#------------------------------------------------------------------------------ #$Date: 2017-09-11 14:43:28 +0300 (Mon, 11 Sep 2017) $ #$Revision: 200442 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/69/1546982.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_1546982 loop_ _publ_author_name 'McKinnie, Shaun M. K.' 'Wang, Wang' 'Fischer, Conrad' 'McDonald, Tyler' 'Kalin, Kevin R.' 'Iturrioz, Xavier' 'Llorens-Cortes, Catherine' 'Oudit, Gavin Y.' 'Vederas, John C.' _publ_section_title ; Synthetic Modification within the "RPRL" Region of Apelin Peptides: Impact on Cardiovascular Activity and Stability to Neprilysin and Plasma Degradation. ; _journal_issue 14 _journal_name_full 'Journal of medicinal chemistry' _journal_page_first 6408 _journal_page_last 6427 _journal_paper_doi 10.1021/acs.jmedchem.7b00723 _journal_volume 60 _journal_year 2017 _chemical_absolute_configuration ad _chemical_formula_moiety 'C32 H35 N3 Ni O3' _chemical_formula_sum 'C32 H35 N3 Ni O3' _chemical_formula_weight 568.34 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 105.0306(9) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.1064(3) _cell_length_b 21.5351(6) _cell_length_c 12.1674(3) _cell_measurement_reflns_used 9062 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 73.50 _cell_measurement_theta_min 3.76 _cell_volume 2810.60(13) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'DIRDIF-2008 (Beurskens et al., 2008)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0126 _diffrn_reflns_av_unetI/netI 0.0189 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 20104 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 74.032 _diffrn_reflns_theta_min 3.761 _exptl_absorpt_coefficient_mu 1.294 _exptl_absorpt_correction_T_max 0.8166 _exptl_absorpt_correction_T_min 0.6952 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.343 _exptl_crystal_description fragment _exptl_crystal_F_000 1200 _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.309 _exptl_crystal_size_min 0.230 _refine_diff_density_max 0.226 _refine_diff_density_min -0.220 _refine_diff_density_rms 0.031 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.012(12) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 704 _refine_ls_number_reflns 11035 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.028 _refine_ls_R_factor_all 0.0213 _refine_ls_R_factor_gt 0.0212 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+0.3055P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.0574 _reflns_Friedel_coverage 0.949 _reflns_Friedel_fraction_full 0.998 _reflns_Friedel_fraction_max 0.993 _reflns_number_gt 10977 _reflns_number_total 11035 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jm7b00723_si_003.cif _cod_data_source_block jcv1503 _cod_database_code 1546982 _shelx_shelxl_version_number 2014/7 _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 0.653 _shelx_estimated_absorpt_t_max 0.755 _shelx_res_file ; jcv1503.res created by SHELXL-2014/7 TITL jcv1503 in P2(1) CELL 1.54178 11.1064 21.5351 12.1674 90.0 105.0306 90.0 ZERR 4.00 0.0003 0.0006 0.0003 0.0 0.0009 0.0 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O NI UNIT 128 140 12 12 4 SIZE 0.23 0.309 0.36 TEMP -100 L.S. 4 ACTA CONF 2.0 178.0 TWIN WGHT 0.037200 0.305500 BASF 0.01199 FVAR 0.18647 NIA 5 0.141477 0.393699 0.233595 11.00000 0.02795 0.02263 = 0.01782 -0.00191 0.00104 -0.00077 O1A 4 0.196469 0.313455 0.265979 11.00000 0.04222 0.02686 = 0.02215 0.00094 -0.00169 0.00231 O2A 4 0.220162 0.223278 0.185903 11.00000 0.04169 0.02624 = 0.03146 0.00270 -0.00021 0.00482 O3A 4 0.179255 0.573394 0.262471 11.00000 0.03697 0.02680 = 0.03680 -0.00398 0.00196 -0.00750 N1A 3 0.055696 0.364411 0.090230 11.00000 0.02586 0.02007 = 0.01992 -0.00074 0.00555 -0.00060 N2A 3 0.093880 0.475807 0.207123 11.00000 0.02632 0.02370 = 0.01971 -0.00309 0.00401 -0.00266 N3A 3 0.230533 0.420365 0.385687 11.00000 0.03202 0.02863 = 0.02135 -0.00216 -0.00025 -0.00136 C1A 1 0.182156 0.276464 0.179356 11.00000 0.02748 0.02436 = 0.02447 0.00179 0.00253 -0.00134 C2A 1 0.114182 0.304826 0.062827 11.00000 0.02640 0.02066 = 0.02167 -0.00042 0.00439 0.00198 C3A 1 0.215689 0.326578 0.003665 11.00000 0.03232 0.02862 = 0.03004 0.00374 0.01144 0.00429 AFIX 23 H3A 2 0.174390 0.351976 -0.063330 11.00000 -1.20000 H3B 2 0.274607 0.354037 0.057115 11.00000 -1.20000 AFIX 0 C4A 1 0.291887 0.275451 -0.036243 11.00000 0.04794 0.04143 = 0.04853 0.00868 0.02631 0.01632 AFIX 13 H4A 2 0.297559 0.238801 0.015319 11.00000 -1.20000 AFIX 0 C5A 1 0.424235 0.299238 -0.027434 11.00000 0.04962 0.07295 = 0.08433 0.02366 0.04036 0.02177 AFIX 33 H5A 2 0.462642 0.312551 0.050835 11.00000 -1.20000 H5B 2 0.474140 0.265893 -0.048310 11.00000 -1.20000 H5C 2 0.420479 0.334467 -0.079199 11.00000 -1.20000 AFIX 0 C6A 1 0.231416 0.254648 -0.157601 11.00000 0.09015 0.07047 = 0.05354 -0.01362 0.03703 0.01534 AFIX 33 H6A 2 0.146935 0.239511 -0.162676 11.00000 -1.20000 H6B 2 0.227363 0.289809 -0.209568 11.00000 -1.20000 H6C 2 0.281024 0.221235 -0.178679 11.00000 -1.20000 AFIX 0 C7A 1 0.027818 0.254115 -0.002465 11.00000 0.03517 0.02189 = 0.02821 -0.00195 -0.00097 0.00182 AFIX 33 H7A 2 0.077729 0.218417 -0.014298 11.00000 -1.20000 H7B 2 -0.030297 0.241089 0.041492 11.00000 -1.20000 H7C 2 -0.019205 0.270410 -0.076342 11.00000 -1.20000 AFIX 0 C8A 1 -0.038238 0.391907 0.021256 11.00000 0.02296 0.02377 = 0.01834 -0.00027 0.00547 -0.00198 C9A 1 -0.114230 0.361605 -0.085468 11.00000 0.02508 0.01987 = 0.02305 -0.00192 0.00210 0.00249 C10A 1 -0.217038 0.326022 -0.078908 11.00000 0.02602 0.02735 = 0.02899 -0.00203 0.00519 0.00165 AFIX 43 H10A 2 -0.237825 0.321297 -0.008394 11.00000 -1.20000 AFIX 0 C11A 1 -0.288797 0.297536 -0.176548 11.00000 0.02528 0.03005 = 0.04169 -0.01013 0.00248 -0.00163 AFIX 43 H11A 2 -0.357544 0.272246 -0.172340 11.00000 -1.20000 AFIX 0 C12A 1 -0.260530 0.305854 -0.279997 11.00000 0.03739 0.03747 = 0.03250 -0.01484 -0.00263 0.00394 AFIX 43 H12A 2 -0.309977 0.286309 -0.346469 11.00000 -1.20000 AFIX 0 C13A 1 -0.160633 0.342494 -0.286671 11.00000 0.04310 0.03392 = 0.02227 -0.00505 0.00468 0.00681 AFIX 43 H13A 2 -0.142432 0.348538 -0.358021 11.00000 -1.20000 AFIX 0 C14A 1 -0.086182 0.370722 -0.189241 11.00000 0.03350 0.02158 = 0.02385 0.00013 0.00584 0.00279 AFIX 43 H14A 2 -0.017295 0.395818 -0.193792 11.00000 -1.20000 AFIX 0 C15A 1 -0.079290 0.455083 0.041720 11.00000 0.02428 0.02353 = 0.01983 -0.00010 0.00776 -0.00013 C16A 1 -0.013714 0.495679 0.128662 11.00000 0.02424 0.02394 = 0.02167 0.00003 0.00946 -0.00204 C17A 1 -0.063087 0.555907 0.134772 11.00000 0.02820 0.02514 = 0.03028 -0.00461 0.01212 -0.00183 AFIX 43 H17A 2 -0.022415 0.582969 0.194561 11.00000 -1.20000 AFIX 0 C18A 1 -0.168383 0.576099 0.056285 11.00000 0.02895 0.02514 = 0.03785 -0.00186 0.01427 0.00335 AFIX 43 H18A 2 -0.197873 0.617110 0.061612 11.00000 -1.20000 AFIX 0 C19A 1 -0.232306 0.537366 -0.030748 11.00000 0.02836 0.03238 = 0.03064 -0.00033 0.00592 0.00708 AFIX 43 H19A 2 -0.304386 0.551637 -0.085499 11.00000 -1.20000 AFIX 0 C20A 1 -0.188693 0.477672 -0.035853 11.00000 0.02581 0.02941 = 0.02472 -0.00279 0.00502 0.00292 AFIX 43 H20A 2 -0.233841 0.450647 -0.093702 11.00000 -1.20000 AFIX 0 C21A 1 0.173722 0.517336 0.275313 11.00000 0.02757 0.02912 = 0.02381 -0.00533 0.00592 -0.00358 C22A 1 0.265853 0.486585 0.373787 11.00000 0.02960 0.02953 = 0.02359 -0.00732 0.00241 -0.00440 AFIX 13 H22A 2 0.266235 0.509375 0.445485 11.00000 -1.20000 AFIX 0 C23A 1 0.400476 0.485144 0.358896 11.00000 0.02994 0.04147 = 0.03379 -0.00591 0.00282 -0.00123 AFIX 23 H23A 2 0.403048 0.503069 0.284615 11.00000 -1.20000 H23B 2 0.458147 0.508754 0.420395 11.00000 -1.20000 AFIX 0 C24A 1 0.435310 0.416254 0.364985 11.00000 0.03299 0.04564 = 0.04534 -0.01115 0.00079 0.00427 AFIX 23 H24A 2 0.417999 0.397763 0.287974 11.00000 -1.20000 H24B 2 0.524509 0.410216 0.404062 11.00000 -1.20000 AFIX 0 C25A 1 0.352902 0.388284 0.432547 11.00000 0.03762 0.03791 = 0.03032 -0.00482 -0.01077 0.00417 AFIX 23 H25A 2 0.344775 0.342842 0.420605 11.00000 -1.20000 H25B 2 0.385875 0.396782 0.514844 11.00000 -1.20000 AFIX 0 C26A 1 0.150035 0.412666 0.466960 11.00000 0.04564 0.03721 = 0.02022 0.00052 0.00501 -0.00497 AFIX 23 H26A 2 0.194736 0.430245 0.541568 11.00000 -1.20000 H26B 2 0.138320 0.367740 0.478010 11.00000 -1.20000 AFIX 0 C27A 1 0.023642 0.442899 0.429511 11.00000 0.04223 0.03783 = 0.02280 -0.00074 0.01144 -0.00589 C28A 1 -0.077973 0.410695 0.362885 11.00000 0.04611 0.03659 = 0.03556 -0.00105 0.01244 -0.00857 AFIX 43 H28A 2 -0.067024 0.369496 0.339290 11.00000 -1.20000 AFIX 0 C29A 1 -0.195230 0.438007 0.330419 11.00000 0.04319 0.04958 = 0.04263 -0.00163 0.00878 -0.00970 AFIX 43 H29A 2 -0.263790 0.415426 0.285105 11.00000 -1.20000 AFIX 0 C30A 1 -0.212356 0.498398 0.364205 11.00000 0.04601 0.05575 = 0.04205 0.00124 0.01282 0.00436 AFIX 43 H30A 2 -0.292552 0.517058 0.342550 11.00000 -1.20000 AFIX 0 C31A 1 -0.111498 0.531160 0.429731 11.00000 0.05798 0.04389 = 0.03992 -0.00798 0.01678 0.00298 AFIX 43 H31A 2 -0.122497 0.572598 0.452087 11.00000 -1.20000 AFIX 0 C32A 1 0.005420 0.503675 0.462782 11.00000 0.05015 0.04367 = 0.02803 -0.00937 0.01236 -0.00688 AFIX 43 H32A 2 0.073697 0.526316 0.508398 11.00000 -1.20000 AFIX 0 NIB 5 0.239081 0.620979 0.785040 11.00000 0.02891 0.02109 = 0.02176 -0.00007 0.01191 0.00067 O1B 4 0.214502 0.700238 0.831888 11.00000 0.04348 0.02532 = 0.03252 -0.00286 0.02046 -0.00008 O2B 4 0.235622 0.799883 0.795228 11.00000 0.05830 0.02449 = 0.04179 -0.00307 0.02193 0.00446 O3B 4 0.174737 0.441281 0.747551 11.00000 0.04451 0.02502 = 0.04349 -0.00371 0.01671 -0.00531 N1B 3 0.339894 0.656790 0.699591 11.00000 0.02523 0.02374 = 0.01951 0.00094 0.00534 0.00020 N2B 3 0.267179 0.539060 0.754224 11.00000 0.03010 0.02231 = 0.02137 0.00162 0.00906 0.00056 N3B 3 0.116437 0.590582 0.860592 11.00000 0.03040 0.02725 = 0.02512 -0.00116 0.01191 -0.00112 C1B 1 0.250201 0.744934 0.776979 11.00000 0.03534 0.02579 = 0.02725 -0.00182 0.01034 0.00186 C2B 1 0.312242 0.725249 0.681929 11.00000 0.03061 0.01959 = 0.02594 0.00099 0.01047 0.00034 C3B 1 0.221284 0.738237 0.564981 11.00000 0.03355 0.02482 = 0.02866 0.00553 0.00935 0.00373 AFIX 23 H3C 2 0.202089 0.783203 0.560883 11.00000 -1.20000 H3D 2 0.265618 0.729320 0.505880 11.00000 -1.20000 AFIX 0 C4B 1 0.096768 0.702789 0.533161 11.00000 0.03229 0.02656 = 0.03996 0.00666 0.00373 0.00160 AFIX 13 H4B 2 0.111514 0.660356 0.567397 11.00000 -1.20000 AFIX 0 C5B 1 -0.003532 0.734092 0.578651 11.00000 0.03227 0.05102 = 0.06145 0.00851 0.01146 0.00603 AFIX 33 H5D 2 0.026303 0.738646 0.661414 11.00000 -1.20000 H5E 2 -0.022182 0.775151 0.543645 11.00000 -1.20000 H5F 2 -0.079228 0.708612 0.560154 11.00000 -1.20000 AFIX 0 C6B 1 0.050963 0.695498 0.404020 11.00000 0.05011 0.04926 = 0.04255 -0.00364 -0.00441 0.00023 AFIX 33 H6D 2 0.115801 0.675351 0.375228 11.00000 -1.20000 H6E 2 -0.024659 0.669965 0.385285 11.00000 -1.20000 H6F 2 0.032387 0.736504 0.368776 11.00000 -1.20000 AFIX 0 C7B 1 0.428596 0.766112 0.696658 11.00000 0.03708 0.02648 = 0.04400 -0.00478 0.01358 -0.00710 AFIX 33 H7D 2 0.403411 0.809691 0.683972 11.00000 -1.20000 H7E 2 0.482240 0.761145 0.773959 11.00000 -1.20000 H7F 2 0.474420 0.753588 0.641445 11.00000 -1.20000 AFIX 0 C8B 1 0.411965 0.626647 0.649610 11.00000 0.02004 0.02689 = 0.01743 -0.00043 0.00240 -0.00094 C9B 1 0.464844 0.653130 0.557779 11.00000 0.02315 0.02476 = 0.02382 -0.00121 0.00688 -0.00057 C10B 1 0.581331 0.681744 0.579107 11.00000 0.02358 0.04028 = 0.04213 -0.00636 0.00751 -0.00540 AFIX 43 H10B 2 0.629838 0.687919 0.654994 11.00000 -1.20000 AFIX 0 C11B 1 0.625473 0.701132 0.487451 11.00000 0.03521 0.04680 = 0.07807 0.00143 0.03225 -0.00823 AFIX 43 H11B 2 0.703524 0.721816 0.501299 11.00000 -1.20000 AFIX 0 C12B 1 0.557386 0.690712 0.376764 11.00000 0.06302 0.05829 = 0.05441 0.01323 0.03987 0.00173 AFIX 43 H12B 2 0.589068 0.703899 0.315189 11.00000 -1.20000 AFIX 0 C13B 1 0.443888 0.661297 0.355589 11.00000 0.05713 0.04464 = 0.02751 0.00417 0.01838 0.00604 AFIX 43 H13B 2 0.397310 0.653792 0.279497 11.00000 -1.20000 AFIX 0 C14B 1 0.397550 0.642576 0.446030 11.00000 0.03007 0.02770 = 0.02404 -0.00204 0.00743 -0.00076 AFIX 43 H14B 2 0.318980 0.622335 0.431294 11.00000 -1.20000 AFIX 0 C15B 1 0.444651 0.560707 0.676164 11.00000 0.02344 0.02814 = 0.01849 -0.00142 0.00264 0.00386 C16B 1 0.376262 0.519510 0.728116 11.00000 0.02873 0.02634 = 0.01675 -0.00107 0.00356 0.00307 C17B 1 0.424128 0.459116 0.756274 11.00000 0.03618 0.02822 = 0.02865 0.00350 0.00368 0.00529 AFIX 43 H17B 2 0.380942 0.431406 0.793393 11.00000 -1.20000 AFIX 0 C18B 1 0.532039 0.439519 0.731096 11.00000 0.03720 0.03044 = 0.03238 -0.00130 -0.00305 0.01228 AFIX 43 H18B 2 0.562202 0.398716 0.751409 11.00000 -1.20000 AFIX 0 C19B 1 0.597214 0.478658 0.676425 11.00000 0.02717 0.03963 = 0.03314 -0.00619 0.00109 0.01079 AFIX 43 H19B 2 0.670590 0.464677 0.657747 11.00000 -1.20000 AFIX 0 C20B 1 0.553614 0.538210 0.649671 11.00000 0.02356 0.03747 = 0.02660 -0.00269 0.00463 0.00382 AFIX 43 H20B 2 0.598167 0.565016 0.612233 11.00000 -1.20000 AFIX 0 C21B 1 0.181379 0.496876 0.771363 11.00000 0.03350 0.02506 = 0.02351 0.00106 0.00893 -0.00157 C22B 1 0.083853 0.524844 0.823169 11.00000 0.03208 0.02699 = 0.02641 0.00027 0.01132 -0.00545 AFIX 13 H22B 2 0.079572 0.499627 0.891064 11.00000 -1.20000 AFIX 0 C23B 1 -0.047348 0.526743 0.739308 11.00000 0.03038 0.03514 = 0.03325 0.00019 0.01000 -0.00615 AFIX 23 H23C 2 -0.048919 0.503081 0.669190 11.00000 -1.20000 H23D 2 -0.110795 0.509356 0.774734 11.00000 -1.20000 AFIX 0 C24B 1 -0.070455 0.595643 0.713323 11.00000 0.03172 0.03639 = 0.03818 0.00162 0.00897 -0.00088 AFIX 23 H24C 2 -0.034123 0.609088 0.651015 11.00000 -1.20000 H24D 2 -0.160668 0.605349 0.692502 11.00000 -1.20000 AFIX 0 C25B 1 -0.004354 0.625670 0.824885 11.00000 0.03006 0.03383 = 0.03820 -0.00035 0.01527 0.00307 AFIX 23 H25C 2 0.010565 0.670346 0.814457 11.00000 -1.20000 H25D 2 -0.053305 0.621135 0.881808 11.00000 -1.20000 AFIX 0 C26B 1 0.169556 0.596061 0.986711 11.00000 0.03750 0.03813 = 0.02372 -0.00206 0.01595 -0.00449 AFIX 23 H26C 2 0.114114 0.574145 1.025806 11.00000 -1.20000 H26D 2 0.171623 0.640419 1.008493 11.00000 -1.20000 AFIX 0 C27B 1 0.299048 0.569554 1.026570 11.00000 0.03733 0.04584 = 0.01937 -0.00122 0.01181 -0.00628 C28B 1 0.401674 0.608782 1.046611 11.00000 0.03982 0.05126 = 0.04056 -0.00782 0.01582 -0.00908 AFIX 43 H28B 2 0.389688 0.652258 1.035808 11.00000 -1.20000 AFIX 0 C29B 1 0.521658 0.584966 1.082310 11.00000 0.03814 0.07551 = 0.05559 -0.00588 0.01669 -0.01158 AFIX 43 H29B 2 0.591084 0.612348 1.097602 11.00000 -1.20000 AFIX 0 C30B 1 0.540821 0.521702 1.095760 11.00000 0.03903 0.08225 = 0.03896 0.00762 0.01412 0.00823 AFIX 43 H30B 2 0.623117 0.505523 1.118791 11.00000 -1.20000 AFIX 0 C31B 1 0.439729 0.482236 1.075537 11.00000 0.05222 0.05950 = 0.03448 0.01325 0.01313 0.00825 AFIX 43 H31B 2 0.452427 0.438679 1.083800 11.00000 -1.20000 AFIX 0 C32B 1 0.319578 0.505882 1.043178 11.00000 0.04405 0.04786 = 0.02942 0.00781 0.00787 -0.00427 AFIX 43 H32B 2 0.250475 0.478457 1.032188 11.00000 -1.20000 AFIX 0 HKLF 4 REM jcv1503 in P2(1) REM R1 = 0.0212 for 10977 Fo > 4sig(Fo) and 0.0213 for all 11035 data REM 704 parameters refined using 1 restraints END WGHT 0.0372 0.3055 REM Highest difference peak 0.226, deepest hole -0.220, 1-sigma level 0.031 Q1 1 0.4119 0.8043 0.7347 11.00000 0.05 0.23 Q2 1 0.4401 0.7777 0.6200 11.00000 0.05 0.19 Q3 1 0.5038 0.7451 0.7431 11.00000 0.05 0.17 Q4 1 0.2806 0.7360 0.7285 11.00000 0.05 0.17 Q5 1 0.1189 0.5130 0.7886 11.00000 0.05 0.17 Q6 1 0.4232 0.5948 0.6561 11.00000 0.05 0.17 Q7 1 0.0216 0.2582 -0.0856 11.00000 0.05 0.17 Q8 1 0.0645 0.2161 0.0247 11.00000 0.05 0.16 Q9 1 0.2181 0.4990 0.3297 11.00000 0.05 0.16 Q10 1 0.1687 0.3148 0.0332 11.00000 0.05 0.16 Q11 1 -0.0406 0.4741 0.0871 11.00000 0.05 0.16 Q12 1 0.1136 0.3157 0.2878 11.00000 0.05 0.15 Q13 1 0.4995 0.5481 0.6610 11.00000 0.05 0.15 Q14 1 0.1480 0.2871 0.1199 11.00000 0.05 0.15 Q15 1 0.3625 0.7471 0.6865 11.00000 0.05 0.14 Q16 1 0.0184 0.6704 0.8613 11.00000 0.05 0.14 Q17 1 0.0210 0.5267 0.7791 11.00000 0.05 0.14 Q18 1 0.5182 0.6658 0.5662 11.00000 0.05 0.14 Q19 1 0.0198 0.4698 0.4452 11.00000 0.05 0.13 Q20 1 0.4816 0.5082 1.1261 11.00000 0.05 0.13 ; _shelx_res_checksum 34745 _shelx_hkl_file ; 2 -10 -14 17.67 0.47 3 -10 -14 0.91 0.04 4 -10 -14 0.75 0.04 1 -9 -14 0.81 0.05 2 -9 -14 2.99 0.06 3 -9 -14 0.78 0.04 4 -9 -14 0.16 0.02 5 -9 -14 5.08 0.08 1 -8 -14 1.11 0.04 2 -8 -14 9.46 0.11 3 -8 -14 0.47 0.03 4 -8 -14 7.43 0.10 5 -8 -14 2.74 0.06 6 -8 -14 11.22 0.12 0 -7 -14 11.60 0.17 1 -7 -14 25.82 0.23 2 -7 -14 5.36 0.08 3 -7 -14 4.89 0.08 4 -7 -14 5.67 0.09 5 -7 -14 4.95 0.08 6 -7 -14 2.63 0.06 7 -7 -14 3.05 0.14 0 -6 -14 8.97 0.12 1 -6 -14 5.26 0.08 2 -6 -14 13.69 0.15 3 -6 -14 9.30 0.12 4 -6 -14 8.82 0.11 5 -6 -14 9.18 0.12 6 -6 -14 7.84 0.10 7 -6 -14 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7.80 0.23 -8 -13 0 1.49 0.11 -7 -13 0 26.72 0.49 -6 -13 0 25.89 1.09 -5 -13 0 11.61 0.48 -4 -13 0 13.84 0.51 -3 -13 0 0.93 0.16 -2 -13 0 52.77 1.71 -1 -13 0 28.29 0.67 0 -13 0 0.07 0.06 1 -13 0 29.56 0.70 2 -13 0 52.41 1.03 3 -13 0 0.90 0.21 4 -13 0 14.23 0.59 5 -13 0 11.23 0.56 6 -13 0 23.84 0.89 7 -13 0 25.68 0.68 8 -13 0 1.56 0.16 9 -13 0 7.63 0.25 10 -13 0 6.41 0.22 11 -13 0 0.55 0.06 -11 -12 0 3.74 0.14 -10 -12 0 0.54 0.07 -9 -12 0 1.74 0.11 -8 -12 0 5.36 0.19 -7 -12 0 14.35 0.79 -6 -12 0 82.83 2.44 -5 -12 0 5.62 0.45 -4 -12 0 5.29 0.28 -3 -12 0 8.32 0.33 -2 -12 0 35.31 0.75 -1 -12 0 1.96 0.16 0 -12 0 44.92 0.81 1 -12 0 2.22 0.20 2 -12 0 36.08 0.78 3 -12 0 9.34 0.47 4 -12 0 5.80 0.37 5 -12 0 5.55 0.45 6 -12 0 77.76 1.89 7 -12 0 13.55 0.66 8 -12 0 5.09 0.28 9 -12 0 1.48 0.14 10 -12 0 0.72 0.09 11 -12 0 3.92 0.15 -12 -11 0 0.99 0.09 -11 -11 0 0.20 0.05 -10 -11 0 0.81 0.08 -9 -11 0 2.00 0.12 -8 -11 0 4.29 0.18 -7 -11 0 11.87 0.70 -6 -11 0 88.82 2.50 -5 -11 0 96.59 2.08 -4 -11 0 25.06 0.62 -3 -11 0 151.92 2.32 -2 -11 0 82.74 1.38 -1 -11 0 6.20 0.27 1 -11 0 6.44 0.23 2 -11 0 83.29 1.22 3 -11 0 160.68 2.95 4 -11 0 25.52 0.66 5 -11 0 93.08 1.78 6 -11 0 81.91 1.92 7 -11 0 10.96 0.59 8 -11 0 4.40 0.27 9 -11 0 1.90 0.15 10 -11 0 0.77 0.09 11 -11 0 0.19 0.05 12 -11 0 0.92 0.07 -12 -10 0 0.09 0.04 -11 -10 0 6.53 0.22 -10 -10 0 0.43 0.07 -9 -10 0 17.10 0.31 -8 -10 0 32.92 1.30 -7 -10 0 31.41 1.22 -6 -10 0 18.99 0.85 -5 -10 0 37.99 1.05 -4 -10 0 177.26 3.35 -3 -10 0 20.06 0.50 -2 -10 0 171.55 2.55 -1 -10 0 40.61 1.02 0 -10 0 242.27 4.35 1 -10 0 40.95 1.02 2 -10 0 177.66 2.56 3 -10 0 20.58 0.67 4 -10 0 182.96 2.72 5 -10 0 37.41 0.87 6 -10 0 17.54 0.70 7 -10 0 29.26 0.97 8 -10 0 31.67 1.55 9 -10 0 17.18 0.45 10 -10 0 0.42 0.08 11 -10 0 6.57 0.18 12 -10 0 0.13 0.04 -12 -9 0 12.90 0.22 -11 -9 0 8.37 0.20 -10 -9 0 0.46 0.07 -9 -9 0 6.09 0.20 -8 -9 0 1.64 0.31 -7 -9 0 30.01 1.17 -6 -9 0 9.83 0.48 -5 -9 0 33.64 0.96 -4 -9 0 67.30 1.19 -3 -9 0 14.12 0.48 -2 -9 0 59.07 1.30 -1 -9 0 215.77 3.89 0 -9 0 0.02 0.05 1 -9 0 214.61 3.97 2 -9 0 61.89 1.91 3 -9 0 14.54 0.51 4 -9 0 69.05 1.23 5 -9 0 33.76 0.80 6 -9 0 9.59 0.42 7 -9 0 27.74 0.92 8 -9 0 1.49 0.40 9 -9 0 5.45 0.27 10 -9 0 0.42 0.09 11 -9 0 8.59 0.24 12 -9 0 13.33 0.25 -12 -8 0 6.75 0.16 -11 -8 0 7.57 0.21 -10 -8 0 25.69 0.39 -9 -8 0 0.63 0.06 -8 -8 0 56.53 1.26 -7 -8 0 31.68 0.80 -6 -8 0 3.66 0.23 -5 -8 0 17.34 0.61 -4 -8 0 8.24 0.38 -3 -8 0 82.19 2.72 -2 -8 0 17.48 0.55 -1 -8 0 102.52 1.93 0 -8 0 91.89 1.74 1 -8 0 104.16 1.93 2 -8 0 17.92 0.80 3 -8 0 90.15 2.58 4 -8 0 8.31 0.31 5 -8 0 16.79 0.50 6 -8 0 3.98 0.31 7 -8 0 31.58 1.01 8 -8 0 57.41 2.20 9 -8 0 0.59 0.11 10 -8 0 25.72 0.43 11 -8 0 7.84 0.24 12 -8 0 7.08 0.18 -12 -7 0 6.61 0.16 -11 -7 0 7.05 0.21 -10 -7 0 15.70 0.27 -9 -7 0 9.02 0.19 -8 -7 0 10.23 0.42 -7 -7 0 28.62 0.74 -6 -7 0 12.77 0.38 -5 -7 0 153.27 2.29 -4 -7 0 14.28 0.50 -3 -7 0 6.44 0.32 -2 -7 0 228.13 4.36 -1 -7 0 15.37 0.47 1 -7 0 16.00 0.69 2 -7 0 237.12 6.76 3 -7 0 7.09 0.49 4 -7 0 14.44 0.77 5 -7 0 153.52 2.36 6 -7 0 12.44 0.45 7 -7 0 28.06 1.35 8 -7 0 10.57 0.87 9 -7 0 9.30 0.30 10 -7 0 16.41 0.37 11 -7 0 7.18 0.21 12 -7 0 6.70 0.18 -13 -6 0 1.12 0.18 -12 -6 0 12.32 0.21 -11 -6 0 4.35 0.16 -10 -6 0 23.01 0.35 -9 -6 0 3.68 0.23 -8 -6 0 3.33 0.28 -7 -6 0 9.02 0.37 -6 -6 0 38.39 0.78 -5 -6 0 100.11 1.55 -4 -6 0 103.65 3.17 -3 -6 0 49.53 1.13 -2 -6 0 84.67 1.64 -1 -6 0 239.45 4.57 0 -6 0 12.20 0.37 1 -6 0 244.95 6.86 2 -6 0 88.70 2.34 3 -6 0 51.50 1.59 4 -6 0 110.33 2.93 5 -6 0 96.02 1.60 6 -6 0 36.91 0.84 7 -6 0 9.18 0.74 8 -6 0 2.76 0.50 9 -6 0 4.21 0.62 10 -6 0 23.33 0.45 11 -6 0 4.83 0.19 12 -6 0 12.30 0.23 -13 -5 0 5.31 0.15 -12 -5 0 8.86 0.20 -11 -5 0 5.73 0.17 -10 -5 0 30.42 0.38 -9 -5 0 55.87 1.74 -8 -5 0 13.69 0.49 -7 -5 0 33.85 0.81 -6 -5 0 5.31 0.23 -5 -5 0 36.30 0.69 -4 -5 0 166.49 4.51 -3 -5 0 58.07 1.21 -2 -5 0 10.68 0.35 -1 -5 0 294.75 5.69 0 -5 0 0.14 0.05 1 -5 0 284.66 5.18 2 -5 0 10.48 0.29 3 -5 0 60.16 1.14 4 -5 0 167.38 4.21 5 -5 0 34.58 0.92 6 -5 0 5.10 0.36 7 -5 0 33.07 1.44 8 -5 0 13.95 0.95 9 -5 0 57.37 2.12 10 -5 0 30.99 0.54 11 -5 0 5.99 0.20 12 -5 0 8.87 0.22 13 -5 0 5.44 0.18 -13 -4 0 1.66 0.09 -12 -4 0 1.14 0.08 -11 -4 0 25.13 0.45 -10 -4 0 32.91 0.40 -9 -4 0 3.27 0.38 -8 -4 0 28.09 1.03 -7 -4 0 0.94 0.13 -6 -4 0 2.13 0.17 -5 -4 0 35.32 0.90 -4 -4 0 182.65 3.24 -3 -4 0 114.79 2.06 -2 -4 0 179.79 3.42 -1 -4 0 35.88 0.70 0 -4 0 80.63 1.50 1 -4 0 35.89 0.68 2 -4 0 181.92 3.45 3 -4 0 114.16 2.09 4 -4 0 183.77 3.24 5 -4 0 33.93 0.71 6 -4 0 2.14 0.20 7 -4 0 0.88 0.30 8 -4 0 27.44 1.32 9 -4 0 4.15 0.62 10 -4 0 32.74 0.50 11 -4 0 25.00 0.42 12 -4 0 1.20 0.10 13 -4 0 1.76 0.12 -13 -3 0 7.81 0.17 -12 -3 0 12.83 0.25 -11 -3 0 6.09 0.16 -10 -3 0 12.93 0.21 -9 -3 0 17.66 0.81 -8 -3 0 20.79 0.86 -7 -3 0 12.16 0.37 -6 -3 0 25.46 0.56 -5 -3 0 19.70 1.02 -4 -3 0 22.52 0.62 -3 -3 0 29.04 0.68 -2 -3 0 57.57 1.11 -1 -3 0 54.71 0.98 0 -3 0 0.05 0.02 1 -3 0 55.51 1.00 2 -3 0 58.61 1.05 3 -3 0 28.59 0.63 4 -3 0 22.02 0.59 5 -3 0 18.46 0.48 6 -3 0 24.44 0.53 7 -3 0 11.40 0.59 8 -3 0 20.21 1.10 9 -3 0 19.01 1.07 10 -3 0 13.11 0.29 11 -3 0 6.27 0.25 12 -3 0 13.29 0.28 13 -3 0 7.50 0.17 -13 -2 0 2.84 0.11 -12 -2 0 8.34 0.18 -11 -2 0 8.13 0.17 -10 -2 0 1.82 0.09 -9 -2 0 13.80 0.71 -8 -2 0 5.89 0.50 -7 -2 0 15.18 0.55 -6 -2 0 34.14 0.68 -5 -2 0 19.60 0.71 -4 -2 0 159.44 2.95 -3 -2 0 140.01 2.15 -2 -2 0 183.01 3.69 -1 -2 0 298.72 5.28 1 -2 0 297.79 7.46 2 -2 0 185.92 3.51 3 -2 0 142.03 2.91 4 -2 0 157.67 2.91 5 -2 0 17.86 0.57 6 -2 0 32.67 0.64 7 -2 0 14.81 0.49 8 -2 0 6.28 0.70 9 -2 0 13.33 0.89 10 -2 0 1.71 0.14 11 -2 0 8.09 0.23 12 -2 0 8.65 0.21 13 -2 0 2.77 0.12 -13 -1 0 5.85 0.13 -12 -1 0 0.35 0.06 -11 -1 0 7.69 0.18 -10 -1 0 4.39 0.14 -9 -1 0 5.30 0.48 -8 -1 0 36.17 1.23 -7 -1 0 44.83 1.09 -6 -1 0 17.23 0.55 -5 -1 0 133.13 3.67 -4 -1 0 122.23 2.21 -3 -1 0 91.24 1.34 -2 -1 0 38.69 0.58 2 -1 0 38.87 0.71 3 -1 0 88.90 1.61 4 -1 0 121.29 2.16 5 -1 0 129.15 2.42 6 -1 0 16.42 0.48 7 -1 0 42.38 0.92 8 -1 0 35.40 1.01 9 -1 0 5.05 0.60 10 -1 0 4.47 0.19 11 -1 0 7.95 0.22 12 -1 0 0.35 0.06 13 -1 0 5.85 0.17 -13 0 0 4.55 0.11 -12 0 0 2.64 0.12 -11 0 0 1.27 0.08 -10 0 0 3.33 0.12 -9 0 0 15.25 0.74 -8 0 0 1.39 0.25 -7 0 0 5.83 0.25 -6 0 0 116.37 1.49 -5 0 0 283.92 8.48 -4 0 0 41.64 1.41 -3 0 0 407.22 6.03 -2 0 0 114.87 1.86 2 0 0 116.50 2.32 3 0 0 406.29 7.62 4 0 0 40.44 0.88 5 0 0 281.38 5.36 6 0 0 115.55 1.83 7 0 0 6.06 0.34 8 0 0 1.70 0.25 9 0 0 15.72 0.92 10 0 0 3.53 0.17 11 0 0 1.25 0.10 12 0 0 2.48 0.12 13 0 0 4.73 0.15 -13 1 0 5.70 0.14 -12 1 0 0.56 0.06 -11 1 0 7.56 0.16 -10 1 0 4.17 0.13 -9 1 0 5.45 0.51 -8 1 0 37.52 1.24 -7 1 0 43.62 0.83 -6 1 0 18.73 0.36 -5 1 0 140.90 3.68 -4 1 0 124.46 3.23 -3 1 0 91.95 1.62 -2 1 0 35.31 0.71 2 1 0 36.00 0.91 3 1 0 92.13 1.68 4 1 0 117.16 2.14 5 1 0 132.59 2.42 6 1 0 18.28 0.49 7 1 0 43.17 0.92 8 1 0 37.67 1.01 9 1 0 5.82 0.45 10 1 0 4.41 0.19 11 1 0 7.72 0.21 12 1 0 0.66 0.08 13 1 0 5.59 0.14 -13 2 0 2.62 0.10 -12 2 0 8.06 0.17 -11 2 0 7.60 0.16 -10 2 0 1.81 0.09 -9 2 0 14.50 0.71 -8 2 0 5.96 0.29 -7 2 0 16.38 0.36 -6 2 0 35.26 0.57 -5 2 0 19.02 0.93 -4 2 0 166.27 2.91 -3 2 0 140.42 2.85 -2 2 0 191.86 3.65 -1 2 0 295.11 5.27 1 2 0 299.63 5.17 2 2 0 195.79 3.65 3 2 0 143.55 2.82 4 2 0 166.04 2.94 5 2 0 18.59 0.88 6 2 0 35.76 0.75 7 2 0 16.91 0.50 8 2 0 5.36 0.39 9 2 0 13.92 0.58 10 2 0 1.78 0.12 11 2 0 8.02 0.25 12 2 0 8.01 0.22 13 2 0 2.75 0.10 -13 3 0 7.49 0.15 -12 3 0 13.19 0.27 -11 3 0 6.54 0.15 -10 3 0 13.31 0.20 -9 3 0 17.98 0.58 -8 3 0 22.28 0.62 -7 3 0 10.68 0.29 -6 3 0 27.02 0.47 -5 3 0 21.31 0.99 -4 3 0 22.21 0.58 -3 3 0 26.37 0.63 -2 3 0 58.87 1.08 -1 3 0 53.59 0.97 0 3 0 0.03 0.01 1 3 0 53.26 1.04 2 3 0 58.28 1.05 3 3 0 27.00 0.60 4 3 0 22.27 0.91 5 3 0 20.82 0.94 6 3 0 27.63 0.63 7 3 0 10.86 0.40 8 3 0 22.00 0.72 9 3 0 18.55 0.67 10 3 0 13.41 0.26 11 3 0 6.72 0.20 12 3 0 13.32 0.28 13 3 0 7.64 0.19 -13 4 0 1.75 0.08 -12 4 0 1.26 0.09 -11 4 0 24.53 0.32 -10 4 0 32.10 0.39 -9 4 0 3.65 0.28 -8 4 0 27.53 0.72 -7 4 0 0.74 0.11 -6 4 0 1.81 0.12 -5 4 0 34.39 0.82 -4 4 0 183.76 3.51 -3 4 0 108.59 1.99 -2 4 0 173.22 3.32 -1 4 0 33.30 0.68 0 4 0 80.92 1.28 1 4 0 33.01 0.66 2 4 0 176.78 3.51 3 4 0 111.68 2.02 4 4 0 187.92 4.61 5 4 0 34.73 0.87 6 4 0 1.97 0.18 7 4 0 0.75 0.14 8 4 0 27.13 0.81 9 4 0 3.96 0.35 10 4 0 31.79 0.45 11 4 0 24.84 0.41 12 4 0 1.27 0.10 13 4 0 1.71 0.10 -13 5 0 5.31 0.14 -12 5 0 8.65 0.17 -11 5 0 5.53 0.14 -10 5 0 30.91 0.34 -9 5 0 55.98 1.23 -8 5 0 14.89 0.49 -7 5 0 33.65 0.71 -6 5 0 5.64 0.20 -5 5 0 36.58 0.86 -4 5 0 166.61 2.95 -3 5 0 56.83 1.17 -2 5 0 11.28 0.35 -1 5 0 296.18 5.38 0 5 0 0.08 0.04 1 5 0 296.38 5.41 2 5 0 11.26 0.33 3 5 0 57.12 1.13 4 5 0 171.11 4.28 5 5 0 35.73 0.90 6 5 0 5.21 0.26 7 5 0 34.50 0.89 8 5 0 15.07 0.56 9 5 0 56.14 1.32 10 5 0 30.71 0.46 11 5 0 5.32 0.19 12 5 0 8.75 0.19 13 5 0 5.50 0.19 -13 6 0 1.42 0.16 -12 6 0 12.16 0.22 -11 6 0 4.14 0.13 -10 6 0 22.03 0.27 -9 6 0 4.13 0.26 -8 6 0 3.66 0.28 -7 6 0 12.30 0.41 -6 6 0 40.92 0.76 -5 6 0 101.24 1.52 -4 6 0 105.41 2.02 -3 6 0 53.84 1.12 -2 6 0 87.54 1.62 -1 6 0 237.51 3.69 0 6 0 12.52 0.27 1 6 0 238.61 4.52 2 6 0 88.04 1.58 3 6 0 52.81 1.07 4 6 0 105.89 2.93 5 6 0 99.70 1.55 6 6 0 40.88 0.81 7 6 0 11.33 0.45 8 6 0 3.64 0.32 9 6 0 4.08 0.33 10 6 0 21.86 0.37 11 6 0 4.15 0.17 12 6 0 12.28 0.25 -12 7 0 6.26 0.15 -11 7 0 7.21 0.14 -10 7 0 15.58 0.22 -9 7 0 9.21 0.16 -8 7 0 11.23 0.62 -7 7 0 29.11 1.05 -6 7 0 14.09 0.51 -5 7 0 159.28 1.94 -4 7 0 14.53 0.38 -3 7 0 6.58 0.31 -2 7 0 237.10 4.80 -1 7 0 16.49 0.47 0 7 0 0.26 0.05 1 7 0 16.16 0.43 2 7 0 238.11 4.72 3 7 0 6.71 0.29 4 7 0 14.38 0.47 5 7 0 156.29 2.28 6 7 0 14.09 0.42 7 7 0 29.05 0.79 8 7 0 11.75 0.69 9 7 0 9.22 0.23 10 7 0 15.51 0.33 11 7 0 7.16 0.22 12 7 0 6.29 0.17 -12 8 0 7.05 0.15 -11 8 0 7.36 0.15 -10 8 0 28.03 0.30 -9 8 0 0.60 0.05 -8 8 0 59.23 1.82 -7 8 0 31.83 1.13 -6 8 0 4.08 0.32 -5 8 0 17.50 0.36 -4 8 0 8.81 0.20 -3 8 0 89.94 1.77 -2 8 0 15.33 0.50 -1 8 0 101.69 1.90 0 8 0 89.94 2.41 1 8 0 101.85 1.84 2 8 0 15.99 0.48 3 8 0 90.27 1.72 4 8 0 8.51 0.35 5 8 0 17.35 0.58 6 8 0 3.26 0.30 7 8 0 32.45 1.22 8 8 0 60.18 1.90 9 8 0 0.55 0.08 10 8 0 27.71 0.41 11 8 0 7.41 0.22 12 8 0 7.05 0.20 -12 9 0 13.01 0.21 -11 9 0 8.65 0.16 -10 9 0 0.49 0.05 -9 9 0 5.88 0.14 -8 9 0 1.77 0.29 -7 9 0 31.48 1.12 -6 9 0 9.68 0.32 -5 9 0 35.50 0.59 -4 9 0 70.61 0.88 -3 9 0 12.99 0.29 -2 9 0 56.78 1.26 -1 9 0 219.04 3.89 0 9 0 0.03 0.07 1 9 0 219.04 5.65 2 9 0 56.99 1.21 3 9 0 12.97 0.36 4 9 0 70.10 1.44 5 9 0 35.66 0.92 6 9 0 9.60 0.46 7 9 0 30.17 1.17 8 9 0 1.72 0.32 9 9 0 5.74 0.20 10 9 0 0.54 0.07 11 9 0 8.66 0.23 12 9 0 13.10 0.24 -12 10 0 0.19 0.03 -11 10 0 7.10 0.14 -10 10 0 0.70 0.06 -9 10 0 17.52 0.23 -8 10 0 33.56 1.24 -7 10 0 31.01 1.14 -6 10 0 18.52 0.52 -5 10 0 38.19 0.69 -4 10 0 184.17 2.21 -3 10 0 20.78 0.35 -2 10 0 174.58 2.48 -1 10 0 40.32 0.99 0 10 0 248.53 6.84 1 10 0 43.07 1.41 2 10 0 172.05 3.00 3 10 0 20.72 0.40 4 10 0 180.27 3.22 5 10 0 38.21 0.99 6 10 0 18.37 0.83 7 10 0 32.25 1.22 8 10 0 34.47 1.30 9 10 0 17.48 0.32 10 10 0 0.75 0.08 11 10 0 6.95 0.20 12 10 0 0.17 0.04 -12 11 0 1.06 0.06 -11 11 0 0.29 0.04 -10 11 0 0.73 0.06 -9 11 0 1.94 0.08 -8 11 0 3.51 0.11 -7 11 0 11.08 0.62 -6 11 0 87.01 1.65 -5 11 0 100.03 1.47 -4 11 0 25.72 0.47 -3 11 0 154.08 1.73 -2 11 0 86.99 1.16 -1 11 0 5.86 0.21 1 11 0 5.92 0.21 2 11 0 86.16 1.30 3 11 0 152.68 2.20 4 11 0 24.89 0.92 5 11 0 96.84 1.98 6 11 0 91.17 2.48 7 11 0 12.11 0.69 8 11 0 3.40 0.17 9 11 0 1.95 0.13 10 11 0 0.73 0.08 11 11 0 0.29 0.06 12 11 0 0.91 0.07 -11 12 0 3.83 0.11 -10 12 0 0.54 0.05 -9 12 0 2.01 0.08 -8 12 0 6.06 0.14 -7 12 0 15.22 0.75 -6 12 0 85.74 1.62 -5 12 0 5.00 0.24 -4 12 0 5.66 0.20 -3 12 0 9.69 0.25 -2 12 0 38.60 0.59 -1 12 0 1.51 0.11 0 12 0 45.84 0.69 1 12 0 1.57 0.11 2 12 0 39.06 0.71 3 12 0 9.61 0.29 5 12 0 5.80 0.51 6 12 0 89.81 2.45 7 12 0 14.69 0.78 8 12 0 6.10 0.21 9 12 0 1.93 0.13 10 12 0 0.64 0.08 11 12 0 3.93 0.14 -11 13 0 0.40 0.05 -10 13 0 6.61 0.14 -9 13 0 7.60 0.15 -8 13 0 1.46 0.07 -7 13 0 26.53 0.37 -6 13 0 25.68 0.68 -5 13 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5.83 0.51 6 -15 3 8.15 0.85 7 -15 3 1.38 0.22 8 -15 3 15.94 0.53 9 -15 3 0.06 0.06 10 -15 3 6.96 0.31 -11 -14 3 2.38 0.11 -10 -14 3 1.35 0.11 -9 -14 3 2.26 0.13 -8 -14 3 10.10 0.24 -7 -14 3 7.67 0.27 -6 -14 3 9.29 0.46 -5 -14 3 83.78 1.77 -4 -14 3 25.98 1.14 -3 -14 3 36.77 1.40 -2 -14 3 20.62 0.96 -1 -14 3 2.92 0.32 0 -14 3 3.49 0.32 1 -14 3 62.48 2.00 2 -14 3 103.74 2.92 3 -14 3 40.32 1.58 4 -14 3 27.72 0.92 5 -14 3 24.54 0.91 7 -14 3 4.10 0.31 8 -14 3 1.33 0.20 9 -14 3 1.25 0.13 10 -14 3 3.29 0.13 -12 -13 3 0.84 0.09 -11 -13 3 0.78 0.07 -10 -13 3 5.02 0.18 -9 -13 3 6.24 0.20 -8 -13 3 1.94 0.14 -7 -13 3 4.86 0.53 -6 -13 3 38.75 1.03 -5 -13 3 9.09 0.42 -4 -13 3 42.86 1.02 -3 -13 3 2.48 0.31 -2 -13 3 2.98 0.32 -1 -13 3 23.71 0.78 0 -13 3 22.61 0.76 1 -13 3 64.61 1.29 2 -13 3 19.23 0.64 3 -13 3 53.18 1.81 4 -13 3 14.51 0.63 5 -13 3 30.09 1.00 6 -13 3 20.75 1.22 7 -13 3 3.24 0.55 8 -13 3 5.81 0.38 9 -13 3 1.34 0.18 10 -13 3 5.92 0.17 -12 -12 3 3.57 0.13 -11 -12 3 1.04 0.09 -10 -12 3 0.38 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79.06 2.53 2 -16 4 16.87 0.98 3 -16 4 18.22 1.06 4 -16 4 33.81 1.06 5 -16 4 1.94 0.31 6 -16 4 4.36 0.51 7 -16 4 1.65 0.28 8 -16 4 2.68 0.17 9 -16 4 0.89 0.08 -11 -15 4 1.75 0.09 -10 -15 4 5.38 0.17 -9 -15 4 4.16 0.17 -8 -15 4 32.26 0.58 -7 -15 4 17.93 0.38 -6 -15 4 2.47 0.21 -5 -15 4 20.87 1.07 -4 -15 4 16.74 0.93 -3 -15 4 28.36 1.24 -2 -15 4 36.01 1.45 -1 -15 4 20.43 1.00 0 -15 4 22.84 0.77 1 -15 4 21.14 1.05 2 -15 4 28.00 1.28 3 -15 4 22.74 1.19 4 -15 4 47.79 1.31 5 -15 4 35.93 1.60 6 -15 4 18.06 0.74 7 -15 4 4.06 0.45 8 -15 4 4.64 0.28 9 -15 4 8.02 0.23 -11 -14 4 6.17 0.16 -10 -14 4 3.48 0.16 -9 -14 4 7.95 0.22 -8 -14 4 7.28 0.22 -7 -14 4 1.11 0.12 -6 -14 4 11.96 0.53 -5 -14 4 21.66 0.71 -4 -14 4 1.89 0.37 -3 -14 4 60.62 2.00 -2 -14 4 27.06 1.15 -1 -14 4 86.35 2.55 0 -14 4 86.22 1.77 1 -14 4 6.64 0.66 2 -14 4 0.24 0.19 3 -14 4 19.29 1.01 4 -14 4 9.51 0.58 5 -14 4 10.36 0.84 6 -14 4 19.26 1.16 7 -14 4 4.53 0.49 8 -14 4 17.61 0.55 9 -14 4 2.99 0.17 -12 -13 4 4.23 0.16 -11 -13 4 3.62 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1.74 6 -7 4 61.46 2.30 7 -7 4 3.87 0.41 8 -7 4 17.03 0.74 9 -7 4 5.32 0.35 10 -7 4 1.27 0.16 11 -7 4 0.99 0.08 -13 -6 4 0.93 0.07 -12 -6 4 0.51 0.06 -11 -6 4 3.92 0.16 -10 -6 4 5.24 0.19 -9 -6 4 67.14 2.13 -8 -6 4 32.87 1.25 -7 -6 4 61.18 1.87 -6 -6 4 34.46 0.80 -5 -6 4 27.35 0.81 -4 -6 4 32.41 0.83 -3 -6 4 86.03 2.63 -2 -6 4 26.11 1.08 -1 -6 4 51.84 1.13 0 -6 4 52.89 1.18 1 -6 4 121.00 3.25 2 -6 4 61.44 1.95 3 -6 4 4.75 0.46 4 -6 4 142.69 2.66 5 -6 4 3.63 0.51 6 -6 4 17.18 1.05 7 -6 4 61.42 1.59 8 -6 4 5.39 0.45 9 -6 4 3.69 0.29 10 -6 4 5.36 0.31 11 -6 4 5.16 0.16 -13 -5 4 0.67 0.06 -12 -5 4 22.53 0.39 -11 -5 4 5.30 0.17 -10 -5 4 15.64 0.28 -9 -5 4 37.94 0.95 -8 -5 4 0.53 0.13 -7 -5 4 3.58 0.24 -6 -5 4 54.58 0.89 -5 -5 4 55.44 1.06 -4 -5 4 75.65 1.54 -3 -5 4 111.64 3.08 -2 -5 4 95.93 2.67 -1 -5 4 21.85 0.58 0 -5 4 4.80 0.33 1 -5 4 103.04 2.66 2 -5 4 35.45 1.31 3 -5 4 11.27 0.69 4 -5 4 47.71 1.17 5 -5 4 3.71 0.38 6 -5 4 15.20 0.95 7 -5 4 20.84 0.81 8 -5 4 15.94 0.71 9 -5 4 12.66 0.45 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10.83 0.70 -11 0 11 18.98 0.36 -10 0 11 2.01 0.23 -7 0 11 7.91 0.52 -6 0 11 0.44 0.18 -5 0 11 2.60 0.36 -4 0 11 4.69 0.48 -11 1 11 0.96 0.08 -10 1 11 24.24 0.56 -9 1 11 7.89 0.42 -7 1 11 9.44 0.58 -6 1 11 55.47 1.72 -5 1 11 9.00 0.57 -4 1 11 7.06 0.50 -11 2 11 10.85 0.21 -10 2 11 2.89 0.19 -9 2 11 7.57 0.42 -6 2 11 11.71 0.65 -5 2 11 2.28 0.34 -4 2 11 2.56 0.36 -11 3 11 4.06 0.12 -10 3 11 2.37 0.17 -9 3 11 3.71 0.33 -7 3 11 15.06 0.75 -6 3 11 1.80 0.31 -5 3 11 6.21 0.56 -4 3 11 5.74 0.53 -1 3 11 10.05 0.63 -11 4 11 5.97 0.14 -10 4 11 0.98 0.09 -9 4 11 7.98 0.29 -7 4 11 4.44 0.44 -6 4 11 2.01 0.32 -5 4 11 1.95 0.33 -4 4 11 3.79 0.45 -2 4 11 13.98 0.74 -1 4 11 27.22 1.12 0 4 11 8.38 0.59 -11 5 11 0.41 0.05 -10 5 11 6.20 0.19 -7 5 11 5.74 0.51 -6 5 11 12.19 0.67 -5 5 11 5.35 0.52 -4 5 11 13.96 0.74 -2 5 11 26.72 1.10 -1 5 11 6.36 0.58 0 5 11 16.67 0.86 -11 6 11 0.44 0.05 -10 6 11 7.55 0.21 -9 6 11 8.61 0.31 -8 6 11 11.17 0.49 -6 6 11 13.05 0.70 -5 6 11 12.05 0.68 -4 6 11 1.44 0.29 -3 6 11 23.28 1.00 -2 6 11 0.59 0.21 -1 6 11 15.83 0.82 0 6 11 21.52 0.99 1 6 11 2.65 0.39 -11 7 11 0.01 0.04 -10 7 11 9.84 0.24 -9 7 11 3.01 0.15 -8 7 11 5.25 0.32 -6 7 11 29.25 1.11 -5 7 11 9.21 0.59 -4 7 11 15.95 0.57 -3 7 11 7.73 0.54 -2 7 11 42.06 1.51 -1 7 11 5.59 0.55 0 7 11 7.45 0.65 1 7 11 1.58 0.32 5 7 11 9.95 0.41 -10 8 11 0.63 0.05 -9 8 11 13.01 0.29 -8 8 11 8.94 0.42 -7 8 11 3.54 0.28 -6 8 11 1.47 0.28 -5 8 11 3.02 0.38 -4 8 11 2.73 0.26 -3 8 11 32.07 1.23 -2 8 11 30.06 1.18 -1 8 11 13.23 0.74 0 8 11 2.67 0.39 -10 9 11 5.87 0.12 -9 9 11 0.70 0.08 -8 9 11 1.52 0.12 -7 9 11 1.06 0.17 -5 9 11 8.40 0.44 -4 9 11 2.10 0.23 -3 9 11 10.81 0.66 -2 9 11 37.57 1.38 -1 9 11 33.44 1.29 0 9 11 4.01 0.46 5 9 11 1.91 0.18 -10 10 11 1.76 0.09 -9 10 11 2.26 0.12 -8 10 11 6.08 0.19 -7 10 11 6.77 0.26 -6 10 11 4.13 0.46 -4 10 11 37.90 0.98 -3 10 11 3.91 0.45 -2 10 11 9.71 0.62 -1 10 11 16.46 0.85 3 10 11 7.26 0.40 4 10 11 1.26 0.16 -9 11 11 0.59 0.05 -8 11 11 6.77 0.19 -7 11 11 3.55 0.20 -6 11 11 13.42 0.40 -5 11 11 17.87 0.72 -4 11 11 26.69 0.93 3 11 11 0.85 0.14 4 11 11 2.17 0.19 -9 12 11 5.32 0.14 -8 12 11 0.33 0.05 -7 12 11 4.37 0.16 -6 12 11 15.73 0.43 -5 12 11 20.14 0.75 -4 12 11 12.53 0.55 1 12 11 6.41 0.37 2 12 11 3.44 0.30 3 12 11 4.30 0.23 4 12 11 5.39 0.27 -9 13 11 1.69 0.12 -8 13 11 0.85 0.06 -7 13 11 0.77 0.07 -6 13 11 0.12 0.07 -5 13 11 6.94 0.27 -4 13 11 9.90 0.48 -3 13 11 3.84 0.31 -2 13 11 14.18 0.58 -1 13 11 0.64 0.16 0 13 11 2.23 0.28 1 13 11 6.42 0.37 2 13 11 1.14 0.17 3 13 11 2.71 0.21 -8 14 11 9.90 0.19 -7 14 11 14.09 0.24 -6 14 11 5.49 0.18 -5 14 11 4.54 0.17 -4 14 11 8.98 0.32 -3 14 11 6.52 0.26 -2 14 11 0.73 0.16 -1 14 11 4.31 0.24 0 14 11 18.75 0.69 1 14 11 0.03 0.06 2 14 11 1.63 0.13 3 14 11 4.61 0.18 -7 15 11 0.25 0.04 -6 15 11 10.83 0.21 -5 15 11 4.60 0.16 -4 15 11 8.36 0.29 -3 15 11 3.08 0.18 -2 15 11 5.08 0.22 -1 15 11 1.60 0.14 0 15 11 1.74 0.15 1 15 11 0.18 0.05 2 15 11 0.16 0.04 -7 16 11 18.23 0.38 -6 16 11 1.02 0.06 -5 16 11 20.57 0.32 -4 16 11 2.82 0.14 -3 16 11 2.05 0.12 -2 16 11 4.43 0.19 -1 16 11 3.83 0.15 0 16 11 0.75 0.07 1 16 11 1.93 0.10 -6 17 11 4.52 0.22 -5 17 11 2.96 0.09 -4 17 11 11.85 0.21 -3 17 11 2.03 0.09 -2 17 11 6.80 0.18 -1 17 11 2.84 0.11 0 17 11 0.56 0.05 -4 18 11 3.30 0.16 -3 18 11 12.72 0.30 -2 18 11 4.49 0.14 -1 18 11 10.12 0.29 -9 -8 12 6.54 0.29 -10 -6 12 4.45 0.22 -10 -5 12 5.43 0.26 -10 -4 12 4.35 0.25 -5 -4 12 2.32 0.58 -10 -3 12 0.42 0.07 -10 -2 12 16.62 0.57 -10 -1 12 7.76 0.34 -9 -1 12 14.86 0.58 -11 0 12 0.54 0.13 -10 0 12 0.27 0.07 -10 1 12 7.66 0.25 -5 1 12 6.77 0.56 -10 2 12 18.80 0.44 -9 2 12 3.21 0.27 -5 2 12 1.80 0.30 -4 2 12 2.10 0.31 -10 3 12 0.51 0.07 -9 3 12 7.64 0.38 -5 3 12 3.76 0.40 -4 3 12 2.67 0.37 -10 4 12 4.89 0.19 -9 4 12 2.38 0.23 -8 4 12 18.16 0.65 -5 4 12 4.01 0.44 -4 4 12 0.77 0.22 -10 5 12 5.49 0.20 -9 5 12 9.35 0.29 -8 5 12 1.92 0.21 -4 5 12 0.84 0.23 -10 6 12 4.53 0.14 -9 6 12 2.06 0.14 -8 6 12 4.31 0.29 -4 6 12 7.25 0.63 -10 7 12 0.65 0.06 -9 7 12 4.59 0.19 -8 7 12 2.45 0.16 -7 7 12 10.13 0.44 -9 8 12 7.59 0.20 -8 8 12 5.84 0.22 -7 8 12 3.84 0.29 -9 9 12 0.08 0.03 -8 9 12 0.89 0.10 -7 9 12 24.06 0.54 -6 9 12 5.28 0.31 -9 10 12 11.14 0.23 -8 10 12 6.70 0.22 -7 10 12 2.15 0.14 -6 10 12 7.90 0.37 -5 10 12 0.79 0.16 3 10 12 9.40 0.37 -8 11 12 1.51 0.08 -7 11 12 1.07 0.10 -6 11 12 3.76 0.27 -5 11 12 1.86 0.22 3 11 12 3.56 0.34 -8 12 12 5.92 0.15 -7 12 12 6.49 0.17 -6 12 12 16.22 0.32 -5 12 12 2.11 0.22 -4 12 12 1.25 0.13 -3 12 12 5.06 0.32 -2 12 12 16.32 0.61 0 12 12 2.49 0.25 1 12 12 1.48 0.18 2 12 12 8.21 0.35 -7 13 12 19.02 0.32 -6 13 12 1.15 0.08 -5 13 12 3.33 0.18 -4 13 12 8.15 0.27 -3 13 12 0.96 0.16 -2 13 12 0.01 0.08 -1 13 12 3.21 0.26 0 13 12 3.39 0.18 1 13 12 2.89 0.22 2 13 12 0.92 0.13 -7 14 12 1.58 0.16 -6 14 12 5.72 0.13 -5 14 12 11.26 0.30 -4 14 12 4.46 0.19 -3 14 12 2.82 0.17 -2 14 12 5.50 0.20 -1 14 12 4.56 0.18 0 14 12 7.97 0.23 1 14 12 4.59 0.23 -6 15 12 0.53 0.08 -5 15 12 0.80 0.07 -4 15 12 0.02 0.04 -3 15 12 14.97 0.35 -2 15 12 1.31 0.09 -1 15 12 9.85 0.26 0 15 12 1.84 0.12 -4 16 12 5.53 0.17 -3 16 12 5.96 0.18 -2 16 12 14.97 0.29 -9 -4 13 1.64 0.17 -9 -2 13 4.81 0.24 -9 1 13 8.72 0.37 -9 2 13 5.15 0.27 -9 3 13 5.11 0.19 -9 4 13 1.75 0.11 -9 5 13 0.75 0.08 -8 5 13 4.90 0.25 -9 6 13 7.53 0.22 -8 6 13 3.57 0.22 -9 7 13 8.27 0.40 -8 7 13 7.34 0.32 -7 7 13 10.73 0.41 -8 8 13 2.04 0.12 -7 8 13 3.32 0.21 -8 9 13 0.59 0.07 -7 9 13 1.00 0.12 -7 10 13 16.27 0.36 -6 10 13 1.47 0.10 -5 10 13 6.46 0.30 -4 10 13 8.59 0.38 -7 11 13 0.67 0.10 -6 11 13 14.19 0.33 -5 11 13 2.35 0.19 -4 11 13 0.10 0.08 -2 11 13 0.23 0.09 0 11 13 1.08 0.15 -6 12 13 3.50 0.19 -5 12 13 4.86 0.23 -4 12 13 11.70 0.43 -3 12 13 4.57 0.26 -2 12 13 1.70 0.16 -1 12 13 0.47 0.10 -5 13 13 1.85 0.15 -4 13 13 4.98 0.23 -3 13 13 0.36 0.09 -2 13 13 10.22 0.37 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 60593 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, 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 NiA Ni 0.14148(3) 0.39370(2) 0.23359(2) 0.02371(7) Uani 1 1 d . . O1A O 0.19647(14) 0.31345(6) 0.26598(12) 0.0323(3) Uani 1 1 d . . O2A O 0.22016(14) 0.22328(6) 0.18590(12) 0.0349(3) Uani 1 1 d . . O3A O 0.17926(14) 0.57339(7) 0.26247(13) 0.0349(3) Uani 1 1 d . . N1A N 0.05570(14) 0.36441(7) 0.09023(13) 0.0220(3) Uani 1 1 d . . N2A N 0.09388(14) 0.47581(7) 0.20712(13) 0.0236(3) Uani 1 1 d . . N3A N 0.23053(15) 0.42037(8) 0.38569(14) 0.0287(3) Uani 1 1 d . . C1A C 0.18216(17) 0.27646(8) 0.17936(16) 0.0262(3) Uani 1 1 d . . C2A C 0.11418(16) 0.30483(8) 0.06283(15) 0.0233(3) Uani 1 1 d . . C3A C 0.21569(19) 0.32658(9) 0.00367(17) 0.0297(4) Uani 1 1 d . . H3A H 0.1744 0.3520 -0.0633 0.036 Uiso 1 1 calc R U H3B H 0.2746 0.3540 0.0571 0.036 Uiso 1 1 calc R U C4A C 0.2919(2) 0.27545(11) -0.0362(2) 0.0434(5) Uani 1 1 d . . H4A H 0.2976 0.2388 0.0153 0.052 Uiso 1 1 calc R U C5A C 0.4242(3) 0.29924(16) -0.0274(3) 0.0647(8) Uani 1 1 d . . H5A H 0.4626 0.3126 0.0508 0.078 Uiso 1 1 calc R U H5B H 0.4741 0.2659 -0.0483 0.078 Uiso 1 1 calc R U H5C H 0.4205 0.3345 -0.0792 0.078 Uiso 1 1 calc R U C6A C 0.2314(4) 0.25465(16) -0.1576(3) 0.0680(9) Uani 1 1 d . . H6A H 0.1469 0.2395 -0.1627 0.082 Uiso 1 1 calc R U H6B H 0.2274 0.2898 -0.2096 0.082 Uiso 1 1 calc R U H6C H 0.2810 0.2212 -0.1787 0.082 Uiso 1 1 calc R U C7A C 0.02782(18) 0.25411(8) -0.00247(17) 0.0301(4) Uani 1 1 d . . H7A H 0.0777 0.2184 -0.0143 0.036 Uiso 1 1 calc R U H7B H -0.0303 0.2411 0.0415 0.036 Uiso 1 1 calc R U H7C H -0.0192 0.2704 -0.0763 0.036 Uiso 1 1 calc R U C8A C -0.03824(15) 0.39191(8) 0.02126(14) 0.0217(3) Uani 1 1 d . . C9A C -0.11423(16) 0.36161(8) -0.08547(15) 0.0234(3) Uani 1 1 d . . C10A C -0.21704(17) 0.32602(9) -0.07891(17) 0.0278(4) Uani 1 1 d . . H10A H -0.2378 0.3213 -0.0084 0.033 Uiso 1 1 calc R U C11A C -0.28880(17) 0.29754(9) -0.17655(19) 0.0335(4) Uani 1 1 d . . H11A H -0.3575 0.2722 -0.1723 0.040 Uiso 1 1 calc R U C12A C -0.2605(2) 0.30585(10) -0.28000(19) 0.0380(5) Uani 1 1 d . . H12A H -0.3100 0.2863 -0.3465 0.046 Uiso 1 1 calc R U C13A C -0.1606(2) 0.34249(10) -0.28667(17) 0.0338(4) Uani 1 1 d . . H13A H -0.1424 0.3485 -0.3580 0.041 Uiso 1 1 calc R U C14A C -0.08618(18) 0.37072(8) -0.18924(16) 0.0266(3) Uani 1 1 d . . H14A H -0.0173 0.3958 -0.1938 0.032 Uiso 1 1 calc R U C15A C -0.07929(16) 0.45508(8) 0.04172(15) 0.0222(3) Uani 1 1 d . . C16A C -0.01371(15) 0.49568(8) 0.12866(15) 0.0226(3) Uani 1 1 d . . C17A C -0.06309(17) 0.55591(8) 0.13477(16) 0.0270(4) Uani 1 1 d . . H17A H -0.0224 0.5830 0.1946 0.032 Uiso 1 1 calc R U C18A C -0.16838(17) 0.57610(9) 0.05628(18) 0.0296(4) Uani 1 1 d . . H18A H -0.1979 0.6171 0.0616 0.036 Uiso 1 1 calc R U C19A C -0.23231(18) 0.53737(9) -0.03075(17) 0.0308(4) Uani 1 1 d . . H19A H -0.3044 0.5516 -0.0855 0.037 Uiso 1 1 calc R U C20A C -0.18869(17) 0.47767(9) -0.03585(16) 0.0269(3) Uani 1 1 d . . H20A H -0.2338 0.4506 -0.0937 0.032 Uiso 1 1 calc R U C21A C 0.17372(17) 0.51734(9) 0.27531(16) 0.0270(4) Uani 1 1 d . . C22A C 0.26585(17) 0.48658(9) 0.37379(16) 0.0284(4) Uani 1 1 d . . H22A H 0.2662 0.5094 0.4455 0.034 Uiso 1 1 calc R U C23A C 0.40048(19) 0.48514(10) 0.35890(19) 0.0361(4) Uani 1 1 d . . H23A H 0.4030 0.5031 0.2846 0.043 Uiso 1 1 calc R U H23B H 0.4581 0.5088 0.4204 0.043 Uiso 1 1 calc R U C24A C 0.4353(2) 0.41625(12) 0.3650(2) 0.0431(5) Uani 1 1 d . . H24A H 0.4180 0.3978 0.2880 0.052 Uiso 1 1 calc R U H24B H 0.5245 0.4102 0.4041 0.052 Uiso 1 1 calc R U C25A C 0.35290(19) 0.38828(11) 0.43255(18) 0.0389(5) Uani 1 1 d . . H25A H 0.3448 0.3428 0.4206 0.047 Uiso 1 1 calc R U H25B H 0.3859 0.3968 0.5148 0.047 Uiso 1 1 calc R U C26A C 0.1500(2) 0.41267(10) 0.46696(17) 0.0350(4) Uani 1 1 d . . H26A H 0.1947 0.4302 0.5416 0.042 Uiso 1 1 calc R U H26B H 0.1383 0.3677 0.4780 0.042 Uiso 1 1 calc R U C27A C 0.0236(2) 0.44290(10) 0.42951(17) 0.0337(4) Uani 1 1 d . . C28A C -0.0780(2) 0.41070(10) 0.36288(19) 0.0391(5) Uani 1 1 d . . H28A H -0.0670 0.3695 0.3393 0.047 Uiso 1 1 calc R U C29A C -0.1952(2) 0.43801(12) 0.3304(2) 0.0456(5) Uani 1 1 d . . H29A H -0.2638 0.4154 0.2851 0.055 Uiso 1 1 calc R U C30A C -0.2124(2) 0.49840(13) 0.3642(2) 0.0477(5) Uani 1 1 d . . H30A H -0.2926 0.5171 0.3426 0.057 Uiso 1 1 calc R U C31A C -0.1115(3) 0.53116(12) 0.4297(2) 0.0465(5) Uani 1 1 d . . H31A H -0.1225 0.5726 0.4521 0.056 Uiso 1 1 calc R U C32A C 0.0054(2) 0.50368(11) 0.46278(19) 0.0402(5) Uani 1 1 d . . H32A H 0.0737 0.5263 0.5084 0.048 Uiso 1 1 calc R U NiB Ni 0.23908(3) 0.62098(2) 0.78504(2) 0.02293(7) Uani 1 1 d . . O1B O 0.21450(14) 0.70024(6) 0.83189(12) 0.0318(3) Uani 1 1 d . . O2B O 0.23562(16) 0.79988(7) 0.79523(14) 0.0399(3) Uani 1 1 d . . O3B O 0.17474(15) 0.44128(7) 0.74755(14) 0.0367(3) Uani 1 1 d . . N1B N 0.33989(13) 0.65679(7) 0.69959(13) 0.0229(3) Uani 1 1 d . . N2B N 0.26718(14) 0.53906(7) 0.75422(13) 0.0242(3) Uani 1 1 d . . N3B N 0.11644(15) 0.59058(7) 0.86059(14) 0.0267(3) Uani 1 1 d . . C1B C 0.25020(18) 0.74493(9) 0.77698(16) 0.0290(4) Uani 1 1 d . . C2B C 0.31224(17) 0.72525(8) 0.68193(16) 0.0248(3) Uani 1 1 d . . C3B C 0.22128(18) 0.73824(9) 0.56498(16) 0.0288(4) Uani 1 1 d . . H3C H 0.2021 0.7832 0.5609 0.035 Uiso 1 1 calc R U H3D H 0.2656 0.7293 0.5059 0.035 Uiso 1 1 calc R U C4B C 0.09677(18) 0.70279(9) 0.53316(19) 0.0340(4) Uani 1 1 d . . H4B H 0.1115 0.6604 0.5674 0.041 Uiso 1 1 calc R U C5B C -0.0035(2) 0.73409(13) 0.5787(3) 0.0484(6) Uani 1 1 d . . H5D H 0.0263 0.7386 0.6614 0.058 Uiso 1 1 calc R U H5E H -0.0222 0.7752 0.5436 0.058 Uiso 1 1 calc R U H5F H -0.0792 0.7086 0.5602 0.058 Uiso 1 1 calc R U C6B C 0.0510(2) 0.69550(13) 0.4040(2) 0.0504(6) Uani 1 1 d . . H6D H 0.1158 0.6754 0.3752 0.060 Uiso 1 1 calc R U H6E H -0.0247 0.6700 0.3853 0.060 Uiso 1 1 calc R U H6F H 0.0324 0.7365 0.3688 0.060 Uiso 1 1 calc R U C7B C 0.4286(2) 0.76611(9) 0.6967(2) 0.0353(4) Uani 1 1 d . . H7D H 0.4034 0.8097 0.6840 0.042 Uiso 1 1 calc R U H7E H 0.4822 0.7611 0.7740 0.042 Uiso 1 1 calc R U H7F H 0.4744 0.7536 0.6414 0.042 Uiso 1 1 calc R U C8B C 0.41196(14) 0.62665(8) 0.64961(14) 0.0219(3) Uani 1 1 d . . C9B C 0.46484(16) 0.65313(8) 0.55778(15) 0.0238(3) Uani 1 1 d . . C10B C 0.58133(17) 0.68174(10) 0.57911(19) 0.0355(4) Uani 1 1 d . . H10B H 0.6298 0.6879 0.6550 0.043 Uiso 1 1 calc R U C11B C 0.6255(2) 0.70113(12) 0.4875(3) 0.0501(6) Uani 1 1 d . . H11B H 0.7035 0.7218 0.5013 0.060 Uiso 1 1 calc R U C12B C 0.5574(3) 0.69071(14) 0.3768(2) 0.0540(6) Uani 1 1 d . . H12B H 0.5891 0.7039 0.3152 0.065 Uiso 1 1 calc R U C13B C 0.4439(2) 0.66130(11) 0.35559(19) 0.0417(5) Uani 1 1 d . . H13B H 0.3973 0.6538 0.2795 0.050 Uiso 1 1 calc R U C14B C 0.39755(17) 0.64258(8) 0.44603(16) 0.0272(3) Uani 1 1 d . . H14B H 0.3190 0.6223 0.4313 0.033 Uiso 1 1 calc R U C15B C 0.44465(16) 0.56071(8) 0.67616(15) 0.0239(3) Uani 1 1 d . . C16B C 0.37626(17) 0.51951(8) 0.72812(15) 0.0244(3) Uani 1 1 d . . C17B C 0.42413(19) 0.45912(9) 0.75627(18) 0.0319(4) Uani 1 1 d . . H17B H 0.3809 0.4314 0.7934 0.038 Uiso 1 1 calc R U C18B C 0.5320(2) 0.43952(10) 0.73110(18) 0.0356(4) Uani 1 1 d . . H18B H 0.5622 0.3987 0.7514 0.043 Uiso 1 1 calc R U C19B C 0.59721(18) 0.47866(10) 0.67642(18) 0.0346(4) Uani 1 1 d . . H19B H 0.6706 0.4647 0.6577 0.041 Uiso 1 1 calc R U C20B C 0.55361(17) 0.53821(10) 0.64967(16) 0.0296(4) Uani 1 1 d . . H20B H 0.5982 0.5650 0.6122 0.035 Uiso 1 1 calc R U C21B C 0.18138(17) 0.49688(9) 0.77136(16) 0.0271(4) Uani 1 1 d . . C22B C 0.08385(18) 0.52484(8) 0.82317(16) 0.0278(4) Uani 1 1 d . . H22B H 0.0796 0.4996 0.8911 0.033 Uiso 1 1 calc R U C23B C -0.04735(18) 0.52674(9) 0.73931(18) 0.0326(4) Uani 1 1 d . . H23C H -0.0489 0.5031 0.6692 0.039 Uiso 1 1 calc R U H23D H -0.1108 0.5094 0.7747 0.039 Uiso 1 1 calc R U C24B C -0.07046(19) 0.59564(10) 0.71332(19) 0.0354(4) Uani 1 1 d . . H24C H -0.0341 0.6091 0.6510 0.043 Uiso 1 1 calc R U H24D H -0.1607 0.6053 0.6925 0.043 Uiso 1 1 calc R U C25B C -0.00435(17) 0.62567(10) 0.82489(18) 0.0328(4) Uani 1 1 d . . H25C H 0.0106 0.6703 0.8145 0.039 Uiso 1 1 calc R U H25D H -0.0533 0.6211 0.8818 0.039 Uiso 1 1 calc R U C26B C 0.16956(19) 0.59606(10) 0.98671(17) 0.0316(4) Uani 1 1 d . . H26C H 0.1141 0.5741 1.0258 0.038 Uiso 1 1 calc R U H26D H 0.1716 0.6404 1.0085 0.038 Uiso 1 1 calc R U C27B C 0.2990(2) 0.56955(11) 1.02657(16) 0.0334(4) Uani 1 1 d . . C28B C 0.4017(2) 0.60878(12) 1.0466(2) 0.0429(5) Uani 1 1 d . . H28B H 0.3897 0.6523 1.0358 0.051 Uiso 1 1 calc R U C29B C 0.5217(2) 0.58497(15) 1.0823(3) 0.0556(7) Uani 1 1 d . . H29B H 0.5911 0.6123 1.0976 0.067 Uiso 1 1 calc R U C30B C 0.5408(2) 0.52170(15) 1.0958(2) 0.0527(6) Uani 1 1 d . . H30B H 0.6231 0.5055 1.1188 0.063 Uiso 1 1 calc R U C31B C 0.4397(2) 0.48224(14) 1.0755(2) 0.0484(6) Uani 1 1 d . . H31B H 0.4524 0.4387 1.0838 0.058 Uiso 1 1 calc R U C32B C 0.3196(2) 0.50588(12) 1.04318(19) 0.0408(5) Uani 1 1 d . . H32B H 0.2505 0.4785 1.0322 0.049 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 NiA 0.02795(14) 0.02263(14) 0.01782(14) -0.00191(11) 0.00104(10) -0.00077(11) O1A 0.0422(7) 0.0269(6) 0.0221(7) 0.0009(5) -0.0017(5) 0.0023(5) O2A 0.0417(7) 0.0262(7) 0.0315(7) 0.0027(5) -0.0002(6) 0.0048(6) O3A 0.0370(7) 0.0268(7) 0.0368(8) -0.0040(6) 0.0020(6) -0.0075(5) N1A 0.0259(7) 0.0201(6) 0.0199(7) -0.0007(5) 0.0055(5) -0.0006(5) N2A 0.0263(7) 0.0237(7) 0.0197(7) -0.0031(5) 0.0040(6) -0.0027(6) N3A 0.0320(8) 0.0286(8) 0.0213(8) -0.0022(6) -0.0002(6) -0.0014(6) C1A 0.0275(8) 0.0244(8) 0.0245(9) 0.0018(7) 0.0025(7) -0.0013(6) C2A 0.0264(8) 0.0207(8) 0.0217(8) -0.0004(6) 0.0044(6) 0.0020(6) C3A 0.0323(9) 0.0286(9) 0.0300(10) 0.0037(7) 0.0114(7) 0.0043(7) C4A 0.0479(12) 0.0414(11) 0.0485(13) 0.0087(10) 0.0263(10) 0.0163(10) C5A 0.0496(14) 0.0730(19) 0.084(2) 0.0237(17) 0.0404(15) 0.0218(14) C6A 0.090(2) 0.0705(19) 0.0535(18) -0.0136(14) 0.0370(16) 0.0153(17) C7A 0.0352(9) 0.0219(8) 0.0282(9) -0.0019(7) -0.0010(7) 0.0018(7) C8A 0.0230(7) 0.0238(7) 0.0183(7) -0.0003(7) 0.0055(6) -0.0020(6) C9A 0.0251(8) 0.0199(8) 0.0230(9) -0.0019(6) 0.0021(6) 0.0025(6) C10A 0.0260(8) 0.0274(9) 0.0290(10) -0.0020(7) 0.0052(7) 0.0017(6) C11A 0.0253(8) 0.0301(9) 0.0417(11) -0.0101(8) 0.0025(8) -0.0016(7) C12A 0.0374(10) 0.0375(11) 0.0325(11) -0.0148(8) -0.0026(8) 0.0039(8) C13A 0.0431(11) 0.0339(10) 0.0223(10) -0.0051(7) 0.0047(8) 0.0068(8) C14A 0.0335(9) 0.0216(7) 0.0238(9) 0.0001(6) 0.0058(7) 0.0028(7) C15A 0.0243(8) 0.0235(8) 0.0198(8) -0.0001(6) 0.0078(6) -0.0001(6) C16A 0.0242(7) 0.0239(8) 0.0217(8) 0.0000(6) 0.0095(6) -0.0020(6) C17A 0.0282(8) 0.0251(8) 0.0303(9) -0.0046(7) 0.0121(7) -0.0018(6) C18A 0.0290(8) 0.0251(8) 0.0379(11) -0.0019(7) 0.0143(8) 0.0033(7) C19A 0.0284(8) 0.0324(9) 0.0306(10) -0.0003(8) 0.0059(7) 0.0071(7) C20A 0.0258(8) 0.0294(9) 0.0247(9) -0.0028(7) 0.0050(7) 0.0029(7) C21A 0.0276(8) 0.0291(9) 0.0238(9) -0.0053(7) 0.0059(7) -0.0036(7) C22A 0.0296(9) 0.0295(9) 0.0236(9) -0.0073(7) 0.0024(7) -0.0044(7) C23A 0.0299(9) 0.0415(11) 0.0338(11) -0.0059(8) 0.0028(8) -0.0012(8) C24A 0.0330(10) 0.0456(12) 0.0453(13) -0.0112(9) 0.0008(9) 0.0043(9) C25A 0.0376(10) 0.0379(10) 0.0303(10) -0.0048(9) -0.0108(8) 0.0042(9) C26A 0.0456(11) 0.0372(10) 0.0202(9) 0.0005(7) 0.0050(8) -0.0050(8) C27A 0.0422(10) 0.0378(10) 0.0228(9) -0.0007(8) 0.0114(8) -0.0059(8) C28A 0.0461(11) 0.0366(11) 0.0356(11) -0.0011(8) 0.0124(9) -0.0086(8) C29A 0.0432(12) 0.0496(13) 0.0426(13) -0.0016(10) 0.0088(9) -0.0097(10) C30A 0.0460(12) 0.0557(14) 0.0421(13) 0.0012(11) 0.0128(10) 0.0044(11) C31A 0.0580(14) 0.0439(12) 0.0399(13) -0.0080(10) 0.0168(10) 0.0030(10) C32A 0.0502(12) 0.0437(12) 0.0280(11) -0.0094(9) 0.0124(9) -0.0069(9) NiB 0.02891(14) 0.02109(14) 0.02176(15) -0.00007(11) 0.01191(11) 0.00067(11) O1B 0.0435(7) 0.0253(6) 0.0325(7) -0.0029(5) 0.0205(6) -0.0001(5) O2B 0.0583(9) 0.0245(7) 0.0418(9) -0.0031(6) 0.0219(7) 0.0045(6) O3B 0.0445(8) 0.0250(7) 0.0435(9) -0.0037(6) 0.0167(6) -0.0053(6) N1B 0.0252(6) 0.0237(7) 0.0195(7) 0.0009(5) 0.0053(5) 0.0002(5) N2B 0.0301(7) 0.0223(7) 0.0214(7) 0.0016(5) 0.0091(6) 0.0006(6) N3B 0.0304(7) 0.0273(7) 0.0251(8) -0.0012(6) 0.0119(6) -0.0011(6) C1B 0.0353(9) 0.0258(9) 0.0272(10) -0.0018(7) 0.0103(7) 0.0019(7) C2B 0.0306(8) 0.0196(8) 0.0259(9) 0.0010(6) 0.0105(7) 0.0003(6) C3B 0.0336(9) 0.0248(8) 0.0287(9) 0.0055(7) 0.0093(7) 0.0037(7) C4B 0.0323(9) 0.0266(9) 0.0400(11) 0.0067(8) 0.0037(8) 0.0016(7) C5B 0.0323(10) 0.0510(13) 0.0614(16) 0.0085(11) 0.0115(10) 0.0060(9) C6B 0.0501(13) 0.0493(13) 0.0426(14) -0.0036(10) -0.0044(10) 0.0002(10) C7B 0.0371(10) 0.0265(9) 0.0440(12) -0.0048(8) 0.0136(9) -0.0071(8) C8B 0.0200(7) 0.0269(8) 0.0174(8) -0.0004(6) 0.0024(5) -0.0009(6) C9B 0.0232(7) 0.0248(8) 0.0238(9) -0.0012(6) 0.0069(6) -0.0006(6) C10B 0.0236(8) 0.0403(10) 0.0421(12) -0.0064(9) 0.0075(8) -0.0054(8) C11B 0.0352(11) 0.0468(13) 0.0781(19) 0.0014(12) 0.0323(12) -0.0082(9) C12B 0.0630(15) 0.0583(15) 0.0544(16) 0.0132(12) 0.0399(13) 0.0017(12) C13B 0.0571(13) 0.0446(12) 0.0275(11) 0.0042(9) 0.0184(9) 0.0060(10) C14B 0.0301(8) 0.0277(8) 0.0240(9) -0.0020(7) 0.0074(7) -0.0008(7) C15B 0.0234(8) 0.0281(8) 0.0185(8) -0.0014(6) 0.0026(6) 0.0039(6) C16B 0.0287(8) 0.0263(8) 0.0168(8) -0.0011(6) 0.0036(6) 0.0031(7) C17B 0.0362(10) 0.0282(9) 0.0287(10) 0.0035(7) 0.0037(7) 0.0053(7) C18B 0.0372(10) 0.0304(9) 0.0324(10) -0.0013(8) -0.0031(8) 0.0123(8) C19B 0.0272(9) 0.0396(11) 0.0331(10) -0.0062(8) 0.0011(7) 0.0108(8) C20B 0.0236(8) 0.0375(10) 0.0266(9) -0.0027(8) 0.0046(7) 0.0038(7) C21B 0.0335(9) 0.0251(9) 0.0235(9) 0.0011(7) 0.0089(7) -0.0016(7) C22B 0.0321(9) 0.0270(9) 0.0264(9) 0.0003(7) 0.0113(7) -0.0055(7) C23B 0.0304(9) 0.0351(10) 0.0332(10) 0.0002(8) 0.0100(8) -0.0061(7) C24B 0.0317(9) 0.0364(10) 0.0382(12) 0.0016(8) 0.0090(8) -0.0009(8) C25B 0.0301(9) 0.0338(9) 0.0382(10) -0.0004(8) 0.0153(8) 0.0031(8) C26B 0.0375(10) 0.0381(10) 0.0237(10) -0.0021(7) 0.0159(7) -0.0045(8) C27B 0.0373(10) 0.0458(11) 0.0194(9) -0.0012(8) 0.0118(7) -0.0063(8) C28B 0.0398(11) 0.0513(14) 0.0406(13) -0.0078(9) 0.0158(9) -0.0091(9) C29B 0.0381(12) 0.0755(19) 0.0556(16) -0.0059(14) 0.0167(11) -0.0116(12) C30B 0.0390(11) 0.082(2) 0.0390(13) 0.0076(12) 0.0141(10) 0.0082(12) C31B 0.0522(13) 0.0595(15) 0.0345(12) 0.0132(10) 0.0131(10) 0.0083(11) C32B 0.0441(11) 0.0479(12) 0.0294(11) 0.0078(9) 0.0079(8) -0.0043(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 '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 O1A NiA N2A 176.83(7) O1A NiA N1A 86.76(6) N2A NiA N1A 96.12(7) O1A NiA N3A 90.85(6) N2A NiA N3A 86.29(7) N1A NiA N3A 177.36(7) C1A O1A NiA 116.00(12) C8A N1A C2A 124.22(15) C8A N1A NiA 125.38(12) C2A N1A NiA 110.36(11) C21A N2A C16A 121.27(15) C21A N2A NiA 113.95(13) C16A N2A NiA 124.75(12) C22A N3A C25A 103.97(15) C22A N3A C26A 112.59(15) C25A N3A C26A 109.51(16) C22A N3A NiA 105.71(11) C25A N3A NiA 114.39(13) C26A N3A NiA 110.52(12) O2A C1A O1A 123.89(17) O2A C1A C2A 120.66(16) O1A C1A C2A 115.44(15) N1A C2A C7A 118.13(14) N1A C2A C1A 105.53(14) C7A C2A C1A 106.53(14) N1A C2A C3A 104.48(13) C7A C2A C3A 113.90(15) C1A C2A C3A 107.58(14) C4A C3A C2A 116.91(16) C6A C4A C5A 109.9(2) C6A C4A C3A 112.1(2) C5A C4A C3A 109.5(2) N1A C8A C15A 122.83(15) N1A C8A C9A 122.50(16) C15A C8A C9A 114.66(14) C14A C9A C10A 120.60(17) C14A C9A C8A 121.04(16) C10A C9A C8A 118.30(16) C11A C10A C9A 119.35(18) C12A C11A C10A 120.31(19) C13A C12A C11A 120.14(18) C12A C13A C14A 120.44(19) C9A C14A C13A 119.12(18) C20A C15A C16A 118.07(16) C20A C15A C8A 116.93(15) C16A C15A C8A 124.90(15) N2A C16A C17A 121.41(16) N2A C16A C15A 120.40(15) C17A C16A C15A 118.16(16) C18A C17A C16A 121.60(17) C17A C18A C19A 120.93(17) C20A C19A C18A 118.50(18) C19A C20A C15A 122.66(18) O3A C21A N2A 127.70(18) O3A C21A C22A 119.24(16) N2A C21A C22A 113.03(16) N3A C22A C21A 110.71(14) N3A C22A C23A 106.08(16) C21A C22A C23A 113.00(16) C24A C23A C22A 104.64(17) C25A C24A C23A 103.44(19) N3A C25A C24A 103.15(17) N3A C26A C27A 114.80(16) C28A C27A C32A 118.6(2) C28A C27A C26A 120.8(2) C32A C27A C26A 120.64(19) C29A C28A C27A 120.9(2) C28A C29A C30A 120.1(2) C31A C30A C29A 119.5(2) C30A C31A C32A 120.3(2) C31A C32A C27A 120.6(2) O1B NiB N2B 173.87(7) O1B NiB N1B 87.04(6) N2B NiB N1B 97.09(7) O1B NiB N3B 89.28(6) N2B NiB N3B 87.15(7) N1B NiB N3B 172.20(7) C1B O1B NiB 116.14(12) C8B N1B C2B 123.30(15) C8B N1B NiB 125.61(12) C2B N1B NiB 110.55(11) C21B N2B C16B 120.91(15) C21B N2B NiB 116.19(12) C16B N2B NiB 122.48(12) C26B N3B C22B 112.60(15) C26B N3B C25B 109.96(15) C22B N3B C25B 105.04(15) C26B N3B NiB 108.64(11) C22B N3B NiB 108.50(11) C25B N3B NiB 112.12(12) O2B C1B O1B 123.69(18) O2B C1B C2B 120.36(17) O1B C1B C2B 115.94(16) N1B C2B C7B 114.15(15) N1B C2B C3B 111.64(14) C7B C2B C3B 109.51(15) N1B C2B C1B 105.91(14) C7B C2B C1B 106.24(15) C3B C2B C1B 109.09(15) C4B C3B C2B 118.24(15) C5B C4B C6B 109.82(19) C5B C4B C3B 112.53(18) C6B C4B C3B 110.32(18) N1B C8B C15B 121.57(15) N1B C8B C9B 124.47(16) C15B C8B C9B 113.90(14) C14B C9B C10B 119.44(17) C14B C9B C8B 116.78(15) C10B C9B C8B 123.47(17) C11B C10B C9B 119.0(2) C12B C11B C10B 121.0(2) C13B C12B C11B 120.1(2) C12B C13B C14B 119.7(2) C9B C14B C13B 120.76(19) C20B C15B C16B 118.38(17) C20B C15B C8B 117.01(17) C16B C15B C8B 124.59(15) N2B C16B C17B 121.13(17) N2B C16B C15B 120.65(16) C17B C16B C15B 118.19(17) C18B C17B C16B 121.48(19) C17B C18B C19B 120.82(18) C20B C19B C18B 118.87(18) C19B C20B C15B 122.19(19) O3B C21B N2B 127.66(18) O3B C21B C22B 118.70(17) N2B C21B C22B 113.62(15) N3B C22B C21B 111.06(14) N3B C22B C23B 106.65(15) C21B C22B C23B 112.92(16) C24B C23B C22B 103.97(16) C25B C24B C23B 102.34(17) N3B C25B C24B 103.53(15) N3B C26B C27B 112.91(15) C28B C27B C32B 118.4(2) C28B C27B C26B 119.9(2) C32B C27B C26B 121.70(19) C29B C28B C27B 120.5(2) C30B C29B C28B 120.5(2) C31B C30B C29B 119.6(2) C30B C31B C32B 120.2(3) C31B C32B C27B 120.7(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance NiA O1A 1.8411(14) NiA N2A 1.8497(15) NiA N1A 1.8672(15) NiA N3A 1.9451(16) O1A C1A 1.298(2) O2A C1A 1.216(2) O3A C21A 1.221(2) N1A C8A 1.300(2) N1A C2A 1.514(2) N2A C21A 1.376(2) N2A C16A 1.390(2) N3A C22A 1.496(2) N3A C25A 1.499(2) N3A C26A 1.504(3) C1A C2A 1.549(2) C2A C7A 1.533(2) C2A C3A 1.559(2) C3A C4A 1.542(3) C4A C6A 1.522(4) C4A C5A 1.534(4) C8A C15A 1.476(2) C8A C9A 1.502(2) C9A C14A 1.391(3) C9A C10A 1.395(3) C10A C11A 1.390(3) C11A C12A 1.386(3) C12A C13A 1.381(3) C13A C14A 1.396(3) C15A C20A 1.417(2) C15A C16A 1.419(2) C16A C17A 1.418(2) C17A C18A 1.375(3) C18A C19A 1.390(3) C19A C20A 1.381(3) C21A C22A 1.512(3) C22A C23A 1.552(3) C23A C24A 1.530(3) C24A C25A 1.505(4) C26A C27A 1.507(3) C27A C28A 1.392(3) C27A C32A 1.400(3) C28A C29A 1.390(4) C29A C30A 1.392(4) C30A C31A 1.387(4) C31A C32A 1.388(4) NiB O1B 1.8421(13) NiB N2B 1.8468(15) NiB N1B 1.8797(15) NiB N3B 1.9438(16) O1B C1B 1.291(2) O2B C1B 1.222(2) O3B C21B 1.230(2) N1B C8B 1.298(2) N1B C2B 1.510(2) N2B C21B 1.371(2) N2B C16B 1.395(2) N3B C26B 1.499(3) N3B C22B 1.502(2) N3B C25B 1.502(2) C1B C2B 1.551(2) C2B C7B 1.535(2) C2B C3B 1.542(3) C3B C4B 1.539(3) C4B C5B 1.524(3) C4B C6B 1.529(3) C8B C15B 1.480(2) C8B C9B 1.503(2) C9B C14B 1.390(3) C9B C10B 1.395(2) C10B C11B 1.394(3) C11B C12B 1.381(4) C12B C13B 1.374(4) C13B C14B 1.390(3) C15B C20B 1.416(2) C15B C16B 1.419(3) C16B C17B 1.413(3) C17B C18B 1.378(3) C18B C19B 1.388(3) C19B C20B 1.380(3) C21B C22B 1.512(3) C22B C23B 1.548(3) C23B C24B 1.525(3) C24B C25B 1.511(3) C26B C27B 1.506(3) C27B C28B 1.389(3) C27B C32B 1.396(3) C28B C29B 1.388(4) C29B C30B 1.382(5) C30B C31B 1.378(4) C31B C32B 1.387(3) 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 N2A NiA O1A C1A -140.7(12) N1A NiA O1A C1A 15.00(14) N3A NiA O1A C1A -166.12(14) O1A NiA N1A C8A 159.96(15) N2A NiA N1A C8A -21.35(15) N3A NiA N1A C8A 134.7(15) O1A NiA N1A C2A -22.27(11) N2A NiA N1A C2A 156.42(11) N3A NiA N1A C2A -47.5(16) O1A NiA N2A C21A -0.8(14) N1A NiA N2A C21A -156.38(13) N3A NiA N2A C21A 24.69(13) O1A NiA N2A C16A -179(100) N1A NiA N2A C16A 25.36(14) N3A NiA N2A C16A -153.56(14) O1A NiA N3A C22A 149.65(12) N2A NiA N3A C22A -28.98(12) N1A NiA N3A C22A 174.9(15) O1A NiA N3A C25A 35.89(15) N2A NiA N3A C25A -142.75(15) N1A NiA N3A C25A 61.1(16) O1A NiA N3A C26A -88.25(13) N2A NiA N3A C26A 93.11(13) N1A NiA N3A C26A -63.0(16) NiA O1A C1A O2A 175.52(16) NiA O1A C1A C2A -3.3(2) C8A N1A C2A C7A -39.2(2) NiA N1A C2A C7A 142.98(13) C8A N1A C2A C1A -158.14(16) NiA N1A C2A C1A 24.06(15) C8A N1A C2A C3A 88.56(19) NiA N1A C2A C3A -89.24(14) O2A C1A C2A N1A 167.37(17) O1A C1A C2A N1A -13.8(2) O2A C1A C2A C7A 41.0(2) O1A C1A C2A C7A -140.15(17) O2A C1A C2A C3A -81.5(2) O1A C1A C2A C3A 97.34(18) N1A C2A C3A C4A -179.34(18) C7A C2A C3A C4A -49.0(2) C1A C2A C3A C4A 68.8(2) C2A C3A C4A C6A 90.0(3) C2A C3A C4A C5A -147.9(2) C2A N1A C8A C15A -169.07(15) NiA N1A C8A C15A 8.4(2) C2A N1A C8A C9A 11.3(2) NiA N1A C8A C9A -171.19(12) N1A C8A C9A C14A -93.3(2) C15A C8A C9A C14A 87.02(19) N1A C8A C9A C10A 89.2(2) C15A C8A C9A C10A -90.40(19) C14A C9A C10A C11A 2.6(3) C8A C9A C10A C11A 179.99(16) C9A C10A C11A C12A -1.8(3) C10A C11A C12A C13A 0.1(3) C11A C12A C13A C14A 0.9(3) C10A C9A C14A C13A -1.5(3) C8A C9A C14A C13A -178.91(17) C12A C13A C14A C9A -0.2(3) N1A C8A C15A C20A -175.40(16) C9A C8A C15A C20A 4.2(2) N1A C8A C15A C16A 8.4(3) C9A C8A C15A C16A -171.95(15) C21A N2A C16A C17A -16.5(2) NiA N2A C16A C17A 161.60(13) C21A N2A C16A C15A 165.32(16) NiA N2A C16A C15A -16.5(2) C20A C15A C16A N2A 179.81(15) C8A C15A C16A N2A -4.1(3) C20A C15A C16A C17A 1.6(2) C8A C15A C16A C17A 177.74(15) N2A C16A C17A C18A 178.96(17) C15A C16A C17A C18A -2.9(3) C16A C17A C18A C19A 1.6(3) C17A C18A C19A C20A 0.9(3) C18A C19A C20A C15A -2.1(3) C16A C15A C20A C19A 0.8(3) C8A C15A C20A C19A -175.59(17) C16A N2A C21A O3A -16.9(3) NiA N2A C21A O3A 164.76(17) C16A N2A C21A C22A 165.38(15) NiA N2A C21A C22A -12.95(19) C25A N3A C22A C21A 149.05(16) C26A N3A C22A C21A -92.52(18) NiA N3A C22A C21A 28.25(17) C25A N3A C22A C23A 26.11(19) C26A N3A C22A C23A 144.55(16) NiA N3A C22A C23A -94.69(14) O3A C21A C22A N3A 170.66(17) N2A C21A C22A N3A -11.4(2) O3A C21A C22A C23A -70.5(2) N2A C21A C22A C23A 107.41(18) N3A C22A C23A C24A -0.8(2) C21A C22A C23A C24A -122.23(18) C22A C23A C24A C25A -24.7(2) C22A N3A C25A C24A -42.11(19) C26A N3A C25A C24A -162.65(16) NiA N3A C25A C24A 72.67(18) C23A C24A C25A N3A 41.3(2) C22A N3A C26A C27A 64.9(2) C25A N3A C26A C27A -179.93(17) NiA N3A C26A C27A -53.0(2) N3A C26A C27A C28A 89.1(2) N3A C26A C27A C32A -92.1(2) C32A C27A C28A C29A -0.3(3) C26A C27A C28A C29A 178.5(2) C27A C28A C29A C30A 0.2(4) C28A C29A C30A C31A 0.4(4) C29A C30A C31A C32A -0.9(4) C30A C31A C32A C27A 0.7(4) C28A C27A C32A C31A -0.1(3) C26A C27A C32A C31A -179.0(2) N2B NiB O1B C1B 144.7(6) N1B NiB O1B C1B 12.25(14) N3B NiB O1B C1B -160.87(15) O1B NiB N1B C8B 169.14(15) N2B NiB N1B C8B -6.31(15) N3B NiB N1B C8B -128.9(5) O1B NiB N1B C2B -19.12(12) N2B NiB N1B C2B 165.43(11) N3B NiB N1B C2B 42.8(6) O1B NiB N2B C21B 67.6(7) N1B NiB N2B C21B -160.37(13) N3B NiB N2B C21B 13.06(14) O1B NiB N2B C16B -105.0(6) N1B NiB N2B C16B 27.05(15) N3B NiB N2B C16B -159.52(15) O1B NiB N3B C26B -69.29(13) N2B NiB N3B C26B 105.73(13) N1B NiB N3B C26B -131.1(5) O1B NiB N3B C22B 167.99(13) N2B NiB N3B C22B -17.00(12) N1B NiB N3B C22B 106.2(5) O1B NiB N3B C25B 52.44(13) N2B NiB N3B C25B -132.55(13) N1B NiB N3B C25B -9.4(6) NiB O1B C1B O2B 177.03(17) NiB O1B C1B C2B -1.8(2) C8B N1B C2B C7B -50.4(2) NiB N1B C2B C7B 137.63(13) C8B N1B C2B C3B 74.5(2) NiB N1B C2B C3B -97.51(14) C8B N1B C2B C1B -166.92(16) NiB N1B C2B C1B 21.11(16) O2B C1B C2B N1B 168.24(18) O1B C1B C2B N1B -12.9(2) O2B C1B C2B C7B 46.5(2) O1B C1B C2B C7B -134.65(18) O2B C1B C2B C3B -71.5(2) O1B C1B C2B C3B 107.39(18) N1B C2B C3B C4B 53.5(2) C7B C2B C3B C4B -179.06(16) C1B C2B C3B C4B -63.2(2) C2B C3B C4B C5B 85.0(2) C2B C3B C4B C6B -151.95(18) C2B N1B C8B C15B 175.08(15) NiB N1B C8B C15B -14.2(2) C2B N1B C8B C9B -7.7(3) NiB N1B C8B C9B 163.01(13) N1B C8B C9B C14B -93.5(2) C15B C8B C9B C14B 83.90(19) N1B C8B C9B C10B 92.9(2) C15B C8B C9B C10B -89.7(2) C14B C9B C10B C11B 2.3(3) C8B C9B C10B C11B 175.8(2) C9B C10B C11B C12B -2.0(4) C10B C11B C12B C13B 0.5(4) C11B C12B C13B C14B 0.5(4) C10B C9B C14B C13B -1.3(3) C8B C9B C14B C13B -175.19(18) C12B C13B C14B C9B -0.2(3) N1B C8B C15B C20B -158.72(17) C9B C8B C15B C20B 23.8(2) N1B C8B C15B C16B 19.8(3) C9B C8B C15B C16B -157.65(16) C21B N2B C16B C17B -22.3(3) NiB N2B C16B C17B 149.95(15) C21B N2B C16B C15B 160.04(17) NiB N2B C16B C15B -27.7(2) C20B C15B C16B N2B -178.94(16) C8B C15B C16B N2B 2.5(3) C20B C15B C16B C17B 3.3(3) C8B C15B C16B C17B -175.19(17) N2B C16B C17B C18B -179.79(18) C15B C16B C17B C18B -2.1(3) C16B C17B C18B C19B -0.3(3) C17B C18B C19B C20B 1.4(3) C18B C19B C20B C15B 0.0(3) C16B C15B C20B C19B -2.4(3) C8B C15B C20B C19B 176.24(17) C16B N2B C21B O3B -14.1(3) NiB N2B C21B O3B 173.19(17) C16B N2B C21B C22B 167.52(16) NiB N2B C21B C22B -5.2(2) C26B N3B C22B C21B -102.44(17) C25B N3B C22B C21B 137.91(16) NiB N3B C22B C21B 17.84(18) C26B N3B C22B C23B 134.15(15) C25B N3B C22B C23B 14.50(18) NiB N3B C22B C23B -105.57(14) O3B C21B C22B N3B 172.46(17) N2B C21B C22B N3B -9.0(2) O3B C21B C22B C23B -67.8(2) N2B C21B C22B C23B 110.74(18) N3B C22B C23B C24B 12.14(19) C21B C22B C23B C24B -110.11(18) C22B C23B C24B C25B -33.81(19) C26B N3B C25B C24B -157.46(15) C22B N3B C25B C24B -36.06(18) NiB N3B C25B C24B 81.57(16) C23B C24B C25B N3B 43.50(18) C22B N3B C26B C27B 71.2(2) C25B N3B C26B C27B -172.07(16) NiB N3B C26B C27B -49.03(19) N3B C26B C27B C28B 98.7(2) N3B C26B C27B C32B -80.6(2) C32B C27B C28B C29B 0.0(3) C26B C27B C28B C29B -179.4(2) C27B C28B C29B C30B 1.6(4) C28B C29B C30B C31B -1.2(4) C29B C30B C31B C32B -0.7(4) C30B C31B C32B C27B 2.3(4) C28B C27B C32B C31B -2.0(3) C26B C27B C32B C31B 177.4(2)