#------------------------------------------------------------------------------ #$Date: 2023-11-22 01:37:46 +0200 (Wed, 22 Nov 2023) $ #$Revision: 287712 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/77/7247755.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_7247755 loop_ _publ_author_name 'Zhang, Lingfeng' 'Wang, Yu' 'Wang, Yefeng' 'Liu, Shuai' 'Zhang, Na' 'Yang, Mingmin' 'Ma, Haixia' 'Guo, Zhaoqi' _publ_section_title ; N-methylene-C bridged tetrazole and 1,2,4-triazole energetic salts as promising primary explosives ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D3CE01051A _journal_year 2023 _chemical_formula_moiety 'C4 H6 K2 N11 O6' _chemical_formula_sum 'C4 H6 K2 N11 O6' _chemical_formula_weight 382.40 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2021-03-20 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-05-20 deposited with the CCDC. 2023-11-21 downloaded from the CCDC. ; _cell_angle_alpha 96.88(2) _cell_angle_beta 90.38(4) _cell_angle_gamma 95.16(3) _cell_formula_units_Z 2 _cell_length_a 4.0899(18) _cell_length_b 8.238(5) _cell_length_c 20.690(11) _cell_measurement_reflns_used 9310 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 54.86 _cell_measurement_theta_min 3.74 _cell_volume 689.2(6) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _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_temperature 173(2) _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34139 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_unetI/netI 0.0303 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 11667 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.985 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 55.167 _diffrn_reflns_theta_min 3.745 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 4.359 _exptl_absorpt_correction_T_max 0.7508 _exptl_absorpt_correction_T_min 0.5252 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1634 before and 0.0623 after correction. The Ratio of minimum to maximum transmission is 0.6995. The \l/2 correction factor is Not present. ; _exptl_crystal_colour clear _exptl_crystal_colour_lustre clear _exptl_crystal_density_diffrn 1.843 _exptl_crystal_description block _exptl_crystal_F_000 386 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.772 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.060 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 224 _refine_ls_number_reflns 2586 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.075 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0281 _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^)+(0.0470P)^2^+0.2804P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0802 _refine_ls_wR_factor_ref 0.0811 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2468 _reflns_number_total 2586 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce01051a2.cif _cod_data_source_block 20210312fl_0m_a _cod_database_code 7247755 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.918 _shelx_estimated_absorpt_t_min 0.812 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups 2.a Secondary CH2 refined with riding coordinates: C00N(H00C,H00D) ; _shelx_res_file ; TITL 20210312fl_0m_a_a.res in P-1 20210312fl_0m_a.res created by SHELXL-2018/3 at 11:48:07 on 20-Mar-2021 REM Old TITL 20210312fL_0m_a.res in P-1 REM SHELXT solution in P-1 REM R1 0.118, Rweak 0.006, Alpha 0.027, Orientation as input REM Formula found by SHELXT: C15 O2 O4 Cl2 CELL 1.34139 4.0899 8.2378 20.6902 96.876 90.375 95.16 ZERR 2 0.0018 0.0046 0.0111 0.022 0.038 0.029 LATT 1 SFAC C H K N O DISP C 0.0148 0.007 57.7477 DISP H -0 0 0.6481 DISP K 0.3891 0.8535 6202.7055 DISP N 0.0253 0.0136 110.5121 DISP O 0.0412 0.025 193.9543 UNIT 8 12 4 22 12 L.S. 10 PLAN 20 SIZE 0.05 0.02 0.02 TEMP -100.15 MPLA N9 N10 N11 MPLA N12 N13 N14 N15 BOND $H list 4 fmap 2 acta REM REM REM WGHT 0.047000 0.280400 FVAR 1.19926 K2 3 0.869971 0.854207 0.587173 11.00000 0.01913 0.01635 = 0.01614 0.00070 0.00026 0.00358 K1 3 0.446553 -0.221087 0.065263 11.00000 0.03521 0.02767 = 0.01815 0.00320 0.00321 0.01664 O003 5 0.568901 0.907945 0.371558 11.00000 0.02574 0.01322 = 0.02033 0.00339 -0.00103 0.00268 O2 5 1.317234 0.651233 0.543274 11.00000 0.02704 0.01859 = 0.01747 0.00308 0.00264 0.00597 O005 5 0.840531 0.848038 0.454872 11.00000 0.03313 0.02572 = 0.01565 0.00035 -0.00887 -0.00833 O006 5 0.907276 -0.388201 0.118473 11.00000 0.04788 0.02219 = 0.02285 0.00249 -0.00854 0.00997 O6 5 0.066432 0.310262 0.027972 11.00000 0.04804 0.03190 = 0.01776 0.00915 0.00169 0.01916 N12 4 -0.039329 0.168778 0.229161 11.00000 0.01872 0.01271 = 0.01311 -0.00051 -0.00166 0.00210 N11 4 0.012898 0.583546 0.257464 11.00000 0.02348 0.01634 = 0.01613 0.00111 -0.00374 0.00380 N9 4 0.158024 0.449790 0.340633 11.00000 0.01792 0.01349 = 0.01367 0.00076 -0.00032 0.00295 N10 4 0.219895 0.683644 0.299492 11.00000 0.02218 0.01390 = 0.01526 0.00127 -0.00403 0.00303 N8 4 0.640163 0.805253 0.408424 11.00000 0.02083 0.01504 = 0.01311 -0.00032 0.00214 0.00109 N7 4 0.516066 0.651494 0.401284 11.00000 0.02103 0.01286 = 0.01480 0.00121 -0.00189 0.00182 O00E 5 0.281278 0.090509 0.047952 11.00000 0.06543 0.03524 = 0.02232 0.00713 0.01435 0.03225 N15 4 0.248394 0.003795 0.168707 11.00000 0.02910 0.01524 = 0.01551 0.00150 -0.00069 0.00634 N16 4 0.006941 0.238085 0.125061 11.00000 0.03242 0.02181 = 0.01348 0.00211 0.00165 0.01295 N14 4 0.232614 -0.035510 0.230584 11.00000 0.03053 0.01479 = 0.01714 0.00248 -0.00128 0.00354 N13 4 0.061990 0.062134 0.267285 11.00000 0.02559 0.01394 = 0.01659 0.00304 -0.00123 0.00072 N17 4 0.123302 0.208018 0.066290 11.00000 0.03414 0.02302 = 0.01609 0.00326 0.00082 0.01166 C00K 1 0.305928 0.602632 0.348625 11.00000 0.01638 0.01265 = 0.01236 0.00079 0.00147 0.00544 C00L 1 -0.017894 0.447164 0.284630 11.00000 0.01557 0.01516 = 0.01356 -0.00015 0.00117 0.00579 C00M 1 0.077767 0.134271 0.168777 11.00000 0.01905 0.01541 = 0.01445 -0.00080 -0.00177 0.00271 C00N 1 -0.231850 0.301689 0.254903 11.00000 0.01637 0.01832 = 0.01677 -0.00148 0.00040 0.00467 AFIX 23 H00C 2 -0.383218 0.262867 0.288108 11.00000 -1.20000 H00D 2 -0.365931 0.333593 0.219278 11.00000 -1.20000 AFIX 0 H2A 2 1.307193 0.565055 0.558006 11.00000 0.04728 H2B 2 1.321341 0.636424 0.504100 11.00000 0.04159 H00A 2 0.939086 -0.388656 0.159804 11.00000 0.04802 H00B 2 0.925523 -0.483921 0.101514 11.00000 0.07235 HKLF 4 REM 20210312fl_0m_a_a.res in P-1 REM wR2 = 0.0811, GooF = S = 1.075, Restrained GooF = 1.075 for all data REM R1 = 0.0281 for 2468 Fo > 4sig(Fo) and 0.0293 for all 2586 data REM 224 parameters refined using 0 restraints END WGHT 0.0408 0.3648 REM Highest difference peak 0.772, deepest hole -0.374, 1-sigma level 0.060 Q1 1 0.2886 0.7828 0.2903 11.00000 0.05 0.77 Q2 1 -0.1139 0.3681 0.2726 11.00000 0.05 0.32 Q3 1 -0.1195 0.2332 0.2433 11.00000 0.05 0.26 Q4 1 0.0857 0.4396 0.3114 11.00000 0.05 0.24 Q5 1 0.2792 0.6527 0.3210 11.00000 0.05 0.23 Q6 1 0.3344 -0.3332 0.0585 11.00000 0.05 0.22 Q7 1 0.6243 0.5804 0.4183 11.00000 0.05 0.21 Q8 1 0.0064 0.1213 0.2505 11.00000 0.05 0.21 Q9 1 0.0357 0.4956 0.2677 11.00000 0.05 0.20 Q10 1 0.7455 -0.3042 0.1035 11.00000 0.05 0.19 Q11 1 0.2325 0.5252 0.3459 11.00000 0.05 0.19 Q12 1 0.3305 -0.1016 0.2510 11.00000 0.05 0.19 Q13 1 0.1100 0.6411 0.2792 11.00000 0.05 0.19 Q14 1 -0.2282 0.2489 0.0293 11.00000 0.05 0.19 Q15 1 0.7444 0.9394 0.5644 11.00000 0.05 0.19 Q16 1 -0.0657 0.5107 0.2783 11.00000 0.05 0.19 Q17 1 0.2237 0.0838 0.1670 11.00000 0.05 0.18 Q18 1 0.2399 -0.0121 0.1966 11.00000 0.05 0.18 Q19 1 0.5506 -0.3259 0.0946 11.00000 0.05 0.18 Q20 1 0.0028 0.0692 0.3008 11.00000 0.05 0.18 ; _shelx_res_checksum 32756 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 K2 K 0.86997(8) 0.85421(4) 0.58717(2) 0.01719(12) Uani 1 1 d . . . . . K1 K 0.44655(10) -0.22109(5) 0.06526(2) 0.02613(13) Uani 1 1 d . . . . . O003 O 0.5689(3) 0.90794(13) 0.37156(6) 0.0196(3) Uani 1 1 d . . . . . O2 O 1.3172(3) 0.65123(15) 0.54327(7) 0.0207(3) Uani 1 1 d . . . . . O005 O 0.8405(3) 0.84804(15) 0.45487(6) 0.0257(3) Uani 1 1 d . . . . . O006 O 0.9073(4) -0.38820(17) 0.11847(7) 0.0306(3) Uani 1 1 d . . . . . O6 O 0.0664(4) 0.31026(17) 0.02797(6) 0.0311(3) Uani 1 1 d . . . . . N12 N -0.0393(3) 0.16878(16) 0.22916(6) 0.0150(3) Uani 1 1 d . . . . . N11 N 0.0129(3) 0.58355(16) 0.25746(7) 0.0186(3) Uani 1 1 d . . . . . N9 N 0.1580(3) 0.44979(16) 0.34063(6) 0.0150(3) Uani 1 1 d . . . . . N10 N 0.2199(3) 0.68364(16) 0.29949(6) 0.0171(3) Uani 1 1 d . . . . . N8 N 0.6402(3) 0.80525(16) 0.40842(6) 0.0165(3) Uani 1 1 d . . . . . N7 N 0.5161(3) 0.65149(16) 0.40128(6) 0.0163(3) Uani 1 1 d . . . . . O00E O 0.2813(4) 0.09051(18) 0.04795(6) 0.0390(4) Uani 1 1 d . . . . . N15 N 0.2484(4) 0.00379(16) 0.16871(7) 0.0197(3) Uani 1 1 d . . . . . N16 N 0.0069(4) 0.23809(17) 0.12506(7) 0.0219(3) Uani 1 1 d . . . . . N14 N 0.2326(4) -0.03551(16) 0.23058(7) 0.0207(3) Uani 1 1 d . . . . . N13 N 0.0620(4) 0.06213(16) 0.26729(7) 0.0187(3) Uani 1 1 d . . . . . N17 N 0.1233(4) 0.20802(18) 0.06629(7) 0.0238(3) Uani 1 1 d . . . . . C00K C 0.3059(4) 0.60263(18) 0.34863(7) 0.0136(3) Uani 1 1 d . . . . . C00L C -0.0179(4) 0.44716(19) 0.28463(7) 0.0146(3) Uani 1 1 d . . . . . C00M C 0.0778(4) 0.13427(19) 0.16878(8) 0.0165(3) Uani 1 1 d . . . . . C00N C -0.2318(4) 0.3017(2) 0.25490(8) 0.0173(3) Uani 1 1 d . . . . . H00C H -0.383218 0.262867 0.288108 0.021 Uiso 1 1 calc R . . . . H00D H -0.365931 0.333593 0.219278 0.021 Uiso 1 1 calc R . . . . H2A H 1.307(7) 0.565(4) 0.5580(14) 0.047(8) Uiso 1 1 d . . . . . H2B H 1.321(6) 0.636(3) 0.5041(14) 0.042(7) Uiso 1 1 d . . . . . H00A H 0.939(7) -0.389(3) 0.1598(15) 0.048(7) Uiso 1 1 d . . . . . H00B H 0.926(9) -0.484(5) 0.1015(17) 0.072(10) Uiso 1 1 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 K2 0.0191(2) 0.01635(19) 0.01614(19) 0.00070(13) 0.00026(13) 0.00358(13) K1 0.0352(2) 0.0277(2) 0.0182(2) 0.00320(15) 0.00321(16) 0.01664(17) O003 0.0257(6) 0.0132(5) 0.0203(6) 0.0034(4) -0.0010(5) 0.0027(4) O2 0.0270(7) 0.0186(6) 0.0175(7) 0.0031(5) 0.0026(5) 0.0060(5) O005 0.0331(7) 0.0257(6) 0.0157(6) 0.0003(5) -0.0089(5) -0.0083(5) O006 0.0479(9) 0.0222(7) 0.0229(7) 0.0025(5) -0.0085(6) 0.0100(6) O6 0.0480(8) 0.0319(7) 0.0178(6) 0.0091(5) 0.0017(6) 0.0192(6) N12 0.0187(7) 0.0127(6) 0.0131(6) -0.0005(5) -0.0017(5) 0.0021(5) N11 0.0235(7) 0.0163(7) 0.0161(7) 0.0011(5) -0.0037(5) 0.0038(5) N9 0.0179(7) 0.0135(6) 0.0137(6) 0.0008(5) -0.0003(5) 0.0030(5) N10 0.0222(7) 0.0139(6) 0.0153(7) 0.0013(5) -0.0040(5) 0.0030(5) N8 0.0208(7) 0.0150(6) 0.0131(6) -0.0003(5) 0.0021(5) 0.0011(5) N7 0.0210(7) 0.0129(6) 0.0148(7) 0.0012(5) -0.0019(5) 0.0018(5) O00E 0.0654(10) 0.0352(8) 0.0223(7) 0.0071(6) 0.0143(7) 0.0323(7) N15 0.0291(8) 0.0152(7) 0.0155(7) 0.0015(5) -0.0007(6) 0.0063(6) N16 0.0324(8) 0.0218(7) 0.0135(7) 0.0021(5) 0.0017(6) 0.0129(6) N14 0.0305(8) 0.0148(7) 0.0171(7) 0.0025(5) -0.0013(6) 0.0035(6) N13 0.0256(8) 0.0139(6) 0.0166(7) 0.0030(5) -0.0012(6) 0.0007(5) N17 0.0341(9) 0.0230(7) 0.0161(7) 0.0033(6) 0.0008(6) 0.0117(6) C00K 0.0164(8) 0.0126(7) 0.0124(7) 0.0008(5) 0.0015(6) 0.0054(6) C00L 0.0156(8) 0.0152(7) 0.0136(7) -0.0002(6) 0.0012(6) 0.0058(6) C00M 0.0190(8) 0.0154(7) 0.0145(7) -0.0008(6) -0.0018(6) 0.0027(6) C00N 0.0164(8) 0.0183(8) 0.0168(8) -0.0015(6) 0.0004(6) 0.0047(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0148 0.0070 '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' K K 0.3891 0.8535 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0412 0.0250 '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 K2 K2 K2 79.19(3) 1_655 2_776 ? K2 K2 K2 100.81(3) 1_455 2_776 ? K2 K2 K2 180.0 1_455 1_655 ? K2 K2 H2B 49.0(5) 1_655 . ? K2 K2 H2B 131.0(5) 1_455 . ? K2 K2 H2B 76.2(5) 2_776 . ? O003 K2 K2 134.19(3) 2_676 1_655 ? O003 K2 K2 72.78(4) 2_776 2_776 ? O003 K2 K2 87.96(4) 2_676 2_776 ? O003 K2 K2 45.81(4) 2_676 1_455 ? O003 K2 K2 43.90(3) 2_776 1_655 ? O003 K2 K2 136.10(3) 2_776 1_455 ? O003 K2 O003 90.29(5) 2_676 2_776 ? O003 K2 O005 75.27(5) 2_676 2_776 ? O003 K2 N9 116.61(5) 2_676 2_666 ? O003 K2 N9 112.77(5) 2_776 2_666 ? O003 K2 N8 79.13(5) 2_676 2_776 ? O003 K2 N8 22.37(4) 2_776 2_776 ? O003 K2 N13 71.29(5) 2_676 2_666 ? O003 K2 N13 66.34(5) 2_776 2_666 ? O003 K2 H2B 163.1(5) 2_676 . ? O003 K2 H2B 90.6(5) 2_776 . ? O2 K2 K2 137.84(4) . 1_455 ? O2 K2 K2 87.42(5) . 2_776 ? O2 K2 K2 103.51(5) 1_455 2_776 ? O2 K2 K2 42.16(4) . 1_655 ? O2 K2 K2 139.49(3) 1_455 1_655 ? O2 K2 K2 40.51(3) 1_455 1_455 ? O2 K2 O003 85.94(5) . 2_776 ? O2 K2 O003 174.74(4) . 2_676 ? O2 K2 O003 86.20(5) 1_455 2_676 ? O2 K2 O003 175.01(4) 1_455 2_776 ? O2 K2 O2 97.33(6) . 1_455 ? O2 K2 O005 131.31(5) 1_455 2_776 ? O2 K2 O005 75.61(5) . . ? O2 K2 O005 99.47(6) . 2_776 ? O2 K2 N9 72.04(5) 1_455 2_666 ? O2 K2 N9 68.35(5) . 2_666 ? O2 K2 N8 152.77(4) 1_455 2_776 ? O2 K2 N8 96.09(5) . 2_776 ? O2 K2 N13 110.35(5) . 2_666 ? O2 K2 N13 115.65(5) 1_455 2_666 ? O2 K2 H2B 14.0(5) . . ? O2 K2 H2B 91.7(5) 1_455 . ? O005 K2 K2 109.81(4) 2_776 1_455 ? O005 K2 K2 70.19(4) 2_776 1_655 ? O005 K2 K2 87.95(5) . 1_455 ? O005 K2 K2 92.05(5) . 1_655 ? O005 K2 K2 34.72(3) . 2_776 ? O005 K2 K2 32.99(3) 2_776 2_776 ? O005 K2 O003 104.39(5) . 2_776 ? O005 K2 O003 44.07(4) 2_776 2_776 ? O005 K2 O003 101.85(5) . 2_676 ? O005 K2 O2 72.94(5) . 1_455 ? O005 K2 O005 67.71(5) . 2_776 ? O005 K2 N9 156.07(4) 2_776 2_666 ? O005 K2 N9 124.92(4) . 2_666 ? O005 K2 N8 87.69(5) . 2_776 ? O005 K2 N8 22.18(4) 2_776 2_776 ? O005 K2 N13 100.49(5) 2_776 2_666 ? O005 K2 N13 167.85(4) . 2_666 ? O005 K2 H2B 93.9(5) 2_776 . ? O005 K2 H2B 61.7(5) . . ? N9 K2 K2 154.09(3) 2_666 2_776 ? N9 K2 K2 91.89(4) 2_666 1_455 ? N9 K2 K2 88.11(4) 2_666 1_655 ? N9 K2 N8 135.13(5) 2_666 2_776 ? N9 K2 H2B 78.4(5) 2_666 . ? N8 K2 K2 57.84(4) 2_776 1_655 ? N8 K2 K2 122.16(4) 2_776 1_455 ? N8 K2 K2 53.58(4) 2_776 2_776 ? N8 K2 H2B 95.8(5) 2_776 . ? N13 K2 K2 93.74(5) 2_666 1_455 ? N13 K2 K2 86.26(5) 2_666 1_655 ? N13 K2 K2 133.42(4) 2_666 2_776 ? N13 K2 N9 67.09(5) 2_666 2_666 ? N13 K2 N8 81.22(5) 2_666 2_776 ? N13 K2 H2B 124.2(5) 2_666 . ? K1 K1 K1 180.0 1_655 1_455 ? K1 K1 K1 91.53(3) 1_455 2_655 ? K1 K1 K1 88.47(3) 1_655 2_655 ? O006 K1 K1 133.17(4) 1_455 2_655 ? O006 K1 K1 131.34(4) . 2_655 ? O006 K1 K1 41.67(4) 1_455 1_455 ? O006 K1 K1 138.33(4) 1_455 1_655 ? O006 K1 K1 137.10(4) . 1_455 ? O006 K1 K1 42.90(4) . 1_655 ? O006 K1 O006 95.43(6) . 1_455 ? O006 K1 O6 135.05(5) 1_455 2_655 ? O006 K1 O6 134.20(5) . 2 ? O006 K1 O6 69.02(5) . 2_655 ? O006 K1 O6 68.67(5) 1_455 2 ? O006 K1 O00E 146.67(5) 1_455 2_655 ? O006 K1 O00E 143.69(5) . . ? O006 K1 O00E 108.62(6) . 2_655 ? O006 K1 N15 105.36(6) . . ? O006 K1 N15 75.32(6) 1_455 . ? O006 K1 N17 90.46(5) . 2_655 ? O006 K1 N17 143.26(5) 1_455 2_655 ? O6 K1 K1 135.58(4) 2 1_655 ? O6 K1 K1 75.51(4) 2_655 2_655 ? O6 K1 K1 77.58(4) 2 2_655 ? O6 K1 K1 43.70(4) 2_655 1_655 ? O6 K1 K1 136.30(4) 2_655 1_455 ? O6 K1 K1 44.42(4) 2 1_455 ? O6 K1 O6 91.88(5) 2 2_655 ? O6 K1 O00E 78.00(6) 2 2_655 ? O6 K1 O00E 44.24(5) 2_655 2_655 ? O6 K1 N15 110.92(5) 2 . ? O6 K1 N17 81.34(6) 2 2_655 ? O6 K1 N17 22.57(4) 2_655 2_655 ? O00E K1 K1 70.98(5) . 1_455 ? O00E K1 K1 109.02(5) . 1_655 ? O00E K1 K1 31.68(3) 2_655 2_655 ? O00E K1 K1 110.98(5) 2_655 1_455 ? O00E K1 K1 69.02(5) 2_655 1_655 ? O00E K1 K1 33.05(3) . 2_655 ? O00E K1 O006 108.08(5) . 1_455 ? O00E K1 O6 81.12(5) . 2 ? O00E K1 O6 108.24(5) . 2_655 ? O00E K1 O00E 64.73(5) . 2_655 ? O00E K1 N15 57.12(5) . . ? O00E K1 N17 22.14(4) 2_655 2_655 ? O00E K1 N17 86.86(5) . 2_655 ? N15 K1 K1 110.49(5) . 1_655 ? N15 K1 K1 88.09(5) . 2_655 ? N15 K1 K1 69.51(5) . 1_455 ? N15 K1 O6 148.48(5) . 2_655 ? N15 K1 O00E 117.87(5) . 2_655 ? N15 K1 N17 137.51(5) . 2_655 ? N17 K1 K1 53.81(4) 2_655 2_655 ? N17 K1 K1 57.15(4) 2_655 1_655 ? N17 K1 K1 122.85(4) 2_655 1_455 ? K2 O003 K2 90.29(5) 2_676 2_776 ? N8 O003 K2 120.39(9) . 2_676 ? N8 O003 K2 94.98(9) . 2_776 ? K2 O2 K2 97.33(5) . 1_655 ? K2 O2 H2A 112(2) 1_655 . ? K2 O2 H2A 115(2) . . ? K2 O2 H2B 112.6(19) . . ? K2 O2 H2B 108.1(19) 1_655 . ? H2A O2 H2B 110(3) . . ? K2 O005 K2 112.29(5) . 2_776 ? N8 O005 K2 139.34(10) . . ? N8 O005 K2 98.52(9) . 2_776 ? K1 O006 K1 95.43(6) . 1_655 ? K1 O006 H00A 110.0(18) 1_655 . ? K1 O006 H00A 124.5(18) . . ? K1 O006 H00B 101(2) 1_655 . ? K1 O006 H00B 117(2) . . ? H00A O006 H00B 106(3) . . ? K1 O6 K1 91.88(5) 2 2_655 ? N17 O6 K1 96.58(10) . 2_655 ? N17 O6 K1 117.68(12) . 2 ? N13 N12 C00M 109.16(13) . . ? N13 N12 C00N 121.38(13) . . ? C00M N12 C00N 129.40(14) . . ? C00L N11 N10 102.65(14) . . ? C00K N9 K2 137.27(11) . 2_666 ? C00K N9 C00L 102.44(13) . . ? C00L N9 K2 120.29(10) . 2_666 ? C00K N10 N11 109.80(13) . . ? O003 N8 K2 62.66(8) . 2_776 ? O003 N8 N7 123.46(14) . . ? O005 N8 K2 59.30(8) . 2_776 ? O005 N8 O003 119.89(13) . . ? O005 N8 N7 116.65(13) . . ? N7 N8 K2 164.61(10) . 2_776 ? N8 N7 C00K 116.68(13) . . ? K1 O00E K1 115.27(5) . 2_655 ? N17 O00E K1 96.31(11) . 2_655 ? N17 O00E K1 148.35(12) . . ? N14 N15 K1 121.11(10) . . ? C00M N15 K1 131.26(11) . . ? C00M N15 N14 105.18(13) . . ? N17 N16 C00M 116.73(14) . . ? N13 N14 N15 111.84(13) . . ? N12 N13 K2 121.76(10) . 2_666 ? N14 N13 K2 126.72(11) . 2_666 ? N14 N13 N12 105.97(13) . . ? O6 N17 K1 60.84(9) . 2_655 ? O6 N17 N16 115.19(14) . . ? O00E N17 K1 61.55(9) . 2_655 ? O00E N17 O6 120.31(15) . . ? O00E N17 N16 124.50(14) . . ? N16 N17 K1 164.07(12) . 2_655 ? N9 C00K N10 109.76(14) . . ? N9 C00K N7 119.50(14) . . ? N10 C00K N7 130.73(14) . . ? N11 C00L N9 115.35(15) . . ? N11 C00L C00N 121.19(15) . . ? N9 C00L C00N 123.46(14) . . ? N12 C00M N16 115.84(14) . . ? N15 C00M N12 107.84(14) . . ? N15 C00M N16 136.28(15) . . ? N12 C00N C00L 111.47(13) . . ? N12 C00N H00C 109.3 . . ? N12 C00N H00D 109.3 . . ? C00L C00N H00C 109.3 . . ? C00L C00N H00D 109.3 . . ? H00C C00N H00D 108.0 . . ? 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 K2 K2 4.0899(18) 1_455 ? K2 K2 4.0899(18) 1_655 ? K2 K2 4.645(2) 2_776 ? K2 O003 2.8358(17) 2_676 ? K2 O003 2.9326(18) 2_776 ? K2 O2 2.7678(18) 1_455 ? K2 O2 2.6787(17) . ? K2 O005 2.8596(19) 2_776 ? K2 O005 2.7334(19) . ? K2 N9 3.0597(19) 2_666 ? K2 N8 3.289(2) 2_776 ? K2 N13 3.013(2) 2_666 ? K2 H2B 3.08(3) . ? K1 K1 4.0899(18) 1_455 ? K1 K1 4.0899(18) 1_655 ? K1 K1 4.779(2) 2_655 ? K1 O006 2.7965(19) 1_455 ? K1 O006 2.7313(18) . ? K1 O6 2.8640(19) 2_655 ? K1 O6 2.827(2) 2 ? K1 O00E 2.8819(19) 2_655 ? K1 O00E 2.775(2) . ? K1 N15 2.8307(19) . ? K1 N17 3.258(2) 2_655 ? O003 N8 1.2563(18) . ? O2 H2A 0.80(3) . ? O2 H2B 0.81(3) . ? O005 N8 1.255(2) . ? O006 H00A 0.86(3) . ? O006 H00B 0.83(4) . ? O6 N17 1.259(2) . ? N12 N13 1.3390(19) . ? N12 C00M 1.348(2) . ? N12 C00N 1.457(2) . ? N11 N10 1.359(2) . ? N11 C00L 1.312(2) . ? N9 C00K 1.338(2) . ? N9 C00L 1.357(2) . ? N10 C00K 1.343(2) . ? N8 N7 1.312(2) . ? N7 C00K 1.381(2) . ? O00E N17 1.235(2) . ? N15 N14 1.358(2) . ? N15 C00M 1.333(2) . ? N16 N17 1.313(2) . ? N16 C00M 1.364(2) . ? N14 N13 1.293(2) . ? C00L C00N 1.486(2) . ? C00N H00C 0.9900 . ? C00N H00D 0.9900 . ?