# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1677 # CIF produced by WinGX routine CIF_UPDATE # Created on 1999-07-16 at 10:56:34 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.1beta3 # Request file : c:\wingx\files\archive.dat # CIF files read : herb09 erg struct # # CCDC ELECTRONIC DATA DEPOSITION FORM (CIF) # # This electronic data deposition form can be used: # # (a) WHEN SUBMITTING A PAPER TO A JOURNAL FOR PUBLICATION or # (b) WHEN SUBMITTING A PRIVATE COMMUNICATION TO THE CCDC # # A comprehensive archive of CIF resources is maintained by the IUCr # at its Chester office. This can be accessed # by anonymous ftp to ftp.iucr.org # or via the WWW at http://www.iucr.org/cif/home.html # If data items in this form are not available or not applicable # then ignore these items # A few items specific to CCDC input are indicated by _ccdc_ # # Submission and help information is provided at the end of this form #------------------------------------------------------------------------- #1 Global data block identification for start of deposition data_global # #------------------------------------------------------------------------- #2 Person making the deposition # _publ_contact_author 'Dahlenburg, Lutz' _publ_contact_author_email dahlenburg@chemie.uni-erlangen.de #------------------------------------------------------------------------- #3 Publication details # # The structure has been submitted for publication in J. Chem. Soc., # Dalton Trans. # # The CCDC journal deposition number, eg. 182/357, # should be included only if it has been assigned by the journal # loop_ _publ_author_name 'Dahlenburg, Lutz; Herbst, Konrad' _journal_name_full 'J. Chem. Soc., Dalton Trans.' _journal_volume ? _journal_page_first ? _journal_page_last ? _journal_year ? _ccdc_journal_depnumber ? # #------------------------------------------------------------------------- #4 Chemical and physical data # # Note that the units for melting point are Kelvin # The compound_id is the identifier for the compound in the published # paper, eg. 4a, II, etc. # Provide a brief description of any significant biological activity, # eg. antimalarial activity # If the compound exhibits polymorphism provide brief details, # eg. monoclinic form, low-temperature phase, etc. # For chemdiag leave blank - no longer necessary _ccdc_compound_id 6 _ccdc_biological_activity ? _ccdc_polymorph ? _ccdc_chemdiag_type ? _ccdc_chemdiag_records ; ? ; # #------------------------------------------------------------------------- #5 Other data relating to the structure determination and refinement # # Record the radiation type if not X-rays, eg. neutron # Record the temperature of the data collection (Kelvin) # if not room-temperature # Record R_squared if this is the only reliability factor given by # your refinement program # Describe briefly any disorder, eg. t-Butyl C31-33 disordered over # two sites with occupancies 0.6 and 0.4 # Under ccdc_comments record any other important information _ccdc_temp_data_collection 293 _ccdc_ls_R_squared 0.0734 _ccdc_disorder none _ccdc_comments ; none ; #------------------------------------------------------------------------- #6 Include your "standard" CIF file here # It should contain the following data items: # unit cell parameters and volume, z value, space group symbol, # R-factor(s), atomic coordinates with standard deviations, # occupancy factors, bond lengths and bond angles # Other data items may be present but will not necessarily be # included in the Cambridge Structural Database # # Do NOT include structure factors # # #------------------------------------------------------------------------- #SUBMISSION INFORMATION # # For a journal send the form to the address specified by the journal # # For a private communication to the CCDC send the form to the address # deposit@ccdc.cam.ac.uk # # For up-to-date information on deposition procedures, check the website # http://www.ccdc.cam.ac.uk/ data_herb09 _audit_creation_date 1999-07-16T10:56:34-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # SUBMISSION DETAILS # #----------------------------------------------------------------------------# # Name and address of author for correspondence _publ_contact_author_name 'Dahlenburg, Lutz' _publ_contact_author_address ; Institut f\"ur Anorganische Chemie Universita\"t Erlangen-N\"uernberg Egerlandstrasse 1 91058 Erlangen Germany ; _publ_contact_author_email 'dahlenburg@.chemie.uni-erlangen.de' _publ_contact_author_fax 'xx49 9131 8527353' _publ_contact_author_phone 'xx49 9131 8527387' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_contact_letter ; Date of submission: August 2, 1999 Please consider this CIF submission as supplementary data for assessment and/or deposition at the CCDC. ; #----------------------------------------------------------------------------# # TITLE AND AUTHOR LIST # #----------------------------------------------------------------------------# _publ_section_title ; Rhodium and iridium complexes with 2-(diphenylphosphanyl)anilido ligands: reactions with phenylacetylene and dimethyl acetylenedicarboxylate ; _publ_section_title_footnote ; Coordination Chemistry of Functional Phosphanes; Part 9. ; loop_ _publ_author_name _publ_author_address 'Dahlenburg, Lutz' ; Institut f\"ur Anorganische Chemie Universit\"at Erlangen-N\"urnberg Egerlandstrasse 1 91058 Erlangen Germany ; 'Herbst, Konrad' ; Institut f\"ur Anorganische Chemie Universit\"at Erlangen-N\"urnberg Egerlandstrasse 1 91058 Erlangen Germany ; #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; [1,2-Bis(methoxycarbonyl)vinyl-C,O-][2-(diphenylphosphanyl)phenylamido-N,P]- methoxycarbonyl(triphenylphosphane)iridium(III) ; _chemical_formula_moiety 'C44 H40 Ir1 N1 O6 P2' _chemical_formula_structural 'C44 H40 IR N O6 P2' _chemical_formula_sum 'C44 H40 Ir N O6 P2' _chemical_formula_weight 932.91 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.3200(10) _cell_length_b 18.325(9) _cell_length_c 16.1970(10) _cell_angle_alpha 90 _cell_angle_beta 98.093(7) _cell_angle_gamma 90 _cell_volume 3914(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.1 _cell_measurement_theta_max 14.3 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_special_details ; Crystals were grown from toluene/pentane. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.543 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 5 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.2416 _exptl_absorpt_correction_T_max 0.7648 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius TurboCAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 4 _diffrn_standards_decay_corr_max 1.079 _diffrn_standards_decay_corr_min 0.97 _diffrn_reflns_number 8169 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0799 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 6873 _reflns_number_gt 4605 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SIR-97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; All non-hydrogen atoms were located by direct methods and subsequent alternate cycles of difference Fourier synthesis and full matrix least-squares refinement. The resulting structural model was refined to convergence with allowance for anisotropic thermal motion of the non-H atoms. Hydrogen atoms were included in geometrically idealized positions employing appropriate riding models with isotropic displacement parameters constrained to 1.2 times the U~eq~ of their carrier atoms. The highest peaks in the final difference map were located at distances less than 1.0 \%A from the heavy metal atom. 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6873 _refine_ls_number_parameters 490 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0918 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0621 _refine_ls_wR_factor_all 0.0734 _refine_ls_goodness_of_fit_all 1.051 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.78 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.117 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 Ir Ir 0.103858(19) 0.213880(14) 0.285655(16) 0.03695(8) Uani 1 1 d . . . P1 P 0.24031(13) 0.16090(10) 0.23346(11) 0.0422(4) Uani 1 1 d . . . P2 P -0.00878(12) 0.28119(10) 0.35531(10) 0.0394(4) Uani 1 1 d . . . O1 O 0.1102(4) 0.2997(3) 0.1366(3) 0.0605(14) Uani 1 1 d . . . O2 O -0.0431(3) 0.2597(2) 0.1550(3) 0.0540(13) Uani 1 1 d . . . O3 O 0.1336(3) 0.1501(3) 0.4061(3) 0.0499(12) Uani 1 1 d . . . O4 O 0.0774(4) 0.0481(3) 0.4627(3) 0.0858(18) Uani 1 1 d . . . O5 O -0.1379(4) 0.0848(3) 0.1775(3) 0.0791(18) Uani 1 1 d . . . O6 O -0.0006(4) 0.1079(3) 0.1185(3) 0.0699(16) Uani 1 1 d . . . N N 0.2170(4) 0.2926(3) 0.3206(3) 0.0485(14) Uani 1 1 d . . . H0 H 0.2058 0.326 0.3555 0.058 Uiso 1 1 calc R . . C1 C 0.0592(5) 0.2649(3) 0.1787(4) 0.0432(17) Uani 1 1 d . . . C2 C -0.0827(6) 0.2994(5) 0.0807(5) 0.086(3) Uani 1 1 d . . . H2A H -0.1553 0.2958 0.0718 0.103 Uiso 1 1 calc R . . H2B H -0.0559 0.2791 0.0337 0.103 Uiso 1 1 calc R . . H2C H -0.0632 0.3498 0.0871 0.103 Uiso 1 1 calc R . . C3 C 0.0789(6) 0.0942(4) 0.3996(5) 0.059(2) Uani 1 1 d . . . C4 C 0.0133(5) 0.0769(4) 0.3243(4) 0.0550(19) Uani 1 1 d . . . H4 H -0.0266 0.0351 0.319 0.066 Uiso 1 1 calc R . . C5 C 0.0131(5) 0.1251(4) 0.2619(4) 0.0426(17) Uani 1 1 d . . . C6 C -0.0511(6) 0.1037(4) 0.1824(5) 0.0513(19) Uani 1 1 d . . . C7 C 0.1423(7) 0.0640(5) 0.5390(5) 0.113(4) Uani 1 1 d . . . H7A H 0.1402 0.0242 0.5773 0.135 Uiso 1 1 calc R . . H7B H 0.1195 0.1078 0.5631 0.135 Uiso 1 1 calc R . . H7C H 0.2105 0.0706 0.5277 0.135 Uiso 1 1 calc R . . C8 C -0.0552(6) 0.0923(5) 0.0379(5) 0.100(3) Uani 1 1 d . . . H8A H -0.0111 0.0984 -0.0037 0.12 Uiso 1 1 calc R . . H8B H -0.1117 0.1251 0.0266 0.12 Uiso 1 1 calc R . . H8C H -0.0795 0.0429 0.0367 0.12 Uiso 1 1 calc R . . C9 C 0.3306(5) 0.2340(3) 0.2425(4) 0.0446(18) Uani 1 1 d . . . C10 C 0.3062(5) 0.2927(4) 0.2906(4) 0.0449(16) Uani 1 1 d . . . C11 C 0.3785(5) 0.3488(4) 0.3050(4) 0.056(2) Uani 1 1 d . . . H11 H 0.366 0.3883 0.3381 0.068 Uiso 1 1 calc R . . C12 C 0.4662(6) 0.3463(5) 0.2713(5) 0.074(2) Uani 1 1 d . . . H12 H 0.5121 0.3846 0.2815 0.088 Uiso 1 1 calc R . . C13 C 0.4895(5) 0.2889(5) 0.2225(5) 0.079(2) Uani 1 1 d . . . H13 H 0.5498 0.2884 0.1997 0.095 Uiso 1 1 calc R . . C14 C 0.4216(5) 0.2326(4) 0.2085(5) 0.064(2) Uani 1 1 d . . . H14 H 0.436 0.193 0.1762 0.077 Uiso 1 1 calc R . . C15 C 0.2395(5) 0.1196(4) 0.1313(4) 0.0512(19) Uani 1 1 d . . . C16 C 0.1987(5) 0.1558(4) 0.0601(4) 0.063(2) Uani 1 1 d . . . H16 H 0.1719 0.2022 0.065 0.076 Uiso 1 1 calc R . . C17 C 0.1960(6) 0.1259(6) -0.0178(5) 0.080(3) Uani 1 1 d . . . H17 H 0.167 0.1518 -0.0646 0.096 Uiso 1 1 calc R . . C18 C 0.2363(6) 0.0575(5) -0.0265(5) 0.074(3) Uani 1 1 d . . . H18 H 0.2335 0.0363 -0.079 0.089 Uiso 1 1 calc R . . C19 C 0.2804(6) 0.0214(5) 0.0430(6) 0.079(3) Uani 1 1 d . . . H19 H 0.3091 -0.0244 0.0376 0.095 Uiso 1 1 calc R . . C20 C 0.2830(5) 0.0518(4) 0.1210(5) 0.063(2) Uani 1 1 d . . . H20 H 0.3142 0.0266 0.1675 0.076 Uiso 1 1 calc R . . C21 C 0.2902(5) 0.0905(4) 0.3056(4) 0.0486(18) Uani 1 1 d . . . C22 C 0.3676(6) 0.1060(4) 0.3710(5) 0.066(2) Uani 1 1 d . . . H22 H 0.3989 0.1514 0.3739 0.079 Uiso 1 1 calc R . . C23 C 0.3978(8) 0.0539(6) 0.4311(6) 0.098(3) Uani 1 1 d . . . H23 H 0.4468 0.0651 0.4761 0.117 Uiso 1 1 calc R . . C24 C 0.3552(9) -0.0141(6) 0.4240(7) 0.108(4) Uani 1 1 d . . . H24 H 0.3784 -0.0499 0.4628 0.13 Uiso 1 1 calc R . . C25 C 0.2786(8) -0.0307(5) 0.3606(7) 0.096(3) Uani 1 1 d . . . H25 H 0.2492 -0.0768 0.3568 0.116 Uiso 1 1 calc R . . C26 C 0.2464(6) 0.0221(4) 0.3033(5) 0.065(2) Uani 1 1 d . . . H26 H 0.1932 0.0116 0.2614 0.079 Uiso 1 1 calc R . . C27 C -0.0661(5) 0.3609(4) 0.2991(4) 0.0448(17) Uani 1 1 d . . . C28 C -0.1679(6) 0.3769(4) 0.2889(4) 0.057(2) Uani 1 1 d . . . H28 H -0.2121 0.3453 0.3106 0.068 Uiso 1 1 calc R . . C29 C -0.2054(7) 0.4384(5) 0.2474(5) 0.081(3) Uani 1 1 d . . . H29 H -0.2745 0.4485 0.2417 0.097 Uiso 1 1 calc R . . C30 C -0.1409(9) 0.4848(5) 0.2145(5) 0.089(3) Uani 1 1 d . . . H30 H -0.1661 0.5263 0.1856 0.107 Uiso 1 1 calc R . . C31 C -0.0395(8) 0.4699(5) 0.2243(5) 0.080(3) Uani 1 1 d . . . H31 H 0.0045 0.5017 0.2025 0.097 Uiso 1 1 calc R . . C32 C -0.0021(6) 0.4083(4) 0.2663(5) 0.064(2) Uani 1 1 d . . . H32 H 0.0671 0.3986 0.2725 0.076 Uiso 1 1 calc R . . C33 C 0.0483(5) 0.3228(3) 0.4529(4) 0.0391(16) Uani 1 1 d . . . C34 C 0.0011(5) 0.3805(4) 0.4862(4) 0.0515(18) Uani 1 1 d . . . H34 H -0.0583 0.3994 0.457 0.062 Uiso 1 1 calc R . . C35 C 0.0405(6) 0.4109(4) 0.5623(4) 0.056(2) Uani 1 1 d . . . H35 H 0.0068 0.4492 0.5842 0.067 Uiso 1 1 calc R . . C36 C 0.1280(6) 0.3849(4) 0.6048(4) 0.058(2) Uani 1 1 d . . . H36 H 0.1554 0.4062 0.6551 0.069 Uiso 1 1 calc R . . C37 C 0.1760(6) 0.3274(4) 0.5740(4) 0.063(2) Uani 1 1 d . . . H37 H 0.2351 0.3089 0.6041 0.076 Uiso 1 1 calc R . . C38 C 0.1373(5) 0.2965(4) 0.4981(4) 0.0545(19) Uani 1 1 d . . . H38 H 0.1712 0.2578 0.4772 0.065 Uiso 1 1 calc R . . C39 C -0.1159(5) 0.2312(3) 0.3852(4) 0.0449(17) Uani 1 1 d . . . C40 C -0.1918(5) 0.2077(4) 0.3231(5) 0.060(2) Uani 1 1 d . . . H40 H -0.1839 0.2138 0.2673 0.072 Uiso 1 1 calc R . . C41 C -0.2782(6) 0.1756(4) 0.3429(6) 0.076(3) Uani 1 1 d . . . H41 H -0.3298 0.1621 0.301 0.091 Uiso 1 1 calc R . . C42 C -0.2882(7) 0.1636(5) 0.4253(7) 0.095(3) Uani 1 1 d . . . H42 H -0.3474 0.143 0.4392 0.114 Uiso 1 1 calc R . . C43 C -0.2108(8) 0.1818(5) 0.4863(6) 0.098(3) Uani 1 1 d . . . H43 H -0.2161 0.1705 0.5415 0.118 Uiso 1 1 calc R . . C44 C -0.1248(6) 0.2170(4) 0.4677(4) 0.065(2) Uani 1 1 d . . . H44 H -0.0737 0.2308 0.51 0.078 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir 0.04003(13) 0.03456(13) 0.03681(13) -0.00039(17) 0.00730(9) -0.00047(17) P1 0.0440(10) 0.0408(10) 0.0423(10) -0.0032(9) 0.0077(8) 0.0012(9) P2 0.0410(9) 0.0396(9) 0.0382(9) -0.0006(9) 0.0078(7) 0.0009(10) O1 0.076(3) 0.051(3) 0.059(3) 0.017(3) 0.023(3) -0.002(3) O2 0.055(3) 0.058(3) 0.046(3) 0.012(2) -0.004(2) -0.007(2) O3 0.057(3) 0.051(3) 0.042(3) 0.007(2) 0.007(2) -0.003(3) O4 0.101(5) 0.090(4) 0.064(4) 0.038(3) 0.003(3) -0.025(4) O5 0.054(3) 0.110(5) 0.072(4) -0.011(4) 0.006(3) -0.021(4) O6 0.062(3) 0.094(4) 0.054(3) -0.025(3) 0.011(3) -0.018(3) N 0.053(3) 0.044(3) 0.048(3) -0.013(3) 0.009(3) -0.003(3) C1 0.055(4) 0.033(4) 0.041(4) -0.003(3) 0.002(3) 0.000(3) C2 0.082(6) 0.091(7) 0.075(6) 0.035(5) -0.017(5) -0.006(5) C3 0.062(5) 0.061(5) 0.058(5) 0.023(4) 0.017(4) 0.010(4) C4 0.062(5) 0.046(4) 0.057(5) 0.003(4) 0.009(4) -0.019(4) C5 0.034(4) 0.049(4) 0.047(4) -0.002(4) 0.012(3) -0.002(3) C6 0.049(5) 0.041(4) 0.063(5) 0.000(4) 0.005(4) -0.001(4) C7 0.136(9) 0.143(10) 0.054(6) 0.038(6) -0.003(6) -0.025(8) C8 0.095(7) 0.144(9) 0.061(6) -0.039(6) 0.007(5) -0.021(7) C9 0.038(4) 0.049(5) 0.048(4) 0.001(3) 0.010(3) 0.001(3) C10 0.044(4) 0.045(4) 0.045(4) 0.001(4) 0.005(3) 0.000(4) C11 0.056(5) 0.046(5) 0.064(5) -0.002(4) -0.001(4) -0.010(4) C12 0.056(5) 0.071(6) 0.094(7) -0.001(5) 0.011(5) -0.031(5) C13 0.046(4) 0.100(7) 0.094(6) -0.003(7) 0.018(4) -0.023(6) C14 0.052(5) 0.073(6) 0.069(5) -0.009(5) 0.014(4) 0.007(4) C15 0.044(4) 0.059(5) 0.053(5) -0.013(4) 0.014(4) -0.012(4) C16 0.067(5) 0.075(6) 0.050(5) 0.005(5) 0.018(4) 0.008(5) C17 0.080(6) 0.115(8) 0.049(5) -0.012(5) 0.016(5) -0.011(6) C18 0.081(6) 0.094(7) 0.052(5) -0.032(5) 0.027(5) -0.037(6) C19 0.088(7) 0.066(6) 0.090(7) -0.034(6) 0.035(6) -0.010(5) C20 0.068(5) 0.065(5) 0.059(5) -0.017(4) 0.022(4) 0.005(4) C21 0.049(4) 0.046(4) 0.050(5) -0.002(4) 0.006(4) 0.011(4) C22 0.072(6) 0.062(5) 0.062(5) -0.007(5) 0.002(5) 0.020(4) C23 0.115(8) 0.096(8) 0.075(7) -0.001(6) -0.015(6) 0.038(7) C24 0.146(11) 0.081(8) 0.096(8) 0.040(7) 0.010(8) 0.033(8) C25 0.106(8) 0.055(6) 0.127(9) 0.026(6) 0.013(7) 0.009(6) C26 0.078(6) 0.052(5) 0.069(6) 0.009(4) 0.021(5) 0.014(5) C27 0.059(5) 0.041(4) 0.033(4) -0.002(3) 0.005(3) 0.003(4) C28 0.059(5) 0.058(5) 0.051(5) -0.006(4) 0.003(4) 0.017(4) C29 0.095(7) 0.081(7) 0.064(6) -0.004(5) -0.002(5) 0.046(6) C30 0.147(10) 0.050(6) 0.063(6) 0.005(5) -0.006(7) 0.030(6) C31 0.119(8) 0.046(5) 0.075(6) 0.008(5) 0.008(6) -0.008(6) C32 0.076(6) 0.042(4) 0.071(5) 0.005(4) 0.006(5) 0.000(4) C33 0.046(4) 0.039(4) 0.035(4) 0.001(3) 0.013(3) 0.000(3) C34 0.052(4) 0.050(5) 0.051(5) 0.003(4) 0.001(4) 0.000(4) C35 0.064(5) 0.048(4) 0.057(5) -0.014(4) 0.014(4) 0.005(4) C36 0.065(5) 0.066(5) 0.042(4) -0.013(4) 0.010(4) -0.008(4) C37 0.064(5) 0.080(6) 0.043(5) -0.004(4) -0.002(4) 0.004(5) C38 0.054(4) 0.058(5) 0.052(4) -0.010(4) 0.007(3) 0.006(4) C39 0.051(4) 0.035(4) 0.053(4) 0.002(3) 0.019(4) 0.007(3) C40 0.059(5) 0.060(5) 0.063(5) -0.010(5) 0.013(4) -0.009(5) C41 0.066(6) 0.068(6) 0.099(7) -0.018(5) 0.028(5) -0.017(5) C42 0.089(7) 0.078(7) 0.130(9) -0.008(7) 0.051(7) -0.040(6) C43 0.134(9) 0.083(7) 0.083(7) 0.014(6) 0.038(7) -0.033(7) C44 0.073(5) 0.066(5) 0.057(5) 0.010(5) 0.012(4) -0.011(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Ir C1 1.985(6) . ? Ir C5 2.032(6) . ? Ir N 2.105(5) . ? Ir O3 2.262(4) . ? Ir P1 2.3223(18) . ? Ir P2 2.3498(17) . ? P1 C9 1.793(6) . ? P1 C21 1.804(7) . ? P1 C15 1.818(7) . ? P2 C39 1.817(6) . ? P2 C33 1.822(6) . ? P2 C27 1.831(7) . ? O1 C1 1.210(7) . ? O2 C1 1.367(7) . ? O2 C2 1.440(7) . ? O3 C3 1.253(8) . ? O4 C3 1.328(8) . ? O4 C7 1.435(9) . ? O5 C6 1.199(8) . ? O6 C6 1.314(8) . ? O6 C8 1.431(8) . ? N C10 1.346(7) . ? N H0 0.86 . ? C2 H2A 0.96 . ? C2 H2B 0.96 . ? C2 H2C 0.96 . ? C3 C4 1.433(9) . ? C4 C5 1.342(8) . ? C4 H4 0.93 . ? C5 C6 1.494(9) . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? C9 C10 1.392(9) . ? C9 C14 1.399(9) . ? C10 C11 1.406(9) . ? C11 C12 1.359(9) . ? C11 H11 0.93 . ? C12 C13 1.376(11) . ? C12 H12 0.93 . ? C13 C14 1.371(10) . ? C13 H13 0.93 . ? C14 H14 0.93 . ? C15 C16 1.374(9) . ? C15 C20 1.390(9) . ? C16 C17 1.372(9) . ? C16 H16 0.93 . ? C17 C18 1.380(11) . ? C17 H17 0.93 . ? C18 C19 1.366(11) . ? C18 H18 0.93 . ? C19 C20 1.377(9) . ? C19 H19 0.93 . ? C20 H20 0.93 . ? C21 C26 1.381(9) . ? C21 C22 1.399(9) . ? C22 C23 1.382(10) . ? C22 H22 0.93 . ? C23 C24 1.369(13) . ? C23 H23 0.93 . ? C24 C25 1.376(12) . ? C24 H24 0.93 . ? C25 C26 1.366(10) . ? C25 H25 0.93 . ? C26 H26 0.93 . ? C27 C28 1.374(9) . ? C27 C32 1.374(9) . ? C28 C29 1.370(10) . ? C28 H28 0.93 . ? C29 C30 1.370(12) . ? C29 H29 0.93 . ? C30 C31 1.365(11) . ? C30 H30 0.93 . ? C31 C32 1.375(10) . ? C31 H31 0.93 . ? C32 H32 0.93 . ? C33 C34 1.379(8) . ? C33 C38 1.388(8) . ? C34 C35 1.387(9) . ? C34 H34 0.93 . ? C35 C36 1.355(9) . ? C35 H35 0.93 . ? C36 C37 1.361(9) . ? C36 H36 0.93 . ? C37 C38 1.386(8) . ? C37 H37 0.93 . ? C38 H38 0.93 . ? C39 C44 1.383(9) . ? C39 C40 1.391(9) . ? C40 C41 1.370(9) . ? C40 H40 0.93 . ? C41 C42 1.377(11) . ? C41 H41 0.93 . ? C42 C43 1.366(11) . ? C42 H42 0.93 . ? C43 C44 1.385(10) . ? C43 H43 0.93 . ? C44 H44 0.93 . ? 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 C1 Ir C5 96.6(3) . . ? C1 Ir N 91.6(2) . . ? C5 Ir N 169.8(2) . . ? C1 Ir O3 172.5(2) . . ? C5 Ir O3 77.1(2) . . ? N Ir O3 95.16(18) . . ? C1 Ir P1 91.9(2) . . ? C5 Ir P1 94.11(18) . . ? N Ir P1 79.45(15) . . ? O3 Ir P1 92.68(12) . . ? C1 Ir P2 92.22(19) . . ? C5 Ir P2 96.21(18) . . ? N Ir P2 89.57(15) . . ? O3 Ir P2 84.46(12) . . ? P1 Ir P2 168.38(6) . . ? C9 P1 C21 107.5(3) . . ? C9 P1 C15 107.7(3) . . ? C21 P1 C15 104.2(3) . . ? C9 P1 Ir 102.0(2) . . ? C21 P1 Ir 107.4(2) . . ? C15 P1 Ir 126.9(2) . . ? C39 P2 C33 103.1(3) . . ? C39 P2 C27 104.3(3) . . ? C33 P2 C27 101.1(3) . . ? C39 P2 Ir 116.2(2) . . ? C33 P2 Ir 114.8(2) . . ? C27 P2 Ir 115.4(2) . . ? C1 O2 C2 115.7(5) . . ? C3 O3 Ir 108.7(4) . . ? C3 O4 C7 117.4(7) . . ? C6 O6 C8 117.1(6) . . ? C10 N Ir 122.6(5) . . ? C10 N H0 118.7 . . ? Ir N H0 118.7 . . ? O1 C1 O2 119.6(6) . . ? O1 C1 Ir 128.1(5) . . ? O2 C1 Ir 112.2(5) . . ? O2 C2 H2A 109.5 . . ? O2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O3 C3 O4 121.8(7) . . ? O3 C3 C4 122.0(6) . . ? O4 C3 C4 116.1(7) . . ? C5 C4 C3 115.6(6) . . ? C5 C4 H4 122.2 . . ? C3 C4 H4 122.2 . . ? C4 C5 C6 114.7(6) . . ? C4 C5 Ir 116.5(5) . . ? C6 C5 Ir 128.8(5) . . ? O5 C6 O6 124.2(7) . . ? O5 C6 C5 124.2(7) . . ? O6 C6 C5 111.7(6) . . ? O4 C7 H7A 109.5 . . ? O4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O6 C8 H8A 109.5 . . ? O6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C14 121.2(6) . . ? C10 C9 P1 114.6(5) . . ? C14 C9 P1 124.2(6) . . ? N C10 C9 119.3(6) . . ? N C10 C11 124.0(7) . . ? C9 C10 C11 116.7(6) . . ? C12 C11 C10 121.1(7) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C13 122.2(7) . . ? C11 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? C14 C13 C12 118.3(7) . . ? C14 C13 H13 120.9 . . ? C12 C13 H13 120.9 . . ? C13 C14 C9 120.5(7) . . ? C13 C14 H14 119.7 . . ? C9 C14 H14 119.7 . . ? C16 C15 C20 116.9(7) . . ? C16 C15 P1 120.9(6) . . ? C20 C15 P1 122.2(6) . . ? C17 C16 C15 122.4(8) . . ? C17 C16 H16 118.8 . . ? C15 C16 H16 118.8 . . ? C16 C17 C18 119.7(9) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C19 C18 C17 119.0(8) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C20 120.8(8) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C19 C20 C15 121.0(8) . . ? C19 C20 H20 119.5 . . ? C15 C20 H20 119.5 . . ? C26 C21 C22 117.9(7) . . ? C26 C21 P1 121.1(6) . . ? C22 C21 P1 120.7(6) . . ? C23 C22 C21 120.3(8) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C24 C23 C22 119.5(9) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 121.3(9) . . ? C23 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C26 C25 C24 118.7(9) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C25 C26 C21 122.2(8) . . ? C25 C26 H26 118.9 . . ? C21 C26 H26 118.9 . . ? C28 C27 C32 118.3(7) . . ? C28 C27 P2 124.4(6) . . ? C32 C27 P2 117.3(6) . . ? C29 C28 C27 121.3(8) . . ? C29 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C28 C29 C30 119.7(9) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C31 C30 C29 119.7(9) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C30 C31 C32 120.4(9) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C27 C32 C31 120.5(8) . . ? C27 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C34 C33 C38 117.6(6) . . ? C34 C33 P2 120.2(5) . . ? C38 C33 P2 122.2(5) . . ? C33 C34 C35 121.3(7) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? C36 C35 C34 120.1(7) . . ? C36 C35 H35 120 . . ? C34 C35 H35 120 . . ? C35 C36 C37 120.0(7) . . ? C35 C36 H36 120 . . ? C37 C36 H36 120 . . ? C36 C37 C38 120.4(7) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C37 C38 C33 120.6(7) . . ? C37 C38 H38 119.7 . . ? C33 C38 H38 119.7 . . ? C44 C39 C40 119.2(7) . . ? C44 C39 P2 122.0(6) . . ? C40 C39 P2 118.8(5) . . ? C41 C40 C39 120.8(7) . . ? C41 C40 H40 119.6 . . ? C39 C40 H40 119.6 . . ? C40 C41 C42 119.7(8) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? C43 C42 C41 119.8(9) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C42 C43 C44 121.3(9) . . ? C42 C43 H43 119.4 . . ? C44 C43 H43 119.4 . . ? C39 C44 C43 119.0(7) . . ? C39 C44 H44 120.5 . . ? C43 C44 H44 120.5 . . ? 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 C1 Ir P1 C9 79.8(3) . . . . ? C5 Ir P1 C9 176.6(3) . . . . ? N Ir P1 C9 -11.4(3) . . . . ? O3 Ir P1 C9 -106.2(2) . . . . ? P2 Ir P1 C9 -30.8(4) . . . . ? C1 Ir P1 C21 -167.3(3) . . . . ? C5 Ir P1 C21 -70.6(3) . . . . ? N Ir P1 C21 101.4(3) . . . . ? O3 Ir P1 C21 6.7(3) . . . . ? P2 Ir P1 C21 82.1(4) . . . . ? C1 Ir P1 C15 -43.4(4) . . . . ? C5 Ir P1 C15 53.3(4) . . . . ? N Ir P1 C15 -134.7(3) . . . . ? O3 Ir P1 C15 130.6(3) . . . . ? P2 Ir P1 C15 -154.1(4) . . . . ? C1 Ir P2 C39 109.7(3) . . . . ? C5 Ir P2 C39 12.9(3) . . . . ? N Ir P2 C39 -158.7(3) . . . . ? O3 Ir P2 C39 -63.5(3) . . . . ? P1 Ir P2 C39 -139.7(4) . . . . ? C1 Ir P2 C33 -129.9(3) . . . . ? C5 Ir P2 C33 133.3(3) . . . . ? N Ir P2 C33 -38.3(3) . . . . ? O3 Ir P2 C33 56.9(3) . . . . ? P1 Ir P2 C33 -19.3(4) . . . . ? C1 Ir P2 C27 -12.9(3) . . . . ? C5 Ir P2 C27 -109.7(3) . . . . ? N Ir P2 C27 78.7(3) . . . . ? O3 Ir P2 C27 173.9(3) . . . . ? P1 Ir P2 C27 97.7(4) . . . . ? C1 Ir O3 C3 31.8(18) . . . . ? C5 Ir O3 C3 -1.8(5) . . . . ? N Ir O3 C3 -175.0(5) . . . . ? P1 Ir O3 C3 -95.4(5) . . . . ? P2 Ir O3 C3 95.9(5) . . . . ? C1 Ir N C10 -79.1(5) . . . . ? C5 Ir N C10 64.1(14) . . . . ? O3 Ir N C10 104.3(5) . . . . ? P1 Ir N C10 12.6(5) . . . . ? P2 Ir N C10 -171.3(5) . . . . ? C2 O2 C1 O1 -1.8(9) . . . . ? C2 O2 C1 Ir 176.0(5) . . . . ? C5 Ir C1 O1 -141.5(6) . . . . ? N Ir C1 O1 32.4(6) . . . . ? O3 Ir C1 O1 -174.4(12) . . . . ? P1 Ir C1 O1 -47.1(6) . . . . ? P2 Ir C1 O1 122.0(6) . . . . ? C5 Ir C1 O2 40.9(5) . . . . ? N Ir C1 O2 -145.3(4) . . . . ? O3 Ir C1 O2 8.0(19) . . . . ? P1 Ir C1 O2 135.2(4) . . . . ? P2 Ir C1 O2 -55.6(4) . . . . ? Ir O3 C3 O4 -177.0(6) . . . . ? Ir O3 C3 C4 2.1(8) . . . . ? C7 O4 C3 O3 -0.9(11) . . . . ? C7 O4 C3 C4 -179.9(7) . . . . ? O3 C3 C4 C5 -1.1(11) . . . . ? O4 C3 C4 C5 178.0(7) . . . . ? C3 C4 C5 C6 176.5(6) . . . . ? C3 C4 C5 Ir -0.7(8) . . . . ? C1 Ir C5 C4 -174.5(5) . . . . ? N Ir C5 C4 42.7(16) . . . . ? O3 Ir C5 C4 1.3(5) . . . . ? P1 Ir C5 C4 93.1(5) . . . . ? P2 Ir C5 C4 -81.5(5) . . . . ? C1 Ir C5 C6 8.8(6) . . . . ? N Ir C5 C6 -134.1(12) . . . . ? O3 Ir C5 C6 -175.4(6) . . . . ? P1 Ir C5 C6 -83.6(6) . . . . ? P2 Ir C5 C6 101.7(6) . . . . ? C8 O6 C6 O5 3.3(11) . . . . ? C8 O6 C6 C5 -177.0(6) . . . . ? C4 C5 C6 O5 50.8(10) . . . . ? Ir C5 C6 O5 -132.4(7) . . . . ? C4 C5 C6 O6 -129.0(7) . . . . ? Ir C5 C6 O6 47.8(8) . . . . ? C21 P1 C9 C10 -100.6(5) . . . . ? C15 P1 C9 C10 147.7(5) . . . . ? Ir P1 C9 C10 12.2(5) . . . . ? C21 P1 C9 C14 76.3(6) . . . . ? C15 P1 C9 C14 -35.5(7) . . . . ? Ir P1 C9 C14 -170.9(5) . . . . ? Ir N C10 C9 -8.0(8) . . . . ? Ir N C10 C11 172.4(5) . . . . ? C14 C9 C10 N 178.6(6) . . . . ? P1 C9 C10 N -4.4(8) . . . . ? C14 C9 C10 C11 -1.7(10) . . . . ? P1 C9 C10 C11 175.2(5) . . . . ? N C10 C11 C12 -178.6(7) . . . . ? C9 C10 C11 C12 1.8(10) . . . . ? C10 C11 C12 C13 -0.7(12) . . . . ? C11 C12 C13 C14 -0.5(13) . . . . ? C12 C13 C14 C9 0.6(12) . . . . ? C10 C9 C14 C13 0.6(11) . . . . ? P1 C9 C14 C13 -176.0(6) . . . . ? C9 P1 C15 C16 -71.0(6) . . . . ? C21 P1 C15 C16 175.1(6) . . . . ? Ir P1 C15 C16 49.9(7) . . . . ? C9 P1 C15 C20 106.6(6) . . . . ? C21 P1 C15 C20 -7.4(7) . . . . ? Ir P1 C15 C20 -132.6(5) . . . . ? C20 C15 C16 C17 2.9(11) . . . . ? P1 C15 C16 C17 -179.4(6) . . . . ? C15 C16 C17 C18 -0.8(12) . . . . ? C16 C17 C18 C19 -1.5(13) . . . . ? C17 C18 C19 C20 1.4(13) . . . . ? C18 C19 C20 C15 0.9(12) . . . . ? C16 C15 C20 C19 -3.0(11) . . . . ? P1 C15 C20 C19 179.4(6) . . . . ? C9 P1 C21 C26 -168.9(6) . . . . ? C15 P1 C21 C26 -54.8(7) . . . . ? Ir P1 C21 C26 82.0(6) . . . . ? C9 P1 C21 C22 17.8(7) . . . . ? C15 P1 C21 C22 131.9(6) . . . . ? Ir P1 C21 C22 -91.3(6) . . . . ? C26 C21 C22 C23 -0.5(11) . . . . ? P1 C21 C22 C23 173.0(6) . . . . ? C21 C22 C23 C24 3.4(14) . . . . ? C22 C23 C24 C25 -3.7(17) . . . . ? C23 C24 C25 C26 1.1(17) . . . . ? C24 C25 C26 C21 2.0(14) . . . . ? C22 C21 C26 C25 -2.2(12) . . . . ? P1 C21 C26 C25 -175.7(7) . . . . ? C39 P2 C27 C28 3.1(7) . . . . ? C33 P2 C27 C28 -103.6(6) . . . . ? Ir P2 C27 C28 131.9(5) . . . . ? C39 P2 C27 C32 -178.0(5) . . . . ? C33 P2 C27 C32 75.2(6) . . . . ? Ir P2 C27 C32 -49.3(6) . . . . ? C32 C27 C28 C29 -0.1(11) . . . . ? P2 C27 C28 C29 178.7(5) . . . . ? C27 C28 C29 C30 0.7(12) . . . . ? C28 C29 C30 C31 -0.9(13) . . . . ? C29 C30 C31 C32 0.7(14) . . . . ? C28 C27 C32 C31 -0.1(11) . . . . ? P2 C27 C32 C31 -179.0(6) . . . . ? C30 C31 C32 C27 -0.1(13) . . . . ? C39 P2 C33 C34 -72.7(6) . . . . ? C27 P2 C33 C34 34.9(6) . . . . ? Ir P2 C33 C34 159.9(5) . . . . ? C39 P2 C33 C38 104.7(6) . . . . ? C27 P2 C33 C38 -147.7(6) . . . . ? Ir P2 C33 C38 -22.7(6) . . . . ? C38 C33 C34 C35 -0.5(10) . . . . ? P2 C33 C34 C35 177.0(5) . . . . ? C33 C34 C35 C36 1.2(11) . . . . ? C34 C35 C36 C37 -1.8(11) . . . . ? C35 C36 C37 C38 1.7(11) . . . . ? C36 C37 C38 C33 -1.0(11) . . . . ? C34 C33 C38 C37 0.4(10) . . . . ? P2 C33 C38 C37 -177.1(5) . . . . ? C33 P2 C39 C44 -15.1(7) . . . . ? C27 P2 C39 C44 -120.3(6) . . . . ? Ir P2 C39 C44 111.4(6) . . . . ? C33 P2 C39 C40 163.9(5) . . . . ? C27 P2 C39 C40 58.7(6) . . . . ? Ir P2 C39 C40 -69.6(6) . . . . ? C44 C39 C40 C41 4.9(11) . . . . ? P2 C39 C40 C41 -174.2(6) . . . . ? C39 C40 C41 C42 -2.9(13) . . . . ? C40 C41 C42 C43 -1.7(14) . . . . ? C41 C42 C43 C44 4.4(15) . . . . ? C40 C39 C44 C43 -2.2(11) . . . . ? P2 C39 C44 C43 176.8(6) . . . . ? C42 C43 C44 C39 -2.4(14) . . . . ?