# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_Ir-Me-Campy
_database_code_depnum_ccdc_archive 'CCDC 1414409'
_audit_update_record             
;
2015-10-31 deposited with the CCDC.
2015-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C32 H30 Cl Ir N4, H2 O'
_chemical_formula_sum            'C32 H32 Cl Ir N4 O'
_chemical_melting_point          ?

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            orange

_diffrn_ambient_temperature      298(2)
_chemical_formula_weight         716.27
_chemical_absolute_configuration rm

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'
Cl Cl 0.1484 0.1585 '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'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'

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

_cell_length_a                   10.662(3)
_cell_length_b                   14.595(3)
_cell_length_c                   18.403(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2863.7(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9823
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      26.17
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1416
_exptl_absorpt_coefficient_mu    4.788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7420
_exptl_absorpt_correction_T_max  0.9897
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            31815
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.21
_diffrn_reflns_theta_max         26.18
_reflns_number_total             5716
_reflns_number_gt                5421
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
;

_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)+(0.0245P)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     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(5)
_refine_ls_number_reflns         5716
_refine_ls_number_parameters     354
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0183
_refine_ls_wR_factor_ref         0.0457
_refine_ls_wR_factor_gt          0.0444
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_restrained_S_all      0.957
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001

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
Ir Ir 0.409046(12) 0.098339(8) 0.816825(6) 0.02874(4) Uani 1 1 d . . .
N1 N 0.4022(3) 0.03435(18) 0.71734(15) 0.0344(6) Uani 1 1 d . . .
N2 N 0.4201(3) 0.17452(18) 0.91151(15) 0.0317(6) Uani 1 1 d . . .
N3 N 0.4871(3) -0.0283(2) 0.86186(17) 0.0360(7) Uani 1 1 d . . .
H3A H 0.4960 -0.0697 0.8260 0.043 Uiso 1 1 calc R . .
H3B H 0.5636 -0.0167 0.8804 0.043 Uiso 1 1 calc R . .
N4 N 0.2393(3) 0.02515(18) 0.86089(14) 0.0323(6) Uani 1 1 d . . .
Cl Cl 0.71806(10) -0.03284(7) 0.97985(6) 0.0509(2) Uani 1 1 d . . .
O1 O 0.5108(14) -0.0213(9) 1.1084(6) 0.283(5) Uiso 1 1 d D . .
H1W H 0.519(15) -0.085(3) 1.126(7) 0.340 Uiso 1 1 d D . .
H2W H 0.524(15) 0.019(7) 1.151(5) 0.340 Uiso 1 1 d D . .
C1 C 0.3071(4) -0.0197(3) 0.6927(2) 0.0437(9) Uani 1 1 d . . .
H1A H 0.2397 -0.0312 0.7235 0.052 Uiso 1 1 calc R . .
C2 C 0.3061(4) -0.0586(3) 0.6237(2) 0.0499(10) Uani 1 1 d . . .
H2A H 0.2387 -0.0942 0.6085 0.060 Uiso 1 1 calc R . .
C3 C 0.4069(5) -0.0433(3) 0.5782(2) 0.0503(10) Uani 1 1 d . . .
H3C H 0.4087 -0.0689 0.5319 0.060 Uiso 1 1 calc R . .
C4 C 0.5057(4) 0.0107(3) 0.6024(2) 0.0455(10) Uani 1 1 d . . .
H4A H 0.5745 0.0206 0.5724 0.055 Uiso 1 1 calc R . .
C5 C 0.5024(3) 0.0506(2) 0.6719(2) 0.0345(8) Uani 1 1 d . . .
C6 C 0.6002(3) 0.1104(2) 0.70373(18) 0.0339(7) Uani 1 1 d . . .
C7 C 0.7115(4) 0.1341(3) 0.6665(2) 0.0441(9) Uani 1 1 d . . .
H7A H 0.7283 0.1099 0.6208 0.053 Uiso 1 1 calc R . .
C8 C 0.7954(4) 0.1942(3) 0.6994(2) 0.0505(11) Uani 1 1 d . . .
H8A H 0.8686 0.2109 0.6752 0.061 Uiso 1 1 calc R . .
C9 C 0.7705(4) 0.2297(3) 0.7684(2) 0.0495(10) Uani 1 1 d . . .
H9A H 0.8269 0.2701 0.7898 0.059 Uiso 1 1 calc R . .
C10 C 0.6596(4) 0.2045(3) 0.8058(2) 0.0447(9) Uani 1 1 d . . .
H10A H 0.6443 0.2282 0.8519 0.054 Uiso 1 1 calc R . .
C11 C 0.5722(3) 0.1440(2) 0.77428(19) 0.0331(8) Uani 1 1 d . . .
C12 C 0.4808(4) 0.1496(3) 0.9731(2) 0.0388(9) Uani 1 1 d . . .
H12A H 0.5285 0.0963 0.9729 0.047 Uiso 1 1 calc R . .
C13 C 0.4742(4) 0.2009(3) 1.0365(2) 0.0486(10) Uani 1 1 d . . .
H13A H 0.5175 0.1825 1.0779 0.058 Uiso 1 1 calc R . .
C14 C 0.4017(4) 0.2804(3) 1.0373(2) 0.0487(10) Uani 1 1 d . . .
H14A H 0.3921 0.3139 1.0800 0.058 Uiso 1 1 calc R . .
C15 C 0.3442(4) 0.3087(3) 0.9739(2) 0.0442(9) Uani 1 1 d . . .
H15A H 0.2977 0.3626 0.9734 0.053 Uiso 1 1 calc R . .
C16 C 0.3558(3) 0.2566(2) 0.9106(2) 0.0337(8) Uani 1 1 d . . .
C17 C 0.3112(3) 0.2834(2) 0.8380(2) 0.0375(8) Uani 1 1 d . . .
C18 C 0.2569(4) 0.3690(3) 0.8233(3) 0.0555(11) Uani 1 1 d . . .
H18A H 0.2420 0.4102 0.8609 0.067 Uiso 1 1 calc R . .
C19 C 0.2255(5) 0.3921(3) 0.7522(3) 0.0636(13) Uani 1 1 d . . .
H19A H 0.1866 0.4477 0.7422 0.076 Uiso 1 1 calc R . .
C20 C 0.2526(4) 0.3316(3) 0.6961(2) 0.0575(12) Uani 1 1 d . . .
H20A H 0.2348 0.3485 0.6485 0.069 Uiso 1 1 calc R . .
C21 C 0.3063(4) 0.2456(3) 0.7097(2) 0.0482(11) Uani 1 1 d . . .
H21A H 0.3234 0.2062 0.6712 0.058 Uiso 1 1 calc R . .
C22 C 0.3344(3) 0.2185(2) 0.78174(19) 0.0347(8) Uani 1 1 d . . .
C23 C 0.4058(4) -0.0671(2) 0.9195(2) 0.0388(8) Uani 1 1 d . . .
H23A H 0.4259 -0.0333 0.9641 0.047 Uiso 1 1 calc R . .
C24 C 0.4300(4) -0.1678(3) 0.9362(3) 0.0664(14) Uani 1 1 d . . .
H24A H 0.5178 -0.1766 0.9481 0.080 Uiso 1 1 calc R . .
H24B H 0.4108 -0.2046 0.8938 0.080 Uiso 1 1 calc R . .
C25 C 0.3484(5) -0.1980(4) 1.0000(3) 0.091(2) Uani 1 1 d . . .
H25A H 0.3701 -0.1621 1.0425 0.109 Uiso 1 1 calc R . .
H25B H 0.3656 -0.2618 1.0108 0.109 Uiso 1 1 calc R . .
C26 C 0.2080(5) -0.1865(3) 0.9840(3) 0.0634(13) Uani 1 1 d . . .
H26A H 0.1775 -0.2419 0.9607 0.076 Uiso 1 1 calc R . .
H26B H 0.1636 -0.1799 1.0297 0.076 Uiso 1 1 calc R . .
C27 C 0.1765(4) -0.1051(3) 0.9359(2) 0.0445(9) Uani 1 1 d . . .
C28 C 0.0500(4) -0.0841(3) 0.9212(2) 0.0536(11) Uani 1 1 d . . .
H28A H -0.0136 -0.1202 0.9407 0.064 Uiso 1 1 calc R . .
C29 C 0.0206(4) -0.0098(3) 0.8780(2) 0.0512(11) Uani 1 1 d . . .
H29A H -0.0629 0.0050 0.8693 0.061 Uiso 1 1 calc R . .
C30 C 0.1159(4) 0.0429(3) 0.8475(2) 0.0387(9) Uani 1 1 d . . .
C31 C 0.2679(3) -0.0488(2) 0.90404(18) 0.0334(7) Uani 1 1 d . . .
C32 C 0.0809(4) 0.1202(3) 0.7968(3) 0.0553(11) Uani 1 1 d . . .
H32A H 0.1557 0.1498 0.7797 0.083 Uiso 1 1 calc R . .
H32B H 0.0300 0.1639 0.8224 0.083 Uiso 1 1 calc R . .
H32C H 0.0348 0.0962 0.7563 0.083 Uiso 1 1 calc R . .


_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
Ir C11 2.021(4) . ?
Ir C22 2.031(4) . ?
Ir N1 2.057(3) . ?
Ir N2 2.071(3) . ?
Ir N3 2.189(3) . ?
Ir N4 2.252(3) . ?
N1 C1 1.362(5) . ?
N1 C5 1.377(5) . ?
N2 C12 1.354(4) . ?
N2 C16 1.381(4) . ?
N3 C23 1.482(5) . ?
N4 C30 1.364(5) . ?
N4 C31 1.375(4) . ?
Cl Cl 0.000(3) 1 ?
C1 C2 1.391(5) . ?
C2 C3 1.381(6) . ?
C3 C4 1.389(6) . ?
C4 C5 1.406(5) . ?
C5 C6 1.480(5) . ?
C6 C7 1.413(5) . ?
C6 C11 1.419(5) . ?
C7 C8 1.392(6) . ?
C8 C9 1.397(6) . ?
C9 C10 1.417(5) . ?
C10 C11 1.409(5) . ?
C12 C13 1.388(5) . ?
C13 C14 1.394(6) . ?
C14 C15 1.382(6) . ?
C15 C16 1.396(5) . ?
C16 C17 1.471(5) . ?
C17 C18 1.403(5) . ?
C17 C22 1.425(5) . ?
C18 C19 1.392(6) . ?
C19 C20 1.387(6) . ?
C20 C21 1.402(6) . ?
C21 C22 1.416(5) . ?
C23 C31 1.522(5) . ?
C23 C24 1.523(5) . ?
C24 C25 1.526(8) . ?
C25 C26 1.535(7) . ?
C26 C27 1.519(6) . ?
C27 C31 1.402(5) . ?
C27 C28 1.410(6) . ?
C28 C29 1.380(6) . ?
C29 C30 1.393(6) . ?
C30 C32 1.511(6) . ?

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
C11 Ir C22 85.98(14) . . ?
C11 Ir N1 80.52(13) . . ?
C22 Ir N1 95.45(13) . . ?
C11 Ir N2 95.74(13) . . ?
C22 Ir N2 80.00(13) . . ?
N1 Ir N2 174.35(10) . . ?
C11 Ir N3 95.60(12) . . ?
C22 Ir N3 176.29(13) . . ?
N1 Ir N3 88.12(11) . . ?
N2 Ir N3 96.49(11) . . ?
C11 Ir N4 170.93(12) . . ?
C22 Ir N4 102.06(13) . . ?
N1 Ir N4 94.39(11) . . ?
N2 Ir N4 89.86(11) . . ?
N3 Ir N4 76.63(11) . . ?
C1 N1 C5 118.4(3) . . ?
C1 N1 Ir 125.8(3) . . ?
C5 N1 Ir 115.7(2) . . ?
C12 N2 C16 118.7(3) . . ?
C12 N2 Ir 126.0(2) . . ?
C16 N2 Ir 115.3(2) . . ?
C23 N3 Ir 111.8(2) . . ?
C30 N4 C31 117.9(3) . . ?
C30 N4 Ir 128.3(2) . . ?
C31 N4 Ir 113.7(2) . . ?
N1 C1 C2 123.0(4) . . ?
C3 C2 C1 118.9(4) . . ?
C2 C3 C4 119.1(4) . . ?
C3 C4 C5 120.6(4) . . ?
N1 C5 C4 120.0(3) . . ?
N1 C5 C6 114.1(3) . . ?
C4 C5 C6 125.9(3) . . ?
C7 C6 C11 122.4(3) . . ?
C7 C6 C5 123.0(3) . . ?
C11 C6 C5 114.6(3) . . ?
C8 C7 C6 118.9(4) . . ?
C7 C8 C9 120.4(4) . . ?
C8 C9 C10 120.3(4) . . ?
C11 C10 C9 120.9(4) . . ?
C10 C11 C6 117.0(3) . . ?
C10 C11 Ir 128.0(3) . . ?
C6 C11 Ir 114.9(3) . . ?
N2 C12 C13 122.4(4) . . ?
C12 C13 C14 119.0(4) . . ?
C15 C14 C13 119.1(4) . . ?
C14 C15 C16 120.2(4) . . ?
N2 C16 C15 120.4(3) . . ?
N2 C16 C17 113.7(3) . . ?
C15 C16 C17 125.8(3) . . ?
C18 C17 C22 121.5(4) . . ?
C18 C17 C16 123.0(3) . . ?
C22 C17 C16 115.3(3) . . ?
C19 C18 C17 119.7(4) . . ?
C20 C19 C18 119.7(4) . . ?
C19 C20 C21 121.5(4) . . ?
C20 C21 C22 120.2(4) . . ?
C21 C22 C17 117.3(3) . . ?
C21 C22 Ir 128.4(3) . . ?
C17 C22 Ir 114.3(2) . . ?
N3 C23 C31 111.3(3) . . ?
N3 C23 C24 114.4(4) . . ?
C31 C23 C24 111.7(3) . . ?
C23 C24 C25 109.7(4) . . ?
C24 C25 C26 112.1(4) . . ?
C27 C26 C25 114.4(4) . . ?
C31 C27 C28 117.2(4) . . ?
C31 C27 C26 123.3(4) . . ?
C28 C27 C26 119.5(4) . . ?
C29 C28 C27 119.9(4) . . ?
C28 C29 C30 120.0(4) . . ?
N4 C30 C29 121.7(4) . . ?
N4 C30 C32 119.5(4) . . ?
C29 C30 C32 118.8(4) . . ?
N4 C31 C27 123.2(3) . . ?
N4 C31 C23 117.4(3) . . ?
C27 C31 C23 119.4(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 Ir N1 C1 -178.3(3) . . . . ?
C22 Ir N1 C1 -93.4(3) . . . . ?
N2 Ir N1 C1 -129.5(13) . . . . ?
N3 Ir N1 C1 85.7(3) . . . . ?
N4 Ir N1 C1 9.2(3) . . . . ?
C11 Ir N1 C5 0.0(2) . . . . ?
C22 Ir N1 C5 85.0(2) . . . . ?
N2 Ir N1 C5 48.8(15) . . . . ?
N3 Ir N1 C5 -96.0(2) . . . . ?
N4 Ir N1 C5 -172.5(2) . . . . ?
C11 Ir N2 C12 -85.9(3) . . . . ?
C22 Ir N2 C12 -170.8(3) . . . . ?
N1 Ir N2 C12 -134.2(13) . . . . ?
N3 Ir N2 C12 10.4(3) . . . . ?
N4 Ir N2 C12 86.9(3) . . . . ?
C11 Ir N2 C16 96.0(3) . . . . ?
C22 Ir N2 C16 11.2(2) . . . . ?
N1 Ir N2 C16 47.8(15) . . . . ?
N3 Ir N2 C16 -167.6(2) . . . . ?
N4 Ir N2 C16 -91.1(2) . . . . ?
C11 Ir N3 C23 160.3(2) . . . . ?
C22 Ir N3 C23 45(2) . . . . ?
N1 Ir N3 C23 -119.4(2) . . . . ?
N2 Ir N3 C23 63.9(2) . . . . ?
N4 Ir N3 C23 -24.4(2) . . . . ?
C11 Ir N4 C30 -133.9(7) . . . . ?
C22 Ir N4 C30 18.1(3) . . . . ?
N1 Ir N4 C30 -78.4(3) . . . . ?
N2 Ir N4 C30 97.9(3) . . . . ?
N3 Ir N4 C30 -165.4(3) . . . . ?
C11 Ir N4 C31 43.0(8) . . . . ?
C22 Ir N4 C31 -165.0(2) . . . . ?
N1 Ir N4 C31 98.5(2) . . . . ?
N2 Ir N4 C31 -85.2(2) . . . . ?
N3 Ir N4 C31 11.5(2) . . . . ?
C5 N1 C1 C2 -0.6(5) . . . . ?
Ir N1 C1 C2 177.7(3) . . . . ?
N1 C1 C2 C3 1.3(6) . . . . ?
C1 C2 C3 C4 -0.4(6) . . . . ?
C2 C3 C4 C5 -1.0(6) . . . . ?
C1 N1 C5 C4 -0.9(5) . . . . ?
Ir N1 C5 C4 -179.3(3) . . . . ?
C1 N1 C5 C6 179.8(3) . . . . ?
Ir N1 C5 C6 1.3(4) . . . . ?
C3 C4 C5 N1 1.7(6) . . . . ?
C3 C4 C5 C6 -179.1(4) . . . . ?
N1 C5 C6 C7 178.9(3) . . . . ?
C4 C5 C6 C7 -0.4(6) . . . . ?
N1 C5 C6 C11 -2.4(4) . . . . ?
C4 C5 C6 C11 178.3(3) . . . . ?
C11 C6 C7 C8 -1.6(5) . . . . ?
C5 C6 C7 C8 177.0(3) . . . . ?
C6 C7 C8 C9 0.7(6) . . . . ?
C7 C8 C9 C10 0.3(6) . . . . ?
C8 C9 C10 C11 -0.4(6) . . . . ?
C9 C10 C11 C6 -0.4(5) . . . . ?
C9 C10 C11 Ir 179.9(3) . . . . ?
C7 C6 C11 C10 1.4(5) . . . . ?
C5 C6 C11 C10 -177.3(3) . . . . ?
C7 C6 C11 Ir -178.9(3) . . . . ?
C5 C6 C11 Ir 2.4(4) . . . . ?
C22 Ir C11 C10 82.1(3) . . . . ?
N1 Ir C11 C10 178.3(3) . . . . ?
N2 Ir C11 C10 2.6(3) . . . . ?
N3 Ir C11 C10 -94.5(3) . . . . ?
N4 Ir C11 C10 -125.3(7) . . . . ?
C22 Ir C11 C6 -97.6(3) . . . . ?
N1 Ir C11 C6 -1.3(2) . . . . ?
N2 Ir C11 C6 -177.1(2) . . . . ?
N3 Ir C11 C6 85.8(2) . . . . ?
N4 Ir C11 C6 55.1(9) . . . . ?
C16 N2 C12 C13 4.0(5) . . . . ?
Ir N2 C12 C13 -174.0(3) . . . . ?
N2 C12 C13 C14 0.7(6) . . . . ?
C12 C13 C14 C15 -3.6(6) . . . . ?
C13 C14 C15 C16 1.9(6) . . . . ?
C12 N2 C16 C15 -5.7(5) . . . . ?
Ir N2 C16 C15 172.5(3) . . . . ?
C12 N2 C16 C17 170.7(3) . . . . ?
Ir N2 C16 C17 -11.2(4) . . . . ?
C14 C15 C16 N2 2.7(6) . . . . ?
C14 C15 C16 C17 -173.1(4) . . . . ?
N2 C16 C17 C18 -172.2(4) . . . . ?
C15 C16 C17 C18 3.8(6) . . . . ?
N2 C16 C17 C22 3.7(5) . . . . ?
C15 C16 C17 C22 179.8(4) . . . . ?
C22 C17 C18 C19 -0.5(6) . . . . ?
C16 C17 C18 C19 175.2(4) . . . . ?
C17 C18 C19 C20 -2.5(7) . . . . ?
C18 C19 C20 C21 2.8(7) . . . . ?
C19 C20 C21 C22 -0.1(7) . . . . ?
C20 C21 C22 C17 -2.8(6) . . . . ?
C20 C21 C22 Ir 179.0(3) . . . . ?
C18 C17 C22 C21 3.1(6) . . . . ?
C16 C17 C22 C21 -172.9(4) . . . . ?
C18 C17 C22 Ir -178.4(3) . . . . ?
C16 C17 C22 Ir 5.6(4) . . . . ?
C11 Ir C22 C21 72.9(4) . . . . ?
N1 Ir C22 C21 -7.1(4) . . . . ?
N2 Ir C22 C21 169.5(4) . . . . ?
N3 Ir C22 C21 -171.7(19) . . . . ?
N4 Ir C22 C21 -102.8(4) . . . . ?
C11 Ir C22 C17 -105.3(3) . . . . ?
N1 Ir C22 C17 174.6(3) . . . . ?
N2 Ir C22 C17 -8.8(3) . . . . ?
N3 Ir C22 C17 10(2) . . . . ?
N4 Ir C22 C17 78.9(3) . . . . ?
Ir N3 C23 C31 33.5(3) . . . . ?
Ir N3 C23 C24 161.4(3) . . . . ?
N3 C23 C24 C25 175.7(4) . . . . ?
C31 C23 C24 C25 -56.6(5) . . . . ?
C23 C24 C25 C26 60.0(6) . . . . ?
C24 C25 C26 C27 -33.5(7) . . . . ?
C25 C26 C27 C31 4.6(7) . . . . ?
C25 C26 C27 C28 -175.9(5) . . . . ?
C31 C27 C28 C29 -1.0(6) . . . . ?
C26 C27 C28 C29 179.5(4) . . . . ?
C27 C28 C29 C30 1.6(7) . . . . ?
C31 N4 C30 C29 2.1(5) . . . . ?
Ir N4 C30 C29 178.9(3) . . . . ?
C31 N4 C30 C32 -176.5(3) . . . . ?
Ir N4 C30 C32 0.3(5) . . . . ?
C28 C29 C30 N4 -2.2(6) . . . . ?
C28 C29 C30 C32 176.4(4) . . . . ?
C30 N4 C31 C27 -1.5(5) . . . . ?
Ir N4 C31 C27 -178.7(3) . . . . ?
C30 N4 C31 C23 -179.1(3) . . . . ?
Ir N4 C31 C23 3.6(4) . . . . ?
C28 C27 C31 N4 0.9(6) . . . . ?
C26 C27 C31 N4 -179.6(3) . . . . ?
C28 C27 C31 C23 178.5(4) . . . . ?
C26 C27 C31 C23 -2.0(6) . . . . ?
N3 C23 C31 N4 -24.7(4) . . . . ?
C24 C23 C31 N4 -154.0(4) . . . . ?
N3 C23 C31 C27 157.6(3) . . . . ?
C24 C23 C31 C27 28.2(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3B Cl 0.90 2.47 3.284(3) 150.0 1

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.18
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.082


#===END



