data_mjr17066_0m _audit_creation_date 2017-10-30 _audit_creation_method ; Olex2 1.2 (compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337) ; _shelx_SHELXL_version_number '2017/1' _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_id_orcid ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C30 H27 N3 O2' _chemical_formula_sum 'C30 H27 N3 O2' _chemical_formula_weight 461.54 _chemical_absolute_configuration rmad _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0150 0.0070 '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' 0.0250 0.0140 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0410 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 4 _space_group_name_H-M_alt 'P 1 21 1' _space_group_name_Hall 'P 2yb' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.4544(2) _cell_length_b 9.3869(2) _cell_length_c 12.7713(3) _cell_angle_alpha 90 _cell_angle_beta 115.0800(10) _cell_angle_gamma 90 _cell_volume 1243.72(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6911 _cell_measurement_temperature 302(2) _cell_measurement_theta_max 59.716 _cell_measurement_theta_min 3.708 _shelx_estimated_absorpt_T_max 0.980 _shelx_estimated_absorpt_T_min 0.943 _exptl_absorpt_coefficient_mu 0.397 _exptl_absorpt_correction_T_max 0.7519 _exptl_absorpt_correction_T_min 0.6147 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1481 before and 0.0625 after correction. The Ratio of minimum to maximum transmission is 0.8175. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 488 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_unetI/netI 0.0335 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 15748 _diffrn_reflns_point_group_measured_fraction_full 0.979 _diffrn_reflns_point_group_measured_fraction_max 0.964 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 60.650 _diffrn_reflns_theta_min 3.707 _diffrn_ambient_temperature 301.72 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method ? _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34139 _diffrn_source ? _reflns_Friedel_coverage 0.834 _reflns_Friedel_fraction_full 0.964 _reflns_Friedel_fraction_max 0.933 _reflns_number_gt 4886 _reflns_number_total 5520 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_collection ? _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.222 _refine_diff_density_min -0.151 _refine_diff_density_rms 0.033 _refine_ls_abs_structure_details ; Flack x determined using 1925 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.05(17) _refine_ls_extinction_coef 0.020(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_extinction_method 'SHELXL-2017/1 (Sheldrick 2017)' _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 346 _refine_ls_number_reflns 5520 _refine_ls_number_restraints 77 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0491 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+0.2890P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1060 _refine_ls_wR_factor_ref 0.1128 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C29'-C30' = C29'-C28' = C29-C28 = C29-C30 1.53 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints O2 \\sim C28 \\sim C29 \\sim C30 \\sim C28' \\sim C29' \\sim C30': within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Others Fixed Sof: C28(0.5) H28A(0.5) H28B(0.5) C29(0.5) H29A(0.5) H29B(0.5) C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C28'(0.5) H28C(0.5) H28D(0.5) C29'(0.5) H29C(0.5) H29D(0.5) C30'(0.5) H30D(0.5) H30E(0.5) H30F(0.5) 5.a Ternary CH refined with riding coordinates: C1(H1), C2(H2A) 5.b Secondary CH2 refined with riding coordinates: C28(H28A,H28B), C29(H29A,H29B), C28'(H28C,H28D), C29'(H29C,H29D) 5.c Aromatic/amide H refined with riding coordinates: N2(H2), N3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26) 5.d Idealised Me refined as rotating group: C30(H30A,H30B,H30C), C30'(H30D,H30E,H30F) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 O1 O 1.0254(3) 0.7543(4) 0.2930(3) 0.1110(11) Uani 1 1 d . . . . . O2 O 0.8178(3) 0.6848(4) 0.2261(2) 0.0877(9) Uani 1 1 d . U . . . N1 N 0.8503(2) 0.6025(2) 0.43588(19) 0.0464(5) Uani 1 1 d . . . . . N2 N 0.9438(2) 0.6736(3) 0.4133(3) 0.0625(7) Uani 1 1 d . . . . . H2 H 1.013456 0.697137 0.471949 0.075 Uiso 1 1 calc R . . . . N3 N 0.7984(3) 0.9578(3) 0.6585(3) 0.0661(8) Uani 1 1 d . . . . . H3 H 0.793945 1.042728 0.681792 0.079 Uiso 1 1 calc R . . . . C1 C 0.7397(2) 0.6883(3) 0.4322(2) 0.0422(6) Uani 1 1 d . . . . . H1 H 0.711087 0.752388 0.365423 0.051 Uiso 1 1 calc R . . . . C2 C 0.6325(2) 0.5730(3) 0.4113(2) 0.0395(5) Uani 1 1 d . . . . . H2A H 0.632247 0.548583 0.485764 0.047 Uiso 1 1 calc R . . . . C3 C 0.6809(2) 0.4458(3) 0.3684(2) 0.0392(5) Uani 1 1 d . . . . . C4 C 0.6231(3) 0.3125(3) 0.3276(2) 0.0422(6) Uani 1 1 d . . . . . C5 C 0.4984(3) 0.2739(3) 0.3162(2) 0.0474(6) Uani 1 1 d . . . . . H5 H 0.449767 0.339563 0.335279 0.057 Uiso 1 1 calc R . . . . C6 C 0.4490(3) 0.1418(3) 0.2777(3) 0.0565(7) Uani 1 1 d . . . . . H6 H 0.367614 0.118145 0.271874 0.068 Uiso 1 1 calc R . . . . C7 C 0.5194(3) 0.0412(3) 0.2466(3) 0.0629(8) Uani 1 1 d . . . . . H7 H 0.484530 -0.048351 0.220268 0.075 Uiso 1 1 calc R . . . . C8 C 0.6382(3) 0.0745(3) 0.2552(3) 0.0598(8) Uani 1 1 d . . . . . H8 H 0.683885 0.007261 0.234020 0.072 Uiso 1 1 calc R . . . . C9 C 0.6944(3) 0.2097(3) 0.2956(2) 0.0472(6) Uani 1 1 d . . . . . C10 C 0.8198(3) 0.2445(3) 0.3067(3) 0.0557(7) Uani 1 1 d . . . . . H10 H 0.864765 0.178416 0.283658 0.067 Uiso 1 1 calc R . . . . C11 C 0.8759(3) 0.3720(3) 0.3501(3) 0.0530(7) Uani 1 1 d . . . . . H11 H 0.958838 0.392640 0.358600 0.064 Uiso 1 1 calc R . . . . C12 C 0.8051(2) 0.4717(3) 0.3818(2) 0.0430(6) Uani 1 1 d . . . . . C13 C 0.7534(3) 0.9164(3) 0.5456(3) 0.0572(8) Uani 1 1 d . . . . . H13 H 0.713298 0.976014 0.482183 0.069 Uiso 1 1 calc R . . . . C14 C 0.7758(2) 0.7748(3) 0.5397(2) 0.0440(6) Uani 1 1 d . . . . . C15 C 0.8393(2) 0.7253(3) 0.6572(2) 0.0425(6) Uani 1 1 d . . . . . C16 C 0.8899(3) 0.5941(3) 0.7085(3) 0.0502(7) Uani 1 1 d . . . . . H16 H 0.884455 0.514622 0.663171 0.060 Uiso 1 1 calc R . . . . C17 C 0.9479(3) 0.5847(4) 0.8272(3) 0.0643(9) Uani 1 1 d . . . . . H17 H 0.981161 0.497734 0.861910 0.077 Uiso 1 1 calc R . . . . C18 C 0.9576(4) 0.7023(5) 0.8961(3) 0.0760(11) Uani 1 1 d . . . . . H18 H 0.997462 0.692769 0.976112 0.091 Uiso 1 1 calc R . . . . C19 C 0.9100(4) 0.8311(5) 0.8489(3) 0.0730(10) Uani 1 1 d . . . . . H19 H 0.916148 0.909414 0.895615 0.088 Uiso 1 1 calc R . . . . C20 C 0.8516(3) 0.8432(4) 0.7288(3) 0.0537(7) Uani 1 1 d . . . . . C21 C 0.5017(2) 0.6315(3) 0.3328(2) 0.0442(6) Uani 1 1 d . . . . . C22 C 0.4499(3) 0.6148(4) 0.2144(3) 0.0604(8) Uani 1 1 d . . . . . H22 H 0.493550 0.561667 0.180762 0.072 Uiso 1 1 calc R . . . . C23 C 0.3315(4) 0.6782(4) 0.1449(4) 0.0816(12) Uani 1 1 d . . . . . H23 H 0.295695 0.665519 0.065195 0.098 Uiso 1 1 calc R . . . . C24 C 0.2682(3) 0.7587(4) 0.1939(4) 0.0841(13) Uani 1 1 d . . . . . H24 H 0.189944 0.801132 0.147161 0.101 Uiso 1 1 calc R . . . . C25 C 0.3189(3) 0.7770(4) 0.3105(4) 0.0758(11) Uani 1 1 d . . . . . H25 H 0.276116 0.832688 0.343434 0.091 Uiso 1 1 calc R . . . . C26 C 0.4340(3) 0.7125(3) 0.3792(3) 0.0575(8) Uani 1 1 d . . . . . H26 H 0.467307 0.723519 0.458985 0.069 Uiso 1 1 calc R . . . . C27 C 0.9354(4) 0.7088(4) 0.3086(4) 0.0728(10) Uani 1 1 d . . . . . C28 C 0.8146(17) 0.7288(19) 0.1199(12) 0.124(4) Uani 0.5 1 d D U P A 1 H28A H 0.887687 0.692201 0.108702 0.148 Uiso 0.5 1 calc R . P A 1 H28B H 0.812493 0.831840 0.113261 0.148 Uiso 0.5 1 calc R . P A 1 C29 C 0.6881(15) 0.6617(16) 0.0351(8) 0.124(3) Uani 0.5 1 d D U P A 1 H29A H 0.618494 0.713341 0.042331 0.149 Uiso 0.5 1 calc R . P A 1 H29B H 0.680729 0.679548 -0.042253 0.149 Uiso 0.5 1 calc R . P A 1 C30 C 0.665(2) 0.513(2) 0.0426(11) 0.199(7) Uani 0.5 1 d D U P A 1 H30A H 0.582907 0.487811 -0.018029 0.298 Uiso 0.5 1 calc GR . P A 1 H30B H 0.664669 0.493143 0.116209 0.298 Uiso 0.5 1 calc GR . P A 1 H30C H 0.731621 0.458685 0.034574 0.298 Uiso 0.5 1 calc GR . P A 1 C28' C 0.7908(19) 0.6734(16) 0.0951(13) 0.116(3) Uani 0.5 1 d D U P A 2 H28C H 0.871338 0.669432 0.087187 0.139 Uiso 0.5 1 calc R . P A 2 H28D H 0.741809 0.587848 0.061205 0.139 Uiso 0.5 1 calc R . P A 2 C29' C 0.7154(14) 0.8034(17) 0.0357(11) 0.143(4) Uani 0.5 1 d D U P A 2 H29C H 0.756265 0.887142 0.080841 0.171 Uiso 0.5 1 calc R . P A 2 H29D H 0.716561 0.812977 -0.039489 0.171 Uiso 0.5 1 calc R . P A 2 C30' C 0.5862(11) 0.7963(17) 0.0214(9) 0.123(4) Uani 0.5 1 d D U P A 2 H30D H 0.546134 0.712195 -0.021504 0.184 Uiso 0.5 1 calc GR . P A 2 H30E H 0.540280 0.878990 -0.019796 0.184 Uiso 0.5 1 calc GR . P A 2 H30F H 0.584550 0.792962 0.095909 0.184 Uiso 0.5 1 calc GR . P A 2 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 0.103(2) 0.094(2) 0.182(3) 0.017(2) 0.105(2) -0.0143(18) O2 0.0928(19) 0.114(2) 0.0716(16) 0.0122(15) 0.0498(15) -0.0137(18) N1 0.0348(11) 0.0528(14) 0.0554(13) -0.0094(11) 0.0227(10) -0.0051(10) N2 0.0422(13) 0.0734(18) 0.0787(18) -0.0186(15) 0.0322(12) -0.0202(12) N3 0.0695(18) 0.0465(14) 0.0808(19) -0.0196(14) 0.0305(15) -0.0004(13) C1 0.0351(12) 0.0450(14) 0.0471(13) -0.0018(11) 0.0181(10) -0.0041(11) C2 0.0341(12) 0.0405(13) 0.0447(13) -0.0018(10) 0.0174(10) -0.0010(10) C3 0.0345(12) 0.0421(13) 0.0408(12) 0.0028(11) 0.0159(10) 0.0028(10) C4 0.0391(13) 0.0433(14) 0.0438(13) 0.0031(10) 0.0173(11) 0.0031(10) C5 0.0437(14) 0.0474(14) 0.0546(15) -0.0007(12) 0.0241(12) -0.0028(12) C6 0.0529(16) 0.0521(17) 0.0676(19) -0.0034(14) 0.0287(15) -0.0112(14) C7 0.070(2) 0.0433(16) 0.077(2) -0.0074(14) 0.0323(17) -0.0110(14) C8 0.066(2) 0.0450(16) 0.0688(19) -0.0053(14) 0.0290(16) 0.0054(15) C9 0.0477(14) 0.0432(14) 0.0511(15) 0.0004(12) 0.0213(12) 0.0054(12) C10 0.0460(15) 0.0565(18) 0.0688(18) -0.0039(15) 0.0285(14) 0.0104(13) C11 0.0374(14) 0.0606(18) 0.0647(18) -0.0004(14) 0.0253(13) 0.0049(13) C12 0.0368(13) 0.0474(14) 0.0450(14) -0.0007(11) 0.0176(11) 0.0008(11) C13 0.0537(17) 0.0449(16) 0.0685(19) -0.0004(13) 0.0214(14) 0.0044(13) C14 0.0356(12) 0.0426(13) 0.0535(15) -0.0042(12) 0.0187(11) -0.0035(11) C15 0.0344(12) 0.0459(14) 0.0502(14) -0.0055(11) 0.0209(11) -0.0078(11) C16 0.0419(14) 0.0497(16) 0.0603(16) 0.0007(13) 0.0231(12) -0.0052(12) C17 0.0558(18) 0.076(2) 0.0598(18) 0.0110(17) 0.0228(15) -0.0054(16) C18 0.068(2) 0.106(3) 0.0502(18) -0.004(2) 0.0217(16) -0.015(2) C19 0.072(2) 0.089(3) 0.0581(19) -0.0293(19) 0.0278(17) -0.014(2) C20 0.0475(15) 0.0563(17) 0.0610(17) -0.0138(15) 0.0265(14) -0.0057(14) C21 0.0350(12) 0.0372(12) 0.0591(16) -0.0052(11) 0.0188(11) -0.0025(10) C22 0.0542(17) 0.0567(18) 0.0593(17) -0.0041(14) 0.0135(14) 0.0070(14) C23 0.066(2) 0.068(2) 0.077(2) 0.0033(19) -0.0024(18) -0.0005(19) C24 0.0436(17) 0.0507(19) 0.134(4) 0.001(2) 0.014(2) 0.0067(15) C25 0.0500(18) 0.0500(17) 0.132(4) -0.004(2) 0.044(2) 0.0039(15) C26 0.0469(15) 0.0463(16) 0.087(2) -0.0080(15) 0.0359(15) -0.0014(13) C27 0.073(2) 0.062(2) 0.108(3) -0.004(2) 0.061(2) -0.0116(19) C28 0.162(7) 0.146(8) 0.068(6) 0.007(6) 0.054(5) -0.027(7) C29 0.171(7) 0.139(7) 0.051(4) 0.005(5) 0.035(5) -0.036(7) C30 0.254(15) 0.211(14) 0.079(7) -0.035(9) 0.020(9) -0.006(13) C28' 0.161(7) 0.139(7) 0.068(5) 0.001(5) 0.068(5) -0.027(7) C29' 0.180(8) 0.157(8) 0.089(5) -0.001(6) 0.055(6) -0.018(7) C30' 0.122(8) 0.165(10) 0.074(6) 0.000(6) 0.033(6) -0.014(8) _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 O1 C27 1.208(4) . ? O2 C27 1.331(5) . ? O2 C28 1.404(16) . ? O2 C28' 1.571(15) . ? N1 N2 1.392(3) . ? N1 C1 1.486(3) . ? N1 C12 1.397(4) . ? N2 H2 0.8600 . ? N2 C27 1.340(5) . ? N3 H3 0.8600 . ? N3 C13 1.366(4) . ? N3 C20 1.367(4) . ? C1 H1 0.9800 . ? C1 C2 1.572(3) . ? C1 C14 1.494(4) . ? C2 H2A 0.9800 . ? C2 C3 1.514(4) . ? C2 C21 1.509(4) . ? C3 C4 1.408(4) . ? C3 C12 1.380(4) . ? C4 C5 1.420(4) . ? C4 C9 1.430(4) . ? C5 H5 0.9300 . ? C5 C6 1.366(4) . ? C6 H6 0.9300 . ? C6 C7 1.404(5) . ? C7 H7 0.9300 . ? C7 C8 1.355(5) . ? C8 H8 0.9300 . ? C8 C9 1.417(4) . ? C9 C10 1.421(4) . ? C10 H10 0.9300 . ? C10 C11 1.360(4) . ? C11 H11 0.9300 . ? C11 C12 1.405(4) . ? C13 H13 0.9300 . ? C13 C14 1.362(4) . ? C14 C15 1.440(4) . ? C15 C16 1.400(4) . ? C15 C20 1.405(4) . ? C16 H16 0.9300 . ? C16 C17 1.376(4) . ? C17 H17 0.9300 . ? C17 C18 1.386(6) . ? C18 H18 0.9300 . ? C18 C19 1.358(6) . ? C19 H19 0.9300 . ? C19 C20 1.394(5) . ? C21 C22 1.379(4) . ? C21 C26 1.386(4) . ? C22 H22 0.9300 . ? C22 C23 1.400(5) . ? C23 H23 0.9300 . ? C23 C24 1.368(6) . ? C24 H24 0.9300 . ? C24 C25 1.360(6) . ? C25 H25 0.9300 . ? C25 C26 1.377(5) . ? C26 H26 0.9300 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 C29 1.529(16) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 C30 1.431(17) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C28' H28C 0.9700 . ? C28' H28D 0.9700 . ? C28' C29' 1.502(18) . ? C29' H29C 0.9700 . ? C29' H29D 0.9700 . ? C29' C30' 1.414(15) . ? C30' H30D 0.9600 . ? C30' H30E 0.9600 . ? C30' H30F 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 C27 O2 C28 108.5(7) . . ? C27 O2 C28' 122.0(8) . . ? N2 N1 C1 117.0(2) . . ? N2 N1 C12 118.4(2) . . ? C12 N1 C1 109.2(2) . . ? N1 N2 H2 117.0 . . ? C27 N2 N1 126.1(3) . . ? C27 N2 H2 117.0 . . ? C13 N3 H3 125.3 . . ? C13 N3 C20 109.5(3) . . ? C20 N3 H3 125.3 . . ? N1 C1 H1 109.0 . . ? N1 C1 C2 103.1(2) . . ? N1 C1 C14 111.4(2) . . ? C2 C1 H1 109.0 . . ? C14 C1 H1 109.0 . . ? C14 C1 C2 115.0(2) . . ? C1 C2 H2A 108.6 . . ? C3 C2 C1 103.0(2) . . ? C3 C2 H2A 108.6 . . ? C21 C2 C1 110.3(2) . . ? C21 C2 H2A 108.6 . . ? C21 C2 C3 117.4(2) . . ? C4 C3 C2 130.4(2) . . ? C12 C3 C2 109.4(2) . . ? C12 C3 C4 120.0(2) . . ? C3 C4 C5 124.0(2) . . ? C3 C4 C9 118.0(2) . . ? C5 C4 C9 118.0(2) . . ? C4 C5 H5 119.5 . . ? C6 C5 C4 120.9(3) . . ? C6 C5 H5 119.5 . . ? C5 C6 H6 119.6 . . ? C5 C6 C7 120.8(3) . . ? C7 C6 H6 119.6 . . ? C6 C7 H7 120.0 . . ? C8 C7 C6 120.0(3) . . ? C8 C7 H7 120.0 . . ? C7 C8 H8 119.3 . . ? C7 C8 C9 121.4(3) . . ? C9 C8 H8 119.3 . . ? C8 C9 C4 118.8(3) . . ? C8 C9 C10 121.7(3) . . ? C10 C9 C4 119.4(3) . . ? C9 C10 H10 119.1 . . ? C11 C10 C9 121.7(3) . . ? C11 C10 H10 119.1 . . ? C10 C11 H11 120.9 . . ? C10 C11 C12 118.2(3) . . ? C12 C11 H11 120.9 . . ? N1 C12 C11 126.1(2) . . ? C3 C12 N1 111.3(2) . . ? C3 C12 C11 122.5(3) . . ? N3 C13 H13 125.0 . . ? C14 C13 N3 109.9(3) . . ? C14 C13 H13 125.0 . . ? C13 C14 C1 126.6(3) . . ? C13 C14 C15 106.3(3) . . ? C15 C14 C1 127.1(2) . . ? C16 C15 C14 134.3(3) . . ? C16 C15 C20 118.8(3) . . ? C20 C15 C14 106.9(2) . . ? C15 C16 H16 120.6 . . ? C17 C16 C15 118.8(3) . . ? C17 C16 H16 120.6 . . ? C16 C17 H17 119.3 . . ? C16 C17 C18 121.3(3) . . ? C18 C17 H17 119.3 . . ? C17 C18 H18 119.4 . . ? C19 C18 C17 121.2(3) . . ? C19 C18 H18 119.4 . . ? C18 C19 H19 120.8 . . ? C18 C19 C20 118.4(3) . . ? C20 C19 H19 120.8 . . ? N3 C20 C15 107.4(2) . . ? N3 C20 C19 131.2(3) . . ? C19 C20 C15 121.4(3) . . ? C22 C21 C2 122.1(3) . . ? C22 C21 C26 118.2(3) . . ? C26 C21 C2 119.6(3) . . ? C21 C22 H22 120.1 . . ? C21 C22 C23 119.8(3) . . ? C23 C22 H22 120.1 . . ? C22 C23 H23 119.9 . . ? C24 C23 C22 120.2(4) . . ? C24 C23 H23 119.9 . . ? C23 C24 H24 119.8 . . ? C25 C24 C23 120.5(3) . . ? C25 C24 H24 119.8 . . ? C24 C25 H25 120.3 . . ? C24 C25 C26 119.4(3) . . ? C26 C25 H25 120.3 . . ? C21 C26 H26 119.1 . . ? C25 C26 C21 121.8(3) . . ? C25 C26 H26 119.1 . . ? O1 C27 O2 125.3(4) . . ? O1 C27 N2 123.1(4) . . ? O2 C27 N2 111.6(3) . . ? O2 C28 H28A 111.6 . . ? O2 C28 H28B 111.6 . . ? O2 C28 C29 101.0(11) . . ? H28A C28 H28B 109.4 . . ? C29 C28 H28A 111.6 . . ? C29 C28 H28B 111.6 . . ? C28 C29 H29A 107.3 . . ? C28 C29 H29B 107.3 . . ? H29A C29 H29B 106.9 . . ? C30 C29 C28 120.1(15) . . ? C30 C29 H29A 107.3 . . ? C30 C29 H29B 107.3 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O2 C28' H28C 110.3 . . ? O2 C28' H28D 110.3 . . ? H28C C28' H28D 108.6 . . ? C29' C28' O2 107.1(11) . . ? C29' C28' H28C 110.3 . . ? C29' C28' H28D 110.3 . . ? C28' C29' H29C 109.2 . . ? C28' C29' H29D 109.2 . . ? H29C C29' H29D 107.9 . . ? C30' C29' C28' 111.9(14) . . ? C30' C29' H29C 109.2 . . ? C30' C29' H29D 109.2 . . ? C29' C30' H30D 109.5 . . ? C29' C30' H30E 109.5 . . ? C29' C30' H30F 109.5 . . ? H30D C30' H30E 109.5 . . ? H30D C30' H30F 109.5 . . ? H30E C30' H30F 109.5 . . ? _shelx_res_file ; TITL mjr17066_0m_a.res in P2(1) mjr17066_0m.res created by SHELXL-2017/1 at 10:05:52 on 30-Oct-2017 REM Old TITL mjr17066_0m in P2(1) REM SHELXT solution in P2(1) REM R1 0.179, Rweak 0.044, Alpha 0.008, Orientation as input REM Flack x = 0.389 ( 0.182 ) from Parsons' quotients REM Formula found by SHELXT: C28 N3 O CELL 1.34139 11.4544 9.3869 12.7713 90 115.08 90 ZERR 2 0.0002 0.0002 0.0003 0 0.001 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O DISP C 0.015 0.007 57.748 DISP H -0 0 0.648 DISP N 0.025 0.014 110.512 DISP O 0.041 0.025 193.954 UNIT 60 54 6 4 DFIX 1.53 C29' C30' C29' C28' C29 C28 C29 C30 SIMU 0.01 0.02 2 O2 C28 > C30' L.S. 4 PLAN 20 SIZE 0.05 0.12 0.15 TEMP 28.57 BOND $H list 4 fmap 2 ACTA REM REM REM WGHT 0.034300 0.289000 EXTI 0.019618 FVAR 1.43641 O1 4 1.025417 0.754347 0.292983 11.00000 0.10284 0.09410 = 0.18181 0.01732 0.10451 -0.01435 O2 4 0.817804 0.684796 0.226128 11.00000 0.09285 0.11405 = 0.07163 0.01220 0.04976 -0.01365 N1 3 0.850329 0.602494 0.435878 11.00000 0.03484 0.05278 = 0.05537 -0.00944 0.02270 -0.00512 N2 3 0.943828 0.673600 0.413290 11.00000 0.04222 0.07338 = 0.07874 -0.01865 0.03223 -0.02023 AFIX 43 H2 2 1.013456 0.697137 0.471949 11.00000 -1.20000 AFIX 0 N3 3 0.798390 0.957777 0.658526 11.00000 0.06948 0.04655 = 0.08083 -0.01957 0.03048 -0.00037 AFIX 43 H3 2 0.793945 1.042728 0.681792 11.00000 -1.20000 AFIX 0 C1 1 0.739667 0.688273 0.432221 11.00000 0.03514 0.04503 = 0.04707 -0.00185 0.01806 -0.00414 AFIX 13 H1 2 0.711087 0.752388 0.365423 11.00000 -1.20000 AFIX 0 C2 1 0.632516 0.572988 0.411258 11.00000 0.03414 0.04047 = 0.04471 -0.00178 0.01738 -0.00101 AFIX 13 H2A 2 0.632247 0.548583 0.485764 11.00000 -1.20000 AFIX 0 C3 1 0.680936 0.445766 0.368395 11.00000 0.03454 0.04209 = 0.04082 0.00284 0.01587 0.00278 C4 1 0.623118 0.312462 0.327551 11.00000 0.03914 0.04332 = 0.04380 0.00308 0.01726 0.00312 C5 1 0.498433 0.273921 0.316202 11.00000 0.04371 0.04740 = 0.05457 -0.00071 0.02412 -0.00280 AFIX 43 H5 2 0.449767 0.339563 0.335279 11.00000 -1.20000 AFIX 0 C6 1 0.448979 0.141764 0.277651 11.00000 0.05289 0.05215 = 0.06764 -0.00339 0.02872 -0.01118 AFIX 43 H6 2 0.367614 0.118145 0.271874 11.00000 -1.20000 AFIX 0 C7 1 0.519394 0.041161 0.246646 11.00000 0.06981 0.04327 = 0.07687 -0.00740 0.03228 -0.01104 AFIX 43 H7 2 0.484530 -0.048351 0.220268 11.00000 -1.20000 AFIX 0 C8 1 0.638217 0.074517 0.255166 11.00000 0.06582 0.04503 = 0.06884 -0.00529 0.02896 0.00536 AFIX 43 H8 2 0.683885 0.007261 0.234020 11.00000 -1.20000 AFIX 0 C9 1 0.694386 0.209681 0.295603 11.00000 0.04769 0.04320 = 0.05108 0.00043 0.02133 0.00543 C10 1 0.819819 0.244514 0.306689 11.00000 0.04603 0.05646 = 0.06883 -0.00387 0.02847 0.01037 AFIX 43 H10 2 0.864765 0.178416 0.283658 11.00000 -1.20000 AFIX 0 C11 1 0.875878 0.371996 0.350103 11.00000 0.03741 0.06064 = 0.06467 -0.00041 0.02527 0.00492 AFIX 43 H11 2 0.958838 0.392640 0.358600 11.00000 -1.20000 AFIX 0 C12 1 0.805096 0.471669 0.381771 11.00000 0.03678 0.04743 = 0.04497 -0.00074 0.01763 0.00084 C13 1 0.753351 0.916366 0.545598 11.00000 0.05366 0.04486 = 0.06850 -0.00036 0.02140 0.00440 AFIX 43 H13 2 0.713298 0.976014 0.482183 11.00000 -1.20000 AFIX 0 C14 1 0.775807 0.774788 0.539662 11.00000 0.03561 0.04258 = 0.05350 -0.00422 0.01871 -0.00349 C15 1 0.839307 0.725252 0.657236 11.00000 0.03441 0.04591 = 0.05018 -0.00546 0.02087 -0.00784 C16 1 0.889912 0.594063 0.708532 11.00000 0.04188 0.04974 = 0.06034 0.00074 0.02309 -0.00516 AFIX 43 H16 2 0.884455 0.514622 0.663171 11.00000 -1.20000 AFIX 0 C17 1 0.947856 0.584693 0.827210 11.00000 0.05581 0.07552 = 0.05975 0.01097 0.02278 -0.00538 AFIX 43 H17 2 0.981161 0.497734 0.861910 11.00000 -1.20000 AFIX 0 C18 1 0.957593 0.702281 0.896110 11.00000 0.06786 0.10646 = 0.05024 -0.00390 0.02166 -0.01540 AFIX 43 H18 2 0.997462 0.692769 0.976112 11.00000 -1.20000 AFIX 0 C19 1 0.909971 0.831134 0.848914 11.00000 0.07190 0.08937 = 0.05810 -0.02932 0.02785 -0.01385 AFIX 43 H19 2 0.916148 0.909414 0.895615 11.00000 -1.20000 AFIX 0 C20 1 0.851631 0.843239 0.728835 11.00000 0.04749 0.05628 = 0.06104 -0.01377 0.02651 -0.00574 C21 1 0.501706 0.631518 0.332762 11.00000 0.03502 0.03720 = 0.05906 -0.00521 0.01878 -0.00251 C22 1 0.449925 0.614838 0.214372 11.00000 0.05418 0.05667 = 0.05935 -0.00408 0.01352 0.00698 AFIX 43 H22 2 0.493550 0.561667 0.180762 11.00000 -1.20000 AFIX 0 C23 1 0.331474 0.678192 0.144912 11.00000 0.06567 0.06792 = 0.07732 0.00331 -0.00237 -0.00053 AFIX 43 H23 2 0.295695 0.665519 0.065195 11.00000 -1.20000 AFIX 0 C24 1 0.268188 0.758671 0.193904 11.00000 0.04363 0.05070 = 0.13378 0.00111 0.01423 0.00671 AFIX 43 H24 2 0.189944 0.801132 0.147161 11.00000 -1.20000 AFIX 0 C25 1 0.318864 0.777032 0.310457 11.00000 0.05002 0.04999 = 0.13244 -0.00448 0.04359 0.00386 AFIX 43 H25 2 0.276116 0.832688 0.343434 11.00000 -1.20000 AFIX 0 C26 1 0.434039 0.712475 0.379207 11.00000 0.04686 0.04628 = 0.08714 -0.00804 0.03591 -0.00145 AFIX 43 H26 2 0.467307 0.723519 0.458985 11.00000 -1.20000 AFIX 0 C27 1 0.935421 0.708796 0.308601 11.00000 0.07254 0.06185 = 0.10754 -0.00381 0.06082 -0.01159 PART 1 C28 1 0.814611 0.728837 0.119905 10.50000 0.16233 0.14572 = 0.06805 0.00701 0.05372 -0.02714 AFIX 23 H28A 2 0.887687 0.692201 0.108702 10.50000 -1.20000 H28B 2 0.812493 0.831840 0.113261 10.50000 -1.20000 AFIX 0 C29 1 0.688094 0.661739 0.035122 10.50000 0.17066 0.13897 = 0.05118 0.00457 0.03489 -0.03553 AFIX 23 H29A 2 0.618494 0.713341 0.042331 10.50000 -1.20000 H29B 2 0.680729 0.679548 -0.042253 10.50000 -1.20000 AFIX 0 C30 1 0.664916 0.513118 0.042583 10.50000 0.25363 0.21142 = 0.07872 -0.03488 0.02007 -0.00617 AFIX 137 H30A 2 0.582907 0.487811 -0.018029 10.50000 -1.50000 H30B 2 0.664669 0.493143 0.116209 10.50000 -1.50000 H30C 2 0.731621 0.458685 0.034574 10.50000 -1.50000 AFIX 0 PART 0 PART 2 C28' 1 0.790827 0.673363 0.095089 10.50000 0.16067 0.13880 = 0.06779 0.00127 0.06828 -0.02675 AFIX 23 H28C 2 0.871338 0.669432 0.087187 10.50000 -1.20000 H28D 2 0.741809 0.587848 0.061205 10.50000 -1.20000 AFIX 0 C29' 1 0.715423 0.803375 0.035696 10.50000 0.18034 0.15737 = 0.08850 -0.00100 0.05513 -0.01756 AFIX 23 H29C 2 0.756265 0.887142 0.080841 10.50000 -1.20000 H29D 2 0.716561 0.812977 -0.039489 10.50000 -1.20000 AFIX 0 C30' 1 0.586229 0.796314 0.021431 10.50000 0.12156 0.16479 = 0.07412 -0.00017 0.03347 -0.01437 AFIX 137 H30D 2 0.546134 0.712195 -0.021504 10.50000 -1.50000 H30E 2 0.540280 0.878990 -0.019796 10.50000 -1.50000 H30F 2 0.584550 0.792962 0.095909 10.50000 -1.50000 AFIX 0 HKLF 4 REM mjr17066_0m_a.res in P2(1) REM R1 = 0.0491 for 4886 Fo > 4sig(Fo) and 0.0576 for all 5520 data REM 346 parameters refined using 77 restraints END WGHT 0.0344 0.2887 REM Highest difference peak 0.222, deepest hole -0.151, 1-sigma level 0.033 Q1 1 0.7764 0.5610 0.0476 11.00000 0.05 0.22 Q2 1 0.3568 0.6621 0.0803 11.00000 0.05 0.15 Q3 1 0.9537 0.8230 0.2626 11.00000 0.05 0.13 Q4 1 0.7246 0.7214 0.1018 11.00000 0.05 0.13 Q5 1 0.8620 1.0392 0.6569 11.00000 0.05 0.13 Q6 1 0.8552 0.7798 0.6995 11.00000 0.05 0.12 Q7 1 0.5192 0.3218 0.2753 11.00000 0.05 0.12 Q8 1 0.3656 0.7781 0.4394 11.00000 0.05 0.12 Q9 1 0.8413 0.6532 0.1367 11.00000 0.05 0.12 Q10 1 0.6239 0.6508 0.0419 11.00000 0.05 0.12 Q11 1 0.5425 0.6958 0.3728 11.00000 0.05 0.11 Q12 1 0.9091 0.2805 0.4363 11.00000 0.05 0.11 Q13 1 0.6877 0.6295 0.4256 11.00000 0.05 0.11 Q14 1 0.3310 0.1352 0.2185 11.00000 0.05 0.11 Q15 1 0.4544 0.3826 0.3048 11.00000 0.05 0.11 Q16 1 0.8989 0.6361 0.8452 11.00000 0.05 0.11 Q17 1 0.7360 0.7291 0.4831 11.00000 0.05 0.11 Q18 1 0.3797 0.6303 0.0025 11.00000 0.05 0.11 Q19 1 0.6601 0.5014 0.3954 11.00000 0.05 0.11 Q20 1 0.8578 0.9022 0.7009 11.00000 0.05 0.10 ; _shelx_res_checksum 21628 _shelx_hkl_file ; -1 0 0 110.995 3.75867 7 2 0 0 731.306 22.0695 7 -2 0 0 782.606 22.7862 7 3 0 0 950.269 28.5490 7 -3 0 0 998.020 29.6662 7 4 0 0 123.135 4.68980 7 -4 0 0 122.826 5.75276 7 -5 0 0 162.829 7.55671 7 5 0 0 150.600 5.91572 7 -5 0 0 157.583 6.99230 2 -6 0 0 995.549 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-1 -1 14 -0.0765 1.57566 4 -1 -1 14 0.44942 1.82307 6 -1 1 14 3.09629 1.92690 4 -1 1 14 5.62173 2.14027 6 0 -1 14 2.64870 1.86378 6 0 -1 14 1.78852 1.64075 4 1 -1 14 1.00706 1.84472 6 1 -1 14 1.76701 1.60979 4 -12 2 14 7.76833 3.84360 5 -11 -2 14 52.5418 4.70384 2 -11 2 14 55.0776 6.60368 5 -10 -2 14 11.0477 3.27362 6 -10 -2 14 6.12459 6.81883 7 -10 -2 14 12.5087 2.84754 2 -10 2 14 8.66786 4.59222 5 -10 2 14 9.51334 2.51053 6 -9 -2 14 -3.8868 3.64996 7 -9 -2 14 2.97230 2.35029 6 -8 -2 14 9.52351 2.25164 2 -8 -2 14 12.0350 4.05564 7 -7 -2 14 20.3099 3.38948 2 -7 -2 14 22.5350 4.18035 7 -7 -2 14 15.8047 3.12651 6 -6 -2 14 1.88663 1.49746 2 -6 -2 14 -0.5759 1.32097 6 -6 2 14 -0.1281 2.24524 6 -5 -2 14 -0.7885 1.29059 6 -5 -2 14 -2.4156 1.16215 2 -5 -2 14 1.39238 3.25467 7 -5 2 14 -1.3037 2.00711 4 5 2 -14 5.01502 3.29468 1 -5 2 14 2.78857 1.86005 6 -4 -2 14 7.73596 2.04798 2 -4 -2 14 8.76175 2.99484 6 -4 2 14 5.90549 1.88979 6 -4 2 14 9.88189 2.17327 4 -3 -2 14 -0.8039 1.17123 6 -3 -2 14 4.37676 3.19460 4 -3 -2 14 -0.5080 3.66149 7 -2 -2 14 10.3276 2.41521 4 -2 -2 14 16.0485 3.26579 6 -2 2 14 11.5121 2.95542 4 -2 2 14 12.4430 3.55195 6 -1 -2 14 2.93526 1.82622 4 -1 -2 14 1.93308 2.12207 2 -1 2 14 4.74965 2.30023 6 -1 2 14 1.05896 1.36078 4 0 -2 14 5.89316 1.75007 6 0 -2 14 7.88490 1.83472 4 0 2 14 8.44033 2.33616 6 0 2 14 6.13478 2.08817 4 1 -2 14 6.43851 2.39240 4 1 -2 14 4.57383 2.08977 6 1 2 14 7.56874 1.94036 4 -11 -3 14 5.53889 1.86099 2 -11 3 14 7.51031 2.24206 6 -10 -3 14 2.59537 1.78764 2 -10 -3 14 5.14849 3.64832 7 -9 -3 14 11.5892 3.39302 7 -9 -3 14 6.00059 1.90484 2 -8 -3 14 4.48086 2.86540 7 -8 -3 14 5.85010 2.22060 2 8 3 -14 2.61865 1.77737 1 -8 3 14 3.22286 2.69062 6 -7 -3 14 8.82656 2.41775 2 -7 -3 14 3.97422 2.73289 6 -7 3 14 7.90754 2.64562 6 7 3 -14 8.70390 2.23195 1 -6 -3 14 6.03470 2.11013 2 -6 -3 14 4.74619 3.34555 7 -6 3 14 9.87945 2.70352 4 -6 3 14 11.4784 3.17729 6 -5 -3 14 12.2750 3.17182 7 -5 -3 14 5.54660 2.19900 6 -5 -3 14 9.33141 2.13964 2 5 3 -14 11.1548 2.24029 1 -5 3 14 7.47874 2.98014 6 -5 3 14 2.65372 3.44775 4 -4 -3 14 11.0201 2.44710 2 -4 -3 14 8.82406 2.60456 4 -4 -3 14 11.7770 2.82400 6 -4 3 14 12.3098 3.57236 4 4 3 -14 7.98616 3.33738 1 -3 -3 14 20.7089 5.56067 6 -3 -3 14 28.2007 3.17330 4 -3 3 14 25.9788 5.78414 6 -3 3 14 28.8733 4.74810 4 -2 -3 14 4.03532 1.68450 6 -2 -3 14 2.34973 1.44635 2 -2 3 14 4.12892 1.99806 6 -2 3 14 5.56018 2.49588 4 -1 -3 14 3.65205 1.50960 6 -1 3 14 5.35955 2.19471 6 -1 3 14 2.22164 1.79791 4 0 -3 14 5.74328 1.78764 4 0 -3 14 10.7823 2.50592 2 0 3 14 6.20182 2.93239 6 1 -3 14 1.75973 1.67823 4 1 -3 14 3.51537 1.89598 6 1 3 14 0.75956 1.39364 4 -11 -4 14 23.0059 3.34970 2 -11 4 14 15.3194 3.04010 6 -10 4 14 12.1265 2.83613 6 -9 -4 14 2.59044 1.69768 2 -9 -4 14 0.23763 3.17771 7 -9 4 14 6.33600 2.22349 6 9 4 -14 1.69629 1.17512 1 -8 -4 14 12.9505 2.80732 6 -8 -4 14 19.0494 3.91299 7 -8 -4 14 18.5356 2.93936 2 -8 4 14 23.9453 3.74373 6 8 4 -14 16.2123 2.77909 1 -7 -4 14 4.47596 2.04242 2 -7 -4 14 7.65282 1.81761 6 -7 4 14 6.70719 2.50960 6 7 4 -14 9.98080 2.39942 1 -6 -4 14 1.69418 1.52196 6 -6 -4 14 -0.3454 3.36537 7 -6 4 14 5.13804 1.78374 4 6 4 -14 -1.4561 1.62874 1 -6 4 14 5.08495 2.49962 6 -5 -4 14 1.42337 2.41827 7 5 -4 -14 5.83674 2.85554 2 -5 4 14 6.62264 2.23690 4 5 4 -14 5.71325 2.12133 1 -5 4 14 2.68436 2.10189 6 4 -4 -14 4.96641 2.05665 2 -4 -4 14 2.64877 1.39725 2 -4 -4 14 -1.1375 3.04297 7 -4 4 14 4.19679 1.95344 6 -4 4 14 6.31458 1.81724 4 -3 -4 14 31.5011 4.25511 6 3 -4 -14 28.3447 3.00422 2 -3 -4 14 33.9619 3.89427 2 -3 -4 14 20.6225 3.22215 4 -3 4 14 25.2929 4.50041 4 -3 4 14 24.8885 4.22626 6 -2 -4 14 9.74775 2.03434 4 -2 -4 14 8.84726 2.56722 6 2 -4 -14 9.34251 2.28212 2 -2 -4 14 8.65505 1.82092 2 -2 4 14 9.11642 2.40141 4 -2 4 14 15.7758 3.38387 6 1 -4 -14 75.8446 5.05248 2 -1 -4 14 74.1078 4.87593 2 -1 -4 14 71.2839 4.87958 4 -1 -4 14 63.6745 5.36253 6 -1 4 14 71.5608 5.72121 4 -1 4 14 65.8580 5.62851 6 0 -4 14 20.2269 3.57747 4 0 -4 14 16.6809 2.71293 2 0 4 14 20.8979 3.27069 4 -9 -5 14 1.22846 1.53160 2 9 5 -14 0.21338 1.42082 1 -8 -5 14 0.42560 2.29030 6 8 5 -14 2.97044 1.95253 1 -8 5 14 3.47681 1.94644 6 -7 -5 14 1.89315 1.42683 6 -7 -5 14 5.32516 1.74476 2 7 5 -14 3.53775 1.58797 1 -7 5 14 4.38851 1.59406 6 -6 -5 14 9.09425 2.04973 6 -6 -5 14 10.6143 3.34037 7 -6 -5 14 10.3332 2.17019 2 6 -5 -14 4.81575 3.00551 2 6 5 -14 6.29450 2.32048 1 -6 5 14 6.31431 2.35812 6 -5 -5 14 31.4614 4.12605 6 -5 -5 14 31.9073 3.92702 2 5 -5 -14 39.3101 3.25886 2 -5 -5 14 32.5985 6.55053 7 5 5 -14 36.2003 3.57559 1 -5 5 14 28.5012 4.10240 4 -5 5 14 38.6711 5.84597 6 -4 -5 14 7.83053 1.84961 2 -4 -5 14 4.50405 1.71843 6 4 5 -14 11.2968 2.50268 1 -4 5 14 6.52383 2.55418 6 -4 5 14 10.3491 2.66033 4 -3 -5 14 22.5721 3.50471 6 -3 -5 14 21.6006 3.02094 2 3 -5 -14 26.1459 2.76845 2 3 5 -14 17.5501 2.83089 1 -3 5 14 22.2257 3.60415 4 -3 5 14 28.8589 4.55361 6 -2 -5 14 3.22893 1.67047 2 -2 -5 14 4.49357 1.78409 6 -2 5 14 8.21544 2.79188 4 -1 -5 14 3.29698 2.08601 4 -1 5 14 8.39303 2.26990 6 -1 5 14 3.94899 1.74556 4 -8 -6 14 2.63287 1.63811 2 -8 6 14 0.32338 1.48942 6 8 6 -14 1.02761 1.24089 1 -7 -6 14 6.49763 1.92052 2 -7 -6 14 4.88383 2.11511 6 -7 6 14 1.64868 2.04914 6 -6 -6 14 14.1403 2.71051 6 6 -6 -14 12.6831 2.04814 2 -6 6 14 16.5737 3.85258 6 -5 -6 14 1.38076 1.39001 6 5 -6 -14 4.56748 1.81039 2 5 6 -14 -0.7595 1.53354 1 -5 6 14 0.34435 2.32911 6 -4 -6 14 18.0792 2.57883 2 4 -6 -14 16.8039 2.48643 2 -4 -6 14 16.2239 2.61598 6 4 6 -14 11.9426 2.32255 1 -4 6 14 10.5691 3.04943 6 -3 -6 14 3.17006 1.77894 6 -3 -6 14 0.58685 1.28765 2 3 6 -14 2.62018 1.69843 1 -3 6 14 4.45963 3.55876 6 -11 0 15 -0.1144 2.87985 5 -11 0 15 5.05334 2.82939 2 -11 0 15 5.65895 2.73396 6 -10 0 15 11.3190 2.61803 6 -9 0 15 2.16512 1.63744 6 -8 0 15 32.4244 4.90457 6 -8 0 15 29.2981 3.65013 2 -7 0 15 0.66678 1.79348 6 -6 0 15 0.66279 2.22349 2 -6 0 15 2.22795 2.05021 6 -5 0 15 -2.5669 2.23033 4 -5 0 15 2.06854 2.70996 2 -5 0 15 0.77892 1.47526 6 -4 0 15 23.3220 3.45265 4 -4 0 15 27.4023 4.50679 6 -3 0 15 2.02024 1.41635 4 -3 0 15 0.44795 1.39780 6 -2 0 15 5.70785 1.98008 4 -1 0 15 1.04520 1.44005 4 -1 0 15 1.34967 1.87074 6 -11 1 15 -1.2241 2.40411 6 -11 1 15 0.56346 4.33063 5 -10 -1 15 26.1471 3.49220 2 -10 1 15 31.9744 3.73046 6 -9 -1 15 30.7284 4.20896 6 -9 1 15 28.2042 3.69321 6 -9 1 15 30.4256 7.87094 5 -8 -1 15 -1.9236 1.37228 6 -8 -1 15 2.14487 1.64994 2 -8 1 15 -0.0435 1.86904 6 -7 -1 15 13.4204 2.41940 2 -7 -1 15 19.8189 6.49523 7 -6 -1 15 -1.2908 1.52209 6 -6 1 15 -1.5094 1.23537 6 -6 1 15 -1.5077 2.75862 4 -5 -1 15 0.25430 1.81412 2 -5 -1 15 3.68236 2.05630 6 -5 1 15 1.99142 1.48196 6 -4 -1 15 3.76614 2.20136 2 -4 1 15 3.91490 2.14254 4 -3 -1 15 4.14289 2.14105 6 -3 -1 15 -0.5980 1.54491 4 -3 -1 15 -4.0641 2.75721 2 -3 1 15 0.42346 2.06612 6 -2 -1 15 5.35517 1.76115 4 -2 1 15 9.02826 2.25004 4 -1 -1 15 29.7472 3.68767 4 -1 1 15 21.6395 3.53920 4 -1 1 15 26.2204 4.60690 6 -11 -2 15 20.5806 2.77250 2 -11 2 15 15.4264 3.27451 6 -10 -2 15 32.9635 4.05402 2 -10 -2 15 33.6926 3.90358 6 -10 2 15 37.8752 4.44133 6 -9 -2 15 30.3966 3.75448 6 -9 -2 15 32.8657 3.70542 2 -8 -2 15 16.1313 2.76742 2 -8 -2 15 14.8760 3.15779 6 -8 2 15 14.4627 3.29922 6 -7 -2 15 11.9079 4.35588 7 -7 -2 15 7.71464 2.12440 2 -7 -2 15 8.67890 2.43379 6 -7 2 15 4.70889 2.25500 6 -6 -2 15 10.7657 2.11249 2 -6 -2 15 22.0114 5.59701 7 -6 -2 15 11.8888 2.77897 6 -6 2 15 9.70156 3.28394 6 -5 -2 15 3.56616 2.11309 6 -5 -2 15 7.34970 2.15987 2 -5 2 15 6.14196 2.32892 4 -5 2 15 6.96271 2.58353 6 -4 -2 15 2.08261 1.92759 6 -4 -2 15 3.29589 2.40950 4 -4 -2 15 -0.3415 1.80787 2 -4 2 15 3.51783 1.99888 6 -4 2 15 2.47398 1.63257 4 -3 2 15 5.60171 1.64190 4 -3 2 15 4.16474 2.05470 6 -2 -2 15 -1.2653 1.42725 6 -2 2 15 4.64444 1.93648 6 -2 2 15 4.38737 1.69794 4 -1 -2 15 8.80291 2.19282 4 -1 2 15 10.0620 2.08744 4 -1 2 15 13.5100 3.22298 6 -10 -3 15 14.5958 2.47964 2 -10 3 15 11.7551 2.40864 6 -9 -3 15 3.93769 2.44297 6 -9 -3 15 3.53653 1.89738 2 -9 3 15 5.47244 2.19974 6 -8 -3 15 16.9582 3.33102 6 -8 -3 15 20.0585 3.16127 2 -7 -3 15 -2.0066 3.84828 7 -7 -3 15 1.75493 1.51409 6 -7 -3 15 1.57394 1.29602 2 -6 -3 15 0.85983 1.43656 6 -6 -3 15 3.61050 1.64937 2 -6 3 15 1.53654 1.83117 6 -6 3 15 2.22641 1.93538 4 -5 -3 15 8.28220 1.88286 6 -5 -3 15 5.77820 1.76547 2 -5 3 15 9.69119 3.14826 6 -4 -3 15 1.29594 1.02258 6 -4 -3 15 -1.3477 1.58618 2 -4 3 15 -1.5571 1.77367 4 -4 3 15 0.49074 1.21840 6 -3 -3 15 1.94079 1.23495 6 -3 -3 15 -3.1101 1.92647 4 -3 3 15 3.39572 2.02464 4 -2 -3 15 27.3882 3.33480 4 -2 -3 15 16.8970 2.56353 6 -2 3 15 21.9923 3.36776 4 -1 -3 15 5.97827 1.81130 4 -1 3 15 4.89082 2.18281 6 -1 3 15 4.90899 1.61026 4 -9 4 15 3.42596 1.89773 6 -8 -4 15 3.72098 1.75094 2 -8 -4 15 1.88304 2.39082 6 8 4 -15 0.55722 1.97854 1 -8 4 15 4.57208 1.79721 6 -7 -4 15 7.83733 2.04518 2 7 4 -15 3.77284 2.19639 1 -7 4 15 5.55358 2.11053 6 -6 -4 15 3.02734 1.68766 2 -6 -4 15 3.75587 1.55111 6 6 4 -15 5.55154 2.08626 1 -5 -4 15 11.3118 2.84146 6 -5 4 15 7.20522 2.15494 6 -5 4 15 7.14356 1.99382 4 -4 -4 15 5.10658 2.12660 6 -4 -4 15 1.49683 1.20279 2 -4 4 15 1.06589 2.09339 6 -3 -4 15 15.8461 2.96683 6 -3 4 15 17.3890 3.96049 6 -7 -5 15 1.30030 1.84329 6 7 5 -15 0.60115 1.62965 1 -7 5 15 -1.4492 1.33819 6 -6 -5 15 8.20887 1.75999 6 -5 -5 15 14.8634 2.60007 2 -5 -5 15 16.8789 3.13051 6 -5 5 15 17.8073 3.70013 6 -9 0 16 12.5022 2.15645 6 -8 0 16 0.67827 1.64364 6 -7 0 16 2.41742 1.91450 6 -6 0 16 4.78572 1.92692 6 -5 0 16 4.61614 1.97342 6 -4 0 16 4.05769 2.25521 6 -4 0 16 1.03523 2.01085 4 -3 0 16 8.65753 2.16548 4 -3 0 16 8.28442 2.95929 6 -9 -1 16 16.1140 2.80319 2 -9 1 16 20.1177 3.09637 6 -8 -1 16 6.80943 2.87947 2 -8 -1 16 9.68872 2.13511 6 -7 -1 16 1.92576 1.67735 6 -7 1 16 3.48788 1.76264 6 -6 -1 16 11.3146 2.69311 2 -5 -1 16 -0.6027 1.28590 6 -5 1 16 1.54804 1.61518 6 -5 1 16 1.74355 2.41958 4 -4 -1 16 -0.2942 1.36245 6 -4 1 16 2.21508 1.91699 6 -3 -1 16 16.3519 3.03449 6 -3 1 16 11.6129 1.88702 4 -3 1 16 11.6493 2.51537 6 -8 -2 16 24.4237 3.85409 6 -8 2 16 24.9011 3.82476 6 -7 -2 16 6.48664 2.25010 6 -7 2 16 3.21004 1.83756 6 -6 -2 16 3.08751 2.04315 6 -6 2 16 3.32058 1.93388 6 -5 2 16 2.85673 2.08698 4 -4 -2 16 7.26444 2.19456 6 -4 -2 16 -1.3001 3.00147 2 -4 2 16 2.87409 2.09870 4 -4 2 16 4.10613 2.24990 6 -7 -3 16 14.5781 2.65153 2 -7 -3 16 11.0127 2.79923 6 -7 3 16 11.8702 3.01652 6 -6 -3 16 0.21350 1.45104 2 -6 3 16 -0.0299 1.63375 6 -5 -3 16 5.40647 1.93738 6 -5 -3 16 6.07177 2.37275 2 -5 3 16 7.91125 1.84073 4 -5 3 16 4.70977 2.02140 6 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7519 _exptl_absorpt_correction_T_min 0.6147 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 1.34181 11.452 9.390 12.774 90.001 115.068 90.004 ) ; _shelx_hkl_checksum 18060 _olex2_submission_special_instructions 'No special instructions were received'