#------------------------------------------------------------------------------ #$Date: 2021-10-15 03:39:09 +0300 (Fri, 15 Oct 2021) $ #$Revision: 269964 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/10/7061022.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_7061022 loop_ _publ_author_name 'Asad, Muhammad' 'Wang, Shan' 'Wang, Qian-You' 'Li, Linke' 'Anwar , Muhammad Imran' 'Younas, Ayesha' 'Zang, Shuang-Quan' _publ_section_title ; Aqueous media ultra-sensitive detection of antibiotics via highly stable luminescent 3D Cadmium-based MOF ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D1NJ04413C _journal_year 2021 _chemical_formula_moiety 'C84 H56 Cd2 N4 O8, 3(C3 H7 N O)' _chemical_formula_sum 'C93 H77 Cd2 N7 O11' _chemical_formula_weight 1693.41 _space_group_crystal_system monoclinic _space_group_IT_number 13 _space_group_name_Hall '-P 2yc' _space_group_name_H-M_alt 'P 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2021-10-05 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-10-05 deposited with the CCDC. 2021-10-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 104.140(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 14.4126(2) _cell_length_b 20.6834(4) _cell_length_c 16.4770(3) _cell_measurement_reflns_used 8965 _cell_measurement_temperature 200.00(10) _cell_measurement_theta_max 72.2990 _cell_measurement_theta_min 3.4640 _cell_volume 4763.00(15) _computing_cell_refinement 'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 200.00(10) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.968 _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 -36.00 72.00 0.50 1.10 -- 53.30 -57.00-150.00 216 2 \w 78.00 142.00 0.50 1.10 -- 53.30 38.00 120.00 128 3 \w 92.00 121.00 0.50 1.10 -- 53.30 77.00 60.00 58 4 \w 32.00 77.00 0.50 1.10 -- 53.30 77.00 60.00 90 5 \w 6.00 103.00 0.50 3.00 -- 93.00 -30.00 90.00 194 6 \w 70.00 164.00 0.50 3.00 -- 93.00 15.00 60.00 188 7 \w 66.00 112.00 0.50 3.00 -- 93.00 -30.00 -60.00 92 8 \w 95.00 121.00 0.50 3.00 -- 93.00 -82.00 -30.00 52 9 \w 37.00 125.00 0.50 3.00 -- 93.00 -82.00 -90.00 176 10 \w 66.00 92.00 0.50 3.00 -- 93.00 82.00 30.00 52 11 \w 132.00 158.00 0.50 3.00 -- 93.00 82.00 30.00 52 12 \w 7.00 33.00 0.50 3.00 -- 93.00 -82.00 -30.00 52 13 \w 122.00 177.00 0.50 3.00 -- 93.00 61.00 60.00 110 14 \w 7.00 117.00 0.50 3.00 -- 93.00 -61.00 -90.00 220 15 \w 14.00 39.00 0.50 3.00 -- 93.00 -30.00 -60.00 50 ; _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 0.0978918000 _diffrn_orient_matrix_UB_12 -0.0140279000 _diffrn_orient_matrix_UB_13 0.0600894000 _diffrn_orient_matrix_UB_21 -0.0470791000 _diffrn_orient_matrix_UB_22 -0.0003826000 _diffrn_orient_matrix_UB_23 0.0744566000 _diffrn_orient_matrix_UB_31 -0.0184844000 _diffrn_orient_matrix_UB_32 -0.0731929000 _diffrn_orient_matrix_UB_33 -0.0117726000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_unetI/netI 0.0572 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.968 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 31299 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.968 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.775 _diffrn_reflns_theta_min 3.162 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 4.030 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.67182 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.181 _exptl_crystal_description block _exptl_crystal_F_000 1736 _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.131 _refine_diff_density_min -1.067 _refine_diff_density_rms 0.105 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 536 _refine_ls_number_reflns 9196 _refine_ls_number_restraints 95 _refine_ls_restrained_S_all 1.062 _refine_ls_R_factor_all 0.0798 _refine_ls_R_factor_gt 0.0574 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+18.3872P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1524 _refine_ls_wR_factor_ref 0.1627 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6995 _reflns_number_total 9196 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1nj04413c2.cif _cod_data_source_block hy _cod_database_code 7061022 _shelx_shelxl_version_number 2016/4 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.924 _shelx_estimated_absorpt_t_min 0.889 _reflns_odcompleteness_completeness 99.75 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances O6-C46 1.15 with sigma of 0.02 N4-C47 = N4-C46 1.4 with sigma of 0.02 N4-C48 1.4 with sigma of 0.02 C47-C48 2.5 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints C46 \\sim C47 \\sim C48 \\sim N4 \\sim O6: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 Uanis(C45) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C43) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C48) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C47) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Others Fixed Sof: C46(0.5) H46(0.5) C47(0.5) H47A(0.5) H47B(0.5) H47C(0.5) C48(0.5) H48A(0.5) H48B(0.5) H48C(0.5) N4(0.5) O6(0.5) 5.a Aromatic/amide H refined with riding coordinates: C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C23(H23), C24(H24), C26(H26), C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C46(H46) 5.b Idealised Me refined as rotating group: C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,H48B, H48C) ; _shelx_res_file ; TITL hy_a.res in P2/c hy.res created by SHELXL-2016/4 at 16:19:04 on 05-Oct-2021 REM Old TITL HY in P2/c REM SHELXT solution in P2/c REM R1 0.139, Rweak 0.031, Alpha 0.039, Orientation as input REM Formula found by SHELXT: Cd C46 N9 CELL 1.54184 14.4126 20.6834 16.477 90 104.14 90 ZERR 2 0.0002 0.0004 0.0003 0 0.002 0 LATT 1 SYMM -X,+Y,0.5-Z SFAC C H Cd N O UNIT 186 154 4 14 22 DFIX 1.15 O6 C46 DFIX 1.4 N4 C47 N4 C46 DFIX 1.4 N4 C48 DFIX 2.5 C47 C48 SIMU 0.01 0.01 2 C46 > O6 ISOR 0.01 0.02 C45 O5 C44 N3 C43 ISOR 0.01 0.02 C48 O6 C46 N4 C47 ISOR 0.01 0.02 C34 L.S. 10 PLAN 20 SIZE 0.03 0.03 0.02 BOND $H list 4 MORE -1 CONF ABIN fmap 2 acta OMIT -3 2 1 OMIT 0 1 0 OMIT -2 2 1 OMIT -3 3 1 OMIT -2 3 1 OMIT 1 24 2 OMIT 0 0 2 OMIT 1 23 6 OMIT 1 23 5 OMIT 0 23 3 OMIT 2 24 4 OMIT 3 23 5 OMIT 1 22 6 OMIT 0 1 2 OMIT 1 22 7 OMIT 2 23 6 REM REM REM WGHT 0.063800 18.387199 FVAR 0.19471 C1 1 0.254220 0.827132 0.301371 11.00000 0.02325 0.03321 = 0.03395 0.00079 0.00622 -0.00081 C2 1 0.360512 0.834950 0.323268 11.00000 0.02136 0.03100 = 0.03692 0.00405 0.00527 0.00076 C3 1 0.956285 0.843852 0.714992 11.00000 0.02844 0.05083 = 0.02884 -0.00312 -0.00274 -0.00211 C4 1 0.791428 0.844087 0.581242 11.00000 0.02835 0.05143 = 0.02497 -0.00063 0.00147 0.00386 C5 1 0.704473 0.843815 0.509703 11.00000 0.02547 0.04395 = 0.02881 0.00040 -0.00186 0.00012 C6 1 0.053352 0.817188 0.260887 11.00000 0.02124 0.05394 = 0.03844 -0.00103 0.00638 -0.00026 C7 1 0.627193 -0.021002 0.317154 11.00000 0.04903 0.03498 = 0.04510 -0.00637 0.02067 -0.00369 AFIX 43 H7 2 0.663299 -0.047150 0.290657 11.00000 -1.20000 AFIX 0 C8 1 0.516473 -0.009322 0.394039 11.00000 0.04309 0.04631 = 0.04219 -0.00367 0.01856 -0.00266 AFIX 43 H8 2 0.474158 -0.027772 0.421890 11.00000 -1.20000 AFIX 0 C9 1 0.522835 0.056616 0.393456 11.00000 0.05682 0.02538 = 0.04820 -0.00783 0.02265 0.00256 AFIX 43 H9 2 0.485739 0.081594 0.420349 11.00000 -1.20000 AFIX 0 C10 1 0.585544 0.086255 0.352118 11.00000 0.05659 0.02361 = 0.03483 0.00065 0.01135 -0.00210 C11 1 0.866483 0.857776 0.728313 11.00000 0.03461 0.07371 = 0.02664 -0.00224 0.00296 -0.00055 AFIX 43 H11 2 0.860916 0.867380 0.782061 11.00000 -1.20000 AFIX 0 C12 1 0.784857 0.857494 0.662073 11.00000 0.02502 0.06617 = 0.03393 -0.00734 0.00386 0.00225 AFIX 43 H12 2 0.725471 0.866388 0.672268 11.00000 -1.20000 AFIX 0 C13 1 0.567881 0.271007 0.381998 11.00000 0.09916 0.02950 = 0.04303 0.00305 0.02942 0.00161 C14 1 0.962402 0.830557 0.633640 11.00000 0.02612 0.08273 = 0.03743 -0.01120 -0.00056 0.00953 AFIX 43 H14 2 1.021585 0.821410 0.623181 11.00000 -1.20000 AFIX 0 C15 1 0.201544 0.832646 0.219939 11.00000 0.02673 0.10529 = 0.03154 0.00000 0.00929 -0.00626 AFIX 43 H15 2 0.232879 0.839160 0.177518 11.00000 -1.20000 AFIX 0 C16 1 0.637926 0.045303 0.313484 11.00000 0.05865 0.03560 = 0.04606 -0.00402 0.02639 -0.00908 AFIX 43 H16 2 0.680477 0.062554 0.284971 11.00000 -1.20000 AFIX 0 C17 1 0.106927 0.809290 0.342183 11.00000 0.02698 0.12028 = 0.03761 0.01126 0.00994 -0.00741 AFIX 43 H17 2 0.075842 0.800199 0.384124 11.00000 -1.20000 AFIX 0 C18 1 0.880714 0.830825 0.567759 11.00000 0.03333 0.07958 = 0.02677 -0.00991 0.00096 0.00539 AFIX 43 H18 2 0.886188 0.821950 0.513792 11.00000 -1.20000 AFIX 0 C19 1 0.596048 0.156245 0.346526 11.00000 0.06898 0.03720 = 0.04345 0.00172 0.02394 -0.00324 AFIX 43 H19 2 0.630493 0.171378 0.309488 11.00000 -1.20000 AFIX 0 C20 1 0.482338 0.307067 0.363978 11.00000 0.09674 0.02725 = 0.05186 0.00756 0.03436 0.00894 C21 1 0.206180 0.814602 0.362829 11.00000 0.02846 0.10963 = 0.03300 0.01301 0.00340 0.00044 AFIX 43 H21 2 0.240368 0.809710 0.418167 11.00000 -1.20000 AFIX 0 C22 1 0.485455 0.376214 0.355884 11.00000 0.09813 0.04532 = 0.05169 0.00812 0.03617 0.01013 C23 1 0.561092 0.199879 0.389261 11.00000 0.07871 0.03988 = 0.04477 0.00511 0.02645 0.00049 AFIX 43 H23 2 0.528933 0.184455 0.427851 11.00000 -1.20000 AFIX 0 C24 1 0.102635 0.828664 0.200046 11.00000 0.02453 0.11988 = 0.02982 0.00007 0.00424 -0.00388 AFIX 43 H24 2 0.068672 0.833807 0.144683 11.00000 -1.20000 AFIX 0 C25 1 0.574195 0.408115 0.366911 11.00000 0.10933 0.03559 = 0.06332 0.00766 0.03139 0.00478 C26 1 0.497141 0.699379 0.417905 11.00000 0.09103 0.04584 = 0.04530 0.00633 0.02663 0.00570 AFIX 43 H26 2 0.460728 0.725049 0.444671 11.00000 -1.20000 AFIX 0 C27 1 0.656329 0.302359 0.392456 11.00000 0.09613 0.03868 = 0.05580 0.00633 0.02520 0.00401 C28 1 0.658775 0.371427 0.383819 11.00000 0.11144 0.02938 = 0.07632 0.00524 0.02714 -0.00518 C29 1 0.392099 0.275838 0.351987 11.00000 0.09481 0.04387 = 0.07300 0.00312 0.03940 0.00631 AFIX 43 H29 2 0.389750 0.231188 0.357831 11.00000 -1.20000 AFIX 0 C30 1 0.545148 0.592997 0.387022 11.00000 0.13153 0.02574 = 0.06865 0.01079 0.03602 -0.00203 C31 1 0.600633 0.689881 0.333732 11.00000 0.09583 0.05517 = 0.10496 0.02258 0.05912 0.02583 AFIX 43 H31 2 0.637298 0.709168 0.301165 11.00000 -1.20000 AFIX 0 C32 1 0.395210 0.408869 0.333383 11.00000 0.11846 0.04456 = 0.08703 0.01264 0.05526 0.01084 AFIX 43 H32 2 0.394716 0.453481 0.326248 11.00000 -1.20000 AFIX 0 C33 1 0.746061 0.268523 0.414012 11.00000 0.09812 0.03550 = 0.07427 0.00234 0.01118 0.00180 AFIX 43 H33 2 0.746107 0.223965 0.421585 11.00000 -1.20000 AFIX 0 C34 1 0.600157 0.623849 0.338401 11.00000 0.11470 0.02674 = 0.11797 0.01198 0.05483 0.01796 AFIX 43 H34 2 0.635940 0.599432 0.309647 11.00000 -1.20000 AFIX 0 C35 1 0.492441 0.633004 0.426211 11.00000 0.13341 0.02511 = 0.06060 0.00014 0.04350 -0.01017 AFIX 43 H35 2 0.453843 0.615210 0.458150 11.00000 -1.20000 AFIX 0 C36 1 0.539990 0.522039 0.395361 11.00000 0.15537 0.04545 = 0.07316 0.00988 0.05228 0.01334 AFIX 43 H36 2 0.503790 0.506408 0.430730 11.00000 -1.20000 AFIX 0 C37 1 0.581334 0.479252 0.357876 11.00000 0.11942 0.04465 = 0.08397 0.01268 0.04177 0.00963 AFIX 43 H37 2 0.618141 0.494455 0.322765 11.00000 -1.20000 AFIX 0 C38 1 0.311455 0.377835 0.322180 11.00000 0.11139 0.05498 = 0.12361 0.01987 0.05827 0.02460 AFIX 43 H38 2 0.254456 0.400970 0.307776 11.00000 -1.20000 AFIX 0 C39 1 0.309489 0.310074 0.332186 11.00000 0.09899 0.06441 = 0.10604 0.00851 0.04916 0.00779 AFIX 43 H39 2 0.251182 0.288841 0.325146 11.00000 -1.20000 AFIX 0 C40 1 0.829612 0.299468 0.423481 11.00000 0.08486 0.05808 = 0.13241 -0.00083 0.01185 0.00538 AFIX 43 H40 2 0.886132 0.275751 0.436629 11.00000 -1.20000 AFIX 0 C41 1 0.834186 0.366911 0.414071 11.00000 0.09459 0.04369 = 0.19629 0.01989 0.01844 -0.00064 AFIX 43 H41 2 0.892918 0.387475 0.420475 11.00000 -1.20000 AFIX 0 C42 1 0.753134 0.400962 0.395836 11.00000 0.12721 0.03192 = 0.14565 0.00740 0.03728 -0.00964 AFIX 43 H42 2 0.756926 0.445587 0.390536 11.00000 -1.20000 AFIX 0 CD1 3 0.557725 0.840083 0.368746 11.00000 0.02045 0.02804 = 0.02689 -0.00008 0.00012 -0.00022 N1 4 0.567422 -0.049460 0.356944 11.00000 0.03036 0.04161 = 0.03029 -0.00370 0.00653 -0.00278 N2 4 0.550961 0.728526 0.373672 11.00000 0.05113 0.04166 = 0.04374 0.00575 0.00922 0.00440 O1 5 0.403901 0.834266 0.264796 11.00000 0.02193 0.04210 = 0.03162 0.00126 0.00664 -0.00115 O2 5 0.404510 0.841695 0.398091 11.00000 0.02716 0.05694 = 0.03053 -0.00405 0.00035 -0.00102 O3 5 0.623816 0.855351 0.522115 11.00000 0.02263 0.05567 = 0.03297 -0.00281 0.00189 0.00130 O4 5 0.716782 0.831880 0.437567 11.00000 0.02772 0.08674 = 0.02473 -0.00932 -0.00034 0.00457 C43 1 0.237856 0.970039 0.454032 11.00000 0.14458 0.12836 = 0.19059 -0.01916 -0.01359 -0.01298 AFIX 137 H43A 2 0.256373 1.009477 0.484392 11.00000 -1.50000 H43B 2 0.247622 0.974142 0.398679 11.00000 -1.50000 H43C 2 0.275928 0.934996 0.482580 11.00000 -1.50000 AFIX 0 C44 1 0.105371 0.916183 0.505171 11.00000 0.15979 0.15425 = 0.13120 0.00601 0.03481 -0.00528 AFIX 43 H44 2 0.039502 0.910753 0.495308 11.00000 -1.20000 AFIX 0 C45 1 0.065774 0.981064 0.375138 11.00000 0.17507 0.13038 = 0.16360 0.03729 -0.02721 0.00275 AFIX 137 H45A 2 0.069625 1.027325 0.372542 11.00000 -1.50000 H45B 2 0.003043 0.968772 0.379769 11.00000 -1.50000 H45C 2 0.077784 0.962623 0.325217 11.00000 -1.50000 AFIX 0 N3 4 0.137744 0.957220 0.448670 11.00000 0.14376 0.11346 = 0.09754 0.00828 0.01789 -0.01319 O5 5 0.151113 0.888964 0.561569 11.00000 0.14107 0.15200 = 0.09706 0.03396 0.02927 -0.00098 C46 1 0.193248 0.549382 0.269173 10.50000 0.09864 0.08297 = 0.12737 0.00989 0.04430 0.00493 AFIX 43 H46 2 0.141230 0.523433 0.244720 10.50000 -1.20000 AFIX 0 C47 1 0.237376 0.640362 0.352934 10.50000 0.12496 0.13478 = 0.14249 -0.00109 0.03830 0.00577 AFIX 137 H47A 2 0.299435 0.621533 0.374263 10.50000 -1.50000 H47B 2 0.216871 0.661018 0.397743 10.50000 -1.50000 H47C 2 0.240640 0.671771 0.310825 10.50000 -1.50000 AFIX 0 C48 1 0.074894 0.602865 0.324816 10.50000 0.13188 0.13453 = 0.14562 -0.00244 0.03538 0.00594 AFIX 137 H48A 2 0.039185 0.624023 0.275092 10.50000 -1.50000 H48B 2 0.072942 0.628601 0.372856 10.50000 -1.50000 H48C 2 0.047341 0.561213 0.329636 10.50000 -1.50000 AFIX 0 N4 4 0.175869 0.594748 0.319957 10.50000 0.10658 0.10614 = 0.12473 0.00040 0.04562 0.00170 O6 5 0.258754 0.538065 0.251967 10.50000 0.09751 0.05425 = 0.13838 0.00636 0.06699 0.00190 HKLF 4 REM hy_a.res in P2/c REM R1 = 0.0574 for 6995 Fo > 4sig(Fo) and 0.0798 for all 9196 data REM 536 parameters refined using 95 restraints END WGHT 0.0639 18.3726 REM Highest difference peak 1.131, deepest hole -1.067, 1-sigma level 0.105 Q1 1 0.5583 0.8807 0.3678 11.00000 0.05 1.13 Q2 1 0.1953 0.5524 0.1916 11.00000 0.05 0.95 Q3 1 0.2122 0.5909 0.3413 11.00000 0.05 0.87 Q4 1 0.5602 0.7946 0.3687 11.00000 0.05 0.81 Q5 1 0.1983 0.6574 0.2803 11.00000 0.05 0.72 Q6 1 0.2792 0.5389 0.2962 11.00000 0.05 0.63 Q7 1 0.1380 0.9884 0.5474 11.00000 0.05 0.63 Q8 1 0.1924 0.8991 0.5112 11.00000 0.05 0.63 Q9 1 0.1205 0.9393 0.5791 11.00000 0.05 0.63 Q10 1 0.6110 0.8391 0.3675 11.00000 0.05 0.57 Q11 1 0.1809 0.6320 0.3905 11.00000 0.05 0.56 Q12 1 0.2000 0.5521 0.3755 11.00000 0.05 0.55 Q13 1 -0.1124 0.9493 0.4320 11.00000 0.05 0.54 Q14 1 0.1756 0.5407 0.3545 11.00000 0.05 0.54 Q15 1 0.2030 0.5408 0.3013 11.00000 0.05 0.51 Q16 1 0.5000 0.8961 0.2500 10.50000 0.05 0.51 Q17 1 0.5000 0.7814 0.2500 10.50000 0.05 0.46 Q18 1 0.5023 0.8592 0.2988 11.00000 0.05 0.45 Q19 1 0.1986 0.7872 0.2214 11.00000 0.05 0.43 Q20 1 0.5736 0.8401 0.4038 11.00000 0.05 0.41 ; _shelx_res_checksum 86869 _shelx_fab_file ; -17 0 2 0.1378 -0.6368 -17 0 4 0.8582 -0.9303 -17 0 6 -0.0433 0.2944 -17 0 8 0.2143 0.6769 -17 1 1 0.2605 0.2189 -17 1 2 -0.2827 0.0944 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0.4466 16 1 3 1.3847 -0.5156 16 2 0 -0.0174 -0.3116 16 2 1 -0.6026 -0.1380 16 2 2 -0.3831 -0.4012 16 2 3 -1.2429 -0.1095 16 3 0 0.3824 -0.1394 16 3 1 0.7042 -0.2216 16 3 2 0.1332 -0.3214 16 3 3 -0.2145 -0.1017 16 4 0 -0.4925 0.2829 16 4 1 0.4968 0.4972 16 4 2 0.1573 0.5240 16 4 3 1.3051 0.1770 16 5 0 -0.0628 0.3109 16 5 2 -0.1945 -0.0630 16 6 0 0.5172 -0.4676 16 6 1 0.1882 -0.2176 16 6 2 0.3274 -0.1010 16 6 3 0.0070 -0.1825 16 7 0 -0.1296 -0.1941 16 7 1 0.8978 -0.0083 16 7 2 -0.4361 -0.1071 16 8 0 -0.5759 0.0717 16 8 1 -0.6489 -0.4623 16 9 0 0.6777 1.1034 17 1 0 -0.1209 0.0396 17 2 0 0.0156 -0.2473 17 3 0 0.0809 -0.3547 17 4 0 -0.2837 0.2406 0 0 0 0.0 0.0 ; _shelx_fab_checksum 31802 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.507 _oxdiff_exptl_absorpt_empirical_full_min 0.493 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, 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 0.2542(3) 0.8271(2) 0.3014(3) 0.0303(11) Uani 1 1 d . . . . . C2 C 0.3605(3) 0.8350(3) 0.3233(3) 0.0301(11) Uani 1 1 d . . . . . C3 C 0.9563(4) 0.8439(3) 0.7150(3) 0.0377(12) Uani 1 1 d . . . . . C4 C 0.7914(4) 0.8441(3) 0.5812(3) 0.0358(12) Uani 1 1 d . . . . . C5 C 0.7045(4) 0.8438(3) 0.5097(3) 0.0342(11) Uani 1 1 d . . . . . C6 C 0.0534(3) 0.8172(3) 0.2609(3) 0.0380(13) Uani 1 1 d . . . . . C7 C 0.6272(4) -0.0210(3) 0.3172(4) 0.0414(13) Uani 1 1 d . . . . . H7 H 0.663299 -0.047150 0.290657 0.050 Uiso 1 1 calc R . . . . C8 C 0.5165(4) -0.0093(3) 0.3940(4) 0.0425(14) Uani 1 1 d . . . . . H8 H 0.474158 -0.027772 0.421890 0.051 Uiso 1 1 calc R . . . . C9 C 0.5228(4) 0.0566(3) 0.3935(4) 0.0418(14) Uani 1 1 d . . . . . H9 H 0.485739 0.081594 0.420349 0.050 Uiso 1 1 calc R . . . . C10 C 0.5855(4) 0.0863(3) 0.3521(3) 0.0383(12) Uani 1 1 d . . . . . C11 C 0.8665(4) 0.8578(3) 0.7283(3) 0.0458(15) Uani 1 1 d . . . . . H11 H 0.860916 0.867380 0.782061 0.055 Uiso 1 1 calc R . . . . C12 C 0.7849(4) 0.8575(3) 0.6621(3) 0.0423(14) Uani 1 1 d . . . . . H12 H 0.725471 0.866388 0.672268 0.051 Uiso 1 1 calc R . . . . C13 C 0.5679(6) 0.2710(3) 0.3820(4) 0.0551(18) Uani 1 1 d . . . . . C14 C 0.9624(4) 0.8306(3) 0.6336(4) 0.0502(17) Uani 1 1 d . . . . . H14 H 1.021585 0.821410 0.623181 0.060 Uiso 1 1 calc R . . . . C15 C 0.2015(4) 0.8326(4) 0.2199(4) 0.0541(18) Uani 1 1 d . . . . . H15 H 0.232879 0.839160 0.177518 0.065 Uiso 1 1 calc R . . . . C16 C 0.6379(5) 0.0453(3) 0.3135(4) 0.0444(14) Uani 1 1 d . . . . . H16 H 0.680477 0.062554 0.284971 0.053 Uiso 1 1 calc R . . . . C17 C 0.1069(4) 0.8093(4) 0.3422(4) 0.061(2) Uani 1 1 d . . . . . H17 H 0.075842 0.800199 0.384124 0.074 Uiso 1 1 calc R . . . . C18 C 0.8807(4) 0.8308(3) 0.5678(3) 0.0477(16) Uani 1 1 d . . . . . H18 H 0.886188 0.821950 0.513792 0.057 Uiso 1 1 calc R . . . . C19 C 0.5960(5) 0.1562(3) 0.3465(4) 0.0481(15) Uani 1 1 d . . . . . H19 H 0.630493 0.171378 0.309488 0.058 Uiso 1 1 calc R . . . . C20 C 0.4823(6) 0.3071(3) 0.3640(4) 0.0558(18) Uani 1 1 d . . . . . C21 C 0.2062(4) 0.8146(4) 0.3628(4) 0.0577(19) Uani 1 1 d . . . . . H21 H 0.240368 0.809710 0.418167 0.069 Uiso 1 1 calc R . . . . C22 C 0.4855(6) 0.3762(4) 0.3559(4) 0.062(2) Uani 1 1 d . . . . . C23 C 0.5611(5) 0.1999(3) 0.3893(4) 0.0525(16) Uani 1 1 d . . . . . H23 H 0.528933 0.184455 0.427851 0.063 Uiso 1 1 calc R . . . . C24 C 0.1026(4) 0.8287(4) 0.2000(4) 0.058(2) Uani 1 1 d . . . . . H24 H 0.068672 0.833807 0.144683 0.070 Uiso 1 1 calc R . . . . C25 C 0.5742(7) 0.4081(4) 0.3669(5) 0.068(2) Uani 1 1 d . . . . . C26 C 0.4971(6) 0.6994(3) 0.4179(4) 0.0590(18) Uani 1 1 d . . . . . H26 H 0.460728 0.725049 0.444671 0.071 Uiso 1 1 calc R . . . . C27 C 0.6563(6) 0.3024(3) 0.3925(4) 0.0624(19) Uani 1 1 d . . . . . C28 C 0.6588(7) 0.3714(4) 0.3838(5) 0.072(2) Uani 1 1 d . . . . . C29 C 0.3921(6) 0.2758(4) 0.3520(5) 0.067(2) Uani 1 1 d . . . . . H29 H 0.389750 0.231188 0.357831 0.081 Uiso 1 1 calc R . . . . C30 C 0.5451(7) 0.5930(3) 0.3870(5) 0.073(2) Uani 1 1 d . . . . . C31 C 0.6006(7) 0.6899(4) 0.3337(6) 0.079(3) Uani 1 1 d . . . . . H31 H 0.637298 0.709168 0.301165 0.095 Uiso 1 1 calc R . . . . C32 C 0.3952(7) 0.4089(4) 0.3334(5) 0.078(3) Uani 1 1 d . . . . . H32 H 0.394716 0.453481 0.326248 0.094 Uiso 1 1 calc R . . . . C33 C 0.7461(7) 0.2685(4) 0.4140(5) 0.071(2) Uani 1 1 d . . . . . H33 H 0.746107 0.223965 0.421585 0.085 Uiso 1 1 calc R . . . . C34 C 0.6002(7) 0.6238(3) 0.3384(6) 0.082(3) Uani 1 1 d . U . . . H34 H 0.635940 0.599432 0.309647 0.098 Uiso 1 1 calc R . . . . C35 C 0.4924(7) 0.6330(3) 0.4262(5) 0.070(2) Uani 1 1 d . . . . . H35 H 0.453843 0.615210 0.458150 0.084 Uiso 1 1 calc R . . . . C36 C 0.5400(8) 0.5220(4) 0.3954(5) 0.087(3) Uani 1 1 d . . . . . H36 H 0.503790 0.506408 0.430730 0.105 Uiso 1 1 calc R . . . . C37 C 0.5813(7) 0.4793(4) 0.3579(5) 0.080(2) Uani 1 1 d . . . . . H37 H 0.618141 0.494455 0.322765 0.096 Uiso 1 1 calc R . . . . C38 C 0.3115(8) 0.3778(4) 0.3222(7) 0.092(3) Uani 1 1 d . . . . . H38 H 0.254456 0.400970 0.307776 0.110 Uiso 1 1 calc R . . . . C39 C 0.3095(7) 0.3101(5) 0.3322(6) 0.086(3) Uani 1 1 d . . . . . H39 H 0.251182 0.288841 0.325146 0.103 Uiso 1 1 calc R . . . . C40 C 0.8296(7) 0.2995(4) 0.4235(7) 0.094(3) Uani 1 1 d . . . . . H40 H 0.886132 0.275751 0.436629 0.113 Uiso 1 1 calc R . . . . C41 C 0.8342(8) 0.3669(5) 0.4141(9) 0.114(4) Uani 1 1 d . . . . . H41 H 0.892918 0.387475 0.420475 0.137 Uiso 1 1 calc R . . . . C42 C 0.7531(8) 0.4010(4) 0.3958(7) 0.101(3) Uani 1 1 d . . . . . H42 H 0.756926 0.445587 0.390536 0.121 Uiso 1 1 calc R . . . . Cd1 Cd 0.55773(2) 0.84008(2) 0.36875(2) 0.02611(12) Uani 1 1 d . . . . . N1 N 0.5674(3) -0.0495(2) 0.3569(3) 0.0342(10) Uani 1 1 d . . . . . N2 N 0.5510(4) 0.7285(2) 0.3737(3) 0.0459(12) Uani 1 1 d . . . . . O1 O 0.4039(2) 0.83427(18) 0.2648(2) 0.0319(8) Uani 1 1 d . . . . . O2 O 0.4045(2) 0.8417(2) 0.3981(2) 0.0394(9) Uani 1 1 d . . . . . O3 O 0.6238(2) 0.85535(19) 0.5221(2) 0.0379(9) Uani 1 1 d . . . . . O4 O 0.7168(3) 0.8319(2) 0.4376(2) 0.0476(11) Uani 1 1 d . . . . . C43 C 0.2379(11) 0.9700(7) 0.4540(10) 0.164(6) Uani 1 1 d . U . . . H43A H 0.256373 1.009477 0.484392 0.246 Uiso 1 1 calc GR . . . . H43B H 0.247622 0.974142 0.398679 0.246 Uiso 1 1 calc GR . . . . H43C H 0.275928 0.934996 0.482580 0.246 Uiso 1 1 calc GR . . . . C44 C 0.1054(12) 0.9162(8) 0.5052(10) 0.149(5) Uani 1 1 d . U . . . H44 H 0.039502 0.910753 0.495308 0.178 Uiso 1 1 calc R . . . . C45 C 0.0658(11) 0.9811(7) 0.3751(9) 0.168(6) Uani 1 1 d . U . . . H45A H 0.069625 1.027325 0.372542 0.252 Uiso 1 1 calc GR . . . . H45B H 0.003043 0.968772 0.379769 0.252 Uiso 1 1 calc GR . . . . H45C H 0.077784 0.962623 0.325217 0.252 Uiso 1 1 calc GR . . . . N3 N 0.1377(9) 0.9572(5) 0.4487(6) 0.120(3) Uani 1 1 d . U . . . O5 O 0.1511(7) 0.8890(5) 0.5616(5) 0.130(3) Uani 1 1 d . U . . . C46 C 0.1932(14) 0.5494(10) 0.2692(14) 0.100(4) Uani 0.5 1 d D U P . . H46 H 0.141230 0.523433 0.244720 0.120 Uiso 0.5 1 calc R . P . . C47 C 0.2374(15) 0.6404(12) 0.3529(17) 0.133(6) Uani 0.5 1 d D U P . . H47A H 0.299435 0.621533 0.374263 0.200 Uiso 0.5 1 calc GR . P . . H47B H 0.216871 0.661018 0.397743 0.200 Uiso 0.5 1 calc GR . P . . H47C H 0.240640 0.671771 0.310825 0.200 Uiso 0.5 1 calc GR . P . . C48 C 0.0749(13) 0.6029(13) 0.3248(17) 0.137(6) Uani 0.5 1 d D U P . . H48A H 0.039185 0.624023 0.275092 0.206 Uiso 0.5 1 calc GR . P . . H48B H 0.072942 0.628601 0.372856 0.206 Uiso 0.5 1 calc GR . P . . H48C H 0.047341 0.561213 0.329636 0.206 Uiso 0.5 1 calc GR . P . . N4 N 0.1759(13) 0.5947(9) 0.3200(12) 0.109(4) Uani 0.5 1 d D U P . . O6 O 0.2588(9) 0.5381(5) 0.2520(9) 0.090(3) Uani 0.5 1 d D U P . . 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 0.023(2) 0.033(3) 0.034(3) 0.001(2) 0.006(2) -0.001(2) C2 0.021(2) 0.031(3) 0.037(3) 0.004(2) 0.0053(19) 0.001(2) C3 0.028(3) 0.051(4) 0.029(3) -0.003(2) -0.003(2) -0.002(3) C4 0.028(3) 0.051(3) 0.025(2) -0.001(2) 0.001(2) 0.004(2) C5 0.025(2) 0.044(3) 0.029(2) 0.000(2) -0.0019(19) 0.000(2) C6 0.021(3) 0.054(4) 0.038(3) -0.001(3) 0.006(2) 0.000(2) C7 0.049(3) 0.035(3) 0.045(3) -0.006(3) 0.021(3) -0.004(3) C8 0.043(3) 0.046(4) 0.042(3) -0.004(3) 0.019(3) -0.003(3) C9 0.057(4) 0.025(3) 0.048(3) -0.008(2) 0.023(3) 0.003(3) C10 0.057(3) 0.024(3) 0.035(3) 0.001(2) 0.011(2) -0.002(2) C11 0.035(3) 0.074(5) 0.027(3) -0.002(3) 0.003(2) -0.001(3) C12 0.025(3) 0.066(4) 0.034(3) -0.007(3) 0.004(2) 0.002(3) C13 0.099(6) 0.030(3) 0.043(3) 0.003(3) 0.029(4) 0.002(4) C14 0.026(3) 0.083(5) 0.037(3) -0.011(3) -0.001(2) 0.010(3) C15 0.027(3) 0.105(6) 0.032(3) 0.000(3) 0.009(2) -0.006(3) C16 0.059(4) 0.036(3) 0.046(3) -0.004(3) 0.026(3) -0.009(3) C17 0.027(3) 0.120(7) 0.038(3) 0.011(4) 0.010(2) -0.007(3) C18 0.033(3) 0.080(5) 0.027(3) -0.010(3) 0.001(2) 0.005(3) C19 0.069(4) 0.037(3) 0.043(3) 0.002(3) 0.024(3) -0.003(3) C20 0.097(6) 0.027(3) 0.052(4) 0.008(3) 0.034(4) 0.009(4) C21 0.028(3) 0.110(6) 0.033(3) 0.013(3) 0.003(2) 0.000(3) C22 0.098(6) 0.045(4) 0.052(4) 0.008(3) 0.036(4) 0.010(4) C23 0.079(5) 0.040(4) 0.045(3) 0.005(3) 0.026(3) 0.000(3) C24 0.025(3) 0.120(7) 0.030(3) 0.000(3) 0.004(2) -0.004(3) C25 0.109(7) 0.036(4) 0.063(5) 0.008(3) 0.031(5) 0.005(4) C26 0.091(5) 0.046(4) 0.045(4) 0.006(3) 0.027(4) 0.006(4) C27 0.096(6) 0.039(4) 0.056(4) 0.006(3) 0.025(4) 0.004(4) C28 0.111(7) 0.029(4) 0.076(5) 0.005(3) 0.027(5) -0.005(4) C29 0.095(6) 0.044(4) 0.073(5) 0.003(4) 0.039(5) 0.006(4) C30 0.132(8) 0.026(4) 0.069(5) 0.011(3) 0.036(5) -0.002(4) C31 0.096(6) 0.055(5) 0.105(7) 0.023(5) 0.059(5) 0.026(5) C32 0.118(8) 0.045(5) 0.087(6) 0.013(4) 0.055(6) 0.011(5) C33 0.098(6) 0.035(4) 0.074(5) 0.002(3) 0.011(5) 0.002(4) C34 0.115(6) 0.027(4) 0.118(6) 0.012(4) 0.055(5) 0.018(4) C35 0.133(7) 0.025(3) 0.061(4) 0.000(3) 0.044(5) -0.010(4) C36 0.155(9) 0.045(5) 0.073(5) 0.010(4) 0.052(6) 0.013(5) C37 0.119(7) 0.045(5) 0.084(6) 0.013(4) 0.042(5) 0.010(5) C38 0.111(8) 0.055(6) 0.124(8) 0.020(5) 0.058(7) 0.025(5) C39 0.099(7) 0.064(6) 0.106(7) 0.009(5) 0.049(6) 0.008(5) C40 0.085(6) 0.058(6) 0.132(9) -0.001(5) 0.012(6) 0.005(5) C41 0.095(7) 0.044(5) 0.196(13) 0.020(7) 0.018(8) -0.001(5) C42 0.127(9) 0.032(5) 0.146(9) 0.007(5) 0.037(7) -0.010(5) Cd1 0.02045(17) 0.0280(2) 0.02689(18) -0.00008(15) 0.00012(11) -0.00022(15) N1 0.030(2) 0.042(3) 0.030(2) -0.0037(19) 0.0065(18) -0.0028(19) N2 0.051(3) 0.042(3) 0.044(3) 0.006(2) 0.009(2) 0.004(2) O1 0.0219(16) 0.042(2) 0.0316(18) 0.0013(16) 0.0066(13) -0.0011(15) O2 0.0272(18) 0.057(3) 0.0305(18) -0.0040(17) 0.0003(14) -0.0010(18) O3 0.0226(17) 0.056(3) 0.0330(19) -0.0028(17) 0.0019(14) 0.0013(16) O4 0.0277(18) 0.087(3) 0.0247(18) -0.0093(19) -0.0003(14) 0.005(2) C43 0.145(11) 0.128(11) 0.191(13) -0.019(10) -0.014(10) -0.013(9) C44 0.160(9) 0.154(9) 0.131(8) 0.006(7) 0.035(7) -0.005(8) C45 0.175(12) 0.130(11) 0.164(12) 0.037(9) -0.027(10) 0.003(9) N3 0.144(7) 0.113(6) 0.098(6) 0.008(5) 0.018(5) -0.013(6) O5 0.141(7) 0.152(7) 0.097(5) 0.034(5) 0.029(5) -0.001(6) C46 0.099(7) 0.083(6) 0.127(7) 0.010(6) 0.044(6) 0.005(6) C47 0.125(10) 0.135(10) 0.142(10) -0.001(9) 0.038(9) 0.006(9) C48 0.132(10) 0.135(10) 0.146(10) -0.002(9) 0.035(9) 0.006(9) N4 0.107(6) 0.106(7) 0.125(7) 0.000(6) 0.046(6) 0.002(6) O6 0.098(7) 0.054(6) 0.138(8) 0.006(6) 0.067(6) 0.002(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _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 C15 C1 C2 121.0(5) . . ? C15 C1 C21 118.3(5) . . ? C21 C1 C2 120.7(5) . . ? C1 C2 Cd1 175.7(4) . . ? O1 C2 C1 118.8(4) . . ? O1 C2 Cd1 62.7(2) . . ? O2 C2 C1 119.6(4) . . ? O2 C2 Cd1 59.1(2) . . ? O2 C2 O1 121.6(4) . . ? C11 C3 C3 121.4(6) . 2_756 ? C14 C3 C3 120.4(6) . 2_756 ? C14 C3 C11 118.2(5) . . ? C12 C4 C5 121.1(5) . . ? C18 C4 C5 120.3(5) . . ? C18 C4 C12 118.5(5) . . ? C4 C5 Cd1 174.1(4) . . ? O3 C5 C4 120.2(5) . . ? O3 C5 Cd1 65.6(3) . . ? O3 C5 O4 122.6(4) . . ? O4 C5 C4 117.2(5) . . ? O4 C5 Cd1 56.9(2) . . ? C17 C6 C6 122.1(6) . 2 ? C17 C6 C24 117.3(5) . . ? C24 C6 C6 120.5(6) . 2 ? C16 C7 H7 118.3 . . ? N1 C7 H7 118.3 . . ? N1 C7 C16 123.3(5) . . ? C9 C8 H8 117.8 . . ? N1 C8 H8 117.8 . . ? N1 C8 C9 124.4(5) . . ? C8 C9 H9 120.2 . . ? C8 C9 C10 119.5(5) . . ? C10 C9 H9 120.2 . . ? C9 C10 C19 123.7(5) . . ? C16 C10 C9 116.4(5) . . ? C16 C10 C19 120.0(5) . . ? C3 C11 H11 119.6 . . ? C3 C11 C12 120.9(5) . . ? C12 C11 H11 119.6 . . ? C4 C12 C11 120.7(5) . . ? C4 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C20 C13 C23 118.1(7) . . ? C27 C13 C20 120.2(6) . . ? C27 C13 C23 121.7(7) . . ? C3 C14 H14 119.7 . . ? C3 C14 C18 120.6(5) . . ? C18 C14 H14 119.7 . . ? C1 C15 H15 119.4 . . ? C1 C15 C24 121.1(5) . . ? C24 C15 H15 119.4 . . ? C7 C16 C10 120.4(5) . . ? C7 C16 H16 119.8 . . ? C10 C16 H16 119.8 . . ? C6 C17 H17 119.2 . . ? C6 C17 C21 121.7(5) . . ? C21 C17 H17 119.2 . . ? C4 C18 C14 121.1(5) . . ? C4 C18 H18 119.4 . . ? C14 C18 H18 119.4 . . ? C10 C19 H19 117.1 . . ? C23 C19 C10 125.9(6) . . ? C23 C19 H19 117.1 . . ? C13 C20 C22 120.0(7) . . ? C13 C20 C29 120.8(6) . . ? C29 C20 C22 119.1(7) . . ? C1 C21 C17 120.3(5) . . ? C1 C21 H21 119.9 . . ? C17 C21 H21 119.9 . . ? C25 C22 C20 120.1(7) . . ? C25 C22 C32 123.4(7) . . ? C32 C22 C20 116.5(8) . . ? C13 C23 H23 116.7 . . ? C19 C23 C13 126.5(6) . . ? C19 C23 H23 116.7 . . ? C6 C24 C15 121.3(5) . . ? C6 C24 H24 119.3 . . ? C15 C24 H24 119.3 . . ? C22 C25 C37 122.2(8) . . ? C28 C25 C22 119.2(7) . . ? C28 C25 C37 118.5(8) . . ? C35 C26 H26 118.2 . . ? N2 C26 H26 118.2 . . ? N2 C26 C35 123.6(7) . . ? C13 C27 C28 119.4(7) . . ? C13 C27 C33 122.8(7) . . ? C33 C27 C28 117.8(8) . . ? C25 C28 C27 121.0(8) . . ? C25 C28 C42 122.4(7) . . ? C27 C28 C42 116.6(8) . . ? C20 C29 H29 119.5 . . ? C39 C29 C20 121.1(8) . . ? C39 C29 H29 119.5 . . ? C34 C30 C36 123.4(8) . . ? C35 C30 C34 116.3(6) . . ? C35 C30 C36 120.3(7) . . ? C34 C31 H31 118.2 . . ? N2 C31 H31 118.2 . . ? N2 C31 C34 123.7(8) . . ? C22 C32 H32 118.6 . . ? C38 C32 C22 122.7(8) . . ? C38 C32 H32 118.6 . . ? C27 C33 H33 119.1 . . ? C40 C33 C27 121.7(8) . . ? C40 C33 H33 119.1 . . ? C30 C34 H34 120.2 . . ? C31 C34 C30 119.7(8) . . ? C31 C34 H34 120.2 . . ? C26 C35 C30 120.1(7) . . ? C26 C35 H35 120.0 . . ? C30 C35 H35 120.0 . . ? C30 C36 H36 116.9 . . ? C37 C36 C30 126.2(9) . . ? C37 C36 H36 116.9 . . ? C25 C37 H37 117.5 . . ? C36 C37 C25 125.0(8) . . ? C36 C37 H37 117.5 . . ? C32 C38 H38 119.9 . . ? C32 C38 C39 120.2(9) . . ? C39 C38 H38 119.9 . . ? C29 C39 C38 120.3(9) . . ? C29 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C33 C40 H40 119.1 . . ? C33 C40 C41 121.8(9) . . ? C41 C40 H40 119.1 . . ? C40 C41 H41 120.5 . . ? C42 C41 C40 119.1(10) . . ? C42 C41 H41 120.5 . . ? C28 C42 H42 118.5 . . ? C41 C42 C28 123.0(8) . . ? C41 C42 H42 118.5 . . ? C5 Cd1 C2 139.80(15) . . ? N1 Cd1 C2 95.46(15) 1_565 . ? N1 Cd1 C5 89.62(16) 1_565 . ? N1 Cd1 N2 176.73(17) 1_565 . ? N1 Cd1 O1 86.56(13) 1_565 2_655 ? N1 Cd1 O1 93.04(14) 1_565 . ? N1 Cd1 O2 94.71(14) 1_565 . ? N1 Cd1 O3 86.78(14) 1_565 . ? N1 Cd1 O4 92.35(16) 1_565 . ? N2 Cd1 C2 85.51(17) . . ? N2 Cd1 C5 91.65(17) . . ? N2 Cd1 O1 86.38(15) . . ? N2 Cd1 O1 90.19(15) . 2_655 ? N2 Cd1 O2 87.57(17) . . ? N2 Cd1 O3 95.73(15) . . ? O1 Cd1 C2 101.65(13) 2_655 . ? O1 Cd1 C2 27.42(13) . . ? O1 Cd1 C5 118.47(14) 2_655 . ? O1 Cd1 C5 167.17(13) . . ? O1 Cd1 O1 74.25(12) 2_655 . ? O1 Cd1 O3 145.01(11) 2_655 . ? O1 Cd1 O3 140.43(11) . . ? O2 Cd1 C2 26.84(13) . . ? O2 Cd1 C5 113.06(14) . . ? O2 Cd1 O1 54.22(11) . . ? O2 Cd1 O1 128.46(11) . 2_655 ? O2 Cd1 O3 86.32(11) . . ? O3 Cd1 C2 113.16(13) . . ? O3 Cd1 C5 27.21(13) . . ? O4 Cd1 C2 165.20(14) . . ? O4 Cd1 C5 27.50(14) . . ? O4 Cd1 N2 87.40(17) . . ? O4 Cd1 O1 91.33(12) . 2_655 ? O4 Cd1 O1 164.25(12) . . ? O4 Cd1 O2 139.89(12) . . ? O4 Cd1 O3 54.70(12) . . ? C7 N1 C8 115.9(5) . . ? C7 N1 Cd1 122.5(4) . 1_545 ? C8 N1 Cd1 121.4(4) . 1_545 ? C26 N2 C31 116.7(6) . . ? C26 N2 Cd1 120.4(4) . . ? C31 N2 Cd1 122.9(5) . . ? C2 O1 Cd1 89.9(3) . . ? C2 O1 Cd1 164.0(3) . 2_655 ? Cd1 O1 Cd1 105.46(12) 2_655 . ? C2 O2 Cd1 94.1(3) . . ? C5 O3 Cd1 87.2(3) . . ? C5 O4 Cd1 95.6(3) . . ? H43A C43 H43B 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N3 C43 H43A 109.5 . . ? N3 C43 H43B 109.5 . . ? N3 C43 H43C 109.5 . . ? N3 C44 H44 116.3 . . ? O5 C44 H44 116.3 . . ? O5 C44 N3 127.5(16) . . ? H45A C45 H45B 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N3 C45 H45A 109.5 . . ? N3 C45 H45B 109.5 . . ? N3 C45 H45C 109.5 . . ? C43 N3 C45 118.6(12) . . ? C44 N3 C43 123.5(13) . . ? C44 N3 C45 117.4(13) . . ? N4 C46 H46 115.3 . . ? O6 C46 H46 115.3 . . ? O6 C46 N4 129(2) . . ? H47A C47 H47B 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N4 C47 H47A 109.5 . . ? N4 C47 H47B 109.5 . . ? N4 C47 H47C 109.5 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N4 C48 H48A 109.5 . . ? N4 C48 H48B 109.5 . . ? N4 C48 H48C 109.5 . . ? C46 N4 C48 117.0(19) . . ? C47 N4 C46 124(2) . . ? C47 N4 C48 117.8(16) . . ? 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 C2 1.494(6) . ? C1 C15 1.376(7) . ? C1 C21 1.384(8) . ? C2 Cd1 2.759(5) . ? C2 O1 1.270(6) . ? C2 O2 1.249(6) . ? C3 C3 1.486(9) 2_756 ? C3 C11 1.395(8) . ? C3 C14 1.392(8) . ? C4 C5 1.496(7) . ? C4 C12 1.386(7) . ? C4 C18 1.386(8) . ? C5 Cd1 2.734(5) . ? C5 O3 1.251(6) . ? C5 O4 1.268(6) . ? C6 C6 1.491(10) 2 ? C6 C17 1.383(8) . ? C6 C24 1.383(8) . ? C7 H7 0.9300 . ? C7 C16 1.383(8) . ? C7 N1 1.340(7) . ? C8 H8 0.9300 . ? C8 C9 1.367(8) . ? C8 N1 1.350(7) . ? C9 H9 0.9300 . ? C9 C10 1.399(8) . ? C10 C16 1.388(8) . ? C10 C19 1.461(8) . ? C11 H11 0.9300 . ? C11 C12 1.396(7) . ? C12 H12 0.9300 . ? C13 C20 1.409(10) . ? C13 C23 1.481(9) . ? C13 C27 1.403(11) . ? C14 H14 0.9300 . ? C14 C18 1.393(7) . ? C15 H15 0.9300 . ? C15 C24 1.385(8) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C17 C21 1.392(8) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C19 C23 1.318(9) . ? C20 C22 1.438(9) . ? C20 C29 1.422(11) . ? C21 H21 0.9300 . ? C22 C25 1.411(11) . ? C22 C32 1.432(12) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C28 1.405(12) . ? C25 C37 1.485(11) . ? C26 H26 0.9300 . ? C26 C35 1.383(10) . ? C26 N2 1.331(8) . ? C27 C28 1.437(10) . ? C27 C33 1.437(11) . ? C28 C42 1.460(13) . ? C29 H29 0.9300 . ? C29 C39 1.355(12) . ? C30 C34 1.410(11) . ? C30 C35 1.385(11) . ? C30 C36 1.478(10) . ? C31 H31 0.9300 . ? C31 C34 1.368(11) . ? C31 N2 1.347(9) . ? C32 H32 0.9300 . ? C32 C38 1.340(13) . ? C33 H33 0.9300 . ? C33 C40 1.339(12) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C36 C37 1.304(11) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C38 C39 1.412(12) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C40 C41 1.407(13) . ? C41 H41 0.9300 . ? C41 C42 1.334(14) . ? C42 H42 0.9300 . ? Cd1 N1 2.300(5) 1_565 ? Cd1 N2 2.312(5) . ? Cd1 O1 2.451(3) . ? Cd1 O1 2.399(3) 2_655 ? Cd1 O2 2.373(4) . ? Cd1 O3 2.493(3) . ? Cd1 O4 2.302(4) . ? N1 Cd1 2.300(5) 1_545 ? O1 Cd1 2.399(3) 2_655 ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C43 N3 1.448(16) . ? C44 H44 0.9300 . ? C44 N3 1.420(17) . ? C44 O5 1.147(16) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C45 N3 1.474(15) . ? C46 H46 0.9300 . ? C46 N4 1.321(16) . ? C46 O6 1.076(15) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C47 N4 1.318(16) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C48 N4 1.486(16) . ? 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 O1 Cd1 -175.4(4) . . . . ? C1 C2 O1 Cd1 20.2(16) . . . 2_655 ? C1 C2 O2 Cd1 175.2(4) . . . . ? C1 C15 C24 C6 -1.9(12) . . . . ? C2 C1 C15 C24 -176.7(6) . . . . ? C2 C1 C21 C17 178.1(7) . . . . ? C3 C3 C11 C12 -179.9(5) 2_756 . . . ? C3 C3 C14 C18 -179.7(5) 2_756 . . . ? C3 C11 C12 C4 -0.8(10) . . . . ? C3 C14 C18 C4 -0.2(11) . . . . ? C4 C5 O3 Cd1 -179.9(5) . . . . ? C4 C5 O4 Cd1 179.8(5) . . . . ? C5 C4 C12 C11 -179.8(6) . . . . ? C5 C4 C18 C14 -179.7(6) . . . . ? C6 C6 C17 C21 -174.7(6) 2 . . . ? C6 C6 C24 C15 176.1(6) 2 . . . ? C6 C17 C21 C1 -1.0(13) . . . . ? C8 C9 C10 C16 0.2(9) . . . . ? C8 C9 C10 C19 178.7(6) . . . . ? C9 C8 N1 C7 -0.3(8) . . . . ? C9 C8 N1 Cd1 176.2(5) . . . 1_545 ? C9 C10 C16 C7 -0.2(9) . . . . ? C9 C10 C19 C23 11.4(11) . . . . ? C10 C19 C23 C13 -177.5(7) . . . . ? C11 C3 C14 C18 -0.4(10) . . . . ? C12 C4 C5 O3 -0.5(9) . . . . ? C12 C4 C5 O4 179.1(6) . . . . ? C12 C4 C18 C14 0.3(10) . . . . ? C13 C20 C22 C25 -0.7(10) . . . . ? C13 C20 C22 C32 177.0(6) . . . . ? C13 C20 C29 C39 -178.0(7) . . . . ? C13 C27 C28 C25 1.4(11) . . . . ? C13 C27 C28 C42 179.7(8) . . . . ? C13 C27 C33 C40 179.8(8) . . . . ? C14 C3 C11 C12 0.9(10) . . . . ? C15 C1 C2 O1 -13.5(8) . . . . ? C15 C1 C2 O2 166.8(6) . . . . ? C15 C1 C21 C17 -1.4(11) . . . . ? C16 C7 N1 C8 0.3(8) . . . . ? C16 C7 N1 Cd1 -176.2(5) . . . 1_545 ? C16 C10 C19 C23 -170.1(7) . . . . ? C17 C6 C24 C15 -0.6(11) . . . . ? C18 C4 C5 O3 179.5(6) . . . . ? C18 C4 C5 O4 -0.9(9) . . . . ? C18 C4 C12 C11 0.2(10) . . . . ? C19 C10 C16 C7 -178.8(6) . . . . ? C20 C13 C23 C19 124.2(8) . . . . ? C20 C13 C27 C28 -0.6(10) . . . . ? C20 C13 C27 C33 177.6(7) . . . . ? C20 C22 C25 C28 1.5(11) . . . . ? C20 C22 C25 C37 179.0(7) . . . . ? C20 C22 C32 C38 1.6(12) . . . . ? C20 C29 C39 C38 0.7(13) . . . . ? C21 C1 C2 O1 167.0(6) . . . . ? C21 C1 C2 O2 -12.8(8) . . . . ? C21 C1 C15 C24 2.8(11) . . . . ? C22 C20 C29 C39 0.8(11) . . . . ? C22 C25 C28 C27 -1.9(11) . . . . ? C22 C25 C28 C42 179.9(8) . . . . ? C22 C25 C37 C36 51.3(14) . . . . ? C22 C32 C38 C39 -0.2(14) . . . . ? C23 C13 C20 C22 -179.6(6) . . . . ? C23 C13 C20 C29 -0.9(9) . . . . ? C23 C13 C27 C28 179.3(6) . . . . ? C23 C13 C27 C33 -2.5(10) . . . . ? C24 C6 C17 C21 2.0(12) . . . . ? C25 C22 C32 C38 179.2(8) . . . . ? C25 C28 C42 C41 178.2(11) . . . . ? C27 C13 C20 C22 0.3(10) . . . . ? C27 C13 C20 C29 179.1(6) . . . . ? C27 C13 C23 C19 -55.7(10) . . . . ? C27 C28 C42 C41 -0.1(16) . . . . ? C27 C33 C40 C41 1.0(16) . . . . ? C28 C25 C37 C36 -131.2(11) . . . . ? C28 C27 C33 C40 -2.0(12) . . . . ? C29 C20 C22 C25 -179.5(7) . . . . ? C29 C20 C22 C32 -1.8(10) . . . . ? C30 C36 C37 C25 -179.5(9) . . . . ? C32 C22 C25 C28 -176.0(7) . . . . ? C32 C22 C25 C37 1.5(12) . . . . ? C32 C38 C39 C29 -0.9(15) . . . . ? C33 C27 C28 C25 -176.8(7) . . . . ? C33 C27 C28 C42 1.5(11) . . . . ? C33 C40 C41 C42 0.5(19) . . . . ? C34 C30 C35 C26 -1.3(13) . . . . ? C34 C30 C36 C37 -2.6(17) . . . . ? C34 C31 N2 C26 -1.8(13) . . . . ? C34 C31 N2 Cd1 177.6(7) . . . . ? C35 C26 N2 C31 1.9(11) . . . . ? C35 C26 N2 Cd1 -177.5(6) . . . . ? C35 C30 C34 C31 1.4(14) . . . . ? C35 C30 C36 C37 175.7(10) . . . . ? C36 C30 C34 C31 179.7(9) . . . . ? C36 C30 C35 C26 -179.7(8) . . . . ? C37 C25 C28 C27 -179.4(7) . . . . ? C37 C25 C28 C42 2.3(12) . . . . ? C40 C41 C42 C28 -0.9(19) . . . . ? Cd1 C2 O1 Cd1 -164.4(13) . . . 2_655 ? N1 C7 C16 C10 0.0(10) . . . . ? N1 C8 C9 C10 0.1(10) . . . . ? N2 C26 C35 C30 -0.3(13) . . . . ? N2 C31 C34 C30 0.2(15) . . . . ? O1 C2 O2 Cd1 -4.5(5) . . . . ? O2 C2 O1 Cd1 4.3(5) . . . . ? O2 C2 O1 Cd1 -160.1(9) . . . 2_655 ? O3 C5 O4 Cd1 -0.5(6) . . . . ? O4 C5 O3 Cd1 0.5(6) . . . . ? O5 C44 N3 C43 1(3) . . . . ? O5 C44 N3 C45 173.2(16) . . . . ? O6 C46 N4 C47 8(4) . . . . ? O6 C46 N4 C48 174(2) . . . . ? 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 0.000 0.500 -0.650 855.1 236.1 ? 2 0.162 0.028 0.656 34.6 0.0 ? 3 0.162 0.972 0.156 34.6 0.0 ? 4 0.838 -0.028 0.344 34.6 0.0 ? 5 0.838 0.028 0.844 34.6 0.0 ?