#------------------------------------------------------------------------------ #$Date: 2021-07-05 20:41:51 +0300 (Mon, 05 Jul 2021) $ #$Revision: 267185 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/71/7707194.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_7707194 loop_ _publ_author_name 'Muthuramalingam, Sethuraman' 'Velusamy, Marappan' 'Mayilmurugan, Ramasamy' _publ_section_title ; Fixation of atmospheric CO2 as C1-feedstock by nickel(ii) complexes. ; _journal_issue 23 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 7984 _journal_page_last 7994 _journal_paper_doi 10.1039/d0dt03887c _journal_volume 50 _journal_year 2021 _chemical_absolute_configuration ad _chemical_formula_moiety 'C31 H54 N6 Ni2 O7, 2(Cl O4), C3 H6 O, 2(H2 O)' _chemical_formula_sum 'C34 H64 Cl2 N6 Ni2 O18' _chemical_formula_weight 1033.23 _chemical_name_common '(mu2-carbonatato)-diaqua-bis(1-[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]-4-methyl-1,4-diazepane-N,N',N")-di-nickel(II) diperchlorate acetone solvate dihydrate' _chemical_name_systematic '(mu2-carbonatato)-diaqua-bis(1-[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]-4-methyl-1,4-diazepane-N,N',N")-di-nickel(II) diperchlorate acetone solvate dihydrate' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens mixed _audit_creation_method 'manual edited SHELXL-2014/6.cif file' _audit_update_record ; 2021-04-23 deposited with the CCDC. 2021-04-26 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.7462(7) _cell_length_b 15.1861(9) _cell_length_c 25.9560(16) _cell_measurement_reflns_used 3853 _cell_measurement_temperature 290.9(4) _cell_measurement_theta_max 28.570 _cell_measurement_theta_min 3.985 _cell_volume 4630.0(5) _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 290.9(4) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.0640 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _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 -25.00 23.00 0.50 3.40 -- -17.74 -99.00 120.00 96 2 \w -49.00 50.00 0.50 3.40 -- 20.09 -77.00-150.00 198 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_unetI/netI 0.0753 _diffrn_reflns_Laue_measured_fraction_full 0.984 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 13024 _diffrn_reflns_point_group_measured_fraction_full 0.899 _diffrn_reflns_point_group_measured_fraction_max 0.899 _diffrn_reflns_theta_full 27.000 _diffrn_reflns_theta_max 27.000 _diffrn_reflns_theta_min 3.414 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.005 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.62614 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.482 _exptl_crystal_description block _exptl_crystal_F_000 2176 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.613 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.073 _refine_ls_abs_structure_details ; Flack x determined using 2513 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.025(13) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 612 _refine_ls_number_reflns 9085 _refine_ls_number_restraints 90 _refine_ls_restrained_S_all 1.026 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0522 _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^)+(0.0636P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1178 _refine_ls_wR_factor_ref 0.1285 _reflns_Friedel_coverage 0.649 _reflns_Friedel_fraction_full 0.793 _reflns_Friedel_fraction_max 0.793 _reflns_number_gt 7600 _reflns_number_total 9085 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt03887c2.cif _cod_data_source_block MU4a _cod_depositor_comments 'Adding full bibliography for 7707193--7707196.cif.' _cod_database_code 7707194 _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 0.880 _shelx_estimated_absorpt_t_max 0.924 _exptl_absorpt_special_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _shelxl_version_number 2014/6 _shelx_res_file ; TITL sm-nc3_a.res in P2(1)2(1)2(1) blue 290.9(4)K CELL 0.71073 11.7462 15.1861 25.9560 90.000 90.000 90.000 ZERR 4 0.0007 0.0009 0.0016 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z EQIV $1 X-1/2, 3/2-Y, 1-Z EQIV $2 X+1/2, 3/2-Y, 1-Z EQIV $3 X+1/2, 1/2-Y, 1-Z SFAC C H N NI O CL UNIT 136 256 24 8 72 8 TEMP 17.8 SIZE 0.08 0.10 0.13 ACTA 54.0004 MERG 2 OMIT -2 54.0004 OMIT 0 2 4 L.S. 4 BOND $H CONF HTAB O5 O2_$1 HTAB O5 O9_$1 HTAB O7 O8 HTAB O7 O3_$2 HTAB O8 O10 HTAB O8 O12_$3 HTAB O8 O13_$3 HTAB O9 O21_$1 HTAB O9 O32_$1 HTAB O9 O10 FMAP 2 PLAN 20 DFIX 0.84 0.0001 O5 H51 O5 H52 O7 H71 O7 H72 O8 H81 O8 H82 O9 H91 O9 H92 DFIX 1.40 0.0050 H81 H82 H91 H92 WGHT 0.063600 FVAR 0.11867 0.04981 0.11250 0.69687 1.40683 NI1 4 0.265788 0.650465 0.420492 11.00000 0.02342 0.02466 = 0.03396 -0.00102 0.00087 0.00195 NI2 4 0.629270 0.597646 0.459582 11.00000 0.02372 0.02322 = 0.04266 -0.00418 -0.00261 -0.00070 C31 1 0.448102 0.683155 0.467175 11.00000 0.02758 0.01940 = 0.03232 -0.00156 0.00094 -0.00146 O1 5 0.448506 0.616455 0.436464 11.00000 0.02493 0.02209 = 0.04090 -0.00597 0.00059 0.00102 O2 5 0.542712 0.706009 0.487207 11.00000 0.03027 0.02427 = 0.04472 -0.00670 -0.00559 -0.00126 O3 5 0.352836 0.720793 0.475713 11.00000 0.03575 0.02608 = 0.03693 -0.00698 -0.00072 0.00811 N1 3 0.323627 0.719864 0.357610 11.00000 0.02877 0.03048 = 0.03684 0.00216 0.00096 0.00222 C1 1 0.391635 0.790211 0.358450 11.00000 0.04201 0.03298 = 0.03907 -0.00432 0.00183 0.00204 AFIX 43 H1 2 0.410290 0.814500 0.390239 11.00000 -1.20000 AFIX 0 C2 1 0.435442 0.828567 0.315018 11.00000 0.04775 0.03558 = 0.04889 0.00380 0.00411 0.00003 C3 1 0.404617 0.792879 0.267943 11.00000 0.06084 0.04921 = 0.03830 0.01784 0.00876 0.00579 C4 1 0.329933 0.721207 0.265710 11.00000 0.04843 0.05826 = 0.03220 0.00948 -0.00157 0.00025 C5 1 0.291037 0.687694 0.312107 11.00000 0.03445 0.04471 = 0.03033 0.00173 -0.00231 0.00476 C6 1 0.511790 0.909049 0.319033 11.00000 0.08292 0.04312 = 0.08225 0.01301 0.02803 -0.01914 AFIX 137 H61 2 0.516901 0.927194 0.354387 11.00000 -1.50000 H62 2 0.480327 0.956051 0.298810 11.00000 -1.50000 H63 2 0.586378 0.894750 0.306440 11.00000 -1.50000 AFIX 0 C7 1 0.289956 0.685366 0.214632 11.00000 0.09383 0.12032 = 0.03621 0.00470 -0.00197 -0.02513 AFIX 137 H701 2 0.328139 0.630782 0.207599 11.00000 -1.50000 H702 2 0.307007 0.726978 0.187880 11.00000 -1.50000 H703 2 0.209273 0.675524 0.215905 11.00000 -1.50000 AFIX 0 O4 5 0.443484 0.828365 0.223207 11.00000 0.08433 0.07479 = 0.05391 0.02706 0.01519 0.00198 C8 1 0.547864 0.797143 0.207334 11.00000 0.09525 0.14193 = 0.06404 0.01567 0.04025 -0.01109 AFIX 137 H801 2 0.602673 0.805441 0.234337 11.00000 -1.50000 H802 2 0.571835 0.828670 0.177167 11.00000 -1.50000 H803 2 0.541821 0.735563 0.199436 11.00000 -1.50000 AFIX 0 C9 1 0.205382 0.614292 0.314357 11.00000 0.04831 0.04486 = 0.03850 -0.00045 -0.00663 -0.00555 AFIX 23 H901 2 0.129768 0.638489 0.309333 11.00000 -1.20000 H902 2 0.220143 0.573346 0.286464 11.00000 -1.20000 AFIX 0 N2 3 0.208473 0.566397 0.363559 11.00000 0.02214 0.03245 = 0.04013 -0.00253 -0.00001 0.00135 C10 1 0.094396 0.535560 0.379909 11.00000 0.02545 0.04782 = 0.05456 -0.00044 -0.00934 -0.00609 AFIX 23 H101 2 0.077907 0.479434 0.363705 11.00000 -1.20000 H102 2 0.037167 0.577531 0.368825 11.00000 -1.20000 AFIX 0 C11 1 0.089231 0.525277 0.438944 11.00000 0.02541 0.04111 = 0.05400 -0.00037 -0.00086 -0.00626 AFIX 23 H111 2 0.030669 0.563873 0.452520 11.00000 -1.20000 H112 2 0.068219 0.465182 0.447308 11.00000 -1.20000 AFIX 0 N3 3 0.198685 0.546346 0.463871 11.00000 0.02640 0.03518 = 0.04489 0.00558 -0.00035 -0.00253 C12 1 0.290629 0.492534 0.361600 11.00000 0.02996 0.03606 = 0.05715 -0.00955 0.00179 0.00383 AFIX 23 H121 2 0.367322 0.516208 0.361200 11.00000 -1.20000 H122 2 0.279406 0.460138 0.329795 11.00000 -1.20000 AFIX 0 C13 1 0.279064 0.429591 0.406698 11.00000 0.03951 0.02595 = 0.07409 -0.00261 -0.00349 0.00091 AFIX 23 H131 2 0.210090 0.395501 0.401750 11.00000 -1.20000 H132 2 0.342518 0.388765 0.405486 11.00000 -1.20000 AFIX 0 C14 1 0.275114 0.469191 0.459812 11.00000 0.03535 0.02960 = 0.06174 0.01437 -0.00476 -0.00228 AFIX 23 H141 2 0.250014 0.424540 0.484001 11.00000 -1.20000 H142 2 0.351442 0.486857 0.469642 11.00000 -1.20000 AFIX 0 C15 1 0.179467 0.568476 0.518385 11.00000 0.04973 0.05331 = 0.04940 0.01082 0.00268 -0.00530 AFIX 137 H151 2 0.141121 0.520518 0.535104 11.00000 -1.50000 H152 2 0.133442 0.620572 0.520647 11.00000 -1.50000 H153 2 0.251302 0.578773 0.534964 11.00000 -1.50000 AFIX 0 O5 5 0.114829 0.719077 0.423929 11.00000 0.03999 0.04446 = 0.04283 -0.00214 0.00005 0.01410 H51 2 0.099754 0.739418 0.453240 11.00000 21.00000 H52 2 0.111266 0.752294 0.398102 11.00000 21.00000 N4 3 0.572260 0.512626 0.515249 11.00000 0.02881 0.02596 = 0.04480 0.00254 -0.00993 0.00227 C16 1 0.499367 0.529902 0.552358 11.00000 0.03779 0.03448 = 0.04663 0.00686 -0.00862 -0.00195 AFIX 43 H16 2 0.473885 0.587625 0.555558 11.00000 -1.20000 AFIX 0 C17 1 0.457723 0.468471 0.587039 11.00000 0.04976 0.05000 = 0.04315 0.00891 -0.00660 -0.01127 C18 1 0.504241 0.385326 0.582822 11.00000 0.06042 0.04298 = 0.05126 0.00970 -0.01990 -0.01127 C19 1 0.587188 0.364985 0.547283 11.00000 0.05126 0.02745 = 0.06282 0.00822 -0.01986 -0.00568 C20 1 0.614792 0.430761 0.511177 11.00000 0.03099 0.02704 = 0.05249 -0.00125 -0.01398 -0.00053 C21 1 0.369147 0.492258 0.625801 11.00000 0.07184 0.06709 = 0.05008 0.01197 0.00918 -0.00805 AFIX 137 H211 2 0.299232 0.462696 0.617571 11.00000 -1.50000 H212 2 0.357093 0.554776 0.625307 11.00000 -1.50000 H213 2 0.394113 0.474609 0.659471 11.00000 -1.50000 AFIX 0 C22 1 0.648865 0.279476 0.547472 11.00000 0.07878 0.03362 = 0.10049 0.01218 -0.01107 0.00900 AFIX 137 H221 2 0.640492 0.251947 0.580550 11.00000 -1.50000 H222 2 0.728139 0.289512 0.540656 11.00000 -1.50000 H223 2 0.617783 0.241765 0.521333 11.00000 -1.50000 AFIX 0 O6 5 0.469459 0.323738 0.618617 11.00000 0.12438 0.05308 = 0.06801 0.02898 -0.00890 -0.02537 C23 1 0.400838 0.253811 0.599155 11.00000 0.11427 0.06056 = 0.11527 0.01827 0.00481 -0.04386 AFIX 137 H231 2 0.322266 0.271182 0.599732 11.00000 -1.50000 H232 2 0.410951 0.202451 0.620227 11.00000 -1.50000 H233 2 0.423090 0.240714 0.564401 11.00000 -1.50000 AFIX 0 C24 1 0.699039 0.415276 0.468459 11.00000 0.03471 0.02856 = 0.06940 -0.00220 -0.00743 0.00958 AFIX 23 H241 2 0.775377 0.415538 0.482711 11.00000 -1.20000 H242 2 0.685566 0.357580 0.453629 11.00000 -1.20000 AFIX 0 N5 3 0.691703 0.482609 0.427164 11.00000 0.02426 0.02950 = 0.05920 -0.00835 -0.00252 0.00061 C25 1 0.804722 0.503883 0.405218 11.00000 0.02725 0.04757 = 0.08029 -0.01645 0.00498 0.00375 AFIX 23 H251 2 0.822712 0.462344 0.378022 11.00000 -1.20000 H252 2 0.862346 0.498429 0.431796 11.00000 -1.20000 AFIX 0 C26 1 0.806258 0.598022 0.383362 11.00000 0.02400 0.05317 = 0.06399 -0.00718 0.01088 0.00072 AFIX 23 H261 2 0.863750 0.632206 0.401240 11.00000 -1.20000 H262 2 0.826816 0.595906 0.347188 11.00000 -1.20000 AFIX 0 N6 3 0.695139 0.641852 0.388835 11.00000 0.02910 0.03891 = 0.04656 0.00239 0.00110 0.00187 C27 1 0.610899 0.456905 0.386809 11.00000 0.03804 0.03574 = 0.06484 -0.01989 -0.00251 0.00626 AFIX 23 H271 2 0.534142 0.461178 0.400365 11.00000 -1.20000 H272 2 0.624375 0.395885 0.377599 11.00000 -1.20000 AFIX 0 C28 1 0.619810 0.513406 0.338573 11.00000 0.03987 0.06287 = 0.05039 -0.02009 -0.00120 0.00192 AFIX 23 H281 2 0.556733 0.498528 0.316078 11.00000 -1.20000 H282 2 0.689375 0.497543 0.320701 11.00000 -1.20000 AFIX 0 C29 1 0.619693 0.613211 0.346537 11.00000 0.03403 0.05869 = 0.04731 0.00407 0.00395 0.00408 AFIX 23 H291 2 0.643699 0.641565 0.314861 11.00000 -1.20000 H292 2 0.542626 0.632392 0.353907 11.00000 -1.20000 AFIX 0 C30 1 0.708713 0.739010 0.385689 11.00000 0.05211 0.04604 = 0.07216 0.00841 0.00704 -0.01298 AFIX 137 H301 2 0.741997 0.754375 0.353128 11.00000 -1.50000 H302 2 0.757368 0.758760 0.413068 11.00000 -1.50000 H303 2 0.635541 0.766651 0.388840 11.00000 -1.50000 AFIX 0 O7 5 0.780322 0.621028 0.495819 11.00000 0.03925 0.03126 = 0.06297 -0.00719 -0.01851 -0.00694 H71 2 0.795266 0.597415 0.524292 11.00000 21.00000 H72 2 0.802624 0.671774 0.503818 11.00000 21.00000 O8 5 0.833637 0.524797 0.576190 11.00000 0.12004 0.05437 = 0.09071 0.00727 -0.03394 0.02528 H81 2 0.797657 0.528902 0.604055 11.00000 31.00000 H82 2 0.868648 0.476823 0.573280 11.00000 31.00000 O9 5 0.583485 0.667573 0.651965 11.00000 0.10095 0.07669 = 0.08960 0.02359 0.03004 -0.00757 H91 2 0.537849 0.672640 0.676704 11.00000 31.00000 H92 2 0.632932 0.628492 0.656840 11.00000 31.00000 O10 5 0.717740 0.519531 0.666710 11.00000 0.12040 0.06364 = 0.15471 0.01674 0.01261 -0.00351 C32 1 0.691830 0.451973 0.688333 11.00000 0.07175 0.08175 = 0.08458 0.01168 -0.01631 0.00239 C33 1 0.744787 0.376934 0.678340 11.00000 0.08466 0.05260 = 0.11835 0.02809 0.02306 0.00889 AFIX 137 H331 2 0.775656 0.378801 0.644112 11.00000 -1.50000 H332 2 0.691762 0.329040 0.680974 11.00000 -1.50000 H333 2 0.805343 0.368548 0.702690 11.00000 -1.50000 AFIX 0 C34 1 0.599398 0.446219 0.726450 11.00000 0.10653 0.10947 = 0.09799 0.00244 -0.01025 0.03327 AFIX 137 H341 2 0.566726 0.503512 0.731521 11.00000 -1.50000 H342 2 0.629289 0.424872 0.758528 11.00000 -1.50000 H343 2 0.541876 0.406519 0.714169 11.00000 -1.50000 AFIX 0 EADP CL2 CL3 EADP O21 O31 EADP O22 O32 EADP O23 O33 EADP O24 O34 RIGU CL1 > O24 DFIX 51 0.005 CL2 O21 CL2 O22 CL2 O23 CL2 O24 CL3 O31 CL3 O32 CL3 O33 CL3 O34 DFIX 51.633 0.010 O21 O22 O21 O23 O21 O24 O22 O23 O22 O24 O23 O24 = O31 O32 O31 O33 O31 O34 O32 O33 O32 O34 O33 O34 CL1 6 0.509344 0.172296 0.427901 11.00000 0.06692 0.05899 = 0.08382 0.01474 -0.01939 -0.01281 O11 5 0.475209 0.258919 0.430567 11.00000 0.17486 0.08303 = 0.21123 0.03102 -0.02565 0.01901 O12 5 0.476447 0.126068 0.472740 11.00000 0.11209 0.10017 = 0.09826 0.02160 0.00224 -0.01912 O13 5 0.465704 0.129817 0.384945 11.00000 0.21389 0.14381 = 0.11953 0.01356 -0.05034 -0.07757 O14 5 0.626475 0.173818 0.423894 11.00000 0.08686 0.21794 = 0.14460 -0.01209 0.01183 -0.01508 PART 1 41 CL2 6 0.895720 0.838786 0.232956 41.00000 0.12780 0.06281 = 0.07370 0.00329 -0.03901 0.00280 O21 5 0.909453 0.771826 0.270105 41.00000 0.19775 0.14027 = 0.12526 0.04506 -0.06387 -0.00795 O22 5 1.005872 0.866293 0.218072 41.00000 0.15478 0.16597 = 0.18801 -0.02209 -0.03209 -0.01443 O23 5 0.835606 0.910436 0.252910 41.00000 0.22065 0.13033 = 0.13556 -0.06249 -0.06719 0.05261 O24 5 0.838589 0.805301 0.189479 41.00000 0.15495 0.08235 = 0.08569 -0.01095 -0.04261 0.01279 PART 2 -41 CL3 6 0.891856 0.821293 0.239781 -41.00000 0.12780 0.06281 = 0.07370 0.00329 -0.03901 0.00280 O31 5 0.811341 0.769462 0.265987 -41.00000 0.19775 0.14027 = 0.12526 0.04506 -0.06387 -0.00795 O32 5 1.001014 0.785154 0.247068 -41.00000 0.15478 0.16597 = 0.18801 -0.02209 -0.03209 -0.01443 O33 5 0.890467 0.907815 0.258931 -41.00000 0.22065 0.13033 = 0.13556 -0.06249 -0.06719 0.05261 O34 5 0.866227 0.822554 0.186795 -41.00000 0.15495 0.08235 = 0.08569 -0.01095 -0.04261 0.01279 PART 0 HKLF 4 REM sm-nc3_a.res in P2(1)2(1)2(1) blue 290.9(4)K REM R1 = 0.0522 for 7600 Fo > 4sig(Fo) and 0.0648 for all 9085 data REM 612 parameters refined using 90 restraints END WGHT 0.0634 0.0000 REM Highest difference peak 0.613, deepest hole -0.454, 1-sigma level 0.073 Q1 1 0.2469 0.6497 0.4539 11.00000 0.05 0.61 Q2 1 0.2992 0.6484 0.3860 11.00000 0.05 0.58 Q3 1 0.2384 0.6589 0.3855 11.00000 0.05 0.54 Q4 1 0.6424 0.6015 0.4947 11.00000 0.05 0.53 Q5 1 0.6631 0.6021 0.4230 11.00000 0.05 0.52 Q6 1 0.5984 0.5946 0.4241 11.00000 0.05 0.47 Q7 1 1.0075 0.8409 0.2496 11.00000 0.05 0.33 Q8 1 0.2593 0.6046 0.4617 11.00000 0.05 0.33 Q9 1 0.5817 0.5092 0.5449 11.00000 0.05 0.32 Q10 1 0.9379 0.8410 0.1936 11.00000 0.05 0.31 Q11 1 0.2009 0.6964 0.4191 11.00000 0.05 0.29 Q12 1 0.6402 0.5468 0.4211 11.00000 0.05 0.28 Q13 1 0.4596 0.8575 0.2660 11.00000 0.05 0.28 Q14 1 0.3958 0.1571 0.4172 11.00000 0.05 0.28 Q15 1 0.5896 0.2262 0.4202 11.00000 0.05 0.28 Q16 1 0.9549 0.8410 0.2680 11.00000 0.05 0.27 Q17 1 0.2671 0.6554 0.3139 11.00000 0.05 0.27 Q18 1 0.5595 0.1553 0.3882 11.00000 0.05 0.27 Q19 1 0.3377 0.7205 0.5085 11.00000 0.05 0.26 Q20 1 0.9139 0.7018 0.2966 11.00000 0.05 0.26 ; _shelx_res_checksum 10791 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 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 0.26579(5) 0.65047(4) 0.42049(3) 0.02735(17) Uani 1 1 d . . . . . Ni2 Ni 0.62927(5) 0.59765(4) 0.45958(3) 0.02986(18) Uani 1 1 d . . . . . C31 C 0.4481(4) 0.6832(3) 0.4672(2) 0.0264(11) Uani 1 1 d . . . . . O1 O 0.4485(3) 0.6165(2) 0.43646(15) 0.0293(8) Uani 1 1 d . . . . . O2 O 0.5427(3) 0.7060(2) 0.48721(15) 0.0331(9) Uani 1 1 d . . . . . O3 O 0.3528(3) 0.7208(2) 0.47571(15) 0.0329(9) Uani 1 1 d . . . . . N1 N 0.3236(4) 0.7199(3) 0.35761(19) 0.0320(11) Uani 1 1 d . . . . . C1 C 0.3916(5) 0.7902(4) 0.3584(2) 0.0380(13) Uani 1 1 d . . . . . H1 H 0.4103 0.8145 0.3902 0.046 Uiso 1 1 calc R U . . . C2 C 0.4354(6) 0.8286(4) 0.3150(3) 0.0441(15) Uani 1 1 d . . . . . C3 C 0.4046(6) 0.7929(5) 0.2679(2) 0.0495(17) Uani 1 1 d . . . . . C4 C 0.3299(6) 0.7212(5) 0.2657(2) 0.0463(16) Uani 1 1 d . . . . . C5 C 0.2910(5) 0.6877(4) 0.3121(2) 0.0365(13) Uani 1 1 d . . . . . C6 C 0.5118(7) 0.9090(5) 0.3190(3) 0.069(2) Uani 1 1 d . . . . . H61 H 0.5169 0.9272 0.3544 0.104 Uiso 1 1 calc R U . . . H62 H 0.4803 0.9561 0.2988 0.104 Uiso 1 1 calc R U . . . H63 H 0.5864 0.8948 0.3064 0.104 Uiso 1 1 calc R U . . . C7 C 0.2900(8) 0.6854(7) 0.2146(3) 0.083(3) Uani 1 1 d . . . . . H701 H 0.3281 0.6308 0.2076 0.125 Uiso 1 1 calc R U . . . H702 H 0.3070 0.7270 0.1879 0.125 Uiso 1 1 calc R U . . . H703 H 0.2093 0.6755 0.2159 0.125 Uiso 1 1 calc R U . . . O4 O 0.4435(5) 0.8284(4) 0.2232(2) 0.0710(16) Uani 1 1 d . . . . . C8 C 0.5479(9) 0.7971(9) 0.2073(4) 0.100(4) Uani 1 1 d . . . . . H801 H 0.6027 0.8054 0.2343 0.151 Uiso 1 1 calc R U . . . H802 H 0.5718 0.8287 0.1772 0.151 Uiso 1 1 calc R U . . . H803 H 0.5418 0.7356 0.1994 0.151 Uiso 1 1 calc R U . . . C9 C 0.2054(6) 0.6143(4) 0.3144(2) 0.0439(15) Uani 1 1 d . . . . . H901 H 0.1298 0.6385 0.3093 0.053 Uiso 1 1 calc R U . . . H902 H 0.2201 0.5733 0.2865 0.053 Uiso 1 1 calc R U . . . N2 N 0.2085(4) 0.5664(3) 0.36356(19) 0.0316(10) Uani 1 1 d . . . . . C10 C 0.0944(5) 0.5356(5) 0.3799(2) 0.0426(15) Uani 1 1 d . . . . . H101 H 0.0779 0.4794 0.3637 0.051 Uiso 1 1 calc R U . . . H102 H 0.0372 0.5775 0.3688 0.051 Uiso 1 1 calc R U . . . C11 C 0.0892(5) 0.5253(4) 0.4389(2) 0.0402(14) Uani 1 1 d . . . . . H111 H 0.0307 0.5639 0.4525 0.048 Uiso 1 1 calc R U . . . H112 H 0.0682 0.4652 0.4473 0.048 Uiso 1 1 calc R U . . . N3 N 0.1987(4) 0.5463(3) 0.4639(2) 0.0355(11) Uani 1 1 d . . . . . C12 C 0.2906(5) 0.4925(4) 0.3616(3) 0.0411(15) Uani 1 1 d . . . . . H121 H 0.3673 0.5162 0.3612 0.049 Uiso 1 1 calc R U . . . H122 H 0.2794 0.4601 0.3298 0.049 Uiso 1 1 calc R U . . . C13 C 0.2791(5) 0.4296(4) 0.4067(3) 0.0465(16) Uani 1 1 d . . . . . H131 H 0.2101 0.3955 0.4017 0.056 Uiso 1 1 calc R U . . . H132 H 0.3425 0.3888 0.4055 0.056 Uiso 1 1 calc R U . . . C14 C 0.2751(5) 0.4692(4) 0.4598(3) 0.0422(14) Uani 1 1 d . . . . . H141 H 0.2500 0.4245 0.4840 0.051 Uiso 1 1 calc R U . . . H142 H 0.3514 0.4869 0.4696 0.051 Uiso 1 1 calc R U . . . C15 C 0.1795(6) 0.5685(5) 0.5184(3) 0.0508(17) Uani 1 1 d . . . . . H151 H 0.1411 0.5205 0.5351 0.076 Uiso 1 1 calc R U . . . H152 H 0.1334 0.6206 0.5206 0.076 Uiso 1 1 calc R U . . . H153 H 0.2513 0.5788 0.5350 0.076 Uiso 1 1 calc R U . . . O5 O 0.1148(3) 0.7191(2) 0.42393(11) 0.0424(10) Uani 1 1 d D . . . . H51 H 0.0998(17) 0.7394(8) 0.45324(18) 0.050(10) Uiso 1 1 d D U . . . H52 H 0.111(5) 0.7523(4) 0.3981(2) 0.050(10) Uiso 1 1 d D U . . . N4 N 0.5723(4) 0.5126(3) 0.51525(19) 0.0332(11) Uani 1 1 d . . . . . C16 C 0.4994(5) 0.5299(4) 0.5524(2) 0.0396(14) Uani 1 1 d . . . . . H16 H 0.4739 0.5876 0.5556 0.048 Uiso 1 1 calc R U . . . C17 C 0.4577(6) 0.4685(5) 0.5870(3) 0.0476(16) Uani 1 1 d . . . . . C18 C 0.5042(6) 0.3853(4) 0.5828(3) 0.0516(17) Uani 1 1 d . . . . . C19 C 0.5872(6) 0.3650(4) 0.5473(3) 0.0472(16) Uani 1 1 d . . . . . C20 C 0.6148(5) 0.4308(4) 0.5112(3) 0.0368(14) Uani 1 1 d . . . . . C21 C 0.3691(7) 0.4923(5) 0.6258(3) 0.063(2) Uani 1 1 d . . . . . H211 H 0.2992 0.4627 0.6176 0.095 Uiso 1 1 calc R U . . . H212 H 0.3571 0.5548 0.6253 0.095 Uiso 1 1 calc R U . . . H213 H 0.3941 0.4746 0.6595 0.095 Uiso 1 1 calc R U . . . C22 C 0.6489(7) 0.2795(4) 0.5475(4) 0.071(2) Uani 1 1 d . . . . . H221 H 0.6405 0.2519 0.5806 0.106 Uiso 1 1 calc R U . . . H222 H 0.7281 0.2895 0.5407 0.106 Uiso 1 1 calc R U . . . H223 H 0.6178 0.2418 0.5213 0.106 Uiso 1 1 calc R U . . . O6 O 0.4695(6) 0.3237(4) 0.6186(2) 0.0818(19) Uani 1 1 d . . . . . C23 C 0.4008(9) 0.2538(6) 0.5992(4) 0.097(3) Uani 1 1 d . . . . . H231 H 0.3223 0.2712 0.5997 0.145 Uiso 1 1 calc R U . . . H232 H 0.4110 0.2025 0.6202 0.145 Uiso 1 1 calc R U . . . H233 H 0.4231 0.2407 0.5644 0.145 Uiso 1 1 calc R U . . . C24 C 0.6990(5) 0.4153(4) 0.4685(3) 0.0442(16) Uani 1 1 d . . . . . H241 H 0.7754 0.4155 0.4827 0.053 Uiso 1 1 calc R U . . . H242 H 0.6856 0.3576 0.4536 0.053 Uiso 1 1 calc R U . . . N5 N 0.6917(4) 0.4826(3) 0.4272(2) 0.0377(12) Uani 1 1 d . . . . . C25 C 0.8047(5) 0.5039(4) 0.4052(3) 0.0517(19) Uani 1 1 d . . . . . H251 H 0.8227 0.4623 0.3780 0.062 Uiso 1 1 calc R U . . . H252 H 0.8623 0.4984 0.4318 0.062 Uiso 1 1 calc R U . . . C26 C 0.8063(5) 0.5980(5) 0.3834(3) 0.0471(16) Uani 1 1 d . . . . . H261 H 0.8638 0.6322 0.4012 0.056 Uiso 1 1 calc R U . . . H262 H 0.8268 0.5959 0.3472 0.056 Uiso 1 1 calc R U . . . N6 N 0.6951(4) 0.6419(3) 0.3888(2) 0.0382(11) Uani 1 1 d . . . . . C27 C 0.6109(5) 0.4569(4) 0.3868(3) 0.0462(16) Uani 1 1 d . . . . . H271 H 0.5341 0.4612 0.4004 0.055 Uiso 1 1 calc R U . . . H272 H 0.6244 0.3959 0.3776 0.055 Uiso 1 1 calc R U . . . C28 C 0.6198(6) 0.5134(5) 0.3386(3) 0.0510(17) Uani 1 1 d . . . . . H281 H 0.5567 0.4985 0.3161 0.061 Uiso 1 1 calc R U . . . H282 H 0.6894 0.4975 0.3207 0.061 Uiso 1 1 calc R U . . . C29 C 0.6197(5) 0.6132(4) 0.3465(3) 0.0467(16) Uani 1 1 d . . . . . H291 H 0.6437 0.6416 0.3149 0.056 Uiso 1 1 calc R U . . . H292 H 0.5426 0.6324 0.3539 0.056 Uiso 1 1 calc R U . . . C30 C 0.7087(6) 0.7390(4) 0.3857(3) 0.0568(19) Uani 1 1 d . . . . . H301 H 0.7420 0.7544 0.3531 0.085 Uiso 1 1 calc R U . . . H302 H 0.7574 0.7588 0.4131 0.085 Uiso 1 1 calc R U . . . H303 H 0.6355 0.7667 0.3888 0.085 Uiso 1 1 calc R U . . . O7 O 0.7803(3) 0.6210(2) 0.49582(13) 0.0445(10) Uani 1 1 d D . . . . H71 H 0.7953(17) 0.5974(7) 0.52429(19) 0.050(10) Uiso 1 1 d D U . . . H72 H 0.8026(11) 0.6718(3) 0.5038(6) 0.050(10) Uiso 1 1 d D U . . . O8 O 0.8336(4) 0.5248(2) 0.57619(15) 0.088(2) Uani 1 1 d D . . . . H81 H 0.7977(7) 0.529(2) 0.60405(19) 0.113(19) Uiso 1 1 d D U . . . H82 H 0.8686(7) 0.4768(3) 0.5733(13) 0.113(19) Uiso 1 1 d D U . . . O9 O 0.5835(3) 0.6676(3) 0.65196(16) 0.0891(19) Uani 1 1 d D . . . . H91 H 0.5378(6) 0.6726(19) 0.6767(2) 0.113(19) Uiso 1 1 d D U . . . H92 H 0.6329(5) 0.6285(4) 0.6568(9) 0.113(19) Uiso 1 1 d D U . . . O10 O 0.7177(7) 0.5195(5) 0.6667(4) 0.113(3) Uani 1 1 d . . . . . C32 C 0.6918(8) 0.4520(7) 0.6883(4) 0.079(3) Uani 1 1 d . . . . . C33 C 0.7448(8) 0.3769(5) 0.6783(4) 0.085(3) Uani 1 1 d . . . . . H331 H 0.7757 0.3788 0.6441 0.128 Uiso 1 1 calc R U . . . H332 H 0.6918 0.3290 0.6810 0.128 Uiso 1 1 calc R U . . . H333 H 0.8053 0.3685 0.7027 0.128 Uiso 1 1 calc R U . . . C34 C 0.5994(10) 0.4462(8) 0.7265(4) 0.105(4) Uani 1 1 d . . . . . H341 H 0.5667 0.5035 0.7315 0.157 Uiso 1 1 calc R U . . . H342 H 0.6293 0.4249 0.7585 0.157 Uiso 1 1 calc R U . . . H343 H 0.5419 0.4065 0.7142 0.157 Uiso 1 1 calc R U . . . Cl1 Cl 0.50934(18) 0.17230(14) 0.42790(9) 0.0699(6) Uani 1 1 d . U . . . O11 O 0.4752(9) 0.2589(5) 0.4306(5) 0.156(4) Uani 1 1 d . U . . . O12 O 0.4764(7) 0.1261(5) 0.4727(3) 0.104(2) Uani 1 1 d . U . . . O13 O 0.4657(10) 0.1298(7) 0.3849(4) 0.159(4) Uani 1 1 d . U . . . O14 O 0.6265(7) 0.1738(8) 0.4239(4) 0.150(3) Uani 1 1 d . U . . . Cl2 Cl 0.8957(8) 0.8388(5) 0.2330(3) 0.0881(14) Uani 0.697(11) 1 d D U P A 1 O21 O 0.9095(14) 0.7718(8) 0.2701(5) 0.154(6) Uani 0.697(11) 1 d D U P A 1 O22 O 1.0059(10) 0.8663(10) 0.2181(6) 0.170(6) Uani 0.697(11) 1 d D U P A 1 O23 O 0.8356(13) 0.9104(9) 0.2529(6) 0.162(6) Uani 0.697(11) 1 d D U P A 1 O24 O 0.8386(14) 0.8053(11) 0.1895(5) 0.108(4) Uani 0.697(11) 1 d D U P A 1 Cl3 Cl 0.8919(18) 0.8213(13) 0.2398(8) 0.0881(14) Uani 0.303(11) 1 d D . P A 2 O31 O 0.811(2) 0.769(2) 0.2660(11) 0.154(6) Uani 0.303(11) 1 d D . P A 2 O32 O 1.001(2) 0.785(2) 0.2471(14) 0.170(6) Uani 0.303(11) 1 d D . P A 2 O33 O 0.890(3) 0.9078(15) 0.2589(15) 0.162(6) Uani 0.303(11) 1 d D . P A 2 O34 O 0.866(4) 0.823(3) 0.1868(9) 0.108(4) Uani 0.303(11) 1 d D . 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 0.0234(3) 0.0247(3) 0.0340(3) -0.0010(3) 0.0009(3) 0.0019(3) Ni2 0.0237(3) 0.0232(3) 0.0427(4) -0.0042(3) -0.0026(3) -0.0007(3) C31 0.028(2) 0.019(2) 0.032(3) -0.002(2) 0.001(2) -0.001(2) O1 0.0249(16) 0.0221(17) 0.041(2) -0.0060(17) 0.0006(17) 0.0010(14) O2 0.0303(18) 0.0243(18) 0.045(2) -0.0067(18) -0.0056(18) -0.0013(15) O3 0.036(2) 0.0261(18) 0.037(2) -0.0070(17) -0.0007(18) 0.0081(16) N1 0.029(2) 0.030(2) 0.037(3) 0.002(2) 0.001(2) 0.0022(19) C1 0.042(3) 0.033(3) 0.039(3) -0.004(3) 0.002(3) 0.002(3) C2 0.048(3) 0.036(3) 0.049(4) 0.004(3) 0.004(3) 0.000(3) C3 0.061(4) 0.049(4) 0.038(3) 0.018(3) 0.009(3) 0.006(3) C4 0.048(4) 0.058(4) 0.032(3) 0.009(3) -0.002(3) 0.000(3) C5 0.034(3) 0.045(3) 0.030(3) 0.002(3) -0.002(3) 0.005(3) C6 0.083(5) 0.043(4) 0.082(5) 0.013(4) 0.028(5) -0.019(4) C7 0.094(7) 0.120(8) 0.036(4) 0.005(5) -0.002(4) -0.025(6) O4 0.084(4) 0.075(4) 0.054(3) 0.027(3) 0.015(3) 0.002(3) C8 0.095(7) 0.142(10) 0.064(6) 0.016(7) 0.040(6) -0.011(7) C9 0.048(3) 0.045(3) 0.038(3) 0.000(3) -0.007(3) -0.006(3) N2 0.022(2) 0.032(2) 0.040(3) -0.003(2) 0.000(2) 0.0014(18) C10 0.025(3) 0.048(4) 0.055(4) 0.000(3) -0.009(3) -0.006(3) C11 0.025(2) 0.041(3) 0.054(4) 0.000(3) -0.001(3) -0.006(2) N3 0.026(2) 0.035(2) 0.045(3) 0.006(2) 0.000(2) -0.0025(19) C12 0.030(3) 0.036(3) 0.057(4) -0.010(3) 0.002(3) 0.004(2) C13 0.040(3) 0.026(3) 0.074(5) -0.003(3) -0.003(4) 0.001(2) C14 0.035(3) 0.030(3) 0.062(4) 0.014(3) -0.005(3) -0.002(2) C15 0.050(4) 0.053(4) 0.049(4) 0.011(4) 0.003(3) -0.005(3) O5 0.040(2) 0.044(2) 0.043(2) -0.002(2) 0.000(2) 0.0141(19) N4 0.029(2) 0.026(2) 0.045(3) 0.003(2) -0.010(2) 0.0023(19) C16 0.038(3) 0.034(3) 0.047(4) 0.007(3) -0.009(3) -0.002(3) C17 0.050(4) 0.050(4) 0.043(4) 0.009(3) -0.007(3) -0.011(3) C18 0.060(4) 0.043(4) 0.051(4) 0.010(4) -0.020(4) -0.011(3) C19 0.051(3) 0.027(3) 0.063(4) 0.008(3) -0.020(4) -0.006(3) C20 0.031(3) 0.027(3) 0.052(4) -0.001(3) -0.014(3) -0.001(2) C21 0.072(5) 0.067(5) 0.050(4) 0.012(4) 0.009(4) -0.008(4) C22 0.079(5) 0.034(3) 0.100(6) 0.012(4) -0.011(5) 0.009(4) O6 0.124(5) 0.053(3) 0.068(4) 0.029(3) -0.009(4) -0.025(3) C23 0.114(8) 0.061(5) 0.115(8) 0.018(6) 0.005(7) -0.044(6) C24 0.035(3) 0.029(3) 0.069(4) -0.002(3) -0.007(3) 0.010(2) N5 0.024(2) 0.029(2) 0.059(3) -0.008(3) -0.003(2) 0.0006(18) C25 0.027(3) 0.048(4) 0.080(5) -0.016(4) 0.005(3) 0.004(3) C26 0.024(2) 0.053(4) 0.064(4) -0.007(4) 0.011(3) 0.001(3) N6 0.029(2) 0.039(3) 0.047(3) 0.002(3) 0.001(2) 0.002(2) C27 0.038(3) 0.036(3) 0.065(4) -0.020(3) -0.003(3) 0.006(3) C28 0.040(3) 0.063(4) 0.050(4) -0.020(4) -0.001(3) 0.002(3) C29 0.034(3) 0.059(4) 0.047(3) 0.004(3) 0.004(3) 0.004(3) C30 0.052(4) 0.046(4) 0.072(5) 0.008(4) 0.007(4) -0.013(3) O7 0.039(2) 0.031(2) 0.063(3) -0.007(2) -0.019(2) -0.0069(18) O8 0.120(5) 0.054(3) 0.091(4) 0.007(4) -0.034(4) 0.025(3) O9 0.101(5) 0.077(4) 0.090(4) 0.024(4) 0.030(4) -0.008(4) O10 0.120(6) 0.064(4) 0.155(7) 0.017(5) 0.013(6) -0.004(4) C32 0.072(6) 0.082(7) 0.085(7) 0.012(6) -0.016(5) 0.002(5) C33 0.085(6) 0.053(5) 0.118(8) 0.028(5) 0.023(6) 0.009(5) C34 0.107(8) 0.109(8) 0.098(7) 0.002(7) -0.010(7) 0.033(7) Cl1 0.0669(11) 0.0590(11) 0.0838(15) 0.0147(11) -0.0194(12) -0.0128(9) O11 0.175(8) 0.083(5) 0.211(10) 0.031(6) -0.026(8) 0.019(5) O12 0.112(5) 0.100(5) 0.098(4) 0.022(4) 0.002(4) -0.019(4) O13 0.214(10) 0.144(8) 0.120(6) 0.014(5) -0.050(6) -0.078(8) O14 0.087(4) 0.218(10) 0.145(7) -0.012(8) 0.012(5) -0.015(5) Cl2 0.128(2) 0.063(4) 0.074(3) 0.003(2) -0.039(2) 0.003(2) O21 0.198(15) 0.140(8) 0.125(7) 0.045(7) -0.064(10) -0.008(10) O22 0.155(8) 0.166(13) 0.188(13) -0.022(10) -0.032(8) -0.014(8) O23 0.221(15) 0.130(7) 0.136(8) -0.062(7) -0.067(10) 0.053(9) O24 0.155(10) 0.082(8) 0.086(4) -0.011(5) -0.043(6) 0.013(6) Cl3 0.128(2) 0.063(4) 0.074(3) 0.003(2) -0.039(2) 0.003(2) O31 0.198(15) 0.140(8) 0.125(7) 0.045(7) -0.064(10) -0.008(10) O32 0.155(8) 0.166(13) 0.188(13) -0.022(10) -0.032(8) -0.014(8) O33 0.221(15) 0.130(7) 0.136(8) -0.062(7) -0.067(10) 0.053(9) O34 0.155(10) 0.082(8) 0.086(4) -0.011(5) -0.043(6) 0.013(6) 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' Cl Cl 0.1484 0.1585 '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 N1 Ni1 O5 93.41(16) . . ? N1 Ni1 O3 97.04(17) . . ? O5 Ni1 O3 97.76(14) . . ? N1 Ni1 N2 81.8(2) . . ? O5 Ni1 N2 93.62(16) . . ? O3 Ni1 N2 168.61(16) . . ? N1 Ni1 N3 159.5(2) . . ? O5 Ni1 N3 91.99(16) . . ? O3 Ni1 N3 101.78(18) . . ? N2 Ni1 N3 78.2(2) . . ? N1 Ni1 O1 87.06(16) . . ? O5 Ni1 O1 158.66(14) . . ? O3 Ni1 O1 61.07(13) . . ? N2 Ni1 O1 107.54(15) . . ? N3 Ni1 O1 94.98(16) . . ? N1 Ni1 C31 90.00(18) . . ? O5 Ni1 C31 127.87(15) . . ? O3 Ni1 C31 30.44(15) . . ? N2 Ni1 C31 138.21(17) . . ? N3 Ni1 C31 102.17(18) . . ? O1 Ni1 C31 30.81(14) . . ? O7 Ni2 N4 93.94(16) . . ? O7 Ni2 O2 97.45(14) . . ? N4 Ni2 O2 95.53(17) . . ? O7 Ni2 N5 91.50(16) . . ? N4 Ni2 N5 82.6(2) . . ? O2 Ni2 N5 170.97(16) . . ? O7 Ni2 N6 91.55(17) . . ? N4 Ni2 N6 159.5(2) . . ? O2 Ni2 N6 103.31(18) . . ? N5 Ni2 N6 77.5(2) . . ? O7 Ni2 O1 158.80(14) . . ? N4 Ni2 O1 87.66(16) . . ? O2 Ni2 O1 61.38(13) . . ? N5 Ni2 O1 109.65(16) . . ? N6 Ni2 O1 94.28(16) . . ? O7 Ni2 C31 127.85(16) . . ? N4 Ni2 C31 89.63(18) . . ? O2 Ni2 C31 30.57(15) . . ? N5 Ni2 C31 140.41(17) . . ? N6 Ni2 C31 102.48(18) . . ? O1 Ni2 C31 30.96(14) . . ? O2 C31 O3 124.9(5) . . ? O2 C31 O1 117.6(4) . . ? O3 C31 O1 117.6(4) . . ? O2 C31 Ni2 55.4(2) . . ? O3 C31 Ni2 173.0(4) . . ? O1 C31 Ni2 62.6(2) . . ? O2 C31 Ni1 173.9(4) . . ? O3 C31 Ni1 54.8(3) . . ? O1 C31 Ni1 63.2(3) . . ? Ni2 C31 Ni1 125.8(2) . . ? C31 O1 Ni2 86.4(3) . . ? C31 O1 Ni1 86.0(3) . . ? Ni2 O1 Ni1 172.40(18) . . ? C31 O2 Ni2 94.1(3) . . ? C31 O3 Ni1 94.7(3) . . ? C1 N1 C5 118.7(5) . . ? C1 N1 Ni1 126.5(4) . . ? C5 N1 Ni1 114.8(4) . . ? N1 C1 C2 123.5(6) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C1 C2 C3 117.5(6) . . ? C1 C2 C6 120.5(6) . . ? C3 C2 C6 122.0(6) . . ? O4 C3 C2 120.7(6) . . ? O4 C3 C4 118.9(6) . . ? C2 C3 C4 120.3(6) . . ? C5 C4 C3 117.2(6) . . ? C5 C4 C7 121.9(6) . . ? C3 C4 C7 120.8(6) . . ? N1 C5 C4 122.7(6) . . ? N1 C5 C9 115.4(5) . . ? C4 C5 C9 121.8(5) . . ? C2 C6 H61 109.5 . . ? C2 C6 H62 109.5 . . ? H61 C6 H62 109.5 . . ? C2 C6 H63 109.5 . . ? H61 C6 H63 109.5 . . ? H62 C6 H63 109.5 . . ? C4 C7 H701 109.5 . . ? C4 C7 H702 109.5 . . ? H701 C7 H702 109.5 . . ? C4 C7 H703 109.5 . . ? H701 C7 H703 109.5 . . ? H702 C7 H703 109.5 . . ? C3 O4 C8 114.7(7) . . ? O4 C8 H801 109.5 . . ? O4 C8 H802 109.5 . . ? H801 C8 H802 109.5 . . ? O4 C8 H803 109.5 . . ? H801 C8 H803 109.5 . . ? H802 C8 H803 109.5 . . ? N2 C9 C5 112.6(5) . . ? N2 C9 H901 109.1 . . ? C5 C9 H901 109.1 . . ? N2 C9 H902 109.1 . . ? C5 C9 H902 109.1 . . ? H901 C9 H902 107.8 . . ? C9 N2 C12 111.2(5) . . ? C9 N2 C10 112.5(5) . . ? C12 N2 C10 111.1(5) . . ? C9 N2 Ni1 108.9(3) . . ? C12 N2 Ni1 106.3(3) . . ? C10 N2 Ni1 106.6(4) . . ? N2 C10 C11 110.6(5) . . ? N2 C10 H101 109.5 . . ? C11 C10 H101 109.5 . . ? N2 C10 H102 109.5 . . ? C11 C10 H102 109.5 . . ? H101 C10 H102 108.1 . . ? N3 C11 C10 112.3(5) . . ? N3 C11 H111 109.1 . . ? C10 C11 H111 109.1 . . ? N3 C11 H112 109.1 . . ? C10 C11 H112 109.1 . . ? H111 C11 H112 107.9 . . ? C15 N3 C11 109.7(5) . . ? C15 N3 C14 110.0(5) . . ? C11 N3 C14 109.0(5) . . ? C15 N3 Ni1 113.7(4) . . ? C11 N3 Ni1 104.8(4) . . ? C14 N3 Ni1 109.3(3) . . ? N2 C12 C13 113.1(5) . . ? N2 C12 H121 109.0 . . ? C13 C12 H121 109.0 . . ? N2 C12 H122 109.0 . . ? C13 C12 H122 109.0 . . ? H121 C12 H122 107.8 . . ? C14 C13 C12 117.2(5) . . ? C14 C13 H131 108.0 . . ? C12 C13 H131 108.0 . . ? C14 C13 H132 108.0 . . ? C12 C13 H132 108.0 . . ? H131 C13 H132 107.2 . . ? N3 C14 C13 113.6(5) . . ? N3 C14 H141 108.8 . . ? C13 C14 H141 108.8 . . ? N3 C14 H142 108.8 . . ? C13 C14 H142 108.8 . . ? H141 C14 H142 107.7 . . ? N3 C15 H151 109.5 . . ? N3 C15 H152 109.5 . . ? H151 C15 H152 109.5 . . ? N3 C15 H153 109.5 . . ? H151 C15 H153 109.5 . . ? H152 C15 H153 109.5 . . ? Ni1 O5 H51 114.0(12) . . ? Ni1 O5 H52 108(3) . . ? H51 O5 H52 119.4(13) . . ? C16 N4 C20 119.0(5) . . ? C16 N4 Ni2 127.1(4) . . ? C20 N4 Ni2 113.9(4) . . ? N4 C16 C17 124.8(6) . . ? N4 C16 H16 117.6 . . ? C17 C16 H16 117.6 . . ? C18 C17 C16 115.1(6) . . ? C18 C17 C21 123.4(7) . . ? C16 C17 C21 121.4(6) . . ? C19 C18 C17 122.6(6) . . ? C19 C18 O6 120.6(6) . . ? C17 C18 O6 116.7(7) . . ? C18 C19 C20 116.7(6) . . ? C18 C19 C22 122.6(7) . . ? C20 C19 C22 120.6(7) . . ? N4 C20 C19 121.2(6) . . ? N4 C20 C24 116.6(5) . . ? C19 C20 C24 122.1(5) . . ? C17 C21 H211 109.5 . . ? C17 C21 H212 109.5 . . ? H211 C21 H212 109.5 . . ? C17 C21 H213 109.5 . . ? H211 C21 H213 109.5 . . ? H212 C21 H213 109.5 . . ? C19 C22 H221 109.5 . . ? C19 C22 H222 109.5 . . ? H221 C22 H222 109.5 . . ? C19 C22 H223 109.5 . . ? H221 C22 H223 109.5 . . ? H222 C22 H223 109.5 . . ? C18 O6 C23 115.7(6) . . ? O6 C23 H231 109.5 . . ? O6 C23 H232 109.5 . . ? H231 C23 H232 109.5 . . ? O6 C23 H233 109.5 . . ? H231 C23 H233 109.5 . . ? H232 C23 H233 109.5 . . ? N5 C24 C20 112.7(4) . . ? N5 C24 H241 109.0 . . ? C20 C24 H241 109.0 . . ? N5 C24 H242 109.0 . . ? C20 C24 H242 109.0 . . ? H241 C24 H242 107.8 . . ? C27 N5 C25 111.3(5) . . ? C27 N5 C24 111.7(5) . . ? C25 N5 C24 112.1(5) . . ? C27 N5 Ni2 106.6(3) . . ? C25 N5 Ni2 106.8(4) . . ? C24 N5 Ni2 107.9(4) . . ? N5 C25 C26 110.8(5) . . ? N5 C25 H251 109.5 . . ? C26 C25 H251 109.5 . . ? N5 C25 H252 109.5 . . ? C26 C25 H252 109.5 . . ? H251 C25 H252 108.1 . . ? N6 C26 C25 112.0(5) . . ? N6 C26 H261 109.2 . . ? C25 C26 H261 109.2 . . ? N6 C26 H262 109.2 . . ? C25 C26 H262 109.2 . . ? H261 C26 H262 107.9 . . ? C26 N6 C29 109.1(5) . . ? C26 N6 C30 110.4(5) . . ? C29 N6 C30 108.4(5) . . ? C26 N6 Ni2 105.4(4) . . ? C29 N6 Ni2 109.5(4) . . ? C30 N6 Ni2 113.9(5) . . ? N5 C27 C28 113.2(5) . . ? N5 C27 H271 108.9 . . ? C28 C27 H271 108.9 . . ? N5 C27 H272 108.9 . . ? C28 C27 H272 108.9 . . ? H271 C27 H272 107.8 . . ? C27 C28 C29 116.6(6) . . ? C27 C28 H281 108.1 . . ? C29 C28 H281 108.1 . . ? C27 C28 H282 108.1 . . ? C29 C28 H282 108.1 . . ? H281 C28 H282 107.3 . . ? N6 C29 C28 113.1(5) . . ? N6 C29 H291 109.0 . . ? C28 C29 H291 109.0 . . ? N6 C29 H292 109.0 . . ? C28 C29 H292 109.0 . . ? H291 C29 H292 107.8 . . ? N6 C30 H301 109.5 . . ? N6 C30 H302 109.5 . . ? H301 C30 H302 109.5 . . ? N6 C30 H303 109.5 . . ? H301 C30 H303 109.5 . . ? H302 C30 H303 109.5 . . ? Ni2 O7 H71 120.9(14) . . ? Ni2 O7 H72 123.0(9) . . ? H71 O7 H72 96.3(14) . . ? H81 O8 H82 112.8(8) . . ? H91 O9 H92 113.0(8) . . ? O10 C32 C33 121.4(10) . . ? O10 C32 C34 123.3(10) . . ? C33 C32 C34 115.3(10) . . ? C32 C33 H331 109.5 . . ? C32 C33 H332 109.5 . . ? H331 C33 H332 109.5 . . ? C32 C33 H333 109.5 . . ? H331 C33 H333 109.5 . . ? H332 C33 H333 109.5 . . ? C32 C34 H341 109.5 . . ? C32 C34 H342 109.5 . . ? H341 C34 H342 109.5 . . ? C32 C34 H343 109.5 . . ? H341 C34 H343 109.5 . . ? H342 C34 H343 109.5 . . ? O11 Cl1 O14 106.1(7) . . ? O11 Cl1 O13 112.2(7) . . ? O14 Cl1 O13 108.4(7) . . ? O11 Cl1 O12 110.7(7) . . ? O14 Cl1 O12 110.1(6) . . ? O13 Cl1 O12 109.3(5) . . ? O23 Cl2 O24 109.7(7) . . ? O23 Cl2 O21 111.5(7) . . ? O24 Cl2 O21 110.0(7) . . ? O23 Cl2 O22 109.5(8) . . ? O24 Cl2 O22 108.9(7) . . ? O21 Cl2 O22 107.2(7) . . ? O33 Cl3 O31 110.2(9) . . ? O33 Cl3 O32 109.1(9) . . ? O31 Cl3 O32 109.2(9) . . ? O33 Cl3 O34 109.3(9) . . ? O31 Cl3 O34 109.7(9) . . ? O32 Cl3 O34 109.4(9) . . ? 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 N1 2.058(5) . ? Ni1 O5 2.059(4) . ? Ni1 O3 2.059(4) . ? Ni1 N2 2.066(5) . ? Ni1 N3 2.095(5) . ? Ni1 O1 2.246(3) . ? Ni1 C31 2.510(5) . ? Ni2 O7 2.039(4) . ? Ni2 N4 2.050(5) . ? Ni2 O2 2.063(4) . ? Ni2 N5 2.073(5) . ? Ni2 N6 2.103(5) . ? Ni2 O1 2.225(4) . ? Ni2 C31 2.501(5) . ? C31 O2 1.275(6) . ? C31 O3 1.276(6) . ? C31 O1 1.289(6) . ? N1 C1 1.334(8) . ? N1 C5 1.334(7) . ? C1 C2 1.369(9) . ? C1 H1 0.93 . ? C2 C3 1.385(9) . ? C2 C6 1.520(10) . ? C3 O4 1.359(8) . ? C3 C4 1.399(10) . ? C4 C5 1.385(8) . ? C4 C7 1.508(10) . ? C5 C9 1.503(9) . ? C6 H61 0.96 . ? C6 H62 0.96 . ? C6 H63 0.96 . ? C7 H701 0.96 . ? C7 H702 0.96 . ? C7 H703 0.96 . ? O4 C8 1.378(11) . ? C8 H801 0.96 . ? C8 H802 0.96 . ? C8 H803 0.96 . ? C9 N2 1.470(8) . ? C9 H901 0.97 . ? C9 H902 0.97 . ? N2 C12 1.481(7) . ? N2 C10 1.482(7) . ? C10 C11 1.541(9) . ? C10 H101 0.97 . ? C10 H102 0.97 . ? C11 N3 1.474(7) . ? C11 H111 0.97 . ? C11 H112 0.97 . ? N3 C15 1.472(9) . ? N3 C14 1.480(7) . ? C12 C13 1.517(9) . ? C12 H121 0.97 . ? C12 H122 0.97 . ? C13 C14 1.505(9) . ? C13 H131 0.97 . ? C13 H132 0.97 . ? C14 H141 0.97 . ? C14 H142 0.97 . ? C15 H151 0.96 . ? C15 H152 0.96 . ? C15 H153 0.96 . ? O5 H51 0.84 . ? O5 H52 0.84 . ? N4 C16 1.315(8) . ? N4 C20 1.344(7) . ? C16 C17 1.386(9) . ? C16 H16 0.93 . ? C17 C18 1.380(10) . ? C17 C21 1.492(10) . ? C18 C19 1.377(11) . ? C18 O6 1.380(8) . ? C19 C20 1.408(9) . ? C19 C22 1.487(9) . ? C20 C24 1.505(9) . ? C21 H211 0.96 . ? C21 H212 0.96 . ? C21 H213 0.96 . ? C22 H221 0.96 . ? C22 H222 0.96 . ? C22 H223 0.96 . ? O6 C23 1.426(10) . ? C23 H231 0.96 . ? C23 H232 0.96 . ? C23 H233 0.96 . ? C24 N5 1.484(8) . ? C24 H241 0.97 . ? C24 H242 0.97 . ? N5 C27 1.466(8) . ? N5 C25 1.480(8) . ? C25 C26 1.538(10) . ? C25 H251 0.97 . ? C25 H252 0.97 . ? C26 N6 1.472(7) . ? C26 H261 0.97 . ? C26 H262 0.97 . ? N6 C29 1.476(8) . ? N6 C30 1.486(8) . ? C27 C28 1.521(10) . ? C27 H271 0.97 . ? C27 H272 0.97 . ? C28 C29 1.530(10) . ? C28 H281 0.97 . ? C28 H282 0.97 . ? C29 H291 0.97 . ? C29 H292 0.97 . ? C30 H301 0.96 . ? C30 H302 0.96 . ? C30 H303 0.96 . ? O7 H71 0.84 . ? O7 H72 0.84 . ? O8 H81 0.84 . ? O8 H82 0.84 . ? O9 H91 0.84 . ? O9 H92 0.84 . ? O10 C32 1.208(11) . ? C32 C33 1.324(12) . ? C32 C34 1.471(14) . ? C33 H331 0.96 . ? C33 H332 0.96 . ? C33 H333 0.96 . ? C34 H341 0.96 . ? C34 H342 0.96 . ? C34 H343 0.96 . ? Cl1 O11 1.377(8) . ? Cl1 O14 1.380(8) . ? Cl1 O13 1.386(9) . ? Cl1 O12 1.413(7) . ? Cl2 O23 1.397(7) . ? Cl2 O24 1.408(7) . ? Cl2 O21 1.411(8) . ? Cl2 O22 1.413(8) . ? Cl3 O33 1.405(8) . ? Cl3 O31 1.406(8) . ? Cl3 O32 1.407(8) . ? Cl3 O34 1.408(8) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H51 O2 0.84 1.878(6) 2.708(5) 169.5(16) 4_466 O5 H52 O9 0.84 1.810(9) 2.642(5) 170(4) 4_466 O7 H71 O8 0.84 1.798(6) 2.623(5) 166.7(10) . O7 H72 O3 0.84 1.814(5) 2.654(4) 177.1(15) 4_566 O8 H81 O10 0.84 1.883(11) 2.717(10) 171(3) . O8 H82 O12 0.84 2.339(17) 3.111(8) 153(3) 4_556 O8 H82 O13 0.84 2.26(2) 2.990(10) 146(3) 4_556 O9 H91 O21 0.84 2.212(17) 3.019(15) 161(2) 4_466 O9 H91 O32 0.84 2.12(4) 2.88(3) 150.4(16) 4_466 O9 H92 O10 0.84 1.948(8) 2.773(9) 166.8(9) . 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 O2 C31 O1 Ni2 7.1(4) . . . . ? O3 C31 O1 Ni2 -172.1(5) . . . . ? Ni1 C31 O1 Ni2 -179.76(18) . . . . ? O2 C31 O1 Ni1 -173.1(5) . . . . ? O3 C31 O1 Ni1 7.6(4) . . . . ? Ni2 C31 O1 Ni1 179.76(18) . . . . ? O3 C31 O2 Ni2 171.5(5) . . . . ? O1 C31 O2 Ni2 -7.7(5) . . . . ? O2 C31 O3 Ni1 172.5(5) . . . . ? O1 C31 O3 Ni1 -8.3(5) . . . . ? C5 N1 C1 C2 -3.9(9) . . . . ? Ni1 N1 C1 C2 173.8(5) . . . . ? N1 C1 C2 C3 1.5(10) . . . . ? N1 C1 C2 C6 179.6(6) . . . . ? C1 C2 C3 O4 179.0(6) . . . . ? C6 C2 C3 O4 1.0(11) . . . . ? C1 C2 C3 C4 1.0(10) . . . . ? C6 C2 C3 C4 -177.0(7) . . . . ? O4 C3 C4 C5 -179.1(6) . . . . ? C2 C3 C4 C5 -1.1(10) . . . . ? O4 C3 C4 C7 -1.9(11) . . . . ? C2 C3 C4 C7 176.1(7) . . . . ? C1 N1 C5 C4 3.7(9) . . . . ? Ni1 N1 C5 C4 -174.2(5) . . . . ? C1 N1 C5 C9 -174.1(5) . . . . ? Ni1 N1 C5 C9 7.9(7) . . . . ? C3 C4 C5 N1 -1.3(10) . . . . ? C7 C4 C5 N1 -178.5(7) . . . . ? C3 C4 C5 C9 176.4(6) . . . . ? C7 C4 C5 C9 -0.8(11) . . . . ? C2 C3 O4 C8 86.5(10) . . . . ? C4 C3 O4 C8 -95.5(9) . . . . ? N1 C5 C9 N2 -24.3(7) . . . . ? C4 C5 C9 N2 157.8(6) . . . . ? C5 C9 N2 C12 -89.0(6) . . . . ? C5 C9 N2 C10 145.6(5) . . . . ? C5 C9 N2 Ni1 27.7(6) . . . . ? C9 N2 C10 C11 -154.1(5) . . . . ? C12 N2 C10 C11 80.5(7) . . . . ? Ni1 N2 C10 C11 -34.8(6) . . . . ? N2 C10 C11 N3 -1.4(8) . . . . ? C10 C11 N3 C15 158.5(6) . . . . ? C10 C11 N3 C14 -80.9(7) . . . . ? C10 C11 N3 Ni1 36.1(6) . . . . ? C9 N2 C12 C13 -167.7(5) . . . . ? C10 N2 C12 C13 -41.5(7) . . . . ? Ni1 N2 C12 C13 74.0(5) . . . . ? N2 C12 C13 C14 -49.2(7) . . . . ? C15 N3 C14 C13 167.2(5) . . . . ? C11 N3 C14 C13 46.9(6) . . . . ? Ni1 N3 C14 C13 -67.2(5) . . . . ? C12 C13 C14 N3 45.3(7) . . . . ? C20 N4 C16 C17 -3.1(9) . . . . ? Ni2 N4 C16 C17 175.5(5) . . . . ? N4 C16 C17 C18 4.3(9) . . . . ? N4 C16 C17 C21 -175.8(6) . . . . ? C16 C17 C18 C19 0.9(10) . . . . ? C21 C17 C18 C19 -179.0(6) . . . . ? C16 C17 C18 O6 176.5(6) . . . . ? C21 C17 C18 O6 -3.4(10) . . . . ? C17 C18 C19 C20 -6.6(10) . . . . ? O6 C18 C19 C20 178.0(6) . . . . ? C17 C18 C19 C22 171.2(7) . . . . ? O6 C18 C19 C22 -4.3(10) . . . . ? C16 N4 C20 C19 -3.2(8) . . . . ? Ni2 N4 C20 C19 178.0(4) . . . . ? C16 N4 C20 C24 -179.2(5) . . . . ? Ni2 N4 C20 C24 2.0(6) . . . . ? C18 C19 C20 N4 7.9(9) . . . . ? C22 C19 C20 N4 -169.9(6) . . . . ? C18 C19 C20 C24 -176.5(6) . . . . ? C22 C19 C20 C24 5.7(9) . . . . ? C19 C18 O6 C23 -73.2(10) . . . . ? C17 C18 O6 C23 111.2(8) . . . . ? N4 C20 C24 N5 -20.1(7) . . . . ? C19 C20 C24 N5 164.0(5) . . . . ? C20 C24 N5 C27 -90.0(6) . . . . ? C20 C24 N5 C25 144.3(5) . . . . ? C20 C24 N5 Ni2 26.9(5) . . . . ? C27 N5 C25 C26 80.9(7) . . . . ? C24 N5 C25 C26 -153.1(5) . . . . ? Ni2 N5 C25 C26 -35.1(7) . . . . ? N5 C25 C26 N6 -1.2(8) . . . . ? C25 C26 N6 C29 -81.5(7) . . . . ? C25 C26 N6 C30 159.4(6) . . . . ? C25 C26 N6 Ni2 36.0(6) . . . . ? C25 N5 C27 C28 -41.2(7) . . . . ? C24 N5 C27 C28 -167.4(5) . . . . ? Ni2 N5 C27 C28 74.9(5) . . . . ? N5 C27 C28 C29 -49.4(8) . . . . ? C26 N6 C29 C28 47.3(7) . . . . ? C30 N6 C29 C28 167.5(6) . . . . ? Ni2 N6 C29 C28 -67.7(6) . . . . ? C27 C28 C29 N6 45.2(8) . . . . ?