# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1701 data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H51 N3 O3 P Rh' _chemical_formula_weight 719.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9370(18) _cell_length_b 14.420(3) _cell_length_c 15.427(3) _cell_angle_alpha 82.42(3) _cell_angle_beta 88.44(3) _cell_angle_gamma 75.80(3) _cell_volume 1910.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used Fylli _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description 'Plate' _exptl_crystal_colour 'Yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 0.525 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.473 _exptl_absorpt_correction_T_max 0.946 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD system' _diffrn_measurement_method 'w-scan' _diffrn_detector_area_resol_mean 512*512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 15771 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.1289 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 31.66 _reflns_number_total 10954 _reflns_number_gt 4189 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SHELXTL' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+0.0100P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10954 _refine_ls_number_parameters 412 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1857 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1713 _refine_ls_wR_factor_gt 0.1179 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.927 _refine_ls_shift/su_max 0.905 _refine_ls_shift/su_mean 0.058 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh Rh 0.60151(4) 0.82082(3) 0.65141(3) 0.07321(18) Uani 1 d . . . P P 0.55268(11) 0.69917(8) 0.59014(8) 0.0576(3) Uani 1 d . . . O1 O 0.6735(3) 0.8795(2) 0.5354(2) 0.0808(10) Uani 1 d . . . O2 O 0.6449(4) 0.9343(3) 0.7077(3) 0.1084(13) Uani 1 d . . . O3 O 0.5106(7) 0.7359(4) 0.8223(3) 0.149(2) Uani 1 d . . . N1 N 0.8551(5) 0.3008(3) 0.8871(3) 0.0884(12) Uani 1 d . . . N2 N 1.1817(12) 0.0813(6) 0.9010(7) 0.193(4) Uani 1 d . . . N3 N 0.8337(18) 0.4197(12) 1.0894(8) 0.268(6) Uani 1 d . . . C1 C 0.5446(7) 0.7694(5) 0.7534(5) 0.105(2) Uani 1 d . . . C2 C 0.7686(8) 0.9790(4) 0.4270(5) 0.129(2) Uani 1 d . . . H2A H 0.8482 1.0135 0.4252 0.194 Uiso 1 calc R . . H2B H 0.6808 1.0181 0.3939 0.194 Uiso 1 calc R . . H2C H 0.8066 0.9201 0.4022 0.194 Uiso 1 calc R . . C3 C 0.7226(6) 0.9567(4) 0.5189(5) 0.0921(18) Uani 1 d . . . C4 C 0.7363(7) 1.0147(4) 0.5815(7) 0.120(3) Uani 1 d . . . H4 H 0.7760 1.0677 0.5625 0.144 Uiso 1 calc R . . C5 C 0.6978(8) 1.0028(5) 0.6684(7) 0.112(2) Uani 1 d . . . C6 C 0.7176(10) 1.0763(5) 0.7272(6) 0.179(4) Uani 1 d . . . H6A H 0.7510 1.1279 0.6928 0.268 Uiso 1 calc R . . H6B H 0.7934 1.0455 0.7716 0.268 Uiso 1 calc R . . H6C H 0.6209 1.1017 0.7543 0.268 Uiso 1 calc R . . C7 C 0.6537(4) 0.6759(3) 0.4874(3) 0.0585(11) Uani 1 d . . . C8 C 0.6268(5) 0.7485(3) 0.4157(4) 0.0725(13) Uani 1 d . . . H8 H 0.5563 0.8069 0.4206 0.087 Uiso 1 calc R . . C9 C 0.7039(6) 0.7344(4) 0.3375(4) 0.0856(15) Uani 1 d . . . H9 H 0.6847 0.7833 0.2905 0.103 Uiso 1 calc R . . C10 C 0.8073(6) 0.6497(5) 0.3291(4) 0.0876(15) Uani 1 d . . . H10 H 0.8592 0.6407 0.2766 0.105 Uiso 1 calc R . . C11 C 0.8351(5) 0.5774(4) 0.3982(4) 0.0830(15) Uani 1 d . . . H11 H 0.9050 0.5192 0.3920 0.100 Uiso 1 calc R . . C12 C 0.7596(5) 0.5900(3) 0.4778(3) 0.0669(12) Uani 1 d . . . H12 H 0.7805 0.5407 0.5244 0.080 Uiso 1 calc R . . C13 C 0.3508(4) 0.7130(3) 0.5599(3) 0.0561(10) Uani 1 d . . . C14 C 0.2345(5) 0.7628(3) 0.6101(3) 0.0698(12) Uani 1 d . . . H14 H 0.2593 0.7892 0.6581 0.084 Uiso 1 calc R . . C15 C 0.0801(5) 0.7731(3) 0.5882(4) 0.0821(15) Uani 1 d . . . H15 H 0.0023 0.8050 0.6226 0.098 Uiso 1 calc R . . C16 C 0.0418(5) 0.7364(3) 0.5163(4) 0.0823(15) Uani 1 d . . . H16 H -0.0612 0.7443 0.5015 0.099 Uiso 1 calc R . . C17 C 0.1565(5) 0.6884(4) 0.4669(4) 0.0817(14) Uani 1 d . . . H17 H 0.1315 0.6634 0.4182 0.098 Uiso 1 calc R . . C18 C 0.3095(5) 0.6765(3) 0.4887(3) 0.0711(13) Uani 1 d . . . H18 H 0.3862 0.6432 0.4544 0.085 Uiso 1 calc R . . C19 C 0.6054(4) 0.5825(3) 0.6574(3) 0.0575(10) Uani 1 d . . . C20 C 0.5170(5) 0.5147(3) 0.6638(3) 0.0648(11) Uani 1 d . . . H20 H 0.4239 0.5290 0.6335 0.078 Uiso 1 calc R . . C21 C 0.5662(6) 0.4264(3) 0.7145(3) 0.0735(13) Uani 1 d . . . H21 H 0.5056 0.3821 0.7176 0.088 Uiso 1 calc R . . C22 C 0.7032(6) 0.4025(3) 0.7608(3) 0.0695(12) Uani 1 d . . . C23 C 0.7908(5) 0.4697(4) 0.7552(3) 0.0743(13) Uani 1 d . . . H23 H 0.8838 0.4551 0.7856 0.089 Uiso 1 calc R . . C24 C 0.7421(5) 0.5585(3) 0.7049(3) 0.0692(12) Uani 1 d . . . H24 H 0.8022 0.6030 0.7029 0.083 Uiso 1 calc R . . C25 C 0.7576(7) 0.3033(4) 0.8119(4) 0.0898(16) Uani 1 d . . . H25A H 0.6681 0.2800 0.8323 0.108 Uiso 1 calc R . . H25B H 0.8148 0.2596 0.7731 0.108 Uiso 1 calc R . . C26 C 0.9415(7) 0.2023(4) 0.9184(4) 0.108(2) Uani 1 d . . . H26A H 0.8771 0.1580 0.9135 0.130 Uiso 1 calc R . . H26B H 0.9674 0.1982 0.9797 0.130 Uiso 1 calc R . . C27 C 1.0850(9) 0.1732(5) 0.8681(5) 0.147(3) Uani 1 d . . . H27A H 1.0577 0.1717 0.8079 0.177 Uiso 1 calc R . . H27B H 1.1434 0.2218 0.8680 0.177 Uiso 1 calc R . . C28 C 1.212(3) 0.0143(11) 0.8656(14) 0.44(2) Uani 1 d D . . H28A H 1.2621 -0.0313 0.9143 0.528 Uiso 1 calc R . . H28B H 1.2982 0.0299 0.8318 0.528 Uiso 1 calc R . . C29 C 1.186(2) -0.0435(12) 0.8215(10) 0.322(9) Uani 1 d D . . H29A H 1.2754 -0.0965 0.8212 0.483 Uiso 1 calc R . . H29B H 1.1619 -0.0129 0.7627 0.483 Uiso 1 calc R . . H29C H 1.1002 -0.0670 0.8456 0.483 Uiso 1 calc R . . C30 C 1.2582(19) 0.0764(13) 0.9865(15) 0.309(10) Uani 1 d . . . H30A H 1.1792 0.0894 1.0307 0.371 Uiso 1 calc R . . H30B H 1.3200 0.0112 1.0024 0.371 Uiso 1 calc R . . C31 C 1.349(3) 0.1380(15) 0.988(2) 0.54(3) Uani 1 d . . . H31A H 1.2907 0.2026 0.9695 0.817 Uiso 1 calc R . . H31B H 1.4344 0.1216 0.9488 0.817 Uiso 1 calc R . . H31C H 1.3877 0.1338 1.0461 0.817 Uiso 1 calc R . . C32 C 0.7703(8) 0.3489(5) 0.9572(4) 0.117(2) Uani 1 d . . . H32A H 0.7282 0.3034 0.9963 0.141 Uiso 1 calc R . . H32B H 0.6850 0.4007 0.9327 0.141 Uiso 1 calc R . . C33 C 0.8815(9) 0.3914(6) 1.0097(5) 0.137(3) Uani 1 d . . . H33A H 0.9786 0.3431 1.0185 0.165 Uiso 1 calc R . . H33B H 0.9027 0.4466 0.9730 0.165 Uiso 1 calc R . . C34 C 0.869(2) 0.3618(15) 1.1647(15) 0.360(14) Uani 1 d . . . H34A H 0.7893 0.3270 1.1767 0.432 Uiso 1 calc R . . H34B H 0.8648 0.4023 1.2107 0.432 Uiso 1 calc R . . C35 C 1.020(2) 0.2905(13) 1.1717(7) 0.314(10) Uani 1 d . . . H35A H 1.0050 0.2285 1.1956 0.471 Uiso 1 calc R . . H35B H 1.0870 0.3099 1.2092 0.471 Uiso 1 calc R . . H35C H 1.0647 0.2868 1.1146 0.471 Uiso 1 calc R . . C36 C 0.7013(18) 0.4872(14) 1.0983(11) 0.304(11) Uani 1 d . . . H36A H 0.6865 0.4940 1.1598 0.365 Uiso 1 calc R . . H36B H 0.6160 0.4640 1.0793 0.365 Uiso 1 calc R . . C37 C 0.6941(17) 0.5831(10) 1.0495(13) 0.333(12) Uani 1 d . . . H37A H 0.6874 0.6292 1.0900 0.500 Uiso 1 calc R . . H37B H 0.6049 0.6020 1.0121 0.500 Uiso 1 calc R . . H37C H 0.7855 0.5808 1.0148 0.500 Uiso 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 Rh 0.0541(2) 0.0613(2) 0.1101(4) -0.0332(2) -0.0141(2) -0.01200(17) P 0.0389(5) 0.0543(6) 0.0834(8) -0.0197(6) -0.0060(5) -0.0121(5) O1 0.070(2) 0.0536(18) 0.123(3) -0.0152(18) -0.0071(19) -0.0206(16) O2 0.100(3) 0.077(2) 0.158(4) -0.051(2) -0.037(2) -0.017(2) O3 0.185(5) 0.175(5) 0.105(4) -0.051(4) 0.018(4) -0.064(4) N1 0.095(3) 0.083(3) 0.078(3) -0.008(2) -0.014(3) -0.005(2) N2 0.205(8) 0.131(6) 0.189(8) -0.010(6) -0.018(6) 0.060(6) N3 0.286(15) 0.329(16) 0.173(9) -0.092(10) 0.090(10) -0.024(12) C1 0.100(4) 0.119(5) 0.107(5) -0.069(4) -0.008(4) -0.020(4) C2 0.129(5) 0.077(4) 0.180(7) 0.016(4) 0.002(5) -0.038(4) C3 0.062(3) 0.052(3) 0.155(6) -0.002(4) -0.024(3) -0.004(2) C4 0.091(4) 0.057(3) 0.216(9) -0.028(5) -0.046(5) -0.017(3) C5 0.091(4) 0.062(4) 0.191(7) -0.048(5) -0.056(5) -0.012(3) C6 0.205(8) 0.087(4) 0.259(10) -0.068(5) -0.107(7) -0.028(5) C7 0.041(2) 0.060(3) 0.082(3) -0.019(2) -0.004(2) -0.019(2) C8 0.050(2) 0.071(3) 0.098(4) -0.012(3) -0.010(3) -0.016(2) C9 0.068(3) 0.104(4) 0.088(4) -0.009(3) 0.003(3) -0.029(3) C10 0.066(3) 0.115(5) 0.089(4) -0.027(4) 0.012(3) -0.029(3) C11 0.053(3) 0.090(4) 0.109(4) -0.035(4) 0.007(3) -0.012(3) C12 0.047(2) 0.063(3) 0.093(4) -0.020(2) 0.001(2) -0.012(2) C13 0.039(2) 0.047(2) 0.083(3) -0.011(2) -0.002(2) -0.0109(18) C14 0.050(2) 0.070(3) 0.089(3) -0.017(3) -0.003(2) -0.011(2) C15 0.044(2) 0.077(3) 0.122(4) -0.020(3) 0.008(3) -0.006(2) C16 0.042(2) 0.065(3) 0.140(5) -0.005(3) -0.014(3) -0.016(2) C17 0.054(3) 0.086(3) 0.112(4) -0.025(3) -0.019(3) -0.020(3) C18 0.045(2) 0.074(3) 0.100(4) -0.030(3) -0.004(2) -0.015(2) C19 0.044(2) 0.059(2) 0.072(3) -0.017(2) -0.005(2) -0.0103(19) C20 0.056(2) 0.064(3) 0.078(3) -0.015(2) -0.009(2) -0.020(2) C21 0.078(3) 0.071(3) 0.082(3) -0.014(3) -0.011(3) -0.034(3) C22 0.080(3) 0.059(3) 0.071(3) -0.016(2) -0.008(3) -0.015(2) C23 0.054(3) 0.077(3) 0.090(4) -0.016(3) -0.020(2) -0.008(2) C24 0.053(2) 0.064(3) 0.095(4) -0.017(3) -0.016(2) -0.018(2) C25 0.107(4) 0.071(3) 0.092(4) -0.011(3) -0.020(3) -0.020(3) C26 0.113(5) 0.089(4) 0.102(4) 0.014(3) -0.006(4) 0.003(4) C27 0.127(6) 0.120(6) 0.156(7) 0.014(5) 0.011(5) 0.027(5) C28 0.73(5) 0.152(12) 0.36(3) -0.129(14) -0.17(3) 0.107(19) C29 0.39(2) 0.31(2) 0.312(19) -0.158(16) 0.128(17) -0.120(17) C30 0.207(16) 0.226(19) 0.41(3) 0.008(19) -0.048(17) 0.088(13) C31 0.41(3) 0.29(2) 0.92(6) 0.08(3) -0.41(4) -0.09(2) C32 0.111(5) 0.133(5) 0.097(5) -0.022(4) -0.006(4) -0.004(4) C33 0.130(6) 0.178(7) 0.107(6) -0.039(5) -0.013(5) -0.031(5) C34 0.27(2) 0.41(3) 0.31(2) 0.10(2) 0.11(2) -0.009(19) C35 0.33(2) 0.54(3) 0.120(8) -0.008(13) -0.056(11) -0.22(2) C36 0.213(14) 0.39(3) 0.31(2) -0.19(2) 0.095(15) -0.006(17) C37 0.159(11) 0.247(17) 0.60(4) -0.038(19) 0.056(16) -0.078(13) _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 Rh C1 1.765(8) . ? Rh O1 2.034(4) . ? Rh O2 2.070(4) . ? Rh P 2.2352(12) . ? P C19 1.818(4) . ? P C7 1.832(4) . ? P C13 1.832(4) . ? O1 C3 1.286(6) . ? O2 C5 1.274(8) . ? O3 C1 1.172(7) . ? N1 C32 1.457(7) . ? N1 C25 1.460(6) . ? N1 C26 1.466(6) . ? N2 C28 1.145(14) . ? N2 C27 1.430(9) . ? N2 C30 1.49(2) . ? N3 C34 1.334(18) . ? N3 C36 1.352(17) . ? N3 C33 1.371(10) . ? C2 C3 1.483(8) . ? C3 C4 1.384(9) . ? C4 C5 1.375(9) . ? C5 C6 1.527(8) . ? C7 C12 1.384(6) . ? C7 C8 1.400(6) . ? C8 C9 1.386(6) . ? C9 C10 1.358(7) . ? C10 C11 1.371(7) . ? C11 C12 1.396(6) . ? C13 C18 1.376(6) . ? C13 C14 1.390(6) . ? C14 C15 1.398(6) . ? C15 C16 1.375(7) . ? C16 C17 1.363(7) . ? C17 C18 1.381(6) . ? C19 C24 1.386(6) . ? C19 C20 1.392(5) . ? C20 C21 1.381(6) . ? C21 C22 1.379(6) . ? C22 C23 1.381(6) . ? C22 C25 1.512(6) . ? C23 C24 1.383(6) . ? C26 C27 1.480(8) . ? C28 C29 1.212(14) . ? C30 C31 1.35(2) . ? C32 C33 1.579(9) . ? C34 C35 1.48(2) . ? C36 C37 1.473(19) . ? 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 Rh O1 178.3(2) . . ? C1 Rh O2 90.9(2) . . ? O1 Rh O2 88.30(16) . . ? C1 Rh P 89.17(19) . . ? O1 Rh P 91.61(10) . . ? O2 Rh P 179.49(10) . . ? C19 P C7 103.14(19) . . ? C19 P C13 104.40(18) . . ? C7 P C13 102.38(19) . . ? C19 P Rh 114.51(14) . . ? C7 P Rh 115.21(13) . . ? C13 P Rh 115.57(14) . . ? C3 O1 Rh 128.5(4) . . ? C5 O2 Rh 125.9(4) . . ? C32 N1 C25 112.8(5) . . ? C32 N1 C26 112.0(4) . . ? C25 N1 C26 111.7(5) . . ? C28 N2 C27 126.2(15) . . ? C28 N2 C30 117.9(14) . . ? C27 N2 C30 115.8(10) . . ? C34 N3 C36 109.9(13) . . ? C34 N3 C33 123.0(18) . . ? C36 N3 C33 121.7(15) . . ? O3 C1 Rh 178.0(6) . . ? O1 C3 C4 123.7(7) . . ? O1 C3 C2 115.1(6) . . ? C4 C3 C2 121.2(6) . . ? C5 C4 C3 127.4(7) . . ? O2 C5 C4 126.3(6) . . ? O2 C5 C6 114.0(8) . . ? C4 C5 C6 119.8(7) . . ? C12 C7 C8 118.1(4) . . ? C12 C7 P 122.7(4) . . ? C8 C7 P 119.1(3) . . ? C9 C8 C7 120.8(5) . . ? C10 C9 C8 120.5(5) . . ? C9 C10 C11 119.8(5) . . ? C10 C11 C12 120.8(5) . . ? C7 C12 C11 120.0(5) . . ? C18 C13 C14 118.4(4) . . ? C18 C13 P 122.4(3) . . ? C14 C13 P 119.2(3) . . ? C13 C14 C15 119.7(5) . . ? C16 C15 C14 120.8(5) . . ? C17 C16 C15 119.2(4) . . ? C16 C17 C18 120.6(5) . . ? C13 C18 C17 121.3(4) . . ? C24 C19 C20 117.5(4) . . ? C24 C19 P 118.7(3) . . ? C20 C19 P 123.8(3) . . ? C21 C20 C19 120.7(4) . . ? C22 C21 C20 121.5(4) . . ? C21 C22 C23 118.0(4) . . ? C21 C22 C25 120.2(4) . . ? C23 C22 C25 121.8(5) . . ? C22 C23 C24 120.9(4) . . ? C23 C24 C19 121.4(4) . . ? N1 C25 C22 113.9(4) . . ? N1 C26 C27 111.7(5) . . ? N2 C27 C26 114.2(6) . . ? N2 C28 C29 155(3) . . ? C31 C30 N2 115(2) . . ? N1 C32 C33 109.8(5) . . ? N3 C33 C32 118.2(8) . . ? N3 C34 C35 118.1(17) . . ? N3 C36 C37 115.5(16) . . ? _diffrn_measured_fraction_theta_max 0.851 _diffrn_reflns_theta_full 31.66 _diffrn_measured_fraction_theta_full 0.851 _refine_diff_density_max 0.441 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.091