# Electronic Supplementary Material (ESI) for Chemical Science. # This journal is © The Royal Society of Chemistry 2023 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_rjii-95 _database_code_depnum_ccdc_archive 'CCDC 2207616' loop_ _audit_author_name _audit_author_address 'Richard Staples' ;Michigan State University United States of America ; _audit_update_record ; 2022-09-15 deposited with the CCDC. 2023-03-21 downloaded from the CCDC. ; _audit_creation_date 2022-07-15 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _shelxl_version_number 2013-3 loop_ _audit_author_email jenarash@msu.edu _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C72 H100 N2 Y, C4 H8 O' _chemical_formula_sum 'C76 H108 N2 O Y' _chemical_formula_weight 1154.55 _chemical_melting_point ? _chemical_oxdiff_formula C72H100N2Y _chemical_oxdiff_usercomment 3-22-21 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' Y Y -0.2670 2.0244 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.0163(3) _cell_length_b 17.0386(3) _cell_length_c 22.7773(4) _cell_angle_alpha 90 _cell_angle_beta 106.062(2) _cell_angle_gamma 90 _cell_volume 6719.1(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 14802 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 75.4650 _cell_measurement_theta_min 3.6150 _shelx_estimated_absorpt_T_max 0.964 _shelx_estimated_absorpt_T_min 0.892 _exptl_absorpt_coefficient_mu 1.539 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.835 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.100a (Rigaku Oxford Diffraction, 2021) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'metallic light brown' _exptl_crystal_colour_lustre metallic _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary brown _exptl_crystal_density_diffrn 1.141 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description irregular _exptl_crystal_F_000 2500 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -9 -4 -5 0.0265 -5 -1 15 0.0401 8 3 -13 0.0252 9 -4 3 0.0027 6 7 5 0.0323 -7 8 -1 0.0198 1 -2 0 0.0038 _exptl_crystal_size_max 0.076 _exptl_crystal_size_mid 0.059 _exptl_crystal_size_min 0.024 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -8.6833 -4.1366 -4.8504 0.0043 0.0081 1.0000 -4.9751 -1.2274 14.5001 0.3299 0.9320 -0.1504 8.0582 2.7141 -12.5064 -0.3263 -0.9202 -0.2160 9.4373 -4.1486 3.1905 0.6607 -0.2331 -0.7135 6.3624 7.4618 4.8496 -0.3386 0.1212 -0.9331 -7.0296 8.4328 -0.9711 -0.9005 0.3186 0.2961 1.0032 -1.9965 -0.0027 0.1908 -0.0634 -0.0100 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_unetI/netI 0.0278 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.938 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 23782 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.938 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.963 _diffrn_reflns_theta_min 3.640 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.938 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -4.00 22.00 0.50 12.00 -- -47.36 94.00-133.00 52 2 \w 17.00 43.00 0.50 12.00 -- 47.36 -94.00 115.00 52 3 \w -72.00 -46.00 0.50 48.00 -- -91.75 94.00-133.00 52 4 \w -159.00 -85.00 0.50 48.00 -- -91.75 -94.00 115.00 148 5 \w 127.00 153.00 0.50 48.00 -- 106.58 94.00-133.00 52 6 \w 40.00 102.00 0.50 48.00 -- 106.58 -94.00 115.00 124 7 \w -26.00 26.00 0.50 12.00 -- -47.36 19.00 -30.00 104 8 \w -16.00 25.00 0.50 12.00 -- -47.36 19.00-150.00 82 9 \w -26.00 10.00 0.50 12.00 -- 47.36 -19.00-180.00 72 10 \w 46.00 120.00 0.50 12.00 -- 47.36 19.00 -30.00 148 11 \w -162.00-127.00 0.50 48.00 -- -91.75 -77.00 30.00 70 12 \w -50.00 -21.00 0.50 48.00 -- -91.75 45.00 0.00 58 13 \w -162.00-137.00 0.50 48.00 -- -91.75 -77.00 0.00 50 14 \w -47.00 -20.00 0.50 48.00 -- -91.75 45.00 60.00 54 15 \w -52.00 -22.00 0.50 48.00 -- -91.75 45.00 150.00 60 16 \w -158.00-133.00 0.50 48.00 -- -91.75 -61.00 -90.00 50 17 \w -153.00-122.00 0.50 48.00 -- -91.75 -45.00-120.00 62 18 \w -72.00 -31.00 0.50 48.00 -- -91.75 61.00-150.00 82 19 \w 37.00 65.00 0.50 48.00 -- 106.58 -61.00 -90.00 56 20 \w 144.00 178.00 0.50 48.00 -- 106.58 45.00 120.00 68 21 \w 37.00 70.00 0.50 48.00 -- 106.58 -61.00-180.00 66 22 \w 145.00 177.00 0.50 48.00 -- 106.58 125.00 -60.00 64 23 \w 39.00 69.00 0.50 48.00 -- 106.58 -61.00 -60.00 60 24 \w 45.00 70.00 0.50 48.00 -- 106.58 -61.00 120.00 50 25 \w 127.00 177.00 0.50 48.00 -- 106.58 61.00-180.00 100 26 \w 40.00 66.00 0.50 48.00 -- 106.58 -61.00 150.00 52 27 \w 127.00 173.00 0.50 48.00 -- 106.58 77.00 -90.00 92 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0253286000 _diffrn_orient_matrix_UB_12 -0.0828540000 _diffrn_orient_matrix_UB_13 0.0244312000 _diffrn_orient_matrix_UB_21 -0.0367281000 _diffrn_orient_matrix_UB_22 0.0132454000 _diffrn_orient_matrix_UB_23 0.0527913000 _diffrn_orient_matrix_UB_31 -0.0769941000 _diffrn_orient_matrix_UB_32 -0.0336392000 _diffrn_orient_matrix_UB_33 -0.0396349000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6185 _reflns_number_total 6674 _reflns_odcompleteness_completeness 99.57 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.41.100a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.41.100a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.100a (Rigaku OD, 2021)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2013/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _refine_diff_density_max 0.594 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.059 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 427 _refine_ls_number_reflns 6674 _refine_ls_number_restraints 198 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0417 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+10.2826P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1130 _refine_ls_wR_factor_ref 0.1150 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C11-C12 \\sim C12-C13 \\sim C13-C14 with sigma of 0.02 O1-C8 \\sim O1-C9 with sigma of 0.04 O2-C11 \\sim O2-C14 with sigma of 0.02 O2-C12 \\sim O2-C13 with sigma of 0.04 C8-C10 \\sim C7-C9 with sigma of 0.04 C12-C14 \\sim C11-C13 with sigma of 0.04 C7-C8 \\sim C8-C9 \\sim C9-C10 with sigma of 0.02 O1-C7 \\sim O1-C10 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints O2 \\sim C11 \\sim C12 \\sim C13 \\sim C14: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A O1 \\sim C7 \\sim C8 \\sim C9 \\sim C10: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A 4. Rigid body (RIGU) restrains O2, C11, C12, C13, C14 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O1, C7, C8, C9, C10 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Fixed Sof: O1(0.25) C7(0.25) H7A(0.25) H7B(0.25) C8(0.25) H8A(0.25) H8B(0.25) C9(0.25) H9A(0.25) H9B(0.25) C10(0.25) H10A(0.25) H10B(0.25) O2(0.25) C11(0.25) H3A(0.25) H3B(0.25) C12(0.25) H4A(0.25) H4B(0.25) C13(0.25) H5A(0.25) H5B(0.25) C14(0.25) H6A(0.25) H6B(0.25) 6.a Free rotating group: O1(C7,C8,C9,C10), O2(C11,C12,C13,C14) 6.b Ternary CH refined with riding coordinates: C221(H221), C241(H241), C261(H261), C621(H621), C641(H641), C661(H661) 6.c Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H3A,H3B), C12(H4A, H4B), C13(H5A,H5B), C14(H6A,H6B) 6.d Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C23(H23), C25(H25), C63(H63), C65(H65) 6.e Idealised Me refined as rotating group: C222(H222,H223,H224), C223(H225,H226,H227), C242(H242,H243,H244), C243(H245, H246,H247), C262(H262,H263,H264), C263(H265,H266,H267), C622(H622,H623,H624), C623(H625,H626,H627), C642(H642,H643,H644), C643(H645,H646,H647), C662(H662, H663,H664), C663(H665,H666,H667) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.5000 0.39593(2) 0.7500 0.02766(10) Uani 1 2 d S T P . . N1 N 0.52790(10) 0.31270(10) 0.68166(8) 0.0269(3) Uani 1 1 d . . . . . H1 H 0.4952(14) 0.2733(15) 0.6639(11) 0.030(6) Uiso 1 1 d . . . . . C1 C 0.59300(11) 0.30745(11) 0.66096(9) 0.0249(4) Uani 1 1 d . . . . . C2 C 0.65517(11) 0.35925(11) 0.68630(9) 0.0259(4) Uani 1 1 d . . . . . C3 C 0.72068(12) 0.36003(12) 0.66550(9) 0.0288(4) Uani 1 1 d . . . . . H3 H 0.7618 0.3950 0.6834 0.035 Uiso 1 1 calc R U . . . C4 C 0.72661(12) 0.30985(12) 0.61847(10) 0.0324(4) Uani 1 1 d . . . . . H4 H 0.7703 0.3120 0.6029 0.039 Uiso 1 1 calc R U . . . C5 C 0.66742(12) 0.25684(12) 0.59501(10) 0.0308(4) Uani 1 1 d . . . . . H5 H 0.6719 0.2216 0.5639 0.037 Uiso 1 1 calc R U . . . C6 C 0.60137(12) 0.25366(11) 0.61574(9) 0.0268(4) Uani 1 1 d . . . . . C21 C 0.64548(11) 0.40989(11) 0.73696(9) 0.0256(4) Uani 1 1 d . . . . . C22 C 0.65885(12) 0.37478(12) 0.79667(9) 0.0278(4) Uani 1 1 d . . . . . C23 C 0.64736(12) 0.42076(12) 0.84481(9) 0.0292(4) Uani 1 1 d . . . . . H23 H 0.6596 0.3988 0.8847 0.035 Uiso 1 1 calc R U . . . C24 C 0.61872(12) 0.49702(12) 0.83627(9) 0.0289(4) Uani 1 1 d . . . . . C25 C 0.59784(12) 0.52678(12) 0.77577(9) 0.0300(4) Uani 1 1 d . . . . . H25 H 0.5706 0.5751 0.7676 0.036 Uiso 1 1 calc R U . . . C26 C 0.61625(11) 0.48681(11) 0.72732(9) 0.0259(4) Uani 1 1 d . . . . . C61 C 0.54159(12) 0.19158(11) 0.59310(9) 0.0266(4) Uani 1 1 d . . . . . C62 C 0.55057(12) 0.11767(12) 0.62207(9) 0.0276(4) Uani 1 1 d . . . . . C63 C 0.49355(12) 0.06092(12) 0.60184(10) 0.0296(4) Uani 1 1 d . . . . . H63 H 0.4994 0.0114 0.6218 0.035 Uiso 1 1 calc R U . . . C64 C 0.42836(12) 0.07447(12) 0.55332(9) 0.0283(4) Uani 1 1 d . . . . . C65 C 0.42093(12) 0.14734(12) 0.52484(9) 0.0303(4) Uani 1 1 d . . . . . H65 H 0.3771 0.1572 0.4912 0.036 Uiso 1 1 calc R U . . . C66 C 0.47585(12) 0.20641(12) 0.54409(9) 0.0291(4) Uani 1 1 d . . . . . C221 C 0.69939(12) 0.29567(12) 0.80966(9) 0.0287(4) Uani 1 1 d . . . . . H221 H 0.6837 0.2640 0.7712 0.034 Uiso 1 1 calc R U . . . C222 C 0.78713(14) 0.30888(14) 0.82515(12) 0.0422(5) Uani 1 1 d . . . . . H222 H 0.7994 0.3377 0.7918 0.063 Uiso 1 1 calc R U . . . H223 H 0.8136 0.2581 0.8306 0.063 Uiso 1 1 calc R U . . . H224 H 0.8043 0.3394 0.8630 0.063 Uiso 1 1 calc R U . . . C223 C 0.68020(15) 0.24810(14) 0.85997(12) 0.0415(5) Uani 1 1 d . . . . . H225 H 0.7048 0.1964 0.8627 0.062 Uiso 1 1 calc R U . . . H226 H 0.6241 0.2416 0.8506 0.062 Uiso 1 1 calc R U . . . H227 H 0.6993 0.2756 0.8990 0.062 Uiso 1 1 calc R U . . . C241 C 0.61521(13) 0.55126(13) 0.88817(10) 0.0341(5) Uani 1 1 d . . . . . H241 H 0.5627 0.5757 0.8774 0.041 Uiso 1 1 calc R U . . . C242 C 0.67440(18) 0.61743(16) 0.89440(14) 0.0526(7) Uani 1 1 d . . . . . H242 H 0.6653 0.6451 0.8553 0.079 Uiso 1 1 calc R U . . . H243 H 0.7266 0.5952 0.9058 0.079 Uiso 1 1 calc R U . . . H244 H 0.6692 0.6543 0.9261 0.079 Uiso 1 1 calc R U . . . C243 C 0.62777(15) 0.51085(16) 0.94960(10) 0.0426(6) Uani 1 1 d . . . . . H245 H 0.6805 0.4901 0.9629 0.064 Uiso 1 1 calc R U . . . H246 H 0.5908 0.4677 0.9457 0.064 Uiso 1 1 calc R U . . . H247 H 0.6201 0.5487 0.9798 0.064 Uiso 1 1 calc R U . . . C261 C 0.60541(12) 0.53356(12) 0.66854(9) 0.0285(4) Uani 1 1 d . . . . . H261 H 0.5664 0.5751 0.6691 0.034 Uiso 1 1 calc R U . . . C262 C 0.68064(13) 0.57672(14) 0.67125(11) 0.0369(5) Uani 1 1 d . . . . . H262 H 0.6723 0.6128 0.6365 0.055 Uiso 1 1 calc R U . . . H263 H 0.7206 0.5386 0.6695 0.055 Uiso 1 1 calc R U . . . H264 H 0.6972 0.6065 0.7095 0.055 Uiso 1 1 calc R U . . . C263 C 0.57518(13) 0.49007(13) 0.60785(10) 0.0333(5) Uani 1 1 d . . . . . H265 H 0.5539 0.5280 0.5752 0.050 Uiso 1 1 calc R U . . . H266 H 0.5347 0.4532 0.6109 0.050 Uiso 1 1 calc R U . . . H267 H 0.6176 0.4612 0.5986 0.050 Uiso 1 1 calc R U . . . C621 C 0.62046(12) 0.09852(12) 0.67553(10) 0.0312(4) Uani 1 1 d . . . . . H621 H 0.6595 0.1410 0.6778 0.037 Uiso 1 1 calc R U . . . C622 C 0.59850(15) 0.09963(18) 0.73517(12) 0.0480(6) Uani 1 1 d . . . . . H622 H 0.6450 0.0934 0.7694 0.072 Uiso 1 1 calc R U . . . H623 H 0.5626 0.0565 0.7355 0.072 Uiso 1 1 calc R U . . . H624 H 0.5736 0.1497 0.7392 0.072 Uiso 1 1 calc R U . . . C623 C 0.65816(15) 0.02124(15) 0.66658(12) 0.0451(6) Uani 1 1 d . . . . . H625 H 0.7057 0.0140 0.6997 0.068 Uiso 1 1 calc R U . . . H626 H 0.6705 0.0220 0.6273 0.068 Uiso 1 1 calc R U . . . H627 H 0.6226 -0.0221 0.6670 0.068 Uiso 1 1 calc R U . . . C641 C 0.36512(13) 0.01338(12) 0.53371(10) 0.0315(4) Uani 1 1 d . . . . . H641 H 0.3309 0.0299 0.4931 0.038 Uiso 1 1 calc R U . . . C642 C 0.31583(14) 0.01165(15) 0.57858(11) 0.0408(5) Uani 1 1 d . . . . . H642 H 0.2747 -0.0274 0.5652 0.061 Uiso 1 1 calc R U . . . H643 H 0.2929 0.0635 0.5800 0.061 Uiso 1 1 calc R U . . . H644 H 0.3483 -0.0022 0.6194 0.061 Uiso 1 1 calc R U . . . C643 C 0.39569(15) -0.06819(14) 0.52609(12) 0.0421(5) Uani 1 1 d . . . . . H645 H 0.4275 -0.0871 0.5657 0.063 Uiso 1 1 calc R U . . . H646 H 0.4270 -0.0659 0.4971 0.063 Uiso 1 1 calc R U . . . H647 H 0.3522 -0.1041 0.5105 0.063 Uiso 1 1 calc R U . . . C661 C 0.46609(14) 0.28464(13) 0.51043(10) 0.0357(5) Uani 1 1 d . . . . . H661 H 0.4961 0.3250 0.5392 0.043 Uiso 1 1 calc R U . . . C662 C 0.38202(15) 0.31206(14) 0.48908(11) 0.0414(5) Uani 1 1 d . . . . . H662 H 0.3800 0.3652 0.4723 0.062 Uiso 1 1 calc R U . . . H663 H 0.3598 0.3122 0.5238 0.062 Uiso 1 1 calc R U . . . H664 H 0.3524 0.2763 0.4575 0.062 Uiso 1 1 calc R U . . . C663 C 0.49992(17) 0.27955(17) 0.45613(13) 0.0508(6) Uani 1 1 d . . . . . H665 H 0.4716 0.2401 0.4272 0.076 Uiso 1 1 calc R U . . . H666 H 0.5545 0.2645 0.4705 0.076 Uiso 1 1 calc R U . . . H667 H 0.4955 0.3307 0.4358 0.076 Uiso 1 1 calc R U . . . O1 O 1.0631(7) 0.3183(8) 0.8132(4) 0.118(4) Uani 0.25 1 d DG U P A -2 C7 C 1.0279(7) 0.3801(6) 0.7720(5) 0.084(3) Uani 0.25 1 d DG U P A -2 H7A H 1.0613 0.4273 0.7791 0.100 Uiso 0.25 1 calc R U P A -2 H7B H 0.9772 0.3944 0.7779 0.100 Uiso 0.25 1 calc R U P A -2 C8 C 1.0178(8) 0.3482(8) 0.7074(5) 0.088(3) Uani 0.25 1 d DG U P A -2 H8A H 1.0643 0.3581 0.6934 0.105 Uiso 0.25 1 calc R U P A -2 H8B H 0.9722 0.3715 0.6779 0.105 Uiso 0.25 1 calc R U P A -2 C9 C 1.0064(8) 0.2601(7) 0.7164(6) 0.104(3) Uani 0.25 1 d DG U P A -2 H9A H 0.9522 0.2481 0.7151 0.125 Uiso 0.25 1 calc R U P A -2 H9B H 1.0214 0.2284 0.6851 0.125 Uiso 0.25 1 calc R U P A -2 C10 C 1.0610(8) 0.2461(7) 0.7802(6) 0.105(3) Uani 0.25 1 d DG U P A -2 H10A H 1.0416 0.2028 0.8009 0.126 Uiso 0.25 1 calc R U P A -2 H10B H 1.1133 0.2323 0.7774 0.126 Uiso 0.25 1 calc R U P A -2 O2 O 1.0179(7) 0.3178(6) 0.8164(5) 0.083(3) Uani 0.25 1 d DG U P B -1 C11 C 1.0564(7) 0.3670(5) 0.7829(5) 0.078(3) Uani 0.25 1 d DG U P B -1 H3A H 1.0988 0.3966 0.8112 0.094 Uiso 0.25 1 calc R U P B -1 H3B H 1.0197 0.4049 0.7573 0.094 Uiso 0.25 1 calc R U P B -1 C12 C 1.0886(7) 0.3120(9) 0.7426(6) 0.106(3) Uani 0.25 1 d DG U P B -1 H4A H 1.1408 0.2929 0.7644 0.127 Uiso 0.25 1 calc R U P B -1 H4B H 1.0904 0.3380 0.7042 0.127 Uiso 0.25 1 calc R U P B -1 C13 C 1.0292(8) 0.2450(7) 0.7304(5) 0.089(3) Uani 0.25 1 d DG U P B -1 H5A H 0.9831 0.2580 0.6965 0.107 Uiso 0.25 1 calc R U P B -1 H5B H 1.0519 0.1953 0.7209 0.107 Uiso 0.25 1 calc R U P B -1 C14 C 1.0093(8) 0.2399(5) 0.7915(6) 0.090(3) Uani 0.25 1 d DG U P B -1 H6A H 0.9556 0.2212 0.7851 0.108 Uiso 0.25 1 calc R U P B -1 H6B H 1.0447 0.2032 0.8195 0.108 Uiso 0.25 1 calc R U P B -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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.04199(16) 0.01772(14) 0.02493(14) 0.000 0.01201(10) 0.000 N1 0.0301(8) 0.0228(8) 0.0273(8) -0.0035(7) 0.0070(7) -0.0032(7) C1 0.0306(9) 0.0185(9) 0.0243(9) 0.0016(7) 0.0053(7) -0.0011(7) C2 0.0325(9) 0.0192(9) 0.0246(10) 0.0007(7) 0.0056(8) -0.0010(7) C3 0.0321(10) 0.0215(9) 0.0316(10) -0.0008(8) 0.0067(8) -0.0035(8) C4 0.0352(10) 0.0277(10) 0.0367(11) -0.0027(8) 0.0139(9) -0.0020(8) C5 0.0401(11) 0.0233(10) 0.0305(11) -0.0048(8) 0.0125(9) -0.0004(8) C6 0.0344(10) 0.0190(9) 0.0263(10) -0.0013(7) 0.0073(8) -0.0020(8) C21 0.0316(9) 0.0181(9) 0.0254(10) -0.0015(7) 0.0050(8) -0.0034(7) C22 0.0344(10) 0.0204(9) 0.0264(10) 0.0005(7) 0.0050(8) -0.0003(8) C23 0.0369(10) 0.0255(10) 0.0223(10) 0.0004(8) 0.0033(8) -0.0018(8) C24 0.0347(10) 0.0239(10) 0.0265(10) -0.0036(8) 0.0056(8) -0.0026(8) C25 0.0399(11) 0.0198(9) 0.0298(10) -0.0018(8) 0.0088(8) 0.0004(8) C26 0.0318(9) 0.0182(9) 0.0255(10) -0.0001(7) 0.0045(8) -0.0026(7) C61 0.0357(10) 0.0196(9) 0.0255(10) -0.0050(7) 0.0104(8) -0.0018(8) C62 0.0326(10) 0.0219(9) 0.0284(10) -0.0028(8) 0.0086(8) -0.0001(8) C63 0.0360(10) 0.0199(9) 0.0323(11) -0.0006(8) 0.0087(8) -0.0014(8) C64 0.0357(10) 0.0237(10) 0.0259(10) -0.0053(8) 0.0092(8) -0.0036(8) C65 0.0374(10) 0.0262(10) 0.0244(10) -0.0021(8) 0.0039(8) -0.0022(8) C66 0.0400(11) 0.0213(9) 0.0259(10) -0.0023(7) 0.0091(8) -0.0014(8) C221 0.0346(10) 0.0203(9) 0.0286(10) 0.0021(7) 0.0043(8) 0.0018(8) C222 0.0403(12) 0.0319(12) 0.0500(14) 0.0061(10) 0.0051(10) 0.0022(9) C223 0.0508(13) 0.0319(12) 0.0440(13) 0.0111(10) 0.0169(11) 0.0100(10) C241 0.0413(11) 0.0299(11) 0.0303(11) -0.0060(8) 0.0084(9) -0.0004(9) C242 0.0637(17) 0.0421(14) 0.0548(16) -0.0225(12) 0.0209(13) -0.0168(13) C243 0.0477(13) 0.0507(14) 0.0259(11) -0.0054(10) 0.0042(9) 0.0083(11) C261 0.0362(10) 0.0209(9) 0.0268(10) 0.0022(7) 0.0062(8) -0.0003(8) C262 0.0432(12) 0.0323(11) 0.0339(11) 0.0059(9) 0.0083(9) -0.0081(9) C263 0.0420(11) 0.0249(10) 0.0288(11) 0.0024(8) 0.0027(9) 0.0012(9) C621 0.0325(10) 0.0240(10) 0.0346(11) -0.0007(8) 0.0053(9) -0.0014(8) C622 0.0424(13) 0.0644(18) 0.0332(13) -0.0009(11) 0.0037(10) 0.0060(12) C623 0.0447(13) 0.0374(13) 0.0482(14) -0.0032(11) 0.0044(11) 0.0116(10) C641 0.0379(11) 0.0267(10) 0.0283(10) -0.0039(8) 0.0064(8) -0.0067(8) C642 0.0422(12) 0.0411(13) 0.0413(13) -0.0108(10) 0.0150(10) -0.0125(10) C643 0.0492(13) 0.0299(12) 0.0473(14) -0.0146(10) 0.0138(11) -0.0092(10) C661 0.0490(12) 0.0237(10) 0.0302(11) 0.0015(8) 0.0038(9) -0.0044(9) C662 0.0564(14) 0.0308(12) 0.0354(12) 0.0067(9) 0.0100(10) 0.0067(10) C663 0.0604(16) 0.0439(14) 0.0533(16) 0.0210(12) 0.0246(13) 0.0041(12) O1 0.101(9) 0.134(8) 0.098(7) 0.005(5) -0.008(6) 0.009(7) C7 0.063(7) 0.096(6) 0.078(6) 0.008(4) -0.003(5) -0.012(5) C8 0.066(6) 0.094(5) 0.085(5) 0.000(4) -0.009(4) -0.008(5) C9 0.094(7) 0.099(5) 0.094(5) 0.008(4) -0.015(5) 0.002(5) C10 0.096(7) 0.097(5) 0.097(6) 0.011(5) -0.016(5) 0.010(5) O2 0.100(8) 0.068(5) 0.077(6) -0.013(4) 0.021(6) -0.025(5) C11 0.054(6) 0.090(5) 0.073(6) 0.008(4) -0.013(5) -0.018(5) C12 0.092(6) 0.108(5) 0.097(5) 0.004(4) -0.006(4) -0.003(4) C13 0.080(6) 0.080(5) 0.093(5) 0.008(4) -0.001(5) 0.018(4) C14 0.095(7) 0.069(5) 0.088(6) 0.009(4) -0.007(5) 0.015(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 N1 2.2627(17) 2_656 ? Y1 N1 2.2627(17) . ? Y1 C21 2.729(2) . ? Y1 C21 2.729(2) 2_656 ? Y1 C22 2.787(2) 2_656 ? Y1 C22 2.787(2) . ? Y1 C23 2.953(2) 2_656 ? Y1 C23 2.953(2) . ? Y1 C25 2.802(2) 2_656 ? Y1 C25 2.802(2) . ? Y1 C26 2.7658(19) 2_656 ? Y1 C26 2.766(2) . ? N1 H1 0.91(3) . ? N1 C1 1.383(3) . ? C1 C2 1.417(3) . ? C1 C6 1.418(3) . ? C2 C3 1.388(3) . ? C2 C21 1.489(3) . ? C3 H3 0.9500 . ? C3 C4 1.398(3) . ? C4 H4 0.9500 . ? C4 C5 1.387(3) . ? C5 H5 0.9500 . ? C5 C6 1.397(3) . ? C6 C61 1.496(3) . ? C21 C22 1.444(3) . ? C21 C26 1.407(3) . ? C22 C23 1.409(3) . ? C22 C221 1.522(3) . ? C23 H23 0.9500 . ? C23 C24 1.392(3) . ? C24 C25 1.418(3) . ? C24 C241 1.516(3) . ? C25 H25 0.9500 . ? C25 C26 1.412(3) . ? C26 C261 1.523(3) . ? C61 C62 1.410(3) . ? C61 C66 1.408(3) . ? C62 C63 1.393(3) . ? C62 C621 1.525(3) . ? C63 H63 0.9500 . ? C63 C64 1.391(3) . ? C64 C65 1.390(3) . ? C64 C641 1.516(3) . ? C65 H65 0.9500 . ? C65 C66 1.394(3) . ? C66 C661 1.523(3) . ? C221 H221 1.0000 . ? C221 C222 1.538(3) . ? C221 C223 1.519(3) . ? C222 H222 0.9800 . ? C222 H223 0.9800 . ? C222 H224 0.9800 . ? C223 H225 0.9800 . ? C223 H226 0.9800 . ? C223 H227 0.9800 . ? C241 H241 1.0000 . ? C241 C242 1.531(3) . ? C241 C243 1.519(3) . ? C242 H242 0.9800 . ? C242 H243 0.9800 . ? C242 H244 0.9800 . ? C243 H245 0.9800 . ? C243 H246 0.9800 . ? C243 H247 0.9800 . ? C261 H261 1.0000 . ? C261 C262 1.528(3) . ? C261 C263 1.530(3) . ? C262 H262 0.9800 . ? C262 H263 0.9800 . ? C262 H264 0.9800 . ? C263 H265 0.9800 . ? C263 H266 0.9800 . ? C263 H267 0.9800 . ? C621 H621 1.0000 . ? C621 C622 1.517(3) . ? C621 C623 1.521(3) . ? C622 H622 0.9800 . ? C622 H623 0.9800 . ? C622 H624 0.9800 . ? C623 H625 0.9800 . ? C623 H626 0.9800 . ? C623 H627 0.9800 . ? C641 H641 1.0000 . ? C641 C642 1.528(3) . ? C641 C643 1.522(3) . ? C642 H642 0.9800 . ? C642 H643 0.9800 . ? C642 H644 0.9800 . ? C643 H645 0.9800 . ? C643 H646 0.9800 . ? C643 H647 0.9800 . ? C661 H661 1.0000 . ? C661 C662 1.530(3) . ? C661 C663 1.525(3) . ? C662 H662 0.9800 . ? C662 H663 0.9800 . ? C662 H664 0.9800 . ? C663 H665 0.9800 . ? C663 H666 0.9800 . ? C663 H667 0.9800 . ? O1 C7 1.4364 . ? O1 C10 1.4361 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.5315 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C9 1.5357 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.5319 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? O2 C11 1.4362 . ? O2 C14 1.4362 . ? C11 H3A 0.9900 . ? C11 H3B 0.9900 . ? C11 C12 1.5323 . ? C12 H4A 0.9900 . ? C12 H4B 0.9900 . ? C12 C13 1.5364 . ? C13 H5A 0.9900 . ? C13 H5B 0.9900 . ? C13 C14 1.5319 . ? C14 H6A 0.9900 . ? C14 H6B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Y1 N1 102.37(9) 2_656 . ? N1 Y1 C21 122.17(6) . 2_656 ? N1 Y1 C21 64.96(6) . . ? N1 Y1 C21 64.96(6) 2_656 2_656 ? N1 Y1 C21 122.17(6) 2_656 . ? N1 Y1 C22 77.36(6) . . ? N1 Y1 C22 93.25(6) . 2_656 ? N1 Y1 C22 77.36(6) 2_656 2_656 ? N1 Y1 C22 93.25(6) 2_656 . ? N1 Y1 C23 84.99(6) 2_656 . ? N1 Y1 C23 84.99(6) . 2_656 ? N1 Y1 C23 105.49(6) 2_656 2_656 ? N1 Y1 C23 105.49(6) . . ? N1 Y1 C25 113.35(6) . . ? N1 Y1 C25 126.96(6) . 2_656 ? N1 Y1 C25 113.35(6) 2_656 2_656 ? N1 Y1 C25 126.96(6) 2_656 . ? N1 Y1 C26 143.44(6) . 2_656 ? N1 Y1 C26 84.18(6) . . ? N1 Y1 C26 143.44(6) 2_656 . ? N1 Y1 C26 84.18(6) 2_656 2_656 ? C21 Y1 C21 170.00(8) 2_656 . ? C21 Y1 C22 152.34(6) . 2_656 ? C21 Y1 C22 30.33(6) 2_656 2_656 ? C21 Y1 C22 152.34(6) 2_656 . ? C21 Y1 C22 30.33(6) . . ? C21 Y1 C23 51.01(6) . . ? C21 Y1 C23 127.18(6) 2_656 . ? C21 Y1 C23 51.01(6) 2_656 2_656 ? C21 Y1 C23 127.18(6) . 2_656 ? C21 Y1 C25 52.11(6) 2_656 2_656 ? C21 Y1 C25 52.11(6) . . ? C21 Y1 C25 118.39(6) 2_656 . ? C21 Y1 C25 118.39(6) . 2_656 ? C21 Y1 C26 29.66(6) . . ? C21 Y1 C26 29.66(6) 2_656 2_656 ? C21 Y1 C26 140.48(6) 2_656 . ? C21 Y1 C26 140.48(6) . 2_656 ? C22 Y1 C22 165.13(8) . 2_656 ? C22 Y1 C23 156.65(6) 2_656 . ? C22 Y1 C23 156.66(6) . 2_656 ? C22 Y1 C23 28.23(6) 2_656 2_656 ? C22 Y1 C23 28.23(6) . . ? C22 Y1 C25 134.67(6) 2_656 . ? C22 Y1 C25 134.67(6) . 2_656 ? C22 Y1 C25 60.19(6) . . ? C22 Y1 C25 60.19(6) 2_656 2_656 ? C23 Y1 C23 163.53(8) . 2_656 ? C25 Y1 C23 115.18(6) . 2_656 ? C25 Y1 C23 115.18(6) 2_656 . ? C25 Y1 C23 49.19(6) 2_656 2_656 ? C25 Y1 C23 49.19(6) . . ? C25 Y1 C25 74.55(9) 2_656 . ? C26 Y1 C22 138.76(6) . 2_656 ? C26 Y1 C22 52.62(6) 2_656 2_656 ? C26 Y1 C22 52.62(6) . . ? C26 Y1 C22 138.76(6) 2_656 . ? C26 Y1 C23 58.82(6) . . ? C26 Y1 C23 110.93(6) . 2_656 ? C26 Y1 C23 110.94(6) 2_656 . ? C26 Y1 C23 58.82(6) 2_656 2_656 ? C26 Y1 C25 88.88(6) 2_656 . ? C26 Y1 C25 88.88(6) . 2_656 ? C26 Y1 C25 29.38(6) . . ? C26 Y1 C25 29.38(6) 2_656 2_656 ? C26 Y1 C26 111.91(8) 2_656 . ? Y1 N1 H1 121.9(15) . . ? C1 N1 Y1 130.24(13) . . ? C1 N1 H1 107.8(15) . . ? N1 C1 C2 118.04(17) . . ? N1 C1 C6 124.08(17) . . ? C6 C1 C2 117.88(18) . . ? C1 C2 C21 115.31(17) . . ? C3 C2 C1 121.17(18) . . ? C3 C2 C21 123.50(18) . . ? C2 C3 H3 119.7 . . ? C2 C3 C4 120.55(19) . . ? C4 C3 H3 119.7 . . ? C3 C4 H4 120.7 . . ? C5 C4 C3 118.69(19) . . ? C5 C4 H4 120.7 . . ? C4 C5 H5 119.0 . . ? C4 C5 C6 122.07(19) . . ? C6 C5 H5 119.0 . . ? C1 C6 C61 119.77(17) . . ? C5 C6 C1 119.48(18) . . ? C5 C6 C61 120.68(18) . . ? C2 C21 Y1 110.85(12) . . ? C22 C21 Y1 77.07(12) . . ? C22 C21 C2 117.71(17) . . ? C26 C21 Y1 76.63(12) . . ? C26 C21 C2 122.54(18) . . ? C26 C21 C22 119.39(18) . . ? C21 C22 Y1 72.60(11) . . ? C21 C22 C221 119.73(18) . . ? C23 C22 Y1 82.44(12) . . ? C23 C22 C21 118.72(18) . . ? C23 C22 C221 120.47(18) . . ? C221 C22 Y1 125.13(13) . . ? Y1 C23 H23 124.6 . . ? C22 C23 Y1 69.34(11) . . ? C22 C23 H23 118.7 . . ? C24 C23 Y1 78.93(12) . . ? C24 C23 C22 122.62(19) . . ? C24 C23 H23 118.7 . . ? C23 C24 Y1 74.11(12) . . ? C23 C24 C25 117.27(18) . . ? C23 C24 C241 123.66(19) . . ? C25 C24 Y1 67.73(11) . . ? C25 C24 C241 118.87(18) . . ? C241 C24 Y1 133.00(14) . . ? Y1 C25 H25 112.8 . . ? C24 C25 Y1 84.34(12) . . ? C24 C25 H25 119.0 . . ? C26 C25 Y1 73.90(11) . . ? C26 C25 C24 122.03(19) . . ? C26 C25 H25 119.0 . . ? C21 C26 Y1 73.70(11) . . ? C21 C26 C25 119.09(18) . . ? C21 C26 C261 125.15(18) . . ? C25 C26 Y1 76.72(12) . . ? C25 C26 C261 115.71(17) . . ? C261 C26 Y1 122.50(13) . . ? C62 C61 C6 119.46(18) . . ? C66 C61 C6 120.93(18) . . ? C66 C61 C62 119.60(18) . . ? C61 C62 C621 121.81(18) . . ? C63 C62 C61 119.11(19) . . ? C63 C62 C621 119.08(18) . . ? C62 C63 H63 119.0 . . ? C64 C63 C62 122.05(19) . . ? C64 C63 H63 119.0 . . ? C63 C64 C641 121.36(19) . . ? C65 C64 C63 118.04(19) . . ? C65 C64 C641 120.54(19) . . ? C64 C65 H65 119.0 . . ? C64 C65 C66 121.98(19) . . ? C66 C65 H65 119.0 . . ? C61 C66 C661 120.73(18) . . ? C65 C66 C61 119.21(18) . . ? C65 C66 C661 120.01(19) . . ? C22 C221 H221 107.7 . . ? C22 C221 C222 108.81(17) . . ? C222 C221 H221 107.7 . . ? C223 C221 C22 114.94(18) . . ? C223 C221 H221 107.7 . . ? C223 C221 C222 109.81(18) . . ? C221 C222 H222 109.5 . . ? C221 C222 H223 109.5 . . ? C221 C222 H224 109.5 . . ? H222 C222 H223 109.5 . . ? H222 C222 H224 109.5 . . ? H223 C222 H224 109.5 . . ? C221 C223 H225 109.5 . . ? C221 C223 H226 109.5 . . ? C221 C223 H227 109.5 . . ? H225 C223 H226 109.5 . . ? H225 C223 H227 109.5 . . ? H226 C223 H227 109.5 . . ? C24 C241 H241 107.7 . . ? C24 C241 C242 110.05(19) . . ? C24 C241 C243 114.48(19) . . ? C242 C241 H241 107.7 . . ? C243 C241 H241 107.7 . . ? C243 C241 C242 109.0(2) . . ? C241 C242 H242 109.5 . . ? C241 C242 H243 109.5 . . ? C241 C242 H244 109.5 . . ? H242 C242 H243 109.5 . . ? H242 C242 H244 109.5 . . ? H243 C242 H244 109.5 . . ? C241 C243 H245 109.5 . . ? C241 C243 H246 109.5 . . ? C241 C243 H247 109.5 . . ? H245 C243 H246 109.5 . . ? H245 C243 H247 109.5 . . ? H246 C243 H247 109.5 . . ? C26 C261 H261 106.2 . . ? C26 C261 C262 108.63(17) . . ? C26 C261 C263 117.90(17) . . ? C262 C261 H261 106.2 . . ? C262 C261 C263 111.08(18) . . ? C263 C261 H261 106.2 . . ? C261 C262 H262 109.5 . . ? C261 C262 H263 109.5 . . ? C261 C262 H264 109.5 . . ? H262 C262 H263 109.5 . . ? H262 C262 H264 109.5 . . ? H263 C262 H264 109.5 . . ? C261 C263 H265 109.5 . . ? C261 C263 H266 109.5 . . ? C261 C263 H267 109.5 . . ? H265 C263 H266 109.5 . . ? H265 C263 H267 109.5 . . ? H266 C263 H267 109.5 . . ? C62 C621 H621 107.4 . . ? C622 C621 C62 110.50(18) . . ? C622 C621 H621 107.4 . . ? C622 C621 C623 111.6(2) . . ? C623 C621 C62 112.26(18) . . ? C623 C621 H621 107.4 . . ? C621 C622 H622 109.5 . . ? C621 C622 H623 109.5 . . ? C621 C622 H624 109.5 . . ? H622 C622 H623 109.5 . . ? H622 C622 H624 109.5 . . ? H623 C622 H624 109.5 . . ? C621 C623 H625 109.5 . . ? C621 C623 H626 109.5 . . ? C621 C623 H627 109.5 . . ? H625 C623 H626 109.5 . . ? H625 C623 H627 109.5 . . ? H626 C623 H627 109.5 . . ? C64 C641 H641 107.5 . . ? C64 C641 C642 110.15(17) . . ? C64 C641 C643 113.22(18) . . ? C642 C641 H641 107.5 . . ? C643 C641 H641 107.5 . . ? C643 C641 C642 110.73(19) . . ? C641 C642 H642 109.5 . . ? C641 C642 H643 109.5 . . ? C641 C642 H644 109.5 . . ? H642 C642 H643 109.5 . . ? H642 C642 H644 109.5 . . ? H643 C642 H644 109.5 . . ? C641 C643 H645 109.5 . . ? C641 C643 H646 109.5 . . ? C641 C643 H647 109.5 . . ? H645 C643 H646 109.5 . . ? H645 C643 H647 109.5 . . ? H646 C643 H647 109.5 . . ? C66 C661 H661 107.8 . . ? C66 C661 C662 113.16(19) . . ? C66 C661 C663 110.00(19) . . ? C662 C661 H661 107.8 . . ? C663 C661 H661 107.8 . . ? C663 C661 C662 110.0(2) . . ? C661 C662 H662 109.5 . . ? C661 C662 H663 109.5 . . ? C661 C662 H664 109.5 . . ? H662 C662 H663 109.5 . . ? H662 C662 H664 109.5 . . ? H663 C662 H664 109.5 . . ? C661 C663 H665 109.5 . . ? C661 C663 H666 109.5 . . ? C661 C663 H667 109.5 . . ? H665 C663 H666 109.5 . . ? H665 C663 H667 109.5 . . ? H666 C663 H667 109.5 . . ? C10 O1 C7 110.1 . . ? O1 C7 H7A 110.5 . . ? O1 C7 H7B 110.5 . . ? O1 C7 C8 106.2 . . ? H7A C7 H7B 108.7 . . ? C8 C7 H7A 110.5 . . ? C8 C7 H7B 110.5 . . ? C7 C8 H8A 111.4 . . ? C7 C8 H8B 111.4 . . ? C7 C8 C9 101.8 . . ? H8A C8 H8B 109.3 . . ? C9 C8 H8A 111.4 . . ? C9 C8 H8B 111.4 . . ? C8 C9 H9A 111.4 . . ? C8 C9 H9B 111.4 . . ? H9A C9 H9B 109.3 . . ? C10 C9 C8 101.7 . . ? C10 C9 H9A 111.4 . . ? C10 C9 H9B 111.4 . . ? O1 C10 C9 106.3 . . ? O1 C10 H10A 110.5 . . ? O1 C10 H10B 110.5 . . ? C9 C10 H10A 110.5 . . ? C9 C10 H10B 110.5 . . ? H10A C10 H10B 108.7 . . ? C14 O2 C11 110.1 . . ? O2 C11 H3A 110.5 . . ? O2 C11 H3B 110.5 . . ? O2 C11 C12 106.3 . . ? H3A C11 H3B 108.7 . . ? C12 C11 H3A 110.5 . . ? C12 C11 H3B 110.5 . . ? C11 C12 H4A 111.4 . . ? C11 C12 H4B 111.4 . . ? C11 C12 C13 101.7 . . ? H4A C12 H4B 109.3 . . ? C13 C12 H4A 111.4 . . ? C13 C12 H4B 111.4 . . ? C12 C13 H5A 111.4 . . ? C12 C13 H5B 111.4 . . ? H5A C13 H5B 109.3 . . ? C14 C13 C12 101.8 . . ? C14 C13 H5A 111.4 . . ? C14 C13 H5B 111.4 . . ? O2 C14 C13 106.3 . . ? O2 C14 H6A 110.5 . . ? O2 C14 H6B 110.5 . . ? C13 C14 H6A 110.5 . . ? C13 C14 H6B 110.5 . . ? H6A C14 H6B 108.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Y1 N1 C1 C2 2.3(3) . . . . ? Y1 N1 C1 C6 -177.43(14) . . . . ? Y1 C21 C22 C23 -70.79(17) . . . . ? Y1 C21 C22 C221 121.03(17) . . . . ? Y1 C21 C26 C25 64.12(17) . . . . ? Y1 C21 C26 C261 -118.60(19) . . . . ? Y1 C22 C23 C24 -61.0(2) . . . . ? Y1 C22 C221 C222 171.11(15) . . . . ? Y1 C22 C221 C223 -65.3(2) . . . . ? Y1 C23 C24 C25 -53.84(17) . . . . ? Y1 C23 C24 C241 131.5(2) . . . . ? Y1 C24 C25 C26 -67.00(18) . . . . ? Y1 C24 C241 C242 -150.51(18) . . . . ? Y1 C24 C241 C243 86.3(2) . . . . ? Y1 C25 C26 C21 -62.54(16) . . . . ? Y1 C25 C26 C261 119.94(16) . . . . ? Y1 C26 C261 C262 179.94(14) . . . . ? Y1 C26 C261 C263 -52.6(2) . . . . ? N1 C1 C2 C3 -176.69(18) . . . . ? N1 C1 C2 C21 4.9(3) . . . . ? N1 C1 C6 C5 175.59(19) . . . . ? N1 C1 C6 C61 -7.6(3) . . . . ? C1 C2 C3 C4 0.5(3) . . . . ? C1 C2 C21 Y1 -7.9(2) . . . . ? C1 C2 C21 C22 78.0(2) . . . . ? C1 C2 C21 C26 -95.1(2) . . . . ? C1 C6 C61 C62 -91.1(2) . . . . ? C1 C6 C61 C66 87.7(2) . . . . ? C2 C1 C6 C5 -4.1(3) . . . . ? C2 C1 C6 C61 172.69(17) . . . . ? C2 C3 C4 C5 -3.0(3) . . . . ? C2 C21 C22 Y1 -106.97(16) . . . . ? C2 C21 C22 C23 -177.76(18) . . . . ? C2 C21 C22 C221 14.1(3) . . . . ? C2 C21 C26 Y1 106.40(18) . . . . ? C2 C21 C26 C25 170.52(18) . . . . ? C2 C21 C26 C261 -12.2(3) . . . . ? C3 C2 C21 Y1 173.68(15) . . . . ? C3 C2 C21 C22 -100.4(2) . . . . ? C3 C2 C21 C26 86.6(3) . . . . ? C3 C4 C5 C6 1.8(3) . . . . ? C4 C5 C6 C1 1.8(3) . . . . ? C4 C5 C6 C61 -175.0(2) . . . . ? C5 C6 C61 C62 85.7(2) . . . . ? C5 C6 C61 C66 -95.5(2) . . . . ? C6 C1 C2 C3 3.1(3) . . . . ? C6 C1 C2 C21 -175.36(17) . . . . ? C6 C61 C62 C63 178.18(18) . . . . ? C6 C61 C62 C621 -1.0(3) . . . . ? C6 C61 C66 C65 -179.17(19) . . . . ? C6 C61 C66 C661 3.5(3) . . . . ? C21 C2 C3 C4 178.79(19) . . . . ? C21 C22 C23 Y1 65.37(16) . . . . ? C21 C22 C23 C24 4.4(3) . . . . ? C21 C22 C221 C222 82.2(2) . . . . ? C21 C22 C221 C223 -154.2(2) . . . . ? C21 C26 C261 C262 -87.7(2) . . . . ? C21 C26 C261 C263 39.8(3) . . . . ? C22 C21 C26 Y1 -66.56(17) . . . . ? C22 C21 C26 C25 -2.4(3) . . . . ? C22 C21 C26 C261 174.83(18) . . . . ? C22 C23 C24 Y1 56.49(19) . . . . ? C22 C23 C24 C25 2.6(3) . . . . ? C22 C23 C24 C241 -172.0(2) . . . . ? C23 C22 C221 C222 -85.8(2) . . . . ? C23 C22 C221 C223 37.8(3) . . . . ? C23 C24 C25 Y1 57.05(18) . . . . ? C23 C24 C25 C26 -10.0(3) . . . . ? C23 C24 C241 C242 109.6(3) . . . . ? C23 C24 C241 C243 -13.6(3) . . . . ? C24 C25 C26 Y1 72.45(19) . . . . ? C24 C25 C26 C21 9.9(3) . . . . ? C24 C25 C26 C261 -167.62(18) . . . . ? C25 C24 C241 C242 -65.0(3) . . . . ? C25 C24 C241 C243 171.8(2) . . . . ? C25 C26 C261 C262 89.7(2) . . . . ? C25 C26 C261 C263 -142.9(2) . . . . ? C26 C21 C22 Y1 66.33(16) . . . . ? C26 C21 C22 C23 -4.5(3) . . . . ? C26 C21 C22 C221 -172.64(18) . . . . ? C61 C62 C63 C64 0.9(3) . . . . ? C61 C62 C621 C622 104.5(2) . . . . ? C61 C62 C621 C623 -130.3(2) . . . . ? C61 C66 C661 C662 -145.0(2) . . . . ? C61 C66 C661 C663 91.5(2) . . . . ? C62 C61 C66 C65 -0.4(3) . . . . ? C62 C61 C66 C661 -177.72(19) . . . . ? C62 C63 C64 C65 -0.1(3) . . . . ? C62 C63 C64 C641 -177.23(19) . . . . ? C63 C62 C621 C622 -74.7(3) . . . . ? C63 C62 C621 C623 50.6(3) . . . . ? C63 C64 C65 C66 -0.9(3) . . . . ? C63 C64 C641 C642 76.0(3) . . . . ? C63 C64 C641 C643 -48.6(3) . . . . ? C64 C65 C66 C61 1.2(3) . . . . ? C64 C65 C66 C661 178.5(2) . . . . ? C65 C64 C641 C642 -101.1(2) . . . . ? C65 C64 C641 C643 134.3(2) . . . . ? C65 C66 C661 C662 37.7(3) . . . . ? C65 C66 C661 C663 -85.8(3) . . . . ? C66 C61 C62 C63 -0.6(3) . . . . ? C66 C61 C62 C621 -179.75(19) . . . . ? C221 C22 C23 Y1 -126.54(19) . . . . ? C221 C22 C23 C24 172.47(19) . . . . ? C241 C24 C25 Y1 -128.01(18) . . . . ? C241 C24 C25 C26 164.99(19) . . . . ? C621 C62 C63 C64 -179.96(19) . . . . ? C641 C64 C65 C66 176.19(19) . . . . ? O1 C7 C8 C9 30.6 . . . . ? C7 O1 C10 C9 -12.0 . . . . ? C7 C8 C9 C10 -36.4 . . . . ? C8 C9 C10 O1 30.6 . . . . ? C10 O1 C7 C8 -12.0 . . . . ? O2 C11 C12 C13 30.6 . . . . ? C11 O2 C14 C13 -11.9 . . . . ? C11 C12 C13 C14 -36.3 . . . . ? C12 C13 C14 O2 30.5 . . . . ? C14 O2 C11 C12 -12.0 . . . . ? _shelx_res_file ; TITL rjii-95_a.res in C2/c REM Old TITL RJII-95 in C2/c #15 REM SHELXT solution in C2/c REM R1 0.136, Rweak 0.010, Alpha 0.023, Orientation as input REM Formula found by SHELXT: C72 N2 Y CELL 1.54184 18.0163 17.0386 22.7773 90 106.062 90 ZERR 4 0.0003 0.0003 0.0004 0 0.002 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H N O Y UNIT 304 432 8 4 4 SADI C11 C12 C12 C13 C13 C14 SIMU O2 > C14 SADI 0.04 O1 C8 O1 C9 SADI O2 C11 O2 C14 RIGU O2 > C14 SADI 0.04 O2 C12 O2 C13 SADI 0.04 C8 C10 C7 C9 SADI 0.04 C12 C14 C11 C13 SIMU O1 > C10 SADI C7 C8 C8 C9 C9 C10 RIGU O1 > C10 SADI O1 C7 O1 C10 SIMU 0.01 0.02 2 C7 > C10 C11 > C14 L.S. 31 0 0 PLAN 11 SIZE 0.024 0.059 0.076 TEMP -173.15(10) CONF BOND $H MORE -1 fmap 2 53 acta REM REM REM WGHT 0.065100 10.282595 FVAR 0.17350 Y1 5 0.500000 0.395933 0.750000 10.50000 0.04199 0.01772 = 0.02493 0.00000 0.01201 0.00000 N1 3 0.527902 0.312697 0.681661 11.00000 0.03015 0.02281 = 0.02732 -0.00346 0.00700 -0.00318 H1 2 0.495177 0.273276 0.663856 11.00000 0.03017 C1 1 0.593000 0.307451 0.660955 11.00000 0.03064 0.01849 = 0.02430 0.00156 0.00531 -0.00107 C2 1 0.655168 0.359254 0.686303 11.00000 0.03251 0.01921 = 0.02461 0.00068 0.00560 -0.00096 C3 1 0.720679 0.360026 0.665503 11.00000 0.03207 0.02148 = 0.03162 -0.00081 0.00673 -0.00351 AFIX 43 H3 2 0.761824 0.394954 0.683386 11.00000 -1.20000 AFIX 0 C4 1 0.726605 0.309847 0.618472 11.00000 0.03518 0.02773 = 0.03672 -0.00270 0.01395 -0.00205 AFIX 43 H4 2 0.770320 0.312009 0.602882 11.00000 -1.20000 AFIX 0 C5 1 0.667419 0.256840 0.595013 11.00000 0.04010 0.02333 = 0.03049 -0.00480 0.01254 -0.00041 AFIX 43 H5 2 0.671917 0.221579 0.563870 11.00000 -1.20000 AFIX 0 C6 1 0.601370 0.253659 0.615739 11.00000 0.03439 0.01903 = 0.02627 -0.00133 0.00727 -0.00203 C21 1 0.645480 0.409890 0.736958 11.00000 0.03165 0.01806 = 0.02538 -0.00149 0.00501 -0.00342 C22 1 0.658849 0.374775 0.796671 11.00000 0.03445 0.02042 = 0.02642 0.00054 0.00500 -0.00034 C23 1 0.647355 0.420761 0.844811 11.00000 0.03692 0.02548 = 0.02232 0.00035 0.00333 -0.00179 AFIX 43 H23 2 0.659639 0.398837 0.884694 11.00000 -1.20000 AFIX 0 C24 1 0.618724 0.497019 0.836274 11.00000 0.03473 0.02388 = 0.02651 -0.00362 0.00560 -0.00265 C25 1 0.597838 0.526784 0.775774 11.00000 0.03986 0.01977 = 0.02981 -0.00179 0.00883 0.00042 AFIX 43 H25 2 0.570618 0.575103 0.767581 11.00000 -1.20000 AFIX 0 C26 1 0.616254 0.486809 0.727325 11.00000 0.03182 0.01822 = 0.02550 -0.00010 0.00453 -0.00262 C61 1 0.541594 0.191575 0.593103 11.00000 0.03574 0.01961 = 0.02551 -0.00503 0.01042 -0.00183 C62 1 0.550572 0.117673 0.622070 11.00000 0.03256 0.02190 = 0.02844 -0.00280 0.00863 -0.00014 C63 1 0.493546 0.060920 0.601837 11.00000 0.03603 0.01994 = 0.03231 -0.00062 0.00873 -0.00137 AFIX 43 H63 2 0.499353 0.011422 0.621792 11.00000 -1.20000 AFIX 0 C64 1 0.428359 0.074471 0.553319 11.00000 0.03566 0.02371 = 0.02591 -0.00533 0.00919 -0.00363 C65 1 0.420935 0.147344 0.524835 11.00000 0.03744 0.02620 = 0.02443 -0.00214 0.00394 -0.00216 AFIX 43 H65 2 0.377126 0.157195 0.491239 11.00000 -1.20000 AFIX 0 C66 1 0.475855 0.206415 0.544093 11.00000 0.03997 0.02125 = 0.02591 -0.00231 0.00907 -0.00141 C221 1 0.699390 0.295673 0.809659 11.00000 0.03461 0.02034 = 0.02860 0.00208 0.00430 0.00183 AFIX 13 H221 2 0.683697 0.263989 0.771247 11.00000 -1.20000 AFIX 0 C222 1 0.787127 0.308885 0.825151 11.00000 0.04030 0.03187 = 0.04996 0.00612 0.00510 0.00215 AFIX 137 H222 2 0.799394 0.337660 0.791768 11.00000 -1.50000 H223 2 0.813616 0.258057 0.830570 11.00000 -1.50000 H224 2 0.804280 0.339356 0.862987 11.00000 -1.50000 AFIX 0 C223 1 0.680198 0.248103 0.859966 11.00000 0.05082 0.03191 = 0.04400 0.01106 0.01692 0.01005 AFIX 137 H225 2 0.704800 0.196428 0.862670 11.00000 -1.50000 H226 2 0.624092 0.241589 0.850644 11.00000 -1.50000 H227 2 0.699322 0.275612 0.899028 11.00000 -1.50000 AFIX 0 C241 1 0.615212 0.551259 0.888173 11.00000 0.04132 0.02991 = 0.03025 -0.00603 0.00837 -0.00036 AFIX 13 H241 2 0.562699 0.575681 0.877431 11.00000 -1.20000 AFIX 0 C242 1 0.674397 0.617426 0.894397 11.00000 0.06373 0.04208 = 0.05480 -0.02247 0.02091 -0.01680 AFIX 137 H242 2 0.665298 0.645132 0.855342 11.00000 -1.50000 H243 2 0.726617 0.595231 0.905783 11.00000 -1.50000 H244 2 0.669156 0.654265 0.926051 11.00000 -1.50000 AFIX 0 C243 1 0.627773 0.510855 0.949599 11.00000 0.04767 0.05070 = 0.02590 -0.00536 0.00416 0.00828 AFIX 137 H245 2 0.680506 0.490082 0.962914 11.00000 -1.50000 H246 2 0.590798 0.467675 0.945743 11.00000 -1.50000 H247 2 0.620120 0.548741 0.979770 11.00000 -1.50000 AFIX 0 C261 1 0.605406 0.533565 0.668542 11.00000 0.03622 0.02095 = 0.02683 0.00222 0.00618 -0.00033 AFIX 13 H261 2 0.566365 0.575072 0.669100 11.00000 -1.20000 AFIX 0 C262 1 0.680638 0.576720 0.671249 11.00000 0.04320 0.03226 = 0.03391 0.00586 0.00830 -0.00810 AFIX 137 H262 2 0.672304 0.612832 0.636542 11.00000 -1.50000 H263 2 0.720643 0.538550 0.669455 11.00000 -1.50000 H264 2 0.697212 0.606451 0.709485 11.00000 -1.50000 AFIX 0 C263 1 0.575176 0.490065 0.607852 11.00000 0.04197 0.02487 = 0.02883 0.00244 0.00268 0.00120 AFIX 137 H265 2 0.553851 0.527987 0.575189 11.00000 -1.50000 H266 2 0.534681 0.453151 0.610872 11.00000 -1.50000 H267 2 0.617632 0.461193 0.598614 11.00000 -1.50000 AFIX 0 C621 1 0.620462 0.098523 0.675532 11.00000 0.03249 0.02395 = 0.03462 -0.00074 0.00526 -0.00141 AFIX 13 H621 2 0.659478 0.140972 0.677767 11.00000 -1.20000 AFIX 0 C622 1 0.598500 0.099632 0.735175 11.00000 0.04241 0.06442 = 0.03315 -0.00086 0.00368 0.00597 AFIX 137 H622 2 0.645041 0.093384 0.769399 11.00000 -1.50000 H623 2 0.562637 0.056494 0.735497 11.00000 -1.50000 H624 2 0.573630 0.149736 0.739169 11.00000 -1.50000 AFIX 0 C623 1 0.658164 0.021236 0.666585 11.00000 0.04473 0.03735 = 0.04824 -0.00317 0.00437 0.01156 AFIX 137 H625 2 0.705719 0.014015 0.699695 11.00000 -1.50000 H626 2 0.670512 0.022006 0.627302 11.00000 -1.50000 H627 2 0.622553 -0.022106 0.666993 11.00000 -1.50000 AFIX 0 C641 1 0.365122 0.013380 0.533709 11.00000 0.03794 0.02670 = 0.02826 -0.00393 0.00638 -0.00666 AFIX 13 H641 2 0.330889 0.029853 0.493072 11.00000 -1.20000 AFIX 0 C642 1 0.315832 0.011650 0.578577 11.00000 0.04220 0.04106 = 0.04128 -0.01082 0.01501 -0.01252 AFIX 137 H642 2 0.274724 -0.027445 0.565158 11.00000 -1.50000 H643 2 0.292852 0.063504 0.579983 11.00000 -1.50000 H644 2 0.348318 -0.002219 0.619359 11.00000 -1.50000 AFIX 0 C643 1 0.395692 -0.068189 0.526093 11.00000 0.04919 0.02994 = 0.04729 -0.01462 0.01379 -0.00918 AFIX 137 H645 2 0.427531 -0.087101 0.565701 11.00000 -1.50000 H646 2 0.427010 -0.065853 0.497150 11.00000 -1.50000 H647 2 0.352214 -0.104119 0.510527 11.00000 -1.50000 AFIX 0 C661 1 0.466091 0.284635 0.510426 11.00000 0.04902 0.02368 = 0.03022 0.00148 0.00385 -0.00437 AFIX 13 H661 2 0.496095 0.325042 0.539213 11.00000 -1.20000 AFIX 0 C662 1 0.382021 0.312056 0.489081 11.00000 0.05643 0.03081 = 0.03538 0.00666 0.01004 0.00665 AFIX 137 H662 2 0.379973 0.365227 0.472301 11.00000 -1.50000 H663 2 0.359817 0.312159 0.523799 11.00000 -1.50000 H664 2 0.352428 0.276345 0.457473 11.00000 -1.50000 AFIX 0 C663 1 0.499918 0.279546 0.456129 11.00000 0.06040 0.04392 = 0.05325 0.02097 0.02459 0.00407 AFIX 137 H665 2 0.471570 0.240102 0.427204 11.00000 -1.50000 H666 2 0.554471 0.264542 0.470478 11.00000 -1.50000 H667 2 0.495452 0.330724 0.435813 11.00000 -1.50000 AFIX 6 PART -2 O1 4 1.063110 0.318258 0.813185 10.25000 0.10076 0.13395 = 0.09771 0.00492 -0.00779 0.00869 C7 1 1.027878 0.380118 0.772036 10.25000 0.06315 0.09603 = 0.07812 0.00794 -0.00333 -0.01151 AFIX 23 H7A 2 1.061291 0.427269 0.779137 10.25000 -1.20000 H7B 2 0.977175 0.394437 0.777945 10.25000 -1.20000 AFIX 5 C8 1 1.017840 0.348201 0.707446 10.25000 0.06623 0.09431 = 0.08501 0.00001 -0.00918 -0.00790 AFIX 23 H8A 2 1.064303 0.358056 0.693375 10.25000 -1.20000 H8B 2 0.972195 0.371509 0.677927 10.25000 -1.20000 AFIX 5 C9 1 1.006394 0.260140 0.716364 10.25000 0.09402 0.09885 = 0.09431 0.00779 -0.01550 0.00187 AFIX 23 H9A 2 0.952201 0.248144 0.715082 10.25000 -1.20000 H9B 2 1.021442 0.228389 0.685100 10.25000 -1.20000 AFIX 5 C10 1 1.061023 0.246109 0.780174 10.25000 0.09598 0.09695 = 0.09683 0.01056 -0.01617 0.01044 AFIX 23 H10A 2 1.041643 0.202812 0.800895 10.25000 -1.20000 H10B 2 1.113317 0.232256 0.777413 10.25000 -1.20000 AFIX 6 PART -1 O2 4 1.017859 0.317850 0.816423 10.25000 0.10024 0.06805 = 0.07744 -0.01337 0.02143 -0.02470 C11 1 1.056444 0.366994 0.782862 10.25000 0.05408 0.09016 = 0.07263 0.00786 -0.01288 -0.01786 AFIX 23 H3A 2 1.098837 0.396553 0.811163 10.25000 -1.20000 H3B 2 1.019731 0.404919 0.757346 10.25000 -1.20000 AFIX 5 C12 1 1.088565 0.311958 0.742619 10.25000 0.09215 0.10779 = 0.09747 0.00427 -0.00618 -0.00335 AFIX 23 H4A 2 1.140838 0.292895 0.764409 10.25000 -1.20000 H4B 2 1.090423 0.338002 0.704198 10.25000 -1.20000 AFIX 5 C13 1 1.029179 0.244964 0.730410 10.25000 0.07994 0.07951 = 0.09290 0.00832 -0.00076 0.01825 AFIX 23 H5A 2 0.983137 0.258045 0.696487 10.25000 -1.20000 H5B 2 1.051922 0.195289 0.720915 10.25000 -1.20000 AFIX 5 C14 1 1.009262 0.239890 0.791472 10.25000 0.09460 0.06894 = 0.08803 0.00950 -0.00680 0.01526 AFIX 23 H6A 2 0.955589 0.221183 0.785103 10.25000 -1.20000 H6B 2 1.044663 0.203170 0.819482 10.25000 -1.20000 AFIX 0 HKLF 4 REM rjii-95_a.res in C2/c REM R1 = 0.0417 for 6185 Fo > 4sig(Fo) and 0.0446 for all 6674 data REM 427 parameters refined using 198 restraints END WGHT 0.0646 10.3563 REM Highest difference peak 0.594, deepest hole -0.697, 1-sigma level 0.059 Q1 1 1.0393 0.3947 0.7817 11.00000 0.05 0.59 Q2 1 1.0201 0.3234 0.7163 11.00000 0.05 0.56 Q3 1 1.0780 0.2607 0.7638 11.00000 0.05 0.54 Q4 1 0.5579 0.1957 0.8133 11.00000 0.05 0.47 Q5 1 1.0178 0.2368 0.7177 11.00000 0.05 0.41 Q6 1 0.6024 0.0411 0.7342 11.00000 0.05 0.40 Q7 1 1.0381 0.3330 0.8173 11.00000 0.05 0.40 Q8 1 0.9548 0.2689 0.6808 11.00000 0.05 0.40 Q9 1 1.0776 0.3033 0.8594 11.00000 0.05 0.39 Q10 1 0.5000 0.1835 0.7500 10.50000 0.05 0.37 Q11 1 1.0604 0.3611 0.7987 11.00000 0.05 0.37 ; _shelx_res_checksum 47464 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.603 _oxdiff_exptl_absorpt_empirical_full_min 0.605 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_rj4_74_fast _database_code_depnum_ccdc_archive 'CCDC 2207618' loop_ _audit_author_name _audit_author_address 'Richard Staples' ;Michigan State University United States of America ; _audit_update_record ; 2022-09-15 deposited with the CCDC. 2023-03-21 downloaded from the CCDC. ; _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73 H100 N3 Y' _chemical_formula_weight 1108.46 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' Y Y -0.2670 2.0244 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.82162(15) _cell_length_b 28.6809(3) _cell_length_c 17.1150(2) _cell_angle_alpha 90 _cell_angle_beta 106.3655(13) _cell_angle_gamma 90 _cell_volume 6509.79(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.131 _exptl_crystal_F_000 2392 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_absorpt_coefficient_mu 1.564 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_source ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 50292 _diffrn_reflns_av_unetI/netI 0.0388 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.101 _diffrn_reflns_theta_max 77.267 _diffrn_reflns_theta_full 67.684 _diffrn_measured_fraction_theta_max 0.935 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.935 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.935 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 12920 _reflns_number_gt 11192 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+5.9830P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 12920 _refine_ls_number_parameters 726 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0951 _refine_ls_wR_factor_gt 0.0910 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Y001 Y 0.78320(2) 0.40208(2) 0.85684(2) 0.01843(6) Uani 1 1 d . . . . . N26 N 0.83691(12) 0.47954(6) 0.88457(9) 0.0138(3) Uani 1 1 d . . . . . N003 N 0.83171(13) 0.37950(6) 0.74963(11) 0.0203(4) Uani 1 1 d . . . . . N004 N 0.63372(13) 0.37318(7) 0.85557(11) 0.0200(4) Uani 1 1 d . . . . . C005 C 0.86050(15) 0.31342(8) 0.91469(12) 0.0208(4) Uani 1 1 d . . . . . C006 C 0.63971(17) 0.49191(8) 0.68698(13) 0.0261(5) Uani 1 1 d . . . . . H006 H 0.6623 0.4875 0.6400 0.031 Uiso 1 1 calc R U . . . C007 C 0.83929(16) 0.33274(8) 0.98332(12) 0.0231(4) Uani 1 1 d . . . . . H007 H 0.7884 0.3186 1.0028 0.028 Uiso 1 1 calc R U . . . C008 C 0.95629(15) 0.32147(7) 0.80793(12) 0.0198(4) Uani 1 1 d . . . . . C009 C 0.43886(17) 0.27570(9) 0.72983(13) 0.0285(5) Uani 1 1 d . . . . . H009 H 0.4275 0.3101 0.7234 0.034 Uiso 1 1 calc R U . . . C00A C 0.93604(15) 0.33480(7) 0.88602(12) 0.0199(4) Uani 1 1 d . . . . . C00B C 0.54665(19) 0.41514(8) 0.65375(14) 0.0293(5) Uani 1 1 d . . . . . H00B H 0.5559 0.3862 0.6875 0.035 Uiso 1 1 calc R U . . . C00C C 0.58539(16) 0.45614(8) 0.71059(13) 0.0224(4) Uani 1 1 d . . . . . C00D C 0.72911(18) 0.45149(9) 0.37902(13) 0.0285(5) Uani 1 1 d . . . . . H00D H 0.7443 0.4851 0.3929 0.034 Uiso 1 1 calc R U . . . C00E C 0.92773(15) 0.34105(7) 0.66546(12) 0.0194(4) Uani 1 1 d . . . . . C00F C 0.49221(15) 0.42611(7) 0.80782(12) 0.0187(4) Uani 1 1 d . . . . . C00G C 0.76057(16) 0.37526(8) 0.45668(13) 0.0239(4) Uani 1 1 d . . . . . H00G H 0.7137 0.3611 0.4114 0.029 Uiso 1 1 calc R U . . . C00H C 0.46282(15) 0.34869(8) 0.85352(12) 0.0207(4) Uani 1 1 d . . . . . C00I C 0.54418(16) 0.32586(8) 1.02712(13) 0.0227(4) Uani 1 1 d . . . . . H00I H 0.5502 0.3573 1.0039 0.027 Uiso 1 1 calc R U . . . C00J C 0.96469(16) 0.39219(8) 0.99534(12) 0.0220(4) Uani 1 1 d . . . . . H00J H 0.9989 0.4190 1.0219 0.026 Uiso 1 1 calc R U . . . C00K C 0.49360(16) 0.26615(8) 0.81914(13) 0.0226(4) Uani 1 1 d . . . . . C00L C 0.38935(16) 0.43557(8) 0.79447(13) 0.0233(4) Uani 1 1 d . . . . . H00L H 0.3641 0.4653 0.7743 0.028 Uiso 1 1 calc R U . . . C00M C 0.63001(18) 0.32067(9) 1.10494(13) 0.0287(5) Uani 1 1 d . . . . . H00A H 0.6319 0.3480 1.1396 0.043 Uiso 1 1 calc R U . . . H00C H 0.6941 0.3181 1.0913 0.043 Uiso 1 1 calc R U . . . H00E H 0.6194 0.2926 1.1340 0.043 Uiso 1 1 calc R U . . . C00N C 0.86335(17) 0.39073(9) 1.09856(13) 0.0281(5) Uani 1 1 d . . . . . H00N H 0.8235 0.3663 1.1175 0.034 Uiso 1 1 calc R U . . . C00O C 0.90286(15) 0.34779(7) 0.73956(12) 0.0192(4) Uani 1 1 d . . . . . C00P C 0.60012(19) 0.40805(11) 0.58776(15) 0.0380(6) Uani 1 1 d . . . . . H00F H 0.5840 0.4340 0.5491 0.057 Uiso 1 1 calc R U . . . H00H H 0.5775 0.3787 0.5590 0.057 Uiso 1 1 calc R U . . . H00K H 0.6732 0.4068 0.6129 0.057 Uiso 1 1 calc R U . . . C00Q C 0.53127(15) 0.38253(7) 0.83964(12) 0.0183(4) Uani 1 1 d . . . . . C00R C 0.44384(18) 0.32423(9) 1.04861(15) 0.0312(5) Uani 1 1 d . . . . . H00M H 0.4343 0.2931 1.0689 0.047 Uiso 1 1 calc R U . . . H00O H 0.3884 0.3311 0.9999 0.047 Uiso 1 1 calc R U . . . H00P H 0.4446 0.3474 1.0908 0.047 Uiso 1 1 calc R U . . . C00S C 0.66216(16) 0.53389(8) 0.72941(14) 0.0257(5) Uani 1 1 d . . . . . C00T C 0.55722(15) 0.46201(7) 0.78387(12) 0.0197(4) Uani 1 1 d . . . . . C00U C 0.36098(15) 0.35921(8) 0.83861(13) 0.0235(4) Uani 1 1 d . . . . . H00U H 0.3162 0.3362 0.8482 0.028 Uiso 1 1 calc R U . . . C00V C 0.4351(2) 0.42046(14) 0.61121(18) 0.0581(10) Uani 1 1 d . . . . . H00Q H 0.3979 0.4234 0.6520 0.087 Uiso 1 1 calc R U . . . H00R H 0.4110 0.3930 0.5773 0.087 Uiso 1 1 calc R U . . . H00S H 0.4242 0.4484 0.5769 0.087 Uiso 1 1 calc R U . . . C00W C 0.97607(17) 0.44109(8) 0.65808(13) 0.0256(5) Uani 1 1 d . . . . . H00W H 0.9898 0.4203 0.7069 0.031 Uiso 1 1 calc R U . . . C00X C 0.58161(15) 0.50353(7) 0.82828(12) 0.0205(4) Uani 1 1 d . . . . . C00Y C 0.80804(16) 0.34773(8) 0.52385(12) 0.0221(4) Uani 1 1 d . . . . . C00Z C 0.50037(15) 0.30047(7) 0.87916(12) 0.0203(4) Uani 1 1 d . . . . . C010 C 0.58377(16) 0.24518(8) 0.98244(13) 0.0222(4) Uani 1 1 d . . . . . H010 H 0.6144 0.2380 1.0381 0.027 Uiso 1 1 calc R U . . . C011 C 0.77959(17) 0.42273(8) 0.45390(13) 0.0248(5) Uani 1 1 d . . . . . C012 C 0.62035(17) 0.16169(8) 0.94379(14) 0.0280(5) Uani 1 1 d . . . . . H012 H 0.6557 0.1533 0.9022 0.034 Uiso 1 1 calc R U . . . C013 C 0.32369(16) 0.40293(8) 0.80980(13) 0.0260(5) Uani 1 1 d . . . . . H013 H 0.2543 0.4102 0.8009 0.031 Uiso 1 1 calc R U . . . C014 C 1.03040(16) 0.28977(8) 0.80370(13) 0.0236(4) Uani 1 1 d . . . . . H014 H 1.0653 0.2726 0.8507 0.028 Uiso 1 1 calc R U . . . C015 C 1.00242(16) 0.30886(8) 0.66305(13) 0.0239(4) Uani 1 1 d . . . . . H015 H 1.0189 0.3044 0.6133 0.029 Uiso 1 1 calc R U . . . C016 C 0.88935(16) 0.37157(8) 1.02412(12) 0.0227(4) Uani 1 1 d . . . . . C017 C 0.87645(15) 0.36902(7) 0.59145(12) 0.0201(4) Uani 1 1 d . . . . . C018 C 0.55221(16) 0.51224(8) 0.90662(13) 0.0238(4) Uani 1 1 d . . . . . H018 H 0.5323 0.4817 0.9258 0.029 Uiso 1 1 calc R U . . . C019 C 0.84785(16) 0.44285(8) 0.52036(13) 0.0235(4) Uani 1 1 d . . . . . H019 H 0.8617 0.4752 0.5190 0.028 Uiso 1 1 calc R U . . . C01A C 0.63171(16) 0.53909(8) 0.79920(13) 0.0245(4) Uani 1 1 d . . . . . H01A H 0.6452 0.5677 0.8284 0.029 Uiso 1 1 calc R U . . . C01B C 0.99033(15) 0.37382(8) 0.92794(12) 0.0214(4) Uani 1 1 d . . . . . C01C C 0.80555(17) 0.26840(8) 0.88033(13) 0.0252(5) Uani 1 1 d . . . . . H01C H 0.7461 0.2660 0.9026 0.030 Uiso 1 1 calc R U . . . C01D C 0.54450(15) 0.28962(7) 0.96180(12) 0.0207(4) Uani 1 1 d . . . . . C01E C 0.46127(19) 0.54541(10) 0.89085(15) 0.0354(6) Uani 1 1 d . . . . . H01B H 0.4763 0.5741 0.8656 0.053 Uiso 1 1 calc R U . . . H01D H 0.4476 0.5529 0.9426 0.053 Uiso 1 1 calc R U . . . H01E H 0.4020 0.5303 0.8544 0.053 Uiso 1 1 calc R U . . . C01F C 0.89707(16) 0.41710(7) 0.58937(12) 0.0212(4) Uani 1 1 d . . . . . C01G C 0.69701(19) 0.15639(9) 1.02682(16) 0.0341(5) Uani 1 1 d . . . . . H01F H 0.7518 0.1789 1.0318 0.051 Uiso 1 1 calc R U . . . H01G H 0.7246 0.1247 1.0324 0.051 Uiso 1 1 calc R U . . . H01H H 0.6641 0.1622 1.0696 0.051 Uiso 1 1 calc R U . . . C01H C 0.7734(2) 0.43908(10) 0.30917(14) 0.0362(6) Uani 1 1 d . . . . . H01I H 0.8467 0.4435 0.3269 0.054 Uiso 1 1 calc R U . . . H01J H 0.7439 0.4594 0.2624 0.054 Uiso 1 1 calc R U . . . H01K H 0.7580 0.4065 0.2934 0.054 Uiso 1 1 calc R U . . . C01I C 1.07468(19) 0.44635(10) 0.63507(16) 0.0376(6) Uani 1 1 d . . . . . H01L H 1.0987 0.4155 0.6244 0.056 Uiso 1 1 calc R U . . . H01M H 1.1254 0.4612 0.6800 0.056 Uiso 1 1 calc R U . . . H01N H 1.0631 0.4657 0.5861 0.056 Uiso 1 1 calc R U . . . C01J C 0.8734(2) 0.22669(9) 0.91414(16) 0.0389(6) Uani 1 1 d . . . . . H01O H 0.9319 0.2270 0.8925 0.058 Uiso 1 1 calc R U . . . H01P H 0.8354 0.1977 0.8979 0.058 Uiso 1 1 calc R U . . . H01Q H 0.8963 0.2286 0.9737 0.058 Uiso 1 1 calc R U . . . C01K C 0.6152(2) 0.44563(11) 0.35340(17) 0.0410(6) Uani 1 1 d . . . . . H01R H 0.5981 0.4134 0.3358 0.061 Uiso 1 1 calc R U . . . H01S H 0.5851 0.4669 0.3083 0.061 Uiso 1 1 calc R U . . . H01T H 0.5889 0.4528 0.3996 0.061 Uiso 1 1 calc R U . . . C01L C 0.57964(16) 0.21075(8) 0.92392(13) 0.0240(4) Uani 1 1 d . . . . . C01M C 1.08122(16) 0.39275(8) 0.90489(13) 0.0242(5) Uani 1 1 d . . . . . H01U H 1.0784 0.3805 0.8496 0.029 Uiso 1 1 calc R U . . . C01N C 0.63892(18) 0.53225(9) 0.97405(14) 0.0317(5) Uani 1 1 d . . . . . H01V H 0.6992 0.5130 0.9802 0.048 Uiso 1 1 calc R U . . . H01W H 0.6205 0.5324 1.0253 0.048 Uiso 1 1 calc R U . . . H01X H 0.6528 0.5642 0.9600 0.048 Uiso 1 1 calc R U . . . C01O C 0.9576(2) 0.40051(11) 1.16867(15) 0.0437(7) Uani 1 1 d . . . . . H01Y H 0.9996 0.3724 1.1803 0.066 Uiso 1 1 calc R U . . . H H 0.9377 0.4094 1.2172 0.066 Uiso 1 1 calc R U . . . HA H 0.9959 0.4260 1.1535 0.066 Uiso 1 1 calc R U . . . C01P C 1.08741(17) 0.44547(8) 0.90177(14) 0.0286(5) Uani 1 1 d . . . . . H01Z H 1.0266 0.4576 0.8626 0.043 Uiso 1 1 calc R U . . . HB H 1.1468 0.4545 0.8848 0.043 Uiso 1 1 calc R U . . . HC H 1.0928 0.4584 0.9559 0.043 Uiso 1 1 calc R U . . . C01Q C 0.5335(2) 0.12693(8) 0.93390(16) 0.0345(5) Uani 1 1 d . . . . . H01 H 0.5604 0.0951 0.9410 0.052 Uiso 1 1 calc R U . . . HD H 0.4864 0.1301 0.8794 0.052 Uiso 1 1 calc R U . . . HE H 0.4981 0.1333 0.9750 0.052 Uiso 1 1 calc R U . . . C01R C 1.05362(17) 0.28308(8) 0.73065(13) 0.0257(5) Uani 1 1 d . . . . . H1 H 1.1038 0.2612 0.7270 0.031 Uiso 1 1 calc R U . . . C01S C 0.9409(2) 0.48809(9) 0.68192(15) 0.0359(6) Uani 1 1 d . . . . . H2 H 0.9303 0.5098 0.6360 0.054 Uiso 1 1 calc R U . . . HF H 0.9923 0.5007 0.7289 0.054 Uiso 1 1 calc R U . . . HG H 0.8775 0.4839 0.6961 0.054 Uiso 1 1 calc R U . . . C01T C 0.7859(2) 0.27298(9) 0.44174(15) 0.0329(5) Uani 1 1 d . . . . . H3 H 0.7345 0.2871 0.3964 0.049 Uiso 1 1 calc R U . . . HH H 0.7726 0.2395 0.4440 0.049 Uiso 1 1 calc R U . . . HI H 0.8527 0.2776 0.4337 0.049 Uiso 1 1 calc R U . . . C01U C 1.17500(17) 0.37210(9) 0.96566(16) 0.0331(5) Uani 1 1 d . . . . . H4 H 1.1793 0.3834 1.0206 0.050 Uiso 1 1 calc R U . . . HJ H 1.2354 0.3817 0.9506 0.050 Uiso 1 1 calc R U . . . HK H 1.1702 0.3380 0.9647 0.050 Uiso 1 1 calc R U . . . C01V C 0.76460(19) 0.26444(9) 0.78817(14) 0.0321(5) Uani 1 1 d . . . . . H5 H 0.7293 0.2933 0.7662 0.048 Uiso 1 1 calc R U . . . HL H 0.7176 0.2382 0.7745 0.048 Uiso 1 1 calc R U . . . HM H 0.8206 0.2593 0.7645 0.048 Uiso 1 1 calc R U . . . C01W C 0.78267(17) 0.29596(8) 0.52176(13) 0.0266(5) Uani 1 1 d . . . . . H6 H 0.8347 0.2805 0.5670 0.032 Uiso 1 1 calc R U . . . C01X C 0.7504(2) 0.61309(10) 0.75489(18) 0.0461(7) Uani 1 1 d . . . . . H7 H 0.6910 0.6288 0.7630 0.069 Uiso 1 1 calc R U . . . HN H 0.7889 0.6351 0.7316 0.069 Uiso 1 1 calc R U . . . HO H 0.7929 0.6017 0.8073 0.069 Uiso 1 1 calc R U . . . C01Y C 0.53298(16) 0.22208(8) 0.84285(13) 0.0241(4) Uani 1 1 d . . . . . H8 H 0.5279 0.1989 0.8023 0.029 Uiso 1 1 calc R U . . . C01Z C 0.7972(3) 0.43303(12) 1.07588(18) 0.0520(8) Uani 1 1 d . . . . . H9 H 0.8332 0.4573 1.0552 0.078 Uiso 1 1 calc R U . . . HP H 0.7797 0.4446 1.1240 0.078 Uiso 1 1 calc R U . . . HQ H 0.7354 0.4247 1.0337 0.078 Uiso 1 1 calc R U . . . C020 C 0.6797(2) 0.28795(10) 0.5365(2) 0.0482(7) Uani 1 1 d . . . . . H02A H 0.6800 0.3010 0.5895 0.072 Uiso 1 1 calc R U . . . H02B H 0.6658 0.2544 0.5359 0.072 Uiso 1 1 calc R U . . . H02C H 0.6273 0.3033 0.4935 0.072 Uiso 1 1 calc R U . . . C021 C 0.3370(2) 0.25224(14) 0.7082(2) 0.0647(10) Uani 1 1 d . . . . . H02D H 0.3460 0.2185 0.7153 0.097 Uiso 1 1 calc R U . . . H02E H 0.3009 0.2591 0.6513 0.097 Uiso 1 1 calc R U . . . H02F H 0.2980 0.2640 0.7438 0.097 Uiso 1 1 calc R U . . . C022 C 0.7170(2) 0.57222(9) 0.69706(16) 0.0346(5) Uani 1 1 d . . . . . H022 H 0.7786 0.5581 0.6871 0.042 Uiso 1 1 calc R U . . . C023 C 0.4973(3) 0.26060(17) 0.67157(17) 0.0709(12) Uani 1 1 d . . . . . H02G H 0.5615 0.2774 0.6841 0.106 Uiso 1 1 calc R U . . . H02H H 0.4579 0.2676 0.6156 0.106 Uiso 1 1 calc R U . . . H02I H 0.5103 0.2270 0.6772 0.106 Uiso 1 1 calc R U . . . C025 C 0.6507(3) 0.58978(12) 0.61636(19) 0.0627(10) Uani 1 1 d . . . . . H02J H 0.6277 0.5634 0.5795 0.094 Uiso 1 1 calc R U . . . H02K H 0.6892 0.6114 0.5923 0.094 Uiso 1 1 calc R U . . . H02L H 0.5921 0.6060 0.6250 0.094 Uiso 1 1 calc R U . . . C5 C 0.8710(2) 0.51214(12) 0.89355(16) 0.0435(7) Uani 1 1 d . . . . . H003 H 0.805(2) 0.3944(10) 0.7018(18) 0.039(8) Uiso 1 1 d . . . . . H004 H 0.645(2) 0.3440(10) 0.8738(16) 0.032(7) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y001 0.01581(9) 0.02155(10) 0.01984(9) -0.00284(7) 0.00814(6) -0.00151(7) N26 0.0108(7) 0.0155(9) 0.0166(8) 0.0015(7) 0.0063(6) 0.0016(7) N003 0.0199(8) 0.0237(9) 0.0186(8) -0.0004(7) 0.0073(7) 0.0033(7) N004 0.0160(8) 0.0195(9) 0.0255(9) 0.0035(7) 0.0075(7) 0.0001(7) C005 0.0196(10) 0.0237(11) 0.0195(10) 0.0013(8) 0.0061(8) 0.0020(8) C006 0.0264(11) 0.0310(12) 0.0246(11) 0.0046(9) 0.0135(9) 0.0007(9) C007 0.0210(10) 0.0287(12) 0.0209(10) 0.0017(9) 0.0081(8) -0.0006(9) C008 0.0181(9) 0.0236(11) 0.0188(10) -0.0028(8) 0.0069(8) -0.0024(8) C009 0.0286(12) 0.0318(13) 0.0232(11) 0.0000(9) 0.0038(9) -0.0020(10) C00A 0.0173(9) 0.0237(11) 0.0184(9) -0.0008(8) 0.0047(7) 0.0040(8) C00B 0.0388(13) 0.0284(12) 0.0222(11) -0.0020(9) 0.0111(10) -0.0040(10) C00C 0.0227(10) 0.0235(11) 0.0223(10) 0.0008(8) 0.0082(8) 0.0010(9) C00D 0.0309(12) 0.0303(12) 0.0250(11) 0.0053(9) 0.0091(9) 0.0032(10) C00E 0.0204(10) 0.0202(10) 0.0191(9) -0.0025(8) 0.0078(8) -0.0016(8) C00F 0.0173(9) 0.0224(10) 0.0172(9) 0.0013(8) 0.0063(7) 0.0004(8) C00G 0.0231(10) 0.0293(12) 0.0194(10) -0.0028(9) 0.0064(8) 0.0006(9) C00H 0.0180(10) 0.0233(11) 0.0214(10) 0.0036(8) 0.0066(8) -0.0008(8) C00I 0.0247(11) 0.0196(10) 0.0238(10) 0.0033(8) 0.0070(8) -0.0016(8) C00J 0.0197(10) 0.0261(11) 0.0198(10) -0.0044(8) 0.0048(8) -0.0033(8) C00K 0.0187(10) 0.0269(11) 0.0229(10) 0.0024(9) 0.0071(8) -0.0047(8) C00L 0.0218(10) 0.0230(11) 0.0262(11) 0.0038(9) 0.0085(8) 0.0038(8) C00M 0.0283(11) 0.0339(13) 0.0241(11) 0.0011(10) 0.0077(9) -0.0024(10) C00N 0.0292(11) 0.0363(13) 0.0234(11) -0.0066(9) 0.0151(9) -0.0082(10) C00O 0.0175(9) 0.0199(10) 0.0208(10) -0.0020(8) 0.0066(8) -0.0023(8) C00P 0.0290(12) 0.0561(17) 0.0269(12) -0.0107(12) 0.0046(10) 0.0084(12) C00Q 0.0173(9) 0.0218(10) 0.0165(9) 0.0019(8) 0.0058(7) 0.0000(8) C00R 0.0279(12) 0.0328(13) 0.0341(12) -0.0055(10) 0.0107(10) 0.0023(10) C00S 0.0224(10) 0.0244(11) 0.0313(11) 0.0062(9) 0.0092(9) 0.0001(9) C00T 0.0171(9) 0.0229(11) 0.0198(10) 0.0055(8) 0.0063(8) 0.0018(8) C00U 0.0175(10) 0.0261(11) 0.0283(11) 0.0054(9) 0.0086(8) -0.0023(8) C00V 0.0329(14) 0.106(3) 0.0390(15) -0.0355(17) 0.0153(12) -0.0216(16) C00W 0.0294(11) 0.0241(11) 0.0235(10) -0.0007(9) 0.0076(9) -0.0036(9) C00X 0.0181(9) 0.0214(10) 0.0219(10) 0.0031(8) 0.0054(8) 0.0027(8) C00Y 0.0214(10) 0.0264(11) 0.0208(10) -0.0019(8) 0.0095(8) 0.0006(9) C00Z 0.0152(9) 0.0220(11) 0.0246(10) 0.0039(8) 0.0071(8) -0.0031(8) C010 0.0207(10) 0.0250(11) 0.0220(10) 0.0053(8) 0.0079(8) 0.0010(8) C011 0.0250(11) 0.0292(12) 0.0234(10) 0.0035(9) 0.0122(9) 0.0035(9) C012 0.0286(11) 0.0261(12) 0.0341(12) 0.0030(10) 0.0167(10) 0.0054(9) C013 0.0159(9) 0.0322(12) 0.0314(11) 0.0047(10) 0.0090(8) 0.0021(9) C014 0.0232(10) 0.0247(11) 0.0223(10) -0.0007(9) 0.0054(8) 0.0020(9) C015 0.0256(11) 0.0267(11) 0.0217(10) -0.0039(9) 0.0105(8) 0.0019(9) C016 0.0208(10) 0.0302(12) 0.0176(10) 0.0003(8) 0.0060(8) 0.0013(9) C017 0.0200(10) 0.0233(11) 0.0196(10) -0.0011(8) 0.0100(8) 0.0013(8) C018 0.0248(11) 0.0246(11) 0.0234(10) -0.0017(9) 0.0092(8) -0.0005(9) C019 0.0253(11) 0.0235(11) 0.0242(10) 0.0014(9) 0.0112(8) 0.0000(9) C01A 0.0234(10) 0.0219(11) 0.0286(11) 0.0021(9) 0.0079(9) 0.0009(9) C01B 0.0165(9) 0.0281(11) 0.0194(10) 0.0004(8) 0.0048(8) 0.0014(8) C01C 0.0274(11) 0.0228(11) 0.0275(11) -0.0006(9) 0.0111(9) -0.0051(9) C01D 0.0177(9) 0.0218(11) 0.0236(10) 0.0022(8) 0.0074(8) -0.0034(8) C01E 0.0323(13) 0.0422(15) 0.0332(13) -0.0040(11) 0.0117(10) 0.0083(11) C01F 0.0227(10) 0.0223(11) 0.0215(10) -0.0014(8) 0.0107(8) 0.0001(8) C01G 0.0303(12) 0.0305(13) 0.0424(14) 0.0092(11) 0.0120(11) 0.0096(10) C01H 0.0392(14) 0.0445(15) 0.0262(12) 0.0088(11) 0.0113(10) 0.0057(12) C01I 0.0288(12) 0.0464(16) 0.0372(13) -0.0095(12) 0.0089(10) -0.0096(11) C01J 0.0441(15) 0.0288(13) 0.0399(14) 0.0033(11) 0.0055(11) -0.0020(11) C01K 0.0320(13) 0.0500(17) 0.0404(14) 0.0174(13) 0.0094(11) 0.0067(12) C01L 0.0216(10) 0.0234(11) 0.0303(11) 0.0030(9) 0.0127(9) -0.0014(9) C01M 0.0180(10) 0.0321(12) 0.0244(10) -0.0067(9) 0.0093(8) -0.0035(9) C01N 0.0294(12) 0.0382(14) 0.0280(12) -0.0042(10) 0.0088(9) -0.0022(10) C01O 0.0444(15) 0.0625(19) 0.0267(12) -0.0098(13) 0.0141(11) -0.0084(14) C01P 0.0243(11) 0.0339(13) 0.0310(12) -0.0017(10) 0.0134(9) -0.0044(10) C01Q 0.0411(14) 0.0234(12) 0.0407(14) 0.0012(10) 0.0140(11) -0.0027(10) C01R 0.0254(11) 0.0261(11) 0.0273(11) -0.0044(9) 0.0100(9) 0.0068(9) C01S 0.0456(15) 0.0289(13) 0.0316(12) -0.0065(10) 0.0081(11) -0.0003(11) C01T 0.0381(13) 0.0267(12) 0.0336(12) -0.0095(10) 0.0094(10) -0.0004(10) C01U 0.0200(11) 0.0375(14) 0.0427(14) 0.0021(11) 0.0102(10) 0.0018(10) C01V 0.0320(12) 0.0317(13) 0.0306(12) -0.0043(10) 0.0053(10) -0.0098(10) C01W 0.0298(11) 0.0241(11) 0.0250(11) -0.0025(9) 0.0061(9) 0.0002(9) C01X 0.0517(17) 0.0383(15) 0.0478(16) 0.0061(13) 0.0133(13) -0.0175(13) C01Y 0.0249(11) 0.0226(11) 0.0268(11) -0.0030(9) 0.0103(9) -0.0053(9) C01Z 0.0606(19) 0.063(2) 0.0411(15) -0.0045(14) 0.0290(14) 0.0173(16) C020 0.0541(18) 0.0301(14) 0.075(2) -0.0080(14) 0.0418(16) -0.0117(13) C021 0.0381(17) 0.090(3) 0.0501(18) 0.0198(18) -0.0141(14) -0.0199(17) C022 0.0363(13) 0.0314(13) 0.0420(14) 0.0054(11) 0.0205(11) -0.0060(11) C023 0.0494(19) 0.141(4) 0.0216(13) 0.0109(17) 0.0088(12) 0.025(2) C025 0.082(2) 0.058(2) 0.0437(17) 0.0172(15) 0.0098(16) -0.0347(18) C5 0.0347(14) 0.066(2) 0.0312(13) 0.0035(14) 0.0118(11) 0.0134(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y001 N003 2.2202(17) . ? Y001 N004 2.2206(17) . ? Y001 N26 2.3481(18) . ? Y001 C00A 2.800(2) . ? Y001 C005 2.827(2) . ? Y001 C007 2.880(2) . ? Y001 C01B 2.893(2) . ? Y001 C00J 2.939(2) . ? Y001 C016 2.958(2) . ? N26 C5 1.039(4) . ? N003 C00O 1.386(3) . ? N003 H003 0.90(3) . ? N004 C00Q 1.391(3) . ? N004 H004 0.89(3) . ? C005 C007 1.402(3) . ? C005 C00A 1.413(3) . ? C005 C01C 1.529(3) . ? C006 C00S 1.395(3) . ? C006 C00C 1.397(3) . ? C006 H006 0.9500 . ? C007 C016 1.391(3) . ? C007 H007 0.9500 . ? C008 C014 1.387(3) . ? C008 C00O 1.413(3) . ? C008 C00A 1.491(3) . ? C009 C021 1.509(4) . ? C009 C023 1.513(4) . ? C009 C00K 1.527(3) . ? C009 H009 1.0000 . ? C00A C01B 1.424(3) . ? C00B C00V 1.517(4) . ? C00B C00C 1.524(3) . ? C00B C00P 1.528(3) . ? C00B H00B 1.0000 . ? C00C C00T 1.424(3) . ? C00D C011 1.518(3) . ? C00D C01K 1.520(3) . ? C00D C01H 1.531(3) . ? C00D H00D 1.0000 . ? C00E C015 1.394(3) . ? C00E C00O 1.418(3) . ? C00E C017 1.498(3) . ? C00F C00L 1.401(3) . ? C00F C00Q 1.409(3) . ? C00F C00T 1.498(3) . ? C00G C011 1.390(3) . ? C00G C00Y 1.397(3) . ? C00G H00G 0.9500 . ? C00H C00U 1.391(3) . ? C00H C00Q 1.421(3) . ? C00H C00Z 1.499(3) . ? C00I C00M 1.521(3) . ? C00I C01D 1.527(3) . ? C00I C00R 1.532(3) . ? C00I H00I 1.0000 . ? C00J C01B 1.401(3) . ? C00J C016 1.402(3) . ? C00J H00J 0.9500 . ? C00K C01Y 1.391(3) . ? C00K C00Z 1.407(3) . ? C00L C013 1.380(3) . ? C00L H00L 0.9500 . ? C00M H00A 0.9800 . ? C00M H00C 0.9800 . ? C00M H00E 0.9800 . ? C00N C01Z 1.503(4) . ? C00N C016 1.521(3) . ? C00N C01O 1.528(4) . ? C00N H00N 1.0000 . ? C00P H00F 0.9800 . ? C00P H00H 0.9800 . ? C00P H00K 0.9800 . ? C00R H00M 0.9800 . ? C00R H00O 0.9800 . ? C00R H00P 0.9800 . ? C00S C01A 1.382(3) . ? C00S C022 1.525(3) . ? C00T C00X 1.402(3) . ? C00U C013 1.392(3) . ? C00U H00U 0.9500 . ? C00V H00Q 0.9800 . ? C00V H00R 0.9800 . ? C00V H00S 0.9800 . ? C00W C01F 1.525(3) . ? C00W C01S 1.527(3) . ? C00W C01I 1.529(3) . ? C00W H00W 1.0000 . ? C00X C01A 1.401(3) . ? C00X C018 1.527(3) . ? C00Y C017 1.410(3) . ? C00Y C01W 1.524(3) . ? C00Z C01D 1.408(3) . ? C010 C01D 1.391(3) . ? C010 C01L 1.396(3) . ? C010 H010 0.9500 . ? C011 C019 1.383(3) . ? C012 C01L 1.518(3) . ? C012 C01G 1.522(3) . ? C012 C01Q 1.533(3) . ? C012 H012 1.0000 . ? C013 H013 0.9500 . ? C014 C01R 1.389(3) . ? C014 H014 0.9500 . ? C015 C01R 1.387(3) . ? C015 H015 0.9500 . ? C017 C01F 1.411(3) . ? C018 C01N 1.523(3) . ? C018 C01E 1.538(3) . ? C018 H018 1.0000 . ? C019 C01F 1.397(3) . ? C019 H019 0.9500 . ? C01A H01A 0.9500 . ? C01B C01M 1.519(3) . ? C01C C01V 1.523(3) . ? C01C C01J 1.529(3) . ? C01C H01C 1.0000 . ? C01E H01B 0.9800 . ? C01E H01D 0.9800 . ? C01E H01E 0.9800 . ? C01G H01F 0.9800 . ? C01G H01G 0.9800 . ? C01G H01H 0.9800 . ? C01H H01I 0.9800 . ? C01H H01J 0.9800 . ? C01H H01K 0.9800 . ? C01I H01L 0.9800 . ? C01I H01M 0.9800 . ? C01I H01N 0.9800 . ? C01J H01O 0.9800 . ? C01J H01P 0.9800 . ? C01J H01Q 0.9800 . ? C01K H01R 0.9800 . ? C01K H01S 0.9800 . ? C01K H01T 0.9800 . ? C01L C01Y 1.394(3) . ? C01M C01P 1.516(3) . ? C01M C01U 1.534(3) . ? C01M H01U 1.0000 . ? C01N H01V 0.9800 . ? C01N H01W 0.9800 . ? C01N H01X 0.9800 . ? C01O H01Y 0.9800 . ? C01O H 0.9800 . ? C01O HA 0.9800 . ? C01P H01Z 0.9800 . ? C01P HB 0.9800 . ? C01P HC 0.9800 . ? C01Q H01 0.9800 . ? C01Q HD 0.9800 . ? C01Q HE 0.9800 . ? C01R H1 0.9500 . ? C01S H2 0.9800 . ? C01S HF 0.9800 . ? C01S HG 0.9800 . ? C01T C01W 1.532(3) . ? C01T H3 0.9800 . ? C01T HH 0.9800 . ? C01T HI 0.9800 . ? C01U H4 0.9800 . ? C01U HJ 0.9800 . ? C01U HK 0.9800 . ? C01V H5 0.9800 . ? C01V HL 0.9800 . ? C01V HM 0.9800 . ? C01W C020 1.531(3) . ? C01W H6 1.0000 . ? C01X C022 1.520(4) . ? C01X H7 0.9800 . ? C01X HN 0.9800 . ? C01X HO 0.9800 . ? C01Y H8 0.9500 . ? C01Z H9 0.9800 . ? C01Z HP 0.9800 . ? C01Z HQ 0.9800 . ? C020 H02A 0.9800 . ? C020 H02B 0.9800 . ? C020 H02C 0.9800 . ? C021 H02D 0.9800 . ? C021 H02E 0.9800 . ? C021 H02F 0.9800 . ? C022 C025 1.513(4) . ? C022 H022 1.0000 . ? C023 H02G 0.9800 . ? C023 H02H 0.9800 . ? C023 H02I 0.9800 . ? C025 H02J 0.9800 . ? C025 H02K 0.9800 . ? C025 H02L 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N003 Y001 N004 112.32(7) . . ? N003 Y001 N26 106.93(6) . . ? N004 Y001 N26 126.54(6) . . ? N003 Y001 C00A 63.78(6) . . ? N004 Y001 C00A 113.43(7) . . ? N26 Y001 C00A 115.87(6) . . ? N003 Y001 C005 81.65(6) . . ? N004 Y001 C005 85.79(6) . . ? N26 Y001 C005 135.52(6) . . ? C00A Y001 C005 29.07(6) . . ? N003 Y001 C007 109.86(6) . . ? N004 Y001 C007 78.60(6) . . ? N26 Y001 C007 119.91(6) . . ? C00A Y001 C007 50.24(6) . . ? C005 Y001 C007 28.43(6) . . ? N003 Y001 C01B 76.85(6) . . ? N004 Y001 C01B 135.01(6) . . ? N26 Y001 C01B 87.76(6) . . ? C00A Y001 C01B 28.90(6) . . ? C005 Y001 C01B 50.89(6) . . ? C007 Y001 C01B 57.70(6) . . ? N003 Y001 C00J 104.51(6) . . ? N004 Y001 C00J 123.52(6) . . ? N26 Y001 C00J 77.23(6) . . ? C00A Y001 C00J 50.22(6) . . ? C005 Y001 C00J 58.56(6) . . ? C007 Y001 C00J 48.67(6) . . ? C01B Y001 C00J 27.79(6) . . ? N003 Y001 C016 122.06(6) . . ? N004 Y001 C016 96.06(6) . . ? N26 Y001 C016 92.40(6) . . ? C00A Y001 C016 58.66(6) . . ? C005 Y001 C016 50.17(6) . . ? C007 Y001 C016 27.53(6) . . ? C01B Y001 C016 49.29(6) . . ? C00J Y001 C016 27.51(6) . . ? C5 N26 Y001 170.38(19) . . ? C00O N003 Y001 133.19(14) . . ? C00O N003 H003 108.7(18) . . ? Y001 N003 H003 117.9(18) . . ? C00Q N004 Y001 145.40(15) . . ? C00Q N004 H004 108.7(18) . . ? Y001 N004 H004 105.9(18) . . ? C007 C005 C00A 117.96(19) . . ? C007 C005 C01C 117.20(18) . . ? C00A C005 C01C 124.66(18) . . ? C007 C005 Y001 77.90(13) . . ? C00A C005 Y001 74.41(12) . . ? C01C C005 Y001 121.81(14) . . ? C00S C006 C00C 122.8(2) . . ? C00S C006 H006 118.6 . . ? C00C C006 H006 118.6 . . ? C016 C007 C005 123.02(19) . . ? C016 C007 Y001 79.33(13) . . ? C005 C007 Y001 73.66(12) . . ? C016 C007 H007 118.5 . . ? C005 C007 H007 118.5 . . ? Y001 C007 H007 119.3 . . ? C014 C008 C00O 121.89(18) . . ? C014 C008 C00A 122.90(19) . . ? C00O C008 C00A 114.77(18) . . ? C021 C009 C023 110.2(3) . . ? C021 C009 C00K 109.3(2) . . ? C023 C009 C00K 113.7(2) . . ? C021 C009 H009 107.8 . . ? C023 C009 H009 107.8 . . ? C00K C009 H009 107.8 . . ? C005 C00A C01B 120.17(18) . . ? C005 C00A C008 122.95(19) . . ? C01B C00A C008 116.61(18) . . ? C005 C00A Y001 76.52(12) . . ? C01B C00A Y001 79.18(12) . . ? C008 C00A Y001 109.86(13) . . ? C00V C00B C00C 110.8(2) . . ? C00V C00B C00P 107.3(2) . . ? C00C C00B C00P 114.7(2) . . ? C00V C00B H00B 107.9 . . ? C00C C00B H00B 107.9 . . ? C00P C00B H00B 107.9 . . ? C006 C00C C00T 118.1(2) . . ? C006 C00C C00B 120.20(19) . . ? C00T C00C C00B 121.29(19) . . ? C011 C00D C01K 112.07(19) . . ? C011 C00D C01H 110.07(19) . . ? C01K C00D C01H 111.0(2) . . ? C011 C00D H00D 107.8 . . ? C01K C00D H00D 107.8 . . ? C01H C00D H00D 107.8 . . ? C015 C00E C00O 119.00(19) . . ? C015 C00E C017 120.49(18) . . ? C00O C00E C017 120.49(18) . . ? C00L C00F C00Q 119.70(19) . . ? C00L C00F C00T 118.79(18) . . ? C00Q C00F C00T 121.44(17) . . ? C011 C00G C00Y 122.2(2) . . ? C011 C00G H00G 118.9 . . ? C00Y C00G H00G 118.9 . . ? C00U C00H C00Q 120.5(2) . . ? C00U C00H C00Z 120.21(18) . . ? C00Q C00H C00Z 119.15(18) . . ? C00M C00I C01D 114.33(18) . . ? C00M C00I C00R 108.80(18) . . ? C01D C00I C00R 110.15(18) . . ? C00M C00I H00I 107.8 . . ? C01D C00I H00I 107.8 . . ? C00R C00I H00I 107.8 . . ? C01B C00J C016 121.0(2) . . ? C01B C00J Y001 74.27(12) . . ? C016 C00J Y001 76.97(12) . . ? C01B C00J H00J 119.5 . . ? C016 C00J H00J 119.5 . . ? Y001 C00J H00J 120.3 . . ? C01Y C00K C00Z 118.87(19) . . ? C01Y C00K C009 119.9(2) . . ? C00Z C00K C009 121.2(2) . . ? C013 C00L C00F 122.0(2) . . ? C013 C00L H00L 119.0 . . ? C00F C00L H00L 119.0 . . ? C00I C00M H00A 109.5 . . ? C00I C00M H00C 109.5 . . ? H00A C00M H00C 109.5 . . ? C00I C00M H00E 109.5 . . ? H00A C00M H00E 109.5 . . ? H00C C00M H00E 109.5 . . ? C01Z C00N C016 110.2(2) . . ? C01Z C00N C01O 112.1(2) . . ? C016 C00N C01O 111.97(19) . . ? C01Z C00N H00N 107.4 . . ? C016 C00N H00N 107.4 . . ? C01O C00N H00N 107.4 . . ? N003 C00O C008 118.12(18) . . ? N003 C00O C00E 124.07(19) . . ? C008 C00O C00E 117.78(18) . . ? C00B C00P H00F 109.5 . . ? C00B C00P H00H 109.5 . . ? H00F C00P H00H 109.5 . . ? C00B C00P H00K 109.5 . . ? H00F C00P H00K 109.5 . . ? H00H C00P H00K 109.5 . . ? N004 C00Q C00F 120.33(18) . . ? N004 C00Q C00H 121.64(19) . . ? C00F C00Q C00H 118.02(18) . . ? C00I C00R H00M 109.5 . . ? C00I C00R H00O 109.5 . . ? H00M C00R H00O 109.5 . . ? C00I C00R H00P 109.5 . . ? H00M C00R H00P 109.5 . . ? H00O C00R H00P 109.5 . . ? C01A C00S C006 117.8(2) . . ? C01A C00S C022 122.7(2) . . ? C006 C00S C022 119.6(2) . . ? C00X C00T C00C 119.62(19) . . ? C00X C00T C00F 120.45(18) . . ? C00C C00T C00F 119.58(19) . . ? C00H C00U C013 121.01(19) . . ? C00H C00U H00U 119.5 . . ? C013 C00U H00U 119.5 . . ? C00B C00V H00Q 109.5 . . ? C00B C00V H00R 109.5 . . ? H00Q C00V H00R 109.5 . . ? C00B C00V H00S 109.5 . . ? H00Q C00V H00S 109.5 . . ? H00R C00V H00S 109.5 . . ? C01F C00W C01S 113.1(2) . . ? C01F C00W C01I 110.02(18) . . ? C01S C00W C01I 110.8(2) . . ? C01F C00W H00W 107.6 . . ? C01S C00W H00W 107.6 . . ? C01I C00W H00W 107.6 . . ? C01A C00X C00T 119.56(19) . . ? C01A C00X C018 118.25(19) . . ? C00T C00X C018 122.16(18) . . ? C00G C00Y C017 118.8(2) . . ? C00G C00Y C01W 118.68(19) . . ? C017 C00Y C01W 122.53(19) . . ? C00K C00Z C01D 120.0(2) . . ? C00K C00Z C00H 119.04(18) . . ? C01D C00Z C00H 120.95(19) . . ? C01D C010 C01L 122.1(2) . . ? C01D C010 H010 118.9 . . ? C01L C010 H010 118.9 . . ? C019 C011 C00G 118.2(2) . . ? C019 C011 C00D 120.8(2) . . ? C00G C011 C00D 121.0(2) . . ? C01L C012 C01G 114.7(2) . . ? C01L C012 C01Q 110.41(19) . . ? C01G C012 C01Q 110.8(2) . . ? C01L C012 H012 106.8 . . ? C01G C012 H012 106.8 . . ? C01Q C012 H012 106.8 . . ? C00L C013 C00U 118.73(19) . . ? C00L C013 H013 120.6 . . ? C00U C013 H013 120.6 . . ? C008 C014 C01R 119.9(2) . . ? C008 C014 H014 120.0 . . ? C01R C014 H014 120.0 . . ? C01R C015 C00E 122.43(19) . . ? C01R C015 H015 118.8 . . ? C00E C015 H015 118.8 . . ? C007 C016 C00J 118.37(19) . . ? C007 C016 C00N 120.55(19) . . ? C00J C016 C00N 121.1(2) . . ? C007 C016 Y001 73.14(12) . . ? C00J C016 Y001 75.53(12) . . ? C00N C016 Y001 122.30(15) . . ? C00Y C017 C01F 119.73(19) . . ? C00Y C017 C00E 120.67(19) . . ? C01F C017 C00E 119.60(18) . . ? C01N C018 C00X 112.32(18) . . ? C01N C018 C01E 109.24(19) . . ? C00X C018 C01E 110.70(18) . . ? C01N C018 H018 108.2 . . ? C00X C018 H018 108.2 . . ? C01E C018 H018 108.2 . . ? C011 C019 C01F 122.1(2) . . ? C011 C019 H019 118.9 . . ? C01F C019 H019 118.9 . . ? C00S C01A C00X 122.0(2) . . ? C00S C01A H01A 119.0 . . ? C00X C01A H01A 119.0 . . ? C00J C01B C00A 119.38(19) . . ? C00J C01B C01M 119.92(19) . . ? C00A C01B C01M 120.47(18) . . ? C00J C01B Y001 77.94(12) . . ? C00A C01B Y001 71.91(11) . . ? C01M C01B Y001 125.69(14) . . ? C01V C01C C005 117.43(18) . . ? C01V C01C C01J 110.1(2) . . ? C005 C01C C01J 109.27(19) . . ? C01V C01C H01C 106.5 . . ? C005 C01C H01C 106.5 . . ? C01J C01C H01C 106.5 . . ? C010 C01D C00Z 119.0(2) . . ? C010 C01D C00I 121.26(18) . . ? C00Z C01D C00I 119.67(19) . . ? C018 C01E H01B 109.5 . . ? C018 C01E H01D 109.5 . . ? H01B C01E H01D 109.5 . . ? C018 C01E H01E 109.5 . . ? H01B C01E H01E 109.5 . . ? H01D C01E H01E 109.5 . . ? C019 C01F C017 119.0(2) . . ? C019 C01F C00W 119.08(19) . . ? C017 C01F C00W 121.83(19) . . ? C012 C01G H01F 109.5 . . ? C012 C01G H01G 109.5 . . ? H01F C01G H01G 109.5 . . ? C012 C01G H01H 109.5 . . ? H01F C01G H01H 109.5 . . ? H01G C01G H01H 109.5 . . ? C00D C01H H01I 109.5 . . ? C00D C01H H01J 109.5 . . ? H01I C01H H01J 109.5 . . ? C00D C01H H01K 109.5 . . ? H01I C01H H01K 109.5 . . ? H01J C01H H01K 109.5 . . ? C00W C01I H01L 109.5 . . ? C00W C01I H01M 109.5 . . ? H01L C01I H01M 109.5 . . ? C00W C01I H01N 109.5 . . ? H01L C01I H01N 109.5 . . ? H01M C01I H01N 109.5 . . ? C01C C01J H01O 109.5 . . ? C01C C01J H01P 109.5 . . ? H01O C01J H01P 109.5 . . ? C01C C01J H01Q 109.5 . . ? H01O C01J H01Q 109.5 . . ? H01P C01J H01Q 109.5 . . ? C00D C01K H01R 109.5 . . ? C00D C01K H01S 109.5 . . ? H01R C01K H01S 109.5 . . ? C00D C01K H01T 109.5 . . ? H01R C01K H01T 109.5 . . ? H01S C01K H01T 109.5 . . ? C01Y C01L C010 117.6(2) . . ? C01Y C01L C012 118.5(2) . . ? C010 C01L C012 123.9(2) . . ? C01P C01M C01B 115.12(18) . . ? C01P C01M C01U 111.32(19) . . ? C01B C01M C01U 106.78(18) . . ? C01P C01M H01U 107.8 . . ? C01B C01M H01U 107.8 . . ? C01U C01M H01U 107.8 . . ? C018 C01N H01V 109.5 . . ? C018 C01N H01W 109.5 . . ? H01V C01N H01W 109.5 . . ? C018 C01N H01X 109.5 . . ? H01V C01N H01X 109.5 . . ? H01W C01N H01X 109.5 . . ? C00N C01O H01Y 109.5 . . ? C00N C01O H 109.5 . . ? H01Y C01O H 109.5 . . ? C00N C01O HA 109.5 . . ? H01Y C01O HA 109.5 . . ? H C01O HA 109.5 . . ? C01M C01P H01Z 109.5 . . ? C01M C01P HB 109.5 . . ? H01Z C01P HB 109.5 . . ? C01M C01P HC 109.5 . . ? H01Z C01P HC 109.5 . . ? HB C01P HC 109.5 . . ? C012 C01Q H01 109.5 . . ? C012 C01Q HD 109.5 . . ? H01 C01Q HD 109.5 . . ? C012 C01Q HE 109.5 . . ? H01 C01Q HE 109.5 . . ? HD C01Q HE 109.5 . . ? C015 C01R C014 119.0(2) . . ? C015 C01R H1 120.5 . . ? C014 C01R H1 120.5 . . ? C00W C01S H2 109.5 . . ? C00W C01S HF 109.5 . . ? H2 C01S HF 109.5 . . ? C00W C01S HG 109.5 . . ? H2 C01S HG 109.5 . . ? HF C01S HG 109.5 . . ? C01W C01T H3 109.5 . . ? C01W C01T HH 109.5 . . ? H3 C01T HH 109.5 . . ? C01W C01T HI 109.5 . . ? H3 C01T HI 109.5 . . ? HH C01T HI 109.5 . . ? C01M C01U H4 109.5 . . ? C01M C01U HJ 109.5 . . ? H4 C01U HJ 109.5 . . ? C01M C01U HK 109.5 . . ? H4 C01U HK 109.5 . . ? HJ C01U HK 109.5 . . ? C01C C01V H5 109.5 . . ? C01C C01V HL 109.5 . . ? H5 C01V HL 109.5 . . ? C01C C01V HM 109.5 . . ? H5 C01V HM 109.5 . . ? HL C01V HM 109.5 . . ? C00Y C01W C020 111.16(19) . . ? C00Y C01W C01T 112.08(19) . . ? C020 C01W C01T 110.2(2) . . ? C00Y C01W H6 107.7 . . ? C020 C01W H6 107.7 . . ? C01T C01W H6 107.7 . . ? C022 C01X H7 109.5 . . ? C022 C01X HN 109.5 . . ? H7 C01X HN 109.5 . . ? C022 C01X HO 109.5 . . ? H7 C01X HO 109.5 . . ? HN C01X HO 109.5 . . ? C00K C01Y C01L 122.4(2) . . ? C00K C01Y H8 118.8 . . ? C01L C01Y H8 118.8 . . ? C00N C01Z H9 109.5 . . ? C00N C01Z HP 109.5 . . ? H9 C01Z HP 109.5 . . ? C00N C01Z HQ 109.5 . . ? H9 C01Z HQ 109.5 . . ? HP C01Z HQ 109.5 . . ? C01W C020 H02A 109.5 . . ? C01W C020 H02B 109.5 . . ? H02A C020 H02B 109.5 . . ? C01W C020 H02C 109.5 . . ? H02A C020 H02C 109.5 . . ? H02B C020 H02C 109.5 . . ? C009 C021 H02D 109.5 . . ? C009 C021 H02E 109.5 . . ? H02D C021 H02E 109.5 . . ? C009 C021 H02F 109.5 . . ? H02D C021 H02F 109.5 . . ? H02E C021 H02F 109.5 . . ? C025 C022 C01X 109.4(2) . . ? C025 C022 C00S 109.7(2) . . ? C01X C022 C00S 114.3(2) . . ? C025 C022 H022 107.8 . . ? C01X C022 H022 107.8 . . ? C00S C022 H022 107.8 . . ? C009 C023 H02G 109.5 . . ? C009 C023 H02H 109.5 . . ? H02G C023 H02H 109.5 . . ? C009 C023 H02I 109.5 . . ? H02G C023 H02I 109.5 . . ? H02H C023 H02I 109.5 . . ? C022 C025 H02J 109.5 . . ? C022 C025 H02K 109.5 . . ? H02J C025 H02K 109.5 . . ? C022 C025 H02L 109.5 . . ? H02J C025 H02L 109.5 . . ? H02K C025 H02L 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C00A C005 C007 C016 -0.3(3) . . . . ? C01C C005 C007 C016 175.1(2) . . . . ? Y001 C005 C007 C016 -65.1(2) . . . . ? C00A C005 C007 Y001 64.85(17) . . . . ? C01C C005 C007 Y001 -119.74(18) . . . . ? C007 C005 C00A C01B 2.0(3) . . . . ? C01C C005 C00A C01B -173.1(2) . . . . ? Y001 C005 C00A C01B 68.74(18) . . . . ? C007 C005 C00A C008 -171.9(2) . . . . ? C01C C005 C00A C008 13.1(3) . . . . ? Y001 C005 C00A C008 -105.12(19) . . . . ? C007 C005 C00A Y001 -66.77(18) . . . . ? C01C C005 C00A Y001 118.2(2) . . . . ? C014 C008 C00A C005 -95.5(3) . . . . ? C00O C008 C00A C005 92.0(2) . . . . ? C014 C008 C00A C01B 90.5(3) . . . . ? C00O C008 C00A C01B -82.1(2) . . . . ? C014 C008 C00A Y001 178.05(17) . . . . ? C00O C008 C00A Y001 5.5(2) . . . . ? C00S C006 C00C C00T -3.8(3) . . . . ? C00S C006 C00C C00B 168.7(2) . . . . ? C00V C00B C00C C006 -101.8(3) . . . . ? C00P C00B C00C C006 19.9(3) . . . . ? C00V C00B C00C C00T 70.4(3) . . . . ? C00P C00B C00C C00T -167.9(2) . . . . ? C021 C009 C00K C01Y 73.2(3) . . . . ? C023 C009 C00K C01Y -50.4(3) . . . . ? C021 C009 C00K C00Z -103.3(3) . . . . ? C023 C009 C00K C00Z 133.1(3) . . . . ? C00Q C00F C00L C013 -1.5(3) . . . . ? C00T C00F C00L C013 175.5(2) . . . . ? Y001 N003 C00O C008 3.1(3) . . . . ? Y001 N003 C00O C00E -174.91(15) . . . . ? C014 C008 C00O N003 -178.5(2) . . . . ? C00A C008 C00O N003 -5.9(3) . . . . ? C014 C008 C00O C00E -0.4(3) . . . . ? C00A C008 C00O C00E 172.26(18) . . . . ? C015 C00E C00O N003 178.5(2) . . . . ? C017 C00E C00O N003 0.1(3) . . . . ? C015 C00E C00O C008 0.5(3) . . . . ? C017 C00E C00O C008 -177.90(18) . . . . ? Y001 N004 C00Q C00F 3.9(4) . . . . ? Y001 N004 C00Q C00H -177.07(17) . . . . ? C00L C00F C00Q N004 -178.00(19) . . . . ? C00T C00F C00Q N004 5.0(3) . . . . ? C00L C00F C00Q C00H 2.9(3) . . . . ? C00T C00F C00Q C00H -174.03(18) . . . . ? C00U C00H C00Q N004 178.73(19) . . . . ? C00Z C00H C00Q N004 -5.3(3) . . . . ? C00U C00H C00Q C00F -2.2(3) . . . . ? C00Z C00H C00Q C00F 173.78(18) . . . . ? C00C C006 C00S C01A 2.2(3) . . . . ? C00C C006 C00S C022 -176.7(2) . . . . ? C006 C00C C00T C00X 2.0(3) . . . . ? C00B C00C C00T C00X -170.4(2) . . . . ? C006 C00C C00T C00F 175.32(19) . . . . ? C00B C00C C00T C00F 2.9(3) . . . . ? C00L C00F C00T C00X 71.3(3) . . . . ? C00Q C00F C00T C00X -111.7(2) . . . . ? C00L C00F C00T C00C -102.0(2) . . . . ? C00Q C00F C00T C00C 75.0(3) . . . . ? C00Q C00H C00U C013 0.0(3) . . . . ? C00Z C00H C00U C013 -175.9(2) . . . . ? C00C C00T C00X C01A 1.2(3) . . . . ? C00F C00T C00X C01A -172.06(19) . . . . ? C00C C00T C00X C018 179.10(19) . . . . ? C00F C00T C00X C018 5.8(3) . . . . ? C011 C00G C00Y C017 0.9(3) . . . . ? C011 C00G C00Y C01W 179.98(19) . . . . ? C01Y C00K C00Z C01D -1.4(3) . . . . ? C009 C00K C00Z C01D 175.14(19) . . . . ? C01Y C00K C00Z C00H 176.90(18) . . . . ? C009 C00K C00Z C00H -6.6(3) . . . . ? C00U C00H C00Z C00K 83.8(2) . . . . ? C00Q C00H C00Z C00K -92.2(2) . . . . ? C00U C00H C00Z C01D -98.0(2) . . . . ? C00Q C00H C00Z C01D 86.0(2) . . . . ? C00Y C00G C011 C019 -0.1(3) . . . . ? C00Y C00G C011 C00D 178.20(19) . . . . ? C01K C00D C011 C019 -129.1(2) . . . . ? C01H C00D C011 C019 106.8(2) . . . . ? C01K C00D C011 C00G 52.6(3) . . . . ? C01H C00D C011 C00G -71.4(3) . . . . ? C00F C00L C013 C00U -0.7(3) . . . . ? C00H C00U C013 C00L 1.4(3) . . . . ? C00O C008 C014 C01R -0.2(3) . . . . ? C00A C008 C014 C01R -172.2(2) . . . . ? C00O C00E C015 C01R 0.0(3) . . . . ? C017 C00E C015 C01R 178.3(2) . . . . ? C005 C007 C016 C00J -0.2(3) . . . . ? Y001 C007 C016 C00J -62.59(18) . . . . ? C005 C007 C016 C00N -179.6(2) . . . . ? Y001 C007 C016 C00N 118.0(2) . . . . ? C005 C007 C016 Y001 62.37(19) . . . . ? C01B C00J C016 C007 -1.0(3) . . . . ? Y001 C00J C016 C007 61.33(18) . . . . ? C01B C00J C016 C00N 178.4(2) . . . . ? Y001 C00J C016 C00N -119.3(2) . . . . ? C01B C00J C016 Y001 -62.34(19) . . . . ? C01Z C00N C016 C007 -101.5(3) . . . . ? C01O C00N C016 C007 133.0(2) . . . . ? C01Z C00N C016 C00J 79.1(3) . . . . ? C01O C00N C016 C00J -46.4(3) . . . . ? C01Z C00N C016 Y001 -12.9(3) . . . . ? C01O C00N C016 Y001 -138.45(19) . . . . ? C00G C00Y C017 C01F -1.3(3) . . . . ? C01W C00Y C017 C01F 179.68(18) . . . . ? C00G C00Y C017 C00E 178.88(18) . . . . ? C01W C00Y C017 C00E -0.2(3) . . . . ? C015 C00E C017 C00Y 71.2(3) . . . . ? C00O C00E C017 C00Y -110.4(2) . . . . ? C015 C00E C017 C01F -108.6(2) . . . . ? C00O C00E C017 C01F 69.7(3) . . . . ? C01A C00X C018 C01N -47.8(3) . . . . ? C00T C00X C018 C01N 134.3(2) . . . . ? C01A C00X C018 C01E 74.6(3) . . . . ? C00T C00X C018 C01E -103.3(2) . . . . ? C00G C011 C019 C01F -0.3(3) . . . . ? C00D C011 C019 C01F -178.62(19) . . . . ? C006 C00S C01A C00X 1.2(3) . . . . ? C022 C00S C01A C00X -179.9(2) . . . . ? C00T C00X C01A C00S -2.9(3) . . . . ? C018 C00X C01A C00S 179.1(2) . . . . ? C016 C00J C01B C00A 2.7(3) . . . . ? Y001 C00J C01B C00A -61.01(17) . . . . ? C016 C00J C01B C01M -171.9(2) . . . . ? Y001 C00J C01B C01M 124.42(19) . . . . ? C016 C00J C01B Y001 63.70(19) . . . . ? C005 C00A C01B C00J -3.2(3) . . . . ? C008 C00A C01B C00J 171.07(19) . . . . ? Y001 C00A C01B C00J 64.15(18) . . . . ? C005 C00A C01B C01M 171.36(19) . . . . ? C008 C00A C01B C01M -14.4(3) . . . . ? Y001 C00A C01B C01M -121.32(19) . . . . ? C005 C00A C01B Y001 -67.32(17) . . . . ? C008 C00A C01B Y001 106.92(17) . . . . ? C007 C005 C01C C01V 137.5(2) . . . . ? C00A C005 C01C C01V -47.4(3) . . . . ? Y001 C005 C01C C01V 45.1(2) . . . . ? C007 C005 C01C C01J -96.3(2) . . . . ? C00A C005 C01C C01J 78.8(3) . . . . ? Y001 C005 C01C C01J 171.34(15) . . . . ? C01L C010 C01D C00Z -0.9(3) . . . . ? C01L C010 C01D C00I 176.32(19) . . . . ? C00K C00Z C01D C010 2.0(3) . . . . ? C00H C00Z C01D C010 -176.21(18) . . . . ? C00K C00Z C01D C00I -175.21(18) . . . . ? C00H C00Z C01D C00I 6.6(3) . . . . ? C00M C00I C01D C010 29.5(3) . . . . ? C00R C00I C01D C010 -93.4(2) . . . . ? C00M C00I C01D C00Z -153.33(19) . . . . ? C00R C00I C01D C00Z 83.8(2) . . . . ? C011 C019 C01F C017 -0.1(3) . . . . ? C011 C019 C01F C00W 176.31(19) . . . . ? C00Y C017 C01F C019 0.9(3) . . . . ? C00E C017 C01F C019 -179.27(18) . . . . ? C00Y C017 C01F C00W -175.40(19) . . . . ? C00E C017 C01F C00W 4.4(3) . . . . ? C01S C00W C01F C019 47.1(3) . . . . ? C01I C00W C01F C019 -77.4(3) . . . . ? C01S C00W C01F C017 -136.6(2) . . . . ? C01I C00W C01F C017 98.9(2) . . . . ? C01D C010 C01L C01Y -0.9(3) . . . . ? C01D C010 C01L C012 -179.24(19) . . . . ? C01G C012 C01L C01Y 161.8(2) . . . . ? C01Q C012 C01L C01Y -72.1(2) . . . . ? C01G C012 C01L C010 -19.9(3) . . . . ? C01Q C012 C01L C010 106.2(2) . . . . ? C00J C01B C01M C01P -47.7(3) . . . . ? C00A C01B C01M C01P 137.8(2) . . . . ? Y001 C01B C01M C01P 49.0(2) . . . . ? C00J C01B C01M C01U 76.4(3) . . . . ? C00A C01B C01M C01U -98.1(2) . . . . ? Y001 C01B C01M C01U 173.07(15) . . . . ? C00E C015 C01R C014 -0.5(3) . . . . ? C008 C014 C01R C015 0.7(3) . . . . ? C00G C00Y C01W C020 -76.1(3) . . . . ? C017 C00Y C01W C020 102.9(3) . . . . ? C00G C00Y C01W C01T 47.6(3) . . . . ? C017 C00Y C01W C01T -133.3(2) . . . . ? C00Z C00K C01Y C01L -0.5(3) . . . . ? C009 C00K C01Y C01L -177.0(2) . . . . ? C010 C01L C01Y C00K 1.6(3) . . . . ? C012 C01L C01Y C00K -179.98(19) . . . . ? C01A C00S C022 C025 -113.7(3) . . . . ? C006 C00S C022 C025 65.3(3) . . . . ? C01A C00S C022 C01X 9.6(4) . . . . ? C006 C00S C022 C01X -171.5(2) . . . . ? _refine_diff_density_max 0.614 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.055 _shelxl_version_number 2013-3 _shelx_res_file ; TITL rj4_74_fast_a.res in P2(1)/n REM Old TITL RJ4_74_FAST in P21/n #14 REM SHELXT solution in P2(1)/n: R1 0.101, Rweak 0.007, Alpha 0.037 REM 0.482 for 164 systematic absences, Orientation as input REM Formula found by SHELXT: C72 N2 Y N26 CELL 1.54184 13.821617 28.680894 17.115035 90 106.3655 90 ZERR 4 0.000152 0.000338 0.000243 0 0.0013 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N Y UNIT 292 400 12 4 L.S. 20 PLAN 10 TEMP -173.15(10) CONF BOND list 4 MORE -1 BOND $H fmap 2 ACTA REM REM REM WGHT 0.035700 5.983000 FVAR 0.42378 Y001 4 0.783204 0.402077 0.856842 11.00000 0.01581 0.02155 = 0.01984 -0.00284 0.00814 -0.00151 N26 3 0.836913 0.479537 0.884572 11.00000 0.01082 0.01550 = 0.01656 0.00148 0.00626 0.00164 N003 3 0.831706 0.379499 0.749628 11.00000 0.01987 0.02367 = 0.01856 -0.00037 0.00729 0.00334 N004 3 0.633717 0.373179 0.855570 11.00000 0.01603 0.01947 = 0.02551 0.00352 0.00747 0.00007 C005 1 0.860504 0.313422 0.914685 11.00000 0.01962 0.02370 = 0.01948 0.00131 0.00611 0.00202 C006 1 0.639707 0.491910 0.686984 11.00000 0.02641 0.03098 = 0.02464 0.00460 0.01346 0.00073 AFIX 43 H006 2 0.662343 0.487465 0.640002 11.00000 -1.20000 AFIX 0 C007 1 0.839286 0.332737 0.983322 11.00000 0.02096 0.02871 = 0.02085 0.00173 0.00806 -0.00061 AFIX 43 H007 2 0.788380 0.318649 1.002847 11.00000 -1.20000 AFIX 0 C008 1 0.956293 0.321472 0.807928 11.00000 0.01810 0.02364 = 0.01877 -0.00284 0.00694 -0.00244 C009 1 0.438859 0.275699 0.729834 11.00000 0.02855 0.03175 = 0.02319 0.00001 0.00381 -0.00204 AFIX 13 H009 2 0.427491 0.310089 0.723362 11.00000 -1.20000 AFIX 0 C00A 1 0.936037 0.334804 0.886022 11.00000 0.01732 0.02375 = 0.01844 -0.00078 0.00466 0.00400 C00B 1 0.546654 0.415137 0.653752 11.00000 0.03877 0.02842 = 0.02220 -0.00197 0.01112 -0.00405 AFIX 13 H00B 2 0.555854 0.386155 0.687537 11.00000 -1.20000 AFIX 0 C00C 1 0.585393 0.456140 0.710594 11.00000 0.02268 0.02345 = 0.02230 0.00080 0.00821 0.00095 C00D 1 0.729114 0.451485 0.379020 11.00000 0.03086 0.03028 = 0.02504 0.00534 0.00909 0.00318 AFIX 13 H00D 2 0.744323 0.485061 0.392932 11.00000 -1.20000 AFIX 0 C00E 1 0.927726 0.341052 0.665455 11.00000 0.02040 0.02018 = 0.01912 -0.00252 0.00780 -0.00157 C00F 1 0.492213 0.426109 0.807817 11.00000 0.01726 0.02241 = 0.01723 0.00130 0.00634 0.00035 C00G 1 0.760568 0.375262 0.456685 11.00000 0.02309 0.02933 = 0.01945 -0.00277 0.00641 0.00058 AFIX 43 H00G 2 0.713727 0.361077 0.411405 11.00000 -1.20000 AFIX 0 C00H 1 0.462816 0.348687 0.853519 11.00000 0.01799 0.02326 = 0.02137 0.00360 0.00656 -0.00079 C00I 1 0.544177 0.325856 1.027123 11.00000 0.02472 0.01960 = 0.02384 0.00328 0.00701 -0.00164 AFIX 13 H00I 2 0.550181 0.357349 1.003853 11.00000 -1.20000 AFIX 0 C00J 1 0.964691 0.392192 0.995337 11.00000 0.01972 0.02609 = 0.01983 -0.00439 0.00479 -0.00330 AFIX 43 H00J 2 0.998896 0.419041 1.021940 11.00000 -1.20000 AFIX 0 C00K 1 0.493596 0.266154 0.819137 11.00000 0.01873 0.02692 = 0.02292 0.00236 0.00708 -0.00472 C00L 1 0.389352 0.435571 0.794469 11.00000 0.02175 0.02296 = 0.02616 0.00377 0.00847 0.00382 AFIX 43 H00L 2 0.364099 0.465342 0.774262 11.00000 -1.20000 AFIX 0 C00M 1 0.630011 0.320668 1.104945 11.00000 0.02834 0.03392 = 0.02409 0.00111 0.00769 -0.00242 AFIX 137 H00A 2 0.631896 0.348028 1.139643 11.00000 -1.50000 H00C 2 0.694083 0.318076 1.091328 11.00000 -1.50000 H00E 2 0.619361 0.292557 1.134008 11.00000 -1.50000 AFIX 0 C00N 1 0.863350 0.390726 1.098558 11.00000 0.02922 0.03633 = 0.02339 -0.00662 0.01509 -0.00815 AFIX 13 H00N 2 0.823539 0.366271 1.117479 11.00000 -1.20000 AFIX 0 C00O 1 0.902861 0.347787 0.739561 11.00000 0.01751 0.01991 = 0.02082 -0.00201 0.00662 -0.00229 C00P 1 0.600119 0.408048 0.587759 11.00000 0.02904 0.05608 = 0.02694 -0.01074 0.00456 0.00839 AFIX 137 H00F 2 0.584001 0.434028 0.549058 11.00000 -1.50000 H00H 2 0.577507 0.378729 0.558998 11.00000 -1.50000 H00K 2 0.673150 0.406840 0.612883 11.00000 -1.50000 AFIX 0 C00Q 1 0.531272 0.382530 0.839641 11.00000 0.01729 0.02180 = 0.01653 0.00189 0.00576 0.00001 C00R 1 0.443836 0.324228 1.048609 11.00000 0.02793 0.03279 = 0.03405 -0.00550 0.01070 0.00228 AFIX 137 H00M 2 0.434323 0.293096 1.068862 11.00000 -1.50000 H00O 2 0.388409 0.331099 0.999919 11.00000 -1.50000 H00P 2 0.444605 0.347449 1.090785 11.00000 -1.50000 AFIX 0 C00S 1 0.662159 0.533890 0.729415 11.00000 0.02236 0.02439 = 0.03125 0.00615 0.00925 0.00006 C00T 1 0.557224 0.462009 0.783875 11.00000 0.01711 0.02288 = 0.01977 0.00551 0.00626 0.00176 C00U 1 0.360985 0.359215 0.838606 11.00000 0.01753 0.02611 = 0.02831 0.00537 0.00861 -0.00226 AFIX 43 H00U 2 0.316209 0.336219 0.848223 11.00000 -1.20000 AFIX 0 C00V 1 0.435051 0.420462 0.611212 11.00000 0.03288 0.10566 = 0.03904 -0.03548 0.01531 -0.02155 AFIX 137 H00Q 2 0.397874 0.423426 0.651988 11.00000 -1.50000 H00R 2 0.410964 0.392988 0.577259 11.00000 -1.50000 H00S 2 0.424197 0.448413 0.576898 11.00000 -1.50000 AFIX 0 C00W 1 0.976074 0.441093 0.658083 11.00000 0.02943 0.02407 = 0.02351 -0.00071 0.00760 -0.00358 AFIX 13 H00W 2 0.989758 0.420332 0.706924 11.00000 -1.20000 AFIX 0 C00X 1 0.581609 0.503527 0.828284 11.00000 0.01807 0.02140 = 0.02191 0.00314 0.00536 0.00274 C00Y 1 0.808037 0.347732 0.523853 11.00000 0.02140 0.02638 = 0.02080 -0.00187 0.00955 0.00060 C00Z 1 0.500375 0.300470 0.879160 11.00000 0.01517 0.02204 = 0.02456 0.00393 0.00715 -0.00314 C010 1 0.583768 0.245177 0.982443 11.00000 0.02071 0.02503 = 0.02200 0.00535 0.00790 0.00101 AFIX 43 H010 2 0.614368 0.238030 1.038143 11.00000 -1.20000 AFIX 0 C011 1 0.779593 0.422734 0.453895 11.00000 0.02501 0.02924 = 0.02344 0.00353 0.01220 0.00346 C012 1 0.620349 0.161689 0.943791 11.00000 0.02857 0.02610 = 0.03409 0.00301 0.01673 0.00539 AFIX 13 H012 2 0.655714 0.153267 0.902202 11.00000 -1.20000 AFIX 0 C013 1 0.323686 0.402934 0.809802 11.00000 0.01591 0.03218 = 0.03136 0.00465 0.00898 0.00210 AFIX 43 H013 2 0.254336 0.410157 0.800877 11.00000 -1.20000 AFIX 0 C014 1 1.030403 0.289770 0.803696 11.00000 0.02323 0.02465 = 0.02225 -0.00068 0.00539 0.00201 AFIX 43 H014 2 1.065259 0.272646 0.850718 11.00000 -1.20000 AFIX 0 C015 1 1.002420 0.308859 0.663049 11.00000 0.02564 0.02670 = 0.02166 -0.00388 0.01047 0.00189 AFIX 43 H015 2 1.018862 0.304414 0.613281 11.00000 -1.20000 AFIX 0 C016 1 0.889353 0.371572 1.024118 11.00000 0.02076 0.03018 = 0.01760 0.00025 0.00602 0.00126 C017 1 0.876452 0.369015 0.591449 11.00000 0.02001 0.02326 = 0.01960 -0.00111 0.00998 0.00129 C018 1 0.552213 0.512238 0.906621 11.00000 0.02479 0.02461 = 0.02344 -0.00170 0.00923 -0.00051 AFIX 13 H018 2 0.532286 0.481740 0.925826 11.00000 -1.20000 AFIX 0 C019 1 0.847849 0.442849 0.520358 11.00000 0.02528 0.02350 = 0.02419 0.00139 0.01116 0.00003 AFIX 43 H019 2 0.861710 0.475236 0.519032 11.00000 -1.20000 AFIX 0 C01A 1 0.631713 0.539086 0.799204 11.00000 0.02336 0.02190 = 0.02862 0.00215 0.00792 0.00092 AFIX 43 H01A 2 0.645178 0.567652 0.828354 11.00000 -1.20000 AFIX 0 C01B 1 0.990334 0.373820 0.927942 11.00000 0.01655 0.02813 = 0.01938 0.00038 0.00478 0.00143 C01C 1 0.805549 0.268399 0.880334 11.00000 0.02736 0.02280 = 0.02750 -0.00064 0.01114 -0.00506 AFIX 13 H01C 2 0.746137 0.266007 0.902570 11.00000 -1.20000 AFIX 0 C01D 1 0.544502 0.289622 0.961801 11.00000 0.01765 0.02176 = 0.02362 0.00220 0.00735 -0.00340 C01E 1 0.461269 0.545410 0.890848 11.00000 0.03225 0.04220 = 0.03318 -0.00403 0.01174 0.00826 AFIX 137 H01B 2 0.476286 0.574146 0.865555 11.00000 -1.50000 H01D 2 0.447585 0.552909 0.942582 11.00000 -1.50000 H01E 2 0.402004 0.530304 0.854359 11.00000 -1.50000 AFIX 0 C01F 1 0.897070 0.417104 0.589368 11.00000 0.02270 0.02228 = 0.02149 -0.00141 0.01070 0.00014 C01G 1 0.697012 0.156386 1.026820 11.00000 0.03032 0.03048 = 0.04244 0.00917 0.01197 0.00964 AFIX 137 H01F 2 0.751778 0.178892 1.031839 11.00000 -1.50000 H01G 2 0.724564 0.124683 1.032436 11.00000 -1.50000 H01H 2 0.664053 0.162168 1.069645 11.00000 -1.50000 AFIX 0 C01H 1 0.773402 0.439082 0.309172 11.00000 0.03922 0.04446 = 0.02618 0.00877 0.01127 0.00568 AFIX 137 H01I 2 0.846671 0.443478 0.326948 11.00000 -1.50000 H01J 2 0.743873 0.459353 0.262439 11.00000 -1.50000 H01K 2 0.758019 0.406472 0.293409 11.00000 -1.50000 AFIX 0 C01I 1 1.074679 0.446350 0.635066 11.00000 0.02883 0.04638 = 0.03724 -0.00953 0.00892 -0.00956 AFIX 137 H01L 2 1.098749 0.415521 0.624366 11.00000 -1.50000 H01M 2 1.125405 0.461204 0.679988 11.00000 -1.50000 H01N 2 1.063081 0.465696 0.586092 11.00000 -1.50000 AFIX 0 C01J 1 0.873358 0.226685 0.914137 11.00000 0.04408 0.02885 = 0.03986 0.00329 0.00548 -0.00197 AFIX 137 H01O 2 0.931869 0.226976 0.892481 11.00000 -1.50000 H01P 2 0.835365 0.197730 0.897901 11.00000 -1.50000 H01Q 2 0.896293 0.228619 0.973692 11.00000 -1.50000 AFIX 0 C01K 1 0.615167 0.445626 0.353400 11.00000 0.03199 0.04999 = 0.04040 0.01740 0.00940 0.00665 AFIX 137 H01R 2 0.598071 0.413403 0.335823 11.00000 -1.50000 H01S 2 0.585093 0.466903 0.308289 11.00000 -1.50000 H01T 2 0.588893 0.452796 0.399573 11.00000 -1.50000 AFIX 0 C01L 1 0.579637 0.210751 0.923918 11.00000 0.02157 0.02340 = 0.03034 0.00296 0.01270 -0.00136 C01M 1 1.081216 0.392748 0.904894 11.00000 0.01803 0.03209 = 0.02443 -0.00665 0.00927 -0.00349 AFIX 13 H01U 2 1.078423 0.380466 0.849619 11.00000 -1.20000 AFIX 0 C01N 1 0.638922 0.532254 0.974052 11.00000 0.02937 0.03819 = 0.02798 -0.00425 0.00875 -0.00225 AFIX 137 H01V 2 0.699216 0.513018 0.980234 11.00000 -1.50000 H01W 2 0.620538 0.532427 1.025328 11.00000 -1.50000 H01X 2 0.652821 0.564202 0.959996 11.00000 -1.50000 AFIX 0 C01O 1 0.957554 0.400508 1.168667 11.00000 0.04435 0.06250 = 0.02671 -0.00984 0.01413 -0.00840 AFIX 137 H01Y 2 0.999550 0.372420 1.180275 11.00000 -1.50000 H 2 0.937663 0.409387 1.217242 11.00000 -1.50000 HA 2 0.995885 0.425994 1.153462 11.00000 -1.50000 AFIX 0 C01P 1 1.087408 0.445473 0.901771 11.00000 0.02429 0.03386 = 0.03104 -0.00169 0.01342 -0.00435 AFIX 137 H01Z 2 1.026553 0.457649 0.862648 11.00000 -1.50000 HB 2 1.146841 0.454468 0.884787 11.00000 -1.50000 HC 2 1.092833 0.458376 0.955858 11.00000 -1.50000 AFIX 0 C01Q 1 0.533480 0.126930 0.933904 11.00000 0.04107 0.02338 = 0.04069 0.00118 0.01399 -0.00271 AFIX 137 H01 2 0.560428 0.095119 0.941026 11.00000 -1.50000 HD 2 0.486385 0.130149 0.879393 11.00000 -1.50000 HE 2 0.498090 0.133299 0.974970 11.00000 -1.50000 AFIX 0 C01R 1 1.053619 0.283080 0.730650 11.00000 0.02542 0.02613 = 0.02726 -0.00440 0.01000 0.00677 AFIX 43 H1 2 1.103770 0.261194 0.727032 11.00000 -1.20000 AFIX 0 C01S 1 0.940911 0.488086 0.681924 11.00000 0.04561 0.02887 = 0.03163 -0.00652 0.00813 -0.00029 AFIX 137 H2 2 0.930309 0.509781 0.636043 11.00000 -1.50000 HF 2 0.992318 0.500698 0.728911 11.00000 -1.50000 HG 2 0.877535 0.483944 0.696120 11.00000 -1.50000 AFIX 0 C01T 1 0.785893 0.272980 0.441739 11.00000 0.03807 0.02673 = 0.03356 -0.00948 0.00944 -0.00035 AFIX 137 H3 2 0.734487 0.287088 0.396379 11.00000 -1.50000 HH 2 0.772596 0.239516 0.443986 11.00000 -1.50000 HI 2 0.852658 0.277632 0.433658 11.00000 -1.50000 AFIX 0 C01U 1 1.175000 0.372104 0.965663 11.00000 0.01995 0.03754 = 0.04274 0.00207 0.01018 0.00181 AFIX 137 H4 2 1.179310 0.383448 1.020552 11.00000 -1.50000 HJ 2 1.235409 0.381667 0.950584 11.00000 -1.50000 HK 2 1.170199 0.338007 0.964676 11.00000 -1.50000 AFIX 0 C01V 1 0.764603 0.264442 0.788168 11.00000 0.03197 0.03172 = 0.03056 -0.00434 0.00527 -0.00983 AFIX 137 H5 2 0.729343 0.293302 0.766242 11.00000 -1.50000 HL 2 0.717560 0.238153 0.774453 11.00000 -1.50000 HM 2 0.820552 0.259326 0.764488 11.00000 -1.50000 AFIX 0 C01W 1 0.782669 0.295964 0.521762 11.00000 0.02976 0.02411 = 0.02503 -0.00253 0.00609 0.00016 AFIX 13 H6 2 0.834675 0.280454 0.566979 11.00000 -1.20000 AFIX 0 C01X 1 0.750432 0.613094 0.754890 11.00000 0.05171 0.03833 = 0.04779 0.00611 0.01333 -0.01755 AFIX 137 H7 2 0.691033 0.628800 0.762997 11.00000 -1.50000 HN 2 0.788916 0.635132 0.731622 11.00000 -1.50000 HO 2 0.792930 0.601706 0.807340 11.00000 -1.50000 AFIX 0 C01Y 1 0.532984 0.222083 0.842847 11.00000 0.02487 0.02256 = 0.02677 -0.00301 0.01032 -0.00533 AFIX 43 H8 2 0.527905 0.198859 0.802309 11.00000 -1.20000 AFIX 0 C01Z 1 0.797173 0.433030 1.075875 11.00000 0.06058 0.06330 = 0.04114 -0.00455 0.02904 0.01731 AFIX 137 H9 2 0.833243 0.457347 1.055151 11.00000 -1.50000 HP 2 0.779714 0.444646 1.124025 11.00000 -1.50000 HQ 2 0.735418 0.424679 1.033662 11.00000 -1.50000 AFIX 0 C020 1 0.679683 0.287948 0.536467 11.00000 0.05410 0.03008 = 0.07491 -0.00804 0.04180 -0.01174 AFIX 137 H02A 2 0.679990 0.300958 0.589483 11.00000 -1.50000 H02B 2 0.665846 0.254417 0.535863 11.00000 -1.50000 H02C 2 0.627296 0.303337 0.493468 11.00000 -1.50000 AFIX 0 C021 1 0.336982 0.252244 0.708175 11.00000 0.03811 0.08957 = 0.05010 0.01982 -0.01412 -0.01995 AFIX 137 H02D 2 0.345962 0.218467 0.715350 11.00000 -1.50000 H02E 2 0.300886 0.259083 0.651330 11.00000 -1.50000 H02F 2 0.297957 0.263954 0.743783 11.00000 -1.50000 AFIX 0 C022 1 0.716963 0.572221 0.697064 11.00000 0.03626 0.03140 = 0.04205 0.00545 0.02048 -0.00604 AFIX 13 H022 2 0.778609 0.558137 0.687107 11.00000 -1.20000 AFIX 0 C023 1 0.497302 0.260599 0.671571 11.00000 0.04938 0.14081 = 0.02162 0.01093 0.00876 0.02497 AFIX 137 H02G 2 0.561545 0.277441 0.684136 11.00000 -1.50000 H02H 2 0.457915 0.267572 0.615591 11.00000 -1.50000 H02I 2 0.510308 0.227003 0.677242 11.00000 -1.50000 AFIX 0 C025 1 0.650666 0.589785 0.616356 11.00000 0.08208 0.05759 = 0.04365 0.01724 0.00981 -0.03471 AFIX 137 H02J 2 0.627712 0.563360 0.579488 11.00000 -1.50000 H02K 2 0.689192 0.611368 0.592269 11.00000 -1.50000 H02L 2 0.592141 0.606006 0.625024 11.00000 -1.50000 AFIX 0 C5 1 0.871005 0.512145 0.893550 11.00000 0.03472 0.06605 = 0.03124 0.00348 0.01183 0.01342 H003 2 0.804946 0.394379 0.701799 11.00000 0.03885 H004 2 0.645189 0.344007 0.873817 11.00000 0.03236 HKLF 4 REM rj4_74_fast_a.res in P2(1)/n REM R1 = 0.0411 for 11192 Fo > 4sig(Fo) and 0.0508 for all 12920 data REM 726 parameters refined using 0 restraints END WGHT 0.0356 5.9899 REM Highest difference peak 0.614, deepest hole -0.551, 1-sigma level 0.055 Q1 1 0.8253 0.4581 0.8833 11.00000 0.05 0.61 Q2 1 0.8359 0.4842 0.8660 11.00000 0.05 0.51 Q3 1 0.7838 0.4385 0.8618 11.00000 0.05 0.48 Q4 1 0.9036 0.3678 1.1662 11.00000 0.05 0.45 Q5 1 0.7956 0.5901 0.7393 11.00000 0.05 0.43 Q6 1 0.8784 0.4485 1.1069 11.00000 0.05 0.39 Q7 1 0.5603 0.5074 0.8624 11.00000 0.05 0.33 Q8 1 0.7777 0.3654 0.8557 11.00000 0.05 0.32 Q9 1 0.5174 0.2904 0.6778 11.00000 0.05 0.30 Q10 1 0.3714 0.2340 0.6827 11.00000 0.05 0.28 ; _shelx_res_checksum 57523 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_cem _database_code_depnum_ccdc_archive 'CCDC 2207617' loop_ _audit_author_name _audit_author_address 'Richard Staples' ;Michigan State University United States of America ; _audit_update_record ; 2022-09-15 deposited with the CCDC. 2023-03-21 downloaded from the CCDC. ; _audit_creation_date 2022-07-15 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _shelxl_version_number 2013-3 _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C72 H100 Cl N2 Y, 0.75(C6 H14), 0.25(C6 H12), C6 H11.5' _chemical_formula_sum 'C84 H125 Cl N2 Y' _chemical_formula_weight 1287.21 _chemical_melting_point ? _chemical_oxdiff_formula C36H51N2 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' Cl Cl 0.3639 0.7018 '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' Y Y -0.2670 2.0244 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 39.6030(5) _cell_length_b 16.4949(2) _cell_length_c 25.0473(3) _cell_angle_alpha 90 _cell_angle_beta 91.0170(10) _cell_angle_gamma 90 _cell_volume 16359.5(3) _cell_formula_units_Z 8 _cell_measurement_reflns_used 24642 _cell_measurement_temperature 99.99(10) _cell_measurement_theta_max 76.1960 _cell_measurement_theta_min 2.8660 _shelx_estimated_absorpt_T_max 0.856 _shelx_estimated_absorpt_T_min 0.746 _exptl_absorpt_coefficient_mu 1.590 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.599 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.98a (Rigaku Oxford Diffraction, 2021) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.045 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 5592 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -11 7 7 0.0621 8 8 13 0.0882 16 -3 0 0.0458 6 -9 -11 0.0449 -12 7 5 0.0646 16 -2 1 0.0454 10 -8 -8 0.0442 3 10 4 0.0917 0 5 22 0.0821 -3 -7 19 0.0523 -2 -10 -8 0.0367 2 0 -26 0.0373 3 7 -19 0.0486 -1 3 24 0.0737 _exptl_crystal_size_max 0.196 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.101 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -11.3655 7.2085 6.5088 -0.1830 -0.7655 0.6168 7.9917 7.6209 12.6283 0.0933 0.3833 0.9189 15.5152 -3.1885 0.1337 0.2313 0.9637 -0.1330 5.5887 -9.0483 -10.6626 0.1053 0.4437 -0.8900 -12.4371 6.5749 5.3419 -0.1966 -0.8216 0.5350 15.7900 -2.4504 1.2134 0.2332 0.9711 -0.0507 10.1897 -7.7657 -7.6020 0.1677 0.7022 -0.6919 2.7436 10.4114 3.9831 -0.3531 0.0836 0.9318 0.2372 5.4287 22.1362 0.4778 -0.1159 0.8708 -3.1469 -7.1109 18.6774 0.9473 -0.2273 -0.2258 -2.3692 -9.9976 -8.2854 0.1919 -0.0449 -0.9804 1.5016 -0.0848 -25.6483 -0.8424 0.2030 -0.4991 3.1545 7.1009 -18.6964 -0.9474 0.2279 0.2247 -0.5197 3.2712 24.4767 0.6554 -0.1584 0.7385 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0751 _diffrn_reflns_av_unetI/netI 0.0692 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.918 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 59902 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.918 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 77.287 _diffrn_reflns_theta_min 2.902 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 99.99(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.918 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 95.00 174.00 0.50 0.57 -- 106.58 41.00 84.00 158 2 \w 129.00 173.00 0.50 0.57 -- 106.58 61.00 150.00 88 3 \w 76.00 101.00 0.50 0.14 -- 47.61 41.00 84.00 50 4 \w -27.00 25.00 0.50 0.14 -- 47.61 -19.00 60.00 104 5 \w -6.00 25.00 0.50 0.14 -- 47.61 -41.00 -68.00 62 6 \w -19.00 24.00 0.50 0.14 -- 47.61 -19.00-180.00 86 7 \w 34.00 70.00 0.50 0.57 -- 106.58 -61.00-150.00 72 8 \w 38.00 69.00 0.50 0.57 -- 106.58 -61.00-180.00 62 9 \w 40.00 65.00 0.50 0.57 -- 106.58 -61.00 -90.00 50 10 \w 35.00 69.00 0.50 0.57 -- 106.58 -61.00 -60.00 68 11 \w 34.00 70.00 0.50 0.57 -- 106.58 -61.00 150.00 72 12 \w -70.00 -19.00 0.50 0.57 -- -91.75 61.00-180.00 102 13 \w -48.00 -21.00 0.50 0.57 -- -91.75 45.00-180.00 54 14 \w -47.00 -21.00 0.50 0.57 -- -91.75 45.00 -90.00 52 15 \w -52.00 -23.00 0.50 0.57 -- -91.75 45.00 0.00 58 16 \w -47.00 14.00 0.50 0.14 -- -47.61 41.00 84.00 122 17 \w -70.00 -19.00 0.50 0.57 -- -91.75 61.00 120.00 102 18 \w -47.00 -22.00 0.50 0.57 -- -91.75 41.00 84.00 50 19 \w -49.00 -24.00 0.50 0.57 -- -91.75 45.00 60.00 50 20 \w -119.00 -52.00 0.50 0.14 -- -47.61 -41.00 -68.00 134 21 \w -159.00-133.00 0.50 0.57 -- -91.75 -61.00-150.00 52 22 \w -155.00-130.00 0.50 0.57 -- -91.75 -45.00-120.00 50 23 \w -163.00-126.00 0.50 0.57 -- -91.75 -77.00 60.00 74 24 \w -82.00 -57.00 0.50 0.57 -- -91.75 125.00-180.00 50 25 \w -78.00 -34.00 0.50 0.14 -- -47.61 125.00-150.00 88 26 \w -128.00-102.00 0.50 0.57 -- -91.75 -41.00 -68.00 52 27 \w -150.00-122.00 0.50 0.57 -- -91.75 -94.00 0.00 56 28 \w -159.00-131.00 0.50 0.57 -- -91.75 -94.00-120.00 56 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0047761000 _diffrn_orient_matrix_UB_12 -0.0479108000 _diffrn_orient_matrix_UB_13 0.0332825000 _diffrn_orient_matrix_UB_21 0.0608499000 _diffrn_orient_matrix_UB_22 -0.0063442000 _diffrn_orient_matrix_UB_23 -0.0043309000 _diffrn_orient_matrix_UB_31 0.0076908000 _diffrn_orient_matrix_UB_32 0.0799573000 _diffrn_orient_matrix_UB_33 0.0196471000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 12491 _reflns_number_total 15940 _reflns_odcompleteness_completeness 91.15 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 77.83 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.41.98a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.41.98a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.98a (Rigaku OD, 2021)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2013/3 (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve 1.3 (Bourhis et al., 2015)' _refine_diff_density_max 0.802 _refine_diff_density_min -0.747 _refine_diff_density_rms 0.077 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 1044 _refine_ls_number_reflns 15940 _refine_ls_number_restraints 287 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0598 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0862P)^2^+26.7012P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1564 _refine_ls_wR_factor_ref 0.1727 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, {H15A,H15B} of C15, {H14A,H14B} of C14, {H16A,H16B} of C16, {H37A,H37B} of C37, {H38A,H38B} of C38, {H29A,H29B} of C29, {H43A,H43B} of C43, {H42A,H42B} of C42, {H20A,H20B} of C20, {H33A,H33B} of C33, {H34A,H34B} of C34, {H17A,H17B} of C17, {H35A,H35B} of C35, {H52A,H52B} of C52, {H53A, H53B} of C53, {H28A,H28B} of C28, All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups, {H1BA,H1BB} of C1B 2. Restrained distances C13-C14 = C14-C15 = C15-C16 = C16-C17 = C17-C18 1.52 with sigma of 0.02 C14-C16 = C15-C17 2.54 with sigma of 0.04 C13-C15 = C16-C18 2.53 with sigma of 0.04 C27-C29 \\sim C42-C28 \\sim C28-C30 with sigma of 0.04 C42-C27 \\sim C27-C28 \\sim C28-C29 \\sim C29-C30 with sigma of 0.02 C20-C53 \\sim C53-C44 \\sim C52-C43 \\sim C43-C41 with sigma of 0.04 C20-C52 \\sim C52-C53 \\sim C53-C43 \\sim C43-C44 \\sim C44-C41 with sigma of 0.02 C13-C14 \\sim C14-C15 \\sim C15-C16 \\sim C16-C17 \\sim C17-C18 with sigma of 0.02 C13-C15 \\sim C15-C17 \\sim C14-C16 \\sim C16-C18 with sigma of 0.04 3. Uiso/Uaniso restraints and constraints C27 \\sim C28 \\sim C29 \\sim C30 \\sim C42: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004 within 2A C19 \\sim C20 \\sim C43 \\sim C44 \\sim C52 \\sim C53 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C41 \\sim C42: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A C20 \\sim C43 \\sim C44 \\sim C52 \\sim C53 \\sim C41: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.0004 within 2A C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A 4. Rigid body (RIGU) restrains C27, C28, C29, C30, C42 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C20, C43, C44, C52, C53, C41 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C13, C14, C15, C16, C17, C18 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Fixed Sof: C641(0.5) H641(0.5) C642(0.5) H642(0.5) C643(0.5) H64A(0.5) H64B(0.5) H64C(0.5) C644(0.5) H64D(0.5) H64E(0.5) H64F(0.5) C645(0.5) H64G(0.5) H64H(0.5) H64I(0.5) C646(0.5) H64J(0.5) H64K(0.5) H64L(0.5) C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C14(0.5) H14A(0.5) H14B(0.5) C15(0.5) H15A(0.5) H15B(0.5) C16(0.5) H16A(0.5) H16B(0.5) C17(0.5) H17A(0.5) H17B(0.5) C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C19(0.25) H19A(0.25) H19B(0.25) H19C(0.25) C20(0.25) H20A(0.25) H20B(0.25) C52(0.25) H52A(0.25) H52B(0.25) C43(0.25) H43A(0.25) H43B(0.25) C44(0.25) H44A(0.25) H44B(0.25) H44C(0.25) C53(0.25) H53A(0.25) H53B(0.25) C27(0.25) C28(0.25) H28A(0.25) H28B(0.25) C29(0.25) H29A(0.25) H29B(0.25) C30(0.25) H30A(0.25) H30B(0.25) H30C(0.25) C41(0.25) H41A(0.25) H41B(0.25) H41C(0.25) C42(0.25) H42A(0.25) H42B(0.25) H32C(0.5) H32D(0.5) H32A(0.5) H32B(0.5) C33(0.5) H33A(0.5) H33B(0.5) C34(0.5) H34A(0.5) H34B(0.5) C35(0.5) H35A(0.5) H35B(0.5) C36(0.5) C37(0.5) H37A(0.5) H37B(0.5) C38(0.5) H38A(0.5) H38B(0.5) C39(0.5) H39A(0.5) H39B(0.5) H39C(0.5) C40(0.5) 6.a Riding coordinates: C13(H13A,H13B,H13C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C52(H52A,H52B), C44(H44A,H44B,H44C), C29(H29A,H29B), C41(H41A,H41B,H41C) 6.b Free rotating group: C20(C52) 6.c Ternary CH refined with riding coordinates: C46(H46), C51(H51), C126(H126), C221(H221), C241(H241), C261(H261), C621(H621), C641(H641), C642(H642), C661(H661), C821(H821), C841(H841), C861(H861) 6.d Secondary CH2 refined with riding coordinates: C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C20(H20A, H20B), C43(H43A,H43B), C53(H53A,H53B), C28(H28A,H28B), C42(H42A,H42B), C32(H32C,H32D), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C37(H37A,H37B), C38(H38A,H38B) 6.e Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C11(H11), C63(H63), C65(H65), C123(H123), C125(H125) 6.f Idealised Me refined as rotating group: C1A(H1AA,H1AB,H1AC), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C122(H12A,H12B, H12C), C124(H12D,H12E,H12F), C222(H22A,H22B,H22C), C223(H22D,H22E,H22F), C242(H24A,H24B,H24C), C243(H24D,H24E,H24F), C262(H26A,H26B,H26C), C263(H26D, H26E,H26F), C622(H62A,H62B,H62C), C623(H62D,H62E,H62F), C643(H64A,H64B,H64C), C644(H64D,H64E,H64F), C645(H64G,H64H,H64I), C646(H64J,H64K,H64L), C662(H66A, H66B,H66C), C663(H66D,H66E,H66F), C822(H82A,H82B,H82C), C823(H82D,H82E,H82F), C842(H84A,H84B,H84C), C843(H84D,H84E,H84F), C863(H86D,H86E,H86F), C30(H30A, H30B,H30C), C31(H31A,H31B,H31C), C39(H39A,H39B,H39C) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.32719(2) 0.55254(2) 0.44643(2) 0.03275(10) Uani 1 1 d . . . . . H2 H 0.2732(12) 0.567(3) 0.3900(18) 0.064(13) Uiso 1 1 d . . . . . Cl1 Cl 0.30498(2) 0.62051(6) 0.52816(3) 0.0517(2) Uani 1 1 d . . . . . N1 N 0.37612(6) 0.48829(16) 0.46477(10) 0.0343(5) Uani 1 1 d . . . . . H1 H 0.3756(11) 0.447(3) 0.4869(18) 0.056(12) Uiso 1 1 d . . . . . N2 N 0.28142(6) 0.52050(16) 0.39903(10) 0.0338(5) Uani 1 1 d . . . . . C1 C 0.40905(7) 0.50583(18) 0.45101(11) 0.0329(6) Uani 1 1 d . . . . . C1A C 0.20335(10) 0.6088(2) 0.46494(13) 0.0521(9) Uani 1 1 d . . . . . H1AA H 0.1931 0.6612 0.4609 0.078 Uiso 1 1 calc R U . . . H1AB H 0.2274 0.6148 0.4673 0.078 Uiso 1 1 calc R U . . . H1AC H 0.1954 0.5836 0.4969 0.078 Uiso 1 1 calc R U . . . C1B C 0.15641(10) 0.5361(3) 0.41454(17) 0.0535(9) Uani 1 1 d . . . . . H1BA H 0.1477(12) 0.510(3) 0.449(2) 0.080 Uiso 1 1 d . U . . . H1BB H 0.1503(13) 0.502(3) 0.384(2) 0.080 Uiso 1 1 d . U . . . H1BC H 0.1449(11) 0.588(3) 0.4128(16) 0.056(11) Uiso 1 1 d . . . . . C2 C 0.41433(8) 0.57000(19) 0.41450(12) 0.0356(6) Uani 1 1 d . . . . . C3 C 0.44610(8) 0.5888(2) 0.39599(13) 0.0410(7) Uani 1 1 d . . . . . H3 H 0.4487 0.6303 0.3713 0.049 Uiso 1 1 calc R U . . . C4 C 0.47403(8) 0.5461(2) 0.41411(13) 0.0413(7) Uani 1 1 d . . . . . H4 H 0.4954 0.5573 0.4010 0.050 Uiso 1 1 calc R U . . . C5 C 0.46961(8) 0.4864(2) 0.45209(12) 0.0387(7) Uani 1 1 d . . . . . H5 H 0.4890(10) 0.458(2) 0.4677(15) 0.043(9) Uiso 1 1 d . . . . . C6 C 0.43820(7) 0.46596(19) 0.47230(11) 0.0343(6) Uani 1 1 d . . . . . C7 C 0.26300(8) 0.45668(17) 0.37765(11) 0.0322(6) Uani 1 1 d . . . . . C8 C 0.27034(8) 0.37665(18) 0.39441(11) 0.0333(6) Uani 1 1 d . . . . . C9 C 0.25310(8) 0.31183(19) 0.37020(12) 0.0379(7) Uani 1 1 d . . . . . H9 H 0.2582(9) 0.253(2) 0.3816(14) 0.045 Uiso 1 1 d . U . . . C10 C 0.22835(9) 0.3241(2) 0.33144(12) 0.0410(7) Uani 1 1 d . . . . . H10 H 0.2163(10) 0.277(2) 0.3155(15) 0.049 Uiso 1 1 d . U . . . C11 C 0.21949(8) 0.40317(19) 0.31788(11) 0.0379(7) Uani 1 1 d . . . . . H11 H 0.2020 0.4118 0.2933 0.045 Uiso 1 1 calc R U . . . C12 C 0.23609(8) 0.46943(19) 0.34019(11) 0.0342(6) Uani 1 1 d . . . . . C21 C 0.38406(7) 0.61919(18) 0.39981(12) 0.0359(6) Uani 1 1 d . . . . . C22 C 0.37409(8) 0.68337(19) 0.43359(13) 0.0407(7) Uani 1 1 d . . . . . C23 C 0.34288(8) 0.7210(2) 0.42398(15) 0.0438(7) Uani 1 1 d . . . . . H23 H 0.3361(10) 0.760(3) 0.4510(16) 0.052(11) Uiso 1 1 d . . . . . C24 C 0.32182(8) 0.69862(19) 0.38097(13) 0.0409(7) Uani 1 1 d . . . . . C25 C 0.33287(8) 0.6381(2) 0.34711(13) 0.0394(7) Uani 1 1 d . . . . . H25 H 0.3174(10) 0.621(2) 0.3177(17) 0.056(11) Uiso 1 1 d . . . . . C26 C 0.36332(8) 0.59782(19) 0.35502(12) 0.0368(6) Uani 1 1 d . . . . . C45 C 0.27652(9) 0.6002(2) 0.20700(13) 0.0442(7) Uani 1 1 d . . . . . H45A H 0.2648 0.6394 0.1853 0.066 Uiso 1 1 calc R U . . . H45B H 0.2903 0.5669 0.1848 0.066 Uiso 1 1 calc R U . . . H45C H 0.2905 0.6276 0.2329 0.066 Uiso 1 1 calc R U . . . C46 C 0.18028(10) 0.7877(2) 0.28710(14) 0.0524(9) Uani 1 1 d . . . . . H46 H 0.1856 0.7995 0.2499 0.063 Uiso 1 1 calc R U . . . C47 C 0.19276(11) 0.8576(3) 0.32103(16) 0.0635(11) Uani 1 1 d . . . . . H47A H 0.1800 0.9054 0.3123 0.095 Uiso 1 1 calc R U . . . H47B H 0.2162 0.8672 0.3143 0.095 Uiso 1 1 calc R U . . . H47C H 0.1900 0.8448 0.3581 0.095 Uiso 1 1 calc R U . . . C48 C 0.20435(8) 0.5949(2) 0.36459(12) 0.0387(7) Uani 1 1 d . . . . . C49 C 0.19771(9) 0.7083(2) 0.30254(13) 0.0454(8) Uani 1 1 d . . . . . C50 C 0.23123(8) 0.5909(2) 0.27812(12) 0.0382(7) Uani 1 1 d . . . . . C51 C 0.25078(8) 0.5467(2) 0.23573(12) 0.0395(7) Uani 1 1 d . . . . . H51 H 0.2631 0.5021 0.2530 0.047 Uiso 1 1 calc R U . . . C61 C 0.43789(7) 0.4085(2) 0.51874(12) 0.0388(7) Uani 1 1 d . . . . . C62 C 0.42985(8) 0.4387(2) 0.57036(13) 0.0432(7) Uani 1 1 d . . . . . C63 C 0.43465(9) 0.3873(3) 0.61433(14) 0.0545(10) Uani 1 1 d . . . . . H63 H 0.4292 0.4066 0.6480 0.065 Uiso 1 1 calc R U . . . C64 C 0.44696(9) 0.3101(3) 0.61036(18) 0.0658(12) Uani 1 1 d . . . . . C65 C 0.45391(9) 0.2812(3) 0.55992(18) 0.0624(11) Uani 1 1 d . . . . . H65 H 0.4617 0.2284 0.5564 0.075 Uiso 1 1 calc R U . . . C66 C 0.44960(9) 0.3284(2) 0.51425(15) 0.0503(8) Uani 1 1 d . . . . . C81 C 0.29452(8) 0.36058(17) 0.43967(11) 0.0341(6) Uani 1 1 d . . . . . C82 C 0.28524(8) 0.37975(18) 0.49282(12) 0.0355(6) Uani 1 1 d . . . . . C83 C 0.30670(8) 0.35697(19) 0.53528(12) 0.0375(6) Uani 1 1 d . . . . . H83 H 0.2996(8) 0.3710(18) 0.5717(13) 0.029(8) Uiso 1 1 d . . . . . C84 C 0.33644(8) 0.31331(19) 0.52758(12) 0.0375(6) Uani 1 1 d . . . . . C85 C 0.34493(8) 0.29584(19) 0.47523(12) 0.0371(6) Uani 1 1 d . . . . . H85 H 0.3650(10) 0.266(2) 0.4704(14) 0.044(9) Uiso 1 1 d . . . . . C86 C 0.32495(8) 0.31884(18) 0.43189(12) 0.0354(6) Uani 1 1 d . . . . . C121 C 0.22425(8) 0.55394(18) 0.32734(12) 0.0350(6) Uani 1 1 d . . . . . C122 C 0.22630(9) 0.5103(2) 0.19446(13) 0.0457(8) Uani 1 1 d . . . . . H12A H 0.2110 0.4742 0.2119 0.069 Uiso 1 1 calc R U . . . H12B H 0.2388 0.4807 0.1683 0.069 Uiso 1 1 calc R U . . . H12C H 0.2138 0.5529 0.1772 0.069 Uiso 1 1 calc R U . . . C123 C 0.21756(8) 0.6674(2) 0.26703(13) 0.0436(7) Uani 1 1 d . . . . . H123 H 0.2221 0.6915 0.2344 0.052 Uiso 1 1 calc R U . . . C124 C 0.14224(12) 0.7785(3) 0.29080(19) 0.0722(12) Uani 1 1 d . . . . . H12D H 0.1348 0.7343 0.2687 0.108 Uiso 1 1 calc R U . . . H12E H 0.1315 0.8276 0.2789 0.108 Uiso 1 1 calc R U . . . H12F H 0.1364 0.7680 0.3272 0.108 Uiso 1 1 calc R U . . . C125 C 0.19199(9) 0.6715(2) 0.35193(13) 0.0443(7) Uani 1 1 d . . . . . H125 H 0.1795 0.6994 0.3771 0.053 Uiso 1 1 calc R U . . . C126 C 0.19398(9) 0.5561(2) 0.41669(13) 0.0437(7) Uani 1 1 d . . . . . H126 H 0.2063 0.5048 0.4204 0.052 Uiso 1 1 calc R U . . . C221 C 0.39797(9) 0.7136(2) 0.47758(16) 0.0504(9) Uani 1 1 d . . . . . H221 H 0.4118 0.6677 0.4897 0.060 Uiso 1 1 calc R U . . . C222 C 0.38064(11) 0.7488(3) 0.52579(18) 0.0686(12) Uani 1 1 d . . . . . H22A H 0.3684 0.7967 0.5154 0.103 Uiso 1 1 calc R U . . . H22B H 0.3973 0.7623 0.5527 0.103 Uiso 1 1 calc R U . . . H22C H 0.3652 0.7096 0.5398 0.103 Uiso 1 1 calc R U . . . C223 C 0.42148(10) 0.7769(2) 0.4538(2) 0.0710(13) Uani 1 1 d . . . . . H22D H 0.4338 0.7531 0.4251 0.107 Uiso 1 1 calc R U . . . H22E H 0.4370 0.7957 0.4809 0.107 Uiso 1 1 calc R U . . . H22F H 0.4084 0.8218 0.4405 0.107 Uiso 1 1 calc R U . . . C241 C 0.28839(8) 0.7403(2) 0.36746(15) 0.0462(8) Uani 1 1 d . . . . . H241 H 0.2721 0.6981 0.3571 0.055 Uiso 1 1 calc R U . . . C242 C 0.29366(11) 0.7952(3) 0.31813(17) 0.0618(10) Uani 1 1 d . . . . . H24A H 0.3081 0.8397 0.3278 0.093 Uiso 1 1 calc R U . . . H24B H 0.2722 0.8156 0.3057 0.093 Uiso 1 1 calc R U . . . H24C H 0.3039 0.7642 0.2903 0.093 Uiso 1 1 calc R U . . . C243 C 0.27374(11) 0.7865(3) 0.41211(17) 0.0669(11) Uani 1 1 d . . . . . H24D H 0.2703 0.7509 0.4418 0.100 Uiso 1 1 calc R U . . . H24E H 0.2525 0.8094 0.4008 0.100 Uiso 1 1 calc R U . . . H24F H 0.2889 0.8293 0.4226 0.100 Uiso 1 1 calc R U . . . C261 C 0.37475(9) 0.5336(2) 0.31591(12) 0.0445(8) Uani 1 1 d . . . . . H261 H 0.3898 0.4962 0.3352 0.053 Uiso 1 1 calc R U . . . C262 C 0.39485(12) 0.5737(3) 0.27183(16) 0.0701(12) Uani 1 1 d . . . . . H26A H 0.4025 0.5331 0.2474 0.105 Uiso 1 1 calc R U . . . H26B H 0.4140 0.6013 0.2873 0.105 Uiso 1 1 calc R U . . . H26C H 0.3808 0.6120 0.2531 0.105 Uiso 1 1 calc R U . . . C263 C 0.34547(10) 0.4843(3) 0.29204(15) 0.0549(9) Uani 1 1 d . . . . . H26D H 0.3325 0.5177 0.2679 0.082 Uiso 1 1 calc R U . . . H26E H 0.3313 0.4657 0.3202 0.082 Uiso 1 1 calc R U . . . H26F H 0.3542 0.4385 0.2731 0.082 Uiso 1 1 calc R U . . . C621 C 0.41786(9) 0.5248(2) 0.57988(13) 0.0477(8) Uani 1 1 d . . . . . H621 H 0.4167 0.5525 0.5453 0.057 Uiso 1 1 calc R U . . . C622 C 0.38282(10) 0.5275(3) 0.60420(16) 0.0602(10) Uani 1 1 d . . . . . H62A H 0.3838 0.5047 0.6394 0.090 Uiso 1 1 calc R U . . . H62B H 0.3673 0.4968 0.5823 0.090 Uiso 1 1 calc R U . . . H62C H 0.3753 0.5827 0.6061 0.090 Uiso 1 1 calc R U . . . C623 C 0.44281(10) 0.5713(3) 0.61598(17) 0.0631(11) Uani 1 1 d . . . . . H62D H 0.4354 0.6264 0.6195 0.095 Uiso 1 1 calc R U . . . H62E H 0.4648 0.5703 0.6005 0.095 Uiso 1 1 calc R U . . . H62F H 0.4438 0.5463 0.6506 0.095 Uiso 1 1 calc R U . . . C641 C 0.4554(3) 0.2409(7) 0.6516(4) 0.048(2) Uani 0.5 1 d . . P A 2 H641 H 0.4442 0.1906 0.6404 0.058 Uiso 0.5 1 calc R U P A 2 C642 C 0.4528(3) 0.2753(8) 0.6685(4) 0.053(2) Uani 0.5 1 d . . P A 1 H642 H 0.4326 0.2872 0.6889 0.064 Uiso 0.5 1 calc R U P A 1 C643 C 0.4551(3) 0.1840(7) 0.6623(4) 0.083(3) Uani 0.5 1 d . . P A 1 H64A H 0.4353 0.1645 0.6435 0.124 Uiso 0.5 1 calc R U P A 1 H64B H 0.4564 0.1592 0.6970 0.124 Uiso 0.5 1 calc R U P A 1 H64C H 0.4748 0.1704 0.6426 0.124 Uiso 0.5 1 calc R U P A 1 C644 C 0.49383(19) 0.2273(6) 0.6557(3) 0.059(2) Uani 0.5 1 d . . P A 2 H64D H 0.5020 0.2093 0.6219 0.089 Uiso 0.5 1 calc R U P A 2 H64E H 0.4987 0.1869 0.6824 0.089 Uiso 0.5 1 calc R U P A 2 H64F H 0.5048 0.2772 0.6655 0.089 Uiso 0.5 1 calc R U P A 2 C645 C 0.4824(4) 0.3106(9) 0.6984(5) 0.123(6) Uani 0.5 1 d . . P A 1 H64G H 0.4835 0.2880 0.7337 0.185 Uiso 0.5 1 calc R U P A 1 H64H H 0.4798 0.3684 0.7007 0.185 Uiso 0.5 1 calc R U P A 1 H64I H 0.5028 0.2982 0.6800 0.185 Uiso 0.5 1 calc R U P A 1 C646 C 0.4421(2) 0.2676(6) 0.7039(4) 0.067(2) Uani 0.5 1 d . . P A 2 H64J H 0.4514 0.3196 0.7130 0.100 Uiso 0.5 1 calc R U P A 2 H64K H 0.4484 0.2289 0.7310 0.100 Uiso 0.5 1 calc R U P A 2 H64L H 0.4179 0.2714 0.7016 0.100 Uiso 0.5 1 calc R U P A 2 C661 C 0.45896(10) 0.2906(2) 0.46091(18) 0.0591(10) Uani 1 1 d . . . . . H661 H 0.4518 0.3278 0.4324 0.071 Uiso 1 1 calc R U . . . C662 C 0.44174(12) 0.2087(3) 0.4509(2) 0.0741(13) Uani 1 1 d . . . . . H66A H 0.4502 0.1698 0.4764 0.111 Uiso 1 1 calc R U . . . H66B H 0.4465 0.1905 0.4155 0.111 Uiso 1 1 calc R U . . . H66C H 0.4178 0.2146 0.4547 0.111 Uiso 1 1 calc R U . . . C663 C 0.49736(12) 0.2792(3) 0.4573(2) 0.0792(14) Uani 1 1 d . . . . . H66D H 0.5084 0.3301 0.4640 0.119 Uiso 1 1 calc R U . . . H66E H 0.5029 0.2603 0.4223 0.119 Uiso 1 1 calc R U . . . H66F H 0.5048 0.2402 0.4835 0.119 Uiso 1 1 calc R U . . . C821 C 0.25091(8) 0.4166(2) 0.50451(12) 0.0381(7) Uani 1 1 d . . . . . H821 H 0.2467 0.4599 0.4784 0.046 Uiso 1 1 calc R U . . . C822 C 0.22292(8) 0.3542(2) 0.49766(13) 0.0446(7) Uani 1 1 d . . . . . H82A H 0.2232 0.3328 0.4620 0.067 Uiso 1 1 calc R U . . . H82B H 0.2015 0.3794 0.5038 0.067 Uiso 1 1 calc R U . . . H82C H 0.2264 0.3109 0.5228 0.067 Uiso 1 1 calc R U . . . C823 C 0.24826(9) 0.4540(2) 0.56037(12) 0.0439(7) Uani 1 1 d . . . . . H82D H 0.2480 0.4116 0.5866 0.066 Uiso 1 1 calc R U . . . H82E H 0.2278 0.4850 0.5624 0.066 Uiso 1 1 calc R U . . . H82F H 0.2673 0.4888 0.5671 0.066 Uiso 1 1 calc R U . . . C841 C 0.35906(8) 0.2838(2) 0.57325(12) 0.0416(7) Uani 1 1 d . . . . . H841 H 0.3819 0.3038 0.5666 0.050 Uiso 1 1 calc R U . . . C842 C 0.36076(10) 0.1910(2) 0.57435(15) 0.0543(9) Uani 1 1 d . . . . . H84A H 0.3390 0.1696 0.5829 0.081 Uiso 1 1 calc R U . . . H84B H 0.3770 0.1740 0.6009 0.081 Uiso 1 1 calc R U . . . H84C H 0.3673 0.1714 0.5400 0.081 Uiso 1 1 calc R U . . . C843 C 0.34890(9) 0.3147(3) 0.62797(13) 0.0518(9) Uani 1 1 d . . . . . H84D H 0.3481 0.3729 0.6275 0.078 Uiso 1 1 calc R U . . . H84E H 0.3651 0.2970 0.6544 0.078 Uiso 1 1 calc R U . . . H84F H 0.3270 0.2938 0.6365 0.078 Uiso 1 1 calc R U . . . C861 C 0.33650(9) 0.2939(2) 0.37595(12) 0.0419(7) Uani 1 1 d . . . . . H861 H 0.3220 0.3217 0.3496 0.050 Uiso 1 1 calc R U . . . C862 C 0.33219(11) 0.2022(2) 0.36782(16) 0.0533(9) Uani 1 1 d . . . . . H86A H 0.3483(13) 0.171(3) 0.395(2) 0.080 Uiso 1 1 d . U . . . H86B H 0.3394(13) 0.187(3) 0.336(2) 0.080 Uiso 1 1 d . U . . . H86C H 0.3038(13) 0.186(3) 0.3707(19) 0.080 Uiso 1 1 d . U . . . C863 C 0.37282(9) 0.3187(3) 0.36589(14) 0.0503(8) Uani 1 1 d . . . . . H86D H 0.3762 0.3738 0.3770 0.075 Uiso 1 1 calc R U . . . H86E H 0.3774 0.3138 0.3285 0.075 Uiso 1 1 calc R U . . . H86F H 0.3879 0.2839 0.3858 0.075 Uiso 1 1 calc R U . . . C13 C 0.4395(7) -0.016(2) 0.5739(14) 0.234(13) Uani 0.5 1 d D U P B -1 H13A H 0.4345 0.0026 0.6091 0.352 Uiso 0.5 1 d R U P B -1 H13B H 0.4378 -0.0744 0.5729 0.352 Uiso 0.5 1 d R U P B -1 H13C H 0.4236 0.0066 0.5488 0.352 Uiso 0.5 1 d R U P B -1 C14 C 0.4750(7) 0.0084(19) 0.5595(11) 0.179(8) Uani 0.5 1 d D U P B -1 H14A H 0.4908 -0.0172 0.5844 0.214 Uiso 0.5 1 calc R U P B -1 H14B H 0.4772 0.0666 0.5639 0.214 Uiso 0.5 1 calc R U P B -1 C15 C 0.4849(6) -0.0138(15) 0.5029(12) 0.140(7) Uani 0.5 1 d D U P B -1 H15A H 0.4869 -0.0723 0.5012 0.168 Uiso 0.5 1 calc R U P B -1 H15B H 0.4663 0.0015 0.4792 0.168 Uiso 0.5 1 calc R U P B -1 C16 C 0.5169(9) 0.022(3) 0.4807(15) 0.209(12) Uani 0.5 1 d D U P B -1 H16A H 0.5361 -0.0065 0.4960 0.251 Uiso 0.5 1 calc R U P B -1 H16B H 0.5185 0.0783 0.4922 0.251 Uiso 0.5 1 calc R U P B -1 C17 C 0.5194(10) 0.020(3) 0.4202(14) 0.243(14) Uani 0.5 1 d D U P B -1 H17A H 0.5196 -0.0367 0.4093 0.292 Uiso 0.5 1 calc R U P B -1 H17B H 0.4991 0.0440 0.4051 0.292 Uiso 0.5 1 calc R U P B -1 C18 C 0.5496(9) 0.061(2) 0.3958(17) 0.278(17) Uani 0.5 1 d D U P B -1 H18A H 0.5495 0.0498 0.3582 0.418 Uiso 0.5 1 d R U P B -1 H18B H 0.5705 0.0431 0.4117 0.418 Uiso 0.5 1 d R U P B -1 H18C H 0.5473 0.1186 0.4012 0.418 Uiso 0.5 1 d R U P B -1 C19 C 0.4872(7) 0.0101(16) 0.250(2) 0.167(15) Uani 0.25 1 d . U P C -1 H19A H 0.5041 0.0257 0.2762 0.250 Uiso 0.25 1 d R U P C -1 H19B H 0.4977 -0.0189 0.2217 0.250 Uiso 0.25 1 d R U P C -1 H19C H 0.4708 -0.0240 0.2668 0.250 Uiso 0.25 1 d R U P C -1 C20 C 0.4702(8) 0.0919(18) 0.2251(12) 0.146(4) Uani 0.25 1 d DG U P C -1 H20A H 0.4838 0.1138 0.1966 0.175 Uiso 0.25 1 calc R U P C -1 H20B H 0.4476 0.0813 0.2113 0.175 Uiso 0.25 1 calc R U P C -1 C52 C 0.4695(7) 0.1494(16) 0.2725(11) 0.145(3) Uani 0.25 1 d DG U P C -1 H52A H 0.4816 0.1248 0.3024 0.175 Uiso 0.25 1 d R U P C -1 H52B H 0.4463 0.1574 0.2830 0.175 Uiso 0.25 1 d R U P C -1 C43 C 0.4516(10) 0.2758(13) 0.2929(12) 0.143(3) Uani 0.25 1 d D U P C -1 H43A H 0.4725 0.2693 0.3132 0.172 Uiso 0.25 1 calc R U P C -1 H43B H 0.4327 0.2720 0.3170 0.172 Uiso 0.25 1 calc R U P C -1 C44 C 0.4510(8) 0.3528(16) 0.2640(13) 0.143(3) Uani 0.25 1 d D U P C -1 H44A H 0.4269 0.3554 0.2667 0.215 Uiso 0.25 1 d R U P C -1 H44B H 0.4574 0.3666 0.2283 0.215 Uiso 0.25 1 d R U P C -1 H44C H 0.4612 0.3904 0.2887 0.215 Uiso 0.25 1 d R U P C -1 C53 C 0.4488(7) 0.2165(14) 0.2508(12) 0.145(3) Uani 0.25 1 d D U P C -1 H53A H 0.4579 0.2369 0.2177 0.174 Uiso 0.25 1 calc R U P C -1 H53B H 0.4256 0.1999 0.2447 0.174 Uiso 0.25 1 calc R U P C -1 C27 C 0.5051(7) 0.3829(18) 0.2473(16) 0.127(5) Uani 0.25 1 d D U P D -2 C28 C 0.5265(6) 0.4260(17) 0.2132(12) 0.125(5) Uani 0.25 1 d D U P D -2 H28A H 0.5134 0.4494 0.1840 0.150 Uiso 0.25 1 calc R U P D -2 H28B H 0.5374 0.4698 0.2327 0.150 Uiso 0.25 1 calc R U P D -2 C29 C 0.5499(6) 0.375(2) 0.1940(13) 0.124(5) Uani 0.25 1 d D U P D -2 H29A H 0.5706 0.3814 0.2147 0.149 Uiso 0.25 1 d R U P D -2 H29B H 0.5546 0.3900 0.1574 0.149 Uiso 0.25 1 d R U P D -2 C30 C 0.5401(7) 0.294(2) 0.1957(13) 0.125(5) Uani 0.25 1 d D U P D -2 H30A H 0.5478 0.2704 0.2287 0.187 Uiso 0.25 1 calc R U P D -2 H30B H 0.5497 0.2654 0.1664 0.187 Uiso 0.25 1 calc R U P D -2 H30C H 0.5159 0.2907 0.1932 0.187 Uiso 0.25 1 calc R U P D -2 C41 C 0.4620(9) 0.4051(19) 0.3064(15) 0.143(3) Uani 0.25 1 d D U P D -2 H41A H 0.4534 0.4585 0.3128 0.215 Uiso 0.25 1 d R U P D -2 H41B H 0.4436 0.3688 0.2987 0.215 Uiso 0.25 1 d R U P D -2 H41C H 0.4743 0.3865 0.3375 0.215 Uiso 0.25 1 d R U P D -2 C42 C 0.4840(6) 0.4423(19) 0.2719(14) 0.128(5) Uani 0.25 1 d D U P D -2 H42A H 0.4980 0.4809 0.2914 0.153 Uiso 0.25 1 calc R U P D -2 H42B H 0.4713 0.4715 0.2446 0.153 Uiso 0.25 1 calc R U P D -2 C31 C 0.3758(3) 1.0108(5) 0.4415(3) 0.163(4) Uani 1 1 d . U . . . H31A H 0.3602 1.0553 0.4394 0.245 Uiso 1 1 calc R U . . . H31B H 0.3911 1.0188 0.4712 0.245 Uiso 1 1 calc R U . . . H31C H 0.3636 0.9611 0.4462 0.245 Uiso 1 1 calc R U . . . C32 C 0.3943(2) 1.0066(5) 0.3938(3) 0.117(2) Uani 1 1 d . U . . . H32C H 0.4183 1.0029 0.4023 0.141 Uiso 0.5 1 calc R U P E 2 H32D H 0.3906 1.0556 0.3731 0.141 Uiso 0.5 1 calc R U P E 2 H32A H 0.4115 0.9652 0.3981 0.141 Uiso 0.5 1 calc R U P F 1 H32B H 0.4058 1.0579 0.3890 0.141 Uiso 0.5 1 calc R U P F 1 C33 C 0.3831(4) 0.9310(10) 0.3599(6) 0.112(4) Uani 0.5 1 d . U P G 2 H33A H 0.3643 0.9465 0.3367 0.134 Uiso 0.5 1 calc R U P G 2 H33B H 0.3751 0.8894 0.3839 0.134 Uiso 0.5 1 calc R U P G 2 C34 C 0.3748(4) 0.9891(11) 0.3449(8) 0.131(5) Uani 0.5 1 d . U P G 1 H34A H 0.3525 1.0125 0.3484 0.157 Uiso 0.5 1 calc R U P G 1 H34B H 0.3720 0.9308 0.3422 0.157 Uiso 0.5 1 calc R U P G 1 C35 C 0.4118(4) 0.8935(11) 0.3245(7) 0.139(5) Uani 0.5 1 d . U P G 2 H35A H 0.4191 0.9340 0.2991 0.167 Uiso 0.5 1 calc R U P G 2 H35B H 0.4311 0.8801 0.3473 0.167 Uiso 0.5 1 calc R U P G 2 C36 C 0.3909(6) 1.0223(16) 0.2879(7) 0.164(7) Uani 0.5 1 d . U P G 1 C37 C 0.3735(5) 1.0086(17) 0.2377(10) 0.176(8) Uani 0.5 1 d . U P G 1 H37A H 0.3855 1.0294 0.2071 0.211 Uiso 0.5 1 calc R U P G 1 H37B H 0.3503 1.0272 0.2373 0.211 Uiso 0.5 1 calc R U P G 1 C38 C 0.4006(5) 0.8176(11) 0.2942(6) 0.139(6) Uani 0.5 1 d . U P G 2 H38A H 0.3886 0.7807 0.3173 0.167 Uiso 0.5 1 calc R U P G 2 H38B H 0.4197 0.7896 0.2792 0.167 Uiso 0.5 1 calc R U P G 2 C39 C 0.3765(5) 0.8517(17) 0.2490(9) 0.189(11) Uani 0.5 1 d . U P G 2 H39A H 0.3893 0.8844 0.2249 0.284 Uiso 0.5 1 calc R U P G 2 H39B H 0.3592 0.8843 0.2647 0.284 Uiso 0.5 1 calc R U P G 2 H39C H 0.3663 0.8075 0.2298 0.284 Uiso 0.5 1 calc R U P G 2 C40 C 0.3769(6) 0.9221(16) 0.2447(18) 0.241(14) Uani 0.5 1 d . U P G 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.03107(15) 0.03836(15) 0.02855(14) -0.00314(10) -0.00709(10) 0.00213(10) Cl1 0.0440(4) 0.0695(5) 0.0415(4) -0.0199(4) -0.0024(3) 0.0036(4) N1 0.0314(12) 0.0406(14) 0.0308(12) 0.0023(11) -0.0052(9) 0.0040(11) N2 0.0351(13) 0.0345(13) 0.0315(12) -0.0027(10) -0.0075(10) -0.0006(11) C1 0.0324(14) 0.0378(15) 0.0282(13) -0.0033(11) -0.0073(11) -0.0006(12) C1A 0.062(2) 0.065(2) 0.0296(16) 0.0000(15) -0.0075(15) 0.0138(19) C1B 0.054(2) 0.060(2) 0.046(2) 0.0035(18) 0.0067(17) 0.0021(19) C2 0.0346(15) 0.0405(16) 0.0315(14) -0.0006(12) -0.0083(12) 0.0008(12) C3 0.0367(16) 0.0496(18) 0.0365(16) 0.0058(14) -0.0062(12) -0.0039(14) C4 0.0310(15) 0.0537(19) 0.0393(17) 0.0047(14) -0.0036(12) -0.0032(14) C5 0.0318(15) 0.0489(18) 0.0352(15) -0.0002(13) -0.0053(12) 0.0072(14) C6 0.0337(15) 0.0412(15) 0.0276(14) -0.0009(12) -0.0050(11) 0.0026(12) C7 0.0366(15) 0.0356(15) 0.0242(13) -0.0030(11) 0.0000(11) -0.0031(12) C8 0.0376(15) 0.0370(15) 0.0254(13) -0.0001(11) -0.0010(11) -0.0019(12) C9 0.0485(18) 0.0350(15) 0.0301(14) 0.0007(12) -0.0024(13) -0.0042(13) C10 0.0545(19) 0.0393(16) 0.0291(15) -0.0018(12) -0.0051(13) -0.0124(15) C11 0.0444(17) 0.0462(17) 0.0226(13) -0.0001(12) -0.0088(12) -0.0101(14) C12 0.0388(15) 0.0407(15) 0.0231(13) 0.0014(11) -0.0026(11) -0.0032(13) C21 0.0335(15) 0.0376(15) 0.0363(15) 0.0061(12) -0.0081(12) -0.0023(12) C22 0.0383(16) 0.0346(15) 0.0487(18) 0.0017(13) -0.0132(14) -0.0035(13) C23 0.0396(17) 0.0358(16) 0.055(2) -0.0010(15) -0.0127(15) -0.0001(14) C24 0.0382(16) 0.0360(16) 0.0482(18) 0.0089(13) -0.0105(13) -0.0011(13) C25 0.0393(16) 0.0421(17) 0.0365(16) 0.0074(13) -0.0096(13) -0.0030(14) C26 0.0355(15) 0.0415(16) 0.0331(15) 0.0080(12) -0.0079(12) -0.0051(13) C45 0.0450(18) 0.055(2) 0.0327(15) 0.0082(14) -0.0047(13) -0.0009(15) C46 0.058(2) 0.059(2) 0.0401(18) 0.0089(16) -0.0033(16) 0.0136(18) C47 0.065(2) 0.073(3) 0.052(2) 0.0082(19) -0.0132(18) 0.016(2) C48 0.0394(16) 0.0465(17) 0.0300(14) 0.0007(13) -0.0081(12) 0.0009(14) C49 0.0440(18) 0.0513(19) 0.0405(17) 0.0075(14) -0.0045(14) 0.0042(15) C50 0.0384(16) 0.0446(17) 0.0314(15) 0.0041(13) -0.0076(12) -0.0032(14) C51 0.0423(17) 0.0457(17) 0.0303(15) 0.0062(12) -0.0015(12) 0.0029(14) C61 0.0295(14) 0.0498(18) 0.0368(16) 0.0074(13) -0.0037(12) 0.0026(13) C62 0.0297(15) 0.065(2) 0.0350(16) 0.0056(15) -0.0067(12) -0.0010(14) C63 0.0360(17) 0.092(3) 0.0352(17) 0.0174(18) -0.0081(13) -0.0111(19) C64 0.0336(18) 0.094(3) 0.069(3) 0.047(2) -0.0094(17) -0.001(2) C65 0.0411(19) 0.067(2) 0.079(3) 0.035(2) 0.0036(18) 0.0104(18) C66 0.0365(17) 0.058(2) 0.057(2) 0.0163(17) 0.0009(15) 0.0105(15) C81 0.0413(16) 0.0327(14) 0.0283(14) 0.0010(11) -0.0039(12) -0.0016(12) C82 0.0409(16) 0.0360(15) 0.0294(14) 0.0019(12) -0.0045(12) -0.0018(13) C83 0.0434(17) 0.0405(16) 0.0285(14) 0.0020(12) -0.0028(12) -0.0005(13) C84 0.0391(16) 0.0398(16) 0.0335(15) 0.0048(12) -0.0038(12) -0.0045(13) C85 0.0362(16) 0.0383(16) 0.0368(16) 0.0009(12) -0.0029(12) -0.0004(13) C86 0.0356(15) 0.0355(15) 0.0351(15) 0.0028(12) -0.0001(12) -0.0042(12) C121 0.0361(15) 0.0401(16) 0.0283(14) 0.0002(12) -0.0095(11) -0.0020(13) C122 0.057(2) 0.0461(18) 0.0339(16) 0.0046(14) -0.0026(14) -0.0050(16) C123 0.0435(17) 0.0525(19) 0.0345(16) 0.0113(14) -0.0039(13) 0.0035(15) C124 0.065(3) 0.085(3) 0.067(3) 0.020(2) -0.006(2) 0.020(2) C125 0.0453(18) 0.0499(19) 0.0375(16) 0.0003(14) -0.0037(13) 0.0071(15) C126 0.0500(19) 0.0483(18) 0.0329(16) 0.0020(13) -0.0008(13) 0.0084(15) C221 0.0429(18) 0.0388(17) 0.068(2) -0.0124(16) -0.0262(17) 0.0020(14) C222 0.057(2) 0.071(3) 0.077(3) -0.035(2) -0.028(2) 0.006(2) C223 0.045(2) 0.048(2) 0.120(4) -0.010(2) -0.021(2) -0.0038(17) C241 0.0376(17) 0.0393(17) 0.061(2) 0.0064(15) -0.0150(15) 0.0028(14) C242 0.055(2) 0.062(2) 0.068(3) 0.019(2) -0.0065(19) 0.0102(19) C243 0.056(2) 0.081(3) 0.062(2) -0.014(2) -0.0194(19) 0.019(2) C261 0.0435(17) 0.063(2) 0.0267(15) 0.0004(14) -0.0044(12) 0.0056(16) C262 0.067(3) 0.105(4) 0.038(2) 0.011(2) 0.0046(18) 0.003(3) C263 0.056(2) 0.067(2) 0.0421(19) -0.0114(17) -0.0150(16) 0.0107(19) C621 0.0447(18) 0.067(2) 0.0311(16) -0.0037(15) -0.0002(13) -0.0003(17) C622 0.049(2) 0.087(3) 0.044(2) -0.0031(19) -0.0013(16) 0.007(2) C623 0.051(2) 0.086(3) 0.052(2) -0.019(2) 0.0009(17) -0.007(2) C641 0.043(4) 0.060(7) 0.042(6) 0.012(5) -0.009(4) -0.004(4) C642 0.054(5) 0.068(7) 0.038(6) 0.015(5) -0.004(4) 0.003(5) C643 0.116(9) 0.068(6) 0.063(6) 0.034(5) -0.004(5) 0.015(6) C644 0.047(4) 0.086(6) 0.043(4) 0.023(4) -0.009(3) 0.022(4) C645 0.127(10) 0.149(12) 0.091(8) 0.075(8) -0.071(8) -0.060(9) C646 0.060(5) 0.092(7) 0.047(5) 0.019(4) -0.007(4) 0.013(5) C661 0.058(2) 0.048(2) 0.071(3) 0.0042(18) 0.0108(19) 0.0133(18) C662 0.069(3) 0.050(2) 0.105(4) 0.001(2) 0.014(3) 0.016(2) C663 0.059(3) 0.061(3) 0.118(4) 0.006(3) 0.029(3) 0.014(2) C821 0.0445(17) 0.0435(16) 0.0260(14) 0.0032(12) -0.0035(12) 0.0043(14) C822 0.0407(17) 0.055(2) 0.0385(17) -0.0023(14) 0.0014(13) -0.0028(15) C823 0.0496(19) 0.054(2) 0.0276(15) -0.0010(13) -0.0001(13) 0.0056(15) C841 0.0363(16) 0.0524(19) 0.0358(16) 0.0087(14) -0.0045(12) -0.0020(14) C842 0.055(2) 0.056(2) 0.051(2) 0.0147(17) -0.0129(17) 0.0028(18) C843 0.0491(19) 0.072(2) 0.0345(17) 0.0103(16) -0.0052(14) 0.0055(18) C861 0.0456(18) 0.0476(18) 0.0324(15) -0.0048(13) -0.0018(13) -0.0015(14) C862 0.064(2) 0.053(2) 0.0428(19) -0.0132(16) 0.0018(17) 0.0003(18) C863 0.0481(19) 0.066(2) 0.0371(17) -0.0023(16) 0.0025(14) 0.0026(17) C13 0.165(15) 0.24(3) 0.30(3) -0.04(2) -0.005(17) -0.035(18) C14 0.171(13) 0.119(16) 0.24(2) -0.032(12) -0.025(12) -0.002(13) C15 0.119(9) 0.064(8) 0.236(19) -0.018(10) -0.049(10) 0.011(7) C16 0.183(13) 0.142(19) 0.30(2) -0.039(16) 0.006(15) -0.027(13) C17 0.25(2) 0.18(3) 0.30(3) -0.031(17) 0.022(17) 0.00(2) C18 0.23(3) 0.23(3) 0.37(3) 0.03(2) 0.03(2) 0.01(2) C19 0.091(19) 0.080(15) 0.33(4) 0.01(3) 0.06(3) 0.003(14) C20 0.113(6) 0.143(7) 0.184(7) 0.041(6) 0.061(6) 0.043(6) C52 0.113(6) 0.142(7) 0.183(7) 0.042(6) 0.061(6) 0.044(6) C43 0.110(6) 0.141(6) 0.181(7) 0.043(6) 0.062(6) 0.045(5) C44 0.110(6) 0.141(6) 0.181(7) 0.044(6) 0.062(6) 0.045(5) C53 0.112(6) 0.142(6) 0.182(7) 0.043(6) 0.062(6) 0.044(6) C27 0.056(8) 0.212(14) 0.114(9) -0.030(11) 0.023(6) -0.002(8) C28 0.053(8) 0.210(14) 0.112(9) -0.030(11) 0.024(6) -0.002(8) C29 0.052(8) 0.209(14) 0.111(9) -0.031(11) 0.025(6) -0.002(8) C30 0.052(8) 0.209(14) 0.113(9) -0.031(11) 0.028(7) -0.001(8) C41 0.110(6) 0.141(6) 0.181(7) 0.043(6) 0.062(6) 0.046(5) C42 0.057(8) 0.212(14) 0.114(9) -0.030(11) 0.021(6) -0.001(8) C31 0.269(12) 0.103(5) 0.121(6) 0.024(5) 0.095(7) 0.021(7) C32 0.132(6) 0.128(6) 0.092(5) -0.019(4) 0.005(4) 0.010(5) C33 0.132(11) 0.115(10) 0.089(8) -0.001(8) -0.007(8) -0.012(9) C34 0.114(10) 0.116(10) 0.161(13) -0.050(10) -0.040(9) 0.025(9) C35 0.134(12) 0.154(13) 0.130(12) -0.040(10) 0.028(10) 0.004(11) C36 0.166(15) 0.239(18) 0.087(10) -0.050(11) 0.022(10) -0.007(14) C37 0.099(11) 0.23(2) 0.194(18) 0.006(17) -0.039(11) 0.017(14) C38 0.187(16) 0.132(12) 0.099(10) -0.025(9) 0.034(11) 0.016(12) C39 0.142(15) 0.26(3) 0.163(17) -0.131(19) -0.013(13) -0.031(18) C40 0.110(14) 0.127(16) 0.49(4) 0.06(2) 0.03(2) 0.018(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 H2 2.56(5) . ? Y1 Cl1 2.5071(8) . ? Y1 N1 2.249(2) . ? Y1 N2 2.213(2) . ? Y1 C21 2.782(3) . ? Y1 C22 2.869(3) . ? Y1 C23 2.904(3) . ? Y1 C24 2.920(3) . ? Y1 C25 2.873(3) . ? Y1 C26 2.822(3) . ? N1 H1 0.88(4) . ? N1 C1 1.386(4) . ? N2 H2 0.87(5) . ? N2 C7 1.383(4) . ? C1 C2 1.417(4) . ? C1 C6 1.424(4) . ? C1A H1AA 0.9600 . ? C1A H1AB 0.9600 . ? C1A H1AC 0.9600 . ? C1A C126 1.530(5) . ? C1B H1BA 1.03(5) . ? C1B H1BB 0.97(5) . ? C1B H1BC 0.97(4) . ? C1B C126 1.524(5) . ? C2 C3 1.384(4) . ? C2 C21 1.488(4) . ? C3 H3 0.9300 . ? C3 C4 1.381(5) . ? C4 H4 0.9300 . ? C4 C5 1.383(5) . ? C5 H5 0.98(4) . ? C5 C6 1.393(4) . ? C6 C61 1.501(4) . ? C7 C8 1.414(4) . ? C7 C12 1.423(4) . ? C8 C9 1.401(4) . ? C8 C81 1.495(4) . ? C9 H9 1.03(4) . ? C9 C10 1.382(5) . ? C10 H10 0.99(4) . ? C10 C11 1.390(5) . ? C11 H11 0.9300 . ? C11 C12 1.388(4) . ? C12 C121 1.504(4) . ? C21 C22 1.416(5) . ? C21 C26 1.423(4) . ? C22 C23 1.400(5) . ? C22 C221 1.523(4) . ? C23 H23 0.97(4) . ? C23 C24 1.400(5) . ? C24 C25 1.386(5) . ? C24 C241 1.524(4) . ? C25 H25 0.99(4) . ? C25 C26 1.388(4) . ? C26 C261 1.517(5) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C45 C51 1.536(5) . ? C46 H46 0.9800 . ? C46 C47 1.511(6) . ? C46 C49 1.527(5) . ? C46 C124 1.519(6) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 C121 1.405(4) . ? C48 C125 1.390(5) . ? C48 C126 1.517(4) . ? C49 C123 1.374(5) . ? C49 C125 1.399(5) . ? C50 C51 1.512(5) . ? C50 C121 1.407(4) . ? C50 C123 1.399(5) . ? C51 H51 0.9800 . ? C51 C122 1.528(5) . ? C61 C62 1.427(5) . ? C61 C66 1.405(5) . ? C62 C63 1.400(5) . ? C62 C621 1.517(5) . ? C63 H63 0.9300 . ? C63 C64 1.367(7) . ? C64 C65 1.383(7) . ? C64 C641 1.572(11) . ? C64 C642 1.578(11) . ? C65 H65 0.9300 . ? C65 C66 1.391(5) . ? C66 C661 1.526(6) . ? C81 C82 1.423(4) . ? C81 C86 1.404(4) . ? C82 C83 1.401(4) . ? C82 C821 1.522(4) . ? C83 H83 0.99(3) . ? C83 C84 1.397(5) . ? C84 C85 1.390(4) . ? C84 C841 1.520(4) . ? C85 H85 0.95(4) . ? C85 C86 1.385(4) . ? C86 C861 1.537(4) . ? C122 H12A 0.9600 . ? C122 H12B 0.9600 . ? C122 H12C 0.9600 . ? C123 H123 0.9300 . ? C124 H12D 0.9600 . ? C124 H12E 0.9600 . ? C124 H12F 0.9600 . ? C125 H125 0.9300 . ? C126 H126 0.9800 . ? C221 H221 0.9800 . ? C221 C222 1.515(6) . ? C221 C223 1.527(6) . ? C222 H22A 0.9600 . ? C222 H22B 0.9600 . ? C222 H22C 0.9600 . ? C223 H22D 0.9600 . ? C223 H22E 0.9600 . ? C223 H22F 0.9600 . ? C241 H241 0.9800 . ? C241 C242 1.549(5) . ? C241 C243 1.481(6) . ? C242 H24A 0.9600 . ? C242 H24B 0.9600 . ? C242 H24C 0.9600 . ? C243 H24D 0.9600 . ? C243 H24E 0.9600 . ? C243 H24F 0.9600 . ? C261 H261 0.9800 . ? C261 C262 1.524(5) . ? C261 C263 1.530(5) . ? C262 H26A 0.9600 . ? C262 H26B 0.9600 . ? C262 H26C 0.9600 . ? C263 H26D 0.9600 . ? C263 H26E 0.9600 . ? C263 H26F 0.9600 . ? C621 H621 0.9800 . ? C621 C622 1.526(5) . ? C621 C623 1.533(5) . ? C622 H62A 0.9600 . ? C622 H62B 0.9600 . ? C622 H62C 0.9600 . ? C623 H62D 0.9600 . ? C623 H62E 0.9600 . ? C623 H62F 0.9600 . ? C641 H641 0.9800 . ? C641 C644 1.540(12) . ? C641 C646 1.487(13) . ? C642 H642 0.9800 . ? C642 C643 1.517(15) . ? C642 C645 1.496(15) . ? C643 H64A 0.9600 . ? C643 H64B 0.9600 . ? C643 H64C 0.9600 . ? C644 H64D 0.9600 . ? C644 H64E 0.9600 . ? C644 H64F 0.9600 . ? C645 H64G 0.9600 . ? C645 H64H 0.9600 . ? C645 H64I 0.9600 . ? C646 H64J 0.9600 . ? C646 H64K 0.9600 . ? C646 H64L 0.9600 . ? C661 H661 0.9800 . ? C661 C662 1.531(6) . ? C661 C663 1.537(6) . ? C662 H66A 0.9600 . ? C662 H66B 0.9600 . ? C662 H66C 0.9600 . ? C663 H66D 0.9600 . ? C663 H66E 0.9600 . ? C663 H66F 0.9600 . ? C821 H821 0.9800 . ? C821 C822 1.521(5) . ? C821 C823 1.534(4) . ? C822 H82A 0.9600 . ? C822 H82B 0.9600 . ? C822 H82C 0.9600 . ? C823 H82D 0.9600 . ? C823 H82E 0.9600 . ? C823 H82F 0.9600 . ? C841 H841 0.9800 . ? C841 C842 1.532(5) . ? C841 C843 1.523(5) . ? C842 H84A 0.9600 . ? C842 H84B 0.9600 . ? C842 H84C 0.9600 . ? C843 H84D 0.9600 . ? C843 H84E 0.9600 . ? C843 H84F 0.9600 . ? C861 H861 0.9800 . ? C861 C862 1.536(5) . ? C861 C863 1.521(5) . ? C862 H86A 1.06(5) . ? C862 H86B 0.89(5) . ? C862 H86C 1.16(5) . ? C863 H86D 0.9600 . ? C863 H86E 0.9600 . ? C863 H86F 0.9600 . ? C13 H13A 0.9599 . ? C13 H13B 0.9600 . ? C13 H13C 0.9598 . ? C13 C14 1.516(12) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 C15 1.521(12) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 C16 1.515(11) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 C17 1.520(13) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 C18 1.517(13) . ? C18 H18A 0.9599 . ? C18 H18B 0.9600 . ? C18 H18C 0.9603 . ? C19 H19A 0.9602 . ? C19 H19B 0.9599 . ? C19 H19C 0.9603 . ? C19 C20 1.63(4) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 C52 1.5211 . ? C52 H52A 0.9703 . ? C52 H52B 0.9692 . ? C52 C53 1.475(18) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 C44 1.462(18) . ? C43 C53 1.443(19) . ? C44 H44A 0.9598 . ? C44 H44B 0.9599 . ? C44 H44C 0.9602 . ? C53 H52B 1.2694 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C27 C28 1.41(2) . ? C27 C42 1.43(2) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 C29 1.346(18) . ? C29 H29A 0.9701 . ? C29 H29B 0.9700 . ? C29 C30 1.39(2) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C41 H41A 0.9596 . ? C41 H41B 0.9598 . ? C41 H41C 0.9604 . ? C41 C42 1.38(4) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C31 C32 1.414(9) . ? C32 H32C 0.9700 . ? C32 H32D 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 C33 1.569(16) . ? C32 C34 1.465(16) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 C35 1.58(2) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 C36 1.67(3) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 C38 1.53(2) . ? C36 C37 1.44(3) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 C40 1.44(3) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 C39 1.57(3) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Y1 H2 96.1(10) . . ? Cl1 Y1 C21 117.67(7) . . ? Cl1 Y1 C22 89.56(7) . . ? Cl1 Y1 C23 79.03(8) . . ? Cl1 Y1 C24 93.80(7) . . ? Cl1 Y1 C25 121.42(7) . . ? Cl1 Y1 C26 137.26(7) . . ? N1 Y1 H2 150.2(10) . . ? N1 Y1 Cl1 110.95(7) . . ? N1 Y1 C21 64.58(9) . . ? N1 Y1 C22 79.64(9) . . ? N1 Y1 C23 107.69(10) . . ? N1 Y1 C24 123.88(10) . . ? N1 Y1 C25 109.15(9) . . ? N1 Y1 C26 80.97(9) . . ? N2 Y1 H2 19.3(10) . . ? N2 Y1 Cl1 104.41(7) . . ? N2 Y1 N1 133.75(10) . . ? N2 Y1 C21 122.05(9) . . ? N2 Y1 C22 130.18(9) . . ? N2 Y1 C23 107.49(10) . . ? N2 Y1 C24 81.09(9) . . ? N2 Y1 C25 74.26(9) . . ? N2 Y1 C26 92.88(9) . . ? C21 Y1 H2 114.0(10) . . ? C21 Y1 C22 28.97(9) . . ? C21 Y1 C23 50.44(10) . . ? C21 Y1 C24 59.31(9) . . ? C21 Y1 C25 50.65(9) . . ? C21 Y1 C26 29.41(8) . . ? C22 Y1 H2 113.8(10) . . ? C22 Y1 C23 28.06(9) . . ? C22 Y1 C24 50.00(9) . . ? C22 Y1 C25 58.17(9) . . ? C23 Y1 H2 89.0(10) . . ? C23 Y1 C24 27.81(9) . . ? C24 Y1 H2 63.8(10) . . ? C25 Y1 H2 63.4(10) . . ? C25 Y1 C23 48.85(10) . . ? C25 Y1 C24 27.66(10) . . ? C26 Y1 H2 87.6(10) . . ? C26 Y1 C22 51.06(9) . . ? C26 Y1 C23 58.43(10) . . ? C26 Y1 C24 50.13(9) . . ? C26 Y1 C25 28.20(9) . . ? Y1 N1 H1 118(3) . . ? C1 N1 Y1 131.5(2) . . ? C1 N1 H1 111(3) . . ? Y1 N2 H2 103(3) . . ? C7 N2 Y1 144.2(2) . . ? C7 N2 H2 112(3) . . ? N1 C1 C2 117.8(3) . . ? N1 C1 C6 124.8(3) . . ? C2 C1 C6 117.3(3) . . ? H1AA C1A H1AB 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? C126 C1A H1AA 109.5 . . ? C126 C1A H1AB 109.5 . . ? C126 C1A H1AC 109.5 . . ? H1BA C1B H1BB 109(4) . . ? H1BA C1B H1BC 104(4) . . ? H1BB C1B H1BC 111(4) . . ? C126 C1B H1BA 114(3) . . ? C126 C1B H1BB 113(3) . . ? C126 C1B H1BC 106(2) . . ? C1 C2 C21 116.1(3) . . ? C3 C2 C1 121.9(3) . . ? C3 C2 C21 121.9(3) . . ? C2 C3 H3 119.9 . . ? C4 C3 C2 120.2(3) . . ? C4 C3 H3 119.9 . . ? C3 C4 H4 120.7 . . ? C3 C4 C5 118.6(3) . . ? C5 C4 H4 120.7 . . ? C4 C5 H5 121(2) . . ? C4 C5 C6 123.2(3) . . ? C6 C5 H5 116(2) . . ? C1 C6 C61 124.4(3) . . ? C5 C6 C1 118.4(3) . . ? C5 C6 C61 117.0(3) . . ? N2 C7 C8 119.4(3) . . ? N2 C7 C12 121.8(3) . . ? C8 C7 C12 118.8(3) . . ? C7 C8 C81 121.1(3) . . ? C9 C8 C7 119.2(3) . . ? C9 C8 C81 119.6(3) . . ? C8 C9 H9 120(2) . . ? C10 C9 C8 121.7(3) . . ? C10 C9 H9 118(2) . . ? C9 C10 H10 120(2) . . ? C9 C10 C11 118.8(3) . . ? C11 C10 H10 121(2) . . ? C10 C11 H11 119.2 . . ? C12 C11 C10 121.6(3) . . ? C12 C11 H11 119.2 . . ? C7 C12 C121 120.3(3) . . ? C11 C12 C7 119.5(3) . . ? C11 C12 C121 120.0(3) . . ? C2 C21 Y1 109.60(19) . . ? C22 C21 Y1 78.94(18) . . ? C22 C21 C2 119.5(3) . . ? C22 C21 C26 119.5(3) . . ? C26 C21 Y1 76.85(17) . . ? C26 C21 C2 120.7(3) . . ? C21 C22 Y1 72.10(17) . . ? C21 C22 C221 120.1(3) . . ? C23 C22 Y1 77.34(19) . . ? C23 C22 C21 118.9(3) . . ? C23 C22 C221 121.0(3) . . ? C221 C22 Y1 124.0(2) . . ? Y1 C23 H23 116(2) . . ? C22 C23 Y1 74.59(18) . . ? C22 C23 H23 115(2) . . ? C22 C23 C24 121.9(3) . . ? C24 C23 Y1 76.74(18) . . ? C24 C23 H23 123(2) . . ? C23 C24 Y1 75.44(18) . . ? C23 C24 C241 123.7(3) . . ? C25 C24 Y1 74.26(18) . . ? C25 C24 C23 118.1(3) . . ? C25 C24 C241 118.1(3) . . ? C241 C24 Y1 123.4(2) . . ? Y1 C25 H25 117(2) . . ? C24 C25 Y1 78.08(18) . . ? C24 C25 H25 118(2) . . ? C24 C25 C26 122.7(3) . . ? C26 C25 Y1 73.87(17) . . ? C26 C25 H25 120(2) . . ? C21 C26 Y1 73.73(17) . . ? C21 C26 C261 120.5(3) . . ? C25 C26 Y1 77.93(18) . . ? C25 C26 C21 118.8(3) . . ? C25 C26 C261 120.7(3) . . ? C261 C26 Y1 120.0(2) . . ? H45A C45 H45B 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C51 C45 H45A 109.5 . . ? C51 C45 H45B 109.5 . . ? C51 C45 H45C 109.5 . . ? C47 C46 H46 108.0 . . ? C47 C46 C49 111.8(3) . . ? C47 C46 C124 110.9(4) . . ? C49 C46 H46 108.0 . . ? C124 C46 H46 108.0 . . ? C124 C46 C49 110.1(3) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47B 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C121 C48 C126 122.1(3) . . ? C125 C48 C121 119.0(3) . . ? C125 C48 C126 118.8(3) . . ? C123 C49 C46 121.2(3) . . ? C123 C49 C125 117.6(3) . . ? C125 C49 C46 121.0(3) . . ? C121 C50 C51 121.2(3) . . ? C123 C50 C51 119.7(3) . . ? C123 C50 C121 118.9(3) . . ? C45 C51 H51 108.0 . . ? C50 C51 C45 113.9(3) . . ? C50 C51 H51 108.0 . . ? C50 C51 C122 109.8(3) . . ? C122 C51 C45 109.1(3) . . ? C122 C51 H51 108.0 . . ? C62 C61 C6 119.1(3) . . ? C66 C61 C6 121.6(3) . . ? C66 C61 C62 118.7(3) . . ? C61 C62 C621 123.0(3) . . ? C63 C62 C61 118.1(3) . . ? C63 C62 C621 118.8(3) . . ? C62 C63 H63 118.3 . . ? C64 C63 C62 123.4(4) . . ? C64 C63 H63 118.3 . . ? C63 C64 C65 117.7(3) . . ? C63 C64 C641 134.5(6) . . ? C63 C64 C642 108.6(6) . . ? C65 C64 C641 107.9(6) . . ? C65 C64 C642 133.5(6) . . ? C64 C65 H65 118.8 . . ? C64 C65 C66 122.3(4) . . ? C66 C65 H65 118.8 . . ? C61 C66 C661 122.7(3) . . ? C65 C66 C61 119.7(4) . . ? C65 C66 C661 117.6(4) . . ? C82 C81 C8 119.8(3) . . ? C86 C81 C8 121.4(3) . . ? C86 C81 C82 118.4(3) . . ? C81 C82 C821 121.0(3) . . ? C83 C82 C81 119.2(3) . . ? C83 C82 C821 119.5(3) . . ? C82 C83 H83 117.3(18) . . ? C84 C83 C82 122.4(3) . . ? C84 C83 H83 120.3(18) . . ? C83 C84 C841 123.2(3) . . ? C85 C84 C83 117.1(3) . . ? C85 C84 C841 119.6(3) . . ? C84 C85 H85 116(2) . . ? C86 C85 C84 122.6(3) . . ? C86 C85 H85 121(2) . . ? C81 C86 C861 121.8(3) . . ? C85 C86 C81 120.3(3) . . ? C85 C86 C861 117.8(3) . . ? C48 C121 C12 118.7(3) . . ? C48 C121 C50 119.6(3) . . ? C50 C121 C12 121.6(3) . . ? C51 C122 H12A 109.5 . . ? C51 C122 H12B 109.5 . . ? C51 C122 H12C 109.5 . . ? H12A C122 H12B 109.5 . . ? H12A C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? C49 C123 C50 122.5(3) . . ? C49 C123 H123 118.7 . . ? C50 C123 H123 118.7 . . ? C46 C124 H12D 109.5 . . ? C46 C124 H12E 109.5 . . ? C46 C124 H12F 109.5 . . ? H12D C124 H12E 109.5 . . ? H12D C124 H12F 109.5 . . ? H12E C124 H12F 109.5 . . ? C48 C125 C49 122.2(3) . . ? C48 C125 H125 118.9 . . ? C49 C125 H125 118.9 . . ? C1A C126 H126 107.6 . . ? C1B C126 C1A 112.0(3) . . ? C1B C126 H126 107.6 . . ? C48 C126 C1A 111.9(3) . . ? C48 C126 C1B 109.9(3) . . ? C48 C126 H126 107.6 . . ? C22 C221 H221 107.9 . . ? C22 C221 C223 108.5(3) . . ? C222 C221 C22 114.7(3) . . ? C222 C221 H221 107.9 . . ? C222 C221 C223 109.6(3) . . ? C223 C221 H221 107.9 . . ? C221 C222 H22A 109.5 . . ? C221 C222 H22B 109.5 . . ? C221 C222 H22C 109.5 . . ? H22A C222 H22B 109.5 . . ? H22A C222 H22C 109.5 . . ? H22B C222 H22C 109.5 . . ? C221 C223 H22D 109.5 . . ? C221 C223 H22E 109.5 . . ? C221 C223 H22F 109.5 . . ? H22D C223 H22E 109.5 . . ? H22D C223 H22F 109.5 . . ? H22E C223 H22F 109.5 . . ? C24 C241 H241 107.6 . . ? C24 C241 C242 108.2(3) . . ? C242 C241 H241 107.6 . . ? C243 C241 C24 114.5(3) . . ? C243 C241 H241 107.6 . . ? C243 C241 C242 111.2(3) . . ? C241 C242 H24A 109.5 . . ? C241 C242 H24B 109.5 . . ? C241 C242 H24C 109.5 . . ? H24A C242 H24B 109.5 . . ? H24A C242 H24C 109.5 . . ? H24B C242 H24C 109.5 . . ? C241 C243 H24D 109.5 . . ? C241 C243 H24E 109.5 . . ? C241 C243 H24F 109.5 . . ? H24D C243 H24E 109.5 . . ? H24D C243 H24F 109.5 . . ? H24E C243 H24F 109.5 . . ? C26 C261 H261 108.0 . . ? C26 C261 C262 109.3(3) . . ? C26 C261 C263 113.0(3) . . ? C262 C261 H261 108.0 . . ? C262 C261 C263 110.5(3) . . ? C263 C261 H261 108.0 . . ? C261 C262 H26A 109.5 . . ? C261 C262 H26B 109.5 . . ? C261 C262 H26C 109.5 . . ? H26A C262 H26B 109.5 . . ? H26A C262 H26C 109.5 . . ? H26B C262 H26C 109.5 . . ? C261 C263 H26D 109.5 . . ? C261 C263 H26E 109.5 . . ? C261 C263 H26F 109.5 . . ? H26D C263 H26E 109.5 . . ? H26D C263 H26F 109.5 . . ? H26E C263 H26F 109.5 . . ? C62 C621 H621 108.0 . . ? C62 C621 C622 112.3(3) . . ? C62 C621 C623 111.2(3) . . ? C622 C621 H621 108.0 . . ? C622 C621 C623 109.3(3) . . ? C623 C621 H621 108.0 . . ? C621 C622 H62A 109.5 . . ? C621 C622 H62B 109.5 . . ? C621 C622 H62C 109.5 . . ? H62A C622 H62B 109.5 . . ? H62A C622 H62C 109.5 . . ? H62B C622 H62C 109.5 . . ? C621 C623 H62D 109.5 . . ? C621 C623 H62E 109.5 . . ? C621 C623 H62F 109.5 . . ? H62D C623 H62E 109.5 . . ? H62D C623 H62F 109.5 . . ? H62E C623 H62F 109.5 . . ? C64 C641 H641 109.7 . . ? C644 C641 C64 110.4(7) . . ? C644 C641 H641 109.7 . . ? C646 C641 C64 106.9(9) . . ? C646 C641 H641 109.7 . . ? C646 C641 C644 110.5(8) . . ? C64 C642 H642 107.5 . . ? C643 C642 C64 106.0(9) . . ? C643 C642 H642 107.5 . . ? C645 C642 C64 115.0(8) . . ? C645 C642 H642 107.5 . . ? C645 C642 C643 113.0(11) . . ? C642 C643 H64A 109.5 . . ? C642 C643 H64B 109.5 . . ? C642 C643 H64C 109.5 . . ? H64A C643 H64B 109.5 . . ? H64A C643 H64C 109.5 . . ? H64B C643 H64C 109.5 . . ? C641 C644 H64D 109.5 . . ? C641 C644 H64E 109.5 . . ? C641 C644 H64F 109.5 . . ? H64D C644 H64E 109.5 . . ? H64D C644 H64F 109.5 . . ? H64E C644 H64F 109.5 . . ? C642 C645 H64G 109.5 . . ? C642 C645 H64H 109.5 . . ? C642 C645 H64I 109.5 . . ? H64G C645 H64H 109.5 . . ? H64G C645 H64I 109.5 . . ? H64H C645 H64I 109.5 . . ? C641 C646 H64J 109.5 . . ? C641 C646 H64K 109.5 . . ? C641 C646 H64L 109.5 . . ? H64J C646 H64K 109.5 . . ? H64J C646 H64L 109.5 . . ? H64K C646 H64L 109.5 . . ? C66 C661 H661 108.1 . . ? C66 C661 C662 112.9(3) . . ? C66 C661 C663 110.9(4) . . ? C662 C661 H661 108.1 . . ? C662 C661 C663 108.7(3) . . ? C663 C661 H661 108.1 . . ? C661 C662 H66A 109.5 . . ? C661 C662 H66B 109.5 . . ? C661 C662 H66C 109.5 . . ? H66A C662 H66B 109.5 . . ? H66A C662 H66C 109.5 . . ? H66B C662 H66C 109.5 . . ? C661 C663 H66D 109.5 . . ? C661 C663 H66E 109.5 . . ? C661 C663 H66F 109.5 . . ? H66D C663 H66E 109.5 . . ? H66D C663 H66F 109.5 . . ? H66E C663 H66F 109.5 . . ? C82 C821 H821 107.7 . . ? C82 C821 C823 114.3(3) . . ? C822 C821 C82 111.0(3) . . ? C822 C821 H821 107.7 . . ? C822 C821 C823 108.3(3) . . ? C823 C821 H821 107.7 . . ? C821 C822 H82A 109.5 . . ? C821 C822 H82B 109.5 . . ? C821 C822 H82C 109.5 . . ? H82A C822 H82B 109.5 . . ? H82A C822 H82C 109.5 . . ? H82B C822 H82C 109.5 . . ? C821 C823 H82D 109.5 . . ? C821 C823 H82E 109.5 . . ? C821 C823 H82F 109.5 . . ? H82D C823 H82E 109.5 . . ? H82D C823 H82F 109.5 . . ? H82E C823 H82F 109.5 . . ? C84 C841 H841 107.4 . . ? C84 C841 C842 111.0(3) . . ? C84 C841 C843 114.1(3) . . ? C842 C841 H841 107.4 . . ? C843 C841 H841 107.4 . . ? C843 C841 C842 109.3(3) . . ? C841 C842 H84A 109.5 . . ? C841 C842 H84B 109.5 . . ? C841 C842 H84C 109.5 . . ? H84A C842 H84B 109.5 . . ? H84A C842 H84C 109.5 . . ? H84B C842 H84C 109.5 . . ? C841 C843 H84D 109.5 . . ? C841 C843 H84E 109.5 . . ? C841 C843 H84F 109.5 . . ? H84D C843 H84E 109.5 . . ? H84D C843 H84F 109.5 . . ? H84E C843 H84F 109.5 . . ? C86 C861 H861 108.0 . . ? C862 C861 C86 110.5(3) . . ? C862 C861 H861 108.0 . . ? C863 C861 C86 112.1(3) . . ? C863 C861 H861 108.0 . . ? C863 C861 C862 110.2(3) . . ? C861 C862 H86A 109(3) . . ? C861 C862 H86B 111(3) . . ? C861 C862 H86C 109(2) . . ? H86A C862 H86B 104(4) . . ? H86A C862 H86C 115(4) . . ? H86B C862 H86C 108(4) . . ? C861 C863 H86D 109.5 . . ? C861 C863 H86E 109.5 . . ? C861 C863 H86F 109.5 . . ? H86D C863 H86E 109.5 . . ? H86D C863 H86F 109.5 . . ? H86E C863 H86F 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C14 C13 H13A 109.6 . . ? C14 C13 H13B 108.9 . . ? C14 C13 H13C 109.9 . . ? C13 C14 H14A 108.7 . . ? C13 C14 H14B 108.7 . . ? C13 C14 C15 114.3(15) . . ? H14A C14 H14B 107.6 . . ? C15 C14 H14A 108.7 . . ? C15 C14 H14B 108.7 . . ? C14 C15 H15A 107.7 . . ? C14 C15 H15B 107.7 . . ? H15A C15 H15B 107.1 . . ? C16 C15 C14 118.6(13) . . ? C16 C15 H15A 107.7 . . ? C16 C15 H15B 107.7 . . ? C15 C16 H16A 108.5 . . ? C15 C16 H16B 108.5 . . ? C15 C16 C17 115.1(18) . . ? H16A C16 H16B 107.5 . . ? C17 C16 H16A 108.5 . . ? C17 C16 H16B 108.5 . . ? C16 C17 H17A 108.0 . . ? C16 C17 H17B 108.0 . . ? H17A C17 H17B 107.3 . . ? C18 C17 C16 117.0(19) . . ? C18 C17 H17A 108.0 . . ? C18 C17 H17B 108.0 . . ? C17 C18 H18A 108.4 . . ? C17 C18 H18B 111.9 . . ? C17 C18 H18C 108.1 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.4 . . ? H19B C19 H19C 109.4 . . ? C20 C19 H19A 108.6 . . ? C20 C19 H19B 107.9 . . ? C20 C19 H19C 111.9 . . ? C19 C20 H20A 111.1 . . ? C19 C20 H20B 111.1 . . ? H20A C20 H20B 109.1 . . ? C52 C20 C19 103(3) . . ? C52 C20 H20A 111.1 . . ? C52 C20 H20B 111.1 . . ? C20 C52 H52A 109.0 . . ? C20 C52 H52B 109.1 . . ? H52A C52 H52B 107.9 . . ? C53 C52 C20 101.4(18) . . ? C53 C52 H52A 149.5 . . ? C53 C52 H52B 58.3 . . ? H43A C43 H43B 109.1 . . ? C44 C43 H43A 111.1 . . ? C44 C43 H43B 111.1 . . ? C53 C43 H43A 111.1 . . ? C53 C43 H43B 111.1 . . ? C53 C43 C44 103(2) . . ? C43 C44 H44A 90.6 . . ? C43 C44 H44B 131.7 . . ? C43 C44 H44C 103.8 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.4 . . ? H44B C44 H44C 109.5 . . ? C52 C53 H52B 40.5 . . ? C52 C53 H53A 111.4 . . ? C52 C53 H53B 111.4 . . ? H52B C53 H53A 147.6 . . ? H52B C53 H53B 78.3 . . ? C43 C53 C52 102(2) . . ? C43 C53 H52B 93.6 . . ? C43 C53 H53A 111.4 . . ? C43 C53 H53B 111.4 . . ? H53A C53 H53B 109.3 . . ? C28 C27 C42 106(2) . . ? C27 C28 H28A 109.8 . . ? C27 C28 H28B 109.8 . . ? H28A C28 H28B 108.3 . . ? C29 C28 C27 109.3(19) . . ? C29 C28 H28A 109.8 . . ? C29 C28 H28B 109.8 . . ? C28 C29 H29A 108.9 . . ? C28 C29 H29B 109.1 . . ? C28 C29 C30 113.0(17) . . ? H29A C29 H29B 107.8 . . ? C30 C29 H29A 108.6 . . ? C30 C29 H29B 109.3 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? H41A C41 H41B 109.6 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C42 C41 H41A 85.7 . . ? C42 C41 H41B 129.6 . . ? C42 C41 H41C 109.6 . . ? C27 C42 H42A 109.6 . . ? C27 C42 H42B 109.6 . . ? C41 C42 C27 110(3) . . ? C41 C42 H42A 109.6 . . ? C41 C42 H42B 109.6 . . ? H42A C42 H42B 108.2 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? C31 C32 H32C 109.6 . . ? C31 C32 H32D 109.6 . . ? C31 C32 H32A 108.2 . . ? C31 C32 H32B 108.2 . . ? C31 C32 C33 110.5(9) . . ? C31 C32 C34 116.3(11) . . ? H32C C32 H32D 108.1 . . ? H32A C32 H32B 107.4 . . ? C33 C32 H32C 109.6 . . ? C33 C32 H32D 109.6 . . ? C34 C32 H32A 108.2 . . ? C34 C32 H32B 108.2 . . ? C32 C33 H33A 108.6 . . ? C32 C33 H33B 108.6 . . ? C32 C33 C35 114.5(13) . . ? H33A C33 H33B 107.6 . . ? C35 C33 H33A 108.6 . . ? C35 C33 H33B 108.6 . . ? C32 C34 H34A 108.2 . . ? C32 C34 H34B 108.2 . . ? C32 C34 C36 116.6(15) . . ? H34A C34 H34B 107.3 . . ? C36 C34 H34A 108.2 . . ? C36 C34 H34B 108.2 . . ? C33 C35 H35A 109.0 . . ? C33 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? C38 C35 C33 113.1(14) . . ? C38 C35 H35A 109.0 . . ? C38 C35 H35B 109.0 . . ? C37 C36 C34 120.7(19) . . ? C36 C37 H37A 113.6 . . ? C36 C37 H37B 113.6 . . ? C36 C37 C40 90(2) . . ? H37A C37 H37B 110.8 . . ? C40 C37 H37A 113.6 . . ? C40 C37 H37B 113.6 . . ? C35 C38 H38A 111.1 . . ? C35 C38 H38B 111.1 . . ? C35 C38 C39 103.4(16) . . ? H38A C38 H38B 109.0 . . ? C39 C38 H38A 111.1 . . ? C39 C38 H38B 111.1 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Y1 N1 C1 C2 -7.6(4) . . . . ? Y1 N1 C1 C6 170.1(2) . . . . ? Y1 N2 C7 C8 13.0(5) . . . . ? Y1 N2 C7 C12 -168.8(2) . . . . ? Y1 C21 C22 C23 -63.8(3) . . . . ? Y1 C21 C22 C221 119.5(3) . . . . ? Y1 C21 C26 C25 65.9(3) . . . . ? Y1 C21 C26 C261 -115.7(3) . . . . ? Y1 C22 C23 C24 -63.2(3) . . . . ? Y1 C22 C221 C222 -63.3(4) . . . . ? Y1 C22 C221 C223 173.8(2) . . . . ? Y1 C23 C24 C25 -62.9(3) . . . . ? Y1 C23 C24 C241 120.7(3) . . . . ? Y1 C24 C25 C26 -61.8(3) . . . . ? Y1 C24 C241 C242 -160.8(2) . . . . ? Y1 C24 C241 C243 74.6(4) . . . . ? Y1 C25 C26 C21 -63.6(2) . . . . ? Y1 C25 C26 C261 117.9(3) . . . . ? Y1 C26 C261 C262 -177.6(2) . . . . ? Y1 C26 C261 C263 58.9(3) . . . . ? N1 C1 C2 C3 -176.1(3) . . . . ? N1 C1 C2 C21 7.5(4) . . . . ? N1 C1 C6 C5 175.8(3) . . . . ? N1 C1 C6 C61 -10.0(5) . . . . ? N2 C7 C8 C9 -176.0(3) . . . . ? N2 C7 C8 C81 7.9(4) . . . . ? N2 C7 C12 C11 176.8(3) . . . . ? N2 C7 C12 C121 -7.0(4) . . . . ? C1 C2 C3 C4 -1.8(5) . . . . ? C1 C2 C21 Y1 -4.7(3) . . . . ? C1 C2 C21 C22 83.4(4) . . . . ? C1 C2 C21 C26 -90.7(4) . . . . ? C1 C6 C61 C62 -66.4(4) . . . . ? C1 C6 C61 C66 122.2(3) . . . . ? C2 C1 C6 C5 -6.5(4) . . . . ? C2 C1 C6 C61 167.7(3) . . . . ? C2 C3 C4 C5 -2.0(5) . . . . ? C2 C21 C22 Y1 -106.4(3) . . . . ? C2 C21 C22 C23 -170.2(3) . . . . ? C2 C21 C22 C221 13.1(5) . . . . ? C2 C21 C26 Y1 105.2(3) . . . . ? C2 C21 C26 C25 171.0(3) . . . . ? C2 C21 C26 C261 -10.5(4) . . . . ? C3 C2 C21 Y1 179.0(2) . . . . ? C3 C2 C21 C22 -92.9(4) . . . . ? C3 C2 C21 C26 92.9(4) . . . . ? C3 C4 C5 C6 1.3(5) . . . . ? C4 C5 C6 C1 3.0(5) . . . . ? C4 C5 C6 C61 -171.6(3) . . . . ? C5 C6 C61 C62 107.9(3) . . . . ? C5 C6 C61 C66 -63.5(4) . . . . ? C6 C1 C2 C3 6.0(4) . . . . ? C6 C1 C2 C21 -170.3(3) . . . . ? C6 C61 C62 C63 -170.5(3) . . . . ? C6 C61 C62 C621 6.8(5) . . . . ? C6 C61 C66 C65 169.8(3) . . . . ? C6 C61 C66 C661 -8.4(5) . . . . ? C7 C8 C9 C10 -2.0(5) . . . . ? C7 C8 C81 C82 71.0(4) . . . . ? C7 C8 C81 C86 -115.9(3) . . . . ? C7 C12 C121 C48 -75.7(4) . . . . ? C7 C12 C121 C50 107.5(3) . . . . ? C8 C7 C12 C11 -5.0(4) . . . . ? C8 C7 C12 C121 171.2(3) . . . . ? C8 C9 C10 C11 -2.7(5) . . . . ? C8 C81 C82 C83 173.7(3) . . . . ? C8 C81 C82 C821 -0.1(4) . . . . ? C8 C81 C86 C85 -172.0(3) . . . . ? C8 C81 C86 C861 5.4(4) . . . . ? C9 C8 C81 C82 -105.1(3) . . . . ? C9 C8 C81 C86 67.9(4) . . . . ? C9 C10 C11 C12 3.5(5) . . . . ? C10 C11 C12 C7 0.4(5) . . . . ? C10 C11 C12 C121 -175.9(3) . . . . ? C11 C12 C121 C48 100.5(3) . . . . ? C11 C12 C121 C50 -76.3(4) . . . . ? C12 C7 C8 C9 5.8(4) . . . . ? C12 C7 C8 C81 -170.4(3) . . . . ? C21 C2 C3 C4 174.4(3) . . . . ? C21 C22 C23 Y1 61.1(3) . . . . ? C21 C22 C23 C24 -2.1(5) . . . . ? C21 C22 C221 C222 -151.1(3) . . . . ? C21 C22 C221 C223 85.9(4) . . . . ? C21 C26 C261 C262 -89.6(4) . . . . ? C21 C26 C261 C263 146.9(3) . . . . ? C22 C21 C26 Y1 -69.0(3) . . . . ? C22 C21 C26 C25 -3.1(4) . . . . ? C22 C21 C26 C261 175.3(3) . . . . ? C22 C23 C24 Y1 62.1(3) . . . . ? C22 C23 C24 C25 -0.8(5) . . . . ? C22 C23 C24 C241 -177.2(3) . . . . ? C23 C22 C221 C222 32.3(5) . . . . ? C23 C22 C221 C223 -90.7(4) . . . . ? C23 C24 C25 Y1 63.5(3) . . . . ? C23 C24 C25 C26 1.7(5) . . . . ? C23 C24 C241 C242 104.7(4) . . . . ? C23 C24 C241 C243 -19.9(5) . . . . ? C24 C25 C26 Y1 63.8(3) . . . . ? C24 C25 C26 C21 0.2(5) . . . . ? C24 C25 C26 C261 -178.3(3) . . . . ? C25 C24 C241 C242 -71.7(4) . . . . ? C25 C24 C241 C243 163.7(3) . . . . ? C25 C26 C261 C262 88.9(4) . . . . ? C25 C26 C261 C263 -34.6(4) . . . . ? C26 C21 C22 Y1 67.8(3) . . . . ? C26 C21 C22 C23 4.0(5) . . . . ? C26 C21 C22 C221 -172.6(3) . . . . ? C46 C49 C123 C50 -173.8(3) . . . . ? C46 C49 C125 C48 172.4(3) . . . . ? C47 C46 C49 C123 -117.1(4) . . . . ? C47 C46 C49 C125 67.8(5) . . . . ? C51 C50 C121 C12 0.5(4) . . . . ? C51 C50 C121 C48 -176.3(3) . . . . ? C51 C50 C123 C49 175.7(3) . . . . ? C61 C62 C63 C64 0.8(5) . . . . ? C61 C62 C621 C622 119.7(3) . . . . ? C61 C62 C621 C623 -117.5(4) . . . . ? C61 C66 C661 C662 -128.7(4) . . . . ? C61 C66 C661 C663 108.9(4) . . . . ? C62 C61 C66 C65 -1.6(5) . . . . ? C62 C61 C66 C661 -179.8(3) . . . . ? C62 C63 C64 C65 -2.1(6) . . . . ? C62 C63 C64 C641 178.7(6) . . . . ? C62 C63 C64 C642 173.3(5) . . . . ? C63 C62 C621 C622 -63.1(4) . . . . ? C63 C62 C621 C623 59.8(4) . . . . ? C63 C64 C65 C66 1.7(6) . . . . ? C63 C64 C641 C644 -111.1(8) . . . . ? C63 C64 C641 C646 9.1(11) . . . . ? C63 C64 C642 C643 161.8(7) . . . . ? C63 C64 C642 C645 -72.6(12) . . . . ? C64 C65 C66 C61 0.2(6) . . . . ? C64 C65 C66 C661 178.5(4) . . . . ? C65 C64 C641 C644 69.7(9) . . . . ? C65 C64 C641 C646 -170.1(6) . . . . ? C65 C64 C642 C643 -23.8(11) . . . . ? C65 C64 C642 C645 101.9(12) . . . . ? C65 C66 C661 C662 53.0(5) . . . . ? C65 C66 C661 C663 -69.3(5) . . . . ? C66 C61 C62 C63 1.1(5) . . . . ? C66 C61 C62 C621 178.4(3) . . . . ? C81 C8 C9 C10 174.2(3) . . . . ? C81 C82 C83 C84 -2.4(5) . . . . ? C81 C82 C821 C822 72.5(4) . . . . ? C81 C82 C821 C823 -164.7(3) . . . . ? C81 C86 C861 C862 -106.3(4) . . . . ? C81 C86 C861 C863 130.3(3) . . . . ? C82 C81 C86 C85 1.2(4) . . . . ? C82 C81 C86 C861 178.5(3) . . . . ? C82 C83 C84 C85 2.7(5) . . . . ? C82 C83 C84 C841 -176.4(3) . . . . ? C83 C82 C821 C822 -101.2(3) . . . . ? C83 C82 C821 C823 21.6(4) . . . . ? C83 C84 C85 C86 -1.0(5) . . . . ? C83 C84 C841 C842 116.9(3) . . . . ? C83 C84 C841 C843 -7.1(5) . . . . ? C84 C85 C86 C81 -0.9(5) . . . . ? C84 C85 C86 C861 -178.3(3) . . . . ? C85 C84 C841 C842 -62.2(4) . . . . ? C85 C84 C841 C843 173.8(3) . . . . ? C85 C86 C861 C862 71.1(4) . . . . ? C85 C86 C861 C863 -52.3(4) . . . . ? C86 C81 C82 C83 0.4(4) . . . . ? C86 C81 C82 C821 -173.3(3) . . . . ? C121 C48 C125 C49 2.2(5) . . . . ? C121 C48 C126 C1A 126.6(3) . . . . ? C121 C48 C126 C1B -108.4(4) . . . . ? C121 C50 C51 C45 -139.1(3) . . . . ? C121 C50 C51 C122 98.2(3) . . . . ? C121 C50 C123 C49 0.4(5) . . . . ? C123 C49 C125 C48 -2.9(5) . . . . ? C123 C50 C51 C45 45.8(4) . . . . ? C123 C50 C51 C122 -76.9(4) . . . . ? C123 C50 C121 C12 175.6(3) . . . . ? C123 C50 C121 C48 -1.2(4) . . . . ? C124 C46 C49 C123 119.2(4) . . . . ? C124 C46 C49 C125 -55.9(5) . . . . ? C125 C48 C121 C12 -177.0(3) . . . . ? C125 C48 C121 C50 -0.1(5) . . . . ? C125 C48 C126 C1A -57.5(4) . . . . ? C125 C48 C126 C1B 67.5(4) . . . . ? C125 C49 C123 C50 1.6(5) . . . . ? C126 C48 C121 C12 -1.1(4) . . . . ? C126 C48 C121 C50 175.8(3) . . . . ? C126 C48 C125 C49 -173.8(3) . . . . ? C221 C22 C23 Y1 -122.3(3) . . . . ? C221 C22 C23 C24 174.5(3) . . . . ? C241 C24 C25 Y1 -119.9(3) . . . . ? C241 C24 C25 C26 178.3(3) . . . . ? C621 C62 C63 C64 -176.6(3) . . . . ? C641 C64 C65 C66 -179.0(5) . . . . ? C641 C64 C642 C643 -9.5(12) . . . . ? C641 C64 C642 C645 116(2) . . . . ? C642 C64 C65 C66 -172.4(7) . . . . ? C642 C64 C641 C644 -99.5(17) . . . . ? C642 C64 C641 C646 20.7(12) . . . . ? C821 C82 C83 C84 171.4(3) . . . . ? C841 C84 C85 C86 178.1(3) . . . . ? C13 C14 C15 C16 168(2) . . . . ? C14 C15 C16 C17 -162(4) . . . . ? C15 C16 C17 C18 175(3) . . . . ? C19 C20 C52 C53 -171(2) . . . . ? C20 C52 C53 C43 -173(3) . . . . ? C44 C43 C53 C52 146(3) . . . . ? C27 C28 C29 C30 22(4) . . . . ? C28 C27 C42 C41 -180(3) . . . . ? C42 C27 C28 C29 172(3) . . . . ? C31 C32 C33 C35 -149.8(13) . . . . ? C31 C32 C34 C36 154.1(13) . . . . ? C32 C33 C35 C38 177.2(14) . . . . ? C32 C34 C36 C37 -179.5(19) . . . . ? C33 C32 C34 C36 -114(2) . . . . ? C33 C35 C38 C39 73.1(19) . . . . ? C34 C32 C33 C35 103(2) . . . . ? C34 C36 C37 C40 -63(2) . . . . ? _shelx_res_file ; TITL cem_a.res in C2/c REM Old TITL CEM in C2/c REM SHELXT solution in C2/c: R1 0.221, Rweak 0.009, Alpha 0.043 REM 0.387 for 585 systematic absences, Orientation as input REM Formula found by SHELXT: C1A N8 I CELL 1.54178 39.603 16.4949 25.0473 90 91.017 90 ZERR 8 0.0005 0.0002 0.0003 0 0.001 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Cl N Y UNIT 672 1000 8 16 8 DFIX 1.52 C13 C14 C14 C15 C15 C16 C16 C17 C17 C18 SIMU 0.002 0.004 2 C27 > C30 C42 SIMU C19 C20 C43 C44 C52 C53 > C42 SADI 0.04 C27 C29 C42 C28 C28 C30 RIGU C27 > C30 C42 SADI C42 C27 C27 C28 C28 C29 C29 C30 SIMU 0.002 0.0004 2 C20 C43 C44 C52 C53 C41 SADI 0.04 C20 C53 C53 C44 C52 C43 C43 C41 RIGU C20 C43 C44 C52 C53 C41 SADI C20 C52 C52 C53 C53 C43 C43 C44 C44 C41 RIGU C13 > C18 SADI C13 C14 C14 C15 C15 C16 C16 C17 C17 C18 DANG 2.54 C14 C16 C15 C17 SIMU C13 > C18 SADI 0.04 C13 C15 C15 C17 C14 C16 C16 C18 DANG 2.53 C13 C15 C16 C18 SIMU C31 > C40 L.S. 16 PLAN 44 SIZE 0.101 0.12 0.196 CONF MORE -1 BOND $H fmap 2 acta OMIT -1 1 1 REM REM REM WGHT 0.086200 26.701200 FVAR 0.12377 Y1 5 0.327189 0.552541 0.446427 11.00000 0.03107 0.03836 = 0.02855 -0.00314 -0.00709 0.00213 H2 2 0.273159 0.567225 0.389952 11.00000 0.06364 CL1 3 0.304976 0.620512 0.528156 11.00000 0.04398 0.06948 = 0.04147 -0.01990 -0.00239 0.00355 N1 4 0.376118 0.488294 0.464766 11.00000 0.03144 0.04059 = 0.03078 0.00228 -0.00516 0.00405 H1 2 0.375607 0.447110 0.486939 11.00000 0.05643 N2 4 0.281422 0.520502 0.399026 11.00000 0.03510 0.03450 = 0.03149 -0.00266 -0.00753 -0.00059 C1 1 0.409054 0.505831 0.451011 11.00000 0.03240 0.03777 = 0.02816 -0.00332 -0.00731 -0.00061 C1A 1 0.203354 0.608813 0.464941 11.00000 0.06160 0.06468 = 0.02958 0.00002 -0.00751 0.01375 AFIX 137 H1AA 2 0.193072 0.661218 0.460943 11.00000 -1.50000 H1AB 2 0.227448 0.614779 0.467269 11.00000 -1.50000 H1AC 2 0.195425 0.583553 0.496892 11.00000 -1.50000 AFIX 0 C1B 1 0.156406 0.536101 0.414544 11.00000 0.05433 0.06003 = 0.04631 0.00351 0.00667 0.00206 H1BA 2 0.147685 0.509957 0.449020 11.00000 -1.50000 H1BB 2 0.150304 0.502014 0.384404 11.00000 -1.50000 H1BC 2 0.144856 0.588062 0.412754 11.00000 0.05562 C2 1 0.414333 0.569999 0.414498 11.00000 0.03464 0.04053 = 0.03145 -0.00060 -0.00826 0.00084 C3 1 0.446102 0.588801 0.395991 11.00000 0.03667 0.04961 = 0.03653 0.00580 -0.00623 -0.00385 AFIX 43 H3 2 0.448655 0.630322 0.371270 11.00000 -1.20000 AFIX 0 C4 1 0.474025 0.546116 0.414107 11.00000 0.03096 0.05365 = 0.03926 0.00474 -0.00357 -0.00319 AFIX 43 H4 2 0.495359 0.557298 0.401031 11.00000 -1.20000 AFIX 0 C5 1 0.469610 0.486407 0.452091 11.00000 0.03179 0.04885 = 0.03517 -0.00017 -0.00528 0.00718 H5 2 0.488986 0.457689 0.467718 11.00000 0.04330 C6 1 0.438202 0.465961 0.472301 11.00000 0.03373 0.04123 = 0.02762 -0.00095 -0.00501 0.00265 C7 1 0.263002 0.456678 0.377655 11.00000 0.03664 0.03562 = 0.02424 -0.00299 -0.00001 -0.00305 C8 1 0.270339 0.376653 0.394412 11.00000 0.03756 0.03696 = 0.02535 -0.00006 -0.00096 -0.00190 C9 1 0.253103 0.311828 0.370203 11.00000 0.04853 0.03498 = 0.03011 0.00070 -0.00239 -0.00417 H9 2 0.258224 0.253071 0.381563 11.00000 -1.20000 C10 1 0.228347 0.324145 0.331443 11.00000 0.05447 0.03927 = 0.02908 -0.00178 -0.00506 -0.01237 H10 2 0.216293 0.276890 0.315497 11.00000 -1.20000 C11 1 0.219491 0.403170 0.317881 11.00000 0.04443 0.04622 = 0.02257 -0.00013 -0.00881 -0.01011 AFIX 43 H11 2 0.202014 0.411835 0.293252 11.00000 -1.20000 AFIX 0 C12 1 0.236088 0.469430 0.340189 11.00000 0.03878 0.04070 = 0.02313 0.00140 -0.00255 -0.00319 C21 1 0.384065 0.619189 0.399811 11.00000 0.03351 0.03762 = 0.03629 0.00610 -0.00813 -0.00229 C22 1 0.374093 0.683369 0.433593 11.00000 0.03826 0.03457 = 0.04865 0.00173 -0.01321 -0.00349 C23 1 0.342877 0.720958 0.423983 11.00000 0.03964 0.03582 = 0.05549 -0.00102 -0.01271 -0.00013 H23 2 0.336066 0.759748 0.451029 11.00000 0.05194 C24 1 0.321824 0.698624 0.380971 11.00000 0.03817 0.03600 = 0.04817 0.00894 -0.01054 -0.00111 C25 1 0.332867 0.638118 0.347106 11.00000 0.03926 0.04205 = 0.03649 0.00743 -0.00956 -0.00295 H25 2 0.317384 0.620969 0.317653 11.00000 0.05618 C26 1 0.363317 0.597820 0.355019 11.00000 0.03548 0.04153 = 0.03312 0.00798 -0.00785 -0.00505 C45 1 0.276520 0.600152 0.207004 11.00000 0.04502 0.05477 = 0.03275 0.00822 -0.00468 -0.00092 AFIX 137 H45A 2 0.264783 0.639413 0.185315 11.00000 -1.50000 H45B 2 0.290340 0.566851 0.184792 11.00000 -1.50000 H45C 2 0.290525 0.627570 0.232946 11.00000 -1.50000 AFIX 0 C46 1 0.180279 0.787662 0.287099 11.00000 0.05827 0.05860 = 0.04014 0.00892 -0.00330 0.01355 AFIX 13 H46 2 0.185610 0.799549 0.249852 11.00000 -1.20000 AFIX 0 C47 1 0.192760 0.857647 0.321032 11.00000 0.06457 0.07338 = 0.05201 0.00820 -0.01320 0.01562 AFIX 137 H47A 2 0.179982 0.905444 0.312299 11.00000 -1.50000 H47B 2 0.216213 0.867158 0.314266 11.00000 -1.50000 H47C 2 0.190013 0.844791 0.358082 11.00000 -1.50000 AFIX 0 C48 1 0.204345 0.594943 0.364585 11.00000 0.03941 0.04650 = 0.03002 0.00071 -0.00807 0.00090 C49 1 0.197714 0.708267 0.302544 11.00000 0.04404 0.05131 = 0.04055 0.00753 -0.00448 0.00424 C50 1 0.231233 0.590876 0.278123 11.00000 0.03841 0.04458 = 0.03136 0.00413 -0.00756 -0.00319 C51 1 0.250780 0.546749 0.235735 11.00000 0.04233 0.04570 = 0.03026 0.00618 -0.00152 0.00290 AFIX 13 H51 2 0.263105 0.502120 0.253032 11.00000 -1.20000 AFIX 0 C61 1 0.437891 0.408476 0.518737 11.00000 0.02946 0.04984 = 0.03681 0.00742 -0.00366 0.00264 C62 1 0.429854 0.438720 0.570357 11.00000 0.02972 0.06471 = 0.03499 0.00565 -0.00673 -0.00101 C63 1 0.434646 0.387287 0.614328 11.00000 0.03595 0.09191 = 0.03519 0.01744 -0.00814 -0.01110 AFIX 43 H63 2 0.429172 0.406617 0.647963 11.00000 -1.20000 AFIX 0 C64 1 0.446956 0.310138 0.610362 11.00000 0.03355 0.09432 = 0.06928 0.04671 -0.00940 -0.00064 C65 1 0.453906 0.281235 0.559924 11.00000 0.04112 0.06669 = 0.07944 0.03522 0.00356 0.01038 AFIX 43 H65 2 0.461735 0.228384 0.556395 11.00000 -1.20000 AFIX 0 C66 1 0.449603 0.328410 0.514253 11.00000 0.03654 0.05761 = 0.05660 0.01626 0.00093 0.01053 C81 1 0.294523 0.360580 0.439667 11.00000 0.04126 0.03269 = 0.02829 0.00103 -0.00388 -0.00161 C82 1 0.285237 0.379750 0.492825 11.00000 0.04091 0.03595 = 0.02944 0.00189 -0.00455 -0.00181 C83 1 0.306701 0.356970 0.535278 11.00000 0.04344 0.04052 = 0.02851 0.00198 -0.00279 -0.00047 H83 2 0.299571 0.371029 0.571691 11.00000 0.02904 C84 1 0.336442 0.313312 0.527584 11.00000 0.03914 0.03976 = 0.03351 0.00477 -0.00382 -0.00449 C85 1 0.344929 0.295844 0.475230 11.00000 0.03621 0.03827 = 0.03684 0.00095 -0.00292 -0.00038 H85 2 0.365033 0.265932 0.470431 11.00000 0.04379 C86 1 0.324953 0.318841 0.431893 11.00000 0.03556 0.03546 = 0.03506 0.00284 -0.00012 -0.00416 C121 1 0.224248 0.553943 0.327342 11.00000 0.03613 0.04008 = 0.02831 0.00024 -0.00953 -0.00204 C122 1 0.226298 0.510276 0.194455 11.00000 0.05696 0.04606 = 0.03386 0.00460 -0.00257 -0.00501 AFIX 137 H12A 2 0.210995 0.474243 0.211931 11.00000 -1.50000 H12B 2 0.238771 0.480734 0.168315 11.00000 -1.50000 H12C 2 0.213751 0.552939 0.177188 11.00000 -1.50000 AFIX 0 C123 1 0.217562 0.667399 0.267029 11.00000 0.04354 0.05248 = 0.03449 0.01135 -0.00387 0.00353 AFIX 43 H123 2 0.222083 0.691525 0.234367 11.00000 -1.20000 AFIX 0 C124 1 0.142235 0.778540 0.290804 11.00000 0.06467 0.08482 = 0.06692 0.01997 -0.00568 0.02038 AFIX 137 H12D 2 0.134829 0.734260 0.268651 11.00000 -1.50000 H12E 2 0.131465 0.827635 0.278936 11.00000 -1.50000 H12F 2 0.136362 0.767958 0.327166 11.00000 -1.50000 AFIX 0 C125 1 0.191986 0.671548 0.351926 11.00000 0.04534 0.04995 = 0.03751 0.00031 -0.00366 0.00711 AFIX 43 H125 2 0.179486 0.699350 0.377127 11.00000 -1.20000 AFIX 0 C126 1 0.193980 0.556053 0.416689 11.00000 0.05000 0.04827 = 0.03290 0.00199 -0.00084 0.00837 AFIX 13 H126 2 0.206338 0.504825 0.420353 11.00000 -1.20000 AFIX 0 C221 1 0.397971 0.713574 0.477584 11.00000 0.04290 0.03878 = 0.06849 -0.01242 -0.02621 0.00202 AFIX 13 H221 2 0.411811 0.667657 0.489710 11.00000 -1.20000 AFIX 0 C222 1 0.380643 0.748782 0.525786 11.00000 0.05716 0.07075 = 0.07674 -0.03475 -0.02837 0.00612 AFIX 137 H22A 2 0.368446 0.796728 0.515431 11.00000 -1.50000 H22B 2 0.397277 0.762336 0.552669 11.00000 -1.50000 H22C 2 0.365224 0.709590 0.539802 11.00000 -1.50000 AFIX 0 C223 1 0.421480 0.776914 0.453820 11.00000 0.04495 0.04753 = 0.11984 -0.00978 -0.02104 -0.00376 AFIX 137 H22D 2 0.433799 0.753097 0.425120 11.00000 -1.50000 H22E 2 0.437037 0.795706 0.480922 11.00000 -1.50000 H22F 2 0.408382 0.821754 0.440482 11.00000 -1.50000 AFIX 0 C241 1 0.288392 0.740285 0.367463 11.00000 0.03765 0.03927 = 0.06118 0.00637 -0.01495 0.00282 AFIX 13 H241 2 0.272147 0.698051 0.357121 11.00000 -1.20000 AFIX 0 C242 1 0.293659 0.795175 0.318131 11.00000 0.05464 0.06216 = 0.06823 0.01937 -0.00647 0.01020 AFIX 137 H24A 2 0.308128 0.839688 0.327836 11.00000 -1.50000 H24B 2 0.272231 0.815642 0.305708 11.00000 -1.50000 H24C 2 0.303883 0.764214 0.290275 11.00000 -1.50000 AFIX 0 C243 1 0.273741 0.786543 0.412112 11.00000 0.05636 0.08133 = 0.06234 -0.01389 -0.01944 0.01911 AFIX 137 H24D 2 0.270302 0.750929 0.441838 11.00000 -1.50000 H24E 2 0.252500 0.809431 0.400828 11.00000 -1.50000 H24F 2 0.288923 0.829259 0.422619 11.00000 -1.50000 AFIX 0 C261 1 0.374745 0.533644 0.315910 11.00000 0.04354 0.06296 = 0.02672 0.00039 -0.00445 0.00559 AFIX 13 H261 2 0.389826 0.496203 0.335163 11.00000 -1.20000 AFIX 0 C262 1 0.394854 0.573729 0.271831 11.00000 0.06707 0.10524 = 0.03807 0.01071 0.00460 0.00253 AFIX 137 H26A 2 0.402470 0.533096 0.247387 11.00000 -1.50000 H26B 2 0.414000 0.601348 0.287268 11.00000 -1.50000 H26C 2 0.380760 0.611998 0.253066 11.00000 -1.50000 AFIX 0 C263 1 0.345466 0.484312 0.292039 11.00000 0.05552 0.06651 = 0.04214 -0.01139 -0.01497 0.01069 AFIX 137 H26D 2 0.332538 0.517720 0.267858 11.00000 -1.50000 H26E 2 0.331250 0.465724 0.320173 11.00000 -1.50000 H26F 2 0.354231 0.438529 0.273103 11.00000 -1.50000 AFIX 0 C621 1 0.417863 0.524792 0.579885 11.00000 0.04466 0.06735 = 0.03113 -0.00368 -0.00023 -0.00032 AFIX 13 H621 2 0.416652 0.552530 0.545304 11.00000 -1.20000 AFIX 0 C622 1 0.382819 0.527517 0.604198 11.00000 0.04945 0.08739 = 0.04383 -0.00312 -0.00130 0.00661 AFIX 137 H62A 2 0.383795 0.504665 0.639441 11.00000 -1.50000 H62B 2 0.367319 0.496850 0.582300 11.00000 -1.50000 H62C 2 0.375300 0.582750 0.606146 11.00000 -1.50000 AFIX 0 C623 1 0.442809 0.571313 0.615976 11.00000 0.05139 0.08608 = 0.05193 -0.01901 0.00094 -0.00736 AFIX 137 H62D 2 0.435407 0.626449 0.619471 11.00000 -1.50000 H62E 2 0.464806 0.570345 0.600490 11.00000 -1.50000 H62F 2 0.443834 0.546277 0.650567 11.00000 -1.50000 AFIX 0 PART 2 C641 1 0.455400 0.240930 0.651622 10.50000 0.04284 0.06012 = 0.04169 0.01156 -0.00871 -0.00449 AFIX 13 H641 2 0.444197 0.190601 0.640417 10.50000 -1.20000 AFIX 0 PART 1 C642 1 0.452839 0.275314 0.668457 10.50000 0.05371 0.06820 = 0.03791 0.01461 -0.00382 0.00268 AFIX 13 H642 2 0.432564 0.287174 0.688922 10.50000 -1.20000 AFIX 0 C643 1 0.455063 0.183990 0.662327 10.50000 0.11648 0.06781 = 0.06314 0.03432 -0.00381 0.01456 AFIX 137 H64A 2 0.435334 0.164536 0.643548 10.50000 -1.50000 H64B 2 0.456433 0.159234 0.696985 10.50000 -1.50000 H64C 2 0.474828 0.170404 0.642568 10.50000 -1.50000 AFIX 0 PART 2 C644 1 0.493832 0.227270 0.655720 10.50000 0.04715 0.08638 = 0.04349 0.02314 -0.00889 0.02216 AFIX 137 H64D 2 0.501972 0.209254 0.621851 10.50000 -1.50000 H64E 2 0.498687 0.186888 0.682367 10.50000 -1.50000 H64F 2 0.504791 0.277155 0.665495 10.50000 -1.50000 AFIX 0 PART 1 C645 1 0.482377 0.310614 0.698393 10.50000 0.12712 0.14902 = 0.09138 0.07481 -0.07063 -0.06030 AFIX 137 H64G 2 0.483507 0.287973 0.733687 10.50000 -1.50000 H64H 2 0.479790 0.368367 0.700723 10.50000 -1.50000 H64I 2 0.502787 0.298154 0.679976 10.50000 -1.50000 AFIX 0 PART 2 C646 1 0.442098 0.267575 0.703941 10.50000 0.06044 0.09171 = 0.04722 0.01858 -0.00669 0.01296 AFIX 137 H64J 2 0.451380 0.319639 0.713039 10.50000 -1.50000 H64K 2 0.448399 0.228903 0.730973 10.50000 -1.50000 H64L 2 0.417928 0.271378 0.701578 10.50000 -1.50000 AFIX 0 PART 0 C661 1 0.458961 0.290590 0.460915 11.00000 0.05844 0.04761 = 0.07149 0.00424 0.01078 0.01328 AFIX 13 H661 2 0.451752 0.327775 0.432405 11.00000 -1.20000 AFIX 0 C662 1 0.441739 0.208718 0.450943 11.00000 0.06854 0.04955 = 0.10478 0.00060 0.01403 0.01594 AFIX 137 H66A 2 0.450154 0.169785 0.476371 11.00000 -1.50000 H66B 2 0.446483 0.190486 0.415459 11.00000 -1.50000 H66C 2 0.417784 0.214561 0.454748 11.00000 -1.50000 AFIX 0 C663 1 0.497363 0.279219 0.457348 11.00000 0.05914 0.06114 = 0.11820 0.00551 0.02877 0.01449 AFIX 137 H66D 2 0.508450 0.330068 0.464019 11.00000 -1.50000 H66E 2 0.502852 0.260263 0.422319 11.00000 -1.50000 H66F 2 0.504779 0.240220 0.483478 11.00000 -1.50000 AFIX 0 C821 1 0.250912 0.416637 0.504511 11.00000 0.04453 0.04354 = 0.02599 0.00317 -0.00347 0.00426 AFIX 13 H821 2 0.246730 0.459861 0.478377 11.00000 -1.20000 AFIX 0 C822 1 0.222915 0.354169 0.497658 11.00000 0.04067 0.05475 = 0.03849 -0.00230 0.00138 -0.00276 AFIX 137 H82A 2 0.223189 0.332808 0.462016 11.00000 -1.50000 H82B 2 0.201485 0.379361 0.503835 11.00000 -1.50000 H82C 2 0.226404 0.310913 0.522799 11.00000 -1.50000 AFIX 0 C823 1 0.248258 0.454020 0.560373 11.00000 0.04964 0.05447 = 0.02762 -0.00101 -0.00005 0.00564 AFIX 137 H82D 2 0.248005 0.411619 0.586616 11.00000 -1.50000 H82E 2 0.227808 0.485032 0.562377 11.00000 -1.50000 H82F 2 0.267302 0.488799 0.567076 11.00000 -1.50000 AFIX 0 C841 1 0.359063 0.283815 0.573248 11.00000 0.03634 0.05236 = 0.03581 0.00871 -0.00453 -0.00196 AFIX 13 H841 2 0.381914 0.303808 0.566641 11.00000 -1.20000 AFIX 0 C842 1 0.360759 0.191035 0.574345 11.00000 0.05546 0.05557 = 0.05136 0.01471 -0.01286 0.00284 AFIX 137 H84A 2 0.338979 0.169558 0.582865 11.00000 -1.50000 H84B 2 0.377044 0.174010 0.600888 11.00000 -1.50000 H84C 2 0.367317 0.171403 0.539970 11.00000 -1.50000 AFIX 0 C843 1 0.348899 0.314731 0.627968 11.00000 0.04906 0.07168 = 0.03446 0.01033 -0.00524 0.00553 AFIX 137 H84D 2 0.348107 0.372896 0.627526 11.00000 -1.50000 H84E 2 0.365149 0.297026 0.654369 11.00000 -1.50000 H84F 2 0.327036 0.293755 0.636495 11.00000 -1.50000 AFIX 0 C861 1 0.336501 0.293944 0.375954 11.00000 0.04559 0.04757 = 0.03243 -0.00479 -0.00180 -0.00147 AFIX 13 H861 2 0.321997 0.321673 0.349631 11.00000 -1.20000 AFIX 0 C862 1 0.332191 0.202183 0.367821 11.00000 0.06380 0.05318 = 0.04282 -0.01324 0.00182 0.00030 H86A 2 0.348330 0.171248 0.394935 11.00000 -1.50000 H86B 2 0.339364 0.187365 0.335883 11.00000 -1.50000 H86C 2 0.303795 0.185618 0.370705 11.00000 -1.50000 C863 1 0.372825 0.318672 0.365893 11.00000 0.04809 0.06560 = 0.03713 -0.00232 0.00248 0.00256 AFIX 137 H86D 2 0.376193 0.373838 0.376978 11.00000 -1.50000 H86E 2 0.377359 0.313844 0.328504 11.00000 -1.50000 H86F 2 0.387855 0.283945 0.385845 11.00000 -1.50000 AFIX 0 PART -1 C13 1 0.439456 -0.016316 0.573873 10.50000 0.16542 0.23897 = 0.29859 -0.03728 -0.00509 -0.03494 AFIX 3 H13A 2 0.434546 0.002614 0.609133 10.50000 -1.50000 H13B 2 0.437836 -0.074366 0.572893 10.50000 -1.50000 H13C 2 0.423566 0.006644 0.548753 10.50000 -1.50000 AFIX 0 C14 1 0.475033 0.008389 0.559512 10.50000 0.17065 0.11937 = 0.24456 -0.03170 -0.02516 -0.00161 AFIX 23 H14A 2 0.490783 -0.017228 0.584351 10.50000 -1.20000 H14B 2 0.477223 0.066583 0.563937 10.50000 -1.20000 AFIX 0 C15 1 0.484872 -0.013772 0.502936 10.50000 0.11937 0.06350 = 0.23550 -0.01804 -0.04933 0.01109 AFIX 23 H15A 2 0.486906 -0.072313 0.501214 10.50000 -1.20000 H15B 2 0.466298 0.001479 0.479248 10.50000 -1.20000 AFIX 0 C16 1 0.516885 0.022278 0.480684 10.50000 0.18320 0.14165 = 0.30184 -0.03869 0.00608 -0.02725 AFIX 23 H16A 2 0.536083 -0.006490 0.496048 10.50000 -1.20000 H16B 2 0.518526 0.078325 0.492161 10.50000 -1.20000 AFIX 0 C17 1 0.519379 0.019665 0.420209 10.50000 0.24940 0.18262 = 0.29795 -0.03112 0.02156 -0.00256 AFIX 23 H17A 2 0.519571 -0.036737 0.409260 10.50000 -1.20000 H17B 2 0.499073 0.044000 0.405064 10.50000 -1.20000 AFIX 0 C18 1 0.549600 0.061269 0.395828 10.50000 0.23394 0.23165 = 0.37074 0.02712 0.03090 0.00947 AFIX 3 H18A 2 0.549501 0.049829 0.358248 10.50000 -1.50000 H18B 2 0.570500 0.043079 0.411708 10.50000 -1.50000 H18C 2 0.547280 0.118619 0.401238 10.50000 -1.50000 AFIX 0 C19 1 0.487221 0.010141 0.250217 10.25000 0.09125 0.07973 = 0.33209 0.00965 0.06389 0.00284 AFIX 3 H19A 2 0.504101 0.025731 0.276227 10.25000 -1.50000 H19B 2 0.497671 -0.018939 0.221717 10.25000 -1.50000 H19C 2 0.470791 -0.023999 0.266777 10.25000 -1.50000 AFIX 6 C20 1 0.470200 0.091906 0.225064 10.25000 0.11341 0.14288 = 0.18377 0.04145 0.06098 0.04331 AFIX 23 H20A 2 0.483788 0.113767 0.196617 10.25000 -1.20000 H20B 2 0.447585 0.081263 0.211300 10.25000 -1.20000 AFIX 5 C52 1 0.469483 0.149382 0.272521 10.25000 0.11288 0.14249 = 0.18300 0.04182 0.06121 0.04380 AFIX 3 H52A 2 0.481581 0.124770 0.302393 10.25000 -1.20000 H52B 2 0.446274 0.157412 0.282960 10.25000 -1.20000 AFIX 0 C43 1 0.451574 0.275849 0.292903 10.25000 0.11018 0.14104 = 0.18134 0.04348 0.06164 0.04546 AFIX 23 H43A 2 0.472493 0.269343 0.313181 10.25000 -1.20000 H43B 2 0.432721 0.271958 0.316969 10.25000 -1.20000 AFIX 0 C44 1 0.451026 0.352848 0.263972 10.25000 0.11012 0.14102 = 0.18130 0.04351 0.06162 0.04549 AFIX 3 H44A 2 0.426906 0.355448 0.266682 10.25000 -1.50000 H44B 2 0.457396 0.366618 0.228302 10.25000 -1.50000 H44C 2 0.461216 0.390428 0.288702 10.25000 -1.50000 AFIX 0 C53 1 0.448822 0.216450 0.250771 10.25000 0.11223 0.14210 = 0.18214 0.04265 0.06181 0.04448 AFIX 23 H53A 2 0.457897 0.236886 0.217667 10.25000 -1.20000 H53B 2 0.425569 0.199854 0.244731 10.25000 -1.20000 AFIX 0 PART -2 C27 1 0.505055 0.382916 0.247312 10.25000 0.05574 0.21168 = 0.11374 -0.02985 0.02267 -0.00199 C28 1 0.526469 0.425993 0.213226 10.25000 0.05341 0.21025 = 0.11207 -0.03002 0.02425 -0.00195 AFIX 23 H28A 2 0.513374 0.449357 0.183972 10.25000 -1.20000 H28B 2 0.537425 0.469760 0.232744 10.25000 -1.20000 AFIX 0 C29 1 0.549896 0.375176 0.193957 10.25000 0.05205 0.20906 = 0.11145 -0.03058 0.02499 -0.00164 AFIX 3 H29A 2 0.570636 0.381406 0.214747 10.25000 -1.20000 H29B 2 0.554606 0.390046 0.157367 10.25000 -1.20000 AFIX 0 C30 1 0.540051 0.294102 0.195707 10.25000 0.05232 0.20915 = 0.11298 -0.03094 0.02772 -0.00145 AFIX 137 H30A 2 0.547770 0.270371 0.228724 10.25000 -1.50000 H30B 2 0.549729 0.265402 0.166353 10.25000 -1.50000 H30C 2 0.515875 0.290695 0.193250 10.25000 -1.50000 AFIX 0 C41 1 0.462035 0.405052 0.306371 10.25000 0.11010 0.14098 = 0.18128 0.04350 0.06160 0.04553 AFIX 3 H41A 2 0.453435 0.458502 0.312761 10.25000 -1.50000 H41B 2 0.443615 0.368812 0.298731 10.25000 -1.50000 H41C 2 0.474255 0.386472 0.337491 10.25000 -1.50000 AFIX 0 C42 1 0.484036 0.442271 0.271883 10.25000 0.05740 0.21247 = 0.11439 -0.03042 0.02133 -0.00133 AFIX 23 H42A 2 0.497977 0.480915 0.291415 10.25000 -1.20000 H42B 2 0.471325 0.471544 0.244613 10.25000 -1.20000 AFIX 0 PART 0 C31 1 0.375832 1.010792 0.441483 11.00000 0.26852 0.10309 = 0.12067 0.02412 0.09505 0.02110 AFIX 137 H31A 2 0.360242 1.055294 0.439397 11.00000 -1.50000 H31B 2 0.391107 1.018759 0.471209 11.00000 -1.50000 H31C 2 0.363593 0.961149 0.446228 11.00000 -1.50000 AFIX 0 C32 1 0.394326 1.006627 0.393771 11.00000 0.13154 0.12815 = 0.09244 -0.01907 0.00481 0.00982 PART 2 AFIX 23 H32C 2 0.418257 1.002874 0.402339 10.50000 -1.20000 H32D 2 0.390586 1.055612 0.373071 10.50000 -1.20000 AFIX 23 PART 1 H32A 2 0.411520 0.965153 0.398113 10.50000 -1.20000 H32B 2 0.405850 1.057950 0.389045 10.50000 -1.20000 AFIX 0 PART 2 C33 1 0.383121 0.930953 0.359906 10.50000 0.13230 0.11478 = 0.08853 -0.00128 -0.00734 -0.01167 AFIX 23 H33A 2 0.364341 0.946523 0.336725 10.50000 -1.20000 H33B 2 0.375080 0.889390 0.383950 10.50000 -1.20000 AFIX 0 PART 1 C34 1 0.374839 0.989058 0.344854 10.50000 0.11419 0.11569 = 0.16077 -0.04990 -0.04016 0.02481 AFIX 23 H34A 2 0.352520 1.012450 0.348421 10.50000 -1.20000 H34B 2 0.372049 0.930768 0.342174 10.50000 -1.20000 AFIX 0 PART 2 C35 1 0.411824 0.893521 0.324529 10.50000 0.13423 0.15367 = 0.13049 -0.04035 0.02777 0.00419 AFIX 23 H35A 2 0.419094 0.933970 0.299080 10.50000 -1.20000 H35B 2 0.431068 0.880074 0.347336 10.50000 -1.20000 AFIX 0 PART 1 C36 1 0.390943 1.022253 0.287915 10.50000 0.16633 0.23924 = 0.08715 -0.04963 0.02176 -0.00667 C37 1 0.373502 1.008593 0.237706 10.50000 0.09941 0.23310 = 0.19379 0.00628 -0.03862 0.01702 AFIX 23 H37A 2 0.385472 1.029364 0.207145 10.50000 -1.20000 H37B 2 0.350270 1.027237 0.237270 10.50000 -1.20000 AFIX 0 PART 2 C38 1 0.400567 0.817611 0.294216 10.50000 0.18689 0.13241 = 0.09898 -0.02501 0.03397 0.01568 AFIX 23 H38A 2 0.388604 0.780675 0.317343 10.50000 -1.20000 H38B 2 0.419734 0.789615 0.279209 10.50000 -1.20000 AFIX 0 C39 1 0.376528 0.851744 0.248990 10.50000 0.14163 0.26225 = 0.16263 -0.13148 -0.01278 -0.03069 AFIX 137 H39A 2 0.389346 0.884350 0.224911 10.50000 -1.50000 H39B 2 0.359217 0.884269 0.264668 10.50000 -1.50000 H39C 2 0.366331 0.807470 0.229756 10.50000 -1.50000 AFIX 0 PART 1 C40 1 0.376851 0.922132 0.244706 10.50000 0.10978 0.12667 = 0.48826 0.05845 0.02549 0.01769 HKLF 4 REM cem_a.res in C2/c REM R1 = 0.0598 for 12491 Fo > 4sig(Fo) and 0.0765 for all 15940 data REM 1044 parameters refined using 287 restraints END WGHT 0.0857 26.7395 REM Highest difference peak 0.802, deepest hole -0.747, 1-sigma level 0.077 Q1 1 0.2082 0.8556 0.2813 11.00000 0.05 0.80 Q2 1 0.3032 0.5811 0.5488 11.00000 0.05 0.71 Q3 1 0.2639 0.7361 0.4408 11.00000 0.05 0.70 Q4 1 0.4185 0.1379 0.2715 11.00000 0.05 0.65 Q5 1 0.3503 0.5524 0.4501 11.00000 0.05 0.56 Q6 1 0.4628 0.2269 0.2693 11.00000 0.05 0.56 Q7 1 0.3753 0.9474 0.3031 11.00000 0.05 0.54 Q8 1 0.2923 0.8300 0.3714 11.00000 0.05 0.53 Q9 1 0.3002 0.5490 0.4407 11.00000 0.05 0.53 Q10 1 0.3884 1.0811 0.2382 11.00000 0.05 0.52 Q11 1 0.4259 0.2207 0.2488 11.00000 0.05 0.50 Q12 1 0.1515 0.8176 0.3259 11.00000 0.05 0.48 Q13 1 0.5463 0.2967 0.2320 11.00000 0.05 0.45 Q14 1 0.1905 0.7967 0.3224 11.00000 0.05 0.44 Q15 1 0.3778 0.9160 0.2207 11.00000 0.05 0.44 Q16 1 0.3925 0.9525 0.3002 11.00000 0.05 0.43 Q17 1 0.3268 0.4891 0.4476 11.00000 0.05 0.41 Q18 1 0.4317 0.1417 0.1686 11.00000 0.05 0.41 Q19 1 0.4371 0.1617 0.2236 11.00000 0.05 0.40 Q20 1 0.4366 0.1543 0.1773 11.00000 0.05 0.39 Q21 1 0.4265 0.1153 0.1990 11.00000 0.05 0.37 Q22 1 0.5591 0.1235 0.3583 11.00000 0.05 0.37 Q23 1 0.4825 0.5075 0.2728 11.00000 0.05 0.36 Q24 1 0.3148 0.5780 0.4893 11.00000 0.05 0.35 Q25 1 0.4231 0.0635 0.1816 11.00000 0.05 0.33 Q26 1 0.4801 0.0603 0.2919 11.00000 0.05 0.32 Q27 1 0.5646 0.0883 0.3464 11.00000 0.05 0.32 Q28 1 0.3177 0.5178 0.4789 11.00000 0.05 0.31 Q29 1 0.3808 0.8239 0.2473 11.00000 0.05 0.31 Q30 1 0.5000 0.4664 0.2500 10.50000 0.05 0.31 Q31 1 0.5183 -0.0520 0.1612 11.00000 0.05 0.31 Q32 1 0.3036 0.5200 0.4059 11.00000 0.05 0.30 Q33 1 0.5259 0.0064 0.3416 11.00000 0.05 0.30 Q34 1 0.3230 0.6174 0.4462 11.00000 0.05 0.30 Q35 1 0.4246 0.9977 0.4897 11.00000 0.05 0.30 Q36 1 0.4974 0.0220 0.3210 11.00000 0.05 0.30 Q37 1 0.4004 0.9932 0.2573 11.00000 0.05 0.29 Q38 1 0.2051 0.7158 0.3319 11.00000 0.05 0.29 Q39 1 0.3519 0.5014 0.4567 11.00000 0.05 0.28 Q40 1 0.3932 1.0150 0.2120 11.00000 0.05 0.28 Q41 1 0.5396 0.0761 0.3386 11.00000 0.05 0.28 Q42 1 0.5000 0.0660 0.2500 10.50000 0.05 0.27 Q43 1 0.5104 0.3576 0.2190 11.00000 0.05 0.27 Q44 1 0.3812 0.8802 0.2758 11.00000 0.05 0.27 ; _shelx_res_checksum 7531 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.838 _oxdiff_exptl_absorpt_empirical_full_min 0.573