data_global # # Mechanistic Insights in Transfer Hydrogenation Catalysis # by [Ir(cod)(NHC)2]+ Complexes with Functionalized # N-Heterocyclic Carbene Ligands # # by M. Victoria Jimenez, Javier Fernandez-Tornos, Jesus # Perez-Torrente, Francisco J. Modrego, Pilar Garcia-Orduņa # and Luis A. Oro # # # # # Submitted to Organometallics # Manuscript number ........... # ----------------------------------------------------------- # # Person for contact _publ_contact_author_name 'Dr. Fernando J. Lahoz' _publ_contact_author_address ; Dr. Fernando J. Lahoz Departamento de Qu\'imica Inorg\'anica Instituto de S\'intesis Qu\'imica y Cat\'alisis Homog\'enea - ISQCH Universidad de Zaragoza - C.S.I.C. C/ Pedro Cerbuna, 12 50009 Zaragoza, Spain ; _publ_contact_author_phone '+34 976 761147' _publ_contact_author_fax '+34 976 761187' _publ_contact_author_email lahoz@unizar.es # ------------------------------------------------------------ # Publication details loop_ _publ_author_name 'Jimenez, M.V.' 'Fernandez-Tornos, J.' 'Perez-Torrente, J.J.' 'Modrego, F.J.' 'Garcia-Ordu\~a,P.' 'Oro,L.A.' _publ_requested_journal 'Organometallics' _journal_name_full 'Organometallics' _journal_volume '?' _journal_page_first '?' _journal_page_last '?' _journal_year '2014' # ---------------------------------------------------------- # Data for cmpnd_4 (local labelling as fjl72ds) data_cmpnd_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H40 Ir N4 O2, F6 P' _chemical_formula_sum 'C32 H40 F6 Ir N4 O2 P' _chemical_formula_weight 849.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0030 0.0020 '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' 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1020 0.0940 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4440 7.9890 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.946(4) _cell_length_b 11.935(4) _cell_length_c 14.097(5) _cell_angle_alpha 101.745(7) _cell_angle_beta 107.631(6) _cell_angle_gamma 101.754(7) _cell_volume 1647.4(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2080 _cell_measurement_theta_min 2.312 _cell_measurement_theta_max 19.55 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.116 _exptl_crystal_size_mid 0.037 _exptl_crystal_size_min 0.030 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 4.171 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5253 _exptl_absorpt_correction_T_max 0.8282 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within APEX2 package. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX DUO CCD system' _diffrn_measurement_method 'narrow \w frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9840 _diffrn_reflns_av_R_equivalents 0.0747 _diffrn_reflns_av_sigmaI/netI 0.0868 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 21.36 _reflns_number_total 3674 _reflns_number_gt 3133 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_data_reduction 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material 'XCIF program, PLATON(Spek, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hydrogen atoms have been included in the model in calculated positions and refined with a riding model. When convergence is achieved, residual peaks higher than 1 e/A^3^ are observed. They are close to iridium atom. They have no chemical sence. ; _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^)+(0.0985P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3674 _refine_ls_number_parameters 419 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1435 _refine_ls_wR_factor_gt 0.1353 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL fjl72dm in P-1 CELL 0.71073 10.9459 11.9350 14.0966 101.745 107.631 101.754 ZERR 2.00 0.0039 0.0043 0.0050 0.007 0.006 0.007 LATT 1 SFAC C 2.31000 20.84392 1.02000 10.20751 1.58860 0.56870 = 0.86500 51.65125 0.21560 0.003 0.002 11.500 0.770 12.011 SFAC H 0.49300 10.51091 0.32291 26.12573 0.14019 3.14236 = 0.04081 57.79977 0.00304 0.000 0.000 0.620 0.320 1.008 SFAC N 12.21261 0.00570 3.13220 9.89331 2.01250 28.99754 = 1.16630 0.58260 -11.52901 0.006 0.003 19.600 0.700 14.007 SFAC O 3.04850 13.27711 2.28680 5.70111 1.54630 0.32390 = 0.86700 32.90894 0.25080 0.011 0.006 32.500 0.660 15.999 SFAC F 3.53920 10.28251 2.64120 4.29440 1.51700 0.26150 = 1.02430 26.14763 0.27760 0.017 0.010 51.500 0.640 18.998 SFAC P 6.43451 1.90670 4.17910 27.15704 1.78000 0.52600 = 1.49080 68.16457 1.11490 0.102 0.094 410.000 1.100 30.974 SFAC IR 27.30493 1.59279 16.72961 8.86554 15.61152 0.41792 = 5.83378 45.00114 11.47221 -1.444 7.989 33100.000 1.350 192.217 UNIT 64 80 8 4 12 2 2 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H CONF L.S. 5 TEMP -173.00 WGHT 0.098500 FVAR 0.35438 IR1 7 0.127708 0.247605 0.301370 11.00000 0.02934 0.03173 = 0.02671 0.00338 0.01138 0.00631 O1 4 -0.256402 0.015658 0.321601 11.00000 0.02847 0.04012 = 0.05875 0.00567 0.02279 0.00566 O2 4 -0.173430 0.473448 0.075672 11.00000 0.08825 0.05213 = 0.03666 0.01583 0.01841 0.00394 N1 3 -0.069542 0.133845 0.077747 11.00000 0.04373 0.03395 = 0.03217 -0.00078 0.01090 0.00549 N2 3 -0.093303 0.011981 0.168710 11.00000 0.02873 0.02697 = 0.02317 0.00026 0.00738 -0.00488 N3 3 -0.018893 0.279017 0.453769 11.00000 0.04024 0.04142 = 0.02407 0.00486 0.01697 0.00773 N4 3 -0.077558 0.374748 0.343495 11.00000 0.02431 0.03936 = 0.03515 0.00639 0.01017 0.00710 C1 1 0.300198 0.351699 0.447236 11.00000 0.02663 0.03965 = 0.02380 -0.01469 -0.00063 -0.01037 AFIX 43 H1 2 0.243671 0.342876 0.486387 11.00000 -1.20000 AFIX 0 C2 1 0.276432 0.420533 0.380712 11.00000 0.05604 0.03656 = 0.03707 0.01320 0.01485 0.00198 AFIX 43 H2 2 0.204351 0.454536 0.376461 11.00000 -1.20000 AFIX 0 C3 1 0.357504 0.446105 0.313367 11.00000 0.05909 0.04471 = 0.05464 -0.00011 0.03013 -0.00739 AFIX 23 H3A 2 0.309339 0.482201 0.261786 11.00000 -1.20000 H3B 2 0.444157 0.505587 0.357691 11.00000 -1.20000 AFIX 0 C4 1 0.384210 0.337900 0.256640 11.00000 0.04937 0.05086 = 0.04872 -0.00251 0.02989 -0.01306 AFIX 23 H4A 2 0.468132 0.327865 0.301337 11.00000 -1.20000 H4B 2 0.397667 0.351732 0.193149 11.00000 -1.20000 AFIX 0 C5 1 0.273610 0.224328 0.226407 11.00000 0.02883 0.05078 = 0.04804 -0.00215 0.02153 0.01675 AFIX 43 H5 2 0.202980 0.204395 0.161327 11.00000 -1.20000 AFIX 0 C6 1 0.267972 0.147306 0.286860 11.00000 0.03710 0.03773 = 0.04114 0.00265 0.01682 -0.00425 AFIX 43 H6 2 0.195091 0.076661 0.257839 11.00000 -1.20000 AFIX 0 C7 1 0.364700 0.162973 0.393805 11.00000 0.03478 0.03685 = 0.05648 -0.00066 0.00754 0.01200 AFIX 23 H7A 2 0.445118 0.141200 0.387657 11.00000 -1.20000 H7B 2 0.322674 0.107560 0.426020 11.00000 -1.20000 AFIX 0 C8 1 0.407059 0.288991 0.464037 11.00000 0.04335 0.05987 = 0.04136 0.00731 0.01122 0.02593 AFIX 23 H8A 2 0.436865 0.286576 0.537088 11.00000 -1.20000 H8B 2 0.484705 0.336251 0.453345 11.00000 -1.20000 AFIX 0 C9 1 -0.023541 0.120558 0.174527 11.00000 0.03679 0.04726 = 0.01938 0.00189 0.00945 0.01570 C10 1 -0.165365 0.031653 0.013772 11.00000 0.03612 0.05084 = 0.03370 0.00520 0.01040 0.00708 AFIX 43 H10 2 -0.213907 0.018112 -0.057897 11.00000 -1.20000 AFIX 0 C11 1 -0.180128 -0.047298 0.068830 11.00000 0.02352 0.03716 = 0.02791 -0.00898 0.00307 0.00240 AFIX 43 H11 2 -0.237851 -0.126456 0.044005 11.00000 -1.20000 AFIX 0 C15 1 -0.022490 0.235966 0.042854 11.00000 0.05007 0.04593 = 0.02421 0.00750 0.01520 0.00501 AFIX 137 H15A 2 0.031177 0.304737 0.103298 11.00000 -1.50000 H15B 2 -0.099430 0.255600 -0.000129 11.00000 -1.50000 H15C 2 0.032345 0.216060 0.001988 11.00000 -1.50000 AFIX 0 C16 1 -0.060016 -0.041981 0.254986 11.00000 0.01640 0.04504 = 0.05350 0.01823 0.01644 0.00976 AFIX 23 H16A 2 -0.029027 0.021168 0.321624 11.00000 -1.20000 H16B 2 0.014356 -0.076747 0.253431 11.00000 -1.20000 AFIX 0 C17 1 -0.176044 -0.136951 0.249852 11.00000 0.01808 0.04024 = 0.03249 0.01274 -0.00077 0.00731 C18 1 -0.189568 -0.256048 0.212252 11.00000 0.02012 0.04361 = 0.04673 0.01921 0.00568 0.00995 AFIX 43 H18 2 -0.126126 -0.279329 0.185085 11.00000 -1.20000 AFIX 0 C19 1 -0.295178 -0.343641 0.213284 11.00000 0.04129 0.04100 = 0.04008 0.00683 -0.00611 0.00808 AFIX 43 H19 2 -0.303022 -0.425736 0.187200 11.00000 -1.20000 AFIX 0 C20 1 -0.386473 -0.311142 0.251630 11.00000 0.03090 0.05239 = 0.05297 0.02083 0.00461 0.00445 AFIX 43 H20 2 -0.457617 -0.371197 0.252520 11.00000 -1.20000 AFIX 0 C21 1 -0.377900 -0.190856 0.289910 11.00000 0.02999 0.05602 = 0.04608 0.01157 0.00798 0.00500 AFIX 43 H21 2 -0.441906 -0.169150 0.317193 11.00000 -1.20000 AFIX 0 C22 1 -0.273972 -0.103597 0.287307 11.00000 0.03708 0.03249 = 0.02174 0.00884 0.00216 0.00435 C23 1 -0.352480 0.052523 0.359810 11.00000 0.04341 0.04478 = 0.08209 -0.00178 0.03659 0.00261 AFIX 137 H23A 2 -0.441866 0.016811 0.306270 11.00000 -1.50000 H23B 2 -0.331787 0.139717 0.377699 11.00000 -1.50000 H23C 2 -0.349954 0.026429 0.421776 11.00000 -1.50000 AFIX 0 C12 1 -0.000352 0.303179 0.369048 11.00000 0.04652 0.02907 = 0.01588 0.00153 0.00703 0.00026 C13 1 -0.106499 0.336692 0.481173 11.00000 0.03546 0.05863 = 0.02933 0.00645 0.02193 0.00949 AFIX 43 H13 2 -0.134311 0.334564 0.538574 11.00000 -1.20000 AFIX 0 C14 1 -0.143797 0.394964 0.412502 11.00000 0.03075 0.04002 = 0.03304 -0.00627 0.01661 0.00738 AFIX 43 H14 2 -0.204474 0.441904 0.410536 11.00000 -1.20000 AFIX 0 C24 1 0.040910 0.199947 0.509933 11.00000 0.04584 0.04706 = 0.02775 0.01146 0.00508 0.01432 AFIX 137 H24A 2 0.101992 0.171552 0.479023 11.00000 -1.50000 H24B 2 -0.030117 0.131536 0.504891 11.00000 -1.50000 H24C 2 0.090479 0.244364 0.583099 11.00000 -1.50000 AFIX 0 C25 1 -0.099685 0.414433 0.251555 11.00000 0.03637 0.03205 = 0.03458 0.00929 0.01113 0.00709 AFIX 23 H25A 2 -0.022870 0.413454 0.228537 11.00000 -1.20000 H25B 2 -0.104019 0.497858 0.268587 11.00000 -1.20000 AFIX 0 C26 1 -0.227954 0.337284 0.162735 11.00000 0.03462 0.03757 = 0.04796 0.01169 0.02124 0.01406 C27 1 -0.303037 0.234201 0.166473 11.00000 0.05542 0.03805 = 0.04109 0.01644 0.01058 0.00303 AFIX 43 H27 2 -0.275417 0.206040 0.225628 11.00000 -1.20000 AFIX 0 C28 1 -0.422756 0.168409 0.082142 11.00000 0.06715 0.05030 = 0.03288 0.00743 0.00206 -0.02406 AFIX 43 H28 2 -0.481454 0.100950 0.086870 11.00000 -1.20000 AFIX 0 C29 1 -0.451504 0.203710 -0.004993 11.00000 0.05512 0.10305 = 0.05787 0.02515 -0.00473 -0.01257 AFIX 43 H29 2 -0.528864 0.157639 -0.063523 11.00000 -1.20000 AFIX 0 C30 1 -0.372263 0.303858 -0.011088 11.00000 0.04798 0.08939 = 0.03730 0.02058 0.01282 0.02064 AFIX 43 H30 2 -0.392910 0.325481 -0.074114 11.00000 -1.20000 AFIX 0 C31 1 -0.265247 0.371885 0.071708 11.00000 0.04617 0.03474 = 0.03374 0.00883 0.01044 0.00418 C32 1 -0.204911 0.515786 -0.014299 11.00000 0.23927 0.06764 = 0.04730 0.03043 0.03949 -0.01000 AFIX 137 H32A 2 -0.178706 0.470020 -0.067008 11.00000 -1.50000 H32B 2 -0.156290 0.600465 0.004804 11.00000 -1.50000 H32C 2 -0.301284 0.505854 -0.042280 11.00000 -1.50000 AFIX 0 P1 6 -0.235516 0.230273 0.704055 11.00000 0.03006 0.04474 = 0.05293 0.01549 0.02094 0.01186 F1 5 -0.308598 0.301173 0.766060 11.00000 0.06811 0.06256 = 0.08547 0.00747 0.04572 0.02404 F2 5 -0.165574 0.158766 0.638305 11.00000 0.06689 0.08799 = 0.06043 0.03076 0.04269 0.04999 F3A 5 -0.349105 0.116069 0.673730 11.00000 0.12250 0.05137 = 0.33009 -0.00552 0.16044 0.00058 F4A 5 -0.125075 0.344890 0.725081 11.00000 0.11531 0.06275 = 0.20020 -0.01746 0.08393 -0.01981 F5A 5 -0.156066 0.198911 0.798616 11.00000 0.24022 0.28433 = 0.06744 0.09587 0.09547 0.20087 F6A 5 -0.315159 0.260456 0.605945 11.00000 0.12106 0.21334 = 0.10337 0.05177 0.04095 0.13435 HKLF 4 REM fjl72dm in P-1 REM R1 = 0.0540 for 3133 Fo > 4sig(Fo) and 0.0664 for all 3674 data REM 419 parameters refined using 0 restraints END ; 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 0.12771(5) 0.24760(4) 0.30137(3) 0.0301(3) Uani 1 1 d . . . O1 O -0.2564(8) 0.0157(7) 0.3216(7) 0.043(2) Uani 1 1 d . . . O2 O -0.1734(11) 0.4734(9) 0.0757(7) 0.062(3) Uani 1 1 d . . . N1 N -0.0695(11) 0.1338(9) 0.0777(8) 0.040(3) Uani 1 1 d . . . N2 N -0.0933(10) 0.0120(8) 0.1687(7) 0.030(2) Uani 1 1 d . . . N3 N -0.0189(10) 0.2790(9) 0.4538(7) 0.035(3) Uani 1 1 d . . . N4 N -0.0776(10) 0.3747(9) 0.3435(8) 0.034(3) Uani 1 1 d . . . C1 C 0.3002(13) 0.3517(11) 0.4472(9) 0.039(3) Uani 1 1 d . . . H1 H 0.2437 0.3429 0.4864 0.047 Uiso 1 1 calc R . . C2 C 0.2764(15) 0.4205(11) 0.3807(10) 0.045(4) Uani 1 1 d . . . H2 H 0.2044 0.4545 0.3765 0.054 Uiso 1 1 calc R . . C3 C 0.3575(16) 0.4461(12) 0.3134(11) 0.056(4) Uani 1 1 d . . . H3A H 0.3093 0.4822 0.2618 0.067 Uiso 1 1 calc R . . H3B H 0.4442 0.5056 0.3577 0.067 Uiso 1 1 calc R . . C4 C 0.3842(15) 0.3379(12) 0.2566(11) 0.054(4) Uani 1 1 d . . . H4A H 0.4681 0.3279 0.3013 0.064 Uiso 1 1 calc R . . H4B H 0.3977 0.3517 0.1931 0.064 Uiso 1 1 calc R . . C5 C 0.2736(13) 0.2243(12) 0.2264(11) 0.042(4) Uani 1 1 d . . . H5 H 0.2030 0.2044 0.1613 0.051 Uiso 1 1 calc R . . C6 C 0.2680(13) 0.1473(12) 0.2869(10) 0.042(3) Uani 1 1 d . . . H6 H 0.1951 0.0767 0.2578 0.050 Uiso 1 1 calc R . . C7 C 0.3647(14) 0.1630(12) 0.3938(11) 0.047(4) Uani 1 1 d . . . H7A H 0.4451 0.1412 0.3877 0.056 Uiso 1 1 calc R . . H7B H 0.3227 0.1076 0.4260 0.056 Uiso 1 1 calc R . . C8 C 0.4071(14) 0.2890(12) 0.4640(10) 0.048(4) Uani 1 1 d . . . H8A H 0.4369 0.2866 0.5371 0.058 Uiso 1 1 calc R . . H8B H 0.4847 0.3363 0.4533 0.058 Uiso 1 1 calc R . . C9 C -0.0235(13) 0.1206(12) 0.1745(9) 0.035(3) Uani 1 1 d . . . C10 C -0.1654(13) 0.0317(12) 0.0138(10) 0.043(3) Uani 1 1 d . . . H10 H -0.2139 0.0181 -0.0579 0.051 Uiso 1 1 calc R . . C11 C -0.1801(12) -0.0473(11) 0.0688(9) 0.035(3) Uani 1 1 d . . . H11 H -0.2379 -0.1265 0.0440 0.042 Uiso 1 1 calc R . . C15 C -0.0225(14) 0.2360(11) 0.0429(9) 0.041(3) Uani 1 1 d . . . H15A H 0.0312 0.3047 0.1033 0.062 Uiso 1 1 calc R . . H15B H -0.0994 0.2556 -0.0001 0.062 Uiso 1 1 calc R . . H15C H 0.0323 0.2161 0.0020 0.062 Uiso 1 1 calc R . . C16 C -0.0600(12) -0.0420(11) 0.2550(10) 0.037(3) Uani 1 1 d . . . H16A H -0.0290 0.0212 0.3216 0.044 Uiso 1 1 calc R . . H16B H 0.0144 -0.0767 0.2534 0.044 Uiso 1 1 calc R . . C17 C -0.1760(11) -0.1370(11) 0.2499(9) 0.032(3) Uani 1 1 d . . . C18 C -0.1896(12) -0.2560(11) 0.2123(10) 0.037(3) Uani 1 1 d . . . H18 H -0.1261 -0.2793 0.1851 0.045 Uiso 1 1 calc R . . C19 C -0.2952(14) -0.3436(12) 0.2133(10) 0.047(4) Uani 1 1 d . . . H19 H -0.3030 -0.4257 0.1872 0.057 Uiso 1 1 calc R . . C20 C -0.3865(14) -0.3111(13) 0.2516(11) 0.048(4) Uani 1 1 d . . . H20 H -0.4576 -0.3712 0.2525 0.058 Uiso 1 1 calc R . . C21 C -0.3779(13) -0.1909(13) 0.2899(10) 0.047(4) Uani 1 1 d . . . H21 H -0.4419 -0.1691 0.3172 0.056 Uiso 1 1 calc R . . C22 C -0.2740(13) -0.1036(11) 0.2873(9) 0.033(3) Uani 1 1 d . . . C23 C -0.3525(15) 0.0525(12) 0.3598(12) 0.058(4) Uani 1 1 d . . . H23A H -0.4419 0.0168 0.3063 0.087 Uiso 1 1 calc R . . H23B H -0.3318 0.1397 0.3777 0.087 Uiso 1 1 calc R . . H23C H -0.3500 0.0264 0.4218 0.087 Uiso 1 1 calc R . . C12 C -0.0004(13) 0.3032(11) 0.3690(8) 0.034(3) Uani 1 1 d . . . C13 C -0.1065(13) 0.3367(12) 0.4812(10) 0.040(3) Uani 1 1 d . . . H13 H -0.1343 0.3346 0.5386 0.048 Uiso 1 1 calc R . . C14 C -0.1438(13) 0.3950(11) 0.4125(10) 0.036(3) Uani 1 1 d . . . H14 H -0.2045 0.4419 0.4105 0.044 Uiso 1 1 calc R . . C24 C 0.0409(13) 0.1999(11) 0.5099(9) 0.042(3) Uani 1 1 d . . . H24A H 0.1020 0.1716 0.4790 0.063 Uiso 1 1 calc R . . H24B H -0.0301 0.1315 0.5049 0.063 Uiso 1 1 calc R . . H24C H 0.0905 0.2444 0.5831 0.063 Uiso 1 1 calc R . . C25 C -0.0997(13) 0.4144(11) 0.2516(9) 0.035(3) Uani 1 1 d . . . H25A H -0.0229 0.4135 0.2285 0.042 Uiso 1 1 calc R . . H25B H -0.1040 0.4979 0.2686 0.042 Uiso 1 1 calc R . . C26 C -0.2280(13) 0.3373(11) 0.1627(10) 0.038(3) Uani 1 1 d . . . C27 C -0.3030(14) 0.2342(11) 0.1665(10) 0.047(4) Uani 1 1 d . . . H27 H -0.2754 0.2060 0.2256 0.057 Uiso 1 1 calc R . . C28 C -0.4228(16) 0.1684(13) 0.0821(10) 0.061(5) Uani 1 1 d . . . H28 H -0.4815 0.1009 0.0869 0.073 Uiso 1 1 calc R . . C29 C -0.4515(18) 0.2037(18) -0.0050(14) 0.083(6) Uani 1 1 d . . . H29 H -0.5289 0.1576 -0.0635 0.100 Uiso 1 1 calc R . . C30 C -0.3723(16) 0.3039(15) -0.0111(11) 0.058(4) Uani 1 1 d . . . H30 H -0.3929 0.3255 -0.0741 0.070 Uiso 1 1 calc R . . C31 C -0.2652(14) 0.3719(11) 0.0717(10) 0.040(3) Uani 1 1 d . . . C32 C -0.205(3) 0.5158(17) -0.0143(13) 0.127(11) Uani 1 1 d . . . H32A H -0.1787 0.4700 -0.0670 0.191 Uiso 1 1 calc R . . H32B H -0.1563 0.6005 0.0048 0.191 Uiso 1 1 calc R . . H32C H -0.3013 0.5059 -0.0423 0.191 Uiso 1 1 calc R . . P1 P -0.2355(3) 0.2303(3) 0.7041(3) 0.0407(9) Uani 1 1 d . . . F1 F -0.3086(9) 0.3012(7) 0.7661(7) 0.069(2) Uani 1 1 d . . . F2 F -0.1656(9) 0.1588(8) 0.6383(6) 0.061(2) Uani 1 1 d . . . F3A F -0.3491(14) 0.1161(9) 0.6737(15) 0.162(7) Uani 1 1 d . . . F4A F -0.1251(13) 0.3449(9) 0.7251(12) 0.135(5) Uani 1 1 d . . . F5A F -0.1561(18) 0.1989(16) 0.7986(9) 0.160(7) Uani 1 1 d . . . F6A F -0.3152(13) 0.2605(14) 0.6059(9) 0.131(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.0293(4) 0.0317(4) 0.0267(3) 0.0034(2) 0.0114(2) 0.0063(2) O1 0.028(5) 0.040(6) 0.059(6) 0.006(5) 0.023(5) 0.006(4) O2 0.088(8) 0.052(6) 0.037(6) 0.016(5) 0.018(5) 0.004(6) N1 0.044(7) 0.034(7) 0.032(7) -0.001(5) 0.011(6) 0.005(6) N2 0.029(6) 0.027(6) 0.023(6) 0.000(5) 0.007(5) -0.005(5) N3 0.040(7) 0.041(7) 0.024(6) 0.005(5) 0.017(5) 0.008(5) N4 0.024(6) 0.039(6) 0.035(6) 0.006(5) 0.010(5) 0.007(5) C1 0.027(8) 0.040(8) 0.024(7) -0.015(6) -0.001(6) -0.010(6) C2 0.056(10) 0.037(8) 0.037(8) 0.013(7) 0.015(7) 0.002(7) C3 0.059(10) 0.045(9) 0.055(9) 0.000(7) 0.030(8) -0.007(8) C4 0.049(10) 0.051(9) 0.049(9) -0.003(7) 0.030(8) -0.013(8) C5 0.029(8) 0.051(9) 0.048(8) -0.002(7) 0.022(7) 0.017(7) C6 0.037(8) 0.038(8) 0.041(8) 0.003(7) 0.017(7) -0.004(6) C7 0.035(8) 0.037(8) 0.056(9) -0.001(7) 0.008(7) 0.012(6) C8 0.043(9) 0.060(10) 0.041(8) 0.007(7) 0.011(7) 0.026(8) C9 0.037(8) 0.047(9) 0.019(7) 0.002(6) 0.009(6) 0.016(7) C10 0.036(8) 0.051(9) 0.034(8) 0.005(8) 0.010(7) 0.007(7) C11 0.024(7) 0.037(8) 0.028(7) -0.009(7) 0.003(6) 0.002(6) C15 0.050(9) 0.046(8) 0.024(7) 0.007(6) 0.015(6) 0.005(7) C16 0.016(7) 0.045(8) 0.053(9) 0.018(7) 0.016(6) 0.010(6) C17 0.018(7) 0.040(9) 0.032(7) 0.013(6) -0.001(6) 0.007(6) C18 0.020(7) 0.044(9) 0.047(8) 0.019(7) 0.006(6) 0.010(6) C19 0.041(9) 0.041(9) 0.040(8) 0.007(7) -0.006(7) 0.008(7) C20 0.031(9) 0.052(10) 0.053(9) 0.021(8) 0.005(7) 0.004(7) C21 0.030(8) 0.056(10) 0.046(9) 0.012(7) 0.008(7) 0.005(7) C22 0.037(8) 0.032(8) 0.022(7) 0.009(6) 0.002(6) 0.004(6) C23 0.043(9) 0.045(9) 0.082(11) -0.002(8) 0.037(9) 0.003(7) C12 0.047(9) 0.029(7) 0.016(7) 0.002(6) 0.007(6) 0.000(7) C13 0.035(8) 0.059(9) 0.029(7) 0.006(7) 0.022(6) 0.009(7) C14 0.031(8) 0.040(8) 0.033(8) -0.006(7) 0.017(6) 0.007(6) C24 0.046(9) 0.047(9) 0.028(7) 0.011(6) 0.005(6) 0.014(7) C25 0.036(8) 0.032(7) 0.035(8) 0.009(6) 0.011(6) 0.007(6) C26 0.035(8) 0.038(8) 0.048(9) 0.012(7) 0.021(7) 0.014(7) C27 0.055(10) 0.038(8) 0.041(8) 0.016(7) 0.011(8) 0.003(7) C28 0.067(11) 0.050(10) 0.033(9) 0.007(8) 0.002(8) -0.024(8) C29 0.055(12) 0.103(15) 0.058(12) 0.025(11) -0.005(9) -0.013(11) C30 0.048(10) 0.089(13) 0.037(9) 0.021(9) 0.013(8) 0.021(10) C31 0.046(9) 0.035(8) 0.034(8) 0.009(7) 0.010(7) 0.004(7) C32 0.24(3) 0.068(13) 0.047(11) 0.030(10) 0.039(14) -0.010(15) P1 0.030(2) 0.045(2) 0.053(2) 0.0155(18) 0.0209(18) 0.0119(17) F1 0.068(6) 0.063(6) 0.085(6) 0.007(5) 0.046(5) 0.024(5) F2 0.067(6) 0.088(6) 0.060(5) 0.031(5) 0.043(5) 0.050(5) F3A 0.122(11) 0.051(7) 0.33(2) -0.006(9) 0.160(14) 0.001(7) F4A 0.115(10) 0.063(7) 0.200(14) -0.017(8) 0.084(10) -0.020(7) F5A 0.240(17) 0.284(19) 0.067(8) 0.096(10) 0.095(10) 0.201(16) F6A 0.121(10) 0.213(15) 0.103(9) 0.052(9) 0.041(8) 0.134(11) _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 C12 2.061(13) . ? Ir1 C9 2.078(12) . ? Ir1 C6 2.161(14) . ? Ir1 C2 2.179(12) . ? Ir1 C5 2.197(12) . ? Ir1 C1 2.234(11) . ? O1 C22 1.360(14) . ? O1 C23 1.423(16) . ? O2 C31 1.387(16) . ? O2 C32 1.432(18) . ? N1 C9 1.358(15) . ? N1 C10 1.363(16) . ? N1 C15 1.461(15) . ? N2 C9 1.336(15) . ? N2 C11 1.377(15) . ? N2 C16 1.474(15) . ? N3 C12 1.347(14) . ? N3 C13 1.388(16) . ? N3 C24 1.479(16) . ? N4 C12 1.345(16) . ? N4 C14 1.390(15) . ? N4 C25 1.438(15) . ? C1 C2 1.369(18) . ? C1 C8 1.498(19) . ? C1 H1 0.9500 . ? C2 C3 1.517(19) . ? C2 H2 0.9500 . ? C3 C4 1.51(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.506(18) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.379(18) . ? C5 H5 0.9500 . ? C6 C7 1.505(19) . ? C6 H6 0.9500 . ? C7 C8 1.513(18) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C10 C11 1.352(18) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.492(17) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.372(17) . ? C17 C22 1.420(18) . ? C18 C19 1.398(19) . ? C18 H18 0.9500 . ? C19 C20 1.36(2) . ? C19 H19 0.9500 . ? C20 C21 1.40(2) . ? C20 H20 0.9500 . ? C21 C22 1.392(18) . ? C21 H21 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C13 C14 1.318(18) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.525(18) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.354(17) . ? C26 C31 1.397(18) . ? C27 C28 1.416(19) . ? C27 H27 0.9500 . ? C28 C29 1.35(2) . ? C28 H28 0.9500 . ? C29 C30 1.36(2) . ? C29 H29 0.9500 . ? C30 C31 1.339(19) . ? C30 H30 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? P1 F5A 1.519(11) . ? P1 F3A 1.529(11) . ? P1 F4A 1.538(11) . ? P1 F6A 1.550(12) . ? P1 F1 1.587(9) . ? P1 F2 1.596(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 C12 Ir1 C9 94.6(5) . . ? C12 Ir1 C6 152.8(5) . . ? C9 Ir1 C6 90.8(5) . . ? C12 Ir1 C2 90.3(5) . . ? C9 Ir1 C2 154.5(5) . . ? C6 Ir1 C2 96.2(5) . . ? C12 Ir1 C5 168.7(5) . . ? C9 Ir1 C5 90.3(5) . . ? C6 Ir1 C5 36.9(5) . . ? C2 Ir1 C5 81.0(5) . . ? C12 Ir1 C1 89.4(5) . . ? C9 Ir1 C1 168.2(5) . . ? C6 Ir1 C1 80.7(5) . . ? C2 Ir1 C1 36.1(5) . . ? C5 Ir1 C1 87.7(5) . . ? C22 O1 C23 117.6(10) . . ? C31 O2 C32 116.2(13) . . ? C9 N1 C10 108.7(10) . . ? C9 N1 C15 127.4(10) . . ? C10 N1 C15 123.8(11) . . ? C9 N2 C11 111.2(10) . . ? C9 N2 C16 122.3(9) . . ? C11 N2 C16 125.5(10) . . ? C12 N3 C13 110.5(11) . . ? C12 N3 C24 126.0(11) . . ? C13 N3 C24 123.4(10) . . ? C12 N4 C14 110.5(10) . . ? C12 N4 C25 124.7(10) . . ? C14 N4 C25 124.5(11) . . ? C2 C1 C8 126.1(13) . . ? C2 C1 Ir1 69.8(7) . . ? C8 C1 Ir1 110.0(8) . . ? C2 C1 H1 117.0 . . ? C8 C1 H1 117.0 . . ? Ir1 C1 H1 90.2 . . ? C1 C2 C3 124.4(14) . . ? C1 C2 Ir1 74.1(7) . . ? C3 C2 Ir1 108.3(9) . . ? C1 C2 H2 117.8 . . ? C3 C2 H2 117.8 . . ? Ir1 C2 H2 87.6 . . ? C4 C3 C2 114.3(11) . . ? C4 C3 H3A 108.7 . . ? C2 C3 H3A 108.7 . . ? C4 C3 H3B 108.7 . . ? C2 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C3 C4 C5 113.7(12) . . ? C3 C4 H4A 108.8 . . ? C5 C4 H4A 108.8 . . ? C3 C4 H4B 108.8 . . ? C5 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C6 C5 C4 124.4(13) . . ? C6 C5 Ir1 70.1(8) . . ? C4 C5 Ir1 111.8(9) . . ? C6 C5 H5 117.8 . . ? C4 C5 H5 117.8 . . ? Ir1 C5 H5 88.0 . . ? C5 C6 C7 127.1(12) . . ? C5 C6 Ir1 73.0(8) . . ? C7 C6 Ir1 108.5(8) . . ? C5 C6 H6 116.4 . . ? C7 C6 H6 116.4 . . ? Ir1 C6 H6 88.4 . . ? C6 C7 C8 113.1(11) . . ? C6 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? C6 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C1 C8 C7 114.6(11) . . ? C1 C8 H8A 108.6 . . ? C7 C8 H8A 108.6 . . ? C1 C8 H8B 108.6 . . ? C7 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? N2 C9 N1 106.1(10) . . ? N2 C9 Ir1 129.1(9) . . ? N1 C9 Ir1 124.8(9) . . ? C11 C10 N1 109.0(11) . . ? C11 C10 H10 125.5 . . ? N1 C10 H10 125.5 . . ? C10 C11 N2 105.0(11) . . ? C10 C11 H11 127.5 . . ? N2 C11 H11 127.5 . . ? N1 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 C17 112.6(10) . . ? N2 C16 H16A 109.1 . . ? C17 C16 H16A 109.1 . . ? N2 C16 H16B 109.1 . . ? C17 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? C18 C17 C22 118.8(11) . . ? C18 C17 C16 122.0(12) . . ? C22 C17 C16 119.2(11) . . ? C17 C18 C19 121.1(13) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C20 C19 C18 119.8(13) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 121.3(13) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C22 C21 C20 118.9(14) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? O1 C22 C21 123.9(12) . . ? O1 C22 C17 115.9(10) . . ? C21 C22 C17 120.1(12) . . ? O1 C23 H23A 109.5 . . ? O1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C12 N3 104.9(11) . . ? N4 C12 Ir1 128.9(8) . . ? N3 C12 Ir1 126.2(10) . . ? C14 C13 N3 107.1(11) . . ? C14 C13 H13 126.5 . . ? N3 C13 H13 126.5 . . ? C13 C14 N4 107.1(11) . . ? C13 C14 H14 126.5 . . ? N4 C14 H14 126.5 . . ? N3 C24 H24A 109.5 . . ? N3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N4 C25 C26 112.8(10) . . ? N4 C25 H25A 109.0 . . ? C26 C25 H25A 109.0 . . ? N4 C25 H25B 109.0 . . ? C26 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C27 C26 C31 118.8(12) . . ? C27 C26 C25 122.9(12) . . ? C31 C26 C25 118.2(11) . . ? C26 C27 C28 119.9(12) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 118.4(13) . . ? C29 C28 H28 120.8 . . ? C27 C28 H28 120.8 . . ? C28 C29 C30 121.5(15) . . ? C28 C29 H29 119.2 . . ? C30 C29 H29 119.2 . . ? C31 C30 C29 120.0(14) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 O2 126.3(12) . . ? C30 C31 C26 120.8(12) . . ? O2 C31 C26 112.6(11) . . ? O2 C32 H32A 109.5 . . ? O2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? F5A P1 F3A 91.0(11) . . ? F5A P1 F4A 93.2(10) . . ? F3A P1 F4A 175.3(10) . . ? F5A P1 F6A 178.6(7) . . ? F3A P1 F6A 88.9(10) . . ? F4A P1 F6A 86.8(9) . . ? F5A P1 F1 93.1(6) . . ? F3A P1 F1 90.0(6) . . ? F4A P1 F1 91.8(6) . . ? F6A P1 F1 88.3(6) . . ? F5A P1 F2 88.7(5) . . ? F3A P1 F2 89.5(6) . . ? F4A P1 F2 88.6(6) . . ? F6A P1 F2 89.9(5) . . ? F1 P1 F2 178.2(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 Ir1 C1 C2 -91.3(9) . . . . ? C9 Ir1 C1 C2 158(2) . . . . ? C6 Ir1 C1 C2 114.1(9) . . . . ? C5 Ir1 C1 C2 77.7(9) . . . . ? C12 Ir1 C1 C8 146.4(10) . . . . ? C9 Ir1 C1 C8 36(3) . . . . ? C6 Ir1 C1 C8 -8.1(9) . . . . ? C2 Ir1 C1 C8 -122.2(14) . . . . ? C5 Ir1 C1 C8 -44.5(10) . . . . ? C8 C1 C2 C3 -1(2) . . . . ? Ir1 C1 C2 C3 -101.5(12) . . . . ? C8 C1 C2 Ir1 100.6(12) . . . . ? C12 Ir1 C2 C1 88.6(9) . . . . ? C9 Ir1 C2 C1 -170.0(10) . . . . ? C6 Ir1 C2 C1 -64.9(9) . . . . ? C5 Ir1 C2 C1 -98.6(9) . . . . ? C12 Ir1 C2 C3 -149.8(11) . . . . ? C9 Ir1 C2 C3 -48.4(18) . . . . ? C6 Ir1 C2 C3 56.7(11) . . . . ? C5 Ir1 C2 C3 23.0(10) . . . . ? C1 Ir1 C2 C3 121.6(15) . . . . ? C1 C2 C3 C4 46.1(19) . . . . ? Ir1 C2 C3 C4 -36.8(16) . . . . ? C2 C3 C4 C5 32.4(19) . . . . ? C3 C4 C5 C6 -91.4(17) . . . . ? C3 C4 C5 Ir1 -11.1(16) . . . . ? C12 Ir1 C5 C6 153(2) . . . . ? C9 Ir1 C5 C6 -90.8(8) . . . . ? C2 Ir1 C5 C6 113.2(8) . . . . ? C1 Ir1 C5 C6 77.5(8) . . . . ? C12 Ir1 C5 C4 33(3) . . . . ? C9 Ir1 C5 C4 149.0(11) . . . . ? C6 Ir1 C5 C4 -120.2(14) . . . . ? C2 Ir1 C5 C4 -6.9(10) . . . . ? C1 Ir1 C5 C4 -42.6(11) . . . . ? C4 C5 C6 C7 3(2) . . . . ? Ir1 C5 C6 C7 -100.6(13) . . . . ? C4 C5 C6 Ir1 103.4(12) . . . . ? C12 Ir1 C6 C5 -168.8(9) . . . . ? C9 Ir1 C6 C5 89.5(8) . . . . ? C2 Ir1 C6 C5 -65.9(8) . . . . ? C1 Ir1 C6 C5 -98.7(8) . . . . ? C12 Ir1 C6 C7 -44.6(15) . . . . ? C9 Ir1 C6 C7 -146.2(9) . . . . ? C2 Ir1 C6 C7 58.3(9) . . . . ? C5 Ir1 C6 C7 124.2(13) . . . . ? C1 Ir1 C6 C7 25.6(9) . . . . ? C5 C6 C7 C8 42.3(19) . . . . ? Ir1 C6 C7 C8 -40.0(14) . . . . ? C2 C1 C8 C7 -90.5(16) . . . . ? Ir1 C1 C8 C7 -11.4(15) . . . . ? C6 C7 C8 C1 34.7(17) . . . . ? C11 N2 C9 N1 2.4(14) . . . . ? C16 N2 C9 N1 171.7(10) . . . . ? C11 N2 C9 Ir1 -176.7(9) . . . . ? C16 N2 C9 Ir1 -7.5(17) . . . . ? C10 N1 C9 N2 -1.1(14) . . . . ? C15 N1 C9 N2 -178.0(12) . . . . ? C10 N1 C9 Ir1 178.0(9) . . . . ? C15 N1 C9 Ir1 1.2(18) . . . . ? C12 Ir1 C9 N2 -77.7(12) . . . . ? C6 Ir1 C9 N2 75.6(12) . . . . ? C2 Ir1 C9 N2 -178.2(11) . . . . ? C5 Ir1 C9 N2 112.5(12) . . . . ? C1 Ir1 C9 N2 32(3) . . . . ? C12 Ir1 C9 N1 103.3(11) . . . . ? C6 Ir1 C9 N1 -103.3(11) . . . . ? C2 Ir1 C9 N1 2.9(19) . . . . ? C5 Ir1 C9 N1 -66.5(11) . . . . ? C1 Ir1 C9 N1 -147(2) . . . . ? C9 N1 C10 C11 -0.5(14) . . . . ? C15 N1 C10 C11 176.5(12) . . . . ? N1 C10 C11 N2 1.9(14) . . . . ? C9 N2 C11 C10 -2.7(14) . . . . ? C16 N2 C11 C10 -171.5(11) . . . . ? C9 N2 C16 C17 157.5(11) . . . . ? C11 N2 C16 C17 -34.8(16) . . . . ? N2 C16 C17 C18 100.4(13) . . . . ? N2 C16 C17 C22 -81.2(14) . . . . ? C22 C17 C18 C19 -1.9(18) . . . . ? C16 C17 C18 C19 176.5(11) . . . . ? C17 C18 C19 C20 0.2(19) . . . . ? C18 C19 C20 C21 0(2) . . . . ? C19 C20 C21 C22 1(2) . . . . ? C23 O1 C22 C21 -1.7(17) . . . . ? C23 O1 C22 C17 -179.9(12) . . . . ? C20 C21 C22 O1 179.5(11) . . . . ? C20 C21 C22 C17 -2.3(18) . . . . ? C18 C17 C22 O1 -178.7(10) . . . . ? C16 C17 C22 O1 2.8(16) . . . . ? C18 C17 C22 C21 2.9(17) . . . . ? C16 C17 C22 C21 -175.5(11) . . . . ? C14 N4 C12 N3 0.1(13) . . . . ? C25 N4 C12 N3 -173.8(10) . . . . ? C14 N4 C12 Ir1 -176.9(8) . . . . ? C25 N4 C12 Ir1 9.3(17) . . . . ? C13 N3 C12 N4 -0.6(13) . . . . ? C24 N3 C12 N4 177.8(10) . . . . ? C13 N3 C12 Ir1 176.4(9) . . . . ? C24 N3 C12 Ir1 -5.2(16) . . . . ? C9 Ir1 C12 N4 -77.3(11) . . . . ? C6 Ir1 C12 N4 -178.0(9) . . . . ? C2 Ir1 C12 N4 77.7(11) . . . . ? C5 Ir1 C12 N4 38(3) . . . . ? C1 Ir1 C12 N4 113.8(11) . . . . ? C9 Ir1 C12 N3 106.4(10) . . . . ? C6 Ir1 C12 N3 5.7(17) . . . . ? C2 Ir1 C12 N3 -98.6(10) . . . . ? C5 Ir1 C12 N3 -138(2) . . . . ? C1 Ir1 C12 N3 -62.5(10) . . . . ? C12 N3 C13 C14 1.0(14) . . . . ? C24 N3 C13 C14 -177.5(11) . . . . ? N3 C13 C14 N4 -0.9(14) . . . . ? C12 N4 C14 C13 0.5(14) . . . . ? C25 N4 C14 C13 174.4(11) . . . . ? C12 N4 C25 C26 95.9(14) . . . . ? C14 N4 C25 C26 -77.1(14) . . . . ? N4 C25 C26 C27 -7.8(18) . . . . ? N4 C25 C26 C31 175.5(11) . . . . ? C31 C26 C27 C28 -5(2) . . . . ? C25 C26 C27 C28 178.5(13) . . . . ? C26 C27 C28 C29 7(2) . . . . ? C27 C28 C29 C30 -4(3) . . . . ? C28 C29 C30 C31 -2(3) . . . . ? C29 C30 C31 O2 177.6(16) . . . . ? C29 C30 C31 C26 4(2) . . . . ? C32 O2 C31 C30 7(2) . . . . ? C32 O2 C31 C26 -179.3(16) . . . . ? C27 C26 C31 C30 -1(2) . . . . ? C25 C26 C31 C30 175.9(13) . . . . ? C27 C26 C31 O2 -174.8(13) . . . . ? C25 C26 C31 O2 1.9(17) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 21.36 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.841 _refine_diff_density_min -1.486 _refine_diff_density_rms 0.198 # start Validation Reply Form _vrf_THETM01_cmpnd_4 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Sample crystallizes in tiny plates, mutually stuck. Several crystals were tested before selecting the one used in the data collection. Most of them have shown to be slightly twinned. Eventually, a very weakly diffracting crystal was selected. No detectable intensity was observed over 43 degres and therefore this value has been used as cut-off during the integration process. ; _vrf_PLAT971_cmpnd_4 ; PROBLEM: Check Calcd Residual Density 1.21A From Ir1 3.02 eA-3 RESPONSE: When convergence is achieved, residual density peaks higher than 1 e/A^3^ are observed close to the iridium atom. They have no chemical sence and may be related to improper absorption corrections applied to this weakly diffracting crystal. ; #===END # # # ---------------------------------------------------------- # Data for cmpnd_5 (local labelling as fjl128dsq) data_cmpnd_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C28 H34 Ir N6),2Br,H2 O,C H2 Cl2' _chemical_formula_sum 'C57 H72 Br2 Cl2 Ir2 N12 O' _chemical_formula_weight 1556.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.390(6) _cell_length_b 14.148(8) _cell_length_c 20.021(11) _cell_angle_alpha 88.505(8) _cell_angle_beta 89.648(8) _cell_angle_gamma 78.507(8) _cell_volume 2883(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6044 _cell_measurement_theta_min 2.234 _cell_measurement_theta_max 27.019 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.099 _exptl_crystal_size_mid 0.082 _exptl_crystal_size_min 0.043 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.793 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 6.141 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4322 _exptl_absorpt_correction_T_max 0.7173 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within APEX2 package. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX DUO CCD system' _diffrn_measurement_method 'narrow \w frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 30565 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0990 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 29.49 _reflns_number_total 14370 _reflns_number_gt 9250 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_data_reduction 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material 'XCIF program, PLATON(Spek, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Asymmetric unit contains two Ir complex cations, two Br atoms as counterions and a water solvent molecule. Moreover, residual density peaks and voids are found in the unit cell, indicating the presence of CH2Cl2. However, dichlomethane is highly disordered. Several refinement strategies have been tested. All of them lead to unrealistic geometrical and thermal parameters. Therefore, the contribution of CH2Cl2 to scattered intensities have been taken into account with SQUEEZE program. Hydrogen atoms (except those of water molecule) have been included in the model in calculated positions and refined with a riding model. When convergence is achieved, residual peaks higher than 1 e/A^3^ are observed. They are close to iridium atoms. They have no chemical sence. ; _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^)+(0.0670P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14370 _refine_ls_number_parameters 662 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0885 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1215 _refine_ls_wR_factor_gt 0.1081 _refine_ls_goodness_of_fit_ref 0.879 _refine_ls_restrained_S_all 0.879 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL fjl128dm in P-1 CELL 0.71073 10.3897 14.1479 20.0213 88.505 89.648 78.507 ZERR 2.00 0.0058 0.0080 0.0113 0.008 0.008 0.008 LATT 1 SFAC C H N BR IR O CL UNIT 114 144 24 4 4 2 4 MERG 2 OMIT -6 -15 7 FMAP 2 omit 0 1 0 PLAN 30 ACTA 55 BOND $H CONF L.S. 5 TEMP -173.00 WGHT 0.067000 FVAR 2.09518 IR1 5 0.378066 0.252266 0.080025 11.00000 0.02073 0.03056 = 0.01831 -0.00584 -0.00112 -0.00709 IR51 5 0.508074 0.772388 0.411902 11.00000 0.02002 0.02398 = 0.01916 -0.00612 -0.00292 -0.00306 BR1 4 0.964996 0.765099 0.623721 11.00000 0.02680 0.04906 = 0.03104 -0.00068 -0.00078 -0.00461 BR51 4 0.848220 0.230303 0.876844 11.00000 0.02915 0.05471 = 0.04108 -0.01199 -0.00785 -0.00482 N1 3 0.241569 0.077628 0.082222 11.00000 0.02373 0.02672 = 0.03839 -0.01053 -0.00443 -0.00962 N2 3 0.114004 0.201365 0.037811 11.00000 0.02198 0.03293 = 0.03563 -0.01286 -0.00656 0.00124 N3 3 0.217183 0.432392 0.145138 11.00000 0.02664 0.02462 = 0.03013 -0.00011 -0.00276 -0.00917 N4 3 0.256909 0.316606 0.216960 11.00000 0.02404 0.03325 = 0.01703 -0.00711 -0.00135 -0.00962 N5 3 -0.120437 0.427016 0.068436 11.00000 0.04527 0.04102 = 0.04918 -0.00852 -0.01410 0.00619 N6 3 0.482173 0.293872 0.296886 11.00000 0.02260 0.02862 = 0.03232 -0.00645 -0.00318 -0.00739 N52 3 0.219568 0.823691 0.458557 11.00000 0.02499 0.02350 = 0.02650 -0.00489 0.00393 -0.00835 N51 3 0.272089 0.943214 0.403748 11.00000 0.02062 0.02300 = 0.02909 -0.00207 -0.00007 -0.00205 N54 3 0.425772 0.700918 0.276872 11.00000 0.02574 0.03107 = 0.02010 -0.00117 -0.00779 -0.00742 N53 3 0.452726 0.587154 0.351841 11.00000 0.02427 0.02575 = 0.02633 -0.00272 -0.00510 -0.00391 N55 3 0.121006 0.588285 0.456880 11.00000 0.02506 0.03070 = 0.04121 0.00025 -0.00324 -0.01007 N56 3 0.576985 0.890772 0.201338 11.00000 0.03787 0.03753 = 0.05177 0.00495 -0.00683 -0.00798 C1 1 0.565781 0.276225 0.117993 11.00000 0.02152 0.04593 = 0.02615 -0.00419 0.00289 -0.01835 AFIX 43 H1 2 0.527325 0.282782 0.161222 11.00000 -1.20000 AFIX 0 C2 1 0.519957 0.349344 0.071012 11.00000 0.02397 0.02675 = 0.03040 -0.00774 0.00380 -0.00839 AFIX 43 H2 2 0.449197 0.399396 0.083360 11.00000 -1.20000 AFIX 0 C3 1 0.575869 0.353521 0.002194 11.00000 0.03490 0.03883 = 0.03254 0.00071 0.00751 -0.00457 AFIX 23 H3A 2 0.669174 0.320170 0.002765 11.00000 -1.20000 H3B 2 0.572547 0.421780 -0.011310 11.00000 -1.20000 AFIX 0 C4 1 0.500846 0.306305 -0.049887 11.00000 0.03577 0.06111 = 0.02069 0.00851 -0.00071 -0.00292 AFIX 23 H4A 2 0.426970 0.355473 -0.067861 11.00000 -1.20000 H4B 2 0.560674 0.284152 -0.087482 11.00000 -1.20000 AFIX 0 C5 1 0.448204 0.222684 -0.021916 11.00000 0.02377 0.05609 = 0.01418 -0.00978 0.00180 -0.00911 AFIX 43 H5 2 0.360033 0.220333 -0.032774 11.00000 -1.20000 AFIX 0 C6 1 0.515578 0.148387 0.018268 11.00000 0.02296 0.03377 = 0.02625 -0.00727 0.00675 -0.00537 AFIX 43 H6 2 0.470483 0.099528 0.033131 11.00000 -1.20000 AFIX 0 C7 1 0.655679 0.140137 0.039881 11.00000 0.02747 0.03846 = 0.03333 -0.00314 -0.00137 -0.00528 AFIX 23 H7A 2 0.703160 0.170282 0.004888 11.00000 -1.20000 H7B 2 0.697693 0.070976 0.043703 11.00000 -1.20000 AFIX 0 C8 1 0.670416 0.187794 0.106832 11.00000 0.02388 0.05038 = 0.02854 0.00255 -0.00516 -0.01246 AFIX 23 H8A 2 0.666923 0.140320 0.143675 11.00000 -1.20000 H8B 2 0.757605 0.205897 0.108212 11.00000 -1.20000 AFIX 0 C9 1 0.233222 0.174118 0.067311 11.00000 0.01816 0.03288 = 0.02241 -0.00880 0.00242 -0.00316 C10 1 0.130692 0.045964 0.061703 11.00000 0.03030 0.02485 = 0.04615 -0.00883 -0.00807 -0.00356 AFIX 43 H10 2 0.114709 -0.017720 0.066129 11.00000 -1.20000 AFIX 0 C11 1 0.050189 0.123242 0.034282 11.00000 0.03184 0.03425 = 0.04860 -0.01694 -0.01227 -0.01428 AFIX 43 H11 2 -0.034284 0.124635 0.015920 11.00000 -1.20000 AFIX 0 C12 1 0.276123 0.338823 0.151981 11.00000 0.02852 0.02413 = 0.02379 -0.00261 -0.00898 -0.01119 C14 1 0.187562 0.394237 0.250075 11.00000 0.02779 0.03083 = 0.02000 -0.01048 0.00049 -0.00203 AFIX 43 H14 2 0.163470 0.395574 0.295941 11.00000 -1.20000 AFIX 0 C13 1 0.159908 0.468586 0.205115 11.00000 0.02815 0.02987 = 0.03158 -0.01413 0.00221 -0.00500 AFIX 43 H13 2 0.111831 0.531898 0.212661 11.00000 -1.20000 AFIX 0 C15 1 0.347345 0.013403 0.121394 11.00000 0.03530 0.03504 = 0.03709 -0.00202 -0.00771 -0.00504 AFIX 137 H15A 2 0.417842 0.048108 0.130498 11.00000 -1.50000 H15B 2 0.382567 -0.044064 0.095706 11.00000 -1.50000 H15C 2 0.311137 -0.006039 0.163718 11.00000 -1.50000 AFIX 0 C16 1 0.050158 0.300303 0.024464 11.00000 0.03631 0.03892 = 0.03259 -0.00420 -0.01590 -0.00666 AFIX 23 H16A 2 -0.004655 0.303631 -0.016130 11.00000 -1.20000 H16B 2 0.117702 0.339525 0.015645 11.00000 -1.20000 AFIX 0 C17 1 -0.035772 0.342503 0.082559 11.00000 0.02743 0.02868 = 0.04223 -0.00990 -0.00831 -0.00865 C18 1 -0.030019 0.299760 0.146211 11.00000 0.02348 0.03302 = 0.03377 -0.00466 -0.00362 -0.00904 AFIX 43 H18 2 0.030159 0.240909 0.155171 11.00000 -1.20000 AFIX 0 C19 1 -0.110622 0.342141 0.195869 11.00000 0.03580 0.04574 = 0.03485 -0.00298 0.00156 -0.00969 AFIX 43 H19 2 -0.107664 0.312247 0.239026 11.00000 -1.20000 AFIX 0 C20 1 -0.195968 0.428204 0.183076 11.00000 0.03704 0.05087 = 0.05555 -0.01047 0.00257 0.00106 AFIX 43 H20 2 -0.251805 0.460219 0.216743 11.00000 -1.20000 AFIX 0 C21 1 -0.196163 0.465390 0.119036 11.00000 0.03860 0.04811 = 0.06486 -0.01242 -0.00804 0.00929 AFIX 43 H21 2 -0.256073 0.524258 0.109739 11.00000 -1.20000 AFIX 0 C22 1 0.199708 0.490460 0.082686 11.00000 0.03994 0.02830 = 0.02976 0.00736 -0.00032 -0.00979 AFIX 137 H22A 2 0.260213 0.458471 0.048701 11.00000 -1.50000 H22B 2 0.218191 0.554491 0.090676 11.00000 -1.50000 H22C 2 0.109071 0.497127 0.067047 11.00000 -1.50000 AFIX 0 C23 1 0.309194 0.221474 0.249295 11.00000 0.02719 0.02313 = 0.01779 -0.00032 0.00063 -0.00680 AFIX 23 H23A 2 0.307412 0.170169 0.216820 11.00000 -1.20000 H23B 2 0.251785 0.211141 0.287319 11.00000 -1.20000 AFIX 0 C24 1 0.447563 0.213427 0.274195 11.00000 0.02545 0.03259 = 0.02273 -0.00492 0.00259 -0.00928 C25 1 0.533537 0.122961 0.274910 11.00000 0.02372 0.03660 = 0.03637 0.00340 -0.00120 -0.01046 AFIX 43 H25 2 0.506726 0.068260 0.257280 11.00000 -1.20000 AFIX 0 C26 1 0.656938 0.115054 0.301538 11.00000 0.03211 0.02999 = 0.04611 0.00717 0.00174 0.00138 AFIX 43 H26 2 0.715932 0.054421 0.303897 11.00000 -1.20000 AFIX 0 C27 1 0.694396 0.198497 0.325280 11.00000 0.02823 0.05759 = 0.03988 0.00847 -0.00749 -0.01318 AFIX 43 H27 2 0.778805 0.195194 0.344258 11.00000 -1.20000 AFIX 0 C28 1 0.605481 0.285409 0.320343 11.00000 0.02976 0.04427 = 0.02688 -0.00538 -0.00199 -0.01912 AFIX 43 H28 2 0.632751 0.342050 0.334204 11.00000 -1.20000 AFIX 0 C51 1 0.711422 0.751245 0.376442 11.00000 0.02051 0.03377 = 0.02867 -0.00731 -0.00319 -0.00687 AFIX 43 H51 2 0.679991 0.744470 0.332719 11.00000 -1.20000 AFIX 0 C52 1 0.703371 0.676345 0.422087 11.00000 0.01968 0.02516 = 0.04235 -0.01768 -0.00816 0.00033 AFIX 43 H52 2 0.664587 0.624963 0.407730 11.00000 -1.20000 AFIX 0 C53 1 0.752718 0.672578 0.492697 11.00000 0.02672 0.03504 = 0.03952 0.00155 -0.01183 -0.00285 AFIX 23 H53A 2 0.828821 0.704902 0.494065 11.00000 -1.20000 H53B 2 0.783694 0.604283 0.506823 11.00000 -1.20000 AFIX 0 C54 1 0.647278 0.721234 0.543024 11.00000 0.04123 0.04207 = 0.02222 -0.00077 -0.00449 -0.01739 AFIX 23 H54A 2 0.599477 0.672130 0.560930 11.00000 -1.20000 H54B 2 0.692116 0.744490 0.580943 11.00000 -1.20000 AFIX 0 C55 1 0.551019 0.803040 0.514223 11.00000 0.03248 0.03512 = 0.02421 -0.00609 -0.00225 -0.00821 AFIX 43 H55 2 0.461053 0.804531 0.523989 11.00000 -1.20000 AFIX 0 C56 1 0.579644 0.878530 0.473943 11.00000 0.03182 0.02933 = 0.02881 -0.01794 -0.01022 0.00593 AFIX 43 H56 2 0.509196 0.926925 0.457651 11.00000 -1.20000 AFIX 0 C57 1 0.719864 0.885879 0.455271 11.00000 0.03152 0.02538 = 0.04689 -0.01092 -0.01016 -0.01153 AFIX 23 H57A 2 0.780240 0.852979 0.490519 11.00000 -1.20000 H57B 2 0.726661 0.954710 0.453581 11.00000 -1.20000 AFIX 0 C58 1 0.763516 0.841140 0.387791 11.00000 0.02350 0.04339 = 0.04548 -0.00317 -0.00470 -0.01032 AFIX 23 H58A 2 0.732402 0.888918 0.351480 11.00000 -1.20000 H58B 2 0.860672 0.825497 0.386019 11.00000 -1.20000 AFIX 0 C59 1 0.321015 0.849719 0.422929 11.00000 0.02426 0.02945 = 0.02454 -0.01035 0.00361 -0.00856 C61 1 0.109868 0.899298 0.459610 11.00000 0.01988 0.03032 = 0.03521 -0.01351 0.00228 -0.00545 AFIX 43 H61 2 0.027695 0.898122 0.480347 11.00000 -1.20000 AFIX 0 C60 1 0.143193 0.973339 0.425815 11.00000 0.02339 0.02924 = 0.04280 -0.00798 -0.00272 -0.00625 AFIX 43 H60 2 0.089113 1.035172 0.418188 11.00000 -1.20000 AFIX 0 C62 1 0.457366 0.683219 0.342076 11.00000 0.01678 0.01431 = 0.02459 -0.00634 -0.00465 -0.00066 C63 1 0.416433 0.548135 0.293148 11.00000 0.03646 0.02728 = 0.03626 -0.01306 -0.00693 -0.01627 AFIX 43 H63 2 0.405176 0.483849 0.287336 11.00000 -1.20000 AFIX 0 C64 1 0.400750 0.618809 0.246997 11.00000 0.03855 0.03151 = 0.02918 -0.01207 -0.00616 -0.00705 AFIX 43 H64 2 0.376728 0.614041 0.201686 11.00000 -1.20000 AFIX 0 C65 1 0.342693 1.004203 0.364089 11.00000 0.02908 0.02951 = 0.03332 -0.00358 -0.00420 -0.00488 AFIX 137 H65A 2 0.430905 0.967986 0.353870 11.00000 -1.50000 H65B 2 0.349604 1.061373 0.389365 11.00000 -1.50000 H65C 2 0.295065 1.024277 0.322355 11.00000 -1.50000 AFIX 0 C66 1 0.216123 0.726006 0.482372 11.00000 0.02944 0.03245 = 0.02352 -0.00020 0.00089 -0.00732 AFIX 23 H66A 2 0.167819 0.728728 0.525280 11.00000 -1.20000 H66B 2 0.306885 0.690069 0.490400 11.00000 -1.20000 AFIX 0 C67 1 0.149716 0.673301 0.431841 11.00000 0.02306 0.03097 = 0.02653 -0.00894 0.00752 -0.00655 C68 1 0.118395 0.705766 0.368438 11.00000 0.02809 0.02221 = 0.02829 -0.00600 -0.00405 -0.00432 AFIX 43 H68 2 0.142230 0.763622 0.352235 11.00000 -1.20000 AFIX 0 C69 1 0.051284 0.654259 0.327099 11.00000 0.03929 0.02922 = 0.03028 -0.01160 -0.00147 -0.00583 AFIX 43 H69 2 0.029427 0.675855 0.282510 11.00000 -1.20000 AFIX 0 C70 1 0.017648 0.571463 0.352602 11.00000 0.02588 0.03051 = 0.04968 -0.01853 -0.00316 -0.00363 AFIX 43 H70 2 -0.031160 0.535964 0.326429 11.00000 -1.20000 AFIX 0 C71 1 0.055461 0.540562 0.416474 11.00000 0.02858 0.03142 = 0.03951 -0.00506 0.00040 -0.01243 AFIX 43 H71 2 0.033870 0.482043 0.432873 11.00000 -1.20000 AFIX 0 C72 1 0.473295 0.533609 0.416653 11.00000 0.03388 0.03282 = 0.02720 0.00367 -0.00422 -0.00549 AFIX 137 H72A 2 0.486509 0.577722 0.451752 11.00000 -1.50000 H72B 2 0.550934 0.481615 0.413741 11.00000 -1.50000 H72C 2 0.396060 0.506040 0.427376 11.00000 -1.50000 AFIX 0 C73 1 0.427026 0.792160 0.241951 11.00000 0.03227 0.02284 = 0.02305 0.00017 -0.01048 -0.00191 AFIX 23 H73A 2 0.398736 0.845439 0.273201 11.00000 -1.20000 H73B 2 0.362659 0.800564 0.204946 11.00000 -1.20000 AFIX 0 C74 1 0.562903 0.799310 0.213291 11.00000 0.02832 0.03329 = 0.01365 -0.00209 -0.00428 -0.00712 C75 1 0.660123 0.719490 0.199725 11.00000 0.04198 0.02640 = 0.02213 -0.00447 -0.00549 -0.00437 AFIX 43 H75 2 0.646028 0.656126 0.208942 11.00000 -1.20000 AFIX 0 C76 1 0.777730 0.733571 0.172610 11.00000 0.03123 0.05578 = 0.03261 -0.00726 -0.00822 0.00782 AFIX 43 H76 2 0.846430 0.680280 0.163476 11.00000 -1.20000 AFIX 0 C77 1 0.793184 0.827945 0.158964 11.00000 0.03787 0.06360 = 0.05148 0.00978 -0.00210 -0.02081 AFIX 43 H77 2 0.872488 0.840169 0.139997 11.00000 -1.20000 AFIX 0 C78 1 0.692425 0.902181 0.173350 11.00000 0.03389 0.04742 = 0.08689 0.02443 -0.00473 -0.00815 AFIX 43 H78 2 0.703666 0.965992 0.163147 11.00000 -1.20000 AFIX 0 O1 6 0.202508 0.571396 0.605001 11.00000 0.04724 0.03918 = 0.05583 0.00433 -0.01535 -0.01299 HKLF 4 REM fjl128dm in P-1 REM R1 = 0.0498 for 9250 Fo > 4sig(Fo) and 0.0885 for all 14370 data REM 662 parameters refined using 0 restraints END ; 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 0.37807(3) 0.25227(2) 0.080025(13) 0.02283(8) Uani 1 1 d . . . Ir51 Ir 0.50807(3) 0.77239(2) 0.411902(13) 0.02113(8) Uani 1 1 d . . . Br1 Br 0.96500(8) 0.76510(7) 0.62372(4) 0.0360(2) Uani 1 1 d . . . Br51 Br 0.84822(8) 0.23030(7) 0.87684(4) 0.0419(2) Uani 1 1 d . . . N1 N 0.2416(6) 0.0776(5) 0.0822(3) 0.0288(14) Uani 1 1 d . . . N2 N 0.1140(6) 0.2014(5) 0.0378(3) 0.0309(15) Uani 1 1 d . . . N3 N 0.2172(6) 0.4324(4) 0.1451(3) 0.0266(14) Uani 1 1 d . . . N4 N 0.2569(6) 0.3166(5) 0.2170(3) 0.0241(13) Uani 1 1 d . . . N5 N -0.1204(7) 0.4270(6) 0.0684(4) 0.0470(19) Uani 1 1 d . . . N6 N 0.4822(6) 0.2939(5) 0.2969(3) 0.0274(14) Uani 1 1 d . . . N52 N 0.2196(6) 0.8237(4) 0.4586(3) 0.0245(13) Uani 1 1 d . . . N51 N 0.2721(6) 0.9432(4) 0.4037(3) 0.0245(13) Uani 1 1 d . . . N54 N 0.4258(6) 0.7009(5) 0.2769(3) 0.0254(14) Uani 1 1 d . . . N53 N 0.4527(6) 0.5872(4) 0.3518(3) 0.0255(13) Uani 1 1 d . . . N55 N 0.1210(6) 0.5883(5) 0.4569(3) 0.0317(15) Uani 1 1 d . . . N56 N 0.5770(7) 0.8908(5) 0.2013(4) 0.0424(18) Uani 1 1 d . . . C1 C 0.5658(7) 0.2762(6) 0.1180(4) 0.0295(18) Uani 1 1 d . . . H1 H 0.5273 0.2828 0.1612 0.035 Uiso 1 1 calc R . . C2 C 0.5200(7) 0.3493(5) 0.0710(4) 0.0265(16) Uani 1 1 d . . . H2 H 0.4492 0.3994 0.0834 0.032 Uiso 1 1 calc R . . C3 C 0.5759(8) 0.3535(6) 0.0022(4) 0.0359(19) Uani 1 1 d . . . H3A H 0.6692 0.3202 0.0028 0.043 Uiso 1 1 calc R . . H3B H 0.5725 0.4218 -0.0113 0.043 Uiso 1 1 calc R . . C4 C 0.5008(8) 0.3063(7) -0.0499(4) 0.040(2) Uani 1 1 d . . . H4A H 0.4270 0.3555 -0.0679 0.048 Uiso 1 1 calc R . . H4B H 0.5607 0.2842 -0.0875 0.048 Uiso 1 1 calc R . . C5 C 0.4482(7) 0.2227(6) -0.0219(3) 0.0310(19) Uani 1 1 d . . . H5 H 0.3600 0.2203 -0.0328 0.037 Uiso 1 1 calc R . . C6 C 0.5156(7) 0.1484(6) 0.0183(4) 0.0276(17) Uani 1 1 d . . . H6 H 0.4705 0.0995 0.0331 0.033 Uiso 1 1 calc R . . C7 C 0.6557(7) 0.1401(6) 0.0399(4) 0.0332(18) Uani 1 1 d . . . H7A H 0.7032 0.1703 0.0049 0.040 Uiso 1 1 calc R . . H7B H 0.6977 0.0710 0.0437 0.040 Uiso 1 1 calc R . . C8 C 0.6704(7) 0.1878(6) 0.1068(4) 0.0336(19) Uani 1 1 d . . . H8A H 0.6669 0.1403 0.1437 0.040 Uiso 1 1 calc R . . H8B H 0.7576 0.2059 0.1082 0.040 Uiso 1 1 calc R . . C9 C 0.2332(7) 0.1741(6) 0.0673(3) 0.0246(16) Uani 1 1 d . . . C10 C 0.1307(8) 0.0460(6) 0.0617(4) 0.0339(19) Uani 1 1 d . . . H10 H 0.1147 -0.0177 0.0661 0.041 Uiso 1 1 calc R . . C11 C 0.0502(8) 0.1232(6) 0.0343(4) 0.037(2) Uani 1 1 d . . . H11 H -0.0343 0.1246 0.0159 0.044 Uiso 1 1 calc R . . C12 C 0.2761(7) 0.3388(5) 0.1520(3) 0.0246(16) Uani 1 1 d . . . C14 C 0.1876(7) 0.3942(5) 0.2501(3) 0.0266(16) Uani 1 1 d . . . H14 H 0.1635 0.3956 0.2959 0.032 Uiso 1 1 calc R . . C13 C 0.1599(7) 0.4686(6) 0.2051(4) 0.0297(17) Uani 1 1 d . . . H13 H 0.1118 0.5319 0.2127 0.036 Uiso 1 1 calc R . . C15 C 0.3473(8) 0.0134(6) 0.1214(4) 0.0360(19) Uani 1 1 d . . . H15A H 0.4178 0.0481 0.1305 0.054 Uiso 1 1 calc R . . H15B H 0.3826 -0.0441 0.0957 0.054 Uiso 1 1 calc R . . H15C H 0.3111 -0.0060 0.1637 0.054 Uiso 1 1 calc R . . C16 C 0.0502(8) 0.3003(6) 0.0245(4) 0.036(2) Uani 1 1 d . . . H16A H -0.0047 0.3036 -0.0161 0.043 Uiso 1 1 calc R . . H16B H 0.1177 0.3395 0.0156 0.043 Uiso 1 1 calc R . . C17 C -0.0358(7) 0.3425(6) 0.0826(4) 0.0322(18) Uani 1 1 d . . . C18 C -0.0300(7) 0.2998(6) 0.1462(4) 0.0295(17) Uani 1 1 d . . . H18 H 0.0302 0.2409 0.1552 0.035 Uiso 1 1 calc R . . C19 C -0.1106(8) 0.3421(7) 0.1959(4) 0.039(2) Uani 1 1 d . . . H19 H -0.1077 0.3122 0.2390 0.046 Uiso 1 1 calc R . . C20 C -0.1960(9) 0.4282(7) 0.1831(5) 0.049(2) Uani 1 1 d . . . H20 H -0.2518 0.4602 0.2167 0.059 Uiso 1 1 calc R . . C21 C -0.1962(9) 0.4654(7) 0.1190(5) 0.053(3) Uani 1 1 d . . . H21 H -0.2561 0.5243 0.1097 0.063 Uiso 1 1 calc R . . C22 C 0.1997(8) 0.4905(6) 0.0827(4) 0.0324(18) Uani 1 1 d . . . H22A H 0.2602 0.4585 0.0487 0.049 Uiso 1 1 calc R . . H22B H 0.2182 0.5545 0.0907 0.049 Uiso 1 1 calc R . . H22C H 0.1091 0.4971 0.0670 0.049 Uiso 1 1 calc R . . C23 C 0.3092(7) 0.2215(5) 0.2493(3) 0.0225(15) Uani 1 1 d . . . H23A H 0.3074 0.1702 0.2168 0.027 Uiso 1 1 calc R . . H23B H 0.2518 0.2111 0.2873 0.027 Uiso 1 1 calc R . . C24 C 0.4476(7) 0.2134(6) 0.2742(3) 0.0264(16) Uani 1 1 d . . . C25 C 0.5335(7) 0.1230(6) 0.2749(4) 0.0317(18) Uani 1 1 d . . . H25 H 0.5067 0.0683 0.2573 0.038 Uiso 1 1 calc R . . C26 C 0.6569(8) 0.1151(6) 0.3015(4) 0.0373(19) Uani 1 1 d . . . H26 H 0.7159 0.0544 0.3039 0.045 Uiso 1 1 calc R . . C27 C 0.6944(8) 0.1985(7) 0.3253(4) 0.041(2) Uani 1 1 d . . . H27 H 0.7788 0.1952 0.3443 0.050 Uiso 1 1 calc R . . C28 C 0.6055(7) 0.2854(6) 0.3203(4) 0.0319(18) Uani 1 1 d . . . H28 H 0.6328 0.3421 0.3342 0.038 Uiso 1 1 calc R . . C51 C 0.7114(7) 0.7512(6) 0.3764(4) 0.0273(17) Uani 1 1 d . . . H51 H 0.6800 0.7445 0.3327 0.033 Uiso 1 1 calc R . . C52 C 0.7034(7) 0.6763(6) 0.4221(4) 0.0294(18) Uani 1 1 d . . . H52 H 0.6646 0.6250 0.4077 0.035 Uiso 1 1 calc R . . C53 C 0.7527(7) 0.6726(6) 0.4927(4) 0.0342(19) Uani 1 1 d . . . H53A H 0.8288 0.7049 0.4941 0.041 Uiso 1 1 calc R . . H53B H 0.7837 0.6043 0.5068 0.041 Uiso 1 1 calc R . . C54 C 0.6473(8) 0.7212(6) 0.5430(4) 0.0339(19) Uani 1 1 d . . . H54A H 0.5995 0.6721 0.5609 0.041 Uiso 1 1 calc R . . H54B H 0.6921 0.7445 0.5809 0.041 Uiso 1 1 calc R . . C55 C 0.5510(8) 0.8030(6) 0.5142(4) 0.0303(17) Uani 1 1 d . . . H55 H 0.4611 0.8045 0.5240 0.036 Uiso 1 1 calc R . . C56 C 0.5796(7) 0.8785(6) 0.4739(4) 0.0313(19) Uani 1 1 d . . . H56 H 0.5092 0.9269 0.4577 0.038 Uiso 1 1 calc R . . C57 C 0.7199(7) 0.8859(6) 0.4553(4) 0.0336(19) Uani 1 1 d . . . H57A H 0.7802 0.8530 0.4905 0.040 Uiso 1 1 calc R . . H57B H 0.7267 0.9547 0.4536 0.040 Uiso 1 1 calc R . . C58 C 0.7635(8) 0.8411(6) 0.3878(4) 0.037(2) Uani 1 1 d . . . H58A H 0.7324 0.8889 0.3515 0.044 Uiso 1 1 calc R . . H58B H 0.8607 0.8255 0.3860 0.044 Uiso 1 1 calc R . . C59 C 0.3210(7) 0.8497(6) 0.4229(3) 0.0255(16) Uani 1 1 d . . . C61 C 0.1099(7) 0.8993(6) 0.4596(4) 0.0282(17) Uani 1 1 d . . . H61 H 0.0277 0.8981 0.4803 0.034 Uiso 1 1 calc R . . C60 C 0.1432(7) 0.9733(6) 0.4258(4) 0.0315(18) Uani 1 1 d . . . H60 H 0.0891 1.0352 0.4182 0.038 Uiso 1 1 calc R . . C62 C 0.4574(6) 0.6832(5) 0.3421(3) 0.0188(14) Uani 1 1 d . . . C63 C 0.4164(7) 0.5481(6) 0.2931(4) 0.0317(18) Uani 1 1 d . . . H63 H 0.4052 0.4838 0.2873 0.038 Uiso 1 1 calc R . . C64 C 0.4007(8) 0.6188(6) 0.2470(4) 0.0328(18) Uani 1 1 d . . . H64 H 0.3767 0.6140 0.2017 0.039 Uiso 1 1 calc R . . C65 C 0.3427(7) 1.0042(6) 0.3641(4) 0.0307(17) Uani 1 1 d . . . H65A H 0.4309 0.9680 0.3539 0.046 Uiso 1 1 calc R . . H65B H 0.3496 1.0614 0.3894 0.046 Uiso 1 1 calc R . . H65C H 0.2951 1.0243 0.3224 0.046 Uiso 1 1 calc R . . C66 C 0.2161(7) 0.7260(6) 0.4824(3) 0.0283(17) Uani 1 1 d . . . H66A H 0.1678 0.7287 0.5253 0.034 Uiso 1 1 calc R . . H66B H 0.3069 0.6901 0.4904 0.034 Uiso 1 1 calc R . . C67 C 0.1497(7) 0.6733(6) 0.4318(3) 0.0266(16) Uani 1 1 d . . . C68 C 0.1184(7) 0.7058(5) 0.3684(4) 0.0262(16) Uani 1 1 d . . . H68 H 0.1422 0.7636 0.3522 0.031 Uiso 1 1 calc R . . C69 C 0.0513(8) 0.6543(6) 0.3271(4) 0.0329(18) Uani 1 1 d . . . H69 H 0.0294 0.6759 0.2825 0.039 Uiso 1 1 calc R . . C70 C 0.0176(7) 0.5715(6) 0.3526(4) 0.0353(19) Uani 1 1 d . . . H70 H -0.0312 0.5360 0.3264 0.042 Uiso 1 1 calc R . . C71 C 0.0555(7) 0.5406(6) 0.4165(4) 0.0322(18) Uani 1 1 d . . . H71 H 0.0339 0.4820 0.4329 0.039 Uiso 1 1 calc R . . C72 C 0.4733(8) 0.5336(6) 0.4167(4) 0.0315(18) Uani 1 1 d . . . H72A H 0.4865 0.5777 0.4518 0.047 Uiso 1 1 calc R . . H72B H 0.5509 0.4816 0.4137 0.047 Uiso 1 1 calc R . . H72C H 0.3961 0.5060 0.4274 0.047 Uiso 1 1 calc R . . C73 C 0.4270(7) 0.7922(5) 0.2420(3) 0.0265(16) Uani 1 1 d . . . H73A H 0.3987 0.8454 0.2732 0.032 Uiso 1 1 calc R . . H73B H 0.3627 0.8006 0.2049 0.032 Uiso 1 1 calc R . . C74 C 0.5629(7) 0.7993(6) 0.2133(3) 0.0249(16) Uani 1 1 d . . . C75 C 0.6601(8) 0.7195(6) 0.1997(3) 0.0304(18) Uani 1 1 d . . . H75 H 0.6460 0.6561 0.2089 0.037 Uiso 1 1 calc R . . C76 C 0.7777(8) 0.7336(7) 0.1726(4) 0.042(2) Uani 1 1 d . . . H76 H 0.8464 0.6803 0.1635 0.050 Uiso 1 1 calc R . . C77 C 0.7932(9) 0.8279(8) 0.1590(5) 0.050(2) Uani 1 1 d . . . H77 H 0.8725 0.8402 0.1400 0.060 Uiso 1 1 calc R . . C78 C 0.6924(9) 0.9022(8) 0.1734(5) 0.057(3) Uani 1 1 d . . . H78 H 0.7037 0.9660 0.1631 0.068 Uiso 1 1 calc R . . O1 O 0.2025(6) 0.5714(4) 0.6050(3) 0.0468(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.02073(15) 0.03056(18) 0.01831(14) -0.00584(11) -0.00112(10) -0.00709(12) Ir51 0.02002(15) 0.02398(17) 0.01916(14) -0.00612(11) -0.00292(10) -0.00306(12) Br1 0.0268(4) 0.0491(5) 0.0310(4) -0.0007(4) -0.0008(3) -0.0046(4) Br51 0.0291(4) 0.0547(6) 0.0411(5) -0.0120(4) -0.0079(3) -0.0048(4) N1 0.024(3) 0.027(4) 0.038(4) -0.011(3) -0.004(3) -0.010(3) N2 0.022(3) 0.033(4) 0.036(4) -0.013(3) -0.007(3) 0.001(3) N3 0.027(3) 0.025(4) 0.030(3) 0.000(3) -0.003(2) -0.009(3) N4 0.024(3) 0.033(4) 0.017(3) -0.007(2) -0.001(2) -0.010(3) N5 0.045(5) 0.041(5) 0.049(5) -0.009(4) -0.014(3) 0.006(4) N6 0.023(3) 0.029(4) 0.032(3) -0.006(3) -0.003(2) -0.007(3) N52 0.025(3) 0.024(3) 0.027(3) -0.005(3) 0.004(2) -0.008(3) N51 0.021(3) 0.023(3) 0.029(3) -0.002(3) 0.000(2) -0.002(3) N54 0.026(3) 0.031(4) 0.020(3) -0.001(3) -0.008(2) -0.007(3) N53 0.024(3) 0.026(4) 0.026(3) -0.003(3) -0.005(2) -0.004(3) N55 0.025(3) 0.031(4) 0.041(4) 0.000(3) -0.003(3) -0.010(3) N56 0.038(4) 0.038(5) 0.052(5) 0.005(4) -0.007(3) -0.008(3) C1 0.022(4) 0.046(5) 0.026(4) -0.004(3) 0.003(3) -0.018(4) C2 0.024(4) 0.027(4) 0.030(4) -0.008(3) 0.004(3) -0.008(3) C3 0.035(5) 0.039(5) 0.033(4) 0.001(4) 0.008(3) -0.005(4) C4 0.036(5) 0.061(6) 0.021(4) 0.009(4) -0.001(3) -0.003(4) C5 0.024(4) 0.056(6) 0.014(3) -0.010(3) 0.002(3) -0.009(4) C6 0.023(4) 0.034(5) 0.026(4) -0.007(3) 0.007(3) -0.005(3) C7 0.027(4) 0.038(5) 0.033(4) -0.003(4) -0.001(3) -0.005(4) C8 0.024(4) 0.050(6) 0.029(4) 0.003(4) -0.005(3) -0.012(4) C9 0.018(4) 0.033(5) 0.022(3) -0.009(3) 0.002(3) -0.003(3) C10 0.030(4) 0.025(4) 0.046(5) -0.009(4) -0.008(3) -0.004(4) C11 0.032(4) 0.034(5) 0.049(5) -0.017(4) -0.012(4) -0.014(4) C12 0.029(4) 0.024(4) 0.024(4) -0.003(3) -0.009(3) -0.011(3) C14 0.028(4) 0.031(4) 0.020(3) -0.010(3) 0.000(3) -0.002(3) C13 0.028(4) 0.030(5) 0.032(4) -0.014(3) 0.002(3) -0.005(3) C15 0.035(5) 0.035(5) 0.037(5) -0.002(4) -0.008(3) -0.005(4) C16 0.036(5) 0.039(5) 0.033(4) -0.004(4) -0.016(3) -0.007(4) C17 0.027(4) 0.029(5) 0.042(5) -0.010(4) -0.008(3) -0.009(4) C18 0.023(4) 0.033(5) 0.034(4) -0.005(3) -0.004(3) -0.009(3) C19 0.036(5) 0.046(6) 0.035(5) -0.003(4) 0.002(3) -0.010(4) C20 0.037(5) 0.051(6) 0.056(6) -0.010(5) 0.003(4) 0.001(5) C21 0.039(5) 0.048(6) 0.065(7) -0.012(5) -0.008(5) 0.009(5) C22 0.040(5) 0.028(4) 0.030(4) 0.007(3) 0.000(3) -0.010(4) C23 0.027(4) 0.023(4) 0.018(3) 0.000(3) 0.001(3) -0.007(3) C24 0.025(4) 0.033(5) 0.023(4) -0.005(3) 0.003(3) -0.009(3) C25 0.024(4) 0.037(5) 0.036(4) 0.003(4) -0.001(3) -0.010(4) C26 0.032(5) 0.030(5) 0.046(5) 0.007(4) 0.002(4) 0.001(4) C27 0.028(4) 0.058(6) 0.040(5) 0.008(4) -0.007(3) -0.013(4) C28 0.030(4) 0.044(5) 0.027(4) -0.005(3) -0.002(3) -0.019(4) C51 0.021(4) 0.034(5) 0.029(4) -0.007(3) -0.003(3) -0.007(3) C52 0.020(4) 0.025(4) 0.042(4) -0.018(3) -0.008(3) 0.000(3) C53 0.027(4) 0.035(5) 0.040(5) 0.002(4) -0.012(3) -0.003(4) C54 0.041(5) 0.042(5) 0.022(4) -0.001(3) -0.004(3) -0.017(4) C55 0.032(4) 0.035(5) 0.024(4) -0.006(3) -0.002(3) -0.008(4) C56 0.032(4) 0.029(5) 0.029(4) -0.018(3) -0.010(3) 0.006(3) C57 0.032(4) 0.025(4) 0.047(5) -0.011(4) -0.010(3) -0.012(4) C58 0.023(4) 0.043(5) 0.045(5) -0.003(4) -0.005(3) -0.010(4) C59 0.024(4) 0.029(4) 0.025(4) -0.010(3) 0.004(3) -0.009(3) C61 0.020(4) 0.030(5) 0.035(4) -0.014(3) 0.002(3) -0.005(3) C60 0.023(4) 0.029(5) 0.043(5) -0.008(4) -0.003(3) -0.006(3) C62 0.017(3) 0.014(4) 0.025(3) -0.006(3) -0.005(3) -0.001(3) C63 0.036(4) 0.027(4) 0.036(4) -0.013(3) -0.007(3) -0.016(4) C64 0.039(5) 0.032(5) 0.029(4) -0.012(3) -0.006(3) -0.007(4) C65 0.029(4) 0.030(5) 0.033(4) -0.004(3) -0.004(3) -0.005(3) C66 0.029(4) 0.032(5) 0.024(4) 0.000(3) 0.001(3) -0.007(3) C67 0.023(4) 0.031(5) 0.027(4) -0.009(3) 0.008(3) -0.007(3) C68 0.028(4) 0.022(4) 0.028(4) -0.006(3) -0.004(3) -0.004(3) C69 0.039(5) 0.029(5) 0.030(4) -0.012(3) -0.001(3) -0.006(4) C70 0.026(4) 0.031(5) 0.050(5) -0.019(4) -0.003(3) -0.004(4) C71 0.029(4) 0.031(5) 0.040(5) -0.005(4) 0.000(3) -0.012(4) C72 0.034(4) 0.033(5) 0.027(4) 0.004(3) -0.004(3) -0.005(4) C73 0.032(4) 0.023(4) 0.023(4) 0.000(3) -0.010(3) -0.002(3) C74 0.028(4) 0.033(5) 0.014(3) -0.002(3) -0.004(3) -0.007(3) C75 0.042(5) 0.026(4) 0.022(4) -0.004(3) -0.005(3) -0.004(4) C76 0.031(5) 0.056(6) 0.033(4) -0.007(4) -0.008(3) 0.008(4) C77 0.038(5) 0.064(7) 0.051(6) 0.010(5) -0.002(4) -0.021(5) C78 0.034(5) 0.047(6) 0.087(8) 0.024(6) -0.005(5) -0.008(5) O1 0.047(4) 0.039(4) 0.056(4) 0.004(3) -0.015(3) -0.013(3) _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 C9 2.058(7) . ? Ir1 C12 2.062(7) . ? Ir1 C5 2.186(7) . ? Ir1 C1 2.189(7) . ? Ir1 C2 2.210(7) . ? Ir1 C6 2.229(7) . ? Ir51 C59 2.045(7) . ? Ir51 C62 2.047(6) . ? Ir51 C55 2.172(7) . ? Ir51 C51 2.190(7) . ? Ir51 C52 2.213(7) . ? Ir51 C56 2.215(7) . ? N1 C9 1.376(10) . ? N1 C10 1.385(9) . ? N1 C15 1.491(10) . ? N2 C9 1.356(9) . ? N2 C11 1.401(10) . ? N2 C16 1.443(10) . ? N3 C12 1.347(9) . ? N3 C13 1.400(9) . ? N3 C22 1.470(9) . ? N4 C12 1.353(9) . ? N4 C14 1.372(9) . ? N4 C23 1.481(9) . ? N5 C21 1.337(12) . ? N5 C17 1.360(10) . ? N6 C28 1.349(9) . ? N6 C24 1.350(9) . ? N52 C59 1.374(9) . ? N52 C61 1.400(9) . ? N52 C66 1.457(9) . ? N51 C59 1.365(9) . ? N51 C60 1.395(9) . ? N51 C65 1.457(9) . ? N54 C62 1.353(8) . ? N54 C64 1.390(9) . ? N54 C73 1.454(9) . ? N53 C62 1.378(9) . ? N53 C63 1.396(8) . ? N53 C72 1.480(9) . ? N55 C71 1.339(9) . ? N55 C67 1.377(10) . ? N56 C74 1.346(10) . ? N56 C78 1.357(12) . ? C1 C2 1.393(11) . ? C1 C8 1.506(11) . ? C1 H1 0.9500 . ? C2 C3 1.496(10) . ? C2 H2 0.9500 . ? C3 C4 1.548(11) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.494(12) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.383(11) . ? C5 H5 0.9500 . ? C6 C7 1.502(10) . ? C6 H6 0.9500 . ? C7 C8 1.538(10) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C10 C11 1.344(11) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C14 C13 1.354(11) . ? C14 H14 0.9500 . ? C13 H13 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.522(11) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.393(11) . ? C18 C19 1.368(11) . ? C18 H18 0.9500 . ? C19 C20 1.375(12) . ? C19 H19 0.9500 . ? C20 C21 1.373(13) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.506(10) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.407(11) . ? C25 C26 1.374(11) . ? C25 H25 0.9500 . ? C26 C27 1.409(12) . ? C26 H26 0.9500 . ? C27 C28 1.385(12) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C51 C52 1.396(11) . ? C51 C58 1.501(11) . ? C51 H51 0.9500 . ? C52 C53 1.503(10) . ? C52 H52 0.9500 . ? C53 C54 1.553(11) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.478(11) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.399(11) . ? C55 H55 0.9500 . ? C56 C57 1.525(11) . ? C56 H56 0.9500 . ? C57 C58 1.534(11) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C61 C60 1.334(11) . ? C61 H61 0.9500 . ? C60 H60 0.9500 . ? C63 C64 1.330(11) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C67 1.519(10) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.358(10) . ? C68 C69 1.394(10) . ? C68 H68 0.9500 . ? C69 C70 1.373(11) . ? C69 H69 0.9500 . ? C70 C71 1.375(11) . ? C70 H70 0.9500 . ? C71 H71 0.9500 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C74 1.542(10) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.388(10) . ? C75 C76 1.382(12) . ? C75 H75 0.9500 . ? C76 C77 1.396(13) . ? C76 H76 0.9500 . ? C77 C78 1.362(13) . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? 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 C9 Ir1 C12 94.4(3) . . ? C9 Ir1 C5 90.9(3) . . ? C12 Ir1 C5 153.1(3) . . ? C9 Ir1 C1 154.6(3) . . ? C12 Ir1 C1 91.3(3) . . ? C5 Ir1 C1 95.2(3) . . ? C9 Ir1 C2 167.1(3) . . ? C12 Ir1 C2 90.1(3) . . ? C5 Ir1 C2 79.8(3) . . ? C1 Ir1 C2 36.9(3) . . ? C9 Ir1 C6 90.4(3) . . ? C12 Ir1 C6 168.9(3) . . ? C5 Ir1 C6 36.5(3) . . ? C1 Ir1 C6 80.3(3) . . ? C2 Ir1 C6 87.4(3) . . ? C59 Ir51 C62 94.4(3) . . ? C59 Ir51 C55 89.7(3) . . ? C62 Ir51 C55 151.2(3) . . ? C59 Ir51 C51 153.9(3) . . ? C62 Ir51 C51 92.9(3) . . ? C55 Ir51 C51 95.8(3) . . ? C59 Ir51 C52 167.5(3) . . ? C62 Ir51 C52 89.8(3) . . ? C55 Ir51 C52 81.1(3) . . ? C51 Ir51 C52 37.0(3) . . ? C59 Ir51 C56 89.0(3) . . ? C62 Ir51 C56 170.7(3) . . ? C55 Ir51 C56 37.2(3) . . ? C51 Ir51 C56 80.5(3) . . ? C52 Ir51 C56 88.7(3) . . ? C9 N1 C10 111.7(6) . . ? C9 N1 C15 126.6(6) . . ? C10 N1 C15 121.5(7) . . ? C9 N2 C11 110.9(7) . . ? C9 N2 C16 124.3(6) . . ? C11 N2 C16 123.7(6) . . ? C12 N3 C13 111.6(6) . . ? C12 N3 C22 126.6(6) . . ? C13 N3 C22 121.5(6) . . ? C12 N4 C14 111.7(6) . . ? C12 N4 C23 124.3(6) . . ? C14 N4 C23 123.9(6) . . ? C21 N5 C17 115.9(8) . . ? C28 N6 C24 117.4(7) . . ? C59 N52 C61 111.2(6) . . ? C59 N52 C66 124.9(6) . . ? C61 N52 C66 123.0(6) . . ? C59 N51 C60 111.3(6) . . ? C59 N51 C65 125.1(6) . . ? C60 N51 C65 123.6(6) . . ? C62 N54 C64 111.1(6) . . ? C62 N54 C73 124.0(6) . . ? C64 N54 C73 124.7(6) . . ? C62 N53 C63 110.8(6) . . ? C62 N53 C72 125.1(6) . . ? C63 N53 C72 123.9(6) . . ? C71 N55 C67 116.7(7) . . ? C74 N56 C78 116.3(8) . . ? C2 C1 C8 126.2(7) . . ? C2 C1 Ir1 72.4(4) . . ? C8 C1 Ir1 109.3(5) . . ? C2 C1 H1 116.9 . . ? C8 C1 H1 116.9 . . ? Ir1 C1 H1 88.3 . . ? C1 C2 C3 123.7(7) . . ? C1 C2 Ir1 70.7(4) . . ? C3 C2 Ir1 113.1(5) . . ? C1 C2 H2 118.1 . . ? C3 C2 H2 118.1 . . ? Ir1 C2 H2 86.2 . . ? C2 C3 C4 112.4(7) . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 113.2(6) . . ? C5 C4 H4A 108.9 . . ? C3 C4 H4A 108.9 . . ? C5 C4 H4B 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C6 C5 C4 126.2(7) . . ? C6 C5 Ir1 73.4(4) . . ? C4 C5 Ir1 109.8(5) . . ? C6 C5 H5 116.9 . . ? C4 C5 H5 116.9 . . ? Ir1 C5 H5 86.6 . . ? C5 C6 C7 124.1(7) . . ? C5 C6 Ir1 70.1(4) . . ? C7 C6 Ir1 111.7(5) . . ? C5 C6 H6 118.0 . . ? C7 C6 H6 118.0 . . ? Ir1 C6 H6 88.3 . . ? C6 C7 C8 113.8(6) . . ? C6 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? C6 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C1 C8 C7 113.1(6) . . ? C1 C8 H8A 109.0 . . ? C7 C8 H8A 109.0 . . ? C1 C8 H8B 109.0 . . ? C7 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? N2 C9 N1 103.8(6) . . ? N2 C9 Ir1 129.3(6) . . ? N1 C9 Ir1 126.7(5) . . ? C11 C10 N1 106.3(7) . . ? C11 C10 H10 126.8 . . ? N1 C10 H10 126.8 . . ? C10 C11 N2 107.3(7) . . ? C10 C11 H11 126.4 . . ? N2 C11 H11 126.4 . . ? N3 C12 N4 104.1(6) . . ? N3 C12 Ir1 127.3(5) . . ? N4 C12 Ir1 128.5(5) . . ? C13 C14 N4 107.1(6) . . ? C13 C14 H14 126.4 . . ? N4 C14 H14 126.4 . . ? C14 C13 N3 105.4(7) . . ? C14 C13 H13 127.3 . . ? N3 C13 H13 127.3 . . ? N1 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 C17 112.0(7) . . ? N2 C16 H16A 109.2 . . ? C17 C16 H16A 109.2 . . ? N2 C16 H16B 109.2 . . ? C17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? N5 C17 C18 121.1(7) . . ? N5 C17 C16 115.2(7) . . ? C18 C17 C16 123.7(7) . . ? C19 C18 C17 120.3(8) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 119.7(8) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C21 C20 C19 116.4(9) . . ? C21 C20 H20 121.8 . . ? C19 C20 H20 121.8 . . ? N5 C21 C20 126.5(9) . . ? N5 C21 H21 116.7 . . ? C20 C21 H21 116.7 . . ? N3 C22 H22A 109.5 . . ? N3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N4 C23 C24 112.3(6) . . ? N4 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? N4 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.9 . . ? N6 C24 C25 122.8(7) . . ? N6 C24 C23 117.9(7) . . ? C25 C24 C23 119.3(7) . . ? C26 C25 C24 118.9(8) . . ? C26 C25 H25 120.6 . . ? C24 C25 H25 120.6 . . ? C25 C26 C27 118.8(8) . . ? C25 C26 H26 120.6 . . ? C27 C26 H26 120.6 . . ? C28 C27 C26 118.5(7) . . ? C28 C27 H27 120.7 . . ? C26 C27 H27 120.7 . . ? N6 C28 C27 123.4(7) . . ? N6 C28 H28 118.3 . . ? C27 C28 H28 118.3 . . ? C52 C51 C58 128.1(7) . . ? C52 C51 Ir51 72.4(4) . . ? C58 C51 Ir51 109.2(5) . . ? C52 C51 H51 115.9 . . ? C58 C51 H51 115.9 . . ? Ir51 C51 H51 88.3 . . ? C51 C52 C53 123.6(7) . . ? C51 C52 Ir51 70.6(4) . . ? C53 C52 Ir51 111.3(5) . . ? C51 C52 H52 118.2 . . ? C53 C52 H52 118.2 . . ? Ir51 C52 H52 88.1 . . ? C52 C53 C54 113.4(6) . . ? C52 C53 H53A 108.9 . . ? C54 C53 H53A 108.9 . . ? C52 C53 H53B 108.9 . . ? C54 C53 H53B 108.9 . . ? H53A C53 H53B 107.7 . . ? C55 C54 C53 114.2(6) . . ? C55 C54 H54A 108.7 . . ? C53 C54 H54A 108.7 . . ? C55 C54 H54B 108.7 . . ? C53 C54 H54B 108.7 . . ? H54A C54 H54B 107.6 . . ? C56 C55 C54 126.3(7) . . ? C56 C55 Ir51 73.1(4) . . ? C54 C55 Ir51 109.4(5) . . ? C56 C55 H55 116.9 . . ? C54 C55 H55 116.9 . . ? Ir51 C55 H55 87.4 . . ? C55 C56 C57 122.3(7) . . ? C55 C56 Ir51 69.8(4) . . ? C57 C56 Ir51 111.3(5) . . ? C55 C56 H56 118.8 . . ? C57 C56 H56 118.8 . . ? Ir51 C56 H56 89.0 . . ? C56 C57 C58 113.0(6) . . ? C56 C57 H57A 109.0 . . ? C58 C57 H57A 109.0 . . ? C56 C57 H57B 109.0 . . ? C58 C57 H57B 109.0 . . ? H57A C57 H57B 107.8 . . ? C51 C58 C57 112.3(7) . . ? C51 C58 H58A 109.2 . . ? C57 C58 H58A 109.2 . . ? C51 C58 H58B 109.2 . . ? C57 C58 H58B 109.2 . . ? H58A C58 H58B 107.9 . . ? N51 C59 N52 103.5(6) . . ? N51 C59 Ir51 128.2(5) . . ? N52 C59 Ir51 127.9(6) . . ? C60 C61 N52 106.6(7) . . ? C60 C61 H61 126.7 . . ? N52 C61 H61 126.7 . . ? C61 C60 N51 107.4(7) . . ? C61 C60 H60 126.3 . . ? N51 C60 H60 126.3 . . ? N54 C62 N53 103.8(5) . . ? N54 C62 Ir51 130.0(5) . . ? N53 C62 Ir51 126.2(5) . . ? C64 C63 N53 106.4(7) . . ? C64 C63 H63 126.8 . . ? N53 C63 H63 126.8 . . ? C63 C64 N54 107.8(6) . . ? C63 C64 H64 126.1 . . ? N54 C64 H64 126.1 . . ? N51 C65 H65A 109.5 . . ? N51 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? N51 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N52 C66 C67 111.0(6) . . ? N52 C66 H66A 109.4 . . ? C67 C66 H66A 109.4 . . ? N52 C66 H66B 109.4 . . ? C67 C66 H66B 109.4 . . ? H66A C66 H66B 108.0 . . ? C68 C67 N55 122.1(6) . . ? C68 C67 C66 124.6(7) . . ? N55 C67 C66 113.3(6) . . ? C67 C68 C69 120.0(7) . . ? C67 C68 H68 120.0 . . ? C69 C68 H68 120.0 . . ? C70 C69 C68 118.2(7) . . ? C70 C69 H69 120.9 . . ? C68 C69 H69 120.9 . . ? C69 C70 C71 119.2(7) . . ? C69 C70 H70 120.4 . . ? C71 C70 H70 120.4 . . ? N55 C71 C70 123.7(8) . . ? N55 C71 H71 118.2 . . ? C70 C71 H71 118.2 . . ? N53 C72 H72A 109.5 . . ? N53 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? N53 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? N54 C73 C74 113.3(6) . . ? N54 C73 H73A 108.9 . . ? C74 C73 H73A 108.9 . . ? N54 C73 H73B 108.9 . . ? C74 C73 H73B 108.9 . . ? H73A C73 H73B 107.7 . . ? N56 C74 C75 123.3(7) . . ? N56 C74 C73 113.2(7) . . ? C75 C74 C73 123.5(7) . . ? C76 C75 C74 119.0(8) . . ? C76 C75 H75 120.5 . . ? C74 C75 H75 120.5 . . ? C75 C76 C77 118.4(8) . . ? C75 C76 H76 120.8 . . ? C77 C76 H76 120.8 . . ? C78 C77 C76 118.8(9) . . ? C78 C77 H77 120.6 . . ? C76 C77 H77 120.6 . . ? N56 C78 C77 124.2(9) . . ? N56 C78 H78 117.9 . . ? C77 C78 H78 117.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 Ir1 C1 C2 168.6(5) . . . . ? C12 Ir1 C1 C2 -88.5(5) . . . . ? C5 Ir1 C1 C2 65.4(5) . . . . ? C6 Ir1 C1 C2 98.8(5) . . . . ? C9 Ir1 C1 C8 45.5(9) . . . . ? C12 Ir1 C1 C8 148.4(5) . . . . ? C5 Ir1 C1 C8 -57.7(6) . . . . ? C2 Ir1 C1 C8 -123.1(7) . . . . ? C6 Ir1 C1 C8 -24.3(5) . . . . ? C8 C1 C2 C3 -4.2(11) . . . . ? Ir1 C1 C2 C3 -105.5(7) . . . . ? C8 C1 C2 Ir1 101.3(7) . . . . ? C9 Ir1 C2 C1 -157.6(11) . . . . ? C12 Ir1 C2 C1 92.0(5) . . . . ? C5 Ir1 C2 C1 -113.1(5) . . . . ? C6 Ir1 C2 C1 -77.1(5) . . . . ? C9 Ir1 C2 C3 -38.3(15) . . . . ? C12 Ir1 C2 C3 -148.7(6) . . . . ? C5 Ir1 C2 C3 6.3(6) . . . . ? C1 Ir1 C2 C3 119.3(8) . . . . ? C6 Ir1 C2 C3 42.2(6) . . . . ? C1 C2 C3 C4 93.6(9) . . . . ? Ir1 C2 C3 C4 12.0(9) . . . . ? C2 C3 C4 C5 -33.2(10) . . . . ? C3 C4 C5 C6 -45.8(11) . . . . ? C3 C4 C5 Ir1 37.7(8) . . . . ? C9 Ir1 C5 C6 -89.4(5) . . . . ? C12 Ir1 C5 C6 169.1(5) . . . . ? C1 Ir1 C5 C6 65.9(5) . . . . ? C2 Ir1 C5 C6 99.6(5) . . . . ? C9 Ir1 C5 C4 147.3(5) . . . . ? C12 Ir1 C5 C4 45.9(9) . . . . ? C1 Ir1 C5 C4 -57.3(6) . . . . ? C2 Ir1 C5 C4 -23.6(5) . . . . ? C6 Ir1 C5 C4 -123.2(7) . . . . ? C4 C5 C6 C7 -0.5(12) . . . . ? Ir1 C5 C6 C7 -103.2(7) . . . . ? C4 C5 C6 Ir1 102.7(7) . . . . ? C9 Ir1 C6 C5 91.0(5) . . . . ? C12 Ir1 C6 C5 -153.8(13) . . . . ? C1 Ir1 C6 C5 -112.7(5) . . . . ? C2 Ir1 C6 C5 -76.3(5) . . . . ? C9 Ir1 C6 C7 -149.2(6) . . . . ? C12 Ir1 C6 C7 -34.0(18) . . . . ? C5 Ir1 C6 C7 119.8(8) . . . . ? C1 Ir1 C6 C7 7.1(6) . . . . ? C2 Ir1 C6 C7 43.5(6) . . . . ? C5 C6 C7 C8 91.5(9) . . . . ? Ir1 C6 C7 C8 11.5(9) . . . . ? C2 C1 C8 C7 -43.6(10) . . . . ? Ir1 C1 C8 C7 38.2(8) . . . . ? C6 C7 C8 C1 -33.4(10) . . . . ? C11 N2 C9 N1 -0.3(8) . . . . ? C16 N2 C9 N1 167.9(7) . . . . ? C11 N2 C9 Ir1 174.6(5) . . . . ? C16 N2 C9 Ir1 -17.3(11) . . . . ? C10 N1 C9 N2 0.7(8) . . . . ? C15 N1 C9 N2 -173.5(7) . . . . ? C10 N1 C9 Ir1 -174.3(5) . . . . ? C15 N1 C9 Ir1 11.5(10) . . . . ? C12 Ir1 C9 N2 71.8(7) . . . . ? C5 Ir1 C9 N2 -81.8(7) . . . . ? C1 Ir1 C9 N2 174.1(6) . . . . ? C2 Ir1 C9 N2 -38.1(16) . . . . ? C6 Ir1 C9 N2 -118.2(7) . . . . ? C12 Ir1 C9 N1 -114.4(6) . . . . ? C5 Ir1 C9 N1 92.0(6) . . . . ? C1 Ir1 C9 N1 -12.1(10) . . . . ? C2 Ir1 C9 N1 135.6(11) . . . . ? C6 Ir1 C9 N1 55.5(6) . . . . ? C9 N1 C10 C11 -0.8(9) . . . . ? C15 N1 C10 C11 173.7(7) . . . . ? N1 C10 C11 N2 0.6(9) . . . . ? C9 N2 C11 C10 -0.2(9) . . . . ? C16 N2 C11 C10 -168.5(7) . . . . ? C13 N3 C12 N4 -0.7(8) . . . . ? C22 N3 C12 N4 -174.6(6) . . . . ? C13 N3 C12 Ir1 -178.5(5) . . . . ? C22 N3 C12 Ir1 7.5(10) . . . . ? C14 N4 C12 N3 0.0(7) . . . . ? C23 N4 C12 N3 -177.4(6) . . . . ? C14 N4 C12 Ir1 177.9(5) . . . . ? C23 N4 C12 Ir1 0.4(9) . . . . ? C9 Ir1 C12 N3 -107.0(6) . . . . ? C5 Ir1 C12 N3 -6.4(10) . . . . ? C1 Ir1 C12 N3 97.7(6) . . . . ? C2 Ir1 C12 N3 60.8(6) . . . . ? C6 Ir1 C12 N3 138.1(13) . . . . ? C9 Ir1 C12 N4 75.6(6) . . . . ? C5 Ir1 C12 N4 176.3(5) . . . . ? C1 Ir1 C12 N4 -79.6(6) . . . . ? C2 Ir1 C12 N4 -116.5(6) . . . . ? C6 Ir1 C12 N4 -39.2(18) . . . . ? C12 N4 C14 C13 0.6(8) . . . . ? C23 N4 C14 C13 178.1(6) . . . . ? N4 C14 C13 N3 -1.0(8) . . . . ? C12 N3 C13 C14 1.1(8) . . . . ? C22 N3 C13 C14 175.4(6) . . . . ? C9 N2 C16 C17 -89.8(9) . . . . ? C11 N2 C16 C17 76.9(9) . . . . ? C21 N5 C17 C18 0.0(12) . . . . ? C21 N5 C17 C16 -179.6(7) . . . . ? N2 C16 C17 N5 -166.3(6) . . . . ? N2 C16 C17 C18 14.0(10) . . . . ? N5 C17 C18 C19 0.4(11) . . . . ? C16 C17 C18 C19 -180.0(7) . . . . ? C17 C18 C19 C20 -1.2(12) . . . . ? C18 C19 C20 C21 1.4(13) . . . . ? C17 N5 C21 C20 0.3(14) . . . . ? C19 C20 C21 N5 -1.1(15) . . . . ? C12 N4 C23 C24 85.5(8) . . . . ? C14 N4 C23 C24 -91.6(8) . . . . ? C28 N6 C24 C25 0.7(11) . . . . ? C28 N6 C24 C23 178.7(6) . . . . ? N4 C23 C24 N6 33.5(9) . . . . ? N4 C23 C24 C25 -148.5(6) . . . . ? N6 C24 C25 C26 1.9(12) . . . . ? C23 C24 C25 C26 -176.0(7) . . . . ? C24 C25 C26 C27 -2.0(12) . . . . ? C25 C26 C27 C28 -0.5(12) . . . . ? C24 N6 C28 C27 -3.4(11) . . . . ? C26 C27 C28 N6 3.3(12) . . . . ? C59 Ir51 C51 C52 168.0(5) . . . . ? C62 Ir51 C51 C52 -85.8(4) . . . . ? C55 Ir51 C51 C52 66.7(5) . . . . ? C56 Ir51 C51 C52 100.7(5) . . . . ? C59 Ir51 C51 C58 42.9(9) . . . . ? C62 Ir51 C51 C58 149.1(5) . . . . ? C55 Ir51 C51 C58 -58.4(6) . . . . ? C52 Ir51 C51 C58 -125.1(7) . . . . ? C56 Ir51 C51 C58 -24.4(5) . . . . ? C58 C51 C52 C53 -2.3(12) . . . . ? Ir51 C51 C52 C53 -103.2(7) . . . . ? C58 C51 C52 Ir51 100.9(8) . . . . ? C59 Ir51 C52 C51 -155.2(11) . . . . ? C62 Ir51 C52 C51 95.1(4) . . . . ? C55 Ir51 C52 C51 -112.3(5) . . . . ? C56 Ir51 C52 C51 -75.7(5) . . . . ? C59 Ir51 C52 C53 -35.7(15) . . . . ? C62 Ir51 C52 C53 -145.5(6) . . . . ? C55 Ir51 C52 C53 7.2(6) . . . . ? C51 Ir51 C52 C53 119.5(7) . . . . ? C56 Ir51 C52 C53 43.7(6) . . . . ? C51 C52 C53 C54 90.3(9) . . . . ? Ir51 C52 C53 C54 10.0(9) . . . . ? C52 C53 C54 C55 -31.3(10) . . . . ? C53 C54 C55 C56 -46.5(10) . . . . ? C53 C54 C55 Ir51 36.4(8) . . . . ? C59 Ir51 C55 C56 -88.7(5) . . . . ? C62 Ir51 C55 C56 172.7(5) . . . . ? C51 Ir51 C55 C56 65.8(5) . . . . ? C52 Ir51 C55 C56 99.8(5) . . . . ? C59 Ir51 C55 C54 148.1(6) . . . . ? C62 Ir51 C55 C54 49.5(9) . . . . ? C51 Ir51 C55 C54 -57.5(6) . . . . ? C52 Ir51 C55 C54 -23.5(6) . . . . ? C56 Ir51 C55 C54 -123.2(8) . . . . ? C54 C55 C56 C57 -0.9(11) . . . . ? Ir51 C55 C56 C57 -102.9(6) . . . . ? C54 C55 C56 Ir51 102.0(7) . . . . ? C59 Ir51 C56 C55 90.8(5) . . . . ? C51 Ir51 C56 C55 -113.1(5) . . . . ? C52 Ir51 C56 C55 -76.9(5) . . . . ? C59 Ir51 C56 C57 -151.2(6) . . . . ? C55 Ir51 C56 C57 117.9(8) . . . . ? C51 Ir51 C56 C57 4.8(6) . . . . ? C52 Ir51 C56 C57 41.1(6) . . . . ? C55 C56 C57 C58 94.4(9) . . . . ? Ir51 C56 C57 C58 15.6(9) . . . . ? C52 C51 C58 C57 -41.8(11) . . . . ? Ir51 C51 C58 C57 40.5(8) . . . . ? C56 C57 C58 C51 -37.6(10) . . . . ? C60 N51 C59 N52 -1.1(7) . . . . ? C65 N51 C59 N52 -179.9(6) . . . . ? C60 N51 C59 Ir51 -174.0(5) . . . . ? C65 N51 C59 Ir51 7.2(10) . . . . ? C61 N52 C59 N51 1.4(7) . . . . ? C66 N52 C59 N51 171.3(6) . . . . ? C61 N52 C59 Ir51 174.3(5) . . . . ? C66 N52 C59 Ir51 -15.7(9) . . . . ? C62 Ir51 C59 N51 -110.7(6) . . . . ? C55 Ir51 C59 N51 97.8(6) . . . . ? C51 Ir51 C59 N51 -4.9(10) . . . . ? C52 Ir51 C59 N51 140.1(11) . . . . ? C56 Ir51 C59 N51 60.7(6) . . . . ? C62 Ir51 C59 N52 78.1(6) . . . . ? C55 Ir51 C59 N52 -73.4(6) . . . . ? C51 Ir51 C59 N52 -176.1(5) . . . . ? C52 Ir51 C59 N52 -31.2(16) . . . . ? C56 Ir51 C59 N52 -110.6(6) . . . . ? C59 N52 C61 C60 -1.2(8) . . . . ? C66 N52 C61 C60 -171.3(6) . . . . ? N52 C61 C60 N51 0.4(8) . . . . ? C59 N51 C60 C61 0.5(8) . . . . ? C65 N51 C60 C61 179.2(6) . . . . ? C64 N54 C62 N53 0.6(8) . . . . ? C73 N54 C62 N53 -175.4(6) . . . . ? C64 N54 C62 Ir51 178.5(5) . . . . ? C73 N54 C62 Ir51 2.5(10) . . . . ? C63 N53 C62 N54 -1.0(7) . . . . ? C72 N53 C62 N54 -176.7(6) . . . . ? C63 N53 C62 Ir51 -179.0(5) . . . . ? C72 N53 C62 Ir51 5.3(9) . . . . ? C59 Ir51 C62 N54 74.3(6) . . . . ? C55 Ir51 C62 N54 171.7(6) . . . . ? C51 Ir51 C62 N54 -80.6(6) . . . . ? C52 Ir51 C62 N54 -117.5(6) . . . . ? C59 Ir51 C62 N53 -108.3(6) . . . . ? C55 Ir51 C62 N53 -10.9(10) . . . . ? C51 Ir51 C62 N53 96.8(6) . . . . ? C52 Ir51 C62 N53 59.9(6) . . . . ? C62 N53 C63 C64 1.0(9) . . . . ? C72 N53 C63 C64 176.7(7) . . . . ? N53 C63 C64 N54 -0.6(9) . . . . ? C62 N54 C64 C63 -0.1(9) . . . . ? C73 N54 C64 C63 176.0(7) . . . . ? C59 N52 C66 C67 -92.1(8) . . . . ? C61 N52 C66 C67 76.7(8) . . . . ? C71 N55 C67 C68 -2.7(11) . . . . ? C71 N55 C67 C66 176.2(7) . . . . ? N52 C66 C67 C68 10.7(10) . . . . ? N52 C66 C67 N55 -168.1(6) . . . . ? N55 C67 C68 C69 2.1(11) . . . . ? C66 C67 C68 C69 -176.6(7) . . . . ? C67 C68 C69 C70 0.5(11) . . . . ? C68 C69 C70 C71 -2.5(11) . . . . ? C67 N55 C71 C70 0.6(11) . . . . ? C69 C70 C71 N55 2.0(12) . . . . ? C62 N54 C73 C74 86.3(8) . . . . ? C64 N54 C73 C74 -89.2(8) . . . . ? C78 N56 C74 C75 1.4(11) . . . . ? C78 N56 C74 C73 -177.3(7) . . . . ? N54 C73 C74 N56 -159.0(6) . . . . ? N54 C73 C74 C75 22.3(9) . . . . ? N56 C74 C75 C76 0.0(10) . . . . ? C73 C74 C75 C76 178.5(6) . . . . ? C74 C75 C76 C77 -1.0(11) . . . . ? C75 C76 C77 C78 0.5(13) . . . . ? C74 N56 C78 C77 -1.9(14) . . . . ? C76 C77 C78 N56 1.0(15) . . . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.168 _refine_diff_density_min -3.353 _refine_diff_density_rms 0.209 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.004 0.001 0.243 85 39 'C H2 Cl2' 2 -0.004 -0.001 0.757 85 39 'C H2 Cl2' _platon_squeeze_details ; The unit cell contains 2 diclhloromethane molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; _vrf_CHEMW03_cmpnd_5 ; PROBLEM: WARNING: The ratio of given/expected molecular weight as RESPONSE: Difference between given/ expected molecular weight is due to the contribution of highly disordered dichlomethane. The presence of dichloromethane in the unit cell has been established according to accesible voids volume and residual density peaks. Its contribution has been taken into account with SQUEEZE program, although the atoms have not been included in the model atom list as their refinement leads to unrealistic parameters. ; _vrf_PLAT306_cmpnd_5 ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1 Check RESPONSE: Hydrogen atoms of water molecule have not been included in the model, as they have not been observed in Fourier difference maps. ; # end Validation Reply Form #===END # # # ---------------------------------------------------------- # Data for cmpnd_6 (local labelling as fjl230asq) data_cmpnd_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H38 Ir N6, F6 P, 0.5(C4 H10 O)' _chemical_formula_sum 'C38 H43 F6 Ir N6 O0.50 P' _chemical_formula_weight 928.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.1243(9) _cell_length_b 19.5765(15) _cell_length_c 15.7923(12) _cell_angle_alpha 90.00 _cell_angle_beta 102.8500(10) _cell_angle_gamma 90.00 _cell_volume 3654.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9876 _cell_measurement_theta_min 2.188 _cell_measurement_theta_max 28.137 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.265 _exptl_crystal_size_mid 0.235 _exptl_crystal_size_min 0.211 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1852 _exptl_absorpt_coefficient_mu 3.767 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4073 _exptl_absorpt_correction_T_max 0.5286 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within APEX2 package. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD system' _diffrn_measurement_method 'narrow \w frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 42545 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0186 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.41 _reflns_number_total 8498 _reflns_number_gt 7514 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_data_reduction 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material 'XCIF program, PLATON(Spek, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. There are large solvent accessible VOIDS in the structure and two different zones where residual density peaks are observed. However the solvent is disordered so badly that it cannot be modelled even with restraints. Therefore, SQUEEZE corrections have been applied. The total potential solvent accesible void volume (390 \A3) and the electron count (92 e in the unit cell) agree with the presence of two diethyl ether molecules (C4 H10 O). They have been included in the chemical formula, F00 and density. Results of the SQUEEZE calculations are included at the end of this cif file. PF6 counterion has been found to be disordered. Four fluorine atoms have been included in the model in two sets of positions, with complementary occupancy factors (0.746/0.254(6)) and refined with a similarity restraint in P-F bond lengths. Two non-olefinic carbon atoms of cod fragment have also been found to be disordered. They have been isotropically refined, with equal occupancy factors. Restraints in C-C bond lengths have been included in the refinement. Hydrogen atoms have been included in the model in calculated positions and refined with a riding model. ; _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^)+(0.0278P)^2^+4.2871P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8498 _refine_ls_number_parameters 469 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0281 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0569 _refine_ls_wR_factor_gt 0.0549 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL fjl230am in P2(1)/c CELL 0.71073 12.1243 19.5765 15.7923 90.000 102.850 90.000 ZERR 4.00 0.0009 0.0015 0.0012 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N F P IR O UNIT 152 172 24 24 4 4 2 MERG 2 DFIX 1.57 0.02 P1 F1 P1 F2 P1 F3A P1 F4A P1 F5A P1 F6A DFIX 1.57 0.02 P1 F3B P1 F4B P1 F5B P1 F6B DFIX 31.00 0.02 C2 C3A C2 C3B C4 C3A C4 C3B FMAP 2 BOND $H CONF PLAN 30 ACTA 55.00 L.S. 5 TEMP -173.00 WGHT 0.027800 4.287100 FVAR 2.00258 0.74610 1.51633 IR1 6 0.042636 0.066010 0.250438 11.00000 0.03007 0.01574 = 0.01527 0.00145 0.00669 0.00027 N1 3 -0.041471 0.084612 0.417157 11.00000 0.03037 0.02096 = 0.02152 0.00381 0.00894 0.00330 N2 3 0.139767 0.084298 0.448099 11.00000 0.03089 0.01686 = 0.01801 0.00185 0.00832 0.00158 N5 3 0.290288 -0.058473 0.435332 11.00000 0.03046 0.02500 = 0.03120 0.00146 0.00800 -0.00078 N3 3 0.170888 0.196139 0.223854 11.00000 0.02650 0.02121 = 0.02187 0.00567 0.00743 0.00049 N4 3 -0.003869 0.219081 0.214480 11.00000 0.02817 0.01794 = 0.02534 0.00245 0.00657 0.00020 N6 3 -0.341477 0.250774 0.224988 11.00000 0.02715 0.02807 = 0.03193 0.00556 0.00281 -0.00128 C1 1 0.081510 0.042080 0.124461 11.00000 0.08892 0.02351 = 0.02139 0.00314 0.02342 0.00996 AFIX 43 H1 2 0.117422 0.084926 0.121925 11.00000 -1.20000 AFIX 0 C2 1 -0.033964 0.049192 0.113550 11.00000 0.07454 0.03709 = 0.01798 0.00177 0.00221 -0.01935 AFIX 43 H2 2 -0.072012 0.091432 0.115170 11.00000 -1.20000 AFIX 0 PART 3 C3A 1 -0.092166 -0.020427 0.098484 10.50000 0.04203 AFIX 23 H3A1 2 -0.162897 -0.015402 0.053420 10.50000 -1.20000 H3A2 2 -0.042317 -0.052234 0.075643 10.50000 -1.20000 AFIX 0 PART 4 C3B 1 -0.139643 0.002710 0.105648 10.50000 0.03747 AFIX 23 H3B1 2 -0.205784 0.030976 0.110207 10.50000 -1.20000 H3B2 2 -0.156565 -0.019836 0.048094 10.50000 -1.20000 AFIX 0 PART 0 C4 1 -0.119764 -0.050986 0.176273 11.00000 0.06136 0.03866 = 0.03918 0.00995 -0.00901 -0.01841 part 3 AFIX 23 H4A 2 -0.124471 -0.101202 0.168951 10.50000 -1.20000 H4B 2 -0.195048 -0.034433 0.181678 10.50000 -1.20000 AFIX 23 part 0 part 4 H4AB 2 -0.193020 -0.060660 0.191683 10.50000 -1.20000 H4BB 2 -0.095381 -0.093518 0.151852 10.50000 -1.20000 AFIX 0 part 0 C5 1 -0.034648 -0.034533 0.258509 11.00000 0.04643 0.02042 = 0.02597 0.00192 0.00491 -0.00594 AFIX 43 H5 2 -0.062809 -0.017536 0.305955 11.00000 -1.20000 AFIX 0 C6 1 0.080900 -0.042057 0.270813 11.00000 0.04993 0.01740 = 0.02101 -0.00112 0.00884 -0.00026 AFIX 43 H6 2 0.125808 -0.029345 0.325815 11.00000 -1.20000 AFIX 0 C7 1 0.141774 -0.068745 0.204316 11.00000 0.08340 0.03102 = 0.03960 0.00725 0.03055 0.01852 PART 3 AFIX 23 H7A 2 0.094974 -0.105469 0.171218 10.50000 -1.20000 H7B 2 0.213401 -0.089926 0.235678 10.50000 -1.20000 AFIX 23 part 4 H7AB 2 0.224290 -0.065450 0.228328 10.50000 -1.20000 H7BB 2 0.122938 -0.117679 0.193924 10.50000 -1.20000 AFIX 0 part 0 part 3 C8A 1 0.169664 -0.018316 0.140023 10.50000 0.03516 AFIX 23 H8A1 2 0.168576 -0.041754 0.084294 10.50000 -1.20000 H8A2 2 0.246662 0.000156 0.162328 10.50000 -1.20000 AFIX 0 PART 4 C8B 1 0.113930 -0.032051 0.119799 10.50000 0.03470 AFIX 23 H8B1 2 0.050668 -0.056234 0.080908 10.50000 -1.20000 H8B2 2 0.180210 -0.034675 0.092932 10.50000 -1.20000 AFIX 0 PART 0 C9 1 0.049023 0.080056 0.379969 11.00000 0.02611 0.01212 = 0.02218 0.00235 0.00777 0.00111 C10 1 -0.007346 0.092716 0.506163 11.00000 0.03904 0.02734 = 0.01929 0.00245 0.01262 0.00469 AFIX 43 H10 2 -0.055182 0.097210 0.546012 11.00000 -1.20000 AFIX 0 C11 1 0.105559 0.093021 0.525412 11.00000 0.03823 0.02421 = 0.01910 0.00018 0.00869 0.00123 AFIX 43 H11 2 0.153367 0.098231 0.581496 11.00000 -1.20000 AFIX 0 C15 1 -0.159526 0.080935 0.370993 11.00000 0.02897 0.03084 = 0.03159 0.00820 0.01026 0.00238 AFIX 137 H15A 2 -0.163954 0.080330 0.308275 11.00000 -1.50000 H15B 2 -0.200330 0.120823 0.385778 11.00000 -1.50000 H15C 2 -0.193731 0.039176 0.387865 11.00000 -1.50000 AFIX 0 C16 1 0.258747 0.084549 0.440101 11.00000 0.02940 0.01951 = 0.02374 0.00294 0.00900 -0.00107 AFIX 23 H16A 2 0.285193 0.132377 0.439833 11.00000 -1.20000 H16B 2 0.263455 0.063515 0.384005 11.00000 -1.20000 AFIX 0 C17 1 0.335570 0.046293 0.512940 11.00000 0.02612 0.02733 = 0.02446 0.00272 0.00851 -0.00163 C18 1 0.395420 0.080362 0.584679 11.00000 0.03119 0.02844 = 0.03179 -0.00044 0.00567 -0.00029 AFIX 43 H18 2 0.387300 0.128460 0.588477 11.00000 -1.20000 AFIX 0 C19 1 0.469149 0.045122 0.653239 11.00000 0.03476 0.03945 = 0.03501 -0.00312 -0.00102 0.00203 AFIX 43 H19 2 0.509181 0.069603 0.702500 11.00000 -1.20000 AFIX 0 C20 1 0.482459 -0.023459 0.648445 11.00000 0.02845 0.04120 = 0.03375 0.00433 0.00167 0.00493 AFIX 43 H20 2 0.531803 -0.046739 0.694577 11.00000 -1.20000 AFIX 0 C21 1 0.423820 -0.060607 0.575694 11.00000 0.02084 0.02887 = 0.03364 0.00517 0.00881 0.00040 C22 1 0.436974 -0.131837 0.565990 11.00000 0.02607 0.03290 = 0.04195 0.00765 0.01039 0.00397 AFIX 43 H22 2 0.485768 -0.157214 0.610310 11.00000 -1.20000 AFIX 0 C23 1 0.379221 -0.163933 0.492638 11.00000 0.03335 0.02503 = 0.04827 0.00371 0.01451 0.00118 AFIX 43 H23 2 0.388385 -0.211495 0.484431 11.00000 -1.20000 AFIX 0 C24 1 0.306037 -0.124832 0.429756 11.00000 0.03433 0.02436 = 0.03937 -0.00034 0.01012 -0.00248 AFIX 43 H24 2 0.264895 -0.147779 0.379590 11.00000 -1.20000 AFIX 0 C25 1 0.349752 -0.025422 0.507371 11.00000 0.02274 0.02772 = 0.02856 0.00374 0.01018 -0.00144 C12 1 0.072064 0.166878 0.229967 11.00000 0.02716 0.02186 = 0.01561 0.00116 0.00597 0.00127 C13 1 0.157397 0.265155 0.205839 11.00000 0.03460 0.02162 = 0.03201 0.00506 0.00893 -0.00322 AFIX 43 H13 2 0.214791 0.296305 0.198840 11.00000 -1.20000 AFIX 0 C14 1 0.048417 0.279698 0.200149 11.00000 0.03959 0.01742 = 0.03276 0.00696 0.00876 -0.00010 AFIX 43 H14 2 0.013430 0.323149 0.188534 11.00000 -1.20000 AFIX 0 C26 1 0.279757 0.161355 0.237792 11.00000 0.02634 0.03790 = 0.03235 0.01167 0.01142 0.00494 AFIX 137 H26A 2 0.329331 0.178278 0.291356 11.00000 -1.50000 H26B 2 0.314714 0.170322 0.188601 11.00000 -1.50000 H26C 2 0.268413 0.112083 0.242790 11.00000 -1.50000 AFIX 0 C27 1 -0.122296 0.214120 0.217284 11.00000 0.02378 0.02530 = 0.02587 0.00256 0.00082 0.00313 AFIX 23 H27A 2 -0.145367 0.165517 0.212064 11.00000 -1.20000 H27B 2 -0.168125 0.238846 0.166872 11.00000 -1.20000 AFIX 0 C28 1 -0.147331 0.243160 0.299957 11.00000 0.02714 0.01701 = 0.02787 0.00435 0.00540 -0.00096 C29 1 -0.064829 0.252347 0.373957 11.00000 0.02662 0.02202 = 0.03161 0.00145 0.00440 -0.00147 AFIX 43 H29 2 0.010989 0.239923 0.374213 11.00000 -1.20000 AFIX 0 C30 1 -0.090715 0.279969 0.449783 11.00000 0.03467 0.03050 = 0.02693 0.00242 0.00298 -0.00638 AFIX 43 H30 2 -0.032390 0.285457 0.500565 11.00000 -1.20000 AFIX 0 C31 1 -0.198920 0.298899 0.450838 11.00000 0.03798 0.02923 = 0.02823 0.00161 0.01184 -0.00552 AFIX 43 H31 2 -0.215377 0.317849 0.502020 11.00000 -1.20000 AFIX 0 C32 1 -0.286710 0.290240 0.375447 11.00000 0.02915 0.02236 = 0.03296 0.00640 0.01026 -0.00278 C33 1 -0.400225 0.309001 0.371744 11.00000 0.03600 0.03197 = 0.03960 0.00755 0.01915 -0.00088 AFIX 43 H33 2 -0.421066 0.329063 0.420691 11.00000 -1.20000 AFIX 0 C34 1 -0.479506 0.297919 0.296931 11.00000 0.02660 0.03772 = 0.04743 0.01030 0.01263 -0.00006 AFIX 43 H34 2 -0.556295 0.310007 0.293335 11.00000 -1.20000 AFIX 0 C35 1 -0.446565 0.268475 0.225271 11.00000 0.02628 0.03522 = 0.03979 0.00992 0.00284 -0.00098 AFIX 43 H35 2 -0.503193 0.260838 0.173979 11.00000 -1.20000 AFIX 0 C36 1 -0.261150 0.261382 0.299769 11.00000 0.02809 0.01886 = 0.02899 0.00558 0.00682 -0.00206 P1 5 0.312405 0.202342 0.982931 11.00000 0.03586 0.03726 = 0.02488 0.00053 0.00371 -0.01675 F1 4 0.333757 0.149808 0.910799 11.00000 0.06293 0.05186 = 0.04918 -0.01626 0.02009 -0.02385 F2 4 0.295001 0.255263 1.056639 11.00000 0.06566 0.04727 = 0.03887 -0.00729 0.01991 -0.01737 PART 1 F3A 4 0.399471 0.256151 0.958327 21.00000 0.04000 0.04039 = 0.07916 -0.01425 0.03312 -0.01967 F4A 4 0.215271 0.156482 1.006654 21.00000 0.09179 0.06511 = 0.06575 -0.01671 0.04443 -0.05187 F5A 4 0.404219 0.168289 1.053554 21.00000 0.10093 0.06095 = 0.05632 0.00296 -0.02652 0.03223 F6A 4 0.213740 0.243639 0.914870 21.00000 0.04282 0.09115 = 0.04170 0.00877 -0.00395 0.01433 PART 2 F3B 4 0.355413 0.255718 0.925806 -21.00000 0.03712 F4B 4 0.292552 0.133927 1.037688 -21.00000 0.03930 F5B 4 0.452456 0.187057 1.028993 -21.00000 0.03912 F6B 4 0.195881 0.202091 0.933014 -21.00000 0.04315 HKLF 4 REM fjl230am in P2(1)/c REM R1 = 0.0233 for 7514 Fo > 4sig(Fo) and 0.0281 for all 8498 data REM 469 parameters refined using 14 restraints END ; 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 0.042636(8) 0.066010(5) 0.250438(6) 0.02010(4) Uani 1 1 d . C . N1 N -0.04147(19) 0.08461(11) 0.41716(14) 0.0238(5) Uani 1 1 d . C . N2 N 0.13977(19) 0.08430(11) 0.44810(14) 0.0215(4) Uani 1 1 d . C . N5 N 0.2903(2) -0.05847(12) 0.43533(16) 0.0287(5) Uani 1 1 d . C . N3 N 0.17089(18) 0.19614(11) 0.22385(14) 0.0229(4) Uani 1 1 d . C . N4 N -0.00387(19) 0.21908(11) 0.21448(15) 0.0237(5) Uani 1 1 d . C . N6 N -0.3415(2) 0.25077(12) 0.22499(16) 0.0296(5) Uani 1 1 d . C . C1 C 0.0815(4) 0.04208(16) 0.12446(19) 0.0429(9) Uani 1 1 d . . . H1 H 0.1174 0.0849 0.1219 0.051 Uiso 1 1 calc R A 3 C2 C -0.0340(4) 0.04919(18) 0.11355(19) 0.0445(9) Uani 1 1 d D C . H2 H -0.0720 0.0914 0.1152 0.053 Uiso 1 1 calc R B 3 C3A C -0.0922(6) -0.0204(4) 0.0985(4) 0.0420(15) Uiso 0.50 1 d PD C 3 H3A1 H -0.1629 -0.0154 0.0534 0.050 Uiso 0.50 1 calc PR C 3 H3A2 H -0.0423 -0.0522 0.0756 0.050 Uiso 0.50 1 calc PR C 3 C3B C -0.1396(6) 0.0027(3) 0.1056(4) 0.0375(14) Uiso 0.50 1 d PD C 4 H3B1 H -0.2058 0.0310 0.1102 0.045 Uiso 0.50 1 calc PR C 4 H3B2 H -0.1566 -0.0198 0.0481 0.045 Uiso 0.50 1 calc PR C 4 C4 C -0.1198(3) -0.05099(18) 0.1763(2) 0.0495(9) Uani 1 1 d D . . H4A H -0.1245 -0.1012 0.1690 0.059 Uiso 0.50 1 calc PR C 3 H4B H -0.1950 -0.0344 0.1817 0.059 Uiso 0.50 1 calc PR C 3 H4AB H -0.1930 -0.0607 0.1917 0.059 Uiso 0.50 1 calc PR C 4 H4BB H -0.0954 -0.0935 0.1519 0.059 Uiso 0.50 1 calc PR C 4 C5 C -0.0346(3) -0.03453(15) 0.25851(18) 0.0314(6) Uani 1 1 d . C . H5 H -0.0628 -0.0175 0.3060 0.038 Uiso 1 1 calc R . . C6 C 0.0809(3) -0.04206(14) 0.27081(18) 0.0293(6) Uani 1 1 d . . . H6 H 0.1258 -0.0293 0.3258 0.035 Uiso 1 1 calc R C . C7 C 0.1418(4) -0.06875(17) 0.2043(2) 0.0487(9) Uani 1 1 d . C . H7A H 0.0950 -0.1055 0.1712 0.058 Uiso 0.50 1 calc PR D 3 H7B H 0.2134 -0.0899 0.2357 0.058 Uiso 0.50 1 calc PR D 3 H7AB H 0.2243 -0.0655 0.2283 0.058 Uiso 0.50 1 calc PR D 4 H7BB H 0.1229 -0.1177 0.1939 0.058 Uiso 0.50 1 calc PR D 4 C8A C 0.1697(6) -0.0183(3) 0.1400(4) 0.0352(13) Uiso 0.50 1 d P C 3 H8A1 H 0.1686 -0.0418 0.0843 0.042 Uiso 0.50 1 calc PR C 3 H8A2 H 0.2467 0.0002 0.1623 0.042 Uiso 0.50 1 calc PR C 3 C8B C 0.1139(6) -0.0321(3) 0.1198(4) 0.0347(13) Uiso 0.50 1 d P C 4 H8B1 H 0.0507 -0.0562 0.0809 0.042 Uiso 0.50 1 calc PR C 4 H8B2 H 0.1802 -0.0347 0.0929 0.042 Uiso 0.50 1 calc PR C 4 C9 C 0.0490(2) 0.08006(12) 0.37997(17) 0.0198(5) Uani 1 1 d . . . C10 C -0.0073(2) 0.09272(14) 0.50616(17) 0.0276(6) Uani 1 1 d . . . H10 H -0.0552 0.0972 0.5460 0.033 Uiso 1 1 calc R C . C11 C 0.1056(2) 0.09302(14) 0.52541(17) 0.0268(6) Uani 1 1 d . C . H11 H 0.1534 0.0982 0.5815 0.032 Uiso 1 1 calc R . . C15 C -0.1595(2) 0.08093(15) 0.3710(2) 0.0299(6) Uani 1 1 d . . . H15A H -0.1640 0.0803 0.3083 0.045 Uiso 1 1 calc R C . H15B H -0.2003 0.1208 0.3858 0.045 Uiso 1 1 calc R . . H15C H -0.1937 0.0392 0.3879 0.045 Uiso 1 1 calc R . . C16 C 0.2587(2) 0.08455(13) 0.44010(17) 0.0237(5) Uani 1 1 d . . . H16A H 0.2852 0.1324 0.4398 0.028 Uiso 1 1 calc R C . H16B H 0.2635 0.0635 0.3840 0.028 Uiso 1 1 calc R . . C17 C 0.3356(2) 0.04629(14) 0.51294(18) 0.0255(5) Uani 1 1 d . C . C18 C 0.3954(2) 0.08036(15) 0.58468(19) 0.0307(6) Uani 1 1 d . . . H18 H 0.3873 0.1285 0.5885 0.037 Uiso 1 1 calc R C . C19 C 0.4691(3) 0.04512(17) 0.6532(2) 0.0378(7) Uani 1 1 d . C . H19 H 0.5092 0.0696 0.7025 0.045 Uiso 1 1 calc R . . C20 C 0.4825(2) -0.02346(17) 0.6484(2) 0.0353(7) Uani 1 1 d . . . H20 H 0.5318 -0.0467 0.6946 0.042 Uiso 1 1 calc R C . C21 C 0.4238(2) -0.06061(14) 0.57569(19) 0.0274(6) Uani 1 1 d . C . C22 C 0.4370(2) -0.13184(16) 0.5660(2) 0.0332(6) Uani 1 1 d . . . H22 H 0.4858 -0.1572 0.6103 0.040 Uiso 1 1 calc R C . C23 C 0.3792(3) -0.16393(16) 0.4926(2) 0.0347(7) Uani 1 1 d . C . H23 H 0.3884 -0.2115 0.4844 0.042 Uiso 1 1 calc R . . C24 C 0.3060(3) -0.12483(15) 0.4298(2) 0.0324(6) Uani 1 1 d . . . H24 H 0.2649 -0.1478 0.3796 0.039 Uiso 1 1 calc R C . C25 C 0.3498(2) -0.02542(14) 0.50737(18) 0.0256(5) Uani 1 1 d . . . C12 C 0.0721(2) 0.16688(13) 0.22997(16) 0.0214(5) Uani 1 1 d . . . C13 C 0.1574(3) 0.26515(14) 0.20584(19) 0.0292(6) Uani 1 1 d . . . H13 H 0.2148 0.2963 0.1988 0.035 Uiso 1 1 calc R C . C14 C 0.0484(3) 0.27970(14) 0.20015(19) 0.0298(6) Uani 1 1 d . C . H14 H 0.0134 0.3231 0.1885 0.036 Uiso 1 1 calc R . . C26 C 0.2798(2) 0.16136(16) 0.23779(19) 0.0314(6) Uani 1 1 d . . . H26A H 0.3293 0.1783 0.2914 0.047 Uiso 1 1 calc R C . H26B H 0.3147 0.1703 0.1886 0.047 Uiso 1 1 calc R . . H26C H 0.2684 0.1121 0.2428 0.047 Uiso 1 1 calc R . . C27 C -0.1223(2) 0.21412(14) 0.21728(18) 0.0257(5) Uani 1 1 d . . . H27A H -0.1454 0.1655 0.2121 0.031 Uiso 1 1 calc R C . H27B H -0.1681 0.2388 0.1669 0.031 Uiso 1 1 calc R . . C28 C -0.1473(2) 0.24316(13) 0.29996(18) 0.0241(5) Uani 1 1 d . C . C29 C -0.0648(2) 0.25235(14) 0.37396(18) 0.0271(6) Uani 1 1 d . . . H29 H 0.0110 0.2399 0.3742 0.032 Uiso 1 1 calc R C . C30 C -0.0907(3) 0.27997(15) 0.44978(19) 0.0313(6) Uani 1 1 d . C . H30 H -0.0324 0.2855 0.5006 0.038 Uiso 1 1 calc R . . C31 C -0.1989(2) 0.29890(15) 0.45084(19) 0.0311(6) Uani 1 1 d . . . H31 H -0.2154 0.3178 0.5020 0.037 Uiso 1 1 calc R C . C32 C -0.2867(2) 0.29024(14) 0.37545(19) 0.0276(6) Uani 1 1 d . C . C33 C -0.4002(3) 0.30900(15) 0.3717(2) 0.0342(6) Uani 1 1 d . . . H33 H -0.4211 0.3291 0.4207 0.041 Uiso 1 1 calc R C . C34 C -0.4795(3) 0.29792(16) 0.2969(2) 0.0366(7) Uani 1 1 d . C . H34 H -0.5563 0.3100 0.2933 0.044 Uiso 1 1 calc R . . C35 C -0.4466(2) 0.26848(16) 0.2253(2) 0.0345(7) Uani 1 1 d . . . H35 H -0.5032 0.2608 0.1740 0.041 Uiso 1 1 calc R C . C36 C -0.2612(2) 0.26138(13) 0.29977(18) 0.0252(5) Uani 1 1 d . . . P1 P 0.31241(7) 0.20234(4) 0.98293(5) 0.03314(17) Uani 1 1 d D . . F1 F 0.33376(19) 0.14981(11) 0.91080(14) 0.0535(5) Uani 1 1 d D E . F2 F 0.29500(18) 0.25526(11) 1.05664(13) 0.0493(5) Uani 1 1 d D E . F3A F 0.3995(3) 0.25615(15) 0.9583(3) 0.0501(9) Uani 0.746(6) 1 d PD E 1 F4A F 0.2153(4) 0.15648(18) 1.0067(2) 0.0700(15) Uani 0.746(6) 1 d PD E 1 F5A F 0.4042(4) 0.1683(2) 1.0536(3) 0.0796(16) Uani 0.746(6) 1 d PD E 1 F6A F 0.2137(2) 0.2436(2) 0.91487(19) 0.0606(11) Uani 0.746(6) 1 d PD E 1 F3B F 0.3554(8) 0.2557(5) 0.9258(6) 0.037(2) Uiso 0.254(6) 1 d PD E 2 F4B F 0.2926(8) 0.1339(4) 1.0377(5) 0.039(2) Uiso 0.254(6) 1 d PD E 2 F5B F 0.4525(7) 0.1871(5) 1.0290(6) 0.039(2) Uiso 0.254(6) 1 d PD E 2 F6B F 0.1959(6) 0.2021(5) 0.9330(6) 0.043(2) Uiso 0.254(6) 1 d PD E 2 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 0.03007(6) 0.01574(5) 0.01527(5) 0.00145(3) 0.00669(4) 0.00027(4) N1 0.0304(12) 0.0210(10) 0.0215(11) 0.0038(8) 0.0089(9) 0.0033(9) N2 0.0309(12) 0.0169(10) 0.0180(10) 0.0019(8) 0.0083(9) 0.0016(8) N5 0.0305(12) 0.0250(12) 0.0312(13) 0.0015(9) 0.0080(10) -0.0008(9) N3 0.0265(11) 0.0212(10) 0.0219(11) 0.0057(9) 0.0074(9) 0.0005(9) N4 0.0282(11) 0.0179(10) 0.0253(11) 0.0024(8) 0.0066(9) 0.0002(9) N6 0.0271(12) 0.0281(12) 0.0319(13) 0.0056(10) 0.0028(10) -0.0013(10) C1 0.089(3) 0.0235(14) 0.0214(14) 0.0031(11) 0.0234(16) 0.0100(16) C2 0.075(3) 0.0371(17) 0.0180(14) 0.0018(12) 0.0022(15) -0.0193(17) C4 0.061(2) 0.0387(18) 0.0392(19) 0.0100(15) -0.0090(16) -0.0184(16) C5 0.0464(18) 0.0204(13) 0.0260(14) 0.0019(11) 0.0049(13) -0.0059(12) C6 0.0499(17) 0.0174(12) 0.0210(13) -0.0011(10) 0.0088(12) -0.0003(12) C7 0.083(3) 0.0310(17) 0.0396(19) 0.0072(14) 0.0306(19) 0.0185(17) C9 0.0261(13) 0.0121(11) 0.0222(12) 0.0024(9) 0.0078(10) 0.0011(9) C10 0.0390(15) 0.0273(13) 0.0193(13) 0.0024(10) 0.0126(11) 0.0047(12) C11 0.0382(15) 0.0242(13) 0.0191(13) 0.0002(10) 0.0087(11) 0.0012(12) C15 0.0290(14) 0.0308(15) 0.0316(15) 0.0082(12) 0.0103(12) 0.0024(11) C16 0.0294(13) 0.0195(12) 0.0237(13) 0.0029(10) 0.0090(11) -0.0011(10) C17 0.0261(13) 0.0273(13) 0.0245(13) 0.0027(11) 0.0085(11) -0.0016(11) C18 0.0312(15) 0.0284(14) 0.0318(15) -0.0004(11) 0.0057(12) -0.0003(11) C19 0.0348(16) 0.0394(17) 0.0350(17) -0.0031(14) -0.0010(13) 0.0020(13) C20 0.0284(15) 0.0412(17) 0.0337(16) 0.0043(13) 0.0017(12) 0.0049(13) C21 0.0208(12) 0.0289(14) 0.0336(15) 0.0052(11) 0.0088(11) 0.0004(11) C22 0.0261(14) 0.0329(15) 0.0419(17) 0.0076(13) 0.0104(13) 0.0040(12) C23 0.0333(15) 0.0250(14) 0.0483(19) 0.0037(13) 0.0145(14) 0.0012(12) C24 0.0343(15) 0.0244(14) 0.0394(17) -0.0003(12) 0.0101(13) -0.0025(12) C25 0.0227(13) 0.0277(14) 0.0286(14) 0.0037(11) 0.0102(11) -0.0014(10) C12 0.0272(13) 0.0219(12) 0.0156(11) 0.0012(9) 0.0060(10) 0.0013(10) C13 0.0346(15) 0.0216(13) 0.0320(15) 0.0051(11) 0.0089(12) -0.0032(11) C14 0.0396(16) 0.0174(12) 0.0328(15) 0.0070(11) 0.0088(12) -0.0001(11) C26 0.0263(14) 0.0379(16) 0.0323(15) 0.0117(12) 0.0114(12) 0.0049(12) C27 0.0238(13) 0.0253(13) 0.0259(13) 0.0026(10) 0.0008(10) 0.0031(10) C28 0.0271(13) 0.0170(12) 0.0279(14) 0.0044(10) 0.0054(11) -0.0010(10) C29 0.0266(14) 0.0220(13) 0.0316(14) 0.0014(11) 0.0044(11) -0.0015(11) C30 0.0347(15) 0.0305(15) 0.0269(14) 0.0024(11) 0.0030(12) -0.0064(12) C31 0.0380(16) 0.0292(14) 0.0282(14) 0.0016(12) 0.0118(12) -0.0055(12) C32 0.0292(14) 0.0224(13) 0.0330(15) 0.0064(11) 0.0103(11) -0.0028(11) C33 0.0360(16) 0.0320(15) 0.0396(17) 0.0076(13) 0.0192(13) -0.0009(13) C34 0.0266(14) 0.0377(16) 0.0474(18) 0.0103(14) 0.0126(13) -0.0001(13) C35 0.0263(14) 0.0352(16) 0.0398(17) 0.0099(13) 0.0028(12) -0.0010(12) C36 0.0281(14) 0.0189(12) 0.0290(14) 0.0056(10) 0.0068(11) -0.0021(10) P1 0.0359(4) 0.0373(4) 0.0249(4) 0.0005(3) 0.0037(3) -0.0168(3) F1 0.0629(13) 0.0519(13) 0.0492(12) -0.0163(10) 0.0201(10) -0.0238(10) F2 0.0657(14) 0.0473(12) 0.0389(11) -0.0073(9) 0.0199(10) -0.0174(10) F3A 0.0400(19) 0.0404(16) 0.079(3) -0.0142(16) 0.033(2) -0.0197(14) F4A 0.092(3) 0.065(2) 0.066(2) -0.0167(18) 0.044(2) -0.052(2) F5A 0.101(4) 0.061(2) 0.056(2) 0.0030(18) -0.027(2) 0.032(2) F6A 0.0428(17) 0.091(3) 0.0417(17) 0.0088(17) -0.0040(13) 0.0143(17) _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 C12 2.045(3) . ? Ir1 C9 2.048(3) . ? Ir1 C6 2.174(3) . ? Ir1 C2 2.180(3) . ? Ir1 C1 2.195(3) . ? Ir1 C5 2.196(3) . ? N1 C9 1.358(3) . ? N1 C10 1.383(3) . ? N1 C15 1.456(4) . ? N2 C9 1.360(3) . ? N2 C11 1.385(3) . ? N2 C16 1.476(3) . ? N5 C24 1.319(4) . ? N5 C25 1.367(4) . ? N3 C12 1.351(3) . ? N3 C13 1.383(3) . ? N3 C26 1.458(3) . ? N4 C12 1.361(3) . ? N4 C14 1.387(3) . ? N4 C27 1.450(3) . ? N6 C35 1.321(4) . ? N6 C36 1.369(4) . ? C1 C2 1.379(5) . ? C1 C8B 1.510(7) . ? C1 C8A 1.576(7) . ? C1 H1 0.9500 . ? C2 C3A 1.529(7) . ? C2 C3B 1.554(7) . ? C2 H2 0.9500 . ? C3A C4 1.470(7) . ? C3A H3A1 0.9900 . ? C3A H3A2 0.9900 . ? C3B C4 1.512(7) . ? C3B H3B1 0.9900 . ? C3B H3B2 0.9900 . ? C4 C5 1.503(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 H4AB 0.9900 . ? C4 H4BB 0.9900 . ? C5 C6 1.379(4) . ? C5 H5 0.9500 . ? C6 C7 1.505(4) . ? C6 H6 0.9500 . ? C7 C8B 1.487(7) . ? C7 C8A 1.507(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 H7AB 0.9900 . ? C7 H7BB 0.9900 . ? C8A H8A1 0.9900 . ? C8A H8A2 0.9900 . ? C8B H8B1 0.9900 . ? C8B H8B2 0.9900 . ? C10 C11 1.335(4) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.508(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.374(4) . ? C17 C25 1.420(4) . ? C18 C19 1.420(4) . ? C18 H18 0.9500 . ? C19 C20 1.356(5) . ? C19 H19 0.9500 . ? C20 C21 1.411(4) . ? C20 H20 0.9500 . ? C21 C22 1.416(4) . ? C21 C25 1.419(4) . ? C22 C23 1.366(5) . ? C22 H22 0.9500 . ? C23 C24 1.403(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C13 C14 1.335(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.515(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.371(4) . ? C28 C36 1.425(4) . ? C29 C30 1.411(4) . ? C29 H29 0.9500 . ? C30 C31 1.367(4) . ? C30 H30 0.9500 . ? C31 C32 1.420(4) . ? C31 H31 0.9500 . ? C32 C33 1.413(4) . ? C32 C36 1.417(4) . ? C33 C34 1.364(5) . ? C33 H33 0.9500 . ? C34 C35 1.405(5) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? P1 F6B 1.457(8) . ? P1 F5A 1.541(3) . ? P1 F3B 1.545(9) . ? P1 F4A 1.590(3) . ? P1 F1 1.598(2) . ? P1 F3A 1.599(3) . ? P1 F2 1.607(2) . ? P1 F6A 1.633(3) . ? P1 F4B 1.641(7) . ? P1 F5B 1.718(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 C12 Ir1 C9 93.39(9) . . ? C12 Ir1 C6 157.49(11) . . ? C9 Ir1 C6 91.34(10) . . ? C12 Ir1 C2 92.29(11) . . ? C9 Ir1 C2 157.50(14) . . ? C6 Ir1 C2 91.70(12) . . ? C12 Ir1 C1 89.00(11) . . ? C9 Ir1 C1 164.99(13) . . ? C6 Ir1 C1 81.07(11) . . ? C2 Ir1 C1 36.75(15) . . ? C12 Ir1 C5 165.11(11) . . ? C9 Ir1 C5 89.09(10) . . ? C6 Ir1 C5 36.78(11) . . ? C2 Ir1 C5 80.15(11) . . ? C1 Ir1 C5 92.39(12) . . ? C9 N1 C10 111.1(2) . . ? C9 N1 C15 125.4(2) . . ? C10 N1 C15 123.6(2) . . ? C9 N2 C11 110.9(2) . . ? C9 N2 C16 124.5(2) . . ? C11 N2 C16 124.4(2) . . ? C24 N5 C25 117.7(3) . . ? C12 N3 C13 111.3(2) . . ? C12 N3 C26 125.4(2) . . ? C13 N3 C26 123.3(2) . . ? C12 N4 C14 110.9(2) . . ? C12 N4 C27 125.4(2) . . ? C14 N4 C27 123.6(2) . . ? C35 N6 C36 117.3(3) . . ? C2 C1 C8B 111.0(4) . . ? C2 C1 C8A 136.9(4) . . ? C2 C1 Ir1 71.03(18) . . ? C8B C1 Ir1 111.1(3) . . ? C8A C1 Ir1 107.1(3) . . ? C2 C1 H1 111.6 . . ? C8B C1 H1 136.1 . . ? C8A C1 H1 111.6 . . ? Ir1 C1 H1 92.4 . . ? C1 C2 C3A 110.5(4) . . ? C1 C2 C3B 138.3(4) . . ? C1 C2 Ir1 72.21(18) . . ? C3A C2 Ir1 111.7(3) . . ? C3B C2 Ir1 109.3(3) . . ? C1 C2 H2 124.8 . . ? C3A C2 H2 124.8 . . ? C3B C2 H2 96.6 . . ? Ir1 C2 H2 86.8 . . ? C4 C3A C2 114.6(5) . . ? C4 C3A H3A1 108.6 . . ? C2 C3A H3A1 108.6 . . ? C4 C3A H3A2 108.6 . . ? C2 C3A H3A2 108.6 . . ? H3A1 C3A H3A2 107.6 . . ? C4 C3B C2 110.8(4) . . ? C4 C3B H3B1 109.5 . . ? C2 C3B H3B1 109.5 . . ? C4 C3B H3B2 109.5 . . ? C2 C3B H3B2 109.5 . . ? H3B1 C3B H3B2 108.1 . . ? C3A C4 C5 113.2(4) . . ? C5 C4 C3B 117.0(3) . . ? C3A C4 H4A 108.9 . . ? C5 C4 H4A 108.9 . . ? C3B C4 H4A 127.5 . . ? C3A C4 H4B 108.9 . . ? C5 C4 H4B 108.9 . . ? C3B C4 H4B 80.6 . . ? H4A C4 H4B 107.7 . . ? C3A C4 H4AB 131.8 . . ? C5 C4 H4AB 108.0 . . ? C3B C4 H4AB 108.0 . . ? H4A C4 H4AB 78.9 . . ? C3A C4 H4BB 82.7 . . ? C5 C4 H4BB 108.0 . . ? C3B C4 H4BB 108.0 . . ? H4B C4 H4BB 132.1 . . ? H4AB C4 H4BB 107.3 . . ? C6 C5 C4 125.4(3) . . ? C6 C5 Ir1 70.77(16) . . ? C4 C5 Ir1 111.21(19) . . ? C6 C5 H5 117.3 . . ? C4 C5 H5 117.3 . . ? Ir1 C5 H5 88.0 . . ? C5 C6 C7 125.4(3) . . ? C5 C6 Ir1 72.45(17) . . ? C7 C6 Ir1 110.86(19) . . ? C5 C6 H6 117.3 . . ? C7 C6 H6 117.3 . . ? Ir1 C6 H6 86.6 . . ? C8B C7 C6 114.2(4) . . ? C6 C7 C8A 117.4(3) . . ? C8B C7 H7A 83.6 . . ? C6 C7 H7A 107.9 . . ? C8A C7 H7A 107.9 . . ? C8B C7 H7B 130.6 . . ? C6 C7 H7B 107.9 . . ? C8A C7 H7B 107.9 . . ? H7A C7 H7B 107.2 . . ? C8B C7 H7AB 108.7 . . ? C6 C7 H7AB 108.7 . . ? C8A C7 H7AB 81.7 . . ? H7A C7 H7AB 131.4 . . ? C8B C7 H7BB 108.7 . . ? C6 C7 H7BB 108.7 . . ? C8A C7 H7BB 126.9 . . ? H7B C7 H7BB 79.7 . . ? H7AB C7 H7BB 107.6 . . ? C7 C8A C1 110.5(4) . . ? C7 C8A H8A1 109.5 . . ? C1 C8A H8A1 109.5 . . ? C7 C8A H8A2 109.5 . . ? C1 C8A H8A2 109.5 . . ? H8A1 C8A H8A2 108.1 . . ? C7 C8B C1 115.5(4) . . ? C7 C8B H8B1 108.4 . . ? C1 C8B H8B1 108.4 . . ? C7 C8B H8B2 108.4 . . ? C1 C8B H8B2 108.4 . . ? H8B1 C8B H8B2 107.5 . . ? N1 C9 N2 104.1(2) . . ? N1 C9 Ir1 125.88(19) . . ? N2 C9 Ir1 130.00(18) . . ? C11 C10 N1 107.0(2) . . ? C11 C10 H10 126.5 . . ? N1 C10 H10 126.5 . . ? C10 C11 N2 107.0(2) . . ? C10 C11 H11 126.5 . . ? N2 C11 H11 126.5 . . ? N1 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 C17 112.5(2) . . ? N2 C16 H16A 109.1 . . ? C17 C16 H16A 109.1 . . ? N2 C16 H16B 109.1 . . ? C17 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? C18 C17 C25 118.8(3) . . ? C18 C17 C16 120.7(3) . . ? C25 C17 C16 120.4(2) . . ? C17 C18 C19 121.3(3) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C20 C19 C18 120.1(3) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.7(3) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C20 C21 C22 123.2(3) . . ? C20 C21 C25 119.2(3) . . ? C22 C21 C25 117.6(3) . . ? C23 C22 C21 119.7(3) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 118.3(3) . . ? C22 C23 H23 120.9 . . ? C24 C23 H23 120.9 . . ? N5 C24 C23 124.6(3) . . ? N5 C24 H24 117.7 . . ? C23 C24 H24 117.7 . . ? N5 C25 C21 122.0(3) . . ? N5 C25 C17 118.1(2) . . ? C21 C25 C17 119.9(3) . . ? N3 C12 N4 104.1(2) . . ? N3 C12 Ir1 127.55(19) . . ? N4 C12 Ir1 128.22(19) . . ? C14 C13 N3 107.0(2) . . ? C14 C13 H13 126.5 . . ? N3 C13 H13 126.5 . . ? C13 C14 N4 106.7(2) . . ? C13 C14 H14 126.6 . . ? N4 C14 H14 126.6 . . ? N3 C26 H26A 109.5 . . ? N3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N4 C27 C28 113.0(2) . . ? N4 C27 H27A 109.0 . . ? C28 C27 H27A 109.0 . . ? N4 C27 H27B 109.0 . . ? C28 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C29 C28 C36 119.5(3) . . ? C29 C28 C27 122.4(2) . . ? C36 C28 C27 118.1(2) . . ? C28 C29 C30 121.1(3) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C31 C30 C29 120.6(3) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C30 C31 C32 120.0(3) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C33 C32 C36 117.5(3) . . ? C33 C32 C31 123.0(3) . . ? C36 C32 C31 119.4(3) . . ? C34 C33 C32 119.1(3) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C33 C34 C35 119.4(3) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? N6 C35 C34 123.9(3) . . ? N6 C35 H35 118.1 . . ? C34 C35 H35 118.1 . . ? N6 C36 C32 122.7(3) . . ? N6 C36 C28 117.8(2) . . ? C32 C36 C28 119.4(3) . . ? F6B P1 F5A 148.0(4) . . ? F6B P1 F3B 95.7(5) . . ? F5A P1 F3B 115.6(4) . . ? F6B P1 F4A 56.3(4) . . ? F5A P1 F4A 92.2(3) . . ? F3B P1 F4A 152.0(4) . . ? F6B P1 F1 84.5(3) . . ? F5A P1 F1 91.84(18) . . ? F3B P1 F1 83.7(4) . . ? F4A P1 F1 92.89(14) . . ? F6B P1 F3A 118.9(4) . . ? F5A P1 F3A 92.9(2) . . ? F4A P1 F3A 172.9(2) . . ? F1 P1 F3A 91.74(14) . . ? F6B P1 F2 97.3(3) . . ? F5A P1 F2 86.83(17) . . ? F3B P1 F2 95.9(4) . . ? F4A P1 F2 88.27(14) . . ? F1 P1 F2 178.26(12) . . ? F3A P1 F2 87.22(14) . . ? F5A P1 F6A 174.7(2) . . ? F3B P1 F6A 64.8(4) . . ? F4A P1 F6A 87.8(2) . . ? F1 P1 F6A 93.47(15) . . ? F3A P1 F6A 86.6(2) . . ? F2 P1 F6A 87.86(15) . . ? F6B P1 F4B 92.5(5) . . ? F5A P1 F4B 55.4(3) . . ? F3B P1 F4B 165.5(4) . . ? F1 P1 F4B 85.2(3) . . ? F3A P1 F4B 148.0(3) . . ? F2 P1 F4B 94.9(3) . . ? F6A P1 F4B 125.4(3) . . ? F6B P1 F5B 167.6(5) . . ? F3B P1 F5B 86.3(4) . . ? F4A P1 F5B 121.0(3) . . ? F1 P1 F5B 83.6(3) . . ? F3A P1 F5B 64.8(3) . . ? F2 P1 F5B 94.7(3) . . ? F6A P1 F5B 151.0(3) . . ? F4B P1 F5B 83.2(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 Ir1 C1 C2 -95.2(2) . . . . ? C9 Ir1 C1 C2 165.4(4) . . . . ? C6 Ir1 C1 C2 105.1(2) . . . . ? C5 Ir1 C1 C2 70.0(2) . . . . ? C12 Ir1 C1 C8B 158.9(4) . . . . ? C9 Ir1 C1 C8B 59.5(6) . . . . ? C6 Ir1 C1 C8B -0.8(4) . . . . ? C2 Ir1 C1 C8B -105.9(4) . . . . ? C5 Ir1 C1 C8B -35.9(4) . . . . ? C12 Ir1 C1 C8A 130.3(3) . . . . ? C9 Ir1 C1 C8A 30.9(6) . . . . ? C6 Ir1 C1 C8A -29.4(3) . . . . ? C2 Ir1 C1 C8A -134.5(4) . . . . ? C5 Ir1 C1 C8A -64.5(3) . . . . ? C8B C1 C2 C3A -1.1(5) . . . . ? C8A C1 C2 C3A -12.1(6) . . . . ? Ir1 C1 C2 C3A -107.1(3) . . . . ? C8B C1 C2 C3B 6.8(6) . . . . ? C8A C1 C2 C3B -4.2(8) . . . . ? Ir1 C1 C2 C3B -99.3(5) . . . . ? C8B C1 C2 Ir1 106.0(3) . . . . ? C8A C1 C2 Ir1 95.0(5) . . . . ? C12 Ir1 C2 C1 85.3(2) . . . . ? C9 Ir1 C2 C1 -170.2(2) . . . . ? C6 Ir1 C2 C1 -72.6(2) . . . . ? C5 Ir1 C2 C1 -107.7(2) . . . . ? C12 Ir1 C2 C3A -169.2(4) . . . . ? C9 Ir1 C2 C3A -64.6(5) . . . . ? C6 Ir1 C2 C3A 33.0(4) . . . . ? C1 Ir1 C2 C3A 105.6(5) . . . . ? C5 Ir1 C2 C3A -2.1(4) . . . . ? C12 Ir1 C2 C3B -138.8(3) . . . . ? C9 Ir1 C2 C3B -34.2(5) . . . . ? C6 Ir1 C2 C3B 63.4(4) . . . . ? C1 Ir1 C2 C3B 136.0(4) . . . . ? C5 Ir1 C2 C3B 28.3(3) . . . . ? C1 C2 C3A C4 98.3(6) . . . . ? C3B C2 C3A C4 -70.8(8) . . . . ? Ir1 C2 C3A C4 19.9(7) . . . . ? C1 C2 C3B C4 47.7(8) . . . . ? C3A C2 C3B C4 63.3(7) . . . . ? Ir1 C2 C3B C4 -36.9(6) . . . . ? C2 C3A C4 C5 -33.9(7) . . . . ? C2 C3A C4 C3B 70.3(8) . . . . ? C2 C3B C4 C3A -64.3(7) . . . . ? C2 C3B C4 C5 25.6(7) . . . . ? C3A C4 C5 C6 -50.1(5) . . . . ? C3B C4 C5 C6 -82.5(5) . . . . ? C3A C4 C5 Ir1 30.9(5) . . . . ? C3B C4 C5 Ir1 -1.5(5) . . . . ? C12 Ir1 C5 C6 166.7(3) . . . . ? C9 Ir1 C5 C6 -93.45(17) . . . . ? C2 Ir1 C5 C6 106.4(2) . . . . ? C1 Ir1 C5 C6 71.61(19) . . . . ? C12 Ir1 C5 C4 45.2(5) . . . . ? C9 Ir1 C5 C4 145.0(3) . . . . ? C6 Ir1 C5 C4 -121.5(3) . . . . ? C2 Ir1 C5 C4 -15.1(3) . . . . ? C1 Ir1 C5 C4 -49.9(3) . . . . ? C4 C5 C6 C7 -0.7(5) . . . . ? Ir1 C5 C6 C7 -103.5(3) . . . . ? C4 C5 C6 Ir1 102.8(3) . . . . ? C12 Ir1 C6 C5 -171.1(2) . . . . ? C9 Ir1 C6 C5 86.69(17) . . . . ? C2 Ir1 C6 C5 -71.01(19) . . . . ? C1 Ir1 C6 C5 -106.3(2) . . . . ? C12 Ir1 C6 C7 -49.1(4) . . . . ? C9 Ir1 C6 C7 -151.3(3) . . . . ? C2 Ir1 C6 C7 51.0(3) . . . . ? C1 Ir1 C6 C7 15.7(3) . . . . ? C5 Ir1 C6 C7 122.0(3) . . . . ? C5 C6 C7 C8B 54.1(5) . . . . ? Ir1 C6 C7 C8B -28.8(5) . . . . ? C5 C6 C7 C8A 85.3(5) . . . . ? Ir1 C6 C7 C8A 2.5(5) . . . . ? C8B C7 C8A C1 62.5(7) . . . . ? C6 C7 C8A C1 -28.0(7) . . . . ? C2 C1 C8A C7 -41.6(7) . . . . ? C8B C1 C8A C7 -64.4(7) . . . . ? Ir1 C1 C8A C7 38.6(5) . . . . ? C6 C7 C8B C1 29.4(7) . . . . ? C8A C7 C8B C1 -74.0(8) . . . . ? C2 C1 C8B C7 -91.9(5) . . . . ? C8A C1 C8B C7 71.6(8) . . . . ? Ir1 C1 C8B C7 -14.9(6) . . . . ? C10 N1 C9 N2 1.0(3) . . . . ? C15 N1 C9 N2 -178.4(2) . . . . ? C10 N1 C9 Ir1 178.81(18) . . . . ? C15 N1 C9 Ir1 -0.6(4) . . . . ? C11 N2 C9 N1 -1.5(3) . . . . ? C16 N2 C9 N1 -177.4(2) . . . . ? C11 N2 C9 Ir1 -179.12(18) . . . . ? C16 N2 C9 Ir1 5.0(3) . . . . ? C12 Ir1 C9 N1 101.2(2) . . . . ? C6 Ir1 C9 N1 -100.9(2) . . . . ? C2 Ir1 C9 N1 -3.2(4) . . . . ? C1 Ir1 C9 N1 -160.0(4) . . . . ? C5 Ir1 C9 N1 -64.1(2) . . . . ? C12 Ir1 C9 N2 -81.7(2) . . . . ? C6 Ir1 C9 N2 76.3(2) . . . . ? C2 Ir1 C9 N2 174.0(3) . . . . ? C1 Ir1 C9 N2 17.2(5) . . . . ? C5 Ir1 C9 N2 113.0(2) . . . . ? C9 N1 C10 C11 -0.2(3) . . . . ? C15 N1 C10 C11 179.2(2) . . . . ? N1 C10 C11 N2 -0.7(3) . . . . ? C9 N2 C11 C10 1.4(3) . . . . ? C16 N2 C11 C10 177.3(2) . . . . ? C9 N2 C16 C17 -143.3(2) . . . . ? C11 N2 C16 C17 41.3(3) . . . . ? N2 C16 C17 C18 -96.0(3) . . . . ? N2 C16 C17 C25 85.8(3) . . . . ? C25 C17 C18 C19 -1.0(4) . . . . ? C16 C17 C18 C19 -179.2(3) . . . . ? C17 C18 C19 C20 0.6(5) . . . . ? C18 C19 C20 C21 0.1(5) . . . . ? C19 C20 C21 C22 178.1(3) . . . . ? C19 C20 C21 C25 -0.4(4) . . . . ? C20 C21 C22 C23 -178.4(3) . . . . ? C25 C21 C22 C23 0.0(4) . . . . ? C21 C22 C23 C24 -1.5(4) . . . . ? C25 N5 C24 C23 0.2(4) . . . . ? C22 C23 C24 N5 1.4(5) . . . . ? C24 N5 C25 C21 -1.8(4) . . . . ? C24 N5 C25 C17 178.4(3) . . . . ? C20 C21 C25 N5 -179.8(3) . . . . ? C22 C21 C25 N5 1.7(4) . . . . ? C20 C21 C25 C17 0.0(4) . . . . ? C22 C21 C25 C17 -178.5(2) . . . . ? C18 C17 C25 N5 -179.5(2) . . . . ? C16 C17 C25 N5 -1.3(4) . . . . ? C18 C17 C25 C21 0.7(4) . . . . ? C16 C17 C25 C21 178.9(2) . . . . ? C13 N3 C12 N4 0.6(3) . . . . ? C26 N3 C12 N4 178.1(2) . . . . ? C13 N3 C12 Ir1 177.25(19) . . . . ? C26 N3 C12 Ir1 -5.2(4) . . . . ? C14 N4 C12 N3 -0.7(3) . . . . ? C27 N4 C12 N3 -177.3(2) . . . . ? C14 N4 C12 Ir1 -177.36(19) . . . . ? C27 N4 C12 Ir1 6.0(4) . . . . ? C9 Ir1 C12 N3 100.3(2) . . . . ? C6 Ir1 C12 N3 -1.5(4) . . . . ? C2 Ir1 C12 N3 -101.5(2) . . . . ? C1 Ir1 C12 N3 -64.9(2) . . . . ? C5 Ir1 C12 N3 -160.5(3) . . . . ? C9 Ir1 C12 N4 -83.8(2) . . . . ? C6 Ir1 C12 N4 174.4(2) . . . . ? C2 Ir1 C12 N4 74.4(2) . . . . ? C1 Ir1 C12 N4 111.0(2) . . . . ? C5 Ir1 C12 N4 15.4(5) . . . . ? C12 N3 C13 C14 -0.2(3) . . . . ? C26 N3 C13 C14 -177.8(3) . . . . ? N3 C13 C14 N4 -0.2(3) . . . . ? C12 N4 C14 C13 0.6(3) . . . . ? C27 N4 C14 C13 177.3(2) . . . . ? C12 N4 C27 C28 102.1(3) . . . . ? C14 N4 C27 C28 -74.1(3) . . . . ? N4 C27 C28 C29 -19.6(4) . . . . ? N4 C27 C28 C36 160.3(2) . . . . ? C36 C28 C29 C30 -0.4(4) . . . . ? C27 C28 C29 C30 179.6(2) . . . . ? C28 C29 C30 C31 -0.7(4) . . . . ? C29 C30 C31 C32 0.6(4) . . . . ? C30 C31 C32 C33 -179.6(3) . . . . ? C30 C31 C32 C36 0.5(4) . . . . ? C36 C32 C33 C34 0.8(4) . . . . ? C31 C32 C33 C34 -179.0(3) . . . . ? C32 C33 C34 C35 -0.3(4) . . . . ? C36 N6 C35 C34 0.8(4) . . . . ? C33 C34 C35 N6 -0.5(5) . . . . ? C35 N6 C36 C32 -0.2(4) . . . . ? C35 N6 C36 C28 -179.4(2) . . . . ? C33 C32 C36 N6 -0.6(4) . . . . ? C31 C32 C36 N6 179.3(2) . . . . ? C33 C32 C36 C28 178.6(2) . . . . ? C31 C32 C36 C28 -1.6(4) . . . . ? C29 C28 C36 N6 -179.3(2) . . . . ? C27 C28 C36 N6 0.7(4) . . . . ? C29 C28 C36 C32 1.5(4) . . . . ? C27 C28 C36 C32 -178.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.426 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.088 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.500 0.500 195 46 ' ' 2 0.500 1.000 1.000 195 46 ' ' _platon_squeeze_details ; The unit cell contains 2 diethyl ether molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON ;