Uani . . . . . .
C35 C 0.5874(3) 0.3380(3) 0.8210(4) 0.0322 1.0000 Uani . . . . . .
C36 C 0.5223(3) 0.3287(3) 0.7595(4) 0.0290 1.0000 Uani . . . . . .
C37 C 0.5285(3) 0.3457(3) 0.6628(4) 0.0396 1.0000 Uani . . . . . .
C38 C 0.6585(4) 0.3292(4) 0.9748(4) 0.0501 1.0000 Uani . . . . . .
C39 C 0.3882(3) 0.2127(3) 0.6870(4) 0.0335 1.0000 Uani . . . . . .
C40 C 0.3052(3) 0.2076(3) 0.6421(4) 0.0328 1.0000 Uani . . . . . .
N41 N 0.2720(2) 0.2772(2) 0.6633(3) 0.0270 1.0000 Uani . . . . . .
C42 C 0.1906(3) 0.2897(3) 0.6372(3) 0.0272 1.0000 Uani . . . . . .
C43 C 0.1658(3) 0.3224(3) 0.5564(4) 0.0299 1.0000 Uani . . . . . .
C44 C 0.2217(3) 0.3391(3) 0.4893(3) 0.0358 1.0000 Uani . . . . . .
C45 C 0.0871(3) 0.3359(3) 0.5360(3) 0.0323 1.0000 Uani . . . . . .
C46 C 0.0324(3) 0.3156(3) 0.5907(4) 0.0368 1.0000 Uani . . . . . .
C47 C 0.0580(3) 0.2762(3) 0.6668(4) 0.0363 1.0000 Uani . . . . . .
C48 C 0.1357(3) 0.2621(3) 0.6903(4) 0.0321 1.0000 Uani . . . . . .
C49 C 0.1593(4) 0.2155(3) 0.7694(4) 0.0447 1.0000 Uani . . . . . .
C50 C 0.1452(4) 0.3816(4) 0.9835(4) 0.0521 1.0000 Uani . . . . . .
O1 O 0.8265(3) 0.3076(2) 0.7490(3) 0.0583 1.0000 Uani . . . . . .
C2 C 0.1021(3) 0.3846(4) 0.8898(4) 0.0440 1.0000 Uani . . . . . .
C3 C 0.0449(3) 0.5880(3) 0.7770(4) 0.0363 1.0000 Uani . . . . . .
C4 C 0.1594(4) 0.6427(3) 0.8657(4) 0.0418 1.0000 Uani . . . . . .
C5 C 0.1728(4) 0.4525(4) 1.0222(4) 0.0558 1.0000 Uani . . . . . .
C6 C -0.0518(3) 0.3351(4) 0.5703(5) 0.0515 1.0000 Uani . . . . . .
C7 C 0.6944(4) 0.5340(4) 0.6755(5) 0.0539 1.0000 Uani . . . . . .
C8 C 0.7847(4) 0.3625(4) 0.7008(5) 0.0581 1.0000 Uani . . . . . .
C9 C 0.7383(4) 0.3305(4) 0.6223(6) 0.0671 1.0000 Uani . . . . . .
C10 C 0.8767(6) 0.3341(5) 0.8217(6) 0.0828 1.0000 Uani . . . . . .
C13 C 0.9098(6) 0.2724(5) 0.8757(6) 0.0980 1.0000 Uani . . . . . .
H551 H 0.2298 0.3389 0.8249 0.0340 1.0000 Uiso R . . . . .
H561 H 0.3300 0.3887 0.9022 0.0299 1.0000 Uiso R . . . . .
H581 H 0.3343 0.5128 0.9343 0.0382 1.0000 Uiso R . . . . .
H582 H 0.2458 0.5187 0.8941 0.0377 1.0000 Uiso R . . . . .
H511 H 0.2898 0.4340 1.0457 0.0477 1.0000 Uiso R . . . . .
H512 H 0.2682 0.5153 1.0546 0.0479 1.0000 Uiso R . . . . .
H571 H 0.1496 0.4700 0.8278 0.0380 1.0000 Uiso R . . . . .
H572 H 0.1214 0.4087 0.7591 0.0379 1.0000 Uiso R . . . . .
H531 H 0.2493 0.6931 0.7448 0.0419 1.0000 Uiso R . . . . .
H532 H 0.2671 0.6689 0.6473 0.0417 1.0000 Uiso R . . . . .
H112 H 0.3750 0.6693 0.8022 0.0428 1.0000 Uiso R . . . . .
H111 H 0.3939 0.6804 0.7024 0.0430 1.0000 Uiso R . . . . .
H152 H 0.5269 0.4994 0.9173 0.0558 1.0000 Uiso R . . . . .
H151 H 0.4461 0.4725 0.8716 0.0561 1.0000 Uiso R . . . . .
H153 H 0.4568 0.5524 0.9014 0.0561 1.0000 Uiso R . . . . .
H161 H 0.6195 0.5045 0.8171 0.0388 1.0000 Uiso R . . . . .
H181 H 0.5717 0.5733 0.5680 0.0430 1.0000 Uiso R . . . . .
H201 H 0.4378 0.5803 0.5042 0.0671 1.0000 Uiso R . . . . .
H202 H 0.3711 0.5867 0.5668 0.0671 1.0000 Uiso R . . . . .
H203 H 0.4276 0.6513 0.5560 0.0672 1.0000 Uiso R . . . . .
H243 H 0.1419 0.5084 0.5170 0.0602 1.0000 Uiso R . . . . .
H241 H 0.2090 0.4788 0.5868 0.0602 1.0000 Uiso R . . . . .
H242 H 0.2110 0.5584 0.5549 0.0603 1.0000 Uiso R . . . . .
H251 H 0.0290 0.5071 0.5882 0.0420 1.0000 Uiso R . . . . .
H273 H -0.0976 0.5494 0.7519 0.0772 1.0000 Uiso R . . . . .
H271 H -0.0845 0.4820 0.6968 0.0773 1.0000 Uiso R . . . . .
H272 H -0.1051 0.5539 0.6491 0.0773 1.0000 Uiso R . . . . .
H321 H 0.3907 0.2396 0.9724 0.0542 1.0000 Uiso R . . . . .
H322 H 0.3748 0.2018 0.8805 0.0544 1.0000 Uiso R . . . . .
H323 H 0.3373 0.2765 0.8956 0.0541 1.0000 Uiso R . . . . .
H331 H 0.5175 0.2816 0.9979 0.0372 1.0000 Uiso R . . . . .
H351 H 0.6328 0.3561 0.8009 0.0389 1.0000 Uiso R . . . . .
H371 H 0.5450 0.3938 0.6564 0.0593 1.0000 Uiso R . . . . .
H373 H 0.5658 0.3146 0.6399 0.0592 1.0000 Uiso R . . . . .
H372 H 0.4790 0.3388 0.6286 0.0594 1.0000 Uiso R . . . . .
H382 H 0.7036 0.3344 0.9437 0.0750 1.0000 Uiso R . . . . .
H381 H 0.6645 0.2881 1.0125 0.0752 1.0000 Uiso R . . . . .
H383 H 0.6535 0.3704 1.0110 0.0753 1.0000 Uiso R . . . . .
H391 H 0.3988 0.1763 0.7322 0.0398 1.0000 Uiso R . . . . .
H392 H 0.4253 0.2083 0.6439 0.0400 1.0000 Uiso R . . . . .
H401 H 0.2769 0.1688 0.6667 0.0401 1.0000 Uiso R . . . . .
H402 H 0.3043 0.2016 0.5777 0.0401 1.0000 Uiso R . . . . .
H441 H 0.2008 0.3744 0.4476 0.0541 1.0000 Uiso R . . . . .
H443 H 0.2310 0.2967 0.4565 0.0543 1.0000 Uiso R . . . . .
H442 H 0.2706 0.3552 0.5183 0.0541 1.0000 Uiso R . . . . .
H451 H 0.0706 0.3599 0.4832 0.0391 1.0000 Uiso R . . . . .
H471 H 0.0214 0.2591 0.7030 0.0440 1.0000 Uiso R . . . . .
H491 H 0.1227 0.2213 0.8120 0.0670 1.0000 Uiso R . . . . .
H493 H 0.1595 0.1667 0.7507 0.0671 1.0000 Uiso R . . . . .
H492 H 0.2107 0.2280 0.7965 0.0670 1.0000 Uiso R . . . . .
H502 H 0.1912 0.3508 0.9819 0.0620 1.0000 Uiso R . . . . .
H501 H 0.1100 0.3603 1.0231 0.0622 1.0000 Uiso R . . . . .
H22 H 0.0893 0.3359 0.8708 0.0530 1.0000 Uiso R . . . . .
H21 H 0.0550 0.4114 0.8921 0.0530 1.0000 Uiso R . . . . .
H31 H 0.0146 0.6049 0.8201 0.0440 1.0000 Uiso R . . . . .
H41 H 0.1348 0.6295 0.9176 0.0631 1.0000 Uiso R . . . . .
H42 H 0.2141 0.6339 0.8761 0.0629 1.0000 Uiso R . . . . .
H43 H 0.1511 0.6928 0.8550 0.0630 1.0000 Uiso R . . . . .
H52 H 0.1638 0.4519 1.0848 0.0669 1.0000 Uiso R . . . . .
H51 H 0.1405 0.4891 0.9901 0.0671 1.0000 Uiso R . . . . .
H62 H -0.0838 0.2964 0.5854 0.0783 1.0000 Uiso R . . . . .
H61 H -0.0631 0.3452 0.5078 0.0780 1.0000 Uiso R . . . . .
H63 H -0.0638 0.3763 0.6040 0.0782 1.0000 Uiso R . . . . .
H72 H 0.7001 0.5067 0.6230 0.0811 1.0000 Uiso R . . . . .
H73 H 0.7231 0.5108 0.7249 0.0810 1.0000 Uiso R . . . . .
H71 H 0.7155 0.5808 0.6690 0.0810 1.0000 Uiso R . . . . .
H81 H 0.7502 0.3860 0.7391 0.0700 1.0000 Uiso R . . . . .
H82 H 0.8214 0.3973 0.6806 0.0701 1.0000 Uiso R . . . . .
H92 H 0.7064 0.3667 0.5915 0.1009 1.0000 Uiso R . . . . .
H93 H 0.7053 0.2934 0.6419 0.1010 1.0000 Uiso R . . . . .
H91 H 0.7734 0.3106 0.5829 0.1009 1.0000 Uiso R . . . . .
H102 H 0.8472 0.3644 0.8587 0.0991 1.0000 Uiso R . . . . .
H101 H 0.9187 0.3619 0.7997 0.0990 1.0000 Uiso R . . . . .
H132 H 0.9479 0.2894 0.9221 0.1470 1.0000 Uiso R . . . . .
H131 H 0.8686 0.2480 0.9018 0.1469 1.0000 Uiso R . . . . .
H133 H 0.9341 0.2402 0.8376 0.1471 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.077498(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ir1 . Cl2 . 2.3674(11) yes
Ir1 . C55 . 2.134(5) yes
Ir1 . C56 . 2.131(4) yes
Ir1 . C54 . 2.076(4) yes
Ir1 . C28 . 2.062(5) yes
C55 . C56 . 1.426(6) yes
C55 . C57 . 1.497(7) yes
C55 . H551 . 0.979 no
C56 . C58 . 1.507(7) yes
C56 . H561 . 0.972 no
C58 . C51 . 1.540(7) yes
C58 . H581 . 0.977 no
C58 . H582 . 0.977 no
C51 . C5 . 1.526(9) yes
C51 . H511 . 0.977 no
C51 . H512 . 0.974 no
C57 . C2 . 1.544(7) yes
C57 . H571 . 0.977 no
C57 . H572 . 0.976 no
C54 . N9 . 1.361(6) yes
C54 . N12 . 1.370(6) yes
N9 . C53 . 1.482(6) yes
N9 . C21 . 1.432(6) yes
C53 . C11 . 1.520(7) yes
C53 . H531 . 0.983 no
C53 . H532 . 0.977 no
C11 . N12 . 1.483(7) yes
C11 . H112 . 0.976 no
C11 . H111 . 0.973 no
N12 . C52 . 1.434(6) yes
C52 . C14 . 1.396(7) yes
C52 . C19 . 1.409(6) yes
C14 . C15 . 1.513(7) yes
C14 . C16 . 1.393(7) yes
C15 . H152 . 0.962 no
C15 . H151 . 0.967 no
C15 . H153 . 0.969 no
C16 . C17 . 1.388(7) yes
C16 . H161 . 0.930 no
C17 . C18 . 1.388(8) yes
C17 . C7 . 1.515(8) yes
C18 . C19 . 1.374(7) yes
C18 . H181 . 0.926 no
C19 . C20 . 1.508(7) yes
C20 . H201 . 0.966 no
C20 . H202 . 0.965 no
C20 . H203 . 0.965 no
C21 . C22 . 1.401(7) yes
C21 . C23 . 1.400(7) yes
C22 . C3 . 1.393(7) yes
C22 . C4 . 1.513(7) yes
C23 . C24 . 1.500(8) yes
C23 . C25 . 1.387(8) yes
C24 . H243 . 0.969 no
C24 . H241 . 0.970 no
C24 . H242 . 0.964 no
C25 . C26 . 1.387(8) yes
C25 . H251 . 0.940 no
C26 . C27 . 1.515(8) yes
C26 . C3 . 1.389(8) yes
C27 . H273 . 0.952 no
C27 . H271 . 0.957 no
C27 . H272 . 0.957 no
C28 . N29 . 1.335(6) yes
C28 . N41 . 1.350(6) yes
N29 . C30 . 1.448(6) yes
N29 . C39 . 1.472(6) yes
C30 . C31 . 1.403(7) yes
C30 . C36 . 1.382(7) yes
C31 . C32 . 1.506(7) yes
C31 . C33 . 1.391(7) yes
C32 . H321 . 0.956 no
C32 . H322 . 0.968 no
C32 . H323 . 0.963 no
C33 . C34 . 1.390(7) yes
C33 . H331 . 0.938 no
C34 . C35 . 1.380(8) yes
C34 . C38 . 1.517(7) yes
C35 . C36 . 1.396(7) yes
C35 . H351 . 0.936 no
C36 . C37 . 1.511(7) yes
C37 . H371 . 0.960 no
C37 . H373 . 0.963 no
C37 . H372 . 0.963 no
C38 . H382 . 0.956 no
C38 . H381 . 0.960 no
C38 . H383 . 0.959 no
C39 . C40 . 1.526(7) yes
C39 . H391 . 0.972 no
C39 . H392 . 0.966 no
C40 . N41 . 1.481(6) yes
C40 . H401 . 0.974 no
C40 . H402 . 0.979 no
N41 . C42 . 1.444(6) yes
C42 . C43 . 1.394(7) yes
C42 . C48 . 1.407(7) yes
C43 . C44 . 1.508(7) yes
C43 . C45 . 1.390(7) yes
C44 . H441 . 0.962 no
C44 . H443 . 0.963 no
C44 . H442 . 0.961 no
C45 . C46 . 1.376(8) yes
C45 . H451 . 0.936 no
C46 . C47 . 1.401(8) yes
C46 . C6 . 1.504(8) yes
C47 . C48 . 1.382(8) yes
C47 . H471 . 0.938 no
C48 . C49 . 1.504(7) yes
C49 . H491 . 0.957 no
C49 . H493 . 0.963 no
C49 . H492 . 0.970 no
C50 . C2 . 1.532(9) yes
C50 . C5 . 1.517(9) yes
C50 . H502 . 0.986 no
C50 . H501 . 0.985 no
O1 . C8 . 1.419(8) yes
O1 . C10 . 1.419(9) yes
C2 . H22 . 0.980 no
C2 . H21 . 0.964 no
C3 . H31 . 0.934 no
C4 . H41 . 0.964 no
C4 . H42 . 0.959 no
C4 . H43 . 0.965 no
C5 . H52 . 0.976 no
C5 . H51 . 0.984 no
C6 . H62 . 0.958 no
C6 . H61 . 0.964 no
C6 . H63 . 0.962 no
C7 . H72 . 0.960 no
C7 . H73 . 0.959 no
C7 . H71 . 0.964 no
C8 . C9 . 1.490(10) yes
C8 . H81 . 0.981 no
C8 . H82 . 0.984 no
C9 . H92 . 0.967 no
C9 . H93 . 0.968 no
C9 . H91 . 0.970 no
C10 . C13 . 1.499(12) yes
C10 . H102 . 0.980 no
C10 . H101 . 0.982 no
C13 . H132 . 0.966 no
C13 . H131 . 0.967 no
C13 . H133 . 0.965 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl2 . Ir1 . C55 . 156.02(14) yes
Cl2 . Ir1 . C56 . 163.83(12) yes
C55 . Ir1 . C56 . 39.09(17) yes
Cl2 . Ir1 . C54 . 85.04(16) yes
C55 . Ir1 . C54 . 108.6(2) yes
C56 . Ir1 . C54 . 92.0(2) yes
Cl2 . Ir1 . C28 . 82.81(14) yes
C55 . Ir1 . C28 . 83.63(19) yes
C56 . Ir1 . C28 . 99.0(2) yes
C54 . Ir1 . C28 . 167.6(2) yes
Ir1 . C55 . C56 . 70.3(3) yes
Ir1 . C55 . C57 . 122.5(3) yes
C56 . C55 . C57 . 124.2(5) yes
Ir1 . C55 . H551 . 109.9 no
C56 . C55 . H551 . 112.3 no
C57 . C55 . H551 . 111.6 no
Ir1 . C56 . C55 . 70.6(3) yes
Ir1 . C56 . C58 . 122.5(3) yes
C55 . C56 . C58 . 120.7(4) yes
Ir1 . C56 . H561 . 110.4 no
C55 . C56 . H561 . 114.2 no
C58 . C56 . H561 . 112.4 no
C56 . C58 . C51 . 113.9(4) yes
C56 . C58 . H581 . 108.0 no
C51 . C58 . H581 . 109.2 no
C56 . C58 . H582 . 108.3 no
C51 . C58 . H582 . 108.3 no
H581 . C58 . H582 . 109.1 no
C58 . C51 . C5 . 117.2(5) yes
C58 . C51 . H511 . 107.7 no
C5 . C51 . H511 . 107.9 no
C58 . C51 . H512 . 106.8 no
C5 . C51 . H512 . 108.1 no
H511 . C51 . H512 . 108.8 no
C55 . C57 . C2 . 111.9(4) yes
C55 . C57 . H571 . 108.8 no
C2 . C57 . H571 . 108.8 no
C55 . C57 . H572 . 107.9 no
C2 . C57 . H572 . 109.8 no
H571 . C57 . H572 . 109.6 no
Ir1 . C54 . N9 . 131.9(4) yes
Ir1 . C54 . N12 . 122.3(4) yes
N9 . C54 . N12 . 105.6(4) yes
C54 . N9 . C53 . 112.9(4) yes
C54 . N9 . C21 . 128.9(4) yes
C53 . N9 . C21 . 116.3(4) yes
N9 . C53 . C11 . 101.1(4) yes
N9 . C53 . H531 . 109.8 no
C11 . C53 . H531 . 113.4 no
N9 . C53 . H532 . 111.2 no
C11 . C53 . H532 . 111.4 no
H531 . C53 . H532 . 109.8 no
C53 . C11 . N12 . 101.1(4) yes
C53 . C11 . H112 . 111.7 no
N12 . C11 . H112 . 110.6 no
C53 . C11 . H111 . 112.0 no
N12 . C11 . H111 . 111.8 no
H112 . C11 . H111 . 109.4 no
C11 . N12 . C54 . 112.7(4) yes
C11 . N12 . C52 . 114.9(4) yes
C54 . N12 . C52 . 132.1(5) yes
N12 . C52 . C14 . 121.8(4) yes
N12 . C52 . C19 . 117.5(4) yes
C14 . C52 . C19 . 120.2(5) yes
C52 . C14 . C15 . 121.6(5) yes
C52 . C14 . C16 . 119.1(5) yes
C15 . C14 . C16 . 119.3(5) yes
C14 . C15 . H152 . 109.6 no
C14 . C15 . H151 . 109.5 no
H152 . C15 . H151 . 109.9 no
C14 . C15 . H153 . 109.8 no
H152 . C15 . H153 . 108.8 no
H151 . C15 . H153 . 109.2 no
C14 . C16 . C17 . 121.3(5) yes
C14 . C16 . H161 . 119.6 no
C17 . C16 . H161 . 119.1 no
C16 . C17 . C18 . 118.4(5) yes
C16 . C17 . C7 . 121.5(6) yes
C18 . C17 . C7 . 120.1(5) yes
C17 . C18 . C19 . 122.2(5) yes
C17 . C18 . H181 . 118.9 no
C19 . C18 . H181 . 118.9 no
C52 . C19 . C18 . 118.8(5) yes
C52 . C19 . C20 . 122.3(5) yes
C18 . C19 . C20 . 119.0(5) yes
C19 . C20 . H201 . 109.0 no
C19 . C20 . H202 . 110.0 no
H201 . C20 . H202 . 109.3 no
C19 . C20 . H203 . 109.8 no
H201 . C20 . H203 . 108.8 no
H202 . C20 . H203 . 110.0 no
N9 . C21 . C22 . 118.8(4) yes
N9 . C21 . C23 . 120.0(4) yes
C22 . C21 . C23 . 120.9(5) yes
C21 . C22 . C3 . 118.4(5) yes
C21 . C22 . C4 . 123.1(5) yes
C3 . C22 . C4 . 118.4(5) yes
C21 . C23 . C24 . 122.0(5) yes
C21 . C23 . C25 . 117.7(5) yes
C24 . C23 . C25 . 120.3(5) yes
C23 . C24 . H243 . 109.7 no
C23 . C24 . H241 . 108.7 no
H243 . C24 . H241 . 109.9 no
C23 . C24 . H242 . 109.3 no
H243 . C24 . H242 . 109.9 no
H241 . C24 . H242 . 109.4 no
C23 . C25 . C26 . 122.8(5) yes
C23 . C25 . H251 . 118.4 no
C26 . C25 . H251 . 118.8 no
C25 . C26 . C27 . 121.1(6) yes
C25 . C26 . C3 . 117.7(5) yes
C27 . C26 . C3 . 121.2(6) yes
C26 . C27 . H273 . 109.0 no
C26 . C27 . H271 . 110.6 no
H273 . C27 . H271 . 108.5 no
C26 . C27 . H272 . 111.1 no
H273 . C27 . H272 . 108.5 no
H271 . C27 . H272 . 109.1 no
Ir1 . C28 . N29 . 125.6(4) yes
Ir1 . C28 . N41 . 126.7(3) yes
N29 . C28 . N41 . 106.8(4) yes
C28 . N29 . C30 . 127.1(4) yes
C28 . N29 . C39 . 114.9(4) yes
C30 . N29 . C39 . 117.1(4) yes
N29 . C30 . C31 . 117.8(4) yes
N29 . C30 . C36 . 120.3(5) yes
C31 . C30 . C36 . 121.3(5) yes
C30 . C31 . C32 . 121.6(5) yes
C30 . C31 . C33 . 118.5(5) yes
C32 . C31 . C33 . 119.8(5) yes
C31 . C32 . H321 . 109.7 no
C31 . C32 . H322 . 109.4 no
H321 . C32 . H322 . 108.3 no
C31 . C32 . H323 . 109.8 no
H321 . C32 . H323 . 109.9 no
H322 . C32 . H323 . 109.7 no
C31 . C33 . C34 . 121.2(5) yes
C31 . C33 . H331 . 119.4 no
C34 . C33 . H331 . 119.4 no
C33 . C34 . C35 . 118.8(5) yes
C33 . C34 . C38 . 120.2(5) yes
C35 . C34 . C38 . 120.9(5) yes
C34 . C35 . C36 . 121.7(5) yes
C34 . C35 . H351 . 119.7 no
C36 . C35 . H351 . 118.5 no
C35 . C36 . C30 . 118.5(5) yes
C35 . C36 . C37 . 118.9(5) yes
C30 . C36 . C37 . 122.6(5) yes
C36 . C37 . H371 . 110.5 no
C36 . C37 . H373 . 109.7 no
H371 . C37 . H373 . 108.7 no
C36 . C37 . H372 . 110.1 no
H371 . C37 . H372 . 109.2 no
H373 . C37 . H372 . 108.6 no
C34 . C38 . H382 . 110.5 no
C34 . C38 . H381 . 109.6 no
H382 . C38 . H381 . 109.4 no
C34 . C38 . H383 . 109.4 no
H382 . C38 . H383 . 109.0 no
H381 . C38 . H383 . 108.9 no
N29 . C39 . C40 . 102.1(4) yes
N29 . C39 . H391 . 111.5 no
C40 . C39 . H391 . 111.7 no
N29 . C39 . H392 . 111.8 no
C40 . C39 . H392 . 110.9 no
H391 . C39 . H392 . 108.8 no
C39 . C40 . N41 . 102.5(4) yes
C39 . C40 . H401 . 111.5 no
N41 . C40 . H401 . 111.0 no
C39 . C40 . H402 . 111.6 no
N41 . C40 . H402 . 110.4 no
H401 . C40 . H402 . 109.7 no
C40 . N41 . C28 . 113.7(4) yes
C40 . N41 . C42 . 118.4(4) yes
C28 . N41 . C42 . 127.8(4) yes
N41 . C42 . C43 . 120.9(5) yes
N41 . C42 . C48 . 118.8(4) yes
C43 . C42 . C48 . 120.0(5) yes
C42 . C43 . C44 . 121.4(5) yes
C42 . C43 . C45 . 118.7(5) yes
C44 . C43 . C45 . 119.8(5) yes
C43 . C44 . H441 . 111.1 no
C43 . C44 . H443 . 109.1 no
H441 . C44 . H443 . 108.0 no
C43 . C44 . H442 . 110.8 no
H441 . C44 . H442 . 109.6 no
H443 . C44 . H442 . 108.1 no
C43 . C45 . C46 . 122.5(5) yes
C43 . C45 . H451 . 118.9 no
C46 . C45 . H451 . 118.6 no
C45 . C46 . C47 . 117.5(5) yes
C45 . C46 . C6 . 121.5(5) yes
C47 . C46 . C6 . 121.0(5) yes
C46 . C47 . C48 . 122.0(5) yes
C46 . C47 . H471 . 119.0 no
C48 . C47 . H471 . 118.9 no
C42 . C48 . C47 . 118.6(5) yes
C42 . C48 . C49 . 121.8(5) yes
C47 . C48 . C49 . 119.6(5) yes
C48 . C49 . H491 . 108.9 no
C48 . C49 . H493 . 109.5 no
H491 . C49 . H493 . 109.3 no
C48 . C49 . H492 . 110.8 no
H491 . C49 . H492 . 109.4 no
H493 . C49 . H492 . 109.0 no
C2 . C50 . C5 . 115.3(6) yes
C2 . C50 . H502 . 108.4 no
C5 . C50 . H502 . 107.7 no
C2 . C50 . H501 . 107.8 no
C5 . C50 . H501 . 108.3 no
H502 . C50 . H501 . 109.2 no
C8 . O1 . C10 . 112.4(6) yes
C57 . C2 . C50 . 115.4(5) yes
C57 . C2 . H22 . 107.6 no
C50 . C2 . H22 . 108.0 no
C57 . C2 . H21 . 107.6 no
C50 . C2 . H21 . 108.5 no
H22 . C2 . H21 . 109.6 no
C22 . C3 . C26 . 121.8(5) yes
C22 . C3 . H31 . 119.8 no
C26 . C3 . H31 . 118.5 no
C22 . C4 . H41 . 109.9 no
C22 . C4 . H42 . 110.2 no
H41 . C4 . H42 . 109.6 no
C22 . C4 . H43 . 109.6 no
H41 . C4 . H43 . 108.6 no
H42 . C4 . H43 . 108.8 no
C51 . C5 . C50 . 118.3(6) yes
C51 . C5 . H52 . 106.7 no
C50 . C5 . H52 . 106.8 no
C51 . C5 . H51 . 108.1 no
C50 . C5 . H51 . 106.7 no
H52 . C5 . H51 . 110.2 no
C46 . C6 . H62 . 109.7 no
C46 . C6 . H61 . 110.0 no
H62 . C6 . H61 . 108.8 no
C46 . C6 . H63 . 110.2 no
H62 . C6 . H63 . 109.1 no
H61 . C6 . H63 . 109.0 no
C17 . C7 . H72 . 109.9 no
C17 . C7 . H73 . 110.1 no
H72 . C7 . H73 . 108.0 no
C17 . C7 . H71 . 110.2 no
H72 . C7 . H71 . 109.5 no
H73 . C7 . H71 . 109.0 no
O1 . C8 . C9 . 108.6(6) yes
O1 . C8 . H81 . 109.6 no
C9 . C8 . H81 . 110.1 no
O1 . C8 . H82 . 109.5 no
C9 . C8 . H82 . 109.5 no
H81 . C8 . H82 . 109.5 no
C8 . C9 . H92 . 109.3 no
C8 . C9 . H93 . 109.5 no
H92 . C9 . H93 . 109.4 no
C8 . C9 . H91 . 109.0 no
H92 . C9 . H91 . 109.9 no
H93 . C9 . H91 . 109.8 no
O1 . C10 . C13 . 108.5(7) yes
O1 . C10 . H102 . 109.4 no
C13 . C10 . H102 . 109.5 no
O1 . C10 . H101 . 109.9 no
C13 . C10 . H101 . 110.1 no
H102 . C10 . H101 . 109.5 no
C10 . C13 . H132 . 109.4 no
C10 . C13 . H131 . 109.6 no
H132 . C13 . H131 . 109.7 no
C10 . C13 . H133 . 109.3 no
H132 . C13 . H133 . 109.5 no
H131 . C13 . H133 . 109.3 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C57 . H571 . C21 . 131.43 0.977 2.576 3.304(8) yes
C57 . H571 . C22 . 155.35 0.977 2.571 3.482(8) yes
C53 . H531 . O1 3_656 149.93 0.983 2.534 3.420(8) yes
_database_code_depnum_ccdc_archive 'CCDC 1002301'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3
#==============================================================================
_audit_creation_date             13-06-01
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 066nprt13
_chemical_name_systematic        .
_chemical_melting_point          .


_refine_special_details          
; 
The difference map indicated the presence of diffuse electron
density believed to be disordered solvent.  SQUEEZE was used 
leaving a void 
from which the electron density was removed.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.500 166 16 ' '
2 1.000 0.500 1.000 166 16 ' '
_platon_squeeze_details          
;
The discrete Fourier transform of the void region were treated as 
contributions to the A and B parts of the calculated structure factors.
;

_cell_length_a                   15.8693(1)
_cell_length_b                   12.3445(1)
_cell_length_c                   21.1450(2)
_cell_angle_alpha                90
_cell_angle_beta                 104.6968(4)
_cell_angle_gamma                90
_cell_volume                     4006.75(6)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ir -1.4442 7.9887 27.3049 1.5928 16.7296 8.8655 15.6115 0.4179 5.8338 45.0011
11.4722 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C42 H50 Cl1 Ir1 N4 
# Dc =      1.39 Fooo =   1704.00 Mu =     34.31 M =    838.56
# Found Formula = C42 H52 Cl1 Ir1 N4 
# Dc =      1.39 FOOO =   1704.00 Mu =     34.31 M =    840.57

_chemical_formula_sum            'C42 H52 Cl Ir N4'
_chemical_formula_moiety         'C42 H52 Cl Ir N4'
_chemical_compound_source        .
_chemical_formula_weight         840.57


_cell_measurement_reflns_used    9434
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.180
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_max          0.260

_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1704
_exptl_absorpt_coefficient_mu    3.431

# Sheldrick geometric approximatio 0.44 0.54 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_T_max  0.54
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            138077
_reflns_number_total             9099
_diffrn_reflns_av_R_equivalents  0.024


_diffrn_reflns_theta_min         5.130
_diffrn_reflns_theta_max         27.474
_diffrn_measured_fraction_theta_max 0.993

_diffrn_reflns_theta_full        26.925
_diffrn_measured_fraction_theta_full 0.993


_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       27
_reflns_limit_h_min              -20
_reflns_limit_h_max              19
_reflns_limit_k_min              0
_reflns_limit_k_max              15
_reflns_limit_l_min              0
_reflns_limit_l_max              27

_oxford_diffrn_Wilson_B_factor   1.84
_oxford_diffrn_Wilson_scale      69.36

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.43
_refine_diff_density_max         1.50


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_refine_ls_number_reflns         9099
_refine_ls_number_restraints     0
_refine_ls_number_parameters     437
_oxford_refine_ls_R_factor_ref   0.0424
_refine_ls_wR_factor_ref         0.0732
_refine_ls_goodness_of_fit_ref   0.9283
_refine_ls_shift/su_max          0.0027828
_refine_ls_shift/su_mean         0.0000294


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        9099
_refine_ls_R_factor_all          0.0424
_refine_ls_wR_factor_all         0.0732

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                7269
_refine_ls_R_factor_gt           0.0282
_refine_ls_wR_factor_gt          0.0611

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    mixed #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 9.29 13.0 6.35 1.76 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ir1 Ir 0.510898(9) 0.594152(11) 0.742671(7) 0.0223 1.0000 Uani . . . . . .
Cl2 Cl 0.56327(7) 0.75111(8) 0.69609(5) 0.0361 1.0000 Uani . . . . . .
C3 C 0.4471(2) 0.4540(3) 0.76234(19) 0.0286 1.0000 Uani . . . . . .
C4 C 0.3844(2) 0.4227(3) 0.69880(19) 0.0270 1.0000 Uani . . . . . .
C5 C 0.3873(3) 0.3231(3) 0.6686(2) 0.0312 1.0000 Uani . . . . . .
C6 C 0.3300(3) 0.2954(3) 0.6090(2) 0.0352 1.0000 Uani . . . . . .
C7 C 0.2692(3) 0.3717(4) 0.5786(2) 0.0352 1.0000 Uani . . . . . .
C8 C 0.2640(3) 0.4734(3) 0.6062(2) 0.0325 1.0000 Uani . . . . . .
C9 C 0.3210(3) 0.4970(3) 0.6663(2) 0.0290 1.0000 Uani . . . . . .
N10 N 0.3164(2) 0.6001(3) 0.69591(17) 0.0315 1.0000 Uani . . . . . .
C11 C 0.3888(3) 0.6529(3) 0.72978(19) 0.0279 1.0000 Uani . . . . . .
N12 N 0.3615(2) 0.7365(3) 0.75997(17) 0.0321 1.0000 Uani . . . . . .
C13 C 0.4138(3) 0.8215(3) 0.7961(2) 0.0300 1.0000 Uani . . . . . .
C14 C 0.4296(3) 0.9144(4) 0.7639(2) 0.0376 1.0000 Uani . . . . . .
C15 C 0.4768(3) 0.9976(4) 0.8014(3) 0.0442 1.0000 Uani . . . . . .
C16 C 0.5058(3) 0.9914(4) 0.8683(3) 0.0434 1.0000 Uani . . . . . .
C17 C 0.4874(3) 0.8978(4) 0.8990(2) 0.0377 1.0000 Uani . . . . . .
C18 C 0.4416(3) 0.8123(3) 0.8641(2) 0.0309 1.0000 Uani . . . . . .
C19 C 0.4208(3) 0.7132(4) 0.8987(2) 0.0392 1.0000 Uani . . . . . .
C20 C 0.5561(4) 1.0830(5) 0.9080(3) 0.0665 1.0000 Uani . . . . . .
C21 C 0.3962(4) 0.9262(5) 0.6906(2) 0.0555 1.0000 Uani . . . . . .
C22 C 0.2657(3) 0.7457(4) 0.7447(3) 0.0434 1.0000 Uani . . . . . .
C23 C 0.2376(3) 0.6349(4) 0.7162(3) 0.0435 1.0000 Uani . . . . . .
C24 C 0.2026(3) 0.5566(4) 0.5674(2) 0.0459 1.0000 Uani . . . . . .
C25 C 0.3358(4) 0.1874(4) 0.5775(3) 0.0509 1.0000 Uani . . . . . .
C26 C 0.6353(2) 0.5339(3) 0.76747(18) 0.0250 1.0000 Uani . . . . . .
N27 N 0.6876(2) 0.5325(3) 0.82884(16) 0.0290 1.0000 Uani . . . . . .
C28 C 0.6641(2) 0.5615(3) 0.88782(19) 0.0268 1.0000 Uani . . . . . .
C29 C 0.6670(2) 0.6692(3) 0.90750(19) 0.0259 1.0000 Uani . . . . . .
C30 C 0.6484(3) 0.6923(3) 0.96734(19) 0.0324 1.0000 Uani . . . . . .
C31 C 0.6270(3) 0.6124(4) 1.0065(2) 0.0361 1.0000 Uani . . . . . .
C32 C 0.6247(3) 0.5065(4) 0.9850(2) 0.0372 1.0000 Uani . . . . . .
C33 C 0.6433(3) 0.4786(3) 0.9261(2) 0.0330 1.0000 Uani . . . . . .
C34 C 0.6390(4) 0.3623(4) 0.9050(3) 0.0471 1.0000 Uani . . . . . .
C35 C 0.6074(4) 0.6398(5) 1.0708(2) 0.0517 1.0000 Uani . . . . . .
C36 C 0.6886(3) 0.7604(4) 0.8671(2) 0.0355 1.0000 Uani . . . . . .
C37 C 0.7785(3) 0.5008(4) 0.8323(2) 0.0369 1.0000 Uani . . . . . .
C38 C 0.7743(3) 0.4711(5) 0.7618(2) 0.0489 1.0000 Uani . . . . . .
N39 N 0.6837(2) 0.5004(3) 0.72748(17) 0.0310 1.0000 Uani . . . . . .
C40 C 0.6517(3) 0.4724(4) 0.6600(2) 0.0314 1.0000 Uani . . . . . .
C41 C 0.6680(3) 0.5401(4) 0.6118(2) 0.0382 1.0000 Uani . . . . . .
C42 C 0.7161(4) 0.6456(5) 0.6276(3) 0.0547 1.0000 Uani . . . . . .
C43 C 0.6381(3) 0.5088(4) 0.5468(2) 0.0452 1.0000 Uani . . . . . .
C44 C 0.5941(3) 0.4123(5) 0.5284(2) 0.0432 1.0000 Uani . . . . . .
C45 C 0.5812(3) 0.3445(4) 0.5779(2) 0.0417 1.0000 Uani . . . . . .
C46 C 0.6115(3) 0.3723(4) 0.6443(2) 0.0337 1.0000 Uani . . . . . .
C47 C 0.6073(3) 0.2913(4) 0.6962(2) 0.0442 1.0000 Uani . . . . . .
C48 C 0.5638(4) 0.3809(6) 0.4571(2) 0.0606 1.0000 Uani . . . . . .
H31 H 0.4149 0.4708 0.7946 0.0353 1.0000 Uiso R . . . . .
H32 H 0.4882 0.3951 0.7786 0.0350 1.0000 Uiso R . . . . .
H51 H 0.4295 0.2723 0.6893 0.0381 1.0000 Uiso R . . . . .
H71 H 0.2303 0.3545 0.5388 0.0431 1.0000 Uiso R . . . . .
H151 H 0.4886 1.0605 0.7805 0.0543 1.0000 Uiso R . . . . .
H171 H 0.5063 0.8934 0.9443 0.0470 1.0000 Uiso R . . . . .
H191 H 0.4416 0.7236 0.9454 0.0601 1.0000 Uiso R . . . . .
H193 H 0.3588 0.7034 0.8868 0.0599 1.0000 Uiso R . . . . .
H192 H 0.4492 0.6515 0.8857 0.0602 1.0000 Uiso R . . . . .
H201 H 0.5409 1.0877 0.9492 0.0992 1.0000 Uiso R . . . . .
H203 H 0.5415 1.1494 0.8843 0.0991 1.0000 Uiso R . . . . .
H202 H 0.6173 1.0694 0.9153 0.0991 1.0000 Uiso R . . . . .
H211 H 0.4299 0.9819 0.6763 0.0840 1.0000 Uiso R . . . . .
H213 H 0.3355 0.9466 0.6801 0.0840 1.0000 Uiso R . . . . .
H212 H 0.4031 0.8587 0.6703 0.0840 1.0000 Uiso R . . . . .
H221 H 0.2459 0.7608 0.7843 0.0520 1.0000 Uiso R . . . . .
H222 H 0.2453 0.8027 0.7120 0.0520 1.0000 Uiso R . . . . .
H232 H 0.2265 0.5860 0.7499 0.0552 1.0000 Uiso R . . . . .
H231 H 0.1862 0.6379 0.6788 0.0549 1.0000 Uiso R . . . . .
H243 H 0.2283 0.6278 0.5776 0.0709 1.0000 Uiso R . . . . .
H242 H 0.1482 0.5535 0.5794 0.0710 1.0000 Uiso R . . . . .
H241 H 0.1930 0.5428 0.5216 0.0711 1.0000 Uiso R . . . . .
H253 H 0.2807 0.1512 0.5673 0.0792 1.0000 Uiso R . . . . .
H252 H 0.3783 0.1437 0.6069 0.0791 1.0000 Uiso R . . . . .
H251 H 0.3542 0.1985 0.5374 0.0791 1.0000 Uiso R . . . . .
H301 H 0.6504 0.7643 0.9815 0.0392 1.0000 Uiso R . . . . .
H321 H 0.6106 0.4520 1.0109 0.0450 1.0000 Uiso R . . . . .
H342 H 0.6298 0.3161 0.9392 0.0732 1.0000 Uiso R . . . . .
H341 H 0.6936 0.3425 0.8961 0.0731 1.0000 Uiso R . . . . .
H343 H 0.5925 0.3508 0.8658 0.0733 1.0000 Uiso R . . . . .
H352 H 0.5593 0.5966 1.0757 0.0781 1.0000 Uiso R . . . . .
H351 H 0.6575 0.6257 1.1063 0.0782 1.0000 Uiso R . . . . .
H353 H 0.5921 0.7150 1.0705 0.0783 1.0000 Uiso R . . . . .
H362 H 0.7054 0.8244 0.8938 0.0562 1.0000 Uiso R . . . . .
H361 H 0.7358 0.7389 0.8491 0.0563 1.0000 Uiso R . . . . .
H363 H 0.6388 0.7765 0.8318 0.0563 1.0000 Uiso R . . . . .
H372 H 0.8180 0.5614 0.8465 0.0469 1.0000 Uiso R . . . . .
H371 H 0.7959 0.4393 0.8613 0.0470 1.0000 Uiso R . . . . .
H382 H 0.8167 0.5120 0.7457 0.0623 1.0000 Uiso R . . . . .
H381 H 0.7847 0.3940 0.7588 0.0622 1.0000 Uiso R . . . . .
H421 H 0.7188 0.6815 0.5880 0.0821 1.0000 Uiso R . . . . .
H423 H 0.7742 0.6302 0.6528 0.0822 1.0000 Uiso R . . . . .
H422 H 0.6867 0.6898 0.6524 0.0821 1.0000 Uiso R . . . . .
H431 H 0.6475 0.5548 0.5132 0.0562 1.0000 Uiso R . . . . .
H451 H 0.5504 0.2790 0.5666 0.0512 1.0000 Uiso R . . . . .
H472 H 0.5732 0.2292 0.6758 0.0681 1.0000 Uiso R . . . . .
H471 H 0.6655 0.2680 0.7179 0.0680 1.0000 Uiso R . . . . .
H473 H 0.5804 0.3242 0.7274 0.0678 1.0000 Uiso R . . . . .
H482 H 0.5148 0.3328 0.4524 0.0957 1.0000 Uiso R . . . . .
H481 H 0.6104 0.3444 0.4444 0.0959 1.0000 Uiso R . . . . .
H483 H 0.5468 0.4442 0.4309 0.0962 1.0000 Uiso R . . . . .
H8 H 0.520(3) 0.622(4) 0.814(2) 0.031(12) 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.12102(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ir1 . Cl2 . 2.4146(10) yes
Ir1 . C3 . 2.099(4) yes
Ir1 . C11 . 2.021(4) yes
Ir1 . C26 . 2.049(4) yes
Ir1 . H8 . 1.52(4) no
C3 . C4 . 1.505(5) yes
C3 . H31 . 0.972 no
C3 . H32 . 0.980 no
C4 . C5 . 1.390(6) yes
C4 . C9 . 1.406(5) yes
C5 . C6 . 1.399(6) yes
C5 . H51 . 0.940 no
C6 . C7 . 1.385(6) yes
C6 . C25 . 1.502(6) yes
C7 . C8 . 1.395(6) yes
C7 . H71 . 0.932 no
C8 . C9 . 1.391(6) yes
C8 . C24 . 1.508(6) yes
C9 . N10 . 1.428(5) yes
N10 . C11 . 1.357(5) yes
N10 . C23 . 1.485(5) yes
C11 . N12 . 1.342(5) yes
N12 . C13 . 1.433(5) yes
N12 . C22 . 1.476(5) yes
C13 . C14 . 1.388(6) yes
C13 . C18 . 1.397(6) yes
C14 . C15 . 1.392(7) yes
C14 . C21 . 1.514(6) yes
C15 . C16 . 1.374(7) yes
C15 . H151 . 0.936 no
C16 . C17 . 1.392(7) yes
C16 . C20 . 1.511(7) yes
C17 . C18 . 1.384(6) yes
C17 . H171 . 0.931 no
C18 . C19 . 1.504(6) yes
C19 . H191 . 0.967 no
C19 . H193 . 0.959 no
C19 . H192 . 0.960 no
C20 . H201 . 0.962 no
C20 . H203 . 0.958 no
C20 . H202 . 0.959 no
C21 . H211 . 0.965 no
C21 . H213 . 0.966 no
C21 . H212 . 0.956 no
C22 . C23 . 1.516(7) yes
C22 . H221 . 0.983 no
C22 . H222 . 0.982 no
C23 . H232 . 0.984 no
C23 . H231 . 0.981 no
C24 . H243 . 0.969 no
C24 . H242 . 0.961 no
C24 . H241 . 0.957 no
C25 . H253 . 0.957 no
C25 . H252 . 0.959 no
C25 . H251 . 0.973 no
C26 . N27 . 1.352(5) yes
C26 . N39 . 1.344(5) yes
N27 . C28 . 1.436(5) yes
N27 . C37 . 1.478(5) yes
C28 . C29 . 1.390(5) yes
C28 . C33 . 1.396(6) yes
C29 . C30 . 1.400(5) yes
C29 . C36 . 1.505(5) yes
C30 . C31 . 1.385(6) yes
C30 . H301 . 0.936 no
C31 . C32 . 1.381(6) yes
C31 . C35 . 1.508(6) yes
C32 . C33 . 1.393(6) yes
C32 . H321 . 0.930 no
C33 . C34 . 1.500(6) yes
C34 . H342 . 0.962 no
C34 . H341 . 0.963 no
C34 . H343 . 0.969 no
C35 . H352 . 0.958 no
C35 . H351 . 0.962 no
C35 . H353 . 0.959 no
C36 . H362 . 0.967 no
C36 . H361 . 0.960 no
C36 . H363 . 0.959 no
C37 . C38 . 1.521(6) yes
C37 . H372 . 0.973 no
C37 . H371 . 0.972 no
C38 . N39 . 1.482(5) yes
C38 . H382 . 0.969 no
C38 . H381 . 0.971 no
N39 . C40 . 1.431(5) yes
C40 . C41 . 1.392(6) yes
C40 . C46 . 1.392(6) yes
C41 . C42 . 1.503(7) yes
C41 . C43 . 1.391(6) yes
C42 . H421 . 0.957 no
C42 . H423 . 0.959 no
C42 . H422 . 0.958 no
C43 . C44 . 1.385(7) yes
C43 . H431 . 0.951 no
C44 . C45 . 1.394(7) yes
C44 . C48 . 1.514(6) yes
C45 . C46 . 1.406(6) yes
C45 . H451 . 0.944 no
C46 . C47 . 1.499(7) yes
C47 . H472 . 0.973 no
C47 . H471 . 0.966 no
C47 . H473 . 0.963 no
C48 . H482 . 0.963 no
C48 . H481 . 0.961 no
C48 . H483 . 0.955 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl2 . Ir1 . C3 . 167.30(11) yes
Cl2 . Ir1 . C11 . 94.26(11) yes
C3 . Ir1 . C11 . 80.12(16) yes
Cl2 . Ir1 . C26 . 89.24(11) yes
C3 . Ir1 . C26 . 97.59(15) yes
C11 . Ir1 . C26 . 173.13(15) yes
Cl2 . Ir1 . H8 . 105.6(17) no
C3 . Ir1 . H8 . 85.4(17) no
C11 . Ir1 . H8 . 84.4(17) no
C26 . Ir1 . H8 . 88.9(17) no
Ir1 . C3 . C4 . 106.1(2) yes
Ir1 . C3 . H31 . 109.2 no
C4 . C3 . H31 . 109.6 no
Ir1 . C3 . H32 . 111.7 no
C4 . C3 . H32 . 110.7 no
H31 . C3 . H32 . 109.5 no
C3 . C4 . C5 . 123.0(4) yes
C3 . C4 . C9 . 119.8(4) yes
C5 . C4 . C9 . 117.1(4) yes
C4 . C5 . C6 . 122.7(4) yes
C4 . C5 . H51 . 118.7 no
C6 . C5 . H51 . 118.6 no
C5 . C6 . C7 . 118.0(4) yes
C5 . C6 . C25 . 121.2(4) yes
C7 . C6 . C25 . 120.8(4) yes
C6 . C7 . C8 . 121.8(4) yes
C6 . C7 . H71 . 119.1 no
C8 . C7 . H71 . 119.1 no
C7 . C8 . C9 . 118.5(4) yes
C7 . C8 . C24 . 119.0(4) yes
C9 . C8 . C24 . 122.3(4) yes
C4 . C9 . C8 . 121.9(4) yes
C4 . C9 . N10 . 118.5(4) yes
C8 . C9 . N10 . 119.6(4) yes
C9 . N10 . C11 . 121.9(3) yes
C9 . N10 . C23 . 121.7(3) yes
C11 . N10 . C23 . 111.8(3) yes
Ir1 . C11 . N10 . 123.6(3) yes
Ir1 . C11 . N12 . 128.8(3) yes
N10 . C11 . N12 . 106.7(3) yes
C11 . N12 . C13 . 127.1(3) yes
C11 . N12 . C22 . 113.3(3) yes
C13 . N12 . C22 . 119.0(3) yes
N12 . C13 . C14 . 119.8(4) yes
N12 . C13 . C18 . 118.5(4) yes
C14 . C13 . C18 . 121.5(4) yes
C13 . C14 . C15 . 117.9(4) yes
C13 . C14 . C21 . 121.5(5) yes
C15 . C14 . C21 . 120.6(4) yes
C14 . C15 . C16 . 122.4(4) yes
C14 . C15 . H151 . 119.1 no
C16 . C15 . H151 . 118.5 no
C15 . C16 . C17 . 118.1(4) yes
C15 . C16 . C20 . 121.6(5) yes
C17 . C16 . C20 . 120.3(5) yes
C16 . C17 . C18 . 121.9(4) yes
C16 . C17 . H171 . 118.5 no
C18 . C17 . H171 . 119.5 no
C13 . C18 . C17 . 118.1(4) yes
C13 . C18 . C19 . 121.1(4) yes
C17 . C18 . C19 . 120.8(4) yes
C18 . C19 . H191 . 109.3 no
C18 . C19 . H193 . 108.1 no
H191 . C19 . H193 . 110.3 no
C18 . C19 . H192 . 109.2 no
H191 . C19 . H192 . 109.5 no
H193 . C19 . H192 . 110.4 no
C16 . C20 . H201 . 109.4 no
C16 . C20 . H203 . 109.0 no
H201 . C20 . H203 . 109.8 no
C16 . C20 . H202 . 109.1 no
H201 . C20 . H202 . 110.0 no
H203 . C20 . H202 . 109.5 no
C14 . C21 . H211 . 108.1 no
C14 . C21 . H213 . 109.2 no
H211 . C21 . H213 . 110.1 no
C14 . C21 . H212 . 109.0 no
H211 . C21 . H212 . 110.2 no
H213 . C21 . H212 . 110.2 no
N12 . C22 . C23 . 101.5(3) yes
N12 . C22 . H221 . 111.3 no
C23 . C22 . H221 . 112.6 no
N12 . C22 . H222 . 110.3 no
C23 . C22 . H222 . 110.7 no
H221 . C22 . H222 . 110.2 no
C22 . C23 . N10 . 101.1(4) yes
C22 . C23 . H232 . 110.7 no
N10 . C23 . H232 . 110.5 no
C22 . C23 . H231 . 112.8 no
N10 . C23 . H231 . 111.5 no
H232 . C23 . H231 . 110.0 no
C8 . C24 . H243 . 108.6 no
C8 . C24 . H242 . 109.1 no
H243 . C24 . H242 . 109.5 no
C8 . C24 . H241 . 110.1 no
H243 . C24 . H241 . 109.7 no
H242 . C24 . H241 . 109.7 no
C6 . C25 . H253 . 111.0 no
C6 . C25 . H252 . 108.9 no
H253 . C25 . H252 . 109.5 no
C6 . C25 . H251 . 109.1 no
H253 . C25 . H251 . 109.1 no
H252 . C25 . H251 . 109.1 no
Ir1 . C26 . N27 . 124.6(3) yes
Ir1 . C26 . N39 . 128.2(3) yes
N27 . C26 . N39 . 106.8(3) yes
C26 . N27 . C28 . 126.8(3) yes
C26 . N27 . C37 . 113.9(3) yes
C28 . N27 . C37 . 119.3(3) yes
N27 . C28 . C29 . 120.2(4) yes
N27 . C28 . C33 . 118.2(4) yes
C29 . C28 . C33 . 121.5(4) yes
C28 . C29 . C30 . 117.8(4) yes
C28 . C29 . C36 . 122.8(4) yes
C30 . C29 . C36 . 119.4(4) yes
C29 . C30 . C31 . 122.3(4) yes
C29 . C30 . H301 . 119.0 no
C31 . C30 . H301 . 118.6 no
C30 . C31 . C32 . 117.9(4) yes
C30 . C31 . C35 . 121.1(4) yes
C32 . C31 . C35 . 121.0(4) yes
C31 . C32 . C33 . 122.3(4) yes
C31 . C32 . H321 . 118.7 no
C33 . C32 . H321 . 119.0 no
C28 . C33 . C32 . 118.2(4) yes
C28 . C33 . C34 . 121.9(4) yes
C32 . C33 . C34 . 120.0(4) yes
C33 . C34 . H342 . 110.3 no
C33 . C34 . H341 . 109.1 no
H342 . C34 . H341 . 108.2 no
C33 . C34 . H343 . 111.2 no
H342 . C34 . H343 . 109.1 no
H341 . C34 . H343 . 108.9 no
C31 . C35 . H352 . 109.0 no
C31 . C35 . H351 . 110.1 no
H352 . C35 . H351 . 109.8 no
C31 . C35 . H353 . 108.8 no
H352 . C35 . H353 . 109.4 no
H351 . C35 . H353 . 109.7 no
C29 . C36 . H362 . 110.4 no
C29 . C36 . H361 . 109.3 no
H362 . C36 . H361 . 109.2 no
C29 . C36 . H363 . 109.6 no
H362 . C36 . H363 . 109.6 no
H361 . C36 . H363 . 108.7 no
N27 . C37 . C38 . 102.5(3) yes
N27 . C37 . H372 . 110.9 no
C38 . C37 . H372 . 110.7 no
N27 . C37 . H371 . 110.8 no
C38 . C37 . H371 . 111.5 no
H372 . C37 . H371 . 110.4 no
C37 . C38 . N39 . 102.5(3) yes
C37 . C38 . H382 . 110.9 no
N39 . C38 . H382 . 112.0 no
C37 . C38 . H381 . 109.6 no
N39 . C38 . H381 . 111.5 no
H382 . C38 . H381 . 110.1 no
C38 . N39 . C26 . 114.0(3) yes
C38 . N39 . C40 . 118.9(3) yes
C26 . N39 . C40 . 126.0(3) yes
N39 . C40 . C41 . 120.0(4) yes
N39 . C40 . C46 . 118.6(4) yes
C41 . C40 . C46 . 121.2(4) yes
C40 . C41 . C42 . 122.4(4) yes
C40 . C41 . C43 . 118.4(4) yes
C42 . C41 . C43 . 119.1(5) yes
C41 . C42 . H421 . 109.9 no
C41 . C42 . H423 . 108.3 no
H421 . C42 . H423 . 109.1 no
C41 . C42 . H422 . 109.0 no
H421 . C42 . H422 . 110.6 no
H423 . C42 . H422 . 109.9 no
C41 . C43 . C44 . 122.5(5) yes
C41 . C43 . H431 . 119.6 no
C44 . C43 . H431 . 117.9 no
C43 . C44 . C45 . 117.8(4) yes
C43 . C44 . C48 . 120.6(5) yes
C45 . C44 . C48 . 121.6(5) yes
C44 . C45 . C46 . 121.6(4) yes
C44 . C45 . H451 . 119.3 no
C46 . C45 . H451 . 119.0 no
C45 . C46 . C40 . 118.3(4) yes
C45 . C46 . C47 . 120.1(4) yes
C40 . C46 . C47 . 121.3(4) yes
C46 . C47 . H472 . 108.9 no
C46 . C47 . H471 . 109.4 no
H472 . C47 . H471 . 109.4 no
C46 . C47 . H473 . 109.3 no
H472 . C47 . H473 . 110.0 no
H471 . C47 . H473 . 109.7 no
C44 . C48 . H482 . 107.7 no
C44 . C48 . H481 . 109.0 no
H482 . C48 . H481 . 109.9 no
C44 . C48 . H483 . 109.9 no
H482 . C48 . H483 . 110.1 no
H481 . C48 . H483 . 110.2 no
_database_code_depnum_ccdc_archive 'CCDC 1002302'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_5
#==============================================================================
_audit_creation_date             12-11-29
_audit_creation_method           CRYSTALS_ver_14.23

_oxford_structure_analysis_title 024np11
_chemical_name_systematic        .
_chemical_melting_point          .

_cell_length_a                   17.0027(1)
_cell_length_b                   19.4001(1)
_cell_length_c                   23.4149(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7723.50(9)

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P b c a '
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,z
x+1/2,-y+1/2,-z
x,-y+1/2,z+1/2
-x,y+1/2,-z+1/2
-x+1/2,-y,z+1/2
x+1/2,y,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ir -1.4442 7.9887 27.3049 1.5928 16.7296 8.8655 15.6115 0.4179 5.8338 45.0011
11.4722 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            8

# Given Formula = C42 H54 Cl1 Ir1 N4 
# Dc =      1.45 Fooo =   3424.00 Mu =     35.60 M =    842.59
# Found Formula = C42 H54 Cl1 Ir1 N4 
# Dc =      1.45 FOOO =   3424.00 Mu =     35.60 M =    842.59

_chemical_formula_sum            'C42 H54 Cl Ir N4'
_chemical_formula_moiety         'C42 H54 Cl Ir N4'
_chemical_compound_source        .
_chemical_formula_weight         842.59


_cell_measurement_reflns_used    9552
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.060
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_max          0.180

_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             3424
_exptl_absorpt_coefficient_mu    3.560

# Sheldrick geometric approximatio 0.57 0.81 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_T_max  0.81
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            158718
_reflns_number_total             8784
_diffrn_reflns_av_R_equivalents  0.033
# Number of reflections without Friedels Law is 16830 
# Number of reflections with Friedels Law is 8784 
# Theoretical number of reflections is about 8845 


_diffrn_reflns_theta_min         5.103
_diffrn_reflns_theta_max         27.470
_diffrn_measured_fraction_theta_max 0.992

_diffrn_reflns_theta_full        26.921
_diffrn_measured_fraction_theta_full 0.993


_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_reflns_limit_h_min              0
_reflns_limit_h_max              22
_reflns_limit_k_min              0
_reflns_limit_k_max              25
_reflns_limit_l_min              0
_reflns_limit_l_max              30

_oxford_diffrn_Wilson_B_factor   1.97
_oxford_diffrn_Wilson_scale      518.47

_atom_sites_solution_primary     Direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.75
_refine_diff_density_max         2.51


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         8784
_refine_ls_number_restraints     0
_refine_ls_number_parameters     434
_oxford_refine_ls_R_factor_ref   0.0643
_refine_ls_wR_factor_ref         0.0768
_refine_ls_goodness_of_fit_ref   1.0092
_refine_ls_shift/su_max          0.0013191
_refine_ls_shift/su_mean         0.0000265


# The values computed from all data 
_oxford_reflns_number_all        8784
_refine_ls_R_factor_all          0.0643
_refine_ls_wR_factor_all         0.0768

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5861
_refine_ls_R_factor_gt           0.0311
_refine_ls_wR_factor_gt          0.0542

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 2.09 2.22 0.572 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ir1 Ir 0.617175(12) 0.649707(9) 0.665697(8) 0.0240 1.0000 Uani . . . . . .
Cl2 Cl 0.75395(9) 0.63004(8) 0.64545(7) 0.0423 1.0000 Uani . . . . . .
C3 C 0.6339(3) 0.7513(3) 0.6791(2) 0.0295 1.0000 Uani . . . . . .
N4 N 0.6083(3) 0.8041(2) 0.64679(19) 0.0355 1.0000 Uani . . . . . .
C5 C 0.5604(4) 0.7984(3) 0.5970(2) 0.0344 1.0000 Uani . . . . . .
C6 C 0.4803(4) 0.8137(3) 0.6014(3) 0.0428 1.0000 Uani . . . . . .
C7 C 0.4453(4) 0.8350(3) 0.6579(3) 0.0540 1.0000 Uani . . . . . .
H73 H 0.3891 0.8306 0.6563 0.0810 1.0000 Uiso R . . . . .
H72 H 0.4587 0.8824 0.6657 0.0810 1.0000 Uiso R . . . . .
H71 H 0.4653 0.8063 0.6880 0.0809 1.0000 Uiso R . . . . .
C8 C 0.4332(4) 0.8075(3) 0.5531(3) 0.0497 1.0000 Uani . . . . . .
C9 C 0.4632(4) 0.7876(3) 0.5011(3) 0.0462 1.0000 Uani . . . . . .
C10 C 0.5441(4) 0.7751(3) 0.4974(3) 0.0435 1.0000 Uani . . . . . .
C11 C 0.5936(4) 0.7801(3) 0.5441(2) 0.0351 1.0000 Uani . . . . . .
C12 C 0.6798(4) 0.7644(3) 0.5386(3) 0.0397 1.0000 Uani . . . . . .
H123 H 0.6941 0.7630 0.4991 0.0589 1.0000 Uiso R . . . . .
H122 H 0.7103 0.7992 0.5573 0.0593 1.0000 Uiso R . . . . .
H121 H 0.6912 0.7204 0.5558 0.0590 1.0000 Uiso R . . . . .
H101 H 0.5650 0.7630 0.4623 0.0519 1.0000 Uiso R . . . . .
C13 C 0.4107(5) 0.7778(5) 0.4495(3) 0.0706 1.0000 Uani . . . . . .
H132 H 0.4359 0.7962 0.4161 0.1050 1.0000 Uiso R . . . . .
H131 H 0.3620 0.8013 0.4555 0.1050 1.0000 Uiso R . . . . .
H133 H 0.4005 0.7297 0.4438 0.1050 1.0000 Uiso R . . . . .
H81 H 0.3797 0.8172 0.5561 0.0590 1.0000 Uiso R . . . . .
C14 C 0.6351(5) 0.8719(3) 0.6669(3) 0.0527 1.0000 Uani . . . . . .
C15 C 0.6660(5) 0.8552(3) 0.7259(3) 0.0541 1.0000 Uani . . . . . .
N16 N 0.6730(3) 0.7801(2) 0.7239(2) 0.0347 1.0000 Uani . . . . . .
C17 C 0.7027(4) 0.7420(3) 0.7721(2) 0.0333 1.0000 Uani . . . . . .
C18 C 0.6516(4) 0.7195(3) 0.8150(2) 0.0338 1.0000 Uani . . . . . .
C19 C 0.6831(4) 0.6848(3) 0.8614(2) 0.0365 1.0000 Uani . . . . . .
C20 C 0.7628(4) 0.6717(3) 0.8663(3) 0.0430 1.0000 Uani . . . . . .
C21 C 0.8119(4) 0.6964(3) 0.8236(3) 0.0461 1.0000 Uani . . . . . .
C22 C 0.7836(4) 0.7309(3) 0.7761(3) 0.0417 1.0000 Uani . . . . . .
C23 C 0.8385(4) 0.7560(4) 0.7302(3) 0.0580 1.0000 Uani . . . . . .
H233 H 0.8894 0.7357 0.7352 0.0871 1.0000 Uiso R . . . . .
H231 H 0.8436 0.8048 0.7325 0.0870 1.0000 Uiso R . . . . .
H232 H 0.8188 0.7435 0.6933 0.0870 1.0000 Uiso R . . . . .
H211 H 0.8656 0.6896 0.8270 0.0550 1.0000 Uiso R . . . . .
C24 C 0.7956(5) 0.6324(4) 0.9167(3) 0.0633 1.0000 Uani . . . . . .
H241 H 0.8366 0.6589 0.9341 0.0950 1.0000 Uiso R . . . . .
H242 H 0.7551 0.6236 0.9442 0.0951 1.0000 Uiso R . . . . .
H243 H 0.8170 0.5895 0.9036 0.0950 1.0000 Uiso R . . . . .
H191 H 0.6496 0.6694 0.8898 0.0441 1.0000 Uiso R . . . . .
C25 C 0.5643(4) 0.7334(3) 0.8130(3) 0.0409 1.0000 Uani . . . . . .
H252 H 0.5359 0.6920 0.8205 0.0613 1.0000 Uiso R . . . . .
H253 H 0.5507 0.7672 0.8412 0.0611 1.0000 Uiso R . . . . .
H251 H 0.5496 0.7506 0.7761 0.0610 1.0000 Uiso R . . . . .
H151 H 0.7163 0.8766 0.7326 0.0652 1.0000 Uiso R . . . . .
H152 H 0.6288 0.8694 0.7552 0.0652 1.0000 Uiso R . . . . .
H141 H 0.6770 0.8899 0.6431 0.0630 1.0000 Uiso R . . . . .
H142 H 0.5927 0.9050 0.6682 0.0629 1.0000 Uiso R . . . . .
C26 C 0.5935(3) 0.5493(3) 0.6537(2) 0.0294 1.0000 Uani . . . . . .
N27 N 0.6060(3) 0.5119(2) 0.60555(19) 0.0370 1.0000 Uani . . . . . .
C28 C 0.6312(4) 0.5395(3) 0.5513(2) 0.0345 1.0000 Uani . . . . . .
C29 C 0.7059(4) 0.5233(3) 0.5315(3) 0.0404 1.0000 Uani . . . . . .
C30 C 0.7300(4) 0.5499(3) 0.4791(3) 0.0431 1.0000 Uani . . . . . .
C31 C 0.6818(4) 0.5915(3) 0.4469(2) 0.0369 1.0000 Uani . . . . . .
C32 C 0.7092(4) 0.6210(4) 0.3903(3) 0.0513 1.0000 Uani . . . . . .
H321 H 0.6719 0.6096 0.3610 0.0772 1.0000 Uiso R . . . . .
H323 H 0.7145 0.6704 0.3930 0.0770 1.0000 Uiso R . . . . .
H322 H 0.7591 0.6012 0.3805 0.0771 1.0000 Uiso R . . . . .
C33 C 0.6076(4) 0.6058(3) 0.4671(2) 0.0367 1.0000 Uani . . . . . .
C34 C 0.5800(4) 0.5803(3) 0.5192(2) 0.0350 1.0000 Uani . . . . . .
C35 C 0.4972(4) 0.5947(4) 0.5384(3) 0.0481 1.0000 Uani . . . . . .
H351 H 0.4726 0.6263 0.5122 0.0721 1.0000 Uiso R . . . . .
H353 H 0.4975 0.6152 0.5759 0.0722 1.0000 Uiso R . . . . .
H352 H 0.4671 0.5528 0.5392 0.0721 1.0000 Uiso R . . . . .
H331 H 0.5745 0.6335 0.4454 0.0440 1.0000 Uiso R . . . . .
H301 H 0.7804 0.5396 0.4662 0.0520 1.0000 Uiso R . . . . .
C36 C 0.7608(5) 0.4779(4) 0.5648(3) 0.0552 1.0000 Uani . . . . . .
H362 H 0.8119 0.4789 0.5471 0.0830 1.0000 Uiso R . . . . .
H361 H 0.7649 0.4941 0.6032 0.0830 1.0000 Uiso R . . . . .
H363 H 0.7416 0.4315 0.5651 0.0829 1.0000 Uiso R . . . . .
C37 C 0.5749(6) 0.4411(3) 0.6088(3) 0.0613 1.0000 Uani . . . . . .
C38 C 0.5528(5) 0.4343(3) 0.6710(3) 0.0558 1.0000 Uani . . . . . .
N39 N 0.5608(3) 0.5057(2) 0.6919(2) 0.0345 1.0000 Uani . . . . . .
C40 C 0.5465(3) 0.5198(3) 0.7509(2) 0.0300 1.0000 Uani . . . . . .
C41 C 0.6083(4) 0.5182(3) 0.7895(2) 0.0340 1.0000 Uani . . . . . .
C42 C 0.5912(5) 0.5266(3) 0.8471(3) 0.0467 1.0000 Uani . . . . . .
C43 C 0.5168(5) 0.5378(3) 0.8666(3) 0.0564 1.0000 Uani . . . . . .
C44 C 0.4562(4) 0.5428(3) 0.8277(4) 0.0536 1.0000 Uani . . . . . .
C45 C 0.4697(4) 0.5332(3) 0.7691(3) 0.0425 1.0000 Uani . . . . . .
C46 C 0.4037(4) 0.5381(4) 0.7266(4) 0.0722 1.0000 Uani . . . . . .
H462 H 0.3591 0.5597 0.7438 0.1081 1.0000 Uiso R . . . . .
H461 H 0.4203 0.5648 0.6942 0.1080 1.0000 Uiso R . . . . .
H463 H 0.3892 0.4928 0.7138 0.1080 1.0000 Uiso R . . . . .
H441 H 0.4044 0.5530 0.8397 0.0634 1.0000 Uiso R . . . . .
C47 C 0.5001(8) 0.5431(5) 0.9301(4) 0.1085 1.0000 Uani . . . . . .
H472 H 0.4462 0.5567 0.9357 0.1650 1.0000 Uiso R . . . . .
H471 H 0.5343 0.5768 0.9470 0.1649 1.0000 Uiso R . . . . .
H473 H 0.5088 0.4993 0.9478 0.1650 1.0000 Uiso R . . . . .
H421 H 0.6318 0.5248 0.8733 0.0559 1.0000 Uiso R . . . . .
C48 C 0.6918(4) 0.5087(4) 0.7704(3) 0.0541 1.0000 Uani . . . . . .
H481 H 0.7251 0.5031 0.8030 0.0810 1.0000 Uiso R . . . . .
H483 H 0.7090 0.5485 0.7494 0.0812 1.0000 Uiso R . . . . .
H482 H 0.6957 0.4686 0.7467 0.0811 1.0000 Uiso R . . . . .
H382 H 0.5890 0.4040 0.6907 0.0669 1.0000 Uiso R . . . . .
H381 H 0.4994 0.4173 0.6754 0.0672 1.0000 Uiso R . . . . .
H372 H 0.6147 0.4079 0.5985 0.0731 1.0000 Uiso R . . . . .
H371 H 0.5296 0.4353 0.5844 0.0730 1.0000 Uiso R . . . . .
H12 H 0.5559 0.6504 0.7177 0.0457 1.0000 Uiso R . . . . .
H11 H 0.5314 0.6662 0.6521 0.0699 1.0000 Uiso R . . . . .

_refine_ls_extinction_coef       131(7)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.046670(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ir1 . Cl2 . 2.4038(15) yes
Ir1 . C3 . 2.016(5) yes
Ir1 . C26 . 2.008(5) yes
Ir1 . H12 . 1.603 no
Ir1 . H11 . 1.526 no
C3 . N4 . 1.346(7) yes
C3 . N16 . 1.362(7) yes
N4 . C5 . 1.426(8) yes
N4 . C14 . 1.470(7) yes
C5 . C6 . 1.400(9) yes
C5 . C11 . 1.407(8) yes
C6 . C7 . 1.509(9) yes
C6 . C8 . 1.390(10) yes
C7 . H73 . 0.961 no
C7 . H72 . 0.965 no
C7 . H71 . 0.960 no
C8 . C9 . 1.375(10) yes
C8 . H81 . 0.932 no
C9 . C10 . 1.399(9) yes
C9 . C13 . 1.516(10) yes
C10 . C11 . 1.383(9) yes
C10 . H101 . 0.925 no
C11 . C12 . 1.501(8) yes
C12 . H123 . 0.956 no
C12 . H122 . 0.956 no
C12 . H121 . 0.963 no
C13 . H132 . 0.960 no
C13 . H131 . 0.956 no
C13 . H133 . 0.959 no
C14 . C15 . 1.514(9) yes
C14 . H141 . 0.969 no
C14 . H142 . 0.966 no
C15 . N16 . 1.463(8) yes
C15 . H151 . 0.964 no
C15 . H152 . 0.973 no
N16 . C17 . 1.439(7) yes
C17 . C18 . 1.399(8) yes
C17 . C22 . 1.395(8) yes
C18 . C19 . 1.384(8) yes
C18 . C25 . 1.511(8) yes
C19 . C20 . 1.384(9) yes
C19 . H191 . 0.926 no
C20 . C21 . 1.387(9) yes
C20 . C24 . 1.512(9) yes
C21 . C22 . 1.386(9) yes
C21 . H211 . 0.925 no
C22 . C23 . 1.504(9) yes
C23 . H233 . 0.958 no
C23 . H231 . 0.954 no
C23 . H232 . 0.958 no
C24 . H241 . 0.957 no
C24 . H242 . 0.958 no
C24 . H243 . 0.957 no
C25 . H252 . 0.954 no
C25 . H253 . 0.959 no
C25 . H251 . 0.958 no
C26 . N27 . 1.357(7) yes
C26 . N39 . 1.353(7) yes
N27 . C28 . 1.444(7) yes
N27 . C37 . 1.473(7) yes
C28 . C29 . 1.388(9) yes
C28 . C34 . 1.397(8) yes
C29 . C30 . 1.392(9) yes
C29 . C36 . 1.502(8) yes
C30 . C31 . 1.375(8) yes
C30 . H301 . 0.931 no
C31 . C32 . 1.516(8) yes
C31 . C33 . 1.376(9) yes
C32 . H321 . 0.961 no
C32 . H323 . 0.964 no
C32 . H322 . 0.960 no
C33 . C34 . 1.397(8) yes
C33 . H331 . 0.929 no
C34 . C35 . 1.504(9) yes
C35 . H351 . 0.964 no
C35 . H353 . 0.962 no
C35 . H352 . 0.961 no
C36 . H362 . 0.962 no
C36 . H361 . 0.954 no
C36 . H363 . 0.957 no
C37 . C38 . 1.510(9) yes
C37 . H372 . 0.966 no
C37 . H371 . 0.965 no
C38 . N39 . 1.476(7) yes
C38 . H382 . 0.968 no
C38 . H381 . 0.973 no
N39 . C40 . 1.429(7) yes
C40 . C41 . 1.385(8) yes
C40 . C45 . 1.398(8) yes
C41 . C42 . 1.390(8) yes
C41 . C48 . 1.499(9) yes
C42 . C43 . 1.362(10) yes
C42 . H421 . 0.925 no
C43 . C44 . 1.379(11) yes
C43 . C47 . 1.519(10) yes
C44 . C45 . 1.402(10) yes
C44 . H441 . 0.946 no
C45 . C46 . 1.502(10) yes
C46 . H462 . 0.956 no
C46 . H461 . 0.962 no
C46 . H463 . 0.960 no
C47 . H472 . 0.962 no
C47 . H471 . 0.960 no
C47 . H473 . 0.956 no
C48 . H481 . 0.956 no
C48 . H483 . 0.960 no
C48 . H482 . 0.958 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl2 . Ir1 . C3 . 92.81(15) yes
Cl2 . Ir1 . C26 . 90.70(16) yes
C3 . Ir1 . C26 . 176.5(2) yes
Cl2 . Ir1 . H12 . 141.3 no
C3 . Ir1 . H12 . 88.0 no
C26 . Ir1 . H12 . 89.1 no
Cl2 . Ir1 . H11 . 156.4 no
C3 . Ir1 . H11 . 87.8 no
C26 . Ir1 . H11 . 89.0 no
H12 . Ir1 . H11 . 62.3 no
Ir1 . C3 . N4 . 127.7(4) yes
Ir1 . C3 . N16 . 126.1(4) yes
N4 . C3 . N16 . 106.2(5) yes
C3 . N4 . C5 . 125.8(4) yes
C3 . N4 . C14 . 113.7(5) yes
C5 . N4 . C14 . 120.6(5) yes
N4 . C5 . C6 . 118.6(5) yes
N4 . C5 . C11 . 120.7(6) yes
C6 . C5 . C11 . 120.6(6) yes
C5 . C6 . C7 . 120.4(6) yes
C5 . C6 . C8 . 118.8(6) yes
C7 . C6 . C8 . 120.7(6) yes
C6 . C7 . H73 . 109.5 no
C6 . C7 . H72 . 109.6 no
H73 . C7 . H72 . 109.1 no
C6 . C7 . H71 . 110.2 no
H73 . C7 . H71 . 109.3 no
H72 . C7 . H71 . 109.3 no
C6 . C8 . C9 . 122.1(6) yes
C6 . C8 . H81 . 118.9 no
C9 . C8 . H81 . 119.0 no
C8 . C9 . C10 . 117.9(6) yes
C8 . C9 . C13 . 121.5(6) yes
C10 . C9 . C13 . 120.5(7) yes
C9 . C10 . C11 . 122.5(6) yes
C9 . C10 . H101 . 118.6 no
C11 . C10 . H101 . 118.9 no
C5 . C11 . C10 . 118.0(6) yes
C5 . C11 . C12 . 121.1(6) yes
C10 . C11 . C12 . 120.9(5) yes
C11 . C12 . H123 . 109.6 no
C11 . C12 . H122 . 110.4 no
H123 . C12 . H122 . 108.8 no
C11 . C12 . H121 . 109.9 no
H123 . C12 . H121 . 109.1 no
H122 . C12 . H121 . 109.0 no
C9 . C13 . H132 . 109.8 no
C9 . C13 . H131 . 109.4 no
H132 . C13 . H131 . 109.3 no
C9 . C13 . H133 . 109.8 no
H132 . C13 . H133 . 109.3 no
H131 . C13 . H133 . 109.3 no
N4 . C14 . C15 . 102.0(5) yes
N4 . C14 . H141 . 111.5 no
C15 . C14 . H141 . 110.3 no
N4 . C14 . H142 . 111.9 no
C15 . C14 . H142 . 111.8 no
H141 . C14 . H142 . 109.2 no
C14 . C15 . N16 . 102.3(5) yes
C14 . C15 . H151 . 111.3 no
N16 . C15 . H151 . 111.2 no
C14 . C15 . H152 . 110.9 no
N16 . C15 . H152 . 111.0 no
H151 . C15 . H152 . 109.9 no
C15 . N16 . C3 . 113.1(5) yes
C15 . N16 . C17 . 121.0(5) yes
C3 . N16 . C17 . 124.4(4) yes
N16 . C17 . C18 . 120.4(5) yes
N16 . C17 . C22 . 118.6(5) yes
C18 . C17 . C22 . 121.0(6) yes
C17 . C18 . C19 . 118.4(6) yes
C17 . C18 . C25 . 122.1(6) yes
C19 . C18 . C25 . 119.5(6) yes
C18 . C19 . C20 . 122.2(6) yes
C18 . C19 . H191 . 118.9 no
C20 . C19 . H191 . 118.9 no
C19 . C20 . C21 . 117.8(6) yes
C19 . C20 . C24 . 121.3(7) yes
C21 . C20 . C24 . 121.0(6) yes
C20 . C21 . C22 . 122.4(6) yes
C20 . C21 . H211 . 118.9 no
C22 . C21 . H211 . 118.7 no
C17 . C22 . C21 . 118.2(6) yes
C17 . C22 . C23 . 120.9(6) yes
C21 . C22 . C23 . 120.9(6) yes
C22 . C23 . H233 . 110.0 no
C22 . C23 . H231 . 109.8 no
H233 . C23 . H231 . 108.6 no
C22 . C23 . H232 . 110.2 no
H233 . C23 . H232 . 108.9 no
H231 . C23 . H232 . 109.4 no
C20 . C24 . H241 . 109.2 no
C20 . C24 . H242 . 110.5 no
H241 . C24 . H242 . 109.4 no
C20 . C24 . H243 . 109.2 no
H241 . C24 . H243 . 109.2 no
H242 . C24 . H243 . 109.4 no
C18 . C25 . H252 . 109.9 no
C18 . C25 . H253 . 109.7 no
H252 . C25 . H253 . 109.1 no
C18 . C25 . H251 . 110.3 no
H252 . C25 . H251 . 109.2 no
H253 . C25 . H251 . 108.8 no
Ir1 . C26 . N27 . 127.2(4) yes
Ir1 . C26 . N39 . 126.6(4) yes
N27 . C26 . N39 . 106.2(4) yes
C26 . N27 . C28 . 125.3(4) yes
C26 . N27 . C37 . 113.5(5) yes
C28 . N27 . C37 . 119.9(5) yes
N27 . C28 . C29 . 118.8(5) yes
N27 . C28 . C34 . 119.9(6) yes
C29 . C28 . C34 . 121.2(5) yes
C28 . C29 . C30 . 118.7(6) yes
C28 . C29 . C36 . 121.8(6) yes
C30 . C29 . C36 . 119.5(6) yes
C29 . C30 . C31 . 121.7(6) yes
C29 . C30 . H301 . 118.6 no
C31 . C30 . H301 . 119.7 no
C30 . C31 . C32 . 121.2(6) yes
C30 . C31 . C33 . 118.4(6) yes
C32 . C31 . C33 . 120.4(6) yes
C31 . C32 . H321 . 109.5 no
C31 . C32 . H323 . 110.4 no
H321 . C32 . H323 . 109.8 no
C31 . C32 . H322 . 109.2 no
H321 . C32 . H322 . 108.7 no
H323 . C32 . H322 . 109.2 no
C31 . C33 . C34 . 122.5(6) yes
C31 . C33 . H331 . 118.9 no
C34 . C33 . H331 . 118.6 no
C33 . C34 . C28 . 117.5(6) yes
C33 . C34 . C35 . 120.6(6) yes
C28 . C34 . C35 . 121.9(6) yes
C34 . C35 . H351 . 109.5 no
C34 . C35 . H353 . 110.2 no
H351 . C35 . H353 . 108.8 no
C34 . C35 . H352 . 110.3 no
H351 . C35 . H352 . 108.6 no
H353 . C35 . H352 . 109.5 no
C29 . C36 . H362 . 109.0 no
C29 . C36 . H361 . 110.0 no
H362 . C36 . H361 . 109.5 no
C29 . C36 . H363 . 110.0 no
H362 . C36 . H363 . 109.2 no
H361 . C36 . H363 . 109.2 no
N27 . C37 . C38 . 102.8(5) yes
N27 . C37 . H372 . 110.9 no
C38 . C37 . H372 . 110.9 no
N27 . C37 . H371 . 111.3 no
C38 . C37 . H371 . 111.3 no
H372 . C37 . H371 . 109.5 no
C37 . C38 . N39 . 102.4(5) yes
C37 . C38 . H382 . 110.8 no
N39 . C38 . H382 . 110.7 no
C37 . C38 . H381 . 111.3 no
N39 . C38 . H381 . 111.6 no
H382 . C38 . H381 . 109.8 no
C38 . N39 . C26 . 113.9(5) yes
C38 . N39 . C40 . 119.0(5) yes
C26 . N39 . C40 . 126.2(4) yes
N39 . C40 . C41 . 119.8(5) yes
N39 . C40 . C45 . 119.3(5) yes
C41 . C40 . C45 . 120.9(6) yes
C40 . C41 . C42 . 118.1(6) yes
C40 . C41 . C48 . 121.8(6) yes
C42 . C41 . C48 . 120.1(6) yes
C41 . C42 . C43 . 122.5(7) yes
C41 . C42 . H421 . 119.0 no
C43 . C42 . H421 . 118.5 no
C42 . C43 . C44 . 118.9(6) yes
C42 . C43 . C47 . 120.9(9) yes
C44 . C43 . C47 . 120.2(9) yes
C43 . C44 . C45 . 121.0(6) yes
C43 . C44 . H441 . 121.0 no
C45 . C44 . H441 . 118.0 no
C44 . C45 . C40 . 118.4(6) yes
C44 . C45 . C46 . 121.2(7) yes
C40 . C45 . C46 . 120.5(6) yes
C45 . C46 . H462 . 110.0 no
C45 . C46 . H461 . 109.8 no
H462 . C46 . H461 . 109.2 no
C45 . C46 . H463 . 110.0 no
H462 . C46 . H463 . 109.2 no
H461 . C46 . H463 . 108.6 no
C43 . C47 . H472 . 109.3 no
C43 . C47 . H471 . 109.6 no
H472 . C47 . H471 . 109.5 no
C43 . C47 . H473 . 109.5 no
H472 . C47 . H473 . 109.4 no
H471 . C47 . H473 . 109.4 no
C41 . C48 . H481 . 109.7 no
C41 . C48 . H483 . 110.0 no
H481 . C48 . H483 . 108.7 no
C41 . C48 . H482 . 109.7 no
H481 . C48 . H482 . 109.2 no
H483 . C48 . H482 . 109.6 no
_database_code_depnum_ccdc_archive 'CCDC 1002303'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_8
#==============================================================================
_audit_creation_date             14-02-10
_audit_creation_method           CRYSTALS_ver_14.23

_oxford_structure_analysis_title 049NPMK11
_chemical_name_systematic        .
_chemical_melting_point          .

_cell_length_a                   42.9414(5)
_cell_length_b                   21.5369(3)
_cell_length_c                   8.42331(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7790.10(15)

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'F d d 2 '
_symmetry_space_group_name_Hall  'F 2 -2d'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x,y+1/2,z+1/2
x+1/2,y,z+1/2
x+1/2,y+1/2,z
-x+1/4,y+1/4,z+1/4
-x+1/4,y+3/4,z+3/4
-x+3/4,y+1/4,z+3/4
-x+3/4,y+3/4,z+1/4
x+1/4,-y+1/4,z+1/4
x+1/4,-y+3/4,z+3/4
x+3/4,-y+1/4,z+3/4
x+3/4,-y+3/4,z+1/4
-x+1/2,-y,z+1/2
-x+1/2,-y+1/2,z+1
-x+1,-y,z+1
-x+1,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ir -4.7710 6.5667 27.3049 1.5928 16.7296 8.8655 15.6115 0.4179 5.8338 45.0011
11.4722 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            8

# Given Formula = C88 H116 Cl2 Ir2 N8 
# Dc =      2.97 Fooo =   3536.00 Mu =    150.60 M =    870.64
# Found Formula = C44 H56 Cl1 Ir1 N4 
# Dc =      1.48 FOOO =   3536.00 Mu =     75.30 M =    434.31

_chemical_formula_sum            'C44 H56 Cl1 Ir1 N4'
_chemical_formula_moiety         'C44 H56 Cl1 Ir1 N4'
_chemical_compound_source        .
_chemical_formula_weight         868.63


_cell_measurement_reflns_used    14970
_cell_measurement_theta_min      4
_cell_measurement_theta_max      76
_cell_measurement_temperature    150

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.080
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.250

_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             3536
_exptl_absorpt_coefficient_mu    7.530

# Sheldrick geometric approximatio 0.32 0.55 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.25
_exptl_absorpt_correction_T_max  0.55
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω/2θ

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            21447
_reflns_number_total             3523
_diffrn_reflns_av_R_equivalents  0.029
# Number of reflections without Friedels Law is 3523 
# Number of reflections with Friedels Law is 2192 
# Theoretical number of reflections is about 2050 


_diffrn_reflns_theta_min         4.118
_diffrn_reflns_theta_max         76.634
_diffrn_measured_fraction_theta_max 0.997

_diffrn_reflns_theta_full        76.634
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       10
_reflns_limit_h_min              0
_reflns_limit_h_max              54
_reflns_limit_k_min              0
_reflns_limit_k_max              27
_reflns_limit_l_min              -8
_reflns_limit_l_max              10

_oxford_diffrn_Wilson_B_factor   1.30
_oxford_diffrn_Wilson_scale      1.56

_atom_sites_solution_primary     Direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.01
_refine_diff_density_max         1.06


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         3506
_refine_ls_number_restraints     1
_refine_ls_number_parameters     229
_oxford_refine_ls_R_factor_ref   0.0211
_refine_ls_wR_factor_ref         0.0571
_refine_ls_goodness_of_fit_ref   1.0634
_refine_ls_shift/su_max          0.0006405
_refine_ls_shift/su_mean         0.0000962


# The values computed from all data 
_oxford_reflns_number_all        3506
_refine_ls_R_factor_all          0.0211
_refine_ls_wR_factor_all         0.0571

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3501
_refine_ls_R_factor_gt           0.0211
_refine_ls_wR_factor_gt          0.0571

_refine_ls_abs_structure_Flack   -0.038(11)
_refine_ls_abs_structure_details 'Flack (1983), 1331 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² +26.61P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ir1 Ir 0.5000 0.5000 0.10004(10) 0.0145 1.0000 Uani S T . . . .
Cl2 Cl 0.5000 0.5000 0.3850(2) 0.0367 1.0000 Uani S T . . . .
C3 C 0.53388(6) 0.43283(13) 0.1055(4) 0.0141 1.0000 Uani . . . . . .
C5 C 0.49766(7) 0.34982(17) 0.1898(5) 0.0170 1.0000 Uani . . . . . .
C6 C 0.48090(7) 0.32736(14) 0.0594(4) 0.0167 1.0000 Uani . . . . . .
C7 C 0.45377(7) 0.29421(14) 0.0896(5) 0.0219 1.0000 Uani . . . . . .
C8 C 0.44314(8) 0.28361(15) 0.2435(5) 0.0241 1.0000 Uani . . . . . .
C9 C 0.46035(8) 0.30739(14) 0.3681(5) 0.0263 1.0000 Uani . . . . . .
C10 C 0.48837(8) 0.33904(15) 0.3437(5) 0.0208 1.0000 Uani . . . . . .
C11 C 0.50787(12) 0.3564(2) 0.4873(5) 0.0317 1.0000 Uani . . . . . .
C12 C 0.41437(11) 0.24483(18) 0.2725(7) 0.0384 1.0000 Uani . . . . . .
C13 C 0.49099(10) 0.33664(17) -0.1100(5) 0.0276 1.0000 Uani . . . . . .
C14 C 0.55286(8) 0.32624(16) 0.1773(5) 0.0270 1.0000 Uani . . . . . .
C15 C 0.58360(8) 0.35687(18) 0.2151(5) 0.0294 1.0000 Uani . . . . . .
C16 C 0.59045(7) 0.40230(15) 0.0824(6) 0.0261 1.0000 Uani . . . . . .
C18 C 0.57244(9) 0.50291(13) -0.0131(5) 0.0194 1.0000 Uani . . . . . .
C19 C 0.58503(7) 0.55070(14) 0.0795(5) 0.0204 1.0000 Uani . . . . . .
C20 C 0.58544(9) 0.54673(17) 0.2573(5) 0.0254 1.0000 Uani . . . . . .
C21 C 0.59605(7) 0.60305(16) 0.0009(5) 0.0234 1.0000 Uani . . . . . .
C22 C 0.59490(8) 0.60910(16) -0.1632(6) 0.0278 1.0000 Uani . . . . . .
C23 C 0.60555(11) 0.66816(19) -0.2441(6) 0.0395 1.0000 Uani . . . . . .
C24 C 0.58236(9) 0.55982(18) -0.2509(5) 0.0283 1.0000 Uani . . . . . .
C25 C 0.57151(10) 0.50648(16) -0.1784(6) 0.0250 1.0000 Uani . . . . . .
C26 C 0.55734(11) 0.4554(2) -0.2793(5) 0.0333 1.0000 Uani . . . . . .
N4 N 0.52871(6) 0.37465(12) 0.1607(4) 0.0170 1.0000 Uani . . . . . .
N17 N 0.56396(6) 0.44520(12) 0.0640(4) 0.0177 1.0000 Uani . . . . . .
H71 H 0.4425 0.2781 0.0014 0.0263 1.0000 Uiso R . . . . .
H91 H 0.4531 0.3020 0.4731 0.0300 1.0000 Uiso R . . . . .
H111 H 0.5145 0.3184 0.5360 0.0489 1.0000 Uiso R . . . . .
H112 H 0.5259 0.3796 0.4520 0.0475 1.0000 Uiso R . . . . .
H113 H 0.4951 0.3803 0.5605 0.0477 1.0000 Uiso R . . . . .
H121 H 0.4073 0.2539 0.3792 0.0572 1.0000 Uiso R . . . . .
H122 H 0.3983 0.2583 0.2008 0.0568 1.0000 Uiso R . . . . .
H123 H 0.4176 0.2011 0.2617 0.0564 1.0000 Uiso R . . . . .
H131 H 0.4805 0.3117 -0.1810 0.0397 1.0000 Uiso R . . . . .
H132 H 0.5127 0.3269 -0.1184 0.0418 1.0000 Uiso R . . . . .
H133 H 0.4881 0.3788 -0.1452 0.0405 1.0000 Uiso R . . . . .
H141 H 0.5544 0.3028 0.0792 0.0333 1.0000 Uiso R . . . . .
H142 H 0.5463 0.2996 0.2637 0.0328 1.0000 Uiso R . . . . .
H151 H 0.5829 0.3786 0.3169 0.0332 1.0000 Uiso R . . . . .
H152 H 0.5999 0.3252 0.2191 0.0331 1.0000 Uiso R . . . . .
H161 H 0.5942 0.3780 -0.0152 0.0298 1.0000 Uiso R . . . . .
H162 H 0.6088 0.4269 0.1075 0.0284 1.0000 Uiso R . . . . .
H201 H 0.5993 0.5147 0.2920 0.0394 1.0000 Uiso R . . . . .
H202 H 0.5926 0.5871 0.2955 0.0391 1.0000 Uiso R . . . . .
H203 H 0.5651 0.5383 0.2927 0.0395 1.0000 Uiso R . . . . .
H211 H 0.6046 0.6350 0.0637 0.0288 1.0000 Uiso R . . . . .
H231 H 0.6123 0.6573 -0.3507 0.0579 1.0000 Uiso R . . . . .
H232 H 0.5885 0.6973 -0.2507 0.0589 1.0000 Uiso R . . . . .
H233 H 0.6228 0.6858 -0.1850 0.0577 1.0000 Uiso R . . . . .
H241 H 0.5816 0.5627 -0.3625 0.0343 1.0000 Uiso R . . . . .
H261 H 0.5358 0.4566 -0.2658 0.0500 1.0000 Uiso R . . . . .
H262 H 0.5651 0.4170 -0.2419 0.0492 1.0000 Uiso R . . . . .
H263 H 0.5627 0.4623 -0.3885 0.0489 1.0000 Uiso R . . . . .

_refine_ls_extinction_coef       28(3)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.917(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ir1 . C3 15_564 2.052(3) yes
Ir1 . Cl2 . 2.4000(17) yes
Ir1 . C3 . 2.052(3) yes
C3 . N4 . 1.355(4) yes
C3 . N17 . 1.364(4) yes
C5 . C6 . 1.399(5) yes
C5 . C10 . 1.376(6) yes
C5 . N4 . 1.457(4) yes
C6 . C7 . 1.390(4) yes
C6 . C13 . 1.504(5) yes
C7 . C8 . 1.393(6) yes
C7 . H71 . 0.953 no
C8 . C9 . 1.382(6) yes
C8 . C12 . 1.511(5) yes
C9 . C10 . 1.398(5) yes
C9 . H91 . 0.945 no
C10 . C11 . 1.517(6) yes
C11 . H111 . 0.958 no
C11 . H112 . 0.969 no
C11 . H113 . 0.974 no
C12 . H121 . 0.969 no
C12 . H122 . 0.961 no
C12 . H123 . 0.956 no
C13 . H131 . 0.922 no
C13 . H132 . 0.960 no
C13 . H133 . 0.963 no
C14 . C15 . 1.509(5) yes
C14 . N4 . 1.477(4) yes
C14 . H141 . 0.970 no
C14 . H142 . 0.969 no
C15 . C16 . 1.514(6) yes
C15 . H151 . 0.978 no
C15 . H152 . 0.976 no
C16 . N17 . 1.474(4) yes
C16 . H161 . 0.988 no
C16 . H162 . 0.972 no
C18 . C19 . 1.400(5) yes
C18 . C25 . 1.395(6) yes
C18 . N17 . 1.449(4) yes
C19 . C20 . 1.500(6) yes
C19 . C21 . 1.390(5) yes
C20 . H201 . 0.957 no
C20 . H202 . 0.978 no
C20 . H203 . 0.941 no
C21 . C22 . 1.389(6) yes
C21 . H211 . 0.943 no
C22 . C23 . 1.514(5) yes
C22 . C24 . 1.401(6) yes
C23 . H231 . 0.971 no
C23 . H232 . 0.965 no
C23 . H233 . 0.970 no
C24 . C25 . 1.382(6) yes
C24 . H241 . 0.943 no
C25 . C26 . 1.517(5) yes
C26 . H261 . 0.934 no
C26 . H262 . 0.946 no
C26 . H263 . 0.960 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C3 15_564 Ir1 . Cl2 . 88.72(10) yes
C3 15_564 Ir1 . C3 . 177.4(2) yes
Cl2 . Ir1 . C3 . 88.72(10) yes
Ir1 . C3 . N4 . 122.9(2) yes
Ir1 . C3 . N17 . 121.9(2) yes
N4 . C3 . N17 . 115.1(2) yes
C6 . C5 . C10 . 122.2(3) yes
C6 . C5 . N4 . 117.7(3) yes
C10 . C5 . N4 . 119.0(3) yes
C5 . C6 . C7 . 117.7(3) yes
C5 . C6 . C13 . 123.4(3) yes
C7 . C6 . C13 . 118.9(3) yes
C6 . C7 . C8 . 122.0(3) yes
C6 . C7 . H71 . 118.1 no
C8 . C7 . H71 . 120.0 no
C7 . C8 . C9 . 118.1(3) yes
C7 . C8 . C12 . 120.6(4) yes
C9 . C8 . C12 . 121.3(4) yes
C8 . C9 . C10 . 122.0(4) yes
C8 . C9 . H91 . 119.3 no
C10 . C9 . H91 . 118.7 no
C9 . C10 . C5 . 118.0(4) yes
C9 . C10 . C11 . 118.5(4) yes
C5 . C10 . C11 . 123.3(3) yes
C10 . C11 . H111 . 107.2 no
C10 . C11 . H112 . 108.9 no
H111 . C11 . H112 . 109.5 no
C10 . C11 . H113 . 108.9 no
H111 . C11 . H113 . 110.5 no
H112 . C11 . H113 . 111.7 no
C8 . C12 . H121 . 107.1 no
C8 . C12 . H122 . 108.6 no
H121 . C12 . H122 . 107.3 no
C8 . C12 . H123 . 114.1 no
H121 . C12 . H123 . 109.4 no
H122 . C12 . H123 . 110.0 no
C6 . C13 . H131 . 113.4 no
C6 . C13 . H132 . 108.8 no
H131 . C13 . H132 . 107.5 no
C6 . C13 . H133 . 112.4 no
H131 . C13 . H133 . 106.7 no
H132 . C13 . H133 . 107.9 no
C15 . C14 . N4 . 109.0(3) yes
C15 . C14 . H141 . 110.4 no
N4 . C14 . H141 . 109.4 no
C15 . C14 . H142 . 110.8 no
N4 . C14 . H142 . 106.6 no
H141 . C14 . H142 . 110.5 no
C14 . C15 . C16 . 107.3(3) yes
C14 . C15 . H151 . 111.5 no
C16 . C15 . H151 . 110.1 no
C14 . C15 . H152 . 109.1 no
C16 . C15 . H152 . 109.8 no
H151 . C15 . H152 . 109.1 no
C15 . C16 . N17 . 109.4(3) yes
C15 . C16 . H161 . 107.7 no
N17 . C16 . H161 . 111.7 no
C15 . C16 . H162 . 110.4 no
N17 . C16 . H162 . 107.8 no
H161 . C16 . H162 . 109.7 no
C19 . C18 . C25 . 121.8(3) yes
C19 . C18 . N17 . 118.5(4) yes
C25 . C18 . N17 . 119.2(3) yes
C18 . C19 . C20 . 121.3(3) yes
C18 . C19 . C21 . 117.5(4) yes
C20 . C19 . C21 . 121.2(3) yes
C19 . C20 . H201 . 110.7 no
C19 . C20 . H202 . 106.4 no
H201 . C20 . H202 . 110.1 no
C19 . C20 . H203 . 108.5 no
H201 . C20 . H203 . 110.0 no
H202 . C20 . H203 . 111.1 no
C19 . C21 . C22 . 122.5(3) yes
C19 . C21 . H211 . 117.2 no
C22 . C21 . H211 . 120.2 no
C21 . C22 . C23 . 121.1(4) yes
C21 . C22 . C24 . 117.9(3) yes
C23 . C22 . C24 . 121.0(4) yes
C22 . C23 . H231 . 107.7 no
C22 . C23 . H232 . 110.1 no
H231 . C23 . H232 . 109.2 no
C22 . C23 . H233 . 109.2 no
H231 . C23 . H233 . 110.1 no
H232 . C23 . H233 . 110.6 no
C22 . C24 . C25 . 121.8(4) yes
C22 . C24 . H241 . 119.4 no
C25 . C24 . H241 . 118.8 no
C18 . C25 . C24 . 118.5(4) yes
C18 . C25 . C26 . 122.1(4) yes
C24 . C25 . C26 . 119.3(4) yes
C25 . C26 . H261 . 108.1 no
C25 . C26 . H262 . 107.9 no
H261 . C26 . H262 . 109.3 no
C25 . C26 . H263 . 109.2 no
H261 . C26 . H263 . 110.5 no
H262 . C26 . H263 . 111.8 no
C14 . N4 . C5 . 111.6(3) yes
C14 . N4 . C3 . 124.8(3) yes
C5 . N4 . C3 . 123.2(3) yes
C16 . N17 . C18 . 113.0(3) yes
C16 . N17 . C3 . 125.6(3) yes
C18 . N17 . C3 . 121.3(3) yes
_database_code_depnum_ccdc_archive 'CCDC 1002304'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_9-prime
#==============================================================================
_audit_creation_date             13-11-05
_audit_creation_method           CRYSTALS_ver_14.23

_oxford_structure_analysis_title 031np11
_chemical_name_systematic        .
_chemical_melting_point          .

_cell_length_a                   22.1025(2)
_cell_length_b                   14.5368(1)
_cell_length_c                   23.3691(2)
_cell_angle_alpha                90
_cell_angle_beta                 111.9727(4)
_cell_angle_gamma                90
_cell_volume                     6963.08(10)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1 '
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ir -1.4442 7.9887 27.3049 1.5928 16.7296 8.8655 15.6115 0.4179 5.8338 45.0011
11.4722 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C64 H56 B1 F24 Ir1 N4 
# Dc =      1.47 Fooo =   3280.00 Mu =     20.22 M =   1540.16
# Found Formula = C72 H62 B1 F24 Ir1 N4 
# Dc =      1.57 FOOO =   3280.00 Mu =     20.27 M =   1642.29

_chemical_formula_sum            'C72 H62 B1 F24 Ir1 N4'
_chemical_formula_moiety         'C32 H12 B F24, C40 H50 Ir N4'
_chemical_compound_source        .
_chemical_formula_weight         1642.29


_cell_measurement_reflns_used    16156
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.14
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_max          0.20

_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             3280
_exptl_absorpt_coefficient_mu    2.027

# Sheldrick geometric approximatio 0.72 0.75 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_T_max  0.75
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            88057
_reflns_number_total             15868
_diffrn_reflns_av_R_equivalents  0.055
# Number of reflections without Friedels Law is 30555 
# Number of reflections with Friedels Law is 15868 
# Theoretical number of reflections is about 15989 


_diffrn_reflns_theta_min         5.158
_diffrn_reflns_theta_max         27.496
_diffrn_measured_fraction_theta_max 0.992

_diffrn_reflns_theta_full        26.946
_diffrn_measured_fraction_theta_full 0.993


_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_reflns_limit_h_min              -28
_reflns_limit_h_max              26
_reflns_limit_k_min              0
_reflns_limit_k_max              18
_reflns_limit_l_min              0
_reflns_limit_l_max              30

_oxford_diffrn_Wilson_B_factor   1.92
_oxford_diffrn_Wilson_scale      244.63

_atom_sites_solution_primary     Direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -2.84
_refine_diff_density_max         2.84


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         15868
_refine_ls_number_restraints     324
_refine_ls_number_parameters     1003
_oxford_refine_ls_R_factor_ref   0.0879
_refine_ls_wR_factor_ref         0.1074
_refine_ls_goodness_of_fit_ref   0.9852
_refine_ls_shift/su_max          0.0431384
_refine_ls_shift/su_mean         0.0007632


# The values computed from all data 
_oxford_reflns_number_all        15868
_refine_ls_R_factor_all          0.0879
_refine_ls_wR_factor_all         0.1074

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                10627
_refine_ls_R_factor_gt           0.0476
_refine_ls_wR_factor_gt          0.0777

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 3.46 3.31 0.778 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C2 C 0.7668(3) 0.3692(4) 1.0086(3) 0.0274 1.0000 Uani . . . . . .
C4 C 0.7027(3) 0.4111(4) 1.0693(3) 0.0324 1.0000 Uani . . . . . .
C5 C 0.6547(4) 0.4776(5) 1.0447(4) 0.0396 1.0000 Uani . . . . . .
C6 C 0.6616(4) 0.5504(5) 1.0012(4) 0.0552 1.0000 Uani . . . . . .
C7 C 0.6007(4) 0.4745(6) 1.0621(4) 0.0521 1.0000 Uani . . . . . .
C8 C 0.5954(4) 0.4080(6) 1.1026(4) 0.0576 1.0000 Uani . . . . . .
C9 C 0.6445(4) 0.3444(6) 1.1264(4) 0.0497 1.0000 Uani . . . . . .
C10 C 0.6993(3) 0.3447(5) 1.1115(3) 0.0362 1.0000 Uani . . . . . .
C11 C 0.7527(4) 0.2751(6) 1.1390(4) 0.0505 1.0000 Uani . . . . . .
C12 C 0.8119(4) 0.4785(6) 1.0954(4) 0.0494 1.0000 Uani . . . . . .
C13 C 0.8496(5) 0.5194(6) 1.0603(5) 0.0650 1.0000 Uani . . . . . .
C14 C 0.8758(3) 0.4441(5) 1.0313(4) 0.0412 1.0000 Uani . . . . . .
C16 C 0.8275(3) 0.3260(5) 0.9496(3) 0.0342 1.0000 Uani . . . . . .
C17 C 0.8062(3) 0.3622(5) 0.8902(3) 0.0393 1.0000 Uani . . . . . .
C18 C 0.8175(4) 0.3112(7) 0.8444(4) 0.0543 1.0000 Uani . . . . . .
C19 C 0.8486(4) 0.2262(7) 0.8585(4) 0.0559 1.0000 Uani . . . . . .
C20 C 0.8701(4) 0.1924(6) 0.9171(4) 0.0512 1.0000 Uani . . . . . .
C21 C 0.8607(3) 0.2403(5) 0.9644(3) 0.0401 1.0000 Uani . . . . . .
C22 C 0.8865(4) 0.2033(5) 1.0295(4) 0.0522 1.0000 Uani . . . . . .
C23 C 0.7755(4) 0.4566(6) 0.8773(4) 0.0548 1.0000 Uani . . . . . .
C24 C 0.6457(3) 0.1700(4) 0.9027(3) 0.0271 1.0000 Uani . . . . . .
C26 C 0.5332(3) 0.1484(5) 0.8220(4) 0.0464 1.0000 Uani . . . . . .
C27 C 0.5332(4) 0.0620(6) 0.8581(5) 0.0624 1.0000 Uani . . . . . .
C28 C 0.5984(4) 0.0145(5) 0.8767(4) 0.0505 1.0000 Uani . . . . . .
C30 C 0.7101(4) 0.0394(4) 0.9541(3) 0.0340 1.0000 Uani . . . . . .
C31 C 0.7572(4) 0.0099(5) 0.9317(4) 0.0448 1.0000 Uani . . . . . .
C32 C 0.7490(4) 0.0222(6) 0.8657(4) 0.0568 1.0000 Uani . . . . . .
C33 C 0.8134(4) -0.0310(6) 0.9736(5) 0.0619 1.0000 Uani . . . . . .
C34 C 0.8208(5) -0.0405(6) 1.0347(5) 0.0767 1.0000 Uani . . . . . .
C35 C 0.7732(6) -0.0134(6) 1.0554(4) 0.0669 1.0000 Uani . . . . . .
C36 C 0.7158(4) 0.0269(5) 1.0152(3) 0.0479 1.0000 Uani . . . . . .
C37 C 0.6630(5) 0.0576(6) 1.0365(4) 0.0614 1.0000 Uani . . . . . .
C38 C 0.5896(3) 0.3023(5) 0.8519(3) 0.0358 1.0000 Uani . . . . . .
C39 C 0.5574(4) 0.3547(5) 0.8815(4) 0.0429 1.0000 Uani . . . . . .
C40 C 0.5248(4) 0.3135(6) 0.9216(4) 0.0606 1.0000 Uani . . . . . .
C41 C 0.5533(4) 0.4493(6) 0.8708(5) 0.0586 1.0000 Uani . . . . . .
C42 C 0.5806(5) 0.4884(6) 0.8329(5) 0.0681 1.0000 Uani . . . . . .
C43 C 0.6114(4) 0.4351(6) 0.8039(4) 0.0594 1.0000 Uani . . . . . .
C44 C 0.6162(3) 0.3401(5) 0.8122(3) 0.0437 1.0000 Uani . . . . . .
C45 C 0.6458(4) 0.2807(8) 0.7767(4) 0.0612 1.0000 Uani . . . . . .
C47 C 0.5357(4) 0.4578(5) 0.6289(4) 0.0413 1.0000 Uani . . . . . .
C50 C 0.4953(3) 0.4934(5) 0.6625(3) 0.0307 1.0000 Uani . . . . . .
C51 C 0.4596(3) 0.4337(4) 0.6837(3) 0.0316 1.0000 Uani . . . . . .
C52 C 0.4237(3) 0.4711(4) 0.7159(3) 0.0274 1.0000 Uani . . . . . .
C53 C 0.4230(3) 0.5658(4) 0.7253(3) 0.0278 1.0000 Uani . . . . . .
C54 C 0.4580(3) 0.6273(4) 0.7033(3) 0.0241 1.0000 Uani . . . . . .
C55 C 0.4948(3) 0.5873(4) 0.6725(3) 0.0265 1.0000 Uani . . . . . .
C57 C 0.4812(3) 0.7978(4) 0.6687(3) 0.0263 1.0000 Uani . . . . . .
C58 C 0.4589(3) 0.7760(5) 0.6061(3) 0.0281 1.0000 Uani . . . . . .
C59 C 0.4753(3) 0.8273(5) 0.5641(3) 0.0347 1.0000 Uani . . . . . .
C60 C 0.5130(3) 0.9051(5) 0.5823(3) 0.0373 1.0000 Uani . . . . . .
C61 C 0.5329(3) 0.9319(5) 0.6434(3) 0.0339 1.0000 Uani . . . . . .
C62 C 0.5177(3) 0.8788(4) 0.6856(3) 0.0307 1.0000 Uani . . . . . .
C63 C 0.5703(4) 1.0192(6) 0.6650(4) 0.0507 1.0000 Uani . . . . . .
C67 C 0.4506(4) 0.7975(6) 0.4983(3) 0.0489 1.0000 Uani . . . . . .
C71 C 0.3900(3) 0.7798(4) 0.7136(2) 0.0245 1.0000 Uani . . . . . .
C72 C 0.3869(3) 0.8652(4) 0.7404(3) 0.0282 1.0000 Uani . . . . . .
C73 C 0.3281(3) 0.9072(4) 0.7347(3) 0.0291 1.0000 Uani . . . . . .
C74 C 0.2691(3) 0.8661(5) 0.6995(3) 0.0338 1.0000 Uani . . . . . .
C75 C 0.2708(3) 0.7834(5) 0.6709(3) 0.0330 1.0000 Uani . . . . . .
C76 C 0.3297(3) 0.7403(5) 0.6777(3) 0.0317 1.0000 Uani . . . . . .
C77 C 0.20992(19) 0.7436(3) 0.6279(2) 0.0699 1.0000 Uani D . . . . .
C81 C 0.3302(2) 0.9959(2) 0.76650(19) 0.0487 1.0000 Uani D . . . . .
C85 C 0.5166(3) 0.7495(4) 0.7876(3) 0.0248 1.0000 Uani . . . . . .
C86 C 0.5043(3) 0.7662(5) 0.8411(3) 0.0273 1.0000 Uani . . . . . .
C87 C 0.5544(3) 0.7742(5) 0.8991(3) 0.0353 1.0000 Uani . . . . . .
C88 C 0.6186(3) 0.7639(5) 0.9060(3) 0.0368 1.0000 Uani . . . . . .
C89 C 0.6329(3) 0.7448(4) 0.8543(3) 0.0363 1.0000 Uani . . . . . .
C90 C 0.5826(3) 0.7387(5) 0.7967(3) 0.0300 1.0000 Uani . . . . . .
C91 C 0.70050(17) 0.7312(4) 0.8592(3) 0.0653 1.0000 Uani D . . . . .
C95 C 0.5377(4) 0.7947(6) 0.9541(3) 0.0488 1.0000 Uani . . . . . .
C99 C 0.3849(3) 0.4087(5) 0.7399(4) 0.0381 1.0000 Uani . . . . . .
F46 F 0.5419(2) 0.3656(3) 0.6307(2) 0.0539 1.0000 Uani . . . . . .
F48 F 0.5120(3) 0.4806(4) 0.5691(2) 0.0641 1.0000 Uani . . . . . .
F49 F 0.5972(2) 0.4914(3) 0.6510(2) 0.0576 1.0000 Uani . . . . . .
F64 F 0.5307(3) 1.0878(4) 0.6690(3) 0.0697 1.0000 Uani . . . . . .
F65 F 0.5977(3) 1.0505(3) 0.6277(3) 0.0738 1.0000 Uani . . . . . .
F66 F 0.6174(3) 1.0121(4) 0.7205(3) 0.0965 1.0000 Uani . . . . . .
F68 F 0.4848(2) 0.8321(4) 0.4669(2) 0.0714 1.0000 Uani . . . . . .
F69 F 0.3887(2) 0.8246(4) 0.4677(2) 0.0685 1.0000 Uani . . . . . .
F70 F 0.4517(3) 0.7067(4) 0.4920(2) 0.0848 1.0000 Uani . . . . . .
F96 F 0.5424(3) 0.7197(5) 0.9884(2) 0.0893 1.0000 Uani . . . . . .
F97 F 0.5792(3) 0.8517(5) 0.9931(3) 0.0981 1.0000 Uani . . . . . .
F98 F 0.4783(3) 0.8241(5) 0.9413(2) 0.0999 1.0000 Uani . . . . . .
F100 F 0.3212(2) 0.4134(4) 0.7061(2) 0.0630 1.0000 Uani . . . . . .
F101 F 0.4012(3) 0.3208(3) 0.7411(3) 0.0757 1.0000 Uani . . . . . .
F102 F 0.3905(3) 0.4306(4) 0.7974(2) 0.0651 1.0000 Uani . . . . . .
F400 F 0.7461(3) 0.7453(8) 0.9154(3) 0.0825 0.600(11) Uani D . P 1 1 .
F401 F 0.7174(4) 0.7893(6) 0.8231(4) 0.0693 0.600(11) Uani D . P 1 1 .
F402 F 0.7131(4) 0.6487(5) 0.8418(5) 0.0802 0.600(11) Uani D . P 1 1 .
F403 F 0.7360(5) 0.6841(10) 0.9108(5) 0.0724 0.400(11) Uani D . P 1 2 .
F404 F 0.7357(5) 0.8058(7) 0.8619(8) 0.0823 0.400(11) Uani D . P 1 2 .
F405 F 0.7056(6) 0.6830(10) 0.8118(5) 0.0731 0.400(11) Uani D . P 1 2 .
F500 F 0.1640(7) 0.7963(11) 0.5863(8) 0.0731 0.228(7) Uani D . P 2 1 .
F501 F 0.1865(8) 0.7161(16) 0.6705(6) 0.0794 0.228(7) Uani D . P 2 1 .
F502 F 0.2022(9) 0.6732(11) 0.5874(8) 0.0838 0.228(7) Uani D . P 2 1 .
F503 F 0.2088(3) 0.7314(5) 0.5688(3) 0.0837 0.772(7) Uani D . P 2 2 .
F504 F 0.1558(3) 0.7832(5) 0.6235(3) 0.0822 0.772(7) Uani D . P 2 2 .
F505 F 0.2042(3) 0.6520(4) 0.6369(3) 0.0663 0.772(7) Uani D . P 2 2 .
F600 F 0.3629(7) 1.0590(7) 0.7466(7) 0.0512 0.55(3) Uani D . P 3 1 .
F601 F 0.3637(9) 0.9884(6) 0.8280(3) 0.0541 0.55(3) Uani D . P 3 1 .
F602 F 0.2730(4) 1.0355(9) 0.7601(8) 0.0591 0.55(3) Uani D . P 3 1 .
F603 F 0.3762(6) 1.0565(9) 0.7669(9) 0.0484 0.45(3) Uani D . P 3 2 .
F604 F 0.3371(11) 0.9859(8) 0.8255(4) 0.0617 0.45(3) Uani D . P 3 2 .
F605 F 0.2724(4) 1.0394(9) 0.7385(8) 0.0472 0.45(3) Uani D . P 3 2 .
Ir1 Ir 0.706491(12) 0.271803(16) 0.953055(12) 0.0241 1.0000 Uani . . . . . .
N3 N 0.7606(3) 0.4167(4) 1.0547(3) 0.0324 1.0000 Uani . . . . . .
N15 N 0.8219(3) 0.3805(4) 0.9980(3) 0.0321 1.0000 Uani . . . . . .
N25 N 0.5908(2) 0.2033(4) 0.8592(2) 0.0308 1.0000 Uani . . . . . .
N29 N 0.6506(3) 0.0793(4) 0.9106(3) 0.0324 1.0000 Uani . . . . . .
B56 B 0.4603(3) 0.7380(5) 0.7180(3) 0.0244 1.0000 Uani . . . . . .
H61 H 0.6228 0.5889 0.9859 0.0849 1.0000 Uiso . . . . . .
H63 H 0.6987 0.5900 1.0222 0.0849 1.0000 Uiso . . . . . .
H62 H 0.6677 0.5215 0.9661 0.0851 1.0000 Uiso . . . . . .
H71 H 0.5673 0.5194 1.0455 0.0652 1.0000 Uiso . . . . . .
H81 H 0.5580 0.4061 1.1137 0.0712 1.0000 Uiso . . . . . .
H91 H 0.6406 0.2995 1.1546 0.0612 1.0000 Uiso . . . . . .
H111 H 0.7411 0.2319 1.1652 0.0792 1.0000 Uiso . . . . . .
H112 H 0.7933 0.3060 1.1638 0.0792 1.0000 Uiso . . . . . .
H113 H 0.7602 0.2406 1.1065 0.0792 1.0000 Uiso . . . . . .
H122 H 0.8421 0.4420 1.1305 0.0644 1.0000 Uiso . . . . . .
H121 H 0.7923 0.5270 1.1124 0.0643 1.0000 Uiso . . . . . .
H132 H 0.8854 0.5588 1.0869 0.0791 1.0000 Uiso . . . . . .
H131 H 0.8198 0.5604 1.0261 0.0794 1.0000 Uiso . . . . . .
H141 H 0.9107 0.4102 1.0642 0.0543 1.0000 Uiso . . . . . .
H142 H 0.8945 0.4692 1.0027 0.0543 1.0000 Uiso . . . . . .
H181 H 0.8036 0.3353 0.8033 0.0682 1.0000 Uiso . . . . . .
H191 H 0.8546 0.1902 0.8267 0.0692 1.0000 Uiso . . . . . .
H201 H 0.8925 0.1345 0.9257 0.0641 1.0000 Uiso . . . . . .
H221 H 0.8854 0.1371 1.0293 0.0823 1.0000 Uiso . . . . . .
H223 H 0.9311 0.2233 1.0516 0.0823 1.0000 Uiso . . . . . .
H222 H 0.8597 0.2254 1.0515 0.0823 1.0000 Uiso . . . . . .
H231 H 0.7610 0.4701 0.8334 0.0861 1.0000 Uiso . . . . . .
H232 H 0.8070 0.5037 0.9005 0.0862 1.0000 Uiso . . . . . .
H233 H 0.7383 0.4583 0.8903 0.0860 1.0000 Uiso . . . . . .
H262 H 0.4930 0.1833 0.8134 0.0600 1.0000 Uiso . . . . . .
H261 H 0.5364 0.1317 0.7824 0.0601 1.0000 Uiso . . . . . .
H272 H 0.5250 0.0798 0.8961 0.0803 1.0000 Uiso . . . . . .
H271 H 0.4980 0.0204 0.8341 0.0801 1.0000 Uiso . . . . . .
H281 H 0.6001 -0.0391 0.9029 0.0642 1.0000 Uiso . . . . . .
H282 H 0.6052 -0.0068 0.8393 0.0643 1.0000 Uiso . . . . . .
H321 H 0.7878 -0.0004 0.8593 0.0872 1.0000 Uiso . . . . . .
H323 H 0.7433 0.0870 0.8544 0.0873 1.0000 Uiso . . . . . .
H322 H 0.7115 -0.0118 0.8388 0.0872 1.0000 Uiso . . . . . .
H331 H 0.8464 -0.0527 0.9608 0.0802 1.0000 Uiso . . . . . .
H341 H 0.8599 -0.0673 1.0627 0.0891 1.0000 Uiso . . . . . .
H351 H 0.7798 -0.0214 1.0974 0.0843 1.0000 Uiso . . . . . .
H371 H 0.6771 0.0517 1.0808 0.0932 1.0000 Uiso . . . . . .
H372 H 0.6527 0.1219 1.0254 0.0932 1.0000 Uiso . . . . . .
H373 H 0.6238 0.0220 1.0170 0.0932 1.0000 Uiso . . . . . .
H402 H 0.5333 0.3504 0.9582 0.0941 1.0000 Uiso . . . . . .
H401 H 0.5415 0.2515 0.9346 0.0942 1.0000 Uiso . . . . . .
H403 H 0.4780 0.3100 0.8994 0.0942 1.0000 Uiso . . . . . .
H411 H 0.5312 0.4872 0.8902 0.0733 1.0000 Uiso . . . . . .
H421 H 0.5785 0.5537 0.8271 0.0812 1.0000 Uiso . . . . . .
H431 H 0.6301 0.4638 0.7779 0.0763 1.0000 Uiso . . . . . .
H451 H 0.6654 0.3180 0.7541 0.0951 1.0000 Uiso . . . . . .
H453 H 0.6797 0.2406 0.8053 0.0952 1.0000 Uiso . . . . . .
H452 H 0.6123 0.2410 0.7477 0.0952 1.0000 Uiso . . . . . .
H511 H 0.4594 0.3696 0.6766 0.0411 1.0000 Uiso . . . . . .
H531 H 0.3975 0.5900 0.7473 0.0364 1.0000 Uiso . . . . . .
H551 H 0.5211 0.6258 0.6585 0.0342 1.0000 Uiso . . . . . .
H581 H 0.4319 0.7232 0.5917 0.0372 1.0000 Uiso . . . . . .
H601 H 0.5251 0.9393 0.5542 0.0473 1.0000 Uiso . . . . . .
H621 H 0.5330 0.8979 0.7275 0.0390 1.0000 Uiso . . . . . .
H721 H 0.4273 0.8959 0.7641 0.0344 1.0000 Uiso . . . . . .
H741 H 0.2285 0.8942 0.6951 0.0432 1.0000 Uiso . . . . . .
H761 H 0.3287 0.6835 0.6573 0.0420 1.0000 Uiso . . . . . .
H861 H 0.4601 0.7727 0.8379 0.0351 1.0000 Uiso . . . . . .
H881 H 0.6522 0.7697 0.9455 0.0463 1.0000 Uiso . . . . . .
H901 H 0.5934 0.7260 0.7618 0.0403 1.0000 Uiso . . . . . .
H24 H 0.6517 0.2897 0.9858 0.0765 1.0000 Uiso . . . . . .
H26 H 0.7541 0.1946 1.0070 0.0788 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.067276(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C2 . Ir1 . 2.042(6) yes
C2 . N3 . 1.330(8) yes
C2 . N15 . 1.342(8) yes
C4 . C5 . 1.391(9) yes
C4 . C10 . 1.402(9) yes
C4 . N3 . 1.443(8) yes
C5 . C6 . 1.516(11) yes
C5 . C7 . 1.398(10) yes
C6 . H61 . 0.973 no
C6 . H63 . 0.971 no
C6 . H62 . 0.974 no
C7 . C8 . 1.388(12) yes
C7 . H71 . 0.954 no
C8 . C9 . 1.375(12) yes
C8 . H81 . 0.956 no
C9 . C10 . 1.379(10) yes
C9 . H91 . 0.954 no
C10 . C11 . 1.505(10) yes
C11 . H111 . 0.975 no
C11 . H112 . 0.976 no
C11 . H113 . 0.975 no
C12 . C13 . 1.494(11) yes
C12 . N3 . 1.480(8) yes
C12 . H122 . 0.995 no
C12 . H121 . 0.986 no
C13 . C14 . 1.512(11) yes
C13 . H132 . 0.987 no
C13 . H131 . 1.017 no
C14 . N15 . 1.479(8) yes
C14 . H141 . 0.993 no
C14 . H142 . 0.977 no
C16 . C17 . 1.392(10) yes
C16 . C21 . 1.421(10) yes
C16 . N15 . 1.423(8) yes
C17 . C18 . 1.398(10) yes
C17 . C23 . 1.510(11) yes
C18 . C19 . 1.393(12) yes
C18 . H181 . 0.958 no
C19 . C20 . 1.363(12) yes
C19 . H191 . 0.958 no
C20 . C21 . 1.386(10) yes
C20 . H201 . 0.958 no
C21 . C22 . 1.510(10) yes
C22 . H221 . 0.963 no
C22 . H223 . 0.972 no
C22 . H222 . 0.972 no
C23 . H231 . 0.973 no
C23 . H232 . 0.982 no
C23 . H233 . 0.978 no
C24 . Ir1 . 2.049(6) yes
C24 . N25 . 1.349(7) yes
C24 . N29 . 1.330(8) yes
C26 . C27 . 1.514(11) yes
C26 . N25 . 1.478(8) yes
C26 . H262 . 0.976 no
C26 . H261 . 0.984 no
C27 . C28 . 1.506(11) yes
C27 . H272 . 1.006 no
C27 . H271 . 0.978 no
C28 . N29 . 1.471(8) yes
C28 . H281 . 0.984 no
C28 . H282 . 0.991 no
C30 . C31 . 1.397(11) yes
C30 . C36 . 1.398(10) yes
C30 . N29 . 1.449(8) yes
C31 . C32 . 1.495(12) yes
C31 . C33 . 1.396(11) yes
C32 . H321 . 0.979 no
C32 . H323 . 0.974 no
C32 . H322 . 0.967 no
C33 . C34 . 1.381(15) yes
C33 . H331 . 0.939 no
C34 . C35 . 1.372(15) yes
C34 . H341 . 0.950 no
C35 . C36 . 1.393(12) yes
C35 . H351 . 0.943 no
C36 . C37 . 1.497(13) yes
C37 . H371 . 0.967 no
C37 . H372 . 0.973 no
C37 . H373 . 0.965 no
C38 . C39 . 1.392(10) yes
C38 . C44 . 1.385(10) yes
C38 . N25 . 1.449(9) yes
C39 . C40 . 1.503(11) yes
C39 . C41 . 1.395(11) yes
C40 . H402 . 0.966 no
C40 . H401 . 0.977 no
C40 . H403 . 0.970 no
C41 . C42 . 1.369(14) yes
C41 . H411 . 0.954 no
C42 . C43 . 1.365(14) yes
C42 . H421 . 0.958 no
C43 . C44 . 1.393(11) yes
C43 . H431 . 0.949 no
C44 . C45 . 1.505(12) yes
C45 . H451 . 0.967 no
C45 . H453 . 0.986 no
C45 . H452 . 0.981 no
C47 . C50 . 1.485(9) yes
C47 . F46 . 1.347(8) yes
C47 . F48 . 1.337(9) yes
C47 . F49 . 1.353(9) yes
C50 . C51 . 1.385(9) yes
C50 . C55 . 1.385(9) yes
C51 . C52 . 1.390(9) yes
C51 . H511 . 0.947 no
C52 . C53 . 1.395(8) yes
C52 . C99 . 1.496(9) yes
C53 . C54 . 1.400(8) yes
C53 . H531 . 0.959 no
C54 . C55 . 1.400(8) yes
C54 . B56 . 1.643(9) yes
C55 . H551 . 0.949 no
C57 . C58 . 1.394(8) yes
C57 . C62 . 1.398(8) yes
C57 . B56 . 1.642(9) yes
C58 . C59 . 1.385(8) yes
C58 . H581 . 0.953 no
C59 . C60 . 1.375(10) yes
C59 . C67 . 1.490(10) yes
C60 . C61 . 1.384(10) yes
C60 . H601 . 0.940 no
C61 . C62 . 1.389(9) yes
C61 . C63 . 1.495(10) yes
C62 . H621 . 0.951 no
C63 . F64 . 1.352(10) yes
C63 . F65 . 1.317(9) yes
C63 . F66 . 1.329(9) yes
C67 . F68 . 1.335(8) yes
C67 . F69 . 1.343(9) yes
C67 . F70 . 1.328(10) yes
C71 . C72 . 1.404(8) yes
C71 . C76 . 1.405(8) yes
C71 . B56 . 1.634(8) yes
C72 . C73 . 1.395(8) yes
C72 . H721 . 0.966 no
C73 . C74 . 1.390(9) yes
C73 . C81 . 1.480(7) yes
C74 . C75 . 1.383(9) yes
C74 . H741 . 0.956 no
C75 . C76 . 1.401(8) yes
C75 . C77 . 1.464(7) yes
C76 . H761 . 0.949 no
C77 . F500 . 1.350(7) yes
C77 . F501 . 1.344(7) yes
C77 . F502 . 1.360(7) yes
C77 . F503 . 1.384(6) yes
C77 . F504 . 1.296(5) yes
C77 . F505 . 1.362(5) yes
C81 . F600 . 1.353(6) yes
C81 . F601 . 1.352(6) yes
C81 . F602 . 1.346(6) yes
C81 . F603 . 1.343(6) yes
C81 . F604 . 1.337(6) yes
C81 . F605 . 1.355(6) yes
C85 . C86 . 1.395(8) yes
C85 . C90 . 1.403(8) yes
C85 . B56 . 1.646(8) yes
C86 . C87 . 1.398(8) yes
C86 . H861 . 0.956 no
C87 . C88 . 1.377(9) yes
C87 . C95 . 1.493(9) yes
C88 . C89 . 1.384(9) yes
C88 . H881 . 0.947 no
C89 . C90 . 1.391(8) yes
C89 . C91 . 1.470(7) yes
C90 . H901 . 0.949 no
C91 . F400 . 1.339(6) yes
C91 . F401 . 1.342(6) yes
C91 . F402 . 1.328(6) yes
C91 . F403 . 1.354(6) yes
C91 . F404 . 1.322(6) yes
C91 . F405 . 1.349(7) yes
C95 . F96 . 1.334(9) yes
C95 . F97 . 1.316(9) yes
C95 . F98 . 1.304(9) yes
C99 . F100 . 1.332(8) yes
C99 . F101 . 1.325(8) yes
C99 . F102 . 1.341(9) yes
Ir1 . H24 . 1.677 no
Ir1 . H26 . 1.722 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Ir1 . C2 . N3 . 129.4(4) yes
Ir1 . C2 . N15 . 112.9(4) yes
N3 . C2 . N15 . 117.5(5) yes
C5 . C4 . C10 . 122.3(6) yes
C5 . C4 . N3 . 118.1(6) yes
C10 . C4 . N3 . 119.4(6) yes
C4 . C5 . C6 . 120.6(7) yes
C4 . C5 . C7 . 117.4(7) yes
C6 . C5 . C7 . 122.0(7) yes
C5 . C6 . H61 . 110.6 no
C5 . C6 . H63 . 110.6 no
H61 . C6 . H63 . 107.9 no
C5 . C6 . H62 . 110.0 no
H61 . C6 . H62 . 108.6 no
H63 . C6 . H62 . 109.0 no
C5 . C7 . C8 . 121.3(7) yes
C5 . C7 . H71 . 118.4 no
C8 . C7 . H71 . 120.4 no
C7 . C8 . C9 . 119.3(7) yes
C7 . C8 . H81 . 120.4 no
C9 . C8 . H81 . 120.2 no
C8 . C9 . C10 . 122.0(7) yes
C8 . C9 . H91 . 118.5 no
C10 . C9 . H91 . 119.5 no
C4 . C10 . C9 . 117.7(7) yes
C4 . C10 . C11 . 121.6(6) yes
C9 . C10 . C11 . 120.8(7) yes
C10 . C11 . H111 . 110.7 no
C10 . C11 . H112 . 110.1 no
H111 . C11 . H112 . 108.9 no
C10 . C11 . H113 . 110.3 no
H111 . C11 . H113 . 108.6 no
H112 . C11 . H113 . 108.2 no
C13 . C12 . N3 . 109.9(6) yes
C13 . C12 . H122 . 108.9 no
N3 . C12 . H122 . 108.8 no
C13 . C12 . H121 . 110.9 no
N3 . C12 . H121 . 110.2 no
H122 . C12 . H121 . 108.0 no
C12 . C13 . C14 . 110.2(7) yes
C12 . C13 . H132 . 111.5 no
C14 . C13 . H132 . 110.6 no
C12 . C13 . H131 . 109.5 no
C14 . C13 . H131 . 108.4 no
H132 . C13 . H131 . 106.6 no
C13 . C14 . N15 . 108.6(6) yes
C13 . C14 . H141 . 109.2 no
N15 . C14 . H141 . 109.6 no
C13 . C14 . H142 . 111.6 no
N15 . C14 . H142 . 109.7 no
H141 . C14 . H142 . 108.1 no
C17 . C16 . C21 . 121.7(6) yes
C17 . C16 . N15 . 118.9(6) yes
C21 . C16 . N15 . 119.0(6) yes
C16 . C17 . C18 . 118.2(7) yes
C16 . C17 . C23 . 120.2(7) yes
C18 . C17 . C23 . 121.6(7) yes
C17 . C18 . C19 . 120.2(8) yes
C17 . C18 . H181 . 119.5 no
C19 . C18 . H181 . 120.3 no
C18 . C19 . C20 . 120.8(7) yes
C18 . C19 . H191 . 120.1 no
C20 . C19 . H191 . 119.1 no
C19 . C20 . C21 . 121.4(8) yes
C19 . C20 . H201 . 119.1 no
C21 . C20 . H201 . 119.5 no
C16 . C21 . C20 . 117.7(7) yes
C16 . C21 . C22 . 121.5(6) yes
C20 . C21 . C22 . 120.8(7) yes
C21 . C22 . H221 . 110.6 no
C21 . C22 . H223 . 110.8 no
H221 . C22 . H223 . 108.6 no
C21 . C22 . H222 . 109.9 no
H221 . C22 . H222 . 108.3 no
H223 . C22 . H222 . 108.6 no
C17 . C23 . H231 . 109.9 no
C17 . C23 . H232 . 110.5 no
H231 . C23 . H232 . 109.1 no
C17 . C23 . H233 . 109.1 no
H231 . C23 . H233 . 109.9 no
H232 . C23 . H233 . 108.3 no
Ir1 . C24 . N25 . 112.6(4) yes
Ir1 . C24 . N29 . 129.4(4) yes
N25 . C24 . N29 . 117.6(5) yes
C27 . C26 . N25 . 107.4(6) yes
C27 . C26 . H262 . 110.9 no
N25 . C26 . H262 . 110.9 no
C27 . C26 . H261 . 109.5 no
N25 . C26 . H261 . 109.8 no
H262 . C26 . H261 . 108.3 no
C26 . C27 . C28 . 110.0(7) yes
C26 . C27 . H272 . 108.4 no
C28 . C27 . H272 . 109.4 no
C26 . C27 . H271 . 111.1 no
C28 . C27 . H271 . 110.6 no
H272 . C27 . H271 . 107.2 no
C27 . C28 . N29 . 109.6(6) yes
C27 . C28 . H281 . 110.6 no
N29 . C28 . H281 . 109.4 no
C27 . C28 . H282 . 109.5 no
N29 . C28 . H282 . 109.1 no
H281 . C28 . H282 . 108.6 no
C31 . C30 . C36 . 123.3(7) yes
C31 . C30 . N29 . 117.8(7) yes
C36 . C30 . N29 . 118.8(7) yes
C30 . C31 . C32 . 122.2(7) yes
C30 . C31 . C33 . 117.4(8) yes
C32 . C31 . C33 . 120.5(8) yes
C31 . C32 . H321 . 110.0 no
C31 . C32 . H323 . 110.3 no
H321 . C32 . H323 . 108.4 no
C31 . C32 . H322 . 110.6 no
H321 . C32 . H322 . 108.5 no
H323 . C32 . H322 . 108.9 no
C31 . C33 . C34 . 119.9(9) yes
C31 . C33 . H331 . 120.8 no
C34 . C33 . H331 . 119.3 no
C33 . C34 . C35 . 121.7(8) yes
C33 . C34 . H341 . 118.6 no
C35 . C34 . H341 . 119.7 no
C34 . C35 . C36 . 120.6(9) yes
C34 . C35 . H351 . 119.3 no
C36 . C35 . H351 . 120.1 no
C30 . C36 . C35 . 117.0(9) yes
C30 . C36 . C37 . 121.1(7) yes
C35 . C36 . C37 . 121.9(8) yes
C36 . C37 . H371 . 110.4 no
C36 . C37 . H372 . 109.4 no
H371 . C37 . H372 . 108.6 no
C36 . C37 . H373 . 111.0 no
H371 . C37 . H373 . 109.3 no
H372 . C37 . H373 . 108.1 no
C39 . C38 . C44 . 122.8(7) yes
C39 . C38 . N25 . 118.3(6) yes
C44 . C38 . N25 . 118.7(7) yes
C38 . C39 . C40 . 123.1(7) yes
C38 . C39 . C41 . 117.4(8) yes
C40 . C39 . C41 . 119.4(8) yes
C39 . C40 . H402 . 110.5 no
C39 . C40 . H401 . 110.3 no
H402 . C40 . H401 . 108.2 no
C39 . C40 . H403 . 110.5 no
H402 . C40 . H403 . 108.5 no
H401 . C40 . H403 . 108.8 no
C39 . C41 . C42 . 120.7(9) yes
C39 . C41 . H411 . 119.6 no
C42 . C41 . H411 . 119.7 no
C41 . C42 . C43 . 120.5(8) yes
C41 . C42 . H421 . 119.5 no
C43 . C42 . H421 . 120.0 no
C42 . C43 . C44 . 121.3(8) yes
C42 . C43 . H431 . 119.0 no
C44 . C43 . H431 . 119.7 no
C43 . C44 . C38 . 117.2(8) yes
C43 . C44 . C45 . 121.3(8) yes
C38 . C44 . C45 . 121.5(7) yes
C44 . C45 . H451 . 110.8 no
C44 . C45 . H453 . 110.0 no
H451 . C45 . H453 . 108.7 no
C44 . C45 . H452 . 110.3 no
H451 . C45 . H452 . 109.1 no
H453 . C45 . H452 . 107.8 no
C50 . C47 . F46 . 113.9(6) yes
C50 . C47 . F48 . 112.9(6) yes
F46 . C47 . F48 . 106.0(6) yes
C50 . C47 . F49 . 112.9(6) yes
F46 . C47 . F49 . 105.7(6) yes
F48 . C47 . F49 . 104.7(6) yes
C47 . C50 . C51 . 120.5(6) yes
C47 . C50 . C55 . 118.5(6) yes
C51 . C50 . C55 . 121.0(6) yes
C50 . C51 . C52 . 117.7(6) yes
C50 . C51 . H511 . 121.3 no
C52 . C51 . H511 . 121.0 no
C51 . C52 . C53 . 121.0(6) yes
C51 . C52 . C99 . 119.2(6) yes
C53 . C52 . C99 . 119.8(6) yes
C52 . C53 . C54 . 122.1(6) yes
C52 . C53 . H531 . 119.4 no
C54 . C53 . H531 . 118.5 no
C53 . C54 . C55 . 115.6(6) yes
C53 . C54 . B56 . 121.8(5) yes
C55 . C54 . B56 . 122.4(5) yes
C54 . C55 . C50 . 122.6(6) yes
C54 . C55 . H551 . 118.8 no
C50 . C55 . H551 . 118.6 no
C58 . C57 . C62 . 115.4(6) yes
C58 . C57 . B56 . 122.3(5) yes
C62 . C57 . B56 . 122.1(5) yes
C57 . C58 . C59 . 122.5(6) yes
C57 . C58 . H581 . 118.9 no
C59 . C58 . H581 . 118.5 no
C58 . C59 . C60 . 120.8(6) yes
C58 . C59 . C67 . 118.9(7) yes
C60 . C59 . C67 . 120.3(6) yes
C59 . C60 . C61 . 118.3(6) yes
C59 . C60 . H601 . 121.1 no
C61 . C60 . H601 . 120.6 no
C60 . C61 . C62 . 120.5(6) yes
C60 . C61 . C63 . 120.7(6) yes
C62 . C61 . C63 . 118.9(7) yes
C57 . C62 . C61 . 122.4(6) yes
C57 . C62 . H621 . 118.9 no
C61 . C62 . H621 . 118.7 no
C61 . C63 . F64 . 111.1(7) yes
C61 . C63 . F65 . 113.8(7) yes
F64 . C63 . F65 . 105.2(6) yes
C61 . C63 . F66 . 113.3(6) yes
F64 . C63 . F66 . 106.3(8) yes
F65 . C63 . F66 . 106.7(7) yes
C59 . C67 . F68 . 113.2(7) yes
C59 . C67 . F69 . 111.7(6) yes
F68 . C67 . F69 . 105.7(6) yes
C59 . C67 . F70 . 112.9(6) yes
F68 . C67 . F70 . 106.0(7) yes
F69 . C67 . F70 . 106.9(8) yes
C72 . C71 . C76 . 115.7(5) yes
C72 . C71 . B56 . 120.3(5) yes
C76 . C71 . B56 . 123.5(5) yes
C71 . C72 . C73 . 122.9(6) yes
C71 . C72 . H721 . 118.3 no
C73 . C72 . H721 . 118.8 no
C72 . C73 . C74 . 120.2(6) yes
C72 . C73 . C81 . 118.7(6) yes
C74 . C73 . C81 . 121.1(5) yes
C73 . C74 . C75 . 118.0(6) yes
C73 . C74 . H741 . 121.1 no
C75 . C74 . H741 . 120.9 no
C74 . C75 . C76 . 121.8(6) yes
C74 . C75 . C77 . 119.4(6) yes
C76 . C75 . C77 . 118.5(6) yes
C71 . C76 . C75 . 121.3(6) yes
C71 . C76 . H761 . 119.6 no
C75 . C76 . H761 . 119.1 no
C75 . C77 . F500 . 121.4(9) yes
C75 . C77 . F501 . 96.8(8) yes
F500 . C77 . F501 . 107.92(7) yes
C75 . C77 . F502 . 128.3(9) yes
F500 . C77 . F502 . 93.50(7) yes
F501 . C77 . F502 . 107.93(7) yes
C75 . C77 . F503 . 113.9(5) yes
C75 . C77 . F504 . 117.5(5) yes
F503 . C77 . F504 . 107.86(7) yes
C75 . C77 . F505 . 113.3(5) yes
F503 . C77 . F505 . 93.52(7) yes
F504 . C77 . F505 . 108.04(7) yes
C73 . C81 . F600 . 109.8(7) yes
C73 . C81 . F601 . 111.5(5) yes
F600 . C81 . F601 . 105.65(7) yes
C73 . C81 . F602 . 117.7(7) yes
F600 . C81 . F602 . 105.77(7) yes
F601 . C81 . F602 . 105.69(7) yes
C73 . C81 . F603 . 117.1(8) yes
C73 . C81 . F604 . 113.2(6) yes
F603 . C81 . F604 . 105.71(7) yes
C73 . C81 . F605 . 108.5(7) yes
F603 . C81 . F605 . 105.77(7) yes
F604 . C81 . F605 . 105.69(7) yes
C86 . C85 . C90 . 115.1(5) yes
C86 . C85 . B56 . 125.0(5) yes
C90 . C85 . B56 . 119.9(5) yes
C85 . C86 . C87 . 122.3(6) yes
C85 . C86 . H861 . 118.9 no
C87 . C86 . H861 . 118.8 no
C86 . C87 . C88 . 120.7(6) yes
C86 . C87 . C95 . 119.4(6) yes
C88 . C87 . C95 . 119.9(6) yes
C87 . C88 . C89 . 118.8(6) yes
C87 . C88 . H881 . 120.1 no
C89 . C88 . H881 . 121.1 no
C88 . C89 . C90 . 119.9(6) yes
C88 . C89 . C91 . 121.1(6) yes
C90 . C89 . C91 . 119.1(6) yes
C85 . C90 . C89 . 123.2(6) yes
C85 . C90 . H901 . 118.1 no
C89 . C90 . H901 . 118.7 no
C89 . C91 . F400 . 115.1(5) yes
C89 . C91 . F401 . 112.4(5) yes
F400 . C91 . F401 . 103.70(7) yes
C89 . C91 . F402 . 114.9(6) yes
F400 . C91 . F402 . 105.75(7) yes
F401 . C91 . F402 . 103.74(7) yes
C89 . C91 . F403 . 111.7(6) yes
C89 . C91 . F404 . 117.2(7) yes
F403 . C91 . F404 . 103.76(7) yes
C89 . C91 . F405 . 113.7(6) yes
F403 . C91 . F405 . 105.66(7) yes
F404 . C91 . F405 . 103.75(7) yes
C87 . C95 . F96 . 111.4(7) yes
C87 . C95 . F97 . 112.8(7) yes
F96 . C95 . F97 . 102.8(6) yes
C87 . C95 . F98 . 114.8(6) yes
F96 . C95 . F98 . 104.5(7) yes
F97 . C95 . F98 . 109.5(8) yes
C52 . C99 . F100 . 112.0(6) yes
C52 . C99 . F101 . 113.7(6) yes
F100 . C99 . F101 . 106.3(6) yes
C52 . C99 . F102 . 112.4(6) yes
F100 . C99 . F102 . 105.2(6) yes
F101 . C99 . F102 . 106.6(6) yes
C24 . Ir1 . C2 . 176.1(3) yes
C24 . Ir1 . H24 . 86.8 no
C2 . Ir1 . H24 . 90.8 no
C24 . Ir1 . H26 . 92.3 no
C2 . Ir1 . H26 . 84.9 no
H24 . Ir1 . H26 . 96.6 no
C12 . N3 . C4 . 114.7(5) yes
C12 . N3 . C2 . 123.3(5) yes
C4 . N3 . C2 . 122.0(5) yes
C14 . N15 . C16 . 118.2(5) yes
C14 . N15 . C2 . 126.0(5) yes
C16 . N15 . C2 . 115.7(5) yes
C26 . N25 . C38 . 119.5(5) yes
C26 . N25 . C24 . 125.7(5) yes
C38 . N25 . C24 . 114.7(5) yes
C28 . N29 . C30 . 116.4(5) yes
C28 . N29 . C24 . 123.6(6) yes
C30 . N29 . C24 . 119.9(5) yes
C85 . B56 . C54 . 105.0(5) yes
C85 . B56 . C57 . 109.4(5) yes
C54 . B56 . C57 . 111.5(5) yes
C85 . B56 . C71 . 112.0(5) yes
C54 . B56 . C71 . 113.4(5) yes
C57 . B56 . C71 . 105.7(5) yes
_database_code_depnum_ccdc_archive 'CCDC 1002305'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_10
#==============================================================================
_audit_creation_date             13-11-01
_audit_creation_method           CRYSTALS_ver_14.23

_oxford_structure_analysis_title 033np11
_chemical_name_systematic        .
_chemical_melting_point          .


_cell_length_a                   12.5841(2)
_cell_length_b                   17.9389(3)
_cell_length_c                   18.2196(3)
_cell_angle_alpha                86.8231(6)
_cell_angle_beta                 69.9280(7)
_cell_angle_gamma                87.6703(6)
_cell_volume                     3856.21(11)

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ir -1.4442 7.9887 27.3049 1.5928 16.7296 8.8655 15.6115 0.4179 5.8338 45.0011
11.4722 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C138 H152 B4 F48 Ir2 N10 
# Dc =      2.83 Fooo =   1756.00 Mu =     36.60 M =   3290.38
# Found Formula = C77 H78 B2 F24 Ir1 N5 
# Dc =      1.50 FOOO =   1756.00 Mu =     18.35 M =   1743.29

_chemical_formula_sum            'C77 H78 B2 F24 Ir N5'
_chemical_formula_moiety         'C32 H12 B F24, C45 H66 B Ir N5'
_chemical_compound_source        .
_chemical_formula_weight         1743.29


_cell_measurement_reflns_used    15766
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_min          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_max          0.24

_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1756
_exptl_absorpt_coefficient_mu    1.835

# Sheldrick geometric approximatio 0.69 0.69 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_T_max  0.69
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            60623
_reflns_number_total             17332
_diffrn_reflns_av_R_equivalents  0.070
# Number of reflections without Friedels Law is 30078 
# Number of reflections with Friedels Law is 17332 
# Theoretical number of reflections is about 17546 


_diffrn_reflns_theta_min         5.084
_diffrn_reflns_theta_max         27.403
_diffrn_measured_fraction_theta_max 0.988

_diffrn_reflns_theta_full        25.759
_diffrn_measured_fraction_theta_full 0.991


_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_reflns_limit_h_min              -15
_reflns_limit_h_max              16
_reflns_limit_k_min              -23
_reflns_limit_k_max              23
_reflns_limit_l_min              0
_reflns_limit_l_max              23

_oxford_diffrn_Wilson_B_factor   1.67
_oxford_diffrn_Wilson_scale      178.89

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -4.41
_refine_diff_density_max         6.73


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         17332
_refine_ls_number_restraints     540
_refine_ls_number_parameters     1121
_oxford_refine_ls_R_factor_ref   0.1004
_refine_ls_wR_factor_ref         0.1205
_refine_ls_goodness_of_fit_ref   0.9790
_refine_ls_shift/su_max          0.0153303
_refine_ls_shift/su_mean         0.0004469


# The values computed from all data 
_oxford_reflns_number_all        17332
_refine_ls_R_factor_all          0.1004
_refine_ls_wR_factor_all         0.1205

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                11803
_refine_ls_R_factor_gt           0.0552
_refine_ls_wR_factor_gt          0.0877

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 2.40 1.51 0.157 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 1.2397(4) 0.7548(3) 0.4590(4) 0.0664 1.0000 Uani D . . . . .
C2 C 0.5758(6) 0.1946(4) 0.1267(4) 0.0243 1.0000 Uani . . . . . .
C4 C 0.4981(6) 0.0819(4) 0.0941(4) 0.0255 1.0000 Uani . . . . . .
C5 C 0.5434(6) 0.0220(4) 0.1261(4) 0.0256 1.0000 Uani . . . . . .
C6 C 0.6650(6) 0.0189(4) 0.1241(5) 0.0358 1.0000 Uani . . . . . .
C7 C 0.4760(7) -0.0389(4) 0.1579(4) 0.0317 1.0000 Uani . . . . . .
C8 C 0.3662(7) -0.0419(4) 0.1572(4) 0.0351 1.0000 Uani . . . . . .
C9 C 0.3305(7) 0.0139(4) 0.1141(5) 0.0348 1.0000 Uani . . . . . .
C10 C 0.3966(6) 0.0755(4) 0.0799(4) 0.0284 1.0000 Uani . . . . . .
C11 C 0.3575(7) 0.1309(5) 0.0289(5) 0.0416 1.0000 Uani . . . . . .
C12 C 0.2894(7) -0.1046(5) 0.2013(5) 0.0460 1.0000 Uani . . . . . .
C13 C 0.6398(7) 0.1638(4) -0.0066(4) 0.0320 1.0000 Uani . . . . . .
C14 C 0.6981(7) 0.2339(4) -0.0002(4) 0.0371 1.0000 Uani . . . . . .
C16 C 0.7086(6) 0.2991(4) 0.1154(4) 0.0299 1.0000 Uani . . . . . .
C17 C 0.6593(7) 0.3706(4) 0.1246(4) 0.0333 1.0000 Uani . . . . . .
C18 C 0.5454(9) 0.3881(5) 0.1166(6) 0.0531 1.0000 Uani . . . . . .
C19 C 0.7163(8) 0.4261(5) 0.1453(4) 0.0435 1.0000 Uani . . . . . .
C20 C 0.8105(6) 0.2814(5) 0.1275(4) 0.0353 1.0000 Uani . . . . . .
C21 C 0.8574(7) 0.2045(5) 0.1212(5) 0.0443 1.0000 Uani . . . . . .
C22 C 0.8633(7) 0.3395(5) 0.1473(5) 0.0451 1.0000 Uani . . . . . .
C23 C 0.4825(6) 0.1701(4) 0.3625(4) 0.0230 1.0000 Uani . . . . . .
C25 C 0.4851(7) 0.1121(4) 0.4820(4) 0.0355 1.0000 Uani . . . . . .
C26 C 0.4531(7) 0.1939(4) 0.4947(4) 0.0324 1.0000 Uani . . . . . .
C28 C 0.4246(6) 0.2981(4) 0.4041(4) 0.0239 1.0000 Uani . . . . . .
C29 C 0.3133(6) 0.3263(4) 0.4316(4) 0.0297 1.0000 Uani . . . . . .
C30 C 0.2167(6) 0.2802(4) 0.4835(5) 0.0380 1.0000 Uani . . . . . .
C31 C 0.2930(7) 0.4000(4) 0.4110(5) 0.0345 1.0000 Uani . . . . . .
C32 C 0.3791(7) 0.4456(4) 0.3646(5) 0.0365 1.0000 Uani . . . . . .
C33 C 0.3520(8) 0.5236(5) 0.3384(6) 0.0553 1.0000 Uani . . . . . .
C34 C 0.4898(7) 0.4176(4) 0.3433(4) 0.0334 1.0000 Uani . . . . . .
C35 C 0.5142(6) 0.3455(4) 0.3649(4) 0.0276 1.0000 Uani . . . . . .
C36 C 0.6361(6) 0.3206(4) 0.3477(5) 0.0368 1.0000 Uani . . . . . .
C37 C 0.5512(6) 0.0375(4) 0.3619(4) 0.0263 1.0000 Uani . . . . . .
C38 C 0.4772(6) -0.0168(4) 0.3585(4) 0.0281 1.0000 Uani . . . . . .
C39 C 0.3513(7) -0.0008(5) 0.3835(5) 0.0424 1.0000 Uani . . . . . .
C40 C 0.5220(7) -0.0849(4) 0.3286(4) 0.0312 1.0000 Uani . . . . . .
C41 C 0.6369(7) -0.1014(4) 0.3037(4) 0.0338 1.0000 Uani . . . . . .
C42 C 0.6830(8) -0.1756(5) 0.2695(5) 0.0548 1.0000 Uani . . . . . .
C43 C 0.7086(7) -0.0457(5) 0.3088(5) 0.0357 1.0000 Uani . . . . . .
C44 C 0.6677(7) 0.0226(4) 0.3381(4) 0.0326 1.0000 Uani . . . . . .
C45 C 0.7490(8) 0.0812(5) 0.3425(5) 0.0476 1.0000 Uani . . . . . .
C47 C 0.6337(6) 0.6034(4) 0.3774(5) 0.0332 1.0000 Uani . . . . . .
C50 C 0.7552(6) 0.5896(4) 0.3666(4) 0.0263 1.0000 Uani . . . . . .
C51 C 0.8348(6) 0.6409(4) 0.3229(4) 0.0251 1.0000 Uani . . . . . .
C52 C 0.9507(6) 0.6306(4) 0.3091(4) 0.0258 1.0000 Uani . . . . . .
C53 C 0.9806(6) 0.5647(4) 0.3429(4) 0.0287 1.0000 Uani . . . . . .
C54 C 0.9016(6) 0.5128(4) 0.3860(5) 0.0349 1.0000 Uani . . . . . .
C55 C 0.7886(6) 0.5247(4) 0.3987(4) 0.0315 1.0000 Uani . . . . . .
C56 C 0.9410(5) 0.4410(2) 0.4142(3) 0.0638 1.0000 Uani D . . . . .
C61 C 1.0103(7) 0.9429(5) 0.1143(5) 0.0391 1.0000 Uani . . . . . .
C64 C 0.9886(6) 0.8606(4) 0.1266(4) 0.0303 1.0000 Uani . . . . . .
C65 C 1.0227(6) 0.8189(4) 0.1816(4) 0.0274 1.0000 Uani . . . . . .
C66 C 1.0044(5) 0.7427(4) 0.1972(4) 0.0231 1.0000 Uani . . . . . .
C67 C 0.9519(6) 0.7094(4) 0.1505(4) 0.0299 1.0000 Uani . . . . . .
C68 C 0.9192(6) 0.7498(5) 0.0948(4) 0.0345 1.0000 Uani . . . . . .
C69 C 0.9355(6) 0.8262(5) 0.0826(4) 0.0371 1.0000 Uani . . . . . .
C71 C 0.2885(10) 0.2593(7) 0.1640(6) 0.0740 1.0000 Uani . . . . . .
C72 C 0.1597(9) 0.1676(6) 0.2389(7) 0.0731 1.0000 Uani . . . . . .
C73 C 0.1604(8) 0.2902(6) 0.2884(6) 0.0644 1.0000 Uani . . . . . .
C74 C 1.0844(7) 0.8322(4) 0.4470(5) 0.0370 1.0000 Uani . . . . . .
C75 C 1.1547(7) 0.7707(4) 0.4218(5) 0.0363 1.0000 Uani . . . . . .
C76 C 1.1424(6) 0.7270(4) 0.3654(4) 0.0282 1.0000 Uani . . . . . .
C77 C 1.0614(6) 0.7433(4) 0.3284(4) 0.0252 1.0000 Uani . . . . . .
C78 C 0.9889(6) 0.8043(4) 0.3584(4) 0.0266 1.0000 Uani . . . . . .
C79 C 1.0006(6) 0.8481(4) 0.4160(4) 0.0307 1.0000 Uani . . . . . .
C80 C 1.1634(6) 0.6500(4) 0.2088(4) 0.0246 1.0000 Uani . . . . . .
C81 C 1.2713(6) 0.6776(4) 0.1947(4) 0.0263 1.0000 Uani . . . . . .
C82 C 1.3693(6) 0.6418(4) 0.1462(5) 0.0333 1.0000 Uani . . . . . .
C83 C 1.3635(7) 0.5780(4) 0.1097(5) 0.0379 1.0000 Uani . . . . . .
C84 C 1.2574(6) 0.5498(4) 0.1207(4) 0.0312 1.0000 Uani . . . . . .
C85 C 1.1600(6) 0.5854(4) 0.1700(4) 0.0320 1.0000 Uani . . . . . .
C86 C 0.8188(8) 0.4121(5) 0.1570(5) 0.0481 1.0000 Uani . . . . . .
C87 C 1.2450(8) 0.4823(5) 0.0820(6) 0.0470 1.0000 Uani . . . . . .
C88 C 0.8588(5) 0.7135(4) 0.0517(3) 0.0686 1.0000 Uani D . . . . .
C89 C 1.4831(3) 0.6716(3) 0.1338(3) 0.0573 1.0000 Uani D . . . . .
C90 C 0.9247(3) 0.9152(2) 0.4406(3) 0.0478 1.0000 Uani D . . . . .
C91 C 0.8798(10) 0.4742(6) 0.1761(6) 0.0744 1.0000 Uani . . . . . .
F46 F 0.5638(4) 0.5563(3) 0.4275(3) 0.0552 1.0000 Uani . . . . . .
F48 F 0.6142(4) 0.5984(3) 0.3097(3) 0.0578 1.0000 Uani . . . . . .
F49 F 0.5977(4) 0.6719(3) 0.4015(3) 0.0546 1.0000 Uani . . . . . .
F60 F 1.0213(5) 0.9734(3) 0.1755(3) 0.0592 1.0000 Uani . . . . . .
F62 F 1.1054(4) 0.9570(3) 0.0540(3) 0.0585 1.0000 Uani . . . . . .
F63 F 0.9283(5) 0.9807(3) 0.0964(4) 0.0708 1.0000 Uani . . . . . .
F300 F 0.8535(10) 0.7509(6) -0.0136(5) 0.0634 0.536(12) Uani D . P 1 1 .
F301 F 0.7545(8) 0.6904(8) 0.0898(6) 0.0920 0.536(12) Uani D . P 1 1 .
F302 F 0.9201(10) 0.6506(6) 0.0208(7) 0.0716 0.536(12) Uani D . P 1 1 .
F303 F 0.8941(10) 0.7285(8) -0.0262(4) 0.0690 0.464(12) Uani D . P 1 2 .
F304 F 0.7493(7) 0.7386(8) 0.0791(7) 0.0687 0.464(12) Uani D . P 1 2 .
F305 F 0.8536(13) 0.6389(5) 0.0551(8) 0.0768 0.464(12) Uani D . P 1 2 .
F400 F 1.1981(7) 0.7517(5) 0.5376(4) 0.0779 0.708(9) Uani D . P 2 1 .
F401 F 1.3215(7) 0.8060(4) 0.4397(6) 0.0789 0.708(9) Uani D . P 2 1 .
F402 F 1.2941(7) 0.6897(4) 0.4442(5) 0.0633 0.708(9) Uani D . P 2 1 .
F403 F 1.2516(14) 0.7934(9) 0.5145(9) 0.0741 0.292(9) Uani D . P 2 2 .
F404 F 1.3407(9) 0.7631(11) 0.3964(7) 0.0674 0.292(9) Uani D . P 2 2 .
F405 F 1.2439(15) 0.6853(6) 0.4868(11) 0.0756 0.292(9) Uani D . P 2 2 .
F500 F 0.9280(19) 0.4425(9) 0.4911(6) 0.0714 0.41(2) Uani D . P 3 1 .
F501 F 1.0489(8) 0.4266(9) 0.3764(10) 0.0607 0.41(2) Uani D . P 3 1 .
F502 F 0.8840(14) 0.3791(7) 0.4123(13) 0.0714 0.41(2) Uani D . P 3 1 .
F503 F 0.8785(12) 0.4252(7) 0.4909(5) 0.0743 0.59(2) Uani D . P 3 2 .
F504 F 1.0479(7) 0.4338(7) 0.4080(10) 0.0783 0.59(2) Uani D . P 3 2 .
F505 F 0.9179(12) 0.3828(5) 0.3782(8) 0.0693 0.59(2) Uani D . P 3 2 .
F600 F 1.4839(16) 0.7050(14) 0.1968(10) 0.0606 0.257(16) Uani D . P 4 1 .
F601 F 1.5289(16) 0.7221(12) 0.0751(11) 0.0629 0.257(16) Uani D . P 4 1 .
F602 F 1.5582(14) 0.6153(8) 0.1187(15) 0.0574 0.257(16) Uani D . P 4 1 .
F603 F 1.4815(6) 0.7371(5) 0.1636(6) 0.0759 0.743(16) Uani D . P 4 2 .
F604 F 1.5389(6) 0.6846(6) 0.0560(4) 0.0627 0.743(16) Uani D . P 4 2 .
F605 F 1.5517(6) 0.6249(5) 0.1557(6) 0.0638 0.743(16) Uani D . P 4 2 .
F700 F 0.9575(13) 0.9712(7) 0.3848(10) 0.0578 0.57(5) Uani D . P 5 1 .
F701 F 0.9195(13) 0.9441(12) 0.5090(8) 0.0537 0.57(5) Uani D . P 5 1 .
F702 F 0.8173(7) 0.9003(9) 0.4471(11) 0.0464 0.57(5) Uani D . P 5 1 .
F703 F 0.9683(13) 0.9812(6) 0.4075(14) 0.0522 0.43(5) Uani D . P 5 2 .
F704 F 0.9017(18) 0.9192(14) 0.5191(5) 0.0496 0.43(5) Uani D . P 5 2 .
F705 F 0.8238(10) 0.9121(12) 0.4298(12) 0.0471 0.43(5) Uani D . P 5 2 .
Ir1 Ir 0.50927(3) 0.184542(17) 0.245721(18) 0.0221 1.0000 Uani . . . . . .
N3 N 0.5587(5) 0.1509(3) 0.0724(3) 0.0276 1.0000 Uani . . . . . .
N15 N 0.6588(5) 0.2420(3) 0.0857(3) 0.0283 1.0000 Uani . . . . . .
N24 N 0.5079(5) 0.1066(3) 0.3977(3) 0.0272 1.0000 Uani . . . . . .
N27 N 0.4465(5) 0.2208(3) 0.4175(3) 0.0266 1.0000 Uani . . . . . .
N70 N 0.2298(6) 0.2262(4) 0.2477(5) 0.0547 1.0000 Uani . . . . . .
B13 B 0.3212(10) 0.2006(6) 0.2840(6) 0.0516 1.0000 Uani . . . . . .
B17 B 1.0453(6) 0.6920(4) 0.2614(5) 0.0234 1.0000 Uani . . . . . .
H12 H 0.3932 0.2586 0.2762 0.0595 1.0000 Uiso R . . . . .
H13 H 0.6014 0.1155 0.2357 0.0185 1.0000 Uiso R . . . . .
H14 H 0.6233 0.2343 0.2422 0.0335 1.0000 Uiso R . . . . .
H61 H 0.6685 0.0019 0.1743 0.0542 1.0000 Uiso R . . . . .
H62 H 0.6972 0.0675 0.1109 0.0541 1.0000 Uiso R . . . . .
H63 H 0.7091 -0.0151 0.0853 0.0541 1.0000 Uiso R . . . . .
H71 H 0.5051 -0.0788 0.1806 0.0379 1.0000 Uiso R . . . . .
H91 H 0.2605 0.0098 0.1083 0.0423 1.0000 Uiso R . . . . .
H111 H 0.2766 0.1368 0.0500 0.0630 1.0000 Uiso R . . . . .
H112 H 0.3791 0.1130 -0.0230 0.0629 1.0000 Uiso R . . . . .
H113 H 0.3910 0.1788 0.0269 0.0629 1.0000 Uiso R . . . . .
H121 H 0.2284 -0.0849 0.2443 0.0691 1.0000 Uiso R . . . . .
H122 H 0.2589 -0.1283 0.1673 0.0691 1.0000 Uiso R . . . . .
H123 H 0.3321 -0.1411 0.2214 0.0690 1.0000 Uiso R . . . . .
H11 H 0.3702 0.1448 0.2461 0.0361 1.0000 Uiso R . . . . .
H131 H 0.6010 0.1718 -0.0440 0.0381 1.0000 Uiso R . . . . .
H132 H 0.6930 0.1219 -0.0219 0.0378 1.0000 Uiso R . . . . .
H141 H 0.7795 0.2274 -0.0209 0.0452 1.0000 Uiso R . . . . .
H142 H 0.6757 0.2765 -0.0274 0.0449 1.0000 Uiso R . . . . .
H181 H 0.5404 0.4398 0.1019 0.0800 1.0000 Uiso R . . . . .
H182 H 0.4857 0.3774 0.1653 0.0801 1.0000 Uiso R . . . . .
H183 H 0.5356 0.3585 0.0775 0.0802 1.0000 Uiso R . . . . .
H191 H 0.6844 0.4740 0.1521 0.0520 1.0000 Uiso R . . . . .
H211 H 0.9242 0.2017 0.1357 0.0670 1.0000 Uiso R . . . . .
H212 H 0.8774 0.1905 0.0678 0.0668 1.0000 Uiso R . . . . .
H213 H 0.8016 0.1709 0.1547 0.0670 1.0000 Uiso R . . . . .
H221 H 0.9319 0.3290 0.1543 0.0541 1.0000 Uiso R . . . . .
H251 H 0.5514 0.0981 0.4959 0.0432 1.0000 Uiso R . . . . .
H252 H 0.4231 0.0807 0.5126 0.0430 1.0000 Uiso R . . . . .
H261 H 0.5101 0.2200 0.5071 0.0389 1.0000 Uiso R . . . . .
H262 H 0.3801 0.2005 0.5358 0.0388 1.0000 Uiso R . . . . .
H301 H 0.2276 0.2289 0.4692 0.0572 1.0000 Uiso R . . . . .
H302 H 0.1465 0.2995 0.4793 0.0570 1.0000 Uiso R . . . . .
H303 H 0.2133 0.2818 0.5368 0.0571 1.0000 Uiso R . . . . .
H311 H 0.2191 0.4193 0.4288 0.0408 1.0000 Uiso R . . . . .
H331 H 0.3377 0.5561 0.3810 0.0831 1.0000 Uiso R . . . . .
H332 H 0.2861 0.5227 0.3229 0.0830 1.0000 Uiso R . . . . .
H333 H 0.4155 0.5414 0.2949 0.0831 1.0000 Uiso R . . . . .
H341 H 0.5491 0.4480 0.3138 0.0399 1.0000 Uiso R . . . . .
H361 H 0.6693 0.3483 0.3775 0.0553 1.0000 Uiso R . . . . .
H362 H 0.6407 0.2683 0.3614 0.0552 1.0000 Uiso R . . . . .
H363 H 0.6778 0.3286 0.2927 0.0551 1.0000 Uiso R . . . . .
H391 H 0.3156 -0.0397 0.3673 0.0642 1.0000 Uiso R . . . . .
H392 H 0.3208 0.0017 0.4393 0.0642 1.0000 Uiso R . . . . .
H393 H 0.3366 0.0460 0.3601 0.0641 1.0000 Uiso R . . . . .
H401 H 0.4726 -0.1206 0.3248 0.0383 1.0000 Uiso R . . . . .
H421 H 0.6436 -0.2156 0.3040 0.0819 1.0000 Uiso R . . . . .
H422 H 0.6731 -0.1791 0.2199 0.0821 1.0000 Uiso R . . . . .
H423 H 0.7620 -0.1815 0.2622 0.0821 1.0000 Uiso R . . . . .
H431 H 0.7865 -0.0549 0.2915 0.0431 1.0000 Uiso R . . . . .
H451 H 0.7344 0.0928 0.3960 0.0710 1.0000 Uiso R . . . . .
H452 H 0.7393 0.1258 0.3129 0.0712 1.0000 Uiso R . . . . .
H453 H 0.8252 0.0623 0.3199 0.0711 1.0000 Uiso R . . . . .
H511 H 0.8101 0.6837 0.3017 0.0302 1.0000 Uiso R . . . . .
H531 H 1.0567 0.5552 0.3360 0.0349 1.0000 Uiso R . . . . .
H551 H 0.7355 0.4898 0.4284 0.0381 1.0000 Uiso R . . . . .
H651 H 1.0592 0.8435 0.2096 0.0328 1.0000 Uiso R . . . . .
H671 H 0.9392 0.6579 0.1572 0.0361 1.0000 Uiso R . . . . .
H691 H 0.9123 0.8535 0.0454 0.0441 1.0000 Uiso R . . . . .
H711 H 0.3543 0.2279 0.1381 0.1091 1.0000 Uiso R . . . . .
H712 H 0.2352 0.2617 0.1352 0.1090 1.0000 Uiso R . . . . .
H713 H 0.3133 0.3094 0.1674 0.1092 1.0000 Uiso R . . . . .
H721 H 0.1197 0.1448 0.2895 0.1100 1.0000 Uiso R . . . . .
H722 H 0.2061 0.1305 0.2055 0.1100 1.0000 Uiso R . . . . .
H723 H 0.1062 0.1888 0.2162 0.1100 1.0000 Uiso R . . . . .
H731 H 0.2085 0.3265 0.2973 0.0961 1.0000 Uiso R . . . . .
H732 H 0.1193 0.3129 0.2569 0.0960 1.0000 Uiso R . . . . .
H733 H 0.1081 0.2721 0.3377 0.0961 1.0000 Uiso R . . . . .
H741 H 1.0931 0.8622 0.4843 0.0441 1.0000 Uiso R . . . . .
H761 H 1.1890 0.6850 0.3507 0.0341 1.0000 Uiso R . . . . .
H781 H 0.9308 0.8163 0.3388 0.0320 1.0000 Uiso R . . . . .
H811 H 1.2784 0.7211 0.2182 0.0318 1.0000 Uiso R . . . . .
H831 H 1.4291 0.5538 0.0780 0.0459 1.0000 Uiso R . . . . .
H851 H 1.0901 0.5646 0.1773 0.0392 1.0000 Uiso R . . . . .
H911 H 0.9333 0.4953 0.1289 0.1110 1.0000 Uiso R . . . . .
H912 H 0.8266 0.5120 0.2021 0.1108 1.0000 Uiso R . . . . .
H913 H 0.9201 0.4549 0.2094 0.1110 1.0000 Uiso R . . . . .
H133 H 0.2857 0.1857 0.3389 0.0614 1.0000 Uiso R . . . . .
F1 F 1.1784(6) 0.4929(3) 0.0398(4) 0.0783 1.0000 Uani . . . . . .
F2 F 1.1970(7) 0.4270(3) 0.1323(4) 0.0941 1.0000 Uani . . . . . .
F3 F 1.3422(5) 0.4555(4) 0.0341(4) 0.1006 1.0000 Uani . . . . . .

_refine_ls_extinction_coef       149.918
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.080
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . C75 . 1.461(8) yes
C1 . F400 . 1.344(6) yes
C1 . F401 . 1.349(6) yes
C1 . F402 . 1.321(6) yes
C1 . C75 . 1.461(8) yes
C1 . F403 . 1.310(7) yes
C1 . F404 . 1.393(7) yes
C1 . F405 . 1.324(7) yes
C2 . Ir1 . 2.039(7) yes
C2 . N3 . 1.374(9) yes
C2 . N15 . 1.355(9) yes
C4 . C5 . 1.389(9) yes
C4 . C10 . 1.398(10) yes
C4 . N3 . 1.445(8) yes
C5 . C6 . 1.517(10) yes
C5 . C7 . 1.384(10) yes
C6 . H61 . 0.963 no
C6 . H62 . 0.960 no
C6 . H63 . 0.964 no
C7 . C8 . 1.389(11) yes
C7 . H71 . 0.932 no
C8 . C9 . 1.392(11) yes
C8 . C12 . 1.516(10) yes
C9 . C10 . 1.394(10) yes
C9 . H91 . 0.930 no
C10 . C11 . 1.505(10) yes
C11 . H111 . 0.961 no
C11 . H112 . 0.959 no
C11 . H113 . 0.966 no
C12 . H121 . 0.960 no
C12 . H122 . 0.959 no
C12 . H123 . 0.965 no
C13 . C14 . 1.510(10) yes
C13 . N3 . 1.464(9) yes
C13 . H131 . 0.967 no
C13 . H132 . 0.973 no
C14 . N15 . 1.486(8) yes
C14 . H141 . 0.967 no
C14 . H142 . 0.973 no
C16 . C17 . 1.396(10) yes
C16 . C20 . 1.396(10) yes
C16 . N15 . 1.442(9) yes
C17 . C18 . 1.508(12) yes
C17 . C19 . 1.390(11) yes
C18 . H181 . 0.957 no
C18 . H182 . 0.961 no
C18 . H183 . 0.955 no
C19 . C86 . 1.389(13) yes
C19 . H191 . 0.930 no
C20 . C21 . 1.473(11) yes
C20 . C22 . 1.385(11) yes
C21 . H211 . 0.963 no
C21 . H212 . 0.963 no
C21 . H213 . 0.963 no
C22 . C86 . 1.392(13) yes
C22 . H221 . 0.925 no
C23 . Ir1 . 2.040(7) yes
C23 . N24 . 1.357(8) yes
C23 . N27 . 1.339(9) yes
C25 . C26 . 1.514(10) yes
C25 . N24 . 1.470(8) yes
C25 . H251 . 0.972 no
C25 . H252 . 0.970 no
C26 . N27 . 1.489(8) yes
C26 . H261 . 0.968 no
C26 . H262 . 0.973 no
C28 . C29 . 1.399(10) yes
C28 . C35 . 1.400(10) yes
C28 . N27 . 1.428(8) yes
C29 . C30 . 1.505(10) yes
C29 . C31 . 1.393(10) yes
C30 . H301 . 0.962 no
C30 . H302 . 0.961 no
C30 . H303 . 0.959 no
C31 . C32 . 1.386(11) yes
C31 . H311 . 0.932 no
C32 . C33 . 1.517(10) yes
C32 . C34 . 1.393(11) yes
C33 . H331 . 0.960 no
C33 . H332 . 0.964 no
C33 . H333 . 0.962 no
C34 . C35 . 1.385(10) yes
C34 . H341 . 0.932 no
C35 . C36 . 1.510(10) yes
C36 . H361 . 0.959 no
C36 . H362 . 0.962 no
C36 . H363 . 0.964 no
C37 . C38 . 1.392(10) yes
C37 . C44 . 1.398(10) yes
C37 . N24 . 1.432(8) yes
C38 . C39 . 1.511(10) yes
C38 . C40 . 1.384(10) yes
C39 . H391 . 0.958 no
C39 . H392 . 0.958 no
C39 . H393 . 0.961 no
C40 . C41 . 1.384(10) yes
C40 . H401 . 0.931 no
C41 . C42 . 1.509(10) yes
C41 . C43 . 1.402(11) yes
C42 . H421 . 0.958 no
C42 . H422 . 0.960 no
C42 . H423 . 0.958 no
C43 . C44 . 1.372(10) yes
C43 . H431 . 0.932 no
C44 . C45 . 1.519(11) yes
C45 . H451 . 0.961 no
C45 . H452 . 0.966 no
C45 . H453 . 0.961 no
C47 . C50 . 1.485(10) yes
C47 . F46 . 1.321(9) yes
C47 . F48 . 1.347(9) yes
C47 . F49 . 1.338(8) yes
C50 . C51 . 1.389(9) yes
C50 . C55 . 1.388(10) yes
C51 . C52 . 1.398(9) yes
C51 . H511 . 0.931 no
C52 . C53 . 1.399(10) yes
C52 . B17 . 1.637(10) yes
C53 . C54 . 1.390(10) yes
C53 . H531 . 0.932 no
C54 . C55 . 1.371(10) yes
C54 . C56 . 1.489(8) yes
C55 . H551 . 0.938 no
C56 . F500 . 1.355(7) yes
C56 . F501 . 1.317(7) yes
C56 . F502 . 1.355(7) yes
C56 . F503 . 1.367(6) yes
C56 . F504 . 1.312(6) yes
C56 . F505 . 1.356(6) yes
C61 . C64 . 1.502(11) yes
C61 . F60 . 1.320(10) yes
C61 . F62 . 1.340(9) yes
C61 . F63 . 1.334(8) yes
C64 . C65 . 1.391(9) yes
C64 . C69 . 1.388(10) yes
C65 . C66 . 1.393(9) yes
C65 . H651 . 0.931 no
C66 . C67 . 1.412(9) yes
C66 . B17 . 1.648(10) yes
C67 . C68 . 1.380(10) yes
C67 . H671 . 0.937 no
C68 . C69 . 1.389(11) yes
C68 . C88 . 1.458(8) yes
C69 . H691 . 0.933 no
C71 . N70 . 1.544(13) yes
C71 . H711 . 0.975 no
C71 . H712 . 0.981 no
C71 . H713 . 0.975 no
C72 . N70 . 1.448(12) yes
C72 . H721 . 0.963 no
C72 . H722 . 0.962 no
C72 . H723 . 0.961 no
C73 . N70 . 1.483(10) yes
C73 . H731 . 0.963 no
C73 . H732 . 0.961 no
C73 . H733 . 0.961 no
C74 . C75 . 1.382(11) yes
C74 . C79 . 1.370(10) yes
C74 . H741 . 0.928 no
C75 . C76 . 1.380(10) yes
C76 . C77 . 1.414(9) yes
C76 . H761 . 0.928 no
C77 . C78 . 1.404(9) yes
C77 . B17 . 1.641(10) yes
C78 . C79 . 1.395(9) yes
C78 . H781 . 0.931 no
C79 . C90 . 1.496(8) yes
C80 . C81 . 1.398(9) yes
C80 . C85 . 1.400(9) yes
C80 . B17 . 1.645(10) yes
C81 . C82 . 1.401(10) yes
C81 . H811 . 0.934 no
C82 . C83 . 1.372(11) yes
C82 . C89 . 1.488(8) yes
C83 . C84 . 1.393(10) yes
C83 . H831 . 0.935 no
C84 . C85 . 1.400(9) yes
C84 . C87 . 1.474(11) yes
C85 . H851 . 0.934 no
C86 . C91 . 1.499(11) yes
C87 . F1 . 1.321(11) yes
C87 . F2 . 1.325(10) yes
C87 . F3 . 1.325(10) yes
C88 . F300 . 1.354(6) yes
C88 . F301 . 1.327(6) yes
C88 . F302 . 1.373(6) yes
C88 . F303 . 1.349(7) yes
C88 . F304 . 1.361(6) yes
C88 . F305 . 1.339(6) yes
C89 . F600 . 1.327(7) yes
C89 . F601 . 1.345(7) yes
C89 . F602 . 1.327(7) yes
C89 . F603 . 1.318(6) yes
C89 . F604 . 1.360(6) yes
C89 . F605 . 1.322(6) yes
C90 . F700 . 1.357(6) yes
C90 . F701 . 1.357(6) yes
C90 . F702 . 1.351(6) yes
C90 . F703 . 1.347(7) yes
C90 . F704 . 1.363(7) yes
C90 . F705 . 1.353(7) yes
C91 . H911 . 0.961 no
C91 . H912 . 0.956 no
C91 . H913 . 0.958 no
Ir1 . H12 . 1.890 no
Ir1 . H13 . 1.635 no
Ir1 . H14 . 1.701 no
Ir1 . H11 . 1.914 no
N70 . B13 . 1.554(12) yes
B13 . H12 . 1.377 no
B13 . H11 . 1.262 no
B13 . H133 . 0.973 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C75 . C1 . F400 . 114.3(6) yes
C75 . C1 . F401 . 113.3(5) yes
F400 . C1 . F401 . 105.04(7) yes
C75 . C1 . F402 . 116.0(6) yes
F400 . C1 . F402 . 101.83(7) yes
F401 . C1 . F402 . 105.17(7) yes
C75 . C1 . F403 . 124.8(8) yes
C75 . C1 . F404 . 102.4(7) yes
F403 . C1 . F404 . 105.08(7) yes
C75 . C1 . F405 . 115.8(9) yes
F403 . C1 . F405 . 101.84(7) yes
F404 . C1 . F405 . 105.05(7) yes
Ir1 . C2 . N3 . 128.8(5) yes
Ir1 . C2 . N15 . 125.0(5) yes
N3 . C2 . N15 . 105.8(6) yes
C5 . C4 . C10 . 120.9(6) yes
C5 . C4 . N3 . 119.6(6) yes
C10 . C4 . N3 . 119.4(6) yes
C4 . C5 . C6 . 122.8(6) yes
C4 . C5 . C7 . 118.3(7) yes
C6 . C5 . C7 . 118.8(7) yes
C5 . C6 . H61 . 110.4 no
C5 . C6 . H62 . 110.2 no
H61 . C6 . H62 . 108.8 no
C5 . C6 . H63 . 109.8 no
H61 . C6 . H63 . 108.8 no
H62 . C6 . H63 . 108.8 no
C5 . C7 . C8 . 121.9(7) yes
C5 . C7 . H71 . 118.9 no
C8 . C7 . H71 . 119.2 no
C7 . C8 . C9 . 117.6(7) yes
C7 . C8 . C12 . 120.6(7) yes
C9 . C8 . C12 . 121.8(7) yes
C8 . C9 . C10 . 121.9(7) yes
C8 . C9 . H91 . 118.7 no
C10 . C9 . H91 . 119.3 no
C4 . C10 . C9 . 117.5(7) yes
C4 . C10 . C11 . 123.1(7) yes
C9 . C10 . C11 . 119.4(7) yes
C10 . C11 . H111 . 109.4 no
C10 . C11 . H112 . 109.4 no
H111 . C11 . H112 . 109.5 no
C10 . C11 . H113 . 110.3 no
H111 . C11 . H113 . 108.8 no
H112 . C11 . H113 . 109.4 no
C8 . C12 . H121 . 109.7 no
C8 . C12 . H122 . 110.3 no
H121 . C12 . H122 . 109.3 no
C8 . C12 . H123 . 109.4 no
H121 . C12 . H123 . 109.0 no
H122 . C12 . H123 . 109.1 no
C14 . C13 . N3 . 103.3(6) yes
C14 . C13 . H131 . 110.7 no
N3 . C13 . H131 . 110.7 no
C14 . C13 . H132 . 111.7 no
N3 . C13 . H132 . 111.1 no
H131 . C13 . H132 . 109.3 no
C13 . C14 . N15 . 102.0(6) yes
C13 . C14 . H141 . 111.3 no
N15 . C14 . H141 . 110.6 no
C13 . C14 . H142 . 111.6 no
N15 . C14 . H142 . 112.2 no
H141 . C14 . H142 . 109.1 no
C17 . C16 . C20 . 122.6(7) yes
C17 . C16 . N15 . 119.5(7) yes
C20 . C16 . N15 . 117.6(7) yes
C16 . C17 . C18 . 122.3(7) yes
C16 . C17 . C19 . 117.8(8) yes
C18 . C17 . C19 . 119.8(8) yes
C17 . C18 . H181 . 109.8 no
C17 . C18 . H182 . 110.5 no
H181 . C18 . H182 . 108.9 no
C17 . C18 . H183 . 110.0 no
H181 . C18 . H183 . 109.1 no
H182 . C18 . H183 . 108.6 no
C17 . C19 . C86 . 122.1(8) yes
C17 . C19 . H191 . 119.0 no
C86 . C19 . H191 . 119.0 no
C16 . C20 . C21 . 121.3(7) yes
C16 . C20 . C22 . 116.5(8) yes
C21 . C20 . C22 . 122.2(8) yes
C20 . C21 . H211 . 110.1 no
C20 . C21 . H212 . 108.8 no
H211 . C21 . H212 . 108.9 no
C20 . C21 . H213 . 109.7 no
H211 . C21 . H213 . 109.9 no
H212 . C21 . H213 . 109.3 no
C20 . C22 . C86 . 123.6(8) yes
C20 . C22 . H221 . 117.6 no
C86 . C22 . H221 . 118.8 no
Ir1 . C23 . N24 . 124.8(5) yes
Ir1 . C23 . N27 . 128.2(5) yes
N24 . C23 . N27 . 106.8(6) yes
C26 . C25 . N24 . 102.7(5) yes
C26 . C25 . H251 . 111.7 no
N24 . C25 . H251 . 111.6 no
C26 . C25 . H252 . 110.9 no
N24 . C25 . H252 . 111.3 no
H251 . C25 . H252 . 108.6 no
C25 . C26 . N27 . 102.4(5) yes
C25 . C26 . H261 . 111.5 no
N27 . C26 . H261 . 111.2 no
C25 . C26 . H262 . 111.8 no
N27 . C26 . H262 . 110.4 no
H261 . C26 . H262 . 109.4 no
C29 . C28 . C35 . 120.5(6) yes
C29 . C28 . N27 . 119.4(6) yes
C35 . C28 . N27 . 120.1(6) yes
C28 . C29 . C30 . 122.2(6) yes
C28 . C29 . C31 . 118.2(7) yes
C30 . C29 . C31 . 119.6(7) yes
C29 . C30 . H301 . 110.4 no
C29 . C30 . H302 . 110.0 no
H301 . C30 . H302 . 109.7 no
C29 . C30 . H303 . 109.6 no
H301 . C30 . H303 . 108.0 no
H302 . C30 . H303 . 109.2 no
C29 . C31 . C32 . 122.1(7) yes
C29 . C31 . H311 . 118.9 no
C32 . C31 . H311 . 119.0 no
C31 . C32 . C33 . 120.4(8) yes
C31 . C32 . C34 . 118.1(7) yes
C33 . C32 . C34 . 121.5(8) yes
C32 . C33 . H331 . 108.8 no
C32 . C33 . H332 . 109.8 no
H331 . C33 . H332 . 109.6 no
C32 . C33 . H333 . 109.5 no
H331 . C33 . H333 . 109.3 no
H332 . C33 . H333 . 109.7 no
C32 . C34 . C35 . 121.5(7) yes
C32 . C34 . H341 . 119.4 no
C35 . C34 . H341 . 119.1 no
C28 . C35 . C34 . 118.9(7) yes
C28 . C35 . C36 . 121.7(7) yes
C34 . C35 . C36 . 119.4(7) yes
C35 . C36 . H361 . 109.8 no
C35 . C36 . H362 . 110.4 no
H361 . C36 . H362 . 108.7 no
C35 . C36 . H363 . 109.7 no
H361 . C36 . H363 . 109.5 no
H362 . C36 . H363 . 108.7 no
C38 . C37 . C44 . 120.7(6) yes
C38 . C37 . N24 . 120.1(6) yes
C44 . C37 . N24 . 118.8(7) yes
C37 . C38 . C39 . 120.9(7) yes
C37 . C38 . C40 . 118.5(7) yes
C39 . C38 . C40 . 120.5(7) yes
C38 . C39 . H391 . 109.5 no
C38 . C39 . H392 . 109.5 no
H391 . C39 . H392 . 109.6 no
C38 . C39 . H393 . 110.2 no
H391 . C39 . H393 . 109.0 no
H392 . C39 . H393 . 109.1 no
C38 . C40 . C41 . 122.4(7) yes
C38 . C40 . H401 . 118.4 no
C41 . C40 . H401 . 119.2 no
C40 . C41 . C42 . 121.0(8) yes
C40 . C41 . C43 . 117.4(7) yes
C42 . C41 . C43 . 121.6(7) yes
C41 . C42 . H421 . 110.0 no
C41 . C42 . H422 . 110.0 no
H421 . C42 . H422 . 108.7 no
C41 . C42 . H423 . 111.0 no
H421 . C42 . H423 . 108.4 no
H422 . C42 . H423 . 108.7 no
C41 . C43 . C44 . 122.0(7) yes
C41 . C43 . H431 . 119.3 no
C44 . C43 . H431 . 118.6 no
C37 . C44 . C43 . 118.9(7) yes
C37 . C44 . C45 . 121.1(7) yes
C43 . C44 . C45 . 120.0(7) yes
C44 . C45 . H451 . 110.2 no
C44 . C45 . H452 . 109.1 no
H451 . C45 . H452 . 109.7 no
C44 . C45 . H453 . 109.0 no
H451 . C45 . H453 . 109.9 no
H452 . C45 . H453 . 109.0 no
C50 . C47 . F46 . 114.9(7) yes
C50 . C47 . F48 . 111.3(6) yes
F46 . C47 . F48 . 105.4(6) yes
C50 . C47 . F49 . 112.5(6) yes
F46 . C47 . F49 . 106.5(6) yes
F48 . C47 . F49 . 105.5(6) yes
C47 . C50 . C51 . 119.8(7) yes
C47 . C50 . C55 . 119.6(6) yes
C51 . C50 . C55 . 120.6(6) yes
C50 . C51 . C52 . 122.7(7) yes
C50 . C51 . H511 . 118.7 no
C52 . C51 . H511 . 118.7 no
C51 . C52 . C53 . 115.0(6) yes
C51 . C52 . B17 . 123.5(6) yes
C53 . C52 . B17 . 121.4(6) yes
C52 . C53 . C54 . 122.8(7) yes
C52 . C53 . H531 . 118.6 no
C54 . C53 . H531 . 118.6 no
C53 . C54 . C55 . 120.8(7) yes
C53 . C54 . C56 . 119.6(6) yes
C55 . C54 . C56 . 119.5(6) yes
C50 . C55 . C54 . 118.3(7) yes
C50 . C55 . H551 . 121.3 no
C54 . C55 . H551 . 120.4 no
C54 . C56 . F500 . 111.0(7) yes
C54 . C56 . F501 . 112.1(7) yes
F500 . C56 . F501 . 106.95(7) yes
C54 . C56 . F502 . 116.8(8) yes
F500 . C56 . F502 . 102.11(7) yes
F501 . C56 . F502 . 106.95(7) yes
C54 . C56 . F503 . 110.7(6) yes
C54 . C56 . F504 . 118.2(7) yes
F503 . C56 . F504 . 106.97(7) yes
C54 . C56 . F505 . 110.6(7) yes
F503 . C56 . F505 . 102.10(7) yes
F504 . C56 . F505 . 106.95(7) yes
C64 . C61 . F60 . 113.4(6) yes
C64 . C61 . F62 . 111.3(7) yes
F60 . C61 . F62 . 106.6(7) yes
C64 . C61 . F63 . 112.0(7) yes
F60 . C61 . F63 . 107.6(7) yes
F62 . C61 . F63 . 105.4(6) yes
C61 . C64 . C65 . 119.9(7) yes
C61 . C64 . C69 . 120.0(7) yes
C65 . C64 . C69 . 120.1(7) yes
C64 . C65 . C66 . 123.4(7) yes
C64 . C65 . H651 . 118.0 no
C66 . C65 . H651 . 118.6 no
C65 . C66 . C67 . 114.9(6) yes
C65 . C66 . B17 . 124.3(6) yes
C67 . C66 . B17 . 120.8(6) yes
C66 . C67 . C68 . 122.3(7) yes
C66 . C67 . H671 . 118.9 no
C68 . C67 . H671 . 118.8 no
C67 . C68 . C69 . 121.2(7) yes
C67 . C68 . C88 . 120.0(7) yes
C69 . C68 . C88 . 118.6(7) yes
C68 . C69 . C64 . 118.0(7) yes
C68 . C69 . H691 . 121.0 no
C64 . C69 . H691 . 121.0 no
N70 . C71 . H711 . 108.5 no
N70 . C71 . H712 . 109.8 no
H711 . C71 . H712 . 110.8 no
N70 . C71 . H713 . 108.7 no
H711 . C71 . H713 . 109.2 no
H712 . C71 . H713 . 109.8 no
N70 . C72 . H721 . 109.3 no
N70 . C72 . H722 . 109.9 no
H721 . C72 . H722 . 109.5 no
N70 . C72 . H723 . 109.3 no
H721 . C72 . H723 . 109.5 no
H722 . C72 . H723 . 109.3 no
N70 . C73 . H731 . 109.9 no
N70 . C73 . H732 . 109.5 no
H731 . C73 . H732 . 109.5 no
N70 . C73 . H733 . 108.8 no
H731 . C73 . H733 . 109.5 no
H732 . C73 . H733 . 109.6 no
C75 . C74 . C79 . 118.7(7) yes
C75 . C74 . H741 . 121.0 no
C79 . C74 . H741 . 120.3 no
C1 . C75 . C74 . 116.4(7) yes
C1 . C75 . C76 . 123.0(7) yes
C74 . C75 . C76 . 120.7(7) yes
C75 . C76 . C77 . 122.9(7) yes
C75 . C76 . H761 . 119.1 no
C77 . C76 . H761 . 118.1 no
C76 . C77 . C78 . 114.2(6) yes
C76 . C77 . B17 . 123.6(6) yes
C78 . C77 . B17 . 122.0(6) yes
C77 . C78 . C79 . 122.8(7) yes
C77 . C78 . H781 . 118.7 no
C79 . C78 . H781 . 118.5 no
C78 . C79 . C74 . 120.5(7) yes
C78 . C79 . C90 . 119.3(6) yes
C74 . C79 . C90 . 120.1(6) yes
C81 . C80 . C85 . 115.5(6) yes
C81 . C80 . B17 . 124.1(6) yes
C85 . C80 . B17 . 120.3(6) yes
C80 . C81 . C82 . 122.0(7) yes
C80 . C81 . H811 . 119.1 no
C82 . C81 . H811 . 118.9 no
C81 . C82 . C83 . 121.2(7) yes
C81 . C82 . C89 . 120.7(7) yes
C83 . C82 . C89 . 118.1(7) yes
C82 . C83 . C84 . 118.5(7) yes
C82 . C83 . H831 . 121.1 no
C84 . C83 . H831 . 120.3 no
C83 . C84 . C85 . 119.8(7) yes
C83 . C84 . C87 . 121.3(7) yes
C85 . C84 . C87 . 118.9(7) yes
C80 . C85 . C84 . 122.9(7) yes
C80 . C85 . H851 . 119.1 no
C84 . C85 . H851 . 118.0 no
C22 . C86 . C19 . 117.4(8) yes
C22 . C86 . C91 . 122.2(9) yes
C19 . C86 . C91 . 120.4(9) yes
C84 . C87 . F1 . 113.4(7) yes
C84 . C87 . F2 . 113.0(8) yes
F1 . C87 . F2 . 103.5(8) yes
C84 . C87 . F3 . 113.4(8) yes
F1 . C87 . F3 . 105.9(8) yes
F2 . C87 . F3 . 106.9(8) yes
C68 . C88 . F300 . 116.2(7) yes
C68 . C88 . F301 . 118.9(6) yes
F300 . C88 . F301 . 105.42(7) yes
C68 . C88 . F302 . 107.8(6) yes
F300 . C88 . F302 . 101.27(7) yes
F301 . C88 . F302 . 105.36(7) yes
C68 . C88 . F303 . 116.3(7) yes
C68 . C88 . F304 . 107.3(6) yes
F303 . C88 . F304 . 105.35(7) yes
C68 . C88 . F305 . 119.9(7) yes
F303 . C88 . F305 . 101.32(7) yes
F304 . C88 . F305 . 105.37(7) yes
C82 . C89 . F600 . 110.7(9) yes
C82 . C89 . F601 . 120.1(10) yes
F600 . C89 . F601 . 103.62(7) yes
C82 . C89 . F602 . 108.6(10) yes
F600 . C89 . F602 . 109.61(7) yes
F601 . C89 . F602 . 103.62(7) yes
C82 . C89 . F603 . 114.5(5) yes
C82 . C89 . F604 . 109.8(6) yes
F603 . C89 . F604 . 103.58(7) yes
C82 . C89 . F605 . 114.6(5) yes
F603 . C89 . F605 . 109.63(7) yes
F604 . C89 . F605 . 103.62(7) yes
C79 . C90 . F700 . 109.9(7) yes
C79 . C90 . F701 . 116.3(8) yes
F700 . C90 . F701 . 106.68(7) yes
C79 . C90 . F702 . 110.9(8) yes
F700 . C90 . F702 . 105.76(7) yes
F701 . C90 . F702 . 106.70(7) yes
C79 . C90 . F703 . 116.0(8) yes
C79 . C90 . F704 . 106.2(9) yes
F703 . C90 . F704 . 106.69(7) yes
C79 . C90 . F705 . 114.9(10) yes
F703 . C90 . F705 . 105.76(7) yes
F704 . C90 . F705 . 106.68(7) yes
C86 . C91 . H911 . 109.9 no
C86 . C91 . H912 . 109.8 no
H911 . C91 . H912 . 109.6 no
C86 . C91 . H913 . 109.5 no
H911 . C91 . H913 . 108.6 no
H912 . C91 . H913 . 109.4 no
C23 . Ir1 . C2 . 166.2(3) yes
C23 . Ir1 . H12 . 84.9 no
C2 . Ir1 . H12 . 106.0 no
C23 . Ir1 . H13 . 85.3 no
C2 . Ir1 . H13 . 84.1 no
H12 . Ir1 . H13 . 169.8 no
C23 . Ir1 . H14 . 85.3 no
C2 . Ir1 . H14 . 84.2 no
H12 . Ir1 . H14 . 100.6 no
H13 . Ir1 . H14 . 81.3 no
C23 . Ir1 . H11 . 98.0 no
C2 . Ir1 . H11 . 93.8 no
H12 . Ir1 . H11 . 70.6 no
H13 . Ir1 . H11 . 108.1 no
H14 . Ir1 . H11 . 170.2 no
C13 . N3 . C4 . 120.5(6) yes
C13 . N3 . C2 . 113.4(6) yes
C4 . N3 . C2 . 122.3(6) yes
C14 . N15 . C16 . 118.0(6) yes
C14 . N15 . C2 . 114.0(6) yes
C16 . N15 . C2 . 128.0(6) yes
C25 . N24 . C37 . 119.0(5) yes
C25 . N24 . C23 . 113.9(5) yes
C37 . N24 . C23 . 127.1(6) yes
C26 . N27 . C28 . 119.7(6) yes
C26 . N27 . C23 . 113.6(6) yes
C28 . N27 . C23 . 125.6(6) yes
C71 . N70 . C73 . 102.8(8) yes
C71 . N70 . C72 . 105.1(8) yes
C73 . N70 . C72 . 111.5(8) yes
C71 . N70 . B13 . 109.3(8) yes
C73 . N70 . B13 . 111.7(7) yes
C72 . N70 . B13 . 115.4(8) yes
N70 . B13 . H12 . 108.9 no
N70 . B13 . H11 . 104.9 no
H12 . B13 . H11 . 112.7 no
N70 . B13 . H133 . 110.3 no
H12 . B13 . H133 . 110.1 no
H11 . B13 . H133 . 109.7 no
C66 . B17 . C80 . 104.7(5) yes
C66 . B17 . C77 . 111.8(6) yes
C80 . B17 . C77 . 113.0(5) yes
C66 . B17 . C52 . 111.5(5) yes
C80 . B17 . C52 . 110.6(6) yes
C77 . B17 . C52 . 105.5(6) yes
B13 . H12 . Ir1 . 84.9 no
B13 . H11 . Ir1 . 87.0 no
_database_code_depnum_ccdc_archive 'CCDC 1002306'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_11-and-12(X-ray)
#==============================================================================
_audit_creation_date             2014-01-22
_audit_creation_method           CRYSTALS_ver_14.52

_oxford_structure_analysis_title '069npmk12 (formerly 078npmk11)'
_chemical_name_systematic        .
_chemical_melting_point          'not measured'

_cell_length_a                   12.7291(1)
_cell_length_b                   17.5467(2)
_cell_length_c                   18.0265(2)
_cell_angle_alpha                88.2727(4)
_cell_angle_beta                 70.2021(5)
_cell_angle_gamma                87.5305(4)
_cell_volume                     3784.27(7)

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
Ir -1.4442 7.9887 27.3049 1.5928 16.7296 8.8655 15.6115 0.4179 5.8338 45.0011
11.4722 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C50 H100 B2 F12 Ir1 N4 O6 
# Dc =      1.14 Fooo =   1737.71 Mu =     18.31 M =   1295.19
# Found Formula = C76 H74.86 B2 F24.00 Ir1 N5 
# Dc =      1.52 FOOO =   1737.71 Mu =     18.69 M =   1728.11

_chemical_formula_sum            'C76 H74.86 B2 F24 Ir1 N5'
_chemical_formula_moiety         
'0.57(C44 H62 B Ir N5), 0.43(C44 H64 B Ir N5), C32 H12 B F24'
_chemical_compound_source        .
_chemical_formula_weight         1728.11

_cell_measurement_reflns_used    16488
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    100

_exptl_crystal_description       prism
_exptl_crystal_colour            clear_intense_yellow
_exptl_crystal_size_min          0.10
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_max          0.24

_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1737.713
_exptl_absorpt_coefficient_mu    1.869

# Sheldrick geometric approximatio 0.80 0.83 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_T_max  0.83
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      100
_diffrn_reflns_number            66843
_reflns_number_total             17238
_diffrn_reflns_av_R_equivalents  0.027
# Number of reflections without Friedels Law is 29207 
# Number of reflections with Friedels Law is 17238 
# Theoretical number of reflections is about 17376 


_diffrn_reflns_theta_min         5.110
_diffrn_reflns_theta_max         27.493
_diffrn_measured_fraction_theta_max 0.991

_diffrn_reflns_theta_full        26.393
_diffrn_measured_fraction_theta_full 0.992


_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_reflns_limit_h_min              -15
_reflns_limit_h_max              16
_reflns_limit_k_min              -22
_reflns_limit_k_max              22
_reflns_limit_l_min              0
_reflns_limit_l_max              23

_oxford_diffrn_Wilson_B_factor   1.77
_oxford_diffrn_Wilson_scale      29.58

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.22
_refine_diff_density_max         2.80


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         17238
_refine_ls_number_restraints     652
_refine_ls_number_parameters     1082
_oxford_refine_ls_R_factor_ref   0.0486
_refine_ls_wR_factor_ref         0.1042
_refine_ls_goodness_of_fit_ref   0.9128
_refine_ls_shift/su_max          0.0030306
_refine_ls_shift/su_mean         0.0000258


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        17238
_refine_ls_R_factor_all          0.0486
_refine_ls_wR_factor_all         0.1042

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                15356
_refine_ls_R_factor_gt           0.0411
_refine_ls_wR_factor_gt          0.0947

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 18.5 27.1 12.8 3.30 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ir1 Ir 0.522238(12) 0.679598(8) 0.242213(8) 0.0198 1.0000 Uani . . . . . .
C2 C 0.4903(3) 0.6650(2) 0.3610(2) 0.0190 1.0000 Uani . . . . . .
N3 N 0.4524(3) 0.71760(17) 0.41723(17) 0.0205 1.0000 Uani . . . . . .
C4 C 0.4557(4) 0.6916(2) 0.4952(2) 0.0259 1.0000 Uani . . . . . .
C5 C 0.4873(4) 0.6065(2) 0.4816(2) 0.0256 1.0000 Uani . . . . . .
N6 N 0.5133(3) 0.60052(18) 0.39576(17) 0.0210 1.0000 Uani . . . . . .
C7 C 0.5552(3) 0.5291(2) 0.3584(2) 0.0207 1.0000 Uani . . . . . .
C8 C 0.4798(3) 0.4761(2) 0.3522(2) 0.0203 1.0000 Uani . . . . . .
C9 C 0.3564(3) 0.4944(2) 0.3778(3) 0.0296 1.0000 Uani . . . . . .
C10 C 0.5223(3) 0.4051(2) 0.3203(2) 0.0215 1.0000 Uani . . . . . .
C11 C 0.6364(3) 0.3868(2) 0.2945(2) 0.0235 1.0000 Uani . . . . . .
C12 C 0.7085(3) 0.4410(2) 0.3025(2) 0.0252 1.0000 Uani . . . . . .
C13 C 0.6698(3) 0.5122(2) 0.3344(2) 0.0234 1.0000 Uani . . . . . .
C14 C 0.7501(4) 0.5699(3) 0.3413(3) 0.0312 1.0000 Uani . . . . . .
C15 C 0.6795(4) 0.3107(3) 0.2572(3) 0.0359 1.0000 Uani . . . . . .
C16 C 0.4304(3) 0.7966(2) 0.4022(2) 0.0212 1.0000 Uani . . . . . .
C17 C 0.5195(3) 0.8439(2) 0.3636(2) 0.0239 1.0000 Uani . . . . . .
C18 C 0.6404(4) 0.8183(3) 0.3476(3) 0.0368 1.0000 Uani . . . . . .
C19 C 0.4947(4) 0.9176(2) 0.3430(2) 0.0263 1.0000 Uani . . . . . .
C20 C 0.3860(4) 0.9464(2) 0.3624(3) 0.0314 1.0000 Uani . . . . . .
C21 C 0.2993(4) 0.9002(2) 0.4063(3) 0.0332 1.0000 Uani . . . . . .
C22 C 0.3199(3) 0.8246(2) 0.4264(2) 0.0265 1.0000 Uani . . . . . .
C23 C 0.2242(4) 0.7764(3) 0.4736(3) 0.0387 1.0000 Uani . . . . . .
C24 C 0.3610(5) 1.0262(3) 0.3369(4) 0.0473 1.0000 Uani . . . . . .
C25 C 0.5880(3) 0.6874(2) 0.1218(2) 0.0224 1.0000 Uani . . . . . .
N26 N 0.6699(3) 0.73402(19) 0.08100(18) 0.0248 1.0000 Uani . . . . . .
C27 C 0.7022(4) 0.7265(2) -0.0058(2) 0.0306 1.0000 Uani . . . . . .
C28 C 0.6377(4) 0.6570(2) -0.0126(2) 0.0297 1.0000 Uani . . . . . .
N29 N 0.5636(3) 0.64473(19) 0.06924(18) 0.0260 1.0000 Uani . . . . . .
C30 C 0.4934(3) 0.5799(2) 0.0921(2) 0.0246 1.0000 Uani . . . . . .
C31 C 0.5340(3) 0.5129(2) 0.1175(2) 0.0243 1.0000 Uani . . . . . .
C32 C 0.6555(4) 0.5008(2) 0.1091(3) 0.0307 1.0000 Uani . . . . . .
C33 C 0.4592(4) 0.4561(2) 0.1517(2) 0.0272 1.0000 Uani . . . . . .
C34 C 0.3460(4) 0.4654(2) 0.1605(2) 0.0302 1.0000 Uani . . . . . .
C35 C 0.3115(4) 0.5295(3) 0.1273(3) 0.0320 1.0000 Uani . . . . . .
C36 C 0.3837(4) 0.5876(2) 0.0916(3) 0.0307 1.0000 Uani . . . . . .
C37 C 0.3437(5) 0.6562(3) 0.0553(4) 0.0510 1.0000 Uani . . . . . .
C38 C 0.2638(4) 0.4063(3) 0.2059(3) 0.0401 1.0000 Uani . . . . . .
C39 C 0.7223(4) 0.7904(2) 0.1114(2) 0.0282 1.0000 Uani . . . . . .
C40 C 0.6771(4) 0.8652(3) 0.1209(3) 0.0363 1.0000 Uani . . . . . .
C41 C 0.5701(6) 0.8866(3) 0.1080(4) 0.0557 1.0000 Uani . . . . . .
C42 C 0.7378(6) 0.9197(3) 0.1442(3) 0.0492 1.0000 Uani . . . . . .
C43 C 0.8353(5) 0.9014(3) 0.1579(3) 0.0508 1.0000 Uani . . . . . .
C44 C 0.8993(7) 0.9625(4) 0.1802(4) 0.0804 1.0000 Uani . . . . . .
C45 C 0.8757(4) 0.8258(3) 0.1491(3) 0.0448 1.0000 Uani . . . . . .
C46 C 0.8201(4) 0.7698(3) 0.1258(2) 0.0323 1.0000 Uani . . . . . .
C47 C 0.8651(4) 0.6883(3) 0.1176(3) 0.0381 1.0000 Uani . . . . . .
F56 F 0.8978(2) 0.55141(17) 0.94034(17) 0.0444 1.0000 Uani . . . . . .
C57 C 0.9986(4) 0.5653(3) 0.8865(3) 0.0330 1.0000 Uani . . . . . .
F58 F 1.0015(3) 0.52807(16) 0.82156(17) 0.0466 1.0000 Uani . . . . . .
F59 F 1.0741(3) 0.53012(19) 0.9128(2) 0.0572 1.0000 Uani . . . . . .
C60 C 1.0163(3) 0.6490(2) 0.8715(2) 0.0269 1.0000 Uani . . . . . .
C61 C 0.9822(3) 0.6864(2) 0.8139(2) 0.0211 1.0000 Uani . . . . . .
C62 C 0.9949(3) 0.7650(2) 0.7978(2) 0.0195 1.0000 Uani . . . . . .
C63 C 1.0412(3) 0.8034(2) 0.8458(2) 0.0255 1.0000 Uani . . . . . .
C64 C 1.0735(3) 0.7669(3) 0.9043(2) 0.0308 1.0000 Uani . . . . . .
C65 C 1.0628(3) 0.6889(3) 0.9173(2) 0.0314 1.0000 Uani . . . . . .
C66 C 1.1265(4) 0.8124(4) 0.9509(3) 0.0440 1.0000 Uani . . . . . .
F67 F 1.0658(3) 0.8763(2) 0.9792(2) 0.0586 1.0000 Uani . . . . . .
F68 F 1.1338(4) 0.7751(2) 1.0144(2) 0.0704 1.0000 Uani . . . . . .
F69 F 1.2257(3) 0.8357(4) 0.9069(2) 0.1082 1.0000 Uani . . . . . .
B70 B 0.9535(3) 0.8123(2) 0.7320(2) 0.0189 1.0000 Uani . . . . . .
C71 C 1.0454(3) 0.8753(2) 0.6846(2) 0.0213 1.0000 Uani . . . . . .
C72 C 1.1597(3) 0.8645(2) 0.6717(2) 0.0253 1.0000 Uani . . . . . .
C73 C 1.2388(3) 0.9164(2) 0.6277(2) 0.0263 1.0000 Uani . . . . . .
C74 C 1.2066(4) 0.9810(3) 0.5957(3) 0.0357 1.0000 Uani . . . . . .
C75 C 1.0945(4) 0.9922(3) 0.6065(3) 0.0428 1.0000 Uani . . . . . .
C76 C 1.0155(4) 0.9411(2) 0.6498(3) 0.0323 1.0000 Uani . . . . . .
C77 C 1.0624(3) 1.06365(19) 0.5711(3) 0.0851 1.0000 Uani D . . . . .
C81 C 1.3586(3) 0.9013(2) 0.6196(2) 0.0293 1.0000 Uani . . . . . .
F82 F 1.4281(2) 0.94869(18) 0.56800(18) 0.0458 1.0000 Uani . . . . . .
F83 F 1.3758(2) 0.90893(17) 0.68825(16) 0.0382 1.0000 Uani . . . . . .
F84 F 1.3944(2) 0.83017(17) 0.59581(19) 0.0452 1.0000 Uani . . . . . .
C85 C 0.8341(3) 0.8536(2) 0.7838(2) 0.0216 1.0000 Uani . . . . . .
C86 C 0.7301(3) 0.8207(2) 0.7978(2) 0.0238 1.0000 Uani . . . . . .
C87 C 0.6304(3) 0.8544(2) 0.8453(2) 0.0268 1.0000 Uani . . . . . .
C88 C 0.6295(3) 0.9226(3) 0.8832(3) 0.0312 1.0000 Uani . . . . . .
C89 C 0.7303(4) 0.9552(2) 0.8724(3) 0.0307 1.0000 Uani . . . . . .
C90 C 0.8303(3) 0.9223(2) 0.8227(2) 0.0271 1.0000 Uani . . . . . .
C91 C 0.7343(3) 1.02699(17) 0.9137(2) 0.0536 1.0000 Uani D . . . . .
C95 C 0.52162(19) 0.81864(18) 0.8570(2) 0.0420 1.0000 Uani D . . . . .
C99 C 0.9422(3) 0.7567(2) 0.6630(2) 0.0192 1.0000 Uani . . . . . .
C100 C 1.0165(3) 0.6947(2) 0.6344(2) 0.0211 1.0000 Uani . . . . . .
C101 C 1.0093(3) 0.6480(2) 0.5753(2) 0.0235 1.0000 Uani . . . . . .
C104 C 0.8621(3) 0.7709(2) 0.6255(2) 0.0231 1.0000 Uani . . . . . .
C105 C 0.7690(2) 0.73668(17) 0.52796(19) 0.0409 1.0000 Uani D . . . . .
C109 C 1.0872(3) 0.5801(3) 0.5507(3) 0.0296 1.0000 Uani . . . . . .
F110 F 1.0485(3) 0.51780(16) 0.5962(2) 0.0513 1.0000 Uani . . . . . .
F111 F 1.1883(2) 0.59083(16) 0.55562(17) 0.0364 1.0000 Uani . . . . . .
F112 F 1.1042(3) 0.5593(2) 0.47689(19) 0.0543 1.0000 Uani . . . . . .
C114 C 0.9274(3) 0.6613(2) 0.5414(2) 0.0245 1.0000 Uani . . . . . .
C115 C 0.8548(3) 0.7240(2) 0.5666(2) 0.0246 1.0000 Uani . . . . . .
F200 F 0.6921(3) 0.6835(3) 0.5480(3) 0.0595 0.801(9) Uani D . P 1 1 .
F201 F 0.7123(4) 0.8029(2) 0.5454(3) 0.0506 0.801(9) Uani D . P 1 1 .
F202 F 0.8110(4) 0.7358(3) 0.4496(2) 0.0535 0.801(9) Uani D . P 1 1 .
F210 F 0.7699(14) 0.7038(8) 0.4635(7) 0.0522 0.199(9) Uani D . P 1 2 .
F211 F 0.6748(7) 0.7153(10) 0.5837(7) 0.0502 0.199(9) Uani D . P 1 2 .
F212 F 0.7534(13) 0.8108(4) 0.5160(10) 0.0426 0.199(9) Uani D . P 1 2 .
F300 F 0.6385(5) 1.0412(5) 0.9728(5) 0.0601 0.523(15) Uani D . P 2 1 .
F301 F 0.7501(11) 1.0875(4) 0.8661(4) 0.0766 0.523(15) Uani D . P 2 1 .
F302 F 0.8143(7) 1.0263(5) 0.9452(6) 0.0636 0.523(15) Uani D . P 2 1 .
F310 F 0.6368(5) 1.0643(6) 0.9448(7) 0.0682 0.477(15) Uani D . P 2 2 .
F311 F 0.8034(10) 1.0770(4) 0.8661(4) 0.0689 0.477(15) Uani D . P 2 2 .
F312 F 0.7728(10) 1.0121(5) 0.9730(5) 0.0618 0.477(15) Uani D . P 2 2 .
F400 F 1.1221(5) 1.0720(3) 0.4929(3) 0.0926 0.845(8) Uani D . P 3 1 .
F401 F 1.0790(5) 1.1273(2) 0.6070(3) 0.0897 0.845(8) Uani D . P 3 1 .
F402 F 0.9549(4) 1.0663(3) 0.5773(4) 0.1095 0.845(8) Uani D . P 3 1 .
F410 F 1.1502(13) 1.0991(12) 0.5189(13) 0.0910 0.155(8) Uani D . P 3 2 .
F411 F 1.007(2) 1.1159(10) 0.6248(10) 0.0906 0.155(8) Uani D . P 3 2 .
F412 F 0.9934(19) 1.0471(13) 0.5312(15) 0.0889 0.155(8) Uani D . P 3 2 .
F500 F 0.5351(4) 0.7457(3) 0.8321(5) 0.0504 0.644(18) Uani D . P 4 1 .
F501 F 0.4580(5) 0.8546(5) 0.8201(5) 0.0557 0.644(18) Uani D . P 4 1 .
F502 F 0.4587(6) 0.8156(5) 0.9335(3) 0.0488 0.644(18) Uani D . P 4 1 .
F510 F 0.5237(7) 0.7660(8) 0.8047(7) 0.0549 0.356(18) Uani D . P 4 2 .
F511 F 0.4508(7) 0.8754(5) 0.8482(9) 0.0427 0.356(18) Uani D . P 4 2 .
F512 F 0.4715(8) 0.7873(8) 0.9274(5) 0.0469 0.356(18) Uani D . P 4 2 .
B600 B 0.3469(9) 0.6962(7) 0.2596(7) 0.039(3) 0.570(19) Uiso . . P 5 1 .
N601 N 0.2429(7) 0.7044(6) 0.2770(6) 0.054(3) 0.570(19) Uiso D . P 5 1 .
C602 C 0.1812(11) 0.7824(7) 0.2823(8) 0.063(3) 0.570(19) Uiso D . P 5 1 .
C603 C 0.1597(10) 0.6432(7) 0.2857(8) 0.060(3) 0.570(19) Uiso D . P 5 1 .
B610 B 0.3638(11) 0.7218(9) 0.2316(9) 0.038(3) 0.430(19) Uiso . . P 5 2 .
N611 N 0.2545(13) 0.7362(10) 0.2979(11) 0.078(5) 0.430(19) Uiso D . P 5 2 .
C612 C 0.1735(18) 0.6725(13) 0.3049(15) 0.093(7) 0.430(19) Uiso D . P 5 2 .
C613 C 0.209(2) 0.8140(12) 0.2781(14) 0.087(6) 0.430(19) Uiso D . P 5 2 .
H12 H 0.5973 0.6093 0.2364 0.0364 1.0000 Uiso R . . . . .
H11 H 0.6348 0.7044 0.2352 0.0433 1.0000 Uiso R . . . . .
H41 H 0.5105 0.7188 0.5091 0.0309 1.0000 Uiso R . . . . .
H42 H 0.3826 0.6990 0.5359 0.0311 1.0000 Uiso R . . . . .
H51 H 0.5522 0.5924 0.4970 0.0299 1.0000 Uiso R . . . . .
H52 H 0.4253 0.5747 0.5103 0.0299 1.0000 Uiso R . . . . .
H91 H 0.3160 0.4512 0.3717 0.0444 1.0000 Uiso R . . . . .
H92 H 0.3285 0.5083 0.4324 0.0449 1.0000 Uiso R . . . . .
H93 H 0.3414 0.5361 0.3476 0.0448 1.0000 Uiso R . . . . .
H101 H 0.4728 0.3695 0.3162 0.0261 1.0000 Uiso R . . . . .
H121 H 0.7854 0.4295 0.2857 0.0301 1.0000 Uiso R . . . . .
H141 H 0.8255 0.5508 0.3159 0.0470 1.0000 Uiso R . . . . .
H142 H 0.7395 0.5788 0.3957 0.0472 1.0000 Uiso R . . . . .
H143 H 0.7391 0.6172 0.3160 0.0469 1.0000 Uiso R . . . . .
H151 H 0.7547 0.3011 0.2556 0.0539 1.0000 Uiso R . . . . .
H152 H 0.6351 0.2704 0.2873 0.0539 1.0000 Uiso R . . . . .
H153 H 0.6784 0.3098 0.2044 0.0542 1.0000 Uiso R . . . . .
H181 H 0.6769 0.8547 0.3693 0.0557 1.0000 Uiso R . . . . .
H182 H 0.6447 0.7684 0.3707 0.0552 1.0000 Uiso R . . . . .
H183 H 0.6779 0.8159 0.2919 0.0555 1.0000 Uiso R . . . . .
H191 H 0.5534 0.9487 0.3152 0.0319 1.0000 Uiso R . . . . .
H211 H 0.2255 0.9199 0.4225 0.0404 1.0000 Uiso R . . . . .
H231 H 0.1546 0.7972 0.4708 0.0582 1.0000 Uiso R . . . . .
H232 H 0.2196 0.7733 0.5279 0.0581 1.0000 Uiso R . . . . .
H233 H 0.2343 0.7253 0.4532 0.0581 1.0000 Uiso R . . . . .
H241 H 0.2982 1.0269 0.3195 0.0712 1.0000 Uiso R . . . . .
H242 H 0.3445 1.0598 0.3804 0.0713 1.0000 Uiso R . . . . .
H243 H 0.4244 1.0445 0.2948 0.0713 1.0000 Uiso R . . . . .
H271 H 0.6783 0.7719 -0.0290 0.0369 1.0000 Uiso R . . . . .
H272 H 0.7828 0.7177 -0.0297 0.0373 1.0000 Uiso R . . . . .
H281 H 0.5954 0.6672 -0.0478 0.0358 1.0000 Uiso R . . . . .
H282 H 0.6878 0.6127 -0.0310 0.0359 1.0000 Uiso R . . . . .
H321 H 0.6644 0.4616 0.1447 0.0464 1.0000 Uiso R . . . . .
H322 H 0.6867 0.5465 0.1186 0.0467 1.0000 Uiso R . . . . .
H323 H 0.6972 0.4846 0.0562 0.0467 1.0000 Uiso R . . . . .
H331 H 0.4852 0.4111 0.1695 0.0329 1.0000 Uiso R . . . . .
H351 H 0.2382 0.5346 0.1297 0.0382 1.0000 Uiso R . . . . .
H371 H 0.2640 0.6619 0.0759 0.0770 1.0000 Uiso R . . . . .
H372 H 0.3759 0.7013 0.0655 0.0770 1.0000 Uiso R . . . . .
H373 H 0.3670 0.6501 -0.0008 0.0772 1.0000 Uiso R . . . . .
H381 H 0.1969 0.4305 0.2412 0.0600 1.0000 Uiso R . . . . .
H382 H 0.2975 0.3741 0.2364 0.0602 1.0000 Uiso R . . . . .
H383 H 0.2441 0.3748 0.1700 0.0601 1.0000 Uiso R . . . . .
H411 H 0.5649 0.9406 0.1011 0.0842 1.0000 Uiso R . . . . .
H412 H 0.5669 0.8625 0.0619 0.0842 1.0000 Uiso R . . . . .
H413 H 0.5082 0.8716 0.1525 0.0844 1.0000 Uiso R . . . . .
H421 H 0.7096 0.9696 0.1507 0.0590 1.0000 Uiso R . . . . .
H441 H 0.9366 0.9412 0.2145 0.1200 1.0000 Uiso R . . . . .
H442 H 0.9527 0.9832 0.1335 0.1199 1.0000 Uiso R . . . . .
H443 H 0.8482 1.0022 0.2069 0.1201 1.0000 Uiso R . . . . .
H451 H 0.9421 0.8128 0.1586 0.0539 1.0000 Uiso R . . . . .
H471 H 0.9372 0.6852 0.1239 0.0570 1.0000 Uiso R . . . . .
H472 H 0.8723 0.6705 0.0660 0.0570 1.0000 Uiso R . . . . .
H473 H 0.8142 0.6567 0.1571 0.0568 1.0000 Uiso R . . . . .
H61 H 0.9498 0.6582 0.7849 0.0250 1.0000 Uiso R . . . . .
H63 H 1.0500 0.8558 0.8383 0.0301 1.0000 Uiso R . . . . .
H65 H 1.0861 0.6643 0.9556 0.0379 1.0000 Uiso R . . . . .
H72 H 1.1848 0.8211 0.6929 0.0301 1.0000 Uiso R . . . . .
H74 H 1.2584 1.0160 0.5670 0.0430 1.0000 Uiso R . . . . .
H76 H 0.9408 0.9513 0.6559 0.0389 1.0000 Uiso R . . . . .
H86 H 0.7274 0.7747 0.7745 0.0282 1.0000 Uiso R . . . . .
H88 H 0.5628 0.9456 0.9149 0.0372 1.0000 Uiso R . . . . .
H90 H 0.8968 0.9471 0.8157 0.0318 1.0000 Uiso R . . . . .
H100 H 1.0727 0.6839 0.6559 0.0250 1.0000 Uiso R . . . . .
H104 H 0.8134 0.8133 0.6403 0.0268 1.0000 Uiso R . . . . .
H114 H 0.9210 0.6289 0.5029 0.0298 1.0000 Uiso R . . . . .
H6001 H 0.3904 0.7404 0.2490 0.0516 0.570(19) Uiso R . P 5 1 .
H6002 H 0.3822 0.6470 0.2568 0.0516 0.570(19) Uiso R . P 5 1 .
H6021 H 0.1031 0.7764 0.2963 0.0824 0.570(19) Uiso R . P 5 1 .
H6022 H 0.1956 0.8117 0.3211 0.0824 0.570(19) Uiso R . P 5 1 .
H6023 H 0.2085 0.8078 0.2326 0.0824 0.570(19) Uiso R . P 5 1 .
H6031 H 0.0874 0.6670 0.2990 0.0717 0.570(19) Uiso R . P 5 1 .
H6032 H 0.1620 0.6087 0.3268 0.0717 0.570(19) Uiso R . P 5 1 .
H6033 H 0.1758 0.6161 0.2381 0.0717 0.570(19) Uiso R . P 5 1 .
H6101 H 0.3963 0.6736 0.2388 0.0419 0.430(19) Uiso R . P 5 2 .
H6102 H 0.4131 0.7609 0.2317 0.0419 0.430(19) Uiso R . P 5 2 .
H6103 H 0.3510 0.7229 0.1826 0.0419 0.430(19) Uiso R . P 5 2 .
H6111 H 0.2712 0.7401 0.3451 0.0795 0.430(19) Uiso R . P 5 2 .
H6121 H 0.1077 0.6856 0.3475 0.1354 0.430(19) Uiso R . P 5 2 .
H6122 H 0.2054 0.6258 0.3170 0.1354 0.430(19) Uiso R . P 5 2 .
H6123 H 0.1552 0.6667 0.2585 0.1354 0.430(19) Uiso R . P 5 2 .
H6131 H 0.1395 0.8255 0.3180 0.1004 0.430(19) Uiso R . P 5 2 .
H6132 H 0.2609 0.8517 0.2774 0.1004 0.430(19) Uiso R . P 5 2 .
H6133 H 0.1988 0.8136 0.2283 0.1004 0.430(19) Uiso R . P 5 2 .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.17356(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ir1 . C2 . 2.050(3) yes
Ir1 . C25 . 2.047(4) yes
Ir1 . B600 . 2.155(10) yes
Ir1 . H12 . 1.511 no
Ir1 . H11 . 1.479 no
Ir1 . H6001 . 1.920 no
Ir1 . H6002 . 1.827 no
Ir1 . C2 . 2.050(3) yes
Ir1 . C25 . 2.047(4) yes
Ir1 . B610 . 2.186(14) yes
Ir1 . H12 . 1.511 no
Ir1 . H11 . 1.479 no
Ir1 . H6101 . 1.633 no
Ir1 . H6102 . 1.999 no
C2 . N3 . 1.341(5) yes
C2 . N6 . 1.346(5) yes
N3 . C4 . 1.478(4) yes
N3 . C16 . 1.438(4) yes
C4 . C5 . 1.536(5) yes
C4 . H41 . 0.964 no
C4 . H42 . 0.976 no
C5 . N6 . 1.475(4) yes
C5 . H51 . 0.977 no
C5 . H52 . 0.972 no
N6 . C7 . 1.435(5) yes
C7 . C8 . 1.399(5) yes
C7 . C13 . 1.394(5) yes
C8 . C9 . 1.502(5) yes
C8 . C10 . 1.397(5) yes
C9 . H91 . 0.965 no
C9 . H92 . 0.962 no
C9 . H93 . 0.951 no
C10 . C11 . 1.393(5) yes
C10 . H101 . 0.927 no
C11 . C12 . 1.393(6) yes
C11 . C15 . 1.508(5) yes
C12 . C13 . 1.389(5) yes
C12 . H121 . 0.937 no
C13 . C14 . 1.507(6) yes
C14 . H141 . 0.963 no
C14 . H142 . 0.960 no
C14 . H143 . 0.962 no
C15 . H151 . 0.956 no
C15 . H152 . 0.958 no
C15 . H153 . 0.956 no
C16 . C17 . 1.403(5) yes
C16 . C22 . 1.396(6) yes
C17 . C18 . 1.517(6) yes
C17 . C19 . 1.387(5) yes
C18 . H181 . 0.969 no
C18 . H182 . 0.965 no
C18 . H183 . 0.956 no
C19 . C20 . 1.383(6) yes
C19 . H191 . 0.934 no
C20 . C21 . 1.396(6) yes
C20 . C24 . 1.515(6) yes
C21 . C22 . 1.402(6) yes
C21 . H211 . 0.938 no
C22 . C23 . 1.505(6) yes
C23 . H231 . 0.960 no
C23 . H232 . 0.961 no
C23 . H233 . 0.966 no
C24 . H241 . 0.952 no
C24 . H242 . 0.955 no
C24 . H243 . 0.960 no
C25 . N26 . 1.347(5) yes
C25 . N29 . 1.348(5) yes
N26 . C27 . 1.485(5) yes
N26 . C39 . 1.435(5) yes
C27 . C28 . 1.530(6) yes
C27 . H271 . 0.973 no
C27 . H272 . 0.976 no
C28 . N29 . 1.473(5) yes
C28 . H281 . 0.970 no
C28 . H282 . 0.975 no
N29 . C30 . 1.439(5) yes
C30 . C31 . 1.391(6) yes
C30 . C36 . 1.399(6) yes
C31 . C32 . 1.509(6) yes
C31 . C33 . 1.388(5) yes
C32 . H321 . 0.956 no
C32 . H322 . 0.954 no
C32 . H323 . 0.965 no
C33 . C34 . 1.398(6) yes
C33 . H331 . 0.933 no
C34 . C35 . 1.383(6) yes
C34 . C38 . 1.517(6) yes
C35 . C36 . 1.391(6) yes
C35 . H351 . 0.919 no
C36 . C37 . 1.505(7) yes
C37 . H371 . 0.957 no
C37 . H372 . 0.956 no
C37 . H373 . 0.960 no
C38 . H381 . 0.963 no
C38 . H382 . 0.963 no
C38 . H383 . 0.965 no
C39 . C40 . 1.402(6) yes
C39 . C46 . 1.386(7) yes
C40 . C41 . 1.487(8) yes
C40 . C42 . 1.413(7) yes
C41 . H411 . 0.954 no
C41 . H412 . 0.959 no
C41 . H413 . 0.954 no
C42 . C43 . 1.369(9) yes
C42 . H421 . 0.927 no
C43 . C44 . 1.515(7) yes
C43 . C45 . 1.396(9) yes
C44 . H441 . 0.958 no
C44 . H442 . 0.957 no
C44 . H443 . 0.953 no
C45 . C46 . 1.390(6) yes
C45 . H451 . 0.935 no
C46 . C47 . 1.509(7) yes
C47 . H471 . 0.962 no
C47 . H472 . 0.964 no
C47 . H473 . 0.963 no
F56 . C57 . 1.348(5) yes
C57 . F58 . 1.347(6) yes
C57 . F59 . 1.330(5) yes
C57 . C60 . 1.499(6) yes
C60 . C61 . 1.391(5) yes
C60 . C65 . 1.387(6) yes
C61 . C62 . 1.405(5) yes
C61 . H61 . 0.931 no
C62 . C63 . 1.402(5) yes
C62 . B70 . 1.643(5) yes
C63 . C64 . 1.387(6) yes
C63 . H63 . 0.932 no
C64 . C65 . 1.385(7) yes
C64 . C66 . 1.507(6) yes
C65 . H65 . 0.929 no
C66 . F67 . 1.344(7) yes
C66 . F68 . 1.330(6) yes
C66 . F69 . 1.318(6) yes
B70 . C71 . 1.642(5) yes
B70 . C85 . 1.641(5) yes
B70 . C99 . 1.651(5) yes
C71 . C72 . 1.398(5) yes
C71 . C76 . 1.398(5) yes
C72 . C73 . 1.403(5) yes
C72 . H72 . 0.934 no
C73 . C74 . 1.366(6) yes
C73 . C81 . 1.495(6) yes
C74 . C75 . 1.380(7) yes
C74 . H74 . 0.930 no
C75 . C76 . 1.388(6) yes
C75 . C77 . 1.493(5) yes
C76 . H76 . 0.930 no
C77 . F400 . 1.363(5) yes
C77 . F401 . 1.367(5) yes
C77 . F402 . 1.334(4) yes
C77 . F410 . 1.353(6) yes
C77 . F411 . 1.345(6) yes
C77 . F412 . 1.355(6) yes
C81 . F82 . 1.340(5) yes
C81 . F83 . 1.339(5) yes
C81 . F84 . 1.342(5) yes
C85 . C86 . 1.408(5) yes
C85 . C90 . 1.403(5) yes
C86 . C87 . 1.388(5) yes
C86 . H86 . 0.927 no
C87 . C88 . 1.393(6) yes
C87 . C95 . 1.492(4) yes
C88 . C89 . 1.378(6) yes
C88 . H88 . 0.931 no
C89 . C90 . 1.397(6) yes
C89 . C91 . 1.494(5) yes
C90 . H90 . 0.937 no
C91 . F300 . 1.339(5) yes
C91 . F301 . 1.323(5) yes
C91 . F302 . 1.323(5) yes
C91 . F310 . 1.328(5) yes
C91 . F311 . 1.339(5) yes
C91 . F312 . 1.333(5) yes
C95 . F500 . 1.354(5) yes
C95 . F501 . 1.339(5) yes
C95 . F502 . 1.341(5) yes
C95 . F510 . 1.333(5) yes
C95 . F511 . 1.357(5) yes
C95 . F512 . 1.327(5) yes
C99 . C100 . 1.399(5) yes
C99 . C104 . 1.411(5) yes
C100 . C101 . 1.393(5) yes
C100 . H100 . 0.933 no
C101 . C109 . 1.493(6) yes
C101 . C114 . 1.385(5) yes
C104 . C115 . 1.394(5) yes
C104 . H104 . 0.932 no
C105 . C115 . 1.488(4) yes
C105 . F200 . 1.333(4) yes
C105 . F201 . 1.328(4) yes
C105 . F202 . 1.331(4) yes
C105 . C115 . 1.488(4) yes
C105 . F210 . 1.309(6) yes
C105 . F211 . 1.337(6) yes
C105 . F212 . 1.329(6) yes
C109 . F110 . 1.353(5) yes
C109 . F111 . 1.341(5) yes
C109 . F112 . 1.333(5) yes
C114 . C115 . 1.388(6) yes
C114 . H114 . 0.936 no
B600 . N601 . 1.255(13) yes
B600 . H6001 . 0.950 no
B600 . H6002 . 0.950 no
N601 . C602 . 1.537(9) yes
N601 . C603 . 1.508(9) yes
C602 . H6021 . 0.950 no
C602 . H6022 . 0.950 no
C602 . H6023 . 0.950 no
C603 . H6031 . 0.950 no
C603 . H6032 . 0.950 no
C603 . H6033 . 0.950 no
B610 . N611 . 1.51(2) yes
B610 . H6101 . 0.950 no
B610 . H6102 . 0.950 no
B610 . H6103 . 0.950 no
N611 . C612 . 1.527(10) yes
N611 . C613 . 1.540(9) yes
N611 . H6111 . 0.950 no
C612 . H6121 . 0.950 no
C612 . H6122 . 0.950 no
C612 . H6123 . 0.950 no
C613 . H6131 . 0.950 no
C613 . H6132 . 0.950 no
C613 . H6133 . 0.950 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . Ir1 . C25 . 167.86(15) yes
C2 . Ir1 . B600 . 91.6(3) yes
C25 . Ir1 . B600 . 100.4(3) yes
C2 . Ir1 . H12 . 83.7 no
C25 . Ir1 . H12 . 86.9 no
B600 . Ir1 . H12 . 133.1 no
C2 . Ir1 . H11 . 88.2 no
C25 . Ir1 . H11 . 81.6 no
B600 . Ir1 . H11 . 154.9 no
H12 . Ir1 . H11 . 71.8 no
C2 . Ir1 . H6001 . 97.2 no
C25 . Ir1 . H6001 . 94.3 no
B600 . Ir1 . H6001 . 26.2 no
H12 . Ir1 . H6001 . 159.0 no
H11 . Ir1 . H6001 . 129.2 no
C2 . Ir1 . H6002 . 88.5 no
C25 . Ir1 . H6002 . 101.6 no
B600 . Ir1 . H6002 . 26.0 no
H12 . Ir1 . H6002 . 107.1 no
H11 . Ir1 . H6002 . 176.6 no
H6001 . Ir1 . H6002 . 52.0 no
C2 . Ir1 . C25 . 167.86(15) yes
C2 . Ir1 . B610 . 105.0(4) yes
C25 . Ir1 . B610 . 87.1(4) yes
C2 . Ir1 . H12 . 83.7 no
C25 . Ir1 . H12 . 86.9 no
B610 . Ir1 . H12 . 143.9 no
C2 . Ir1 . H11 . 88.2 no
C25 . Ir1 . H11 . 81.6 no
B610 . Ir1 . H11 . 142.0 no
H12 . Ir1 . H11 . 71.8 no
C2 . Ir1 . H6101 . 100.2 no
C25 . Ir1 . H6101 . 91.2 no
B610 . Ir1 . H6101 . 23.6 no
H12 . Ir1 . H6101 . 121.1 no
H11 . Ir1 . H6101 . 165.1 no
C2 . Ir1 . H6102 . 105.6 no
C25 . Ir1 . H6102 . 84.9 no
B610 . Ir1 . H6102 . 25.8 no
H12 . Ir1 . H6102 . 167.2 no
H11 . Ir1 . H6102 . 116.6 no
H6101 . Ir1 . H6102 . 49.3 no
Ir1 . C2 . N3 . 127.7(3) yes
Ir1 . C2 . N6 . 124.9(3) yes
N3 . C2 . N6 . 107.2(3) yes
C2 . N3 . C4 . 114.0(3) yes
C2 . N3 . C16 . 124.1(3) yes
C4 . N3 . C16 . 120.9(3) yes
N3 . C4 . C5 . 101.9(3) yes
N3 . C4 . H41 . 110.7 no
C5 . C4 . H41 . 112.6 no
N3 . C4 . H42 . 110.9 no
C5 . C4 . H42 . 111.2 no
H41 . C4 . H42 . 109.5 no
C4 . C5 . N6 . 102.2(3) yes
C4 . C5 . H51 . 110.9 no
N6 . C5 . H51 . 111.6 no
C4 . C5 . H52 . 111.5 no
N6 . C5 . H52 . 110.9 no
H51 . C5 . H52 . 109.7 no
C5 . N6 . C2 . 113.9(3) yes
C5 . N6 . C7 . 119.2(3) yes
C2 . N6 . C7 . 126.8(3) yes
N6 . C7 . C8 . 119.3(3) yes
N6 . C7 . C13 . 118.9(3) yes
C8 . C7 . C13 . 121.7(3) yes
C7 . C8 . C9 . 121.6(3) yes
C7 . C8 . C10 . 118.1(3) yes
C9 . C8 . C10 . 120.3(3) yes
C8 . C9 . H91 . 111.2 no
C8 . C9 . H92 . 110.4 no
H91 . C9 . H92 . 108.0 no
C8 . C9 . H93 . 110.3 no
H91 . C9 . H93 . 108.7 no
H92 . C9 . H93 . 108.1 no
C8 . C10 . C11 . 121.7(4) yes
C8 . C10 . H101 . 118.6 no
C11 . C10 . H101 . 119.7 no
C10 . C11 . C12 . 118.2(3) yes
C10 . C11 . C15 . 120.1(4) yes
C12 . C11 . C15 . 121.7(4) yes
C11 . C12 . C13 . 122.0(4) yes
C11 . C12 . H121 . 119.2 no
C13 . C12 . H121 . 118.8 no
C7 . C13 . C12 . 118.3(4) yes
C7 . C13 . C14 . 121.1(4) yes
C12 . C13 . C14 . 120.6(4) yes
C13 . C14 . H141 . 109.2 no
C13 . C14 . H142 . 110.5 no
H141 . C14 . H142 . 108.6 no
C13 . C14 . H143 . 110.0 no
H141 . C14 . H143 . 109.1 no
H142 . C14 . H143 . 109.5 no
C11 . C15 . H151 . 109.9 no
C11 . C15 . H152 . 110.6 no
H151 . C15 . H152 . 108.0 no
C11 . C15 . H153 . 111.1 no
H151 . C15 . H153 . 108.3 no
H152 . C15 . H153 . 108.9 no
N3 . C16 . C17 . 119.9(3) yes
N3 . C16 . C22 . 118.8(3) yes
C17 . C16 . C22 . 121.3(3) yes
C16 . C17 . C18 . 122.2(4) yes
C16 . C17 . C19 . 118.2(4) yes
C18 . C17 . C19 . 119.5(4) yes
C17 . C18 . H181 . 109.7 no
C17 . C18 . H182 . 110.4 no
H181 . C18 . H182 . 109.7 no
C17 . C18 . H183 . 109.1 no
H181 . C18 . H183 . 108.9 no
H182 . C18 . H183 . 108.9 no
C17 . C19 . C20 . 122.2(4) yes
C17 . C19 . H191 . 118.7 no
C20 . C19 . H191 . 119.1 no
C19 . C20 . C21 . 118.4(4) yes
C19 . C20 . C24 . 121.1(4) yes
C21 . C20 . C24 . 120.5(4) yes
C20 . C21 . C22 . 121.5(4) yes
C20 . C21 . H211 . 119.5 no
C22 . C21 . H211 . 119.1 no
C21 . C22 . C16 . 118.1(4) yes
C21 . C22 . C23 . 120.0(4) yes
C16 . C22 . C23 . 121.9(4) yes
C22 . C23 . H231 . 110.9 no
C22 . C23 . H232 . 110.6 no
H231 . C23 . H232 . 108.9 no
C22 . C23 . H233 . 110.4 no
H231 . C23 . H233 . 107.6 no
H232 . C23 . H233 . 108.4 no
C20 . C24 . H241 . 110.8 no
C20 . C24 . H242 . 109.6 no
H241 . C24 . H242 . 108.4 no
C20 . C24 . H243 . 110.3 no
H241 . C24 . H243 . 109.0 no
H242 . C24 . H243 . 108.8 no
Ir1 . C25 . N26 . 125.1(3) yes
Ir1 . C25 . N29 . 127.2(3) yes
N26 . C25 . N29 . 107.6(3) yes
C25 . N26 . C27 . 113.2(3) yes
C25 . N26 . C39 . 127.9(3) yes
C27 . N26 . C39 . 118.8(3) yes
N26 . C27 . C28 . 102.1(3) yes
N26 . C27 . H271 . 110.5 no
C28 . C27 . H271 . 111.3 no
N26 . C27 . H272 . 110.8 no
C28 . C27 . H272 . 111.9 no
H271 . C27 . H272 . 110.0 no
C27 . C28 . N29 . 102.5(3) yes
C27 . C28 . H281 . 111.6 no
N29 . C28 . H281 . 111.5 no
C27 . C28 . H282 . 111.2 no
N29 . C28 . H282 . 110.6 no
H281 . C28 . H282 . 109.4 no
C28 . N29 . C25 . 113.5(3) yes
C28 . N29 . C30 . 121.8(3) yes
C25 . N29 . C30 . 122.8(3) yes
N29 . C30 . C31 . 119.5(4) yes
N29 . C30 . C36 . 118.6(4) yes
C31 . C30 . C36 . 121.8(4) yes
C30 . C31 . C32 . 122.0(3) yes
C30 . C31 . C33 . 118.3(4) yes
C32 . C31 . C33 . 119.7(4) yes
C31 . C32 . H321 . 110.5 no
C31 . C32 . H322 . 111.7 no
H321 . C32 . H322 . 109.2 no
C31 . C32 . H323 . 109.3 no
H321 . C32 . H323 . 107.7 no
H322 . C32 . H323 . 108.3 no
C31 . C33 . C34 . 121.3(4) yes
C31 . C33 . H331 . 119.1 no
C34 . C33 . H331 . 119.6 no
C33 . C34 . C35 . 118.4(4) yes
C33 . C34 . C38 . 120.3(4) yes
C35 . C34 . C38 . 121.3(4) yes
C34 . C35 . C36 . 122.0(4) yes
C34 . C35 . H351 . 119.2 no
C36 . C35 . H351 . 118.8 no
C30 . C36 . C35 . 117.5(4) yes
C30 . C36 . C37 . 121.8(4) yes
C35 . C36 . C37 . 120.6(4) yes
C36 . C37 . H371 . 110.9 no
C36 . C37 . H372 . 110.1 no
H371 . C37 . H372 . 109.4 no
C36 . C37 . H373 . 109.1 no
H371 . C37 . H373 . 109.1 no
H372 . C37 . H373 . 108.2 no
C34 . C38 . H381 . 110.8 no
C34 . C38 . H382 . 109.4 no
H381 . C38 . H382 . 108.7 no
C34 . C38 . H383 . 110.4 no
H381 . C38 . H383 . 109.1 no
H382 . C38 . H383 . 108.4 no
N26 . C39 . C40 . 119.1(4) yes
N26 . C39 . C46 . 118.5(4) yes
C40 . C39 . C46 . 122.3(4) yes
C39 . C40 . C41 . 122.2(4) yes
C39 . C40 . C42 . 116.6(5) yes
C41 . C40 . C42 . 121.2(5) yes
C40 . C41 . H411 . 109.5 no
C40 . C41 . H412 . 110.2 no
H411 . C41 . H412 . 108.9 no
C40 . C41 . H413 . 110.4 no
H411 . C41 . H413 . 108.6 no
H412 . C41 . H413 . 109.1 no
C40 . C42 . C43 . 122.6(5) yes
C40 . C42 . H421 . 118.1 no
C43 . C42 . H421 . 119.3 no
C42 . C43 . C44 . 120.5(6) yes
C42 . C43 . C45 . 118.6(4) yes
C44 . C43 . C45 . 120.9(6) yes
C43 . C44 . H441 . 109.8 no
C43 . C44 . H442 . 109.6 no
H441 . C44 . H442 . 110.0 no
C43 . C44 . H443 . 109.1 no
H441 . C44 . H443 . 109.1 no
H442 . C44 . H443 . 109.3 no
C43 . C45 . C46 . 121.5(5) yes
C43 . C45 . H451 . 119.1 no
C46 . C45 . H451 . 119.4 no
C45 . C46 . C39 . 118.5(5) yes
C45 . C46 . C47 . 120.3(5) yes
C39 . C46 . C47 . 121.2(4) yes
C46 . C47 . H471 . 110.2 no
C46 . C47 . H472 . 109.3 no
H471 . C47 . H472 . 109.0 no
C46 . C47 . H473 . 109.5 no
H471 . C47 . H473 . 109.6 no
H472 . C47 . H473 . 109.3 no
F56 . C57 . F58 . 105.2(4) yes
F56 . C57 . F59 . 106.6(3) yes
F58 . C57 . F59 . 106.5(4) yes
F56 . C57 . C60 . 112.0(4) yes
F58 . C57 . C60 . 112.6(3) yes
F59 . C57 . C60 . 113.3(4) yes
C57 . C60 . C61 . 119.8(4) yes
C57 . C60 . C65 . 119.4(4) yes
C61 . C60 . C65 . 120.7(4) yes
C60 . C61 . C62 . 122.6(4) yes
C60 . C61 . H61 . 118.7 no
C62 . C61 . H61 . 118.7 no
C61 . C62 . C63 . 115.0(3) yes
C61 . C62 . B70 . 124.6(3) yes
C63 . C62 . B70 . 120.4(3) yes
C62 . C63 . C64 . 122.8(4) yes
C62 . C63 . H63 . 118.5 no
C64 . C63 . H63 . 118.6 no
C63 . C64 . C65 . 120.8(4) yes
C63 . C64 . C66 . 119.0(4) yes
C65 . C64 . C66 . 120.1(4) yes
C60 . C65 . C64 . 118.1(4) yes
C60 . C65 . H65 . 121.2 no
C64 . C65 . H65 . 120.8 no
C64 . C66 . F67 . 111.7(4) yes
C64 . C66 . F68 . 113.1(5) yes
F67 . C66 . F68 . 104.5(4) yes
C64 . C66 . F69 . 111.8(4) yes
F67 . C66 . F69 . 105.4(5) yes
F68 . C66 . F69 . 109.9(5) yes
C62 . B70 . C71 . 110.7(3) yes
C62 . B70 . C85 . 104.3(3) yes
C71 . B70 . C85 . 111.5(3) yes
C62 . B70 . C99 . 112.5(3) yes
C71 . B70 . C99 . 105.1(3) yes
C85 . B70 . C99 . 112.8(3) yes
B70 . C71 . C72 . 122.5(3) yes
B70 . C71 . C76 . 122.1(3) yes
C72 . C71 . C76 . 115.3(3) yes
C71 . C72 . C73 . 122.5(4) yes
C71 . C72 . H72 . 119.1 no
C73 . C72 . H72 . 118.4 no
C72 . C73 . C74 . 120.8(4) yes
C72 . C73 . C81 . 118.6(4) yes
C74 . C73 . C81 . 120.6(4) yes
C73 . C74 . C75 . 117.8(4) yes
C73 . C74 . H74 . 121.3 no
C75 . C74 . H74 . 120.9 no
C74 . C75 . C76 . 121.9(4) yes
C74 . C75 . C77 . 116.2(4) yes
C76 . C75 . C77 . 121.9(4) yes
C71 . C76 . C75 . 121.8(4) yes
C71 . C76 . H76 . 119.4 no
C75 . C76 . H76 . 118.8 no
C75 . C77 . F400 . 112.7(4) yes
C75 . C77 . F401 . 111.9(4) yes
F400 . C77 . F401 . 106.51(6) yes
C75 . C77 . F402 . 112.3(3) yes
F400 . C77 . F402 . 106.51(6) yes
F401 . C77 . F402 . 106.50(6) yes
C75 . C77 . F410 . 113.7(10) yes
C75 . C77 . F411 . 113.5(10) yes
F410 . C77 . F411 . 106.51(6) yes
C75 . C77 . F412 . 109.6(10) yes
F410 . C77 . F412 . 106.51(6) yes
F411 . C77 . F412 . 106.51(6) yes
C73 . C81 . F82 . 113.2(4) yes
C73 . C81 . F83 . 111.7(3) yes
F82 . C81 . F83 . 106.3(3) yes
C73 . C81 . F84 . 112.5(3) yes
F82 . C81 . F84 . 106.7(3) yes
F83 . C81 . F84 . 106.0(4) yes
B70 . C85 . C86 . 123.2(3) yes
B70 . C85 . C90 . 121.2(3) yes
C86 . C85 . C90 . 115.3(4) yes
C85 . C86 . C87 . 122.5(4) yes
C85 . C86 . H86 . 119.3 no
C87 . C86 . H86 . 118.2 no
C86 . C87 . C88 . 120.8(4) yes
C86 . C87 . C95 . 120.8(4) yes
C88 . C87 . C95 . 118.5(4) yes
C87 . C88 . C89 . 118.1(4) yes
C87 . C88 . H88 . 121.0 no
C89 . C88 . H88 . 120.9 no
C88 . C89 . C90 . 121.0(4) yes
C88 . C89 . C91 . 120.2(4) yes
C90 . C89 . C91 . 118.8(4) yes
C85 . C90 . C89 . 122.3(4) yes
C85 . C90 . H90 . 119.4 no
C89 . C90 . H90 . 118.3 no
C89 . C91 . F300 . 111.6(4) yes
C89 . C91 . F301 . 112.3(4) yes
F300 . C91 . F301 . 106.17(6) yes
C89 . C91 . F302 . 113.9(4) yes
F300 . C91 . F302 . 106.17(6) yes
F301 . C91 . F302 . 106.19(6) yes
C89 . C91 . F310 . 115.2(4) yes
C89 . C91 . F311 . 112.2(4) yes
F310 . C91 . F311 . 106.17(6) yes
C89 . C91 . F312 . 110.4(5) yes
F310 . C91 . F312 . 106.17(6) yes
F311 . C91 . F312 . 106.14(6) yes
C87 . C95 . F500 . 112.3(3) yes
C87 . C95 . F501 . 114.9(3) yes
F500 . C95 . F501 . 105.92(6) yes
C87 . C95 . F502 . 111.3(4) yes
F500 . C95 . F502 . 105.86(6) yes
F501 . C95 . F502 . 105.94(6) yes
C87 . C95 . F510 . 115.5(4) yes
C87 . C95 . F511 . 106.4(5) yes
F510 . C95 . F511 . 105.93(6) yes
C87 . C95 . F512 . 116.3(6) yes
F510 . C95 . F512 . 105.95(6) yes
F511 . C95 . F512 . 105.91(6) yes
B70 . C99 . C100 . 121.8(3) yes
B70 . C99 . C104 . 122.6(3) yes
C100 . C99 . C104 . 115.5(3) yes
C99 . C100 . C101 . 122.6(3) yes
C99 . C100 . H100 . 118.9 no
C101 . C100 . H100 . 118.6 no
C100 . C101 . C109 . 119.8(3) yes
C100 . C101 . C114 . 121.0(4) yes
C109 . C101 . C114 . 119.2(3) yes
C99 . C104 . C115 . 121.9(4) yes
C99 . C104 . H104 . 118.9 no
C115 . C104 . H104 . 119.2 no
C115 . C105 . F200 . 112.6(3) yes
C115 . C105 . F201 . 113.8(3) yes
F200 . C105 . F201 . 105.48(6) yes
C115 . C105 . F202 . 113.5(3) yes
F200 . C105 . F202 . 105.27(6) yes
F201 . C105 . F202 . 105.37(6) yes
C115 . C105 . F210 . 125.4(6) yes
C115 . C105 . F211 . 103.3(6) yes
F210 . C105 . F211 . 105.38(6) yes
C115 . C105 . F212 . 110.4(6) yes
F210 . C105 . F212 . 105.37(6) yes
F211 . C105 . F212 . 105.34(6) yes
C101 . C109 . F110 . 112.2(4) yes
C101 . C109 . F111 . 113.1(3) yes
F110 . C109 . F111 . 105.6(4) yes
C101 . C109 . F112 . 113.3(4) yes
F110 . C109 . F112 . 105.5(4) yes
F111 . C109 . F112 . 106.5(3) yes
C101 . C114 . C115 . 117.8(3) yes
C101 . C114 . H114 . 121.0 no
C115 . C114 . H114 . 121.1 no
C105 . C115 . C104 . 122.7(4) yes
C105 . C115 . C114 . 116.1(3) yes
C104 . C115 . C114 . 121.2(3) yes
Ir1 . B600 . N601 . 174.1(10) yes
Ir1 . B600 . H6001 . 63.0 no
N601 . B600 . H6001 . 118.6 no
Ir1 . B600 . H6002 . 57.4 no
N601 . B600 . H6002 . 121.4 no
H6001 . B600 . H6002 . 120.0 no
B600 . N601 . C602 . 123.6(10) yes
B600 . N601 . C603 . 127.7(10) yes
C602 . N601 . C603 . 108.2(9) yes
N601 . C602 . H6021 . 110.7 no
N601 . C602 . H6022 . 108.8 no
H6021 . C602 . H6022 . 109.5 no
N601 . C602 . H6023 . 108.9 no
H6021 . C602 . H6023 . 109.5 no
H6022 . C602 . H6023 . 109.5 no
N601 . C603 . H6031 . 108.2 no
N601 . C603 . H6032 . 109.2 no
H6031 . C603 . H6032 . 109.5 no
N601 . C603 . H6033 . 111.1 no
H6031 . C603 . H6033 . 109.5 no
H6032 . C603 . H6033 . 109.5 no
Ir1 . B610 . N611 . 127.1(12) yes
Ir1 . B610 . H6101 . 43.5 no
N611 . B610 . H6101 . 110.4 no
Ir1 . B610 . H6102 . 66.1 no
N611 . B610 . H6102 . 108.4 no
H6101 . B610 . H6102 . 109.5 no
Ir1 . B610 . H6103 . 122.0 no
N611 . B610 . H6103 . 109.6 no
H6101 . B610 . H6103 . 109.5 no
H6102 . B610 . H6103 . 109.5 no
B610 . N611 . C612 . 111.4(15) yes
B610 . N611 . C613 . 105.3(15) yes
C612 . N611 . C613 . 112.3(16) yes
B610 . N611 . H6111 . 107.5 no
C612 . N611 . H6111 . 111.0 no
C613 . N611 . H6111 . 109.1 no
N611 . C612 . H6121 . 106.1 no
N611 . C612 . H6122 . 108.9 no
H6121 . C612 . H6122 . 109.5 no
N611 . C612 . H6123 . 113.3 no
H6121 . C612 . H6123 . 109.5 no
H6122 . C612 . H6123 . 109.5 no
N611 . C613 . H6131 . 108.6 no
N611 . C613 . H6132 . 108.4 no
H6131 . C613 . H6132 . 109.5 no
N611 . C613 . H6133 . 111.4 no
H6131 . C613 . H6133 . 109.5 no
H6132 . C613 . H6133 . 109.5 no
Ir1 . H6001 . B600 . 90.9 no
Ir1 . H6002 . B600 . 96.7 no
Ir1 . H6101 . B610 . 112.9 no
Ir1 . H6102 . B610 . 88.2 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
N611 . H6111 . C22 . 144.5 0.950 2.356 3.178(7) yes
N611 . H6111 . C23 . 151.3 0.950 2.290 3.156(7) yes
_database_code_depnum_ccdc_archive 'CCDC 1002307'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_11-and-12(Neutron)
#==============================================================================
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 . 
;
_chemical_name_common            .
_chemical_melting_point          'not measured'
_chemical_formula_moiety         
'0.65(C44 H62 B Ir N5), 0.35(C44 H64 B Ir N5), C32 H12 B F24'
_chemical_formula_sum            'C76 H74.70 B2 F24 Ir N5'
_chemical_formula_weight         1727.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ir Ir 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0000 -0.2130 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0000 0.0000 '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'
N N 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.689(3)
_cell_length_b                   17.5549(16)
_cell_length_c                   17.948(4)
_cell_angle_alpha                88.275(19)
_cell_angle_beta                 70.175(17)
_cell_angle_gamma                87.82(2)
_cell_volume                     3757.7(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1100
_cell_measurement_theta_min      .
_cell_measurement_theta_max      .

_exptl_crystal_description       block
_exptl_crystal_colour            clear_intense_yellow
_exptl_crystal_size_max          6.0
_exptl_crystal_size_mid          3.0
_exptl_crystal_size_min          2.0
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             859
_exptl_absorpt_coefficient_mu    '3.59353 + 0.589577 * lambda'
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.4149
_exptl_absorpt_correction_T_max  0.7174
_exptl_absorpt_process_details   
;
Calculated using custom ISIS software program SXD-2001.
;
_exptl_special_details           
;
For peak integration a local UB matrix refined for each frame,
using approximately 100 reflections per run from each of the 11 detectors.
Hence _cell_measurement_reflns_used      1100
For final cell dimensions a weighted average of all local
cells was calculated.
Because of the nature of the experiment, it is not possible to give values of
theta_min and theta_max for the cell determination.
The same applies for the wavelength used for the experiment.
The range of wavelengths used was 0.48-7.0 Angstroms,
but the bulk of the diffraction information is obtained from
wavelengths in the range 0.7-2.5 Angstroms.
The data collection procedures on the SXD instrument used
for the single crystal neutron data collection are most
recently summarised in the Appendix to the following paper
Wilson, C.C. (1997).  J. Mol. Struct. 405, 207-217
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     Laue
_diffrn_radiation_type           Neutron
_diffrn_radiation_source         'ISIS spallation neutron source'
_diffrn_radiation_monochromator  none
_diffrn_measurement_device_type  'SXD at ISIS neutron source'
_diffrn_measurement_method       'time-of-flight Laue diffraction'
_diffrn_detector_area_resol_mean .
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7639
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1570
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         9.17
_diffrn_reflns_theta_max         84.73
_reflns_number_total             7639
_reflns_number_gt                6529
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       SXD2001
_computing_cell_refinement       SXD2001
_computing_data_reduction        SXD2001
_computing_structure_solution    'Refinement of known model'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    .
_computing_publication_material  .

_refine_special_details          
; 
Refining hydrogen atoms using isotropic displacement parameters leads to
a poor data to parameter ratio.  The nature of the sample, time constraints
and other experimental considerations meant it was not possible to collect
more data, so extensive restraints were used.  Thermal similarity and 
vibrational restraints were used to maintain sensible displacement ellipsoids;
same distance restraints were also used to maintain sensible geometries for
the methyl groups
.


Refinement of F² against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F², conventional R-factors R are based 
on F, with F set to zero for negative F². The threshold expression of 
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F² are statistically about twice as large as those based on F, and R- 
factors based on ALL data will be even larger. 

The variable wavelength nature of the data collection
procedure means that sensible values of
_diffrn_reflns_theta_min & _diffrn_reflns_theta_max
cannot be given.

_refine_diff_density_max/min is given in Fermi per per angstrom cubed not
electons per angstrom cubed. Another way to consider the _refine_diff_density_
is as a percentage of the diffracted intensity of a given atom:
_refine_diff_density_max =  12% of Carbon
_refine_diff_density_min = -12% of Carbon
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1436P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.000536(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7639
_refine_ls_number_parameters     1480
_refine_ls_number_restraints     4446
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0937
_refine_ls_wR_factor_ref         0.2162
_refine_ls_wR_factor_gt          0.2053
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      0.879
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.002

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.5215(4) 0.6793(2) 0.2419(2) 0.0109(11) Uani 1 1 d U . .
C2 C 0.4902(6) 0.6645(4) 0.3603(3) 0.0102(15) Uani 1 1 d U B .
N3 N 0.4541(4) 0.7176(3) 0.4172(2) 0.0124(12) Uani 1 1 d U . .
C4 C 0.4552(7) 0.6908(4) 0.4961(3) 0.0138(12) Uani 1 1 d U B .
C5 C 0.4874(7) 0.6066(4) 0.4811(3) 0.0138(12) Uani 1 1 d U . .
N6 N 0.5146(5) 0.6008(3) 0.3949(2) 0.0145(12) Uani 1 1 d U B .
C7 C 0.5549(6) 0.5291(4) 0.3582(3) 0.0103(14) Uani 1 1 d U . .
C8 C 0.4789(6) 0.4762(4) 0.3517(3) 0.0103(14) Uani 1 1 d U B .
C9 C 0.3562(6) 0.4946(4) 0.3782(4) 0.0174(19) Uani 1 1 d DU . .
C10 C 0.5201(6) 0.4058(4) 0.3198(4) 0.0155(16) Uani 1 1 d U . .
C11 C 0.6342(6) 0.3881(4) 0.2942(4) 0.0144(16) Uani 1 1 d U B .
C12 C 0.7075(6) 0.4415(4) 0.3010(4) 0.0130(16) Uani 1 1 d U . .
C13 C 0.6711(6) 0.5130(4) 0.3336(4) 0.0111(15) Uani 1 1 d U B .
C14 C 0.7492(8) 0.5719(5) 0.3398(5) 0.019(2) Uani 1 1 d U . .
C15 C 0.6787(6) 0.3125(4) 0.2553(3) 0.020(2) Uani 1 1 d DU . .
C16 C 0.4300(6) 0.7961(4) 0.4026(3) 0.0110(14) Uani 1 1 d U B .
C17 C 0.5209(6) 0.8436(4) 0.3660(3) 0.0111(14) Uani 1 1 d U . .
C18 C 0.6421(7) 0.8194(4) 0.3507(4) 0.0205(18) Uani 1 1 d DU B .
C19 C 0.4971(7) 0.9176(4) 0.3451(4) 0.0161(15) Uani 1 1 d U B .
C20 C 0.3858(7) 0.9453(4) 0.3623(4) 0.0177(16) Uani 1 1 d U . .
C21 C 0.2988(8) 0.8969(4) 0.4062(4) 0.0221(18) Uani 1 1 d U B .
C22 C 0.3210(6) 0.8220(4) 0.4255(4) 0.0180(17) Uani 1 1 d U . .
C23 C 0.2237(6) 0.7749(4) 0.4713(4) 0.028(2) Uani 1 1 d DU B .
C24 C 0.3609(7) 1.0253(4) 0.3378(4) 0.029(2) Uani 1 1 d DU B .
C25 C 0.5879(6) 0.6882(4) 0.1213(3) 0.0103(16) Uani 1 1 d U B .
N26 N 0.6703(4) 0.7342(3) 0.0803(2) 0.0156(12) Uani 1 1 d U . .
C27 C 0.7012(7) 0.7284(5) -0.0058(4) 0.0204(18) Uani 1 1 d U B .
C28 C 0.6393(7) 0.6574(4) -0.0140(4) 0.0177(18) Uani 1 1 d U . .
N29 N 0.5643(5) 0.6446(3) 0.0677(2) 0.0153(13) Uani 1 1 d U B .
C30 C 0.4957(6) 0.5803(4) 0.0909(3) 0.0134(14) Uani 1 1 d U . .
C31 C 0.5347(6) 0.5143(4) 0.1162(3) 0.0129(14) Uani 1 1 d U B .
C32 C 0.6569(6) 0.5013(4) 0.1070(3) 0.0188(17) Uani 1 1 d DU . .
C33 C 0.4586(7) 0.4570(4) 0.1509(3) 0.0163(16) Uani 1 1 d U . .
C34 C 0.3460(6) 0.4650(4) 0.1612(4) 0.0162(16) Uani 1 1 d U B .
C35 C 0.3100(7) 0.5298(4) 0.1274(4) 0.0201(17) Uani 1 1 d U . .
C36 C 0.3835(7) 0.5882(4) 0.0911(4) 0.0179(15) Uani 1 1 d U B .
C37 C 0.3436(7) 0.6567(5) 0.0563(5) 0.040(2) Uani 1 1 d DU . .
C38 C 0.2654(6) 0.4054(4) 0.2069(3) 0.027(2) Uani 1 1 d DU . .
C39 C 0.7211(7) 0.7918(4) 0.1108(3) 0.0174(14) Uani 1 1 d U B .
C40 C 0.6733(7) 0.8660(4) 0.1212(4) 0.0232(16) Uani 1 1 d U . .
C41 C 0.5640(8) 0.8850(4) 0.1093(4) 0.037(2) Uani 1 1 d DU B .
C42 C 0.7300(8) 0.9227(5) 0.1449(4) 0.0307(18) Uani 1 1 d U B .
C43 C 0.8301(8) 0.9043(5) 0.1575(4) 0.033(2) Uani 1 1 d U . .
C44 C 0.8913(7) 0.9668(5) 0.1806(4) 0.051(3) Uani 1 1 d DU B .
C45 C 0.8722(8) 0.8309(5) 0.1486(4) 0.0292(19) Uani 1 1 d U B .
C46 C 0.8201(7) 0.7733(4) 0.1252(4) 0.0201(16) Uani 1 1 d U . .
C47 C 0.8650(9) 0.6923(5) 0.1175(5) 0.029(2) Uani 1 1 d U B .
F56 F 0.8995(9) 0.5487(6) 0.9422(5) 0.037(3) Uani 1 1 d U . .
C57 C 0.9982(7) 0.5651(5) 0.8878(4) 0.0244(18) Uani 1 1 d U . .
F58 F 0.9999(10) 0.5273(6) 0.8221(5) 0.039(3) Uani 1 1 d U . .
F59 F 1.0734(11) 0.5286(6) 0.9119(6) 0.043(3) Uani 1 1 d U . .
C60 C 1.0169(6) 0.6480(4) 0.8728(4) 0.0170(15) Uani 1 1 d U . .
C61 C 0.9826(6) 0.6853(4) 0.8136(3) 0.0126(15) Uani 1 1 d U . .
C62 C 0.9972(6) 0.7636(4) 0.7978(3) 0.0122(13) Uani 1 1 d U . .
C63 C 1.0424(6) 0.8024(4) 0.8454(3) 0.0180(16) Uani 1 1 d U . .
C64 C 1.0743(7) 0.7660(5) 0.9048(4) 0.0236(16) Uani 1 1 d U . .
C65 C 1.0637(7) 0.6869(5) 0.9181(4) 0.0223(17) Uani 1 1 d U . .
C66 C 1.1268(8) 0.8110(5) 0.9508(4) 0.033(2) Uani 1 1 d U . .
F67 F 1.0703(11) 0.8755(7) 0.9780(6) 0.046(3) Uani 1 1 d U . .
F68 F 1.1314(12) 0.7740(8) 1.0157(6) 0.053(3) Uani 1 1 d U . .
F69 F 1.2267(11) 0.8337(9) 0.9081(6) 0.072(4) Uani 1 1 d U . .
B70 B 0.9564(7) 0.8102(5) 0.7304(4) 0.0098(14) Uani 1 1 d U . .
C71 C 1.0475(6) 0.8742(4) 0.6831(4) 0.0121(15) Uani 1 1 d U . .
C72 C 1.1620(6) 0.8627(4) 0.6705(4) 0.0148(16) Uani 1 1 d U . .
C73 C 1.2427(6) 0.9138(4) 0.6268(4) 0.0145(14) Uani 1 1 d U . .
C74 C 1.2113(6) 0.9789(4) 0.5941(4) 0.0177(16) Uani 1 1 d U . .
C75 C 1.0981(7) 0.9911(4) 0.6042(5) 0.0273(17) Uani 1 1 d U . .
C76 C 1.0184(7) 0.9380(4) 0.6486(4) 0.0180(16) Uani 1 1 d U . .
C77 C 1.0634(9) 1.0638(5) 0.5703(6) 0.048(2) Uani 1 1 d U . .
C81 C 1.3632(6) 0.8992(4) 0.6193(4) 0.0163(15) Uani 1 1 d U . .
F82 F 1.4317(8) 0.9458(6) 0.5664(5) 0.029(3) Uani 1 1 d U . .
F83 F 1.3782(7) 0.9075(5) 0.6882(5) 0.020(2) Uani 1 1 d U . .
F84 F 1.3978(8) 0.8283(5) 0.5952(5) 0.026(2) Uani 1 1 d U . .
C85 C 0.8366(6) 0.8523(4) 0.7829(3) 0.0135(15) Uani 1 1 d U . .
C86 C 0.7315(6) 0.8197(4) 0.7959(3) 0.0153(16) Uani 1 1 d U . .
C87 C 0.6303(6) 0.8533(4) 0.8442(4) 0.0170(16) Uani 1 1 d U . .
C88 C 0.6306(7) 0.9211(4) 0.8829(4) 0.0195(18) Uani 1 1 d U . .
C89 C 0.7332(6) 0.9530(4) 0.8712(4) 0.0211(17) Uani 1 1 d U A .
C90 C 0.8326(6) 0.9218(4) 0.8211(4) 0.0167(17) Uani 1 1 d U . .
C91 C 0.7367(7) 1.0257(4) 0.9111(4) 0.031(2) Uani 1 1 d DU . .
C95 C 0.5225(7) 0.8173(5) 0.8567(5) 0.032(2) Uani 1 1 d U . .
C99 C 0.9450(6) 0.7547(4) 0.6619(3) 0.0106(14) Uani 1 1 d U . .
C100 C 1.0189(7) 0.6923(4) 0.6349(4) 0.0145(15) Uani 1 1 d U . .
C101 C 1.0118(6) 0.6453(4) 0.5754(3) 0.0143(14) Uani 1 1 d U . .
C104 C 0.8633(6) 0.7698(4) 0.6241(3) 0.0118(14) Uani 1 1 d U . .
C105 C 0.7701(7) 0.7360(5) 0.5273(4) 0.0238(16) Uani 1 1 d U . .
C109 C 1.0874(7) 0.5773(4) 0.5522(4) 0.0203(16) Uani 1 1 d U . .
F110 F 1.0456(10) 0.5182(6) 0.5976(6) 0.043(3) Uani 1 1 d U . .
F111 F 1.1880(8) 0.5893(6) 0.5558(5) 0.031(2) Uani 1 1 d U . .
F112 F 1.1043(9) 0.5554(6) 0.4783(5) 0.032(3) Uani 1 1 d U . .
C114 C 0.9298(7) 0.6596(4) 0.5408(4) 0.0175(15) Uani 1 1 d U . .
C115 C 0.8578(6) 0.7229(4) 0.5651(4) 0.0163(14) Uani 1 1 d U . .
F200 F 0.6963(11) 0.6805(7) 0.5446(8) 0.054(3) Uani 1 1 d U . .
F201 F 0.7157(11) 0.8028(7) 0.5423(7) 0.048(3) Uani 1 1 d U . .
F202 F 0.8146(11) 0.7350(8) 0.4484(6) 0.050(3) Uani 1 1 d U . .
F300 F 0.6402(13) 1.0385(11) 0.9720(11) 0.040(4) Uani 0.67(2) 1 d PDU A 1
F301 F 0.752(2) 1.0852(8) 0.8607(9) 0.047(4) Uani 0.67(2) 1 d PDU A 1
F302 F 0.8155(16) 1.0199(10) 0.9451(12) 0.046(4) Uani 0.67(2) 1 d PDU A 1
F310 F 0.641(2) 1.068(2) 0.940(3) 0.040(5) Uani 0.33(2) 1 d PDU A 2
F311 F 0.818(3) 1.0759(18) 0.877(2) 0.039(6) Uani 0.33(2) 1 d PDU A 2
F312 F 0.762(3) 1.016(2) 0.9775(14) 0.039(4) Uani 0.33(2) 1 d PDU A 2
F400 F 1.1288(12) 1.0746(8) 0.4962(8) 0.072(4) Uani 1 1 d U . .
F401 F 1.0765(14) 1.1229(8) 0.6082(10) 0.086(4) Uani 1 1 d U . .
F402 F 0.9578(13) 1.0646(9) 0.5738(10) 0.093(4) Uani 1 1 d U . .
F500 F 0.5342(11) 0.7492(7) 0.8246(8) 0.065(4) Uani 1 1 d U . .
F501 F 0.4579(10) 0.8605(8) 0.8278(8) 0.063(3) Uani 1 1 d U . .
F502 F 0.4637(9) 0.8060(7) 0.9319(6) 0.051(3) Uani 1 1 d U . .
B600 B 0.3539(16) 0.6953(12) 0.2553(10) 0.029(3) Uiso 0.650(13) 1 d PU B 1
N601 N 0.2384(9) 0.7093(6) 0.2764(6) 0.041(2) Uiso 0.650(13) 1 d PDU B 1
C602 C 0.1795(11) 0.7866(8) 0.2822(7) 0.040(3) Uiso 0.650(13) 1 d PDU B 1
C603 C 0.1580(11) 0.6456(8) 0.2873(7) 0.041(4) Uiso 0.650(13) 1 d PDU B 1
B610 B 0.365(3) 0.726(2) 0.2277(19) 0.029(4) Uiso 0.350(13) 1 d PU B 2
N611 N 0.2529(16) 0.7409(11) 0.2964(12) 0.038(4) Uiso 0.350(13) 1 d PDU B 2
C612 C 0.174(2) 0.6743(15) 0.3038(15) 0.054(7) Uiso 0.350(13) 1 d PDU B 2
C613 C 0.206(2) 0.8159(15) 0.2758(14) 0.055(7) Uiso 0.350(13) 1 d PDU B 2
H12 H 0.6033(15) 0.6113(10) 0.2329(8) 0.041(5) Uani 1 1 d . . .
H11 H 0.6306(16) 0.7165(13) 0.2402(9) 0.059(7) Uani 1 1 d . . .
H41 H 0.5200(17) 0.7208(10) 0.5096(9) 0.040(4) Uani 1 1 d . . .
H42 H 0.3733(14) 0.7005(9) 0.5425(8) 0.034(3) Uani 1 1 d . . .
H51 H 0.5621(17) 0.5888(10) 0.4994(9) 0.040(4) Uani 1 1 d . . .
H52 H 0.4200(14) 0.5700(8) 0.5124(8) 0.034(3) Uani 1 1 d . . .
H91 H 0.312(3) 0.4579(17) 0.3513(17) 0.045(4) Uiso 0.44(2) 1 d PD C 1
H92 H 0.323(3) 0.4836(19) 0.4423(6) 0.045(4) Uiso 0.44(2) 1 d PD C 1
H93 H 0.331(3) 0.5537(8) 0.3691(19) 0.045(4) Uiso 0.44(2) 1 d PD C 1
H94 H 0.305(2) 0.4437(10) 0.3882(15) 0.045(4) Uiso 0.56(2) 1 d PD C 2
H95 H 0.320(2) 0.5302(13) 0.4305(11) 0.045(4) Uiso 0.56(2) 1 d PD C 2
H96 H 0.341(2) 0.5259(14) 0.3286(11) 0.045(4) Uiso 0.56(2) 1 d PD C 2
H101 H 0.4635(12) 0.3641(8) 0.3136(9) 0.027(3) Uani 1 1 d . . .
H121 H 0.7997(12) 0.4273(8) 0.2790(8) 0.027(3) Uani 1 1 d . . .
H141 H 0.8368(18) 0.5513(14) 0.3096(11) 0.064(7) Uani 1 1 d . . .
H142 H 0.7446(16) 0.5813(10) 0.3992(10) 0.048(6) Uani 1 1 d . . .
H143 H 0.7384(17) 0.6247(10) 0.3117(11) 0.054(6) Uani 1 1 d . . .
H151 H 0.7705(8) 0.311(3) 0.232(3) 0.040(3) Uiso 0.32(6) 1 d PD D 1
H152 H 0.653(5) 0.2651(18) 0.298(2) 0.040(3) Uiso 0.32(6) 1 d PD D 1
H153 H 0.651(5) 0.300(3) 0.206(2) 0.040(3) Uiso 0.32(6) 1 d PD D 1
H154 H 0.7612(13) 0.2958(16) 0.2579(17) 0.040(3) Uiso 0.68(6) 1 d PD D 2
H155 H 0.6221(19) 0.2657(11) 0.2817(16) 0.040(3) Uiso 0.68(6) 1 d PD D 2
H156 H 0.686(3) 0.3155(15) 0.1926(7) 0.040(3) Uiso 0.68(6) 1 d PD D 2
H181 H 0.657(4) 0.833(3) 0.4059(14) 0.044(4) Uiso 0.35(2) 1 d PD E 1
H182 H 0.677(5) 0.7597(19) 0.337(2) 0.044(4) Uiso 0.35(2) 1 d PD E 1
H183 H 0.699(5) 0.855(2) 0.3048(18) 0.044(4) Uiso 0.35(2) 1 d PD E 1
H184 H 0.683(3) 0.8596(13) 0.3755(14) 0.044(4) Uiso 0.65(2) 1 d PD E 2
H185 H 0.652(3) 0.7628(12) 0.3764(14) 0.044(4) Uiso 0.65(2) 1 d PD E 2
H186 H 0.691(2) 0.8152(15) 0.2868(10) 0.044(4) Uiso 0.65(2) 1 d PD E 2
H191 H 0.5635(15) 0.9562(10) 0.3134(10) 0.042(4) Uani 1 1 d . . .
H211 H 0.2148(16) 0.9167(10) 0.4215(10) 0.042(4) Uani 1 1 d . . .
H231 H 0.1476(18) 0.7937(18) 0.460(2) 0.040(3) Uiso 0.53(6) 1 d PD F 1
H232 H 0.207(3) 0.782(3) 0.5348(6) 0.040(3) Uiso 0.53(6) 1 d PD F 1
H233 H 0.237(2) 0.7138(7) 0.461(2) 0.040(3) Uiso 0.53(6) 1 d PD F 1
H234 H 0.1400(14) 0.8021(17) 0.485(3) 0.040(3) Uiso 0.47(6) 1 d PD F 2
H235 H 0.229(3) 0.754(3) 0.5279(15) 0.040(3) Uiso 0.47(6) 1 d PD F 2
H236 H 0.226(3) 0.7252(18) 0.435(2) 0.040(3) Uiso 0.47(6) 1 d PD F 2
H241 H 0.303(2) 1.0267(19) 0.3046(18) 0.068(5) Uiso 0.60(3) 1 d PD G 1
H242 H 0.329(3) 1.0662(15) 0.3857(13) 0.068(5) Uiso 0.60(3) 1 d PD G 1
H243 H 0.4409(16) 1.0467(18) 0.2983(16) 0.068(5) Uiso 0.60(3) 1 d PD G 1
H244 H 0.2720(12) 1.042(3) 0.354(3) 0.068(5) Uiso 0.40(3) 1 d PD G 2
H245 H 0.396(4) 1.061(2) 0.372(2) 0.068(5) Uiso 0.40(3) 1 d PD G 2
H246 H 0.401(4) 1.042(3) 0.2755(9) 0.068(5) Uiso 0.40(3) 1 d PD G 2
H271 H 0.6790(15) 0.7779(10) -0.0317(8) 0.034(3) Uani 1 1 d . . .
H272 H 0.7935(15) 0.7185(9) -0.0346(8) 0.040(4) Uani 1 1 d . . .
H281 H 0.5900(16) 0.6672(9) -0.0528(8) 0.034(3) Uani 1 1 d . . .
H282 H 0.6920(14) 0.6074(10) -0.0357(8) 0.040(4) Uani 1 1 d . . .
H321 H 0.668(2) 0.4552(10) 0.1463(12) 0.050(4) Uiso 0.63(2) 1 d PD H 1
H322 H 0.698(2) 0.5515(10) 0.1183(14) 0.050(4) Uiso 0.63(2) 1 d PD H 1
H323 H 0.705(2) 0.4846(14) 0.0463(7) 0.050(4) Uiso 0.63(2) 1 d PD H 1
H324 H 0.659(4) 0.497(2) 0.1676(10) 0.050(4) Uiso 0.37(2) 1 d PD H 2
H325 H 0.717(3) 0.5444(17) 0.076(2) 0.050(4) Uiso 0.37(2) 1 d PD H 2
H326 H 0.688(3) 0.4465(12) 0.079(2) 0.050(4) Uiso 0.37(2) 1 d PD H 2
H331 H 0.4897(16) 0.4029(10) 0.1762(9) 0.038(3) Uani 1 1 d . . .
H351 H 0.2221(17) 0.5363(10) 0.1333(9) 0.038(3) Uani 1 1 d . . .
H371 H 0.2557(15) 0.644(3) 0.067(3) 0.057(5) Uiso 0.40(3) 1 d PD I 1
H372 H 0.343(4) 0.7060(17) 0.092(2) 0.057(5) Uiso 0.40(3) 1 d PD I 1
H373 H 0.380(4) 0.674(3) -0.0059(9) 0.057(5) Uiso 0.40(3) 1 d PD I 1
H374 H 0.2539(10) 0.6712(18) 0.0810(18) 0.057(5) Uiso 0.60(3) 1 d PD I 2
H375 H 0.389(2) 0.7095(11) 0.0509(19) 0.057(5) Uiso 0.60(3) 1 d PD I 2
H376 H 0.361(2) 0.6385(19) -0.0048(9) 0.057(5) Uiso 0.60(3) 1 d PD I 2
H381 H 0.1833(14) 0.4332(13) 0.2359(18) 0.036(3) Uiso 0.55(4) 1 d PD J 1
H382 H 0.291(2) 0.3768(16) 0.2530(15) 0.036(3) Uiso 0.55(4) 1 d PD J 1
H383 H 0.253(3) 0.3619(13) 0.1686(12) 0.036(3) Uiso 0.55(4) 1 d PD J 1
H384 H 0.206(3) 0.4277(17) 0.2616(14) 0.036(3) Uiso 0.45(4) 1 d PD J 2
H385 H 0.314(2) 0.3581(14) 0.222(2) 0.036(3) Uiso 0.45(4) 1 d PD J 2
H386 H 0.219(3) 0.383(2) 0.1714(16) 0.036(3) Uiso 0.45(4) 1 d PD J 2
H411 H 0.534(3) 0.9439(8) 0.1240(19) 0.066(5) Uiso 0.59(3) 1 d PD K 1
H412 H 0.570(3) 0.8767(19) 0.0477(8) 0.066(5) Uiso 0.59(3) 1 d PD K 1
H413 H 0.497(2) 0.8486(15) 0.1465(16) 0.066(5) Uiso 0.59(3) 1 d PD K 1
H414 H 0.559(4) 0.9401(13) 0.080(3) 0.066(5) Uiso 0.41(3) 1 d PD K 2
H415 H 0.540(4) 0.841(2) 0.076(2) 0.066(5) Uiso 0.41(3) 1 d PD K 2
H416 H 0.499(3) 0.886(3) 0.1679(13) 0.066(5) Uiso 0.41(3) 1 d PD K 2
H421 H 0.6942(17) 0.9768(13) 0.1512(10) 0.055(5) Uani 1 1 d . . .
H441 H 0.908(4) 0.954(2) 0.2355(15) 0.057(4) Uiso 0.51(4) 1 d PD L 1
H442 H 0.971(2) 0.978(2) 0.1344(17) 0.057(4) Uiso 0.51(4) 1 d PD L 1
H443 H 0.839(2) 1.0193(12) 0.190(3) 0.057(4) Uiso 0.51(4) 1 d PD L 1
H444 H 0.955(3) 0.945(2) 0.204(3) 0.057(4) Uiso 0.49(4) 1 d PD L 1
H445 H 0.934(3) 1.002(2) 0.1284(14) 0.057(4) Uiso 0.49(4) 1 d PD L 1
H446 H 0.835(3) 1.0047(19) 0.225(2) 0.057(4) Uiso 0.49(4) 1 d PD L 1
H451 H 0.9545(18) 0.8124(11) 0.1593(10) 0.055(5) Uani 1 1 d . . .
H471 H 0.9475(19) 0.6887(11) 0.1228(14) 0.063(7) Uani 1 1 d . . .
H472 H 0.8772(18) 0.6676(11) 0.0608(11) 0.050(5) Uani 1 1 d . . .
H473 H 0.8113(18) 0.6527(10) 0.1606(11) 0.057(6) Uani 1 1 d . . .
H61 H 0.9454(15) 0.6529(9) 0.7797(8) 0.036(3) Uani 1 1 d . . .
H63 H 1.0550(15) 0.8639(10) 0.8356(8) 0.036(3) Uani 1 1 d . . .
H65 H 1.0934(15) 0.6569(10) 0.9612(9) 0.036(3) Uani 1 1 d . . .
H72 H 1.1925(14) 0.8095(10) 0.6969(9) 0.036(3) Uani 1 1 d . . .
H74 H 1.2728(14) 1.0189(9) 0.5580(9) 0.036(3) Uani 1 1 d . . .
H76 H 0.9343(15) 0.9482(10) 0.6551(9) 0.036(3) Uani 1 1 d . . .
H86 H 0.7280(13) 0.7655(9) 0.7670(8) 0.031(3) Uani 1 1 d . . .
H88 H 0.5546(14) 0.9470(9) 0.9199(8) 0.031(3) Uani 1 1 d . . .
H90 H 0.9134(13) 0.9471(9) 0.8146(8) 0.031(3) Uani 1 1 d . . .
H100 H 1.0844(16) 0.6805(9) 0.6594(8) 0.033(3) Uani 1 1 d . . .
H104 H 0.8084(15) 0.8170(10) 0.6393(8) 0.033(3) Uani 1 1 d . . .
H114 H 0.9241(14) 0.6212(9) 0.4940(8) 0.033(3) Uani 1 1 d . . .
H60A H 0.413(3) 0.7571(16) 0.2528(15) 0.031(4) Uiso 0.650(13) 1 d P B 1
H60B H 0.398(2) 0.6279(15) 0.2440(14) 0.031(4) Uiso 0.650(13) 1 d P B 1
H62A H 0.113(2) 0.789(2) 0.3374(12) 0.074(4) Uiso 0.650(13) 1 d PD B 1
H62B H 0.239(2) 0.8279(17) 0.2792(15) 0.074(4) Uiso 0.650(13) 1 d PD B 1
H62C H 0.146(3) 0.796(2) 0.2358(13) 0.074(4) Uiso 0.650(13) 1 d PD B 1
H63A H 0.096(2) 0.6503(18) 0.3442(12) 0.074(4) Uiso 0.650(13) 1 d PD B 1
H63B H 0.204(2) 0.5934(13) 0.2826(17) 0.074(4) Uiso 0.650(13) 1 d PD B 1
H63C H 0.120(2) 0.6488(19) 0.2429(13) 0.074(4) Uiso 0.650(13) 1 d PD B 1
H60C H 0.390(5) 0.660(3) 0.237(3) 0.031(4) Uiso 0.350(13) 1 d P B 2
H60D H 0.437(5) 0.769(3) 0.241(3) 0.031(4) Uiso 0.350(13) 1 d P B 2
H60E H 0.356(4) 0.743(2) 0.169(2) 0.029(9) Uiso 0.350(13) 1 d P B 2
H61A H 0.262(5) 0.731(3) 0.348(3) 0.045(12) Uiso 0.350(13) 1 d P B 2
H62D H 0.097(3) 0.691(3) 0.346(2) 0.074(4) Uiso 0.350(13) 1 d PD B 2
H62E H 0.203(5) 0.622(2) 0.323(3) 0.074(4) Uiso 0.350(13) 1 d PD B 2
H62F H 0.164(5) 0.667(3) 0.248(2) 0.074(4) Uiso 0.350(13) 1 d PD B 2
H63D H 0.137(3) 0.832(3) 0.326(2) 0.074(4) Uiso 0.350(13) 1 d PD B 2
H63E H 0.272(4) 0.854(3) 0.265(3) 0.074(4) Uiso 0.350(13) 1 d PD B 2
H63F H 0.179(4) 0.814(4) 0.226(2) 0.074(4) Uiso 0.350(13) 1 d PDU B 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 C2 2.036(7) . ?
Ir1 C25 2.042(6) . ?
Ir1 B600 2.07(2) . ?
Ir1 B610 2.21(4) . ?
Ir1 H12 1.53(2) . ?
Ir1 H11 1.544(18) . ?
Ir1 H60A 1.87(4) . ?
Ir1 H60B 1.82(3) . ?
Ir1 H60C 1.75(6) . ?
Ir1 H60D 1.88(7) . ?
C2 N6 1.341(9) . ?
C2 N3 1.352(7) . ?
N3 C16 1.435(9) . ?
N3 C4 1.484(9) . ?
C4 C5 1.526(10) . ?
C4 H41 1.09(2) . ?
C4 H42 1.101(16) . ?
C5 N6 1.471(7) . ?
C5 H51 1.13(3) . ?
C5 H52 1.074(16) . ?
N6 C7 1.432(8) . ?
C7 C8 1.398(9) . ?
C7 C13 1.408(11) . ?
C8 C10 1.385(10) . ?
C8 C9 1.492(11) . ?
C9 H91 1.095(7) . ?
C9 H92 1.097(7) . ?
C9 H93 1.095(7) . ?
C9 H94 1.096(7) . ?
C9 H95 1.096(7) . ?
C9 H96 1.098(7) . ?
C10 C11 1.388(12) . ?
C10 H101 1.079(16) . ?
C11 C12 1.382(9) . ?
C11 C15 1.516(9) . ?
C12 C13 1.395(9) . ?
C12 H121 1.121(18) . ?
C13 C14 1.492(10) . ?
C14 H141 1.11(3) . ?
C14 H142 1.06(2) . ?
C14 H143 1.07(3) . ?
C15 H151 1.095(8) . ?
C15 H152 1.095(7) . ?
C15 H153 1.095(7) . ?
C15 H154 1.091(7) . ?
C15 H155 1.098(7) . ?
C15 H156 1.095(7) . ?
C16 C22 1.367(12) . ?
C16 C17 1.409(8) . ?
C17 C19 1.391(11) . ?
C17 C18 1.513(12) . ?
C18 H181 1.100(8) . ?
C18 H182 1.12(4) . ?
C18 H183 1.09(3) . ?
C18 H184 1.08(2) . ?
C18 H185 1.10(3) . ?
C18 H186 1.11(2) . ?
C19 C20 1.410(12) . ?
C19 H191 1.090(16) . ?
C20 C21 1.415(9) . ?
C20 C24 1.513(12) . ?
C21 C22 1.392(12) . ?
C21 H211 1.05(3) . ?
C22 C23 1.494(8) . ?
C23 H231 1.093(7) . ?
C23 H232 1.096(7) . ?
C23 H233 1.092(7) . ?
C23 H234 1.098(7) . ?
C23 H235 1.096(7) . ?
C23 H236 1.095(7) . ?
C24 H241 1.093(7) . ?
C24 H242 1.095(7) . ?
C24 H243 1.095(7) . ?
C24 H244 1.096(8) . ?
C24 H245 1.096(7) . ?
C24 H246 1.094(7) . ?
C25 N26 1.339(7) . ?
C25 N29 1.363(8) . ?
N26 C39 1.436(8) . ?
N26 C27 1.465(8) . ?
C27 C28 1.535(9) . ?
C27 H271 1.05(2) . ?
C27 H272 1.12(2) . ?
C28 N29 1.469(7) . ?
C28 H281 1.09(2) . ?
C28 H282 1.08(2) . ?
N29 C30 1.417(7) . ?
C30 C31 1.367(11) . ?
C30 C36 1.424(12) . ?
C31 C33 1.400(8) . ?
C31 C32 1.513(11) . ?
C32 H321 1.094(7) . ?
C32 H322 1.098(7) . ?
C32 H323 1.095(7) . ?
C32 H324 1.096(7) . ?
C32 H325 1.095(7) . ?
C32 H326 1.093(7) . ?
C33 C34 1.379(12) . ?
C33 H331 1.15(2) . ?
C34 C35 1.407(13) . ?
C34 C38 1.508(8) . ?
C35 C36 1.403(9) . ?
C35 H351 1.09(3) . ?
C36 C37 1.487(13) . ?
C37 H371 1.095(7) . ?
C37 H372 1.094(7) . ?
C37 H373 1.091(7) . ?
C37 H374 1.095(7) . ?
C37 H375 1.096(7) . ?
C37 H376 1.100(7) . ?
C38 H381 1.097(7) . ?
C38 H382 1.090(7) . ?
C38 H383 1.094(7) . ?
C38 H384 1.088(7) . ?
C38 H385 1.093(7) . ?
C38 H386 1.092(7) . ?
C39 C46 1.391(12) . ?
C39 C40 1.405(12) . ?
C40 C42 1.407(10) . ?
C40 C41 1.497(13) . ?
C41 H411 1.096(7) . ?
C41 H412 1.094(7) . ?
C41 H413 1.097(7) . ?
C41 H414 1.094(8) . ?
C41 H415 1.097(7) . ?
C41 H416 1.096(7) . ?
C42 C43 1.388(15) . ?
C42 H421 1.03(3) . ?
C43 C45 1.369(13) . ?
C43 C44 1.513(10) . ?
C44 H441 1.093(7) . ?
C44 H442 1.091(7) . ?
C44 H443 1.096(7) . ?
C44 H444 1.095(7) . ?
C44 H445 1.095(7) . ?
C44 H446 1.094(7) . ?
C45 C46 1.380(10) . ?
C45 H451 1.16(3) . ?
C46 C47 1.504(13) . ?
C47 H471 1.08(3) . ?
C47 H472 1.08(2) . ?
C47 H473 1.092(19) . ?
F56 C57 1.337(11) . ?
C57 F59 1.313(16) . ?
C57 F58 1.364(12) . ?
C57 C60 1.485(11) . ?
C60 C65 1.369(11) . ?
C60 C61 1.412(11) . ?
C61 C62 1.402(9) . ?
C61 H61 1.074(19) . ?
C62 C63 1.386(10) . ?
C62 B70 1.653(13) . ?
C63 C64 1.394(12) . ?
C63 H63 1.098(19) . ?
C64 C65 1.404(11) . ?
C64 C66 1.483(11) . ?
C65 H65 1.08(2) . ?
C66 F69 1.309(12) . ?
C66 F67 1.330(15) . ?
C66 F68 1.334(15) . ?
B70 C71 1.641(9) . ?
B70 C99 1.640(10) . ?
B70 C85 1.652(11) . ?
C71 C76 1.362(11) . ?
C71 C72 1.400(12) . ?
C72 C73 1.396(8) . ?
C72 H72 1.15(2) . ?
C73 C74 1.377(12) . ?
C73 C81 1.501(12) . ?
C74 C75 1.394(12) . ?
C74 H74 1.092(15) . ?
C75 C76 1.417(9) . ?
C75 C77 1.512(14) . ?
C76 H76 1.04(2) . ?
C77 F401 1.305(18) . ?
C77 F400 1.320(15) . ?
C77 F402 1.32(2) . ?
C81 F83 1.326(11) . ?
C81 F82 1.332(9) . ?
C81 F84 1.338(12) . ?
C85 C90 1.408(9) . ?
C85 C86 1.414(9) . ?
C86 C87 1.403(10) . ?
C86 H86 1.106(16) . ?
C87 C88 1.396(10) . ?
C87 C95 1.473(10) . ?
C88 C89 1.385(11) . ?
C88 H88 1.062(18) . ?
C89 C90 1.381(10) . ?
C89 C91 1.492(10) . ?
C90 H90 1.102(18) . ?
C91 F301 1.336(12) . ?
C91 F302 1.336(13) . ?
C91 F312 1.340(15) . ?
C91 F311 1.349(14) . ?
C91 F310 1.346(15) . ?
C91 F300 1.353(11) . ?
C95 F502 1.316(12) . ?
C95 F500 1.323(14) . ?
C95 F501 1.316(17) . ?
C99 C100 1.399(11) . ?
C99 C104 1.434(12) . ?
C100 C101 1.397(9) . ?
C100 H100 1.08(3) . ?
C101 C114 1.394(12) . ?
C101 C109 1.479(12) . ?
C104 C115 1.382(9) . ?
C104 H104 1.04(2) . ?
C105 F201 1.325(15) . ?
C105 F202 1.336(12) . ?
C105 F200 1.333(12) . ?
C105 C115 1.496(13) . ?
C109 F110 1.311(12) . ?
C109 F111 1.326(13) . ?
C109 F112 1.337(11) . ?
C114 C115 1.392(11) . ?
C114 H114 1.116(16) . ?
B600 N601 1.40(2) . ?
B600 H60A 1.33(3) . ?
B600 H60B 1.28(4) . ?
B600 H60C 0.76(8) . ?
B600 H60D 1.66(5) . ?
N601 C603 1.505(14) . ?
N601 C602 1.513(15) . ?
C602 H62A 1.060(13) . ?
C602 H62B 1.057(13) . ?
C602 H62C 1.059(13) . ?
C603 H63A 1.057(13) . ?
C603 H63B 1.059(13) . ?
C603 H63C 1.060(13) . ?
B610 N611 1.55(4) . ?
B610 H60A 1.06(5) . ?
B610 H60C 1.20(8) . ?
B610 H60D 1.30(6) . ?
B610 H60E 1.13(6) . ?
N611 C613 1.514(17) . ?
N611 C612 1.538(18) . ?
N611 H61A 0.98(7) . ?
C612 H62D 1.060(14) . ?
C612 H62E 1.060(14) . ?
C612 H62F 1.061(14) . ?
C613 H63D 1.059(14) . ?
C613 H63E 1.058(14) . ?
C613 H63F 1.059(14) . ?

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
C2 Ir1 C25 167.6(4) . . ?
C2 Ir1 B600 93.4(6) . . ?
C25 Ir1 B600 99.0(6) . . ?
C2 Ir1 B610 106.7(8) . . ?
C25 Ir1 B610 85.6(8) . . ?
B600 Ir1 B610 18.4(7) . . ?
C2 Ir1 H12 85.3(6) . . ?
C25 Ir1 H12 85.0(6) . . ?
B600 Ir1 H12 136.4(9) . . ?
B610 Ir1 H12 147.5(11) . . ?
C2 Ir1 H11 85.7(7) . . ?
C25 Ir1 H11 84.6(6) . . ?
B600 Ir1 H11 146.6(11) . . ?
B610 Ir1 H11 132.9(12) . . ?
H12 Ir1 H11 76.9(12) . . ?
C2 Ir1 H60A 95.0(9) . . ?
C25 Ir1 H60A 95.3(9) . . ?
B600 Ir1 H60A 39.2(9) . . ?
B610 Ir1 H60A 28.4(13) . . ?
H12 Ir1 H60A 175.6(11) . . ?
H11 Ir1 H60A 107.6(12) . . ?
C2 Ir1 H60B 93.5(8) . . ?
C25 Ir1 H60B 95.6(8) . . ?
B600 Ir1 H60B 37.8(11) . . ?
B610 Ir1 H60B 51.6(13) . . ?
H12 Ir1 H60B 98.6(12) . . ?
H11 Ir1 H60B 175.5(14) . . ?
H60A Ir1 H60B 76.9(12) . . ?
C2 Ir1 H60C 100.3(16) . . ?
C25 Ir1 H60C 91.0(16) . . ?
B600 Ir1 H60C 21(2) . . ?
B610 Ir1 H60C 33(2) . . ?
H12 Ir1 H60C 117(2) . . ?
H11 Ir1 H60C 165(2) . . ?
H60A Ir1 H60C 59(2) . . ?
H60B Ir1 H60C 19(2) . . ?
C2 Ir1 H60D 100.5(15) . . ?
C25 Ir1 H60D 88.5(15) . . ?
B600 Ir1 H60D 49.4(16) . . ?
B610 Ir1 H60D 35.8(18) . . ?
H12 Ir1 H60D 172.0(15) . . ?
H11 Ir1 H60D 97.9(19) . . ?
H60A Ir1 H60D 11.3(16) . . ?
H60B Ir1 H60D 86.6(18) . . ?
H60C Ir1 H60D 68(2) . . ?
N6 C2 N3 106.8(5) . . ?
N6 C2 Ir1 125.0(4) . . ?
N3 C2 Ir1 127.8(5) . . ?
C2 N3 C16 124.2(5) . . ?
C2 N3 C4 114.1(6) . . ?
C16 N3 C4 121.2(5) . . ?
N3 C4 C5 101.4(5) . . ?
N3 C4 H41 108.3(10) . . ?
C5 C4 H41 111.3(12) . . ?
N3 C4 H42 111.7(13) . . ?
C5 C4 H42 113.4(9) . . ?
H41 C4 H42 110.3(13) . . ?
N6 C5 C4 103.2(6) . . ?
N6 C5 H51 111.1(9) . . ?
C4 C5 H51 112.0(10) . . ?
N6 C5 H52 110.8(11) . . ?
C4 C5 H52 112.4(10) . . ?
H51 C5 H52 107.5(15) . . ?
C2 N6 C7 127.0(5) . . ?
C2 N6 C5 113.8(5) . . ?
C7 N6 C5 119.0(6) . . ?
C8 C7 C13 122.2(6) . . ?
C8 C7 N6 119.9(7) . . ?
C13 C7 N6 117.8(6) . . ?
C10 C8 C7 118.5(7) . . ?
C10 C8 C9 120.3(6) . . ?
C7 C8 C9 121.2(6) . . ?
C8 C9 H91 112.4(19) . . ?
C8 C9 H92 107.3(19) . . ?
H91 C9 H92 106.7(12) . . ?
C8 C9 H93 116.5(19) . . ?
H91 C9 H93 107.3(12) . . ?
H92 C9 H93 106.0(12) . . ?
C8 C9 H94 112.8(17) . . ?
H91 C9 H94 36.2(17) . . ?
H92 C9 H94 72.4(16) . . ?
H93 C9 H94 128(3) . . ?
C8 C9 H95 117.9(16) . . ?
H91 C9 H95 128(2) . . ?
H92 C9 H95 45.1(17) . . ?
H93 C9 H95 62.0(18) . . ?
H94 C9 H95 106.9(11) . . ?
C8 C9 H96 106.0(16) . . ?
H91 C9 H96 71(2) . . ?
H92 C9 H96 144(2) . . ?
H93 C9 H96 46.1(18) . . ?
H94 C9 H96 105.8(12) . . ?
H95 C9 H96 106.6(12) . . ?
C8 C10 C11 121.1(6) . . ?
C8 C10 H101 120.1(11) . . ?
C11 C10 H101 118.8(10) . . ?
C12 C11 C10 119.3(7) . . ?
C12 C11 C15 120.2(7) . . ?
C10 C11 C15 120.5(6) . . ?
C11 C12 C13 122.4(7) . . ?
C11 C12 H121 119.0(9) . . ?
C13 C12 H121 118.6(8) . . ?
C12 C13 C7 116.6(6) . . ?
C12 C13 C14 123.1(7) . . ?
C7 C13 C14 120.3(7) . . ?
C13 C14 H141 109.0(11) . . ?
C13 C14 H142 113.2(10) . . ?
H141 C14 H142 104.5(17) . . ?
C13 C14 H143 112.5(13) . . ?
H141 C14 H143 107.0(16) . . ?
H142 C14 H143 110.1(16) . . ?
C11 C15 H151 111(3) . . ?
C11 C15 H152 111(2) . . ?
H151 C15 H152 107.1(13) . . ?
C11 C15 H153 114(3) . . ?
H151 C15 H153 106.5(12) . . ?
H152 C15 H153 106.8(12) . . ?
C11 C15 H154 113.2(14) . . ?
H151 C15 H154 27(3) . . ?
H152 C15 H154 82(3) . . ?
H153 C15 H154 124(3) . . ?
C11 C15 H155 112.2(14) . . ?
H151 C15 H155 128(3) . . ?
H152 C15 H155 30(3) . . ?
H153 C15 H155 80(3) . . ?
H154 C15 H155 107.6(11) . . ?
C11 C15 H156 110.1(14) . . ?
H151 C15 H156 84(3) . . ?
H152 C15 H156 129(3) . . ?
H153 C15 H156 27(2) . . ?
H154 C15 H156 107.3(11) . . ?
H155 C15 H156 106.0(10) . . ?
C22 C16 C17 122.7(7) . . ?
C22 C16 N3 119.2(5) . . ?
C17 C16 N3 118.1(7) . . ?
C19 C17 C16 117.8(7) . . ?
C19 C17 C18 118.5(5) . . ?
C16 C17 C18 123.6(7) . . ?
C17 C18 H181 104(3) . . ?
C17 C18 H182 125(3) . . ?
H181 C18 H182 104(3) . . ?
C17 C18 H183 111(3) . . ?
H181 C18 H183 106(2) . . ?
H182 C18 H183 105(3) . . ?
C17 C18 H184 111.1(17) . . ?
H181 C18 H184 38(2) . . ?
H182 C18 H184 121(3) . . ?
H183 C18 H184 68(2) . . ?
C17 C18 H185 113.0(16) . . ?
H181 C18 H185 76(3) . . ?
H182 C18 H185 35(2) . . ?
H183 C18 H185 134(3) . . ?
H184 C18 H185 107(2) . . ?
C17 C18 H186 112.8(17) . . ?
H181 C18 H186 138(3) . . ?
H182 C18 H186 70(2) . . ?
H183 C18 H186 43(2) . . ?
H184 C18 H186 107.2(16) . . ?
H185 C18 H186 105.2(18) . . ?
C17 C19 C20 121.4(6) . . ?
C17 C19 H191 121.6(13) . . ?
C20 C19 H191 117.0(13) . . ?
C19 C20 C21 117.7(8) . . ?
C19 C20 C24 120.9(6) . . ?
C21 C20 C24 121.3(8) . . ?
C22 C21 C20 121.5(9) . . ?
C22 C21 H211 119.0(10) . . ?
C20 C21 H211 119.4(11) . . ?
C16 C22 C21 118.4(6) . . ?
C16 C22 C23 123.8(7) . . ?
C21 C22 C23 117.8(8) . . ?
C22 C23 H231 111.3(16) . . ?
C22 C23 H232 108.9(15) . . ?
H231 C23 H232 107.2(11) . . ?
C22 C23 H233 114.4(16) . . ?
H231 C23 H233 108.3(12) . . ?
H232 C23 H233 106.5(11) . . ?
C22 C23 H234 116.7(17) . . ?
H231 C23 H234 24(2) . . ?
H232 C23 H234 83(2) . . ?
H233 C23 H234 121(3) . . ?
C22 C23 H235 112.7(17) . . ?
H231 C23 H235 127(2) . . ?
H232 C23 H235 30(2) . . ?
H233 C23 H235 79(2) . . ?
H234 C23 H235 106.1(11) . . ?
C22 C23 H236 106.7(17) . . ?
H231 C23 H236 87(2) . . ?
H232 C23 H236 133(2) . . ?
H233 C23 H236 29(2) . . ?
H234 C23 H236 107.0(12) . . ?
H235 C23 H236 107.1(11) . . ?
C20 C24 H241 112.7(18) . . ?
C20 C24 H242 115.8(19) . . ?
H241 C24 H242 107.8(12) . . ?
C20 C24 H243 106.1(19) . . ?
H241 C24 H243 107.6(12) . . ?
H242 C24 H243 106.3(12) . . ?
C20 C24 H244 116(2) . . ?
H241 C24 H244 47(2) . . ?
H242 C24 H244 64(2) . . ?
H243 C24 H244 137(3) . . ?
C20 C24 H245 103(3) . . ?
H241 C24 H245 142(3) . . ?
H242 C24 H245 43(2) . . ?
H243 C24 H245 72(2) . . ?
H244 C24 H245 106.6(12) . . ?
C20 C24 H246 117(3) . . ?
H241 C24 H246 67(2) . . ?
H242 C24 H246 124(3) . . ?
H243 C24 H246 41(2) . . ?
H244 C24 H246 107.0(13) . . ?
H245 C24 H246 106.7(12) . . ?
N26 C25 N29 107.0(4) . . ?
N26 C25 Ir1 125.8(5) . . ?
N29 C25 Ir1 126.9(4) . . ?
C25 N26 C39 127.5(4) . . ?
C25 N26 C27 113.9(5) . . ?
C39 N26 C27 118.3(4) . . ?
N26 C27 C28 102.3(5) . . ?
N26 C27 H271 112.2(9) . . ?
C28 C27 H271 114.0(11) . . ?
N26 C27 H272 111.3(12) . . ?
C28 C27 H272 109.7(10) . . ?
H271 C27 H272 107.3(13) . . ?
N29 C28 C27 101.9(5) . . ?
N29 C28 H281 109.7(10) . . ?
C27 C28 H281 112.8(10) . . ?
N29 C28 H282 110.7(9) . . ?
C27 C28 H282 115.3(11) . . ?
H281 C28 H282 106.4(14) . . ?
C25 N29 C30 122.2(4) . . ?
C25 N29 C28 113.3(5) . . ?
C30 N29 C28 122.5(5) . . ?
C31 C30 N29 120.7(7) . . ?
C31 C30 C36 121.4(6) . . ?
N29 C30 C36 117.7(7) . . ?
C30 C31 C33 118.5(8) . . ?
C30 C31 C32 122.1(5) . . ?
C33 C31 C32 119.4(7) . . ?
C31 C32 H321 111.3(15) . . ?
C31 C32 H322 114.6(16) . . ?
H321 C32 H322 107.5(12) . . ?
C31 C32 H323 110.2(16) . . ?
H321 C32 H323 107.0(11) . . ?
H322 C32 H323 105.9(11) . . ?
C31 C32 H324 105(2) . . ?
H321 C32 H324 45(2) . . ?
H322 C32 H324 71(2) . . ?
H323 C32 H324 142(3) . . ?
C31 C32 H325 119(3) . . ?
H321 C32 H325 128(3) . . ?
H322 C32 H325 39.0(18) . . ?
H323 C32 H325 68.1(18) . . ?
H324 C32 H325 106.7(12) . . ?
C31 C32 H326 111(2) . . ?
H321 C32 H326 64(2) . . ?
H322 C32 H326 134(3) . . ?
H323 C32 H326 46(2) . . ?
H324 C32 H326 107.3(13) . . ?
H325 C32 H326 107.5(12) . . ?
C34 C33 C31 122.5(8) . . ?
C34 C33 H331 118.5(10) . . ?
C31 C33 H331 118.8(11) . . ?
C33 C34 C35 117.8(6) . . ?
C33 C34 C38 120.5(8) . . ?
C35 C34 C38 121.8(8) . . ?
C36 C35 C34 121.4(8) . . ?
C36 C35 H351 119.4(11) . . ?
C34 C35 H351 119.0(10) . . ?
C35 C36 C30 117.5(8) . . ?
C35 C36 C37 120.6(8) . . ?
C30 C36 C37 121.8(6) . . ?
C36 C37 H371 102(3) . . ?
C36 C37 H372 109(2) . . ?
H371 C37 H372 106.8(12) . . ?
C36 C37 H373 123(3) . . ?
H371 C37 H373 107.2(13) . . ?
H372 C37 H373 108.1(13) . . ?
C36 C37 H374 116.5(19) . . ?
H371 C37 H374 29(2) . . ?
H372 C37 H374 79(2) . . ?
H373 C37 H374 112(4) . . ?
C36 C37 H375 118.1(18) . . ?
H371 C37 H375 134(3) . . ?
H372 C37 H375 41.4(18) . . ?
H373 C37 H375 70(2) . . ?
H374 C37 H375 107.6(12) . . ?
C36 C37 H376 101(2) . . ?
H371 C37 H376 87(3) . . ?
H372 C37 H376 143(2) . . ?
H373 C37 H376 35(2) . . ?
H374 C37 H376 107.0(12) . . ?
H375 C37 H376 105.2(11) . . ?
C34 C38 H381 108.7(14) . . ?
C34 C38 H382 113.0(14) . . ?
H381 C38 H382 107.4(11) . . ?
C34 C38 H383 112.5(13) . . ?
H381 C38 H383 106.6(11) . . ?
H382 C38 H383 108.3(11) . . ?
C34 C38 H384 111.8(16) . . ?
H381 C38 H384 33.2(18) . . ?
H382 C38 H384 76.3(18) . . ?
H383 C38 H384 129(2) . . ?
C34 C38 H385 108.4(17) . . ?
H381 C38 H385 135(2) . . ?
H382 C38 H385 33.6(17) . . ?
H383 C38 H385 81(2) . . ?
H384 C38 H385 108.5(12) . . ?
C34 C38 H386 111.4(17) . . ?
H381 C38 H386 80.8(19) . . ?
H382 C38 H386 129(2) . . ?
H383 C38 H386 28(2) . . ?
H384 C38 H386 109.3(12) . . ?
H385 C38 H386 107.4(12) . . ?
C46 C39 C40 122.0(6) . . ?
C46 C39 N26 118.5(7) . . ?
C40 C39 N26 119.4(8) . . ?
C39 C40 C42 118.1(9) . . ?
C39 C40 C41 121.9(6) . . ?
C42 C40 C41 120.0(8) . . ?
C40 C41 H411 114(2) . . ?
C40 C41 H412 111(2) . . ?
H411 C41 H412 107.1(12) . . ?
C40 C41 H413 111(2) . . ?
H411 C41 H413 106.0(12) . . ?
H412 C41 H413 107.3(12) . . ?
C40 C41 H414 116(3) . . ?
H411 C41 H414 40(2) . . ?
H412 C41 H414 70(2) . . ?
H413 C41 H414 131(3) . . ?
C40 C41 H415 113(3) . . ?
H411 C41 H415 132(3) . . ?
H412 C41 H415 43(2) . . ?
H413 C41 H415 67(2) . . ?
H414 C41 H415 107.3(13) . . ?
C40 C41 H416 107(3) . . ?
H411 C41 H416 71(2) . . ?
H412 C41 H416 138(3) . . ?
H413 C41 H416 41.4(19) . . ?
H414 C41 H416 107.5(13) . . ?
H415 C41 H416 106.0(12) . . ?
C43 C42 C40 119.8(9) . . ?
C43 C42 H421 123.4(14) . . ?
C40 C42 H421 116.8(15) . . ?
C45 C43 C42 120.2(7) . . ?
C45 C43 C44 121.0(10) . . ?
C42 C43 C44 118.8(9) . . ?
C43 C44 H441 113.6(19) . . ?
C43 C44 H442 111.8(19) . . ?
H441 C44 H442 107.6(12) . . ?
C43 C44 H443 109(2) . . ?
H441 C44 H443 106.4(12) . . ?
H442 C44 H443 108.2(12) . . ?
C43 C44 H444 113(2) . . ?
H441 C44 H444 36(2) . . ?
H442 C44 H444 75(2) . . ?
H443 C44 H444 133(3) . . ?
C43 C44 H445 110(2) . . ?
H441 C44 H445 132(3) . . ?
H442 C44 H445 35(2) . . ?
H443 C44 H445 77(2) . . ?
H444 C44 H445 107.3(12) . . ?
C43 C44 H446 113(2) . . ?
H441 C44 H446 74(2) . . ?
H442 C44 H446 130(3) . . ?
H443 C44 H446 35(2) . . ?
H444 C44 H446 106.9(12) . . ?
H445 C44 H446 107.1(12) . . ?
C43 C45 C46 122.3(10) . . ?
C43 C45 H451 122.9(10) . . ?
C46 C45 H451 114.7(11) . . ?
C45 C46 C39 117.6(8) . . ?
C45 C46 C47 122.2(9) . . ?
C39 C46 C47 120.1(7) . . ?
C46 C47 H471 110.9(12) . . ?
C46 C47 H472 114.4(15) . . ?
H471 C47 H472 103.9(17) . . ?
C46 C47 H473 114.0(13) . . ?
H471 C47 H473 108.3(19) . . ?
H472 C47 H473 104.6(16) . . ?
F59 C57 F56 105.1(9) . . ?
F59 C57 F58 104.7(10) . . ?
F56 C57 F58 104.5(8) . . ?
F59 C57 C60 114.3(9) . . ?
F56 C57 C60 114.2(8) . . ?
F58 C57 C60 113.0(7) . . ?
C65 C60 C61 121.6(7) . . ?
C65 C60 C57 119.3(8) . . ?
C61 C60 C57 119.1(7) . . ?
C62 C61 C60 121.3(6) . . ?
C62 C61 H61 119.3(11) . . ?
C60 C61 H61 119.4(11) . . ?
C63 C62 C61 116.4(7) . . ?
C63 C62 B70 120.3(6) . . ?
C61 C62 B70 123.2(6) . . ?
C62 C63 C64 122.4(7) . . ?
C62 C63 H63 119.1(12) . . ?
C64 C63 H63 118.5(11) . . ?
C63 C64 C65 120.8(7) . . ?
C63 C64 C66 119.1(7) . . ?
C65 C64 C66 120.0(8) . . ?
C60 C65 C64 117.5(8) . . ?
C60 C65 H65 120.5(10) . . ?
C64 C65 H65 122.0(10) . . ?
F69 C66 F67 103.6(10) . . ?
F69 C66 F68 109.8(12) . . ?
F67 C66 F68 104.0(9) . . ?
F69 C66 C64 112.8(7) . . ?
F67 C66 C64 113.2(10) . . ?
F68 C66 C64 112.7(9) . . ?
C71 B70 C99 105.6(5) . . ?
C71 B70 C62 111.1(7) . . ?
C99 B70 C62 112.9(6) . . ?
C71 B70 C85 110.3(6) . . ?
C99 B70 C85 113.3(7) . . ?
C62 B70 C85 103.7(5) . . ?
C76 C71 C72 116.0(6) . . ?
C76 C71 B70 122.6(7) . . ?
C72 C71 B70 121.2(7) . . ?
C73 C72 C71 122.8(8) . . ?
C73 C72 H72 117.5(10) . . ?
C71 C72 H72 119.7(9) . . ?
C74 C73 C72 120.2(8) . . ?
C74 C73 C81 120.2(5) . . ?
C72 C73 C81 119.5(8) . . ?
C73 C74 C75 118.2(6) . . ?
C73 C74 H74 121.8(14) . . ?
C75 C74 H74 119.8(14) . . ?
C74 C75 C76 120.1(8) . . ?
C74 C75 C77 118.1(6) . . ?
C76 C75 C77 121.7(8) . . ?
C71 C76 C75 122.5(8) . . ?
C71 C76 H76 118.9(10) . . ?
C75 C76 H76 118.6(11) . . ?
F401 C77 F400 105.4(12) . . ?
F401 C77 F402 107.6(14) . . ?
F400 C77 F402 109.4(14) . . ?
F401 C77 C75 110.8(13) . . ?
F400 C77 C75 110.4(10) . . ?
F402 C77 C75 112.9(8) . . ?
F83 C81 F82 108.2(7) . . ?
F83 C81 F84 107.4(9) . . ?
F82 C81 F84 106.2(7) . . ?
F83 C81 C73 111.1(6) . . ?
F82 C81 C73 112.2(9) . . ?
F84 C81 C73 111.4(7) . . ?
C90 C85 C86 115.2(6) . . ?
C90 C85 B70 121.9(6) . . ?
C86 C85 B70 122.7(6) . . ?
C87 C86 C85 122.6(6) . . ?
C87 C86 H86 118.1(10) . . ?
C85 C86 H86 119.3(10) . . ?
C88 C87 C86 120.2(7) . . ?
C88 C87 C95 118.8(7) . . ?
C86 C87 C95 121.0(6) . . ?
C89 C88 C87 117.6(7) . . ?
C89 C88 H88 121.5(10) . . ?
C87 C88 H88 120.9(10) . . ?
C88 C89 C90 122.4(6) . . ?
C88 C89 C91 119.1(6) . . ?
C90 C89 C91 118.4(6) . . ?
C89 C90 C85 121.8(6) . . ?
C89 C90 H90 120.9(9) . . ?
C85 C90 H90 117.0(10) . . ?
F301 C91 F302 112.0(13) . . ?
F301 C91 F312 130.3(18) . . ?
F302 C91 F312 31.6(14) . . ?
F301 C91 F311 43(2) . . ?
F302 C91 F311 70(2) . . ?
F312 C91 F311 95(2) . . ?
F301 C91 F310 77(2) . . ?
F302 C91 F310 123.8(19) . . ?
F312 C91 F310 99(2) . . ?
F311 C91 F310 106(2) . . ?
F301 C91 F300 108.2(13) . . ?
F302 C91 F300 104.4(13) . . ?
F312 C91 F300 73.8(18) . . ?
F311 C91 F300 127.3(17) . . ?
F310 C91 F300 32.4(17) . . ?
F301 C91 C89 111.4(9) . . ?
F302 C91 C89 109.7(10) . . ?
F312 C91 C89 113.7(16) . . ?
F311 C91 C89 120.3(14) . . ?
F310 C91 C89 118.2(17) . . ?
F300 C91 C89 110.9(10) . . ?
F502 C95 F500 105.0(10) . . ?
F502 C95 F501 105.5(11) . . ?
F500 C95 F501 108.4(13) . . ?
F502 C95 C87 113.2(9) . . ?
F500 C95 C87 113.1(9) . . ?
F501 C95 C87 111.1(9) . . ?
C100 C99 C104 116.9(6) . . ?
C100 C99 B70 121.2(7) . . ?
C104 C99 B70 121.8(7) . . ?
C101 C100 C99 122.0(8) . . ?
C101 C100 H100 118.5(10) . . ?
C99 C100 H100 119.5(9) . . ?
C114 C101 C100 120.3(7) . . ?
C114 C101 C109 119.6(6) . . ?
C100 C101 C109 120.0(8) . . ?
C115 C104 C99 120.3(7) . . ?
C115 C104 H104 118.8(12) . . ?
C99 C104 H104 120.9(10) . . ?
F201 C105 F202 104.2(11) . . ?
F201 C105 F200 109.4(10) . . ?
F202 C105 F200 103.6(9) . . ?
F201 C105 C115 114.9(7) . . ?
F202 C105 C115 111.4(9) . . ?
F200 C105 C115 112.4(9) . . ?
F110 C109 F111 108.5(10) . . ?
F110 C109 F112 105.5(7) . . ?
F111 C109 F112 106.1(7) . . ?
F110 C109 C101 111.2(7) . . ?
F111 C109 C101 111.9(7) . . ?
F112 C109 C101 113.4(9) . . ?
C101 C114 C115 118.5(6) . . ?
C101 C114 H114 119.8(13) . . ?
C115 C114 H114 121.7(13) . . ?
C104 C115 C114 121.9(8) . . ?
C104 C115 C105 121.0(7) . . ?
C114 C115 C105 117.1(6) . . ?
N601 B600 Ir1 171.1(13) . . ?
N601 B600 H60A 115(2) . . ?
Ir1 B600 H60A 62.3(17) . . ?
N601 B600 H60B 122.5(18) . . ?
Ir1 B600 H60B 60.7(15) . . ?
H60A B600 H60B 123(3) . . ?
N601 B600 H60C 130(4) . . ?
Ir1 B600 H60C 56(4) . . ?
H60A B600 H60C 114(4) . . ?
H60B B600 H60C 17(4) . . ?
N601 B600 H60D 118(3) . . ?
Ir1 B600 H60D 59(2) . . ?
H60A B600 H60D 7(2) . . ?
H60B B600 H60D 119(3) . . ?
H60C B600 H60D 109(4) . . ?
B600 N601 C603 121.8(12) . . ?
B600 N601 C602 126.4(11) . . ?
C603 N601 C602 111.6(10) . . ?
B600 N601 H61A 77(2) . . ?
C603 N601 H61A 115.7(19) . . ?
C602 N601 H61A 86(2) . . ?
B600 N601 H62F 125(2) . . ?
C603 N601 H62F 30(2) . . ?
C602 N601 H62F 98(2) . . ?
H61A N601 H62F 144(2) . . ?
N601 C602 H62A 109(2) . . ?
N601 C602 H62B 107(2) . . ?
H62A C602 H62B 110.0(14) . . ?
N601 C602 H62C 112(2) . . ?
H62A C602 H62C 109.2(14) . . ?
H62B C602 H62C 110.0(14) . . ?
N601 C602 H63D 142(3) . . ?
H62A C602 H63D 44(3) . . ?
H62B C602 H63D 72(3) . . ?
H62C C602 H63D 104(4) . . ?
N601 C602 H63F 117(4) . . ?
H62A C602 H63F 125(4) . . ?
H62B C602 H63F 84(3) . . ?
H62C C602 H63F 27(3) . . ?
H63D C602 H63F 101(4) . . ?
N601 C603 H63A 108.2(19) . . ?
N601 C603 H63B 108(2) . . ?
H63A C603 H63B 110.6(13) . . ?
N601 C603 H63C 110.5(19) . . ?
H63A C603 H63C 110.5(13) . . ?
H63B C603 H63C 109.3(14) . . ?
N601 C603 H62D 80(2) . . ?
H63A C603 H62D 32(2) . . ?
H63B C603 H62D 136(3) . . ?
H63C C603 H62D 107(3) . . ?
N601 C603 H62E 82(3) . . ?
H63A C603 H62E 80(3) . . ?
H63B C603 H62E 50(3) . . ?
H63C C603 H62E 159(3) . . ?
H62D C603 H62E 91(3) . . ?
N601 C603 H62F 71(4) . . ?
H63A C603 H62F 131(5) . . ?
H63B C603 H62F 116(4) . . ?
H63C C603 H62F 40(4) . . ?
H62D C603 H62F 107(4) . . ?
H62E C603 H62F 143(5) . . ?
N611 B610 Ir1 125(2) . . ?
N611 B610 H60A 94(2) . . ?
Ir1 B610 H60A 57(3) . . ?
N611 B610 H60C 105(3) . . ?
Ir1 B610 H60C 52(3) . . ?
H60A B610 H60C 104(5) . . ?
N611 B610 H60D 105(3) . . ?
Ir1 B610 H60D 58(3) . . ?
H60A B610 H60D 14(3) . . ?
H60C B610 H60D 109(5) . . ?
N611 B610 H60E 111(4) . . ?
Ir1 B610 H60E 124(3) . . ?
H60A B610 H60E 121(3) . . ?
H60C B610 H60E 117(4) . . ?
H60D B610 H60E 109(4) . . ?
C613 N611 C612 113(2) . . ?
C613 N611 B610 106(2) . . ?
C612 N611 B610 109.4(19) . . ?
C613 N611 H61A 123(3) . . ?
C612 N611 H61A 95(3) . . ?
B610 N611 H61A 111(4) . . ?
N611 C612 H63A 141(3) . . ?
N611 C612 H63B 129(2) . . ?
H63A C612 H63B 83(2) . . ?
N611 C612 H63C 128(2) . . ?
H63A C612 H63C 80(2) . . ?
H63B C612 H63C 69.1(13) . . ?
N611 C612 H62D 105(3) . . ?
H63A C612 H62D 39(3) . . ?
H63B C612 H62D 122(3) . . ?
H63C C612 H62D 94(3) . . ?
N611 C612 H62E 114(3) . . ?
H63A C612 H62E 78(4) . . ?
H63B C612 H62E 36(3) . . ?
H63C C612 H62E 103(3) . . ?
H62D C612 H62E 109.5(15) . . ?
N611 C612 H62F 109(3) . . ?
H63A C612 H62F 101(4) . . ?
H63B C612 H62F 73(3) . . ?
H63C C612 H62F 21(3) . . ?
H62D C612 H62F 109.9(16) . . ?
H62E C612 H62F 109.1(15) . . ?
N611 C613 H62A 79(2) . . ?
N611 C613 H62B 86(5) . . ?
H62A C613 H62B 125(4) . . ?
N611 C613 H62C 104(3) . . ?
H62A C613 H62C 80.9(18) . . ?
H62B C613 H62C 154(4) . . ?
N611 C613 H63D 107(4) . . ?
H62A C613 H63D 36(3) . . ?
H62B C613 H63D 105(4) . . ?
H62C C613 H63D 96(4) . . ?
N611 C613 H63E 105(4) . . ?
H62A C613 H63E 141(3) . . ?
H62B C613 H63E 23(5) . . ?
H62C C613 H63E 133(3) . . ?
H63D C613 H63E 110.5(16) . . ?
N611 C613 H63F 115(4) . . ?
H62A C613 H63F 103(3) . . ?
H62B C613 H63F 131(4) . . ?
H62C C613 H63F 23(3) . . ?
H63D C613 H63F 109.4(16) . . ?
H63E C613 H63F 110.3(16) . . ?

_diffrn_measured_fraction_theta_max 0.027
_diffrn_reflns_theta_full        84.73
_diffrn_measured_fraction_theta_full 0.027
_refine_diff_density_max         1.256
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.256

#==============================================================================
# start Validation Reply Form
#==============================================================================
_vrf_TYPE031_11-and-12(Neutron)  
;
PROBLEM: _diffrn_radiation_wavelength is not of type numb.
RESPONSE: Data collected with Time of Flight Neutron Diffraction Data; 
see _exptl_special_details and _refine_special_details for information.
;
_vrf_PLAT029_11-and-12(Neutron)  
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.220      
RESPONSE: Data collected with Time of Flight Neutron Diffraction Data; 
see _exptl_special_details and _refine_special_details for information.
;
_vrf_PLAT051_11-and-12(Neutron)  
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .    957.54 %
RESPONSE: Data collected with Time of Flight Neutron Diffraction Data; 
see _exptl_special_details and _refine_special_details for information.
;
_vrf_CELL004_11-and-12(Neutron)  
;
PROBLEM: _cell_measurement_theta_min is missing
RESPONSE: Data collected with Time of Flight Neutron Diffraction Data; 
see _exptl_special_details and _refine_special_details for information.
;
_vrf_CELL005_11-and-12(Neutron)  
;
PROBLEM: _cell_measurement_theta_max is missing
RESPONSE: Data collected with Time of Flight Neutron Diffraction Data; 
see _exptl_special_details and _refine_special_details for information.
;
#==============================================================================
# End Validation Reply Form
#==============================================================================
_database_code_depnum_ccdc_archive 'CCDC 1002308'
