#------------------------------------------------------------------------------ #$Date: 2019-11-17 15:48:35 +0200 (Sun, 17 Nov 2019) $ #$Revision: 230975 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/00/1550030.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_1550030 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 monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _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 93.3110(10) _cell_angle_gamma 90 _cell_formula_units_Z 12 _cell_length_a 12.9354(2) _cell_length_b 11.9200(2) _cell_length_c 27.3126(4) _cell_measurement_reflns_used 12558 _cell_measurement_temperature 150 _cell_measurement_theta_max 73.3470 _cell_measurement_theta_min 3.9880 _cell_volume 4204.30(11) _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 N~2~ _diffrn_ambient_temperature 150 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2031 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.987 _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 -66.00 32.00 1.00 4.58 -- -42.62 38.00-180.00 98 2 \w -110.00 -22.00 1.00 4.58 -- -42.62 -57.00-120.00 88 3 \w -71.00 31.00 1.00 4.58 -- -42.62 57.00 30.00 102 4 \w 53.00 97.00 1.00 4.58 -- 42.62-130.00 179.00 44 5 \w 85.00 174.00 1.00 44.08 -- 106.36 45.00 -60.00 89 6 \w 34.00 132.00 1.00 44.08 -- 106.36 -77.00-150.00 98 7 \w 37.00 71.00 1.00 44.08 -- 106.36-125.00 90.00 34 8 \w 81.00 162.00 1.00 44.08 -- 106.36 45.00 30.00 81 9 \w 76.00 169.00 1.00 44.08 -- 106.36 77.00 -30.00 93 10 \w 44.00 120.00 1.00 44.08 -- 106.36-125.00-150.00 76 11 \w 35.00 111.00 1.00 44.08 -- 106.36 -45.00 30.00 76 12 \w 59.00 111.00 1.00 44.08 -- 106.36-125.00 -30.00 52 13 \w 54.00 124.00 1.00 44.08 -- 106.36 -77.00 -30.00 70 14 \w 95.00 123.00 1.00 44.08 -- 106.36 125.00-150.00 28 15 \w 95.00 120.00 1.00 44.08 -- 106.36-125.00 90.00 25 16 \w 130.00 155.00 1.00 44.08 -- 106.36 45.00 -90.00 25 17 \w 150.00 175.00 1.00 44.08 -- 106.36 125.00-120.00 25 18 \w 81.00 119.00 1.00 44.08 -- 106.36 45.00 -90.00 38 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w and \f scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0118363000 _diffrn_orient_matrix_UB_12 0.0731888000 _diffrn_orient_matrix_UB_13 -0.0458376000 _diffrn_orient_matrix_UB_21 -0.0203478000 _diffrn_orient_matrix_UB_22 -0.1035139000 _diffrn_orient_matrix_UB_23 -0.0329540000 _diffrn_orient_matrix_UB_31 -0.1169083000 _diffrn_orient_matrix_UB_32 0.0253726000 _diffrn_orient_matrix_UB_33 -0.0022499000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_unetI/netI 0.0261 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_number 29459 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.619 _diffrn_reflns_theta_min 3.422 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.549 _exptl_absorpt_correction_T_max 0.982 _exptl_absorpt_correction_T_min 0.871 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.111 _exptl_crystal_description needle _exptl_crystal_F_000 1536 _exptl_crystal_size_max 0.481 _exptl_crystal_size_mid 0.048 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.341 _refine_diff_density_min -0.277 _refine_diff_density_rms 0.038 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 487 _refine_ls_number_reflns 8377 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.027 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0427 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0556P)^2^+1.1562P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1074 _refine_ls_wR_factor_ref 0.1152 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7048 _reflns_number_total 8377 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; xstr0776.res created by SHELXL-2014/7 TITL xstr0776_a.res in P2(1)/c CELL 1.54184 12.9354 11.92 27.3126 90 93.311 90 ZERR 12 0.0002 0.0002 0.0004 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 168 264 24 12 L.S. 5 PLAN 2 TEMP -123 BOND MORE -1 BOND $H CONF HTAB 2.3 list 4 fmap 2 53 acta REM REM REM WGHT 0.055600 1.156200 FVAR 0.34254 PART 1 O1A 4 0.114311 0.223702 0.298947 11.00000 0.02298 0.03491 = 0.03242 0.00335 0.00055 -0.00278 N1A 3 -0.010749 0.147260 0.344125 11.00000 0.02006 0.03091 = 0.02794 0.00166 0.00053 0.00076 N2A 3 -0.052197 0.271335 0.279422 11.00000 0.02571 0.04707 = 0.03571 0.01410 0.00204 0.00567 C1A 1 0.201301 -0.050987 0.383076 11.00000 0.02770 0.03020 = 0.04188 -0.00065 0.00293 0.00388 AFIX 43 H1A 2 0.262595 -0.081577 0.370907 11.00000 -1.20000 AFIX 0 C2A 1 0.144256 0.025670 0.354333 11.00000 0.02916 0.03234 = 0.03105 0.00008 0.00332 0.00174 AFIX 43 H2A 2 0.166568 0.046486 0.323068 11.00000 -1.20000 AFIX 0 C3A 1 0.054125 0.072054 0.371452 11.00000 0.02226 0.02588 = 0.02799 -0.00133 -0.00208 -0.00182 C4A 1 0.023266 0.038088 0.417137 11.00000 0.03195 0.04068 = 0.03324 0.00537 0.00655 0.00831 AFIX 43 H4A 2 -0.038204 0.068064 0.429382 11.00000 -1.20000 AFIX 0 C5A 1 0.081430 -0.039113 0.444946 11.00000 0.04473 0.04424 = 0.03475 0.01117 0.00772 0.00880 AFIX 43 H5A 2 0.058527 -0.061545 0.475890 11.00000 -1.20000 AFIX 0 C6A 1 0.172138 -0.084429 0.428775 11.00000 0.03575 0.02913 = 0.03949 0.00286 -0.00249 0.00438 C7A 1 0.235944 -0.167052 0.459504 11.00000 0.05195 0.04290 = 0.05171 0.01120 -0.00097 0.01451 AFIX 137 H7AA 2 0.203464 -0.241274 0.457090 11.00000 -1.50000 H7AB 2 0.239951 -0.142441 0.493796 11.00000 -1.50000 H7AC 2 0.305868 -0.171118 0.447587 11.00000 -1.50000 AFIX 0 C8A 1 0.021525 0.215282 0.307013 11.00000 0.02575 0.02722 = 0.02503 -0.00093 -0.00075 -0.00080 C9A 1 -0.020824 0.339575 0.237524 11.00000 0.03432 0.03765 = 0.02856 0.00726 -0.00105 0.00173 AFIX 13 H9A 2 -0.086278 0.371456 0.221980 11.00000 -1.20000 AFIX 0 C10A 1 0.046031 0.439852 0.253130 11.00000 0.06439 0.03708 = 0.04352 0.00852 -0.01032 -0.00612 AFIX 137 H10A 2 0.013205 0.481024 0.279133 11.00000 -1.50000 H10B 2 0.053408 0.489456 0.224931 11.00000 -1.50000 H10C 2 0.114536 0.413654 0.265377 11.00000 -1.50000 AFIX 0 C11A 1 0.027614 0.271429 0.197794 11.00000 0.04718 0.05742 = 0.03133 -0.00057 0.00218 0.00258 AFIX 137 H11A 2 0.096559 0.245920 0.209723 11.00000 -1.50000 H11B 2 0.033647 0.318151 0.168573 11.00000 -1.50000 H11C 2 -0.016121 0.206262 0.189459 11.00000 -1.50000 AFIX 0 C12A 1 -0.164972 0.262042 0.284976 11.00000 0.02861 0.08527 = 0.05613 0.03730 0.00547 0.01453 AFIX 13 H12A 2 -0.174937 0.215537 0.314809 11.00000 -1.20000 AFIX 0 C13A 1 -0.212296 0.376743 0.293641 11.00000 0.04863 0.12515 = 0.04117 -0.01094 0.00147 0.03829 AFIX 137 H13A 2 -0.172536 0.414811 0.320380 11.00000 -1.50000 H13B 2 -0.284175 0.367529 0.302457 11.00000 -1.50000 H13C 2 -0.210646 0.421737 0.263666 11.00000 -1.50000 AFIX 0 C14A 1 -0.219183 0.201366 0.241213 11.00000 0.03007 0.05653 = 0.12379 0.01128 -0.01510 0.00199 AFIX 137 H14A 2 -0.214791 0.247308 0.211650 11.00000 -1.50000 H14B 2 -0.292073 0.189010 0.247623 11.00000 -1.50000 H14C 2 -0.185364 0.128962 0.236369 11.00000 -1.50000 AFIX 0 PART 0 PART 2 O1B 4 0.452671 0.382824 0.375222 11.00000 0.02013 0.03597 = 0.02852 -0.00406 -0.00174 0.00226 N1B 3 0.316629 0.335067 0.322059 11.00000 0.01981 0.04258 = 0.02769 -0.00999 0.00204 -0.00265 N2B 3 0.289166 0.412800 0.398532 11.00000 0.02062 0.04275 = 0.02519 -0.00779 -0.00068 0.00365 C1B 1 0.517685 0.324551 0.230065 11.00000 0.02445 0.04488 = 0.03119 0.00119 0.00340 0.00061 AFIX 43 H1B 2 0.580280 0.361226 0.222960 11.00000 -1.20000 AFIX 0 C2B 1 0.466189 0.358515 0.270730 11.00000 0.02694 0.03732 = 0.02956 -0.00509 0.00133 -0.00144 AFIX 43 H2B 2 0.493154 0.417925 0.290833 11.00000 -1.20000 AFIX 0 C3B 1 0.374808 0.305039 0.281896 11.00000 0.02241 0.03470 = 0.02477 -0.00305 0.00036 0.00401 C4B 1 0.336098 0.219570 0.251157 11.00000 0.02505 0.03682 = 0.02692 -0.00331 -0.00015 -0.00065 AFIX 43 H4B 2 0.273149 0.183282 0.257987 11.00000 -1.20000 AFIX 0 C5B 1 0.388724 0.187246 0.210779 11.00000 0.03340 0.03775 = 0.02703 -0.00716 -0.00115 0.00200 AFIX 43 H5B 2 0.361398 0.128569 0.190357 11.00000 -1.20000 AFIX 0 C6B 1 0.480811 0.238867 0.199459 11.00000 0.03090 0.04371 = 0.02746 -0.00266 0.00283 0.00655 C7B 1 0.537100 0.202987 0.155090 11.00000 0.04284 0.06389 = 0.03726 -0.01099 0.01192 0.00270 AFIX 137 H7BA 2 0.600358 0.247597 0.153104 11.00000 -1.50000 H7BB 2 0.492206 0.214747 0.125392 11.00000 -1.50000 H7BC 2 0.555239 0.123347 0.157999 11.00000 -1.50000 AFIX 0 C8B 1 0.357914 0.377464 0.366064 11.00000 0.02316 0.02806 = 0.02442 -0.00161 0.00044 0.00182 C9B 1 0.325804 0.437968 0.449771 11.00000 0.02686 0.03708 = 0.02292 -0.00535 0.00005 0.00179 AFIX 13 H9B 2 0.262352 0.454886 0.467681 11.00000 -1.20000 AFIX 0 C10B 1 0.376052 0.336410 0.475372 11.00000 0.04253 0.04042 = 0.02907 0.00010 -0.00023 0.00236 AFIX 137 H10D 2 0.330544 0.271105 0.470643 11.00000 -1.50000 H10E 2 0.387232 0.352011 0.510508 11.00000 -1.50000 H10F 2 0.442681 0.320834 0.461421 11.00000 -1.50000 AFIX 0 C11B 1 0.393043 0.542476 0.454386 11.00000 0.03379 0.03751 = 0.03181 -0.00722 -0.00210 -0.00038 AFIX 137 H11D 2 0.460465 0.527106 0.441189 11.00000 -1.50000 H11E 2 0.402963 0.563642 0.489010 11.00000 -1.50000 H11F 2 0.359042 0.604042 0.435933 11.00000 -1.50000 AFIX 0 C12B 1 0.176817 0.424241 0.386840 11.00000 0.02163 0.05550 = 0.03117 -0.01431 -0.00219 0.00624 AFIX 13 H12B 2 0.163843 0.406322 0.351246 11.00000 -1.20000 AFIX 0 C13B 1 0.115970 0.340555 0.415501 11.00000 0.02937 0.05252 = 0.06374 -0.02307 0.00782 -0.00791 AFIX 137 H13D 2 0.142938 0.264862 0.410442 11.00000 -1.50000 H13E 2 0.042779 0.343492 0.404105 11.00000 -1.50000 H13F 2 0.122861 0.359215 0.450481 11.00000 -1.50000 AFIX 0 C14B 1 0.140880 0.544246 0.394472 11.00000 0.03438 0.05815 = 0.04486 0.00112 0.00035 0.01620 AFIX 137 H14D 2 0.149571 0.563402 0.429361 11.00000 -1.50000 H14E 2 0.067689 0.551075 0.383470 11.00000 -1.50000 H14F 2 0.182243 0.595524 0.375500 11.00000 -1.50000 AFIX 0 PART 0 PART 3 O1C 4 0.795504 0.162768 0.401112 11.00000 0.02255 0.03029 = 0.04666 -0.00319 0.00383 0.00342 N1C 3 0.664379 0.289670 0.405382 11.00000 0.02036 0.02549 = 0.04051 0.00069 0.00016 0.00173 N2C 3 0.630587 0.098656 0.392649 11.00000 0.02424 0.02351 = 0.04727 -0.00035 0.00106 0.00176 C1C 1 0.879759 0.479796 0.448438 11.00000 0.02337 0.03476 = 0.03141 -0.00280 -0.00200 0.00091 AFIX 43 H1C 2 0.946244 0.475670 0.465036 11.00000 -1.20000 AFIX 0 C2C 1 0.824642 0.381373 0.439805 11.00000 0.02699 0.02845 = 0.03126 0.00288 -0.00174 0.00281 AFIX 43 H2C 2 0.853477 0.311563 0.450375 11.00000 -1.20000 AFIX 0 C3C 1 0.726786 0.384959 0.415576 11.00000 0.02236 0.02640 = 0.02582 -0.00044 0.00406 0.00055 C4C 1 0.686225 0.489393 0.401565 11.00000 0.02403 0.02851 = 0.03041 -0.00209 -0.00094 0.00384 AFIX 43 H4C 2 0.618929 0.493829 0.385809 11.00000 -1.20000 AFIX 0 C5C 1 0.742917 0.586665 0.410360 11.00000 0.03107 0.02511 = 0.03378 -0.00134 -0.00009 0.00423 AFIX 43 H5C 2 0.713890 0.656681 0.400200 11.00000 -1.20000 AFIX 0 C6C 1 0.841690 0.584202 0.433799 11.00000 0.02700 0.02956 = 0.02991 -0.00541 0.00364 -0.00045 C7C 1 0.904469 0.689777 0.442699 11.00000 0.03511 0.03236 = 0.04971 -0.00713 -0.00005 -0.00287 AFIX 137 H7CA 2 0.870045 0.738094 0.465796 11.00000 -1.50000 H7CB 2 0.910375 0.729693 0.411617 11.00000 -1.50000 H7CC 2 0.973738 0.670072 0.456461 11.00000 -1.50000 AFIX 0 C8C 1 0.701442 0.182042 0.399626 11.00000 0.02497 0.02617 = 0.02970 0.00043 0.00235 0.00218 C9C 1 0.666856 -0.018542 0.388162 11.00000 0.03129 0.02434 = 0.07278 -0.00738 0.00366 0.00107 AFIX 13 H9C 2 0.602869 -0.065120 0.382950 11.00000 -1.20000 AFIX 0 C10C 1 0.728895 -0.038493 0.343766 11.00000 0.04805 0.05395 = 0.09801 -0.03821 0.02202 -0.00816 AFIX 137 H10G 2 0.693288 -0.004099 0.314887 11.00000 -1.50000 H10H 2 0.735866 -0.119351 0.338365 11.00000 -1.50000 H10I 2 0.797766 -0.004968 0.349253 11.00000 -1.50000 AFIX 0 C11C 1 0.721082 -0.060983 0.436180 11.00000 0.04844 0.03281 = 0.10053 0.01518 -0.01046 0.00633 AFIX 137 H11G 2 0.789465 -0.025894 0.440794 11.00000 -1.50000 H11H 2 0.729032 -0.142642 0.434602 11.00000 -1.50000 H11I 2 0.679327 -0.041479 0.463765 11.00000 -1.50000 AFIX 0 C12C 1 0.517445 0.113707 0.393382 11.00000 0.02477 0.02734 = 0.05963 0.00026 0.00132 -0.00027 AFIX 13 H12C 2 0.504181 0.196037 0.396205 11.00000 -1.20000 AFIX 0 C13C 1 0.462996 0.074678 0.346121 11.00000 0.04170 0.06286 = 0.06329 0.01419 -0.01497 -0.00608 AFIX 137 H13G 2 0.494199 0.110964 0.318357 11.00000 -1.50000 H13H 2 0.389479 0.094604 0.345998 11.00000 -1.50000 H13I 2 0.469921 -0.006901 0.343292 11.00000 -1.50000 AFIX 0 C14C 1 0.473455 0.058058 0.437388 11.00000 0.04209 0.05967 = 0.06237 -0.00508 0.01504 -0.00648 AFIX 137 H14G 2 0.485660 -0.022993 0.436024 11.00000 -1.50000 H14H 2 0.398839 0.072471 0.437145 11.00000 -1.50000 H14I 2 0.507362 0.088638 0.467510 11.00000 -1.50000 AFIX 0 PART 0 H15B 2 0.253257 0.309008 0.321629 11.00000 0.03508 H15C 2 0.598610 0.304249 0.395722 11.00000 0.03660 H15A 2 -0.071435 0.158841 0.354334 11.00000 0.03041 HKLF 4 REM xstr0776_a.res in P2(1)/c REM R1 = 0.0427 for 7048 Fo > 4sig(Fo) and 0.0524 for all 8377 data REM 487 parameters refined using 0 restraints END WGHT 0.0556 1.1562 REM Instructions for potential hydrogen bonds HTAB C2A O1A EQIV $1 -x, y+1/2, -z+1/2 HTAB C10A N1A_$1 HTAB C10A O1A HTAB C11A O1A HTAB C10B O1B HTAB C11B O1B HTAB C2C O1C HTAB C10C O1C HTAB C11C O1C REM Highest difference peak 0.341, deepest hole -0.277, 1-sigma level 0.038 Q1 1 0.7394 -0.0753 0.4010 11.00000 0.05 0.34 Q2 1 -0.2205 0.2041 0.2798 11.00000 0.05 0.28 REM The information below was added by Olex2. REM REM R1 = 0.0427 for 7048 Fo > 4sig(Fo) and 0.0524 for all 30291 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.34, deepest hole -0.28 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0524 REM R1_gt = 0.0427 REM wR_ref = 0.1152 REM GOOF = 1.027 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 30291 REM Reflections_gt = 7048 REM Parameters = n/a REM Hole = -0.28 REM Peak = 0.34 REM Flack = n/a ; _cod_data_source_file c8sm01682h2.cif _cod_data_source_block xstr0776 _cod_depositor_comments 'Adding full bibliography for 1550029--1550031.cif.' _cod_database_code 1550030 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula 'C14 H22 N2 O' _chemical_oxdiff_usercomment 'Molecule 6' _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 99.97 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.49 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(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) 2.b Aromatic/amide H refined with riding coordinates: C1A(H1A), C2A(H2A), C4A(H4A), C5A(H5A), C1B(H1B), C2B(H2B), C4B(H4B), C5B(H5B), C1C(H1C), C2C(H2C), C4C(H4C), C5C(H5C) 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) ; _olex2_date_sample_data_collection 2017-08-03 _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 1.499 _oxdiff_exptl_absorpt_empirical_full_min 0.715 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 0.11431(7) 0.22370(8) 0.29895(3) 0.0301(2) Uani 1 1 d . A 1 N1A N -0.01075(8) 0.14726(9) 0.34413(4) 0.0263(2) Uani 1 1 d . A 1 N2A N -0.05220(9) 0.27134(11) 0.27942(5) 0.0362(3) Uani 1 1 d . A 1 C1A C 0.20130(10) -0.05099(11) 0.38308(5) 0.0332(3) Uani 1 1 d . A 1 H1A H 0.2626 -0.0816 0.3709 0.040 Uiso 1 1 calc R A 1 C2A C 0.14426(10) 0.02567(11) 0.35433(5) 0.0308(3) Uani 1 1 d . A 1 H2A H 0.1666 0.0465 0.3231 0.037 Uiso 1 1 calc R A 1 C3A C 0.05412(9) 0.07205(10) 0.37145(5) 0.0255(2) Uani 1 1 d . A 1 C4A C 0.02327(11) 0.03809(13) 0.41714(5) 0.0351(3) Uani 1 1 d . A 1 H4A H -0.0382 0.0681 0.4294 0.042 Uiso 1 1 calc R A 1 C5A C 0.08143(12) -0.03911(13) 0.44495(6) 0.0410(3) Uani 1 1 d . A 1 H5A H 0.0585 -0.0615 0.4759 0.049 Uiso 1 1 calc R A 1 C6A C 0.17214(11) -0.08443(12) 0.42878(5) 0.0350(3) Uani 1 1 d . A 1 C7A C 0.23594(14) -0.16705(14) 0.45950(7) 0.0490(4) Uani 1 1 d . A 1 H7AA H 0.2035 -0.2413 0.4571 0.074 Uiso 1 1 calc GR A 1 H7AB H 0.2400 -0.1424 0.4938 0.074 Uiso 1 1 calc GR A 1 H7AC H 0.3059 -0.1711 0.4476 0.074 Uiso 1 1 calc GR A 1 C8A C 0.02153(9) 0.21528(10) 0.30701(5) 0.0261(2) Uani 1 1 d . A 1 C9A C -0.02082(11) 0.33957(12) 0.23752(5) 0.0336(3) Uani 1 1 d . A 1 H9A H -0.0863 0.3715 0.2220 0.040 Uiso 1 1 calc R A 1 C10A C 0.04603(14) 0.43985(14) 0.25313(6) 0.0488(4) Uani 1 1 d . A 1 H10A H 0.0132 0.4810 0.2791 0.073 Uiso 1 1 calc GR A 1 H10B H 0.0534 0.4895 0.2249 0.073 Uiso 1 1 calc GR A 1 H10C H 0.1145 0.4137 0.2654 0.073 Uiso 1 1 calc GR A 1 C11A C 0.02761(13) 0.27143(15) 0.19779(6) 0.0453(4) Uani 1 1 d . A 1 H11A H 0.0966 0.2459 0.2097 0.068 Uiso 1 1 calc GR A 1 H11B H 0.0336 0.3182 0.1686 0.068 Uiso 1 1 calc GR A 1 H11C H -0.0161 0.2063 0.1895 0.068 Uiso 1 1 calc GR A 1 C12A C -0.16497(12) 0.26204(18) 0.28498(7) 0.0566(5) Uani 1 1 d . A 1 H12A H -0.1749 0.2155 0.3148 0.068 Uiso 1 1 calc R A 1 C13A C -0.21230(15) 0.3767(2) 0.29364(7) 0.0717(7) Uani 1 1 d . A 1 H13A H -0.1725 0.4148 0.3204 0.108 Uiso 1 1 calc GR A 1 H13B H -0.2842 0.3675 0.3025 0.108 Uiso 1 1 calc GR A 1 H13C H -0.2106 0.4217 0.2637 0.108 Uiso 1 1 calc GR A 1 C14A C -0.21918(13) 0.20137(18) 0.24121(10) 0.0709(7) Uani 1 1 d . A 1 H14A H -0.2148 0.2473 0.2116 0.106 Uiso 1 1 calc GR A 1 H14B H -0.2921 0.1890 0.2476 0.106 Uiso 1 1 calc GR A 1 H14C H -0.1854 0.1290 0.2364 0.106 Uiso 1 1 calc GR A 1 O1B O 0.45267(6) 0.38282(8) 0.37522(3) 0.02833(19) Uani 1 1 d . B 2 N1B N 0.31663(8) 0.33507(10) 0.32206(4) 0.0300(2) Uani 1 1 d . B 2 N2B N 0.28917(8) 0.41280(10) 0.39853(4) 0.0296(2) Uani 1 1 d . B 2 C1B C 0.51769(10) 0.32455(13) 0.23006(5) 0.0334(3) Uani 1 1 d . B 2 H1B H 0.5803 0.3612 0.2230 0.040 Uiso 1 1 calc R B 2 C2B C 0.46619(10) 0.35851(12) 0.27073(5) 0.0313(3) Uani 1 1 d . B 2 H2B H 0.4932 0.4179 0.2908 0.038 Uiso 1 1 calc R B 2 C3B C 0.37481(9) 0.30504(11) 0.28190(5) 0.0273(3) Uani 1 1 d . B 2 C4B C 0.33610(10) 0.21957(11) 0.25116(5) 0.0297(3) Uani 1 1 d . B 2 H4B H 0.2731 0.1833 0.2580 0.036 Uiso 1 1 calc R B 2 C5B C 0.38872(10) 0.18725(12) 0.21078(5) 0.0328(3) Uani 1 1 d . B 2 H5B H 0.3614 0.1286 0.1904 0.039 Uiso 1 1 calc R B 2 C6B C 0.48081(10) 0.23887(13) 0.19946(5) 0.0340(3) Uani 1 1 d . B 2 C7B C 0.53710(13) 0.20299(16) 0.15509(6) 0.0476(4) Uani 1 1 d . B 2 H7BA H 0.6004 0.2476 0.1531 0.071 Uiso 1 1 calc GR B 2 H7BB H 0.4922 0.2147 0.1254 0.071 Uiso 1 1 calc GR B 2 H7BC H 0.5552 0.1233 0.1580 0.071 Uiso 1 1 calc GR B 2 C8B C 0.35791(9) 0.37746(10) 0.36606(4) 0.0252(2) Uani 1 1 d . B 2 C9B C 0.32580(10) 0.43797(11) 0.44977(5) 0.0290(3) Uani 1 1 d . B 2 H9B H 0.2624 0.4549 0.4677 0.035 Uiso 1 1 calc R B 2 C10B C 0.37605(12) 0.33641(13) 0.47537(5) 0.0374(3) Uani 1 1 d . B 2 H10D H 0.3305 0.2711 0.4706 0.056 Uiso 1 1 calc GR B 2 H10E H 0.3872 0.3520 0.5105 0.056 Uiso 1 1 calc GR B 2 H10F H 0.4427 0.3208 0.4614 0.056 Uiso 1 1 calc GR B 2 C11B C 0.39304(11) 0.54248(12) 0.45439(5) 0.0345(3) Uani 1 1 d . B 2 H11D H 0.4605 0.5271 0.4412 0.052 Uiso 1 1 calc GR B 2 H11E H 0.4030 0.5636 0.4890 0.052 Uiso 1 1 calc GR B 2 H11F H 0.3590 0.6040 0.4359 0.052 Uiso 1 1 calc GR B 2 C12B C 0.17682(10) 0.42424(14) 0.38684(5) 0.0362(3) Uani 1 1 d . B 2 H12B H 0.1638 0.4063 0.3512 0.043 Uiso 1 1 calc R B 2 C13B C 0.11597(12) 0.34055(15) 0.41550(7) 0.0483(4) Uani 1 1 d . B 2 H13D H 0.1429 0.2649 0.4104 0.073 Uiso 1 1 calc GR B 2 H13E H 0.0428 0.3435 0.4041 0.073 Uiso 1 1 calc GR B 2 H13F H 0.1229 0.3592 0.4505 0.073 Uiso 1 1 calc GR B 2 C14B C 0.14088(12) 0.54425(15) 0.39447(6) 0.0459(4) Uani 1 1 d . B 2 H14D H 0.1496 0.5634 0.4294 0.069 Uiso 1 1 calc GR B 2 H14E H 0.0677 0.5511 0.3835 0.069 Uiso 1 1 calc GR B 2 H14F H 0.1822 0.5955 0.3755 0.069 Uiso 1 1 calc GR B 2 O1C O 0.79550(7) 0.16277(8) 0.40111(4) 0.0331(2) Uani 1 1 d . C 3 N1C N 0.66438(8) 0.28967(9) 0.40538(4) 0.0289(2) Uani 1 1 d . C 3 N2C N 0.63059(8) 0.09866(9) 0.39265(5) 0.0317(2) Uani 1 1 d . C 3 C1C C 0.87976(9) 0.47980(11) 0.44844(5) 0.0300(3) Uani 1 1 d . C 3 H1C H 0.9462 0.4757 0.4650 0.036 Uiso 1 1 calc R C 3 C2C C 0.82464(10) 0.38137(11) 0.43980(5) 0.0290(3) Uani 1 1 d . C 3 H2C H 0.8535 0.3116 0.4504 0.035 Uiso 1 1 calc R C 3 C3C C 0.72679(9) 0.38496(10) 0.41558(4) 0.0248(2) Uani 1 1 d . C 3 C4C C 0.68622(9) 0.48939(11) 0.40157(5) 0.0277(3) Uani 1 1 d . C 3 H4C H 0.6189 0.4938 0.3858 0.033 Uiso 1 1 calc R C 3 C5C C 0.74292(10) 0.58666(11) 0.41036(5) 0.0301(3) Uani 1 1 d . C 3 H5C H 0.7139 0.6567 0.4002 0.036 Uiso 1 1 calc R C 3 C6C C 0.84169(10) 0.58420(11) 0.43380(5) 0.0287(3) Uani 1 1 d . C 3 C7C C 0.90447(11) 0.68978(12) 0.44270(6) 0.0392(3) Uani 1 1 d . C 3 H7CA H 0.8700 0.7381 0.4658 0.059 Uiso 1 1 calc GR C 3 H7CB H 0.9104 0.7297 0.4116 0.059 Uiso 1 1 calc GR C 3 H7CC H 0.9737 0.6701 0.4565 0.059 Uiso 1 1 calc GR C 3 C8C C 0.70144(9) 0.18204(11) 0.39963(5) 0.0269(3) Uani 1 1 d . C 3 C9C C 0.66686(11) -0.01854(12) 0.38816(7) 0.0428(4) Uani 1 1 d . C 3 H9C H 0.6029 -0.0651 0.3830 0.051 Uiso 1 1 calc R C 3 C10C C 0.72889(15) -0.03849(17) 0.34377(9) 0.0660(6) Uani 1 1 d . C 3 H10G H 0.6933 -0.0041 0.3149 0.099 Uiso 1 1 calc GR C 3 H10H H 0.7359 -0.1194 0.3384 0.099 Uiso 1 1 calc GR C 3 H10I H 0.7978 -0.0050 0.3493 0.099 Uiso 1 1 calc GR C 3 C11C C 0.72108(14) -0.06098(14) 0.43618(9) 0.0612(5) Uani 1 1 d . C 3 H11G H 0.7895 -0.0259 0.4408 0.092 Uiso 1 1 calc GR C 3 H11H H 0.7290 -0.1426 0.4346 0.092 Uiso 1 1 calc GR C 3 H11I H 0.6793 -0.0415 0.4638 0.092 Uiso 1 1 calc GR C 3 C12C C 0.51744(10) 0.11371(12) 0.39338(6) 0.0373(3) Uani 1 1 d . C 3 H12C H 0.5042 0.1960 0.3962 0.045 Uiso 1 1 calc R C 3 C13C C 0.46300(14) 0.07468(17) 0.34612(8) 0.0566(5) Uani 1 1 d . C 3 H13G H 0.4942 0.1110 0.3184 0.085 Uiso 1 1 calc GR C 3 H13H H 0.3895 0.0946 0.3460 0.085 Uiso 1 1 calc GR C 3 H13I H 0.4699 -0.0069 0.3433 0.085 Uiso 1 1 calc GR C 3 C14C C 0.47346(14) 0.05806(17) 0.43739(7) 0.0542(4) Uani 1 1 d . C 3 H14G H 0.4857 -0.0230 0.4360 0.081 Uiso 1 1 calc GR C 3 H14H H 0.3988 0.0725 0.4371 0.081 Uiso 1 1 calc GR C 3 H14I H 0.5074 0.0886 0.4675 0.081 Uiso 1 1 calc GR C 3 H15B H 0.2533(14) 0.3090(15) 0.3216(6) 0.035(4) Uiso 1 1 d . . . H15C H 0.5986(14) 0.3042(15) 0.3957(6) 0.037(4) Uiso 1 1 d . . . H15A H -0.0714(13) 0.1588(14) 0.3543(6) 0.030(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1A 0.0230(4) 0.0349(5) 0.0324(5) 0.0034(4) 0.0006(3) -0.0028(3) N1A 0.0201(5) 0.0309(5) 0.0279(5) 0.0017(4) 0.0005(4) 0.0008(4) N2A 0.0257(5) 0.0471(7) 0.0357(6) 0.0141(5) 0.0020(5) 0.0057(5) C1A 0.0277(6) 0.0302(6) 0.0419(7) -0.0007(5) 0.0029(5) 0.0039(5) C2A 0.0292(6) 0.0323(6) 0.0310(6) 0.0001(5) 0.0033(5) 0.0017(5) C3A 0.0223(5) 0.0259(6) 0.0280(6) -0.0013(5) -0.0021(4) -0.0018(4) C4A 0.0319(7) 0.0407(7) 0.0332(7) 0.0054(6) 0.0066(5) 0.0083(6) C5A 0.0447(8) 0.0442(8) 0.0347(7) 0.0112(6) 0.0077(6) 0.0088(6) C6A 0.0358(7) 0.0291(6) 0.0395(7) 0.0029(5) -0.0025(6) 0.0044(5) C7A 0.0519(9) 0.0429(9) 0.0517(10) 0.0112(7) -0.0010(7) 0.0145(7) C8A 0.0258(6) 0.0272(6) 0.0250(6) -0.0009(5) -0.0007(5) -0.0008(5) C9A 0.0343(7) 0.0377(7) 0.0286(6) 0.0073(5) -0.0011(5) 0.0017(5) C10A 0.0644(10) 0.0371(8) 0.0435(9) 0.0085(7) -0.0103(8) -0.0061(7) C11A 0.0472(9) 0.0574(10) 0.0313(7) -0.0006(7) 0.0022(6) 0.0026(7) C12A 0.0286(7) 0.0853(13) 0.0561(10) 0.0373(10) 0.0055(7) 0.0145(8) C13A 0.0486(10) 0.125(2) 0.0412(9) -0.0109(11) 0.0015(8) 0.0383(12) C14A 0.0301(8) 0.0565(11) 0.124(2) 0.0113(12) -0.0151(10) 0.0020(7) O1B 0.0201(4) 0.0360(5) 0.0285(4) -0.0041(4) -0.0017(3) 0.0023(3) N1B 0.0198(5) 0.0426(6) 0.0277(5) -0.0100(5) 0.0020(4) -0.0027(4) N2B 0.0206(5) 0.0428(6) 0.0252(5) -0.0078(4) -0.0007(4) 0.0036(4) C1B 0.0245(6) 0.0449(8) 0.0312(7) 0.0012(6) 0.0034(5) 0.0006(5) C2B 0.0269(6) 0.0373(7) 0.0296(6) -0.0051(5) 0.0013(5) -0.0014(5) C3B 0.0224(6) 0.0347(6) 0.0248(6) -0.0030(5) 0.0004(5) 0.0040(5) C4B 0.0251(6) 0.0368(7) 0.0269(6) -0.0033(5) -0.0002(5) -0.0006(5) C5B 0.0334(7) 0.0378(7) 0.0270(6) -0.0072(5) -0.0012(5) 0.0020(5) C6B 0.0309(6) 0.0437(8) 0.0275(6) -0.0027(6) 0.0028(5) 0.0066(6) C7B 0.0428(8) 0.0639(10) 0.0373(8) -0.0110(7) 0.0119(7) 0.0027(7) C8B 0.0232(6) 0.0281(6) 0.0244(6) -0.0016(5) 0.0004(4) 0.0018(4) C9B 0.0269(6) 0.0371(7) 0.0229(6) -0.0053(5) 0.0000(5) 0.0018(5) C10B 0.0425(8) 0.0404(8) 0.0291(7) 0.0001(6) -0.0002(6) 0.0024(6) C11B 0.0338(7) 0.0375(7) 0.0318(7) -0.0072(5) -0.0021(5) -0.0004(5) C12B 0.0216(6) 0.0555(9) 0.0312(7) -0.0143(6) -0.0022(5) 0.0062(6) C13B 0.0294(7) 0.0525(9) 0.0637(11) -0.0231(8) 0.0078(7) -0.0079(6) C14B 0.0344(7) 0.0582(10) 0.0449(9) 0.0011(7) 0.0004(6) 0.0162(7) O1C 0.0226(4) 0.0303(5) 0.0467(6) -0.0032(4) 0.0038(4) 0.0034(3) N1C 0.0204(5) 0.0255(5) 0.0405(6) 0.0007(4) 0.0002(4) 0.0017(4) N2C 0.0242(5) 0.0235(5) 0.0473(7) -0.0003(5) 0.0011(5) 0.0018(4) C1C 0.0234(6) 0.0348(7) 0.0314(6) -0.0028(5) -0.0020(5) 0.0009(5) C2C 0.0270(6) 0.0285(6) 0.0313(6) 0.0029(5) -0.0017(5) 0.0028(5) C3C 0.0224(5) 0.0264(6) 0.0258(6) -0.0004(5) 0.0041(4) 0.0005(4) C4C 0.0240(6) 0.0285(6) 0.0304(6) -0.0021(5) -0.0009(5) 0.0038(5) C5C 0.0311(6) 0.0251(6) 0.0338(7) -0.0013(5) -0.0001(5) 0.0042(5) C6C 0.0270(6) 0.0296(6) 0.0299(6) -0.0054(5) 0.0036(5) -0.0005(5) C7C 0.0351(7) 0.0324(7) 0.0497(9) -0.0071(6) -0.0001(6) -0.0029(6) C8C 0.0250(6) 0.0262(6) 0.0297(6) 0.0004(5) 0.0024(5) 0.0022(5) C9C 0.0313(7) 0.0243(6) 0.0728(11) -0.0074(7) 0.0037(7) 0.0011(5) C10C 0.0481(10) 0.0540(10) 0.0980(16) -0.0382(11) 0.0220(10) -0.0082(8) C11C 0.0484(9) 0.0328(8) 0.1005(16) 0.0152(9) -0.0105(10) 0.0063(7) C12C 0.0248(6) 0.0273(6) 0.0596(9) 0.0003(6) 0.0013(6) -0.0003(5) C13C 0.0417(9) 0.0629(11) 0.0633(11) 0.0142(9) -0.0150(8) -0.0061(8) C14C 0.0421(8) 0.0597(11) 0.0624(11) -0.0051(9) 0.0150(8) -0.0065(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' 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 -8 0 2 0.2118 8 0 -2 0.2636 0 -4 -15 0.0250 0 -6 11 0.0216 0 6 -11 0.0216 0 1 18 0.0131 0 6 12 0.0148 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C3A N1A H15A 117.2(11) C8A N1A C3A 124.41(10) C8A N1A H15A 117.7(11) C8A N2A C9A 119.01(11) C8A N2A C12A 124.87(12) C12A N2A C9A 115.88(11) C2A C1A H1A 118.8 C6A C1A H1A 118.8 C6A C1A C2A 122.41(12) C1A C2A H2A 120.1 C1A C2A C3A 119.89(13) C3A C2A H2A 120.1 C2A C3A N1A 123.87(12) C4A C3A N1A 117.79(11) C4A C3A C2A 118.27(12) C3A C4A H4A 119.7 C5A C4A C3A 120.62(13) C5A C4A H4A 119.7 C4A C5A H5A 119.1 C6A C5A C4A 121.75(14) C6A C5A H5A 119.1 C1A C6A C5A 117.06(13) C1A C6A C7A 121.41(13) C5A C6A C7A 121.53(14) C6A C7A H7AA 109.5 C6A C7A H7AB 109.5 C6A C7A H7AC 109.5 H7AA C7A H7AB 109.5 H7AA C7A H7AC 109.5 H7AB C7A H7AC 109.5 O1A C8A N1A 121.06(11) O1A C8A N2A 121.28(12) N2A C8A N1A 117.65(11) N2A C9A H9A 105.9 N2A C9A C10A 113.08(12) N2A C9A C11A 113.66(12) C10A C9A H9A 105.9 C11A C9A H9A 105.9 C11A C9A C10A 111.65(13) 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 110.88(17) N2A C12A C14A 111.41(16) C13A C12A H12A 107.4 C13A C12A C14A 112.05(14) C14A C12A H12A 107.4 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 116.1(11) C8B N1B C3B 124.87(11) C8B N1B H15B 117.1(11) C8B N2B C9B 119.57(10) C8B N2B C12B 124.11(11) C12B N2B C9B 116.28(10) C2B C1B H1B 118.9 C6B C1B H1B 118.9 C6B C1B C2B 122.20(13) C1B C2B H2B 120.2 C1B C2B C3B 119.64(12) C3B C2B H2B 120.2 C2B C3B N1B 123.47(12) C2B C3B C4B 118.85(12) C4B C3B N1B 117.65(11) C3B C4B H4B 119.8 C5B C4B C3B 120.47(12) C5B C4B H4B 119.8 C4B C5B H5B 119.3 C4B C5B C6B 121.39(13) C6B C5B H5B 119.3 C1B C6B C5B 117.44(12) C1B C6B C7B 121.80(13) C5B C6B C7B 120.76(13) C6B C7B H7BA 109.5 C6B C7B H7BB 109.5 C6B C7B H7BC 109.5 H7BA C7B H7BB 109.5 H7BA C7B H7BC 109.5 H7BB C7B H7BC 109.5 O1B C8B N1B 121.51(11) O1B C8B N2B 121.99(11) N2B C8B N1B 116.51(10) N2B C9B H9B 106.0 N2B C9B C10B 112.15(11) N2B C9B C11B 113.23(11) C10B C9B H9B 106.0 C11B C9B H9B 106.0 C11B C9B C10B 112.70(11) 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 107.4 N2B C12B C13B 111.19(13) N2B C12B C14B 111.21(12) C13B C12B H12B 107.4 C13B C12B C14B 112.08(12) C14B C12B H12B 107.4 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 115.2(11) C8C N1C C3C 124.83(10) C8C N1C H15C 118.5(11) C8C N2C C9C 119.18(11) C8C N2C C12C 124.81(11) C12C N2C C9C 115.78(11) C2C C1C H1C 118.7 C2C C1C C6C 122.63(11) C6C C1C H1C 118.7 C1C C2C H2C 120.0 C1C C2C C3C 119.91(12) C3C C2C H2C 120.0 C2C C3C N1C 124.18(11) C2C C3C C4C 118.29(11) C4C C3C N1C 117.51(11) C3C C4C H4C 119.6 C5C C4C C3C 120.80(11) C5C C4C H4C 119.6 C4C C5C H5C 119.2 C4C C5C C6C 121.55(12) C6C C5C H5C 119.2 C1C C6C C5C 116.80(12) C1C C6C C7C 121.48(12) C5C C6C C7C 121.73(12) C6C C7C H7CA 109.5 C6C C7C H7CB 109.5 C6C C7C H7CC 109.5 H7CA C7C H7CB 109.5 H7CA C7C H7CC 109.5 H7CB C7C H7CC 109.5 O1C C8C N1C 121.06(12) O1C C8C N2C 121.56(11) N2C C8C N1C 117.37(11) N2C C9C H9C 105.8 N2C C9C C10C 113.60(15) N2C C9C C11C 111.78(14) C10C C9C H9C 105.8 C10C C9C C11C 113.31(16) C11C C9C H9C 105.8 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 107.2 N2C C12C C13C 111.43(14) N2C C12C C14C 112.11(13) C13C C12C H12C 107.2 C13C C12C C14C 111.49(14) C14C C12C H12C 107.2 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 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1A C8A 1.2368(16) N1A C3A 1.4116(16) N1A C8A 1.3813(17) N1A H15A 0.859(17) N2A C8A 1.3567(17) N2A C9A 1.4797(18) N2A C12A 1.4795(19) C1A H1A 0.9500 C1A C2A 1.3888(19) C1A C6A 1.383(2) C2A H2A 0.9500 C2A C3A 1.3952(18) C3A C4A 1.3920(19) C4A H4A 0.9500 C4A C5A 1.387(2) C5A H5A 0.9500 C5A C6A 1.387(2) C6A C7A 1.508(2) C7A H7AA 0.9800 C7A H7AB 0.9800 C7A H7AC 0.9800 C9A H9A 1.0000 C9A C10A 1.522(2) C9A C11A 1.519(2) C10A H10A 0.9800 C10A H10B 0.9800 C10A H10C 0.9800 C11A H11A 0.9800 C11A H11B 0.9800 C11A H11C 0.9800 C12A H12A 1.0000 C12A C13A 1.522(3) C12A C14A 1.532(3) C13A H13A 0.9800 C13A H13B 0.9800 C13A H13C 0.9800 C14A H14A 0.9800 C14A H14B 0.9800 C14A H14C 0.9800 O1B C8B 1.2384(15) N1B C3B 1.4118(16) N1B C8B 1.3824(16) N1B H15B 0.876(18) N2B C8B 1.3586(16) N2B C9B 1.4821(16) N2B C12B 1.4761(16) C1B H1B 0.9500 C1B C2B 1.3881(19) C1B C6B 1.387(2) C2B H2B 0.9500 C2B C3B 1.3922(19) C3B C4B 1.3946(18) C4B H4B 0.9500 C4B C5B 1.3838(19) C5B H5B 0.9500 C5B C6B 1.391(2) C6B C7B 1.511(2) C7B H7BA 0.9800 C7B H7BB 0.9800 C7B H7BC 0.9800 C9B H9B 1.0000 C9B C10B 1.5246(19) C9B C11B 1.5204(19) C10B H10D 0.9800 C10B H10E 0.9800 C10B H10F 0.9800 C11B H11D 0.9800 C11B H11E 0.9800 C11B H11F 0.9800 C12B H12B 1.0000 C12B C13B 1.516(2) C12B C14B 1.522(2) C13B H13D 0.9800 C13B H13E 0.9800 C13B H13F 0.9800 C14B H14D 0.9800 C14B H14E 0.9800 C14B H14F 0.9800 O1C C8C 1.2366(15) N1C C3C 1.4119(16) N1C C8C 1.3817(17) N1C H15C 0.893(18) N2C C8C 1.3580(17) N2C C9C 1.4810(17) N2C C12C 1.4758(17) C1C H1C 0.9500 C1C C2C 1.3860(19) C1C C6C 1.3887(19) C2C H2C 0.9500 C2C C3C 1.3947(18) C3C C4C 1.3958(18) C4C H4C 0.9500 C4C C5C 1.3855(18) C5C H5C 0.9500 C5C C6C 1.3959(19) C6C C7C 1.5098(19) C7C H7CA 0.9800 C7C H7CB 0.9800 C7C H7CC 0.9800 C9C H9C 1.0000 C9C C10C 1.511(3) C9C C11C 1.537(3) C10C H10G 0.9800 C10C H10H 0.9800 C10C H10I 0.9800 C11C H11G 0.9800 C11C H11H 0.9800 C11C H11I 0.9800 C12C H12C 1.0000 C12C C13C 1.508(2) C12C C14C 1.512(2) C13C H13G 0.9800 C13C H13H 0.9800 C13C H13I 0.9800 C14C H14G 0.9800 C14C H14H 0.9800 C14C H14I 0.9800 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 177.42(13) C1A C2A C3A N1A -177.57(12) C1A C2A C3A C4A -0.9(2) C2A C1A C6A C5A 0.9(2) C2A C1A C6A C7A -179.44(14) C2A C3A C4A C5A 0.6(2) C3A N1A C8A O1A -8.37(19) C3A N1A C8A N2A 170.86(12) C3A C4A C5A C6A 0.5(2) C4A C5A C6A C1A -1.3(2) C4A C5A C6A C7A 179.07(15) C6A C1A C2A C3A 0.2(2) C8A N1A C3A C2A -24.76(19) C8A N1A C3A C4A 158.59(13) C8A N2A C9A C10A -65.89(18) C8A N2A C9A C11A 62.75(17) C8A N2A C12A C13A 123.97(16) C8A N2A C12A C14A -110.51(17) C9A N2A C8A O1A 2.8(2) C9A N2A C8A N1A -176.40(12) C9A N2A C12A C13A -61.71(19) C9A N2A C12A C14A 63.8(2) C12A N2A C8A O1A 176.99(15) C12A N2A C8A N1A -2.2(2) C12A N2A C9A C10A 119.43(17) C12A N2A C9A C11A -111.93(17) N1B C3B C4B C5B 179.12(12) C1B C2B C3B N1B -179.07(13) C1B C2B C3B C4B -1.2(2) C2B C1B C6B C5B 0.3(2) C2B C1B C6B C7B 179.61(14) C2B C3B C4B C5B 1.2(2) C3B N1B C8B O1B -6.8(2) C3B N1B C8B N2B 173.19(12) C3B C4B C5B C6B -0.4(2) C4B C5B C6B C1B -0.4(2) C4B C5B C6B C7B -179.70(14) C6B C1B C2B C3B 0.5(2) C8B N1B C3B C2B -31.7(2) C8B N1B C3B C4B 150.48(13) C8B N2B C9B C10B -59.36(16) C8B N2B C9B C11B 69.54(15) C8B N2B C12B C13B 113.61(15) C8B N2B C12B C14B -120.73(14) C9B N2B C8B O1B -12.10(19) C9B N2B C8B N1B 167.94(12) C9B N2B C12B C13B -63.95(16) C9B N2B C12B C14B 61.71(17) C12B N2B C8B O1B 170.42(13) C12B N2B C8B N1B -9.5(2) C12B N2B C9B C10B 118.32(13) C12B N2B C9B C11B -112.78(13) N1C C3C C4C C5C 179.99(12) C1C C2C C3C N1C -179.53(12) C1C C2C C3C C4C -1.35(19) C2C C1C C6C C5C 1.2(2) C2C C1C C6C C7C -178.62(13) C2C C3C C4C C5C 1.68(19) C3C N1C C8C O1C -3.2(2) C3C N1C C8C N2C 176.40(12) C3C C4C C5C C6C -0.6(2) C4C C5C C6C C1C -0.8(2) C4C C5C C6C C7C 178.96(13) C6C C1C C2C C3C -0.1(2) C8C N1C C3C C2C -26.7(2) C8C N1C C3C C4C 155.13(12) C8C N2C C9C C10C -63.84(19) C8C N2C C9C C11C 65.92(18) C8C N2C C12C C13C 122.93(15) C8C N2C C12C C14C -111.31(16) C9C N2C C8C O1C 1.8(2) C9C N2C C8C N1C -177.74(13) C9C N2C C12C C13C -62.56(18) C9C N2C C12C C14C 63.20(18) C12C N2C C8C O1C 176.15(13) C12C N2C C8C N1C -3.4(2) C12C N2C C9C C10C 121.32(15) C12C N2C C9C C11C -108.92(15) loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 0 -3 0.51 0.55 0 0 -4 2676.14 31.76 0 0 -5 0.11 0.97 0 0 -6 9999 106.82 0 0 -7 0.13 1.45 0 0 -8 309.95 9.08 0 0 -9 1.29 1.46 0 0 -10 105.87 5.98 0 0 -11 -1.22 1.67 0 0 -12 453.35 13.68 0 0 -13 0.72 2.18 0 0 -14 54.35 5.32 0 0 -15 1.76 2.13 0 0 -16 75.84 6.65 0 0 -17 -1.76 1.86 0 0 -18 142.17 9.79 0 0 -18 132.21 10.4 0 0 -19 2.23 2.39 0 0 19 -0.11 0.53 0 0 -19 0.1 1.81 0 0 -20 472.57 21.05 0 0 20 492.05 8.2 0 0 21 0.5 0.73 0 0 -21 -0.39 1.75 0 0 -22 17.62 4.31 0 0 22 17.99 1.5 0 0 -23 -3.76 2.55 0 0 23 0.47 0.79 0 0 -24 26.5 5.57 0 0 24 33.7 2.09 0 0 25 0.46 0.85 0 0 26 24.61 1.88 0 0 27 -0.45 0.85 0 0 28 34.34 2.08 0 0 29 0.95 1.01 0 0 30 1.88 0.88 0 0 31 0.22 0.74 0 0 32 4.99 0.76 0 0 33 0.27 0.45 0 1 0 0.39 0.3 0 -1 0 -0.09 0.33 0 -1 -1 70.89 2.11 0 1 1 68.2 2.26 0 1 -1 71.02 2.2 0 1 -2 4386.2 46.32 0 -1 -2 4228.33 45.51 0 -1 -2 4300.13 46.89 0 -1 -3 547.1 8.73 0 -1 -3 537.63 9.58 0 -1 -4 42.89 2.64 0 1 -4 38.53 2.38 0 -1 -4 39.68 2.17 0 1 -5 43.76 2.72 0 1 -5 44.25 2.86 0 -1 -5 43.08 2.84 0 1 -6 441.66 10.4 0 -1 -6 475.16 10.66 0 1 -6 465.09 9.99 0 1 -7 1006.09 17.16 0 -1 -7 959.24 17.65 0 -1 -8 1250.59 21.6 0 1 -8 1258.06 21.16 0 1 -9 224.29 8.09 0 -1 -9 221.55 8.34 0 1 -10 100.92 5.76 0 -1 -10 98.77 5.91 0 1 -11 -0.28 1.66 0 -1 -11 -0.37 1.8 0 1 -11 0.03 1.61 0 1 -12 631.91 17.63 0 1 -12 638.75 16.84 0 -1 -12 668.98 17.41 0 1 -13 214.27 9.71 0 -1 -13 214.13 10.22 0 1 -13 207.07 10.15 0 1 -14 83.91 6.99 0 -1 -14 93.86 6.82 0 1 -14 97.5 6.83 0 1 -15 16.01 3.27 0 -1 -15 15.35 3.4 0 1 -15 11.88 3.27 0 -1 -16 -0.55 2.21 0 1 -16 -0.26 1.71 0 1 -17 -0.88 2.01 0 -1 -17 0.75 1.91 0 -1 -18 87.79 7.75 0 1 -18 79.45 7.95 0 -1 -19 1.88 1.81 0 -1 19 2.86 0.68 0 1 19 2.19 0.62 0 1 -19 1.83 1.62 0 -1 -20 1.62 1.84 0 1 -20 -0.95 2.01 0 -1 -20 -0.79 1.53 0 1 20 0.11 0.58 0 -1 20 0.67 0.59 0 1 21 16.31 1.42 0 -1 -21 20.93 4.5 0 -1 21 16.92 1.37 0 -1 -21 15.67 4.51 0 1 -21 13.42 3.73 0 -1 -22 7.33 3.17 0 -1 22 7.46 1.08 0 1 -22 4.88 2.65 0 1 22 7.1 1.1 0 1 23 123.67 3.86 0 -1 -23 116.38 11.27 0 -1 23 129.7 3.87 0 1 -23 116.74 10.99 0 1 24 106.91 3.64 0 -1 24 108.97 3.64 0 1 25 23.84 1.85 0 -1 25 23.75 1.77 0 -1 26 34.97 2.15 0 1 26 32.49 2.12 0 -1 27 49.96 2.43 0 1 27 46.13 2.42 0 1 28 2.38 0.91 0 -1 28 1.77 0.92 0 1 29 -0.89 0.88 0 -1 29 -0.24 0.83 0 -1 30 16.13 1.33 0 1 30 17.43 1.48 0 -1 31 2.82 0.8 0 1 31 1.45 0.7 0 -1 32 -0.39 0.49 0 1 32 -0.7 0.6 0 -1 33 0.06 0.43 0 1 33 -0.07 0.41 0 -2 0 -0.37 0.6 0 2 0 0.04 0.7 0 -2 1 712.45 11.65 0 -2 -1 684.19 10.98 0 2 1 688.11 11.48 0 2 -1 689.88 11.25 0 -2 -2 7483 79.98 0 -2 -2 7254.27 77.65 0 2 -2 7394.54 78.44 0 2 2 7236.56 78.94 0 2 -3 91.87 3.75 0 -2 -3 89.07 4.08 0 -2 -3 87.52 3.37 0 2 -4 4646.34 52.75 0 -2 -4 4490.74 51.37 0 -2 -4 4625.44 53.89 0 -2 -5 1436.44 20.7 0 2 -5 1472.48 21.82 0 -2 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5 10 1.85 0.42 -14 5 10 2.11 0.34 -14 -5 10 2.68 0.56 -14 5 9 2.07 0.49 -14 5 9 1.59 0.33 -14 -5 9 1.08 0.53 -14 -5 8 0.18 0.3 -14 5 8 0.07 0.41 -14 5 8 0.15 0.25 -14 -5 8 0.97 0.48 -14 -5 7 3.03 0.49 -14 5 7 3.26 0.62 -14 5 7 3.12 0.4 -14 -5 7 3.6 0.64 -14 -5 6 1.45 0.46 -14 5 6 0.04 0.52 -14 5 6 0.56 0.24 -14 -5 6 0.23 0.44 -14 -5 5 13.65 0.94 -14 5 5 11.66 1.07 -14 -5 4 2.82 0.56 -14 5 4 1.87 0.64 -14 -5 4 1.91 0.49 -14 -5 3 54.13 1.87 -14 5 3 59.04 2.2 -14 -5 2 10.49 0.92 -14 5 2 11.2 1.06 -14 -5 2 8.55 0.69 -14 -5 1 12.15 0.99 -14 5 1 12.33 1.1 -14 -5 0 10.5 0.93 -14 5 0 8.41 1.71 -14 5 0 8.34 0.93 -14 -5 -1 4.57 0.73 -14 5 -1 4.69 0.77 -14 -5 -2 23.13 1.32 -14 5 -2 22.94 1.51 -14 5 -2 25.27 1.4 -14 -5 -3 16.89 1.13 -14 5 -3 13.97 1.24 -14 -5 -4 1.2 0.55 -14 5 -4 0.95 0.83 -14 -5 -5 43.16 1.58 -14 5 -5 37.54 1.45 -14 -5 -6 0.21 0.39 -14 5 -6 -0.31 0.59 -14 -5 -7 -0.16 0.39 -14 5 -7 0.8 0.56 -14 -5 -8 4.1 0.48 -14 -6 10 10.32 0.67 -14 6 9 1.21 0.37 -14 -6 9 -0.67 0.35 -14 6 8 8.97 0.73 -14 -6 8 7.52 0.62 -14 6 7 0.88 0.41 -14 -6 7 0.69 0.34 -14 -6 6 0.5 0.32 -14 6 6 0.07 0.43 -14 -6 6 0.84 0.34 -14 -6 5 3.91 0.49 -14 6 5 3.98 0.65 -14 -6 5 2.43 0.41 -14 -6 4 6.71 0.62 -14 6 4 7.46 0.81 -14 -6 3 1.99 0.49 -14 6 3 2.35 0.59 -14 -6 2 0.04 0.41 -14 6 2 -0.29 0.49 -14 -6 1 5.84 0.67 -14 6 1 6.02 0.74 -14 -6 0 1.82 0.5 -14 6 0 2.03 0.57 -14 -6 -1 -0.42 0.44 -14 6 -1 -0.19 0.45 -14 -6 -2 0.35 0.44 -14 6 -2 1.18 0.54 -14 -6 -3 3.42 0.56 -14 -6 -4 -0.82 0.43 -14 -6 -5 8.46 0.67 -14 -6 -6 3.89 0.49 -14 7 5 -0.2 0.32 -14 7 4 0.97 0.38 -14 7 3 9.94 0.72 -14 -7 2 8.33 0.59 -14 7 2 9.69 0.75 -14 -7 1 11.69 0.7 -14 7 1 12.04 0.82 -14 -7 0 0.23 0.33 -14 7 0 -0.58 0.35 -14 -7 -1 32.21 1.13 -14 -7 -2 0.58 0.32 -14 -7 -3 4.63 0.47 -15 0 13 0.38 0.27 -15 0 12 50.59 1.44 -15 0 11 -0.34 0.36 -15 0 10 32.14 1.25 -15 0 9 -0.18 0.42 -15 0 8 41.01 1.5 -15 0 7 1.02 0.51 -15 0 6 1.64 0.6 -15 0 5 0.19 0.55 -15 0 4 33.56 1.42 -15 0 3 0.16 0.58 -15 0 2 19.31 2.02 -15 0 2 22.83 1.17 -15 0 1 1.54 1.5 -15 0 1 0.67 0.48 -15 0 0 13.42 1.42 -15 0 0 15.29 0.94 -15 0 -1 1.89 1.14 -15 0 -1 -0.11 0.41 -15 0 -2 29.36 1.51 -15 0 -2 31.74 1.25 -15 0 -3 0.96 0.86 -15 0 -3 0.43 0.35 -15 0 -4 2.75 0.72 -15 0 -4 2.6 0.39 -15 0 -5 0.18 0.56 -15 0 -6 1.27 0.54 -15 0 -7 -0.36 0.44 -15 0 -8 -0.64 0.45 -15 0 -9 1 0.43 -15 0 -10 2.99 0.46 -15 -1 13 1.47 0.3 -15 1 12 10.08 0.63 -15 -1 12 8.15 0.62 -15 1 11 0.84 0.37 -15 -1 11 -0.28 0.39 -15 1 10 25.35 1.08 -15 -1 10 24 1.09 -15 1 9 0.2 0.39 -15 -1 9 0.41 0.42 -15 1 8 7.48 0.68 -15 -1 8 6.51 0.7 -15 1 7 6.43 0.69 -15 -1 7 4.33 0.62 -15 1 6 5.23 0.69 -15 -1 6 5.89 0.69 -15 1 5 17.22 1.02 -15 -1 5 15.5 0.98 -15 1 4 19.17 1.11 -15 -1 4 16.11 1 -15 1 3 2.1 0.6 -15 -1 3 1.94 0.52 -15 1 2 9.61 1.93 -15 1 2 10.08 0.83 -15 -1 2 7.66 0.74 -15 1 1 0.54 1.49 -15 1 1 0.39 0.51 -15 -1 1 0.28 0.42 -15 -1 0 49.38 2.01 -15 -1 0 52.43 1.66 -15 1 -1 3.4 1.51 -15 -1 -1 2.24 1.19 -15 1 -1 3.6 0.63 -15 -1 -1 4.13 0.53 -15 1 -2 11.11 1.4 -15 -1 -2 10.44 1.18 -15 1 -2 14.06 0.88 -15 -1 -2 13.91 0.85 -15 -1 -3 28.79 1.43 -15 1 -3 29.32 1.55 -15 1 -3 33.74 1.21 -15 -1 -3 30.91 1.12 -15 -1 -4 5.33 0.82 -15 1 -4 5.39 0.89 -15 -1 -5 1.07 0.63 -15 1 -5 1.28 0.66 -15 -1 -6 2.8 0.64 -15 1 -6 1.83 0.56 -15 -1 -7 32.27 1.22 -15 1 -7 35.66 1.35 -15 -1 -8 18.48 0.92 -15 1 -8 19.57 1.01 -15 -1 -9 0.43 0.37 -15 1 -9 0.34 0.38 -15 1 -10 0.8 0.4 -15 -2 13 3.7 0.42 -15 -2 12 92.71 2.03 -15 2 11 10.61 0.67 -15 -2 11 9.44 0.67 -15 2 10 8.64 0.64 -15 -2 10 8.7 0.71 -15 2 9 7.09 0.65 -15 -2 9 6.17 0.64 -15 2 8 0.27 0.4 -15 -2 8 0.83 0.44 -15 2 7 -0.2 0.42 -15 -2 7 -0.21 0.42 -15 2 6 3.1 0.55 -15 -2 6 3.38 0.56 -15 2 5 0.1 0.47 -15 -2 5 -0.4 0.45 -15 2 4 2.26 0.57 -15 -2 4 1.99 0.52 -15 2 3 -0.32 0.52 -15 -2 3 -0.46 0.4 -15 2 2 13.92 2.1 -15 -2 2 12.45 0.84 -15 2 1 6.1 1.8 -15 2 1 6.64 0.72 -15 -2 1 4.3 0.56 -15 -2 0 18.1 1.51 -15 2 0 18.41 1.69 -15 -2 0 20.24 0.96 -15 -2 -1 0.48 1.18 -15 2 -1 0.62 0.46 -15 -2 -1 -0.11 0.33 -15 -2 -2 19.92 1.26 -15 2 -2 22.4 1.43 -15 -2 -2 20.11 0.89 -15 -2 -3 1.73 0.85 -15 2 -3 -1.08 0.81 -15 -2 -4 2.23 0.74 -15 2 -4 1.04 0.7 -15 -2 -5 4.86 0.7 -15 2 -5 5.41 0.76 -15 -2 -6 2.59 0.6 -15 2 -6 2.95 0.62 -15 2 -7 10.52 0.81 -15 2 -8 6.97 0.64 -15 2 -9 2.48 0.48 -15 -3 12 11.92 0.67 -15 -3 11 4.43 0.5 -15 3 10 12.13 0.65 -15 -3 10 10.9 0.73 -15 3 9 1.07 0.3 -15 -3 9 0.83 0.41 -15 3 8 2.86 0.43 -15 -3 8 4.2 0.58 -15 3 7 0.2 0.36 -15 -3 7 -0.71 0.44 -15 3 6 21.58 1.01 -15 -3 6 16.06 0.9 -15 3 5 0.25 0.41 -15 -3 5 0.24 0.38 -15 3 4 1.81 0.47 -15 -3 4 0.98 0.37 -15 3 3 19.58 1.02 -15 -3 3 12.73 0.78 -15 -3 2 0.83 0.5 -15 3 2 0.89 0.48 -15 -3 2 0.28 0.33 -15 -3 1 6.19 0.7 -15 3 1 4.73 1.8 -15 3 1 6.08 0.64 -15 -3 1 5 0.51 -15 -3 0 6.43 0.69 -15 3 0 5.48 1.55 -15 -3 0 5.33 0.46 -15 -3 -1 0.37 0.43 -15 3 -1 1.17 1.33 -15 -3 -2 17.6 1.02 -15 3 -2 13.78 1.34 -15 -3 -3 6.03 0.65 -15 3 -3 5.06 1.07 -15 -3 -4 42.04 1.44 -15 3 -4 33.36 1.47 -15 3 -5 7.87 0.88 -15 3 -6 31.14 1.24 -15 3 -7 1.31 0.58 -15 -4 9 0.78 0.33 -15 -4 8 4.76 0.52 -15 -4 7 1.36 0.35 -15 -4 6 0.09 0.3 -15 -4 5 3.94 0.44 -15 -4 4 24.03 0.94 -15 -4 3 4 0.54 -15 -4 3 3.57 0.4 -15 -4 2 5.91 0.61 -15 -4 1 3.43 0.54 -15 -4 0 7.23 0.69 -15 -4 -1 1.41 0.46 -15 -4 -2 96.17 2.29 -15 4 -2 81.16 2.28 -15 -4 -3 4.84 0.56 -15 4 -3 5.09 1.17 -15 -4 -4 -0.25 0.34 -15 4 -4 -1.12 0.89 -15 -4 -5 1.92 0.36 -15 -5 3 0.56 0.29 -15 -5 2 33.07 1.15 -15 -5 1 5.06 0.52 -15 -5 0 65.83 1.68 -15 -5 -1 -0.12 0.32 -15 -5 -2 1.16 0.33 -16 0 5 -0.04 0.3 -16 0 4 4.01 0.45 -16 1 4 6.51 0.5 -16 1 3 -0.07 0.26 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -8.3849 0.1998 1.9721 -0.1750 0.0849 0.9809 8.3849 -0.1939 -1.9792 0.1758 -0.0853 -0.9807 0.1437 -4.0565 -15.0855 0.3963 0.9141 -0.0858 -0.2988 -6.0246 11.1170 -0.9540 0.2634 -0.1429 0.2988 6.0246 -11.1170 0.9540 -0.2634 0.1429 -0.2925 0.5819 17.6745 -0.7710 -0.6367 0.0092 -0.0598 5.5320 12.3780 -0.1632 -0.9793 0.1195