data_rob716_mo _audit_creation_date 2014-09-23 _audit_creation_method ; Olex2 1.2 (compiled 2014.06.18 svn.r2945 for OlexSys, GUI svn.r4846) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C16 H26 Ir N3, 2(F6 Sb)' _chemical_formula_sum 'C16 H26 F12 Ir N3 Sb2' _chemical_formula_weight 924.10 _chemical_melting_point ? _chemical_oxdiff_formula 'C64 H104 F48 Ir4 N12 Sb8' 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.7369(2) _cell_length_b 17.1539(5) _cell_length_c 19.0464(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.724(3) _cell_angle_gamma 90.00 _cell_volume 2504.86(12) _cell_formula_units_Z 4 _cell_measurement_reflns_used 14850 _cell_measurement_temperature 119.99(13) _cell_measurement_theta_max 31.0580 _cell_measurement_theta_min 3.9640 _exptl_absorpt_coefficient_mu 7.540 _exptl_absorpt_correction_T_max 0.743 _exptl_absorpt_correction_T_min 0.288 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.450 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1720 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_unetI/netI 0.0402 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 31514 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_theta_min 3.00 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 119.99(13) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.3095 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -15.00 22.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 12.9509 -19.0000 -180.0000 37 #__ type_ start__ end____ width___ exp.time_ 2 omega -28.00 29.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 12.9509 -37.0000 0.0000 57 #__ type_ start__ end____ width___ exp.time_ 3 omega -6.00 55.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 12.9509 37.0000 -90.0000 61 #__ type_ start__ end____ width___ exp.time_ 4 omega -30.00 54.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -13.7322 37.0000 -180.0000 84 #__ type_ start__ end____ width___ exp.time_ 5 omega -32.00 11.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -13.7322 -57.0000 0.0000 43 #__ type_ start__ end____ width___ exp.time_ 6 omega -45.00 -18.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -13.7322 -37.0000 90.0000 27 #__ type_ start__ end____ width___ exp.time_ 7 omega -60.00 33.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 12.9509 -32.0000 -83.0000 93 #__ type_ start__ end____ width___ exp.time_ 8 omega -82.00 -25.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -13.7322 -57.0000 -120.0000 57 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0472799000 _diffrn_orient_matrix_UB_12 -0.0287236000 _diffrn_orient_matrix_UB_13 -0.0162437000 _diffrn_orient_matrix_UB_21 0.0721092000 _diffrn_orient_matrix_UB_22 0.0257686000 _diffrn_orient_matrix_UB_23 0.0013705000 _diffrn_orient_matrix_UB_31 0.0336867000 _diffrn_orient_matrix_UB_32 -0.0148025000 _diffrn_orient_matrix_UB_33 0.0338623000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'SuperNova (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 5737 _reflns_number_total 6212 _reflns_odcompleteness_completeness 99.83 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 28.22 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _refine_diff_density_max 1.223 _refine_diff_density_min -1.169 _refine_diff_density_rms 0.155 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 313 _refine_ls_number_reflns 6212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0273 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0213P)^2^+1.4740P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.0604 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups, All N(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: N1(H1A,H1B), C1(H1C,H1D), C2(H2A,H2B), C3(H3A,H3B) 2.b Idealised Me refined as rotating group: C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B, H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_refinement_flags_posn Ir1 Ir 0.541055(18) 0.270360(8) 0.106211(7) 0.01466(5) Uani 1 d . . . N1 N 0.6790(4) 0.1957(2) 0.18382(16) 0.0217(7) Uani 1 d . . . H1A H 0.6175 0.1925 0.2206 0.026 Uiso 1 calc . . R H1B H 0.6813 0.1477 0.1650 0.026 Uiso 1 calc . . R C1 C 0.8602(5) 0.2176(2) 0.2119(2) 0.0218(8) Uani 1 d . . . H1C H 0.9100 0.1780 0.2449 0.026 Uiso 1 calc . . R H1D H 0.8592 0.2665 0.2376 0.026 Uiso 1 calc . . R N2 N 0.4081(4) 0.31053(19) 0.18742(15) 0.0192(7) Uani 1 d . . . C2 C 0.9743(5) 0.2266(2) 0.1528(2) 0.0252(9) Uani 1 d . . . H2A H 0.9500 0.1834 0.1201 0.030 Uiso 1 calc . . R H2B H 1.0955 0.2225 0.1735 0.030 Uiso 1 calc . . R N3 N 0.3750(4) 0.17554(19) 0.09189(15) 0.0187(7) Uani 1 d . . . C3 C 0.9507(5) 0.3029(3) 0.1105(2) 0.0253(9) Uani 1 d . . . H3A H 0.9830 0.3458 0.1429 0.030 Uiso 1 calc . . R H3B H 1.0320 0.3027 0.0759 0.030 Uiso 1 calc . . R C4 C 0.7727(5) 0.3186(2) 0.07263(18) 0.0196(8) Uani 1 d . . . C5 C 0.6576(5) 0.3804(2) 0.08667(19) 0.0197(8) Uani 1 d . . . C6 C 0.4948(5) 0.3719(2) 0.03808(19) 0.0217(8) Uani 1 d . . . C7 C 0.5143(5) 0.3056(2) -0.00472(18) 0.0208(8) Uani 1 d . . . C8 C 0.6814(5) 0.2696(2) 0.01691(19) 0.0197(8) Uani 1 d . . . C9 C 0.6972(6) 0.4458(2) 0.1388(2) 0.0251(9) Uani 1 d . . . H9A H 0.5904 0.4650 0.1529 0.038 Uiso 1 calc . . GR H9B H 0.7547 0.4872 0.1171 0.038 Uiso 1 calc . . GR H9C H 0.7718 0.4272 0.1797 0.038 Uiso 1 calc . . GR C10 C 0.3420(5) 0.4261(3) 0.0336(2) 0.0286(9) Uani 1 d . . . H10A H 0.2416 0.4014 0.0078 0.043 Uiso 1 calc . . GR H10B H 0.3680 0.4730 0.0096 0.043 Uiso 1 calc . . GR H10C H 0.3185 0.4387 0.0805 0.043 Uiso 1 calc . . GR C11 C 0.3795(6) 0.2759(3) -0.0629(2) 0.0307(10) Uani 1 d . . . H11A H 0.3966 0.2211 -0.0695 0.046 Uiso 1 calc . . GR H11B H 0.3908 0.3030 -0.1062 0.046 Uiso 1 calc . . GR H11C H 0.2651 0.2846 -0.0503 0.046 Uiso 1 calc . . GR C12 C 0.7573(6) 0.2032(3) -0.0197(2) 0.0268(9) Uani 1 d . . . H12A H 0.8522 0.1808 0.0114 0.040 Uiso 1 calc . . GR H12B H 0.7993 0.2219 -0.0618 0.040 Uiso 1 calc . . GR H12C H 0.6692 0.1644 -0.0322 0.040 Uiso 1 calc . . GR C13 C 0.3407(5) 0.3408(2) 0.22931(19) 0.0190(8) Uani 1 d . . . C14 C 0.2515(5) 0.3798(2) 0.2817(2) 0.0237(8) Uani 1 d . . . H14A H 0.2314 0.4333 0.2683 0.036 Uiso 1 calc . . GR H14B H 0.3222 0.3774 0.3271 0.036 Uiso 1 calc . . GR H14C H 0.1419 0.3545 0.2844 0.036 Uiso 1 calc . . GR C15 C 0.3002(5) 0.1187(2) 0.08503(18) 0.0182(8) Uani 1 d . . . C16 C 0.2035(5) 0.0459(2) 0.0773(2) 0.0234(8) Uani 1 d . . . H16A H 0.1029 0.0521 0.0423 0.035 Uiso 1 calc . . GR H16B H 0.1669 0.0319 0.1218 0.035 Uiso 1 calc . . GR H16C H 0.2768 0.0055 0.0626 0.035 Uiso 1 calc . . GR Sb1 Sb 0.76142(3) 0.459474(15) 0.365222(12) 0.01918(7) Uani 1 d . . . F1 F 0.9264(4) 0.51226(18) 0.31972(14) 0.0444(7) Uani 1 d . . . F2 F 0.9361(3) 0.42947(16) 0.43775(13) 0.0360(6) Uani 1 d . . . F3 F 0.5965(3) 0.40881(16) 0.41281(12) 0.0346(6) Uani 1 d . . . F4 F 0.5823(3) 0.49031(17) 0.29472(12) 0.0370(6) Uani 1 d . . . F5 F 0.7970(4) 0.36930(16) 0.31484(13) 0.0449(7) Uani 1 d . . . F6 F 0.7293(4) 0.55190(15) 0.41448(13) 0.0383(6) Uani 1 d . . . Sb2 Sb 0.83701(4) 0.390449(15) -0.163062(12) 0.02140(7) Uani 1 d . . . F7 F 1.0586(4) 0.36709(19) -0.18655(13) 0.0441(7) Uani 1 d . . . F8 F 0.9214(4) 0.37452(17) -0.06769(11) 0.0393(7) Uani 1 d . . . F9 F 0.6152(3) 0.41170(17) -0.13911(15) 0.0427(7) Uani 1 d . . . F10 F 0.7564(4) 0.40504(17) -0.25926(12) 0.0409(7) Uani 1 d . . . F11 F 0.8928(4) 0.49618(15) -0.15503(14) 0.0381(6) Uani 1 d . . . F12 F 0.7725(5) 0.28558(16) -0.17352(14) 0.0481(8) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01568(8) 0.01499(8) 0.01352(8) 0.00047(5) 0.00269(5) -0.00297(5) N1 0.0228(17) 0.0203(18) 0.0223(16) 0.0033(13) 0.0044(13) 0.0007(14) C1 0.0211(19) 0.020(2) 0.0233(19) 0.0018(16) -0.0001(15) 0.0029(16) N2 0.0212(16) 0.0193(17) 0.0169(15) 0.0006(13) 0.0015(13) -0.0016(14) C2 0.0182(19) 0.023(2) 0.034(2) -0.0022(17) 0.0029(17) -0.0002(17) N3 0.0188(16) 0.0206(17) 0.0169(14) -0.0011(13) 0.0033(12) -0.0043(14) C3 0.0189(19) 0.027(2) 0.031(2) -0.0019(17) 0.0073(16) -0.0080(17) C4 0.0223(19) 0.0190(19) 0.0186(17) -0.0008(15) 0.0066(15) -0.0095(16) C5 0.024(2) 0.0156(19) 0.0199(17) 0.0041(15) 0.0058(15) -0.0054(16) C6 0.026(2) 0.022(2) 0.0172(17) 0.0033(15) 0.0012(15) -0.0077(17) C7 0.026(2) 0.022(2) 0.0144(16) 0.0043(15) 0.0026(15) -0.0081(17) C8 0.025(2) 0.019(2) 0.0171(17) 0.0013(14) 0.0077(15) -0.0090(16) C9 0.033(2) 0.019(2) 0.0222(19) -0.0026(16) -0.0029(17) -0.0070(18) C10 0.025(2) 0.024(2) 0.034(2) 0.0081(18) -0.0037(18) 0.0003(18) C11 0.043(3) 0.028(2) 0.0189(19) 0.0001(16) -0.0068(18) -0.010(2) C12 0.036(2) 0.025(2) 0.0209(19) -0.0034(17) 0.0120(17) -0.0028(19) C13 0.0190(18) 0.0162(19) 0.0214(18) 0.0011(15) 0.0010(15) -0.0030(16) C14 0.031(2) 0.017(2) 0.0240(19) 0.0010(16) 0.0078(16) 0.0032(17) C15 0.0173(18) 0.021(2) 0.0168(17) 0.0012(15) 0.0025(14) -0.0004(16) C16 0.024(2) 0.021(2) 0.0256(19) -0.0014(16) 0.0055(16) -0.0085(17) Sb1 0.02228(13) 0.01648(13) 0.01898(12) 0.00046(10) 0.00356(10) 0.00258(10) F1 0.0384(15) 0.0496(19) 0.0480(15) 0.0167(14) 0.0160(13) -0.0083(14) F2 0.0321(14) 0.0372(16) 0.0353(13) 0.0082(12) -0.0078(11) 0.0068(12) F3 0.0342(14) 0.0408(16) 0.0294(12) 0.0028(11) 0.0066(11) -0.0118(12) F4 0.0352(14) 0.0478(17) 0.0254(12) 0.0061(12) -0.0054(11) 0.0066(13) F5 0.073(2) 0.0296(15) 0.0329(13) -0.0079(12) 0.0119(13) 0.0157(15) F6 0.0520(17) 0.0223(14) 0.0385(14) -0.0086(11) -0.0008(12) 0.0087(13) Sb2 0.02813(15) 0.01793(14) 0.01826(12) 0.00054(10) 0.00361(10) -0.00080(11) F7 0.0397(15) 0.058(2) 0.0378(14) 0.0005(13) 0.0147(12) 0.0194(15) F8 0.0492(17) 0.0505(18) 0.0171(11) 0.0022(11) 0.0007(11) -0.0045(14) F9 0.0289(14) 0.0429(17) 0.0590(17) -0.0032(14) 0.0161(13) -0.0057(13) F10 0.0498(17) 0.0474(18) 0.0230(12) 0.0099(11) -0.0046(11) -0.0102(14) F11 0.0440(16) 0.0214(14) 0.0513(16) -0.0033(12) 0.0157(13) -0.0105(12) F12 0.087(2) 0.0190(14) 0.0384(15) -0.0031(11) 0.0086(15) -0.0062(15) _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 2.131(3) . ? Ir1 N2 2.086(3) . ? Ir1 N3 2.068(3) . ? Ir1 C4 2.148(4) . ? Ir1 C5 2.146(4) . ? Ir1 C6 2.172(4) . ? Ir1 C7 2.180(3) . ? Ir1 C8 2.138(4) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N1 C1 1.481(5) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C1 C2 1.528(5) . ? N2 C13 1.135(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 C3 1.535(6) . ? N3 C15 1.132(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 C4 1.491(6) . ? C4 C5 1.432(6) . ? C4 C8 1.460(5) . ? C5 C6 1.467(5) . ? C5 C9 1.503(5) . ? C6 C7 1.419(6) . ? C6 C10 1.498(6) . ? C7 C8 1.442(6) . ? C7 C11 1.505(5) . ? C8 C12 1.495(5) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.451(5) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.453(5) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? Sb1 F1 1.870(3) . ? Sb1 F2 1.870(2) . ? Sb1 F3 1.875(2) . ? Sb1 F4 1.872(2) . ? Sb1 F5 1.860(3) . ? Sb1 F6 1.876(2) . ? Sb2 F7 1.873(3) . ? Sb2 F8 1.866(2) . ? Sb2 F9 1.870(3) . ? Sb2 F10 1.871(2) . ? Sb2 F11 1.866(3) . ? Sb2 F12 1.870(3) . ? 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 C4 94.48(13) . . ? N1 Ir1 C5 117.78(14) . . ? N1 Ir1 C6 157.39(14) . . ? N1 Ir1 C7 144.32(14) . . ? N1 Ir1 C8 106.72(14) . . ? N2 Ir1 N1 86.28(12) . . ? N2 Ir1 C4 127.41(13) . . ? N2 Ir1 C5 95.67(13) . . ? N2 Ir1 C6 96.90(14) . . ? N2 Ir1 C7 129.40(14) . . ? N2 Ir1 C8 161.05(13) . . ? N3 Ir1 N1 82.13(12) . . ? N3 Ir1 N2 89.89(12) . . ? N3 Ir1 C4 142.41(13) . . ? N3 Ir1 C5 159.57(13) . . ? N3 Ir1 C6 120.14(13) . . ? N3 Ir1 C7 96.53(13) . . ? N3 Ir1 C8 105.26(13) . . ? C4 Ir1 C6 65.80(15) . . ? C4 Ir1 C7 65.11(14) . . ? C5 Ir1 C4 38.95(15) . . ? C5 Ir1 C6 39.71(14) . . ? C5 Ir1 C7 64.89(14) . . ? C6 Ir1 C7 38.04(15) . . ? C8 Ir1 C4 39.84(14) . . ? C8 Ir1 C5 66.24(14) . . ? C8 Ir1 C6 65.80(15) . . ? C8 Ir1 C7 39.01(15) . . ? Ir1 N1 H1A 108.0 . . ? Ir1 N1 H1B 108.0 . . ? H1A N1 H1B 107.2 . . ? C1 N1 Ir1 117.3(2) . . ? C1 N1 H1A 108.0 . . ? C1 N1 H1B 108.0 . . ? N1 C1 H1C 109.2 . . ? N1 C1 H1D 109.2 . . ? N1 C1 C2 111.8(3) . . ? H1C C1 H1D 107.9 . . ? C2 C1 H1C 109.2 . . ? C2 C1 H1D 109.2 . . ? C13 N2 Ir1 172.1(3) . . ? C1 C2 H2A 108.4 . . ? C1 C2 H2B 108.4 . . ? C1 C2 C3 115.6(3) . . ? H2A C2 H2B 107.4 . . ? C3 C2 H2A 108.4 . . ? C3 C2 H2B 108.4 . . ? C15 N3 Ir1 172.4(3) . . ? C2 C3 H3A 108.2 . . ? C2 C3 H3B 108.2 . . ? H3A C3 H3B 107.3 . . ? C4 C3 C2 116.4(3) . . ? C4 C3 H3A 108.2 . . ? C4 C3 H3B 108.2 . . ? C3 C4 Ir1 122.6(3) . . ? C5 C4 Ir1 70.4(2) . . ? C5 C4 C3 126.9(3) . . ? C5 C4 C8 108.1(3) . . ? C8 C4 Ir1 69.7(2) . . ? C8 C4 C3 124.9(4) . . ? C4 C5 Ir1 70.6(2) . . ? C4 C5 C6 108.1(3) . . ? C4 C5 C9 126.8(3) . . ? C6 C5 Ir1 71.1(2) . . ? C6 C5 C9 124.9(4) . . ? C9 C5 Ir1 126.6(3) . . ? C5 C6 Ir1 69.2(2) . . ? C5 C6 C10 125.3(4) . . ? C7 C6 Ir1 71.3(2) . . ? C7 C6 C5 107.1(4) . . ? C7 C6 C10 127.5(4) . . ? C10 C6 Ir1 126.7(3) . . ? C6 C7 Ir1 70.7(2) . . ? C6 C7 C8 109.8(3) . . ? C6 C7 C11 125.3(4) . . ? C8 C7 Ir1 68.9(2) . . ? C8 C7 C11 124.8(4) . . ? C11 C7 Ir1 125.9(3) . . ? C4 C8 Ir1 70.5(2) . . ? C4 C8 C12 126.5(4) . . ? C7 C8 Ir1 72.1(2) . . ? C7 C8 C4 106.8(3) . . ? C7 C8 C12 125.9(3) . . ? C12 C8 Ir1 130.5(3) . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 H10A 109.5 . . ? C6 C10 H10B 109.5 . . ? C6 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 C14 178.8(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 C16 179.2(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? F1 Sb1 F2 90.29(12) . . ? F1 Sb1 F3 178.36(13) . . ? F1 Sb1 F4 90.94(12) . . ? F1 Sb1 F6 88.11(13) . . ? F2 Sb1 F3 89.23(11) . . ? F2 Sb1 F4 178.26(11) . . ? F2 Sb1 F6 89.67(12) . . ? F3 Sb1 F6 90.32(12) . . ? F4 Sb1 F3 89.52(11) . . ? F4 Sb1 F6 89.14(12) . . ? F5 Sb1 F1 90.34(14) . . ? F5 Sb1 F2 90.56(12) . . ? F5 Sb1 F3 91.23(13) . . ? F5 Sb1 F4 90.66(12) . . ? F5 Sb1 F6 178.43(13) . . ? F8 Sb2 F7 89.40(12) . . ? F8 Sb2 F9 90.20(12) . . ? F8 Sb2 F10 178.72(13) . . ? F8 Sb2 F12 90.93(13) . . ? F9 Sb2 F7 178.86(13) . . ? F9 Sb2 F10 90.97(13) . . ? F9 Sb2 F12 88.45(14) . . ? F10 Sb2 F7 89.42(12) . . ? F11 Sb2 F7 91.06(13) . . ? F11 Sb2 F8 90.90(12) . . ? F11 Sb2 F9 90.01(12) . . ? F11 Sb2 F10 89.61(12) . . ? F11 Sb2 F12 177.61(13) . . ? F12 Sb2 F7 90.49(15) . . ? F12 Sb2 F10 88.59(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ir1 N1 C1 C2 -56.4(4) . . . . ? Ir1 N2 C13 C14 78(21) . . . . ? Ir1 N3 C15 C16 106(31) . . . . ? Ir1 C4 C5 C6 -61.5(2) . . . . ? Ir1 C4 C5 C9 121.7(4) . . . . ? Ir1 C4 C8 C7 63.4(2) . . . . ? Ir1 C4 C8 C12 -126.5(4) . . . . ? Ir1 C5 C6 C7 -61.6(3) . . . . ? Ir1 C5 C6 C10 120.9(4) . . . . ? Ir1 C6 C7 C8 -57.8(2) . . . . ? Ir1 C6 C7 C11 120.8(4) . . . . ? Ir1 C7 C8 C4 -62.3(2) . . . . ? Ir1 C7 C8 C12 127.4(4) . . . . ? N1 Ir1 N2 C13 129(2) . . . . ? N1 Ir1 N3 C15 -39(2) . . . . ? N1 Ir1 C4 C3 -8.3(3) . . . . ? N1 Ir1 C4 C5 -130.3(2) . . . . ? N1 Ir1 C4 C8 110.9(2) . . . . ? N1 Ir1 C5 C4 59.3(2) . . . . ? N1 Ir1 C5 C6 177.2(2) . . . . ? N1 Ir1 C5 C9 -62.8(4) . . . . ? N1 Ir1 C6 C5 -6.4(5) . . . . ? N1 Ir1 C6 C7 111.1(4) . . . . ? N1 Ir1 C6 C10 -125.6(4) . . . . ? N1 Ir1 C7 C6 -142.0(2) . . . . ? N1 Ir1 C7 C8 -20.7(3) . . . . ? N1 Ir1 C7 C11 97.8(4) . . . . ? N1 Ir1 C8 C4 -76.5(2) . . . . ? N1 Ir1 C8 C7 167.6(2) . . . . ? N1 Ir1 C8 C12 45.3(4) . . . . ? N1 C1 C2 C3 78.1(4) . . . . ? C1 C2 C3 C4 -59.9(5) . . . . ? N2 Ir1 N1 C1 -104.1(3) . . . . ? N2 Ir1 N3 C15 -125(2) . . . . ? N2 Ir1 C4 C3 80.4(4) . . . . ? N2 Ir1 C4 C5 -41.5(3) . . . . ? N2 Ir1 C4 C8 -160.4(2) . . . . ? N2 Ir1 C5 C4 148.0(2) . . . . ? N2 Ir1 C5 C6 -94.0(2) . . . . ? N2 Ir1 C5 C9 26.0(4) . . . . ? N2 Ir1 C6 C5 90.6(2) . . . . ? N2 Ir1 C6 C7 -152.0(2) . . . . ? N2 Ir1 C6 C10 -28.7(3) . . . . ? N2 Ir1 C7 C6 37.1(3) . . . . ? N2 Ir1 C7 C8 158.5(2) . . . . ? N2 Ir1 C7 C11 -83.0(4) . . . . ? N2 Ir1 C8 C4 55.2(5) . . . . ? N2 Ir1 C8 C7 -60.6(5) . . . . ? N2 Ir1 C8 C12 177.1(3) . . . . ? C2 C3 C4 Ir1 25.6(5) . . . . ? C2 C3 C4 C5 114.7(4) . . . . ? C2 C3 C4 C8 -61.2(5) . . . . ? N3 Ir1 N1 C1 165.5(3) . . . . ? N3 Ir1 N2 C13 -149(2) . . . . ? N3 Ir1 C4 C3 -91.3(4) . . . . ? N3 Ir1 C4 C5 146.8(2) . . . . ? N3 Ir1 C4 C8 28.0(3) . . . . ? N3 Ir1 C5 C4 -106.8(4) . . . . ? N3 Ir1 C5 C6 11.1(5) . . . . ? N3 Ir1 C5 C9 131.1(4) . . . . ? N3 Ir1 C6 C5 -175.5(2) . . . . ? N3 Ir1 C6 C7 -58.1(3) . . . . ? N3 Ir1 C6 C10 65.2(4) . . . . ? N3 Ir1 C7 C6 132.4(2) . . . . ? N3 Ir1 C7 C8 -106.2(2) . . . . ? N3 Ir1 C7 C11 12.2(4) . . . . ? N3 Ir1 C8 C4 -162.8(2) . . . . ? N3 Ir1 C8 C7 81.4(2) . . . . ? N3 Ir1 C8 C12 -40.9(4) . . . . ? C3 C4 C5 Ir1 -116.7(4) . . . . ? C3 C4 C5 C6 -178.2(3) . . . . ? C3 C4 C5 C9 5.0(6) . . . . ? C3 C4 C8 Ir1 116.3(4) . . . . ? C3 C4 C8 C7 179.7(3) . . . . ? C3 C4 C8 C12 -10.2(6) . . . . ? C4 Ir1 N1 C1 23.2(3) . . . . ? C4 Ir1 N2 C13 36(2) . . . . ? C4 Ir1 N3 C15 48(2) . . . . ? C4 Ir1 C5 C6 118.0(3) . . . . ? C4 Ir1 C5 C9 -122.0(4) . . . . ? C4 Ir1 C6 C5 -37.5(2) . . . . ? C4 Ir1 C6 C7 80.0(2) . . . . ? C4 Ir1 C6 C10 -156.7(4) . . . . ? C4 Ir1 C7 C6 -81.9(2) . . . . ? C4 Ir1 C7 C8 39.5(2) . . . . ? C4 Ir1 C7 C11 157.9(4) . . . . ? C4 Ir1 C8 C7 -115.9(3) . . . . ? C4 Ir1 C8 C12 121.9(5) . . . . ? C4 C5 C6 Ir1 61.2(2) . . . . ? C4 C5 C6 C7 -0.3(4) . . . . ? C4 C5 C6 C10 -177.9(3) . . . . ? C5 Ir1 N1 C1 -9.6(3) . . . . ? C5 Ir1 N2 C13 11(2) . . . . ? C5 Ir1 N3 C15 128(2) . . . . ? C5 Ir1 C4 C3 122.0(4) . . . . ? C5 Ir1 C4 C8 -118.8(3) . . . . ? C5 Ir1 C6 C7 117.4(3) . . . . ? C5 Ir1 C6 C10 -119.2(4) . . . . ? C5 Ir1 C7 C6 -38.8(2) . . . . ? C5 Ir1 C7 C8 82.6(2) . . . . ? C5 Ir1 C7 C11 -158.9(4) . . . . ? C5 Ir1 C8 C4 37.0(2) . . . . ? C5 Ir1 C8 C7 -78.9(2) . . . . ? C5 Ir1 C8 C12 158.9(4) . . . . ? C5 C4 C8 Ir1 -60.3(2) . . . . ? C5 C4 C8 C7 3.2(4) . . . . ? C5 C4 C8 C12 173.3(3) . . . . ? C5 C6 C7 Ir1 60.2(2) . . . . ? C5 C6 C7 C8 2.4(4) . . . . ? C5 C6 C7 C11 -179.0(3) . . . . ? C6 Ir1 N1 C1 -5.0(5) . . . . ? C6 Ir1 N2 C13 -29(2) . . . . ? C6 Ir1 N3 C15 137(2) . . . . ? C6 Ir1 C4 C3 160.2(4) . . . . ? C6 Ir1 C4 C5 38.2(2) . . . . ? C6 Ir1 C4 C8 -80.6(2) . . . . ? C6 Ir1 C5 C4 -118.0(3) . . . . ? C6 Ir1 C5 C9 120.0(4) . . . . ? C6 Ir1 C7 C8 121.4(3) . . . . ? C6 Ir1 C7 C11 -120.1(5) . . . . ? C6 Ir1 C8 C4 80.6(2) . . . . ? C6 Ir1 C8 C7 -35.2(2) . . . . ? C6 Ir1 C8 C12 -157.5(4) . . . . ? C6 C7 C8 Ir1 58.9(3) . . . . ? C6 C7 C8 C4 -3.5(4) . . . . ? C6 C7 C8 C12 -173.7(3) . . . . ? C7 Ir1 N1 C1 75.3(4) . . . . ? C7 Ir1 N2 C13 -51(2) . . . . ? C7 Ir1 N3 C15 105(2) . . . . ? C7 Ir1 C4 C3 -157.9(4) . . . . ? C7 Ir1 C4 C5 80.2(2) . . . . ? C7 Ir1 C4 C8 -38.6(2) . . . . ? C7 Ir1 C5 C4 -80.8(2) . . . . ? C7 Ir1 C5 C6 37.2(2) . . . . ? C7 Ir1 C5 C9 157.2(4) . . . . ? C7 Ir1 C6 C5 -117.4(3) . . . . ? C7 Ir1 C6 C10 123.3(4) . . . . ? C7 Ir1 C8 C4 115.9(3) . . . . ? C7 Ir1 C8 C12 -122.3(5) . . . . ? C8 Ir1 N1 C1 61.9(3) . . . . ? C8 Ir1 N2 C13 -5(2) . . . . ? C8 Ir1 N3 C15 66(2) . . . . ? C8 Ir1 C4 C3 -119.2(4) . . . . ? C8 Ir1 C4 C5 118.8(3) . . . . ? C8 Ir1 C5 C4 -37.8(2) . . . . ? C8 Ir1 C5 C6 80.2(2) . . . . ? C8 Ir1 C5 C9 -159.8(4) . . . . ? C8 Ir1 C6 C5 -81.4(2) . . . . ? C8 Ir1 C6 C7 36.1(2) . . . . ? C8 Ir1 C6 C10 159.4(4) . . . . ? C8 Ir1 C7 C6 -121.4(3) . . . . ? C8 Ir1 C7 C11 118.5(5) . . . . ? C8 C4 C5 Ir1 59.8(2) . . . . ? C8 C4 C5 C6 -1.8(4) . . . . ? C8 C4 C5 C9 -178.5(3) . . . . ? C9 C5 C6 Ir1 -121.9(4) . . . . ? C9 C5 C6 C7 176.5(3) . . . . ? C9 C5 C6 C10 -1.0(6) . . . . ? C10 C6 C7 Ir1 -122.3(4) . . . . ? C10 C6 C7 C8 179.8(4) . . . . ? C10 C6 C7 C11 -1.5(6) . . . . ? C11 C7 C8 Ir1 -119.8(4) . . . . ? C11 C7 C8 C4 177.9(3) . . . . ? C11 C7 C8 C12 7.7(6) . . . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 5 20 -9 0.0484 5.0001 20.0000 -8.9998 -0.1919 0.8636 -0.4324 -9 2 -11 0.0817 -9.0002 1.9995 -10.9995 -0.3043 -0.6125 -0.7053 9 -2 11 0.0817 9.0002 -1.9995 10.9995 0.3043 0.6125 0.7053 3 -22 7 0.0336 3.0001 -21.9995 6.9997 0.6600 -0.3410 0.6637 -5 2 25 0.1738 -5.0000 1.9994 24.9993 -0.6999 -0.2748 0.6485 -1 -15 21 0.1035 -1.0000 -15.0000 20.9993 0.0425 -0.4299 0.8994 6 -20 -7 0.0446 6.0001 -19.9992 -6.9999 0.9718 -0.0923 0.2611 6 -4 -24 0.1272 6.0001 -3.9993 -23.9993 0.7884 0.2967 -0.5513 -9 -15 2 0.0295 -9.0002 -15.0003 2.0001 -0.0272 -1.0328 -0.0134 -3 -5 26 0.1545 -3.0000 -5.0003 25.9992 -0.4205 -0.3095 0.8534 -8 -13 -10 0.0696 -8.0002 -13.0001 -9.9995 0.1576 -0.9256 -0.4157 -9 14 -3 0.0732 -9.0002 13.9992 -2.9997 -0.7789 -0.2924 -0.6120 -1 12 23 0.1610 -1.0000 11.9995 22.9993 -0.7655 0.2686 0.5675 2 23 -5 0.0433 2.0000 22.9997 -4.9999 -0.4849 0.7300 -0.4424 6 21 1 0.0559 6.0001 21.0000 0.9998 -0.3358 0.9752 -0.0749 -3 -23 5 0.0037 -3.0000 -22.9998 4.9999 0.4376 -0.8021 0.4087 3 22 6 0.0770 3.0000 21.9997 5.9997 -0.5875 0.7915 -0.0214 _olex2_submission_special_instructions 'No special instructions were received'