#------------------------------------------------------------------------------ #$Date: 2021-12-07 05:38:46 +0200 (Tue, 07 Dec 2021) $ #$Revision: 271189 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/10/7061003.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_7061003 loop_ _publ_author_name 'Guo, Benyue' 'Zhang, Xiya' 'Lin, Xiangyang' 'Huang, Haifeng' 'Yang, Jun' _publ_section_title ; Combining potassium with positive oxygen-balanced polynitropyrazole: a promising way to develop green primary explosives ; _journal_issue 43 _journal_name_full 'New Journal of Chemistry' _journal_page_first 20426 _journal_page_last 20431 _journal_paper_doi 10.1039/D1NJ04452D _journal_volume 45 _journal_year 2021 _chemical_formula_moiety 'C4 K2 N8 O10' _chemical_formula_sum 'C4 K2 N8 O10' _chemical_formula_weight 398.32 _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _atom_sites_solution_primary dual _audit_creation_date 2021-04-28 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-04-30 deposited with the CCDC. 2021-10-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 10.7902(3) _cell_length_b 12.9624(4) _cell_length_c 17.9460(6) _cell_measurement_reflns_used 6978 _cell_measurement_temperature 170 _cell_measurement_theta_max 26.324 _cell_measurement_theta_min 2.269 _cell_volume 2510.05(13) _computing_cell_refinement 'SAINT V8.40A (?, 2016)' _computing_data_reduction 'SAINT V8.40A (?, 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 170.0 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Bruker D8 VENTURE' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_unetI/netI 0.0307 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 19689 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.386 _diffrn_reflns_theta_min 2.270 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.838 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6343 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1086 before and 0.0616 after correction. The Ratio of minimum to maximum transmission is 0.8510. The \l/2 correction factor is Not present.' _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 2.108 _exptl_crystal_description block _exptl_crystal_F_000 1584 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.277 _refine_diff_density_min -0.306 _refine_diff_density_rms 0.060 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 217 _refine_ls_number_reflns 2551 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.057 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0285 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+1.4495P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.0686 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2119 _reflns_number_total 2551 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL mo_2021536_0m_a.res in Pbca mo_2021536_0m.res created by SHELXL-2018/3 at 22:43:29 on 28-Apr-2021 REM Old TITL mo_2021536_0m in Pbca REM SHELXT solution in Pbca: R1 0.123, Rweak 0.003, Alpha 0.014 REM 0.474 for 351 systematic absences, Orientation as input REM Formula found by SHELXT: C14 N O7 K2 CELL 0.71073 10.7902 12.9624 17.946 90 90 90 ZERR 8 0.0003 0.0004 0.0006 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C K N O UNIT 32 16 64 80 L.S. 4 PLAN 20 SIZE 0.12 0.11 0.06 TEMP -103.15 list 4 fmap 2 acta OMIT 0 6 20 OMIT 3 2 2 REM REM REM WGHT 0.026400 1.449500 FVAR 0.39176 K1 2 0.951118 0.198009 0.852445 11.00000 0.02252 0.02400 = 0.01908 0.00153 -0.00071 0.00409 K2 2 0.459187 0.707622 0.626531 11.00000 0.01788 0.03434 = 0.02021 0.00113 -0.00033 0.00068 O2 4 0.871703 0.275716 0.720927 11.00000 0.01771 0.03177 = 0.02405 0.00644 -0.00020 0.00079 O8 4 0.744205 0.730027 0.440860 11.00000 0.02496 0.02706 = 0.02640 0.01039 0.00120 0.00288 O4 4 0.981549 0.539367 0.758768 11.00000 0.02629 0.02632 = 0.02656 -0.00190 -0.00664 -0.00336 O1 4 0.712031 0.196215 0.767383 11.00000 0.03319 0.02119 = 0.02152 0.00460 0.00487 -0.00545 O7 4 0.670484 0.705554 0.552837 11.00000 0.02458 0.03041 = 0.02866 -0.00079 0.00989 0.00604 O10 4 0.566721 0.329651 0.547561 11.00000 0.03002 0.03010 = 0.02978 0.00337 -0.00482 -0.01236 O9 4 0.617973 0.453526 0.472391 11.00000 0.03347 0.03356 = 0.02211 0.00710 -0.00845 -0.00401 O5 4 0.894485 0.447651 0.461025 11.00000 0.03462 0.01799 = 0.03369 -0.00467 0.00593 0.00313 O6 4 0.904928 0.589008 0.395595 11.00000 0.03519 0.03424 = 0.02213 0.00356 0.01064 0.00448 N1 3 0.755393 0.267135 0.727355 11.00000 0.02056 0.01950 = 0.01189 -0.00147 0.00160 -0.00162 N6 3 0.736992 0.677882 0.499464 11.00000 0.01497 0.01844 = 0.01985 0.00114 0.00099 -0.00134 O3 4 0.834271 0.447434 0.807173 11.00000 0.05171 0.05095 = 0.01547 0.00291 0.00113 -0.01972 N4 3 0.855440 0.551278 0.632352 11.00000 0.02114 0.01888 = 0.01600 -0.00296 -0.00085 -0.00008 N2 3 0.676942 0.327161 0.692569 11.00000 0.01812 0.02081 = 0.02101 0.00181 -0.00085 -0.00136 N5 3 0.783282 0.531178 0.573145 11.00000 0.02201 0.01817 = 0.01604 -0.00008 -0.00075 -0.00128 N7 3 0.870172 0.540663 0.451266 11.00000 0.02069 0.02292 = 0.02236 -0.00226 -0.00040 0.00067 N8 3 0.625973 0.407969 0.532413 11.00000 0.01956 0.02329 = 0.02325 -0.00001 -0.00170 -0.00123 N3 3 0.885174 0.489022 0.754369 11.00000 0.02669 0.01964 = 0.01983 -0.00257 -0.00158 -0.00220 C1 1 0.825768 0.481181 0.682278 11.00000 0.02070 0.01899 = 0.01319 -0.00113 0.00064 -0.00015 C3 1 0.734287 0.409764 0.657684 11.00000 0.01731 0.01991 = 0.01820 -0.00099 0.00091 0.00094 C00N 1 0.802042 0.588288 0.507829 11.00000 0.02273 0.01781 = 0.01776 0.00197 0.00262 0.00031 C2 1 0.709038 0.446799 0.587245 11.00000 0.01621 0.01711 = 0.02197 -0.00078 -0.00150 -0.00103 HKLF 4 REM mo_2021536_0m_a.res in Pbca REM wR2 = 0.0686, GooF = S = 1.057, Restrained GooF = 1.057 for all data REM R1 = 0.0285 for 2119 Fo > 4sig(Fo) and 0.0403 for all 2551 data REM 217 parameters refined using 0 restraints END WGHT 0.0288 1.2340 REM Highest difference peak 0.277, deepest hole -0.306, 1-sigma level 0.060 Q1 1 0.7931 0.4352 0.6724 11.00000 0.05 0.28 Q2 1 0.7346 0.4973 0.5838 11.00000 0.05 0.25 Q3 1 0.8363 0.7593 0.4539 11.00000 0.05 0.23 Q4 1 0.6580 0.4417 0.5634 11.00000 0.05 0.22 Q5 1 0.5169 0.8235 0.6292 11.00000 0.05 0.22 Q6 1 0.5178 0.3801 0.5694 11.00000 0.05 0.21 Q7 1 0.7864 0.5574 0.5409 11.00000 0.05 0.20 Q8 1 0.6211 0.2400 0.7663 11.00000 0.05 0.19 Q9 1 0.8998 0.1406 0.8412 11.00000 0.05 0.19 Q10 1 0.9823 0.5135 0.8024 11.00000 0.05 0.19 Q11 1 0.8535 0.4227 0.4983 11.00000 0.05 0.19 Q12 1 0.7806 0.6382 0.5068 11.00000 0.05 0.19 Q13 1 0.7506 0.4268 0.4229 11.00000 0.05 0.18 Q14 1 0.7533 0.7083 0.4691 11.00000 0.05 0.18 Q15 1 0.6880 0.4431 0.6221 11.00000 0.05 0.18 Q16 1 0.8519 0.6220 0.6468 11.00000 0.05 0.18 Q17 1 1.0295 0.5622 0.6932 11.00000 0.05 0.18 Q18 1 0.7583 0.5159 0.3838 11.00000 0.05 0.18 Q19 1 0.3975 0.6371 0.6127 11.00000 0.05 0.17 Q20 1 0.8340 0.5451 0.6056 11.00000 0.05 0.17 REM The information below was added by Olex2. REM REM R1 = 0.0285 for 2119 Fo > 4sig(Fo) and 0.0403 for all 21106 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.28, deepest hole -0.31 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0403 REM R1_gt = 0.0285 REM wR_ref = 0.0686 REM GOOF = 1.057 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 21106 REM Reflections_gt = 2119 REM Parameters = n/a REM Hole = -0.31 REM Peak = 0.28 REM Flack = n/a ; _cod_data_source_file d1nj04452d2.cif _cod_data_source_block mo_2021536_0m _cod_depositor_comments 'Adding full bibliography for 7061003--7061004.cif.' _cod_database_code 7061003 _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 0.951 _shelx_estimated_absorpt_t_min 0.906 _olex2_refinement_description ; ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, 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 K1 K 0.95112(4) 0.19801(3) 0.85244(2) 0.02186(12) Uani 1 1 d . . . . . K2 K 0.45919(4) 0.70762(3) 0.62653(2) 0.02414(12) Uani 1 1 d . . . . . O2 O 0.87170(12) 0.27572(10) 0.72093(8) 0.0245(3) Uani 1 1 d . . . . . O8 O 0.74420(12) 0.73003(10) 0.44086(8) 0.0261(3) Uani 1 1 d . . . . . O4 O 0.98155(12) 0.53937(10) 0.75877(8) 0.0264(3) Uani 1 1 d . . . . . O1 O 0.71203(13) 0.19622(10) 0.76738(8) 0.0253(3) Uani 1 1 d . . . . . O7 O 0.67048(12) 0.70555(11) 0.55284(8) 0.0279(3) Uani 1 1 d . . . . . O10 O 0.56672(13) 0.32965(11) 0.54756(8) 0.0300(3) Uani 1 1 d . . . . . O9 O 0.61797(13) 0.45353(11) 0.47239(8) 0.0297(3) Uani 1 1 d . . . . . O5 O 0.89448(13) 0.44765(10) 0.46102(8) 0.0288(3) Uani 1 1 d . . . . . O6 O 0.90493(13) 0.58901(11) 0.39559(8) 0.0305(3) Uani 1 1 d . . . . . N1 N 0.75539(14) 0.26714(12) 0.72736(9) 0.0173(3) Uani 1 1 d . . . . . N6 N 0.73699(13) 0.67788(11) 0.49946(9) 0.0178(3) Uani 1 1 d . . . . . O3 O 0.83427(16) 0.44743(13) 0.80717(8) 0.0394(4) Uani 1 1 d . . . . . N4 N 0.85544(14) 0.55128(11) 0.63235(9) 0.0187(3) Uani 1 1 d . . . . . N2 N 0.67694(14) 0.32716(12) 0.69257(9) 0.0200(4) Uani 1 1 d . . . . . N5 N 0.78328(14) 0.53118(11) 0.57315(9) 0.0187(3) Uani 1 1 d . . . . . N7 N 0.87017(15) 0.54066(12) 0.45127(9) 0.0220(4) Uani 1 1 d . . . . . N8 N 0.62597(14) 0.40797(12) 0.53241(9) 0.0220(4) Uani 1 1 d . . . . . N3 N 0.88517(15) 0.48902(12) 0.75437(9) 0.0221(4) Uani 1 1 d . . . . . C1 C 0.82577(17) 0.48118(14) 0.68228(10) 0.0176(4) Uani 1 1 d . . . . . C3 C 0.73429(16) 0.40976(14) 0.65768(11) 0.0185(4) Uani 1 1 d . . . . . C00N C 0.80204(17) 0.58829(14) 0.50783(11) 0.0194(4) Uani 1 1 d . . . . . C2 C 0.70904(17) 0.44680(13) 0.58724(11) 0.0184(4) Uani 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 K1 0.0225(2) 0.0240(2) 0.0191(3) 0.00153(17) -0.00071(16) 0.00409(16) K2 0.0179(2) 0.0343(2) 0.0202(3) 0.00113(18) -0.00033(16) 0.00068(17) O2 0.0177(7) 0.0318(8) 0.0240(8) 0.0064(6) -0.0002(6) 0.0008(6) O8 0.0250(7) 0.0271(7) 0.0264(9) 0.0104(6) 0.0012(6) 0.0029(6) O4 0.0263(7) 0.0263(7) 0.0266(9) -0.0019(6) -0.0066(6) -0.0034(6) O1 0.0332(8) 0.0212(7) 0.0215(8) 0.0046(6) 0.0049(6) -0.0054(6) O7 0.0246(7) 0.0304(7) 0.0287(9) -0.0008(6) 0.0099(6) 0.0060(6) O10 0.0300(8) 0.0301(8) 0.0298(9) 0.0034(6) -0.0048(6) -0.0124(6) O9 0.0335(8) 0.0336(8) 0.0221(9) 0.0071(7) -0.0085(6) -0.0040(6) O5 0.0346(8) 0.0180(7) 0.0337(9) -0.0047(6) 0.0059(7) 0.0031(6) O6 0.0352(8) 0.0342(8) 0.0221(9) 0.0036(7) 0.0106(6) 0.0045(7) N1 0.0206(8) 0.0195(8) 0.0119(9) -0.0015(6) 0.0016(6) -0.0016(6) N6 0.0150(7) 0.0184(7) 0.0199(9) 0.0011(7) 0.0010(6) -0.0013(6) O3 0.0517(10) 0.0509(10) 0.0155(9) 0.0029(7) 0.0011(7) -0.0197(8) N4 0.0211(8) 0.0189(8) 0.0160(9) -0.0030(7) -0.0008(6) -0.0001(6) N2 0.0181(8) 0.0208(8) 0.0210(10) 0.0018(7) -0.0009(7) -0.0014(6) N5 0.0220(8) 0.0182(7) 0.0160(9) -0.0001(7) -0.0007(6) -0.0013(6) N7 0.0207(8) 0.0229(8) 0.0224(10) -0.0023(7) -0.0004(7) 0.0007(6) N8 0.0196(8) 0.0233(8) 0.0232(10) 0.0000(7) -0.0017(7) -0.0012(7) N3 0.0267(9) 0.0196(8) 0.0198(10) -0.0026(7) -0.0016(7) -0.0022(7) C1 0.0207(9) 0.0190(9) 0.0132(11) -0.0011(8) 0.0006(7) -0.0001(7) C3 0.0173(9) 0.0199(9) 0.0182(11) -0.0010(8) 0.0009(7) 0.0009(7) C00N 0.0227(9) 0.0178(9) 0.0178(11) 0.0020(8) 0.0026(8) 0.0003(7) C2 0.0162(9) 0.0171(9) 0.0220(11) -0.0008(8) -0.0015(7) -0.0010(7) 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' K K 0.2009 0.2494 '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 _geom_angle_publ_flag K2 K1 K2 108.230(12) 8_755 3_646 ? O2 K1 K2 38.21(3) . 8_755 ? O2 K1 K2 75.41(3) . 3_646 ? O2 K1 O8 97.58(4) . 2_665 ? O2 K1 O4 75.40(4) . 3_746 ? O2 K1 O1 44.44(4) . . ? O2 K1 O10 118.55(4) . 6_657 ? O2 K1 O5 142.60(4) . 7_566 ? O2 K1 N1 22.71(4) . . ? O2 K1 N4 124.51(5) . 3_746 ? O2 K1 N2 79.54(4) . 6_657 ? O8 K1 K2 36.13(3) 2_665 3_646 ? O8 K1 K2 135.74(3) 2_665 8_755 ? O8 K1 O4 143.11(4) 2_665 3_746 ? O8 K1 O1 69.09(4) 2_665 . ? O8 K1 N1 78.93(4) 2_665 . ? O8 K1 N4 136.31(5) 2_665 3_746 ? O8 K1 N2 124.49(4) 2_665 6_657 ? O4 K1 K2 108.76(3) 3_746 3_646 ? O4 K1 K2 46.16(3) 3_746 8_755 ? O4 K1 O1 82.09(4) 3_746 . ? O4 K1 N1 83.32(4) 3_746 . ? O4 K1 N2 90.38(4) 3_746 6_657 ? O1 K1 K2 72.84(3) . 8_755 ? O1 K1 K2 35.54(3) . 3_646 ? O1 K1 N1 23.04(4) . . ? O1 K1 N2 123.66(4) . 6_657 ? O10 K1 K2 112.08(3) 6_657 3_646 ? O10 K1 K2 120.43(3) 6_657 8_755 ? O10 K1 O8 76.51(4) 6_657 2_665 ? O10 K1 O4 138.98(4) 6_657 3_746 ? O10 K1 O1 136.18(4) 6_657 . ? O10 K1 O5 93.62(4) 6_657 7_566 ? O10 K1 N1 125.23(4) 6_657 . ? O10 K1 N4 91.11(5) 6_657 3_746 ? O10 K1 N2 58.45(4) 6_657 6_657 ? O5 K1 K2 138.80(3) 7_566 8_755 ? O5 K1 K2 74.97(3) 7_566 3_646 ? O5 K1 O8 70.34(4) 7_566 2_665 ? O5 K1 O4 93.14(4) 7_566 3_746 ? O5 K1 O1 99.35(4) 7_566 . ? O5 K1 N1 122.34(4) 7_566 . ? O5 K1 N4 68.85(4) 7_566 3_746 ? O5 K1 N2 136.90(5) 7_566 6_657 ? N1 K1 K2 52.86(3) . 3_646 ? N1 K1 K2 57.62(3) . 8_755 ? N4 K1 K2 138.02(3) 3_746 3_646 ? N4 K1 K2 86.72(3) 3_746 8_755 ? N4 K1 O4 54.40(4) 3_746 3_746 ? N4 K1 O1 132.60(4) 3_746 . ? N4 K1 N1 137.60(4) 3_746 . ? N4 K1 N2 78.85(4) 3_746 6_657 ? N2 K1 K2 62.80(3) 6_657 8_755 ? N2 K1 K2 143.03(3) 6_657 3_646 ? N2 K1 N1 100.74(4) 6_657 . ? K1 K2 K1 98.499(11) 8_765 3_656 ? O2 K2 K1 39.30(3) 8_765 8_765 ? O2 K2 K1 130.01(3) 8_765 3_656 ? O2 K2 O8 140.34(5) 8_765 4_466 ? O2 K2 O4 75.41(4) 8_765 6_557 ? O2 K2 O1 92.26(4) 8_765 3_656 ? O2 K2 O10 137.99(4) 8_765 5_666 ? O2 K2 O9 147.32(4) 8_765 5_666 ? O2 K2 O6 85.34(4) 8_765 4_466 ? O2 K2 N8 152.23(4) 8_765 5_666 ? O8 K2 K1 37.06(3) 4_466 3_656 ? O8 K2 K1 129.41(3) 4_466 8_765 ? O8 K2 O4 125.74(4) 4_466 6_557 ? O8 K2 O10 62.32(4) 4_466 5_666 ? O8 K2 O9 72.26(4) 4_466 5_666 ? O8 K2 N8 61.55(4) 4_466 5_666 ? O4 K2 K1 90.09(3) 6_557 3_656 ? O4 K2 K1 45.14(3) 6_557 8_765 ? O4 K2 O10 124.76(4) 6_557 5_666 ? O4 K2 N8 106.28(4) 6_557 5_666 ? O1 K2 K1 57.53(3) 3_656 8_765 ? O1 K2 K1 40.98(3) 3_656 3_656 ? O1 K2 O8 75.16(4) 3_656 4_466 ? O1 K2 O4 61.65(4) 3_656 6_557 ? O1 K2 O10 129.47(4) 3_656 5_666 ? O1 K2 O9 101.62(4) 3_656 5_666 ? O1 K2 O6 90.51(4) 3_656 4_466 ? O1 K2 N8 113.23(4) 3_656 5_666 ? O7 K2 K1 106.66(3) . 8_765 ? O7 K2 K1 154.66(4) . 3_656 ? O7 K2 O2 74.20(4) . 8_765 ? O7 K2 O8 120.94(5) . 4_466 ? O7 K2 O4 105.46(4) . 6_557 ? O7 K2 O1 163.82(5) . 3_656 ? O7 K2 O10 65.21(4) . 5_666 ? O7 K2 O9 86.16(5) . 5_666 ? O7 K2 O6 97.03(5) . 4_466 ? O7 K2 N8 78.79(4) . 5_666 ? O10 K2 K1 166.65(3) 5_666 8_765 ? O10 K2 K1 89.52(3) 5_666 3_656 ? O10 K2 N8 21.52(4) 5_666 5_666 ? O9 K2 K1 130.40(3) 5_666 8_765 ? O9 K2 K1 75.09(3) 5_666 3_656 ? O9 K2 O4 85.34(4) 5_666 6_557 ? O9 K2 O10 41.71(4) 5_666 5_666 ? O9 K2 N8 21.05(4) 5_666 5_666 ? O6 K2 K1 102.71(3) 4_466 8_765 ? O6 K2 K1 79.97(3) 4_466 3_656 ? O6 K2 O8 57.92(4) 4_466 4_466 ? O6 K2 O4 144.77(4) 4_466 6_557 ? O6 K2 O10 89.14(4) 4_466 5_666 ? O6 K2 O9 123.48(4) 4_466 5_666 ? O6 K2 N8 104.43(4) 4_466 5_666 ? N8 K2 K1 151.40(3) 5_666 8_765 ? N8 K2 K1 77.68(3) 5_666 3_656 ? K2 O2 K1 102.49(4) 8_755 . ? N1 O2 K1 101.65(10) . . ? N1 O2 K2 135.58(11) . 8_755 ? K2 O8 K1 106.81(5) 4_566 2_664 ? N6 O8 K1 127.53(10) . 2_664 ? N6 O8 K2 125.65(10) . 4_566 ? K1 O4 K2 88.70(4) 3_756 6_657 ? N3 O4 K1 122.24(11) . 3_756 ? N3 O4 K2 111.14(11) . 6_657 ? K2 O1 K1 103.48(5) 3_646 . ? N1 O1 K1 87.99(10) . . ? N1 O1 K2 128.87(11) . 3_646 ? N6 O7 K2 152.17(12) . . ? K1 O10 K2 120.25(5) 6_557 5_666 ? N8 O10 K1 152.22(13) . 6_557 ? N8 O10 K2 87.36(11) . 5_666 ? N8 O9 K2 102.28(11) . 5_666 ? N7 O5 K1 127.20(12) . 7_565 ? N7 O6 K2 132.19(12) . 4_566 ? O2 N1 K1 55.64(9) . . ? O2 N1 N2 123.09(15) . . ? O1 N1 K1 68.97(9) . . ? O1 N1 O2 119.05(15) . . ? O1 N1 N2 117.83(15) . . ? N2 N1 K1 157.74(12) . . ? O8 N6 C00N 121.29(16) . . ? O7 N6 O8 121.63(15) . . ? O7 N6 C00N 117.08(16) . . ? N5 N4 K1 129.26(11) . 3_756 ? C1 N4 K1 125.21(12) . 3_756 ? C1 N4 N5 105.29(15) . . ? N1 N2 K1 108.38(10) . 6_557 ? N1 N2 C3 112.71(14) . . ? C3 N2 K1 131.13(12) . 6_557 ? N4 N5 C00N 118.41(15) . . ? N4 N5 C2 110.21(15) . . ? C2 N5 C00N 131.03(16) . . ? O5 N7 C00N 115.86(16) . . ? O6 N7 O5 122.65(16) . . ? O6 N7 C00N 121.48(16) . . ? O10 N8 K2 71.13(10) . 5_666 ? O10 N8 O9 123.55(16) . . ? O10 N8 C2 117.80(16) . . ? O9 N8 K2 56.67(9) . 5_666 ? O9 N8 C2 118.65(15) . . ? C2 N8 K2 156.87(12) . 5_666 ? O4 N3 C1 117.97(16) . . ? O3 N3 O4 124.38(17) . . ? O3 N3 C1 117.62(16) . . ? N4 C1 N3 116.90(16) . . ? N4 C1 C3 114.00(17) . . ? C3 C1 N3 129.05(17) . . ? N2 C3 C1 132.21(18) . . ? C2 C3 N2 126.48(17) . . ? C2 C3 C1 101.23(16) . . ? N6 C00N N5 117.85(16) . . ? N6 C00N N7 124.51(17) . . ? N7 C00N N5 116.77(16) . . ? N5 C2 N8 121.30(17) . . ? N5 C2 C3 109.23(16) . . ? C3 C2 N8 129.42(17) . . ? 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 K1 K2 4.4451(6) 3_646 ? K1 K2 4.1700(6) 8_755 ? K1 O2 2.7055(14) . ? K1 O8 2.7981(14) 2_665 ? K1 O4 2.9564(15) 3_746 ? K1 O1 2.9977(15) . ? K1 O10 2.7727(15) 6_657 ? K1 O5 2.7812(14) 7_566 ? K1 N1 3.2097(16) . ? K1 N4 2.8371(16) 3_746 ? K1 N2 3.0648(16) 6_657 ? K2 O2 2.6417(14) 8_765 ? K2 O8 2.7380(14) 4_466 ? K2 O4 3.0086(15) 6_557 ? K2 O1 2.6570(14) 3_656 ? K2 O7 2.6359(14) . ? K2 O10 3.1737(16) 5_666 ? K2 O9 2.8650(15) 5_666 ? K2 O6 2.7294(16) 4_466 ? K2 N8 3.3504(17) 5_666 ? O2 N1 1.2652(19) . ? O8 N6 1.253(2) . ? O4 N3 1.230(2) . ? O1 N1 1.257(2) . ? O7 N6 1.249(2) . ? O10 N8 1.230(2) . ? O9 N8 1.231(2) . ? O5 N7 1.246(2) . ? O6 N7 1.238(2) . ? N1 N2 1.308(2) . ? N6 C00N 1.365(2) . ? O3 N3 1.221(2) . ? N4 N5 1.343(2) . ? N4 C1 1.316(2) . ? N2 C3 1.386(2) . ? N5 C00N 1.401(2) . ? N5 C2 1.379(2) . ? N7 C00N 1.397(2) . ? N8 C2 1.423(2) . ? N3 C1 1.447(2) . ? C1 C3 1.423(3) . ? C3 C2 1.379(3) . ?