#------------------------------------------------------------------------------ #$Date: 2024-10-06 10:06:31 +0300 (Sun, 06 Oct 2024) $ #$Revision: 295190 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572146.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_1572146 loop_ _publ_author_name 'Kreimer, Lisa N.' 'Hadlington, Terrance J.' _publ_section_title ; Macrocyclic bis-diphosphenes demonstrating bimetallic exo- and endo-cyclic binding modes. ; _journal_issue 35 _journal_name_full 'Chemical science' _journal_page_first 14154 _journal_page_last 14160 _journal_paper_doi 10.1039/d4sc03516j _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C22.50 H34 N2 Ni0.50 O P' _chemical_formula_sum 'C22.5 H34 N2 Ni0.5 O P' _chemical_formula_weight 408.84 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2024-05-23 deposited with the CCDC. 2024-07-16 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 97.35(3) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 15.304(3) _cell_length_b 34.054(7) _cell_length_c 9.7484(19) _cell_measurement_reflns_used 2000 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 32.50 _cell_measurement_theta_min 1.92 _cell_volume 5038.8(18) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 150(2) _diffrn_detector Pilatus300K _diffrn_detector_area_resol_mean 5.81 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'STOE StadiVari' _diffrn_measurement_method '\w scans' _diffrn_radiation_collimation '0.6 mm diameter' _diffrn_radiation_monochromator 'Graded multilayer mirror' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1622 _diffrn_reflns_av_unetI/netI 0.2289 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 38479 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.000 _diffrn_reflns_theta_min 2.190 _diffrn_source 'Genix 3D HF Mo' _diffrn_source_current 1.000 _diffrn_source_power 0.050 _diffrn_source_voltage 50 _exptl_absorpt_coefficient_mu 0.484 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.899 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'STOE X-AREA 1.76' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.078 _exptl_crystal_description block _exptl_crystal_F_000 1760 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.758 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.107 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.894 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 503 _refine_ls_number_reflns 9847 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.894 _refine_ls_R_factor_all 0.2087 _refine_ls_R_factor_gt 0.0772 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1144P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1869 _refine_ls_wR_factor_ref 0.2419 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3922 _reflns_number_total 9847 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03516j2.cif _cod_data_source_block 2b_prime _cod_depositor_comments 'Adding full bibliography for 1572143--1572150.cif.' _cod_original_cell_volume 5038.9(18) _cod_original_sg_symbol_H-M 'P 21/c' _cod_original_formula_sum 'C22.50 H34 N2 Ni0.50 O P' _cod_database_code 1572146 _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_res_file ; REM Old TITL P21n in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.208, Rweak 0.019, Alpha 0.064 REM 0.339 for 158 systematic absences, Orientation as input REM Formula found by SHELXT: C45 N4 O P2 Br REM C:\XRay\LNK011\P21n_a.res in P2(1)/c REM wR2 = 0.2963, GooF = S = 1.007, Restrained GooF = 1.007 for all data REM R1 = 0.0833 for 3935 Fo > 4sig(Fo) and 0.2136 for all 9860 data REM 503 parameters refined using 0 restraints REM Highest difference peak 0.853, deepest hole -0.443, 1-sigma level 0.119 REM C:\XRay\LNK011\P21n_a.res in P2(1)/c REM wR2 = 0.2497, GooF = S = 0.900, Restrained GooF = 0.900 for all data REM R1 = 0.0799 for 3922 Fo > 4sig(Fo) and 0.2115 for all 9847 data REM 503 parameters refined using 0 restraints REM Highest difference peak 0.770, deepest hole -0.488, 1-sigma level 0.110 REM C:\XRay\LNK011\P21n_a.res in P2(1)/c REM wR2 = 0.2494, GooF = S = 0.901, Restrained GooF = 0.901 for all data REM R1 = 0.0799 for 3922 Fo > 4sig(Fo) and 0.2115 for all 9847 data REM 503 parameters refined using 0 restraints REM Highest difference peak 0.770, deepest hole -0.488, 1-sigma level 0.110 TITL C:\XRay\LNK011\P21n_a.res in P2(1)/c C:\XRay\LNK011~1\P21n_a.res created by SHELXL-2018/3 at 11:49:44 on 16-May-2024 CELL 0.71073 15.3044 34.0543 9.7484 90.000 97.354 90.000 ZERR 8.0000 0.0031 0.0068 0.0019 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O P NI UNIT 180 272 16 8 8 4 MERG 2 OMIT -2 52 FMAP 2 GRID PLAN 20 TEMP -123 BOND OMIT 2 2 0 OMIT -1 4 1 OMIT 0 4 1 OMIT 4 1 0 OMIT 2 3 0 OMIT -1 6 1 OMIT -2 6 1 OMIT 3 1 0 OMIT 1 3 1 OMIT 1 4 0 OMIT 3 3 0 OMIT 2 1 0 OMIT 1 5 1 L.S. 20 ACTA WGHT 0.114400 FVAR 0.35481 NI1 6 0.497668 0.390371 0.436677 11.00000 0.03415 0.02704 = 0.02643 0.00034 0.00540 -0.00082 P1 5 0.513823 0.454338 0.486674 11.00000 0.02850 0.02692 = 0.02758 -0.00064 0.00668 -0.00082 P2 5 0.508827 0.584451 0.350065 11.00000 0.02845 0.02998 = 0.02750 0.00046 0.00700 0.00074 O1 4 0.630759 0.508547 0.347473 11.00000 0.02262 0.02994 = 0.03570 0.00304 0.00853 0.00058 N2 3 0.594035 0.383424 0.196733 11.00000 0.04800 0.03262 = 0.03898 0.00154 0.01512 0.00134 N4 3 0.409227 0.314398 0.373688 11.00000 0.04596 0.02657 = 0.03990 0.00421 -0.00113 0.00260 N1 3 0.478075 0.418554 0.146048 11.00000 0.04743 0.03672 = 0.02310 -0.00015 0.00640 0.00270 N3 3 0.516821 0.308085 0.537724 11.00000 0.04326 0.03178 = 0.03941 0.00317 0.00111 -0.00045 C12 1 0.635839 0.455940 0.511794 11.00000 0.03027 0.02131 = 0.03330 0.00090 0.00783 0.00222 C13 1 0.680130 0.480398 0.428511 11.00000 0.03037 0.02780 = 0.02906 0.00359 0.00780 0.00090 C2 1 0.628363 0.578812 0.340247 11.00000 0.03679 0.03029 = 0.02206 -0.00306 0.01076 -0.00053 C1 1 0.675115 0.544246 0.335310 11.00000 0.03263 0.03200 = 0.02335 0.00074 0.00584 -0.00948 C11 1 0.689503 0.431994 0.604085 11.00000 0.03583 0.03073 = 0.02957 0.00117 0.01106 -0.00145 AFIX 43 H11 2 0.661867 0.415525 0.664374 11.00000 -1.20000 AFIX 0 C6 1 0.764143 0.543851 0.317887 11.00000 0.02376 0.03726 = 0.03021 0.00627 0.00723 0.00703 C9 1 0.820517 0.454080 0.518043 11.00000 0.02093 0.04128 = 0.04222 0.00710 0.00568 0.00222 AFIX 43 H9 2 0.882458 0.452857 0.517186 11.00000 -1.20000 AFIX 0 C3 1 0.675206 0.613792 0.322852 11.00000 0.03535 0.03757 = 0.02578 0.00304 0.01016 0.00634 AFIX 43 H3 2 0.644381 0.637959 0.324787 11.00000 -1.20000 AFIX 0 C24 1 0.522292 0.397567 0.252699 11.00000 0.04020 0.02879 = 0.03443 -0.00302 0.00853 -0.00267 C33 1 0.473851 0.335631 0.451070 11.00000 0.04109 0.03133 = 0.02735 -0.00881 0.01053 -0.00129 C4 1 0.762305 0.615154 0.303343 11.00000 0.02948 0.03937 = 0.03110 0.00273 0.00619 -0.00064 C8 1 0.771233 0.478753 0.425458 11.00000 0.03199 0.03331 = 0.02820 -0.00102 0.00984 -0.00565 C5 1 0.806341 0.578926 0.302712 11.00000 0.03185 0.03878 = 0.03286 0.00509 0.00888 -0.00486 AFIX 43 H5 2 0.867086 0.578680 0.291459 11.00000 -1.20000 AFIX 0 C14 1 0.813743 0.653183 0.283886 11.00000 0.03515 0.03483 = 0.04269 0.00333 0.00993 -0.01501 C7 1 0.807507 0.503582 0.314820 11.00000 0.02714 0.03126 = 0.03859 0.00535 0.01273 0.00123 C10 1 0.782384 0.430873 0.612870 11.00000 0.03250 0.03622 = 0.03588 0.00711 0.00929 -0.00323 C30 1 0.660716 0.358432 0.272973 11.00000 0.04847 0.03100 = 0.03979 -0.00159 0.00613 0.00380 AFIX 13 H30 2 0.651204 0.359136 0.372537 11.00000 -1.20000 AFIX 0 C29 1 0.413791 0.484845 0.137866 11.00000 0.05714 0.04286 = 0.04531 -0.00095 -0.00183 -0.00018 AFIX 137 H29A 2 0.462949 0.493545 0.205400 11.00000 -1.50000 H29B 2 0.360458 0.499398 0.152164 11.00000 -1.50000 H29C 2 0.427889 0.489748 0.044102 11.00000 -1.50000 AFIX 0 C26 1 0.592655 0.395161 0.059958 11.00000 0.07219 0.05118 = 0.03032 0.00141 0.02635 -0.00198 AFIX 43 H26 2 0.634568 0.388597 -0.000265 11.00000 -1.20000 AFIX 0 C25 1 0.521760 0.417221 0.029867 11.00000 0.07281 0.04072 = 0.02797 0.00211 0.01255 0.00664 AFIX 43 H25 2 0.503895 0.429899 -0.055951 11.00000 -1.20000 AFIX 0 C34 1 0.411353 0.275215 0.410933 11.00000 0.05294 0.03418 = 0.06592 0.01070 -0.00504 -0.00945 AFIX 43 H34 2 0.372970 0.255098 0.371804 11.00000 -1.20000 AFIX 0 C36 1 0.348764 0.330916 0.261216 11.00000 0.05117 0.03157 = 0.05134 -0.00651 -0.00078 -0.00269 AFIX 13 H36 2 0.355437 0.360124 0.264614 11.00000 -1.20000 AFIX 0 C39 1 0.589803 0.317126 0.644417 11.00000 0.05513 0.03351 = 0.04783 0.01099 -0.00741 0.00044 AFIX 13 H39 2 0.605351 0.345453 0.635524 11.00000 -1.20000 AFIX 0 C27 1 0.398476 0.441391 0.156280 11.00000 0.04810 0.04210 = 0.03065 0.00122 0.00032 0.00276 AFIX 13 H27 2 0.381288 0.437293 0.250815 11.00000 -1.20000 AFIX 0 C19 1 0.909148 0.505968 0.337037 11.00000 0.03069 0.05091 = 0.05296 0.01217 0.01667 0.00094 AFIX 137 H19A 2 0.929511 0.520943 0.261352 11.00000 -1.50000 H19B 2 0.933864 0.479400 0.338668 11.00000 -1.50000 H19C 2 0.928539 0.519075 0.425184 11.00000 -1.50000 AFIX 0 C16 1 0.889874 0.657470 0.401919 11.00000 0.03807 0.05208 = 0.05802 -0.00329 0.00201 -0.01064 AFIX 137 H16A 2 0.866014 0.659895 0.490152 11.00000 -1.50000 H16B 2 0.924244 0.680978 0.386507 11.00000 -1.50000 H16C 2 0.927933 0.634271 0.404400 11.00000 -1.50000 AFIX 0 C15 1 0.852797 0.651494 0.146581 11.00000 0.04388 0.04882 = 0.05595 0.00712 0.01900 -0.01183 AFIX 137 H15A 2 0.895356 0.629911 0.149603 11.00000 -1.50000 H15B 2 0.882518 0.676358 0.132051 11.00000 -1.50000 H15C 2 0.805446 0.647134 0.070443 11.00000 -1.50000 AFIX 0 C35 1 0.478932 0.271124 0.514214 11.00000 0.06406 0.01814 = 0.07149 0.00599 0.00000 -0.00785 AFIX 43 H35 2 0.497017 0.247531 0.561568 11.00000 -1.20000 AFIX 0 C18 1 0.780669 0.483934 0.171528 11.00000 0.05012 0.05021 = 0.03989 0.00118 0.01831 0.00910 AFIX 137 H18A 2 0.716900 0.479435 0.157839 11.00000 -1.50000 H18B 2 0.811444 0.458785 0.168136 11.00000 -1.50000 H18C 2 0.796758 0.501206 0.098353 11.00000 -1.50000 AFIX 0 C20 1 0.836549 0.405127 0.716584 11.00000 0.03151 0.05040 = 0.05214 0.02654 0.00163 -0.00013 C28 1 0.322715 0.426217 0.049926 11.00000 0.05759 0.05030 = 0.05299 0.00610 -0.01044 -0.01141 AFIX 137 H28A 2 0.338277 0.429776 -0.043717 11.00000 -1.50000 H28B 2 0.268847 0.440964 0.059530 11.00000 -1.50000 H28C 2 0.312880 0.398269 0.066386 11.00000 -1.50000 AFIX 0 C17 1 0.754535 0.689363 0.281257 11.00000 0.04889 0.03709 = 0.07033 0.00445 0.01540 -0.00630 AFIX 137 H17A 2 0.705451 0.686655 0.206772 11.00000 -1.50000 H17B 2 0.788762 0.712866 0.265222 11.00000 -1.50000 H17C 2 0.731409 0.691776 0.370090 11.00000 -1.50000 AFIX 0 C41 1 0.670885 0.292440 0.622880 11.00000 0.05734 0.03983 = 0.08027 0.00657 -0.00595 0.00629 AFIX 137 H41A 2 0.657209 0.264518 0.631901 11.00000 -1.50000 H41B 2 0.720216 0.299593 0.692644 11.00000 -1.50000 H41C 2 0.686985 0.297452 0.530349 11.00000 -1.50000 AFIX 0 C38 1 0.373106 0.316791 0.122412 11.00000 0.07768 0.07878 = 0.04226 -0.01739 -0.00558 0.02246 AFIX 137 H38A 2 0.436635 0.319929 0.120987 11.00000 -1.50000 H38B 2 0.341071 0.332339 0.047652 11.00000 -1.50000 H38C 2 0.357239 0.289035 0.109485 11.00000 -1.50000 AFIX 0 C31 1 0.753387 0.373667 0.263723 11.00000 0.04601 0.06134 = 0.06534 -0.00581 0.01611 -0.00237 AFIX 137 H31A 2 0.764685 0.373349 0.167022 11.00000 -1.50000 H31B 2 0.796395 0.356853 0.318967 11.00000 -1.50000 H31C 2 0.758684 0.400600 0.299233 11.00000 -1.50000 AFIX 0 C32 1 0.648163 0.315538 0.222947 11.00000 0.06457 0.04085 = 0.05891 -0.00400 0.00199 0.00203 AFIX 137 H32A 2 0.590768 0.305888 0.242776 11.00000 -1.50000 H32B 2 0.695001 0.299148 0.271212 11.00000 -1.50000 H32C 2 0.650753 0.314355 0.123104 11.00000 -1.50000 AFIX 0 C37 1 0.255129 0.321376 0.277503 11.00000 0.05394 0.08227 = 0.08564 0.02787 0.00417 -0.00169 AFIX 137 H37A 2 0.245755 0.292998 0.267530 11.00000 -1.50000 H37B 2 0.215602 0.335174 0.206353 11.00000 -1.50000 H37C 2 0.242754 0.329714 0.369285 11.00000 -1.50000 AFIX 0 C21 1 0.787798 0.389577 0.829109 11.00000 0.05193 0.08660 = 0.05586 0.03727 -0.00069 0.01119 AFIX 137 H21A 2 0.764364 0.411565 0.878020 11.00000 -1.50000 H21B 2 0.828082 0.374137 0.894325 11.00000 -1.50000 H21C 2 0.739097 0.372870 0.788501 11.00000 -1.50000 AFIX 0 C40 1 0.563202 0.310839 0.787275 11.00000 0.08549 0.06873 = 0.04182 0.00625 -0.00501 -0.00030 AFIX 137 H40A 2 0.512002 0.327268 0.798360 11.00000 -1.50000 H40B 2 0.612317 0.318022 0.857381 11.00000 -1.50000 H40C 2 0.548084 0.283160 0.798477 11.00000 -1.50000 AFIX 0 C22 1 0.865983 0.368314 0.638406 11.00000 0.08999 0.09354 = 0.08377 0.04660 0.02600 0.05098 AFIX 137 H22A 2 0.813818 0.353775 0.597439 11.00000 -1.50000 H22B 2 0.902509 0.351324 0.703614 11.00000 -1.50000 H22C 2 0.900075 0.376764 0.565151 11.00000 -1.50000 AFIX 0 C23 1 0.919043 0.426113 0.778246 11.00000 0.06070 0.10499 = 0.10835 0.07316 -0.04033 -0.02952 AFIX 137 H23A 2 0.953480 0.433679 0.704343 11.00000 -1.50000 H23B 2 0.954244 0.408630 0.843390 11.00000 -1.50000 H23C 2 0.903041 0.449674 0.827097 11.00000 -1.50000 AFIX 0 C43 1 0.931463 0.551706 0.880095 11.00000 0.09479 0.12949 = 0.07582 -0.02610 0.00259 0.02735 AFIX 23 H43A 2 0.901948 0.556776 0.962978 11.00000 -1.20000 H43B 2 0.977398 0.531490 0.903831 11.00000 -1.20000 AFIX 0 C42 1 0.970846 0.587265 0.837295 11.00000 0.13484 0.11819 = 0.08142 0.00614 0.00502 -0.00705 AFIX 23 H42A 2 0.969027 0.607983 0.908115 11.00000 -1.20000 H42B 2 1.033074 0.582575 0.824165 11.00000 -1.20000 AFIX 0 C45 1 0.845538 0.575836 0.688196 11.00000 0.17262 0.09192 = 0.07449 -0.00789 -0.00929 -0.03361 AFIX 23 H45A 2 0.830593 0.571649 0.587428 11.00000 -1.20000 H45B 2 0.795594 0.589325 0.723393 11.00000 -1.20000 AFIX 0 C44 1 0.864323 0.537267 0.761295 11.00000 0.11958 0.10144 = 0.14624 -0.04078 0.03714 0.02858 AFIX 23 H44A 2 0.890030 0.517816 0.702473 11.00000 -1.20000 H44B 2 0.811165 0.526098 0.794665 11.00000 -1.20000 AFIX 0 O2 4 0.923456 0.598437 0.715997 11.00000 0.34637 0.24236 = 0.32916 0.20536 -0.18322 -0.13144 HKLF 4 REM C:\XRay\LNK011\P21n_a.res in P2(1)/c REM wR2 = 0.2419, GooF = S = 0.894, Restrained GooF = 0.894 for all data REM R1 = 0.0772 for 3922 Fo > 4sig(Fo) and 0.2087 for all 9847 data REM 503 parameters refined using 0 restraints END WGHT 0.1143 0.0000 REM Highest difference peak 0.758, deepest hole -0.495, 1-sigma level 0.107 Q1 1 1.0025 0.7139 0.7546 11.00000 0.05 0.76 Q2 1 0.9270 0.2722 0.1952 11.00000 0.05 0.74 Q3 1 1.0336 0.7119 -0.0813 11.00000 0.05 0.72 Q4 1 1.0066 0.7806 0.3651 11.00000 0.05 0.69 Q5 1 1.0461 0.7659 0.4549 11.00000 0.05 0.60 Q6 1 0.8869 0.2751 0.1207 11.00000 0.05 0.57 Q7 1 1.0046 0.6108 0.7142 11.00000 0.05 0.53 Q8 1 0.8887 0.6115 0.7137 11.00000 0.05 0.46 Q9 1 0.9505 0.5798 0.5847 11.00000 0.05 0.41 Q10 1 0.4400 0.4160 0.4215 11.00000 0.05 0.40 Q11 1 0.4236 0.4037 0.4557 11.00000 0.05 0.38 Q12 1 0.5569 0.3599 0.4604 11.00000 0.05 0.38 Q13 1 0.9228 0.4569 0.2694 11.00000 0.05 0.37 Q14 1 0.5530 0.5736 0.3474 11.00000 0.05 0.36 Q15 1 0.8864 0.4532 0.8689 11.00000 0.05 0.35 Q16 1 0.4554 0.3734 0.3191 11.00000 0.05 0.35 Q17 1 0.9127 0.5800 0.8282 11.00000 0.05 0.35 Q18 1 0.5610 0.4163 0.4581 11.00000 0.05 0.35 Q19 1 0.3403 0.2934 -0.0091 11.00000 0.05 0.34 Q20 1 0.4573 0.4788 0.4648 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154.58 60.99 -10 -31 2 73.79 58.49 -9 -33 2 -14.50 51.49 -5 -37 2 3.50 47.10 -3 -38 2 -10.80 46.30 -2 -38 2 -35.60 45.10 -16 -16 3 5.60 50.39 -16 -17 3 101.19 53.79 -7 -10 0 415.96 44.60 -7 -11 0 50.99 34.00 -7 -12 0 70.29 34.10 -7 -13 0 17.80 35.80 -6 -18 0 30.00 40.00 -5 -20 0 88.39 40.90 -2 -23 0 23.70 39.50 -1 -23 0 25.30 36.30 -10 0 1 -1.20 32.00 -11 -5 1 186.38 45.40 -11 -16 1 24.60 41.80 -11 -17 1 129.09 47.00 -10 -22 1 202.78 53.99 -9 -25 1 180.98 54.19 -8 -27 1 66.99 50.39 -7 -29 1 -2.80 48.80 -6 -30 1 142.99 52.99 -5 -31 1 315.77 56.29 -4 -32 1 14.20 47.30 0 -32 1 20.90 38.10 -14 -6 2 10.30 42.60 -14 -17 2 144.99 52.89 -13 -23 2 -22.50 48.60 -12 -27 2 -46.20 54.09 -10 -32 2 48.20 60.19 -8 -35 2 18.80 55.99 -7 -36 2 3.50 51.99 -6 -37 2 -17.00 47.20 -4 -38 2 -8.70 50.59 -16 -18 3 30.20 54.89 -16 -19 3 -12.30 58.59 -7 -8 0 54.59 28.90 -7 -9 0 -5.40 29.10 -7 -14 0 196.98 41.80 -7 -15 0 145.69 41.70 -6 -19 0 12.90 38.60 -5 -21 0 129.29 42.90 1 -22 0 10.90 30.80 -3 -23 0 23.20 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52.99 0 -32 4 11.00 52.99 0 -33 4 128.79 56.19 0 -35 4 78.89 48.80 6 -3 2 175.18 26.20 8 -3 2 3.10 29.00 9 -3 2 8.70 29.70 11 -4 2 21.50 37.90 14 -7 2 129.19 50.39 11 -10 3 128.39 46.00 12 -11 3 52.19 47.10 13 -12 3 35.20 45.90 1 -13 3 586.34 43.20 14 -14 3 40.60 46.50 15 -16 3 64.99 57.19 -3 -29 3 -3.50 37.50 7 -16 4 11.80 40.20 5 -17 4 553.34 59.19 9 -17 4 98.79 48.60 3 -19 4 29.40 35.60 11 -19 4 80.79 52.59 12 -21 4 71.99 57.69 13 -23 4 10.10 58.29 1 -24 4 56.59 41.00 13 -24 4 42.80 63.29 1 -25 4 262.67 53.59 1 -38 4 3.70 54.79 1 -39 4 62.69 55.59 7 -3 2 -13.50 21.50 12 -5 2 156.68 40.40 13 -6 2 181.48 47.20 5 -9 3 98.39 34.30 9 -9 3 127.69 43.70 13 -13 3 81.89 52.39 15 -17 3 21.00 49.10 -1 -18 3 0.50 29.90 -2 -22 3 -4.10 30.80 6 -17 4 138.79 45.10 7 -17 4 -0.40 43.70 8 -17 4 52.19 44.00 3 -20 4 338.27 47.80 12 -22 4 52.29 53.29 1 -26 4 226.88 47.50 1 -27 4 51.09 47.70 1 -37 4 33.80 51.89 11 0 1 -5.60 28.50 10 -4 2 67.79 33.70 -4 -20 2 65.29 34.20 8 -9 3 16.40 39.30 4 -10 3 258.47 39.80 10 -10 3 181.98 45.70 3 -11 3 575.04 45.60 2 -12 3 8.70 31.00 12 -12 3 15.60 44.40 14 -15 3 -6.00 43.80 15 -18 3 40.10 54.49 -2 -23 3 90.99 36.70 5 -18 4 131.19 45.90 6 -18 4 250.97 50.99 8 -18 4 121.99 49.20 9 -18 4 219.18 54.69 4 -19 4 29.20 38.00 3 -21 4 56.79 40.10 12 -23 4 27.50 59.29 1 -28 4 133.19 47.20 1 -31 4 27.10 52.19 1 -32 4 44.20 51.49 1 -33 4 118.69 54.99 1 -34 4 73.19 48.90 1 -35 4 81.89 51.59 2 -38 4 22.60 55.99 2 -39 4 -15.70 58.99 5 -4 2 349.77 34.70 14 -8 2 -3.00 43.20 15 -10 2 5.90 40.90 11 -11 3 87.89 43.00 1 -14 3 -11.10 29.50 13 -14 3 25.20 49.20 14 -16 3 23.90 47.40 -1 -19 3 267.37 39.10 15 -19 3 28.00 57.29 -2 -24 3 90.49 39.90 7 -18 4 83.89 46.50 5 -19 4 -51.29 39.10 8 -19 4 280.17 58.29 9 -19 4 202.58 56.29 4 -20 4 67.79 42.30 10 -20 4 138.39 55.59 10 -21 4 80.09 52.49 3 -22 4 78.89 40.70 11 -23 4 -29.50 53.79 12 -27 4 -6.60 63.79 2 -36 4 25.50 60.39 2 -37 4 34.20 53.99 12 -1 1 170.88 31.50 9 -4 2 103.49 35.00 12 -6 2 156.78 42.00 13 -7 2 341.57 49.10 5 -10 3 12.70 33.80 9 -10 3 34.20 34.60 10 -11 3 169.38 45.60 11 -12 3 224.28 53.79 2 -13 3 326.77 39.70 12 -13 3 -6.40 42.50 13 -15 3 -39.80 45.30 0 -17 3 278.87 40.70 14 -17 3 -11.40 53.29 15 -20 3 25.00 59.69 -2 -25 3 10.90 35.90 -2 -26 3 31.30 37.00 6 -19 4 30.40 40.30 7 -19 4 479.55 58.69 5 -20 4 -56.69 42.00 8 -20 4 -63.29 43.00 9 -20 4 117.59 54.79 4 -21 4 146.39 45.80 10 -22 4 13.20 49.70 3 -23 4 94.09 45.10 11 -24 4 -32.70 54.09 11 -25 4 40.10 61.49 2 -26 4 62.29 41.80 2 -27 4 94.09 46.40 2 -28 4 16.90 50.39 2 -29 4 61.99 51.29 2 -31 4 91.69 59.19 2 -32 4 33.10 50.89 2 -33 4 121.49 53.79 2 -34 4 46.50 50.69 2 -35 4 -10.50 49.70 3 -37 4 -44.50 62.79 3 -38 4 -12.00 62.49 10 0 1 -15.30 31.50 6 -4 2 -28.50 22.50 7 -4 2 153.58 32.20 8 -4 2 254.37 38.50 14 -9 2 55.79 46.40 15 -11 2 110.99 47.60 16 -13 2 40.10 51.69 -4 -22 2 10.20 32.10 6 -10 3 301.47 45.90 7 -10 3 214.18 45.00 4 -11 3 39.50 32.10 3 -12 3 352.16 41.60 12 -14 3 38.30 50.89 1 -15 3 811.52 49.70 14 -18 3 1.90 53.29 -2 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55.49 4 -34 4 48.00 54.49 5 -35 4 69.69 59.99 5 -36 4 20.00 61.49 12 -2 1 10.10 28.70 5 -5 2 22.80 24.70 13 -9 2 -31.00 44.30 15 -13 2 -2.70 42.60 -3 -18 2 518.75 36.30 -4 -24 2 181.58 36.00 5 -12 3 24.00 38.70 9 -12 3 22.10 36.20 10 -13 3 175.08 44.70 11 -14 3 -9.70 44.10 12 -16 3 9.40 47.60 13 -18 3 26.70 48.50 0 -19 3 429.56 45.90 14 -22 3 63.79 57.39 -1 -23 3 106.69 39.00 14 -23 3 71.79 63.79 -1 -24 3 128.89 41.80 -1 -36 3 90.89 50.49 6 -25 4 25.20 53.39 7 -25 4 102.99 59.69 5 -26 4 -4.10 50.39 6 -26 4 -3.80 50.19 7 -26 4 17.90 51.79 5 -27 4 -6.90 50.99 6 -27 4 43.70 55.99 7 -27 4 -3.90 46.60 8 -27 4 44.50 52.39 5 -28 4 21.00 55.79 7 -28 4 1.80 50.09 8 -28 4 25.30 54.89 5 -29 4 179.28 58.69 7 -29 4 94.09 57.19 8 -29 4 37.20 57.89 5 -30 4 7.90 48.50 8 -30 4 -3.10 58.79 6 -31 4 -4.00 56.89 7 -31 4 2.60 58.49 8 -31 4 32.80 61.59 6 -32 4 16.70 54.29 7 -32 4 -26.00 57.89 8 -32 4 50.09 56.19 7 -33 4 -52.39 59.59 8 -33 4 92.59 63.89 5 -34 4 29.80 60.59 7 -34 4 96.59 68.09 8 -34 4 101.79 61.99 7 -35 4 52.39 61.99 7 -5 2 492.65 42.80 8 -5 2 229.08 34.50 10 -6 2 47.20 37.40 11 -7 2 46.30 35.00 12 -8 2 30.40 39.90 14 -11 2 72.09 50.39 16 -16 2 7.90 49.40 -4 -25 2 30.70 30.70 6 -12 3 366.66 46.30 7 -12 3 165.38 42.90 4 -13 3 41.50 36.20 3 -14 3 34.10 30.80 10 -14 3 -11.30 39.80 2 -15 3 30.40 32.50 11 -15 3 -30.70 43.00 13 -19 3 47.70 49.30 0 -20 3 307.57 48.70 13 -20 3 186.18 60.29 14 -24 3 67.89 58.59 -1 -25 3 -2.60 35.90 -1 -26 3 6.70 34.60 -1 -33 3 144.79 51.29 -1 -34 3 178.28 50.69 -1 -35 3 47.80 41.20 0 -39 3 5.70 54.29 6 -29 4 90.79 53.89 6 -30 4 33.00 50.59 7 -30 4 50.89 50.39 10 -1 1 438.96 42.60 4 -6 2 224.78 35.30 13 -10 2 9.60 42.40 14 -12 2 8.80 45.60 15 -14 2 -2.50 45.80 16 -17 2 -0.30 50.49 16 -18 2 27.00 56.79 -3 -19 2 161.68 35.10 5 -13 3 34.40 38.70 8 -13 3 56.99 38.90 2 -16 3 350.66 45.20 11 -16 3 412.06 60.69 12 -18 3 -56.69 45.40 0 -21 3 -18.30 37.90 13 -21 3 -49.80 51.29 13 -22 3 79.39 60.59 -1 -27 3 222.28 46.40 -1 -28 3 727.93 62.59 -1 -29 3 3.50 42.80 -1 -30 3 392.06 61.29 -1 -31 3 -56.99 44.60 -1 -32 3 18.70 47.20 0 -38 3 57.49 49.80 9 -6 2 126.69 35.00 12 -9 2 -6.50 37.80 15 -15 2 35.70 53.09 16 -19 2 39.60 61.99 6 -13 3 785.52 60.79 7 -13 3 1340.57 75.79 4 -14 3 49.60 36.80 3 -15 3 12.90 35.80 10 -15 3 -5.90 40.50 11 -17 3 -3.40 50.69 12 -19 3 7.00 42.80 0 -22 3 171.68 44.40 13 -23 3 -3.10 54.69 13 -24 3 16.30 60.29 0 -36 3 74.09 50.69 0 -37 3 11.20 44.60 1 -39 3 -33.70 53.79 11 -2 1 20.80 27.20 12 -3 1 82.59 30.90 5 -6 2 237.58 35.00 8 -6 2 -2.40 34.00 10 -7 2 393.86 49.99 11 -8 2 -20.30 34.60 13 -11 2 36.00 47.30 14 -13 2 -11.70 42.70 15 -16 2 -9.00 46.20 -3 -20 2 38.10 33.80 5 -14 3 32.60 38.50 2 -17 3 335.97 46.00 11 -18 3 18.80 49.20 12 -20 3 196.28 59.19 12 -21 3 -6.00 47.20 0 -23 3 208.58 43.70 13 -25 3 -2.00 57.09 13 -26 3 92.69 68.79 0 -34 3 218.08 52.79 9 -1 1 462.75 38.50 7 -6 2 374.46 38.70 12 -10 2 -14.50 38.70 14 -14 2 49.70 46.40 -2 -16 2 12.00 22.40 15 -17 2 -35.50 52.79 -3 -21 2 836.32 54.19 7 -14 3 -32.80 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310.37 49.30 8 -16 3 253.67 46.30 9 -17 3 167.48 48.70 9 -18 3 -11.30 44.50 2 -19 3 457.15 51.29 10 -20 3 253.57 60.29 1 -22 3 88.09 42.20 1 -23 3 59.59 40.70 11 -23 3 51.79 48.50 1 -33 3 165.08 60.39 1 -34 3 62.99 47.40 2 -37 3 27.00 48.10 3 -39 3 15.60 53.89 11 -3 1 28.20 28.70 14 -7 1 135.29 42.10 6 -7 2 60.59 32.30 3 -8 2 134.19 31.50 9 -8 2 -7.80 39.80 2 -9 2 40.10 28.90 11 -10 2 161.68 44.60 13 -14 2 55.79 52.49 14 -16 2 53.39 42.80 14 -17 2 109.89 51.69 15 -21 2 90.69 58.79 15 -22 2 4.60 61.19 -3 -23 2 2.60 29.10 -3 -24 2 94.49 32.20 6 -16 3 207.28 43.70 4 -17 3 -2.00 39.90 7 -17 3 311.77 49.90 8 -17 3 108.39 44.90 3 -18 3 71.09 38.60 9 -19 3 270.97 54.39 2 -20 3 679.23 57.69 10 -21 3 -1.60 50.79 1 -24 3 101.99 36.90 11 -24 3 9.50 50.59 1 -25 3 -8.20 35.00 11 -25 3 18.00 52.89 1 -26 3 399.06 52.59 1 -27 3 61.79 42.30 11 -27 3 68.79 57.59 1 -28 3 120.59 47.20 11 -28 3 -19.50 58.69 1 -29 3 1.50 43.90 11 -29 3 29.60 60.79 1 -30 3 51.49 46.70 11 -30 3 33.80 60.49 1 -31 3 15.80 48.80 11 -31 3 48.10 64.99 1 -32 3 -8.60 46.40 2 -35 3 21.70 47.60 2 -36 3 -0.90 45.70 3 -37 3 3.80 53.59 4 -38 3 -0.40 66.19 4 -39 3 -42.00 56.79 13 -6 1 209.58 40.80 15 -10 1 -6.50 37.80 16 -13 1 20.00 45.50 12 -12 2 154.68 44.50 14 -18 2 -29.80 45.30 -3 -25 2 39.60 31.20 -3 -27 2 75.19 34.60 -3 -28 2 44.00 34.70 -3 -29 2 93.49 38.80 5 -17 3 71.79 39.80 4 -18 3 -15.60 39.90 7 -18 3 -9.40 38.80 9 -20 3 298.17 59.29 10 -22 3 79.09 52.09 10 -23 3 19.00 46.10 10 -24 3 83.89 52.09 10 -25 3 -8.80 49.00 10 -30 3 75.59 64.59 10 -31 3 57.79 62.09 10 -32 3 -10.30 60.29 10 -33 3 63.49 67.69 3 -36 3 -1.80 49.60 4 -37 3 20.00 57.49 5 -38 3 68.99 59.69 14 -8 1 -5.60 39.00 4 -8 2 -1.40 24.20 8 -8 2 71.29 34.10 1 -11 2 516.15 42.20 11 -11 2 367.76 49.70 12 -13 2 96.09 46.80 -1 -15 2 1112.19 43.80 -2 -19 2 309.87 36.20 14 -19 2 115.09 54.09 5 -18 3 29.60 38.30 6 -18 3 -28.50 36.80 4 -19 3 81.99 44.40 5 -19 3 47.40 38.60 7 -19 3 19.60 40.50 8 -20 3 196.38 50.59 3 -21 3 14.10 35.00 9 -21 3 -17.50 47.90 9 -22 3 19.10 48.50 9 -23 3 44.90 50.59 2 -24 3 4.00 37.20 2 -25 3 77.49 44.60 2 -26 3 198.28 52.29 10 -26 3 198.98 61.49 10 -27 3 37.60 53.09 2 -28 3 24.90 46.10 10 -28 3 -3.40 55.09 2 -29 3 13.30 47.80 10 -29 3 79.39 61.29 2 -30 3 193.68 56.79 2 -32 3 32.50 48.00 9 -32 3 -4.30 62.99 9 -33 3 54.49 59.39 3 -34 3 107.69 53.69 8 -34 3 56.19 66.69 9 -34 3 -5.90 66.29 8 -35 3 -44.70 60.69 4 -36 3 46.70 54.69 5 -36 3 -24.00 56.09 7 -36 3 -29.50 59.99 5 -37 3 6.10 56.79 6 -37 3 29.50 58.29 10 -3 1 37.00 30.10 11 -4 1 -19.60 30.90 12 -5 1 110.09 34.50 16 -14 1 -32.50 43.80 5 -8 2 1.70 27.20 3 -9 2 53.29 30.70 9 -9 2 76.29 39.60 2 -10 2 -16.90 34.00 10 -10 2 102.69 35.00 11 -12 2 235.28 50.19 12 -14 2 252.47 53.19 13 -16 2 70.69 49.00 14 -20 2 60.09 52.99 14 -21 2 159.48 60.89 14 -22 2 42.50 55.19 6 -19 3 81.49 40.50 6 -20 3 555.94 57.49 7 -20 3 376.06 55.59 7 -21 3 65.09 46.90 8 -21 3 -9.20 43.00 3 -23 3 125.69 42.30 9 -24 3 123.19 58.79 9 -25 3 90.99 52.99 9 -26 3 222.58 59.69 2 -27 3 56.59 39.70 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54.09 43.80 2 11 -6 4.80 49.30 4 10 -6 148.99 47.70 -6 9 -5 68.89 45.10 4 9 -5 89.69 36.60 -2 9 -4 271.57 42.90 -7 7 -4 91.39 45.00 -1 12 -11 74.29 76.79 0 12 -11 -39.10 73.49 1 12 -11 -16.70 70.89 6 10 -11 66.09 61.79 -2 12 -10 51.99 66.79 -5 11 -10 26.10 70.39 5 11 -10 79.99 58.49 -3 12 -9 -18.90 57.29 -7 10 -9 36.20 63.19 -8 9 -9 -10.80 67.39 -9 8 -9 23.00 72.69 -10 7 -9 -32.10 68.89 -3 12 -8 -20.00 51.29 -2 12 -8 -3.20 57.89 -5 11 -8 -16.40 61.59 6 10 -8 109.19 56.09 -8 9 -8 -47.00 59.29 -9 8 -8 164.78 63.09 -10 7 -8 7.70 62.89 -2 11 -6 201.48 46.70 1 11 -6 -35.90 50.49 -11 5 -6 -16.60 54.19 -3 10 -5 52.59 44.20 1 10 -5 37.10 42.40 -7 8 -5 346.57 56.39 -11 4 -5 77.29 54.49 -1 9 -4 26.70 37.50 3 8 -4 249.38 35.20 -4 7 -3 4.20 28.60 -3 11 -11 41.10 69.69 4 11 -11 -11.90 63.69 7 9 -11 -28.30 58.49 0 12 -10 65.89 67.09 1 12 -10 209.38 72.89 6 10 -10 49.40 56.29 -2 12 -9 7.40 58.59 -1 12 -9 -0.20 64.99 0 12 -9 38.00 64.99 1 12 -9 78.29 56.69 -5 11 -9 93.19 57.59 6 10 -9 -35.10 55.59 -1 12 -8 95.19 58.99 0 12 -8 12.30 49.70 1 12 -8 54.79 52.59 7 9 -8 36.30 53.19 -4 11 -7 61.59 54.29 3 11 -7 225.98 49.00 -6 10 -7 -19.10 54.69 5 10 -7 9.30 39.40 -1 11 -6 23.00 45.80 0 11 -6 5.70 49.10 -8 8 -6 117.69 50.09 -9 7 -6 318.17 66.39 -10 6 -6 105.89 56.79 -2 10 -5 -52.99 44.90 -1 10 -5 5.30 44.30 0 10 -5 215.48 50.09 5 8 -5 60.79 40.80 -8 7 -5 134.39 47.10 -10 5 -5 52.99 46.70 -8 6 -4 47.30 40.50 -10 4 -4 -42.10 41.20 -3 7 -3 6.70 34.60 -2 11 -11 39.10 76.39 3 11 -11 49.20 63.89 5 10 -11 -41.80 63.49 4 11 -10 42.70 55.19 -7 9 -10 -2.20 71.29 7 9 -10 -0.60 53.79 -4 11 -9 38.10 59.29 4 11 -9 43.70 57.29 7 9 -9 188.28 62.99 -4 11 -8 -18.40 59.49 8 8 -8 -9.30 45.70 -11 5 -8 -52.19 64.19 -3 11 -7 122.29 52.69 -7 9 -7 229.88 67.29 6 9 -7 275.87 54.29 -11 5 -7 -47.60 50.59 3 10 -6 143.39 48.20 5 9 -6 18.80 40.50 3 9 -5 66.59 38.00 0 7 -3 25.30 31.20 -7 5 -3 104.99 38.60 -1 11 -11 -37.10 72.09 0 11 -11 0.90 71.79 1 11 -11 -8.60 72.89 2 11 -11 26.00 61.39 -3 11 -10 2.60 68.79 3 11 -10 -4.70 54.09 -5 10 -10 26.50 73.79 8 8 -10 -1.20 48.80 -3 11 -9 54.59 60.79 3 11 -9 62.49 57.69 -7 9 -9 128.39 67.39 -8 8 -9 -40.60 64.89 8 8 -9 168.98 52.79 -10 6 -9 14.80 63.59 -3 11 -8 8.30 52.89 3 11 -8 28.70 49.00 5 10 -8 16.50 45.90 -7 9 -8 33.60 58.69 -2 11 -7 -52.49 45.40 1 11 -7 32.30 45.30 -5 10 -7 22.20 50.79 4 10 -7 27.50 44.70 -8 8 -7 -5.20 55.79 7 8 -7 40.80 41.80 -9 7 -7 -7.10 62.49 -10 6 -7 32.30 51.59 -4 10 -6 369.16 54.19 -6 9 -6 -29.40 43.70 6 8 -6 304.17 47.00 -4 9 -5 239.08 53.39 6 7 -5 18.80 36.70 -4 8 -4 91.79 38.10 2 8 -4 9.60 29.90 -6 7 -4 377.86 53.29 4 7 -4 187.18 32.40 -2 7 -3 -17.60 31.60 -1 7 -3 819.42 51.99 -3 10 -11 22.00 72.39 4 10 -11 99.49 68.39 6 9 -11 -33.00 55.09 -2 11 -10 18.20 57.79 -1 11 -10 10.20 62.89 0 11 -10 42.70 61.69 1 11 -10 136.89 62.99 -2 11 -9 135.99 65.39 -5 10 -9 26.70 57.19 5 10 -9 8.60 53.59 -2 11 -8 5.00 58.39 -5 10 -8 322.67 74.09 -8 8 -8 70.09 61.49 -9 7 -8 38.20 55.39 -1 11 -7 39.40 44.50 0 11 -7 58.59 46.60 8 7 -7 -26.00 39.00 -3 10 -6 301.57 51.19 2 10 -6 178.98 53.99 -7 8 -6 65.19 49.99 7 7 -6 49.90 36.30 -11 4 -6 -7.90 51.99 2 9 -5 176.08 45.40 -6 8 -5 165.98 51.79 7 6 -5 87.99 40.30 -5 6 -3 165.28 31.90 -8 4 -3 28.70 36.10 -9 3 -3 75.29 43.70 -2 10 -11 7.10 70.39 3 10 -11 27.50 65.29 7 8 -11 0.40 56.89 4 10 -10 157.88 62.19 6 9 -10 55.99 52.49 -7 8 -10 8.60 72.49 -1 11 -9 244.18 71.39 0 11 -9 211.68 71.59 1 11 -9 265.87 67.89 6 9 -9 259.27 62.29 -1 11 -8 161.78 58.09 0 11 -8 49.20 54.99 4 10 -8 126.49 54.89 6 9 -8 111.49 46.90 -4 10 -7 -3.10 49.80 3 10 -7 111.19 45.80 -6 9 -7 217.88 62.89 -11 4 -7 -4.00 50.49 -2 10 -6 222.68 52.09 1 10 -6 173.38 53.49 4 9 -6 15.70 40.00 -8 7 -6 167.18 56.09 -9 6 -6 -7.60 54.99 8 6 -6 37.10 34.00 -10 5 -6 -45.80 52.99 -3 9 -5 433.86 55.19 4 8 -5 391.56 50.59 -7 7 -5 -32.80 44.50 -3 8 -4 77.19 36.80 1 8 -4 49.99 36.80 -7 6 -4 0.30 43.70 -1 10 -11 -22.30 67.99 0 10 -11 94.59 75.79 1 10 -11 104.09 75.19 2 10 -11 76.29 70.69 -4 9 -11 -68.39 70.69 5 9 -11 63.89 59.29 -3 10 -10 102.49 73.69 3 10 -10 143.19 62.09 -5 9 -10 2.00 69.99 7 8 -10 0.10 52.49 -4 10 -9 9.60 51.19 4 10 -9 -54.19 53.79 -7 8 -9 12.90 61.99 -8 7 -9 -1.60 63.89 -9 6 -9 53.19 62.79 -4 10 -8 137.29 65.09 -7 8 -8 242.88 71.49 7 8 -8 155.98 52.49 8 7 -8 15.30 44.70 -11 4 -8 -3.30 60.29 -3 10 -7 -1.00 45.70 5 9 -7 218.78 47.30 -7 8 -7 30.00 55.49 -10 5 -7 -7.00 52.89 0 10 -6 170.38 51.59 -2 9 -5 181.98 49.60 0 9 -5 355.66 52.09 1 9 -5 688.93 56.69 -8 6 -5 50.99 46.90 -9 5 -5 -0.60 40.60 -10 4 -5 42.40 48.20 -2 8 -4 4.50 34.30 -1 8 -4 2.90 35.20 0 8 -4 -39.40 37.50 5 6 -4 6.20 24.40 -8 5 -4 38.70 45.30 -9 4 -4 171.58 46.90 -10 3 -4 1.80 38.90 -3 9 -11 25.30 74.79 -2 10 -10 157.78 69.99 -3 10 -9 -13.20 56.79 3 10 -9 -13.90 54.09 -5 9 -9 194.18 64.59 7 8 -9 96.39 54.09 -3 10 -8 136.99 60.39 3 10 -8 446.76 61.79 -8 7 -8 -18.70 52.59 -9 6 -8 -9.70 53.39 -10 5 -8 54.69 56.99 -2 10 -7 24.60 47.30 -5 9 -7 364.96 63.89 -8 7 -7 62.19 56.29 -9 6 -7 73.29 56.29 -4 9 -6 140.19 45.60 -6 8 -6 231.48 50.79 -1 9 -5 387.86 52.09 -4 6 -3 663.53 44.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 13398 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 0.49767(5) 0.39037(2) 0.43668(9) 0.0291(3) Uani 1 1 d . . . . . P1 P 0.51382(11) 0.45434(5) 0.48667(18) 0.0274(4) Uani 1 1 d . . . . . P2 P 0.50883(11) 0.58445(5) 0.35007(18) 0.0283(4) Uani 1 1 d . . . . . O1 O 0.6308(3) 0.50855(12) 0.3475(4) 0.0290(11) Uani 1 1 d . . . . . N2 N 0.5940(4) 0.38342(16) 0.1967(6) 0.0390(15) Uani 1 1 d . . . . . N4 N 0.4092(4) 0.31440(16) 0.3737(6) 0.0381(15) Uani 1 1 d . . . . . N1 N 0.4781(4) 0.41855(16) 0.1460(6) 0.0356(14) Uani 1 1 d . . . . . N3 N 0.5168(4) 0.30808(16) 0.5377(6) 0.0385(15) Uani 1 1 d . . . . . C12 C 0.6358(4) 0.45594(18) 0.5118(7) 0.0280(15) Uani 1 1 d . . . . . C13 C 0.6801(4) 0.48040(18) 0.4285(7) 0.0287(15) Uani 1 1 d . . . . . C2 C 0.6284(4) 0.57881(19) 0.3402(7) 0.0291(16) Uani 1 1 d . . . . . C1 C 0.6751(4) 0.54425(19) 0.3353(6) 0.0291(15) Uani 1 1 d . . . . . C11 C 0.6895(4) 0.43199(19) 0.6041(7) 0.0314(16) Uani 1 1 d . . . . . H11 H 0.661867 0.415525 0.664374 0.038 Uiso 1 1 calc R U . . . C6 C 0.7641(4) 0.5439(2) 0.3179(7) 0.0301(16) Uani 1 1 d . . . . . C9 C 0.8205(4) 0.4541(2) 0.5180(7) 0.0347(17) Uani 1 1 d . . . . . H9 H 0.882458 0.452857 0.517186 0.042 Uiso 1 1 calc R U . . . C3 C 0.6752(4) 0.6138(2) 0.3229(6) 0.0324(16) Uani 1 1 d . . . . . H3 H 0.644381 0.637959 0.324787 0.039 Uiso 1 1 calc R U . . . C24 C 0.5223(4) 0.39757(19) 0.2527(7) 0.0341(17) Uani 1 1 d . . . . . C33 C 0.4739(4) 0.33563(19) 0.4511(7) 0.0327(17) Uani 1 1 d . . . . . C4 C 0.7623(4) 0.6152(2) 0.3033(7) 0.0331(16) Uani 1 1 d . . . . . C8 C 0.7712(4) 0.47875(19) 0.4255(7) 0.0306(16) Uani 1 1 d . . . . . C5 C 0.8063(5) 0.5789(2) 0.3027(7) 0.0341(17) Uani 1 1 d . . . . . H5 H 0.867086 0.578680 0.291459 0.041 Uiso 1 1 calc R U . . . C14 C 0.8137(4) 0.6532(2) 0.2839(8) 0.0371(18) Uani 1 1 d . . . . . C7 C 0.8075(4) 0.50358(19) 0.3148(7) 0.0316(16) Uani 1 1 d . . . . . C10 C 0.7824(4) 0.43087(19) 0.6129(7) 0.0344(17) Uani 1 1 d . . . . . C30 C 0.6607(5) 0.35843(19) 0.2730(8) 0.0397(18) Uani 1 1 d . . . . . H30 H 0.651204 0.359136 0.372537 0.048 Uiso 1 1 calc R U . . . C29 C 0.4138(5) 0.4848(2) 0.1379(8) 0.049(2) Uani 1 1 d . . . . . H29A H 0.462949 0.493545 0.205400 0.074 Uiso 1 1 calc R U . . . H29B H 0.360458 0.499398 0.152164 0.074 Uiso 1 1 calc R U . . . H29C H 0.427889 0.489748 0.044102 0.074 Uiso 1 1 calc R U . . . C26 C 0.5927(6) 0.3952(2) 0.0600(8) 0.050(2) Uani 1 1 d . . . . . H26 H 0.634568 0.388597 -0.000265 0.059 Uiso 1 1 calc R U . . . C25 C 0.5218(6) 0.4172(2) 0.0299(8) 0.047(2) Uani 1 1 d . . . . . H25 H 0.503895 0.429899 -0.055951 0.056 Uiso 1 1 calc R U . . . C34 C 0.4114(5) 0.2752(2) 0.4109(9) 0.052(2) Uani 1 1 d . . . . . H34 H 0.372970 0.255098 0.371804 0.063 Uiso 1 1 calc R U . . . C36 C 0.3488(5) 0.3309(2) 0.2612(8) 0.045(2) Uani 1 1 d . . . . . H36 H 0.355437 0.360124 0.264614 0.054 Uiso 1 1 calc R U . . . C39 C 0.5898(5) 0.3171(2) 0.6444(8) 0.047(2) Uani 1 1 d . . . . . H39 H 0.605351 0.345453 0.635524 0.056 Uiso 1 1 calc R U . . . C27 C 0.3985(5) 0.4414(2) 0.1563(8) 0.0407(18) Uani 1 1 d . . . . . H27 H 0.381288 0.437293 0.250815 0.049 Uiso 1 1 calc R U . . . C19 C 0.9091(4) 0.5060(2) 0.3370(8) 0.0439(19) Uani 1 1 d . . . . . H19A H 0.929511 0.520943 0.261352 0.066 Uiso 1 1 calc R U . . . H19B H 0.933864 0.479400 0.338668 0.066 Uiso 1 1 calc R U . . . H19C H 0.928539 0.519075 0.425184 0.066 Uiso 1 1 calc R U . . . C16 C 0.8899(5) 0.6575(2) 0.4019(8) 0.050(2) Uani 1 1 d . . . . . H16A H 0.866014 0.659895 0.490152 0.075 Uiso 1 1 calc R U . . . H16B H 0.924244 0.680978 0.386507 0.075 Uiso 1 1 calc R U . . . H16C H 0.927933 0.634271 0.404400 0.075 Uiso 1 1 calc R U . . . C15 C 0.8528(5) 0.6515(2) 0.1466(8) 0.048(2) Uani 1 1 d . . . . . H15A H 0.895356 0.629911 0.149603 0.073 Uiso 1 1 calc R U . . . H15B H 0.882518 0.676358 0.132051 0.073 Uiso 1 1 calc R U . . . H15C H 0.805446 0.647134 0.070443 0.073 Uiso 1 1 calc R U . . . C35 C 0.4789(5) 0.2711(2) 0.5142(9) 0.052(2) Uani 1 1 d . . . . . H35 H 0.497017 0.247531 0.561568 0.062 Uiso 1 1 calc R U . . . C18 C 0.7807(5) 0.4839(2) 0.1715(7) 0.0457(19) Uani 1 1 d . . . . . H18A H 0.716900 0.479435 0.157839 0.068 Uiso 1 1 calc R U . . . H18B H 0.811444 0.458785 0.168136 0.068 Uiso 1 1 calc R U . . . H18C H 0.796758 0.501206 0.098353 0.068 Uiso 1 1 calc R U . . . C20 C 0.8365(5) 0.4051(2) 0.7166(8) 0.045(2) Uani 1 1 d . . . . . C28 C 0.3227(5) 0.4262(2) 0.0499(9) 0.055(2) Uani 1 1 d . . . . . H28A H 0.338277 0.429776 -0.043717 0.083 Uiso 1 1 calc R U . . . H28B H 0.268847 0.440964 0.059530 0.083 Uiso 1 1 calc R U . . . H28C H 0.312880 0.398269 0.066386 0.083 Uiso 1 1 calc R U . . . C17 C 0.7545(5) 0.6894(2) 0.2813(9) 0.051(2) Uani 1 1 d . . . . . H17A H 0.705451 0.686655 0.206772 0.077 Uiso 1 1 calc R U . . . H17B H 0.788762 0.712866 0.265222 0.077 Uiso 1 1 calc R U . . . H17C H 0.731409 0.691776 0.370090 0.077 Uiso 1 1 calc R U . . . C41 C 0.6709(5) 0.2924(2) 0.6229(9) 0.060(2) Uani 1 1 d . . . . . H41A H 0.657209 0.264518 0.631901 0.091 Uiso 1 1 calc R U . . . H41B H 0.720216 0.299593 0.692644 0.091 Uiso 1 1 calc R U . . . H41C H 0.686985 0.297452 0.530349 0.091 Uiso 1 1 calc R U . . . C38 C 0.3731(6) 0.3168(3) 0.1224(8) 0.067(3) Uani 1 1 d . . . . . H38A H 0.436635 0.319929 0.120987 0.101 Uiso 1 1 calc R U . . . H38B H 0.341071 0.332339 0.047652 0.101 Uiso 1 1 calc R U . . . H38C H 0.357239 0.289035 0.109485 0.101 Uiso 1 1 calc R U . . . C31 C 0.7534(5) 0.3737(2) 0.2637(9) 0.057(2) Uani 1 1 d . . . . . H31A H 0.764685 0.373349 0.167022 0.085 Uiso 1 1 calc R U . . . H31B H 0.796395 0.356853 0.318967 0.085 Uiso 1 1 calc R U . . . H31C H 0.758684 0.400600 0.299233 0.085 Uiso 1 1 calc R U . . . C32 C 0.6482(5) 0.3155(2) 0.2229(9) 0.055(2) Uani 1 1 d . . . . . H32A H 0.590768 0.305888 0.242776 0.083 Uiso 1 1 calc R U . . . H32B H 0.695001 0.299148 0.271212 0.083 Uiso 1 1 calc R U . . . H32C H 0.650753 0.314355 0.123104 0.083 Uiso 1 1 calc R U . . . C37 C 0.2551(5) 0.3214(3) 0.2775(10) 0.074(3) Uani 1 1 d . . . . . H37A H 0.245755 0.292998 0.267530 0.112 Uiso 1 1 calc R U . . . H37B H 0.215602 0.335174 0.206353 0.112 Uiso 1 1 calc R U . . . H37C H 0.242754 0.329714 0.369285 0.112 Uiso 1 1 calc R U . . . C21 C 0.7878(5) 0.3896(3) 0.8291(9) 0.065(3) Uani 1 1 d . . . . . H21A H 0.764364 0.411565 0.878020 0.098 Uiso 1 1 calc R U . . . H21B H 0.828082 0.374137 0.894325 0.098 Uiso 1 1 calc R U . . . H21C H 0.739097 0.372870 0.788501 0.098 Uiso 1 1 calc R U . . . C40 C 0.5632(6) 0.3108(3) 0.7873(8) 0.066(3) Uani 1 1 d . . . . . H40A H 0.512002 0.327268 0.798360 0.100 Uiso 1 1 calc R U . . . H40B H 0.612317 0.318022 0.857381 0.100 Uiso 1 1 calc R U . . . H40C H 0.548084 0.283160 0.798477 0.100 Uiso 1 1 calc R U . . . C22 C 0.8660(7) 0.3683(3) 0.6384(10) 0.088(3) Uani 1 1 d . . . . . H22A H 0.813818 0.353775 0.597439 0.132 Uiso 1 1 calc R U . . . H22B H 0.902509 0.351324 0.703614 0.132 Uiso 1 1 calc R U . . . H22C H 0.900075 0.376764 0.565151 0.132 Uiso 1 1 calc R U . . . C23 C 0.9190(6) 0.4261(3) 0.7782(11) 0.096(4) Uani 1 1 d . . . . . H23A H 0.953480 0.433679 0.704343 0.144 Uiso 1 1 calc R U . . . H23B H 0.954244 0.408630 0.843390 0.144 Uiso 1 1 calc R U . . . H23C H 0.903041 0.449674 0.827097 0.144 Uiso 1 1 calc R U . . . C43 C 0.9315(8) 0.5517(4) 0.8801(12) 0.101(4) Uani 1 1 d . . . . . H43A H 0.901948 0.556776 0.962978 0.121 Uiso 1 1 calc R U . . . H43B H 0.977398 0.531490 0.903831 0.121 Uiso 1 1 calc R U . . . C42 C 0.9708(10) 0.5873(4) 0.8373(14) 0.112(4) Uani 1 1 d . . . . . H42A H 0.969027 0.607983 0.908115 0.135 Uiso 1 1 calc R U . . . H42B H 1.033074 0.582575 0.824165 0.135 Uiso 1 1 calc R U . . . C45 C 0.8455(11) 0.5758(4) 0.6882(13) 0.115(4) Uani 1 1 d . . . . . H45A H 0.830593 0.571649 0.587428 0.138 Uiso 1 1 calc R U . . . H45B H 0.795594 0.589325 0.723393 0.138 Uiso 1 1 calc R U . . . C44 C 0.8643(9) 0.5373(4) 0.7613(15) 0.121(5) Uani 1 1 d . . . . . H44A H 0.890030 0.517816 0.702473 0.145 Uiso 1 1 calc R U . . . H44B H 0.811165 0.526098 0.794665 0.145 Uiso 1 1 calc R U . . . O2 O 0.9235(12) 0.5984(5) 0.716(2) 0.326(13) 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 0.0341(5) 0.0270(4) 0.0264(5) 0.0003(4) 0.0054(4) -0.0008(4) P1 0.0285(9) 0.0269(9) 0.0276(10) -0.0006(8) 0.0067(7) -0.0008(8) P2 0.0284(9) 0.0300(10) 0.0275(10) 0.0005(8) 0.0070(8) 0.0007(8) O1 0.023(2) 0.030(2) 0.036(3) 0.003(2) 0.009(2) 0.001(2) N2 0.048(4) 0.033(3) 0.039(4) 0.002(3) 0.015(3) 0.001(3) N4 0.046(4) 0.027(3) 0.040(4) 0.004(3) -0.001(3) 0.003(3) N1 0.047(4) 0.037(3) 0.023(3) 0.000(3) 0.006(3) 0.003(3) N3 0.043(4) 0.032(3) 0.039(4) 0.003(3) 0.001(3) 0.000(3) C12 0.030(4) 0.021(3) 0.033(4) 0.001(3) 0.008(3) 0.002(3) C13 0.030(4) 0.028(4) 0.029(4) 0.004(3) 0.008(3) 0.001(3) C2 0.037(4) 0.030(4) 0.022(4) -0.003(3) 0.011(3) -0.001(3) C1 0.033(4) 0.032(4) 0.023(4) 0.001(3) 0.006(3) -0.009(3) C11 0.036(4) 0.031(4) 0.030(4) 0.001(3) 0.011(3) -0.001(3) C6 0.024(4) 0.037(4) 0.030(4) 0.006(3) 0.007(3) 0.007(3) C9 0.021(3) 0.041(4) 0.042(4) 0.007(4) 0.006(3) 0.002(3) C3 0.035(4) 0.038(4) 0.026(4) 0.003(3) 0.010(3) 0.006(3) C24 0.040(4) 0.029(4) 0.034(4) -0.003(3) 0.009(3) -0.003(3) C33 0.041(4) 0.031(4) 0.027(4) -0.009(3) 0.011(3) -0.001(3) C4 0.029(4) 0.039(4) 0.031(4) 0.003(3) 0.006(3) -0.001(3) C8 0.032(4) 0.033(4) 0.028(4) -0.001(3) 0.010(3) -0.006(3) C5 0.032(4) 0.039(4) 0.033(4) 0.005(3) 0.009(3) -0.005(3) C14 0.035(4) 0.035(4) 0.043(5) 0.003(3) 0.010(3) -0.015(3) C7 0.027(4) 0.031(4) 0.039(4) 0.005(3) 0.013(3) 0.001(3) C10 0.033(4) 0.036(4) 0.036(4) 0.007(3) 0.009(3) -0.003(3) C30 0.048(5) 0.031(4) 0.040(5) -0.002(3) 0.006(4) 0.004(4) C29 0.057(5) 0.043(4) 0.045(5) -0.001(4) -0.002(4) 0.000(4) C26 0.072(6) 0.051(5) 0.030(4) 0.001(4) 0.026(4) -0.002(5) C25 0.073(6) 0.041(4) 0.028(5) 0.002(4) 0.013(4) 0.007(4) C34 0.053(5) 0.034(4) 0.066(6) 0.011(4) -0.005(4) -0.009(4) C36 0.051(5) 0.032(4) 0.051(5) -0.007(4) -0.001(4) -0.003(4) C39 0.055(5) 0.034(4) 0.048(5) 0.011(4) -0.007(4) 0.000(4) C27 0.048(5) 0.042(4) 0.031(4) 0.001(4) 0.000(3) 0.003(4) C19 0.031(4) 0.051(5) 0.053(5) 0.012(4) 0.017(3) 0.001(4) C16 0.038(4) 0.052(5) 0.058(5) -0.003(4) 0.002(4) -0.011(4) C15 0.044(4) 0.049(5) 0.056(5) 0.007(4) 0.019(4) -0.012(4) C35 0.064(5) 0.018(4) 0.071(6) 0.006(4) 0.000(5) -0.008(4) C18 0.050(5) 0.050(5) 0.040(5) 0.001(4) 0.018(4) 0.009(4) C20 0.032(4) 0.050(5) 0.052(5) 0.027(4) 0.002(4) 0.000(4) C28 0.058(5) 0.050(5) 0.053(6) 0.006(4) -0.010(4) -0.011(4) C17 0.049(5) 0.037(4) 0.070(6) 0.004(4) 0.015(4) -0.006(4) C41 0.057(5) 0.040(5) 0.080(7) 0.007(4) -0.006(5) 0.006(4) C38 0.078(6) 0.079(6) 0.042(5) -0.017(5) -0.006(5) 0.022(5) C31 0.046(5) 0.061(5) 0.065(6) -0.006(5) 0.016(4) -0.002(4) C32 0.065(5) 0.041(5) 0.059(6) -0.004(4) 0.002(4) 0.002(4) C37 0.054(6) 0.082(7) 0.086(7) 0.028(6) 0.004(5) -0.002(5) C21 0.052(5) 0.087(6) 0.056(6) 0.037(5) -0.001(4) 0.011(5) C40 0.085(6) 0.069(6) 0.042(5) 0.006(5) -0.005(5) 0.000(5) C22 0.090(7) 0.094(7) 0.084(8) 0.047(6) 0.026(6) 0.051(6) C23 0.061(6) 0.105(8) 0.108(9) 0.073(7) -0.040(6) -0.030(6) C43 0.095(9) 0.129(11) 0.076(8) -0.026(8) 0.003(7) 0.027(8) C42 0.135(11) 0.118(11) 0.081(9) 0.006(8) 0.005(8) -0.007(10) C45 0.173(13) 0.092(9) 0.074(9) -0.008(7) -0.009(8) -0.034(10) C44 0.120(10) 0.101(10) 0.146(13) -0.041(10) 0.037(10) 0.029(9) O2 0.35(2) 0.242(16) 0.33(2) 0.205(16) -0.183(18) -0.131(16) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C24 Ni1 C33 105.0(3) . . ? C24 Ni1 P1 92.9(2) . . ? C33 Ni1 P1 162.1(2) . . ? C24 Ni1 P2 149.1(2) . 3_666 ? C33 Ni1 P2 105.7(2) . 3_666 ? P1 Ni1 P2 56.49(7) . 3_666 ? C12 P1 P2 100.2(2) . 3_666 ? C12 P1 Ni1 98.0(2) . . ? P2 P1 Ni1 62.32(7) 3_666 . ? C2 P2 P1 103.3(2) . 3_666 ? C2 P2 Ni1 104.3(2) . 3_666 ? P1 P2 Ni1 61.19(7) 3_666 3_666 ? C13 O1 C1 114.1(4) . . ? C24 N2 C26 111.4(6) . . ? C24 N2 C30 123.0(6) . . ? C26 N2 C30 125.5(6) . . ? C33 N4 C34 111.9(6) . . ? C33 N4 C36 123.7(5) . . ? C34 N4 C36 124.2(6) . . ? C24 N1 C25 111.1(6) . . ? C24 N1 C27 124.2(6) . . ? C25 N1 C27 124.5(6) . . ? C33 N3 C35 111.1(6) . . ? C33 N3 C39 123.9(5) . . ? C35 N3 C39 125.0(6) . . ? C13 C12 C11 115.6(6) . . ? C13 C12 P1 119.8(5) . . ? C11 C12 P1 124.5(5) . . ? C12 C13 C8 123.2(6) . . ? C12 C13 O1 118.0(5) . . ? C8 C13 O1 118.8(6) . . ? C1 C2 C3 116.2(6) . . ? C1 C2 P2 127.5(5) . . ? C3 C2 P2 116.0(5) . . ? C2 C1 C6 122.1(6) . . ? C2 C1 O1 118.4(5) . . ? C6 C1 O1 119.5(6) . . ? C12 C11 C10 123.9(6) . . ? C5 C6 C1 119.0(6) . . ? C5 C6 C7 124.6(6) . . ? C1 C6 C7 116.4(6) . . ? C8 C9 C10 122.4(6) . . ? C4 C3 C2 124.3(6) . . ? N1 C24 N2 103.0(6) . . ? N1 C24 Ni1 130.4(5) . . ? N2 C24 Ni1 126.6(5) . . ? N4 C33 N3 103.5(5) . . ? N4 C33 Ni1 127.3(5) . . ? N3 C33 Ni1 129.2(5) . . ? C3 C4 C5 116.5(6) . . ? C3 C4 C14 124.5(6) . . ? C5 C4 C14 119.0(6) . . ? C9 C8 C13 118.1(6) . . ? C9 C8 C7 125.4(6) . . ? C13 C8 C7 116.4(6) . . ? C6 C5 C4 122.0(6) . . ? C17 C14 C15 108.2(6) . . ? C17 C14 C16 109.1(6) . . ? C15 C14 C16 108.3(6) . . ? C17 C14 C4 111.6(5) . . ? C15 C14 C4 109.8(6) . . ? C16 C14 C4 109.8(6) . . ? C6 C7 C8 106.6(5) . . ? C6 C7 C19 112.5(6) . . ? C8 C7 C19 112.3(5) . . ? C6 C7 C18 109.8(5) . . ? C8 C7 C18 108.5(5) . . ? C19 C7 C18 107.1(5) . . ? C9 C10 C11 116.5(6) . . ? C9 C10 C20 122.2(6) . . ? C11 C10 C20 121.3(6) . . ? N2 C30 C31 111.5(6) . . ? N2 C30 C32 109.9(6) . . ? C31 C30 C32 112.5(6) . . ? C25 C26 N2 106.7(7) . . ? C26 C25 N1 107.8(7) . . ? C35 C34 N4 106.5(7) . . ? N4 C36 C37 111.2(6) . . ? N4 C36 C38 110.0(6) . . ? C37 C36 C38 111.8(7) . . ? N3 C39 C40 110.8(6) . . ? N3 C39 C41 110.2(6) . . ? C40 C39 C41 111.4(6) . . ? N1 C27 C29 111.7(6) . . ? N1 C27 C28 109.7(6) . . ? C29 C27 C28 111.3(6) . . ? C34 C35 N3 106.9(6) . . ? C21 C20 C10 114.5(6) . . ? C21 C20 C23 110.2(7) . . ? C10 C20 C23 110.7(6) . . ? C21 C20 C22 105.9(7) . . ? C10 C20 C22 107.9(7) . . ? C23 C20 C22 107.2(8) . . ? C42 C43 C44 108.5(12) . . ? O2 C42 C43 106.9(12) . . ? O2 C45 C44 106.2(12) . . ? C45 C44 C43 98.5(11) . . ? C42 O2 C45 110.9(12) . . ? 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 C24 1.895(7) . ? Ni1 C33 1.908(7) . ? Ni1 P1 2.2390(19) . ? Ni1 P2 2.263(2) 3_666 ? P1 C12 1.853(6) . ? P1 P2 2.131(3) 3_666 ? P2 C2 1.854(7) . ? O1 C13 1.400(7) . ? O1 C1 1.405(7) . ? N2 C24 1.374(8) . ? N2 C26 1.390(9) . ? N2 C30 1.457(8) . ? N4 C33 1.371(8) . ? N4 C34 1.382(9) . ? N4 C36 1.454(9) . ? N1 C24 1.367(8) . ? N1 C25 1.388(9) . ? N1 C27 1.459(9) . ? N3 C33 1.373(8) . ? N3 C35 1.392(8) . ? N3 C39 1.458(9) . ? C12 C13 1.398(8) . ? C12 C11 1.400(8) . ? C13 C8 1.400(9) . ? C2 C1 1.382(9) . ? C2 C3 1.412(9) . ? C1 C6 1.395(8) . ? C11 C10 1.414(9) . ? C6 C5 1.375(9) . ? C6 C7 1.525(9) . ? C9 C8 1.384(9) . ? C9 C10 1.399(9) . ? C3 C4 1.371(9) . ? C4 C5 1.406(9) . ? C4 C14 1.540(9) . ? C8 C7 1.530(9) . ? C14 C17 1.528(10) . ? C14 C15 1.535(10) . ? C14 C16 1.536(10) . ? C7 C19 1.545(9) . ? C7 C18 1.556(9) . ? C10 C20 1.504(9) . ? C30 C31 1.524(10) . ? C30 C32 1.544(10) . ? C29 C27 1.513(10) . ? C26 C25 1.321(10) . ? C34 C35 1.355(10) . ? C36 C37 1.498(10) . ? C36 C38 1.526(10) . ? C39 C40 1.515(11) . ? C39 C41 1.535(10) . ? C27 C28 1.542(10) . ? C20 C21 1.500(10) . ? C20 C23 1.507(11) . ? C20 C22 1.563(12) . ? C43 C42 1.438(16) . ? C43 C44 1.528(15) . ? C42 O2 1.360(15) . ? C45 O2 1.416(16) . ? C45 C44 1.504(16) . ?