#------------------------------------------------------------------------------ #$Date: 2019-06-05 04:02:48 +0300 (Wed, 05 Jun 2019) $ #$Revision: 215694 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/12/1551214.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_1551214 _journal_paper_doi 10.1039/C9DT02118C _chemical_formula_moiety 'C38 H68 B2 Ca N13 O3 P3, C6 H18 N3 O P' _chemical_formula_sum 'C44 H86 B2 Ca N16 O4 P4' _chemical_formula_weight 1088.86 _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 geom _atom_sites_solution_primary iterative _audit_creation_date 2019-04-16 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-04-28 deposited with the CCDC. 2019-06-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 106.430(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 22.1723(9) _cell_length_b 14.0207(5) _cell_length_c 20.0498(8) _cell_measurement_reflns_used 16833 _cell_measurement_temperature 180.00(10) _cell_measurement_theta_max 30.0260 _cell_measurement_theta_min 3.7980 _cell_volume 5978.4(4) _computing_cell_refinement 'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)' _computing_data_collection 'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)' _computing_data_reduction 'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)' _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 'olex2.solve (Bourhis et al., 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 180.00(10) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.991 _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 -95.00 -13.00 0.50 14.00 -- -5.70 0.00 90.00 164 2 \w -33.00 7.00 0.50 14.00 -- -5.70 -82.00-120.00 80 3 \w -33.00 23.00 0.50 14.00 -- -5.70 -82.00 60.00 112 4 \w 29.00 80.00 0.50 14.00 -- -5.70 0.00 90.00 102 5 \w 5.00 30.00 0.50 14.00 -- -5.70 -77.00-180.00 50 6 \w -18.00 8.00 0.50 14.00 -- 6.00 -82.00-180.00 52 7 \w -46.00 27.00 0.50 14.00 -- 6.00 -77.00 120.00 146 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC12 (RINC): Kappa single' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0090946000 _diffrn_orient_matrix_UB_12 0.0476946000 _diffrn_orient_matrix_UB_13 -0.0037637000 _diffrn_orient_matrix_UB_21 0.0294437000 _diffrn_orient_matrix_UB_22 -0.0085224000 _diffrn_orient_matrix_UB_23 0.0247712000 _diffrn_orient_matrix_UB_31 0.0127921000 _diffrn_orient_matrix_UB_32 -0.0144391000 _diffrn_orient_matrix_UB_33 -0.0270929000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_unetI/netI 0.0285 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 66463 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.485 _diffrn_reflns_theta_min 3.477 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.264 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.65629 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.210 _exptl_crystal_description block _exptl_crystal_F_000 2336 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.258 _refine_diff_density_min -0.918 _refine_diff_density_rms 0.076 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 829 _refine_ls_number_reflns 13570 _refine_ls_number_restraints 606 _refine_ls_restrained_S_all 1.097 _refine_ls_R_factor_all 0.1004 _refine_ls_R_factor_gt 0.0826 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0972P)^2^+11.2799P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2082 _refine_ls_wR_factor_ref 0.2216 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10683 _reflns_number_total 13570 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL exp_1985_a.res in P2(1)/c exp_1985.res created by SHELXL-2017/1 at 20:12:02 on 16-Apr-2019 REM Old TITL exp_1985 in P21/c #14 REM SHELXT solution in P2(1)/c REM R1 0.244, Rweak 0.022, Alpha 0.050, Orientation as input REM Formula found by SHELXT: C53 Ca N5AA O8 P4 CELL 0.71073 22.172329 14.02066 20.049749 90 106.4303 90 ZERR 4 0.000861 0.000521 0.000802 0 0.0042 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H B Ca N O P UNIT 176 344 8 4 64 16 16 SIMU 0.01 0.02 2 $C $N L.S. 10 0 0 PLAN 40 SIZE 0.1 0.1 0.1 list 4 fmap 2 53 acta SHEL 999 0.77 OMIT -1 0 4 OMIT -7 1 3 OMIT -2 2 2 OMIT 2 4 6 OMIT -1 4 1 OMIT 1 2 3 OMIT -4 1 1 OMIT -6 1 3 OMIT -4 2 2 OMIT -1 2 6 OMIT -2 7 6 OMIT -2 0 4 OMIT -13 2 11 OMIT -12 3 16 OMIT 4 2 2 OMIT 0 3 1 REM REM REM WGHT 0.097200 11.279900 FVAR 0.24635 0.45384 CA1 4 0.217494 0.714684 0.479862 11.00000 0.03072 0.02592 = 0.03553 -0.00771 0.00328 -0.00053 P002 7 0.241045 0.950568 0.574628 11.00000 0.05135 0.03077 = 0.03187 -0.00942 0.01368 -0.00861 P003 7 0.242737 0.586995 0.644993 11.00000 0.04162 0.03125 = 0.06045 0.01273 0.00020 -0.00724 P004 7 0.406633 0.329250 0.357080 11.00000 0.08476 0.02885 = 0.03088 0.00097 0.00152 0.00507 O2 6 0.232804 0.866730 0.528851 11.00000 0.05352 0.02960 = 0.04274 -0.00975 0.01659 -0.00538 O3 6 0.219456 0.655766 0.587426 11.00000 0.04801 0.03401 = 0.04300 0.00265 0.00392 0.00101 O4 6 0.363313 0.396810 0.310124 11.00000 0.06594 0.03502 = 0.03436 0.00003 0.01302 0.00966 O1 6 0.116515 0.769332 0.430422 11.00000 0.04226 0.05199 = 0.04392 -0.00611 -0.00169 0.00860 N3 5 0.305564 0.710950 0.432161 11.00000 0.03815 0.02925 = 0.03458 -0.00438 0.00795 -0.00432 N1 5 0.246495 0.447042 0.364491 11.00000 0.05108 0.02722 = 0.03345 -0.00221 0.01685 -0.00118 AFIX 43 H1 2 0.277071 0.433491 0.347632 11.00000 -1.20000 AFIX 0 N4 5 0.353841 0.597834 0.367883 11.00000 0.04513 0.02716 = 0.03377 -0.00142 0.01050 0.00033 AFIX 43 H4 2 0.352466 0.543697 0.347340 11.00000 -1.20000 AFIX 0 N2 5 0.195437 0.561290 0.424116 11.00000 0.03570 0.03416 = 0.06569 -0.02335 0.00779 -0.00417 N11 5 0.295536 0.633759 0.709533 11.00000 0.06310 0.03740 = 0.03689 0.00257 0.00989 0.00448 C11 1 0.403110 0.658559 0.369426 11.00000 0.04089 0.03738 = 0.02690 0.00697 0.00494 0.00437 C4 1 0.200589 0.379496 0.360412 11.00000 0.05431 0.02332 = 0.02767 0.00040 0.00910 -0.00081 C5 1 0.150695 0.402235 0.388819 11.00000 0.03777 0.03089 = 0.03500 -0.00783 -0.00167 -0.00244 N8 5 0.201013 0.937334 0.630876 11.00000 0.05729 0.07114 = 0.03885 -0.01667 0.02036 -0.01449 C17 1 0.354595 0.772779 0.433223 11.00000 0.04049 0.03261 = 0.03205 -0.00251 0.00630 -0.00531 C16 1 0.404118 0.748395 0.403033 11.00000 0.03774 0.03575 = 0.02710 0.00509 0.00342 -0.00113 C6 1 0.102129 0.333825 0.385796 11.00000 0.04400 0.04011 = 0.05135 -0.01495 0.00091 -0.01071 N00M 5 0.480302 0.356579 0.364670 11.00000 0.07956 0.06335 = 0.04538 0.01017 0.00403 0.02060 N00N 5 0.406332 0.325908 0.438668 11.00000 0.12035 0.06164 = 0.03376 0.00947 0.01127 -0.01350 C12 1 0.450125 0.634803 0.338864 11.00000 0.05292 0.04962 = 0.04231 0.00489 0.01771 0.00640 AFIX 43 H12 2 0.449472 0.575954 0.317270 11.00000 -1.20000 AFIX 0 C15 1 0.454638 0.813401 0.405712 11.00000 0.03990 0.04848 = 0.03506 0.00743 0.00446 -0.00668 C1 1 0.106083 0.243499 0.355605 11.00000 0.06457 0.03159 = 0.04938 -0.00556 0.01117 -0.01349 AFIX 43 H1A 2 0.075736 0.197335 0.354670 11.00000 -1.20000 AFIX 0 C20 1 0.455245 0.902428 0.438859 11.00000 0.05170 0.04832 = 0.05001 -0.00144 0.00947 -0.01996 AFIX 43 H20 2 0.487844 0.945309 0.441524 11.00000 -1.20000 AFIX 0 C14 1 0.501268 0.785986 0.373142 11.00000 0.04635 0.06235 = 0.05001 0.01327 0.01438 -0.00686 AFIX 43 H14 2 0.534198 0.827475 0.373968 11.00000 -1.20000 AFIX 0 C13 1 0.498490 0.700025 0.340781 11.00000 0.05314 0.06695 = 0.05254 0.01109 0.02483 0.00526 AFIX 43 H13 2 0.529361 0.684257 0.319489 11.00000 -1.20000 AFIX 0 C18 1 0.357926 0.862731 0.464294 11.00000 0.05623 0.04167 = 0.05918 -0.01714 0.02386 -0.01406 AFIX 43 H18 2 0.326297 0.881457 0.483634 11.00000 -1.20000 AFIX 0 C3 1 0.201154 0.290520 0.329555 11.00000 0.08661 0.03131 = 0.06980 -0.01430 0.04388 -0.00681 AFIX 43 H3 2 0.233159 0.275230 0.309822 11.00000 -1.20000 AFIX 0 B1 3 0.245719 0.540129 0.395932 11.00000 0.03925 0.02504 = 0.02566 -0.00242 0.00018 0.00170 B2 3 0.304495 0.620798 0.399089 11.00000 0.03648 0.02847 = 0.02587 0.00181 0.00259 0.00035 C10 1 0.149262 0.493906 0.420541 11.00000 0.03470 0.04377 = 0.08434 -0.03299 0.01288 -0.00802 N10 5 0.314568 0.967827 0.614763 11.00000 0.06110 0.15415 = 0.04761 -0.04287 0.02040 -0.05469 C19 1 0.407869 0.925214 0.466910 11.00000 0.06354 0.04485 = 0.06488 -0.01892 0.02006 -0.02013 AFIX 43 H19 2 0.408701 0.984114 0.488483 11.00000 -1.20000 AFIX 0 C2 1 0.153784 0.224302 0.328204 11.00000 0.09588 0.02853 = 0.07708 -0.01581 0.03508 -0.01344 AFIX 43 H2 2 0.155146 0.165091 0.307774 11.00000 -1.20000 AFIX 0 PART 1 N012 5 0.287983 0.496969 0.618489 21.00000 0.02903 0.03863 = 0.05842 -0.00367 0.02086 0.00348 PART 0 N9 5 0.216571 1.048038 0.530795 11.00000 0.15579 0.03986 = 0.13629 0.02790 0.10075 0.02996 PART 1 N014 5 0.402332 0.221907 0.321080 21.00000 0.09626 0.03093 = 0.05928 -0.00594 0.00245 0.01196 PART 0 C015 1 0.345651 0.583897 0.760498 11.00000 0.07539 0.06273 = 0.04638 -0.00160 -0.00465 0.01356 AFIX 137 H01A 2 0.334248 0.576576 0.802976 11.00000 -1.50000 H01B 2 0.383852 0.620098 0.769308 11.00000 -1.50000 H01C 2 0.351853 0.522182 0.742771 11.00000 -1.50000 AFIX 0 C016 1 0.497954 0.387021 0.303075 11.00000 0.08229 0.08059 = 0.05876 -0.00382 0.02093 0.02373 AFIX 137 H01 2 0.519461 0.335952 0.287513 11.00000 -1.50000 H 2 0.525177 0.441490 0.314402 11.00000 -1.50000 HA 2 0.460824 0.403627 0.266832 11.00000 -1.50000 AFIX 0 C017 1 0.217830 0.979297 0.700424 11.00000 0.08227 0.08040 = 0.04188 -0.01922 0.02615 -0.00513 AFIX 137 H01D 2 0.260142 1.002994 0.711736 11.00000 -1.50000 H01E 2 0.214764 0.931623 0.733679 11.00000 -1.50000 H01F 2 0.189632 1.030839 0.701545 11.00000 -1.50000 AFIX 0 C018 1 0.345505 0.199890 0.262843 11.00000 0.09527 0.04980 = 0.06761 -0.02435 -0.00191 0.00285 PART 1 AFIX 137 H7AA 2 0.317194 0.161290 0.279720 21.00000 -1.50000 HB 2 0.357703 0.165926 0.227148 21.00000 -1.50000 HC 2 0.324953 0.258248 0.244086 21.00000 -1.50000 AFIX 137 PART 0 PART 2 HD 2 0.318513 0.252665 0.243870 -21.00000 -1.50000 HE 2 0.320522 0.143763 0.262091 -21.00000 -1.50000 HF 2 0.374094 0.189118 0.235505 -21.00000 -1.50000 AFIX 0 PART 0 C019 1 0.139740 0.889859 0.610373 11.00000 0.06292 0.12836 = 0.06661 -0.02562 0.03036 -0.03115 AFIX 137 H01G 2 0.107117 0.936153 0.607041 11.00000 -1.50000 H01H 2 0.138022 0.842778 0.644554 11.00000 -1.50000 H01I 2 0.133886 0.859504 0.566075 11.00000 -1.50000 AFIX 0 C9 1 0.099982 0.510234 0.449770 11.00000 0.05402 0.07013 = 0.18291 -0.07194 0.05476 -0.02374 AFIX 43 H9 2 0.097982 0.568379 0.471364 11.00000 -1.20000 AFIX 0 C01C 1 0.281319 0.727253 0.734472 11.00000 0.14121 0.06075 = 0.04810 -0.00413 0.00546 0.03381 AFIX 137 H01J 2 0.249096 0.758064 0.698700 11.00000 -1.50000 H01K 2 0.318565 0.765936 0.745995 11.00000 -1.50000 H01L 2 0.267003 0.718872 0.775024 11.00000 -1.50000 AFIX 0 C7 1 0.053067 0.356545 0.414188 11.00000 0.05144 0.07741 = 0.14805 -0.05828 0.03844 -0.03319 AFIX 43 H7 2 0.020234 0.313699 0.410318 11.00000 -1.20000 AFIX 0 C01E 1 0.427243 0.410332 0.481495 11.00000 0.17515 0.07148 = 0.03150 -0.00402 0.01297 0.00374 AFIX 137 H8BA 2 0.452875 0.449036 0.460862 11.00000 -1.50000 HG 2 0.451308 0.391150 0.527246 11.00000 -1.50000 HH 2 0.391307 0.446367 0.484560 11.00000 -1.50000 AFIX 0 PART 1 C01F 1 0.342780 0.528095 0.596769 21.00000 0.02964 0.06007 = 0.04405 -0.00409 0.01722 0.00506 AFIX 137 H01M 2 0.331000 0.535285 0.547137 21.00000 -1.50000 H01N 2 0.375557 0.481298 0.610619 21.00000 -1.50000 H01O 2 0.357612 0.588054 0.618351 21.00000 -1.50000 AFIX 0 PART 0 C8 1 0.053328 0.441431 0.447528 11.00000 0.06005 0.09451 = 0.20808 -0.07668 0.06565 -0.03358 AFIX 43 H8 2 0.022159 0.453977 0.469108 11.00000 -1.20000 AFIX 0 PART 1 N01H 5 0.183872 0.529717 0.650333 21.00000 0.06199 0.09688 = 0.06249 0.01946 0.02369 -0.02037 PART 0 C01I 1 0.534913 0.325527 0.422874 11.00000 0.10457 0.11715 = 0.08639 0.03232 -0.01085 0.03156 AFIX 137 H9BA 2 0.520520 0.306984 0.461861 11.00000 -1.50000 HI 2 0.564229 0.377258 0.436174 11.00000 -1.50000 HJ 2 0.555192 0.272326 0.408102 11.00000 -1.50000 AFIX 0 C01J 1 0.355371 0.888734 0.640922 11.00000 0.05496 0.29493 = 0.07331 0.03657 -0.00659 0.02044 AFIX 137 H01P 2 0.334026 0.830279 0.623803 11.00000 -1.50000 H01Q 2 0.366858 0.888903 0.690820 11.00000 -1.50000 H01R 2 0.392555 0.894052 0.625662 11.00000 -1.50000 AFIX 0 C01K 1 0.361509 0.266178 0.461257 11.00000 0.15403 0.16575 = 0.06027 0.05856 0.01044 -0.04839 AFIX 137 H0CA 2 0.326822 0.304592 0.465148 11.00000 -1.50000 HK 2 0.382033 0.238355 0.505625 11.00000 -1.50000 HL 2 0.346317 0.216468 0.427790 11.00000 -1.50000 AFIX 0 PART 1 C01L 1 0.446705 0.144702 0.346378 21.00000 0.11216 0.03083 = 0.07917 0.00488 0.00619 0.01283 AFIX 137 H1CA 2 0.470486 0.133414 0.313892 21.00000 -1.50000 HM 2 0.424182 0.087859 0.351239 21.00000 -1.50000 HN 2 0.474740 0.161866 0.390703 21.00000 -1.50000 AFIX 0 PART 0 C01O 1 0.242792 1.074143 0.474100 11.00000 0.18589 0.10172 = 0.18230 0.09056 0.11661 0.04037 AFIX 137 H01S 2 0.281411 1.108407 0.492540 11.00000 -1.50000 H01T 2 0.213381 1.113729 0.441383 11.00000 -1.50000 H01U 2 0.250798 1.017432 0.451153 11.00000 -1.50000 AFIX 0 C01P 1 0.340438 1.063687 0.635309 11.00000 0.17459 0.22508 = 0.10245 -0.09212 0.05535 -0.15543 AFIX 137 H01V 2 0.307133 1.109842 0.623189 11.00000 -1.50000 H01W 2 0.371250 1.078461 0.611514 11.00000 -1.50000 H01X 2 0.359785 1.065209 0.684607 11.00000 -1.50000 AFIX 0 PART 1 C01S 1 0.257621 0.415345 0.577719 21.00000 0.06089 0.03339 = 0.08632 -0.01537 0.00294 0.00470 AFIX 137 H01Y 2 0.217591 0.404316 0.585941 21.00000 -1.50000 HO 2 0.283650 0.359912 0.591121 21.00000 -1.50000 HP 2 0.251602 0.427988 0.529214 21.00000 -1.50000 AFIX 0 PART 0 C01T 1 0.175607 1.119336 0.543008 11.00000 0.26504 0.09347 = 0.20970 0.03411 0.14258 0.09430 AFIX 137 H01Z 2 0.144585 1.090392 0.561593 11.00000 -1.50000 HQ 2 0.155115 1.150841 0.500064 11.00000 -1.50000 HR 2 0.199382 1.165051 0.575637 11.00000 -1.50000 AFIX 0 PART 1 C5BA 1 0.120845 0.522782 0.596187 21.00000 0.06011 0.12594 = 0.08314 0.00295 0.00769 -0.03434 AFIX 137 H5BA 2 0.115490 0.576446 0.565323 21.00000 -1.50000 H5BB 2 0.087964 0.522603 0.618708 21.00000 -1.50000 H5BC 2 0.119031 0.464889 0.570127 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C22 1 0.191887 0.526105 0.752075 -21.00000 0.13897 0.17075 = 0.07075 0.03112 0.02362 -0.06883 AFIX 137 H22A 2 0.225971 0.481212 0.762863 -21.00000 -1.50000 H22B 2 0.153854 0.494557 0.753535 -21.00000 -1.50000 H22C 2 0.200965 0.576947 0.785506 -21.00000 -1.50000 AFIX 0 PART 0 P1 7 0.064234 0.786179 0.368554 11.00000 0.04918 0.09744 = 0.04436 -0.01733 -0.00995 0.02616 PART 1 N5A 5 0.042992 0.692969 0.314681 21.00000 0.03912 0.03700 = 0.02691 -0.01289 0.00757 -0.00156 PART 0 PART 2 N5AA 5 -0.003282 0.758187 0.395606 -21.00000 0.04736 0.09133 = 0.13564 -0.02042 -0.00328 0.00566 N3AA 5 0.058333 0.890448 0.341569 -21.00000 0.08683 0.12324 = 0.06985 0.05904 0.03448 0.06239 N5B 5 0.070785 0.759048 0.290690 -21.00000 0.07954 0.09790 = 0.06722 -0.00576 0.00881 0.00186 PART 0 PART 1 N6 5 0.006308 0.819408 0.377360 21.00000 0.05852 0.14283 = 0.07944 0.02496 0.02971 0.04777 N7 5 0.101695 0.844458 0.316244 21.00000 0.09142 0.10935 = 0.07136 0.01416 0.01778 0.00229 PART 0 PART 2 C1BA 1 0.049219 0.669790 0.275942 -21.00000 0.08382 0.11477 = 0.10326 -0.00183 -0.00122 -0.02144 AFIX 137 H1BA 2 0.083774 0.625797 0.288384 -21.00000 -1.50000 H1BB 2 0.028474 0.664607 0.227083 -21.00000 -1.50000 H1BC 2 0.019985 0.655139 0.301814 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 C2BA 1 -0.002776 0.618942 0.316233 21.00000 0.09488 0.07254 = 0.08419 0.04106 -0.05016 -0.05694 AFIX 137 H2BA 2 -0.023296 0.634171 0.351112 21.00000 -1.50000 H2BB 2 0.018315 0.558697 0.326980 21.00000 -1.50000 H2BC 2 -0.033483 0.615218 0.271629 21.00000 -1.50000 AFIX 0 C3BA 1 0.075428 0.858426 0.240494 21.00000 0.09815 0.14363 = 0.06472 0.01921 0.02553 0.01214 AFIX 137 H3BA 2 0.050257 0.915255 0.231965 21.00000 -1.50000 H3BB 2 0.049822 0.804559 0.220823 21.00000 -1.50000 H3BC 2 0.109140 0.864537 0.219485 21.00000 -1.50000 AFIX 0 C0AA 1 0.087338 0.661273 0.276459 21.00000 0.06304 0.15638 = 0.04875 -0.04796 0.00643 0.03464 AFIX 137 H0AA 2 0.129199 0.680539 0.301364 21.00000 -1.50000 H0AB 2 0.075951 0.689597 0.231012 21.00000 -1.50000 H0AC 2 0.085713 0.593065 0.272138 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C4BA 1 0.128431 0.776843 0.270770 -21.00000 0.11262 0.15110 = 0.09525 -0.00991 0.04671 0.01966 AFIX 137 H4BA 2 0.151524 0.827888 0.298448 -21.00000 -1.50000 H4BB 2 0.117791 0.794124 0.222507 -21.00000 -1.50000 H4BC 2 0.153771 0.720181 0.278296 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 C6BA 1 0.148549 0.917971 0.351057 21.00000 0.11447 0.10570 = 0.11555 0.02393 0.00889 -0.01694 AFIX 137 H6BA 2 0.127014 0.972863 0.361565 21.00000 -1.50000 H6BB 2 0.173177 0.936178 0.320707 21.00000 -1.50000 H6BC 2 0.175654 0.892254 0.393337 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C1AA 1 0.013186 0.914010 0.273551 -21.00000 0.12094 0.21111 = 0.08058 0.07447 0.02519 0.10233 AFIX 137 H1AA 2 0.024294 0.974236 0.257531 -21.00000 -1.50000 H1AB 2 -0.028495 0.917791 0.278704 -21.00000 -1.50000 H1AC 2 0.014530 0.865258 0.240382 -21.00000 -1.50000 AFIX 0 C3AA 1 -0.001733 0.740048 0.460546 -21.00000 0.08704 0.08007 = 0.17986 -0.02323 0.06825 -0.00722 AFIX 137 H3AA 2 -0.013808 0.674984 0.464414 -21.00000 -1.50000 H3AB 2 -0.030364 0.781766 0.474378 -21.00000 -1.50000 H3AC 2 0.040101 0.750176 0.490166 -21.00000 -1.50000 AFIX 0 C2AA 1 -0.066887 0.779468 0.345681 -21.00000 0.06407 0.14595 = 0.17289 -0.01431 -0.02053 0.01366 AFIX 137 H2AA 2 -0.082182 0.839083 0.357967 -21.00000 -1.50000 H2AB 2 -0.095775 0.729480 0.348124 -21.00000 -1.50000 H2AC 2 -0.063131 0.783366 0.299219 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 C4AA 1 -0.046080 0.864428 0.321808 21.00000 0.08209 0.19218 = 0.09882 0.03024 0.01912 0.07795 AFIX 137 H4AA 2 -0.069507 0.815696 0.291813 21.00000 -1.50000 H4AB 2 -0.028785 0.907915 0.295104 21.00000 -1.50000 H4AC 2 -0.073429 0.898446 0.343005 21.00000 -1.50000 AFIX 0 C7BA 1 -0.003620 0.820441 0.448421 21.00000 0.09037 0.16856 = 0.14304 -0.00028 0.02707 0.02062 AFIX 137 H7BA 2 0.018967 0.768418 0.475364 21.00000 -1.50000 H7BB 2 -0.047649 0.813949 0.444184 21.00000 -1.50000 H7BC 2 0.011477 0.879618 0.471135 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C8AA 1 0.079677 0.961982 0.384242 -21.00000 0.08749 0.07950 = 0.17681 0.09855 0.05731 0.02839 AFIX 137 H8AA 2 0.047985 0.981559 0.405556 -21.00000 -1.50000 H8AB 2 0.090007 1.014437 0.358716 -21.00000 -1.50000 H8AC 2 0.116603 0.942118 0.419572 -21.00000 -1.50000 AFIX 0 C5AA 1 0.223770 0.406143 0.611550 -21.00000 0.12764 0.03844 = 0.10299 -0.00880 -0.04418 0.00227 AFIX 137 H5AA 2 0.194941 0.402506 0.639288 -21.00000 -1.50000 H5AB 2 0.247884 0.348355 0.616786 -21.00000 -1.50000 H5AC 2 0.200699 0.414362 0.563582 -21.00000 -1.50000 AFIX 0 N12 5 0.266866 0.488666 0.634805 -21.00000 0.07945 0.04177 = 0.06422 -0.00895 -0.00525 0.01357 C9AA 1 0.314836 0.491082 0.602803 -21.00000 0.09308 0.08396 = 0.06311 -0.00607 -0.00125 0.03585 AFIX 137 H9AA 2 0.297488 0.505183 0.554286 -21.00000 -1.50000 H9AB 2 0.335479 0.430222 0.607904 -21.00000 -1.50000 H9AC 2 0.344687 0.539511 0.624103 -21.00000 -1.50000 AFIX 0 N13 5 0.184180 0.564584 0.683415 -21.00000 0.07053 0.13437 = 0.03724 0.00779 0.01672 -0.05865 C0BA 1 0.118466 0.564317 0.640004 -21.00000 0.06449 0.20333 = 0.05191 -0.01569 0.01187 -0.06694 AFIX 137 H0BA 2 0.115352 0.598520 0.597683 -21.00000 -1.50000 H0BB 2 0.092406 0.594512 0.664757 -21.00000 -1.50000 H0BC 2 0.104746 0.499747 0.629238 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 C6AA 1 0.194695 0.464695 0.711016 21.00000 0.08621 0.07496 = 0.11363 0.04346 0.05833 0.00069 AFIX 137 H6AA 2 0.202407 0.401324 0.697248 21.00000 -1.50000 H6AB 2 0.158226 0.464411 0.727826 21.00000 -1.50000 H6AC 2 0.230450 0.486304 0.747218 21.00000 -1.50000 AFIX 0 PART 0 PART 2 N2AA 5 0.380664 0.221124 0.333600 -21.00000 0.10323 0.03034 = 0.06363 -0.00612 -0.01901 0.00624 C7AA 1 0.417863 0.138783 0.369123 -21.00000 0.14408 0.04262 = 0.10846 0.00178 -0.03560 0.01062 AFIX 137 H7AB 2 0.446520 0.118975 0.343782 -21.00000 -1.50000 H7AC 2 0.390085 0.087058 0.371209 -21.00000 -1.50000 H7AD 2 0.441128 0.156876 0.415433 -21.00000 -1.50000 AFIX 0 HKLF 4 REM exp_1985_a.res in P2(1)/c REM R1 = 0.0826 for 10683 Fo > 4sig(Fo) and 0.1004 for all 13570 data REM 829 parameters refined using 606 restraints END WGHT 0.0972 11.2801 REM Highest difference peak 1.258, deepest hole -0.918, 1-sigma level 0.076 Q1 1 0.0406 0.9787 0.2947 11.00000 0.05 1.26 Q2 1 0.0390 0.4675 0.3992 11.00000 0.05 1.17 Q3 1 0.0840 0.5349 0.4045 11.00000 0.05 0.94 Q4 1 0.0589 0.8379 0.3634 11.00000 0.05 0.92 Q5 1 0.1006 0.9859 0.4210 11.00000 0.05 0.88 Q6 1 0.0794 0.9348 0.3538 11.00000 0.05 0.79 Q7 1 0.0438 0.7679 0.3740 11.00000 0.05 0.65 Q8 1 0.1030 0.4965 0.4636 11.00000 0.05 0.60 Q9 1 0.0580 0.4360 0.4635 11.00000 0.05 0.54 Q10 1 0.0420 0.8791 0.3295 11.00000 0.05 0.51 Q11 1 0.0252 0.6079 0.3020 11.00000 0.05 0.51 Q12 1 0.2022 1.0404 0.5219 11.00000 0.05 0.48 Q13 1 -0.0588 0.8052 0.3133 11.00000 0.05 0.48 Q14 1 0.1341 0.5201 0.6480 11.00000 0.05 0.48 Q15 1 0.1175 0.6146 0.6408 11.00000 0.05 0.44 Q16 1 0.0435 0.3782 0.3775 11.00000 0.05 0.44 Q17 1 0.1620 0.5806 0.6799 11.00000 0.05 0.44 Q18 1 0.0006 0.8859 0.2635 11.00000 0.05 0.44 Q19 1 0.1403 1.0636 0.5192 11.00000 0.05 0.43 Q20 1 0.3663 1.0123 0.6564 11.00000 0.05 0.43 Q21 1 0.2166 1.1267 0.5800 11.00000 0.05 0.43 Q22 1 0.4416 0.3438 0.3704 11.00000 0.05 0.42 Q23 1 0.1015 0.7054 0.2758 11.00000 0.05 0.39 Q24 1 0.3522 0.8405 0.6398 11.00000 0.05 0.38 Q25 1 -0.0006 0.7729 0.3664 11.00000 0.05 0.38 Q26 1 -0.0124 0.7548 0.4218 11.00000 0.05 0.36 Q27 1 0.2033 0.5349 0.6852 11.00000 0.05 0.36 Q28 1 0.5225 0.2731 0.3939 11.00000 0.05 0.36 Q29 1 -0.0201 0.6544 0.3265 11.00000 0.05 0.36 Q30 1 0.0787 0.7674 0.3640 11.00000 0.05 0.36 Q31 1 0.0396 0.6995 0.3377 11.00000 0.05 0.35 Q32 1 0.2151 0.5876 0.6654 11.00000 0.05 0.35 Q33 1 0.3136 1.0005 0.6155 11.00000 0.05 0.34 Q34 1 0.2411 1.0297 0.5643 11.00000 0.05 0.32 Q35 1 0.0188 0.7133 0.3966 11.00000 0.05 0.32 Q36 1 0.2819 1.0885 0.5123 11.00000 0.05 0.31 Q37 1 0.3557 0.9292 0.6437 11.00000 0.05 0.31 Q38 1 0.1371 0.7837 0.4050 11.00000 0.05 0.30 Q39 1 0.3256 0.9241 0.6319 11.00000 0.05 0.29 Q40 1 0.2959 0.9795 0.6046 11.00000 0.05 0.29 REM The information below was added by Olex2. REM REM R1 = 0.0826 for 10683 Fo > 4sig(Fo) and 0.1004 for all 70840 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.26, deepest hole -0.92 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1004 REM R1_gt = 0.0826 REM wR_ref = 0.2216 REM GOOF = 1.036 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 70840 REM Reflections_gt = 10683 REM Parameters = n/a REM Hole = -0.92 REM Peak = 1.26 REM Flack = n/a ; _cod_data_source_file c9dt02118c2.cif _cod_data_source_block 3a-HMPA _cod_database_code 1551214 _shelx_shelxl_version_number 2017/1 _chemical_oxdiff_formula 'C H B N Ca O' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.974 _shelx_estimated_absorpt_t_min 0.974 _reflns_odcompleteness_completeness 99.11 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 27.42 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups, All C(H,H,H,H,H,H) groups 2. Uiso/Uaniso restraints and constraints C11 \\sim C4 \\sim C5 \\sim C17 \\sim C16 \\sim C6 \\sim C12 \\sim C15 \\sim C1 \\sim C20 \\sim C14 \\sim C13 \\sim C18 \\sim C3 \\sim C10 \\sim C19 \\sim C2 \\sim C015 \\sim C016 \\sim C017 \\sim C018 \\sim C019 \\sim C9 \\sim C01C \\sim C7 \\sim C01E \\sim C01F \\sim C8 \\sim C01I \\sim C01J \\sim C01K \\sim C01L \\sim C01O \\sim C01P \\sim C01S \\sim C01T \\sim C5BA \\sim C22 \\sim C1BA \\sim C2BA \\sim C3BA \\sim C0AA \\sim C4BA \\sim C6BA \\sim C1AA \\sim C3AA \\sim C2AA \\sim C4AA \\sim C7BA \\sim C8AA \\sim C5AA \\sim C9AA \\sim C0BA \\sim C6AA \\sim C7AA \\sim N3 \\sim N1 \\sim N4 \\sim N2 \\sim N11 \\sim N8 \\sim N00M \\sim N00N \\sim N10 \\sim N012 \\sim N9 \\sim N014 \\sim N01H \\sim N5A \\sim N5AA \\sim N3AA \\sim N5B \\sim N6 \\sim N7 \\sim N12 \\sim N13 \\sim N2AA: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 3. Others Sof(Hd)=Sof(He)=Sof(Hf)=Sof(C22)=Sof(H22a)=Sof(H22b)=Sof(H22c)=Sof(N5AA)= Sof(N3AA)=Sof(N5B)=Sof(C1BA)=Sof(H1Ba)=Sof(H1Bb)=Sof(H1Bc)=Sof(C4BA)=Sof(H4Ba)= Sof(H4Bb)=Sof(H4Bc)=Sof(C1AA)=Sof(H1Aa)=Sof(H1Ab)=Sof(H1Ac)=Sof(C3AA)= Sof(H3Aa)=Sof(H3Ab)=Sof(H3Ac)=Sof(C2AA)=Sof(H2Aa)=Sof(H2Ab)=Sof(H2Ac)= Sof(C8AA)=Sof(H8Aa)=Sof(H8Ab)=Sof(H8Ac)=Sof(C5AA)=Sof(H5Aa)=Sof(H5Ab)= Sof(H5Ac)=Sof(N12)=Sof(C9AA)=Sof(H9Aa)=Sof(H9Ab)=Sof(H9Ac)=Sof(N13)=Sof(C0BA)= Sof(H0Ba)=Sof(H0Bb)=Sof(H0Bc)=Sof(N2AA)=Sof(C7AA)=Sof(H7Ab)=Sof(H7Ac)= Sof(H7Ad)=1-FVAR(1) Sof(N012)=Sof(N014)=Sof(H7aa)=Sof(Hb)=Sof(Hc)=Sof(C01F)=Sof(H01m)=Sof(H01n)= Sof(H01o)=Sof(N01H)=Sof(C01L)=Sof(H1ca)=Sof(Hm)=Sof(Hn)=Sof(C01S)=Sof(H01y)= Sof(Ho)=Sof(Hp)=Sof(C5BA)=Sof(H5Ba)=Sof(H5Bb)=Sof(H5Bc)=Sof(N5A)=Sof(N6)= Sof(N7)=Sof(C2BA)=Sof(H2Ba)=Sof(H2Bb)=Sof(H2Bc)=Sof(C3BA)=Sof(H3Ba)=Sof(H3Bb)= Sof(H3Bc)=Sof(C0AA)=Sof(H0Aa)=Sof(H0Ab)=Sof(H0Ac)=Sof(C6BA)=Sof(H6Ba)= Sof(H6Bb)=Sof(H6Bc)=Sof(C4AA)=Sof(H4Aa)=Sof(H4Ab)=Sof(H4Ac)=Sof(C7BA)= Sof(H7Ba)=Sof(H7Bb)=Sof(H7Bc)=Sof(C6AA)=Sof(H6Aa)=Sof(H6Ab)=Sof(H6Ac)=FVAR(1) 4.a Aromatic/amide H refined with riding coordinates: N1(H1), N4(H4), C12(H12), C1(H1a), C20(H20), C14(H14), C13(H13), C18(H18), C3(H3), C19(H19), C2(H2), C9(H9), C7(H7), C8(H8) 4.b Idealised Me refined as rotating group: C015(H01a,H01b,H01c), C016(H01,H,Ha), C017(H01d,H01e,H01f), C018(H7aa,Hb,Hc), C018(Hd,He,Hf), C019(H01g,H01h,H01i), C01C(H01j,H01k,H01l), C01E(H8ba,Hg,Hh), C01F(H01m,H01n,H01o), C01I(H9ba,Hi,Hj), C01J(H01p,H01q,H01r), C01K(H0ca,Hk,Hl), C01L(H1ca,Hm,Hn), C01O(H01s,H01t,H01u), C01P(H01v,H01w,H01x), C01S(H01y,Ho, Hp), C01T(H01z,Hq,Hr), C5BA(H5Ba,H5Bb,H5Bc), C22(H22a,H22b,H22c), C1BA(H1Ba, H1Bb,H1Bc), C2BA(H2Ba,H2Bb,H2Bc), C3BA(H3Ba,H3Bb,H3Bc), C0AA(H0Aa,H0Ab,H0Ac), C4BA(H4Ba,H4Bb,H4Bc), C6BA(H6Ba,H6Bb,H6Bc), C1AA(H1Aa,H1Ab,H1Ac), C3AA(H3Aa, H3Ab,H3Ac), C2AA(H2Aa,H2Ab,H2Ac), C4AA(H4Aa,H4Ab,H4Ac), C7BA(H7Ba,H7Bb,H7Bc), C8AA(H8Aa,H8Ab,H8Ac), C5AA(H5Aa,H5Ab,H5Ac), C9AA(H9Aa,H9Ab,H9Ac), C0BA(H0Ba, H0Bb,H0Bc), C6AA(H6Aa,H6Ab,H6Ac), C7AA(H7Ab,H7Ac,H7Ad) ; _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 2.022 _oxdiff_exptl_absorpt_empirical_full_min 0.626 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_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.21749(3) 0.71468(4) 0.47986(3) 0.03197(16) Uani 1 1 d . . . . . P002 P 0.24104(4) 0.95057(6) 0.57463(4) 0.0376(2) Uani 1 1 d . . . . . P003 P 0.24274(4) 0.58700(6) 0.64499(5) 0.0474(2) Uani 1 1 d . . . . . P004 P 0.40663(6) 0.32925(6) 0.35708(5) 0.0512(3) Uani 1 1 d . . . . . O2 O 0.23280(11) 0.86673(15) 0.52885(12) 0.0413(5) Uani 1 1 d . . . . . O3 O 0.21946(11) 0.65577(16) 0.58743(12) 0.0435(5) Uani 1 1 d . . . . . O4 O 0.36331(12) 0.39681(16) 0.31012(12) 0.0453(6) Uani 1 1 d . . . . . O1 O 0.11651(11) 0.76933(18) 0.43042(13) 0.0489(6) Uani 1 1 d . . . . . N3 N 0.30556(12) 0.71095(17) 0.43216(13) 0.0345(5) Uani 1 1 d . U . . . N1 N 0.24649(13) 0.44704(17) 0.36449(13) 0.0362(6) Uani 1 1 d . U . . . H1 H 0.277071 0.433491 0.347632 0.043 Uiso 1 1 calc R . . . . N4 N 0.35384(12) 0.59783(18) 0.36788(13) 0.0355(5) Uani 1 1 d . U . . . H4 H 0.352466 0.543697 0.347340 0.043 Uiso 1 1 calc R . . . . N2 N 0.19544(13) 0.5613(2) 0.42412(17) 0.0465(7) Uani 1 1 d . U . . . N11 N 0.29554(15) 0.6338(2) 0.70953(15) 0.0467(7) Uani 1 1 d . U . . . C11 C 0.40311(15) 0.6586(2) 0.36943(15) 0.0360(6) Uani 1 1 d . U . . . C4 C 0.20059(16) 0.3795(2) 0.36041(15) 0.0356(6) Uani 1 1 d . U . . . C5 C 0.15070(15) 0.4022(2) 0.38882(16) 0.0370(7) Uani 1 1 d . U . . . N8 N 0.20101(16) 0.9373(3) 0.63088(16) 0.0544(8) Uani 1 1 d . U . . . C17 C 0.35459(15) 0.7728(2) 0.43322(16) 0.0359(6) Uani 1 1 d . U . . . C16 C 0.40412(14) 0.7484(2) 0.40303(15) 0.0347(6) Uani 1 1 d . U . . . C6 C 0.10213(17) 0.3338(3) 0.38580(19) 0.0477(8) Uani 1 1 d . U . . . N00M N 0.48030(19) 0.3566(3) 0.36467(18) 0.0656(10) Uani 1 1 d . U . . . N00N N 0.4063(2) 0.3259(3) 0.43867(17) 0.0741(11) Uani 1 1 d . U . . . C12 C 0.45012(17) 0.6348(3) 0.33886(18) 0.0474(8) Uani 1 1 d . U . . . H12 H 0.449472 0.575954 0.317270 0.057 Uiso 1 1 calc R . . . . C15 C 0.45464(16) 0.8134(3) 0.40571(17) 0.0424(7) Uani 1 1 d . U . . . C1 C 0.10608(19) 0.2435(2) 0.35561(19) 0.0495(8) Uani 1 1 d . U . . . H1A H 0.075736 0.197335 0.354670 0.059 Uiso 1 1 calc R . . . . C20 C 0.45525(18) 0.9024(3) 0.4389(2) 0.0510(9) Uani 1 1 d . U . . . H20 H 0.487844 0.945309 0.441524 0.061 Uiso 1 1 calc R . . . . C14 C 0.50127(18) 0.7860(3) 0.3731(2) 0.0527(9) Uani 1 1 d . U . . . H14 H 0.534198 0.827475 0.373968 0.063 Uiso 1 1 calc R . . . . C13 C 0.49849(19) 0.7000(3) 0.3408(2) 0.0555(9) Uani 1 1 d . U . . . H13 H 0.529361 0.684257 0.319489 0.067 Uiso 1 1 calc R . . . . C18 C 0.35793(18) 0.8627(3) 0.4643(2) 0.0508(8) Uani 1 1 d . U . . . H18 H 0.326297 0.881457 0.483634 0.061 Uiso 1 1 calc R . . . . C3 C 0.2012(2) 0.2905(2) 0.3296(2) 0.0581(10) Uani 1 1 d . U . . . H3 H 0.233159 0.275230 0.309822 0.070 Uiso 1 1 calc R . . . . B1 B 0.24572(16) 0.5401(2) 0.39593(16) 0.0318(7) Uani 1 1 d . . . . . B2 B 0.30449(16) 0.6208(2) 0.39909(16) 0.0315(7) Uani 1 1 d . . . . . C10 C 0.14926(16) 0.4939(3) 0.4205(2) 0.0551(10) Uani 1 1 d . U . . . N10 N 0.31457(19) 0.9678(4) 0.61476(19) 0.0866(15) Uani 1 1 d . U . . . C19 C 0.4079(2) 0.9252(3) 0.4669(2) 0.0574(10) Uani 1 1 d . U . . . H19 H 0.408701 0.984114 0.488483 0.069 Uiso 1 1 calc R . . . . C2 C 0.1538(2) 0.2243(3) 0.3282(2) 0.0650(11) Uani 1 1 d . U . . . H2 H 0.155146 0.165091 0.307774 0.078 Uiso 1 1 calc R . . . . N012 N 0.2880(4) 0.4970(7) 0.6185(5) 0.0403(19) Uani 0.454(4) 1 d . U P A 1 N9 N 0.2166(3) 1.0480(3) 0.5308(3) 0.0985(17) Uani 1 1 d . U . . . N014 N 0.4023(7) 0.2219(13) 0.3211(9) 0.066(3) Uani 0.454(4) 1 d . U P A 1 C015 C 0.3457(2) 0.5839(3) 0.7605(2) 0.0660(12) Uani 1 1 d . U . . . H01A H 0.334248 0.576576 0.802976 0.099 Uiso 1 1 calc GR . . . . H01B H 0.383852 0.620098 0.769308 0.099 Uiso 1 1 calc GR . . . . H01C H 0.351853 0.522182 0.742771 0.099 Uiso 1 1 calc GR . . . . C016 C 0.4980(2) 0.3870(4) 0.3031(2) 0.0737(13) Uani 1 1 d . U . . . H01 H 0.519461 0.335952 0.287513 0.111 Uiso 1 1 calc GR . . . . H H 0.525177 0.441490 0.314402 0.111 Uiso 1 1 calc GR . . . . HA H 0.460824 0.403627 0.266832 0.111 Uiso 1 1 calc GR . . . . C017 C 0.2178(2) 0.9793(4) 0.7004(2) 0.0664(12) Uani 1 1 d . U . . . H01D H 0.260142 1.002994 0.711736 0.100 Uiso 1 1 calc GR . . . . H01E H 0.214764 0.931623 0.733679 0.100 Uiso 1 1 calc GR . . . . H01F H 0.189632 1.030839 0.701545 0.100 Uiso 1 1 calc GR . . . . C018 C 0.3455(3) 0.1999(3) 0.2628(3) 0.0760(14) Uani 1 1 d . U . . . H7AA H 0.317194 0.161290 0.279720 0.114 Uiso 0.454(4) 1 calc GR . P A 1 HB H 0.357703 0.165926 0.227148 0.114 Uiso 0.454(4) 1 calc GR . P A 1 HC H 0.324953 0.258248 0.244086 0.114 Uiso 0.454(4) 1 calc GR . P A 1 HD H 0.318513 0.252665 0.243870 0.114 Uiso 0.546(4) 1 calc GR . P A 2 HE H 0.320522 0.143763 0.262091 0.114 Uiso 0.546(4) 1 calc GR . P A 2 HF H 0.374094 0.189118 0.235505 0.114 Uiso 0.546(4) 1 calc GR . P A 2 C019 C 0.1397(2) 0.8899(5) 0.6104(3) 0.0835(16) Uani 1 1 d . U . . . H01G H 0.107117 0.936153 0.607041 0.125 Uiso 1 1 calc GR . . . . H01H H 0.138022 0.842778 0.644554 0.125 Uiso 1 1 calc GR . . . . H01I H 0.133886 0.859504 0.566075 0.125 Uiso 1 1 calc GR . . . . C9 C 0.1000(2) 0.5102(4) 0.4498(4) 0.0980(18) Uani 1 1 d . U . . . H9 H 0.097982 0.568379 0.471364 0.118 Uiso 1 1 calc R . . . . C01C C 0.2813(3) 0.7273(3) 0.7345(2) 0.0877(18) Uani 1 1 d . U . . . H01J H 0.249096 0.758064 0.698700 0.132 Uiso 1 1 calc GR . . . . H01K H 0.318565 0.765936 0.745995 0.132 Uiso 1 1 calc GR . . . . H01L H 0.267003 0.718872 0.775024 0.132 Uiso 1 1 calc GR . . . . C7 C 0.0531(2) 0.3565(4) 0.4142(3) 0.0902(16) Uani 1 1 d . U . . . H7 H 0.020234 0.313699 0.410318 0.108 Uiso 1 1 calc R . . . . C01E C 0.4272(4) 0.4103(4) 0.4815(2) 0.096(2) Uani 1 1 d . U . . . H8BA H 0.452875 0.449036 0.460862 0.144 Uiso 1 1 calc GR . . . . HG H 0.451308 0.391150 0.527246 0.144 Uiso 1 1 calc GR . . . . HH H 0.391307 0.446367 0.484560 0.144 Uiso 1 1 calc GR . . . . C01F C 0.3428(4) 0.5281(7) 0.5968(5) 0.0432(19) Uani 0.454(4) 1 d . U P A 1 H01M H 0.331000 0.535285 0.547137 0.065 Uiso 0.454(4) 1 calc GR . P A 1 H01N H 0.375557 0.481298 0.610619 0.065 Uiso 0.454(4) 1 calc GR . P A 1 H01O H 0.357612 0.588054 0.618351 0.065 Uiso 0.454(4) 1 calc GR . P A 1 C8 C 0.0533(2) 0.4414(4) 0.4475(4) 0.115(2) Uani 1 1 d . U . . . H8 H 0.022159 0.453977 0.469108 0.138 Uiso 1 1 calc R . . . . N01H N 0.1839(5) 0.5297(8) 0.6503(6) 0.073(2) Uani 0.454(4) 1 d . U P A 1 C01I C 0.5349(3) 0.3255(5) 0.4229(3) 0.110(2) Uani 1 1 d . U . . . H9BA H 0.520520 0.306984 0.461861 0.166 Uiso 1 1 calc GR . . . . HI H 0.564229 0.377258 0.436174 0.166 Uiso 1 1 calc GR . . . . HJ H 0.555192 0.272326 0.408102 0.166 Uiso 1 1 calc GR . . . . C01J C 0.3554(3) 0.8887(8) 0.6409(3) 0.146(3) Uani 1 1 d . U . . . H01P H 0.334026 0.830279 0.623803 0.219 Uiso 1 1 calc GR . . . . H01Q H 0.366858 0.888903 0.690820 0.219 Uiso 1 1 calc GR . . . . H01R H 0.392555 0.894052 0.625662 0.219 Uiso 1 1 calc GR . . . . C01K C 0.3615(4) 0.2662(6) 0.4613(3) 0.131(3) Uani 1 1 d . U . . . H0CA H 0.326822 0.304592 0.465148 0.196 Uiso 1 1 calc GR . . . . HK H 0.382033 0.238355 0.505625 0.196 Uiso 1 1 calc GR . . . . HL H 0.346317 0.216468 0.427790 0.196 Uiso 1 1 calc GR . . . . C01L C 0.4467(8) 0.1447(10) 0.3464(8) 0.078(4) Uani 0.454(4) 1 d . U P A 1 H1CA H 0.470486 0.133414 0.313892 0.118 Uiso 0.454(4) 1 calc GR . P A 1 HM H 0.424182 0.087859 0.351239 0.118 Uiso 0.454(4) 1 calc GR . P A 1 HN H 0.474740 0.161866 0.390703 0.118 Uiso 0.454(4) 1 calc GR . P A 1 C01O C 0.2428(4) 1.0741(5) 0.4741(5) 0.143(3) Uani 1 1 d . U . . . H01S H 0.281411 1.108407 0.492540 0.215 Uiso 1 1 calc GR . . . . H01T H 0.213381 1.113729 0.441383 0.215 Uiso 1 1 calc GR . . . . H01U H 0.250798 1.017432 0.451153 0.215 Uiso 1 1 calc GR . . . . C01P C 0.3404(4) 1.0637(7) 0.6353(4) 0.164(4) Uani 1 1 d . U . . . H01V H 0.307133 1.109842 0.623189 0.246 Uiso 1 1 calc GR . . . . H01W H 0.371250 1.078461 0.611514 0.246 Uiso 1 1 calc GR . . . . H01X H 0.359785 1.065209 0.684607 0.246 Uiso 1 1 calc GR . . . . C01S C 0.2576(5) 0.4153(7) 0.5777(6) 0.064(3) Uani 0.454(4) 1 d . U P A 1 H01Y H 0.217591 0.404316 0.585941 0.096 Uiso 0.454(4) 1 calc GR . P A 1 HO H 0.283650 0.359912 0.591121 0.096 Uiso 0.454(4) 1 calc GR . P A 1 HP H 0.251602 0.427988 0.529214 0.096 Uiso 0.454(4) 1 calc GR . P A 1 C01T C 0.1756(5) 1.1193(6) 0.5430(6) 0.174(4) Uani 1 1 d . U . . . H01Z H 0.144585 1.090392 0.561593 0.261 Uiso 1 1 calc GR . . . . HQ H 0.155115 1.150841 0.500064 0.261 Uiso 1 1 calc GR . . . . HR H 0.199382 1.165051 0.575637 0.261 Uiso 1 1 calc GR . . . . C5BA C 0.1208(5) 0.5228(12) 0.5962(8) 0.092(3) Uani 0.454(4) 1 d . U P A 1 H5BA H 0.115490 0.576446 0.565323 0.138 Uiso 0.454(4) 1 calc GR . P A 1 H5BB H 0.087964 0.522603 0.618708 0.138 Uiso 0.454(4) 1 calc GR . P A 1 H5BC H 0.119031 0.464889 0.570127 0.138 Uiso 0.454(4) 1 calc GR . P A 1 C22 C 0.1919(8) 0.5261(13) 0.7521(6) 0.128(4) Uani 0.546(4) 1 d . U P A 2 H22A H 0.225971 0.481212 0.762863 0.192 Uiso 0.546(4) 1 calc GR . P A 2 H22B H 0.153854 0.494557 0.753535 0.192 Uiso 0.546(4) 1 calc GR . P A 2 H22C H 0.200965 0.576947 0.785506 0.192 Uiso 0.546(4) 1 calc GR . P A 2 P1 P 0.06423(5) 0.78618(10) 0.36855(6) 0.0684(4) Uani 1 1 d . . . . . N5A N 0.0430(3) 0.6930(4) 0.3147(3) 0.0347(13) Uani 0.454(4) 1 d . U P A 1 N5AA N -0.0033(4) 0.7582(8) 0.3956(7) 0.097(3) Uani 0.546(4) 1 d . U P A 2 N3AA N 0.0583(4) 0.8904(8) 0.3416(4) 0.091(2) Uani 0.546(4) 1 d . U P A 2 N5B N 0.0708(4) 0.7590(7) 0.2907(4) 0.084(2) Uani 0.546(4) 1 d . U P A 2 N6 N 0.0063(5) 0.8194(11) 0.3774(6) 0.092(3) Uani 0.454(4) 1 d . U P A 1 N7 N 0.1017(5) 0.8445(9) 0.3162(5) 0.092(2) Uani 0.454(4) 1 d . U P A 1 C1BA C 0.0492(7) 0.6698(11) 0.2759(8) 0.106(4) Uani 0.546(4) 1 d . U P A 2 H1BA H 0.083774 0.625797 0.288384 0.159 Uiso 0.546(4) 1 calc GR . P A 2 H1BB H 0.028474 0.664607 0.227083 0.159 Uiso 0.546(4) 1 calc GR . P A 2 H1BC H 0.019985 0.655139 0.301814 0.159 Uiso 0.546(4) 1 calc GR . P A 2 C2BA C -0.0028(6) 0.6189(8) 0.3162(6) 0.099(4) Uani 0.454(4) 1 d . U P A 1 H2BA H -0.023296 0.634171 0.351112 0.149 Uiso 0.454(4) 1 calc GR . P A 1 H2BB H 0.018315 0.558697 0.326980 0.149 Uiso 0.454(4) 1 calc GR . P A 1 H2BC H -0.033483 0.615218 0.271629 0.149 Uiso 0.454(4) 1 calc GR . P A 1 C3BA C 0.0754(7) 0.8584(12) 0.2405(6) 0.102(3) Uani 0.454(4) 1 d . U P A 1 H3BA H 0.050257 0.915255 0.231965 0.152 Uiso 0.454(4) 1 calc GR . P A 1 H3BB H 0.049822 0.804559 0.220823 0.152 Uiso 0.454(4) 1 calc GR . P A 1 H3BC H 0.109140 0.864537 0.219485 0.152 Uiso 0.454(4) 1 calc GR . P A 1 C0AA C 0.0873(6) 0.6613(12) 0.2765(6) 0.091(3) Uani 0.454(4) 1 d . U P A 1 H0AA H 0.129199 0.680539 0.301364 0.137 Uiso 0.454(4) 1 calc GR . P A 1 H0AB H 0.075951 0.689597 0.231012 0.137 Uiso 0.454(4) 1 calc GR . P A 1 H0AC H 0.085713 0.593065 0.272138 0.137 Uiso 0.454(4) 1 calc GR . P A 1 C4BA C 0.1284(6) 0.7768(11) 0.2708(7) 0.116(3) Uani 0.546(4) 1 d . U P A 2 H4BA H 0.151524 0.827888 0.298448 0.174 Uiso 0.546(4) 1 calc GR . P A 2 H4BB H 0.117791 0.794124 0.222507 0.174 Uiso 0.546(4) 1 calc GR . P A 2 H4BC H 0.153771 0.720181 0.278296 0.174 Uiso 0.546(4) 1 calc GR . P A 2 C6BA C 0.1485(8) 0.9180(12) 0.3511(9) 0.117(4) Uani 0.454(4) 1 d . U P A 1 H6BA H 0.127014 0.972863 0.361565 0.175 Uiso 0.454(4) 1 calc GR . P A 1 H6BB H 0.173177 0.936178 0.320707 0.175 Uiso 0.454(4) 1 calc GR . P A 1 H6BC H 0.175654 0.892254 0.393337 0.175 Uiso 0.454(4) 1 calc GR . P A 1 C1AA C 0.0132(6) 0.9140(12) 0.2736(6) 0.138(4) Uani 0.546(4) 1 d . U P A 2 H1AA H 0.024294 0.974236 0.257531 0.207 Uiso 0.546(4) 1 calc GR . P A 2 H1AB H -0.028495 0.917791 0.278704 0.207 Uiso 0.546(4) 1 calc GR . P A 2 H1AC H 0.014530 0.865258 0.240382 0.207 Uiso 0.546(4) 1 calc GR . P A 2 C3AA C -0.0017(6) 0.7400(9) 0.4605(9) 0.109(4) Uani 0.546(4) 1 d . U P A 2 H3AA H -0.013808 0.674984 0.464414 0.164 Uiso 0.546(4) 1 calc GR . P A 2 H3AB H -0.030364 0.781766 0.474378 0.164 Uiso 0.546(4) 1 calc GR . P A 2 H3AC H 0.040101 0.750176 0.490166 0.164 Uiso 0.546(4) 1 calc GR . P A 2 C2AA C -0.0669(6) 0.7795(13) 0.3457(9) 0.139(5) Uani 0.546(4) 1 d . U P A 2 H2AA H -0.082182 0.839083 0.357967 0.208 Uiso 0.546(4) 1 calc GR . P A 2 H2AB H -0.095775 0.729480 0.348124 0.208 Uiso 0.546(4) 1 calc GR . P A 2 H2AC H -0.063131 0.783366 0.299219 0.208 Uiso 0.546(4) 1 calc GR . P A 2 C4AA C -0.0461(7) 0.8644(16) 0.3218(8) 0.126(4) Uani 0.454(4) 1 d . U P A 1 H4AA H -0.069507 0.815696 0.291813 0.189 Uiso 0.454(4) 1 calc GR . P A 1 H4AB H -0.028785 0.907915 0.295104 0.189 Uiso 0.454(4) 1 calc GR . P A 1 H4AC H -0.073429 0.898446 0.343005 0.189 Uiso 0.454(4) 1 calc GR . P A 1 C7BA C -0.0036(8) 0.8204(18) 0.4484(11) 0.135(5) Uani 0.454(4) 1 d . U P A 1 H7BA H 0.018967 0.768418 0.475364 0.203 Uiso 0.454(4) 1 calc GR . P A 1 H7BB H -0.047649 0.813949 0.444184 0.203 Uiso 0.454(4) 1 calc GR . P A 1 H7BC H 0.011477 0.879618 0.471135 0.203 Uiso 0.454(4) 1 calc GR . P A 1 C8AA C 0.0797(5) 0.9620(8) 0.3842(8) 0.111(4) Uani 0.546(4) 1 d . U P A 2 H8AA H 0.047985 0.981559 0.405556 0.166 Uiso 0.546(4) 1 calc GR . P A 2 H8AB H 0.090007 1.014437 0.358716 0.166 Uiso 0.546(4) 1 calc GR . P A 2 H8AC H 0.116603 0.942118 0.419572 0.166 Uiso 0.546(4) 1 calc GR . P A 2 C5AA C 0.2238(6) 0.4061(7) 0.6115(7) 0.105(4) Uani 0.546(4) 1 d . U P A 2 H5AA H 0.194941 0.402506 0.639288 0.158 Uiso 0.546(4) 1 calc GR . P A 2 H5AB H 0.247884 0.348355 0.616786 0.158 Uiso 0.546(4) 1 calc GR . P A 2 H5AC H 0.200699 0.414362 0.563582 0.158 Uiso 0.546(4) 1 calc GR . P A 2 N12 N 0.2669(5) 0.4887(7) 0.6348(5) 0.067(2) Uani 0.546(4) 1 d . U P A 2 C9AA C 0.3148(7) 0.4911(10) 0.6028(6) 0.085(3) Uani 0.546(4) 1 d . U P A 2 H9AA H 0.297488 0.505183 0.554286 0.127 Uiso 0.546(4) 1 calc GR . P A 2 H9AB H 0.335479 0.430222 0.607904 0.127 Uiso 0.546(4) 1 calc GR . P A 2 H9AC H 0.344687 0.539511 0.624103 0.127 Uiso 0.546(4) 1 calc GR . P A 2 N13 N 0.1842(4) 0.5646(8) 0.6834(4) 0.080(2) Uani 0.546(4) 1 d . U P A 2 C0BA C 0.1185(5) 0.5643(11) 0.6400(5) 0.108(3) Uani 0.546(4) 1 d . U P A 2 H0BA H 0.115352 0.598520 0.597683 0.161 Uiso 0.546(4) 1 calc GR . P A 2 H0BB H 0.092406 0.594512 0.664757 0.161 Uiso 0.546(4) 1 calc GR . P A 2 H0BC H 0.104746 0.499747 0.629238 0.161 Uiso 0.546(4) 1 calc GR . P A 2 C6AA C 0.1947(6) 0.4647(9) 0.7110(8) 0.085(3) Uani 0.454(4) 1 d . U P A 1 H6AA H 0.202407 0.401324 0.697248 0.128 Uiso 0.454(4) 1 calc GR . P A 1 H6AB H 0.158226 0.464411 0.727826 0.128 Uiso 0.454(4) 1 calc GR . P A 1 H6AC H 0.230450 0.486304 0.747218 0.128 Uiso 0.454(4) 1 calc GR . P A 1 N2AA N 0.3807(6) 0.2211(10) 0.3336(7) 0.074(3) Uani 0.546(4) 1 d . U P A 2 C7AA C 0.4179(8) 0.1388(10) 0.3691(8) 0.113(5) Uani 0.546(4) 1 d . U P A 2 H7AB H 0.446520 0.118975 0.343782 0.170 Uiso 0.546(4) 1 calc GR . P A 2 H7AC H 0.390085 0.087058 0.371209 0.170 Uiso 0.546(4) 1 calc GR . P A 2 H7AD H 0.441128 0.156876 0.415433 0.170 Uiso 0.546(4) 1 calc GR . P A 2 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 Ca1 0.0307(3) 0.0259(3) 0.0355(3) -0.0077(2) 0.0033(2) -0.0005(2) P002 0.0513(5) 0.0308(4) 0.0319(4) -0.0094(3) 0.0137(3) -0.0086(3) P003 0.0416(5) 0.0312(4) 0.0604(6) 0.0127(4) 0.0002(4) -0.0072(3) P004 0.0848(7) 0.0289(4) 0.0309(4) 0.0010(3) 0.0015(4) 0.0051(4) O2 0.0535(13) 0.0296(11) 0.0427(12) -0.0098(9) 0.0166(10) -0.0054(9) O3 0.0480(13) 0.0340(11) 0.0430(12) 0.0026(10) 0.0039(10) 0.0010(10) O4 0.0659(15) 0.0350(12) 0.0344(11) 0.0000(9) 0.0130(11) 0.0097(11) O1 0.0423(13) 0.0520(14) 0.0439(13) -0.0061(11) -0.0017(10) 0.0086(11) N3 0.0381(13) 0.0292(12) 0.0346(13) -0.0044(10) 0.0079(10) -0.0043(10) N1 0.0511(15) 0.0272(12) 0.0334(13) -0.0022(10) 0.0169(11) -0.0012(11) N4 0.0451(14) 0.0272(12) 0.0338(13) -0.0014(10) 0.0105(11) 0.0003(10) N2 0.0357(13) 0.0342(14) 0.0657(19) -0.0233(13) 0.0078(13) -0.0042(11) N11 0.0631(18) 0.0374(14) 0.0369(14) 0.0026(12) 0.0099(13) 0.0045(13) C11 0.0409(15) 0.0374(15) 0.0269(13) 0.0070(12) 0.0049(12) 0.0044(12) C4 0.0543(17) 0.0233(13) 0.0277(13) 0.0004(11) 0.0091(12) -0.0008(12) C5 0.0378(15) 0.0309(14) 0.0350(15) -0.0078(12) -0.0017(12) -0.0024(12) N8 0.0573(18) 0.071(2) 0.0389(15) -0.0167(15) 0.0204(14) -0.0145(16) C17 0.0405(15) 0.0326(14) 0.0320(14) -0.0025(12) 0.0063(12) -0.0053(12) C16 0.0377(15) 0.0358(15) 0.0271(13) 0.0051(11) 0.0034(11) -0.0011(12) C6 0.0440(17) 0.0401(17) 0.0513(19) -0.0149(15) 0.0009(15) -0.0107(14) N00M 0.080(2) 0.063(2) 0.0454(18) 0.0102(16) 0.0040(17) 0.0206(19) N00N 0.120(3) 0.062(2) 0.0338(16) 0.0095(15) 0.0113(18) -0.014(2) C12 0.0529(19) 0.0496(19) 0.0423(17) 0.0049(15) 0.0177(15) 0.0064(16) C15 0.0399(16) 0.0485(18) 0.0351(15) 0.0074(14) 0.0045(13) -0.0067(14) C1 0.065(2) 0.0316(16) 0.0494(19) -0.0056(14) 0.0112(17) -0.0135(15) C20 0.0517(19) 0.0483(19) 0.0500(19) -0.0014(16) 0.0095(16) -0.0200(16) C14 0.0463(19) 0.062(2) 0.050(2) 0.0133(17) 0.0144(16) -0.0069(17) C13 0.053(2) 0.067(2) 0.053(2) 0.0111(18) 0.0248(17) 0.0053(18) C18 0.056(2) 0.0417(18) 0.059(2) -0.0171(16) 0.0239(17) -0.0141(15) C3 0.087(3) 0.0313(16) 0.070(2) -0.0143(16) 0.044(2) -0.0068(17) B1 0.0392(17) 0.0250(15) 0.0257(14) -0.0024(12) 0.0002(13) 0.0017(13) B2 0.0365(16) 0.0285(15) 0.0259(15) 0.0018(12) 0.0026(12) 0.0004(13) C10 0.0347(16) 0.0438(18) 0.084(3) -0.0330(18) 0.0129(16) -0.0080(14) N10 0.061(2) 0.154(4) 0.0476(19) -0.043(2) 0.0204(17) -0.055(3) C19 0.064(2) 0.0448(19) 0.065(2) -0.0189(17) 0.0201(19) -0.0201(17) C2 0.096(3) 0.0285(16) 0.077(3) -0.0158(17) 0.035(2) -0.0134(18) N012 0.029(4) 0.039(3) 0.058(5) -0.004(3) 0.021(3) 0.003(3) N9 0.156(4) 0.0399(19) 0.136(4) 0.028(2) 0.101(4) 0.030(2) N014 0.096(7) 0.031(3) 0.059(5) -0.006(4) 0.002(5) 0.012(5) C015 0.075(3) 0.063(3) 0.046(2) -0.0016(19) -0.005(2) 0.014(2) C016 0.082(3) 0.081(3) 0.059(3) -0.004(2) 0.021(2) 0.024(3) C017 0.082(3) 0.080(3) 0.042(2) -0.019(2) 0.026(2) -0.005(2) C018 0.095(3) 0.050(2) 0.068(3) -0.024(2) -0.002(2) 0.003(2) C019 0.063(3) 0.128(5) 0.067(3) -0.026(3) 0.030(2) -0.031(3) C9 0.054(2) 0.070(3) 0.183(5) -0.072(3) 0.055(3) -0.024(2) C01C 0.141(5) 0.061(3) 0.048(2) -0.004(2) 0.005(3) 0.034(3) C7 0.051(2) 0.077(3) 0.148(4) -0.058(3) 0.038(3) -0.033(2) C01E 0.175(6) 0.071(3) 0.031(2) -0.004(2) 0.013(3) 0.004(4) C01F 0.030(4) 0.060(5) 0.044(4) -0.004(4) 0.017(3) 0.005(3) C8 0.060(3) 0.095(3) 0.208(5) -0.077(4) 0.066(3) -0.034(2) N01H 0.062(4) 0.097(6) 0.062(5) 0.019(4) 0.024(4) -0.020(4) C01I 0.105(4) 0.117(5) 0.086(4) 0.032(4) -0.011(3) 0.032(4) C01J 0.055(3) 0.295(11) 0.073(4) 0.037(5) -0.007(3) 0.020(5) C01K 0.154(6) 0.166(7) 0.060(3) 0.059(4) 0.010(4) -0.048(5) C01L 0.112(9) 0.031(4) 0.079(7) 0.005(5) 0.006(6) 0.013(6) C01O 0.186(7) 0.102(5) 0.182(7) 0.091(5) 0.117(6) 0.040(5) C01P 0.175(7) 0.225(8) 0.102(5) -0.092(5) 0.055(5) -0.155(7) C01S 0.061(5) 0.033(4) 0.086(6) -0.015(4) 0.003(5) 0.005(4) C01T 0.265(10) 0.093(5) 0.210(9) 0.034(5) 0.143(8) 0.094(6) C5BA 0.060(5) 0.126(9) 0.083(7) 0.003(7) 0.008(5) -0.034(6) C22 0.139(8) 0.171(10) 0.071(6) 0.031(7) 0.024(6) -0.069(8) P1 0.0492(6) 0.0974(9) 0.0444(5) -0.0173(6) -0.0100(4) 0.0262(6) N5A 0.039(3) 0.037(3) 0.027(3) -0.013(2) 0.008(2) -0.002(2) N5AA 0.047(4) 0.091(6) 0.136(7) -0.020(6) -0.003(5) 0.006(4) N3AA 0.087(4) 0.123(5) 0.070(4) 0.059(4) 0.034(3) 0.062(4) N5B 0.080(4) 0.098(5) 0.067(4) -0.006(4) 0.009(3) 0.002(4) N6 0.059(4) 0.143(6) 0.079(5) 0.025(5) 0.030(4) 0.048(5) N7 0.091(5) 0.109(5) 0.071(4) 0.014(4) 0.018(4) 0.002(5) C1BA 0.084(6) 0.115(7) 0.103(7) -0.002(7) -0.001(7) -0.021(6) C2BA 0.095(7) 0.073(6) 0.084(6) 0.041(5) -0.050(6) -0.057(5) C3BA 0.098(7) 0.144(8) 0.065(6) 0.019(6) 0.026(5) 0.012(7) C0AA 0.063(5) 0.156(8) 0.049(5) -0.048(5) 0.006(5) 0.035(6) C4BA 0.113(7) 0.151(8) 0.095(6) -0.010(6) 0.047(6) 0.020(7) C6BA 0.114(8) 0.106(8) 0.116(9) 0.024(7) 0.009(7) -0.017(7) C1AA 0.121(7) 0.211(10) 0.081(6) 0.074(7) 0.025(6) 0.102(7) C3AA 0.087(7) 0.080(7) 0.180(11) -0.023(8) 0.068(7) -0.007(6) C2AA 0.064(6) 0.146(10) 0.173(10) -0.014(9) -0.021(7) 0.014(7) C4AA 0.082(7) 0.192(11) 0.099(8) 0.030(8) 0.019(6) 0.078(8) C7BA 0.090(8) 0.169(11) 0.143(10) 0.000(10) 0.027(8) 0.021(9) C8AA 0.087(6) 0.080(6) 0.177(10) 0.099(7) 0.057(7) 0.028(5) C5AA 0.128(8) 0.038(4) 0.103(7) -0.009(5) -0.044(6) 0.002(5) N12 0.079(6) 0.042(3) 0.064(5) -0.009(3) -0.005(4) 0.014(4) C9AA 0.093(9) 0.084(6) 0.063(6) -0.006(5) -0.001(6) 0.036(6) N13 0.071(4) 0.134(6) 0.037(3) 0.008(4) 0.017(3) -0.059(4) C0BA 0.064(5) 0.203(10) 0.052(5) -0.016(6) 0.012(4) -0.067(6) C6AA 0.086(6) 0.075(7) 0.114(8) 0.043(6) 0.058(6) 0.001(5) N2AA 0.103(7) 0.030(3) 0.064(5) -0.006(4) -0.019(5) 0.006(5) C7AA 0.144(10) 0.043(5) 0.108(9) 0.002(6) -0.036(7) 0.011(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O2 Ca1 N3 98.60(8) O2 Ca1 N2 176.29(10) O2 Ca1 B1 155.99(9) O2 Ca1 B2 124.30(9) O3 Ca1 O2 88.36(8) O3 Ca1 O1 106.32(9) O3 Ca1 N3 124.28(9) O3 Ca1 N2 93.55(10) O3 Ca1 B1 105.65(9) O3 Ca1 B2 118.84(9) O1 Ca1 O2 83.42(9) O1 Ca1 N3 129.37(9) O1 Ca1 N2 92.99(9) O1 Ca1 B1 110.22(9) O1 Ca1 B2 125.52(9) N3 Ca1 N2 82.95(9) N3 Ca1 B1 57.41(9) N3 Ca1 B2 25.70(8) N2 Ca1 B1 25.63(10) N2 Ca1 B2 57.30(9) B1 Ca1 B2 31.72(9) O2 P002 N8 110.17(16) O2 P002 N10 111.1(2) O2 P002 N9 111.7(2) N8 P002 N9 107.7(2) N10 P002 N8 109.98(18) N10 P002 N9 106.1(3) O3 P003 N11 111.93(14) O3 P003 N012 109.3(3) O3 P003 N01H 105.9(4) O3 P003 N12 123.1(4) O3 P003 N13 109.2(4) N11 P003 N012 100.6(3) N11 P003 N13 100.6(3) N01H P003 N11 125.7(4) N01H P003 N012 102.0(5) N12 P003 N11 105.9(4) N12 P003 N13 103.6(6) O4 P004 N00M 111.03(17) O4 P004 N00N 117.9(2) O4 P004 N014 110.9(6) O4 P004 N2AA 107.2(5) N00M P004 N014 100.7(5) N00M P004 N2AA 120.0(5) N00N P004 N00M 101.5(2) N00N P004 N014 113.1(6) N00N P004 N2AA 99.2(5) P002 O2 Ca1 166.25(15) P003 O3 Ca1 151.12(16) P1 O1 Ca1 149.39(16) C17 N3 Ca1 134.6(2) C17 N3 B2 118.2(3) B2 N3 Ca1 107.21(19) C4 N1 B1 123.0(3) C11 N4 B2 123.1(3) B1 N2 Ca1 107.02(19) C10 N2 Ca1 133.3(2) C10 N2 B1 119.5(3) C015 N11 P003 127.0(3) C015 N11 C01C 112.6(3) C01C N11 P003 117.2(3) N4 C11 C16 117.6(3) N4 C11 C12 122.0(3) C12 C11 C16 120.4(3) N1 C4 C5 118.0(3) N1 C4 C3 122.9(3) C3 C4 C5 119.1(3) C4 C5 C6 119.8(3) C4 C5 C10 119.8(3) C6 C5 C10 120.5(3) C017 N8 P002 124.9(3) C017 N8 C019 114.7(3) C019 N8 P002 120.1(3) N3 C17 C16 122.3(3) N3 C17 C18 120.9(3) C18 C17 C16 116.8(3) C11 C16 C17 119.8(3) C11 C16 C15 119.2(3) C15 C16 C17 121.0(3) C1 C6 C5 118.7(3) C7 C6 C5 119.5(3) C7 C6 C1 121.8(3) C016 N00M P004 119.1(3) C016 N00M C01I 113.3(5) C01I N00M P004 124.8(4) C01E N00N P004 118.3(3) C01E N00N C01K 114.3(5) C01K N00N P004 121.3(4) C11 C12 C13 119.6(4) C20 C15 C16 118.9(3) C20 C15 C14 122.9(3) C14 C15 C16 118.2(3) C2 C1 C6 120.2(3) C19 C20 C15 119.7(3) C13 C14 C15 121.1(3) C14 C13 C12 121.4(4) C17 C18 C19 121.5(3) C4 C3 C2 120.2(4) N1 B1 Ca1 164.7(2) N1 B1 B2 120.5(3) N2 B1 Ca1 47.36(14) N2 B1 N1 118.0(3) N2 B1 B2 121.6(3) B2 B1 Ca1 74.32(16) N3 B2 Ca1 47.09(15) N3 B2 N4 119.0(3) N3 B2 B1 121.0(3) N4 B2 Ca1 166.0(2) N4 B2 B1 119.9(3) B1 B2 Ca1 73.96(16) N2 C10 C5 121.7(3) N2 C10 C9 121.5(3) C9 C10 C5 116.7(3) C01J N10 P002 120.6(5) C01J N10 C01P 116.6(6) C01P N10 P002 122.2(6) C20 C19 C18 122.1(3) C1 C2 C3 122.1(3) C01F N012 P003 117.4(7) C01S N012 P003 120.9(7) C01S N012 C01F 110.9(9) C01O N9 P002 118.9(4) C01T N9 P002 129.0(5) C01T N9 C01O 111.9(5) C018 N014 P004 117.5(10) C01L N014 P004 125.0(12) C01L N014 C018 117.3(13) C10 C9 C8 122.0(4) C8 C7 C6 120.1(4) C7 C8 C9 121.0(5) C5BA N01H P003 127.2(8) C6AA N01H P003 115.3(8) C6AA N01H C5BA 116.8(10) O1 P1 N5A 115.7(2) O1 P1 N5AA 103.9(4) O1 P1 N3AA 114.7(4) O1 P1 N5B 120.4(3) O1 P1 N7 101.0(4) N5A P1 N7 94.2(5) N3AA P1 N5AA 108.7(5) N3AA P1 N5B 84.8(5) N5B P1 N5AA 123.0(5) N6 P1 O1 118.4(5) N6 P1 N5A 103.7(7) N6 P1 N7 121.9(7) C2BA N5A P1 127.7(8) C2BA N5A C0AA 111.5(10) C0AA N5A P1 117.5(7) C3AA N5AA P1 123.8(8) C3AA N5AA C2AA 116.8(13) C2AA N5AA P1 117.6(12) C1AA N3AA P1 119.9(11) C8AA N3AA P1 120.8(7) C8AA N3AA C1AA 116.9(11) C1BA N5B P1 107.6(10) C1BA N5B C4BA 112.5(11) C4BA N5B P1 122.4(8) P1 N6 C4AA 125.5(10) P1 N6 C7BA 120.0(10) C7BA N6 C4AA 114.2(11) C3BA N7 P1 124.9(10) C3BA N7 C6BA 114.2(12) C6BA N7 P1 115.9(10) C5AA N12 P003 122.0(9) C9AA N12 P003 112.7(9) C9AA N12 C5AA 112.4(11) C22 N13 P003 126.6(9) C22 N13 C0BA 113.2(9) C0BA N13 P003 118.9(6) C018 N2AA P004 121.3(10) C018 N2AA C7AA 112.6(10) C7AA N2AA P004 118.7(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ca1 O2 2.332(2) Ca1 O3 2.298(2) Ca1 O1 2.308(2) Ca1 N3 2.406(3) Ca1 N2 2.409(3) Ca1 B1 3.132(3) Ca1 B2 3.137(4) P002 O2 1.471(2) P002 N8 1.631(3) P002 N10 1.619(4) P002 N9 1.632(4) P003 O3 1.480(2) P003 N11 1.618(3) P003 N012 1.784(10) P003 N01H 1.562(9) P003 N12 1.513(9) P003 N13 1.716(8) P004 O4 1.481(2) P004 N00M 1.642(4) P004 N00N 1.638(3) P004 N014 1.660(17) P004 N2AA 1.643(14) O1 P1 1.458(2) N3 C17 1.386(4) N3 B2 1.424(4) N1 C4 1.376(4) N1 B1 1.452(4) N4 C11 1.378(4) N4 B2 1.442(4) N2 B1 1.417(5) N2 C10 1.380(4) N11 C015 1.458(5) N11 C01C 1.469(5) C11 C16 1.426(4) C11 C12 1.391(5) C4 C5 1.416(5) C4 C3 1.394(4) C5 C6 1.430(5) C5 C10 1.438(4) N8 C017 1.461(5) N8 C019 1.463(5) C17 C16 1.437(4) C17 C18 1.399(4) C16 C15 1.433(4) C6 C1 1.417(5) C6 C7 1.400(6) N00M C016 1.461(6) N00M C01I 1.489(6) N00N C01E 1.459(6) N00N C01K 1.466(7) C12 C13 1.402(6) C15 C20 1.412(5) C15 C14 1.423(5) C1 C2 1.350(6) C20 C19 1.362(6) C14 C13 1.362(6) C18 C19 1.401(5) C3 C2 1.396(6) B1 B2 1.713(5) C10 C9 1.397(6) N10 C01J 1.433(10) N10 C01P 1.474(8) N012 C01F 1.468(10) N012 C01S 1.456(13) N9 C01O 1.462(7) N9 C01T 1.418(7) N014 C018 1.488(17) N014 C01L 1.45(2) C018 N2AA 1.443(14) C9 C8 1.406(7) C7 C8 1.364(7) N01H C5BA 1.511(15) N01H C6AA 1.485(14) C22 N13 1.443(12) P1 N5A 1.676(6) P1 N5AA 1.774(13) P1 N3AA 1.551(10) P1 N5B 1.653(9) P1 N6 1.423(9) P1 N7 1.718(11) N5A C2BA 1.458(11) N5A C0AA 1.476(12) N5AA C3AA 1.318(18) N5AA C2AA 1.510(15) N3AA C1AA 1.483(12) N3AA C8AA 1.316(16) N5B C1BA 1.342(16) N5B C4BA 1.464(15) N6 C4AA 1.502(15) N6 C7BA 1.50(2) N7 C3BA 1.478(15) N7 C6BA 1.489(18) C5AA N12 1.489(14) N12 C9AA 1.389(16) N13 C0BA 1.471(12) N2AA C7AA 1.479(17)