data_1415 _audit_creation_method 'SHELXL-97 & ZCIF' _chemical_name_systematic ; dimer ; _chemical_name_common dimer _chemical_formula_moiety 'C30 H46 N2 O6' _chemical_formula_sum 'C30 H46 N2 O6' _chemical_formula_weight 530.69 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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I41/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 18.5020(12) _cell_length_b 18.5020(12) _cell_length_c 36.985(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12661(2) _cell_formula_units_Z 16 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 2966 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 15.6 _exptl_crystal_description prism _exptl_crystal_colour redish-black _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.114 _exptl_crystal_density_method not-measured _exptl_crystal_F_000 4608 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.970 _exptl_absorpt_correction_T_max 0.985 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_ambient_temperature 220(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 'three-circle diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_decay_% ? _diffrn_reflns_number 29588 _diffrn_reflns_av_R_equivalents 0.0716 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 20.01 _reflns_number_total 2966 _reflns_number_gt 2135 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker, 1999)' _computing_publication_material SHELXL-97 _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 'w=1/[\s^2^(Fo^2^)+(0.02P)^2^+23.1P], P=(max(Fo^2^,0)+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 SHELXL _refine_ls_extinction_coef 0.00013(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2966 _refine_ls_number_parameters 397 _refine_ls_number_restraints 69 _refine_ls_R_factor_all 0.0879 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1221 _refine_ls_wR_factor_gt 0.1090 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 0.999 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.04830(18) 0.15538(18) 0.49796(8) 0.0959(10) Uani 1 1 d . . . N1 N 0.1134(2) 0.13210(18) 0.49816(9) 0.0712(10) Uani 1 1 d . . . C1 C 0.1553(2) 0.1257(2) 0.53014(11) 0.0656(11) Uani 1 1 d . . . C11 C 0.1242(2) 0.1435(2) 0.56689(11) 0.0747(12) Uani 1 1 d U . . C12 C 0.1804(3) 0.1293(3) 0.59606(11) 0.0989(15) Uani 1 1 d U . . H12A H 0.1599 0.1402 0.6196 0.148 Uiso 1 1 calc R . . H12B H 0.2223 0.1596 0.5919 0.148 Uiso 1 1 calc R . . H12C H 0.1947 0.0789 0.5953 0.148 Uiso 1 1 calc R . . C13 C 0.0583(3) 0.0955(3) 0.57389(13) 0.1096(17) Uani 1 1 d U . . H13A H 0.0415 0.1028 0.5985 0.164 Uiso 1 1 calc R . . H13B H 0.0716 0.0452 0.5706 0.164 Uiso 1 1 calc R . . H13C H 0.0201 0.1080 0.5571 0.164 Uiso 1 1 calc R . . C14 C 0.1028(3) 0.2241(2) 0.56837(12) 0.0984(15) Uani 1 1 d U . . H14A H 0.0802 0.2345 0.5915 0.148 Uiso 1 1 calc R . . H14B H 0.0690 0.2347 0.5490 0.148 Uiso 1 1 calc R . . H14C H 0.1456 0.2538 0.5656 0.148 Uiso 1 1 calc R . . C2 C 0.2189(2) 0.0985(2) 0.51848(11) 0.0637(11) Uani 1 1 d U . . C21 C 0.2860(3) 0.0809(3) 0.53926(11) 0.0802(13) Uani 1 1 d DU . . O21 O 0.29190(19) 0.0117(2) 0.54433(10) 0.1171(13) Uani 1 1 d DU . . O22 O 0.32970(19) 0.1244(2) 0.54902(10) 0.1200(13) Uani 1 1 d DU . . C22 C 0.3619(3) -0.0127(4) 0.5590(2) 0.169(3) Uani 1 1 d DU . . H22A H 0.4010 0.0021 0.5427 0.203 Uiso 1 1 calc R . . H22B H 0.3703 0.0097 0.5826 0.203 Uiso 1 1 calc R . . C23 C 0.3617(4) -0.0838(4) 0.5624(3) 0.232(5) Uani 1 1 d DU . . H23A H 0.3218 -0.0984 0.5778 0.348 Uiso 1 1 calc R . . H23B H 0.4069 -0.0995 0.5731 0.348 Uiso 1 1 calc R . . H23C H 0.3562 -0.1059 0.5387 0.348 Uiso 1 1 calc R . . C3 C 0.2174(2) 0.0883(2) 0.47911(11) 0.0635(11) Uani 1 1 d . . . C4 C 0.1515(2) 0.1096(2) 0.46689(11) 0.0656(11) Uani 1 1 d . . . C41 C 0.1158(3) 0.1148(3) 0.43000(11) 0.0820(13) Uani 1 1 d U . . C42 C 0.0519(3) 0.0619(3) 0.42803(13) 0.1073(17) Uani 1 1 d U . . H42A H 0.0167 0.0742 0.4465 0.161 Uiso 1 1 calc R . . H42B H 0.0692 0.0131 0.4320 0.161 Uiso 1 1 calc R . . H42C H 0.0295 0.0651 0.4044 0.161 Uiso 1 1 calc R . . C43 C 0.1701(3) 0.0937(3) 0.40055(11) 0.1037(16) Uani 1 1 d U . . H43A H 0.1851 0.0440 0.4041 0.156 Uiso 1 1 calc R . . H43B H 0.2120 0.1251 0.4020 0.156 Uiso 1 1 calc R . . H43C H 0.1477 0.0987 0.3770 0.156 Uiso 1 1 calc R . . C44 C 0.0911(3) 0.1925(3) 0.42296(14) 0.126(2) Uani 1 1 d U . . H44A H 0.1327 0.2245 0.4234 0.189 Uiso 1 1 calc R . . H44B H 0.0571 0.2070 0.4415 0.189 Uiso 1 1 calc R . . H44C H 0.0680 0.1953 0.3995 0.189 Uiso 1 1 calc R . . O2 O 0.4440(2) 0.0306(2) 0.42031(12) 0.1531(17) Uani 1 1 d . . . N2 N 0.3805(2) 0.0253(3) 0.43379(11) 0.1033(14) Uani 1 1 d . A . C5 C 0.3412(3) -0.0405(3) 0.43500(12) 0.0862(14) Uani 1 1 d . A . C51 C 0.3732(3) -0.1100(3) 0.42095(16) 0.1145(18) Uani 1 1 d U . . C52 C 0.3848(3) -0.1033(3) 0.37980(16) 0.154(2) Uani 1 1 d U . . H52A H 0.4202 -0.0658 0.3750 0.231 Uiso 1 1 calc R . . H52B H 0.3394 -0.0909 0.3682 0.231 Uiso 1 1 calc R . . H52C H 0.4022 -0.1489 0.3703 0.231 Uiso 1 1 calc R . . C53 C 0.3209(3) -0.1729(3) 0.42724(17) 0.141(2) Uani 1 1 d U . . H53A H 0.3429 -0.2175 0.4189 0.212 Uiso 1 1 calc R . . H53B H 0.2766 -0.1644 0.4139 0.212 Uiso 1 1 calc R . . H53C H 0.3102 -0.1768 0.4528 0.212 Uiso 1 1 calc R . . C54 C 0.4445(4) -0.1271(4) 0.4400(2) 0.189(3) Uani 1 1 d U . . H54A H 0.4380 -0.1229 0.4659 0.283 Uiso 1 1 calc R . . H54B H 0.4813 -0.0934 0.4321 0.283 Uiso 1 1 calc R . . H54C H 0.4593 -0.1760 0.4341 0.283 Uiso 1 1 calc R . . C6 C 0.2785(2) -0.0227(2) 0.45100(11) 0.0690(11) Uani 1 1 d . . . C61 C 0.2144(3) -0.0684(3) 0.45874(14) 0.0813(14) Uani 0.592(17) 1 d PDU A 1 O61 O 0.2222(7) -0.0986(7) 0.49122(18) 0.112(4) Uani 0.592(17) 1 d PDU A 1 O62 O 0.1670(9) -0.0868(10) 0.4387(4) 0.113(5) Uani 0.592(17) 1 d PDU A 1 C62 C 0.1594(12) -0.1396(9) 0.5044(4) 0.169(10) Uani 0.592(17) 1 d PDU A 1 H62A H 0.1231 -0.1430 0.4852 0.203 Uiso 0.592(17) 1 calc PR A 1 H62B H 0.1744 -0.1887 0.5108 0.203 Uiso 0.592(17) 1 calc PR A 1 C63 C 0.1299(10) -0.1072(11) 0.5336(6) 0.203(10) Uani 0.592(17) 1 d PDU A 1 H63A H 0.1667 -0.1007 0.5520 0.304 Uiso 0.592(17) 1 calc PR A 1 H63B H 0.0913 -0.1372 0.5431 0.304 Uiso 0.592(17) 1 calc PR A 1 H63C H 0.1106 -0.0605 0.5266 0.304 Uiso 0.592(17) 1 calc PR A 1 C61A C 0.2144(3) -0.0684(3) 0.45874(14) 0.0813(14) Uani 0.408(17) 1 d PDU A 2 O61A O 0.1936(7) -0.0652(7) 0.4924(2) 0.075(4) Uani 0.408(17) 1 d PDU A 2 O62A O 0.1760(14) -0.0840(17) 0.4339(5) 0.134(10) Uani 0.408(17) 1 d PDU A 2 C62A C 0.1256(7) -0.0998(8) 0.5031(5) 0.078(5) Uani 0.408(17) 1 d PDU A 2 H62C H 0.0970 -0.0661 0.5177 0.094 Uiso 0.408(17) 1 calc PR A 2 H62D H 0.0977 -0.1121 0.4815 0.094 Uiso 0.408(17) 1 calc PR A 2 C63A C 0.1385(12) -0.1606(9) 0.5225(7) 0.139(11) Uani 0.408(17) 1 d PDU A 2 H63D H 0.1521 -0.1995 0.5063 0.209 Uiso 0.408(17) 1 calc PR A 2 H63E H 0.0952 -0.1741 0.5356 0.209 Uiso 0.408(17) 1 calc PR A 2 H63F H 0.1775 -0.1518 0.5395 0.209 Uiso 0.408(17) 1 calc PR A 2 C7 C 0.2783(2) 0.0547(2) 0.45958(10) 0.0675(11) Uani 1 1 d . A . C8 C 0.3410(3) 0.0840(3) 0.44870(13) 0.0896(14) Uani 1 1 d . . . C81 C 0.3742(3) 0.1590(3) 0.44923(17) 0.1212(19) Uani 1 1 d U A . C82 C 0.3191(3) 0.2127(3) 0.46447(15) 0.126(2) Uani 1 1 d U . . H82A H 0.3397 0.2610 0.4643 0.190 Uiso 1 1 calc R A . H82B H 0.3069 0.1993 0.4891 0.190 Uiso 1 1 calc R . . H82C H 0.2758 0.2120 0.4497 0.190 Uiso 1 1 calc R . . C83 C 0.3923(4) 0.1828(3) 0.41034(17) 0.180(3) Uani 1 1 d U . . H83A H 0.4271 0.1496 0.3999 0.270 Uiso 1 1 calc R A . H83B H 0.4125 0.2311 0.4107 0.270 Uiso 1 1 calc R . . H83C H 0.3486 0.1826 0.3959 0.270 Uiso 1 1 calc R . . C84 C 0.4422(3) 0.1587(4) 0.4740(2) 0.173(3) Uani 1 1 d U . . H84A H 0.4287 0.1431 0.4981 0.260 Uiso 1 1 calc R A . H84B H 0.4624 0.2070 0.4751 0.260 Uiso 1 1 calc R . . H84C H 0.4779 0.1257 0.4642 0.260 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 O1 0.079(2) 0.116(3) 0.092(2) -0.0144(19) -0.0144(19) 0.017(2) N1 0.064(2) 0.080(3) 0.070(3) -0.003(2) -0.008(2) 0.001(2) C1 0.067(3) 0.071(3) 0.059(3) -0.002(2) -0.003(3) -0.003(2) C11 0.083(3) 0.081(3) 0.060(3) -0.012(2) 0.009(3) -0.002(3) C12 0.114(4) 0.123(4) 0.059(3) -0.007(3) -0.004(3) 0.010(3) C13 0.114(4) 0.124(4) 0.090(4) -0.014(3) 0.033(3) -0.032(4) C14 0.107(4) 0.095(4) 0.093(4) -0.024(3) -0.001(3) 0.013(3) C2 0.065(3) 0.068(3) 0.058(3) -0.001(2) -0.008(2) -0.004(2) C21 0.082(4) 0.097(4) 0.062(3) -0.013(3) 0.000(3) -0.005(3) O21 0.128(3) 0.092(3) 0.132(3) -0.029(2) -0.060(2) 0.031(2) O22 0.092(3) 0.134(3) 0.134(3) 0.000(2) -0.037(2) -0.020(2) C22 0.163(6) 0.142(6) 0.203(7) -0.047(5) -0.113(6) 0.065(5) C23 0.201(8) 0.135(6) 0.361(13) -0.037(8) -0.127(8) 0.057(6) C3 0.068(3) 0.065(3) 0.058(3) -0.003(2) 0.004(3) -0.011(2) C4 0.073(3) 0.072(3) 0.052(3) -0.003(2) 0.004(3) -0.008(2) C41 0.100(4) 0.092(4) 0.053(3) 0.003(2) -0.010(3) -0.005(3) C42 0.092(4) 0.141(5) 0.089(4) -0.010(3) -0.025(3) -0.023(3) C43 0.127(4) 0.131(4) 0.053(3) 0.005(3) -0.013(3) -0.027(3) C44 0.171(6) 0.107(4) 0.100(4) 0.024(3) -0.035(4) 0.020(4) O2 0.095(3) 0.169(4) 0.195(4) -0.061(3) 0.072(3) -0.042(3) N2 0.074(3) 0.121(4) 0.115(3) -0.031(3) 0.036(3) -0.025(3) C5 0.084(4) 0.086(4) 0.088(3) -0.023(3) 0.017(3) -0.017(3) C51 0.102(4) 0.109(5) 0.132(5) -0.041(4) 0.025(4) -0.001(4) C52 0.164(6) 0.161(6) 0.137(5) -0.060(5) 0.060(4) -0.011(5) C53 0.154(5) 0.097(4) 0.173(6) -0.042(4) 0.036(5) -0.003(4) C54 0.127(6) 0.179(7) 0.259(9) -0.074(6) -0.040(6) 0.044(5) C6 0.070(3) 0.073(3) 0.063(3) -0.009(2) 0.012(2) -0.016(3) C61 0.099(4) 0.072(3) 0.073(4) -0.015(3) 0.007(3) -0.017(3) O61 0.135(9) 0.135(9) 0.067(5) -0.011(4) 0.024(4) -0.054(7) O62 0.110(9) 0.118(10) 0.110(8) 0.034(7) -0.027(7) -0.033(8) C62 0.21(2) 0.16(2) 0.138(14) -0.037(11) 0.074(13) -0.111(16) C63 0.175(14) 0.183(18) 0.25(2) -0.079(16) 0.142(15) -0.071(13) C61A 0.099(4) 0.072(3) 0.073(4) -0.015(3) 0.007(3) -0.017(3) O61A 0.073(7) 0.073(7) 0.080(7) -0.013(5) 0.031(4) -0.020(5) O62A 0.151(16) 0.152(18) 0.099(11) -0.019(12) -0.002(10) -0.106(13) C62A 0.074(10) 0.067(10) 0.094(11) -0.008(8) 0.024(8) -0.025(8) C63A 0.132(18) 0.111(14) 0.17(3) 0.053(15) -0.021(16) -0.034(15) C7 0.065(3) 0.077(3) 0.060(3) -0.007(2) 0.009(2) -0.016(3) C8 0.090(4) 0.082(4) 0.096(4) -0.018(3) 0.027(3) -0.026(3) C81 0.126(5) 0.105(4) 0.133(5) -0.026(4) 0.043(4) -0.048(4) C82 0.167(5) 0.077(4) 0.135(5) -0.014(3) 0.042(4) -0.047(4) C83 0.238(8) 0.139(6) 0.162(6) -0.010(4) 0.106(6) -0.088(5) C84 0.110(5) 0.177(7) 0.232(8) -0.075(6) 0.016(5) -0.079(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. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 6.3216 (0.0204) x + 17.2268 (0.0089) y - 4.7302 (0.0695) z = 0.6328 (0.0354) * 0.0032 (0.0030) N1 * 0.0061 (0.0027) C1 * -0.0051 (0.0027) C2 * -0.0030 (0.0027) C3 * 0.0049 (0.0027) C4 * -0.0062 (0.0020) O1 -0.1046 (0.0062) C7 -0.0575 (0.0067) C11 0.0181 (0.0071) C21 0.0440 (0.0069) C41 Rms deviation of fitted atoms = 0.0049 7.3267 (0.0255) x - 3.6417 (0.0409) y + 33.1723 (0.0283) z = 17.0823 (0.0093) Angle to previous plane (with approximate esd) = 80.64 ( 0.16 ) * 0.0031 (0.0040) N2 * -0.0046 (0.0031) C5 * 0.0018 (0.0030) C6 * 0.0033 (0.0030) C7 * -0.0055 (0.0032) C8 * 0.0019 (0.0026) O2 0.0821 (0.0068) C3 0.0164 (0.0090) C51 -0.0447 (0.0076) C61_a -0.0181 (0.0092) C81 Rms deviation of fitted atoms = 0.0036 ; 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 O1 N1 1.279(4) . ? N1 C4 1.417(5) . ? N1 C1 1.419(5) . ? C1 C2 1.351(5) . ? C1 C11 1.512(5) . ? C11 C12 1.521(6) . ? C11 C13 1.531(6) . ? C11 C14 1.545(6) . ? C2 C3 1.469(5) . ? C2 C21 1.497(6) . ? C21 O22 1.196(5) . ? C21 O21 1.299(5) . ? O21 C22 1.475(5) . ? C22 C23 1.322(7) . ? C3 C4 1.359(5) . ? C3 C7 1.476(5) . ? C4 C41 1.519(6) . ? C41 C44 1.531(6) . ? C41 C43 1.532(6) . ? C41 C42 1.537(6) . ? O2 N2 1.281(4) . ? N2 C5 1.419(5) . ? N2 C8 1.420(6) . ? C5 C6 1.343(6) . ? C5 C51 1.507(7) . ? C51 C54 1.528(7) . ? C51 C53 1.532(7) . ? C51 C52 1.542(7) . ? C6 C7 1.466(5) . ? C6 C61 1.486(6) . ? C61 O62 1.197(7) . ? C61 O61 1.333(7) . ? O61 C62 1.471(8) . ? C62 C63 1.349(10) . ? O61A C62A 1.466(8) . ? C62A C63A 1.354(10) . ? C7 C8 1.341(5) . ? C8 C81 1.517(7) . ? C81 C82 1.532(7) . ? C81 C83 1.541(7) . ? C81 C84 1.557(8) . ? 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 O1 N1 C4 124.3(4) . . ? O1 N1 C1 123.2(4) . . ? C4 N1 C1 112.6(3) . . ? C2 C1 N1 104.0(3) . . ? C2 C1 C11 134.3(4) . . ? N1 C1 C11 121.6(4) . . ? C1 C11 C12 109.9(4) . . ? C1 C11 C13 109.2(3) . . ? C12 C11 C13 108.9(4) . . ? C1 C11 C14 109.9(4) . . ? C12 C11 C14 108.5(4) . . ? C13 C11 C14 110.5(4) . . ? C1 C2 C3 110.4(4) . . ? C1 C2 C21 129.8(4) . . ? C3 C2 C21 119.8(4) . . ? O22 C21 O21 124.3(5) . . ? O22 C21 C2 124.7(5) . . ? O21 C21 C2 111.0(4) . . ? C21 O21 C22 115.3(4) . . ? C23 C22 O21 109.7(6) . . ? C4 C3 C2 108.0(4) . . ? C4 C3 C7 130.2(4) . . ? C2 C3 C7 121.7(4) . . ? C3 C4 N1 105.1(3) . . ? C3 C4 C41 135.0(4) . . ? N1 C4 C41 119.9(4) . . ? C4 C41 C44 110.0(4) . . ? C4 C41 C43 109.7(4) . . ? C44 C41 C43 108.3(4) . . ? C4 C41 C42 109.6(4) . . ? C44 C41 C42 111.1(4) . . ? C43 C41 C42 108.0(4) . . ? O2 N2 C5 123.2(4) . . ? O2 N2 C8 124.4(4) . . ? C5 N2 C8 112.4(4) . . ? C6 C5 N2 104.2(4) . . ? C6 C5 C51 134.5(5) . . ? N2 C5 C51 121.4(5) . . ? C5 C51 C54 110.9(5) . . ? C5 C51 C53 110.4(4) . . ? C54 C51 C53 108.5(6) . . ? C5 C51 C52 109.1(5) . . ? C54 C51 C52 110.6(5) . . ? C53 C51 C52 107.4(5) . . ? C5 C6 C7 109.7(4) . . ? C5 C6 C61 129.4(4) . . ? C7 C6 C61 120.9(4) . . ? O62 C61 O61 121.2(10) . . ? O62 C61 C6 128.9(10) . . ? O61 C61 C6 109.0(6) . . ? C61 O61 C62 115.4(9) . . ? C63 C62 O61 110.9(10) . . ? C63A C62A O61A 110.8(10) . . ? C8 C7 C6 109.1(4) . . ? C8 C7 C3 129.5(4) . . ? C6 C7 C3 121.3(4) . . ? C7 C8 N2 104.6(4) . . ? C7 C8 C81 135.7(5) . . ? N2 C8 C81 119.7(4) . . ? C8 C81 C82 109.2(4) . . ? C8 C81 C83 109.7(5) . . ? C82 C81 C83 107.6(5) . . ? C8 C81 C84 109.3(5) . . ? C82 C81 C84 108.9(5) . . ? C83 C81 C84 112.0(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 N1 C1 C2 179.1(4) . . . . ? C4 N1 C1 C2 -0.6(4) . . . . ? O1 N1 C1 C11 2.5(6) . . . . ? C4 N1 C1 C11 -177.2(4) . . . . ? C2 C1 C11 C12 2.8(7) . . . . ? N1 C1 C11 C12 178.1(4) . . . . ? C2 C1 C11 C13 -116.6(5) . . . . ? N1 C1 C11 C13 58.7(5) . . . . ? C2 C1 C11 C14 122.1(5) . . . . ? N1 C1 C11 C14 -62.5(5) . . . . ? N1 C1 C2 C3 0.5(4) . . . . ? C11 C1 C2 C3 176.4(4) . . . . ? N1 C1 C2 C21 178.7(4) . . . . ? C11 C1 C2 C21 -5.4(8) . . . . ? C1 C2 C21 O22 -78.8(7) . . . . ? C3 C2 C21 O22 99.3(5) . . . . ? C1 C2 C21 O21 103.3(5) . . . . ? C3 C2 C21 O21 -78.7(5) . . . . ? O22 C21 O21 C22 -7.9(7) . . . . ? C2 C21 O21 C22 170.0(4) . . . . ? C21 O21 C22 C23 -179.0(7) . . . . ? C1 C2 C3 C4 -0.2(5) . . . . ? C21 C2 C3 C4 -178.6(4) . . . . ? C1 C2 C3 C7 -175.8(4) . . . . ? C21 C2 C3 C7 5.8(6) . . . . ? C2 C3 C4 N1 -0.2(4) . . . . ? C7 C3 C4 N1 175.0(4) . . . . ? C2 C3 C4 C41 178.2(4) . . . . ? C7 C3 C4 C41 -6.6(8) . . . . ? O1 N1 C4 C3 -179.2(4) . . . . ? C1 N1 C4 C3 0.5(4) . . . . ? O1 N1 C4 C41 2.1(6) . . . . ? C1 N1 C4 C41 -178.2(4) . . . . ? C3 C4 C41 C44 -122.3(5) . . . . ? N1 C4 C41 C44 55.9(5) . . . . ? C3 C4 C41 C43 -3.2(7) . . . . ? N1 C4 C41 C43 175.0(4) . . . . ? C3 C4 C41 C42 115.2(5) . . . . ? N1 C4 C41 C42 -66.5(5) . . . . ? O2 N2 C5 C6 179.9(5) . . . . ? C8 N2 C5 C6 -0.9(5) . . . . ? O2 N2 C5 C51 1.4(8) . . . . ? C8 N2 C5 C51 -179.4(5) . . . . ? C6 C5 C51 C54 -121.0(7) . . . . ? N2 C5 C51 C54 57.0(7) . . . . ? C6 C5 C51 C53 -0.7(9) . . . . ? N2 C5 C51 C53 177.3(5) . . . . ? C6 C5 C51 C52 117.0(6) . . . . ? N2 C5 C51 C52 -65.0(6) . . . . ? N2 C5 C6 C7 0.4(5) . . . . ? C51 C5 C6 C7 178.7(5) . . . . ? N2 C5 C6 C61 177.8(4) . . . . ? C51 C5 C6 C61 -3.9(9) . . . . ? C5 C6 C61 O62 -79.6(15) . . . . ? C7 C6 C61 O62 97.5(14) . . . . ? C5 C6 C61 O61 89.5(9) . . . . ? C7 C6 C61 O61 -93.3(9) . . . . ? O62 C61 O61 C62 -16.1(19) . . . . ? C6 C61 O61 C62 173.8(9) . . . . ? C61 O61 C62 C63 -114(3) . . . . ? C5 C6 C7 C8 0.1(5) . . . . ? C61 C6 C7 C8 -177.5(4) . . . . ? C5 C6 C7 C3 -176.7(4) . . . . ? C61 C6 C7 C3 5.6(6) . . . . ? C4 C3 C7 C8 104.6(6) . . . . ? C2 C3 C7 C8 -80.9(6) . . . . ? C4 C3 C7 C6 -79.3(6) . . . . ? C2 C3 C7 C6 95.3(5) . . . . ? C6 C7 C8 N2 -0.6(5) . . . . ? C3 C7 C8 N2 175.9(4) . . . . ? C6 C7 C8 C81 179.5(6) . . . . ? C3 C7 C8 C81 -4.0(9) . . . . ? O2 N2 C8 C7 -179.8(5) . . . . ? C5 N2 C8 C7 1.0(6) . . . . ? O2 N2 C8 C81 0.1(8) . . . . ? C5 N2 C8 C81 -179.2(5) . . . . ? C7 C8 C81 C82 -3.6(9) . . . . ? N2 C8 C81 C82 176.6(5) . . . . ? C7 C8 C81 C83 -121.3(7) . . . . ? N2 C8 C81 C83 58.8(7) . . . . ? C7 C8 C81 C84 115.5(7) . . . . ? N2 C8 C81 C84 -64.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 20.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.227 _refine_diff_density_min -0.157 _refine_diff_density_rms 0.028 _exptl_crystal_id 'Kao black-tar' _diffrn_measurement_details 366,366,366 _diffrn_measurement_total_frames-CCD 1098 _diffrn_measurement_frame_width-CCD 0.5 _diffrn_detector_distance-CCD 4.939 _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_measurement_frame_time-CCD 23 _diffrn_measurement_total_time-CCD 9.20 _diffrn_measurement_frame_size-CCD 512 _diffrn_orient_matrix_type standard _diffrn_orient_matrix_UB_11 -0.0538558 _diffrn_orient_matrix_UB_12 -0.0007989 _diffrn_orient_matrix_UB_13 -0.0021744 _diffrn_orient_matrix_UB_21 -0.0044553 _diffrn_orient_matrix_UB_22 0.0075164 _diffrn_orient_matrix_UB_23 0.0266806 _diffrn_orient_matrix_UB_31 -0.0001447 _diffrn_orient_matrix_UB_32 0.0535229 _diffrn_orient_matrix_UB_33 -0.0037843 _symmetry_space_group_name_Hall '-I 4ad' _diffrn_measurement_specimen_support 'glass capillary' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker Smart1000' #_______________________________________________________________________________ # _publ_section_references ; Bruker (1999). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1990). Acta Cryst. A46, 467-473. Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (1997). SHELXL-97. University of G\"ottingen, Germany. Spek, A. L. (1990). Acta Cryst., A46, C-34. ;