#------------------------------------------------------------------------------ #$Date: 2026-05-22 23:51:24 +0100 (Fri, 22 May 2026) $ #$Revision: 306072 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/10/7721043.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_7721043 loop_ _publ_author_name 'Zuo, Jing' 'Zhang, Jun' 'Li, Hongxiu' 'Hu, Chaojie' 'Zhao, Mei-Xin' _publ_section_title ; Nickel Complexes Supported by a New Class of Fused Imidazonaphthyridine Tridentate N,N,N-Ligands for Ethylene Oligomerization and Isolation of a Key Ni-Al Intermediate ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D6DT00825A _journal_year 2026 _chemical_formula_moiety 'C23 H25 Cl2 N5 Ni O' _chemical_formula_sum 'C23 H25 Cl2 N5 Ni O' _chemical_formula_weight 517.09 _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 geom _atom_sites_solution_primary direct _audit_creation_date 2026-01-29 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _audit_update_record ; 2026-03-31 deposited with the CCDC. 2026-05-19 downloaded from the CCDC. ; _cell_angle_alpha 65.2764(9) _cell_angle_beta 82.8550(9) _cell_angle_gamma 65.3355(9) _cell_formula_units_Z 2 _cell_length_a 10.4692(2) _cell_length_b 11.8245(2) _cell_length_c 13.6613(2) _cell_measurement_reflns_used 9882 _cell_measurement_temperature 290.0 _cell_measurement_theta_max 74.46 _cell_measurement_theta_min 4.50 _cell_volume 1393.43(4) _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _diffrn_ambient_temperature 290.0 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.979 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_unetI/netI 0.0321 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.979 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 19502 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.979 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 74.698 _diffrn_reflns_theta_min 3.568 _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.941 _exptl_absorpt_correction_T_max 0.7538 _exptl_absorpt_correction_T_min 0.6369 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0971 before and 0.0457 after correction. The Ratio of minimum to maximum transmission is 0.8449. The \l/2 correction factor is Not present. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.232 _exptl_crystal_description block _exptl_crystal_F_000 536 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.336 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.051 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 313 _refine_ls_number_reflns 5581 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.079 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0419 _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^)+(0.0576P)^2^+0.6748P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1209 _refine_ls_wR_factor_ref 0.1228 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5108 _reflns_number_total 5581 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00825a2.cif _cod_data_source_block a _cod_database_code 7721043 _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 0.757 _shelx_estimated_absorpt_t_min 0.757 _olex2_refinement_description ; 1. Others Fixed Uiso: H1A(0.097) H1B(0.097) H1C(0.097) H4(0.06) H5(0.063) H10(0.068) H11(0.066) H12(0.069) H13(0.067) H16(0.092) H17(0.101) H18(0.095) H20A(0.115) H20B(0.115) H20C(0.115) H21A(0.122) H21B(0.122) H21C(0.122) H22A(0.161) H22B(0.161) H22C(0.161) H23A(0.188) H23B(0.188) H23C(0.188) H24(0.058) H24A(0.057) Fixed X: H1A(0.293988) H1B(0.444609) H1C(0.335199) H4(0.416684) H5(0.42879) H10(0.253721) H11(0.363671) H12(0.098207) H13(0.03003) H16(-0.004995) H17(0.153132) H18(0.359827) H20A(-0.082131) H20B(-0.049157) H20C(0.037192) H21A(0.511117) H21B(0.438686) H21C(0.50943) H22A(-0.127016) H22B(-0.115517) H22C(-0.056101) H23A(0.189908) H23B(0.222499) H23C(0.093779) H24(0.222397) H24A(-0.04267) Fixed Y: H1A(0.481401) H1B(0.37414) H1C(0.44751) H4(0.303561) H5(0.175002) H10(-0.148573) H11(-0.006715) H12(-0.24556) H13(-0.196622) H16(0.567536) H17(0.46096) H18(0.276964) H20A(0.595576) H20B(0.455983) H20C(0.541736) H21A(0.181039) H21B(0.079087) H21C(0.115254) H22A(0.173366) H22B(0.269124) H22C(0.27446) H23A(0.090667) H23B(-0.042488) H23C(0.01052) H24(0.006726) H24A(0.222015) Fixed Z: H1A(0.500845) H1B(0.553039) H1C(0.619426) H4(0.418441) H5(0.325449) H10(0.383675) H11(0.313123) H12(0.55824) H13(0.718075) H16(0.837614) H17(0.980858) H18(0.991169) H20A(0.671393) H20B(0.666579) H20C(0.600406) H21A(0.800202) H21B(0.855481) H21C(0.926343) H22A(1.079772) H22B(0.961003) H22C(1.058078) H23A(1.13631) H23B(1.1206) H23C(1.185498) H24(0.965809) H24A(0.872677) ; _smtbx_masks_special_details ; A solvent mask was calculated and 82 electrons were found in a volume of 312\%A^3^ in 1 void per unit cell. This is consistent with the presence of 2 [C3H7NO] per Asymmetric Unit which account for 80 electrons per unit cell. ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL A in P-1 #2 a.res created by SHELXL-2018/3 at 14:41:28 on 14-Nov-2025 REM reset to P-1 #2 CELL 1.54178 10.4692 11.8245 13.6613 65.2764 82.855 65.3355 ZERR 2 0.0002 0.0002 0.0002 0.0009 0.0009 0.0009 LATT 1 SFAC C H Cl N Ni O UNIT 46 50 4 10 2 2 DFIX 2.1 0.01 C24A C22 L.S. 10 PLAN 99 SIZE 0.1 0.1 0.1 TEMP 16.85 CONF BOND MORE -1 BOND $H ABIN fmap 2 53 acta OMIT 1 1 3 OMIT -1 -1 4 OMIT 0 -1 3 OMIT 1 1 2 OMIT 1 0 2 OMIT 0 -1 5 OMIT 0 0 5 REM REM REM WGHT 0.057600 0.674800 FVAR 0.18017 0.61045 NI1 5 0.164843 0.110687 0.725967 11.00000 0.05400 0.05472 = 0.03157 -0.02349 0.01248 -0.02747 CL1 3 -0.064346 0.252966 0.644596 11.00000 0.05164 0.07033 = 0.07685 -0.04753 0.00553 -0.02144 CL2 3 0.371533 -0.084312 0.813160 11.00000 0.07436 0.05888 = 0.04683 -0.01966 -0.00249 -0.02097 PART 1 O1 6 0.067938 0.123420 0.862611 21.00000 0.05297 0.06362 = 0.02834 -0.02095 0.00865 -0.01982 PART 2 O1A 6 0.125486 0.070519 0.884482 -21.00000 0.05920 0.05477 = 0.03404 -0.01623 0.01177 -0.01385 PART 0 N1 4 0.250094 0.133126 0.581434 11.00000 0.04478 0.04602 = 0.02850 -0.01920 0.00502 -0.01666 N2 4 0.124698 -0.062389 0.662210 11.00000 0.05690 0.05780 = 0.03952 -0.02547 0.00805 -0.02331 N3 4 0.236322 0.264443 0.697157 11.00000 0.04550 0.04471 = 0.03630 -0.02193 0.00492 -0.01802 N4 4 0.060920 0.116285 1.028167 11.00000 0.10110 0.08712 = 0.04374 -0.04063 0.02946 -0.05318 N9 4 0.190354 -0.108704 0.516501 11.00000 0.05106 0.05617 = 0.04638 -0.03190 -0.00173 -0.01471 C1 1 0.346725 0.410663 0.566645 11.00000 0.08284 0.06445 = 0.06206 -0.02960 0.02166 -0.04444 AFIX 137 H1A 2 0.293988 0.481401 0.500845 11.00000 -1.50000 H1B 2 0.444609 0.374140 0.553039 11.00000 -1.50000 H1C 2 0.335199 0.447510 0.619426 11.00000 -1.50000 AFIX 0 C2 1 0.294302 0.299860 0.608160 11.00000 0.04667 0.04433 = 0.03955 -0.01796 0.00430 -0.01874 C3 1 0.307930 0.223379 0.541281 11.00000 0.04465 0.04712 = 0.03136 -0.01589 0.00380 -0.01681 C4 1 0.375981 0.240762 0.445073 11.00000 0.05128 0.05845 = 0.03664 -0.01584 0.00903 -0.02328 AFIX 43 H4 2 0.416684 0.303561 0.418441 11.00000 -1.20000 AFIX 0 C5 1 0.382762 0.164339 0.389385 11.00000 0.04917 0.06734 = 0.03133 -0.02052 0.01015 -0.01760 AFIX 43 H5 2 0.428790 0.175002 0.325449 11.00000 -1.20000 AFIX 0 C6 1 0.320996 0.071961 0.428872 11.00000 0.04307 0.05915 = 0.03142 -0.02444 0.00251 -0.00989 C7 1 0.255131 0.059009 0.527484 11.00000 0.04155 0.04849 = 0.03038 -0.02221 0.00179 -0.01090 C8 1 0.191254 -0.035288 0.572748 11.00000 0.04643 0.04980 = 0.03683 -0.02618 0.00109 -0.01351 C10 1 0.255216 -0.096986 0.419177 11.00000 0.05643 0.07494 = 0.04957 -0.04525 0.00200 -0.01512 AFIX 43 H10 2 0.253721 -0.148573 0.383675 11.00000 -1.20000 AFIX 0 C11 1 0.319101 -0.012162 0.377220 11.00000 0.05275 0.07969 = 0.03836 -0.03893 0.00650 -0.01710 AFIX 43 H11 2 0.363671 -0.006715 0.313123 11.00000 -1.20000 AFIX 0 C12 1 0.117697 -0.185800 0.575278 11.00000 0.05883 0.05910 = 0.06704 -0.03486 -0.00050 -0.02428 AFIX 43 H12 2 0.098207 -0.245560 0.558240 11.00000 -1.20000 AFIX 0 C13 1 0.080017 -0.157130 0.663392 11.00000 0.05818 0.06005 = 0.05424 -0.02487 0.00575 -0.02824 AFIX 43 H13 2 0.030030 -0.196622 0.718075 11.00000 -1.20000 AFIX 0 C14 1 0.217884 0.328836 0.770414 11.00000 0.05592 0.05096 = 0.04568 -0.02986 0.01401 -0.02880 C15 1 0.095804 0.443952 0.760306 11.00000 0.05818 0.05336 = 0.07361 -0.03759 0.01724 -0.02901 C16 1 0.075802 0.491201 0.841841 11.00000 0.07998 0.07890 = 0.10764 -0.07030 0.04263 -0.04384 AFIX 43 H16 2 -0.004995 0.567536 0.837614 11.00000 -1.20000 AFIX 0 C17 1 0.170917 0.428815 0.926848 11.00000 0.11444 0.11055 = 0.07962 -0.07208 0.03959 -0.06828 AFIX 43 H17 2 0.153132 0.460960 0.980858 11.00000 -1.20000 AFIX 0 C18 1 0.294164 0.317677 0.933575 11.00000 0.11286 0.10086 = 0.06064 -0.04834 0.00908 -0.06121 AFIX 43 H18 2 0.359827 0.276964 0.991169 11.00000 -1.20000 AFIX 0 C19 1 0.320578 0.266344 0.854676 11.00000 0.07205 0.06761 = 0.05096 -0.03245 0.00361 -0.03508 C20 1 -0.008945 0.515734 0.666256 11.00000 0.06354 0.05383 = 0.11274 -0.04045 -0.00500 -0.01419 AFIX 137 H20A 2 -0.082131 0.595576 0.671393 11.00000 -1.50000 H20B 2 -0.049157 0.455983 0.666579 11.00000 -1.50000 H20C 2 0.037192 0.541736 0.600406 11.00000 -1.50000 AFIX 0 C21 1 0.457245 0.149963 0.859620 11.00000 0.07859 0.07920 = 0.08388 -0.03636 -0.02849 -0.01742 AFIX 137 H21A 2 0.511117 0.181039 0.800202 11.00000 -1.50000 H21B 2 0.438686 0.079087 0.855481 11.00000 -1.50000 H21C 2 0.509430 0.115254 0.926343 11.00000 -1.50000 AFIX 0 C22 1 -0.069644 0.216120 1.032060 11.00000 0.09341 0.08987 = 0.09749 -0.01087 -0.01059 -0.02224 AFIX 137 H22A 2 -0.127016 0.173366 1.079772 11.00000 -1.50000 H22B 2 -0.115517 0.269124 0.961003 11.00000 -1.50000 H22C 2 -0.056101 0.274460 1.058078 11.00000 -1.50000 AFIX 0 C23 1 0.149005 0.037261 1.125643 11.00000 0.07202 0.12855 = 0.11940 -0.02330 0.01131 -0.01925 AFIX 137 H23A 2 0.189908 0.090667 1.136310 11.00000 -1.50000 H23B 2 0.222499 -0.042488 1.120600 11.00000 -1.50000 H23C 2 0.093779 0.010520 1.185498 11.00000 -1.50000 AFIX 0 PART 1 C24 1 0.130520 0.072682 0.951748 21.00000 0.04539 0.06511 = 0.03154 -0.02090 0.00617 -0.01853 AFIX 43 H24 2 0.222397 0.006726 0.965809 21.00000 -1.20000 AFIX 0 PART 2 C24A 1 0.035232 0.148691 0.915674 -21.00000 0.05345 0.05282 = 0.03633 -0.01693 0.01130 -0.02506 AFIX 43 H24A 2 -0.042670 0.222015 0.872677 -21.00000 -1.20000 AFIX 0 HKLF 4 REM A in P-1 #2 REM wR2 = 0.1228, GooF = S = 1.078, Restrained GooF = 1.079 for all data REM R1 = 0.0419 for 5108 Fo > 4sig(Fo) and 0.0443 for all 5581 data REM 313 parameters refined using 1 restraints END WGHT 0.0578 0.6734 REM Highest difference peak 0.336, deepest hole -0.399, 1-sigma level 0.051 Q1 1 -0.0437 0.2138 0.7006 11.00000 0.05 0.34 Q2 1 0.1579 0.0179 1.0788 11.00000 0.05 0.25 Q3 1 0.2788 0.2772 0.5662 11.00000 0.05 0.24 Q4 1 -0.0159 0.3058 0.6053 11.00000 0.05 0.23 Q5 1 0.1598 0.0985 1.1214 11.00000 0.05 0.21 Q6 1 0.0574 0.4641 0.7204 11.00000 0.05 0.20 Q7 1 0.2938 0.0560 0.4766 11.00000 0.05 0.20 Q8 1 0.2029 0.2052 0.7034 11.00000 0.05 0.20 Q9 1 0.3361 -0.1123 0.8697 11.00000 0.05 0.19 Q10 1 -0.2238 0.3670 1.1386 11.00000 0.05 0.18 Q11 1 0.2698 0.2074 0.5457 11.00000 0.05 0.18 Q12 1 0.1226 -0.0241 1.1808 11.00000 0.05 0.18 Q13 1 0.1015 0.4937 0.7810 11.00000 0.05 0.17 Q14 1 0.2236 0.3044 0.6404 11.00000 0.05 0.17 Q15 1 0.1020 -0.0553 1.1757 11.00000 0.05 0.17 Q16 1 0.2244 0.1265 0.6377 11.00000 0.05 0.17 Q17 1 0.2269 0.0042 0.5580 11.00000 0.05 0.17 Q18 1 0.4786 -0.0716 0.8259 11.00000 0.05 0.17 Q19 1 0.3376 0.2236 0.5006 11.00000 0.05 0.17 Q20 1 0.3275 0.5093 0.9369 11.00000 0.05 0.16 Q21 1 0.2518 0.0905 0.5606 11.00000 0.05 0.16 Q22 1 0.1515 -0.0021 1.1612 11.00000 0.05 0.16 Q23 1 -0.1745 0.3746 0.7546 11.00000 0.05 0.16 Q24 1 0.2021 -0.0727 0.5458 11.00000 0.05 0.16 Q25 1 0.1004 0.0654 0.8164 11.00000 0.05 0.16 Q26 1 -0.1441 0.7390 0.7169 11.00000 0.05 0.16 Q27 1 0.2326 0.2996 0.7252 11.00000 0.05 0.16 Q28 1 0.3590 0.0984 0.4184 11.00000 0.05 0.16 Q29 1 0.1293 0.3780 0.7803 11.00000 0.05 0.16 Q30 1 0.5334 0.1551 0.8852 11.00000 0.05 0.15 Q31 1 0.5130 0.3959 0.1747 11.00000 0.05 0.15 Q32 1 -0.1407 0.5314 0.7058 11.00000 0.05 0.15 Q33 1 0.3724 -0.0983 0.7603 11.00000 0.05 0.15 Q34 1 0.3399 -0.0918 0.4151 11.00000 0.05 0.15 Q35 1 0.2549 0.2865 0.8287 11.00000 0.05 0.15 Q36 1 0.3399 0.1229 0.4097 11.00000 0.05 0.14 Q37 1 0.2141 0.5401 0.6580 11.00000 0.05 0.14 Q38 1 0.2560 0.2422 0.2977 11.00000 0.05 0.14 Q39 1 -0.1393 0.3381 0.9800 11.00000 0.05 0.14 Q40 1 0.1214 0.0373 0.7815 11.00000 0.05 0.14 Q41 1 0.2530 0.2186 1.1039 11.00000 0.05 0.14 Q42 1 0.3230 0.3410 0.5990 11.00000 0.05 0.14 Q43 1 -0.3437 0.4719 0.8006 11.00000 0.05 0.14 Q44 1 -0.1410 0.2034 0.6909 11.00000 0.05 0.14 Q45 1 0.4629 0.0932 0.8231 11.00000 0.05 0.14 Q46 1 -0.2701 0.2814 1.1224 11.00000 0.05 0.14 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0.5552 0.0052 4 10 9 -1.3395 -0.0003 4 10 10 -0.4151 -0.0293 4 10 11 -0.1514 -0.0246 4 10 12 0.0436 -0.0136 4 10 13 0.1979 -0.0082 4 10 14 -0.2788 -0.0362 4 10 15 -0.2687 0.0190 4 10 16 0.0556 0.0976 4 11 0 1.4723 -0.0018 4 11 1 0.6210 -0.0053 4 11 2 -2.1252 -0.0187 4 11 3 -0.9468 -0.0054 4 11 4 1.2607 0.0026 4 11 5 1.6872 -0.0151 4 11 6 0.1812 0.0099 4 11 7 -2.0547 0.0152 4 11 8 -0.4761 0.0034 4 11 9 1.2524 0.0028 4 11 10 0.4190 -0.0010 4 11 11 -0.2966 -0.0046 4 11 12 -0.1621 0.0224 4 11 13 0.1426 0.0195 4 11 14 0.1922 0.0421 4 11 15 0.0042 0.0273 4 12 0 -0.4424 0.0260 4 12 1 -0.5824 0.0312 4 12 2 1.2952 -0.0344 4 12 3 0.9888 -0.0371 4 12 4 -1.0232 -0.0226 4 12 5 -1.1955 0.0073 4 12 6 -0.2183 -0.0012 4 12 7 1.2183 -0.0162 4 12 8 0.5553 0.0060 4 12 9 -0.8331 0.0037 4 12 10 -0.3966 -0.0056 4 12 11 0.4932 0.0221 4 12 12 0.1238 0.0032 4 12 13 -0.2733 -0.0568 4 12 14 -0.0054 -0.0153 4 13 0 -0.1006 0.0145 4 13 1 0.2239 -0.0513 4 13 2 -0.5235 -0.0262 4 13 3 -0.6767 -0.0230 4 13 4 0.5818 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0.0051 10 7 5 0.7230 0.0052 10 7 6 0.9894 0.0180 10 7 7 0.3277 0.0062 10 7 8 -0.3600 0.0050 10 7 9 0.4497 -0.0116 10 7 10 0.5798 -0.0212 10 7 11 -0.5430 -0.0043 10 7 12 -0.3768 0.0105 10 8 0 0.2539 0.0270 10 8 1 -1.9448 -0.0061 10 8 2 -1.0599 -0.0259 10 8 3 1.5097 -0.0015 10 8 4 0.8773 -0.0091 10 8 5 -0.2094 -0.0122 10 8 6 -0.5448 0.0053 10 8 7 -0.7040 0.0222 10 8 8 0.3064 0.0128 10 8 9 0.0022 0.0242 10 8 10 -0.6901 0.0142 10 8 11 0.3280 -0.0013 10 8 12 0.3332 -0.0408 10 9 0 -0.3266 0.0213 10 9 1 0.9339 0.0077 10 9 2 1.0850 -0.0221 10 9 3 -0.7542 -0.0276 10 9 4 -0.8876 -0.0017 10 9 5 -0.3644 0.0080 10 9 6 -0.0193 -0.0085 10 9 7 0.5960 -0.0085 10 9 8 -0.1581 -0.0012 10 9 9 -0.1471 0.0078 10 9 10 0.5959 0.0449 10 9 11 -0.3273 0.0064 10 9 12 -0.4791 -0.0045 10 10 0 0.4418 -0.0487 10 10 1 -0.0213 -0.0127 10 10 2 -0.9729 0.0371 10 10 3 -0.1391 0.0113 10 10 4 0.5904 0.0217 10 10 5 0.6265 0.0158 10 10 6 0.4346 -0.0049 10 10 7 -0.4060 -0.0235 10 10 8 -0.0656 -0.0246 10 10 9 0.2501 -0.0139 10 10 10 -0.4587 -0.0446 10 10 11 0.1680 -0.0034 10 10 12 0.6503 0.0752 10 11 0 -0.2128 0.0333 10 11 1 -0.1668 -0.0010 10 11 2 0.9878 -0.0197 10 11 3 0.6964 0.0391 10 11 4 -0.3903 -0.0060 10 11 5 -0.5590 -0.0143 10 11 6 -0.3098 0.0078 10 11 7 0.4697 0.0024 10 11 8 0.1919 0.0109 10 11 9 -0.5756 0.0028 10 11 10 0.1221 0.0176 10 11 11 0.2134 0.0048 10 12 0 0.0419 -0.0263 10 12 1 0.2490 0.0337 10 12 2 -0.6319 0.0332 10 12 3 -0.7031 -0.0243 10 12 4 0.3846 0.0259 10 12 5 0.5355 -0.0035 10 12 6 0.1696 -0.0460 10 12 7 -0.3204 0.0217 10 12 8 -0.1317 0.0509 10 12 9 0.5840 0.0107 10 12 10 0.1616 -0.0421 10 13 3 0.3845 -0.0040 10 13 4 -0.1777 -0.0685 10 13 5 -0.2832 -0.0082 10 13 6 -0.1189 0.0863 10 13 7 -0.0143 0.0011 10 13 8 0.0168 -0.0897 11 -1 0 0.0164 -0.0056 11 -1 1 -0.2016 0.0515 11 -1 2 0.0236 -0.0262 11 -1 3 0.3190 -0.0302 11 0 0 -0.0294 -0.0305 11 0 1 0.0156 0.0026 11 0 2 0.1173 0.0082 11 0 3 -0.3740 -0.0170 11 0 4 -0.0305 0.0175 11 1 0 -0.3767 0.0560 11 1 1 0.0321 -0.0290 11 1 2 0.0159 -0.0072 11 1 3 0.4183 0.0135 11 1 4 0.3216 0.0051 11 1 5 -0.2571 -0.0185 11 1 6 -0.1006 0.0004 11 2 0 0.9854 -0.0112 11 2 1 -0.0300 0.0038 11 2 2 -0.2519 -0.0178 11 2 4 -0.6133 -0.0092 11 2 5 -0.1886 -0.0184 11 2 6 -0.0139 0.0170 11 2 7 -0.0553 -0.0105 11 3 0 -1.3094 -0.0546 11 3 1 0.0402 0.0043 11 3 2 0.1950 0.0167 11 3 3 -0.1874 -0.0178 11 3 4 0.4892 0.0129 11 3 6 0.1142 -0.0335 11 3 7 -0.0049 -0.0011 11 3 8 -0.2935 -0.0070 11 4 0 1.2722 0.0236 11 4 1 0.0238 -0.0036 11 4 2 -0.2233 0.0150 11 4 3 0.4910 0.0134 11 4 4 -0.3120 -0.0147 11 4 5 -0.4279 0.0065 11 4 6 -0.0701 0.0048 11 4 7 -0.1054 -0.0129 11 4 8 0.3350 -0.0032 11 4 9 0.2140 -0.0271 11 5 0 -1.1645 0.0395 11 5 1 -0.4642 0.0185 11 5 2 0.4832 -0.0018 11 5 3 -0.0426 -0.0078 11 5 4 0.4359 0.0013 11 5 5 0.2251 -0.0061 11 5 6 -0.1859 0.0353 11 5 7 0.3323 0.0319 11 5 8 -0.0869 0.0202 11 5 9 -0.3237 0.0138 11 5 10 0.0899 -0.0020 11 6 0 0.8951 -0.0015 11 6 1 1.1751 -0.0028 11 6 2 -0.4099 -0.0205 11 6 3 -0.5762 0.0080 11 6 4 -0.4798 -0.0001 11 6 5 0.1559 -0.0012 11 6 6 0.4352 -0.0131 11 6 7 -0.4929 -0.0076 11 6 8 -0.2219 -0.0173 11 6 9 0.4725 0.0031 11 6 10 0.0853 0.0102 11 7 0 -0.1192 -0.0376 11 7 1 -1.5630 -0.0067 11 7 2 -0.1933 0.0045 11 7 3 0.8265 -0.0138 11 7 4 0.3294 0.0145 11 7 5 -0.4134 0.0043 11 7 6 -0.4051 -0.0293 11 7 7 0.4211 -0.0185 11 7 8 0.4396 -0.0012 11 7 9 -0.3462 -0.0013 11 7 10 -0.2738 0.0115 11 8 0 -0.6108 -0.0086 11 8 1 1.4629 -0.0114 11 8 2 0.8810 0.0145 11 8 3 -0.7309 -0.0012 11 8 4 -0.2437 -0.0095 11 8 5 0.3883 0.0126 11 8 6 0.2437 0.0151 11 8 7 -0.1849 -0.0236 11 8 8 -0.5791 -0.0151 11 8 9 0.0357 -0.0098 11 8 10 0.4572 -0.0272 11 9 0 0.6458 0.0340 11 9 1 -0.8302 0.0036 11 9 2 -0.7718 -0.0249 11 9 3 0.6106 0.0127 11 9 4 0.2031 0.0013 11 9 5 -0.1945 -0.0126 11 9 6 -0.0091 0.0264 11 9 7 0.0924 0.0590 11 9 8 0.6559 0.0304 11 9 9 0.1417 -0.0106 11 9 10 -0.6498 -0.0395 11 10 0 -0.3552 0.0072 11 10 1 0.0063 -0.0022 11 10 2 0.0743 -0.0070 11 10 3 -0.4683 0.0047 11 10 4 -0.0540 0.0043 11 10 5 0.0055 -0.0153 11 10 6 -0.2856 -0.0452 11 10 7 -0.0302 -0.0340 11 10 8 -0.4017 0.0006 11 10 9 -0.2222 0.0342 11 10 10 0.4932 0.0852 11 11 0 0.1152 -0.0680 11 11 1 0.2758 -0.0151 11 11 2 0.0233 0.0515 11 11 3 -0.0194 -0.0083 11 11 4 -0.0623 -0.0086 11 11 5 0.1530 0.0071 11 11 6 0.4460 0.0156 11 11 7 -0.0911 0.0092 11 11 8 -0.0511 -0.0228 11 11 9 0.2686 -0.0192 11 12 3 0.3615 0.0091 11 12 4 -0.0552 -0.0290 11 12 5 -0.2811 -0.0099 11 12 6 -0.3944 0.0305 11 12 7 -0.0210 0.0052 11 12 8 0.1113 0.0119 12 1 1 0.1881 -0.0072 12 1 2 0.2553 0.0110 12 2 0 0.0493 0.0393 12 2 1 -0.2639 -0.0167 12 2 2 -0.3493 0.0146 12 2 3 0.0457 0.0145 12 2 4 0.3043 0.0135 12 3 0 0.1317 0.0156 12 3 1 0.0037 0.0308 12 3 2 0.1928 -0.0089 12 3 3 0.2028 0.0108 12 3 4 -0.3085 -0.0170 12 3 5 -0.1710 -0.0285 12 4 1 0.3130 -0.0145 12 4 2 0.0308 -0.0066 12 4 3 -0.4626 -0.0264 12 4 4 0.0770 0.0110 12 4 5 0.0607 0.0009 12 4 6 0.0168 -0.0365 12 5 0 0.4104 0.0235 12 5 1 -0.3089 -0.0162 12 5 2 -0.2158 -0.0183 12 5 3 0.5223 -0.0091 12 5 4 -0.0202 -0.0158 12 5 5 -0.0707 0.0304 12 5 6 0.1910 0.0182 12 5 7 -0.2624 -0.0422 12 6 0 -0.4270 0.0377 12 6 1 -0.0933 0.0170 12 6 2 0.2937 0.0180 12 6 3 -0.3849 0.0077 12 6 4 -0.0371 0.0287 12 6 5 0.0782 -0.0065 12 6 6 -0.2645 -0.0027 12 6 7 0.2215 0.0219 12 6 8 0.2204 0.0275 12 7 1 0.4366 -0.0076 12 7 2 -0.1727 0.0024 12 7 3 0.1152 0.0442 12 7 4 0.1422 -0.0227 12 7 5 0.1035 -0.0314 12 7 6 0.2105 0.0131 12 7 7 -0.3119 0.0137 12 7 8 -0.2755 -0.0064 12 8 0 0.3757 -0.0351 12 8 1 -0.3875 0.0177 12 8 2 -0.1338 0.0112 12 8 3 0.1351 -0.0215 12 8 4 -0.1045 0.0244 12 8 5 -0.2749 0.0181 12 8 6 -0.2321 -0.0335 12 8 7 0.2924 0.0021 12 8 8 0.4668 0.0294 12 9 0 -0.4954 -0.0177 12 9 1 0.2814 -0.0317 12 9 2 0.2452 0.0037 12 9 3 -0.4292 -0.0103 12 9 4 -0.0536 -0.0153 12 9 5 0.2933 0.0096 12 9 6 0.2987 0.0149 12 9 7 -0.0812 -0.0420 12 9 8 -0.6307 -0.0616 12 10 1 -0.1559 0.0392 12 10 2 0.1004 -0.0112 12 10 3 0.7635 -0.0158 12 10 4 0.1459 -0.0270 12 10 5 -0.2077 -0.0099 12 10 6 -0.1478 0.0390 12 10 7 -0.0889 0.0546 12 11 5 0.1578 0.0049 13 5 2 0.1635 -0.0092 13 6 2 -0.1463 0.0026 13 6 3 0.2168 -0.0123 13 7 2 0.1027 0.0185 13 7 3 -0.2727 -0.0410 0 0 0 0.0 0.0 ; _shelx_fab_checksum 15279 _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 Ni1 Ni 0.16484(4) 0.11069(4) 0.72597(3) 0.04354(12) Uani 1 1 d . . . . . Cl2 Cl -0.06435(6) 0.25297(7) 0.64460(6) 0.06112(17) Uani 1 1 d . . . . . Cl1 Cl 0.37153(7) -0.08431(6) 0.81316(5) 0.06230(17) Uani 1 1 d . . . . . O1 O 0.0679(5) 0.1234(5) 0.8626(4) 0.0495(11) Uani 0.610(10) 1 d . . P A 1 O1A O 0.1255(8) 0.0705(7) 0.8845(6) 0.0543(18) Uani 0.390(10) 1 d . . P A 2 N2 N 0.25009(17) 0.13313(17) 0.58143(12) 0.0392(3) Uani 1 1 d . . . . . N3 N 0.1247(2) -0.0624(2) 0.66221(14) 0.0498(4) Uani 1 1 d . . . . . N1 N 0.23632(18) 0.26444(17) 0.69716(13) 0.0405(4) Uani 1 1 d . . . . . N5 N 0.0609(3) 0.1163(3) 1.02817(17) 0.0691(6) Uani 1 1 d . . . . . N4 N 0.1904(2) -0.1087(2) 0.51650(15) 0.0492(4) Uani 1 1 d . . . . . C1 C 0.3467(3) 0.4107(3) 0.5666(2) 0.0647(7) Uani 1 1 d . . . . . H1A H 0.293988 0.481401 0.500845 0.097 Uiso 1 1 calc R U . . . H1B H 0.444609 0.374140 0.553039 0.097 Uiso 1 1 calc R U . . . H1C H 0.335199 0.447510 0.619426 0.097 Uiso 1 1 calc R U . . . C2 C 0.2943(2) 0.2999(2) 0.60816(16) 0.0432(4) Uani 1 1 d . . . . . C3 C 0.3079(2) 0.2234(2) 0.54128(15) 0.0419(4) Uani 1 1 d . . . . . C4 C 0.3760(2) 0.2408(2) 0.44507(17) 0.0503(5) Uani 1 1 d . . . . . H4 H 0.416684 0.303561 0.418441 0.060 Uiso 1 1 calc R U . . . C5 C 0.3828(2) 0.1643(3) 0.38939(17) 0.0521(5) Uani 1 1 d . . . . . H5 H 0.428790 0.175002 0.325449 0.063 Uiso 1 1 calc R U . . . C6 C 0.3210(2) 0.0720(2) 0.42887(16) 0.0463(5) Uani 1 1 d . . . . . C12 C 0.2551(2) 0.0590(2) 0.52748(15) 0.0405(4) Uani 1 1 d . . . . . C11 C 0.1913(2) -0.0353(2) 0.57275(16) 0.0432(4) Uani 1 1 d . . . . . C8 C 0.2552(3) -0.0970(3) 0.41918(19) 0.0570(6) Uani 1 1 d . . . . . H10 H 0.253721 -0.148573 0.383675 0.068 Uiso 1 1 calc R U . . . C7 C 0.3191(2) -0.0122(3) 0.37722(18) 0.0554(6) Uani 1 1 d . . . . . H11 H 0.363671 -0.006715 0.313123 0.066 Uiso 1 1 calc R U . . . C9 C 0.1177(3) -0.1858(3) 0.5753(2) 0.0577(6) Uani 1 1 d . . . . . H12 H 0.098207 -0.245560 0.558240 0.069 Uiso 1 1 calc R U . . . C10 C 0.0800(3) -0.1571(3) 0.6634(2) 0.0555(5) Uani 1 1 d . . . . . H13 H 0.030030 -0.196622 0.718075 0.067 Uiso 1 1 calc R U . . . C13 C 0.2179(2) 0.3288(2) 0.77041(17) 0.0455(5) Uani 1 1 d . . . . . C18 C 0.0958(3) 0.4440(2) 0.7603(2) 0.0563(6) Uani 1 1 d . . . . . C17 C 0.0758(3) 0.4912(3) 0.8418(3) 0.0763(9) Uani 1 1 d . . . . . H16 H -0.004995 0.567536 0.837614 0.092 Uiso 1 1 calc R U . . . C16 C 0.1709(4) 0.4288(4) 0.9268(3) 0.0842(10) Uani 1 1 d . . . . . H17 H 0.153132 0.460960 0.980858 0.101 Uiso 1 1 calc R U . . . C15 C 0.2942(4) 0.3177(4) 0.9336(2) 0.0795(9) Uani 1 1 d . . . . . H18 H 0.359827 0.276964 0.991169 0.095 Uiso 1 1 calc R U . . . C14 C 0.3206(3) 0.2663(3) 0.8547(2) 0.0579(6) Uani 1 1 d . . . . . C20 C -0.0089(3) 0.5157(3) 0.6663(3) 0.0767(8) Uani 1 1 d . . . . . H20A H -0.082131 0.595576 0.671393 0.115 Uiso 1 1 calc R U . . . H20B H -0.049157 0.455983 0.666579 0.115 Uiso 1 1 calc R U . . . H20C H 0.037192 0.541736 0.600406 0.115 Uiso 1 1 calc R U . . . C19 C 0.4572(3) 0.1500(3) 0.8596(3) 0.0814(9) Uani 1 1 d . . . . . H21A H 0.511117 0.181039 0.800202 0.122 Uiso 1 1 calc R U . . . H21B H 0.438686 0.079087 0.855481 0.122 Uiso 1 1 calc R U . . . H21C H 0.509430 0.115254 0.926343 0.122 Uiso 1 1 calc R U . . . C21 C -0.0696(4) 0.2161(4) 1.0321(3) 0.1075(13) Uani 1 1 d D . . . . H22A H -0.127016 0.173366 1.079772 0.161 Uiso 1 1 calc R U . . . H22B H -0.115517 0.269124 0.961003 0.161 Uiso 1 1 calc R U . . . H22C H -0.056101 0.274460 1.058078 0.161 Uiso 1 1 calc R U . . . C22 C 0.1490(4) 0.0373(5) 1.1256(4) 0.1251(17) Uani 1 1 d . . . . . H23A H 0.189908 0.090667 1.136310 0.188 Uiso 1 1 calc R U . . . H23B H 0.222499 -0.042488 1.120600 0.188 Uiso 1 1 calc R U . . . H23C H 0.093779 0.010520 1.185498 0.188 Uiso 1 1 calc R U . . . C23A C 0.1305(4) 0.0727(5) 0.9517(4) 0.0487(13) Uani 0.610(10) 1 d . . P A 1 H24 H 0.222397 0.006726 0.965809 0.058 Uiso 0.610(10) 1 calc R U P A 1 C23 C 0.0352(7) 0.1487(7) 0.9157(5) 0.048(2) Uani 0.390(10) 1 d D . P A 2 H24A H -0.042670 0.222015 0.872677 0.057 Uiso 0.390(10) 1 calc R U P A 2 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 Ni1 0.0540(2) 0.0547(2) 0.03157(19) -0.02349(16) 0.01248(15) -0.02747(18) Cl2 0.0516(3) 0.0703(4) 0.0769(4) -0.0475(3) 0.0055(3) -0.0214(3) Cl1 0.0744(4) 0.0589(3) 0.0468(3) -0.0197(3) -0.0025(3) -0.0210(3) O1 0.053(2) 0.064(3) 0.028(2) -0.0209(18) 0.0087(16) -0.0198(18) O1A 0.059(4) 0.055(4) 0.034(4) -0.016(3) 0.012(3) -0.014(3) N2 0.0448(9) 0.0460(9) 0.0285(7) -0.0192(7) 0.0050(6) -0.0167(7) N3 0.0569(11) 0.0578(11) 0.0395(9) -0.0255(8) 0.0080(8) -0.0233(9) N1 0.0455(9) 0.0447(9) 0.0363(8) -0.0219(7) 0.0049(7) -0.0180(7) N5 0.1011(18) 0.0871(16) 0.0437(11) -0.0406(11) 0.0295(11) -0.0532(15) N4 0.0511(10) 0.0562(10) 0.0464(10) -0.0319(9) -0.0017(8) -0.0147(8) C1 0.0828(18) 0.0644(15) 0.0621(15) -0.0296(13) 0.0217(13) -0.0444(14) C2 0.0467(11) 0.0443(10) 0.0396(10) -0.0180(8) 0.0043(8) -0.0187(9) C3 0.0446(10) 0.0471(10) 0.0314(9) -0.0159(8) 0.0038(8) -0.0168(9) C4 0.0513(12) 0.0584(13) 0.0366(10) -0.0158(9) 0.0090(9) -0.0233(10) C5 0.0492(12) 0.0673(14) 0.0313(10) -0.0205(10) 0.0102(8) -0.0176(10) C6 0.0431(11) 0.0591(12) 0.0314(9) -0.0244(9) 0.0025(8) -0.0099(9) C12 0.0415(10) 0.0485(10) 0.0304(9) -0.0222(8) 0.0018(7) -0.0109(8) C11 0.0464(11) 0.0498(11) 0.0368(10) -0.0262(9) 0.0011(8) -0.0135(9) C8 0.0564(13) 0.0749(16) 0.0496(12) -0.0452(12) 0.0020(10) -0.0151(12) C7 0.0528(12) 0.0797(16) 0.0384(11) -0.0389(11) 0.0065(9) -0.0171(12) C9 0.0588(14) 0.0591(13) 0.0670(15) -0.0349(12) -0.0005(11) -0.0243(11) C10 0.0582(13) 0.0600(13) 0.0542(13) -0.0249(11) 0.0058(10) -0.0282(11) C13 0.0559(12) 0.0510(11) 0.0457(11) -0.0299(9) 0.0140(9) -0.0288(10) C18 0.0582(13) 0.0534(12) 0.0736(16) -0.0376(12) 0.0172(12) -0.0290(11) C17 0.0800(19) 0.0789(19) 0.108(2) -0.0703(19) 0.0426(18) -0.0438(16) C16 0.114(3) 0.111(3) 0.080(2) -0.072(2) 0.0396(19) -0.068(2) C15 0.113(3) 0.101(2) 0.0606(16) -0.0483(17) 0.0091(16) -0.061(2) C14 0.0720(16) 0.0676(15) 0.0510(13) -0.0324(12) 0.0036(11) -0.0351(13) C20 0.0635(16) 0.0538(14) 0.113(3) -0.0405(16) -0.0050(16) -0.0142(12) C19 0.0786(19) 0.0792(19) 0.084(2) -0.0364(17) -0.0285(16) -0.0174(16) C21 0.093(3) 0.090(3) 0.097(3) -0.011(2) -0.011(2) -0.022(2) C22 0.072(2) 0.129(4) 0.119(4) -0.023(3) 0.011(2) -0.019(2) C23A 0.045(2) 0.065(3) 0.032(2) -0.0209(18) 0.0062(17) -0.019(2) C23 0.053(4) 0.053(4) 0.036(3) -0.017(3) 0.011(3) -0.025(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 Cl2 Ni1 Cl1 162.32(3) . . ? O1 Ni1 Cl2 83.13(14) . . ? O1 Ni1 Cl1 96.89(14) . . ? O1 Ni1 N1 94.31(13) . . ? O1A Ni1 Cl2 100.5(2) . . ? O1A Ni1 Cl1 78.7(2) . . ? O1A Ni1 N1 97.2(2) . . ? N2 Ni1 Cl2 92.24(5) . . ? N2 Ni1 Cl1 90.17(5) . . ? N2 Ni1 O1 170.12(14) . . ? N2 Ni1 O1A 166.9(2) . . ? N2 Ni1 N1 77.66(6) . . ? N1 Ni1 Cl2 98.09(5) . . ? N1 Ni1 Cl1 99.53(5) . . ? C23A O1 Ni1 124.2(4) . . ? C23 O1A Ni1 124.4(6) . . ? C3 N2 Ni1 116.93(13) . . ? C3 N2 C12 119.60(17) . . ? C12 N2 Ni1 123.42(14) . . ? C11 N3 C10 104.26(18) . . ? C2 N1 Ni1 115.20(13) . . ? C2 N1 C13 121.55(18) . . ? C13 N1 Ni1 123.23(13) . . ? C21 N5 C22 116.4(3) . . ? C21 N5 C23 92.9(4) . . ? C22 N5 C23 150.6(4) . . ? C23A N5 C21 135.6(3) . . ? C23A N5 C22 108.0(3) . . ? C11 N4 C8 122.0(2) . . ? C9 N4 C11 106.41(19) . . ? C9 N4 C8 131.6(2) . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? N1 C2 C1 125.5(2) . . ? N1 C2 C3 115.68(18) . . ? C3 C2 C1 118.82(19) . . ? N2 C3 C2 114.43(17) . . ? N2 C3 C4 121.15(19) . . ? C4 C3 C2 124.4(2) . . ? C3 C4 H4 120.1 . . ? C5 C4 C3 119.7(2) . . ? C5 C4 H4 120.1 . . ? C4 C5 H5 120.1 . . ? C4 C5 C6 119.89(19) . . ? C6 C5 H5 120.1 . . ? C5 C6 C12 117.11(19) . . ? C5 C6 C7 125.1(2) . . ? C12 C6 C7 117.8(2) . . ? N2 C12 C6 122.5(2) . . ? N2 C12 C11 117.76(17) . . ? C6 C12 C11 119.74(18) . . ? N3 C11 N4 111.8(2) . . ? N3 C11 C12 129.39(18) . . ? N4 C11 C12 118.71(18) . . ? N4 C8 H10 120.0 . . ? C7 C8 N4 120.0(2) . . ? C7 C8 H10 120.0 . . ? C6 C7 H11 119.2 . . ? C8 C7 C6 121.6(2) . . ? C8 C7 H11 119.2 . . ? N4 C9 H12 127.1 . . ? C10 C9 N4 105.7(2) . . ? C10 C9 H12 127.1 . . ? N3 C10 H13 124.1 . . ? C9 C10 N3 111.7(2) . . ? C9 C10 H13 124.1 . . ? C18 C13 N1 119.8(2) . . ? C18 C13 C14 122.1(2) . . ? C14 C13 N1 117.9(2) . . ? C13 C18 C17 117.0(3) . . ? C13 C18 C20 121.9(2) . . ? C17 C18 C20 121.1(3) . . ? C18 C17 H16 119.0 . . ? C16 C17 C18 121.9(3) . . ? C16 C17 H16 119.0 . . ? C17 C16 H17 119.8 . . ? C17 C16 C15 120.4(3) . . ? C15 C16 H17 119.8 . . ? C16 C15 H18 119.8 . . ? C16 C15 C14 120.4(3) . . ? C14 C15 H18 119.8 . . ? C13 C14 C19 121.8(2) . . ? C15 C14 C13 118.0(3) . . ? C15 C14 C19 120.2(3) . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C14 C19 H21A 109.5 . . ? C14 C19 H21B 109.5 . . ? C14 C19 H21C 109.5 . . ? H21A C19 H21B 109.5 . . ? H21A C19 H21C 109.5 . . ? H21B C19 H21C 109.5 . . ? N5 C21 H22A 109.5 . . ? N5 C21 H22B 109.5 . . ? N5 C21 H22C 109.5 . . ? H22A C21 H22B 109.5 . . ? H22A C21 H22C 109.5 . . ? H22B C21 H22C 109.5 . . ? N5 C22 H23A 109.5 . . ? N5 C22 H23B 109.5 . . ? N5 C22 H23C 109.5 . . ? H23A C22 H23B 109.5 . . ? H23A C22 H23C 109.5 . . ? H23B C22 H23C 109.5 . . ? O1 C23A N5 117.9(5) . . ? O1 C23A H24 121.1 . . ? N5 C23A H24 121.1 . . ? O1A C23 N5 112.4(7) . . ? O1A C23 H24A 123.8 . . ? N5 C23 H24A 123.8 . . ? 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 Ni1 Cl2 2.3566(7) . ? Ni1 Cl1 2.3659(7) . ? Ni1 O1 2.043(4) . ? Ni1 O1A 2.041(7) . ? Ni1 N2 2.0216(16) . ? Ni1 N1 2.1175(17) . ? O1 C23A 1.237(8) . ? O1A C23 1.195(12) . ? N2 C3 1.332(3) . ? N2 C12 1.344(2) . ? N3 C11 1.315(3) . ? N3 C10 1.376(3) . ? N1 C2 1.275(3) . ? N1 C13 1.444(2) . ? N5 C21 1.397(4) . ? N5 C22 1.429(5) . ? N5 C23A 1.354(5) . ? N5 C23 1.451(7) . ? N4 C11 1.382(3) . ? N4 C8 1.396(3) . ? N4 C9 1.367(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 C2 1.497(3) . ? C2 C3 1.491(3) . ? C3 C4 1.393(3) . ? C4 H4 0.9300 . ? C4 C5 1.381(3) . ? C5 H5 0.9300 . ? C5 C6 1.383(3) . ? C6 C12 1.414(3) . ? C6 C7 1.447(3) . ? C12 C11 1.420(3) . ? C8 H10 0.9300 . ? C8 C7 1.329(4) . ? C7 H11 0.9300 . ? C9 H12 0.9300 . ? C9 C10 1.353(3) . ? C10 H13 0.9300 . ? C13 C18 1.393(3) . ? C13 C14 1.400(3) . ? C18 C17 1.401(4) . ? C18 C20 1.495(4) . ? C17 H16 0.9300 . ? C17 C16 1.357(5) . ? C16 H17 0.9300 . ? C16 C15 1.383(5) . ? C15 H18 0.9300 . ? C15 C14 1.393(4) . ? C14 C19 1.499(4) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C19 H21A 0.9600 . ? C19 H21B 0.9600 . ? C19 H21C 0.9600 . ? C21 H22A 0.9600 . ? C21 H22B 0.9600 . ? C21 H22C 0.9600 . ? C22 H23A 0.9600 . ? C22 H23B 0.9600 . ? C22 H23C 0.9600 . ? C23A H24 0.9300 . ? C23 H24A 0.9300 . ? 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 Ni1 O1 C23A N5 163.8(3) . . . . ? Ni1 O1A C23 N5 -159.4(4) . . . . ? Ni1 N2 C3 C2 -2.8(2) . . . . ? Ni1 N2 C3 C4 176.50(16) . . . . ? Ni1 N2 C12 C6 -177.02(15) . . . . ? Ni1 N2 C12 C11 3.0(3) . . . . ? Ni1 N1 C2 C1 176.76(19) . . . . ? Ni1 N1 C2 C3 -2.5(2) . . . . ? Ni1 N1 C13 C18 -88.6(2) . . . . ? Ni1 N1 C13 C14 87.0(2) . . . . ? N2 C3 C4 C5 0.6(3) . . . . ? N2 C12 C11 N3 0.4(3) . . . . ? N2 C12 C11 N4 177.49(18) . . . . ? N1 C2 C3 N2 3.6(3) . . . . ? N1 C2 C3 C4 -175.7(2) . . . . ? N1 C13 C18 C17 172.0(2) . . . . ? N1 C13 C18 C20 -8.8(4) . . . . ? N1 C13 C14 C15 -171.6(2) . . . . ? N1 C13 C14 C19 10.0(4) . . . . ? N4 C8 C7 C6 -1.4(4) . . . . ? N4 C9 C10 N3 0.8(3) . . . . ? C1 C2 C3 N2 -175.8(2) . . . . ? C1 C2 C3 C4 4.9(3) . . . . ? C2 N1 C13 C18 89.5(3) . . . . ? C2 N1 C13 C14 -95.0(3) . . . . ? C2 C3 C4 C5 179.9(2) . . . . ? C3 N2 C12 C6 0.5(3) . . . . ? C3 N2 C12 C11 -179.54(18) . . . . ? C3 C4 C5 C6 0.6(3) . . . . ? C4 C5 C6 C12 -1.2(3) . . . . ? C4 C5 C6 C7 179.0(2) . . . . ? C5 C6 C12 N2 0.7(3) . . . . ? C5 C6 C12 C11 -179.29(19) . . . . ? C5 C6 C7 C8 -178.7(2) . . . . ? C6 C12 C11 N3 -179.6(2) . . . . ? C6 C12 C11 N4 -2.5(3) . . . . ? C12 N2 C3 C2 179.51(17) . . . . ? C12 N2 C3 C4 -1.2(3) . . . . ? C12 C6 C7 C8 1.4(3) . . . . ? C11 N3 C10 C9 -0.7(3) . . . . ? C11 N4 C8 C7 -0.7(3) . . . . ? C11 N4 C9 C10 -0.6(3) . . . . ? C8 N4 C11 N3 -179.7(2) . . . . ? C8 N4 C11 C12 2.7(3) . . . . ? C8 N4 C9 C10 179.3(2) . . . . ? C7 C6 C12 N2 -179.47(19) . . . . ? C7 C6 C12 C11 0.6(3) . . . . ? C9 N4 C11 N3 0.3(3) . . . . ? C9 N4 C11 C12 -177.31(19) . . . . ? C9 N4 C8 C7 179.3(2) . . . . ? C10 N3 C11 N4 0.2(2) . . . . ? C10 N3 C11 C12 177.5(2) . . . . ? C13 N1 C2 C1 -1.4(3) . . . . ? C13 N1 C2 C3 179.26(18) . . . . ? C13 C18 C17 C16 0.4(4) . . . . ? C18 C13 C14 C15 3.8(4) . . . . ? C18 C13 C14 C19 -174.6(3) . . . . ? C18 C17 C16 C15 2.0(5) . . . . ? C17 C16 C15 C14 -1.6(5) . . . . ? C16 C15 C14 C13 -1.2(4) . . . . ? C16 C15 C14 C19 177.2(3) . . . . ? C14 C13 C18 C17 -3.3(4) . . . . ? C14 C13 C18 C20 175.9(2) . . . . ? C20 C18 C17 C16 -178.8(3) . . . . ? C21 N5 C23A O1 -4.8(7) . . . . ? C21 N5 C23 O1A -173.5(6) . . . . ? C22 N5 C23A O1 175.8(4) . . . . ? C22 N5 C23 O1A 6.2(11) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.500 0.500 0.000 312.4 81.5 '2 DMF'