#------------------------------------------------------------------------------ #$Date: 2024-09-06 02:44:38 +0300 (Fri, 06 Sep 2024) $ #$Revision: 294461 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572136.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_1572136 loop_ _publ_author_name 'Sakurai, Takahiro' 'Tanabe, Tappei' 'Iguchi, Hiroaki' 'Li, Zhuowei' 'Matsuda, Wakana' 'Tsutsui, Yusuke' 'Seki, Shu' 'Matsuda, Ryotaro' 'Shinokubo, Hiroshi' _publ_section_title ; An n-type semiconducting diazaporphyrin-based hydrogen-bonded organic framework. ; _journal_issue 32 _journal_name_full 'Chemical science' _journal_page_first 12922 _journal_page_last 12927 _journal_paper_doi 10.1039/d4sc03455d _journal_volume 15 _journal_year 2024 _chemical_formula_moiety '2(C16 H9 N3 Ni0.5 O2), 4(C2 H3 N)' _chemical_formula_sum 'C40 H30 N10 Ni O4' _chemical_formula_weight 773.45 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-12-07 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2024-02-09 deposited with the CCDC. 2024-07-16 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.948(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.6006(2) _cell_length_b 22.3585(4) _cell_length_c 20.9221(4) _cell_measurement_reflns_used 10778 _cell_measurement_temperature 93 _cell_measurement_theta_max 30.7480 _cell_measurement_theta_min 2.1190 _cell_volume 3554.97(13) _computing_cell_refinement 'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 93 _diffrn_detector CCD _diffrn_detector_type 'Rigaku Saturn-N' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.911 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -110.00 70.00 0.50 3.00 -- -20.00 45.00 0.00 360 2 \w -110.00 70.00 0.50 3.00 -- -20.00 45.00 90.00 360 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku VariMax Saturn' _diffrn_measurement_method 'omega scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0229901000 _diffrn_orient_matrix_UB_12 -0.0022122000 _diffrn_orient_matrix_UB_13 -0.0329240000 _diffrn_orient_matrix_UB_21 -0.0327900000 _diffrn_orient_matrix_UB_22 0.0297024000 _diffrn_orient_matrix_UB_23 0.0005702000 _diffrn_orient_matrix_UB_31 0.0842819000 _diffrn_orient_matrix_UB_32 0.0109176000 _diffrn_orient_matrix_UB_33 -0.0081242000 _diffrn_radiation_monochromator Confocal _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_unetI/netI 0.0704 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.911 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 31951 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.911 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 30.987 _diffrn_reflns_theta_min 2.667 _diffrn_source 'rotating-anode X-ray tubee' _diffrn_source_target Mo _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.605 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.92337 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour purple _exptl_crystal_colour_lustre purple _exptl_crystal_density_diffrn 1.445 _exptl_crystal_description plate _exptl_crystal_F_000 1600 _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.490 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.089 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 505 _refine_ls_number_reflns 10301 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.073 _refine_ls_R_factor_all 0.1202 _refine_ls_R_factor_gt 0.0741 _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^)+(0.0635P)^2^+4.5776P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1546 _refine_ls_wR_factor_ref 0.1761 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6975 _reflns_number_total 10301 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03455d2.cif _cod_data_source_block nidap-cooh-take13_autored _cod_depositor_comments 'Adding full bibliography for 1572136.cif.' _cod_database_code 1572136 _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 0.899 _shelx_estimated_absorpt_t_min 0.764 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Aromatic/amide H refined with riding coordinates: C00D(H00D), C00F(H00F), C00M(H00M), C00N(H00N), C00O(H00O), C00P(H00P), C00R(H00R), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00Y(H00Y), C011(H011), C016(H016), C017(H017), C018(H018) 2.b Idealised Me refined as rotating group: C01F(H01D,H01E,H01F), C01H(H01A,H01B,H01C), C01J(H01J,H01K,H01L), C01K(H01G, H01H,H01I) 2.c Idealised tetrahedral OH refined as rotating group: O003(H003), O004(H004) ; _shelx_res_file ; TITL nidap-cooh-take13_autored_a.res in P2(1)/n nidap-cooh-take13_autored.res created by SHELXL-2018/3 at 20:14:35 on 07-Dec-2023 REM Old TITL NiDAP-COOH-take13_autored in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.148, Rweak 0.013, Alpha 0.044 REM 0.840 for 206 systematic absences, Orientation as input REM Formula found by SHELXT: C40 N10 O4 Br CELL 0.71073 7.6006 22.3585 20.9221 90 90.948 90 ZERR 4 0.0002 0.0004 0.0004 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N Ni O UNIT 160 120 40 4 16 L.S. 4 0 0 PLAN 5 SIZE 0.47 0.22 0.18 TEMP 93 CONF BOND list 4 fmap 2 53 MORE -1 BOND $H acta 52 OMIT 0 0 2 OMIT 0 1 2 OMIT 0 2 0 OMIT 0 2 1 OMIT 1 3 2 REM REM REM WGHT 0.063500 4.577600 FVAR 0.16371 NI01 4 0.500000 0.000000 0.500000 10.50000 0.02243 0.01196 = 0.01389 -0.00048 -0.00428 0.00054 NI02 4 0.000000 0.000000 0.500000 10.50000 0.02230 0.01284 = 0.01470 0.00024 -0.00359 -0.00038 O003 5 0.753133 0.323627 0.803920 11.00000 0.03283 0.01605 = 0.01829 -0.00498 -0.00555 -0.00269 AFIX 147 H003 2 0.776846 0.354606 0.823191 11.00000 -1.50000 AFIX 0 O004 5 -0.323784 0.292987 0.169999 11.00000 0.03325 0.01655 = 0.01712 0.00547 -0.00598 0.00156 AFIX 147 H004 2 -0.335744 0.313250 0.137549 11.00000 -1.50000 AFIX 0 O005 5 -0.246929 0.222231 0.100013 11.00000 0.03935 0.02099 = 0.01722 0.00061 -0.00353 0.00445 O006 5 0.825876 0.378079 0.718276 11.00000 0.03884 0.01676 = 0.02323 -0.00130 -0.00051 -0.00519 N007 3 -0.003463 0.084020 0.482085 11.00000 0.02190 0.01436 = 0.01378 0.00040 -0.00409 0.00002 N008 3 0.493366 0.084961 0.488268 11.00000 0.02227 0.01192 = 0.01462 -0.00057 -0.00394 -0.00053 N009 3 0.130106 0.121838 0.579974 11.00000 0.02294 0.01031 = 0.01661 0.00089 -0.00216 -0.00063 N00A 3 0.356476 0.089834 0.383049 11.00000 0.02334 0.01576 = 0.01285 0.00026 -0.00337 0.00047 N00B 3 0.109516 0.013996 0.581998 11.00000 0.02110 0.01212 = 0.01512 -0.00002 -0.00265 -0.00178 N00C 3 0.390992 -0.012437 0.417557 11.00000 0.02055 0.01262 = 0.01470 -0.00068 -0.00363 0.00033 C00D 1 0.497009 0.187732 0.502459 11.00000 0.02070 0.01333 = 0.01740 -0.00112 -0.00084 -0.00082 AFIX 43 H00D 2 0.512780 0.224837 0.521810 11.00000 -1.20000 AFIX 0 C00E 1 0.061111 0.128061 0.521899 11.00000 0.02160 0.01354 = 0.01554 -0.00247 -0.00190 -0.00027 C00F 1 0.647631 0.229165 0.729620 11.00000 0.02142 0.01963 = 0.01422 -0.00162 -0.00361 0.00199 AFIX 43 H00F 2 0.611669 0.230598 0.771864 11.00000 -1.20000 AFIX 0 C00G 1 0.738341 0.276729 0.704026 11.00000 0.01695 0.01479 = 0.02085 -0.00390 -0.00395 0.00087 C00H 1 0.424890 0.114106 0.435871 11.00000 0.02162 0.01242 = 0.01567 0.00206 0.00031 -0.00067 C00I 1 0.542641 0.130351 0.529799 11.00000 0.02082 0.01224 = 0.01594 -0.00082 -0.00018 0.00013 C00J 1 0.622717 0.122131 0.589331 11.00000 0.01908 0.01470 = 0.01566 -0.00237 -0.00247 0.00008 C00K 1 -0.057198 0.114547 0.427542 11.00000 0.02333 0.01462 = 0.01421 0.00138 -0.00174 -0.00028 C00L 1 0.666135 0.175521 0.629080 11.00000 0.02231 0.01321 = 0.01710 -0.00244 -0.00467 0.00078 C00M 1 -0.311102 0.214292 0.270602 11.00000 0.02097 0.01523 = 0.02357 0.00217 -0.00386 0.00212 AFIX 43 H00M 2 -0.375349 0.249345 0.275505 11.00000 -1.20000 AFIX 0 C00N 1 0.258338 -0.052367 0.326844 11.00000 0.02710 0.01837 = 0.01554 -0.00306 -0.00748 0.00033 AFIX 43 H00N 2 0.210869 -0.080317 0.298516 11.00000 -1.20000 AFIX 0 C00O 1 -0.278431 0.177438 0.322998 11.00000 0.02134 0.01813 = 0.01550 0.00009 -0.00141 0.00097 AFIX 43 H00O 2 -0.322590 0.187861 0.362664 11.00000 -1.20000 AFIX 0 C00P 1 -0.019525 0.177088 0.433911 11.00000 0.02415 0.01244 = 0.01827 0.00293 -0.00131 -0.00017 AFIX 43 H00P 2 -0.040134 0.206319 0.403063 11.00000 -1.20000 AFIX 0 C00Q 1 -0.180812 0.125284 0.316966 11.00000 0.01786 0.01632 = 0.01640 0.00272 -0.00685 -0.00023 C00R 1 0.050707 0.185855 0.492292 11.00000 0.02203 0.01352 = 0.01834 -0.00161 -0.00182 0.00102 AFIX 43 H00R 2 0.085734 0.222156 0.510083 11.00000 -1.20000 AFIX 0 C00S 1 -0.247936 0.198806 0.211037 11.00000 0.02276 0.01593 = 0.01856 0.00403 -0.00548 -0.00361 C00T 1 0.260495 0.007000 0.318717 11.00000 0.02384 0.01688 = 0.01537 -0.00036 -0.00592 0.00209 AFIX 43 H00T 2 0.218274 0.028122 0.283376 11.00000 -1.20000 AFIX 0 C00U 1 0.238562 0.062985 0.668511 11.00000 0.02410 0.01924 = 0.01390 -0.00107 -0.00404 -0.00149 AFIX 43 H00U 2 0.278685 0.093921 0.694647 11.00000 -1.20000 AFIX 0 C00V 1 0.609955 0.179215 0.692485 11.00000 0.02430 0.01745 = 0.01759 0.00145 -0.00215 -0.00060 AFIX 43 H00V 2 0.546584 0.147755 0.709873 11.00000 -1.20000 AFIX 0 C00W 1 0.793167 0.274151 0.641126 11.00000 0.02232 0.01427 = 0.02053 -0.00092 -0.00202 0.00007 AFIX 43 H00W 2 0.853024 0.306327 0.623575 11.00000 -1.20000 AFIX 0 C00X 1 0.341115 0.031599 0.375534 11.00000 0.02042 0.01791 = 0.01438 0.00018 -0.00203 0.00140 C00Y 1 0.427908 0.177730 0.444205 11.00000 0.02334 0.01275 = 0.01749 0.00142 -0.00340 0.00169 AFIX 43 H00Y 2 0.389460 0.206376 0.414929 11.00000 -1.20000 AFIX 0 C00Z 1 -0.134123 0.087669 0.373708 11.00000 0.02211 0.01783 = 0.01530 0.00005 -0.00141 0.00123 C010 1 0.154004 0.068756 0.606718 11.00000 0.01968 0.01825 = 0.01558 -0.00221 -0.00333 -0.00034 C011 1 0.758869 0.223651 0.604340 11.00000 0.02237 0.01766 = 0.01419 -0.00162 -0.00179 0.00169 AFIX 43 H011 2 0.798477 0.221987 0.562558 11.00000 -1.20000 AFIX 0 C012 1 0.162967 -0.026614 0.628663 11.00000 0.02165 0.01362 = 0.01392 -0.00019 -0.00282 0.00074 C013 1 -0.272297 0.238451 0.154344 11.00000 0.02292 0.01680 = 0.01942 0.00341 -0.00649 -0.00164 C014 1 0.778213 0.331554 0.742206 11.00000 0.02281 0.01734 = 0.01808 -0.00076 -0.00512 0.00289 C015 1 0.657110 0.065093 0.612570 11.00000 0.02016 0.01767 = 0.01356 -0.00013 -0.00150 -0.00047 C016 1 0.248006 0.004602 0.680876 11.00000 0.02105 0.01911 = 0.01804 0.00103 -0.00431 -0.00109 AFIX 43 H016 2 0.300181 -0.012872 0.716798 11.00000 -1.20000 AFIX 0 C017 1 -0.155115 0.146034 0.204198 11.00000 0.02627 0.01725 = 0.01669 0.00060 -0.00374 -0.00209 AFIX 43 H017 2 -0.116065 0.134708 0.164082 11.00000 -1.20000 AFIX 0 C018 1 -0.120050 0.110066 0.256501 11.00000 0.02170 0.01400 = 0.01995 -0.00072 -0.00302 -0.00007 AFIX 43 H018 2 -0.055032 0.075207 0.251385 11.00000 -1.20000 AFIX 0 N019 3 1.481600 0.483443 0.328578 11.00000 0.08033 0.04340 = 0.05298 0.00438 -0.00253 0.00301 N01A 3 1.009319 0.597208 0.679693 11.00000 0.12089 0.05701 = 0.03739 -0.00649 0.01667 0.00089 C01B 1 1.491919 0.433157 0.327033 11.00000 0.05281 0.04682 = 0.03693 0.00340 -0.00460 -0.00255 C01C 1 1.022154 0.548323 0.664928 11.00000 0.05953 0.05093 = 0.02818 0.00548 0.00170 -0.00747 N01D 3 1.228647 0.682644 0.543368 11.00000 0.10060 0.04981 = 0.09057 0.01027 0.00008 0.00248 N01E 3 1.241985 0.508599 0.501702 11.00000 0.05927 0.07833 = 0.06839 0.02329 0.00804 -0.00414 C01F 1 1.039158 0.486682 0.646321 11.00000 0.06275 0.04435 = 0.03960 0.00505 -0.00310 -0.01065 AFIX 137 H01D 2 1.012227 0.482747 0.601528 11.00000 -1.50000 H01E 2 0.959075 0.462676 0.670357 11.00000 -1.50000 H01F 2 1.157520 0.473488 0.654663 11.00000 -1.50000 AFIX 0 C01G 1 1.324508 0.543044 0.474348 11.00000 0.05219 0.06334 = 0.05858 0.00968 0.00915 0.00697 C01H 1 1.505102 0.368462 0.322420 11.00000 0.09240 0.04276 = 0.07062 0.00019 -0.00445 0.00199 AFIX 137 H01A 2 1.557816 0.357873 0.282604 11.00000 -1.50000 H01B 2 1.389681 0.351195 0.324414 11.00000 -1.50000 H01C 2 1.576517 0.353583 0.357195 11.00000 -1.50000 AFIX 0 C01I 1 1.089187 0.663393 0.534674 11.00000 0.09209 0.04027 = 0.05377 0.00971 0.00509 0.01652 C01J 1 1.425611 0.585733 0.439667 11.00000 0.06957 0.05199 = 0.07189 0.01654 0.01583 0.00247 AFIX 137 H01J 2 1.368667 0.593778 0.399279 11.00000 -1.50000 H01K 2 1.541131 0.569953 0.432593 11.00000 -1.50000 H01L 2 1.434884 0.622115 0.463855 11.00000 -1.50000 AFIX 0 C01K 1 0.913134 0.638314 0.523716 11.00000 0.10563 0.07133 = 0.07489 0.02258 -0.02694 -0.00047 AFIX 137 H01G 2 0.862496 0.655116 0.485403 11.00000 -1.50000 H01H 2 0.840057 0.647713 0.559331 11.00000 -1.50000 H01I 2 0.921514 0.595682 0.519235 11.00000 -1.50000 AFIX 0 HKLF 4 REM nidap-cooh-take13_autored_a.res in P2(1)/n REM wR2 = 0.1761, GooF = S = 1.073, Restrained GooF = 1.073 for all data REM R1 = 0.0741 for 6975 Fo > 4sig(Fo) and 0.1202 for all 10301 data REM 505 parameters refined using 0 restraints END WGHT 0.0623 4.6992 REM Highest difference peak 0.490, deepest hole -0.596, 1-sigma level 0.089 Q1 1 0.0066 0.1016 0.4990 11.00000 0.05 0.49 Q2 1 -0.1562 0.0616 0.3784 11.00000 0.05 0.49 Q3 1 -0.1215 0.1008 0.4019 11.00000 0.05 0.47 Q4 1 0.7334 0.3004 0.7199 11.00000 0.05 0.46 Q5 1 0.6931 0.0608 0.6416 11.00000 0.05 0.45 ; _shelx_res_checksum 85633 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.360 _oxdiff_exptl_absorpt_empirical_full_min 0.841 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_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 Ni01 Ni 0.500000 0.000000 0.500000 0.01614(13) Uani 1 2 d S . P . . Ni02 Ni 0.000000 0.000000 0.500000 0.01665(13) Uani 1 2 d S . P . . O003 O 0.7531(3) 0.32363(9) 0.80392(10) 0.0225(5) Uani 1 1 d . . . . . H003 H 0.776846 0.354606 0.823191 0.034 Uiso 1 1 calc R U . . . O004 O -0.3238(3) 0.29299(9) 0.17000(10) 0.0224(5) Uani 1 1 d . . . . . H004 H -0.335744 0.313250 0.137549 0.034 Uiso 1 1 calc R U . . . O005 O -0.2469(3) 0.22223(10) 0.10001(10) 0.0259(5) Uani 1 1 d . . . . . O006 O 0.8259(3) 0.37808(9) 0.71828(10) 0.0263(5) Uani 1 1 d . . . . . N007 N -0.0035(3) 0.08402(11) 0.48209(11) 0.0167(5) Uani 1 1 d . . . . . N008 N 0.4934(3) 0.08496(10) 0.48827(11) 0.0163(5) Uani 1 1 d . . . . . N009 N 0.1301(3) 0.12184(10) 0.57997(11) 0.0166(5) Uani 1 1 d . . . . . N00A N 0.3565(3) 0.08983(10) 0.38305(11) 0.0174(5) Uani 1 1 d . . . . . N00B N 0.1095(3) 0.01400(10) 0.58200(11) 0.0161(5) Uani 1 1 d . . . . . N00C N 0.3910(3) -0.01244(10) 0.41756(11) 0.0160(5) Uani 1 1 d . . . . . C00D C 0.4970(4) 0.18773(13) 0.50246(13) 0.0172(6) Uani 1 1 d . . . . . H00D H 0.512780 0.224837 0.521810 0.021 Uiso 1 1 calc R U . . . C00E C 0.0611(4) 0.12806(12) 0.52190(13) 0.0169(6) Uani 1 1 d . . . . . C00F C 0.6476(4) 0.22916(13) 0.72962(13) 0.0185(6) Uani 1 1 d . . . . . H00F H 0.611669 0.230598 0.771864 0.022 Uiso 1 1 calc R U . . . C00G C 0.7383(4) 0.27673(13) 0.70403(14) 0.0176(6) Uani 1 1 d . . . . . C00H C 0.4249(4) 0.11411(12) 0.43587(13) 0.0166(6) Uani 1 1 d . . . . . C00I C 0.5426(4) 0.13035(12) 0.52980(13) 0.0163(6) Uani 1 1 d . . . . . C00J C 0.6227(4) 0.12213(13) 0.58933(13) 0.0165(6) Uani 1 1 d . . . . . C00K C -0.0572(4) 0.11455(13) 0.42754(13) 0.0174(6) Uani 1 1 d . . . . . C00L C 0.6661(4) 0.17552(12) 0.62908(14) 0.0176(6) Uani 1 1 d . . . . . C00M C -0.3111(4) 0.21429(13) 0.27060(14) 0.0200(6) Uani 1 1 d . . . . . H00M H -0.375349 0.249345 0.275505 0.024 Uiso 1 1 calc R U . . . C00N C 0.2583(4) -0.05237(13) 0.32684(14) 0.0204(6) Uani 1 1 d . . . . . H00N H 0.210869 -0.080317 0.298516 0.025 Uiso 1 1 calc R U . . . C00O C -0.2784(4) 0.17744(13) 0.32300(14) 0.0183(6) Uani 1 1 d . . . . . H00O H -0.322590 0.187861 0.362664 0.022 Uiso 1 1 calc R U . . . C00P C -0.0195(4) 0.17709(12) 0.43391(14) 0.0183(6) Uani 1 1 d . . . . . H00P H -0.040134 0.206319 0.403063 0.022 Uiso 1 1 calc R U . . . C00Q C -0.1808(4) 0.12528(13) 0.31697(13) 0.0169(6) Uani 1 1 d . . . . . C00R C 0.0507(4) 0.18585(13) 0.49229(14) 0.0180(6) Uani 1 1 d . . . . . H00R H 0.085734 0.222156 0.510083 0.022 Uiso 1 1 calc R U . . . C00S C -0.2479(4) 0.19881(13) 0.21104(14) 0.0191(6) Uani 1 1 d . . . . . C00T C 0.2605(4) 0.00700(13) 0.31872(14) 0.0188(6) Uani 1 1 d . . . . . H00T H 0.218274 0.028122 0.283376 0.023 Uiso 1 1 calc R U . . . C00U C 0.2386(4) 0.06298(13) 0.66851(13) 0.0191(6) Uani 1 1 d . . . . . H00U H 0.278685 0.093921 0.694647 0.023 Uiso 1 1 calc R U . . . C00V C 0.6100(4) 0.17922(13) 0.69249(14) 0.0198(6) Uani 1 1 d . . . . . H00V H 0.546584 0.147755 0.709873 0.024 Uiso 1 1 calc R U . . . C00W C 0.7932(4) 0.27415(13) 0.64113(14) 0.0191(6) Uani 1 1 d . . . . . H00W H 0.853024 0.306327 0.623575 0.023 Uiso 1 1 calc R U . . . C00X C 0.3411(4) 0.03160(13) 0.37553(13) 0.0176(6) Uani 1 1 d . . . . . C00Y C 0.4279(4) 0.17773(12) 0.44421(14) 0.0179(6) Uani 1 1 d . . . . . H00Y H 0.389460 0.206376 0.414929 0.021 Uiso 1 1 calc R U . . . C00Z C -0.1341(4) 0.08767(13) 0.37371(14) 0.0184(6) Uani 1 1 d . . . . . C010 C 0.1540(4) 0.06876(13) 0.60672(13) 0.0179(6) Uani 1 1 d . . . . . C011 C 0.7589(4) 0.22365(13) 0.60434(13) 0.0181(6) Uani 1 1 d . . . . . H011 H 0.798477 0.221987 0.562558 0.022 Uiso 1 1 calc R U . . . C012 C 0.1630(4) -0.02661(12) 0.62866(13) 0.0164(6) Uani 1 1 d . . . . . C013 C -0.2723(4) 0.23845(13) 0.15434(14) 0.0198(6) Uani 1 1 d . . . . . C014 C 0.7782(4) 0.33155(13) 0.74221(14) 0.0195(6) Uani 1 1 d . . . . . C015 C 0.6571(4) 0.06509(13) 0.61257(13) 0.0171(6) Uani 1 1 d . . . . . C016 C 0.2480(4) 0.00460(13) 0.68088(14) 0.0195(6) Uani 1 1 d . . . . . H016 H 0.300181 -0.012872 0.716798 0.023 Uiso 1 1 calc R U . . . C017 C -0.1551(4) 0.14603(13) 0.20420(14) 0.0201(6) Uani 1 1 d . . . . . H017 H -0.116065 0.134708 0.164082 0.024 Uiso 1 1 calc R U . . . C018 C -0.1200(4) 0.11007(13) 0.25650(14) 0.0186(6) Uani 1 1 d . . . . . H018 H -0.055032 0.075207 0.251385 0.022 Uiso 1 1 calc R U . . . N019 N 1.4816(6) 0.48344(19) 0.32858(19) 0.0589(11) Uani 1 1 d . . . . . N01A N 1.0093(7) 0.5972(2) 0.67969(19) 0.0716(13) Uani 1 1 d . . . . . C01B C 1.4919(6) 0.4332(2) 0.3270(2) 0.0456(10) Uani 1 1 d . . . . . C01C C 1.0222(6) 0.5483(2) 0.66493(19) 0.0462(11) Uani 1 1 d . . . . . N01D N 1.2286(8) 0.6826(2) 0.5434(3) 0.0803(15) Uani 1 1 d . . . . . N01E N 1.2420(5) 0.5086(2) 0.5017(2) 0.0686(13) Uani 1 1 d . . . . . C01F C 1.0392(6) 0.48668(19) 0.6463(2) 0.0489(11) Uani 1 1 d . . . . . H01D H 1.012227 0.482747 0.601528 0.073 Uiso 1 1 calc R U . . . H01E H 0.959075 0.462676 0.670357 0.073 Uiso 1 1 calc R U . . . H01F H 1.157520 0.473488 0.654663 0.073 Uiso 1 1 calc R U . . . C01G C 1.3245(7) 0.5430(2) 0.4743(2) 0.0579(13) Uani 1 1 d . . . . . C01H C 1.5051(8) 0.3685(2) 0.3224(3) 0.0687(15) Uani 1 1 d . . . . . H01A H 1.557816 0.357873 0.282604 0.103 Uiso 1 1 calc R U . . . H01B H 1.389681 0.351195 0.324414 0.103 Uiso 1 1 calc R U . . . H01C H 1.576517 0.353583 0.357195 0.103 Uiso 1 1 calc R U . . . C01I C 1.0892(9) 0.6634(2) 0.5347(2) 0.0620(14) Uani 1 1 d . . . . . C01J C 1.4256(7) 0.5857(2) 0.4397(3) 0.0643(14) Uani 1 1 d . . . . . H01J H 1.368667 0.593778 0.399279 0.096 Uiso 1 1 calc R U . . . H01K H 1.541131 0.569953 0.432593 0.096 Uiso 1 1 calc R U . . . H01L H 1.434884 0.622115 0.463855 0.096 Uiso 1 1 calc R U . . . C01K C 0.9131(9) 0.6383(3) 0.5237(3) 0.0843(19) Uani 1 1 d . . . . . H01G H 0.862496 0.655116 0.485403 0.126 Uiso 1 1 calc R U . . . H01H H 0.840057 0.647713 0.559331 0.126 Uiso 1 1 calc R U . . . H01I H 0.921514 0.595682 0.519235 0.126 Uiso 1 1 calc R U . . . 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 Ni01 0.0224(3) 0.0120(3) 0.0139(2) -0.00048(19) -0.0043(2) 0.0005(2) Ni02 0.0223(3) 0.0128(3) 0.0147(2) 0.00024(19) -0.0036(2) -0.0004(2) O003 0.0328(13) 0.0161(11) 0.0183(10) -0.0050(8) -0.0055(9) -0.0027(9) O004 0.0332(13) 0.0165(11) 0.0171(10) 0.0055(8) -0.0060(9) 0.0016(9) O005 0.0394(14) 0.0210(11) 0.0172(10) 0.0006(8) -0.0035(10) 0.0045(10) O006 0.0388(14) 0.0168(11) 0.0232(11) -0.0013(9) -0.0005(10) -0.0052(10) N007 0.0219(13) 0.0144(12) 0.0138(11) 0.0004(9) -0.0041(10) 0.0000(9) N008 0.0223(13) 0.0119(12) 0.0146(11) -0.0006(9) -0.0039(10) -0.0005(9) N009 0.0229(13) 0.0103(11) 0.0166(12) 0.0009(9) -0.0022(10) -0.0006(9) N00A 0.0233(13) 0.0158(12) 0.0128(11) 0.0003(9) -0.0034(10) 0.0005(10) N00B 0.0211(13) 0.0121(11) 0.0151(11) 0.0000(9) -0.0026(10) -0.0018(9) N00C 0.0206(13) 0.0126(12) 0.0147(11) -0.0007(9) -0.0036(9) 0.0003(9) C00D 0.0207(15) 0.0133(14) 0.0174(13) -0.0011(10) -0.0008(11) -0.0008(11) C00E 0.0216(15) 0.0135(14) 0.0155(13) -0.0025(10) -0.0019(11) -0.0003(11) C00F 0.0214(15) 0.0196(15) 0.0142(13) -0.0016(11) -0.0036(11) 0.0020(12) C00G 0.0170(15) 0.0148(14) 0.0209(14) -0.0039(11) -0.0040(11) 0.0009(11) C00H 0.0216(15) 0.0124(13) 0.0157(13) 0.0021(10) 0.0003(11) -0.0007(11) C00I 0.0208(15) 0.0122(14) 0.0159(13) -0.0008(10) -0.0002(11) 0.0001(11) C00J 0.0191(15) 0.0147(14) 0.0157(13) -0.0024(10) -0.0025(11) 0.0001(11) C00K 0.0233(16) 0.0146(14) 0.0142(13) 0.0014(10) -0.0017(11) -0.0003(11) C00L 0.0223(16) 0.0132(14) 0.0171(13) -0.0024(10) -0.0047(11) 0.0008(11) C00M 0.0210(16) 0.0152(14) 0.0236(15) 0.0022(11) -0.0039(12) 0.0021(12) C00N 0.0271(17) 0.0184(15) 0.0155(13) -0.0031(11) -0.0075(12) 0.0003(12) C00O 0.0213(15) 0.0181(14) 0.0155(13) 0.0001(11) -0.0014(11) 0.0010(12) C00P 0.0242(16) 0.0124(14) 0.0183(14) 0.0029(11) -0.0013(12) -0.0002(11) C00Q 0.0179(15) 0.0163(14) 0.0164(13) 0.0027(10) -0.0068(11) -0.0002(11) C00R 0.0220(15) 0.0135(14) 0.0183(14) -0.0016(10) -0.0018(12) 0.0010(11) C00S 0.0228(16) 0.0159(14) 0.0186(14) 0.0040(11) -0.0055(12) -0.0036(12) C00T 0.0238(16) 0.0169(15) 0.0154(13) -0.0004(10) -0.0059(11) 0.0021(11) C00U 0.0241(16) 0.0192(15) 0.0139(13) -0.0011(11) -0.0040(12) -0.0015(12) C00V 0.0243(16) 0.0175(15) 0.0176(14) 0.0015(11) -0.0021(12) -0.0006(12) C00W 0.0223(16) 0.0143(14) 0.0205(14) -0.0009(11) -0.0020(12) 0.0001(11) C00X 0.0204(15) 0.0179(15) 0.0144(13) 0.0002(11) -0.0020(11) 0.0014(11) C00Y 0.0233(16) 0.0127(14) 0.0175(13) 0.0014(11) -0.0034(12) 0.0017(11) C00Z 0.0221(16) 0.0178(15) 0.0153(13) 0.0000(11) -0.0014(11) 0.0012(12) C010 0.0197(15) 0.0183(15) 0.0156(13) -0.0022(11) -0.0033(11) -0.0003(12) C011 0.0224(15) 0.0177(14) 0.0142(13) -0.0016(11) -0.0018(11) 0.0017(12) C012 0.0216(15) 0.0136(14) 0.0139(13) -0.0002(10) -0.0028(11) 0.0007(11) C013 0.0229(16) 0.0168(15) 0.0194(14) 0.0034(11) -0.0065(12) -0.0016(12) C014 0.0228(16) 0.0173(15) 0.0181(14) -0.0008(11) -0.0051(12) 0.0029(12) C015 0.0202(15) 0.0177(14) 0.0136(13) -0.0001(10) -0.0015(11) -0.0005(11) C016 0.0210(15) 0.0191(15) 0.0180(14) 0.0010(11) -0.0043(11) -0.0011(12) C017 0.0263(17) 0.0173(15) 0.0167(14) 0.0006(11) -0.0037(12) -0.0021(12) C018 0.0217(16) 0.0140(14) 0.0199(14) -0.0007(11) -0.0030(12) -0.0001(11) N019 0.080(3) 0.043(2) 0.053(2) 0.0044(18) -0.003(2) 0.003(2) N01A 0.121(4) 0.057(3) 0.037(2) -0.0065(19) 0.017(2) 0.001(3) C01B 0.053(3) 0.047(3) 0.037(2) 0.0034(18) -0.0046(19) -0.003(2) C01C 0.060(3) 0.051(3) 0.028(2) 0.0055(18) 0.0017(19) -0.007(2) N01D 0.101(4) 0.050(3) 0.091(4) 0.010(2) 0.000(3) 0.002(3) N01E 0.059(3) 0.078(3) 0.068(3) 0.023(2) 0.008(2) -0.004(2) C01F 0.063(3) 0.044(3) 0.040(2) 0.0050(18) -0.003(2) -0.011(2) C01G 0.052(3) 0.063(3) 0.059(3) 0.010(2) 0.009(2) 0.007(2) C01H 0.092(4) 0.043(3) 0.071(4) 0.000(2) -0.004(3) 0.002(3) C01I 0.092(4) 0.040(3) 0.054(3) 0.010(2) 0.005(3) 0.017(3) C01J 0.070(3) 0.052(3) 0.072(3) 0.017(3) 0.016(3) 0.002(2) C01K 0.106(5) 0.071(4) 0.075(4) 0.023(3) -0.027(4) 0.000(4) 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' 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' 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 N008 Ni01 N008 180.0 . 3_656 ? N008 Ni01 N00C 91.06(10) . . ? N008 Ni01 N00C 88.95(10) 3_656 . ? N008 Ni01 N00C 88.94(10) . 3_656 ? N008 Ni01 N00C 91.06(10) 3_656 3_656 ? N00C Ni01 N00C 180.00(6) . 3_656 ? N007 Ni02 N007 180.0 . 3_556 ? N007 Ni02 N00B 88.89(10) . 3_556 ? N007 Ni02 N00B 91.11(10) 3_556 3_556 ? N007 Ni02 N00B 88.89(10) 3_556 . ? N007 Ni02 N00B 91.11(10) . . ? N00B Ni02 N00B 180.0 . 3_556 ? C014 O003 H003 109.5 . . ? C013 O004 H004 109.5 . . ? C00E N007 Ni02 125.46(19) . . ? C00E N007 C00K 104.1(2) . . ? C00K N007 Ni02 130.3(2) . . ? C00H N008 Ni01 125.64(19) . . ? C00H N008 C00I 104.4(2) . . ? C00I N008 Ni01 129.83(19) . . ? C00E N009 C010 122.2(2) . . ? C00X N00A C00H 122.4(2) . . ? C010 N00B Ni02 125.72(19) . . ? C010 N00B C012 104.6(2) . . ? C012 N00B Ni02 129.71(19) . . ? C00X N00C Ni01 125.66(19) . . ? C00X N00C C015 104.6(2) . 3_656 ? C015 N00C Ni01 129.77(19) 3_656 . ? C00I C00D H00D 126.3 . . ? C00Y C00D H00D 126.3 . . ? C00Y C00D C00I 107.5(2) . . ? N007 C00E C00R 111.5(2) . . ? N009 C00E N007 127.8(3) . . ? N009 C00E C00R 120.6(3) . . ? C00G C00F H00F 119.9 . . ? C00G C00F C00V 120.2(3) . . ? C00V C00F H00F 119.9 . . ? C00F C00G C00W 119.7(3) . . ? C00F C00G C014 121.6(3) . . ? C00W C00G C014 118.7(3) . . ? N008 C00H C00Y 111.7(3) . . ? N00A C00H N008 127.5(3) . . ? N00A C00H C00Y 120.8(3) . . ? N008 C00I C00D 110.0(2) . . ? N008 C00I C00J 125.2(3) . . ? C00J C00I C00D 124.8(3) . . ? C00I C00J C00L 119.0(2) . . ? C015 C00J C00I 120.8(3) . . ? C015 C00J C00L 120.1(2) . . ? N007 C00K C00P 110.4(2) . . ? N007 C00K C00Z 124.5(3) . . ? C00Z C00K C00P 125.1(3) . . ? C00V C00L C00J 120.5(3) . . ? C011 C00L C00J 121.4(3) . . ? C011 C00L C00V 118.1(3) . . ? C00O C00M H00M 120.0 . . ? C00S C00M H00M 120.0 . . ? C00S C00M C00O 120.0(3) . . ? C00T C00N H00N 126.2 . . ? C00T C00N C015 107.6(3) . 3_656 ? C015 C00N H00N 126.2 3_656 . ? C00M C00O H00O 119.5 . . ? C00Q C00O C00M 121.0(3) . . ? C00Q C00O H00O 119.5 . . ? C00K C00P H00P 126.2 . . ? C00R C00P C00K 107.7(3) . . ? C00R C00P H00P 126.2 . . ? C00O C00Q C00Z 121.4(3) . . ? C00O C00Q C018 118.2(3) . . ? C018 C00Q C00Z 120.4(3) . . ? C00E C00R H00R 126.9 . . ? C00P C00R C00E 106.3(3) . . ? C00P C00R H00R 126.9 . . ? C00M C00S C013 121.8(3) . . ? C017 C00S C00M 119.4(3) . . ? C017 C00S C013 118.8(3) . . ? C00N C00T H00T 126.9 . . ? C00N C00T C00X 106.3(3) . . ? C00X C00T H00T 126.9 . . ? C010 C00U H00U 126.8 . . ? C016 C00U H00U 126.8 . . ? C016 C00U C010 106.5(3) . . ? C00F C00V C00L 120.9(3) . . ? C00F C00V H00V 119.5 . . ? C00L C00V H00V 119.5 . . ? C00G C00W H00W 119.9 . . ? C00G C00W C011 120.2(3) . . ? C011 C00W H00W 119.9 . . ? N00A C00X N00C 127.7(3) . . ? N00A C00X C00T 120.9(3) . . ? N00C C00X C00T 111.4(2) . . ? C00D C00Y C00H 106.4(3) . . ? C00D C00Y H00Y 126.8 . . ? C00H C00Y H00Y 126.8 . . ? C00K C00Z C00Q 119.3(3) . . ? C012 C00Z C00K 121.2(3) 3_556 . ? C012 C00Z C00Q 119.5(3) 3_556 . ? N009 C010 N00B 127.7(3) . . ? N009 C010 C00U 121.1(3) . . ? N00B C010 C00U 111.3(3) . . ? C00L C011 H011 119.5 . . ? C00W C011 C00L 121.0(3) . . ? C00W C011 H011 119.5 . . ? N00B C012 C016 109.8(2) . . ? C00Z C012 N00B 125.1(3) 3_556 . ? C00Z C012 C016 125.0(3) 3_556 . ? O004 C013 C00S 112.6(3) . . ? O005 C013 O004 124.1(3) . . ? O005 C013 C00S 123.3(3) . . ? O003 C014 C00G 112.5(3) . . ? O006 C014 O003 124.6(3) . . ? O006 C014 C00G 122.9(3) . . ? N00C C015 C00J 125.2(3) 3_656 . ? N00C C015 C00N 110.1(2) 3_656 3_656 ? C00J C015 C00N 124.7(3) . 3_656 ? C00U C016 C012 107.8(3) . . ? C00U C016 H016 126.1 . . ? C012 C016 H016 126.1 . . ? C00S C017 H017 119.8 . . ? C018 C017 C00S 120.5(3) . . ? C018 C017 H017 119.8 . . ? C00Q C018 H018 119.5 . . ? C017 C018 C00Q 120.9(3) . . ? C017 C018 H018 119.5 . . ? N019 C01B C01H 177.8(5) . . ? N01A C01C C01F 179.8(6) . . ? C01C C01F H01D 109.5 . . ? C01C C01F H01E 109.5 . . ? C01C C01F H01F 109.5 . . ? H01D C01F H01E 109.5 . . ? H01D C01F H01F 109.5 . . ? H01E C01F H01F 109.5 . . ? N01E C01G C01J 179.3(6) . . ? C01B C01H H01A 109.5 . . ? C01B C01H H01B 109.5 . . ? C01B C01H H01C 109.5 . . ? H01A C01H H01B 109.5 . . ? H01A C01H H01C 109.5 . . ? H01B C01H H01C 109.5 . . ? N01D C01I C01K 179.4(6) . . ? C01G C01J H01J 109.5 . . ? C01G C01J H01K 109.5 . . ? C01G C01J H01L 109.5 . . ? H01J C01J H01K 109.5 . . ? H01J C01J H01L 109.5 . . ? H01K C01J H01L 109.5 . . ? C01I C01K H01G 109.5 . . ? C01I C01K H01H 109.5 . . ? C01I C01K H01I 109.5 . . ? H01G C01K H01H 109.5 . . ? H01G C01K H01I 109.5 . . ? H01H C01K H01I 109.5 . . ? 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 Ni01 N008 1.916(2) . ? Ni01 N008 1.916(2) 3_656 ? Ni01 N00C 1.921(2) 3_656 ? Ni01 N00C 1.921(2) . ? Ni02 N007 1.916(2) 3_556 ? Ni02 N007 1.916(2) . ? Ni02 N00B 1.920(2) . ? Ni02 N00B 1.920(2) 3_556 ? O003 H003 0.8200 . ? O003 C014 1.320(3) . ? O004 H004 0.8200 . ? O004 C013 1.323(4) . ? O005 C013 1.212(4) . ? O006 C014 1.212(4) . ? N007 C00E 1.375(4) . ? N007 C00K 1.385(4) . ? N008 C00H 1.371(4) . ? N008 C00I 1.384(4) . ? N009 C00E 1.323(4) . ? N009 C010 1.323(4) . ? N00A C00H 1.329(4) . ? N00A C00X 1.316(4) . ? N00B C010 1.369(4) . ? N00B C012 1.389(4) . ? N00C C00X 1.369(4) . ? N00C C015 1.382(4) 3_656 ? C00D H00D 0.9300 . ? C00D C00I 1.445(4) . ? C00D C00Y 1.338(4) . ? C00E C00R 1.435(4) . ? C00F H00F 0.9300 . ? C00F C00G 1.380(4) . ? C00F C00V 1.388(4) . ? C00G C00W 1.388(4) . ? C00G C014 1.491(4) . ? C00H C00Y 1.433(4) . ? C00I C00J 1.389(4) . ? C00J C00L 1.489(4) . ? C00J C015 1.388(4) . ? C00K C00P 1.433(4) . ? C00K C00Z 1.396(4) . ? C00L C00V 1.403(4) . ? C00L C011 1.391(4) . ? C00M H00M 0.9300 . ? C00M C00O 1.390(4) . ? C00M C00S 1.387(4) . ? C00N H00N 0.9300 . ? C00N C00T 1.338(4) . ? C00N C015 1.440(4) 3_656 ? C00O H00O 0.9300 . ? C00O C00Q 1.389(4) . ? C00P H00P 0.9300 . ? C00P C00R 1.339(4) . ? C00Q C00Z 1.493(4) . ? C00Q C018 1.396(4) . ? C00R H00R 0.9300 . ? C00S C013 1.490(4) . ? C00S C017 1.383(4) . ? C00T H00T 0.9300 . ? C00T C00X 1.438(4) . ? C00U H00U 0.9300 . ? C00U C010 1.440(4) . ? C00U C016 1.332(4) . ? C00V H00V 0.9300 . ? C00W H00W 0.9300 . ? C00W C011 1.389(4) . ? C00Y H00Y 0.9300 . ? C00Z C012 1.383(4) 3_556 ? C011 H011 0.9300 . ? C012 C016 1.440(4) . ? C016 H016 0.9300 . ? C017 H017 0.9300 . ? C017 C018 1.380(4) . ? C018 H018 0.9300 . ? N019 C01B 1.128(5) . ? N01A C01C 1.140(6) . ? C01B C01H 1.453(6) . ? C01C C01F 1.439(6) . ? N01D C01I 1.156(7) . ? N01E C01G 1.151(6) . ? C01F H01D 0.9600 . ? C01F H01E 0.9600 . ? C01F H01F 0.9600 . ? C01G C01J 1.431(7) . ? C01H H01A 0.9600 . ? C01H H01B 0.9600 . ? C01H H01C 0.9600 . ? C01I C01K 1.465(8) . ? C01J H01J 0.9600 . ? C01J H01K 0.9600 . ? C01J H01L 0.9600 . ? C01K H01G 0.9600 . ? C01K H01H 0.9600 . ? C01K H01I 0.9600 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ni01 N008 C00H N00A -2.4(4) . . . . ? Ni01 N008 C00H C00Y 175.4(2) . . . . ? Ni01 N008 C00I C00D -174.1(2) . . . . ? Ni01 N008 C00I C00J 5.3(4) . . . . ? Ni01 N00C C00X N00A -0.4(5) . . . . ? Ni01 N00C C00X C00T -178.9(2) . . . . ? Ni02 N007 C00E N009 -2.9(4) . . . . ? Ni02 N007 C00E C00R 175.5(2) . . . . ? Ni02 N007 C00K C00P -174.3(2) . . . . ? Ni02 N007 C00K C00Z 4.6(5) . . . . ? Ni02 N00B C010 N009 0.5(4) . . . . ? Ni02 N00B C010 C00U -178.3(2) . . . . ? Ni02 N00B C012 C00Z -5.1(4) . . . 3_556 ? Ni02 N00B C012 C016 176.7(2) . . . . ? N007 C00E C00R C00P -0.4(4) . . . . ? N007 C00K C00P C00R -2.2(4) . . . . ? N007 C00K C00Z C00Q -177.9(3) . . . . ? N007 C00K C00Z C012 0.1(5) . . . 3_556 ? N008 C00H C00Y C00D -0.7(3) . . . . ? N008 C00I C00J C00L -179.3(3) . . . . ? N008 C00I C00J C015 -1.3(5) . . . . ? N009 C00E C00R C00P 178.2(3) . . . . ? N00A C00H C00Y C00D 177.4(3) . . . . ? N00B C012 C016 C00U 3.3(4) . . . . ? C00D C00I C00J C00L 0.1(4) . . . . ? C00D C00I C00J C015 178.1(3) . . . . ? C00E N007 C00K C00P 1.8(3) . . . . ? C00E N007 C00K C00Z -179.3(3) . . . . ? C00E N009 C010 N00B -2.3(5) . . . . ? C00E N009 C010 C00U 176.4(3) . . . . ? C00F C00G C00W C011 -0.8(4) . . . . ? C00F C00G C014 O003 13.9(4) . . . . ? C00F C00G C014 O006 -165.1(3) . . . . ? C00G C00F C00V C00L 1.4(4) . . . . ? C00G C00W C011 C00L 1.5(4) . . . . ? C00H N008 C00I C00D 2.0(3) . . . . ? C00H N008 C00I C00J -178.6(3) . . . . ? C00H N00A C00X N00C -0.7(5) . . . . ? C00H N00A C00X C00T 177.7(3) . . . . ? C00I N008 C00H N00A -178.8(3) . . . . ? C00I N008 C00H C00Y -0.9(3) . . . . ? C00I C00D C00Y C00H 1.8(3) . . . . ? C00I C00J C00L C00V 127.5(3) . . . . ? C00I C00J C00L C011 -50.8(4) . . . . ? C00I C00J C015 N00C -3.8(5) . . . 3_656 ? C00I C00J C015 C00N 179.1(3) . . . 3_656 ? C00J C00L C00V C00F -179.1(3) . . . . ? C00J C00L C011 C00W 177.7(3) . . . . ? C00K N007 C00E N009 -179.3(3) . . . . ? C00K N007 C00E C00R -0.9(3) . . . . ? C00K C00P C00R C00E 1.5(3) . . . . ? C00L C00J C015 N00C 174.2(3) . . . 3_656 ? C00L C00J C015 C00N -3.0(5) . . . 3_656 ? C00M C00O C00Q C00Z 175.6(3) . . . . ? C00M C00O C00Q C018 -1.6(4) . . . . ? C00M C00S C013 O004 13.5(4) . . . . ? C00M C00S C013 O005 -166.7(3) . . . . ? C00M C00S C017 C018 -2.3(5) . . . . ? C00N C00T C00X N00A -177.5(3) . . . . ? C00N C00T C00X N00C 1.2(4) . . . . ? C00O C00M C00S C013 -176.9(3) . . . . ? C00O C00M C00S C017 1.1(4) . . . . ? C00O C00Q C00Z C00K -50.6(4) . . . . ? C00O C00Q C00Z C012 131.3(3) . . . 3_556 ? C00O C00Q C018 C017 0.4(4) . . . . ? C00P C00K C00Z C00Q 0.8(5) . . . . ? C00P C00K C00Z C012 178.9(3) . . . 3_556 ? C00S C00M C00O C00Q 0.9(5) . . . . ? C00S C017 C018 C00Q 1.6(5) . . . . ? C00V C00F C00G C00W -0.6(4) . . . . ? C00V C00F C00G C014 178.9(3) . . . . ? C00V C00L C011 C00W -0.7(4) . . . . ? C00W C00G C014 O003 -166.6(3) . . . . ? C00W C00G C014 O006 14.3(4) . . . . ? C00X N00A C00H N008 2.2(5) . . . . ? C00X N00A C00H C00Y -175.5(3) . . . . ? C00Y C00D C00I N008 -2.5(3) . . . . ? C00Y C00D C00I C00J 178.1(3) . . . . ? C00Z C00K C00P C00R 178.9(3) . . . . ? C00Z C00Q C018 C017 -176.8(3) . . . . ? C00Z C012 C016 C00U -174.8(3) 3_556 . . . ? C010 N009 C00E N007 3.6(5) . . . . ? C010 N009 C00E C00R -174.7(3) . . . . ? C010 N00B C012 C00Z 175.6(3) . . . 3_556 ? C010 N00B C012 C016 -2.6(3) . . . . ? C010 C00U C016 C012 -2.5(3) . . . . ? C011 C00L C00V C00F -0.7(4) . . . . ? C012 N00B C010 N009 179.8(3) . . . . ? C012 N00B C010 C00U 1.1(3) . . . . ? C013 C00S C017 C018 175.8(3) . . . . ? C014 C00G C00W C011 179.7(3) . . . . ? C015 N00C C00X N00A 178.8(3) 3_656 . . . ? C015 N00C C00X C00T 0.3(3) 3_656 . . . ? C015 C00J C00L C00V -50.6(4) . . . . ? C015 C00J C00L C011 131.2(3) . . . . ? C015 C00N C00T C00X -2.0(3) 3_656 . . . ? C016 C00U C010 N009 -177.9(3) . . . . ? C016 C00U C010 N00B 1.0(4) . . . . ? C017 C00S C013 O004 -164.5(3) . . . . ? C017 C00S C013 O005 15.3(5) . . . . ? C018 C00Q C00Z C00K 126.5(3) . . . . ? C018 C00Q C00Z C012 -51.6(4) . . . 3_556 ?