# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_1157yng
_database_code_depnum_ccdc_archive 'CCDC 962389'
_audit_update_record             
;
2013-09-20 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H49 Ir Lu N Si'
_chemical_formula_weight         794.94

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 '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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_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                   9.3823(11)
_cell_length_b                   20.167(2)
_cell_length_c                   16.4339(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.864(2)
_cell_angle_gamma                90.00
_cell_volume                     3063.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    163(2)
_cell_measurement_reflns_used    16244
_cell_measurement_theta_min      1.61
_cell_measurement_theta_max      25.08

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1544
_exptl_absorpt_coefficient_mu    7.597
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5171
_exptl_absorpt_correction_T_max  0.9279
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      163(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16244
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_sigmaI/netI    0.1403
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         25.08
_reflns_number_total             5395
_reflns_number_gt                2943
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0576P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5395
_refine_ls_number_parameters     162
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1231
_refine_ls_R_factor_gt           0.0631
_refine_ls_wR_factor_ref         0.1379
_refine_ls_wR_factor_gt          0.1233
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_restrained_S_all      0.913
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.25103(7) 0.13938(3) 0.84209(4) 0.03588(19) Uani 1 1 d . . .
Lu1 Lu 0.25641(9) 0.27727(3) 0.91356(5) 0.0534(3) Uani 1 1 d . . .
N1 N 0.4014(14) 0.2029(6) 0.8836(8) 0.049(4) Uani 1 1 d . . .
Si1 Si 0.1632(6) 0.1864(3) 1.0356(3) 0.0591(14) Uani 1 1 d . . .
C1 C 0.2343(8) 0.4088(3) 0.9109(5) 0.061(2) Uani 1 1 d G . .
C2 C 0.0895(8) 0.3864(4) 0.9031(5) 0.061(2) Uani 1 1 d G . .
C3 C 0.0540(9) 0.3529(4) 0.8265(5) 0.061(2) Uani 1 1 d G . .
C4 C 0.1769(8) 0.3546(4) 0.7870(5) 0.061(2) Uani 1 1 d G . .
C5 C 0.2884(8) 0.3892(3) 0.8392(5) 0.061(2) Uani 1 1 d G . .
C6 C 0.3165(12) 0.4469(6) 0.9829(7) 0.109(4) Uani 1 1 d G . .
H6A H 0.2485 0.4645 1.0166 0.163 Uiso 1 1 calc R . .
H6B H 0.3689 0.4836 0.9624 0.163 Uiso 1 1 calc R . .
H6C H 0.3855 0.4173 1.0166 0.163 Uiso 1 1 calc R . .
C7 C -0.0094(13) 0.3964(6) 0.9652(7) 0.109(4) Uani 1 1 d G . .
H7A H 0.0486 0.4046 1.0198 0.163 Uiso 1 1 calc R . .
H7B H -0.0685 0.3565 0.9674 0.163 Uiso 1 1 calc R . .
H7C H -0.0726 0.4345 0.9489 0.163 Uiso 1 1 calc R . .
C8 C -0.0893(13) 0.3210(6) 0.7929(7) 0.109(4) Uani 1 1 d G . .
H8A H -0.0741 0.2841 0.7565 0.163 Uiso 1 1 calc R . .
H8B H -0.1535 0.3539 0.7616 0.163 Uiso 1 1 calc R . .
H8C H -0.1334 0.3043 0.8388 0.163 Uiso 1 1 calc R . .
C9 C 0.1873(13) 0.3249(6) 0.7041(7) 0.109(4) Uani 1 1 d G . .
H9A H 0.0941 0.3297 0.6671 0.163 Uiso 1 1 calc R . .
H9B H 0.2119 0.2778 0.7108 0.163 Uiso 1 1 calc R . .
H9C H 0.2625 0.3480 0.6803 0.163 Uiso 1 1 calc R . .
C10 C 0.4380(12) 0.4027(6) 0.8215(7) 0.109(4) Uani 1 1 d G . .
H10A H 0.4793 0.3616 0.8038 0.163 Uiso 1 1 calc R . .
H10B H 0.4995 0.4194 0.8716 0.163 Uiso 1 1 calc R . .
H10C H 0.4326 0.4360 0.7776 0.163 Uiso 1 1 calc R . .
C11 C 0.274(2) 0.2602(9) 1.0591(11) 0.075(6) Uani 1 1 d . . .
H11A H 0.3733 0.2511 1.0882 0.090 Uiso 1 1 calc R . .
H11B H 0.2274 0.2955 1.0874 0.090 Uiso 1 1 calc R . .
C12 C -0.008(2) 0.1926(12) 1.0787(12) 0.100(8) Uani 1 1 d . . .
H12A H 0.0112 0.1807 1.1375 0.150 Uiso 1 1 calc R . .
H12B H -0.0800 0.1621 1.0490 0.150 Uiso 1 1 calc R . .
H12C H -0.0448 0.2381 1.0725 0.150 Uiso 1 1 calc R . .
C13 C 0.258(2) 0.1073(8) 1.0673(10) 0.074(6) Uani 1 1 d . . .
H13A H 0.3604 0.1116 1.0638 0.111 Uiso 1 1 calc R . .
H13B H 0.2147 0.0716 1.0307 0.111 Uiso 1 1 calc R . .
H13C H 0.2475 0.0969 1.1243 0.111 Uiso 1 1 calc R . .
C14 C 0.1009(19) 0.1847(8) 0.9151(10) 0.055(5) Uani 1 1 d . . .
C15 C 0.1980(8) 0.0955(3) 0.7155(5) 0.057(2) Uani 1 1 d G . .
C16 C 0.0794(8) 0.0863(3) 0.7568(5) 0.057(2) Uani 1 1 d G . .
C17 C 0.1245(8) 0.0445(3) 0.8253(5) 0.057(2) Uani 1 1 d G . .
C18 C 0.2710(8) 0.0279(3) 0.8263(5) 0.057(2) Uani 1 1 d G . .
C19 C 0.3164(8) 0.0594(4) 0.7584(5) 0.057(2) Uani 1 1 d G . .
C20 C 0.1982(11) 0.1365(5) 0.6392(7) 0.092(3) Uani 1 1 d G . .
H20A H 0.1984 0.1071 0.5917 0.137 Uiso 1 1 calc R . .
H20B H 0.2847 0.1646 0.6467 0.137 Uiso 1 1 calc R . .
H20C H 0.1115 0.1645 0.6295 0.137 Uiso 1 1 calc R . .
C21 C -0.0687(11) 0.1157(5) 0.7322(7) 0.092(3) Uani 1 1 d G . .
H21A H -0.0612 0.1579 0.7037 0.137 Uiso 1 1 calc R . .
H21B H -0.1117 0.1234 0.7817 0.137 Uiso 1 1 calc R . .
H21C H -0.1298 0.0851 0.6953 0.137 Uiso 1 1 calc R . .
C22 C 0.0328(11) 0.0217(5) 0.8864(7) 0.092(3) Uani 1 1 d G . .
H22A H -0.0319 0.0577 0.8968 0.137 Uiso 1 1 calc R . .
H22B H 0.0952 0.0092 0.9382 0.137 Uiso 1 1 calc R . .
H22C H -0.0249 -0.0167 0.8640 0.137 Uiso 1 1 calc R . .
C23 C 0.3624(11) -0.0157(5) 0.8886(7) 0.092(3) Uani 1 1 d G . .
H23A H 0.3427 -0.0055 0.9439 0.137 Uiso 1 1 calc R . .
H23B H 0.4649 -0.0077 0.8869 0.137 Uiso 1 1 calc R . .
H23C H 0.3392 -0.0623 0.8756 0.137 Uiso 1 1 calc R . .
C24 C 0.4646(11) 0.0553(6) 0.7359(7) 0.092(3) Uani 1 1 d G . .
H24A H 0.5290 0.0869 0.7693 0.137 Uiso 1 1 calc R . .
H24B H 0.4588 0.0659 0.6772 0.137 Uiso 1 1 calc R . .
H24C H 0.5027 0.0103 0.7464 0.137 Uiso 1 1 calc R . .
C25 C 0.5616(15) 0.2040(7) 0.8826(9) 0.036(4) Uani 1 1 d . . .
C26 C 0.625(2) 0.2552(9) 0.9396(13) 0.081(7) Uani 1 1 d . . .
H26A H 0.5945 0.2988 0.9170 0.121 Uiso 1 1 calc R . .
H26B H 0.7308 0.2520 0.9476 0.121 Uiso 1 1 calc R . .
H26C H 0.5928 0.2492 0.9928 0.121 Uiso 1 1 calc R . .
C27 C 0.6241(16) 0.1341(8) 0.9206(12) 0.068(6) Uani 1 1 d . . .
H27A H 0.7199 0.1264 0.9063 0.102 Uiso 1 1 calc R . .
H27B H 0.5585 0.0983 0.8978 0.102 Uiso 1 1 calc R . .
H27C H 0.6317 0.1350 0.9808 0.102 Uiso 1 1 calc R . .
C28 C 0.579(2) 0.2128(10) 0.7931(13) 0.089(7) Uani 1 1 d . . .
H28A H 0.5328 0.2542 0.7716 0.134 Uiso 1 1 calc R . .
H28B H 0.5341 0.1754 0.7603 0.134 Uiso 1 1 calc R . .
H28C H 0.6825 0.2144 0.7896 0.134 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
Ir1 N1 1.940(13) . ?
Ir1 C14 2.200(16) . ?
Ir1 C16 2.221(7) . ?
Ir1 C15 2.237(7) . ?
Ir1 C17 2.244(7) . ?
Ir1 C19 2.271(7) . ?
Ir1 C18 2.275(7) . ?
Ir1 Lu1 3.0158(9) . ?
Lu1 N1 2.138(13) . ?
Lu1 C14 2.373(17) . ?
Lu1 C11 2.395(18) . ?
Lu1 C4 2.605(7) . ?
Lu1 C5 2.609(7) . ?
Lu1 C3 2.655(7) . ?
Lu1 C1 2.661(7) . ?
Lu1 C2 2.689(7) . ?
Lu1 Si1 2.956(5) . ?
N1 C25 1.507(18) . ?
Si1 C11 1.818(18) . ?
Si1 C13 1.856(17) . ?
Si1 C12 1.867(18) . ?
Si1 C14 1.966(17) . ?
C1 C2 1.417(5) . ?
C1 C5 1.417(5) . ?
C1 C6 1.507(5) . ?
C2 C3 1.417(5) . ?
C2 C7 1.507(5) . ?
C3 C4 1.417(5) . ?
C3 C8 1.507(5) . ?
C4 C5 1.417(5) . ?
C4 C9 1.507(5) . ?
C5 C10 1.507(5) . ?
C15 C16 1.412(4) . ?
C15 C19 1.412(4) . ?
C15 C20 1.501(5) . ?
C16 C17 1.412(4) . ?
C16 C21 1.501(5) . ?
C17 C18 1.412(4) . ?
C17 C22 1.501(5) . ?
C18 C19 1.412(4) . ?
C18 C23 1.501(5) . ?
C19 C24 1.501(5) . ?
C25 C26 1.45(2) . ?
C25 C28 1.52(2) . ?
C25 C27 1.61(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ir1 C14 91.7(6) . . ?
N1 Ir1 C16 160.9(4) . . ?
C14 Ir1 C16 94.7(5) . . ?
N1 Ir1 C15 128.3(4) . . ?
C14 Ir1 C15 127.6(5) . . ?
C16 Ir1 C15 36.93(13) . . ?
N1 Ir1 C17 160.7(4) . . ?
C14 Ir1 C17 92.6(5) . . ?
C16 Ir1 C17 36.87(13) . . ?
C15 Ir1 C17 61.3(2) . . ?
N1 Ir1 C19 115.2(4) . . ?
C14 Ir1 C19 152.9(5) . . ?
C16 Ir1 C19 61.1(2) . . ?
C15 Ir1 C19 36.50(13) . . ?
C17 Ir1 C19 60.8(2) . . ?
N1 Ir1 C18 128.6(4) . . ?
C14 Ir1 C18 123.0(5) . . ?
C16 Ir1 C18 61.1(2) . . ?
C15 Ir1 C18 60.8(2) . . ?
C17 Ir1 C18 36.40(13) . . ?
C19 Ir1 C18 36.19(13) . . ?
N1 Ir1 Lu1 44.9(4) . . ?
C14 Ir1 Lu1 51.3(4) . . ?
C16 Ir1 Lu1 130.72(19) . . ?
C15 Ir1 Lu1 135.49(19) . . ?
C17 Ir1 Lu1 143.84(19) . . ?
C19 Ir1 Lu1 154.49(19) . . ?
C18 Ir1 Lu1 163.66(19) . . ?
N1 Lu1 C14 82.4(5) . . ?
N1 Lu1 C11 101.1(6) . . ?
C14 Lu1 C11 79.2(6) . . ?
N1 Lu1 C4 110.0(4) . . ?
C14 Lu1 C4 112.8(5) . . ?
C11 Lu1 C4 147.7(5) . . ?
N1 Lu1 C5 111.7(4) . . ?
C14 Lu1 C5 143.7(5) . . ?
C11 Lu1 C5 126.8(5) . . ?
C4 Lu1 C5 31.54(12) . . ?
N1 Lu1 C3 134.7(4) . . ?
C14 Lu1 C3 94.2(5) . . ?
C11 Lu1 C3 122.8(5) . . ?
C4 Lu1 C3 31.24(11) . . ?
C5 Lu1 C3 51.64(18) . . ?
N1 Lu1 C1 138.3(4) . . ?
C14 Lu1 C1 137.6(4) . . ?
C11 Lu1 C1 98.7(5) . . ?
C4 Lu1 C1 51.62(18) . . ?
C5 Lu1 C1 31.18(12) . . ?
C3 Lu1 C1 51.11(18) . . ?
N1 Lu1 C2 161.0(4) . . ?
C14 Lu1 C2 107.0(4) . . ?
C11 Lu1 C2 96.9(5) . . ?
C4 Lu1 C2 51.31(18) . . ?
C5 Lu1 C2 51.27(18) . . ?
C3 Lu1 C2 30.75(11) . . ?
C1 Lu1 C2 30.72(11) . . ?
N1 Lu1 Si1 89.7(3) . . ?
C14 Lu1 Si1 41.5(4) . . ?
C11 Lu1 Si1 37.9(4) . . ?
C4 Lu1 Si1 146.6(2) . . ?
C5 Lu1 Si1 157.7(2) . . ?
C3 Lu1 Si1 117.0(2) . . ?
C1 Lu1 Si1 126.7(2) . . ?
C2 Lu1 Si1 108.3(2) . . ?
N1 Lu1 Ir1 39.8(3) . . ?
C14 Lu1 Ir1 46.3(4) . . ?
C11 Lu1 Ir1 104.5(4) . . ?
C4 Lu1 Ir1 104.94(18) . . ?
C5 Lu1 Ir1 127.66(19) . . ?
C3 Lu1 Ir1 110.91(18) . . ?
C1 Lu1 Ir1 156.49(18) . . ?
C2 Lu1 Ir1 139.36(17) . . ?
Si1 Lu1 Ir1 72.88(11) . . ?
C25 N1 Ir1 132.2(10) . . ?
C25 N1 Lu1 131.9(9) . . ?
Ir1 N1 Lu1 95.2(5) . . ?
C11 Si1 C13 114.6(9) . . ?
C11 Si1 C12 111.2(10) . . ?
C13 Si1 C12 110.5(10) . . ?
C11 Si1 C14 106.9(8) . . ?
C13 Si1 C14 108.2(7) . . ?
C12 Si1 C14 104.9(8) . . ?
C11 Si1 Lu1 54.0(6) . . ?
C13 Si1 Lu1 122.8(6) . . ?
C12 Si1 Lu1 126.2(8) . . ?
C14 Si1 Lu1 53.1(5) . . ?
C2 C1 C5 108.0 . . ?
C2 C1 C6 126.0 . . ?
C5 C1 C6 126.0 . . ?
C2 C1 Lu1 75.7(2) . . ?
C5 C1 Lu1 72.4(3) . . ?
C6 C1 Lu1 117.8(2) . . ?
C1 C2 C3 108.0 . . ?
C1 C2 C7 126.0 . . ?
C3 C2 C7 126.0 . . ?
C1 C2 Lu1 73.5(2) . . ?
C3 C2 Lu1 73.3(2) . . ?
C7 C2 Lu1 119.0(2) . . ?
C2 C3 C4 108.0 . . ?
C2 C3 C8 126.0 . . ?
C4 C3 C8 126.0 . . ?
C2 C3 Lu1 76.0(3) . . ?
C4 C3 Lu1 72.4(3) . . ?
C8 C3 Lu1 117.6(2) . . ?
C5 C4 C3 108.0 . . ?
C5 C4 C9 126.0 . . ?
C3 C4 C9 126.0 . . ?
C5 C4 Lu1 74.4(2) . . ?
C3 C4 Lu1 76.3(3) . . ?
C9 C4 Lu1 115.5(3) . . ?
C4 C5 C1 108.0 . . ?
C4 C5 C10 126.0 . . ?
C1 C5 C10 126.0 . . ?
C4 C5 Lu1 74.1(2) . . ?
C1 C5 Lu1 76.4(3) . . ?
C10 C5 Lu1 115.6(2) . . ?
Si1 C11 Lu1 88.0(7) . . ?
Si1 C14 Ir1 116.7(8) . . ?
Si1 C14 Lu1 85.4(6) . . ?
Ir1 C14 Lu1 82.4(6) . . ?
C16 C15 C19 108.0 . . ?
C16 C15 C20 126.0 . . ?
C19 C15 C20 126.0 . . ?
C16 C15 Ir1 70.9(2) . . ?
C19 C15 Ir1 73.0(2) . . ?
C20 C15 Ir1 121.8(2) . . ?
C17 C16 C15 108.0 . . ?
C17 C16 C21 126.0 . . ?
C15 C16 C21 126.0 . . ?
C17 C16 Ir1 72.5(2) . . ?
C15 C16 Ir1 72.2(2) . . ?
C21 C16 Ir1 121.1(2) . . ?
C16 C17 C18 108.0 . . ?
C16 C17 C22 126.0 . . ?
C18 C17 C22 126.0 . . ?
C16 C17 Ir1 70.7(2) . . ?
C18 C17 Ir1 73.0(2) . . ?
C22 C17 Ir1 122.0(2) . . ?
C17 C18 C19 108.0 . . ?
C17 C18 C23 126.0 . . ?
C19 C18 C23 126.0 . . ?
C17 C18 Ir1 70.6(2) . . ?
C19 C18 Ir1 71.7(2) . . ?
C23 C18 Ir1 123.3(2) . . ?
C15 C19 C18 108.0 . . ?
C15 C19 C24 126.0 . . ?
C18 C19 C24 126.0 . . ?
C15 C19 Ir1 70.5(2) . . ?
C18 C19 Ir1 72.1(2) . . ?
C24 C19 Ir1 123.1(2) . . ?
C26 C25 N1 107.6(13) . . ?
C26 C25 C28 116.2(15) . . ?
N1 C25 C28 106.7(13) . . ?
C26 C25 C27 106.9(13) . . ?
N1 C25 C27 106.3(12) . . ?
C28 C25 C27 112.6(14) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.08
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         3.258
_refine_diff_density_min         -2.680
_refine_diff_density_rms         0.201
####################################################################### 
# 
# 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_15166ts
_database_code_depnum_ccdc_archive 'CCDC 962390'
_audit_update_record             
;
2013-09-20 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H60 Ir N2 Sc Si2'
_chemical_formula_weight         802.19

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sc Sc 0.2519 0.3716 '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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.6879(10)
_cell_length_b                   10.9527(11)
_cell_length_c                   18.836(2)
_cell_angle_alpha                73.1590(10)
_cell_angle_beta                 85.811(2)
_cell_angle_gamma                78.9610(10)
_cell_volume                     1877.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    11447
_cell_measurement_theta_min      1.97
_cell_measurement_theta_max      27.00

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             820
_exptl_absorpt_coefficient_mu    3.810
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.3110
_exptl_absorpt_correction_T_max  0.3110
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11447
_diffrn_reflns_av_R_equivalents  0.0858
_diffrn_reflns_av_sigmaI/netI    0.0706
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         27.00
_reflns_number_total             7820
_reflns_number_gt                7043
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1490P)²+4.8271P] 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_number_reflns         7820
_refine_ls_number_parameters     391
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0733
_refine_ls_wR_factor_ref         0.2178
_refine_ls_wR_factor_gt          0.2075
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_restrained_S_all      1.142
_refine_ls_shift/su_max          0.003
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.70982(3) 0.69421(3) 0.660861(16) 0.02640(16) Uani 1 1 d . . .
Sc1 Sc 0.84319(16) 0.46341(15) 0.77439(8) 0.0229(3) Uani 1 1 d . . .
N1 N 0.7458(8) 0.5080(7) 0.6752(4) 0.0287(15) Uani 1 1 d . . .
N2 N 0.6719(7) 0.3460(7) 0.8376(4) 0.0279(15) Uani 1 1 d . . .
Si1 Si 0.6354(3) 0.6847(3) 0.85160(14) 0.0320(5) Uani 1 1 d . . .
Si2 Si 1.0870(3) 0.1045(3) 0.81560(18) 0.0407(6) Uani 1 1 d . . .
C1 C 0.7581(10) 0.6573(9) 0.7770(6) 0.0332(19) Uani 1 1 d . . .
C2 C 0.6533(14) 0.8316(13) 0.8833(6) 0.051(3) Uani 1 1 d . . .
H2A H 0.7505 0.8233 0.8978 0.076 Uiso 1 1 calc R . .
H2B H 0.5898 0.8359 0.9259 0.076 Uiso 1 1 calc R . .
H2C H 0.6287 0.9108 0.8426 0.076 Uiso 1 1 calc R . .
C3 C 0.4445(11) 0.6973(11) 0.8340(7) 0.045(2) Uani 1 1 d . . .
H3A H 0.4245 0.7451 0.7820 0.067 Uiso 1 1 calc R . .
H3B H 0.3869 0.7433 0.8665 0.067 Uiso 1 1 calc R . .
H3C H 0.4223 0.6102 0.8442 0.067 Uiso 1 1 calc R . .
C4 C 0.6698(13) 0.5520(12) 0.9415(6) 0.047(3) Uani 1 1 d . . .
H4A H 0.6231 0.4803 0.9411 0.070 Uiso 1 1 calc R . .
H4B H 0.6329 0.5861 0.9831 0.070 Uiso 1 1 calc R . .
H4C H 0.7713 0.5206 0.9469 0.070 Uiso 1 1 calc R . .
C5 C 0.7137(9) 0.4402(8) 0.6214(4) 0.0261(16) Uani 1 1 d . . .
C6 C 0.5554(12) 0.4703(11) 0.6066(6) 0.045(3) Uani 1 1 d . . .
H6A H 0.5042 0.4361 0.6527 0.068 Uiso 1 1 calc R . .
H6B H 0.5365 0.4298 0.5692 0.068 Uiso 1 1 calc R . .
H6C H 0.5245 0.5644 0.5886 0.068 Uiso 1 1 calc R . .
C7 C 0.7977(14) 0.4764(12) 0.5508(6) 0.049(3) Uani 1 1 d . . .
H7A H 0.7773 0.5706 0.5290 0.073 Uiso 1 1 calc R . .
H7B H 0.7725 0.4335 0.5158 0.073 Uiso 1 1 calc R . .
H7C H 0.8982 0.4487 0.5614 0.073 Uiso 1 1 calc R . .
C8 C 0.7553(14) 0.2923(10) 0.6578(6) 0.046(3) Uani 1 1 d . . .
H8A H 0.8554 0.2710 0.6696 0.070 Uiso 1 1 calc R . .
H8B H 0.7371 0.2453 0.6234 0.070 Uiso 1 1 calc R . .
H8C H 0.6995 0.2671 0.7035 0.070 Uiso 1 1 calc R . .
C9 C 0.6873(10) 0.2493(11) 0.9017(6) 0.041(2) Uani 1 1 d . . .
H9 H 0.7785 0.2191 0.9222 0.049 Uiso 1 1 calc R . .
C10 C 0.5799(14) 0.1933(13) 0.9383(6) 0.053(3) Uani 1 1 d . . .
H10 H 0.5959 0.1272 0.9839 0.063 Uiso 1 1 calc R . .
C11 C 0.4455(12) 0.2331(13) 0.9085(6) 0.046(3) Uani 1 1 d . . .
H11 H 0.3690 0.1928 0.9318 0.055 Uiso 1 1 calc R . .
C12 C 0.4285(11) 0.3333(12) 0.8438(6) 0.045(2) Uani 1 1 d . . .
H12 H 0.3383 0.3659 0.8225 0.054 Uiso 1 1 calc R . .
C13 C 0.5431(10) 0.3858(10) 0.8104(5) 0.0332(19) Uani 1 1 d . . .
H13 H 0.5295 0.4540 0.7655 0.040 Uiso 1 1 calc R . .
C14 C 1.0633(9) 0.2833(9) 0.8047(5) 0.0302(18) Uani 1 1 d . . .
C15 C 1.0453(8) 0.3422(9) 0.8656(5) 0.0295(18) Uani 1 1 d . . .
C16 C 1.0651(9) 0.4686(9) 0.8401(5) 0.0301(18) Uani 1 1 d . . .
C17 C 1.0965(9) 0.4945(10) 0.7628(5) 0.0323(19) Uani 1 1 d . . .
C18 C 1.0968(9) 0.3824(10) 0.7413(5) 0.0297(18) Uani 1 1 d . . .
C19 C 1.0253(11) 0.2709(12) 0.9467(5) 0.041(2) Uani 1 1 d . . .
H19A H 1.1063 0.2716 0.9748 0.062 Uiso 1 1 calc R . .
H19B H 1.0173 0.1811 0.9512 0.062 Uiso 1 1 calc R . .
H19C H 0.9394 0.3139 0.9665 0.062 Uiso 1 1 calc R . .
C20 C 1.0697(11) 0.5603(12) 0.8863(6) 0.044(2) Uani 1 1 d . . .
H20A H 1.0276 0.5271 0.9354 0.065 Uiso 1 1 calc R . .
H20B H 1.0169 0.6462 0.8616 0.065 Uiso 1 1 calc R . .
H20C H 1.1677 0.5668 0.8918 0.065 Uiso 1 1 calc R . .
C21 C 1.1382(12) 0.6191(12) 0.7134(7) 0.047(3) Uani 1 1 d . . .
H21A H 1.2410 0.6089 0.7099 0.071 Uiso 1 1 calc R . .
H21B H 1.1003 0.6907 0.7347 0.071 Uiso 1 1 calc R . .
H21C H 1.1002 0.6381 0.6638 0.071 Uiso 1 1 calc R . .
C22 C 1.1396(12) 0.3719(14) 0.6640(6) 0.048(3) Uani 1 1 d . . .
H22A H 1.1093 0.4558 0.6277 0.072 Uiso 1 1 calc R . .
H22B H 1.0951 0.3060 0.6535 0.072 Uiso 1 1 calc R . .
H22C H 1.2421 0.3471 0.6609 0.072 Uiso 1 1 calc R . .
C23 C 1.1460(16) 0.0622(14) 0.7257(8) 0.063(3) Uani 1 1 d . . .
H23A H 1.0671 0.0895 0.6915 0.094 Uiso 1 1 calc R . .
H23B H 1.1778 -0.0317 0.7363 0.094 Uiso 1 1 calc R . .
H23C H 1.2235 0.1070 0.7029 0.094 Uiso 1 1 calc R . .
C24 C 1.2280(17) 0.0142(14) 0.8842(10) 0.076(5) Uani 1 1 d . . .
H24A H 1.3158 0.0466 0.8677 0.115 Uiso 1 1 calc R . .
H24B H 1.2423 -0.0785 0.8880 0.115 Uiso 1 1 calc R . .
H24C H 1.1995 0.0273 0.9329 0.115 Uiso 1 1 calc R . .
C25 C 0.9249(16) 0.0292(15) 0.8463(10) 0.069(4) Uani 1 1 d . . .
H25A H 0.9022 0.0267 0.8982 0.104 Uiso 1 1 calc R . .
H25B H 0.9427 -0.0593 0.8415 0.104 Uiso 1 1 calc R . .
H25C H 0.8458 0.0810 0.8151 0.104 Uiso 1 1 calc R . .
C26 C 0.6307(13) 0.8125(10) 0.5457(5) 0.043(2) Uani 1 1 d . . .
C27 C 0.5475(9) 0.8539(9) 0.6024(5) 0.0299(18) Uani 1 1 d . . .
C28 C 0.6234(11) 0.9050(9) 0.6437(5) 0.033(2) Uani 1 1 d . . .
C29 C 0.7662(12) 0.8875(10) 0.6161(6) 0.042(2) Uani 1 1 d . . .
C30 C 0.7714(10) 0.8283(10) 0.5580(6) 0.037(2) Uani 1 1 d . . .
C31 C 0.578(2) 0.7843(14) 0.4797(7) 0.069(4) Uani 1 1 d . . .
H31A H 0.5015 0.7353 0.4955 0.104 Uiso 1 1 calc R . .
H31B H 0.6555 0.7331 0.4583 0.104 Uiso 1 1 calc R . .
H31C H 0.5444 0.8660 0.4424 0.104 Uiso 1 1 calc R . .
C32 C 0.3857(10) 0.8547(11) 0.6109(7) 0.047(3) Uani 1 1 d . . .
H32A H 0.3591 0.8320 0.6636 0.071 Uiso 1 1 calc R . .
H32B H 0.3618 0.7914 0.5884 0.071 Uiso 1 1 calc R . .
H32C H 0.3349 0.9413 0.5859 0.071 Uiso 1 1 calc R . .
C33 C 0.5668(14) 0.9778(11) 0.6985(6) 0.047(3) Uani 1 1 d . . .
H33A H 0.5318 1.0687 0.6721 0.071 Uiso 1 1 calc R . .
H33B H 0.6417 0.9732 0.7319 0.071 Uiso 1 1 calc R . .
H33C H 0.4897 0.9393 0.7274 0.071 Uiso 1 1 calc R . .
C34 C 0.8823(13) 0.9355(12) 0.6406(8) 0.052(3) Uani 1 1 d . . .
H34A H 0.9718 0.9002 0.6201 0.078 Uiso 1 1 calc R . .
H34B H 0.8855 0.9076 0.6949 0.078 Uiso 1 1 calc R . .
H34C H 0.8664 1.0304 0.6231 0.078 Uiso 1 1 calc R . .
C35 C 0.8972(14) 0.8037(13) 0.5099(8) 0.057(3) Uani 1 1 d . . .
H35A H 0.9121 0.8857 0.4745 0.086 Uiso 1 1 calc R . .
H35B H 0.8819 0.7436 0.4828 0.086 Uiso 1 1 calc R . .
H35C H 0.9803 0.7658 0.5409 0.086 Uiso 1 1 calc R . .
H1 H 0.831(14) 0.700(13) 0.779(7) 0.050 Uiso 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
Ir1 N1 1.943(8) . ?
Ir1 C1 2.175(10) . ?
Ir1 C30 2.188(9) . ?
Ir1 C27 2.197(9) . ?
Ir1 C29 2.198(11) . ?
Ir1 C28 2.237(9) . ?
Ir1 C26 2.281(9) . ?
Ir1 Sc1 2.9416(15) . ?
Sc1 N1 2.042(7) . ?
Sc1 C1 2.139(9) . ?
Sc1 N2 2.338(7) . ?
Sc1 C17 2.527(9) . ?
Sc1 C18 2.545(9) . ?
Sc1 C16 2.575(8) . ?
Sc1 C14 2.584(9) . ?
Sc1 C15 2.593(8) . ?
N1 C5 1.499(10) . ?
N2 C13 1.329(11) . ?
N2 C9 1.351(12) . ?
Si1 C1 1.828(10) . ?
Si1 C3 1.874(11) . ?
Si1 C4 1.887(11) . ?
Si1 C2 1.912(11) . ?
Si2 C24 1.874(13) . ?
Si2 C14 1.880(10) . ?
Si2 C25 1.888(14) . ?
Si2 C23 1.903(14) . ?
C5 C7 1.500(14) . ?
C5 C6 1.534(14) . ?
C5 C8 1.550(13) . ?
C9 C10 1.352(16) . ?
C10 C11 1.396(17) . ?
C11 C12 1.379(16) . ?
C12 C13 1.375(14) . ?
C14 C18 1.428(14) . ?
C14 C15 1.455(12) . ?
C15 C16 1.374(14) . ?
C15 C19 1.517(13) . ?
C16 C17 1.422(13) . ?
C16 C20 1.516(13) . ?
C17 C18 1.399(14) . ?
C17 C21 1.520(15) . ?
C18 C22 1.515(12) . ?
C26 C27 1.418(15) . ?
C26 C30 1.449(16) . ?
C26 C31 1.508(15) . ?
C27 C28 1.399(13) . ?
C27 C32 1.562(12) . ?
C28 C29 1.439(16) . ?
C28 C33 1.492(14) . ?
C29 C30 1.418(16) . ?
C29 C34 1.483(16) . ?
C30 C35 1.493(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ir1 C1 88.5(3) . . ?
N1 Ir1 C30 121.5(4) . . ?
C1 Ir1 C30 133.6(4) . . ?
N1 Ir1 C27 133.8(3) . . ?
C1 Ir1 C27 123.3(4) . . ?
C30 Ir1 C27 62.2(4) . . ?
N1 Ir1 C29 152.1(4) . . ?
C1 Ir1 C29 99.6(4) . . ?
C30 Ir1 C29 37.7(4) . . ?
C27 Ir1 C29 62.0(3) . . ?
N1 Ir1 C28 168.6(4) . . ?
C1 Ir1 C28 94.7(4) . . ?
C30 Ir1 C28 63.1(4) . . ?
C27 Ir1 C28 36.8(3) . . ?
C29 Ir1 C28 37.9(4) . . ?
N1 Ir1 C26 113.9(3) . . ?
C1 Ir1 C26 157.1(4) . . ?
C30 Ir1 C26 37.8(4) . . ?
C27 Ir1 C26 36.8(4) . . ?
C29 Ir1 C26 62.8(4) . . ?
C28 Ir1 C26 62.4(4) . . ?
N1 Ir1 Sc1 43.7(2) . . ?
C1 Ir1 Sc1 46.5(2) . . ?
C30 Ir1 Sc1 137.8(3) . . ?
C27 Ir1 Sc1 160.0(2) . . ?
C29 Ir1 Sc1 131.2(3) . . ?
C28 Ir1 Sc1 141.2(3) . . ?
C26 Ir1 Sc1 156.3(3) . . ?
N1 Sc1 C1 87.0(3) . . ?
N1 Sc1 N2 92.4(3) . . ?
C1 Sc1 N2 103.2(3) . . ?
N1 Sc1 C17 114.1(3) . . ?
C1 Sc1 C17 95.0(4) . . ?
N2 Sc1 C17 148.6(3) . . ?
N1 Sc1 C18 102.2(3) . . ?
C1 Sc1 C18 125.4(4) . . ?
N2 Sc1 C18 129.5(3) . . ?
C17 Sc1 C18 32.0(3) . . ?
N1 Sc1 C16 145.9(3) . . ?
C1 Sc1 C16 90.3(3) . . ?
N2 Sc1 C16 121.2(3) . . ?
C17 Sc1 C16 32.3(3) . . ?
C18 Sc1 C16 53.3(3) . . ?
N1 Sc1 C14 120.4(3) . . ?
C1 Sc1 C14 143.5(3) . . ?
N2 Sc1 C14 99.5(3) . . ?
C17 Sc1 C14 53.4(3) . . ?
C18 Sc1 C14 32.3(3) . . ?
C16 Sc1 C14 53.3(3) . . ?
N1 Sc1 C15 152.7(3) . . ?
C1 Sc1 C15 115.7(3) . . ?
N2 Sc1 C15 96.5(3) . . ?
C17 Sc1 C15 52.3(3) . . ?
C18 Sc1 C15 52.9(3) . . ?
C16 Sc1 C15 30.8(3) . . ?
C14 Sc1 C15 32.7(3) . . ?
N1 Sc1 Ir1 41.2(2) . . ?
C1 Sc1 Ir1 47.5(3) . . ?
N2 Sc1 Ir1 109.73(19) . . ?
C17 Sc1 Ir1 101.4(2) . . ?
C18 Sc1 Ir1 112.9(2) . . ?
C16 Sc1 Ir1 120.4(2) . . ?
C14 Sc1 Ir1 144.5(2) . . ?
C15 Sc1 Ir1 151.0(2) . . ?
C5 N1 Ir1 126.0(6) . . ?
C5 N1 Sc1 138.7(6) . . ?
Ir1 N1 Sc1 95.1(3) . . ?
C13 N2 C9 116.7(8) . . ?
C13 N2 Sc1 116.0(6) . . ?
C9 N2 Sc1 127.0(6) . . ?
C1 Si1 C3 116.0(5) . . ?
C1 Si1 C4 112.8(5) . . ?
C3 Si1 C4 104.5(6) . . ?
C1 Si1 C2 114.2(5) . . ?
C3 Si1 C2 107.5(6) . . ?
C4 Si1 C2 100.2(6) . . ?
C24 Si2 C14 110.1(6) . . ?
C24 Si2 C25 107.5(8) . . ?
C14 Si2 C25 115.6(6) . . ?
C24 Si2 C23 106.0(7) . . ?
C14 Si2 C23 112.5(6) . . ?
C25 Si2 C23 104.5(7) . . ?
Si1 C1 Sc1 119.7(6) . . ?
Si1 C1 Ir1 127.1(5) . . ?
Sc1 C1 Ir1 86.0(3) . . ?
N1 C5 C7 110.9(8) . . ?
N1 C5 C6 110.2(7) . . ?
C7 C5 C6 111.4(9) . . ?
N1 C5 C8 107.7(7) . . ?
C7 C5 C8 108.7(8) . . ?
C6 C5 C8 107.9(9) . . ?
N2 C9 C10 123.6(9) . . ?
C9 C10 C11 119.5(10) . . ?
C12 C11 C10 117.2(11) . . ?
C13 C12 C11 119.6(10) . . ?
N2 C13 C12 123.4(9) . . ?
C18 C14 C15 105.2(8) . . ?
C18 C14 Si2 127.7(7) . . ?
C15 C14 Si2 125.0(7) . . ?
C18 C14 Sc1 72.3(5) . . ?
C15 C14 Sc1 74.0(5) . . ?
Si2 C14 Sc1 131.0(4) . . ?
C16 C15 C14 109.8(8) . . ?
C16 C15 C19 124.6(9) . . ?
C14 C15 C19 125.2(9) . . ?
C16 C15 Sc1 73.9(5) . . ?
C14 C15 Sc1 73.3(5) . . ?
C19 C15 Sc1 125.0(6) . . ?
C15 C16 C17 107.5(8) . . ?
C15 C16 C20 126.8(9) . . ?
C17 C16 C20 125.3(9) . . ?
C15 C16 Sc1 75.3(5) . . ?
C17 C16 Sc1 71.9(5) . . ?
C20 C16 Sc1 123.6(6) . . ?
C18 C17 C16 109.0(9) . . ?
C18 C17 C21 125.4(9) . . ?
C16 C17 C21 125.3(9) . . ?
C18 C17 Sc1 74.7(5) . . ?
C16 C17 Sc1 75.7(5) . . ?
C21 C17 Sc1 120.9(6) . . ?
C17 C18 C14 108.5(8) . . ?
C17 C18 C22 123.0(10) . . ?
C14 C18 C22 128.3(9) . . ?
C17 C18 Sc1 73.3(5) . . ?
C14 C18 Sc1 75.4(5) . . ?
C22 C18 Sc1 121.6(6) . . ?
C27 C26 C30 104.3(9) . . ?
C27 C26 C31 126.8(12) . . ?
C30 C26 C31 127.9(12) . . ?
C27 C26 Ir1 68.4(5) . . ?
C30 C26 Ir1 67.6(5) . . ?
C31 C26 Ir1 136.2(8) . . ?
C28 C27 C26 112.4(9) . . ?
C28 C27 C32 124.7(10) . . ?
C26 C27 C32 122.6(9) . . ?
C28 C27 Ir1 73.2(5) . . ?
C26 C27 Ir1 74.8(6) . . ?
C32 C27 Ir1 124.9(6) . . ?
C27 C28 C29 105.8(9) . . ?
C27 C28 C33 127.5(10) . . ?
C29 C28 C33 126.3(10) . . ?
C27 C28 Ir1 70.1(5) . . ?
C29 C28 Ir1 69.6(6) . . ?
C33 C28 Ir1 130.4(7) . . ?
C30 C29 C28 108.2(9) . . ?
C30 C29 C34 127.0(11) . . ?
C28 C29 C34 124.5(11) . . ?
C30 C29 Ir1 70.7(6) . . ?
C28 C29 Ir1 72.5(6) . . ?
C34 C29 Ir1 126.8(7) . . ?
C29 C30 C26 109.0(9) . . ?
C29 C30 C35 125.4(10) . . ?
C26 C30 C35 125.1(11) . . ?
C29 C30 Ir1 71.5(6) . . ?
C26 C30 Ir1 74.6(5) . . ?
C35 C30 Ir1 126.7(8) . . ?

_diffrn_measured_fraction_theta_max 0.955
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.955
_refine_diff_density_max         4.787
_refine_diff_density_min         -3.732
_refine_diff_density_rms         0.273
####################################################################### 
# 
# 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_16073ts
_database_code_depnum_ccdc_archive 'CCDC 962391'
_audit_update_record             
;
2013-09-20 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H62 Ir Lu N3 Si'
_chemical_formula_weight         1040.24

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 '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           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   46.05(3)
_cell_length_b                   9.620(6)
_cell_length_c                   19.635(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.619(11)
_cell_angle_gamma                90.00
_cell_volume                     8698(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    24115
_cell_measurement_theta_min      1.77
_cell_measurement_theta_max      26.24

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4120
_exptl_absorpt_coefficient_mu    5.374
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.2224
_exptl_absorpt_correction_T_max  0.6156
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24115
_diffrn_reflns_av_R_equivalents  0.1608
_diffrn_reflns_av_sigmaI/netI    0.3188
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         26.24
_reflns_number_total             8632
_reflns_number_gt                2888
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 
 [0.00000+1.00000exp(3.00(sinθ/λ)²)]/ 
   [σ²(Fo²)+0.0000+0.0000*P+(0.0000P)²+0.0000sinθ/λ] 
 where P = 0.33333Fo² + 0.66667Fc² 
;
_atom_sites_solution_primary     direct
_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         8632
_refine_ls_number_parameters     391
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1749
_refine_ls_R_factor_gt           0.0524
_refine_ls_wR_factor_ref         0.1112
_refine_ls_wR_factor_gt          0.0809
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_restrained_S_all      0.885
_refine_ls_shift/su_max          0.000
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.181391(12) 0.20513(7) 0.36376(3) 0.03055(17) Uani 1 1 d . . .
Lu1 Lu 0.135703(13) 0.22025(8) 0.24391(3) 0.03272(19) Uani 1 1 d . . .
N1 N 0.0958(2) 0.1694(13) 0.2984(7) 0.048(4) Uani 1 1 d . . .
N2 N 0.1621(2) 0.3462(12) 0.3139(7) 0.038(4) Uani 1 1 d . . .
N3 N 0.1042(3) 0.3974(14) 0.2093(8) 0.057(5) Uani 1 1 d . . .
Si1 Si 0.11029(10) 0.0627(5) 0.3626(3) 0.0465(13) Uani 1 1 d . . .
C1 C 0.1493(3) 0.0488(15) 0.3381(7) 0.027(4) Uani 1 1 d . . .
C2 C 0.1078(3) 0.1311(15) 0.4520(7) 0.038(4) Uani 1 1 d . . .
H2A H 0.1169 0.2230 0.4546 0.058 Uiso 1 1 calc R . .
H2B H 0.1178 0.0673 0.4833 0.058 Uiso 1 1 calc R . .
H2C H 0.0873 0.1387 0.4647 0.058 Uiso 1 1 calc R . .
C3 C 0.0938(3) -0.1141(16) 0.3624(8) 0.059(6) Uani 1 1 d . . .
H3A H 0.0728 -0.1065 0.3689 0.089 Uiso 1 1 calc R . .
H3B H 0.1024 -0.1693 0.3995 0.089 Uiso 1 1 calc R . .
H3C H 0.0976 -0.1597 0.3188 0.089 Uiso 1 1 calc R . .
C4 C 0.0665(4) 0.208(2) 0.2955(9) 0.063(6) Uani 1 1 d . . .
C5 C 0.0486(4) 0.142(2) 0.2535(12) 0.106(9) Uani 1 1 d . . .
H5A H 0.0557 0.0685 0.2258 0.127 Uiso 1 1 calc R . .
H5B H 0.0287 0.1671 0.2511 0.127 Uiso 1 1 calc R . .
C6 C 0.0576(5) 0.335(2) 0.3421(12) 0.085(3) Uani 1 1 d . . .
C7 C 0.0765(5) 0.415(2) 0.3715(11) 0.085(3) Uani 1 1 d . . .
H7 H 0.0967 0.3967 0.3670 0.102 Uiso 1 1 calc R . .
C8 C 0.0671(4) 0.527(2) 0.4098(11) 0.085(3) Uani 1 1 d . . .
H8 H 0.0807 0.5861 0.4324 0.102 Uiso 1 1 calc R . .
C9 C 0.0382(4) 0.551(2) 0.4142(12) 0.085(3) Uani 1 1 d . . .
H9 H 0.0318 0.6293 0.4395 0.102 Uiso 1 1 calc R . .
C10 C 0.0189(5) 0.473(2) 0.3860(12) 0.085(3) Uani 1 1 d . . .
H10 H -0.0011 0.4890 0.3939 0.102 Uiso 1 1 calc R . .
C11 C 0.0277(4) 0.3631(19) 0.3432(11) 0.085(3) Uani 1 1 d . . .
H11 H 0.0142 0.3112 0.3166 0.102 Uiso 1 1 calc R . .
C12 C 0.1655(3) 0.5475(15) 0.3888(7) 0.041(4) Uani 1 1 d . . .
H12A H 0.1699 0.6469 0.3919 0.061 Uiso 1 1 calc R . .
H12B H 0.1780 0.4960 0.4206 0.061 Uiso 1 1 calc R . .
H12C H 0.1451 0.5323 0.4006 0.061 Uiso 1 1 calc R . .
C13 C 0.2015(3) 0.5201(16) 0.2977(9) 0.061(6) Uani 1 1 d . . .
H13A H 0.2045 0.4904 0.2505 0.092 Uiso 1 1 calc R . .
H13B H 0.2142 0.4661 0.3281 0.092 Uiso 1 1 calc R . .
H13C H 0.2062 0.6191 0.3021 0.092 Uiso 1 1 calc R . .
C14 C 0.1509(4) 0.5791(15) 0.2711(9) 0.059(5) Uani 1 1 d . . .
H14A H 0.1541 0.6786 0.2787 0.088 Uiso 1 1 calc R . .
H14B H 0.1306 0.5562 0.2814 0.088 Uiso 1 1 calc R . .
H14C H 0.1548 0.5564 0.2235 0.088 Uiso 1 1 calc R . .
C15 C 0.1707(4) 0.4969(18) 0.3166(8) 0.045(5) Uani 1 1 d . . .
C16 C 0.0867(4) 0.4789(19) 0.1884(9) 0.051(5) Uani 1 1 d . . .
C17 C 0.0676(5) 0.591(2) 0.1731(14) 0.096(4) Uani 1 1 d . . .
C18 C 0.0541(4) 0.664(2) 0.2213(14) 0.096(4) Uani 1 1 d . . .
H18 H 0.0572 0.6427 0.2681 0.115 Uiso 1 1 calc R . .
C19 C 0.0355(4) 0.771(2) 0.2018(13) 0.096(4) Uani 1 1 d . . .
H19 H 0.0260 0.8255 0.2351 0.115 Uiso 1 1 calc R . .
C20 C 0.0308(4) 0.797(2) 0.1317(13) 0.096(4) Uani 1 1 d . . .
H20 H 0.0177 0.8677 0.1173 0.115 Uiso 1 1 calc R . .
C21 C 0.0442(4) 0.726(2) 0.0890(13) 0.096(4) Uani 1 1 d . . .
H21 H 0.0420 0.7513 0.0425 0.115 Uiso 1 1 calc R . .
C22 C 0.0617(4) 0.614(2) 0.1035(14) 0.096(4) Uani 1 1 d . . .
H22 H 0.0693 0.5557 0.0689 0.115 Uiso 1 1 calc R . .
C23 C 0.1248(3) 0.1507(18) 0.1161(9) 0.046(5) Uani 1 1 d . . .
C24 C 0.1368(3) 0.0345(16) 0.1454(8) 0.035(4) Uani 1 1 d . . .
C25 C 0.1663(3) 0.0664(16) 0.1614(7) 0.033(4) Uani 1 1 d . . .
C26 C 0.1715(3) 0.205(2) 0.1404(8) 0.051(5) Uani 1 1 d . . .
C27 C 0.1455(4) 0.2567(15) 0.1120(8) 0.042(4) Uani 1 1 d . . .
C28 C 0.0945(3) 0.1586(16) 0.0896(8) 0.051(5) Uani 1 1 d . . .
H28A H 0.0872 0.0646 0.0807 0.077 Uiso 1 1 calc R . .
H28B H 0.0941 0.2124 0.0472 0.077 Uiso 1 1 calc R . .
H28C H 0.0822 0.2041 0.1234 0.077 Uiso 1 1 calc R . .
C29 C 0.1227(3) -0.1013(15) 0.1587(8) 0.050(5) Uani 1 1 d . . .
H29A H 0.1017 -0.0878 0.1632 0.075 Uiso 1 1 calc R . .
H29B H 0.1306 -0.1411 0.2009 0.075 Uiso 1 1 calc R . .
H29C H 0.1265 -0.1646 0.1207 0.075 Uiso 1 1 calc R . .
C30 C 0.1897(3) -0.0323(18) 0.1873(8) 0.063(6) Uani 1 1 d . . .
H30A H 0.2016 -0.0633 0.1491 0.094 Uiso 1 1 calc R . .
H30B H 0.1806 -0.1130 0.2088 0.094 Uiso 1 1 calc R . .
H30C H 0.2021 0.0158 0.2207 0.094 Uiso 1 1 calc R . .
C31 C 0.2012(3) 0.274(2) 0.1421(9) 0.093(8) Uani 1 1 d . . .
H31A H 0.2074 0.2879 0.1895 0.139 Uiso 1 1 calc R . .
H31B H 0.2000 0.3644 0.1190 0.139 Uiso 1 1 calc R . .
H31C H 0.2152 0.2147 0.1188 0.139 Uiso 1 1 calc R . .
C32 C 0.1416(4) 0.3905(17) 0.0752(8) 0.064(6) Uani 1 1 d . . .
H32A H 0.1504 0.4659 0.1020 0.096 Uiso 1 1 calc R . .
H32B H 0.1208 0.4090 0.0687 0.096 Uiso 1 1 calc R . .
H32C H 0.1510 0.3850 0.0308 0.096 Uiso 1 1 calc R . .
C33 C 0.1966(3) 0.0663(17) 0.4512(8) 0.0344(18) Uani 1 1 d . . .
C34 C 0.1982(3) 0.2112(18) 0.4682(7) 0.0344(18) Uani 1 1 d . . .
C35 C 0.2188(3) 0.2764(17) 0.4290(7) 0.0344(18) Uani 1 1 d . . .
C36 C 0.2273(3) 0.1820(16) 0.3780(7) 0.0344(18) Uani 1 1 d . . .
C37 C 0.2151(3) 0.0528(17) 0.3906(7) 0.0344(18) Uani 1 1 d . . .
C38 C 0.1797(3) -0.0442(16) 0.4861(8) 0.052(5) Uani 1 1 d . . .
H38A H 0.1925 -0.0941 0.5180 0.078 Uiso 1 1 calc R . .
H38B H 0.1720 -0.1095 0.4521 0.078 Uiso 1 1 calc R . .
H38C H 0.1637 -0.0020 0.5110 0.078 Uiso 1 1 calc R . .
C39 C 0.1837(3) 0.2708(17) 0.5304(7) 0.052(5) Uani 1 1 d . . .
H39A H 0.1967 0.2610 0.5700 0.079 Uiso 1 1 calc R . .
H39B H 0.1656 0.2206 0.5388 0.079 Uiso 1 1 calc R . .
H39C H 0.1795 0.3694 0.5228 0.079 Uiso 1 1 calc R . .
C40 C 0.2334(4) 0.4131(17) 0.4456(9) 0.063(6) Uani 1 1 d . . .
H40A H 0.2465 0.4007 0.4848 0.094 Uiso 1 1 calc R . .
H40B H 0.2187 0.4827 0.4566 0.094 Uiso 1 1 calc R . .
H40C H 0.2446 0.4444 0.4063 0.094 Uiso 1 1 calc R . .
C41 C 0.2514(3) 0.2046(18) 0.3268(8) 0.057(5) Uani 1 1 d . . .
H41A H 0.2697 0.1677 0.3452 0.086 Uiso 1 1 calc R . .
H41B H 0.2535 0.3043 0.3178 0.086 Uiso 1 1 calc R . .
H41C H 0.2464 0.1564 0.2842 0.086 Uiso 1 1 calc R . .
C42 C 0.2212(3) -0.0825(16) 0.3605(8) 0.050(5) Uani 1 1 d . . .
H42A H 0.2183 -0.0773 0.3110 0.076 Uiso 1 1 calc R . .
H42B H 0.2079 -0.1520 0.3794 0.076 Uiso 1 1 calc R . .
H42C H 0.2413 -0.1090 0.3708 0.076 Uiso 1 1 calc R . .
C45 C 0.0260(4) 0.942(2) 0.4883(13) 0.078(7) Uani 1 1 d . . .
H45 H 0.0442 0.8993 0.4793 0.093 Uiso 1 1 calc R . .
C46 C 0.0099(4) 0.8906(19) 0.5408(11) 0.072(6) Uani 1 1 d . . .
H46 H 0.0172 0.8176 0.5687 0.086 Uiso 1 1 calc R . .
C47 C 0.0174(4) 1.0529(19) 0.4474(10) 0.056(5) Uani 1 1 d . . .
H47 H 0.0296 1.0886 0.4128 0.067 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
Ir1 N2 1.890(12) . ?
Ir1 C36 2.142(13) . ?
Ir1 C1 2.163(14) . ?
Ir1 C34 2.186(13) . ?
Ir1 C37 2.195(15) . ?
Ir1 C35 2.243(14) . ?
Ir1 C33 2.279(15) . ?
Ir1 Lu1 3.1429(18) . ?
Lu1 N2 2.190(12) . ?
Lu1 N1 2.191(11) . ?
Lu1 N3 2.336(15) . ?
Lu1 C1 2.552(14) . ?
Lu1 C25 2.617(14) . ?
Lu1 C26 2.633(13) . ?
Lu1 C24 2.634(15) . ?
Lu1 C23 2.642(17) . ?
Lu1 C27 2.657(15) . ?
Lu1 Si1 3.025(5) . ?
N1 C4 1.401(19) . ?
N1 Si1 1.752(14) . ?
N2 C15 1.505(18) . ?
N3 C16 1.19(2) . ?
Si1 C3 1.863(15) . ?
Si1 C1 1.870(13) . ?
Si1 C2 1.880(14) . ?
C4 C5 1.32(2) . ?
C4 C6 1.58(3) . ?
C6 C7 1.29(3) . ?
C6 C11 1.40(2) . ?
C7 C8 1.39(2) . ?
C8 C9 1.36(2) . ?
C9 C10 1.28(3) . ?
C10 C11 1.41(2) . ?
C12 C15 1.522(19) . ?
C13 C15 1.488(19) . ?
C14 C15 1.50(2) . ?
C16 C17 1.42(3) . ?
C17 C18 1.34(3) . ?
C17 C22 1.41(3) . ?
C18 C19 1.39(2) . ?
C19 C20 1.41(3) . ?
C20 C21 1.25(3) . ?
C21 C22 1.37(2) . ?
C23 C24 1.37(2) . ?
C23 C27 1.399(19) . ?
C23 C28 1.484(19) . ?
C24 C25 1.424(19) . ?
C24 C29 1.483(18) . ?
C25 C26 1.42(2) . ?
C25 C30 1.52(2) . ?
C26 C27 1.41(2) . ?
C26 C31 1.52(2) . ?
C27 C32 1.49(2) . ?
C33 C34 1.44(2) . ?
C33 C37 1.477(19) . ?
C33 C38 1.487(19) . ?
C34 C35 1.379(17) . ?
C34 C39 1.510(17) . ?
C35 C36 1.411(18) . ?
C35 C40 1.51(2) . ?
C36 C37 1.388(19) . ?
C36 C41 1.519(17) . ?
C37 C42 1.458(19) . ?
C45 C46 1.37(2) . ?
C45 C47 1.39(3) . ?
C46 C47 1.39(2) 5_576 ?
C47 C46 1.39(2) 5_576 ?

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
N2 Ir1 C36 126.9(5) . . ?
N2 Ir1 C1 93.6(5) . . ?
C36 Ir1 C1 129.0(5) . . ?
N2 Ir1 C34 128.8(6) . . ?
C36 Ir1 C34 62.7(5) . . ?
C1 Ir1 C34 118.1(6) . . ?
N2 Ir1 C37 158.7(5) . . ?
C36 Ir1 C37 37.3(5) . . ?
C1 Ir1 C37 94.1(5) . . ?
C34 Ir1 C37 63.2(5) . . ?
N2 Ir1 C35 115.5(6) . . ?
C36 Ir1 C35 37.4(5) . . ?
C1 Ir1 C35 149.7(6) . . ?
C34 Ir1 C35 36.3(4) . . ?
C37 Ir1 C35 62.0(6) . . ?
N2 Ir1 C33 161.7(5) . . ?
C36 Ir1 C33 63.0(5) . . ?
C1 Ir1 C33 88.3(6) . . ?
C34 Ir1 C33 37.4(5) . . ?
C37 Ir1 C33 38.5(5) . . ?
C35 Ir1 C33 61.4(6) . . ?
N2 Ir1 Lu1 43.2(4) . . ?
C36 Ir1 Lu1 139.0(4) . . ?
C1 Ir1 Lu1 53.7(4) . . ?
C34 Ir1 Lu1 158.3(3) . . ?
C37 Ir1 Lu1 132.6(4) . . ?
C35 Ir1 Lu1 156.5(4) . . ?
C33 Ir1 Lu1 142.0(4) . . ?
N2 Lu1 N1 106.2(5) . . ?
N2 Lu1 N3 96.8(5) . . ?
N1 Lu1 N3 77.4(5) . . ?
N2 Lu1 C1 76.8(5) . . ?
N1 Lu1 C1 72.7(4) . . ?
N3 Lu1 C1 146.1(5) . . ?
N2 Lu1 C25 113.8(4) . . ?
N1 Lu1 C25 129.5(5) . . ?
N3 Lu1 C25 124.7(5) . . ?
C1 Lu1 C25 87.3(4) . . ?
N2 Lu1 C26 99.7(5) . . ?
N1 Lu1 C26 154.0(5) . . ?
N3 Lu1 C26 102.0(6) . . ?
C1 Lu1 C26 111.9(5) . . ?
C25 Lu1 C26 31.3(5) . . ?
N2 Lu1 C24 145.2(4) . . ?
N1 Lu1 C24 103.3(5) . . ?
N3 Lu1 C24 107.3(5) . . ?
C1 Lu1 C24 95.0(5) . . ?
C25 Lu1 C24 31.5(4) . . ?
C26 Lu1 C24 51.6(5) . . ?
N2 Lu1 C23 146.7(5) . . ?
N1 Lu1 C23 104.8(5) . . ?
N3 Lu1 C23 78.3(5) . . ?
C1 Lu1 C23 124.6(5) . . ?
C25 Lu1 C23 50.7(5) . . ?
C26 Lu1 C23 50.7(5) . . ?
C24 Lu1 C23 30.1(4) . . ?
N2 Lu1 C27 116.1(5) . . ?
N1 Lu1 C27 131.1(5) . . ?
N3 Lu1 C27 74.4(5) . . ?
C1 Lu1 C27 138.5(4) . . ?
C25 Lu1 C27 51.2(5) . . ?
C26 Lu1 C27 30.8(5) . . ?
C24 Lu1 C27 50.9(5) . . ?
C23 Lu1 C27 30.6(4) . . ?
N2 Lu1 Si1 90.6(4) . . ?
N1 Lu1 Si1 34.8(3) . . ?
N3 Lu1 Si1 110.2(4) . . ?
C1 Lu1 Si1 38.0(3) . . ?
C25 Lu1 Si1 114.1(3) . . ?
C26 Lu1 Si1 144.8(5) . . ?
C24 Lu1 Si1 103.7(4) . . ?
C23 Lu1 Si1 122.2(4) . . ?
C27 Lu1 Si1 152.6(3) . . ?
N2 Lu1 Ir1 36.2(3) . . ?
N1 Lu1 Ir1 100.5(4) . . ?
N3 Lu1 Ir1 131.4(4) . . ?
C1 Lu1 Ir1 43.1(3) . . ?
C25 Lu1 Ir1 94.4(3) . . ?
C26 Lu1 Ir1 99.0(4) . . ?
C24 Lu1 Ir1 120.0(3) . . ?
C23 Lu1 Ir1 145.0(3) . . ?
C27 Lu1 Ir1 128.1(4) . . ?
Si1 Lu1 Ir1 70.22(11) . . ?
C4 N1 Si1 123.0(11) . . ?
C4 N1 Lu1 137.2(11) . . ?
Si1 N1 Lu1 99.6(5) . . ?
C15 N2 Ir1 123.5(10) . . ?
C15 N2 Lu1 134.4(10) . . ?
Ir1 N2 Lu1 100.5(5) . . ?
C16 N3 Lu1 174.1(16) . . ?
N1 Si1 C3 112.5(7) . . ?
N1 Si1 C1 102.5(6) . . ?
C3 Si1 C1 109.0(7) . . ?
N1 Si1 C2 116.1(7) . . ?
C3 Si1 C2 107.0(7) . . ?
C1 Si1 C2 109.5(7) . . ?
N1 Si1 Lu1 45.6(4) . . ?
C3 Si1 Lu1 128.1(5) . . ?
C1 Si1 Lu1 57.2(5) . . ?
C2 Si1 Lu1 124.9(5) . . ?
Si1 C1 Ir1 123.1(7) . . ?
Si1 C1 Lu1 84.8(5) . . ?
Ir1 C1 Lu1 83.2(5) . . ?
C5 C4 N1 119(2) . . ?
C5 C4 C6 124.8(19) . . ?
N1 C4 C6 115.9(16) . . ?
C7 C6 C11 122(2) . . ?
C7 C6 C4 122.7(19) . . ?
C11 C6 C4 115(2) . . ?
C6 C7 C8 120(2) . . ?
C9 C8 C7 119(2) . . ?
C10 C9 C8 123(2) . . ?
C9 C10 C11 120(2) . . ?
C6 C11 C10 116(2) . . ?
C13 C15 C14 110.5(15) . . ?
C13 C15 N2 112.9(13) . . ?
C14 C15 N2 109.2(13) . . ?
C13 C15 C12 110.2(14) . . ?
C14 C15 C12 106.5(14) . . ?
N2 C15 C12 107.2(13) . . ?
N3 C16 C17 170(2) . . ?
C18 C17 C22 121(2) . . ?
C18 C17 C16 123(3) . . ?
C22 C17 C16 116(2) . . ?
C17 C18 C19 119(3) . . ?
C18 C19 C20 119(2) . . ?
C21 C20 C19 119(2) . . ?
C20 C21 C22 126(3) . . ?
C21 C22 C17 116(2) . . ?
C24 C23 C27 110.2(15) . . ?
C24 C23 C28 124.2(16) . . ?
C27 C23 C28 125.5(16) . . ?
C24 C23 Lu1 74.6(10) . . ?
C27 C23 Lu1 75.3(9) . . ?
C28 C23 Lu1 119.2(10) . . ?
C23 C24 C25 107.3(14) . . ?
C23 C24 C29 128.0(15) . . ?
C25 C24 C29 124.7(15) . . ?
C23 C24 Lu1 75.3(10) . . ?
C25 C24 Lu1 73.6(9) . . ?
C29 C24 Lu1 117.2(10) . . ?
C26 C25 C24 107.6(14) . . ?
C26 C25 C30 124.3(15) . . ?
C24 C25 C30 127.7(15) . . ?
C26 C25 Lu1 75.0(8) . . ?
C24 C25 Lu1 74.9(8) . . ?
C30 C25 Lu1 122.0(10) . . ?
C27 C26 C25 107.6(14) . . ?
C27 C26 C31 128.0(18) . . ?
C25 C26 C31 124.0(18) . . ?
C27 C26 Lu1 75.5(8) . . ?
C25 C26 Lu1 73.7(8) . . ?
C31 C26 Lu1 122.0(11) . . ?
C23 C27 C26 107.4(14) . . ?
C23 C27 C32 125.5(17) . . ?
C26 C27 C32 126.6(16) . . ?
C23 C27 Lu1 74.1(9) . . ?
C26 C27 Lu1 73.7(9) . . ?
C32 C27 Lu1 124.5(10) . . ?
C34 C33 C37 104.1(13) . . ?
C34 C33 C38 127.9(14) . . ?
C37 C33 C38 128.0(14) . . ?
C34 C33 Ir1 67.8(8) . . ?
C37 C33 Ir1 67.7(8) . . ?
C38 C33 Ir1 127.5(11) . . ?
C35 C34 C33 110.3(13) . . ?
C35 C34 C39 126.3(15) . . ?
C33 C34 C39 122.3(14) . . ?
C35 C34 Ir1 74.1(8) . . ?
C33 C34 Ir1 74.8(8) . . ?
C39 C34 Ir1 127.9(9) . . ?
C34 C35 C36 107.6(14) . . ?
C34 C35 C40 125.6(14) . . ?
C36 C35 C40 125.9(13) . . ?
C34 C35 Ir1 69.6(8) . . ?
C36 C35 Ir1 67.4(8) . . ?
C40 C35 Ir1 136.6(11) . . ?
C37 C36 C35 109.5(13) . . ?
C37 C36 C41 123.1(14) . . ?
C35 C36 C41 126.0(14) . . ?
C37 C36 Ir1 73.4(9) . . ?
C35 C36 Ir1 75.2(8) . . ?
C41 C36 Ir1 128.6(10) . . ?
C36 C37 C42 130.3(14) . . ?
C36 C37 C33 107.7(14) . . ?
C42 C37 C33 121.3(14) . . ?
C36 C37 Ir1 69.3(9) . . ?
C42 C37 Ir1 129.5(11) . . ?
C33 C37 Ir1 73.8(8) . . ?
C46 C45 C47 123.8(19) . . ?
C45 C46 C47 118.9(19) . 5_576 ?
C46 C47 C45 117.2(18) 5_576 . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        26.24
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.687
_refine_diff_density_min         -1.230
_refine_diff_density_rms         0.177
####################################################################### 
# 
# 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_16047ts
_database_code_depnum_ccdc_archive 'CCDC 962392'
_audit_update_record             
;
2013-09-20 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H59 Ir Lu N3 Si'
_chemical_formula_weight         1001.18

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 '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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_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                   12.688(7)
_cell_length_b                   15.745(9)
_cell_length_c                   20.071(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.867(9)
_cell_angle_gamma                90.00
_cell_volume                     3989(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    24414
_cell_measurement_theta_min      1.65
_cell_measurement_theta_max      27.50

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1976
_exptl_absorpt_coefficient_mu    5.856
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.2029
_exptl_absorpt_correction_T_max  0.7584
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24414
_diffrn_reflns_av_R_equivalents  0.0938
_diffrn_reflns_av_sigmaI/netI    0.1962
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         27.50
_reflns_number_total             8868
_reflns_number_gt                4460
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 
 [0.00000+1.00000exp(3.00(sinθ/λ)²)]/ 
   [σ²(Fo²)+0.0000+0.0000*P+(0.0000P)²+0.0000sinθ/λ] 
 where P = 0.33333Fo² + 0.66667Fc² 
;
_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_number_reflns         8868
_refine_ls_number_parameters     451
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0424
_refine_ls_wR_factor_ref         0.0824
_refine_ls_wR_factor_gt          0.0698
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_restrained_S_all      0.963
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.55470(3) 0.58120(2) 0.218663(19) 0.02191(9) Uani 1 1 d . . .
Lu1 Lu 0.35466(3) 0.62005(2) 0.29828(2) 0.02120(10) Uani 1 1 d . . .
N1 N 0.2232(5) 0.5881(4) 0.2166(3) 0.0245(17) Uani 1 1 d . . .
N2 N 0.2481(6) 0.5327(4) 0.3527(4) 0.0276(19) Uani 1 1 d . . .
H2 H 0.2803 0.5097 0.3892 0.033 Uiso 1 1 calc R . .
N3 N 0.4935(5) 0.5366(4) 0.2949(4) 0.0223(17) Uani 1 1 d . . .
Si1 Si 0.28666(19) 0.60081(15) 0.14583(13) 0.0251(6) Uani 1 1 d . . .
C1 C 0.4119(6) 0.6527(5) 0.1829(4) 0.021(2) Uani 1 1 d . . .
C2 C 0.3107(7) 0.4970(6) 0.1078(5) 0.040(3) Uani 1 1 d . . .
H2A H 0.3586 0.4634 0.1389 0.061 Uiso 1 1 calc R . .
H2B H 0.3429 0.5056 0.0660 0.061 Uiso 1 1 calc R . .
H2C H 0.2433 0.4668 0.0984 0.061 Uiso 1 1 calc R . .
C3 C 0.2213(7) 0.6695(6) 0.0778(5) 0.045(3) Uani 1 1 d . . .
H3A H 0.1558 0.6423 0.0583 0.068 Uiso 1 1 calc R . .
H3B H 0.2692 0.6774 0.0430 0.068 Uiso 1 1 calc R . .
H3C H 0.2045 0.7248 0.0964 0.068 Uiso 1 1 calc R . .
C4 C 0.0882(7) 0.5276(5) 0.2797(5) 0.021(2) Uani 1 1 d . . .
C5 C 0.1241(7) 0.5605(5) 0.2228(4) 0.022(2) Uani 1 1 d . . .
C6 C 0.0423(6) 0.5699(6) 0.1644(5) 0.026(2) Uani 1 1 d . . .
C7 C 0.0136(8) 0.5018(6) 0.1219(5) 0.044(3) Uani 1 1 d . . .
H7 H 0.0475 0.4483 0.1283 0.053 Uiso 1 1 calc R . .
C8 C -0.0671(10) 0.5145(9) 0.0693(6) 0.069(4) Uani 1 1 d . . .
H8 H -0.0897 0.4680 0.0413 0.083 Uiso 1 1 calc R . .
C9 C -0.1137(9) 0.5921(10) 0.0573(6) 0.070(4) Uani 1 1 d . . .
H9 H -0.1652 0.5995 0.0200 0.084 Uiso 1 1 calc R . .
C10 C -0.0868(9) 0.6586(8) 0.0987(6) 0.063(4) Uani 1 1 d . . .
H10 H -0.1211 0.7120 0.0918 0.076 Uiso 1 1 calc R . .
C11 C -0.0092(8) 0.6474(7) 0.1507(5) 0.045(3) Uani 1 1 d . . .
H11 H 0.0105 0.6945 0.1788 0.054 Uiso 1 1 calc R . .
C12 C 0.1471(6) 0.5095(5) 0.3403(5) 0.023(2) Uani 1 1 d . . .
C13 C 0.0964(8) 0.4591(5) 0.3914(5) 0.028(2) Uani 1 1 d . . .
C14 C -0.0079(8) 0.4692(6) 0.4018(5) 0.035(2) Uani 1 1 d . . .
H14 H -0.0497 0.5089 0.3749 0.042 Uiso 1 1 calc R . .
C15 C -0.0535(8) 0.4249(7) 0.4488(5) 0.043(3) Uani 1 1 d . . .
H15 H -0.1258 0.4342 0.4552 0.052 Uiso 1 1 calc R . .
C16 C 0.0051(9) 0.3665(6) 0.4871(5) 0.046(3) Uani 1 1 d . . .
H16 H -0.0271 0.3342 0.5195 0.056 Uiso 1 1 calc R . .
C17 C 0.1095(10) 0.3544(6) 0.4790(6) 0.052(3) Uani 1 1 d . . .
H17 H 0.1502 0.3145 0.5062 0.062 Uiso 1 1 calc R . .
C18 C 0.1559(8) 0.4003(6) 0.4312(5) 0.041(3) Uani 1 1 d . . .
H18 H 0.2285 0.3917 0.4253 0.049 Uiso 1 1 calc R . .
C19 C 0.5421(8) 0.4688(6) 0.3385(5) 0.040(3) Uani 1 1 d . . .
C20 C 0.4686(8) 0.4472(7) 0.3913(5) 0.055(3) Uani 1 1 d . . .
H20A H 0.4625 0.4964 0.4206 0.083 Uiso 1 1 calc R . .
H20B H 0.4975 0.3988 0.4180 0.083 Uiso 1 1 calc R . .
H20C H 0.3984 0.4325 0.3693 0.083 Uiso 1 1 calc R . .
C21 C 0.5554(8) 0.3894(6) 0.2984(6) 0.053(3) Uani 1 1 d . . .
H21A H 0.4858 0.3693 0.2791 0.080 Uiso 1 1 calc R . .
H21B H 0.5895 0.3454 0.3277 0.080 Uiso 1 1 calc R . .
H21C H 0.5997 0.4018 0.2624 0.080 Uiso 1 1 calc R . .
C22 C 0.6498(7) 0.5013(6) 0.3740(5) 0.047(3) Uani 1 1 d . . .
H22A H 0.6928 0.5248 0.3406 0.071 Uiso 1 1 calc R . .
H22B H 0.6878 0.4539 0.3973 0.071 Uiso 1 1 calc R . .
H22C H 0.6364 0.5454 0.4065 0.071 Uiso 1 1 calc R . .
C23 C 0.3160(8) 0.7832(5) 0.3103(5) 0.031(2) Uani 1 1 d . . .
C24 C 0.4246(7) 0.7707(5) 0.3307(5) 0.032(2) Uani 1 1 d . . .
C25 C 0.4318(8) 0.7255(6) 0.3922(5) 0.040(3) Uani 1 1 d . . .
C26 C 0.3268(8) 0.7080(6) 0.4072(5) 0.033(2) Uani 1 1 d . . .
C27 C 0.2579(7) 0.7435(5) 0.3564(5) 0.029(2) Uani 1 1 d . . .
C28 C 0.2711(8) 0.8323(6) 0.2497(5) 0.042(3) Uani 1 1 d . . .
H28A H 0.2131 0.8000 0.2258 0.063 Uiso 1 1 calc R . .
H28B H 0.3267 0.8418 0.2201 0.063 Uiso 1 1 calc R . .
H28C H 0.2443 0.8871 0.2639 0.063 Uiso 1 1 calc R . .
C29 C 0.5182(8) 0.8041(5) 0.2998(6) 0.046(3) Uani 1 1 d . . .
H29A H 0.5562 0.8449 0.3304 0.068 Uiso 1 1 calc R . .
H29B H 0.4944 0.8325 0.2575 0.068 Uiso 1 1 calc R . .
H29C H 0.5655 0.7570 0.2913 0.068 Uiso 1 1 calc R . .
C30 C 0.5329(8) 0.7077(7) 0.4375(5) 0.055(3) Uani 1 1 d . . .
H30A H 0.5933 0.7072 0.4107 0.082 Uiso 1 1 calc R . .
H30B H 0.5272 0.6523 0.4592 0.082 Uiso 1 1 calc R . .
H30C H 0.5434 0.7521 0.4718 0.082 Uiso 1 1 calc R . .
C31 C 0.2961(8) 0.6685(7) 0.4709(5) 0.052(3) Uani 1 1 d . . .
H31A H 0.2812 0.7134 0.5024 0.078 Uiso 1 1 calc R . .
H31B H 0.3543 0.6329 0.4909 0.078 Uiso 1 1 calc R . .
H31C H 0.2326 0.6334 0.4607 0.078 Uiso 1 1 calc R . .
C32 C 0.1368(7) 0.7433(6) 0.3537(6) 0.046(3) Uani 1 1 d . . .
H32A H 0.1115 0.6848 0.3565 0.069 Uiso 1 1 calc R . .
H32B H 0.1065 0.7688 0.3114 0.069 Uiso 1 1 calc R . .
H32C H 0.1150 0.7764 0.3913 0.069 Uiso 1 1 calc R . .
C33 C 0.6142(7) 0.5992(6) 0.1198(5) 0.030(2) Uani 1 1 d . . .
C34 C 0.6443(7) 0.5170(6) 0.1450(5) 0.029(2) Uani 1 1 d . . .
C35 C 0.7149(6) 0.5288(5) 0.2059(5) 0.026(2) Uani 1 1 d . . .
C36 C 0.7200(6) 0.6165(6) 0.2192(5) 0.028(2) Uani 1 1 d . . .
C37 C 0.6626(6) 0.6615(5) 0.1646(5) 0.025(2) Uani 1 1 d . . .
C38 C 0.5545(7) 0.6156(6) 0.0531(5) 0.040(3) Uani 1 1 d . . .
H38A H 0.6029 0.6120 0.0181 0.060 Uiso 1 1 calc R . .
H38B H 0.5231 0.6725 0.0527 0.060 Uiso 1 1 calc R . .
H38C H 0.4982 0.5732 0.0445 0.060 Uiso 1 1 calc R . .
C39 C 0.6208(8) 0.4348(6) 0.1111(5) 0.052(3) Uani 1 1 d . . .
H39A H 0.5526 0.4384 0.0837 0.077 Uiso 1 1 calc R . .
H39B H 0.6177 0.3901 0.1448 0.077 Uiso 1 1 calc R . .
H39C H 0.6767 0.4215 0.0825 0.077 Uiso 1 1 calc R . .
C40 C 0.7883(7) 0.4611(6) 0.2359(5) 0.042(3) Uani 1 1 d . . .
H40A H 0.8452 0.4519 0.2072 0.062 Uiso 1 1 calc R . .
H40B H 0.7487 0.4081 0.2397 0.062 Uiso 1 1 calc R . .
H40C H 0.8188 0.4790 0.2805 0.062 Uiso 1 1 calc R . .
C41 C 0.7889(7) 0.6608(6) 0.2751(5) 0.042(3) Uani 1 1 d . . .
H41A H 0.8058 0.6211 0.3123 0.062 Uiso 1 1 calc R . .
H41B H 0.7507 0.7097 0.2909 0.062 Uiso 1 1 calc R . .
H41C H 0.8546 0.6802 0.2583 0.062 Uiso 1 1 calc R . .
C42 C 0.6557(7) 0.7560(5) 0.1561(5) 0.035(3) Uani 1 1 d . . .
H42A H 0.6789 0.7838 0.1988 0.053 Uiso 1 1 calc R . .
H42B H 0.5822 0.7721 0.1417 0.053 Uiso 1 1 calc R . .
H42C H 0.7014 0.7740 0.1221 0.053 Uiso 1 1 calc R . .
H4 H 0.018(7) 0.507(5) 0.271(5) 0.050 Uiso 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
Ir1 N3 1.919(7) . ?
Ir1 C36 2.169(8) . ?
Ir1 C1 2.191(8) . ?
Ir1 C34 2.202(9) . ?
Ir1 C33 2.213(9) . ?
Ir1 C37 2.226(8) . ?
Ir1 C35 2.233(8) . ?
Ir1 Lu1 3.1934(14) . ?
Lu1 N3 2.204(7) . ?
Lu1 N1 2.272(6) . ?
Lu1 N2 2.283(7) . ?
Lu1 C1 2.549(9) . ?
Lu1 C24 2.592(8) . ?
Lu1 C25 2.625(9) . ?
Lu1 C23 2.631(9) . ?
Lu1 C27 2.634(9) . ?
Lu1 C26 2.641(10) . ?
Lu1 Si1 3.108(3) . ?
N1 C5 1.348(10) . ?
N1 Si1 1.715(7) . ?
N2 C12 1.332(10) . ?
N3 C19 1.475(10) . ?
Si1 C2 1.842(9) . ?
Si1 C3 1.869(9) . ?
Si1 C1 1.872(8) . ?
C4 C5 1.373(12) . ?
C4 C12 1.389(11) . ?
C5 C6 1.492(11) . ?
C6 C7 1.394(12) . ?
C6 C11 1.398(12) . ?
C7 C8 1.408(14) . ?
C8 C9 1.367(16) . ?
C9 C10 1.359(15) . ?
C10 C11 1.371(13) . ?
C12 C13 1.493(12) . ?
C13 C14 1.370(12) . ?
C13 C18 1.394(12) . ?
C14 C15 1.351(12) . ?
C15 C16 1.369(14) . ?
C16 C17 1.365(13) . ?
C17 C18 1.380(13) . ?
C19 C21 1.506(13) . ?
C19 C20 1.520(13) . ?
C19 C22 1.561(13) . ?
C23 C27 1.388(12) . ?
C23 C24 1.410(12) . ?
C23 C28 1.503(12) . ?
C24 C25 1.420(13) . ?
C24 C29 1.490(12) . ?
C25 C26 1.422(12) . ?
C25 C30 1.521(12) . ?
C26 C27 1.391(12) . ?
C26 C31 1.509(13) . ?
C27 C32 1.532(12) . ?
C33 C34 1.427(12) . ?
C33 C37 1.428(12) . ?
C33 C38 1.492(12) . ?
C34 C35 1.452(12) . ?
C34 C39 1.476(12) . ?
C35 C36 1.407(11) . ?
C35 C40 1.500(11) . ?
C36 C37 1.438(11) . ?
C36 C41 1.521(11) . ?
C37 C42 1.500(11) . ?

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
N3 Ir1 C36 124.1(3) . . ?
N3 Ir1 C1 93.5(3) . . ?
C36 Ir1 C1 129.6(3) . . ?
N3 Ir1 C34 130.3(3) . . ?
C36 Ir1 C34 63.6(3) . . ?
C1 Ir1 C34 118.8(3) . . ?
N3 Ir1 C33 164.9(3) . . ?
C36 Ir1 C33 63.4(3) . . ?
C1 Ir1 C33 89.3(3) . . ?
C34 Ir1 C33 37.7(3) . . ?
N3 Ir1 C37 156.3(3) . . ?
C36 Ir1 C37 38.2(3) . . ?
C1 Ir1 C37 94.5(3) . . ?
C34 Ir1 C37 63.1(3) . . ?
C33 Ir1 C37 37.5(3) . . ?
N3 Ir1 C35 113.8(3) . . ?
C36 Ir1 C35 37.2(3) . . ?
C1 Ir1 C35 152.2(3) . . ?
C34 Ir1 C35 38.2(3) . . ?
C33 Ir1 C35 63.0(3) . . ?
C37 Ir1 C35 62.7(3) . . ?
N3 Ir1 Lu1 42.60(19) . . ?
C36 Ir1 Lu1 140.0(2) . . ?
C1 Ir1 Lu1 52.6(2) . . ?
C34 Ir1 Lu1 156.3(2) . . ?
C33 Ir1 Lu1 141.8(2) . . ?
C37 Ir1 Lu1 134.0(2) . . ?
C35 Ir1 Lu1 155.2(2) . . ?
N3 Lu1 N1 112.1(3) . . ?
N3 Lu1 N2 99.8(2) . . ?
N1 Lu1 N2 77.6(3) . . ?
N3 Lu1 C1 77.9(3) . . ?
N1 Lu1 C1 69.2(3) . . ?
N2 Lu1 C1 142.5(3) . . ?
N3 Lu1 C24 107.4(3) . . ?
N1 Lu1 C24 126.2(3) . . ?
N2 Lu1 C24 129.5(3) . . ?
C1 Lu1 C24 85.5(3) . . ?
N3 Lu1 C25 99.1(3) . . ?
N1 Lu1 C25 148.2(3) . . ?
N2 Lu1 C25 103.5(3) . . ?
C1 Lu1 C25 113.9(3) . . ?
C24 Lu1 C25 31.6(3) . . ?
N3 Lu1 C23 137.9(3) . . ?
N1 Lu1 C23 98.8(3) . . ?
N2 Lu1 C23 114.8(3) . . ?
C1 Lu1 C23 87.7(3) . . ?
C24 Lu1 C23 31.3(3) . . ?
C25 Lu1 C23 51.4(3) . . ?
N3 Lu1 C27 149.7(3) . . ?
N1 Lu1 C27 98.2(3) . . ?
N2 Lu1 C27 84.7(3) . . ?
C1 Lu1 C27 116.3(3) . . ?
C24 Lu1 C27 51.4(3) . . ?
C25 Lu1 C27 51.1(3) . . ?
C23 Lu1 C27 30.6(3) . . ?
N3 Lu1 C26 120.8(3) . . ?
N1 Lu1 C26 124.2(3) . . ?
N2 Lu1 C26 77.5(3) . . ?
C1 Lu1 C26 136.1(3) . . ?
C24 Lu1 C26 52.0(3) . . ?
C25 Lu1 C26 31.3(3) . . ?
C23 Lu1 C26 51.0(3) . . ?
C27 Lu1 C26 30.6(3) . . ?
N3 Lu1 Si1 93.10(19) . . ?
N1 Lu1 Si1 32.73(18) . . ?
N2 Lu1 Si1 107.08(19) . . ?
C1 Lu1 Si1 37.00(18) . . ?
C24 Lu1 Si1 112.9(2) . . ?
C25 Lu1 Si1 144.5(2) . . ?
C23 Lu1 Si1 98.6(2) . . ?
C27 Lu1 Si1 114.4(2) . . ?
C26 Lu1 Si1 144.9(2) . . ?
N3 Lu1 Ir1 36.10(18) . . ?
N1 Lu1 Ir1 99.15(18) . . ?
N2 Lu1 Ir1 131.58(18) . . ?
C1 Lu1 Ir1 43.05(18) . . ?
C24 Lu1 Ir1 91.8(2) . . ?
C25 Lu1 Ir1 102.9(2) . . ?
C23 Lu1 Ir1 113.5(2) . . ?
C27 Lu1 Ir1 142.5(2) . . ?
C26 Lu1 Ir1 134.0(2) . . ?
Si1 Lu1 Ir1 69.12(6) . . ?
C5 N1 Si1 129.5(6) . . ?
C5 N1 Lu1 128.9(6) . . ?
Si1 N1 Lu1 101.5(3) . . ?
C12 N2 Lu1 133.0(6) . . ?
C19 N3 Ir1 124.0(6) . . ?
C19 N3 Lu1 134.5(6) . . ?
Ir1 N3 Lu1 101.3(3) . . ?
N1 Si1 C2 110.6(4) . . ?
N1 Si1 C3 117.5(4) . . ?
C2 Si1 C3 106.9(5) . . ?
N1 Si1 C1 100.0(4) . . ?
C2 Si1 C1 112.5(4) . . ?
C3 Si1 C1 109.5(4) . . ?
N1 Si1 Lu1 45.8(2) . . ?
C2 Si1 Lu1 116.9(3) . . ?
C3 Si1 Lu1 136.1(3) . . ?
C1 Si1 Lu1 55.1(3) . . ?
Si1 C1 Ir1 123.1(4) . . ?
Si1 C1 Lu1 87.9(3) . . ?
Ir1 C1 Lu1 84.4(3) . . ?
C5 C4 C12 127.6(8) . . ?
N1 C5 C4 126.2(8) . . ?
N1 C5 C6 118.4(8) . . ?
C4 C5 C6 115.3(8) . . ?
C7 C6 C11 117.6(9) . . ?
C7 C6 C5 121.4(9) . . ?
C11 C6 C5 121.0(8) . . ?
C6 C7 C8 118.3(10) . . ?
C9 C8 C7 121.8(11) . . ?
C10 C9 C8 120.3(12) . . ?
C9 C10 C11 118.8(11) . . ?
C10 C11 C6 123.2(11) . . ?
N2 C12 C4 121.9(8) . . ?
N2 C12 C13 119.4(8) . . ?
C4 C12 C13 118.7(8) . . ?
C14 C13 C18 117.7(9) . . ?
C14 C13 C12 122.2(8) . . ?
C18 C13 C12 120.0(9) . . ?
C15 C14 C13 122.4(10) . . ?
C14 C15 C16 119.5(11) . . ?
C17 C16 C15 120.4(10) . . ?
C16 C17 C18 119.9(11) . . ?
C17 C18 C13 120.1(10) . . ?
N3 C19 C21 110.3(9) . . ?
N3 C19 C20 109.0(8) . . ?
C21 C19 C20 107.3(9) . . ?
N3 C19 C22 109.1(8) . . ?
C21 C19 C22 112.1(8) . . ?
C20 C19 C22 109.0(9) . . ?
C27 C23 C24 108.3(9) . . ?
C27 C23 C28 125.9(9) . . ?
C24 C23 C28 125.8(9) . . ?
C27 C23 Lu1 74.8(5) . . ?
C24 C23 Lu1 72.8(5) . . ?
C28 C23 Lu1 119.1(6) . . ?
C23 C24 C25 107.2(9) . . ?
C23 C24 C29 128.8(10) . . ?
C25 C24 C29 123.7(9) . . ?
C23 C24 Lu1 75.9(5) . . ?
C25 C24 Lu1 75.5(5) . . ?
C29 C24 Lu1 119.1(6) . . ?
C24 C25 C26 107.6(9) . . ?
C24 C25 C30 126.0(9) . . ?
C26 C25 C30 126.1(10) . . ?
C24 C25 Lu1 72.9(5) . . ?
C26 C25 Lu1 74.9(5) . . ?
C30 C25 Lu1 122.8(7) . . ?
C27 C26 C25 107.4(9) . . ?
C27 C26 C31 126.1(9) . . ?
C25 C26 C31 126.0(9) . . ?
C27 C26 Lu1 74.4(6) . . ?
C25 C26 Lu1 73.7(6) . . ?
C31 C26 Lu1 123.6(6) . . ?
C23 C27 C26 109.4(9) . . ?
C23 C27 C32 125.2(9) . . ?
C26 C27 C32 125.3(9) . . ?
C23 C27 Lu1 74.6(5) . . ?
C26 C27 Lu1 75.0(5) . . ?
C32 C27 Lu1 119.6(6) . . ?
C34 C33 C37 108.5(8) . . ?
C34 C33 C38 124.6(8) . . ?
C37 C33 C38 126.4(8) . . ?
C34 C33 Ir1 70.7(5) . . ?
C37 C33 Ir1 71.7(5) . . ?
C38 C33 Ir1 129.7(6) . . ?
C33 C34 C35 107.6(8) . . ?
C33 C34 C39 126.7(9) . . ?
C35 C34 C39 125.3(8) . . ?
C33 C34 Ir1 71.6(5) . . ?
C35 C34 Ir1 72.0(5) . . ?
C39 C34 Ir1 128.1(7) . . ?
C36 C35 C34 107.3(8) . . ?
C36 C35 C40 127.4(8) . . ?
C34 C35 C40 123.5(8) . . ?
C36 C35 Ir1 68.9(4) . . ?
C34 C35 Ir1 69.7(5) . . ?
C40 C35 Ir1 138.7(7) . . ?
C35 C36 C37 109.3(8) . . ?
C35 C36 C41 127.0(8) . . ?
C37 C36 C41 123.0(9) . . ?
C35 C36 Ir1 73.8(5) . . ?
C37 C36 Ir1 73.1(5) . . ?
C41 C36 Ir1 127.1(6) . . ?
C33 C37 C36 107.1(8) . . ?
C33 C37 C42 126.4(8) . . ?
C36 C37 C42 126.5(8) . . ?
C33 C37 Ir1 70.8(5) . . ?
C36 C37 Ir1 68.8(5) . . ?
C42 C37 Ir1 126.0(6) . . ?

_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.968
_refine_diff_density_max         2.441
_refine_diff_density_min         -1.567
_refine_diff_density_rms         0.194
####################################################################### 
# 
# 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_16109ts
_database_code_depnum_ccdc_archive 'CCDC 962393'
_audit_update_record             
;
2013-09-20 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H54 Ir Lu N2 O Si'
_chemical_formula_weight         926.07

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 '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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.431(2)
_cell_length_b                   10.568(3)
_cell_length_c                   18.813(5)
_cell_angle_alpha                85.387(4)
_cell_angle_beta                 79.968(3)
_cell_angle_gamma                74.367(3)
_cell_volume                     1776.9(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    10513
_cell_measurement_theta_min      2.00
_cell_measurement_theta_max      26.50

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             908
_exptl_absorpt_coefficient_mu    6.565
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.1787
_exptl_absorpt_correction_T_max  0.5597
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10513
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_av_sigmaI/netI    0.1299
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         26.50
_reflns_number_total             7120
_reflns_number_gt                4577
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0924P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7120
_refine_ls_number_parameters     340
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0715
_refine_ls_wR_factor_ref         0.1743
_refine_ls_wR_factor_gt          0.1669
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_restrained_S_all      0.924
_refine_ls_shift/su_max          0.017
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.35760(5) 0.74075(5) 0.34094(3) 0.02167(17) Uani 1 1 d . . .
Lu1 Lu 0.31138(6) 0.98377(5) 0.22617(3) 0.02274(17) Uani 1 1 d . . .
N1 N 0.2074(12) 0.8374(12) 0.2854(6) 0.029(3) Uani 1 1 d . . .
N2 N 0.1307(13) 1.0738(14) 0.1470(7) 0.037(3) Uani 1 1 d . . .
O1 O 0.4294(11) 0.9241(10) 0.1253(5) 0.037(2) Uani 1 1 d . . .
Si1 Si 0.6043(4) 0.7013(4) 0.1750(2) 0.0267(8) Uani 1 1 d . . .
C1 C 0.5366(14) 0.7902(12) 0.2619(6) 0.020(3) Uani 1 1 d . . .
C2 C 0.508(2) 0.5702(16) 0.1699(8) 0.046(4) Uani 1 1 d . . .
H2A H 0.4026 0.6016 0.1902 0.070 Uiso 1 1 calc R . .
H2B H 0.5542 0.4917 0.1976 0.070 Uiso 1 1 calc R . .
H2C H 0.5180 0.5482 0.1194 0.070 Uiso 1 1 calc R . .
C3 C 0.8113(17) 0.6227(16) 0.1606(8) 0.042(4) Uani 1 1 d . . .
H3A H 0.8436 0.5924 0.1111 0.063 Uiso 1 1 calc R . .
H3B H 0.8337 0.5477 0.1947 0.063 Uiso 1 1 calc R . .
H3C H 0.8641 0.6873 0.1685 0.063 Uiso 1 1 calc R . .
C4 C 0.5570(15) 0.8327(14) 0.1031(7) 0.029(3) Uani 1 1 d . . .
C5 C 0.6389(18) 0.8338(18) 0.0393(8) 0.048(5) Uani 1 1 d . . .
H5A H 0.6096 0.9025 0.0049 0.058 Uiso 1 1 calc R . .
H5B H 0.7277 0.7659 0.0275 0.058 Uiso 1 1 calc R . .
C6 C 0.0497(15) 0.8233(13) 0.3012(8) 0.031(3) Uani 1 1 d . . .
C7 C 0.0516(17) 0.6781(15) 0.2980(9) 0.040(4) Uani 1 1 d . . .
H7A H -0.0458 0.6655 0.3202 0.060 Uiso 1 1 calc R . .
H7B H 0.1290 0.6234 0.3241 0.060 Uiso 1 1 calc R . .
H7C H 0.0730 0.6528 0.2475 0.060 Uiso 1 1 calc R . .
C8 C -0.0371(16) 0.8975(16) 0.2433(10) 0.045(4) Uani 1 1 d . . .
H8A H -0.0420 0.9912 0.2439 0.068 Uiso 1 1 calc R . .
H8B H -0.1384 0.8857 0.2527 0.068 Uiso 1 1 calc R . .
H8C H 0.0129 0.8635 0.1959 0.068 Uiso 1 1 calc R . .
C9 C -0.0289(16) 0.8806(17) 0.3740(8) 0.043(4) Uani 1 1 d . . .
H9A H -0.0384 0.9755 0.3720 0.065 Uiso 1 1 calc R . .
H9B H 0.0296 0.8384 0.4118 0.065 Uiso 1 1 calc R . .
H9C H -0.1282 0.8648 0.3850 0.065 Uiso 1 1 calc R . .
C10 C 0.5185(15) 0.5735(14) 0.3867(8) 0.031(3) Uani 1 1 d . . .
C11 C 0.3808(16) 0.5374(14) 0.3911(7) 0.030(3) Uani 1 1 d . . .
C12 C 0.2721(15) 0.6263(13) 0.4366(7) 0.028(3) Uani 1 1 d . . .
C13 C 0.3405(15) 0.7167(13) 0.4587(6) 0.023(3) Uani 1 1 d . . .
C14 C 0.4966(14) 0.6829(15) 0.4288(6) 0.026(3) Uani 1 1 d . . .
C15 C 0.6707(16) 0.4928(16) 0.3487(9) 0.042(4) Uani 1 1 d . . .
H15A H 0.7366 0.5509 0.3335 0.063 Uiso 1 1 calc R . .
H15B H 0.6564 0.4525 0.3062 0.063 Uiso 1 1 calc R . .
H15C H 0.7158 0.4239 0.3821 0.063 Uiso 1 1 calc R . .
C16 C 0.365(2) 0.4216(16) 0.3570(9) 0.050(5) Uani 1 1 d . . .
H16A H 0.4198 0.3410 0.3801 0.076 Uiso 1 1 calc R . .
H16B H 0.4060 0.4239 0.3054 0.076 Uiso 1 1 calc R . .
H16C H 0.2595 0.4230 0.3628 0.076 Uiso 1 1 calc R . .
C17 C 0.1269(17) 0.6035(17) 0.4745(9) 0.046(4) Uani 1 1 d . . .
H17A H 0.0864 0.5583 0.4425 0.070 Uiso 1 1 calc R . .
H17B H 0.0561 0.6881 0.4872 0.070 Uiso 1 1 calc R . .
H17C H 0.1435 0.5491 0.5185 0.070 Uiso 1 1 calc R . .
C18 C 0.2704(19) 0.8213(17) 0.5117(8) 0.042(4) Uani 1 1 d . . .
H18A H 0.1659 0.8591 0.5060 0.063 Uiso 1 1 calc R . .
H18B H 0.3238 0.8902 0.5033 0.063 Uiso 1 1 calc R . .
H18C H 0.2753 0.7834 0.5608 0.063 Uiso 1 1 calc R . .
C19 C 0.6152(16) 0.7390(14) 0.4453(9) 0.036(4) Uani 1 1 d . . .
H19A H 0.6752 0.6773 0.4772 0.054 Uiso 1 1 calc R . .
H19B H 0.5693 0.8224 0.4694 0.054 Uiso 1 1 calc R . .
H19C H 0.6793 0.7543 0.4003 0.054 Uiso 1 1 calc R . .
C20 C 0.4414(16) 1.1717(15) 0.2347(8) 0.034(3) Uani 1 1 d . . .
C21 C 0.4133(16) 1.1188(12) 0.3057(8) 0.030(3) Uani 1 1 d . . .
C22 C 0.2549(17) 1.1546(14) 0.3295(7) 0.033(3) Uani 1 1 d . . .
C23 C 0.1875(16) 1.2232(13) 0.2697(9) 0.034(3) Uani 1 1 d . . .
C24 C 0.2995(18) 1.2363(14) 0.2140(8) 0.034(3) Uani 1 1 d . . .
C25 C 0.5921(18) 1.1623(17) 0.1920(10) 0.052(2) Uani 1 1 d . . .
H25A H 0.6643 1.1541 0.2248 0.078 Uiso 1 1 calc R . .
H25B H 0.5897 1.2417 0.1609 0.078 Uiso 1 1 calc R . .
H25C H 0.6214 1.0850 0.1620 0.078 Uiso 1 1 calc R . .
C26 C 0.5259(19) 1.0581(17) 0.3537(10) 0.052(2) Uani 1 1 d . . .
H26A H 0.5920 0.9769 0.3328 0.078 Uiso 1 1 calc R . .
H26B H 0.4747 1.0379 0.4015 0.078 Uiso 1 1 calc R . .
H26C H 0.5848 1.1196 0.3584 0.078 Uiso 1 1 calc R . .
C27 C 0.1784(19) 1.1315(18) 0.4027(10) 0.052(2) Uani 1 1 d . . .
H27A H 0.2047 1.1831 0.4370 0.078 Uiso 1 1 calc R . .
H27B H 0.2093 1.0379 0.4164 0.078 Uiso 1 1 calc R . .
H27C H 0.0702 1.1583 0.4034 0.078 Uiso 1 1 calc R . .
C28 C 0.0255(18) 1.2904(17) 0.2767(10) 0.052(2) Uani 1 1 d . . .
H28A H 0.0075 1.3790 0.2944 0.078 Uiso 1 1 calc R . .
H28B H -0.0311 1.2400 0.3109 0.078 Uiso 1 1 calc R . .
H28C H -0.0066 1.2965 0.2295 0.078 Uiso 1 1 calc R . .
C29 C 0.2801(19) 1.3179(17) 0.1431(10) 0.052(2) Uani 1 1 d . . .
H29A H 0.3705 1.2899 0.1075 0.078 Uiso 1 1 calc R . .
H29B H 0.2626 1.4112 0.1522 0.078 Uiso 1 1 calc R . .
H29C H 0.1947 1.3044 0.1244 0.078 Uiso 1 1 calc R . .
C30 C 0.0488(16) 1.1222(15) 0.1082(8) 0.031(3) Uani 1 1 d . . .
C31 C -0.057(2) 1.179(2) 0.0608(10) 0.061(2) Uani 1 1 d . . .
C32 C -0.146(2) 1.110(2) 0.0407(10) 0.061(2) Uani 1 1 d . . .
H32 H -0.1402 1.0226 0.0591 0.073 Uiso 1 1 calc R . .
C33 C -0.245(2) 1.167(2) -0.0065(10) 0.061(2) Uani 1 1 d . . .
H33 H -0.3015 1.1178 -0.0240 0.073 Uiso 1 1 calc R . .
C34 C -0.259(2) 1.294(2) -0.0270(10) 0.061(2) Uani 1 1 d . . .
H34 H -0.3286 1.3337 -0.0583 0.073 Uiso 1 1 calc R . .
C35 C -0.178(2) 1.370(2) -0.0055(10) 0.061(2) Uani 1 1 d . . .
H35 H -0.1929 1.4599 -0.0199 0.073 Uiso 1 1 calc R . .
C36 C -0.074(2) 1.309(2) 0.0382(10) 0.061(2) Uani 1 1 d . . .
H36 H -0.0135 1.3575 0.0530 0.073 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
Ir1 N1 1.925(11) . ?
Ir1 C13 2.192(11) . ?
Ir1 C1 2.194(12) . ?
Ir1 C10 2.222(13) . ?
Ir1 C14 2.233(12) . ?
Ir1 C12 2.240(13) . ?
Ir1 C11 2.247(14) . ?
Ir1 Lu1 3.2063(9) . ?
Lu1 O1 2.077(9) . ?
Lu1 N1 2.181(11) . ?
Lu1 N2 2.410(12) . ?
Lu1 C21 2.604(14) . ?
Lu1 C23 2.617(14) . ?
Lu1 C20 2.628(14) . ?
Lu1 C24 2.634(14) . ?
Lu1 C22 2.646(13) . ?
Lu1 C1 2.661(12) . ?
N1 C6 1.510(17) . ?
N2 C30 1.146(18) . ?
O1 C4 1.349(16) . ?
Si1 C2 1.864(17) . ?
Si1 C1 1.876(13) . ?
Si1 C4 1.879(14) . ?
Si1 C3 1.885(15) . ?
C4 C5 1.310(19) . ?
C6 C8 1.516(19) . ?
C6 C9 1.53(2) . ?
C6 C7 1.535(19) . ?
C10 C14 1.40(2) . ?
C10 C11 1.437(19) . ?
C10 C15 1.54(2) . ?
C11 C12 1.404(19) . ?
C11 C16 1.48(2) . ?
C12 C13 1.411(19) . ?
C12 C17 1.501(19) . ?
C13 C14 1.439(17) . ?
C13 C18 1.48(2) . ?
C14 C19 1.486(18) . ?
C20 C21 1.414(19) . ?
C20 C24 1.43(2) . ?
C20 C25 1.49(2) . ?
C21 C22 1.44(2) . ?
C21 C26 1.49(2) . ?
C22 C23 1.44(2) . ?
C22 C27 1.47(2) . ?
C23 C24 1.38(2) . ?
C23 C28 1.49(2) . ?
C24 C29 1.54(2) . ?
C30 C31 1.43(2) . ?
C31 C32 1.37(3) . ?
C31 C36 1.38(3) . ?
C32 C33 1.39(2) . ?
C33 C34 1.34(3) . ?
C34 C35 1.37(3) . ?
C35 C36 1.38(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ir1 C13 128.1(5) . . ?
N1 Ir1 C1 92.0(4) . . ?
C13 Ir1 C1 129.0(5) . . ?
N1 Ir1 C10 160.5(5) . . ?
C13 Ir1 C10 61.6(5) . . ?
C1 Ir1 C10 91.5(5) . . ?
N1 Ir1 C14 161.4(5) . . ?
C13 Ir1 C14 38.0(5) . . ?
C1 Ir1 C14 94.3(5) . . ?
C10 Ir1 C14 36.7(5) . . ?
N1 Ir1 C12 114.4(5) . . ?
C13 Ir1 C12 37.1(5) . . ?
C1 Ir1 C12 152.9(5) . . ?
C10 Ir1 C12 61.6(5) . . ?
C14 Ir1 C12 62.7(5) . . ?
N1 Ir1 C11 127.3(5) . . ?
C13 Ir1 C11 61.7(5) . . ?
C1 Ir1 C11 121.7(5) . . ?
C10 Ir1 C11 37.5(5) . . ?
C14 Ir1 C11 62.6(5) . . ?
C12 Ir1 C11 36.5(5) . . ?
N1 Ir1 Lu1 41.6(3) . . ?
C13 Ir1 Lu1 136.0(4) . . ?
C1 Ir1 Lu1 55.3(3) . . ?
C10 Ir1 Lu1 146.7(4) . . ?
C14 Ir1 Lu1 133.2(4) . . ?
C12 Ir1 Lu1 151.4(3) . . ?
C11 Ir1 Lu1 161.5(4) . . ?
O1 Lu1 N1 113.5(4) . . ?
O1 Lu1 N2 77.2(4) . . ?
N1 Lu1 N2 98.8(4) . . ?
O1 Lu1 C21 120.3(4) . . ?
N1 Lu1 C21 114.9(4) . . ?
N2 Lu1 C21 125.7(4) . . ?
O1 Lu1 C23 128.4(4) . . ?
N1 Lu1 C23 113.5(4) . . ?
N2 Lu1 C23 75.9(5) . . ?
C21 Lu1 C23 52.5(4) . . ?
O1 Lu1 C20 95.2(4) . . ?
N1 Lu1 C20 146.2(4) . . ?
N2 Lu1 C20 104.9(5) . . ?
C21 Lu1 C20 31.4(4) . . ?
C23 Lu1 C20 51.9(4) . . ?
O1 Lu1 C24 100.1(4) . . ?
N1 Lu1 C24 144.0(5) . . ?
N2 Lu1 C24 75.6(5) . . ?
C21 Lu1 C24 51.9(4) . . ?
C23 Lu1 C24 30.5(5) . . ?
C20 Lu1 C24 31.6(5) . . ?
O1 Lu1 C22 147.0(4) . . ?
N1 Lu1 C22 98.7(4) . . ?
N2 Lu1 C22 105.8(5) . . ?
C21 Lu1 C22 31.8(4) . . ?
C23 Lu1 C22 31.7(4) . . ?
C20 Lu1 C22 51.9(4) . . ?
C24 Lu1 C22 51.3(4) . . ?
O1 Lu1 C1 78.4(4) . . ?
N1 Lu1 C1 74.9(4) . . ?
N2 Lu1 C1 149.7(4) . . ?
C21 Lu1 C1 82.5(4) . . ?
C23 Lu1 C1 134.1(4) . . ?
C20 Lu1 C1 95.0(4) . . ?
C24 Lu1 C1 126.6(4) . . ?
C22 Lu1 C1 104.5(4) . . ?
O1 Lu1 Ir1 110.0(3) . . ?
N1 Lu1 Ir1 35.9(3) . . ?
N2 Lu1 Ir1 134.2(3) . . ?
C21 Lu1 Ir1 90.7(3) . . ?
C23 Lu1 Ir1 120.4(3) . . ?
C20 Lu1 Ir1 118.7(3) . . ?
C24 Lu1 Ir1 140.9(3) . . ?
C22 Lu1 Ir1 91.6(3) . . ?
C1 Lu1 Ir1 42.7(3) . . ?
C6 N1 Ir1 121.7(8) . . ?
C6 N1 Lu1 134.0(8) . . ?
Ir1 N1 Lu1 102.5(5) . . ?
C30 N2 Lu1 176.1(13) . . ?
C4 O1 Lu1 133.7(8) . . ?
C2 Si1 C1 112.0(7) . . ?
C2 Si1 C4 110.1(6) . . ?
C1 Si1 C4 104.3(6) . . ?
C2 Si1 C3 107.7(8) . . ?
C1 Si1 C3 112.9(6) . . ?
C4 Si1 C3 109.9(7) . . ?
Si1 C1 Ir1 120.3(6) . . ?
Si1 C1 Lu1 101.3(5) . . ?
Ir1 C1 Lu1 82.1(4) . . ?
C5 C4 O1 124.8(14) . . ?
C5 C4 Si1 123.5(12) . . ?
O1 C4 Si1 111.7(9) . . ?
N1 C6 C8 109.6(11) . . ?
N1 C6 C9 110.6(12) . . ?
C8 C6 C9 108.2(12) . . ?
N1 C6 C7 109.6(11) . . ?
C8 C6 C7 106.8(12) . . ?
C9 C6 C7 112.0(13) . . ?
C14 C10 C11 110.0(13) . . ?
C14 C10 C15 125.3(13) . . ?
C11 C10 C15 124.3(14) . . ?
C14 C10 Ir1 72.1(8) . . ?
C11 C10 Ir1 72.2(8) . . ?
C15 C10 Ir1 127.9(9) . . ?
C12 C11 C10 107.1(13) . . ?
C12 C11 C16 128.3(14) . . ?
C10 C11 C16 124.5(14) . . ?
C12 C11 Ir1 71.5(8) . . ?
C10 C11 Ir1 70.3(8) . . ?
C16 C11 Ir1 126.5(10) . . ?
C11 C12 C13 108.0(12) . . ?
C11 C12 C17 125.2(14) . . ?
C13 C12 C17 123.9(13) . . ?
C11 C12 Ir1 72.0(8) . . ?
C13 C12 Ir1 69.6(7) . . ?
C17 C12 Ir1 139.2(10) . . ?
C12 C13 C14 109.5(12) . . ?
C12 C13 C18 126.4(13) . . ?
C14 C13 C18 123.7(13) . . ?
C12 C13 Ir1 73.3(7) . . ?
C14 C13 Ir1 72.5(7) . . ?
C18 C13 Ir1 126.3(10) . . ?
C10 C14 C13 105.4(12) . . ?
C10 C14 C19 126.0(13) . . ?
C13 C14 C19 128.2(13) . . ?
C10 C14 Ir1 71.2(7) . . ?
C13 C14 Ir1 69.5(6) . . ?
C19 C14 Ir1 129.3(9) . . ?
C21 C20 C24 107.1(12) . . ?
C21 C20 C25 125.1(14) . . ?
C24 C20 C25 127.8(14) . . ?
C21 C20 Lu1 73.4(8) . . ?
C24 C20 Lu1 74.4(8) . . ?
C25 C20 Lu1 118.8(10) . . ?
C20 C21 C22 108.1(12) . . ?
C20 C21 C26 126.8(14) . . ?
C22 C21 C26 124.2(14) . . ?
C20 C21 Lu1 75.2(8) . . ?
C22 C21 Lu1 75.7(8) . . ?
C26 C21 Lu1 123.6(10) . . ?
C23 C22 C21 106.9(12) . . ?
C23 C22 C27 127.0(14) . . ?
C21 C22 C27 126.0(14) . . ?
C23 C22 Lu1 73.0(8) . . ?
C21 C22 Lu1 72.5(8) . . ?
C27 C22 Lu1 122.5(10) . . ?
C24 C23 C22 108.4(13) . . ?
C24 C23 C28 128.0(14) . . ?
C22 C23 C28 122.4(14) . . ?
C24 C23 Lu1 75.4(9) . . ?
C22 C23 Lu1 75.3(8) . . ?
C28 C23 Lu1 125.3(11) . . ?
C23 C24 C20 109.3(13) . . ?
C23 C24 C29 126.5(14) . . ?
C20 C24 C29 124.0(14) . . ?
C23 C24 Lu1 74.1(8) . . ?
C20 C24 Lu1 74.0(8) . . ?
C29 C24 Lu1 122.9(10) . . ?
N2 C30 C31 177.7(18) . . ?
C32 C31 C36 119.5(17) . . ?
C32 C31 C30 121.6(19) . . ?
C36 C31 C30 118.8(19) . . ?
C31 C32 C33 120(2) . . ?
C34 C33 C32 118(2) . . ?
C33 C34 C35 123.8(18) . . ?
C34 C35 C36 117(2) . . ?
C35 C36 C31 121(2) . . ?

_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.968
_refine_diff_density_max         5.223
_refine_diff_density_min         -4.148
_refine_diff_density_rms         0.349
