#------------------------------------------------------------------------------ #$Date: 2021-09-29 10:47:37 +0300 (Wed, 29 Sep 2021) $ #$Revision: 269364 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/47/1564743.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_1564743 loop_ _publ_author_name 'Mou, Wen-Yu' 'Li, Tao' 'Xie, Bin' 'Zhang, Dong-Liang' 'Lai, Chuan' 'Deng, Cheng-Long' 'Cao, Jia-Xi' 'Bai, Xiao-Xue' 'Liu, Xiao-Qiang' _publ_section_title ; Neutral heteroleptic nickel complexes incorporating maleonitriledithiolate and bis(diphenylphosphanyl)amine as robust molecular electrocatalysts for hydrogen evolution ; _journal_name_full 'Inorganica Chimica Acta' _journal_page_first 119587 _journal_paper_doi 10.1016/j.ica.2020.119587 _journal_volume 507 _journal_year 2020 _chemical_formula_sum 'C32 H29 N3 Ni P2 S3' _chemical_formula_weight 672.41 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 103.4270(14) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.18441(13) _cell_length_b 17.6653(2) _cell_length_c 19.7935(3) _cell_measurement_reflns_used 3331 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 73.2910 _cell_measurement_theta_min 4.5730 _cell_volume 3123.62(8) _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-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.950 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_unetI/netI 0.0375 _diffrn_reflns_Laue_measured_fraction_full 0.950 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 10605 _diffrn_reflns_point_group_measured_fraction_full 0.950 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 65.999 _diffrn_reflns_theta_min 3.395 _exptl_absorpt_coefficient_mu 3.950 _exptl_absorpt_correction_T_max 0.532 _exptl_absorpt_correction_T_min 0.496 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour pink _exptl_crystal_density_diffrn 1.430 _exptl_crystal_description block _exptl_crystal_F_000 1392 _exptl_crystal_size_max 0.190 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.160 _refine_diff_density_max 0.728 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.087 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 371 _refine_ls_number_reflns 5366 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.018 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0416 _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^)+(0.0799P)^2^+0.2181P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1107 _refine_ls_wR_factor_ref 0.1164 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 4744 _reflns_number_total 5366 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ICA-2020-507-119587.cif _cod_data_source_block 2 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1564743 _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 0.521 _shelx_estimated_absorpt_t_max 0.571 _shelxl_version_number 2013-2 _shelx_res_file ; TITL exp_26472_a.res in P2(1)/n CELL 1.54184 9.184412 17.665269 19.793478 90 103.427 90 ZERR 4 0.000127 0.000226 0.000307 0 0.0014 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N Ni P S UNIT 128 116 12 4 8 12 OMIT -3 132 REM Old TITL exp_26472_a.res in P2(1)/n New: P21/c REM SHELXT solution in P2(1)/n REM R1 0.105, Rweak 0.008, Alpha 0.027, Orientation as input REM Formula found by SHELXT: C32 N3 Ni S5 REM REM REM L.S. 20 ACTA BOND $H FMAP 2 PLAN -20 SIZE 0.19 0.17 0.16 WGHT 0.079900 0.218100 FVAR 0.31411 NI1 4 0.616808 0.621269 0.341199 11.00000 0.02060 0.01333 = 0.01567 0.00122 0.00727 0.00092 S1 6 0.543822 0.631537 0.436286 11.00000 0.03456 0.01730 = 0.01955 0.00341 0.01411 0.00391 S2 6 0.603141 0.740559 0.320114 11.00000 0.03498 0.01447 = 0.02472 0.00325 0.01653 0.00223 S3 6 0.373523 0.329737 0.088577 11.00000 0.04085 0.02992 = 0.02259 -0.00371 0.00133 -0.01333 P1 5 0.631742 0.499316 0.340611 11.00000 0.01833 0.01387 = 0.01458 0.00154 0.00474 0.00021 P2 5 0.694726 0.591198 0.250511 11.00000 0.01872 0.01467 = 0.01452 0.00188 0.00572 0.00087 N1 3 0.679907 0.496708 0.262747 11.00000 0.02096 0.01473 = 0.01549 0.00194 0.00494 0.00193 N2 3 0.425390 0.777279 0.547019 11.00000 0.04702 0.03406 = 0.02263 0.00042 0.00997 0.01425 N3 3 0.516038 0.921132 0.396843 11.00000 0.06606 0.02066 = 0.05467 -0.00046 0.03455 0.00201 C1 1 0.464525 0.443604 0.333159 11.00000 0.01983 0.02037 = 0.01359 0.00088 0.00607 -0.00015 C2 1 0.465328 0.366787 0.349608 11.00000 0.02407 0.01888 = 0.01923 0.00065 0.00255 -0.00120 AFIX 43 H2 2 0.555087 0.342532 0.369172 11.00000 -1.20000 AFIX 0 C3 1 0.332268 0.326816 0.336736 11.00000 0.03276 0.02108 = 0.02301 -0.00055 0.00401 -0.00538 AFIX 43 H3 2 0.332479 0.276084 0.349310 11.00000 -1.20000 AFIX 0 C4 1 0.198925 0.361656 0.305327 11.00000 0.02424 0.03853 = 0.03086 -0.00320 0.00522 -0.01215 AFIX 43 H4 2 0.110346 0.333998 0.295518 11.00000 -1.20000 AFIX 0 C5 1 0.197425 0.437693 0.288510 11.00000 0.01775 0.04194 = 0.03794 0.00848 0.00324 0.00247 AFIX 43 H5 2 0.107871 0.461095 0.267123 11.00000 -1.20000 AFIX 0 C6 1 0.329420 0.479091 0.303522 11.00000 0.02294 0.02500 = 0.03205 0.00819 0.00778 0.00260 AFIX 43 H6 2 0.327644 0.530628 0.293771 11.00000 -1.20000 AFIX 0 C7 1 0.775732 0.453204 0.404860 11.00000 0.02147 0.01333 = 0.01702 -0.00025 0.00098 -0.00113 C8 1 0.921725 0.447529 0.396507 11.00000 0.02523 0.02111 = 0.02087 -0.00049 0.00458 -0.00125 AFIX 43 H8 2 0.944475 0.464329 0.355630 11.00000 -1.20000 AFIX 0 C9 1 1.033160 0.417015 0.448725 11.00000 0.02367 0.02353 = 0.03047 -0.00813 -0.00110 0.00315 AFIX 43 H9 2 1.130376 0.413233 0.442734 11.00000 -1.20000 AFIX 0 C10 1 1.000475 0.392121 0.509792 11.00000 0.03121 0.02210 = 0.02174 0.00128 -0.00857 0.00254 AFIX 43 H10 2 1.075405 0.371219 0.544623 11.00000 -1.20000 AFIX 0 C11 1 0.855234 0.398399 0.519050 11.00000 0.03781 0.02737 = 0.01797 0.00342 -0.00006 -0.00569 AFIX 43 H11 2 0.833489 0.382047 0.560277 11.00000 -1.20000 AFIX 0 C12 1 0.743072 0.428899 0.467095 11.00000 0.02424 0.02494 = 0.01813 -0.00053 0.00261 -0.00530 AFIX 43 H12 2 0.646254 0.433244 0.473491 11.00000 -1.20000 AFIX 0 C13 1 0.582120 0.620747 0.167438 11.00000 0.02312 0.01990 = 0.01691 0.00317 0.00841 0.00601 C14 1 0.444870 0.588260 0.138119 11.00000 0.02424 0.02895 = 0.02160 0.00517 0.00741 0.00365 AFIX 43 H14 2 0.412485 0.546493 0.159215 11.00000 -1.20000 AFIX 0 C15 1 0.355103 0.617513 0.077458 11.00000 0.02274 0.04956 = 0.02746 0.00512 0.00451 0.00720 AFIX 43 H15 2 0.264093 0.594701 0.057361 11.00000 -1.20000 AFIX 0 C16 1 0.402172 0.681271 0.046852 11.00000 0.03800 0.05151 = 0.02378 0.01646 0.00662 0.01853 AFIX 43 H16 2 0.341485 0.701637 0.006741 11.00000 -1.20000 AFIX 0 C17 1 0.537775 0.714054 0.075742 11.00000 0.04293 0.03611 = 0.03306 0.01777 0.00942 0.00772 AFIX 43 H17 2 0.569142 0.756218 0.054809 11.00000 -1.20000 AFIX 0 C18 1 0.627888 0.684767 0.135726 11.00000 0.03279 0.02385 = 0.03012 0.00623 0.00912 0.00214 AFIX 43 H18 2 0.719293 0.707532 0.155216 11.00000 -1.20000 AFIX 0 C19 1 0.883844 0.612899 0.245343 11.00000 0.02068 0.01619 = 0.01794 0.00556 0.00631 0.00207 C20 1 0.977639 0.655290 0.297284 11.00000 0.02770 0.02157 = 0.02082 0.00027 0.00550 0.00018 AFIX 43 H20 2 0.943408 0.672036 0.335376 11.00000 -1.20000 AFIX 0 C21 1 1.121907 0.672389 0.292001 11.00000 0.02468 0.02277 = 0.03199 0.00171 0.00028 -0.00296 AFIX 43 H21 2 1.184494 0.700666 0.326544 11.00000 -1.20000 AFIX 0 C22 1 1.172955 0.647301 0.235142 11.00000 0.01974 0.02334 = 0.03824 0.00993 0.00920 0.00314 AFIX 43 H22 2 1.269437 0.659233 0.231466 11.00000 -1.20000 AFIX 0 C23 1 1.080747 0.604594 0.183916 11.00000 0.03011 0.02992 = 0.02870 0.00465 0.01525 0.00406 AFIX 43 H23 2 1.116148 0.587151 0.146379 11.00000 -1.20000 AFIX 0 C24 1 0.936613 0.587802 0.188305 11.00000 0.02613 0.02237 = 0.02142 -0.00154 0.00614 0.00026 AFIX 43 H24 2 0.874464 0.559810 0.153383 11.00000 -1.20000 AFIX 0 C25 1 0.731722 0.431392 0.227741 11.00000 0.02167 0.01705 = 0.02029 0.00040 0.00620 0.00151 AFIX 23 H25A 2 0.744518 0.388322 0.258963 11.00000 -1.20000 H25B 2 0.829060 0.443467 0.219374 11.00000 -1.20000 AFIX 0 C26 1 0.627784 0.408441 0.159084 11.00000 0.02696 0.01919 = 0.01797 -0.00194 0.00759 0.00061 AFIX 23 H26A 2 0.605842 0.452784 0.129566 11.00000 -1.20000 H26B 2 0.679358 0.372316 0.136001 11.00000 -1.20000 AFIX 0 C27 1 0.480933 0.373585 0.166778 11.00000 0.03071 0.02587 = 0.01994 -0.00325 0.00616 -0.00669 AFIX 23 H27A 2 0.420501 0.412769 0.181116 11.00000 -1.20000 H27B 2 0.502426 0.335860 0.203356 11.00000 -1.20000 AFIX 0 C28 1 0.315964 0.411232 0.034862 11.00000 0.04173 0.03770 = 0.03406 0.00208 0.00014 -0.00905 AFIX 137 H28A 2 0.254619 0.395467 -0.009001 11.00000 -1.50000 H28B 2 0.402726 0.437188 0.027407 11.00000 -1.50000 H28C 2 0.259760 0.444630 0.057449 11.00000 -1.50000 AFIX 0 C29 1 0.525211 0.856457 0.394857 11.00000 0.03600 0.02242 = 0.03016 0.00054 0.01648 0.00092 C30 1 0.543014 0.776246 0.391305 11.00000 0.02187 0.01907 = 0.02344 -0.00178 0.00790 0.00205 C31 1 0.516112 0.728352 0.441055 11.00000 0.01957 0.01951 = 0.02065 -0.00083 0.00455 0.00196 C32 1 0.465496 0.756574 0.499477 11.00000 0.02905 0.02113 = 0.01936 0.00445 0.00371 0.00627 HKLF 4 REM exp_26472_a.res in P2(1)/n REM R1 = 0.0416 for 4744 Fo > 4sig(Fo) and 0.0465 for all 5366 data REM 371 parameters refined using 0 restraints END WGHT 0.0799 0.2181 REM Highest difference peak 0.728, deepest hole -0.660, 1-sigma level 0.087 Q1 1 0.5033 0.6218 0.3130 11.00000 0.05 0.73 Q2 1 0.5380 0.6247 0.3753 11.00000 0.05 0.69 Q3 1 0.7075 0.6179 0.3092 11.00000 0.05 0.58 Q4 1 0.6143 0.6301 0.4025 11.00000 0.05 0.57 Q5 1 0.7323 0.6223 0.3714 11.00000 0.05 0.57 Q6 1 0.6625 0.6308 0.4635 11.00000 0.05 0.45 Q7 1 0.6305 0.6113 0.2892 11.00000 0.05 0.45 Q8 1 0.8006 0.6012 0.2643 11.00000 0.05 0.44 Q9 1 0.6407 0.4967 0.2876 11.00000 0.05 0.43 Q10 1 0.7207 0.7402 0.3482 11.00000 0.05 0.43 Q11 1 0.4928 0.7344 0.2918 11.00000 0.05 0.41 Q12 1 0.7155 0.4974 0.3130 11.00000 0.05 0.38 Q13 1 0.4478 0.6288 0.4100 11.00000 0.05 0.38 Q14 1 0.7336 0.4967 0.3745 11.00000 0.05 0.36 Q15 1 0.5998 0.6033 0.2155 11.00000 0.05 0.36 Q16 1 0.4997 0.6181 0.1721 11.00000 0.05 0.35 Q17 1 0.6881 0.7456 0.2943 11.00000 0.05 0.34 Q18 1 0.5863 0.7556 0.3715 11.00000 0.05 0.33 Q19 1 0.5232 0.7436 0.3520 11.00000 0.05 0.32 Q20 1 0.6660 0.6014 0.1964 11.00000 0.05 0.32 ; _shelx_res_checksum 24154 _shelx_hkl_file ; 0 0 2 1653.91 17.70 0 0 3 0.47 0.23 0 0 4 508.63 7.97 0 0 5 0.75 0.47 0 0 6 563.54 10.02 0 0 7 -0.17 0.30 0 0 8 1051.20 17.17 0 0 9 -0.12 0.38 0 0 10 1437.47 23.18 0 0 -11 -0.46 1.32 0 0 11 -0.30 0.63 0 0 -12 2698.10 50.17 0 0 -13 1.08 1.42 0 0 14 156.67 11.30 0 0 -14 163.26 12.00 0 0 -15 1.86 1.22 0 0 15 -0.18 2.00 0 0 -16 59.48 7.96 0 0 16 74.44 8.14 0 0 17 1.78 1.45 0 0 18 52.93 6.86 0 0 19 -1.50 1.47 0 0 20 259.62 13.95 0 0 21 3.24 1.62 0 0 22 213.12 9.97 0 0 22 182.28 9.84 0 0 23 2.56 1.31 0 1 -1 739.00 9.42 0 -1 -1 754.31 9.67 0 -1 -2 987.20 12.03 0 -1 2 963.14 11.39 0 1 -3 291.27 6.60 0 -1 3 300.60 5.12 0 1 3 303.10 5.39 0 -1 4 11.25 0.96 0 1 4 9.97 0.95 0 -1 5 999.96 13.76 0 1 5 993.13 14.02 0 -1 6 3.95 0.76 0 1 6 0.49 0.53 0 1 7 78.04 3.59 0 -1 7 74.31 3.39 0 1 -7 76.99 4.91 0 1 8 48.50 3.05 0 1 -8 50.07 4.30 0 -1 8 44.00 2.82 0 1 9 568.59 12.48 0 1 -9 558.11 16.36 0 -1 9 550.40 11.83 0 1 10 438.71 11.53 0 1 -10 464.45 15.79 0 -1 10 432.55 10.86 0 -1 11 13.36 1.92 0 1 11 19.17 2.40 0 1 -11 23.47 3.79 0 -1 -12 98.15 8.45 0 1 -12 94.37 7.93 0 1 -13 248.12 13.81 0 -1 -13 264.26 14.83 0 -1 14 173.88 11.99 0 1 14 167.49 11.68 0 -1 -14 173.55 12.69 0 1 -14 188.45 12.73 0 1 15 18.74 4.13 0 -1 15 18.74 4.29 0 -1 -15 10.36 3.25 0 1 -15 16.27 3.66 0 1 16 8.16 3.11 0 -1 16 6.38 2.77 0 1 -16 1.64 1.69 0 -1 -16 5.04 2.66 0 -1 17 2.39 2.13 0 1 17 6.53 2.83 0 1 18 4.75 2.93 0 -1 18 5.06 2.92 0 1 19 395.17 17.82 0 -1 19 413.21 18.87 0 -1 20 125.78 9.81 0 1 20 122.07 9.19 0 1 21 72.95 6.63 0 -1 21 69.74 6.85 0 1 22 3.68 1.51 0 -1 22 4.17 1.54 0 -1 22 4.13 1.72 0 1 23 182.67 8.19 0 -1 23 170.54 7.56 0 2 0 154.20 3.57 0 -2 -1 1306.54 17.44 0 2 -1 1296.49 15.87 0 2 -2 1256.69 16.48 0 -2 -2 1264.76 17.04 0 2 -3 787.17 12.89 0 -2 -3 798.03 12.43 0 2 4 95.39 3.38 0 -2 -4 91.14 3.65 0 2 -4 89.81 4.02 0 -2 5 243.62 5.79 0 2 5 240.53 5.95 0 2 -5 240.51 7.49 0 2 -6 7.26 1.48 0 2 6 7.81 1.08 0 -2 6 7.91 1.05 0 2 7 464.47 9.81 0 -2 7 445.30 9.47 0 2 -7 476.70 12.77 0 2 8 539.63 11.27 0 -2 8 534.83 10.93 0 2 -8 545.81 14.69 0 2 9 571.04 12.63 0 -2 9 538.39 11.94 0 2 -9 545.18 15.96 0 2 -10 291.46 12.25 0 2 10 287.26 9.18 0 2 -11 1603.44 33.80 0 2 11 1623.08 27.34 0 2 -12 35.99 4.80 0 2 -13 29.25 4.72 0 2 14 7.44 2.81 0 2 -14 14.22 3.72 0 -2 -14 9.44 3.20 0 -2 14 19.12 4.41 0 -2 -15 78.77 9.12 0 2 -15 65.74 7.83 0 2 15 59.94 6.99 0 -2 15 74.05 8.19 0 -2 -16 173.89 14.03 0 -2 16 205.16 13.76 0 2 16 193.54 12.62 0 -2 17 377.16 18.75 0 2 17 357.90 17.29 0 -2 18 4.12 2.57 0 2 18 -0.62 2.34 0 -2 19 53.78 6.92 0 2 19 37.75 5.18 0 -2 20 35.90 5.28 0 -2 21 295.77 14.57 0 2 22 206.86 9.93 0 -2 22 193.91 8.98 0 -2 22 193.22 10.77 0 2 23 42.07 3.90 0 -2 23 32.71 3.03 0 -3 0 3.49 0.96 0 -3 -1 716.34 13.10 0 3 -1 706.20 11.11 0 3 -2 157.74 4.67 0 -3 -2 160.53 5.51 0 3 -3 53.07 2.90 0 -3 -3 49.58 3.05 0 3 -4 823.84 14.83 0 -3 -4 806.66 14.42 0 -3 -5 834.12 15.22 0 3 -5 826.75 15.95 0 3 5 821.77 13.82 0 3 6 60.58 3.26 0 3 -6 61.45 4.16 0 3 -7 74.47 4.91 0 3 7 71.61 3.76 0 -3 7 65.87 3.92 0 -3 8 296.08 8.53 0 3 8 317.40 8.76 0 3 9 289.09 8.81 0 3 -9 300.39 11.64 0 3 10 74.07 4.64 0 3 -10 75.09 6.09 0 3 11 102.87 5.89 0 3 -11 92.24 7.22 0 3 12 494.21 14.35 0 3 -12 497.30 18.55 0 3 -13 6.75 2.37 0 -3 13 9.94 3.42 0 -3 14 228.86 14.18 0 3 -14 208.72 13.41 0 3 -15 348.18 18.20 0 -3 15 383.32 18.76 0 -3 -15 403.51 21.21 0 -3 16 12.60 3.70 0 -3 -16 10.84 3.91 0 -3 17 34.50 5.87 0 -3 18 60.31 7.49 0 -3 19 30.35 5.31 0 -3 20 228.84 13.41 0 -3 21 62.48 6.66 0 3 22 0.93 0.87 0 -3 22 -0.24 1.00 0 -3 22 0.45 1.29 0 3 23 78.60 5.24 0 -3 23 78.93 6.07 0 -4 0 6979.01 78.90 0 -4 1 456.53 11.70 0 4 -1 461.04 9.33 0 -4 -1 483.06 11.66 0 -4 -2 110.48 5.19 0 4 -2 107.56 4.23 0 4 -3 259.02 7.21 0 -4 -3 266.24 8.23 0 4 -4 11.78 1.63 0 -4 -4 11.46 1.74 0 -4 -5 447.64 11.47 0 4 -5 457.43 11.53 0 -4 6 8.32 1.73 0 4 -6 11.09 1.84 0 4 6 9.09 1.45 0 -4 -6 6.82 1.35 0 4 -7 607.63 15.42 0 4 7 592.33 12.76 0 -4 7 569.79 14.24 0 4 8 -0.10 0.45 0 4 -8 0.88 1.18 0 -4 8 0.86 0.70 0 4 9 2.75 1.02 0 4 -9 1.58 1.17 0 4 -10 585.99 18.04 0 4 10 533.59 13.75 0 4 11 143.97 7.28 0 4 -11 148.92 9.39 0 4 -12 271.38 13.64 0 4 12 256.30 10.41 0 -4 13 401.81 18.49 0 4 -13 423.72 18.06 0 -4 14 54.46 7.07 0 4 -14 42.75 5.86 0 -4 15 1.21 2.00 0 -4 -15 6.79 2.83 0 -4 16 9.35 3.21 0 -4 17 221.61 14.49 0 -4 18 43.52 6.28 0 -4 19 57.26 7.33 0 -4 20 37.81 5.48 0 -4 21 5.40 1.77 0 -4 22 239.76 11.98 0 4 22 245.96 10.46 0 4 23 9.77 1.89 0 -4 23 9.23 2.03 0 -5 0 0.66 1.06 0 -5 -1 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10.45 -8 8 -5 3.10 1.21 -8 8 -5 1.89 1.07 -8 8 -4 -0.74 1.05 -8 8 -3 64.74 6.16 -8 8 -2 32.98 4.68 -8 8 -1 41.62 5.33 -8 8 0 90.32 7.99 -8 8 1 62.71 6.69 -8 8 2 120.49 9.27 -8 8 3 203.01 10.04 -8 8 3 217.97 12.61 -8 8 4 300.71 12.36 -8 8 4 304.10 14.92 -8 8 5 4.51 1.54 -8 8 5 5.29 2.16 -8 8 6 295.02 12.07 -8 8 6 285.79 14.35 -8 8 7 4.10 1.59 -8 8 7 4.73 1.42 -8 8 7 4.41 2.13 -8 8 8 2.97 1.22 -8 8 8 4.10 1.27 -8 8 8 2.63 1.93 -8 8 9 0.67 0.88 -8 8 9 -0.19 0.60 -8 8 9 1.04 1.33 -8 8 10 58.07 6.10 -8 8 10 48.40 4.02 -8 8 11 1.49 0.82 -8 8 11 2.15 1.30 -8 8 12 390.71 15.42 -8 8 12 413.23 11.95 -8 8 13 1.93 1.00 -8 8 13 1.56 0.91 -8 8 14 3.93 1.22 -8 8 14 3.49 1.56 -8 8 15 39.81 4.10 -8 8 15 43.77 3.49 -8 8 16 72.51 5.02 -8 8 16 107.23 5.20 -8 8 17 74.48 4.06 -8 8 18 30.84 2.35 8 -9 9 43.16 4.35 8 -9 8 19.78 3.15 -8 9 -8 17.21 1.84 8 -9 7 75.35 6.37 -8 9 -7 72.66 4.20 -8 9 -6 65.97 5.13 -8 9 -6 66.69 4.36 -8 9 -5 22.91 3.30 -8 9 -5 24.00 2.75 -8 9 -4 50.57 5.13 -8 9 -3 152.91 9.33 -8 9 -2 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-4 9 0.57 0.78 9 -4 8 7.02 1.95 -9 4 -8 7.60 1.30 -9 4 -7 52.36 3.59 -9 4 -6 24.60 2.64 -9 4 -5 -0.55 0.80 -9 4 -4 7.38 1.55 -9 4 -3 7.07 1.67 -9 -4 -2 3.65 1.46 -9 4 -2 4.76 1.14 -9 4 -1 35.10 4.47 -9 -4 -1 35.66 3.74 -9 4 -1 37.79 4.01 -9 4 0 117.82 8.43 -9 -4 0 109.10 6.43 -9 4 0 122.06 7.32 -9 4 1 -0.40 0.81 -9 4 1 -0.68 1.22 -9 -4 1 1.00 0.78 -9 4 2 6.55 1.77 -9 4 2 4.68 2.09 -9 -4 2 7.37 1.76 -9 4 3 1.54 1.32 -9 4 4 92.94 7.99 -9 4 5 19.14 3.82 -9 4 6 89.21 7.84 -9 4 7 16.20 3.51 -9 -4 8 15.03 3.26 -9 4 8 12.08 3.12 -9 -4 9 125.38 8.73 -9 4 9 133.87 9.42 -9 4 9 142.54 7.02 -9 -4 10 87.75 7.37 -9 4 10 88.49 7.62 -9 4 10 97.41 5.77 -9 -4 11 158.55 9.85 -9 4 11 165.79 10.34 -9 4 11 177.58 7.77 -9 -4 12 134.14 8.96 -9 4 12 133.20 9.04 -9 4 12 129.06 6.54 -9 -4 13 88.37 7.25 -9 4 13 89.09 7.16 -9 4 13 93.40 5.39 -9 4 14 2.03 0.88 -9 4 14 0.68 0.84 -9 4 15 0.94 0.51 -9 4 15 1.24 1.18 -9 4 16 1.90 1.00 -9 4 16 -0.69 0.46 -9 4 17 89.98 5.64 -9 4 17 97.95 4.55 -9 4 18 45.62 2.79 9 -5 9 89.83 5.66 9 -5 8 32.91 3.74 -9 5 -8 30.75 2.39 -9 5 -7 10.17 1.55 -9 5 -6 43.50 3.36 -9 5 -5 86.31 5.06 -9 5 -4 2.63 0.98 -9 5 -3 3.61 1.06 -9 5 -2 103.90 7.34 -9 5 -2 104.28 6.32 -9 5 -1 2.04 1.05 -9 5 -1 1.11 0.93 -9 5 0 2.13 1.04 -9 5 0 0.87 1.22 -9 5 1 0.19 1.42 -9 5 2 34.00 4.70 -9 5 3 11.02 3.01 -9 5 4 1.25 1.27 -9 5 5 1.56 1.15 -9 5 6 29.87 4.54 -9 5 7 -0.08 1.55 -9 5 8 16.25 3.41 -9 -5 9 91.45 7.13 -9 5 9 96.23 7.84 -9 -5 10 1.86 1.51 -9 5 10 2.75 1.20 -9 5 10 -0.47 1.15 -9 -5 11 1.85 1.47 -9 5 11 2.25 0.91 -9 5 11 1.75 1.31 -9 5 12 7.39 1.64 -9 5 12 4.50 1.82 -9 5 13 0.88 0.57 -9 5 13 2.42 1.43 -9 5 14 25.03 3.61 -9 5 14 22.54 2.51 -9 5 15 144.72 8.12 -9 5 15 145.94 6.17 -9 5 16 58.92 4.79 -9 5 16 65.04 3.86 -9 5 17 41.70 3.57 -9 5 17 45.84 3.01 -9 5 18 17.62 1.67 9 -6 8 104.42 6.28 -9 6 -8 93.07 3.96 9 -6 7 50.45 4.66 -9 6 -7 54.28 3.35 -9 6 -6 47.09 3.37 -9 6 -5 4.90 1.22 -9 6 -4 39.48 3.47 -9 6 -3 1.86 1.11 -9 6 -3 0.22 0.74 -9 6 -2 2.81 1.17 -9 6 -2 3.38 1.57 -9 6 -1 4.15 1.42 -9 6 -1 3.25 1.72 -9 6 0 4.52 1.79 -9 6 1 260.98 12.89 -9 6 2 2.57 1.97 -9 6 3 107.48 8.39 -9 6 4 95.08 8.00 -9 6 5 2.93 1.55 -9 6 6 10.22 2.86 -9 6 7 5.50 2.05 -9 6 8 48.76 5.49 -9 6 9 9.94 2.40 -9 6 10 3.51 1.14 -9 6 10 2.49 1.64 -9 6 11 82.06 6.83 -9 6 11 79.14 4.89 -9 6 12 34.07 4.38 -9 6 12 36.04 3.25 -9 6 13 11.84 1.83 -9 6 13 10.53 2.27 -9 6 14 118.73 7.43 -9 6 14 118.54 5.60 -9 6 15 58.96 4.90 -9 6 15 65.02 3.93 -9 6 16 2.28 1.08 -9 6 16 2.22 0.77 -9 6 17 24.01 2.06 9 -7 7 51.65 4.48 -9 7 -7 50.04 3.01 -9 7 -6 24.25 2.29 -9 7 -5 0.16 0.53 -9 7 -4 69.46 4.98 -9 7 -4 86.09 4.90 -9 7 -3 0.88 0.94 -9 7 -3 0.38 0.75 -9 7 -2 116.29 7.55 -9 7 -2 121.97 6.41 -9 7 -1 2.13 1.11 -9 7 -1 2.91 1.45 -9 7 0 8.29 2.32 -9 7 1 121.78 8.56 -9 7 2 290.80 13.66 -9 7 3 2.30 1.43 -9 7 4 2.88 1.73 -9 7 5 236.56 12.42 -9 7 6 67.94 6.56 -9 7 7 14.47 3.13 -9 7 8 0.45 1.50 -9 7 9 82.69 6.98 -9 7 10 66.12 6.10 -9 7 11 48.67 5.15 -9 7 11 40.68 3.38 -9 7 12 73.87 6.12 -9 7 12 78.45 4.59 -9 7 13 122.46 7.59 -9 7 13 117.35 5.50 -9 7 14 25.60 3.25 -9 7 14 22.70 2.32 -9 7 15 5.04 1.10 -9 7 15 3.83 1.28 -9 7 16 93.28 4.24 9 -8 6 27.97 3.42 -9 8 -6 26.56 2.24 -9 8 -5 0.36 0.40 -9 8 -4 3.16 1.20 -9 8 -4 4.11 1.03 -9 8 -3 95.92 6.23 -9 8 -3 103.76 5.44 -9 8 -2 3.16 1.13 -9 8 -2 1.59 1.09 -9 8 -1 99.33 7.09 -9 8 -1 97.44 5.61 -9 8 0 124.12 8.22 -9 8 1 -0.10 1.31 -9 8 2 57.11 5.88 -9 8 3 427.63 16.52 -9 8 4 25.11 4.11 -9 8 5 69.04 6.48 -9 8 6 42.43 5.09 -9 8 7 36.04 4.65 -9 8 8 17.28 3.19 -9 8 9 46.16 5.00 -9 8 10 28.36 3.96 -9 8 11 194.93 9.88 -9 8 12 165.62 8.75 -9 8 13 15.63 2.47 -9 8 14 44.35 4.01 -9 8 15 118.46 5.85 9 -9 5 4.02 1.47 -9 9 -5 3.13 0.84 -9 9 -4 104.54 5.61 9 -9 4 116.56 6.77 -9 9 -4 121.47 5.23 -9 9 -3 7.89 1.76 -9 9 -3 5.52 1.25 -9 9 -2 0.49 0.57 -9 9 -2 1.14 0.73 -9 9 -1 22.04 3.26 -9 9 -1 21.94 2.53 -9 9 0 25.07 3.56 -9 9 1 123.36 8.09 -9 9 2 142.88 8.95 -9 9 3 10.40 2.68 -9 9 4 38.46 4.77 -9 9 5 155.27 9.48 -9 9 6 350.61 14.32 -9 9 7 1.20 1.31 -9 9 8 264.42 11.99 -9 9 9 -1.74 1.47 -9 9 10 6.31 1.71 -9 9 11 37.75 4.07 -9 9 12 168.39 8.30 -9 9 13 70.25 5.00 -9 9 14 26.24 2.69 -9 10 -4 114.44 5.41 -9 10 -4 139.43 5.16 -9 10 -3 38.34 3.52 9 -10 3 28.33 3.14 -9 10 -3 36.70 2.79 -9 10 -2 69.83 5.07 -9 10 -2 71.69 4.15 -9 10 -1 12.75 1.76 -9 10 -1 11.18 2.26 -9 10 0 19.67 2.94 -9 10 1 5.01 1.92 -9 10 2 8.01 2.19 -9 10 3 79.84 6.40 -9 10 4 22.60 3.58 -9 10 5 160.70 9.21 -9 10 6 0.68 1.21 -9 10 7 84.51 6.49 -9 10 8 91.19 6.67 -9 10 9 6.08 1.76 -9 10 10 122.18 7.17 -9 10 11 -0.04 0.72 -9 10 12 44.41 3.87 -9 11 -3 1.43 0.79 -9 11 -3 2.46 0.65 -9 11 -2 39.61 3.51 -9 11 -2 38.62 2.78 -9 11 -1 2.49 0.76 -9 11 -1 1.44 0.65 -9 11 0 -0.04 0.72 -9 11 1 23.18 3.19 -9 11 2 23.84 3.23 -9 11 3 -0.51 0.86 -9 11 4 12.80 2.53 -9 11 5 16.38 2.81 -9 11 6 10.04 2.22 -9 11 7 0.07 0.87 -9 11 8 16.52 2.57 -9 11 9 -0.96 0.93 -9 11 10 5.97 1.57 -9 11 11 0.09 0.64 -9 12 -1 2.45 0.64 -9 12 -1 2.65 1.09 -9 12 0 2.17 0.63 -9 12 0 2.86 1.06 -9 12 1 11.27 1.91 -9 12 2 0.94 0.68 -9 12 3 -0.03 0.66 -9 12 4 -0.84 0.83 -9 12 5 115.04 6.74 -9 12 6 4.55 1.48 -9 12 7 93.84 5.89 -9 12 8 5.39 1.41 -9 12 9 19.09 2.38 -9 13 1 30.85 2.92 -9 13 1 26.40 2.05 -9 13 2 2.18 0.96 -9 13 3 5.64 1.39 -9 13 4 24.71 2.79 -9 13 5 37.98 3.42 -9 13 6 13.21 1.96 -10 0 -4 20.77 2.25 -10 0 -3 0.34 0.58 -10 0 -2 3.09 1.11 -10 0 -1 -0.27 0.71 -10 0 0 10.25 1.82 -10 0 1 -0.20 0.66 -10 0 2 944.99 19.49 -10 0 3 0.66 0.88 -10 0 5 0.76 1.31 -10 0 6 8.78 2.45 -10 0 7 -1.06 0.94 -10 0 8 11.74 2.50 -10 0 9 0.47 1.37 -10 0 10 129.25 8.39 -10 0 11 -0.17 0.97 -10 0 12 52.24 5.09 -10 0 13 0.50 1.11 -10 0 14 585.82 16.52 -10 0 15 1.62 0.93 -10 1 -5 49.09 3.22 -10 1 -4 12.49 1.76 -10 -1 -3 1.57 0.78 -10 1 -3 1.12 0.58 -10 -1 -2 1.40 0.85 -10 1 -2 0.07 0.49 -10 -1 -1 3.62 1.02 -10 1 -1 2.56 0.97 -10 -1 0 58.64 4.28 -10 1 0 62.19 4.53 -10 -1 1 41.87 3.65 -10 1 1 45.33 3.86 -10 -1 2 57.30 4.16 -10 1 2 58.27 4.42 -10 1 3 64.71 4.55 -10 1 4 331.65 13.11 -10 1 4 304.13 9.96 -10 1 5 117.24 7.92 -10 -1 6 2.67 1.62 -10 1 6 -0.67 1.32 -10 -1 7 193.51 10.16 -10 1 7 180.65 10.16 -10 -1 8 1.54 1.07 -10 1 8 1.03 1.10 -10 -1 9 8.68 2.38 -10 1 9 8.88 2.40 -10 -1 10 33.36 4.22 -10 1 10 33.89 4.39 -10 -1 11 31.93 4.08 -10 1 11 37.56 4.49 -10 -1 12 16.72 2.91 -10 1 12 19.00 3.17 -10 -1 13 40.97 4.37 -10 1 13 39.39 4.30 -10 -1 14 47.33 4.50 -10 1 14 48.99 4.55 -10 1 15 29.17 3.27 10 -2 6 52.16 4.33 -10 2 -5 39.68 2.82 -10 2 -4 0.64 0.51 -10 2 -3 0.10 0.45 -10 2 -2 3.47 1.01 -10 -2 -1 20.87 2.45 -10 2 -1 22.24 2.64 -10 -2 0 10.76 1.80 -10 2 0 14.45 2.17 -10 -2 1 66.12 4.43 -10 2 1 68.97 4.78 -10 -2 2 1.31 0.73 -10 2 2 1.16 0.78 -10 2 3 200.92 9.98 -10 2 3 208.34 8.34 -10 2 4 44.14 4.83 -10 2 4 43.47 3.64 -10 2 5 28.39 3.87 -10 2 6 68.97 6.23 -10 -2 7 1.58 0.86 -10 2 7 3.69 1.79 -10 -2 8 7.40 4.73 -10 2 8 -0.70 1.35 -10 -2 9 3.65 1.83 -10 2 9 2.89 1.31 -10 -2 10 5.65 1.68 -10 2 10 3.63 1.45 -10 -2 11 121.23 7.75 -10 2 11 130.50 8.33 -10 -2 12 0.97 1.11 -10 2 12 0.50 0.86 -10 -2 13 538.79 16.14 -10 2 13 550.71 16.51 -10 2 14 17.74 2.72 -10 2 15 54.04 4.36 -10 3 -6 107.20 4.14 -10 3 -5 6.29 1.11 -10 3 -4 52.23 3.42 -10 3 -3 32.03 2.87 -10 3 -2 0.87 0.79 -10 3 -1 8.55 1.66 -10 3 0 7.70 1.64 -10 3 1 34.91 3.36 -10 3 2 1.86 1.06 -10 3 2 1.61 0.81 -10 3 3 33.37 3.99 -10 3 3 34.75 3.37 -10 3 4 31.01 4.07 -10 3 4 28.72 3.02 -10 3 5 1.18 1.03 -10 3 5 -0.03 0.71 -10 3 6 3.82 1.60 -10 3 7 4.92 1.96 -10 3 8 13.29 2.71 -10 -3 9 13.42 2.47 -10 3 9 11.70 2.36 -10 -3 10 49.66 4.82 -10 3 10 56.16 5.49 -10 -3 11 39.49 4.29 -10 3 11 37.19 4.32 -10 3 12 2.93 1.29 -10 3 13 47.69 4.55 -10 3 14 85.27 5.75 -10 3 15 4.52 1.23 -10 4 -5 35.70 2.53 -10 4 -4 20.09 2.02 -10 4 -3 -0.32 0.46 -10 4 -2 12.73 1.87 -10 4 -1 2.97 0.95 -10 4 0 3.37 1.11 -10 4 1 31.76 3.65 -10 4 1 33.94 3.28 -10 4 2 121.35 7.48 -10 4 2 125.29 6.38 -10 4 3 71.48 5.94 -10 4 3 58.91 4.33 -10 4 4 -1.04 1.20 -10 4 4 0.16 0.52 -10 4 5 5.35 1.86 -10 4 5 5.21 1.27 -10 4 6 7.91 2.22 -10 4 7 6.60 2.08 -10 4 8 158.47 9.23 -10 4 9 18.44 3.02 -10 4 10 2.97 1.54 -10 4 11 17.97 2.96 -10 4 12 81.85 6.09 -10 4 13 75.43 5.54 -10 4 14 93.06 5.81 -10 4 15 42.67 3.62 -10 5 -5 15.52 1.56 10 -5 5 14.11 2.13 -10 5 -4 0.07 0.34 -10 5 -3 2.99 0.92 -10 5 -2 29.77 2.70 -10 5 -1 12.37 1.78 -10 5 0 26.85 3.07 -10 5 0 38.53 3.33 -10 5 1 11.05 2.23 -10 5 1 8.56 1.58 -10 5 2 6.55 1.94 -10 5 2 6.05 1.40 -10 5 3 100.09 6.95 -10 5 3 101.84 5.60 -10 5 4 33.22 4.07 -10 5 4 33.09 3.12 -10 5 5 0.07 1.22 -10 5 5 -0.52 0.75 -10 5 6 28.69 3.84 -10 5 6 21.30 2.36 -10 5 7 53.29 5.29 -10 5 8 -0.55 0.82 -10 5 9 -0.56 0.82 -10 5 10 40.49 4.44 -10 5 11 6.39 1.73 -10 5 12 0.29 0.88 -10 5 13 41.97 3.98 -10 5 14 91.42 5.51 -10 6 -4 24.81 2.04 -10 6 -3 1.48 0.70 -10 6 -2 190.01 6.66 -10 6 -1 24.72 2.45 -10 6 0 39.13 3.65 -10 6 0 55.58 3.82 -10 6 1 53.49 4.58 -10 6 1 50.72 3.75 -10 6 2 1.85 1.36 -10 6 2 0.62 1.61 -10 6 3 140.91 8.06 -10 6 3 139.72 6.42 -10 6 4 3.72 1.46 -10 6 4 3.74 1.08 -10 6 5 12.41 2.60 -10 6 5 11.16 1.74 -10 6 6 1.31 1.14 -10 6 6 0.64 0.47 -10 6 7 -1.67 1.42 -10 6 8 -0.66 1.36 -10 6 9 2.44 1.15 -10 6 10 86.13 6.22 -10 6 11 10.73 2.23 -10 6 12 65.68 5.05 -10 6 13 97.36 5.79 -10 6 14 0.13 0.78 -10 7 -3 8.42 1.20 -10 7 -2 28.03 2.32 -10 7 -1 4.96 1.06 -10 7 0 1.63 0.85 -10 7 0 0.63 0.51 -10 7 1 13.61 2.31 -10 7 1 11.38 1.72 -10 7 2 8.15 2.14 -10 7 2 6.94 1.34 -10 7 3 15.63 2.67 -10 7 3 15.98 2.10 -10 7 4 68.22 5.51 -10 7 4 61.79 4.03 -10 7 5 107.85 7.00 -10 7 5 91.97 4.83 -10 7 6 86.30 6.30 -10 7 6 64.69 3.90 -10 7 7 4.96 1.78 -10 7 8 1.05 0.94 -10 7 9 3.44 1.09 -10 7 10 43.19 4.25 -10 7 11 44.03 4.11 -10 7 12 -0.32 0.60 -10 7 13 19.62 2.41 -10 8 -2 24.24 1.99 -10 8 -1 11.58 1.48 -10 8 0 3.72 1.17 -10 8 0 3.29 0.87 -10 8 1 68.81 4.78 -10 8 1 69.22 3.91 -10 8 2 292.15 10.54 -10 8 2 282.95 8.40 -10 8 3 69.55 5.23 -10 8 3 65.39 3.95 -10 8 4 87.07 6.01 -10 8 4 81.26 4.37 -10 8 5 36.63 3.97 -10 8 5 37.43 2.89 -10 8 6 107.20 6.72 -10 8 6 79.01 4.09 -10 8 7 2.92 1.50 -10 8 8 171.13 8.37 -10 8 9 6.43 1.73 -10 8 10 73.96 5.19 -10 8 11 2.77 1.12 -10 8 12 89.10 5.14 -10 9 -1 43.11 2.55 -10 9 0 20.68 1.92 -10 9 1 5.04 1.30 -10 9 1 5.67 1.05 -10 9 2 2.48 1.00 -10 9 2 1.32 0.57 -10 9 3 85.72 5.42 -10 9 3 77.82 3.99 -10 9 4 86.77 5.61 -10 9 4 79.97 4.03 -10 9 5 39.50 3.86 -10 9 5 31.22 2.46 -10 9 6 -0.51 0.75 -10 9 6 0.83 0.51 -10 9 7 28.32 3.27 -10 9 8 2.44 1.18 -10 9 9 0.27 0.88 -10 9 10 105.78 5.78 -10 10 2 5.23 1.20 -10 10 2 5.07 0.88 -10 10 3 25.97 2.76 -10 10 3 23.57 1.98 -10 10 4 144.83 6.68 -10 10 4 112.02 4.38 -10 10 5 191.68 7.88 -10 10 6 68.90 4.67 -10 10 7 33.23 3.23 -10 10 8 2.37 0.90 -11 1 9 59.28 4.20 -11 2 7 -0.20 0.80 -11 2 8 2.53 0.91 -11 2 9 21.15 2.55 -11 2 10 13.96 2.07 -11 3 7 6.28 1.42 -11 3 8 4.14 1.05 -11 3 9 23.35 2.71 -11 3 10 2.68 1.04 -11 4 7 121.44 6.04 -11 4 8 32.59 3.10 -11 4 9 16.97 2.28 0 0 0 0.00 0.00 TITL exp_26472 in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 9.184412 17.665269 19.793478 90.0000 103.4270 90.0000 ZERR 27.00 0.000127 0.000226 0.000307 0.0000 0.0014 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O UNIT 297.00 270.00 27.00 27.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 37948 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.61681(4) 0.62127(2) 0.34120(2) 0.01603(13) Uani 1 1 d . . . . . S1 S 0.54382(7) 0.63154(3) 0.43629(3) 0.02252(16) Uani 1 1 d . . . . . S2 S 0.60314(7) 0.74056(3) 0.32011(3) 0.02315(16) Uani 1 1 d . . . . . S3 S 0.37352(8) 0.32974(4) 0.08858(3) 0.03211(18) Uani 1 1 d . . . . . P1 P 0.63174(6) 0.49932(3) 0.34061(3) 0.01544(15) Uani 1 1 d . . . . . P2 P 0.69473(6) 0.59120(3) 0.25051(3) 0.01567(15) Uani 1 1 d . . . . . N1 N 0.6799(2) 0.49671(10) 0.26275(10) 0.0169(4) Uani 1 1 d . . . . . N2 N 0.4254(3) 0.77728(14) 0.54702(11) 0.0343(5) Uani 1 1 d . . . . . N3 N 0.5160(3) 0.92113(14) 0.39684(15) 0.0438(7) Uani 1 1 d . . . . . C1 C 0.4645(2) 0.44360(13) 0.33316(12) 0.0176(5) Uani 1 1 d . . . . . C2 C 0.4653(3) 0.36679(13) 0.34961(12) 0.0211(5) Uani 1 1 d . . . . . H2 H 0.5551 0.3425 0.3692 0.025 Uiso 1 1 calc R U . . . C3 C 0.3323(3) 0.32682(14) 0.33674(13) 0.0260(5) Uani 1 1 d . . . . . H3 H 0.3325 0.2761 0.3493 0.031 Uiso 1 1 calc R U . . . C4 C 0.1989(3) 0.36166(17) 0.30533(14) 0.0314(6) Uani 1 1 d . . . . . H4 H 0.1103 0.3340 0.2955 0.038 Uiso 1 1 calc R U . . . C5 C 0.1974(3) 0.43769(17) 0.28851(15) 0.0331(6) Uani 1 1 d . . . . . H5 H 0.1079 0.4611 0.2671 0.040 Uiso 1 1 calc R U . . . C6 C 0.3294(3) 0.47909(15) 0.30352(13) 0.0264(5) Uani 1 1 d . . . . . H6 H 0.3276 0.5306 0.2938 0.032 Uiso 1 1 calc R U . . . C7 C 0.7757(2) 0.45320(13) 0.40486(12) 0.0178(5) Uani 1 1 d . . . . . C8 C 0.9217(3) 0.44753(14) 0.39651(13) 0.0225(5) Uani 1 1 d . . . . . H8 H 0.9445 0.4643 0.3556 0.027 Uiso 1 1 calc R U . . . C9 C 1.0332(3) 0.41701(14) 0.44872(14) 0.0271(6) Uani 1 1 d . . . . . H9 H 1.1304 0.4132 0.4427 0.033 Uiso 1 1 calc R U . . . C10 C 1.0005(3) 0.39212(15) 0.50979(13) 0.0274(5) Uani 1 1 d . . . . . H10 H 1.0754 0.3712 0.5446 0.033 Uiso 1 1 calc R U . . . C11 C 0.8552(3) 0.39840(15) 0.51905(13) 0.0288(6) Uani 1 1 d . . . . . H11 H 0.8335 0.3820 0.5603 0.035 Uiso 1 1 calc R U . . . C12 C 0.7431(3) 0.42890(14) 0.46710(13) 0.0228(5) Uani 1 1 d . . . . . H12 H 0.6463 0.4332 0.4735 0.027 Uiso 1 1 calc R U . . . C13 C 0.5821(3) 0.62075(13) 0.16744(12) 0.0194(5) Uani 1 1 d . . . . . C14 C 0.4449(3) 0.58826(15) 0.13812(13) 0.0246(5) Uani 1 1 d . . . . . H14 H 0.4125 0.5465 0.1592 0.030 Uiso 1 1 calc R U . . . C15 C 0.3551(3) 0.61751(18) 0.07746(14) 0.0335(6) Uani 1 1 d . . . . . H15 H 0.2641 0.5947 0.0574 0.040 Uiso 1 1 calc R U . . . C16 C 0.4022(3) 0.68127(18) 0.04685(15) 0.0379(7) Uani 1 1 d . . . . . H16 H 0.3415 0.7016 0.0067 0.045 Uiso 1 1 calc R U . . . C17 C 0.5378(3) 0.71405(17) 0.07574(15) 0.0373(7) Uani 1 1 d . . . . . H17 H 0.5691 0.7562 0.0548 0.045 Uiso 1 1 calc R U . . . C18 C 0.6279(3) 0.68477(14) 0.13573(14) 0.0286(6) Uani 1 1 d . . . . . H18 H 0.7193 0.7075 0.1552 0.034 Uiso 1 1 calc R U . . . C19 C 0.8838(3) 0.61290(13) 0.24534(12) 0.0180(5) Uani 1 1 d . . . . . C20 C 0.9776(3) 0.65529(14) 0.29728(13) 0.0234(5) Uani 1 1 d . . . . . H20 H 0.9434 0.6720 0.3354 0.028 Uiso 1 1 calc R U . . . C21 C 1.1219(3) 0.67239(14) 0.29200(14) 0.0275(6) Uani 1 1 d . . . . . H21 H 1.1845 0.7007 0.3265 0.033 Uiso 1 1 calc R U . . . C22 C 1.1730(3) 0.64730(14) 0.23514(14) 0.0267(6) Uani 1 1 d . . . . . H22 H 1.2694 0.6592 0.2315 0.032 Uiso 1 1 calc R U . . . C23 C 1.0807(3) 0.60459(16) 0.18392(14) 0.0282(6) Uani 1 1 d . . . . . H23 H 1.1161 0.5872 0.1464 0.034 Uiso 1 1 calc R U . . . C24 C 0.9366(3) 0.58780(14) 0.18831(13) 0.0232(5) Uani 1 1 d . . . . . H24 H 0.8745 0.5598 0.1534 0.028 Uiso 1 1 calc R U . . . C25 C 0.7317(3) 0.43139(13) 0.22774(12) 0.0195(5) Uani 1 1 d . . . . . H25A H 0.7445 0.3883 0.2590 0.023 Uiso 1 1 calc R U . . . H25B H 0.8291 0.4435 0.2194 0.023 Uiso 1 1 calc R U . . . C26 C 0.6278(3) 0.40844(13) 0.15908(12) 0.0210(5) Uani 1 1 d . . . . . H26A H 0.6058 0.4528 0.1296 0.025 Uiso 1 1 calc R U . . . H26B H 0.6794 0.3723 0.1360 0.025 Uiso 1 1 calc R U . . . C27 C 0.4809(3) 0.37359(14) 0.16678(13) 0.0255(5) Uani 1 1 d . . . . . H27A H 0.4205 0.4128 0.1811 0.031 Uiso 1 1 calc R U . . . H27B H 0.5024 0.3359 0.2034 0.031 Uiso 1 1 calc R U . . . C28 C 0.3160(3) 0.41123(17) 0.03486(16) 0.0392(7) Uani 1 1 d . . . . . H28A H 0.2546 0.3955 -0.0090 0.059 Uiso 1 1 calc R U . . . H28B H 0.4027 0.4372 0.0274 0.059 Uiso 1 1 calc R U . . . H28C H 0.2598 0.4446 0.0574 0.059 Uiso 1 1 calc R U . . . C29 C 0.5252(3) 0.85646(15) 0.39486(14) 0.0281(6) Uani 1 1 d . . . . . C30 C 0.5430(3) 0.77625(14) 0.39131(13) 0.0210(5) Uani 1 1 d . . . . . C31 C 0.5161(2) 0.72835(13) 0.44106(12) 0.0199(5) Uani 1 1 d . . . . . C32 C 0.4655(3) 0.75657(14) 0.49948(13) 0.0235(5) Uani 1 1 d . . . . . 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 0.0206(2) 0.0133(2) 0.0157(2) 0.00122(15) 0.00727(17) 0.00092(14) S1 0.0346(3) 0.0173(3) 0.0195(3) 0.0034(2) 0.0141(3) 0.0039(2) S2 0.0350(3) 0.0145(3) 0.0247(3) 0.0033(2) 0.0165(3) 0.0022(2) S3 0.0408(4) 0.0299(3) 0.0226(3) -0.0037(3) 0.0013(3) -0.0133(3) P1 0.0183(3) 0.0139(3) 0.0146(3) 0.0015(2) 0.0047(2) 0.0002(2) P2 0.0187(3) 0.0147(3) 0.0145(3) 0.0019(2) 0.0057(2) 0.0009(2) N1 0.0210(9) 0.0147(9) 0.0155(10) 0.0019(8) 0.0049(8) 0.0019(7) N2 0.0470(14) 0.0341(13) 0.0226(12) 0.0004(10) 0.0100(11) 0.0142(11) N3 0.0661(17) 0.0207(12) 0.0547(17) -0.0005(11) 0.0346(15) 0.0020(11) C1 0.0198(11) 0.0204(11) 0.0136(11) 0.0009(9) 0.0061(9) -0.0001(9) C2 0.0241(12) 0.0189(11) 0.0192(12) 0.0006(10) 0.0026(10) -0.0012(9) C3 0.0328(13) 0.0211(12) 0.0230(13) -0.0006(10) 0.0040(11) -0.0054(10) C4 0.0242(13) 0.0385(15) 0.0309(15) -0.0032(12) 0.0052(11) -0.0121(11) C5 0.0177(12) 0.0419(16) 0.0379(16) 0.0085(13) 0.0032(11) 0.0025(11) C6 0.0229(12) 0.0250(13) 0.0321(15) 0.0082(11) 0.0078(11) 0.0026(10) C7 0.0215(11) 0.0133(10) 0.0170(12) -0.0003(9) 0.0010(9) -0.0011(9) C8 0.0252(12) 0.0211(12) 0.0209(13) -0.0005(10) 0.0046(10) -0.0013(9) C9 0.0237(12) 0.0235(13) 0.0305(15) -0.0081(11) -0.0011(10) 0.0032(10) C10 0.0312(13) 0.0221(12) 0.0217(13) 0.0013(11) -0.0086(11) 0.0025(10) C11 0.0378(14) 0.0274(13) 0.0180(13) 0.0034(11) -0.0001(11) -0.0057(11) C12 0.0242(12) 0.0249(12) 0.0181(12) -0.0005(10) 0.0026(10) -0.0053(10) C13 0.0231(12) 0.0199(12) 0.0169(12) 0.0032(9) 0.0084(10) 0.0060(9) C14 0.0242(12) 0.0289(14) 0.0216(13) 0.0052(11) 0.0074(10) 0.0036(10) C15 0.0227(13) 0.0496(18) 0.0275(15) 0.0051(13) 0.0045(11) 0.0072(11) C16 0.0380(15) 0.0515(19) 0.0238(14) 0.0165(13) 0.0066(12) 0.0185(13) C17 0.0429(16) 0.0361(16) 0.0331(16) 0.0178(13) 0.0094(13) 0.0077(13) C18 0.0328(13) 0.0239(13) 0.0301(14) 0.0062(11) 0.0091(11) 0.0021(10) C19 0.0207(11) 0.0162(11) 0.0179(12) 0.0056(9) 0.0063(9) 0.0021(9) C20 0.0277(12) 0.0216(12) 0.0208(13) 0.0003(10) 0.0055(10) 0.0002(10) C21 0.0247(12) 0.0228(12) 0.0320(15) 0.0017(11) 0.0003(11) -0.0030(10) C22 0.0197(11) 0.0233(12) 0.0382(15) 0.0099(11) 0.0092(11) 0.0031(10) C23 0.0301(13) 0.0299(13) 0.0287(14) 0.0046(11) 0.0152(11) 0.0041(11) C24 0.0261(12) 0.0224(12) 0.0214(13) -0.0015(10) 0.0061(10) 0.0003(10) C25 0.0217(11) 0.0170(11) 0.0203(12) 0.0004(9) 0.0062(10) 0.0015(9) C26 0.0270(12) 0.0192(12) 0.0180(12) -0.0019(9) 0.0076(10) 0.0006(9) C27 0.0307(13) 0.0259(13) 0.0199(13) -0.0032(10) 0.0062(10) -0.0067(10) C28 0.0417(16) 0.0377(17) 0.0341(16) 0.0021(13) 0.0001(13) -0.0090(13) C29 0.0360(14) 0.0224(14) 0.0302(14) 0.0005(11) 0.0165(12) 0.0009(11) C30 0.0219(11) 0.0191(11) 0.0234(13) -0.0018(10) 0.0079(9) 0.0021(9) C31 0.0196(11) 0.0195(11) 0.0206(12) -0.0008(10) 0.0045(9) 0.0020(9) C32 0.0291(12) 0.0211(12) 0.0194(13) 0.0045(10) 0.0037(10) 0.0063(10) 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' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 S2 Ni1 S1 94.10(3) . . S2 Ni1 P2 95.52(2) . . S1 Ni1 P2 170.36(3) . . S2 Ni1 P1 168.42(3) . . S1 Ni1 P1 97.02(2) . . P2 Ni1 P1 73.43(2) . . C31 S1 Ni1 102.16(8) . . C30 S2 Ni1 102.28(9) . . C28 S3 C27 101.00(13) . . N1 P1 C1 107.90(10) . . N1 P1 C7 108.95(10) . . C1 P1 C7 106.43(11) . . N1 P1 Ni1 93.56(7) . . C1 P1 Ni1 119.45(8) . . C7 P1 Ni1 118.97(8) . . N1 P1 P2 40.66(6) . . C1 P1 P2 127.75(8) . . C7 P1 P2 121.84(8) . . Ni1 P1 P2 53.088(19) . . N1 P2 C13 111.51(10) . . N1 P2 C19 109.10(10) . . C13 P2 C19 104.03(11) . . N1 P2 Ni1 94.05(7) . . C13 P2 Ni1 117.28(7) . . C19 P2 Ni1 120.44(8) . . N1 P2 P1 40.76(6) . . C13 P2 P1 129.80(8) . . C19 P2 P1 123.17(8) . . Ni1 P2 P1 53.484(19) . . C25 N1 P2 130.91(15) . . C25 N1 P1 128.69(15) . . P2 N1 P1 98.58(10) . . C6 C1 C2 119.5(2) . . C6 C1 P1 116.62(18) . . C2 C1 P1 123.66(18) . . C3 C2 C1 119.8(2) . . C3 C2 H2 120.1 . . C1 C2 H2 120.1 . . C4 C3 C2 120.5(2) . . C4 C3 H3 119.7 . . C2 C3 H3 119.7 . . C3 C4 C5 119.9(2) . . C3 C4 H4 120.0 . . C5 C4 H4 120.0 . . C4 C5 C6 120.1(2) . . C4 C5 H5 120.0 . . C6 C5 H5 120.0 . . C5 C6 C1 120.1(2) . . C5 C6 H6 119.9 . . C1 C6 H6 119.9 . . C8 C7 C12 119.4(2) . . C8 C7 P1 121.19(18) . . C12 C7 P1 119.14(18) . . C9 C8 C7 120.3(2) . . C9 C8 H8 119.8 . . C7 C8 H8 119.8 . . C10 C9 C8 120.2(2) . . C10 C9 H9 119.9 . . C8 C9 H9 119.9 . . C9 C10 C11 119.9(2) . . C9 C10 H10 120.0 . . C11 C10 H10 120.0 . . C12 C11 C10 120.2(2) . . C12 C11 H11 119.9 . . C10 C11 H11 119.9 . . C11 C12 C7 119.9(2) . . C11 C12 H12 120.1 . . C7 C12 H12 120.1 . . C14 C13 C18 119.0(2) . . C14 C13 P2 122.39(18) . . C18 C13 P2 118.2(2) . . C13 C14 C15 120.5(2) . . C13 C14 H14 119.7 . . C15 C14 H14 119.7 . . C14 C15 C16 119.6(3) . . C14 C15 H15 120.2 . . C16 C15 H15 120.2 . . C17 C16 C15 120.2(3) . . C17 C16 H16 119.9 . . C15 C16 H16 119.9 . . C16 C17 C18 120.3(3) . . C16 C17 H17 119.8 . . C18 C17 H17 119.8 . . C17 C18 C13 120.3(3) . . C17 C18 H18 119.9 . . C13 C18 H18 119.9 . . C20 C19 C24 119.6(2) . . C20 C19 P2 120.64(17) . . C24 C19 P2 119.76(18) . . C21 C20 C19 119.9(2) . . C21 C20 H20 120.1 . . C19 C20 H20 120.1 . . C20 C21 C22 120.0(2) . . C20 C21 H21 120.0 . . C22 C21 H21 120.0 . . C23 C22 C21 120.2(2) . . C23 C22 H22 119.9 . . C21 C22 H22 119.9 . . C24 C23 C22 120.3(2) . . C24 C23 H23 119.9 . . C22 C23 H23 119.9 . . C23 C24 C19 120.0(2) . . C23 C24 H24 120.0 . . C19 C24 H24 120.0 . . N1 C25 C26 114.97(19) . . N1 C25 H25A 108.5 . . C26 C25 H25A 108.5 . . N1 C25 H25B 108.5 . . C26 C25 H25B 108.5 . . H25A C25 H25B 107.5 . . C27 C26 C25 113.88(19) . . C27 C26 H26A 108.8 . . C25 C26 H26A 108.8 . . C27 C26 H26B 108.8 . . C25 C26 H26B 108.8 . . H26A C26 H26B 107.7 . . C26 C27 S3 114.09(17) . . C26 C27 H27A 108.7 . . S3 C27 H27A 108.7 . . C26 C27 H27B 108.7 . . S3 C27 H27B 108.7 . . H27A C27 H27B 107.6 . . S3 C28 H28A 109.5 . . S3 C28 H28B 109.5 . . H28A C28 H28B 109.5 . . S3 C28 H28C 109.5 . . H28A C28 H28C 109.5 . . H28B C28 H28C 109.5 . . N3 C29 C30 177.3(3) . . C31 C30 C29 122.5(2) . . C31 C30 S2 120.20(19) . . C29 C30 S2 117.30(18) . . C30 C31 C32 120.9(2) . . C30 C31 S1 121.26(18) . . C32 C31 S1 117.79(18) . . N2 C32 C31 178.2(3) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ni1 S2 2.1462(7) . Ni1 S1 2.1472(6) . Ni1 P2 2.1478(6) . Ni1 P1 2.1589(7) . S1 C31 1.735(2) . S2 C30 1.746(2) . S3 C28 1.795(3) . S3 C27 1.806(3) . P1 N1 1.6999(19) . P1 C1 1.801(2) . P1 C7 1.802(2) . P1 P2 2.5746(7) . P2 N1 1.6967(19) . P2 C13 1.804(2) . P2 C19 1.805(2) . N1 C25 1.480(3) . N2 C32 1.147(3) . N3 C29 1.147(4) . C1 C6 1.392(3) . C1 C2 1.395(3) . C2 C3 1.383(3) . C2 H2 0.9300 . C3 C4 1.383(4) . C3 H3 0.9300 . C4 C5 1.383(4) . C4 H4 0.9300 . C5 C6 1.388(4) . C5 H5 0.9300 . C6 H6 0.9300 . C7 C8 1.392(3) . C7 C12 1.401(3) . C8 C9 1.384(4) . C8 H8 0.9300 . C9 C10 1.383(4) . C9 H9 0.9300 . C10 C11 1.392(4) . C10 H10 0.9300 . C11 C12 1.385(4) . C11 H11 0.9300 . C12 H12 0.9300 . C13 C14 1.384(4) . C13 C18 1.404(3) . C14 C15 1.389(4) . C14 H14 0.9300 . C15 C16 1.394(4) . C15 H15 0.9300 . C16 C17 1.372(4) . C16 H16 0.9300 . C17 C18 1.381(4) . C17 H17 0.9300 . C18 H18 0.9300 . C19 C20 1.396(3) . C19 C24 1.400(3) . C20 C21 1.386(3) . C20 H20 0.9300 . C21 C22 1.388(4) . C21 H21 0.9300 . C22 C23 1.384(4) . C22 H22 0.9300 . C23 C24 1.379(3) . C23 H23 0.9300 . C24 H24 0.9300 . C25 C26 1.523(3) . C25 H25A 0.9700 . C25 H25B 0.9700 . C26 C27 1.522(3) . C26 H26A 0.9700 . C26 H26B 0.9700 . C27 H27A 0.9700 . C27 H27B 0.9700 . C28 H28A 0.9600 . C28 H28B 0.9600 . C28 H28C 0.9600 . C29 C30 1.430(4) . C30 C31 1.364(3) . C31 C32 1.432(3) .