#------------------------------------------------------------------------------ #$Date: 2021-04-27 04:54:06 +0300 (Tue, 27 Apr 2021) $ #$Revision: 264567 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/71/7707195.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_7707195 loop_ _publ_author_name 'Sethuraman, Muthuramalingam' 'Velusamy, Marappan' 'Mayilmurugan, Ramasamy' _publ_section_title ; Fixation of atmospheric CO2 as C1-feedstock by nickel(II) complexes ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT03887C _journal_year 2021 _chemical_absolute_configuration ad _chemical_formula_moiety 'C31 H48 N8 Ni2 O3, 2(C24 H20 B), 2(C2 H3 N)' _chemical_formula_sum 'C83 H94 B2 N10 Ni2 O3' _chemical_formula_weight 1418.72 _chemical_name_common '(mu2-carbonatato)-bis(acetonitrile)-bis[1-methyl-4-(2-pyridin-2-ylethyl)-1,4-diazepane-N,N',N"]-di-nickel(II) bis(tetraphenylborate) acetonitrile solvate (1:2)' _chemical_name_systematic '(mu2-carbonatato)-bis(acetonitrile)-bis[1-methyl-4-(2-pyridin-2-ylethyl)-1,4-diazepane-N,N',N"]-di-nickel(II) bis(tetraphenylborate) acetonitrile solvate (1:2)' _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' _space_group_name_H-M_alt 'P n a 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _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 31.3574(16) _cell_length_b 11.0783(5) _cell_length_c 21.4842(10) _cell_measurement_reflns_used 4963 _cell_measurement_temperature 291.19(18) _cell_measurement_theta_max 25.682 _cell_measurement_theta_min 3.607 _cell_volume 7463.3(6) _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 291.19(18) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1279 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -99.00 -56.00 1.0000 8.8100 omega____ theta____ kappa____ phi______ frames - -20.2184 178.0000 -90.0000 43 #__ type_ start__ end____ width___ exp.time_ 2 omega -23.00 13.00 1.0000 8.8100 omega____ theta____ kappa____ phi______ frames - -20.2184 57.0000 -150.0000 36 #__ type_ start__ end____ width___ exp.time_ 3 omega -45.00 73.00 1.0000 8.8100 omega____ theta____ kappa____ phi______ frames - 22.5622 0.0000 -90.0000 118 ; _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 0.0350 _diffrn_reflns_av_unetI/netI 0.0623 _diffrn_reflns_Laue_measured_fraction_full 0.987 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 24457 _diffrn_reflns_point_group_measured_fraction_full 0.786 _diffrn_reflns_point_group_measured_fraction_max 0.786 _diffrn_reflns_theta_full 27.00 _diffrn_reflns_theta_max 27.00 _diffrn_reflns_theta_min 3.127 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.561 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.90123 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.263 _exptl_crystal_description block _exptl_crystal_F_000 3008 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.313 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.042 _refine_ls_abs_structure_details ; Flack x determined using 3225 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.019(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 907 _refine_ls_number_reflns 12818 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.019 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0396 _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^)+(0.0019P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.0708 _reflns_Friedel_coverage 0.550 _reflns_Friedel_fraction_full 0.573 _reflns_Friedel_fraction_max 0.573 _reflns_number_gt 10349 _reflns_number_total 12818 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt03887c2.cif _cod_data_source_block MU2a _cod_database_code 7707195 _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 0.926 _shelx_estimated_absorpt_t_max 0.951 _shelxl_version_number 2014/6 _shelx_res_file ; TITL M-1 in Pna2(1) F.Belaj blue 291.19(18)K CELL 0.71073 31.3574 11.0783 21.4842 90.0000 90.0000 90.0000 ZERR 4 0.0016 0.0005 0.0010 0.0000 0.0000 0.0000 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5-X,0.5+Y,0.5+Z SYMM 0.5+X,0.5-Y,+Z SFAC C H B N Ni O UNIT 332 376 8 40 8 12 TEMP 18.04 SIZE 0.14 0.12 0.09 ACTA 54.0004 MERG 2 OMIT -2 54.0004 L.S. 4 BOND $H CONF FMAP 2 PLAN 20 WGHT 0.001900 FVAR 0.06781 N3 4 0.469067 0.267267 0.514533 11.00000 0.03737 0.06188 = 0.04899 0.00071 0.00675 0.00387 C28 1 0.279102 0.456400 0.660874 11.00000 0.05999 0.07248 = 0.06095 -0.02021 0.01773 -0.00279 AFIX 137 H281 2 0.267259 0.521030 0.636641 11.00000 -1.50000 H282 2 0.307744 0.476505 0.672776 11.00000 -1.50000 H283 2 0.262101 0.444375 0.697513 11.00000 -1.50000 AFIX 0 C10 1 0.433095 0.047072 0.570994 11.00000 0.06697 0.04711 = 0.07758 -0.01640 -0.00077 0.00619 AFIX 23 H101 2 0.404012 0.070986 0.580184 11.00000 -1.20000 H102 2 0.436211 -0.037019 0.582724 11.00000 -1.20000 AFIX 0 C11 1 0.440452 0.058649 0.503201 11.00000 0.06972 0.07375 = 0.07890 -0.02508 -0.01176 0.00733 AFIX 23 H111 2 0.418359 0.014156 0.481470 11.00000 -1.20000 H112 2 0.467555 0.021199 0.493163 11.00000 -1.20000 AFIX 0 C13 1 0.475123 0.379289 0.479106 11.00000 0.08152 0.08565 = 0.06574 0.01856 0.03166 0.01454 AFIX 137 H131 2 0.491716 0.435023 0.503277 11.00000 -1.50000 H132 2 0.447844 0.414384 0.469946 11.00000 -1.50000 H133 2 0.489771 0.361710 0.440930 11.00000 -1.50000 AFIX 0 C9 1 0.510920 0.207541 0.527426 11.00000 0.03975 0.08716 = 0.07003 -0.00773 0.01309 0.01319 AFIX 23 H91 2 0.532161 0.268320 0.537176 11.00000 -1.20000 H92 2 0.520322 0.164119 0.490701 11.00000 -1.20000 AFIX 0 C8 1 0.506613 0.118914 0.582598 11.00000 0.03664 0.07441 = 0.08674 -0.01176 -0.00738 0.02114 AFIX 23 H81 2 0.513355 0.037879 0.568612 11.00000 -1.20000 H82 2 0.526881 0.140740 0.614796 11.00000 -1.20000 AFIX 0 C12 1 0.440846 0.184611 0.479497 11.00000 0.05940 0.08386 = 0.05187 -0.01823 0.00411 0.01439 AFIX 23 H121 2 0.449819 0.183654 0.436291 11.00000 -1.20000 H122 2 0.411999 0.216118 0.480821 11.00000 -1.20000 AFIX 0 N4 4 0.498788 0.378567 0.636652 11.00000 0.03871 0.05945 = 0.06160 -0.00164 -0.00588 -0.00926 N8 4 0.261762 0.479359 0.504771 11.00000 0.03922 0.06160 = 0.07133 0.00849 -0.00679 0.00308 C14 1 0.521898 0.451809 0.651230 11.00000 0.03632 0.05143 = 0.06848 0.00048 -0.00498 0.00409 C15 1 0.551365 0.544270 0.670629 11.00000 0.04672 0.05469 = 0.13747 -0.01256 -0.01625 0.00137 AFIX 137 H151 2 0.538105 0.594394 0.701517 11.00000 -1.50000 H152 2 0.559219 0.592669 0.635381 11.00000 -1.50000 H153 2 0.576402 0.507343 0.687912 11.00000 -1.50000 AFIX 0 C29 1 0.236265 0.541161 0.486878 11.00000 0.04212 0.04563 = 0.08435 0.01199 -0.00368 -0.00781 C30 1 0.202315 0.619315 0.464666 11.00000 0.05264 0.06107 = 0.17061 0.03812 -0.03052 0.00287 AFIX 137 H301 2 0.209465 0.649260 0.424054 11.00000 -1.50000 H302 2 0.198875 0.685901 0.492819 11.00000 -1.50000 H303 2 0.176172 0.574426 0.462449 11.00000 -1.50000 AFIX 0 C81 1 0.477930 0.723350 0.529673 11.00000 0.08742 0.07212 = 0.08462 -0.00095 -0.00294 0.00585 N9 4 0.508546 0.743859 0.556663 11.00000 0.11587 0.15655 = 0.10384 -0.01241 -0.00415 -0.01013 C80 1 0.440173 0.701489 0.496523 11.00000 0.11663 0.07557 = 0.11720 0.02577 -0.03010 -0.01173 AFIX 137 H801 2 0.417945 0.679232 0.525025 11.00000 -1.50000 H802 2 0.444745 0.637069 0.467391 11.00000 -1.50000 H803 2 0.431990 0.773205 0.474467 11.00000 -1.50000 AFIX 0 NI1 5 0.442764 0.299273 0.605226 11.00000 0.03081 0.03749 = 0.04096 -0.00111 -0.00050 -0.00014 NI2 5 0.310729 0.367084 0.535512 11.00000 0.02904 0.03835 = 0.04448 0.00095 0.00011 -0.00099 N6 4 0.278683 0.205515 0.525254 11.00000 0.03094 0.04623 = 0.05451 -0.00135 -0.00154 -0.00886 N5 4 0.335715 0.367252 0.444360 11.00000 0.03819 0.05234 = 0.03929 0.00447 -0.00456 -0.00644 O1 6 0.374779 0.314913 0.569754 11.00000 0.03340 0.02960 = 0.04053 -0.00237 0.00298 -0.00134 O2 6 0.418874 0.466543 0.588261 11.00000 0.03471 0.03325 = 0.05065 0.00161 -0.00234 -0.00770 N2 4 0.462498 0.120669 0.609081 11.00000 0.04237 0.04371 = 0.05333 -0.00252 -0.00058 0.00861 O3 6 0.351064 0.502527 0.561495 11.00000 0.03755 0.03511 = 0.05322 0.00166 -0.00164 0.00489 N1 4 0.417558 0.297366 0.696905 11.00000 0.04153 0.04403 = 0.03919 -0.00145 -0.00622 0.00062 C44 1 0.620920 0.378878 0.409384 11.00000 0.04120 0.03646 = 0.03385 0.00248 0.00222 0.00019 C62 1 0.077268 0.313116 0.798659 11.00000 0.03420 0.04880 = 0.03432 0.00584 0.00045 0.00188 C31 1 0.381798 0.429806 0.573398 11.00000 0.03471 0.03555 = 0.02833 -0.00110 0.00336 -0.00339 N7 4 0.279414 0.345413 0.623767 11.00000 0.03649 0.05314 = 0.04775 -0.00167 0.00884 -0.00380 C25 1 0.301049 0.112285 0.564004 11.00000 0.05009 0.03702 = 0.07333 0.00243 0.00096 -0.00606 AFIX 23 H251 2 0.291969 0.032805 0.550470 11.00000 -1.20000 H252 2 0.331491 0.118383 0.556621 11.00000 -1.20000 AFIX 0 C67 1 0.056484 0.203980 0.790254 11.00000 0.03988 0.06351 = 0.04960 -0.00232 0.00299 -0.00426 AFIX 43 H67 2 0.070425 0.143158 0.768434 11.00000 -1.20000 AFIX 0 C56 1 0.139420 0.234787 0.723293 11.00000 0.03460 0.03728 = 0.03905 0.00705 0.00562 -0.00061 C61 1 0.122753 0.232031 0.663369 11.00000 0.04421 0.03946 = 0.04157 0.00897 -0.00192 0.00088 AFIX 43 H61 2 0.104505 0.293724 0.651023 11.00000 -1.20000 AFIX 0 C74 1 0.126338 0.471749 0.735450 11.00000 0.03518 0.03768 = 0.03231 -0.00390 0.00156 -0.00160 C43 1 0.671812 0.225145 0.344953 11.00000 0.03435 0.05604 = 0.03687 -0.00375 -0.00138 0.00277 B2 3 0.125885 0.341474 0.772745 11.00000 0.03095 0.03716 = 0.04040 0.00046 0.00146 0.00134 C52 1 0.625644 0.147457 0.486572 11.00000 0.04592 0.04339 = 0.04248 -0.00748 -0.00493 0.00419 AFIX 43 H52 2 0.639998 0.216312 0.499774 11.00000 -1.20000 AFIX 0 C51 1 0.613096 0.140679 0.424186 11.00000 0.02855 0.04021 = 0.03857 -0.00747 -0.00040 0.00304 C26 1 0.293019 0.123621 0.631983 11.00000 0.05704 0.06176 = 0.06288 0.02042 0.00259 -0.00864 AFIX 23 H261 2 0.311323 0.066682 0.653494 11.00000 -1.20000 H262 2 0.263759 0.099906 0.640051 11.00000 -1.20000 AFIX 0 C59 1 0.158785 0.047662 0.636784 11.00000 0.06922 0.04195 = 0.04782 -0.00329 0.01949 -0.00537 AFIX 43 H59 2 0.165199 -0.012978 0.608351 11.00000 -1.20000 AFIX 0 B1 3 0.623829 0.248193 0.373595 11.00000 0.03141 0.04053 = 0.03312 -0.00323 -0.00298 0.00227 C45 1 0.655987 0.430688 0.440195 11.00000 0.04532 0.04377 = 0.04601 0.00070 -0.00573 0.00007 AFIX 43 H45 2 0.682122 0.391229 0.438030 11.00000 -1.20000 AFIX 0 C79 1 0.089944 0.524911 0.711221 11.00000 0.03400 0.05930 = 0.06833 0.01307 0.00182 0.00619 AFIX 43 H79 2 0.063789 0.487970 0.718543 11.00000 -1.20000 AFIX 0 C68 1 0.159355 0.341243 0.831804 11.00000 0.04025 0.03894 = 0.04256 0.00356 -0.00177 -0.00009 C5 1 0.407177 0.198188 0.729482 11.00000 0.05060 0.04938 = 0.04449 0.00698 -0.00125 -0.00204 C50 1 0.592749 0.032473 0.409007 11.00000 0.05015 0.04381 = 0.04079 -0.00462 -0.01086 0.00085 AFIX 43 H50 2 0.584152 0.021109 0.367994 11.00000 -1.20000 AFIX 0 C37 1 0.600234 0.264773 0.254588 11.00000 0.06163 0.05583 = 0.04239 -0.00454 -0.00523 -0.00269 AFIX 43 H37 2 0.628856 0.278307 0.245650 11.00000 -1.20000 AFIX 0 C1 1 0.408051 0.404262 0.721500 11.00000 0.05824 0.04708 = 0.04332 -0.00521 -0.00113 -0.00052 AFIX 43 H1 2 0.416295 0.473108 0.699849 11.00000 -1.20000 AFIX 0 C24 1 0.235028 0.307852 0.607174 11.00000 0.03277 0.06895 = 0.06970 0.00129 0.01155 -0.00475 AFIX 23 H241 2 0.217861 0.379015 0.599167 11.00000 -1.20000 H242 2 0.222416 0.264842 0.641927 11.00000 -1.20000 AFIX 0 C4 1 0.384585 0.208360 0.784558 11.00000 0.06729 0.07162 = 0.04992 0.02161 0.00537 -0.00076 AFIX 43 H4 2 0.376455 0.139064 0.805919 11.00000 -1.20000 AFIX 0 C57 1 0.166104 0.137709 0.737572 11.00000 0.05582 0.05598 = 0.04329 0.00920 0.00548 0.01161 AFIX 43 H57 2 0.178088 0.133992 0.777122 11.00000 -1.20000 AFIX 0 C19 1 0.361596 0.275562 0.351849 11.00000 0.06155 0.08732 = 0.04404 -0.00609 0.00399 -0.00253 AFIX 43 H19 2 0.364324 0.207319 0.326955 11.00000 -1.20000 AFIX 0 C27 1 0.300115 0.247825 0.660117 11.00000 0.06005 0.06542 = 0.05033 0.00472 0.01191 -0.01281 AFIX 23 H271 2 0.288943 0.248618 0.702216 11.00000 -1.20000 H272 2 0.330509 0.263501 0.662411 11.00000 -1.20000 AFIX 0 C34 1 0.516009 0.222031 0.276606 11.00000 0.04475 0.06962 = 0.08399 -0.00394 -0.02290 0.01041 AFIX 43 H34 2 0.487400 0.206875 0.284923 11.00000 -1.20000 AFIX 0 C20 1 0.339758 0.269291 0.408162 11.00000 0.03861 0.06321 = 0.04171 -0.00015 -0.00710 -0.00009 C42 1 0.688712 0.109894 0.338913 11.00000 0.05142 0.06786 = 0.08867 -0.01525 0.02249 0.00834 AFIX 43 H42 2 0.672643 0.044292 0.352306 11.00000 -1.20000 AFIX 0 C49 1 0.583060 0.443720 0.415524 11.00000 0.04163 0.05382 = 0.06262 -0.00414 0.00864 0.00175 AFIX 43 H49 2 0.558732 0.414920 0.395713 11.00000 -1.20000 AFIX 0 C53 1 0.617892 0.057525 0.529652 11.00000 0.07081 0.05484 = 0.03915 -0.00151 -0.00978 0.00788 AFIX 43 H53 2 0.626794 0.066963 0.570656 11.00000 -1.20000 AFIX 0 C47 1 0.615425 0.595727 0.479350 11.00000 0.10179 0.04502 = 0.05379 -0.00700 0.01062 0.00053 AFIX 43 H47 2 0.613377 0.665924 0.502901 11.00000 -1.20000 AFIX 0 C23 1 0.234871 0.226377 0.549366 11.00000 0.03067 0.06808 = 0.07035 -0.00228 0.00499 -0.01453 AFIX 23 H231 2 0.221962 0.149449 0.559850 11.00000 -1.20000 H232 2 0.217701 0.263615 0.517091 11.00000 -1.20000 AFIX 0 C46 1 0.653656 0.537174 0.473531 11.00000 0.07320 0.04351 = 0.05045 -0.00398 -0.00900 -0.01150 AFIX 43 H46 2 0.678018 0.568992 0.491977 11.00000 -1.20000 AFIX 0 C73 1 0.146990 0.330958 0.893247 11.00000 0.05657 0.06547 = 0.03927 0.00007 -0.00593 0.00205 AFIX 43 H73 2 0.118022 0.325864 0.902152 11.00000 -1.20000 AFIX 0 C60 1 0.132270 0.140538 0.620981 11.00000 0.06285 0.04836 = 0.04002 -0.00028 0.00594 -0.00783 AFIX 43 H60 2 0.120374 0.142816 0.581345 11.00000 -1.20000 AFIX 0 C32 1 0.588780 0.244363 0.315844 11.00000 0.04274 0.03789 = 0.04143 -0.00209 -0.00402 0.00252 C63 1 0.054247 0.399175 0.832157 11.00000 0.05190 0.06379 = 0.05734 -0.00203 0.01698 0.00579 AFIX 43 H63 2 0.066836 0.473767 0.839691 11.00000 -1.20000 AFIX 0 C2 1 0.386906 0.419173 0.776648 11.00000 0.07867 0.07161 = 0.04913 -0.01656 0.00492 0.01194 AFIX 43 H2 2 0.381395 0.495768 0.792433 11.00000 -1.20000 AFIX 0 C54 1 0.596955 -0.046158 0.511782 11.00000 0.06693 0.04605 = 0.05658 0.00948 -0.00006 0.00198 AFIX 43 H54 2 0.591331 -0.106672 0.540639 11.00000 -1.20000 AFIX 0 C58 1 0.175608 0.046084 0.695265 11.00000 0.06198 0.04586 = 0.06688 0.00648 0.01455 0.01339 AFIX 43 H58 2 0.193585 -0.016640 0.707068 11.00000 -1.20000 AFIX 0 C78 1 0.090630 0.630480 0.676600 11.00000 0.05394 0.06116 = 0.08573 0.02336 0.00206 0.01703 AFIX 43 H78 2 0.065266 0.661265 0.660749 11.00000 -1.20000 AFIX 0 C77 1 0.127817 0.689653 0.665479 11.00000 0.07668 0.04167 = 0.05893 0.01281 0.00208 0.00292 AFIX 43 H77 2 0.128225 0.761702 0.643271 11.00000 -1.20000 AFIX 0 C65 1 -0.005838 0.269630 0.845011 11.00000 0.03799 0.11291 = 0.06823 -0.00394 0.01357 -0.00344 AFIX 43 H65 2 -0.033233 0.255508 0.859912 11.00000 -1.20000 AFIX 0 C39 1 0.737280 0.297595 0.295983 11.00000 0.04490 0.10657 = 0.06367 -0.00500 0.01412 -0.01050 AFIX 43 H39 2 0.753111 0.362471 0.281122 11.00000 -1.20000 AFIX 0 C38 1 0.697494 0.316913 0.321708 11.00000 0.04188 0.06578 = 0.05199 0.00063 0.00620 -0.00022 AFIX 43 H38 2 0.687328 0.395692 0.323577 11.00000 -1.20000 AFIX 0 C17 1 0.373803 0.482898 0.369266 11.00000 0.08434 0.08880 = 0.05165 0.02196 0.00572 -0.02176 AFIX 43 H17 2 0.384804 0.556928 0.356665 11.00000 -1.20000 AFIX 0 C76 1 0.164225 0.640391 0.687748 11.00000 0.05784 0.06787 = 0.08673 0.02852 -0.00447 -0.02214 AFIX 43 H76 2 0.190242 0.677870 0.680107 11.00000 -1.20000 AFIX 0 C70 1 0.232217 0.349131 0.873026 11.00000 0.04681 0.08742 = 0.07871 0.00976 -0.02135 0.00291 AFIX 43 H70 2 0.261244 0.356433 0.864982 11.00000 -1.20000 AFIX 0 C75 1 0.162929 0.534652 0.721790 11.00000 0.03914 0.06889 = 0.07897 0.02530 -0.01012 -0.00564 AFIX 43 H75 2 0.188621 0.503891 0.736489 11.00000 -1.20000 AFIX 0 C33 1 0.545608 0.222320 0.324526 11.00000 0.03957 0.06931 = 0.05561 0.00435 -0.00757 0.00474 AFIX 43 H33 2 0.536015 0.206897 0.364707 11.00000 -1.20000 AFIX 0 C3 1 0.374189 0.318294 0.807677 11.00000 0.06782 0.09970 = 0.04400 0.00224 0.01132 0.01117 AFIX 43 H3 2 0.358552 0.324734 0.844309 11.00000 -1.20000 AFIX 0 C48 1 0.580109 0.549458 0.449946 11.00000 0.05986 0.05557 = 0.08157 -0.00899 0.01312 0.01227 AFIX 43 H48 2 0.554077 0.589205 0.453121 11.00000 -1.20000 AFIX 0 C22 1 0.276170 0.166126 0.459849 11.00000 0.04771 0.05141 = 0.05928 -0.01257 -0.00289 -0.01400 AFIX 23 H221 2 0.259151 0.223898 0.436741 11.00000 -1.20000 H222 2 0.261614 0.088937 0.458150 11.00000 -1.20000 AFIX 0 C66 1 0.015554 0.181067 0.813039 11.00000 0.05285 0.08218 = 0.06939 -0.00133 0.00134 -0.02908 AFIX 43 H66 2 0.002868 0.106227 0.806583 11.00000 -1.20000 AFIX 0 C69 1 0.203419 0.348785 0.823797 11.00000 0.04759 0.08872 = 0.05308 0.01577 -0.00663 0.00476 AFIX 43 H69 2 0.214082 0.353839 0.783488 11.00000 -1.20000 AFIX 0 C40 1 0.753406 0.183121 0.292354 11.00000 0.04436 0.12185 = 0.08978 -0.02543 0.02136 0.00864 AFIX 43 H40 2 0.780419 0.169654 0.275887 11.00000 -1.20000 AFIX 0 C21 1 0.319480 0.153596 0.428234 11.00000 0.05618 0.06159 = 0.05045 -0.01398 -0.00302 -0.00478 AFIX 23 H211 2 0.338726 0.112871 0.456667 11.00000 -1.20000 H212 2 0.316172 0.102319 0.391957 11.00000 -1.20000 AFIX 0 C55 1 0.584591 -0.059036 0.451398 11.00000 0.06177 0.04009 = 0.05859 0.00112 -0.01403 -0.00917 AFIX 43 H55 2 0.570719 -0.128980 0.438626 11.00000 -1.20000 AFIX 0 C35 1 0.529206 0.244238 0.216891 11.00000 0.08219 0.05496 = 0.07162 -0.00672 -0.04471 0.01511 AFIX 43 H35 2 0.509653 0.244357 0.184344 11.00000 -1.20000 AFIX 0 C72 1 0.175682 0.327857 0.942309 11.00000 0.09715 0.08397 = 0.04458 0.00052 -0.01010 0.00435 AFIX 43 H72 2 0.165565 0.318022 0.982683 11.00000 -1.20000 AFIX 0 C36 1 0.571245 0.266130 0.205688 11.00000 0.09003 0.07532 = 0.04018 -0.00162 -0.01954 0.00448 AFIX 43 H36 2 0.580529 0.281955 0.165394 11.00000 -1.20000 AFIX 0 C7 1 0.464075 0.075054 0.673591 11.00000 0.09090 0.05274 = 0.07244 0.01196 0.00472 0.02609 AFIX 23 H701 2 0.484181 0.123573 0.697072 11.00000 -1.20000 H702 2 0.474752 -0.007115 0.672992 11.00000 -1.20000 AFIX 0 C16 1 0.352054 0.472279 0.424217 11.00000 0.05805 0.06376 = 0.04750 0.01687 -0.00827 -0.00770 AFIX 43 H16 2 0.348430 0.540777 0.448677 11.00000 -1.20000 AFIX 0 C71 1 0.218479 0.338965 0.932469 11.00000 0.07905 0.06830 = 0.07025 -0.00636 -0.03481 0.01337 AFIX 43 H71 2 0.237593 0.339529 0.965567 11.00000 -1.20000 AFIX 0 C18 1 0.378949 0.382640 0.333518 11.00000 0.07529 0.12337 = 0.04917 0.01796 0.01084 -0.01106 AFIX 43 H18 2 0.394309 0.387130 0.296560 11.00000 -1.20000 AFIX 0 C64 1 0.013358 0.378485 0.854776 11.00000 0.05110 0.08608 = 0.07181 -0.00372 0.01986 0.01226 AFIX 43 H64 2 -0.000893 0.438800 0.876545 11.00000 -1.20000 AFIX 0 C6 1 0.421652 0.076518 0.706865 11.00000 0.09727 0.05179 = 0.07038 0.01854 0.02027 -0.00113 AFIX 23 H601 2 0.400121 0.044669 0.678915 11.00000 -1.20000 H62 2 0.423368 0.022507 0.742313 11.00000 -1.20000 AFIX 0 C41 1 0.729295 0.088968 0.313237 11.00000 0.07503 0.08266 = 0.13079 -0.02716 0.03996 0.01907 AFIX 43 H41 2 0.739744 0.010585 0.310481 11.00000 -1.20000 AFIX 0 N10 4 0.242068 0.810926 0.588882 11.00000 0.11138 0.11814 = 0.10583 0.01903 0.00234 -0.00450 C101 1 0.274442 0.792135 0.608872 11.00000 0.11480 0.06746 = 0.07148 0.01650 0.00925 -0.01179 C102 1 0.316402 0.769152 0.634604 11.00000 0.12392 0.10568 = 0.12744 0.01877 -0.03790 0.00158 AFIX 137 H103 2 0.328512 0.699241 0.614991 11.00000 -1.50000 H104 2 0.314039 0.755281 0.678577 11.00000 -1.50000 H105 2 0.334440 0.837714 0.627285 11.00000 -1.50000 AFIX 0 HKLF 4 REM M-1 in Pna2(1) F.Belaj blue 291.19(18)K REM R1 = 0.0396 for 10349 Fo > 4sig(Fo) and 0.0572 for all 12818 data REM 907 parameters refined using 1 restraints END WGHT 0.0019 0.0000 REM Highest difference peak 0.313, deepest hole -0.261, 1-sigma level 0.042 Q1 1 0.4288 0.2195 0.6044 11.00000 0.05 0.28 Q2 1 0.4603 0.2190 0.6089 11.00000 0.05 0.26 Q3 1 0.2983 0.2789 0.5362 11.00000 0.05 0.25 Q4 1 0.2924 0.3640 0.5855 11.00000 0.05 0.23 Q5 1 0.3744 0.2271 0.5575 11.00000 0.05 0.22 Q6 1 0.0783 0.2736 0.6727 11.00000 0.05 0.22 Q7 1 0.4250 0.3756 0.6015 11.00000 0.05 0.22 Q8 1 0.3096 0.4622 0.5451 11.00000 0.05 0.22 Q9 1 0.5772 0.2309 0.5391 11.00000 0.05 0.21 Q10 1 0.3296 0.3603 0.4889 11.00000 0.05 0.20 Q11 1 0.4438 0.3934 0.5935 11.00000 0.05 0.20 Q12 1 0.3291 0.4440 0.5326 11.00000 0.05 0.20 Q13 1 0.3455 0.2757 0.6596 11.00000 0.05 0.19 Q14 1 0.4598 0.3787 0.6011 11.00000 0.05 0.19 Q15 1 0.3746 0.1192 0.5588 11.00000 0.05 0.19 Q16 1 0.3076 0.3055 0.5784 11.00000 0.05 0.19 Q17 1 0.4297 0.2960 0.6602 11.00000 0.05 0.19 Q18 1 0.4434 0.1085 0.5377 11.00000 0.05 0.18 Q19 1 0.3307 0.2920 0.5390 11.00000 0.05 0.18 Q20 1 0.1753 0.3024 0.6014 11.00000 0.05 0.18 ; _shelx_res_checksum 64733 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, 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 N3 N 0.46907(12) 0.2673(4) 0.51453(18) 0.0494(10) Uani 1 1 d . . . . . C28 C 0.27910(17) 0.4564(5) 0.6609(2) 0.0645(15) Uani 1 1 d . . . . . H281 H 0.2673 0.5210 0.6366 0.097 Uiso 1 1 calc R U . . . H282 H 0.3077 0.4765 0.6728 0.097 Uiso 1 1 calc R U . . . H283 H 0.2621 0.4444 0.6975 0.097 Uiso 1 1 calc R U . . . C10 C 0.43310(18) 0.0471(5) 0.5710(3) 0.0639(15) Uani 1 1 d . . . . . H101 H 0.4040 0.0710 0.5802 0.077 Uiso 1 1 calc R U . . . H102 H 0.4362 -0.0370 0.5827 0.077 Uiso 1 1 calc R U . . . C11 C 0.4405(2) 0.0586(6) 0.5032(3) 0.0741(17) Uani 1 1 d . . . . . H111 H 0.4184 0.0142 0.4815 0.089 Uiso 1 1 calc R U . . . H112 H 0.4676 0.0212 0.4932 0.089 Uiso 1 1 calc R U . . . C13 C 0.47512(19) 0.3793(5) 0.4791(3) 0.0776(18) Uani 1 1 d . . . . . H131 H 0.4917 0.4350 0.5033 0.116 Uiso 1 1 calc R U . . . H132 H 0.4478 0.4144 0.4699 0.116 Uiso 1 1 calc R U . . . H133 H 0.4898 0.3617 0.4409 0.116 Uiso 1 1 calc R U . . . C9 C 0.51092(15) 0.2075(5) 0.5274(3) 0.0656(14) Uani 1 1 d . . . . . H91 H 0.5322 0.2683 0.5372 0.079 Uiso 1 1 calc R U . . . H92 H 0.5203 0.1641 0.4907 0.079 Uiso 1 1 calc R U . . . C8 C 0.50661(15) 0.1189(5) 0.5826(3) 0.0659(16) Uani 1 1 d . . . . . H81 H 0.5134 0.0379 0.5686 0.079 Uiso 1 1 calc R U . . . H82 H 0.5269 0.1407 0.6148 0.079 Uiso 1 1 calc R U . . . C12 C 0.44085(18) 0.1846(5) 0.4795(2) 0.0650(16) Uani 1 1 d . . . . . H121 H 0.4498 0.1837 0.4363 0.078 Uiso 1 1 calc R U . . . H122 H 0.4120 0.2161 0.4808 0.078 Uiso 1 1 calc R U . . . N4 N 0.49879(12) 0.3786(4) 0.63665(19) 0.0533(10) Uani 1 1 d . . . . . N8 N 0.26176(13) 0.4794(4) 0.50477(19) 0.0574(11) Uani 1 1 d . . . . . C14 C 0.52190(15) 0.4518(5) 0.6512(2) 0.0521(12) Uani 1 1 d . . . . . C15 C 0.55137(17) 0.5443(5) 0.6706(3) 0.0796(18) Uani 1 1 d . . . . . H151 H 0.5381 0.5944 0.7015 0.119 Uiso 1 1 calc R U . . . H152 H 0.5592 0.5927 0.6354 0.119 Uiso 1 1 calc R U . . . H153 H 0.5764 0.5073 0.6879 0.119 Uiso 1 1 calc R U . . . C29 C 0.23627(16) 0.5412(4) 0.4869(3) 0.0574(13) Uani 1 1 d . . . . . C30 C 0.20232(18) 0.6193(5) 0.4647(3) 0.095(2) Uani 1 1 d . . . . . H301 H 0.2095 0.6493 0.4241 0.142 Uiso 1 1 calc R U . . . H302 H 0.1989 0.6859 0.4928 0.142 Uiso 1 1 calc R U . . . H303 H 0.1762 0.5744 0.4624 0.142 Uiso 1 1 calc R U . . . C81 C 0.4779(2) 0.7233(6) 0.5297(4) 0.0814(17) Uani 1 1 d . . . . . N9 N 0.5085(3) 0.7439(7) 0.5567(3) 0.125(3) Uani 1 1 d . . . . . C80 C 0.4402(3) 0.7015(6) 0.4965(3) 0.103(3) Uani 1 1 d . . . . . H801 H 0.4179 0.6792 0.5250 0.155 Uiso 1 1 calc R U . . . H802 H 0.4447 0.6371 0.4674 0.155 Uiso 1 1 calc R U . . . H803 H 0.4320 0.7732 0.4745 0.155 Uiso 1 1 calc R U . . . Ni1 Ni 0.44276(2) 0.29927(5) 0.60523(3) 0.03642(12) Uani 1 1 d . . . . . Ni2 Ni 0.31073(2) 0.36708(4) 0.53551(3) 0.03729(12) Uani 1 1 d . . . . . N6 N 0.27868(11) 0.2055(3) 0.52525(18) 0.0439(9) Uani 1 1 d . . . . . N5 N 0.33572(11) 0.3673(4) 0.44436(16) 0.0433(9) Uani 1 1 d . . . . . O1 O 0.37478(9) 0.3149(2) 0.56975(13) 0.0345(6) Uani 1 1 d . . . . . O2 O 0.41887(8) 0.4665(2) 0.58826(12) 0.0395(7) Uani 1 1 d . . . . . N2 N 0.46250(11) 0.1207(3) 0.60908(19) 0.0465(9) Uani 1 1 d . . . . . O3 O 0.35106(9) 0.5025(3) 0.56149(13) 0.0420(7) Uani 1 1 d . . . . . N1 N 0.41756(12) 0.2974(3) 0.69691(16) 0.0416(9) Uani 1 1 d . . . . . C44 C 0.62092(14) 0.3789(4) 0.40938(19) 0.0372(10) Uani 1 1 d . . . . . C62 C 0.07727(14) 0.3131(4) 0.79866(19) 0.0391(10) Uani 1 1 d . . . . . C31 C 0.38180(13) 0.4298(4) 0.57340(18) 0.0329(9) Uani 1 1 d . . . . . N7 N 0.27941(12) 0.3454(3) 0.62377(17) 0.0458(10) Uani 1 1 d . . . . . C25 C 0.30105(16) 0.1123(4) 0.5640(2) 0.0535(13) Uani 1 1 d . . . . . H251 H 0.2920 0.0328 0.5505 0.064 Uiso 1 1 calc R U . . . H252 H 0.3315 0.1184 0.5566 0.064 Uiso 1 1 calc R U . . . C67 C 0.05648(15) 0.2040(5) 0.7903(2) 0.0510(12) Uani 1 1 d . . . . . H67 H 0.0704 0.1432 0.7684 0.061 Uiso 1 1 calc R U . . . C56 C 0.13942(14) 0.2348(4) 0.7233(2) 0.0370(10) Uani 1 1 d . . . . . C61 C 0.12275(14) 0.2320(4) 0.6634(2) 0.0417(11) Uani 1 1 d . . . . . H61 H 0.1045 0.2937 0.6510 0.050 Uiso 1 1 calc R U . . . C74 C 0.12634(13) 0.4717(4) 0.73545(18) 0.0351(9) Uani 1 1 d . . . . . C43 C 0.67181(14) 0.2251(4) 0.34495(19) 0.0424(11) Uani 1 1 d . . . . . B2 B 0.12589(16) 0.3415(4) 0.7727(2) 0.0362(11) Uani 1 1 d . . . . . C52 C 0.62564(14) 0.1475(4) 0.4866(2) 0.0439(11) Uani 1 1 d . . . . . H52 H 0.6400 0.2163 0.4998 0.053 Uiso 1 1 calc R U . . . C51 C 0.61310(13) 0.1407(4) 0.42419(19) 0.0358(10) Uani 1 1 d . . . . . C26 C 0.29302(18) 0.1236(5) 0.6320(2) 0.0606(14) Uani 1 1 d . . . . . H261 H 0.3113 0.0667 0.6535 0.073 Uiso 1 1 calc R U . . . H262 H 0.2638 0.0999 0.6401 0.073 Uiso 1 1 calc R U . . . C59 C 0.15879(17) 0.0477(4) 0.6368(2) 0.0530(13) Uani 1 1 d . . . . . H59 H 0.1652 -0.0130 0.6084 0.064 Uiso 1 1 calc R U . . . B1 B 0.62383(16) 0.2482(4) 0.3736(2) 0.0350(11) Uani 1 1 d . . . . . C45 C 0.65599(15) 0.4307(4) 0.4402(2) 0.0450(11) Uani 1 1 d . . . . . H45 H 0.6821 0.3912 0.4380 0.054 Uiso 1 1 calc R U . . . C79 C 0.08994(15) 0.5249(5) 0.7112(2) 0.0539(13) Uani 1 1 d . . . . . H79 H 0.0638 0.4880 0.7185 0.065 Uiso 1 1 calc R U . . . C68 C 0.15935(14) 0.3412(4) 0.8318(2) 0.0406(10) Uani 1 1 d . . . . . C5 C 0.40718(16) 0.1982(4) 0.7295(2) 0.0482(11) Uani 1 1 d . . . . . C50 C 0.59275(15) 0.0325(4) 0.4090(2) 0.0449(11) Uani 1 1 d . . . . . H50 H 0.5842 0.0211 0.3680 0.054 Uiso 1 1 calc R U . . . C37 C 0.60023(18) 0.2648(4) 0.2546(2) 0.0533(13) Uani 1 1 d . . . . . H37 H 0.6289 0.2783 0.2456 0.064 Uiso 1 1 calc R U . . . C1 C 0.40805(16) 0.4043(4) 0.7215(2) 0.0495(12) Uani 1 1 d . . . . . H1 H 0.4163 0.4731 0.6998 0.059 Uiso 1 1 calc R U . . . C24 C 0.23503(13) 0.3079(5) 0.6072(3) 0.0571(12) Uani 1 1 d . . . . . H241 H 0.2179 0.3790 0.5992 0.069 Uiso 1 1 calc R U . . . H242 H 0.2224 0.2648 0.6419 0.069 Uiso 1 1 calc R U . . . C4 C 0.38458(17) 0.2084(5) 0.7846(2) 0.0629(14) Uani 1 1 d . . . . . H4 H 0.3765 0.1391 0.8059 0.076 Uiso 1 1 calc R U . . . C57 C 0.16610(16) 0.1377(4) 0.7376(2) 0.0517(12) Uani 1 1 d . . . . . H57 H 0.1781 0.1340 0.7771 0.062 Uiso 1 1 calc R U . . . C19 C 0.36160(18) 0.2756(6) 0.3518(2) 0.0643(15) Uani 1 1 d . . . . . H19 H 0.3643 0.2073 0.3270 0.077 Uiso 1 1 calc R U . . . C27 C 0.30012(18) 0.2478(5) 0.6601(2) 0.0586(14) Uani 1 1 d . . . . . H271 H 0.2889 0.2486 0.7022 0.070 Uiso 1 1 calc R U . . . H272 H 0.3305 0.2635 0.6624 0.070 Uiso 1 1 calc R U . . . C34 C 0.51601(17) 0.2220(5) 0.2766(3) 0.0661(15) Uani 1 1 d . . . . . H34 H 0.4874 0.2069 0.2849 0.079 Uiso 1 1 calc R U . . . C20 C 0.33976(15) 0.2693(5) 0.4082(2) 0.0478(12) Uani 1 1 d . . . . . C42 C 0.68871(17) 0.1099(5) 0.3389(3) 0.0693(16) Uani 1 1 d . . . . . H42 H 0.6726 0.0443 0.3523 0.083 Uiso 1 1 calc R U . . . C49 C 0.58306(16) 0.4437(4) 0.4155(2) 0.0527(12) Uani 1 1 d . . . . . H49 H 0.5587 0.4149 0.3957 0.063 Uiso 1 1 calc R U . . . C53 C 0.61789(16) 0.0575(4) 0.5297(2) 0.0549(12) Uani 1 1 d . . . . . H53 H 0.6268 0.0670 0.5707 0.066 Uiso 1 1 calc R U . . . C47 C 0.6154(2) 0.5957(5) 0.4793(2) 0.0669(16) Uani 1 1 d . . . . . H47 H 0.6134 0.6659 0.5029 0.080 Uiso 1 1 calc R U . . . C23 C 0.23487(14) 0.2264(5) 0.5494(2) 0.0564(13) Uani 1 1 d . . . . . H231 H 0.2220 0.1494 0.5598 0.068 Uiso 1 1 calc R U . . . H232 H 0.2177 0.2636 0.5171 0.068 Uiso 1 1 calc R U . . . C46 C 0.65366(18) 0.5372(4) 0.4735(2) 0.0557(13) Uani 1 1 d . . . . . H46 H 0.6780 0.5690 0.4920 0.067 Uiso 1 1 calc R U . . . C73 C 0.14699(17) 0.3310(4) 0.8932(2) 0.0538(13) Uani 1 1 d . . . . . H73 H 0.1180 0.3259 0.9022 0.065 Uiso 1 1 calc R U . . . C60 C 0.13227(16) 0.1405(4) 0.6210(2) 0.0504(12) Uani 1 1 d . . . . . H60 H 0.1204 0.1428 0.5813 0.060 Uiso 1 1 calc R U . . . C32 C 0.58878(14) 0.2444(4) 0.3158(2) 0.0407(10) Uani 1 1 d . . . . . C63 C 0.05425(16) 0.3992(5) 0.8322(2) 0.0577(13) Uani 1 1 d . . . . . H63 H 0.0668 0.4738 0.8397 0.069 Uiso 1 1 calc R U . . . C2 C 0.38691(19) 0.4192(5) 0.7766(2) 0.0665(15) Uani 1 1 d . . . . . H2 H 0.3814 0.4958 0.7924 0.080 Uiso 1 1 calc R U . . . C54 C 0.59696(17) -0.0462(5) 0.5118(2) 0.0565(13) Uani 1 1 d . . . . . H54 H 0.5913 -0.1067 0.5406 0.068 Uiso 1 1 calc R U . . . C58 C 0.17561(17) 0.0461(4) 0.6953(2) 0.0582(14) Uani 1 1 d . . . . . H58 H 0.1936 -0.0166 0.7071 0.070 Uiso 1 1 calc R U . . . C78 C 0.09063(17) 0.6305(5) 0.6766(3) 0.0669(15) Uani 1 1 d . . . . . H78 H 0.0653 0.6613 0.6607 0.080 Uiso 1 1 calc R U . . . C77 C 0.12782(18) 0.6897(4) 0.6655(2) 0.0591(14) Uani 1 1 d . . . . . H77 H 0.1282 0.7617 0.6433 0.071 Uiso 1 1 calc R U . . . C65 C -0.00584(18) 0.2696(6) 0.8450(3) 0.0730(18) Uani 1 1 d . . . . . H65 H -0.0332 0.2555 0.8599 0.088 Uiso 1 1 calc R U . . . C39 C 0.73728(17) 0.2976(6) 0.2960(3) 0.0717(17) Uani 1 1 d . . . . . H39 H 0.7531 0.3625 0.2811 0.086 Uiso 1 1 calc R U . . . C38 C 0.69749(15) 0.3169(5) 0.3217(2) 0.0532(12) Uani 1 1 d . . . . . H38 H 0.6873 0.3957 0.3236 0.064 Uiso 1 1 calc R U . . . C17 C 0.37380(19) 0.4829(6) 0.3693(3) 0.0749(17) Uani 1 1 d . . . . . H17 H 0.3848 0.5569 0.3567 0.090 Uiso 1 1 calc R U . . . C76 C 0.16422(18) 0.6404(5) 0.6877(3) 0.0708(16) Uani 1 1 d . . . . . H76 H 0.1902 0.6779 0.6801 0.085 Uiso 1 1 calc R U . . . C70 C 0.23222(18) 0.3491(5) 0.8730(3) 0.0710(16) Uani 1 1 d . . . . . H70 H 0.2612 0.3564 0.8650 0.085 Uiso 1 1 calc R U . . . C75 C 0.16293(16) 0.5347(5) 0.7218(2) 0.0623(15) Uani 1 1 d . . . . . H75 H 0.1886 0.5039 0.7365 0.075 Uiso 1 1 calc R U . . . C33 C 0.54561(15) 0.2223(5) 0.3245(2) 0.0548(13) Uani 1 1 d . . . . . H33 H 0.5360 0.2069 0.3647 0.066 Uiso 1 1 calc R U . . . C3 C 0.37419(19) 0.3183(6) 0.8077(2) 0.0705(17) Uani 1 1 d . . . . . H3 H 0.3586 0.3247 0.8443 0.085 Uiso 1 1 calc R U . . . C48 C 0.58011(18) 0.5495(5) 0.4499(3) 0.0657(15) Uani 1 1 d . . . . . H48 H 0.5541 0.5892 0.4531 0.079 Uiso 1 1 calc R U . . . C22 C 0.27617(15) 0.1661(4) 0.4598(2) 0.0528(12) Uani 1 1 d . . . . . H221 H 0.2592 0.2239 0.4367 0.063 Uiso 1 1 calc R U . . . H222 H 0.2616 0.0889 0.4582 0.063 Uiso 1 1 calc R U . . . C66 C 0.01555(18) 0.1811(6) 0.8130(3) 0.0681(16) Uani 1 1 d . . . . . H66 H 0.0029 0.1062 0.8066 0.082 Uiso 1 1 calc R U . . . C69 C 0.20342(17) 0.3488(5) 0.8238(2) 0.0631(15) Uani 1 1 d . . . . . H69 H 0.2141 0.3538 0.7835 0.076 Uiso 1 1 calc R U . . . C40 C 0.75341(19) 0.1831(7) 0.2924(3) 0.085(2) Uani 1 1 d . . . . . H40 H 0.7804 0.1697 0.2759 0.102 Uiso 1 1 calc R U . . . C21 C 0.31948(16) 0.1536(5) 0.4282(2) 0.0561(13) Uani 1 1 d . . . . . H211 H 0.3387 0.1129 0.4567 0.067 Uiso 1 1 calc R U . . . H212 H 0.3162 0.1023 0.3920 0.067 Uiso 1 1 calc R U . . . C55 C 0.58459(16) -0.0590(4) 0.4514(2) 0.0535(13) Uani 1 1 d . . . . . H55 H 0.5707 -0.1290 0.4386 0.064 Uiso 1 1 calc R U . . . C35 C 0.5292(2) 0.2442(5) 0.2169(3) 0.0696(17) Uani 1 1 d . . . . . H35 H 0.5097 0.2444 0.1843 0.084 Uiso 1 1 calc R U . . . C72 C 0.1757(2) 0.3279(5) 0.9423(3) 0.0752(18) Uani 1 1 d . . . . . H72 H 0.1656 0.3180 0.9827 0.090 Uiso 1 1 calc R U . . . C36 C 0.5712(2) 0.2661(5) 0.2057(2) 0.0685(17) Uani 1 1 d . . . . . H36 H 0.5805 0.2820 0.1654 0.082 Uiso 1 1 calc R U . . . C7 C 0.46407(19) 0.0751(5) 0.6736(3) 0.0720(17) Uani 1 1 d . . . . . H701 H 0.4842 0.1236 0.6971 0.086 Uiso 1 1 calc R U . . . H702 H 0.4748 -0.0071 0.6730 0.086 Uiso 1 1 calc R U . . . C16 C 0.35205(16) 0.4723(5) 0.4242(2) 0.0564(13) Uani 1 1 d . . . . . H16 H 0.3484 0.5408 0.4487 0.068 Uiso 1 1 calc R U . . . C71 C 0.2185(2) 0.3390(5) 0.9325(3) 0.0725(18) Uani 1 1 d . . . . . H71 H 0.2376 0.3395 0.9656 0.087 Uiso 1 1 calc R U . . . C18 C 0.3789(2) 0.3826(7) 0.3335(3) 0.083(2) Uani 1 1 d . . . . . H18 H 0.3943 0.3871 0.2966 0.099 Uiso 1 1 calc R U . . . C64 C 0.01336(18) 0.3785(6) 0.8548(3) 0.0697(16) Uani 1 1 d . . . . . H64 H -0.0009 0.4388 0.8765 0.084 Uiso 1 1 calc R U . . . C6 C 0.4217(2) 0.0765(5) 0.7069(3) 0.0731(18) Uani 1 1 d . . . . . H601 H 0.4001 0.0447 0.6789 0.088 Uiso 1 1 calc R U . . . H62 H 0.4234 0.0225 0.7423 0.088 Uiso 1 1 calc R U . . . C41 C 0.7293(2) 0.0890(7) 0.3132(3) 0.096(2) Uani 1 1 d . . . . . H41 H 0.7397 0.0106 0.3105 0.115 Uiso 1 1 calc R U . . . N10 N 0.2421(2) 0.8109(7) 0.5889(3) 0.112(2) Uani 1 1 d . . . . . C101 C 0.2744(3) 0.7921(6) 0.6089(4) 0.0846(18) Uani 1 1 d . . . . . C102 C 0.3164(3) 0.7692(7) 0.6346(4) 0.119(3) Uani 1 1 d . . . . . H103 H 0.3285 0.6992 0.6150 0.179 Uiso 1 1 calc R U . . . H104 H 0.3140 0.7553 0.6786 0.179 Uiso 1 1 calc R U . . . H105 H 0.3344 0.8377 0.6273 0.179 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 N3 0.037(2) 0.062(3) 0.049(3) 0.0007(19) 0.0067(18) 0.0039(19) C28 0.060(4) 0.072(4) 0.061(3) -0.020(3) 0.018(3) -0.003(3) C10 0.067(4) 0.047(3) 0.078(4) -0.016(3) -0.001(3) 0.006(3) C11 0.070(4) 0.074(4) 0.079(4) -0.025(3) -0.012(3) 0.007(3) C13 0.082(5) 0.086(4) 0.066(4) 0.019(3) 0.032(3) 0.015(3) C9 0.040(3) 0.087(4) 0.070(4) -0.008(3) 0.013(3) 0.013(3) C8 0.037(3) 0.074(4) 0.087(4) -0.012(3) -0.007(3) 0.021(3) C12 0.059(4) 0.084(4) 0.052(3) -0.018(3) 0.004(3) 0.014(3) N4 0.039(2) 0.059(3) 0.062(3) -0.002(2) -0.0059(19) -0.009(2) N8 0.039(2) 0.062(3) 0.071(3) 0.008(2) -0.007(2) 0.003(2) C14 0.036(3) 0.051(3) 0.068(3) 0.000(3) -0.005(2) 0.004(2) C15 0.047(3) 0.055(3) 0.137(5) -0.013(3) -0.016(3) 0.001(3) C29 0.042(3) 0.046(3) 0.084(4) 0.012(3) -0.004(3) -0.008(2) C30 0.053(4) 0.061(4) 0.171(7) 0.038(4) -0.031(4) 0.003(3) C81 0.087(5) 0.072(4) 0.085(5) -0.001(4) -0.003(4) 0.006(4) N9 0.116(6) 0.157(7) 0.104(6) -0.012(4) -0.004(4) -0.010(5) C80 0.117(7) 0.076(5) 0.117(6) 0.026(4) -0.030(5) -0.012(5) Ni1 0.0308(3) 0.0375(3) 0.0410(3) -0.0011(3) -0.0005(3) -0.0001(2) Ni2 0.0290(2) 0.0383(3) 0.0445(3) 0.0010(3) 0.0001(3) -0.0010(2) N6 0.0309(19) 0.046(2) 0.055(2) -0.0013(19) -0.0015(17) -0.0089(15) N5 0.038(2) 0.052(2) 0.039(2) 0.0045(18) -0.0046(17) -0.0064(18) O1 0.0334(15) 0.0296(16) 0.0405(14) -0.0024(12) 0.0030(11) -0.0013(11) O2 0.0347(16) 0.0333(15) 0.0507(19) 0.0016(12) -0.0023(13) -0.0077(12) N2 0.042(2) 0.044(2) 0.053(2) -0.003(2) -0.001(2) 0.0086(16) O3 0.0376(17) 0.0351(16) 0.0532(18) 0.0017(13) -0.0016(13) 0.0049(13) N1 0.042(2) 0.044(2) 0.039(2) -0.0015(17) -0.0062(17) 0.0006(17) C44 0.041(2) 0.036(2) 0.034(2) 0.0025(18) 0.0022(19) 0.0002(19) C62 0.034(2) 0.049(3) 0.034(2) 0.006(2) 0.0005(19) 0.002(2) C31 0.035(2) 0.036(2) 0.028(2) -0.0011(17) 0.0034(17) -0.0034(18) N7 0.036(2) 0.053(2) 0.048(2) -0.0017(18) 0.0088(17) -0.0038(17) C25 0.050(3) 0.037(3) 0.073(4) 0.002(2) 0.001(2) -0.006(2) C67 0.040(3) 0.064(3) 0.050(3) -0.002(2) 0.003(2) -0.004(2) C56 0.035(2) 0.037(2) 0.039(3) 0.0070(19) 0.0056(19) -0.0006(18) C61 0.044(3) 0.039(2) 0.042(3) 0.009(2) -0.002(2) 0.001(2) C74 0.035(2) 0.038(2) 0.032(2) -0.0039(18) 0.0016(18) -0.0016(19) C43 0.034(2) 0.056(3) 0.037(3) -0.004(2) -0.0014(19) 0.003(2) B2 0.031(3) 0.037(3) 0.040(3) 0.000(2) 0.001(2) 0.001(2) C52 0.046(3) 0.043(3) 0.042(3) -0.007(2) -0.005(2) 0.004(2) C51 0.029(2) 0.040(2) 0.039(2) -0.0075(19) -0.0004(18) 0.0030(19) C26 0.057(3) 0.062(3) 0.063(4) 0.020(3) 0.003(3) -0.009(3) C59 0.069(4) 0.042(3) 0.048(3) -0.003(2) 0.019(3) -0.005(3) B1 0.031(3) 0.041(3) 0.033(3) -0.003(2) -0.003(2) 0.002(2) C45 0.045(3) 0.044(3) 0.046(3) 0.001(2) -0.006(2) 0.000(2) C79 0.034(3) 0.059(3) 0.068(3) 0.013(3) 0.002(2) 0.006(2) C68 0.040(3) 0.039(2) 0.043(3) 0.0036(19) -0.002(2) -0.0001(19) C5 0.051(3) 0.049(3) 0.044(3) 0.007(2) -0.001(2) -0.002(2) C50 0.050(3) 0.044(3) 0.041(3) -0.005(2) -0.011(2) 0.001(2) C37 0.062(3) 0.056(3) 0.042(3) -0.005(2) -0.005(2) -0.003(3) C1 0.058(3) 0.047(3) 0.043(3) -0.005(2) -0.001(2) -0.001(2) C24 0.033(2) 0.069(3) 0.070(3) 0.001(3) 0.012(3) -0.005(2) C4 0.067(4) 0.072(4) 0.050(3) 0.022(3) 0.005(3) -0.001(3) C57 0.056(3) 0.056(3) 0.043(3) 0.009(2) 0.005(2) 0.012(2) C19 0.062(4) 0.087(4) 0.044(3) -0.006(3) 0.004(3) -0.003(3) C27 0.060(3) 0.065(4) 0.050(3) 0.005(3) 0.012(3) -0.013(3) C34 0.045(3) 0.070(4) 0.084(4) -0.004(3) -0.023(3) 0.010(3) C20 0.039(3) 0.063(3) 0.042(3) 0.000(2) -0.007(2) 0.000(2) C42 0.051(3) 0.068(4) 0.089(4) -0.015(3) 0.022(3) 0.008(3) C49 0.042(3) 0.054(3) 0.063(3) -0.004(2) 0.009(2) 0.002(2) C53 0.071(3) 0.055(3) 0.039(3) -0.002(2) -0.010(3) 0.008(2) C47 0.102(5) 0.045(3) 0.054(3) -0.007(2) 0.011(3) 0.001(3) C23 0.031(2) 0.068(3) 0.070(4) -0.002(3) 0.005(2) -0.015(2) C46 0.073(4) 0.044(3) 0.050(3) -0.004(2) -0.009(3) -0.011(3) C73 0.057(3) 0.065(3) 0.039(3) 0.000(2) -0.006(2) 0.002(3) C60 0.063(3) 0.048(3) 0.040(3) 0.000(2) 0.006(2) -0.008(2) C32 0.043(3) 0.038(2) 0.041(3) -0.0021(19) -0.004(2) 0.003(2) C63 0.052(3) 0.064(3) 0.057(3) -0.002(3) 0.017(3) 0.006(3) C2 0.079(4) 0.072(4) 0.049(3) -0.017(3) 0.005(3) 0.012(3) C54 0.067(4) 0.046(3) 0.057(3) 0.009(2) 0.000(3) 0.002(3) C58 0.062(3) 0.046(3) 0.067(4) 0.006(3) 0.015(3) 0.013(2) C78 0.054(3) 0.061(3) 0.086(4) 0.023(3) 0.002(3) 0.017(3) C77 0.077(4) 0.042(3) 0.059(3) 0.013(2) 0.002(3) 0.003(3) C65 0.038(3) 0.113(5) 0.068(4) -0.004(4) 0.014(3) -0.003(3) C39 0.045(3) 0.107(5) 0.064(4) -0.005(3) 0.014(3) -0.011(3) C38 0.042(3) 0.066(3) 0.052(3) 0.001(2) 0.006(2) 0.000(2) C17 0.084(4) 0.089(5) 0.052(4) 0.022(3) 0.006(3) -0.022(4) C76 0.058(4) 0.068(4) 0.087(4) 0.029(3) -0.004(3) -0.022(3) C70 0.047(3) 0.087(4) 0.079(4) 0.010(3) -0.021(3) 0.003(3) C75 0.039(3) 0.069(4) 0.079(4) 0.025(3) -0.010(3) -0.006(3) C33 0.040(3) 0.069(3) 0.056(3) 0.004(3) -0.008(2) 0.005(2) C3 0.068(4) 0.100(5) 0.044(3) 0.002(3) 0.011(3) 0.011(4) C48 0.060(4) 0.056(3) 0.082(4) -0.009(3) 0.013(3) 0.012(3) C22 0.048(3) 0.051(3) 0.059(3) -0.013(2) -0.003(2) -0.014(2) C66 0.053(3) 0.082(4) 0.069(4) -0.001(3) 0.001(3) -0.029(3) C69 0.048(3) 0.089(4) 0.053(3) 0.016(3) -0.007(2) 0.005(3) C40 0.044(4) 0.122(6) 0.090(5) -0.025(4) 0.021(3) 0.009(4) C21 0.056(3) 0.062(3) 0.050(3) -0.014(2) -0.003(2) -0.005(3) C55 0.062(3) 0.040(3) 0.059(3) 0.001(2) -0.014(3) -0.009(2) C35 0.082(5) 0.055(3) 0.072(4) -0.007(3) -0.045(3) 0.015(3) C72 0.097(5) 0.084(5) 0.045(3) 0.001(3) -0.010(3) 0.004(4) C36 0.090(5) 0.075(4) 0.040(3) -0.002(3) -0.020(3) 0.004(3) C7 0.091(5) 0.053(3) 0.072(4) 0.012(3) 0.005(3) 0.026(3) C16 0.058(3) 0.064(3) 0.048(3) 0.017(2) -0.008(2) -0.008(3) C71 0.079(5) 0.068(4) 0.070(4) -0.006(3) -0.035(3) 0.013(3) C18 0.075(4) 0.123(6) 0.049(4) 0.018(4) 0.011(3) -0.011(4) C64 0.051(3) 0.086(5) 0.072(4) -0.004(3) 0.020(3) 0.012(3) C6 0.097(5) 0.052(3) 0.070(4) 0.019(3) 0.020(3) -0.001(3) C41 0.075(5) 0.083(5) 0.131(6) -0.027(4) 0.040(4) 0.019(4) N10 0.111(6) 0.118(5) 0.106(6) 0.019(4) 0.002(4) -0.005(5) C101 0.115(6) 0.067(4) 0.071(4) 0.016(4) 0.009(5) -0.012(4) C102 0.124(7) 0.106(6) 0.127(7) 0.019(5) -0.038(5) 0.002(5) 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 N3 C12 109.7(4) . . ? C13 N3 C9 110.9(4) . . ? C12 N3 C9 110.2(4) . . ? C13 N3 Ni1 112.4(3) . . ? C12 N3 Ni1 109.5(3) . . ? C9 N3 Ni1 104.0(3) . . ? N7 C28 H281 109.5 . . ? N7 C28 H282 109.5 . . ? H281 C28 H282 109.5 . . ? N7 C28 H283 109.5 . . ? H281 C28 H283 109.5 . . ? H282 C28 H283 109.5 . . ? N2 C10 C11 113.6(5) . . ? N2 C10 H101 108.9 . . ? C11 C10 H101 108.9 . . ? N2 C10 H102 108.9 . . ? C11 C10 H102 108.9 . . ? H101 C10 H102 107.7 . . ? C10 C11 C12 114.8(5) . . ? C10 C11 H111 108.6 . . ? C12 C11 H111 108.6 . . ? C10 C11 H112 108.6 . . ? C12 C11 H112 108.6 . . ? H111 C11 H112 107.5 . . ? N3 C13 H131 109.5 . . ? N3 C13 H132 109.5 . . ? H131 C13 H132 109.5 . . ? N3 C13 H133 109.5 . . ? H131 C13 H133 109.5 . . ? H132 C13 H133 109.5 . . ? N3 C9 C8 110.3(4) . . ? N3 C9 H91 109.6 . . ? C8 C9 H91 109.6 . . ? N3 C9 H92 109.6 . . ? C8 C9 H92 109.6 . . ? H91 C9 H92 108.1 . . ? N2 C8 C9 111.4(4) . . ? N2 C8 H81 109.4 . . ? C9 C8 H81 109.4 . . ? N2 C8 H82 109.4 . . ? C9 C8 H82 109.4 . . ? H81 C8 H82 108.0 . . ? N3 C12 C11 114.3(5) . . ? N3 C12 H121 108.7 . . ? C11 C12 H121 108.7 . . ? N3 C12 H122 108.7 . . ? C11 C12 H122 108.7 . . ? H121 C12 H122 107.6 . . ? C14 N4 Ni1 159.2(4) . . ? C29 N8 Ni2 177.8(5) . . ? N4 C14 C15 179.2(6) . . ? C14 C15 H151 109.5 . . ? C14 C15 H152 109.5 . . ? H151 C15 H152 109.5 . . ? C14 C15 H153 109.5 . . ? H151 C15 H153 109.5 . . ? H152 C15 H153 109.5 . . ? N8 C29 C30 178.4(6) . . ? C29 C30 H301 109.5 . . ? C29 C30 H302 109.5 . . ? H301 C30 H302 109.5 . . ? C29 C30 H303 109.5 . . ? H301 C30 H303 109.5 . . ? H302 C30 H303 109.5 . . ? N9 C81 C80 178.5(8) . . ? C81 C80 H801 109.5 . . ? C81 C80 H802 109.5 . . ? H801 C80 H802 109.5 . . ? C81 C80 H803 109.5 . . ? H801 C80 H803 109.5 . . ? H802 C80 H803 109.5 . . ? O2 Ni1 N2 170.73(13) . . ? O2 Ni1 N4 89.11(14) . . ? N2 Ni1 N4 97.94(15) . . ? O2 Ni1 N1 92.19(12) . . ? N2 Ni1 N1 93.70(15) . . ? N4 Ni1 N1 91.00(15) . . ? O2 Ni1 N3 97.44(13) . . ? N2 Ni1 N3 76.35(15) . . ? N4 Ni1 N3 92.29(16) . . ? N1 Ni1 N3 169.86(15) . . ? O2 Ni1 O1 61.58(10) . . ? N2 Ni1 O1 111.48(12) . . ? N4 Ni1 O1 150.57(14) . . ? N1 Ni1 O1 87.86(12) . . ? N3 Ni1 O1 93.94(13) . . ? O2 Ni1 C31 30.56(12) . . ? N2 Ni1 C31 142.46(14) . . ? N4 Ni1 C31 119.51(15) . . ? N1 Ni1 C31 88.55(13) . . ? N3 Ni1 C31 98.14(14) . . ? O1 Ni1 C31 31.08(11) . . ? O3 Ni2 N6 165.59(13) . . ? O3 Ni2 N8 96.00(14) . . ? N6 Ni2 N8 97.18(15) . . ? O3 Ni2 N5 91.32(13) . . ? N6 Ni2 N5 94.73(15) . . ? N8 Ni2 N5 88.79(15) . . ? O3 Ni2 N7 97.13(13) . . ? N6 Ni2 N7 76.99(14) . . ? N8 Ni2 N7 90.55(15) . . ? N5 Ni2 N7 171.55(15) . . ? O3 Ni2 O1 62.55(10) . . ? N6 Ni2 O1 104.51(12) . . ? N8 Ni2 O1 158.28(14) . . ? N5 Ni2 O1 88.38(12) . . ? N7 Ni2 O1 95.29(13) . . ? O3 Ni2 C31 31.17(12) . . ? N6 Ni2 C31 135.86(14) . . ? N8 Ni2 C31 126.94(16) . . ? N5 Ni2 C31 88.31(13) . . ? N7 Ni2 C31 98.79(13) . . ? O1 Ni2 C31 31.44(11) . . ? C22 N6 C23 109.2(3) . . ? C22 N6 C25 110.5(4) . . ? C23 N6 C25 110.2(4) . . ? C22 N6 Ni2 112.6(3) . . ? C23 N6 Ni2 106.1(3) . . ? C25 N6 Ni2 108.1(3) . . ? C20 N5 C16 118.6(4) . . ? C20 N5 Ni2 124.9(3) . . ? C16 N5 Ni2 116.2(3) . . ? C31 O1 Ni2 85.3(2) . . ? C31 O1 Ni1 84.0(2) . . ? Ni2 O1 Ni1 169.25(14) . . ? C31 O2 Ni1 95.2(2) . . ? C7 N2 C10 110.6(4) . . ? C7 N2 C8 108.8(4) . . ? C10 N2 C8 111.0(4) . . ? C7 N2 Ni1 112.0(3) . . ? C10 N2 Ni1 108.5(3) . . ? C8 N2 Ni1 105.8(3) . . ? C31 O3 Ni2 93.4(2) . . ? C1 N1 C5 117.8(4) . . ? C1 N1 Ni1 116.3(3) . . ? C5 N1 Ni1 125.6(3) . . ? C49 C44 C45 114.3(4) . . ? C49 C44 B1 123.1(4) . . ? C45 C44 B1 122.5(4) . . ? C67 C62 C63 114.8(4) . . ? C67 C62 B2 123.8(4) . . ? C63 C62 B2 121.4(4) . . ? O2 C31 O3 122.4(4) . . ? O2 C31 O1 119.0(4) . . ? O3 C31 O1 118.6(4) . . ? O2 C31 Ni2 174.9(3) . . ? O3 C31 Ni2 55.5(2) . . ? O1 C31 Ni2 63.3(2) . . ? O2 C31 Ni1 54.3(2) . . ? O3 C31 Ni1 174.8(3) . . ? O1 C31 Ni1 64.9(2) . . ? Ni2 C31 Ni1 128.21(17) . . ? C28 N7 C27 109.2(4) . . ? C28 N7 C24 110.9(4) . . ? C27 N7 C24 109.3(4) . . ? C28 N7 Ni2 112.9(3) . . ? C27 N7 Ni2 110.2(3) . . ? C24 N7 Ni2 104.2(3) . . ? C26 C25 N6 114.0(4) . . ? C26 C25 H251 108.7 . . ? N6 C25 H251 108.7 . . ? C26 C25 H252 108.7 . . ? N6 C25 H252 108.7 . . ? H251 C25 H252 107.6 . . ? C62 C67 C66 123.0(5) . . ? C62 C67 H67 118.5 . . ? C66 C67 H67 118.5 . . ? C61 C56 C57 114.3(4) . . ? C61 C56 B2 121.1(4) . . ? C57 C56 B2 124.5(4) . . ? C56 C61 C60 122.7(4) . . ? C56 C61 H61 118.6 . . ? C60 C61 H61 118.6 . . ? C75 C74 C79 113.1(4) . . ? C75 C74 B2 123.7(4) . . ? C79 C74 B2 123.1(4) . . ? C42 C43 C38 114.7(4) . . ? C42 C43 B1 121.8(4) . . ? C38 C43 B1 123.4(4) . . ? C56 B2 C68 109.4(4) . . ? C56 B2 C74 108.2(4) . . ? C68 B2 C74 111.7(4) . . ? C56 B2 C62 108.6(4) . . ? C68 B2 C62 109.1(4) . . ? C74 B2 C62 109.7(3) . . ? C53 C52 C51 123.6(4) . . ? C53 C52 H52 118.2 . . ? C51 C52 H52 118.2 . . ? C50 C51 C52 113.5(4) . . ? C50 C51 B1 124.0(4) . . ? C52 C51 B1 122.4(4) . . ? C25 C26 C27 116.3(4) . . ? C25 C26 H261 108.2 . . ? C27 C26 H261 108.2 . . ? C25 C26 H262 108.2 . . ? C27 C26 H262 108.2 . . ? H261 C26 H262 107.4 . . ? C58 C59 C60 118.3(4) . . ? C58 C59 H59 120.8 . . ? C60 C59 H59 120.8 . . ? C44 B1 C43 111.3(4) . . ? C44 B1 C51 108.5(4) . . ? C43 B1 C51 108.7(3) . . ? C44 B1 C32 109.6(3) . . ? C43 B1 C32 108.8(4) . . ? C51 B1 C32 109.9(3) . . ? C46 C45 C44 123.4(5) . . ? C46 C45 H45 118.3 . . ? C44 C45 H45 118.3 . . ? C74 C79 C78 123.2(5) . . ? C74 C79 H79 118.4 . . ? C78 C79 H79 118.4 . . ? C73 C68 C69 113.6(4) . . ? C73 C68 B2 123.9(4) . . ? C69 C68 B2 122.4(4) . . ? N1 C5 C4 120.2(5) . . ? N1 C5 C6 119.5(4) . . ? C4 C5 C6 120.3(5) . . ? C55 C50 C51 123.9(4) . . ? C55 C50 H50 118.0 . . ? C51 C50 H50 118.0 . . ? C32 C37 C36 123.5(5) . . ? C32 C37 H37 118.3 . . ? C36 C37 H37 118.3 . . ? N1 C1 C2 124.1(5) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? N7 C24 C23 111.1(4) . . ? N7 C24 H241 109.4 . . ? C23 C24 H241 109.4 . . ? N7 C24 H242 109.4 . . ? C23 C24 H242 109.4 . . ? H241 C24 H242 108.0 . . ? C3 C4 C5 120.7(5) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C58 C57 C56 123.0(5) . . ? C58 C57 H57 118.5 . . ? C56 C57 H57 118.5 . . ? C18 C19 C20 119.4(6) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? N7 C27 C26 112.7(4) . . ? N7 C27 H271 109.0 . . ? C26 C27 H271 109.0 . . ? N7 C27 H272 109.0 . . ? C26 C27 H272 109.0 . . ? H271 C27 H272 107.8 . . ? C35 C34 C33 119.5(5) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? N5 C20 C19 120.7(5) . . ? N5 C20 C21 119.1(4) . . ? C19 C20 C21 120.2(5) . . ? C43 C42 C41 122.3(6) . . ? C43 C42 H42 118.9 . . ? C41 C42 H42 118.9 . . ? C48 C49 C44 122.8(5) . . ? C48 C49 H49 118.6 . . ? C44 C49 H49 118.6 . . ? C54 C53 C52 119.9(5) . . ? C54 C53 H53 120.1 . . ? C52 C53 H53 120.0 . . ? C46 C47 C48 119.1(5) . . ? C46 C47 H47 120.4 . . ? C48 C47 H47 120.4 . . ? N6 C23 C24 111.7(4) . . ? N6 C23 H231 109.3 . . ? C24 C23 H231 109.3 . . ? N6 C23 H232 109.3 . . ? C24 C23 H232 109.3 . . ? H231 C23 H232 107.9 . . ? C47 C46 C45 119.9(5) . . ? C47 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? C68 C73 C72 123.1(5) . . ? C68 C73 H73 118.4 . . ? C72 C73 H73 118.4 . . ? C59 C60 C61 121.0(4) . . ? C59 C60 H60 119.5 . . ? C61 C60 H60 119.5 . . ? C37 C32 C33 114.2(4) . . ? C37 C32 B1 122.4(4) . . ? C33 C32 B1 123.4(4) . . ? C64 C63 C62 123.0(5) . . ? C64 C63 H63 118.5 . . ? C62 C63 H63 118.5 . . ? C3 C2 C1 117.9(5) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C55 C54 C53 119.3(5) . . ? C55 C54 H54 120.4 . . ? C53 C54 H54 120.4 . . ? C59 C58 C57 120.6(5) . . ? C59 C58 H58 119.7 . . ? C57 C58 H58 119.7 . . ? C77 C78 C79 121.0(5) . . ? C77 C78 H78 119.5 . . ? C79 C78 H78 119.5 . . ? C76 C77 C78 117.9(5) . . ? C76 C77 H77 121.1 . . ? C78 C77 H77 121.1 . . ? C64 C65 C66 119.6(5) . . ? C64 C65 H65 120.2 . . ? C66 C65 H65 120.2 . . ? C40 C39 C38 120.0(6) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C39 C38 C43 123.6(5) . . ? C39 C38 H38 118.2 . . ? C43 C38 H38 118.2 . . ? C18 C17 C16 118.4(6) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? C77 C76 C75 120.3(5) . . ? C77 C76 H76 119.9 . . ? C75 C76 H76 119.9 . . ? C71 C70 C69 120.7(6) . . ? C71 C70 H70 119.6 . . ? C69 C70 H70 119.6 . . ? C74 C75 C76 124.6(5) . . ? C74 C75 H75 117.7 . . ? C76 C75 H75 117.7 . . ? C34 C33 C32 123.6(5) . . ? C34 C33 H33 118.2 . . ? C32 C33 H33 118.2 . . ? C4 C3 C2 119.2(5) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C47 C48 C49 120.4(5) . . ? C47 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? N6 C22 C21 113.8(4) . . ? N6 C22 H221 108.8 . . ? C21 C22 H221 108.8 . . ? N6 C22 H222 108.8 . . ? C21 C22 H222 108.8 . . ? H221 C22 H222 107.7 . . ? C65 C66 C67 119.6(5) . . ? C65 C66 H66 120.2 . . ? C67 C66 H66 120.2 . . ? C70 C69 C68 123.3(5) . . ? C70 C69 H69 118.3 . . ? C68 C69 H69 118.3 . . ? C41 C40 C39 119.0(6) . . ? C41 C40 H40 120.5 . . ? C39 C40 H40 120.5 . . ? C20 C21 C22 115.4(4) . . ? C20 C21 H211 108.4 . . ? C22 C21 H211 108.4 . . ? C20 C21 H212 108.4 . . ? C22 C21 H212 108.4 . . ? H211 C21 H212 107.5 . . ? C54 C55 C50 119.8(5) . . ? C54 C55 H55 120.1 . . ? C50 C55 H55 120.1 . . ? C36 C35 C34 119.3(5) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C71 C72 C73 121.2(6) . . ? C71 C72 H72 119.4 . . ? C73 C72 H72 119.4 . . ? C35 C36 C37 119.9(5) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? N2 C7 C6 114.3(5) . . ? N2 C7 H701 108.7 . . ? C6 C7 H701 108.7 . . ? N2 C7 H702 108.7 . . ? C6 C7 H702 108.7 . . ? H701 C7 H702 107.6 . . ? N5 C16 C17 122.9(5) . . ? N5 C16 H16 118.6 . . ? C17 C16 H16 118.6 . . ? C70 C71 C72 117.9(5) . . ? C70 C71 H71 121.1 . . ? C72 C71 H71 121.1 . . ? C17 C18 C19 120.0(6) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C65 C64 C63 119.9(5) . . ? C65 C64 H64 120.0 . . ? C63 C64 H64 120.0 . . ? C5 C6 C7 115.4(5) . . ? C5 C6 H601 108.4 . . ? C7 C6 H601 108.4 . . ? C5 C6 H62 108.4 . . ? C7 C6 H62 108.4 . . ? H601 C6 H62 107.5 . . ? C40 C41 C42 120.3(6) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? N10 C101 C102 179.4(9) . . ? C101 C102 H103 109.5 . . ? C101 C102 H104 109.5 . . ? H103 C102 H104 109.5 . . ? C101 C102 H105 109.5 . . ? H103 C102 H105 109.5 . . ? H104 C102 H105 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N3 C13 1.468(6) . ? N3 C12 1.479(6) . ? N3 C9 1.496(6) . ? N3 Ni1 2.145(4) . ? C28 N7 1.465(6) . ? C28 H281 0.9600 . ? C28 H282 0.9600 . ? C28 H283 0.9600 . ? C10 N2 1.478(6) . ? C10 C11 1.480(7) . ? C10 H101 0.9700 . ? C10 H102 0.9700 . ? C11 C12 1.486(8) . ? C11 H111 0.9700 . ? C11 H112 0.9700 . ? C13 H131 0.9600 . ? C13 H132 0.9600 . ? C13 H133 0.9600 . ? C9 C8 1.545(7) . ? C9 H91 0.9700 . ? C9 H92 0.9700 . ? C8 N2 1.496(6) . ? C8 H81 0.9700 . ? C8 H82 0.9700 . ? C12 H121 0.9700 . ? C12 H122 0.9700 . ? N4 C14 1.132(6) . ? N4 Ni1 2.077(4) . ? N8 C29 1.121(6) . ? N8 Ni2 2.083(4) . ? C14 C15 1.441(7) . ? C15 H151 0.9600 . ? C15 H152 0.9600 . ? C15 H153 0.9600 . ? C29 C30 1.453(7) . ? C30 H301 0.9600 . ? C30 H302 0.9600 . ? C30 H303 0.9600 . ? C81 N9 1.144(8) . ? C81 C80 1.403(9) . ? C80 H801 0.9600 . ? C80 H802 0.9600 . ? C80 H803 0.9600 . ? Ni1 O2 2.032(3) . ? Ni1 N2 2.075(3) . ? Ni1 N1 2.122(4) . ? Ni1 O1 2.271(3) . ? Ni1 C31 2.493(4) . ? Ni2 O3 2.040(3) . ? Ni2 N6 2.064(3) . ? Ni2 N5 2.109(4) . ? Ni2 N7 2.149(4) . ? Ni2 O1 2.216(3) . ? Ni2 C31 2.472(4) . ? N6 C22 1.473(6) . ? N6 C23 1.486(5) . ? N6 C25 1.501(6) . ? N5 C20 1.341(6) . ? N5 C16 1.343(6) . ? O1 C31 1.294(5) . ? O2 C31 1.272(5) . ? N2 C7 1.476(6) . ? O3 C31 1.282(5) . ? N1 C1 1.331(6) . ? N1 C5 1.343(6) . ? C44 C49 1.394(6) . ? C44 C45 1.406(6) . ? C44 B1 1.642(6) . ? C62 C67 1.385(6) . ? C62 C63 1.396(6) . ? C62 B2 1.653(6) . ? N7 C27 1.483(6) . ? N7 C24 1.496(5) . ? C25 C26 1.487(6) . ? C25 H251 0.9700 . ? C25 H252 0.9700 . ? C67 C66 1.397(7) . ? C67 H67 0.9300 . ? C56 C61 1.390(6) . ? C56 C57 1.397(6) . ? C56 B2 1.645(6) . ? C61 C60 1.395(6) . ? C61 H61 0.9300 . ? C74 C75 1.374(6) . ? C74 C79 1.386(6) . ? C74 B2 1.651(6) . ? C43 C42 1.388(7) . ? C43 C38 1.390(6) . ? C43 B1 1.646(6) . ? B2 C68 1.647(7) . ? C52 C53 1.381(6) . ? C52 C51 1.399(6) . ? C52 H52 0.9300 . ? C51 C50 1.397(6) . ? C51 B1 1.647(7) . ? C26 C27 1.519(7) . ? C26 H261 0.9700 . ? C26 H262 0.9700 . ? C59 C58 1.363(7) . ? C59 C60 1.366(6) . ? C59 H59 0.9300 . ? B1 C32 1.658(6) . ? C45 C46 1.382(6) . ? C45 H45 0.9300 . ? C79 C78 1.386(7) . ? C79 H79 0.9300 . ? C68 C73 1.381(6) . ? C68 C69 1.395(7) . ? C5 C4 1.384(7) . ? C5 C6 1.503(7) . ? C50 C55 1.387(6) . ? C50 H50 0.9300 . ? C37 C32 1.383(6) . ? C37 C36 1.389(7) . ? C37 H37 0.9300 . ? C1 C2 1.368(7) . ? C1 H1 0.9300 . ? C24 C23 1.535(7) . ? C24 H241 0.9700 . ? C24 H242 0.9700 . ? C4 C3 1.355(8) . ? C4 H4 0.9300 . ? C57 C58 1.395(6) . ? C57 H57 0.9300 . ? C19 C18 1.363(8) . ? C19 C20 1.392(7) . ? C19 H19 0.9300 . ? C27 H271 0.9700 . ? C27 H272 0.9700 . ? C34 C35 1.370(8) . ? C34 C33 1.386(7) . ? C34 H34 0.9300 . ? C20 C21 1.494(7) . ? C42 C41 1.406(7) . ? C42 H42 0.9300 . ? C49 C48 1.388(7) . ? C49 H49 0.9300 . ? C53 C54 1.378(7) . ? C53 H53 0.9300 . ? C47 C46 1.369(7) . ? C47 C48 1.374(8) . ? C47 H47 0.9300 . ? C23 H231 0.9700 . ? C23 H232 0.9700 . ? C46 H46 0.9300 . ? C73 C72 1.386(7) . ? C73 H73 0.9300 . ? C60 H60 0.9300 . ? C32 C33 1.388(6) . ? C63 C64 1.390(7) . ? C63 H63 0.9300 . ? C2 C3 1.361(8) . ? C2 H2 0.9300 . ? C54 C55 1.362(6) . ? C54 H54 0.9300 . ? C58 H58 0.9300 . ? C78 C77 1.359(7) . ? C78 H78 0.9300 . ? C77 C76 1.353(7) . ? C77 H77 0.9300 . ? C65 C64 1.364(8) . ? C65 C66 1.373(8) . ? C65 H65 0.9300 . ? C39 C40 1.367(8) . ? C39 C38 1.381(7) . ? C39 H39 0.9300 . ? C38 H38 0.9300 . ? C17 C18 1.360(8) . ? C17 C16 1.368(7) . ? C17 H17 0.9300 . ? C76 C75 1.382(7) . ? C76 H76 0.9300 . ? C70 C71 1.352(8) . ? C70 C69 1.391(7) . ? C70 H70 0.9300 . ? C75 H75 0.9300 . ? C33 H33 0.9300 . ? C3 H3 0.9300 . ? C48 H48 0.9300 . ? C22 C21 1.525(6) . ? C22 H221 0.9700 . ? C22 H222 0.9700 . ? C66 H66 0.9300 . ? C69 H69 0.9300 . ? C40 C41 1.364(9) . ? C40 H40 0.9300 . ? C21 H211 0.9700 . ? C21 H212 0.9700 . ? C55 H55 0.9300 . ? C35 C36 1.362(9) . ? C35 H35 0.9300 . ? C72 C71 1.364(8) . ? C72 H72 0.9300 . ? C36 H36 0.9300 . ? C7 C6 1.510(7) . ? C7 H701 0.9700 . ? C7 H702 0.9700 . ? C16 H16 0.9300 . ? C71 H71 0.9300 . ? C18 H18 0.9300 . ? C64 H64 0.9300 . ? C6 H601 0.9700 . ? C6 H62 0.9700 . ? C41 H41 0.9300 . ? N10 C101 1.122(8) . ? C101 C102 1.450(10) . ? C102 H103 0.9600 . ? C102 H104 0.9600 . ? C102 H105 0.9600 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C10 C11 C12 -52.9(7) . . . . ? C13 N3 C9 C8 159.8(5) . . . . ? C12 N3 C9 C8 -78.5(5) . . . . ? Ni1 N3 C9 C8 38.8(5) . . . . ? N3 C9 C8 N2 -2.0(6) . . . . ? C13 N3 C12 C11 166.4(5) . . . . ? C9 N3 C12 C11 44.1(6) . . . . ? Ni1 N3 C12 C11 -69.8(5) . . . . ? C10 C11 C12 N3 50.4(7) . . . . ? C11 C10 N2 C7 -160.3(5) . . . . ? C11 C10 N2 C8 -39.4(6) . . . . ? C11 C10 N2 Ni1 76.5(5) . . . . ? C9 C8 N2 C7 -158.0(4) . . . . ? C9 C8 N2 C10 80.0(5) . . . . ? C9 C8 N2 Ni1 -37.6(5) . . . . ? Ni1 O2 C31 O3 175.2(3) . . . . ? Ni1 O2 C31 O1 -5.2(4) . . . . ? Ni2 O3 C31 O2 174.5(3) . . . . ? Ni2 O3 C31 O1 -5.1(4) . . . . ? Ni2 O1 C31 O2 -174.9(3) . . . . ? Ni1 O1 C31 O2 4.7(3) . . . . ? Ni2 O1 C31 O3 4.7(3) . . . . ? Ni1 O1 C31 O3 -175.7(3) . . . . ? Ni1 O1 C31 Ni2 179.57(13) . . . . ? Ni2 O1 C31 Ni1 -179.57(13) . . . . ? C22 N6 C25 C26 -161.2(4) . . . . ? C23 N6 C25 C26 -40.4(5) . . . . ? Ni2 N6 C25 C26 75.2(4) . . . . ? C63 C62 C67 C66 0.3(7) . . . . ? B2 C62 C67 C66 179.3(5) . . . . ? C57 C56 C61 C60 -0.6(6) . . . . ? B2 C56 C61 C60 -177.6(4) . . . . ? C61 C56 B2 C68 -165.5(4) . . . . ? C57 C56 B2 C68 17.8(6) . . . . ? C61 C56 B2 C74 -43.6(5) . . . . ? C57 C56 B2 C74 139.8(4) . . . . ? C61 C56 B2 C62 75.4(5) . . . . ? C57 C56 B2 C62 -101.2(5) . . . . ? C75 C74 B2 C56 -78.2(5) . . . . ? C79 C74 B2 C56 97.5(5) . . . . ? C75 C74 B2 C68 42.3(6) . . . . ? C79 C74 B2 C68 -142.0(4) . . . . ? C75 C74 B2 C62 163.5(4) . . . . ? C79 C74 B2 C62 -20.8(6) . . . . ? C67 C62 B2 C56 13.2(6) . . . . ? C63 C62 B2 C56 -167.9(4) . . . . ? C67 C62 B2 C68 -106.0(5) . . . . ? C63 C62 B2 C68 72.9(5) . . . . ? C67 C62 B2 C74 131.3(4) . . . . ? C63 C62 B2 C74 -49.8(6) . . . . ? C53 C52 C51 C50 -1.5(6) . . . . ? C53 C52 C51 B1 -178.5(4) . . . . ? N6 C25 C26 C27 -51.1(6) . . . . ? C49 C44 B1 C43 153.1(4) . . . . ? C45 C44 B1 C43 -31.5(6) . . . . ? C49 C44 B1 C51 -87.3(5) . . . . ? C45 C44 B1 C51 88.1(5) . . . . ? C49 C44 B1 C32 32.7(6) . . . . ? C45 C44 B1 C32 -151.9(4) . . . . ? C42 C43 B1 C44 149.8(4) . . . . ? C38 C43 B1 C44 -34.1(6) . . . . ? C42 C43 B1 C51 30.4(6) . . . . ? C38 C43 B1 C51 -153.5(4) . . . . ? C42 C43 B1 C32 -89.3(5) . . . . ? C38 C43 B1 C32 86.8(5) . . . . ? C50 C51 B1 C44 147.6(4) . . . . ? C52 C51 B1 C44 -35.7(5) . . . . ? C50 C51 B1 C43 -91.3(5) . . . . ? C52 C51 B1 C43 85.5(5) . . . . ? C50 C51 B1 C32 27.7(6) . . . . ? C52 C51 B1 C32 -155.5(4) . . . . ? C49 C44 C45 C46 -0.4(7) . . . . ? B1 C44 C45 C46 -176.3(4) . . . . ? C75 C74 C79 C78 0.2(7) . . . . ? B2 C74 C79 C78 -175.9(5) . . . . ? C56 B2 C68 C73 -124.7(5) . . . . ? C74 B2 C68 C73 115.5(5) . . . . ? C62 B2 C68 C73 -6.0(6) . . . . ? C56 B2 C68 C69 53.8(6) . . . . ? C74 B2 C68 C69 -66.0(6) . . . . ? C62 B2 C68 C69 172.5(4) . . . . ? C1 N1 C5 C4 4.6(7) . . . . ? Ni1 N1 C5 C4 -169.3(4) . . . . ? C1 N1 C5 C6 -173.2(5) . . . . ? Ni1 N1 C5 C6 12.9(7) . . . . ? C52 C51 C50 C55 1.5(7) . . . . ? B1 C51 C50 C55 178.5(4) . . . . ? C5 N1 C1 C2 -2.7(7) . . . . ? Ni1 N1 C1 C2 171.8(4) . . . . ? C28 N7 C24 C23 157.4(4) . . . . ? C27 N7 C24 C23 -82.2(5) . . . . ? Ni2 N7 C24 C23 35.6(5) . . . . ? N1 C5 C4 C3 -2.8(8) . . . . ? C6 C5 C4 C3 175.0(6) . . . . ? C61 C56 C57 C58 0.5(7) . . . . ? B2 C56 C57 C58 177.4(4) . . . . ? C28 N7 C27 C26 166.9(4) . . . . ? C24 N7 C27 C26 45.5(5) . . . . ? Ni2 N7 C27 C26 -68.5(5) . . . . ? C25 C26 C27 N7 48.1(6) . . . . ? C16 N5 C20 C19 2.0(7) . . . . ? Ni2 N5 C20 C19 -171.7(4) . . . . ? C16 N5 C20 C21 -176.4(4) . . . . ? Ni2 N5 C20 C21 9.9(6) . . . . ? C18 C19 C20 N5 -0.1(8) . . . . ? C18 C19 C20 C21 178.3(5) . . . . ? C38 C43 C42 C41 2.1(8) . . . . ? B1 C43 C42 C41 178.6(5) . . . . ? C45 C44 C49 C48 -1.0(7) . . . . ? B1 C44 C49 C48 174.8(5) . . . . ? C51 C52 C53 C54 0.4(7) . . . . ? C22 N6 C23 C24 -159.9(4) . . . . ? C25 N6 C23 C24 78.5(5) . . . . ? Ni2 N6 C23 C24 -38.3(5) . . . . ? N7 C24 C23 N6 0.3(6) . . . . ? C48 C47 C46 C45 -2.2(8) . . . . ? C44 C45 C46 C47 2.0(7) . . . . ? C69 C68 C73 C72 -0.3(7) . . . . ? B2 C68 C73 C72 178.3(5) . . . . ? C58 C59 C60 C61 0.4(7) . . . . ? C56 C61 C60 C59 0.2(7) . . . . ? C36 C37 C32 C33 1.4(7) . . . . ? C36 C37 C32 B1 -177.7(4) . . . . ? C44 B1 C32 C37 99.8(5) . . . . ? C43 B1 C32 C37 -22.1(6) . . . . ? C51 B1 C32 C37 -141.0(4) . . . . ? C44 B1 C32 C33 -79.2(5) . . . . ? C43 B1 C32 C33 158.9(4) . . . . ? C51 B1 C32 C33 39.9(6) . . . . ? C67 C62 C63 C64 -0.9(7) . . . . ? B2 C62 C63 C64 -179.9(5) . . . . ? N1 C1 C2 C3 -1.2(8) . . . . ? C52 C53 C54 C55 0.8(7) . . . . ? C60 C59 C58 C57 -0.4(7) . . . . ? C56 C57 C58 C59 0.0(8) . . . . ? C74 C79 C78 C77 -1.3(9) . . . . ? C79 C78 C77 C76 1.9(9) . . . . ? C40 C39 C38 C43 0.0(8) . . . . ? C42 C43 C38 C39 -1.7(7) . . . . ? B1 C43 C38 C39 -178.1(5) . . . . ? C78 C77 C76 C75 -1.4(9) . . . . ? C79 C74 C75 C76 0.2(8) . . . . ? B2 C74 C75 C76 176.3(5) . . . . ? C77 C76 C75 C74 0.4(9) . . . . ? C35 C34 C33 C32 0.1(8) . . . . ? C37 C32 C33 C34 -0.8(7) . . . . ? B1 C32 C33 C34 178.3(5) . . . . ? C5 C4 C3 C2 -1.2(9) . . . . ? C1 C2 C3 C4 3.1(9) . . . . ? C46 C47 C48 C49 0.9(8) . . . . ? C44 C49 C48 C47 0.7(8) . . . . ? C23 N6 C22 C21 174.4(4) . . . . ? C25 N6 C22 C21 -64.2(5) . . . . ? Ni2 N6 C22 C21 56.8(5) . . . . ? C64 C65 C66 C67 -0.8(9) . . . . ? C62 C67 C66 C65 0.5(8) . . . . ? C71 C70 C69 C68 1.6(9) . . . . ? C73 C68 C69 C70 -1.6(8) . . . . ? B2 C68 C69 C70 179.8(5) . . . . ? C38 C39 C40 C41 1.4(10) . . . . ? N5 C20 C21 C22 37.6(6) . . . . ? C19 C20 C21 C22 -140.8(5) . . . . ? N6 C22 C21 C20 -77.8(5) . . . . ? C53 C54 C55 C50 -0.7(8) . . . . ? C51 C50 C55 C54 -0.5(8) . . . . ? C33 C34 C35 C36 0.1(8) . . . . ? C68 C73 C72 C71 2.2(9) . . . . ? C34 C35 C36 C37 0.5(9) . . . . ? C32 C37 C36 C35 -1.3(8) . . . . ? C10 N2 C7 C6 -60.0(6) . . . . ? C8 N2 C7 C6 177.8(4) . . . . ? Ni1 N2 C7 C6 61.2(5) . . . . ? C20 N5 C16 C17 -2.1(7) . . . . ? Ni2 N5 C16 C17 172.1(4) . . . . ? C18 C17 C16 N5 0.2(9) . . . . ? C69 C70 C71 C72 0.3(9) . . . . ? C73 C72 C71 C70 -2.1(9) . . . . ? C16 C17 C18 C19 1.8(10) . . . . ? C20 C19 C18 C17 -1.9(9) . . . . ? C66 C65 C64 C63 0.3(9) . . . . ? C62 C63 C64 C65 0.6(9) . . . . ? N1 C5 C6 C7 32.6(7) . . . . ? C4 C5 C6 C7 -145.2(5) . . . . ? N2 C7 C6 C5 -76.7(7) . . . . ? C39 C40 C41 C42 -0.9(11) . . . . ? C43 C42 C41 C40 -0.9(10) . . . . ?