#------------------------------------------------------------------------------ #$Date: 2020-04-10 04:23:44 +0300 (Fri, 10 Apr 2020) $ #$Revision: 250578 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/77/1557769.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_1557769 loop_ _publ_author_name 'Cliffe, Matthew' 'Grey, Clare P.' 'Keyzer, Evan N.' 'Bond, Andrew David' 'Astle, Maxwell A.' _publ_section_title ; The structures of ordered defects in thiocyanate analogues of Prussian Blue  ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D0SC01246G _journal_year 2020 _chemical_formula_moiety 'C30 H74 Bi5 N33 Ni6 O16 S30' _chemical_formula_sum 'C30 H74 Bi5 N33 Ni6 O16 S30' _chemical_formula_weight 3512.13 _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 difmap _atom_sites_solution_primary dual _audit_creation_date 2019-01-09 _audit_creation_method ; Olex2 1.2 (compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-02-27 deposited with the CCDC. 2020-04-09 downloaded from the CCDC. ; _cell_angle_alpha 84.0731(7) _cell_angle_beta 76.7140(7) _cell_angle_gamma 85.1942(8) _cell_formula_units_Z 1 _cell_length_a 11.8567(2) _cell_length_b 11.8653(2) _cell_length_c 18.3824(4) _cell_measurement_reflns_used 10868 _cell_measurement_temperature 111 _cell_measurement_theta_max 27.485 _cell_measurement_theta_min 0.998 _cell_volume 2498.60(8) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_collection KappaCCD _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _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 111 _diffrn_detector 'CCD plate' _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device Area _diffrn_measurement_device_type 'Nonius Kappa' _diffrn_measurement_method \w/2\q _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_UB_11 0.05014 _diffrn_orient_matrix_UB_12 -0.02513 _diffrn_orient_matrix_UB_13 -0.06629 _diffrn_orient_matrix_UB_21 -0.06661 _diffrn_orient_matrix_UB_22 -0.04567 _diffrn_orient_matrix_UB_23 -0.02617 _diffrn_orient_matrix_UB_31 -0.02052 _diffrn_orient_matrix_UB_32 0.04912 _diffrn_orient_matrix_UB_33 -0.01774 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_unetI/netI 0.0752 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 20614 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.479 _diffrn_reflns_theta_min 2.983 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 10.562 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 2.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_description irregular _exptl_crystal_F_000 1610 _exptl_crystal_preparation 'precipitated from acidic solution' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.222 _refine_diff_density_min -1.096 _refine_diff_density_rms 0.218 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 584 _refine_ls_number_reflns 11356 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0433 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+14.5070P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.0742 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8490 _reflns_number_total 11356 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc01246g3.cif _cod_data_source_block 4_Ni6Bi5NCS30_3NH4 _cod_database_code 1557769 _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 0.620 _shelx_estimated_absorpt_t_min 0.418 _olex2_refinement_description ; 1. Restrained distances N17-H17C 0.88 with sigma of 0.02 N17-H17A 0.88 with sigma of 0.02 N17-H17B 0.88 with sigma of 0.02 N17-H17D 0.88 with sigma of 0.02 2. Others Fixed Sof: N16A(0.5) O4WA(0.5) O5WA(0.5) O4W(0.5) O5W(0.5) ; _shelx_res_file ; TITL import_2_a.res in P-1 import_2.res created by SHELXL-2018/3 at 11:59:34 on 09-Jan-2019 REM Old TITL GLOBAL OLEX2: imported from CIF REM SHELXT solution in P-1: R1 0.099, Rweak 0.008, Alpha 0.060 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: Ni6 Bi5 S30 C30 N48 CELL 0.71073 11.8567 11.8653 18.3824 84.073 76.714 85.194 ZERR 1 0.0002 0.0002 0.0004 0.001 0.001 0.001 LATT 1 SFAC C H Bi N Ni O S UNIT 30 8 5 33 6 16 30 DFIX 0.88 N17 H17c DFIX 0.88 N17 H17a DFIX 0.88 N17 H17b DFIX 0.88 N17 H17d L.S. 4 PLAN 20 SIZE 0.05 0.05 0.1 TEMP -162.15 list 4 fmap 2 acta OMIT 0 0 3 OMIT 0 2 0 OMIT -1 -1 1 OMIT -1 1 1 OMIT 1 1 2 OMIT 2 -1 1 OMIT 1 -1 2 OMIT -1 0 1 OMIT -1 0 2 OMIT 1 1 1 OMIT -1 0 2 OMIT 1 0 2 OMIT 0 1 0 OMIT 0 1 1 OMIT 1 0 1 OMIT 0 0 2 OMIT 1 -1 1 OMIT 1 0 0 OMIT 1 1 0 OMIT -1 -1 2 OMIT 0 -1 1 OMIT 0 2 1 OMIT 0 1 2 OMIT 1 2 1 OMIT 0 1 3 OMIT 2 0 0 OMIT 2 1 0 OMIT -1 1 0 REM REM REM WGHT 0.000000 14.507000 FVAR 0.16819 BI1 3 0.214981 0.989177 0.178854 11.00000 0.01699 0.01547 = 0.01660 0.00005 -0.00455 -0.00304 BI2 3 0.675658 0.488286 0.167364 11.00000 0.01891 0.01923 = 0.02033 -0.00385 -0.00635 0.00166 BI3 3 1.000000 0.500000 0.500000 10.50000 0.01795 0.01626 = 0.02343 0.00105 -0.00342 -0.00297 NI2 5 0.696170 0.980996 0.176014 11.00000 0.01441 0.01549 = 0.01669 0.00067 -0.00375 -0.00297 NI4 5 1.000000 1.000000 0.500000 10.50000 0.02581 0.01366 = 0.01317 -0.00127 -0.00272 -0.00167 NI1 5 0.178593 0.514004 0.163370 11.00000 0.01434 0.01575 = 0.01677 -0.00251 -0.00230 -0.00183 NI3 5 0.500000 0.500000 0.500000 10.50000 0.01750 0.02533 = 0.01594 -0.00138 -0.00279 -0.00648 S9 7 1.037228 0.835642 0.269345 11.00000 0.01990 0.01950 = 0.02380 0.00269 -0.00847 -0.00222 S11 7 0.928521 0.960570 -0.074590 11.00000 0.01800 0.03421 = 0.01588 -0.00059 -0.00290 -0.00004 S3 7 0.055200 0.138177 0.261975 11.00000 0.03249 0.01757 = 0.02391 0.00119 0.00308 -0.00432 S5 7 0.580727 0.393660 0.066043 11.00000 0.01711 0.02950 = 0.02289 -0.00813 -0.00226 -0.00018 S7 7 0.346079 1.161919 0.109465 11.00000 0.01828 0.01937 = 0.04330 0.00865 -0.01038 -0.00163 S8 7 0.487832 0.634757 0.219186 11.00000 0.01622 0.01738 = 0.03571 -0.00373 -0.00436 -0.00452 S1 7 0.235286 0.334282 -0.058012 11.00000 0.02890 0.02758 = 0.03174 -0.01295 -0.00207 -0.00377 S2 7 -0.224462 0.571360 0.278630 11.00000 0.01698 0.03323 = 0.02077 -0.00313 -0.00163 -0.00258 S6 7 0.375289 0.857390 0.076500 11.00000 0.02312 0.01909 = 0.03191 -0.00201 -0.00013 -0.00515 S10 7 0.881631 1.337675 0.117798 11.00000 0.02074 0.01648 = 0.04175 0.00020 -0.00303 -0.00490 S4 7 0.181700 0.625869 0.408858 11.00000 0.02247 0.03828 = 0.01824 -0.00572 -0.00515 -0.00959 S15 7 1.333876 0.923748 0.296558 11.00000 0.02114 0.04616 = 0.01894 -0.00221 -0.00368 0.00480 S12 7 0.560684 0.320036 0.267914 11.00000 0.05715 0.02586 = 0.02650 -0.01052 -0.00995 0.00413 S13 7 0.863543 0.677287 0.446741 11.00000 0.02822 0.02427 = 0.07658 0.01867 -0.02658 -0.01203 S14 7 1.056289 0.619988 0.609567 11.00000 0.09616 0.02365 = 0.02156 0.00195 -0.01328 0.01398 O1 6 0.619617 1.008296 0.290484 11.00000 0.02188 0.02821 = 0.01510 -0.00598 0.00123 -0.00511 O2 6 0.557745 0.345000 0.555471 11.00000 0.02445 0.02525 = 0.02756 0.00067 -0.01071 -0.00438 O1W 6 0.625306 0.799417 0.371889 11.00000 0.03929 0.02541 = 0.02312 0.00182 -0.00654 -0.00250 N3 4 0.131004 0.354107 0.203091 11.00000 0.02231 0.01700 = 0.02567 -0.00151 -0.00365 -0.00394 O3 6 1.100523 1.037950 0.575279 11.00000 0.03070 0.02187 = 0.01874 -0.00156 -0.00792 -0.00587 N11 4 0.772801 0.958387 0.066153 11.00000 0.02420 0.02050 = 0.02559 -0.00574 -0.01036 -0.00376 N6 4 0.231848 0.674229 0.119206 11.00000 0.02464 0.02288 = 0.02381 -0.00363 -0.00795 -0.00035 N10 4 0.770394 1.132799 0.163837 11.00000 0.02101 0.01817 = 0.02583 -0.00133 -0.00357 -0.00393 N8 4 0.615587 0.830543 0.193264 11.00000 0.01512 0.02122 = 0.01830 -0.00021 -0.00412 -0.00218 N4 4 0.194450 0.548370 0.266543 11.00000 0.01654 0.02296 = 0.02700 0.00135 -0.00121 -0.00756 N1 4 0.158169 0.478956 0.058044 11.00000 0.02580 0.02779 = 0.01954 -0.00205 -0.00942 -0.01044 N2 4 0.005552 0.573450 0.191331 11.00000 0.02341 0.02379 = 0.02305 -0.00719 -0.00827 0.00245 N7 4 0.550406 1.061577 0.148950 11.00000 0.01215 0.02840 = 0.02245 0.00705 -0.00523 -0.00480 N17 4 0.024183 0.751719 0.058451 11.00000 0.03485 0.02868 = 0.03582 0.01198 -0.01837 -0.00588 N9 4 0.838624 0.904297 0.211838 11.00000 0.01788 0.02338 = 0.02242 0.00128 -0.00810 -0.00561 N13 4 0.657436 0.562244 0.479425 11.00000 0.02331 0.02963 = 0.02374 -0.00260 -0.00451 -0.00982 N5 4 0.348474 0.455598 0.133687 11.00000 0.01656 0.02053 = 0.02047 -0.00324 -0.00582 -0.00504 N14 4 1.014498 0.836106 0.538800 11.00000 0.03393 0.01870 = 0.02032 -0.00624 -0.00986 -0.00184 O2W 6 0.772669 0.126255 0.348863 11.00000 0.04258 0.03922 = 0.04644 -0.00609 -0.02397 -0.00121 N12 4 0.538211 0.427294 0.400517 11.00000 0.02238 0.03561 = 0.02864 -0.00718 -0.00665 0.00161 N15 4 1.149135 0.972262 0.418032 11.00000 0.02502 0.02462 = 0.01781 -0.00080 -0.00554 -0.00412 C1 1 0.188284 0.421391 0.009789 11.00000 0.01981 0.02491 = 0.01763 -0.00228 -0.00912 -0.00709 C4 1 0.187955 0.579394 0.325647 11.00000 0.01240 0.02092 = 0.02472 0.00718 -0.00532 -0.00620 C3 1 0.101528 0.265257 0.225184 11.00000 0.01624 0.02544 = 0.00862 -0.00311 -0.00277 0.00573 C8 1 0.564056 0.750615 0.203340 11.00000 0.01820 0.02497 = 0.01621 -0.00011 -0.00524 -0.00419 C11 1 0.832879 0.961096 0.007590 11.00000 0.01989 0.01537 = 0.02273 -0.00130 -0.00349 -0.00320 C6 1 0.292525 0.747695 0.101737 11.00000 0.01756 0.01689 = 0.01444 -0.00507 -0.00438 0.00230 C14 1 1.031850 0.746448 0.567858 11.00000 0.03018 0.02104 = 0.01652 -0.00682 -0.00378 -0.00155 O3W 6 0.597552 0.150933 0.475061 11.00000 0.05174 0.08155 = 0.09281 -0.05534 -0.00557 0.00077 C10 1 0.815105 1.217330 0.145269 11.00000 0.01823 0.02457 = 0.01353 -0.00470 -0.00688 0.00842 C12 1 0.549110 0.384471 0.345839 11.00000 0.02510 0.02654 = 0.02634 -0.00476 -0.00763 0.00452 C9 1 0.920236 0.877467 0.235212 11.00000 0.02409 0.00817 = 0.01408 -0.00234 0.00018 -0.01011 C2 1 -0.089306 0.573270 0.226635 11.00000 0.03335 0.01075 = 0.01677 0.00001 -0.00692 -0.00198 C5 1 0.443191 0.430706 0.105723 11.00000 0.02629 0.01226 = 0.01872 -0.00245 -0.01077 -0.01062 C7 1 0.467455 1.102707 0.133263 11.00000 0.03020 0.01529 = 0.01836 0.00310 -0.00063 -0.00918 C15 1 1.223585 0.953593 0.367643 11.00000 0.02580 0.02195 = 0.01773 0.00073 -0.00527 -0.00479 C13 1 0.741508 0.607999 0.467260 11.00000 0.02995 0.02031 = 0.03019 0.00180 -0.01731 0.00218 PART 1 N16A 4 1.430411 1.140290 0.381721 10.50000 0.07802 0.04753 = 0.05850 0.01038 -0.01380 -0.02423 PART 0 PART 2 O4WA 6 1.354155 1.110263 0.477407 10.50000 0.11472 0.05301 = 0.04244 0.00584 -0.00895 -0.03405 O5WA 6 1.285656 1.220933 0.359435 10.50000 0.07438 0.06327 = 0.06228 0.03339 -0.01666 -0.04125 PART 0 PART 1 O4W 6 1.327986 1.068297 0.515064 10.50000 0.04502 0.06359 = 0.09145 -0.03182 -0.02483 -0.00388 O5W 6 1.277617 1.287356 0.336025 10.50000 0.10266 0.09739 = 0.14404 -0.03169 -0.07121 0.00188 PART 0 H17A 2 0.049000 0.708587 0.094272 11.00000 0.01576 H17B 2 0.057960 0.735765 0.012384 11.00000 0.10247 H17C 2 0.028034 0.824640 0.061124 11.00000 0.02190 H17D 2 -0.051159 0.744613 0.076899 11.00000 0.06338 HKLF 4 REM import_2_a.res in P-1 REM wR2 = 0.0742, GooF = S = 1.036, Restrained GooF = 1.036 for all data REM R1 = 0.0433 for 8490 Fo > 4sig(Fo) and 0.0737 for all 11356 data REM 584 parameters refined using 4 restraints END WGHT 0.0000 14.5067 REM Highest difference peak 1.222, deepest hole -1.096, 1-sigma level 0.218 Q1 1 1.4550 1.0127 0.4898 11.00000 0.05 1.22 Q2 1 0.5742 0.5598 0.2020 11.00000 0.05 1.19 Q3 1 0.1193 1.0316 0.1525 11.00000 0.05 1.16 Q4 1 0.5698 0.5262 0.1392 11.00000 0.05 1.09 Q5 1 0.5378 1.0862 0.2640 11.00000 0.05 1.06 Q6 1 0.6798 0.7759 0.3423 11.00000 0.05 0.92 Q7 1 0.8985 0.5374 0.4759 11.00000 0.05 0.90 Q8 1 0.7552 0.4934 0.1906 11.00000 0.05 0.90 Q9 1 1.1385 0.9744 0.5950 11.00000 0.05 0.89 Q10 1 0.7927 0.1785 0.3232 11.00000 0.05 0.88 Q11 1 1.3952 1.1769 0.5126 11.00000 0.05 0.87 Q12 1 -0.0601 0.8258 0.0756 11.00000 0.05 0.84 Q13 1 1.1218 0.6057 0.5243 11.00000 0.05 0.83 Q14 1 -0.1348 0.6751 0.2972 11.00000 0.05 0.82 Q15 1 0.2592 0.3789 0.1141 11.00000 0.05 0.81 Q16 1 0.6539 0.3645 0.5638 11.00000 0.05 0.81 Q17 1 0.6976 0.8015 0.1992 11.00000 0.05 0.80 Q18 1 0.8394 1.4463 0.1493 11.00000 0.05 0.80 Q19 1 1.0505 1.0819 0.5967 11.00000 0.05 0.80 Q20 1 0.8003 1.1754 0.1233 11.00000 0.05 0.80 ; _shelx_res_checksum 4187 _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 Bi1 Bi 0.21498(2) 0.98918(2) 0.17885(2) 0.01621(7) Uani 1 1 d . . . . . Bi2 Bi 0.67566(2) 0.48829(2) 0.16736(2) 0.01918(7) Uani 1 1 d . . . . . Bi3 Bi 1.000000 0.500000 0.500000 0.01950(9) Uani 1 2 d S T P . . Ni2 Ni 0.69617(7) 0.98100(7) 0.17601(5) 0.01552(19) Uani 1 1 d . . . . . Ni4 Ni 1.000000 1.000000 0.500000 0.0178(3) Uani 1 2 d S T P . . Ni1 Ni 0.17859(7) 0.51400(7) 0.16337(5) 0.01568(19) Uani 1 1 d . . . . . Ni3 Ni 0.500000 0.500000 0.500000 0.0195(3) Uani 1 2 d S T P . . S9 S 1.03723(15) 0.83564(14) 0.26935(10) 0.0208(4) Uani 1 1 d . . . . . S11 S 0.92852(15) 0.96057(16) -0.07459(10) 0.0230(4) Uani 1 1 d . . . . . S3 S 0.05520(17) 0.13818(15) 0.26197(10) 0.0262(4) Uani 1 1 d . . . . . S5 S 0.58073(15) 0.39366(15) 0.06604(10) 0.0232(4) Uani 1 1 d . . . . . S7 S 0.34608(16) 1.16192(15) 0.10947(12) 0.0272(4) Uani 1 1 d . . . . . S8 S 0.48783(15) 0.63476(14) 0.21919(11) 0.0230(4) Uani 1 1 d . . . . . S1 S 0.23529(17) 0.33428(16) -0.05801(11) 0.0293(4) Uani 1 1 d . . . . . S2 S -0.22446(15) 0.57136(16) 0.27863(10) 0.0240(4) Uani 1 1 d . . . . . S6 S 0.37529(16) 0.85739(15) 0.07650(11) 0.0255(4) Uani 1 1 d . . . . . S10 S 0.88163(16) 1.33767(15) 0.11780(12) 0.0269(4) Uani 1 1 d . . . . . S4 S 0.18170(16) 0.62587(17) 0.40886(10) 0.0256(4) Uani 1 1 d . . . . . S15 S 1.33388(16) 0.92375(18) 0.29656(10) 0.0293(4) Uani 1 1 d . . . . . S12 S 0.5607(2) 0.32004(17) 0.26791(11) 0.0362(5) Uani 1 1 d . . . . . S13 S 0.86354(18) 0.67729(17) 0.44674(15) 0.0416(6) Uani 1 1 d . . . . . S14 S 1.0563(2) 0.61999(17) 0.60957(12) 0.0484(7) Uani 1 1 d . . . . . O1 O 0.6196(4) 1.0083(4) 0.2905(3) 0.0221(11) Uani 1 1 d . . . . . O2 O 0.5577(4) 0.3450(4) 0.5555(3) 0.0250(11) Uani 1 1 d . . . . . O1W O 0.6253(4) 0.7994(4) 0.3719(3) 0.0296(12) Uani 1 1 d . . . . . N3 N 0.1310(5) 0.3541(5) 0.2031(3) 0.0218(13) Uani 1 1 d . . . . . O3 O 1.1005(4) 1.0379(4) 0.5753(3) 0.0231(11) Uani 1 1 d . . . . . N11 N 0.7728(5) 0.9584(5) 0.0662(3) 0.0222(13) Uani 1 1 d . . . . . N6 N 0.2318(5) 0.6742(5) 0.1192(3) 0.0233(14) Uani 1 1 d . . . . . N10 N 0.7704(5) 1.1328(5) 0.1638(3) 0.0218(13) Uani 1 1 d . . . . . N8 N 0.6156(5) 0.8305(5) 0.1933(3) 0.0182(12) Uani 1 1 d . . . . . N4 N 0.1945(5) 0.5484(5) 0.2665(3) 0.0226(13) Uani 1 1 d . . . . . N1 N 0.1582(5) 0.4790(5) 0.0580(3) 0.0232(14) Uani 1 1 d . . . . . N2 N 0.0056(5) 0.5735(5) 0.1913(3) 0.0228(13) Uani 1 1 d . . . . . N7 N 0.5504(5) 1.0616(5) 0.1490(3) 0.0212(13) Uani 1 1 d . . . . . N17 N 0.0242(7) 0.7517(6) 0.0585(5) 0.0322(16) Uani 1 1 d D . . . . N9 N 0.8386(5) 0.9043(5) 0.2118(3) 0.0206(13) Uani 1 1 d . . . . . N13 N 0.6574(5) 0.5622(5) 0.4794(3) 0.0252(14) Uani 1 1 d . . . . . N5 N 0.3485(5) 0.4556(5) 0.1337(3) 0.0186(12) Uani 1 1 d . . . . . N14 N 1.0145(5) 0.8361(5) 0.5388(3) 0.0234(14) Uani 1 1 d . . . . . O2W O 0.7727(5) 0.1263(5) 0.3489(3) 0.0404(14) Uani 1 1 d . . . . . N12 N 0.5382(5) 0.4273(5) 0.4005(4) 0.0286(15) Uani 1 1 d . . . . . N15 N 1.1491(5) 0.9723(5) 0.4180(3) 0.0223(13) Uani 1 1 d . . . . . C1 C 0.1883(6) 0.4214(6) 0.0098(4) 0.0196(15) Uani 1 1 d . . . . . C4 C 0.1880(6) 0.5794(6) 0.3256(4) 0.0195(15) Uani 1 1 d . . . . . C3 C 0.1015(6) 0.2653(6) 0.2252(4) 0.0171(15) Uani 1 1 d . . . . . C8 C 0.5641(6) 0.7506(6) 0.2033(4) 0.0195(15) Uani 1 1 d . . . . . C11 C 0.8329(6) 0.9611(5) 0.0076(4) 0.0194(15) Uani 1 1 d . . . . . C6 C 0.2925(6) 0.7477(6) 0.1017(4) 0.0161(14) Uani 1 1 d . . . . . C14 C 1.0318(6) 0.7464(6) 0.5679(4) 0.0224(16) Uani 1 1 d . . . . . O3W O 0.5976(6) 0.1509(6) 0.4751(4) 0.074(2) Uani 1 1 d . . . . . C10 C 0.8151(6) 1.2173(6) 0.1453(4) 0.0186(15) Uani 1 1 d . . . . . C12 C 0.5491(6) 0.3845(6) 0.3458(4) 0.0259(17) Uani 1 1 d . . . . . C9 C 0.9202(6) 0.8775(5) 0.2352(4) 0.0155(14) Uani 1 1 d . . . . . C2 C -0.0893(7) 0.5733(5) 0.2266(4) 0.0201(15) Uani 1 1 d . . . . . C5 C 0.4432(6) 0.4307(5) 0.1057(4) 0.0175(15) Uani 1 1 d . . . . . C7 C 0.4675(6) 1.1027(6) 0.1333(4) 0.0219(16) Uani 1 1 d . . . . . C15 C 1.2236(6) 0.9536(6) 0.3676(4) 0.0217(16) Uani 1 1 d . . . . . C13 C 0.7415(7) 0.6080(6) 0.4673(4) 0.0256(17) Uani 1 1 d . . . . . N16A N 1.4304(15) 1.1403(13) 0.3817(10) 0.061(5) Uani 0.5 1 d . . . A 1 O4WA O 1.354(2) 1.1103(16) 0.4774(10) 0.070(6) Uani 0.5 1 d . . . B 2 O5WA O 1.2857(17) 1.2209(15) 0.3594(10) 0.067(5) Uani 0.5 1 d . . . C 2 O4W O 1.3280(14) 1.0683(15) 0.5151(11) 0.063(5) Uani 0.5 1 d . . . D 1 O5W O 1.278(2) 1.2874(19) 0.3360(15) 0.107(8) Uani 0.5 1 d . . . E 1 H17A H 0.049(5) 0.709(5) 0.094(3) 0.016(18) Uiso 1 1 d D . . . . H17B H 0.058(9) 0.736(10) 0.012(3) 0.10(5) Uiso 1 1 d D . . . . H17C H 0.028(6) 0.825(2) 0.061(4) 0.02(2) Uiso 1 1 d D . . . . H17D H -0.051(3) 0.745(8) 0.077(5) 0.06(3) Uiso 1 1 d 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 Bi1 0.01699(14) 0.01547(13) 0.01660(14) 0.00005(10) -0.00455(11) -0.00304(10) Bi2 0.01891(14) 0.01923(14) 0.02033(15) -0.00385(11) -0.00635(11) 0.00166(11) Bi3 0.0179(2) 0.01626(19) 0.0234(2) 0.00105(15) -0.00342(16) -0.00297(15) Ni2 0.0144(4) 0.0155(4) 0.0167(5) 0.0007(4) -0.0038(4) -0.0030(4) Ni4 0.0258(7) 0.0137(6) 0.0132(6) -0.0013(5) -0.0027(5) -0.0017(5) Ni1 0.0143(4) 0.0158(4) 0.0168(5) -0.0025(4) -0.0023(4) -0.0018(4) Ni3 0.0175(7) 0.0253(7) 0.0159(7) -0.0014(5) -0.0028(5) -0.0065(5) S9 0.0199(9) 0.0195(9) 0.0238(10) 0.0027(7) -0.0085(8) -0.0022(7) S11 0.0180(9) 0.0342(10) 0.0159(9) -0.0006(8) -0.0029(7) 0.0000(8) S3 0.0325(11) 0.0176(9) 0.0239(10) 0.0012(8) 0.0031(8) -0.0043(8) S5 0.0171(9) 0.0295(10) 0.0229(10) -0.0081(8) -0.0023(8) -0.0002(8) S7 0.0183(9) 0.0194(9) 0.0433(12) 0.0086(8) -0.0104(9) -0.0016(8) S8 0.0162(9) 0.0174(9) 0.0357(11) -0.0037(8) -0.0044(8) -0.0045(7) S1 0.0289(11) 0.0276(10) 0.0317(11) -0.0130(9) -0.0021(9) -0.0038(8) S2 0.0170(9) 0.0332(10) 0.0208(10) -0.0031(8) -0.0016(8) -0.0026(8) S6 0.0231(10) 0.0191(9) 0.0319(11) -0.0020(8) -0.0001(8) -0.0052(8) S10 0.0207(10) 0.0165(9) 0.0418(12) 0.0002(8) -0.0030(9) -0.0049(7) S4 0.0225(10) 0.0383(11) 0.0182(10) -0.0057(8) -0.0051(8) -0.0096(8) S15 0.0211(10) 0.0462(12) 0.0189(10) -0.0022(9) -0.0037(8) 0.0048(9) S12 0.0571(14) 0.0259(10) 0.0265(11) -0.0105(9) -0.0100(10) 0.0041(10) S13 0.0282(11) 0.0243(10) 0.0766(17) 0.0187(11) -0.0266(11) -0.0120(9) S14 0.096(2) 0.0237(11) 0.0216(11) 0.0020(9) -0.0133(12) 0.0140(12) O1 0.022(3) 0.028(3) 0.015(3) -0.006(2) 0.001(2) -0.005(2) O2 0.024(3) 0.025(3) 0.028(3) 0.001(2) -0.011(2) -0.004(2) O1W 0.039(3) 0.025(3) 0.023(3) 0.002(2) -0.007(2) -0.002(2) N3 0.022(3) 0.017(3) 0.026(3) -0.002(3) -0.004(3) -0.004(3) O3 0.031(3) 0.022(3) 0.019(3) -0.002(2) -0.008(2) -0.006(2) N11 0.024(3) 0.021(3) 0.026(4) -0.006(3) -0.010(3) -0.004(3) N6 0.025(3) 0.023(3) 0.024(3) -0.004(3) -0.008(3) 0.000(3) N10 0.021(3) 0.018(3) 0.026(3) -0.001(3) -0.004(3) -0.004(3) N8 0.015(3) 0.021(3) 0.018(3) 0.000(2) -0.004(2) -0.002(3) N4 0.017(3) 0.023(3) 0.027(4) 0.001(3) -0.001(3) -0.008(3) N1 0.026(3) 0.028(3) 0.020(3) -0.002(3) -0.009(3) -0.010(3) N2 0.023(3) 0.024(3) 0.023(3) -0.007(3) -0.008(3) 0.002(3) N7 0.012(3) 0.028(3) 0.022(3) 0.007(3) -0.005(3) -0.005(3) N17 0.035(4) 0.029(4) 0.036(5) 0.012(4) -0.018(4) -0.006(3) N9 0.018(3) 0.023(3) 0.022(3) 0.001(3) -0.008(3) -0.006(3) N13 0.023(3) 0.030(3) 0.024(4) -0.003(3) -0.005(3) -0.010(3) N5 0.017(3) 0.021(3) 0.020(3) -0.003(2) -0.006(3) -0.005(3) N14 0.034(4) 0.019(3) 0.020(3) -0.006(3) -0.010(3) -0.002(3) O2W 0.043(3) 0.039(3) 0.046(4) -0.006(3) -0.024(3) -0.001(3) N12 0.022(3) 0.036(4) 0.029(4) -0.007(3) -0.007(3) 0.002(3) N15 0.025(3) 0.025(3) 0.018(3) -0.001(3) -0.006(3) -0.004(3) C1 0.020(4) 0.025(4) 0.018(4) -0.002(3) -0.009(3) -0.007(3) C4 0.012(3) 0.021(4) 0.025(4) 0.007(3) -0.005(3) -0.006(3) C3 0.016(4) 0.025(4) 0.009(3) -0.003(3) -0.003(3) 0.006(3) C8 0.018(4) 0.025(4) 0.016(4) 0.000(3) -0.005(3) -0.004(3) C11 0.020(4) 0.015(3) 0.023(4) -0.001(3) -0.003(3) -0.003(3) C6 0.018(4) 0.017(3) 0.014(4) -0.005(3) -0.004(3) 0.002(3) C14 0.030(4) 0.021(4) 0.017(4) -0.007(3) -0.004(3) -0.002(3) O3W 0.052(4) 0.082(5) 0.093(6) -0.055(5) -0.006(4) 0.001(4) C10 0.018(4) 0.025(4) 0.014(4) -0.005(3) -0.007(3) 0.008(3) C12 0.025(4) 0.027(4) 0.026(4) -0.005(3) -0.008(3) 0.005(3) C9 0.024(4) 0.008(3) 0.014(4) -0.002(3) 0.000(3) -0.010(3) C2 0.033(4) 0.011(3) 0.017(4) 0.000(3) -0.007(3) -0.002(3) C5 0.026(4) 0.012(3) 0.019(4) -0.002(3) -0.011(3) -0.011(3) C7 0.030(4) 0.015(4) 0.018(4) 0.003(3) -0.001(3) -0.009(3) C15 0.026(4) 0.022(4) 0.018(4) 0.001(3) -0.005(3) -0.005(3) C13 0.030(4) 0.020(4) 0.030(4) 0.002(3) -0.017(4) 0.002(3) N16A 0.078(13) 0.048(10) 0.058(11) 0.010(8) -0.014(10) -0.024(9) O4WA 0.115(16) 0.053(11) 0.042(11) 0.006(8) -0.009(10) -0.034(10) O5WA 0.074(12) 0.063(12) 0.062(11) 0.033(9) -0.017(9) -0.041(10) O4W 0.045(10) 0.064(13) 0.091(16) -0.032(10) -0.025(10) -0.004(9) O5W 0.103(16) 0.097(17) 0.14(2) -0.032(15) -0.071(16) 0.002(15) 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' Bi Bi -4.1077 10.2566 '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' Ni Ni 0.3393 1.1124 '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' S S 0.1246 0.1234 '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 S11 Bi1 S9 88.60(5) 2_675 1_455 ? S11 Bi1 S6 91.07(5) 2_675 . ? S11 Bi1 S15 172.33(6) 2_675 1_455 ? S3 Bi1 S9 77.18(5) 1_565 1_455 ? S3 Bi1 S11 82.81(5) 1_565 2_675 ? S3 Bi1 S6 172.17(5) 1_565 . ? S3 Bi1 S15 94.19(6) 1_565 1_455 ? S7 Bi1 S9 168.46(5) . 1_455 ? S7 Bi1 S11 88.97(6) . 2_675 ? S7 Bi1 S3 91.32(6) . 1_565 ? S7 Bi1 S6 83.65(6) . . ? S7 Bi1 S15 98.18(6) . 1_455 ? S6 Bi1 S9 107.68(5) . 1_455 ? S6 Bi1 S15 92.47(5) . 1_455 ? S15 Bi1 S9 83.84(5) 1_455 1_455 ? S5 Bi2 S8 96.88(5) . . ? S5 Bi2 S1 91.53(6) . 2_665 ? S5 Bi2 S2 175.95(5) . 1_655 ? S5 Bi2 S10 86.21(5) . 1_545 ? S5 Bi2 S12 83.10(6) . . ? S8 Bi2 S1 88.11(5) . 2_665 ? S8 Bi2 S2 85.02(5) . 1_655 ? S8 Bi2 S10 176.90(5) . 1_545 ? S8 Bi2 S12 87.08(6) . . ? S1 Bi2 S2 92.10(5) 2_665 1_655 ? S1 Bi2 S10 91.76(5) 2_665 1_545 ? S2 Bi2 S10 91.90(5) 1_655 1_545 ? S12 Bi2 S1 172.31(6) . 2_665 ? S12 Bi2 S2 93.45(6) . 1_655 ? S12 Bi2 S10 93.37(6) . 1_545 ? S4 Bi3 S4 180.00(7) 2_666 1_655 ? S13 Bi3 S4 82.00(6) 2_766 2_666 ? S13 Bi3 S4 82.01(6) . 1_655 ? S13 Bi3 S4 97.99(6) 2_766 1_655 ? S13 Bi3 S4 97.99(6) . 2_666 ? S13 Bi3 S13 180.00(9) . 2_766 ? S13 Bi3 S14 95.42(7) . . ? S13 Bi3 S14 95.42(7) 2_766 2_766 ? S13 Bi3 S14 84.58(7) 2_766 . ? S13 Bi3 S14 84.58(7) . 2_766 ? S14 Bi3 S4 80.36(6) . 1_655 ? S14 Bi3 S4 80.36(6) 2_766 2_666 ? S14 Bi3 S4 99.64(6) . 2_666 ? S14 Bi3 S4 99.64(6) 2_766 1_655 ? S14 Bi3 S14 180.0 . 2_766 ? N11 Ni2 O1 178.4(2) . . ? N11 Ni2 N8 93.7(2) . . ? N11 Ni2 N9 91.8(2) . . ? N10 Ni2 O1 89.3(2) . . ? N10 Ni2 N11 89.2(2) . . ? N10 Ni2 N8 177.0(2) . . ? N10 Ni2 N7 90.1(2) . . ? N10 Ni2 N9 88.9(2) . . ? N8 Ni2 O1 87.9(2) . . ? N8 Ni2 N9 91.8(2) . . ? N7 Ni2 O1 87.8(2) . . ? N7 Ni2 N11 92.7(2) . . ? N7 Ni2 N8 89.0(2) . . ? N7 Ni2 N9 175.4(2) . . ? N9 Ni2 O1 87.7(2) . . ? O3 Ni4 O3 180.0 2_776 . ? N14 Ni4 O3 88.2(2) 2_776 2_776 ? N14 Ni4 O3 91.8(2) . 2_776 ? N14 Ni4 O3 88.2(2) . . ? N14 Ni4 O3 91.8(2) 2_776 . ? N14 Ni4 N14 180.0 2_776 . ? N14 Ni4 N15 91.2(2) 2_776 . ? N14 Ni4 N15 88.8(2) 2_776 2_776 ? N14 Ni4 N15 91.2(2) . 2_776 ? N14 Ni4 N15 88.8(2) . . ? N15 Ni4 O3 89.2(2) 2_776 . ? N15 Ni4 O3 90.8(2) . . ? N15 Ni4 O3 90.8(2) 2_776 2_776 ? N15 Ni4 O3 89.2(2) . 2_776 ? N15 Ni4 N15 180.0 2_776 . ? N3 Ni1 N6 177.7(2) . . ? N3 Ni1 N1 88.3(2) . . ? N3 Ni1 N2 89.6(2) . . ? N3 Ni1 N5 90.6(2) . . ? N6 Ni1 N1 90.2(2) . . ? N4 Ni1 N3 91.4(2) . . ? N4 Ni1 N6 90.2(2) . . ? N4 Ni1 N1 178.7(2) . . ? N4 Ni1 N2 88.6(2) . . ? N4 Ni1 N5 92.6(2) . . ? N2 Ni1 N6 92.2(2) . . ? N2 Ni1 N1 90.2(2) . . ? N5 Ni1 N6 87.6(2) . . ? N5 Ni1 N1 88.7(2) . . ? N5 Ni1 N2 178.8(2) . . ? O2 Ni3 O2 180.0 . 2_666 ? N13 Ni3 O2 87.6(2) 2_666 . ? N13 Ni3 O2 87.6(2) . 2_666 ? N13 Ni3 O2 92.4(2) . . ? N13 Ni3 O2 92.4(2) 2_666 2_666 ? N13 Ni3 N13 180.0 . 2_666 ? N13 Ni3 N12 91.9(2) 2_666 2_666 ? N13 Ni3 N12 88.1(2) . 2_666 ? N13 Ni3 N12 88.1(2) 2_666 . ? N13 Ni3 N12 91.9(2) . . ? N12 Ni3 O2 89.8(2) 2_666 . ? N12 Ni3 O2 90.2(2) . . ? N12 Ni3 O2 90.2(2) 2_666 2_666 ? N12 Ni3 O2 89.8(2) . 2_666 ? N12 Ni3 N12 180.0 2_666 . ? C9 S9 Bi1 102.5(2) . 1_655 ? C11 S11 Bi1 102.5(2) . 2_675 ? C3 S3 Bi1 102.9(2) . 1_545 ? C5 S5 Bi2 95.4(2) . . ? C7 S7 Bi1 94.0(2) . . ? C8 S8 Bi2 95.0(2) . . ? C1 S1 Bi2 93.7(3) . 2_665 ? C2 S2 Bi2 96.0(2) . 1_455 ? C6 S6 Bi1 90.3(2) . . ? C10 S10 Bi2 95.7(2) . 1_565 ? C4 S4 Bi3 100.8(2) . 1_455 ? C15 S15 Bi1 97.0(2) . 1_655 ? C12 S12 Bi2 97.3(3) . . ? C13 S13 Bi3 95.5(2) . . ? C14 S14 Bi3 94.9(3) . . ? C3 N3 Ni1 178.3(6) . . ? C11 N11 Ni2 164.9(6) . . ? C6 N6 Ni1 158.1(5) . . ? C10 N10 Ni2 169.5(6) . . ? C8 N8 Ni2 175.7(5) . . ? C4 N4 Ni1 169.2(5) . . ? C1 N1 Ni1 145.5(6) . . ? C2 N2 Ni1 154.6(6) . . ? C7 N7 Ni2 177.3(6) . . ? C9 N9 Ni2 169.5(5) . . ? C13 N13 Ni3 173.2(6) . . ? C5 N5 Ni1 169.0(6) . . ? C14 N14 Ni4 170.3(6) . . ? C12 N12 Ni3 173.7(6) . . ? C15 N15 Ni4 172.1(6) . . ? N1 C1 S1 177.5(7) . . ? N4 C4 S4 178.4(7) . . ? N3 C3 S3 176.9(6) . . ? N8 C8 S8 179.2(7) . . ? N11 C11 S11 175.6(7) . . ? N6 C6 S6 177.6(6) . . ? N14 C14 S14 179.6(6) . . ? N10 C10 S10 179.0(7) . . ? N12 C12 S12 178.0(8) . . ? N9 C9 S9 178.7(6) . . ? N2 C2 S2 178.9(7) . . ? N5 C5 S5 179.3(7) . . ? N7 C7 S7 179.3(7) . . ? N15 C15 S15 178.0(7) . . ? N13 C13 S13 178.0(7) . . ? 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 Bi1 S9 2.9889(18) 1_455 ? Bi1 S11 2.8314(17) 2_675 ? Bi1 S3 2.7777(18) 1_565 ? Bi1 S7 2.7068(19) . ? Bi1 S6 2.8397(18) . ? Bi1 S15 2.8536(19) 1_455 ? Bi2 S5 2.7575(18) . ? Bi2 S8 2.7578(17) . ? Bi2 S1 2.848(2) 2_665 ? Bi2 S2 2.8780(18) 1_655 ? Bi2 S10 2.9275(18) 1_545 ? Bi2 S12 2.792(2) . ? Bi3 S4 2.8359(19) 1_655 ? Bi3 S4 2.8359(19) 2_666 ? Bi3 S13 2.7809(19) . ? Bi3 S13 2.7810(19) 2_766 ? Bi3 S14 2.810(2) . ? Bi3 S14 2.810(2) 2_766 ? Ni2 O1 2.138(4) . ? Ni2 N11 2.050(6) . ? Ni2 N10 2.040(6) . ? Ni2 N8 2.057(6) . ? Ni2 N7 2.042(6) . ? Ni2 N9 2.060(6) . ? Ni4 O3 2.125(5) . ? Ni4 O3 2.125(5) 2_776 ? Ni4 N14 2.008(6) 2_776 ? Ni4 N14 2.008(6) . ? Ni4 N15 2.070(6) . ? Ni4 N15 2.070(6) 2_776 ? Ni1 N3 2.038(6) . ? Ni1 N6 2.078(6) . ? Ni1 N4 2.033(6) . ? Ni1 N1 2.093(6) . ? Ni1 N2 2.078(6) . ? Ni1 N5 2.043(6) . ? Ni3 O2 2.148(5) 2_666 ? Ni3 O2 2.148(5) . ? Ni3 N13 2.005(6) . ? Ni3 N13 2.005(6) 2_666 ? Ni3 N12 2.043(6) 2_666 ? Ni3 N12 2.043(6) . ? S9 C9 1.669(7) . ? S11 C11 1.668(7) . ? S3 C3 1.670(8) . ? S5 C5 1.669(7) . ? S7 C7 1.677(8) . ? S8 C8 1.672(7) . ? S1 C1 1.668(7) . ? S2 C2 1.667(8) . ? S6 C6 1.659(7) . ? S10 C10 1.665(8) . ? S4 C4 1.663(8) . ? S15 C15 1.666(8) . ? S12 C12 1.665(8) . ? S13 C13 1.672(8) . ? S14 C14 1.648(7) . ? N3 C3 1.143(8) . ? N11 C11 1.145(8) . ? N6 C6 1.150(8) . ? N10 C10 1.157(8) . ? N8 C8 1.147(8) . ? N4 C4 1.167(9) . ? N1 C1 1.149(8) . ? N2 C2 1.162(9) . ? N7 C7 1.144(8) . ? N9 C9 1.155(8) . ? N13 C13 1.141(9) . ? N5 C5 1.150(8) . ? N14 C14 1.164(8) . ? N12 C12 1.149(9) . ? N15 C15 1.149(9) . ?