#------------------------------------------------------------------------------ #$Date: 2019-12-20 12:28:44 +0200 (Fri, 20 Dec 2019) $ #$Revision: 245431 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/66/1556694.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_1556694 loop_ _publ_author_name 'Wang, D.' 'Moutet, J.' 'Tricoire, M.' 'Cordier, M.' 'Nocton, G.' _publ_section_title ; Reactive Heterobimetallic Complex Combining Divalent Ytterbium and Dimethyl Nickel Fragments ; _journal_name_full Inorganics _journal_page_first 58 _journal_paper_doi 10.3390/inorganics7050058 _journal_volume 7 _journal_year 2019 _chemical_formula_moiety 'C10 H12 N4 Ni' _chemical_formula_sum 'C10 H12 N4 Ni' _chemical_formula_weight 246.95 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _cell_angle_alpha 90 _cell_angle_beta 105.255(3) _cell_angle_gamma 90 _cell_formula_units_Z 16 _cell_length_a 9.5916(10) _cell_length_b 33.666(3) _cell_length_c 13.3219(13) _cell_measurement_reflns_used 4640 _cell_measurement_temperature 150.0(1) _cell_measurement_theta_max 27.5370 _cell_measurement_theta_min 2.4199 _cell_volume 4150.2(7) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution SHELXT(Sheldrick,2014) _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'Kappa APEX II' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_unetI/netI 0.0368 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 13457 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.240 _diffrn_reflns_theta_max 25.680 _diffrn_reflns_theta_min 2.282 _exptl_absorpt_coefficient_mu 1.839 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6496 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.581 _exptl_crystal_description needle _exptl_crystal_F_000 2048 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.020 _refine_diff_density_max 0.376 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.062 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 275 _refine_ls_number_reflns 3910 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.038 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0308 _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^)+(0.0391P)^2^+2.5054P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0742 _refine_ls_wR_factor_ref 0.0793 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3204 _reflns_number_total 3910 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file Inorganics-2019-7-58.cif _cod_data_source_block 1 _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 1556694 _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_min 0.608 _shelx_estimated_absorpt_t_max 0.964 _shelx_res_file ; aj222_a.res created by SHELXL-2014/7 TITL aj222_a.res in P-1 New: C2/c CELL 0.71069 9.5916 33.6660 13.3219 90.000 105.255 90.000 ZERR 16 0.0010 0.0030 0.0013 0.000 0.003 0.000 LATT 7 SYMM - X , Y , 0.50000 - Z SFAC C H N NI UNIT 160 192 64 16 L.S. 5 FMAP 2 PLAN -20 ACTA BOND $H SHEL 20.0 0.82 OMIT 0 2 0 SIZE 0.30 0.04 0.02 TEMP -123 CONF WGHT 0.039100 2.505400 FVAR 0.14336 RESI 0 NI1 4 0.808342 0.048536 0.690060 11.00000 0.03850 0.01894 = 0.02866 0.00014 0.01640 -0.00454 N1 3 0.896116 0.078166 0.596056 11.00000 0.03271 0.01820 = 0.02660 -0.00222 0.01326 0.00093 N2 3 0.942686 0.144758 0.548688 11.00000 0.03515 0.02220 = 0.02768 0.00002 0.01696 -0.00271 N3 3 0.775088 0.102414 0.735071 11.00000 0.03032 0.02201 = 0.02459 0.00115 0.01073 -0.00248 N4 3 0.803344 0.171024 0.695418 11.00000 0.03490 0.02211 = 0.03178 -0.00122 0.01645 0.00076 C1 1 0.962325 0.064671 0.525244 11.00000 0.04442 0.02073 = 0.03546 -0.00290 0.02102 -0.00047 AFIX 43 H1 2 0.970484 0.036801 0.517154 11.00000 -1.20000 AFIX 0 C2 1 1.018284 0.089550 0.464511 11.00000 0.04539 0.03145 = 0.03376 -0.00199 0.02510 0.00182 AFIX 43 H2 2 1.064826 0.079470 0.415095 11.00000 -1.20000 AFIX 0 C3 1 1.004396 0.129899 0.477929 11.00000 0.04232 0.02910 = 0.03240 0.00306 0.02431 -0.00299 AFIX 43 H3 2 1.040044 0.147728 0.435265 11.00000 -1.20000 AFIX 0 C4 1 0.891598 0.118312 0.604237 11.00000 0.02417 0.02114 = 0.02046 0.00045 0.00838 -0.00094 C5 1 0.819973 0.132278 0.683261 11.00000 0.02365 0.02261 = 0.02064 -0.00101 0.00959 0.00061 C6 1 0.733188 0.181041 0.766265 11.00000 0.04210 0.02461 = 0.03737 -0.00165 0.01966 0.00503 AFIX 43 H6 2 0.719537 0.208418 0.778137 11.00000 -1.20000 AFIX 0 C7 1 0.680042 0.153396 0.822587 11.00000 0.03774 0.03684 = 0.03295 -0.00213 0.01935 0.00318 AFIX 43 H7 2 0.629176 0.161214 0.871659 11.00000 -1.20000 AFIX 0 C8 1 0.703312 0.114070 0.805180 11.00000 0.03893 0.02837 = 0.02989 0.00315 0.02088 -0.00351 AFIX 43 H8 2 0.668053 0.094414 0.843422 11.00000 -1.20000 AFIX 0 C9 1 0.729822 0.020996 0.789692 11.00000 0.07196 0.02856 = 0.04895 0.00145 0.03457 -0.01250 AFIX 137 H9A 2 0.625939 0.016854 0.760262 11.00000 -1.50000 H9B 2 0.745624 0.036897 0.853318 11.00000 -1.50000 H9C 2 0.777977 -0.004767 0.806157 11.00000 -1.50000 AFIX 0 C10 1 0.831832 -0.002677 0.631430 11.00000 0.05310 0.02063 = 0.04061 -0.00133 0.02007 -0.00434 AFIX 137 H10A 2 0.934630 -0.009641 0.649161 11.00000 -1.50000 H10B 2 0.794008 -0.001609 0.555607 11.00000 -1.50000 H10C 2 0.778785 -0.022780 0.659757 11.00000 -1.50000 AFIX 0 NI2 4 0.300464 0.160017 0.200689 11.00000 0.02512 0.02592 = 0.02407 -0.00013 0.01168 -0.00020 N5 3 0.379963 0.119729 0.125384 11.00000 0.02463 0.02220 = 0.02445 0.00089 0.00898 -0.00281 N6 3 0.491270 0.112649 -0.015314 11.00000 0.03622 0.02030 = 0.02893 -0.00366 0.01599 -0.00163 N7 3 0.381642 0.195784 0.114687 11.00000 0.02571 0.02121 = 0.02506 -0.00173 0.00926 0.00398 N8 3 0.509114 0.195307 -0.017951 11.00000 0.03705 0.02103 = 0.02825 0.00265 0.01532 -0.00426 C11 1 0.379033 0.079574 0.133210 11.00000 0.03366 0.02207 = 0.03155 0.00335 0.01157 -0.00587 AFIX 43 H11 2 0.338538 0.067801 0.183925 11.00000 -1.20000 AFIX 0 C12 1 0.434346 0.055458 0.070651 11.00000 0.04562 0.01763 = 0.04299 0.00006 0.01672 -0.00298 AFIX 43 H12 2 0.436354 0.027431 0.079207 11.00000 -1.20000 AFIX 0 C13 1 0.486961 0.073024 -0.005005 11.00000 0.04641 0.02521 = 0.03850 -0.00674 0.01903 -0.00093 AFIX 43 H13 2 0.521328 0.056641 -0.051423 11.00000 -1.20000 AFIX 0 C14 1 0.439844 0.133688 0.050484 11.00000 0.02381 0.02124 = 0.02341 0.00108 0.00652 -0.00296 C15 1 0.444737 0.177820 0.047240 11.00000 0.02389 0.02070 = 0.02147 0.00065 0.00616 -0.00049 C16 1 0.512216 0.235079 -0.014600 11.00000 0.03807 0.02573 = 0.03401 0.00701 0.01340 -0.00287 AFIX 43 H16 2 0.557101 0.248910 -0.059869 11.00000 -1.20000 AFIX 0 C17 1 0.453202 0.256749 0.051570 11.00000 0.03834 0.02301 = 0.03814 0.00288 0.01166 0.00296 AFIX 43 H17 2 0.457455 0.284941 0.053158 11.00000 -1.20000 AFIX 0 C18 1 0.387877 0.235867 0.115232 11.00000 0.03149 0.02171 = 0.03233 -0.00202 0.01084 0.00383 AFIX 43 H18 2 0.345567 0.250119 0.161294 11.00000 -1.20000 AFIX 0 C19 1 0.212315 0.202058 0.261766 11.00000 0.04132 0.03961 = 0.04222 0.00083 0.02456 0.00503 AFIX 137 H19A 2 0.151588 0.190449 0.302908 11.00000 -1.50000 H19B 2 0.152737 0.218646 0.206417 11.00000 -1.50000 H19C 2 0.287964 0.218376 0.306916 11.00000 -1.50000 AFIX 0 C20 1 0.229303 0.123746 0.287650 11.00000 0.04672 0.03923 = 0.04325 0.00519 0.02984 -0.00047 AFIX 137 H20A 2 0.287210 0.099377 0.297536 11.00000 -1.50000 H20B 2 0.128103 0.117267 0.254265 11.00000 -1.50000 H20C 2 0.236416 0.136151 0.355362 11.00000 -1.50000 AFIX 0 HKLF 4 1 1.0000 0.0000 0.0000 -1.0000 0.0000 2.0000 0.0000 -1.0000 0.0000 REM aj222_a.res in P-1 New: C2/c REM R1 = 0.0308 for 3204 Fo > 4sig(Fo) and 0.0423 for all 3910 data REM 275 parameters refined using 0 restraints END WGHT 0.0336 3.7809 REM Highest difference peak 0.376, deepest hole -0.244, 1-sigma level 0.062 Q1 1 0.6934 0.0462 0.6583 11.00000 0.05 0.38 Q2 1 0.8866 0.0993 0.5983 11.00000 0.05 0.30 Q3 1 0.3770 0.1015 0.1253 11.00000 0.05 0.29 Q4 1 0.4146 0.1609 0.2271 11.00000 0.05 0.28 Q5 1 0.8643 0.1226 0.6455 11.00000 0.05 0.28 Q6 1 0.9125 0.0460 0.7190 11.00000 0.05 0.27 Q7 1 0.3788 0.1328 0.1821 11.00000 0.05 0.26 Q8 1 0.1351 0.1325 0.2817 11.00000 0.05 0.25 Q9 1 0.7636 0.0200 0.6048 11.00000 0.05 0.25 Q10 1 0.5331 0.1193 -0.0434 11.00000 0.05 0.25 Q11 1 0.3838 0.2169 0.1165 11.00000 0.05 0.25 Q12 1 0.6415 0.0304 0.7585 11.00000 0.05 0.25 Q13 1 0.3927 0.1288 0.0769 11.00000 0.05 0.24 Q14 1 0.2025 0.1471 0.1753 11.00000 0.05 0.24 Q15 1 0.9140 0.0708 0.5582 11.00000 0.05 0.24 Q16 1 0.3231 0.1896 0.1953 11.00000 0.05 0.24 Q17 1 0.4381 0.1539 0.0434 11.00000 0.05 0.24 Q18 1 0.3701 0.2469 0.0586 11.00000 0.05 0.23 Q19 1 0.7641 0.0279 0.7193 11.00000 0.05 0.23 Q20 1 0.8896 0.1328 0.5583 11.00000 0.05 0.23 ; _shelx_res_checksum 75086 _shelx_hkl_file ; -1 0 0 4.49 0.45 1 0 0 4.27 0.47 1 0 0 4.82 0.47 -2 0 0 173.53 6.67 -2 0 0 162.01 6.66 2 0 0 175.15 6.65 2 0 0 168.31 6.68 -3 0 0 948.49 37.37 -3 0 0 986.98 37.39 3 0 0 1048.57 37.44 3 0 0 1000.41 37.35 -4 0 0 50.48 3.07 -4 0 0 56.72 3.02 4 0 0 58.44 3.21 4 0 0 60.60 3.16 -5 0 0 5.06 1.33 -5 0 0 4.49 1.43 5 0 0 4.94 1.49 5 0 0 4.43 1.36 -6 0 0 9.84 1.75 -6 0 0 9.66 1.87 6 0 0 16.01 2.08 6 0 0 12.93 2.01 -7 0 0 254.29 11.10 7 0 0 263.74 11.08 7 0 0 256.73 11.11 -8 0 0 79.87 5.55 8 0 0 86.75 5.54 8 0 0 86.45 5.32 -9 0 0 1.43 2.54 9 0 0 -0.40 2.25 -10 0 0 48.59 4.95 10 0 0 56.35 4.93 -11 0 0 10.53 3.95 -11 1 0 1.20 3.68 10 -1 0 12.21 3.12 -10 1 0 22.37 4.06 9 -1 0 1.66 2.33 -9 1 0 3.08 2.80 8 -1 0 -0.49 2.25 8 -1 0 3.23 2.14 -8 1 0 1.87 2.47 7 -1 0 342.02 14.94 7 -1 0 381.84 15.28 -7 1 0 375.90 15.22 6 -1 0 6.40 1.68 6 -1 0 7.41 1.84 -6 1 0 4.39 1.78 5 -1 0 -1.09 1.18 -5 1 0 0.97 1.22 -5 1 0 1.24 1.35 4 -1 0 217.32 8.92 4 -1 0 222.56 9.05 -4 1 0 222.96 9.03 -4 1 0 216.05 8.97 3 -1 0 1072.12 40.32 3 -1 0 1082.61 40.28 3 -1 0 1098.64 40.22 -3 1 0 1054.97 40.28 -3 1 0 1051.75 40.29 2 -1 0 32.81 1.88 2 -1 0 30.74 1.94 -2 1 0 30.57 1.93 -2 1 0 31.99 1.88 -1 1 0 9.09 0.75 0 -1 0 -1.12 0.09 0 -1 0 -1.16 0.19 0 1 0 -0.87 0.20 0 1 0 -1.03 0.09 -2 -1 0 128.58 5.42 -2 -1 0 136.79 5.36 2 1 0 137.44 5.38 2 1 0 133.75 5.45 2 1 0 138.74 5.28 -3 -1 0 147.92 6.40 3 1 0 159.28 6.55 3 1 0 168.94 6.37 3 1 0 156.87 6.46 -4 -1 0 34.58 2.29 -4 -1 0 27.72 2.08 4 1 0 26.89 2.06 4 1 0 31.92 2.40 -5 -1 0 43.00 2.62 -5 -1 0 38.09 2.70 5 1 0 39.25 2.74 5 1 0 31.72 2.60 -6 -1 0 259.58 10.63 -6 -1 0 270.38 10.74 6 1 0 254.53 10.71 6 1 0 247.01 10.77 -7 -1 0 12.62 1.98 -7 -1 0 10.10 2.06 7 1 0 10.04 2.22 7 1 0 13.16 2.12 -8 -1 0 34.25 3.41 8 1 0 28.79 3.20 8 1 0 32.57 3.32 -9 -1 0 18.73 3.28 9 1 0 24.52 3.28 -10 -1 0 14.60 3.52 10 1 0 15.56 3.37 -11 -1 0 13.05 3.86 -10 2 0 190.64 10.54 9 -2 0 26.26 3.36 -9 2 0 22.92 3.84 8 -2 0 11.12 3.01 8 -2 0 8.44 2.32 -8 2 0 15.68 3.04 7 -2 0 150.96 7.80 7 -2 0 152.74 7.34 -7 2 0 159.08 7.79 6 -2 0 23.53 2.42 -6 2 0 25.24 2.73 5 -2 0 0.86 1.35 5 -2 0 0.84 1.52 -5 2 0 1.10 1.58 4 -2 0 46.76 3.08 4 -2 0 39.12 2.65 -4 2 0 41.13 2.80 -4 2 0 40.94 2.87 3 -2 0 338.38 13.42 3 -2 0 346.26 13.50 -3 2 0 325.58 13.43 -3 2 0 361.20 13.50 2 -2 0 3.73 1.24 2 -2 0 3.71 1.07 -2 2 0 1.97 1.16 -2 2 0 2.62 1.07 1 -2 0 18.46 1.29 1 -2 0 15.60 1.24 -1 2 0 15.55 1.22 -1 2 0 14.06 1.19 0 -2 0 773.37 27.46 0 2 0 693.20 27.42 -1 -2 0 244.68 9.61 1 2 0 253.50 9.66 1 2 0 234.51 9.60 1 2 0 283.76 9.59 -2 -2 0 126.07 4.85 -2 -2 0 118.49 4.97 2 2 0 119.81 4.99 -3 -2 0 797.67 31.80 -3 -2 0 851.53 31.79 3 2 0 893.98 31.72 3 2 0 816.56 31.83 3 2 0 878.11 31.99 -4 -2 0 7.24 1.19 4 2 0 8.23 1.27 4 2 0 6.35 1.03 4 2 0 7.24 1.43 -5 -2 0 84.94 4.12 -5 -2 0 81.90 4.05 5 2 0 87.63 4.39 5 2 0 89.97 4.25 -6 -2 0 506.14 19.43 -6 -2 0 474.90 19.41 6 2 0 491.03 19.47 6 2 0 525.06 19.72 -7 -2 0 0.45 1.31 -7 -2 0 1.10 1.64 7 2 0 0.38 1.67 7 2 0 1.48 1.63 -8 -2 0 81.57 5.20 8 2 0 81.89 5.14 8 2 0 77.42 5.08 -9 -2 0 23.97 3.40 9 2 0 24.76 3.40 -10 -2 0 52.19 4.74 10 2 0 40.08 4.40 -11 -2 0 27.08 4.11 10 -3 0 15.09 3.27 -10 3 0 19.04 4.31 9 -3 0 51.63 4.23 -9 3 0 45.89 4.77 8 -3 0 6.98 2.82 8 -3 0 5.53 2.31 -8 3 0 9.62 2.98 7 -3 0 244.35 10.54 -7 3 0 241.83 11.09 6 -3 0 70.57 4.62 6 -3 0 72.25 4.17 -6 3 0 67.59 4.59 5 -3 0 1.60 1.39 5 -3 0 0.84 1.56 -5 3 0 0.26 1.58 4 -3 0 906.89 35.73 -4 3 0 967.05 35.72 3 -3 0 3.58 1.42 -3 3 0 2.91 1.30 -3 3 0 3.11 1.27 2 -3 0 15.38 1.71 2 -3 0 11.74 1.39 -2 3 0 12.14 1.51 -2 3 0 11.39 1.48 1 -3 0 1932.11 69.87 1 -3 0 1865.99 69.85 -1 3 0 1883.51 69.86 -1 3 0 1811.69 69.83 0 -3 0 -0.64 0.64 0 -3 0 0.70 0.76 0 3 0 0.02 0.63 0 3 0 -0.56 0.67 -1 -3 0 46.70 2.15 -1 -3 0 43.70 2.17 -1 -3 0 42.68 2.07 1 3 0 49.27 2.09 1 3 0 48.09 2.16 -2 -3 0 17.85 1.35 -2 -3 0 20.84 1.55 2 3 0 24.33 1.61 -3 -3 0 179.92 7.44 -3 -3 0 184.37 7.26 3 3 0 179.63 7.43 -4 -3 0 200.44 8.23 -4 -3 0 195.84 8.19 4 3 0 216.48 8.24 4 3 0 205.40 8.46 -5 -3 0 49.12 2.87 5 3 0 44.74 2.86 5 3 0 52.58 3.16 -6 -3 0 70.85 3.85 -6 -3 0 73.97 3.75 6 3 0 65.86 3.84 6 3 0 68.30 4.14 -7 -3 0 140.78 6.47 -7 -3 0 130.54 6.15 7 3 0 128.10 6.34 7 3 0 137.07 6.63 -8 -3 0 22.97 2.86 8 3 0 20.90 2.96 -9 -3 0 10.34 2.73 9 3 0 17.74 3.12 -10 -3 0 7.76 2.95 10 3 0 7.61 2.94 -11 -3 0 52.66 5.09 -10 4 0 9.50 4.09 9 -4 0 3.86 2.55 -9 4 0 5.36 3.45 8 -4 0 -0.40 2.12 -8 4 0 2.25 2.78 7 -4 0 121.09 6.23 -7 4 0 119.26 7.07 6 -4 0 207.63 9.66 6 -4 0 215.36 9.08 -6 4 0 212.69 9.72 5 -4 0 41.33 3.26 5 -4 0 37.60 2.83 -5 4 0 37.70 3.24 4 -4 0 636.71 24.55 -4 4 0 623.75 24.47 3 -4 0 352.87 13.87 -3 4 0 340.18 13.80 2 -4 0 28.98 2.28 2 -4 0 29.94 2.23 -2 4 0 25.46 2.09 -2 4 0 27.84 2.16 1 -4 0 74.55 3.54 1 -4 0 71.74 3.58 -1 4 0 72.78 3.52 -1 4 0 70.68 3.56 0 -4 0 988.65 36.93 0 -4 0 941.79 36.92 0 4 0 1025.75 36.95 0 4 0 977.91 36.90 -1 -4 0 48.80 2.31 -1 -4 0 43.02 2.22 -1 -4 0 42.00 2.36 1 4 0 45.22 2.23 1 4 0 45.94 2.36 -2 -4 0 158.48 6.30 -2 -4 0 157.99 6.42 2 4 0 155.57 6.34 -3 -4 0 3.32 1.16 3 4 0 5.58 1.20 -4 -4 0 58.99 3.22 -4 -4 0 53.51 2.99 4 4 0 52.39 3.19 -5 -4 0 184.64 7.56 -5 -4 0 183.85 7.51 5 4 0 173.55 7.80 -6 -4 0 38.67 2.92 6 4 0 40.95 3.17 -7 -4 0 24.91 2.27 -7 -4 0 26.04 2.55 7 4 0 32.17 3.10 -8 -4 0 31.73 3.10 8 4 0 28.48 3.27 -9 -4 0 34.53 3.55 9 4 0 32.57 3.78 -10 -4 0 7.61 2.81 10 4 0 11.13 3.11 -11 -4 0 15.24 3.45 -10 5 0 0.42 5.01 -9 5 0 17.54 3.93 8 -5 0 6.71 2.35 -8 5 0 13.01 3.64 7 -5 0 18.92 2.64 7 -5 0 16.94 3.10 -7 5 0 17.88 3.52 6 -5 0 60.24 3.93 6 -5 0 61.78 4.84 -6 5 0 62.92 4.78 5 -5 0 3.33 1.38 5 -5 0 -0.56 1.80 -5 5 0 -0.71 1.75 4 -5 0 445.05 18.01 -4 5 0 454.50 17.98 3 -5 0 114.76 5.58 -3 5 0 113.42 5.54 2 -5 0 12.63 1.75 -2 5 0 7.20 1.51 1 -5 0 185.38 7.96 1 -5 0 201.54 7.97 -1 5 0 190.02 7.95 0 -5 0 -1.84 1.00 0 -5 0 -0.57 0.95 0 5 0 -1.44 0.97 0 5 0 -0.74 0.99 -1 -5 0 93.81 4.13 -1 -5 0 90.80 4.02 -1 -5 0 96.96 4.27 1 5 0 97.19 4.09 1 5 0 93.17 4.20 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-3 -19 123.87 7.64 -4 -3 -19 61.94 5.13 -5 -3 -19 7.37 2.80 -6 -3 -19 65.73 5.17 -7 -3 -19 -1.51 2.37 -8 -3 -19 59.94 5.03 -9 -3 -19 -0.97 2.72 2 -4 -19 12.60 4.56 1 -4 -19 52.31 6.01 0 -4 -19 1.28 3.44 -1 -4 -19 19.60 3.96 -2 -4 -19 3.05 3.20 -3 -4 -19 16.34 3.53 -4 -4 -19 97.84 6.58 -5 -4 -19 6.72 2.84 -6 -4 -19 30.96 3.71 -7 -4 -19 67.95 5.46 -8 -4 -19 0.66 2.66 -9 -4 -19 -0.24 2.55 1 -5 -19 5.42 3.94 0 -5 -19 7.81 3.95 -1 -5 -19 65.75 6.02 -2 -5 -19 3.40 3.10 -3 -5 -19 22.99 3.86 -4 -5 -19 124.19 7.51 -5 -5 -19 20.01 3.30 -6 -5 -19 54.92 4.66 -7 -5 -19 1.89 2.26 -8 -5 -19 16.53 3.06 -9 -5 -19 13.78 3.03 1 -6 -19 11.32 4.55 0 -6 -19 9.78 3.96 -1 -6 -19 32.34 4.74 -2 -6 -19 5.07 3.38 -3 -6 -19 2.69 2.84 -4 -6 -19 142.64 8.23 -5 -6 -19 57.01 4.76 -6 -6 -19 4.12 2.62 -7 -6 -19 222.29 10.32 0 -7 -19 8.98 4.08 -1 -7 -19 0.51 3.49 -2 -7 -19 -1.51 3.04 -3 -7 -19 30.26 4.23 -4 -7 -19 110.21 7.30 -5 -7 -19 0.69 2.59 -6 -7 -19 24.13 3.33 -7 -7 -19 3.04 2.41 -1 -8 -19 3.71 3.66 -2 -8 -19 2.72 3.45 -3 -8 -19 2.57 3.16 -4 -8 -19 -2.55 2.65 -5 -8 -19 16.41 3.31 -6 -8 -19 13.89 2.93 -2 -9 -19 16.05 4.07 -3 -9 -19 35.23 4.65 -4 -9 -19 -2.27 2.78 -5 -9 -19 10.51 3.07 -6 -9 -19 6.20 2.80 -3 -10 -19 5.26 3.51 -4 -10 -19 -0.75 2.93 -5 -10 -19 -2.26 2.71 -6 -10 -19 63.71 4.93 -1 7 -20 6.88 3.98 1 -7 20 16.93 4.63 -2 7 -20 -1.28 3.79 2 -7 20 11.79 4.24 -1 -6 20 130.16 9.40 0 6 -20 0.77 3.69 0 -6 20 -2.18 3.38 -1 6 -20 14.29 4.26 1 -6 20 10.78 4.20 -2 6 -20 -0.40 3.43 2 -6 20 0.89 3.93 -3 6 -20 1.74 3.97 -4 6 -20 8.03 5.40 1 5 -20 3.66 3.88 -1 -5 20 5.85 3.94 0 5 -20 9.63 4.18 0 -5 20 8.14 3.83 -1 5 -20 4.67 3.88 1 -5 20 3.68 3.67 -2 5 -20 18.64 4.37 2 -5 20 25.58 5.44 -3 5 -20 23.52 4.53 -4 5 -20 7.22 3.94 2 4 -20 18.53 4.94 -2 -4 20 17.90 4.50 1 4 -20 131.91 9.37 -1 -4 20 135.45 9.27 0 4 -20 1.84 3.72 0 -4 20 2.05 3.39 -1 4 -20 54.50 6.07 1 -4 20 41.81 5.11 -2 4 -20 59.44 5.89 2 -4 20 38.13 8.14 -3 4 -20 1.27 3.34 -4 4 -20 1.62 3.47 -5 4 -20 2.44 3.78 2 3 -20 -2.68 3.57 -2 -3 20 2.51 3.60 1 3 -20 14.99 4.32 -1 -3 20 10.20 3.84 0 3 -20 -1.71 3.45 0 -3 20 0.87 3.39 -1 3 -20 2.77 3.61 1 -3 20 0.13 3.24 -2 3 -20 98.94 7.76 -3 3 -20 2.72 3.30 -4 3 -20 10.34 3.57 -5 3 -20 50.28 5.54 -6 3 -20 43.48 5.32 2 2 -20 7.40 4.33 -2 -2 20 6.12 3.90 1 2 -20 140.70 9.46 -1 -2 20 146.25 9.45 0 2 -20 18.86 4.45 0 -2 20 15.34 3.97 -1 2 -20 0.57 3.44 1 -2 20 -3.78 3.16 -2 2 -20 128.87 8.63 -3 2 -20 5.18 3.36 -4 2 -20 -1.15 2.95 -5 2 -20 10.58 3.38 -6 2 -20 5.57 3.51 -7 2 -20 12.77 4.20 2 1 -20 9.80 4.21 -2 -1 20 9.85 4.00 1 1 -20 0.42 3.46 -1 -1 20 6.06 3.49 0 1 -20 50.25 5.61 0 -1 20 34.97 4.66 -1 1 -20 -0.20 3.23 -2 1 -20 110.54 7.88 -3 1 -20 52.41 5.57 -4 1 -20 3.93 2.87 -5 1 -20 164.02 9.22 -6 1 -20 4.56 3.22 -7 1 -20 23.54 4.10 2 0 -20 4.15 3.90 -2 0 20 13.61 4.47 1 0 -20 31.51 5.02 -1 0 20 33.00 4.89 0 0 -20 31.69 5.21 -1 0 -20 3.66 3.28 -2 0 -20 96.29 7.28 -3 0 -20 0.53 3.10 -4 0 -20 0.59 2.76 -5 0 -20 11.81 3.23 -6 0 -20 35.63 4.35 -7 0 -20 23.49 4.08 -8 0 -20 1.65 3.20 2 -1 -20 26.46 5.10 -2 1 20 20.95 7.41 1 -1 -20 -1.15 3.61 0 -1 -20 47.92 5.59 -1 -1 -20 -2.55 2.97 -2 -1 -20 29.63 4.27 -3 -1 -20 119.97 7.83 -4 -1 -20 4.36 3.20 -5 -1 -20 102.08 6.98 -6 -1 -20 39.44 4.51 -7 -1 -20 3.62 2.90 -8 -1 -20 31.80 4.20 2 -2 -20 22.21 4.80 1 -2 -20 39.29 5.58 0 -2 -20 18.78 4.31 -1 -2 -20 66.48 6.13 -2 -2 -20 4.60 3.15 -3 -2 -20 18.74 3.50 -4 -2 -20 -1.30 2.80 -5 -2 -20 15.32 3.30 -6 -2 -20 74.05 5.89 -7 -2 -20 4.75 2.88 -8 -2 -20 9.49 3.27 1 -3 -20 2.43 3.80 0 -3 -20 -2.43 3.32 -1 -3 -20 -0.04 3.37 -2 -3 -20 12.98 3.53 -3 -3 -20 65.97 5.56 -4 -3 -20 -1.26 2.69 -5 -3 -20 22.00 3.65 -6 -3 -20 94.44 6.50 -7 -3 -20 3.96 2.75 -8 -3 -20 36.81 4.29 1 -4 -20 132.61 9.70 0 -4 -20 7.36 3.85 -1 -4 -20 37.11 4.91 -2 -4 -20 11.59 3.55 -3 -4 -20 37.26 4.53 -4 -4 -20 2.07 2.78 -5 -4 -20 4.31 2.83 -6 -4 -20 108.68 6.93 -7 -4 -20 34.65 4.04 -8 -4 -20 -0.35 2.77 0 -5 -20 12.32 4.10 -1 -5 -20 14.64 4.00 -2 -5 -20 17.45 3.93 -3 -5 -20 6.55 3.19 -4 -5 -20 0.70 2.75 -5 -5 -20 30.19 3.89 -6 -5 -20 82.00 6.14 -7 -5 -20 -0.40 2.33 -8 -5 -20 15.79 3.26 -1 -6 -20 -2.15 3.44 -2 -6 -20 58.61 5.65 -3 -6 -20 1.62 3.15 -4 -6 -20 2.31 2.92 -5 -6 -20 4.81 2.90 -6 -6 -20 1.38 2.75 -7 -6 -20 14.91 3.08 -8 -6 -20 5.11 2.60 -1 -7 -20 23.33 5.71 -2 -7 -20 69.63 6.37 -3 -7 -20 17.59 3.86 -4 -7 -20 12.39 3.50 -5 -7 -20 38.61 4.18 -6 -7 -20 3.04 2.72 -7 -7 -20 4.07 2.65 -2 -8 -20 40.03 8.09 -3 -8 -20 -0.46 3.32 -4 -8 -20 5.24 3.13 -5 -8 -20 3.75 3.04 -6 -8 -20 -0.92 2.58 -4 -9 -20 17.81 3.69 -5 -9 -20 39.73 4.55 -1 5 -21 9.47 4.17 1 -5 21 14.79 6.36 -2 5 -21 2.44 3.79 0 4 -21 0.56 3.80 0 -4 21 0.87 3.62 -1 4 -21 120.56 8.96 -2 4 -21 11.83 4.14 -3 4 -21 0.31 3.45 -4 4 -21 61.10 7.68 -1 -3 21 -4.45 3.57 0 3 -21 12.45 4.35 0 -3 21 11.13 4.30 -1 3 -21 0.03 3.52 -2 3 -21 42.38 5.40 -3 3 -21 -1.66 3.24 -4 3 -21 59.85 6.10 1 2 -21 12.01 4.42 -1 -2 21 6.21 3.68 0 2 -21 4.65 3.91 -1 2 -21 33.20 5.16 -2 2 -21 22.57 4.38 -3 2 -21 -0.26 3.28 -4 2 -21 57.94 5.78 -5 2 -21 5.04 3.26 1 1 -21 11.80 4.29 0 1 -21 33.48 4.96 -1 1 -21 -1.23 3.42 -2 1 -21 38.19 5.12 -3 1 -21 2.26 3.22 -4 1 -21 21.52 4.09 -5 1 -21 92.89 7.11 -6 1 -21 2.81 3.25 1 0 -21 4.35 3.96 0 0 -21 42.45 5.56 -1 0 -21 30.77 4.72 -2 0 -21 28.44 4.68 -3 0 -21 54.40 5.62 -4 0 -21 2.03 3.08 -5 0 -21 9.46 3.35 -6 0 -21 0.03 2.89 -7 0 -21 21.74 5.56 1 -1 -21 4.01 3.98 0 -1 -21 26.97 4.82 -1 -1 -21 6.09 3.53 -2 -1 -21 2.55 3.20 -3 -1 -21 3.00 3.14 -4 -1 -21 10.77 3.43 -5 -1 -21 56.83 5.33 -6 -1 -21 3.18 3.02 -7 -1 -21 13.56 3.51 0 -2 -21 6.46 3.96 -1 -2 -21 155.99 9.69 -2 -2 -21 4.95 3.29 -3 -2 -21 30.61 4.49 -4 -2 -21 13.78 3.70 -5 -2 -21 24.55 3.86 -6 -2 -21 4.27 2.87 -7 -2 -21 -0.64 2.77 0 -3 -21 7.32 4.02 -1 -3 -21 16.40 4.11 -2 -3 -21 11.64 3.66 -3 -3 -21 9.69 3.60 -4 -3 -21 28.01 4.41 -5 -3 -21 3.32 3.07 -6 -3 -21 -1.10 2.56 -7 -3 -21 11.88 3.29 -1 -4 -21 123.94 8.72 -2 -4 -21 2.14 3.18 -3 -4 -21 1.03 2.99 -4 -4 -21 58.43 5.37 -5 -4 -21 7.73 3.20 -6 -4 -21 2.33 2.81 -7 -4 -21 0.13 2.74 -2 -5 -21 65.75 6.15 -3 -5 -21 22.87 4.06 -4 -5 -21 69.34 5.72 -5 -5 -21 19.73 3.67 -6 -5 -21 8.64 3.22 -7 -5 -21 37.75 4.12 -2 -6 -21 5.54 4.26 -3 -6 -21 12.02 3.80 -4 -6 -21 62.93 5.69 -5 -6 -21 4.73 2.98 -6 -6 -21 3.23 2.94 -3 -7 -21 4.54 4.09 -4 -7 -21 6.85 3.48 -5 -7 -21 56.28 5.12 -6 -7 -21 17.09 3.55 -2 2 -22 31.25 7.56 -2 1 -22 27.73 5.03 -3 1 -22 0.39 3.56 -4 1 -22 3.57 4.71 -2 0 -22 1.91 3.64 -3 0 -22 131.27 8.74 -4 0 -22 0.87 3.25 -2 -1 -22 11.13 4.18 -3 -1 -22 8.18 3.68 -4 -1 -22 5.74 3.36 -5 -1 -22 10.18 3.62 -2 -2 -22 9.06 4.06 -3 -2 -22 124.29 8.33 -4 -2 -22 -0.14 3.11 -5 -2 -22 -0.11 2.99 -3 -3 -22 0.69 3.16 -4 -3 -22 54.60 5.49 -5 -3 -22 18.45 3.81 -6 -3 -22 53.80 6.58 -4 -4 -22 7.26 3.49 -5 -4 -22 10.85 3.53 -5 -5 -22 -2.95 3.89 _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6496 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71109 9.602 13.371 17.492 86.004 74.125 74.649 ) _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 72510 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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 Ni1 Ni 0.80834(3) 0.04854(2) 0.69006(2) 0.02728(11) Uani 1 1 d . . . . . N1 N 0.8961(2) 0.07817(6) 0.59606(15) 0.0248(4) Uani 1 1 d . . . . . N2 N 0.9427(2) 0.14476(6) 0.54869(15) 0.0267(5) Uani 1 1 d . . . . . N3 N 0.7751(2) 0.10241(6) 0.73507(15) 0.0250(4) Uani 1 1 d . . . . . N4 N 0.8033(2) 0.17102(6) 0.69542(15) 0.0281(5) Uani 1 1 d . . . . . C1 C 0.9623(3) 0.06467(8) 0.52524(19) 0.0316(6) Uani 1 1 d . . . . . H1 H 0.9705 0.0368 0.5172 0.038 Uiso 1 1 calc R U . . . C2 C 1.0183(3) 0.08955(8) 0.4645(2) 0.0341(6) Uani 1 1 d . . . . . H2 H 1.0648 0.0795 0.4151 0.041 Uiso 1 1 calc R U . . . C3 C 1.0044(3) 0.12990(8) 0.47793(19) 0.0319(6) Uani 1 1 d . . . . . H3 H 1.0400 0.1477 0.4353 0.038 Uiso 1 1 calc R U . . . C4 C 0.8916(2) 0.11831(7) 0.60424(17) 0.0215(5) Uani 1 1 d . . . . . C5 C 0.8200(2) 0.13228(7) 0.68326(17) 0.0216(5) Uani 1 1 d . . . . . C6 C 0.7332(3) 0.18104(8) 0.7663(2) 0.0330(6) Uani 1 1 d . . . . . H6 H 0.7195 0.2084 0.7781 0.040 Uiso 1 1 calc R U . . . C7 C 0.6800(3) 0.15340(8) 0.8226(2) 0.0340(6) Uani 1 1 d . . . . . H7 H 0.6292 0.1612 0.8717 0.041 Uiso 1 1 calc R U . . . C8 C 0.7033(3) 0.11407(8) 0.80518(19) 0.0302(6) Uani 1 1 d . . . . . H8 H 0.6681 0.0944 0.8434 0.036 Uiso 1 1 calc R U . . . C9 C 0.7298(4) 0.02100(8) 0.7897(2) 0.0463(8) Uani 1 1 d . . . . . H9A H 0.6259 0.0169 0.7603 0.069 Uiso 1 1 calc R U . . . H9B H 0.7456 0.0369 0.8533 0.069 Uiso 1 1 calc R U . . . H9C H 0.7780 -0.0048 0.8062 0.069 Uiso 1 1 calc R U . . . C10 C 0.8318(3) -0.00268(7) 0.6314(2) 0.0367(6) Uani 1 1 d . . . . . H10A H 0.9346 -0.0096 0.6492 0.055 Uiso 1 1 calc R U . . . H10B H 0.7940 -0.0016 0.5556 0.055 Uiso 1 1 calc R U . . . H10C H 0.7788 -0.0228 0.6598 0.055 Uiso 1 1 calc R U . . . Ni2 Ni 0.30046(3) 0.16002(2) 0.20069(2) 0.02406(10) Uani 1 1 d . . . . . N5 N 0.3800(2) 0.11973(6) 0.12538(15) 0.0233(4) Uani 1 1 d . . . . . N6 N 0.4913(2) 0.11265(6) -0.01531(15) 0.0271(5) Uani 1 1 d . . . . . N7 N 0.3816(2) 0.19578(5) 0.11469(15) 0.0235(4) Uani 1 1 d . . . . . N8 N 0.5091(2) 0.19531(6) -0.01795(15) 0.0275(5) Uani 1 1 d . . . . . C11 C 0.3790(3) 0.07957(7) 0.13321(19) 0.0285(6) Uani 1 1 d . . . . . H11 H 0.3385 0.0678 0.1839 0.034 Uiso 1 1 calc R U . . . C12 C 0.4343(3) 0.05546(7) 0.0707(2) 0.0345(6) Uani 1 1 d . . . . . H12 H 0.4364 0.0274 0.0792 0.041 Uiso 1 1 calc R U . . . C13 C 0.4870(3) 0.07302(8) -0.0050(2) 0.0352(6) Uani 1 1 d . . . . . H13 H 0.5213 0.0566 -0.0514 0.042 Uiso 1 1 calc R U . . . C14 C 0.4398(2) 0.13369(7) 0.05048(17) 0.0228(5) Uani 1 1 d . . . . . C15 C 0.4447(2) 0.17782(7) 0.04724(17) 0.0220(5) Uani 1 1 d . . . . . C16 C 0.5122(3) 0.23508(7) -0.0146(2) 0.0319(6) Uani 1 1 d . . . . . H16 H 0.5571 0.2489 -0.0599 0.038 Uiso 1 1 calc R U . . . C17 C 0.4532(3) 0.25675(8) 0.05157(19) 0.0329(6) Uani 1 1 d . . . . . H17 H 0.4575 0.2849 0.0532 0.039 Uiso 1 1 calc R U . . . C18 C 0.3879(3) 0.23587(7) 0.11523(19) 0.0281(6) Uani 1 1 d . . . . . H18 H 0.3456 0.2501 0.1613 0.034 Uiso 1 1 calc R U . . . C19 C 0.2123(3) 0.20206(8) 0.2618(2) 0.0385(7) Uani 1 1 d . . . . . H19A H 0.1516 0.1904 0.3029 0.058 Uiso 1 1 calc R U . . . H19B H 0.1527 0.2186 0.2064 0.058 Uiso 1 1 calc R U . . . H19C H 0.2880 0.2184 0.3069 0.058 Uiso 1 1 calc R U . . . C20 C 0.2293(3) 0.12375(8) 0.2876(2) 0.0397(7) Uani 1 1 d . . . . . H20A H 0.2872 0.0994 0.2975 0.060 Uiso 1 1 calc R U . . . H20B H 0.1281 0.1173 0.2543 0.060 Uiso 1 1 calc R U . . . H20C H 0.2364 0.1362 0.3554 0.060 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 Ni1 0.0385(2) 0.01894(17) 0.02866(18) 0.00014(13) 0.01640(15) -0.00454(14) N1 0.0327(11) 0.0182(10) 0.0266(10) -0.0022(8) 0.0133(9) 0.0009(9) N2 0.0352(11) 0.0222(11) 0.0277(11) 0.0000(9) 0.0170(9) -0.0027(9) N3 0.0303(11) 0.0220(10) 0.0246(10) 0.0011(8) 0.0107(9) -0.0025(9) N4 0.0349(12) 0.0221(11) 0.0318(11) -0.0012(9) 0.0165(10) 0.0008(9) C1 0.0444(15) 0.0207(13) 0.0355(14) -0.0029(11) 0.0210(12) -0.0005(11) C2 0.0454(16) 0.0315(15) 0.0338(14) -0.0020(11) 0.0251(13) 0.0018(12) C3 0.0423(15) 0.0291(14) 0.0324(14) 0.0031(11) 0.0243(13) -0.0030(12) C4 0.0242(12) 0.0211(12) 0.0205(11) 0.0005(9) 0.0084(10) -0.0009(10) C5 0.0236(12) 0.0226(12) 0.0206(11) -0.0010(9) 0.0096(10) 0.0006(10) C6 0.0421(15) 0.0246(13) 0.0374(14) -0.0016(12) 0.0197(12) 0.0050(12) C7 0.0377(15) 0.0368(16) 0.0330(14) -0.0021(11) 0.0193(12) 0.0032(12) C8 0.0389(14) 0.0284(14) 0.0299(14) 0.0032(11) 0.0209(12) -0.0035(11) C9 0.072(2) 0.0286(15) 0.0489(17) 0.0015(13) 0.0346(16) -0.0125(15) C10 0.0531(17) 0.0206(13) 0.0406(15) -0.0013(11) 0.0201(13) -0.0043(12) Ni2 0.02512(17) 0.02592(18) 0.02407(17) -0.00013(13) 0.01168(13) -0.00020(13) N5 0.0246(10) 0.0222(10) 0.0245(10) 0.0009(8) 0.0090(9) -0.0028(8) N6 0.0362(12) 0.0203(11) 0.0289(11) -0.0037(8) 0.0160(10) -0.0016(9) N7 0.0257(10) 0.0212(10) 0.0251(10) -0.0017(8) 0.0093(9) 0.0040(8) N8 0.0371(12) 0.0210(11) 0.0282(11) 0.0026(8) 0.0153(10) -0.0043(9) C11 0.0337(13) 0.0221(13) 0.0316(13) 0.0034(11) 0.0116(11) -0.0059(11) C12 0.0456(16) 0.0176(13) 0.0430(15) 0.0001(11) 0.0167(13) -0.0030(12) C13 0.0464(16) 0.0252(14) 0.0385(15) -0.0067(11) 0.0190(13) -0.0009(12) C14 0.0238(12) 0.0212(12) 0.0234(12) 0.0011(10) 0.0065(10) -0.0030(10) C15 0.0239(12) 0.0207(12) 0.0215(12) 0.0007(10) 0.0062(10) -0.0005(10) C16 0.0381(14) 0.0257(14) 0.0340(14) 0.0070(11) 0.0134(12) -0.0029(11) C17 0.0383(15) 0.0230(14) 0.0381(15) 0.0029(11) 0.0117(12) 0.0030(12) C18 0.0315(13) 0.0217(13) 0.0323(13) -0.0020(10) 0.0108(11) 0.0038(11) C19 0.0413(16) 0.0396(16) 0.0422(16) 0.0008(13) 0.0246(13) 0.0050(13) C20 0.0467(16) 0.0392(16) 0.0433(16) 0.0052(13) 0.0298(14) -0.0005(13) 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' 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 C9 Ni1 C10 87.56(12) . . C9 Ni1 N1 176.49(11) . . C10 Ni1 N1 94.63(10) . . C9 Ni1 N3 96.31(11) . . C10 Ni1 N3 174.13(10) . . N1 Ni1 N3 81.73(8) . . C1 N1 C4 115.0(2) . . C1 N1 Ni1 129.63(16) . . C4 N1 Ni1 115.34(15) . . C4 N2 C3 116.0(2) . . C5 N3 C8 115.1(2) . . C5 N3 Ni1 115.59(15) . . C8 N3 Ni1 129.10(17) . . C5 N4 C6 115.6(2) . . N1 C1 C2 122.6(2) . . N1 C1 H1 118.7 . . C2 C1 H1 118.7 . . C1 C2 C3 117.3(2) . . C1 C2 H2 121.3 . . C3 C2 H2 121.3 . . N2 C3 C2 122.4(2) . . N2 C3 H3 118.8 . . C2 C3 H3 118.8 . . N2 C4 N1 126.7(2) . . N2 C4 C5 119.5(2) . . N1 C4 C5 113.9(2) . . N4 C5 N3 127.1(2) . . N4 C5 C4 119.5(2) . . N3 C5 C4 113.4(2) . . N4 C6 C7 122.8(2) . . N4 C6 H6 118.6 . . C7 C6 H6 118.6 . . C8 C7 C6 117.4(2) . . C8 C7 H7 121.3 . . C6 C7 H7 121.3 . . N3 C8 C7 122.0(2) . . N3 C8 H8 119.0 . . C7 C8 H8 119.0 . . Ni1 C9 H9A 109.5 . . Ni1 C9 H9B 109.5 . . H9A C9 H9B 109.5 . . Ni1 C9 H9C 109.5 . . H9A C9 H9C 109.5 . . H9B C9 H9C 109.5 . . Ni1 C10 H10A 109.5 . . Ni1 C10 H10B 109.5 . . H10A C10 H10B 109.5 . . Ni1 C10 H10C 109.5 . . H10A C10 H10C 109.5 . . H10B C10 H10C 109.5 . . C20 Ni2 C19 87.00(12) . . C20 Ni2 N5 96.68(10) . . C19 Ni2 N5 174.29(10) . . C20 Ni2 N7 177.36(10) . . C19 Ni2 N7 94.66(10) . . N5 Ni2 N7 81.82(8) . . C11 N5 C14 114.4(2) . . C11 N5 Ni2 129.80(16) . . C14 N5 Ni2 115.69(15) . . C14 N6 C13 116.0(2) . . C18 N7 C15 115.1(2) . . C18 N7 Ni2 129.40(16) . . C15 N7 Ni2 115.48(15) . . C15 N8 C16 115.5(2) . . N5 C11 C12 122.3(2) . . N5 C11 H11 118.9 . . C12 C11 H11 118.9 . . C11 C12 C13 117.9(2) . . C11 C12 H12 121.0 . . C13 C12 H12 121.0 . . N6 C13 C12 122.0(2) . . N6 C13 H13 119.0 . . C12 C13 H13 119.0 . . N6 C14 N5 127.3(2) . . N6 C14 C15 119.8(2) . . N5 C14 C15 112.91(19) . . N8 C15 N7 127.1(2) . . N8 C15 C14 119.0(2) . . N7 C15 C14 113.87(19) . . N8 C16 C17 122.8(2) . . N8 C16 H16 118.6 . . C17 C16 H16 118.6 . . C18 C17 C16 117.1(2) . . C18 C17 H17 121.4 . . C16 C17 H17 121.4 . . N7 C18 C17 122.3(2) . . N7 C18 H18 118.8 . . C17 C18 H18 118.8 . . Ni2 C19 H19A 109.5 . . Ni2 C19 H19B 109.5 . . H19A C19 H19B 109.5 . . Ni2 C19 H19C 109.5 . . H19A C19 H19C 109.5 . . H19B C19 H19C 109.5 . . Ni2 C20 H20A 109.5 . . Ni2 C20 H20B 109.5 . . H20A C20 H20B 109.5 . . Ni2 C20 H20C 109.5 . . H20A C20 H20C 109.5 . . H20B C20 H20C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ni1 C9 1.927(3) . Ni1 C10 1.930(3) . Ni1 N1 1.956(2) . Ni1 N3 1.963(2) . N1 C1 1.347(3) . N1 C4 1.358(3) . N2 C4 1.331(3) . N2 C3 1.335(3) . N3 C5 1.352(3) . N3 C8 1.356(3) . N4 C5 1.329(3) . N4 C6 1.338(3) . C1 C2 1.368(4) . C1 H1 0.9500 . C2 C3 1.381(4) . C2 H2 0.9500 . C3 H3 0.9500 . C4 C5 1.477(3) . C6 C7 1.375(4) . C6 H6 0.9500 . C7 C8 1.372(4) . C7 H7 0.9500 . C8 H8 0.9500 . C9 H9A 0.9800 . C9 H9B 0.9800 . C9 H9C 0.9800 . C10 H10A 0.9800 . C10 H10B 0.9800 . C10 H10C 0.9800 . Ni2 C20 1.927(3) . Ni2 C19 1.934(3) . Ni2 N5 1.9571(19) . Ni2 N7 1.959(2) . N5 C11 1.356(3) . N5 C14 1.359(3) . N6 C14 1.319(3) . N6 C13 1.343(3) . N7 C18 1.351(3) . N7 C15 1.351(3) . N8 C15 1.328(3) . N8 C16 1.340(3) . C11 C12 1.367(4) . C11 H11 0.9500 . C12 C13 1.374(4) . C12 H12 0.9500 . C13 H13 0.9500 . C14 C15 1.487(3) . C16 C17 1.376(3) . C16 H16 0.9500 . C17 C18 1.373(3) . C17 H17 0.9500 . C18 H18 0.9500 . C19 H19A 0.9800 . C19 H19B 0.9800 . C19 H19C 0.9800 . C20 H20A 0.9800 . C20 H20B 0.9800 . C20 H20C 0.9800 . 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 C4 N1 C1 C2 -1.3(4) . . . . Ni1 N1 C1 C2 179.7(2) . . . . N1 C1 C2 C3 -0.2(4) . . . . C4 N2 C3 C2 -1.6(4) . . . . C1 C2 C3 N2 1.7(4) . . . . C3 N2 C4 N1 0.0(4) . . . . C3 N2 C4 C5 -179.2(2) . . . . C1 N1 C4 N2 1.4(4) . . . . Ni1 N1 C4 N2 -179.47(19) . . . . C1 N1 C4 C5 -179.3(2) . . . . Ni1 N1 C4 C5 -0.2(3) . . . . C6 N4 C5 N3 -0.7(3) . . . . C6 N4 C5 C4 177.9(2) . . . . C8 N3 C5 N4 1.3(3) . . . . Ni1 N3 C5 N4 176.36(18) . . . . C8 N3 C5 C4 -177.3(2) . . . . Ni1 N3 C5 C4 -2.3(2) . . . . N2 C4 C5 N4 2.2(3) . . . . N1 C4 C5 N4 -177.1(2) . . . . N2 C4 C5 N3 -179.1(2) . . . . N1 C4 C5 N3 1.6(3) . . . . C5 N4 C6 C7 -0.6(4) . . . . N4 C6 C7 C8 1.1(4) . . . . C5 N3 C8 C7 -0.8(3) . . . . Ni1 N3 C8 C7 -175.00(19) . . . . C6 C7 C8 N3 -0.3(4) . . . . C14 N5 C11 C12 0.1(3) . . . . Ni2 N5 C11 C12 176.90(19) . . . . N5 C11 C12 C13 -2.6(4) . . . . C14 N6 C13 C12 -1.0(4) . . . . C11 C12 C13 N6 3.1(4) . . . . C13 N6 C14 N5 -1.8(4) . . . . C13 N6 C14 C15 177.9(2) . . . . C11 N5 C14 N6 2.3(3) . . . . Ni2 N5 C14 N6 -174.99(19) . . . . C11 N5 C14 C15 -177.51(19) . . . . Ni2 N5 C14 C15 5.2(2) . . . . C16 N8 C15 N7 0.8(3) . . . . C16 N8 C15 C14 -178.5(2) . . . . C18 N7 C15 N8 -0.9(3) . . . . Ni2 N7 C15 N8 -178.90(18) . . . . C18 N7 C15 C14 178.36(19) . . . . Ni2 N7 C15 C14 0.4(2) . . . . N6 C14 C15 N8 -4.1(3) . . . . N5 C14 C15 N8 175.7(2) . . . . N6 C14 C15 N7 176.6(2) . . . . N5 C14 C15 N7 -3.6(3) . . . . C15 N8 C16 C17 0.0(4) . . . . N8 C16 C17 C18 -0.6(4) . . . . C15 N7 C18 C17 0.2(3) . . . . Ni2 N7 C18 C17 177.86(18) . . . . C16 C17 C18 N7 0.5(4) . . . .