#------------------------------------------------------------------------------ #$Date: 2021-10-03 03:40:19 +0300 (Sun, 03 Oct 2021) $ #$Revision: 269453 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/09/7060990.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_7060990 loop_ _publ_author_name 'Chen, Changjuan' 'Zhang, Aijiang' _publ_section_title ; Radii-dependent self-assembly polynuclear lanthanide complexes as catalysts for CO2 transformation into cyclic carbonates ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D1NJ03652A _journal_year 2021 _chemical_formula_moiety 'C48 H49 N11 O14 Pr2' _chemical_formula_sum 'C48 H49 N11 O14 Pr2' _chemical_formula_weight 1285.80 _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' _atom_sites_solution_hydrogens mixed _audit_creation_date 2021-08-31 _audit_creation_method ; Olex2 1.5 (compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6392) ; _audit_update_record ; 2021-09-25 deposited with the CCDC. 2021-10-01 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 106.684(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.4217(14) _cell_length_b 14.6810(11) _cell_length_c 27.191(2) _cell_measurement_reflns_used 2789 _cell_measurement_temperature 296.15 _cell_measurement_theta_max 27.855 _cell_measurement_theta_min 1.220 _cell_volume 6661.8(9) _computing_cell_refinement 'SAINT v7.68A (Bruker, 2009)' _computing_data_collection 'SAINT v7.68A (Bruker, 2009)' _computing_data_reduction 'SAINT v7.68A (Bruker, 2009)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 296.15 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measurement_device_type 'Bruker APEX2 CCD' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_unetI/netI 0.0514 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.981 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_number 45163 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.981 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.855 _diffrn_reflns_theta_min 1.564 _exptl_absorpt_coefficient_mu 1.504 _exptl_absorpt_correction_T_max 0.8456 _exptl_absorpt_correction_T_min 0.6885 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour green _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.282 _exptl_crystal_description block _exptl_crystal_F_000 2576 _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _refine_diff_density_max 1.796 _refine_diff_density_min -2.453 _refine_diff_density_rms 0.113 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 697 _refine_ls_number_reflns 15550 _refine_ls_number_restraints 194 _refine_ls_restrained_S_all 1.086 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0414 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+0.3993P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1122 _refine_ls_wR_factor_ref 0.1174 _reflns_Friedel_coverage 0.000 _reflns_number_gt 12367 _reflns_number_total 15550 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1nj03652a2.cif _cod_data_source_block 1_CCDC1 _cod_original_cell_volume 6661.9(9) _cod_database_code 7060990 _shelx_shelxl_version_number 2018/3 _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 0.864 _shelx_estimated_absorpt_t_min 0.840 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups, All O(H,H) groups 2. Restrained distances N11-C45 1.3 with sigma of 0.002 O9-H9A 0.87 with sigma of 0.01 C45A-C46A 2.5 with sigma of 0.002 C48A-C46A 2.4 with sigma of 0.002 Pr2-H9A 3.189366 with sigma of 0.02 C47-H9A 1.899329 with sigma of 0.02 N11-C46 \\sim N11-C48 with sigma of 0.02 C46-N11 \\sim C46A-N11A with sigma of 0.02 C48-N11 \\sim C48A-N11A with sigma of 0.02 C48-C46 \\sim C48A-C46A with sigma of 0.04 C45-O13 \\sim C45A-O13 with sigma of 0.02 C45-C46 \\sim C45A-C46A with sigma of 0.04 C45-N11 \\sim C45A-N11A with sigma of 0.02 N11-O13 \\sim N11A-O13 with sigma of 0.04 C45-C48 \\sim C45A-C48A with sigma of 0.04 N11A-C45A \\sim C12-C11 \\sim N11-C45 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints N11A \\sim C46A \\sim C48A \\sim C45A \\sim O13 \\sim C45 \\sim N11 \\sim C46 \\sim C48: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A 4. Rigid body (RIGU) restrains C46, C48, N11, C45, O13 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 C46A, N11A, C48A, C45A, O13 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 5. Others Sof(C45A)=Sof(H45A)=Sof(N11A)=Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)= Sof(C46A)=Sof(H46D)=Sof(H46E)=Sof(H46F)=1-FVAR(1) Sof(C45)=Sof(H45)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C46)=Sof(H46A)= Sof(H46B)=Sof(H46C)=Sof(N11)=FVAR(1) 6.a Everything fixed: C48, C46 6.b Fixed occupancy and ADP/Uiso: C45 6.c Riding coordinates: C46(H46A,H46B,H46C), N1(H1A), N4(H4A), N7(H7A), O14(H14C,H14D), C48A(H48D, H48E,H48F) 6.d Secondary CH2 refined with riding coordinates: C14(H14A,H14B), C29(H29A,H29B), C47(H47A,H47B) 6.e Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C9(H9), C11(H11), C16(H16), C17(H17), C18(H18), C20(H20), C22(H22), C24(H24), C26(H26), C31(H31), C32(H32), C34(H34), C35(H35), C37(H37), C39(H39), C41(H41), C45(H45), C45A(H45A) 6.f Idealised Me refined as rotating group: C15(H15A,H15B,H15C), C30(H30A,H30B,H30C), C44(H44A,H44B,H44C), C48(H48A,H48B, H48C), C46A(H46D,H46E,H46F) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL mo_20131016cc_0m in P2(1)/c 1.res created by SHELXL-2018/3 at 17:30:23 on 31-Aug-2021 CELL 0.71073 17.4217 14.681 27.1914 90 106.684 90 ZERR 4 0.0014 0.0011 0.0022 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O Pr UNIT 192 196 44 56 8 DFIX 1.3 0.002 N11 C45 SADI N11 C46 N11 C48 SADI C46 N11 C46A N11A SADI C48 N11 C48A N11A SADI 0.04 C48 C46 C48A C46A SADI C45 O13 C45A O13 SADI 0.04 C45 C46 C45A C46A SADI C45 N11 C45A N11A RIGU 0.001 0.001 C46 C48 N11 C45 O13 SIMU 0.01 0.02 2 N11A C46A C48A C45A O13 C45 N11 C46 C48 SADI 0.04 N11 O13 N11A O13 SADI 0.04 C45 C48 C45A C48A RIGU 0.001 0.001 C46A N11A C48A C45A O13 SADI N11A C45A C12 C11 N11 C45 DANG 2.5 0.002 C45A C46A DANG 2.4 0.002 C48A C46A DFIX 0.87 0.01 O9 H9a DANG 3.189366 0.02 Pr2 H9a DANG 1.899329 0.02 C47 H9a L.S. 20 PLAN 10 SIZE 0.1 0.12 0.1 TEMP -80.15 CONF BOND $H HTAB MORE -1 fmap 2 acta ABIN SIZE 0.1 0.12 0.1 TEMP -80.15 OMIT -1 0 6 OMIT 0 2 3 OMIT 1 2 1 OMIT -2 1 5 OMIT -3 4 5 OMIT 1 1 6 OMIT 1 0 0 OMIT -2 5 4 OMIT -1 1 1 OMIT -2 3 1 REM REM REM WGHT 0.062200 0.399300 FVAR 0.52855 0.67919 C1 1 0.231668 -0.133696 0.293454 11.00000 0.02668 0.03105 = 0.04927 0.00304 0.00765 0.00517 AFIX 43 H1 2 0.273285 -0.092660 0.309907 11.00000 -1.20000 AFIX 0 C2 1 0.241202 -0.226512 0.301671 11.00000 0.02837 0.03504 = 0.06639 0.01320 0.01172 0.00607 AFIX 43 H2 2 0.289907 -0.247760 0.324612 11.00000 -1.20000 AFIX 0 C3 1 0.118867 -0.256235 0.248362 11.00000 0.03279 0.02702 = 0.05602 -0.00746 0.01552 -0.00915 AFIX 43 H3 2 0.079035 -0.299103 0.231691 11.00000 -1.20000 AFIX 0 C4 1 0.102197 -0.164541 0.238431 11.00000 0.03050 0.02746 = 0.04008 0.00008 0.01068 0.00348 AFIX 43 H4 2 0.051699 -0.145651 0.216650 11.00000 -1.20000 AFIX 0 C5 1 0.160130 -0.101496 0.260702 11.00000 0.02877 0.02050 = 0.03240 -0.00061 0.01157 0.00124 C6 1 0.150897 -0.001077 0.250870 11.00000 0.02521 0.02578 = 0.02888 0.00089 0.01186 0.00001 C7 1 0.012470 0.153743 0.189953 11.00000 0.02368 0.02732 = 0.03252 0.00144 0.00726 -0.00509 AFIX 43 H7 2 -0.029545 0.110912 0.177645 11.00000 -1.20000 AFIX 0 C8 1 -0.004043 0.247765 0.174428 11.00000 0.02595 0.02464 = 0.02884 0.00414 0.00578 0.00127 C9 1 -0.076662 0.264348 0.136833 11.00000 0.02992 0.02756 = 0.03686 0.00292 0.00238 -0.00298 AFIX 43 H9 2 -0.108217 0.213646 0.121220 11.00000 -1.20000 AFIX 0 C10 1 -0.104448 0.350211 0.121456 11.00000 0.03205 0.03046 = 0.03746 0.00804 -0.00217 0.00152 C11 1 -0.058090 0.422957 0.145332 11.00000 0.03217 0.03046 = 0.03507 0.00676 0.00245 0.00449 AFIX 43 H11 2 -0.076850 0.483097 0.136072 11.00000 -1.20000 AFIX 0 C12 1 0.014618 0.411107 0.182214 11.00000 0.02851 0.01924 = 0.02802 0.00380 0.00958 0.00284 C13 1 0.043306 0.322270 0.197459 11.00000 0.02570 0.02644 = 0.02244 0.00059 0.01157 0.00218 C14 1 0.060813 0.490357 0.209222 11.00000 0.03269 0.02366 = 0.02734 0.00309 0.00931 0.00276 AFIX 23 H14A 2 0.114507 0.490760 0.203620 11.00000 -1.20000 H14B 2 0.033029 0.547305 0.194654 11.00000 -1.20000 AFIX 0 C15 1 -0.184289 0.364444 0.080663 11.00000 0.04684 0.03425 = 0.06579 0.00289 -0.01114 0.00045 AFIX 137 H15A 2 -0.174534 0.384937 0.048683 11.00000 -1.50000 H15B 2 -0.215574 0.410605 0.092490 11.00000 -1.50000 H15C 2 -0.214098 0.306940 0.074585 11.00000 -1.50000 AFIX 0 C16 1 0.541564 0.104632 0.168419 11.00000 0.04062 0.07334 = 0.07756 0.00695 0.03319 0.01324 AFIX 43 H16 2 0.532653 0.091685 0.132988 11.00000 -1.20000 AFIX 0 C17 1 0.626182 0.121348 0.247721 11.00000 0.02540 0.04960 = 0.09078 0.00103 0.01234 0.00295 AFIX 43 H17 2 0.679330 0.120888 0.270010 11.00000 -1.20000 AFIX 0 C18 1 0.564742 0.139367 0.269057 11.00000 0.03473 0.05616 = 0.07707 -0.00333 0.01718 0.00147 AFIX 43 H18 2 0.575606 0.151993 0.304666 11.00000 -1.20000 AFIX 0 C19 1 0.487697 0.138528 0.237445 11.00000 0.02743 0.01773 = 0.06669 0.00696 0.01936 0.00275 C20 1 0.476239 0.122325 0.185792 11.00000 0.02984 0.05996 = 0.06936 0.01076 0.02137 0.00996 AFIX 43 H20 2 0.423840 0.123382 0.162512 11.00000 -1.20000 AFIX 0 C21 1 0.414525 0.152473 0.254605 11.00000 0.02713 0.02255 = 0.05156 0.00325 0.01477 0.00279 C22 1 0.355774 0.136102 0.365285 11.00000 0.03622 0.02497 = 0.04197 0.00321 0.00372 0.00517 AFIX 43 H22 2 0.406464 0.116322 0.386388 11.00000 -1.20000 AFIX 0 C23 1 0.290910 0.140156 0.387743 11.00000 0.03921 0.02196 = 0.03353 0.00244 0.00588 -0.00124 C24 1 0.302553 0.099970 0.436806 11.00000 0.05660 0.02720 = 0.03346 0.00260 0.00429 0.00117 AFIX 43 H24 2 0.353357 0.074224 0.453582 11.00000 -1.20000 AFIX 0 C25 1 0.243540 0.096724 0.461039 11.00000 0.07891 0.02847 = 0.02384 0.00327 0.01341 -0.00570 C26 1 0.167459 0.134767 0.434895 11.00000 0.06246 0.03434 = 0.03420 0.00164 0.02592 -0.01473 AFIX 43 H26 2 0.125118 0.131244 0.450381 11.00000 -1.20000 AFIX 0 C27 1 0.153576 0.176901 0.387317 11.00000 0.04168 0.03024 = 0.02560 0.00802 0.00644 -0.00867 C28 1 0.217298 0.181469 0.364105 11.00000 0.03638 0.02180 = 0.02341 0.00077 0.00599 -0.00671 C29 1 0.074855 0.214358 0.358427 11.00000 0.03438 0.04064 = 0.04089 -0.00007 0.01576 -0.01464 AFIX 23 H29A 2 0.055830 0.181968 0.325205 11.00000 -1.20000 H29B 2 0.035945 0.202453 0.377991 11.00000 -1.20000 AFIX 0 C30 1 0.257143 0.057479 0.513641 11.00000 0.10224 0.05182 = 0.03385 0.00906 0.01018 -0.01360 AFIX 137 H30A 2 0.222448 0.004301 0.511861 11.00000 -1.50000 H30B 2 0.244563 0.103431 0.536303 11.00000 -1.50000 H30C 2 0.313327 0.039005 0.527208 11.00000 -1.50000 AFIX 0 C31 1 0.369212 0.262577 0.573061 11.00000 0.06406 0.05488 = 0.03507 0.00940 0.00670 -0.00079 AFIX 43 H31 2 0.414951 0.233820 0.595315 11.00000 -1.20000 AFIX 0 C32 1 0.373288 0.289005 0.524628 11.00000 0.04799 0.05470 = 0.03135 0.00651 0.00920 -0.00300 AFIX 43 H32 2 0.420320 0.278827 0.514379 11.00000 -1.20000 AFIX 0 C33 1 0.307294 0.330154 0.492236 11.00000 0.04439 0.03071 = 0.02529 0.00010 0.01006 -0.00313 C34 1 0.240249 0.344477 0.509193 11.00000 0.06045 0.05761 = 0.02941 0.00621 0.01510 0.00700 AFIX 43 H34 2 0.193838 0.373230 0.487685 11.00000 -1.20000 AFIX 0 C35 1 0.242575 0.315792 0.558354 11.00000 0.07554 0.06628 = 0.03243 0.00459 0.02848 0.00737 AFIX 43 H35 2 0.196737 0.325846 0.569916 11.00000 -1.20000 AFIX 0 C36 1 0.299096 0.356313 0.438043 11.00000 0.03978 0.02528 = 0.02388 -0.00193 0.00728 -0.00167 C37 1 0.411296 0.367098 0.352978 11.00000 0.02589 0.03091 = 0.03563 -0.00515 0.00732 -0.00147 AFIX 43 H37 2 0.461243 0.356481 0.377917 11.00000 -1.20000 AFIX 0 C38 1 0.411352 0.377392 0.300201 11.00000 0.02563 0.02366 = 0.04183 -0.00624 0.01566 -0.00323 C39 1 0.484981 0.385227 0.289071 11.00000 0.02931 0.02713 = 0.05519 -0.00743 0.02047 -0.00662 AFIX 43 H39 2 0.533001 0.384136 0.316659 11.00000 -1.20000 AFIX 0 C40 1 0.490301 0.394392 0.239961 11.00000 0.03917 0.02947 = 0.06423 -0.00906 0.03653 -0.00702 C41 1 0.420549 0.397814 0.200668 11.00000 0.05871 0.02311 = 0.04795 -0.00663 0.03576 -0.00644 AFIX 43 H41 2 0.423308 0.407546 0.166677 11.00000 -1.20000 AFIX 0 C42 1 0.345781 0.387518 0.208851 11.00000 0.05462 0.01883 = 0.03020 -0.00209 0.02457 -0.00268 C43 1 0.340289 0.374954 0.259584 11.00000 0.02829 0.01325 = 0.03562 -0.00177 0.01679 -0.00173 C44 1 0.570807 0.399650 0.229647 11.00000 0.05090 0.05542 = 0.09465 -0.00373 0.05256 -0.00747 AFIX 137 H44A 2 0.564373 0.427003 0.195825 11.00000 -1.50000 H44B 2 0.593085 0.338209 0.230346 11.00000 -1.50000 H44C 2 0.607239 0.437152 0.256071 11.00000 -1.50000 AFIX 2 PART 1 C45 1 0.150019 0.045275 0.134476 21.00000 0.08996 0.08996 = 0.08996 0.00000 0.02583 0.00000 AFIX 43 H45 2 0.094222 0.045814 0.131130 21.00000 -1.20000 AFIX 0 PART 0 C47 1 0.267112 0.384767 0.165861 11.00000 0.04936 0.02430 = 0.02317 -0.00177 0.01799 -0.00271 AFIX 23 H47A 2 0.228427 0.427785 0.173660 11.00000 -1.20000 H47B 2 0.276578 0.403795 0.133160 11.00000 -1.20000 AFIX 1 PART 1 C48 1 0.135770 -0.116630 0.094950 21.00000 0.07782 0.07782 = 0.07782 0.00000 0.02234 0.00000 AFIX 137 H48A 2 0.126486 -0.118314 0.057666 21.00000 -1.50000 H48B 2 0.084484 -0.122270 0.102806 21.00000 -1.50000 H48C 2 0.170912 -0.167189 0.110828 21.00000 -1.50000 AFIX 1 C46 1 0.262020 -0.048840 0.132720 21.00000 0.07782 0.07782 = 0.07782 0.00000 0.02234 0.00000 AFIX 3 H46A 2 0.293220 0.007490 0.141140 21.00000 -1.50000 H46B 2 0.276450 -0.080570 0.104930 21.00000 -1.50000 H46C 2 0.273660 -0.088150 0.163100 21.00000 -1.50000 AFIX 0 PART 0 N1 3 0.078891 0.029307 0.228801 11.00000 0.02249 0.02147 = 0.03580 0.00283 0.00917 -0.00245 AFIX 3 H1A 2 0.034781 -0.005933 0.221751 11.00000 -1.20000 AFIX 0 N2 3 0.079525 0.123512 0.219101 11.00000 0.02403 0.01561 = 0.02729 0.00277 0.00889 -0.00054 PART 1 N11 3 0.175390 -0.026443 0.116062 21.00000 0.07904 0.09404 = 0.10687 -0.01925 0.02643 -0.00768 PART 0 N3 3 0.185867 -0.287669 0.279194 11.00000 0.03296 0.02700 = 0.06964 0.00452 0.02200 0.00007 N4 3 0.362303 0.354935 0.420909 11.00000 0.02865 0.03309 = 0.02465 -0.00032 0.00471 0.00127 AFIX 3 H4A 2 0.411263 0.343915 0.438329 11.00000 -1.20000 AFIX 0 N5 3 0.348211 0.371300 0.368649 11.00000 0.02818 0.02361 = 0.02476 -0.00153 0.00849 -0.00021 N6 3 0.306312 0.274673 0.590193 11.00000 0.08340 0.05000 = 0.02726 0.01007 0.01406 0.00425 N7 3 0.421241 0.146184 0.304987 11.00000 0.02747 0.03153 = 0.05013 0.00261 0.00703 0.00712 AFIX 3 H7A 2 0.469221 0.122734 0.331127 11.00000 -1.20000 AFIX 0 N8 3 0.350078 0.157562 0.318153 11.00000 0.02624 0.01947 = 0.04080 -0.00151 0.00924 0.00115 N9 3 0.616353 0.104766 0.198708 11.00000 0.03366 0.03401 = 0.10096 0.00019 0.03520 0.00324 N10 3 0.100888 0.496378 0.411519 11.00000 0.07930 0.05199 = 0.04240 -0.00160 0.03252 0.01086 O1 4 0.214786 0.045967 0.263579 11.00000 0.02490 0.01937 = 0.04680 -0.00109 0.00688 0.00178 O2 4 0.112871 0.313247 0.233402 11.00000 0.02008 0.02177 = 0.02647 0.00066 0.00556 0.00250 O3 4 0.069661 0.487454 0.263890 11.00000 0.02767 0.02685 = 0.02792 -0.00293 0.00738 0.00201 O4 4 0.350004 0.166525 0.222229 11.00000 0.02528 0.03813 = 0.04525 0.00570 0.01456 0.00531 O5 4 0.204857 0.229080 0.320735 11.00000 0.02874 0.02326 = 0.02763 0.00430 0.00989 -0.00185 O6 4 0.076335 0.311878 0.348579 11.00000 0.02850 0.04103 = 0.03661 0.00110 0.01444 -0.00364 O7 4 0.231680 0.377026 0.409631 11.00000 0.03555 0.05442 = 0.02415 0.00939 0.01130 0.00795 O8 4 0.269255 0.357658 0.265638 11.00000 0.02410 0.02656 = 0.02292 -0.00049 0.01026 -0.00150 O9 4 0.234897 0.295569 0.160735 11.00000 0.04235 0.03846 = 0.02547 -0.00106 0.01219 -0.00220 H9A 2 0.253613 0.269985 0.136749 11.00000 -1.50000 O10 4 0.116254 0.501232 0.369028 11.00000 0.05023 0.04400 = 0.03175 0.00617 0.01955 0.01662 O11 4 0.118564 0.558830 0.442077 11.00000 0.24815 0.06464 = 0.07315 -0.02162 0.09109 -0.01943 O12 4 0.067752 0.424430 0.422795 11.00000 0.06061 0.06174 = 0.05825 0.00505 0.03456 0.00250 O13 4 0.186610 0.111974 0.155373 11.00000 0.05423 0.08175 = 0.04668 -0.00294 0.03626 -0.00282 O14 4 0.239472 0.540287 0.309914 11.00000 0.02149 0.02437 = 0.06718 0.00703 0.01549 0.00054 AFIX 3 H14C 2 0.226012 0.577137 0.330094 11.00000 -1.50000 H14D 2 0.290232 0.535747 0.318374 11.00000 -1.50000 AFIX 0 PR1 5 0.181676 0.392025 0.316046 11.00000 0.02089 0.02155 = 0.02261 0.00068 0.00922 0.00074 PR2 5 0.218246 0.200567 0.236978 11.00000 0.02105 0.02024 = 0.02710 -0.00075 0.00900 0.00031 PART 2 C45A 1 0.233063 0.042327 0.164191 -21.00000 0.07258 0.08866 = 0.08857 -0.00949 0.02959 0.00620 AFIX 43 H45A 2 0.287523 0.041248 0.184363 -21.00000 -1.20000 AFIX 0 N11A 3 0.190604 -0.028389 0.139731 -21.00000 0.07387 0.09234 = 0.08426 -0.01193 0.03437 0.00050 C48A 1 0.186505 -0.129177 0.148821 -21.00000 0.11434 0.09674 = 0.12200 -0.00183 0.00550 -0.00832 AFIX 3 H48D 2 0.214205 -0.152327 0.183141 -21.00000 -1.50000 H48E 2 0.219585 -0.140227 0.125721 -21.00000 -1.50000 H48F 2 0.135025 -0.160587 0.135661 -21.00000 -1.50000 AFIX 0 C46A 1 0.119336 -0.011520 0.091136 -21.00000 0.06830 0.09365 = 0.08224 -0.01438 0.03751 0.00207 AFIX 137 H46D 2 0.108949 0.054033 0.086851 -21.00000 -1.50000 H46E 2 0.071494 -0.042409 0.094931 -21.00000 -1.50000 H46F 2 0.132548 -0.035529 0.060929 -21.00000 -1.50000 AFIX 0 HKLF 4 REM mo_20131016cc_0m in P2(1)/c REM wR2 = 0.1174, GooF = S = 1.078, Restrained GooF = 1.086 for all data REM R1 = 0.0414 for 12367 Fo > 4sig(Fo) and 0.0513 for all 15550 data REM 697 parameters refined using 194 restraints END WGHT 0.0623 0.3036 REM Instructions for potential hydrogen bonds EQIV $1 -x, y-1/2, -z+1/2 HTAB C4 O6_$1 HTAB C7 O3_$1 HTAB C7 O10_$1 HTAB C34 O12 EQIV $2 x, -y+1/2, z+1/2 HTAB C35 O13_$2 HTAB C48 O12_$1 HTAB N1 O3_$1 EQIV $3 x, -y+1/2, z-1/2 HTAB O9 N6_$3 EQIV $4 -x+1, y+1/2, -z+1/2 HTAB O14 N9_$4 HTAB C45A O4 HTAB C46A O12_$1 REM Highest difference peak 1.796, deepest hole -2.453, 1-sigma level 0.113 Q1 1 0.2288 0.4001 0.3180 11.00000 0.05 1.80 Q2 1 0.1702 0.0328 0.1404 11.00000 0.05 1.68 Q3 1 0.2660 0.2042 0.2415 11.00000 0.05 1.49 Q4 1 0.2089 0.3907 0.3500 11.00000 0.05 1.42 Q5 1 0.1997 0.1790 0.2110 11.00000 0.05 0.93 Q6 1 0.1336 -0.0680 0.0805 11.00000 0.05 0.80 Q7 1 0.1421 -0.0028 0.0990 11.00000 0.05 0.80 Q8 1 0.1627 0.2013 0.2273 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16 5 7 0.8398 -0.1261 16 5 8 0.1902 -0.2876 16 5 9 0.7376 -0.2711 16 5 10 -0.0078 -0.4391 16 5 11 1.3895 -0.2644 16 5 12 0.2539 0.1777 16 5 13 1.5166 0.0350 16 5 14 0.2737 0.2080 16 5 15 0.3853 -0.3547 16 6 0 -1.9309 -0.1935 16 6 1 0.1653 -0.1712 16 6 2 -2.3209 -0.1667 16 6 3 1.0914 0.0402 16 6 4 0.8808 -0.0564 16 6 5 0.4787 0.0687 16 6 6 2.4758 0.1380 16 6 7 -0.7392 -0.3512 16 6 8 0.3943 0.0686 16 6 9 -0.4387 -0.0842 16 6 10 -1.8404 -0.4079 16 6 11 -1.3560 -0.0498 16 6 12 -0.2994 -0.4310 16 6 13 -1.2319 0.3962 16 6 14 1.5577 -0.1916 16 7 0 -0.5044 0.0035 16 7 1 1.4498 0.0476 16 7 2 0.2857 0.0279 16 7 3 -0.2349 0.0738 16 7 4 0.6105 0.0532 16 7 5 -1.3924 -0.0040 16 7 6 0.8958 -0.0120 16 7 7 -1.0860 -0.1312 16 7 8 -0.1027 -0.2021 16 7 9 -0.5405 0.4361 16 7 10 -1.4988 0.1616 16 7 11 0.0626 0.2808 16 7 12 -0.5655 1.1379 16 7 13 -0.6025 -0.3385 16 8 0 -0.8814 0.0955 16 8 1 -0.2205 -0.0961 16 8 2 -1.3896 -0.0722 16 8 3 -0.1106 -0.1574 16 8 4 -0.1783 -0.1923 16 8 5 -0.3001 -0.0784 16 8 6 -0.8864 0.0340 16 8 7 0.3115 -0.4038 16 8 8 -1.5005 0.0365 16 8 9 1.2367 -0.5622 16 8 10 -0.8739 -0.1107 16 8 11 2.4535 -0.0635 16 8 12 -0.4938 -0.1699 16 9 0 -0.9800 -0.2509 16 9 1 0.4293 -0.0602 16 9 2 -1.1628 -0.0449 16 9 3 1.3831 0.1079 16 9 4 0.7096 0.3211 16 9 5 0.8429 0.2283 16 9 6 2.1857 -0.0504 16 9 7 2.0347 0.4893 16 9 8 0.8453 -0.2504 16 9 9 3.4846 -0.1856 16 9 10 -0.1268 -0.0055 16 10 0 1.3604 0.0425 16 10 1 -1.2054 -0.1185 16 10 2 1.2726 -0.2704 16 10 3 0.6363 0.0168 16 10 4 -0.0023 0.0366 16 10 5 -0.0432 -0.1153 16 10 6 0.3020 0.5407 16 10 7 -0.0040 0.1310 16 10 8 -0.5541 1.1860 16 10 9 2.4701 0.6599 16 11 0 0.2920 -0.0809 16 11 1 -2.4410 0.3026 16 11 2 -0.3774 0.0673 16 11 3 -0.0604 0.0510 16 11 4 -0.4127 0.0354 16 11 5 2.7394 -0.0862 16 11 6 1.9765 -0.4494 16 11 7 0.6637 0.2127 16 12 0 1.1366 0.1126 16 12 1 -0.7250 0.0366 16 12 2 3.2629 -0.1364 16 12 3 -0.2930 0.6571 16 12 4 2.2102 -0.5839 16 13 0 0.6210 -0.4101 17 0 0 -1.5872 -2.1271 17 0 2 -1.0047 -0.2203 17 0 4 -0.0159 0.2292 17 0 6 0.4148 -0.6143 17 0 8 -0.7400 0.4014 17 0 10 -1.5265 -0.2668 17 0 12 -0.4225 0.6092 17 0 14 -0.0220 -0.0598 17 1 0 0.3940 0.8762 17 1 1 -0.2937 1.1789 17 1 2 0.1166 -0.5187 17 1 3 -0.8413 -0.4039 17 1 4 -0.2303 0.5888 17 1 5 -3.7278 0.2675 17 1 6 -1.3209 -0.1402 17 1 7 -5.2088 -0.0003 17 1 8 -0.1487 0.0442 17 1 9 -1.9086 0.0448 17 1 10 1.1586 0.1226 17 1 11 0.6387 -0.0551 17 1 12 0.8827 0.0318 17 1 13 0.9215 0.1526 17 1 14 0.2878 0.1015 17 2 0 1.2366 0.2873 17 2 1 -0.6231 0.8668 17 2 2 0.2818 0.1012 17 2 3 -0.5009 0.1292 17 2 4 -0.3577 0.1311 17 2 5 0.7914 -0.1645 17 2 6 0.8334 0.2281 17 2 7 1.0603 0.6809 17 2 8 0.5557 -0.0766 17 2 9 0.6243 -0.5821 17 2 10 -0.3006 -0.1951 17 2 11 0.6533 -0.3637 17 2 12 -0.4573 0.3689 17 2 13 -0.0708 -0.3424 17 2 14 -0.2683 1.0569 17 3 0 -0.0679 0.1464 17 3 1 -0.3957 -0.2373 17 3 2 0.0188 -0.0154 17 3 3 1.4862 0.2894 17 3 4 -0.2055 0.3590 17 3 5 1.5409 -0.3439 17 3 6 0.0209 -0.3233 17 3 7 0.4371 0.1259 17 3 8 0.3131 0.1954 17 3 9 -0.4154 0.0331 17 3 10 -0.3710 -0.1094 17 3 11 1.0087 0.3982 17 3 12 0.1846 -0.5661 17 3 13 2.0428 0.6041 17 3 14 -0.1192 -0.4707 17 4 0 0.2386 0.1113 17 4 1 -0.8855 -0.1197 17 4 2 0.5566 -0.3359 17 4 3 -0.1344 -0.0300 17 4 4 0.8822 0.0547 17 4 5 -0.1486 0.1973 17 4 6 0.0454 -0.1417 17 4 7 0.2561 0.0558 17 4 8 0.6554 -0.0565 17 4 9 1.5665 -0.2618 17 4 10 0.5970 0.8687 17 4 11 0.1099 -0.1302 17 4 12 -0.7354 -0.2868 17 4 13 -1.4961 0.4171 17 5 0 1.9071 0.2019 17 5 1 1.2393 0.0320 17 5 2 0.4861 -0.1863 17 5 3 0.3868 -0.2240 17 5 4 -0.9441 -0.3824 17 5 5 -0.3451 -0.4333 17 5 6 -0.2333 0.2250 17 5 7 0.5051 0.3176 17 5 8 -0.1303 0.0148 17 5 9 0.3355 0.2811 17 5 10 0.2665 0.1341 17 5 11 -0.0931 -0.0278 17 5 12 0.6083 -0.1882 17 5 13 -0.8693 -0.2029 17 6 0 -0.0985 -0.0524 17 6 1 -0.2665 -0.0522 17 6 2 0.8334 0.0121 17 6 3 0.4132 0.0220 17 6 4 0.5138 -0.1632 17 6 5 0.8319 -0.1885 17 6 6 -0.5646 -0.0570 17 6 7 0.6051 -0.0822 17 6 8 0.0758 -0.1052 17 6 9 0.0109 -0.2849 17 6 10 0.9077 0.2803 17 6 11 -0.6539 -0.4512 17 6 12 -0.3310 0.7763 17 7 0 -0.5396 0.1240 17 7 1 -1.1684 -0.1132 17 7 2 0.8253 0.0547 17 7 3 -2.0188 -0.1772 17 7 4 1.1967 -0.1932 17 7 5 -1.3532 -0.2141 17 7 6 0.3591 -0.2198 17 7 7 -0.8343 -0.3427 17 7 8 -0.3562 0.0440 17 7 9 -0.8371 -0.4018 17 7 10 0.3922 -0.2838 17 7 11 -2.2387 -0.6147 17 8 0 -0.1292 -0.0734 17 8 1 -0.3803 -0.1763 17 8 2 0.1974 -0.1178 17 8 3 -0.0398 -0.0261 17 8 4 -0.3576 0.1155 17 8 5 0.2221 0.3580 17 8 6 -1.6102 0.2256 17 8 7 1.0982 0.1853 17 8 8 -1.3963 0.3036 17 8 9 1.2267 0.2137 17 9 0 2.1845 0.1226 17 9 1 0.1434 0.0863 17 9 2 -0.1362 -0.1304 17 9 3 -0.7154 0.0146 17 9 4 -0.1589 -0.2102 17 9 5 -0.0732 -0.1146 17 9 6 -0.2094 0.4875 17 9 7 1.5526 -0.7096 17 9 8 -0.9084 0.7568 17 10 0 0.5143 0.0103 17 10 1 0.4101 0.2172 17 10 2 0.0621 0.2457 17 10 3 -0.5105 0.3071 17 10 4 0.7093 -0.2127 17 10 5 -2.3704 0.1718 17 10 6 1.1464 -1.1073 17 11 0 0.4524 -0.2398 17 11 1 -0.3939 0.0386 17 11 2 -0.9144 -0.4869 17 11 3 1.4486 0.6711 17 12 0 1.7190 -0.3416 18 0 0 0.2367 -1.9095 18 0 2 -0.2573 0.9209 18 0 4 -0.1901 -0.4650 18 0 6 1.5011 0.2304 18 0 8 0.0289 0.2152 18 0 10 -1.6648 -0.2846 18 0 12 -0.4643 -0.3500 18 1 0 -0.8075 -0.8346 18 1 1 -0.6239 -0.8463 18 1 2 -0.1939 0.1037 18 1 3 -1.2240 -0.4153 18 1 4 0.1374 0.1455 18 1 5 -0.6646 0.6236 18 1 6 0.3571 -0.5718 18 1 7 2.0616 -0.5208 18 1 8 0.2047 0.4266 18 1 9 2.6952 0.1177 18 1 10 -0.2103 -0.4658 18 1 11 0.2521 -0.4113 18 1 12 0.7193 -0.5867 18 2 0 -0.1218 0.0330 18 2 1 0.0823 0.8475 18 2 2 -0.8234 0.2541 18 2 3 0.7596 -0.6670 18 2 4 0.8354 0.3527 18 2 5 -0.3124 0.6040 18 2 6 0.7190 -0.1665 18 2 7 -1.9256 0.2298 18 2 8 0.3253 -0.1413 18 2 9 -0.7401 0.4680 18 2 10 2.1707 0.5058 18 2 11 -0.5039 1.2990 18 2 12 2.5651 0.5855 18 3 0 0.3511 0.0547 18 3 1 2.1034 0.4887 18 3 2 -0.9044 0.1788 18 3 3 0.2978 -0.0485 18 3 4 -1.3427 0.0499 18 3 5 -1.3436 -0.4015 18 3 6 -0.2452 -0.0478 18 3 7 -0.2740 0.1878 18 3 8 -1.4681 0.5190 18 3 9 0.4760 -0.7604 18 3 10 -1.6253 0.4089 18 3 11 0.4691 -0.8064 18 4 0 0.2508 0.1405 18 4 1 -0.5548 0.2586 18 4 2 0.1651 -0.0651 18 4 3 -0.1223 0.2019 18 4 4 0.6190 0.1035 18 4 5 -0.0321 -0.2947 18 4 6 0.7989 -0.4691 18 4 7 0.0569 -0.1691 18 4 8 0.5162 -0.1781 18 4 9 -0.1159 0.3441 18 4 10 -0.8736 -0.8509 18 4 11 -0.7708 0.6929 18 5 0 -0.3353 -0.0249 18 5 1 -0.1887 -0.1002 18 5 2 -1.0802 0.0050 18 5 3 -0.6098 0.0671 18 5 4 -0.4276 0.3448 18 5 5 -0.3832 0.1953 18 5 6 -1.1777 -0.1548 18 5 7 -0.6277 -0.0172 18 5 8 -1.7161 -0.2923 18 5 9 0.7264 0.0769 18 5 10 -0.0601 0.1677 18 6 0 1.8091 -0.1431 18 6 1 2.6666 0.3329 18 6 2 0.3329 -0.0236 18 6 3 2.2272 -0.0312 18 6 4 -0.2838 0.1670 18 6 5 0.3389 -0.2202 18 6 6 0.5131 -0.0807 18 6 7 0.4584 0.6699 18 6 8 -0.2346 -0.6894 18 6 9 -0.2320 0.9918 18 7 0 0.8943 0.1327 18 7 1 -0.5189 -0.1631 18 7 2 -0.4090 -0.2698 18 7 3 -0.8556 -0.0204 18 7 4 0.2535 -0.4571 18 7 5 -0.5449 -0.0403 18 7 6 1.0419 0.0412 18 7 7 -0.3166 0.6464 18 7 8 0.0786 0.2662 18 8 0 0.1757 -0.0416 18 8 1 -0.2052 0.2534 18 8 2 2.4531 -0.1405 18 8 3 -0.7044 0.1690 18 8 4 2.3377 -0.2171 18 8 5 -1.2020 -0.0286 18 8 6 0.8661 -0.0403 18 9 0 0.0224 -0.3522 18 9 1 -0.0762 -0.2222 18 9 2 -0.2572 -0.0773 18 9 3 0.4743 0.0708 18 9 4 0.8492 0.8521 18 10 0 1.6915 -0.0718 18 10 1 -0.6937 -0.1049 18 10 2 -0.1168 -0.6301 19 0 0 0.8243 1.3243 19 0 2 1.0724 1.0416 19 0 4 0.2796 -0.2456 19 0 6 -1.5732 0.3775 19 0 8 -0.8376 -0.4558 19 0 10 0.8272 1.2082 19 1 0 0.6710 -1.3457 19 1 1 -0.6916 -1.1033 19 1 2 -0.5961 0.0877 19 1 3 -0.5287 0.0565 19 1 4 -0.5435 -0.2295 19 1 5 -0.7555 -0.3244 19 1 6 1.7733 0.3544 19 1 7 -1.7060 0.1635 19 1 8 1.8404 -0.2877 19 1 9 -2.8967 -0.0247 19 2 0 0.6335 -0.1105 19 2 1 -0.4586 -0.6942 19 2 2 0.4442 0.1146 19 2 3 -0.0106 0.2033 19 2 4 0.5338 0.0087 19 2 5 0.4017 1.2383 19 2 6 1.1590 0.2888 19 2 7 1.7584 -0.5183 19 2 8 2.3329 0.4150 19 2 9 2.0961 0.0364 19 3 0 0.3848 -0.5891 19 3 1 -0.4773 0.1548 19 3 2 -0.4483 0.8183 19 3 3 0.9771 -0.2464 19 3 4 0.1421 0.1927 19 3 5 1.7609 0.5937 19 3 6 -0.0771 -0.3743 19 3 7 0.0316 -0.2604 19 3 8 -0.7642 -0.0343 19 3 9 -0.5070 -0.3008 19 4 0 -0.5365 -0.1525 19 4 1 0.5270 0.1682 19 4 2 0.2916 -0.3430 19 4 3 0.0784 0.3221 19 4 4 0.2857 -0.1256 19 4 5 -0.6606 0.7670 19 4 6 0.0819 0.0300 19 4 7 1.2462 0.2003 19 4 8 -0.8127 0.4926 19 5 0 -1.8411 0.0522 19 5 1 -1.0046 0.1153 19 5 2 -1.1526 -0.3100 19 5 3 -0.9047 -0.1046 19 5 4 0.0150 -0.1975 19 5 5 -0.1193 -0.3236 19 5 6 -0.8029 0.1325 19 5 7 -0.3813 -0.0721 19 6 0 -2.2044 -0.0056 19 6 1 1.3719 -0.3078 19 6 2 -1.1471 -0.0861 19 6 3 -0.3428 -0.0435 19 6 4 -1.4687 -0.0201 19 6 5 -0.6373 -0.2116 19 6 6 -2.9366 -0.5075 19 7 0 -1.5923 -0.1342 19 7 1 0.9031 0.2787 19 7 2 0.0628 0.2443 19 7 3 0.8655 -0.1203 19 7 4 0.7410 0.0436 19 7 5 0.9831 -0.1998 19 8 0 0.3047 -0.0777 19 8 1 0.3435 -0.0259 19 8 2 -0.5233 0.0192 19 8 3 -0.8475 0.5718 19 9 0 0.0713 0.2744 19 9 1 0.2263 0.9666 20 0 0 0.2111 3.3545 20 0 2 1.2229 0.1666 20 0 4 0.2623 -0.0947 20 0 6 -1.5753 0.6391 20 1 0 -0.0667 0.5065 20 1 1 0.0002 0.0374 20 1 2 1.6246 0.5294 20 1 3 0.0917 0.6107 20 1 4 1.2179 -0.7277 20 1 5 -0.0574 -0.0303 20 1 6 -1.0136 -0.9919 20 2 0 -0.5841 -0.0702 20 2 1 0.5036 -1.1176 20 2 2 -0.4417 -0.6773 20 2 3 -0.0769 -0.6553 20 2 4 0.4852 -0.2289 20 2 5 -1.1543 -0.4736 20 2 6 0.4993 0.4306 20 3 0 0.7973 0.4168 20 3 1 0.4021 0.2092 20 3 2 -0.0692 -0.2660 20 3 3 -0.0794 -0.0589 20 3 4 -0.0034 -1.2597 20 3 5 0.0090 -0.6550 20 3 6 -0.1716 -0.0640 20 4 0 2.5890 -0.3983 20 4 1 -0.4375 -0.1871 20 4 2 2.0499 0.6664 20 4 3 0.0935 -0.3894 20 4 4 0.2783 0.0072 20 4 5 1.3046 -0.2285 20 5 0 -0.1412 -0.0911 20 5 1 -0.7018 0.2384 20 5 2 0.7673 0.2135 20 5 3 0.6371 0.2069 20 5 4 0.2596 0.3124 20 6 0 -0.4271 -0.0486 20 6 1 -1.4826 -0.1611 20 6 2 -1.8416 -0.3538 20 7 0 -0.6191 -0.0923 20 7 1 0.3286 -0.7879 21 0 0 -2.2033 0.8360 21 0 2 -4.8055 0.2411 21 1 0 0.3809 1.4329 21 1 1 -0.0069 0.8249 21 1 2 0.0592 0.1106 21 1 3 -0.0994 0.5712 21 2 0 0.0854 -0.4853 21 2 1 0.4194 -0.2378 21 2 2 -0.1769 0.8102 21 3 0 -1.5047 0.4056 21 3 1 0.7204 -0.4060 21 3 2 -0.7219 -0.6382 21 4 0 0.0254 -0.2010 21 4 1 0.8227 0.3326 0 0 0 0.0 0.0 ; _shelx_fab_checksum 2063 _olex2_submission_special_instructions 'No special instructions were received' 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 C1 C 0.2317(2) -0.1337(3) 0.29345(17) 0.0363(10) Uani 1 1 d . . . . . H1 H 0.273285 -0.092660 0.309907 0.044 Uiso 1 1 calc R U . . . C2 C 0.2412(3) -0.2265(3) 0.30167(19) 0.0437(11) Uani 1 1 d . . . . . H2 H 0.289907 -0.247760 0.324612 0.052 Uiso 1 1 calc R U . . . C3 C 0.1189(3) -0.2562(3) 0.24836(18) 0.0380(10) Uani 1 1 d . . . . . H3 H 0.079035 -0.299103 0.231691 0.046 Uiso 1 1 calc R U . . . C4 C 0.1022(2) -0.1645(3) 0.23843(16) 0.0326(9) Uani 1 1 d . . . . . H4 H 0.051699 -0.145651 0.216650 0.039 Uiso 1 1 calc R U . . . C5 C 0.1601(2) -0.1015(2) 0.26070(15) 0.0266(8) Uani 1 1 d . . . . . C6 C 0.1509(2) -0.0011(3) 0.25087(14) 0.0258(8) Uani 1 1 d . . . . . C7 C 0.0125(2) 0.1537(3) 0.18995(15) 0.0280(8) Uani 1 1 d . . . . . H7 H -0.029545 0.110912 0.177645 0.034 Uiso 1 1 calc R U . . . C8 C -0.0040(2) 0.2478(3) 0.17443(14) 0.0269(8) Uani 1 1 d . . . . . C9 C -0.0767(2) 0.2643(3) 0.13683(16) 0.0329(9) Uani 1 1 d . . . . . H9 H -0.108217 0.213646 0.121220 0.040 Uiso 1 1 calc R U . . . C10 C -0.1044(2) 0.3502(3) 0.12146(16) 0.0359(10) Uani 1 1 d . . . . . C11 C -0.0581(2) 0.4230(3) 0.14533(15) 0.0341(9) Uani 1 1 d D . . . . H11 H -0.076850 0.483097 0.136072 0.041 Uiso 1 1 calc R U . . . C12 C 0.0146(2) 0.4111(2) 0.18221(14) 0.0250(8) Uani 1 1 d D . . . . C13 C 0.0433(2) 0.3223(3) 0.19746(14) 0.0239(8) Uani 1 1 d . . . . . C14 C 0.0608(2) 0.4904(3) 0.20922(14) 0.0278(8) Uani 1 1 d . . . . . H14A H 0.114507 0.490760 0.203620 0.033 Uiso 1 1 calc R U . . . H14B H 0.033029 0.547305 0.194654 0.033 Uiso 1 1 calc R U . . . C15 C -0.1843(3) 0.3644(3) 0.0807(2) 0.0547(14) Uani 1 1 d . . . . . H15A H -0.174534 0.384937 0.048683 0.082 Uiso 1 1 calc R U . . . H15B H -0.215574 0.410605 0.092490 0.082 Uiso 1 1 calc R U . . . H15C H -0.214098 0.306940 0.074585 0.082 Uiso 1 1 calc R U . . . C16 C 0.5416(3) 0.1046(4) 0.1684(2) 0.0605(15) Uani 1 1 d . . . . . H16 H 0.532653 0.091685 0.132988 0.073 Uiso 1 1 calc R U . . . C17 C 0.6262(3) 0.1213(3) 0.2477(3) 0.0562(14) Uani 1 1 d . . . . . H17 H 0.679330 0.120888 0.270010 0.067 Uiso 1 1 calc R U . . . C18 C 0.5647(3) 0.1394(4) 0.2691(2) 0.0558(13) Uani 1 1 d . . . . . H18 H 0.575606 0.151993 0.304666 0.067 Uiso 1 1 calc R U . . . C19 C 0.4877(2) 0.1385(3) 0.23745(19) 0.0361(10) Uani 1 1 d . . . . . C20 C 0.4762(3) 0.1223(3) 0.1858(2) 0.0516(13) Uani 1 1 d . . . . . H20 H 0.423840 0.123382 0.162512 0.062 Uiso 1 1 calc R U . . . C21 C 0.4145(2) 0.1525(3) 0.25461(17) 0.0330(9) Uani 1 1 d . . . . . C22 C 0.3558(3) 0.1361(3) 0.36528(17) 0.0360(9) Uani 1 1 d . . . . . H22 H 0.406464 0.116322 0.386388 0.043 Uiso 1 1 calc R U . . . C23 C 0.2909(3) 0.1402(3) 0.38774(16) 0.0325(9) Uani 1 1 d . . . . . C24 C 0.3026(3) 0.1000(3) 0.43681(17) 0.0409(11) Uani 1 1 d . . . . . H24 H 0.353357 0.074224 0.453582 0.049 Uiso 1 1 calc R U . . . C25 C 0.2435(3) 0.0967(3) 0.46104(16) 0.0440(12) Uani 1 1 d . . . . . C26 C 0.1675(3) 0.1348(3) 0.43489(16) 0.0412(11) Uani 1 1 d . . . . . H26 H 0.125118 0.131244 0.450381 0.049 Uiso 1 1 calc R U . . . C27 C 0.1536(3) 0.1769(3) 0.38732(15) 0.0332(9) Uani 1 1 d . . . . . C28 C 0.2173(2) 0.1815(3) 0.36411(14) 0.0277(8) Uani 1 1 d . . . . . C29 C 0.0749(3) 0.2144(3) 0.35843(17) 0.0376(10) Uani 1 1 d . . . . . H29A H 0.055830 0.181968 0.325205 0.045 Uiso 1 1 calc R U . . . H29B H 0.035945 0.202453 0.377991 0.045 Uiso 1 1 calc R U . . . C30 C 0.2571(4) 0.0575(4) 0.51364(19) 0.0646(16) Uani 1 1 d . . . . . H30A H 0.222448 0.004301 0.511861 0.097 Uiso 1 1 calc R U . . . H30B H 0.244563 0.103431 0.536303 0.097 Uiso 1 1 calc R U . . . H30C H 0.313327 0.039005 0.527208 0.097 Uiso 1 1 calc R U . . . C31 C 0.3692(3) 0.2626(4) 0.57306(18) 0.0529(13) Uani 1 1 d . . . . . H31 H 0.414951 0.233820 0.595315 0.063 Uiso 1 1 calc R U . . . C32 C 0.3733(3) 0.2890(3) 0.52463(17) 0.0451(11) Uani 1 1 d . . . . . H32 H 0.420320 0.278827 0.514379 0.054 Uiso 1 1 calc R U . . . C33 C 0.3073(3) 0.3302(3) 0.49224(15) 0.0335(9) Uani 1 1 d . . . . . C34 C 0.2402(3) 0.3445(4) 0.50919(17) 0.0487(12) Uani 1 1 d . . . . . H34 H 0.193838 0.373230 0.487685 0.058 Uiso 1 1 calc R U . . . C35 C 0.2426(4) 0.3158(4) 0.55835(18) 0.0554(14) Uani 1 1 d . . . . . H35 H 0.196737 0.325846 0.569916 0.066 Uiso 1 1 calc R U . . . C36 C 0.2991(2) 0.3563(3) 0.43804(14) 0.0300(8) Uani 1 1 d . . . . . C37 C 0.4113(2) 0.3671(3) 0.35298(16) 0.0311(9) Uani 1 1 d . . . . . H37 H 0.461243 0.356481 0.377917 0.037 Uiso 1 1 calc R U . . . C38 C 0.4114(2) 0.3774(3) 0.30020(16) 0.0291(8) Uani 1 1 d . . . . . C39 C 0.4850(3) 0.3852(3) 0.28907(18) 0.0355(10) Uani 1 1 d . . . . . H39 H 0.533001 0.384136 0.316659 0.043 Uiso 1 1 calc R U . . . C40 C 0.4903(3) 0.3944(3) 0.2400(2) 0.0398(11) Uani 1 1 d . . . . . C41 C 0.4205(3) 0.3978(3) 0.20067(18) 0.0390(11) Uani 1 1 d . . . . . H41 H 0.423308 0.407546 0.166677 0.047 Uiso 1 1 calc R U . . . C42 C 0.3458(3) 0.3875(2) 0.20885(16) 0.0320(9) Uani 1 1 d . . . . . C43 C 0.3403(2) 0.3750(2) 0.25958(15) 0.0241(8) Uani 1 1 d . . . . . C44 C 0.5708(3) 0.3996(4) 0.2296(2) 0.0604(16) Uani 1 1 d . . . . . H44A H 0.564373 0.427003 0.195825 0.091 Uiso 1 1 calc R U . . . H44B H 0.593085 0.338209 0.230346 0.091 Uiso 1 1 calc R U . . . H44C H 0.607239 0.437152 0.256071 0.091 Uiso 1 1 calc R U . . . C45 C 0.1500(7) 0.0453(6) 0.1345(4) 0.090 Uani 0.6792 1 d D U P A 1 H45 H 0.094222 0.045814 0.131130 0.108 Uiso 0.679(7) 1 calc R U P A 1 C47 C 0.2671(3) 0.3848(3) 0.16586(15) 0.0307(9) Uani 1 1 d D . . . . H47A H 0.228427 0.427785 0.173660 0.037 Uiso 1 1 calc R U . . . H47B H 0.276578 0.403795 0.133160 0.037 Uiso 1 1 calc R U . . . C48 C 0.135770 -0.116630 0.094950 0.078 Uani 0.6792 1 d D U P A 1 H48A H 0.126486 -0.118314 0.057666 0.117 Uiso 0.679(7) 1 calc R U P A 1 H48B H 0.084484 -0.122270 0.102806 0.117 Uiso 0.679(7) 1 calc R U P A 1 H48C H 0.170912 -0.167189 0.110828 0.117 Uiso 0.679(7) 1 calc R U P A 1 C46 C 0.262020 -0.048840 0.132720 0.078 Uani 0.6792 1 d D U P A 1 H46A H 0.293220 0.007490 0.141140 0.117 Uiso 0.679(7) 1 d R U P A 1 H46B H 0.276450 -0.080570 0.104930 0.117 Uiso 0.679(7) 1 d R U P A 1 H46C H 0.273660 -0.088150 0.163100 0.117 Uiso 0.679(7) 1 d R U P A 1 N1 N 0.07889(18) 0.0293(2) 0.22880(12) 0.0264(7) Uani 1 1 d . . . . . H1A H 0.034781 -0.005933 0.221751 0.032 Uiso 1 1 d R U . . . N2 N 0.07953(18) 0.12351(19) 0.21910(11) 0.0220(6) Uani 1 1 d . . . . . N11 N 0.1754(5) -0.0264(6) 0.1161(4) 0.0934(18) Uani 0.679(7) 1 d D U P A 1 N3 N 0.1859(2) -0.2877(2) 0.27919(16) 0.0417(9) Uani 1 1 d . . . . . N4 N 0.36230(19) 0.3549(2) 0.42091(12) 0.0294(7) Uani 1 1 d . . . . . H4A H 0.411263 0.343915 0.438329 0.035 Uiso 1 1 d R U . . . N5 N 0.34821(19) 0.3713(2) 0.36865(12) 0.0253(7) Uani 1 1 d . . . . . N6 N 0.3063(3) 0.2747(3) 0.59019(15) 0.0539(11) Uani 1 1 d . . . . . N7 N 0.4212(2) 0.1462(2) 0.30499(15) 0.0372(8) Uani 1 1 d . . . . . H7A H 0.469221 0.122734 0.331127 0.045 Uiso 1 1 d R U . . . N8 N 0.35008(19) 0.1576(2) 0.31815(13) 0.0289(7) Uani 1 1 d . . . . . N9 N 0.6164(2) 0.1048(3) 0.1987(2) 0.0529(12) Uani 1 1 d . . . . . N10 N 0.1009(3) 0.4964(3) 0.41152(16) 0.0548(11) Uani 1 1 d . . . . . O1 O 0.21479(15) 0.04597(17) 0.26358(11) 0.0311(6) Uani 1 1 d . . . . . O2 O 0.11287(14) 0.31325(16) 0.23340(9) 0.0230(5) Uani 1 1 d . . . . . O3 O 0.06966(15) 0.48745(17) 0.26389(10) 0.0276(6) Uani 1 1 d . . . . . O4 O 0.35000(16) 0.1665(2) 0.22223(11) 0.0353(7) Uani 1 1 d . . . . . O5 O 0.20486(15) 0.22908(17) 0.32073(10) 0.0262(6) Uani 1 1 d . . . . . O6 O 0.07634(16) 0.31188(19) 0.34858(11) 0.0343(7) Uani 1 1 d . . . . . O7 O 0.23168(17) 0.3770(2) 0.40963(10) 0.0375(7) Uani 1 1 d . . . . . O8 O 0.26925(14) 0.35766(17) 0.26564(9) 0.0238(5) Uani 1 1 d . . . . . O9 O 0.23490(18) 0.29557(19) 0.16074(11) 0.0349(7) Uani 1 1 d D . . . . H9A H 0.254(2) 0.2700(13) 0.1367(10) 0.052 Uiso 1 1 d D U . . . O10 O 0.11625(19) 0.5012(2) 0.36903(11) 0.0404(7) Uani 1 1 d . . . . . O11 O 0.1186(4) 0.5588(3) 0.44208(18) 0.119(2) Uani 1 1 d . . . . . O12 O 0.0678(2) 0.4244(3) 0.42279(14) 0.0565(9) Uani 1 1 d . . . . . O13 O 0.1866(2) 0.1120(3) 0.15537(13) 0.0563(8) Uani 1 1 d D U . . . O14 O 0.23947(16) 0.54029(18) 0.30991(12) 0.0371(7) Uani 1 1 d . . . . . H14C H 0.226012 0.577137 0.330094 0.056 Uiso 1 1 d R U . . . H14D H 0.290232 0.535747 0.318374 0.056 Uiso 1 1 d R U . . . Pr1 Pr 0.18168(2) 0.39202(2) 0.31605(2) 0.02106(6) Uani 1 1 d . . . . . Pr2 Pr 0.21825(2) 0.20057(2) 0.23698(2) 0.02236(7) Uani 1 1 d D . . . . C45A C 0.2331(9) 0.0423(11) 0.1642(7) 0.082(2) Uani 0.321(7) 1 d D U P A 2 H45A H 0.287523 0.041248 0.184363 0.098 Uiso 0.321(7) 1 calc R U P A 2 N11A N 0.1906(10) -0.0284(9) 0.1397(7) 0.081(3) Uani 0.321(7) 1 d D U P A 2 C48A C 0.1865(16) -0.1292(11) 0.1488(9) 0.117(5) Uani 0.321(7) 1 d D U P A 2 H48D H 0.214205 -0.152327 0.183141 0.175 Uiso 0.321(7) 1 d R U P A 2 H48E H 0.219585 -0.140227 0.125721 0.175 Uiso 0.321(7) 1 d R U P A 2 H48F H 0.135025 -0.160587 0.135661 0.175 Uiso 0.321(7) 1 d R U P A 2 C46A C 0.1193(10) -0.0115(12) 0.0911(5) 0.078(4) Uani 0.321(7) 1 d D U P A 2 H46D H 0.108949 0.054033 0.086851 0.117 Uiso 0.321(7) 1 calc R U P A 2 H46E H 0.071494 -0.042409 0.094931 0.117 Uiso 0.321(7) 1 calc R U P A 2 H46F H 0.132548 -0.035529 0.060929 0.117 Uiso 0.321(7) 1 calc R U 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 C1 0.027(2) 0.031(2) 0.049(3) 0.0030(19) 0.0076(18) 0.0052(17) C2 0.028(2) 0.035(3) 0.066(3) 0.013(2) 0.012(2) 0.0061(19) C3 0.033(2) 0.027(2) 0.056(3) -0.007(2) 0.016(2) -0.0091(18) C4 0.030(2) 0.027(2) 0.040(2) 0.0001(18) 0.0107(17) 0.0035(17) C5 0.0288(19) 0.020(2) 0.032(2) -0.0006(15) 0.0116(16) 0.0012(15) C6 0.0252(18) 0.026(2) 0.0289(19) 0.0009(16) 0.0119(15) 0.0000(15) C7 0.0237(18) 0.027(2) 0.033(2) 0.0014(16) 0.0073(15) -0.0051(16) C8 0.0259(19) 0.025(2) 0.0288(19) 0.0041(16) 0.0058(15) 0.0013(15) C9 0.030(2) 0.028(2) 0.037(2) 0.0029(18) 0.0024(17) -0.0030(17) C10 0.032(2) 0.030(2) 0.037(2) 0.0080(18) -0.0022(17) 0.0015(18) C11 0.032(2) 0.030(2) 0.035(2) 0.0068(18) 0.0024(17) 0.0045(17) C12 0.0285(19) 0.0192(19) 0.0280(19) 0.0038(15) 0.0096(15) 0.0028(15) C13 0.0257(18) 0.026(2) 0.0224(18) 0.0006(15) 0.0116(14) 0.0022(15) C14 0.033(2) 0.024(2) 0.0273(19) 0.0031(16) 0.0093(16) 0.0028(16) C15 0.047(3) 0.034(3) 0.066(3) 0.003(2) -0.011(2) 0.000(2) C16 0.041(3) 0.073(4) 0.078(4) 0.007(3) 0.033(3) 0.013(3) C17 0.025(2) 0.050(3) 0.091(4) 0.001(3) 0.012(2) 0.003(2) C18 0.035(3) 0.056(3) 0.077(4) -0.003(3) 0.017(2) 0.001(2) C19 0.027(2) 0.018(2) 0.067(3) 0.007(2) 0.019(2) 0.0028(16) C20 0.030(2) 0.060(3) 0.069(4) 0.011(3) 0.021(2) 0.010(2) C21 0.027(2) 0.023(2) 0.052(3) 0.0032(18) 0.0148(19) 0.0028(16) C22 0.036(2) 0.025(2) 0.042(2) 0.0032(18) 0.0037(18) 0.0052(18) C23 0.039(2) 0.022(2) 0.034(2) 0.0024(17) 0.0059(18) -0.0012(17) C24 0.057(3) 0.027(2) 0.033(2) 0.0026(18) 0.004(2) 0.001(2) C25 0.079(4) 0.028(2) 0.024(2) 0.0033(17) 0.013(2) -0.006(2) C26 0.062(3) 0.034(2) 0.034(2) 0.0016(19) 0.026(2) -0.015(2) C27 0.042(2) 0.030(2) 0.026(2) 0.0080(17) 0.0064(17) -0.0087(18) C28 0.036(2) 0.022(2) 0.0234(19) 0.0008(15) 0.0060(16) -0.0067(16) C29 0.034(2) 0.041(3) 0.041(2) -0.0001(19) 0.0158(19) -0.0146(19) C30 0.102(5) 0.052(3) 0.034(3) 0.009(2) 0.010(3) -0.014(3) C31 0.064(3) 0.055(3) 0.035(3) 0.009(2) 0.007(2) -0.001(3) C32 0.048(3) 0.055(3) 0.031(2) 0.007(2) 0.009(2) -0.003(2) C33 0.044(2) 0.031(2) 0.025(2) 0.0001(17) 0.0101(17) -0.0031(19) C34 0.060(3) 0.058(3) 0.029(2) 0.006(2) 0.015(2) 0.007(3) C35 0.076(4) 0.066(4) 0.032(3) 0.005(2) 0.028(3) 0.007(3) C36 0.040(2) 0.025(2) 0.0239(19) -0.0019(16) 0.0073(17) -0.0017(17) C37 0.0259(19) 0.031(2) 0.036(2) -0.0052(17) 0.0073(16) -0.0015(16) C38 0.0256(19) 0.024(2) 0.042(2) -0.0062(17) 0.0157(17) -0.0032(15) C39 0.029(2) 0.027(2) 0.055(3) -0.0074(19) 0.0205(19) -0.0066(17) C40 0.039(2) 0.029(2) 0.064(3) -0.009(2) 0.037(2) -0.0070(18) C41 0.059(3) 0.023(2) 0.048(3) -0.0066(19) 0.036(2) -0.0064(19) C42 0.055(3) 0.019(2) 0.030(2) -0.0021(16) 0.0246(19) -0.0027(18) C43 0.0283(19) 0.0133(18) 0.036(2) -0.0018(15) 0.0168(16) -0.0017(14) C44 0.051(3) 0.055(3) 0.095(4) -0.004(3) 0.053(3) -0.007(2) C45 0.090 0.090 0.090 0.000 0.026 0.000 C47 0.049(3) 0.024(2) 0.0232(19) -0.0018(15) 0.0180(18) -0.0027(17) C48 0.078 0.078 0.078 0.000 0.022 0.000 C46 0.078 0.078 0.078 0.000 0.022 0.000 N1 0.0225(15) 0.0215(17) 0.0358(18) 0.0028(13) 0.0092(13) -0.0024(13) N2 0.0240(15) 0.0156(16) 0.0273(16) 0.0028(12) 0.0089(12) -0.0005(12) N11 0.079(2) 0.094(2) 0.107(4) -0.019(3) 0.026(3) -0.0077(19) N3 0.033(2) 0.027(2) 0.070(3) 0.0045(18) 0.0220(19) 0.0001(16) N4 0.0286(17) 0.0331(19) 0.0247(16) -0.0003(14) 0.0047(13) 0.0013(14) N5 0.0282(16) 0.0236(17) 0.0248(16) -0.0015(13) 0.0085(13) -0.0002(13) N6 0.083(3) 0.050(3) 0.027(2) 0.0101(18) 0.014(2) 0.004(2) N7 0.0275(18) 0.032(2) 0.050(2) 0.0026(17) 0.0070(16) 0.0071(15) N8 0.0262(16) 0.0195(17) 0.041(2) -0.0015(14) 0.0092(14) 0.0012(13) N9 0.034(2) 0.034(2) 0.101(4) 0.000(2) 0.035(2) 0.0032(17) N10 0.079(3) 0.052(3) 0.042(2) -0.002(2) 0.033(2) 0.011(2) O1 0.0249(14) 0.0194(14) 0.0468(17) -0.0011(12) 0.0069(12) 0.0018(11) O2 0.0201(12) 0.0218(14) 0.0265(13) 0.0007(10) 0.0056(10) 0.0025(10) O3 0.0277(14) 0.0269(15) 0.0279(14) -0.0029(11) 0.0074(11) 0.0020(11) O4 0.0253(14) 0.0381(17) 0.0453(17) 0.0057(14) 0.0146(13) 0.0053(12) O5 0.0287(13) 0.0233(14) 0.0276(14) 0.0043(11) 0.0099(11) -0.0019(11) O6 0.0285(14) 0.0410(18) 0.0366(16) 0.0011(13) 0.0144(12) -0.0036(12) O7 0.0356(16) 0.054(2) 0.0242(14) 0.0094(13) 0.0113(12) 0.0079(14) O8 0.0241(13) 0.0266(14) 0.0229(13) -0.0005(10) 0.0103(10) -0.0015(11) O9 0.0424(17) 0.0385(18) 0.0255(14) -0.0011(12) 0.0122(12) -0.0022(13) O10 0.0502(18) 0.0440(19) 0.0317(16) 0.0062(13) 0.0195(13) 0.0166(15) O11 0.248(7) 0.065(3) 0.073(3) -0.022(3) 0.091(4) -0.019(4) O12 0.061(2) 0.062(2) 0.058(2) 0.0051(18) 0.0346(19) 0.0025(19) O13 0.0542(19) 0.0817(19) 0.0467(19) -0.0029(14) 0.0363(16) -0.0028(14) O14 0.0215(14) 0.0244(15) 0.067(2) 0.0070(14) 0.0155(13) 0.0005(11) Pr1 0.02089(11) 0.02155(12) 0.02261(11) 0.00068(8) 0.00922(8) 0.00074(7) Pr2 0.02105(11) 0.02024(12) 0.02710(11) -0.00075(8) 0.00900(8) 0.00031(7) C45A 0.073(4) 0.089(3) 0.089(5) -0.009(3) 0.030(4) 0.006(3) N11A 0.074(4) 0.092(3) 0.084(5) -0.012(4) 0.034(4) 0.000(3) C48A 0.114(9) 0.097(4) 0.122(9) -0.002(5) 0.006(8) -0.008(5) C46A 0.068(6) 0.094(8) 0.082(6) -0.014(5) 0.038(4) 0.002(6) 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' 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' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1 120.6 . . ? C2 C1 C5 118.8(4) . . ? C5 C1 H1 120.6 . . ? C1 C2 H2 118.2 . . ? N3 C2 C1 123.6(4) . . ? N3 C2 H2 118.2 . . ? C4 C3 H3 117.8 . . ? N3 C3 H3 117.8 . . ? N3 C3 C4 124.4(4) . . ? C3 C4 H4 120.6 . . ? C5 C4 C3 118.8(4) . . ? C5 C4 H4 120.6 . . ? C1 C5 C6 118.6(3) . . ? C4 C5 C1 117.6(4) . . ? C4 C5 C6 123.8(4) . . ? N1 C6 C5 117.3(3) . . ? O1 C6 C5 116.4(3) . . ? O1 C6 N1 126.2(3) . . ? C8 C7 H7 117.4 . . ? N2 C7 H7 117.4 . . ? N2 C7 C8 125.3(3) . . ? C9 C8 C7 116.1(3) . . ? C9 C8 C13 118.8(4) . . ? C13 C8 C7 124.8(3) . . ? C8 C9 H9 118.4 . . ? C10 C9 C8 123.2(4) . . ? C10 C9 H9 118.4 . . ? C9 C10 C11 117.3(4) . . ? C9 C10 C15 121.1(4) . . ? C11 C10 C15 121.6(4) . . ? C10 C11 H11 118.9 . . ? C12 C11 C10 122.2(4) . . ? C12 C11 H11 118.9 . . ? C11 C12 C13 120.1(4) . . ? C11 C12 C14 120.9(3) . . ? C13 C12 C14 118.8(3) . . ? C8 C13 C12 118.3(3) . . ? O2 C13 C8 123.1(3) . . ? O2 C13 C12 118.6(3) . . ? C12 C14 H14A 109.3 . . ? C12 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? O3 C14 C12 111.5(3) . . ? O3 C14 H14A 109.3 . . ? O3 C14 H14B 109.3 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C20 C16 H16 118.4 . . ? N9 C16 H16 118.4 . . ? N9 C16 C20 123.2(6) . . ? C18 C17 H17 117.7 . . ? N9 C17 H17 117.7 . . ? N9 C17 C18 124.7(5) . . ? C17 C18 H18 120.9 . . ? C19 C18 C17 118.2(5) . . ? C19 C18 H18 120.9 . . ? C18 C19 C20 118.0(4) . . ? C18 C19 C21 125.0(5) . . ? C20 C19 C21 117.0(4) . . ? C16 C20 C19 119.3(5) . . ? C16 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? N7 C21 C19 118.5(4) . . ? O4 C21 C19 119.1(4) . . ? O4 C21 N7 122.4(4) . . ? C23 C22 H22 117.8 . . ? N8 C22 H22 117.8 . . ? N8 C22 C23 124.5(4) . . ? C24 C23 C22 117.8(4) . . ? C28 C23 C22 123.7(4) . . ? C28 C23 C24 118.5(4) . . ? C23 C24 H24 118.6 . . ? C25 C24 C23 122.8(4) . . ? C25 C24 H24 118.6 . . ? C24 C25 C26 117.7(4) . . ? C24 C25 C30 122.5(5) . . ? C26 C25 C30 119.8(5) . . ? C25 C26 H26 119.1 . . ? C27 C26 C25 121.8(4) . . ? C27 C26 H26 119.1 . . ? C26 C27 C28 118.8(4) . . ? C26 C27 C29 123.2(4) . . ? C28 C27 C29 117.9(3) . . ? C23 C28 C27 120.3(4) . . ? O5 C28 C23 121.9(4) . . ? O5 C28 C27 117.8(3) . . ? C27 C29 H29A 108.8 . . ? C27 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? O6 C29 C27 113.6(3) . . ? O6 C29 H29A 108.8 . . ? O6 C29 H29B 108.8 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 H31 117.7 . . ? N6 C31 H31 117.7 . . ? N6 C31 C32 124.6(5) . . ? C31 C32 H32 121.0 . . ? C33 C32 C31 117.9(5) . . ? C33 C32 H32 121.0 . . ? C32 C33 C34 118.9(4) . . ? C32 C33 C36 125.0(4) . . ? C34 C33 C36 116.0(4) . . ? C33 C34 H34 120.7 . . ? C33 C34 C35 118.5(5) . . ? C35 C34 H34 120.7 . . ? C34 C35 H35 118.4 . . ? N6 C35 C34 123.2(5) . . ? N6 C35 H35 118.4 . . ? N4 C36 C33 119.7(4) . . ? O7 C36 C33 118.9(4) . . ? O7 C36 N4 121.4(4) . . ? C38 C37 H37 117.7 . . ? N5 C37 H37 117.7 . . ? N5 C37 C38 124.6(4) . . ? C39 C38 C37 119.0(4) . . ? C43 C38 C37 121.8(3) . . ? C43 C38 C39 119.1(4) . . ? C38 C39 H39 118.7 . . ? C40 C39 C38 122.6(4) . . ? C40 C39 H39 118.7 . . ? C39 C40 C44 120.8(5) . . ? C41 C40 C39 118.1(4) . . ? C41 C40 C44 121.1(5) . . ? C40 C41 H41 118.9 . . ? C40 C41 C42 122.2(4) . . ? C42 C41 H41 118.9 . . ? C41 C42 C43 119.7(4) . . ? C41 C42 C47 123.8(4) . . ? C43 C42 C47 116.4(4) . . ? C38 C43 C42 118.1(3) . . ? O8 C43 C38 123.6(3) . . ? O8 C43 C42 118.2(4) . . ? C40 C44 H44A 109.5 . . ? C40 C44 H44B 109.5 . . ? C40 C44 H44C 109.5 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N11 C45 H45 115.0 . . ? O13 C45 H45 115.0 . . ? O13 C45 N11 130.0(10) . . ? C42 C47 H47A 109.6 . . ? C42 C47 H47B 109.6 . . ? H47A C47 H47B 108.2 . . ? O9 C47 C42 110.1(3) . . ? O9 C47 H47A 109.6 . . ? O9 C47 H47B 109.6 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N11 C48 H48A 109.5 . . ? N11 C48 H48B 109.5 . . ? N11 C48 H48C 109.5 . . ? H46A C46 H46B 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N11 C46 H46A 109.4 . . ? N11 C46 H46B 109.5 . . ? N11 C46 H46C 109.5 . . ? C6 N1 H1A 123.4 . . ? C6 N1 N2 111.3(3) . . ? N2 N1 H1A 125.2 . . ? C7 N2 N1 113.5(3) . . ? C7 N2 Pr2 126.8(2) . . ? N1 N2 Pr2 116.8(2) . . ? C45 N11 C48 133.0(9) . . ? C45 N11 C46 119.5(8) . . ? C46 N11 C48 103.5(5) . . ? C3 N3 C2 116.8(4) . . ? C36 N4 H4A 127.2 . . ? C36 N4 N5 116.1(3) . . ? N5 N4 H4A 116.7 . . ? C37 N5 N4 114.3(3) . . ? C37 N5 Pr1 132.7(3) . . ? N4 N5 Pr1 112.7(2) . . ? C31 N6 C35 116.8(4) . . ? C21 N7 H7A 124.3 . . ? C21 N7 N8 115.4(3) . . ? N8 N7 H7A 119.1 . . ? C22 N8 N7 113.8(3) . . ? C22 N8 Pr2 131.0(3) . . ? N7 N8 Pr2 114.7(2) . . ? C17 N9 C16 116.6(4) . . ? O10 N10 O12 119.6(4) . . ? O11 N10 O10 120.3(5) . . ? O11 N10 O12 120.0(4) . . ? C6 O1 Pr2 122.0(2) . . ? C13 O2 Pr1 135.6(2) . . ? C13 O2 Pr2 127.7(2) . . ? Pr2 O2 Pr1 96.65(8) . . ? C14 O3 Pr1 115.8(2) . . ? C21 O4 Pr2 127.8(3) . . ? C28 O5 Pr1 123.1(2) . . ? C28 O5 Pr2 135.6(2) . . ? Pr2 O5 Pr1 100.54(9) . . ? C29 O6 Pr1 124.8(2) . . ? C36 O7 Pr1 131.1(3) . . ? C43 O8 Pr1 144.2(2) . . ? C43 O8 Pr2 113.5(2) . . ? Pr1 O8 Pr2 98.34(8) . . ? C47 O9 H9A 104.1(15) . . ? C47 O9 Pr2 123.6(2) . . ? Pr2 O9 H9A 120.6(15) . . ? N10 O10 Pr1 135.1(3) . . ? C45 O13 Pr2 142.0(6) . . ? C45A O13 Pr2 106.4(7) . . ? H14C O14 H14D 109.5 . . ? Pr1 O14 H14C 109.3 . . ? Pr1 O14 H14D 109.4 . . ? N5 Pr1 Pr2 83.72(6) . . ? O2 Pr1 N5 123.72(8) . . ? O2 Pr1 O6 83.75(9) . . ? O2 Pr1 O10 127.08(9) . . ? O2 Pr1 Pr2 41.13(5) . . ? O3 Pr1 N5 149.56(9) . . ? O3 Pr1 O2 69.74(8) . . ? O3 Pr1 O6 86.13(9) . . ? O3 Pr1 O10 64.90(8) . . ? O3 Pr1 Pr2 109.51(6) . . ? O5 Pr1 N5 74.86(9) . . ? O5 Pr1 O2 67.73(8) . . ? O5 Pr1 O3 132.63(9) . . ? O5 Pr1 O6 69.57(9) . . ? O5 Pr1 O7 81.52(9) . . ? O5 Pr1 O10 131.78(9) . . ? O5 Pr1 O14 145.47(9) . . ? O5 Pr1 Pr2 39.42(6) . . ? O6 Pr1 N5 120.45(9) . . ? O6 Pr1 O10 67.74(10) . . ? O6 Pr1 Pr2 96.45(6) . . ? O7 Pr1 N5 57.59(9) . . ? O7 Pr1 O2 145.63(9) . . ? O7 Pr1 O3 128.97(9) . . ? O7 Pr1 O6 70.99(9) . . ? O7 Pr1 O10 64.28(9) . . ? O7 Pr1 Pr2 117.73(7) . . ? O8 Pr1 N5 62.56(8) . . ? O8 Pr1 O2 66.81(8) . . ? O8 Pr1 O3 108.58(8) . . ? O8 Pr1 O5 72.32(8) . . ? O8 Pr1 O6 138.45(9) . . ? O8 Pr1 O7 118.90(9) . . ? O8 Pr1 O10 153.78(9) . . ? O8 Pr1 O14 78.64(9) . . ? O8 Pr1 Pr2 42.19(6) . . ? O10 Pr1 N5 109.19(9) . . ? O10 Pr1 Pr2 163.04(7) . . ? O14 Pr1 N5 75.41(9) . . ? O14 Pr1 O2 117.00(9) . . ? O14 Pr1 O3 74.25(9) . . ? O14 Pr1 O6 142.65(9) . . ? O14 Pr1 O7 96.96(10) . . ? O14 Pr1 O10 75.15(10) . . ? O14 Pr1 Pr2 119.84(7) . . ? N2 Pr2 N8 124.61(9) . . ? N2 Pr2 Pr1 97.70(7) . . ? N8 Pr2 Pr1 87.23(7) . . ? O1 Pr2 N2 62.45(9) . . ? O1 Pr2 N8 68.18(9) . . ? O1 Pr2 O2 124.71(9) . . ? O1 Pr2 O4 87.86(9) . . ? O1 Pr2 O5 81.96(9) . . ? O1 Pr2 O8 144.64(9) . . ? O1 Pr2 O9 140.77(9) . . ? O1 Pr2 O13 75.84(11) . . ? O1 Pr2 Pr1 121.47(7) . . ? O2 Pr2 N2 68.83(9) . . ? O2 Pr2 N8 128.82(9) . . ? O2 Pr2 O4 147.43(9) . . ? O2 Pr2 O8 65.63(8) . . ? O2 Pr2 O9 81.91(9) . . ? O2 Pr2 O13 110.18(11) . . ? O2 Pr2 Pr1 42.22(6) . . ? O4 Pr2 N2 137.45(9) . . ? O4 Pr2 N8 59.33(10) . . ? O4 Pr2 O8 88.50(9) . . ? O4 Pr2 O9 70.01(9) . . ? O4 Pr2 O13 74.37(10) . . ? O4 Pr2 Pr1 124.45(7) . . ? O5 Pr2 N2 85.08(9) . . ? O5 Pr2 N8 64.23(9) . . ? O5 Pr2 O2 69.09(8) . . ? O5 Pr2 O4 122.31(9) . . ? O5 Pr2 O8 70.53(8) . . ? O5 Pr2 O9 137.20(9) . . ? O5 Pr2 O13 151.83(10) . . ? O5 Pr2 Pr1 40.04(6) . . ? O8 Pr2 N2 133.48(8) . . ? O8 Pr2 N8 79.82(9) . . ? O8 Pr2 O9 69.04(8) . . ? O8 Pr2 Pr1 39.47(5) . . ? O9 Pr2 N2 113.56(9) . . ? O9 Pr2 N8 120.36(9) . . ? O9 Pr2 Pr1 97.69(6) . . ? O13 Pr2 N2 69.42(10) . . ? O13 Pr2 N8 120.82(11) . . ? O13 Pr2 O8 136.27(10) . . ? O13 Pr2 O9 67.32(10) . . ? O13 Pr2 Pr1 151.84(9) . . ? O13 C45A H45A 126.4 . . ? O13 C45A N11A 107.3(11) . . ? N11A C45A H45A 126.4 . . ? C45A N11A C48A 136.7(14) . . ? C45A N11A C46A 119.6(10) . . ? C48A N11A C46A 103.5(9) . . ? N11A C48A H48D 117.6 . . ? N11A C48A H48E 89.6 . . ? N11A C48A H48F 119.0 . . ? H48D C48A H48E 109.5 . . ? H48D C48A H48F 109.5 . . ? H48E C48A H48F 109.4 . . ? N11A C46A H46D 109.5 . . ? N11A C46A H46E 109.5 . . ? N11A C46A H46F 109.5 . . ? H46D C46A H46E 109.5 . . ? H46D C46A H46F 109.5 . . ? H46E C46A H46F 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 C1 H1 0.9500 . ? C1 C2 1.383(6) . ? C1 C5 1.390(5) . ? C2 H2 0.9500 . ? C2 N3 1.331(6) . ? C3 H3 0.9500 . ? C3 C4 1.387(6) . ? C3 N3 1.310(6) . ? C4 H4 0.9500 . ? C4 C5 1.375(5) . ? C5 C6 1.499(5) . ? C6 N1 1.304(5) . ? C6 O1 1.271(4) . ? C7 H7 0.9500 . ? C7 C8 1.448(5) . ? C7 N2 1.288(5) . ? C8 C9 1.401(5) . ? C8 C13 1.404(5) . ? C9 H9 0.9500 . ? C9 C10 1.372(6) . ? C10 C11 1.383(6) . ? C10 C15 1.524(6) . ? C11 H11 0.9500 . ? C11 C12 1.382(5) . ? C12 C13 1.415(5) . ? C12 C14 1.484(5) . ? C13 O2 1.327(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C14 O3 1.450(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16 0.9500 . ? C16 C20 1.376(6) . ? C16 N9 1.327(7) . ? C17 H17 0.9500 . ? C17 C18 1.382(7) . ? C17 N9 1.317(7) . ? C18 H18 0.9500 . ? C18 C19 1.370(6) . ? C19 C20 1.381(7) . ? C19 C21 1.492(5) . ? C20 H20 0.9500 . ? C21 N7 1.344(5) . ? C21 O4 1.230(5) . ? C22 H22 0.9500 . ? C22 C23 1.432(6) . ? C22 N8 1.296(5) . ? C23 C24 1.419(6) . ? C23 C28 1.397(6) . ? C24 H24 0.9500 . ? C24 C25 1.372(7) . ? C25 C26 1.426(7) . ? C25 C30 1.496(6) . ? C26 H26 0.9500 . ? C26 C27 1.391(5) . ? C27 C28 1.427(6) . ? C27 C29 1.477(6) . ? C28 O5 1.334(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C29 O6 1.458(5) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31 0.9500 . ? C31 C32 1.394(6) . ? C31 N6 1.320(7) . ? C32 H32 0.9500 . ? C32 C33 1.372(6) . ? C33 C34 1.389(6) . ? C33 C36 1.489(5) . ? C34 H34 0.9500 . ? C34 C35 1.391(6) . ? C35 H35 0.9500 . ? C35 N6 1.340(7) . ? C36 N4 1.313(5) . ? C36 O7 1.244(5) . ? C37 H37 0.9500 . ? C37 C38 1.443(6) . ? C37 N5 1.289(5) . ? C38 C39 1.405(5) . ? C38 C43 1.403(5) . ? C39 H39 0.9500 . ? C39 C40 1.372(6) . ? C40 C41 1.369(7) . ? C40 C44 1.509(6) . ? C41 H41 0.9500 . ? C41 C42 1.391(6) . ? C42 C43 1.422(5) . ? C42 C47 1.525(6) . ? C43 O8 1.319(4) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45 0.9500 . ? C45 N11 1.297(2) . ? C45 O13 1.217(10) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C47 O9 1.416(5) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C48 N11 1.527(8) . ? C46 H46A 0.9800 . ? C46 H46B 0.9799 . ? C46 H46C 0.9800 . ? C46 N11 1.483(9) . ? N1 H1A 0.9002 . ? N1 N2 1.409(4) . ? N2 Pr2 2.585(3) . ? N4 H4A 0.8638 . ? N4 N5 1.392(4) . ? N5 Pr1 2.859(3) . ? N7 H7A 0.9906 . ? N7 N8 1.396(4) . ? N8 Pr2 2.763(3) . ? N10 O10 1.261(5) . ? N10 O11 1.216(6) . ? N10 O12 1.282(5) . ? O1 Pr2 2.388(3) . ? O2 Pr1 2.506(2) . ? O2 Pr2 2.452(2) . ? O3 Pr1 2.489(3) . ? O4 Pr2 2.492(3) . ? O5 Pr1 2.423(3) . ? O5 Pr2 2.392(2) . ? O6 Pr1 2.543(3) . ? O7 Pr1 2.452(3) . ? O8 Pr1 2.380(2) . ? O8 Pr2 2.514(3) . ? O9 H9A 0.892(9) . ? O9 Pr2 2.583(3) . ? O10 Pr1 2.624(3) . ? O13 Pr2 2.493(4) . ? O13 C45A 1.283(15) . ? O14 H14C 0.8501 . ? O14 H14D 0.8501 . ? O14 Pr1 2.424(3) . ? Pr1 Pr2 3.7034(3) . ? C45A H45A 0.9500 . ? C45A N11A 1.336(13) . ? N11A C48A 1.505(13) . ? N11A C46A 1.551(13) . ? C48A H48D 0.9801 . ? C48A H48E 0.9802 . ? C48A H48F 0.9802 . ? C46A H46D 0.9800 . ? C46A H46E 0.9800 . ? C46A H46F 0.9800 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 N3 C3 -1.0(7) . . . . ? C1 C5 C6 N1 -166.5(4) . . . . ? C1 C5 C6 O1 15.5(5) . . . . ? C2 C1 C5 C4 0.4(6) . . . . ? C2 C1 C5 C6 -178.5(4) . . . . ? C3 C4 C5 C1 -2.0(6) . . . . ? C3 C4 C5 C6 176.8(4) . . . . ? C4 C3 N3 C2 -0.8(7) . . . . ? C4 C5 C6 N1 14.7(6) . . . . ? C4 C5 C6 O1 -163.3(4) . . . . ? C5 C1 C2 N3 1.2(7) . . . . ? C5 C6 N1 N2 -176.5(3) . . . . ? C5 C6 O1 Pr2 167.8(2) . . . . ? C6 N1 N2 C7 169.1(3) . . . . ? C6 N1 N2 Pr2 6.9(4) . . . . ? C7 C8 C9 C10 173.8(4) . . . . ? C7 C8 C13 C12 -172.6(3) . . . . ? C7 C8 C13 O2 6.2(6) . . . . ? C8 C7 N2 N1 179.0(3) . . . . ? C8 C7 N2 Pr2 -20.8(5) . . . . ? C8 C9 C10 C11 -1.0(6) . . . . ? C8 C9 C10 C15 -179.5(4) . . . . ? C8 C13 O2 Pr1 -138.3(3) . . . . ? C8 C13 O2 Pr2 40.5(5) . . . . ? C9 C8 C13 C12 1.1(5) . . . . ? C9 C8 C13 O2 179.9(3) . . . . ? C9 C10 C11 C12 1.9(6) . . . . ? C10 C11 C12 C13 -1.2(6) . . . . ? C10 C11 C12 C14 -176.6(4) . . . . ? C11 C12 C13 C8 -0.3(5) . . . . ? C11 C12 C13 O2 -179.2(3) . . . . ? C11 C12 C14 O3 117.1(4) . . . . ? C12 C13 O2 Pr1 40.5(5) . . . . ? C12 C13 O2 Pr2 -140.7(3) . . . . ? C12 C14 O3 Pr1 83.5(3) . . . . ? C13 C8 C9 C10 -0.5(6) . . . . ? C13 C12 C14 O3 -58.3(4) . . . . ? C14 C12 C13 C8 175.1(3) . . . . ? C14 C12 C13 O2 -3.8(5) . . . . ? C15 C10 C11 C12 -179.7(4) . . . . ? C17 C18 C19 C20 -1.9(7) . . . . ? C17 C18 C19 C21 177.2(4) . . . . ? C18 C17 N9 C16 -0.8(8) . . . . ? C18 C19 C20 C16 2.3(7) . . . . ? C18 C19 C21 N7 -15.1(6) . . . . ? C18 C19 C21 O4 167.1(4) . . . . ? C19 C21 N7 N8 -178.4(3) . . . . ? C19 C21 O4 Pr2 -176.5(2) . . . . ? C20 C16 N9 C17 1.2(8) . . . . ? C20 C19 C21 N7 164.0(4) . . . . ? C20 C19 C21 O4 -13.9(6) . . . . ? C21 C19 C20 C16 -176.9(4) . . . . ? C21 N7 N8 C22 169.0(4) . . . . ? C21 N7 N8 Pr2 -3.7(4) . . . . ? C22 C23 C24 C25 -177.4(4) . . . . ? C22 C23 C28 C27 175.4(4) . . . . ? C22 C23 C28 O5 -7.2(6) . . . . ? C23 C22 N8 N7 -178.8(4) . . . . ? C23 C22 N8 Pr2 -7.5(6) . . . . ? C23 C24 C25 C26 0.8(7) . . . . ? C23 C24 C25 C30 -177.6(4) . . . . ? C23 C28 O5 Pr1 -113.3(4) . . . . ? C23 C28 O5 Pr2 54.7(5) . . . . ? C24 C23 C28 C27 -4.7(6) . . . . ? C24 C23 C28 O5 172.6(4) . . . . ? C24 C25 C26 C27 -2.3(7) . . . . ? C25 C26 C27 C28 0.4(6) . . . . ? C25 C26 C27 C29 178.0(4) . . . . ? C26 C27 C28 C23 3.2(6) . . . . ? C26 C27 C28 O5 -174.2(4) . . . . ? C26 C27 C29 O6 119.8(4) . . . . ? C27 C28 O5 Pr1 64.1(4) . . . . ? C27 C28 O5 Pr2 -127.9(3) . . . . ? C27 C29 O6 Pr1 45.9(4) . . . . ? C28 C23 C24 C25 2.7(6) . . . . ? C28 C27 C29 O6 -62.6(5) . . . . ? C29 C27 C28 C23 -174.5(4) . . . . ? C29 C27 C28 O5 8.1(6) . . . . ? C30 C25 C26 C27 176.0(4) . . . . ? C31 C32 C33 C34 0.7(7) . . . . ? C31 C32 C33 C36 -175.2(4) . . . . ? C32 C31 N6 C35 -0.4(8) . . . . ? C32 C33 C34 C35 -0.5(7) . . . . ? C32 C33 C36 N4 -11.9(7) . . . . ? C32 C33 C36 O7 166.5(4) . . . . ? C33 C34 C35 N6 -0.2(8) . . . . ? C33 C36 N4 N5 173.7(3) . . . . ? C33 C36 O7 Pr1 -165.0(3) . . . . ? C34 C33 C36 N4 172.1(4) . . . . ? C34 C33 C36 O7 -9.6(6) . . . . ? C34 C35 N6 C31 0.6(8) . . . . ? C36 C33 C34 C35 175.8(4) . . . . ? C36 N4 N5 C37 -178.3(4) . . . . ? C36 N4 N5 Pr1 -3.4(4) . . . . ? C37 C38 C39 C40 179.4(4) . . . . ? C37 C38 C43 C42 178.8(3) . . . . ? C37 C38 C43 O8 -4.4(6) . . . . ? C38 C37 N5 N4 177.0(4) . . . . ? C38 C37 N5 Pr1 3.4(6) . . . . ? C38 C39 C40 C41 1.4(6) . . . . ? C38 C39 C40 C44 -178.1(4) . . . . ? C38 C43 O8 Pr1 45.6(6) . . . . ? C38 C43 O8 Pr2 -105.2(3) . . . . ? C39 C38 C43 C42 -4.7(5) . . . . ? C39 C38 C43 O8 172.2(3) . . . . ? C39 C40 C41 C42 -3.5(6) . . . . ? C40 C41 C42 C43 1.4(6) . . . . ? C40 C41 C42 C47 -175.9(4) . . . . ? C41 C42 C43 C38 2.7(5) . . . . ? C41 C42 C43 O8 -174.3(3) . . . . ? C41 C42 C47 O9 109.2(4) . . . . ? C42 C43 O8 Pr1 -137.6(3) . . . . ? C42 C43 O8 Pr2 71.7(3) . . . . ? C42 C47 O9 Pr2 49.6(4) . . . . ? C43 C38 C39 C40 2.7(6) . . . . ? C43 C42 C47 O9 -68.2(4) . . . . ? C44 C40 C41 C42 176.0(4) . . . . ? C47 C42 C43 C38 -179.8(3) . . . . ? C47 C42 C43 O8 3.2(5) . . . . ? N1 C6 O1 Pr2 -9.9(5) . . . . ? N2 C7 C8 C9 171.2(4) . . . . ? N2 C7 C8 C13 -14.9(6) . . . . ? N11 C45 O13 Pr2 -121.7(11) . . . . ? N3 C3 C4 C5 2.3(6) . . . . ? N4 C36 O7 Pr1 13.4(6) . . . . ? N5 C37 C38 C39 170.4(4) . . . . ? N5 C37 C38 C43 -13.0(6) . . . . ? N6 C31 C32 C33 -0.3(8) . . . . ? N7 C21 O4 Pr2 5.8(6) . . . . ? N8 C22 C23 C24 169.4(4) . . . . ? N8 C22 C23 C28 -10.7(7) . . . . ? N9 C16 C20 C19 -2.0(8) . . . . ? N9 C17 C18 C19 1.2(8) . . . . ? O1 C6 N1 N2 1.3(5) . . . . ? O4 C21 N7 N8 -0.6(6) . . . . ? O7 C36 N4 N5 -4.6(6) . . . . ? O11 N10 O10 Pr1 132.7(5) . . . . ? O12 N10 O10 Pr1 -46.0(7) . . . . ? O13 C45 N11 C48 172.0(9) . . . . ? O13 C45 N11 C46 18.8(19) . . . . ? O13 C45A N11A C48A -146(3) . . . . ? O13 C45A N11A C46A 27(2) . . . . ? Pr2 O13 C45A N11A 141.2(13) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.191 -0.510 0.000 1081.8 12.0 ? 2 -0.199 0.205 0.500 1081.8 12.0 ?