# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_l2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H44 N3' _chemical_formula_weight 482.71 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.228(3) _cell_length_b 21.695(4) _cell_length_c 9.1700(18) _cell_angle_alpha 90.00 _cell_angle_beta 94.70(3) _cell_angle_gamma 90.00 _cell_volume 3019.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4528 _cell_measurement_theta_min 1.34 _cell_measurement_theta_max 24.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.062 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 0.062 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9662 _exptl_absorpt_correction_T_max 0.9898 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4528 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0872 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 24.00 _reflns_number_total 4528 _reflns_number_gt 2060 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4528 _refine_ls_number_parameters 325 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1208 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1845 _refine_ls_wR_factor_gt 0.1596 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.002 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.08859(17) 0.38145(14) 0.7898(3) 0.0506(8) Uani 1 1 d . . . N2 N 0.25332(17) 0.49203(13) 0.7378(3) 0.0415(7) Uani 1 1 d . . . H2A H 0.2342 0.5209 0.7909 0.050 Uiso 1 1 calc R . . N3 N 0.44393(18) 0.56787(12) 0.6339(3) 0.0434(7) Uani 1 1 d . . . C1 C 0.1277(2) 0.43295(18) 0.8011(4) 0.0449(9) Uani 1 1 d . . . C2 C 0.2098(2) 0.43879(17) 0.7234(4) 0.0422(9) Uani 1 1 d . . . C3 C 0.2392(2) 0.39167(18) 0.6395(4) 0.0570(10) Uani 1 1 d . . . H3B H 0.2085 0.3547 0.6304 0.068 Uiso 1 1 calc R . . C4 C 0.3146(2) 0.40000(19) 0.5696(4) 0.0651(12) Uani 1 1 d . . . H4A H 0.3358 0.3686 0.5130 0.078 Uiso 1 1 calc R . . C5 C 0.3584(2) 0.45541(17) 0.5844(4) 0.0521(10) Uani 1 1 d . . . H5A H 0.4091 0.4622 0.5367 0.063 Uiso 1 1 calc R . . C6 C 0.3264(2) 0.50048(16) 0.6701(3) 0.0393(8) Uani 1 1 d . . . C7 C 0.3727(2) 0.56035(16) 0.6952(4) 0.0418(9) Uani 1 1 d . . . C8 C 0.0992(2) 0.48724(18) 0.8849(5) 0.0750(13) Uani 1 1 d . . . H8A H 0.0457 0.4775 0.9286 0.112 Uiso 1 1 calc R . . H8B H 0.0891 0.5217 0.8199 0.112 Uiso 1 1 calc R . . H8C H 0.1444 0.4976 0.9601 0.112 Uiso 1 1 calc R . . C9 C 0.3322(2) 0.60664(18) 0.7908(5) 0.0696(12) Uani 1 1 d . . . H9A H 0.3680 0.6431 0.7977 0.104 Uiso 1 1 calc R . . H9B H 0.3286 0.5895 0.8866 0.104 Uiso 1 1 calc R . . H9C H 0.2742 0.6169 0.7492 0.104 Uiso 1 1 calc R . . C10 C 0.0081(2) 0.36988(17) 0.8553(4) 0.0528(10) Uani 1 1 d . . . C11 C -0.0708(3) 0.3776(2) 0.7705(5) 0.0732(13) Uani 1 1 d . . . C12 C -0.1487(3) 0.3614(3) 0.8333(7) 0.1033(18) Uani 1 1 d . . . H12A H -0.2028 0.3675 0.7805 0.124 Uiso 1 1 calc R . . C13 C -0.1461(4) 0.3368(3) 0.9711(7) 0.1032(18) Uani 1 1 d . . . H13A H -0.1981 0.3253 1.0101 0.124 Uiso 1 1 calc R . . C14 C -0.0679(3) 0.3293(2) 1.0508(5) 0.0889(15) Uani 1 1 d . . . H14A H -0.0674 0.3130 1.1447 0.107 Uiso 1 1 calc R . . C15 C 0.0116(3) 0.34511(19) 0.9963(5) 0.0624(11) Uani 1 1 d . . . C16 C -0.0723(3) 0.4013(3) 0.6140(6) 0.1040(18) Uani 1 1 d . . . H16A H -0.0112 0.4066 0.5899 0.125 Uiso 1 1 calc R . . C17 C -0.1167(5) 0.4634(4) 0.6053(9) 0.194(3) Uani 1 1 d U . . H17A H -0.1164 0.4792 0.5075 0.292 Uiso 1 1 calc R . . H17B H -0.0856 0.4913 0.6724 0.292 Uiso 1 1 calc R . . H17C H -0.1764 0.4593 0.6303 0.292 Uiso 1 1 calc R . . C18 C -0.1175(5) 0.3584(3) 0.5031(7) 0.163(3) Uani 1 1 d . . . H18A H -0.0882 0.3192 0.5077 0.244 Uiso 1 1 calc R . . H18B H -0.1155 0.3756 0.4070 0.244 Uiso 1 1 calc R . . H18C H -0.1778 0.3531 0.5239 0.244 Uiso 1 1 calc R . . C19 C 0.0972(3) 0.3361(2) 1.0859(5) 0.0771(13) Uani 1 1 d . . . H19A H 0.1415 0.3610 1.0412 0.093 Uiso 1 1 calc R . . C20 C 0.0962(4) 0.3567(4) 1.2427(6) 0.160(3) Uani 1 1 d . . . H20A H 0.1532 0.3498 1.2930 0.240 Uiso 1 1 calc R . . H20B H 0.0527 0.3336 1.2896 0.240 Uiso 1 1 calc R . . H20C H 0.0822 0.3998 1.2454 0.240 Uiso 1 1 calc R . . C21 C 0.1258(4) 0.2709(3) 1.0806(8) 0.159(3) Uani 1 1 d U . . H21A H 0.1274 0.2583 0.9805 0.239 Uiso 1 1 calc R . . H21B H 0.0851 0.2454 1.1277 0.239 Uiso 1 1 calc R . . H21C H 0.1835 0.2668 1.1302 0.239 Uiso 1 1 calc R . . C22 C 0.4940(2) 0.62308(16) 0.6521(4) 0.0448(9) Uani 1 1 d . . . C23 C 0.4759(2) 0.67245(17) 0.5563(4) 0.0504(10) Uani 1 1 d . . . C24 C 0.5309(3) 0.72348(19) 0.5703(5) 0.0662(12) Uani 1 1 d . . . H24A H 0.5204 0.7569 0.5078 0.079 Uiso 1 1 calc R . . C25 C 0.6009(3) 0.7254(2) 0.6754(5) 0.0726(13) Uani 1 1 d . . . H25A H 0.6368 0.7602 0.6831 0.087 Uiso 1 1 calc R . . C26 C 0.6182(3) 0.6768(2) 0.7686(4) 0.0671(12) Uani 1 1 d . . . H26A H 0.6652 0.6791 0.8397 0.080 Uiso 1 1 calc R . . C27 C 0.5661(2) 0.62407(19) 0.7582(4) 0.0533(10) Uani 1 1 d . . . C28 C 0.3997(2) 0.66931(18) 0.4384(4) 0.0610(11) Uani 1 1 d . . . H28A H 0.3526 0.6455 0.4786 0.073 Uiso 1 1 calc R . . C29 C 0.4267(3) 0.6345(2) 0.3054(5) 0.1003(17) Uani 1 1 d . . . H29A H 0.4503 0.5950 0.3353 0.150 Uiso 1 1 calc R . . H29B H 0.4707 0.6577 0.2599 0.150 Uiso 1 1 calc R . . H29C H 0.3762 0.6288 0.2369 0.150 Uiso 1 1 calc R . . C30 C 0.3616(3) 0.7316(2) 0.3934(6) 0.1160(19) Uani 1 1 d . . . H30A H 0.3432 0.7525 0.4780 0.174 Uiso 1 1 calc R . . H30B H 0.3118 0.7260 0.3234 0.174 Uiso 1 1 calc R . . H30C H 0.4056 0.7557 0.3504 0.174 Uiso 1 1 calc R . . C31 C 0.5858(3) 0.5693(2) 0.8579(4) 0.0703(13) Uani 1 1 d . . . H31A H 0.5454 0.5363 0.8230 0.084 Uiso 1 1 calc R . . C32 C 0.6787(3) 0.5442(3) 0.8512(6) 0.128(2) Uani 1 1 d . . . H32A H 0.6893 0.5360 0.7512 0.193 Uiso 1 1 calc R . . H32B H 0.6849 0.5067 0.9067 0.193 Uiso 1 1 calc R . . H32C H 0.7206 0.5740 0.8914 0.193 Uiso 1 1 calc R . . C33 C 0.5672(4) 0.5827(3) 1.0125(5) 0.149(3) Uani 1 1 d . . . H33A H 0.5079 0.5974 1.0144 0.223 Uiso 1 1 calc R . . H33B H 0.6075 0.6135 1.0527 0.223 Uiso 1 1 calc R . . H33C H 0.5742 0.5457 1.0697 0.223 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 N1 0.0416(17) 0.051(2) 0.061(2) 0.0029(17) 0.0123(15) -0.0059(16) N2 0.0461(16) 0.0361(19) 0.0445(17) -0.0052(14) 0.0161(14) 0.0057(14) N3 0.0450(17) 0.0392(19) 0.0473(17) 0.0014(15) 0.0121(15) -0.0018(15) C1 0.041(2) 0.044(2) 0.051(2) 0.001(2) 0.0117(18) 0.0001(19) C2 0.044(2) 0.039(2) 0.044(2) -0.0003(18) 0.0071(17) -0.0010(18) C3 0.056(2) 0.046(3) 0.071(3) -0.010(2) 0.021(2) -0.012(2) C4 0.065(3) 0.057(3) 0.078(3) -0.024(2) 0.036(2) -0.008(2) C5 0.051(2) 0.049(3) 0.060(2) -0.009(2) 0.0212(19) -0.008(2) C6 0.0373(18) 0.042(2) 0.0395(19) 0.0023(18) 0.0087(17) 0.0035(17) C7 0.044(2) 0.039(2) 0.043(2) 0.0016(18) 0.0120(18) -0.0004(18) C8 0.066(3) 0.061(3) 0.104(3) -0.012(3) 0.043(2) -0.004(2) C9 0.073(3) 0.050(3) 0.090(3) -0.021(2) 0.040(2) -0.013(2) C10 0.044(2) 0.045(3) 0.071(3) 0.001(2) 0.019(2) -0.0071(19) C11 0.045(2) 0.082(3) 0.093(3) 0.016(3) 0.013(2) -0.005(2) C12 0.051(3) 0.117(5) 0.144(5) 0.011(4) 0.018(3) -0.015(3) C13 0.075(4) 0.103(5) 0.138(5) -0.009(4) 0.050(4) -0.033(3) C14 0.094(4) 0.092(4) 0.086(3) 0.001(3) 0.040(3) -0.027(3) C15 0.062(3) 0.057(3) 0.070(3) 0.002(2) 0.019(2) -0.014(2) C16 0.051(3) 0.131(5) 0.126(5) 0.040(4) -0.018(3) 0.002(3) C17 0.196(3) 0.194(3) 0.193(3) 0.0013(10) 0.0141(11) 0.0010(10) C18 0.192(7) 0.186(8) 0.111(5) -0.018(5) 0.016(5) -0.028(6) C19 0.095(3) 0.061(3) 0.076(3) 0.013(3) 0.014(3) -0.014(3) C20 0.156(6) 0.231(8) 0.090(4) -0.041(5) -0.010(4) 0.003(5) C21 0.158(3) 0.158(3) 0.161(3) -0.0009(10) 0.0093(10) 0.0011(10) C22 0.048(2) 0.038(2) 0.052(2) -0.0044(19) 0.0207(19) -0.0040(18) C23 0.054(2) 0.038(2) 0.063(2) 0.001(2) 0.025(2) -0.002(2) C24 0.077(3) 0.046(3) 0.080(3) 0.002(2) 0.031(3) -0.005(2) C25 0.077(3) 0.051(3) 0.093(3) -0.015(3) 0.032(3) -0.020(2) C26 0.066(3) 0.077(3) 0.061(3) -0.018(3) 0.017(2) -0.021(3) C27 0.052(2) 0.059(3) 0.051(2) -0.009(2) 0.015(2) -0.008(2) C28 0.062(2) 0.053(3) 0.070(3) 0.018(2) 0.012(2) 0.004(2) C29 0.099(4) 0.127(5) 0.074(3) -0.018(3) 0.001(3) 0.007(3) C30 0.120(4) 0.074(4) 0.149(5) 0.029(4) -0.012(4) 0.024(3) C31 0.064(3) 0.083(3) 0.062(3) 0.014(3) -0.008(2) -0.018(2) C32 0.120(5) 0.129(5) 0.141(5) 0.041(4) 0.036(4) 0.049(4) C33 0.199(7) 0.181(7) 0.070(4) 0.040(4) 0.034(4) 0.058(5) _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 N1 C1 1.266(4) . ? N1 C10 1.430(4) . ? N2 C6 1.331(4) . ? N2 C2 1.333(4) . ? N3 C7 1.272(4) . ? N3 C22 1.422(4) . ? C1 C8 1.490(5) . ? C1 C2 1.495(4) . ? C2 C3 1.376(5) . ? C3 C4 1.372(5) . ? C4 C5 1.376(5) . ? C5 C6 1.369(4) . ? C6 C7 1.487(4) . ? C7 C9 1.498(5) . ? C10 C11 1.387(5) . ? C10 C15 1.398(5) . ? C11 C12 1.405(6) . ? C11 C16 1.523(6) . ? C12 C13 1.369(7) . ? C13 C14 1.355(6) . ? C14 C15 1.389(5) . ? C15 C19 1.496(5) . ? C16 C18 1.502(7) . ? C16 C17 1.508(8) . ? C19 C21 1.481(7) . ? C19 C20 1.506(6) . ? C22 C23 1.398(5) . ? C22 C27 1.406(5) . ? C23 C24 1.388(5) . ? C23 C28 1.521(5) . ? C24 C25 1.378(5) . ? C25 C26 1.369(6) . ? C26 C27 1.391(5) . ? C27 C31 1.514(5) . ? C28 C30 1.514(5) . ? C28 C29 1.520(5) . ? C31 C33 1.498(6) . ? C31 C32 1.522(6) . ? 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 N1 C10 122.2(3) . . ? C6 N2 C2 120.1(3) . . ? C7 N3 C22 121.6(3) . . ? N1 C1 C8 125.8(3) . . ? N1 C1 C2 116.2(3) . . ? C8 C1 C2 118.0(3) . . ? N2 C2 C3 121.1(3) . . ? N2 C2 C1 117.1(3) . . ? C3 C2 C1 121.8(3) . . ? C4 C3 C2 119.1(3) . . ? C3 C4 C5 119.1(4) . . ? C6 C5 C4 119.2(3) . . ? N2 C6 C5 121.3(3) . . ? N2 C6 C7 116.9(3) . . ? C5 C6 C7 121.8(3) . . ? N3 C7 C6 117.0(3) . . ? N3 C7 C9 125.4(3) . . ? C6 C7 C9 117.6(3) . . ? C11 C10 C15 122.0(3) . . ? C11 C10 N1 118.5(4) . . ? C15 C10 N1 119.2(3) . . ? C10 C11 C12 117.5(4) . . ? C10 C11 C16 120.9(4) . . ? C12 C11 C16 121.5(4) . . ? C13 C12 C11 120.9(5) . . ? C14 C13 C12 120.1(5) . . ? C13 C14 C15 121.9(5) . . ? C14 C15 C10 117.4(4) . . ? C14 C15 C19 121.0(4) . . ? C10 C15 C19 121.6(3) . . ? C18 C16 C17 109.8(5) . . ? C18 C16 C11 113.6(5) . . ? C17 C16 C11 108.8(5) . . ? C21 C19 C15 110.6(4) . . ? C21 C19 C20 109.9(5) . . ? C15 C19 C20 114.2(4) . . ? C23 C22 C27 121.7(3) . . ? C23 C22 N3 119.7(3) . . ? C27 C22 N3 118.3(3) . . ? C24 C23 C22 117.8(4) . . ? C24 C23 C28 121.4(4) . . ? C22 C23 C28 120.8(3) . . ? C25 C24 C23 121.1(4) . . ? C26 C25 C24 120.7(4) . . ? C25 C26 C27 120.8(4) . . ? C26 C27 C22 117.9(4) . . ? C26 C27 C31 121.4(4) . . ? C22 C27 C31 120.7(3) . . ? C30 C28 C29 110.4(4) . . ? C30 C28 C23 114.0(4) . . ? C29 C28 C23 110.6(3) . . ? C33 C31 C27 112.1(4) . . ? C33 C31 C32 110.9(4) . . ? C27 C31 C32 113.3(4) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.381 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.055 _database_code_depnum_ccdc_archive 'CCDC 952322' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(I) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H35 N3' _chemical_formula_sum 'C29 H35 N3' _chemical_formula_weight 425.60 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.9390(8) _cell_length_b 12.3208(13) _cell_length_c 25.998(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.234(2) _cell_angle_gamma 90.00 _cell_volume 2528.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13906 _cell_measurement_theta_min 1.58 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 0.066 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9832 _exptl_absorpt_correction_T_max 0.9870 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 13906 _diffrn_reflns_av_R_equivalents 0.0770 _diffrn_reflns_av_sigmaI/netI 0.1092 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 26.02 _reflns_number_total 4938 _reflns_number_gt 2362 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4938 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1315 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1012 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.000 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N -0.5544(2) 0.61937(15) -0.15400(7) 0.0377(5) Uani 1 1 d . . . N2 N -0.2647(2) 0.69242(15) -0.04651(7) 0.0342(5) Uani 1 1 d . . . N3 N 0.0206(2) 0.83861(14) 0.04282(7) 0.0328(5) Uani 1 1 d . . . C1 C -0.4636(3) 0.60967(19) -0.11083(9) 0.0353(6) Uani 1 1 d . . . C2 C -0.3645(3) 0.70650(19) -0.09065(9) 0.0315(6) Uani 1 1 d . . . C3 C -0.3771(3) 0.80441(18) -0.11695(9) 0.0379(7) Uani 1 1 d . . . H3B H -0.4480 0.8113 -0.1477 0.045 Uiso 1 1 calc R . . C4 C -0.2830(3) 0.89137(19) -0.09692(9) 0.0401(7) Uani 1 1 d . . . H4A H -0.2893 0.9580 -0.1139 0.048 Uiso 1 1 calc R . . C5 C -0.1790(3) 0.87807(18) -0.05110(9) 0.0346(6) Uani 1 1 d . . . H5A H -0.1140 0.9355 -0.0367 0.041 Uiso 1 1 calc R . . C6 C -0.1734(3) 0.77816(18) -0.02709(9) 0.0321(6) Uani 1 1 d . . . C7 C -0.0646(3) 0.75836(19) 0.02294(9) 0.0328(6) Uani 1 1 d . . . C8 C -0.4473(3) 0.50849(18) -0.07891(9) 0.0551(8) Uani 1 1 d . . . H8A H -0.5166 0.4524 -0.0959 0.083 Uiso 1 1 calc R . . H8B H -0.4837 0.5227 -0.0455 0.083 Uiso 1 1 calc R . . H8C H -0.3311 0.4854 -0.0748 0.083 Uiso 1 1 calc R . . C9 C -0.0684(3) 0.64705(18) 0.04624(9) 0.0516(8) Uani 1 1 d . . . H9A H 0.0057 0.6450 0.0780 0.077 Uiso 1 1 calc R . . H9B H -0.0314 0.5947 0.0225 0.077 Uiso 1 1 calc R . . H9C H -0.1818 0.6302 0.0531 0.077 Uiso 1 1 calc R . . C10 C -0.6522(3) 0.52973(18) -0.17576(9) 0.0350(6) Uani 1 1 d . . . C11 C -0.5797(3) 0.46024(19) -0.20928(9) 0.0354(6) Uani 1 1 d . . . C12 C -0.6793(3) 0.3774(2) -0.23284(9) 0.0460(7) Uani 1 1 d . . . H12A H -0.6339 0.3312 -0.2560 0.055 Uiso 1 1 calc R . . C13 C -0.8439(4) 0.3630(2) -0.22238(10) 0.0529(8) Uani 1 1 d . . . H13A H -0.9089 0.3071 -0.2382 0.063 Uiso 1 1 calc R . . C14 C -0.9118(3) 0.4313(2) -0.18850(10) 0.0531(8) Uani 1 1 d . . . H14A H -1.0227 0.4202 -0.1813 0.064 Uiso 1 1 calc R . . C15 C -0.8197(3) 0.5162(2) -0.16479(10) 0.0442(7) Uani 1 1 d . . . C16 C -0.3966(3) 0.4759(2) -0.21860(9) 0.0542(8) Uani 1 1 d . . . H16A H -0.3738 0.5533 -0.2186 0.065 Uiso 1 1 calc R . . H16B H -0.3261 0.4447 -0.1895 0.065 Uiso 1 1 calc R . . C17 C -0.3415(3) 0.4290(2) -0.26723(10) 0.0677(9) Uani 1 1 d . . . H17A H -0.2233 0.4437 -0.2685 0.102 Uiso 1 1 calc R . . H17B H -0.4061 0.4613 -0.2967 0.102 Uiso 1 1 calc R . . H17C H -0.3599 0.3520 -0.2677 0.102 Uiso 1 1 calc R . . C18 C -0.8989(3) 0.5920(2) -0.12862(10) 0.0595(8) Uani 1 1 d . . . H18A H -0.9946 0.5565 -0.1155 0.071 Uiso 1 1 calc R . . H18B H -0.8167 0.6094 -0.0994 0.071 Uiso 1 1 calc R . . C19 C -0.9567(4) 0.6936(2) -0.15592(11) 0.0843(11) Uani 1 1 d . . . H19A H -1.0065 0.7408 -0.1324 0.126 Uiso 1 1 calc R . . H19B H -1.0392 0.6764 -0.1845 0.126 Uiso 1 1 calc R . . H19C H -0.8616 0.7292 -0.1685 0.126 Uiso 1 1 calc R . . C20 C 0.1215(3) 0.82874(17) 0.09135(9) 0.0314(6) Uani 1 1 d . . . C21 C 0.2917(3) 0.79922(18) 0.09253(10) 0.0366(6) Uani 1 1 d . . . C22 C 0.3912(3) 0.80093(19) 0.14006(11) 0.0481(7) Uani 1 1 d . . . H22A H 0.5045 0.7806 0.1417 0.058 Uiso 1 1 calc R . . C23 C 0.3256(4) 0.8321(2) 0.18473(11) 0.0512(8) Uani 1 1 d . . . H23A H 0.3947 0.8347 0.2160 0.061 Uiso 1 1 calc R . . C24 C 0.1569(4) 0.85952(19) 0.18268(10) 0.0466(7) Uani 1 1 d . . . H24A H 0.1129 0.8799 0.2130 0.056 Uiso 1 1 calc R . . C25 C 0.0504(3) 0.85759(18) 0.13639(9) 0.0367(6) Uani 1 1 d . . . C26 C 0.3694(3) 0.76989(19) 0.04370(9) 0.0458(7) Uani 1 1 d . . . H26A H 0.2924 0.7225 0.0227 0.055 Uiso 1 1 calc R . . H26B H 0.4738 0.7302 0.0530 0.055 Uiso 1 1 calc R . . C27 C 0.4070(3) 0.86848(19) 0.01206(10) 0.0595(8) Uani 1 1 d . . . H27A H 0.4547 0.8456 -0.0185 0.089 Uiso 1 1 calc R . . H27B H 0.4862 0.9146 0.0323 0.089 Uiso 1 1 calc R . . H27C H 0.3040 0.9077 0.0024 0.089 Uiso 1 1 calc R . . C28 C -0.1336(3) 0.8865(2) 0.13489(9) 0.0482(7) Uani 1 1 d . . . H28A H -0.1670 0.8812 0.1696 0.058 Uiso 1 1 calc R . . H28B H -0.1999 0.8342 0.1134 0.058 Uiso 1 1 calc R . . C29 C -0.1747(4) 0.9995(2) 0.11419(10) 0.0685(9) Uani 1 1 d . . . H29A H -0.2938 1.0131 0.1142 0.103 Uiso 1 1 calc R . . H29B H -0.1447 1.0051 0.0795 0.103 Uiso 1 1 calc R . . H29C H -0.1117 1.0520 0.1357 0.103 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 N1 0.0406(14) 0.0347(13) 0.0358(13) -0.0046(10) -0.0047(11) -0.0017(10) N2 0.0406(14) 0.0297(12) 0.0312(12) -0.0022(10) -0.0010(10) -0.0026(10) N3 0.0371(13) 0.0301(12) 0.0309(12) -0.0034(10) 0.0030(10) -0.0024(10) C1 0.0411(17) 0.0318(15) 0.0320(15) -0.0012(12) -0.0001(13) 0.0018(12) C2 0.0369(16) 0.0278(15) 0.0293(15) -0.0022(12) 0.0020(12) 0.0002(12) C3 0.0455(18) 0.0329(15) 0.0340(15) -0.0007(13) -0.0009(13) -0.0013(13) C4 0.0536(18) 0.0265(15) 0.0396(16) 0.0026(12) 0.0026(14) -0.0012(13) C5 0.0408(16) 0.0291(15) 0.0337(15) -0.0028(12) 0.0029(13) -0.0042(12) C6 0.0357(16) 0.0269(14) 0.0337(15) -0.0011(12) 0.0044(12) -0.0014(12) C7 0.0369(16) 0.0295(15) 0.0318(15) 0.0007(12) 0.0039(13) -0.0001(12) C8 0.072(2) 0.0370(16) 0.0509(18) 0.0078(14) -0.0163(16) -0.0122(15) C9 0.064(2) 0.0381(16) 0.0479(17) 0.0096(14) -0.0170(15) -0.0114(14) C10 0.0386(17) 0.0332(15) 0.0311(15) 0.0008(12) -0.0057(13) -0.0026(13) C11 0.0316(16) 0.0389(16) 0.0344(15) -0.0005(13) -0.0021(13) -0.0021(13) C12 0.053(2) 0.0466(17) 0.0372(16) -0.0079(13) -0.0017(14) -0.0019(15) C13 0.052(2) 0.055(2) 0.0492(18) -0.0064(15) -0.0035(16) -0.0161(16) C14 0.0335(18) 0.071(2) 0.0537(19) -0.0030(17) 0.0004(15) -0.0119(16) C15 0.0375(18) 0.0504(18) 0.0439(17) -0.0038(14) 0.0000(14) 0.0016(14) C16 0.0444(19) 0.071(2) 0.0471(18) -0.0214(15) 0.0047(14) 0.0011(15) C17 0.063(2) 0.087(2) 0.054(2) -0.0043(17) 0.0091(16) 0.0008(18) C18 0.049(2) 0.061(2) 0.070(2) 0.0072(17) 0.0126(16) 0.0079(16) C19 0.110(3) 0.054(2) 0.096(3) 0.006(2) 0.042(2) 0.007(2) C20 0.0345(16) 0.0256(14) 0.0327(15) 0.0009(11) -0.0028(13) -0.0062(12) C21 0.0391(17) 0.0291(15) 0.0410(16) 0.0062(12) 0.0016(14) -0.0041(12) C22 0.0389(18) 0.0431(17) 0.060(2) 0.0111(15) -0.0057(16) -0.0043(13) C23 0.056(2) 0.0497(18) 0.0442(19) 0.0052(15) -0.0113(16) -0.0110(16) C24 0.062(2) 0.0439(17) 0.0340(16) -0.0012(13) 0.0035(15) -0.0109(15) C25 0.0407(17) 0.0341(15) 0.0351(16) 0.0008(12) 0.0038(14) -0.0057(13) C26 0.0416(18) 0.0397(16) 0.0567(18) 0.0047(14) 0.0072(14) 0.0045(13) C27 0.070(2) 0.0473(18) 0.066(2) 0.0120(15) 0.0282(17) 0.0092(15) C28 0.051(2) 0.0554(19) 0.0396(16) -0.0067(14) 0.0118(14) -0.0051(15) C29 0.064(2) 0.076(2) 0.068(2) 0.0168(18) 0.0232(17) 0.0192(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.272(3) . yes N1 C10 1.431(3) . yes N2 C2 1.333(2) . yes N2 C6 1.348(2) . yes N3 C7 1.275(2) . yes N3 C20 1.424(3) . yes C1 C2 1.493(3) . ? C1 C8 1.495(3) . ? C2 C3 1.385(3) . ? C3 C4 1.376(3) . ? C3 H3B 0.9300 . ? C4 C5 1.383(3) . ? C4 H4A 0.9300 . ? C5 C6 1.379(3) . ? C5 H5A 0.9300 . ? C6 C7 1.501(3) . ? C7 C9 1.501(3) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.390(3) . ? C10 C15 1.399(3) . ? C11 C12 1.391(3) . ? C11 C16 1.511(3) . ? C12 C13 1.375(3) . ? C12 H12A 0.9300 . ? C13 C14 1.370(3) . ? C13 H13A 0.9300 . ? C14 C15 1.383(3) . ? C14 H14A 0.9300 . ? C15 C18 1.511(3) . ? C16 C17 1.498(3) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.486(3) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.397(3) . ? C20 C25 1.400(3) . ? C21 C22 1.393(3) . ? C21 C26 1.514(3) . ? C22 C23 1.378(3) . ? C22 H22A 0.9300 . ? C23 C24 1.376(3) . ? C23 H23A 0.9300 . ? C24 C25 1.394(3) . ? C24 H24A 0.9300 . ? C25 C28 1.500(3) . ? C26 C27 1.515(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.515(3) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? 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 N1 C10 120.5(2) . . ? C2 N2 C6 117.7(2) . . ? C7 N3 C20 121.0(2) . . ? N1 C1 C2 117.5(2) . . ? N1 C1 C8 125.1(2) . . ? C2 C1 C8 117.4(2) . . ? N2 C2 C3 122.9(2) . . ? N2 C2 C1 116.1(2) . . ? C3 C2 C1 121.0(2) . . ? C4 C3 C2 119.0(2) . . ? C4 C3 H3B 120.5 . . ? C2 C3 H3B 120.5 . . ? C3 C4 C5 118.8(2) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? C6 C5 C4 118.9(2) . . ? C6 C5 H5A 120.6 . . ? C4 C5 H5A 120.6 . . ? N2 C6 C5 122.7(2) . . ? N2 C6 C7 115.6(2) . . ? C5 C6 C7 121.7(2) . . ? N3 C7 C9 125.3(2) . . ? N3 C7 C6 117.1(2) . . ? C9 C7 C6 117.6(2) . . ? C1 C8 H8A 109.5 . . ? C1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 121.4(2) . . ? C11 C10 N1 118.6(2) . . ? C15 C10 N1 119.9(2) . . ? C10 C11 C12 118.2(2) . . ? C10 C11 C16 119.5(2) . . ? C12 C11 C16 122.2(2) . . ? C13 C12 C11 121.0(3) . . ? C13 C12 H12A 119.5 . . ? C11 C12 H12A 119.5 . . ? C14 C13 C12 119.8(3) . . ? C14 C13 H13A 120.1 . . ? C12 C13 H13A 120.1 . . ? C13 C14 C15 121.7(3) . . ? C13 C14 H14A 119.2 . . ? C15 C14 H14A 119.2 . . ? C14 C15 C10 117.9(2) . . ? C14 C15 C18 120.7(3) . . ? C10 C15 C18 121.4(2) . . ? C17 C16 C11 117.4(2) . . ? C17 C16 H16A 108.0 . . ? C11 C16 H16A 108.0 . . ? C17 C16 H16B 108.0 . . ? C11 C16 H16B 108.0 . . ? H16A C16 H16B 107.2 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C15 110.6(2) . . ? C19 C18 H18A 109.5 . . ? C15 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C25 121.7(2) . . ? C21 C20 N3 119.4(2) . . ? C25 C20 N3 118.7(2) . . ? C22 C21 C20 118.0(2) . . ? C22 C21 C26 120.3(2) . . ? C20 C21 C26 121.7(2) . . ? C23 C22 C21 121.5(3) . . ? C23 C22 H22A 119.3 . . ? C21 C22 H22A 119.3 . . ? C24 C23 C22 119.4(3) . . ? C24 C23 H23A 120.3 . . ? C22 C23 H23A 120.3 . . ? C23 C24 C25 121.7(3) . . ? C23 C24 H24A 119.1 . . ? C25 C24 H24A 119.1 . . ? C24 C25 C20 117.7(2) . . ? C24 C25 C28 121.1(2) . . ? C20 C25 C28 121.2(2) . . ? C21 C26 C27 112.7(2) . . ? C21 C26 H26A 109.0 . . ? C27 C26 H26A 109.0 . . ? C21 C26 H26B 109.0 . . ? C27 C26 H26B 109.0 . . ? H26A C26 H26B 107.8 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 C29 113.5(2) . . ? C25 C28 H28A 108.9 . . ? C29 C28 H28A 108.9 . . ? C25 C28 H28B 108.9 . . ? C29 C28 H28B 108.9 . . ? H28A C28 H28B 107.7 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.296 _refine_diff_density_min -0.187 _refine_diff_density_rms 0.036 _database_code_depnum_ccdc_archive 'CCDC 952323'