#============================================================================== # 1. SUBMISSION DETAILS data_global _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 '.' #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; trans-Selective Arene Hydrogenation of Phenol Derivatives. ; loop_ _publ_author_name _publ_author_address 'Wollenburg, Marco' ; Organisch-Chemisches Institut Westf\"alische Wilhelms-Universit\"at M\"unster Corrensstrasse 40 48149 M\"unster Germany ; 'Heusler, Arne' ; Organisch-Chemisches Institut Westf\"alische Wilhelms-Universit\"at M\"unster Corrensstrasse 40 48149 M\"unster Germany ; 'Bergander, Klaus' ; Organisch-Chemisches Institut Westf\"alische Wilhelms-Universit\"at M\"unster Corrensstrasse 40 48149 M\"unster Germany ; 'Glorius, Frank' ; Organisch-Chemisches Institut Westf\"alische Wilhelms-Universit\"at M\"unster Corrensstrasse 40 48149 M\"unster Germany ; #============================================================================= # cif data for "glo9616" (compound 2f) #============================================================================= data_glo9616 _audit_creation_method 'APEX3 v2016.1-0' _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H21 N O3' _chemical_formula_iupac ? _chemical_formula_weight 215.29 _chemical_absolute_configuration . _chemical_melting_point ? _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'P c a 21' _space_group_name_Hall 'P 2c -2ac' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 9.8601(3) _cell_length_b 5.6544(2) _cell_length_c 44.1243(15) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2460.06(14) _cell_formula_units_Z 8 _cell_measurement_reflns_used 9942 _cell_measurement_theta_min 4.0075 _cell_measurement_theta_max 69.1964 _cell_measurement_temperature 100.(2) _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.069 _exptl_crystal_size_min 0.052 _exptl_crystal_density_diffrn 1.163 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.679 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Bruker AXS (2014). SADABS, Version 2014/5, Bruker AXS Inc., Madison, Wisconsin, USA. ; _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.97 _exptl_special_details ; ; _diffrn_ambient_temperature 100.(2) _diffrn_source 'Cu ImS' _diffrn_source_type 'micro focus tube' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _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 7.3910 _diffrn_reflns_number 33803 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_unetI/netI 0.0469 _diffrn_reflns_theta_min 4.01 _diffrn_reflns_theta_max 69.27 _diffrn_reflns_theta_full 69.27 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 53 _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. The hydrogens at O1A, O1B, N1A and N1B atoms were refined freely, but with distance restraints (SADI, DFIX, U-fixed value). ; _reflns_number_total 4551 _reflns_number_gt 4145 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_gt 0.1283 _refine_ls_wR_factor_ref 0.1308 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_number_reflns 4551 _refine_ls_number_parameters 290 _refine_ls_number_restraints 5 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+3.5147P] 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 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.226 _refine_diff_density_min -0.215 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; Flack x determined using 1777 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.06(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ; APEX3 v2016.1-0 (Bruker AXS Inc., 2016) ; _computing_cell_refinement 'SAINT V8.37A (Bruker AXS Inc., 2015)' _computing_data_reduction 'SAINT V8.37A (Bruker AXS Inc., 2015)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'XP (Sheldrick, 2014)' _computing_publication_material 'SHELXL-2014/7 (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 N N1A 0.5053(4) 0.5144(8) 0.37268(13) 0.0272(12) Uani d . . D 1 . . H H01A 0.418(3) 0.531(11) 0.3682(18) 0.041 Uiso d U . D 1 . . C C1A 0.5335(5) 0.5848(10) 0.40395(12) 0.0279(11) Uani d . . . 1 . . H H1A 0.6078 0.4815 0.4119 0.034 Uiso calc U . R 1 . . C C2A 0.4102(6) 0.5501(12) 0.42389(13) 0.0339(12) Uani d . . . 1 . . H H201 0.3841 0.381 0.4237 0.041 Uiso calc U . R 1 . . H H202 0.3335 0.6423 0.4155 0.041 Uiso calc U . R 1 . . C C3A 0.4362(5) 0.6274(11) 0.45649(12) 0.0362(13) Uani d . . . 1 . . H H301 0.3522 0.6081 0.4685 0.043 Uiso calc U . R 1 . . H H302 0.5072 0.5259 0.4656 0.043 Uiso calc U . R 1 . . C C4A 0.4813(5) 0.8839(10) 0.45750(11) 0.0309(12) Uani d . . . 1 . . H H4A 0.4068 0.9857 0.4494 0.037 Uiso calc U . R 1 . . O O1A 0.5116(4) 0.9566(9) 0.48784(11) 0.0446(12) Uani d . . D 1 . . H H02A 0.427(4) 0.968(11) 0.4949(14) 0.045(19) Uiso d . . D 1 . . C C5A 0.6059(5) 0.9191(11) 0.43847(13) 0.0335(12) Uani d . . . 1 . . H H501 0.6816 0.826 0.4471 0.04 Uiso calc U . R 1 . . H H502 0.6322 1.0881 0.4389 0.04 Uiso calc U . R 1 . . C C6A 0.5824(5) 0.8429(11) 0.40547(13) 0.0321(12) Uani d . . . 1 . . H H601 0.6679 0.8593 0.3939 0.039 Uiso calc U . R 1 . . H H602 0.5137 0.9474 0.3961 0.039 Uiso calc U . R 1 . . C C7A 0.5925(5) 0.4165(10) 0.35458(12) 0.0289(11) Uani d . . . 1 . . O O2A 0.7116(4) 0.3763(8) 0.36130(8) 0.0345(9) Uani d . . . 1 . . O O3A 0.5381(3) 0.3749(7) 0.32710(8) 0.0284(8) Uani d . . . 1 . . C C8A 0.6066(5) 0.2217(10) 0.30498(12) 0.0272(11) Uani d . . . 1 . . C C9A 0.7360(5) 0.3396(11) 0.29347(13) 0.0338(12) Uani d . . . 1 . . H H901 0.7139 0.4952 0.285 0.051 Uiso calc U . R 1 . . H H902 0.7771 0.2409 0.2777 0.051 Uiso calc U . R 1 . . H H903 0.7999 0.3584 0.3103 0.051 Uiso calc U . R 1 . . C C10A 0.6356(7) -0.0205(11) 0.3189(2) 0.0408(17) Uani d . . . 1 . . H H10A 0.713 -0.0084 0.3327 0.061 Uiso calc U . R 1 . . H H10B 0.6566 -0.1337 0.3027 0.061 Uiso calc U . R 1 . . H H10C 0.5557 -0.0746 0.3301 0.061 Uiso calc U . R 1 . . C C11A 0.5036(6) 0.2040(12) 0.27962(13) 0.0397(14) Uani d . . . 1 . . H H11A 0.4194 0.1354 0.2875 0.059 Uiso calc U . R 1 . . H H11B 0.5396 0.103 0.2635 0.059 Uiso calc U . R 1 . . H H11C 0.4853 0.3621 0.2715 0.059 Uiso calc U . R 1 . . N N1B 0.2348(4) 0.5171(9) 0.62611(12) 0.0286(12) Uani d . . D 1 . . H H01B 0.153(4) 0.526(12) 0.6330(17) 0.043 Uiso d U . D 1 . . C C1B 0.2711(5) 0.5939(10) 0.59582(12) 0.0295(11) Uani d . . . 1 . . H H1B 0.3436 0.4861 0.5881 0.035 Uiso calc U . R 1 . . C C2B 0.1483(5) 0.5676(11) 0.57541(13) 0.0315(12) Uani d . . . 1 . . H H211 0.0723 0.6611 0.5839 0.038 Uiso calc U . R 1 . . H H212 0.1201 0.3995 0.5751 0.038 Uiso calc U . R 1 . . C C3B 0.1765(5) 0.6498(11) 0.54297(12) 0.0350(12) Uani d . . . 1 . . H H311 0.2453 0.5457 0.5336 0.042 Uiso calc U . R 1 . . H H312 0.0923 0.6394 0.5308 0.042 Uiso calc U . R 1 . . C C4B 0.2278(5) 0.9052(11) 0.54316(12) 0.0314(12) Uani d . . . 1 . . H H4B 0.1554 1.0091 0.5518 0.038 Uiso calc U . R 1 . . O O1B 0.2604(4) 0.9873(8) 0.51352(12) 0.0353(11) Uani d . . D 1 . . H H02B 0.204(6) 0.944(13) 0.4998(12) 0.053 Uiso d U . D 1 . . C C5B 0.3537(5) 0.9270(12) 0.56265(13) 0.0342(12) Uani d . . . 1 . . H H511 0.3842 1.0937 0.5629 0.041 Uiso calc U . R 1 . . H H512 0.4273 0.8299 0.5538 0.041 Uiso calc U . R 1 . . C C6B 0.3256(5) 0.8450(11) 0.59511(13) 0.0331(12) Uani d . . . 1 . . H H611 0.4105 0.8529 0.607 0.04 Uiso calc U . R 1 . . H H612 0.2589 0.9527 0.6046 0.04 Uiso calc U . R 1 . . C C7B 0.3306(5) 0.4203(10) 0.64505(12) 0.0259(11) Uani d . . . 1 . . O O2B 0.4472(3) 0.3752(7) 0.63819(8) 0.0326(9) Uani d . . . 1 . . O O3B 0.2725(3) 0.3734(7) 0.67242(8) 0.0300(8) Uani d . . . 1 . . C C8B 0.3445(5) 0.2240(9) 0.69439(12) 0.0279(11) Uani d . . . 1 . . C C9B 0.4719(5) 0.3413(10) 0.70617(13) 0.0325(12) Uani d . . . 1 . . H H911 0.5414 0.3406 0.6903 0.049 Uiso calc U . R 1 . . H H912 0.5053 0.2546 0.7239 0.049 Uiso calc U . R 1 . . H H913 0.4516 0.5049 0.712 0.049 Uiso calc U . R 1 . . C C10B 0.2388(5) 0.2084(11) 0.71967(13) 0.0373(13) Uani d . . . 1 . . H H10D 0.2159 0.368 0.7267 0.056 Uiso calc U . R 1 . . H H10E 0.2757 0.1167 0.7366 0.056 Uiso calc U . R 1 . . H H10F 0.157 0.1306 0.712 0.056 Uiso calc U . R 1 . . C C11B 0.3691(7) -0.0193(11) 0.68104(18) 0.0410(17) Uani d . . . 1 . . H H11D 0.2839 -0.0824 0.673 0.062 Uiso calc U . R 1 . . H H11E 0.4036 -0.1252 0.6968 0.062 Uiso calc U . R 1 . . H H11F 0.4359 -0.0076 0.6646 0.062 Uiso calc U . R 1 . . 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 N1A 0.0074(17) 0.035(3) 0.039(3) -0.0018(16) -0.0007(17) -0.004(2) C1A 0.016(2) 0.035(3) 0.033(3) 0.002(2) -0.001(2) 0.001(3) C2A 0.030(3) 0.036(3) 0.035(3) -0.008(3) 0.000(2) 0.001(3) C3A 0.029(3) 0.044(3) 0.036(3) -0.004(2) 0.004(2) 0.000(3) C4A 0.021(2) 0.042(3) 0.030(3) -0.004(2) -0.002(2) -0.007(2) O1A 0.032(2) 0.069(3) 0.033(3) -0.002(2) -0.0005(18) -0.016(2) C5A 0.029(3) 0.031(3) 0.041(3) -0.006(2) 0.001(2) -0.005(3) C6A 0.022(2) 0.039(3) 0.036(3) -0.008(2) 0.003(2) 0.002(3) C7A 0.032(3) 0.025(3) 0.030(3) -0.002(2) -0.001(2) 0.002(2) O2A 0.0227(19) 0.046(3) 0.034(2) 0.0062(16) -0.0004(15) -0.0007(17) O3A 0.0233(17) 0.033(2) 0.0288(18) 0.0050(15) 0.0008(15) -0.0039(16) C8A 0.022(2) 0.026(3) 0.033(3) -0.004(2) 0.004(2) -0.006(2) C9A 0.027(3) 0.035(3) 0.039(3) 0.001(2) 0.008(2) -0.002(3) C10A 0.039(3) 0.031(4) 0.053(5) 0.004(3) 0.011(3) 0.001(3) C11A 0.035(3) 0.047(4) 0.037(3) -0.004(3) -0.002(2) -0.012(3) N1B 0.015(2) 0.044(3) 0.027(3) 0.0053(18) -0.0002(18) 0.003(2) C1B 0.026(3) 0.034(3) 0.028(3) -0.001(2) 0.001(2) 0.002(3) C2B 0.026(3) 0.031(3) 0.037(3) -0.004(2) -0.005(2) 0.004(3) C3B 0.027(3) 0.045(3) 0.033(3) -0.001(2) -0.005(2) -0.001(3) C4B 0.019(2) 0.042(3) 0.032(3) 0.010(2) 0.005(2) 0.004(2) O1B 0.0231(19) 0.052(3) 0.031(2) 0.0025(16) -0.0002(15) 0.0106(17) C5B 0.028(3) 0.042(3) 0.032(3) -0.003(3) 0.000(2) 0.001(3) C6B 0.027(2) 0.041(3) 0.031(3) -0.001(2) -0.004(2) 0.001(3) C7B 0.014(2) 0.029(3) 0.035(3) 0.003(2) 0.0011(19) 0.001(2) O2B 0.0171(18) 0.042(2) 0.038(2) -0.0012(16) 0.0012(14) 0.0063(17) O3B 0.0260(18) 0.033(2) 0.0309(18) 0.0018(15) 0.0005(15) 0.0092(16) C8B 0.030(3) 0.021(3) 0.033(3) 0.007(2) 0.001(2) 0.003(2) C9B 0.028(3) 0.027(3) 0.042(3) 0.000(2) -0.003(2) 0.004(2) C10B 0.026(3) 0.046(4) 0.040(3) 0.001(3) 0.001(2) 0.013(3) C11B 0.059(4) 0.026(3) 0.038(4) -0.003(3) -0.008(3) -0.004(2) _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 N1A C7A . 1.297(8) ? N1A C1A . 1.463(8) ? N1A H01A . 0.89(3) ? C1A C2A . 1.513(7) ? C1A C6A . 1.538(8) ? C1A H1A . 1.0 ? C2A C3A . 1.525(8) ? C2A H201 . 0.99 ? C2A H202 . 0.99 ? C3A C4A . 1.518(8) ? C3A H301 . 0.99 ? C3A H302 . 0.99 ? C4A O1A . 1.432(7) ? C4A C5A . 1.501(7) ? C4A H4A . 1.0 ? O1A H02A . 0.89(3) ? C5A C6A . 1.536(8) ? C5A H501 . 0.99 ? C5A H502 . 0.99 ? C6A H601 . 0.99 ? C6A H602 . 0.99 ? C7A O2A . 1.233(6) ? C7A O3A . 1.347(6) ? O3A C8A . 1.470(6) ? C8A C11A . 1.514(7) ? C8A C9A . 1.526(7) ? C8A C10A . 1.527(9) ? C9A H901 . 0.98 ? C9A H902 . 0.98 ? C9A H903 . 0.98 ? C10A H10A . 0.98 ? C10A H10B . 0.98 ? C10A H10C . 0.98 ? C11A H11A . 0.98 ? C11A H11B . 0.98 ? C11A H11C . 0.98 ? N1B C7B . 1.375(7) ? N1B C1B . 1.450(8) ? N1B H01B . 0.86(3) ? C1B C2B . 1.516(7) ? C1B C6B . 1.519(8) ? C1B H1B . 1.0 ? C2B C3B . 1.531(8) ? C2B H211 . 0.99 ? C2B H212 . 0.99 ? C3B C4B . 1.530(8) ? C3B H311 . 0.99 ? C3B H312 . 0.99 ? C4B O1B . 1.424(8) ? C4B C5B . 1.515(7) ? C4B H4B . 1.0 ? O1B H02B . 0.86(3) ? C5B C6B . 1.531(8) ? C5B H511 . 0.99 ? C5B H512 . 0.99 ? C6B H611 . 0.99 ? C6B H612 . 0.99 ? C7B O2B . 1.216(6) ? C7B O3B . 1.363(6) ? O3B C8B . 1.469(6) ? C8B C9B . 1.513(7) ? C8B C11B . 1.516(8) ? C8B C10B . 1.529(7) ? C9B H911 . 0.98 ? C9B H912 . 0.98 ? C9B H913 . 0.98 ? C10B H10D . 0.98 ? C10B H10E . 0.98 ? C10B H10F . 0.98 ? C11B H11D . 0.98 ? C11B H11E . 0.98 ? C11B H11F . 0.98 ? 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 C7A N1A C1A . . 124.8(4) ? C7A N1A H01A . . 123.(5) ? C1A N1A H01A . . 111.(5) ? N1A C1A C2A . . 111.1(4) ? N1A C1A C6A . . 111.0(5) ? C2A C1A C6A . . 110.5(5) ? N1A C1A H1A . . 108.0 ? C2A C1A H1A . . 108.0 ? C6A C1A H1A . . 108.0 ? C1A C2A C3A . . 112.1(5) ? C1A C2A H201 . . 109.2 ? C3A C2A H201 . . 109.2 ? C1A C2A H202 . . 109.2 ? C3A C2A H202 . . 109.2 ? H201 C2A H202 . . 107.9 ? C4A C3A C2A . . 110.6(5) ? C4A C3A H301 . . 109.5 ? C2A C3A H301 . . 109.5 ? C4A C3A H302 . . 109.5 ? C2A C3A H302 . . 109.5 ? H301 C3A H302 . . 108.1 ? O1A C4A C5A . . 108.3(4) ? O1A C4A C3A . . 111.3(5) ? C5A C4A C3A . . 110.5(5) ? O1A C4A H4A . . 108.9 ? C5A C4A H4A . . 108.9 ? C3A C4A H4A . . 108.9 ? C4A O1A H02A . . 99.(4) ? C4A C5A C6A . . 111.7(4) ? C4A C5A H501 . . 109.3 ? C6A C5A H501 . . 109.3 ? C4A C5A H502 . . 109.3 ? C6A C5A H502 . . 109.3 ? H501 C5A H502 . . 107.9 ? C5A C6A C1A . . 110.8(5) ? C5A C6A H601 . . 109.5 ? C1A C6A H601 . . 109.5 ? C5A C6A H602 . . 109.5 ? C1A C6A H602 . . 109.5 ? H601 C6A H602 . . 108.1 ? O2A C7A N1A . . 124.2(5) ? O2A C7A O3A . . 124.3(5) ? N1A C7A O3A . . 111.4(5) ? C7A O3A C8A . . 121.2(4) ? O3A C8A C11A . . 102.8(4) ? O3A C8A C9A . . 110.3(4) ? C11A C8A C9A . . 110.1(5) ? O3A C8A C10A . . 110.3(5) ? C11A C8A C10A . . 111.3(5) ? C9A C8A C10A . . 111.7(5) ? C8A C9A H901 . . 109.5 ? C8A C9A H902 . . 109.5 ? H901 C9A H902 . . 109.5 ? C8A C9A H903 . . 109.5 ? H901 C9A H903 . . 109.5 ? H902 C9A H903 . . 109.5 ? C8A C10A H10A . . 109.5 ? C8A C10A H10B . . 109.5 ? H10A C10A H10B . . 109.5 ? C8A C10A H10C . . 109.5 ? H10A C10A H10C . . 109.5 ? H10B C10A H10C . . 109.5 ? C8A C11A H11A . . 109.5 ? C8A C11A H11B . . 109.5 ? H11A C11A H11B . . 109.5 ? C8A C11A H11C . . 109.5 ? H11A C11A H11C . . 109.5 ? H11B C11A H11C . . 109.5 ? C7B N1B C1B . . 120.6(4) ? C7B N1B H01B . . 117.(5) ? C1B N1B H01B . . 123.(5) ? N1B C1B C2B . . 108.7(4) ? N1B C1B C6B . . 112.7(5) ? C2B C1B C6B . . 111.2(5) ? N1B C1B H1B . . 108.0 ? C2B C1B H1B . . 108.0 ? C6B C1B H1B . . 108.0 ? C1B C2B C3B . . 112.4(4) ? C1B C2B H211 . . 109.1 ? C3B C2B H211 . . 109.1 ? C1B C2B H212 . . 109.1 ? C3B C2B H212 . . 109.1 ? H211 C2B H212 . . 107.9 ? C4B C3B C2B . . 110.0(5) ? C4B C3B H311 . . 109.7 ? C2B C3B H311 . . 109.7 ? C4B C3B H312 . . 109.7 ? C2B C3B H312 . . 109.7 ? H311 C3B H312 . . 108.2 ? O1B C4B C5B . . 108.0(4) ? O1B C4B C3B . . 112.1(5) ? C5B C4B C3B . . 110.5(5) ? O1B C4B H4B . . 108.7 ? C5B C4B H4B . . 108.7 ? C3B C4B H4B . . 108.7 ? C4B O1B H02B . . 114.(5) ? C4B C5B C6B . . 111.0(4) ? C4B C5B H511 . . 109.4 ? C6B C5B H511 . . 109.4 ? C4B C5B H512 . . 109.4 ? C6B C5B H512 . . 109.4 ? H511 C5B H512 . . 108.0 ? C1B C6B C5B . . 111.5(5) ? C1B C6B H611 . . 109.3 ? C5B C6B H611 . . 109.3 ? C1B C6B H612 . . 109.3 ? C5B C6B H612 . . 109.3 ? H611 C6B H612 . . 108.0 ? O2B C7B O3B . . 125.3(5) ? O2B C7B N1B . . 125.6(5) ? O3B C7B N1B . . 109.1(4) ? C7B O3B C8B . . 119.6(4) ? O3B C8B C9B . . 112.1(4) ? O3B C8B C11B . . 110.1(5) ? C9B C8B C11B . . 113.5(5) ? O3B C8B C10B . . 100.7(4) ? C9B C8B C10B . . 109.9(5) ? C11B C8B C10B . . 109.9(5) ? C8B C9B H911 . . 109.5 ? C8B C9B H912 . . 109.5 ? H911 C9B H912 . . 109.5 ? C8B C9B H913 . . 109.5 ? H911 C9B H913 . . 109.5 ? H912 C9B H913 . . 109.5 ? C8B C10B H10D . . 109.5 ? C8B C10B H10E . . 109.5 ? H10D C10B H10E . . 109.5 ? C8B C10B H10F . . 109.5 ? H10D C10B H10F . . 109.5 ? H10E C10B H10F . . 109.5 ? C8B C11B H11D . . 109.5 ? C8B C11B H11E . . 109.5 ? H11D C11B H11E . . 109.5 ? C8B C11B H11F . . 109.5 ? H11D C11B H11F . . 109.5 ? H11E C11B H11F . . 109.5 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C7A N1A C1A C2A . . . . -145.2(6) ? C7A N1A C1A C6A . . . . 91.4(6) ? N1A C1A C2A C3A . . . . -178.8(5) ? C6A C1A C2A C3A . . . . -55.1(6) ? C1A C2A C3A C4A . . . . 56.9(7) ? C2A C3A C4A O1A . . . . -177.6(4) ? C2A C3A C4A C5A . . . . -57.2(6) ? O1A C4A C5A C6A . . . . 179.5(5) ? C3A C4A C5A C6A . . . . 57.3(6) ? C4A C5A C6A C1A . . . . -55.8(6) ? N1A C1A C6A C5A . . . . 177.6(4) ? C2A C1A C6A C5A . . . . 53.8(6) ? C1A N1A C7A O2A . . . . -2.0(9) ? C1A N1A C7A O3A . . . . -179.1(5) ? O2A C7A O3A C8A . . . . 16.0(8) ? N1A C7A O3A C8A . . . . -167.0(4) ? C7A O3A C8A C11A . . . . 173.8(5) ? C7A O3A C8A C9A . . . . -68.8(6) ? C7A O3A C8A C10A . . . . 55.0(6) ? C7B N1B C1B C2B . . . . 150.2(5) ? C7B N1B C1B C6B . . . . -86.0(6) ? N1B C1B C2B C3B . . . . 178.8(5) ? C6B C1B C2B C3B . . . . 54.1(6) ? C1B C2B C3B C4B . . . . -55.7(6) ? C2B C3B C4B O1B . . . . 177.8(4) ? C2B C3B C4B C5B . . . . 57.2(6) ? O1B C4B C5B C6B . . . . 179.2(5) ? C3B C4B C5B C6B . . . . -57.8(6) ? N1B C1B C6B C5B . . . . -176.0(4) ? C2B C1B C6B C5B . . . . -53.6(6) ? C4B C5B C6B C1B . . . . 56.0(6) ? C1B N1B C7B O2B . . . . -5.3(9) ? C1B N1B C7B O3B . . . . 177.2(5) ? O2B C7B O3B C8B . . . . -10.5(8) ? N1B C7B O3B C8B . . . . 167.0(4) ? C7B O3B C8B C9B . . . . 66.9(6) ? C7B O3B C8B C11B . . . . -60.3(6) ? C7B O3B C8B C10B . . . . -176.3(5) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1A H01A O2A 3_465 0.89(3) 2.12(3) 3.003(6) 171.(6) ? O1A H02A O1B . 0.89(3) 1.84(3) 2.729(7) 174.(6) ? N1B H01B O2B 3_465 0.86(3) 2.12(4) 2.949(5) 162.(7) ? O1B H02B O1A 3_475 0.86(3) 2.05(6) 2.721(7) 135.(7) ? _shelx_res_file ; glo9616.res created by SHELXL-2014/7 TITL glo9616.res in Pca2(1) CELL 1.54178 9.8601 5.6544 44.1243 90.000 90.000 90.000 ZERR 8.000 0.0003 0.0002 0.0015 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 1/2+Z SYMM 1/2+X, -Y, Z SYMM 1/2-X, Y, 1/2+Z SFAC C H N O UNIT 88 168 8 24 SIZE 0.052 0.069 0.12 TEMP -173.150 ACTA CONF OMIT 7 2 5 OMIT 7 2 2 OMIT 6 4 6 OMIT 7 2 -5 OMIT 6 1 0 OMIT 6 4 0 OMIT 10 0 -3 OMIT 7 2 -2 OMIT 4 4 7 L.S. 30 BOND $H FMAP 2 PLAN 10 HTAB EQIV $1 x-1/2, -y+1, z HTAB N1A O2A_$1 HTAB O1A O1B HTAB N1B O2B_$1 EQIV $2 x-1/2, -y+2, z HTAB O1B O1A_$2 DFIX 0.88 N1A H01A SADI N1A H01A WGHT 0.000000 3.514700 FVAR 0.48918 N1A 3 0.505288 0.514362 0.372677 11.00000 0.00740 0.03480 = 0.03934 -0.00352 -0.00067 -0.00176 H01A 2 0.417504 0.531450 0.368188 11.00000 -1.50000 C1A 1 0.533475 0.584845 0.403953 11.00000 0.01565 0.03488 = 0.03323 0.00115 -0.00060 0.00166 AFIX 13 H1A 2 0.607767 0.481511 0.411870 11.00000 -1.20000 AFIX 0 C2A 1 0.410181 0.550088 0.423893 11.00000 0.03005 0.03635 = 0.03529 0.00093 -0.00001 -0.00770 AFIX 23 H201 2 0.384120 0.381010 0.423694 11.00000 -1.20000 H202 2 0.333475 0.642345 0.415537 11.00000 -1.20000 AFIX 0 C3A 1 0.436191 0.627369 0.456487 11.00000 0.02946 0.04351 = 0.03561 -0.00050 0.00370 -0.00438 AFIX 23 H301 2 0.352229 0.608075 0.468539 11.00000 -1.20000 H302 2 0.507235 0.525919 0.465562 11.00000 -1.20000 AFIX 0 C4A 1 0.481302 0.883935 0.457504 11.00000 0.02057 0.04241 = 0.02965 -0.00718 -0.00161 -0.00366 AFIX 13 H4A 2 0.406784 0.985710 0.449366 11.00000 -1.20000 AFIX 0 DFIX 0.88 O1A h02A SADI O1A H02A O1A 4 0.511612 0.956568 0.487844 11.00000 0.03199 0.06898 = 0.03285 -0.01637 -0.00045 -0.00187 H02A 2 0.427032 0.968455 0.494881 11.00000 0.04550 C5A 1 0.605886 0.919125 0.438471 11.00000 0.02918 0.03066 = 0.04060 -0.00514 0.00112 -0.00613 AFIX 23 H501 2 0.681555 0.825968 0.447129 11.00000 -1.20000 H502 2 0.632157 1.088070 0.438941 11.00000 -1.20000 AFIX 0 C6A 1 0.582363 0.842867 0.405471 11.00000 0.02214 0.03871 = 0.03558 0.00156 0.00343 -0.00783 AFIX 23 H601 2 0.667886 0.859303 0.393907 11.00000 -1.20000 H602 2 0.513707 0.947365 0.396053 11.00000 -1.20000 AFIX 0 C7A 1 0.592484 0.416540 0.354580 11.00000 0.03189 0.02476 = 0.03013 0.00223 -0.00086 -0.00216 O2A 4 0.711602 0.376336 0.361303 11.00000 0.02274 0.04629 = 0.03443 -0.00071 -0.00044 0.00622 O3A 4 0.538113 0.374900 0.327098 11.00000 0.02332 0.03295 = 0.02884 -0.00395 0.00082 0.00504 C8A 1 0.606645 0.221675 0.304978 11.00000 0.02216 0.02636 = 0.03300 -0.00555 0.00431 -0.00413 C9A 1 0.735975 0.339604 0.293474 11.00000 0.02734 0.03543 = 0.03857 -0.00208 0.00781 0.00083 AFIX 137 H901 2 0.713915 0.495228 0.285033 11.00000 -1.50000 H902 2 0.777122 0.240900 0.277702 11.00000 -1.50000 H903 2 0.799949 0.358419 0.310300 11.00000 -1.50000 AFIX 0 C10A 1 0.635579 -0.020457 0.318884 11.00000 0.03854 0.03072 = 0.05323 0.00062 0.01073 0.00356 AFIX 137 H10A 2 0.713044 -0.008389 0.332713 11.00000 -1.50000 H10B 2 0.656585 -0.133720 0.302741 11.00000 -1.50000 H10C 2 0.555676 -0.074638 0.330121 11.00000 -1.50000 AFIX 0 C11A 1 0.503635 0.203977 0.279623 11.00000 0.03465 0.04714 = 0.03718 -0.01198 -0.00157 -0.00413 AFIX 137 H11A 2 0.419395 0.135399 0.287478 11.00000 -1.50000 H11B 2 0.539597 0.102952 0.263465 11.00000 -1.50000 H11C 2 0.485251 0.362127 0.271519 11.00000 -1.50000 AFIX 0 N1B 3 0.234767 0.517122 0.626108 11.00000 0.01508 0.04389 = 0.02692 0.00294 -0.00019 0.00529 DFIX 0.88 n1b h01b SADI N1B H01B H01B 2 0.153181 0.526308 0.633006 11.00000 -1.50000 C1B 1 0.271051 0.593859 0.595821 11.00000 0.02566 0.03448 = 0.02824 0.00209 0.00147 -0.00081 AFIX 13 H1B 2 0.343643 0.486121 0.588083 11.00000 -1.20000 AFIX 0 C2B 1 0.148270 0.567561 0.575412 11.00000 0.02574 0.03140 = 0.03733 0.00352 -0.00526 -0.00403 AFIX 23 H211 2 0.072318 0.661133 0.583871 11.00000 -1.20000 H212 2 0.120096 0.399533 0.575053 11.00000 -1.20000 AFIX 0 C3B 1 0.176477 0.649811 0.542970 11.00000 0.02684 0.04483 = 0.03337 -0.00070 -0.00455 -0.00072 AFIX 23 H311 2 0.245338 0.545720 0.533553 11.00000 -1.20000 H312 2 0.092319 0.639352 0.530807 11.00000 -1.20000 AFIX 0 C4B 1 0.227808 0.905232 0.543159 11.00000 0.01944 0.04247 = 0.03234 0.00417 0.00515 0.00951 AFIX 13 H4B 2 0.155431 1.009103 0.551812 11.00000 -1.20000 AFIX 0 DFIX 0.88 O1b h02b SADI O1B H02B O1B 4 0.260416 0.987273 0.513521 11.00000 0.02309 0.05207 = 0.03074 0.01064 -0.00023 0.00251 H02B 2 0.203937 0.944234 0.499826 11.00000 -1.50000 C5B 1 0.353694 0.926965 0.562648 11.00000 0.02785 0.04236 = 0.03224 0.00084 -0.00036 -0.00349 AFIX 23 H511 2 0.384219 1.093750 0.562901 11.00000 -1.20000 H512 2 0.427338 0.829893 0.553825 11.00000 -1.20000 AFIX 0 C6B 1 0.325619 0.845009 0.595113 11.00000 0.02656 0.04134 = 0.03127 0.00073 -0.00438 -0.00146 AFIX 23 H611 2 0.410530 0.852937 0.607044 11.00000 -1.20000 H612 2 0.258894 0.952707 0.604632 11.00000 -1.20000 AFIX 0 C7B 1 0.330624 0.420297 0.645048 11.00000 0.01363 0.02870 = 0.03543 0.00144 0.00110 0.00250 O2B 4 0.447205 0.375217 0.638193 11.00000 0.01710 0.04245 = 0.03825 0.00632 0.00121 -0.00116 O3B 4 0.272458 0.373425 0.672424 11.00000 0.02600 0.03318 = 0.03091 0.00915 0.00050 0.00183 C8B 1 0.344473 0.223962 0.694393 11.00000 0.02955 0.02145 = 0.03276 0.00301 0.00134 0.00685 C9B 1 0.471914 0.341335 0.706168 11.00000 0.02817 0.02746 = 0.04189 0.00408 -0.00275 -0.00004 AFIX 137 H911 2 0.541406 0.340612 0.690289 11.00000 -1.50000 H912 2 0.505307 0.254553 0.723886 11.00000 -1.50000 H913 2 0.451570 0.504861 0.711955 11.00000 -1.50000 AFIX 0 C10B 1 0.238790 0.208409 0.719671 11.00000 0.02623 0.04598 = 0.03965 0.01292 0.00066 0.00096 AFIX 137 H10D 2 0.215912 0.368021 0.726656 11.00000 -1.50000 H10E 2 0.275744 0.116650 0.736607 11.00000 -1.50000 H10F 2 0.156974 0.130587 0.711953 11.00000 -1.50000 AFIX 0 C11B 1 0.369143 -0.019315 0.681035 11.00000 0.05893 0.02584 = 0.03832 -0.00351 -0.00787 -0.00318 AFIX 137 H11D 2 0.283860 -0.082377 0.672986 11.00000 -1.50000 H11E 2 0.403630 -0.125200 0.696840 11.00000 -1.50000 H11F 2 0.435884 -0.007613 0.664646 11.00000 -1.50000 AFIX 0 HKLF 4 REM glo9616.res in Pca2(1) REM R1 = 0.0572 for 4145 Fo > 4sig(Fo) and 0.0624 for all 4551 data REM 290 parameters refined using 5 restraints END WGHT 0.0000 3.5146 REM Instructions for potential hydrogen bonds HTAB N1A O2A_$1 HTAB O1A O1B HTAB C9A O2A HTAB C10A O2A HTAB N1B O2B_$1 HTAB O1B O1A_$2 HTAB C9B O2B HTAB C11B O2B REM Highest difference peak 0.226, deepest hole -0.215, 1-sigma level 0.053 Q1 1 0.2569 0.9603 0.5621 11.00000 0.05 0.22 Q2 1 0.7522 0.5565 0.3629 11.00000 0.05 0.22 Q3 1 0.4203 0.5363 0.6413 11.00000 0.05 0.21 Q4 1 0.5751 0.5995 0.3267 11.00000 0.05 0.21 Q5 1 0.2689 0.9949 0.5296 11.00000 0.05 0.21 Q6 1 0.7282 0.3316 0.3413 11.00000 0.05 0.20 Q7 1 0.5213 0.5209 0.3885 11.00000 0.05 0.20 Q8 1 0.5292 0.4895 0.6305 11.00000 0.05 0.20 Q9 1 0.5129 0.5278 0.3485 11.00000 0.05 0.19 Q10 1 0.4239 -0.0894 0.7160 11.00000 0.05 0.19 ; _shelx_res_checksum 71143 _shelx_hkl_file ; 0 -1 0 1226.98 83.59 0 1 0 1212.78 83.49 0 -1 0 1224.28 83.49 0 -2 0 3892.21 266.67 0 -2 0 3978.40 266.57 0 -3 0 366.36 30.50 0 -3 0 412.66 31.00 0 4 0 331.97 25.70 0 4 0 400.36 27.10 0 4 0 372.66 27.40 0 4 0 289.97 26.70 0 4 0 374.86 26.80 0 5 0 437.36 29.60 0 5 0 354.86 28.90 0 5 0 398.96 28.70 0 5 0 401.26 30.50 0 5 0 383.46 29.80 0 -5 0 373.96 28.30 0 6 0 0.80 3.80 0 6 0 -5.00 2.20 0 6 0 1.40 5.20 -1 0 0 -0.60 1.00 1 0 0 0.00 1.00 -1 0 0 0.30 1.10 1 0 0 -0.30 0.50 -1 1 0 680.33 47.00 1 -1 0 680.83 47.00 1 -1 0 650.73 46.80 -1 1 0 679.43 46.80 -1 1 0 645.54 46.10 1 -2 0 439.66 31.00 -1 2 0 395.96 31.20 -1 2 0 394.96 29.50 1 -2 0 419.96 31.70 1 -2 0 434.46 31.60 1 -3 0 682.93 48.10 1 -3 0 613.64 46.50 1 -3 0 538.75 45.90 1 4 0 16.60 5.60 -1 4 0 13.90 4.80 1 -4 0 19.10 3.50 -1 4 0 17.00 6.20 -1 4 0 13.10 4.60 1 4 0 9.50 4.00 1 4 0 17.00 4.50 1 4 0 14.00 5.40 -1 4 0 14.50 4.10 1 4 0 12.40 4.20 1 5 0 8.10 4.50 -1 5 0 12.30 4.50 -1 5 0 12.60 5.00 -1 5 0 7.80 4.30 -1 5 0 16.70 7.30 1 5 0 5.20 3.70 1 5 0 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13.70 -4 0 22 171.88 13.60 -4 1 -22 62.09 10.20 -4 -1 22 67.49 10.40 4 -1 -22 40.50 6.10 4 1 22 58.29 6.70 -4 1 -22 59.59 6.90 -4 1 -22 62.69 14.90 4 -1 -22 57.69 6.90 4 -1 -22 62.99 5.40 4 -1 -22 51.09 6.10 4 1 22 61.89 7.10 4 1 22 69.19 7.40 -4 1 -22 57.39 5.70 -4 -1 -22 78.19 10.60 -4 1 22 60.49 9.90 -4 1 22 47.80 6.70 4 1 -22 56.99 6.60 4 -1 22 55.99 6.40 4 -1 22 78.89 8.40 4 1 -22 54.09 5.90 -4 1 22 53.89 6.00 4 1 -22 54.49 7.20 4 -1 22 53.69 6.30 4 1 -22 47.90 6.20 4 -1 22 49.80 9.50 -4 -1 -22 26.60 10.70 -4 1 22 62.59 7.00 4 1 -22 50.69 6.90 4 2 22 3.40 2.20 4 -2 -22 -1.70 6.50 -4 2 -22 1.60 2.40 4 2 22 2.60 4.30 4 -2 -22 8.50 3.40 4 -2 -22 -1.10 2.50 -4 2 -22 3.10 6.80 4 2 22 0.10 3.80 -4 2 -22 -1.80 3.30 -4 2 -22 2.20 3.20 4 2 -22 4.60 3.70 4 -2 22 1.10 3.10 -4 2 22 3.60 6.00 -4 2 22 4.90 4.20 4 2 -22 1.40 3.50 -4 2 22 2.30 2.50 4 2 -22 1.80 3.70 4 2 -22 1.50 4.00 -4 -2 -22 6.60 4.00 4 -2 22 1.80 6.70 4 -2 22 1.50 3.30 -4 2 22 3.20 3.70 4 2 -22 -0.20 3.70 4 -3 -22 101.89 10.60 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4.40 1 -3 -28 10.70 3.90 1 3 28 12.00 5.50 -1 3 -28 11.60 3.50 1 3 28 17.70 4.20 -1 3 28 8.60 4.40 1 3 -28 11.90 3.90 1 -3 28 13.00 7.40 1 3 -28 15.50 5.00 -1 -3 -28 15.50 4.00 1 3 -28 20.10 5.10 -1 3 28 8.60 4.30 1 3 -28 23.30 6.40 -1 3 28 21.10 5.50 1 3 -28 13.50 5.00 1 -4 -28 94.19 9.70 1 4 28 80.29 12.70 1 4 28 82.19 11.20 -1 4 -28 58.59 11.30 -1 4 -28 81.89 12.00 1 -4 -28 63.49 6.70 -1 4 -28 74.29 10.50 -1 4 -28 73.39 7.50 1 4 -28 48.10 10.00 -1 -4 -28 80.49 7.60 1 4 -28 85.69 9.40 -1 -4 -28 71.99 6.90 -1 4 28 58.19 7.40 -1 4 28 65.69 8.50 1 4 -28 59.99 9.40 1 -5 -28 29.50 4.60 -1 5 -28 25.10 4.20 1 -5 -28 23.20 5.40 -1 5 -28 23.00 4.40 -1 5 -28 30.30 5.60 1 5 28 32.70 6.90 1 5 28 28.30 5.40 -1 5 28 29.30 4.80 1 5 -28 28.30 4.90 1 5 -28 32.40 5.10 1 5 -28 32.10 6.90 -1 5 28 23.10 5.50 -1 -5 -28 27.90 4.50 2 0 -28 251.17 25.30 -2 0 -28 231.48 17.10 2 0 -28 230.68 18.20 -2 0 -28 235.38 17.50 -2 0 28 221.08 18.10 -2 0 -28 254.57 22.10 2 0 -28 247.08 19.20 2 0 28 234.28 17.80 -2 0 28 236.18 17.30 2 0 28 263.97 22.00 2 0 -28 239.18 17.70 -2 0 28 275.97 22.50 2 0 28 233.68 17.90 2 0 -28 198.28 16.80 2 1 28 140.39 11.30 -2 1 -28 138.09 10.40 2 -1 -28 131.19 10.50 -2 1 -28 141.49 11.10 2 1 28 122.79 12.50 -2 -1 28 136.49 15.30 -2 1 -28 142.79 20.60 -2 1 -28 141.99 11.20 -2 1 -28 149.19 16.60 2 -1 -28 123.49 10.90 2 1 28 143.99 11.70 2 -1 -28 122.89 11.80 2 -1 28 135.09 16.30 -2 1 28 142.99 10.70 -2 1 28 147.19 15.20 -2 1 28 131.09 11.80 -2 -1 -28 138.39 10.90 2 1 -28 128.49 11.70 -2 -1 -28 128.29 10.70 2 1 -28 127.29 10.70 2 -1 28 137.09 11.10 2 1 -28 133.59 11.20 2 1 -28 136.69 11.70 2 1 -28 138.29 13.50 2 -1 28 134.19 11.50 -2 2 -28 1.50 3.40 -2 2 -28 -2.50 3.20 2 -2 -28 7.90 10.10 2 -2 -28 2.90 3.00 -2 -2 28 10.10 7.70 2 -2 -28 1.60 3.10 2 2 28 2.20 3.90 -2 2 -28 1.80 2.90 2 2 28 5.90 4.50 2 2 28 4.20 3.20 -2 2 -28 2.20 6.00 2 2 -28 2.50 4.10 2 -2 28 1.20 3.10 -2 -2 -28 4.80 3.10 -2 -2 -28 18.70 10.10 2 2 -28 1.30 3.40 -2 2 28 2.10 5.20 -2 2 28 7.10 3.80 2 -2 28 6.00 3.20 2 -2 28 0.80 6.20 2 2 -28 3.80 3.50 -2 2 28 4.70 4.10 2 2 -28 4.20 4.00 -2 -2 -28 1.20 2.80 -2 3 -28 37.90 5.40 -2 3 -28 37.80 6.20 2 3 28 48.30 5.60 -2 3 -28 40.10 6.80 2 -3 -28 42.20 5.80 -2 3 -28 41.50 5.70 2 -3 -28 19.00 10.30 2 -3 -28 39.30 6.00 2 3 28 39.50 7.10 2 -3 28 50.49 14.50 2 3 -28 42.30 7.50 -2 -3 -28 46.20 5.90 -2 3 28 48.50 7.00 2 -3 28 34.80 4.90 2 3 -28 50.99 7.30 2 3 -28 46.30 6.40 2 -3 28 38.60 5.80 -2 3 28 40.30 6.40 2 3 -28 47.00 6.50 -2 4 -28 1.60 4.10 -2 4 -28 0.20 4.60 -2 4 -28 8.10 4.50 -2 4 -28 4.90 3.10 2 4 28 1.40 5.00 2 -4 -28 4.40 3.40 2 -4 -28 -1.30 2.70 2 -4 -28 17.40 9.60 2 4 28 -1.30 4.10 2 4 -28 5.30 3.00 2 4 -28 1.60 4.10 2 -4 28 8.60 6.60 2 4 -28 -1.60 4.20 2 4 -28 1.70 4.20 -2 -4 -28 8.10 3.20 -2 -4 -28 3.70 3.10 -2 4 28 5.60 3.60 -2 4 28 4.30 3.70 2 -5 -28 0.60 3.90 -2 5 -28 -1.20 3.30 2 5 28 0.60 5.50 -2 5 -28 -3.00 3.20 2 -5 -28 -0.10 2.60 -2 5 -28 7.50 3.30 2 5 28 2.70 3.00 -2 -5 -28 3.20 2.20 2 5 -28 -2.40 3.10 -2 5 28 -2.70 1.90 2 5 -28 2.10 3.10 2 5 -28 1.10 2.80 -2 5 28 1.20 4.10 -3 0 28 0.60 5.70 -3 0 28 -1.60 2.60 -3 0 28 1.90 3.40 -3 0 -28 -1.60 2.40 3 0 -28 -1.90 3.00 3 0 28 -1.10 2.90 3 0 -28 -0.40 2.40 3 0 -28 -5.50 3.30 3 0 28 1.00 5.10 3 0 -28 2.00 8.70 -3 0 -28 -0.60 6.80 -3 0 -28 -2.60 2.50 3 0 28 1.60 3.50 3 0 -28 1.50 3.90 -3 1 -28 55.19 6.50 -3 1 -28 68.99 13.60 -3 -1 28 82.29 11.00 3 -1 -28 61.29 6.70 -3 1 -28 62.59 5.90 3 -1 -28 45.40 6.50 3 1 28 71.69 7.50 3 1 28 65.69 6.80 -3 1 -28 29.80 15.80 3 -1 -28 59.99 5.90 3 -1 28 59.59 6.70 3 1 -28 68.99 7.00 -3 -1 -28 65.69 11.20 -3 1 28 59.19 6.40 3 -1 28 51.79 10.50 3 1 -28 70.09 7.80 -3 1 28 62.69 11.20 3 1 -28 63.29 6.40 3 1 -28 61.99 7.80 3 1 -28 60.19 6.70 -3 1 28 61.89 7.30 3 -1 28 63.29 7.10 3 1 -28 61.99 8.00 -3 1 28 60.59 7.40 -3 -1 -28 60.99 6.20 3 -2 -28 6.00 8.30 3 2 28 8.60 6.30 -3 -2 28 7.90 7.40 -3 2 -28 12.90 10.20 -3 2 -28 15.60 6.50 -3 2 -28 14.30 3.10 -3 2 -28 19.10 4.50 3 -2 -28 17.10 3.90 -3 2 -28 11.50 3.60 3 2 28 10.50 3.60 3 2 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3.60 3.60 -3 -5 -28 5.20 2.20 3 5 -28 6.40 2.90 3 5 -28 4.90 3.30 -3 5 28 4.20 2.30 3 5 -28 5.30 3.10 4 0 -28 41.00 5.90 -4 0 -28 42.70 5.40 4 0 -28 43.40 6.50 -4 0 28 47.20 6.10 4 0 28 40.90 6.30 -4 0 28 48.40 7.10 -4 0 -28 41.90 5.20 4 0 -28 42.00 7.00 4 0 28 42.80 7.50 4 0 -28 61.39 13.40 4 0 28 43.90 5.90 -4 0 -28 40.80 11.00 -4 0 28 54.19 12.10 4 0 -28 41.90 6.50 4 -1 -28 11.10 3.80 4 -1 -28 8.90 2.70 4 -1 -28 17.50 4.60 -4 -1 28 8.40 7.40 -4 1 -28 13.60 4.10 -4 1 -28 13.40 3.40 4 1 28 11.80 3.80 4 1 28 15.50 5.00 4 -1 -28 8.30 8.40 -4 1 -28 12.10 8.20 4 -1 -28 7.90 4.30 4 -1 28 18.40 4.60 -4 1 28 12.70 4.10 4 1 -28 11.90 4.70 -4 -1 -28 8.90 8.20 -4 1 28 11.60 3.70 -4 -1 -28 12.20 3.50 4 1 -28 15.00 4.00 -4 1 28 16.70 8.10 4 -1 28 6.00 6.30 4 1 -28 12.30 5.30 4 1 -28 14.00 4.80 4 -1 28 21.10 5.10 4 1 -28 14.80 4.10 -4 1 28 10.20 4.40 -4 2 -28 446.06 32.30 4 -2 -28 453.65 32.50 -4 2 -28 486.25 33.50 4 2 28 443.66 32.70 -4 2 -28 472.15 33.80 4 -2 -28 455.95 34.10 -4 2 -28 477.45 32.90 4 2 28 472.25 34.40 4 2 28 501.95 34.10 4 -2 -28 464.45 33.20 -4 2 -28 474.35 38.70 4 2 -28 513.65 33.80 4 -2 28 445.76 33.40 4 2 -28 447.26 33.20 4 2 -28 466.65 34.00 -4 2 28 434.36 38.40 4 -2 28 403.56 38.50 -4 2 28 455.05 32.30 4 -2 28 435.96 33.00 -4 2 28 464.75 33.60 -4 -2 -28 437.96 32.60 4 2 -28 503.05 34.40 -4 2 28 497.55 34.10 4 3 28 13.60 5.50 -4 3 -28 23.50 5.40 4 -3 -28 19.50 4.40 -4 3 -28 17.70 4.60 4 -3 -28 13.80 3.80 4 -3 -28 23.30 6.40 4 -3 -28 18.90 5.30 -4 3 -28 16.90 3.60 4 -3 -28 10.40 9.10 -4 3 -28 5.80 5.60 -4 3 28 18.20 5.10 4 -3 28 19.80 4.90 4 3 -28 11.10 5.70 4 -3 28 11.40 3.70 -4 3 28 18.20 7.50 4 3 -28 13.40 4.30 -4 -3 -28 20.00 4.00 4 -3 28 6.80 8.50 4 3 -28 16.60 4.80 4 3 -28 23.20 5.70 -4 4 -28 68.89 8.10 4 4 28 77.09 9.60 4 -4 -28 46.80 14.20 4 -4 -28 72.59 8.50 4 -4 -28 68.99 6.90 -4 4 -28 75.89 7.90 4 -4 -28 70.79 6.50 4 4 -28 74.49 8.00 4 -4 28 53.99 6.80 4 -4 28 78.79 7.80 -4 -4 -28 64.39 6.70 4 4 -28 80.99 8.60 4 -4 28 70.79 12.10 -4 4 28 59.59 7.50 4 4 -28 77.29 8.00 4 -5 -28 1.20 2.10 4 5 28 -0.30 3.30 -4 5 -28 0.00 2.50 4 -5 -28 -1.80 2.70 -4 5 -28 -2.20 2.50 -4 5 -28 2.30 3.00 4 5 -28 1.70 2.80 -4 -5 -28 1.10 1.90 4 5 -28 0.20 3.00 -4 5 28 1.20 2.10 -4 5 28 2.10 3.00 -5 0 -28 2.10 7.20 5 0 -28 -1.60 3.80 5 0 28 -1.80 4.30 5 0 -28 -0.80 3.80 -5 0 -28 3.00 3.00 5 0 -28 10.10 5.70 -5 0 28 -6.10 3.70 -5 0 28 3.30 3.70 5 0 28 1.40 3.30 -5 0 28 0.30 7.10 -5 1 -28 41.00 12.40 5 -1 -28 45.40 7.20 -5 1 -28 30.90 5.10 -5 1 -28 38.50 5.80 5 -1 -28 31.90 5.70 5 1 28 35.90 5.50 -5 -1 28 36.70 5.70 5 -1 -28 44.10 6.10 5 1 28 46.90 7.30 5 1 -28 49.00 6.20 -5 1 28 44.60 6.10 -5 -1 -28 40.50 5.40 5 1 -28 46.70 6.10 -5 1 28 55.19 7.80 5 -1 28 30.20 5.40 -5 -1 -28 25.80 11.70 -5 1 28 45.40 7.30 5 1 -28 42.30 7.10 5 1 -28 47.00 7.00 5 1 -28 48.90 8.30 5 -1 28 34.30 9.50 -5 1 28 34.70 10.70 5 -1 28 33.90 5.80 5 -1 28 29.70 5.80 5 2 28 5.00 5.60 5 2 28 4.50 5.00 5 -2 -28 0.40 4.20 5 -2 -28 1.40 8.10 5 -2 -28 3.80 4.80 5 -2 -28 4.60 4.20 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-5 28 18.60 2.50 5 -5 -28 14.00 2.60 5 -5 -28 12.80 3.10 -5 5 -28 10.50 2.50 -5 5 -28 8.30 2.80 5 5 28 14.50 3.80 -5 5 -28 9.90 2.60 -5 5 28 11.60 2.80 -5 5 28 10.40 2.40 5 5 -28 12.40 2.80 5 5 -28 19.60 3.40 6 0 -28 28.00 4.80 -6 0 -28 16.50 3.70 -6 0 28 23.30 5.10 -6 0 -28 22.70 4.30 6 0 28 21.90 4.70 6 0 28 28.20 6.10 -6 0 28 8.50 7.00 -6 0 -28 18.90 8.50 6 0 -28 17.70 4.30 6 0 -28 27.90 5.60 6 0 -28 7.70 5.50 -6 0 28 25.80 6.00 6 1 28 426.06 31.70 6 1 28 461.95 33.70 6 -1 -28 456.15 32.40 -6 1 -28 437.76 32.30 -6 1 -28 447.66 31.70 6 1 28 454.75 32.90 -6 -1 28 484.55 39.80 6 -1 -28 413.36 32.50 6 -1 -28 461.05 33.60 6 -1 -28 460.35 32.40 -6 -1 28 448.46 32.10 -6 1 -28 410.56 38.30 6 1 -28 479.35 32.90 6 -1 28 447.36 32.30 6 -1 28 410.76 32.60 -6 1 28 395.66 31.90 6 1 -28 459.65 32.30 6 1 -28 435.76 33.30 -6 -1 -28 489.75 32.30 -6 1 28 429.66 32.70 -6 1 28 527.55 39.40 6 1 -28 443.26 32.30 -6 -2 28 9.80 4.90 6 -2 -28 9.50 9.20 -6 2 -28 -1.90 5.70 -6 2 -28 7.70 4.20 6 2 28 3.90 4.80 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23.50 4.40 8 -2 -28 30.30 5.70 8 -2 -28 23.00 4.30 8 -2 -28 19.20 4.60 -8 2 -28 31.50 4.70 -8 -2 28 22.20 4.20 -8 -2 28 21.50 4.50 8 2 28 30.10 5.50 8 -2 28 30.30 5.30 -8 2 28 26.60 5.00 8 -2 28 19.40 3.80 8 2 -28 21.00 4.40 -8 2 28 19.00 4.60 8 2 -28 30.20 5.10 -8 -2 -28 19.50 4.20 8 3 28 5.00 3.70 8 -3 -28 2.30 2.60 -8 3 -28 0.70 2.30 -8 -3 28 2.30 2.30 -8 -3 28 3.80 2.30 8 -3 -28 1.10 1.90 8 -3 -28 -0.30 2.40 8 -3 28 2.00 2.50 8 3 -28 -1.00 2.30 -8 3 28 -1.60 2.20 8 -3 28 -2.70 2.30 -8 3 28 -0.60 2.10 -8 -3 -28 3.70 2.90 9 0 -28 -3.00 2.10 9 0 28 0.30 4.90 -9 0 -28 1.60 2.80 -9 0 28 0.10 2.60 -9 0 28 3.40 2.60 9 0 -28 -0.80 2.10 -9 0 -28 -2.20 1.80 9 0 28 -0.10 1.90 9 0 -28 -2.10 2.60 9 0 28 1.90 3.60 -9 1 -28 6.90 2.70 9 1 28 6.20 4.00 -9 -1 28 3.10 2.70 -9 -1 28 8.00 2.70 9 1 28 19.20 4.40 9 -1 -28 8.90 3.10 9 -1 -28 7.50 2.90 -9 1 -28 4.20 2.50 -9 1 28 5.50 2.80 -9 1 28 1.60 2.10 -9 1 28 9.30 4.20 -9 -1 -28 5.30 2.70 9 -1 28 5.90 2.70 9 -1 28 6.70 3.20 9 1 -28 5.30 2.40 9 1 -28 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-29 78.79 7.70 -1 -3 29 75.49 18.90 -1 3 -29 73.09 8.10 1 -3 -29 48.30 14.90 1 3 29 70.59 9.50 -1 3 -29 80.39 8.80 1 -3 -29 83.69 7.90 1 3 29 80.99 8.10 1 -3 -29 91.29 8.20 -1 3 -29 69.29 8.10 -1 3 -29 72.19 9.00 1 3 -29 83.69 8.70 -1 -3 -29 86.69 8.10 -1 3 29 71.49 8.50 -1 3 29 76.79 8.70 1 -3 29 87.89 13.10 1 3 -29 76.59 7.70 1 3 -29 89.79 9.20 1 3 -29 88.99 10.40 1 3 -29 82.69 8.70 -1 3 29 83.19 8.90 -1 4 -29 31.20 5.60 1 4 29 21.20 6.30 1 -4 -29 28.10 4.30 1 4 29 20.00 5.60 1 -4 -29 25.90 4.60 -1 4 -29 25.20 6.10 -1 4 -29 27.70 5.60 -1 4 -29 37.10 6.20 1 -4 29 32.40 11.70 -1 -4 -29 16.80 4.20 -1 -4 -29 17.70 3.90 -1 4 29 31.80 5.20 -1 4 29 31.60 6.20 1 4 -29 22.30 6.10 1 4 -29 16.90 5.00 1 4 -29 30.90 5.90 1 4 -29 26.00 5.60 -1 5 -29 30.10 4.70 -1 5 -29 18.80 4.20 1 -5 -29 32.40 5.40 1 5 29 22.80 5.20 -1 5 -29 18.60 4.00 1 5 29 24.50 6.10 1 -5 -29 27.70 6.60 -1 5 -29 22.20 4.90 1 5 -29 21.60 4.50 -1 5 29 28.10 4.50 -1 5 29 32.70 5.80 1 5 -29 27.30 4.80 1 5 -29 28.10 4.60 -1 -5 -29 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-2 -49 8.90 2.30 3 -2 -49 9.60 2.20 -3 2 -49 13.70 2.60 -3 -2 49 13.90 2.20 -3 2 -49 9.70 2.20 3 2 -49 16.10 2.60 -3 -2 -49 14.30 2.40 3 -2 49 10.00 2.30 4 0 -49 62.79 5.60 -4 0 -49 69.49 5.40 -4 0 49 60.09 5.50 4 0 49 64.49 5.80 4 0 -49 66.49 5.70 -4 0 -49 58.69 5.50 -4 1 -49 2.00 1.90 4 -1 -49 2.90 2.00 4 -1 -49 4.20 1.60 -4 -1 49 0.40 1.80 4 1 49 0.70 1.50 4 -1 -49 2.80 2.40 4 1 -49 0.80 1.80 -4 1 49 2.10 1.60 -4 -1 -49 1.80 1.40 4 -1 49 -0.90 1.80 -4 -1 -49 2.60 1.70 -4 -1 -49 0.60 1.30 0 0 -50 40.20 4.60 0 0 50 46.90 5.30 0 0 -50 43.60 4.30 0 -1 -50 10.70 2.50 0 -1 -50 8.30 2.30 0 1 -50 12.90 2.90 0 1 50 7.70 2.80 0 -1 50 13.90 3.30 0 2 -50 0.80 1.80 0 -2 -50 -1.50 1.80 0 2 50 1.30 2.20 0 2 -50 0.80 1.70 0 -2 -50 2.10 2.10 1 0 -50 3.10 1.90 1 0 -50 -0.50 2.10 -1 0 50 -0.70 2.40 -1 0 -50 -2.40 1.60 1 0 50 -1.50 2.30 -1 0 -50 1.90 2.10 1 -1 -50 4.40 1.90 1 -1 -50 2.90 2.20 1 1 50 1.40 2.20 -1 1 -50 2.50 2.10 -1 -1 -50 2.70 2.20 -1 1 50 1.70 2.40 1 1 -50 1.30 2.30 -1 -1 -50 2.00 1.80 1 -1 50 4.60 2.40 1 -2 -50 10.20 2.40 -1 2 -50 18.10 2.40 -1 2 -50 10.60 2.30 1 2 50 13.20 2.60 1 2 -50 8.00 2.10 1 -2 50 5.40 2.30 -1 -2 -50 12.30 2.30 -1 2 50 12.10 3.00 1 2 -50 11.00 2.40 2 0 -50 14.70 2.70 -2 0 -50 13.10 2.60 -2 0 50 10.90 2.20 -2 0 50 10.50 3.10 2 0 50 17.60 3.40 2 0 -50 14.90 2.90 -2 0 -50 18.90 2.60 2 -1 -50 -1.00 1.80 -2 -1 50 -3.10 2.30 -2 1 -50 1.30 1.90 -2 -1 50 -2.20 1.60 2 1 50 0.70 2.00 2 -1 -50 3.10 2.10 -2 1 50 -0.90 2.40 2 -1 50 0.50 2.20 2 1 -50 0.30 2.00 -2 -1 -50 1.20 1.70 -2 -1 -50 1.30 1.70 2 -2 -50 2.70 1.80 -2 -2 50 0.40 1.30 -2 2 -50 2.20 1.70 2 -2 -50 1.10 1.80 -2 2 -50 5.40 2.00 2 2 50 2.20 1.90 -2 -2 -50 2.30 1.70 2 2 -50 -0.20 1.70 -2 -2 -50 -0.30 1.00 2 -2 50 3.10 1.80 -3 0 50 1.50 1.90 3 0 -50 1.90 2.00 3 0 -50 0.80 1.70 -3 0 -50 -1.50 1.70 3 0 50 0.20 2.00 -3 0 50 1.10 2.10 -3 0 -50 -0.80 1.90 -3 1 -50 2.80 1.90 3 -1 -50 0.70 1.80 3 -1 -50 2.80 2.20 3 -1 -50 2.70 1.60 3 1 50 0.70 1.80 -3 -1 50 -0.70 1.70 3 -1 50 0.80 1.90 3 1 -50 3.30 2.10 -3 1 50 0.50 1.60 -3 -1 -50 -2.10 1.40 -3 -1 -50 3.90 1.90 4 0 -50 13.60 2.60 -4 0 -50 15.00 2.00 -4 0 -50 17.60 2.60 -4 0 50 16.30 2.60 4 0 -50 13.10 2.80 4 0 -50 14.50 2.20 4 0 50 19.10 2.90 0 0 -51 2.10 1.80 0 0 -51 -0.40 1.80 0 0 51 0.60 2.00 0 -1 51 -2.20 2.10 0 1 51 -1.60 2.00 0 1 -51 -0.10 1.80 0 -1 -51 -0.70 2.00 0 -1 -51 0.90 2.10 0 2 -51 0.40 1.60 1 0 51 -2.90 1.90 -1 0 51 1.20 2.30 1 0 -51 -1.10 1.80 -1 0 -51 0.00 1.70 1 0 -51 -0.40 1.50 -1 0 -51 -1.90 1.40 -1 1 -51 -0.20 1.70 1 -1 -51 0.40 1.90 1 -1 -51 4.00 1.60 1 1 51 0.30 2.10 -1 -1 51 -1.10 1.90 -1 -1 -51 -0.30 1.60 -1 -1 -51 -1.10 1.60 1 1 -51 0.10 1.90 1 -1 51 1.20 2.30 -1 1 51 1.90 2.40 -2 0 51 0.00 2.10 2 0 51 -0.60 1.90 2 0 -51 2.50 1.60 2 0 -51 2.10 1.90 -2 0 -51 0.80 2.30 -2 0 -51 0.40 1.80 2 -1 -51 2.00 1.50 -2 -1 51 -0.80 1.80 -2 -1 51 1.80 2.10 2 -1 -51 -0.40 1.70 2 1 51 1.70 2.20 -2 1 -51 4.60 2.00 -2 -1 -51 1.30 1.60 -2 1 51 2.10 2.40 2 1 -51 -0.20 1.70 -2 -1 -51 1.80 1.50 -3 0 -51 0.20 1.60 -3 0 51 4.60 1.40 -3 0 51 1.50 2.00 3 0 -51 -0.70 1.80 3 0 -51 1.10 1.40 -3 0 -51 1.30 1.20 3 0 51 1.70 2.10 3 -1 -51 0.10 1.70 -3 -1 -51 -1.20 2.00 0 0 52 17.80 3.50 0 0 -52 17.60 2.60 0 0 -52 18.40 2.90 0 1 -52 23.80 3.20 0 -1 52 19.60 3.30 0 -1 -52 23.20 2.90 0 1 52 22.50 3.50 -1 0 -52 0.70 1.70 1 0 52 2.50 2.20 1 0 -52 -0.20 1.50 1 0 -52 -0.80 1.70 -1 0 52 -0.70 1.80 -1 0 -52 -0.30 1.30 1 -1 -52 1.00 1.70 -1 1 -52 2.80 2.00 1 1 52 1.20 2.00 -1 -1 52 5.70 1.90 1 -1 -52 3.70 1.50 1 1 -52 1.00 1.80 -1 -1 -52 2.20 1.80 -1 -1 -52 0.60 1.30 -1 1 52 4.00 2.40 1 -1 52 6.00 2.40 -2 0 52 1.90 2.20 -2 0 -52 0.70 1.50 2 0 -52 2.30 1.90 -2 0 -52 -2.50 1.10 2 0 52 1.00 1.90 2 0 -52 1.80 1.50 0 0 -53 0.10 1.70 0 0 -53 0.50 1.20 0 0 53 0.50 2.00 1 0 -53 1.40 1.10 1 0 -53 1.90 1.70 -1 0 53 -1.10 1.70 -1 0 -53 0.20 1.10 -1 0 -53 0.30 1.60 1 0 53 -0.90 1.80 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 92575 #============================================================================= # end of cif data for "glo9616" (compound 2f) #============================================================================= #============================================================================= # cif data for "glo9753" (compound 2q) #============================================================================= data_glo9753 _audit_creation_method 'APEX3 v2016.1-0' _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H21 N O3' _chemical_formula_iupac ? _chemical_formula_weight 215.29 _chemical_melting_point ? _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'P b c a' _space_group_name_Hall '-P 2ac 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.2362(3) _cell_length_b 10.9879(3) _cell_length_c 23.7378(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2409.06(12) _cell_formula_units_Z 8 _cell_measurement_reflns_used 9865 _cell_measurement_theta_min 3.7242 _cell_measurement_theta_max 67.2060 _cell_measurement_temperature 100.(2) _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.158 _exptl_crystal_size_mid 0.079 _exptl_crystal_size_min 0.075 _exptl_crystal_density_diffrn 1.187 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.693 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Bruker AXS (2014). SADABS, Version 2014/5, Bruker AXS Inc., Madison, Wisconsin, USA. ; _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.95 _exptl_special_details ; ; _diffrn_ambient_temperature 100.(2) _diffrn_source 'Cu ImS' _diffrn_source_type 'micro focus tube' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _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 7.3910 _diffrn_reflns_number 65017 _diffrn_reflns_av_R_equivalents 0.1021 _diffrn_reflns_av_unetI/netI 0.0293 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 66.59 _diffrn_reflns_theta_full 66.59 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _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 2113 _reflns_number_gt 1684 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_gt 0.1449 _refine_ls_wR_factor_ref 0.1549 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_number_reflns 2113 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+1.9585P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.317 _refine_diff_density_min -0.219 _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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ; APEX3 v2016.1-0 (Bruker AXS Inc., 2016) ; _computing_cell_refinement 'SAINT V8.37A (Bruker AXS Inc., 2015)' _computing_data_reduction 'SAINT V8.37A (Bruker AXS Inc., 2015)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'XP (Sheldrick, 2014)' _computing_publication_material 'SHELXL-2014/7 (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 N N1 0.5633(2) 0.70310(19) 0.61499(8) 0.0429(5) Uani d . . . 1 . . O O1 0.6579(2) 0.90576(18) 0.54405(8) 0.0542(5) Uani d . . . 1 . . H H1A 0.6958 0.9569 0.5658 0.081 Uiso calc U . R 1 . . O O2 0.7611(2) 0.57977(14) 0.62625(7) 0.0450(5) Uani d . . . 1 . . O O3 0.7430(2) 0.76166(14) 0.67146(7) 0.0420(4) Uani d . . . 1 . . C C1 0.4979(3) 0.6201(2) 0.57312(10) 0.0452(6) Uani d . . . 1 . . H H1 0.5584 0.5447 0.5716 0.054 Uiso calc U . R 1 . . C C2 0.5015(3) 0.6787(3) 0.51518(10) 0.0509(7) Uani d . . . 1 . . H H2A 0.6028 0.6809 0.5016 0.061 Uiso calc U . R 1 . . H H2B 0.4448 0.6281 0.4887 0.061 Uiso calc U . R 1 . . C C3 0.4409(4) 0.8071(3) 0.51511(11) 0.0551(7) Uani d . . . 1 . . H H3A 0.3352 0.8037 0.5217 0.066 Uiso calc U . R 1 . . H H3B 0.4572 0.8443 0.4776 0.066 Uiso calc U . R 1 . . C C4 0.5109(3) 0.8864(2) 0.56005(10) 0.0444(6) Uani d . . . 1 . . H H4 0.4596 0.9665 0.5617 0.053 Uiso calc U . R 1 . . C C5 0.5033(3) 0.8258(2) 0.61714(9) 0.0421(6) Uani d . . . 1 . . H H5A 0.5579 0.8749 0.6449 0.05 Uiso calc U . R 1 . . H H5B 0.4011 0.8219 0.6297 0.05 Uiso calc U . R 1 . . C C6 0.3458(3) 0.5835(3) 0.59117(12) 0.0577(8) Uani d . . . 1 . . H H6A 0.3491 0.5491 0.6292 0.087 Uiso calc U . R 1 . . H H6B 0.3077 0.5226 0.5649 0.087 Uiso calc U . R 1 . . H H6C 0.2829 0.6553 0.591 0.087 Uiso calc U . R 1 . . C C7 0.6951(3) 0.6752(2) 0.63583(9) 0.0391(6) Uani d . . . 1 . . C C8 0.8897(3) 0.7548(2) 0.69643(10) 0.0404(6) Uani d . . . 1 . . C C9 0.8958(4) 0.6481(2) 0.73676(11) 0.0542(7) Uani d . . . 1 . . H H9A 0.8157 0.6539 0.7637 0.081 Uiso calc U . R 1 . . H H9B 0.9881 0.6493 0.7571 0.081 Uiso calc U . R 1 . . H H9C 0.8876 0.5719 0.7155 0.081 Uiso calc U . R 1 . . C C10 1.0033(3) 0.7496(3) 0.65133(12) 0.0596(8) Uani d . . . 1 . . H H10A 1.0004 0.6699 0.6329 0.089 Uiso calc U . R 1 . . H H10B 1.099 0.7622 0.6682 0.089 Uiso calc U . R 1 . . H H10C 0.9848 0.8135 0.6234 0.089 Uiso calc U . R 1 . . C C11 0.8976(3) 0.8741(2) 0.72850(11) 0.0535(7) Uani d . . . 1 . . H H11A 0.8831 0.942 0.7023 0.08 Uiso calc U . R 1 . . H H11B 0.9928 0.8816 0.7464 0.08 Uiso calc U . R 1 . . H H11C 0.822 0.8757 0.7575 0.08 Uiso calc U . R 1 . . 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 N1 0.0501(13) 0.0412(11) 0.0373(10) 0.0051(10) -0.0100(10) -0.0079(8) O1 0.0574(12) 0.0592(12) 0.0461(10) -0.0099(10) 0.0087(9) -0.0143(8) O2 0.0554(11) 0.0362(9) 0.0433(9) 0.0047(8) -0.0067(8) -0.0052(7) O3 0.0492(10) 0.0391(9) 0.0377(9) 0.0041(8) -0.0129(8) -0.0067(7) C1 0.0468(16) 0.0440(14) 0.0450(13) 0.0012(12) -0.0101(12) -0.0148(11) C2 0.0556(17) 0.0587(17) 0.0385(13) -0.0092(14) 0.0025(13) -0.0133(12) C3 0.069(2) 0.0593(17) 0.0368(13) -0.0070(15) -0.0100(13) 0.0010(12) C4 0.0445(15) 0.0457(14) 0.0430(13) 0.0027(12) -0.0032(12) -0.0031(11) C5 0.0457(15) 0.0462(14) 0.0343(12) 0.0038(12) -0.0001(11) -0.0078(10) C6 0.0629(19) 0.0605(18) 0.0497(15) -0.0151(15) 0.0005(14) -0.0047(13) C7 0.0507(15) 0.0344(12) 0.0322(12) -0.0003(11) -0.0029(11) -0.0020(9) C8 0.0467(15) 0.0413(13) 0.0331(12) -0.0002(11) -0.0126(11) -0.0005(10) C9 0.072(2) 0.0456(15) 0.0452(15) 0.0011(13) -0.0159(14) 0.0061(11) C10 0.0556(19) 0.073(2) 0.0502(16) -0.0120(15) -0.0017(14) -0.0075(14) C11 0.0685(19) 0.0424(14) 0.0497(15) -0.0029(13) -0.0217(14) -0.0061(11) _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 N1 C7 . 1.350(3) ? N1 C5 . 1.459(3) ? N1 C1 . 1.478(3) ? O1 C4 . 1.425(3) ? O1 H1A . 0.84 ? O2 C7 . 1.234(3) ? O3 C7 . 1.346(3) ? O3 C8 . 1.481(3) ? C1 C2 . 1.519(4) ? C1 C6 . 1.522(4) ? C1 H1 . 1.0 ? C2 C3 . 1.517(4) ? C2 H2A . 0.99 ? C2 H2B . 0.99 ? C3 C4 . 1.522(4) ? C3 H3A . 0.99 ? C3 H3B . 0.99 ? C4 C5 . 1.512(3) ? C4 H4 . 1.0 ? C5 H5A . 0.99 ? C5 H5B . 0.99 ? C6 H6A . 0.98 ? C6 H6B . 0.98 ? C6 H6C . 0.98 ? C8 C10 . 1.500(4) ? C8 C9 . 1.515(3) ? C8 C11 . 1.518(3) ? C9 H9A . 0.98 ? C9 H9B . 0.98 ? C9 H9C . 0.98 ? C10 H10A . 0.98 ? C10 H10B . 0.98 ? C10 H10C . 0.98 ? C11 H11A . 0.98 ? C11 H11B . 0.98 ? C11 H11C . 0.98 ? 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 C7 N1 C5 . . 122.7(2) ? C7 N1 C1 . . 118.4(2) ? C5 N1 C1 . . 115.99(19) ? C4 O1 H1A . . 109.5 ? C7 O3 C8 . . 121.04(19) ? N1 C1 C2 . . 109.8(2) ? N1 C1 C6 . . 110.5(2) ? C2 C1 C6 . . 112.8(2) ? N1 C1 H1 . . 107.9 ? C2 C1 H1 . . 107.9 ? C6 C1 H1 . . 107.9 ? C3 C2 C1 . . 112.8(2) ? C3 C2 H2A . . 109.0 ? C1 C2 H2A . . 109.0 ? C3 C2 H2B . . 109.0 ? C1 C2 H2B . . 109.0 ? H2A C2 H2B . . 107.8 ? C2 C3 C4 . . 112.0(2) ? C2 C3 H3A . . 109.2 ? C4 C3 H3A . . 109.2 ? C2 C3 H3B . . 109.2 ? C4 C3 H3B . . 109.2 ? H3A C3 H3B . . 107.9 ? O1 C4 C5 . . 110.4(2) ? O1 C4 C3 . . 107.6(2) ? C5 C4 C3 . . 110.9(2) ? O1 C4 H4 . . 109.3 ? C5 C4 H4 . . 109.3 ? C3 C4 H4 . . 109.3 ? N1 C5 C4 . . 110.98(19) ? N1 C5 H5A . . 109.4 ? C4 C5 H5A . . 109.4 ? N1 C5 H5B . . 109.4 ? C4 C5 H5B . . 109.4 ? H5A C5 H5B . . 108.0 ? C1 C6 H6A . . 109.5 ? C1 C6 H6B . . 109.5 ? H6A C6 H6B . . 109.5 ? C1 C6 H6C . . 109.5 ? H6A C6 H6C . . 109.5 ? H6B C6 H6C . . 109.5 ? O2 C7 O3 . . 123.6(2) ? O2 C7 N1 . . 124.8(2) ? O3 C7 N1 . . 111.5(2) ? O3 C8 C10 . . 110.87(19) ? O3 C8 C9 . . 109.1(2) ? C10 C8 C9 . . 113.3(2) ? O3 C8 C11 . . 101.6(2) ? C10 C8 C11 . . 110.9(2) ? C9 C8 C11 . . 110.5(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 C10 H10A . . 109.5 ? C8 C10 H10B . . 109.5 ? H10A C10 H10B . . 109.5 ? C8 C10 H10C . . 109.5 ? H10A C10 H10C . . 109.5 ? H10B C10 H10C . . 109.5 ? C8 C11 H11A . . 109.5 ? C8 C11 H11B . . 109.5 ? H11A C11 H11B . . 109.5 ? C8 C11 H11C . . 109.5 ? H11A C11 H11C . . 109.5 ? H11B C11 H11C . . 109.5 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C7 N1 C1 C2 . . . . -107.4(3) ? C5 N1 C1 C2 . . . . 53.8(3) ? C7 N1 C1 C6 . . . . 127.6(3) ? C5 N1 C1 C6 . . . . -71.3(3) ? N1 C1 C2 C3 . . . . -50.4(3) ? C6 C1 C2 C3 . . . . 73.3(3) ? C1 C2 C3 C4 . . . . 51.9(3) ? C2 C3 C4 O1 . . . . 68.4(3) ? C2 C3 C4 C5 . . . . -52.5(3) ? C7 N1 C5 C4 . . . . 104.2(3) ? C1 N1 C5 C4 . . . . -56.0(3) ? O1 C4 C5 N1 . . . . -65.8(3) ? C3 C4 C5 N1 . . . . 53.4(3) ? C8 O3 C7 O2 . . . . 8.0(3) ? C8 O3 C7 N1 . . . . -175.7(2) ? C5 N1 C7 O2 . . . . -166.3(2) ? C1 N1 C7 O2 . . . . -6.5(4) ? C5 N1 C7 O3 . . . . 17.5(3) ? C1 N1 C7 O3 . . . . 177.3(2) ? C7 O3 C8 C10 . . . . 57.6(3) ? C7 O3 C8 C9 . . . . -67.9(3) ? C7 O3 C8 C11 . . . . 175.5(2) ? _shelx_res_file ; glo9753.res created by SHELXL-2014/7 TITL glo9753.res in Pbca CELL 1.54178 9.2362 10.9879 23.7378 90.000 90.000 90.000 ZERR 8.000 0.0003 0.0003 0.0007 0.000 0.000 0.000 LATT 1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H N O UNIT 88 168 8 24 SIZE 0.075 0.079 0.158 TEMP -173.150 ACTA CONF L.S. 20 BOND $H FMAP 2 PLAN 10 HTAB OMIT 2 2 6 OMIT 1 2 6 OMIT 1 2 8 OMIT 2 5 0 OMIT 3 1 2 WGHT 0.062200 1.958500 FVAR 0.45944 N1 3 0.563299 0.703096 0.614988 11.00000 0.05009 0.04115 = 0.03733 -0.00790 -0.01003 0.00515 O1 4 0.657870 0.905759 0.544048 11.00000 0.05736 0.05920 = 0.04614 -0.01426 0.00867 -0.00989 AFIX 147 H1A 2 0.695837 0.956887 0.565817 11.00000 -1.50000 AFIX 0 O2 4 0.761080 0.579772 0.626247 11.00000 0.05537 0.03619 = 0.04332 -0.00522 -0.00668 0.00469 O3 4 0.742988 0.761659 0.671463 11.00000 0.04919 0.03908 = 0.03771 -0.00666 -0.01293 0.00409 C1 1 0.497863 0.620125 0.573125 11.00000 0.04679 0.04400 = 0.04495 -0.01476 -0.01011 0.00116 AFIX 13 H1 2 0.558359 0.544718 0.571623 11.00000 -1.20000 AFIX 0 C2 1 0.501501 0.678735 0.515181 11.00000 0.05560 0.05871 = 0.03845 -0.01327 0.00254 -0.00915 AFIX 23 H2A 2 0.602795 0.680854 0.501579 11.00000 -1.20000 H2B 2 0.444783 0.628137 0.488652 11.00000 -1.20000 AFIX 0 C3 1 0.440949 0.807064 0.515106 11.00000 0.06907 0.05932 = 0.03682 0.00099 -0.00996 -0.00695 AFIX 23 H3A 2 0.335200 0.803708 0.521735 11.00000 -1.20000 H3B 2 0.457163 0.844250 0.477646 11.00000 -1.20000 AFIX 0 C4 1 0.510929 0.886414 0.560048 11.00000 0.04448 0.04568 = 0.04303 -0.00307 -0.00317 0.00266 AFIX 13 H4 2 0.459641 0.966485 0.561697 11.00000 -1.20000 AFIX 0 C5 1 0.503253 0.825809 0.617137 11.00000 0.04567 0.04624 = 0.03429 -0.00782 -0.00007 0.00379 AFIX 23 H5A 2 0.557922 0.874891 0.644899 11.00000 -1.20000 H5B 2 0.401116 0.821922 0.629658 11.00000 -1.20000 AFIX 0 C6 1 0.345849 0.583536 0.591168 11.00000 0.06289 0.06051 = 0.04973 -0.00473 0.00053 -0.01515 AFIX 137 H6A 2 0.349082 0.549103 0.629231 11.00000 -1.50000 H6B 2 0.307687 0.522617 0.564924 11.00000 -1.50000 H6C 2 0.282896 0.655330 0.590967 11.00000 -1.50000 AFIX 0 C7 1 0.695145 0.675237 0.635834 11.00000 0.05071 0.03441 = 0.03216 -0.00204 -0.00288 -0.00033 C8 1 0.889721 0.754752 0.696431 11.00000 0.04674 0.04126 = 0.03312 -0.00053 -0.01257 -0.00025 C9 1 0.895795 0.648057 0.736762 11.00000 0.07185 0.04558 = 0.04516 0.00610 -0.01595 0.00107 AFIX 137 H9A 2 0.815696 0.653948 0.763699 11.00000 -1.50000 H9B 2 0.988054 0.649316 0.757144 11.00000 -1.50000 H9C 2 0.887564 0.571872 0.715536 11.00000 -1.50000 AFIX 0 C10 1 1.003306 0.749613 0.651329 11.00000 0.05558 0.07314 = 0.05019 -0.00750 -0.00171 -0.01198 AFIX 137 H10A 2 1.000392 0.669858 0.632885 11.00000 -1.50000 H10B 2 1.098970 0.762163 0.668216 11.00000 -1.50000 H10C 2 0.984764 0.813461 0.623420 11.00000 -1.50000 AFIX 0 C11 1 0.897616 0.874061 0.728496 11.00000 0.06848 0.04241 = 0.04975 -0.00609 -0.02168 -0.00292 AFIX 137 H11A 2 0.883136 0.941972 0.702333 11.00000 -1.50000 H11B 2 0.992797 0.881562 0.746407 11.00000 -1.50000 H11C 2 0.822014 0.875692 0.757453 11.00000 -1.50000 AFIX 0 HKLF 4 REM glo9753.res in Pbca REM R1 = 0.0590 for 1684 Fo > 4sig(Fo) and 0.0744 for all 2113 data REM 141 parameters refined using 0 restraints END WGHT 0.0622 1.9577 REM Instructions for potential hydrogen bonds EQIV $1 -x+3/2, y+1/2, z HTAB O1 O2_$1 HTAB C9 O2 HTAB C10 O2 REM Highest difference peak 0.317, deepest hole -0.219, 1-sigma level 0.045 Q1 1 0.7623 0.9219 0.6282 11.00000 0.05 0.32 Q2 1 0.6524 0.5900 0.5426 11.00000 0.05 0.29 Q3 1 0.3464 0.9103 0.5907 11.00000 0.05 0.27 Q4 1 0.8397 0.7715 0.6314 11.00000 0.05 0.18 Q5 1 0.8788 0.8828 0.6155 11.00000 0.05 0.18 Q6 1 0.6897 0.8321 0.6363 11.00000 0.05 0.18 Q7 1 0.9126 0.8729 0.6171 11.00000 0.05 0.18 Q8 1 0.6764 0.7381 0.5724 11.00000 0.05 0.17 Q9 1 0.7507 0.6815 0.6893 11.00000 0.05 0.16 Q10 1 0.7155 0.5246 0.5864 11.00000 0.05 0.16 ; _shelx_res_checksum 87951 _shelx_hkl_file ; 1 0 0 -0.10 3.20 1 0 0 -4.30 2.70 1 0 0 -4.40 1.00 1 0 0 -3.70 3.10 -1 0 0 -5.80 2.40 -1 0 0 -2.80 3.00 1 0 0 0.60 3.80 -1 0 0 -4.30 1.00 -1 0 0 -5.60 2.10 -1 0 0 -6.20 3.30 -2 0 0 3351.46 305.67 -2 0 0 3620.24 305.77 -2 0 0 3333.37 303.97 -2 0 0 3084.99 303.57 -2 0 0 3657.23 304.57 2 0 0 3492.75 304.47 -2 0 0 3802.02 306.17 2 0 0 3685.23 305.77 2 0 0 3685.33 305.87 2 0 0 3479.85 305.97 2 0 0 3662.73 304.47 3 0 0 1.80 6.60 3 0 0 -4.90 6.60 -3 0 0 -3.90 5.70 3 0 0 -3.20 7.10 3 0 0 5.30 5.60 -3 0 0 -8.60 7.50 -3 0 0 -4.10 5.20 -3 0 0 0.60 4.80 -3 0 0 0.60 3.90 3 0 0 5.40 4.60 -3 0 0 -0.80 6.90 -3 0 0 0.50 1.90 -4 0 0 1739.53 159.88 4 0 0 1709.63 154.98 -4 0 0 1801.02 155.58 -4 0 0 1857.61 155.88 -4 0 0 1832.92 159.58 -4 0 0 1827.12 156.68 4 0 0 1727.03 156.18 4 0 0 1841.02 156.58 4 0 0 1871.61 159.68 -4 0 0 1737.83 159.38 4 0 0 1764.42 159.98 5 0 0 -0.60 7.60 5 0 0 0.40 8.00 5 0 0 -4.00 4.90 -5 0 0 -2.70 5.80 -5 0 0 -3.90 6.10 5 0 0 -0.70 3.90 -5 0 0 -7.60 6.00 -5 0 0 -1.30 7.60 -5 0 0 -6.20 4.80 -5 0 0 -6.00 7.70 -5 0 0 -4.00 6.50 5 0 0 2.60 3.20 5 0 0 -3.00 6.50 5 0 0 -1.10 5.80 -6 0 0 70.89 12.90 -6 0 0 93.59 11.30 6 0 0 70.79 13.60 6 0 0 112.99 10.70 -6 0 0 78.79 10.00 -6 0 0 100.69 11.40 -6 0 0 94.69 12.20 6 0 0 101.19 9.80 6 0 0 88.49 12.10 7 0 0 5.90 7.20 7 0 0 9.80 10.80 -7 0 0 -0.40 5.80 -7 0 0 4.40 6.00 -7 0 0 0.20 4.50 -7 0 0 -0.50 6.20 -7 0 0 -3.50 6.80 7 0 0 -0.60 4.50 7 0 0 -2.40 3.70 -8 0 0 451.45 40.80 -8 0 0 421.36 42.30 8 0 0 454.65 40.10 -9 0 0 5.30 5.00 -9 0 0 -2.20 7.30 9 0 0 -1.80 5.10 9 0 0 -0.40 8.70 9 0 0 -3.10 3.90 -9 0 0 3.90 9.20 9 0 0 -3.90 9.10 9 0 0 2.10 4.50 -10 0 0 33.20 5.10 10 0 0 18.90 5.80 -10 0 0 16.30 5.20 10 0 0 19.50 4.60 0 -1 0 -15.60 1.40 0 -1 0 -13.70 2.10 0 1 0 -13.30 1.60 0 1 0 -14.50 2.70 0 1 0 -14.20 3.10 0 -1 0 -15.80 3.20 0 -1 0 -14.80 2.50 -1 -1 0 -4.30 2.50 1 -1 0 -1.60 3.50 1 -1 0 -3.50 3.90 1 -1 0 -3.90 4.10 -1 -1 0 -2.80 4.20 1 -1 0 -3.50 3.30 1 1 0 -2.10 4.10 -1 -1 0 -3.00 4.10 1 1 0 -4.90 2.80 -1 -1 0 -2.30 2.90 1 1 0 -2.00 2.90 -1 1 0 -0.90 3.70 1 -1 0 -1.50 4.50 -1 1 0 -3.40 1.80 -1 -1 0 0.40 4.10 -1 1 0 -1.80 3.60 1 1 0 -4.00 4.30 -1 1 0 -3.50 4.00 1 1 0 -3.80 2.60 -1 -1 0 2.10 2.10 1 1 0 -1.40 4.10 -2 -1 0 757.62 69.99 2 -1 0 808.72 68.29 -2 -1 0 713.43 67.69 -2 1 0 817.42 70.29 2 -1 0 782.32 69.89 2 1 0 732.03 67.69 2 1 0 810.82 69.99 2 1 0 714.73 67.79 -2 -1 0 851.21 68.29 2 1 0 766.82 69.89 2 -1 0 812.92 70.09 2 -1 0 819.42 68.29 -2 -1 0 784.62 70.09 -2 -1 0 796.92 69.89 -2 1 0 755.52 68.09 -2 1 0 771.42 69.89 -2 -1 0 743.03 67.89 2 1 0 779.62 70.29 -2 1 0 765.32 67.29 -2 1 0 808.42 68.69 2 -1 0 793.32 69.79 -2 1 0 785.02 69.99 -3 -1 0 -3.50 4.90 3 1 0 4.70 7.40 -3 -1 0 -2.20 5.00 3 1 0 -4.40 7.70 -3 1 0 1.50 5.40 3 -1 0 0.80 6.60 -3 -1 0 2.40 5.20 -3 -1 0 1.90 7.00 3 -1 0 -1.10 3.30 3 1 0 -1.80 3.30 -3 1 0 0.60 5.40 3 1 0 0.20 3.30 -3 -1 0 -0.10 5.50 3 -1 0 0.10 7.70 -3 -1 0 -1.10 5.60 3 1 0 0.70 5.60 -3 -1 0 -8.80 5.60 -3 1 0 4.70 6.00 3 1 0 -2.90 3.20 3 1 0 -2.90 4.90 -3 1 0 4.00 6.70 3 -1 0 -2.60 5.40 3 -1 0 1.70 7.30 3 -1 0 -6.30 5.30 -3 1 0 -2.70 6.80 -3 1 0 1.40 6.90 4 1 0 204.68 20.30 4 -1 0 187.58 22.60 -4 1 0 194.38 18.80 4 1 0 196.78 23.80 -4 -1 0 199.18 18.20 -4 1 0 176.38 23.10 4 1 0 196.48 19.70 4 1 0 194.18 18.10 -4 -1 0 190.18 22.90 -4 1 0 195.68 22.40 -4 -1 0 187.58 19.60 -4 1 0 192.68 19.30 -4 1 0 190.28 20.40 4 -1 0 185.78 19.40 4 -1 0 173.18 23.30 -4 -1 0 199.58 22.70 4 -1 0 171.58 17.80 -4 -1 0 194.48 18.50 4 -1 0 189.38 19.80 4 1 0 205.18 22.90 4 -1 0 178.08 22.30 -4 1 0 200.48 23.10 5 1 0 9.30 8.10 5 1 0 -5.80 7.70 -5 1 0 -1.50 5.40 5 1 0 0.70 4.00 5 -1 0 -1.50 3.20 -5 -1 0 -6.20 8.70 -5 1 0 0.70 6.80 5 1 0 -9.40 7.40 -5 -1 0 -0.70 4.80 -5 1 0 5.20 9.10 5 1 0 1.40 3.20 5 -1 0 -12.00 6.10 -5 1 0 -2.00 8.60 5 -1 0 -8.70 7.10 5 1 0 0.60 6.30 -5 1 0 1.10 4.30 5 -1 0 4.10 7.90 5 -1 0 3.30 4.40 -5 -1 0 -10.80 4.40 -5 -1 0 -1.00 5.10 5 -1 0 1.20 8.40 -5 -1 0 5.00 4.80 5 -1 0 5.90 8.80 5 1 0 -0.10 6.90 -5 -1 0 1.30 7.70 6 1 0 358.66 33.60 6 -1 0 321.77 28.20 6 1 0 255.07 30.00 6 1 0 323.17 28.10 -6 -1 0 312.37 28.90 -6 1 0 318.77 29.90 6 -1 0 244.98 30.50 6 1 0 327.47 27.40 -6 1 0 290.47 28.10 -6 1 0 323.67 29.60 6 -1 0 320.97 27.50 6 -1 0 304.57 30.30 -6 1 0 271.27 31.10 -6 -1 0 320.27 29.30 -6 1 0 301.67 29.60 -6 -1 0 282.37 29.40 -6 -1 0 264.07 27.70 7 -1 0 -2.70 3.90 -7 1 0 0.50 8.90 -7 -1 0 2.60 3.50 -7 1 0 -4.10 7.20 -7 -1 0 -6.50 6.80 -7 -1 0 9.60 5.60 -7 -1 0 0.50 8.20 7 -1 0 -6.40 8.00 7 1 0 7.70 10.20 7 1 0 20.40 11.90 -7 -1 0 -8.30 6.50 -7 -1 0 0.70 6.90 7 1 0 -3.50 4.00 -7 1 0 0.40 7.80 7 -1 0 0.90 8.40 7 -1 0 -5.00 4.60 -7 1 0 -2.90 4.80 7 1 0 8.90 4.20 8 -1 0 39.50 6.20 -8 1 0 22.90 10.60 -8 -1 0 5.30 7.10 -8 -1 0 3.10 8.80 8 -1 0 8.90 9.50 8 1 0 9.40 10.40 -8 -1 0 13.00 5.70 -8 -1 0 52.29 11.70 8 -1 0 27.20 10.70 -8 1 0 28.60 11.10 8 -1 0 18.30 6.10 8 1 0 39.90 13.30 9 -1 0 5.20 3.50 9 1 0 0.70 8.70 -9 -1 0 -3.50 4.90 -9 -1 0 2.10 4.70 -9 -1 0 15.10 5.70 9 1 0 -3.70 4.90 9 -1 0 0.30 6.10 9 -1 0 4.40 5.10 -9 1 0 0.50 8.00 9 1 0 0.20 8.80 9 1 0 -3.00 3.90 9 -1 0 4.50 8.50 -9 1 0 -3.50 4.60 9 1 0 8.20 4.30 -9 1 0 6.30 7.10 -10 -1 0 3.60 3.80 10 1 0 -3.20 2.70 10 -1 0 8.20 4.10 -10 1 0 3.70 3.50 -10 1 0 -4.50 5.00 -10 -1 0 0.50 4.30 -10 1 0 0.20 7.20 10 -1 0 2.50 3.30 -10 -1 0 1.30 4.80 10 1 0 2.00 3.50 10 1 0 1.50 4.10 10 -1 0 -0.40 3.70 0 -2 0 9699.23 833.32 0 -2 0 9999.00 833.32 0 2 0 9399.16 833.22 0 2 0 9600.74 833.22 -1 2 0 1.00 3.80 -1 2 0 5.40 5.80 1 2 0 -1.30 5.10 1 -2 0 -0.60 4.60 -1 -2 0 0.20 5.50 1 2 0 -2.20 5.00 1 2 0 -0.10 3.10 -1 2 0 3.60 5.20 -1 -2 0 3.70 3.90 1 -2 0 3.70 4.30 1 -2 0 -1.10 5.40 -1 2 0 -0.70 5.10 -1 2 0 -0.90 5.40 1 -2 0 -1.50 6.10 1 2 0 -1.70 5.40 -1 -2 0 4.50 4.50 -1 -2 0 2.30 5.40 1 -2 0 -0.10 4.30 1 2 0 0.40 5.30 -1 2 0 1.50 4.40 -2 2 0 2110.69 173.28 -2 -2 0 1856.21 170.38 -2 -2 0 2046.60 170.48 -2 -2 0 1982.00 170.38 -2 2 0 2111.19 171.58 -2 2 0 1955.30 170.38 -2 -2 0 1996.60 172.88 2 -2 0 2092.59 173.18 2 2 0 1760.62 170.18 2 2 0 1801.22 170.38 2 -2 0 2008.20 170.68 2 2 0 2045.50 172.98 -2 2 0 1978.60 173.08 2 2 0 2052.59 173.18 -2 -2 0 1864.91 170.48 2 -2 0 2076.59 173.18 -2 -2 0 2017.70 172.88 -2 2 0 1862.61 170.38 -2 2 0 2058.09 172.98 2 2 0 1919.81 170.58 -2 2 0 1952.60 170.68 -2 -2 0 1980.80 172.68 -2 -2 0 2055.19 170.68 2 2 0 1989.40 172.88 2 -2 0 1850.31 170.18 -2 -2 0 1965.90 169.98 2 -2 0 1969.10 170.78 -3 -2 0 -1.90 5.40 3 2 0 -1.30 6.30 -3 2 0 16.10 3.80 -3 2 0 14.50 5.60 3 -2 0 4.70 6.10 3 2 0 -2.00 4.20 -3 -2 0 1.10 4.00 -3 2 0 5.70 6.70 3 2 0 2.20 3.30 -3 -2 0 3.10 2.80 -3 2 0 0.00 2.30 -3 2 0 5.80 6.50 3 2 0 2.20 7.40 -3 2 0 14.00 8.30 -3 -2 0 2.80 5.20 -3 2 0 -0.80 5.60 3 -2 0 8.10 7.10 3 2 0 3.70 4.30 3 -2 0 6.50 5.80 -3 -2 0 -4.10 5.50 -3 2 0 5.50 7.80 3 -2 0 0.60 5.40 3 -2 0 1.30 4.50 -3 -2 0 7.40 5.90 -3 -2 0 5.30 4.50 -3 -2 0 1.00 7.30 3 2 0 9.50 7.20 3 -2 0 4.00 6.50 -3 -2 0 2.80 5.90 4 2 0 537.25 49.50 4 2 0 585.44 54.49 4 -2 0 523.85 48.90 -4 2 0 553.84 54.89 -4 -2 0 559.04 54.19 4 2 0 504.25 48.90 -4 -2 0 554.04 54.39 4 2 0 559.74 54.19 4 2 0 560.94 49.30 4 2 0 577.94 51.19 -4 2 0 563.44 51.79 4 -2 0 589.24 54.79 -4 -2 0 564.94 50.19 4 -2 0 562.04 54.09 -4 2 0 567.64 50.49 4 2 0 557.24 55.39 -4 2 0 590.84 55.09 -4 2 0 527.05 54.29 4 -2 0 601.84 50.89 4 -2 0 573.54 54.49 -4 -2 0 550.34 49.40 4 -2 0 572.74 50.59 5 2 0 5.40 4.10 -5 -2 0 11.00 6.80 5 -2 0 13.10 8.50 5 -2 0 7.30 9.20 5 -2 0 4.40 7.50 5 -2 0 11.60 13.80 -5 2 0 12.20 9.50 -5 2 0 23.30 7.20 5 2 0 15.20 9.70 5 2 0 4.80 9.40 5 -2 0 12.80 5.80 -5 -2 0 -0.70 5.50 -5 2 0 18.90 8.00 -5 2 0 2.90 6.10 5 -2 0 14.60 4.10 -5 -2 0 12.10 4.10 -5 -2 0 10.60 4.60 5 -2 0 5.80 7.40 -5 2 0 -3.20 9.10 -5 -2 0 10.90 6.60 5 2 0 11.00 4.60 5 2 0 18.60 10.10 5 2 0 8.40 8.90 5 2 0 9.20 4.30 6 -2 0 67.09 7.60 -6 -2 0 63.99 10.20 -6 2 0 84.29 11.80 6 2 0 37.50 8.10 -6 2 0 66.19 10.20 6 2 0 67.59 8.10 6 2 0 74.79 11.30 -6 -2 0 57.39 8.80 6 2 0 41.60 12.30 6 -2 0 68.69 9.30 6 2 0 61.39 7.50 -6 2 0 63.69 9.50 -6 2 0 65.09 12.70 -6 -2 0 56.09 10.30 6 -2 0 69.19 17.00 6 -2 0 58.79 10.00 -6 -2 0 61.59 9.20 6 -2 0 62.09 8.90 -7 -2 0 2.50 14.80 -7 -2 0 11.50 7.20 7 -2 0 -1.20 8.40 -7 2 0 2.90 3.90 -7 2 0 -8.20 8.10 7 -2 0 4.40 4.50 7 -2 0 -0.50 7.50 -7 -2 0 -0.70 4.70 7 -2 0 1.30 3.90 -7 2 0 3.40 10.50 7 2 0 -2.30 5.40 7 2 0 7.50 11.00 7 2 0 -1.70 4.70 7 2 0 6.60 9.20 -7 -2 0 0.90 7.70 7 -2 0 2.00 6.40 7 2 0 1.00 4.20 -7 2 0 -1.50 5.00 -7 -2 0 4.10 6.00 8 2 0 22.60 6.80 8 2 0 27.20 13.10 -8 -2 0 19.80 6.60 8 -2 0 6.90 4.40 -8 2 0 1.10 9.40 8 2 0 30.00 6.80 8 -2 0 32.20 8.40 8 2 0 36.20 6.20 8 -2 0 3.30 7.90 -8 2 0 15.90 7.30 8 -2 0 23.00 11.90 8 -2 0 16.50 5.20 8 2 0 -2.80 9.20 -8 2 0 26.80 5.80 -8 -2 0 29.20 10.00 -8 -2 0 16.50 8.70 9 2 0 -2.50 3.40 9 2 0 -3.00 7.20 9 2 0 -3.30 4.40 9 -2 0 -0.20 5.20 9 -2 0 -3.90 3.90 -9 -2 0 -0.30 6.60 -9 -2 0 -3.10 4.80 -9 2 0 1.30 5.10 9 -2 0 0.90 4.30 -9 2 0 -1.60 10.80 9 2 0 4.60 8.70 -9 2 0 -0.30 5.40 9 2 0 -0.90 4.20 -9 -2 0 -3.10 4.60 -10 2 0 -12.80 8.00 10 -2 0 27.20 3.90 10 2 0 31.40 4.60 10 -2 0 13.80 5.20 10 -2 0 30.30 6.60 10 2 0 32.40 5.40 -10 2 0 14.70 4.70 -10 2 0 5.70 3.00 -10 -2 0 12.10 5.00 10 2 0 30.30 4.60 0 -3 0 11.90 5.70 0 3 0 -2.40 6.40 0 -3 0 -2.50 6.50 0 -3 0 4.00 5.60 0 3 0 1.70 6.10 0 -3 0 0.20 5.00 0 3 0 6.50 4.10 0 3 0 -5.40 6.40 0 3 0 5.80 6.90 -1 -3 0 0.90 6.30 1 3 0 -5.80 5.60 1 -3 0 0.40 3.60 -1 3 0 -7.10 6.60 1 3 0 -1.60 5.80 1 3 0 -2.90 6.00 -1 -3 0 -5.00 6.20 1 -3 0 -6.70 6.50 -1 3 0 -2.50 5.20 -1 3 0 -1.10 2.70 1 -3 0 2.30 5.70 -1 3 0 -2.00 6.20 1 -3 0 -1.70 4.20 -1 -3 0 1.00 5.50 1 3 0 -3.90 4.40 -1 -3 0 -0.50 5.40 -1 3 0 -3.20 5.80 1 3 0 -4.50 4.00 1 -3 0 -0.90 3.60 1 3 0 -1.90 5.80 -1 -3 0 -6.10 4.60 1 3 0 -6.10 6.40 2 3 0 119.69 17.10 2 3 0 109.19 11.00 -2 -3 0 111.39 15.70 2 3 0 113.19 12.40 2 3 0 105.09 15.70 -2 -3 0 116.29 12.90 2 -3 0 106.79 11.30 2 -3 0 129.49 12.20 2 -3 0 109.39 12.10 2 -3 0 118.99 11.90 -2 3 0 114.99 16.00 2 -3 0 122.29 15.90 -2 -3 0 115.19 11.30 -2 -3 0 113.69 16.50 -2 -3 0 101.99 12.30 -2 -3 0 113.49 10.80 -2 3 0 110.49 11.60 -2 3 0 113.99 12.00 2 -3 0 125.29 16.40 -2 3 0 123.09 16.90 -2 3 0 116.19 15.80 -2 3 0 106.19 11.10 2 3 0 125.59 15.90 -2 3 0 109.79 13.10 2 3 0 90.99 11.60 -2 3 0 107.19 11.40 2 3 0 111.09 12.30 -2 -3 0 115.39 11.50 -2 3 0 114.59 11.70 -2 -3 0 112.09 11.00 3 3 0 -1.10 6.00 3 -3 0 -10.00 7.00 -3 -3 0 -0.20 4.30 3 3 0 0.60 5.20 -3 3 0 -3.30 8.10 3 3 0 -3.00 7.40 -3 -3 0 1.80 6.40 -3 -3 0 -2.10 4.70 3 3 0 -7.50 5.30 -3 3 0 -0.90 3.50 -3 3 0 2.10 4.70 -3 -3 0 -1.40 7.00 -3 3 0 6.90 5.20 -3 3 0 2.60 6.40 -3 -3 0 3.70 3.10 -3 -3 0 3.50 6.50 -3 -3 0 6.10 5.70 -3 3 0 4.50 3.10 3 -3 0 -1.00 6.50 -3 -3 0 3.20 5.60 3 -3 0 1.20 6.70 -3 3 0 5.70 5.00 -3 -3 0 3.10 6.50 3 3 0 -0.10 6.20 -3 3 0 4.30 6.80 3 -3 0 -2.20 5.20 -4 3 0 -0.30 8.90 4 -3 0 3.80 5.80 -4 -3 0 4.70 4.90 4 3 0 0.80 6.00 4 3 0 8.30 4.30 -4 -3 0 0.70 2.90 4 3 0 -1.70 6.00 4 3 0 -1.70 8.10 4 -3 0 -1.50 6.00 4 -3 0 2.30 3.40 4 3 0 2.10 4.20 4 -3 0 10.50 7.50 -4 -3 0 0.00 4.60 -4 -3 0 2.40 4.80 -4 -3 0 7.60 6.50 4 3 0 -2.20 7.70 -4 3 0 2.20 7.10 -4 -3 0 -7.40 7.80 -4 3 0 2.60 5.90 4 3 0 0.10 5.20 -4 -3 0 5.30 6.70 -4 3 0 1.60 5.20 4 -3 0 3.80 9.10 4 -3 0 0.30 4.00 4 3 0 3.10 6.80 5 -3 0 -6.60 6.40 5 -3 0 2.40 3.50 -5 -3 0 6.20 7.30 -5 3 0 -2.80 3.90 -5 -3 0 -3.70 2.60 5 -3 0 5.50 6.80 5 3 0 0.20 4.00 -5 3 0 3.90 9.10 5 3 0 -16.00 7.40 -5 -3 0 7.00 5.20 5 3 0 4.10 3.90 5 3 0 -3.00 3.30 5 -3 0 4.30 9.40 -5 -3 0 -5.10 5.30 -5 3 0 -13.60 6.60 -5 3 0 10.10 7.40 -5 -3 0 -0.90 4.60 5 3 0 -6.10 8.90 -5 3 0 0.20 3.50 -5 -3 0 1.80 4.40 -5 -3 0 -2.70 6.20 5 -3 0 4.50 7.90 5 3 0 -2.30 6.10 5 3 0 4.80 5.30 5 -3 0 1.80 5.10 -6 -3 0 52.49 9.90 -6 -3 0 55.39 8.30 6 3 0 23.30 12.40 6 3 0 51.89 7.10 -6 3 0 32.90 9.20 -6 -3 0 39.50 10.30 6 3 0 50.09 6.50 6 -3 0 50.99 8.30 6 3 0 38.80 12.30 6 3 0 37.20 7.80 -6 3 0 40.80 14.40 -6 -3 0 44.60 9.90 6 -3 0 46.80 6.70 -6 3 0 37.80 7.10 6 -3 0 52.59 12.40 6 -3 0 50.99 11.90 6 -3 0 46.70 7.80 7 3 0 -2.10 9.90 -7 3 0 4.70 10.60 7 3 0 -2.80 5.70 7 3 0 7.70 5.30 -7 -3 0 2.40 3.70 7 -3 0 -8.20 5.90 7 -3 0 -3.80 3.10 7 -3 0 -2.40 12.80 7 3 0 -0.30 3.90 7 3 0 -3.40 8.90 -7 -3 0 2.30 8.10 7 -3 0 -0.60 4.20 7 -3 0 0.70 10.70 -7 3 0 -2.50 10.60 -7 3 0 -0.20 3.90 -7 -3 0 7.40 8.70 -7 -3 0 3.10 5.30 -7 3 0 2.60 7.00 8 -3 0 65.69 8.00 8 -3 0 65.49 11.00 8 -3 0 42.40 13.20 8 3 0 46.60 9.30 8 3 0 71.99 11.50 8 3 0 68.39 7.90 -8 3 0 34.00 16.10 -8 -3 0 72.99 9.70 8 -3 0 36.00 11.50 -8 3 0 51.49 9.10 -8 3 0 63.79 10.10 -8 -3 0 54.79 10.30 8 -3 0 59.99 7.80 8 3 0 15.20 13.30 8 -3 0 34.30 10.00 8 3 0 68.49 10.90 9 3 0 2.10 4.90 9 3 0 12.10 5.10 9 -3 0 4.90 5.70 9 3 0 1.70 6.60 -9 -3 0 -1.10 5.00 -9 3 0 -2.20 6.60 -9 -3 0 8.30 4.90 -9 3 0 0.10 3.00 9 -3 0 4.10 3.80 9 3 0 -0.50 2.80 -9 -3 0 0.00 4.40 9 -3 0 0.00 4.00 9 3 0 -7.10 7.20 9 -3 0 4.90 5.60 -9 -3 0 -12.50 4.80 -10 -3 0 1.90 2.30 -10 3 0 3.80 8.00 10 3 0 -3.00 3.40 10 -3 0 1.90 3.40 10 -3 0 3.00 3.20 -10 -3 0 -8.40 8.70 10 3 0 3.60 3.90 -10 -3 0 2.10 3.80 10 3 0 -0.30 3.30 -10 -3 0 -1.20 3.40 -10 3 0 1.60 3.00 0 4 0 1945.11 169.68 0 -4 0 1963.90 173.18 0 -4 0 1964.50 169.08 0 4 0 1986.10 173.18 0 -4 0 1988.20 169.38 0 -4 0 1945.51 168.98 0 4 0 1842.72 168.68 0 4 0 1944.71 169.48 0 4 0 1899.71 168.88 0 -4 0 2034.60 173.38 0 4 0 2001.70 173.38 1 4 0 5.60 7.20 -1 4 0 17.20 7.40 1 4 0 9.80 6.70 -1 -4 0 5.70 4.60 -1 4 0 5.80 7.40 1 -4 0 11.40 4.10 1 -4 0 9.50 8.20 1 4 0 5.30 8.10 -1 4 0 12.40 6.60 -1 4 0 16.40 5.00 -1 -4 0 9.80 8.10 1 -4 0 15.80 6.10 -1 -4 0 11.00 5.90 -1 -4 0 14.30 4.50 1 4 0 10.90 7.60 1 4 0 17.70 8.00 1 4 0 9.70 3.90 1 4 0 14.40 4.30 1 -4 0 17.70 5.80 -1 -4 0 5.00 8.90 -1 4 0 22.20 8.30 -1 4 0 15.90 6.40 1 -4 0 11.40 6.40 -1 -4 0 16.00 6.50 1 -4 0 14.10 5.20 -2 -4 0 367.96 34.30 2 4 0 381.06 34.70 -2 4 0 374.96 34.70 2 -4 0 381.26 34.90 -2 -4 0 406.36 34.50 -2 4 0 382.66 38.10 -2 4 0 383.26 39.40 -2 -4 0 370.96 38.80 2 4 0 353.66 34.10 2 4 0 412.56 39.40 -2 4 0 398.26 36.00 2 -4 0 396.76 39.20 -2 -4 0 411.76 35.00 2 4 0 394.46 38.40 2 4 0 384.36 35.20 -2 -4 0 391.66 39.20 -2 -4 0 372.76 33.30 2 -4 0 378.36 34.30 -2 4 0 364.06 33.80 -2 -4 0 400.06 34.50 -2 4 0 351.36 33.90 2 -4 0 361.46 34.30 2 -4 0 383.96 39.50 2 -4 0 371.86 34.00 -2 4 0 383.46 39.20 2 -4 0 340.57 33.80 2 4 0 391.86 39.30 -2 4 0 372.96 34.50 -2 4 0 388.36 34.10 2 -4 0 385.46 34.70 3 -4 0 31.10 8.30 -3 -4 0 30.10 7.50 3 -4 0 19.30 5.40 -3 4 0 13.10 8.30 3 -4 0 24.30 5.70 3 4 0 16.30 9.60 3 4 0 17.20 8.90 3 4 0 32.80 7.30 -3 4 0 16.80 7.20 -3 4 0 14.60 8.90 -3 4 0 19.70 9.40 3 4 0 20.80 6.50 3 -4 0 10.60 7.50 -3 -4 0 19.40 8.70 -3 -4 0 8.40 7.30 3 -4 0 25.30 7.40 -3 4 0 22.70 7.60 3 4 0 26.70 8.30 -3 -4 0 20.60 7.60 -3 4 0 24.70 5.80 -3 4 0 20.70 6.00 3 4 0 38.20 5.30 3 -4 0 14.80 8.00 3 4 0 29.10 7.70 -3 4 0 35.70 10.70 3 -4 0 25.00 4.70 3 4 0 20.30 9.20 3 -4 0 26.00 8.40 -3 -4 0 16.20 5.40 4 4 0 16.80 6.40 -4 4 0 9.60 4.40 4 -4 0 10.00 4.00 -4 -4 0 13.70 5.60 -4 -4 0 10.20 7.10 4 -4 0 14.80 6.10 4 -4 0 1.90 6.50 4 4 0 10.20 9.40 -4 4 0 9.10 5.50 -4 4 0 1.80 7.50 4 -4 0 12.30 6.80 -4 -4 0 7.10 6.20 4 4 0 19.50 9.00 4 4 0 9.60 6.70 4 4 0 11.10 6.10 4 -4 0 3.70 5.80 4 4 0 9.50 7.50 4 4 0 12.50 3.90 -4 4 0 5.00 3.00 4 4 0 13.10 4.70 4 -4 0 2.90 6.60 4 -4 0 7.80 7.80 -4 4 0 0.60 9.00 -4 4 0 5.70 9.20 5 -4 0 10.60 8.90 5 -4 0 2.50 5.90 -5 -4 0 11.20 5.40 5 4 0 0.00 4.30 -5 4 0 -24.80 10.90 5 -4 0 3.60 7.40 -5 4 0 3.40 9.20 -5 4 0 7.10 6.00 -5 -4 0 3.70 4.90 5 4 0 4.70 4.40 -5 -4 0 -2.80 4.00 -5 4 0 6.20 5.50 5 -4 0 2.80 6.40 5 4 0 5.10 5.30 5 -4 0 5.30 4.00 -6 4 0 278.77 34.10 -6 4 0 299.87 30.80 6 4 0 354.16 30.30 -6 -4 0 273.17 29.20 -6 4 0 308.57 29.90 6 -4 0 313.67 29.60 6 -4 0 360.26 30.60 6 -4 0 305.47 31.50 6 -4 0 339.97 29.10 -6 -4 0 321.47 31.30 6 -4 0 305.37 31.30 6 -4 0 368.46 32.00 -6 4 0 319.17 33.00 6 4 0 302.37 32.30 6 4 0 318.77 28.90 7 4 0 105.09 32.00 7 4 0 4.70 5.30 7 -4 0 6.70 8.00 -7 4 0 9.50 11.60 7 4 0 3.00 5.40 7 4 0 6.70 4.60 7 -4 0 -4.10 4.20 -7 -4 0 4.20 5.50 -7 -4 0 2.30 9.00 7 -4 0 9.10 7.60 7 -4 0 10.40 8.70 -7 4 0 11.40 6.30 -7 -4 0 -0.90 6.40 7 -4 0 5.00 8.10 7 -4 0 7.00 5.60 -7 4 0 0.10 4.20 7 4 0 6.90 7.20 8 -4 0 11.70 6.70 8 4 0 16.60 7.90 -8 4 0 3.30 10.90 8 4 0 4.90 5.30 -8 -4 0 0.60 5.30 -8 4 0 14.50 8.30 8 -4 0 9.60 7.90 -8 -4 0 0.70 10.60 8 4 0 10.60 4.50 8 -4 0 24.20 18.80 8 4 0 -0.50 6.10 -8 -4 0 -2.30 5.70 8 4 0 5.10 11.50 8 -4 0 11.00 5.00 8 -4 0 4.50 6.40 -8 4 0 11.10 7.30 9 -4 0 -8.90 6.80 -9 -4 0 3.90 4.40 -9 -4 0 -1.10 5.30 -9 -4 0 -0.30 3.00 9 4 0 0.50 3.80 9 -4 0 2.00 5.00 9 -4 0 5.80 4.00 -9 -4 0 -4.90 4.60 -9 -4 0 0.60 7.60 9 4 0 11.80 10.40 -9 4 0 -3.90 3.90 9 -4 0 -5.70 3.40 -9 4 0 9.80 8.90 9 4 0 2.50 4.20 9 4 0 3.20 4.50 10 -4 0 32.50 5.50 -10 -4 0 31.40 4.70 10 -4 0 7.30 4.50 -10 -4 0 4.40 4.70 10 4 0 15.80 3.10 10 4 0 9.40 3.50 10 -4 0 18.40 4.10 -10 4 0 -3.00 5.70 -10 -4 0 4.30 5.60 10 4 0 17.20 4.60 -10 4 0 14.00 3.30 0 5 0 -4.20 4.60 0 -5 0 0.00 4.10 0 -5 0 0.30 7.70 0 -5 0 -0.30 3.40 0 5 0 -1.50 3.80 0 5 0 -0.90 7.20 0 -5 0 12.30 7.50 0 5 0 -1.10 7.10 0 5 0 4.20 7.80 0 5 0 2.60 8.20 0 -5 0 1.10 4.30 1 5 0 9.80 4.20 -1 5 0 3.80 3.70 1 -5 0 5.80 7.70 -1 5 0 5.70 4.20 1 -5 0 10.40 6.30 -1 -5 0 2.40 6.60 -1 -5 0 4.90 6.00 1 5 0 6.20 8.00 -1 -5 0 -2.50 6.60 1 -5 0 4.30 5.80 1 5 0 1.00 5.70 1 5 0 -5.50 6.40 -1 -5 0 2.00 4.30 1 5 0 11.70 7.90 1 -5 0 2.60 3.20 1 -5 0 0.90 6.80 1 5 0 0.90 5.10 -1 5 0 -2.30 7.40 -1 5 0 -3.60 6.30 -1 5 0 9.40 7.10 -1 -5 0 0.30 6.70 1 -5 0 10.60 8.50 1 5 0 -0.10 7.10 -1 5 0 3.50 9.30 2 -5 0 30.00 5.90 2 5 0 36.00 8.00 2 -5 0 47.90 9.20 -2 -5 0 43.40 8.50 -2 -5 0 47.20 7.30 2 -5 0 35.90 5.80 -2 -5 0 49.00 9.70 2 5 0 44.80 8.00 2 5 0 38.50 10.40 -2 -5 0 23.50 9.60 2 5 0 28.60 5.30 -2 5 0 44.60 7.00 -2 5 0 32.90 6.20 -2 5 0 36.90 12.20 -2 5 0 24.90 10.40 -2 5 0 38.30 8.60 2 -5 0 42.40 6.30 -2 5 0 39.70 5.80 -2 5 0 44.40 12.10 -2 5 0 49.20 12.00 2 -5 0 35.30 6.00 -2 -5 0 30.90 4.60 -2 -5 0 23.20 9.80 2 5 0 30.50 10.30 2 -5 0 43.60 8.30 -2 -5 0 39.20 8.70 2 5 0 40.80 6.90 2 5 0 27.80 9.90 2 -5 0 40.00 11.20 2 5 0 33.30 10.60 -2 5 0 66.39 11.80 -3 5 0 10.20 8.30 -3 -5 0 3.00 6.60 -3 5 0 9.10 8.10 3 5 0 -1.80 4.10 3 -5 0 3.70 4.30 3 -5 0 -0.40 6.50 -3 5 0 -2.10 6.10 -3 -5 0 1.50 6.20 3 5 0 -2.00 6.50 3 5 0 4.60 4.50 -3 -5 0 -2.80 3.80 3 -5 0 2.00 3.30 3 -5 0 2.60 8.20 -3 5 0 0.80 4.00 -3 5 0 5.40 4.70 3 -5 0 5.00 8.10 3 -5 0 7.30 5.60 3 5 0 -5.60 3.40 3 -5 0 5.90 7.80 3 5 0 9.40 8.00 3 5 0 1.40 7.60 -3 -5 0 -6.30 7.80 -3 -5 0 -2.20 5.30 -3 5 0 -0.50 4.30 3 5 0 1.10 7.20 3 -5 0 -2.90 5.30 -3 5 0 -4.90 5.10 3 5 0 9.70 7.10 -4 5 0 84.39 9.90 -4 -5 0 78.59 10.60 4 5 0 87.99 11.60 4 -5 0 59.79 17.90 4 5 0 78.69 17.10 4 -5 0 69.19 8.40 4 -5 0 77.69 9.70 4 -5 0 73.39 17.40 -4 5 0 73.59 9.90 4 5 0 84.29 11.50 -4 -5 0 72.79 12.10 4 5 0 89.39 10.10 4 -5 0 80.69 8.80 4 -5 0 74.39 11.00 -4 5 0 92.99 16.10 4 5 0 81.89 9.90 4 -5 0 71.99 10.50 4 5 0 94.89 12.70 4 -5 0 74.99 11.00 -4 -5 0 106.69 11.50 -4 -5 0 82.89 9.60 4 5 0 89.59 9.60 -4 5 0 84.69 13.60 -4 5 0 71.49 10.30 5 5 0 4.50 4.10 -5 -5 0 -5.40 6.70 5 5 0 4.40 4.30 -5 -5 0 -4.80 4.60 -5 5 0 -0.40 8.60 -5 -5 0 -0.40 6.40 5 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4.10 6.80 5 6 0 -1.70 3.60 -5 -6 0 7.30 6.30 -5 -6 0 0.90 7.30 5 -6 0 3.10 5.10 5 -6 0 3.00 4.10 5 -6 0 -7.30 6.20 -5 -6 0 5.20 7.80 5 -6 0 4.80 6.30 5 -6 0 9.20 5.30 -5 -6 0 7.30 6.00 -5 6 0 0.80 6.80 5 -6 0 -2.70 7.70 -5 -6 0 5.60 4.30 -5 -6 0 -2.00 9.10 5 6 0 1.90 4.30 6 -6 0 25.40 6.60 6 -6 0 30.00 9.10 -6 -6 0 56.09 10.00 6 6 0 30.30 5.80 6 -6 0 19.10 7.40 -6 -6 0 29.60 10.70 6 -6 0 8.60 6.50 6 6 0 30.40 8.20 6 -6 0 20.90 10.90 -6 6 0 9.50 7.20 -6 -6 0 20.00 5.70 6 6 0 3.40 6.30 -6 -6 0 25.60 7.10 -6 -6 0 30.80 7.50 6 6 0 27.10 7.40 -6 6 0 27.70 6.50 6 -6 0 28.50 6.20 6 6 0 1.70 10.10 7 -6 0 3.10 6.00 -7 -6 0 0.20 9.60 7 -6 0 -2.30 5.60 7 6 0 -4.00 8.80 7 -6 0 -2.30 6.30 -7 -6 0 0.30 3.90 7 -6 0 -0.40 6.80 7 6 0 -3.90 5.00 -7 6 0 -6.60 5.50 7 -6 0 -2.30 6.00 -7 -6 0 0.10 6.00 -7 -6 0 0.50 6.60 7 6 0 -7.30 11.20 7 6 0 1.20 4.00 7 6 0 7.20 7.10 7 -6 0 1.60 4.70 -7 -6 0 -4.40 8.40 -7 6 0 7.90 6.70 -8 6 0 97.39 11.50 8 -6 0 88.79 12.50 8 6 0 97.39 11.80 -8 -6 0 97.69 12.40 8 6 0 95.39 11.00 -8 -6 0 109.99 12.10 8 -6 0 98.59 11.10 8 -6 0 104.19 13.60 8 6 0 115.89 13.00 -9 -6 0 5.20 5.30 9 6 0 -1.30 4.10 -9 -6 0 -8.20 8.10 9 -6 0 -0.20 4.10 -9 -6 0 0.50 2.20 9 -6 0 1.60 3.40 9 6 0 3.30 3.80 9 6 0 1.30 3.20 -9 6 0 -0.70 3.50 0 -7 0 1.30 4.10 0 7 0 -1.60 3.00 0 7 0 -18.50 10.50 0 7 0 -0.50 4.70 0 7 0 2.60 4.40 0 -7 0 3.70 5.50 0 -7 0 10.50 5.90 0 -7 0 0.60 6.90 0 7 0 -1.40 8.50 0 -7 0 -3.20 2.80 0 7 0 -1.00 3.50 0 -7 0 0.20 6.30 0 7 0 -0.80 9.30 0 -7 0 3.70 10.40 0 7 0 3.30 5.40 0 -7 0 9.00 9.20 0 -7 0 -0.80 6.20 0 7 0 2.20 9.20 1 -7 0 4.20 3.90 1 7 0 -5.20 9.20 -1 7 0 -3.70 4.80 1 -7 0 -2.40 7.20 -1 -7 0 2.80 6.80 -1 7 0 0.10 3.00 1 -7 0 1.60 4.60 -1 -7 0 3.30 6.70 1 -7 0 23.10 7.10 -1 -7 0 6.40 7.40 -1 7 0 -4.80 8.00 1 -7 0 5.90 4.20 1 -7 0 7.00 6.80 -1 -7 0 5.30 5.70 1 7 0 14.00 10.20 -1 7 0 -3.80 7.20 1 -7 0 3.50 3.10 -1 -7 0 -7.40 9.70 -1 -7 0 1.60 4.90 1 7 0 -4.00 4.00 1 7 0 1.80 5.00 -1 -7 0 2.50 6.80 1 7 0 9.00 9.60 -1 -7 0 1.80 5.80 -1 7 0 -7.10 6.40 -1 -7 0 2.10 3.00 1 7 0 2.40 5.90 -1 7 0 11.80 11.50 1 7 0 -0.40 3.20 1 -7 0 -4.30 4.50 2 -7 0 41.70 7.90 -2 7 0 35.80 8.30 2 7 0 35.30 5.60 2 -7 0 41.50 7.00 -2 7 0 34.80 6.30 -2 -7 0 37.50 7.40 2 -7 0 30.10 5.20 2 7 0 36.60 8.30 2 7 0 28.70 6.80 -2 -7 0 47.00 10.00 2 7 0 32.20 11.20 2 7 0 39.70 7.40 -2 -7 0 52.19 8.40 2 -7 0 47.90 8.90 2 -7 0 33.10 7.80 2 7 0 37.00 8.70 -2 -7 0 36.60 10.20 -2 7 0 16.10 16.00 -2 -7 0 46.50 9.90 -2 7 0 34.40 6.30 2 -7 0 43.80 8.60 -2 -7 0 -0.70 15.20 -2 7 0 22.70 8.40 2 -7 0 42.60 9.50 -2 7 0 49.40 11.90 -2 -7 0 33.10 7.40 -3 7 0 -0.40 4.40 3 -7 0 5.50 4.60 3 -7 0 -2.20 4.40 -3 7 0 3.80 6.40 3 7 0 3.10 8.70 -3 7 0 0.80 4.40 -3 7 0 2.80 6.00 -3 -7 0 6.10 5.60 -3 -7 0 4.20 4.50 3 7 0 -0.30 7.40 3 -7 0 1.50 7.10 3 -7 0 -0.10 4.00 3 7 0 5.00 4.90 -3 -7 0 1.90 6.10 3 7 0 2.50 3.80 -3 -7 0 13.70 7.40 -3 -7 0 -3.10 3.40 3 7 0 -1.60 6.00 3 -7 0 -1.80 5.90 3 -7 0 0.60 3.40 -3 -7 0 -6.10 6.60 3 7 0 20.10 10.30 -3 -7 0 4.60 8.10 -3 -7 0 2.00 4.90 -3 -7 0 -0.10 6.40 -3 7 0 -1.70 5.50 4 7 0 6.50 7.90 4 7 0 7.50 6.50 4 -7 0 2.10 4.30 -4 7 0 -9.40 6.00 -4 -7 0 6.10 6.90 4 7 0 3.50 4.00 4 7 0 6.70 5.60 4 7 0 0.80 4.80 4 7 0 2.20 9.50 -4 7 0 8.90 8.60 -4 -7 0 10.10 5.90 4 -7 0 4.70 5.10 -4 -7 0 2.10 6.30 -4 -7 0 -0.70 8.30 4 -7 0 3.80 4.20 -4 7 0 2.30 4.80 -4 7 0 5.40 6.60 -4 -7 0 13.40 6.40 4 -7 0 2.40 4.90 4 -7 0 7.90 3.80 4 -7 0 13.20 6.20 4 -7 0 4.40 6.90 -4 -7 0 4.00 4.90 4 7 0 -6.20 9.60 4 -7 0 7.70 7.00 5 7 0 18.80 11.60 -5 -7 0 4.10 6.10 5 7 0 4.60 4.60 5 -7 0 -0.80 7.00 5 -7 0 2.30 5.80 -5 -7 0 -9.90 7.10 5 7 0 1.80 6.80 5 7 0 -11.40 7.20 -5 -7 0 1.40 5.70 -5 -7 0 10.40 9.60 5 7 0 6.90 4.30 5 -7 0 -1.20 4.20 -5 -7 0 0.30 6.40 5 -7 0 0.60 4.20 -5 7 0 4.10 7.80 5 -7 0 3.00 7.10 5 -7 0 -8.00 5.00 -5 -7 0 1.20 5.50 -5 -7 0 3.90 7.90 -5 7 0 -9.90 6.20 -5 7 0 -6.60 4.40 5 7 0 0.50 7.10 6 7 0 -0.20 6.90 6 -7 0 4.10 7.40 -6 -7 0 12.50 10.40 -6 -7 0 17.60 7.90 6 -7 0 4.40 5.70 -6 7 0 15.50 5.80 6 7 0 23.30 9.20 6 -7 0 3.80 3.10 -6 -7 0 1.00 4.10 6 7 0 1.70 9.00 6 7 0 6.80 4.40 6 -7 0 -3.00 4.30 -6 7 0 4.70 6.60 6 7 0 0.70 9.30 -6 -7 0 3.00 5.70 6 -7 0 3.10 7.70 6 7 0 -7.10 5.20 6 -7 0 4.00 4.40 6 -7 0 5.40 7.80 6 7 0 1.40 5.60 -6 -7 0 0.00 5.10 -7 -7 0 10.10 7.20 7 7 0 -8.10 3.90 7 7 0 0.90 4.30 7 7 0 -5.60 4.50 -7 -7 0 0.40 5.50 -7 -7 0 -9.60 4.20 -7 7 0 -0.10 4.40 7 -7 0 -0.60 3.90 -7 -7 0 -0.40 5.50 -7 -7 0 2.20 4.40 7 -7 0 8.30 7.90 7 7 0 2.60 4.70 7 -7 0 1.80 3.80 7 -7 0 3.70 5.50 8 -7 0 16.60 4.40 -8 7 0 23.40 5.10 8 7 0 5.20 8.60 -8 -7 0 22.90 4.70 8 7 0 26.80 6.30 -8 -7 0 17.00 6.10 8 -7 0 16.60 4.40 8 7 0 20.90 4.70 8 7 0 22.70 8.30 8 -7 0 20.50 5.70 9 -7 0 -0.40 3.10 9 7 0 -1.20 2.40 -9 7 0 -1.50 2.50 9 -7 0 0.30 2.20 9 7 0 4.20 2.60 -9 7 0 -0.60 4.60 -9 -7 0 0.50 3.20 -9 -7 0 -0.30 2.90 0 -8 0 3.40 7.00 0 -8 0 9.10 3.40 0 -8 0 6.40 5.00 0 8 0 -2.40 5.30 0 8 0 22.50 10.90 0 -8 0 6.60 5.60 0 -8 0 6.30 4.20 0 8 0 4.00 3.50 0 -8 0 13.50 5.90 0 8 0 4.80 5.60 0 8 0 0.40 5.20 0 -8 0 9.50 4.60 0 -8 0 1.30 6.40 0 -8 0 -0.20 5.00 0 8 0 3.20 8.30 0 8 0 6.50 6.80 0 -8 0 16.10 6.60 -1 -8 0 0.40 5.90 1 -8 0 -3.60 6.70 1 -8 0 6.20 7.40 -1 8 0 6.00 8.20 1 8 0 1.70 8.00 -1 8 0 6.50 4.70 -1 -8 0 -3.20 5.40 1 8 0 2.20 10.10 -1 8 0 -2.60 2.80 1 8 0 -2.50 5.60 1 -8 0 -0.40 4.30 1 8 0 1.70 5.80 1 -8 0 1.80 7.10 1 -8 0 0.50 3.80 -1 8 0 6.80 4.60 -1 -8 0 1.80 5.10 -1 -8 0 9.60 6.60 1 -8 0 -10.30 5.50 1 -8 0 -0.80 3.60 -1 8 0 -1.30 5.70 -1 8 0 -0.10 8.40 -1 8 0 3.30 5.50 -1 -8 0 6.20 8.00 1 8 0 2.50 5.80 1 8 0 6.60 4.70 -1 -8 0 8.50 8.00 -1 -8 0 -1.80 6.10 -1 -8 0 -2.60 5.60 -1 8 0 2.60 5.00 1 -8 0 8.80 4.40 -2 -8 0 21.80 7.20 2 8 0 7.80 7.00 2 -8 0 11.80 5.60 -2 8 0 14.80 4.70 -2 8 0 10.30 8.10 -2 -8 0 7.90 6.20 -2 -8 0 14.10 7.60 -2 8 0 21.70 7.60 -2 -8 0 19.90 6.70 -2 -8 0 14.20 6.90 2 -8 0 7.20 3.60 2 -8 0 5.10 7.50 -2 -8 0 14.20 8.60 2 -8 0 15.80 6.30 2 -8 0 30.90 7.40 2 8 0 18.90 4.70 -2 8 0 33.20 10.90 2 8 0 9.30 6.50 2 8 0 1.00 10.70 -2 8 0 17.40 7.40 2 8 0 9.80 5.20 2 -8 0 18.60 9.30 2 -8 0 14.10 6.60 2 8 0 19.80 5.70 -2 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6.20 -2 -2 -26 56.29 7.50 2 2 -26 43.40 5.80 2 -2 26 40.40 5.50 2 2 -26 47.20 7.90 2 2 -26 31.40 5.90 2 2 -26 43.30 5.80 -2 2 26 40.10 6.00 -2 -2 -26 56.49 6.40 -2 2 26 41.00 6.10 -2 -2 26 37.30 6.80 -2 -2 26 21.70 7.20 2 -2 -26 49.50 7.00 2 -2 -26 50.49 7.50 2 -2 -26 44.30 5.60 2 -2 -26 47.50 6.90 2 -2 -26 55.99 7.30 -2 -2 26 55.49 6.40 -2 2 -26 33.10 5.30 -2 2 -26 52.19 6.70 -2 -2 26 31.10 6.80 -2 2 -26 48.40 6.40 -3 -2 -26 -0.80 1.90 -3 -2 -26 -1.50 4.10 3 2 -26 2.90 3.20 -3 2 26 -1.70 2.70 3 2 -26 -0.30 3.30 -3 2 26 3.50 3.50 -3 -2 -26 1.00 2.50 -3 -2 -26 -2.40 3.80 3 2 -26 1.40 2.90 3 2 -26 0.70 3.80 3 -2 -26 0.10 3.40 3 -2 -26 3.80 3.20 3 -2 -26 -1.00 1.90 -3 -2 26 -4.80 5.50 -3 -2 26 4.50 3.30 -3 -2 26 2.80 2.90 -3 2 -26 2.10 3.10 -3 -2 26 0.50 3.50 3 -2 -26 2.00 3.10 -3 2 -26 13.70 2.80 0 -3 -26 -0.50 2.80 0 -3 26 -5.40 2.70 0 3 26 -1.40 2.80 0 -3 -26 -0.40 4.40 0 -3 -26 -1.90 3.00 0 3 -26 3.10 4.10 0 3 -26 -0.30 3.50 0 -3 26 3.20 3.50 0 -3 26 1.00 3.00 0 3 26 2.00 5.10 0 3 -26 -2.80 3.10 -1 -3 -26 -0.50 2.70 1 -3 26 0.70 2.70 -1 3 26 0.20 2.70 -1 -3 -26 -3.80 2.70 1 3 -26 -0.10 3.30 1 3 -26 2.40 2.80 -1 -3 -26 -1.70 3.20 1 3 -26 -0.60 4.40 1 3 -26 0.50 3.90 1 -3 26 3.50 3.30 -1 -3 -26 -5.90 2.80 -1 3 26 1.20 2.50 -1 3 -26 0.80 4.90 -1 -3 26 -2.70 4.20 -1 -3 26 -2.60 3.20 -1 -3 26 1.70 3.70 -1 3 -26 2.50 3.70 1 -3 -26 1.00 3.00 -1 3 -26 3.30 3.50 1 -3 -26 -1.10 4.40 1 -3 -26 -1.50 2.70 1 3 26 -3.10 3.00 1 -3 -26 4.30 4.70 1 3 26 2.60 2.70 2 3 -26 14.40 3.60 2 3 -26 -7.20 5.30 -2 -3 -26 2.40 2.80 -2 -3 -26 -0.60 2.80 2 3 -26 0.30 2.30 -2 -3 -26 1.00 3.20 -2 -3 -26 -0.20 3.60 2 -3 26 3.70 3.40 -2 3 26 -2.70 3.70 2 3 -26 -0.80 3.10 2 -3 -26 2.60 4.70 2 -3 -26 0.80 2.70 2 -3 -26 -0.30 3.60 -2 3 -26 1.80 4.90 -2 -3 26 -0.50 2.70 2 -3 -26 3.70 2.60 2 -3 -26 0.20 2.90 -2 3 -26 4.10 4.80 -2 -3 26 0.60 4.20 -2 -3 26 1.40 4.80 -2 3 -26 0.40 1.90 3 3 -26 32.20 4.60 -3 -3 -26 46.00 5.40 -3 -3 -26 35.40 7.30 -3 -3 -26 36.50 4.90 -3 -3 -26 37.50 5.70 3 3 -26 47.70 7.30 -3 3 26 35.10 4.70 -3 -3 26 39.60 4.90 3 -3 -26 41.40 5.30 3 -3 -26 32.40 4.50 3 -3 -26 42.40 5.20 -3 3 -26 34.40 5.70 -3 3 -26 50.69 6.00 0 4 -26 8.10 3.70 0 -4 -26 -0.30 2.70 0 -4 -26 -0.70 2.80 0 -4 26 -0.90 2.10 0 4 -26 2.30 4.10 0 -4 26 -0.10 2.90 0 -4 -26 -0.50 2.90 0 -4 -26 -0.30 2.70 0 4 26 -0.30 1.90 1 4 -26 2.30 3.40 -1 4 26 4.30 3.80 -1 -4 -26 -2.50 2.60 1 -4 26 2.80 2.10 -1 4 26 -2.40 2.80 1 4 -26 -3.50 2.20 -1 -4 -26 -3.20 2.60 -1 -4 -26 2.50 4.20 -1 -4 -26 -0.30 3.80 -1 4 -26 0.20 3.20 1 -4 -26 -1.40 2.70 -1 4 -26 -0.30 3.10 1 4 26 -0.40 2.40 -1 -4 26 -5.40 2.90 1 -4 -26 0.90 4.40 -1 -4 26 -4.20 3.40 1 -4 -26 -2.30 2.60 1 -4 -26 0.60 2.50 -2 -4 -26 14.40 3.20 -2 4 26 10.90 3.30 2 -4 26 17.80 2.80 2 4 -26 2.80 2.90 2 4 -26 15.90 4.50 -2 -4 -26 8.20 3.20 -2 -4 -26 11.50 3.10 -2 4 26 10.10 3.40 2 4 -26 3.60 2.10 -2 -4 -26 10.30 3.20 -2 -4 26 4.20 3.30 2 -4 -26 16.40 4.10 -2 -4 26 12.50 3.10 2 -4 -26 13.20 3.80 -2 4 -26 11.40 3.60 2 -4 -26 5.90 2.60 -2 4 -26 3.30 4.60 2 -4 -26 10.70 4.70 0 5 -26 -2.50 2.70 0 5 -26 2.70 2.40 0 -5 -26 -2.80 2.40 0 5 26 0.10 1.70 0 -5 -26 -0.80 2.80 0 -5 -26 -1.70 3.20 0 -5 26 -0.50 2.20 0 -5 -26 0.30 2.30 0 -5 26 2.90 3.30 0 0 -27 0.70 3.30 0 0 -27 -0.90 3.30 0 0 -27 -0.80 4.40 0 0 27 0.40 3.50 0 0 27 -0.50 1.90 -1 0 -27 -1.50 2.80 -1 0 27 2.40 6.20 -1 0 27 4.00 3.70 -1 0 27 5.20 3.50 1 0 -27 3.00 4.10 1 0 -27 1.50 3.20 1 0 -27 -0.20 4.20 -1 0 -27 -1.10 3.20 1 0 27 -0.50 2.10 -1 0 -27 -4.70 2.90 -2 0 27 3.80 4.50 2 0 -27 2.60 2.70 -2 0 -27 2.30 3.00 2 0 -27 1.20 3.00 -2 0 -27 4.50 2.80 2 0 -27 -2.20 2.40 -2 0 27 2.60 5.50 -2 0 27 1.00 2.20 -2 0 -27 -2.80 3.10 -2 0 27 2.80 8.40 -3 0 27 0.30 1.90 -3 0 -27 0.90 2.40 3 0 -27 -2.50 2.90 -3 0 -27 0.20 2.10 3 0 -27 0.70 2.20 -3 0 -27 5.10 4.20 -3 0 27 0.50 3.10 3 0 -27 -2.00 2.90 0 1 27 1.90 3.40 0 1 27 1.20 2.80 0 -1 27 -2.60 3.50 0 -1 27 -0.10 2.80 0 -1 -27 0.00 3.00 0 1 -27 1.10 4.60 0 1 -27 -1.80 4.70 0 1 -27 -1.20 3.20 0 -1 27 -6.50 3.70 0 -1 -27 -2.30 2.20 0 -1 -27 -2.10 4.20 0 -1 -27 3.40 3.40 -1 -1 -27 4.10 3.60 1 1 -27 7.20 3.40 1 -1 27 7.00 2.60 -1 1 27 2.10 5.10 -1 -1 -27 2.40 3.50 -1 -1 -27 6.40 3.10 -1 -1 -27 7.40 3.30 -1 1 27 2.60 3.10 1 1 -27 3.90 3.30 1 1 -27 10.10 4.90 -1 1 -27 1.60 2.90 -1 1 -27 8.10 3.70 1 -1 -27 4.30 3.40 1 1 27 2.90 3.00 -1 1 -27 6.00 4.90 -1 -1 27 7.80 4.10 -1 -1 27 5.60 3.20 -1 -1 27 9.30 5.80 1 -1 -27 4.30 4.50 1 -1 -27 11.00 4.40 2 1 -27 -1.10 3.00 -2 -1 -27 6.60 4.40 2 1 -27 -0.60 2.70 -2 -1 -27 -0.10 3.90 -2 -1 -27 3.90 2.30 -2 1 27 1.00 4.10 2 1 -27 5.50 2.80 -2 1 27 1.20 2.30 -2 1 27 5.50 4.70 -2 -1 -27 2.90 3.00 -2 1 -27 0.60 3.30 2 -1 -27 1.20 2.30 2 -1 -27 0.60 3.30 -2 1 -27 1.50 2.50 -2 -1 27 5.30 3.10 -2 -1 27 1.10 4.20 -2 -1 27 2.70 2.60 -2 1 -27 5.10 3.40 2 -1 -27 2.60 3.90 -2 -1 27 1.70 3.10 -3 -1 -27 9.60 3.70 -3 -1 -27 2.70 2.50 3 1 -27 11.00 3.10 -3 1 27 7.70 3.10 3 1 -27 4.80 2.90 3 1 -27 3.00 1.80 -3 1 27 7.20 4.60 -3 -1 -27 -2.60 2.50 -3 1 -27 1.10 2.60 3 -1 -27 4.50 2.20 -3 -1 27 5.80 2.90 3 -1 -27 2.50 1.70 -3 1 -27 1.50 3.10 -3 -1 27 3.20 2.70 3 -1 -27 9.30 2.90 0 2 27 1.40 2.00 0 -2 -27 4.30 2.90 0 -2 27 0.00 1.70 0 2 -27 -1.00 2.80 0 -2 27 8.30 3.40 0 -2 -27 1.20 4.30 0 2 -27 0.10 3.20 0 -2 -27 -2.00 4.20 0 2 -27 0.80 3.30 0 -2 -27 2.40 3.40 1 2 -27 5.40 4.50 -1 2 27 13.60 3.40 1 2 -27 5.10 3.30 1 2 -27 5.30 3.20 -1 -2 -27 0.90 3.00 -1 -2 -27 8.90 3.50 -1 2 27 10.50 4.60 -1 -2 -27 8.00 3.50 -1 -2 -27 7.30 3.50 1 -2 27 5.50 2.70 -1 -2 27 10.50 4.30 -1 2 -27 9.60 4.10 1 -2 -27 7.80 4.50 -1 -2 27 3.50 2.10 1 -2 -27 8.70 3.10 -1 -2 27 7.60 6.00 1 -2 -27 8.20 3.70 -1 2 -27 4.70 4.50 1 -2 -27 10.70 4.40 1 2 27 7.20 2.60 -1 2 -27 0.40 3.50 -2 -2 -27 -0.50 2.70 2 2 -27 4.30 2.60 -2 -2 -27 1.00 2.90 -2 2 27 2.90 2.50 -2 2 27 2.50 3.00 2 2 -27 0.30 2.30 -2 -2 -27 4.80 4.30 -2 -2 -27 5.40 2.90 2 2 -27 1.70 2.90 2 -2 -27 3.10 2.90 -2 2 -27 0.00 4.20 -2 2 -27 0.60 1.70 -2 -2 27 2.10 2.70 -2 2 -27 5.10 3.30 2 -2 -27 -3.00 3.00 2 -2 -27 2.70 3.90 -2 -2 27 -0.40 3.80 -2 -2 27 5.10 2.90 0 3 -27 -1.00 3.90 0 -3 -27 -1.00 2.70 0 3 -27 -2.00 3.40 0 -3 -27 -0.90 2.50 0 3 -27 -2.50 4.10 0 3 27 -1.70 2.50 0 -3 -27 -3.80 2.80 0 -3 27 -3.30 2.60 0 -3 -27 5.20 2.80 -1 -3 -27 5.20 3.00 1 3 -27 0.60 2.80 1 3 -27 7.10 4.30 -1 -3 -27 10.40 3.70 -1 -3 -27 4.90 3.10 -1 -3 -27 11.20 3.30 -1 3 27 6.60 3.20 1 -3 27 9.90 2.60 1 3 -27 5.70 2.80 -1 3 -27 8.90 4.50 -1 3 -27 11.50 3.50 -1 3 -27 8.60 2.30 1 3 27 0.60 2.20 1 -3 -27 5.70 3.10 1 -3 -27 2.30 2.70 1 -3 -27 2.20 3.80 1 -3 -27 7.70 3.30 -1 -3 27 7.50 3.40 -2 -3 -27 -0.30 2.40 2 3 -27 0.00 2.30 -2 -3 -27 -2.60 2.20 -2 -3 -27 0.50 2.60 -2 3 27 -0.40 1.60 -2 -3 -27 -0.90 2.50 2 3 -27 -1.60 2.50 -2 -3 27 1.70 2.10 2 -3 -27 1.40 2.40 2 -3 -27 6.10 4.50 -2 3 -27 -1.40 2.90 -2 3 -27 2.70 2.90 0 0 28 85.09 8.40 0 0 -28 88.99 8.50 0 0 -28 66.59 8.40 1 0 -28 6.00 3.30 -1 0 -28 11.90 3.10 1 0 -28 1.20 3.80 -1 0 28 4.50 2.20 1 0 -28 6.10 2.90 -1 0 -28 10.60 3.50 -1 0 -28 6.70 3.30 0 -1 -28 -4.30 3.90 0 1 -28 1.00 2.70 0 1 -28 5.30 3.00 0 -1 -28 1.90 2.90 0 -1 -28 -1.80 2.80 0 1 28 -1.60 2.80 0 -1 28 -1.90 1.20 0 1 -28 -0.90 2.70 -1 -1 -28 12.10 3.10 -1 -1 -28 6.20 3.20 -1 1 28 6.70 3.10 1 1 -28 1.70 2.80 -1 -1 -28 5.60 3.20 -1 1 28 7.70 2.30 1 1 -28 13.50 4.40 1 1 -28 9.20 3.20 -1 1 -28 8.70 4.30 -1 1 -28 12.00 3.50 1 -1 -28 12.10 2.90 1 -1 -28 11.70 3.40 1 -1 -28 9.10 3.20 -1 -1 28 9.00 2.30 -1 1 -28 8.70 2.80 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 48319 #============================================================================= # end of cif data for "glo9753" (compound 2q) #============================================================================= #============================================================================= # cif data for "glo9768" (compound 2m) #============================================================================= data_glo9768 _audit_creation_method 'APEX3 v2016.1-0' _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H16 O' _chemical_formula_iupac ? _chemical_formula_weight 176.25 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.6389(3) _cell_length_b 5.30300(10) _cell_length_c 13.1361(3) _cell_angle_alpha 90 _cell_angle_beta 106.9940(10) _cell_angle_gamma 90 _cell_volume 975.23(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 5882 _cell_measurement_theta_min 3.1567 _cell_measurement_theta_max 68.7344 _cell_measurement_temperature 100.(2) _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.164 _exptl_crystal_size_mid 0.136 _exptl_crystal_size_min 0.035 _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 384 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Bruker AXS (2014). SADABS, Version 2014/5, Bruker AXS Inc., Madison, Wisconsin, USA. ; _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.98 _exptl_special_details ; ; _diffrn_ambient_temperature 100.(2) _diffrn_source 'Cu ImS' _diffrn_source_type 'micro focus tube' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _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 7.3910 _diffrn_reflns_number 10527 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_unetI/netI 0.0244 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 68.73 _diffrn_reflns_theta_full 68.73 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _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. The hydrogen at O1 atom was refined freely. ; _reflns_number_total 1794 _reflns_number_gt 1589 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_gt 0.0837 _refine_ls_wR_factor_ref 0.0867 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_number_reflns 1794 _refine_ls_number_parameters 122 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.4081P] 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 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.197 _refine_diff_density_min -0.197 _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 0.0181 0.0091 '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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ; APEX3 v2016.1-0 (Bruker AXS Inc., 2016) ; _computing_cell_refinement 'SAINT V8.37A (Bruker AXS Inc., 2015)' _computing_data_reduction 'SAINT V8.37A (Bruker AXS Inc., 2015)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'XP (Sheldrick, 2014)' _computing_publication_material 'SHELXL-2014/7 (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 O O1 0.52144(6) 0.55179(16) 0.28919(7) 0.0247(2) Uani d . . . 1 . . H H1 0.5082(14) 0.396(4) 0.2652(15) 0.059(5) Uiso d . . . 1 . . C C1 0.81531(8) 0.7176(2) 0.68174(9) 0.0169(3) Uani d . . . 1 . . C C2 0.88303(8) 0.9079(2) 0.71565(9) 0.0200(3) Uani d . . . 1 . . H H2 0.8887 1.0346 0.6667 0.024 Uiso calc U . R 1 . . C C3 0.94257(8) 0.9161(2) 0.81981(10) 0.0226(3) Uani d . . . 1 . . H H3 0.9884 1.0472 0.8413 0.027 Uiso calc U . R 1 . . C C4 0.93505(8) 0.7331(2) 0.89204(9) 0.0227(3) Uani d . . . 1 . . H H4 0.9752 0.7388 0.9634 0.027 Uiso calc U . R 1 . . C C5 0.86834(8) 0.5413(2) 0.85952(9) 0.0216(3) Uani d . . . 1 . . H H5 0.8632 0.4145 0.9087 0.026 Uiso calc U . R 1 . . C C6 0.80913(8) 0.5339(2) 0.75566(9) 0.0191(3) Uani d . . . 1 . . H H6 0.7637 0.4018 0.7344 0.023 Uiso calc U . R 1 . . C C11 0.74941(8) 0.7150(2) 0.56901(9) 0.0173(3) Uani d . . . 1 . . H H11 0.7713 0.851 0.5288 0.021 Uiso calc U . R 1 . . C C12 0.75263(8) 0.4650(2) 0.51088(9) 0.0196(3) Uani d . . . 1 . . H H12A 0.8188 0.4333 0.5092 0.023 Uiso calc U . R 1 . . H H12B 0.7339 0.3253 0.5506 0.023 Uiso calc U . R 1 . . C C13 0.68581(8) 0.4689(2) 0.39689(9) 0.0207(3) Uani d . . . 1 . . H H13A 0.7086 0.5958 0.3547 0.025 Uiso calc U . R 1 . . H H13B 0.6868 0.3018 0.3635 0.025 Uiso calc U . R 1 . . C C14 0.58402(8) 0.5322(2) 0.39575(9) 0.0188(3) Uani d . . . 1 . . H H14 0.5599 0.3961 0.4339 0.023 Uiso calc U . R 1 . . C C15 0.58081(8) 0.7812(2) 0.45117(9) 0.0206(3) Uani d . . . 1 . . H H15A 0.5144 0.8163 0.4512 0.025 Uiso calc U . R 1 . . H H15B 0.6013 0.9185 0.4117 0.025 Uiso calc U . R 1 . . C C16 0.64596(8) 0.7756(2) 0.56579(9) 0.0194(3) Uani d . . . 1 . . H H16A 0.6227 0.6465 0.6067 0.023 Uiso calc U . R 1 . . H H16B 0.6439 0.9414 0.5997 0.023 Uiso calc U . R 1 . . 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 O1 0.0309(5) 0.0179(4) 0.0188(4) 0.0002(4) -0.0032(3) -0.0010(3) C1 0.0164(5) 0.0153(5) 0.0199(6) 0.0026(4) 0.0068(4) -0.0014(4) C2 0.0195(6) 0.0166(5) 0.0242(6) 0.0008(4) 0.0069(5) 0.0009(5) C3 0.0185(6) 0.0199(6) 0.0274(6) -0.0007(5) 0.0034(5) -0.0036(5) C4 0.0198(6) 0.0251(6) 0.0203(6) 0.0047(5) 0.0015(4) -0.0024(5) C5 0.0231(6) 0.0212(6) 0.0210(6) 0.0040(5) 0.0074(5) 0.0025(5) C6 0.0186(5) 0.0177(6) 0.0215(6) -0.0006(4) 0.0066(4) -0.0005(4) C11 0.0190(6) 0.0151(5) 0.0184(6) -0.0006(4) 0.0063(4) 0.0004(4) C12 0.0192(6) 0.0179(6) 0.0220(6) 0.0020(4) 0.0065(5) -0.0018(5) C13 0.0248(6) 0.0181(6) 0.0195(6) -0.0008(5) 0.0072(5) -0.0032(4) C14 0.0211(6) 0.0168(6) 0.0159(5) -0.0008(4) 0.0015(4) 0.0016(4) C15 0.0207(6) 0.0187(6) 0.0204(6) 0.0031(4) 0.0028(5) -0.0002(5) C16 0.0196(6) 0.0189(6) 0.0187(6) 0.0026(4) 0.0042(4) -0.0019(4) _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 O1 C14 . 1.4352(13) ? O1 H1 . 0.89(2) ? C1 C2 . 1.3932(16) ? C1 C6 . 1.3973(16) ? C1 C11 . 1.5128(15) ? C2 C3 . 1.3916(16) ? C2 H2 . 0.95 ? C3 C4 . 1.3837(17) ? C3 H3 . 0.95 ? C4 C5 . 1.3882(17) ? C4 H4 . 0.95 ? C5 C6 . 1.3868(16) ? C5 H5 . 0.95 ? C6 H6 . 0.95 ? C11 C16 . 1.5366(15) ? C11 C12 . 1.5376(15) ? C11 H11 . 1.0 ? C12 C13 . 1.5307(15) ? C12 H12A . 0.99 ? C12 H12B . 0.99 ? C13 C14 . 1.5233(16) ? C13 H13A . 0.99 ? C13 H13B . 0.99 ? C14 C15 . 1.5149(15) ? C14 H14 . 1.0 ? C15 C16 . 1.5290(15) ? C15 H15A . 0.99 ? C15 H15B . 0.99 ? C16 H16A . 0.99 ? C16 H16B . 0.99 ? 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 C14 O1 H1 . . 106.8(12) ? C2 C1 C6 . . 117.87(10) ? C2 C1 C11 . . 120.69(10) ? C6 C1 C11 . . 121.43(10) ? C3 C2 C1 . . 121.30(11) ? C3 C2 H2 . . 119.4 ? C1 C2 H2 . . 119.4 ? C4 C3 C2 . . 120.00(11) ? C4 C3 H3 . . 120.0 ? C2 C3 H3 . . 120.0 ? C3 C4 C5 . . 119.51(11) ? C3 C4 H4 . . 120.2 ? C5 C4 H4 . . 120.2 ? C6 C5 C4 . . 120.32(11) ? C6 C5 H5 . . 119.8 ? C4 C5 H5 . . 119.8 ? C5 C6 C1 . . 121.01(11) ? C5 C6 H6 . . 119.5 ? C1 C6 H6 . . 119.5 ? C1 C11 C16 . . 111.49(9) ? C1 C11 C12 . . 113.01(9) ? C16 C11 C12 . . 109.87(9) ? C1 C11 H11 . . 107.4 ? C16 C11 H11 . . 107.4 ? C12 C11 H11 . . 107.4 ? C13 C12 C11 . . 111.76(9) ? C13 C12 H12A . . 109.3 ? C11 C12 H12A . . 109.3 ? C13 C12 H12B . . 109.3 ? C11 C12 H12B . . 109.3 ? H12A C12 H12B . . 107.9 ? C14 C13 C12 . . 110.86(9) ? C14 C13 H13A . . 109.5 ? C12 C13 H13A . . 109.5 ? C14 C13 H13B . . 109.5 ? C12 C13 H13B . . 109.5 ? H13A C13 H13B . . 108.1 ? O1 C14 C15 . . 107.76(9) ? O1 C14 C13 . . 111.67(9) ? C15 C14 C13 . . 110.81(9) ? O1 C14 H14 . . 108.8 ? C15 C14 H14 . . 108.8 ? C13 C14 H14 . . 108.8 ? C14 C15 C16 . . 111.00(9) ? C14 C15 H15A . . 109.4 ? C16 C15 H15A . . 109.4 ? C14 C15 H15B . . 109.4 ? C16 C15 H15B . . 109.4 ? H15A C15 H15B . . 108.0 ? C15 C16 C11 . . 110.93(9) ? C15 C16 H16A . . 109.5 ? C11 C16 H16A . . 109.5 ? C15 C16 H16B . . 109.5 ? C11 C16 H16B . . 109.5 ? H16A C16 H16B . . 108.0 ? 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 C6 C1 C2 C3 . . . . -0.22(16) ? C11 C1 C2 C3 . . . . 178.45(10) ? C1 C2 C3 C4 . . . . -0.12(17) ? C2 C3 C4 C5 . . . . 0.48(17) ? C3 C4 C5 C6 . . . . -0.49(17) ? C4 C5 C6 C1 . . . . 0.15(17) ? C2 C1 C6 C5 . . . . 0.21(16) ? C11 C1 C6 C5 . . . . -178.46(10) ? C2 C1 C11 C16 . . . . -110.01(12) ? C6 C1 C11 C16 . . . . 68.62(13) ? C2 C1 C11 C12 . . . . 125.66(11) ? C6 C1 C11 C12 . . . . -55.71(13) ? C1 C11 C12 C13 . . . . -179.59(9) ? C16 C11 C12 C13 . . . . 55.19(12) ? C11 C12 C13 C14 . . . . -55.68(12) ? C12 C13 C14 O1 . . . . 176.48(9) ? C12 C13 C14 C15 . . . . 56.34(12) ? O1 C14 C15 C16 . . . . 179.98(9) ? C13 C14 C15 C16 . . . . -57.57(12) ? C14 C15 C16 C11 . . . . 57.71(12) ? C1 C11 C16 C15 . . . . 178.05(9) ? C12 C11 C16 C15 . . . . -55.86(12) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H1 O1 2_645 0.89(2) 1.96(2) 2.8472(6) 179.(2) ? _shelx_res_file ; glo9768.res created by SHELXL-2014/7 TITL glo9768.res in P2(1)/c CELL 1.54178 14.6389 5.3030 13.1361 90.000 106.994 90.000 ZERR 4.000 0.0003 0.0001 0.0003 0.000 0.001 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H O UNIT 48 64 4 SIZE 0.035 0.136 0.164 TEMP -173.150 ACTA CONF L.S. 20 BOND $H FMAP 2 PLAN 10 EQIV $1 -x+1, y-1/2, -z+1/2 HTAB O1 O1_$1 WGHT 0.030800 0.408100 FVAR 1.35881 O1 3 0.521439 0.551789 0.289191 11.00000 0.03089 0.01786 = 0.01877 -0.00097 -0.00323 0.00025 H1 2 0.508209 0.395599 0.265227 11.00000 0.05886 C1 1 0.815306 0.717648 0.681738 11.00000 0.01636 0.01527 = 0.01990 -0.00142 0.00678 0.00262 C2 1 0.883031 0.907907 0.715647 11.00000 0.01952 0.01660 = 0.02424 0.00092 0.00692 0.00082 AFIX 43 H2 2 0.888676 1.034570 0.666699 11.00000 -1.20000 AFIX 0 C3 1 0.942568 0.916052 0.819807 11.00000 0.01852 0.01989 = 0.02739 -0.00364 0.00338 -0.00075 AFIX 43 H3 2 0.988376 1.047207 0.841319 11.00000 -1.20000 AFIX 0 C4 1 0.935048 0.733116 0.892044 11.00000 0.01978 0.02513 = 0.02033 -0.00243 0.00148 0.00475 AFIX 43 H4 2 0.975236 0.738760 0.963362 11.00000 -1.20000 AFIX 0 C5 1 0.868343 0.541285 0.859524 11.00000 0.02311 0.02119 = 0.02098 0.00254 0.00739 0.00403 AFIX 43 H5 2 0.863234 0.414486 0.908656 11.00000 -1.20000 AFIX 0 C6 1 0.809128 0.533861 0.755660 11.00000 0.01857 0.01772 = 0.02147 -0.00055 0.00657 -0.00059 AFIX 43 H6 2 0.763670 0.401805 0.734445 11.00000 -1.20000 AFIX 0 C11 1 0.749407 0.714981 0.569014 11.00000 0.01895 0.01514 = 0.01844 0.00040 0.00629 -0.00062 AFIX 13 H11 2 0.771250 0.851042 0.528839 11.00000 -1.20000 AFIX 0 C12 1 0.752630 0.464978 0.510875 11.00000 0.01917 0.01789 = 0.02197 -0.00178 0.00647 0.00199 AFIX 23 H12A 2 0.818813 0.433273 0.509170 11.00000 -1.20000 H12B 2 0.733943 0.325257 0.550633 11.00000 -1.20000 AFIX 0 C13 1 0.685810 0.468855 0.396891 11.00000 0.02484 0.01814 = 0.01947 -0.00320 0.00717 -0.00081 AFIX 23 H13A 2 0.708605 0.595813 0.354688 11.00000 -1.20000 H13B 2 0.686761 0.301847 0.363536 11.00000 -1.20000 AFIX 0 C14 1 0.584021 0.532237 0.395754 11.00000 0.02115 0.01683 = 0.01589 0.00163 0.00152 -0.00081 AFIX 13 H14 2 0.559935 0.396130 0.433923 11.00000 -1.20000 AFIX 0 C15 1 0.580812 0.781189 0.451172 11.00000 0.02074 0.01871 = 0.02036 -0.00024 0.00284 0.00307 AFIX 23 H15A 2 0.514409 0.816332 0.451233 11.00000 -1.20000 H15B 2 0.601289 0.918537 0.411698 11.00000 -1.20000 AFIX 0 C16 1 0.645957 0.775616 0.565790 11.00000 0.01964 0.01888 = 0.01872 -0.00192 0.00417 0.00261 AFIX 23 H16A 2 0.622681 0.646530 0.606674 11.00000 -1.20000 H16B 2 0.643874 0.941447 0.599656 11.00000 -1.20000 AFIX 0 HKLF 4 REM glo9768.res in P2(1)/c REM R1 = 0.0341 for 1589 Fo > 4sig(Fo) and 0.0385 for all 1794 data REM 122 parameters refined using 0 restraints END WGHT 0.0311 0.4069 REM Highest difference peak 0.197, deepest hole -0.197, 1-sigma level 0.032 Q1 1 0.6978 0.7457 0.5669 11.00000 0.05 0.20 Q2 1 0.7418 0.5907 0.5378 11.00000 0.05 0.19 Q3 1 0.8296 0.8348 0.7042 11.00000 0.05 0.18 Q4 1 0.6368 0.5118 0.4003 11.00000 0.05 0.17 Q5 1 0.7776 0.7160 0.6297 11.00000 0.05 0.16 Q6 1 0.7985 0.6654 0.7221 11.00000 0.05 0.14 Q7 1 0.6099 0.7816 0.5036 11.00000 0.05 0.13 Q8 1 0.5756 0.6590 0.4218 11.00000 0.05 0.12 Q9 1 0.9238 0.8676 0.7603 11.00000 0.05 0.12 Q10 1 0.9428 0.7903 0.8460 11.00000 0.05 0.12 ; _shelx_res_checksum 76760 _shelx_hkl_file ; 0 0 1 -0.30 0.50 0 0 -1 0.20 0.60 0 0 -2 43.80 2.90 0 0 2 45.10 2.90 0 0 3 -2.70 1.40 0 0 4 159.28 8.00 0 0 5 -1.00 1.50 0 0 6 1491.65 54.79 0 0 6 1384.86 52.59 0 0 7 -0.20 1.70 0 0 7 -1.00 2.10 0 0 -8 171.08 10.20 0 0 -8 140.19 11.70 0 0 8 153.78 10.30 0 0 9 1.50 2.70 0 0 9 0.40 3.30 0 0 -9 0.20 3.00 0 0 -9 3.60 3.50 0 0 10 357.36 17.30 0 0 -10 343.57 18.10 0 0 10 334.17 16.10 0 0 11 1.60 3.20 0 0 -11 -0.40 4.10 0 0 -11 -2.60 3.50 0 0 11 -0.40 2.70 0 0 12 7.20 3.10 0 0 12 11.90 3.80 0 0 -12 8.40 5.10 0 0 -12 9.20 3.70 0 0 -13 -1.10 2.10 0 0 13 -0.20 2.80 0 0 13 1.30 2.30 0 0 -13 -1.60 3.70 0 0 14 4.80 2.70 0 0 -14 5.40 6.40 0 0 14 5.00 2.20 0 0 -15 -1.70 1.60 0 0 15 0.20 1.30 0 1 0 -3.30 0.60 0 1 0 -2.90 1.50 0 -1 0 -2.10 0.60 0 -1 0 -1.50 1.50 0 1 1 3645.84 128.19 0 1 1 3546.15 129.59 0 -1 -1 3602.54 129.69 0 -1 1 3558.44 128.89 0 -1 1 3624.74 128.69 0 1 2 9.00 2.60 0 -1 -2 9.10 2.70 0 -1 2 12.10 1.80 0 1 3 109.39 7.20 0 -1 -3 109.99 7.30 0 1 4 -3.90 2.20 0 -1 -4 -0.60 2.50 0 -1 4 -2.40 1.00 0 1 5 313.37 15.30 0 -1 -5 297.17 15.20 0 -1 5 288.67 12.60 0 1 6 191.58 11.70 0 1 6 186.28 9.30 0 -1 6 196.38 9.20 0 -1 -6 180.88 11.70 0 1 7 82.39 5.70 0 1 7 87.49 8.20 0 -1 7 87.99 5.40 0 -1 -7 93.99 8.00 0 -1 7 87.49 5.30 0 1 -8 74.39 7.20 0 1 8 74.19 5.80 0 1 8 67.89 6.80 0 1 8 88.69 8.40 0 -1 -8 74.79 7.00 0 -1 8 83.19 5.70 0 -1 -8 83.59 7.20 0 1 -9 428.46 20.00 0 1 -9 423.36 20.60 0 1 9 408.76 19.70 0 1 9 419.46 18.60 0 1 9 425.66 19.90 0 -1 -9 447.66 20.20 0 -1 9 434.56 18.10 0 -1 -9 415.46 20.10 0 1 10 593.14 26.90 0 1 -10 640.24 28.20 0 -1 10 613.54 25.30 0 -1 -10 612.04 27.30 0 -1 -10 601.74 27.50 0 1 -11 792.12 34.40 0 1 11 877.71 35.50 0 1 11 839.32 33.50 0 1 -11 861.81 36.50 0 1 11 791.22 34.80 0 -1 11 881.41 33.50 0 -1 -11 876.51 36.20 0 -1 11 753.72 33.50 0 -1 -11 860.51 35.60 0 1 12 126.19 9.00 0 1 -12 125.59 10.50 0 1 12 128.09 8.70 0 -1 12 132.89 8.40 0 -1 -12 124.89 10.30 0 -1 -12 134.29 9.80 0 -1 12 96.59 7.30 0 1 -13 120.19 9.10 0 1 13 112.39 7.50 0 1 13 127.49 8.20 0 -1 -13 131.49 10.10 0 -1 13 132.19 8.10 0 -1 -13 128.69 9.00 0 1 14 -0.20 2.00 0 1 -14 4.50 2.70 0 1 14 0.10 1.80 0 -1 14 -1.80 2.20 0 -1 -14 0.30 1.50 0 -1 -14 1.20 3.20 0 -1 15 47.60 3.80 0 2 0 1797.72 68.29 0 -2 0 1828.32 68.39 0 2 1 435.46 19.40 0 2 -1 429.76 18.40 0 -2 -1 409.56 19.20 0 -2 1 419.96 16.40 0 -2 1 411.66 18.50 0 2 2 3796.32 136.79 0 -2 2 3772.12 134.99 0 -2 -2 3657.83 136.59 0 -2 2 3650.53 134.09 0 2 3 1193.38 44.20 0 -2 3 1187.48 45.40 0 -2 3 1195.68 44.90 0 -2 -3 1142.19 47.30 0 2 4 214.38 13.30 0 2 4 224.68 10.80 0 -2 -4 218.98 13.30 0 -2 4 235.98 12.20 0 -2 4 223.78 10.30 0 -2 -4 196.28 9.60 0 2 5 30.80 4.00 0 2 5 28.30 4.90 0 -2 5 29.60 4.40 0 -2 5 27.60 2.80 0 -2 -5 24.00 4.80 0 -2 -5 29.40 3.70 0 2 6 90.09 7.50 0 2 6 96.29 7.20 0 2 6 92.29 5.60 0 2 6 97.69 7.40 0 -2 -6 94.39 6.10 0 -2 -6 99.19 7.10 0 -2 -6 77.29 8.60 0 -2 6 88.59 8.70 0 -2 6 85.99 4.60 0 2 7 140.79 8.80 0 2 7 135.89 7.40 0 2 -7 121.29 9.10 0 2 7 135.29 9.50 0 2 7 138.79 9.20 0 -2 -7 140.29 7.70 0 -2 -7 139.99 9.20 0 2 -8 1947.11 77.49 0 2 -8 2130.79 78.59 0 2 8 2033.60 77.69 0 2 8 2032.80 78.19 0 2 8 2125.19 78.29 0 2 8 2034.60 75.49 0 -2 -8 2050.69 75.39 0 -2 -8 2057.49 77.89 0 -2 -8 2114.19 78.29 0 2 -9 146.69 10.70 0 2 9 146.59 11.90 0 2 9 145.99 10.30 0 2 9 149.49 10.40 0 2 9 143.49 8.50 0 2 -9 137.89 10.20 0 -2 -9 158.38 10.80 0 -2 -9 153.78 10.60 0 -2 9 150.48 8.20 0 2 -10 515.85 24.50 0 2 10 497.05 21.20 0 2 10 510.25 24.00 0 2 10 524.85 23.80 0 2 10 522.95 23.40 0 -2 -10 543.65 24.30 0 -2 10 533.85 21.60 0 -2 -10 490.15 23.90 0 2 11 252.67 14.20 0 2 11 231.58 11.60 0 2 11 243.88 14.00 0 2 -11 248.78 14.80 0 -2 11 246.48 12.30 0 -2 -11 245.28 14.40 0 -2 -11 260.37 14.70 0 2 12 3.50 3.10 0 2 -12 -1.20 3.60 0 2 12 -0.90 3.50 0 2 12 3.50 2.30 0 -2 -12 0.80 2.80 0 -2 -12 3.20 3.80 0 -2 12 0.50 2.40 0 2 13 10.10 2.90 0 2 13 10.90 3.90 0 -2 -13 11.60 3.90 0 -2 13 13.70 2.90 0 -2 -13 6.30 3.80 0 2 14 -1.90 1.40 0 2 14 0.90 1.50 0 -2 14 -0.90 1.60 0 -2 -14 2.90 2.70 0 -2 -14 3.80 2.00 0 3 0 -4.40 2.20 0 -3 0 -1.90 1.40 0 3 1 778.62 34.00 0 -3 -1 718.53 28.80 0 -3 -1 730.43 33.50 0 -3 1 765.32 32.80 0 3 2 813.52 31.70 0 -3 2 747.03 32.50 0 -3 -2 715.83 28.70 0 -3 -2 739.73 34.50 0 3 3 235.88 13.10 0 3 3 220.38 12.10 0 3 3 208.58 11.10 0 3 -3 243.08 12.90 0 -3 -3 235.58 10.60 0 -3 3 215.28 10.80 0 -3 3 216.68 12.60 0 3 4 587.34 26.60 0 3 4 584.64 25.50 0 3 4 573.44 24.80 0 3 -4 594.74 26.30 0 -3 -4 618.54 25.80 0 -3 4 639.84 27.10 0 -3 -4 625.34 24.20 0 3 -5 9.70 4.30 0 3 5 14.20 4.60 0 3 5 5.90 3.80 0 3 5 5.00 3.00 0 3 5 9.00 3.20 0 3 5 6.50 3.70 0 -3 -5 9.10 3.30 0 -3 5 1.80 2.30 0 -3 -5 4.70 2.50 0 3 -6 236.08 13.40 0 3 6 248.38 13.10 0 3 6 257.27 13.50 0 3 6 237.78 14.40 0 -3 -6 247.28 11.80 0 -3 -6 231.88 12.90 0 3 -7 87.69 7.90 0 3 7 81.79 7.60 0 3 7 92.09 8.90 0 3 7 85.89 7.60 0 -3 -7 76.79 6.90 0 -3 -7 82.49 7.40 0 3 8 41.20 6.40 0 3 8 41.90 7.00 0 3 8 43.60 5.60 0 -3 -8 45.70 7.10 0 -3 -8 39.50 4.90 0 -3 -8 46.00 6.20 0 3 9 479.85 22.50 0 3 9 478.35 22.20 0 3 9 446.96 22.50 0 -3 -9 470.05 22.40 0 -3 -9 487.65 22.20 0 3 10 299.97 16.10 0 3 10 284.67 15.80 0 3 10 307.57 16.10 0 -3 -10 289.57 16.20 0 -3 -10 315.97 15.60 0 3 11 49.99 5.60 0 3 11 52.29 6.60 0 3 11 50.19 5.90 0 -3 -11 45.60 6.60 0 -3 -11 44.90 6.10 0 -3 11 53.99 4.50 0 3 12 12.30 3.80 0 3 12 13.50 4.10 0 -3 12 15.00 2.50 0 -3 -12 26.50 7.80 0 -3 -12 10.70 3.60 0 3 13 91.59 6.00 0 3 13 84.79 5.70 0 -3 13 84.49 5.00 0 -3 -13 79.59 5.90 0 -3 -13 84.19 6.00 0 4 0 2722.13 102.79 0 4 0 2825.42 104.19 0 4 0 2783.62 104.39 0 -4 0 2745.23 100.49 0 4 1 683.03 29.30 0 4 1 692.83 30.70 0 4 1 691.03 29.70 0 4 -1 706.73 29.40 0 4 1 704.63 30.80 0 4 -1 735.23 31.80 0 4 -1 714.33 30.50 0 4 1 662.73 26.90 0 -4 -1 681.93 27.30 0 4 2 320.67 16.10 0 4 -2 327.17 17.30 0 4 2 329.57 14.70 0 4 2 349.67 17.00 0 4 2 357.66 24.50 0 4 -2 343.67 18.30 0 -4 -2 312.07 15.50 0 -4 -2 316.57 14.70 0 4 3 19.40 5.50 0 4 3 8.50 3.30 0 4 3 11.60 4.40 0 4 3 6.50 4.30 0 4 3 10.10 3.50 0 4 -3 18.40 5.20 0 -4 -3 10.20 3.10 0 -4 -3 14.90 3.90 0 4 4 139.49 10.40 0 4 4 147.79 8.80 0 4 4 141.19 10.90 0 4 -4 140.39 10.60 0 4 4 129.19 9.40 0 -4 -4 136.29 9.10 0 -4 -4 130.49 10.20 0 4 5 50.99 6.30 0 4 5 52.79 7.80 0 4 -5 37.30 6.30 0 4 5 42.50 5.60 0 4 5 47.80 6.50 0 -4 -5 49.40 6.10 0 -4 -5 53.89 5.80 0 4 6 217.98 12.20 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271.67 15.10 10 3 -6 273.67 14.80 -10 3 6 269.07 15.90 -10 3 6 278.07 14.50 -10 3 6 268.97 16.60 10 -3 -6 273.37 14.40 -10 -3 6 289.87 13.90 10 -3 -6 288.47 13.90 -10 3 5 37.80 6.30 10 3 -5 30.20 5.50 10 3 -5 30.20 6.00 -10 3 5 21.40 4.20 -10 3 5 40.60 6.60 10 -3 -5 34.90 5.30 -10 -3 5 43.90 5.50 10 -3 -5 41.50 5.80 10 3 -4 29.00 5.60 -10 3 4 26.70 5.50 -10 3 4 29.20 4.70 -10 3 4 24.80 6.40 10 3 -4 31.70 6.20 10 -3 -4 33.20 5.30 10 -3 -4 22.40 4.10 -10 -3 4 23.00 4.20 10 3 -3 7.80 3.80 -10 3 3 6.00 3.40 10 3 -3 4.40 4.60 10 3 -3 -1.70 3.70 10 3 -3 3.30 3.70 -10 3 3 -0.30 4.50 -10 3 3 3.90 3.10 -10 -3 3 3.40 3.50 10 -3 -3 4.60 2.90 10 -3 -3 14.50 3.60 10 3 -2 58.29 7.60 -10 3 2 77.19 6.10 -10 3 2 79.39 8.00 10 3 -2 77.49 8.50 10 3 -2 73.49 7.80 10 3 -2 66.69 6.90 10 3 -2 66.09 6.50 10 -3 -2 81.99 7.00 10 -3 -2 70.79 5.80 -10 -3 2 68.19 6.80 10 3 -1 2.60 4.30 -10 3 1 -0.50 1.90 10 3 -1 0.50 3.10 -10 3 1 0.10 3.70 10 3 -1 -4.00 3.90 10 3 -1 -0.60 4.40 10 3 -1 5.40 3.50 10 -3 -1 3.40 2.80 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10.80 10 4 -3 134.29 8.30 10 4 -3 142.09 10.80 10 4 -3 123.59 10.00 10 -4 -3 130.69 8.10 -10 4 2 4.80 4.40 10 4 -2 -3.60 3.10 10 4 -2 -0.80 3.60 10 4 -2 -1.40 4.00 10 4 -2 -2.80 3.10 10 -4 -2 -0.40 2.50 10 -4 -2 0.30 3.10 -10 4 1 2.20 3.90 10 4 -1 3.80 3.50 10 4 -1 0.70 3.00 10 4 -1 1.00 3.00 10 4 -1 1.80 4.20 -10 -4 1 3.80 2.90 10 -4 -1 -0.70 2.30 -10 4 0 16.90 3.90 10 4 0 12.00 3.60 10 4 0 16.20 4.50 10 4 0 19.60 4.30 10 4 0 13.20 3.70 -10 -4 0 14.20 3.30 10 -4 0 18.60 3.40 10 4 1 20.40 4.30 10 4 1 18.60 4.00 10 4 1 14.00 4.60 10 4 1 23.00 3.80 -10 4 -1 12.50 4.00 -10 -4 -1 23.40 3.90 -10 -4 -1 16.20 5.00 10 -4 1 20.70 3.40 -10 4 -2 554.14 24.50 10 4 2 593.34 26.00 10 4 2 604.54 25.00 10 4 2 609.34 25.20 -10 -4 -2 568.04 25.20 -10 -4 -2 581.04 23.10 10 -4 2 602.84 23.30 10 4 3 118.99 7.50 10 4 3 104.59 7.50 -10 -4 -3 119.69 7.80 10 -4 3 116.79 6.10 10 4 4 1.20 3.00 10 4 4 1.30 2.20 10 4 4 1.70 2.50 10 -4 4 -0.20 1.30 -10 -4 -4 -0.30 2.80 -10 -4 -4 6.60 1.90 10 4 5 69.09 5.20 10 4 5 70.69 5.50 -10 -4 -5 51.39 5.00 10 5 -6 0.90 2.40 -10 5 6 4.80 2.70 10 -5 -6 4.00 1.70 -10 -5 6 9.30 2.00 10 -5 -6 1.40 1.20 10 5 -5 36.10 3.00 10 5 -5 36.90 4.40 -10 5 5 32.80 4.80 10 -5 -5 38.40 3.20 -10 -5 5 40.50 3.60 10 -5 -5 37.70 3.00 -10 5 4 109.79 8.50 10 5 -4 139.19 7.50 10 5 -4 125.29 8.30 -10 -5 4 156.48 7.30 10 -5 -4 151.88 7.20 10 5 -3 129.09 7.40 -10 5 3 97.29 8.10 10 -5 -3 138.39 6.90 -10 -5 3 142.39 7.00 -10 5 2 119.69 8.20 10 5 -2 105.09 7.30 10 5 -2 108.09 7.00 10 -5 -2 111.79 6.00 -10 -5 2 117.19 6.30 -10 5 1 44.50 4.50 10 5 -1 41.70 4.30 10 5 -1 49.30 4.50 10 -5 -1 47.40 3.50 -10 -5 1 41.10 4.10 -10 -5 1 47.10 3.80 10 5 0 63.19 5.00 -10 5 0 47.60 4.30 -10 -5 0 58.99 3.70 -10 -5 0 65.59 4.80 10 -5 0 53.99 3.60 10 5 1 4.10 1.30 10 5 1 4.10 2.00 10 5 1 5.00 2.00 -10 5 -1 2.90 1.80 -10 -5 -1 2.90 2.20 11 0 -14 36.90 3.10 11 0 -14 38.70 5.40 -11 0 13 4.90 2.00 -11 0 13 -0.40 3.20 11 0 -13 -0.70 2.70 11 0 -13 2.20 3.90 -11 0 12 2.80 2.20 11 0 -12 8.60 4.70 -11 0 12 1.40 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306.57 16.60 11 1 -3 33.00 5.70 11 1 -3 44.70 5.80 -11 1 3 28.00 5.30 -11 -1 3 24.80 5.50 11 -1 -3 22.50 4.20 11 -1 -3 27.90 4.30 -11 -1 3 21.20 3.60 11 1 -2 5.60 3.80 -11 1 2 2.80 3.40 11 1 -2 14.50 2.80 11 1 -2 2.20 2.60 -11 -1 2 8.90 4.80 11 -1 -2 -1.60 1.70 -11 -1 2 -1.80 2.00 11 -1 -2 2.10 2.50 11 1 -1 -3.70 2.00 -11 1 1 -1.70 2.80 11 1 -1 -1.20 2.40 11 1 -1 0.40 1.90 11 -1 -1 -0.50 2.70 -11 -1 1 1.20 2.00 -11 -1 1 -2.10 3.30 11 1 0 190.28 11.10 -11 1 0 240.48 12.50 11 1 0 210.58 12.70 11 1 0 223.98 10.90 11 -1 0 235.38 11.60 11 -1 0 235.38 12.90 -11 -1 0 220.88 13.10 -11 1 -1 191.08 11.00 11 1 1 178.18 11.80 11 1 1 186.18 12.60 11 1 1 185.28 11.50 11 -1 1 191.08 10.50 -11 -1 -1 186.28 10.80 11 -1 1 187.68 11.10 -11 -1 -1 190.08 11.80 -11 1 -2 1325.67 50.39 11 1 2 1256.77 49.40 11 1 2 1318.17 52.99 11 1 2 1307.67 51.99 11 1 2 1326.67 50.99 -11 -1 -2 1340.27 51.69 11 -1 2 1262.87 50.19 11 -1 2 1353.76 49.99 -11 -1 -2 1242.18 50.39 -11 1 -3 71.79 6.40 11 1 3 61.89 5.80 11 1 3 70.29 6.80 11 1 3 70.19 7.60 11 1 3 77.79 7.60 11 -1 3 66.69 6.30 -11 -1 -3 66.69 6.20 11 -1 3 69.59 5.90 -11 -1 -3 75.99 7.80 11 1 4 132.59 7.90 11 1 4 111.59 7.90 11 1 4 148.29 12.80 11 1 4 119.69 9.10 -11 -1 -4 114.49 8.20 11 -1 4 128.69 8.40 11 1 5 4.00 3.20 11 1 5 8.10 4.40 11 1 5 1.00 3.80 11 -1 5 7.30 3.10 -11 -1 -5 2.60 2.60 11 1 6 9.30 3.20 11 1 6 11.20 3.10 11 1 6 8.90 4.40 11 -1 6 10.40 3.40 -11 -1 -6 11.30 3.40 11 -1 6 11.60 3.10 11 1 7 -0.10 2.20 11 1 7 1.20 3.30 11 -1 7 4.20 2.60 11 -1 7 1.90 2.50 -11 -1 -7 1.20 1.80 11 1 8 18.40 3.10 11 1 8 23.20 3.10 11 -1 8 16.30 2.90 11 -1 8 18.10 3.20 -11 2 13 37.00 4.50 11 2 -13 36.00 5.60 11 2 -13 32.70 3.80 -11 -2 13 37.80 3.70 11 -2 -13 35.50 3.70 11 -2 -13 35.80 3.50 11 2 -12 61.09 5.40 -11 2 12 57.89 5.10 -11 2 12 49.30 7.40 11 2 -12 63.09 5.10 11 2 -12 50.69 7.20 -11 -2 12 70.79 5.30 11 -2 -12 66.79 6.10 11 -2 -12 102.99 9.70 11 2 -11 9.90 3.80 -11 2 11 6.40 3.90 -11 2 11 5.20 4.90 11 2 -11 5.00 2.60 11 -2 -11 4.50 3.20 -11 -2 11 4.50 2.80 11 -2 -11 -2.40 1.90 11 -2 -11 1.50 3.30 -11 2 10 10.30 3.40 11 2 -10 3.00 4.50 -11 2 10 4.40 4.00 11 2 -10 8.90 3.40 11 -2 -10 7.00 3.80 -11 -2 10 10.40 3.20 11 -2 -10 9.70 3.50 11 2 -9 25.80 5.60 11 2 -9 12.60 4.10 11 2 -9 8.70 3.50 -11 2 9 15.00 4.00 -11 2 9 22.40 5.30 -11 -2 9 23.20 4.20 11 -2 -9 22.60 4.90 11 -2 -9 13.40 2.80 11 -2 -9 19.90 4.00 -11 2 8 73.49 12.00 -11 2 8 55.99 6.20 11 2 -8 57.19 8.10 11 2 -8 49.70 6.70 11 -2 -8 46.30 5.50 -11 -2 8 54.09 5.80 11 -2 -8 59.79 6.90 -11 2 7 66.79 7.30 11 2 -7 59.39 6.70 11 2 -7 61.79 7.20 -11 2 7 67.09 7.30 11 2 -7 75.39 7.40 11 -2 -7 65.29 6.50 -11 -2 7 59.69 5.90 11 -2 -7 57.39 7.00 -11 2 6 53.99 8.00 -11 2 6 66.39 6.50 -11 2 6 56.99 6.90 11 2 -6 57.29 7.00 11 2 -6 58.49 7.10 -11 -2 6 55.49 6.10 11 -2 -6 65.79 6.00 11 -2 -6 57.99 5.90 -11 2 5 -0.60 3.40 11 2 -5 -2.50 3.30 11 2 -5 4.70 3.50 -11 2 5 0.00 3.30 -11 2 5 -1.20 4.40 -11 -2 5 1.30 3.90 -11 -2 5 0.50 3.40 11 -2 -5 0.50 3.10 11 -2 -5 -0.50 2.60 -11 2 4 229.18 14.00 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55.99 6.30 11 2 2 19.80 5.10 11 2 2 14.90 4.00 11 2 2 23.70 5.80 -11 2 -2 13.20 2.90 11 -2 2 13.80 3.30 -11 -2 -2 19.20 4.70 11 -2 2 16.40 3.60 11 2 3 311.27 16.70 11 2 3 311.47 15.70 11 2 3 326.97 18.00 -11 -2 -3 299.57 15.70 11 -2 3 326.37 14.90 11 2 4 635.44 26.70 11 2 4 574.14 25.00 11 2 4 574.64 25.20 11 2 4 606.94 27.80 11 -2 4 618.04 24.70 -11 -2 -4 571.34 25.50 11 2 5 4.50 2.70 11 2 5 2.60 3.70 11 2 5 3.00 2.50 11 2 5 2.80 3.80 -11 -2 -5 2.90 2.50 11 -2 5 6.30 3.30 11 2 6 12.50 3.30 11 2 6 7.50 3.40 11 2 6 10.00 2.90 11 -2 6 13.30 2.90 11 -2 6 11.30 3.10 -11 -2 -6 7.20 3.00 11 2 7 1.20 1.90 11 2 7 3.30 2.60 11 2 7 -1.00 1.60 -11 -2 -7 -0.60 1.20 11 -2 7 3.70 2.00 11 2 8 27.80 4.70 11 -2 8 18.30 2.70 -11 3 12 31.20 3.10 -11 3 12 24.90 3.80 -11 -3 12 36.50 3.40 11 -3 -12 30.40 3.60 -11 3 11 1.90 2.20 11 3 -11 3.60 2.10 -11 3 11 3.70 2.70 11 3 -11 0.70 2.40 11 -3 -11 -1.70 1.40 11 -3 -11 2.00 2.10 -11 -3 11 1.60 2.10 11 -3 -11 5.90 2.50 -11 3 10 33.60 7.40 11 3 -10 26.80 4.80 11 3 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3 -3 16.00 5.70 11 3 -3 17.10 7.50 11 -3 -3 14.30 4.20 -11 -3 3 9.20 3.30 11 -3 -3 16.20 6.70 11 3 -2 13.30 8.40 11 3 -2 4.20 5.10 11 -3 -2 4.60 3.00 -11 -3 2 5.60 4.20 -11 -3 2 4.40 2.90 -11 3 1 128.49 6.80 11 3 -1 128.89 8.80 -11 3 1 135.39 10.80 11 3 -1 87.69 10.60 11 3 -1 129.39 9.50 11 3 -1 132.89 10.00 11 3 -1 120.79 9.60 11 -3 -1 141.99 8.30 -11 -3 1 134.39 8.10 11 3 0 961.30 38.90 -11 3 0 924.01 39.30 11 3 0 948.71 39.80 11 3 0 994.20 39.50 11 3 0 891.91 38.60 11 -3 0 954.00 37.10 -11 -3 0 957.00 36.70 11 3 1 52.49 5.60 11 3 1 56.29 7.40 11 3 1 54.99 6.80 -11 3 -1 55.59 6.20 11 3 1 53.69 7.30 11 -3 1 53.69 5.80 -11 -3 -1 53.59 6.90 11 3 2 50.99 6.60 11 3 2 45.70 6.40 11 3 2 33.70 5.40 11 -3 2 45.80 5.20 11 -3 2 45.60 5.10 -11 -3 -2 44.30 5.20 11 3 3 41.30 6.10 11 3 3 42.30 6.80 11 3 3 43.40 5.80 -11 -3 -3 50.49 5.90 11 -3 3 45.60 4.90 11 3 4 304.07 15.00 11 3 4 282.97 15.70 11 3 4 292.57 13.90 11 -3 4 302.37 13.10 -11 -3 -4 289.27 14.50 11 3 5 15.00 4.30 11 3 5 20.20 3.60 11 -3 5 13.70 2.70 -11 -3 -5 11.80 3.30 11 3 6 7.60 2.20 11 3 6 6.60 2.30 -11 -3 -6 8.90 2.60 11 -3 6 8.10 1.80 -11 4 10 51.29 3.60 -11 4 10 46.60 4.00 11 4 -10 49.90 4.40 -11 -4 10 55.99 3.80 11 4 -9 4.60 3.00 11 4 -9 1.20 1.30 -11 4 9 2.80 1.70 -11 4 9 3.20 1.90 -11 -4 9 3.50 1.50 11 -4 -9 2.60 1.50 11 -4 -9 3.00 2.10 11 4 -8 167.38 9.20 -11 4 8 158.68 9.90 -11 4 8 153.78 8.00 11 4 -8 190.78 11.10 11 -4 -8 165.38 8.80 -11 -4 8 187.68 8.80 11 4 -7 -1.20 6.80 11 4 -7 2.90 2.20 -11 4 7 9.20 5.80 -11 4 7 1.60 3.20 11 4 -7 0.70 1.70 -11 4 7 3.30 2.00 11 -4 -7 6.50 2.80 11 -4 -7 4.30 2.50 -11 -4 7 2.30 2.30 11 4 -6 208.98 11.10 -11 4 6 204.08 12.30 -11 4 6 234.08 12.70 -11 4 6 203.28 9.40 11 4 -6 221.08 11.50 11 4 -6 191.48 8.80 11 4 -6 229.18 13.60 -11 -4 6 217.88 10.50 11 -4 -6 212.28 10.60 -11 4 5 379.06 15.60 11 4 -5 403.56 18.60 -11 4 5 424.26 20.10 11 4 -5 396.96 18.60 11 4 -5 416.06 20.20 -11 -4 5 415.16 17.50 11 -4 -5 403.96 17.60 11 4 -4 65.29 6.40 -11 4 4 59.89 7.70 11 4 -4 62.49 5.50 11 4 -4 64.19 6.20 11 4 -4 52.19 7.10 11 -4 -4 60.79 5.50 -11 -4 4 69.39 5.60 11 -4 -4 57.59 5.10 11 4 -3 80.49 6.10 11 4 -3 85.19 8.00 11 4 -3 88.99 7.50 -11 4 3 66.49 8.00 11 -4 -3 75.59 5.10 -11 -4 3 81.89 6.10 11 -4 -3 77.89 6.00 11 4 -2 66.59 7.40 11 4 -2 59.59 5.60 -11 4 2 49.90 6.90 11 4 -2 56.29 6.60 11 -4 -2 57.29 5.20 -11 -4 2 60.79 5.30 -11 4 1 5.90 3.80 11 4 -1 1.40 2.30 11 4 -1 1.30 2.60 11 4 -1 1.10 3.90 11 4 -1 -1.40 5.70 11 -4 -1 0.60 2.10 -11 -4 1 0.10 2.60 11 4 0 3.90 2.80 11 4 0 5.70 2.50 11 4 0 5.00 3.00 -11 -4 0 4.50 4.00 -11 -4 0 2.90 2.50 11 -4 0 1.70 1.90 11 4 1 15.70 3.70 -11 4 -1 28.30 4.10 11 4 1 17.60 4.00 11 4 1 22.60 5.30 11 -4 1 23.50 3.20 11 -4 1 26.70 3.30 -11 -4 -1 27.60 4.90 11 4 2 135.79 8.10 11 4 2 130.59 8.90 11 4 2 144.19 8.40 11 -4 2 145.39 7.20 -11 -4 -2 131.69 8.50 11 4 3 87.49 6.10 11 4 3 98.39 6.80 11 4 3 95.99 6.50 11 -4 3 101.69 5.50 -11 -4 -3 96.49 6.30 11 4 4 134.59 6.80 11 4 4 152.38 8.30 11 4 4 150.58 7.70 -11 -4 -4 156.18 7.90 -11 5 3 34.30 4.20 11 5 -3 30.10 3.60 -11 -5 3 35.30 3.10 -11 -5 3 32.80 3.40 11 -5 -3 31.30 2.80 11 5 -2 4.80 1.70 -11 5 2 2.10 1.70 12 0 -14 1.00 1.20 12 0 -14 1.10 1.70 12 0 -13 -1.40 2.10 -12 0 13 -1.50 2.40 12 0 -13 2.40 2.60 -12 0 12 12.70 3.60 12 0 -12 25.20 4.40 12 0 -12 22.90 3.80 12 0 -11 0.00 3.20 -12 0 11 2.20 2.00 -12 0 11 3.30 3.60 12 0 -11 -2.30 4.00 12 0 -10 193.48 12.40 -12 0 10 188.08 11.80 12 0 -10 204.18 11.80 -12 0 9 5.60 2.60 -12 0 9 -2.00 3.90 12 0 -9 1.80 7.00 -12 0 8 122.29 9.50 12 0 -8 110.49 8.30 12 0 -8 101.79 8.50 12 0 -8 108.49 8.80 12 0 -7 -3.30 3.30 12 0 -7 -2.90 3.30 -12 0 7 0.30 1.70 12 0 -7 5.50 3.40 -12 0 7 1.00 3.80 12 0 -6 220.98 13.30 12 0 -6 251.87 13.60 12 0 -6 245.28 13.40 -12 0 6 243.98 14.00 12 0 -5 0.70 2.40 12 0 -5 3.80 3.90 12 0 -5 9.00 3.80 -12 0 5 -2.80 3.40 -12 0 4 256.17 14.50 12 0 -4 245.18 12.20 12 0 -4 264.07 14.30 12 0 -4 273.47 13.50 12 0 -3 -1.00 3.40 12 0 -3 -1.20 2.10 -12 0 3 3.30 3.80 12 0 -3 0.30 2.20 12 0 -2 121.29 8.90 12 0 -2 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13.30 4.30 -14 -3 6 16.60 3.00 14 -3 -6 26.00 3.60 14 -3 -6 21.40 2.50 14 3 -5 13.00 4.50 14 3 -5 14.30 4.00 14 3 -5 34.80 4.60 -14 3 5 30.30 3.60 14 3 -5 32.90 4.80 14 -3 -5 29.10 4.00 14 3 -4 2.80 3.50 14 3 -3 26.90 4.40 14 3 -3 28.80 3.90 14 3 -3 29.60 3.80 -14 3 3 22.20 1.90 14 -3 -3 28.30 3.90 14 3 -2 258.77 13.20 -14 -3 2 266.57 13.10 14 -3 -2 303.37 12.90 14 -3 -2 291.87 13.40 14 3 -1 9.10 3.40 14 3 -1 8.90 2.30 14 3 -1 9.10 3.60 14 3 -1 10.20 2.60 14 -3 -1 8.50 2.50 -14 -3 1 7.80 2.30 14 -3 -1 11.40 2.90 14 3 0 214.38 10.80 14 3 0 223.18 11.00 14 3 0 206.68 10.60 14 -3 0 226.88 10.60 -14 -3 0 202.98 10.10 14 3 1 5.90 2.80 14 3 1 5.50 1.90 14 3 1 10.70 2.50 -14 -3 -1 4.50 1.50 14 -3 1 4.90 2.00 14 3 2 134.69 8.30 14 3 2 128.79 6.50 14 3 2 104.09 6.80 14 -3 2 136.79 6.60 -14 -3 -2 133.39 6.20 -15 0 11 -1.70 2.10 15 0 -11 2.60 2.70 -15 0 10 19.70 3.70 15 0 -10 27.40 3.10 15 0 -10 19.20 3.90 15 0 -9 1.30 3.00 -15 0 9 -4.10 2.40 15 0 -9 3.00 2.50 15 0 -8 16.90 3.90 -15 0 8 13.30 4.20 15 0 -8 18.20 4.20 15 0 -7 -2.20 2.80 15 0 -7 1.30 2.90 -15 0 7 0.40 2.60 15 0 -6 486.15 20.80 15 0 -6 475.05 21.40 -15 0 6 463.45 21.70 15 0 -5 -3.90 2.40 15 0 -5 0.20 3.40 -15 0 5 -2.40 3.40 15 0 -4 86.59 7.10 15 0 -4 76.79 5.90 -15 0 4 94.59 8.00 -15 0 3 -0.60 3.40 15 0 -3 5.20 3.70 15 0 -3 -4.10 1.70 15 0 -2 15.10 4.30 15 0 -2 11.30 2.60 -15 0 2 10.60 4.00 15 0 -2 15.10 4.30 -15 0 1 -2.90 3.10 15 0 -1 6.00 3.60 15 0 -1 -1.40 2.30 15 0 -1 1.30 3.10 15 0 0 240.58 12.70 15 0 0 211.38 12.30 15 0 0 239.88 11.20 15 0 0 254.57 13.60 -15 0 0 266.17 12.90 -15 0 -1 1.10 3.00 15 0 1 0.10 2.30 15 0 1 3.40 2.00 15 0 1 -0.40 3.30 15 0 2 420.06 18.70 15 0 2 369.36 15.90 15 0 3 0.80 1.90 15 0 3 0.10 2.10 15 0 4 8.00 2.30 -15 1 11 10.20 2.30 15 1 -11 9.90 2.40 15 -1 -11 7.70 2.50 15 1 -10 50.99 5.00 -15 1 10 46.20 4.70 15 -1 -10 44.50 4.00 15 -1 -10 43.70 4.80 -15 -1 10 49.40 4.60 15 1 -9 5.30 2.40 -15 1 9 5.80 2.90 15 1 -9 6.10 5.60 -15 -1 9 5.80 2.80 15 -1 -9 6.10 3.00 15 -1 -9 4.40 2.60 15 1 -8 91.99 6.60 -15 1 8 100.09 7.70 15 -1 -8 88.49 6.30 -15 -1 8 78.69 6.70 15 -1 -8 90.49 7.00 15 1 -7 126.89 8.00 -15 1 7 144.19 9.30 15 1 -7 128.99 8.30 15 -1 -7 124.29 8.20 15 -1 -7 120.69 8.00 15 1 -6 4.20 3.70 15 1 -6 2.30 2.70 -15 1 6 1.70 3.80 15 -1 -6 4.90 2.30 -15 -1 6 2.80 3.20 15 -1 -6 4.30 2.70 15 -1 -6 2.70 2.80 15 1 -5 202.18 10.50 15 1 -5 209.98 12.10 -15 1 5 214.08 12.00 15 -1 -5 183.68 10.10 -15 -1 5 204.08 11.90 15 -1 -5 188.98 9.60 15 -1 -5 202.38 11.40 15 1 -4 1.40 3.60 15 1 -4 0.50 2.40 -15 1 4 -1.90 3.00 15 1 -4 2.80 2.80 15 -1 -4 -2.50 2.10 15 -1 -4 -1.40 2.20 -15 -1 4 2.50 3.50 15 -1 -4 2.70 2.60 15 1 -3 1.10 3.60 -15 1 3 3.30 3.20 15 1 -3 -2.40 2.60 15 -1 -3 2.30 3.40 -15 -1 3 5.30 3.50 15 -1 -3 -1.00 1.80 15 1 -2 21.00 4.60 -15 1 2 18.30 4.10 15 1 -2 23.40 3.90 15 1 -2 18.40 4.30 15 -1 -2 18.20 3.30 15 -1 -2 16.40 4.00 -15 -1 2 16.60 4.40 15 1 -1 -0.40 3.00 15 1 -1 6.80 3.20 -15 1 1 2.70 3.00 15 1 -1 -0.60 3.00 15 -1 -1 -0.50 1.90 -15 -1 1 -1.30 3.00 15 -1 -1 -2.70 2.20 15 1 0 4.20 3.20 15 1 0 4.80 2.60 -15 1 0 9.20 2.90 15 1 0 7.80 3.20 15 -1 0 11.40 2.90 -15 -1 0 8.70 3.00 15 1 1 51.19 6.70 15 1 1 64.99 5.60 15 1 1 66.09 6.10 15 -1 1 60.89 5.10 15 -1 1 61.19 4.90 15 1 2 425.66 19.90 15 1 2 407.76 18.90 15 1 2 466.45 18.30 15 -1 2 468.75 20.10 15 1 3 -0.90 1.80 15 -1 3 -0.40 1.40 15 -1 3 -0.70 2.50 15 2 -10 -2.70 1.70 -15 2 10 0.00 1.50 15 2 -10 -0.40 1.90 15 -2 -10 -0.50 1.20 15 -2 -10 -0.10 0.90 15 2 -9 613.54 24.30 -15 2 9 663.23 25.90 15 2 -9 661.43 25.70 15 -2 -9 611.44 25.00 15 -2 -9 642.54 25.30 15 2 -8 68.79 4.90 -15 2 8 75.09 6.00 15 2 -8 73.09 5.50 15 -2 -8 71.69 5.00 15 -2 -8 77.19 5.60 15 2 -7 22.00 4.00 15 2 -7 16.50 3.50 15 -2 -7 15.70 3.00 -15 -2 7 16.60 4.80 15 2 -6 -0.50 3.10 -15 2 6 2.30 2.80 15 -2 -6 1.80 1.80 -15 -2 6 8.20 3.00 15 -2 -6 1.50 3.10 15 -2 -6 3.60 2.30 15 2 -5 4.00 3.30 15 2 -5 10.20 3.10 15 2 -5 10.60 3.90 -15 2 5 4.10 2.90 15 -2 -5 9.90 2.10 15 -2 -5 5.50 3.50 -15 -2 5 7.80 2.70 15 -2 -5 4.50 2.10 15 2 -4 19.50 4.30 -15 2 4 19.10 3.50 15 2 -4 12.40 3.20 15 2 -4 18.20 3.60 -15 -2 4 18.90 4.00 15 -2 -4 14.80 4.30 15 -2 -4 12.40 2.80 -15 2 3 0.80 2.50 15 2 -3 0.60 3.00 15 2 -3 3.40 2.10 15 2 -3 1.00 3.00 15 2 -3 0.20 1.90 -15 -2 3 1.70 2.10 15 -2 -3 1.70 2.40 -15 -2 3 5.10 2.90 15 -2 -3 -0.40 2.20 -15 2 2 121.99 8.30 15 2 -2 130.49 8.30 15 2 -2 134.29 9.00 15 2 -2 123.79 7.90 15 2 -2 154.18 12.30 15 -2 -2 131.19 7.50 -15 -2 2 125.69 8.50 -15 2 1 8.90 2.30 15 2 -1 1.50 2.20 15 2 -1 -1.10 2.40 15 -2 -1 -0.20 2.30 15 -2 -1 4.40 2.20 15 2 0 41.50 5.00 15 2 0 42.40 5.30 15 2 0 40.00 4.20 15 -2 0 40.90 3.50 15 -2 0 44.60 4.30 15 2 1 1.90 1.70 15 2 1 0.70 1.80 15 2 1 -0.20 2.40 15 -2 1 -1.10 2.10 15 2 2 10.70 2.10 15 2 2 2.40 1.80 15 2 2 4.40 1.80 15 -2 2 4.10 1.70 -15 3 7 28.90 3.20 15 3 -7 30.10 2.90 15 3 -7 41.70 3.40 15 3 -7 26.70 4.30 15 3 -7 34.70 2.90 15 -3 -7 42.10 4.20 -15 3 6 -0.70 1.70 15 3 -6 1.40 1.30 15 3 -6 1.20 1.80 15 3 -6 0.80 2.10 15 3 -6 1.70 2.10 15 -3 -6 1.50 2.30 15 -3 -6 2.60 1.40 15 3 -5 7.70 2.10 15 3 -5 11.40 2.70 15 3 -5 12.50 2.50 15 3 -5 15.00 2.80 -15 3 5 18.40 2.60 15 -3 -5 11.60 3.10 15 -3 -5 10.80 2.20 15 3 -4 3.10 2.60 15 3 -4 -1.20 1.50 15 3 -4 1.90 1.80 15 -3 -4 3.30 1.90 -15 -3 4 2.10 2.10 15 -3 -4 0.30 1.60 15 3 -3 37.00 4.00 15 3 -3 31.40 3.60 15 3 -3 35.20 4.30 -15 -3 3 31.10 3.00 15 -3 -3 36.70 3.60 15 -3 -3 30.90 3.00 15 3 -2 5.60 2.60 15 3 -2 8.50 2.50 -15 -3 2 13.30 1.90 15 -3 -2 4.10 1.60 15 -3 -2 6.10 1.50 15 3 -1 3.00 1.70 15 3 -1 0.50 2.40 15 -3 -1 0.70 1.30 15 -3 -1 1.80 1.20 -15 -3 1 6.50 2.80 16 0 -10 43.80 3.70 16 0 -10 34.40 3.10 16 0 -9 -0.10 1.90 -16 0 9 1.00 1.70 16 0 -9 0.10 1.60 -16 0 8 27.30 4.40 16 0 -8 30.80 4.20 16 0 -8 23.40 3.40 16 0 -7 0.10 2.20 -16 0 7 -2.40 2.90 16 0 -7 0.00 1.90 16 0 -6 -1.00 2.00 -16 0 6 0.20 3.30 16 0 -6 1.00 2.30 16 0 -5 -0.10 2.20 16 0 -5 -0.10 1.80 16 0 -5 -1.10 1.80 -16 0 5 -4.00 3.00 16 0 -4 6.80 3.50 -16 0 4 8.60 3.50 16 0 -4 20.00 3.70 16 0 -3 -2.40 3.00 16 0 -3 2.20 2.90 -16 0 3 2.70 2.30 16 0 -3 1.70 3.00 16 0 -2 27.50 4.10 16 0 -2 25.40 4.10 -16 0 2 22.70 3.70 16 0 -1 -6.20 2.40 16 0 -1 -0.10 1.80 16 0 -1 1.00 2.70 -16 0 1 -1.60 4.00 -16 0 0 1189.38 43.20 16 0 0 1075.69 44.20 16 0 0 1129.49 42.90 16 0 1 1.40 1.90 16 0 1 1.90 1.80 16 0 2 22.70 3.90 -16 1 10 13.30 2.80 16 1 -10 14.00 2.60 16 -1 -10 21.10 2.30 16 -1 -10 16.90 2.40 16 1 -9 3.50 1.40 -16 1 9 4.20 2.20 16 1 -9 5.50 2.50 16 -1 -9 1.60 1.40 -16 -1 9 4.10 2.20 16 -1 -9 3.10 1.70 16 1 -8 117.09 7.20 -16 1 8 131.49 7.50 16 1 -8 129.89 7.50 16 -1 -8 115.39 6.70 16 -1 -8 119.19 7.40 -16 -1 8 122.09 7.30 -16 1 7 92.09 6.80 16 1 -7 85.19 5.90 16 1 -7 81.89 6.10 -16 -1 7 86.29 6.60 16 -1 -7 80.79 5.30 16 -1 -7 82.69 6.00 16 1 -6 172.68 9.10 16 -1 -6 168.98 8.50 -16 -1 6 169.08 9.90 -16 1 5 2.90 3.00 16 1 -5 3.70 3.20 16 1 -5 6.00 2.70 16 -1 -5 3.00 1.60 16 -1 -5 1.40 3.10 -16 -1 5 2.80 3.00 16 1 -4 22.00 4.50 16 1 -4 17.00 3.90 -16 1 4 20.30 3.80 16 1 -4 22.90 2.60 -16 -1 4 25.90 3.80 16 -1 -4 22.20 2.90 16 -1 -4 22.80 4.30 16 1 -3 112.49 7.40 16 1 -3 115.09 7.50 -16 1 3 107.49 7.20 16 1 -3 100.89 6.90 -16 -1 3 111.79 7.30 16 1 -2 0.50 1.80 -16 1 2 0.20 2.30 16 1 -2 -1.30 1.80 16 1 -2 0.20 2.20 -16 -1 2 -0.80 2.60 16 -1 -2 -2.20 2.40 16 1 -1 69.99 5.50 16 1 -1 70.89 6.10 -16 1 1 69.99 5.20 16 1 -1 73.79 5.60 16 -1 -1 73.19 4.70 16 -1 -1 80.39 5.90 -16 -1 1 60.49 5.90 16 1 0 220.58 10.30 16 1 0 216.28 10.90 16 -1 0 182.88 11.00 16 -1 0 212.08 9.40 16 -1 0 195.08 9.40 16 1 1 387.66 19.20 16 1 1 443.96 18.90 16 1 1 466.75 18.30 16 -1 1 485.05 18.20 16 -1 1 510.45 20.20 16 2 -8 439.26 17.50 -16 2 8 433.96 17.60 16 2 -8 434.96 17.60 16 2 -8 413.36 16.90 16 -2 -8 415.06 17.30 16 -2 -8 418.96 16.80 16 2 -7 116.29 7.30 -16 2 7 131.79 7.00 16 2 -7 134.09 6.90 16 2 -7 126.09 7.10 16 -2 -7 122.79 6.10 -16 -2 7 113.09 9.30 16 -2 -7 141.89 7.30 16 2 -6 4.90 2.00 16 2 -6 5.90 1.70 -16 2 6 2.90 2.00 16 2 -6 3.50 2.50 16 -2 -6 6.00 2.10 -16 -2 6 6.90 2.00 16 2 -5 3.40 2.00 16 2 -5 5.90 2.20 -16 2 5 5.80 2.20 16 2 -5 4.70 1.60 16 -2 -5 4.70 1.50 -16 -2 5 3.90 1.90 16 -2 -5 0.90 2.30 16 2 -4 93.99 6.90 16 2 -4 105.49 5.60 16 2 -4 120.19 7.10 -16 2 4 101.89 6.00 16 2 -4 108.19 7.20 16 -2 -4 115.49 5.90 16 -2 -4 112.29 7.10 -16 -2 4 112.99 6.90 16 2 -3 172.98 8.80 -16 2 3 153.48 7.30 16 2 -3 135.89 8.80 16 2 -3 163.98 9.10 16 -2 -3 158.98 7.70 16 -2 -3 158.28 8.60 16 2 -2 11.40 2.20 16 2 -2 10.50 2.60 -16 2 2 8.30 1.60 16 2 -2 11.40 2.70 16 -2 -2 11.40 2.10 16 -2 -2 10.80 2.00 16 2 -1 14.30 3.10 16 2 -1 9.80 2.30 16 2 -1 9.40 2.00 16 -2 -1 8.30 2.40 16 -2 -1 9.20 2.10 16 2 0 17.30 2.90 16 2 0 18.10 2.80 16 2 0 13.50 2.50 16 -2 0 10.30 1.80 17 0 -8 301.47 13.20 17 0 -8 304.47 12.70 -17 0 8 301.37 13.50 17 0 -7 -0.10 1.70 17 0 -7 0.80 0.90 -17 0 7 0.10 2.30 17 0 -6 141.39 8.10 -17 0 6 131.59 7.60 17 0 -6 129.79 6.40 17 0 -5 -0.80 1.90 17 0 -5 0.50 2.60 -17 0 5 -0.10 2.30 17 0 -4 1.60 1.50 -17 0 4 0.60 2.50 17 0 -4 -0.70 1.90 17 0 -4 -1.50 1.30 -17 0 3 -0.10 1.70 17 0 -3 1.20 1.70 17 0 -3 -1.90 1.70 17 0 -3 -2.40 2.00 17 0 -2 18.80 2.80 -17 0 2 16.10 3.00 17 0 -2 19.80 3.40 17 0 -1 0.70 2.00 -17 1 7 0.10 1.50 17 1 -7 0.10 1.60 17 1 -7 1.40 1.30 17 1 -7 -0.90 1.40 17 -1 -7 0.20 1.30 -17 -1 7 3.00 2.00 17 1 -6 0.70 1.50 17 1 -6 0.90 2.30 17 1 -6 1.90 1.30 -17 1 6 1.90 2.10 17 -1 -6 5.10 2.00 -17 -1 6 -2.20 1.90 -17 1 5 0.10 1.40 17 1 -5 -1.40 2.10 17 1 -5 1.20 1.70 -17 -1 5 -3.90 1.80 17 -1 -5 0.80 1.70 17 -1 -5 0.90 1.40 -17 1 4 37.20 3.80 17 1 -4 30.10 4.00 17 1 -4 31.10 3.70 17 -1 -4 29.60 3.60 -17 -1 4 31.10 4.10 17 1 -3 -0.10 2.20 -17 1 3 -0.20 1.30 17 1 -3 0.80 1.70 17 1 -3 2.00 1.90 -17 -1 3 0.20 1.40 17 -1 -3 2.50 1.70 17 -1 -3 -0.60 2.10 17 1 -2 1.50 2.10 -17 1 2 -0.10 1.60 17 1 -2 0.40 1.40 17 1 -2 -0.70 1.50 17 -1 -2 -0.20 1.40 17 -1 -2 -0.60 1.30 17 1 -1 5.70 2.00 17 -1 -1 4.60 1.90 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 40633 #============================================================================= # end of cif data for "glo9768" (compound 2m) #============================================================================= #============================================================================= # cif data for "glo9770" (compound 2o) #============================================================================= data_glo9770 _audit_creation_method 'APEX3 v2016.1-0' _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H28 O2' _chemical_formula_iupac ? _chemical_formula_weight 240.37 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.1475(2) _cell_length_b 19.6782(5) _cell_length_c 7.9541(2) _cell_angle_alpha 90 _cell_angle_beta 92.1100(10) _cell_angle_gamma 90 _cell_volume 1430.82(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8274 _cell_measurement_theta_min 4.4939 _cell_measurement_theta_max 66.8256 _cell_measurement_temperature 100.(2) _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.152 _exptl_crystal_size_mid 0.148 _exptl_crystal_size_min 0.056 _exptl_crystal_density_diffrn 1.116 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 0.552 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Bruker AXS (2014). SADABS, Version 2014/5, Bruker AXS Inc., Madison, Wisconsin, USA. ; _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.97 _exptl_special_details ; ; _diffrn_ambient_temperature 100.(2) _diffrn_source 'Cu ImS' _diffrn_source_type 'micro focus tube' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _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 7.3910 _diffrn_reflns_number 15292 _diffrn_reflns_av_R_equivalents 0.0624 _diffrn_reflns_av_unetI/netI 0.0468 _diffrn_reflns_theta_min 4.49 _diffrn_reflns_theta_max 66.87 _diffrn_reflns_theta_full 66.87 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _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. The hydrogens at O1 and O2 atoms were refined freely. ; _reflns_number_total 2523 _reflns_number_gt 2197 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0729 _refine_ls_wR_factor_gt 0.1931 _refine_ls_wR_factor_ref 0.2031 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_number_reflns 2523 _refine_ls_number_parameters 165 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1377P)^2^+0.3989P] 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 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.391 _refine_diff_density_min -0.403 _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_extinction_coef 0.031(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ; APEX3 v2016.1-0 (Bruker AXS Inc., 2016) ; _computing_cell_refinement 'SAINT V8.37A (Bruker AXS Inc., 2015)' _computing_data_reduction 'SAINT V8.37A (Bruker AXS Inc., 2015)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'XP (Sheldrick, 2014)' _computing_publication_material 'SHELXL-2014/7 (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 O O1 1.01728(14) 0.69606(7) 0.17553(17) 0.0218(4) Uani d . . . 1 . . H H1 1.048(3) 0.7344(16) 0.239(4) 0.040(7) Uiso d . . . 1 . . O O2 0.11186(14) 0.69293(7) 0.85953(17) 0.0200(4) Uani d . . . 1 . . H H2 0.072(4) 0.6915(18) 0.965(5) 0.054(9) Uiso d . . . 1 . . C C1 0.68135(18) 0.57888(8) 0.7150(2) 0.0147(5) Uani d . . . 1 . . C C2 0.76228(19) 0.58465(10) 0.8877(2) 0.0191(5) Uani d . . . 1 . . H H2A 0.7054 0.5617 0.973 0.029 Uiso calc U . R 1 . . H H2B 0.7741 0.6327 0.9177 0.029 Uiso calc U . R 1 . . H H2C 0.8587 0.5633 0.8824 0.029 Uiso calc U . R 1 . . C C3 0.67630(19) 0.50342(9) 0.6642(2) 0.0200(5) Uani d . . . 1 . . H H3A 0.7762 0.4856 0.6612 0.03 Uiso calc U . R 1 . . H H3B 0.6282 0.4989 0.5527 0.03 Uiso calc U . R 1 . . H H3C 0.6213 0.4777 0.7465 0.03 Uiso calc U . R 1 . . C C11 0.76958(17) 0.62043(9) 0.5853(2) 0.0139(5) Uani d . . . 1 . . H H11 0.7885 0.6661 0.6366 0.017 Uiso calc U . R 1 . . C C12 0.91999(18) 0.58940(9) 0.5513(2) 0.0168(5) Uani d . . . 1 . . H H12A 0.9729 0.5803 0.6597 0.02 Uiso calc U . R 1 . . H H12B 0.9061 0.5455 0.4919 0.02 Uiso calc U . R 1 . . C C13 1.01196(18) 0.63675(9) 0.4449(2) 0.0174(5) Uani d . . . 1 . . H H13A 1.0296 0.68 0.5059 0.021 Uiso calc U . R 1 . . H H13B 1.1079 0.6154 0.4258 0.021 Uiso calc U . R 1 . . C C14 0.93408(19) 0.65112(9) 0.2768(2) 0.0167(5) Uani d . . . 1 . . H H14 0.9224 0.6071 0.2152 0.02 Uiso calc U . R 1 . . C C15 0.78175(19) 0.67989(9) 0.3037(2) 0.0175(5) Uani d . . . 1 . . H H15A 0.7301 0.6861 0.1932 0.021 Uiso calc U . R 1 . . H H15B 0.791 0.725 0.3581 0.021 Uiso calc U . R 1 . . C C16 0.69108(18) 0.63299(9) 0.4134(2) 0.0163(5) Uani d . . . 1 . . H H16A 0.6749 0.5891 0.355 0.02 Uiso calc U . R 1 . . H H16B 0.5944 0.6539 0.4308 0.02 Uiso calc U . R 1 . . C C21 0.52175(18) 0.60666(8) 0.7251(2) 0.0137(5) Uani d . . . 1 . . H H21 0.4736 0.5995 0.6116 0.016 Uiso calc U . R 1 . . C C22 0.42800(19) 0.56877(9) 0.8516(2) 0.0181(5) Uani d . . . 1 . . H H22A 0.4306 0.5194 0.8276 0.022 Uiso calc U . R 1 . . H H22B 0.4697 0.576 0.9669 0.022 Uiso calc U . R 1 . . C C23 0.26917(18) 0.59346(9) 0.8423(2) 0.0180(5) Uani d . . . 1 . . H H23A 0.2254 0.5836 0.7292 0.022 Uiso calc U . R 1 . . H H23B 0.2122 0.5686 0.9261 0.022 Uiso calc U . R 1 . . C C24 0.26069(18) 0.66923(9) 0.8766(2) 0.0172(5) Uani d . . . 1 . . H H24 0.2984 0.6782 0.9941 0.021 Uiso calc U . R 1 . . C C25 0.35322(19) 0.70842(9) 0.7556(2) 0.0177(5) Uani d . . . 1 . . H H25A 0.3514 0.7573 0.7847 0.021 Uiso calc U . R 1 . . H H25B 0.3113 0.7032 0.6398 0.021 Uiso calc U . R 1 . . C C26 0.51215(19) 0.68303(9) 0.7622(2) 0.0166(5) Uani d . . . 1 . . H H26A 0.5686 0.7084 0.6788 0.02 Uiso calc U . R 1 . . H H26B 0.5568 0.6923 0.8751 0.02 Uiso calc U . R 1 . . 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 O1 0.0238(7) 0.0253(8) 0.0170(7) -0.0043(5) 0.0092(5) -0.0008(5) O2 0.0146(7) 0.0267(8) 0.0190(8) 0.0066(5) 0.0050(5) 0.0020(5) C1 0.0125(9) 0.0137(9) 0.0178(10) 0.0004(6) 0.0000(7) 0.0010(6) C2 0.0151(9) 0.0242(10) 0.0180(10) 0.0002(6) -0.0011(7) 0.0031(7) C3 0.0174(9) 0.0144(9) 0.0283(11) 0.0010(6) 0.0028(7) 0.0002(7) C11 0.0111(9) 0.0157(8) 0.0149(9) 0.0012(6) 0.0004(6) 0.0004(6) C12 0.0125(9) 0.0192(9) 0.0186(10) 0.0023(6) 0.0006(7) 0.0013(7) C13 0.0111(8) 0.0222(9) 0.0190(10) 0.0019(6) 0.0034(7) -0.0015(7) C14 0.0158(9) 0.0196(9) 0.0151(9) -0.0003(6) 0.0056(7) -0.0009(7) C15 0.0162(9) 0.0213(9) 0.0153(10) 0.0028(6) 0.0035(7) 0.0018(7) C16 0.0138(8) 0.0201(9) 0.0150(9) 0.0017(6) 0.0006(7) 0.0008(7) C21 0.0118(9) 0.0145(9) 0.0149(9) -0.0012(6) 0.0005(6) 0.0003(6) C22 0.0143(9) 0.0174(9) 0.0229(10) -0.0004(6) 0.0039(7) 0.0064(7) C23 0.0131(9) 0.0183(9) 0.0230(10) -0.0001(6) 0.0046(7) 0.0049(7) C24 0.0130(9) 0.0224(10) 0.0164(9) 0.0028(6) 0.0031(7) 0.0010(7) C25 0.0164(9) 0.0149(9) 0.0221(10) 0.0011(6) 0.0043(7) 0.0015(7) C26 0.0157(9) 0.0142(9) 0.0201(10) 0.0003(6) 0.0028(7) -0.0006(6) _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 O1 C14 . 1.434(2) ? O1 H1 . 0.94(3) ? O2 C24 . 1.441(2) ? O2 H2 . 0.93(4) ? C1 C3 . 1.539(2) ? C1 C2 . 1.541(2) ? C1 C21 . 1.564(2) ? C1 C11 . 1.564(2) ? C2 H2A . 0.98 ? C2 H2B . 0.98 ? C2 H2C . 0.98 ? C3 H3A . 0.98 ? C3 H3B . 0.98 ? C3 H3C . 0.98 ? C11 C12 . 1.538(2) ? C11 C16 . 1.540(2) ? C11 H11 . 1.0 ? C12 C13 . 1.531(2) ? C12 H12A . 0.99 ? C12 H12B . 0.99 ? C13 C14 . 1.518(3) ? C13 H13A . 0.99 ? C13 H13B . 0.99 ? C14 C15 . 1.526(2) ? C14 H14 . 1.0 ? C15 C16 . 1.535(2) ? C15 H15A . 0.99 ? C15 H15B . 0.99 ? C16 H16A . 0.99 ? C16 H16B . 0.99 ? C21 C26 . 1.535(2) ? C21 C22 . 1.539(2) ? C21 H21 . 1.0 ? C22 C23 . 1.531(2) ? C22 H22A . 0.99 ? C22 H22B . 0.99 ? C23 C24 . 1.518(3) ? C23 H23A . 0.99 ? C23 H23B . 0.99 ? C24 C25 . 1.515(2) ? C24 H24 . 1.0 ? C25 C26 . 1.536(2) ? C25 H25A . 0.99 ? C25 H25B . 0.99 ? C26 H26A . 0.99 ? C26 H26B . 0.99 ? 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 C14 O1 H1 . . 110.4(19) ? C24 O2 H2 . . 108.(2) ? C3 C1 C2 . . 108.28(14) ? C3 C1 C21 . . 109.37(13) ? C2 C1 C21 . . 110.32(14) ? C3 C1 C11 . . 110.04(14) ? C2 C1 C11 . . 107.89(13) ? C21 C1 C11 . . 110.90(13) ? C1 C2 H2A . . 109.5 ? C1 C2 H2B . . 109.5 ? H2A C2 H2B . . 109.5 ? C1 C2 H2C . . 109.5 ? H2A C2 H2C . . 109.5 ? H2B C2 H2C . . 109.5 ? C1 C3 H3A . . 109.5 ? C1 C3 H3B . . 109.5 ? H3A C3 H3B . . 109.5 ? C1 C3 H3C . . 109.5 ? H3A C3 H3C . . 109.5 ? H3B C3 H3C . . 109.5 ? C12 C11 C16 . . 107.36(14) ? C12 C11 C1 . . 113.28(13) ? C16 C11 C1 . . 115.74(14) ? C12 C11 H11 . . 106.6 ? C16 C11 H11 . . 106.6 ? C1 C11 H11 . . 106.6 ? C13 C12 C11 . . 111.65(14) ? C13 C12 H12A . . 109.3 ? C11 C12 H12A . . 109.3 ? C13 C12 H12B . . 109.3 ? C11 C12 H12B . . 109.3 ? H12A C12 H12B . . 108.0 ? C14 C13 C12 . . 110.51(14) ? C14 C13 H13A . . 109.5 ? C12 C13 H13A . . 109.5 ? C14 C13 H13B . . 109.5 ? C12 C13 H13B . . 109.5 ? H13A C13 H13B . . 108.1 ? O1 C14 C13 . . 111.60(14) ? O1 C14 C15 . . 110.85(14) ? C13 C14 C15 . . 110.32(14) ? O1 C14 H14 . . 108.0 ? C13 C14 H14 . . 108.0 ? C15 C14 H14 . . 108.0 ? C14 C15 C16 . . 111.82(14) ? C14 C15 H15A . . 109.3 ? C16 C15 H15A . . 109.3 ? C14 C15 H15B . . 109.3 ? C16 C15 H15B . . 109.3 ? H15A C15 H15B . . 107.9 ? C15 C16 C11 . . 110.93(14) ? C15 C16 H16A . . 109.5 ? C11 C16 H16A . . 109.5 ? C15 C16 H16B . . 109.5 ? C11 C16 H16B . . 109.5 ? H16A C16 H16B . . 108.0 ? C26 C21 C22 . . 108.15(14) ? C26 C21 C1 . . 114.35(13) ? C22 C21 C1 . . 114.09(14) ? C26 C21 H21 . . 106.6 ? C22 C21 H21 . . 106.6 ? C1 C21 H21 . . 106.6 ? C23 C22 C21 . . 111.43(14) ? C23 C22 H22A . . 109.3 ? C21 C22 H22A . . 109.3 ? C23 C22 H22B . . 109.3 ? C21 C22 H22B . . 109.3 ? H22A C22 H22B . . 108.0 ? C24 C23 C22 . . 110.96(14) ? C24 C23 H23A . . 109.4 ? C22 C23 H23A . . 109.4 ? C24 C23 H23B . . 109.4 ? C22 C23 H23B . . 109.4 ? H23A C23 H23B . . 108.0 ? O2 C24 C25 . . 108.87(14) ? O2 C24 C23 . . 110.82(14) ? C25 C24 C23 . . 110.64(14) ? O2 C24 H24 . . 108.8 ? C25 C24 H24 . . 108.8 ? C23 C24 H24 . . 108.8 ? C24 C25 C26 . . 111.27(14) ? C24 C25 H25A . . 109.4 ? C26 C25 H25A . . 109.4 ? C24 C25 H25B . . 109.4 ? C26 C25 H25B . . 109.4 ? H25A C25 H25B . . 108.0 ? C21 C26 C25 . . 111.88(14) ? C21 C26 H26A . . 109.2 ? C25 C26 H26A . . 109.2 ? C21 C26 H26B . . 109.2 ? C25 C26 H26B . . 109.2 ? H26A C26 H26B . . 107.9 ? 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 C3 C1 C11 C12 . . . . -50.75(18) ? C2 C1 C11 C12 . . . . 67.19(18) ? C21 C1 C11 C12 . . . . -171.89(13) ? C3 C1 C11 C16 . . . . 73.87(18) ? C2 C1 C11 C16 . . . . -168.19(14) ? C21 C1 C11 C16 . . . . -47.27(19) ? C16 C11 C12 C13 . . . . 59.48(19) ? C1 C11 C12 C13 . . . . -171.49(14) ? C11 C12 C13 C14 . . . . -59.47(19) ? C12 C13 C14 O1 . . . . 179.29(13) ? C12 C13 C14 C15 . . . . 55.59(19) ? O1 C14 C15 C16 . . . . -179.39(14) ? C13 C14 C15 C16 . . . . -55.3(2) ? C14 C15 C16 C11 . . . . 57.46(19) ? C12 C11 C16 C15 . . . . -57.91(18) ? C1 C11 C16 C15 . . . . 174.47(13) ? C3 C1 C21 C26 . . . . -175.74(15) ? C2 C1 C21 C26 . . . . 65.26(19) ? C11 C1 C21 C26 . . . . -54.21(19) ? C3 C1 C21 C22 . . . . 59.02(19) ? C2 C1 C21 C22 . . . . -59.98(19) ? C11 C1 C21 C22 . . . . -179.45(14) ? C26 C21 C22 C23 . . . . 57.43(19) ? C1 C21 C22 C23 . . . . -174.12(14) ? C21 C22 C23 C24 . . . . -58.4(2) ? C22 C23 C24 O2 . . . . 177.16(14) ? C22 C23 C24 C25 . . . . 56.3(2) ? O2 C24 C25 C26 . . . . -177.37(14) ? C23 C24 C25 C26 . . . . -55.4(2) ? C22 C21 C26 C25 . . . . -56.57(19) ? C1 C21 C26 C25 . . . . 175.12(14) ? C24 C25 C26 C21 . . . . 56.7(2) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H1 O2 4_675 0.94(3) 1.81(3) 2.7511(19) 179.(3) ? O2 H2 O1 1_456 0.93(4) 1.77(4) 2.6888(19) 172.(3) ? _shelx_res_file ; glo9770.res created by SHELXL-2014/7 TITL glo9770.res in P2(1)/c CELL 1.54178 9.1475 19.6782 7.9541 90.000 92.110 90.000 ZERR 4.000 0.0002 0.0005 0.0002 0.000 0.001 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H O UNIT 60 112 8 SIZE 0.056 0.148 0.152 TEMP -173.150 ACTA CONF L.S. 30 BOND $H FMAP 2 PLAN 10 EQIV $1 x+1, -y+3/2, z-1/2 HTAB O1 O2_$1 EQIV $2 x-1, y, z+1 HTAB O2 O1_$2 WGHT 0.137700 0.398900 EXTI 0.031017 FVAR 1.04449 O1 3 1.017283 0.696065 0.175527 11.00000 0.02381 0.02526 = 0.01698 -0.00083 0.00917 -0.00428 H1 2 1.048362 0.734367 0.238865 11.00000 0.03951 O2 3 0.111861 0.692934 0.859534 11.00000 0.01459 0.02672 = 0.01902 0.00204 0.00496 0.00659 H2 2 0.071815 0.691488 0.964643 11.00000 0.05403 C1 1 0.681351 0.578884 0.714983 11.00000 0.01246 0.01371 = 0.01784 0.00098 0.00000 0.00036 C2 1 0.762283 0.584650 0.887735 11.00000 0.01506 0.02423 = 0.01803 0.00314 -0.00111 0.00020 AFIX 137 H2A 2 0.705449 0.561675 0.972980 11.00000 -1.50000 H2B 2 0.774136 0.632689 0.917727 11.00000 -1.50000 H2C 2 0.858740 0.563252 0.882370 11.00000 -1.50000 AFIX 0 C3 1 0.676301 0.503417 0.664229 11.00000 0.01735 0.01440 = 0.02832 0.00025 0.00277 0.00103 AFIX 137 H3A 2 0.776180 0.485561 0.661221 11.00000 -1.50000 H3B 2 0.628185 0.498891 0.552662 11.00000 -1.50000 H3C 2 0.621321 0.477750 0.746491 11.00000 -1.50000 AFIX 0 C11 1 0.769580 0.620429 0.585278 11.00000 0.01106 0.01571 = 0.01494 0.00039 0.00041 0.00115 AFIX 13 H11 2 0.788499 0.666118 0.636642 11.00000 -1.20000 AFIX 0 C12 1 0.919991 0.589402 0.551271 11.00000 0.01247 0.01920 = 0.01860 0.00127 0.00058 0.00233 AFIX 23 H12A 2 0.972937 0.580326 0.659742 11.00000 -1.20000 H12B 2 0.906134 0.545523 0.491917 11.00000 -1.20000 AFIX 0 C13 1 1.011963 0.636748 0.444859 11.00000 0.01114 0.02221 = 0.01905 -0.00146 0.00345 0.00186 AFIX 23 H13A 2 1.029580 0.679987 0.505923 11.00000 -1.20000 H13B 2 1.107936 0.615389 0.425826 11.00000 -1.20000 AFIX 0 C14 1 0.934079 0.651115 0.276831 11.00000 0.01582 0.01958 = 0.01509 -0.00091 0.00559 -0.00026 AFIX 13 H14 2 0.922393 0.607051 0.215167 11.00000 -1.20000 AFIX 0 C15 1 0.781749 0.679891 0.303669 11.00000 0.01616 0.02132 = 0.01529 0.00183 0.00349 0.00278 AFIX 23 H15A 2 0.730145 0.686129 0.193151 11.00000 -1.20000 H15B 2 0.791040 0.724999 0.358133 11.00000 -1.20000 AFIX 0 C16 1 0.691080 0.632992 0.413435 11.00000 0.01378 0.02007 = 0.01497 0.00081 0.00061 0.00167 AFIX 23 H16A 2 0.674866 0.589057 0.355043 11.00000 -1.20000 H16B 2 0.594395 0.653941 0.430752 11.00000 -1.20000 AFIX 0 C21 1 0.521751 0.606656 0.725102 11.00000 0.01176 0.01454 = 0.01488 0.00032 0.00054 -0.00123 AFIX 13 H21 2 0.473627 0.599496 0.611560 11.00000 -1.20000 AFIX 0 C22 1 0.428000 0.568774 0.851640 11.00000 0.01426 0.01738 = 0.02288 0.00644 0.00385 -0.00035 AFIX 23 H22A 2 0.430576 0.519432 0.827636 11.00000 -1.20000 H22B 2 0.469651 0.576016 0.966889 11.00000 -1.20000 AFIX 0 C23 1 0.269171 0.593465 0.842343 11.00000 0.01307 0.01834 = 0.02296 0.00486 0.00457 -0.00009 AFIX 23 H23A 2 0.225435 0.583647 0.729249 11.00000 -1.20000 H23B 2 0.212184 0.568611 0.926076 11.00000 -1.20000 AFIX 0 C24 1 0.260693 0.669231 0.876555 11.00000 0.01296 0.02235 = 0.01641 0.00096 0.00307 0.00282 AFIX 13 H24 2 0.298352 0.678189 0.994087 11.00000 -1.20000 AFIX 0 C25 1 0.353216 0.708421 0.755599 11.00000 0.01637 0.01489 = 0.02209 0.00145 0.00434 0.00111 AFIX 23 H25A 2 0.351444 0.757321 0.784715 11.00000 -1.20000 H25B 2 0.311281 0.703221 0.639792 11.00000 -1.20000 AFIX 0 C26 1 0.512150 0.683029 0.762168 11.00000 0.01571 0.01423 = 0.02008 -0.00056 0.00285 0.00031 AFIX 23 H26A 2 0.568576 0.708363 0.678779 11.00000 -1.20000 H26B 2 0.556808 0.692264 0.875123 11.00000 -1.20000 AFIX 0 HKLF 4 REM glo9770.res in P2(1)/c REM R1 = 0.0729 for 2197 Fo > 4sig(Fo) and 0.0791 for all 2523 data REM 165 parameters refined using 0 restraints END WGHT 0.1378 0.3989 REM Highest difference peak 0.391, deepest hole -0.403, 1-sigma level 0.112 Q1 1 0.4667 0.6078 1.0036 11.00000 0.05 0.39 Q2 1 0.2562 0.6918 1.0365 11.00000 0.05 0.36 Q3 1 0.5510 0.5898 1.0226 11.00000 0.05 0.35 Q4 1 1.0173 0.6796 0.1983 11.00000 0.05 0.34 Q5 1 0.7096 0.4235 0.7827 11.00000 0.05 0.31 Q6 1 1.0231 0.6233 0.0745 11.00000 0.05 0.31 Q7 1 0.9814 0.7759 0.2808 11.00000 0.05 0.30 Q8 1 0.8249 0.6141 0.4008 11.00000 0.05 0.28 Q9 1 1.0868 0.6570 0.2424 11.00000 0.05 0.28 Q10 1 0.1936 0.7311 0.7555 11.00000 0.05 0.28 ; _shelx_res_checksum 7861 _shelx_hkl_file ; 0 0 1 2.10 5.30 0 0 -1 0.30 5.00 0 0 -3 -0.20 14.20 0 0 3 -1.00 7.30 0 0 -3 -1.00 10.40 0 0 4 633.44 61.69 0 0 -4 630.44 67.09 0 0 -5 -1.20 9.60 0 0 -5 -1.10 9.30 0 0 6 47.90 7.40 0 0 6 59.39 9.70 0 0 6 55.79 7.90 0 0 7 1.40 4.00 0 0 7 -1.10 2.80 0 0 7 5.00 3.90 0 0 8 1.90 3.40 0 0 -8 1.90 2.80 0 0 9 1.20 2.00 0 1 0 -1.00 2.40 0 1 0 0.10 2.80 0 -1 0 -1.30 2.80 0 -1 -1 859.11 56.49 0 -1 -1 765.42 55.69 0 -1 1 755.12 46.60 0 1 2 2307.27 144.39 0 1 -3 253.47 32.20 0 1 3 177.98 30.40 0 -1 3 220.58 26.70 0 -1 -3 165.98 33.50 0 1 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7 -2 4 9.10 3.60 7 -2 4 10.40 8.60 7 -2 4 1.40 6.90 7 2 5 1047.30 55.89 7 2 5 940.31 56.49 7 2 5 968.50 55.99 7 -2 5 1006.30 56.39 7 -2 5 975.60 55.49 7 -2 5 966.60 56.39 7 2 6 53.89 8.50 7 2 6 45.00 6.50 7 -2 6 48.40 6.20 7 -2 6 37.90 5.50 -7 3 7 2.50 2.40 7 3 -7 0.90 2.30 -7 -3 7 0.30 2.30 7 -3 -7 0.50 2.30 7 -3 -7 3.70 3.00 -7 3 6 19.80 5.10 7 3 -6 22.40 5.30 -7 3 6 20.50 4.90 -7 -3 6 19.00 4.90 -7 -3 6 24.10 4.70 7 -3 -6 21.30 5.20 -7 3 5 -3.40 3.10 7 3 -5 -2.90 5.00 -7 3 5 0.90 4.50 -7 -3 5 3.70 3.90 -7 -3 5 3.20 4.50 7 -3 -5 -1.40 4.70 -7 3 4 181.58 13.90 -7 3 4 170.08 13.60 7 3 -4 156.08 12.50 -7 3 4 166.68 12.90 7 3 -4 186.88 15.80 -7 -3 4 162.98 13.60 7 -3 -4 162.88 12.30 -7 -3 4 164.38 13.10 7 -3 -4 175.88 15.00 -7 3 3 360.66 23.30 -7 3 3 358.76 23.50 7 3 -3 366.86 24.50 7 3 -3 347.17 23.10 7 -3 -3 373.36 24.90 -7 -3 3 366.56 23.60 -7 -3 3 336.27 22.80 7 -3 -3 380.86 23.30 -7 3 2 2001.30 108.59 7 3 -2 1988.80 108.29 7 3 -2 2007.30 109.49 -7 3 2 2023.80 108.09 7 -3 -2 2052.29 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9.00 8 -4 -6 77.69 6.90 -8 4 5 48.90 6.50 -8 4 5 46.30 6.70 8 4 -5 57.09 7.70 -8 -4 5 47.70 6.60 8 -4 -5 60.19 6.00 -8 -4 5 36.50 5.90 8 -4 -5 51.99 7.70 8 4 -4 1.60 3.10 -8 4 4 -1.20 2.80 -8 4 4 -1.70 3.10 -8 4 4 -1.60 2.20 8 4 -4 4.00 3.80 -8 -4 4 -0.30 4.00 8 -4 -4 -2.20 2.60 8 -4 -4 2.00 3.50 8 -4 -4 0.60 5.50 -8 -4 4 1.70 3.40 8 4 -3 14.60 4.20 8 4 -3 6.40 4.30 -8 4 3 5.20 3.20 -8 4 3 14.90 4.40 8 -4 -3 -3.90 3.30 8 -4 -3 10.20 5.00 -8 -4 3 10.70 5.10 -8 -4 3 13.90 4.40 8 -4 -3 7.90 4.30 -8 4 2 2.30 4.50 8 4 -2 4.30 3.60 -8 -4 2 2.70 3.40 -8 -4 2 4.00 3.80 8 -4 -2 1.60 4.20 8 -4 -2 -0.10 5.20 8 4 -1 285.27 20.50 8 4 -1 273.27 19.60 8 4 -1 300.87 19.80 -8 4 1 298.77 19.80 -8 -4 1 257.27 19.10 -8 -4 1 293.97 20.10 8 -4 -1 285.87 19.20 8 -4 -1 297.77 20.40 8 -4 -1 288.07 20.90 8 4 0 23.60 6.40 8 4 0 57.49 8.50 8 4 0 28.30 5.70 8 4 0 30.70 4.70 8 -4 0 30.50 7.10 8 -4 0 25.20 5.80 8 -4 0 31.30 7.40 -8 -4 0 25.20 6.40 8 -4 0 35.50 4.90 8 4 1 329.07 22.20 8 4 1 342.37 24.90 8 4 1 383.96 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5 -3 246.38 18.00 8 -5 -3 230.78 16.70 -8 -5 3 212.78 15.80 8 -5 -3 228.78 19.00 -8 -5 3 242.68 17.60 -8 -5 2 15.70 3.80 8 5 -1 973.30 55.69 -8 5 1 975.40 55.59 8 5 -1 954.30 55.39 8 5 -1 951.80 56.09 -8 -5 1 993.80 55.69 -8 -5 1 926.51 54.89 8 -5 -1 992.90 57.29 8 -5 -1 1018.70 56.39 8 -5 -1 1042.60 55.79 8 5 0 105.19 10.90 8 5 0 93.49 7.70 8 5 0 107.39 11.00 8 5 0 62.59 9.20 8 -5 0 96.59 10.80 8 -5 0 83.19 7.90 8 -5 0 100.79 10.70 -8 -5 0 99.49 9.50 8 -5 0 100.19 9.50 8 5 1 432.96 28.60 8 5 1 438.66 26.50 8 5 1 448.56 27.70 8 -5 1 428.56 26.30 -8 -5 -1 411.66 27.30 8 -5 1 461.85 28.20 8 -5 1 449.36 28.60 8 5 2 7.90 3.20 8 5 2 9.00 4.70 8 5 2 8.60 4.70 8 -5 2 8.50 3.50 8 -5 2 3.10 4.80 8 -5 2 6.80 3.20 -8 -5 -2 3.10 3.50 8 -5 2 2.60 4.60 8 5 3 185.18 13.70 8 5 3 168.28 14.90 8 5 3 179.58 13.70 8 -5 3 178.08 14.70 8 -5 3 181.38 13.90 8 -5 3 176.48 13.60 -8 -5 -3 187.98 14.20 8 5 4 10.80 3.10 8 5 4 16.70 4.10 8 5 4 3.00 2.90 8 5 4 7.60 5.10 8 -5 4 16.10 3.90 -8 -5 -4 18.70 5.70 8 -5 4 11.70 4.80 8 5 5 4.80 2.50 8 5 5 2.70 4.20 8 5 5 5.00 2.20 8 -5 5 5.30 3.10 -8 -5 -5 5.00 3.60 8 -5 5 4.10 2.50 8 6 -6 280.27 17.70 -8 6 6 250.27 16.90 -8 -6 6 277.27 17.50 -8 6 5 10.50 4.60 8 6 -5 17.10 5.70 8 -6 -5 17.90 5.10 8 -6 -5 17.30 3.80 -8 -6 5 16.30 4.70 -8 6 4 21.20 5.60 -8 6 4 16.70 4.00 8 6 -4 23.10 6.40 8 6 -4 17.00 3.60 8 -6 -4 30.40 6.70 -8 -6 4 23.60 3.90 8 -6 -4 16.00 3.70 -8 -6 4 18.70 4.90 -8 6 3 1.30 2.90 8 6 -3 -0.50 4.70 8 6 -3 -1.80 2.40 8 -6 -3 3.10 3.40 8 -6 -3 8.10 3.60 -8 -6 3 2.40 3.00 8 -6 -3 4.80 5.90 -8 -6 3 1.40 3.00 -8 6 2 37.40 6.90 8 6 -2 38.50 7.80 8 6 -2 43.50 7.00 8 -6 -2 36.60 6.40 -8 -6 2 38.20 6.10 8 -6 -2 38.10 7.70 -8 -6 2 36.30 7.20 -8 -6 2 26.00 5.40 8 6 -1 29.40 6.30 -8 -6 1 31.20 6.20 8 -6 -1 28.60 7.50 -8 -6 1 24.70 6.50 8 -6 -1 50.29 11.50 8 -6 -1 33.00 8.30 -8 6 0 88.89 9.60 8 6 0 64.99 10.40 8 6 0 82.79 9.90 8 6 0 62.89 8.00 8 -6 0 92.49 9.70 8 -6 0 71.89 9.80 8 -6 0 82.09 10.70 8 -6 0 99.29 10.10 -8 -6 0 74.09 9.30 8 6 1 178.68 11.60 8 -6 1 129.59 14.00 8 -6 1 114.39 12.30 8 6 2 22.10 4.50 8 6 2 16.80 5.80 8 6 2 15.50 5.30 8 -6 2 17.30 4.50 -8 -6 -2 26.90 6.00 8 -6 2 17.60 5.90 8 -6 2 18.40 3.90 8 -6 2 13.40 5.40 8 6 3 6.10 4.00 8 6 3 13.40 5.20 8 6 3 10.10 4.10 8 -6 3 12.60 3.80 8 -6 3 14.40 5.10 -8 -6 -3 11.90 5.50 8 -6 3 12.80 4.40 8 6 4 48.30 7.60 8 6 4 45.90 6.80 -8 -6 -4 46.10 7.80 8 -6 4 44.40 5.70 8 -6 4 42.60 6.30 8 6 5 7.70 2.10 8 6 5 14.00 4.00 8 6 5 10.30 3.00 -8 -6 -5 13.10 3.50 8 -6 5 10.00 3.80 8 -6 5 9.10 3.40 -8 7 6 -1.40 1.80 8 7 -6 -0.70 2.00 8 -7 -6 0.20 1.50 8 -7 -6 -1.30 2.70 -8 -7 6 -0.80 1.80 -8 7 5 3.50 4.70 -8 7 5 2.30 1.30 8 -7 -5 4.40 3.60 8 -7 -5 1.30 2.10 -8 7 4 24.80 5.70 -8 7 4 33.80 4.70 8 7 -4 27.00 6.10 8 7 -4 33.30 4.50 8 -7 -4 27.70 6.50 -8 -7 4 29.20 6.10 8 7 -3 4.90 4.80 8 7 -3 13.40 4.20 -8 7 3 7.40 3.60 8 -7 -3 8.20 3.70 -8 -7 3 6.50 4.60 -8 -7 3 7.40 2.70 8 -7 -3 11.80 3.90 8 -7 -3 6.40 5.90 -8 7 2 -3.10 3.60 8 7 -2 6.90 3.90 8 7 -2 7.40 5.40 -8 -7 2 1.80 2.80 -8 -7 2 3.00 2.70 -8 -7 2 2.30 4.20 8 -7 -2 3.70 3.50 8 -7 -2 3.80 4.40 8 7 -1 177.88 15.00 8 7 -1 191.18 14.50 8 7 -1 201.48 15.00 -8 7 1 214.08 14.90 -8 -7 1 178.88 13.40 -8 -7 1 170.78 13.60 8 -7 -1 194.98 17.10 8 -7 -1 204.68 14.70 8 -7 -1 201.68 15.70 -8 -7 1 199.48 15.30 -8 7 0 49.99 7.40 8 7 0 37.30 8.20 8 7 0 37.90 4.70 8 7 0 40.20 7.30 8 -7 0 46.70 7.50 -8 -7 0 41.20 7.80 -8 -7 0 18.60 4.70 8 -7 0 39.80 5.40 8 -7 0 30.00 7.50 8 -7 0 36.30 8.50 8 7 1 5.50 3.70 8 7 1 0.00 3.50 8 7 1 2.70 3.00 8 -7 1 2.90 4.00 -8 -7 -1 3.30 3.20 8 -7 1 9.50 5.00 8 -7 1 1.30 5.10 8 7 2 78.69 11.00 8 7 2 86.69 8.00 8 7 2 81.39 9.40 -8 -7 -2 80.39 9.80 8 -7 2 93.19 10.10 8 -7 2 75.89 8.20 8 -7 2 78.29 10.00 8 -7 2 84.89 8.40 8 7 3 30.00 6.70 8 7 3 35.20 5.20 8 7 3 39.70 5.20 8 -7 3 37.00 6.30 -8 -7 -3 31.70 6.10 8 -7 3 29.70 6.40 8 -7 3 40.20 5.40 8 7 4 0.50 3.40 8 7 4 -0.50 2.40 -8 -7 -4 5.10 3.10 8 -7 4 3.40 3.20 8 -7 4 2.10 3.30 8 7 5 12.80 3.60 8 7 5 16.90 3.50 8 -7 5 16.30 4.40 -8 -7 -5 15.90 4.30 8 -7 5 12.30 3.70 -8 8 5 14.00 3.70 8 8 -5 8.50 4.80 -8 8 5 9.20 2.20 8 -8 -5 14.30 4.30 8 -8 -5 5.30 2.60 -8 -8 5 12.90 3.80 -8 8 4 29.50 5.40 -8 8 4 13.80 4.00 8 8 -4 24.50 5.50 8 8 -4 17.80 3.90 -8 -8 4 19.20 5.40 8 -8 -4 25.30 6.30 8 8 -3 12.50 4.00 8 8 -3 17.10 5.40 -8 8 3 12.40 4.50 -8 8 3 11.90 4.90 -8 -8 3 7.40 2.80 -8 -8 3 13.20 4.90 -8 -8 3 9.20 3.20 8 -8 -3 12.40 6.30 8 -8 -3 8.80 4.20 8 8 -2 231.38 16.30 8 8 -2 225.28 16.70 -8 8 2 224.38 16.10 -8 -8 2 209.68 15.20 8 -8 -2 219.88 16.00 8 -8 -2 223.88 17.80 -8 -8 2 228.48 16.30 8 8 -1 14.60 4.40 -8 8 1 11.20 4.80 8 8 -1 9.40 4.00 -8 -8 1 7.30 3.80 8 -8 -1 6.10 4.10 8 -8 -1 16.30 4.90 -8 -8 1 5.80 3.10 -8 -8 1 8.90 4.80 8 -8 -1 12.40 5.80 -8 8 0 123.89 10.30 8 8 0 85.49 7.90 8 8 0 109.69 10.60 8 8 0 120.29 10.80 -8 -8 0 113.59 9.40 8 -8 0 112.19 12.40 8 -8 0 124.99 10.80 -8 -8 0 113.79 10.30 8 -8 0 111.79 11.70 8 -8 0 104.69 8.50 8 8 1 9.90 5.40 8 8 1 8.90 5.30 8 8 1 16.50 4.10 -8 8 -1 16.10 4.30 8 -8 1 13.10 4.30 8 -8 1 13.60 4.90 8 -8 1 10.10 5.40 8 -8 1 9.60 5.80 -8 -8 -1 18.20 3.70 -8 -8 -1 17.70 5.50 8 8 2 1.70 3.20 8 8 2 4.60 4.00 8 8 2 -2.60 3.10 -8 -8 -2 3.50 3.30 8 -8 2 0.90 3.40 8 -8 2 -3.00 3.40 8 -8 2 8.60 5.20 8 -8 2 1.80 3.30 8 8 3 81.89 11.20 8 8 3 91.79 8.40 8 8 3 95.29 8.70 -8 -8 -3 95.49 10.70 8 -8 3 91.89 9.20 8 -8 3 106.89 10.10 8 -8 3 86.29 8.20 8 8 4 116.69 11.40 8 8 4 105.29 8.90 -8 -8 -4 117.29 10.60 8 -8 4 103.89 10.20 8 -8 4 101.39 9.20 8 8 5 15.90 3.60 8 8 5 12.90 3.20 -8 -8 -5 26.80 4.30 8 -8 5 12.70 3.80 8 -8 5 15.60 3.60 -8 9 5 0.20 1.80 -8 9 5 0.60 3.10 8 9 -5 1.10 3.10 -8 -9 5 3.30 3.40 8 -9 -5 -1.00 2.70 8 9 -4 0.10 3.10 -8 9 4 1.70 3.70 8 9 -4 0.50 2.50 -8 9 4 4.10 3.90 -8 -9 4 2.30 3.00 8 -9 -4 -4.00 1.90 8 -9 -4 1.70 3.60 -8 9 3 24.20 5.60 8 9 -3 19.40 5.10 8 9 -3 16.30 5.60 -8 9 3 28.00 5.20 8 -9 -3 23.30 5.10 -8 -9 3 30.20 5.50 -8 -9 3 17.60 4.60 8 -9 -3 19.60 6.80 8 9 -2 39.30 7.10 -8 9 2 36.00 5.90 8 -9 -2 41.90 7.90 -8 -9 2 35.80 6.70 -8 -9 2 42.30 6.30 8 -9 -2 45.30 7.50 8 9 -1 28.70 5.70 8 9 -1 39.00 5.70 8 9 -1 20.00 5.40 -8 9 1 20.20 5.40 8 -9 -1 27.80 6.20 8 -9 -1 21.30 6.70 -8 -9 1 32.10 6.10 -8 -9 1 31.10 5.40 8 -9 -1 25.60 5.80 8 9 0 140.49 12.60 8 9 0 132.29 10.20 8 9 0 148.09 11.90 -8 9 0 153.98 11.60 -8 -9 0 134.59 10.80 8 -9 0 153.88 14.00 -8 -9 0 103.79 10.00 8 -9 0 157.08 13.30 -8 -9 0 140.79 12.30 8 -9 0 147.59 12.10 8 -9 0 122.89 9.80 8 9 1 61.39 8.90 8 9 1 68.09 8.00 8 9 1 53.59 5.80 -8 9 -1 66.89 7.60 -8 -9 -1 50.39 8.50 8 -9 1 73.99 8.20 8 -9 1 64.49 8.80 8 -9 1 66.29 9.30 8 -9 1 64.59 6.30 8 -9 1 59.09 7.60 -8 -9 -1 50.89 6.70 -8 9 -2 384.46 27.40 8 9 2 345.37 23.40 8 9 2 386.86 25.90 8 9 2 427.76 25.00 8 -9 2 352.86 23.90 -8 -9 -2 406.26 25.10 8 -9 2 420.66 25.40 8 -9 2 404.96 25.60 8 -9 2 383.66 23.60 8 9 3 -0.70 2.10 -8 9 -3 -0.40 2.00 8 9 3 2.10 2.70 8 9 3 3.00 4.60 -8 -9 -3 0.80 3.20 8 -9 3 1.70 2.70 8 -9 3 -0.70 1.30 8 -9 3 -4.60 3.50 8 9 4 4.90 3.90 8 9 4 4.80 2.80 -8 -9 -4 4.20 4.50 8 -9 4 3.80 3.10 8 -9 4 6.50 2.90 8 9 5 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1.70 -10 -8 2 0.70 2.40 -10 8 1 42.90 5.00 10 8 -1 51.69 5.60 10 -8 -1 44.30 5.30 10 -8 -1 49.99 5.20 10 -8 -1 53.99 4.80 -10 -8 1 49.80 5.20 10 8 0 0.60 2.30 -10 8 0 3.00 1.90 10 -8 0 -0.50 1.90 10 -8 0 -4.70 2.00 10 -8 0 2.20 2.40 -10 -8 0 2.30 1.40 -10 -8 0 3.30 3.10 10 8 1 6.40 2.40 10 -8 1 1.40 2.50 10 -8 1 0.60 1.50 10 -8 1 0.60 1.30 -10 -8 -1 1.20 2.00 -10 -8 -1 1.60 1.60 10 9 -1 14.20 3.70 -10 -9 1 31.60 4.10 10 -9 -1 23.90 3.60 -10 9 0 3.40 2.00 10 9 0 9.10 2.60 -10 -9 0 9.80 2.80 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 22904 #============================================================================= # end of cif data for "glo9770" (compound 2o) #============================================================================= #============================================================================= # end of cif file #=============================================================================