#------------------------------------------------------------------------------ #$Date: 2024-10-20 01:10:19 +0300 (Sun, 20 Oct 2024) $ #$Revision: 295550 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/28/1572891.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1572891 loop_ _publ_author_name 'Pedussaut, Lucie' 'Mahieu, Nolwenn' 'Chartier, Camille' 'Rajeshkumar, Thayalan' 'Tricoire, Maxime' 'Douair, Iskander' 'Casaretto, Nicolas' 'Maron, Laurent' 'Danoun, Gr\'egory' 'Nocton, Gr\'egory' _publ_section_title ; The photo-isomerization of the cyclononatetraenyl ligand and related rare earth complexes ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC04767B _journal_year 2024 _chemical_formula_moiety 'C17 H17 Y' _chemical_formula_sum 'C17 H17 Y' _chemical_formula_weight 310.21 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2024-03-11 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2024-07-13 deposited with the CCDC. 2024-10-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.791(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.0169(6) _cell_length_b 8.7585(8) _cell_length_c 11.1560(9) _cell_measurement_reflns_used 11340 _cell_measurement_temperature 150 _cell_measurement_theta_max 28.73 _cell_measurement_theta_min 2.97 _cell_volume 671.15(10) _computing_cell_refinement ; X-Area Recipe 1.37.0.0 (STOE, 2021) ; _computing_data_collection ; X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022) ; _computing_data_reduction ; X-Area Integrate 2.5.3.0 (STOE, 2021) X-Area X-Red 2.3.0.0 (STOE, 2021) ; _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material ; STOE & Cie GmbH, X-Area, software package for collecting single-crystal or multi-domain crystal data on STOE area-detector diffractometers, for image processing, for the correction and scaling of reflection intensities and for outlier rejection, version 2.1, Darmstadt 2022 ; _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _diffrn_ambient_temperature 150 _diffrn_detector 'EIGER2 1M CDTE' _diffrn_detector_area_resol_mean 13.33 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_details ; 1414 frames, detector distance = 60 mm ; _diffrn_measurement_device 'Eulerian 4-circle diffractometer' _diffrn_measurement_device_type 'STOE STADIVARI' _diffrn_measurement_method 'rotation method, \w scans' _diffrn_radiation_collimation '1.2 0.6 mm diameter' _diffrn_radiation_monochromator 'Graded multilayer mirror' _diffrn_radiation_polarisn_norm 270 _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_unetI/netI 0.0344 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 6569 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.484 _diffrn_reflns_theta_min 2.981 _diffrn_source Axo_Mo _diffrn_source_current 1.000 _diffrn_source_power 0.050 _diffrn_source_voltage 50 _exptl_absorpt_coefficient_mu 8.645 _exptl_absorpt_correction_T_max 0.5377 _exptl_absorpt_correction_T_min 0.1133 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details ; STOE X-Red32, absorption correction by Gaussian integration, analogous to P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal Structure Analysis", published in F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard, Copenhagen (1970), 255 - 270 ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 3.070 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 632 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _refine_diff_density_max 3.297 _refine_diff_density_min -4.351 _refine_diff_density_rms 0.318 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.171 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 163 _refine_ls_number_reflns 1534 _refine_ls_number_restraints 166 _refine_ls_restrained_S_all 1.135 _refine_ls_R_factor_all 0.1367 _refine_ls_R_factor_gt 0.1254 _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^)+(0.0304P)^2^+46.9600P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2668 _refine_ls_wR_factor_ref 0.2712 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1314 _reflns_number_total 1534 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc04767b3.cif _cod_data_source_block 2-Y-cis _cod_database_code 1572891 _shelx_shelxl_version_number 2018/3 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2. Restrained distances C12-C11 \\sim C12-C13 \\sim C14-C13 \\sim C14-C15 \\sim C16-C15 \\sim C17-C16 \\sim C17-C9 \\sim C9-C10 ~ C11-C10 with sigma of 0.02 C5-C4 \\sim C5-C6 \\sim C7-C6 \\sim C8-C7 \\sim C1-C8 \\sim C2-C1 \\sim C3-C2 \\sim C4-C3 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints C13 \\sim C14 \\sim C10 \\sim C9 \\sim C15 \\sim C16 \\sim C12 \\sim C11 \\sim C17: within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A C5 \\sim C4 \\sim C6 \\sim C1 \\sim C7 \\sim C2 \\sim C8 \\sim C3: within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A 4.a Aromatic/amide H refined with riding coordinates: C13(H13), C14(H14), C10(H10), C9(H9), C15(H15), C16(H16), C12(H12), C11(H11), C17(H17), C5(H5), C4(H4), C6(H6), C1(H1), C7(H7), C2(H2), C8(H8), C3(H3) ; _shelx_res_file ; TITL LP197 in P21/n #14 lp197.res created by SHELXL-2018/3 at 16:18:59 on 11-Mar-2024 CELL 0.71073 7.0169 8.7585 11.156 90 101.791 90 ZERR 4 0.0006 0.0008 0.0009 0 0.006 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Y UNIT 68 68 4 SADI C12 C11 C12 C13 C14 C13 C14 C15 C16 C15 C17 C16 C17 C9 C9 C10 C11 C10 SIMU 0.004 0.008 2 C13 C14 C10 C9 C15 C16 C12 C11 C17 SADI C5 C4 C5 C6 C7 C6 C8 C7 C1 C8 C2 C1 C3 C2 C4 C3 SIMU 0.004 0.008 2 C5 C4 C6 C1 C7 C2 C8 C3 L.S. 10 PLAN 3 TEMP -123 CONF CONN 34 Y1 BOND MORE -1 BOND $H fmap 2 acta SHEL 20 0.77 REM REM REM WGHT 0.030400 46.960003 FVAR 0.40038 Y1 3 -0.028649 -0.018532 1.025541 11.00000 0.03929 0.02584 = 0.03862 0.00126 -0.00453 0.00619 PART -1 C13 1 -0.241378 -0.010339 0.783226 11.00000 0.04516 0.04353 = 0.03931 -0.01006 0.00227 0.00265 AFIX 43 H13 2 -0.321441 -0.090820 0.744140 11.00000 -1.20000 AFIX 0 C14 1 -0.076834 -0.006532 0.740770 11.00000 0.04774 0.04373 = 0.03869 -0.01267 0.00534 0.00482 AFIX 43 H14 2 -0.051942 -0.099684 0.703126 11.00000 -1.20000 AFIX 0 C10 1 -0.140611 0.262501 1.007342 11.00000 0.04135 0.04499 = 0.03726 -0.00573 0.01085 0.00185 AFIX 43 H10 2 -0.180631 0.318689 1.070744 11.00000 -1.20000 AFIX 0 C9 1 0.047602 0.301120 1.005654 11.00000 0.04145 0.04417 = 0.03638 -0.00683 0.01065 0.00188 AFIX 43 H9 2 0.118275 0.344602 1.079489 11.00000 -1.20000 AFIX 0 C15 1 0.060022 0.097766 0.739143 11.00000 0.04506 0.04504 = 0.03691 -0.01230 0.00835 0.00541 AFIX 43 H15 2 0.108994 0.087289 0.666224 11.00000 -1.20000 AFIX 0 C16 1 0.152566 0.213696 0.806755 11.00000 0.04145 0.04475 = 0.03606 -0.01141 0.00952 0.00519 AFIX 43 H16 2 0.248094 0.257361 0.767877 11.00000 -1.20000 AFIX 0 C12 1 -0.333701 0.061637 0.863361 11.00000 0.04161 0.04420 = 0.03890 -0.00700 0.00549 0.00269 AFIX 43 H12 2 -0.462696 0.024436 0.856296 11.00000 -1.20000 AFIX 0 C11 1 -0.292691 0.172751 0.951394 11.00000 0.04110 0.04473 = 0.03775 -0.00558 0.01032 0.00201 AFIX 43 H11 2 -0.405009 0.194200 0.983707 11.00000 -1.20000 AFIX 0 C17 1 0.149660 0.286996 0.914640 11.00000 0.04061 0.04371 = 0.03548 -0.00919 0.00958 0.00356 AFIX 43 H17 2 0.259797 0.352394 0.932900 11.00000 -1.20000 AFIX 0 C5 1 -0.158996 -0.234104 1.131302 11.00000 0.04896 0.04180 = 0.03556 -0.00634 0.00358 0.00333 AFIX 43 H5 2 -0.284000 -0.271512 1.136806 11.00000 -1.20000 AFIX 0 C4 1 -0.088760 -0.118727 1.217842 11.00000 0.05153 0.04324 = 0.03472 -0.00730 0.00400 0.00582 AFIX 43 H4 2 -0.179868 -0.090649 1.266289 11.00000 -1.20000 AFIX 0 C6 1 -0.081225 -0.304210 1.039174 11.00000 0.04779 0.03886 = 0.03454 -0.00846 0.00183 0.00196 AFIX 43 H6 2 -0.165893 -0.382062 1.000041 11.00000 -1.20000 AFIX 0 C1 1 0.336991 -0.096989 1.104908 11.00000 0.04643 0.03980 = 0.03212 -0.00840 0.00142 0.00296 AFIX 43 H1 2 0.466267 -0.067182 1.102331 11.00000 -1.20000 AFIX 0 C7 1 0.086819 -0.293565 0.986728 11.00000 0.04638 0.03758 = 0.03259 -0.00960 0.00172 0.00149 AFIX 43 H7 2 0.080092 -0.356277 0.916508 11.00000 -1.20000 AFIX 0 C2 1 0.259624 -0.019245 1.196279 11.00000 0.05114 0.04057 = 0.03429 -0.00885 -0.00119 0.00354 AFIX 43 H2 2 0.339929 0.063230 1.231382 11.00000 -1.20000 AFIX 0 C8 1 0.261287 -0.209372 1.017202 11.00000 0.04588 0.03857 = 0.03011 -0.00867 0.00337 0.00165 AFIX 43 H8 2 0.349786 -0.234392 0.966154 11.00000 -1.20000 AFIX 0 C3 1 0.090220 -0.035034 1.248210 11.00000 0.05451 0.04191 = 0.03510 -0.00933 0.00112 0.00640 AFIX 43 H3 2 0.098376 0.024387 1.320322 11.00000 -1.20000 AFIX 0 HKLF 4 REM LP197 in P21/n #14 REM wR2 = 0.2712, GooF = S = 1.171, Restrained GooF = 1.135 for all data REM R1 = 0.1254 for 1314 Fo > 4sig(Fo) and 0.1367 for all 1534 data REM 163 parameters refined using 166 restraints END WGHT 0.0303 46.9707 REM Highest difference peak 3.297, deepest hole -4.351, 1-sigma level 0.318 Q1 1 -0.0400 -0.1024 1.0235 11.00000 0.05 3.30 Q2 1 -0.1817 -0.0054 0.7544 11.00000 0.05 1.33 Q3 1 0.1574 -0.1718 1.0025 11.00000 0.05 1.22 ; _shelx_res_checksum 1253 _olex2_submission_special_instructions 'No special instructions were received' _stoe_detector_distance '60.0 mm' _stoe_detector_pixelsize_x '0.075 mm' _stoe_detector_pixelsize_y '0.075 mm' _stoe_detector_size_x '8.0 cm' _stoe_detector_size_y '7.7 cm' _stoe_evaluation_integration_a 10.0 _stoe_evaluation_integration_b 2.5 _stoe_evaluation_integration_ems 0.024 _stoe_evaluation_lana_bis_l_even_max - _stoe_evaluation_lana_bis_l_odd_max - _stoe_evaluation_lana_bos_l_even_max 6 _stoe_evaluation_lana_bos_l_odd_max 3 _stoe_evaluation_lana_completeness 93.0 _stoe_evaluation_lana_dxs_max_order 3 _stoe_evaluation_lana_dys_max_order 3 _stoe_evaluation_lana_fs_max_order 3 _stoe_evaluation_lana_max_2theta_available 57.7 _stoe_evaluation_lana_max_2theta_desired 57.7 _stoe_evaluation_lana_mean_redundancy 4.1 _stoe_evaluation_lana_number_refls_after_or 6711 _stoe_evaluation_lana_number_refls_outliers 926 _stoe_evaluation_lana_number_refls_total 7637 _stoe_evaluation_lana_number_refls_unique 1635 _stoe_evaluation_lana_number_refls_written 6711 _stoe_evaluation_lana_or_c1 0.050 _stoe_evaluation_lana_or_c2 0 _stoe_evaluation_lana_or_c3 0 _stoe_evaluation_lana_or_c4 1.0 _stoe_evaluation_lana_point_group 2/m _stoe_evaluation_lana_table ; #---------------------------------------------------------------------------- 2Theta 7.2 13.2 19.2 25.2 31.2 37.2 43.2 49.2 55.2 #---------------------------------------------------------------------------- 5.04 2.97 2.11 1.61 1.32 1.11 0.96 0.85 0.78 N(total) 108 354 397 706 1030 1377 1447 1532 686 7.7 8.8 5.1 5.0 5.0 4.9 4.3 3.6 2.2 Complet. [%%] 100.0 100.0 100.0 100.0 100.0 100.0 99.7 100.0 70.9 322.1 140.4 103.9 39.9 24.0 15.2 6.2 4.2 2.6 R(int) 0.020 0.036 0.032 0.044 0.045 0.056 0.106 0.132 0.176 #---------------------------------------------------------------------------- ; _stoe_measurement_identifier LP197 _stoe_measurement_max_exposure_per_frame '180.0 s' _stoe_measurement_mean_exposure_per_frame '180.0 s' _stoe_measurement_min_exposure_per_frame '180.0 s' _stoe_measurement_total_exposure_time '70.7 h' _stoe_measurement_total_frame_number 1414 _stoe_measurement_total_run_number 13 _stoe_measurement_tube_power '50.0 W' 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' 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 -0.0286(3) -0.0185(2) 1.02554(17) 0.0364(5) Uani 1 1 d . . . . . C13 C -0.241(4) -0.010(3) 0.783(2) 0.044(3) Uani 1 1 d D U . A -1 H13 H -0.321441 -0.090820 0.744140 0.052 Uiso 1 1 calc R U . A -1 C14 C -0.077(3) -0.007(3) 0.741(2) 0.044(3) Uani 1 1 d D U . A -1 H14 H -0.051942 -0.099684 0.703126 0.053 Uiso 1 1 calc R U . A -1 C10 C -0.141(3) 0.263(3) 1.007(2) 0.041(3) Uani 1 1 d D U . A -1 H10 H -0.180631 0.318689 1.070744 0.049 Uiso 1 1 calc R U . A -1 C9 C 0.048(3) 0.301(3) 1.0057(19) 0.040(3) Uani 1 1 d D U . A -1 H9 H 0.118275 0.344602 1.079489 0.048 Uiso 1 1 calc R U . A -1 C15 C 0.060(3) 0.098(2) 0.7391(19) 0.042(3) Uani 1 1 d D U . A -1 H15 H 0.108994 0.087289 0.666224 0.051 Uiso 1 1 calc R U . A -1 C16 C 0.153(3) 0.214(2) 0.8068(17) 0.041(3) Uani 1 1 d D U . A -1 H16 H 0.248094 0.257361 0.767877 0.049 Uiso 1 1 calc R U . A -1 C12 C -0.334(4) 0.062(2) 0.8634(19) 0.042(3) Uani 1 1 d D U . A -1 H12 H -0.462696 0.024436 0.856296 0.050 Uiso 1 1 calc R U . A -1 C11 C -0.293(3) 0.173(2) 0.9514(19) 0.041(3) Uani 1 1 d D U . A -1 H11 H -0.405009 0.194200 0.983707 0.049 Uiso 1 1 calc R U . A -1 C17 C 0.150(3) 0.287(2) 0.9146(16) 0.040(3) Uani 1 1 d D U . A -1 H17 H 0.259797 0.352394 0.932900 0.048 Uiso 1 1 calc R U . A -1 C5 C -0.159(3) -0.234(2) 1.1313(18) 0.043(3) Uani 1 1 d D U . B -1 H5 H -0.284000 -0.271512 1.136806 0.051 Uiso 1 1 calc R U . B -1 C4 C -0.089(3) -0.119(3) 1.2178(18) 0.044(3) Uani 1 1 d D U . B -1 H4 H -0.179868 -0.090649 1.266289 0.053 Uiso 1 1 calc R U . B -1 C6 C -0.081(3) -0.304(2) 1.0392(18) 0.041(3) Uani 1 1 d D U . B -1 H6 H -0.165893 -0.382062 1.000041 0.050 Uiso 1 1 calc R U . B -1 C1 C 0.337(4) -0.097(2) 1.1049(18) 0.040(3) Uani 1 1 d D U . B -1 H1 H 0.466267 -0.067182 1.102331 0.048 Uiso 1 1 calc R U . B -1 C7 C 0.087(3) -0.294(3) 0.987(2) 0.040(3) Uani 1 1 d D U . B -1 H7 H 0.080092 -0.356277 0.916508 0.048 Uiso 1 1 calc R U . B -1 C2 C 0.260(4) -0.019(3) 1.196(2) 0.043(3) Uani 1 1 d D U . B -1 H2 H 0.339929 0.063230 1.231382 0.052 Uiso 1 1 calc R U . B -1 C8 C 0.261(3) -0.209(2) 1.0172(18) 0.039(3) Uani 1 1 d D U . B -1 H8 H 0.349786 -0.234392 0.966154 0.047 Uiso 1 1 calc R U . B -1 C3 C 0.090(3) -0.035(3) 1.248(2) 0.045(3) Uani 1 1 d D U . B -1 H3 H 0.098376 0.024387 1.320322 0.054 Uiso 1 1 calc R U . 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 0.0393(12) 0.0258(10) 0.0386(12) 0.0013(9) -0.0045(7) 0.0062(8) C13 0.045(5) 0.044(6) 0.039(6) -0.010(5) 0.002(5) 0.003(5) C14 0.048(5) 0.044(6) 0.039(5) -0.013(5) 0.005(4) 0.005(5) C10 0.041(5) 0.045(6) 0.037(5) -0.006(5) 0.011(5) 0.002(5) C9 0.041(5) 0.044(5) 0.036(5) -0.007(5) 0.011(4) 0.002(4) C15 0.045(5) 0.045(6) 0.037(5) -0.012(5) 0.008(4) 0.005(5) C16 0.041(5) 0.045(5) 0.036(5) -0.011(5) 0.010(4) 0.005(4) C12 0.042(5) 0.044(6) 0.039(6) -0.007(5) 0.005(5) 0.003(5) C11 0.041(5) 0.045(6) 0.038(5) -0.006(5) 0.010(4) 0.002(5) C17 0.041(5) 0.044(5) 0.035(5) -0.009(5) 0.010(4) 0.004(4) C5 0.049(6) 0.042(6) 0.036(5) -0.006(5) 0.004(5) 0.003(5) C4 0.052(6) 0.043(6) 0.035(5) -0.007(5) 0.004(5) 0.006(5) C6 0.048(6) 0.039(5) 0.035(5) -0.008(5) 0.002(5) 0.002(5) C1 0.046(6) 0.040(6) 0.032(6) -0.008(5) 0.001(5) 0.003(5) C7 0.046(6) 0.038(5) 0.033(5) -0.010(5) 0.002(5) 0.001(5) C2 0.051(6) 0.041(6) 0.034(6) -0.009(5) -0.001(5) 0.004(5) C8 0.046(6) 0.039(6) 0.030(5) -0.009(5) 0.003(5) 0.002(5) C3 0.055(6) 0.042(6) 0.035(5) -0.009(5) 0.001(5) 0.006(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 15 -2 -4 0.0480 30 0 17 0.0547 20 1 -30 0.0515 -1 19 30 0.0973 -10 -2 5 0.0439 -9 -3 -10 0.0497 -30 2 17 0.0684 -13 -2 30 0.0609 0 -6 1 0.2325 -8 -1 -30 0.0544 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 Y1 Y1 C13 64.2(6) 3_557 . ? Y1 Y1 C10 75.8(6) 3_557 . ? Y1 Y1 C9 55.9(4) 3_557 . ? Y1 Y1 C12 82.0(6) 3_557 . ? Y1 Y1 C11 86.6(6) 3_557 . ? Y1 Y1 C5 153.9(5) 3_557 . ? Y1 Y1 C4 160.8(6) 3_557 . ? Y1 Y1 C6 121.7(5) 3_557 . ? Y1 Y1 C1 75.9(6) 3_557 . ? Y1 Y1 C7 92.1(5) 3_557 . ? Y1 Y1 C2 95.5(6) 3_557 . ? Y1 Y1 C8 74.9(6) 3_557 . ? Y1 Y1 C3 127.3(6) 3_557 . ? C13 Y1 C9 88.4(7) . . ? C10 Y1 C13 78.8(7) . . ? C10 Y1 C9 28.4(3) . . ? C10 Y1 C12 59.6(5) . . ? C10 Y1 C1 122.5(6) . . ? C10 Y1 C7 165.8(9) . . ? C10 Y1 C8 145.4(6) . . ? C12 Y1 C13 28.8(4) . . ? C12 Y1 C9 79.8(7) . . ? C12 Y1 C1 155.9(8) . . ? C12 Y1 C7 111.9(6) . . ? C12 Y1 C8 132.4(5) . . ? C11 Y1 C13 56.9(5) . . ? C11 Y1 C10 31.2(4) . . ? C11 Y1 C9 57.3(5) . . ? C11 Y1 C12 31.1(3) . . ? C11 Y1 C6 124.8(6) . . ? C11 Y1 C1 152.8(7) . . ? C11 Y1 C7 142.8(6) . . ? C11 Y1 C8 158.5(8) . . ? C5 Y1 C13 107.5(7) . . ? C5 Y1 C10 128.6(6) . . ? C5 Y1 C9 150.1(4) . . ? C5 Y1 C12 101.8(7) . . ? C5 Y1 C11 110.1(7) . . ? C5 Y1 C6 32.3(3) . . ? C5 Y1 C1 94.0(7) . . ? C5 Y1 C7 62.3(5) . . ? C5 Y1 C8 84.1(7) . . ? C4 Y1 C13 134.7(7) . . ? C4 Y1 C10 108.0(8) . . ? C4 Y1 C9 119.3(5) . . ? C4 Y1 C12 116.4(8) . . ? C4 Y1 C11 106.4(8) . . ? C4 Y1 C5 33.3(4) . . ? C4 Y1 C6 62.5(6) . . ? C4 Y1 C1 86.7(7) . . ? C4 Y1 C7 85.9(7) . . ? C4 Y1 C2 65.3(6) . . ? C4 Y1 C8 94.4(7) . . ? C4 Y1 C3 34.1(4) . . ? C6 Y1 C13 91.6(7) . . ? C6 Y1 C10 154.1(6) . . ? C6 Y1 C9 177.2(5) . . ? C6 Y1 C12 101.5(7) . . ? C6 Y1 C1 82.3(7) . . ? C6 Y1 C7 32.1(4) . . ? C6 Y1 C8 60.1(6) . . ? C1 Y1 C13 128.4(6) . . ? C1 Y1 C9 95.5(6) . . ? C1 Y1 C8 31.0(3) . . ? C7 Y1 C13 89.2(7) . . ? C7 Y1 C9 145.1(5) . . ? C7 Y1 C1 59.9(5) . . ? C7 Y1 C8 31.1(3) . . ? C2 Y1 C13 158.3(8) . . ? C2 Y1 C10 104.5(7) . . ? C2 Y1 C9 85.8(7) . . ? C2 Y1 C12 164.0(7) . . ? C2 Y1 C11 133.4(6) . . ? C2 Y1 C5 87.4(8) . . ? C2 Y1 C6 93.3(8) . . ? C2 Y1 C1 32.2(3) . . ? C2 Y1 C7 83.8(7) . . ? C2 Y1 C8 60.9(5) . . ? C8 Y1 C13 104.1(5) . . ? C8 Y1 C9 117.2(5) . . ? C3 Y1 C13 167.9(8) . . ? C3 Y1 C10 99.8(7) . . ? C3 Y1 C9 96.1(6) . . ? C3 Y1 C12 141.3(7) . . ? C3 Y1 C11 116.6(7) . . ? C3 Y1 C5 63.9(6) . . ? C3 Y1 C6 84.5(7) . . ? C3 Y1 C1 62.5(6) . . ? C3 Y1 C7 93.5(7) . . ? C3 Y1 C2 33.7(4) . . ? C3 Y1 C8 83.9(6) . . ? Y1 C13 H13 124.8 . . ? C14 C13 Y1 90.8(16) . . ? C14 C13 H13 109.2 . . ? C14 C13 C12 142(2) . . ? C12 C13 Y1 67.1(13) . . ? C12 C13 H13 109.2 . . ? C13 C14 H14 112.7 . . ? C15 C14 C13 135(2) . . ? C15 C14 H14 112.7 . . ? Y1 C10 H10 124.6 . . ? C9 C10 Y1 87.6(15) . . ? C9 C10 H10 108.4 . . ? C9 C10 C11 143(2) . . ? C11 C10 Y1 71.6(13) . . ? C11 C10 H10 108.4 . . ? Y1 C9 H9 113.4 . . ? C10 C9 Y1 64.0(13) . . ? C10 C9 H9 114.9 . . ? C17 C9 Y1 96.0(14) . . ? C17 C9 C10 130(2) . . ? C17 C9 H9 114.9 . . ? C14 C15 H15 109.5 . . ? C14 C15 C16 141(2) . . ? C16 C15 H15 109.5 . . ? C15 C16 H16 110.6 . . ? C15 C16 C17 139(2) . . ? C17 C16 H16 110.6 . . ? Y1 C12 H12 126.9 . . ? C13 C12 Y1 84.1(15) . . ? C13 C12 H12 111.1 . . ? C13 C12 C11 138(2) . . ? C11 C12 Y1 70.8(13) . . ? C11 C12 H12 111.1 . . ? Y1 C11 H11 128.4 . . ? C10 C11 Y1 77.2(14) . . ? C10 C11 C12 140(2) . . ? C10 C11 H11 110.1 . . ? C12 C11 Y1 78.2(13) . . ? C12 C11 H11 110.1 . . ? C9 C17 C16 143(2) . . ? C9 C17 H17 108.3 . . ? C16 C17 H17 108.3 . . ? Y1 C5 H5 136.3 . . ? C4 C5 Y1 70.9(12) . . ? C4 C5 H5 113.6 . . ? C6 C5 Y1 75.5(13) . . ? C6 C5 H5 113.6 . . ? C6 C5 C4 133(2) . . ? Y1 C4 H4 131.8 . . ? C5 C4 Y1 75.8(12) . . ? C5 C4 H4 113.1 . . ? C5 C4 C3 134(2) . . ? C3 C4 Y1 73.9(14) . . ? C3 C4 H4 113.1 . . ? Y1 C6 H6 139.9 . . ? C5 C6 Y1 72.2(13) . . ? C5 C6 H6 110.6 . . ? C5 C6 C7 139(2) . . ? C7 C6 Y1 76.6(13) . . ? C7 C6 H6 110.6 . . ? Y1 C1 H1 142.2 . . ? C2 C1 Y1 68.1(13) . . ? C2 C1 H1 113.4 . . ? C8 C1 Y1 75.3(13) . . ? C8 C1 H1 113.4 . . ? C8 C1 C2 133(2) . . ? Y1 C7 H7 135.0 . . ? C6 C7 Y1 71.3(13) . . ? C6 C7 H7 113.3 . . ? C8 C7 Y1 76.1(12) . . ? C8 C7 C6 133(2) . . ? C8 C7 H7 113.3 . . ? Y1 C2 H2 129.6 . . ? C1 C2 Y1 79.7(13) . . ? C1 C2 H2 112.2 . . ? C1 C2 C3 136(2) . . ? C3 C2 Y1 72.3(14) . . ? C3 C2 H2 112.2 . . ? Y1 C8 H8 140.1 . . ? C1 C8 Y1 73.7(12) . . ? C1 C8 H8 112.1 . . ? C7 C8 Y1 72.7(13) . . ? C7 C8 C1 136(2) . . ? C7 C8 H8 112.1 . . ? Y1 C3 H3 140.6 . . ? C4 C3 Y1 72.0(14) . . ? C4 C3 H3 112.2 . . ? C2 C3 Y1 74.0(14) . . ? C2 C3 C4 136(2) . . ? C2 C3 H3 112.2 . . ? 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 Y1 0.828(4) 3_557 ? Y1 C13 2.81(3) . ? Y1 C10 2.58(2) . ? Y1 C9 2.87(2) . ? Y1 C12 2.60(2) . ? Y1 C11 2.51(2) . ? Y1 C5 2.50(2) . ? Y1 C4 2.43(2) . ? Y1 C6 2.54(2) . ? Y1 C1 2.63(2) . ? Y1 C7 2.61(2) . ? Y1 C2 2.48(3) . ? Y1 C8 2.65(2) . ? Y1 C3 2.46(3) . ? C13 H13 0.9500 . ? C13 C14 1.335(14) . ? C13 C12 1.361(14) . ? C14 H14 0.9500 . ? C14 C15 1.328(14) . ? C10 H10 0.9500 . ? C10 C9 1.367(14) . ? C10 C11 1.369(14) . ? C9 H9 0.9500 . ? C9 C17 1.362(14) . ? C15 H15 0.9500 . ? C15 C16 1.350(14) . ? C16 H16 0.9500 . ? C16 C17 1.368(13) . ? C12 H12 0.9500 . ? C12 C11 1.371(14) . ? C11 H11 0.9500 . ? C17 H17 0.9500 . ? C5 H5 0.9500 . ? C5 C4 1.415(14) . ? C5 C6 1.400(14) . ? C4 H4 0.9500 . ? C4 C3 1.434(15) . ? C6 H6 0.9500 . ? C6 C7 1.422(15) . ? C1 H1 0.9500 . ? C1 C2 1.423(14) . ? C1 C8 1.413(14) . ? C7 H7 0.9500 . ? C7 C8 1.410(14) . ? C2 H2 0.9500 . ? C2 C3 1.431(15) . ? C8 H8 0.9500 . ? C3 H3 0.9500 . ? 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 C13 C14 C15 -72(3) . . . . ? Y1 C13 C12 C11 53(3) . . . . ? Y1 C10 C9 C17 75(3) . . . . ? Y1 C10 C11 C12 -53(3) . . . . ? Y1 C9 C17 C16 43(3) . . . . ? Y1 C12 C11 C10 53(3) . . . . ? Y1 C5 C4 C3 -50(3) . . . . ? Y1 C5 C6 C7 42(3) . . . . ? Y1 C4 C3 C2 -42(3) . . . . ? Y1 C6 C7 C8 48(3) . . . . ? Y1 C1 C2 C3 51(3) . . . . ? Y1 C1 C8 C7 -42(3) . . . . ? Y1 C7 C8 C1 42(3) . . . . ? Y1 C2 C3 C4 41(3) . . . . ? C13 C14 C15 C16 34(6) . . . . ? C13 C12 C11 Y1 -57(3) . . . . ? C13 C12 C11 C10 -4(6) . . . . ? C14 C13 C12 Y1 -59(4) . . . . ? C14 C13 C12 C11 -7(6) . . . . ? C14 C15 C16 C17 -2(5) . . . . ? C10 C9 C17 C16 -18(5) . . . . ? C9 C10 C11 Y1 59(4) . . . . ? C9 C10 C11 C12 5(6) . . . . ? C15 C16 C17 C9 -10(5) . . . . ? C12 C13 C14 C15 -19(6) . . . . ? C11 C10 C9 Y1 -54(3) . . . . ? C11 C10 C9 C17 21(5) . . . . ? C5 C4 C3 Y1 51(3) . . . . ? C5 C4 C3 C2 9(5) . . . . ? C5 C6 C7 Y1 -41(3) . . . . ? C5 C6 C7 C8 7(5) . . . . ? C4 C5 C6 Y1 -45(2) . . . . ? C4 C5 C6 C7 -3(5) . . . . ? C6 C5 C4 Y1 47(2) . . . . ? C6 C5 C4 C3 -3(4) . . . . ? C6 C7 C8 Y1 -47(2) . . . . ? C6 C7 C8 C1 -4(5) . . . . ? C1 C2 C3 Y1 -54(3) . . . . ? C1 C2 C3 C4 -12(5) . . . . ? C2 C1 C8 Y1 39(3) . . . . ? C2 C1 C8 C7 -3(5) . . . . ? C8 C1 C2 Y1 -41(3) . . . . ? C8 C1 C2 C3 10(5) . . . . ?