# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound_4b_VPX104_OKZ141
_database_code_depnum_ccdc_archive 'CCDC 2083329'
loop_
_audit_author_name
_audit_author_address
'Vincenzo Passarelli'
;Instituto de Sintesis Quimica y Catalisis Homogenea (CSIC)
Spain
;
_audit_update_record             
;
2021-05-12 deposited with the CCDC.	2021-07-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H26 Cl Ir N2 O3, 2 (C H Cl3)'
_chemical_formula_sum            'C25 H28 Cl7 Ir N2 O3'
_chemical_formula_weight         844.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.4363(11)
_cell_length_b                   16.3179(12)
_cell_length_c                   12.9166(9)
_cell_angle_alpha                90
_cell_angle_beta                 113.8900(10)
_cell_angle_gamma                90
_cell_volume                     2974.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6236
_cell_measurement_theta_min      2.887
_cell_measurement_theta_max      27.216

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_F_000             1648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    5.148
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4436
_exptl_absorpt_correction_T_max  0.5633
_exptl_absorpt_process_details   
; 
 Multi-scan correction included in APEX2 package (Bruker AXS, 2008)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       'ω rotations with narrow frames'
_diffrn_detector_area_resol_mean 8.26
_diffrn_reflns_number            33168
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.129
_diffrn_reflns_theta_max         28.258
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7145
_reflns_number_gt                5468
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART in APEX2 (Bruker AXS,2008)'
_computing_cell_refinement       'SAINT+ in APEX2 (Bruker AXS,2008)'
_computing_data_reduction        'SAINT+ in APEX2 (Bruker AXS,2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'
_refine_special_details          
;
 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 structure was solved by the Patterson method and anisotropic refinement
 was applied to all non hydrogen atoms. The hydrogen atoms were included
 in calculated positions and refined with a riding model.

 Each of the two disordered chloroform molecules (per iridium) were included
 in the model using two sets of atomic coordinates with complementary
 occupancy factors. SADI restraints were used and anisotropic refinement
 (except for C91A and C91B) were applied to all non hydrogen atoms.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0186P)²+5.4368P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7145
_refine_ls_number_parameters     409
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0665
_refine_ls_wR_factor_gt          0.0594
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C92A C 0.3424(7) 0.7424(9) 0.1927(9) 0.041(4) Uani 0.348(3) 1 d D . P A 1
H92A H 0.3242 0.6881 0.2137 0.050 Uiso 0.348(3) 1 calc R U P A 1
Cl5A Cl 0.4195(3) 0.7886(3) 0.3187(4) 0.0480(12) Uani 0.348(3) 1 d D . P A 1
Cl6A Cl 0.4007(3) 0.7227(3) 0.1050(4) 0.0583(14) Uani 0.348(3) 1 d D . P A 1
Cl7A Cl 0.2371(3) 0.7986(2) 0.1257(3) 0.0436(11) Uani 0.348(3) 1 d D . P A 1
C92B C 0.4124(6) 0.7693(4) 0.1395(6) 0.039(2) Uani 0.652(3) 1 d D . P A 2
H92B H 0.4722 0.7462 0.1390 0.047 Uiso 0.652(3) 1 calc R U P A 2
Cl5B Cl 0.4126(2) 0.7492(2) 0.2721(3) 0.0649(8) Uani 0.652(3) 1 d D . P A 2
Cl6B Cl 0.41228(19) 0.87245(13) 0.1150(2) 0.0592(7) Uani 0.652(3) 1 d D . P A 2
Cl7B Cl 0.3179(2) 0.72126(19) 0.0313(3) 0.0928(12) Uani 0.652(3) 1 d D . P A 2
C91A C 0.8147(11) 1.0184(11) 0.2784(13) 0.025(6) Uiso 0.33(3) 1 d D . P B 1
H91A H 0.7786 0.9658 0.2644 0.030 Uiso 0.33(3) 1 calc R U P B 1
Cl2A Cl 0.9336(9) 0.9966(10) 0.3064(14) 0.049(3) Uani 0.33(3) 1 d D . P B 1
Cl3A Cl 0.8084(12) 1.0674(8) 0.3969(14) 0.040(2) Uani 0.33(3) 1 d D . P B 1
Cl4A Cl 0.7656(5) 1.0800(7) 0.1578(12) 0.040(3) Uani 0.33(3) 1 d D . P B 1
C91B C 0.8207(8) 1.0154(7) 0.2679(8) 0.041(4) Uiso 0.67(3) 1 d D . P B 2
H91B H 0.7889 0.9608 0.2585 0.049 Uiso 0.67(3) 1 calc R U P B 2
Cl2B Cl 0.9428(6) 1.0001(5) 0.3283(11) 0.059(2) Uani 0.67(3) 1 d D . P B 2
Cl3B Cl 0.7856(6) 1.0761(5) 0.3564(11) 0.0483(16) Uani 0.67(3) 1 d D . P B 2
Cl4B Cl 0.7850(9) 1.0610(6) 0.1343(5) 0.079(2) Uani 0.67(3) 1 d D . P B 2
C1 C 0.4066(3) 0.0890(3) 0.1998(5) 0.0349(12) Uani 1 1 d . . . . .
C3 C 0.5304(4) 0.0406(4) 0.1691(7) 0.065(2) Uani 1 1 d . . . . .
H3 H 0.5882 0.0135 0.1814 0.079 Uiso 1 1 calc R U . . .
C4 C 0.4760(4) 0.0805(3) 0.0764(7) 0.0604(19) Uani 1 1 d . . . . .
H4 H 0.4869 0.0872 0.0096 0.073 Uiso 1 1 calc R U . . .
C6 C 0.5275(4) 0.0074(3) 0.3579(5) 0.064(2) Uani 1 1 d . . . . .
H6A H 0.4898 0.0234 0.4001 0.095 Uiso 1 1 calc R U . . .
H6B H 0.5930 0.0258 0.3990 0.095 Uiso 1 1 calc R U . . .
H6C H 0.5263 -0.0523 0.3498 0.095 Uiso 1 1 calc R U . . .
C7 C 0.3171(4) 0.1513(3) 0.0178(5) 0.0395(13) Uani 1 1 d . . . . .
H7A H 0.2752 0.1116 -0.0380 0.047 Uiso 1 1 calc R U . . .
H7B H 0.3350 0.1944 -0.0237 0.047 Uiso 1 1 calc R U . . .
C8 C 0.2655(3) 0.1893(2) 0.0837(4) 0.0271(10) Uani 1 1 d . . . . .
C9 C 0.3197(3) 0.2409(3) 0.1786(4) 0.0306(11) Uani 1 1 d . . . . .
H9 H 0.3862 0.2493 0.1865 0.037 Uiso 1 1 calc R U . . .
C10 C 0.2794(3) 0.3137(3) 0.2052(4) 0.0291(10) Uani 1 1 d . . . . .
C12 C 0.1313(3) 0.2842(3) 0.0469(4) 0.0294(10) Uani 1 1 d . . . . .
C13 C 0.0411(4) 0.3139(3) -0.0162(4) 0.0371(12) Uani 1 1 d . . . . .
H13 H 0.0174 0.3594 0.0102 0.044 Uiso 1 1 calc R U . . .
C14 C -0.0138(4) 0.2768(3) -0.1177(4) 0.0418(13) Uani 1 1 d . . . . .
H14 H -0.0753 0.2975 -0.1623 0.050 Uiso 1 1 calc R U . . .
C15 C 0.0205(4) 0.2098(3) -0.1543(4) 0.0412(13) Uani 1 1 d . . . . .
C16 C 0.1094(4) 0.1785(3) -0.0893(4) 0.0326(11) Uani 1 1 d . . . . .
H16 H 0.1314 0.1314 -0.1146 0.039 Uiso 1 1 calc R U . . .
C17 C 0.1675(3) 0.2155(3) 0.0136(4) 0.0288(10) Uani 1 1 d . . . . .
C20 C -0.1081(4) 0.2095(3) -0.3345(5) 0.0567(17) Uani 1 1 d . . . . .
H20A H -0.1585 0.2099 -0.3068 0.085 Uiso 1 1 calc R U . . .
H20B H -0.1302 0.1805 -0.4071 0.085 Uiso 1 1 calc R U . . .
H20C H -0.0914 0.2660 -0.3447 0.085 Uiso 1 1 calc R U . . .
C21 C 0.2042(3) 0.1406(3) 0.3358(4) 0.0287(10) Uani 1 1 d . . . . .
H21 H 0.2136 0.1946 0.3756 0.034 Uiso 1 1 calc R U . . .
C22 C 0.1463(3) 0.1444(3) 0.2225(4) 0.0278(10) Uani 1 1 d . . . . .
H22 H 0.1224 0.2008 0.1956 0.033 Uiso 1 1 calc R U . . .
C23 C 0.0798(3) 0.0770(3) 0.1551(4) 0.0342(11) Uani 1 1 d . . . . .
H23A H 0.0241 0.1024 0.0943 0.041 Uiso 1 1 calc R U . . .
H23B H 0.0569 0.0469 0.2057 0.041 Uiso 1 1 calc R U . . .
C24 C 0.1248(3) 0.0156(3) 0.1015(4) 0.0312(11) Uani 1 1 d . . . . .
H24A H 0.0981 -0.0395 0.1020 0.037 Uiso 1 1 calc R U . . .
H24B H 0.1078 0.0313 0.0216 0.037 Uiso 1 1 calc R U . . .
C25 C 0.2306(3) 0.0116(3) 0.1617(4) 0.0274(10) Uani 1 1 d . . . . .
H25 H 0.2616 -0.0155 0.1161 0.033 Uiso 1 1 calc R U . . .
C26 C 0.2800(3) -0.0020(3) 0.2819(4) 0.0281(10) Uani 1 1 d . . . . .
H26 H 0.3381 -0.0367 0.3033 0.034 Uiso 1 1 calc R U . . .
C27 C 0.2274(4) -0.0126(3) 0.3580(4) 0.0380(12) Uani 1 1 d . . . . .
H27A H 0.2621 -0.0524 0.4186 0.046 Uiso 1 1 calc R U . . .
H27B H 0.1638 -0.0357 0.3130 0.046 Uiso 1 1 calc R U . . .
C28 C 0.2162(4) 0.0678(3) 0.4119(4) 0.0362(12) Uani 1 1 d . . . . .
H28A H 0.1604 0.0637 0.4310 0.043 Uiso 1 1 calc R U . . .
H28B H 0.2728 0.0763 0.4833 0.043 Uiso 1 1 calc R U . . .
N2 N 0.4878(3) 0.0453(2) 0.2458(4) 0.0463(12) Uani 1 1 d . . . . .
N5 N 0.4010(3) 0.1101(2) 0.0958(4) 0.0387(10) Uani 1 1 d . . . . .
O11 O 0.1840(2) 0.32812(18) 0.1459(3) 0.0303(7) Uani 1 1 d . . . . .
O18 O 0.3212(2) 0.36507(19) 0.2768(3) 0.0347(8) Uani 1 1 d . . . . .
O19 O -0.0275(3) 0.1692(2) -0.2550(3) 0.0507(10) Uani 1 1 d . . . . .
Cl1 Cl 0.41673(9) 0.16022(8) 0.43287(11) 0.0427(3) Uani 1 1 d . . . . .
Ir1 Ir 0.29863(2) 0.12185(2) 0.24078(2) 0.02341(5) Uani 1 1 d . . . . .


_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
C92A Cl6A 1.739(10) . ?
C92A Cl5A 1.750(10) . ?
C92A Cl7A 1.759(11) . ?
C92A H92A 1.0000 . ?
C92B Cl6B 1.712(7) . ?
C92B Cl5B 1.743(8) . ?
C92B Cl7B 1.745(7) . ?
C92B H92B 1.0000 . ?
C91A Cl4A 1.748(12) . ?
C91A Cl2A 1.757(12) . ?
C91A Cl3A 1.764(12) . ?
C91A H91A 1.0000 . ?
C91B Cl2B 1.741(9) . ?
C91B Cl4B 1.750(9) . ?
C91B Cl3B 1.756(9) . ?
C91B H91B 1.0000 . ?
C1 N2 1.352(6) . ?
C1 N5 1.355(7) . ?
C1 Ir1 2.015(5) . ?
C3 C4 1.322(9) . ?
C3 N2 1.395(8) . ?
C3 H3 0.9500 . ?
C4 N5 1.369(6) . ?
C4 H4 0.9500 . ?
C6 N2 1.461(7) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 N5 1.445(6) . ?
C7 C8 1.514(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.441(6) . ?
C8 C17 1.477(6) . ?
C8 Ir1 2.179(4) . ?
C9 C10 1.446(6) . ?
C9 Ir1 2.176(4) . ?
C9 H9 1.0000 . ?
C10 O18 1.221(5) . ?
C10 O11 1.377(5) . ?
C12 C13 1.384(6) . ?
C12 C17 1.396(6) . ?
C12 O11 1.403(5) . ?
C13 C14 1.380(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.380(7) . ?
C14 H14 0.9500 . ?
C15 O19 1.379(6) . ?
C15 C16 1.384(7) . ?
C16 C17 1.403(6) . ?
C16 H16 0.9500 . ?
C20 O19 1.414(6) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.373(6) . ?
C21 C28 1.506(6) . ?
C21 Ir1 2.274(4) . ?
C21 H21 1.0000 . ?
C22 C23 1.515(6) . ?
C22 Ir1 2.296(4) . ?
C22 H22 1.0000 . ?
C23 C24 1.534(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.500(6) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.442(6) . ?
C25 Ir1 2.125(4) . ?
C25 H25 1.0000 . ?
C26 C27 1.518(7) . ?
C26 Ir1 2.138(4) . ?
C26 H26 1.0000 . ?
C27 C28 1.528(6) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
Cl1 Ir1 2.4917(12) . ?

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
Cl6A C92A Cl5A 110.4(7) . . ?
Cl6A C92A Cl7A 113.3(7) . . ?
Cl5A C92A Cl7A 112.2(6) . . ?
Cl6A C92A H92A 106.8 . . ?
Cl5A C92A H92A 106.8 . . ?
Cl7A C92A H92A 106.8 . . ?
Cl6B C92B Cl5B 111.5(5) . . ?
Cl6B C92B Cl7B 110.9(4) . . ?
Cl5B C92B Cl7B 111.7(4) . . ?
Cl6B C92B H92B 107.5 . . ?
Cl5B C92B H92B 107.5 . . ?
Cl7B C92B H92B 107.5 . . ?
Cl4A C91A Cl2A 109.8(9) . . ?
Cl4A C91A Cl3A 110.9(8) . . ?
Cl2A C91A Cl3A 109.5(9) . . ?
Cl4A C91A H91A 108.9 . . ?
Cl2A C91A H91A 108.9 . . ?
Cl3A C91A H91A 108.9 . . ?
Cl2B C91B Cl4B 110.8(6) . . ?
Cl2B C91B Cl3B 110.6(6) . . ?
Cl4B C91B Cl3B 110.2(5) . . ?
Cl2B C91B H91B 108.4 . . ?
Cl4B C91B H91B 108.4 . . ?
Cl3B C91B H91B 108.4 . . ?
N2 C1 N5 104.2(4) . . ?
N2 C1 Ir1 138.0(4) . . ?
N5 C1 Ir1 117.7(3) . . ?
C4 C3 N2 107.9(5) . . ?
C4 C3 H3 126.1 . . ?
N2 C3 H3 126.1 . . ?
C3 C4 N5 106.4(6) . . ?
C3 C4 H4 126.8 . . ?
N5 C4 H4 126.8 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N5 C7 C8 109.0(4) . . ?
N5 C7 H7A 109.9 . . ?
C8 C7 H7A 109.9 . . ?
N5 C7 H7B 109.9 . . ?
C8 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
C9 C8 C17 116.8(4) . . ?
C9 C8 C7 117.5(4) . . ?
C17 C8 C7 114.5(4) . . ?
C9 C8 Ir1 70.5(3) . . ?
C17 C8 Ir1 120.8(3) . . ?
C7 C8 Ir1 109.8(3) . . ?
C8 C9 C10 121.6(4) . . ?
C8 C9 Ir1 70.8(2) . . ?
C10 C9 Ir1 120.2(3) . . ?
C8 C9 H9 112.7 . . ?
C10 C9 H9 112.7 . . ?
Ir1 C9 H9 112.7 . . ?
O18 C10 O11 114.9(4) . . ?
O18 C10 C9 126.7(4) . . ?
O11 C10 C9 118.3(4) . . ?
C13 C12 C17 122.2(4) . . ?
C13 C12 O11 115.5(4) . . ?
C17 C12 O11 122.3(4) . . ?
C14 C13 C12 119.4(4) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 120.0(5) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
O19 C15 C14 124.8(5) . . ?
O19 C15 C16 114.6(4) . . ?
C14 C15 C16 120.6(5) . . ?
C15 C16 C17 120.8(4) . . ?
C15 C16 H16 119.6 . . ?
C17 C16 H16 119.6 . . ?
C12 C17 C16 117.1(4) . . ?
C12 C17 C8 118.8(4) . . ?
C16 C17 C8 124.0(4) . . ?
O19 C20 H20A 109.5 . . ?
O19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C28 125.9(4) . . ?
C22 C21 Ir1 73.4(2) . . ?
C28 C21 Ir1 108.0(3) . . ?
C22 C21 H21 113.9 . . ?
C28 C21 H21 113.9 . . ?
Ir1 C21 H21 113.9 . . ?
C21 C22 C23 125.3(4) . . ?
C21 C22 Ir1 71.6(3) . . ?
C23 C22 Ir1 111.7(3) . . ?
C21 C22 H22 113.6 . . ?
C23 C22 H22 113.6 . . ?
Ir1 C22 H22 113.6 . . ?
C22 C23 C24 114.1(4) . . ?
C22 C23 H23A 108.7 . . ?
C24 C23 H23A 108.7 . . ?
C22 C23 H23B 108.7 . . ?
C24 C23 H23B 108.7 . . ?
H23A C23 H23B 107.6 . . ?
C25 C24 C23 113.1(4) . . ?
C25 C24 H24A 109.0 . . ?
C23 C24 H24A 109.0 . . ?
C25 C24 H24B 109.0 . . ?
C23 C24 H24B 109.0 . . ?
H24A C24 H24B 107.8 . . ?
C26 C25 C24 123.7(4) . . ?
C26 C25 Ir1 70.7(2) . . ?
C24 C25 Ir1 115.7(3) . . ?
C26 C25 H25 113.3 . . ?
C24 C25 H25 113.3 . . ?
Ir1 C25 H25 113.3 . . ?
C25 C26 C27 121.7(4) . . ?
C25 C26 Ir1 69.7(2) . . ?
C27 C26 Ir1 115.5(3) . . ?
C25 C26 H26 114.2 . . ?
C27 C26 H26 114.2 . . ?
Ir1 C26 H26 114.2 . . ?
C26 C27 C28 112.7(4) . . ?
C26 C27 H27A 109.1 . . ?
C28 C27 H27A 109.1 . . ?
C26 C27 H27B 109.1 . . ?
C28 C27 H27B 109.1 . . ?
H27A C27 H27B 107.8 . . ?
C21 C28 C27 112.8(4) . . ?
C21 C28 H28A 109.0 . . ?
C27 C28 H28A 109.0 . . ?
C21 C28 H28B 109.0 . . ?
C27 C28 H28B 109.0 . . ?
H28A C28 H28B 107.8 . . ?
C1 N2 C3 109.7(5) . . ?
C1 N2 C6 126.9(5) . . ?
C3 N2 C6 123.4(5) . . ?
C1 N5 C4 111.8(5) . . ?
C1 N5 C7 119.3(4) . . ?
C4 N5 C7 128.5(5) . . ?
C10 O11 C12 121.0(3) . . ?
C15 O19 C20 116.1(4) . . ?
C1 Ir1 C25 87.07(18) . . ?
C1 Ir1 C26 91.27(18) . . ?
C25 Ir1 C26 39.55(16) . . ?
C1 Ir1 C9 82.97(18) . . ?
C25 Ir1 C9 134.19(18) . . ?
C26 Ir1 C9 172.08(18) . . ?
C1 Ir1 C8 78.31(19) . . ?
C25 Ir1 C8 95.55(17) . . ?
C26 Ir1 C8 134.77(16) . . ?
C9 Ir1 C8 38.65(17) . . ?
C1 Ir1 C21 163.04(19) . . ?
C25 Ir1 C21 94.22(17) . . ?
C26 Ir1 C21 79.27(17) . . ?
C9 Ir1 C21 107.62(17) . . ?
C8 Ir1 C21 118.29(16) . . ?
C1 Ir1 C22 159.62(18) . . ?
C25 Ir1 C22 78.46(17) . . ?
C26 Ir1 C22 86.68(17) . . ?
C9 Ir1 C22 96.82(16) . . ?
C8 Ir1 C22 88.79(16) . . ?
C21 Ir1 C22 34.96(15) . . ?
C1 Ir1 Cl1 88.78(15) . . ?
C25 Ir1 Cl1 135.34(13) . . ?
C26 Ir1 Cl1 96.20(12) . . ?
C9 Ir1 Cl1 89.14(13) . . ?
C8 Ir1 Cl1 126.95(12) . . ?
C21 Ir1 Cl1 78.41(12) . . ?
C22 Ir1 Cl1 111.60(12) . . ?

_refine_diff_density_max         0.789
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.132



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound_5b_VPX101_OKZ137
_database_code_depnum_ccdc_archive 'CCDC 2083330'
loop_
_audit_author_name
_audit_author_address
'Vincenzo Passarelli'
;Instituto de Sintesis Quimica y Catalisis Homogenea (CSIC)
Spain
;
_audit_update_record             
;
2021-05-12 deposited with the CCDC.	2021-07-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C35 H36 Cl Ir N2 O2, 1.75 (C H Cl3)'
_chemical_formula_sum            'C36.75 H37.75 Cl6.25 Ir N2 O2'
_chemical_formula_weight         953.20

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   15.4666(9)
_cell_length_b                   14.5473(9)
_cell_length_c                   15.8594(9)
_cell_angle_alpha                90
_cell_angle_beta                 96.0530(10)
_cell_angle_gamma                90
_cell_volume                     3548.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8648
_cell_measurement_theta_min      2.240
_cell_measurement_theta_max      28.126

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_F_000             1886
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    4.271
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4667
_exptl_absorpt_correction_T_max  0.6036
_exptl_absorpt_process_details   
; 
 Multi-scan correction included in APEX2 package (Bruker AXS, 2008)
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       'ω rotations with narrow frames'
_diffrn_detector_area_resol_mean 8.26
_diffrn_reflns_number            43969
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.927
_diffrn_reflns_theta_max         28.550
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8481
_reflns_number_gt                6650
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART in APEX2 (Bruker AXS,2008)'
_computing_cell_refinement       'SAINT+ in APEX2 (Bruker AXS,2008)'
_computing_data_reduction        'SAINT+ in APEX2 (Bruker AXS,2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'

_refine_special_details          
;
 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 structure was solved by the Patterson method and anisotropic refinement
 was applied to all non hydrogen atoms. The hydrogen atoms were included
 in calculated positions and refined with a riding model. Four lattice 
 chloroform molecules were also found in the cell (one per asymmetric unit).

 Significant residual electron density was observed but it could not be
 included in the model as disordered solvent molecules. Therefore it was
 treated using the program SQUEEZE (Platon). Two solvent accessible voids
 (2x206 ang^3 per unit cell) were found and 190 residual electrons were
 calculated. On these bases three additional chloroform molecules (per cell)
 should be present. These molecules have been included in the chemical
 formula, F00 and density. Results of the SQUEEZE calculations are included
 at the end of this cif file.

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0350P)²+13.0640P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8481
_refine_ls_number_parameters     409
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_ref         0.0885
_refine_ls_wR_factor_gt          0.0811
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7941(3) 0.0249(3) 0.9068(3) 0.0149(9) Uani 1 1 d . . . . .
C3 C 0.9039(3) -0.0757(3) 0.8956(3) 0.0168(10) Uani 1 1 d . . . . .
C4 C 0.9665(3) -0.1339(3) 0.8679(3) 0.0180(10) Uani 1 1 d . . . . .
H4 H 0.9720 -0.1429 0.8094 0.022 Uiso 1 1 calc R U . . .
C5 C 1.0203(3) -0.1779(3) 0.9304(3) 0.0200(10) Uani 1 1 d . . . . .
H5 H 1.0637 -0.2186 0.9142 0.024 Uiso 1 1 calc R U . . .
C6 C 1.0130(3) -0.1644(3) 1.0168(3) 0.0212(11) Uani 1 1 d . . . . .
H6 H 1.0516 -0.1957 1.0577 0.025 Uiso 1 1 calc R U . . .
C7 C 0.9499(3) -0.1056(3) 1.0439(3) 0.0190(10) Uani 1 1 d . . . . .
H7 H 0.9446 -0.0957 1.1023 0.023 Uiso 1 1 calc R U . . .
C8 C 0.8956(3) -0.0625(3) 0.9808(3) 0.0161(10) Uani 1 1 d . . . . .
C10 C 0.8161(3) -0.0138(3) 0.7612(3) 0.0149(9) Uani 1 1 d . . . . .
H10A H 0.7798 -0.0672 0.7414 0.018 Uiso 1 1 calc R U . . .
H10B H 0.8685 -0.0131 0.7304 0.018 Uiso 1 1 calc R U . . .
C11 C 0.7648(3) 0.0751(3) 0.7443(3) 0.0163(10) Uani 1 1 d . . . . .
C12 C 0.8022(3) 0.1580(3) 0.7818(3) 0.0161(9) Uani 1 1 d . . . . .
H12 H 0.8621 0.1489 0.8110 0.019 Uiso 1 1 calc R U . . .
C13 C 0.7917(3) 0.2456(3) 0.7372(3) 0.0181(10) Uani 1 1 d . . . . .
C15 C 0.7101(3) 0.1686(3) 0.6196(3) 0.0174(10) Uani 1 1 d . . . . .
C16 C 0.6703(3) 0.1809(3) 0.5391(3) 0.0232(11) Uani 1 1 d . . . . .
H16 H 0.6649 0.2409 0.5156 0.028 Uiso 1 1 calc R U . . .
C17 C 0.6377(3) 0.1060(4) 0.4916(3) 0.0239(11) Uani 1 1 d . . . . .
C18 C 0.6457(4) 0.0180(4) 0.5280(3) 0.0233(11) Uani 1 1 d . . . . .
C19 C 0.6866(3) 0.0074(3) 0.6091(3) 0.0192(10) Uani 1 1 d . . . . .
H19 H 0.6927 -0.0527 0.6324 0.023 Uiso 1 1 calc R U . . .
C20 C 0.7193(3) 0.0819(3) 0.6580(3) 0.0164(10) Uani 1 1 d . . . . .
C22 C 0.5946(4) 0.1198(4) 0.4018(4) 0.0361(14) Uani 1 1 d . . . . .
H22A H 0.5336 0.1006 0.3988 0.054 Uiso 1 1 calc R U . . .
H22B H 0.6248 0.0827 0.3624 0.054 Uiso 1 1 calc R U . . .
H22C H 0.5976 0.1848 0.3864 0.054 Uiso 1 1 calc R U . . .
C23 C 0.6112(4) -0.0659(4) 0.4784(4) 0.0295(13) Uani 1 1 d . . . . .
H23A H 0.5481 -0.0604 0.4652 0.044 Uiso 1 1 calc R U . . .
H23B H 0.6246 -0.1213 0.5125 0.044 Uiso 1 1 calc R U . . .
H23C H 0.6386 -0.0702 0.4256 0.044 Uiso 1 1 calc R U . . .
C24 C 0.7961(3) 0.0266(3) 1.0655(3) 0.0175(10) Uani 1 1 d . . . . .
H24A H 0.7493 0.0728 1.0541 0.021 Uiso 1 1 calc R U . . .
H24B H 0.8446 0.0562 1.1013 0.021 Uiso 1 1 calc R U . . .
C25 C 0.7618(3) -0.0539(3) 1.1138(3) 0.0204(10) Uani 1 1 d . . . . .
C26 C 0.7281(3) -0.1327(3) 1.0730(3) 0.0217(11) Uani 1 1 d . . . . .
H26 H 0.7243 -0.1366 1.0129 0.026 Uiso 1 1 calc R U . . .
C27 C 0.6997(4) -0.2059(4) 1.1195(4) 0.0270(12) Uani 1 1 d . . . . .
H27 H 0.6778 -0.2596 1.0908 0.032 Uiso 1 1 calc R U . . .
C28 C 0.7030(4) -0.2015(4) 1.2074(4) 0.0303(13) Uani 1 1 d . . . . .
C29 C 0.7355(4) -0.1220(4) 1.2474(4) 0.0314(13) Uani 1 1 d . . . . .
H29 H 0.7375 -0.1172 1.3074 0.038 Uiso 1 1 calc R U . . .
C30 C 0.7648(4) -0.0495(4) 1.2018(3) 0.0281(12) Uani 1 1 d . . . . .
H30 H 0.7873 0.0039 1.2307 0.034 Uiso 1 1 calc R U . . .
C31 C 0.6718(5) -0.2812(5) 1.2569(5) 0.0472(18) Uani 1 1 d . . . . .
H31A H 0.6915 -0.2732 1.3172 0.071 Uiso 1 1 calc R U . . .
H31B H 0.6956 -0.3387 1.2366 0.071 Uiso 1 1 calc R U . . .
H31C H 0.6082 -0.2837 1.2490 0.071 Uiso 1 1 calc R U . . .
C32 C 0.5956(3) 0.2203(3) 0.8419(3) 0.0190(10) Uani 1 1 d . . . . .
H32 H 0.6183 0.2840 0.8356 0.023 Uiso 1 1 calc R U . . .
C33 C 0.5879(3) 0.1701(3) 0.7678(3) 0.0197(10) Uani 1 1 d . . . . .
H33 H 0.6067 0.2042 0.7181 0.024 Uiso 1 1 calc R U . . .
C34 C 0.5181(3) 0.0982(3) 0.7441(4) 0.0249(11) Uani 1 1 d . . . . .
H34A H 0.5039 0.0984 0.6817 0.030 Uiso 1 1 calc R U . . .
H34B H 0.4648 0.1156 0.7698 0.030 Uiso 1 1 calc R U . . .
C35 C 0.5444(3) 0.0002(4) 0.7726(4) 0.0251(11) Uani 1 1 d . . . . .
H35A H 0.4919 -0.0335 0.7859 0.030 Uiso 1 1 calc R U . . .
H35B H 0.5682 -0.0321 0.7252 0.030 Uiso 1 1 calc R U . . .
C36 C 0.6114(3) -0.0021(3) 0.8498(3) 0.0199(11) Uani 1 1 d . . . . .
H36 H 0.6401 -0.0633 0.8599 0.024 Uiso 1 1 calc R U . . .
C37 C 0.6025(3) 0.0484(3) 0.9259(3) 0.0205(10) Uani 1 1 d . . . . .
H37 H 0.6263 0.0161 0.9790 0.025 Uiso 1 1 calc R U . . .
C38 C 0.5242(3) 0.1085(4) 0.9361(3) 0.0234(11) Uani 1 1 d . . . . .
H38A H 0.5099 0.1043 0.9953 0.028 Uiso 1 1 calc R U . . .
H38B H 0.4737 0.0852 0.8986 0.028 Uiso 1 1 calc R U . . .
C39 C 0.5402(3) 0.2094(3) 0.9144(3) 0.0229(11) Uani 1 1 d . . . . .
H39A H 0.4835 0.2400 0.8991 0.027 Uiso 1 1 calc R U . . .
H39B H 0.5691 0.2407 0.9652 0.027 Uiso 1 1 calc R U . . .
C40 C 0.9949(5) 0.7421(5) 0.3196(4) 0.0461(17) Uani 1 1 d . . . . .
H40 H 1.0224 0.6984 0.2818 0.055 Uiso 1 1 calc R U . . .
N2 N 0.8412(3) -0.0208(3) 0.8521(2) 0.0152(8) Uani 1 1 d . . . . .
N9 N 0.8264(3) -0.0014(3) 0.9856(2) 0.0158(8) Uani 1 1 d . . . . .
O14 O 0.7397(2) 0.2493(2) 0.6622(2) 0.0196(7) Uani 1 1 d . . . . .
O21 O 0.8265(2) 0.3170(2) 0.7621(2) 0.0228(8) Uani 1 1 d . . . . .
Cl1 Cl 0.75408(8) 0.22359(8) 0.96936(8) 0.0203(2) Uani 1 1 d . . . . .
Cl2 Cl 0.97218(15) 0.8447(2) 0.26497(15) 0.0845(8) Uani 1 1 d . . . . .
Cl3 Cl 1.06941(11) 0.76464(13) 0.41012(10) 0.0448(4) Uani 1 1 d . . . . .
Cl4 Cl 0.89978(11) 0.69272(16) 0.34882(13) 0.0579(5) Uani 1 1 d . . . . .
Ir1 Ir 0.70077(2) 0.11093(2) 0.85666(2) 0.01423(6) Uani 1 1 d . . . . .


_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
C1 N9 1.351(6) . ?
C1 N2 1.363(6) . ?
C1 Ir1 2.010(5) . ?
C3 C8 1.384(7) . ?
C3 N2 1.385(6) . ?
C3 C4 1.391(7) . ?
C4 C5 1.382(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.401(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.399(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.387(7) . ?
C7 H7 0.9500 . ?
C8 N9 1.399(6) . ?
C10 N2 1.455(6) . ?
C10 C11 1.525(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.439(6) . ?
C11 C20 1.476(7) . ?
C11 Ir1 2.191(5) . ?
C12 C13 1.458(7) . ?
C12 Ir1 2.175(5) . ?
C12 H12 1.0000 . ?
C13 O21 1.216(6) . ?
C13 O14 1.366(6) . ?
C15 C16 1.370(7) . ?
C15 C20 1.401(6) . ?
C15 O14 1.406(6) . ?
C16 C17 1.389(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.405(7) . ?
C17 C22 1.520(7) . ?
C18 C19 1.381(7) . ?
C18 C23 1.518(7) . ?
C19 C20 1.396(7) . ?
C19 H19 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 N9 1.456(6) . ?
C24 C25 1.524(7) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.391(7) . ?
C25 C30 1.392(7) . ?
C26 C27 1.392(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.390(8) . ?
C27 H27 0.9500 . ?
C28 C29 1.388(8) . ?
C28 C31 1.508(7) . ?
C29 C30 1.383(7) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.378(7) . ?
C32 C39 1.512(7) . ?
C32 Ir1 2.269(5) . ?
C32 H32 1.0000 . ?
C33 C34 1.522(7) . ?
C33 Ir1 2.293(5) . ?
C33 H33 1.0000 . ?
C34 C35 1.537(7) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.519(7) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.432(7) . ?
C36 Ir1 2.143(5) . ?
C36 H36 1.0000 . ?
C37 C38 1.515(7) . ?
C37 Ir1 2.166(5) . ?
C37 H37 1.0000 . ?
C38 C39 1.535(7) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 Cl2 1.743(7) . ?
C40 Cl4 1.743(7) . ?
C40 Cl3 1.774(7) . ?
C40 H40 1.0000 . ?
Cl1 Ir1 2.4999(12) . ?

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
N9 C1 N2 106.3(4) . . ?
N9 C1 Ir1 136.3(4) . . ?
N2 C1 Ir1 117.4(3) . . ?
C8 C3 N2 105.9(4) . . ?
C8 C3 C4 122.2(4) . . ?
N2 C3 C4 131.9(5) . . ?
C5 C4 C3 116.2(5) . . ?
C5 C4 H4 121.9 . . ?
C3 C4 H4 121.9 . . ?
C4 C5 C6 122.1(5) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C7 C6 C5 121.1(5) . . ?
C7 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
C8 C7 C6 116.4(5) . . ?
C8 C7 H7 121.8 . . ?
C6 C7 H7 121.8 . . ?
C3 C8 C7 122.0(5) . . ?
C3 C8 N9 107.0(4) . . ?
C7 C8 N9 131.1(4) . . ?
N2 C10 C11 108.2(4) . . ?
N2 C10 H10A 110.1 . . ?
C11 C10 H10A 110.1 . . ?
N2 C10 H10B 110.1 . . ?
C11 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
C12 C11 C20 117.3(4) . . ?
C12 C11 C10 117.3(4) . . ?
C20 C11 C10 114.1(4) . . ?
C12 C11 Ir1 70.2(3) . . ?
C20 C11 Ir1 121.7(3) . . ?
C10 C11 Ir1 109.3(3) . . ?
C11 C12 C13 120.9(4) . . ?
C11 C12 Ir1 71.3(3) . . ?
C13 C12 Ir1 119.4(3) . . ?
C11 C12 H12 113.0 . . ?
C13 C12 H12 113.0 . . ?
Ir1 C12 H12 113.0 . . ?
O21 C13 O14 116.7(4) . . ?
O21 C13 C12 124.5(5) . . ?
O14 C13 C12 118.8(4) . . ?
C16 C15 C20 122.5(4) . . ?
C16 C15 O14 115.5(4) . . ?
C20 C15 O14 122.0(4) . . ?
C15 C16 C17 120.4(5) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C16 C17 C18 118.7(5) . . ?
C16 C17 C22 120.2(5) . . ?
C18 C17 C22 121.1(5) . . ?
C19 C18 C17 119.8(5) . . ?
C19 C18 C23 119.6(5) . . ?
C17 C18 C23 120.6(5) . . ?
C18 C19 C20 122.3(5) . . ?
C18 C19 H19 118.8 . . ?
C20 C19 H19 118.8 . . ?
C19 C20 C15 116.3(4) . . ?
C19 C20 C11 124.9(4) . . ?
C15 C20 C11 118.7(4) . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C23 H23A 109.5 . . ?
C18 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C18 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N9 C24 C25 112.5(4) . . ?
N9 C24 H24A 109.1 . . ?
C25 C24 H24A 109.1 . . ?
N9 C24 H24B 109.1 . . ?
C25 C24 H24B 109.1 . . ?
H24A C24 H24B 107.8 . . ?
C26 C25 C30 118.3(5) . . ?
C26 C25 C24 122.2(5) . . ?
C30 C25 C24 119.5(5) . . ?
C25 C26 C27 120.5(5) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C28 C27 C26 121.1(5) . . ?
C28 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
C29 C28 C27 118.0(5) . . ?
C29 C28 C31 121.5(6) . . ?
C27 C28 C31 120.5(6) . . ?
C30 C29 C28 121.2(5) . . ?
C30 C29 H29 119.4 . . ?
C28 C29 H29 119.4 . . ?
C29 C30 C25 120.8(5) . . ?
C29 C30 H30 119.6 . . ?
C25 C30 H30 119.6 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 C39 126.0(5) . . ?
C33 C32 Ir1 73.4(3) . . ?
C39 C32 Ir1 107.9(3) . . ?
C33 C32 H32 113.9 . . ?
C39 C32 H32 113.9 . . ?
Ir1 C32 H32 113.9 . . ?
C32 C33 C34 124.8(5) . . ?
C32 C33 Ir1 71.5(3) . . ?
C34 C33 Ir1 111.6(3) . . ?
C32 C33 H33 113.8 . . ?
C34 C33 H33 113.8 . . ?
Ir1 C33 H33 113.8 . . ?
C33 C34 C35 113.9(4) . . ?
C33 C34 H34A 108.8 . . ?
C35 C34 H34A 108.8 . . ?
C33 C34 H34B 108.8 . . ?
C35 C34 H34B 108.8 . . ?
H34A C34 H34B 107.7 . . ?
C36 C35 C34 113.3(4) . . ?
C36 C35 H35A 108.9 . . ?
C34 C35 H35A 108.9 . . ?
C36 C35 H35B 108.9 . . ?
C34 C35 H35B 108.9 . . ?
H35A C35 H35B 107.7 . . ?
C37 C36 C35 123.3(4) . . ?
C37 C36 Ir1 71.5(3) . . ?
C35 C36 Ir1 113.9(3) . . ?
C37 C36 H36 113.7 . . ?
C35 C36 H36 113.7 . . ?
Ir1 C36 H36 113.7 . . ?
C36 C37 C38 122.3(5) . . ?
C36 C37 Ir1 69.7(3) . . ?
C38 C37 Ir1 115.0(3) . . ?
C36 C37 H37 114.1 . . ?
C38 C37 H37 114.1 . . ?
Ir1 C37 H37 114.1 . . ?
C37 C38 C39 112.3(4) . . ?
C37 C38 H38A 109.2 . . ?
C39 C38 H38A 109.2 . . ?
C37 C38 H38B 109.2 . . ?
C39 C38 H38B 109.2 . . ?
H38A C38 H38B 107.9 . . ?
C32 C39 C38 112.8(4) . . ?
C32 C39 H39A 109.0 . . ?
C38 C39 H39A 109.0 . . ?
C32 C39 H39B 109.0 . . ?
C38 C39 H39B 109.0 . . ?
H39A C39 H39B 107.8 . . ?
Cl2 C40 Cl4 110.7(4) . . ?
Cl2 C40 Cl3 108.9(4) . . ?
Cl4 C40 Cl3 110.9(4) . . ?
Cl2 C40 H40 108.8 . . ?
Cl4 C40 H40 108.8 . . ?
Cl3 C40 H40 108.8 . . ?
C1 N2 C3 110.9(4) . . ?
C1 N2 C10 119.5(4) . . ?
C3 N2 C10 129.3(4) . . ?
C1 N9 C8 109.9(4) . . ?
C1 N9 C24 127.2(4) . . ?
C8 N9 C24 122.9(4) . . ?
C13 O14 C15 121.2(4) . . ?
C1 Ir1 C36 88.53(19) . . ?
C1 Ir1 C37 92.91(19) . . ?
C36 Ir1 C37 38.81(19) . . ?
C1 Ir1 C12 83.30(18) . . ?
C36 Ir1 C12 135.41(18) . . ?
C37 Ir1 C12 173.46(18) . . ?
C1 Ir1 C11 78.82(19) . . ?
C36 Ir1 C11 96.91(18) . . ?
C37 Ir1 C11 135.53(18) . . ?
C12 Ir1 C11 38.50(17) . . ?
C1 Ir1 C32 162.58(19) . . ?
C36 Ir1 C32 94.66(18) . . ?
C37 Ir1 C32 79.21(18) . . ?
C12 Ir1 C32 105.86(18) . . ?
C11 Ir1 C32 117.64(18) . . ?
C1 Ir1 C33 161.00(18) . . ?
C36 Ir1 C33 79.15(19) . . ?
C37 Ir1 C33 86.53(19) . . ?
C12 Ir1 C33 95.31(18) . . ?
C11 Ir1 C33 88.28(18) . . ?
C32 Ir1 C33 35.16(17) . . ?
C1 Ir1 Cl1 87.51(13) . . ?
C36 Ir1 Cl1 134.56(14) . . ?
C37 Ir1 Cl1 96.26(14) . . ?
C12 Ir1 Cl1 88.92(13) . . ?
C11 Ir1 Cl1 126.45(13) . . ?
C32 Ir1 Cl1 78.05(13) . . ?
C33 Ir1 Cl1 111.45(13) . . ?

_refine_diff_density_max         1.576
_refine_diff_density_min         -1.175
_refine_diff_density_rms         0.149




