#------------------------------------------------------------------------------ #$Date: 2019-11-17 15:48:35 +0200 (Sun, 17 Nov 2019) $ #$Revision: 230975 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/00/1550029.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_1550029 loop_ _publ_author_name 'Peveler, William J.' 'Packman, Hollie' 'Alexander, Shirin' 'Chauhan, Raamanand R.' 'Hayes, Lilian M.' 'Macdonald, Thomas J.' 'Cockcroft, Jeremy K.' 'Rogers, Sarah' 'Aarts, Dirk G. A. L.' 'Carmalt, Claire J.' 'Parkin, Ivan P.' 'Bear, Joseph C.' _publ_section_title ; A new family of urea-based low molecular-weight organogelators for environmental remediation: the influence of structure. ; _journal_issue 43 _journal_name_full 'Soft matter' _journal_page_first 8821 _journal_page_last 8827 _journal_paper_doi 10.1039/c8sm01682h _journal_volume 14 _journal_year 2018 _chemical_formula_moiety 'C14 H22 N2 O' _chemical_formula_sum 'C14 H22 N2 O' _chemical_formula_weight 234.33 _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' _space_group_name_H-M_alt 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_space_group_name_H-M 'P n a 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2018-03-05 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2018-05-29 deposited with the CCDC. 2018-10-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 16 _cell_length_a 23.0581(13) _cell_length_b 16.6608(12) _cell_length_c 15.1185(10) _cell_measurement_reflns_used 5122 _cell_measurement_temperature 295 _cell_measurement_theta_max 73.1860 _cell_measurement_theta_min 4.3980 _cell_volume 5808.0(7) _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _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 air _diffrn_ambient_temperature 295 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2031 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.970 _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 32.00 1.00 25.00 -- -42.62 38.00 90.00 28 2 \w -89.00 -30.00 1.00 25.00 -- -42.62 125.00-120.00 59 3 \w -113.00 -28.00 1.00 25.00 -- -42.62 -57.00 -60.00 85 4 \w 79.00 178.00 1.00 100.00 -- 106.36 30.00-150.00 99 5 \w 82.00 113.00 1.00 100.00 -- 106.36 77.00 -30.00 31 6 \w 65.00 124.00 1.00 100.00 -- 106.36 -45.00-150.00 59 7 \w 29.00 109.00 1.00 100.00 -- 106.36 -95.00 90.00 80 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0608795717 _diffrn_orient_matrix_UB_12 -0.0375230031 _diffrn_orient_matrix_UB_13 0.0069647926 _diffrn_orient_matrix_UB_21 0.0274354811 _diffrn_orient_matrix_UB_22 -0.0838868052 _diffrn_orient_matrix_UB_23 0.0088315145 _diffrn_orient_matrix_UB_31 0.0017770456 _diffrn_orient_matrix_UB_32 0.0099360078 _diffrn_orient_matrix_UB_33 0.1013336614 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_unetI/netI 0.0527 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.970 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 15196 _diffrn_reflns_point_group_measured_fraction_full 0.774 _diffrn_reflns_point_group_measured_fraction_max 0.738 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.666 _diffrn_reflns_theta_min 3.834 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.530 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.61040 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.072 _exptl_crystal_description needle _exptl_crystal_F_000 2048 _exptl_crystal_size_max 0.347 _exptl_crystal_size_mid 0.091 _exptl_crystal_size_min 0.069 _refine_diff_density_max 1.400 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.109 _refine_ls_abs_structure_details ; Flack x determined using 1216 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.0(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.631 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 633 _refine_ls_number_reflns 8659 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.631 _refine_ls_R_factor_all 0.2145 _refine_ls_R_factor_gt 0.1680 _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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.4150 _refine_ls_wR_factor_ref 0.4677 _reflns_Friedel_coverage 0.464 _reflns_Friedel_fraction_full 0.534 _reflns_Friedel_fraction_max 0.488 _reflns_number_gt 5030 _reflns_number_total 8659 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; exp_1087.res created by SHELXL-2014/7 TITL exp_1087_a.res in Pna2(1) REM Old TITL exp_1087 in Pca21 #29 REM SHELXT solution in Pna2(1) REM R1 0.302, Rweak 0.200, Alpha 0.013, Orientation as input REM Flack x = 0.327 ( 0.140 ) from Parsons' quotients REM Formula found by SHELXT: C51 N11 O7 CELL 1.54184 23.0581 16.6608 15.1185 90 90 90 ZERR 16 0.0013 0.0012 0.001 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,+Z SYMM 0.5-X,0.5+Y,0.5+Z SFAC C H N O UNIT 224 352 32 16 L.S. 50 PLAN 2 TEMP 22 BOND MORE -1 BOND $H CONF list 4 fmap 2 53 acta REM REM REM WGHT 0.200000 FVAR 0.47314 PART 1 O1A 4 0.720697 0.195009 0.059924 11.00000 0.08596 0.05693 = 0.05802 0.00881 0.02135 0.01327 N1A 3 0.672970 0.262588 0.167445 11.00000 0.05026 0.05466 = 0.05093 0.00305 0.01338 0.00645 AFIX 43 H15A 2 0.651230 0.260610 0.213615 11.00000 -1.20000 AFIX 0 N2A 3 0.685907 0.123894 0.175241 11.00000 0.09797 0.06528 = 0.04966 0.01897 0.02402 0.03015 C1A 1 0.758384 0.438772 0.095174 11.00000 0.10437 0.08650 = 0.12588 -0.04400 0.04121 -0.04144 AFIX 43 H1A 2 0.796462 0.457170 0.095694 11.00000 -1.20000 AFIX 0 C2A 1 0.745812 0.365182 0.132127 11.00000 0.06725 0.07739 = 0.07578 -0.01781 0.01301 -0.01176 C3A 1 0.687919 0.339657 0.127891 11.00000 0.04573 0.05439 = 0.06034 -0.00632 0.01172 -0.00368 C4A 1 0.645043 0.386151 0.097776 11.00000 0.08044 0.05005 = 0.07578 0.00050 0.00921 0.01686 AFIX 43 H4A 2 0.606608 0.369738 0.102309 11.00000 -1.20000 AFIX 0 C5A 1 0.659131 0.460313 0.059131 11.00000 0.14774 0.04991 = 0.14101 0.01325 0.06190 0.01798 AFIX 43 H5A 2 0.630427 0.492552 0.034528 11.00000 -1.20000 AFIX 0 C6A 1 0.716871 0.484594 0.058381 11.00000 0.18744 0.05182 = 0.16681 -0.02312 0.09511 -0.02651 AFIX 43 H6A 2 0.726879 0.533126 0.032102 11.00000 -1.20000 AFIX 0 C7A 1 0.792597 0.310747 0.175362 11.00000 0.05450 0.21750 = 0.08950 -0.03860 -0.01100 -0.00014 AFIX 137 H7AA 2 0.775378 0.280284 0.222430 11.00000 -1.50000 H7AB 2 0.823243 0.343527 0.198651 11.00000 -1.50000 H7AC 2 0.808079 0.274792 0.131721 11.00000 -1.50000 AFIX 0 C8A 1 0.694041 0.192756 0.130090 11.00000 0.05620 0.05440 = 0.05354 0.00412 0.01215 0.02146 C9A 1 0.700587 0.046357 0.129958 11.00000 0.12245 0.06361 = 0.10648 0.02058 0.04294 0.02592 AFIX 13 H9A 2 0.688772 0.003517 0.170556 11.00000 -1.20000 AFIX 0 C10A 1 0.667861 0.034113 0.049632 11.00000 0.12316 0.07434 = 0.12139 -0.02247 0.01840 0.00971 AFIX 137 H10A 2 0.627291 0.031020 0.063481 11.00000 -1.50000 H10B 2 0.680008 -0.014985 0.022038 11.00000 -1.50000 H10C 2 0.674532 0.078163 0.009984 11.00000 -1.50000 AFIX 0 C11A 1 0.763495 0.036984 0.117249 11.00000 0.13744 0.10622 = 0.10536 0.02591 0.03692 0.07033 AFIX 137 H11A 2 0.776626 0.074147 0.073047 11.00000 -1.50000 H11B 2 0.771750 -0.016841 0.098402 11.00000 -1.50000 H11C 2 0.783150 0.047531 0.172006 11.00000 -1.50000 AFIX 0 C12A 1 0.666183 0.121450 0.267788 11.00000 0.10188 0.11051 = 0.07211 0.02590 0.01702 0.03623 AFIX 13 H12A 2 0.661028 0.177041 0.287460 11.00000 -1.20000 AFIX 0 C13A 1 0.607311 0.080020 0.274352 11.00000 0.11049 0.12893 = 0.10525 0.03730 0.02356 0.01112 AFIX 137 H13A 2 0.577103 0.119666 0.273532 11.00000 -1.50000 H13B 2 0.605301 0.050094 0.328527 11.00000 -1.50000 H13C 2 0.602495 0.044240 0.225124 11.00000 -1.50000 AFIX 0 C14A 1 0.712078 0.083515 0.326616 11.00000 0.13567 0.16084 = 0.07779 0.05199 -0.02890 0.00861 AFIX 137 H14A 2 0.705697 0.026651 0.329840 11.00000 -1.50000 H14B 2 0.709703 0.106207 0.384871 11.00000 -1.50000 H14C 2 0.749822 0.093729 0.302293 11.00000 -1.50000 AFIX 0 PART 0 PART 2 O1B 4 0.560212 0.279629 0.248130 11.00000 0.04880 0.10092 = 0.04860 -0.01185 0.00399 -0.00576 N1B 3 0.563063 0.289300 0.397463 11.00000 0.04436 0.12640 = 0.04721 -0.00664 -0.00457 -0.00887 AFIX 43 H15B 2 0.544898 0.281421 0.446379 11.00000 -1.20000 AFIX 0 N2B 3 0.476446 0.264925 0.322854 11.00000 0.03721 0.06864 = 0.05368 0.00046 -0.00592 -0.00594 C1B 1 0.698685 0.404144 0.367425 11.00000 0.08323 0.18779 = 0.11490 -0.06589 0.01745 -0.05847 AFIX 43 H1B 2 0.713244 0.449560 0.339389 11.00000 -1.20000 AFIX 0 C2B 1 0.639046 0.386892 0.361400 11.00000 0.05976 0.14390 = 0.09959 -0.07196 0.01904 -0.03725 C3B 1 0.621953 0.313529 0.399405 11.00000 0.05018 0.15303 = 0.04721 -0.04540 -0.01137 -0.01191 C4B 1 0.660666 0.261668 0.441556 11.00000 0.05943 0.15577 = 0.06732 -0.02466 -0.01161 0.00014 AFIX 43 H4B 2 0.646749 0.214278 0.466175 11.00000 -1.20000 AFIX 0 C5B 1 0.718713 0.278863 0.447569 11.00000 0.07223 0.20825 = 0.10234 -0.03235 -0.02345 0.01470 AFIX 43 H5B 2 0.745065 0.242887 0.471996 11.00000 -1.20000 AFIX 0 C6B 1 0.736219 0.354840 0.414299 11.00000 0.06853 0.23229 = 0.12361 -0.08806 -0.01069 -0.02212 AFIX 43 H6B 2 0.774021 0.372079 0.424245 11.00000 -1.20000 AFIX 0 C7B 1 0.598757 0.443334 0.321842 11.00000 0.12156 0.10143 = 0.10242 -0.02354 0.01321 -0.02231 AFIX 137 H7BA 2 0.593600 0.430484 0.260444 11.00000 -1.50000 H7BB 2 0.613917 0.496779 0.327185 11.00000 -1.50000 H7BC 2 0.562095 0.440086 0.351720 11.00000 -1.50000 AFIX 0 C8B 1 0.534759 0.278287 0.319223 11.00000 0.04369 0.06487 = 0.05213 -0.00725 -0.00105 0.00140 C9B 1 0.443527 0.253033 0.238938 11.00000 0.04963 0.06256 = 0.06394 0.00206 -0.01857 -0.00562 AFIX 13 H9B 2 0.402954 0.244679 0.255909 11.00000 -1.20000 AFIX 0 C10B 1 0.444523 0.327071 0.180890 11.00000 0.08888 0.09568 = 0.06306 0.01380 -0.01506 0.00674 AFIX 137 H10D 2 0.438977 0.373970 0.216797 11.00000 -1.50000 H10E 2 0.413990 0.323669 0.137886 11.00000 -1.50000 H10F 2 0.481235 0.330519 0.151180 11.00000 -1.50000 AFIX 0 C11B 1 0.462175 0.178185 0.190323 11.00000 0.07201 0.07461 = 0.09226 -0.02185 -0.00124 -0.01351 AFIX 137 H11D 2 0.497665 0.188538 0.159146 11.00000 -1.50000 H11E 2 0.432584 0.162943 0.148933 11.00000 -1.50000 H11F 2 0.468131 0.135489 0.231984 11.00000 -1.50000 AFIX 0 C12B 1 0.442307 0.265879 0.404093 11.00000 0.04127 0.12863 = 0.05966 -0.00791 0.00429 -0.00230 AFIX 13 H12B 2 0.469636 0.273852 0.452952 11.00000 -1.20000 AFIX 0 C13B 1 0.398747 0.331302 0.410131 11.00000 0.12148 0.16720 = 0.09311 -0.01356 0.03497 0.05845 AFIX 137 H13D 2 0.416487 0.381322 0.393957 11.00000 -1.50000 H13E 2 0.384463 0.334729 0.469655 11.00000 -1.50000 H13F 2 0.367133 0.320150 0.370683 11.00000 -1.50000 AFIX 0 C14B 1 0.412472 0.183178 0.419771 11.00000 0.12254 0.13349 = 0.10139 0.04493 0.03081 -0.02194 AFIX 137 H14D 2 0.386128 0.172220 0.372106 11.00000 -1.50000 H14E 2 0.391477 0.184522 0.474584 11.00000 -1.50000 H14F 2 0.441429 0.141841 0.422282 11.00000 -1.50000 AFIX 0 PART 0 PART 3 O1C 4 0.531652 0.192957 0.557753 11.00000 0.11058 0.07625 = 0.08165 0.00096 -0.03336 -0.00937 N1C 3 0.576479 0.251301 0.669565 11.00000 0.05014 0.09463 = 0.05713 0.01002 -0.01412 -0.00389 AFIX 43 H15C 2 0.598679 0.247053 0.715035 11.00000 -1.20000 AFIX 0 N2C 3 0.567193 0.119186 0.667827 11.00000 0.10451 0.06961 = 0.09784 -0.02242 -0.01645 -0.00127 C1C 1 0.484887 0.433429 0.615384 11.00000 0.11770 0.10965 = 0.16117 0.03954 -0.02042 0.02521 AFIX 43 H1C 2 0.447733 0.452473 0.626898 11.00000 -1.20000 AFIX 0 C2C 1 0.502450 0.356525 0.638852 11.00000 0.07809 0.11175 = 0.09381 0.00701 -0.01669 0.00772 C3C 1 0.558259 0.330243 0.639520 11.00000 0.04498 0.13190 = 0.06997 0.03843 -0.00718 0.01016 C4C 1 0.601178 0.384884 0.602469 11.00000 0.10762 0.08269 = 0.05715 -0.01153 -0.00439 0.00892 AFIX 43 H4C 2 0.639931 0.369538 0.600326 11.00000 -1.20000 AFIX 0 C5C 1 0.584459 0.461559 0.569481 11.00000 0.11415 0.05604 = 0.07510 0.00817 -0.01279 -0.01203 AFIX 43 H5C 2 0.611947 0.496836 0.546784 11.00000 -1.20000 AFIX 0 C6C 1 0.528348 0.481640 0.571902 11.00000 0.26489 0.07534 = 0.12763 -0.02899 -0.07370 0.03216 AFIX 43 H6C 2 0.516793 0.528879 0.544276 11.00000 -1.20000 AFIX 0 C7C 1 0.456207 0.304265 0.678187 11.00000 0.07155 0.22869 = 0.13917 -0.02184 -0.00209 -0.02494 AFIX 137 H7CA 2 0.446442 0.262354 0.637236 11.00000 -1.50000 H7CB 2 0.422385 0.336017 0.690301 11.00000 -1.50000 H7CC 2 0.470189 0.280968 0.732207 11.00000 -1.50000 AFIX 0 C8C 1 0.558921 0.185017 0.626886 11.00000 0.04812 0.10221 = 0.06090 0.02541 -0.01091 -0.01000 C9C 1 0.551959 0.043339 0.622172 11.00000 0.15996 0.06315 = 0.10318 -0.01981 -0.02498 -0.00005 AFIX 13 H9C 2 0.562066 -0.000894 0.662024 11.00000 -1.20000 AFIX 0 C10C 1 0.492566 0.036764 0.603287 11.00000 0.16165 0.09705 = 0.19338 -0.01441 -0.08752 -0.03732 AFIX 137 H10G 2 0.475356 -0.002425 0.641731 11.00000 -1.50000 H10H 2 0.487548 0.020428 0.542877 11.00000 -1.50000 H10I 2 0.474161 0.087793 0.612333 11.00000 -1.50000 AFIX 0 C11C 1 0.591154 0.035870 0.539155 11.00000 0.24826 0.06821 = 0.05823 -0.00174 0.00947 0.07430 AFIX 137 H11G 2 0.567503 0.036849 0.486908 11.00000 -1.50000 H11H 2 0.612230 -0.013774 0.541558 11.00000 -1.50000 H11I 2 0.617979 0.079915 0.537636 11.00000 -1.50000 AFIX 0 C12C 1 0.585678 0.113236 0.764256 11.00000 0.13003 0.06879 = 0.08116 0.01427 -0.02324 -0.01115 AFIX 13 H12C 2 0.592412 0.168098 0.785257 11.00000 -1.20000 AFIX 0 C13C 1 0.544941 0.073565 0.829593 11.00000 0.18702 0.11576 = 0.13470 -0.02559 0.07160 -0.02916 AFIX 137 H13G 2 0.517633 0.112432 0.851109 11.00000 -1.50000 H13H 2 0.566876 0.052419 0.878274 11.00000 -1.50000 H13I 2 0.524498 0.030705 0.800801 11.00000 -1.50000 AFIX 0 C14C 1 0.646042 0.065162 0.774896 11.00000 0.16523 0.13537 = 0.07385 -0.00091 -0.01108 -0.01520 AFIX 137 H14G 2 0.649435 0.026155 0.728447 11.00000 -1.50000 H14H 2 0.646777 0.038482 0.831166 11.00000 -1.50000 H14I 2 0.677821 0.102253 0.771403 11.00000 -1.50000 AFIX 0 PART 0 PART 4 O1D 4 0.689627 0.273218 0.750067 11.00000 0.06217 0.16341 = 0.05732 0.00044 -0.01527 0.00788 N1D 3 0.686850 0.282583 0.899052 11.00000 0.07213 0.09421 = 0.06217 0.01351 -0.00327 -0.00409 AFIX 43 H15D 2 0.705903 0.276999 0.947565 11.00000 -1.20000 AFIX 0 N2D 3 0.773926 0.253825 0.822665 11.00000 0.04010 0.12415 = 0.04894 0.01419 0.00322 0.00167 C1D 1 0.547177 0.394830 0.869080 11.00000 0.08231 0.13397 = 0.11913 -0.02981 0.03833 0.01498 AFIX 43 H1D 2 0.532629 0.439125 0.838932 11.00000 -1.20000 AFIX 0 C2D 1 0.609310 0.376841 0.865742 11.00000 0.09549 0.11206 = 0.06999 -0.01721 -0.02141 0.03162 C3D 1 0.627519 0.301678 0.903378 11.00000 0.06659 0.09651 = 0.08535 -0.01643 -0.01120 -0.00419 C4D 1 0.588805 0.244771 0.943640 11.00000 0.07221 0.25795 = 0.04158 0.00553 0.01432 -0.04545 AFIX 43 H4D 2 0.599357 0.193839 0.962993 11.00000 -1.20000 AFIX 0 C5D 1 0.528623 0.279635 0.949938 11.00000 0.08141 0.22522 = 0.11756 -0.04398 0.02762 -0.05782 AFIX 43 H5D 2 0.500736 0.250826 0.981036 11.00000 -1.20000 AFIX 0 C6D 1 0.512822 0.349776 0.913368 11.00000 0.08926 0.15907 = 0.14442 -0.02581 -0.00893 0.03958 AFIX 43 H6D 2 0.474665 0.366614 0.920648 11.00000 -1.20000 AFIX 0 C7D 1 0.647775 0.427772 0.819447 11.00000 0.08898 0.09193 = 0.14200 0.02891 0.01466 0.01009 AFIX 137 H7DA 2 0.684642 0.428498 0.848939 11.00000 -1.50000 H7DB 2 0.632126 0.481146 0.817783 11.00000 -1.50000 H7DC 2 0.652689 0.408275 0.760166 11.00000 -1.50000 AFIX 0 C8D 1 0.715228 0.272614 0.820868 11.00000 0.05802 0.10664 = 0.05651 0.00283 0.00366 -0.00217 C9D 1 0.806005 0.248894 0.739963 11.00000 0.04090 0.08781 = 0.05510 -0.00601 0.00134 -0.00028 AFIX 13 H9D 2 0.847093 0.245144 0.756016 11.00000 -1.20000 AFIX 0 C10D 1 0.791830 0.173327 0.688885 11.00000 0.11685 0.09478 = 0.09786 -0.03835 -0.01027 -0.00836 AFIX 137 H10J 2 0.782611 0.130939 0.729532 11.00000 -1.50000 H10K 2 0.824694 0.158000 0.653748 11.00000 -1.50000 H10L 2 0.759192 0.183086 0.650958 11.00000 -1.50000 AFIX 0 C11D 1 0.799624 0.324704 0.684859 11.00000 0.11623 0.10244 = 0.04564 0.00626 0.00272 0.00743 AFIX 137 H11J 2 0.801628 0.311236 0.623195 11.00000 -1.50000 H11K 2 0.830316 0.361381 0.699248 11.00000 -1.50000 H11L 2 0.762897 0.349367 0.697336 11.00000 -1.50000 AFIX 0 C12D 1 0.808511 0.257887 0.906585 11.00000 0.04673 0.16689 = 0.03903 -0.00015 -0.00871 -0.00229 AFIX 13 H12D 2 0.781251 0.264588 0.955765 11.00000 -1.20000 AFIX 0 C13D 1 0.839625 0.180930 0.919890 11.00000 0.09976 0.19538 = 0.10947 0.06350 -0.02407 0.00713 AFIX 137 H13J 2 0.819755 0.138899 0.888774 11.00000 -1.50000 H13K 2 0.840787 0.168437 0.981853 11.00000 -1.50000 H13L 2 0.878475 0.185636 0.897658 11.00000 -1.50000 AFIX 0 C14D 1 0.850037 0.332240 0.906073 11.00000 0.13949 0.18222 = 0.09627 -0.01596 -0.03238 -0.05633 AFIX 137 H14J 2 0.873988 0.330601 0.854165 11.00000 -1.50000 H14K 2 0.874118 0.331049 0.957856 11.00000 -1.50000 H14L 2 0.827467 0.380659 0.905885 11.00000 -1.50000 AFIX 0 HKLF 4 REM exp_1087_a.res in Pna2(1) REM R1 = 0.1680 for 5030 Fo > 4sig(Fo) and 0.2145 for all 8659 data REM 633 parameters refined using 1 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.400, deepest hole -0.443, 1-sigma level 0.109 Q1 1 0.5251 0.2997 0.5635 11.00000 0.05 1.40 Q2 1 0.6913 0.2035 0.7392 11.00000 0.05 0.96 REM The information below was added by Olex2. REM REM R1 = 0.1680 for 5030 Fo > 4sig(Fo) and 0.2145 for all 15781 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.40, deepest hole -0.44 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.2145 REM R1_gt = 0.1680 REM wR_ref = 0.4677 REM GOOF = 1.631 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 15781 REM Reflections_gt = 5030 REM Parameters = n/a REM Hole = -0.44 REM Peak = 1.40 REM Flack = -0.0(2) ; _cod_data_source_file c8sm01682h2.cif _cod_data_source_block exp_1087 _cod_depositor_comments 'Adding full bibliography for 1550029--1550031.cif.' _cod_database_code 1550029 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula 'C14 H22 N2 O' _chemical_oxdiff_usercomment 'Molecule 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. ; _reflns_odcompleteness_completeness 99.54 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.49 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C9A(H9A), C12A(H12A), C9B(H9B), C12B(H12B), C9C(H9C), C12C(H12C), C9D(H9D), C12D(H12D) 2.b Aromatic/amide H refined with riding coordinates: N1A(H15A), C1A(H1A), C4A(H4A), C5A(H5A), C6A(H6A), N1B(H15B), C1B(H1B), C4B(H4B), C5B(H5B), C6B(H6B), N1C(H15C), C1C(H1C), C4C(H4C), C5C(H5C), C6C(H6C), N1D(H15D), C1D(H1D), C4D(H4D), C5D(H5D), C6D(H6D) 2.c Idealised Me refined as rotating group: C7A(H7AA,H7AB,H7AC), C10A(H10A,H10B,H10C), C11A(H11A,H11B,H11C), C13A(H13A, H13B,H13C), C14A(H14A,H14B,H14C), C7B(H7BA,H7BB,H7BC), C10B(H10D,H10E,H10F), C11B(H11D,H11E,H11F), C13B(H13D,H13E,H13F), C14B(H14D,H14E,H14F), C7C(H7CA, H7CB,H7CC), C10C(H10G,H10H,H10I), C11C(H11G,H11H,H11I), C13C(H13G,H13H,H13I), C14C(H14G,H14H,H14I), C7D(H7DA,H7DB,H7DC), C10D(H10J,H10K,H10L), C11D(H11J, H11K,H11L), C13D(H13J,H13K,H13L), C14D(H14J,H14K,H14L) ; _olex2_date_sample_data_collection 2017-09-19 _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 1.551 _oxdiff_exptl_absorpt_empirical_full_min 0.404 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' 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_disorder_assembly _atom_site_disorder_group O1A O 0.7207(3) 0.1950(4) 0.0599(5) 0.0670(17) Uani 1 1 d . A 1 N1A N 0.6730(3) 0.2626(4) 0.1674(5) 0.0520(16) Uani 1 1 d . A 1 H15A H 0.6512 0.2606 0.2136 0.062 Uiso 1 1 calc R A 1 N2A N 0.6859(4) 0.1239(5) 0.1752(6) 0.071(2) Uani 1 1 d . A 1 C1A C 0.7584(7) 0.4388(9) 0.0952(12) 0.106(5) Uani 1 1 d . A 1 H1A H 0.7965 0.4572 0.0957 0.127 Uiso 1 1 calc R A 1 C2A C 0.7458(4) 0.3652(7) 0.1321(8) 0.073(3) Uani 1 1 d . A 1 C3A C 0.6879(3) 0.3397(5) 0.1279(6) 0.0535(19) Uani 1 1 d . A 1 C4A C 0.6450(5) 0.3862(5) 0.0978(8) 0.069(3) Uani 1 1 d . A 1 H4A H 0.6066 0.3697 0.1023 0.083 Uiso 1 1 calc R A 1 C5A C 0.6591(7) 0.4603(7) 0.0591(13) 0.113(6) Uani 1 1 d . A 1 H5A H 0.6304 0.4926 0.0345 0.135 Uiso 1 1 calc R A 1 C6A C 0.7169(10) 0.4846(8) 0.0584(15) 0.135(8) Uani 1 1 d . A 1 H6A H 0.7269 0.5331 0.0321 0.162 Uiso 1 1 calc R A 1 C7A C 0.7926(5) 0.3107(12) 0.1754(11) 0.120(6) Uani 1 1 d . A 1 H7AA H 0.7754 0.2803 0.2224 0.181 Uiso 1 1 calc GR A 1 H7AB H 0.8232 0.3435 0.1987 0.181 Uiso 1 1 calc GR A 1 H7AC H 0.8081 0.2748 0.1317 0.181 Uiso 1 1 calc GR A 1 C8A C 0.6940(3) 0.1928(5) 0.1301(7) 0.055(2) Uani 1 1 d . A 1 C9A C 0.7006(6) 0.0464(7) 0.1300(11) 0.098(4) Uani 1 1 d . A 1 H9A H 0.6888 0.0035 0.1706 0.117 Uiso 1 1 calc R A 1 C10A C 0.6679(7) 0.0341(8) 0.0496(12) 0.106(5) Uani 1 1 d . A 1 H10A H 0.6273 0.0310 0.0635 0.159 Uiso 1 1 calc GR A 1 H10B H 0.6800 -0.0150 0.0220 0.159 Uiso 1 1 calc GR A 1 H10C H 0.6745 0.0782 0.0100 0.159 Uiso 1 1 calc GR A 1 C11A C 0.7635(7) 0.0370(9) 0.1172(12) 0.116(6) Uani 1 1 d . A 1 H11A H 0.7766 0.0741 0.0730 0.175 Uiso 1 1 calc GR A 1 H11B H 0.7718 -0.0168 0.0984 0.175 Uiso 1 1 calc GR A 1 H11C H 0.7832 0.0475 0.1720 0.175 Uiso 1 1 calc GR A 1 C12A C 0.6662(6) 0.1215(9) 0.2678(9) 0.095(4) Uani 1 1 d . A 1 H12A H 0.6610 0.1770 0.2875 0.114 Uiso 1 1 calc R A 1 C13A C 0.6073(7) 0.0800(11) 0.2744(12) 0.115(5) Uani 1 1 d . A 1 H13A H 0.5771 0.1197 0.2735 0.172 Uiso 1 1 calc GR A 1 H13B H 0.6053 0.0501 0.3285 0.172 Uiso 1 1 calc GR A 1 H13C H 0.6025 0.0442 0.2251 0.172 Uiso 1 1 calc GR A 1 C14A C 0.7121(7) 0.0835(12) 0.3266(11) 0.125(6) Uani 1 1 d . A 1 H14A H 0.7057 0.0267 0.3298 0.187 Uiso 1 1 calc GR A 1 H14B H 0.7097 0.1062 0.3849 0.187 Uiso 1 1 calc GR A 1 H14C H 0.7498 0.0937 0.3023 0.187 Uiso 1 1 calc GR A 1 O1B O 0.5602(2) 0.2796(5) 0.2481(4) 0.0661(18) Uani 1 1 d . B 2 N1B N 0.5631(3) 0.2893(6) 0.3975(6) 0.073(2) Uani 1 1 d . B 2 H15B H 0.5449 0.2814 0.4464 0.087 Uiso 1 1 calc R B 2 N2B N 0.4764(3) 0.2649(4) 0.3229(5) 0.0532(16) Uani 1 1 d . B 2 C1B C 0.6987(6) 0.4041(13) 0.3674(13) 0.129(7) Uani 1 1 d . B 2 H1B H 0.7132 0.4496 0.3394 0.154 Uiso 1 1 calc R B 2 C2B C 0.6390(5) 0.3869(10) 0.3614(10) 0.101(5) Uani 1 1 d . B 2 C3B C 0.6220(4) 0.3135(9) 0.3994(7) 0.083(4) Uani 1 1 d . B 2 C4B C 0.6607(5) 0.2617(11) 0.4416(9) 0.094(4) Uani 1 1 d . B 2 H4B H 0.6467 0.2143 0.4662 0.113 Uiso 1 1 calc R B 2 C5B C 0.7187(7) 0.2789(16) 0.4476(13) 0.128(7) Uani 1 1 d . B 2 H5B H 0.7451 0.2429 0.4720 0.153 Uiso 1 1 calc R B 2 C6B C 0.7362(6) 0.3548(16) 0.4143(14) 0.141(9) Uani 1 1 d . B 2 H6B H 0.7740 0.3721 0.4242 0.170 Uiso 1 1 calc R B 2 C7B C 0.5988(7) 0.4433(9) 0.3218(12) 0.108(4) Uani 1 1 d . B 2 H7BA H 0.5936 0.4305 0.2604 0.163 Uiso 1 1 calc GR B 2 H7BB H 0.6139 0.4968 0.3272 0.163 Uiso 1 1 calc GR B 2 H7BC H 0.5621 0.4401 0.3517 0.163 Uiso 1 1 calc GR B 2 C8B C 0.5348(3) 0.2783(5) 0.3192(7) 0.0536(18) Uani 1 1 d . B 2 C9B C 0.4435(4) 0.2530(5) 0.2389(7) 0.059(2) Uani 1 1 d . B 2 H9B H 0.4030 0.2447 0.2559 0.070 Uiso 1 1 calc R B 2 C10B C 0.4445(5) 0.3271(8) 0.1809(8) 0.083(3) Uani 1 1 d . B 2 H10D H 0.4390 0.3740 0.2168 0.124 Uiso 1 1 calc GR B 2 H10E H 0.4140 0.3237 0.1379 0.124 Uiso 1 1 calc GR B 2 H10F H 0.4812 0.3305 0.1512 0.124 Uiso 1 1 calc GR B 2 C11B C 0.4622(5) 0.1782(7) 0.1903(10) 0.080(3) Uani 1 1 d . B 2 H11D H 0.4977 0.1885 0.1591 0.119 Uiso 1 1 calc GR B 2 H11E H 0.4326 0.1629 0.1489 0.119 Uiso 1 1 calc GR B 2 H11F H 0.4681 0.1355 0.2320 0.119 Uiso 1 1 calc GR B 2 C12B C 0.4423(4) 0.2659(8) 0.4041(8) 0.077(3) Uani 1 1 d . B 2 H12B H 0.4696 0.2739 0.4530 0.092 Uiso 1 1 calc R B 2 C13B C 0.3987(7) 0.3313(12) 0.4101(12) 0.127(6) Uani 1 1 d . B 2 H13D H 0.4165 0.3813 0.3940 0.191 Uiso 1 1 calc GR B 2 H13E H 0.3845 0.3347 0.4697 0.191 Uiso 1 1 calc GR B 2 H13F H 0.3671 0.3201 0.3707 0.191 Uiso 1 1 calc GR B 2 C14B C 0.4125(8) 0.1832(11) 0.4198(12) 0.119(6) Uani 1 1 d . B 2 H14D H 0.3861 0.1722 0.3721 0.179 Uiso 1 1 calc GR B 2 H14E H 0.3915 0.1845 0.4746 0.179 Uiso 1 1 calc GR B 2 H14F H 0.4414 0.1418 0.4223 0.179 Uiso 1 1 calc GR B 2 O1C O 0.5317(4) 0.1930(5) 0.5578(6) 0.089(2) Uani 1 1 d . C 3 N1C N 0.5765(3) 0.2513(5) 0.6696(6) 0.067(2) Uani 1 1 d . C 3 H15C H 0.5987 0.2471 0.7150 0.081 Uiso 1 1 calc R C 3 N2C N 0.5672(5) 0.1192(6) 0.6678(8) 0.091(3) Uani 1 1 d . C 3 C1C C 0.4849(8) 0.4334(11) 0.6154(15) 0.130(7) Uani 1 1 d . C 3 H1C H 0.4477 0.4525 0.6269 0.155 Uiso 1 1 calc R C 3 C2C C 0.5025(5) 0.3565(9) 0.6389(10) 0.095(4) Uani 1 1 d . C 3 C3C C 0.5583(4) 0.3302(8) 0.6395(8) 0.082(3) Uani 1 1 d . C 3 C4C C 0.6012(6) 0.3849(7) 0.6025(8) 0.082(3) Uani 1 1 d . C 3 H4C H 0.6399 0.3695 0.6003 0.099 Uiso 1 1 calc R C 3 C5C C 0.5845(6) 0.4616(7) 0.5695(9) 0.082(3) Uani 1 1 d . C 3 H5C H 0.6119 0.4968 0.5468 0.098 Uiso 1 1 calc R C 3 C6C C 0.5283(13) 0.4816(10) 0.5719(16) 0.156(10) Uani 1 1 d . C 3 H6C H 0.5168 0.5289 0.5443 0.187 Uiso 1 1 calc R C 3 C7C C 0.4562(6) 0.3043(14) 0.6782(14) 0.146(8) Uani 1 1 d . C 3 H7CA H 0.4464 0.2624 0.6372 0.220 Uiso 1 1 calc GR C 3 H7CB H 0.4224 0.3360 0.6903 0.220 Uiso 1 1 calc GR C 3 H7CC H 0.4702 0.2810 0.7322 0.220 Uiso 1 1 calc GR C 3 C8C C 0.5589(4) 0.1850(7) 0.6269(8) 0.070(3) Uani 1 1 d . C 3 C9C C 0.5520(8) 0.0433(8) 0.6222(12) 0.109(5) Uani 1 1 d . C 3 H9C H 0.5621 -0.0009 0.6620 0.131 Uiso 1 1 calc R C 3 C10C C 0.4926(9) 0.0368(10) 0.6033(17) 0.151(9) Uani 1 1 d . C 3 H10G H 0.4754 -0.0024 0.6417 0.226 Uiso 1 1 calc GR C 3 H10H H 0.4875 0.0204 0.5429 0.226 Uiso 1 1 calc GR C 3 H10I H 0.4742 0.0878 0.6123 0.226 Uiso 1 1 calc GR C 3 C11C C 0.5912(9) 0.0359(8) 0.5392(9) 0.125(7) Uani 1 1 d . C 3 H11G H 0.5675 0.0368 0.4869 0.187 Uiso 1 1 calc GR C 3 H11H H 0.6122 -0.0138 0.5416 0.187 Uiso 1 1 calc GR C 3 H11I H 0.6180 0.0799 0.5376 0.187 Uiso 1 1 calc GR C 3 C12C C 0.5857(6) 0.1132(7) 0.7643(10) 0.093(4) Uani 1 1 d . C 3 H12C H 0.5924 0.1681 0.7853 0.112 Uiso 1 1 calc R C 3 C13C C 0.5449(9) 0.0736(11) 0.8296(15) 0.146(8) Uani 1 1 d . C 3 H13G H 0.5176 0.1124 0.8511 0.219 Uiso 1 1 calc GR C 3 H13H H 0.5669 0.0524 0.8783 0.219 Uiso 1 1 calc GR C 3 H13I H 0.5245 0.0307 0.8008 0.219 Uiso 1 1 calc GR C 3 C14C C 0.6460(8) 0.0652(12) 0.7749(11) 0.125(6) Uani 1 1 d . C 3 H14G H 0.6494 0.0262 0.7284 0.187 Uiso 1 1 calc GR C 3 H14H H 0.6468 0.0385 0.8312 0.187 Uiso 1 1 calc GR C 3 H14I H 0.6778 0.1023 0.7714 0.187 Uiso 1 1 calc GR C 3 O1D O 0.6896(3) 0.2732(7) 0.7501(5) 0.094(3) Uani 1 1 d . D 4 N1D N 0.6869(3) 0.2826(6) 0.8991(7) 0.076(2) Uani 1 1 d . D 4 H15D H 0.7059 0.2770 0.9476 0.091 Uiso 1 1 calc R D 4 N2D N 0.7739(3) 0.2538(6) 0.8227(6) 0.071(2) Uani 1 1 d . D 4 C1D C 0.5472(6) 0.3948(11) 0.8691(12) 0.112(5) Uani 1 1 d . D 4 H1D H 0.5326 0.4391 0.8389 0.134 Uiso 1 1 calc R D 4 C2D C 0.6093(5) 0.3768(9) 0.8657(9) 0.093(4) Uani 1 1 d . D 4 C3D C 0.6275(4) 0.3017(7) 0.9034(9) 0.083(3) Uani 1 1 d . D 4 C4D C 0.5888(6) 0.2448(15) 0.9436(8) 0.124(7) Uani 1 1 d . D 4 H4D H 0.5994 0.1938 0.9630 0.149 Uiso 1 1 calc R D 4 C5D C 0.5286(7) 0.2796(17) 0.9499(14) 0.141(9) Uani 1 1 d . D 4 H5D H 0.5007 0.2508 0.9810 0.170 Uiso 1 1 calc R D 4 C6D C 0.5128(7) 0.3498(14) 0.9134(16) 0.131(7) Uani 1 1 d . D 4 H6D H 0.4747 0.3666 0.9206 0.157 Uiso 1 1 calc R D 4 C7D C 0.6478(6) 0.4278(8) 0.8194(13) 0.108(5) Uani 1 1 d . D 4 H7DA H 0.6846 0.4285 0.8489 0.161 Uiso 1 1 calc GR D 4 H7DB H 0.6321 0.4811 0.8178 0.161 Uiso 1 1 calc GR D 4 H7DC H 0.6527 0.4083 0.7602 0.161 Uiso 1 1 calc GR D 4 C8D C 0.7152(4) 0.2726(8) 0.8209(8) 0.074(3) Uani 1 1 d . D 4 C9D C 0.8060(4) 0.2489(6) 0.7400(7) 0.061(2) Uani 1 1 d . D 4 H9D H 0.8471 0.2451 0.7560 0.074 Uiso 1 1 calc R D 4 C10D C 0.7918(6) 0.1733(8) 0.6889(11) 0.103(4) Uani 1 1 d . D 4 H10J H 0.7826 0.1309 0.7295 0.155 Uiso 1 1 calc GR D 4 H10K H 0.8247 0.1580 0.6537 0.155 Uiso 1 1 calc GR D 4 H10L H 0.7592 0.1831 0.6510 0.155 Uiso 1 1 calc GR D 4 C11D C 0.7996(6) 0.3247(8) 0.6849(8) 0.088(3) Uani 1 1 d . D 4 H11J H 0.8016 0.3112 0.6232 0.132 Uiso 1 1 calc GR D 4 H11K H 0.8303 0.3614 0.6992 0.132 Uiso 1 1 calc GR D 4 H11L H 0.7629 0.3494 0.6973 0.132 Uiso 1 1 calc GR D 4 C12D C 0.8085(4) 0.2579(9) 0.9066(7) 0.084(4) Uani 1 1 d . D 4 H12D H 0.7813 0.2646 0.9558 0.101 Uiso 1 1 calc R D 4 C13D C 0.8396(7) 0.1809(13) 0.9199(13) 0.135(7) Uani 1 1 d . D 4 H13J H 0.8198 0.1389 0.8888 0.202 Uiso 1 1 calc GR D 4 H13K H 0.8408 0.1684 0.9819 0.202 Uiso 1 1 calc GR D 4 H13L H 0.8785 0.1856 0.8977 0.202 Uiso 1 1 calc GR D 4 C14D C 0.8500(8) 0.3322(13) 0.9061(13) 0.139(7) Uani 1 1 d . D 4 H14J H 0.8740 0.3306 0.8542 0.209 Uiso 1 1 calc GR D 4 H14K H 0.8741 0.3310 0.9579 0.209 Uiso 1 1 calc GR D 4 H14L H 0.8275 0.3807 0.9059 0.209 Uiso 1 1 calc GR D 4 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 O1A 0.086(4) 0.057(3) 0.058(4) 0.009(3) 0.021(3) 0.013(3) N1A 0.050(3) 0.055(4) 0.051(4) 0.003(3) 0.013(3) 0.006(3) N2A 0.098(5) 0.065(5) 0.050(5) 0.019(4) 0.024(4) 0.030(4) C1A 0.104(9) 0.086(8) 0.126(13) -0.044(9) 0.041(9) -0.041(8) C2A 0.067(5) 0.077(6) 0.076(7) -0.018(6) 0.013(5) -0.012(4) C3A 0.046(4) 0.054(4) 0.060(5) -0.006(4) 0.012(4) -0.004(3) C4A 0.080(6) 0.050(4) 0.076(7) 0.000(5) 0.009(5) 0.017(4) C5A 0.148(12) 0.050(5) 0.141(14) 0.013(7) 0.062(11) 0.018(7) C6A 0.187(17) 0.052(6) 0.167(19) -0.023(9) 0.095(15) -0.027(9) C7A 0.054(5) 0.218(19) 0.089(10) -0.039(12) -0.011(6) 0.000(8) C8A 0.056(4) 0.054(4) 0.054(5) 0.004(4) 0.012(4) 0.021(3) C9A 0.122(9) 0.064(6) 0.106(11) 0.021(7) 0.043(9) 0.026(6) C10A 0.123(11) 0.074(7) 0.121(13) -0.022(8) 0.018(10) 0.010(7) C11A 0.137(11) 0.106(9) 0.105(12) 0.026(9) 0.037(10) 0.070(9) C12A 0.102(8) 0.111(9) 0.072(8) 0.026(7) 0.017(7) 0.036(7) C13A 0.110(10) 0.129(12) 0.105(12) 0.037(10) 0.024(9) 0.011(9) C14A 0.136(11) 0.161(15) 0.078(9) 0.052(11) -0.029(9) 0.009(10) O1B 0.049(3) 0.101(5) 0.049(4) -0.012(4) 0.004(3) -0.006(3) N1B 0.044(3) 0.126(7) 0.047(4) -0.007(5) -0.005(3) -0.009(4) N2B 0.037(3) 0.069(4) 0.054(4) 0.000(4) -0.006(3) -0.006(2) C1B 0.083(8) 0.188(17) 0.115(13) -0.066(13) 0.017(9) -0.058(10) C2B 0.060(5) 0.144(12) 0.100(10) -0.072(9) 0.019(6) -0.037(7) C3B 0.050(4) 0.153(11) 0.047(6) -0.045(7) -0.011(4) -0.012(6) C4B 0.059(6) 0.156(13) 0.067(7) -0.025(8) -0.012(6) 0.000(6) C5B 0.072(8) 0.21(2) 0.102(13) -0.032(14) -0.023(8) 0.015(11) C6B 0.069(7) 0.23(2) 0.124(15) -0.088(17) -0.011(9) -0.022(11) C7B 0.122(10) 0.101(9) 0.102(11) -0.024(9) 0.013(10) -0.022(8) C8B 0.044(3) 0.065(5) 0.052(5) -0.007(4) -0.001(4) 0.001(3) C9B 0.050(4) 0.063(5) 0.064(6) 0.002(4) -0.019(4) -0.006(3) C10B 0.089(7) 0.096(8) 0.063(7) 0.014(6) -0.015(6) 0.007(6) C11B 0.072(5) 0.075(6) 0.092(8) -0.022(6) -0.001(6) -0.014(5) C12B 0.041(4) 0.129(9) 0.060(6) -0.008(7) 0.004(4) -0.002(4) C13B 0.121(10) 0.167(15) 0.093(11) -0.014(11) 0.035(10) 0.058(10) C14B 0.123(11) 0.133(12) 0.101(12) 0.045(10) 0.031(9) -0.022(9) O1C 0.111(5) 0.076(4) 0.082(6) 0.001(4) -0.033(5) -0.009(4) N1C 0.050(4) 0.095(6) 0.057(5) 0.010(4) -0.014(4) -0.004(3) N2C 0.105(7) 0.070(6) 0.098(8) -0.022(6) -0.016(6) -0.001(5) C1C 0.118(11) 0.110(11) 0.161(19) 0.040(12) -0.020(12) 0.025(9) C2C 0.078(7) 0.112(10) 0.094(10) 0.007(8) -0.017(7) 0.008(6) C3C 0.045(4) 0.132(9) 0.070(7) 0.038(7) -0.007(4) 0.010(5) C4C 0.108(8) 0.083(7) 0.057(6) -0.012(6) -0.004(6) 0.009(6) C5C 0.114(8) 0.056(5) 0.075(8) 0.008(5) -0.013(7) -0.012(5) C6C 0.26(3) 0.075(9) 0.128(17) -0.029(10) -0.074(19) 0.032(13) C7C 0.072(7) 0.23(2) 0.139(16) -0.022(16) -0.002(9) -0.025(10) C8C 0.048(4) 0.102(8) 0.061(6) 0.025(6) -0.011(4) -0.010(4) C9C 0.160(13) 0.063(6) 0.103(12) -0.020(7) -0.025(10) 0.000(7) C10C 0.162(15) 0.097(10) 0.19(2) -0.014(13) -0.088(16) -0.037(10) C11C 0.25(2) 0.068(7) 0.058(7) -0.002(6) 0.009(10) 0.074(10) C12C 0.130(10) 0.069(7) 0.081(9) 0.014(6) -0.023(8) -0.011(6) C13C 0.187(17) 0.116(12) 0.135(17) -0.026(12) 0.072(15) -0.029(12) C14C 0.165(15) 0.135(13) 0.074(10) -0.001(10) -0.011(10) -0.015(12) O1D 0.062(4) 0.163(8) 0.057(5) 0.000(5) -0.015(4) 0.008(4) N1D 0.072(5) 0.094(6) 0.062(5) 0.014(5) -0.003(5) -0.004(4) N2D 0.040(3) 0.124(7) 0.049(4) 0.014(5) 0.003(3) 0.002(3) C1D 0.082(7) 0.134(12) 0.119(13) -0.030(10) 0.038(8) 0.015(8) C2D 0.095(8) 0.112(10) 0.070(8) -0.017(7) -0.021(6) 0.032(7) C3D 0.067(5) 0.097(8) 0.085(8) -0.016(7) -0.011(6) -0.004(5) C4D 0.072(7) 0.26(2) 0.042(6) 0.006(9) 0.014(6) -0.045(9) C5D 0.081(9) 0.23(2) 0.118(15) -0.044(16) 0.028(9) -0.058(13) C6D 0.089(10) 0.159(17) 0.144(18) -0.026(15) -0.009(11) 0.040(11) C7D 0.089(7) 0.092(8) 0.142(14) 0.029(10) 0.015(9) 0.010(6) C8D 0.058(5) 0.107(8) 0.057(6) 0.003(6) 0.004(5) -0.002(5) C9D 0.041(4) 0.088(6) 0.055(6) -0.006(5) 0.001(4) 0.000(3) C10D 0.117(9) 0.095(8) 0.098(10) -0.038(8) -0.010(8) -0.008(7) C11D 0.116(9) 0.102(8) 0.046(6) 0.006(6) 0.003(6) 0.007(7) C12D 0.047(4) 0.167(12) 0.039(5) 0.000(7) -0.009(4) -0.002(5) C13D 0.100(9) 0.195(19) 0.109(13) 0.063(14) -0.024(9) 0.007(11) C14D 0.139(13) 0.182(18) 0.096(12) -0.016(13) -0.032(11) -0.056(13) 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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -14 4 0 0.0344 -4 0 -9 0.1626 5 10 0 0.0297 0 0 10 0.1631 -6 -10 0 0.0329 2 -11 0 0.0478 7 -9 0 0.0493 14 -4 0 0.0541 12 6 0 0.0362 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C3A N1A H15A 120.3 C8A N1A H15A 120.3 C8A N1A C3A 119.4(7) C8A N2A C9A 118.0(8) C8A N2A C12A 123.2(9) C12A N2A C9A 118.7(9) C2A C1A H1A 119.2 C6A C1A H1A 119.2 C6A C1A C2A 121.5(12) C1A C2A C3A 116.8(12) C1A C2A C7A 122.9(12) C3A C2A C7A 120.2(11) C2A C3A N1A 118.3(8) C4A C3A N1A 118.4(7) C4A C3A C2A 123.0(9) C3A C4A H4A 120.6 C3A C4A C5A 118.7(11) C5A C4A H4A 120.6 C4A C5A H5A 120.6 C6A C5A C4A 118.7(16) C6A C5A H5A 120.6 C1A C6A C5A 120.8(13) C1A C6A H6A 119.6 C5A C6A H6A 119.6 C2A C7A H7AA 109.5 C2A C7A H7AB 109.5 C2A C7A H7AC 109.5 H7AA C7A H7AB 109.5 H7AA C7A H7AC 109.5 H7AB C7A H7AC 109.5 O1A C8A N1A 120.3(8) O1A C8A N2A 122.3(7) N2A C8A N1A 117.4(8) N2A C9A H9A 106.2 C10A C9A N2A 112.8(11) C10A C9A H9A 106.2 C10A C9A C11A 113.0(13) C11A C9A N2A 111.9(13) C11A C9A H9A 106.2 C9A C10A H10A 109.5 C9A C10A H10B 109.5 C9A C10A H10C 109.5 H10A C10A H10B 109.5 H10A C10A H10C 109.5 H10B C10A H10C 109.5 C9A C11A H11A 109.5 C9A C11A H11B 109.5 C9A C11A H11C 109.5 H11A C11A H11B 109.5 H11A C11A H11C 109.5 H11B C11A H11C 109.5 N2A C12A H12A 107.4 N2A C12A C13A 110.4(13) N2A C12A C14A 110.6(11) C13A C12A H12A 107.4 C14A C12A H12A 107.4 C14A C12A C13A 113.2(13) C12A C13A H13A 109.5 C12A C13A H13B 109.5 C12A C13A H13C 109.5 H13A C13A H13B 109.5 H13A C13A H13C 109.5 H13B C13A H13C 109.5 C12A C14A H14A 109.5 C12A C14A H14B 109.5 C12A C14A H14C 109.5 H14A C14A H14B 109.5 H14A C14A H14C 109.5 H14B C14A H14C 109.5 C3B N1B H15B 119.5 C8B N1B H15B 119.5 C8B N1B C3B 121.0(8) C8B N2B C9B 119.3(8) C8B N2B C12B 124.3(8) C12B N2B C9B 116.3(6) C2B C1B H1B 119.3 C6B C1B H1B 119.3 C6B C1B C2B 121(2) C1B C2B C7B 121.3(17) C3B C2B C1B 115.1(17) C3B C2B C7B 123.5(10) C2B C3B N1B 120.5(11) C4B C3B N1B 116.5(13) C4B C3B C2B 123.0(11) C3B C4B H4B 119.2 C5B C4B C3B 121.7(18) C5B C4B H4B 119.2 C4B C5B H5B 122.0 C4B C5B C6B 116.1(19) C6B C5B H5B 122.0 C1B C6B C5B 122.1(14) C1B C6B H6B 119.0 C5B C6B H6B 119.0 C2B C7B H7BA 109.5 C2B C7B H7BB 109.5 C2B C7B H7BC 109.5 H7BA C7B H7BB 109.5 H7BA C7B H7BC 109.5 H7BB C7B H7BC 109.5 O1B C8B N1B 122.0(7) O1B C8B N2B 120.7(8) N1B C8B N2B 117.3(8) N2B C9B H9B 106.4 N2B C9B C10B 112.2(8) N2B C9B C11B 112.3(8) C10B C9B H9B 106.4 C11B C9B H9B 106.4 C11B C9B C10B 112.7(10) C9B C10B H10D 109.5 C9B C10B H10E 109.5 C9B C10B H10F 109.5 H10D C10B H10E 109.5 H10D C10B H10F 109.5 H10E C10B H10F 109.5 C9B C11B H11D 109.5 C9B C11B H11E 109.5 C9B C11B H11F 109.5 H11D C11B H11E 109.5 H11D C11B H11F 109.5 H11E C11B H11F 109.5 N2B C12B H12B 106.8 N2B C12B C13B 115.1(11) N2B C12B C14B 110.9(11) C13B C12B H12B 106.8 C13B C12B C14B 109.9(12) C14B C12B H12B 106.8 C12B C13B H13D 109.5 C12B C13B H13E 109.5 C12B C13B H13F 109.5 H13D C13B H13E 109.5 H13D C13B H13F 109.5 H13E C13B H13F 109.5 C12B C14B H14D 109.5 C12B C14B H14E 109.5 C12B C14B H14F 109.5 H14D C14B H14E 109.5 H14D C14B H14F 109.5 H14E C14B H14F 109.5 C3C N1C H15C 119.8 C8C N1C H15C 119.8 C8C N1C C3C 120.5(9) C8C N2C C9C 118.2(12) C8C N2C C12C 124.3(10) C9C N2C C12C 117.2(11) C2C C1C H1C 122.4 C2C C1C C6C 115.3(16) C6C C1C H1C 122.4 C1C C2C C7C 115.4(14) C3C C2C C1C 125.1(15) C3C C2C C7C 118.9(14) N1C C3C C4C 119.3(9) C2C C3C N1C 124.6(11) C2C C3C C4C 116.0(12) C3C C4C H4C 119.6 C5C C4C C3C 120.7(12) C5C C4C H4C 119.6 C4C C5C H5C 120.8 C6C C5C C4C 118.5(15) C6C C5C H5C 120.8 C1C C6C H6C 118.5 C5C C6C C1C 123.1(16) C5C C6C H6C 118.5 C2C C7C H7CA 109.5 C2C C7C H7CB 109.5 C2C C7C H7CC 109.5 H7CA C7C H7CB 109.5 H7CA C7C H7CC 109.5 H7CB C7C H7CC 109.5 O1C C8C N1C 118.4(10) O1C C8C N2C 125.7(11) N2C C8C N1C 115.5(9) N2C C9C H9C 107.4 N2C C9C C11C 107.9(13) C10C C9C N2C 113.1(14) C10C C9C H9C 107.4 C10C C9C C11C 113.4(17) C11C C9C H9C 107.4 C9C C10C H10G 109.5 C9C C10C H10H 109.5 C9C C10C H10I 109.5 H10G C10C H10H 109.5 H10G C10C H10I 109.5 H10H C10C H10I 109.5 C9C C11C H11G 109.5 C9C C11C H11H 109.5 C9C C11C H11I 109.5 H11G C11C H11H 109.5 H11G C11C H11I 109.5 H11H C11C H11I 109.5 N2C C12C H12C 107.1 N2C C12C C14C 111.7(12) C13C C12C N2C 118.6(14) C13C C12C H12C 107.1 C13C C12C C14C 104.7(13) C14C C12C H12C 107.1 C12C C13C H13G 109.5 C12C C13C H13H 109.5 C12C C13C H13I 109.5 H13G C13C H13H 109.5 H13G C13C H13I 109.5 H13H C13C H13I 109.5 C12C C14C H14G 109.5 C12C C14C H14H 109.5 C12C C14C H14I 109.5 H14G C14C H14H 109.5 H14G C14C H14I 109.5 H14H C14C H14I 109.5 C3D N1D H15D 118.8 C8D N1D H15D 118.8 C8D N1D C3D 122.4(10) C8D N2D C9D 119.4(8) C8D N2D C12D 121.6(9) C9D N2D C12D 117.3(7) C2D C1D H1D 119.9 C6D C1D H1D 119.9 C6D C1D C2D 120.2(18) C3D C2D C1D 116.8(15) C7D C2D C1D 120.5(14) C7D C2D C3D 122.4(11) N1D C3D C2D 117.6(11) N1D C3D C4D 118.3(13) C4D C3D C2D 124.1(12) C3D C4D H4D 124.9 C3D C4D C5D 110.1(18) C5D C4D H4D 124.9 C4D C5D H5D 118.0 C6D C5D C4D 124.0(17) C6D C5D H5D 118.0 C1D C6D C5D 123.9(16) C1D C6D H6D 118.1 C5D C6D H6D 118.1 C2D C7D H7DA 109.5 C2D C7D H7DB 109.5 C2D C7D H7DC 109.5 H7DA C7D H7DB 109.5 H7DA C7D H7DC 109.5 H7DB C7D H7DC 109.5 O1D C8D N1D 121.8(9) O1D C8D N2D 119.3(10) N1D C8D N2D 118.6(10) N2D C9D H9D 106.4 N2D C9D C10D 112.1(10) N2D C9D C11D 112.0(9) C10D C9D H9D 106.4 C10D C9D C11D 113.0(11) C11D C9D H9D 106.4 C9D C10D H10J 109.5 C9D C10D H10K 109.5 C9D C10D H10L 109.5 H10J C10D H10K 109.5 H10J C10D H10L 109.5 H10K C10D H10L 109.5 C9D C11D H11J 109.5 C9D C11D H11K 109.5 C9D C11D H11L 109.5 H11J C11D H11K 109.5 H11J C11D H11L 109.5 H11K C11D H11L 109.5 N2D C12D H12D 107.8 N2D C12D C14D 110.9(11) C13D C12D N2D 109.4(12) C13D C12D H12D 107.8 C13D C12D C14D 112.9(13) C14D C12D H12D 107.8 C12D C13D H13J 109.5 C12D C13D H13K 109.5 C12D C13D H13L 109.5 H13J C13D H13K 109.5 H13J C13D H13L 109.5 H13K C13D H13L 109.5 C12D C14D H14J 109.5 C12D C14D H14K 109.5 C12D C14D H14L 109.5 H14J C14D H14K 109.5 H14J C14D H14L 109.5 H14K C14D H14L 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1A C8A 1.227(12) N1A H15A 0.8600 N1A C3A 1.458(11) N1A C8A 1.382(10) N2A C8A 1.348(12) N2A C9A 1.501(15) N2A C12A 1.472(15) C1A H1A 0.9300 C1A C2A 1.38(2) C1A C6A 1.34(3) C2A C3A 1.402(12) C2A C7A 1.55(2) C3A C4A 1.336(13) C4A H4A 0.9300 C4A C5A 1.405(16) C5A H5A 0.9300 C5A C6A 1.39(3) C6A H6A 0.9300 C7A H7AA 0.9600 C7A H7AB 0.9600 C7A H7AC 0.9600 C9A H9A 0.9800 C9A C10A 1.44(2) C9A C11A 1.47(2) C10A H10A 0.9600 C10A H10B 0.9600 C10A H10C 0.9600 C11A H11A 0.9600 C11A H11B 0.9600 C11A H11C 0.9600 C12A H12A 0.9800 C12A C13A 1.53(2) C12A C14A 1.520(18) C13A H13A 0.9600 C13A H13B 0.9600 C13A H13C 0.9600 C14A H14A 0.9600 C14A H14B 0.9600 C14A H14C 0.9600 O1B C8B 1.225(11) N1B H15B 0.8600 N1B C3B 1.417(11) N1B C8B 1.363(12) N2B C8B 1.364(9) N2B C9B 1.492(11) N2B C12B 1.459(13) C1B H1B 0.9300 C1B C2B 1.408(16) C1B C6B 1.39(3) C2B C3B 1.41(2) C2B C7B 1.45(2) C3B C4B 1.40(2) C4B H4B 0.9300 C4B C5B 1.37(2) C5B H5B 0.9300 C5B C6B 1.42(3) C6B H6B 0.9300 C7B H7BA 0.9600 C7B H7BB 0.9600 C7B H7BC 0.9600 C9B H9B 0.9800 C9B C10B 1.514(15) C9B C11B 1.510(15) C10B H10D 0.9600 C10B H10E 0.9600 C10B H10F 0.9600 C11B H11D 0.9600 C11B H11E 0.9600 C11B H11F 0.9600 C12B H12B 0.9800 C12B C13B 1.485(19) C12B C14B 1.56(2) C13B H13D 0.9600 C13B H13E 0.9600 C13B H13F 0.9600 C14B H14D 0.9600 C14B H14E 0.9600 C14B H14F 0.9600 O1C C8C 1.227(13) N1C H15C 0.8600 N1C C3C 1.453(15) N1C C8C 1.342(15) N2C C8C 1.274(15) N2C C9C 1.482(16) N2C C12C 1.522(18) C1C H1C 0.9300 C1C C2C 1.39(2) C1C C6C 1.44(3) C2C C3C 1.359(15) C2C C7C 1.50(2) C3C C4C 1.457(18) C4C H4C 0.9300 C4C C5C 1.425(17) C5C H5C 0.9300 C5C C6C 1.34(3) C6C H6C 0.9300 C7C H7CA 0.9600 C7C H7CB 0.9600 C7C H7CC 0.9600 C9C H9C 0.9800 C9C C10C 1.40(2) C9C C11C 1.55(2) C10C H10G 0.9600 C10C H10H 0.9600 C10C H10I 0.9600 C11C H11G 0.9600 C11C H11H 0.9600 C11C H11I 0.9600 C12C H12C 0.9800 C12C C13C 1.51(2) C12C C14C 1.61(2) C13C H13G 0.9600 C13C H13H 0.9600 C13C H13I 0.9600 C14C H14G 0.9600 C14C H14H 0.9600 C14C H14I 0.9600 O1D C8D 1.222(14) N1D H15D 0.8600 N1D C3D 1.406(13) N1D C8D 1.361(15) N2D C8D 1.389(12) N2D C9D 1.455(12) N2D C12D 1.500(12) C1D H1D 0.9300 C1D C2D 1.465(17) C1D C6D 1.28(3) C2D C3D 1.438(19) C2D C7D 1.41(2) C3D C4D 1.44(2) C4D H4D 0.9300 C4D C5D 1.51(3) C5D H5D 0.9300 C5D C6D 1.34(3) C6D H6D 0.9300 C7D H7DA 0.9600 C7D H7DB 0.9600 C7D H7DC 0.9600 C9D H9D 0.9800 C9D C10D 1.513(15) C9D C11D 1.520(16) C10D H10J 0.9600 C10D H10K 0.9600 C10D H10L 0.9600 C11D H11J 0.9600 C11D H11K 0.9600 C11D H11L 0.9600 C12D H12D 0.9800 C12D C13D 1.48(2) C12D C14D 1.57(2) C13D H13J 0.9600 C13D H13K 0.9600 C13D H13L 0.9600 C14D H14J 0.9600 C14D H14K 0.9600 C14D H14L 0.9600 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 N1A C3A C4A C5A -179.7(11) C1A C2A C3A N1A -179.2(10) C1A C2A C3A C4A -6.4(16) C2A C1A C6A C5A 2(3) C2A C3A C4A C5A 7.6(17) C3A N1A C8A O1A -6.5(13) C3A N1A C8A N2A 171.1(8) C3A C4A C5A C6A -4(2) C4A C5A C6A C1A -1(3) C6A C1A C2A C3A 1(2) C6A C1A C2A C7A -179.9(15) C7A C2A C3A N1A 2.0(15) C7A C2A C3A C4A 174.7(11) C8A N1A C3A C2A -67.5(12) C8A N1A C3A C4A 119.4(10) C8A N2A C9A C10A -59.3(15) C8A N2A C9A C11A 69.4(15) C8A N2A C12A C13A 116.5(13) C8A N2A C12A C14A -117.4(14) C9A N2A C8A O1A -11.2(16) C9A N2A C8A N1A 171.2(10) C9A N2A C12A C13A -66.6(14) C9A N2A C12A C14A 59.5(18) C12A N2A C8A O1A 165.7(10) C12A N2A C8A N1A -11.9(15) C12A N2A C9A C10A 123.6(13) C12A N2A C9A C11A -107.6(14) N1B C3B C4B C5B -180.0(13) C1B C2B C3B N1B -179.9(11) C1B C2B C3B C4B 1.0(17) C2B C1B C6B C5B 9(3) C2B C3B C4B C5B -1(2) C3B N1B C8B O1B 8.6(16) C3B N1B C8B N2B -171.9(10) C3B C4B C5B C6B 4(2) C4B C5B C6B C1B -9(3) C6B C1B C2B C3B -5(2) C6B C1B C2B C7B 172.3(15) C7B C2B C3B N1B 2.6(18) C7B C2B C3B C4B -176.4(13) C8B N1B C3B C2B 60.4(15) C8B N1B C3B C4B -120.5(12) C8B N2B C9B C10B -63.9(11) C8B N2B C9B C11B 64.2(11) C8B N2B C12B C13B 114.5(13) C8B N2B C12B C14B -119.9(12) C9B N2B C8B O1B -0.9(13) C9B N2B C8B N1B 179.6(8) C9B N2B C12B C13B -61.9(14) C9B N2B C12B C14B 63.7(12) C12B N2B C8B O1B -177.1(10) C12B N2B C8B N1B 3.4(14) C12B N2B C9B C10B 112.7(10) C12B N2B C9B C11B -119.2(10) N1C C3C C4C C5C 177.7(11) C1C C2C C3C N1C 175.9(16) C1C C2C C3C C4C -8(2) C2C C1C C6C C5C -13(3) C2C C3C C4C C5C 1.1(18) C3C N1C C8C O1C 6.5(15) C3C N1C C8C N2C -166.4(10) C3C C4C C5C C6C -1(2) C4C C5C C6C C1C 7(3) C6C C1C C2C C3C 13(3) C6C C1C C2C C7C -175.8(18) C7C C2C C3C N1C 5(2) C7C C2C C3C C4C -178.4(14) C8C N1C C3C C2C 63.9(18) C8C N1C C3C C4C -112.4(12) C8C N2C C9C C10C -63(2) C8C N2C C9C C11C 62.9(16) C8C N2C C12C C13C 117.0(15) C8C N2C C12C C14C -121.1(13) C9C N2C C8C O1C 11(2) C9C N2C C8C N1C -176.5(11) C9C N2C C12C C13C -56.2(18) C9C N2C C12C C14C 65.6(16) C12C N2C C8C O1C -161.9(13) C12C N2C C8C N1C 10.4(17) C12C N2C C9C C10C 110.3(18) C12C N2C C9C C11C -123.4(13) N1D C3D C4D C5D 174.4(12) C1D C2D C3D N1D 178.6(12) C1D C2D C3D C4D 0(2) C2D C1D C6D C5D -8(3) C2D C3D C4D C5D -7(2) C3D N1D C8D O1D -6.1(19) C3D N1D C8D N2D 180.0(11) C3D C4D C5D C6D 7(3) C4D C5D C6D C1D 0(3) C6D C1D C2D C3D 8(2) C6D C1D C2D C7D -177.9(18) C7D C2D C3D N1D 5(2) C7D C2D C3D C4D -173.9(15) C8D N1D C3D C2D -62.6(16) C8D N1D C3D C4D 116.5(15) C8D N2D C9D C10D -74.4(13) C8D N2D C9D C11D 53.9(13) C8D N2D C12D C13D 128.0(13) C8D N2D C12D C14D -106.8(14) C9D N2D C8D O1D 10.6(17) C9D N2D C8D N1D -175.4(10) C9D N2D C12D C13D -66.7(14) C9D N2D C12D C14D 58.5(15) C12D N2D C8D O1D 175.6(12) C12D N2D C8D N1D -10.4(17) C12D N2D C9D C10D 120.0(12) C12D N2D C9D C11D -111.8(11) loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 0 3 -0.52 1.75 0 0 5 0.65 2.08 0 0 6 1840.89 34.86 0 0 7 -0.15 2.74 0 0 8 2738.67 50.59 0 0 9 1.76 2.81 0 0 10 294.67 19.17 0 0 11 -1.32 1.62 0 0 12 552.09 13.95 0 0 13 0.75 1.72 0 0 14 524.83 12.97 0 0 15 -4.48 2 0 0 16 125.51 5.04 0 -1 1 -0.04 0.56 0 1 2 1.52 1.76 0 -1 2 2.22 1.34 0 -1 3 -0.34 1.53 0 1 3 -0.19 1.76 0 -1 4 72.92 6.96 0 1 4 40.14 7.14 0 1 5 0.81 2.05 0 -1 5 0.56 2.07 0 1 6 11.98 4.73 0 -1 6 7.88 4.78 0 1 7 -0.63 2.84 0 -1 7 -0.08 2.58 0 -1 8 2.18 2.86 0 1 8 -0.64 2.45 0 -1 9 2.2 3.28 0 1 9 1.23 2.54 0 1 10 11.58 5.68 0 1 11 1.13 1.5 0 1 11 0.01 2.82 0 -1 11 -2.14 1.98 0 -1 12 6.67 2.63 0 1 12 14.23 3.24 0 1 13 3.12 1.8 0 -1 13 0.77 1.55 0 -1 14 29.87 4.14 0 1 14 25.29 3.34 0 1 15 -1.75 1.45 0 -1 15 -4.86 1.92 0 -1 16 -2 1.35 0 1 16 0.54 0.95 0 -1 17 0.02 0.71 0 -2 1 0.36 1.06 0 -2 -1 0.8 0.8 0 -2 3 2.62 1.42 0 -2 -3 -0.13 1.2 0 2 3 0.44 1.92 0 2 5 -1.19 2.47 0 -2 5 3.41 2.63 0 2 6 437.71 18.2 0 -2 6 428.28 16.45 0 2 7 -1.42 3.65 0 2 8 1062.72 33.31 0 -2 -8 1089.91 22.43 0 2 9 -4.19 3.6 0 2 10 138.49 13.73 0 2 11 -0.06 1.45 0 2 11 0.58 3.43 0 -2 11 -1.99 2.32 0 2 12 641.54 14.28 0 -2 12 629.82 16.15 0 -2 13 -1.59 1.91 0 2 13 -5.54 2.06 0 -2 14 223.02 9.05 0 2 14 203.68 7.31 0 2 15 -0.62 1 0 -2 15 1.72 1.47 0 2 16 57.5 3.04 0 -2 16 52.36 3.51 0 -2 17 0.56 0.83 0 -3 0 27.2 2.87 0 -3 1 0.49 1.31 0 -3 -1 1.7 1.04 0 -3 -2 14.28 2.25 0 -3 2 9.38 2.43 0 -3 -3 5.45 1.67 0 -3 3 0.76 1.58 0 3 3 2.69 2.84 0 3 4 5.73 3.82 0 -3 4 6.66 2.76 0 -3 -4 10.45 2.17 0 3 5 0.29 2.23 0 -3 -5 -1.18 1.25 0 3 6 15.19 5.27 0 -3 -6 2.83 1.55 0 -3 -7 -4.27 2.21 0 3 7 2.1 2.96 0 3 8 21.49 7.14 0 3 9 0.06 3.01 0 3 10 5.55 5.14 0 3 11 -2.1 3.67 0 -3 11 2.46 1.78 0 3 11 -5.48 2.07 0 -3 12 4.15 2.21 0 3 12 5.25 2.26 0 -3 13 -1.21 2.33 0 3 13 0.95 1.28 0 3 14 10.78 2.27 0 -3 14 12.61 2.98 0 -3 15 0.3 1.46 0 3 15 4.26 1.33 0 3 16 17.52 1.83 0 -3 16 -0.23 1.23 0 -3 17 -2.3 1.04 0 -4 0 3540.61 28.8 0 -4 1 2.15 2.13 0 -4 -1 -0.1 1.01 0 -4 -2 1294.75 15.65 0 -4 2 1343.69 22.1 0 -4 3 0.42 1.66 0 4 3 -1.33 2.38 0 -4 -3 0.19 0.94 0 4 4 5512.45 57.5 0 -4 -4 5707.77 37.03 0 4 5 1.56 2.31 0 -4 -5 2.17 1.41 0 4 6 510.52 20.66 0 -4 -6 537.24 12.78 0 4 7 0.11 2.7 0 4 8 1130.35 35.65 0 4 9 -0.22 3.05 0 4 10 649.21 31.42 0 -4 10 632.07 15.91 0 -4 11 0.73 1.9 0 4 11 -1.41 1.4 0 4 11 0.26 3.95 0 4 12 603.53 12.49 0 -4 12 606.91 16.69 0 4 12 643.28 33.47 0 4 13 0.31 1.32 0 -4 13 -2.77 2.43 0 -4 14 142.3 7.86 0 4 14 138.68 5.35 0 4 15 11.93 1.76 0 -4 15 -0.13 1.5 0 -4 16 16.31 2.35 0 -4 17 -2.66 1.13 0 -5 0 89.58 7.46 0 -5 -1 3.6 2.29 0 -5 1 2.43 2.3 0 -5 2 16.88 4.84 0 -5 -2 16.31 2.97 0 -5 -3 1.03 1.12 0 -5 3 -1.88 2.18 0 -5 -4 3.63 1.76 0 -5 4 4.48 3.2 0 5 4 3.52 3.22 0 -5 5 2.08 2.82 0 5 5 0.64 2.47 0 -5 -5 1.24 1.29 0 5 6 29.25 7.54 0 -5 -6 24.6 3.21 0 5 7 7.3 5.08 0 5 8 20.73 7.03 0 5 9 3.34 4.28 0 -5 10 2.74 2.11 0 5 10 3.08 1.65 0 5 10 3.91 4.58 0 5 11 2.22 3.54 0 5 11 1.94 1.56 0 -5 11 1.31 2 0 5 12 13.46 3.06 0 5 12 11.57 6.44 0 -5 12 12.22 3.67 0 5 13 8.16 1.93 0 -5 13 2 2.14 0 -5 14 32.5 4.28 0 5 14 40.6 3.18 0 5 15 63.43 3.31 0 -5 15 -0.74 1.61 0 -5 16 6.13 1.92 0 -6 0 324.63 12.6 0 -6 0 334.78 11.43 0 -6 -1 -0.8 1.98 0 -6 1 0.11 2.08 0 -6 2 9936.57 72.02 0 -6 -2 9787.93 56.7 0 -6 3 -0.85 2.61 0 -6 -3 -1.61 1.59 0 6 4 2783.43 45.93 0 -6 4 2688.66 41.4 0 -6 -4 2676.28 28.63 0 -6 -5 0.45 1.29 0 6 5 0.2 2.72 0 -6 5 1.55 2.2 0 6 6 642.17 25.5 0 6 7 -0.61 2.82 0 6 8 910.45 35.83 0 6 9 -1.27 4.32 0 -6 9 -1.81 2.27 0 6 10 148.27 5.74 0 -6 10 127.75 7.95 0 6 10 142.88 15.99 0 6 11 -3.53 3.43 0 6 11 0.53 1.13 0 -6 11 2.18 2.16 0 -6 12 295.82 12.31 0 6 12 313.59 8.08 0 6 12 305.19 23.97 0 6 13 27.14 3.18 0 -6 13 3.47 2.51 0 -6 14 226.14 10.17 0 -6 15 1.56 1.7 0 -6 16 12.7 2.28 0 -7 0 61.82 6.89 0 -7 -1 11.72 4.04 0 -7 -1 11.12 2.97 0 -7 1 7.54 3.72 0 -7 -2 29.04 4.08 0 -7 2 38.72 6.49 0 -7 -3 -1.5 1.81 0 -7 3 -2.25 2.9 0 7 4 13.29 6.48 0 -7 -4 13.31 3.45 0 -7 5 -1.01 2.5 0 -7 -5 1.85 1.65 0 7 5 -1.31 2.97 0 7 6 0.71 2.53 0 7 7 2.75 3.73 0 7 8 10.32 5.9 0 7 9 -0.57 3.34 0 7 9 12.22 2.73 0 7 10 11.52 6.56 0 -7 10 12.93 3.54 0 -7 11 8.27 3.21 0 7 11 2.33 5.39 0 -7 12 3.86 2.83 0 7 12 73.78 4.36 0 -7 13 6.15 2.94 0 -7 14 23.39 3.98 0 -7 15 3.75 1.9 0 -7 16 1.25 1.3 0 -8 0 41.76 5.57 0 -8 1 -1.97 2.71 0 -8 -1 -1.02 2.45 0 -8 2 929.88 26.33 0 -8 -2 986.75 22.37 0 -8 -2 958.57 24.15 0 -8 -3 -1.37 1.87 0 -8 -3 -2.16 2.38 0 -8 3 0.52 2.21 0 -8 -4 498.19 14.96 0 -8 4 490.25 20.8 0 -8 -4 489.37 16.2 0 8 4 496.41 21.97 0 -8 5 -0.31 2.17 0 8 5 0.49 2.97 0 8 6 2.94 2.97 0 8 7 -0.32 3.72 0 8 8 164.3 16.8 0 8 9 -4.8 5.05 0 -8 10 81.58 7.02 0 8 10 100.91 13.8 0 -8 11 -2.87 2.71 0 8 11 5.27 3.77 0 -8 12 101.03 7.41 0 -8 13 4.39 2.53 0 -8 14 129.99 7.58 0 -8 15 -3 1.79 0 -8 16 7.8 1.72 0 -9 0 15.26 4.59 0 -9 1 9.16 5.52 0 -9 -1 13.25 5.19 0 -9 -2 7.25 4.11 0 -9 2 8.93 4.6 0 9 3 -0.66 2.34 0 -9 3 1.86 2.85 0 -9 -3 2.27 2.27 0 -9 4 12.63 4.69 0 9 4 11.37 5.22 0 -9 -4 9.49 3.65 0 -9 -4 8.76 3.52 0 -9 5 0.94 2.52 0 9 5 -0.16 2.48 0 9 6 2.25 4.16 0 -9 7 2.61 1.98 0 9 7 3.19 2.76 0 9 8 3.25 4 0 -9 8 2.17 2.1 0 9 9 -4.85 4.83 0 9 10 -0.4 4.52 0 -9 10 4.96 3.07 0 -9 11 -3.75 3.07 0 -9 12 0.65 2.01 0 -9 13 3.43 2.46 0 -9 14 -1.17 2.36 0 -9 15 -4.29 1.75 0 -9 16 0.75 0.99 0 -10 0 233.62 14.62 0 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160.64 8.37 5 -5 0 6.39 2.19 5 5 1 119.63 5.01 5 -5 -1 164.97 8.58 5 5 2 243.05 9.86 5 -5 -2 257.25 11.16 5 5 3 128.65 8.46 5 -5 -3 119.39 8.5 5 5 4 11.77 3.27 5 -5 -4 11.14 2.79 5 5 5 181.03 12.32 5 -5 -5 178.38 10.47 5 5 6 182.28 13.21 5 -5 -6 155.23 10.74 5 5 7 131.69 12.54 5 -5 -7 129.76 10.1 5 5 8 155.9 14.39 5 -5 -8 176.34 11.75 5 5 9 15.21 5.94 5 5 9 16.78 2.63 5 -5 -9 22.93 4.58 5 5 10 31.92 3.73 5 5 10 40.31 9.61 5 5 11 19.27 2.81 5 5 12 38.86 3.51 5 5 13 8.7 1.91 5 5 14 22.43 2.43 5 5 15 26.54 2.46 5 -6 16 1.31 1.36 5 -6 15 2.94 2.11 5 -6 14 39.82 5.2 5 -6 13 7.9 3.35 5 -6 12 13.01 3.58 -5 6 11 85.96 14.49 5 -6 11 118.26 8.56 5 -6 10 7.84 2.78 -5 6 10 9.4 5.4 5 -6 9 68.54 6.63 -5 6 9 72.57 11.9 -5 6 8 166.45 17.55 5 -6 7 153.02 12.43 -5 6 7 165.92 15.62 -5 6 6 28.49 7.37 5 -6 6 37.02 5.97 5 -6 5 1.21 1.98 5 -6 3 198.95 11.63 5 -6 2 74.8 6.68 5 -6 1 80.51 6.38 5 -6 0 54.23 5.37 5 -6 -1 80.95 6.38 5 6 2 64.64 5.31 5 -6 -2 68.13 6.35 5 6 3 204.98 10.4 5 -6 -3 225.15 11.22 5 6 4 152.24 11.22 5 -6 -4 183.59 10.41 5 -6 -5 -1.05 2.2 5 6 5 -1.7 2.86 5 6 6 28.64 6.97 5 -6 -6 33.34 5.32 5 6 7 173.14 14.42 5 -6 -7 170.92 11.33 5 6 8 179.64 15.48 5 -6 -8 189.31 12.02 5 6 9 74.73 4.63 5 6 9 73.33 11.05 5 6 10 9.9 2.12 5 6 10 8.88 5.38 -5 -6 10 7.38 2.34 -5 -6 11 104.3 6.97 5 6 11 118.16 5.58 5 6 12 17.34 2.74 -5 -6 12 14.01 3.13 5 6 13 28.39 2.77 5 6 14 72.92 3.76 5 -7 17 -2.94 1.12 5 -7 16 2.13 1.4 5 -7 15 10.48 2.59 5 -7 14 15.77 3.72 5 -7 13 8.79 2.97 5 -7 12 82.15 7.24 5 -7 11 34.92 5.02 -5 7 11 22.02 7.65 5 -7 10 48.5 5.65 -5 7 10 55.13 12.49 5 -7 9 10.16 3.12 -5 7 9 7.73 5.02 -5 7 8 23.41 7.42 5 -7 8 31.18 4.38 5 -7 7 124.74 11.28 -5 7 7 120.6 14.41 5 -7 6 22.47 5.31 -5 7 6 28.56 6.88 5 -7 5 2.2 2.19 5 -7 4 87.17 9.05 5 -7 2 406.58 16.14 5 -7 1 85.47 8.11 5 -7 0 29.76 4.69 5 -7 -1 75.17 7.58 5 -7 -2 325.23 14.42 5 7 3 29.71 4.89 5 -7 -3 42.05 5.66 5 7 4 79.42 7.83 5 -7 -4 76.36 7.52 5 -7 -5 2.71 2.1 5 7 5 3.62 2.21 5 7 6 27.81 6.23 5 -7 -6 23.41 4.87 5 -7 -7 113.76 9.97 5 7 7 111.83 12.24 5 7 8 27.61 3.32 5 7 8 22.23 6.45 5 7 9 3.81 3.99 5 7 9 14.11 2.58 5 7 10 53.47 10.02 5 7 10 54.74 3.92 -5 -7 10 36.1 4.96 5 7 11 45.53 3.55 -5 -7 11 28.53 4.12 5 7 12 98.17 4.82 -5 -7 12 66.44 5.88 -5 -7 13 10.45 2.9 5 7 13 91.04 4.17 5 -8 16 5.01 1.72 5 -8 15 10.44 2.64 5 -8 14 5.75 2.9 5 -8 13 1.18 2.19 5 -8 12 15.27 3.72 5 -8 11 40.2 5.48 -5 8 10 29.41 10.12 5 -8 10 18.74 4.16 5 -8 9 15.04 3.86 -5 8 9 17.47 7.37 5 -8 8 100.99 7.15 -5 8 8 89.04 13.87 5 -8 7 92.56 10.96 -5 8 7 93.57 13.71 -5 8 6 7.58 5.03 5 -8 6 9.34 3.99 5 -8 5 54.34 7.88 5 -8 4 75.39 9.16 5 -8 2 16.93 4.24 5 -8 1 45.01 6.37 5 -8 0 133.65 9.88 5 -8 -1 47.25 6.49 5 -8 -2 15.1 3.89 5 -8 -3 7.15 3.03 5 -8 -4 78.02 7.54 5 -8 -5 49.23 6.1 5 8 5 35.61 7.59 5 8 6 5.88 3.37 5 -8 -6 11.59 3.41 5 8 7 108.22 12.69 5 -8 -7 117.89 9.44 5 8 8 89.46 11.83 5 8 8 121.78 5.49 5 8 9 63.68 4.11 5 8 9 17.95 5.99 -5 -8 10 14.73 3.26 5 8 10 18.83 7.3 -5 -8 11 29.49 4.16 -5 -8 12 12.79 3.05 -5 -8 13 7.57 2.6 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-3 -0.18 1.06 -26 -4 -2 -0.17 1.15 -26 -4 -1 0.88 1.04 -26 -4 0 -0.49 1.14 -26 -4 1 -0.09 0.96 26 -4 -5 -1.94 0.99 -26 -5 -6 10.14 1.5 -26 -5 -5 9.4 1.58 -26 -5 -4 5.13 1.47 -26 -5 -3 3.82 1.18 -26 -5 -2 4.3 1.32 -26 -5 -1 34.59 2.93 -26 -5 0 -0.78 1.07 -26 -5 1 35.22 2.76 -26 -6 -5 -0.72 0.87 -26 -6 -4 -0.76 0.94 -26 -6 -3 -1.41 1.11 -26 -6 -2 -0.15 1.1 -26 -6 -1 -0.74 1.03 -26 -6 0 2.31 1.14 -26 -6 1 1.18 1.04 -26 -7 -4 2.81 1 -26 -7 -3 4 1.17 -26 -7 -2 0.91 1.03 -26 -7 -1 27.21 2.43 -26 -7 0 1.31 1.01 -26 -7 1 25.76 2.19 -26 -8 -3 0.8 0.85 -26 -8 -2 0.14 0.79 -26 -8 -1 0.38 0.82 -27 0 0 0.3 0.85 -27 0 -1 0.97 0.96 -27 0 -2 0.04 1.06 -27 0 -3 1.78 1.11 -27 0 -4 1.45 1.04 -27 0 -5 0.27 0.91 27 0 -5 -2.28 1.12 -27 0 -6 0.33 0.81 27 0 -6 -1.73 0.99 -27 -1 -6 2.95 1.01 -27 -1 -5 1.33 0.93 -27 -1 -4 0.27 0.94 -27 -1 -3 0.69 0.98 -27 -1 -2 1.01 1.08 -27 -1 -1 1.3 1.04 -27 -1 0 -0.07 0.84 -27 1 -1 0.23 0.97 -27 1 -2 0.9 1.04 -27 1 -3 0.97 1 -27 1 -4 1.49 1.07 -27 1 -5 0.26 0.99 27 -1 -5 -1.97 1.02 -27 1 -6 2.01 0.99 -27 -2 -6 0.55 0.75 -27 -2 -5 0.96 0.93 -27 -2 -4 0.01 0.85 -27 -2 -3 1.58 1.2 -27 -2 -2 3.21 1.27 -27 -2 -1 1.4 1.05 -27 -2 0 -0.6 0.88 -27 2 -1 0.22 0.9 -27 2 -2 4.53 1.35 -27 2 -6 1.12 0.88 -27 -3 -5 -0.87 0.78 -27 -3 -4 1.13 0.99 -27 -3 -3 1.37 1.07 -27 -3 -2 1.7 1.17 -27 -3 -1 0.67 0.87 -27 -3 0 1.17 0.89 -27 3 -1 2.89 1.13 -27 -4 -5 1.72 0.92 -27 -4 -4 -0.01 0.79 -27 -4 -3 -0.54 0.82 -27 -4 -2 2.43 1.03 -27 -4 -1 -0.44 0.93 -27 -4 0 -0.94 0.98 -27 -5 -4 -0.99 0.88 -27 -5 -3 -0.05 0.79 -27 -5 -2 -0.48 0.91 -27 -5 -1 1.28 0.83 -27 -5 0 1.53 0.94 -27 -6 -3 0.08 0.73 -27 -6 -2 1.07 0.92 -27 -6 -1 0.28 0.81 -28 0 -3 5.48 1.13 -28 -1 -3 0 0.75 -28 -1 -2 -1.36 0.81 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 -13.8528 4.1015 -0.0701 0.6890 -0.7247 0.0090 -4.0113 -0.0692 -9.4499 0.1810 -0.1877 -0.9654 5.4199 10.0838 0.0961 -0.7077 -0.6964 0.1196 -0.1672 0.0448 9.8074 0.0768 0.0783 0.9940 -6.3754 -9.7863 0.1781 0.7566 0.6476 -0.0905 2.2488 -10.6958 0.0830 0.2650 0.9597 -0.0939 7.4072 -9.3990 0.2251 -0.0967 0.9937 -0.0574 14.0345 -3.7645 -0.0852 -0.7138 0.7001 -0.0211 12.4127 6.0438 0.1737 -0.9813 -0.1649 0.0997