#------------------------------------------------------------------------------ #$Date: 2020-03-04 09:46:50 +0200 (Wed, 04 Mar 2020) $ #$Revision: 248752 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/74/1557454.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_1557454 loop_ _publ_author_name 'Sharma, Mahendra K.' 'Blomeyer, Sebastian' 'Glodde, Timo' 'Neumann, Beate' 'Stammler, Hans-Georg' 'Hinz, Alexander' 'van Gastel, Maurice' 'Ghadwal, Rajendra S.' _publ_section_title ; Isolation of singlet carbene derived 2-phospha-1,3-butadienes and their sequential one-electron oxidation to radical cations and dications ; _journal_issue 7 _journal_name_full 'Chemical Science' _journal_page_first 1975 _journal_paper_doi 10.1039/C9SC05598C _journal_volume 11 _journal_year 2020 _chemical_formula_moiety 'C54 H72 N3 P' _chemical_formula_sum 'C54 H72 N3 P' _chemical_formula_weight 794.11 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-06-26 _audit_creation_method ; Olex2 1.3-ac4 (compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739) ; _audit_update_record ; 2019-08-28 deposited with the CCDC. 2020-01-06 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.5540(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.56270(10) _cell_length_b 15.9337(2) _cell_length_c 23.6169(2) _cell_measurement_reflns_used 52810 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 76.3720 _cell_measurement_theta_min 3.2990 _cell_volume 4718.31(8) _computing_cell_refinement 'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)' _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 100.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.3114 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -85.00 -19.00 1.00 3.00 -- -38.50 -38.00 60.00 66 2 \w -51.00 33.00 1.00 3.00 -- -38.50 38.00 30.00 84 3 \w -107.00 -19.00 1.00 3.00 -- -38.50 -38.00-150.00 88 4 \w -69.00 29.00 1.00 3.00 -- -38.50 88.00-112.00 98 5 \w -47.00 30.00 1.00 3.00 -- -38.50 38.00-150.00 77 6 \w 17.00 80.00 1.00 3.00 -- 42.89 77.00 150.00 63 7 \w 1.00 78.00 1.00 3.00 -- 42.89 -99.00 90.00 77 8 \w 13.00 114.00 1.00 3.00 -- 42.89 77.00 -60.00 101 9 \w 16.00 65.00 1.00 3.00 -- 42.89 77.00-150.00 49 10 \w 85.00 111.00 1.00 3.00 -- 42.89 57.00 -90.00 26 11 \w 16.00 60.00 1.00 3.00 -- 42.89 77.00 0.00 44 12 \w 18.00 64.00 1.00 3.00 -- 42.89 57.00 -90.00 46 13 \w 13.00 78.00 1.00 3.00 -- 42.89 77.00 90.00 65 14 \w 21.00 95.00 1.00 3.00 -- 42.89 57.00 60.00 74 15 \w 40.00 77.00 1.00 11.98 -- 111.00 -77.00 -90.00 37 16 \w 81.00 108.00 1.00 11.98 -- 111.00 77.00 -60.00 27 17 \w 81.00 107.00 1.00 11.98 -- 111.00 76.00 86.29 26 18 \w 113.00 175.00 1.00 11.98 -- 111.00 77.00 -30.00 62 19 \w 85.00 112.00 1.00 11.98 -- 111.00 61.00 -60.00 27 20 \w 119.00 153.00 1.00 11.98 -- 111.00 51.00-160.62 34 21 \w 84.00 111.00 1.00 11.98 -- 111.00 64.00 -82.88 27 22 \w 81.00 177.00 1.00 11.98 -- 111.00 77.00 60.00 96 23 \w 48.00 141.00 1.00 11.98 -- 111.00 -77.00 60.00 93 24 \w 81.00 107.00 1.00 11.98 -- 111.00 77.00 -30.00 26 25 \w 85.00 111.00 1.00 11.98 -- 111.00 61.00 0.00 26 26 \w 85.00 111.00 1.00 11.98 -- 111.00 61.00 60.00 26 27 \w 81.00 108.00 1.00 11.98 -- 111.00 77.00-120.00 27 28 \w 89.00 115.00 1.00 11.98 -- 111.00 45.00 90.00 26 29 \w 85.00 178.00 1.00 11.98 -- 111.00 61.00 120.00 93 30 \w 58.00 117.00 1.00 11.98 -- 111.00-125.00 30.00 59 31 \w 81.00 108.00 1.00 11.98 -- 111.00 77.00 120.00 27 32 \w 82.00 118.00 1.00 11.98 -- 111.00-125.00 -60.00 36 33 \w 86.00 177.00 1.00 11.98 -- 111.00 61.00 30.00 91 34 \w 83.00 178.00 1.00 11.98 -- 111.00 68.00-144.88 95 35 \w 87.00 115.00 1.00 11.98 -- 111.00 51.00-160.62 28 36 \w 85.00 111.00 1.00 11.98 -- 111.00 61.00-120.00 26 37 \w 81.00 176.00 1.00 11.98 -- 111.00 77.00 150.00 95 38 \w 41.00 118.00 1.00 11.98 -- 111.00-125.00 90.00 77 39 \w 85.00 111.00 1.00 11.98 -- 111.00 61.00 90.00 26 40 \w 116.00 178.00 1.00 11.98 -- 111.00 77.00 -90.00 62 41 \w 81.00 108.00 1.00 11.98 -- 111.00 77.00 0.00 27 42 \w 111.00 178.00 1.00 11.98 -- 111.00 77.00 0.00 67 43 \w 84.00 110.00 1.00 11.98 -- 111.00 65.00-109.92 26 44 \w 81.00 110.00 1.00 11.98 -- 111.00 77.00 90.00 29 45 \w 121.00 171.00 1.00 11.98 -- 111.00 77.00 90.00 50 46 \w 85.00 120.00 1.00 11.98 -- 111.00 61.00 -30.00 35 47 \w 81.00 107.00 1.00 11.98 -- 111.00 77.00 -90.00 26 48 \w 83.00 109.00 1.00 11.98 -- 111.00 77.00 30.00 26 49 \w 81.00 107.00 1.00 11.98 -- 111.00 77.00-180.00 26 50 \w 85.00 111.00 1.00 11.98 -- 111.00 61.00-180.00 26 51 \w 85.00 147.00 1.00 11.98 -- 111.00 61.00-150.00 62 52 \w 42.00 93.00 1.00 11.98 -- 111.00 -77.00-150.00 51 53 \w 107.00 141.00 1.00 11.98 -- 111.00 -77.00-150.00 34 54 \w 85.00 111.00 1.00 11.98 -- 111.00 61.00 -90.00 26 55 \w 85.00 125.00 1.00 11.98 -- 111.00 61.00 150.00 40 56 \w 109.00 178.00 1.00 11.98 -- 111.00 77.00-120.00 69 57 \w 114.00 139.00 1.00 11.98 -- 111.00 -77.00 -90.00 25 58 \w 82.00 108.00 1.00 11.98 -- 111.00 72.00 0.65 26 59 \w 85.00 177.00 1.00 11.98 -- 111.00 59.00 46.28 92 60 \w 63.00 64.00 1.00 11.98 -- 111.00-125.00-150.00 1 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0035436000 _diffrn_orient_matrix_UB_12 -0.0427493000 _diffrn_orient_matrix_UB_13 -0.0583530000 _diffrn_orient_matrix_UB_21 -0.1218682000 _diffrn_orient_matrix_UB_22 0.0095195000 _diffrn_orient_matrix_UB_23 -0.0093074000 _diffrn_orient_matrix_UB_31 0.0151921000 _diffrn_orient_matrix_UB_32 0.0861936000 _diffrn_orient_matrix_UB_33 -0.0279417000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_unetI/netI 0.0152 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 86959 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.717 _diffrn_reflns_theta_min 3.348 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.788 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.543 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019) 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 yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.118 _exptl_crystal_description irregular _exptl_crystal_F_000 1728 _exptl_crystal_size_max 0.449 _exptl_crystal_size_mid 0.312 _exptl_crystal_size_min 0.219 _refine_diff_density_max 0.267 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.039 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 539 _refine_ls_number_reflns 9876 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.030 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0358 _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^)+(0.0477P)^2^+1.7295P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0921 _refine_ls_wR_factor_ref 0.0933 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9416 _reflns_number_total 9876 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc05598c2.cif _cod_data_source_block compound4 _cod_database_code 1557454 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C54 H72 N3 P' _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. ; _diffrn_oxdiff_digest_frames ; 0180a4d5b456edcbad7a27c7fc6e55b281000283ddf ; _diffrn_oxdiff_digest_hkl ; 01c9c8e4428880672235094ca7806e94f101d2 ; _reflns_odcompleteness_completeness 99.97 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 71.98 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C10(H10), C13(H13), C22(H22), C25(H25), C49(H49), C52(H52) 2.b Secondary CH2 refined with riding coordinates: C37(H37A,H37B) 2.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C45(H45), C46(H46), C47(H47) 2.d Idealised Me refined as rotating group: C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B, H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A, H27B,H27C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B, H53C), C54(H54A,H54B,H54C) ; _shelx_res_file ; TITL sharma40_a.res in P2(1)/n sharma40.res created by SHELXL-2018/3 at 09:40:48 on 26-Jun-2019 REM Old TITL sharma40 in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.111, Rweak 0.007, Alpha 0.040 REM 0.994 for 371 systematic absences, Orientation as input REM Formula found by SHELXT: C54 N1 P1 CELL 1.54184 12.5627 15.9337 23.6169 90 93.554 90 ZERR 4 0.0001 0.0002 0.0002 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N P UNIT 216 288 12 4 L.S. 11 PLAN 13 MORE -1 BOND $H CONF fmap 2 acta OMIT -6 18 5 OMIT -6 18 6 OMIT -6 18 7 REM REM REM WGHT 0.047700 1.729500 FVAR 3.30703 P1 4 0.717372 0.261528 0.408684 11.00000 0.01624 0.01828 = 0.01303 0.00163 0.00016 0.00062 N1 3 0.709070 0.408277 0.315277 11.00000 0.01468 0.02110 = 0.01614 0.00385 -0.00017 -0.00116 N2 3 0.543736 0.383506 0.283659 11.00000 0.01497 0.02095 = 0.01421 0.00288 -0.00103 -0.00059 N3 3 0.766744 0.183892 0.507316 11.00000 0.02005 0.01813 = 0.01253 0.00115 -0.00019 0.00008 C1 1 0.616518 0.366640 0.330023 11.00000 0.01393 0.01740 = 0.01528 -0.00111 -0.00029 0.00064 C2 1 0.691575 0.448101 0.262803 11.00000 0.01892 0.02643 = 0.01872 0.00764 0.00226 -0.00050 AFIX 43 H2 2 0.741501 0.479205 0.244258 11.00000 -1.20000 AFIX 0 C3 1 0.591306 0.433876 0.243960 11.00000 0.01974 0.02691 = 0.01679 0.00681 0.00088 0.00133 AFIX 43 H3 2 0.558570 0.453951 0.210244 11.00000 -1.20000 AFIX 0 C4 1 0.809684 0.424587 0.345845 11.00000 0.01531 0.01969 = 0.01818 0.00511 -0.00070 -0.00296 C5 1 0.900438 0.386704 0.325283 11.00000 0.01794 0.02273 = 0.01882 0.00582 0.00053 0.00019 C6 1 0.999959 0.417606 0.345127 11.00000 0.01582 0.02849 = 0.02567 0.00874 0.00107 -0.00033 AFIX 43 H6 2 1.061587 0.394875 0.331510 11.00000 -1.20000 AFIX 0 C7 1 1.007992 0.481499 0.384720 11.00000 0.01956 0.02809 = 0.02888 0.00797 -0.00430 -0.00715 AFIX 43 H7 2 1.074722 0.502479 0.396677 11.00000 -1.20000 AFIX 0 C8 1 0.917122 0.514542 0.406744 11.00000 0.02653 0.02216 = 0.02498 0.00159 -0.00278 -0.00648 AFIX 43 H8 2 0.923985 0.555387 0.434863 11.00000 -1.20000 AFIX 0 C9 1 0.815588 0.487557 0.387437 11.00000 0.02141 0.01948 = 0.02132 0.00326 0.00106 -0.00298 C10 1 0.892492 0.313864 0.283656 11.00000 0.02006 0.02840 = 0.02379 -0.00072 0.00207 0.00289 AFIX 13 H10 2 0.817086 0.298300 0.278183 11.00000 -1.20000 AFIX 0 C11 1 0.930922 0.338616 0.225618 11.00000 0.03264 0.04427 = 0.02288 0.00221 0.00224 0.01027 AFIX 137 H11A 2 0.888994 0.384743 0.210512 11.00000 -1.50000 H11B 2 0.923294 0.291657 0.200223 11.00000 -1.50000 H11C 2 1.004547 0.354951 0.229769 11.00000 -1.50000 AFIX 0 C12 1 0.953399 0.236983 0.307475 11.00000 0.03302 0.02869 = 0.02951 0.00034 0.00566 0.00724 AFIX 137 H12A 2 1.027850 0.250287 0.312990 11.00000 -1.50000 H12B 2 0.944157 0.191159 0.281240 11.00000 -1.50000 H12C 2 0.926338 0.221350 0.343116 11.00000 -1.50000 AFIX 0 C13 1 0.714895 0.525681 0.409320 11.00000 0.02476 0.02247 = 0.02816 -0.00360 0.00618 -0.00452 AFIX 13 H13 2 0.661461 0.480947 0.410050 11.00000 -1.20000 AFIX 0 C14 1 0.668813 0.594863 0.369824 11.00000 0.03296 0.03208 = 0.04049 -0.00001 0.00791 0.00846 AFIX 137 H14A 2 0.719423 0.639822 0.368287 11.00000 -1.50000 H14B 2 0.603919 0.615744 0.384020 11.00000 -1.50000 H14C 2 0.654258 0.572315 0.332450 11.00000 -1.50000 AFIX 0 C15 1 0.731297 0.560488 0.469591 11.00000 0.03738 0.02921 = 0.03309 -0.00997 0.01032 -0.01211 AFIX 137 H15A 2 0.769210 0.520105 0.493311 11.00000 -1.50000 H15B 2 0.663214 0.571652 0.484347 11.00000 -1.50000 H15C 2 0.771762 0.611551 0.468942 11.00000 -1.50000 AFIX 0 C16 1 0.439907 0.348743 0.269732 11.00000 0.01534 0.02193 = 0.01197 0.00045 -0.00100 -0.00043 C17 1 0.352814 0.404102 0.266342 11.00000 0.01780 0.02072 = 0.01310 -0.00001 0.00021 0.00063 C18 1 0.252297 0.371055 0.250687 11.00000 0.01626 0.02564 = 0.01668 0.00094 -0.00042 0.00172 AFIX 43 H18 2 0.193394 0.406487 0.247627 11.00000 -1.20000 AFIX 0 C19 1 0.239259 0.286352 0.239685 11.00000 0.01835 0.02787 = 0.01864 0.00005 -0.00221 -0.00411 AFIX 43 H19 2 0.171555 0.264913 0.230422 11.00000 -1.20000 AFIX 0 C20 1 0.326898 0.233271 0.242428 11.00000 0.02500 0.02008 = 0.01884 -0.00145 -0.00172 -0.00294 AFIX 43 H20 2 0.316931 0.176465 0.234765 11.00000 -1.20000 AFIX 0 C21 1 0.429505 0.262929 0.256378 11.00000 0.02079 0.02138 = 0.01258 -0.00018 -0.00096 0.00162 C22 1 0.363831 0.497505 0.278517 11.00000 0.01909 0.01975 = 0.02287 -0.00144 -0.00041 0.00110 AFIX 13 H22 2 0.437043 0.507998 0.293619 11.00000 -1.20000 AFIX 0 C23 1 0.345158 0.548388 0.223580 11.00000 0.03105 0.02290 = 0.02962 0.00421 0.00646 0.00359 AFIX 137 H23A 2 0.393852 0.529953 0.196388 11.00000 -1.50000 H23B 2 0.356725 0.606872 0.231558 11.00000 -1.50000 H23C 2 0.273222 0.540151 0.208447 11.00000 -1.50000 AFIX 0 C24 1 0.287914 0.527555 0.322721 11.00000 0.02947 0.02358 = 0.02315 -0.00191 0.00077 0.00699 AFIX 137 H24A 2 0.215483 0.520651 0.308009 11.00000 -1.50000 H24B 2 0.301181 0.585733 0.331037 11.00000 -1.50000 H24C 2 0.299558 0.495092 0.356786 11.00000 -1.50000 AFIX 0 C25 1 0.526205 0.205416 0.255486 11.00000 0.02443 0.02213 = 0.01806 -0.00272 -0.00215 0.00483 AFIX 13 H25 2 0.571716 0.216451 0.289890 11.00000 -1.20000 AFIX 0 C26 1 0.591574 0.224547 0.204182 11.00000 0.03512 0.03957 = 0.02606 -0.00019 0.00789 0.01371 AFIX 137 H26A 2 0.549581 0.212245 0.169837 11.00000 -1.50000 H26B 2 0.654803 0.190572 0.206043 11.00000 -1.50000 H26C 2 0.611200 0.282782 0.204597 11.00000 -1.50000 AFIX 0 C27 1 0.497973 0.112099 0.254875 11.00000 0.03498 0.02315 = 0.02858 -0.00724 -0.00791 0.00609 AFIX 137 H27A 2 0.453983 0.099938 0.285667 11.00000 -1.50000 H27B 2 0.562198 0.079437 0.259002 11.00000 -1.50000 H27C 2 0.460004 0.098311 0.219572 11.00000 -1.50000 AFIX 0 C28 1 0.601939 0.316945 0.377054 11.00000 0.01603 0.01748 = 0.01432 -0.00019 -0.00056 -0.00106 C29 1 0.492498 0.287942 0.387064 11.00000 0.01778 0.02207 = 0.01074 0.00118 -0.00105 -0.00274 C30 1 0.410440 0.345080 0.395365 11.00000 0.01947 0.02443 = 0.01542 0.00198 0.00039 -0.00070 AFIX 43 H30 2 0.425443 0.402235 0.396395 11.00000 -1.20000 AFIX 0 C31 1 0.306693 0.317910 0.402114 11.00000 0.01870 0.03738 = 0.02032 0.00369 0.00219 0.00130 AFIX 43 H31 2 0.253116 0.356919 0.407341 11.00000 -1.20000 AFIX 0 C32 1 0.282909 0.233033 0.401078 11.00000 0.01925 0.04191 = 0.02405 0.00502 0.00189 -0.00941 AFIX 43 H32 2 0.213289 0.214940 0.404737 11.00000 -1.20000 AFIX 0 C33 1 0.363836 0.175206 0.394535 11.00000 0.02787 0.02835 = 0.02114 0.00333 -0.00041 -0.01091 AFIX 43 H33 2 0.348626 0.118083 0.394453 11.00000 -1.20000 AFIX 0 C34 1 0.467318 0.202293 0.388117 11.00000 0.02239 0.02245 = 0.01581 0.00100 -0.00075 -0.00321 AFIX 43 H34 2 0.521030 0.162860 0.384442 11.00000 -1.20000 AFIX 0 C35 1 0.699397 0.241737 0.479682 11.00000 0.01680 0.01603 = 0.01638 -0.00054 -0.00138 -0.00289 C36 1 0.625787 0.276857 0.523841 11.00000 0.02026 0.02193 = 0.01413 -0.00073 0.00058 0.00016 C37 1 0.688811 0.253405 0.579833 11.00000 0.02335 0.02536 = 0.01398 -0.00134 -0.00020 0.00090 AFIX 23 H37A 2 0.737814 0.298144 0.591401 11.00000 -1.20000 H37B 2 0.640355 0.244589 0.609695 11.00000 -1.20000 AFIX 0 C38 1 0.750178 0.172962 0.569061 11.00000 0.02300 0.02267 = 0.01220 0.00075 -0.00013 -0.00098 C39 1 0.613515 0.372026 0.519302 11.00000 0.03002 0.02282 = 0.02035 -0.00221 0.00083 0.00445 AFIX 137 H39A 2 0.682706 0.397816 0.521968 11.00000 -1.50000 H39B 2 0.572624 0.392005 0.549566 11.00000 -1.50000 H39C 2 0.577499 0.386076 0.483519 11.00000 -1.50000 AFIX 0 C40 1 0.514060 0.236196 0.521664 11.00000 0.02065 0.03316 = 0.01725 0.00230 0.00273 -0.00099 AFIX 137 H40A 2 0.468337 0.263966 0.493473 11.00000 -1.50000 H40B 2 0.484624 0.241467 0.558049 11.00000 -1.50000 H40C 2 0.519746 0.177871 0.512117 11.00000 -1.50000 AFIX 0 C41 1 0.854295 0.167739 0.606029 11.00000 0.02551 0.02815 = 0.01498 0.00160 -0.00187 0.00243 AFIX 137 H41A 2 0.900884 0.127536 0.590106 11.00000 -1.50000 H41B 2 0.839218 0.150625 0.643675 11.00000 -1.50000 H41C 2 0.888147 0.221777 0.607513 11.00000 -1.50000 AFIX 0 C42 1 0.687501 0.092288 0.579795 11.00000 0.03175 0.02663 = 0.01942 0.00564 0.00114 -0.00421 AFIX 137 H42A 2 0.623482 0.091311 0.555398 11.00000 -1.50000 H42B 2 0.669312 0.090791 0.618667 11.00000 -1.50000 H42C 2 0.730553 0.044364 0.572025 11.00000 -1.50000 AFIX 0 C43 1 0.844666 0.136404 0.478705 11.00000 0.02216 0.01719 = 0.01339 0.00308 -0.00019 0.00205 C44 1 0.814717 0.063021 0.448269 11.00000 0.02658 0.01770 = 0.01467 0.00271 -0.00112 -0.00009 C45 1 0.893835 0.017443 0.422990 11.00000 0.03575 0.01764 = 0.01956 -0.00089 0.00150 0.00226 AFIX 43 H45 2 0.875300 -0.031299 0.403080 11.00000 -1.20000 AFIX 0 C46 1 0.999115 0.043043 0.426847 11.00000 0.03201 0.02379 = 0.02370 0.00236 0.00788 0.00739 AFIX 43 H46 2 1.050827 0.011269 0.410184 11.00000 -1.20000 AFIX 0 C47 1 1.027183 0.115981 0.455542 11.00000 0.02323 0.02435 = 0.02419 0.00492 0.00437 0.00146 AFIX 43 H47 2 1.098043 0.133224 0.457725 11.00000 -1.20000 AFIX 0 C48 1 0.951352 0.164282 0.481307 11.00000 0.02299 0.01923 = 0.01587 0.00414 0.00036 0.00045 C49 1 0.700051 0.033424 0.439323 11.00000 0.02730 0.02006 = 0.02272 -0.00211 -0.00301 -0.00202 AFIX 13 H49 2 0.654055 0.073520 0.457651 11.00000 -1.20000 AFIX 0 C50 1 0.666914 0.031107 0.375751 11.00000 0.03815 0.02734 = 0.02685 -0.00671 -0.00990 0.00141 AFIX 137 H50A 2 0.680138 0.084861 0.359222 11.00000 -1.50000 H50B 2 0.592337 0.018077 0.370580 11.00000 -1.50000 H50C 2 0.707523 -0.011067 0.357651 11.00000 -1.50000 AFIX 0 C51 1 0.683191 -0.053606 0.464868 11.00000 0.03616 0.02401 = 0.03977 0.00212 -0.00066 -0.00781 AFIX 137 H51A 2 0.723337 -0.094426 0.445225 11.00000 -1.50000 H51B 2 0.608811 -0.067754 0.461078 11.00000 -1.50000 H51C 2 0.706862 -0.053167 0.504304 11.00000 -1.50000 AFIX 0 C52 1 0.986443 0.247091 0.508454 11.00000 0.02019 0.02087 = 0.02043 0.00173 -0.00070 -0.00143 AFIX 13 H52 2 0.928440 0.267630 0.530657 11.00000 -1.20000 AFIX 0 C53 1 1.005898 0.312029 0.462644 11.00000 0.02319 0.02249 = 0.02502 0.00417 -0.00266 -0.00318 AFIX 137 H53A 2 1.062587 0.293167 0.440336 11.00000 -1.50000 H53B 2 1.025288 0.364652 0.480191 11.00000 -1.50000 H53C 2 0.942047 0.319076 0.438618 11.00000 -1.50000 AFIX 0 C54 1 1.086299 0.237110 0.548695 11.00000 0.02610 0.02630 = 0.02469 0.00347 -0.00495 -0.00208 AFIX 137 H54A 2 1.075885 0.191759 0.574535 11.00000 -1.50000 H54B 2 1.098788 0.288125 0.569692 11.00000 -1.50000 H54C 2 1.146702 0.225203 0.527035 11.00000 -1.50000 AFIX 0 HKLF 4 REM sharma40_a.res in P2(1)/n REM wR2 = 0.0933, GooF = S = 1.030, Restrained GooF = 1.030 for all data REM R1 = 0.0358 for 9416 Fo > 4sig(Fo) and 0.0373 for all 9876 data REM 539 parameters refined using 0 restraints END WGHT 0.0477 1.7295 REM Highest difference peak 0.267, deepest hole -0.275, 1-sigma level 0.039 Q1 1 0.6587 0.2607 0.4983 11.00000 0.05 0.27 Q2 1 0.5465 0.3013 0.3801 11.00000 0.05 0.25 Q3 1 0.7255 0.2748 0.4563 11.00000 0.05 0.24 Q4 1 0.4797 0.2380 0.2552 11.00000 0.05 0.23 Q5 1 0.8956 0.3524 0.3038 11.00000 0.05 0.23 Q6 1 0.6110 0.3377 0.3538 11.00000 0.05 0.23 Q7 1 0.5542 0.2196 0.2316 11.00000 0.05 0.23 Q8 1 0.6960 0.2558 0.4505 11.00000 0.05 0.22 Q9 1 0.9671 0.1987 0.4950 11.00000 0.05 0.22 Q10 1 0.6486 0.3009 0.3922 11.00000 0.05 0.22 Q11 1 0.3278 0.5138 0.2978 11.00000 0.05 0.22 Q12 1 0.7652 0.5070 0.3991 11.00000 0.05 0.22 Q13 1 0.8975 0.1600 0.4697 11.00000 0.05 0.21 ; _shelx_res_checksum 20090 _olex2_date_sample_data_collection 2019-06-25 _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 2.523 _oxdiff_exptl_absorpt_empirical_full_min 0.471 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.71737(2) 0.26153(2) 0.40868(2) 0.01588(7) Uani 1 1 d . . . . . N1 N 0.70907(7) 0.40828(6) 0.31528(4) 0.01735(17) Uani 1 1 d . . . . . N2 N 0.54374(7) 0.38351(5) 0.28366(3) 0.01679(17) Uani 1 1 d . . . . . N3 N 0.76674(7) 0.18389(5) 0.50732(3) 0.01695(17) Uani 1 1 d . . . . . C1 C 0.61652(7) 0.36664(6) 0.33002(4) 0.01558(19) Uani 1 1 d . . . . . C2 C 0.69157(8) 0.44810(7) 0.26280(4) 0.0213(2) Uani 1 1 d . . . . . H2 H 0.741501 0.479205 0.244258 0.026 Uiso 1 1 calc R . . . . C3 C 0.59131(8) 0.43388(7) 0.24396(4) 0.0212(2) Uani 1 1 d . . . . . H3 H 0.558570 0.453951 0.210244 0.025 Uiso 1 1 calc R . . . . C4 C 0.80968(8) 0.42459(6) 0.34584(4) 0.0178(2) Uani 1 1 d . . . . . C5 C 0.90044(8) 0.38670(7) 0.32528(4) 0.0199(2) Uani 1 1 d . . . . . C6 C 0.99996(8) 0.41761(7) 0.34513(5) 0.0233(2) Uani 1 1 d . . . . . H6 H 1.061587 0.394875 0.331510 0.028 Uiso 1 1 calc R . . . . C7 C 1.00799(9) 0.48150(7) 0.38472(5) 0.0258(2) Uani 1 1 d . . . . . H7 H 1.074722 0.502479 0.396677 0.031 Uiso 1 1 calc R . . . . C8 C 0.91712(9) 0.51454(7) 0.40674(5) 0.0247(2) Uani 1 1 d . . . . . H8 H 0.923985 0.555387 0.434863 0.030 Uiso 1 1 calc R . . . . C9 C 0.81559(8) 0.48756(7) 0.38744(4) 0.0207(2) Uani 1 1 d . . . . . C10 C 0.89249(9) 0.31386(7) 0.28366(5) 0.0241(2) Uani 1 1 d . . . . . H10 H 0.817086 0.298300 0.278183 0.029 Uiso 1 1 calc R . . . . C11 C 0.93092(10) 0.33862(9) 0.22562(5) 0.0332(3) Uani 1 1 d . . . . . H11A H 0.888994 0.384743 0.210512 0.050 Uiso 1 1 calc GR . . . . H11B H 0.923294 0.291657 0.200223 0.050 Uiso 1 1 calc GR . . . . H11C H 1.004547 0.354951 0.229769 0.050 Uiso 1 1 calc GR . . . . C12 C 0.95340(10) 0.23698(8) 0.30748(5) 0.0303(3) Uani 1 1 d . . . . . H12A H 1.027850 0.250287 0.312990 0.045 Uiso 1 1 calc GR . . . . H12B H 0.944157 0.191159 0.281240 0.045 Uiso 1 1 calc GR . . . . H12C H 0.926338 0.221350 0.343116 0.045 Uiso 1 1 calc GR . . . . C13 C 0.71489(9) 0.52568(7) 0.40932(5) 0.0249(2) Uani 1 1 d . . . . . H13 H 0.661461 0.480947 0.410050 0.030 Uiso 1 1 calc R . . . . C14 C 0.66881(11) 0.59486(8) 0.36982(6) 0.0349(3) Uani 1 1 d . . . . . H14A H 0.719423 0.639822 0.368287 0.052 Uiso 1 1 calc GR . . . . H14B H 0.603919 0.615744 0.384020 0.052 Uiso 1 1 calc GR . . . . H14C H 0.654258 0.572315 0.332450 0.052 Uiso 1 1 calc GR . . . . C15 C 0.73130(11) 0.56049(8) 0.46959(5) 0.0329(3) Uani 1 1 d . . . . . H15A H 0.769210 0.520105 0.493311 0.049 Uiso 1 1 calc GR . . . . H15B H 0.663214 0.571652 0.484347 0.049 Uiso 1 1 calc GR . . . . H15C H 0.771762 0.611551 0.468942 0.049 Uiso 1 1 calc GR . . . . C16 C 0.43991(8) 0.34874(7) 0.26973(4) 0.01649(19) Uani 1 1 d . . . . . C17 C 0.35281(8) 0.40410(7) 0.26634(4) 0.01724(19) Uani 1 1 d . . . . . C18 C 0.25230(8) 0.37105(7) 0.25069(4) 0.0196(2) Uani 1 1 d . . . . . H18 H 0.193394 0.406487 0.247627 0.024 Uiso 1 1 calc R . . . . C19 C 0.23926(8) 0.28635(7) 0.23969(4) 0.0218(2) Uani 1 1 d . . . . . H19 H 0.171555 0.264913 0.230422 0.026 Uiso 1 1 calc R . . . . C20 C 0.32690(9) 0.23327(7) 0.24243(4) 0.0214(2) Uani 1 1 d . . . . . H20 H 0.316931 0.176465 0.234765 0.026 Uiso 1 1 calc R . . . . C21 C 0.42951(8) 0.26293(7) 0.25638(4) 0.0183(2) Uani 1 1 d . . . . . C22 C 0.36383(8) 0.49750(7) 0.27852(5) 0.0206(2) Uani 1 1 d . . . . . H22 H 0.437043 0.507998 0.293619 0.025 Uiso 1 1 calc R . . . . C23 C 0.34516(10) 0.54839(7) 0.22358(5) 0.0277(2) Uani 1 1 d . . . . . H23A H 0.393852 0.529953 0.196388 0.041 Uiso 1 1 calc GR . . . . H23B H 0.356725 0.606872 0.231558 0.041 Uiso 1 1 calc GR . . . . H23C H 0.273222 0.540151 0.208447 0.041 Uiso 1 1 calc GR . . . . C24 C 0.28791(9) 0.52756(7) 0.32272(5) 0.0254(2) Uani 1 1 d . . . . . H24A H 0.215483 0.520651 0.308009 0.038 Uiso 1 1 calc GR . . . . H24B H 0.301181 0.585733 0.331037 0.038 Uiso 1 1 calc GR . . . . H24C H 0.299558 0.495092 0.356786 0.038 Uiso 1 1 calc GR . . . . C25 C 0.52620(9) 0.20542(7) 0.25549(4) 0.0217(2) Uani 1 1 d . . . . . H25 H 0.571716 0.216451 0.289890 0.026 Uiso 1 1 calc R . . . . C26 C 0.59157(10) 0.22455(9) 0.20418(5) 0.0333(3) Uani 1 1 d . . . . . H26A H 0.549581 0.212245 0.169837 0.050 Uiso 1 1 calc GR . . . . H26B H 0.654803 0.190572 0.206043 0.050 Uiso 1 1 calc GR . . . . H26C H 0.611200 0.282782 0.204597 0.050 Uiso 1 1 calc GR . . . . C27 C 0.49797(10) 0.11210(7) 0.25488(5) 0.0293(3) Uani 1 1 d . . . . . H27A H 0.453983 0.099938 0.285667 0.044 Uiso 1 1 calc GR . . . . H27B H 0.562198 0.079437 0.259002 0.044 Uiso 1 1 calc GR . . . . H27C H 0.460004 0.098311 0.219572 0.044 Uiso 1 1 calc GR . . . . C28 C 0.60194(8) 0.31695(6) 0.37705(4) 0.01601(19) Uani 1 1 d . . . . . C29 C 0.49250(8) 0.28794(7) 0.38706(4) 0.01694(19) Uani 1 1 d . . . . . C30 C 0.41044(8) 0.34508(7) 0.39537(4) 0.0198(2) Uani 1 1 d . . . . . H30 H 0.425443 0.402235 0.396395 0.024 Uiso 1 1 calc R . . . . C31 C 0.30669(9) 0.31791(8) 0.40211(5) 0.0254(2) Uani 1 1 d . . . . . H31 H 0.253116 0.356919 0.407341 0.031 Uiso 1 1 calc R . . . . C32 C 0.28291(9) 0.23303(8) 0.40108(5) 0.0284(3) Uani 1 1 d . . . . . H32 H 0.213289 0.214940 0.404737 0.034 Uiso 1 1 calc R . . . . C33 C 0.36384(9) 0.17521(8) 0.39454(5) 0.0259(2) Uani 1 1 d . . . . . H33 H 0.348626 0.118083 0.394453 0.031 Uiso 1 1 calc R . . . . C34 C 0.46732(8) 0.20229(7) 0.38812(4) 0.0203(2) Uani 1 1 d . . . . . H34 H 0.521030 0.162860 0.384442 0.024 Uiso 1 1 calc R . . . . C35 C 0.69940(8) 0.24174(6) 0.47968(4) 0.01651(19) Uani 1 1 d . . . . . C36 C 0.62579(8) 0.27686(7) 0.52384(4) 0.0188(2) Uani 1 1 d . . . . . C37 C 0.68881(9) 0.25341(7) 0.57983(4) 0.0210(2) Uani 1 1 d . . . . . H37A H 0.737814 0.298144 0.591401 0.025 Uiso 1 1 calc R . . . . H37B H 0.640355 0.244589 0.609695 0.025 Uiso 1 1 calc R . . . . C38 C 0.75018(8) 0.17296(7) 0.56906(4) 0.0193(2) Uani 1 1 d . . . . . C39 C 0.61351(9) 0.37203(7) 0.51930(5) 0.0244(2) Uani 1 1 d . . . . . H39A H 0.682706 0.397816 0.521968 0.037 Uiso 1 1 calc GR . . . . H39B H 0.572624 0.392005 0.549566 0.037 Uiso 1 1 calc GR . . . . H39C H 0.577499 0.386076 0.483519 0.037 Uiso 1 1 calc GR . . . . C40 C 0.51406(8) 0.23620(8) 0.52166(5) 0.0236(2) Uani 1 1 d . . . . . H40A H 0.468337 0.263966 0.493473 0.035 Uiso 1 1 calc GR . . . . H40B H 0.484624 0.241467 0.558049 0.035 Uiso 1 1 calc GR . . . . H40C H 0.519746 0.177871 0.512117 0.035 Uiso 1 1 calc GR . . . . C41 C 0.85430(9) 0.16774(7) 0.60603(4) 0.0230(2) Uani 1 1 d . . . . . H41A H 0.900884 0.127536 0.590106 0.035 Uiso 1 1 calc GR . . . . H41B H 0.839218 0.150625 0.643675 0.035 Uiso 1 1 calc GR . . . . H41C H 0.888147 0.221777 0.607513 0.035 Uiso 1 1 calc GR . . . . C42 C 0.68750(9) 0.09229(7) 0.57979(5) 0.0260(2) Uani 1 1 d . . . . . H42A H 0.623482 0.091311 0.555398 0.039 Uiso 1 1 calc GR . . . . H42B H 0.669312 0.090791 0.618667 0.039 Uiso 1 1 calc GR . . . . H42C H 0.730553 0.044364 0.572025 0.039 Uiso 1 1 calc GR . . . . C43 C 0.84467(8) 0.13640(6) 0.47871(4) 0.01763(19) Uani 1 1 d . . . . . C44 C 0.81472(9) 0.06302(7) 0.44827(4) 0.0197(2) Uani 1 1 d . . . . . C45 C 0.89383(10) 0.01744(7) 0.42299(5) 0.0243(2) Uani 1 1 d . . . . . H45 H 0.875300 -0.031299 0.403080 0.029 Uiso 1 1 calc R . . . . C46 C 0.99912(10) 0.04304(7) 0.42685(5) 0.0262(2) Uani 1 1 d . . . . . H46 H 1.050827 0.011269 0.410184 0.031 Uiso 1 1 calc R . . . . C47 C 1.02718(9) 0.11598(7) 0.45554(5) 0.0238(2) Uani 1 1 d . . . . . H47 H 1.098043 0.133224 0.457725 0.029 Uiso 1 1 calc R . . . . C48 C 0.95135(8) 0.16428(7) 0.48131(4) 0.0194(2) Uani 1 1 d . . . . . C49 C 0.70005(9) 0.03342(7) 0.43932(5) 0.0236(2) Uani 1 1 d . . . . . H49 H 0.654055 0.073520 0.457651 0.028 Uiso 1 1 calc R . . . . C50 C 0.66691(10) 0.03111(8) 0.37575(5) 0.0313(3) Uani 1 1 d . . . . . H50A H 0.680138 0.084861 0.359222 0.047 Uiso 1 1 calc GR . . . . H50B H 0.592337 0.018077 0.370580 0.047 Uiso 1 1 calc GR . . . . H50C H 0.707523 -0.011067 0.357651 0.047 Uiso 1 1 calc GR . . . . C51 C 0.68319(11) -0.05361(8) 0.46487(6) 0.0334(3) Uani 1 1 d . . . . . H51A H 0.723337 -0.094426 0.445225 0.050 Uiso 1 1 calc GR . . . . H51B H 0.608811 -0.067754 0.461078 0.050 Uiso 1 1 calc GR . . . . H51C H 0.706862 -0.053167 0.504304 0.050 Uiso 1 1 calc GR . . . . C52 C 0.98644(8) 0.24709(7) 0.50845(4) 0.0206(2) Uani 1 1 d . . . . . H52 H 0.928440 0.267630 0.530657 0.025 Uiso 1 1 calc R . . . . C53 C 1.00590(9) 0.31203(7) 0.46264(5) 0.0237(2) Uani 1 1 d . . . . . H53A H 1.062587 0.293167 0.440336 0.036 Uiso 1 1 calc GR . . . . H53B H 1.025288 0.364652 0.480191 0.036 Uiso 1 1 calc GR . . . . H53C H 0.942047 0.319076 0.438618 0.036 Uiso 1 1 calc GR . . . . C54 C 1.08630(9) 0.23711(7) 0.54870(5) 0.0260(2) Uani 1 1 d . . . . . H54A H 1.075885 0.191759 0.574535 0.039 Uiso 1 1 calc GR . . . . H54B H 1.098788 0.288125 0.569692 0.039 Uiso 1 1 calc GR . . . . H54C H 1.146702 0.225203 0.527035 0.039 Uiso 1 1 calc GR . . . . 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 P1 0.01624(12) 0.01828(13) 0.01303(12) 0.00163(9) 0.00016(9) 0.00062(9) N1 0.0147(4) 0.0211(4) 0.0161(4) 0.0039(3) -0.0002(3) -0.0012(3) N2 0.0150(4) 0.0210(4) 0.0142(4) 0.0029(3) -0.0010(3) -0.0006(3) N3 0.0200(4) 0.0181(4) 0.0125(4) 0.0012(3) -0.0002(3) 0.0001(3) C1 0.0139(4) 0.0174(5) 0.0153(4) -0.0011(4) -0.0003(3) 0.0006(3) C2 0.0189(5) 0.0264(5) 0.0187(5) 0.0076(4) 0.0023(4) -0.0005(4) C3 0.0197(5) 0.0269(5) 0.0168(5) 0.0068(4) 0.0009(4) 0.0013(4) C4 0.0153(4) 0.0197(5) 0.0182(5) 0.0051(4) -0.0007(4) -0.0030(4) C5 0.0179(5) 0.0227(5) 0.0188(5) 0.0058(4) 0.0005(4) 0.0002(4) C6 0.0158(5) 0.0285(6) 0.0257(5) 0.0087(4) 0.0011(4) -0.0003(4) C7 0.0196(5) 0.0281(6) 0.0289(6) 0.0080(4) -0.0043(4) -0.0071(4) C8 0.0265(5) 0.0222(5) 0.0250(5) 0.0016(4) -0.0028(4) -0.0065(4) C9 0.0214(5) 0.0195(5) 0.0213(5) 0.0033(4) 0.0011(4) -0.0030(4) C10 0.0201(5) 0.0284(6) 0.0238(5) -0.0007(4) 0.0021(4) 0.0029(4) C11 0.0326(6) 0.0443(7) 0.0229(6) 0.0022(5) 0.0022(5) 0.0103(5) C12 0.0330(6) 0.0287(6) 0.0295(6) 0.0003(5) 0.0057(5) 0.0072(5) C13 0.0248(5) 0.0225(5) 0.0282(6) -0.0036(4) 0.0062(4) -0.0045(4) C14 0.0330(6) 0.0321(7) 0.0405(7) 0.0000(5) 0.0079(5) 0.0085(5) C15 0.0374(7) 0.0292(6) 0.0331(6) -0.0100(5) 0.0103(5) -0.0121(5) C16 0.0153(4) 0.0219(5) 0.0120(4) 0.0004(4) -0.0010(3) -0.0004(4) C17 0.0178(5) 0.0207(5) 0.0131(4) 0.0000(4) 0.0002(3) 0.0006(4) C18 0.0163(4) 0.0256(5) 0.0167(4) 0.0009(4) -0.0004(4) 0.0017(4) C19 0.0184(5) 0.0279(6) 0.0186(5) 0.0001(4) -0.0022(4) -0.0041(4) C20 0.0250(5) 0.0201(5) 0.0188(5) -0.0015(4) -0.0017(4) -0.0029(4) C21 0.0208(5) 0.0214(5) 0.0126(4) -0.0002(4) -0.0010(4) 0.0016(4) C22 0.0191(5) 0.0197(5) 0.0229(5) -0.0014(4) -0.0004(4) 0.0011(4) C23 0.0310(6) 0.0229(5) 0.0296(6) 0.0042(4) 0.0065(5) 0.0036(4) C24 0.0295(6) 0.0236(5) 0.0231(5) -0.0019(4) 0.0008(4) 0.0070(4) C25 0.0244(5) 0.0221(5) 0.0181(5) -0.0027(4) -0.0022(4) 0.0048(4) C26 0.0351(6) 0.0396(7) 0.0261(6) -0.0002(5) 0.0079(5) 0.0137(5) C27 0.0350(6) 0.0232(6) 0.0286(6) -0.0072(4) -0.0079(5) 0.0061(5) C28 0.0160(4) 0.0175(5) 0.0143(4) -0.0002(4) -0.0006(3) -0.0011(4) C29 0.0178(5) 0.0221(5) 0.0107(4) 0.0012(4) -0.0011(3) -0.0027(4) C30 0.0195(5) 0.0244(5) 0.0154(5) 0.0020(4) 0.0004(4) -0.0007(4) C31 0.0187(5) 0.0374(6) 0.0203(5) 0.0037(4) 0.0022(4) 0.0013(4) C32 0.0193(5) 0.0419(7) 0.0241(5) 0.0050(5) 0.0019(4) -0.0094(5) C33 0.0279(6) 0.0284(6) 0.0211(5) 0.0033(4) -0.0004(4) -0.0109(4) C34 0.0224(5) 0.0225(5) 0.0158(5) 0.0010(4) -0.0008(4) -0.0032(4) C35 0.0168(4) 0.0160(5) 0.0164(5) -0.0005(4) -0.0014(4) -0.0029(4) C36 0.0203(5) 0.0219(5) 0.0141(4) -0.0007(4) 0.0006(4) 0.0002(4) C37 0.0233(5) 0.0254(5) 0.0140(5) -0.0013(4) -0.0002(4) 0.0009(4) C38 0.0230(5) 0.0227(5) 0.0122(4) 0.0008(4) -0.0001(4) -0.0010(4) C39 0.0300(6) 0.0228(5) 0.0203(5) -0.0022(4) 0.0008(4) 0.0045(4) C40 0.0206(5) 0.0332(6) 0.0172(5) 0.0023(4) 0.0027(4) -0.0010(4) C41 0.0255(5) 0.0281(6) 0.0150(5) 0.0016(4) -0.0019(4) 0.0024(4) C42 0.0318(6) 0.0266(6) 0.0194(5) 0.0056(4) 0.0011(4) -0.0042(4) C43 0.0222(5) 0.0172(5) 0.0134(4) 0.0031(4) -0.0002(4) 0.0021(4) C44 0.0266(5) 0.0177(5) 0.0147(4) 0.0027(4) -0.0011(4) -0.0001(4) C45 0.0358(6) 0.0176(5) 0.0196(5) -0.0009(4) 0.0015(4) 0.0023(4) C46 0.0320(6) 0.0238(6) 0.0237(5) 0.0024(4) 0.0079(4) 0.0074(4) C47 0.0232(5) 0.0244(5) 0.0242(5) 0.0049(4) 0.0044(4) 0.0015(4) C48 0.0230(5) 0.0192(5) 0.0159(4) 0.0041(4) 0.0004(4) 0.0004(4) C49 0.0273(5) 0.0201(5) 0.0227(5) -0.0021(4) -0.0030(4) -0.0020(4) C50 0.0382(6) 0.0273(6) 0.0268(6) -0.0067(5) -0.0099(5) 0.0014(5) C51 0.0362(6) 0.0240(6) 0.0398(7) 0.0021(5) -0.0007(5) -0.0078(5) C52 0.0202(5) 0.0209(5) 0.0204(5) 0.0017(4) -0.0007(4) -0.0014(4) C53 0.0232(5) 0.0225(5) 0.0250(5) 0.0042(4) -0.0027(4) -0.0032(4) C54 0.0261(5) 0.0263(6) 0.0247(5) 0.0035(4) -0.0049(4) -0.0021(4) 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' P P 0.2955 0.4335 '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 0 4 5 0.1096 0 -4 -5 0.1096 -1 -2 5 0.1415 1 2 -5 0.1415 -1 0 0 0.1836 1 0 0 0.1836 0 -5 -1 0.1587 0 5 1 0.1587 1 -1 -5 0.1064 2 1 5 0.1967 -1 2 -5 0.1298 -2 -1 -5 0.1065 -2 -5 -1 0.1505 3 5 -2 0.1708 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C35 P1 C28 109.70(5) . . ? C1 N1 C4 132.61(8) . . ? C2 N1 C1 110.37(8) . . ? C2 N1 C4 116.59(8) . . ? C1 N2 C16 129.87(8) . . ? C3 N2 C1 110.33(8) . . ? C3 N2 C16 119.23(8) . . ? C35 N3 C38 114.74(8) . . ? C35 N3 C43 122.80(8) . . ? C43 N3 C38 122.45(8) . . ? N1 C1 N2 103.01(8) . . ? C28 C1 N1 128.52(9) . . ? C28 C1 N2 128.37(9) . . ? N1 C2 H2 125.9 . . ? C3 C2 N1 108.25(9) . . ? C3 C2 H2 125.9 . . ? N2 C3 H3 126.0 . . ? C2 C3 N2 108.02(9) . . ? C2 C3 H3 126.0 . . ? C5 C4 N1 117.11(9) . . ? C9 C4 N1 119.13(9) . . ? C9 C4 C5 122.76(9) . . ? C4 C5 C10 122.01(9) . . ? C6 C5 C4 117.50(10) . . ? C6 C5 C10 120.49(10) . . ? C5 C6 H6 119.6 . . ? C7 C6 C5 120.86(10) . . ? C7 C6 H6 119.6 . . ? C6 C7 H7 119.8 . . ? C6 C7 C8 120.40(10) . . ? C8 C7 H7 119.8 . . ? C7 C8 H8 119.4 . . ? C7 C8 C9 121.15(11) . . ? C9 C8 H8 119.4 . . ? C4 C9 C13 120.94(9) . . ? C8 C9 C4 117.17(10) . . ? C8 C9 C13 121.87(10) . . ? C5 C10 H10 107.6 . . ? C5 C10 C11 111.72(10) . . ? C5 C10 C12 111.19(9) . . ? C11 C10 H10 107.6 . . ? C12 C10 H10 107.6 . . ? C12 C10 C11 110.86(9) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13 107.5 . . ? C9 C13 C14 111.75(9) . . ? C9 C13 C15 113.19(10) . . ? C14 C13 H13 107.5 . . ? C15 C13 H13 107.5 . . ? C15 C13 C14 109.23(10) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 N2 117.66(9) . . ? C17 C16 C21 122.44(9) . . ? C21 C16 N2 119.76(9) . . ? C16 C17 C22 122.87(9) . . ? C18 C17 C16 117.83(9) . . ? C18 C17 C22 119.29(9) . . ? C17 C18 H18 119.6 . . ? C19 C18 C17 120.83(10) . . ? C19 C18 H18 119.6 . . ? C18 C19 H19 119.9 . . ? C18 C19 C20 120.15(10) . . ? C20 C19 H19 119.9 . . ? C19 C20 H20 119.2 . . ? C19 C20 C21 121.63(10) . . ? C21 C20 H20 119.2 . . ? C16 C21 C25 121.64(9) . . ? C20 C21 C16 117.01(9) . . ? C20 C21 C25 121.32(10) . . ? C17 C22 H22 108.0 . . ? C17 C22 C23 110.47(9) . . ? C17 C22 C24 112.41(9) . . ? C23 C22 H22 108.0 . . ? C24 C22 H22 108.0 . . ? C24 C22 C23 109.96(9) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 H25 107.8 . . ? C21 C25 C26 110.95(9) . . ? C21 C25 C27 113.62(9) . . ? C26 C25 H25 107.8 . . ? C27 C25 H25 107.8 . . ? C27 C25 C26 108.71(10) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C1 C28 P1 117.72(7) . . ? C1 C28 C29 118.41(8) . . ? C29 C28 P1 120.45(7) . . ? C30 C29 C28 121.21(9) . . ? C30 C29 C34 117.54(9) . . ? C34 C29 C28 121.24(9) . . ? C29 C30 H30 119.4 . . ? C31 C30 C29 121.15(10) . . ? C31 C30 H30 119.4 . . ? C30 C31 H31 119.9 . . ? C32 C31 C30 120.28(11) . . ? C32 C31 H31 119.9 . . ? C31 C32 H32 120.3 . . ? C31 C32 C33 119.45(10) . . ? C33 C32 H32 120.3 . . ? C32 C33 H33 119.9 . . ? C34 C33 C32 120.24(11) . . ? C34 C33 H33 119.9 . . ? C29 C34 H34 119.4 . . ? C33 C34 C29 121.27(10) . . ? C33 C34 H34 119.4 . . ? N3 C35 P1 117.62(7) . . ? N3 C35 C36 107.28(8) . . ? C36 C35 P1 135.04(8) . . ? C35 C36 C37 101.20(8) . . ? C35 C36 C40 114.05(8) . . ? C39 C36 C35 112.04(9) . . ? C39 C36 C37 110.15(9) . . ? C39 C36 C40 109.07(9) . . ? C40 C36 C37 110.10(9) . . ? C36 C37 H37A 110.2 . . ? C36 C37 H37B 110.2 . . ? H37A C37 H37B 108.5 . . ? C38 C37 C36 107.34(8) . . ? C38 C37 H37A 110.2 . . ? C38 C37 H37B 110.2 . . ? N3 C38 C37 99.62(8) . . ? N3 C38 C41 113.40(8) . . ? N3 C38 C42 111.22(8) . . ? C37 C38 C41 111.95(9) . . ? C37 C38 C42 113.95(9) . . ? C41 C38 C42 106.81(9) . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C36 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? C36 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C38 C42 H42A 109.5 . . ? C38 C42 H42B 109.5 . . ? C38 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 N3 120.49(9) . . ? C48 C43 N3 119.12(9) . . ? C48 C43 C44 120.40(9) . . ? C43 C44 C49 123.30(10) . . ? C45 C44 C43 118.35(10) . . ? C45 C44 C49 118.29(10) . . ? C44 C45 H45 119.2 . . ? C46 C45 C44 121.51(10) . . ? C46 C45 H45 119.2 . . ? C45 C46 H46 120.2 . . ? C47 C46 C45 119.69(10) . . ? C47 C46 H46 120.2 . . ? C46 C47 H47 119.4 . . ? C46 C47 C48 121.25(10) . . ? C48 C47 H47 119.4 . . ? C43 C48 C52 122.81(9) . . ? C47 C48 C43 118.74(10) . . ? C47 C48 C52 118.38(10) . . ? C44 C49 H49 108.4 . . ? C44 C49 C50 109.96(9) . . ? C44 C49 C51 112.30(9) . . ? C50 C49 H49 108.4 . . ? C51 C49 H49 108.4 . . ? C51 C49 C50 109.15(10) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50B 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C48 C52 H52 108.0 . . ? C48 C52 C53 110.13(9) . . ? C48 C52 C54 112.07(9) . . ? C53 C52 H52 108.0 . . ? C53 C52 C54 110.38(9) . . ? C54 C52 H52 108.0 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53B 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54B 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C28 1.8183(10) . ? P1 C35 1.7346(10) . ? N1 C1 1.4012(12) . ? N1 C2 1.3975(13) . ? N1 C4 1.4399(12) . ? N2 C1 1.4082(12) . ? N2 C3 1.3963(13) . ? N2 C16 1.4364(12) . ? N3 C35 1.3867(13) . ? N3 C38 1.4959(12) . ? N3 C43 1.4385(13) . ? C1 C28 1.3855(14) . ? C2 H2 0.9300 . ? C2 C3 1.3291(15) . ? C3 H3 0.9300 . ? C4 C5 1.4031(14) . ? C4 C9 1.4029(15) . ? C5 C6 1.3973(15) . ? C5 C10 1.5203(15) . ? C6 H6 0.9300 . ? C6 C7 1.3817(17) . ? C7 H7 0.9300 . ? C7 C8 1.3873(17) . ? C8 H8 0.9300 . ? C8 C9 1.3956(15) . ? C9 C13 1.5223(15) . ? C10 H10 0.9800 . ? C10 C11 1.5328(16) . ? C10 C12 1.5327(16) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13 0.9800 . ? C13 C14 1.5341(17) . ? C13 C15 1.5296(16) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.4038(14) . ? C16 C21 1.4075(15) . ? C17 C18 1.3967(14) . ? C17 C22 1.5205(14) . ? C18 H18 0.9300 . ? C18 C19 1.3822(16) . ? C19 H19 0.9300 . ? C19 C20 1.3867(15) . ? C20 H20 0.9300 . ? C20 C21 1.3931(15) . ? C21 C25 1.5229(14) . ? C22 H22 0.9800 . ? C22 C23 1.5356(15) . ? C22 C24 1.5337(15) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25 0.9800 . ? C25 C26 1.5358(16) . ? C25 C27 1.5285(16) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.4833(13) . ? C29 C30 1.3982(15) . ? C29 C34 1.4015(15) . ? C30 H30 0.9300 . ? C30 C31 1.3919(15) . ? C31 H31 0.9300 . ? C31 C32 1.3849(18) . ? C32 H32 0.9300 . ? C32 C33 1.3878(18) . ? C33 H33 0.9300 . ? C33 C34 1.3870(15) . ? C34 H34 0.9300 . ? C35 C36 1.5413(14) . ? C36 C37 1.5445(14) . ? C36 C39 1.5273(15) . ? C36 C40 1.5439(14) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 C38 1.5252(15) . ? C38 C41 1.5292(14) . ? C38 C42 1.5367(15) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C44 1.4113(14) . ? C43 C48 1.4097(14) . ? C44 C45 1.3947(15) . ? C44 C49 1.5180(15) . ? C45 H45 0.9300 . ? C45 C46 1.3817(17) . ? C46 H46 0.9300 . ? C46 C47 1.3801(17) . ? C47 H47 0.9300 . ? C47 C48 1.3935(15) . ? C48 C52 1.5203(15) . ? C49 H49 0.9800 . ? C49 C50 1.5334(15) . ? C49 C51 1.5322(16) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52 0.9800 . ? C52 C53 1.5276(15) . ? C52 C54 1.5344(15) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 C28 C29 C30 140.89(8) . . . . ? P1 C28 C29 C34 -39.61(12) . . . . ? P1 C35 C36 C37 -158.21(9) . . . . ? P1 C35 C36 C39 -40.88(14) . . . . ? P1 C35 C36 C40 83.62(12) . . . . ? N1 C1 C28 P1 -28.15(14) . . . . ? N1 C1 C28 C29 172.60(9) . . . . ? N1 C2 C3 N2 -1.02(13) . . . . ? N1 C4 C5 C6 164.47(9) . . . . ? N1 C4 C5 C10 -16.43(14) . . . . ? N1 C4 C9 C8 -165.77(9) . . . . ? N1 C4 C9 C13 12.95(15) . . . . ? N2 C1 C28 P1 147.63(9) . . . . ? N2 C1 C28 C29 -11.61(16) . . . . ? N2 C16 C17 C18 177.60(8) . . . . ? N2 C16 C17 C22 -1.97(14) . . . . ? N2 C16 C21 C20 -179.08(9) . . . . ? N2 C16 C21 C25 -0.82(14) . . . . ? N3 C35 C36 C37 18.75(10) . . . . ? N3 C35 C36 C39 136.08(9) . . . . ? N3 C35 C36 C40 -99.41(10) . . . . ? N3 C43 C44 C45 -177.68(9) . . . . ? N3 C43 C44 C49 5.29(15) . . . . ? N3 C43 C48 C47 177.27(9) . . . . ? N3 C43 C48 C52 -5.91(14) . . . . ? C1 N1 C2 C3 0.50(13) . . . . ? C1 N1 C4 C5 115.15(12) . . . . ? C1 N1 C4 C9 -75.93(14) . . . . ? C1 N2 C3 C2 1.20(12) . . . . ? C1 N2 C16 C17 119.32(11) . . . . ? C1 N2 C16 C21 -64.91(14) . . . . ? C1 C28 C29 C30 -60.45(13) . . . . ? C1 C28 C29 C34 119.05(11) . . . . ? C2 N1 C1 N2 0.23(11) . . . . ? C2 N1 C1 C28 176.84(10) . . . . ? C2 N1 C4 C5 -73.28(12) . . . . ? C2 N1 C4 C9 95.65(12) . . . . ? C3 N2 C1 N1 -0.85(11) . . . . ? C3 N2 C1 C28 -177.47(10) . . . . ? C3 N2 C16 C17 -70.22(12) . . . . ? C3 N2 C16 C21 105.56(11) . . . . ? C4 N1 C1 N2 172.20(10) . . . . ? C4 N1 C1 C28 -11.19(18) . . . . ? C4 N1 C2 C3 -172.90(9) . . . . ? C4 C5 C6 C7 1.78(15) . . . . ? C4 C5 C10 C11 113.20(11) . . . . ? C4 C5 C10 C12 -122.35(11) . . . . ? C4 C9 C13 C14 -82.51(13) . . . . ? C4 C9 C13 C15 153.68(10) . . . . ? C5 C4 C9 C8 2.50(15) . . . . ? C5 C4 C9 C13 -178.79(10) . . . . ? C5 C6 C7 C8 1.86(17) . . . . ? C6 C5 C10 C11 -67.73(13) . . . . ? C6 C5 C10 C12 56.72(13) . . . . ? C6 C7 C8 C9 -3.48(17) . . . . ? C7 C8 C9 C4 1.31(16) . . . . ? C7 C8 C9 C13 -177.39(10) . . . . ? C8 C9 C13 C14 96.15(13) . . . . ? C8 C9 C13 C15 -27.67(15) . . . . ? C9 C4 C5 C6 -4.02(15) . . . . ? C9 C4 C5 C10 175.08(10) . . . . ? C10 C5 C6 C7 -177.34(10) . . . . ? C16 N2 C1 N1 170.28(9) . . . . ? C16 N2 C1 C28 -6.33(17) . . . . ? C16 N2 C3 C2 -171.01(9) . . . . ? C16 C17 C18 C19 0.85(15) . . . . ? C16 C17 C22 C23 109.90(11) . . . . ? C16 C17 C22 C24 -126.86(10) . . . . ? C16 C21 C25 C26 -71.65(13) . . . . ? C16 C21 C25 C27 165.52(9) . . . . ? C17 C16 C21 C20 -3.51(15) . . . . ? C17 C16 C21 C25 174.75(9) . . . . ? C17 C18 C19 C20 -1.95(16) . . . . ? C18 C17 C22 C23 -69.66(12) . . . . ? C18 C17 C22 C24 53.57(13) . . . . ? C18 C19 C20 C21 0.26(16) . . . . ? C19 C20 C21 C16 2.38(15) . . . . ? C19 C20 C21 C25 -175.89(10) . . . . ? C20 C21 C25 C26 106.54(12) . . . . ? C20 C21 C25 C27 -16.30(14) . . . . ? C21 C16 C17 C18 1.94(15) . . . . ? C21 C16 C17 C22 -177.63(9) . . . . ? C22 C17 C18 C19 -179.56(9) . . . . ? C28 P1 C35 N3 165.51(7) . . . . ? C28 P1 C35 C36 -17.77(11) . . . . ? C28 C29 C30 C31 176.97(9) . . . . ? C28 C29 C34 C33 -176.61(9) . . . . ? C29 C30 C31 C32 0.42(16) . . . . ? C30 C29 C34 C33 2.91(15) . . . . ? C30 C31 C32 C33 1.44(17) . . . . ? C31 C32 C33 C34 -1.10(17) . . . . ? C32 C33 C34 C29 -1.13(16) . . . . ? C34 C29 C30 C31 -2.55(14) . . . . ? C35 P1 C28 C1 154.73(8) . . . . ? C35 P1 C28 C29 -46.47(9) . . . . ? C35 N3 C38 C37 -18.34(11) . . . . ? C35 N3 C38 C41 -137.45(9) . . . . ? C35 N3 C38 C42 102.16(10) . . . . ? C35 N3 C43 C44 -82.11(12) . . . . ? C35 N3 C43 C48 97.69(11) . . . . ? C35 C36 C37 C38 -30.53(10) . . . . ? C36 C37 C38 N3 29.67(10) . . . . ? C36 C37 C38 C41 149.84(9) . . . . ? C36 C37 C38 C42 -88.81(10) . . . . ? C38 N3 C35 P1 177.21(7) . . . . ? C38 N3 C35 C36 -0.36(11) . . . . ? C38 N3 C43 C44 96.24(11) . . . . ? C38 N3 C43 C48 -83.96(12) . . . . ? C39 C36 C37 C38 -149.22(9) . . . . ? C40 C36 C37 C38 90.46(10) . . . . ? C43 N3 C35 P1 -4.32(13) . . . . ? C43 N3 C35 C36 178.10(9) . . . . ? C43 N3 C38 C37 163.18(9) . . . . ? C43 N3 C38 C41 44.08(13) . . . . ? C43 N3 C38 C42 -76.32(12) . . . . ? C43 C44 C45 C46 -0.54(16) . . . . ? C43 C44 C49 C50 118.83(11) . . . . ? C43 C44 C49 C51 -119.43(11) . . . . ? C43 C48 C52 C53 -103.90(11) . . . . ? C43 C48 C52 C54 132.81(10) . . . . ? C44 C43 C48 C47 -2.93(15) . . . . ? C44 C43 C48 C52 173.89(9) . . . . ? C44 C45 C46 C47 -1.01(17) . . . . ? C45 C44 C49 C50 -58.21(13) . . . . ? C45 C44 C49 C51 63.54(13) . . . . ? C45 C46 C47 C48 0.59(17) . . . . ? C46 C47 C48 C43 1.37(16) . . . . ? C46 C47 C48 C52 -175.59(10) . . . . ? C47 C48 C52 C53 72.93(12) . . . . ? C47 C48 C52 C54 -50.36(13) . . . . ? C48 C43 C44 C45 2.52(15) . . . . ? C48 C43 C44 C49 -174.51(9) . . . . ? C49 C44 C45 C46 176.64(10) . . . . ? 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 0.0006 4.0039 4.9960 -0.4627 -0.0085 0.2055 -0.0006 -4.0039 -4.9960 0.4627 0.0085 -0.2055 -1.0004 -1.9996 4.9954 -0.2096 0.0564 -0.3271 1.0004 1.9996 -4.9954 0.2096 -0.0564 0.3271 -1.0000 -0.0003 0.0002 -0.0035 0.1219 -0.0152 1.0000 0.0003 -0.0002 0.0035 -0.1219 0.0152 -0.0008 -5.0030 -0.9997 0.2722 -0.0382 -0.4033 0.0008 5.0030 0.9997 -0.2722 0.0382 0.4033 0.9999 -1.0020 -4.9958 0.3379 -0.0849 0.0684 2.0001 1.0028 4.9953 -0.3273 -0.2807 -0.0228 -0.9996 1.9991 -4.9951 0.2025 0.1873 0.2967 -2.0001 -1.0028 -4.9953 0.3273 0.2807 0.0228 -2.0008 -5.0036 -0.9994 0.2651 0.2055 -0.4337 3.0008 5.0028 -1.9980 -0.0866 -0.2995 0.5326