#------------------------------------------------------------------------------ #$Date: 2016-02-14 04:40:26 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176432 $ #$URL: svn://www.crystallography.net/cod/cif/7/11/21/7112164.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_7112164 loop_ _publ_author_name 'Turner, David R.' 'Hawes, Chris S.' 'Batten, Stuart R.' 'Knowles, Gregory P.' 'Chaffee, Alan L.' 'Nolvachai, Yada' 'Kulsing, Chadin' 'Marriott, Philip J.' _publ_section_title ; Metal-organic frameworks as stationary phases for mixed-mode separation applications ; _journal_name_full Chem.Commun. _journal_page_first 3735 _journal_paper_doi 10.1039/C4CC00933A _journal_volume 50 _journal_year 2014 _chemical_formula_moiety '0.25(C160 H160 Cd8 N16 O32)' _chemical_formula_sum 'C40 H40 Cd2 N4 O8' _chemical_formula_weight 929.56 _chemical_name_systematic ? _space_group_crystal_system orthorhombic _space_group_IT_number 64 _symmetry_space_group_name_Hall '-C 2ac 2' _symmetry_space_group_name_H-M 'C m c a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2014-01-28 _audit_creation_method ; Olex2 1.2 (compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736) ; _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 21.722(4) _cell_length_b 39.084(8) _cell_length_c 17.966(4) _cell_measurement_temperature 273 _cell_volume 15253(5) _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_collection 'BluIce (McPhillips, 2002)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 273.15 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'Phi Scan' _diffrn_radiation_monochromator 'Silicon Double Crystal' _diffrn_radiation_type Synchrotron _diffrn_radiation_wavelength 0.71080 _diffrn_reflns_av_R_equivalents 0.0830 _diffrn_reflns_av_unetI/netI 0.0613 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 28405 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 26.89 _diffrn_reflns_theta_min 1.56 _diffrn_source 'Australian Synchrotron' _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'XScale within XDS' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 0.810 _exptl_crystal_density_method 'not measured' _exptl_crystal_description rod _exptl_crystal_F_000 3744 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _platon_squeeze_details '8 H2O, 5.5 DMF per Cd2, bulk dry material' _refine_diff_density_max 1.738 _refine_diff_density_min -0.946 _refine_diff_density_rms 0.101 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 334 _refine_ls_number_reflns 8251 _refine_ls_number_restraints 51 _refine_ls_restrained_S_all 1.007 _refine_ls_R_factor_all 0.0964 _refine_ls_R_factor_gt 0.0788 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1775P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2379 _refine_ls_wR_factor_ref 0.2524 _reflns_number_gt 5513 _reflns_number_total 8251 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL Cmca1 in Cmca #64 CELL 0.7108 21.722 39.0838 17.966 90 90 90 ZERR 8 0.0043 0.0078 0.0036 0 0 0 LATT 7 SYMM -X,0.5-Y,0.5+Z SYMM +X,-Y,-Z SYMM -X,0.5+Y,0.5-Z SFAC C H Cd N O DISP Cd -0.784 1.197 UNIT 320 320 16 32 64 EQIV $1 1-X,+Y,+Z DFIX 0.97 C22 H22b DFIX 0.97 H22a C22 DFIX 0.97 H32 C32 DFIX 0.97 H15 C15 DFIX 1.25 C37 O38 DFIX 1.25 C37 O39 DFIX 0.8 O39 O38 DANG 1.5 H15 H15_$1 DANG 1.5 H32 H32_$1 ISOR 0.01 0.2 C11 ISOR 0.01 0.2 N6 ISOR 0.01 0.2 N12 ISOR 0.01 0.02 O21 ISOR 0.01 0.02 C17 C18 C20 L.S. 4 PLAN 20 TEMP 0 REM reset to Cmca #64 BOND HTAB BOND $H MORE -2 BOND $H fmap 2 acta 50 CONF OMIT 4 2 3 OMIT 3 1 5 OMIT 1 13 2 REM C:\Users\Chris%20H\Desktop\Papers%20in%20Progress\Cadmium%20MOFs\Chem REM Comm\Revised%20Xray\cmca1-sr.hkl WGHT 0.177500 FVAR 0.92925 CD1 3 0.500000 0.656938 0.537238 10.50000 0.06867 0.07952 = 0.06915 0.00057 0.00000 0.00000 CD2 3 0.000000 0.578761 0.657552 10.50000 0.07864 0.09970 = 0.10166 0.00782 0.00000 0.00000 PART -1 N3 4 0.509803 0.599074 0.504744 10.50000 0.04952 0.08392 = 0.08744 -0.00514 -0.00343 -0.00344 C4 1 0.459983 0.579504 0.549649 10.50000 0.09632 0.10254 = 0.09301 -0.01143 -0.00046 -0.01892 AFIX 23 H4A 2 0.455513 0.556558 0.529796 10.50000 -1.20000 H4B 2 0.472745 0.577642 0.601229 10.50000 -1.20000 AFIX 0 C5 1 0.398567 0.598042 0.545412 10.50000 0.07510 0.11111 = 0.10501 -0.01064 0.02076 -0.02371 AFIX 23 H5A 2 0.384371 0.598005 0.494223 10.50000 -1.20000 H5B 2 0.368540 0.585707 0.575028 10.50000 -1.20000 AFIX 0 N6 4 0.402089 0.633915 0.572259 10.50000 0.06672 0.07299 = 0.07600 -0.01011 0.00556 -0.00104 C7 1 0.402921 0.637380 0.655939 10.50000 0.06448 0.09610 = 0.06717 -0.00410 0.00972 0.00387 AFIX 23 H7A 2 0.429433 0.619822 0.676641 10.50000 -1.20000 H7B 2 0.361679 0.633590 0.674928 10.50000 -1.20000 AFIX 0 C8 1 0.425565 0.672487 0.682093 10.50000 0.12028 0.09606 = 0.08793 -0.00773 0.01744 0.00465 AFIX 23 H8A 2 0.398385 0.690086 0.662875 10.50000 -1.20000 H8B 2 0.424116 0.673446 0.736015 10.50000 -1.20000 AFIX 0 N9 4 0.486605 0.679063 0.657782 10.50000 0.08749 0.07514 = 0.06438 -0.00172 0.00236 -0.00145 C10 1 0.530124 0.660995 0.702521 10.50000 0.07539 0.09987 = 0.08143 -0.00577 -0.00505 -0.00596 AFIX 23 H10A 2 0.516656 0.637463 0.707919 10.50000 -1.20000 H10B 2 0.531176 0.671190 0.751731 10.50000 -1.20000 AFIX 0 C11 1 0.592037 0.661341 0.671269 10.50000 0.07551 0.09446 = 0.07628 0.00421 -0.01658 -0.02553 AFIX 23 H11A 2 0.619866 0.649953 0.705463 10.50000 -1.20000 H11B 2 0.605631 0.684860 0.666064 10.50000 -1.20000 AFIX 0 N12 4 0.595615 0.642968 0.592344 10.50000 0.07192 0.09132 = 0.08577 -0.00459 -0.00723 -0.00799 C13 1 0.594137 0.605980 0.601145 10.50000 0.06593 0.10616 = 0.13616 0.02548 -0.01433 0.00607 AFIX 23 H13A 2 0.566141 0.600014 0.641155 10.50000 -1.20000 H13B 2 0.634850 0.597824 0.614456 10.50000 -1.20000 AFIX 0 C14 1 0.572877 0.588317 0.528024 10.50000 0.07474 0.09935 = 0.11529 -0.00680 0.00343 0.01671 AFIX 23 H14A 2 0.601756 0.593799 0.488609 10.50000 -1.20000 H14B 2 0.573418 0.563711 0.535050 10.50000 -1.20000 AFIX 0 PART 0 C15 1 0.500000 0.595915 0.424029 10.50000 0.09721 0.09619 = 0.10348 -0.01465 0.00000 0.00000 H15 2 0.537063 0.607506 0.414263 11.00000 -1.20000 C16 1 0.500000 0.559660 0.389928 10.50000 0.08517 0.09016 = 0.11069 -0.02330 0.00000 0.00000 C17 1 0.445995 0.545152 0.371561 11.00000 0.11481 0.16455 = 0.19433 -0.07785 0.00798 -0.01614 AFIX 43 H17 2 0.408895 0.556690 0.377677 11.00000 -1.20000 AFIX 0 C18 1 0.448185 0.511068 0.342103 11.00000 0.15093 0.16129 = 0.21278 -0.08042 0.02984 -0.04862 AFIX 43 H18 2 0.412358 0.498041 0.341969 11.00000 -1.20000 AFIX 0 C19 1 0.500000 0.497297 0.314747 10.50000 0.17137 0.09845 = 0.15743 -0.02659 0.00000 0.00000 C20 1 0.500000 0.463388 0.272534 10.50000 0.15255 0.18282 = 0.10965 -0.02684 0.00000 0.00000 O21 5 0.546226 0.450508 0.261768 11.00000 0.30499 0.22413 = 0.23685 -0.07797 -0.06128 0.06381 C22 1 0.352030 0.654474 0.541952 11.00000 0.07124 0.12812 = 0.08662 0.00893 0.00493 0.00607 H22A 2 0.360323 0.648830 0.491578 11.00000 -1.20000 H22B 2 0.354142 0.679343 0.543234 11.00000 -1.20000 C23 1 0.287731 0.642844 0.561045 11.00000 0.06858 0.12793 = 0.08910 -0.00615 0.00220 0.00889 C24 1 0.259003 0.618663 0.518857 11.00000 0.07837 0.19100 = 0.09537 -0.05168 0.01207 -0.00750 AFIX 43 H24 2 0.279006 0.609907 0.477243 11.00000 -1.20000 AFIX 0 C25 1 0.200197 0.606722 0.536667 11.00000 0.08119 0.16609 = 0.10544 -0.03894 0.00729 -0.00235 AFIX 43 H25 2 0.181727 0.589819 0.507879 11.00000 -1.20000 AFIX 0 C26 1 0.169744 0.620232 0.597374 11.00000 0.06757 0.11920 = 0.09286 -0.00884 0.00012 -0.00121 C27 1 0.198115 0.644794 0.640278 11.00000 0.07435 0.12180 = 0.09916 -0.01712 0.01648 0.00621 AFIX 43 H27 2 0.177608 0.653778 0.681300 11.00000 -1.20000 AFIX 0 C28 1 0.257061 0.656385 0.623163 11.00000 0.07193 0.12217 = 0.11438 -0.02180 0.00958 0.00232 AFIX 43 H28 2 0.275903 0.672925 0.652588 11.00000 -1.20000 AFIX 0 C29 1 0.107258 0.607212 0.617646 11.00000 0.07197 0.12083 = 0.09761 0.00092 -0.00132 0.00765 O30 5 0.082389 0.584192 0.577373 11.00000 0.08699 0.16964 = 0.13613 -0.04144 0.00825 -0.01671 O31 5 0.081009 0.618503 0.673798 11.00000 0.09523 0.11912 = 0.11719 -0.01103 0.03154 -0.02190 C32 1 0.500000 0.716065 0.652640 10.50000 0.11988 0.09471 = 0.06398 -0.01242 0.00000 0.00000 H32 2 0.532714 0.732861 0.640340 11.00000 -1.20000 C33 1 0.500000 0.735752 0.727321 10.50000 0.11565 0.09747 = 0.09704 -0.02077 0.00000 0.00000 C34 1 0.554171 0.745657 0.761624 11.00000 0.12734 0.14973 = 0.16932 -0.07846 0.04678 -0.04176 AFIX 43 H34 2 0.591733 0.739180 0.741166 11.00000 -1.20000 AFIX 0 C35 1 0.446876 0.734752 0.326560 11.00000 0.11435 0.21836 = 0.13625 0.10221 -0.01976 -0.05082 AFIX 43 H35 2 0.410009 0.729678 0.350451 11.00000 -1.20000 AFIX 0 C36 1 0.500000 0.723049 0.355361 10.50000 0.11173 0.09196 = 0.07759 0.02218 0.00000 0.00000 C37 1 0.500000 0.700420 0.423699 10.50000 0.12547 0.07821 = 0.07524 0.01687 0.00000 0.00000 PART -1 O38 5 0.545386 0.698989 0.464354 10.50000 0.14421 0.17332 = 0.10380 0.05492 0.02686 0.06945 PART 0 PART -2 O39 5 0.545096 0.683683 0.435098 10.50000 0.12491 0.16779 = 0.11097 0.06070 0.02941 0.05561 HKLF 4 REM Cmca1 in Cmca #64 REM R1 = 0.0788 for 5513 Fo > 4sig(Fo) and 0.0964 for all 8251 data REM 334 parameters refined using 51 restraints END WGHT 0.1775 0.0000 REM Highest difference peak 1.738, deepest hole -0.946, 1-sigma level 0.101 Q1 1 0.0000 0.5181 0.6074 10.50000 0.05 1.74 Q2 1 0.5000 0.4373 0.2762 10.50000 0.05 0.64 Q3 1 0.5365 0.6565 0.6021 11.00000 0.05 0.63 Q4 1 0.5358 0.4740 0.1903 11.00000 0.05 0.45 Q5 1 0.0000 0.6195 0.6555 10.50000 0.05 0.44 Q6 1 0.5380 0.6562 0.4721 11.00000 0.05 0.43 Q7 1 0.5473 0.4692 0.2009 11.00000 0.05 0.43 Q8 1 0.5000 0.6822 0.5775 10.50000 0.05 0.40 Q9 1 0.5000 0.8082 0.4913 10.50000 0.05 0.40 Q10 1 0.5000 0.6341 0.4971 10.50000 0.05 0.39 Q11 1 0.0000 0.5568 0.6972 10.50000 0.05 0.38 Q12 1 0.0000 0.6715 0.5210 10.50000 0.05 0.38 Q13 1 0.0000 0.6051 0.7045 10.50000 0.05 0.37 Q14 1 0.5000 0.6151 0.5384 10.50000 0.05 0.36 Q15 1 0.0729 0.5761 0.6572 11.00000 0.05 0.35 Q16 1 0.0352 0.5770 0.5991 11.00000 0.05 0.34 Q17 1 0.4314 0.6553 0.5389 11.00000 0.05 0.33 Q18 1 0.5000 0.6961 0.5369 10.50000 0.05 0.33 Q19 1 0.4618 0.5564 0.3210 11.00000 0.05 0.33 Q20 1 0.0835 0.5611 0.6322 11.00000 0.05 0.33 REM The information below was added by Olex2. REM REM R1 = 0.0788 for 5513 Fo > 4sig(Fo) and 0.0964 for all 28413 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.74, deepest hole -0.95 REM Mean Shift 0.001, Max Shift 0. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0964 REM R1_gt = 0.0788 REM wR_ref = 0.2524 REM GOOF = 0.983 REM Shift_max = 0 REM Shift_mean = 0.001 REM Reflections_all = 28413 REM Reflections_gt = 5513 REM Parameters = n/a REM Hole = -0.95 REM Peak = 1.74 REM Flack = n/a ; _cod_data_source_file c4cc00933a2.cif _cod_data_source_block 1B _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'multi-Scan' changed to 'multi-scan' according to the built-in table from CIF Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius ; _cod_original_sg_symbol_Hall '-C 2bc 2' _cod_database_code 7112164 #BEGIN Tags that were not found in dictionaries: _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2. Restrained distances C22-H22B 0.97 with sigma of 0.02 H22A-C22 0.97 with sigma of 0.02 H32-C32 0.97 with sigma of 0.02 H15-C15 0.97 with sigma of 0.02 C37-O38 1.25 with sigma of 0.02 C37-O39 1.25 with sigma of 0.02 O39-O38 0.8 with sigma of 0.02 H15-H15_$1 1.5 with sigma of 0.04 H32-H32_$1 1.5 with sigma of 0.04 3. Uiso/Uaniso restraints and constraints Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2 Uanis(N6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2 Uanis(N12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2 Uanis(O21) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Others Fixed Sof: N3(0.5) C4(0.5) H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5) N6(0.5) C7(0.5) H7A(0.5) H7B(0.5) C8(0.5) H8A(0.5) H8B(0.5) N9(0.5) C10(0.5) H10A(0.5) H10B(0.5) C11(0.5) H11A(0.5) H11B(0.5) N12(0.5) C13(0.5) H13A(0.5) H13B(0.5) C14(0.5) H14A(0.5) H14B(0.5) O38(0.5) O39(0.5) 5.a Secondary CH2 refined with riding coordinates: C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C11(H11A, H11B), C13(H13A,H13B), C14(H14A,H14B) 5.b Aromatic/amide H refined with riding coordinates: C17(H17), C18(H18), C24(H24), C25(H25), C27(H27), C28(H28), C34(H34), C35(H35) ; #END Tags that were not found in dictionaries loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y+1/2, z+1/2' 3 'x, -y, -z' 4 '-x, y+1/2, -z+1/2' 5 'x+1/2, y+1/2, z' 6 '-x+1/2, -y+1, z+1/2' 7 'x+1/2, -y+1/2, -z' 8 '-x+1/2, y+1, -z+1/2' 9 '-x, -y, -z' 10 'x, y-1/2, -z-1/2' 11 '-x, y, z' 12 'x, -y-1/2, z-1/2' 13 '-x+1/2, -y+1/2, -z' 14 'x+1/2, y, -z-1/2' 15 '-x+1/2, y+1/2, z' 16 'x+1/2, -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_symmetry_multiplicity _atom_site_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Cd1 Cd 0.5000 0.656938(13) 0.53724(2) 0.0724(2) Uani 1 2 d . . S T Cd2 Cd 0.0000 0.578761(17) 0.65755(4) 0.0933(2) Uani 1 2 d . . S T N3 N 0.5098(6) 0.5991(2) 0.5047(4) 0.074(3) Uani 0.50 1 d A -1 . . C4 C 0.4600(7) 0.5795(4) 0.5496(8) 0.097(3) Uani 0.50 1 d A -1 . . H4A H 0.4555 0.5566 0.5298 0.117 Uiso 0.50 1 calc A -1 R . H4B H 0.4727 0.5776 0.6012 0.117 Uiso 0.50 1 calc A -1 R . C5 C 0.3986(7) 0.5980(4) 0.5454(10) 0.097(4) Uani 0.50 1 d A -1 . . H5A H 0.3844 0.5980 0.4942 0.116 Uiso 0.50 1 calc A -1 R . H5B H 0.3685 0.5857 0.5750 0.116 Uiso 0.50 1 calc A -1 R . N6 N 0.4021(8) 0.6339(4) 0.5723(8) 0.072(3) Uani 0.50 1 d A -1 . U C7 C 0.4029(4) 0.6374(4) 0.6559(6) 0.076(2) Uani 0.50 1 d A -1 . . H7A H 0.4294 0.6198 0.6766 0.091 Uiso 0.50 1 calc A -1 R . H7B H 0.3617 0.6336 0.6749 0.091 Uiso 0.50 1 calc A -1 R . C8 C 0.4256(10) 0.6725(5) 0.6821(13) 0.101(6) Uani 0.50 1 d A -1 . . H8A H 0.3984 0.6901 0.6629 0.122 Uiso 0.50 1 calc A -1 R . H8B H 0.4241 0.6734 0.7360 0.122 Uiso 0.50 1 calc A -1 R . N9 N 0.4866(4) 0.6791(2) 0.6578(4) 0.076(3) Uani 0.50 1 d A -1 . . C10 C 0.5301(5) 0.6610(3) 0.7025(6) 0.086(3) Uani 0.50 1 d A -1 . . H10A H 0.5167 0.6375 0.7079 0.103 Uiso 0.50 1 calc A -1 R . H10B H 0.5312 0.6712 0.7517 0.103 Uiso 0.50 1 calc A -1 R . C11 C 0.5920(8) 0.6613(5) 0.6713(11) 0.082(4) Uani 0.50 1 d A -1 . U H11A H 0.6199 0.6500 0.7055 0.098 Uiso 0.50 1 calc A -1 R . H11B H 0.6056 0.6849 0.6661 0.098 Uiso 0.50 1 calc A -1 R . N12 N 0.5956(9) 0.6430(4) 0.5923(8) 0.083(4) Uani 0.50 1 d . -1 . U C13 C 0.5941(5) 0.6060(4) 0.6011(10) 0.103(4) Uani 0.50 1 d A -1 . . H13A H 0.5661 0.6000 0.6412 0.123 Uiso 0.50 1 calc A -1 R . H13B H 0.6348 0.5978 0.6145 0.123 Uiso 0.50 1 calc A -1 R . C14 C 0.5729(8) 0.5883(4) 0.5280(10) 0.096(4) Uani 0.50 1 d A -1 . . H14A H 0.6018 0.5938 0.4886 0.116 Uiso 0.50 1 calc A -1 R . H14B H 0.5734 0.5637 0.5350 0.116 Uiso 0.50 1 calc A -1 R . C15 C 0.5000 0.5959(2) 0.4240(5) 0.099(2) Uani 1 2 d . . DS T H15 H 0.5371(9) 0.6075(12) 0.414(4) 0.119 Uiso 1 1 d . . DR . C16 C 0.5000 0.5597(2) 0.3899(5) 0.095(2) Uani 1 2 d . . S T C17 C 0.4460(4) 0.5452(3) 0.3716(6) 0.158(3) Uani 1 1 d . . . U H17 H 0.4089 0.5567 0.3777 0.189 Uiso 1 1 calc A . R . C18 C 0.4482(5) 0.5111(3) 0.3421(7) 0.175(4) Uani 1 1 d A . . U H18 H 0.4124 0.4980 0.3420 0.210 Uiso 1 1 calc . . R . C19 C 0.5000 0.4973(3) 0.3147(8) 0.142(4) Uani 1 2 d . . S T C20 C 0.5000 0.4634(5) 0.2725(7) 0.148(4) Uani 1 2 d . . S TU O21 O 0.5462(6) 0.4505(3) 0.2618(6) 0.255(5) Uani 1 1 d . . . U C22 C 0.3520(2) 0.65447(18) 0.5420(3) 0.0953(17) Uani 1 1 d . . D . H22A H 0.360(3) 0.6488(16) 0.4916(16) 0.114 Uiso 1 1 d . . DR . H22B H 0.354(3) 0.6793(6) 0.543(3) 0.114 Uiso 1 1 d . . DR . C23 C 0.2877(2) 0.64284(18) 0.5610(3) 0.0952(15) Uani 1 1 d A . . . C24 C 0.2590(3) 0.6187(2) 0.5189(4) 0.122(3) Uani 1 1 d . . . . H24 H 0.2790 0.6099 0.4772 0.146 Uiso 1 1 calc A . R . C25 C 0.2002(3) 0.6067(2) 0.5367(4) 0.118(2) Uani 1 1 d A . . . H25 H 0.1817 0.5898 0.5079 0.141 Uiso 1 1 calc . . R . C26 C 0.1697(2) 0.62023(16) 0.5974(3) 0.0932(15) Uani 1 1 d . . . . C27 C 0.1981(2) 0.64479(17) 0.6403(3) 0.0984(16) Uani 1 1 d A . . . H27 H 0.1776 0.6538 0.6813 0.118 Uiso 1 1 calc . . R . C28 C 0.2571(2) 0.65639(17) 0.6232(4) 0.1028(17) Uani 1 1 d . . . . H28 H 0.2759 0.6729 0.6526 0.123 Uiso 1 1 calc A . R . C29 C 0.1073(2) 0.60721(18) 0.6176(4) 0.0968(16) Uani 1 1 d A . . . O30 O 0.0824(2) 0.58419(16) 0.5774(3) 0.1309(18) Uani 1 1 d . . . . O31 O 0.08101(19) 0.61850(12) 0.6738(3) 0.1105(13) Uani 1 1 d . . . . C32 C 0.5000 0.7161(2) 0.6526(4) 0.093(2) Uani 1 2 d . . DS T H32 H 0.5327(9) 0.7329(10) 0.640(3) 0.111 Uiso 1 1 d . . DR . C33 C 0.5000 0.7358(2) 0.7273(5) 0.103(2) Uani 1 2 d . . S T C34 C 0.5542(4) 0.7457(2) 0.7616(6) 0.149(3) Uani 1 1 d . . . . H34 H 0.5917 0.7392 0.7412 0.179 Uiso 1 1 calc A . R . C35 C 0.4469(4) 0.7348(3) 0.3266(5) 0.156(4) Uani 1 1 d . . . . H35 H 0.4100 0.7297 0.3505 0.188 Uiso 1 1 calc . . R . C36 C 0.5000 0.7230(2) 0.3554(4) 0.094(2) Uani 1 2 d . . S T C37 C 0.5000 0.7004(2) 0.4237(4) 0.093(2) Uani 1 2 d . . DS T O38 O 0.5454(7) 0.6990(5) 0.4644(8) 0.140(6) Uani 0.50 1 d A -1 D . O39 O 0.5451(7) 0.6837(4) 0.4351(9) 0.135(5) Uani 0.50 1 d A -2 D . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0687(3) 0.0795(4) 0.0691(3) 0.0006(2) 0.000 0.000 Cd2 0.0786(3) 0.0997(5) 0.1017(4) 0.0078(3) 0.000 0.000 N3 0.050(10) 0.084(4) 0.087(4) -0.005(3) -0.003(3) -0.003(3) C4 0.096(9) 0.103(9) 0.093(8) -0.011(7) 0.000(7) -0.019(7) C5 0.075(8) 0.111(11) 0.105(10) -0.011(8) 0.021(7) -0.024(7) N6 0.067(4) 0.073(6) 0.076(6) -0.010(5) 0.006(5) -0.001(5) C7 0.064(4) 0.096(8) 0.067(6) -0.004(5) 0.010(4) 0.004(5) C8 0.120(16) 0.096(12) 0.088(9) -0.008(8) 0.017(10) 0.005(9) N9 0.087(10) 0.075(4) 0.064(3) -0.002(3) 0.002(3) -0.001(4) C10 0.075(5) 0.100(7) 0.081(6) -0.006(6) -0.005(5) -0.006(5) C11 0.076(6) 0.094(9) 0.076(7) 0.004(7) -0.017(5) -0.026(7) N12 0.072(5) 0.091(8) 0.086(8) -0.005(6) -0.007(5) -0.008(6) C13 0.066(5) 0.106(9) 0.136(12) 0.025(10) -0.014(7) 0.006(5) C14 0.075(9) 0.099(10) 0.115(12) -0.007(8) 0.003(8) 0.017(7) C15 0.097(5) 0.096(6) 0.103(6) -0.015(5) 0.000 0.000 C16 0.085(4) 0.090(5) 0.111(6) -0.023(5) 0.000 0.000 C17 0.115(4) 0.165(7) 0.194(7) -0.078(6) 0.008(5) -0.016(5) C18 0.151(6) 0.161(7) 0.213(8) -0.080(6) 0.030(6) -0.049(5) C19 0.171(11) 0.098(7) 0.157(10) -0.027(7) 0.000 0.000 C20 0.153(8) 0.183(9) 0.110(6) -0.027(7) 0.000 0.000 O21 0.305(9) 0.224(8) 0.237(7) -0.078(6) -0.061(7) 0.064(7) C22 0.071(3) 0.128(5) 0.087(3) 0.009(3) 0.005(2) 0.006(3) C23 0.069(2) 0.128(5) 0.089(3) -0.006(3) 0.002(2) 0.009(3) C24 0.078(3) 0.191(8) 0.095(4) -0.052(4) 0.012(3) -0.007(4) C25 0.081(3) 0.166(7) 0.105(4) -0.039(4) 0.007(3) -0.002(4) C26 0.068(2) 0.119(4) 0.093(3) -0.009(3) 0.000(2) -0.001(2) C27 0.074(3) 0.122(5) 0.099(4) -0.017(3) 0.016(2) 0.006(3) C28 0.072(3) 0.122(5) 0.114(4) -0.022(4) 0.010(3) 0.002(3) C29 0.072(3) 0.121(5) 0.098(4) 0.001(3) -0.001(3) 0.008(3) O30 0.087(2) 0.170(5) 0.136(4) -0.041(4) 0.008(2) -0.017(3) O31 0.095(2) 0.119(3) 0.117(3) -0.011(3) 0.032(2) -0.022(2) C32 0.120(6) 0.095(5) 0.064(4) -0.012(4) 0.000 0.000 C33 0.116(6) 0.097(6) 0.097(5) -0.021(5) 0.000 0.000 C34 0.127(5) 0.150(7) 0.169(7) -0.078(6) 0.047(5) -0.042(5) C35 0.114(5) 0.218(10) 0.136(6) 0.102(7) -0.020(4) -0.051(6) C36 0.112(5) 0.092(5) 0.078(4) 0.022(4) 0.000 0.000 C37 0.125(6) 0.078(5) 0.075(4) 0.017(4) 0.000 0.000 O38 0.144(9) 0.173(16) 0.104(10) 0.055(8) 0.027(8) 0.069(10) O39 0.125(8) 0.168(15) 0.111(10) 0.061(9) 0.029(7) 0.056(9) 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' Cd Cd -0.7840 1.1970 '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' 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 N3 Cd1 N3 10.4(7) . 11_655 N3 Cd1 N6 77.5(5) 11_655 11_655 N3 Cd1 N6 67.8(5) . 11_655 N3 Cd1 N6 67.8(5) 11_655 . N3 Cd1 N6 77.5(5) . . N3 Cd1 N9 126.5(3) 11_655 11_655 N3 Cd1 N9 125.0(3) 11_655 . N3 Cd1 N9 126.5(3) . . N3 Cd1 N9 125.0(3) . 11_655 N3 Cd1 N12 78.6(5) 11_655 11_655 N3 Cd1 N12 87.8(5) 11_655 . N3 Cd1 N12 87.8(5) . 11_655 N3 Cd1 N12 78.6(5) . . N6 Cd1 N6 125.4(8) 11_655 . N9 Cd1 N6 90.3(4) . 11_655 N9 Cd1 N6 90.3(4) 11_655 . N9 Cd1 N6 77.6(4) . . N9 Cd1 N6 77.6(4) 11_655 11_655 N9 Cd1 N9 14.2(4) . 11_655 N9 Cd1 N12 65.8(4) 11_655 . N9 Cd1 N12 65.8(4) . 11_655 N9 Cd1 N12 78.9(4) . . N9 Cd1 N12 78.9(4) 11_655 11_655 N12 Cd1 N6 12.2(4) 11_655 . N12 Cd1 N6 125.7(3) . . N12 Cd1 N6 12.2(4) . 11_655 N12 Cd1 N6 125.7(3) 11_655 11_655 N12 Cd1 N12 122.9(8) 11_655 . O38 Cd1 N3 120.3(4) 11_655 11_655 O38 Cd1 N3 125.5(4) . 11_655 O38 Cd1 N3 125.5(4) 11_655 . O38 Cd1 N3 120.2(4) . . O38 Cd1 N6 142.4(5) . . O38 Cd1 N6 142.4(5) 11_655 11_655 O38 Cd1 N6 92.1(5) . 11_655 O38 Cd1 N6 92.1(5) 11_655 . O38 Cd1 N9 108.2(4) 11_655 11_655 O38 Cd1 N9 101.9(4) . 11_655 O38 Cd1 N9 108.2(4) . . O38 Cd1 N9 101.9(4) 11_655 . O38 Cd1 N12 91.5(6) . . O38 Cd1 N12 91.5(6) 11_655 11_655 O38 Cd1 N12 140.6(6) 11_655 . O38 Cd1 N12 140.6(6) . 11_655 O38 Cd1 O38 50.3(7) . 11_655 O38 Cd1 O39 54.3(3) 11_655 . O38 Cd1 O39 54.3(3) . 11_655 O38 Cd1 O39 19.7(4) 11_655 11_655 O38 Cd1 O39 19.7(4) . . O39 Cd1 N3 106.0(4) 11_655 . O39 Cd1 N3 101.5(4) 11_655 11_655 O39 Cd1 N3 101.5(4) . . O39 Cd1 N3 106.0(4) . 11_655 O39 Cd1 N6 90.1(5) . 11_655 O39 Cd1 N6 138.6(5) 11_655 11_655 O39 Cd1 N6 90.1(5) 11_655 . O39 Cd1 N6 138.6(5) . . O39 Cd1 N9 127.8(5) 11_655 11_655 O39 Cd1 N9 127.8(5) . . O39 Cd1 N9 120.6(5) . 11_655 O39 Cd1 N9 120.6(5) 11_655 . O39 Cd1 N12 93.7(5) 11_655 11_655 O39 Cd1 N12 143.4(5) . 11_655 O39 Cd1 N12 143.4(5) 11_655 . O39 Cd1 N12 93.7(5) . . O39 Cd1 O39 49.8(7) 11_655 . C20 Cd2 C29 117.90(15) 6 . C20 Cd2 C29 117.90(15) 6 11 O21 Cd2 C20 25.5(3) 16_466 6 O21 Cd2 C20 25.5(3) 6 6 O21 Cd2 O21 49.2(6) 16_466 6 O21 Cd2 C29 92.4(3) 16_466 . O21 Cd2 C29 140.0(3) 6 . O21 Cd2 C29 140.0(3) 16_466 11 O21 Cd2 C29 92.4(3) 6 11 C29 Cd2 C29 120.8(3) 11 . O30 Cd2 C20 123.1(2) 11 6 O30 Cd2 C20 123.1(2) . 6 O30 Cd2 O21 148.3(3) . 6 O30 Cd2 O21 101.8(4) 11 6 O30 Cd2 O21 101.8(4) . 16_466 O30 Cd2 O21 148.3(3) 11 16_466 O30 Cd2 C29 118.0(2) . 11 O30 Cd2 C29 28.38(18) 11 11 O30 Cd2 C29 28.38(18) . . O30 Cd2 C29 118.0(2) 11 . O30 Cd2 O30 101.7(3) . 11 O30 Cd2 O31 126.4(2) . 11 O30 Cd2 O31 55.91(17) 11 11 O30 Cd2 O31 55.91(17) . . O30 Cd2 O31 126.4(2) 11 . O31 Cd2 C20 108.2(3) 11 6 O31 Cd2 C20 108.2(3) . 6 O31 Cd2 O21 84.6(3) 11 6 O31 Cd2 O21 121.7(4) 11 16_466 O31 Cd2 O21 121.7(4) . 6 O31 Cd2 O21 84.6(3) . 16_466 O31 Cd2 C29 27.57(17) 11 11 O31 Cd2 C29 27.57(17) . . O31 Cd2 C29 114.04(19) 11 . O31 Cd2 C29 114.04(19) . 11 O31 Cd2 O31 96.1(2) 11 . C4 N3 Cd1 106.4(7) . . C14 N3 Cd1 106.6(9) . . C14 N3 C4 110.8(13) . . C15 N3 Cd1 108.3(6) . . C15 N3 C4 111.7(9) . . C15 N3 C14 112.7(9) . . N3 C4 H4A 109.5 . . N3 C4 H4B 109.5 . . H4A C4 H4B 108.1 . . C5 C4 N3 110.6(12) . . C5 C4 H4A 109.5 . . C5 C4 H4B 109.5 . . C4 C5 H5A 109.0 . . C4 C5 H5B 109.0 . . H5A C5 H5B 107.8 . . N6 C5 C4 112.9(13) . . N6 C5 H5A 109.0 . . N6 C5 H5B 109.0 . . C5 N6 Cd1 108.4(10) . . C5 N6 C7 114.1(14) . . C7 N6 Cd1 102.6(9) . . C22 N6 Cd1 110.9(9) . . C22 N6 C5 111.1(12) . . C22 N6 C7 109.4(11) . . N6 C7 H7A 109.0 . . N6 C7 H7B 109.0 . . N6 C7 C8 112.9(13) . . H7A C7 H7B 107.8 . . C8 C7 H7A 109.0 . . C8 C7 H7B 109.0 . . C7 C8 H8A 109.3 . . C7 C8 H8B 109.3 . . H8A C8 H8B 108.0 . . N9 C8 C7 111.6(15) . . N9 C8 H8A 109.3 . . N9 C8 H8B 109.3 . . C8 N9 Cd1 109.4(10) . . C8 N9 C10 110.8(13) . . C8 N9 C32 112.4(10) . . C10 N9 Cd1 104.8(6) . . C10 N9 C32 112.9(7) . . C32 N9 Cd1 106.1(5) . . N9 C10 H10A 109.0 . . N9 C10 H10B 109.0 . . N9 C10 C11 112.9(11) . . H10A C10 H10B 107.8 . . C11 C10 H10A 109.0 . . C11 C10 H10B 109.0 . . C10 C11 H11A 109.1 . . C10 C11 H11B 109.1 . . C10 C11 N12 112.6(13) . . H11A C11 H11B 107.8 . . N12 C11 H11A 109.1 . . N12 C11 H11B 109.1 . . C11 N12 Cd1 103.1(11) . . C13 N12 Cd1 104.8(10) . . C13 N12 C11 110.5(15) . . C13 N12 C22 112.0(13) . 11_655 C22 N12 Cd1 109.8(9) 11_655 . C22 N12 C11 115.7(12) 11_655 . N12 C13 H13A 109.5 . . N12 C13 H13B 109.5 . . N12 C13 C14 110.9(13) . . H13A C13 H13B 108.1 . . C14 C13 H13A 109.5 . . C14 C13 H13B 109.5 . . N3 C14 C13 112.6(11) . . N3 C14 H14A 109.1 . . N3 C14 H14B 109.1 . . C13 C14 H14A 109.1 . . C13 C14 H14B 109.1 . . H14A C14 H14B 107.8 . . N3 C15 N3 16.6(10) . 11_655 N3 C15 H15 106(4) 11_655 . N3 C15 H15 91(4) . . N3 C15 C16 117.9(8) 11_655 . N3 C15 C16 117.9(8) . . C16 C15 H15 112(4) . . C17 C16 C15 119.0(5) 11_655 . C17 C16 C15 119.0(5) . . C17 C16 C17 121.6(10) 11_655 . C16 C17 H17 121.5 . . C16 C17 C18 117.0(9) . . C18 C17 H17 121.5 . . C17 C18 H18 118.8 . . C19 C18 C17 122.4(9) . . C19 C18 H18 118.8 . . C18 C19 C18 114.1(12) . 11_655 C18 C19 C20 122.0(6) . . C18 C19 C20 122.0(6) 11_655 . C19 C20 Cd2 158.3(11) . 6_554 O21 C20 Cd2 65.9(9) 11_655 6_554 O21 C20 Cd2 65.9(9) . 6_554 O21 C20 C19 117.9(10) 11_655 . O21 C20 C19 117.9(10) . . O21 C20 O21 124(2) 11_655 . C20 O21 Cd2 88.5(10) . 6_554 N6 C22 N12 19.5(7) . 11_655 N6 C22 H22A 95(4) . . N6 C22 H22B 120(4) . . N6 C22 C23 116.1(8) . . N12 C22 H22A 111(4) 11_655 . N12 C22 H22B 104(4) 11_655 . H22A C22 H22B 104(5) . . C23 C22 N12 117.9(8) . 11_655 C23 C22 H22A 109(4) . . C23 C22 H22B 110(4) . . C24 C23 C22 120.4(5) . . C24 C23 C28 119.1(5) . . C28 C23 C22 120.5(6) . . C23 C24 H24 119.2 . . C23 C24 C25 121.5(5) . . C25 C24 H24 119.2 . . C24 C25 H25 120.3 . . C26 C25 C24 119.4(6) . . C26 C25 H25 120.3 . . C25 C26 C29 119.8(6) . . C27 C26 C25 119.6(5) . . C27 C26 C29 120.5(5) . . C26 C27 H27 119.5 . . C26 C27 C28 121.0(5) . . C28 C27 H27 119.5 . . C23 C28 H28 120.3 . . C27 C28 C23 119.3(6) . . C27 C28 H28 120.3 . . C26 C29 Cd2 175.0(4) . . O30 C29 Cd2 59.4(3) . . O30 C29 C26 119.1(5) . . O31 C29 Cd2 62.0(3) . . O31 C29 C26 119.6(6) . . O31 C29 O30 121.2(5) . . C29 O30 Cd2 92.3(4) . . C29 O31 Cd2 90.5(4) . . N9 C32 N9 22.7(7) 11_655 . N9 C32 H32 121(2) 11_655 . N9 C32 H32 143(2) . . N9 C32 C33 115.6(7) 11_655 . N9 C32 C33 115.6(7) . . C33 C32 H32 82(4) . . C34 C33 C32 121.7(4) 11_655 . C34 C33 C32 121.7(4) . . C34 C33 C34 116.5(8) 11_655 . C33 C34 H34 119.6 . . C33 C34 C35 120.8(7) . 2_665 C35 C34 H34 119.6 2_665 . C34 C35 H35 119.3 2_664 . C36 C35 C34 121.5(7) . 2_664 C36 C35 H35 119.3 . . C35 C36 C35 118.2(8) . 11_655 C35 C36 C37 120.7(4) 11_655 . C35 C36 C37 120.7(4) . . C36 C37 Cd1 176.0(6) . . O38 C37 Cd1 60.9(10) . . O38 C37 Cd1 60.9(10) 11_655 . O38 C37 C36 120.6(10) 11_655 . O38 C37 C36 120.6(10) . . O38 C37 O38 106.8(16) 11_655 . O39 C37 Cd1 61.2(9) 11_655 . O39 C37 Cd1 61.2(9) . . O39 C37 C36 117.3(9) 11_655 . O39 C37 C36 117.3(9) . . O39 C37 O38 38.3(7) . . O39 C37 O38 122.1(9) 11_655 . O39 C37 O38 122.1(9) . 11_655 O39 C37 O38 38.3(7) 11_655 11_655 O39 C37 O39 110.0(19) . 11_655 C37 O38 Cd1 91.5(11) . . C37 O39 Cd1 92.1(9) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cd1 N3 2.345(8) 11_655 Cd1 N3 2.345(8) . Cd1 N6 2.394(17) . Cd1 N6 2.393(17) 11_655 Cd1 N9 2.350(7) 11_655 Cd1 N9 2.350(7) . Cd1 N12 2.365(18) . Cd1 N12 2.365(18) 11_655 Cd1 O38 2.32(2) 11_655 Cd1 O38 2.32(2) . Cd1 O39 2.328(17) 11_655 Cd1 O39 2.328(17) . Cd2 C20 2.642(15) 6 Cd2 O21 2.413(10) 16_466 Cd2 O21 2.413(10) 6 Cd2 C29 2.679(6) . Cd2 C29 2.679(6) 11 Cd2 O30 2.307(5) 11 Cd2 O30 2.307(5) . Cd2 O31 2.365(4) 11 Cd2 O31 2.365(4) . N3 C4 1.551(17) . N3 C14 1.493(19) . N3 C15 1.471(12) . C4 H4A 0.9700 . C4 H4B 0.9700 . C4 C5 1.52(2) . C5 H5A 0.9700 . C5 H5B 0.9700 . C5 N6 1.48(2) . N6 C7 1.510(15) . N6 C22 1.458(18) . C7 H7A 0.9700 . C7 H7B 0.9700 . C7 C8 1.53(2) . C8 H8A 0.9700 . C8 H8B 0.9700 . C8 N9 1.42(2) . N9 C10 1.428(13) . N9 C32 1.478(12) . C10 H10A 0.9700 . C10 H10B 0.9700 . C10 C11 1.46(2) . C11 H11A 0.9700 . C11 H11B 0.9700 . C11 N12 1.59(2) . N12 C13 1.45(2) . N12 C22 1.522(18) 11_655 C13 H13A 0.9700 . C13 H13B 0.9700 . C13 C14 1.55(2) . C14 H14A 0.9700 . C14 H14B 0.9700 . C15 N3 1.471(12) 11_655 C15 H15 0.940(19) . C15 C16 1.544(12) . C16 C17 1.344(9) 11_655 C16 C17 1.344(9) . C17 H17 0.9300 . C17 C18 1.434(13) . C18 H18 0.9300 . C18 C19 1.341(12) . C19 C18 1.341(12) 11_655 C19 C20 1.527(19) . C20 Cd2 2.642(15) 6_554 C20 O21 1.140(12) 11_655 C20 O21 1.140(12) . O21 Cd2 2.413(10) 6_554 C22 N12 1.522(19) 11_655 C22 H22A 0.95(2) . C22 H22B 0.97(2) . C22 C23 1.508(8) . C23 C24 1.363(9) . C23 C28 1.403(8) . C24 H24 0.9300 . C24 C25 1.397(9) . C25 H25 0.9300 . C25 C26 1.381(8) . C26 C27 1.377(8) . C26 C29 1.495(7) . C27 H27 0.9300 . C27 C28 1.393(8) . C28 H28 0.9300 . C29 O30 1.275(8) . C29 O31 1.240(7) . C32 N9 1.478(12) 11_655 C32 H32 0.99(2) . C32 C33 1.547(11) . C33 C34 1.384(9) 11_655 C33 C34 1.384(9) . C34 H34 0.9300 . C34 C35 1.396(10) 2_665 C35 C34 1.396(10) 2_664 C35 H35 0.9300 . C35 C36 1.345(9) . C36 C35 1.345(9) 11_655 C36 C37 1.513(10) . C37 O38 1.228(14) 11_655 C37 O38 1.228(14) . C37 O39 1.196(12) . C37 O39 1.196(12) 11_655 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_4 Cd1 N3 C4 C5 45.8(13) . . Cd1 N3 C14 C13 35.4(15) . . Cd1 N3 C15 N3 -81.7(5) . 11_655 Cd1 N3 C15 C16 -176.1(3) . . Cd1 N6 C7 C8 45.8(14) . . Cd1 N6 C22 N12 -79(4) . 11_655 Cd1 N6 C22 C23 -179.2(5) . . Cd1 N9 C10 C11 50.6(13) . . Cd1 N9 C32 N9 -79.1(3) . 11_655 Cd1 N9 C32 C33 -174.6(2) . . Cd1 N12 C13 C14 48.1(14) . . N3 Cd1 N3 C4 -40.8(8) 11_655 . N3 Cd1 N3 C14 -159.1(8) 11_655 . N3 Cd1 N3 C15 79.5(7) 11_655 . N3 Cd1 N6 C5 -7.5(11) . . N3 Cd1 N6 C5 -3.5(10) 11_655 . N3 Cd1 N6 C7 117.5(10) 11_655 . N3 Cd1 N6 C7 113.5(9) . . N3 Cd1 N6 C22 -125.8(8) 11_655 . N3 Cd1 N6 C22 -129.8(8) . . N3 Cd1 N9 C8 -73.8(12) . . N3 Cd1 N9 C8 -61.1(12) 11_655 . N3 Cd1 N9 C10 45.1(8) . . N3 Cd1 N9 C10 57.8(8) 11_655 . N3 Cd1 N9 C32 164.7(5) . . N3 Cd1 N9 C32 177.4(5) 11_655 . N3 Cd1 N12 C11 -137.7(11) . . N3 Cd1 N12 C11 -132.8(10) 11_655 . N3 Cd1 N12 C13 -22.0(10) . . N3 Cd1 N12 C13 -17.1(11) 11_655 . N3 Cd1 N12 C22 98.5(8) . 11_655 N3 Cd1 N12 C22 103.4(8) 11_655 11_655 N3 Cd1 C37 C36 5.8(4) . . N3 Cd1 C37 C36 -5.8(4) 11_655 . N3 Cd1 C37 O38 107.5(10) 11_655 11_655 N3 Cd1 C37 O38 -107.5(10) . . N3 Cd1 C37 O38 -119.1(9) 11_655 . N3 Cd1 C37 O38 119.1(9) . 11_655 N3 Cd1 C37 O39 -75.0(11) 11_655 . N3 Cd1 C37 O39 -63.5(11) . . N3 Cd1 C37 O39 75.0(11) . 11_655 N3 Cd1 C37 O39 63.5(11) 11_655 11_655 N3 Cd1 O38 C37 76.3(10) 11_655 . N3 Cd1 O38 C37 87.0(9) . . N3 Cd1 O39 C37 114.6(10) 11_655 . N3 Cd1 O39 C37 124.3(10) . . N3 C4 C5 N6 -57.1(16) . . N3 C15 C16 C17 -103.2(10) 11_655 11_655 N3 C15 C16 C17 103.2(10) . . N3 C15 C16 C17 84.4(12) 11_655 . N3 C15 C16 C17 -84.4(12) . 11_655 C4 N3 C14 C13 -80.0(15) . . C4 N3 C15 N3 35.2(9) . 11_655 C4 N3 C15 C16 -59.3(11) . . C4 C5 N6 Cd1 35.7(15) . . C4 C5 N6 C7 -77.9(17) . . C4 C5 N6 C22 157.9(12) . . C5 N6 C7 C8 162.8(15) . . C5 N6 C22 N12 160(4) . 11_655 C5 N6 C22 C23 60.1(13) . . N6 Cd1 N3 C4 117.1(9) 11_655 . N6 Cd1 N3 C4 -19.9(9) . . N6 Cd1 N3 C14 -1.2(9) 11_655 . N6 Cd1 N3 C14 -138.2(9) . . N6 Cd1 N3 C15 100.4(8) . . N6 Cd1 N3 C15 -122.7(8) 11_655 . N6 Cd1 N6 C5 -58.3(14) 11_655 . N6 Cd1 N6 C7 62.7(12) 11_655 . N6 Cd1 N6 C22 179.4(3) 11_655 . N6 Cd1 N9 C8 -136.1(11) 11_655 . N6 Cd1 N9 C8 -9.8(11) . . N6 Cd1 N9 C10 109.1(8) . . N6 Cd1 N9 C10 -17.2(8) 11_655 . N6 Cd1 N9 C32 -131.2(6) . . N6 Cd1 N9 C32 102.5(6) 11_655 . N6 Cd1 N12 C11 -165(4) 11_655 . N6 Cd1 N12 C11 -72.3(11) . . N6 Cd1 N12 C13 43.3(13) . . N6 Cd1 N12 C13 -50(3) 11_655 . N6 Cd1 N12 C22 163.8(7) . 11_655 N6 Cd1 N12 C22 71(3) 11_655 11_655 N6 Cd1 C37 C36 -82.3(4) . . N6 Cd1 C37 C36 82.3(4) 11_655 . N6 Cd1 C37 O38 -31.0(10) 11_655 . N6 Cd1 C37 O38 -164.4(9) 11_655 11_655 N6 Cd1 C37 O38 31.0(10) . 11_655 N6 Cd1 C37 O38 164.4(9) . . N6 Cd1 C37 O39 -151.5(11) . . N6 Cd1 C37 O39 151.5(11) 11_655 11_655 N6 Cd1 C37 O39 -13.0(12) . 11_655 N6 Cd1 C37 O39 13.0(12) 11_655 . N6 Cd1 O38 C37 152.5(9) 11_655 . N6 Cd1 O38 C37 -23.2(13) . . N6 Cd1 O39 C37 -168.3(10) 11_655 . N6 Cd1 O39 C37 40.3(14) . . N6 C7 C8 N9 -60(2) . . N6 C22 C23 C24 -85.9(9) . . N6 C22 C23 C28 93.1(9) . . C7 N6 C22 N12 33(3) . 11_655 C7 N6 C22 C23 -66.8(12) . . C7 C8 N9 Cd1 37.6(18) . . C7 C8 N9 C10 -77.5(17) . . C7 C8 N9 C32 155.2(12) . . C8 N9 C10 C11 168.5(14) . . C8 N9 C32 N9 161.4(11) . 11_655 C8 N9 C32 C33 65.8(12) . . N9 Cd1 N3 C4 61.6(10) 11_655 . N9 Cd1 N3 C4 44.2(10) . . N9 Cd1 N3 C14 -56.7(10) 11_655 . N9 Cd1 N3 C14 -74.1(10) . . N9 Cd1 N3 C15 -178.1(5) 11_655 . N9 Cd1 N3 C15 164.4(5) . . N9 Cd1 N6 C5 -139.8(12) . . N9 Cd1 N6 C5 -133.3(11) 11_655 . N9 Cd1 N6 C7 -12.3(9) 11_655 . N9 Cd1 N6 C7 -18.8(8) . . N9 Cd1 N6 C22 97.9(8) . . N9 Cd1 N6 C22 104.4(7) 11_655 . N9 Cd1 N9 C8 -162.6(11) 11_655 . N9 Cd1 N9 C10 -43.7(7) 11_655 . N9 Cd1 N9 C32 76.0(4) 11_655 . N9 Cd1 N12 C11 -0.7(9) 11_655 . N9 Cd1 N12 C11 -6.5(9) . . N9 Cd1 N12 C13 115.0(12) 11_655 . N9 Cd1 N12 C13 109.2(11) . . N9 Cd1 N12 C22 -124.5(10) 11_655 11_655 N9 Cd1 N12 C22 -130.3(9) . 11_655 N9 Cd1 C37 C36 -171.9(3) . . N9 Cd1 C37 C36 171.9(3) 11_655 . N9 Cd1 C37 O38 58.6(9) 11_655 . N9 Cd1 C37 O38 74.8(9) . . N9 Cd1 C37 O38 -58.6(9) . 11_655 N9 Cd1 C37 O38 -74.8(9) 11_655 11_655 N9 Cd1 C37 O39 -118.8(11) 11_655 11_655 N9 Cd1 C37 O39 118.8(11) . . N9 Cd1 C37 O39 102.7(11) 11_655 . N9 Cd1 C37 O39 -102.7(11) . 11_655 N9 Cd1 O38 C37 -116.5(8) . . N9 Cd1 O38 C37 -129.7(8) 11_655 . N9 Cd1 O39 C37 -77.8(11) . . N9 Cd1 O39 C37 -92.6(10) 11_655 . N9 C10 C11 N12 -62.3(18) . . N9 C32 C33 C34 104.0(10) . . N9 C32 C33 C34 -104.0(10) 11_655 11_655 N9 C32 C33 C34 78.8(11) 11_655 . N9 C32 C33 C34 -78.8(11) . 11_655 C10 N9 C32 N9 35.1(7) . 11_655 C10 N9 C32 C33 -60.4(8) . . C10 C11 N12 Cd1 35.3(16) . . C10 C11 N12 C13 -76.2(19) . . C10 C11 N12 C22 155.2(14) . 11_655 C11 N12 C13 C14 158.5(14) . . N12 Cd1 N3 C4 -13.2(9) 11_655 . N12 Cd1 N3 C4 111.0(9) . . N12 Cd1 N3 C14 -131.5(9) 11_655 . N12 Cd1 N3 C14 -7.3(9) . . N12 Cd1 N3 C15 107.1(8) 11_655 . N12 Cd1 N3 C15 -128.7(8) . . N12 Cd1 N6 C5 -154(4) 11_655 . N12 Cd1 N6 C5 -73.3(12) . . N12 Cd1 N6 C7 47.7(11) . . N12 Cd1 N6 C7 -33(3) 11_655 . N12 Cd1 N6 C22 84(4) 11_655 . N12 Cd1 N6 C22 164.4(6) . . N12 Cd1 N9 C8 -140.5(12) . . N12 Cd1 N9 C8 -6.5(11) 11_655 . N12 Cd1 N9 C10 112.4(8) 11_655 . N12 Cd1 N9 C10 -21.6(8) . . N12 Cd1 N9 C32 -128.0(7) 11_655 . N12 Cd1 N9 C32 98.1(6) . . N12 Cd1 N12 C11 -57.9(14) 11_655 . N12 Cd1 N12 C13 57.8(14) 11_655 . N12 Cd1 N12 C22 178.3(3) 11_655 11_655 N12 Cd1 C37 C36 95.9(4) . . N12 Cd1 C37 C36 -95.9(4) 11_655 . N12 Cd1 C37 O38 150.8(9) 11_655 . N12 Cd1 C37 O38 -150.8(9) . 11_655 N12 Cd1 C37 O38 17.4(10) 11_655 11_655 N12 Cd1 C37 O38 -17.4(10) . . N12 Cd1 C37 O39 165.1(11) . 11_655 N12 Cd1 C37 O39 -26.7(12) 11_655 11_655 N12 Cd1 C37 O39 -165.1(11) 11_655 . N12 Cd1 C37 O39 26.7(12) . . N12 Cd1 O38 C37 164.7(9) . . N12 Cd1 O38 C37 -42.7(13) 11_655 . N12 Cd1 O39 C37 -156.6(10) . . N12 Cd1 O39 C37 22.4(16) 11_655 . N12 C13 C14 N3 -60.3(18) . . N12 C22 C23 C24 -107.7(10) 11_655 . N12 C22 C23 C28 71.3(10) 11_655 . C14 N3 C4 C5 161.3(13) . . C14 N3 C15 N3 160.7(9) . 11_655 C14 N3 C15 C16 66.3(11) . . C15 N3 C4 C5 -72.2(12) . . C15 N3 C14 C13 154.0(11) . . C15 C16 C17 C18 -178.2(10) . . C16 C17 C18 C19 -17.8(19) . . C17 C16 C17 C18 10(2) 11_655 . C17 C18 C19 C18 25(2) . 11_655 C17 C18 C19 C20 -170.2(13) . . C18 C19 C20 Cd2 -98.0(14) 11_655 6_554 C18 C19 C20 Cd2 98.1(14) . 6_554 C18 C19 C20 O21 167.3(17) 11_655 11_655 C18 C19 C20 O21 -167.3(17) . . C18 C19 C20 O21 -3(2) 11_655 . C18 C19 C20 O21 3(2) . 11_655 C19 C20 O21 Cd2 -156.2(13) . 6_554 C20 Cd2 C29 C26 35(5) 6 . C20 Cd2 C29 O30 108.6(6) 6 . C20 Cd2 C29 O31 -75.6(6) 6 . C20 Cd2 O30 C29 -88.3(6) 6 . C20 Cd2 O31 C29 115.7(5) 6 . O21 Cd2 C29 C26 37(5) 16_466 . O21 Cd2 C29 C26 51(5) 6 . O21 Cd2 C29 O30 110.7(5) 16_466 . O21 Cd2 C29 O30 125.4(6) 6 . O21 Cd2 C29 O31 -58.8(6) 6 . O21 Cd2 C29 O31 -73.5(5) 16_466 . O21 Cd2 O30 C29 -72.7(5) 16_466 . O21 Cd2 O30 C29 -94.1(8) 6 . O21 Cd2 O31 C29 105.9(5) 16_466 . O21 Cd2 O31 C29 139.8(4) 6 . O21 C20 O21 Cd2 34(2) 11_655 6_554 C22 N6 C7 C8 -72.0(15) . . C22 N12 C13 C14 -70.9(15) 11_655 . C22 C23 C24 C25 178.1(7) . . C22 C23 C28 C27 -178.9(6) . . C23 C24 C25 C26 1.5(13) . . C24 C23 C28 C27 0.1(10) . . C24 C25 C26 C27 -1.2(11) . . C24 C25 C26 C29 -179.0(7) . . C25 C26 C27 C28 0.3(10) . . C25 C26 C29 Cd2 70(5) . . C25 C26 C29 O30 -1.5(9) . . C25 C26 C29 O31 177.3(6) . . C26 C27 C28 C23 0.2(10) . . C26 C29 O30 Cd2 174.5(5) . . C26 C29 O31 Cd2 -174.6(5) . . C27 C26 C29 Cd2 -108(5) . . C27 C26 C29 O30 -179.2(6) . . C27 C26 C29 O31 -0.4(9) . . C28 C23 C24 C25 -1.0(12) . . C29 Cd2 C29 C26 -167(5) 11 . C29 Cd2 C29 O30 -92.6(5) 11 . C29 Cd2 C29 O31 83.2(5) 11 . C29 Cd2 O30 C29 103.7(5) 11 . C29 Cd2 O31 C29 -111.0(4) 11 . C29 C26 C27 C28 178.1(6) . . O30 Cd2 C29 C26 -74(5) . . O30 Cd2 C29 C26 -134(5) 11 . O30 Cd2 C29 O30 -60.1(4) 11 . O30 Cd2 C29 O31 115.8(4) 11 . O30 Cd2 C29 O31 175.9(7) . . O30 Cd2 O30 C29 128.6(3) 11 . O30 Cd2 O31 C29 -2.4(4) . . O30 Cd2 O31 C29 -81.2(4) 11 . O30 C29 O31 Cd2 4.2(7) . . O31 Cd2 C29 C26 163(5) 11 . O31 Cd2 C29 C26 110(5) . . O31 Cd2 C29 O30 -122.8(4) 11 . O31 Cd2 C29 O30 -175.9(7) . . O31 Cd2 C29 O31 53.0(4) 11 . O31 Cd2 O30 C29 72.5(5) 11 . O31 Cd2 O30 C29 2.3(4) . . O31 Cd2 O31 C29 -132.8(3) 11 . O31 C29 O30 Cd2 -4.3(7) . . C32 N9 C10 C11 -64.4(13) . . C32 C33 C34 C35 176.0(10) . 2_665 C34 C33 C34 C35 -1(2) 11_655 2_665 C34 C35 C36 C35 10(2) 2_664 11_655 C34 C35 C36 C37 -177.0(10) 2_664 . C35 C36 C37 Cd1 93.4(9) . . C35 C36 C37 Cd1 -93.4(9) 11_655 . C35 C36 C37 O38 155.4(12) 11_655 11_655 C35 C36 C37 O38 -17.8(16) . 11_655 C35 C36 C37 O38 -155.4(12) . . C35 C36 C37 O38 17.8(16) 11_655 . C35 C36 C37 O39 26.2(16) . 11_655 C35 C36 C37 O39 -160.6(13) 11_655 11_655 C35 C36 C37 O39 160.6(13) . . C35 C36 C37 O39 -26.2(16) 11_655 . C36 C37 O38 Cd1 -175.7(7) . . C36 C37 O39 Cd1 -175.8(6) . . O38 Cd1 N3 C4 -163.9(8) . . O38 Cd1 N3 C4 -103.5(9) 11_655 . O38 Cd1 N3 C14 138.2(9) 11_655 . O38 Cd1 N3 C14 77.7(9) . . O38 Cd1 N3 C15 16.8(10) 11_655 . O38 Cd1 N3 C15 -43.7(9) . . O38 Cd1 N6 C5 116.4(12) . . O38 Cd1 N6 C5 118.5(11) 11_655 . O38 Cd1 N6 C7 -120.5(9) 11_655 . O38 Cd1 N6 C7 -122.6(10) . . O38 Cd1 N6 C22 -3.8(8) 11_655 . O38 Cd1 N6 C22 -5.9(12) . . O38 Cd1 N9 C8 131.6(11) . . O38 Cd1 N9 C8 79.8(11) 11_655 . O38 Cd1 N9 C10 -161.3(7) 11_655 . O38 Cd1 N9 C10 -109.5(7) . . O38 Cd1 N9 C32 10.1(6) . . O38 Cd1 N9 C32 -41.7(6) 11_655 . O38 Cd1 N12 C11 88.9(12) 11_655 . O38 Cd1 N12 C11 101.7(10) . . O38 Cd1 N12 C13 -142.6(11) . . O38 Cd1 N12 C13 -155.4(10) 11_655 . O38 Cd1 N12 C22 -22.1(9) . 11_655 O38 Cd1 N12 C22 -34.9(13) 11_655 11_655 O38 Cd1 C37 C36 -113.3(9) 11_655 . O38 Cd1 C37 C36 113.3(9) . . O38 Cd1 C37 O38 -133.4(18) . 11_655 O38 Cd1 C37 O38 133.4(18) 11_655 . O38 Cd1 C37 O39 -44.1(8) 11_655 11_655 O38 Cd1 C37 O39 -177.5(18) . 11_655 O38 Cd1 C37 O39 177.5(18) 11_655 . O38 Cd1 C37 O39 44.1(8) . . O38 Cd1 O38 C37 -25.9(10) 11_655 . O38 Cd1 O39 C37 -72.4(15) . . O38 Cd1 O39 C37 -1.4(10) 11_655 . O38 C37 O38 Cd1 41.5(16) 11_655 . O38 C37 O39 Cd1 79(2) . . O38 C37 O39 Cd1 2.6(18) 11_655 . O39 Cd1 N3 C4 -106.4(9) 11_655 . O39 Cd1 N3 C4 -157.5(9) . . O39 Cd1 N3 C14 135.3(9) 11_655 . O39 Cd1 N3 C14 84.2(9) . . O39 Cd1 N3 C15 -37.3(8) . . O39 Cd1 N3 C15 13.9(8) 11_655 . O39 Cd1 N6 C5 85.7(13) . . O39 Cd1 N6 C5 98.8(12) 11_655 . O39 Cd1 N6 C7 -140.1(10) 11_655 . O39 Cd1 N6 C7 -153.3(8) . . O39 Cd1 N6 C22 -23.5(8) 11_655 . O39 Cd1 N6 C22 -36.6(11) . . O39 Cd1 N9 C8 72.9(11) 11_655 . O39 Cd1 N9 C8 133.5(11) . . O39 Cd1 N9 C10 -168.2(7) 11_655 . O39 Cd1 N9 C10 -107.6(7) . . O39 Cd1 N9 C32 -48.5(6) 11_655 . O39 Cd1 N9 C32 12.1(7) . . O39 Cd1 N12 C11 121.4(11) . . O39 Cd1 N12 C11 120.9(11) 11_655 . O39 Cd1 N12 C13 -123.0(11) . . O39 Cd1 N12 C13 -123.4(12) 11_655 . O39 Cd1 N12 C22 -2.5(9) . 11_655 O39 Cd1 N12 C22 -2.9(14) 11_655 11_655 O39 Cd1 C37 C36 69.2(11) . . O39 Cd1 C37 C36 -69.2(11) 11_655 . O39 Cd1 C37 O38 177.5(18) 11_655 . O39 Cd1 C37 O38 -44.1(8) . . O39 Cd1 C37 O38 44.1(8) 11_655 11_655 O39 Cd1 C37 O38 -177.5(18) . 11_655 O39 Cd1 C37 O39 -138(2) 11_655 . O39 Cd1 C37 O39 138(2) . 11_655 O39 Cd1 O38 C37 68.0(16) . . O39 Cd1 O38 C37 -1.4(10) 11_655 . O39 Cd1 O39 C37 23.0(11) 11_655 . O39 C37 O38 Cd1 2.6(18) 11_655 . O39 C37 O38 Cd1 -79(2) . . O39 C37 O39 Cd1 -38.2(16) 11_655 . loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.053 -0.008 -0.005 9212 1298 ' '