#------------------------------------------------------------------------------ #$Date: 2017-06-27 04:39:54 +0300 (Tue, 27 Jun 2017) $ #$Revision: 198149 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/85/7228543.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_7228543 loop_ _publ_author_name 'Xu, Xiao-Wu' 'Tian, Chong-Bin' 'Du, Shaowu' _publ_section_title ; Synthesis, structure and luminescent properties of two Cd(II)/M(I) (M = K, Rb) interpenetrated heterometallic frameworks based on giant double-walled cages ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/C7CE00803A _journal_year 2017 _chemical_formula_sum 'C68 H79.5 Cd3 K6 N16 O39.75' _chemical_formula_weight 2328.77 _space_group_crystal_system cubic _space_group_IT_number 211 _space_group_name_Hall 'I 4 2 3' _space_group_name_H-M_alt 'I 4 3 2' _symmetry_space_group_name_Hall 'I 4 2 3' _symmetry_space_group_name_H-M 'I 4 3 2' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-06-01 deposited with the CCDC. 2017-06-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 27.9730(10) _cell_length_b 27.9730(10) _cell_length_c 27.9730(10) _cell_measurement_reflns_used 30024 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.4816 _cell_measurement_theta_min 2.0587 _cell_volume 21888.6(14) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.978 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_unetI/netI 0.0171 _diffrn_reflns_Laue_measured_fraction_full 0.978 _diffrn_reflns_Laue_measured_fraction_max 0.983 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 94403 _diffrn_reflns_point_group_measured_fraction_full 0.985 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.465 _diffrn_reflns_theta_min 3.714 _exptl_absorpt_coefficient_mu 0.887 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8877 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Sphere(Rigaku Crystalclear)' _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.413 _exptl_crystal_description Cubic _exptl_crystal_F_000 9404 _exptl_crystal_preparation ', Luminescent' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _platon_squeeze_details ; The unit cell contains 32 DMF molecules and 16 CH3OH molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; _refine_diff_density_max 0.728 _refine_diff_density_min -0.808 _refine_diff_density_rms 0.062 _refine_ls_abs_structure_details ; Flack x determined using 1629 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.011(9) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 175 _refine_ls_number_reflns 4166 _refine_ls_number_restraints 30 _refine_ls_restrained_S_all 1.076 _refine_ls_R_factor_all 0.0426 _refine_ls_R_factor_gt 0.0415 _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^)+(0.0593P)^2^+33.2729P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1083 _refine_ls_wR_factor_ref 0.1094 _reflns_Friedel_coverage 0.750 _reflns_Friedel_fraction_full 0.994 _reflns_Friedel_fraction_max 0.996 _reflns_number_gt 4116 _reflns_number_total 4166 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7ce00803a2.cif _cod_data_source_block A _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas ; _cod_original_cell_volume 21889(2) _cod_original_formula_sum 'C68 H79.50 Cd3 K6 N16 O39.75' _cod_database_code 7228543 _shelx_shelxl_version_number 2014/7 _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. ; _platon_squeeze_void_probe_radius 1.20 _shelx_res_file ; A.res created by SHELXL-2014/7 TITL A in I432 CELL 0.71073 27.9730 27.9730 27.9730 90.000 90.000 90.000 ZERR 8.00 0.0010 0.0010 0.0010 0.000 0.000 0.000 LATT -2 SYMM -X, -Y, Z SYMM -X, Y, -Z SYMM X, -Y, -Z SYMM Z, X, Y SYMM Z, -X, -Y SYMM -Z, -X, Y SYMM -Z, X, -Y SYMM Y, Z, X SYMM -Y, Z, -X SYMM Y, -Z, -X SYMM -Y, -Z, X SYMM Y, X, -Z SYMM -Y, -X, -Z SYMM Y, -X, Z SYMM -Y, X, Z SYMM X, Z, -Y SYMM -X, Z, Y SYMM -X, -Z, -Y SYMM X, -Z, Y SYMM Z, Y, -X SYMM Z, -Y, X SYMM -Z, Y, X SYMM -Z, -Y, -X SFAC C H N O K CD UNIT 544 636 128 318 48 24 L.S. 10 isor 0.01 o6 k2 O7 omit 0 3 3 omit 1 1 6 omit 2 4 4 omit 0 0 4 omit 0 1 3 omit 2 3 3 omit 4 6 6 omit 1 1 4 omit 0 0 8 omit 1 1 8 omit 0 3 5 omit 0 0 6 omit 2 2 2 omit 3 3 4 omit 4 4 6 omit 3 3 8 omit 1 3 6 omit 3 3 6 omit -1 2 3 omit 1 2 3 omit 0 1 7 omit 0 4 6 omit 0 5 7 omit -1 3 6 omit 0 2 6 omit 2 6 6 omit 0 6 6 omit 0 2 8 omit 0 4 8 omit -1 5 6 omit 1 5 6 omit 2 2 4 omit 0 1 5 omit 0 4 4 omit 0 3 7 omit 1 2 5 omit -1 2 5 omit 1 2 7 omit 0 3 9 omit -3 4 5 omit 4 5 5 omit 0 2 4 omit 0 5 5 omit -3 5 6 omit 1 5 8 omit -1 5 8 BOND $H FMAP 2 PLAN 20 simu 0.01 0.02 3.8 o6 k2 simu 0.01 0.02 3.8 o7 k2 ACTA WGHT 0.059300 33.272900 FVAR 0.58215 CD1 6 0.446330 0.244886 0.941205 10.50000 0.02957 0.04130 = 0.02780 -0.00266 0.00108 0.00490 K1 5 0.500000 0.176009 0.823991 10.50000 0.05943 0.05102 = 0.05102 -0.01626 -0.00036 -0.00036 N1 3 0.642297 0.273815 0.774767 11.00000 0.06256 0.06262 = 0.05795 -0.02282 0.02888 -0.02777 AFIX 43 H1A 2 0.624607 0.249741 0.767511 11.00000 -1.20000 AFIX 0 C1 1 0.666821 0.392927 0.905653 11.00000 0.05311 0.05107 = 0.05497 -0.00836 -0.00297 -0.01051 C2 1 0.638367 0.355187 0.880673 11.00000 0.05118 0.04500 = 0.04258 -0.00388 0.00423 -0.01953 C3 1 0.654342 0.334798 0.838447 11.00000 0.05545 0.04579 = 0.05028 -0.01219 0.01278 -0.01904 AFIX 43 H3A 2 0.682742 0.345305 0.824722 11.00000 -1.20000 AFIX 0 C4 1 0.628021 0.298552 0.816388 11.00000 0.04206 0.05187 = 0.04290 -0.01217 0.01238 -0.01102 C5 1 0.586447 0.281871 0.838177 11.00000 0.04494 0.05003 = 0.04000 -0.00602 0.00730 -0.01261 AFIX 43 H5A 2 0.569331 0.257099 0.824081 11.00000 -1.20000 AFIX 0 C6 1 0.569963 0.302128 0.881434 11.00000 0.03383 0.04083 = 0.04785 -0.00884 0.00000 -0.00037 C7 1 0.597031 0.338086 0.902562 11.00000 0.04732 0.03844 = 0.03760 -0.00829 0.00406 -0.00013 AFIX 43 H7A 2 0.587405 0.350887 0.931696 11.00000 -1.20000 AFIX 0 C8 1 0.526958 0.281731 0.905046 11.00000 0.03482 0.04170 = 0.03837 -0.00430 -0.00248 0.00298 C9 1 0.678931 0.281557 0.744522 11.00000 0.04640 0.05910 = 0.05278 -0.01617 0.01182 -0.01701 O1 4 0.703196 0.408801 0.885540 11.00000 0.06946 0.07861 = 0.08055 -0.02694 0.01490 -0.03262 O2 4 0.656924 0.404766 0.946747 11.00000 0.08963 0.07171 = 0.04193 -0.01040 -0.00886 -0.03086 O3 4 0.511853 0.301013 0.943291 11.00000 0.04113 0.05511 = 0.03694 -0.01246 0.00544 -0.00583 O4 4 0.507178 0.245996 0.887645 11.00000 0.03883 0.04048 = 0.04857 -0.00839 0.00143 -0.00859 O5 4 0.431475 0.251852 0.799276 11.00000 0.08751 0.09588 = 0.08570 -0.04954 -0.03663 0.03162 O6 4 0.432358 0.432358 1.000000 10.50000 0.21249 0.21249 = 0.20336 0.00520 -0.00520 -0.00214 N2 3 0.708744 0.318604 0.750897 11.00000 0.05864 0.05783 = 0.04755 -0.02204 0.01910 -0.02546 K2 5 0.482997 0.368716 0.992669 10.50000 0.11606 0.12946 = 0.08103 0.00608 0.00672 0.01382 O7 4 0.500000 0.500000 1.000000 10.12500 0.16216 0.16216 = 0.13954 0.00000 0.00000 0.00000 HKLF 4 REM A in I432 REM R1 = 0.0415 for 4116 Fo > 4sig(Fo) and 0.0426 for all 4166 data REM 175 parameters refined using 30 restraints END WGHT 0.0573 23.0478 REM Highest difference peak 0.728, deepest hole -0.808, 1-sigma level 0.062 Q1 1 0.4492 0.2844 0.7805 11.00000 0.05 0.73 Q2 1 0.4569 0.4474 1.0496 11.00000 0.05 0.50 Q3 1 0.6951 0.2500 0.8049 10.50000 0.05 0.34 Q4 1 0.5523 0.3638 0.9395 11.00000 0.05 0.33 Q5 1 0.5000 0.3724 1.0000 10.50000 0.05 0.32 Q6 1 0.6848 0.3711 0.8115 11.00000 0.05 0.27 Q7 1 0.6297 0.2469 0.7587 11.00000 0.05 0.27 Q8 1 0.5106 0.2337 0.8898 11.00000 0.05 0.26 Q9 1 0.5009 0.2440 0.8809 11.00000 0.05 0.25 Q10 1 0.3983 0.4500 1.0098 11.00000 0.05 0.25 Q11 1 0.7130 0.3693 0.9479 11.00000 0.05 0.22 Q12 1 0.5220 0.2494 0.8800 11.00000 0.05 0.22 Q13 1 0.6912 0.3758 0.8196 11.00000 0.05 0.22 Q14 1 0.4695 0.4585 1.0297 11.00000 0.05 0.22 Q15 1 0.6817 0.4329 0.8628 11.00000 0.05 0.21 Q16 1 0.6634 0.3444 0.9102 11.00000 0.05 0.20 Q17 1 0.5011 0.3030 0.9444 11.00000 0.05 0.20 Q18 1 0.5000 0.5000 0.9570 10.25000 0.05 0.20 Q19 1 0.6894 0.3106 0.6894 10.33333 0.05 0.20 Q20 1 0.4254 0.2445 0.7905 11.00000 0.05 0.20 ; _shelx_res_checksum 10685 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y+1/2, -x+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'x+1/2, z+1/2, -y+1/2' '-x+1/2, z+1/2, y+1/2' '-x+1/2, -z+1/2, -y+1/2' 'x+1/2, -z+1/2, y+1/2' 'z+1/2, y+1/2, -x+1/2' 'z+1/2, -y+1/2, x+1/2' '-z+1/2, y+1/2, x+1/2' '-z+1/2, -y+1/2, -x+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 Cd1 Cd 0.44633(12) 0.24489(14) 0.94120(12) 0.0329(5) Uani 0.5 1 d . . P K1 K 0.5000 0.17601(4) 0.82399(4) 0.0538(4) Uani 1 2 d S T P N1 N 0.64230(18) 0.27382(19) 0.77477(18) 0.0610(13) Uani 1 1 d . . . H1A H 0.6246 0.2497 0.7675 0.073 Uiso 1 1 calc R U . C1 C 0.6668(2) 0.3929(2) 0.9057(2) 0.0531(13) Uani 1 1 d . . . C2 C 0.63837(18) 0.35519(17) 0.88067(16) 0.0463(10) Uani 1 1 d . . . C3 C 0.65434(19) 0.33480(18) 0.83845(18) 0.0505(11) Uani 1 1 d . . . H3A H 0.6827 0.3453 0.8247 0.061 Uiso 1 1 calc R U . C4 C 0.62802(18) 0.29855(19) 0.81639(17) 0.0456(11) Uani 1 1 d . . . C5 C 0.58645(18) 0.28187(19) 0.83818(17) 0.0450(10) Uani 1 1 d . . . H5A H 0.5693 0.2571 0.8241 0.054 Uiso 1 1 calc R U . C6 C 0.56996(16) 0.30213(17) 0.88143(18) 0.0408(10) Uani 1 1 d . . . C7 C 0.59703(17) 0.33809(15) 0.90256(17) 0.0411(9) Uani 1 1 d . . . H7A H 0.5874 0.3509 0.9317 0.049 Uiso 1 1 calc R U . C8 C 0.52696(15) 0.28173(16) 0.90505(16) 0.0383(9) Uani 1 1 d . . . C9 C 0.67893(19) 0.2816(2) 0.7445(2) 0.0528(13) Uani 1 1 d . . . O1 O 0.70320(17) 0.40880(18) 0.88554(18) 0.0762(14) Uani 1 1 d . . . O2 O 0.65692(17) 0.40477(16) 0.94675(14) 0.0678(12) Uani 1 1 d . . . O3 O 0.51185(11) 0.30101(12) 0.94329(11) 0.0444(7) Uani 1 1 d . . . O4 O 0.50718(11) 0.24600(12) 0.88765(11) 0.0426(7) Uani 1 1 d . . . O5 O 0.4315(2) 0.2519(2) 0.79928(19) 0.0897(17) Uani 1 1 d . . . O6 O 0.4324(5) 0.4324(5) 1.0000 0.209(5) Uani 1 2 d S TU P N2 N 0.70874(17) 0.31860(17) 0.75090(17) 0.0547(12) Uani 1 1 d . . . K2 K 0.48300(16) 0.36872(18) 0.99267(17) 0.1089(13) Uani 0.5 1 d . U P O7 O 0.5000 0.5000 1.0000 0.155(6) Uani 1 8 d S TU 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 Cd1 0.0296(7) 0.0413(15) 0.0278(7) -0.0027(6) 0.0011(6) 0.0049(6) K1 0.0594(9) 0.0510(5) 0.0510(5) -0.0163(6) -0.0004(5) -0.0004(5) N1 0.063(3) 0.063(3) 0.058(3) -0.023(2) 0.029(2) -0.028(2) C1 0.053(3) 0.051(3) 0.055(3) -0.008(2) -0.003(2) -0.011(2) C2 0.051(3) 0.045(2) 0.043(2) -0.0039(18) 0.004(2) -0.0195(19) C3 0.055(3) 0.046(2) 0.050(3) -0.012(2) 0.013(2) -0.019(2) C4 0.042(2) 0.052(3) 0.043(2) -0.012(2) 0.0124(19) -0.011(2) C5 0.045(2) 0.050(3) 0.040(2) -0.006(2) 0.0073(19) -0.013(2) C6 0.034(2) 0.041(2) 0.048(2) -0.0088(19) 0.0000(17) -0.0004(17) C7 0.047(3) 0.038(2) 0.038(2) -0.0083(18) 0.0041(17) -0.0001(19) C8 0.035(2) 0.042(2) 0.038(2) -0.0043(17) -0.0025(17) 0.0030(17) C9 0.046(2) 0.059(3) 0.053(3) -0.016(2) 0.012(2) -0.017(2) O1 0.069(3) 0.079(3) 0.081(3) -0.027(2) 0.015(2) -0.033(2) O2 0.090(3) 0.072(3) 0.042(2) -0.0104(19) -0.009(2) -0.031(2) O3 0.0411(17) 0.0551(18) 0.0369(15) -0.0125(15) 0.0054(13) -0.0058(13) O4 0.0388(16) 0.0405(15) 0.0486(16) -0.0084(14) 0.0014(13) -0.0086(14) O5 0.088(3) 0.096(4) 0.086(3) -0.050(3) -0.037(3) 0.032(3) O6 0.212(6) 0.212(6) 0.203(8) 0.005(6) -0.005(6) -0.002(8) N2 0.059(2) 0.058(2) 0.048(2) -0.022(2) 0.019(2) -0.025(2) K2 0.116(3) 0.129(3) 0.081(3) 0.006(2) 0.007(2) 0.014(2) O7 0.162(7) 0.162(7) 0.140(10) 0.000 0.000 0.000 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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 Cd1 Cd1 O1 106.1(10) 46_455 29_445 Cd1 Cd1 O4 124.5(19) 46_455 . O1 Cd1 O4 107.93(18) 29_445 . Cd1 Cd1 O3 95.0(15) 46_455 46_455 O1 Cd1 O3 91.6(3) 29_445 46_455 O4 Cd1 O3 126.03(14) . 46_455 Cd1 Cd1 O1 65.7(9) 46_455 15_565 O1 Cd1 O1 73.7(3) 29_445 15_565 O4 Cd1 O1 83.7(2) . 15_565 O3 Cd1 O1 150.1(2) 46_455 15_565 Cd1 Cd1 O3 76.7(15) 46_455 . O1 Cd1 O3 156.9(3) 29_445 . O4 Cd1 O3 55.75(15) . . O3 Cd1 O3 111.17(17) 46_455 . O1 Cd1 O3 87.3(2) 15_565 . Cd1 Cd1 O4 48.9(17) 46_455 46_455 O1 Cd1 O4 81.6(2) 29_445 46_455 O4 Cd1 O4 170.34(18) . 46_455 O3 Cd1 O4 53.79(14) 46_455 46_455 O1 Cd1 O4 97.61(17) 15_565 46_455 O3 Cd1 O4 114.66(14) . 46_455 Cd1 Cd1 C8 100.6(17) 46_455 . O1 Cd1 C8 133.1(2) 29_445 . O4 Cd1 C8 27.52(13) . . O3 Cd1 C8 123.81(13) 46_455 . O1 Cd1 C8 83.6(2) 15_565 . O3 Cd1 C8 28.29(13) . . O4 Cd1 C8 142.93(17) 46_455 . Cd1 Cd1 K2 136.9(13) 46_455 46_455 O1 Cd1 K2 86.89(19) 29_445 46_455 O4 Cd1 K2 87.52(13) . 46_455 O3 Cd1 K2 42.73(12) 46_455 46_455 O1 Cd1 K2 154.93(15) 15_565 46_455 O3 Cd1 K2 106.91(12) . 46_455 O4 Cd1 K2 94.97(17) 46_455 46_455 C8 Cd1 K2 99.09(14) . 46_455 Cd1 Cd1 K2 39.6(12) 46_455 . O1 Cd1 K2 144.03(16) 29_445 . O4 Cd1 K2 91.97(17) . . O3 Cd1 K2 100.62(12) 46_455 . O1 Cd1 K2 79.31(17) 15_565 . O3 Cd1 K2 37.95(11) . . O4 Cd1 K2 78.92(12) 46_455 . C8 Cd1 K2 64.84(14) . . K2 Cd1 K2 124.54(13) 46_455 . Cd1 Cd1 K1 149.6(15) 46_455 . O1 Cd1 K1 73.17(14) 29_445 . O4 Cd1 K1 36.97(8) . . O3 Cd1 K1 115.38(13) 46_455 . O1 Cd1 K1 85.68(15) 15_565 . O3 Cd1 K1 92.70(15) . . O4 Cd1 K1 152.52(17) 46_455 . C8 Cd1 K1 64.48(12) . . K2 Cd1 K1 73.40(9) 46_455 . K2 Cd1 K1 128.30(16) . . Cd1 Cd1 K2 125.4(11) 46_455 48_656 O1 Cd1 K2 96.8(2) 29_445 48_656 O4 Cd1 K2 92.24(13) . 48_656 O3 Cd1 K2 34.56(10) 46_455 48_656 O1 Cd1 K2 167.79(15) 15_565 48_656 O3 Cd1 K2 99.91(11) . 48_656 O4 Cd1 K2 88.34(15) 46_455 48_656 C8 Cd1 K2 98.06(13) . 48_656 K2 Cd1 K2 12.86(11) 46_455 48_656 K2 Cd1 K2 112.42(8) . 48_656 K1 Cd1 K2 84.19(9) . 48_656 O4 K1 O4 174.59(16) . 19_666 O4 K1 O2 115.69(12) . 48_656 O4 K1 O2 68.54(11) 19_666 48_656 O4 K1 O2 68.54(11) . 29_445 O4 K1 O2 115.69(12) 19_666 29_445 O2 K1 O2 88.5(2) 48_656 29_445 O4 K1 O5 71.03(11) . . O4 K1 O5 105.14(11) 19_666 . O2 K1 O5 171.16(13) 48_656 . O2 K1 O5 88.86(16) 29_445 . O4 K1 O5 105.14(11) . 19_666 O4 K1 O5 71.03(11) 19_666 19_666 O2 K1 O5 88.87(16) 48_656 19_666 O2 K1 O5 171.16(13) 29_445 19_666 O5 K1 O5 94.9(3) . 19_666 O4 K1 C1 108.69(12) . 48_656 O4 K1 C1 73.98(11) 19_666 48_656 O2 K1 C1 21.31(13) 48_656 48_656 O2 K1 C1 104.87(15) 29_445 48_656 O5 K1 C1 165.27(18) . 48_656 O5 K1 C1 70.75(17) 19_666 48_656 O4 K1 C1 73.98(11) . 29_445 O4 K1 C1 108.69(12) 19_666 29_445 O2 K1 C1 104.87(15) 48_656 29_445 O2 K1 C1 21.31(13) 29_445 29_445 O5 K1 C1 70.75(17) . 29_445 O5 K1 C1 165.27(18) 19_666 29_445 C1 K1 C1 123.8(2) 48_656 29_445 O4 K1 C7 116.43(10) . 29_445 O4 K1 C7 66.68(10) 19_666 29_445 O2 K1 C7 83.27(11) 48_656 29_445 O2 K1 C7 50.99(10) 29_445 29_445 O5 K1 C7 88.54(15) . 29_445 O5 K1 C7 136.94(11) 19_666 29_445 C1 K1 C7 104.16(12) 48_656 29_445 C1 K1 C7 42.60(11) 29_445 29_445 O4 K1 C7 66.68(10) . 48_656 O4 K1 C7 116.43(10) 19_666 48_656 O2 K1 C7 50.99(10) 48_656 48_656 O2 K1 C7 83.27(11) 29_445 48_656 O5 K1 C7 136.94(11) . 48_656 O5 K1 C7 88.54(15) 19_666 48_656 C1 K1 C7 42.60(11) 48_656 48_656 C1 K1 C7 104.16(12) 29_445 48_656 C7 K1 C7 117.15(14) 29_445 48_656 O4 K1 Cd1 151.63(9) . 19_666 O4 K1 Cd1 30.92(9) 19_666 19_666 O2 K1 Cd1 40.19(12) 48_656 19_666 O2 K1 Cd1 115.41(11) 29_445 19_666 O5 K1 Cd1 134.98(11) . 19_666 O5 K1 Cd1 67.00(10) 19_666 19_666 C1 K1 Cd1 43.09(11) 48_656 19_666 C1 K1 Cd1 120.66(10) 29_445 19_666 C7 K1 Cd1 80.46(8) 29_445 19_666 C7 K1 Cd1 85.52(10) 48_656 19_666 O4 K1 Cd1 30.92(9) . . O4 K1 Cd1 151.64(9) 19_666 . O2 K1 Cd1 115.41(11) 48_656 . O2 K1 Cd1 40.19(12) 29_445 . O5 K1 Cd1 67.00(10) . . O5 K1 Cd1 134.98(11) 19_666 . C1 K1 Cd1 120.66(10) 48_656 . C1 K1 Cd1 43.09(11) 29_445 . C7 K1 Cd1 85.52(10) 29_445 . C7 K1 Cd1 80.46(8) 48_656 . Cd1 K1 Cd1 152.95(13) 19_666 . C9 N1 C4 130.9(4) . . C9 N1 H1A 114.6 . . C4 N1 H1A 114.6 . . O2 C1 O1 120.8(5) . . O2 C1 C2 120.5(5) . . O1 C1 C2 118.4(5) . . O2 C1 K1 54.7(3) . 33_545 O1 C1 K1 120.6(4) . 33_545 C2 C1 K1 90.2(3) . 33_545 C3 C2 C7 120.1(4) . . C3 C2 C1 121.1(4) . . C7 C2 C1 118.6(4) . . C2 C3 C4 120.4(4) . . C2 C3 H3A 119.8 . . C4 C3 H3A 119.8 . . C5 C4 C3 119.3(4) . . C5 C4 N1 115.6(4) . . C3 C4 N1 124.8(4) . . C4 C5 C6 120.8(4) . . C4 C5 H5A 119.6 . . C6 C5 H5A 119.6 . . C7 C6 C5 118.4(4) . . C7 C6 C8 122.0(4) . . C5 C6 C8 119.4(4) . . C6 C7 C2 120.9(4) . . C6 C7 K1 126.0(3) . 33_545 C2 C7 K1 81.9(3) . 33_545 C6 C7 H7A 119.6 . . C2 C7 H7A 119.6 . . K1 C7 H7A 63.1 33_545 . O4 C8 O3 121.6(4) . . O4 C8 C6 119.7(4) . . O3 C8 C6 118.7(4) . . O4 C8 Cd1 57.5(2) . . O3 C8 Cd1 64.2(2) . . C6 C8 Cd1 175.7(3) . . N2 C9 N1 120.9(5) . . N2 C9 N2 125.8(5) . 12_665 N1 C9 N2 113.3(4) . 12_665 C1 O1 Cd1 103.0(4) . 33_545 C1 O1 Cd1 111.2(4) . 16_655 Cd1 O1 Cd1 8.16(13) 33_545 16_655 C1 O2 K2 137.8(4) . 16_655 C1 O2 K1 103.9(4) . 33_545 K2 O2 K1 117.99(18) 16_655 33_545 C8 O3 Cd1 94.5(3) . 46_455 C8 O3 Cd1 87.5(3) . . Cd1 O3 Cd1 8.32(13) 46_455 . C8 O3 K2 154.4(3) . . Cd1 O3 K2 97.06(17) 46_455 . Cd1 O3 K2 105.25(17) . . C8 O3 K2 150.2(3) . 3_657 Cd1 O3 K2 114.61(17) 46_455 3_657 Cd1 O3 K2 122.02(17) . 3_657 K2 O3 K2 23.30(19) . 3_657 C8 O4 Cd1 95.0(3) . . C8 O4 Cd1 89.4(3) . 46_455 Cd1 O4 Cd1 6.7(2) . 46_455 C8 O4 K1 152.9(3) . . Cd1 O4 K1 112.11(14) . . Cd1 O4 K1 117.59(14) 46_455 . K2 O6 K2 167.1(10) 13_557 . K2 O6 K2 170.8(3) 13_557 3_657 K2 O6 K2 17.16(17) . 3_657 K2 O6 K2 17.15(17) 13_557 15_565 K2 O6 K2 170.8(3) . 15_565 K2 O6 K2 163.9(8) 3_657 15_565 C9 N2 C9 114.2(5) . 6_566 K2 K2 O6 122.3(5) 3_657 . K2 K2 O3 85.5(4) 3_657 . O6 K2 O3 147.9(3) . . K2 K2 O3 71.2(3) 3_657 3_657 O6 K2 O3 122.5(3) . 3_657 O3 K2 O3 79.1(2) . 3_657 K2 K2 O2 162.7(3) 3_657 15_565 O6 K2 O2 75.0(4) . 15_565 O3 K2 O2 77.94(18) . 15_565 O3 K2 O2 100.5(2) 3_657 15_565 K2 K2 O6 40.6(4) 3_657 3_657 O6 K2 O6 91.2(9) . 3_657 O3 K2 O6 103.7(4) . 3_657 O3 K2 O6 110.1(3) 3_657 3_657 O2 K2 O6 149.1(3) 15_565 3_657 K2 K2 Cd1 115.96(15) 3_657 46_455 O6 K2 Cd1 121.0(5) . 46_455 O3 K2 Cd1 40.20(12) . 46_455 O3 K2 Cd1 68.12(15) 3_657 46_455 O2 K2 Cd1 47.14(12) 15_565 46_455 O6 K2 Cd1 143.8(4) 3_657 46_455 K2 K2 Cd1 112.88(16) 3_657 . O6 K2 Cd1 124.3(5) . . O3 K2 Cd1 36.79(12) . . O3 K2 Cd1 67.82(14) 3_657 . O2 K2 Cd1 50.10(12) 15_565 . O6 K2 Cd1 140.3(4) 3_657 . Cd1 K2 Cd1 3.54(10) 46_455 . K2 K2 Cd1 51.19(13) 3_657 48_656 O6 K2 Cd1 150.4(2) . 48_656 O3 K2 Cd1 58.80(13) . 48_656 O3 K2 Cd1 30.82(10) 3_657 48_656 O2 K2 Cd1 114.37(18) 15_565 48_656 O6 K2 Cd1 91.3(4) 3_657 48_656 Cd1 K2 Cd1 69.12(10) 46_455 48_656 Cd1 K2 Cd1 66.93(8) . 48_656 K2 K2 K2 127.6(3) 3_657 13_557 O6 K2 K2 6.5(5) . 13_557 O3 K2 K2 144.84(19) . 13_557 O3 K2 K2 119.19(19) 3_657 13_557 O2 K2 K2 69.58(14) 15_565 13_557 O6 K2 K2 97.6(4) 3_657 13_557 Cd1 K2 K2 114.99(9) 46_455 13_557 Cd1 K2 K2 118.36(9) . 13_557 Cd1 K2 K2 148.75(18) 48_656 13_557 K2 K2 K1 149.9(5) 3_657 34_546 O6 K2 K1 67.1(5) . 34_546 O3 K2 K1 97.54(15) . 34_546 O3 K2 K1 80.01(14) 3_657 34_546 O2 K2 K1 31.78(11) 15_565 34_546 O6 K2 K1 157.8(4) 3_657 34_546 Cd1 K2 K1 57.90(9) 46_455 34_546 Cd1 K2 K1 61.43(9) . 34_546 Cd1 K2 K1 105.30(11) 48_656 34_546 K2 K2 K1 60.61(6) 13_557 34_546 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cd1 Cd1 0.351(5) 46_455 Cd1 O1 2.252(5) 29_445 Cd1 O4 2.268(6) . Cd1 O3 2.358(5) 46_455 Cd1 O1 2.374(5) 15_565 Cd1 O3 2.414(5) . Cd1 O4 2.483(5) 46_455 Cd1 C8 2.678(7) . Cd1 K2 3.626(6) 46_455 Cd1 K2 3.889(6) . Cd1 K1 4.089(3) . Cd1 K2 4.184(5) 48_656 K1 O4 2.654(3) . K1 O4 2.654(3) 19_666 K1 O2 2.759(5) 48_656 K1 O2 2.759(5) 29_445 K1 O5 2.942(5) . K1 O5 2.942(5) 19_666 K1 C1 3.279(6) 48_656 K1 C1 3.279(6) 29_445 K1 C7 3.531(5) 29_445 K1 C7 3.531(5) 48_656 K1 Cd1 4.089(3) 19_666 N1 C9 1.346(6) . N1 C4 1.412(6) . N1 H1A 0.8600 . C1 O2 1.228(7) . C1 O1 1.245(7) . C1 C2 1.495(7) . C1 K1 3.279(6) 33_545 C2 C3 1.386(6) . C2 C7 1.393(7) . C3 C4 1.397(6) . C3 H3A 0.9300 . C4 C5 1.393(6) . C5 C6 1.413(6) . C5 H5A 0.9300 . C6 C7 1.391(6) . C6 C8 1.486(6) . C7 K1 3.531(5) 33_545 C7 H7A 0.9300 . C8 O4 1.242(5) . C8 O3 1.270(5) . C9 N2 1.342(6) . C9 N2 1.353(6) 12_665 O1 Cd1 2.252(5) 33_545 O1 Cd1 2.374(5) 16_655 O2 K2 2.637(6) 16_655 O2 K1 2.759(5) 33_545 O3 Cd1 2.358(5) 46_455 O3 K2 2.479(6) . O3 K2 2.611(6) 3_657 O4 Cd1 2.483(5) 46_455 O6 K2 2.284(5) 13_557 O6 K2 2.284(5) . O6 K2 2.969(6) 3_657 O6 K2 2.969(6) 15_565 N2 C9 1.353(6) 6_566 K2 K2 1.036(8) 3_657 K2 O3 2.611(6) 3_657 K2 O2 2.637(6) 15_565 K2 O6 2.969(6) 3_657 K2 Cd1 3.626(6) 46_455 K2 Cd1 4.184(5) 48_656 K2 K2 4.539(9) 13_557 K2 K1 4.625(5) 34_546 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 0.000 0.000 0.000 4802 786 ' ' 2 0.500 0.500 0.500 4802 786 ' '