#============================================================================== # 1. SUBMISSION DETAILS data_global _audit_update_record ; 2013-07-09 # Formatted by publCIF ; _publ_contact_author ; Constantin G. Daniliuc Organisch-Chemisches Institut Westf\"alische Wilhelm-Universit\"at M\"unster 48149 M\"unster Germany ; _publ_contact_author_phone '049 251 83-36522' _publ_contact_author_fax '049 251 83-39772' _publ_contact_author_email 'constantin.daniliuc@uni-muenster.de' _publ_requested_journal 'Org. Lett.' #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Multicomponent 1,3-Bifunctionalization of Donar-Acceptor Cyclopropanes with Arenes and Nitrosoarenes ; loop_ _publ_author_name _publ_author_address 'Das, Saikat' ; Organisch-Chemisches Institut Westf\"alische Wilhelms-Universit\"at M\"unster Corrensstrasse 40 48149 M\"unster Germany ; 'Daniliuc, Constantin G.' ; Organisch-Chemisches Institut Westf\"alische Wilhelms-Universit\"at M\"unster Corrensstrasse 40 48149 M\"unster Germany ; 'Studer, Armido' ; Organisch-Chemisches Institut Westf\"alische Wilhelms-Universit\"at M\"unster Corrensstrasse 40 48149 M\"unster Germany ; #============================================================================= # cif data for "stu8307" (compound 4o) #============================================================================= data_stu8307 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H30 Br N O5' _chemical_formula_iupac ? _chemical_formula_weight 540.44 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.3030(3) _cell_length_b 17.7016(6) _cell_length_c 17.5144(5) _cell_angle_alpha 90 _cell_angle_beta 99.2930(10) _cell_angle_gamma 90 _cell_volume 2540.42(15) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9888 _cell_measurement_theta_min 2.5732 _cell_measurement_theta_max 27.4769 _cell_measurement_temperature 100.(2) _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.229 _exptl_crystal_size_mid 0.125 _exptl_crystal_size_min 0.074 _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 1.657 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Bruker AXS (2014). SADABS, Version 2014/2, Bruker AXS Inc., Madison, Wisconsin, USA. ; _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.89 _exptl_special_details ; ; _diffrn_ambient_temperature 100.(2) _diffrn_source 'Mo ImS' _diffrn_source_type 'micro focus tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'MX mirror' _diffrn_measurement_device_type 'Bruker D8 Venture PHOTON 100 CMOS' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean 10.4167 _diffrn_reflns_number 62057 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_unetI/netI 0.0254 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 27.53 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _refine_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_number_total 5840 _reflns_number_gt 4905 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.0687 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.054 _refine_ls_number_reflns 5840 _refine_ls_number_parameters 334 _refine_ls_number_restraints 1 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+2.0843P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.428 _refine_diff_density_min -0.568 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ; APEX2 v.2014.1-1 (Bruker AXS Inc., 2014) ; _computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics 'XP (Sheldrick, 2014)' _computing_publication_material 'SHELXL-2014 (Sheldrick, 2014)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br Br1 0.35019(2) 0.62728(2) 0.82140(2) 0.02111(6) Uani d . . . 1.0 . . N N1 0.41202(19) 0.69483(8) 0.66886(8) 0.0147(3) Uani d . . . 1.0 . . H H1 0.335(3) 0.6919(12) 0.6898(12) 0.014(5) Uiso d . . . 1.0 . . O O1 0.57624(19) 0.86058(8) 0.60322(8) 0.0285(3) Uani d . . . 1.0 . . O O2 0.47262(16) 0.84292(7) 0.71307(8) 0.0229(3) Uani d . . . 1.0 . . O O3 0.11824(16) 0.75317(8) 0.64799(8) 0.0240(3) Uani d . . . 1.0 . . O O4 0.17128(17) 0.83658(7) 0.55813(9) 0.0282(3) Uani d . . . 1.0 . . O O5 0.99387(16) 0.61101(8) 0.85680(8) 0.0257(3) Uani d . . . 1.0 . . C C1 0.3626(2) 0.65316(9) 0.50726(10) 0.0140(3) Uani d . . . 1.0 . . H H1A 0.4145 0.6176 0.5483 0.017 Uiso calc U . R 1.0 . . C C2 0.4255(2) 0.73247(9) 0.53159(10) 0.0143(3) Uani d . . . 1.0 . . H H2A 0.3738 0.7695 0.4929 0.017 Uiso calc U . R 1.0 . . H H2B 0.5448 0.7342 0.5318 0.017 Uiso calc U . R 1.0 . . C C3 0.3900(2) 0.75561(9) 0.61269(10) 0.0144(3) Uani d . . . 1.0 . . C C4 0.4926(2) 0.82651(10) 0.64123(10) 0.0162(4) Uani d . . . 1.0 . . C C5 0.5610(2) 0.90810(11) 0.75053(11) 0.0233(4) Uani d . . . 1.0 . . H H5A 0.6319 0.9302 0.716 0.028 Uiso calc U . R 1.0 . . H H5B 0.6307 0.8922 0.7992 0.028 Uiso calc U . R 1.0 . . C C6 0.4397(3) 0.96493(12) 0.76736(15) 0.0368(5) Uani d . . . 1.0 . . H H6A 0.3707 0.98 0.719 0.055 Uiso calc U . R 1.0 . . H H6B 0.4968 1.0093 0.7918 0.055 Uiso calc U . R 1.0 . . H H6C 0.3715 0.9429 0.8023 0.055 Uiso calc U . R 1.0 . . C C7 0.2093(2) 0.78047(10) 0.60890(11) 0.0188(4) Uani d . . . 1.0 . . C C8 0.0008(3) 0.86177(12) 0.54713(18) 0.0448(7) Uani d . . D 1.0 . . H H8A -0.0267 0.8841 0.4948 0.054 Uiso calc U P R 0.526(6) A 1 H H8B -0.0698 0.817 0.549 0.054 Uiso calc U P R 0.526(6) A 1 H H8C -0.0529 0.8421 0.5896 0.054 Uiso calc U P R 0.474(6) A 2 H H8D -0.0582 0.8417 0.4977 0.054 Uiso calc U P R 0.474(6) A 2 C C9 -0.0346(5) 0.9127(2) 0.5993(2) 0.0280(12) Uani d . P D 0.526(6) A 1 H H9A -0.0313 0.888 0.6496 0.042 Uiso calc U P R 0.526(6) A 1 H H9B -0.144 0.9333 0.5821 0.042 Uiso calc U P R 0.526(6) A 1 H H9C 0.0456 0.9537 0.6041 0.042 Uiso calc U P R 0.526(6) A 1 C C9A -0.0060(6) 0.9447(2) 0.5463(3) 0.0284(13) Uani d . P D 0.474(6) A 2 H H9A1 0.063 0.9645 0.5927 0.043 Uiso calc U P R 0.474(6) A 2 H H9A2 -0.1189 0.9612 0.5456 0.043 Uiso calc U P R 0.474(6) A 2 H H9A3 0.0333 0.9637 0.5001 0.043 Uiso calc U P R 0.474(6) A 2 C C11 0.5582(2) 0.67750(9) 0.71657(9) 0.0131(3) Uani d . . . 1.0 . . C C12 0.5560(2) 0.64315(9) 0.78852(10) 0.0143(3) Uani d . . . 1.0 . . C C13 0.6963(2) 0.61943(10) 0.83652(10) 0.0165(3) Uani d . . . 1.0 . . H H13 0.6896 0.5958 0.8846 0.02 Uiso calc U . R 1.0 . . C C14 0.8465(2) 0.63069(10) 0.81338(10) 0.0168(3) Uani d . . . 1.0 . . C C15 0.8539(2) 0.66517(10) 0.74258(10) 0.0185(4) Uani d . . . 1.0 . . H H15 0.9567 0.6731 0.7267 0.022 Uiso calc U . R 1.0 . . C C16 0.7123(2) 0.68790(10) 0.69530(10) 0.0154(3) Uani d . . . 1.0 . . H H16 0.7197 0.7112 0.6471 0.019 Uiso calc U . R 1.0 . . C C17 0.9897(3) 0.56556(11) 0.92381(11) 0.0249(4) Uani d . . . 1.0 . . H H17A 0.9372 0.5938 0.9612 0.037 Uiso calc U . R 1.0 . . H H17B 1.1013 0.5523 0.9473 0.037 Uiso calc U . R 1.0 . . H H17C 0.9276 0.5193 0.9089 0.037 Uiso calc U . R 1.0 . . C C21 0.4110(2) 0.62648(10) 0.43140(10) 0.0144(3) Uani d . . . 1.0 . . C C22 0.4629(2) 0.67393(10) 0.37714(11) 0.0191(4) Uani d . . . 1.0 . . H H22 0.4679 0.7269 0.3861 0.023 Uiso calc U . R 1.0 . . C C23 0.5077(3) 0.64480(12) 0.30952(12) 0.0265(4) Uani d . . . 1.0 . . H H23 0.5432 0.6778 0.2728 0.032 Uiso calc U . R 1.0 . . C C24 0.5003(3) 0.56730(12) 0.29608(12) 0.0293(5) Uani d . . . 1.0 . . H H24 0.5331 0.5472 0.2507 0.035 Uiso calc U . R 1.0 . . C C25 0.4454(2) 0.51969(11) 0.34867(12) 0.0263(4) Uani d . . . 1.0 . . H H25 0.4377 0.4669 0.3389 0.032 Uiso calc U . R 1.0 . . C C26 0.4014(2) 0.54894(10) 0.41568(11) 0.0201(4) Uani d . . . 1.0 . . H H26 0.364 0.5157 0.4517 0.024 Uiso calc U . R 1.0 . . C C31 0.1787(2) 0.64493(9) 0.50286(10) 0.0141(3) Uani d . . . 1.0 . . C C32 0.1156(2) 0.59424(10) 0.55106(10) 0.0189(4) Uani d . . . 1.0 . . H H32 0.1877 0.5657 0.5878 0.023 Uiso calc U . R 1.0 . . C C33 -0.0521(2) 0.58502(11) 0.54599(12) 0.0254(4) Uani d . . . 1.0 . . H H33 -0.094 0.5504 0.5793 0.031 Uiso calc U . R 1.0 . . C C34 -0.1582(2) 0.62611(11) 0.49264(12) 0.0266(4) Uani d . . . 1.0 . . H H34 -0.2727 0.6197 0.4892 0.032 Uiso calc U . R 1.0 . . C C35 -0.0967(2) 0.67687(11) 0.44400(12) 0.0244(4) Uani d . . . 1.0 . . H H35 -0.1693 0.7052 0.4073 0.029 Uiso calc U . R 1.0 . . C C36 0.0710(2) 0.68622(10) 0.44903(11) 0.0188(4) Uani d . . . 1.0 . . H H36 0.1126 0.7209 0.4157 0.023 Uiso calc U . R 1.0 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br1 0.01916(10) 0.02482(10) 0.02144(9) -0.00296(8) 0.00959(7) 0.00275(8) N1 0.0142(8) 0.0160(7) 0.0140(7) -0.0020(6) 0.0028(6) 0.0011(6) O1 0.0448(9) 0.0218(7) 0.0175(7) -0.0182(6) 0.0011(6) 0.0010(5) O2 0.0237(7) 0.0211(7) 0.0251(7) -0.0079(6) 0.0070(6) -0.0116(6) O3 0.0185(7) 0.0270(7) 0.0273(7) 0.0001(6) 0.0058(6) -0.0070(6) O4 0.0185(7) 0.0152(7) 0.0468(9) 0.0022(5) -0.0073(6) 0.0031(6) O5 0.0182(7) 0.0354(8) 0.0226(7) 0.0039(6) 0.0008(5) 0.0132(6) C1 0.0132(8) 0.0114(8) 0.0162(8) -0.0014(6) -0.0011(6) 0.0012(6) C2 0.0161(9) 0.0119(8) 0.0141(8) -0.0021(6) -0.0001(6) 0.0010(6) C3 0.0149(9) 0.0106(8) 0.0167(8) -0.0009(6) -0.0006(6) -0.0004(6) C4 0.0168(9) 0.0123(8) 0.0174(8) 0.0012(7) -0.0040(7) 0.0003(7) C5 0.0239(10) 0.0216(10) 0.0230(10) -0.0072(8) -0.0004(8) -0.0092(8) C6 0.0386(13) 0.0204(10) 0.0517(14) -0.0021(9) 0.0087(11) -0.0123(10) C7 0.0180(9) 0.0135(8) 0.0228(9) 0.0003(7) -0.0030(7) -0.0066(7) C8 0.0194(11) 0.0208(11) 0.088(2) 0.0058(9) -0.0110(12) 0.0067(12) C9 0.033(2) 0.026(2) 0.025(2) 0.0085(17) 0.0025(16) -0.0036(17) C9A 0.032(3) 0.021(2) 0.032(3) 0.0103(18) 0.0014(19) 0.0020(18) C11 0.0169(9) 0.0097(7) 0.0127(8) -0.0013(6) 0.0022(6) -0.0026(6) C12 0.0172(9) 0.0123(8) 0.0150(8) -0.0027(6) 0.0076(6) -0.0023(6) C13 0.0218(9) 0.0142(8) 0.0140(8) 0.0004(7) 0.0047(7) 0.0023(7) C14 0.0181(8) 0.0153(8) 0.0162(8) 0.0014(7) 0.0009(7) 0.0030(7) C15 0.0163(9) 0.0205(9) 0.0195(9) -0.0008(7) 0.0057(7) 0.0033(7) C16 0.0181(9) 0.0144(8) 0.0144(8) -0.0005(7) 0.0045(7) 0.0034(7) C17 0.0302(11) 0.0260(10) 0.0173(9) 0.0054(8) -0.0003(8) 0.0077(8) C21 0.0106(8) 0.0134(8) 0.0176(8) 0.0023(7) -0.0019(6) -0.0015(7) C22 0.0195(10) 0.0145(8) 0.0234(9) -0.0011(7) 0.0043(7) -0.0029(7) C23 0.0269(11) 0.0283(11) 0.0267(10) -0.0036(8) 0.0117(8) -0.0045(8) C24 0.0249(11) 0.0330(11) 0.0314(11) 0.0037(9) 0.0088(8) -0.0157(9) C25 0.0244(11) 0.0165(9) 0.0357(11) 0.0063(8) -0.0018(8) -0.0094(8) C26 0.0178(9) 0.0141(9) 0.0256(9) 0.0010(7) -0.0045(7) -0.0001(7) C31 0.0158(9) 0.0114(8) 0.0146(8) -0.0011(6) 0.0004(6) -0.0039(6) C32 0.0204(9) 0.0178(9) 0.0183(9) -0.0024(7) 0.0024(7) 0.0002(7) C33 0.0222(10) 0.0259(10) 0.0296(10) -0.0065(8) 0.0085(8) -0.0003(8) C34 0.0138(9) 0.0267(10) 0.0393(11) -0.0027(8) 0.0043(8) -0.0081(9) C35 0.0187(10) 0.0204(9) 0.0310(11) 0.0019(8) -0.0051(8) -0.0035(8) C36 0.0192(9) 0.0142(8) 0.0219(9) -0.0008(7) -0.0005(7) -0.0010(7) _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Br1 C12 . 1.9098(17) ? N1 C11 . 1.392(2) ? N1 C3 . 1.449(2) ? N1 H1 . 0.79(2) ? O1 C4 . 1.199(2) ? O2 C4 . 1.328(2) ? O2 C5 . 1.465(2) ? O3 C7 . 1.201(2) ? O4 C7 . 1.337(2) ? O4 C8 . 1.466(3) ? O5 C14 . 1.377(2) ? O5 C17 . 1.428(2) ? C1 C31 . 1.523(2) ? C1 C21 . 1.524(2) ? C1 C2 . 1.534(2) ? C1 H1A . 1.0 ? C2 C3 . 1.552(2) ? C2 H2A . 0.99 ? C2 H2B . 0.99 ? C3 C4 . 1.553(2) ? C3 C7 . 1.554(2) ? C5 C6 . 1.487(3) ? C5 H5A . 0.99 ? C5 H5B . 0.99 ? C6 H6A . 0.98 ? C6 H6B . 0.98 ? C6 H6C . 0.98 ? C8 C9 . 1.349(4) ? C8 C9A . 1.469(4) ? C8 H8A . 0.99 ? C8 H8B . 0.99 ? C8 H8C . 0.99 ? C8 H8D . 0.99 ? C9 H9A . 0.98 ? C9 H9B . 0.98 ? C9 H9C . 0.98 ? C9A H9A1 . 0.98 ? C9A H9A2 . 0.98 ? C9A H9A3 . 0.98 ? C11 C16 . 1.401(2) ? C11 C12 . 1.402(2) ? C12 C13 . 1.387(3) ? C13 C14 . 1.386(2) ? C13 H13 . 0.95 ? C14 C15 . 1.392(2) ? C15 C16 . 1.385(3) ? C15 H15 . 0.95 ? C16 H16 . 0.95 ? C17 H17A . 0.98 ? C17 H17B . 0.98 ? C17 H17C . 0.98 ? C21 C22 . 1.388(2) ? C21 C26 . 1.400(2) ? C22 C23 . 1.396(3) ? C22 H22 . 0.95 ? C23 C24 . 1.392(3) ? C23 H23 . 0.95 ? C24 C25 . 1.379(3) ? C24 H24 . 0.95 ? C25 C26 . 1.384(3) ? C25 H25 . 0.95 ? C26 H26 . 0.95 ? C31 C32 . 1.391(2) ? C31 C36 . 1.396(2) ? C32 C33 . 1.390(3) ? C32 H32 . 0.95 ? C33 C34 . 1.383(3) ? C33 H33 . 0.95 ? C34 C35 . 1.391(3) ? C34 H34 . 0.95 ? C35 C36 . 1.391(3) ? C35 H35 . 0.95 ? C36 H36 . 0.95 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C11 N1 C3 . . 124.97(15) ? C11 N1 H1 . . 113.5(15) ? C3 N1 H1 . . 110.0(15) ? C4 O2 C5 . . 117.81(15) ? C7 O4 C8 . . 115.64(17) ? C14 O5 C17 . . 117.31(15) ? C31 C1 C21 . . 109.26(13) ? C31 C1 C2 . . 113.29(14) ? C21 C1 C2 . . 113.55(14) ? C31 C1 H1A . . 106.8 ? C21 C1 H1A . . 106.8 ? C2 C1 H1A . . 106.8 ? C1 C2 C3 . . 112.91(14) ? C1 C2 H2A . . 109.0 ? C3 C2 H2A . . 109.0 ? C1 C2 H2B . . 109.0 ? C3 C2 H2B . . 109.0 ? H2A C2 H2B . . 107.8 ? N1 C3 C2 . . 113.80(14) ? N1 C3 C4 . . 112.26(14) ? C2 C3 C4 . . 109.41(14) ? N1 C3 C7 . . 104.72(14) ? C2 C3 C7 . . 111.13(14) ? C4 C3 C7 . . 105.10(13) ? O1 C4 O2 . . 126.03(16) ? O1 C4 C3 . . 124.36(16) ? O2 C4 C3 . . 109.61(15) ? O2 C5 C6 . . 108.36(16) ? O2 C5 H5A . . 110.0 ? C6 C5 H5A . . 110.0 ? O2 C5 H5B . . 110.0 ? C6 C5 H5B . . 110.0 ? H5A C5 H5B . . 108.4 ? C5 C6 H6A . . 109.5 ? C5 C6 H6B . . 109.5 ? H6A C6 H6B . . 109.5 ? C5 C6 H6C . . 109.5 ? H6A C6 H6C . . 109.5 ? H6B C6 H6C . . 109.5 ? O3 C7 O4 . . 125.13(18) ? O3 C7 C3 . . 123.66(16) ? O4 C7 C3 . . 111.20(16) ? C9 C8 O4 . . 115.2(3) ? O4 C8 C9A . . 109.9(2) ? C9 C8 H8A . . 108.5 ? O4 C8 H8A . . 108.5 ? C9 C8 H8B . . 108.5 ? O4 C8 H8B . . 108.5 ? H8A C8 H8B . . 107.5 ? O4 C8 H8C . . 109.7 ? C9A C8 H8C . . 109.7 ? O4 C8 H8D . . 109.7 ? C9A C8 H8D . . 109.7 ? H8C C8 H8D . . 108.2 ? C8 C9 H9A . . 109.5 ? C8 C9 H9B . . 109.5 ? H9A C9 H9B . . 109.5 ? C8 C9 H9C . . 109.5 ? H9A C9 H9C . . 109.5 ? H9B C9 H9C . . 109.5 ? C8 C9A H9A1 . . 109.5 ? C8 C9A H9A2 . . 109.5 ? H9A1 C9A H9A2 . . 109.5 ? C8 C9A H9A3 . . 109.5 ? H9A1 C9A H9A3 . . 109.5 ? H9A2 C9A H9A3 . . 109.5 ? N1 C11 C16 . . 123.81(15) ? N1 C11 C12 . . 119.89(16) ? C16 C11 C12 . . 116.18(16) ? C13 C12 C11 . . 122.97(16) ? C13 C12 Br1 . . 118.53(12) ? C11 C12 Br1 . . 118.50(13) ? C14 C13 C12 . . 119.11(16) ? C14 C13 H13 . . 120.4 ? C12 C13 H13 . . 120.4 ? O5 C14 C13 . . 124.28(16) ? O5 C14 C15 . . 116.06(16) ? C13 C14 C15 . . 119.65(16) ? C16 C15 C14 . . 120.29(17) ? C16 C15 H15 . . 119.9 ? C14 C15 H15 . . 119.9 ? C15 C16 C11 . . 121.80(16) ? C15 C16 H16 . . 119.1 ? C11 C16 H16 . . 119.1 ? O5 C17 H17A . . 109.5 ? O5 C17 H17B . . 109.5 ? H17A C17 H17B . . 109.5 ? O5 C17 H17C . . 109.5 ? H17A C17 H17C . . 109.5 ? H17B C17 H17C . . 109.5 ? C22 C21 C26 . . 118.23(16) ? C22 C21 C1 . . 124.34(15) ? C26 C21 C1 . . 117.43(16) ? C21 C22 C23 . . 120.79(17) ? C21 C22 H22 . . 119.6 ? C23 C22 H22 . . 119.6 ? C24 C23 C22 . . 119.81(19) ? C24 C23 H23 . . 120.1 ? C22 C23 H23 . . 120.1 ? C25 C24 C23 . . 119.97(18) ? C25 C24 H24 . . 120.0 ? C23 C24 H24 . . 120.0 ? C24 C25 C26 . . 119.90(18) ? C24 C25 H25 . . 120.0 ? C26 C25 H25 . . 120.0 ? C25 C26 C21 . . 121.27(18) ? C25 C26 H26 . . 119.4 ? C21 C26 H26 . . 119.4 ? C32 C31 C36 . . 118.95(17) ? C32 C31 C1 . . 120.26(15) ? C36 C31 C1 . . 120.76(16) ? C33 C32 C31 . . 120.57(17) ? C33 C32 H32 . . 119.7 ? C31 C32 H32 . . 119.7 ? C34 C33 C32 . . 120.23(18) ? C34 C33 H33 . . 119.9 ? C32 C33 H33 . . 119.9 ? C33 C34 C35 . . 119.79(18) ? C33 C34 H34 . . 120.1 ? C35 C34 H34 . . 120.1 ? C36 C35 C34 . . 120.06(18) ? C36 C35 H35 . . 120.0 ? C34 C35 H35 . . 120.0 ? C35 C36 C31 . . 120.40(17) ? C35 C36 H36 . . 119.8 ? C31 C36 H36 . . 119.8 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C31 C1 C2 C3 . . . . 60.28(19) ? C21 C1 C2 C3 . . . . -174.31(14) ? C11 N1 C3 C2 . . . . 88.76(19) ? C11 N1 C3 C4 . . . . -36.2(2) ? C11 N1 C3 C7 . . . . -149.69(15) ? C1 C2 C3 N1 . . . . 39.8(2) ? C1 C2 C3 C4 . . . . 166.24(14) ? C1 C2 C3 C7 . . . . -78.15(18) ? C5 O2 C4 O1 . . . . -0.6(3) ? C5 O2 C4 C3 . . . . 179.57(15) ? N1 C3 C4 O1 . . . . 132.43(19) ? C2 C3 C4 O1 . . . . 5.1(2) ? C7 C3 C4 O1 . . . . -114.3(2) ? N1 C3 C4 O2 . . . . -47.71(19) ? C2 C3 C4 O2 . . . . -175.05(14) ? C7 C3 C4 O2 . . . . 65.55(17) ? C4 O2 C5 C6 . . . . 117.03(19) ? C8 O4 C7 O3 . . . . -4.3(3) ? C8 O4 C7 C3 . . . . 177.01(16) ? N1 C3 C7 O3 . . . . 1.8(2) ? C2 C3 C7 O3 . . . . 125.09(18) ? C4 C3 C7 O3 . . . . -116.66(18) ? N1 C3 C7 O4 . . . . -179.50(14) ? C2 C3 C7 O4 . . . . -56.21(18) ? C4 C3 C7 O4 . . . . 62.04(18) ? C7 O4 C8 C9 . . . . 84.1(3) ? C7 O4 C8 C9A . . . . 135.7(3) ? C3 N1 C11 C16 . . . . -32.2(3) ? C3 N1 C11 C12 . . . . 152.10(16) ? N1 C11 C12 C13 . . . . 175.25(16) ? C16 C11 C12 C13 . . . . -0.8(2) ? N1 C11 C12 Br1 . . . . -4.0(2) ? C16 C11 C12 Br1 . . . . 179.92(12) ? C11 C12 C13 C14 . . . . 0.8(3) ? Br1 C12 C13 C14 . . . . -179.92(13) ? C17 O5 C14 C13 . . . . 10.4(3) ? C17 O5 C14 C15 . . . . -170.75(16) ? C12 C13 C14 O5 . . . . 178.57(16) ? C12 C13 C14 C15 . . . . -0.3(3) ? O5 C14 C15 C16 . . . . -179.15(16) ? C13 C14 C15 C16 . . . . -0.2(3) ? C14 C15 C16 C11 . . . . 0.2(3) ? N1 C11 C16 C15 . . . . -175.59(16) ? C12 C11 C16 C15 . . . . 0.3(2) ? C31 C1 C21 C22 . . . . 109.20(18) ? C2 C1 C21 C22 . . . . -18.3(2) ? C31 C1 C21 C26 . . . . -70.43(19) ? C2 C1 C21 C26 . . . . 162.03(15) ? C26 C21 C22 C23 . . . . -1.4(3) ? C1 C21 C22 C23 . . . . 178.95(17) ? C21 C22 C23 C24 . . . . 0.1(3) ? C22 C23 C24 C25 . . . . 1.4(3) ? C23 C24 C25 C26 . . . . -1.6(3) ? C24 C25 C26 C21 . . . . 0.2(3) ? C22 C21 C26 C25 . . . . 1.3(3) ? C1 C21 C26 C25 . . . . -179.05(16) ? C21 C1 C31 C32 . . . . 114.74(17) ? C2 C1 C31 C32 . . . . -117.58(17) ? C21 C1 C31 C36 . . . . -63.3(2) ? C2 C1 C31 C36 . . . . 64.4(2) ? C36 C31 C32 C33 . . . . -0.3(3) ? C1 C31 C32 C33 . . . . -178.35(16) ? C31 C32 C33 C34 . . . . 0.2(3) ? C32 C33 C34 C35 . . . . -0.1(3) ? C33 C34 C35 C36 . . . . 0.0(3) ? C34 C35 C36 C31 . . . . -0.1(3) ? C32 C31 C36 C35 . . . . 0.2(3) ? C1 C31 C36 C35 . . . . 178.28(16) ? _shelx_res_file ; stu8307.res created by SHELXL-2014/7 TITL stu8307.res in P2(1)/n CELL 0.71073 8.3030 17.7016 17.5144 90.000 99.293 90.000 ZERR 4.000 0.0003 0.0006 0.0005 0.000 0.001 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H N O Br UNIT 112 120 4 20 4 SIZE 0.074 0.125 0.229 TEMP -173.200 ACTA CONF L.S. 20 BOND $H FMAP 2 PLAN 10 OMIT 0 9 9 OMIT 0 14 0 OMIT -1 6 6 OMIT -3 6 6 WGHT 0.025300 2.084300 FVAR 0.46904 0.52607 BR1 5 0.350191 0.627284 0.821401 11.00000 0.01916 0.02482 = 0.02144 0.00275 0.00959 -0.00296 N1 3 0.412017 0.694829 0.668863 11.00000 0.01418 0.01604 = 0.01399 0.00114 0.00280 -0.00202 H1 2 0.335285 0.691909 0.689774 11.00000 0.01449 O1 4 0.576240 0.860585 0.603225 11.00000 0.04476 0.02184 = 0.01753 0.00097 0.00111 -0.01816 O2 4 0.472618 0.842919 0.713067 11.00000 0.02366 0.02107 = 0.02507 -0.01164 0.00703 -0.00792 O3 4 0.118243 0.753169 0.647992 11.00000 0.01852 0.02699 = 0.02731 -0.00704 0.00585 0.00011 O4 4 0.171281 0.836585 0.558132 11.00000 0.01847 0.01524 = 0.04683 0.00306 -0.00729 0.00220 O5 4 0.993869 0.611014 0.856797 11.00000 0.01818 0.03544 = 0.02255 0.01322 0.00078 0.00393 C1 1 0.362561 0.653162 0.507256 11.00000 0.01324 0.01138 = 0.01623 0.00124 -0.00110 -0.00136 AFIX 13 H1A 2 0.414483 0.617589 0.548343 11.00000 -1.20000 AFIX 0 C2 1 0.425535 0.732469 0.531591 11.00000 0.01612 0.01189 = 0.01414 0.00099 -0.00012 -0.00211 AFIX 23 H2A 2 0.373781 0.769540 0.492915 11.00000 -1.20000 H2B 2 0.544792 0.734222 0.531835 11.00000 -1.20000 AFIX 0 C3 1 0.390000 0.755613 0.612693 11.00000 0.01492 0.01063 = 0.01670 -0.00044 -0.00061 -0.00088 C4 1 0.492619 0.826509 0.641229 11.00000 0.01684 0.01226 = 0.01735 0.00029 -0.00403 0.00123 C5 1 0.561045 0.908098 0.750531 11.00000 0.02394 0.02156 = 0.02298 -0.00925 -0.00039 -0.00724 AFIX 23 H5A 2 0.631940 0.930214 0.716017 11.00000 -1.20000 H5B 2 0.630706 0.892197 0.799162 11.00000 -1.20000 AFIX 0 C6 1 0.439652 0.964927 0.767356 11.00000 0.03857 0.02043 = 0.05171 -0.01229 0.00865 -0.00215 AFIX 137 H6A 2 0.370702 0.980032 0.718983 11.00000 -1.50000 H6B 2 0.496789 1.009311 0.791829 11.00000 -1.50000 H6C 2 0.371452 0.942894 0.802347 11.00000 -1.50000 AFIX 0 C7 1 0.209332 0.780467 0.608904 11.00000 0.01805 0.01347 = 0.02284 -0.00664 -0.00299 0.00026 SIMU 0.02 0.04 0.9 C8 C9 C9A SAME C8 C9A SADI C8 C9 C8 1 0.000838 0.861772 0.547128 11.00000 0.01941 0.02077 = 0.08760 0.00669 -0.01103 0.00576 PART 1 21 AFIX 23 H8A 2 -0.026711 0.884107 0.494825 21.00000 -1.20000 H8B 2 -0.069850 0.816991 0.548992 21.00000 -1.20000 AFIX 23 PART 2 -21 H8C 2 -0.052896 0.842129 0.589586 -21.00000 -1.20000 H8D 2 -0.058199 0.841713 0.497651 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 21 C9 1 -0.034639 0.912659 0.599289 21.00000 0.03256 0.02610 = 0.02460 -0.00360 0.00254 0.00854 AFIX 137 H9A 2 -0.031258 0.887959 0.649599 21.00000 -1.50000 H9B 2 -0.144009 0.933285 0.582080 21.00000 -1.50000 H9C 2 0.045576 0.953701 0.604082 21.00000 -1.50000 AFIX 0 PART 2 -21 C9A 1 -0.006021 0.944696 0.546305 -21.00000 0.03173 0.02052 = 0.03170 0.00201 0.00138 0.01030 AFIX 137 H9A1 2 0.062998 0.964531 0.592653 -21.00000 -1.50000 H9A2 2 -0.118908 0.961191 0.545639 -21.00000 -1.50000 H9A3 2 0.033271 0.963687 0.500074 -21.00000 -1.50000 AFIX 0 PART 0 C11 1 0.558198 0.677503 0.716574 11.00000 0.01690 0.00970 = 0.01272 -0.00264 0.00217 -0.00126 C12 1 0.555961 0.643148 0.788521 11.00000 0.01717 0.01233 = 0.01496 -0.00229 0.00765 -0.00271 C13 1 0.696308 0.619427 0.836523 11.00000 0.02183 0.01423 = 0.01401 0.00227 0.00475 0.00040 AFIX 43 H13 2 0.689595 0.595783 0.884601 11.00000 -1.20000 AFIX 0 C14 1 0.846494 0.630691 0.813385 11.00000 0.01813 0.01533 = 0.01618 0.00302 0.00093 0.00143 C15 1 0.853945 0.665171 0.742584 11.00000 0.01626 0.02051 = 0.01955 0.00326 0.00571 -0.00079 AFIX 43 H15 2 0.956697 0.673136 0.726650 11.00000 -1.20000 AFIX 0 C16 1 0.712256 0.687899 0.695303 11.00000 0.01814 0.01436 = 0.01440 0.00337 0.00450 -0.00048 AFIX 43 H16 2 0.719706 0.711178 0.647125 11.00000 -1.20000 AFIX 0 C17 1 0.989657 0.565556 0.923810 11.00000 0.03016 0.02601 = 0.01725 0.00773 -0.00028 0.00540 AFIX 137 H17A 2 0.937216 0.593840 0.961169 11.00000 -1.50000 H17B 2 1.101283 0.552320 0.947342 11.00000 -1.50000 H17C 2 0.927583 0.519313 0.908905 11.00000 -1.50000 AFIX 0 C21 1 0.411040 0.626481 0.431398 11.00000 0.01063 0.01343 = 0.01765 -0.00147 -0.00192 0.00227 C22 1 0.462881 0.673929 0.377139 11.00000 0.01954 0.01452 = 0.02337 -0.00292 0.00425 -0.00108 AFIX 43 H22 2 0.467920 0.726868 0.386110 11.00000 -1.20000 AFIX 0 C23 1 0.507720 0.644796 0.309522 11.00000 0.02686 0.02831 = 0.02665 -0.00449 0.01167 -0.00359 AFIX 43 H23 2 0.543171 0.677784 0.272798 11.00000 -1.20000 AFIX 0 C24 1 0.500328 0.567297 0.296081 11.00000 0.02489 0.03301 = 0.03136 -0.01565 0.00884 0.00370 AFIX 43 H24 2 0.533118 0.547186 0.250699 11.00000 -1.20000 AFIX 0 C25 1 0.445375 0.519692 0.348673 11.00000 0.02442 0.01645 = 0.03573 -0.00941 -0.00183 0.00632 AFIX 43 H25 2 0.437697 0.466914 0.338933 11.00000 -1.20000 AFIX 0 C26 1 0.401421 0.548941 0.415677 11.00000 0.01780 0.01410 = 0.02564 -0.00009 -0.00448 0.00103 AFIX 43 H26 2 0.364015 0.515745 0.451674 11.00000 -1.20000 AFIX 0 C31 1 0.178749 0.644935 0.502856 11.00000 0.01576 0.01143 = 0.01457 -0.00394 0.00037 -0.00110 C32 1 0.115577 0.594238 0.551060 11.00000 0.02043 0.01781 = 0.01828 0.00017 0.00243 -0.00237 AFIX 43 H32 2 0.187651 0.565675 0.587750 11.00000 -1.20000 AFIX 0 C33 1 -0.052125 0.585023 0.545994 11.00000 0.02223 0.02587 = 0.02962 -0.00035 0.00845 -0.00653 AFIX 43 H33 2 -0.093968 0.550380 0.579300 11.00000 -1.20000 AFIX 0 C34 1 -0.158196 0.626109 0.492644 11.00000 0.01384 0.02673 = 0.03925 -0.00810 0.00430 -0.00268 AFIX 43 H34 2 -0.272732 0.619687 0.489222 11.00000 -1.20000 AFIX 0 C35 1 -0.096673 0.676874 0.444003 11.00000 0.01870 0.02038 = 0.03103 -0.00352 -0.00508 0.00185 AFIX 43 H35 2 -0.169273 0.705189 0.407310 11.00000 -1.20000 AFIX 0 C36 1 0.071040 0.686219 0.449034 11.00000 0.01917 0.01424 = 0.02187 -0.00101 -0.00053 -0.00080 AFIX 43 H36 2 0.112567 0.720895 0.415657 11.00000 -1.20000 AFIX 0 HKLF 4 REM stu8307.res in P2(1)/n REM R1 = 0.0310 for 4905 Fo > 4sig(Fo) and 0.0431 for all 5840 data REM 334 parameters refined using 1 restraints END WGHT 0.0253 2.0851 REM Highest difference peak 0.428, deepest hole -0.568, 1-sigma level 0.062 Q1 1 -0.0621 0.8221 0.5223 11.00000 0.05 0.43 Q2 1 0.3059 0.7759 0.6124 11.00000 0.05 0.34 Q3 1 -0.0061 0.8661 0.5835 11.00000 0.05 0.33 Q4 1 0.2629 0.6480 0.5032 11.00000 0.05 0.30 Q5 1 0.4229 0.7428 0.5766 11.00000 0.05 0.30 Q6 1 0.5595 0.6625 0.7522 11.00000 0.05 0.27 Q7 1 0.0303 0.5834 0.5383 11.00000 0.05 0.27 Q8 1 0.4316 0.7879 0.6264 11.00000 0.05 0.25 Q9 1 -0.0488 0.8503 0.6263 11.00000 0.05 0.25 Q10 1 0.0498 0.8551 0.5397 11.00000 0.05 0.24 ; _shelx_res_checksum 97620 _shelx_hkl_file ; 1 0 0 -14.50 1.20 1 0 0 -14.80 1.10 1 0 0 -15.30 1.40 -1 0 0 -14.30 1.60 -1 0 0 -13.40 1.20 -1 0 0 -16.40 1.30 -2 0 0 9999.00 216.28 -3 0 0 -0.80 4.50 3 0 0 3.00 3.50 -3 0 0 -6.70 3.70 -3 0 0 -5.20 3.40 3 0 0 -2.30 3.40 3 0 0 -3.50 3.80 4 0 0 1803.72 49.00 4 0 0 1795.42 48.10 -4 0 0 1889.31 48.40 -4 0 0 1927.01 49.00 -4 0 0 1691.43 45.90 4 0 0 1822.02 46.20 5 0 0 11.20 6.50 5 0 0 14.90 6.50 -5 0 0 16.90 7.00 -5 0 0 15.40 6.90 5 0 0 6.00 6.50 -5 0 0 12.00 7.40 -6 0 0 1146.99 36.80 6 0 0 1176.78 36.40 -6 0 0 1106.09 38.60 6 0 0 1198.28 39.80 6 0 0 1101.49 40.10 -6 0 0 1120.39 39.30 7 0 0 19.20 13.80 -7 0 0 26.70 12.10 -7 0 0 10.80 12.80 7 0 0 24.50 12.50 7 0 0 4.70 9.10 -7 0 0 19.10 13.20 8 0 0 36.40 15.50 -8 0 0 25.80 14.00 -8 0 0 49.90 16.10 -8 0 0 31.00 14.80 8 0 0 18.30 14.90 9 0 0 1.20 17.70 9 0 0 -9.70 15.20 9 0 0 6.90 14.10 -9 0 0 -6.60 14.40 -9 0 0 6.10 17.00 -9 0 0 -8.50 15.00 10 0 0 89.39 23.50 -10 0 0 107.29 25.30 -10 0 0 158.58 25.70 -10 0 0 113.39 23.00 10 0 0 104.79 26.00 -1 -1 0 331.47 9.00 1 -1 0 283.97 8.90 1 -1 0 299.47 9.20 -1 -1 0 292.77 9.00 -1 -1 0 297.07 8.40 -1 1 0 294.87 8.40 -1 1 0 305.07 9.00 -1 1 0 281.37 9.00 1 1 0 313.77 8.50 1 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43.90 -4 -3 2 1669.33 43.90 4 -3 -2 1514.15 44.10 4 -3 -2 1591.84 41.80 -4 -3 2 1592.54 42.10 4 3 -2 1600.94 43.90 4 3 -2 1540.85 44.00 4 3 -2 1642.04 42.40 -4 3 2 1625.94 43.70 -4 3 2 1505.65 43.90 -4 3 2 1520.35 41.20 -3 -3 2 190.58 11.30 3 -3 -2 169.28 10.30 3 -3 -2 173.98 9.30 -3 -3 2 177.98 9.80 3 -3 -2 159.78 10.50 3 3 -2 181.48 10.70 -3 3 2 186.88 11.10 -3 3 2 173.88 9.30 3 3 -2 180.98 10.00 3 3 -2 174.08 10.90 -3 3 2 170.58 10.50 -2 -3 2 199.08 9.70 2 -3 -2 196.68 9.00 2 -3 -2 188.38 9.30 2 -3 -2 207.88 8.30 -2 -3 2 214.88 9.90 -2 -3 2 190.78 8.90 2 3 -2 197.68 8.90 -2 3 2 198.28 8.00 2 3 -2 189.78 9.50 -2 3 2 191.18 9.40 2 3 -2 190.28 9.50 -2 3 2 194.48 8.90 -1 -3 2 1.30 2.80 -1 -3 2 0.40 3.00 1 -3 -2 0.00 1.80 -1 -3 2 3.20 2.80 1 -3 -2 0.90 2.20 1 -3 -2 1.30 2.40 1 3 -2 1.90 2.90 -1 3 2 1.00 1.70 -1 3 2 3.50 2.10 -1 3 2 -0.10 2.10 1 3 -2 2.80 2.60 1 3 -2 0.30 2.50 0 -3 -2 7437.16 159.18 0 -3 2 7323.27 161.18 0 3 2 7494.15 159.28 0 3 2 7488.05 159.18 0 3 -2 7468.85 161.38 0 3 -2 7497.55 161.58 -1 -3 -2 1900.41 44.60 -1 -3 -2 1970.00 44.30 1 -3 2 1917.31 46.90 -1 -3 -2 1900.61 44.60 1 -3 2 2081.59 45.70 1 -3 2 1903.91 46.50 -1 3 -2 1952.10 45.40 -1 3 -2 2070.59 47.30 1 3 2 1937.91 43.90 1 3 2 1945.21 44.80 -1 3 -2 2098.69 47.00 2 -3 2 539.65 16.20 2 -3 2 512.25 17.40 -2 -3 -2 494.55 16.00 2 -3 2 522.95 18.00 -2 -3 -2 507.15 16.00 -2 -3 -2 506.65 15.30 2 3 2 530.75 16.60 -2 3 -2 492.45 17.80 -2 3 -2 554.74 16.40 2 3 2 506.35 15.00 -2 3 -2 556.64 17.80 -3 -3 -2 977.90 28.40 -3 -3 -2 1017.20 28.50 3 -3 2 985.50 28.00 -3 -3 -2 959.50 27.30 3 -3 2 1004.40 30.10 3 -3 2 1007.10 30.50 3 3 2 991.60 27.00 -3 3 -2 975.30 30.20 -3 3 -2 1111.19 30.50 3 3 2 1025.30 29.20 -3 3 -2 1011.30 28.20 3 3 2 967.90 28.80 4 -3 2 10.80 7.30 -4 -3 -2 3.70 6.00 -4 -3 -2 0.10 5.40 4 -3 2 8.20 5.40 -4 -3 -2 14.20 6.50 4 -3 2 7.40 6.80 4 3 2 14.80 5.60 -4 3 -2 7.90 6.00 -4 3 -2 0.20 6.00 4 3 2 6.60 6.00 4 3 2 9.70 5.80 -4 3 -2 12.10 6.80 -5 -3 -2 761.02 29.00 5 -3 2 823.82 30.40 -5 -3 -2 794.62 27.70 -5 -3 -2 785.42 28.80 5 -3 2 774.32 31.30 5 -3 2 846.82 27.70 -5 3 -2 798.62 30.80 -5 3 -2 781.32 29.50 -5 3 -2 804.42 27.80 5 3 2 795.62 30.30 5 3 2 796.92 30.20 5 3 2 785.52 29.10 6 -3 2 705.93 31.60 -6 -3 -2 721.13 28.60 6 -3 2 753.02 33.80 -6 -3 -2 666.13 29.80 -6 -3 -2 773.82 31.60 -6 3 -2 773.42 32.70 -6 3 -2 754.12 29.10 6 3 2 791.42 33.40 -6 3 -2 754.82 31.40 6 3 2 703.93 30.60 6 3 2 743.03 27.70 -7 -3 -2 46.70 11.90 -7 -3 -2 43.40 13.80 7 -3 2 87.19 16.00 -7 -3 -2 54.29 14.10 7 -3 2 80.89 18.20 7 -3 2 59.59 12.80 7 3 2 58.39 14.90 -7 3 -2 57.49 13.60 7 3 2 55.59 14.40 -7 3 -2 55.39 14.20 7 3 2 49.70 12.40 -7 3 -2 53.49 14.50 -8 -3 -2 2.60 15.70 8 -3 2 4.30 14.90 8 -3 2 -9.80 11.20 -8 -3 -2 -3.00 13.40 -8 -3 -2 3.80 12.90 8 -3 2 -4.00 13.50 -8 3 -2 18.50 15.30 -8 3 -2 -20.00 14.60 -8 3 -2 35.10 14.60 8 3 2 19.10 14.00 9 -3 2 30.70 20.40 9 -3 2 28.40 18.30 9 -3 2 58.19 17.10 -9 -3 -2 26.40 17.80 -9 -3 -2 -13.60 16.70 -9 -3 -2 -27.80 19.30 9 3 2 37.00 19.50 -9 3 -2 12.60 18.30 9 3 2 27.70 15.40 9 3 2 84.59 27.50 -9 3 -2 22.10 17.20 -9 3 -2 -11.70 19.90 10 -3 2 5.90 24.80 -10 -3 -2 -7.90 24.70 10 -3 2 -25.00 24.10 -10 -3 -2 -21.10 22.50 -10 -3 -2 -28.30 20.70 -10 3 -2 29.80 21.30 10 3 2 -8.20 22.10 10 3 2 -7.40 19.30 -10 3 -2 -25.20 24.60 10 3 2 -20.30 20.90 -10 3 -2 -29.50 21.40 -10 -4 2 49.40 21.40 10 -4 -2 69.39 23.00 -10 -4 2 35.80 22.30 10 -4 -2 97.69 23.80 -10 -4 2 95.59 28.50 10 4 -2 53.79 24.80 10 4 -2 58.59 23.50 -10 4 2 54.99 20.10 -9 -4 2 -0.10 16.40 -9 -4 2 0.70 16.10 9 -4 -2 8.00 16.80 9 -4 -2 -13.80 19.30 -9 -4 2 29.60 15.30 9 -4 -2 6.60 14.10 9 4 -2 8.40 19.40 -9 4 2 16.90 17.00 9 4 -2 21.20 15.30 9 4 -2 20.30 19.50 -9 4 2 43.70 16.60 -9 4 2 3.60 17.30 -8 -4 2 195.98 22.40 8 -4 -2 146.09 22.40 8 -4 -2 148.89 21.20 -8 -4 2 176.18 20.20 -8 -4 2 180.88 21.40 -8 4 2 133.49 18.90 -8 4 2 150.18 20.40 8 4 -2 153.98 23.10 8 4 -2 222.18 24.70 -8 4 2 166.78 19.50 7 -4 -2 7.50 11.70 7 -4 -2 16.90 9.80 7 -4 -2 3.80 20.40 -7 -4 2 20.00 11.20 -7 -4 2 31.40 11.90 -7 -4 2 41.90 20.40 -7 4 2 18.50 13.10 7 4 -2 12.30 12.00 7 4 -2 44.50 11.70 -7 4 2 31.70 13.00 7 4 -2 25.90 13.10 -7 4 2 18.30 18.50 6 -4 -2 1545.15 49.99 6 -4 -2 1596.04 48.20 -6 -4 2 1695.33 49.10 -6 -4 2 1539.45 48.20 -6 -4 2 1556.44 46.60 6 -4 -2 1697.43 50.49 6 4 -2 1547.15 49.70 6 4 -2 1586.74 46.10 -6 4 2 1499.15 45.40 -6 4 2 1547.15 49.60 -6 4 2 1558.74 48.70 6 4 -2 1605.74 49.20 5 -4 -2 -1.90 7.30 -5 -4 2 -3.30 9.40 5 -4 -2 5.50 7.90 5 -4 -2 -1.10 5.70 -5 -4 2 -1.40 6.40 -5 -4 2 -3.80 6.60 -5 4 2 3.70 8.20 5 4 -2 -1.10 5.90 5 4 -2 -0.20 7.30 -5 4 2 -5.40 6.80 -5 4 2 11.00 7.10 5 4 -2 5.50 6.60 -4 -4 2 37.20 7.10 4 -4 -2 60.49 8.10 -4 -4 2 59.89 8.30 4 -4 -2 46.10 7.80 4 -4 -2 48.70 8.00 -4 -4 2 50.89 8.50 4 4 -2 40.90 9.60 4 4 -2 51.09 7.80 4 4 -2 57.39 8.50 -4 4 2 46.60 7.80 -4 4 2 46.20 7.90 -4 4 2 40.60 7.80 3 -4 -2 538.85 17.90 -3 -4 2 576.24 19.80 3 -4 -2 556.94 20.10 3 -4 -2 527.85 19.10 -3 -4 2 536.15 18.50 -3 -4 2 564.14 19.80 -3 4 2 542.75 19.20 3 4 -2 572.84 20.00 -3 4 2 556.44 19.90 3 4 -2 604.14 20.20 -3 4 2 545.35 17.60 3 4 -2 538.05 18.50 -2 -4 2 1582.94 38.90 2 -4 -2 1532.25 38.60 2 -4 -2 1512.15 38.20 -2 -4 2 1514.35 38.00 2 -4 -2 1556.44 37.00 -2 -4 2 1546.35 38.80 -2 4 2 1578.74 38.80 2 4 -2 1383.56 38.30 2 4 -2 1511.45 38.80 -2 4 2 1542.05 36.40 2 4 -2 1581.64 38.30 -2 4 2 1546.55 38.30 -1 -4 2 125.29 8.00 1 -4 -2 115.09 5.60 1 -4 -2 118.79 6.40 -1 -4 2 124.59 7.90 1 -4 -2 129.59 6.90 -1 -4 2 131.99 7.50 -1 4 2 136.49 7.10 1 4 -2 133.59 7.80 -1 4 2 120.59 6.40 1 4 -2 134.89 7.50 -1 4 2 123.59 5.20 1 4 -2 132.19 7.80 1 4 -2 121.59 7.80 0 -4 2 666.23 18.50 0 -4 2 687.83 17.70 0 -4 2 640.04 18.50 0 -4 -2 645.04 16.60 0 -4 -2 600.74 16.80 0 -4 2 604.04 18.40 0 4 -2 687.43 18.70 0 4 -2 667.73 17.50 0 4 -2 648.94 18.50 0 4 2 664.73 16.80 0 4 2 636.84 16.60 0 4 2 653.93 17.00 0 4 -2 618.04 18.60 0 4 -2 693.73 18.70 0 4 -2 678.93 19.20 -1 -4 -2 62.99 5.40 1 -4 2 64.99 5.70 -1 -4 -2 63.19 5.30 -1 -4 -2 68.09 4.80 1 -4 2 55.19 6.80 1 -4 2 66.69 6.60 1 4 2 63.99 4.60 1 4 2 68.99 5.70 -1 4 -2 54.69 5.50 -1 4 -2 62.69 6.50 -1 4 -2 74.69 6.80 -1 4 -2 64.49 7.20 -2 -4 -2 2006.20 48.80 2 -4 2 2160.08 49.50 2 -4 2 2210.08 51.99 -2 -4 -2 2110.29 49.00 -2 -4 -2 2018.40 48.20 2 -4 2 2182.68 51.29 2 4 2 2071.19 47.80 -2 4 -2 1945.71 48.90 -2 4 -2 1935.71 50.99 -2 4 -2 1913.71 50.59 2 4 2 2058.99 49.20 3 -4 2 1944.21 51.59 3 -4 2 1884.61 48.70 -3 -4 -2 1987.20 48.30 -3 -4 -2 1933.21 49.20 3 -4 2 1967.00 50.99 -3 -4 -2 1889.51 49.00 -3 4 -2 1968.30 51.59 -3 4 -2 2146.09 51.69 3 4 2 1941.11 47.60 3 4 2 1918.01 49.30 -3 4 -2 2022.30 49.10 3 4 2 1959.80 49.80 -4 -4 -2 450.65 19.20 4 -4 2 440.16 20.20 4 -4 2 435.76 18.00 4 -4 2 428.36 21.20 -4 -4 -2 430.86 17.90 -4 -4 -2 427.46 18.80 -4 4 -2 433.96 19.90 4 4 2 457.85 17.40 4 4 2 421.46 19.30 4 4 2 459.15 19.20 -4 4 -2 467.05 21.40 -4 4 -2 431.66 18.00 -5 -4 -2 753.42 28.60 -5 -4 -2 801.42 27.80 -5 -4 -2 814.12 29.50 5 -4 2 792.92 27.30 5 -4 2 769.32 30.30 5 -4 2 788.42 31.30 5 4 2 760.02 29.70 -5 4 -2 746.73 27.50 5 4 2 741.03 26.00 5 4 2 732.63 28.30 -5 4 -2 823.12 30.20 -5 4 -2 783.02 30.80 -6 -4 -2 109.69 14.30 -6 -4 -2 107.69 14.70 6 -4 2 119.79 15.30 -6 -4 -2 95.49 14.20 6 -4 2 93.59 14.60 6 -4 2 115.39 15.70 6 4 2 98.79 11.90 -6 4 -2 99.99 13.20 6 4 2 131.99 16.40 6 4 2 124.09 15.60 -6 4 -2 127.89 15.80 -6 4 -2 133.99 17.40 -7 -4 -2 559.04 31.20 7 -4 2 506.35 32.60 7 -4 2 512.95 31.00 7 -4 2 555.84 26.80 -7 -4 -2 543.65 29.50 -7 -4 -2 558.54 28.50 7 4 2 511.75 32.00 7 4 2 585.84 30.80 7 4 2 558.04 26.90 -7 4 -2 532.95 28.00 -7 4 -2 570.64 30.80 -7 4 -2 473.25 32.10 8 -4 2 296.57 24.20 8 -4 2 277.67 29.10 -8 -4 -2 234.88 25.00 -8 -4 -2 308.07 27.90 -8 -4 -2 317.47 30.70 8 -4 2 276.67 32.10 8 4 2 253.67 28.00 -8 4 -2 283.57 26.50 -8 4 -2 261.87 33.50 8 4 2 303.77 49.50 -8 4 -2 286.77 31.60 -9 -4 -2 -14.40 18.70 -9 -4 -2 31.50 21.60 -9 -4 -2 6.50 16.00 9 -4 2 70.89 18.30 9 -4 2 7.40 20.00 9 -4 2 12.60 29.10 -9 4 -2 37.40 16.80 9 4 2 49.50 22.60 9 4 2 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3 -22 13.50 11.60 1 3 -22 37.40 13.10 0 -3 -22 54.89 9.30 0 3 -22 44.20 12.80 0 3 -22 70.09 15.00 0 3 -22 49.60 15.70 0 3 -22 52.59 13.00 3 4 -22 -18.70 17.60 3 4 -22 3.90 13.10 3 4 -22 -13.20 13.60 2 4 -22 135.79 17.60 2 4 -22 130.69 21.50 2 4 -22 127.79 16.70 2 4 -22 160.08 22.00 1 4 -22 -12.30 19.20 1 4 -22 6.60 13.30 1 4 -22 -8.10 14.70 1 4 -22 11.80 22.80 0 -4 -22 280.57 19.80 0 4 -22 298.07 24.90 0 4 -22 237.58 30.60 3 5 -22 41.90 18.20 3 5 -22 52.89 21.00 2 5 -22 45.90 18.70 2 5 -22 4.70 23.00 2 5 -22 44.60 15.70 1 5 -22 10.20 13.50 1 5 -22 53.19 19.40 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 98597 #============================================================================= # end of cif data for "stu8307" (compound 4o) #============================================================================= #============================================================================= # end of cif file 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