data_shelx _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H63 Ir O3 P2 Si3' _chemical_formula_weight 858.25 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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' _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_H-M_alt 'P 21' _space_group_name_Hall 'P 2yb' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.509(2) _cell_length_b 18.340(3) _cell_length_c 15.539(3) _cell_angle_alpha 90 _cell_angle_beta 96.485(2) _cell_angle_gamma 90 _cell_volume 4108.6(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4973 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _exptl_crystal_description 'irregilar block' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.387 _exptl_crystal_F_000 1760 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.173 _exptl_crystal_size_mid 0.127 _exptl_crystal_size_min 0.119 _exptl_absorpt_coefficient_mu 3.444 _shelx_estimated_absorpt_T_min 0.587 _shelx_estimated_absorpt_T_max 0.685 _exptl_absorpt_correction_T_min 0.597 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; Absorption correction performed with SADABS program. This is based on the method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33. SADABS: Area-Detector Absorption Correction. Bruker-AXS within SAINT+ package, v. 6.1 (2000). ; _exptl_absorpt_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 CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_decay_% 0 _diffrn_reflns_number 47825 _diffrn_reflns_av_unetI/netI 0.1751 _diffrn_reflns_av_R_equivalents 0.1015 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.319 _diffrn_reflns_theta_max 29.702 _diffrn_reflns_theta_full 27.500 _diffrn_measured_fraction_theta_max 0.934 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.934 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.934 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 21062 _reflns_number_gt 12877 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.943 _reflns_Friedel_fraction_max 0.934 _reflns_Friedel_fraction_full 1.000 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'apex2 v. 7.0 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT+ v. 7.56a (Bruker AXS, 2008)' _computing_data_reduction 'SAINT+ v. 7.56a (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics 'XP, SHELXTL v. 6.14 (Bruker, 2000)' _computing_publication_material 'XCIF, SHELXTL v. 6.14 (Bruker, 2000)' _refine_special_details ; Refined as a 2-component inversion twin. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0427P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.021(9) _chemical_absolute_configuration ? _refine_ls_number_reflns 21062 _refine_ls_number_parameters 821 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1413 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1242 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_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 Ir1 Ir 0.16835(4) 0.10715(3) 0.45291(3) 0.02014(15) Uani 1 1 d D . . . . H01 H 0.169(9) 0.058(6) 0.369(5) 0.024 Uiso 1 1 d D U . . . H02 H 0.181(9) 0.158(6) 0.536(5) 0.024 Uiso 1 1 d D U . . . H03 H 0.375(9) 0.331(5) 1.031(6) 0.024 Uiso 1 1 d D U . . . Ir2 Ir 0.35777(4) 0.39038(3) 0.95650(3) 0.01974(14) Uani 1 1 d D . . . . H04 H 0.323619 0.440115 0.875779 0.024 Uiso 1 1 d R U . . . P1 P 0.1580(3) -0.0015(2) 0.5188(2) 0.0194(9) Uani 1 1 d . . . . . P2 P 0.2225(3) 0.1899(2) 0.3630(2) 0.0238(9) Uani 1 1 d . . . . . P3 P 0.4018(3) 0.4947(2) 1.0246(2) 0.0214(9) Uani 1 1 d . . . . . P4 P 0.2680(3) 0.3029(2) 0.8872(2) 0.0236(9) Uani 1 1 d . . . . . Si1 Si 0.0169(3) 0.1392(2) 0.4405(3) 0.0235(10) Uani 1 1 d . . . . . Si2 Si -0.0999(3) 0.1272(3) 0.5979(3) 0.0281(12) Uani 1 1 d . . . . . Si3 Si -0.1429(3) 0.0958(3) 0.2944(2) 0.0313(11) Uani 1 1 d . . . . . Si4 Si 0.5004(3) 0.3508(2) 0.9307(3) 0.0229(10) Uani 1 1 d . . . . . Si5 Si 0.6092(3) 0.3814(3) 0.7712(3) 0.0406(13) Uani 1 1 d D . . . . Si6 Si 0.6672(3) 0.3585(3) 1.0772(3) 0.0300(11) Uani 1 1 d . . . . . O1 O -0.0411(6) 0.1065(7) 0.5196(5) 0.025(2) Uani 1 1 d . . . . . O2 O -0.0430(6) 0.1096(7) 0.3506(5) 0.028(2) Uani 1 1 d . . . . . O3 O 0.3271(6) 0.0855(5) 0.4873(6) 0.021(2) Uani 1 1 d . . . . . O4 O 0.5300(6) 0.3745(6) 0.8359(5) 0.027(3) Uani 1 1 d . . . . . O5 O 0.5866(7) 0.3807(7) 1.0013(6) 0.028(3) Uani 1 1 d . . . . . O6 O 0.2160(6) 0.4246(5) 1.0002(6) 0.022(2) Uani 1 1 d . . . . . C1 C -0.0083(11) 0.2398(9) 0.4399(10) 0.032(4) Uani 1 1 d . . . . . H1A H 0.012181 0.261998 0.387951 0.048 Uiso 1 1 calc R U . . . H1B H 0.024916 0.262404 0.491597 0.048 Uiso 1 1 calc R U . . . H1C H -0.075133 0.247565 0.440013 0.048 Uiso 1 1 calc R U . . . C2 C -0.2170(11) 0.0406(11) 0.3552(10) 0.047(5) Uani 1 1 d . . . . . H2A H -0.187638 -0.006840 0.368185 0.070 Uiso 1 1 calc R U . . . H2B H -0.277127 0.033489 0.320702 0.070 Uiso 1 1 calc R U . . . H2C H -0.226108 0.065469 0.409395 0.070 Uiso 1 1 calc R U . . . C3 C -0.1205(12) 0.0478(10) 0.1944(10) 0.044(5) Uani 1 1 d . . . . . H3A H -0.093241 0.081817 0.155739 0.066 Uiso 1 1 calc R U . . . H3B H -0.178983 0.028685 0.165296 0.066 Uiso 1 1 calc R U . . . H3C H -0.077406 0.007348 0.209038 0.066 Uiso 1 1 calc R U . . . C4 C -0.1991(14) 0.1838(12) 0.2735(14) 0.069(7) Uani 1 1 d . . . . . H4A H -0.217098 0.203603 0.327747 0.103 Uiso 1 1 calc R U . . . H4B H -0.254414 0.177625 0.231793 0.103 Uiso 1 1 calc R U . . . H4C H -0.155973 0.217432 0.249791 0.103 Uiso 1 1 calc R U . . . C5 C -0.0244(12) 0.1724(12) 0.6866(11) 0.053(6) Uani 1 1 d . . . . . H5A H 0.023843 0.138270 0.710538 0.079 Uiso 1 1 calc R U . . . H5B H -0.061825 0.187266 0.732247 0.079 Uiso 1 1 calc R U . . . H5C H 0.004678 0.215413 0.663791 0.079 Uiso 1 1 calc R U . . . C6 C -0.1453(11) 0.0392(10) 0.6377(11) 0.038(4) Uani 1 1 d . . . . . H6A H -0.179195 0.012931 0.589148 0.057 Uiso 1 1 calc R U . . . H6B H -0.187106 0.049452 0.681556 0.057 Uiso 1 1 calc R U . . . H6C H -0.093332 0.009289 0.663332 0.057 Uiso 1 1 calc R U . . . C7 C -0.2027(11) 0.1894(10) 0.5639(11) 0.042(5) Uani 1 1 d . . . . . H7A H -0.180038 0.237357 0.548164 0.064 Uiso 1 1 calc R U . . . H7B H -0.240318 0.194594 0.612029 0.064 Uiso 1 1 calc R U . . . H7C H -0.240543 0.168127 0.513872 0.064 Uiso 1 1 calc R U . . . C8 C 0.1004(10) -0.0796(9) 0.4625(9) 0.025(4) Uani 1 1 d . . . . . H8 H 0.112145 -0.123276 0.500738 0.030 Uiso 1 1 calc R U . . . C9 C 0.1354(10) -0.0971(11) 0.3761(8) 0.038(4) Uani 1 1 d . . . . . H9A H 0.102804 -0.140012 0.350441 0.057 Uiso 1 1 calc R U . . . H9B H 0.202158 -0.107033 0.385303 0.057 Uiso 1 1 calc R U . . . H9C H 0.123847 -0.055381 0.336903 0.057 Uiso 1 1 calc R U . . . C10 C -0.0051(10) -0.0672(9) 0.4484(10) 0.029(4) Uani 1 1 d . . . . . H10A H -0.019303 -0.028784 0.405012 0.044 Uiso 1 1 calc R U . . . H10B H -0.027071 -0.052303 0.503104 0.044 Uiso 1 1 calc R U . . . H10C H -0.036140 -0.112442 0.428003 0.044 Uiso 1 1 calc R U . . . C11 C 0.1225(10) -0.0068(8) 0.6283(8) 0.025(3) Uani 1 1 d . . . . . H11 H 0.060845 0.018089 0.624287 0.030 Uiso 1 1 calc R U . . . C12 C 0.1875(12) 0.0414(11) 0.6886(10) 0.042(5) Uani 1 1 d . . . . . H12A H 0.165286 0.043429 0.745808 0.063 Uiso 1 1 calc R U . . . H12B H 0.188653 0.090677 0.664448 0.063 Uiso 1 1 calc R U . . . H12C H 0.250270 0.020805 0.694135 0.063 Uiso 1 1 calc R U . . . C13 C 0.1070(13) -0.0800(9) 0.6671(10) 0.043(5) Uani 1 1 d . . . . . H13A H 0.164826 -0.108067 0.671779 0.065 Uiso 1 1 calc R U . . . H13B H 0.058817 -0.106270 0.630122 0.065 Uiso 1 1 calc R U . . . H13C H 0.087173 -0.073582 0.724904 0.065 Uiso 1 1 calc R U . . . C14 C 0.2797(10) -0.0318(9) 0.5343(8) 0.024(4) Uani 1 1 d . . . . . C15 C 0.3058(10) -0.1016(11) 0.5622(8) 0.031(4) Uani 1 1 d . . . . . H15 H 0.259245 -0.136472 0.570968 0.037 Uiso 1 1 calc R U . . . C16 C 0.3976(11) -0.1212(10) 0.5775(9) 0.035(4) Uani 1 1 d . . . . . H16 H 0.414145 -0.168896 0.597413 0.042 Uiso 1 1 calc R U . . . C17 C 0.4660(11) -0.0713(9) 0.5639(9) 0.028(4) Uani 1 1 d . . . . . H17 H 0.529357 -0.085335 0.574050 0.034 Uiso 1 1 calc R U . . . C18 C 0.4437(10) -0.0012(9) 0.5359(8) 0.020(3) Uani 1 1 d . . . . . C19 C 0.3507(11) 0.0172(9) 0.5189(9) 0.026(4) Uani 1 1 d . . . . . C20 C 0.5146(10) 0.0557(10) 0.5240(9) 0.031(4) Uani 1 1 d . . . . . C21 C 0.5227(11) 0.1083(12) 0.6032(10) 0.046(4) Uani 1 1 d . . . . . H21A H 0.460516 0.123664 0.614662 0.069 Uiso 1 1 calc R U . . . H21B H 0.559064 0.151236 0.590588 0.069 Uiso 1 1 calc R U . . . H21C H 0.553457 0.083128 0.654166 0.069 Uiso 1 1 calc R U . . . C22 C 0.6134(11) 0.0251(11) 0.5191(11) 0.043(5) Uani 1 1 d . . . . . H22A H 0.632596 -0.003773 0.571105 0.065 Uiso 1 1 calc R U . . . H22B H 0.656873 0.065535 0.515291 0.065 Uiso 1 1 calc R U . . . H22C H 0.613191 -0.005936 0.467691 0.065 Uiso 1 1 calc R U . . . C23 C 0.4780(10) 0.1021(11) 0.4442(9) 0.031(4) Uani 1 1 d . . . . . C24 C 0.5339(12) 0.1321(10) 0.3869(9) 0.043(5) Uani 1 1 d . . . . . H24 H 0.598847 0.123198 0.394929 0.052 Uiso 1 1 calc R U . . . C25 C 0.4972(11) 0.1742(11) 0.3189(10) 0.043(5) Uani 1 1 d . . . . . H25 H 0.535922 0.191381 0.277793 0.052 Uiso 1 1 calc R U . . . C26 C 0.4046(11) 0.1917(10) 0.3098(9) 0.035(4) Uani 1 1 d . . . . . H26 H 0.380186 0.223495 0.264620 0.042 Uiso 1 1 calc R U . . . C27 C 0.3453(11) 0.1623(9) 0.3676(9) 0.028(4) Uani 1 1 d . . . . . C28 C 0.3843(10) 0.1171(10) 0.4312(8) 0.026(4) Uani 1 1 d . . . . . C29 C 0.1819(11) 0.1880(10) 0.2473(8) 0.036(4) Uani 1 1 d . . . . . H29 H 0.227048 0.217311 0.217613 0.043 Uiso 1 1 calc R U . . . C30 C 0.1818(14) 0.1124(12) 0.2096(10) 0.062(6) Uani 1 1 d . . . . . H30A H 0.135023 0.082600 0.234052 0.093 Uiso 1 1 calc R U . . . H30B H 0.243085 0.090253 0.223689 0.093 Uiso 1 1 calc R U . . . H30C H 0.167063 0.115073 0.146582 0.093 Uiso 1 1 calc R U . . . C31 C 0.0872(12) 0.2252(13) 0.2279(11) 0.060(6) Uani 1 1 d . . . . . H31A H 0.065884 0.220764 0.165944 0.090 Uiso 1 1 calc R U . . . H31B H 0.092842 0.276844 0.243620 0.090 Uiso 1 1 calc R U . . . H31C H 0.042347 0.201674 0.261551 0.090 Uiso 1 1 calc R U . . . C32 C 0.2301(11) 0.2882(9) 0.3902(10) 0.032(4) Uani 1 1 d . . . . . H32 H 0.165102 0.304561 0.395142 0.039 Uiso 1 1 calc R U . . . C33 C 0.2837(14) 0.2989(11) 0.4803(11) 0.053(6) Uani 1 1 d . . . . . H33A H 0.348918 0.285748 0.478454 0.079 Uiso 1 1 calc R U . . . H33B H 0.256881 0.267721 0.522250 0.079 Uiso 1 1 calc R U . . . H33C H 0.279567 0.350044 0.497750 0.079 Uiso 1 1 calc R U . . . C34 C 0.2669(12) 0.3384(9) 0.3262(11) 0.043(5) Uani 1 1 d . . . . . H34A H 0.259568 0.389095 0.344306 0.065 Uiso 1 1 calc R U . . . H34B H 0.232439 0.330947 0.268900 0.065 Uiso 1 1 calc R U . . . H34C H 0.332768 0.328135 0.323426 0.065 Uiso 1 1 calc R U . . . C35 C 0.5175(12) 0.2489(9) 0.9346(11) 0.037(4) Uani 1 1 d . . . . . H35A H 0.478621 0.226238 0.886216 0.056 Uiso 1 1 calc R U . . . H35B H 0.500090 0.229923 0.989427 0.056 Uiso 1 1 calc R U . . . H35C H 0.582826 0.237556 0.930086 0.056 Uiso 1 1 calc R U . . . C36A C 0.550(4) 0.402(4) 0.663(2) 0.10(2) Uiso 0.4 1 d D . P A 1 H36A H 0.499751 0.366545 0.648638 0.149 Uiso 0.4 1 calc R U P A 1 H36B H 0.594241 0.398764 0.620193 0.149 Uiso 0.4 1 calc R U P A 1 H36C H 0.523755 0.451168 0.662806 0.149 Uiso 0.4 1 calc R U P A 1 C37A C 0.704(4) 0.439(4) 0.823(5) 0.10(3) Uiso 0.4 1 d D . P A 1 H37A H 0.684068 0.461365 0.875393 0.152 Uiso 0.4 1 calc R U P A 1 H37B H 0.718110 0.477257 0.782772 0.152 Uiso 0.4 1 calc R U P A 1 H37C H 0.758780 0.408942 0.838846 0.152 Uiso 0.4 1 calc R U P A 1 C38A C 0.666(3) 0.2930(16) 0.761(3) 0.048(12) Uiso 0.4 1 d D . P A 1 H38A H 0.697370 0.278075 0.817408 0.073 Uiso 0.4 1 calc R U P A 1 H38B H 0.712478 0.297367 0.719548 0.073 Uiso 0.4 1 calc R U P A 1 H38C H 0.620045 0.256355 0.739954 0.073 Uiso 0.4 1 calc R U P A 1 C36B C 0.578(2) 0.4542(14) 0.6918(16) 0.045(8) Uiso 0.6 1 d D . P A 2 H36D H 0.511814 0.450549 0.670653 0.067 Uiso 0.6 1 calc R U P A 2 H36E H 0.614789 0.449091 0.643093 0.067 Uiso 0.6 1 calc R U P A 2 H36F H 0.590369 0.501777 0.719424 0.067 Uiso 0.6 1 calc R U P A 2 C37B C 0.7217(16) 0.408(2) 0.830(2) 0.044(9) Uiso 0.6 1 d D . P A 2 H37D H 0.712719 0.450156 0.867319 0.066 Uiso 0.6 1 calc R U P A 2 H37E H 0.764736 0.421574 0.788311 0.066 Uiso 0.6 1 calc R U P A 2 H37F H 0.747349 0.367378 0.865563 0.066 Uiso 0.6 1 calc R U P A 2 C38B C 0.628(3) 0.2957(14) 0.716(2) 0.073(12) Uiso 0.6 1 d D . P A 2 H38D H 0.656456 0.260292 0.758117 0.110 Uiso 0.6 1 calc R U P A 2 H38E H 0.668391 0.304063 0.670975 0.110 Uiso 0.6 1 calc R U P A 2 H38F H 0.567878 0.276672 0.689792 0.110 Uiso 0.6 1 calc R U P A 2 C39 C 0.7502(11) 0.2903(10) 1.0413(10) 0.039(5) Uani 1 1 d . . . . . H39A H 0.716006 0.247087 1.018418 0.059 Uiso 1 1 calc R U . . . H39B H 0.794718 0.276187 1.090702 0.059 Uiso 1 1 calc R U . . . H39C H 0.783498 0.311695 0.996024 0.059 Uiso 1 1 calc R U . . . C40 C 0.6162(11) 0.3197(10) 1.1720(10) 0.040(4) Uani 1 1 d . . . . . H40A H 0.583327 0.358121 1.199992 0.060 Uiso 1 1 calc R U . . . H40B H 0.665783 0.299839 1.213430 0.060 Uiso 1 1 calc R U . . . H40C H 0.572599 0.280706 1.152395 0.060 Uiso 1 1 calc R U . . . C41 C 0.7309(13) 0.4443(11) 1.1076(12) 0.052(6) Uani 1 1 d . . . . . H41A H 0.749868 0.467334 1.055519 0.078 Uiso 1 1 calc R U . . . H41B H 0.786023 0.433193 1.147972 0.078 Uiso 1 1 calc R U . . . H41C H 0.690445 0.477521 1.135404 0.078 Uiso 1 1 calc R U . . . C42 C 0.4510(10) 0.5700(9) 0.9684(9) 0.026(4) Uani 1 1 d . . . . . H42 H 0.459000 0.611693 1.009969 0.031 Uiso 1 1 calc R U . . . C43 C 0.3855(10) 0.5958(9) 0.8902(8) 0.031(4) Uani 1 1 d . . . . . H43A H 0.416072 0.633858 0.859467 0.046 Uiso 1 1 calc R U . . . H43B H 0.328747 0.615389 0.909984 0.046 Uiso 1 1 calc R U . . . H43C H 0.369895 0.554562 0.851118 0.046 Uiso 1 1 calc R U . . . C44 C 0.5464(11) 0.5520(10) 0.9427(10) 0.032(4) Uani 1 1 d . . . . . H44A H 0.541076 0.512575 0.899878 0.049 Uiso 1 1 calc R U . . . H44B H 0.587242 0.536593 0.994010 0.049 Uiso 1 1 calc R U . . . H44C H 0.572514 0.595370 0.917576 0.049 Uiso 1 1 calc R U . . . C45 C 0.4719(11) 0.4891(8) 1.1319(8) 0.027(4) Uani 1 1 d . . . . . H45 H 0.523806 0.454652 1.124073 0.032 Uiso 1 1 calc R U . . . C46 C 0.5180(11) 0.5587(9) 1.1687(10) 0.035(4) Uani 1 1 d . . . . . H46A H 0.470372 0.592564 1.184438 0.053 Uiso 1 1 calc R U . . . H46B H 0.552538 0.581412 1.125118 0.053 Uiso 1 1 calc R U . . . H46C H 0.560673 0.546986 1.220306 0.053 Uiso 1 1 calc R U . . . C47 C 0.4171(10) 0.4535(9) 1.1979(8) 0.026(4) Uani 1 1 d . . . . . H47A H 0.459745 0.429337 1.242316 0.040 Uiso 1 1 calc R U . . . H47B H 0.374441 0.417383 1.168949 0.040 Uiso 1 1 calc R U . . . H47C H 0.381529 0.490778 1.225007 0.040 Uiso 1 1 calc R U . . . C48 C 0.2910(11) 0.5331(9) 1.0513(9) 0.027(4) Uani 1 1 d . . . . . C49 C 0.2860(11) 0.6006(10) 1.0877(9) 0.035(4) Uani 1 1 d . . . . . H49 H 0.340940 0.628651 1.099931 0.041 Uiso 1 1 calc R U . . . C50 C 0.2022(12) 0.6289(10) 1.1071(11) 0.044(5) Uani 1 1 d . . . . . H50 H 0.199853 0.676440 1.131031 0.053 Uiso 1 1 calc R U . . . C51 C 0.1243(12) 0.5891(10) 1.0919(9) 0.038(5) Uani 1 1 d . . . . . H51 H 0.067297 0.608833 1.105849 0.045 Uiso 1 1 calc R U . . . C52 C 0.1257(11) 0.5193(9) 1.0561(9) 0.028(4) Uani 1 1 d . . . . . C53 C 0.2087(11) 0.4946(9) 1.0352(9) 0.024(4) Uani 1 1 d . . . . . C54 C 0.0382(10) 0.4726(9) 1.0394(9) 0.036(4) Uani 1 1 d D . . . . C55A C -0.043(2) 0.5258(19) 0.997(2) 0.036(9) Uiso 0.5 1 d D . P B 1 H55A H -0.026157 0.545477 0.941926 0.055 Uiso 0.5 1 calc R U P B 1 H55B H -0.051957 0.565976 1.036404 0.055 Uiso 0.5 1 calc R U P B 1 H55C H -0.101231 0.498136 0.985321 0.055 Uiso 0.5 1 calc R U P B 1 C56A C 0.007(3) 0.441(2) 1.1267(18) 0.049(11) Uiso 0.5 1 d D . P B 1 H56A H -0.031081 0.396922 1.113620 0.073 Uiso 0.5 1 calc R U P B 1 H56B H -0.029357 0.477295 1.153870 0.073 Uiso 0.5 1 calc R U P B 1 H56C H 0.061955 0.427730 1.166255 0.073 Uiso 0.5 1 calc R U P B 1 C55B C -0.060(2) 0.512(3) 1.039(3) 0.071(14) Uiso 0.5 1 d D . P B 2 H55D H -0.075056 0.537625 0.984248 0.106 Uiso 0.5 1 calc R U P B 2 H55E H -0.056207 0.547454 1.087061 0.106 Uiso 0.5 1 calc R U P B 2 H55F H -0.107459 0.475827 1.047032 0.106 Uiso 0.5 1 calc R U P B 2 C56B C 0.049(3) 0.4224(18) 1.1259(16) 0.032(8) Uiso 0.5 1 d D . P B 2 H56D H 0.004537 0.381887 1.118507 0.047 Uiso 0.5 1 calc R U P B 2 H56E H 0.036048 0.451963 1.175786 0.047 Uiso 0.5 1 calc R U P B 2 H56F H 0.112031 0.403078 1.135757 0.047 Uiso 0.5 1 calc R U P B 2 C57 C 0.0487(11) 0.4160(9) 0.9722(9) 0.029(4) Uani 1 1 d . . . C 3 C58 C -0.0281(13) 0.3850(14) 0.9239(13) 0.064(6) Uani 1 1 d . . . C 3 H58 H -0.088334 0.403316 0.929855 0.077 Uiso 1 1 calc R U . C 3 C59 C -0.0183(16) 0.3290(14) 0.8683(17) 0.088(9) Uani 1 1 d . . . C 3 H59 H -0.071435 0.305486 0.839461 0.106 Uiso 1 1 calc R U . C 3 C60 C 0.0722(12) 0.3059(11) 0.8538(12) 0.049(5) Uani 1 1 d . . . C 3 H60 H 0.079102 0.269403 0.811546 0.059 Uiso 1 1 calc R U . C 3 C61 C 0.1495(11) 0.3352(9) 0.8996(9) 0.032(4) Uani 1 1 d . . . C 3 C62 C 0.1358(10) 0.3910(11) 0.9563(8) 0.027(3) Uani 1 1 d . . . C 3 C63 C 0.2704(13) 0.2107(10) 0.9346(11) 0.042(5) Uani 1 1 d . . . D 3 H63 H 0.335976 0.193574 0.936151 0.051 Uiso 1 1 calc R U . D 3 C64 C 0.2508(13) 0.2153(11) 1.0290(11) 0.052(5) Uani 1 1 d . . . D 3 H64A H 0.184785 0.225547 1.031222 0.077 Uiso 1 1 calc R U . D 3 H64B H 0.288029 0.254532 1.058264 0.077 Uiso 1 1 calc R U . D 3 H64C H 0.266907 0.168883 1.058019 0.077 Uiso 1 1 calc R U . D 3 C65 C 0.2115(15) 0.1522(11) 0.8880(13) 0.069(7) Uani 1 1 d . . . D 3 H65A H 0.199632 0.113617 0.929024 0.103 Uiso 1 1 calc R U . D 3 H65B H 0.244031 0.131533 0.841716 0.103 Uiso 1 1 calc R U . D 3 H65C H 0.152376 0.173229 0.862933 0.103 Uiso 1 1 calc R U . D 3 C66 C 0.2588(11) 0.2861(11) 0.7684(8) 0.037(5) Uani 1 1 d . . . E 3 H66 H 0.205051 0.252741 0.752516 0.044 Uiso 1 1 calc R U . E 3 C67 C 0.2410(15) 0.3554(11) 0.7200(10) 0.062(7) Uani 1 1 d . . . E 3 H67A H 0.287967 0.391501 0.741205 0.092 Uiso 1 1 calc R U . E 3 H67B H 0.179280 0.373776 0.728809 0.092 Uiso 1 1 calc R U . E 3 H67C H 0.243874 0.346749 0.658179 0.092 Uiso 1 1 calc R U . E 3 C68 C 0.3458(12) 0.2490(10) 0.7446(10) 0.043(5) Uani 1 1 d . . . E 3 H68A H 0.337198 0.235420 0.683215 0.065 Uiso 1 1 calc R U . E 3 H68B H 0.357937 0.205078 0.780024 0.065 Uiso 1 1 calc R U . E 3 H68C H 0.398522 0.282452 0.755164 0.065 Uiso 1 1 calc R U . E 3 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 0.0166(3) 0.0250(4) 0.0186(3) 0.0021(3) 0.0008(2) -0.0005(3) Ir2 0.0166(3) 0.0235(4) 0.0186(3) -0.0007(3) -0.0005(2) -0.0020(3) P1 0.015(2) 0.025(2) 0.0185(17) 0.0027(16) 0.0005(14) -0.0011(17) P2 0.026(2) 0.027(3) 0.0189(18) 0.0029(16) 0.0031(16) -0.0019(19) P3 0.019(2) 0.024(2) 0.0211(18) 0.0002(16) 0.0004(15) -0.0006(18) P4 0.019(2) 0.027(3) 0.0243(19) -0.0058(17) -0.0015(16) -0.0040(18) Si1 0.019(2) 0.025(3) 0.026(2) 0.0018(18) 0.0009(17) 0.0018(19) Si2 0.023(2) 0.036(3) 0.026(2) -0.0052(19) 0.0030(18) -0.002(2) Si3 0.022(2) 0.042(3) 0.028(2) -0.004(2) -0.0070(16) 0.008(2) Si4 0.019(2) 0.023(3) 0.027(2) 0.0025(19) 0.0016(17) -0.0001(19) Si5 0.042(3) 0.048(4) 0.035(2) 0.005(3) 0.019(2) 0.015(3) Si6 0.021(2) 0.037(3) 0.030(2) 0.003(2) -0.0042(18) 0.000(2) O1 0.021(5) 0.028(6) 0.027(5) -0.004(6) 0.003(4) -0.005(6) O2 0.018(5) 0.037(6) 0.026(5) 0.000(6) -0.008(4) -0.004(6) O3 0.014(5) 0.023(7) 0.027(5) 0.004(4) 0.002(4) 0.003(4) O4 0.022(5) 0.034(8) 0.026(5) -0.004(5) 0.000(4) 0.002(5) O5 0.022(5) 0.029(7) 0.032(5) -0.004(5) 0.000(4) -0.005(5) O6 0.016(5) 0.026(6) 0.025(5) -0.010(4) 0.007(4) -0.006(5) C1 0.022(9) 0.030(11) 0.044(9) 0.006(8) 0.000(7) 0.002(8) C2 0.024(10) 0.085(16) 0.030(9) -0.023(9) -0.001(7) 0.000(10) C3 0.031(10) 0.056(13) 0.042(10) -0.004(9) -0.008(8) 0.001(9) C4 0.058(15) 0.053(15) 0.086(15) -0.011(12) -0.028(12) 0.016(12) C5 0.032(11) 0.070(16) 0.054(11) -0.014(11) -0.010(8) -0.011(10) C6 0.028(10) 0.040(12) 0.045(10) 0.008(8) 0.002(8) 0.001(8) C7 0.024(10) 0.044(13) 0.064(12) -0.016(10) 0.026(8) -0.001(9) C8 0.018(8) 0.030(10) 0.028(8) 0.005(7) 0.002(6) 0.002(7) C9 0.028(9) 0.054(13) 0.032(8) -0.001(8) 0.000(6) 0.003(9) C10 0.022(9) 0.024(10) 0.039(9) 0.002(7) -0.006(7) 0.004(8) C11 0.021(8) 0.029(10) 0.027(7) 0.012(7) 0.008(6) 0.005(7) C12 0.042(11) 0.053(13) 0.031(9) -0.016(8) 0.002(8) -0.014(10) C13 0.054(12) 0.039(12) 0.037(9) 0.015(8) 0.006(8) -0.008(9) C14 0.014(8) 0.041(11) 0.016(7) 0.007(7) 0.003(6) 0.003(7) C15 0.024(8) 0.044(11) 0.023(7) 0.006(8) 0.001(6) -0.007(9) C16 0.030(9) 0.030(12) 0.044(8) 0.007(8) 0.000(7) 0.016(8) C17 0.020(8) 0.035(11) 0.028(8) 0.004(7) 0.002(6) -0.002(8) C18 0.016(8) 0.028(10) 0.014(6) 0.002(6) 0.000(5) 0.001(7) C19 0.022(9) 0.022(10) 0.034(8) 0.003(7) 0.004(7) 0.000(7) C20 0.018(8) 0.047(12) 0.028(8) -0.003(7) 0.000(6) 0.005(8) C21 0.028(9) 0.060(13) 0.052(10) -0.017(12) 0.012(7) -0.010(12) C22 0.022(10) 0.055(14) 0.054(11) 0.005(10) 0.010(8) 0.005(9) C23 0.021(8) 0.040(11) 0.030(7) 0.012(9) -0.005(6) 0.000(9) C24 0.032(10) 0.073(16) 0.024(8) 0.009(8) 0.010(7) -0.006(9) C25 0.028(10) 0.075(15) 0.031(9) 0.002(9) 0.020(7) -0.007(10) C26 0.032(10) 0.045(12) 0.029(8) 0.003(8) 0.010(7) 0.011(9) C27 0.036(10) 0.023(10) 0.029(8) -0.006(7) 0.024(7) -0.003(8) C28 0.026(8) 0.042(11) 0.010(6) -0.002(7) 0.008(5) -0.007(8) C29 0.041(10) 0.055(13) 0.010(6) 0.010(7) 0.000(6) -0.020(9) C30 0.100(16) 0.048(13) 0.039(9) -0.011(11) 0.012(9) -0.042(14) C31 0.030(11) 0.099(19) 0.046(11) 0.022(11) -0.016(8) -0.019(11) C32 0.028(9) 0.034(11) 0.036(9) 0.004(8) 0.010(7) -0.001(8) C33 0.067(15) 0.045(14) 0.049(11) -0.019(10) 0.018(10) -0.014(11) C34 0.034(10) 0.025(11) 0.070(12) 0.008(9) 0.006(9) -0.003(8) C35 0.033(10) 0.029(11) 0.046(10) 0.004(8) -0.006(8) -0.001(8) C39 0.033(10) 0.055(13) 0.029(8) -0.007(8) 0.003(7) -0.009(9) C40 0.033(10) 0.043(12) 0.047(10) 0.023(9) 0.020(8) 0.014(9) C41 0.032(11) 0.063(15) 0.055(12) -0.006(11) -0.021(9) -0.012(10) C42 0.023(9) 0.036(10) 0.018(7) -0.005(7) 0.006(6) 0.000(7) C43 0.035(9) 0.028(11) 0.028(7) 0.002(7) -0.007(6) -0.001(8) C44 0.025(9) 0.036(11) 0.038(9) 0.011(8) 0.011(7) -0.002(8) C45 0.037(10) 0.024(9) 0.019(7) -0.003(6) -0.003(6) -0.004(8) C46 0.036(10) 0.035(11) 0.032(8) -0.005(8) -0.010(7) 0.006(8) C47 0.023(9) 0.037(11) 0.019(7) 0.005(7) 0.001(6) -0.008(8) C48 0.027(9) 0.022(10) 0.029(8) -0.003(7) -0.006(7) 0.004(8) C49 0.045(10) 0.025(10) 0.035(8) -0.009(8) 0.013(7) -0.007(9) C50 0.037(11) 0.028(12) 0.067(12) -0.015(9) 0.005(9) -0.002(8) C51 0.031(10) 0.045(14) 0.038(9) -0.006(8) 0.011(7) 0.012(9) C52 0.022(9) 0.033(11) 0.031(8) -0.003(7) 0.011(7) -0.003(8) C53 0.028(9) 0.024(10) 0.021(7) 0.003(7) 0.010(6) -0.001(8) C54 0.016(8) 0.052(13) 0.041(9) -0.020(9) 0.009(7) -0.012(8) C57 0.018(8) 0.043(12) 0.029(8) -0.008(7) 0.006(6) 0.007(7) C58 0.040(12) 0.054(15) 0.098(15) -0.016(15) 0.006(10) 0.026(13) C59 0.051(15) 0.068(18) 0.14(2) -0.060(17) -0.025(14) -0.002(13) C60 0.021(10) 0.056(14) 0.066(12) -0.036(10) -0.012(8) 0.003(9) C61 0.032(10) 0.034(11) 0.029(8) -0.006(8) 0.005(7) -0.009(8) C62 0.034(9) 0.023(9) 0.023(7) 0.003(8) 0.003(6) -0.004(9) C63 0.043(12) 0.035(12) 0.050(11) 0.000(9) 0.010(9) -0.015(9) C64 0.055(13) 0.046(13) 0.055(12) 0.016(10) 0.013(10) -0.013(11) C65 0.079(17) 0.040(14) 0.085(15) -0.004(12) 0.002(12) -0.035(12) C66 0.028(9) 0.068(14) 0.013(7) -0.012(8) -0.004(6) 0.008(9) C67 0.081(16) 0.073(16) 0.024(8) -0.010(9) -0.024(9) 0.023(12) C68 0.040(11) 0.055(13) 0.032(9) -0.012(8) -0.008(8) -0.006(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 P1 2.252(4) . ? Ir1 Si1 2.262(4) . ? Ir1 P2 2.263(4) . ? Ir1 O3 2.339(9) . ? Ir1 H01 1.590(14) . ? Ir1 H02 1.593(14) . ? Ir2 P3 2.245(4) . ? Ir2 P4 2.262(4) . ? Ir2 Si4 2.271(4) . ? Ir2 O6 2.324(9) . ? Ir2 H03 1.588(14) . ? Ir2 H04 1.5845 . ? P1 C8 1.832(16) . ? P1 C11 1.836(13) . ? P1 C14 1.841(14) . ? P2 C29 1.828(13) . ? P2 C27 1.846(16) . ? P2 C32 1.853(17) . ? P3 C42 1.822(16) . ? P3 C48 1.845(16) . ? P3 C45 1.855(13) . ? P4 C63 1.841(19) . ? P4 C61 1.849(17) . ? P4 C66 1.862(13) . ? Si1 O2 1.650(9) . ? Si1 O1 1.678(10) . ? Si1 C1 1.881(17) . ? Si2 O1 1.607(9) . ? Si2 C5 1.857(16) . ? Si2 C6 1.874(17) . ? Si2 C7 1.904(18) . ? Si3 O2 1.625(9) . ? Si3 C2 1.817(18) . ? Si3 C4 1.82(2) . ? Si3 C3 1.847(17) . ? Si4 O4 1.639(10) . ? Si4 O5 1.661(10) . ? Si4 C35 1.886(18) . ? Si5 O4 1.615(10) . ? Si5 C38B 1.823(18) . ? Si5 C38A 1.837(19) . ? Si5 C36A 1.838(19) . ? Si5 C36B 1.839(17) . ? Si5 C37A 1.842(19) . ? Si5 C37B 1.846(17) . ? Si6 O5 1.617(10) . ? Si6 C41 1.859(19) . ? Si6 C40 1.862(15) . ? Si6 C39 1.864(17) . ? O3 C19 1.375(17) . ? O3 C28 1.394(16) . ? O6 C53 1.403(18) . ? O6 C62 1.422(17) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.522(18) . ? C8 C10 1.538(19) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.50(2) . ? C11 C12 1.53(2) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.39(2) . ? C14 C19 1.41(2) . ? C15 C16 1.37(2) . ? C15 H15 0.9500 . ? C16 C17 1.38(2) . ? C16 H16 0.9500 . ? C17 C18 1.38(2) . ? C17 H17 0.9500 . ? C18 C19 1.387(19) . ? C18 C20 1.49(2) . ? C20 C23 1.55(2) . ? C20 C22 1.55(2) . ? C20 C21 1.56(2) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C28 1.380(19) . ? C23 C24 1.38(2) . ? C24 C25 1.37(2) . ? C24 H24 0.9500 . ? C25 C26 1.37(2) . ? C25 H25 0.9500 . ? C26 C27 1.42(2) . ? C26 H26 0.9500 . ? C27 C28 1.36(2) . ? C29 C30 1.50(3) . ? C29 C31 1.53(2) . ? C29 H29 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C34 1.50(2) . ? C32 C33 1.54(2) . ? C32 H32 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36A H36A 0.9800 . ? C36A H36B 0.9800 . ? C36A H36C 0.9800 . ? C37A H37A 0.9800 . ? C37A H37B 0.9800 . ? C37A H37C 0.9800 . ? C38A H38A 0.9800 . ? C38A H38B 0.9800 . ? C38A H38C 0.9800 . ? C36B H36D 0.9800 . ? C36B H36E 0.9800 . ? C36B H36F 0.9800 . ? C37B H37D 0.9800 . ? C37B H37E 0.9800 . ? C37B H37F 0.9800 . ? C38B H38D 0.9800 . ? C38B H38E 0.9800 . ? C38B H38F 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C44 1.52(2) . ? C42 C43 1.530(18) . ? C42 H42 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C47 1.515(19) . ? C45 C46 1.52(2) . ? C45 H45 1.0000 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.37(2) . ? C48 C53 1.39(2) . ? C49 C50 1.39(2) . ? C49 H49 0.9500 . ? C50 C51 1.34(2) . ? C50 H50 0.9500 . ? C51 C52 1.40(2) . ? C51 H51 0.9500 . ? C52 C53 1.36(2) . ? C52 C54 1.53(2) . ? C54 C57 1.49(2) . ? C54 C56A 1.59(2) . ? C54 C55B 1.59(2) . ? C54 C55A 1.62(2) . ? C54 C56B 1.62(2) . ? C55A H55A 0.9800 . ? C55A H55B 0.9800 . ? C55A H55C 0.9800 . ? C56A H56A 0.9800 . ? C56A H56B 0.9800 . ? C56A H56C 0.9800 . ? C55B H55D 0.9800 . ? C55B H55E 0.9800 . ? C55B H55F 0.9800 . ? C56B H56D 0.9800 . ? C56B H56E 0.9800 . ? C56B H56F 0.9800 . ? C57 C62 1.39(2) . ? C57 C58 1.39(2) . ? C58 C59 1.36(3) . ? C58 H58 0.9500 . ? C59 C60 1.42(3) . ? C59 H59 0.9500 . ? C60 C61 1.37(2) . ? C60 H60 0.9500 . ? C61 C62 1.38(2) . ? C63 C65 1.51(2) . ? C63 C64 1.53(2) . ? C63 H63 1.0000 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C67 1.48(2) . ? C66 C68 1.52(2) . ? C66 H66 1.0000 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? 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 P1 Ir1 Si1 98.91(15) . . ? P1 Ir1 P2 156.83(15) . . ? Si1 Ir1 P2 100.05(15) . . ? P1 Ir1 O3 82.0(3) . . ? Si1 Ir1 O3 170.4(3) . . ? P2 Ir1 O3 81.5(3) . . ? P1 Ir1 H01 83(5) . . ? Si1 Ir1 H01 100(5) . . ? P2 Ir1 H01 81(5) . . ? O3 Ir1 H01 90(5) . . ? P1 Ir1 H02 99(5) . . ? Si1 Ir1 H02 86(5) . . ? P2 Ir1 H02 95(5) . . ? O3 Ir1 H02 84(5) . . ? H01 Ir1 H02 173(7) . . ? P3 Ir2 P4 161.33(14) . . ? P3 Ir2 Si4 98.00(15) . . ? P4 Ir2 Si4 100.18(16) . . ? P3 Ir2 O6 81.1(3) . . ? P4 Ir2 O6 81.4(3) . . ? Si4 Ir2 O6 172.8(3) . . ? P3 Ir2 H03 103(5) . . ? P4 Ir2 H03 84(5) . . ? Si4 Ir2 H03 81(5) . . ? O6 Ir2 H03 92(5) . . ? P3 Ir2 H04 85.9 . . ? P4 Ir2 H04 85.4 . . ? Si4 Ir2 H04 104.7 . . ? O6 Ir2 H04 82.4 . . ? H03 Ir2 H04 169.1 . . ? C8 P1 C11 103.9(7) . . ? C8 P1 C14 101.8(7) . . ? C11 P1 C14 103.2(6) . . ? C8 P1 Ir1 121.7(5) . . ? C11 P1 Ir1 120.6(5) . . ? C14 P1 Ir1 102.4(5) . . ? C29 P2 C27 103.6(7) . . ? C29 P2 C32 104.3(8) . . ? C27 P2 C32 103.1(7) . . ? C29 P2 Ir1 119.9(6) . . ? C27 P2 Ir1 101.2(5) . . ? C32 P2 Ir1 121.9(5) . . ? C42 P3 C48 102.6(7) . . ? C42 P3 C45 105.6(7) . . ? C48 P3 C45 102.9(7) . . ? C42 P3 Ir2 121.7(5) . . ? C48 P3 Ir2 102.9(5) . . ? C45 P3 Ir2 118.3(5) . . ? C63 P4 C61 103.3(8) . . ? C63 P4 C66 103.9(8) . . ? C61 P4 C66 101.1(7) . . ? C63 P4 Ir2 118.5(6) . . ? C61 P4 Ir2 102.4(5) . . ? C66 P4 Ir2 124.2(6) . . ? O2 Si1 O1 104.1(5) . . ? O2 Si1 C1 103.7(7) . . ? O1 Si1 C1 103.9(7) . . ? O2 Si1 Ir1 113.6(4) . . ? O1 Si1 Ir1 114.0(4) . . ? C1 Si1 Ir1 116.2(5) . . ? O1 Si2 C5 110.4(7) . . ? O1 Si2 C6 106.5(7) . . ? C5 Si2 C6 109.8(8) . . ? O1 Si2 C7 113.4(7) . . ? C5 Si2 C7 108.4(9) . . ? C6 Si2 C7 108.3(8) . . ? O2 Si3 C2 110.6(6) . . ? O2 Si3 C4 108.2(8) . . ? C2 Si3 C4 107.9(10) . . ? O2 Si3 C3 107.2(6) . . ? C2 Si3 C3 110.0(8) . . ? C4 Si3 C3 113.0(9) . . ? O4 Si4 O5 104.6(5) . . ? O4 Si4 C35 104.1(7) . . ? O5 Si4 C35 102.7(7) . . ? O4 Si4 Ir2 114.2(4) . . ? O5 Si4 Ir2 114.3(4) . . ? C35 Si4 Ir2 115.5(6) . . ? O4 Si5 C38B 112.1(14) . . ? O4 Si5 C38A 110.2(16) . . ? O4 Si5 C36A 107(2) . . ? C38A Si5 C36A 106(3) . . ? O4 Si5 C36B 109.6(11) . . ? C38B Si5 C36B 110.5(16) . . ? O4 Si5 C37A 109(3) . . ? C38A Si5 C37A 103(3) . . ? C36A Si5 C37A 122(3) . . ? O4 Si5 C37B 111.4(11) . . ? C38B Si5 C37B 107.1(17) . . ? C36B Si5 C37B 106.0(16) . . ? O5 Si6 C41 105.6(8) . . ? O5 Si6 C40 110.7(7) . . ? C41 Si6 C40 110.7(9) . . ? O5 Si6 C39 112.9(7) . . ? C41 Si6 C39 108.9(9) . . ? C40 Si6 C39 108.0(8) . . ? Si2 O1 Si1 145.5(8) . . ? Si3 O2 Si1 149.1(7) . . ? C19 O3 C28 117.4(12) . . ? C19 O3 Ir1 115.8(8) . . ? C28 O3 Ir1 115.3(8) . . ? Si5 O4 Si4 149.1(7) . . ? Si6 O5 Si4 145.8(8) . . ? C53 O6 C62 119.3(12) . . ? C53 O6 Ir2 118.0(8) . . ? C62 O6 Ir2 116.5(8) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si3 C2 H2A 109.5 . . ? Si3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si3 C3 H3A 109.5 . . ? Si3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si3 C4 H4A 109.5 . . ? Si3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C10 109.4(11) . . ? C9 C8 P1 113.9(11) . . ? C10 C8 P1 110.2(11) . . ? C9 C8 H8 107.7 . . ? C10 C8 H8 107.7 . . ? P1 C8 H8 107.7 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C12 112.4(13) . . ? C13 C11 P1 119.4(11) . . ? C12 C11 P1 108.5(10) . . ? C13 C11 H11 105.1 . . ? C12 C11 H11 105.1 . . ? P1 C11 H11 105.1 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 117.6(13) . . ? C15 C14 P1 122.8(12) . . ? C19 C14 P1 119.6(12) . . ? C16 C15 C14 121.2(16) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 120.0(17) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 121.1(14) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 118.3(14) . . ? C17 C18 C20 123.3(14) . . ? C19 C18 C20 118.4(14) . . ? O3 C19 C18 119.2(14) . . ? O3 C19 C14 119.0(13) . . ? C18 C19 C14 121.8(15) . . ? C18 C20 C23 107.7(12) . . ? C18 C20 C22 114.0(15) . . ? C23 C20 C22 113.3(13) . . ? C18 C20 C21 109.1(12) . . ? C23 C20 C21 106.3(15) . . ? C22 C20 C21 106.1(12) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C28 C23 C24 117.8(14) . . ? C28 C23 C20 118.1(13) . . ? C24 C23 C20 124.1(14) . . ? C25 C24 C23 121.1(16) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 120.2(15) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C27 120.2(15) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C28 C27 C26 117.3(14) . . ? C28 C27 P2 120.9(11) . . ? C26 C27 P2 121.6(12) . . ? C27 C28 C23 123.2(14) . . ? C27 C28 O3 118.6(13) . . ? C23 C28 O3 118.1(14) . . ? C30 C29 C31 111.8(15) . . ? C30 C29 P2 112.8(12) . . ? C31 C29 P2 111.5(12) . . ? C30 C29 H29 106.8 . . ? C31 C29 H29 106.8 . . ? P2 C29 H29 106.8 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C34 C32 C33 110.2(14) . . ? C34 C32 P2 117.6(11) . . ? C33 C32 P2 110.0(12) . . ? C34 C32 H32 106.1 . . ? C33 C32 H32 106.1 . . ? P2 C32 H32 106.1 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si4 C35 H35A 109.5 . . ? Si4 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si4 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si5 C36A H36A 109.5 . . ? Si5 C36A H36B 109.5 . . ? H36A C36A H36B 109.5 . . ? Si5 C36A H36C 109.5 . . ? H36A C36A H36C 109.5 . . ? H36B C36A H36C 109.5 . . ? Si5 C37A H37A 109.5 . . ? Si5 C37A H37B 109.5 . . ? H37A C37A H37B 109.5 . . ? Si5 C37A H37C 109.5 . . ? H37A C37A H37C 109.5 . . ? H37B C37A H37C 109.5 . . ? Si5 C38A H38A 109.5 . . ? Si5 C38A H38B 109.5 . . ? H38A C38A H38B 109.5 . . ? Si5 C38A H38C 109.5 . . ? H38A C38A H38C 109.5 . . ? H38B C38A H38C 109.5 . . ? Si5 C36B H36D 109.5 . . ? Si5 C36B H36E 109.5 . . ? H36D C36B H36E 109.5 . . ? Si5 C36B H36F 109.5 . . ? H36D C36B H36F 109.5 . . ? H36E C36B H36F 109.5 . . ? Si5 C37B H37D 109.5 . . ? Si5 C37B H37E 109.5 . . ? H37D C37B H37E 109.5 . . ? Si5 C37B H37F 109.5 . . ? H37D C37B H37F 109.5 . . ? H37E C37B H37F 109.5 . . ? Si5 C38B H38D 109.5 . . ? Si5 C38B H38E 109.5 . . ? H38D C38B H38E 109.5 . . ? Si5 C38B H38F 109.5 . . ? H38D C38B H38F 109.5 . . ? H38E C38B H38F 109.5 . . ? Si6 C39 H39A 109.5 . . ? Si6 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si6 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si6 C40 H40A 109.5 . . ? Si6 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si6 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si6 C41 H41A 109.5 . . ? Si6 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si6 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C44 C42 C43 111.1(12) . . ? C44 C42 P3 112.4(11) . . ? C43 C42 P3 111.9(11) . . ? C44 C42 H42 107.0 . . ? C43 C42 H42 107.0 . . ? P3 C42 H42 107.0 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C47 C45 C46 110.4(12) . . ? C47 C45 P3 110.8(10) . . ? C46 C45 P3 117.6(11) . . ? C47 C45 H45 105.7 . . ? C46 C45 H45 105.7 . . ? P3 C45 H45 105.7 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C49 C48 C53 116.8(15) . . ? C49 C48 P3 121.9(13) . . ? C53 C48 P3 121.3(12) . . ? C48 C49 C50 121.2(16) . . ? C48 C49 H49 119.4 . . ? C50 C49 H49 119.4 . . ? C51 C50 C49 120.0(16) . . ? C51 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C50 C51 C52 121.2(15) . . ? C50 C51 H51 119.4 . . ? C52 C51 H51 119.4 . . ? C53 C52 C51 117.0(15) . . ? C53 C52 C54 120.9(15) . . ? C51 C52 C54 122.2(14) . . ? C52 C53 C48 123.8(15) . . ? C52 C53 O6 120.4(14) . . ? C48 C53 O6 115.8(13) . . ? C57 C54 C52 111.1(13) . . ? C52 C54 C56A 112.0(18) . . ? C52 C54 C55B 118(2) . . ? C52 C54 C55A 106.6(18) . . ? C56A C54 C55A 108(2) . . ? C52 C54 C56B 100.3(16) . . ? C55B C54 C56B 105(2) . . ? C54 C55A H55A 109.5 . . ? C54 C55A H55B 109.5 . . ? H55A C55A H55B 109.5 . . ? C54 C55A H55C 109.5 . . ? H55A C55A H55C 109.5 . . ? H55B C55A H55C 109.5 . . ? C54 C56A H56A 109.5 . . ? C54 C56A H56B 109.5 . . ? H56A C56A H56B 109.5 . . ? C54 C56A H56C 109.5 . . ? H56A C56A H56C 109.5 . . ? H56B C56A H56C 109.5 . . ? C54 C55B H55D 109.5 . . ? C54 C55B H55E 109.5 . . ? H55D C55B H55E 109.5 . . ? C54 C55B H55F 109.5 . . ? H55D C55B H55F 109.5 . . ? H55E C55B H55F 109.5 . . ? C54 C56B H56D 109.5 . . ? C54 C56B H56E 109.5 . . ? H56D C56B H56E 109.5 . . ? C54 C56B H56F 109.5 . . ? H56D C56B H56F 109.5 . . ? H56E C56B H56F 109.5 . . ? C62 C57 C58 117.2(15) . . ? C62 C57 C54 121.3(14) . . ? C58 C57 C54 121.5(15) . . ? C59 C58 C57 121.0(18) . . ? C59 C58 H58 119.5 . . ? C57 C58 H58 119.5 . . ? C58 C59 C60 119.4(19) . . ? C58 C59 H59 120.3 . . ? C60 C59 H59 120.3 . . ? C61 C60 C59 121.2(17) . . ? C61 C60 H60 119.4 . . ? C59 C60 H60 119.4 . . ? C60 C61 C62 117.0(15) . . ? C60 C61 P4 122.5(13) . . ? C62 C61 P4 120.5(11) . . ? C61 C62 C57 123.9(14) . . ? C61 C62 O6 117.3(14) . . ? C57 C62 O6 118.8(15) . . ? C65 C63 C64 110.1(16) . . ? C65 C63 P4 118.6(13) . . ? C64 C63 P4 109.6(13) . . ? C65 C63 H63 105.9 . . ? C64 C63 H63 105.9 . . ? P4 C63 H63 105.9 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C67 C66 C68 111.3(15) . . ? C67 C66 P4 110.5(12) . . ? C68 C66 P4 110.4(10) . . ? C67 C66 H66 108.2 . . ? C68 C66 H66 108.2 . . ? P4 C66 H66 108.2 . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C66 C68 H68A 109.5 . . ? C66 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C66 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? _refine_diff_density_max 3.036 _refine_diff_density_min -3.230 _refine_diff_density_rms 0.227 # start Validation Reply Form _vrf_PLAT973_shelx ; PROBLEM: Check Calcd Positive Resid. Density on Ir2 2.07 eA-3 RESPONSE: Residuals close to heavy metals due to the poorquality of cristals and incomplete absorption correction. ; _vrf_PLAT201_shelx ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 3 Report RESPONSE: Disordered trimethilsilyl group refined with two moieties with complementary occupancy and isotropic displacement factors. ; _vrf_PLAT342_shelx ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.02193 Ang. RESPONSE: Due to poor quality of crystals. ; # end Validation Reply Form _shelx_res_file ; TITL enriquen210b in P2(1) (muxt 0.1) shelx.res created by SHELXL-2016/6 at 12:03:12 on 26-Jun-2020 CELL 0.71073 14.5095 18.3399 15.5395 90.000 96.485 90.000 ZERR 4.00 0.0024 0.0030 0.0025 0.000 0.002 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H O Si P Ir UNIT 136 252 12 12 8 4 omit 0 -2 0 omit 1 -5 1 omit -4 -2 10 omit 0 -4 0 size 0.119 0.127 0.173 L.S. 8 ACTA 55 BOND $h FMAP 2 PLAN 75 twin DFIX 1.59 0.01 IR1 H01 IR1 H02 IR2 H03 DFIX 21.0 0.01 SI5 C36A SI5 C37A SI5 C38A SI5 C36B SI5 C37B SI5 C38B DFIX 31.0 0.01 C54 C55A C54 C56A C54 C55B C54 C56B TEMP -173 WGHT 0.042700 BASF 0.02103 FVAR 0.06833 1.83756 1.60589 IR1 6 0.168346 0.107149 0.452912 11.00000 0.01656 0.02498 = 0.01860 0.00213 0.00076 -0.00055 H01 2 0.168687 0.057838 0.368817 11.00000 -1.20000 H02 2 0.180538 0.158118 0.536397 11.00000 -1.20000 H03 2 0.375217 0.331360 1.031350 11.00000 -1.20000 IR2 6 0.357766 0.390377 0.956504 11.00000 0.01656 0.02354 = 0.01856 -0.00068 -0.00048 -0.00196 AFIX 3 H04 2 0.323619 0.440115 0.875779 11.00000 -1.20000 AFIX 0 P1 5 0.158028 -0.001454 0.518781 11.00000 0.01458 0.02487 = 0.01853 0.00265 0.00050 -0.00107 P2 5 0.222487 0.189900 0.363020 11.00000 0.02594 0.02685 = 0.01886 0.00293 0.00310 -0.00187 P3 5 0.401780 0.494733 1.024601 11.00000 0.01893 0.02380 = 0.02113 0.00017 0.00040 -0.00056 P4 5 0.267950 0.302857 0.887241 11.00000 0.01896 0.02659 = 0.02427 -0.00577 -0.00153 -0.00399 SI1 4 0.016871 0.139201 0.440457 11.00000 0.01883 0.02529 = 0.02599 0.00177 0.00095 0.00182 SI2 4 -0.099905 0.127153 0.597856 11.00000 0.02285 0.03562 = 0.02593 -0.00516 0.00303 -0.00191 SI3 4 -0.142856 0.095806 0.294422 11.00000 0.02201 0.04202 = 0.02772 -0.00359 -0.00696 0.00800 SI4 4 0.500372 0.350812 0.930727 11.00000 0.01867 0.02289 = 0.02706 0.00248 0.00161 -0.00007 SI5 4 0.609182 0.381396 0.771174 11.00000 0.04190 0.04785 = 0.03548 0.00469 0.01891 0.01469 SI6 4 0.667238 0.358468 1.077233 11.00000 0.02116 0.03738 = 0.02976 0.00322 -0.00416 -0.00050 O1 3 -0.041133 0.106531 0.519622 11.00000 0.02059 0.02835 = 0.02670 -0.00396 0.00338 -0.00516 O2 3 -0.042954 0.109580 0.350641 11.00000 0.01789 0.03696 = 0.02601 0.00046 -0.00781 -0.00418 O3 3 0.327125 0.085504 0.487260 11.00000 0.01423 0.02291 = 0.02712 0.00421 0.00185 0.00298 O4 3 0.529995 0.374466 0.835918 11.00000 0.02182 0.03367 = 0.02593 -0.00373 0.00049 0.00243 O5 3 0.586584 0.380732 1.001329 11.00000 0.02188 0.02947 = 0.03226 -0.00440 -0.00008 -0.00484 O6 3 0.216009 0.424645 1.000216 11.00000 0.01627 0.02631 = 0.02544 -0.00971 0.00702 -0.00590 C1 1 -0.008307 0.239848 0.439943 11.00000 0.02171 0.02951 = 0.04386 0.00604 0.00022 0.00225 AFIX 137 H1A 2 0.012181 0.261998 0.387951 11.00000 -1.50000 H1B 2 0.024916 0.262404 0.491597 11.00000 -1.50000 H1C 2 -0.075133 0.247565 0.440013 11.00000 -1.50000 AFIX 0 C2 1 -0.216966 0.040627 0.355171 11.00000 0.02426 0.08539 = 0.02994 -0.02275 -0.00115 -0.00031 AFIX 137 H2A 2 -0.187638 -0.006840 0.368185 11.00000 -1.50000 H2B 2 -0.277127 0.033489 0.320702 11.00000 -1.50000 H2C 2 -0.226108 0.065469 0.409395 11.00000 -1.50000 AFIX 0 C3 1 -0.120498 0.047778 0.194383 11.00000 0.03118 0.05607 = 0.04178 -0.00386 -0.00752 0.00091 AFIX 137 H3A 2 -0.093241 0.081817 0.155739 11.00000 -1.50000 H3B 2 -0.178983 0.028685 0.165296 11.00000 -1.50000 H3C 2 -0.077406 0.007348 0.209038 11.00000 -1.50000 AFIX 0 C4 1 -0.199073 0.183767 0.273527 11.00000 0.05844 0.05338 = 0.08606 -0.01071 -0.02783 0.01573 AFIX 137 H4A 2 -0.217098 0.203603 0.327747 11.00000 -1.50000 H4B 2 -0.254414 0.177625 0.231793 11.00000 -1.50000 H4C 2 -0.155973 0.217432 0.249791 11.00000 -1.50000 AFIX 0 C5 1 -0.024387 0.172363 0.686583 11.00000 0.03191 0.06958 = 0.05383 -0.01429 -0.00990 -0.01080 AFIX 137 H5A 2 0.023843 0.138270 0.710538 11.00000 -1.50000 H5B 2 -0.061825 0.187266 0.732247 11.00000 -1.50000 H5C 2 0.004678 0.215413 0.663791 11.00000 -1.50000 AFIX 0 C6 1 -0.145297 0.039222 0.637727 11.00000 0.02762 0.04043 = 0.04490 0.00779 0.00199 0.00133 AFIX 137 H6A 2 -0.179195 0.012931 0.589148 11.00000 -1.50000 H6B 2 -0.187106 0.049452 0.681556 11.00000 -1.50000 H6C 2 -0.093332 0.009289 0.663332 11.00000 -1.50000 AFIX 0 C7 1 -0.202670 0.189355 0.563855 11.00000 0.02352 0.04415 = 0.06433 -0.01578 0.02567 -0.00143 AFIX 137 H7A 2 -0.180038 0.237357 0.548164 11.00000 -1.50000 H7B 2 -0.240318 0.194594 0.612029 11.00000 -1.50000 H7C 2 -0.240543 0.168127 0.513872 11.00000 -1.50000 AFIX 0 C8 1 0.100361 -0.079640 0.462490 11.00000 0.01771 0.02998 = 0.02809 0.00525 0.00178 0.00217 AFIX 13 H8 2 0.112145 -0.123276 0.500738 11.00000 -1.20000 AFIX 0 C9 1 0.135415 -0.097069 0.376088 11.00000 0.02792 0.05436 = 0.03151 -0.00107 -0.00009 0.00288 AFIX 137 H9A 2 0.102804 -0.140012 0.350441 11.00000 -1.50000 H9B 2 0.202158 -0.107033 0.385303 11.00000 -1.50000 H9C 2 0.123847 -0.055381 0.336903 11.00000 -1.50000 AFIX 0 C10 1 -0.005108 -0.067160 0.448371 11.00000 0.02230 0.02396 = 0.03879 0.00186 -0.00635 0.00448 AFIX 137 H10A 2 -0.019303 -0.028784 0.405012 11.00000 -1.50000 H10B 2 -0.027071 -0.052303 0.503104 11.00000 -1.50000 H10C 2 -0.036140 -0.112442 0.428003 11.00000 -1.50000 AFIX 0 C11 1 0.122507 -0.006797 0.628336 11.00000 0.02127 0.02875 = 0.02715 0.01216 0.00818 0.00494 AFIX 13 H11 2 0.060845 0.018089 0.624287 11.00000 -1.20000 AFIX 0 C12 1 0.187540 0.041370 0.688614 11.00000 0.04216 0.05295 = 0.03082 -0.01636 0.00184 -0.01426 AFIX 137 H12A 2 0.165286 0.043429 0.745808 11.00000 -1.50000 H12B 2 0.188653 0.090677 0.664448 11.00000 -1.50000 H12C 2 0.250270 0.020805 0.694135 11.00000 -1.50000 AFIX 0 C13 1 0.106987 -0.080021 0.667147 11.00000 0.05374 0.03867 = 0.03734 0.01463 0.00636 -0.00810 AFIX 137 H13A 2 0.164826 -0.108067 0.671779 11.00000 -1.50000 H13B 2 0.058817 -0.106270 0.630122 11.00000 -1.50000 H13C 2 0.087173 -0.073582 0.724904 11.00000 -1.50000 AFIX 0 C14 1 0.279707 -0.031840 0.534253 11.00000 0.01415 0.04100 = 0.01644 0.00660 0.00344 0.00331 C15 1 0.305766 -0.101649 0.562249 11.00000 0.02441 0.04422 = 0.02328 0.00637 0.00097 -0.00671 AFIX 43 H15 2 0.259245 -0.136472 0.570968 11.00000 -1.20000 AFIX 0 C16 1 0.397630 -0.121163 0.577530 11.00000 0.03001 0.02971 = 0.04357 0.00707 0.00019 0.01600 AFIX 43 H16 2 0.414145 -0.168896 0.597413 11.00000 -1.20000 AFIX 0 C17 1 0.466048 -0.071261 0.563945 11.00000 0.02003 0.03549 = 0.02842 0.00420 0.00180 -0.00152 AFIX 43 H17 2 0.529357 -0.085335 0.574050 11.00000 -1.20000 AFIX 0 C18 1 0.443735 -0.001233 0.535893 11.00000 0.01618 0.02821 = 0.01382 0.00210 0.00026 0.00087 C19 1 0.350723 0.017229 0.518930 11.00000 0.02225 0.02231 = 0.03352 0.00342 0.00423 0.00027 C20 1 0.514638 0.055737 0.524018 11.00000 0.01822 0.04681 = 0.02763 -0.00335 -0.00024 0.00479 C21 1 0.522662 0.108313 0.603196 11.00000 0.02790 0.05961 = 0.05189 -0.01699 0.01226 -0.01006 AFIX 137 H21A 2 0.460516 0.123664 0.614662 11.00000 -1.50000 H21B 2 0.559064 0.151236 0.590588 11.00000 -1.50000 H21C 2 0.553457 0.083128 0.654166 11.00000 -1.50000 AFIX 0 C22 1 0.613397 0.025074 0.519072 11.00000 0.02210 0.05508 = 0.05438 0.00548 0.00965 0.00504 AFIX 137 H22A 2 0.632596 -0.003773 0.571105 11.00000 -1.50000 H22B 2 0.656873 0.065535 0.515291 11.00000 -1.50000 H22C 2 0.613191 -0.005936 0.467691 11.00000 -1.50000 AFIX 0 C23 1 0.478001 0.102131 0.444215 11.00000 0.02114 0.04012 = 0.02991 0.01239 -0.00518 0.00003 C24 1 0.533936 0.132061 0.386882 11.00000 0.03242 0.07344 = 0.02446 0.00915 0.00984 -0.00584 AFIX 43 H24 2 0.598847 0.123198 0.394929 11.00000 -1.20000 AFIX 0 C25 1 0.497246 0.174177 0.318855 11.00000 0.02814 0.07505 = 0.03104 0.00202 0.01971 -0.00706 AFIX 43 H25 2 0.535922 0.191381 0.277793 11.00000 -1.20000 AFIX 0 C26 1 0.404610 0.191658 0.309765 11.00000 0.03225 0.04528 = 0.02857 0.00321 0.00962 0.01056 AFIX 43 H26 2 0.380186 0.223495 0.264620 11.00000 -1.20000 AFIX 0 C27 1 0.345316 0.162327 0.367565 11.00000 0.03590 0.02290 = 0.02908 -0.00583 0.02414 -0.00347 C28 1 0.384257 0.117093 0.431218 11.00000 0.02625 0.04214 = 0.00989 -0.00152 0.00847 -0.00708 C29 1 0.181908 0.187960 0.247312 11.00000 0.04115 0.05546 = 0.00981 0.00984 0.00047 -0.01990 AFIX 13 H29 2 0.227048 0.217311 0.217613 11.00000 -1.20000 AFIX 0 C30 1 0.181756 0.112384 0.209623 11.00000 0.09989 0.04795 = 0.03949 -0.01092 0.01163 -0.04152 AFIX 137 H30A 2 0.135023 0.082600 0.234052 11.00000 -1.50000 H30B 2 0.243085 0.090253 0.223689 11.00000 -1.50000 H30C 2 0.167063 0.115073 0.146582 11.00000 -1.50000 AFIX 0 C31 1 0.087199 0.225168 0.227851 11.00000 0.02992 0.09906 = 0.04565 0.02218 -0.01558 -0.01935 AFIX 137 H31A 2 0.065884 0.220764 0.165944 11.00000 -1.50000 H31B 2 0.092842 0.276844 0.243620 11.00000 -1.50000 H31C 2 0.042347 0.201674 0.261551 11.00000 -1.50000 AFIX 0 C32 1 0.230052 0.288232 0.390205 11.00000 0.02772 0.03435 = 0.03627 0.00355 0.00974 -0.00148 AFIX 13 H32 2 0.165102 0.304561 0.395142 11.00000 -1.20000 AFIX 0 C33 1 0.283710 0.298902 0.480319 11.00000 0.06712 0.04489 = 0.04890 -0.01914 0.01829 -0.01412 AFIX 137 H33A 2 0.348918 0.285748 0.478454 11.00000 -1.50000 H33B 2 0.256881 0.267721 0.522250 11.00000 -1.50000 H33C 2 0.279567 0.350044 0.497750 11.00000 -1.50000 AFIX 0 C34 1 0.266891 0.338442 0.326174 11.00000 0.03382 0.02520 = 0.07013 0.00848 0.00645 -0.00346 AFIX 137 H34A 2 0.259568 0.389095 0.344306 11.00000 -1.50000 H34B 2 0.232439 0.330947 0.268900 11.00000 -1.50000 H34C 2 0.332768 0.328135 0.323426 11.00000 -1.50000 AFIX 0 C35 1 0.517538 0.248894 0.934576 11.00000 0.03280 0.02941 = 0.04645 0.00408 -0.00630 -0.00110 AFIX 137 H35A 2 0.478621 0.226238 0.886216 11.00000 -1.50000 H35B 2 0.500090 0.229923 0.989427 11.00000 -1.50000 H35C 2 0.582826 0.237556 0.930086 11.00000 -1.50000 PART 1 AFIX 0 C36A 1 0.549804 0.401855 0.663092 10.40000 0.09923 AFIX 137 H36A 2 0.499751 0.366545 0.648638 10.40000 -1.50000 H36B 2 0.594241 0.398764 0.620193 10.40000 -1.50000 H36C 2 0.523755 0.451168 0.662806 10.40000 -1.50000 AFIX 0 C37A 1 0.703579 0.438976 0.823124 10.40000 0.10131 AFIX 137 H37A 2 0.684068 0.461365 0.875393 10.40000 -1.50000 H37B 2 0.718110 0.477257 0.782772 10.40000 -1.50000 H37C 2 0.758780 0.408942 0.838846 10.40000 -1.50000 AFIX 0 C38A 1 0.666449 0.292985 0.760812 10.40000 0.04844 AFIX 137 H38A 2 0.697370 0.278075 0.817408 10.40000 -1.50000 H38B 2 0.712478 0.297367 0.719548 10.40000 -1.50000 H38C 2 0.620045 0.256355 0.739954 10.40000 -1.50000 PART 2 AFIX 0 C36B 1 0.577882 0.454208 0.691816 10.60000 0.04468 AFIX 137 H36D 2 0.511814 0.450549 0.670653 10.60000 -1.50000 H36E 2 0.614789 0.449091 0.643093 10.60000 -1.50000 H36F 2 0.590369 0.501777 0.719424 10.60000 -1.50000 AFIX 0 C37B 1 0.721688 0.408278 0.829988 10.60000 0.04400 AFIX 137 H37D 2 0.712719 0.450156 0.867319 10.60000 -1.50000 H37E 2 0.764736 0.421574 0.788311 10.60000 -1.50000 H37F 2 0.747349 0.367378 0.865563 10.60000 -1.50000 AFIX 0 C38B 1 0.627607 0.295696 0.716153 10.60000 0.07306 AFIX 137 H38D 2 0.656456 0.260292 0.758117 10.60000 -1.50000 H38E 2 0.668391 0.304063 0.670975 10.60000 -1.50000 H38F 2 0.567878 0.276672 0.689792 10.60000 -1.50000 PART 0 AFIX 0 C39 1 0.750204 0.290272 1.041337 11.00000 0.03310 0.05490 = 0.02921 -0.00747 0.00285 -0.00937 AFIX 137 H39A 2 0.716006 0.247087 1.018418 11.00000 -1.50000 H39B 2 0.794718 0.276187 1.090702 11.00000 -1.50000 H39C 2 0.783498 0.311695 0.996024 11.00000 -1.50000 AFIX 0 C40 1 0.616190 0.319690 1.171986 11.00000 0.03254 0.04307 = 0.04706 0.02305 0.01960 0.01440 AFIX 137 H40A 2 0.583327 0.358121 1.199992 11.00000 -1.50000 H40B 2 0.665783 0.299839 1.213430 11.00000 -1.50000 H40C 2 0.572599 0.280706 1.152395 11.00000 -1.50000 AFIX 0 C41 1 0.730919 0.444269 1.107624 11.00000 0.03179 0.06320 = 0.05520 -0.00554 -0.02123 -0.01219 AFIX 137 H41A 2 0.749868 0.467334 1.055519 11.00000 -1.50000 H41B 2 0.786023 0.433193 1.147972 11.00000 -1.50000 H41C 2 0.690445 0.477521 1.135404 11.00000 -1.50000 AFIX 0 C42 1 0.451003 0.569964 0.968374 11.00000 0.02335 0.03613 = 0.01807 -0.00510 0.00599 -0.00022 AFIX 13 H42 2 0.459000 0.611693 1.009969 11.00000 -1.20000 AFIX 0 C43 1 0.385548 0.595761 0.890213 11.00000 0.03462 0.02755 = 0.02757 0.00180 -0.00651 -0.00124 AFIX 137 H43A 2 0.416072 0.633858 0.859467 11.00000 -1.50000 H43B 2 0.328747 0.615389 0.909984 11.00000 -1.50000 H43C 2 0.369895 0.554562 0.851118 11.00000 -1.50000 AFIX 0 C44 1 0.546432 0.552033 0.942678 11.00000 0.02456 0.03639 = 0.03816 0.01059 0.01138 -0.00183 AFIX 137 H44A 2 0.541076 0.512575 0.899878 11.00000 -1.50000 H44B 2 0.587242 0.536593 0.994010 11.00000 -1.50000 H44C 2 0.572514 0.595370 0.917576 11.00000 -1.50000 AFIX 0 C45 1 0.471932 0.489060 1.131870 11.00000 0.03675 0.02356 = 0.01914 -0.00266 -0.00267 -0.00389 AFIX 13 H45 2 0.523806 0.454652 1.124073 11.00000 -1.20000 AFIX 0 C46 1 0.517984 0.558715 1.168718 11.00000 0.03632 0.03470 = 0.03171 -0.00540 -0.00958 0.00638 AFIX 137 H46A 2 0.470372 0.592564 1.184438 11.00000 -1.50000 H46B 2 0.552538 0.581412 1.125118 11.00000 -1.50000 H46C 2 0.560673 0.546986 1.220306 11.00000 -1.50000 AFIX 0 C47 1 0.417069 0.453501 1.197861 11.00000 0.02326 0.03661 = 0.01903 0.00517 0.00060 -0.00787 AFIX 137 H47A 2 0.459745 0.429337 1.242316 11.00000 -1.50000 H47B 2 0.374441 0.417383 1.168949 11.00000 -1.50000 H47C 2 0.381529 0.490778 1.225007 11.00000 -1.50000 AFIX 0 C48 1 0.291011 0.533138 1.051337 11.00000 0.02666 0.02238 = 0.02881 -0.00266 -0.00602 0.00441 C49 1 0.285979 0.600601 1.087688 11.00000 0.04546 0.02512 = 0.03506 -0.00888 0.01293 -0.00734 AFIX 43 H49 2 0.340940 0.628651 1.099931 11.00000 -1.20000 AFIX 0 C50 1 0.202202 0.628916 1.107056 11.00000 0.03690 0.02849 = 0.06675 -0.01548 0.00549 -0.00216 AFIX 43 H50 2 0.199853 0.676440 1.131031 11.00000 -1.20000 AFIX 0 C51 1 0.124333 0.589149 1.091920 11.00000 0.03107 0.04501 = 0.03848 -0.00609 0.01082 0.01174 AFIX 43 H51 2 0.067297 0.608833 1.105849 11.00000 -1.20000 AFIX 0 C52 1 0.125701 0.519340 1.056052 11.00000 0.02237 0.03292 = 0.03125 -0.00264 0.01104 -0.00309 C53 1 0.208667 0.494646 1.035189 11.00000 0.02835 0.02405 = 0.02052 0.00331 0.01025 -0.00079 C54 1 0.038212 0.472550 1.039400 11.00000 0.01607 0.05172 = 0.04134 -0.01979 0.00920 -0.01234 PART 1 C55A 1 -0.043322 0.525783 0.996537 10.50000 0.03635 AFIX 137 H55A 2 -0.026157 0.545477 0.941926 10.50000 -1.50000 H55B 2 -0.051957 0.565976 1.036404 10.50000 -1.50000 H55C 2 -0.101231 0.498136 0.985321 10.50000 -1.50000 AFIX 0 C56A 1 0.006933 0.440556 1.126654 10.50000 0.04863 AFIX 137 H56A 2 -0.031081 0.396922 1.113620 10.50000 -1.50000 H56B 2 -0.029357 0.477295 1.153870 10.50000 -1.50000 H56C 2 0.061955 0.427730 1.166255 10.50000 -1.50000 PART 2 AFIX 0 C55B 1 -0.059538 0.512179 1.039439 10.50000 0.07071 AFIX 137 H55D 2 -0.075056 0.537625 0.984248 10.50000 -1.50000 H55E 2 -0.056207 0.547454 1.087061 10.50000 -1.50000 H55F 2 -0.107459 0.475827 1.047032 10.50000 -1.50000 AFIX 0 C56B 1 0.048749 0.422409 1.125923 10.50000 0.03164 AFIX 137 H56D 2 0.004537 0.381887 1.118507 10.50000 -1.50000 H56E 2 0.036048 0.451963 1.175786 10.50000 -1.50000 H56F 2 0.112031 0.403078 1.135757 10.50000 -1.50000 PART 3 AFIX 0 C57 1 0.048710 0.415980 0.972247 11.00000 0.01819 0.04254 = 0.02859 -0.00836 0.00644 0.00663 C58 1 -0.028131 0.385013 0.923906 11.00000 0.04002 0.05370 = 0.09755 -0.01605 0.00594 0.02560 AFIX 43 H58 2 -0.088334 0.403316 0.929855 11.00000 -1.20000 AFIX 0 C59 1 -0.018310 0.328967 0.868308 11.00000 0.05136 0.06832 = 0.13709 -0.06010 -0.02544 -0.00196 AFIX 43 H59 2 -0.071435 0.305486 0.839461 11.00000 -1.20000 AFIX 0 C60 1 0.072170 0.305857 0.853768 11.00000 0.02093 0.05610 = 0.06563 -0.03592 -0.01179 0.00326 AFIX 43 H60 2 0.079102 0.269403 0.811546 11.00000 -1.20000 AFIX 0 C61 1 0.149503 0.335226 0.899561 11.00000 0.03182 0.03433 = 0.02922 -0.00566 0.00488 -0.00930 C62 1 0.135758 0.390978 0.956329 11.00000 0.03432 0.02305 = 0.02296 0.00313 0.00260 -0.00432 C63 1 0.270394 0.210745 0.934584 11.00000 0.04288 0.03520 = 0.05035 0.00014 0.00992 -0.01544 AFIX 13 H63 2 0.335976 0.193574 0.936151 11.00000 -1.20000 AFIX 0 C64 1 0.250769 0.215339 1.028985 11.00000 0.05490 0.04629 = 0.05511 0.01628 0.01278 -0.01345 AFIX 137 H64A 2 0.184785 0.225547 1.031222 11.00000 -1.50000 H64B 2 0.288029 0.254532 1.058264 11.00000 -1.50000 H64C 2 0.266907 0.168883 1.058019 11.00000 -1.50000 AFIX 0 C65 1 0.211458 0.152162 0.887993 11.00000 0.07925 0.04046 = 0.08486 -0.00414 0.00228 -0.03457 AFIX 137 H65A 2 0.199632 0.113617 0.929024 11.00000 -1.50000 H65B 2 0.244031 0.131533 0.841716 11.00000 -1.50000 H65C 2 0.152376 0.173229 0.862933 11.00000 -1.50000 AFIX 0 C66 1 0.258793 0.286105 0.768419 11.00000 0.02816 0.06807 = 0.01309 -0.01213 -0.00372 0.00760 AFIX 13 H66 2 0.205051 0.252741 0.752516 11.00000 -1.20000 AFIX 0 C67 1 0.240964 0.355423 0.720042 11.00000 0.08135 0.07273 = 0.02375 -0.01039 -0.02395 0.02250 AFIX 137 H67A 2 0.287967 0.391501 0.741205 11.00000 -1.50000 H67B 2 0.179280 0.373776 0.728809 11.00000 -1.50000 H67C 2 0.243874 0.346749 0.658179 11.00000 -1.50000 AFIX 0 C68 1 0.345810 0.248980 0.744598 11.00000 0.03970 0.05509 = 0.03217 -0.01154 -0.00803 -0.00571 AFIX 137 H68A 2 0.337198 0.235420 0.683215 11.00000 -1.50000 H68B 2 0.357937 0.205078 0.780024 11.00000 -1.50000 H68C 2 0.398522 0.282452 0.755164 11.00000 -1.50000 PART AFIX 0 HKLF 4 REM enriquen210b in P2(1) (muxt 0.1) REM R1 = 0.0577 for 12877 Fo > 4sig(Fo) and 0.1413 for all 21062 data REM 821 parameters refined using 14 restraints END WGHT 0.0451 0.0000 REM Highest difference peak 3.036, deepest hole -3.230, 1-sigma level 0.227 Q1 1 0.1614 0.1088 0.4996 11.00000 0.05 3.04 Q2 1 0.3437 0.3899 0.9979 11.00000 0.05 3.01 Q3 1 0.3581 0.3898 0.9056 11.00000 0.05 2.50 Q4 1 0.1810 0.1091 0.4098 11.00000 0.05 2.21 Q5 1 0.3609 0.4207 0.9561 11.00000 0.05 2.06 Q6 1 0.3592 0.3590 0.9565 11.00000 0.05 2.00 Q7 1 0.1681 0.0800 0.4517 11.00000 0.05 1.87 Q8 1 0.2800 0.3662 0.9849 11.00000 0.05 1.83 Q9 1 0.1690 0.1396 0.4515 11.00000 0.05 1.72 Q10 1 0.4423 0.4192 0.9421 11.00000 0.05 1.63 Q11 1 0.2436 0.1377 0.4270 11.00000 0.05 1.63 Q12 1 0.4042 0.4430 0.9086 11.00000 0.05 1.62 Q13 1 0.1250 0.0612 0.4956 11.00000 0.05 1.59 Q14 1 0.0977 0.1393 0.4856 11.00000 0.05 1.59 Q15 1 0.3205 0.3295 0.9825 11.00000 0.05 1.57 Q16 1 0.2812 0.4151 0.9806 11.00000 0.05 1.55 Q17 1 0.3483 0.4674 0.9468 11.00000 0.05 1.49 Q18 1 0.1968 0.1061 0.4425 11.00000 0.05 1.48 Q19 1 0.3176 0.4513 0.9906 11.00000 0.05 1.46 Q20 1 0.0821 0.1270 0.4733 11.00000 0.05 1.46 Q21 1 0.0805 0.0892 0.4728 11.00000 0.05 1.45 Q22 1 0.1606 0.0299 0.4506 11.00000 0.05 1.43 Q23 1 0.4237 0.4332 0.9237 11.00000 0.05 1.42 Q24 1 0.1181 0.1623 0.4879 11.00000 0.05 1.39 Q25 1 0.4017 0.3378 0.9138 11.00000 0.05 1.37 Q26 1 0.1929 0.0544 0.4065 11.00000 0.05 1.36 Q27 1 0.3613 0.4422 1.0201 11.00000 0.05 1.29 Q28 1 0.4413 0.3761 0.9251 11.00000 0.05 1.28 Q29 1 -0.1764 0.1774 0.5451 11.00000 0.05 1.27 Q30 1 0.1847 0.0550 0.5151 11.00000 0.05 1.26 Q31 1 0.2412 0.0872 0.4152 11.00000 0.05 1.26 Q32 1 0.3202 0.3968 0.9455 11.00000 0.05 1.24 Q33 1 0.0983 0.1069 0.4150 11.00000 0.05 1.23 Q34 1 0.4209 0.3517 0.9259 11.00000 0.05 1.22 Q35 1 0.2006 0.1713 0.4129 11.00000 0.05 1.21 Q36 1 0.3981 0.3878 0.9766 11.00000 0.05 1.21 Q37 1 0.1387 0.1796 0.4688 11.00000 0.05 1.19 Q38 1 0.1443 0.1001 0.3281 11.00000 0.05 1.15 Q39 1 0.1612 0.1863 0.4529 11.00000 0.05 1.14 Q40 1 0.3571 0.3134 0.9549 11.00000 0.05 1.14 Q41 1 0.2587 0.3077 0.9584 11.00000 0.05 1.13 Q42 1 0.3628 0.4147 0.7594 11.00000 0.05 1.13 Q43 1 0.6384 0.3226 1.0451 11.00000 0.05 1.12 Q44 1 0.1798 0.0803 0.2685 11.00000 0.05 1.10 Q45 1 0.2231 0.1080 0.4835 11.00000 0.05 1.05 Q46 1 0.0643 0.1364 0.6518 11.00000 0.05 1.03 Q47 1 0.1673 0.0792 0.6452 11.00000 0.05 1.03 Q48 1 0.2793 0.3909 0.9137 11.00000 0.05 1.02 Q49 1 0.1539 0.1612 0.5192 11.00000 0.05 1.02 Q50 1 0.1722 0.1901 0.5874 11.00000 0.05 1.01 Q51 1 0.3588 0.4189 1.1461 11.00000 0.05 0.98 Q52 1 0.1609 0.1693 0.3999 11.00000 0.05 0.95 Q53 1 0.3009 0.2971 1.0153 11.00000 0.05 0.95 Q54 1 0.1746 0.1407 0.6431 11.00000 0.05 0.95 Q55 1 0.6780 0.4910 1.0477 11.00000 0.05 0.93 Q56 1 0.2541 0.4744 0.9613 11.00000 0.05 0.91 Q57 1 0.3971 0.4184 0.8763 11.00000 0.05 0.91 Q58 1 0.3596 0.3510 1.0684 11.00000 0.05 0.91 Q59 1 -0.0225 0.3920 0.9436 11.00000 0.05 0.89 Q60 1 0.1824 0.1438 0.7528 11.00000 0.05 0.89 Q61 1 0.3608 0.3338 1.0125 11.00000 0.05 0.88 Q62 1 0.3029 0.3922 1.1397 11.00000 0.05 0.86 Q63 1 0.0976 0.3977 0.9958 11.00000 0.05 0.86 Q64 1 -0.0554 0.1008 0.4002 11.00000 0.05 0.84 Q65 1 0.6665 0.2796 1.0798 11.00000 0.05 0.83 Q66 1 0.2185 0.1908 0.5540 11.00000 0.05 0.82 Q67 1 0.1423 0.0335 0.3396 11.00000 0.05 0.82 Q68 1 0.3607 0.3627 0.7696 11.00000 0.05 0.82 Q69 1 0.3619 0.4136 1.0733 11.00000 0.05 0.81 Q70 1 0.1746 0.0386 0.5833 11.00000 0.05 0.80 Q71 1 0.1848 0.1065 0.0577 11.00000 0.05 0.80 Q72 1 0.0733 0.3296 1.0719 11.00000 0.05 0.79 Q73 1 0.1908 0.0148 0.3781 11.00000 0.05 0.79 Q74 1 0.1835 0.2016 0.3542 11.00000 0.05 0.79 Q75 1 0.2389 0.3363 1.0053 11.00000 0.05 0.79 ; _shelx_res_checksum 54400 _shelx_hkl_file ; -1 0 0 12.24 0.74 -1 0 0 11.16 0.83 -2 0 0 43.22 2.03 -2 0 0 41.65 1.86 -3 0 0 34.03 2.40 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129.87 5.40 -6 3 0 154.46 5.69 -6 3 0 158.73 5.64 -6 3 0 164.98 5.14 -7 -3 0 107.81 4.78 -7 -3 0 112.19 5.39 -7 3 0 107.73 5.12 -7 3 0 116.52 5.07 -7 3 0 122.72 4.56 -8 -3 0 22.32 2.80 -8 -3 0 21.21 3.31 -8 3 0 21.09 2.97 -8 3 0 25.45 2.64 -9 -3 0 41.53 4.08 -9 -3 0 42.45 3.56 -9 3 0 38.46 3.20 -9 3 0 42.39 3.75 -10 -3 0 56.62 4.83 -10 -3 0 62.46 4.41 -10 3 0 41.23 3.57 -10 3 0 45.53 4.16 -11 -3 0 57.04 5.22 -11 -3 0 62.93 4.62 -11 3 0 53.53 4.09 -11 3 0 45.40 4.48 -12 -3 0 51.77 5.42 -12 -3 0 60.24 4.91 -12 3 0 54.71 5.04 -12 3 0 53.33 4.39 -13 -3 0 38.67 5.14 -13 -3 0 50.29 4.94 -13 3 0 39.93 4.19 -13 3 0 42.32 4.86 -14 -3 0 13.32 4.99 -14 -3 0 21.07 4.70 -14 3 0 13.84 4.41 -15 -3 0 2.07 4.21 -15 -3 0 -3.64 4.74 -15 3 0 6.48 4.48 -16 -3 0 51.83 5.97 -16 -3 0 42.77 6.35 -16 3 0 48.06 5.89 -17 -3 0 3.03 4.93 -17 -3 0 -3.99 5.40 -17 3 0 2.35 5.08 -18 -3 0 5.62 5.22 -18 -3 0 -2.44 6.15 18 3 0 11.13 6.23 -18 3 0 1.46 5.41 -19 -3 0 -3.67 6.58 -19 -3 0 5.76 5.98 19 3 0 7.08 7.09 -19 3 0 16.57 6.21 0 -4 0 563.59 13.82 0 4 0 609.89 14.77 0 4 0 615.48 14.60 -1 -4 0 6.40 1.85 -1 4 0 1.36 1.81 -1 4 0 1.68 1.82 1 4 0 4.08 1.73 -2 -4 0 10.46 2.15 -2 4 0 3.61 2.05 2 4 0 6.36 1.89 -2 4 0 4.36 2.01 -3 -4 0 66.41 3.73 -3 -4 0 53.28 2.92 -3 4 0 59.09 3.41 -3 4 0 57.30 3.45 3 4 0 55.84 3.28 -4 -4 0 111.69 4.08 -4 -4 0 114.16 4.72 4 4 0 102.43 4.10 -4 4 0 99.80 4.41 -4 4 0 111.62 4.26 -5 -4 0 32.88 2.45 -5 -4 0 31.10 2.96 -5 4 0 43.63 3.01 5 4 0 40.40 3.26 -5 4 0 40.14 3.22 -5 4 0 38.86 2.39 -6 -4 0 204.72 7.13 -6 -4 0 205.39 6.44 -6 4 0 196.74 6.71 6 4 0 193.37 6.50 -6 4 0 204.91 6.56 -6 4 0 205.17 5.90 7 -4 0 52.73 3.73 -7 -4 0 54.29 4.47 -7 -4 0 50.53 3.71 -7 4 0 56.66 4.16 -7 4 0 64.17 3.36 -7 4 0 48.57 4.05 -8 -4 0 8.96 2.52 -8 -4 0 8.96 3.03 -8 4 0 8.51 2.78 -8 4 0 8.57 2.05 -8 4 0 6.27 2.89 -9 -4 0 46.69 4.07 -9 -4 0 54.47 4.51 -9 4 0 49.27 4.14 -9 4 0 50.93 3.91 -10 -4 0 45.39 3.93 -10 -4 0 31.56 4.40 -10 4 0 29.14 3.97 -10 4 0 20.77 3.17 -11 -4 0 33.36 4.83 -11 -4 0 36.74 4.15 -11 4 0 44.81 3.77 -11 4 0 39.11 4.42 -12 -4 0 24.90 4.05 -12 -4 0 17.47 4.65 -12 4 0 25.65 4.45 -12 4 0 19.69 3.45 -13 -4 0 1.78 3.73 -13 -4 0 1.27 4.31 -13 4 0 2.82 3.85 -14 -4 0 5.54 4.11 -14 -4 0 7.32 4.89 -14 4 0 13.28 4.44 -15 -4 0 28.47 5.97 -15 -4 0 43.93 5.47 -15 4 0 44.31 5.75 -16 -4 0 2.39 4.65 -16 -4 0 -7.89 5.30 16 4 0 1.11 5.37 -16 4 0 6.95 4.85 -17 -4 0 9.66 5.20 -17 -4 0 0.76 5.63 -17 4 0 18.94 5.64 17 4 0 26.51 6.31 -18 -4 0 -7.96 6.16 -18 -4 0 9.30 5.82 18 4 0 2.20 6.47 -18 4 0 10.84 5.89 -19 -4 0 -3.75 5.56 -19 -4 0 -9.36 6.53 19 4 0 -2.40 6.93 0 -5 0 2.17 1.57 0 5 0 -0.74 2.05 0 5 0 1.96 2.03 -1 -5 0 23.60 2.27 1 5 0 29.10 2.38 -1 5 0 27.19 2.39 -1 5 0 23.01 2.41 -2 -5 0 87.60 4.09 -2 5 0 108.26 4.25 -2 5 0 109.15 4.37 2 5 0 105.54 4.04 -3 -5 0 35.85 2.85 -3 5 0 44.53 3.45 3 5 0 41.12 3.06 -3 5 0 46.44 3.36 -4 -5 0 120.49 5.05 -4 -5 0 118.59 4.24 -4 5 0 124.56 4.89 4 5 0 123.36 4.61 -4 5 0 128.64 4.79 -5 -5 0 35.80 3.16 -5 -5 0 31.99 2.58 -5 5 0 35.05 2.93 -5 5 0 31.28 2.90 5 5 0 33.56 2.79 -6 -5 0 32.10 2.76 -6 -5 0 31.63 3.30 -6 5 0 44.19 3.41 6 5 0 46.76 3.83 -6 5 0 41.85 3.31 -7 -5 0 22.48 3.34 -7 -5 0 26.66 2.81 7 5 0 16.43 3.01 -7 5 0 19.89 2.91 -7 5 0 18.44 1.92 -7 5 0 19.09 2.99 -8 -5 0 121.76 5.24 -8 -5 0 124.52 6.19 -8 5 0 133.22 6.01 -8 5 0 143.52 5.02 8 5 0 136.13 5.95 -8 5 0 143.51 6.11 -9 -5 0 90.81 5.97 -9 -5 0 90.73 5.17 9 5 0 78.33 5.24 -9 5 0 91.98 5.39 -9 5 0 91.09 4.38 -9 5 0 85.08 5.46 -10 -5 0 20.79 3.72 -10 -5 0 22.86 4.22 -10 5 0 21.15 3.85 -10 5 0 22.35 2.84 10 5 0 29.13 4.22 -11 -5 0 0.17 4.01 -11 -5 0 -2.48 3.43 -11 5 0 8.57 3.75 11 5 0 1.14 4.04 -11 5 0 3.34 2.60 -12 -5 0 20.59 4.13 -12 -5 0 13.64 4.68 -12 5 0 18.08 4.24 12 5 0 19.83 4.69 -13 -5 0 113.17 7.28 -13 -5 0 103.90 6.35 13 5 0 100.81 6.97 -13 5 0 110.04 6.86 -14 -5 0 4.92 4.36 -14 -5 0 -5.38 4.76 -14 5 0 4.74 4.26 14 5 0 10.16 5.07 -15 -5 0 17.77 4.84 -15 -5 0 9.53 5.40 15 5 0 24.01 5.66 -15 5 0 11.76 4.96 -16 -5 0 2.01 5.52 -16 -5 0 2.09 4.71 16 5 0 9.99 5.71 -16 5 0 12.25 5.07 -17 -5 0 18.29 5.32 -17 -5 0 1.08 5.95 -17 5 0 10.88 5.59 17 5 0 10.76 6.18 -18 -5 0 1.77 5.31 -18 -5 0 -12.67 5.95 18 5 0 -0.20 6.47 -18 5 0 -0.52 5.54 -19 -5 0 8.69 6.92 -19 -5 0 27.16 6.50 0 -6 0 72.34 3.28 0 6 0 72.65 3.81 0 6 0 76.07 3.89 1 -6 0 145.05 4.22 -1 -6 0 141.31 4.85 1 6 0 144.92 4.99 -1 6 0 149.26 5.17 -1 6 0 144.22 5.04 -2 -6 0 -0.19 1.99 2 6 0 5.33 2.01 -2 6 0 2.16 2.01 -2 6 0 3.63 2.15 -3 -6 0 61.50 3.83 -3 6 0 67.63 3.98 3 6 0 73.63 3.71 -3 6 0 74.03 3.92 -4 -6 0 70.62 4.30 4 6 0 65.96 3.69 -4 6 0 68.95 4.18 -4 6 0 69.32 3.88 -5 -6 0 1.63 2.58 -5 -6 0 -1.48 2.06 -5 6 0 1.61 2.50 5 6 0 0.95 2.35 -5 6 0 -0.44 2.34 -6 -6 0 46.32 4.27 -6 -6 0 45.25 3.60 -6 6 0 39.33 3.43 -6 6 0 40.83 3.42 6 6 0 44.67 3.84 -7 -6 0 106.78 5.55 -7 -6 0 102.19 4.82 7 6 0 103.54 5.02 -7 6 0 100.57 5.13 -7 6 0 96.50 5.20 -8 -6 0 40.73 3.55 -8 -6 0 46.72 4.16 8 -6 0 41.56 3.55 -8 6 0 39.90 3.80 8 6 0 38.31 3.70 -8 6 0 34.73 3.77 -9 -6 0 30.12 4.22 -9 -6 0 40.57 3.83 9 6 0 44.40 4.21 -9 6 0 37.62 3.34 -9 6 0 40.70 4.14 -9 6 0 41.75 4.41 -10 -6 0 29.98 4.59 -10 -6 0 32.12 3.99 -10 6 0 36.12 4.41 -10 6 0 36.80 4.56 10 6 0 28.06 4.39 -11 -6 0 22.15 4.08 -11 -6 0 22.82 4.83 -11 6 0 34.47 4.74 11 6 0 38.36 4.95 -12 -6 0 17.39 4.76 -12 -6 0 15.52 4.05 12 6 0 26.73 4.89 -12 6 0 28.22 4.52 -13 -6 0 5.02 4.76 -13 -6 0 11.73 4.05 13 6 0 12.96 4.81 -13 6 0 8.24 4.33 -14 -6 0 31.25 5.83 -14 -6 0 34.64 5.00 -14 6 0 27.63 5.13 14 6 0 32.17 5.80 -15 -6 0 7.40 4.67 -15 -6 0 6.73 5.55 15 6 0 17.22 5.73 -15 6 0 13.82 4.98 -16 -6 0 3.13 4.69 -16 -6 0 1.86 5.64 16 6 0 -2.46 5.57 -16 6 0 7.55 5.12 -17 -6 0 4.47 6.27 -17 -6 0 10.81 5.34 -17 6 0 15.08 5.74 17 6 0 14.08 6.38 -18 -6 0 25.63 6.01 -18 -6 0 4.74 6.74 18 6 0 22.13 7.05 -18 6 0 22.60 6.21 -19 -6 0 9.18 5.83 -19 -6 0 -6.96 6.85 0 -7 0 -1.60 1.59 0 7 0 0.38 2.20 0 7 0 4.00 2.26 -1 -7 0 69.79 3.63 1 -7 0 70.70 2.92 -1 7 0 81.07 4.03 1 7 0 85.38 4.07 -1 7 0 78.83 4.15 -2 -7 0 2.23 2.16 -2 7 0 0.38 2.22 2 7 0 4.26 2.15 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0 14.10 4.97 -15 -7 0 -0.58 4.44 -15 -7 0 -4.61 5.31 15 7 0 0.22 5.25 -15 7 0 6.25 4.80 -16 -7 0 52.53 5.92 -16 -7 0 34.25 6.85 -16 7 0 42.87 6.28 16 7 0 48.60 6.68 -17 -7 0 -0.72 5.91 -17 -7 0 -4.70 5.03 -17 7 0 1.10 5.50 17 7 0 -9.92 5.77 -18 -7 0 10.13 5.60 -18 -7 0 -7.03 6.52 18 7 0 14.34 6.73 -18 7 0 -0.99 5.94 -19 -7 0 -0.87 5.59 0 -8 0 177.80 5.57 0 8 0 179.61 6.26 0 8 0 197.40 6.38 -1 -8 0 20.23 2.50 1 -8 0 19.47 1.84 1 8 0 17.00 2.73 1 8 0 15.55 2.63 -1 8 0 14.02 2.72 -1 8 0 12.51 2.70 -2 -8 0 5.11 2.36 -2 8 0 2.21 2.60 2 8 0 6.44 2.49 -2 8 0 9.23 2.60 -3 -8 0 121.61 5.40 3 8 0 119.38 4.89 -3 8 0 120.13 5.00 -3 8 0 115.59 5.32 -4 -8 0 143.24 6.04 4 8 0 149.43 5.73 -4 8 0 158.70 5.93 -4 8 0 152.51 6.18 -5 -8 0 19.54 3.25 -5 8 0 22.56 3.24 5 8 0 25.52 3.14 -5 8 0 22.36 3.30 -6 -8 0 89.20 5.34 -6 8 0 100.80 5.49 6 8 0 89.30 4.87 -6 8 0 104.96 5.33 -7 -8 0 40.61 3.79 -7 -8 0 46.80 4.37 -7 8 0 45.24 4.15 -7 8 0 51.75 4.24 7 8 0 54.80 4.08 -8 -8 0 34.28 3.75 -8 -8 0 33.11 4.38 8 8 0 35.07 4.08 -8 8 0 29.93 4.13 -8 8 0 28.67 3.95 -9 -8 0 58.50 5.00 -9 -8 0 63.34 5.45 9 -8 0 72.76 4.93 -9 8 0 60.07 5.07 9 8 0 65.91 4.89 -9 8 0 54.89 4.86 10 -8 0 13.34 3.88 -10 -8 0 19.63 4.09 -10 -8 0 17.99 4.60 -10 8 0 17.31 4.51 -10 8 0 17.03 4.14 10 8 0 15.76 4.26 11 -8 0 14.99 3.88 -11 -8 0 14.46 4.70 -11 -8 0 25.04 4.30 11 8 0 23.60 4.74 -11 8 0 22.95 4.56 -11 8 0 23.88 4.78 -12 -8 0 46.55 4.86 -12 -8 0 38.80 5.56 12 8 0 49.09 5.34 -12 8 0 34.95 5.01 -13 -8 0 3.34 4.10 -13 -8 0 8.85 5.04 13 8 0 0.91 4.81 -13 8 0 8.82 4.68 -14 -8 0 10.95 5.58 -14 -8 0 16.39 4.72 -14 8 0 21.59 5.24 14 8 0 32.48 5.75 -15 -8 0 17.75 6.03 -15 -8 0 12.08 4.93 -15 8 0 9.51 5.35 15 8 0 18.40 5.74 -16 -8 0 -2.74 5.90 -16 -8 0 4.29 4.89 -16 8 0 -4.63 4.91 16 8 0 -0.04 5.79 -17 -8 0 4.05 5.33 -17 -8 0 -2.16 6.32 17 8 0 12.02 6.43 -17 8 0 8.83 5.91 -18 -8 0 7.44 6.96 -18 -8 0 16.69 5.99 18 8 0 24.42 7.39 -18 8 0 27.95 6.71 0 -9 0 2.63 1.93 0 9 0 1.23 2.74 0 9 0 2.66 2.82 1 -9 0 29.00 2.22 -1 -9 0 30.19 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