#------------------------------------------------------------------------------ #$Date: 2017-05-20 04:58:28 +0300 (Sat, 20 May 2017) $ #$Revision: 196815 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/30/7043057.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7043057 loop_ _publ_author_name 'Carmona, Daniel' 'Carmona, Mar\'ia' 'Rodr\'iguez, Ricardo' 'M\'endez, Isabel' 'Passarelli, Vincenzo' 'Lahoz, Fernando J.' 'Garc\'ia-Ordu\~na, Pilar' _publ_section_title ; Stereospecific control of the metal-centred chirality of rhodium(III) and iridium(III) complexes bearing tetradentate CNN’P ligands ; _journal_name_full 'Dalton Trans.' _journal_paper_doi 10.1039/C7DT01446E _journal_year 2017 _chemical_formula_moiety 'C32 H28 Cl2 Ir N2 P, C H2 Cl2' _chemical_formula_sum 'C33 H30 Cl4 Ir N2 P' _chemical_formula_weight 819.56 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014 _audit_update_record ; 2017-04-21 deposited with the CCDC. 2017-05-19 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 100.9780(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 16.3535(7) _cell_length_b 9.8273(4) _cell_length_c 19.2962(9) _cell_measurement_reflns_used 9891 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.482 _cell_measurement_theta_min 2.334 _cell_volume 3044.4(2) _computing_cell_refinement 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_data_collection 'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_data_reduction 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material 'XCIF program, PLATON(Spek, 1998)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 8.26 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.935 _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method 'narrow \w frames' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_unetI/netI 0.0241 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.935 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 34385 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.935 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.642 _diffrn_reflns_theta_min 2.150 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 4.817 _exptl_absorpt_correction_T_max 0.5619 _exptl_absorpt_correction_T_min 0.4086 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within APEX2 package. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.788 _exptl_crystal_description plate _exptl_crystal_F_000 1608 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Dichloromethane' _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.060 _refine_diff_density_max 1.858 _refine_diff_density_min -1.591 _refine_diff_density_rms 0.122 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 480 _refine_ls_number_reflns 7324 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.057 _refine_ls_R_factor_all 0.0330 _refine_ls_R_factor_gt 0.0287 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+11.8796P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.0631 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6693 _reflns_number_total 7324 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt01446e2.cif _cod_data_source_block cmpnd_8 _cod_database_code 7043057 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelxl_version_number 2014-3 _shelx_res_file ; TITL fjl319as in P2(1)/c CELL 0.71073 16.3535 9.8273 19.2962 90.000 100.978 90.000 ZERR 4.00 0.0007 0.0004 0.0009 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H CL IR N P UNIT 132 120 16 4 8 4 MERG 2 OMIT 1 0 0 FMAP 2 PLAN 15 ACTA BOND $H L.S. 4 TEMP -173.00 WGHT 0.019500 11.879600 FVAR 0.17949 0.62607 IR 4 0.327980 0.696769 0.308083 11.00000 0.01540 0.01269 = 0.01621 -0.00003 0.00311 0.00083 CL1 3 0.231521 0.807549 0.366543 11.00000 0.02282 0.02105 = 0.02312 -0.00216 0.00778 0.00386 CL2 3 0.394963 0.918841 0.292754 11.00000 0.02142 0.01564 = 0.02850 0.00037 0.00487 -0.00164 P 6 0.238480 0.704829 0.203439 11.00000 0.01611 0.01481 = 0.01708 0.00040 0.00273 0.00068 N1 5 0.420620 0.594561 0.267304 11.00000 0.01636 0.01426 = 0.01911 0.00060 0.00464 0.00245 N2 5 0.419333 0.683114 0.401136 11.00000 0.01812 0.01752 = 0.01679 0.00175 0.00044 0.00104 C1 1 0.225520 0.873473 0.162569 11.00000 0.01983 0.01727 = 0.02383 0.00459 0.00227 0.00177 C2 1 0.232434 0.895687 0.092403 11.00000 0.02708 0.02564 = 0.02323 0.00338 0.00120 0.00199 C3 1 0.222444 1.025299 0.063554 11.00000 0.03325 0.03636 = 0.02708 0.01411 0.00232 -0.00223 C4 1 0.205527 1.133934 0.103891 11.00000 0.03453 0.02152 = 0.03975 0.01163 -0.00422 -0.00009 C5 1 0.199347 1.113571 0.173421 11.00000 0.03602 0.01670 = 0.04036 0.00076 -0.00398 0.00572 C6 1 0.209983 0.984453 0.203239 11.00000 0.02724 0.02218 = 0.02770 0.00255 0.00074 0.00391 C7 1 0.133101 0.643321 0.200734 11.00000 0.01413 0.02694 = 0.02187 -0.00078 0.00253 -0.00210 C8 1 0.119991 0.502799 0.205614 11.00000 0.02796 0.03006 = 0.02784 0.00437 0.00173 -0.00774 C9 1 0.040477 0.451118 0.199342 11.00000 0.03731 0.04710 = 0.03579 0.00205 0.00501 -0.01916 C10 1 -0.026884 0.537987 0.189837 11.00000 0.02326 0.07000 = 0.03791 -0.00713 0.00682 -0.01813 C11 1 -0.015265 0.675430 0.187070 11.00000 0.01794 0.06420 = 0.04575 -0.00920 0.00288 0.00577 C12 1 0.064650 0.729294 0.191805 11.00000 0.02415 0.03332 = 0.03631 -0.00620 0.00241 0.00328 C13 1 0.272678 0.602158 0.135436 11.00000 0.02515 0.01607 = 0.01728 0.00113 0.00409 0.00140 C14 1 0.214405 0.553240 0.078041 11.00000 0.02175 0.02343 = 0.02301 -0.00101 0.00297 -0.00009 C15 1 0.239609 0.483821 0.022964 11.00000 0.03629 0.02156 = 0.01889 -0.00258 0.00009 -0.00147 C16 1 0.323248 0.459687 0.024899 11.00000 0.03720 0.02645 = 0.02061 -0.00417 0.00551 0.00373 C17 1 0.381890 0.505516 0.081867 11.00000 0.02605 0.02233 = 0.02360 -0.00012 0.00693 0.00673 C18 1 0.357778 0.579280 0.136560 11.00000 0.02339 0.01867 = 0.01620 0.00054 0.00440 -0.00018 C19 1 0.425392 0.636110 0.193162 11.00000 0.01971 0.01910 = 0.01823 0.00056 0.00834 0.00021 C20 1 0.501549 0.637526 0.312733 11.00000 0.01588 0.02386 = 0.02097 -0.00001 0.00347 -0.00043 C21 1 0.494836 0.647365 0.388482 11.00000 0.02017 0.01535 = 0.02305 0.00088 0.00011 -0.00339 C22 1 0.563212 0.633221 0.442997 11.00000 0.02116 0.02077 = 0.03034 0.00118 0.00068 0.00092 C23 1 0.553499 0.657011 0.511578 11.00000 0.02966 0.02505 = 0.02248 0.00027 -0.00492 -0.00481 C24 1 0.476082 0.694538 0.523718 11.00000 0.03711 0.02502 = 0.02082 -0.00116 0.00057 0.00213 C25 1 0.409907 0.705631 0.467394 11.00000 0.02876 0.01977 = 0.02248 0.00062 0.00649 0.00231 C26 1 0.410544 0.440911 0.271457 11.00000 0.01922 0.01508 = 0.02598 0.00098 0.00144 0.00187 C27 1 0.341161 0.402760 0.308188 11.00000 0.02091 0.01852 = 0.01187 0.00014 -0.00124 -0.00145 C28 1 0.292407 0.506428 0.329041 11.00000 0.01955 0.01696 = 0.01554 0.00011 0.00200 -0.00159 C29 1 0.230568 0.469195 0.366596 11.00000 0.02309 0.02222 = 0.02165 0.00109 0.00564 -0.00028 C30 1 0.217294 0.332372 0.380897 11.00000 0.02654 0.02687 = 0.01823 0.00134 0.00411 -0.01023 C31 1 0.263423 0.230591 0.356887 11.00000 0.03377 0.01797 = 0.02272 0.00198 0.00137 -0.00840 C32 1 0.325816 0.265481 0.320485 11.00000 0.02541 0.01475 = 0.02039 -0.00179 -0.00195 0.00002 PART 1 C51A 1 0.060725 0.694894 0.460644 21.00000 0.05824 AFIX 23 H51A 2 0.109105 0.742562 0.447893 21.00000 -1.20000 H51B 2 0.081679 0.637023 0.502231 21.00000 -1.20000 AFIX 0 CL3A 3 0.016285 0.591803 0.391093 21.00000 0.06572 CL4A 3 -0.007557 0.815753 0.483863 21.00000 0.05242 PART 2 CL3B 3 0.021763 0.525845 0.421305 -21.00000 0.07030 CL4B 3 0.002549 0.761777 0.499916 -21.00000 0.10735 C51B 1 0.041738 0.703606 0.426148 -21.00000 0.15595 AFIX 23 H51C 2 0.013150 0.749605 0.382576 -21.00000 -1.20000 H51D 2 0.102261 0.721637 0.432407 -21.00000 -1.20000 AFIX 0 PART 0 H2 2 0.241636 0.826289 0.066030 11.00000 0.03080 H3 2 0.226103 1.035082 0.017623 11.00000 0.03064 H4 2 0.201527 1.218331 0.084174 11.00000 0.02951 H5 2 0.188503 1.187743 0.200327 11.00000 0.04332 H6 2 0.208526 0.973693 0.251397 11.00000 0.02904 H8 2 0.164104 0.443398 0.211175 11.00000 0.03345 H9 2 0.029934 0.352019 0.201212 11.00000 0.05466 H10 2 -0.078457 0.504209 0.184163 11.00000 0.05006 H11 2 -0.056786 0.738223 0.181187 11.00000 0.04827 H12 2 0.071962 0.818897 0.189273 11.00000 0.01497 H14 2 0.158204 0.568669 0.077996 11.00000 0.01197 H15 2 0.198881 0.457740 -0.015011 11.00000 0.02807 H16 2 0.341366 0.419325 -0.010947 11.00000 0.01219 H17 2 0.441424 0.487692 0.083077 11.00000 0.02776 H19A 2 0.423841 0.732448 0.193159 11.00000 0.01288 H19B 2 0.478687 0.608884 0.184723 11.00000 0.00920 H20A 2 0.543374 0.577567 0.304247 11.00000 0.02358 H20B 2 0.513740 0.727176 0.296855 11.00000 0.01271 H22 2 0.613125 0.608231 0.430146 11.00000 0.02659 H23 2 0.599434 0.648091 0.551105 11.00000 0.02589 H24 2 0.467465 0.712140 0.570687 11.00000 0.02447 H25 2 0.355440 0.729109 0.472385 11.00000 0.02085 H26A 2 0.397772 0.403177 0.222018 11.00000 0.02564 H26B 2 0.464795 0.406574 0.294121 11.00000 0.00943 H29 2 0.195947 0.534448 0.380303 11.00000 0.03058 H30 2 0.177539 0.310028 0.404600 11.00000 0.02420 H31 2 0.252738 0.140445 0.364157 11.00000 0.02482 H32 2 0.358343 0.196710 0.303553 11.00000 0.02555 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 REM fjl319as in P2(1)/c REM R1 = 0.0287 for 6693 Fo > 4sig(Fo) and 0.0330 for all 7324 data REM 480 parameters refined using 0 restraints END WGHT 0.0164 12.5152 REM Highest difference peak 1.858, deepest hole -1.591, 1-sigma level 0.122 Q1 1 0.0106 0.5648 0.4093 11.00000 0.05 1.86 Q2 1 0.0221 0.6185 0.3693 11.00000 0.05 1.60 Q3 1 0.0163 0.8022 0.5756 11.00000 0.05 1.21 Q4 1 0.3294 0.9093 0.3085 11.00000 0.05 1.10 Q5 1 0.0313 0.4779 0.4329 11.00000 0.05 1.02 Q6 1 0.3230 0.6979 0.2573 11.00000 0.05 0.93 Q7 1 -0.0278 0.7998 0.4942 11.00000 0.05 0.91 Q8 1 0.0188 0.7979 0.4692 11.00000 0.05 0.88 Q9 1 0.2738 0.6876 0.3094 11.00000 0.05 0.83 Q10 1 0.3925 0.6846 0.3019 11.00000 0.05 0.83 Q11 1 0.3325 0.6959 0.3610 11.00000 0.05 0.75 Q12 1 0.0178 0.8504 0.4706 11.00000 0.05 0.70 Q13 1 0.0152 0.6911 0.4080 11.00000 0.05 0.63 Q14 1 0.0143 0.7315 0.5208 11.00000 0.05 0.59 Q15 1 0.0011 0.6238 0.4835 11.00000 0.05 0.52 ; _shelx_res_checksum 45573 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ir Ir 0.32798(2) 0.69677(2) 0.30808(2) 0.01475(4) Uani 1 1 d . . . . . Cl1 Cl 0.23152(5) 0.80755(9) 0.36654(5) 0.02188(17) Uani 1 1 d . . . . . Cl2 Cl 0.39496(5) 0.91884(9) 0.29275(5) 0.02184(17) Uani 1 1 d . . . . . P P 0.23848(5) 0.70483(9) 0.20344(5) 0.01606(17) Uani 1 1 d . . . . . N1 N 0.42062(17) 0.5946(3) 0.26730(15) 0.0164(6) Uani 1 1 d . . . . . N2 N 0.41933(18) 0.6831(3) 0.40114(15) 0.0179(6) Uani 1 1 d . . . . . C1 C 0.2255(2) 0.8735(4) 0.16257(19) 0.0206(7) Uani 1 1 d . . . . . C2 C 0.2324(2) 0.8957(4) 0.0924(2) 0.0258(8) Uani 1 1 d . . . . . C3 C 0.2224(3) 1.0253(5) 0.0636(2) 0.0327(9) Uani 1 1 d . . . . . C4 C 0.2055(3) 1.1339(4) 0.1039(2) 0.0334(10) Uani 1 1 d . . . . . C5 C 0.1993(3) 1.1136(4) 0.1734(2) 0.0325(9) Uani 1 1 d . . . . . C6 C 0.2100(3) 0.9845(4) 0.2032(2) 0.0263(8) Uani 1 1 d . . . . . C7 C 0.1331(2) 0.6433(4) 0.20073(19) 0.0211(7) Uani 1 1 d . . . . . C8 C 0.1200(3) 0.5028(4) 0.2056(2) 0.0291(9) Uani 1 1 d . . . . . C9 C 0.0405(3) 0.4511(6) 0.1993(3) 0.0403(11) Uani 1 1 d . . . . . C10 C -0.0269(3) 0.5380(6) 0.1898(3) 0.0436(12) Uani 1 1 d . . . . . C11 C -0.0153(3) 0.6754(6) 0.1871(3) 0.0430(12) Uani 1 1 d . . . . . C12 C 0.0647(3) 0.7293(5) 0.1918(2) 0.0317(9) Uani 1 1 d . . . . . C13 C 0.2727(2) 0.6022(4) 0.13544(18) 0.0195(7) Uani 1 1 d . . . . . C14 C 0.2144(2) 0.5532(4) 0.0780(2) 0.0229(7) Uani 1 1 d . . . . . C15 C 0.2396(3) 0.4838(4) 0.0230(2) 0.0263(8) Uani 1 1 d . . . . . C16 C 0.3232(3) 0.4597(4) 0.0249(2) 0.0281(8) Uani 1 1 d . . . . . C17 C 0.3819(2) 0.5055(4) 0.0819(2) 0.0237(8) Uani 1 1 d . . . . . C18 C 0.3578(2) 0.5793(4) 0.13656(18) 0.0193(7) Uani 1 1 d . . . . . C19 C 0.4254(2) 0.6361(4) 0.19316(19) 0.0184(7) Uani 1 1 d . . . . . C20 C 0.5015(2) 0.6375(4) 0.31273(19) 0.0202(7) Uani 1 1 d . . . . . C21 C 0.4948(2) 0.6474(4) 0.38848(19) 0.0200(7) Uani 1 1 d . . . . . C22 C 0.5632(2) 0.6332(4) 0.4430(2) 0.0246(8) Uani 1 1 d . . . . . C23 C 0.5535(3) 0.6570(4) 0.5116(2) 0.0270(8) Uani 1 1 d . . . . . C24 C 0.4761(3) 0.6945(4) 0.5237(2) 0.0283(8) Uani 1 1 d . . . . . C25 C 0.4099(3) 0.7056(4) 0.4674(2) 0.0235(7) Uani 1 1 d . . . . . C26 C 0.4105(2) 0.4409(4) 0.2715(2) 0.0205(7) Uani 1 1 d . . . . . C27 C 0.3412(2) 0.4028(4) 0.30819(17) 0.0177(7) Uani 1 1 d . . . . . C28 C 0.2924(2) 0.5064(4) 0.32904(18) 0.0175(7) Uani 1 1 d . . . . . C29 C 0.2306(2) 0.4692(4) 0.3666(2) 0.0221(7) Uani 1 1 d . . . . . C30 C 0.2173(2) 0.3324(4) 0.3809(2) 0.0239(8) Uani 1 1 d . . . . . C31 C 0.2634(3) 0.2306(4) 0.3569(2) 0.0253(8) Uani 1 1 d . . . . . C32 C 0.3258(2) 0.2655(4) 0.32048(19) 0.0210(7) Uani 1 1 d . . . . . C51A C 0.0607(7) 0.6949(11) 0.4606(6) 0.058(3) Uiso 0.626(6) 1 d . . P A 1 H51A H 0.1091 0.7426 0.4479 0.070 Uiso 0.626(6) 1 calc R U P A 1 H51B H 0.0817 0.6370 0.5022 0.070 Uiso 0.626(6) 1 calc R U P A 1 Cl3A Cl 0.01629(17) 0.5918(3) 0.39109(17) 0.0657(10) Uiso 0.626(6) 1 d . . P A 1 Cl4A Cl -0.00756(16) 0.8158(3) 0.48386(14) 0.0524(7) Uiso 0.626(6) 1 d . . P A 1 Cl3B Cl 0.0218(3) 0.5258(6) 0.4213(3) 0.0703(17) Uiso 0.374(6) 1 d . . P A 2 Cl4B Cl 0.0025(5) 0.7618(10) 0.4999(5) 0.107(2) Uiso 0.374(6) 1 d . . P A 2 C51B C 0.042(3) 0.704(4) 0.426(2) 0.156(15) Uiso 0.374(6) 1 d . . P A 2 H51C H 0.0132 0.7496 0.3826 0.187 Uiso 0.374(6) 1 calc R U P A 2 H51D H 0.1023 0.7216 0.4324 0.187 Uiso 0.374(6) 1 calc R U P A 2 H2 H 0.242(3) 0.826(5) 0.066(2) 0.031(12) Uiso 1 1 d . . . . . H3 H 0.226(3) 1.035(5) 0.018(3) 0.031(12) Uiso 1 1 d . . . . . H4 H 0.202(3) 1.218(5) 0.084(2) 0.030(12) Uiso 1 1 d . . . . . H5 H 0.189(3) 1.188(5) 0.200(3) 0.043(15) Uiso 1 1 d . . . . . H6 H 0.209(3) 0.974(5) 0.251(2) 0.029(12) Uiso 1 1 d . . . . . H8 H 0.164(3) 0.443(5) 0.211(2) 0.033(13) Uiso 1 1 d . . . . . H9 H 0.030(3) 0.352(6) 0.201(3) 0.055(16) Uiso 1 1 d . . . . . H10 H -0.078(3) 0.504(6) 0.184(3) 0.050(16) Uiso 1 1 d . . . . . H11 H -0.057(3) 0.738(6) 0.181(3) 0.048(15) Uiso 1 1 d . . . . . H12 H 0.072(2) 0.819(4) 0.189(2) 0.015(10) Uiso 1 1 d . . . . . H14 H 0.158(2) 0.569(4) 0.078(2) 0.012(9) Uiso 1 1 d . . . . . H15 H 0.199(3) 0.458(5) -0.015(2) 0.028(12) Uiso 1 1 d . . . . . H16 H 0.341(2) 0.419(4) -0.011(2) 0.012(9) Uiso 1 1 d . . . . . H17 H 0.441(3) 0.488(5) 0.083(2) 0.028(12) Uiso 1 1 d . . . . . H19A H 0.424(2) 0.732(4) 0.193(2) 0.013(9) Uiso 1 1 d . . . . . H19B H 0.479(2) 0.609(4) 0.1847(19) 0.009(9) Uiso 1 1 d . . . . . H20A H 0.543(3) 0.578(4) 0.304(2) 0.024(11) Uiso 1 1 d . . . . . H20B H 0.514(2) 0.727(4) 0.297(2) 0.013(9) Uiso 1 1 d . . . . . H22 H 0.613(3) 0.608(5) 0.430(2) 0.027(11) Uiso 1 1 d . . . . . H23 H 0.599(3) 0.648(5) 0.551(2) 0.026(11) Uiso 1 1 d . . . . . H24 H 0.467(3) 0.712(4) 0.571(2) 0.024(11) Uiso 1 1 d . . . . . H25 H 0.355(3) 0.729(4) 0.472(2) 0.021(11) Uiso 1 1 d . . . . . H26A H 0.398(3) 0.403(4) 0.222(2) 0.026(11) Uiso 1 1 d . . . . . H26B H 0.465(2) 0.407(4) 0.2941(19) 0.009(9) Uiso 1 1 d . . . . . H29 H 0.196(3) 0.534(5) 0.380(2) 0.031(12) Uiso 1 1 d . . . . . H30 H 0.178(3) 0.310(4) 0.405(2) 0.024(11) Uiso 1 1 d . . . . . H31 H 0.253(3) 0.140(5) 0.364(2) 0.025(11) Uiso 1 1 d . . . . . H32 H 0.358(3) 0.197(4) 0.304(2) 0.026(11) Uiso 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 Ir 0.01540(7) 0.01269(7) 0.01621(7) -0.00003(5) 0.00311(5) 0.00083(5) Cl1 0.0228(4) 0.0211(4) 0.0231(4) -0.0022(3) 0.0078(3) 0.0039(3) Cl2 0.0214(4) 0.0156(4) 0.0285(4) 0.0004(3) 0.0049(3) -0.0016(3) P 0.0161(4) 0.0148(4) 0.0171(4) 0.0004(3) 0.0027(3) 0.0007(3) N1 0.0164(14) 0.0143(13) 0.0191(14) 0.0006(11) 0.0046(11) 0.0025(11) N2 0.0181(14) 0.0175(14) 0.0168(14) 0.0017(11) 0.0004(11) 0.0010(11) C1 0.0198(17) 0.0173(17) 0.0238(18) 0.0046(14) 0.0023(14) 0.0018(13) C2 0.027(2) 0.026(2) 0.0232(19) 0.0034(16) 0.0012(15) 0.0020(16) C3 0.033(2) 0.036(2) 0.027(2) 0.0141(18) 0.0023(17) -0.0022(18) C4 0.035(2) 0.022(2) 0.040(2) 0.0116(18) -0.0042(18) -0.0001(17) C5 0.036(2) 0.0167(19) 0.040(2) 0.0008(17) -0.0040(19) 0.0057(16) C6 0.027(2) 0.0222(19) 0.028(2) 0.0025(16) 0.0007(16) 0.0039(15) C7 0.0141(16) 0.0269(19) 0.0219(18) -0.0008(14) 0.0025(13) -0.0021(14) C8 0.028(2) 0.030(2) 0.028(2) 0.0044(17) 0.0017(16) -0.0077(17) C9 0.037(3) 0.047(3) 0.036(2) 0.002(2) 0.005(2) -0.019(2) C10 0.023(2) 0.070(4) 0.038(3) -0.007(2) 0.0068(19) -0.018(2) C11 0.018(2) 0.064(3) 0.046(3) -0.009(2) 0.0029(19) 0.006(2) C12 0.024(2) 0.033(2) 0.036(2) -0.0062(18) 0.0024(17) 0.0033(17) C13 0.0251(18) 0.0161(16) 0.0173(16) 0.0011(13) 0.0041(14) 0.0014(14) C14 0.0217(18) 0.0234(18) 0.0230(18) -0.0010(14) 0.0030(14) -0.0001(14) C15 0.036(2) 0.0216(18) 0.0189(18) -0.0026(14) 0.0001(16) -0.0015(16) C16 0.037(2) 0.026(2) 0.0206(19) -0.0042(15) 0.0055(16) 0.0037(17) C17 0.0260(19) 0.0223(18) 0.0236(19) -0.0001(15) 0.0069(15) 0.0067(15) C18 0.0234(18) 0.0187(17) 0.0162(16) 0.0005(13) 0.0044(13) -0.0002(14) C19 0.0197(17) 0.0191(17) 0.0182(17) 0.0006(13) 0.0083(13) 0.0002(14) C20 0.0159(16) 0.0239(18) 0.0210(18) 0.0000(14) 0.0035(13) -0.0004(14) C21 0.0202(17) 0.0153(16) 0.0230(18) 0.0009(13) 0.0001(14) -0.0034(13) C22 0.0212(18) 0.0208(18) 0.030(2) 0.0012(15) 0.0007(15) 0.0009(14) C23 0.030(2) 0.0251(19) 0.0225(19) 0.0003(15) -0.0049(16) -0.0048(16) C24 0.037(2) 0.025(2) 0.0208(19) -0.0012(15) 0.0006(16) 0.0021(17) C25 0.029(2) 0.0198(18) 0.0225(18) 0.0006(14) 0.0065(15) 0.0023(15) C26 0.0192(17) 0.0151(16) 0.0260(19) 0.0010(14) 0.0014(14) 0.0019(13) C27 0.0209(17) 0.0185(16) 0.0119(15) 0.0001(13) -0.0012(12) -0.0015(13) C28 0.0195(16) 0.0170(16) 0.0155(16) 0.0001(13) 0.0020(13) -0.0016(13) C29 0.0231(18) 0.0222(18) 0.0216(18) 0.0011(14) 0.0056(14) -0.0003(15) C30 0.0265(19) 0.027(2) 0.0182(18) 0.0013(14) 0.0041(15) -0.0102(15) C31 0.034(2) 0.0180(18) 0.0227(19) 0.0020(14) 0.0014(16) -0.0084(15) C32 0.0254(18) 0.0148(16) 0.0204(18) -0.0018(13) -0.0020(14) 0.0000(14) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C28 Ir N1 83.55(13) C28 Ir N2 87.42(12) N1 Ir N2 80.99(11) C28 Ir P 92.81(10) N1 Ir P 94.19(8) N2 Ir P 175.12(8) C28 Ir Cl1 94.98(10) N1 Ir Cl1 173.83(8) N2 Ir Cl1 92.96(8) P Ir Cl1 91.87(3) C28 Ir Cl2 170.49(10) N1 Ir Cl2 90.55(8) N2 Ir Cl2 84.28(8) P Ir Cl2 95.05(3) Cl1 Ir Cl2 90.10(3) C7 P C13 102.37(17) C7 P C1 104.92(17) C13 P C1 102.53(17) C7 P Ir 117.61(12) C13 P Ir 112.84(12) C1 P Ir 114.78(12) C20 N1 C19 106.2(3) C20 N1 C26 109.9(3) C19 N1 C26 110.2(3) C20 N1 Ir 105.4(2) C19 N1 Ir 113.6(2) C26 N1 Ir 111.3(2) C25 N2 C21 119.5(3) C25 N2 Ir 127.8(3) C21 N2 Ir 112.7(2) C6 C1 C2 118.7(4) C6 C1 P 119.0(3) C2 C1 P 122.3(3) C3 C2 C1 120.5(4) C3 C2 H2 120(3) C1 C2 H2 120(3) C4 C3 C2 120.3(4) C4 C3 H3 122(3) C2 C3 H3 118(3) C5 C4 C3 119.7(4) C5 C4 H4 122(3) C3 C4 H4 118(3) C4 C5 C6 120.6(4) C4 C5 H5 119(3) C6 C5 H5 120(3) C5 C6 C1 120.2(4) C5 C6 H6 119(3) C1 C6 H6 121(3) C12 C7 C8 118.5(4) C12 C7 P 122.6(3) C8 C7 P 118.8(3) C9 C8 C7 120.7(4) C9 C8 H8 119(3) C7 C8 H8 120(3) C10 C9 C8 120.0(5) C10 C9 H9 118(3) C8 C9 H9 122(3) C11 C10 C9 120.3(4) C11 C10 H10 120(4) C9 C10 H10 120(4) C10 C11 C12 120.5(5) C10 C11 H11 125(4) C12 C11 H11 115(4) C7 C12 C11 120.0(4) C7 C12 H12 120(3) C11 C12 H12 120(3) C14 C13 C18 118.7(3) C14 C13 P 120.2(3) C18 C13 P 121.0(3) C15 C14 C13 121.1(4) C15 C14 H14 121(2) C13 C14 H14 118(2) C16 C15 C14 120.0(4) C16 C15 H15 122(3) C14 C15 H15 118(3) C15 C16 C17 119.8(4) C15 C16 H16 122(2) C17 C16 H16 118(2) C16 C17 C18 120.9(4) C16 C17 H17 119(3) C18 C17 H17 120(3) C17 C18 C13 119.5(3) C17 C18 C19 117.8(3) C13 C18 C19 122.7(3) N1 C19 C18 115.2(3) N1 C19 H19A 105(2) C18 C19 H19A 111(2) N1 C19 H19B 107(2) C18 C19 H19B 110(2) H19A C19 H19B 108(3) C21 C20 N1 111.7(3) C21 C20 H20A 114(3) N1 C20 H20A 108(3) C21 C20 H20B 108(2) N1 C20 H20B 106(2) H20A C20 H20B 108(3) N2 C21 C22 121.4(3) N2 C21 C20 115.8(3) C22 C21 C20 122.5(3) C23 C22 C21 119.0(4) C23 C22 H22 125(3) C21 C22 H22 116(3) C22 C23 C24 118.9(4) C22 C23 H23 122(3) C24 C23 H23 119(3) C23 C24 C25 119.5(4) C23 C24 H24 121(3) C25 C24 H24 120(3) N2 C25 C24 121.6(4) N2 C25 H25 115(3) C24 C25 H25 123(3) C27 C26 N1 111.9(3) C27 C26 H26A 108(2) N1 C26 H26A 109(3) C27 C26 H26B 114(2) N1 C26 H26B 106(2) H26A C26 H26B 108(3) C28 C27 C32 121.5(3) C28 C27 C26 118.6(3) C32 C27 C26 119.9(3) C27 C28 C29 117.8(3) C27 C28 Ir 114.5(2) C29 C28 Ir 127.5(3) C30 C29 C28 120.5(4) C30 C29 H29 119(3) C28 C29 H29 121(3) C31 C30 C29 120.9(4) C31 C30 H30 119(3) C29 C30 H30 120(3) C30 C31 C32 119.4(3) C30 C31 H31 121(3) C32 C31 H31 120(3) C31 C32 C27 119.8(4) C31 C32 H32 121(3) C27 C32 H32 120(3) Cl3A C51A Cl4A 113.8(6) Cl3A C51A H51A 108.8 Cl4A C51A H51A 108.8 Cl3A C51A H51B 108.8 Cl4A C51A H51B 108.8 H51A C51A H51B 107.7 Cl3B C51B Cl4B 106(2) Cl3B C51B H51C 110.6 Cl4B C51B H51C 110.6 Cl3B C51B H51D 110.6 Cl4B C51B H51D 110.6 H51C C51B H51D 108.7 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ir C28 2.022(3) Ir N1 2.092(3) Ir N2 2.110(3) Ir P 2.2584(9) Ir Cl1 2.3714(8) Ir Cl2 2.4847(9) P C7 1.818(4) P C13 1.825(4) P C1 1.830(4) N1 C20 1.502(4) N1 C19 1.504(4) N1 C26 1.523(4) N2 C25 1.335(5) N2 C21 1.350(5) C1 C6 1.395(5) C1 C2 1.397(5) C2 C3 1.387(6) C2 H2 0.88(5) C3 C4 1.380(7) C3 H3 0.90(5) C4 C5 1.379(7) C4 H4 0.91(5) C5 C6 1.390(5) C5 H5 0.93(5) C6 H6 0.94(4) C7 C12 1.387(6) C7 C8 1.403(6) C8 C9 1.380(6) C8 H8 0.92(5) C9 C10 1.378(8) C9 H9 0.99(6) C10 C11 1.366(8) C10 H10 0.89(5) C11 C12 1.397(6) C11 H11 0.91(6) C12 H12 0.89(4) C13 C14 1.401(5) C13 C18 1.406(5) C14 C15 1.390(5) C14 H14 0.93(4) C15 C16 1.382(6) C15 H15 0.93(4) C16 C17 1.389(6) C16 H16 0.90(4) C17 C18 1.398(5) C17 H17 0.99(4) C18 C19 1.506(5) C19 H19A 0.95(4) C19 H19B 0.95(4) C20 C21 1.490(5) C20 H20A 0.94(4) C20 H20B 0.97(4) C21 C22 1.389(5) C22 C23 1.382(6) C22 H22 0.93(4) C23 C24 1.381(6) C23 H23 0.97(4) C24 C25 1.384(5) C24 H24 0.96(4) C25 H25 0.94(4) C26 C27 1.496(5) C26 H26A 1.01(4) C26 H26B 0.97(4) C27 C28 1.399(5) C27 C32 1.401(5) C28 C29 1.400(5) C29 C30 1.398(5) C29 H29 0.93(5) C30 C31 1.385(6) C30 H30 0.89(4) C31 C32 1.387(6) C31 H31 0.92(5) C32 H32 0.96(4) C51A Cl3A 1.727(12) C51A Cl4A 1.746(11) C51A H51A 0.9900 C51A H51B 0.9900 Cl3B C51B 1.78(4) Cl4B C51B 1.76(4) C51B H51C 0.9900 C51B H51D 0.9900