#------------------------------------------------------------------------------ #$Date: 2021-09-06 13:32:54 +0300 (Mon, 06 Sep 2021) $ #$Revision: 268690 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/28/7242835.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_7242835 loop_ _publ_author_name 'Peng, Shuang' 'Qi, Yan-Jie' 'Li, Xin-Hao' 'Sun, Cai' 'Li, Ling-Yun' 'Li, Xin-Xiong' 'Zheng, Shou-Tian' 'Zhang, Qichun' _publ_section_title ; Two isomeric zeolite-like metal--organic frameworks with mechanically responsive luminescence emission and gas adsorption properties ; _journal_issue 34 _journal_name_full CrystEngComm _journal_page_first 5753 _journal_page_last 5757 _journal_paper_doi 10.1039/D1CE00464F _journal_volume 23 _journal_year 2021 _chemical_absolute_configuration ad _chemical_formula_moiety 'C16 H18 N3 Na O5 S' _chemical_formula_sum 'C16 H18 N3 Na O5 S' _chemical_formula_weight 387.38 _chemical_name_common 'amoxicillin sodium' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2020-09-24 _audit_creation_method ; Olex2 1.2-ac3 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2021-02-03 deposited with the CCDC. 2021-05-12 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.6221(10) _cell_length_b 13.075(3) _cell_length_c 13.3414(14) _cell_measurement_reflns_used 507 _cell_measurement_temperature 159.99(10) _cell_measurement_theta_max 46.5060 _cell_measurement_theta_min 6.3150 _cell_volume 1852.9(5) _computing_cell_refinement 'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 159.99(10) _diffrn_detector 'CCD plate' _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.686 _diffrn_measured_fraction_theta_max 0.685 _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 85.00 138.00 0.50 4.00 -- 66.14 129.00 19.00 106 2 \w -6.00 86.00 0.50 4.00 -- 66.14 -29.00 -1.00 184 3 \w -79.00 -53.00 0.50 0.50 -- -1.09-179.00-120.00 52 4 \w -84.00 -50.00 0.50 0.50 -- -1.09-179.00-150.00 68 5 \w -86.00 -48.00 0.50 0.50 -- -1.09-179.00 -90.00 76 6 \w -74.00 -42.00 0.50 4.00 -- -68.33 125.00 -30.00 64 7 \w -113.00 -88.00 0.50 4.00 -- -68.33 125.00 -30.00 50 8 \w -139.00-114.00 0.50 4.00 -- -68.33 -99.00 90.00 50 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'ROD, Synergy Custom system, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0100761000 _diffrn_orient_matrix_UB_12 0.1124693000 _diffrn_orient_matrix_UB_13 -0.0333554000 _diffrn_orient_matrix_UB_21 0.0524874000 _diffrn_orient_matrix_UB_22 -0.0344758000 _diffrn_orient_matrix_UB_23 -0.1020409000 _diffrn_orient_matrix_UB_31 -0.1348808000 _diffrn_orient_matrix_UB_32 -0.0051132000 _diffrn_orient_matrix_UB_33 -0.0426402000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_unetI/netI 0.0732 _diffrn_reflns_Laue_measured_fraction_full 0.686 _diffrn_reflns_Laue_measured_fraction_max 0.685 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 2273 _diffrn_reflns_point_group_measured_fraction_full 0.622 _diffrn_reflns_point_group_measured_fraction_max 0.622 _diffrn_reflns_theta_full 51.706 _diffrn_reflns_theta_max 51.706 _diffrn_reflns_theta_min 4.736 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 2.072 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.51814 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.389 _exptl_crystal_description block _exptl_crystal_F_000 808 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.247 _refine_diff_density_min -0.198 _refine_diff_density_rms 0.058 _refine_ls_abs_structure_details ; Flack x determined using 276 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.07(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 263 _refine_ls_number_reflns 1273 _refine_ls_number_restraints 47 _refine_ls_restrained_S_all 1.007 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0556 _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^)+(0.0845P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1240 _refine_ls_wR_factor_ref 0.1370 _reflns_Friedel_coverage 0.549 _reflns_Friedel_fraction_full 0.531 _reflns_Friedel_fraction_max 0.532 _reflns_number_gt 959 _reflns_number_total 1273 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1ce00464f2.cif _cod_data_source_block exp_152_cpp1 _cod_depositor_comments 'Adding full bibliography for 7242835--7242836.cif.' _cod_database_code 7242835 _shelx_shelxl_version_number 2018/1 _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. ; _shelx_estimated_absorpt_t_max 0.903 _shelx_estimated_absorpt_t_min 0.852 _reflns_odcompleteness_completeness 69.05 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 50.38 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups, All N(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances H007-O007 0.9 with sigma of 0.02 C12-C11 \\sim C12A-C11 with sigma of 0.02 C12-C13 \\sim C12A-C13A with sigma of 0.02 C11-C16 \\sim C11-C16A with sigma of 0.02 C16-C15 \\sim C16A-C15A with sigma of 0.02 C15-C14 \\sim C15A-C14 with sigma of 0.02 C14-C13 \\sim C14-C13A with sigma of 0.02 C12-C14 \\sim C12A-C14 with sigma of 0.04 C11-C15 \\sim C11-C15A with sigma of 0.04 C11-C13 \\sim C11-C13A with sigma of 0.04 C16-C14 \\sim C16A-C14 with sigma of 0.04 3. Rigid bond restraints C11, C16A, C15A, C13A with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 4. Uiso/Uaniso restraints and constraints C11 \\sim C16A \\sim C15A \\sim C13A \\sim C12A: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.001 5. Rigid body (RIGU) restrains C11, C16, C15 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 6. Others Sof(C12A)=Sof(H12A)=Sof(C16A)=Sof(H16A)=Sof(C15A)=Sof(H15A)=Sof(C13A)= Sof(H13A)=1-FVAR(1) Sof(C12)=Sof(H12)=Sof(C16)=Sof(H16)=Sof(C15)=Sof(H15)=Sof(C13)=Sof(H13)=FVAR(1) Fixed X: H007(-0.062531) Fixed Y: H007(0.50821) Fixed Z: H007(0.32349) 7.a Ternary CH refined with riding coordinates: C2(H2A), C10(H10), C8(H8), C6(H6) 7.b Secondary CH2 refined with riding coordinates: N3(H3A,H3B) 7.c Aromatic/amide H refined with riding coordinates: N2(H2), C12(H12), C16(H16), C15(H15), C13(H13), C12A(H12A), C16A(H16A), C15A(H15A), C13A(H13A) 7.d Fitted hexagon refined as free rotating group: C12A(C11,C16A,C15A,C14,C13A) 7.e Idealised Me refined as rotating group: C4(H4A,H4B,H4C), C5(H5A,H5B,H5C) ; _shelx_res_file ; TITL exp_152_cpp1_a.res in P2(1)2(1)2(1) exp_152_cpp1.res created by SHELXL-2018/1 at 15:04:49 on 24-Sep-2020 REM Old TITL exp_152_cpp1 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.166, Rweak 0.045, Alpha 0.011, Orientation as input REM Flack x = -2.447 ( 0.453 ) from Parsons' quotients REM Formula found by SHELXT: C14 N3 O7 CELL 1.54184 10.622129 13.074785 13.341424 90 90 90 ZERR 4 0.000973 0.003358 0.001447 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N Na O S UNIT 64 72 12 4 20 4 EQIV $1 1.5-X,1-Y,-0.5+Z DFIX 0.9 H007 O007 SADI C12 C11 C12A C11 SADI C12 C13 C12A C13A SADI C11 C16 C11 C16A SADI C16 C15 C16A C15A SADI C15 C14 C15A C14 SADI C14 C13 C14 C13A SADI 0.04 C12 C14 C12A C14 SADI 0.04 C11 C15 C11 C15A SADI 0.04 C11 C13 C11 C13A SADI 0.04 C16 C14 C16A C14 DELU 0.001 0.001 C11 C16A C15A C13A SIMU 0.001 0.001 2 C11 C16A C15A C13A C12A RIGU 0.001 0.001 C11 C16 C15 L.S. 80 PLAN 50 SIZE 0.05 0.06 0.08 FREE Na1 C1 FREE Na1 C9_$1 BOND $H LIST 4 fmap 2 acta REM REM REM WGHT 0.084500 FVAR 3.58938 0.74379 S1 6 0.504385 0.588187 0.369001 11.00000 0.05855 0.10071 = 0.07336 0.01890 -0.00845 -0.01012 O3 5 0.708516 0.656524 0.622530 11.00000 0.06870 0.08674 = 0.06706 -0.01373 0.01336 -0.02080 O1 5 0.868882 0.810815 0.329925 11.00000 0.07994 0.06603 = 0.06592 0.01103 0.00430 -0.00463 O4 5 0.495675 0.330011 0.623896 11.00000 0.06607 0.07395 = 0.08935 0.01353 0.01034 0.00332 O2 5 0.931969 0.645462 0.344583 11.00000 0.05563 0.08836 = 0.09920 0.02553 0.01525 0.01736 O007 5 -0.040408 0.451628 0.364316 11.00000 0.06594 0.08703 = 0.09413 -0.01409 -0.03377 0.00216 N1 3 0.720765 0.601010 0.456077 11.00000 0.05840 0.04269 = 0.05605 -0.01017 -0.00362 0.00438 N2 3 0.492390 0.499459 0.592714 11.00000 0.05491 0.03907 = 0.07252 0.00875 0.01616 0.00216 AFIX 43 H2 2 0.450245 0.555459 0.596880 11.00000 -1.20000 AFIX 0 N3 3 0.296210 0.345606 0.750279 11.00000 0.05450 0.11505 = 0.07550 0.02518 0.00745 -0.00751 AFIX 23 H3A 2 0.218181 0.322486 0.741488 11.00000 -1.20000 H3B 2 0.300675 0.370422 0.812296 11.00000 -1.20000 AFIX 0 C7 1 0.687396 0.596168 0.554964 11.00000 0.05654 0.04250 = 0.06059 -0.01915 -0.00373 0.00622 C2 1 0.720291 0.691852 0.394283 11.00000 0.05854 0.03851 = 0.06600 0.00560 0.00277 -0.00305 AFIX 13 H2A 2 0.689969 0.749717 0.434245 11.00000 -1.20000 AFIX 0 C10 1 0.315913 0.429410 0.681239 11.00000 0.05984 0.06676 = 0.05870 0.00147 0.00625 0.00129 AFIX 13 H10 2 0.312894 0.494820 0.717027 11.00000 -1.20000 AFIX 0 C8 1 0.610905 0.500816 0.542932 11.00000 0.05919 0.06136 = 0.06447 -0.00834 0.00348 0.00915 AFIX 13 H8 2 0.660761 0.441263 0.563278 11.00000 -1.20000 AFIX 0 C9 1 0.443996 0.414685 0.633227 11.00000 0.04741 0.09220 = 0.05412 0.01569 -0.00192 -0.01682 C1 1 0.855738 0.716555 0.354966 11.00000 0.07191 0.05155 = 0.05313 0.02324 0.00125 -0.00286 C6 1 0.626775 0.519456 0.430403 11.00000 0.08053 0.03505 = 0.06347 -0.00782 -0.00172 -0.01370 AFIX 13 H6 2 0.660749 0.461442 0.392566 11.00000 -1.20000 AFIX 0 C3 1 0.623679 0.669942 0.308034 11.00000 0.05187 0.06538 = 0.07469 -0.00274 0.00143 -0.01108 PART 1 C12 1 0.131710 0.505993 0.592579 21.00000 0.06355 0.13445 = 0.05766 -0.02101 0.01263 0.01198 AFIX 43 H12 2 0.132599 0.554211 0.643821 21.00000 -1.20000 AFIX 0 C16 1 0.226514 0.366798 0.511269 21.00000 0.06483 0.14714 = 0.12627 -0.05543 -0.02622 0.01782 AFIX 43 H16 2 0.292051 0.320094 0.504816 21.00000 -1.20000 AFIX 0 C15 1 0.136975 0.375591 0.435988 21.00000 0.07682 0.13097 = 0.13212 -0.05387 -0.03627 -0.00053 AFIX 43 H15 2 0.142079 0.334140 0.379487 21.00000 -1.20000 AFIX 0 C13 1 0.044374 0.517382 0.518116 21.00000 0.07419 0.07073 = 0.03875 -0.01110 0.00629 0.03756 AFIX 43 H13 2 -0.010683 0.572686 0.517804 21.00000 -1.20000 AFIX 0 PART 0 C4 1 0.680998 0.615683 0.219949 11.00000 0.07913 0.13420 = 0.05733 -0.00788 -0.00123 -0.02934 AFIX 137 H4A 2 0.712042 0.550122 0.240891 11.00000 -1.50000 H4B 2 0.749252 0.655717 0.193769 11.00000 -1.50000 H4C 2 0.618342 0.606524 0.168874 11.00000 -1.50000 AFIX 0 C5 1 0.557912 0.771417 0.273330 11.00000 0.09162 0.07920 = 0.08540 0.03004 -0.01395 -0.00285 AFIX 137 H5A 2 0.489985 0.755363 0.228549 11.00000 -1.50000 H5B 2 0.617990 0.813998 0.239442 11.00000 -1.50000 H5C 2 0.525528 0.806966 0.330769 11.00000 -1.50000 AFIX 0 NA1 4 1.062153 0.798152 0.239145 11.00000 0.06544 0.06406 = 0.07223 -0.00747 -0.00510 0.00308 PART 2 AFIX 66 C12A 1 0.190813 0.523457 0.556076 -21.00000 0.04756 0.06467 = 0.07859 0.00889 -0.00548 0.00910 AFIX 43 H12A 2 0.231999 0.581387 0.579756 -21.00000 -1.20000 AFIX 65 PART 0 C11 1 0.218131 0.428095 0.596667 11.00000 0.04745 0.06465 = 0.07845 0.00900 -0.00560 0.00914 PART 2 C16A 1 0.156574 0.341511 0.561273 -21.00000 0.04733 0.06462 = 0.07833 0.00894 -0.00553 0.00922 AFIX 43 H16A 2 0.174852 0.277707 0.588432 -21.00000 -1.20000 AFIX 65 C15A 1 0.067697 0.350289 0.485289 -21.00000 0.04727 0.06462 = 0.07833 0.00889 -0.00554 0.00924 AFIX 43 H15A 2 0.026512 0.292358 0.461609 -21.00000 -1.20000 AFIX 65 PART 0 C14 1 0.040378 0.445650 0.444697 11.00000 0.04171 0.07054 = 0.09553 0.00250 -0.01331 0.00742 PART 2 C13A 1 0.101934 0.532235 0.480090 -21.00000 0.04766 0.06470 = 0.07871 0.00891 -0.00535 0.00915 AFIX 43 H13A 2 0.083655 0.596038 0.452931 -21.00000 -1.20000 AFIX 0 PART 0 H007 2 9.937469 10.508210 10.323490 11.00000 1.04481 HKLF 4 REM exp_152_cpp1_a.res in P2(1)2(1)2(1) REM R1 = 0.0556 for 959 Fo > 4sig(Fo) and 0.0796 for all 1273 data REM 263 parameters refined using 47 restraints END WGHT 0.0845 0.0000 REM Highest difference peak 0.247, deepest hole -0.198, 1-sigma level 0.058 Q1 1 0.5318 0.5810 0.4645 11.00000 0.05 0.25 Q2 1 0.4574 0.6421 0.4372 11.00000 0.05 0.24 Q3 1 0.0564 0.3244 0.5231 11.00000 0.05 0.23 Q4 1 0.1917 0.3433 0.5791 11.00000 0.05 0.21 Q5 1 0.5584 0.6013 0.2632 11.00000 0.05 0.20 Q6 1 0.5735 0.6426 0.4219 11.00000 0.05 0.20 Q7 1 0.9225 0.7709 0.2632 11.00000 0.05 0.19 Q8 1 0.4757 0.3811 0.7171 11.00000 0.05 0.19 Q9 1 -0.0496 0.4432 0.4235 11.00000 0.05 0.18 Q10 1 0.9497 0.7524 0.3993 11.00000 0.05 0.17 Q11 1 0.5139 0.3957 0.6981 11.00000 0.05 0.17 Q12 1 0.5442 0.3451 0.5293 11.00000 0.05 0.17 Q13 1 0.0110 0.4553 0.3413 11.00000 0.05 0.16 Q14 1 -0.0081 0.4168 0.3987 11.00000 0.05 0.16 Q15 1 -0.1028 0.4552 0.3482 11.00000 0.05 0.15 Q16 1 -0.0443 0.3886 0.3185 11.00000 0.05 0.15 Q17 1 0.5718 0.4382 0.4974 11.00000 0.05 0.15 Q18 1 0.0794 0.4352 0.4363 11.00000 0.05 0.14 Q19 1 0.0535 0.4842 0.4442 11.00000 0.05 0.14 Q20 1 0.6498 0.6022 0.3448 11.00000 0.05 0.14 Q21 1 0.6468 0.6570 0.5017 11.00000 0.05 0.14 Q22 1 0.6167 0.7325 0.1411 11.00000 0.05 0.14 Q23 1 0.2780 0.4558 0.6414 11.00000 0.05 0.13 Q24 1 0.3709 0.4060 0.6597 11.00000 0.05 0.13 Q25 1 0.1933 0.4958 0.6247 11.00000 0.05 0.13 Q26 1 0.8823 0.5972 0.4220 11.00000 0.05 0.13 Q27 1 0.5352 0.8007 0.1452 11.00000 0.05 0.13 Q28 1 0.0024 0.4065 0.5079 11.00000 0.05 0.13 Q29 1 -0.0052 0.5770 0.4097 11.00000 0.05 0.13 Q30 1 0.5576 0.6656 0.3118 11.00000 0.05 0.13 Q31 1 1.1029 0.7626 0.3348 11.00000 0.05 0.12 Q32 1 1.0250 0.8074 0.1528 11.00000 0.05 0.12 Q33 1 0.5623 0.5167 0.2942 11.00000 0.05 0.12 Q34 1 0.4996 0.8402 0.3618 11.00000 0.05 0.12 Q35 1 0.3522 0.4325 0.8038 11.00000 0.05 0.12 Q36 1 0.4511 0.8196 0.2176 11.00000 0.05 0.12 Q37 1 0.7120 0.6575 0.7354 11.00000 0.05 0.12 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-2 6 3438.00 437.449 8 -8 -2 7 2102.34 355.081 1 -8 -2 7 998.257 403.932 8 -8 -2 8 1158.60 346.478 1 -8 -2 8 282.034 395.810 8 -8 3 8 1128.79 319.279 1 -8 -3 -7 563.393 441.070 7 -8 3 7 919.007 322.967 1 -8 -3 -6 479.200 428.710 7 -8 3 6 605.350 327.755 1 -8 -3 -5 1909.78 434.479 7 -8 3 5 2563.35 359.357 1 -8 -3 -4 3594.06 446.979 7 -8 3 4 4388.38 395.363 1 -8 3 3 4031.22 383.998 1 -8 -3 -3 3327.22 425.692 7 -8 -3 -2 905.950 367.332 7 -8 3 2 527.534 330.048 1 -8 3 0 997.427 387.075 7 -8 -3 2 176.121 347.483 1 -8 -3 3 4576.50 409.357 1 -8 -3 4 4630.66 411.417 1 -8 -3 5 2981.01 375.744 1 -8 -3 5 2637.00 414.464 8 -8 -3 6 654.693 343.720 1 -8 -3 6 565.776 397.965 8 -8 -3 7 1354.68 354.304 1 -8 -3 7 624.984 411.214 8 -8 -3 8 1049.80 356.871 1 -8 -3 8 1373.07 418.413 8 -8 4 7 622.021 325.299 1 -8 -4 -6 1133.75 449.613 7 -8 4 6 810.996 341.176 1 -8 -4 -5 690.658 429.305 7 -8 4 5 549.122 343.132 1 -8 4 4 870.069 348.965 1 -8 -4 -4 819.881 417.374 7 -8 -4 -3 3983.41 459.780 7 -8 4 3 5036.84 413.388 1 -8 -4 3 4861.74 422.963 1 -8 -4 4 869.650 346.506 1 -8 -4 5 651.619 346.613 1 -8 -4 5-151.688 386.241 8 -8 -4 6 801.562 348.258 1 -8 -4 6 263.689 404.194 8 -8 -4 7 1035.55 345.471 1 -8 -4 7 70.8445 408.388 8 -8 -4 8 993.678 423.808 8 -8 -5 4 673.205 342.121 1 -8 -5 5 2532.82 365.951 1 -8 -5 6 849.985 408.842 8 -8 -5 7 1060.81 417.344 8 -9 0 0 339.965 437.356 7 -9 0 1 6442.30 547.643 7 -9 0 -1 6312.09 552.590 7 -9 0 -2 2422.89 468.647 7 -9 0 -3 1769.85 460.820 7 -9 0 3 2326.91 380.041 1 -9 0 4-605.634 360.980 1 -9 0 -5 385.095 442.178 7 -9 0 5 918.746 363.248 1 -9 0 -6 447.323 442.652 7 -9 0 6 355.965 353.843 1 -9 0 -7 358.833 439.422 7 -9 0 7 397.094 353.292 1 -9 -1 -7 202.020 428.425 7 -9 1 7 424.494 346.483 1 -9 -1 -6 560.344 430.061 7 -9 1 6 1305.17 353.931 1 -9 -1 -5 524.598 430.500 7 -9 1 5 725.484 356.998 1 -9 1 4 57.3026 354.766 1 -9 1 3 987.837 368.218 1 -9 -1 -2 1714.53 454.187 7 -9 1 1 7605.81 575.708 7 -9 -1 -1 7886.86 581.107 7 -9 1 0-400.346 437.702 7 -9 -1 0 262.003 432.792 7 -9 1 -1 6767.93 561.846 7 -9 1 -2 1572.30 470.684 7 -9 1 -3 1139.64 469.478 7 -9 -1 3 618.207 373.363 1 -9 -1 4-179.818 360.211 1 -9 1 -4 245.660 465.691 7 -9 -1 5 645.612 362.709 1 -9 1 -6 859.489 459.116 7 -9 -1 6 995.987 364.647 1 -9 1 -7-95.8969 454.329 7 -9 -1 7 191.964 357.315 1 -9 -2 -7 204.872 442.508 7 -9 2 7 77.1714 335.594 1 -9 -2 -6 847.922 449.078 7 -9 2 6 1990.90 356.532 1 -9 2 5 1151.04 358.978 1 -9 -2 -5 72.6521 440.809 7 -9 2 4 6730.38 462.651 1 -9 -2 -4 4513.02 523.073 7 -9 2 3 1518.20 378.171 1 -9 2 1-136.567 413.415 7 -9 -2 -1-126.846 427.286 7 -9 2 0 4925.61 498.682 7 -9 2 -1 648.036 443.178 7 -9 2 -2 166.449 472.941 7 -9 -2 3 1312.11 386.771 1 -9 -2 4 6730.45 491.142 1 -9 -2 5 1199.36 372.754 1 -9 -2 6 1812.75 380.688 1 -9 -2 7 140.955 365.092 1 -9 3 6 397.501 337.048 1 -9 -3 -6 42.8164 442.683 7 -9 -3 -5 663.666 439.511 7 -9 3 5 827.127 351.783 1 -9 -3 -4 756.596 435.390 7 -9 3 4 690.072 372.332 1 -9 -3 -3 3944.48 478.369 7 -9 3 0 935.359 415.227 7 -9 3 -1-451.865 443.071 7 -9 3 -2 284.956 477.185 7 -9 -3 4 866.898 372.587 1 -9 -3 5 263.065 365.002 1 -9 -3 6 154.729 363.016 1 -9 4 6 340.412 336.453 1 -9 4 5 467.672 355.674 1 -9 4 -1 123.313 429.654 7 -9 -4 5 80.9848 362.812 1 -9 -4 6 463.831 352.335 1 -10 0 0 1156.52 496.032 7 -10 0 -1 2896.32 534.715 7 -10 0 -2 687.745 509.717 7 -10 0 -3 524.178 499.264 7 -10 0 -4 1606.48 498.605 7 -10 0 5 5.51340 371.272 1 -10 -1 -5 673.035 460.884 7 -10 1 5 53.8303 371.648 1 -10 -1 -3 312.789 482.734 7 -10 -1 -2-18.8235 491.526 7 -10 -1 -1 1080.85 503.223 7 -10 1 0-201.252 475.643 7 -10 1 -1 1045.84 505.127 7 -10 1 -2-122.337 507.237 7 -10 1 -3 216.922 505.024 7 -10 1 -4 158.227 497.095 7 -10 -1 5 897.452 379.169 1 -10 -2 -4 154.185 456.465 7 -10 2 0 1348.61 459.130 7 -10 2 -1 2437.31 507.661 7 -10 2 -2 1771.40 514.878 7 -10 2 -3 11.2915 515.019 7 -10 2 -4-36.8525 502.163 7 -10 3 -1 2996.28 490.603 7 -10 3 -2 219.761 480.265 7 -10 3 -3 665.513 503.177 7 -10 3 -4-327.162 503.412 7 -10 4 -2 518.070 461.902 7 0 0 0 0.00 0.00 0 TITL exp_152_cpp1 in P2(1)2(1)2(1) REM P2(1)2(1)2(1) (#19 in standard setting) CELL 1.54184 10.622129 13.074785 13.341424 90.0000 90.0000 90.0000 ZERR 8.00 0.000973 0.003358 0.001447 0.0000 0.0000 0.0000 LATT -1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z+1/2 SYMM x+1/2,-y+1/2,-z SFAC C H N O UNIT 88.00 80.00 8.00 8.00 TREF HKLF 4 END ; _shelx_hkl_checksum 46502 _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 1.638 _oxdiff_exptl_absorpt_empirical_full_min 0.694 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 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 S1 S 0.5044(3) 0.5882(5) 0.3690(2) 0.0775(18) Uani 1 1 d . . . . . O3 O 0.7085(8) 0.6565(10) 0.6225(7) 0.074(4) Uani 1 1 d . . . . . O1 O 0.8689(9) 0.8108(14) 0.3299(7) 0.071(5) Uani 1 1 d . . . . . O4 O 0.4957(11) 0.3300(13) 0.6239(7) 0.076(5) Uani 1 1 d . . . . . O2 O 0.9320(10) 0.6455(13) 0.3446(7) 0.081(5) Uani 1 1 d . . . . . O007 O -0.0404(8) 0.4516(9) 0.3643(7) 0.082(5) Uani 1 1 d D . . . . N1 N 0.7208(10) 0.6010(12) 0.4561(7) 0.052(4) Uani 1 1 d . . . . . N2 N 0.4924(10) 0.4995(13) 0.5927(7) 0.056(4) Uani 1 1 d . . . . . H2 H 0.450245 0.555459 0.596880 0.067 Uiso 1 1 calc R . . . . N3 N 0.2962(10) 0.3456(12) 0.7503(8) 0.082(5) Uani 1 1 d . . . . . H3A H 0.218181 0.322486 0.741488 0.098 Uiso 1 1 calc R . . . . H3B H 0.300675 0.370422 0.812296 0.098 Uiso 1 1 calc R . . . . C7 C 0.6874(12) 0.5962(16) 0.5550(11) 0.053(6) Uani 1 1 d . . . . . C2 C 0.7203(12) 0.6919(15) 0.3943(10) 0.054(5) Uani 1 1 d . . . . . H2A H 0.689969 0.749717 0.434245 0.065 Uiso 1 1 calc R . . . . C10 C 0.3159(11) 0.4294(15) 0.6812(9) 0.062(6) Uani 1 1 d . . . . . H10 H 0.312894 0.494820 0.717027 0.074 Uiso 1 1 calc R . . . . C8 C 0.6109(13) 0.5008(18) 0.5429(9) 0.062(6) Uani 1 1 d . . . . . H8 H 0.660761 0.441263 0.563278 0.074 Uiso 1 1 calc R . . . . C9 C 0.4440(14) 0.415(2) 0.6332(10) 0.065(7) Uani 1 1 d . . . . . C1 C 0.8557(16) 0.717(2) 0.3550(10) 0.059(7) Uani 1 1 d . . . . . C6 C 0.6268(13) 0.5195(15) 0.4304(9) 0.060(6) Uani 1 1 d . . . . . H6 H 0.660749 0.461442 0.392566 0.072 Uiso 1 1 calc R . . . . C3 C 0.6237(12) 0.6699(16) 0.3080(10) 0.064(6) Uani 1 1 d . . . . . C12 C 0.1317(19) 0.506(2) 0.5926(13) 0.085(10) Uani 0.74(2) 1 d D . P A 1 H12 H 0.132599 0.554211 0.643821 0.102 Uiso 0.74(2) 1 calc R . P A 1 C16 C 0.227(2) 0.367(2) 0.5113(16) 0.113(11) Uani 0.74(2) 1 d D U P A 1 H16 H 0.292051 0.320094 0.504816 0.135 Uiso 0.74(2) 1 calc R . P A 1 C15 C 0.137(2) 0.376(2) 0.4360(19) 0.113(13) Uani 0.74(2) 1 d D U P A 1 H15 H 0.142079 0.334140 0.379487 0.136 Uiso 0.74(2) 1 calc R . P A 1 C13 C 0.0444(18) 0.5174(18) 0.5181(12) 0.061(8) Uani 0.74(2) 1 d D . P A 1 H13 H -0.010683 0.572686 0.517804 0.073 Uiso 0.74(2) 1 calc R . P A 1 C4 C 0.6810(13) 0.6157(18) 0.2199(9) 0.090(7) Uani 1 1 d . . . . . H4A H 0.712042 0.550122 0.240891 0.135 Uiso 1 1 calc GR . . . . H4B H 0.749252 0.655717 0.193769 0.135 Uiso 1 1 calc GR . . . . H4C H 0.618342 0.606524 0.168874 0.135 Uiso 1 1 calc GR . . . . C5 C 0.5579(14) 0.7714(17) 0.2733(11) 0.085(7) Uani 1 1 d . . . . . H5A H 0.489985 0.755363 0.228549 0.128 Uiso 1 1 calc GR . . . . H5B H 0.617990 0.813998 0.239442 0.128 Uiso 1 1 calc GR . . . . H5C H 0.525528 0.806966 0.330769 0.128 Uiso 1 1 calc GR . . . . Na1 Na 1.0622(5) 0.7982(5) 0.2391(3) 0.067(2) Uani 1 1 d . . . . . C12A C 0.191(3) 0.5235(12) 0.556(2) 0.064(4) Uani 0.26(2) 1 d D U P A 2 H12A H 0.231999 0.581387 0.579756 0.076 Uiso 0.26(2) 1 calc R . P A 2 C11 C 0.2181(10) 0.4281(14) 0.5967(8) 0.064(4) Uani 1 1 d DG U . . . C16A C 0.157(3) 0.3415(12) 0.561(2) 0.063(4) Uani 0.26(2) 1 d DG U P A 2 H16A H 0.174852 0.277707 0.588432 0.076 Uiso 0.26(2) 1 calc R . P A 2 C15A C 0.068(3) 0.3503(13) 0.485(2) 0.063(4) Uani 0.26(2) 1 d DG U P A 2 H15A H 0.026512 0.292358 0.461609 0.076 Uiso 0.26(2) 1 calc R . P A 2 C14 C 0.0404(10) 0.4457(14) 0.4447(9) 0.069(7) Uani 1 1 d DG . . . . C13A C 0.102(3) 0.5322(12) 0.480(2) 0.064(4) Uani 0.26(2) 1 d DG U P A 2 H13A H 0.083655 0.596038 0.452931 0.076 Uiso 0.26(2) 1 calc R . P A 2 H007 H -0.062531 0.508210 0.323490 1.0(10) Uiso 1 1 d 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 S1 0.059(2) 0.101(6) 0.073(2) 0.019(2) -0.0085(17) -0.010(3) O3 0.069(6) 0.087(14) 0.067(6) -0.014(6) 0.013(5) -0.021(7) O1 0.080(7) 0.066(17) 0.066(6) 0.011(7) 0.004(5) -0.005(7) O4 0.066(8) 0.074(18) 0.089(7) 0.014(7) 0.010(5) 0.003(8) O2 0.056(6) 0.088(17) 0.099(7) 0.026(7) 0.015(5) 0.017(8) O007 0.066(6) 0.087(15) 0.094(6) -0.014(6) -0.034(5) 0.002(6) N1 0.058(7) 0.043(15) 0.056(7) -0.010(7) -0.004(5) 0.004(8) N2 0.055(7) 0.039(15) 0.073(7) 0.009(7) 0.016(6) 0.002(7) N3 0.055(7) 0.115(18) 0.075(7) 0.025(9) 0.007(6) -0.008(8) C7 0.057(9) 0.04(2) 0.061(10) -0.019(10) -0.004(6) 0.006(10) C2 0.059(9) 0.039(18) 0.066(8) 0.006(9) 0.003(6) -0.003(9) C10 0.060(9) 0.07(2) 0.059(8) 0.001(9) 0.006(7) 0.001(10) C8 0.059(9) 0.06(2) 0.064(9) -0.008(9) 0.003(7) 0.009(10) C9 0.047(11) 0.09(3) 0.054(8) 0.016(11) -0.002(7) -0.017(12) C1 0.072(13) 0.05(2) 0.053(8) 0.023(10) 0.001(7) -0.003(13) C6 0.081(10) 0.04(2) 0.063(9) -0.008(8) -0.002(7) -0.014(10) C3 0.052(8) 0.07(2) 0.075(9) -0.003(10) 0.001(7) -0.011(10) C12 0.064(13) 0.13(3) 0.058(12) -0.021(14) 0.013(10) 0.012(17) C16 0.065(13) 0.15(2) 0.126(12) -0.055(14) -0.026(10) 0.018(16) C15 0.077(16) 0.13(4) 0.132(14) -0.054(16) -0.036(12) -0.001(18) C13 0.074(13) 0.07(3) 0.039(10) -0.011(10) 0.006(9) 0.038(14) C4 0.079(10) 0.13(3) 0.057(8) -0.008(10) -0.001(7) -0.029(12) C5 0.092(11) 0.08(2) 0.085(10) 0.030(10) -0.014(8) -0.003(13) Na1 0.065(3) 0.064(7) 0.072(3) -0.007(3) -0.005(2) 0.003(3) C12A 0.048(7) 0.065(13) 0.079(7) 0.009(6) -0.005(6) 0.009(8) C11 0.047(7) 0.065(13) 0.078(7) 0.009(6) -0.006(5) 0.009(8) C16A 0.047(7) 0.065(13) 0.078(7) 0.009(6) -0.006(6) 0.009(8) C15A 0.047(7) 0.065(13) 0.078(7) 0.009(7) -0.006(6) 0.009(8) C14 0.042(9) 0.07(2) 0.096(11) 0.003(11) -0.013(7) 0.007(10) C13A 0.048(7) 0.065(13) 0.079(7) 0.009(7) -0.005(6) 0.009(8) 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' Na Na 0.1353 0.1239 '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' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C6 S1 C3 89.6(7) . . ? C7 O3 Na1 126.1(9) . 4_466 ? C1 O1 Na1 99.1(11) . . ? C9 O4 Na1 117.0(12) . 2_665 ? C1 O2 Na1 81.1(12) . . ? Na1 O007 H007 107.0(6) 3_645 . ? C14 O007 Na1 116.9(10) . 3_645 ? C14 O007 H007 130.3(12) . . ? C7 N1 C2 126.0(15) . . ? C7 N1 C6 90.9(12) . . ? C2 N1 C6 116.8(10) . . ? C8 N2 H2 118.7 . . ? C9 N2 H2 118.7 . . ? C9 N2 C8 122.6(17) . . ? H3A N3 H3B 107.2 . . ? C10 N3 H3A 107.9 . . ? C10 N3 H3B 107.9 . . ? C10 N3 Na1 117.4(8) . 2_665 ? Na1 N3 H3A 107.9 2_665 . ? Na1 N3 H3B 107.9 2_665 . ? O3 C7 N1 129.5(18) . . ? O3 C7 C8 135.9(14) . . ? N1 C7 C8 94.3(12) . . ? N1 C2 H2A 109.0 . . ? N1 C2 C1 110.9(14) . . ? N1 C2 C3 105.7(14) . . ? C1 C2 H2A 109.0 . . ? C1 C2 C3 113.2(10) . . ? C3 C2 H2A 109.0 . . ? N3 C10 H10 110.2 . . ? N3 C10 C9 107.6(15) . . ? N3 C10 C11 111.2(13) . . ? C9 C10 H10 110.2 . . ? C9 C10 C11 107.2(10) . . ? C11 C10 H10 110.2 . . ? N2 C8 C7 116.1(15) . . ? N2 C8 H8 109.8 . . ? N2 C8 C6 123.9(12) . . ? C7 C8 H8 109.8 . . ? C7 C8 C6 85.0(12) . . ? C6 C8 H8 109.8 . . ? O4 C9 N2 121.9(16) . . ? O4 C9 C10 124(2) . . ? O4 C9 Na1 42.3(10) . 2_665 ? N2 C9 C10 114(2) . . ? N2 C9 Na1 158.6(11) . 2_665 ? C10 C9 Na1 84.4(12) . 2_665 ? O1 C1 C2 112.6(19) . . ? O2 C1 O1 128.2(17) . . ? O2 C1 C2 119(2) . . ? S1 C6 H6 115.0 . . ? N1 C6 S1 103.4(12) . . ? N1 C6 C8 87.9(11) . . ? N1 C6 H6 115.0 . . ? C8 C6 S1 116.8(11) . . ? C8 C6 H6 115.0 . . ? C2 C3 S1 103.4(10) . . ? C2 C3 C5 110.7(15) . . ? C4 C3 S1 110.5(13) . . ? C4 C3 C2 113.3(12) . . ? C4 C3 C5 110.4(14) . . ? C5 C3 S1 108.3(9) . . ? C13 C12 H12 117.8 . . ? C13 C12 C11 124.3(18) . . ? C11 C12 H12 117.8 . . ? C15 C16 H16 120.0 . . ? C15 C16 C11 120.0(19) . . ? C11 C16 H16 120.0 . . ? C16 C15 H15 119.9 . . ? C14 C15 C16 120.2(18) . . ? C14 C15 H15 119.9 . . ? C12 C13 H13 121.0 . . ? C14 C13 C12 118.1(18) . . ? C14 C13 H13 121.0 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 Na1 O2 96.1(4) 4_566 . ? O1 Na1 O3 98.3(4) . 4_566 ? O1 Na1 O2 51.1(5) . . ? O1 Na1 O007 98.5(5) . 3_655 ? O1 Na1 N3 124.0(5) . 2_664 ? O4 Na1 O3 144.8(6) 2_664 4_566 ? O4 Na1 O1 99.0(5) 2_664 . ? O4 Na1 O2 72.1(4) 2_664 . ? O4 Na1 O007 101.0(5) 2_664 3_655 ? O4 Na1 N3 69.4(5) 2_664 2_664 ? O007 Na1 O3 106.4(4) 3_655 4_566 ? O007 Na1 O2 145.1(4) 3_655 . ? N3 Na1 O3 75.5(4) 2_664 4_566 ? N3 Na1 O2 73.9(5) 2_664 . ? N3 Na1 O007 137.1(4) 2_664 3_655 ? C11 C12A H12A 120.0 . . ? C11 C12A C13A 120.0 . . ? C13A C12A H12A 120.0 . . ? C12 C11 C10 118.3(14) . . ? C12 C11 C16 115.9(14) . . ? C16 C11 C10 124.3(13) . . ? C12A C11 C10 114.7(13) . . ? C16A C11 C10 125.3(13) . . ? C16A C11 C12A 120.0 . . ? C11 C16A H16A 120.0 . . ? C11 C16A C15A 120.0 . . ? C15A C16A H16A 120.0 . . ? C16A C15A H15A 120.0 . . ? C14 C15A C16A 120.0 . . ? C14 C15A H15A 120.0 . . ? O007 C14 C15 115.8(13) . . ? O007 C14 C15A 119.0(13) . . ? O007 C14 C13A 120.8(13) . . ? C13 C14 O007 122.9(14) . . ? C13 C14 C15 119.8(13) . . ? C15A C14 C13A 120.0 . . ? C12A C13A H13A 120.0 . . ? C14 C13A C12A 120.0 . . ? C14 C13A H13A 120.0 . . ? 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 S1 C6 1.780(16) . ? S1 C3 1.847(16) . ? O3 C7 1.219(18) . ? O3 Na1 2.485(10) 4_466 ? O1 C1 1.28(2) . ? O1 Na1 2.389(11) . ? O4 C9 1.24(3) . ? O4 Na1 2.356(15) 2_665 ? O2 C1 1.24(2) . ? O2 Na1 2.807(13) . ? O007 Na1 2.447(13) 3_645 ? O007 C14 1.376(12) . ? O007 H007 0.948(12) . ? N1 C7 1.368(16) . ? N1 C2 1.45(2) . ? N1 C6 1.500(19) . ? N2 H2 0.8600 . ? N2 C8 1.423(16) . ? N2 C9 1.34(3) . ? N3 H3A 0.8900 . ? N3 H3B 0.8900 . ? N3 C10 1.45(2) . ? N3 Na1 2.412(16) 2_665 ? C7 C8 1.50(3) . ? C2 H2A 0.9800 . ? C2 C1 1.57(2) . ? C2 C3 1.568(19) . ? C10 H10 0.9800 . ? C10 C9 1.52(2) . ? C10 C11 1.534(15) . ? C8 H8 0.9800 . ? C8 C6 1.530(18) . ? C9 Na1 3.12(3) 2_665 ? C6 H6 0.9800 . ? C3 C4 1.50(2) . ? C3 C5 1.57(2) . ? C12 H12 0.9300 . ? C12 C13 1.367(18) . ? C12 C11 1.37(2) . ? C16 H16 0.9300 . ? C16 C15 1.39(2) . ? C16 C11 1.40(2) . ? C15 H15 0.9300 . ? C15 C14 1.38(2) . ? C13 H13 0.9300 . ? C13 C14 1.36(2) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C12A H12A 0.9300 . ? C12A C11 1.3900 . ? C12A C13A 1.3900 . ? C11 C16A 1.3900 . ? C16A H16A 0.9300 . ? C16A C15A 1.3900 . ? C15A H15A 0.9300 . ? C15A C14 1.3900 . ? C14 C13A 1.3900 . ? C13A H13A 0.9300 . ?