# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_2-XRD _database_code_depnum_ccdc_archive 'CCDC 880791' #TrackingRef 'CrystallographicData.cif' #============================================================================== _audit_creation_date 10-10-21 _audit_creation_method CRYSTALS_ver_14.06 _oxford_structure_analysis_title 102ct09 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 22.8105(2) _cell_length_b 19.0153(2) _cell_length_c 19.9792(2) _cell_angle_alpha 90 _cell_angle_beta 117.1045(4) _cell_angle_gamma 90 _cell_volume 7714.23(13) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 c 1 ' _symmetry_space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z x,-y,z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ir -1.4442 7.9887 27.3049 1.5928 16.7296 8.8655 15.6115 0.4179 5.8338 45.0011 11.4722 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C90 H60 B3 F24 Ir1 N5 # Dc = 1.63 Fooo = 3456.00 Mu = 18.42 M = 1892.11 # Found Formula = C76 H70 B2 F24 Ir1 N5 # Dc = 1.48 FOOO = 3456.00 Mu = 18.34 M = 1723.22 _chemical_formula_sum 'C76 H70 B2 F24 Ir1 N5' _chemical_formula_moiety 'C44 H58 B Ir N5, C32 H12 B F24' _chemical_compound_source . _chemical_formula_weight 1723.22 _cell_measurement_reflns_used 9007 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour clear_intense_yellow _exptl_crystal_size_min 0.180 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_max 0.220 _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3456 _exptl_absorpt_coefficient_mu 1.834 # Sheldrick geometric approximatio 0.71 0.72 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.72 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 66010 _reflns_number_total 17099 _diffrn_reflns_av_R_equivalents 0.051 # Number of reflections without Friedels Law is 17099 # Number of reflections with Friedels Law is 8779 # Theoretical number of reflections is about 8837 _diffrn_reflns_theta_min 5.122 _diffrn_reflns_theta_max 27.473 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.924 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min -29 _reflns_limit_h_max 29 _reflns_limit_k_min 0 _reflns_limit_k_max 24 _reflns_limit_l_min -25 _reflns_limit_l_max 25 _oxford_diffrn_Wilson_B_factor 2.73 _oxford_diffrn_Wilson_scale 63.08 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.96 _refine_diff_density_max 1.19 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 17099 _refine_ls_number_restraints 686 _refine_ls_number_parameters 1058 _oxford_refine_ls_R_factor_ref 0.0423 _refine_ls_wR_factor_ref 0.0866 _refine_ls_goodness_of_fit_ref 0.9206 _refine_ls_shift/su_max 0.0074376 _refine_ls_shift/su_mean 0.0001781 # The values computed from all data _oxford_reflns_number_all 17099 _refine_ls_R_factor_all 0.0423 _refine_ls_wR_factor_all 0.0866 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 15502 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_gt 0.0813 _refine_ls_abs_structure_Flack 0.487(5) _refine_ls_abs_structure_details 'Flack (1983), 8320 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 40.8 65.8 40.6 18.1 4.72 ; # Insert your own references if required - in alphabetical order loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Ir1 Ir 0.62028(5) 0.577372(7) 0.49838(5) 0.0351 1.0000 Uani . . . . . . . C2 C 0.6245(6) 0.6854(2) 0.5041(7) 0.0413 1.0000 Uani . . . . . . . N3 N 0.6556(4) 0.7249(4) 0.5662(5) 0.0502 1.0000 Uani . . . . . . . C4 C 0.6496(5) 0.7964(4) 0.5483(5) 0.0599 1.0000 Uani . . . . . . . C5 C 0.6175(5) 0.8004(4) 0.4744(4) 0.0562 1.0000 Uani . . . . . . . N6 N 0.6020(3) 0.7323(3) 0.4459(4) 0.0411 1.0000 Uani . . . . . . . C7 C 0.6844(6) 0.6984(4) 0.6416(5) 0.0609 1.0000 Uani . . . . . . . C8 C 0.6495(8) 0.6897(5) 0.6795(6) 0.0856 1.0000 Uani . . . . . . . C9 C 0.6786(8) 0.6676(5) 0.7545(6) 0.0854 1.0000 Uani . . . . . . . C10 C 0.7429(6) 0.6517(5) 0.7878(5) 0.0876 1.0000 Uani . . . . . . . C11 C 0.7821(5) 0.6630(5) 0.7530(5) 0.0867 1.0000 Uani . . . . . . . C12 C 0.7514(4) 0.6863(4) 0.6762(5) 0.0663 1.0000 Uani . . . . . . . C13 C 0.5777(8) 0.7053(6) 0.6433(7) 0.0925 1.0000 Uani . . . . . . . C14 C 0.7813(9) 0.6243(7) 0.8699(5) 0.1679 1.0000 Uani . . . . . . . C15 C 0.7908(5) 0.6955(5) 0.6333(7) 0.0989 1.0000 Uani . . . . . . . C16 C 0.5678(5) 0.7156(4) 0.3675(6) 0.0513 1.0000 Uani . . . . . . . C17 C 0.6059(4) 0.7014(4) 0.3302(5) 0.0514 1.0000 Uani . . . . . . . C18 C 0.5748(6) 0.6880(5) 0.2558(6) 0.0768 1.0000 Uani . . . . . . . C19 C 0.5062(6) 0.6854(5) 0.2153(5) 0.0875 1.0000 Uani . . . . . . . C20 C 0.4711(5) 0.7000(5) 0.2546(5) 0.0903 1.0000 Uani . . . . . . . C21 C 0.5003(4) 0.7165(4) 0.3313(5) 0.0706 1.0000 Uani . . . . . . . C22 C 0.6801(5) 0.7014(5) 0.3704(7) 0.0649 1.0000 Uani . . . . . . . C23 C 0.4713(8) 0.6693(7) 0.1324(5) 0.1496 1.0000 Uani . . . . . . . C24 C 0.4596(5) 0.7342(7) 0.3719(7) 0.1078 1.0000 Uani . . . . . . . C25 C 0.6341(3) 0.4718(2) 0.4910(3) 0.0409 1.0000 Uani . . . . . . . N26 N 0.6866(2) 0.4333(2) 0.5403(3) 0.0475 1.0000 Uani . . . . . . . C27 C 0.6842(4) 0.3645(3) 0.5155(4) 0.0662 1.0000 Uani . . . . . . . C28 C 0.6289(4) 0.3599(3) 0.4492(4) 0.0662 1.0000 Uani . . . . . . . N29 N 0.5985(2) 0.4251(2) 0.4349(3) 0.0479 1.0000 Uani . . . . . . . C30 C 0.7394(3) 0.4555(3) 0.6108(3) 0.0484 1.0000 Uani . . . . . . . C31 C 0.7976(3) 0.4801(3) 0.6116(4) 0.0598 1.0000 Uani . . . . . . . C32 C 0.8492(3) 0.4980(4) 0.6804(4) 0.0715 1.0000 Uani . . . . . . . C33 C 0.8454(3) 0.4907(4) 0.7478(4) 0.0633 1.0000 Uani . . . . . . . C34 C 0.7859(4) 0.4689(4) 0.7433(5) 0.0580 1.0000 Uani . . . . . . . C35 C 0.7312(3) 0.4512(3) 0.6748(4) 0.0512 1.0000 Uani . . . . . . . C36 C 0.8040(4) 0.4877(5) 0.5404(5) 0.0873 1.0000 Uani . . . . . . . C37 C 0.9020(6) 0.5076(7) 0.8216(7) 0.1018 1.0000 Uani . . . . . . . C38 C 0.6675(3) 0.4276(4) 0.6719(4) 0.0695 1.0000 Uani . . . . . . . C39 C 0.5373(3) 0.4395(3) 0.3700(4) 0.0479 1.0000 Uani . . . . . . . C40 C 0.4793(3) 0.4172(3) 0.3725(4) 0.0576 1.0000 Uani . . . . . . . C41 C 0.4199(3) 0.4315(4) 0.3097(4) 0.0665 1.0000 Uani . . . . . . . C42 C 0.4174(4) 0.4671(4) 0.2485(4) 0.0637 1.0000 Uani . . . . . . . C43 C 0.4756(4) 0.4873(5) 0.2488(5) 0.0613 1.0000 Uani . . . . . . . C44 C 0.5362(3) 0.4740(3) 0.3085(3) 0.0501 1.0000 Uani . . . . . . . C45 C 0.4813(4) 0.3785(4) 0.4393(4) 0.0767 1.0000 Uani . . . . . . . C46 C 0.3507(5) 0.4817(7) 0.1818(7) 0.1015 1.0000 Uani . . . . . . . C47 C 0.5990(3) 0.4952(4) 0.3061(4) 0.0611 1.0000 Uani . . . . . . . B48 B 0.5273(3) 0.5697(4) 0.4904(4) 0.0637 1.0000 Uani . . . . . . . N49 N 0.4692(3) 0.5547(3) 0.4881(4) 0.0732 1.0000 Uani . . . . . . . C50 C 0.4639(4) 0.5395(5) 0.5569(5) 0.0874 1.0000 Uani . . . . . . . C51 C 0.4050(3) 0.5612(4) 0.4198(5) 0.0784 1.0000 Uani . . . . . . . B60 B 0.1257(6) 0.5536(2) 0.5013(7) 0.0340 1.0000 Uani . . . . . . . C61 C 0.1393(4) 0.5000(4) 0.4456(5) 0.0327 1.0000 Uani . . . . . . . C62 C 0.2008(3) 0.4702(4) 0.4712(5) 0.0362 1.0000 Uani . . . . . . . C63 C 0.2124(2) 0.4230(3) 0.4233(4) 0.0510 1.0000 Uani D . . . . . . C64 C 0.1686(4) 0.4077(4) 0.3553(5) 0.0411 1.0000 Uani . . . . . . . C65 C 0.1071(4) 0.4361(4) 0.3285(5) 0.0385 1.0000 Uani . . . . . . . C66 C 0.0913(4) 0.4842(4) 0.3735(5) 0.0393 1.0000 Uani . . . . . . . C67 C 0.27946(18) 0.39204(19) 0.4563(2) 0.0649 1.0000 Uani D . . . . . . F68 F 0.2839(3) 0.3304(4) 0.4890(6) 0.0964 0.583(12) Uani D . P 1 1 . . F69 F 0.3020(3) 0.3806(5) 0.4059(3) 0.0817 0.583(12) Uani D . P 1 1 . . F70 F 0.3254(3) 0.4321(3) 0.5092(5) 0.0682 0.583(12) Uani D . P 1 1 . . F681 F 0.2877(3) 0.3445(6) 0.4119(5) 0.0835 0.417(12) Uani D . P 1 2 . . F691 F 0.3269(3) 0.4390(3) 0.4713(7) 0.0772 0.417(12) Uani D . P 1 2 . . F701 F 0.2963(4) 0.3584(6) 0.5214(5) 0.0731 0.417(12) Uani D . P 1 2 . . C71 C 0.0548(5) 0.4196(4) 0.2519(6) 0.0498 1.0000 Uani . . . . . . . F72 F 0.0208(3) 0.4738(3) 0.2129(3) 0.0703 1.0000 Uani . . . . . . . F73 F 0.0763(4) 0.3860(5) 0.2104(3) 0.1133 1.0000 Uani . . . . . . . F74 F 0.0087(3) 0.3757(4) 0.2552(4) 0.0859 1.0000 Uani . . . . . . . C75 C 0.1824(4) 0.6087(4) 0.5462(5) 0.0350 1.0000 Uani . . . . . . . C76 C 0.1923(4) 0.6412(4) 0.6113(5) 0.0387 1.0000 Uani . . . . . . . C77 C 0.2416(3) 0.6913(3) 0.6479(3) 0.0402 1.0000 Uani . . . . . . . C78 C 0.2815(4) 0.7131(4) 0.6195(5) 0.0502 1.0000 Uani . . . . . . . C79 C 0.2734(3) 0.6843(3) 0.5537(5) 0.0483 1.0000 Uani . . . . . . . C80 C 0.2253(5) 0.6316(5) 0.5157(5) 0.0472 1.0000 Uani . . . . . . . C81 C 0.2494(4) 0.7226(3) 0.7210(3) 0.0536 1.0000 Uani . . . . . . . F82 F 0.1975(4) 0.7226(5) 0.7300(5) 0.1378 1.0000 Uani . . . . . . . F83 F 0.2953(5) 0.6850(4) 0.7791(3) 0.1313 1.0000 Uani . . . . . . . F84 F 0.2781(4) 0.7854(3) 0.7347(3) 0.0983 1.0000 Uani . . . . . . . C85 C 0.3164(4) 0.7078(4) 0.5198(5) 0.0733 1.0000 Uani . . . . . . . F86 F 0.2980(5) 0.6901(6) 0.4509(5) 0.1577 1.0000 Uani . . . . . . . F87 F 0.3286(3) 0.7764(3) 0.5276(3) 0.0962 1.0000 Uani . . . . . . . F88 F 0.3812(3) 0.6840(5) 0.5628(5) 0.1444 1.0000 Uani . . . . . . . C89 C 0.0569(5) 0.6031(5) 0.4576(5) 0.0395 1.0000 Uani . . . . . . . C90 C 0.0484(5) 0.6383(5) 0.3910(5) 0.0430 1.0000 Uani . . . . . . . C91 C -0.0057(4) 0.6813(4) 0.3519(3) 0.0647 1.0000 Uani D . . . . . . C92 C -0.0530(4) 0.6916(4) 0.3777(5) 0.0532 1.0000 Uani . . . . . . . C93 C -0.0434(3) 0.6580(4) 0.4452(4) 0.0490 1.0000 Uani . . . . . . . C94 C 0.0117(4) 0.6173(5) 0.4834(5) 0.0464 1.0000 Uani . . . . . . . C95 C -0.0129(2) 0.7164(3) 0.2821(2) 0.0768 1.0000 Uani D . . . . . . F96 F 0.0351(4) 0.7011(5) 0.2640(4) 0.0778 0.542(7) Uani D . P 2 1 . . F97 F -0.0133(5) 0.7861(3) 0.2854(4) 0.0921 0.542(7) Uani D . P 2 1 . . F98 F -0.0685(3) 0.6997(5) 0.2212(4) 0.0814 0.542(7) Uani D . P 2 1 . . F961 F 0.0360(4) 0.7610(5) 0.2933(4) 0.0870 0.458(7) Uani D . P 2 2 . . F971 F -0.0675(4) 0.7544(5) 0.2481(4) 0.0917 0.458(7) Uani D . P 2 2 . . F981 F -0.0146(5) 0.6725(4) 0.2304(4) 0.0876 0.458(7) Uani D . P 2 2 . . C99 C -0.0959(3) 0.6653(4) 0.4719(5) 0.0655 1.0000 Uani . . . . . . . F100 F -0.1431(3) 0.6191(4) 0.4398(5) 0.1376 1.0000 Uani . . . . . . . F101 F -0.1210(4) 0.7297(4) 0.4580(4) 0.1167 1.0000 Uani . . . . . . . F102 F -0.0719(4) 0.6565(5) 0.5425(5) 0.1159 1.0000 Uani . . . . . . . C103 C 0.1153(4) 0.5009(4) 0.5615(5) 0.0337 1.0000 Uani . . . . . . . C104 C 0.0546(4) 0.4629(4) 0.5369(4) 0.0387 1.0000 Uani . . . . . . . C105 C 0.0406(3) 0.4185(3) 0.5819(4) 0.0585 1.0000 Uani D . . . . . . C106 C 0.0909(4) 0.4046(5) 0.6580(5) 0.0455 1.0000 Uani . . . . . . . C107 C 0.1519(4) 0.4370(5) 0.6813(5) 0.0451 1.0000 Uani . . . . . . . C108 C 0.1610(4) 0.4821(4) 0.6332(5) 0.0408 1.0000 Uani . . . . . . . C109 C -0.0259(2) 0.3868(2) 0.5540(3) 0.0731 1.0000 Uani D . . . . . . F110 F -0.0390(3) 0.3629(4) 0.6083(3) 0.0920 0.621(8) Uani D . P 3 1 . . F111 F -0.0749(3) 0.4312(3) 0.5147(5) 0.0779 0.621(8) Uani D . P 3 1 . . F112 F -0.0360(3) 0.3319(4) 0.5084(5) 0.0865 0.621(8) Uani D . P 3 1 . . F1101 F -0.0609(4) 0.4122(5) 0.5880(6) 0.0795 0.379(8) Uani D . P 3 2 . . F1111 F -0.0644(4) 0.3968(6) 0.4807(4) 0.0953 0.379(8) Uani D . P 3 2 . . F1121 F -0.0251(3) 0.3168(3) 0.5635(7) 0.0772 0.379(8) Uani D . P 3 2 . . C113 C 0.2064(5) 0.4192(5) 0.7551(6) 0.0581 1.0000 Uani . . . . . . . F114 F 0.1849(4) 0.3994(5) 0.8063(3) 0.1082 1.0000 Uani . . . . . . . F115 F 0.2472(4) 0.3723(4) 0.7550(4) 0.1148 1.0000 Uani . . . . . . . F116 F 0.2447(3) 0.4764(4) 0.7899(3) 0.0932 1.0000 Uani . . . . . . . H1 H 0.6619 0.5820 0.4526 0.0480 1.0000 Uiso R . . . . . . H2 H 0.6969 0.5828 0.5549 0.0476 1.0000 Uiso R . . . . . . H4 H 0.6651 0.8336 0.5826 0.0780 1.0000 Uiso R . . . . . . H5 H 0.6064 0.8414 0.4451 0.0743 1.0000 Uiso R . . . . . . H9 H 0.6542 0.6637 0.7817 0.1089 1.0000 Uiso R . . . . . . H11 H 0.8266 0.6559 0.7770 0.1040 1.0000 Uiso R . . . . . . H18 H 0.6002 0.6804 0.2298 0.0932 1.0000 Uiso R . . . . . . H20 H 0.4256 0.6988 0.2293 0.1282 1.0000 Uiso R . . . . . . H27 H 0.7153 0.3293 0.5405 0.0861 1.0000 Uiso R . . . . . . H28 H 0.6138 0.3210 0.4183 0.0808 1.0000 Uiso R . . . . . . H32 H 0.8879 0.5156 0.6826 0.0980 1.0000 Uiso R . . . . . . H34 H 0.7810 0.4657 0.7869 0.0708 1.0000 Uiso R . . . . . . H41 H 0.3809 0.4167 0.3091 0.0811 1.0000 Uiso R . . . . . . H43 H 0.4736 0.5117 0.2073 0.0780 1.0000 Uiso R . . . . . . H62 H 0.2334 0.4804 0.5192 0.0508 1.0000 Uiso R . . . . . . H64 H 0.1799 0.3782 0.3253 0.0543 1.0000 Uiso R . . . . . . H66 H 0.0497 0.5051 0.3536 0.0508 1.0000 Uiso R . . . . . . H76 H 0.1653 0.6295 0.6327 0.0515 1.0000 Uiso R . . . . . . H78 H 0.3139 0.7467 0.6432 0.0562 1.0000 Uiso R . . . . . . H80 H 0.2219 0.6114 0.4716 0.0605 1.0000 Uiso R . . . . . . H90 H 0.0793 0.6339 0.3734 0.0487 1.0000 Uiso R . . . . . . H92 H -0.0895 0.7200 0.3508 0.0642 1.0000 Uiso R . . . . . . H94 H 0.0175 0.5986 0.5291 0.0567 1.0000 Uiso R . . . . . . H104 H 0.0233 0.4678 0.4869 0.0489 1.0000 Uiso R . . . . . . H106 H 0.0835 0.3748 0.6908 0.0581 1.0000 Uiso R . . . . . . H108 H 0.2035 0.5006 0.6512 0.0419 1.0000 Uiso R . . . . . . H133 H 0.5615 0.6975 0.6795 0.1170 1.0000 Uiso R . . . . . . H131 H 0.5701 0.7534 0.6265 0.1169 1.0000 Uiso R . . . . . . H132 H 0.5555 0.6742 0.6007 0.1171 1.0000 Uiso R . . . . . . H141 H 0.8272 0.6343 0.8876 0.2610 1.0000 Uiso R . . . . . . H142 H 0.7652 0.6481 0.9006 0.2610 1.0000 Uiso R . . . . . . H143 H 0.7742 0.5742 0.8704 0.2609 1.0000 Uiso R . . . . . . H151 H 0.8355 0.6804 0.6628 0.1420 1.0000 Uiso R . . . . . . H152 H 0.7907 0.7440 0.6208 0.1421 1.0000 Uiso R . . . . . . H153 H 0.7717 0.6696 0.5870 0.1420 1.0000 Uiso R . . . . . . H221 H 0.6964 0.7233 0.3383 0.1004 1.0000 Uiso R . . . . . . H222 H 0.6960 0.7260 0.4173 0.1003 1.0000 Uiso R . . . . . . H223 H 0.6952 0.6533 0.3799 0.1004 1.0000 Uiso R . . . . . . H232 H 0.4255 0.6815 0.1119 0.2010 1.0000 Uiso R . . . . . . H231 H 0.4905 0.6960 0.1066 0.2012 1.0000 Uiso R . . . . . . H233 H 0.4748 0.6199 0.1239 0.2009 1.0000 Uiso R . . . . . . H242 H 0.4178 0.7105 0.3477 0.1700 1.0000 Uiso R . . . . . . H243 H 0.4518 0.7841 0.3697 0.1701 1.0000 Uiso R . . . . . . H241 H 0.4814 0.7201 0.4234 0.1700 1.0000 Uiso R . . . . . . H362 H 0.8474 0.5048 0.5515 0.1349 1.0000 Uiso R . . . . . . H361 H 0.7715 0.5202 0.5080 0.1350 1.0000 Uiso R . . . . . . H363 H 0.7962 0.4427 0.5157 0.1350 1.0000 Uiso R . . . . . . H372 H 0.9258 0.5472 0.8158 0.1209 1.0000 Uiso R . . . . . . H371 H 0.8868 0.5183 0.8585 0.1210 1.0000 Uiso R . . . . . . H373 H 0.9321 0.4680 0.8395 0.1211 1.0000 Uiso R . . . . . . H381 H 0.6725 0.4242 0.7225 0.1071 1.0000 Uiso R . . . . . . H382 H 0.6335 0.4614 0.6444 0.1070 1.0000 Uiso R . . . . . . H383 H 0.6546 0.3821 0.6474 0.1068 1.0000 Uiso R . . . . . . H453 H 0.4379 0.3780 0.4366 0.1110 1.0000 Uiso R . . . . . . H452 H 0.5114 0.4022 0.4842 0.1111 1.0000 Uiso R . . . . . . H451 H 0.4956 0.3310 0.4390 0.1108 1.0000 Uiso R . . . . . . H461 H 0.3174 0.4603 0.1916 0.1430 1.0000 Uiso R . . . . . . H463 H 0.3430 0.5310 0.1747 0.1429 1.0000 Uiso R . . . . . . H462 H 0.3490 0.4612 0.1374 0.1430 1.0000 Uiso R . . . . . . H471 H 0.6205 0.4549 0.2991 0.0951 1.0000 Uiso R . . . . . . H472 H 0.5883 0.5269 0.2645 0.0952 1.0000 Uiso R . . . . . . H473 H 0.6283 0.5170 0.3517 0.0955 1.0000 Uiso R . . . . . . H482 H 0.5448 0.5728 0.4311 0.0640 1.0000 Uiso R . . . . . . H481 H 0.5882 0.5739 0.5564 0.0643 1.0000 Uiso R . . . . . . H502 H 0.4270 0.5650 0.5564 0.1419 1.0000 Uiso R . . . . . . H501 H 0.5041 0.5539 0.6000 0.1418 1.0000 Uiso R . . . . . . H503 H 0.4576 0.4895 0.5596 0.1421 1.0000 Uiso R . . . . . . H511 H 0.3823 0.5168 0.4087 0.1190 1.0000 Uiso R . . . . . . H512 H 0.3773 0.5966 0.4263 0.1189 1.0000 Uiso R . . . . . . H513 H 0.4124 0.5746 0.3775 0.1190 1.0000 Uiso R . . . . . . 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 0.03477(7) 0.02866(6) 0.04139(7) 0.00016(17) 0.01699(5) 0.00112(16) C2 0.047(3) 0.0330(17) 0.045(3) 0.009(4) 0.022(3) 0.002(3) N3 0.060(4) 0.033(3) 0.062(4) -0.004(3) 0.032(3) -0.003(2) C4 0.092(6) 0.035(3) 0.062(5) -0.008(3) 0.043(5) -0.009(4) C5 0.090(6) 0.024(2) 0.066(6) 0.004(3) 0.045(5) 0.003(3) N6 0.049(3) 0.029(2) 0.050(3) 0.004(2) 0.026(3) 0.002(2) C7 0.089(6) 0.035(4) 0.043(4) -0.008(3) 0.017(4) -0.006(4) C8 0.171(12) 0.042(4) 0.052(5) -0.005(3) 0.058(7) 0.003(5) C9 0.138(10) 0.064(6) 0.053(5) -0.008(4) 0.042(6) 0.005(6) C10 0.134(9) 0.057(5) 0.063(5) -0.015(4) 0.038(6) -0.005(5) C11 0.086(6) 0.057(4) 0.074(5) -0.012(4) 0.000(4) -0.006(4) C12 0.077(5) 0.044(4) 0.060(4) -0.003(3) 0.016(4) -0.008(3) C13 0.169(14) 0.059(5) 0.083(7) -0.012(5) 0.086(9) -0.020(7) C14 0.29(2) 0.103(8) 0.045(5) 0.013(5) 0.022(8) 0.040(11) C15 0.060(5) 0.074(6) 0.127(8) 0.004(6) 0.011(5) -0.012(4) C16 0.063(4) 0.029(3) 0.058(5) 0.006(3) 0.024(3) 0.012(3) C17 0.060(4) 0.038(3) 0.059(5) 0.014(3) 0.030(3) 0.012(3) C18 0.114(8) 0.058(5) 0.051(5) 0.004(4) 0.031(5) 0.015(5) C19 0.118(8) 0.051(4) 0.065(5) 0.003(4) 0.017(5) 0.008(5) C20 0.080(6) 0.069(5) 0.071(5) 0.013(4) -0.009(4) 0.004(5) C21 0.067(5) 0.047(4) 0.072(5) 0.003(4) 0.009(4) 0.015(4) C22 0.067(4) 0.057(5) 0.092(6) 0.014(4) 0.054(4) 0.001(3) C23 0.222(15) 0.101(8) 0.047(5) -0.012(5) -0.007(6) 0.006(9) C24 0.061(5) 0.128(9) 0.124(8) 0.035(8) 0.033(5) 0.044(6) C25 0.044(3) 0.033(2) 0.049(3) 0.002(2) 0.024(2) 0.0016(18) N26 0.052(2) 0.033(2) 0.055(2) 0.0068(17) 0.022(2) 0.0135(17) C27 0.090(5) 0.038(3) 0.077(4) 0.005(3) 0.043(4) 0.023(3) C28 0.090(5) 0.033(3) 0.068(4) -0.006(2) 0.029(4) 0.013(3) N29 0.055(2) 0.0312(18) 0.054(2) -0.0024(19) 0.022(2) 0.0078(19) C30 0.045(3) 0.049(3) 0.048(3) 0.002(2) 0.018(2) 0.016(2) C31 0.045(3) 0.067(4) 0.074(4) 0.012(3) 0.033(3) 0.013(3) C32 0.042(3) 0.088(5) 0.079(5) 0.017(4) 0.023(3) 0.013(3) C33 0.042(4) 0.066(4) 0.064(4) 0.010(3) 0.009(3) 0.005(3) C34 0.053(5) 0.061(4) 0.057(4) 0.013(3) 0.022(4) 0.002(4) C35 0.049(3) 0.046(3) 0.062(4) 0.011(3) 0.029(3) 0.008(3) C36 0.070(4) 0.132(7) 0.081(5) 0.015(5) 0.052(4) 0.023(5) C37 0.081(7) 0.108(8) 0.071(6) 0.009(5) -0.004(5) 0.016(6) C38 0.061(4) 0.083(5) 0.072(4) 0.015(4) 0.037(3) 0.005(4) C39 0.051(3) 0.035(3) 0.058(4) -0.010(2) 0.025(3) -0.004(2) C40 0.062(3) 0.043(3) 0.075(4) -0.016(3) 0.038(3) -0.017(3) C41 0.053(3) 0.077(4) 0.070(4) -0.022(3) 0.028(3) -0.017(3) C42 0.042(4) 0.071(5) 0.062(4) -0.018(3) 0.010(3) 0.002(3) C43 0.051(4) 0.080(5) 0.049(4) -0.012(3) 0.019(3) 0.001(3) C44 0.052(3) 0.041(3) 0.058(3) -0.010(2) 0.026(3) 0.001(2) C45 0.086(5) 0.070(4) 0.083(5) -0.004(4) 0.046(4) -0.020(4) C46 0.061(5) 0.139(11) 0.081(7) -0.025(7) 0.012(5) -0.009(6) C47 0.058(3) 0.069(4) 0.063(4) -0.007(3) 0.034(3) -0.009(3) B48 0.049(3) 0.080(5) 0.063(4) -0.014(4) 0.026(3) -0.004(3) N49 0.049(3) 0.080(4) 0.093(4) 0.005(3) 0.034(3) 0.004(3) C50 0.065(4) 0.095(6) 0.115(7) 0.009(5) 0.053(5) -0.011(4) C51 0.042(3) 0.081(5) 0.110(6) -0.006(4) 0.032(4) 0.008(3) B60 0.029(3) 0.0362(17) 0.037(2) 0.011(4) 0.016(3) 0.010(3) C61 0.028(3) 0.035(3) 0.034(3) 0.005(2) 0.013(2) 0.004(2) C62 0.032(3) 0.028(3) 0.050(4) 0.001(2) 0.020(3) 0.003(2) C63 0.057(3) 0.036(3) 0.080(4) 0.005(3) 0.048(3) 0.009(2) C64 0.052(4) 0.037(3) 0.041(4) -0.005(2) 0.028(3) 0.002(3) C65 0.046(4) 0.033(3) 0.034(3) -0.002(2) 0.017(3) -0.002(3) C66 0.046(4) 0.036(3) 0.041(4) -0.003(3) 0.025(3) 0.001(3) C67 0.057(2) 0.054(2) 0.102(3) 0.001(2) 0.052(2) 0.0121(19) F68 0.068(4) 0.055(4) 0.141(6) 0.022(4) 0.026(4) 0.012(4) F69 0.075(4) 0.078(5) 0.112(4) -0.031(4) 0.060(3) 0.012(4) F70 0.054(3) 0.069(4) 0.095(4) -0.012(3) 0.045(3) 0.013(3) F681 0.072(5) 0.065(5) 0.113(5) -0.014(4) 0.042(4) 0.025(4) F691 0.056(4) 0.073(4) 0.122(6) 0.013(4) 0.058(4) -0.004(3) F701 0.061(4) 0.062(5) 0.098(5) 0.009(4) 0.038(4) 0.030(4) C71 0.057(5) 0.044(3) 0.050(5) -0.003(3) 0.026(4) 0.001(3) F72 0.080(3) 0.053(2) 0.049(2) 0.0163(18) 0.004(2) -0.002(2) F73 0.107(5) 0.160(6) 0.049(3) -0.048(3) 0.015(3) 0.042(4) F74 0.088(4) 0.084(3) 0.059(3) -0.008(2) 0.010(3) -0.050(3) C75 0.031(3) 0.030(3) 0.047(4) 0.009(3) 0.020(3) 0.003(2) C76 0.044(5) 0.030(4) 0.041(4) -0.002(3) 0.018(4) -0.001(3) C77 0.037(3) 0.032(3) 0.042(3) 0.008(2) 0.009(2) -0.006(2) C78 0.046(3) 0.038(3) 0.063(4) 0.002(3) 0.021(3) -0.004(3) C79 0.045(3) 0.042(3) 0.069(4) -0.001(3) 0.035(3) -0.003(3) C80 0.056(4) 0.047(4) 0.046(4) 0.001(3) 0.030(3) -0.002(3) C81 0.073(4) 0.033(3) 0.046(3) -0.012(2) 0.019(3) -0.021(3) F82 0.142(6) 0.180(8) 0.141(6) -0.121(6) 0.108(5) -0.098(5) F83 0.205(8) 0.099(4) 0.043(3) 0.007(3) 0.015(4) 0.008(5) F84 0.147(5) 0.052(3) 0.071(3) -0.023(2) 0.027(3) -0.041(3) C85 0.070(5) 0.069(4) 0.105(6) -0.006(4) 0.060(4) -0.003(4) F86 0.189(9) 0.229(10) 0.100(5) -0.063(5) 0.105(6) -0.140(8) F87 0.114(4) 0.076(3) 0.133(4) -0.007(3) 0.086(4) -0.027(3) F88 0.082(4) 0.161(7) 0.226(9) 0.044(7) 0.101(5) 0.034(5) C89 0.051(4) 0.035(3) 0.027(3) 0.003(2) 0.014(3) -0.001(3) C90 0.046(5) 0.039(5) 0.044(5) -0.001(4) 0.021(4) 0.006(4) C91 0.089(4) 0.055(4) 0.047(3) 0.008(3) 0.028(3) 0.017(3) C92 0.050(4) 0.049(4) 0.052(4) 0.002(3) 0.017(3) 0.016(3) C93 0.051(4) 0.048(4) 0.051(3) 0.003(3) 0.025(3) 0.012(3) C94 0.042(4) 0.049(4) 0.044(4) -0.005(3) 0.016(3) 0.008(3) C95 0.099(3) 0.073(3) 0.055(3) 0.018(2) 0.032(2) 0.022(3) F96 0.101(5) 0.084(4) 0.052(4) 0.032(3) 0.038(3) 0.029(4) F97 0.146(6) 0.063(4) 0.058(4) 0.012(3) 0.039(4) 0.028(4) F98 0.082(4) 0.105(5) 0.056(4) 0.014(4) 0.031(3) 0.016(4) F961 0.089(5) 0.102(5) 0.066(4) 0.036(4) 0.031(4) 0.004(4) F971 0.096(5) 0.079(5) 0.077(5) 0.035(4) 0.019(4) 0.032(4) F981 0.128(6) 0.077(5) 0.055(4) 0.013(3) 0.038(4) 0.027(5) C99 0.041(3) 0.073(5) 0.084(5) 0.004(4) 0.030(3) 0.021(3) F100 0.103(4) 0.160(6) 0.189(7) -0.065(5) 0.101(5) -0.048(4) F101 0.117(5) 0.105(4) 0.176(6) 0.045(4) 0.108(5) 0.069(4) F102 0.089(4) 0.179(7) 0.115(5) 0.029(5) 0.076(4) 0.058(4) C103 0.035(3) 0.029(3) 0.039(4) -0.005(2) 0.019(3) -0.005(2) C104 0.038(3) 0.044(3) 0.036(3) 0.002(2) 0.018(3) 0.009(3) C105 0.075(3) 0.051(3) 0.076(4) -0.009(3) 0.057(3) -0.009(3) C106 0.054(5) 0.042(3) 0.042(4) 0.003(3) 0.023(3) 0.004(3) C107 0.052(5) 0.044(3) 0.037(4) -0.001(3) 0.018(3) 0.001(3) C108 0.049(4) 0.032(3) 0.036(3) 0.003(2) 0.014(3) 0.008(3) C109 0.077(3) 0.068(3) 0.095(3) -0.004(2) 0.057(2) -0.012(2) F110 0.089(4) 0.109(5) 0.093(4) 0.024(4) 0.054(3) -0.024(4) F111 0.064(4) 0.096(4) 0.102(4) 0.003(3) 0.063(3) 0.003(3) F112 0.071(4) 0.074(4) 0.118(5) -0.027(4) 0.046(4) -0.014(3) F1101 0.082(5) 0.064(5) 0.117(5) -0.011(4) 0.067(4) -0.019(4) F1111 0.087(5) 0.084(5) 0.110(5) 0.000(5) 0.042(5) -0.021(5) F1121 0.075(5) 0.060(4) 0.105(5) -0.007(4) 0.048(4) -0.020(4) C113 0.065(6) 0.064(5) 0.036(3) 0.013(3) 0.016(4) 0.008(4) F114 0.103(5) 0.163(6) 0.046(3) 0.035(3) 0.022(3) -0.008(4) F115 0.112(5) 0.108(5) 0.064(3) -0.013(3) -0.012(3) 0.060(4) F116 0.092(4) 0.095(4) 0.050(3) 0.011(2) -0.005(3) -0.017(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.13755(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ir1 . C2 . 2.058(4) yes Ir1 . C25 . 2.048(5) yes Ir1 . B48 . 2.058(7) yes Ir1 . H1 . 1.592 no Ir1 . H2 . 1.595 no Ir1 . H482 . 1.635 no Ir1 . H481 . 1.628 no C2 . N3 . 1.343(13) yes C2 . N6 . 1.365(11) yes N3 . C4 . 1.397(10) yes N3 . C7 . 1.433(12) yes C4 . C5 . 1.318(11) yes C4 . H4 . 0.934 no C5 . N6 . 1.395(10) yes C5 . H5 . 0.938 no N6 . C16 . 1.431(11) yes C7 . C8 . 1.336(17) yes C7 . C12 . 1.378(14) yes C8 . C9 . 1.398(15) yes C8 . C13 . 1.488(18) yes C9 . C10 . 1.339(18) yes C9 . H9 . 0.941 no C10 . C11 . 1.378(16) yes C10 . C14 . 1.555(13) yes C11 . C12 . 1.437(13) yes C11 . H11 . 0.914 no C12 . C15 . 1.509(15) yes C13 . H133 . 0.961 no C13 . H131 . 0.962 no C13 . H132 . 0.968 no C14 . H141 . 0.960 no C14 . H142 . 0.959 no C14 . H143 . 0.967 no C15 . H151 . 0.960 no C15 . H152 . 0.955 no C15 . H153 . 0.960 no C16 . C17 . 1.405(13) yes C16 . C21 . 1.370(13) yes C17 . C18 . 1.349(13) yes C17 . C22 . 1.506(12) yes C18 . C19 . 1.398(17) yes C18 . H18 . 0.947 no C19 . C20 . 1.381(16) yes C19 . C23 . 1.506(12) yes C20 . C21 . 1.399(13) yes C20 . H20 . 0.925 no C21 . C24 . 1.523(14) yes C22 . H221 . 0.968 no C22 . H222 . 0.960 no C22 . H223 . 0.965 no C23 . H232 . 0.961 no C23 . H231 . 0.959 no C23 . H233 . 0.965 no C24 . H242 . 0.962 no C24 . H243 . 0.963 no C24 . H241 . 0.955 no C25 . N26 . 1.367(7) yes C25 . N29 . 1.369(7) yes N26 . C27 . 1.389(7) yes N26 . C30 . 1.438(7) yes C27 . C28 . 1.354(10) yes C27 . H27 . 0.938 no C28 . N29 . 1.385(7) yes C28 . H28 . 0.923 no N29 . C39 . 1.434(8) yes C30 . C31 . 1.403(8) yes C30 . C35 . 1.377(9) yes C31 . C32 . 1.384(10) yes C31 . C36 . 1.502(9) yes C32 . C33 . 1.393(11) yes C32 . H32 . 0.928 no C33 . C34 . 1.383(10) yes C33 . C37 . 1.487(13) yes C34 . C35 . 1.409(11) yes C34 . H34 . 0.930 no C35 . C38 . 1.497(9) yes C36 . H362 . 0.965 no C36 . H361 . 0.955 no C36 . H363 . 0.963 no C37 . H372 . 0.966 no C37 . H371 . 0.968 no C37 . H373 . 0.970 no C38 . H381 . 0.968 no C38 . H382 . 0.964 no C38 . H383 . 0.971 no C39 . C40 . 1.410(8) yes C39 . C44 . 1.383(9) yes C40 . C41 . 1.391(10) yes C40 . C45 . 1.506(10) yes C41 . C42 . 1.377(11) yes C41 . H41 . 0.927 no C42 . C43 . 1.379(11) yes C42 . C46 . 1.523(13) yes C43 . C44 . 1.377(10) yes C43 . H43 . 0.933 no C44 . C47 . 1.510(9) yes C45 . H453 . 0.967 no C45 . H452 . 0.958 no C45 . H451 . 0.962 no C46 . H461 . 0.955 no C46 . H463 . 0.953 no C46 . H462 . 0.954 no C47 . H471 . 0.954 no C47 . H472 . 0.964 no C47 . H473 . 0.946 no B48 . N49 . 1.336(9) yes B48 . H482 . 1.414 no B48 . H481 . 1.416 no N49 . C50 . 1.462(10) yes N49 . C51 . 1.483(9) yes C50 . H502 . 0.968 no C50 . H501 . 0.968 no C50 . H503 . 0.968 no C51 . H511 . 0.963 no C51 . H512 . 0.971 no C51 . H513 . 0.967 no B60 . C61 . 1.639(14) yes B60 . C75 . 1.587(12) yes B60 . C89 . 1.692(13) yes B60 . C103 . 1.665(13) yes C61 . C62 . 1.377(10) yes C61 . C66 . 1.388(12) yes C62 . C63 . 1.423(10) yes C62 . H62 . 0.927 no C63 . C64 . 1.301(10) yes C63 . C67 . 1.484(4) yes C64 . C65 . 1.364(11) yes C64 . H64 . 0.939 no C65 . C66 . 1.440(11) yes C65 . C71 . 1.484(13) yes C66 . H66 . 0.934 no C67 . F68 . 1.324(5) yes C67 . F69 . 1.339(5) yes C67 . F70 . 1.337(5) yes C67 . F681 . 1.338(5) yes C67 . F691 . 1.327(5) yes C67 . F701 . 1.340(5) yes C71 . F72 . 1.312(10) yes C71 . F73 . 1.307(12) yes C71 . F74 . 1.368(11) yes C75 . C76 . 1.362(12) yes C75 . C80 . 1.435(12) yes C76 . C77 . 1.399(10) yes C76 . H76 . 0.925 no C77 . C78 . 1.340(11) yes C77 . C81 . 1.511(8) yes C78 . C79 . 1.357(12) yes C78 . H78 . 0.926 no C79 . C80 . 1.423(12) yes C79 . C85 . 1.489(9) yes C80 . H80 . 0.932 no C81 . F82 . 1.275(9) yes C81 . F83 . 1.358(9) yes C81 . F84 . 1.330(7) yes C85 . F86 . 1.289(11) yes C85 . F87 . 1.328(9) yes C85 . F88 . 1.405(10) yes C89 . C90 . 1.422(13) yes C89 . C94 . 1.371(13) yes C90 . C91 . 1.386(11) yes C90 . H90 . 0.925 no C91 . C92 . 1.407(11) yes C91 . C95 . 1.484(4) yes C92 . C93 . 1.416(11) yes C92 . H92 . 0.931 no C93 . C94 . 1.373(11) yes C93 . C99 . 1.523(10) yes C94 . H94 . 0.932 no C95 . F96 . 1.333(5) yes C95 . F97 . 1.327(5) yes C95 . F98 . 1.336(5) yes C95 . F961 . 1.336(5) yes C95 . F971 . 1.328(5) yes C95 . F981 . 1.316(5) yes C99 . F100 . 1.311(10) yes C99 . F101 . 1.326(9) yes C99 . F102 . 1.272(10) yes C103 . C104 . 1.435(11) yes C103 . C108 . 1.380(12) yes C104 . C105 . 1.374(11) yes C104 . H104 . 0.932 no C105 . C106 . 1.451(11) yes C105 . C109 . 1.485(4) yes C106 . C107 . 1.395(12) yes C106 . H106 . 0.938 no C107 . C108 . 1.371(13) yes C107 . C113 . 1.471(12) yes C108 . H108 . 0.936 no C109 . F110 . 1.329(5) yes C109 . F111 . 1.333(5) yes C109 . F112 . 1.335(5) yes C109 . F1101 . 1.352(5) yes C109 . F1111 . 1.334(5) yes C109 . F1121 . 1.343(5) yes C113 . F114 . 1.374(13) yes C113 . F115 . 1.290(12) yes C113 . F116 . 1.369(11) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 . Ir1 . C25 . 168.0(4) yes C2 . Ir1 . B48 . 95.5(4) yes C25 . Ir1 . B48 . 96.4(3) yes C2 . Ir1 . H1 . 87.2 no C25 . Ir1 . H1 . 82.0 no B48 . Ir1 . H1 . 145.3 no C2 . Ir1 . H2 . 83.5 no C25 . Ir1 . H2 . 87.7 no B48 . Ir1 . H2 . 144.9 no H1 . Ir1 . H2 . 69.8 no C2 . Ir1 . H482 . 95.9 no C25 . Ir1 . H482 . 91.6 no B48 . Ir1 . H482 . 43.1 no H1 . Ir1 . H482 . 102.2 no H2 . Ir1 . H482 . 172.0 no C2 . Ir1 . H481 . 91.5 no C25 . Ir1 . H481 . 98.4 no B48 . Ir1 . H481 . 43.2 no H1 . Ir1 . H481 . 171.4 no H2 . Ir1 . H481 . 101.6 no H482 . Ir1 . H481 . 86.4 no Ir1 . C2 . N3 . 127.0(7) yes Ir1 . C2 . N6 . 127.9(8) yes N3 . C2 . N6 . 104.9(4) yes C2 . N3 . C4 . 111.0(7) yes C2 . N3 . C7 . 124.8(7) yes C4 . N3 . C7 . 123.8(7) yes N3 . C4 . C5 . 106.4(9) yes N3 . C4 . H4 . 126.0 no C5 . C4 . H4 . 127.6 no C4 . C5 . N6 . 108.2(8) yes C4 . C5 . H5 . 127.0 no N6 . C5 . H5 . 124.9 no C5 . N6 . C2 . 109.4(7) yes C5 . N6 . C16 . 124.2(7) yes C2 . N6 . C16 . 126.4(7) yes N3 . C7 . C8 . 122.2(11) yes N3 . C7 . C12 . 117.3(10) yes C8 . C7 . C12 . 120.4(10) yes C7 . C8 . C9 . 122.0(15) yes C7 . C8 . C13 . 120.6(10) yes C9 . C8 . C13 . 117.4(13) yes C8 . C9 . C10 . 118.6(14) yes C8 . C9 . H9 . 121.7 no C10 . C9 . H9 . 119.7 no C9 . C10 . C11 . 121.9(10) yes C9 . C10 . C14 . 124.3(13) yes C11 . C10 . C14 . 113.7(12) yes C10 . C11 . C12 . 118.3(9) yes C10 . C11 . H11 . 122.3 no C12 . C11 . H11 . 119.3 no C11 . C12 . C7 . 118.5(9) yes C11 . C12 . C15 . 121.0(9) yes C7 . C12 . C15 . 120.5(8) yes C8 . C13 . H133 . 108.6 no C8 . C13 . H131 . 110.0 no H133 . C13 . H131 . 109.8 no C8 . C13 . H132 . 108.9 no H133 . C13 . H132 . 110.0 no H131 . C13 . H132 . 109.5 no C10 . C14 . H141 . 108.5 no C10 . C14 . H142 . 108.7 no H141 . C14 . H142 . 110.0 no C10 . C14 . H143 . 108.9 no H141 . C14 . H143 . 110.5 no H142 . C14 . H143 . 110.2 no C12 . C15 . H151 . 111.0 no C12 . C15 . H152 . 109.3 no H151 . C15 . H152 . 108.9 no C12 . C15 . H153 . 111.1 no H151 . C15 . H153 . 109.1 no H152 . C15 . H153 . 107.4 no N6 . C16 . C17 . 117.6(8) yes N6 . C16 . C21 . 119.7(9) yes C17 . C16 . C21 . 122.7(9) yes C16 . C17 . C18 . 118.7(10) yes C16 . C17 . C22 . 122.3(9) yes C18 . C17 . C22 . 119.0(10) yes C17 . C18 . C19 . 122.1(11) yes C17 . C18 . H18 . 119.1 no C19 . C18 . H18 . 118.8 no C18 . C19 . C20 . 116.8(9) yes C18 . C19 . C23 . 122.3(12) yes C20 . C19 . C23 . 120.9(12) yes C19 . C20 . C21 . 123.9(9) yes C19 . C20 . H20 . 118.7 no C21 . C20 . H20 . 117.4 no C20 . C21 . C16 . 115.8(9) yes C20 . C21 . C24 . 122.0(9) yes C16 . C21 . C24 . 122.2(9) yes C17 . C22 . H221 . 108.9 no C17 . C22 . H222 . 110.8 no H221 . C22 . H222 . 110.3 no C17 . C22 . H223 . 108.6 no H221 . C22 . H223 . 109.1 no H222 . C22 . H223 . 109.1 no C19 . C23 . H232 . 110.3 no C19 . C23 . H231 . 110.0 no H232 . C23 . H231 . 108.5 no C19 . C23 . H233 . 110.3 no H232 . C23 . H233 . 108.7 no H231 . C23 . H233 . 109.0 no C21 . C24 . H242 . 109.6 no C21 . C24 . H243 . 109.8 no H242 . C24 . H243 . 108.6 no C21 . C24 . H241 . 111.5 no H242 . C24 . H241 . 108.6 no H243 . C24 . H241 . 108.7 no Ir1 . C25 . N26 . 125.9(4) yes Ir1 . C25 . N29 . 129.9(4) yes N26 . C25 . N29 . 103.9(4) yes C25 . N26 . C27 . 111.6(5) yes C25 . N26 . C30 . 128.1(4) yes C27 . N26 . C30 . 120.3(5) yes N26 . C27 . C28 . 106.2(5) yes N26 . C27 . H27 . 125.8 no C28 . C27 . H27 . 128.0 no C27 . C28 . N29 . 107.4(5) yes C27 . C28 . H28 . 127.2 no N29 . C28 . H28 . 125.4 no C28 . N29 . C25 . 111.0(5) yes C28 . N29 . C39 . 123.2(5) yes C25 . N29 . C39 . 125.9(4) yes N26 . C30 . C31 . 118.4(5) yes N26 . C30 . C35 . 119.1(6) yes C31 . C30 . C35 . 122.5(6) yes C30 . C31 . C32 . 117.7(6) yes C30 . C31 . C36 . 121.4(6) yes C32 . C31 . C36 . 120.9(6) yes C31 . C32 . C33 . 122.5(6) yes C31 . C32 . H32 . 119.6 no C33 . C32 . H32 . 117.9 no C32 . C33 . C34 . 117.2(7) yes C32 . C33 . C37 . 122.0(9) yes C34 . C33 . C37 . 120.8(9) yes C33 . C34 . C35 . 122.9(8) yes C33 . C34 . H34 . 119.5 no C35 . C34 . H34 . 117.6 no C34 . C35 . C30 . 117.0(6) yes C34 . C35 . C38 . 121.6(7) yes C30 . C35 . C38 . 121.4(7) yes C31 . C36 . H362 . 110.2 no C31 . C36 . H361 . 108.9 no H362 . C36 . H361 . 109.6 no C31 . C36 . H363 . 108.9 no H362 . C36 . H363 . 110.4 no H361 . C36 . H363 . 108.9 no C33 . C37 . H372 . 109.3 no C33 . C37 . H371 . 110.6 no H372 . C37 . H371 . 110.0 no C33 . C37 . H373 . 110.3 no H372 . C37 . H373 . 107.8 no H371 . C37 . H373 . 108.8 no C35 . C38 . H381 . 109.2 no C35 . C38 . H382 . 109.7 no H381 . C38 . H382 . 108.7 no C35 . C38 . H383 . 110.8 no H381 . C38 . H383 . 109.4 no H382 . C38 . H383 . 109.0 no N29 . C39 . C40 . 117.0(6) yes N29 . C39 . C44 . 120.6(5) yes C40 . C39 . C44 . 122.4(6) yes C39 . C40 . C41 . 117.0(6) yes C39 . C40 . C45 . 121.8(6) yes C41 . C40 . C45 . 121.2(6) yes C40 . C41 . C42 . 121.7(6) yes C40 . C41 . H41 . 119.2 no C42 . C41 . H41 . 119.1 no C41 . C42 . C43 . 118.9(7) yes C41 . C42 . C46 . 119.1(9) yes C43 . C42 . C46 . 122.0(9) yes C42 . C43 . C44 . 122.5(8) yes C42 . C43 . H43 . 118.5 no C44 . C43 . H43 . 119.0 no C39 . C44 . C43 . 117.5(7) yes C39 . C44 . C47 . 121.4(6) yes C43 . C44 . C47 . 121.0(6) yes C40 . C45 . H453 . 109.8 no C40 . C45 . H452 . 108.7 no H453 . C45 . H452 . 109.6 no C40 . C45 . H451 . 109.0 no H453 . C45 . H451 . 109.3 no H452 . C45 . H451 . 110.3 no C42 . C46 . H461 . 108.3 no C42 . C46 . H463 . 110.7 no H461 . C46 . H463 . 109.9 no C42 . C46 . H462 . 109.8 no H461 . C46 . H462 . 108.5 no H463 . C46 . H462 . 109.6 no C44 . C47 . H471 . 110.5 no C44 . C47 . H472 . 108.9 no H471 . C47 . H472 . 108.6 no C44 . C47 . H473 . 110.5 no H471 . C47 . H473 . 108.0 no H472 . C47 . H473 . 110.3 no Ir1 . B48 . N49 . 171.5(6) yes Ir1 . B48 . H482 . 52.3 no N49 . B48 . H482 . 129.4 no Ir1 . B48 . H481 . 52.0 no N49 . B48 . H481 . 125.6 no H482 . B48 . H481 . 104.2 no B48 . N49 . C50 . 121.0(7) yes B48 . N49 . C51 . 124.1(7) yes C50 . N49 . C51 . 114.3(6) yes N49 . C50 . H502 . 109.6 no N49 . C50 . H501 . 109.3 no H502 . C50 . H501 . 109.5 no N49 . C50 . H503 . 108.9 no H502 . C50 . H503 . 110.1 no H501 . C50 . H503 . 109.4 no N49 . C51 . H511 . 109.9 no N49 . C51 . H512 . 111.3 no H511 . C51 . H512 . 108.8 no N49 . C51 . H513 . 109.6 no H511 . C51 . H513 . 108.7 no H512 . C51 . H513 . 108.4 no C61 . B60 . C75 . 115.9(9) yes C61 . B60 . C89 . 114.5(9) yes C75 . B60 . C89 . 104.5(3) yes C61 . B60 . C103 . 104.4(3) yes C75 . B60 . C103 . 109.7(9) yes C89 . B60 . C103 . 107.6(8) yes B60 . C61 . C62 . 118.6(7) yes B60 . C61 . C66 . 122.4(7) yes C62 . C61 . C66 . 119.0(8) yes C61 . C62 . C63 . 118.7(7) yes C61 . C62 . H62 . 120.1 no C63 . C62 . H62 . 121.2 no C62 . C63 . C64 . 123.7(6) yes C62 . C63 . C67 . 115.0(5) yes C64 . C63 . C67 . 121.3(5) yes C63 . C64 . C65 . 118.9(7) yes C63 . C64 . H64 . 119.8 no C65 . C64 . H64 . 121.2 no C64 . C65 . C66 . 120.8(8) yes C64 . C65 . C71 . 121.4(8) yes C66 . C65 . C71 . 117.8(8) yes C65 . C66 . C61 . 118.8(8) yes C65 . C66 . H66 . 120.0 no C61 . C66 . H66 . 121.2 no C63 . C67 . F68 . 113.74(5) yes C63 . C67 . F69 . 113.69(5) yes F68 . C67 . F69 . 104.94(5) yes C63 . C67 . F70 . 113.73(5) yes F68 . C67 . F70 . 104.91(5) yes F69 . C67 . F70 . 104.88(5) yes C63 . C67 . F681 . 113.73(5) yes C63 . C67 . F691 . 113.73(5) yes F681 . C67 . F691 . 104.94(5) yes C63 . C67 . F701 . 113.69(5) yes F681 . C67 . F701 . 104.88(5) yes F691 . C67 . F701 . 104.90(5) yes C65 . C71 . F72 . 115.2(7) yes C65 . C71 . F73 . 113.6(8) yes F72 . C71 . F73 . 107.5(10) yes C65 . C71 . F74 . 110.7(9) yes F72 . C71 . F74 . 104.4(8) yes F73 . C71 . F74 . 104.6(8) yes B60 . C75 . C76 . 125.2(9) yes B60 . C75 . C80 . 119.9(9) yes C76 . C75 . C80 . 114.7(8) yes C75 . C76 . C77 . 123.5(9) yes C75 . C76 . H76 . 118.5 no C77 . C76 . H76 . 118.0 no C76 . C77 . C78 . 121.9(7) yes C76 . C77 . C81 . 119.1(6) yes C78 . C77 . C81 . 119.0(6) yes C77 . C78 . C79 . 117.8(7) yes C77 . C78 . H78 . 122.2 no C79 . C78 . H78 . 120.0 no C78 . C79 . C80 . 122.1(7) yes C78 . C79 . C85 . 119.4(7) yes C80 . C79 . C85 . 118.5(7) yes C75 . C80 . C79 . 119.8(8) yes C75 . C80 . H80 . 119.8 no C79 . C80 . H80 . 120.4 no C77 . C81 . F82 . 115.4(5) yes C77 . C81 . F83 . 108.9(6) yes F82 . C81 . F83 . 106.5(8) yes C77 . C81 . F84 . 112.5(5) yes F82 . C81 . F84 . 111.9(7) yes F83 . C81 . F84 . 100.5(6) yes C79 . C85 . F86 . 116.5(7) yes C79 . C85 . F87 . 112.8(6) yes F86 . C85 . F87 . 109.2(8) yes C79 . C85 . F88 . 110.7(7) yes F86 . C85 . F88 . 107.9(8) yes F87 . C85 . F88 . 98.0(7) yes B60 . C89 . C90 . 116.3(9) yes B60 . C89 . C94 . 126.5(9) yes C90 . C89 . C94 . 116.9(9) yes C89 . C90 . C91 . 120.9(9) yes C89 . C90 . H90 . 120.8 no C91 . C90 . H90 . 118.3 no C90 . C91 . C92 . 120.6(7) yes C90 . C91 . C95 . 119.0(6) yes C92 . C91 . C95 . 120.4(5) yes C91 . C92 . C93 . 118.4(6) yes C91 . C92 . H92 . 120.2 no C93 . C92 . H92 . 121.4 no C92 . C93 . C94 . 119.2(7) yes C92 . C93 . C99 . 119.1(6) yes C94 . C93 . C99 . 121.6(7) yes C93 . C94 . C89 . 123.8(9) yes C93 . C94 . H94 . 116.4 no C89 . C94 . H94 . 119.8 no C91 . C95 . F96 . 113.75(5) yes C91 . C95 . F97 . 113.76(5) yes F96 . C95 . F97 . 104.90(5) yes C91 . C95 . F98 . 113.68(5) yes F96 . C95 . F98 . 104.87(5) yes F97 . C95 . F98 . 104.91(5) yes C91 . C95 . F961 . 113.68(5) yes C91 . C95 . F971 . 113.74(5) yes F961 . C95 . F971 . 104.88(5) yes C91 . C95 . F981 . 113.75(5) yes F961 . C95 . F981 . 104.91(5) yes F971 . C95 . F981 . 104.93(5) yes C93 . C99 . F100 . 111.8(6) yes C93 . C99 . F101 . 110.2(7) yes F100 . C99 . F101 . 109.7(7) yes C93 . C99 . F102 . 111.6(6) yes F100 . C99 . F102 . 107.2(8) yes F101 . C99 . F102 . 106.3(7) yes B60 . C103 . C104 . 119.2(7) yes B60 . C103 . C108 . 128.1(8) yes C104 . C103 . C108 . 112.3(8) yes C103 . C104 . C105 . 124.1(7) yes C103 . C104 . H104 . 117.8 no C105 . C104 . H104 . 118.0 no C104 . C105 . C106 . 119.2(6) yes C104 . C105 . C109 . 120.4(5) yes C106 . C105 . C109 . 120.3(5) yes C105 . C106 . C107 . 117.5(8) yes C105 . C106 . H106 . 122.3 no C107 . C106 . H106 . 120.2 no C106 . C107 . C108 . 119.2(9) yes C106 . C107 . C113 . 119.5(9) yes C108 . C107 . C113 . 121.2(9) yes C103 . C108 . C107 . 127.2(9) yes C103 . C108 . H108 . 117.5 no C107 . C108 . H108 . 115.2 no C105 . C109 . F110 . 113.73(5) yes C105 . C109 . F111 . 113.70(5) yes F110 . C109 . F111 . 104.94(5) yes C105 . C109 . F112 . 113.70(5) yes F110 . C109 . F112 . 104.94(5) yes F111 . C109 . F112 . 104.89(5) yes C105 . C109 . F1101 . 113.71(5) yes C105 . C109 . F1111 . 113.75(5) yes F1101 . C109 . F1111 . 104.90(5) yes C105 . C109 . F1121 . 113.73(5) yes F1101 . C109 . F1121 . 104.87(5) yes F1111 . C109 . F1121 . 104.91(5) yes C107 . C113 . F114 . 112.7(9) yes C107 . C113 . F115 . 115.9(10) yes F114 . C113 . F115 . 108.4(9) yes C107 . C113 . F116 . 112.3(8) yes F114 . C113 . F116 . 101.6(9) yes F115 . C113 . F116 . 104.8(9) yes Ir1 . H482 . B48 . 84.6 no Ir1 . H481 . B48 . 84.8 no data_2-Neutron _database_code_depnum_ccdc_archive 'CCDC 880792' #TrackingRef 'CrystallographicData.cif' #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; . ; _chemical_name_common . _chemical_melting_point 'not measured' _chemical_formula_moiety 'C44 H58 B Ir N5, C32 H12 B F24' _chemical_formula_sum 'C76 H70 B2 F24 Ir N5' _chemical_formula_weight 1723.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0000 -0.2130 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_space_group_name_Hall 'C -2yc' 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' _cell_length_a 22.8105(2) _cell_length_b 19.0153(2) _cell_length_c 19.9792(2) _cell_angle_alpha 90.00 _cell_angle_beta 117.11(10) _cell_angle_gamma 90.00 _cell_volume 7714(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used . _cell_measurement_theta_min . _cell_measurement_theta_max . _exptl_crystal_description block _exptl_crystal_colour clear_intense_yellow _exptl_crystal_size_max 9.00 _exptl_crystal_size_mid 4.00 _exptl_crystal_size_min 4.00 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1788 _exptl_absorpt_coefficient_mu 0.165 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3183 _exptl_absorpt_correction_T_max 0.5583 _exptl_absorpt_process_details ; Calculated using custom ISIS software program SXD-2001. ; _exptl_special_details ; For peak integration a local UB matrix refined for each frame, using approximately 100 reflections per run from each of the 11 detectors. For final cell dimensions a weighted average of all local cells was calculated. Because of the nature of the experiment, it is not possible to give values of theta_min and theta_max for the cell determination. The same applies for the wavelength used for the experiment. The range of wavelengths used was 0.48-7.0 Angstroms, but the bulk of the diffraction information is obtained from wavelengths in the range 0.7-2.5 Angstroms. The data collection procedures on the SXD instrument used for the single crystal neutron data collection are most recently summarised in the Appendix to the following paper Wilson, C.C. (1997). J. Mol. Struct. 405, 207-217 ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength Laue _diffrn_radiation_type Neutron _diffrn_radiation_source 'ISIS spallation neutron source' _diffrn_radiation_monochromator none _diffrn_measurement_device_type 'SXD at ISIS neutron source' _diffrn_measurement_method 'time-of-flight Laue diffraction' _diffrn_detector_area_resol_mean . _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7931 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 8.90 _diffrn_reflns_theta_max 82.53 _reflns_number_total 7931 _reflns_number_gt 7931 _reflns_threshold_expression >2sigma(I) _computing_data_collection SXD2001 _computing_cell_refinement SXD2001 _computing_data_reduction SXD2001 _computing_structure_solution 'Refinement of known model' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics . _computing_publication_material . _refine_special_details ; Refining hydrogen atoms using isotropic displacement parameters leads to a poor data to parameter ratio. The nature of the sample, time constraints and other experimental considerations meant it was not possible to collect more data, so extensive restraints were used. Thermal similarity and vibrational restraints were used to maintain sensible displacement ellipsoids; same distance restraints were also used to maintain sensible geometries for the methyl groups and trifluoromethyl groups . 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. The variable wavelength nature of the data collection procedure means that sensible values of _diffrn_reflns_theta_min & _diffrn_reflns_theta_max cannot be given. _refine_diff_density_max/min is given in Fermi per per angstrom cubed not electons per angstrom cubed. Another way to consider the _refine_diff_density_ is as a percentage of the diffracted intensity of a given atom: _refine_diff_density_max = 12% of Carbon _refine_diff_density_min = -12% of Carbon ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Refinement of known model' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000472(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.22(17) _refine_ls_number_reflns 7931 _refine_ls_number_parameters 1638 _refine_ls_number_restraints 3975 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0921 _refine_ls_wR_factor_ref 0.2330 _refine_ls_wR_factor_gt 0.2330 _refine_ls_goodness_of_fit_ref 1.274 _refine_ls_restrained_S_all 1.171 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.6209(2) 0.5776(2) 0.4973(3) 0.0207(9) Uani 1 1 d U . . C2 C 0.6239(4) 0.6852(4) 0.5042(5) 0.0265(12) Uani 1 1 d U . . N3 N 0.6535(3) 0.7256(3) 0.5669(3) 0.0295(11) Uani 1 1 d U . . C4 C 0.6495(5) 0.7978(5) 0.5498(5) 0.0351(15) Uani 1 1 d U . . C5 C 0.6164(4) 0.8012(4) 0.4739(5) 0.0352(15) Uani 1 1 d U . . N6 N 0.6016(3) 0.7326(3) 0.4461(3) 0.0320(12) Uani 1 1 d U . . C7 C 0.6843(4) 0.6994(5) 0.6421(5) 0.0340(17) Uani 1 1 d U . . C8 C 0.6439(5) 0.6898(5) 0.6780(5) 0.0410(18) Uani 1 1 d U . . C9 C 0.6741(6) 0.6666(6) 0.7523(6) 0.056(2) Uani 1 1 d U . . C10 C 0.7415(6) 0.6531(6) 0.7887(5) 0.057(2) Uani 1 1 d U . . C11 C 0.7816(6) 0.6638(6) 0.7531(6) 0.054(2) Uani 1 1 d U . . C12 C 0.7521(4) 0.6864(5) 0.6767(5) 0.0409(19) Uani 1 1 d U . . C13 C 0.5709(5) 0.7060(6) 0.6420(6) 0.055(3) Uani 1 1 d DU . . C14 C 0.7738(7) 0.6242(7) 0.8710(7) 0.094(4) Uani 1 1 d DU . . C15 C 0.7922(4) 0.6960(5) 0.6365(6) 0.055(2) Uani 1 1 d DU . . C16 C 0.5695(4) 0.7161(4) 0.3688(5) 0.0305(16) Uani 1 1 d U . . C17 C 0.6098(5) 0.7016(5) 0.3327(5) 0.0350(17) Uani 1 1 d U . . C18 C 0.5779(6) 0.6869(5) 0.2547(5) 0.049(2) Uani 1 1 d U . . C19 C 0.5094(6) 0.6857(6) 0.2150(6) 0.065(3) Uani 1 1 d U . . C20 C 0.4724(6) 0.7000(6) 0.2508(6) 0.064(2) Uani 1 1 d U . . C21 C 0.5014(5) 0.7154(5) 0.3297(6) 0.049(2) Uani 1 1 d U . . C22 C 0.6826(4) 0.7033(5) 0.3748(5) 0.041(2) Uani 1 1 d DU . . C23 C 0.4741(7) 0.6718(7) 0.1310(6) 0.098(4) Uani 1 1 d DU . . C24 C 0.4610(5) 0.7354(6) 0.3680(7) 0.076(3) Uani 1 1 d DU . . C25 C 0.6357(4) 0.4718(4) 0.4910(4) 0.0219(13) Uani 1 1 d U . . N26 N 0.6884(3) 0.4340(3) 0.5405(3) 0.0288(11) Uani 1 1 d U . . C27 C 0.6857(4) 0.3655(5) 0.5165(5) 0.0376(16) Uani 1 1 d U . . C28 C 0.6294(4) 0.3591(4) 0.4495(5) 0.0361(16) Uani 1 1 d U . . N29 N 0.5997(3) 0.4248(3) 0.4340(3) 0.0277(11) Uani 1 1 d U . . C30 C 0.7405(4) 0.4580(4) 0.6101(4) 0.0276(15) Uani 1 1 d U . . C31 C 0.7993(4) 0.4822(5) 0.6124(5) 0.0376(18) Uani 1 1 d U . . C32 C 0.8517(5) 0.5000(6) 0.6827(5) 0.0433(19) Uani 1 1 d U . . C33 C 0.8448(4) 0.4928(6) 0.7479(5) 0.043(2) Uani 1 1 d U . . C34 C 0.7863(4) 0.4692(5) 0.7453(5) 0.0396(18) Uani 1 1 d U . . C35 C 0.7322(4) 0.4523(5) 0.6747(5) 0.0330(17) Uani 1 1 d U . . C36 C 0.8066(4) 0.4900(6) 0.5415(5) 0.060(3) Uani 1 1 d DU . . C37 C 0.9032(5) 0.5103(6) 0.8253(5) 0.059(3) Uani 1 1 d DU . . C38 C 0.6677(4) 0.4266(5) 0.6713(5) 0.045(2) Uani 1 1 d DU . . C39 C 0.5374(4) 0.4398(4) 0.3690(4) 0.0283(15) Uani 1 1 d U . . C40 C 0.4799(4) 0.4163(4) 0.3704(5) 0.0329(17) Uani 1 1 d U . . C41 C 0.4191(5) 0.4312(5) 0.3066(5) 0.0419(18) Uani 1 1 d U . . C42 C 0.4171(4) 0.4663(5) 0.2463(5) 0.043(2) Uani 1 1 d U . . C43 C 0.4763(5) 0.4873(5) 0.2470(6) 0.0425(19) Uani 1 1 d U . . H43 H 0.4726(9) 0.5146(11) 0.2002(11) 0.053(4) Uani 1 1 d U . . C44 C 0.5382(4) 0.4747(5) 0.3094(4) 0.0314(16) Uani 1 1 d U . . C45 C 0.4809(4) 0.3784(5) 0.4377(6) 0.052(2) Uani 1 1 d DU . . C46 C 0.3523(5) 0.4829(7) 0.1794(6) 0.074(3) Uani 1 1 d DU . . C47 C 0.6004(4) 0.4971(5) 0.3065(5) 0.045(2) Uani 1 1 d DU . . B48 B 0.5285(5) 0.5702(7) 0.4892(6) 0.041(2) Uani 1 1 d U . . N49 N 0.4693(3) 0.5542(4) 0.4887(4) 0.0501(17) Uani 1 1 d U . . C50 C 0.4636(7) 0.5390(9) 0.5568(8) 0.061(3) Uani 1 1 d U . . C51 C 0.4056(5) 0.5616(8) 0.4203(8) 0.059(3) Uani 1 1 d U . . B60 B 0.1235(5) 0.5524(4) 0.5033(6) 0.0186(13) Uani 1 1 d U . . C61 C 0.1402(3) 0.5018(4) 0.4471(4) 0.0168(13) Uani 1 1 d U . . C62 C 0.2019(4) 0.4697(4) 0.4734(4) 0.0235(15) Uani 1 1 d U . . C63 C 0.2165(4) 0.4234(4) 0.4295(5) 0.0264(14) Uani 1 1 d U A . C64 C 0.1710(4) 0.4062(5) 0.3570(5) 0.0273(16) Uani 1 1 d U . . C65 C 0.1087(3) 0.4370(4) 0.3300(4) 0.0223(14) Uani 1 1 d U . . C66 C 0.0929(4) 0.4828(4) 0.3728(4) 0.0203(15) Uani 1 1 d U . . C67 C 0.2851(3) 0.3918(4) 0.4628(5) 0.0356(16) Uani 1 1 d DU . . F68 F 0.2887(11) 0.3280(8) 0.4884(15) 0.047(3) Uani 0.47(2) 1 d PDU A 1 F69 F 0.3070(11) 0.3867(14) 0.4113(10) 0.049(3) Uani 0.47(2) 1 d PDU A 1 F70 F 0.3306(11) 0.4293(12) 0.5175(12) 0.047(3) Uani 0.47(2) 1 d PDU A 1 F681 F 0.2970(11) 0.3519(12) 0.4175(10) 0.049(3) Uani 0.53(2) 1 d PDU A 2 F691 F 0.3293(10) 0.4416(9) 0.4879(13) 0.047(3) Uani 0.53(2) 1 d PDU A 2 F701 F 0.2936(10) 0.3534(11) 0.5210(10) 0.047(3) Uani 0.53(2) 1 d PDU A 2 C71 C 0.0535(4) 0.4188(4) 0.2510(4) 0.0312(17) Uani 1 1 d DU . . F72 F 0.0213(5) 0.4747(5) 0.2131(6) 0.048(3) Uani 1 1 d DU . . F73 F 0.0765(5) 0.3868(8) 0.2101(6) 0.077(4) Uani 1 1 d DU . . F74 F 0.0082(5) 0.3776(6) 0.2547(6) 0.059(3) Uani 1 1 d DU . . C75 C 0.1847(3) 0.6080(4) 0.5472(4) 0.0185(14) Uani 1 1 d U . . C76 C 0.1925(4) 0.6420(4) 0.6136(4) 0.0229(15) Uani 1 1 d U . . C77 C 0.2410(4) 0.6910(4) 0.6498(4) 0.0280(15) Uani 1 1 d U . . C78 C 0.2833(4) 0.7138(4) 0.6224(5) 0.0268(15) Uani 1 1 d U . . C79 C 0.2757(4) 0.6833(4) 0.5550(5) 0.0287(15) Uani 1 1 d U . . C80 C 0.2268(4) 0.6315(4) 0.5176(4) 0.0228(14) Uani 1 1 d U . . C81 C 0.2495(4) 0.7227(4) 0.7234(4) 0.0352(18) Uani 1 1 d DU . . F82 F 0.1967(6) 0.7187(8) 0.7320(8) 0.085(4) Uani 1 1 d DU . . F83 F 0.2961(7) 0.6895(7) 0.7815(7) 0.088(5) Uani 1 1 d DU . . F84 F 0.2688(7) 0.7892(5) 0.7340(8) 0.078(4) Uani 1 1 d DU . . C85 C 0.3197(4) 0.7075(5) 0.5242(5) 0.045(2) Uani 1 1 d DU . . F86 F 0.2997(7) 0.6896(8) 0.4548(6) 0.093(5) Uani 1 1 d DU . . F87 F 0.3271(6) 0.7770(5) 0.5265(8) 0.065(3) Uani 1 1 d DU . . F88 F 0.3814(5) 0.6844(8) 0.5630(9) 0.092(5) Uani 1 1 d DU . . C89 C 0.0582(3) 0.6022(4) 0.4570(4) 0.0228(15) Uani 1 1 d U . . C90 C 0.0484(4) 0.6376(4) 0.3916(4) 0.0256(15) Uani 1 1 d U . . C91 C -0.0048(4) 0.6805(5) 0.3537(5) 0.0370(16) Uani 1 1 d U B . C92 C -0.0529(4) 0.6911(5) 0.3780(5) 0.0388(18) Uani 1 1 d U . . C93 C -0.0437(4) 0.6574(5) 0.4430(5) 0.0348(17) Uani 1 1 d U . . C94 C 0.0114(4) 0.6148(5) 0.4829(4) 0.0284(16) Uani 1 1 d U . . C95 C -0.0158(4) 0.7149(5) 0.2817(5) 0.0473(18) Uani 1 1 d DU . . F96 F 0.0327(7) 0.7044(11) 0.2645(10) 0.054(3) Uani 0.599(12) 1 d PDU B 1 F97 F -0.0289(11) 0.7815(7) 0.2790(11) 0.063(3) Uani 0.599(12) 1 d PDU B 1 F98 F -0.0681(7) 0.6864(10) 0.2239(9) 0.056(3) Uani 0.599(12) 1 d PDU B 1 F961 F 0.0350(10) 0.7582(13) 0.2964(14) 0.056(3) Uani 0.401(12) 1 d PDU B 2 F971 F -0.0676(9) 0.7551(13) 0.2495(14) 0.054(3) Uani 0.401(12) 1 d PDU B 2 F981 F -0.0154(15) 0.6703(11) 0.2330(13) 0.063(3) Uani 0.401(12) 1 d PDU B 2 C99 C -0.0952(4) 0.6651(5) 0.4698(5) 0.052(2) Uani 1 1 d DU . . F100 F -0.1438(6) 0.6202(8) 0.4372(9) 0.097(5) Uani 1 1 d DU . . F101 F -0.1224(7) 0.7285(6) 0.4562(9) 0.086(4) Uani 1 1 d DU . . F102 F -0.0721(6) 0.6556(8) 0.5426(6) 0.075(4) Uani 1 1 d DU . . C103 C 0.1153(3) 0.4997(4) 0.5619(4) 0.0189(14) Uani 1 1 d U . . C104 C 0.0543(4) 0.4631(4) 0.5368(4) 0.0200(15) Uani 1 1 d U . . C105 C 0.0414(4) 0.4172(4) 0.5833(4) 0.0274(14) Uani 1 1 d U C . C106 C 0.0904(4) 0.4062(4) 0.6571(4) 0.0252(15) Uani 1 1 d U . . C107 C 0.1511(4) 0.4364(4) 0.6809(4) 0.0266(16) Uani 1 1 d U . . C108 C 0.1630(3) 0.4839(4) 0.6338(4) 0.0183(14) Uani 1 1 d U . . C109 C -0.0255(4) 0.3852(4) 0.5547(4) 0.0372(16) Uani 1 1 d DU . . F110 F -0.0372(7) 0.3572(9) 0.6063(7) 0.051(3) Uani 0.724(14) 1 d PDU C 1 F111 F -0.0729(6) 0.4302(7) 0.5168(8) 0.043(3) Uani 0.724(14) 1 d PDU C 1 F112 F -0.0307(7) 0.3350(8) 0.5063(8) 0.052(3) Uani 0.724(14) 1 d PDU C 1 F10A F -0.0564(17) 0.403(2) 0.5939(18) 0.052(3) Uani 0.276(14) 1 d PDU C 2 F11A F -0.0658(16) 0.4028(19) 0.4844(11) 0.051(3) Uani 0.276(14) 1 d PDU C 2 F12A F -0.0241(16) 0.3161(8) 0.555(2) 0.043(3) Uani 0.276(14) 1 d PDU C 2 C113 C 0.2062(4) 0.4209(5) 0.7578(4) 0.043(2) Uani 1 1 d DU . . F114 F 0.1850(6) 0.3996(8) 0.8054(6) 0.079(4) Uani 1 1 d DU . . F115 F 0.2440(6) 0.3707(7) 0.7548(7) 0.088(5) Uani 1 1 d DU . . F116 F 0.2453(6) 0.4752(6) 0.7903(7) 0.070(4) Uani 1 1 d DU . . H1 H 0.6576(7) 0.5869(9) 0.4465(9) 0.037(3) Uani 1 1 d U . . H2 H 0.6960(7) 0.5791(8) 0.5604(10) 0.038(3) Uani 1 1 d U . . H4 H 0.6668(9) 0.8366(9) 0.5905(10) 0.048(3) Uani 1 1 d U . . H5 H 0.6051(9) 0.8480(9) 0.4392(10) 0.044(3) Uani 1 1 d U . . H9 H 0.6476(13) 0.6600(12) 0.7824(13) 0.070(5) Uani 1 1 d U . . H11 H 0.8349(11) 0.6529(12) 0.7830(10) 0.068(5) Uani 1 1 d U . . H18 H 0.6044(13) 0.6807(12) 0.2287(12) 0.067(5) Uani 1 1 d U . . H20 H 0.4175(13) 0.7015(13) 0.2250(13) 0.086(6) Uani 1 1 d U . . H27 H 0.7251(9) 0.3278(9) 0.5477(10) 0.048(3) Uani 1 1 d U . . H28 H 0.6078(9) 0.3153(9) 0.4117(10) 0.047(3) Uani 1 1 d U . . H32 H 0.8955(10) 0.5183(13) 0.6848(12) 0.066(4) Uani 1 1 d U . . H34 H 0.7819(9) 0.4640(11) 0.7963(11) 0.053(4) Uani 1 1 d U . . H41 H 0.3735(10) 0.4158(12) 0.3067(12) 0.063(4) Uani 1 1 d U . . H62 H 0.2391(8) 0.4800(9) 0.5318(9) 0.040(4) Uani 1 1 d U . . H64 H 0.1835(8) 0.3713(10) 0.3234(10) 0.040(3) Uani 1 1 d U . . H66 H 0.0405(7) 0.5049(8) 0.3470(8) 0.031(3) Uani 1 1 d U . . H76 H 0.1614(8) 0.6308(8) 0.6395(8) 0.029(3) Uani 1 1 d U . . H78 H 0.3201(8) 0.7529(9) 0.6497(10) 0.043(4) Uani 1 1 d U . . H80 H 0.2208(8) 0.6096(9) 0.4658(9) 0.037(3) Uani 1 1 d U . . H90 H 0.0843(9) 0.6288(10) 0.3724(10) 0.045(4) Uani 1 1 d U . . H92 H -0.0956(8) 0.7237(9) 0.3436(10) 0.049(4) Uani 1 1 d U . . H94 H 0.0160(8) 0.5885(9) 0.5353(8) 0.036(3) Uani 1 1 d U . . H104 H 0.0151(7) 0.4712(8) 0.4798(8) 0.030(3) Uani 1 1 d U . . H106 H 0.0810(8) 0.3699(10) 0.6927(10) 0.045(4) Uani 1 1 d U . . H108 H 0.2118(7) 0.5102(8) 0.6537(8) 0.034(3) Uani 1 1 d U . . H131 H 0.5458(12) 0.6884(13) 0.6722(13) 0.106(6) Uani 1 1 d DU . . H132 H 0.5575(12) 0.7594(8) 0.6299(14) 0.105(6) Uani 1 1 d DU . . H133 H 0.5456(11) 0.6799(12) 0.5892(10) 0.098(6) Uani 1 1 d DU . . H141 H 0.8185(10) 0.6486(15) 0.9054(13) 0.123(6) Uani 1 1 d DU . . H142 H 0.7425(12) 0.6324(16) 0.8955(13) 0.120(6) Uani 1 1 d DU . . H143 H 0.7817(15) 0.5707(9) 0.8705(14) 0.127(6) Uani 1 1 d DU . . H151 H 0.8416(7) 0.6824(11) 0.6722(11) 0.083(5) Uani 1 1 d DU . . H152 H 0.7930(10) 0.7478(8) 0.6192(13) 0.085(5) Uani 1 1 d DU . . H153 H 0.7769(10) 0.6641(11) 0.5881(10) 0.081(5) Uani 1 1 d DU . . H221 H 0.7047(11) 0.7102(13) 0.3397(11) 0.087(5) Uani 1 1 d DU . . H222 H 0.7027(12) 0.7427(12) 0.4168(11) 0.094(6) Uani 1 1 d DU . . H223 H 0.7033(13) 0.6560(10) 0.4051(14) 0.117(12) Uani 1 1 d D . . H231 H 0.4226(9) 0.6817(17) 0.1046(15) 0.143(7) Uani 1 1 d DU . . H232 H 0.4911(15) 0.7061(16) 0.1009(14) 0.142(7) Uani 1 1 d DU . . H233 H 0.4791(15) 0.6207(11) 0.1135(14) 0.144(7) Uani 1 1 d DU . . H241 H 0.4117(7) 0.7216(12) 0.3347(12) 0.095(5) Uani 1 1 d DU . . H242 H 0.4615(11) 0.7891(8) 0.3808(14) 0.099(5) Uani 1 1 d DU . . H243 H 0.4768(10) 0.7092(12) 0.4202(10) 0.091(5) Uani 1 1 d DU . . H361 H 0.8518(7) 0.5139(12) 0.5532(12) 0.090(5) Uani 1 1 d DU . . H362 H 0.7696(8) 0.5218(12) 0.5020(12) 0.091(5) Uani 1 1 d DU . . H363 H 0.8053(11) 0.4409(9) 0.5181(12) 0.086(5) Uani 1 1 d DU . . H371 H 0.9281(11) 0.5561(10) 0.8250(13) 0.103(6) Uani 1 1 d DU . . H372 H 0.8896(11) 0.5161(14) 0.8687(11) 0.100(6) Uani 1 1 d DU . . H373 H 0.9374(10) 0.4689(10) 0.8410(12) 0.098(6) Uani 1 1 d DU . . H381 H 0.6725(10) 0.4159(11) 0.7252(7) 0.078(4) Uani 1 1 d DU . . H382 H 0.6287(9) 0.4621(9) 0.6452(11) 0.077(4) Uani 1 1 d DU . . H383 H 0.6537(10) 0.3794(8) 0.6410(11) 0.076(4) Uani 1 1 d DU . . H451 H 0.4350(7) 0.3739(11) 0.4353(12) 0.071(4) Uani 1 1 d DU . . H452 H 0.5136(8) 0.4026(10) 0.4883(9) 0.070(4) Uani 1 1 d DU . . H453 H 0.5001(9) 0.3277(8) 0.4394(12) 0.071(4) Uani 1 1 d DU . . H461 H 0.3172(10) 0.4426(12) 0.1705(14) 0.116(6) Uani 1 1 d DU . . H462 H 0.3305(11) 0.5293(11) 0.1848(14) 0.119(7) Uani 1 1 d DU . . H463 H 0.3553(11) 0.4864(16) 0.1285(9) 0.119(7) Uani 1 1 d DU . . H471 H 0.5949(11) 0.4917(12) 0.2515(8) 0.086(5) Uani 1 1 d DU . . H472 H 0.6141(11) 0.5484(8) 0.3240(12) 0.087(5) Uani 1 1 d DU . . H473 H 0.6417(8) 0.4650(10) 0.3390(11) 0.082(4) Uani 1 1 d DU . . H481 H 0.5313(7) 0.5782(10) 0.4260(9) 0.045(4) Uani 1 1 d U . . H482 H 0.5840(8) 0.5653(10) 0.5604(10) 0.049(4) Uani 1 1 d U . . H503 H 0.4383(14) 0.5771(17) 0.5661(15) 0.088(6) Uani 1 1 d U . . H502 H 0.5110(14) 0.5383(16) 0.6035(16) 0.086(5) Uani 1 1 d U . . H501 H 0.4403(14) 0.4880(17) 0.5528(15) 0.092(7) Uani 1 1 d U . . H511 H 0.3805(11) 0.5092(16) 0.4164(16) 0.089(7) Uani 1 1 d U . . H512 H 0.3810(12) 0.6047(17) 0.4273(15) 0.087(7) Uani 1 1 d U . . H513 H 0.4124(11) 0.5699(14) 0.3706(15) 0.075(6) Uani 1 1 d U . . 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 0.026(2) 0.0126(17) 0.024(2) -0.0019(17) 0.0128(18) -0.0028(18) C2 0.043(3) 0.012(2) 0.027(2) 0.001(2) 0.019(2) 0.003(3) N3 0.049(3) 0.012(2) 0.029(2) -0.0025(17) 0.019(2) 0.001(2) C4 0.056(3) 0.013(2) 0.038(3) 0.003(2) 0.023(3) -0.001(3) C5 0.055(3) 0.012(2) 0.040(3) 0.003(2) 0.023(3) 0.001(3) N6 0.049(3) 0.013(2) 0.034(2) 0.0021(18) 0.019(2) 0.005(2) C7 0.048(3) 0.015(4) 0.026(3) -0.008(3) 0.007(3) -0.005(3) C8 0.063(4) 0.026(4) 0.034(4) -0.005(3) 0.022(3) -0.002(3) C9 0.082(5) 0.039(5) 0.037(4) -0.007(4) 0.018(4) -0.002(4) C10 0.086(5) 0.044(5) 0.027(4) -0.007(4) 0.013(3) -0.004(4) C11 0.060(5) 0.044(5) 0.035(4) -0.007(4) 0.000(3) 0.000(4) C12 0.042(4) 0.027(5) 0.035(4) 0.005(3) 0.001(3) -0.003(3) C13 0.062(5) 0.048(7) 0.064(6) -0.010(5) 0.035(5) 0.001(5) C14 0.128(9) 0.103(10) 0.035(5) 0.017(6) 0.024(6) 0.027(7) C15 0.031(5) 0.059(7) 0.063(6) 0.003(5) 0.010(4) -0.010(4) C16 0.042(3) 0.015(4) 0.032(3) 0.004(3) 0.015(3) 0.002(3) C17 0.055(4) 0.019(4) 0.029(3) 0.003(3) 0.018(3) 0.005(3) C18 0.087(5) 0.027(5) 0.021(3) 0.003(3) 0.013(3) 0.007(4) C19 0.087(5) 0.042(5) 0.035(4) 0.002(4) 0.003(4) 0.011(5) C20 0.061(5) 0.048(5) 0.047(4) 0.010(4) -0.007(3) 0.019(4) C21 0.044(4) 0.038(5) 0.051(4) 0.011(4) 0.008(3) 0.018(4) C22 0.053(4) 0.048(6) 0.038(5) 0.016(4) 0.033(4) -0.003(4) C23 0.122(9) 0.086(9) 0.030(5) -0.010(5) -0.013(5) 0.006(7) C24 0.042(6) 0.091(8) 0.080(6) 0.006(6) 0.016(5) 0.031(5) C25 0.031(3) 0.012(2) 0.022(3) -0.001(2) 0.012(2) 0.001(2) N26 0.035(2) 0.019(2) 0.030(2) 0.0015(18) 0.0123(18) 0.0067(18) C27 0.048(3) 0.015(3) 0.043(3) 0.000(2) 0.014(2) 0.012(2) C28 0.046(3) 0.011(3) 0.046(3) -0.002(2) 0.016(2) 0.006(2) N29 0.039(2) 0.010(2) 0.032(2) -0.0024(17) 0.0143(18) 0.0030(17) C30 0.024(3) 0.030(4) 0.030(3) 0.010(3) 0.013(3) 0.009(3) C31 0.031(4) 0.050(5) 0.036(3) 0.011(3) 0.018(3) 0.007(3) C32 0.030(4) 0.055(5) 0.042(4) 0.011(4) 0.014(3) 0.002(3) C33 0.032(4) 0.051(5) 0.035(4) 0.011(4) 0.006(3) 0.005(3) C34 0.040(4) 0.041(5) 0.032(4) 0.004(3) 0.011(3) 0.007(3) C35 0.034(4) 0.036(4) 0.033(3) 0.010(3) 0.018(3) 0.004(3) C36 0.038(5) 0.108(8) 0.049(5) 0.012(5) 0.034(4) 0.014(5) C37 0.039(5) 0.074(7) 0.040(5) 0.008(5) -0.004(4) 0.014(5) C38 0.040(4) 0.055(6) 0.054(5) 0.015(5) 0.034(4) -0.003(4) C39 0.035(3) 0.017(4) 0.035(3) -0.009(3) 0.018(3) -0.005(3) C40 0.040(3) 0.023(4) 0.041(4) -0.010(3) 0.022(3) -0.010(3) C41 0.036(4) 0.040(5) 0.046(4) -0.023(3) 0.015(3) -0.010(3) C42 0.036(4) 0.042(5) 0.041(4) -0.016(3) 0.009(3) -0.003(3) C43 0.037(4) 0.041(5) 0.039(4) -0.008(4) 0.008(3) 0.002(3) H43 0.048(8) 0.049(9) 0.043(7) 0.000(7) 0.005(6) -0.006(6) C44 0.033(4) 0.029(4) 0.029(3) -0.010(3) 0.012(3) -0.006(3) C45 0.061(6) 0.035(6) 0.074(6) 0.014(4) 0.043(5) -0.008(4) C46 0.038(5) 0.104(9) 0.050(6) -0.009(6) -0.005(4) -0.004(6) C47 0.051(5) 0.049(6) 0.043(5) -0.008(4) 0.029(4) -0.019(4) B48 0.025(4) 0.053(6) 0.050(5) -0.007(4) 0.021(4) -0.011(4) N49 0.033(3) 0.055(5) 0.067(4) 0.006(3) 0.027(3) -0.002(3) C50 0.047(6) 0.076(8) 0.078(6) 0.014(6) 0.045(5) -0.009(5) C51 0.019(4) 0.074(7) 0.080(6) -0.004(6) 0.021(4) -0.008(5) B60 0.021(3) 0.011(3) 0.021(3) 0.001(3) 0.008(2) 0.002(3) C61 0.021(3) 0.014(3) 0.020(3) 0.001(2) 0.014(2) 0.001(2) C62 0.019(3) 0.017(4) 0.030(4) 0.000(3) 0.007(3) 0.006(2) C63 0.020(3) 0.014(3) 0.042(3) -0.001(3) 0.012(2) 0.003(2) C64 0.029(3) 0.020(4) 0.032(3) -0.001(3) 0.012(3) 0.003(3) C65 0.023(3) 0.025(4) 0.019(3) 0.000(3) 0.010(2) 0.003(3) C66 0.024(3) 0.019(4) 0.016(3) -0.001(3) 0.008(2) 0.005(3) C67 0.023(3) 0.021(3) 0.057(4) -0.005(3) 0.014(3) 0.005(2) F68 0.033(6) 0.028(6) 0.065(6) 0.005(5) 0.010(6) 0.009(5) F69 0.031(6) 0.037(7) 0.076(6) -0.008(5) 0.022(5) 0.019(6) F70 0.023(4) 0.040(6) 0.064(7) -0.001(5) 0.008(6) -0.004(4) F681 0.031(6) 0.037(7) 0.076(6) -0.008(5) 0.022(5) 0.019(6) F691 0.023(4) 0.040(6) 0.064(7) -0.001(5) 0.008(6) -0.004(4) F701 0.033(6) 0.028(6) 0.065(6) 0.005(5) 0.010(6) 0.009(5) C71 0.031(4) 0.040(5) 0.020(3) 0.001(3) 0.009(3) 0.001(3) F72 0.059(7) 0.038(6) 0.028(5) 0.003(4) 0.003(4) 0.005(5) F73 0.056(7) 0.108(11) 0.039(6) -0.049(7) -0.002(5) 0.025(6) F74 0.061(7) 0.048(8) 0.034(6) -0.001(5) -0.007(5) -0.027(5) C75 0.025(3) 0.013(3) 0.018(3) -0.004(2) 0.010(2) -0.002(2) C76 0.031(4) 0.017(4) 0.022(3) -0.004(2) 0.014(3) 0.001(2) C77 0.040(4) 0.018(4) 0.026(3) -0.007(3) 0.015(3) -0.006(3) C78 0.029(3) 0.016(4) 0.034(3) -0.001(3) 0.012(3) -0.004(3) C79 0.027(3) 0.028(4) 0.038(3) -0.003(3) 0.021(3) -0.006(3) C80 0.029(3) 0.021(4) 0.022(3) -0.001(3) 0.015(3) -0.001(3) C81 0.059(5) 0.020(4) 0.030(4) -0.011(3) 0.023(3) -0.001(3) F82 0.086(8) 0.102(11) 0.093(9) -0.061(8) 0.065(7) -0.029(7) F83 0.129(10) 0.058(9) 0.041(6) -0.005(6) 0.007(7) 0.035(8) F84 0.142(11) 0.019(6) 0.082(9) -0.025(5) 0.058(8) -0.015(6) C85 0.043(4) 0.048(5) 0.058(5) -0.005(4) 0.034(4) -0.015(4) F86 0.112(10) 0.119(11) 0.072(7) -0.035(7) 0.063(6) -0.081(9) F87 0.066(8) 0.051(6) 0.105(9) 0.000(6) 0.062(7) -0.018(5) F88 0.042(6) 0.094(10) 0.145(11) 0.036(10) 0.047(7) 0.003(6) C89 0.024(3) 0.016(4) 0.024(3) -0.001(3) 0.007(3) 0.005(3) C90 0.036(4) 0.010(4) 0.026(3) 0.002(3) 0.010(3) 0.005(3) C91 0.045(4) 0.030(4) 0.025(3) 0.003(2) 0.007(3) 0.012(3) C92 0.037(4) 0.032(4) 0.035(4) 0.002(3) 0.006(3) 0.012(3) C93 0.032(3) 0.037(4) 0.035(3) 0.001(3) 0.015(3) 0.021(3) C94 0.024(3) 0.029(4) 0.023(3) 0.000(3) 0.003(3) 0.005(3) C95 0.058(4) 0.042(4) 0.032(3) 0.011(3) 0.013(3) 0.015(3) F96 0.057(5) 0.058(7) 0.038(6) 0.028(5) 0.014(5) 0.017(5) F97 0.101(8) 0.049(6) 0.031(5) 0.013(4) 0.023(6) 0.019(6) F98 0.060(6) 0.069(7) 0.031(5) 0.014(5) 0.014(5) 0.006(5) F961 0.060(6) 0.069(7) 0.031(5) 0.014(5) 0.014(5) 0.006(5) F971 0.057(5) 0.058(7) 0.038(6) 0.028(5) 0.014(5) 0.017(5) F981 0.101(8) 0.049(6) 0.031(5) 0.013(4) 0.023(6) 0.019(6) C99 0.043(4) 0.057(5) 0.062(5) -0.001(4) 0.030(4) 0.018(4) F100 0.055(8) 0.117(10) 0.131(10) -0.008(10) 0.053(7) -0.017(7) F101 0.083(9) 0.083(8) 0.116(10) 0.021(8) 0.066(8) 0.056(7) F102 0.079(8) 0.093(10) 0.081(7) 0.010(7) 0.059(6) 0.037(7) C103 0.022(3) 0.008(3) 0.020(3) -0.001(2) 0.005(3) 0.000(2) C104 0.021(3) 0.012(4) 0.023(3) 0.007(3) 0.008(3) 0.000(2) C105 0.024(3) 0.031(3) 0.031(3) 0.009(3) 0.016(2) 0.009(2) C106 0.033(3) 0.018(4) 0.025(3) 0.007(3) 0.014(3) 0.001(3) C107 0.023(3) 0.022(4) 0.026(3) 0.010(3) 0.004(3) 0.006(3) C108 0.019(3) 0.012(4) 0.017(3) 0.001(2) 0.003(2) 0.003(3) C109 0.026(3) 0.042(4) 0.044(3) 0.007(3) 0.015(3) 0.001(3) F110 0.037(5) 0.054(7) 0.051(5) 0.019(5) 0.010(4) -0.014(5) F111 0.024(5) 0.045(4) 0.052(6) 0.009(4) 0.011(5) 0.004(4) F112 0.030(5) 0.061(7) 0.067(6) -0.013(5) 0.025(5) -0.007(5) F10A 0.030(5) 0.061(7) 0.067(6) -0.013(5) 0.025(5) -0.007(5) F11A 0.037(5) 0.054(7) 0.051(5) 0.019(5) 0.010(4) -0.014(5) F12A 0.024(5) 0.045(4) 0.052(6) 0.009(4) 0.011(5) 0.004(4) C113 0.046(4) 0.041(5) 0.024(4) 0.006(3) 0.000(3) 0.008(3) F114 0.087(9) 0.101(11) 0.024(6) 0.035(6) 0.002(5) -0.009(7) F115 0.076(9) 0.076(9) 0.057(8) 0.002(7) -0.017(6) 0.053(7) F116 0.063(8) 0.060(8) 0.039(6) 0.004(5) -0.018(5) -0.006(5) H1 0.040(7) 0.036(7) 0.041(6) -0.003(6) 0.024(5) 0.006(5) H2 0.030(6) 0.022(7) 0.048(7) -0.003(6) 0.005(6) -0.005(5) H4 0.066(5) 0.017(5) 0.049(5) 0.003(5) 0.015(5) -0.001(4) H5 0.063(5) 0.014(5) 0.048(5) 0.007(5) 0.018(5) 0.004(4) H9 0.098(9) 0.050(9) 0.054(8) -0.001(7) 0.028(8) 0.004(8) H11 0.067(9) 0.057(9) 0.039(7) 0.010(7) -0.013(7) -0.001(7) H18 0.109(9) 0.036(9) 0.042(7) -0.002(7) 0.023(8) 0.007(8) H20 0.074(9) 0.067(9) 0.062(8) 0.004(8) -0.017(8) 0.005(8) H27 0.057(5) 0.020(5) 0.050(5) -0.003(5) 0.008(5) 0.010(5) H28 0.052(5) 0.019(5) 0.057(5) -0.008(5) 0.012(5) 0.006(4) H32 0.041(8) 0.080(10) 0.068(8) 0.015(8) 0.018(7) -0.005(7) H34 0.054(8) 0.047(9) 0.040(7) 0.003(6) 0.006(6) 0.009(7) H41 0.051(8) 0.061(9) 0.065(8) -0.021(7) 0.016(7) -0.012(7) H62 0.033(7) 0.036(8) 0.038(7) 0.005(6) 0.005(6) 0.014(6) H64 0.038(7) 0.035(8) 0.048(7) -0.003(6) 0.021(6) -0.005(6) H66 0.027(6) 0.021(7) 0.033(6) -0.004(5) 0.004(5) 0.016(5) H76 0.046(7) 0.025(7) 0.029(6) -0.009(5) 0.029(5) -0.009(5) H78 0.034(7) 0.030(8) 0.054(7) 0.003(6) 0.011(6) -0.004(6) H80 0.045(7) 0.040(7) 0.032(6) -0.005(6) 0.023(5) -0.004(6) H90 0.058(8) 0.029(8) 0.045(7) 0.002(6) 0.022(7) 0.006(6) H92 0.042(7) 0.031(8) 0.053(7) -0.008(6) 0.002(6) 0.016(6) H94 0.041(7) 0.042(8) 0.020(6) -0.001(5) 0.009(5) 0.008(6) H104 0.017(6) 0.025(7) 0.034(7) 0.001(5) -0.001(5) -0.006(5) H106 0.048(7) 0.035(8) 0.045(7) 0.013(6) 0.015(6) -0.008(6) H108 0.020(6) 0.030(7) 0.031(6) 0.008(5) -0.006(5) -0.004(5) H131 0.084(9) 0.093(11) 0.113(10) -0.009(9) 0.019(9) 0.016(8) H132 0.083(9) 0.087(10) 0.115(10) -0.015(9) 0.021(9) 0.023(8) H133 0.075(9) 0.087(10) 0.111(10) -0.024(9) 0.023(9) 0.028(8) H141 0.161(12) 0.127(13) 0.045(8) 0.026(8) 0.015(9) 0.030(10) H142 0.162(12) 0.128(13) 0.044(8) 0.030(8) 0.024(9) 0.027(10) H143 0.168(12) 0.126(12) 0.048(8) 0.025(8) 0.015(9) 0.030(10) H151 0.053(8) 0.098(10) 0.093(9) -0.005(8) 0.028(7) -0.007(7) H152 0.057(8) 0.095(10) 0.101(9) 0.002(8) 0.034(7) -0.011(7) H153 0.048(8) 0.097(10) 0.097(9) -0.005(8) 0.031(7) -0.025(7) H221 0.072(9) 0.116(12) 0.087(10) 0.005(10) 0.049(9) -0.001(9) H222 0.074(10) 0.112(12) 0.093(11) -0.009(10) 0.034(9) -0.001(9) H223 0.10(2) 0.10(3) 0.14(3) 0.07(2) 0.045(19) 0.015(16) H231 0.155(13) 0.136(13) 0.057(9) -0.002(10) -0.020(10) 0.009(11) H232 0.157(13) 0.133(12) 0.058(9) 0.002(10) -0.020(10) 0.004(11) H233 0.160(13) 0.131(12) 0.061(9) 0.000(10) -0.018(10) 0.009(11) H241 0.051(8) 0.119(11) 0.111(10) 0.010(9) 0.033(8) 0.022(8) H242 0.063(9) 0.117(11) 0.114(10) 0.009(9) 0.037(8) 0.020(8) H243 0.049(8) 0.118(11) 0.107(10) 0.010(9) 0.036(7) 0.022(8) H361 0.061(8) 0.142(12) 0.070(8) 0.014(9) 0.032(7) -0.001(8) H362 0.057(9) 0.142(13) 0.074(9) 0.016(10) 0.029(8) 0.005(9) H363 0.069(9) 0.137(12) 0.066(9) 0.012(9) 0.043(8) 0.001(9) H371 0.082(9) 0.106(11) 0.072(9) 0.002(8) -0.006(8) 0.003(9) H372 0.080(9) 0.110(11) 0.069(9) 0.000(8) -0.001(8) 0.005(9) H373 0.073(9) 0.105(11) 0.069(9) 0.002(8) -0.008(8) 0.006(9) H381 0.069(8) 0.088(9) 0.083(8) 0.006(8) 0.040(7) -0.020(7) H382 0.065(8) 0.087(9) 0.086(8) 0.014(8) 0.040(7) -0.017(8) H383 0.064(8) 0.083(9) 0.087(8) 0.002(8) 0.040(7) -0.022(7) H451 0.076(9) 0.063(10) 0.092(10) 0.010(8) 0.055(8) 0.002(8) H452 0.083(9) 0.059(10) 0.077(9) 0.001(8) 0.044(8) -0.011(8) H453 0.081(8) 0.055(9) 0.086(9) 0.006(7) 0.046(7) 0.003(7) H461 0.060(9) 0.133(12) 0.083(10) -0.011(9) -0.030(8) 0.000(9) H462 0.060(9) 0.134(12) 0.088(10) -0.013(9) -0.031(8) 0.013(9) H463 0.065(9) 0.140(12) 0.080(10) -0.008(9) -0.029(8) 0.002(9) H471 0.078(8) 0.102(10) 0.091(9) -0.005(8) 0.049(7) -0.029(8) H472 0.074(8) 0.089(10) 0.102(9) -0.008(8) 0.044(7) -0.030(8) H473 0.072(8) 0.096(10) 0.094(9) 0.007(8) 0.052(7) -0.024(8) H481 0.029(7) 0.060(9) 0.040(7) -0.011(6) 0.010(6) 0.001(6) H482 0.038(7) 0.061(9) 0.052(8) -0.018(7) 0.024(6) -0.009(6) H503 0.081(10) 0.100(12) 0.087(11) 0.007(10) 0.041(10) -0.006(10) H502 0.077(10) 0.100(12) 0.083(10) 0.021(9) 0.039(10) -0.005(9) H501 0.085(13) 0.102(16) 0.096(14) 0.008(12) 0.049(11) -0.021(13) H511 0.048(11) 0.093(15) 0.109(15) 0.003(12) 0.022(10) -0.028(11) H512 0.049(11) 0.102(15) 0.095(14) -0.037(12) 0.019(10) 0.004(11) H513 0.053(11) 0.078(14) 0.076(12) -0.021(11) 0.012(10) -0.007(10) _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 B48 2.044(11) . ? Ir1 C2 2.050(8) . ? Ir1 C25 2.054(9) . ? Ir1 H1 1.592(17) . ? Ir1 H2 1.599(15) . ? Ir1 H481 1.886(16) . ? Ir1 H482 1.822(19) . ? C2 N3 1.358(10) . ? C2 N6 1.372(10) . ? N3 C4 1.408(11) . ? N3 C7 1.427(11) . ? C4 C5 1.353(12) . ? C4 H4 1.03(2) . ? C5 N6 1.399(11) . ? C5 H5 1.08(2) . ? N6 C16 1.409(10) . ? C7 C12 1.399(13) . ? C7 C8 1.414(14) . ? C8 C9 1.394(15) . ? C8 C13 1.514(15) . ? C9 C10 1.393(17) . ? C9 H9 1.04(4) . ? C10 C11 1.406(16) . ? C10 C14 1.562(15) . ? C11 C12 1.427(14) . ? C11 H11 1.10(3) . ? C12 C15 1.478(15) . ? C13 H131 1.059(14) . ? C13 H132 1.057(13) . ? C13 H133 1.066(13) . ? C14 H141 1.044(14) . ? C14 H142 1.046(14) . ? C14 H143 1.035(14) . ? C15 H151 1.054(13) . ? C15 H152 1.048(13) . ? C15 H153 1.056(13) . ? C16 C21 1.384(13) . ? C16 C17 1.431(12) . ? C17 C18 1.416(13) . ? C17 C22 1.482(13) . ? C18 C19 1.393(17) . ? C18 H18 0.97(4) . ? C19 C20 1.358(18) . ? C19 C23 1.519(15) . ? C20 C21 1.436(15) . ? C20 H20 1.12(3) . ? C21 C24 1.490(17) . ? C22 H221 1.041(13) . ? C22 H222 1.060(14) . ? C22 H223 1.067(13) . ? C23 H231 1.063(14) . ? C23 H232 1.072(14) . ? C23 H233 1.056(14) . ? C24 H241 1.048(13) . ? C24 H242 1.051(14) . ? C24 H243 1.060(14) . ? C25 N26 1.362(9) . ? C25 N29 1.383(9) . ? N26 C27 1.379(10) . ? N26 C30 1.432(10) . ? C27 C28 1.374(12) . ? C27 H27 1.096(19) . ? C28 N29 1.388(10) . ? C28 H28 1.08(2) . ? N29 C39 1.452(10) . ? C30 C35 1.392(11) . ? C30 C31 1.397(12) . ? C31 C32 1.410(13) . ? C31 C36 1.507(13) . ? C32 C33 1.388(14) . ? C32 H32 1.04(3) . ? C33 C34 1.386(14) . ? C33 C37 1.550(13) . ? C34 C35 1.425(12) . ? C34 H34 1.07(3) . ? C35 C38 1.520(12) . ? C36 H361 1.052(13) . ? C36 H362 1.045(13) . ? C36 H363 1.039(13) . ? C37 H371 1.041(14) . ? C37 H372 1.052(13) . ? C37 H373 1.050(13) . ? C38 H381 1.052(13) . ? C38 H382 1.047(13) . ? C38 H383 1.049(13) . ? C39 C44 1.372(12) . ? C39 C40 1.396(12) . ? C40 C41 1.421(13) . ? C40 C45 1.518(13) . ? C41 C42 1.359(14) . ? C41 H41 1.08(3) . ? C42 C43 1.404(14) . ? C42 C46 1.507(14) . ? C43 C44 1.415(12) . ? C43 H43 1.04(3) . ? C44 C47 1.508(12) . ? C45 H451 1.030(13) . ? C45 H452 1.050(13) . ? C45 H453 1.054(13) . ? C46 H461 1.063(13) . ? C46 H462 1.041(14) . ? C46 H463 1.053(14) . ? C47 H471 1.052(13) . ? C47 H472 1.036(13) . ? C47 H473 1.060(13) . ? B48 N49 1.381(12) . ? B48 H481 1.30(2) . ? B48 H482 1.41(2) . ? N49 C50 1.452(13) . ? N49 C51 1.479(13) . ? C50 H503 0.99(5) . ? C50 H502 1.06(4) . ? C50 H501 1.09(4) . ? C51 H511 1.13(3) . ? C51 H512 1.04(4) . ? C51 H513 1.09(4) . ? B60 C103 1.616(12) . ? B60 C89 1.649(11) . ? B60 C61 1.649(12) . ? B60 C75 1.650(11) . ? C61 C62 1.399(10) . ? C61 C66 1.427(10) . ? C62 C63 1.386(11) . ? C62 H62 1.104(19) . ? C63 C64 1.382(11) . ? C63 C67 1.519(10) . ? C64 C65 1.399(11) . ? C64 H64 1.07(2) . ? C65 C66 1.378(10) . ? C65 C71 1.545(10) . ? C66 H66 1.144(16) . ? C67 F681 1.300(11) . ? C67 F691 1.305(12) . ? C67 F68 1.305(12) . ? C67 F701 1.312(12) . ? C67 F70 1.322(12) . ? C67 F69 1.337(12) . ? C71 F73 1.305(10) . ? C71 F72 1.318(10) . ? C71 F74 1.324(10) . ? C75 C80 1.411(11) . ? C75 C76 1.412(10) . ? C76 C77 1.375(11) . ? C76 H76 1.072(18) . ? C77 C78 1.377(12) . ? C77 C81 1.517(11) . ? C78 C79 1.402(12) . ? C78 H78 1.07(2) . ? C79 C80 1.418(11) . ? C79 C85 1.472(11) . ? C80 H80 1.065(19) . ? C81 F82 1.295(10) . ? C81 F83 1.323(10) . ? C81 F84 1.323(10) . ? C85 F86 1.292(10) . ? C85 F87 1.330(10) . ? C85 F88 1.334(10) . ? C89 C90 1.396(11) . ? C89 C94 1.401(12) . ? C90 C91 1.369(12) . ? C90 H90 1.07(3) . ? C91 C92 1.401(13) . ? C91 C95 1.494(12) . ? C92 C93 1.376(13) . ? C92 H92 1.093(19) . ? C93 C94 1.399(11) . ? C93 C99 1.503(12) . ? C94 H94 1.122(19) . ? C95 F981 1.294(13) . ? C95 F97 1.296(11) . ? C95 F971 1.304(12) . ? C95 F96 1.314(12) . ? C95 F961 1.340(13) . ? C95 F98 1.340(11) . ? C99 F100 1.312(11) . ? C99 F102 1.315(11) . ? C99 F101 1.328(10) . ? C103 C108 1.383(10) . ? C103 C104 1.425(10) . ? C104 C105 1.400(11) . ? C104 H104 1.092(16) . ? C105 C106 1.402(11) . ? C105 C109 1.492(11) . ? C106 C107 1.369(11) . ? C106 H106 1.08(2) . ? C107 C108 1.418(11) . ? C107 C113 1.505(11) . ? C108 H108 1.115(17) . ? C109 F110 1.293(11) . ? C109 F111 1.314(10) . ? C109 F12A 1.315(13) . ? C109 F10A 1.319(13) . ? C109 F11A 1.323(13) . ? C109 F112 1.324(11) . ? C113 F115 1.306(10) . ? C113 F114 1.312(10) . ? C113 F116 1.326(10) . ? 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 B48 Ir1 C2 94.3(5) . . ? B48 Ir1 C25 96.9(4) . . ? C2 Ir1 C25 168.8(4) . . ? B48 Ir1 H1 141.2(7) . . ? C2 Ir1 H1 85.5(7) . . ? C25 Ir1 H1 85.4(7) . . ? B48 Ir1 H2 139.4(8) . . ? C2 Ir1 H2 86.5(6) . . ? C25 Ir1 H2 85.4(6) . . ? H1 Ir1 H2 79.4(9) . . ? B48 Ir1 H481 38.4(7) . . ? C2 Ir1 H481 92.0(7) . . ? C25 Ir1 H481 96.4(6) . . ? H1 Ir1 H481 102.8(8) . . ? H2 Ir1 H481 177.3(9) . . ? B48 Ir1 H482 42.4(6) . . ? C2 Ir1 H482 95.3(7) . . ? C25 Ir1 H482 93.3(7) . . ? H1 Ir1 H482 176.3(9) . . ? H2 Ir1 H482 97.1(9) . . ? H481 Ir1 H482 80.7(8) . . ? N3 C2 N6 104.3(6) . . ? N3 C2 Ir1 127.9(6) . . ? N6 C2 Ir1 127.6(6) . . ? C2 N3 C4 112.1(6) . . ? C2 N3 C7 125.0(6) . . ? C4 N3 C7 122.9(6) . . ? C5 C4 N3 105.1(8) . . ? C5 C4 H4 131.7(13) . . ? N3 C4 H4 123.0(12) . . ? C4 C5 N6 108.1(8) . . ? C4 C5 H5 127.2(12) . . ? N6 C5 H5 124.6(12) . . ? C2 N6 C5 110.3(6) . . ? C2 N6 C16 126.1(6) . . ? C5 N6 C16 123.6(6) . . ? C12 C7 C8 123.8(8) . . ? C12 C7 N3 118.9(8) . . ? C8 C7 N3 117.3(8) . . ? C9 C8 C7 117.4(10) . . ? C9 C8 C13 118.3(10) . . ? C7 C8 C13 124.2(8) . . ? C10 C9 C8 120.5(12) . . ? C10 C9 H9 118.2(15) . . ? C8 C9 H9 121.3(17) . . ? C9 C10 C11 121.8(10) . . ? C9 C10 C14 119.5(11) . . ? C11 C10 C14 118.7(11) . . ? C10 C11 C12 119.1(10) . . ? C10 C11 H11 120.7(15) . . ? C12 C11 H11 120.2(16) . . ? C7 C12 C11 117.3(9) . . ? C7 C12 C15 122.0(8) . . ? C11 C12 C15 120.7(9) . . ? C8 C13 H131 115.4(15) . . ? C8 C13 H132 116.4(16) . . ? H131 C13 H132 105.0(15) . . ? C8 C13 H133 111.0(14) . . ? H131 C13 H133 103.2(15) . . ? H132 C13 H133 104.5(14) . . ? C10 C14 H141 112.8(16) . . ? C10 C14 H142 110.3(15) . . ? H141 C14 H142 107.2(15) . . ? C10 C14 H143 109.6(16) . . ? H141 C14 H143 108.7(16) . . ? H142 C14 H143 108.1(16) . . ? C12 C15 H151 109.7(16) . . ? C12 C15 H152 113.8(15) . . ? H151 C15 H152 106.2(14) . . ? C12 C15 H153 113.5(14) . . ? H151 C15 H153 106.6(15) . . ? H152 C15 H153 106.6(15) . . ? C21 C16 N6 120.7(8) . . ? C21 C16 C17 121.8(8) . . ? N6 C16 C17 117.5(7) . . ? C18 C17 C16 117.9(9) . . ? C18 C17 C22 120.7(9) . . ? C16 C17 C22 121.4(7) . . ? C19 C18 C17 120.6(11) . . ? C19 C18 H18 120.4(15) . . ? C17 C18 H18 118.8(16) . . ? C20 C19 C18 120.2(10) . . ? C20 C19 C23 118.2(12) . . ? C18 C19 C23 121.6(13) . . ? C19 C20 C21 122.2(11) . . ? C19 C20 H20 126.7(18) . . ? C21 C20 H20 111.1(19) . . ? C16 C21 C20 117.3(10) . . ? C16 C21 C24 120.3(9) . . ? C20 C21 C24 122.2(9) . . ? C17 C22 H221 112.4(15) . . ? C17 C22 H222 115.6(15) . . ? H221 C22 H222 106.2(15) . . ? C17 C22 H223 113.3(16) . . ? H221 C22 H223 105.3(15) . . ? H222 C22 H223 103.1(14) . . ? C19 C23 H231 115.3(18) . . ? C19 C23 H232 111.6(16) . . ? H231 C23 H232 102.4(15) . . ? C19 C23 H233 116.4(15) . . ? H231 C23 H233 105.2(15) . . ? H232 C23 H233 104.6(16) . . ? C21 C24 H241 110.3(16) . . ? C21 C24 H242 115.7(17) . . ? H241 C24 H242 106.7(15) . . ? C21 C24 H243 111.9(15) . . ? H241 C24 H243 106.9(15) . . ? H242 C24 H243 104.8(15) . . ? N26 C25 N29 104.7(6) . . ? N26 C25 Ir1 125.9(5) . . ? N29 C25 Ir1 129.0(5) . . ? C25 N26 C27 111.1(6) . . ? C25 N26 C30 127.2(6) . . ? C27 N26 C30 121.7(6) . . ? C28 C27 N26 107.3(7) . . ? C28 C27 H27 131.0(12) . . ? N26 C27 H27 121.6(11) . . ? C27 C28 N29 106.3(7) . . ? C27 C28 H28 132.5(12) . . ? N29 C28 H28 121.2(11) . . ? C25 N29 C28 110.5(6) . . ? C25 N29 C39 125.7(6) . . ? C28 N29 C39 123.7(6) . . ? C35 C30 C31 122.0(7) . . ? C35 C30 N26 118.2(7) . . ? C31 C30 N26 119.7(7) . . ? C30 C31 C32 118.5(8) . . ? C30 C31 C36 121.2(8) . . ? C32 C31 C36 120.3(8) . . ? C33 C32 C31 120.2(9) . . ? C33 C32 H32 120.9(14) . . ? C31 C32 H32 118.9(14) . . ? C34 C33 C32 121.1(8) . . ? C34 C33 C37 118.9(9) . . ? C32 C33 C37 120.1(9) . . ? C33 C34 C35 119.7(9) . . ? C33 C34 H34 120.0(13) . . ? C35 C34 H34 120.3(13) . . ? C30 C35 C34 118.5(8) . . ? C30 C35 C38 121.5(7) . . ? C34 C35 C38 120.1(8) . . ? C31 C36 H361 110.6(15) . . ? C31 C36 H362 111.8(15) . . ? H361 C36 H362 106.9(14) . . ? C31 C36 H363 110.0(14) . . ? H361 C36 H363 108.1(15) . . ? H362 C36 H363 109.4(15) . . ? C33 C37 H371 113.4(14) . . ? C33 C37 H372 113.7(15) . . ? H371 C37 H372 106.6(15) . . ? C33 C37 H373 108.7(14) . . ? H371 C37 H373 107.2(14) . . ? H372 C37 H373 106.9(14) . . ? C35 C38 H381 111.6(13) . . ? C35 C38 H382 113.7(13) . . ? H381 C38 H382 107.6(14) . . ? C35 C38 H383 109.6(12) . . ? H381 C38 H383 106.7(14) . . ? H382 C38 H383 107.4(14) . . ? C44 C39 C40 123.8(7) . . ? C44 C39 N29 118.5(7) . . ? C40 C39 N29 117.7(7) . . ? C39 C40 C41 117.4(8) . . ? C39 C40 C45 122.3(8) . . ? C41 C40 C45 120.2(8) . . ? C42 C41 C40 121.2(9) . . ? C42 C41 H41 119.3(15) . . ? C40 C41 H41 119.4(15) . . ? C41 C42 C43 119.2(9) . . ? C41 C42 C46 120.8(9) . . ? C43 C42 C46 120.0(10) . . ? C42 C43 C44 122.0(10) . . ? C42 C43 H43 116.8(13) . . ? C44 C43 H43 121.2(13) . . ? C39 C44 C43 116.4(8) . . ? C39 C44 C47 123.8(7) . . ? C43 C44 C47 119.8(8) . . ? C40 C45 H451 113.2(14) . . ? C40 C45 H452 111.2(14) . . ? H451 C45 H452 110.1(14) . . ? C40 C45 H453 107.5(14) . . ? H451 C45 H453 108.9(14) . . ? H452 C45 H453 105.5(14) . . ? C42 C46 H461 111.0(14) . . ? C42 C46 H462 114.0(13) . . ? H461 C46 H462 105.7(15) . . ? C42 C46 H463 113.6(14) . . ? H461 C46 H463 105.0(14) . . ? H462 C46 H463 107.0(15) . . ? C44 C47 H471 110.1(13) . . ? C44 C47 H472 113.4(14) . . ? H471 C47 H472 108.6(14) . . ? C44 C47 H473 113.7(13) . . ? H471 C47 H473 103.6(14) . . ? H472 C47 H473 106.9(14) . . ? N49 B48 Ir1 170.4(9) . . ? N49 B48 H481 119.9(11) . . ? Ir1 B48 H481 64.2(8) . . ? N49 B48 H482 114.7(11) . . ? Ir1 B48 H482 60.4(8) . . ? H481 B48 H482 124.6(12) . . ? B48 N49 C50 122.8(9) . . ? B48 N49 C51 122.1(9) . . ? C50 N49 C51 114.5(9) . . ? N49 C50 H503 109.7(18) . . ? N49 C50 H502 109.7(16) . . ? H503 C50 H502 107(3) . . ? N49 C50 H501 110.9(19) . . ? H503 C50 H501 111(3) . . ? H502 C50 H501 109(2) . . ? N49 C51 H511 103.4(16) . . ? N49 C51 H512 108.4(16) . . ? H511 C51 H512 115(2) . . ? N49 C51 H513 111.7(14) . . ? H511 C51 H513 110(2) . . ? H512 C51 H513 109(2) . . ? C103 B60 C89 112.8(7) . . ? C103 B60 C61 105.7(6) . . ? C89 B60 C61 112.6(7) . . ? C103 B60 C75 111.2(7) . . ? C89 B60 C75 105.0(6) . . ? C61 B60 C75 109.6(7) . . ? C62 C61 C66 115.8(7) . . ? C62 C61 B60 120.2(6) . . ? C66 C61 B60 123.8(6) . . ? C63 C62 C61 121.9(7) . . ? C63 C62 H62 119.5(11) . . ? C61 C62 H62 118.5(11) . . ? C64 C63 C62 122.1(7) . . ? C64 C63 C67 119.8(7) . . ? C62 C63 C67 118.1(7) . . ? C63 C64 C65 116.8(8) . . ? C63 C64 H64 121.1(11) . . ? C65 C64 H64 122.1(11) . . ? C66 C65 C64 122.1(7) . . ? C66 C65 C71 117.1(6) . . ? C64 C65 C71 120.8(7) . . ? C65 C66 C61 121.2(6) . . ? C65 C66 H66 117.8(10) . . ? C61 C66 H66 121.0(10) . . ? F681 C67 F691 108.8(11) . . ? F681 C67 F68 74.6(13) . . ? F691 C67 F68 128.6(15) . . ? F681 C67 F701 107.4(11) . . ? F691 C67 F701 106.7(10) . . ? F68 C67 F701 34.5(11) . . ? F681 C67 F70 123.8(17) . . ? F691 C67 F70 27.4(12) . . ? F68 C67 F70 107.0(11) . . ? F701 C67 F70 79.9(13) . . ? F681 C67 F69 32.1(12) . . ? F691 C67 F69 81.7(14) . . ? F68 C67 F69 104.8(11) . . ? F701 C67 F69 133.4(14) . . ? F70 C67 F69 104.4(11) . . ? F681 C67 C63 115.3(11) . . ? F691 C67 C63 110.0(12) . . ? F68 C67 C63 114.1(12) . . ? F701 C67 C63 108.3(11) . . ? F70 C67 C63 114.3(14) . . ? F69 C67 C63 111.4(12) . . ? F73 C71 F72 107.2(9) . . ? F73 C71 F74 107.8(9) . . ? F72 C71 F74 105.3(8) . . ? F73 C71 C65 111.8(7) . . ? F72 C71 C65 112.7(8) . . ? F74 C71 C65 111.6(7) . . ? C80 C75 C76 115.5(7) . . ? C80 C75 B60 123.5(7) . . ? C76 C75 B60 120.5(7) . . ? C77 C76 C75 122.0(7) . . ? C77 C76 H76 115.6(10) . . ? C75 C76 H76 122.3(11) . . ? C76 C77 C78 123.1(8) . . ? C76 C77 C81 119.7(8) . . ? C78 C77 C81 117.1(7) . . ? C77 C78 C79 116.6(7) . . ? C77 C78 H78 123.2(13) . . ? C79 C78 H78 120.2(13) . . ? C78 C79 C80 121.2(7) . . ? C78 C79 C85 117.5(7) . . ? C80 C79 C85 121.3(7) . . ? C75 C80 C79 121.4(7) . . ? C75 C80 H80 118.2(11) . . ? C79 C80 H80 120.5(11) . . ? F82 C81 F83 106.1(10) . . ? F82 C81 F84 107.2(9) . . ? F83 C81 F84 103.9(9) . . ? F82 C81 C77 112.9(9) . . ? F83 C81 C77 111.0(9) . . ? F84 C81 C77 115.0(9) . . ? F86 C85 F87 106.0(9) . . ? F86 C85 F88 107.5(10) . . ? F87 C85 F88 103.0(8) . . ? F86 C85 C79 113.0(9) . . ? F87 C85 C79 113.4(8) . . ? F88 C85 C79 113.2(9) . . ? C90 C89 C94 116.0(7) . . ? C90 C89 B60 121.3(7) . . ? C94 C89 B60 122.5(7) . . ? C91 C90 C89 121.9(8) . . ? C91 C90 H90 121.9(12) . . ? C89 C90 H90 116.1(12) . . ? C90 C91 C92 122.0(9) . . ? C90 C91 C95 120.7(8) . . ? C92 C91 C95 117.2(8) . . ? C93 C92 C91 117.0(8) . . ? C93 C92 H92 124.4(14) . . ? C91 C92 H92 118.5(14) . . ? C92 C93 C94 121.1(8) . . ? C92 C93 C99 118.9(7) . . ? C94 C93 C99 119.9(8) . . ? C93 C94 C89 121.8(8) . . ? C93 C94 H94 117.9(11) . . ? C89 C94 H94 120.3(10) . . ? F981 C95 F97 133.6(16) . . ? F981 C95 F971 109.1(12) . . ? F97 C95 F971 42.9(12) . . ? F981 C95 F96 53.8(14) . . ? F97 C95 F96 110.1(11) . . ? F971 C95 F96 129.9(16) . . ? F981 C95 F961 105.5(12) . . ? F97 C95 F961 64.5(14) . . ? F971 C95 F961 104.4(12) . . ? F96 C95 F961 53.4(13) . . ? F981 C95 F98 52.8(14) . . ? F97 C95 F98 105.1(10) . . ? F971 C95 F98 63.9(13) . . ? F96 C95 F98 103.8(10) . . ? F961 C95 F98 141.2(15) . . ? F981 C95 C91 112.4(14) . . ? F97 C95 C91 113.7(11) . . ? F971 C95 C91 116.6(13) . . ? F96 C95 C91 113.2(10) . . ? F961 C95 C91 108.0(13) . . ? F98 C95 C91 110.2(11) . . ? F100 C99 F102 106.4(10) . . ? F100 C99 F101 106.2(10) . . ? F102 C99 F101 105.3(9) . . ? F100 C99 C93 112.5(10) . . ? F102 C99 C93 113.3(9) . . ? F101 C99 C93 112.6(10) . . ? C108 C103 C104 116.1(7) . . ? C108 C103 B60 126.2(7) . . ? C104 C103 B60 117.7(6) . . ? C105 C104 C103 122.5(6) . . ? C105 C104 H104 117.3(10) . . ? C103 C104 H104 120.1(10) . . ? C104 C105 C106 118.8(7) . . ? C104 C105 C109 119.2(7) . . ? C106 C105 C109 121.8(7) . . ? C107 C106 C105 119.9(7) . . ? C107 C106 H106 120.8(11) . . ? C105 C106 H106 119.0(11) . . ? C106 C107 C108 120.4(6) . . ? C106 C107 C113 121.0(7) . . ? C108 C107 C113 118.6(7) . . ? C103 C108 C107 121.9(7) . . ? C103 C108 H108 117.3(10) . . ? C107 C108 H108 120.7(10) . . ? F110 C109 F111 108.2(9) . . ? F110 C109 F12A 65.9(16) . . ? F111 C109 F12A 131.7(17) . . ? F110 C109 F10A 43.2(17) . . ? F111 C109 F10A 69.4(17) . . ? F12A C109 F10A 105.8(13) . . ? F110 C109 F11A 130.8(18) . . ? F111 C109 F11A 39.9(16) . . ? F12A C109 F11A 105.4(13) . . ? F10A C109 F11A 105.3(13) . . ? F110 C109 F112 107.6(10) . . ? F111 C109 F112 105.8(9) . . ? F12A C109 F112 44.0(16) . . ? F10A C109 F112 136.8(18) . . ? F11A C109 F112 67.7(17) . . ? F110 C109 C105 114.2(9) . . ? F111 C109 C105 112.6(9) . . ? F12A C109 C105 112.9(16) . . ? F10A C109 C105 113.3(17) . . ? F11A C109 C105 113.5(17) . . ? F112 C109 C105 108.0(9) . . ? F115 C113 F114 106.1(9) . . ? F115 C113 F116 106.3(9) . . ? F114 C113 F116 105.8(9) . . ? F115 C113 C107 111.1(8) . . ? F114 C113 C107 112.8(8) . . ? F116 C113 C107 114.1(8) . . ? _diffrn_measured_fraction_theta_max 0.043 _diffrn_reflns_theta_full 82.53 _diffrn_measured_fraction_theta_full 0.043 _refine_diff_density_max 1.032 _refine_diff_density_min -0.967 _refine_diff_density_rms 0.233 data_3-XRD _database_code_depnum_ccdc_archive 'CCDC 880793' #TrackingRef 'CrystallographicData.cif' #============================================================================== _audit_creation_date 10-12-20 _audit_creation_method CRYSTALS_ver_14.10 _oxford_structure_analysis_title 129ct10 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 12.7501(1) _cell_length_b 14.1549(1) _cell_length_c 21.1993(2) _cell_angle_alpha 90 _cell_angle_beta 93.0899(3) _cell_angle_gamma 90 _cell_volume 3820.41(5) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/n ' _symmetry_space_group_name_Hall '-P 2yac' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,-y,z+1/2 -x+1/2,y,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Rh -1.1178 0.9187 19.2957 0.7515 14.3501 8.2176 4.7343 25.8749 1.2892 98.6062 5.3280 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C84 B2 N6 Rh1 # Dc = 1.06 Fooo = 1662.00 Mu = 2.66 M = 608.75 # Found Formula = C76 H69 B2 F24 N5 Rh1 # Dc = 1.42 FOOO = 1662.00 Mu = 3.27 M = 816.45 _chemical_formula_sum 'C76 H69 B2 F24 N5 Rh1' _chemical_formula_moiety 'C44 H57 B N5 Rh, C32 H12 B F24' _chemical_compound_source . _chemical_formula_weight 1632.90 _cell_measurement_reflns_used 8940 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour clear_intense_yellow _exptl_crystal_size_min 0.260 _exptl_crystal_size_mid 0.320 _exptl_crystal_size_max 0.360 _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1662.000 _exptl_absorpt_coefficient_mu 0.327 # Sheldrick geometric approximatio 0.90 0.92 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.92 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 61210 _reflns_number_total 8721 _diffrn_reflns_av_R_equivalents 0.024 # Number of reflections without Friedels Law is 17339 # Number of reflections with Friedels Law is 8721 # Theoretical number of reflections is about 8797 _diffrn_reflns_theta_min 5.135 _diffrn_reflns_theta_max 27.523 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.972 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _reflns_limit_h_min -16 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 27 _oxford_diffrn_Wilson_B_factor 3.50 _oxford_diffrn_Wilson_scale 9.58 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.98 _refine_diff_density_max 1.40 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 8721 _refine_ls_number_restraints 326 _refine_ls_number_parameters 565 _oxford_refine_ls_R_factor_ref 0.0827 _refine_ls_wR_factor_ref 0.1930 _refine_ls_goodness_of_fit_ref 0.9614 _refine_ls_shift/su_max 0.0029940 _refine_ls_shift/su_mean 0.0000348 # The values computed from all data _oxford_reflns_number_all 8721 _refine_ls_R_factor_all 0.0827 _refine_ls_wR_factor_all 0.1930 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6947 _refine_ls_R_factor_gt 0.0669 _refine_ls_wR_factor_gt 0.1807 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.12P)^2^ + 5.19P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Rh1 Rh 0.250000(10) 0.15486(2) 0.750000(10) 0.0382 1.0000 Uani S T . . . . C2 C 0.4103(3) 0.1590(2) 0.75344(17) 0.0437 1.0000 Uani . . . . . . N3 N 0.4810(2) 0.1222(2) 0.79659(15) 0.0487 1.0000 Uani . . . . . . C4 C 0.5831(3) 0.1469(4) 0.7830(2) 0.0687 1.0000 Uani . . . . . . C5 C 0.5760(3) 0.1992(4) 0.7308(2) 0.0737 1.0000 Uani . . . . . . N6 N 0.4703(2) 0.2067(3) 0.71305(16) 0.0554 1.0000 Uani . . . . . . C7 C 0.4524(3) 0.0640(3) 0.84872(16) 0.0457 1.0000 Uani . . . . . . C8 C 0.4118(3) 0.1068(3) 0.90102(18) 0.0542 1.0000 Uani . . . . . . C9 C 0.3806(4) 0.0475(3) 0.9489(2) 0.0639 1.0000 Uani . . . . . . C10 C 0.3895(3) -0.0489(3) 0.94598(18) 0.0570 1.0000 Uani . . . . . . C11 C 0.4362(4) -0.0877(3) 0.89451(19) 0.0590 1.0000 Uani . . . . . . C12 C 0.4678(3) -0.0323(3) 0.84480(19) 0.0571 1.0000 Uani . . . . . . C13 C 0.3991(5) 0.2127(3) 0.9058(3) 0.0797 1.0000 Uani . . . . . . C14 C 0.3518(5) -0.1106(4) 0.9986(2) 0.0768 1.0000 Uani . . . . . . C15 C 0.5158(5) -0.0764(4) 0.7884(2) 0.0877 1.0000 Uani . . . . . . C16 C 0.4279(3) 0.2583(3) 0.6586(2) 0.0575 1.0000 Uani . . . . . . C17 C 0.4236(5) 0.2154(4) 0.6013(2) 0.0835 1.0000 Uani . . . . . . C18 C 0.3827(5) 0.2667(4) 0.5492(2) 0.0859 1.0000 Uani . . . . . . C19 C 0.3464(4) 0.3565(4) 0.5548(2) 0.0741 1.0000 Uani . . . . . . C20 C 0.3495(5) 0.3968(4) 0.6140(3) 0.0783 1.0000 Uani . . . . . . C21 C 0.3902(4) 0.3506(3) 0.6675(2) 0.0659 1.0000 Uani . . . . . . C22 C 0.4632(11) 0.1156(7) 0.5930(3) 0.2030 1.0000 Uani . . . . . . C23 C 0.3010(6) 0.4085(5) 0.4966(3) 0.1021 1.0000 Uani . . . . . . C24 C 0.3976(7) 0.3982(5) 0.7315(3) 0.1133 1.0000 Uani . . . . . . B48 B 0.2441(13) 0.0182(6) 0.7354(5) 0.0573 0.5000 Uani . . . 1 -1 . N49 N 0.2188(7) -0.0576(5) 0.7734(5) 0.0768 0.5000 Uani . . . 1 -1 . C50 C 0.2248(14) -0.1558(7) 0.7579(19) 0.1189 0.5000 Uani . . . 1 -1 . C51 C 0.1826(10) -0.0489(10) 0.8369(6) 0.1026 0.5000 Uani . . . 1 -1 . B60 B 0.2500 0.3661(4) 0.2500 0.0375 1.0000 Uani S T . . . . C61 C 0.1872(2) 0.4308(2) 0.29993(14) 0.0360 1.0000 Uani . . . . . . C62 C 0.2327(3) 0.5131(2) 0.32592(15) 0.0383 1.0000 Uani . . . . . . C63 C 0.1878(3) 0.5630(2) 0.37420(16) 0.0432 1.0000 Uani . . . . . . C64 C 0.0938(3) 0.5330(3) 0.39779(16) 0.0467 1.0000 Uani . . . . . . C65 C 0.0481(3) 0.4522(3) 0.37296(17) 0.0480 1.0000 Uani . . . . . . C66 C 0.0939(3) 0.4014(3) 0.32537(16) 0.0423 1.0000 Uani . . . . . . C67 C 0.2425(4) 0.6484(3) 0.4018(2) 0.0564 1.0000 Uani . . . . . . F68 F 0.3469(3) 0.6411(3) 0.4051(2) 0.1237 1.0000 Uani . . . . . . F69 F 0.2239(4) 0.6655(3) 0.46024(17) 0.1163 1.0000 Uani . . . . . . F70 F 0.2299(4) 0.7229(2) 0.3668(2) 0.1398 1.0000 Uani . . . . . . C71 C -0.0478(2) 0.4124(3) 0.40110(16) 0.0886 1.0000 Uani D . . . . . F72 F -0.0229(4) 0.3594(4) 0.4526(3) 0.0938 0.647(8) Uani D . P 2 1 . F73 F -0.1132(4) 0.4790(4) 0.4203(3) 0.0991 0.647(8) Uani D . P 2 1 . F74 F -0.1065(4) 0.3558(5) 0.3619(2) 0.0920 0.647(8) Uani D . P 2 1 . C75 C 0.1717(3) 0.3009(2) 0.20407(14) 0.0384 1.0000 Uani . . . . . . C76 C 0.0713(3) 0.3288(3) 0.18234(17) 0.0471 1.0000 Uani . . . . . . C77 C 0.0098(3) 0.2749(3) 0.13950(19) 0.0571 1.0000 Uani . . . . . . C78 C 0.0466(3) 0.1904(3) 0.11661(17) 0.0530 1.0000 Uani . . . . . . C79 C 0.1467(3) 0.1611(2) 0.13652(16) 0.0441 1.0000 Uani . . . . . . C80 C 0.2072(3) 0.2164(2) 0.17895(15) 0.0408 1.0000 Uani . . . . . . C81 C -0.0931(2) 0.3116(2) 0.11571(17) 0.1022 1.0000 Uani D . . . . . F82 F -0.1108(13) 0.3541(12) 0.0604(5) 0.1045 0.236(12) Uani D . P 3 1 . F83 F -0.1311(13) 0.3710(11) 0.1591(6) 0.1021 0.236(12) Uani D . P 3 1 . F84 F -0.1579(9) 0.2349(7) 0.1144(10) 0.1034 0.236(12) Uani D . P 3 1 . C85 C 0.1910(3) 0.0711(3) 0.11349(19) 0.0549 1.0000 Uani . . . . . . F86 F 0.1900(2) 0.00264(18) 0.15620(13) 0.0745 1.0000 Uani . . . . . . F87 F 0.2918(2) 0.0800(2) 0.09932(15) 0.0865 1.0000 Uani . . . . . . F88 F 0.1399(2) 0.0384(2) 0.06175(13) 0.0755 1.0000 Uani . . . . . . F721 F -0.0482(7) 0.3280(5) 0.4268(5) 0.0959 0.353(8) Uani D . P 2 2 . F731 F -0.0834(7) 0.4718(6) 0.4451(4) 0.0847 0.353(8) Uani D . P 2 2 . F741 F -0.1238(5) 0.4105(9) 0.3538(3) 0.0945 0.353(8) Uani D . P 2 2 . F821 F -0.0807(4) 0.3845(4) 0.0746(3) 0.1087 0.764(12) Uani D . P 3 2 . F831 F -0.1512(4) 0.3463(4) 0.1613(2) 0.1028 0.764(12) Uani D . P 3 2 . F841 F -0.1544(3) 0.2491(4) 0.0844(4) 0.1108 0.764(12) Uani D . P 3 2 . H11 H 0.2686 0.1352 0.8128 0.0456 1.0000 Uiso R . . . . . H41 H 0.6440 0.1299 0.8059 0.0819 1.0000 Uiso R . . . . . H51 H 0.6316 0.2265 0.7104 0.0869 1.0000 Uiso R . . . . . H91 H 0.3526 0.0742 0.9844 0.0760 1.0000 Uiso R . . . . . H111 H 0.4464 -0.1531 0.8926 0.0710 1.0000 Uiso R . . . . . H131 H 0.3861 0.2305 0.9486 0.1192 1.0000 Uiso R . . . . . H132 H 0.4626 0.2419 0.8931 0.1189 1.0000 Uiso R . . . . . H133 H 0.3413 0.2322 0.8777 0.1188 1.0000 Uiso R . . . . . H141 H 0.3820 -0.1717 0.9951 0.1149 1.0000 Uiso R . . . . . H142 H 0.3736 -0.0830 1.0386 0.1150 1.0000 Uiso R . . . . . H143 H 0.2764 -0.1158 0.9952 0.1149 1.0000 Uiso R . . . . . H153 H 0.5354 -0.1411 0.7978 0.1310 1.0000 Uiso R . . . . . H152 H 0.5769 -0.0418 0.7767 0.1309 1.0000 Uiso R . . . . . H151 H 0.4638 -0.0769 0.7534 0.1309 1.0000 Uiso R . . . . . H181 H 0.3793 0.2385 0.5103 0.1031 1.0000 Uiso R . . . . . H201 H 0.3244 0.4577 0.6182 0.0939 1.0000 Uiso R . . . . . H221 H 0.4717 0.1033 0.5491 0.3089 1.0000 Uiso R . . . . . H222 H 0.5290 0.1084 0.6162 0.3089 1.0000 Uiso R . . . . . H223 H 0.4133 0.0720 0.6089 0.3089 1.0000 Uiso R . . . . . H231 H 0.3425 0.4642 0.4901 0.1532 1.0000 Uiso R . . . . . H232 H 0.3023 0.3688 0.4596 0.1530 1.0000 Uiso R . . . . . H233 H 0.2298 0.4280 0.5026 0.1531 1.0000 Uiso R . . . . . H241 H 0.3658 0.4604 0.7275 0.1738 1.0000 Uiso R . . . . . H242 H 0.4694 0.4051 0.7465 0.1742 1.0000 Uiso R . . . . . H243 H 0.3604 0.3604 0.7617 0.1741 1.0000 Uiso R . . . . . H481 H 0.2607 0.0001 0.6940 0.0724 0.5000 Uiso R . . 1 -1 . H501 H 0.2623 -0.1871 0.7926 0.1820 0.5000 Uiso R . . 1 -1 . H502 H 0.2607 -0.1651 0.7195 0.1821 0.5000 Uiso R . . 1 -1 . H503 H 0.1549 -0.1815 0.7530 0.1820 0.5000 Uiso R . . 1 -1 . H511 H 0.2190 -0.0947 0.8637 0.1570 0.5000 Uiso R . . 1 -1 . H512 H 0.1969 0.0139 0.8525 0.1569 0.5000 Uiso R . . 1 -1 . H513 H 0.1083 -0.0608 0.8359 0.1570 0.5000 Uiso R . . 1 -1 . H621 H 0.2942 0.5354 0.3102 0.0462 1.0000 Uiso R . . . . . H641 H 0.0620 0.5653 0.4298 0.0561 1.0000 Uiso R . . . . . H661 H 0.0609 0.3463 0.3101 0.0499 1.0000 Uiso R . . . . . H761 H 0.0429 0.3849 0.1970 0.0559 1.0000 Uiso R . . . . . H781 H 0.0062 0.1539 0.0877 0.0630 1.0000 Uiso R . . . . . H801 H 0.2743 0.1951 0.1903 0.0491 1.0000 Uiso R . . . . . 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 Rh1 0.0434(2) 0.0373(2) 0.0337(2) 0.0000 0.00161(14) 0.0000 C2 0.0474(18) 0.0446(18) 0.0387(17) 0.0058(14) -0.0014(14) 0.0017(14) N3 0.0451(15) 0.0579(17) 0.0427(16) 0.0116(14) -0.0016(12) 0.0007(14) C4 0.045(2) 0.100(4) 0.060(3) 0.024(2) -0.0067(18) 0.000(2) C5 0.048(2) 0.105(4) 0.068(3) 0.029(3) -0.002(2) -0.008(2) N6 0.0443(16) 0.071(2) 0.0506(18) 0.0201(16) -0.0003(13) -0.0012(15) C7 0.0448(17) 0.054(2) 0.0378(17) 0.0088(15) -0.0018(14) 0.0039(15) C8 0.066(2) 0.053(2) 0.043(2) -0.0028(16) -0.0025(17) -0.0056(18) C9 0.086(3) 0.063(2) 0.045(2) -0.0056(18) 0.013(2) -0.006(2) C10 0.068(2) 0.063(2) 0.0390(19) 0.0088(17) -0.0012(17) -0.005(2) C11 0.079(3) 0.049(2) 0.049(2) 0.0056(17) 0.0022(19) 0.0092(19) C12 0.070(2) 0.059(2) 0.042(2) 0.0035(17) 0.0054(17) 0.017(2) C13 0.118(4) 0.053(2) 0.068(3) -0.011(2) 0.016(3) -0.007(3) C14 0.099(4) 0.074(3) 0.058(3) 0.016(2) 0.013(2) -0.012(3) C15 0.132(5) 0.073(3) 0.060(3) 0.003(2) 0.028(3) 0.032(3) C16 0.054(2) 0.069(3) 0.050(2) 0.0227(19) 0.0023(16) 0.0028(19) C17 0.104(4) 0.095(4) 0.052(3) 0.011(2) 0.007(2) 0.056(3) C18 0.111(4) 0.108(4) 0.040(2) 0.011(2) 0.008(2) 0.052(3) C19 0.077(3) 0.086(3) 0.060(3) 0.034(2) 0.013(2) 0.015(3) C20 0.102(4) 0.058(3) 0.074(3) 0.020(2) 0.004(3) 0.007(3) C21 0.083(3) 0.056(2) 0.059(3) 0.0087(19) 0.003(2) -0.007(2) C22 0.372(17) 0.161(8) 0.070(4) -0.026(5) -0.037(7) 0.198(10) C23 0.115(5) 0.117(5) 0.074(4) 0.047(4) 0.006(3) 0.032(4) C24 0.186(8) 0.073(4) 0.078(4) -0.007(3) -0.018(4) 0.019(4) B48 0.051(5) 0.054(4) 0.064(10) -0.009(4) -0.021(8) 0.007(5) N49 0.077(6) 0.048(4) 0.102(8) 0.013(4) -0.026(4) -0.011(3) C50 0.105(18) 0.045(5) 0.20(2) 0.027(9) -0.013(18) 0.003(6) C51 0.101(8) 0.104(9) 0.100(9) 0.048(7) -0.028(7) -0.046(7) B60 0.036(2) 0.042(3) 0.035(3) 0.0000 0.0064(19) 0.0000 C61 0.0368(15) 0.0416(16) 0.0300(15) 0.0028(12) 0.0055(11) 0.0032(12) C62 0.0411(16) 0.0413(16) 0.0330(16) 0.0037(13) 0.0080(12) 0.0003(13) C63 0.0557(19) 0.0421(17) 0.0324(16) 0.0028(13) 0.0075(14) 0.0068(15) C64 0.058(2) 0.0502(19) 0.0330(16) 0.0012(14) 0.0120(14) 0.0116(16) C65 0.0422(17) 0.066(2) 0.0368(17) 0.0053(16) 0.0126(14) 0.0028(16) C66 0.0417(16) 0.0486(18) 0.0367(17) 0.0016(14) 0.0050(13) 0.0001(14) C67 0.081(3) 0.0427(19) 0.048(2) -0.0041(16) 0.020(2) -0.0015(18) F68 0.083(2) 0.106(3) 0.180(4) -0.076(3) -0.010(2) -0.0127(19) F69 0.169(4) 0.106(3) 0.078(2) -0.0421(19) 0.048(2) -0.059(2) F70 0.211(5) 0.065(2) 0.135(3) 0.038(2) -0.069(3) -0.050(2) C71 0.0641(17) 0.117(2) 0.089(2) -0.0173(17) 0.0384(15) -0.0234(16) F72 0.083(2) 0.116(3) 0.086(3) -0.002(2) 0.039(2) -0.042(2) F73 0.066(2) 0.126(3) 0.109(3) -0.017(2) 0.043(2) -0.005(2) F74 0.062(2) 0.118(3) 0.099(3) -0.022(2) 0.0360(19) -0.032(2) C75 0.0441(16) 0.0425(17) 0.0289(15) 0.0024(12) 0.0046(12) -0.0041(13) C76 0.053(2) 0.0472(19) 0.0398(18) -0.0006(14) -0.0054(15) 0.0050(15) C77 0.060(2) 0.061(2) 0.048(2) -0.0019(18) -0.0151(17) 0.0053(19) C78 0.062(2) 0.059(2) 0.0375(18) -0.0048(16) -0.0085(16) -0.0080(18) C79 0.0558(19) 0.0474(18) 0.0297(15) -0.0021(13) 0.0071(14) -0.0075(15) C80 0.0434(16) 0.0460(17) 0.0335(16) -0.0009(13) 0.0073(13) -0.0032(14) C81 0.0850(19) 0.101(2) 0.113(2) -0.0225(17) -0.0582(17) 0.0232(17) F82 0.087(3) 0.106(4) 0.113(3) -0.021(3) -0.065(3) 0.021(3) F83 0.082(3) 0.101(4) 0.118(3) -0.024(3) -0.052(3) 0.022(3) F84 0.084(3) 0.104(3) 0.114(4) -0.024(3) -0.063(3) 0.023(3) C85 0.061(2) 0.060(2) 0.044(2) -0.0142(17) 0.0091(17) -0.0090(18) F86 0.103(2) 0.0559(14) 0.0645(16) -0.0018(12) 0.0084(14) 0.0124(14) F87 0.0703(16) 0.091(2) 0.101(2) -0.0520(17) 0.0343(15) -0.0122(14) F88 0.0954(19) 0.0719(16) 0.0581(15) -0.0276(13) -0.0051(13) -0.0078(14) F721 0.073(3) 0.117(3) 0.102(3) -0.011(3) 0.037(3) -0.033(3) F731 0.058(3) 0.123(3) 0.076(3) -0.018(3) 0.038(3) -0.019(3) F741 0.066(3) 0.125(4) 0.096(3) -0.018(3) 0.033(2) -0.030(3) F821 0.108(3) 0.105(3) 0.106(3) -0.010(2) -0.063(2) 0.030(2) F831 0.061(2) 0.111(3) 0.132(3) -0.022(2) -0.0408(19) 0.020(2) F841 0.092(2) 0.109(2) 0.123(3) -0.026(2) -0.074(2) 0.0197(19) _refine_ls_extinction_coef 400(120) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.3123(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Rh1 . C2 4_556 2.042(4) yes Rh1 . H11 4_556 1.367 no Rh1 . B48 4_556 1.960(9) yes Rh1 . C2 . 2.042(4) yes Rh1 . B48 . 1.960(9) yes Rh1 . H11 . 1.367 no C2 . N3 . 1.353(4) yes C2 . N6 . 1.358(5) yes N3 . C4 . 1.393(5) yes N3 . C7 . 1.441(5) yes C4 . C5 . 1.331(6) yes C4 . H41 . 0.925 no C5 . N6 . 1.384(5) yes C5 . H51 . 0.934 no N6 . C16 . 1.445(5) yes C7 . C8 . 1.388(5) yes C7 . C12 . 1.380(6) yes C8 . C9 . 1.392(6) yes C8 . C13 . 1.513(6) yes C9 . C10 . 1.372(6) yes C9 . H91 . 0.930 no C10 . C11 . 1.384(6) yes C10 . C14 . 1.514(6) yes C11 . C12 . 1.391(6) yes C11 . H111 . 0.936 no C12 . C15 . 1.508(6) yes C13 . H131 . 0.966 no C13 . H132 . 0.960 no C13 . H133 . 0.962 no C14 . H141 . 0.952 no C14 . H142 . 0.961 no C14 . H143 . 0.963 no C15 . H153 . 0.967 no C15 . H152 . 0.964 no C15 . H151 . 0.969 no C16 . C17 . 1.356(7) yes C16 . C21 . 1.408(6) yes C17 . C18 . 1.398(6) yes C17 . C22 . 1.515(8) yes C18 . C19 . 1.361(7) yes C18 . H181 . 0.916 no C19 . C20 . 1.376(8) yes C19 . C23 . 1.525(7) yes C20 . C21 . 1.387(7) yes C20 . H201 . 0.926 no C21 . C24 . 1.512(8) yes C22 . H221 . 0.958 no C22 . H222 . 0.955 no C22 . H223 . 0.960 no C23 . H231 . 0.964 no C23 . H232 . 0.966 no C23 . H233 . 0.963 no C24 . H241 . 0.971 no C24 . H242 . 0.958 no C24 . H243 . 0.976 no B48 . N49 . 1.390(15) yes B48 . H481 . 0.950 no N49 . C50 . 1.431(16) yes N49 . C51 . 1.450(16) yes C50 . H501 . 0.964 no C50 . H502 . 0.964 no C50 . H503 . 0.963 no C51 . H511 . 0.965 no C51 . H512 . 0.962 no C51 . H513 . 0.961 no B60 . C61 4_555 1.641(4) yes B60 . C75 4_555 1.641(4) yes B60 . C61 . 1.641(4) yes B60 . C75 . 1.641(4) yes C61 . C62 . 1.401(5) yes C61 . C66 . 1.395(4) yes C62 . C63 . 1.392(5) yes C62 . H621 . 0.924 no C63 . C64 . 1.390(5) yes C63 . C67 . 1.499(5) yes C64 . C65 . 1.375(6) yes C64 . H641 . 0.929 no C65 . C66 . 1.392(5) yes C65 . C71 . 1.499(4) yes C66 . H661 . 0.936 no C67 . F68 . 1.333(6) yes C67 . F69 . 1.297(5) yes C67 . F70 . 1.294(5) yes C71 . F72 . 1.347(5) yes C71 . F73 . 1.337(5) yes C71 . F74 . 1.351(4) yes C71 . F721 . 1.313(5) yes C71 . F731 . 1.354(5) yes C71 . F741 . 1.356(5) yes C75 . C76 . 1.394(5) yes C75 . C80 . 1.395(5) yes C76 . C77 . 1.395(5) yes C76 . H761 . 0.933 no C77 . C78 . 1.383(6) yes C77 . C81 . 1.474(4) yes C78 . C79 . 1.386(6) yes C78 . H781 . 0.934 no C79 . C80 . 1.393(5) yes C79 . C85 . 1.487(5) yes C80 . H801 . 0.927 no C81 . F82 . 1.326(6) yes C81 . F83 . 1.355(6) yes C81 . F84 . 1.362(6) yes C81 . F821 . 1.365(5) yes C81 . F831 . 1.342(5) yes C81 . F841 . 1.333(4) yes C85 . F86 . 1.326(5) yes C85 . F87 . 1.342(5) yes C85 . F88 . 1.328(5) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 4_556 Rh1 . H11 4_556 81.4 no C2 4_556 Rh1 . B48 4_556 93.6(5) yes H11 4_556 Rh1 . B48 4_556 87.5 no C2 4_556 Rh1 . C2 . 176.73(19) yes H11 4_556 Rh1 . C2 . 99.3 no B48 4_556 Rh1 . C2 . 89.6(5) yes C2 4_556 Rh1 . B48 . 89.6(5) yes H11 4_556 Rh1 . B48 . 69.1 no B48 4_556 Rh1 . B48 . 18.4(6) yes C2 . Rh1 . B48 . 93.6(5) yes C2 4_556 Rh1 . H11 . 99.3 no H11 4_556 Rh1 . H11 . 156.6 no B48 4_556 Rh1 . H11 . 69.1 no C2 . Rh1 . H11 . 81.4 no B48 . Rh1 . H11 . 87.5 no Rh1 . C2 . N3 . 129.9(3) yes Rh1 . C2 . N6 . 126.0(2) yes N3 . C2 . N6 . 103.9(3) yes C2 . N3 . C4 . 111.0(3) yes C2 . N3 . C7 . 123.5(3) yes C4 . N3 . C7 . 125.4(3) yes N3 . C4 . C5 . 106.8(4) yes N3 . C4 . H41 . 126.4 no C5 . C4 . H41 . 126.8 no C4 . C5 . N6 . 106.9(4) yes C4 . C5 . H51 . 126.6 no N6 . C5 . H51 . 126.5 no C5 . N6 . C2 . 111.3(3) yes C5 . N6 . C16 . 124.9(3) yes C2 . N6 . C16 . 123.8(3) yes N3 . C7 . C8 . 118.9(3) yes N3 . C7 . C12 . 118.4(3) yes C8 . C7 . C12 . 122.7(3) yes C7 . C8 . C9 . 117.0(4) yes C7 . C8 . C13 . 122.1(4) yes C9 . C8 . C13 . 120.9(4) yes C8 . C9 . C10 . 122.6(4) yes C8 . C9 . H91 . 118.9 no C10 . C9 . H91 . 118.5 no C9 . C10 . C11 . 118.1(4) yes C9 . C10 . C14 . 120.6(4) yes C11 . C10 . C14 . 121.3(4) yes C10 . C11 . C12 . 121.9(4) yes C10 . C11 . H111 . 119.5 no C12 . C11 . H111 . 118.6 no C11 . C12 . C7 . 117.6(4) yes C11 . C12 . C15 . 120.9(4) yes C7 . C12 . C15 . 121.5(4) yes C8 . C13 . H131 . 110.2 no C8 . C13 . H132 . 108.2 no H131 . C13 . H132 . 109.9 no C8 . C13 . H133 . 108.9 no H131 . C13 . H133 . 110.1 no H132 . C13 . H133 . 109.5 no C10 . C14 . H141 . 108.7 no C10 . C14 . H142 . 109.2 no H141 . C14 . H142 . 109.8 no C10 . C14 . H143 . 110.2 no H141 . C14 . H143 . 109.4 no H142 . C14 . H143 . 109.7 no C12 . C15 . H153 . 110.0 no C12 . C15 . H152 . 111.1 no H153 . C15 . H152 . 109.3 no C12 . C15 . H151 . 108.7 no H153 . C15 . H151 . 108.0 no H152 . C15 . H151 . 109.6 no N6 . C16 . C17 . 119.0(4) yes N6 . C16 . C21 . 118.5(4) yes C17 . C16 . C21 . 122.5(4) yes C16 . C17 . C18 . 118.1(5) yes C16 . C17 . C22 . 121.6(4) yes C18 . C17 . C22 . 120.2(5) yes C17 . C18 . C19 . 122.0(5) yes C17 . C18 . H181 . 118.9 no C19 . C18 . H181 . 119.1 no C18 . C19 . C20 . 118.3(4) yes C18 . C19 . C23 . 119.8(5) yes C20 . C19 . C23 . 121.9(5) yes C19 . C20 . C21 . 122.8(5) yes C19 . C20 . H201 . 118.8 no C21 . C20 . H201 . 118.4 no C16 . C21 . C20 . 116.3(5) yes C16 . C21 . C24 . 121.9(4) yes C20 . C21 . C24 . 121.7(5) yes C17 . C22 . H221 . 109.8 no C17 . C22 . H222 . 109.2 no H221 . C22 . H222 . 109.9 no C17 . C22 . H223 . 109.0 no H221 . C22 . H223 . 109.7 no H222 . C22 . H223 . 109.3 no C19 . C23 . H231 . 108.8 no C19 . C23 . H232 . 110.7 no H231 . C23 . H232 . 109.0 no C19 . C23 . H233 . 110.5 no H231 . C23 . H233 . 108.3 no H232 . C23 . H233 . 109.4 no C21 . C24 . H241 . 108.7 no C21 . C24 . H242 . 110.8 no H241 . C24 . H242 . 108.8 no C21 . C24 . H243 . 109.6 no H241 . C24 . H243 . 109.8 no H242 . C24 . H243 . 109.2 no Rh1 . B48 . N49 . 132.7(10) yes Rh1 . B48 . H481 . 113.8 no N49 . B48 . H481 . 113.5 no B48 . N49 . C50 . 126.8(16) yes B48 . N49 . C51 . 124.6(9) yes C50 . N49 . C51 . 108.6(16) yes N49 . C50 . H501 . 107.5 no N49 . C50 . H502 . 111.2 no H501 . C50 . H502 . 110.0 no N49 . C50 . H503 . 109.3 no H501 . C50 . H503 . 109.1 no H502 . C50 . H503 . 109.6 no N49 . C51 . H511 . 108.9 no N49 . C51 . H512 . 109.5 no H511 . C51 . H512 . 110.0 no N49 . C51 . H513 . 109.2 no H511 . C51 . H513 . 109.6 no H512 . C51 . H513 . 109.7 no C61 4_555 B60 . C75 4_555 113.20(16) yes C61 4_555 B60 . C61 . 112.1(4) yes C75 4_555 B60 . C61 . 103.53(15) yes C61 4_555 B60 . C75 . 103.53(15) yes C75 4_555 B60 . C75 . 111.6(4) yes C61 . B60 . C75 . 113.20(16) yes B60 . C61 . C62 . 120.8(3) yes B60 . C61 . C66 . 122.6(3) yes C62 . C61 . C66 . 116.1(3) yes C61 . C62 . C63 . 122.2(3) yes C61 . C62 . H621 . 119.0 no C63 . C62 . H621 . 118.8 no C62 . C63 . C64 . 120.4(3) yes C62 . C63 . C67 . 119.7(3) yes C64 . C63 . C67 . 119.9(3) yes C63 . C64 . C65 . 118.2(3) yes C63 . C64 . H641 . 122.1 no C65 . C64 . H641 . 119.7 no C64 . C65 . C66 . 121.4(3) yes C64 . C65 . C71 . 119.9(3) yes C66 . C65 . C71 . 118.5(3) yes C61 . C66 . C65 . 121.6(3) yes C61 . C66 . H661 . 119.5 no C65 . C66 . H661 . 118.9 no C63 . C67 . F68 . 113.6(3) yes C63 . C67 . F69 . 114.7(3) yes F68 . C67 . F69 . 101.4(4) yes C63 . C67 . F70 . 113.1(4) yes F68 . C67 . F70 . 100.7(4) yes F69 . C67 . F70 . 111.9(4) yes C65 . C71 . F72 . 111.7(3) yes C65 . C71 . F73 . 113.1(3) yes F72 . C71 . F73 . 105.61(6) yes C65 . C71 . F74 . 114.5(3) yes F72 . C71 . F74 . 105.52(6) yes F73 . C71 . F74 . 105.72(6) yes C65 . C71 . F721 . 122.0(4) yes C65 . C71 . F731 . 110.6(4) yes F721 . C71 . F731 . 105.65(6) yes C65 . C71 . F741 . 106.2(4) yes F721 . C71 . F741 . 105.68(6) yes F731 . C71 . F741 . 105.63(6) yes B60 . C75 . C76 . 123.7(3) yes B60 . C75 . C80 . 120.6(3) yes C76 . C75 . C80 . 115.4(3) yes C75 . C76 . C77 . 122.3(3) yes C75 . C76 . H761 . 119.9 no C77 . C76 . H761 . 117.8 no C76 . C77 . C78 . 120.8(4) yes C76 . C77 . C81 . 119.3(4) yes C78 . C77 . C81 . 119.8(3) yes C77 . C78 . C79 . 118.5(3) yes C77 . C78 . H781 . 121.5 no C79 . C78 . H781 . 120.0 no C78 . C79 . C80 . 119.8(3) yes C78 . C79 . C85 . 121.1(3) yes C80 . C79 . C85 . 119.1(3) yes C75 . C80 . C79 . 123.2(3) yes C75 . C80 . H801 . 119.7 no C79 . C80 . H801 . 117.1 no C77 . C81 . F82 . 124.6(7) yes C77 . C81 . F83 . 109.3(7) yes F82 . C81 . F83 . 105.63(6) yes C77 . C81 . F84 . 104.7(6) yes F82 . C81 . F84 . 105.64(6) yes F83 . C81 . F84 . 105.62(6) yes C77 . C81 . F821 . 110.6(3) yes C77 . C81 . F831 . 113.4(3) yes F821 . C81 . F831 . 105.65(6) yes C77 . C81 . F841 . 115.1(3) yes F821 . C81 . F841 . 105.61(6) yes F831 . C81 . F841 . 105.68(6) yes C79 . C85 . F86 . 112.6(3) yes C79 . C85 . F87 . 112.2(3) yes F86 . C85 . F87 . 105.4(4) yes C79 . C85 . F88 . 113.1(4) yes F86 . C85 . F88 . 106.7(3) yes F87 . C85 . F88 . 106.3(3) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C15 . H151 . N49 4_556 143 0.97 2.38 3.211(7) yes C22 . H223 . C51 4_556 168 0.96 2.43 3.375(7) yes C50 . H502 . C51 4_556 123 0.96 2.18 2.824(7) yes data_3-Neutron _database_code_depnum_ccdc_archive 'CCDC 880794' #TrackingRef 'CrystallographicData.cif' #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; . ; _chemical_name_common . _chemical_melting_point 'not measured' _chemical_formula_moiety 'C44 H57 B N5 Rh, C32 H12 B F24' _chemical_formula_sum 'C76 H69 B2 F24 N5 Rh' _chemical_formula_weight 1632.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0000 -0.2130 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/n ' _symmetry_space_group_name_Hall '-P 2yac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 12.7649(2) _cell_length_b 14.1705(2) _cell_length_c 21.1902(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.2840(10) _cell_angle_gamma 90.00 _cell_volume 3826.70(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used . _cell_measurement_theta_min . _cell_measurement_theta_max . _exptl_crystal_description block _exptl_crystal_colour clear_intense_yellow _exptl_crystal_size_max 5.00 _exptl_crystal_size_mid 3.00 _exptl_crystal_size_min 2.00 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5042 _exptl_absorpt_correction_T_max 0.7420 _exptl_absorpt_process_details ; Calculated using custom ISIS software program SXD-2001. ; _exptl_special_details ; For peak integration a local UB matrix refined for each frame, using approximately 100 reflections per run from each of the 11 detectors. For final cell dimensions a weighted average of all local cells was calculated. Because of the nature of the experiment, it is not possible to give values of theta_min and theta_max for the cell determination. The same applies for the wavelength used for the experiment. The range of wavelengths used was 0.48-7.0 Angstroms, but the bulk of the diffraction information is obtained from wavelengths in the range 0.7-2.5 Angstroms. The data collection procedures on the SXD instrument used for the single crystal neutron data collection are most recently summarised in the Appendix to the following paper Wilson, C.C. (1997). J. Mol. Struct. 405, 207-217 ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength Laue _diffrn_radiation_type Neutron _diffrn_radiation_source 'ISIS spallation neutron source' _diffrn_radiation_monochromator none _diffrn_measurement_device_type 'SXD at ISIS neutron source' _diffrn_measurement_method 'time-of-flight Laue diffraction' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7166 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 8.09 _diffrn_reflns_theta_max 83.06 _reflns_number_total 7166 _reflns_number_gt 7166 _reflns_threshold_expression >2sigma(I) _computing_data_collection SXD2001 _computing_cell_refinement SXD2001 _computing_data_reduction SXD2001 _computing_structure_solution 'Refinement of known model' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics . _computing_publication_material . _refine_special_details ; Refining hydrogen atoms using isotropic displacement parameters leads to a poor data to parameter ratio. The nature of the sample, time constraints and other experimental considerations meant it was not possible to collect more data, so extensive restraints were used. Thermal similarity and vibrational restraints were used to maintain sensible displacement ellipsoids; same distance restraints were also used to maintain sensible geometries for the methyl groups and trifluoromethyl groups . 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. The variable wavelength nature of the data collection procedure means that sensible values of _diffrn_reflns_theta_min & _diffrn_reflns_theta_max cannot be given. _refine_diff_density_max/min is given in Fermi per per angstrom cubed not electons per angstrom cubed. Another way to consider the _refine_diff_density_ is as a percentage of the diffracted intensity of a given atom: _refine_diff_density_max = 10.2% of Carbon _refine_diff_density_min = -9.8% of Carbon ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1764P)^2^+93.0533P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Refinement of known model' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment anisotropic _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00334(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7166 _refine_ls_number_parameters 820 _refine_ls_number_restraints 1200 _refine_ls_R_factor_all 0.0944 _refine_ls_R_factor_gt 0.0944 _refine_ls_wR_factor_ref 0.2349 _refine_ls_wR_factor_gt 0.2349 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.086 _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 Rh1 Rh 0.2500 0.1549(5) 0.7500 0.0253(16) Uani 1 2 d SU . . H1 H 0.2472(18) 0.149(2) 0.8160(12) 0.170(11) Uani 1 1 d . . . C2 C 0.4096(4) 0.1599(4) 0.7531(2) 0.0327(12) Uani 1 1 d . A . N3 N 0.4811(3) 0.1214(3) 0.79637(17) 0.0386(10) Uani 1 1 d . . . C4 C 0.5835(5) 0.1457(5) 0.7827(3) 0.0571(18) Uani 1 1 d . A . H4 H 0.6500(10) 0.1229(12) 0.8124(7) 0.086(5) Uani 1 1 d . . . C5 C 0.5761(5) 0.1992(5) 0.7302(3) 0.063(2) Uani 1 1 d . . . H5 H 0.6355(11) 0.2344(14) 0.7025(7) 0.094(5) Uani 1 1 d . . . N6 N 0.4702(3) 0.2073(3) 0.71303(19) 0.0446(10) Uani 1 1 d . A . C7 C 0.4533(4) 0.0645(4) 0.8479(2) 0.0324(12) Uani 1 1 d . A . C8 C 0.4117(5) 0.1064(4) 0.9012(2) 0.0439(14) Uani 1 1 d U . . C9 C 0.3807(5) 0.0486(4) 0.9491(3) 0.0481(15) Uani 1 1 d . A . H9 H 0.3471(14) 0.0818(12) 0.9896(6) 0.098(6) Uani 1 1 d . . . C10 C 0.3908(5) -0.0481(4) 0.9465(3) 0.0488(15) Uani 1 1 d U . . C11 C 0.4353(5) -0.0884(5) 0.8939(3) 0.0436(15) Uani 1 1 d . A . H11 H 0.4471(13) -0.1656(11) 0.8917(6) 0.081(4) Uani 1 1 d . . . C12 C 0.4678(5) -0.0325(4) 0.8449(3) 0.0480(16) Uani 1 1 d U . . C13 C 0.3986(6) 0.2147(5) 0.9055(3) 0.069(2) Uani 1 1 d DU A . H13A H 0.4594(13) 0.2515(12) 0.8868(8) 0.116(4) Uani 1 1 d DU . . H13B H 0.3307(11) 0.2376(13) 0.8797(8) 0.115(4) Uani 1 1 d DU . . H13C H 0.3889(15) 0.2336(12) 0.9514(6) 0.116(4) Uani 1 1 d DU . . C14 C 0.3509(6) -0.1121(5) 0.9982(3) 0.0641(19) Uani 1 1 d DU A . H14A H 0.3752(13) -0.0866(10) 1.0433(5) 0.101(4) Uani 1 1 d DU . . H14B H 0.2688(9) -0.1131(12) 0.9976(8) 0.108(4) Uani 1 1 d DU . . H14C H 0.3762(14) -0.1809(9) 0.9959(8) 0.111(4) Uani 1 1 d DU . . C15 C 0.5183(6) -0.0756(5) 0.7883(3) 0.072(2) Uani 1 1 d DU A . H15A H 0.4790(13) -0.0556(11) 0.7463(6) 0.101(4) Uani 1 1 d DU . . H15B H 0.5954(10) -0.0559(12) 0.7857(8) 0.104(4) Uani 1 1 d DU . . H15C H 0.5154(13) -0.1488(8) 0.7907(7) 0.101(4) Uani 1 1 d DU . . C16 C 0.4280(5) 0.2574(4) 0.6582(3) 0.0475(15) Uani 1 1 d . . . C17 C 0.4222(7) 0.2139(6) 0.6005(3) 0.086(3) Uani 1 1 d U A . C18 C 0.3836(7) 0.2665(6) 0.5489(3) 0.081(3) Uani 1 1 d . . . H18 H 0.380(2) 0.2339(18) 0.5021(7) 0.149(11) Uani 1 1 d . . . C19 C 0.3463(5) 0.3561(5) 0.5543(3) 0.062(2) Uani 1 1 d U A . C20 C 0.3492(7) 0.3983(6) 0.6137(3) 0.068(2) Uani 1 1 d . . . H20 H 0.319(2) 0.4696(15) 0.6197(9) 0.119(7) Uani 1 1 d . . . C21 C 0.3900(6) 0.3503(5) 0.6672(3) 0.0583(17) Uani 1 1 d U A . C22 C 0.4815(11) 0.1267(8) 0.5907(4) 0.148(4) Uani 1 1 d DU . . H22A H 0.491(2) 0.0796(13) 0.6274(7) 0.171(6) Uani 1 1 d DU . . H22B H 0.455(2) 0.0902(14) 0.5504(7) 0.170(6) Uani 1 1 d DU . . H22C H 0.5550(14) 0.1527(18) 0.5814(12) 0.177(6) Uani 1 1 d DU . . C23 C 0.2992(7) 0.4106(6) 0.4969(4) 0.092(3) Uani 1 1 d DU . . H23A H 0.3365(15) 0.3984(14) 0.4567(6) 0.149(5) Uani 1 1 d DU . . H23B H 0.2204(11) 0.3905(17) 0.4871(9) 0.150(5) Uani 1 1 d DU . . H23C H 0.293(2) 0.4819(10) 0.5062(8) 0.149(5) Uani 1 1 d DU . . C24 C 0.3976(9) 0.3977(6) 0.7328(4) 0.103(3) Uani 1 1 d DU . . H24A H 0.3681(16) 0.4659(10) 0.7299(8) 0.128(4) Uani 1 1 d DU . . H24B H 0.3583(16) 0.3604(11) 0.7650(7) 0.127(4) Uani 1 1 d DU . . H24C H 0.4752(11) 0.4018(14) 0.7489(9) 0.131(4) Uani 1 1 d DU . . B48 B 0.2453(15) 0.0182(9) 0.7352(6) 0.049(4) Uiso 0.50 1 d PU A -1 H48 H 0.280(2) -0.004(2) 0.6711(13) 0.063(6) Uiso 0.50 1 d PU B -1 N49 N 0.2216(8) -0.0579(8) 0.7733(5) 0.066(3) Uiso 0.50 1 d PDU A -1 C50 C 0.2251(12) -0.1575(11) 0.7503(9) 0.097(5) Uiso 0.50 1 d PDU A -1 H50A H 0.237(3) -0.162(2) 0.7011(10) 0.126(8) Uiso 0.50 1 d PDU C -1 H50B H 0.2880(19) -0.1957(17) 0.7710(16) 0.116(9) Uiso 0.50 1 d PDU D -1 H50C H 0.1580(18) -0.1963(18) 0.7569(16) 0.123(8) Uiso 0.50 1 d PDU E -1 C51 C 0.1821(12) -0.0422(10) 0.8389(7) 0.078(4) Uiso 0.50 1 d PDU A -1 H51A H 0.182(2) 0.0250(13) 0.8596(16) 0.100(7) Uiso 0.50 1 d PDU F -1 H51B H 0.1047(15) -0.066(2) 0.8391(15) 0.103(7) Uiso 0.50 1 d PDU G -1 H51C H 0.225(2) -0.0851(19) 0.8703(14) 0.112(7) Uiso 0.50 1 d PDU H -1 B60 B 0.2500 0.3656(6) 0.2500 0.0226(17) Uani 1 2 d S . . C61 C 0.1880(4) 0.4311(3) 0.2997(2) 0.0258(11) Uani 1 1 d . . . C62 C 0.2328(4) 0.5141(3) 0.3261(2) 0.0258(11) Uani 1 1 d . . . H62 H 0.3079(9) 0.5371(8) 0.3087(5) 0.053(3) Uani 1 1 d . . . C63 C 0.1880(4) 0.5632(3) 0.3742(2) 0.0281(11) Uani 1 1 d . . . C64 C 0.0947(4) 0.5343(4) 0.3986(3) 0.0359(13) Uani 1 1 d . . . H64A H 0.0604(11) 0.5714(10) 0.4348(6) 0.064(3) Uani 1 1 d . . . C65 C 0.0469(4) 0.4523(4) 0.3727(2) 0.0359(13) Uani 1 1 d U I . C66 C 0.0941(4) 0.4011(4) 0.3256(2) 0.0306(12) Uani 1 1 d . . . H66 H 0.0581(9) 0.3369(10) 0.3080(6) 0.062(4) Uani 1 1 d . . . C67 C 0.2434(5) 0.6490(4) 0.4020(2) 0.0442(15) Uani 1 1 d D . . F68 F 0.3474(7) 0.6403(7) 0.4040(6) 0.104(4) Uani 1 1 d D . . F69 F 0.2223(9) 0.6662(7) 0.4599(4) 0.096(4) Uani 1 1 d D . . F70 F 0.2260(12) 0.7245(7) 0.3675(6) 0.118(5) Uani 1 1 d D . . C71 C -0.0511(5) 0.4158(5) 0.3998(3) 0.0607(17) Uani 1 1 d DU . . F72 F -0.0260(9) 0.3566(10) 0.4499(6) 0.085(4) Uani 0.752(17) 1 d PDU I 1 F73 F -0.1087(10) 0.4811(9) 0.4245(7) 0.086(4) Uani 0.752(17) 1 d PDU I 1 F74 F -0.1071(9) 0.3615(10) 0.3609(5) 0.078(4) Uani 0.752(17) 1 d PDU I 1 F721 F -0.053(3) 0.3275(12) 0.4174(18) 0.078(4) Uiso 0.248(17) 1 d PDU I 2 F731 F -0.079(4) 0.468(2) 0.4478(12) 0.078(4) Uiso 0.248(17) 1 d PDU I 2 F741 F -0.122(2) 0.430(3) 0.3527(12) 0.078(4) Uiso 0.248(17) 1 d PDU I 2 C75 C 0.1715(4) 0.3007(4) 0.2042(2) 0.0280(11) Uani 1 1 d . . . C76 C 0.0705(4) 0.3303(4) 0.1823(2) 0.0355(12) Uani 1 1 d . . . H76 H 0.0403(10) 0.3955(9) 0.1984(6) 0.058(3) Uani 1 1 d . . . C77 C 0.0099(5) 0.2750(4) 0.1393(3) 0.0439(14) Uani 1 1 d U J . C78 C 0.0460(5) 0.1897(4) 0.1165(2) 0.0436(15) Uani 1 1 d . . . H78 H -0.0016(11) 0.1477(10) 0.0833(6) 0.073(4) Uani 1 1 d . . . C79 C 0.1478(4) 0.1612(4) 0.1366(2) 0.0331(12) Uani 1 1 d . . . C80 C 0.2078(5) 0.2164(4) 0.1792(2) 0.0293(12) Uani 1 1 d . . . H80 H 0.2869(10) 0.1913(8) 0.1929(5) 0.046(3) Uani 1 1 d . . . C81 C -0.0950(6) 0.3132(5) 0.1157(3) 0.0767(19) Uani 1 1 d DU . . F82 F -0.104(5) 0.333(5) 0.0541(10) 0.085(5) Uiso 0.15(2) 1 d PDU J 1 F83 F -0.136(5) 0.386(3) 0.145(3) 0.085(5) Uiso 0.15(2) 1 d PDU J 1 F84 F -0.161(4) 0.241(3) 0.124(3) 0.085(5) Uiso 0.15(2) 1 d PDU J 1 F821 F -0.0824(11) 0.3824(10) 0.0721(6) 0.097(4) Uani 0.85(2) 1 d PDU J 2 F831 F -0.1479(9) 0.3505(10) 0.1612(5) 0.081(3) Uani 0.85(2) 1 d PDU J 2 F841 F -0.1536(10) 0.2490(8) 0.0858(8) 0.099(4) Uani 0.85(2) 1 d PDU J 2 C85 C 0.1924(4) 0.0704(4) 0.1135(2) 0.0424(14) Uani 1 1 d D . . F86 F 0.1919(7) 0.0023(5) 0.1563(4) 0.062(2) Uani 1 1 d D . . F87 F 0.2924(6) 0.0805(6) 0.0998(4) 0.075(3) Uani 1 1 d D . . F88 F 0.1413(7) 0.0383(6) 0.0609(3) 0.063(2) Uani 1 1 d 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 Rh1 0.027(4) 0.021(4) 0.027(4) 0.000 -0.003(3) 0.000 H1 0.102(18) 0.28(4) 0.124(18) 0.02(2) 0.013(14) 0.043(19) C2 0.027(3) 0.038(3) 0.032(3) 0.009(2) -0.007(2) 0.000(2) N3 0.033(2) 0.050(2) 0.033(2) 0.0127(18) -0.0029(16) 0.0018(18) C4 0.039(4) 0.083(5) 0.048(4) 0.032(3) -0.010(3) 0.002(3) H4 0.028(7) 0.133(13) 0.094(10) 0.028(9) -0.018(7) -0.011(7) C5 0.027(4) 0.101(6) 0.061(4) 0.037(4) 0.002(3) -0.004(3) H5 0.041(8) 0.161(16) 0.079(10) 0.058(10) 0.001(7) -0.023(8) N6 0.032(2) 0.062(3) 0.040(2) 0.023(2) -0.0026(16) -0.0007(19) C7 0.038(3) 0.040(3) 0.019(2) 0.005(2) -0.002(2) 0.005(2) C8 0.063(4) 0.038(3) 0.030(3) -0.003(2) 0.004(3) -0.007(3) C9 0.070(4) 0.047(4) 0.028(3) -0.003(3) 0.012(3) -0.007(3) H9 0.144(15) 0.107(13) 0.048(8) -0.036(8) 0.049(9) 0.000(10) C10 0.066(4) 0.049(4) 0.031(3) 0.010(3) 0.006(3) -0.002(3) C11 0.059(4) 0.037(4) 0.035(3) 0.003(3) 0.005(3) 0.008(3) H11 0.131(14) 0.051(9) 0.062(8) 0.018(7) 0.020(8) 0.002(8) C12 0.067(4) 0.045(4) 0.033(3) 0.009(3) 0.007(3) 0.021(3) C13 0.109(6) 0.037(4) 0.064(4) -0.009(3) 0.022(4) -0.009(4) H13A 0.152(10) 0.069(8) 0.129(9) -0.004(8) 0.036(9) -0.012(8) H13B 0.153(9) 0.071(7) 0.124(8) -0.008(7) 0.027(8) -0.004(8) H13C 0.168(11) 0.067(8) 0.115(9) -0.021(8) 0.027(9) -0.004(8) C14 0.095(5) 0.055(4) 0.043(4) 0.016(3) 0.009(4) -0.018(4) H14A 0.153(10) 0.093(8) 0.060(7) 0.015(6) 0.028(7) -0.023(7) H14B 0.144(10) 0.098(8) 0.085(8) 0.021(6) 0.025(7) -0.029(7) H14C 0.163(10) 0.088(8) 0.083(7) 0.021(7) 0.033(7) -0.016(7) C15 0.105(6) 0.068(5) 0.045(4) -0.004(4) 0.021(4) 0.036(4) H15A 0.140(9) 0.097(8) 0.069(7) -0.010(6) 0.026(7) 0.023(7) H15B 0.133(9) 0.100(8) 0.084(7) -0.008(6) 0.036(7) 0.025(7) H15C 0.131(9) 0.095(8) 0.080(7) -0.010(7) 0.026(7) 0.029(7) C16 0.045(4) 0.058(4) 0.039(3) 0.014(3) 0.004(3) 0.003(3) C17 0.132(7) 0.102(6) 0.023(3) 0.007(3) 0.004(4) 0.081(5) C18 0.115(7) 0.101(7) 0.028(4) 0.003(4) 0.007(4) 0.059(5) H18 0.22(2) 0.20(2) 0.031(8) 0.020(10) 0.013(10) 0.134(19) C19 0.071(5) 0.078(5) 0.040(3) 0.035(3) 0.016(3) 0.022(4) C20 0.095(6) 0.051(5) 0.057(5) 0.018(4) -0.005(4) 0.006(4) H20 0.17(2) 0.083(13) 0.102(14) 0.007(10) -0.002(13) 0.043(13) C21 0.077(5) 0.044(4) 0.053(4) 0.010(3) -0.007(3) 0.000(3) C22 0.265(11) 0.118(7) 0.055(5) -0.016(5) -0.041(6) 0.147(7) H22A 0.288(14) 0.132(10) 0.087(8) -0.010(8) -0.044(9) 0.135(10) H22B 0.286(14) 0.135(10) 0.084(8) -0.024(8) -0.038(9) 0.130(10) H22C 0.288(14) 0.140(10) 0.096(9) -0.016(8) -0.041(9) 0.131(10) C23 0.119(7) 0.117(7) 0.042(4) 0.045(4) 0.012(4) 0.048(5) H23A 0.176(11) 0.199(11) 0.072(7) 0.074(8) 0.004(8) 0.064(9) H23B 0.171(11) 0.196(11) 0.081(8) 0.071(8) -0.008(8) 0.050(9) H23C 0.178(11) 0.189(11) 0.078(8) 0.064(8) -0.008(8) 0.054(9) C24 0.180(9) 0.067(6) 0.058(5) -0.007(4) -0.010(5) 0.018(6) H24A 0.198(11) 0.104(9) 0.078(7) -0.025(7) -0.017(8) 0.017(8) H24B 0.200(11) 0.104(9) 0.075(7) -0.027(7) -0.016(8) 0.016(8) H24C 0.197(11) 0.107(9) 0.087(8) -0.034(7) -0.024(9) 0.014(8) B60 0.017(4) 0.029(5) 0.022(4) 0.000 0.001(3) 0.000 C61 0.026(3) 0.032(3) 0.020(2) 0.004(2) 0.011(2) 0.001(2) C62 0.027(3) 0.031(3) 0.020(2) 0.001(2) 0.007(2) -0.002(2) H62 0.049(7) 0.070(8) 0.042(6) -0.014(5) 0.020(5) -0.025(5) C63 0.039(3) 0.026(3) 0.020(2) 0.001(2) 0.008(2) 0.006(2) C64 0.035(3) 0.047(4) 0.026(3) 0.004(3) 0.009(2) 0.007(2) H64A 0.068(9) 0.069(9) 0.057(7) -0.011(7) 0.027(7) 0.002(6) C65 0.030(3) 0.049(3) 0.031(3) -0.003(2) 0.014(2) 0.001(2) C66 0.023(3) 0.044(4) 0.026(3) 0.000(2) 0.005(2) -0.005(2) H66 0.057(8) 0.074(9) 0.058(7) -0.018(7) 0.030(6) -0.031(7) C67 0.066(4) 0.033(3) 0.036(3) -0.012(3) 0.018(3) -0.005(3) F68 0.067(7) 0.081(7) 0.165(11) -0.066(7) 0.010(7) -0.013(5) F69 0.142(10) 0.087(7) 0.059(5) -0.035(5) 0.023(6) -0.059(7) F70 0.168(13) 0.056(6) 0.122(9) 0.020(6) -0.053(8) -0.038(7) C71 0.043(3) 0.083(4) 0.058(3) -0.017(3) 0.025(3) -0.006(3) F72 0.087(8) 0.108(8) 0.065(6) 0.017(6) 0.032(5) -0.030(6) F73 0.043(7) 0.116(7) 0.102(8) -0.020(6) 0.038(6) 0.011(5) F74 0.053(6) 0.104(9) 0.082(6) -0.016(6) 0.031(5) -0.031(5) C75 0.028(3) 0.037(3) 0.019(2) 0.004(2) 0.0021(19) -0.003(2) C76 0.035(3) 0.036(3) 0.034(3) 0.000(2) -0.012(2) 0.012(2) H76 0.055(8) 0.055(8) 0.064(8) -0.022(6) -0.012(6) 0.016(6) C77 0.051(3) 0.043(3) 0.035(3) -0.010(2) -0.019(2) 0.010(2) C78 0.053(4) 0.051(4) 0.026(3) -0.010(3) -0.012(3) -0.008(3) H78 0.072(9) 0.079(9) 0.063(8) -0.018(7) -0.034(7) -0.006(7) C79 0.040(3) 0.034(3) 0.025(2) -0.002(2) 0.002(2) -0.006(2) C80 0.033(3) 0.033(3) 0.023(2) -0.004(2) 0.009(2) -0.008(2) H80 0.040(7) 0.049(7) 0.049(6) -0.015(5) -0.001(5) 0.006(5) C81 0.068(4) 0.081(4) 0.076(4) -0.014(3) -0.041(3) 0.018(3) F821 0.123(9) 0.083(7) 0.082(7) 0.010(6) -0.040(6) 0.041(6) F831 0.046(6) 0.095(8) 0.100(7) 0.002(6) -0.021(5) 0.029(6) F841 0.073(7) 0.098(7) 0.121(9) -0.019(6) -0.052(6) 0.023(5) C85 0.046(4) 0.047(4) 0.035(3) -0.018(3) 0.010(3) -0.012(3) F86 0.082(6) 0.054(5) 0.049(4) -0.005(4) 0.000(4) 0.016(4) F87 0.062(6) 0.081(6) 0.087(6) -0.054(5) 0.035(5) -0.019(4) F88 0.080(6) 0.059(5) 0.048(4) -0.027(4) -0.003(4) -0.007(4) _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 Rh1 B48 1.963(15) 2_556 ? Rh1 B48 1.963(15) . ? Rh1 C2 2.036(5) . ? Rh1 C2 2.036(5) 2_556 ? Rh1 H1 1.40(2) . ? C2 N6 1.358(6) . ? C2 N3 1.369(6) . ? N3 C4 1.398(7) . ? N3 C7 1.420(6) . ? C4 C5 1.345(9) . ? C4 H4 1.077(17) . ? C5 N6 1.386(8) . ? C5 H5 1.104(15) . ? N6 C16 1.439(7) . ? C7 C12 1.389(8) . ? C7 C8 1.407(7) . ? C8 C9 1.380(8) . ? C8 C13 1.547(9) . ? C9 C10 1.377(8) . ? C9 H9 1.089(14) . ? C10 C11 1.402(8) . ? C10 C14 1.530(9) . ? C11 C12 1.389(8) . ? C11 H11 1.106(19) . ? C12 C15 1.522(9) . ? C13 H13A 1.033(13) . ? C13 H13B 1.049(14) . ? C13 H13C 1.023(13) . ? C14 H14A 1.052(12) . ? C14 H14B 1.048(13) . ? C14 H14C 1.029(13) . ? C15 H15A 1.035(13) . ? C15 H15B 1.027(13) . ? C15 H15C 1.039(13) . ? C16 C17 1.368(9) . ? C16 C21 1.420(9) . ? C17 C18 1.389(9) . ? C17 C22 1.470(11) . ? C18 C19 1.363(10) . ? C18 H18 1.09(2) . ? C19 C20 1.393(10) . ? C19 C23 1.533(10) . ? C20 C21 1.396(9) . ? C20 H20 1.09(3) . ? C21 C24 1.542(11) . ? C22 H22A 1.027(13) . ? C22 H22B 1.039(13) . ? C22 H22C 1.038(14) . ? C23 H23A 1.014(13) . ? C23 H23B 1.054(14) . ? C23 H23C 1.034(14) . ? C24 H24A 1.038(13) . ? C24 H24B 1.018(14) . ? C24 H24C 1.031(14) . ? B48 N49 1.391(17) . ? B48 H48 1.49(3) . ? N49 C50 1.49(2) . ? N49 C51 1.522(18) . ? C50 H50A 1.063(15) . ? C50 H50B 1.043(15) . ? C50 H50C 1.034(15) . ? C51 H51A 1.049(15) . ? C51 H51B 1.046(15) . ? C51 H51C 1.036(15) . ? B60 C75 1.637(7) . ? B60 C75 1.637(7) 2 ? B60 C61 1.641(6) 2 ? B60 C61 1.641(6) . ? C61 C62 1.409(7) . ? C61 C66 1.413(6) . ? C62 C63 1.384(6) . ? C62 H62 1.096(12) . ? C63 C64 1.388(7) . ? C63 C67 1.508(8) . ? C64 C65 1.408(8) . ? C64 H64A 1.048(16) . ? C65 C66 1.398(7) . ? C65 C71 1.499(8) . ? C66 H66 1.076(16) . ? C67 F69 1.295(8) . ? C67 F70 1.307(10) . ? C67 F68 1.333(9) . ? C71 F721 1.305(14) . ? C71 F74 1.309(10) . ? C71 F73 1.309(10) . ? C71 F741 1.326(14) . ? C71 F731 1.327(14) . ? C71 F72 1.376(10) . ? C75 C80 1.397(7) . ? C75 C76 1.409(7) . ? C76 C77 1.400(8) . ? C76 H76 1.066(15) . ? C77 C78 1.390(8) . ? C77 C81 1.503(9) . ? C78 C79 1.403(8) . ? C78 H78 1.081(14) . ? C79 C80 1.391(7) . ? C79 C85 1.500(8) . ? C80 H80 1.093(16) . ? C81 F841 1.317(10) . ? C81 F831 1.320(10) . ? C81 F83 1.331(16) . ? C81 F82 1.333(16) . ? C81 F84 1.347(16) . ? C81 F821 1.363(10) . ? C85 F86 1.323(9) . ? C85 F87 1.334(8) . ? C85 F88 1.338(8) . ? 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 B48 Rh1 B48 18.5(8) 2_556 . ? B48 Rh1 C2 90.5(6) 2_556 . ? B48 Rh1 C2 93.5(6) . . ? B48 Rh1 C2 93.5(6) 2_556 2_556 ? B48 Rh1 C2 90.5(6) . 2_556 ? C2 Rh1 C2 176.0(5) . 2_556 ? B48 Rh1 H1 77.4(15) 2_556 . ? B48 Rh1 H1 95.5(15) . . ? C2 Rh1 H1 93.0(10) . . ? C2 Rh1 H1 87.2(10) 2_556 . ? N6 C2 N3 103.6(4) . . ? N6 C2 Rh1 127.0(4) . . ? N3 C2 Rh1 129.4(4) . . ? C2 N3 C4 111.0(4) . . ? C2 N3 C7 123.7(4) . . ? C4 N3 C7 125.2(4) . . ? C5 C4 N3 106.7(5) . . ? C5 C4 H4 131.9(9) . . ? N3 C4 H4 121.4(9) . . ? C4 C5 N6 106.6(5) . . ? C4 C5 H5 132.6(10) . . ? N6 C5 H5 120.8(9) . . ? C2 N6 C5 112.1(4) . . ? C2 N6 C16 123.3(4) . . ? C5 N6 C16 124.6(4) . . ? C12 C7 C8 120.8(4) . . ? C12 C7 N3 119.2(4) . . ? C8 C7 N3 120.0(5) . . ? C9 C8 C7 118.4(5) . . ? C9 C8 C13 120.6(5) . . ? C7 C8 C13 120.9(5) . . ? C10 C9 C8 122.1(5) . . ? C10 C9 H9 120.2(11) . . ? C8 C9 H9 117.7(11) . . ? C9 C10 C11 118.7(5) . . ? C9 C10 C14 121.7(5) . . ? C11 C10 C14 119.6(6) . . ? C12 C11 C10 120.9(6) . . ? C12 C11 H11 119.1(8) . . ? C10 C11 H11 120.0(8) . . ? C11 C12 C7 119.0(5) . . ? C11 C12 C15 121.3(6) . . ? C7 C12 C15 119.8(5) . . ? C8 C13 H13A 113.0(11) . . ? C8 C13 H13B 111.4(11) . . ? H13A C13 H13B 105.1(13) . . ? C8 C13 H13C 109.5(11) . . ? H13A C13 H13C 111.6(13) . . ? H13B C13 H13C 105.9(13) . . ? C10 C14 H14A 110.8(9) . . ? C10 C14 H14B 111.9(9) . . ? H14A C14 H14B 105.0(12) . . ? C10 C14 H14C 114.2(10) . . ? H14A C14 H14C 106.9(12) . . ? H14B C14 H14C 107.6(12) . . ? C12 C15 H15A 111.2(9) . . ? C12 C15 H15B 112.5(10) . . ? H15A C15 H15B 107.4(12) . . ? C12 C15 H15C 110.0(9) . . ? H15A C15 H15C 107.4(12) . . ? H15B C15 H15C 108.1(12) . . ? C17 C16 C21 122.4(5) . . ? C17 C16 N6 119.9(5) . . ? C21 C16 N6 117.6(5) . . ? C16 C17 C18 117.4(6) . . ? C16 C17 C22 120.2(6) . . ? C18 C17 C22 120.1(6) . . ? C19 C18 C17 123.0(7) . . ? C19 C18 H18 118.1(11) . . ? C17 C18 H18 118.8(12) . . ? C18 C19 C20 118.9(6) . . ? C18 C19 C23 121.7(7) . . ? C20 C19 C23 119.4(6) . . ? C19 C20 C21 121.0(7) . . ? C19 C20 H20 120.6(12) . . ? C21 C20 H20 118.4(13) . . ? C20 C21 C16 117.2(6) . . ? C20 C21 C24 121.3(7) . . ? C16 C21 C24 121.4(6) . . ? C17 C22 H22A 118.5(13) . . ? C17 C22 H22B 112.8(12) . . ? H22A C22 H22B 108.6(14) . . ? C17 C22 H22C 101.9(13) . . ? H22A C22 H22C 108.0(14) . . ? H22B C22 H22C 106.1(14) . . ? C19 C23 H23A 113.5(11) . . ? C19 C23 H23B 110.3(10) . . ? H23A C23 H23B 106.2(14) . . ? C19 C23 H23C 111.8(11) . . ? H23A C23 H23C 111.7(14) . . ? H23B C23 H23C 102.7(14) . . ? C21 C24 H24A 110.4(11) . . ? C21 C24 H24B 111.8(11) . . ? H24A C24 H24B 109.4(13) . . ? C21 C24 H24C 109.5(11) . . ? H24A C24 H24C 107.8(14) . . ? H24B C24 H24C 107.9(14) . . ? N49 B48 Rh1 132.7(10) . . ? N49 B48 H48 116.7(15) . . ? Rh1 B48 H48 110.5(14) . . ? B48 N49 C50 122.1(11) . . ? B48 N49 C51 120.8(10) . . ? C50 N49 C51 116.9(10) . . ? N49 C50 H50A 112.7(15) . . ? N49 C50 H50B 113.0(16) . . ? H50A C50 H50B 103.4(17) . . ? N49 C50 H50C 114.7(16) . . ? H50A C50 H50C 105.2(18) . . ? H50B C50 H50C 106.9(17) . . ? N49 C51 H51A 122(2) . . ? N49 C51 H51B 109(2) . . ? H51A C51 H51B 105.5(17) . . ? N49 C51 H51C 108(2) . . ? H51A C51 H51C 106.2(17) . . ? H51B C51 H51C 105.7(17) . . ? C75 B60 C75 111.6(6) . 2 ? C75 B60 C61 103.8(2) . 2 ? C75 B60 C61 113.4(2) 2 2 ? C75 B60 C61 113.4(2) . . ? C75 B60 C61 103.8(2) 2 . ? C61 B60 C61 111.1(6) 2 . ? C62 C61 C66 115.5(4) . . ? C62 C61 B60 121.8(4) . . ? C66 C61 B60 122.1(5) . . ? C63 C62 C61 122.4(4) . . ? C63 C62 H62 120.3(7) . . ? C61 C62 H62 117.2(7) . . ? C62 C63 C64 121.7(5) . . ? C62 C63 C67 119.3(4) . . ? C64 C63 C67 119.1(4) . . ? C63 C64 C65 117.5(5) . . ? C63 C64 H64A 121.9(9) . . ? C65 C64 H64A 120.6(9) . . ? C66 C65 C64 120.7(5) . . ? C66 C65 C71 119.9(5) . . ? C64 C65 C71 119.2(4) . . ? C65 C66 C61 122.1(5) . . ? C65 C66 H66 119.6(7) . . ? C61 C66 H66 118.3(6) . . ? F69 C67 F70 109.7(9) . . ? F69 C67 F68 104.3(9) . . ? F70 C67 F68 103.4(9) . . ? F69 C67 C63 113.8(6) . . ? F70 C67 C63 112.4(7) . . ? F68 C67 C63 112.5(6) . . ? F721 C71 F74 66.4(16) . . ? F721 C71 F73 123.1(19) . . ? F74 C71 F73 111.6(9) . . ? F721 C71 F741 109.7(14) . . ? F74 C71 F741 44.6(15) . . ? F73 C71 F741 79.6(16) . . ? F721 C71 F731 108.2(14) . . ? F74 C71 F731 131(2) . . ? F73 C71 F731 27.6(16) . . ? F741 C71 F731 106.9(14) . . ? F721 C71 F72 37.2(15) . . ? F74 C71 F72 102.8(8) . . ? F73 C71 F72 103.5(8) . . ? F741 C71 F72 142.3(18) . . ? F731 C71 F72 79.2(15) . . ? F721 C71 C65 117.8(18) . . ? F74 C71 C65 113.5(6) . . ? F73 C71 C65 114.2(8) . . ? F741 C71 C65 102.1(18) . . ? F731 C71 C65 112(2) . . ? F72 C71 C65 110.1(7) . . ? C80 C75 C76 116.5(5) . . ? C80 C75 B60 120.0(4) . . ? C76 C75 B60 123.1(5) . . ? C77 C76 C75 120.6(5) . . ? C77 C76 H76 119.8(8) . . ? C75 C76 H76 119.6(8) . . ? C78 C77 C76 122.1(5) . . ? C78 C77 C81 120.3(5) . . ? C76 C77 C81 117.6(5) . . ? C77 C78 C79 117.6(5) . . ? C77 C78 H78 121.3(9) . . ? C79 C78 H78 121.0(9) . . ? C80 C79 C78 120.1(5) . . ? C80 C79 C85 119.2(5) . . ? C78 C79 C85 120.7(5) . . ? C79 C80 C75 122.9(5) . . ? C79 C80 H80 117.1(7) . . ? C75 C80 H80 120.0(7) . . ? F841 C81 F831 109.1(9) . . ? F841 C81 F83 122(3) . . ? F831 C81 F83 28(3) . . ? F841 C81 F82 70(3) . . ? F831 C81 F82 128(3) . . ? F83 C81 F82 106.4(17) . . ? F841 C81 F84 36(3) . . ? F831 C81 F84 82(3) . . ? F83 C81 F84 105.5(16) . . ? F82 C81 F84 105.2(16) . . ? F841 C81 F821 104.8(8) . . ? F831 C81 F821 107.1(8) . . ? F83 C81 F821 80(3) . . ? F82 C81 F821 36(3) . . ? F84 C81 F821 137(3) . . ? F841 C81 C77 112.5(8) . . ? F831 C81 C77 112.6(7) . . ? F83 C81 C77 119(3) . . ? F82 C81 C77 115(3) . . ? F84 C81 C77 104(3) . . ? F821 C81 C77 110.4(8) . . ? F86 C85 F87 105.6(8) . . ? F86 C85 F88 107.5(6) . . ? F87 C85 F88 106.4(6) . . ? F86 C85 C79 112.7(5) . . ? F87 C85 C79 111.4(6) . . ? F88 C85 C79 112.7(6) . . ? _diffrn_measured_fraction_theta_max 0.034 _diffrn_reflns_theta_full 83.06 _diffrn_measured_fraction_theta_full 0.034 _refine_diff_density_max 1.238 _refine_diff_density_min -1.139 _refine_diff_density_rms 0.232 #============================================================================== # start Validation Reply Form #============================================================================== _vrf_TYPE031_2-Neutron ; PROBLEM: _diffrn_radiation_wavelength is not of type numb. RESPONSE: Data collected with Time of Flight Neutron Diffraction Data; see _exptl_special_details and _refine_special_details for information. ; _vrf_PLAT029_2-Neutron ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.220 RESPONSE: Data collected with Time of Flight Neutron Diffraction Data; see _exptl_special_details and _refine_special_details for information. ; _vrf_PLAT051_2-Neutron ; PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 1011.42 Perc RESPONSE: Data collected with Time of Flight Neutron Diffraction Data; see _exptl_special_details and _refine_special_details for information. ; _vrf_PLAT091_2-Neutron ; PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed ? RESPONSE: Data collected with Time of Flight Neutron Diffraction Data; see _exptl_special_details and _refine_special_details for information. ; _vrf_PLAT982_2-Neutron ; PROBLEM: The C-f'= 0.000 Deviates from the IT-value 0.003 RESPONSE: Data collected with Time of Flight Neutron Diffraction Data; see _exptl_special_details and _refine_special_details for information. ; _vrf_PLAT983_2-Neutron ; PROBLEM: The C-f'= 0.000 Deviates from the IT-value 0.003 RESPONSE: Data collected with Time of Flight Neutron Diffraction Data; see _exptl_special_details and _refine_special_details for information. ; _vrf_TYPE031_3-Neutron ; PROBLEM: _diffrn_radiation_wavelength is not of type numb. RESPONSE: Data collected with Time of Flight Neutron Diffraction Data; see _exptl_special_details and _refine_special_details for information. ; _vrf_PLAT029_3-Neutron ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.340 RESPONSE: Data collected with Time of Flight Neutron Diffraction Data; see _exptl_special_details and _refine_special_details for information. ; _vrf_PLAT051_3-Neutron ; PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 105.58 Perc RESPONSE: Data collected with Time of Flight Neutron Diffraction Data; see _exptl_special_details and _refine_special_details for information. ; _vrf_PLAT091_3-Neutron ; PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed ? RESPONSE: Data collected with Time of Flight Neutron Diffraction Data; see _exptl_special_details and _refine_special_details for information. ; _vrf_PLAT982_3-Neutron ; PROBLEM: The C-f'= 0.000 Deviates from the IT-value 0.003 RESPONSE: Data collected with Time of Flight Neutron Diffraction Data; see _exptl_special_details and _refine_special_details for information. ; _vrf_PLAT983_3-Neutron ; PROBLEM: The C-f'= 0.000 Deviates from the IT-value 0.003 RESPONSE: Data collected with Time of Flight Neutron Diffraction Data; see _exptl_special_details and _refine_special_details for information. ; #============================================================================== # End Validation Reply Form #==============================================================================