#------------------------------------------------------------------------------ #$Date: 2021-01-01 08:40:07 +0200 (Fri, 01 Jan 2021) $ #$Revision: 260340 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/02/7060225.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_7060225 loop_ _publ_author_name 'Shit, Madhusudan' 'Maity, Suvendu' 'Bera, Sachinath' 'Mudi, Prafullya Kumar' 'Biswas, Bhaskar' 'Weyhermueller, Thomas' 'Ghosh, Prasanta' _publ_section_title ; Nickel (II) di-aqua complex containing water cluster: Synthesis, X-ray structure and catecholase activity ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D0NJ05238H _journal_year 2021 _chemical_formula_moiety 'C15 H15 N Ni O6, 1.75(H2 O)' _chemical_formula_sum 'C15 H18.5 N Ni O7.75' _chemical_formula_weight 395.52 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_block_code 7278 _audit_creation_date 2011-03-09 _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-10-24 deposited with the CCDC. 2020-12-29 downloaded from the CCDC. ; _cell_angle_alpha 81.497(9) _cell_angle_beta 89.659(8) _cell_angle_gamma 89.249(9) _cell_formula_units_Z 8 _cell_length_a 12.343(2) _cell_length_b 14.617(3) _cell_length_c 18.348(3) _cell_measurement_reflns_used 9132 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 66.1558 _cell_measurement_theta_min 2.4349 _cell_volume 3273.6(10) _computing_cell_refinement 'SAINT software (Bruker AXS, 2004)' _computing_data_collection 'PROTEUM2 (Bruker AXS, 2008)' _computing_data_reduction 'SAINT software (Bruker AXS, 2004)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXS-97 (G. M. Sheldrick, 2008)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 66.67 _diffrn_measured_fraction_theta_full 0.961 _diffrn_measured_fraction_theta_max 0.961 _diffrn_measurement_device_type 'Bruker AXS X8 Proteum' _diffrn_measurement_method 'CCD \f- and \w-scans' _diffrn_radiation_monochromator 'focusing multilayer optic' _diffrn_radiation_source '0.2 x 2mm^2^ focus rotating anode' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_unetI/netI 0.0406 _diffrn_reflns_Laue_measured_fraction_full 0.961 _diffrn_reflns_Laue_measured_fraction_max 0.961 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 74139 _diffrn_reflns_point_group_measured_fraction_full 0.961 _diffrn_reflns_point_group_measured_fraction_max 0.961 _diffrn_reflns_theta_full 66.924 _diffrn_reflns_theta_max 66.924 _diffrn_reflns_theta_min 2.435 _exptl_absorpt_coefficient_mu 2.114 _exptl_absorpt_correction_T_max 0.88345 _exptl_absorpt_correction_T_min 0.67295 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2008)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.605 _exptl_crystal_description plate _exptl_crystal_F_000 1644 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _refine_diff_density_max 1.047 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.094 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 964 _refine_ls_number_reflns 11191 _refine_ls_number_restraints 30 _refine_ls_restrained_S_all 1.099 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0643 _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^)+(0.0209P)^2^+18.3522P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1538 _refine_ls_wR_factor_ref 0.1572 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9918 _reflns_number_total 11191 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0nj05238h2.cif _cod_data_source_block 7278new _cod_original_formula_sum 'C15 H18.50 N Ni O7.75' _cod_database_code 7060225 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.555 _shelx_estimated_absorpt_t_max 0.849 _shelx_res_file ; TITL 4[LNi(OH2)2] * 7 H2O Four indep. Molecules ; Pseudo-Translation!!! 7278new.res created by SHELXL-2018/3 at 12:05:55 on 06-Jul-2020 TITL 7278 Prasanta Ghosh in P-1 Crystal No.4 ; WGT-PG-500-04 7278new.res created by SHELXL-2018/3 at 12:05:55 on 06-Jul-2020 CELL 1.54178 12.343 14.617 18.348 81.497 89.659 89.249 ZERR 8.00 0.002 0.003 0.003 0.009 0.008 0.009 LATT 1 SFAC C H N O NI UNIT 120 148 8 62 8 OMIT -3 134 TEMP -173 OMIT -1 1 9 OMIT 6 -2 4 OMIT -7 0 2 OMIT -4 -4 12 OMIT -1 -1 8 OMIT 9 0 5 OMIT -2 -1 8 OMIT 2 -2 1 OMIT 1 0 9 SIZE 0.08 0.223 0.316 L.S. 12 BOND FMAP 2 PLAN 20 DFIX 0.84 0.01 O130 H131 O130 H132 O140 H141 O140 H142 = O230 H231 O230 H232 O240 H241 O240 H242 = O330 H331 O330 H332 O340 H341 O340 H342 = O430 H431 O430 H432 O440 H441 O440 H442 = O510 H511 O510 H512 O520 H521 O520 H522 = O530 H531 O530 H532 = O570 H571 O570 H572 SADI 0.01 H511 H512 H521 H522 H531 H532 H571 H572 EQIV $1 x, y+1, z EQIV $2 -x+2, -y, -z+1 EQIV $3 x, y-1, z EQIV $4 -x+1, -y, -z+1 HTAB O130 O301 HTAB O130 O540 HTAB O140 O401 HTAB O140 O520 HTAB O230 O401_$1 HTAB O230 O520_$1 HTAB O240 O301 HTAB O240 O540 HTAB O330 O201 HTAB O330 O530_$1 HTAB O340 O101 HTAB O340 O510_$2 HTAB O430 O101 HTAB O430 O510_$2 HTAB O440 O201_$3 HTAB O440 O530 HTAB O510 O420 HTAB O510 O119_$2 HTAB O520 O120_$4 HTAB O520 O550 HTAB O530 O320_$2 HTAB O570 O120 HTAB O570 O320 ACTA WGHT 0.020900 18.352200 FVAR 0.04780 NI1 5 0.611259 0.140163 0.285462 11.00000 0.01626 0.01884 = 0.01441 -0.00028 0.00315 -0.00039 NI2 5 0.606745 0.641195 0.274214 11.00000 0.01926 0.01902 = 0.01767 0.00098 -0.00385 0.00054 NI3 5 0.899620 0.387388 0.278066 11.00000 0.01830 0.01914 = 0.01480 0.00042 -0.00118 0.00088 NI4 5 0.905371 -0.111333 0.277692 11.00000 0.01739 0.01924 = 0.01624 -0.00124 -0.00049 0.00017 O101 4 0.744901 0.149993 0.221939 11.00000 0.01858 0.02244 = 0.01261 0.00037 -0.00067 -0.00083 C102 1 0.718398 0.157887 0.150813 11.00000 0.01794 0.01859 = 0.01641 -0.00051 0.00470 -0.00121 C103 1 0.798222 0.164683 0.095717 11.00000 0.02120 0.02700 = 0.02038 -0.00042 0.00400 0.00006 AFIX 43 H103 2 0.872593 0.164597 0.108768 11.00000 -1.20000 AFIX 0 C104 1 0.769258 0.171492 0.022668 11.00000 0.02978 0.02978 = 0.01675 0.00117 0.00719 0.00235 AFIX 43 H104 2 0.824005 0.176361 -0.014267 11.00000 -1.20000 AFIX 0 C105 1 0.661220 0.171324 0.002398 11.00000 0.03374 0.03130 = 0.01481 -0.00023 -0.00155 0.00191 AFIX 43 H105 2 0.642394 0.175117 -0.048098 11.00000 -1.20000 AFIX 0 C106 1 0.580786 0.165630 0.055728 11.00000 0.02085 0.02600 = 0.02162 -0.00099 -0.00575 0.00181 AFIX 43 H106 2 0.506690 0.165924 0.041969 11.00000 -1.20000 AFIX 0 C107 1 0.609213 0.159453 0.129875 11.00000 0.01946 0.02060 = 0.01645 -0.00089 -0.00019 0.00098 N108 3 0.533108 0.153879 0.189103 11.00000 0.01480 0.01928 = 0.01972 -0.00039 0.00140 0.00173 C109 1 0.430564 0.157864 0.180082 11.00000 0.02268 0.02404 = 0.02578 -0.00445 -0.00242 0.00142 AFIX 43 H109 2 0.405917 0.166200 0.130562 11.00000 -1.20000 AFIX 0 C110 1 0.346033 0.151022 0.237638 11.00000 0.01567 0.01986 = 0.03193 -0.00238 0.00153 0.00013 C111 1 0.239677 0.157190 0.210735 11.00000 0.01963 0.02981 = 0.03300 -0.00596 -0.00262 0.00209 AFIX 43 H111 2 0.228896 0.165977 0.158934 11.00000 -1.20000 AFIX 0 C112 1 0.149898 0.151007 0.256496 11.00000 0.01416 0.02725 = 0.04767 -0.00619 0.00007 0.00012 AFIX 43 H112 2 0.078753 0.155555 0.236707 11.00000 -1.20000 AFIX 0 C113 1 0.166332 0.138005 0.331985 11.00000 0.02117 0.02507 = 0.03986 -0.00715 0.00750 -0.00067 AFIX 43 H113 2 0.105581 0.133376 0.364296 11.00000 -1.20000 AFIX 0 C114 1 0.269646 0.131663 0.361018 11.00000 0.02855 0.02360 = 0.02653 -0.00209 0.00452 -0.00031 AFIX 43 H114 2 0.279378 0.122970 0.412917 11.00000 -1.20000 AFIX 0 C115 1 0.359600 0.137980 0.314387 11.00000 0.01937 0.01543 = 0.03149 -0.00198 0.00037 0.00106 O116 4 0.463060 0.131194 0.342389 11.00000 0.01992 0.02817 = 0.01973 -0.00164 0.00524 -0.00069 C117 1 0.475287 0.121771 0.421516 11.00000 0.02730 0.03097 = 0.01812 0.00067 0.00358 0.00292 AFIX 23 H11A 2 0.440018 0.064330 0.444964 11.00000 -1.20000 H11B 2 0.439452 0.174759 0.440160 11.00000 -1.20000 AFIX 0 C118 1 0.595021 0.118538 0.441612 11.00000 0.02956 0.02330 = 0.01932 -0.00062 0.00662 0.00045 O119 4 0.664799 0.124338 0.391189 11.00000 0.02651 0.02725 = 0.01559 -0.00028 0.00346 0.00016 O120 4 0.614673 0.109894 0.509255 11.00000 0.03078 0.04424 = 0.01631 -0.00029 0.00291 0.00150 O130 4 0.605413 0.281532 0.283347 11.00000 0.02193 0.02157 = 0.01921 -0.00156 0.00524 -0.00274 H131 2 0.655450 0.308172 0.257620 11.00000 -1.50000 H132 2 0.599831 0.299223 0.324676 11.00000 -1.50000 O140 4 0.613127 -0.000356 0.289095 11.00000 0.02516 0.01900 = 0.02172 -0.00079 0.00845 0.00055 H141 2 0.660787 -0.019650 0.262280 11.00000 -1.50000 H142 2 0.595835 -0.038008 0.326040 11.00000 -1.50000 O201 4 0.750301 0.652318 0.220528 11.00000 0.01972 0.02272 = 0.02494 -0.00217 -0.00337 0.00075 C202 1 0.734771 0.660766 0.147998 11.00000 0.02487 0.01703 = 0.02684 -0.00105 0.00185 0.00246 C203 1 0.821584 0.670279 0.097433 11.00000 0.01856 0.02927 = 0.04440 -0.00301 0.00511 0.00229 AFIX 43 H203 2 0.893572 0.670714 0.115402 11.00000 -1.20000 AFIX 0 C204 1 0.804959 0.678871 0.023419 11.00000 0.03913 0.03223 = 0.03448 0.00072 0.01691 0.00738 AFIX 43 H204 2 0.865122 0.685814 -0.009380 11.00000 -1.20000 AFIX 0 C205 1 0.699869 0.677552 -0.004730 11.00000 0.04341 0.03250 = 0.02494 -0.00211 0.00553 0.00853 AFIX 43 H205 2 0.688622 0.683160 -0.056384 11.00000 -1.20000 AFIX 0 C206 1 0.613683 0.668137 0.042703 11.00000 0.03083 0.02391 = 0.02402 -0.00066 0.00079 0.00652 AFIX 43 H206 2 0.542400 0.666184 0.023797 11.00000 -1.20000 AFIX 0 C207 1 0.629087 0.661349 0.118618 11.00000 0.02353 0.01775 = 0.02561 -0.00060 0.00234 0.00265 N208 3 0.544619 0.655141 0.172693 11.00000 0.01835 0.01793 = 0.01846 -0.00011 -0.00019 0.00023 C209 1 0.445186 0.663452 0.155510 11.00000 0.02707 0.02502 = 0.01692 -0.00034 -0.00433 -0.00125 AFIX 43 H209 2 0.429617 0.674453 0.104294 11.00000 -1.20000 AFIX 0 C210 1 0.351346 0.658073 0.205445 11.00000 0.01910 0.02165 = 0.02308 -0.00096 -0.00167 0.00009 C211 1 0.250810 0.670987 0.169686 11.00000 0.02465 0.03270 = 0.03242 0.00263 -0.00826 0.00022 AFIX 43 H211 2 0.249401 0.684426 0.117432 11.00000 -1.20000 AFIX 0 C212 1 0.154480 0.664808 0.207840 11.00000 0.02115 0.03564 = 0.04445 0.00131 -0.00557 0.00204 AFIX 43 H212 2 0.087536 0.673686 0.182331 11.00000 -1.20000 AFIX 0 C213 1 0.156308 0.645548 0.283651 11.00000 0.02246 0.03375 = 0.05269 -0.01152 0.00971 -0.00343 AFIX 43 H213 2 0.090137 0.640518 0.310572 11.00000 -1.20000 AFIX 0 C214 1 0.254078 0.633456 0.320927 11.00000 0.02871 0.03970 = 0.02917 -0.00587 0.00609 -0.00658 AFIX 43 H214 2 0.254387 0.619795 0.373181 11.00000 -1.20000 AFIX 0 C215 1 0.351383 0.641165 0.282467 11.00000 0.01959 0.02219 = 0.03372 -0.00575 -0.00242 -0.00161 O216 4 0.449901 0.630613 0.318633 11.00000 0.02630 0.03735 = 0.01529 0.00135 -0.00182 -0.00437 C217 1 0.448439 0.612645 0.397875 11.00000 0.04888 0.09167 = 0.01546 0.00055 0.00223 -0.03462 AFIX 23 H21A 2 0.414440 0.552147 0.414586 11.00000 -1.20000 H21B 2 0.405134 0.661120 0.417467 11.00000 -1.20000 AFIX 0 C218 1 0.564005 0.611820 0.426836 11.00000 0.05266 0.05437 = 0.01854 0.01209 -0.01268 -0.02433 O219 4 0.641032 0.625884 0.383627 11.00000 0.03614 0.02819 = 0.02512 0.00214 -0.01221 -0.00306 O220 4 0.573181 0.596904 0.495339 11.00000 0.06981 0.12794 = 0.01864 0.01559 -0.01158 -0.05675 O230 4 0.596562 0.782459 0.272363 11.00000 0.02131 0.02155 = 0.02045 -0.00283 0.00182 -0.00170 H231 2 0.652040 0.811182 0.255595 11.00000 -1.50000 H232 2 0.577636 0.803162 0.310922 11.00000 -1.50000 O240 4 0.609472 0.499744 0.280474 11.00000 0.02492 0.02005 = 0.02443 0.00295 0.00200 0.00156 H241 2 0.661406 0.484303 0.254805 11.00000 -1.50000 H242 2 0.606781 0.473103 0.324177 11.00000 -1.50000 O301 4 0.760615 0.400832 0.220178 11.00000 0.01904 0.02413 = 0.01564 0.00106 0.00022 0.00046 C302 1 0.782197 0.407734 0.148333 11.00000 0.02180 0.01599 = 0.02203 0.00221 -0.00062 -0.00077 C303 1 0.698502 0.414941 0.096245 11.00000 0.02584 0.02618 = 0.02481 0.00135 -0.00622 0.00034 AFIX 43 H303 2 0.625142 0.415167 0.112187 11.00000 -1.20000 AFIX 0 C304 1 0.722041 0.421690 0.022159 11.00000 0.03819 0.02990 = 0.02437 0.00259 -0.01191 -0.00293 AFIX 43 H304 2 0.664479 0.427312 -0.012420 11.00000 -1.20000 AFIX 0 C305 1 0.828391 0.420426 -0.002906 11.00000 0.04733 0.03153 = 0.01406 0.00015 -0.00277 -0.00550 AFIX 43 H305 2 0.843470 0.424030 -0.054077 11.00000 -1.20000 AFIX 0 C306 1 0.912278 0.413847 0.047580 11.00000 0.03296 0.02431 = 0.02083 0.00070 0.00210 -0.00136 AFIX 43 H306 2 0.985216 0.412731 0.030876 11.00000 -1.20000 AFIX 0 C307 1 0.890465 0.408875 0.122417 11.00000 0.02534 0.01754 = 0.01741 0.00002 -0.00255 0.00009 N308 3 0.969388 0.403077 0.178940 11.00000 0.02436 0.01690 = 0.01790 0.00039 -0.00137 0.00249 C309 1 1.071816 0.411551 0.165060 11.00000 0.02308 0.02541 = 0.02102 -0.00049 0.00221 -0.00120 AFIX 43 H309 2 1.092168 0.423281 0.114558 11.00000 -1.20000 AFIX 0 C310 1 1.159436 0.405068 0.218446 11.00000 0.01953 0.02060 = 0.03200 -0.00446 0.00365 0.00047 C311 1 1.263005 0.420127 0.186726 11.00000 0.02279 0.02900 = 0.04696 -0.00452 0.00669 0.00011 AFIX 43 H311 2 1.269365 0.436079 0.134789 11.00000 -1.20000 AFIX 0 C312 1 1.355973 0.412263 0.229377 11.00000 0.01970 0.03259 = 0.06058 -0.01034 -0.00005 -0.00034 AFIX 43 H312 2 1.425040 0.423092 0.206859 11.00000 -1.20000 AFIX 0 C313 1 1.347342 0.388668 0.304507 11.00000 0.01914 0.02946 = 0.06270 -0.01078 -0.01288 0.00527 AFIX 43 H313 2 1.410878 0.381872 0.333881 11.00000 -1.20000 AFIX 0 C314 1 1.246726 0.374748 0.337636 11.00000 0.02636 0.02615 = 0.04078 -0.00411 -0.01439 0.00251 AFIX 43 H314 2 1.241554 0.358689 0.389624 11.00000 -1.20000 AFIX 0 C315 1 1.152939 0.384163 0.295144 11.00000 0.01819 0.01966 = 0.03777 -0.00372 -0.00356 0.00048 O316 4 1.051657 0.371608 0.328211 11.00000 0.02175 0.03014 = 0.01750 0.00132 -0.00545 0.00173 C317 1 1.044954 0.354104 0.407789 11.00000 0.03466 0.03589 = 0.01777 0.00671 -0.00809 -0.00452 AFIX 23 H31A 2 1.085296 0.402044 0.428866 11.00000 -1.20000 H31B 2 1.078303 0.293133 0.426104 11.00000 -1.20000 AFIX 0 C318 1 0.927821 0.355302 0.432014 11.00000 0.03812 0.02255 = 0.02118 -0.00038 -0.00325 -0.00518 O319 4 0.853531 0.369437 0.385368 11.00000 0.02996 0.02651 = 0.01409 0.00326 -0.00018 0.00111 O320 4 0.911674 0.342247 0.500535 11.00000 0.04952 0.05867 = 0.01395 0.00144 -0.00416 -0.02405 O330 4 0.907217 0.528347 0.278373 11.00000 0.02366 0.02074 = 0.02006 -0.00292 -0.00399 0.00225 H331 2 0.851399 0.558513 0.263730 11.00000 -1.50000 H332 2 0.923662 0.551257 0.315897 11.00000 -1.50000 O340 4 0.899037 0.246812 0.279679 11.00000 0.02090 0.01896 = 0.01994 0.00184 -0.00395 -0.00189 H341 2 0.853164 0.221370 0.256435 11.00000 -1.50000 H342 2 0.894818 0.213781 0.320943 11.00000 -1.50000 O401 4 0.760799 -0.100347 0.225038 11.00000 0.01580 0.02342 = 0.01687 -0.00083 0.00192 0.00035 C402 1 0.775121 -0.091951 0.152488 11.00000 0.02201 0.01614 = 0.01821 -0.00087 0.00197 -0.00137 C403 1 0.687842 -0.084264 0.103758 11.00000 0.01933 0.02642 = 0.02378 0.00079 0.00033 -0.00225 AFIX 43 H403 2 0.616061 -0.083604 0.122662 11.00000 -1.20000 AFIX 0 C404 1 0.703868 -0.077634 0.028916 11.00000 0.03319 0.03058 = 0.02149 0.00021 -0.00611 -0.00549 AFIX 43 H404 2 0.643201 -0.071625 -0.003134 11.00000 -1.20000 AFIX 0 C405 1 0.807837 -0.079631 -0.000312 11.00000 0.03763 0.03473 = 0.02022 -0.00375 0.00259 -0.00839 AFIX 43 H405 2 0.818049 -0.076504 -0.051977 11.00000 -1.20000 AFIX 0 C406 1 0.896321 -0.086181 0.046032 11.00000 0.02694 0.02914 = 0.01912 -0.00364 0.00802 -0.00386 AFIX 43 H406 2 0.967532 -0.087266 0.026219 11.00000 -1.20000 AFIX 0 C407 1 0.881087 -0.091203 0.121943 11.00000 0.02028 0.02029 = 0.02177 -0.00228 0.00078 -0.00232 N408 3 0.965196 -0.096018 0.174462 11.00000 0.02050 0.01871 = 0.02123 -0.00398 0.00049 0.00194 C409 1 1.065822 -0.087904 0.155686 11.00000 0.02002 0.02926 = 0.02674 -0.00853 0.00465 -0.00214 AFIX 43 H409 2 1.079960 -0.079072 0.104187 11.00000 -1.20000 AFIX 0 C410 1 1.159966 -0.090425 0.202343 11.00000 0.01883 0.02362 = 0.03294 -0.00846 0.00471 -0.00177 C411 1 1.259447 -0.080282 0.163951 11.00000 0.02425 0.03623 = 0.02688 -0.00821 0.00458 -0.00155 AFIX 43 H411 2 1.259024 -0.073097 0.111640 11.00000 -1.20000 AFIX 0 C412 1 1.356618 -0.080450 0.199605 11.00000 0.01881 0.03455 = 0.04051 -0.00753 0.00521 -0.00002 AFIX 43 H412 2 1.422564 -0.073668 0.172496 11.00000 -1.20000 AFIX 0 C413 1 1.357112 -0.090605 0.275322 11.00000 0.01893 0.03001 = 0.03288 0.00047 -0.00126 0.00285 AFIX 43 H413 2 1.424105 -0.090707 0.300560 11.00000 -1.20000 AFIX 0 C414 1 1.261702 -0.100654 0.315218 11.00000 0.02908 0.02640 = 0.02992 -0.00114 -0.00238 0.00195 AFIX 43 H414 2 1.263625 -0.107013 0.367478 11.00000 -1.20000 AFIX 0 C415 1 1.162518 -0.101530 0.279302 11.00000 0.01793 0.02038 = 0.02809 -0.00504 0.00558 -0.00165 O416 4 1.066240 -0.112967 0.318450 11.00000 0.02314 0.03130 = 0.02286 -0.00524 -0.00292 0.00173 C417 1 1.070567 -0.114303 0.397259 11.00000 0.02607 0.03604 = 0.01693 0.00145 -0.00173 -0.00119 AFIX 23 H41A 2 1.104071 -0.056695 0.408169 11.00000 -1.20000 H41B 2 1.116040 -0.167213 0.419718 11.00000 -1.20000 AFIX 0 C418 1 0.957906 -0.122672 0.430268 11.00000 0.03119 0.02522 = 0.02161 -0.00004 -0.00299 0.00070 O419 4 0.876883 -0.129164 0.387871 11.00000 0.02913 0.02737 = 0.01493 -0.00058 -0.00165 -0.00289 O420 4 0.952151 -0.124502 0.497510 11.00000 0.03112 0.05226 = 0.01690 -0.00186 -0.00019 -0.00057 O430 4 0.906489 0.029612 0.277262 11.00000 0.02074 0.02102 = 0.02039 -0.00354 -0.00413 0.00230 H431 2 0.848759 0.056942 0.262859 11.00000 -1.50000 H432 2 0.911907 0.045509 0.319188 11.00000 -1.50000 O440 4 0.903054 -0.252364 0.282427 11.00000 0.02252 0.02058 = 0.01999 0.00020 -0.00475 -0.00110 H441 2 0.852890 -0.275286 0.260741 11.00000 -1.50000 H442 2 0.901635 -0.285557 0.323826 11.00000 -1.50000 O510 4 1.107185 -0.114698 0.598003 11.00000 0.02434 0.03365 = 0.01985 -0.00230 0.00058 -0.00002 H511 2 1.061834 -0.114959 0.564181 11.00000 -1.50000 H512 2 1.170033 -0.111835 0.580384 11.00000 -1.50000 O520 4 0.557953 -0.138708 0.401025 11.00000 0.03233 0.03511 = 0.01789 0.00150 0.00644 0.00369 H521 2 0.506897 -0.132879 0.430250 11.00000 -1.50000 H522 2 0.613456 -0.159001 0.424587 11.00000 -1.50000 O530 4 0.929819 -0.386183 0.405249 11.00000 0.03147 0.03487 = 0.01571 -0.00005 0.00019 -0.00696 H531 2 0.974749 -0.367034 0.433661 11.00000 -1.50000 H532 2 0.876774 -0.409302 0.430086 11.00000 -1.50000 O540 4 0.592349 0.371511 0.408379 11.00000 0.07549 0.02890 = 0.02336 -0.00017 -0.01827 -0.00016 O550 4 0.723337 -0.232086 0.475564 11.00000 0.02545 0.03994 = 0.03745 -0.00100 -0.00112 -0.00052 O560 4 0.788626 0.516689 0.503335 11.00000 0.03943 0.03762 = 0.08557 0.00755 0.02412 0.00267 O570 4 0.711344 0.277085 0.517538 11.00000 0.06174 0.07150 = 0.06523 -0.00920 -0.00441 -0.00063 H571 2 0.696413 0.223071 0.507926 11.00000 -1.50000 H572 2 0.779394 0.277307 0.525535 11.00000 -1.50000 HKLF 4 REM 7278 Prasanta Ghosh in P-1 Crystal No.4 ; WGT-PG-500-04 REM wR2 = 0.1572, GooF = S = 1.101, Restrained GooF = 1.099 for all data REM R1 = 0.0643 for 9918 Fo > 4sig(Fo) and 0.0701 for all 11191 data REM 964 parameters refined using 30 restraints END WGHT 0.0198 18.4131 REM Highest difference peak 1.047, deepest hole -0.783, 1-sigma level 0.094 Q1 1 0.5932 0.0823 0.2650 11.00000 0.05 1.05 Q2 1 0.5286 0.6396 0.5015 11.00000 0.05 0.96 Q3 1 0.8811 0.4455 0.2976 11.00000 0.05 0.87 Q4 1 0.5926 0.5779 0.2600 11.00000 0.05 0.81 Q5 1 0.8802 0.3226 0.2663 11.00000 0.05 0.71 Q6 1 0.7756 0.5178 0.4579 11.00000 0.05 0.70 Q7 1 0.8858 -0.0470 0.2920 11.00000 0.05 0.63 Q8 1 0.7167 -0.2909 0.4604 11.00000 0.05 0.61 Q9 1 0.5866 0.7039 0.2905 11.00000 0.05 0.55 Q10 1 0.5805 0.2056 0.2906 11.00000 0.05 0.51 Q11 1 0.5444 0.1409 0.4971 11.00000 0.05 0.49 Q12 1 0.8233 -0.0931 0.2818 11.00000 0.05 0.48 Q13 1 0.8949 0.4043 0.5159 11.00000 0.05 0.48 Q14 1 0.7189 0.5375 0.5055 11.00000 0.05 0.47 Q15 1 1.2249 -0.0198 0.5332 11.00000 0.05 0.47 Q16 1 0.7797 -0.2017 0.4561 11.00000 0.05 0.45 Q17 1 0.9338 0.3414 0.1670 11.00000 0.05 0.44 Q18 1 1.3406 -0.1254 0.3349 11.00000 0.05 0.43 Q19 1 0.6336 0.3467 0.4409 11.00000 0.05 0.43 Q20 1 0.8732 -0.1363 0.5102 11.00000 0.05 0.42 ; _shelx_res_checksum 58407 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.61126(5) 0.14016(5) 0.28546(4) 0.01673(17) Uani 1 1 d . . . . . Ni2 Ni 0.60674(6) 0.64119(5) 0.27421(4) 0.01901(18) Uani 1 1 d . . . . . Ni3 Ni 0.89962(6) 0.38739(5) 0.27807(4) 0.01771(17) Uani 1 1 d . . . . . Ni4 Ni 0.90537(6) -0.11133(5) 0.27769(4) 0.01776(17) Uani 1 1 d . . . . . O101 O 0.7449(2) 0.1500(2) 0.22194(15) 0.0182(6) Uani 1 1 d . . . . . C102 C 0.7184(3) 0.1579(3) 0.1508(2) 0.0179(8) Uani 1 1 d . . . . . C103 C 0.7982(4) 0.1647(3) 0.0957(2) 0.0232(9) Uani 1 1 d . . . . . H103 H 0.872593 0.164597 0.108768 0.028 Uiso 1 1 calc R U . . . C104 C 0.7693(4) 0.1715(3) 0.0227(2) 0.0260(10) Uani 1 1 d . . . . . H104 H 0.824005 0.176361 -0.014267 0.031 Uiso 1 1 calc R U . . . C105 C 0.6612(4) 0.1713(3) 0.0024(2) 0.0270(10) Uani 1 1 d . . . . . H105 H 0.642394 0.175117 -0.048098 0.032 Uiso 1 1 calc R U . . . C106 C 0.5808(4) 0.1656(3) 0.0557(2) 0.0231(9) Uani 1 1 d . . . . . H106 H 0.506690 0.165924 0.041969 0.028 Uiso 1 1 calc R U . . . C107 C 0.6092(3) 0.1595(3) 0.1299(2) 0.0190(9) Uani 1 1 d . . . . . N108 N 0.5331(3) 0.1539(2) 0.18910(19) 0.0182(7) Uani 1 1 d . . . . . C109 C 0.4306(4) 0.1579(3) 0.1801(3) 0.0241(10) Uani 1 1 d . . . . . H109 H 0.405917 0.166200 0.130562 0.029 Uiso 1 1 calc R U . . . C110 C 0.3460(3) 0.1510(3) 0.2376(3) 0.0226(9) Uani 1 1 d . . . . . C111 C 0.2397(4) 0.1572(3) 0.2107(3) 0.0274(10) Uani 1 1 d . . . . . H111 H 0.228896 0.165977 0.158934 0.033 Uiso 1 1 calc R U . . . C112 C 0.1499(4) 0.1510(3) 0.2565(3) 0.0296(11) Uani 1 1 d . . . . . H112 H 0.078753 0.155555 0.236707 0.036 Uiso 1 1 calc R U . . . C113 C 0.1663(4) 0.1380(3) 0.3320(3) 0.0285(10) Uani 1 1 d . . . . . H113 H 0.105581 0.133376 0.364296 0.034 Uiso 1 1 calc R U . . . C114 C 0.2696(4) 0.1317(3) 0.3610(3) 0.0264(10) Uani 1 1 d . . . . . H114 H 0.279378 0.122970 0.412917 0.032 Uiso 1 1 calc R U . . . C115 C 0.3596(3) 0.1380(3) 0.3144(3) 0.0223(9) Uani 1 1 d . . . . . O116 O 0.4631(2) 0.1312(2) 0.34239(16) 0.0228(7) Uani 1 1 d . . . . . C117 C 0.4753(4) 0.1218(3) 0.4215(2) 0.0259(10) Uani 1 1 d . . . . . H11A H 0.440018 0.064330 0.444964 0.031 Uiso 1 1 calc R U . . . H11B H 0.439452 0.174759 0.440160 0.031 Uiso 1 1 calc R U . . . C118 C 0.5950(4) 0.1185(3) 0.4416(2) 0.0243(10) Uani 1 1 d . . . . . O119 O 0.6648(2) 0.1243(2) 0.39119(16) 0.0234(7) Uani 1 1 d . . . . . O120 O 0.6147(3) 0.1099(2) 0.50926(17) 0.0309(8) Uani 1 1 d . . . . . O130 O 0.6054(2) 0.2815(2) 0.28335(16) 0.0210(6) Uani 1 1 d D . . . . H131 H 0.655(3) 0.308(3) 0.258(2) 0.032 Uiso 1 1 d D U . . . H132 H 0.600(4) 0.299(3) 0.3247(14) 0.032 Uiso 1 1 d D U . . . O140 O 0.6131(2) -0.0004(2) 0.28909(17) 0.0222(6) Uani 1 1 d D . . . . H141 H 0.661(3) -0.020(3) 0.262(2) 0.033 Uiso 1 1 d D U . . . H142 H 0.596(4) -0.038(3) 0.3260(18) 0.033 Uiso 1 1 d D U . . . O201 O 0.7503(2) 0.6523(2) 0.22053(16) 0.0226(6) Uani 1 1 d . . . . . C202 C 0.7348(4) 0.6608(3) 0.1480(2) 0.0232(9) Uani 1 1 d . . . . . C203 C 0.8216(4) 0.6703(3) 0.0974(3) 0.0310(11) Uani 1 1 d . . . . . H203 H 0.893572 0.670714 0.115402 0.037 Uiso 1 1 calc R U . . . C204 C 0.8050(4) 0.6789(4) 0.0234(3) 0.0360(12) Uani 1 1 d . . . . . H204 H 0.865122 0.685814 -0.009380 0.043 Uiso 1 1 calc R U . . . C205 C 0.6999(4) 0.6776(4) -0.0047(3) 0.0339(11) Uani 1 1 d . . . . . H205 H 0.688622 0.683160 -0.056384 0.041 Uiso 1 1 calc R U . . . C206 C 0.6137(4) 0.6681(3) 0.0427(2) 0.0266(10) Uani 1 1 d . . . . . H206 H 0.542400 0.666184 0.023797 0.032 Uiso 1 1 calc R U . . . C207 C 0.6291(4) 0.6613(3) 0.1186(2) 0.0226(9) Uani 1 1 d . . . . . N208 N 0.5446(3) 0.6551(2) 0.17269(19) 0.0185(7) Uani 1 1 d . . . . . C209 C 0.4452(4) 0.6635(3) 0.1555(2) 0.0233(9) Uani 1 1 d . . . . . H209 H 0.429617 0.674453 0.104294 0.028 Uiso 1 1 calc R U . . . C210 C 0.3513(3) 0.6581(3) 0.2054(2) 0.0215(9) Uani 1 1 d . . . . . C211 C 0.2508(4) 0.6710(3) 0.1697(3) 0.0306(11) Uani 1 1 d . . . . . H211 H 0.249401 0.684426 0.117432 0.037 Uiso 1 1 calc R U . . . C212 C 0.1545(4) 0.6648(4) 0.2078(3) 0.0345(12) Uani 1 1 d . . . . . H212 H 0.087536 0.673686 0.182331 0.041 Uiso 1 1 calc R U . . . C213 C 0.1563(4) 0.6455(4) 0.2837(3) 0.0358(12) Uani 1 1 d . . . . . H213 H 0.090137 0.640518 0.310572 0.043 Uiso 1 1 calc R U . . . C214 C 0.2541(4) 0.6335(4) 0.3209(3) 0.0324(11) Uani 1 1 d . . . . . H214 H 0.254387 0.619795 0.373181 0.039 Uiso 1 1 calc R U . . . C215 C 0.3514(4) 0.6412(3) 0.2825(3) 0.0250(10) Uani 1 1 d . . . . . O216 O 0.4499(3) 0.6306(2) 0.31863(16) 0.0268(7) Uani 1 1 d . . . . . C217 C 0.4484(5) 0.6126(5) 0.3979(3) 0.0526(18) Uani 1 1 d . . . . . H21A H 0.414440 0.552147 0.414586 0.063 Uiso 1 1 calc R U . . . H21B H 0.405134 0.661120 0.417467 0.063 Uiso 1 1 calc R U . . . C218 C 0.5640(5) 0.6118(4) 0.4268(3) 0.0434(15) Uani 1 1 d . . . . . O219 O 0.6410(3) 0.6259(2) 0.38363(18) 0.0304(8) Uani 1 1 d . . . . . O220 O 0.5732(4) 0.5969(4) 0.4953(2) 0.0743(17) Uani 1 1 d . . . . . O230 O 0.5966(2) 0.7825(2) 0.27236(16) 0.0211(6) Uani 1 1 d D . . . . H231 H 0.652(3) 0.811(3) 0.256(3) 0.032 Uiso 1 1 d D U . . . H232 H 0.578(4) 0.803(3) 0.3109(17) 0.032 Uiso 1 1 d D U . . . O240 O 0.6095(3) 0.4997(2) 0.28047(17) 0.0238(7) Uani 1 1 d D . . . . H241 H 0.661(3) 0.484(4) 0.255(3) 0.036 Uiso 1 1 d D U . . . H242 H 0.607(5) 0.473(3) 0.3242(11) 0.036 Uiso 1 1 d D U . . . O301 O 0.7606(2) 0.4008(2) 0.22018(15) 0.0200(6) Uani 1 1 d . . . . . C302 C 0.7822(3) 0.4077(3) 0.1483(2) 0.0204(9) Uani 1 1 d . . . . . C303 C 0.6985(4) 0.4149(3) 0.0962(2) 0.0261(10) Uani 1 1 d . . . . . H303 H 0.625142 0.415167 0.112187 0.031 Uiso 1 1 calc R U . . . C304 C 0.7220(4) 0.4217(3) 0.0222(3) 0.0314(11) Uani 1 1 d . . . . . H304 H 0.664479 0.427312 -0.012420 0.038 Uiso 1 1 calc R U . . . C305 C 0.8284(4) 0.4204(3) -0.0029(2) 0.0313(11) Uani 1 1 d . . . . . H305 H 0.843470 0.424030 -0.054077 0.038 Uiso 1 1 calc R U . . . C306 C 0.9123(4) 0.4138(3) 0.0476(2) 0.0264(10) Uani 1 1 d . . . . . H306 H 0.985216 0.412731 0.030876 0.032 Uiso 1 1 calc R U . . . C307 C 0.8905(4) 0.4089(3) 0.1224(2) 0.0204(9) Uani 1 1 d . . . . . N308 N 0.9694(3) 0.4031(2) 0.17894(19) 0.0200(8) Uani 1 1 d . . . . . C309 C 1.0718(4) 0.4116(3) 0.1651(2) 0.0235(9) Uani 1 1 d . . . . . H309 H 1.092168 0.423281 0.114558 0.028 Uiso 1 1 calc R U . . . C310 C 1.1594(4) 0.4051(3) 0.2184(3) 0.0240(10) Uani 1 1 d . . . . . C311 C 1.2630(4) 0.4201(3) 0.1867(3) 0.0331(11) Uani 1 1 d . . . . . H311 H 1.269365 0.436079 0.134789 0.040 Uiso 1 1 calc R U . . . C312 C 1.3560(4) 0.4123(4) 0.2294(3) 0.0373(12) Uani 1 1 d . . . . . H312 H 1.425040 0.423092 0.206859 0.045 Uiso 1 1 calc R U . . . C313 C 1.3473(4) 0.3887(3) 0.3045(3) 0.0367(12) Uani 1 1 d . . . . . H313 H 1.410878 0.381872 0.333881 0.044 Uiso 1 1 calc R U . . . C314 C 1.2467(4) 0.3747(3) 0.3376(3) 0.0311(11) Uani 1 1 d . . . . . H314 H 1.241554 0.358689 0.389624 0.037 Uiso 1 1 calc R U . . . C315 C 1.1529(4) 0.3842(3) 0.2951(3) 0.0253(10) Uani 1 1 d . . . . . O316 O 1.0517(2) 0.3716(2) 0.32821(16) 0.0236(7) Uani 1 1 d . . . . . C317 C 1.0450(4) 0.3541(4) 0.4078(2) 0.0304(11) Uani 1 1 d . . . . . H31A H 1.085296 0.402044 0.428866 0.037 Uiso 1 1 calc R U . . . H31B H 1.078303 0.293133 0.426104 0.037 Uiso 1 1 calc R U . . . C318 C 0.9278(4) 0.3553(3) 0.4320(2) 0.0275(10) Uani 1 1 d . . . . . O319 O 0.8535(3) 0.3694(2) 0.38537(15) 0.0242(7) Uani 1 1 d . . . . . O320 O 0.9117(3) 0.3422(3) 0.50053(17) 0.0412(9) Uani 1 1 d . . . . . O330 O 0.9072(2) 0.5283(2) 0.27837(16) 0.0215(6) Uani 1 1 d D . . . . H331 H 0.851(3) 0.559(3) 0.264(3) 0.032 Uiso 1 1 d D U . . . H332 H 0.924(4) 0.551(3) 0.3159(18) 0.032 Uiso 1 1 d D U . . . O340 O 0.8990(2) 0.2468(2) 0.27968(16) 0.0204(6) Uani 1 1 d D . . . . H341 H 0.853(3) 0.221(3) 0.256(3) 0.031 Uiso 1 1 d D U . . . H342 H 0.895(4) 0.214(3) 0.3209(14) 0.031 Uiso 1 1 d D U . . . O401 O 0.7608(2) -0.1003(2) 0.22504(15) 0.0189(6) Uani 1 1 d . . . . . C402 C 0.7751(3) -0.0920(3) 0.1525(2) 0.0190(9) Uani 1 1 d . . . . . C403 C 0.6878(4) -0.0843(3) 0.1038(2) 0.0236(9) Uani 1 1 d . . . . . H403 H 0.616061 -0.083604 0.122662 0.028 Uiso 1 1 calc R U . . . C404 C 0.7039(4) -0.0776(3) 0.0289(3) 0.0288(10) Uani 1 1 d . . . . . H404 H 0.643201 -0.071625 -0.003134 0.035 Uiso 1 1 calc R U . . . C405 C 0.8078(4) -0.0796(3) -0.0003(3) 0.0308(11) Uani 1 1 d . . . . . H405 H 0.818049 -0.076504 -0.051977 0.037 Uiso 1 1 calc R U . . . C406 C 0.8963(4) -0.0862(3) 0.0460(2) 0.0251(10) Uani 1 1 d . . . . . H406 H 0.967532 -0.087266 0.026219 0.030 Uiso 1 1 calc R U . . . C407 C 0.8811(3) -0.0912(3) 0.1219(2) 0.0208(9) Uani 1 1 d . . . . . N408 N 0.9652(3) -0.0960(2) 0.17446(19) 0.0201(8) Uani 1 1 d . . . . . C409 C 1.0658(4) -0.0879(3) 0.1557(3) 0.0249(10) Uani 1 1 d . . . . . H409 H 1.079960 -0.079072 0.104187 0.030 Uiso 1 1 calc R U . . . C410 C 1.1600(4) -0.0904(3) 0.2023(3) 0.0247(10) Uani 1 1 d . . . . . C411 C 1.2594(4) -0.0803(3) 0.1640(3) 0.0288(10) Uani 1 1 d . . . . . H411 H 1.259024 -0.073097 0.111640 0.035 Uiso 1 1 calc R U . . . C412 C 1.3566(4) -0.0805(3) 0.1996(3) 0.0311(11) Uani 1 1 d . . . . . H412 H 1.422564 -0.073668 0.172496 0.037 Uiso 1 1 calc R U . . . C413 C 1.3571(4) -0.0906(3) 0.2753(3) 0.0278(10) Uani 1 1 d . . . . . H413 H 1.424105 -0.090707 0.300560 0.033 Uiso 1 1 calc R U . . . C414 C 1.2617(4) -0.1007(3) 0.3152(3) 0.0288(10) Uani 1 1 d . . . . . H414 H 1.263625 -0.107013 0.367478 0.035 Uiso 1 1 calc R U . . . C415 C 1.1625(3) -0.1015(3) 0.2793(2) 0.0220(9) Uani 1 1 d . . . . . O416 O 1.0662(2) -0.1130(2) 0.31845(17) 0.0257(7) Uani 1 1 d . . . . . C417 C 1.0706(4) -0.1143(3) 0.3973(2) 0.0269(10) Uani 1 1 d . . . . . H41A H 1.104071 -0.056695 0.408169 0.032 Uiso 1 1 calc R U . . . H41B H 1.116040 -0.167213 0.419718 0.032 Uiso 1 1 calc R U . . . C418 C 0.9579(4) -0.1227(3) 0.4303(2) 0.0263(10) Uani 1 1 d . . . . . O419 O 0.8769(2) -0.1292(2) 0.38787(16) 0.0240(7) Uani 1 1 d . . . . . O420 O 0.9522(3) -0.1245(3) 0.49751(17) 0.0338(8) Uani 1 1 d . . . . . O430 O 0.9065(2) 0.0296(2) 0.27726(16) 0.0207(6) Uani 1 1 d D . . . . H431 H 0.849(2) 0.057(3) 0.263(3) 0.031 Uiso 1 1 d D U . . . H432 H 0.912(4) 0.046(3) 0.3192(13) 0.031 Uiso 1 1 d D U . . . O440 O 0.9031(2) -0.2524(2) 0.28243(16) 0.0213(6) Uani 1 1 d D . . . . H441 H 0.853(3) -0.275(3) 0.261(3) 0.032 Uiso 1 1 d D U . . . H442 H 0.902(4) -0.286(3) 0.3238(14) 0.032 Uiso 1 1 d D U . . . O510 O 1.1072(3) -0.1147(2) 0.59800(17) 0.0261(7) Uani 1 1 d D . . . . H511 H 1.062(3) -0.115(4) 0.5642(19) 0.039 Uiso 1 1 d D U . . . H512 H 1.1700(16) -0.112(4) 0.580(2) 0.039 Uiso 1 1 d D U . . . O520 O 0.5580(3) -0.1387(2) 0.40102(17) 0.0291(7) Uani 1 1 d D . . . . H521 H 0.507(3) -0.133(4) 0.430(2) 0.044 Uiso 1 1 d D U . . . H522 H 0.613(2) -0.159(4) 0.425(2) 0.044 Uiso 1 1 d D U . . . O530 O 0.9298(3) -0.3862(2) 0.40525(16) 0.0277(7) Uani 1 1 d D . . . . H531 H 0.975(3) -0.367(4) 0.434(2) 0.041 Uiso 1 1 d D U . . . H532 H 0.877(3) -0.409(4) 0.430(2) 0.041 Uiso 1 1 d D U . . . O540 O 0.5923(4) 0.3715(2) 0.40838(19) 0.0429(10) Uani 1 1 d . . . . . O550 O 0.7233(3) -0.2321(2) 0.47556(19) 0.0348(8) Uani 1 1 d . . . . . O560 O 0.7886(3) 0.5167(3) 0.5033(3) 0.0560(12) Uani 1 1 d . . . . . O570 O 0.7113(4) 0.2771(4) 0.5175(3) 0.0662(13) Uani 1 1 d D . . . . H571 H 0.696(6) 0.223(3) 0.508(5) 0.099 Uiso 1 1 d D U . . . H572 H 0.7794(16) 0.277(5) 0.526(5) 0.099 Uiso 1 1 d D U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0163(4) 0.0188(4) 0.0144(3) -0.0003(3) 0.0031(3) -0.0004(3) Ni2 0.0193(4) 0.0190(4) 0.0177(4) 0.0010(3) -0.0039(3) 0.0005(3) Ni3 0.0183(4) 0.0191(4) 0.0148(4) 0.0004(3) -0.0012(3) 0.0009(3) Ni4 0.0174(4) 0.0192(4) 0.0162(4) -0.0012(3) -0.0005(3) 0.0002(3) O101 0.0186(15) 0.0224(16) 0.0126(14) 0.0004(11) -0.0007(11) -0.0008(12) C102 0.018(2) 0.019(2) 0.016(2) -0.0005(16) 0.0047(16) -0.0012(16) C103 0.021(2) 0.027(2) 0.020(2) -0.0004(18) 0.0040(17) 0.0001(18) C104 0.030(3) 0.030(3) 0.017(2) 0.0012(19) 0.0072(18) 0.0023(19) C105 0.034(3) 0.031(3) 0.015(2) -0.0002(19) -0.0016(18) 0.002(2) C106 0.021(2) 0.026(2) 0.022(2) -0.0010(18) -0.0058(18) 0.0018(18) C107 0.019(2) 0.021(2) 0.016(2) -0.0009(17) -0.0002(16) 0.0010(17) N108 0.0148(18) 0.0193(19) 0.0197(18) -0.0004(14) 0.0014(14) 0.0017(14) C109 0.023(2) 0.024(2) 0.026(2) -0.0044(19) -0.0024(18) 0.0014(18) C110 0.016(2) 0.020(2) 0.032(2) -0.0024(19) 0.0015(18) 0.0001(17) C111 0.020(2) 0.030(3) 0.033(3) -0.006(2) -0.0026(19) 0.0021(18) C112 0.014(2) 0.027(3) 0.048(3) -0.006(2) 0.000(2) 0.0001(18) C113 0.021(2) 0.025(3) 0.040(3) -0.007(2) 0.007(2) -0.0007(18) C114 0.029(3) 0.024(2) 0.027(2) -0.0021(19) 0.0045(19) -0.0003(19) C115 0.019(2) 0.015(2) 0.031(2) -0.0020(18) 0.0004(18) 0.0011(16) O116 0.0199(15) 0.0282(17) 0.0197(15) -0.0016(13) 0.0052(12) -0.0007(12) C117 0.027(2) 0.031(3) 0.018(2) 0.0007(19) 0.0036(18) 0.0029(19) C118 0.030(2) 0.023(2) 0.019(2) -0.0006(18) 0.0066(19) 0.0004(18) O119 0.0265(17) 0.0272(17) 0.0156(15) -0.0003(12) 0.0035(12) 0.0002(13) O120 0.0308(18) 0.044(2) 0.0163(16) -0.0003(14) 0.0029(13) 0.0015(15) O130 0.0219(16) 0.0216(16) 0.0192(15) -0.0016(12) 0.0052(12) -0.0027(12) O140 0.0252(17) 0.0190(16) 0.0217(16) -0.0008(12) 0.0084(13) 0.0006(12) O201 0.0197(15) 0.0227(16) 0.0249(16) -0.0022(13) -0.0034(12) 0.0007(12) C202 0.025(2) 0.017(2) 0.027(2) -0.0011(18) 0.0018(18) 0.0025(17) C203 0.019(2) 0.029(3) 0.044(3) -0.003(2) 0.005(2) 0.0023(19) C204 0.039(3) 0.032(3) 0.034(3) 0.001(2) 0.017(2) 0.007(2) C205 0.043(3) 0.033(3) 0.025(2) -0.002(2) 0.006(2) 0.009(2) C206 0.031(3) 0.024(2) 0.024(2) -0.0007(19) 0.0008(19) 0.0065(19) C207 0.024(2) 0.018(2) 0.026(2) -0.0006(18) 0.0023(18) 0.0027(17) N208 0.0183(19) 0.0179(19) 0.0185(17) -0.0001(14) -0.0002(14) 0.0002(14) C209 0.027(2) 0.025(2) 0.017(2) -0.0003(18) -0.0043(18) -0.0013(18) C210 0.019(2) 0.022(2) 0.023(2) -0.0010(18) -0.0017(17) 0.0001(17) C211 0.025(2) 0.033(3) 0.032(3) 0.003(2) -0.008(2) 0.000(2) C212 0.021(2) 0.036(3) 0.044(3) 0.001(2) -0.006(2) 0.002(2) C213 0.022(3) 0.034(3) 0.053(3) -0.012(2) 0.010(2) -0.003(2) C214 0.029(3) 0.040(3) 0.029(3) -0.006(2) 0.006(2) -0.007(2) C215 0.020(2) 0.022(2) 0.034(3) -0.0058(19) -0.0024(19) -0.0016(17) O216 0.0263(17) 0.0374(19) 0.0153(15) 0.0013(13) -0.0018(12) -0.0044(14) C217 0.049(4) 0.092(5) 0.015(2) 0.001(3) 0.002(2) -0.035(3) C218 0.053(4) 0.054(4) 0.019(2) 0.012(2) -0.013(2) -0.024(3) O219 0.0361(19) 0.0282(18) 0.0251(17) 0.0021(14) -0.0122(15) -0.0031(14) O220 0.070(3) 0.128(5) 0.019(2) 0.016(2) -0.0116(19) -0.057(3) O230 0.0213(16) 0.0216(16) 0.0204(15) -0.0028(13) 0.0018(12) -0.0017(12) O240 0.0249(17) 0.0200(17) 0.0244(16) 0.0029(13) 0.0020(13) 0.0016(13) O301 0.0190(15) 0.0241(16) 0.0156(14) 0.0011(12) 0.0002(11) 0.0005(12) C302 0.022(2) 0.016(2) 0.022(2) 0.0022(17) -0.0006(17) -0.0008(17) C303 0.026(2) 0.026(3) 0.025(2) 0.0014(19) -0.0062(19) 0.0003(19) C304 0.038(3) 0.030(3) 0.024(2) 0.003(2) -0.012(2) -0.003(2) C305 0.047(3) 0.032(3) 0.014(2) 0.0001(19) -0.003(2) -0.006(2) C306 0.033(3) 0.024(2) 0.021(2) 0.0007(19) 0.0021(19) -0.0014(19) C307 0.025(2) 0.018(2) 0.017(2) 0.0000(17) -0.0026(17) 0.0001(17) N308 0.024(2) 0.0169(19) 0.0179(18) 0.0004(14) -0.0014(15) 0.0025(14) C309 0.023(2) 0.025(2) 0.021(2) -0.0005(18) 0.0022(18) -0.0012(18) C310 0.020(2) 0.021(2) 0.032(2) -0.0045(19) 0.0036(19) 0.0005(17) C311 0.023(2) 0.029(3) 0.047(3) -0.005(2) 0.007(2) 0.000(2) C312 0.020(2) 0.033(3) 0.061(4) -0.010(3) 0.000(2) 0.000(2) C313 0.019(2) 0.029(3) 0.063(4) -0.011(3) -0.013(2) 0.0053(19) C314 0.026(3) 0.026(3) 0.041(3) -0.004(2) -0.014(2) 0.0025(19) C315 0.018(2) 0.020(2) 0.038(3) -0.004(2) -0.0036(19) 0.0005(17) O316 0.0217(16) 0.0301(18) 0.0175(15) 0.0013(13) -0.0055(12) 0.0017(13) C317 0.035(3) 0.036(3) 0.018(2) 0.007(2) -0.0081(19) -0.005(2) C318 0.038(3) 0.023(2) 0.021(2) -0.0004(18) -0.003(2) -0.005(2) O319 0.0300(17) 0.0265(17) 0.0141(14) 0.0033(12) -0.0002(13) 0.0011(13) O320 0.050(2) 0.059(2) 0.0140(16) 0.0014(15) -0.0042(15) -0.0240(19) O330 0.0237(16) 0.0207(17) 0.0201(15) -0.0029(13) -0.0040(13) 0.0023(12) O340 0.0209(16) 0.0190(16) 0.0199(15) 0.0018(12) -0.0040(12) -0.0019(12) O401 0.0158(14) 0.0234(16) 0.0169(14) -0.0008(12) 0.0019(11) 0.0004(11) C402 0.022(2) 0.016(2) 0.018(2) -0.0009(17) 0.0020(17) -0.0014(16) C403 0.019(2) 0.026(2) 0.024(2) 0.0008(19) 0.0003(18) -0.0023(18) C404 0.033(3) 0.031(3) 0.021(2) 0.0002(19) -0.0061(19) -0.005(2) C405 0.038(3) 0.035(3) 0.020(2) -0.004(2) 0.003(2) -0.008(2) C406 0.027(2) 0.029(3) 0.019(2) -0.0036(19) 0.0080(18) -0.0039(19) C407 0.020(2) 0.020(2) 0.022(2) -0.0023(18) 0.0008(17) -0.0023(17) N408 0.0205(19) 0.0187(19) 0.0212(18) -0.0040(15) 0.0005(15) 0.0019(14) C409 0.020(2) 0.029(3) 0.027(2) -0.009(2) 0.0047(18) -0.0021(18) C410 0.019(2) 0.024(2) 0.033(3) -0.008(2) 0.0047(19) -0.0018(17) C411 0.024(2) 0.036(3) 0.027(2) -0.008(2) 0.0046(19) -0.002(2) C412 0.019(2) 0.035(3) 0.041(3) -0.008(2) 0.005(2) 0.0000(19) C413 0.019(2) 0.030(3) 0.033(3) 0.000(2) -0.0013(19) 0.0029(18) C414 0.029(3) 0.026(3) 0.030(3) -0.001(2) -0.002(2) 0.0020(19) C415 0.018(2) 0.020(2) 0.028(2) -0.0050(18) 0.0056(18) -0.0017(17) O416 0.0231(16) 0.0313(18) 0.0229(16) -0.0052(13) -0.0029(13) 0.0017(13) C417 0.026(2) 0.036(3) 0.017(2) 0.0015(19) -0.0017(18) -0.001(2) C418 0.031(3) 0.025(2) 0.022(2) 0.0000(19) -0.0030(19) 0.0007(19) O419 0.0291(17) 0.0274(17) 0.0149(14) -0.0006(12) -0.0016(13) -0.0029(13) O420 0.0311(19) 0.052(2) 0.0169(16) -0.0019(15) -0.0002(13) -0.0006(16) O430 0.0207(16) 0.0210(16) 0.0204(15) -0.0035(13) -0.0041(12) 0.0023(12) O440 0.0225(16) 0.0206(16) 0.0200(15) 0.0002(12) -0.0048(12) -0.0011(12) O510 0.0243(17) 0.0336(19) 0.0199(16) -0.0023(14) 0.0006(13) 0.0000(14) O520 0.0323(19) 0.0351(19) 0.0179(16) 0.0015(14) 0.0064(13) 0.0037(15) O530 0.0315(19) 0.0349(19) 0.0157(15) 0.0000(13) 0.0002(13) -0.0070(14) O540 0.075(3) 0.029(2) 0.0234(18) -0.0002(15) -0.0183(18) -0.0002(18) O550 0.0254(18) 0.040(2) 0.0375(19) -0.0010(16) -0.0011(15) -0.0005(15) O560 0.039(2) 0.038(2) 0.086(3) 0.008(2) 0.024(2) 0.0027(18) O570 0.062(3) 0.072(3) 0.065(3) -0.009(3) -0.004(3) -0.001(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 0.00 1.00 0.0400 0.00 0.00 -1.00 0.0400 0.00 -1.00 0.00 0.1200 0.00 1.00 0.00 0.1500 -1.00 0.00 -1.00 0.0700 1.00 0.00 1.00 0.0500 1.00 -1.00 1.00 0.0800 2.00 2.00 1.00 0.1200 -2.00 -2.00 -1.00 0.1000 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 N108 Ni1 O101 84.03(13) . . ? N108 Ni1 O119 170.15(13) . . ? O101 Ni1 O119 105.81(12) . . ? N108 Ni1 O140 89.83(14) . . ? O101 Ni1 O140 90.32(12) . . ? O119 Ni1 O140 89.85(13) . . ? N108 Ni1 O130 90.20(13) . . ? O101 Ni1 O130 91.23(12) . . ? O119 Ni1 O130 89.86(12) . . ? O140 Ni1 O130 178.43(12) . . ? N108 Ni1 O116 90.45(13) . . ? O101 Ni1 O116 174.48(12) . . ? O119 Ni1 O116 79.71(12) . . ? O140 Ni1 O116 89.64(12) . . ? O130 Ni1 O116 88.79(12) . . ? N208 Ni2 O201 83.99(13) . . ? N208 Ni2 O219 169.47(14) . . ? O201 Ni2 O219 106.54(13) . . ? N208 Ni2 O240 90.95(14) . . ? O201 Ni2 O240 91.83(12) . . ? O219 Ni2 O240 88.91(13) . . ? N208 Ni2 O230 90.12(13) . . ? O201 Ni2 O230 91.47(12) . . ? O219 Ni2 O230 89.44(13) . . ? O240 Ni2 O230 176.61(13) . . ? N208 Ni2 O216 89.78(13) . . ? O201 Ni2 O216 173.77(12) . . ? O219 Ni2 O216 79.69(13) . . ? O240 Ni2 O216 88.03(13) . . ? O230 Ni2 O216 88.76(13) . . ? N308 Ni3 O301 83.98(13) . . ? N308 Ni3 O319 170.68(14) . . ? O301 Ni3 O319 105.34(12) . . ? N308 Ni3 O340 90.01(13) . . ? O301 Ni3 O340 90.74(12) . . ? O319 Ni3 O340 89.76(12) . . ? N308 Ni3 O330 89.84(13) . . ? O301 Ni3 O330 91.82(12) . . ? O319 Ni3 O330 89.97(12) . . ? O340 Ni3 O330 177.40(12) . . ? N308 Ni3 O316 90.41(13) . . ? O301 Ni3 O316 174.23(12) . . ? O319 Ni3 O316 80.27(12) . . ? O340 Ni3 O316 87.90(12) . . ? O330 Ni3 O316 89.51(12) . . ? N408 Ni4 O401 83.19(13) . . ? N408 Ni4 O419 168.43(14) . . ? O401 Ni4 O419 108.37(12) . . ? N408 Ni4 O440 91.20(13) . . ? O401 Ni4 O440 90.28(12) . . ? O419 Ni4 O440 88.45(12) . . ? N408 Ni4 O430 90.98(13) . . ? O401 Ni4 O430 90.40(12) . . ? O419 Ni4 O430 89.33(12) . . ? O440 Ni4 O430 177.78(12) . . ? N408 Ni4 O416 89.16(13) . . ? O401 Ni4 O416 171.77(12) . . ? O419 Ni4 O416 79.31(12) . . ? O440 Ni4 O416 92.94(12) . . ? O430 Ni4 O416 86.68(12) . . ? C102 O101 Ni1 110.6(2) . . ? O101 C102 C103 121.1(4) . . ? O101 C102 C107 120.2(4) . . ? C103 C102 C107 118.6(4) . . ? C104 C103 C102 120.3(4) . . ? C103 C104 C105 120.8(4) . . ? C106 C105 C104 120.0(4) . . ? C105 C106 C107 119.6(4) . . ? C106 C107 C102 120.6(4) . . ? C106 C107 N108 124.2(4) . . ? C102 C107 N108 115.1(4) . . ? C109 N108 C107 123.7(4) . . ? C109 N108 Ni1 126.4(3) . . ? C107 N108 Ni1 110.0(3) . . ? N108 C109 C110 127.5(4) . . ? C111 C110 C115 117.5(4) . . ? C111 C110 C109 114.5(4) . . ? C115 C110 C109 128.1(4) . . ? C112 C111 C110 122.7(5) . . ? C111 C112 C113 118.3(4) . . ? C114 C113 C112 121.1(4) . . ? C113 C114 C115 120.2(4) . . ? O116 C115 C114 120.9(4) . . ? O116 C115 C110 118.7(4) . . ? C114 C115 C110 120.3(4) . . ? C115 O116 C117 117.8(3) . . ? C115 O116 Ni1 128.8(3) . . ? C117 O116 Ni1 113.2(2) . . ? O116 C117 C118 110.1(3) . . ? O120 C118 O119 125.5(4) . . ? O120 C118 C117 115.3(4) . . ? O119 C118 C117 119.2(4) . . ? C118 O119 Ni1 117.7(3) . . ? C202 O201 Ni2 110.2(3) . . ? O201 C202 C203 122.1(4) . . ? O201 C202 C207 120.8(4) . . ? C203 C202 C207 117.1(4) . . ? C204 C203 C202 121.7(5) . . ? C203 C204 C205 120.5(5) . . ? C206 C205 C204 119.4(5) . . ? C205 C206 C207 120.8(5) . . ? C206 C207 C202 120.4(4) . . ? C206 C207 N208 125.3(4) . . ? C202 C207 N208 114.2(4) . . ? C209 N208 C207 122.4(4) . . ? C209 N208 Ni2 126.8(3) . . ? C207 N208 Ni2 110.6(3) . . ? N208 C209 C210 127.7(4) . . ? C215 C210 C211 117.8(4) . . ? C215 C210 C209 127.8(4) . . ? C211 C210 C209 114.4(4) . . ? C212 C211 C210 122.1(5) . . ? C211 C212 C213 119.1(5) . . ? C212 C213 C214 120.5(5) . . ? C215 C214 C213 120.5(5) . . ? O216 C215 C214 121.4(4) . . ? O216 C215 C210 118.6(4) . . ? C214 C215 C210 120.0(4) . . ? C215 O216 C217 117.9(4) . . ? C215 O216 Ni2 129.0(3) . . ? C217 O216 Ni2 113.2(3) . . ? O216 C217 C218 109.6(4) . . ? O219 C218 O220 124.2(5) . . ? O219 C218 C217 120.3(4) . . ? O220 C218 C217 115.5(5) . . ? C218 O219 Ni2 117.0(3) . . ? C302 O301 Ni3 110.0(3) . . ? O301 C302 C303 121.1(4) . . ? O301 C302 C307 120.8(4) . . ? C303 C302 C307 118.1(4) . . ? C304 C303 C302 120.4(4) . . ? C303 C304 C305 121.2(4) . . ? C306 C305 C304 119.3(4) . . ? C305 C306 C307 120.5(4) . . ? C306 C307 C302 120.4(4) . . ? C306 C307 N308 125.5(4) . . ? C302 C307 N308 114.1(4) . . ? C309 N308 C307 122.5(4) . . ? C309 N308 Ni3 126.4(3) . . ? C307 N308 Ni3 111.0(3) . . ? N308 C309 C310 127.0(4) . . ? C315 C310 C311 117.6(4) . . ? C315 C310 C309 128.3(4) . . ? C311 C310 C309 114.1(4) . . ? C312 C311 C310 121.7(5) . . ? C313 C312 C311 119.4(5) . . ? C312 C313 C314 120.4(5) . . ? C313 C314 C315 120.3(5) . . ? O316 C315 C314 120.6(4) . . ? O316 C315 C310 118.9(4) . . ? C314 C315 C310 120.5(4) . . ? C315 O316 C317 118.8(3) . . ? C315 O316 Ni3 128.1(3) . . ? C317 O316 Ni3 112.8(3) . . ? O316 C317 C318 109.9(4) . . ? O319 C318 O320 123.7(5) . . ? O319 C318 C317 120.5(4) . . ? O320 C318 C317 115.8(4) . . ? C318 O319 Ni3 116.5(3) . . ? C402 O401 Ni4 110.7(2) . . ? O401 C402 C403 121.9(4) . . ? O401 C402 C407 120.5(4) . . ? C403 C402 C407 117.6(4) . . ? C404 C403 C402 121.2(4) . . ? C403 C404 C405 120.7(4) . . ? C406 C405 C404 119.8(4) . . ? C405 C406 C407 120.0(4) . . ? C406 C407 N408 125.1(4) . . ? C406 C407 C402 120.6(4) . . ? N408 C407 C402 114.3(4) . . ? C409 N408 C407 122.3(4) . . ? C409 N408 Ni4 126.5(3) . . ? C407 N408 Ni4 111.2(3) . . ? N408 C409 C410 128.8(4) . . ? C415 C410 C411 118.0(4) . . ? C415 C410 C409 127.6(4) . . ? C411 C410 C409 114.5(4) . . ? C412 C411 C410 122.2(5) . . ? C411 C412 C413 118.9(4) . . ? C412 C413 C414 121.0(4) . . ? C413 C414 C415 120.4(4) . . ? O416 C415 C414 121.2(4) . . ? O416 C415 C410 119.2(4) . . ? C414 C415 C410 119.6(4) . . ? C415 O416 C417 117.7(3) . . ? C415 O416 Ni4 128.7(3) . . ? C417 O416 Ni4 113.0(3) . . ? O416 C417 C418 110.5(4) . . ? O420 C418 O419 125.0(4) . . ? O420 C418 C417 115.9(4) . . ? O419 C418 C417 119.1(4) . . ? C418 O419 Ni4 117.5(3) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N108 2.002(4) . ? Ni1 O101 2.008(3) . ? Ni1 O119 2.033(3) . ? Ni1 O140 2.045(3) . ? Ni1 O130 2.061(3) . ? Ni1 O116 2.097(3) . ? Ni2 N208 2.000(4) . ? Ni2 O201 2.019(3) . ? Ni2 O219 2.033(3) . ? Ni2 O240 2.054(3) . ? Ni2 O230 2.062(3) . ? Ni2 O216 2.095(3) . ? Ni3 N308 1.991(4) . ? Ni3 O301 2.015(3) . ? Ni3 O319 2.026(3) . ? Ni3 O340 2.051(3) . ? Ni3 O330 2.065(3) . ? Ni3 O316 2.090(3) . ? Ni4 N408 2.011(4) . ? Ni4 O401 2.027(3) . ? Ni4 O419 2.029(3) . ? Ni4 O440 2.051(3) . ? Ni4 O430 2.059(3) . ? Ni4 O416 2.125(3) . ? O101 C102 1.335(5) . ? C102 C103 1.401(6) . ? C102 C107 1.403(6) . ? C103 C104 1.378(6) . ? C104 C105 1.387(7) . ? C105 C106 1.384(6) . ? C106 C107 1.397(6) . ? C107 N108 1.426(5) . ? N108 C109 1.277(6) . ? C109 C110 1.474(6) . ? C110 C111 1.402(6) . ? C110 C115 1.404(6) . ? C111 C112 1.382(7) . ? C112 C113 1.386(7) . ? C113 C114 1.382(7) . ? C114 C115 1.393(6) . ? C115 O116 1.376(5) . ? O116 C117 1.447(5) . ? C117 C118 1.524(6) . ? C118 O120 1.254(5) . ? C118 O119 1.255(5) . ? O201 C202 1.333(5) . ? C202 C203 1.408(6) . ? C202 C207 1.414(6) . ? C203 C204 1.362(7) . ? C204 C205 1.400(8) . ? C205 C206 1.366(7) . ? C206 C207 1.396(6) . ? C207 N208 1.429(6) . ? N208 C209 1.269(6) . ? C209 C210 1.468(6) . ? C210 C215 1.398(6) . ? C210 C211 1.405(6) . ? C211 C212 1.373(7) . ? C212 C213 1.378(8) . ? C213 C214 1.387(7) . ? C214 C215 1.387(7) . ? C215 O216 1.385(5) . ? O216 C217 1.439(6) . ? C217 C218 1.524(8) . ? C218 O219 1.234(7) . ? C218 O220 1.249(6) . ? O301 C302 1.333(5) . ? C302 C303 1.404(6) . ? C302 C307 1.415(6) . ? C303 C304 1.378(7) . ? C304 C305 1.389(7) . ? C305 C306 1.386(7) . ? C306 C307 1.389(6) . ? C307 N308 1.420(5) . ? N308 C309 1.292(6) . ? C309 C310 1.456(6) . ? C310 C315 1.397(7) . ? C310 C311 1.408(6) . ? C311 C312 1.387(7) . ? C312 C313 1.374(8) . ? C313 C314 1.384(7) . ? C314 C315 1.393(6) . ? C315 O316 1.389(5) . ? O316 C317 1.447(5) . ? C317 C318 1.511(7) . ? C318 O319 1.252(6) . ? C318 O320 1.258(6) . ? O401 C402 1.330(5) . ? C402 C403 1.397(6) . ? C402 C407 1.419(6) . ? C403 C404 1.376(6) . ? C404 C405 1.390(7) . ? C405 C406 1.382(7) . ? C406 C407 1.396(6) . ? C407 N408 1.415(6) . ? N408 C409 1.289(6) . ? C409 C410 1.444(6) . ? C410 C415 1.398(7) . ? C410 C411 1.410(6) . ? C411 C412 1.369(7) . ? C412 C413 1.375(7) . ? C413 C414 1.381(7) . ? C414 C415 1.395(7) . ? C415 O416 1.384(5) . ? O416 C417 1.445(5) . ? C417 C418 1.513(6) . ? C418 O420 1.232(6) . ? C418 O419 1.284(5) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O130 H131 O301 0.839(10) 1.94(2) 2.742(4) 160(5) . yes O130 H132 O540 0.839(10) 1.990(17) 2.811(5) 166(5) . yes O140 H141 O401 0.837(10) 1.89(2) 2.693(4) 160(5) . yes O140 H142 O520 0.836(10) 1.921(14) 2.750(4) 171(5) . yes O230 H231 O401 0.841(10) 1.900(16) 2.725(4) 167(5) 1_565 yes O230 H232 O520 0.840(10) 1.980(14) 2.811(4) 170(5) 1_565 yes O240 H241 O301 0.841(10) 1.89(3) 2.678(4) 155(5) . yes O240 H242 O540 0.839(10) 1.99(2) 2.787(5) 159(5) . yes O330 H331 O201 0.837(10) 1.926(18) 2.743(4) 165(5) . yes O330 H332 O530 0.836(10) 1.994(16) 2.817(4) 168(5) 1_565 yes O340 H341 O101 0.834(10) 1.875(15) 2.699(4) 169(5) . yes O340 H342 O510 0.837(10) 1.917(17) 2.737(4) 166(5) 2_756 yes O430 H431 O101 0.837(10) 1.929(19) 2.740(4) 163(5) . yes O430 H432 O510 0.839(10) 1.96(2) 2.765(4) 161(5) 2_756 yes O440 H441 O201 0.838(10) 1.883(15) 2.711(4) 170(5) 1_545 yes O440 H442 O530 0.839(10) 1.96(2) 2.775(4) 162(5) . yes O510 H511 O420 0.839(10) 1.850(12) 2.685(5) 173(5) . yes O510 H512 O119 0.838(10) 2.11(3) 2.823(4) 143(4) 2_756 yes O520 H521 O120 0.837(10) 1.917(12) 2.751(5) 175(5) 2_656 yes O520 H522 O550 0.839(10) 1.881(18) 2.703(5) 166(6) . yes O530 H531 O320 0.842(10) 1.928(14) 2.762(5) 171(6) 2_756 yes O570 H571 O120 0.857(10) 1.95(3) 2.758(6) 158(8) . yes O570 H572 O320 0.854(10) 1.92(5) 2.661(6) 145(8) . yes