#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:15:45 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242488 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132518.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_4132518 loop_ _publ_author_name 'Somerville, Rosie J.' 'Hale, Lillian V. A.' 'G\'omez-Bengoa, Enrique' 'Bur\'es, Jordi' 'Martin, Ruben' _publ_section_title ; Intermediacy of Ni-Ni Species in sp2 C-O Bond Cleavage of Aryl Esters: Relevance in Catalytic C-Si Bond Formation. ; _journal_issue 28 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 8771 _journal_page_last 8780 _journal_paper_doi 10.1021/jacs.8b04479 _journal_volume 140 _journal_year 2018 _chemical_formula_sum 'C56 H102 Ni2 O8 P2' _chemical_formula_weight 1082.73 _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 67.3623(9) _cell_angle_beta 76.2290(10) _cell_angle_gamma 70.3121(11) _cell_formula_units_Z 1 _cell_length_a 10.9948(5) _cell_length_b 11.8656(5) _cell_length_c 12.9686(6) _cell_measurement_reflns_used 9479 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 33.76 _cell_measurement_theta_min 2.78 _cell_volume 1458.77(11) _computing_cell_refinement 'Bruker APEX2 v2011.4-0' _computing_data_collection 'Bruker APEX2 v2011.4-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_solution Sir2011 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 512 _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.893 _diffrn_measurement_device_type 'APEX DUO Kappa 4-axis goniometer' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_measurement_specimen_support 'magnetic support with MicroMount' _diffrn_radiation_monochromator 'Quazar MX Multilayer Optics' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_unetI/netI 0.0319 _diffrn_reflns_Laue_measured_fraction_full 0.981 _diffrn_reflns_Laue_measured_fraction_max 0.893 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 19035 _diffrn_reflns_point_group_measured_fraction_full 0.981 _diffrn_reflns_point_group_measured_fraction_max 0.893 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.814 _diffrn_reflns_theta_min 1.715 _diffrn_source 'Microfocus source E025 IuS' _diffrn_source_current 0.6 _diffrn_source_power 50 _diffrn_source_size '0.2 mm x 0.2 mm fine focus' _diffrn_source_type 'Bruker APEX DUO' _exptl_absorpt_coefficient_mu 0.749 _exptl_absorpt_correction_T_max 0.865 _exptl_absorpt_correction_T_min 0.754 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.232 _exptl_crystal_description block _exptl_crystal_F_000 588 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.657 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.057 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 362 _refine_ls_number_reflns 10496 _refine_ls_number_restraints 189 _refine_ls_restrained_S_all 1.019 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_gt 0.0283 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+0.3119P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.0728 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9346 _reflns_number_total 10496 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b04479_si_002.cif _cod_data_source_block mo_RJS272_0m _cod_depositor_comments ; The following automatic conversions were performed: data item '_symmetry_cell_setting' value 'Triclinic' was changed to 'triclinic' in accordance with the /home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas ; _cod_original_sg_symbol_H-M P-1 _cod_database_code 4132518 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.754 _shelx_estimated_absorpt_t_max 0.865 _shelx_res_file ; mo_RJS272_0m.res created by SHELXL-2014/7 TITL mo_RJS272_0m in P-1 CELL 0.71073 10.99480 11.86560 12.96860 67.3623 76.2290 70.3121 ZERR 1.00 0.00050 0.00050 0.00060 0.0009 0.0010 0.0011 LATT 1 SFAC C H O P Ni UNIT 56 102 8 2 2 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! LIST 4 L.S. 20 ACTA CONF BOND $H FMAP 2 PLAN 20 SIZE 0.20 0.30 0.40 TEMP -173.170 SIMU 0.01 O1' > C23' DELU 0.01 O1' > C23' SIMU 0.01 O1 O2 C19 C20 C21 C22 C23 DELU 0.01 O1 O2 C19 C20 C21 C22 C23 ISOR 0.01 C19 > C23' WGHT 0.035100 0.311900 FVAR 0.19814 0.51733 MOLE 1 NI1 5 0.427405 0.464623 0.602520 11.00000 0.00849 0.00968 = 0.00839 -0.00282 -0.00105 -0.00259 P1 4 0.313194 0.377093 0.780863 11.00000 0.00839 0.00918 = 0.00882 -0.00289 -0.00110 -0.00221 PART 1 10.50 O1 3 0.565448 0.297993 0.618269 10.50000 0.01185 0.01376 = 0.01317 -0.00377 0.00619 0.00020 O2 3 0.684366 0.359632 0.452447 10.50000 0.01693 0.01706 = 0.01889 -0.00311 0.00746 0.00335 PART 0 O3 3 0.334629 0.420002 0.514495 11.00000 0.02185 0.03256 = 0.01170 -0.00803 -0.00120 -0.01618 O4 3 0.457616 0.470092 0.348399 11.00000 0.01855 0.02932 = 0.01571 -0.00989 0.00177 -0.01540 C1 1 0.212822 0.284401 0.770511 11.00000 0.01091 0.01077 = 0.01346 -0.00400 -0.00134 -0.00369 AFIX 13 H1 2 0.158514 0.342100 0.708575 11.00000 -1.20000 AFIX 0 C2 1 0.296577 0.169666 0.733922 11.00000 0.01570 0.01215 = 0.01653 -0.00626 -0.00103 -0.00437 AFIX 23 H2A 2 0.356251 0.198078 0.665052 11.00000 -1.20000 H2B 2 0.350002 0.107422 0.793996 11.00000 -1.20000 AFIX 0 C3 1 0.210371 0.106247 0.710708 11.00000 0.02299 0.01453 = 0.02069 -0.00678 -0.00519 -0.00692 AFIX 23 H3A 2 0.165269 0.165458 0.644513 11.00000 -1.20000 H3B 2 0.265900 0.029626 0.692290 11.00000 -1.20000 AFIX 0 C4 1 0.109187 0.068444 0.811162 11.00000 0.02087 0.01589 = 0.02797 -0.00593 -0.00350 -0.01010 AFIX 23 H4A 2 0.153765 -0.000232 0.874118 11.00000 -1.20000 H4B 2 0.050672 0.035434 0.789944 11.00000 -1.20000 AFIX 0 C5 1 0.028634 0.181214 0.849818 11.00000 0.01539 0.02057 = 0.03226 -0.00966 0.00062 -0.00972 AFIX 23 H5A 2 -0.031308 0.152516 0.918383 11.00000 -1.20000 H5B 2 -0.024480 0.245598 0.790324 11.00000 -1.20000 AFIX 0 C6 1 0.116995 0.240887 0.875000 11.00000 0.01526 0.01716 = 0.01990 -0.00757 0.00369 -0.00878 AFIX 23 H6A 2 0.166144 0.178096 0.937715 11.00000 -1.20000 H6B 2 0.063089 0.314572 0.898620 11.00000 -1.20000 AFIX 0 C7 1 0.414750 0.267301 0.895507 11.00000 0.01162 0.01268 = 0.01012 -0.00306 -0.00274 -0.00218 AFIX 13 H7 2 0.436346 0.180694 0.890145 11.00000 -1.20000 AFIX 0 C8 1 0.545299 0.296856 0.878267 11.00000 0.01128 0.02028 = 0.01219 -0.00253 -0.00264 -0.00438 AFIX 23 H8A 2 0.590750 0.297232 0.802477 11.00000 -1.20000 H8B 2 0.529009 0.382397 0.882411 11.00000 -1.20000 AFIX 0 C9 1 0.632185 0.198735 0.967476 11.00000 0.01351 0.02365 = 0.01562 -0.00442 -0.00532 -0.00173 AFIX 23 H9A 2 0.655222 0.114445 0.958746 11.00000 -1.20000 H9B 2 0.713814 0.222320 0.956126 11.00000 -1.20000 AFIX 0 C10 1 0.563693 0.190946 1.086019 11.00000 0.01765 0.01970 = 0.01345 -0.00373 -0.00580 -0.00278 AFIX 23 H10A 2 0.547165 0.273053 1.097198 11.00000 -1.20000 H10B 2 0.620253 0.124477 1.142040 11.00000 -1.20000 AFIX 0 C11 1 0.434809 0.159602 1.103625 11.00000 0.01970 0.01841 = 0.01116 0.00002 -0.00400 -0.00573 AFIX 23 H11A 2 0.452209 0.074374 1.098399 11.00000 -1.20000 H11B 2 0.389915 0.157684 1.179885 11.00000 -1.20000 AFIX 0 C12 1 0.346777 0.257564 1.015832 11.00000 0.01374 0.01795 = 0.01015 -0.00269 -0.00180 -0.00409 AFIX 23 H12A 2 0.323169 0.341489 1.025405 11.00000 -1.20000 H12B 2 0.265537 0.233202 1.027533 11.00000 -1.20000 AFIX 0 C13 1 0.195419 0.499676 0.836818 11.00000 0.01043 0.01199 = 0.01105 -0.00480 -0.00055 -0.00257 AFIX 13 H13 2 0.159642 0.456129 0.915346 11.00000 -1.20000 AFIX 0 C14 1 0.081178 0.573067 0.766580 11.00000 0.01087 0.01238 = 0.01475 -0.00546 -0.00272 -0.00209 AFIX 23 H14A 2 0.114658 0.614814 0.687738 11.00000 -1.20000 H14B 2 0.036605 0.513131 0.766646 11.00000 -1.20000 AFIX 0 C15 1 -0.015990 0.673407 0.814609 11.00000 0.01109 0.01431 = 0.02087 -0.00766 -0.00196 -0.00064 AFIX 23 H15A 2 -0.085840 0.722641 0.765547 11.00000 -1.20000 H15B 2 -0.056596 0.630532 0.890212 11.00000 -1.20000 AFIX 0 C16 1 0.048423 0.763941 0.823681 11.00000 0.01689 0.01310 = 0.02387 -0.00938 -0.00210 -0.00203 AFIX 23 H16A 2 -0.015977 0.822069 0.861267 11.00000 -1.20000 H16B 2 0.078011 0.815876 0.747211 11.00000 -1.20000 AFIX 0 C17 1 0.164750 0.691575 0.890475 11.00000 0.01679 0.01822 = 0.02350 -0.01369 -0.00193 -0.00375 AFIX 23 H17A 2 0.133442 0.649040 0.969790 11.00000 -1.20000 H17B 2 0.208777 0.752367 0.889498 11.00000 -1.20000 AFIX 0 C18 1 0.262620 0.591961 0.841539 11.00000 0.01232 0.01570 = 0.01849 -0.00935 -0.00169 -0.00396 AFIX 23 H18A 2 0.334215 0.543993 0.888905 11.00000 -1.20000 H18B 2 0.300623 0.634878 0.764772 11.00000 -1.20000 AFIX 0 EADP C21 C21' EADP C19 C19' EADP C20 C20' PART 1 10.50 C19 1 0.662850 0.279354 0.546666 10.50000 0.00989 0.01010 = 0.01279 -0.00355 -0.00039 -0.00223 C20 1 0.757455 0.145929 0.572782 10.50000 0.01268 0.01063 = 0.01864 -0.00167 0.00032 0.00011 C21 1 0.730248 0.065631 0.695710 10.50000 0.03190 0.01418 = 0.02479 0.00454 0.00580 0.00376 AFIX 137 H21A 2 0.640590 0.059505 0.711044 10.50000 -1.50000 H21B 2 0.741982 0.105477 0.744937 10.50000 -1.50000 H21C 2 0.790723 -0.019593 0.709996 10.50000 -1.50000 AFIX 0 C22 1 0.741122 0.083341 0.495843 10.50000 0.02723 0.01146 = 0.03686 -0.01138 -0.00154 -0.00363 AFIX 137 H22A 2 0.651577 0.077148 0.510151 10.50000 -1.50000 H22B 2 0.801685 -0.001885 0.510850 10.50000 -1.50000 H22C 2 0.759606 0.134536 0.417078 10.50000 -1.50000 AFIX 0 C23 1 0.896486 0.159197 0.549993 10.50000 0.01708 0.02089 = 0.03466 -0.00272 -0.00539 0.00563 AFIX 137 H23A 2 0.958599 0.074702 0.567846 10.50000 -1.50000 H23B 2 0.904263 0.203514 0.597142 10.50000 -1.50000 H23C 2 0.915287 0.207838 0.470456 10.50000 -1.50000 AFIX 0 PART 2 10.50 SAME 0.005 O1 O2 C19 C20 C21 C22 C23 O1' 3 0.574091 0.306551 0.610382 10.50000 0.01595 0.01103 = 0.01364 0.00245 0.00365 -0.00155 O2' 3 0.695286 0.354488 0.443659 10.50000 0.01293 0.00763 = 0.00979 0.00126 0.00507 0.00206 C19' 1 0.671030 0.280306 0.540746 10.50000 0.00989 0.01010 = 0.01279 -0.00355 -0.00039 -0.00223 C20' 1 0.767553 0.148558 0.577828 10.50000 0.01268 0.01063 = 0.01864 -0.00167 0.00032 0.00011 C21' 1 0.749088 0.084993 0.705531 10.50000 0.03190 0.01418 = 0.02479 0.00454 0.00580 0.00376 AFIX 137 H21D 2 0.803371 -0.003081 0.725613 10.50000 -1.50000 H21E 2 0.657439 0.086253 0.731196 10.50000 -1.50000 H21F 2 0.774611 0.131037 0.741696 10.50000 -1.50000 AFIX 0 C22' 1 0.906963 0.156959 0.539386 10.50000 0.00833 0.02122 = 0.02521 -0.00819 0.00048 -0.00085 AFIX 137 H22D 2 0.921011 0.217756 0.566284 10.50000 -1.50000 H22E 2 0.922781 0.185313 0.456950 10.50000 -1.50000 H22F 2 0.967012 0.073225 0.570131 10.50000 -1.50000 AFIX 0 C23' 1 0.737434 0.070451 0.520398 10.50000 0.03410 0.01698 = 0.05429 -0.01378 -0.00345 -0.00575 AFIX 137 H23D 2 0.746384 0.112881 0.438628 10.50000 -1.50000 H23E 2 0.648233 0.063413 0.547294 10.50000 -1.50000 H23F 2 0.798547 -0.014568 0.538782 10.50000 -1.50000 AFIX 0 PART 0 C24 1 0.364348 0.429922 0.412036 11.00000 0.01217 0.01074 = 0.01224 -0.00363 -0.00331 -0.00283 C25 1 0.283215 0.384397 0.363034 11.00000 0.01802 0.02125 = 0.01206 -0.00542 -0.00260 -0.01123 C26 1 0.345624 0.241297 0.388536 11.00000 0.04093 0.02086 = 0.02304 -0.00955 -0.00347 -0.01487 AFIX 137 H26A 2 0.435531 0.226575 0.351519 11.00000 -1.50000 H26B 2 0.295971 0.206811 0.360311 11.00000 -1.50000 H26C 2 0.345234 0.199101 0.470065 11.00000 -1.50000 AFIX 0 C27 1 0.286419 0.451276 0.235410 11.00000 0.02684 0.03285 = 0.01290 -0.00587 -0.00375 -0.01764 AFIX 137 H27A 2 0.251326 0.543157 0.219200 11.00000 -1.50000 H27B 2 0.233533 0.421038 0.206201 11.00000 -1.50000 H27C 2 0.376448 0.432385 0.199248 11.00000 -1.50000 AFIX 0 C28 1 0.142489 0.408906 0.419903 11.00000 0.01727 0.04313 = 0.01867 -0.00827 -0.00263 -0.01570 AFIX 137 H28A 2 0.141514 0.370199 0.501753 11.00000 -1.50000 H28B 2 0.093535 0.371624 0.393923 11.00000 -1.50000 H28C 2 0.102283 0.500592 0.400457 11.00000 -1.50000 REM ##### AFIX 0 HKLF 4 REM mo_RJS272_0m in P-1 REM R1 = 0.0283 for 9346 Fo > 4sig(Fo) and 0.0337 for all 10496 data REM 362 parameters refined using 189 restraints END WGHT 0.0351 0.3119 REM Highest difference peak 0.657, deepest hole -0.331, 1-sigma level 0.057 Q1 1 0.4082 0.5081 0.5500 11.00000 0.05 0.66 Q2 1 0.4538 0.4172 0.6539 11.00000 0.05 0.49 Q3 1 0.5973 0.2015 1.0234 11.00000 0.05 0.47 Q4 1 0.3620 0.4677 0.6234 11.00000 0.05 0.45 Q5 1 0.3226 0.4090 0.7169 11.00000 0.05 0.44 Q6 1 0.1664 0.2636 0.8259 11.00000 0.05 0.43 Q7 1 0.4712 0.4352 0.5603 11.00000 0.05 0.43 Q8 1 0.1558 0.0903 0.7538 11.00000 0.05 0.43 Q9 1 0.2606 0.2217 0.7516 11.00000 0.05 0.42 Q10 1 0.3448 0.3337 0.8385 11.00000 0.05 0.42 Q11 1 0.2958 0.4089 0.3010 11.00000 0.05 0.41 Q12 1 0.3796 0.2581 0.9500 11.00000 0.05 0.41 Q13 1 0.4782 0.2758 0.8880 11.00000 0.05 0.41 Q14 1 0.3229 0.4063 0.3900 11.00000 0.05 0.40 Q15 1 0.3848 0.2130 1.0634 11.00000 0.05 0.40 Q16 1 0.7097 0.2142 0.5530 11.00000 0.05 0.40 Q17 1 0.0325 0.6114 0.7987 11.00000 0.05 0.39 Q18 1 0.2160 0.6417 0.8710 11.00000 0.05 0.38 Q19 1 0.4060 0.4663 0.3810 11.00000 0.05 0.38 Q20 1 0.3396 0.4384 0.4632 11.00000 0.05 0.38 ; 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4 18 2.97 0.46 -5 -4 -18 5.77 0.43 5 4 18 5.14 0.60 -6 -4 -18 1.81 0.29 6 4 18 2.16 0.43 -7 -4 -18 4.07 0.39 7 4 18 4.18 0.57 8 4 18 8.03 0.76 9 4 18 11.17 0.82 4 -5 -18 1.45 0.31 3 -5 -18 4.38 0.50 3 -5 -18 4.56 0.46 2 -5 -18 3.96 0.45 2 -5 -18 4.89 0.46 1 -5 -18 0.78 0.24 1 -5 -18 0.82 0.27 0 -5 -18 0.22 0.20 0 -5 -18 0.09 0.18 0 5 18 -0.09 0.24 -1 -5 -18 0.85 0.22 -1 -5 -18 0.98 0.25 1 5 18 0.67 0.32 -2 -5 -18 2.30 0.30 2 5 18 1.97 0.39 -3 -5 -18 0.10 0.18 3 5 18 0.25 0.26 -4 -5 -18 10.93 0.54 4 5 18 10.48 0.77 -5 -5 -18 9.78 0.53 5 5 18 9.51 0.75 -6 -5 -18 0.16 0.19 6 5 18 0.15 0.25 -7 -5 -18 6.79 0.46 7 5 18 6.41 0.67 -8 -5 -18 5.00 0.43 8 5 18 5.49 0.63 9 5 18 14.15 0.90 10 5 18 1.14 0.38 3 -6 -18 0.94 0.29 3 -6 -18 1.92 0.49 2 -6 -18 1.68 0.34 1 -6 -18 1.56 0.33 0 -6 -18 2.73 0.36 0 6 18 3.31 0.49 -1 -6 -18 3.66 0.40 1 6 18 3.08 0.48 -2 -6 -18 12.91 0.63 2 6 18 13.36 0.83 -3 -6 -18 -0.04 0.17 3 6 18 -0.09 0.24 -4 -6 -18 8.18 0.49 4 6 18 8.20 0.69 -5 -6 -18 0.08 0.18 5 6 18 -0.07 0.23 -6 -6 -18 1.63 0.27 6 6 18 1.93 0.41 -7 -6 -18 6.04 0.44 7 6 18 6.74 0.69 -8 -6 -18 11.92 0.59 8 6 18 11.06 0.80 9 6 18 5.94 0.64 10 6 18 3.00 0.48 3 -7 -18 -0.08 0.21 2 -7 -18 0.86 0.28 1 -7 -18 4.19 0.46 0 -7 -18 1.81 0.31 0 7 18 1.20 0.33 -1 -7 -18 12.78 0.65 1 7 18 12.89 0.83 -2 -7 -18 26.09 0.92 2 7 18 25.50 1.16 -3 -7 -18 10.95 0.56 3 7 18 11.21 0.77 -4 -7 -18 0.60 0.22 4 7 18 0.64 0.31 -5 -7 -18 1.62 0.26 5 7 18 1.49 0.36 -6 -7 -18 7.71 0.47 6 7 18 7.32 0.65 -7 -7 -18 12.22 0.58 7 7 18 11.92 0.81 -8 -7 -18 12.30 0.59 8 7 18 12.88 0.84 -9 -7 -18 0.55 0.22 9 7 18 1.04 0.35 10 7 18 2.36 0.46 3 -8 -18 0.82 0.49 2 -8 -18 1.42 0.33 1 -8 -18 0.14 0.22 0 -8 -18 0.18 0.21 0 8 18 0.40 0.29 -1 -8 -18 3.80 0.41 1 8 18 2.79 0.45 -2 -8 -18 5.03 0.45 2 8 18 5.75 0.65 -3 -8 -18 8.26 0.51 3 8 18 8.93 0.72 -4 -8 -18 -0.11 0.15 4 8 18 -0.09 0.23 -5 -8 -18 2.05 0.29 5 8 18 1.94 0.40 -6 -8 -18 7.27 0.46 6 8 18 8.85 0.70 -7 -8 -18 4.04 0.37 7 8 18 4.71 0.55 -8 -8 -18 4.59 0.40 8 8 18 5.05 0.59 -9 -8 -18 1.18 0.27 9 8 18 1.00 0.33 10 8 18 0.18 0.27 11 8 18 -0.40 0.23 2 -9 -18 3.40 0.44 1 -9 -18 -0.20 0.18 0 -9 -18 0.26 0.23 0 9 18 -0.05 0.27 -1 -9 -18 1.62 0.31 1 9 18 1.07 0.36 -2 -9 -18 9.32 0.56 2 9 18 9.19 0.73 -3 -9 -18 0.81 0.24 3 9 18 0.67 0.31 -4 -9 -18 0.79 0.22 4 9 18 0.82 0.32 -5 -9 -18 2.19 0.29 5 9 18 2.14 0.42 -6 -9 -18 4.68 0.40 6 9 18 4.94 0.58 -7 -9 -18 5.13 0.43 7 9 18 4.65 0.58 -8 -9 -18 2.09 0.29 8 9 18 2.21 0.41 -9 -9 -18 -0.17 0.17 9 9 18 -0.17 0.24 -10 -9 -18 1.29 0.27 10 9 18 1.21 0.36 11 9 18 0.52 0.34 2 -10 -18 1.44 0.50 1 -10 -18 -0.09 0.21 0 -10 -18 6.65 0.58 0 10 18 5.60 0.67 -1 -10 -18 12.27 0.67 1 10 18 14.17 0.91 -2 -10 -18 14.61 0.71 2 10 18 17.96 0.99 -3 -10 -18 1.37 0.27 3 10 18 1.02 0.37 -4 -10 -18 6.54 0.46 4 10 18 5.97 0.65 -5 -10 -18 5.65 0.42 5 10 18 6.79 0.69 -6 -10 -18 7.94 0.49 6 10 18 8.35 0.70 -7 -10 -18 0.60 0.20 7 10 18 0.71 0.32 -8 -10 -18 4.12 0.38 8 10 18 4.37 0.55 -9 -10 -18 10.99 0.55 9 10 18 12.04 0.80 -10 -10 -18 3.22 0.35 10 10 18 3.03 0.49 -11 -10 -18 1.20 0.26 1 -11 -18 1.80 0.37 0 -11 -18 14.28 0.75 0 11 18 15.85 1.00 -1 -11 -18 10.91 0.64 1 11 18 12.57 0.90 -2 -11 -18 0.28 0.22 2 11 18 0.08 0.28 -3 -11 -18 1.65 0.31 3 11 18 1.99 0.45 -4 -11 -18 10.77 0.58 4 11 18 9.81 0.77 -5 -11 -18 6.06 0.45 5 11 18 4.48 0.58 -6 -11 -18 1.56 0.26 6 11 18 1.00 0.36 -7 -11 -18 0.89 0.23 7 11 18 1.73 0.40 -8 -11 -18 3.99 0.37 8 11 18 3.78 0.53 -9 -11 -18 4.65 0.40 9 11 18 5.38 0.61 -10 -11 -18 -0.15 0.17 10 11 18 0.00 0.24 0 -12 -18 11.14 0.67 0 12 18 11.14 0.90 -1 -12 -18 0.53 0.26 1 12 18 0.76 0.36 -2 -12 -18 0.28 0.22 2 12 18 0.03 0.30 -3 -12 -18 2.19 0.34 3 12 18 2.08 0.45 -4 -12 -18 18.40 0.77 4 12 18 18.46 1.06 -5 -12 -18 0.70 0.23 5 12 18 0.81 0.36 -6 -12 -18 0.22 0.19 6 12 18 0.03 0.27 -7 -12 -18 6.36 0.44 7 12 18 7.47 0.75 -8 -12 -18 0.04 0.17 8 12 18 0.21 0.28 -9 -12 -18 0.85 0.22 9 12 18 0.60 0.32 -10 -12 -18 2.72 0.33 -2 -13 -18 0.92 0.29 2 13 18 1.37 0.43 -3 -13 -18 1.95 0.34 3 13 18 2.54 0.52 -4 -13 -18 6.83 0.49 4 13 18 6.48 0.73 -5 -13 -18 1.73 0.31 5 13 18 1.59 0.43 -6 -13 -18 1.79 0.30 6 13 18 2.16 0.47 7 13 18 6.26 0.70 8 13 18 0.26 0.29 4 14 18 0.51 0.42 5 14 18 0.85 0.46 -1 -1 -19 23.15 0.88 -1 -1 -19 22.30 0.98 -2 -1 -19 12.54 0.64 -2 -1 -19 12.68 0.66 2 1 19 12.62 0.94 -3 -1 -19 0.07 0.20 -3 -1 -19 -0.30 0.19 3 1 19 0.03 0.27 -4 -1 -19 2.76 0.45 -4 -1 -19 3.55 0.40 4 1 19 3.04 0.53 0 -2 -19 12.31 0.67 0 -2 -19 9.73 0.59 -1 -2 -19 8.52 0.55 -1 -2 -19 10.02 0.60 -2 -2 -19 -0.02 0.19 -2 -2 -19 0.13 0.22 2 2 19 0.43 0.33 -3 -2 -19 4.55 0.45 -3 -2 -19 4.01 0.40 3 2 19 3.63 0.55 -4 -2 -19 5.71 0.50 -4 -2 -19 5.91 0.44 4 2 19 6.93 0.71 -5 -2 -19 3.10 0.35 -5 -2 -19 2.38 0.35 5 2 19 3.38 0.58 -6 -2 -19 2.14 0.39 6 2 19 2.43 0.50 1 -3 -19 11.98 0.76 1 -3 -19 11.02 0.62 0 -3 -19 9.25 0.57 0 -3 -19 7.65 0.56 -1 -3 -19 2.79 0.35 -1 -3 -19 2.88 0.38 -2 -3 -19 6.88 0.48 -2 -3 -19 7.62 0.52 2 3 19 9.00 0.75 -3 -3 -19 12.04 0.65 -3 -3 -19 12.72 0.60 3 3 19 14.38 0.91 -4 -3 -19 14.64 0.68 -4 -3 -19 15.94 0.71 4 3 19 16.37 0.98 -5 -3 -19 3.61 0.40 5 3 19 2.74 0.50 -6 -3 -19 0.03 0.21 6 3 19 -0.06 0.27 7 3 19 0.56 0.38 1 -4 -19 12.94 0.72 1 -4 -19 12.88 0.67 0 -4 -19 10.77 0.58 0 -4 -19 9.64 0.61 -1 -4 -19 -0.05 0.18 -1 -4 -19 0.16 0.21 1 4 19 0.11 0.27 -2 -4 -19 28.20 1.01 2 4 19 30.68 1.30 -3 -4 -19 7.05 0.50 3 4 19 6.21 0.69 -4 -4 -19 1.74 0.31 4 4 19 1.72 0.43 -5 -4 -19 -0.30 0.17 5 4 19 0.25 0.29 -6 -4 -19 4.76 0.44 6 4 19 6.51 0.71 -7 -4 -19 5.45 0.48 7 4 19 5.53 0.64 2 -5 -19 16.37 1.11 1 -5 -19 12.53 0.70 0 -5 -19 0.69 0.27 -1 -5 -19 10.28 0.60 1 5 19 9.33 0.75 -2 -5 -19 19.70 0.82 2 5 19 20.92 1.06 -3 -5 -19 2.21 0.32 3 5 19 3.95 0.57 -4 -5 -19 0.84 0.26 4 5 19 1.19 0.39 -5 -5 -19 2.21 0.33 5 5 19 1.91 0.43 -6 -5 -19 20.16 0.78 6 5 19 18.54 1.05 -7 -5 -19 3.64 0.40 7 5 19 4.65 0.61 -8 -5 -19 2.95 0.38 8 5 19 3.64 0.56 1 -6 -19 13.57 0.74 0 -6 -19 0.99 0.29 -1 -6 -19 6.81 0.52 1 6 19 7.94 0.77 -2 -6 -19 1.38 0.29 2 6 19 0.95 0.36 -3 -6 -19 0.55 0.22 3 6 19 0.60 0.32 -4 -6 -19 0.98 0.26 4 6 19 0.79 0.34 -5 -6 -19 15.82 0.70 5 6 19 17.09 0.98 -6 -6 -19 6.22 0.46 6 6 19 6.23 0.68 -7 -6 -19 1.57 0.29 7 6 19 1.58 0.40 -8 -6 -19 15.70 0.70 8 6 19 16.19 0.98 1 -7 -19 2.17 0.39 0 -7 -19 0.34 0.24 -1 -7 -19 0.35 0.23 1 7 19 0.44 0.33 -2 -7 -19 0.27 0.20 2 7 19 0.10 0.28 -3 -7 -19 3.31 0.38 3 7 19 3.99 0.58 -4 -7 -19 3.06 0.36 4 7 19 3.10 0.52 -5 -7 -19 4.86 0.44 5 7 19 5.27 0.64 -6 -7 -19 1.50 0.30 6 7 19 2.55 0.47 -7 -7 -19 0.04 0.19 7 7 19 0.13 0.27 -8 -7 -19 12.07 0.60 8 7 19 12.26 0.87 -9 -7 -19 2.98 0.37 9 7 19 3.56 0.70 1 -8 -19 0.54 0.43 0 -8 -19 9.64 0.63 -1 -8 -19 8.84 0.58 1 8 19 6.50 0.68 -2 -8 -19 5.76 0.49 2 8 19 5.43 0.65 -3 -8 -19 9.18 0.56 3 8 19 10.87 0.81 -4 -8 -19 8.52 0.52 4 8 19 8.71 0.74 -5 -8 -19 0.07 0.19 5 8 19 -0.10 0.25 -6 -8 -19 2.51 0.32 6 8 19 2.35 0.44 -7 -8 -19 5.60 0.44 7 8 19 6.38 0.68 -8 -8 -19 6.32 0.46 8 8 19 6.38 0.68 -9 -8 -19 2.37 0.34 9 8 19 2.10 0.47 0 -9 -19 19.71 0.90 -1 -9 -19 3.66 0.43 1 9 19 3.08 0.52 -2 -9 -19 3.75 0.43 2 9 19 3.84 0.55 -3 -9 -19 12.18 0.64 3 9 19 12.51 0.85 -4 -9 -19 8.45 0.53 4 9 19 10.19 0.79 -5 -9 -19 -0.07 0.18 5 9 19 0.11 0.28 -6 -9 -19 3.42 0.37 6 9 19 3.83 0.56 -7 -9 -19 14.80 0.66 7 9 19 15.99 0.95 -8 -9 -19 5.71 0.44 8 9 19 5.74 0.63 -9 -9 -19 -0.01 0.19 9 9 19 -0.02 0.27 0 -10 -19 3.13 0.56 -1 -10 -19 0.82 0.29 1 10 19 0.74 0.37 -2 -10 -19 0.15 0.22 2 10 19 0.66 0.33 -3 -10 -19 11.98 0.64 3 10 19 13.64 0.90 -4 -10 -19 1.13 0.27 4 10 19 1.26 0.41 -5 -10 -19 2.80 0.35 5 10 19 2.10 0.44 -6 -10 -19 -0.10 0.18 6 10 19 -0.26 0.22 -7 -10 -19 7.55 0.48 7 10 19 6.12 0.67 -8 -10 -19 -0.05 0.19 8 10 19 0.76 0.34 -9 -10 -19 0.18 0.21 -2 -11 -19 0.93 0.29 2 11 19 1.35 0.41 -3 -11 -19 4.79 0.46 3 11 19 4.20 0.60 -4 -11 -19 0.24 0.20 4 11 19 0.46 0.34 -5 -11 -19 2.04 0.31 5 11 19 1.73 0.42 -6 -11 -19 2.07 0.30 6 11 19 1.60 0.41 -7 -11 -19 1.21 0.25 7 11 19 1.46 0.40 -8 -11 -19 0.14 0.19 8 11 19 0.35 0.36 -3 -12 -19 3.67 0.42 3 12 19 4.08 0.60 -4 -12 -19 1.23 0.29 4 12 19 1.31 0.40 -5 -12 -19 13.09 0.65 5 12 19 14.34 0.95 -6 -12 -19 4.13 0.41 6 12 19 4.23 0.60 -7 -12 -19 2.61 0.34 2 5 20 1.43 0.39 3 5 20 21.01 1.11 4 5 20 14.28 0.94 5 5 20 2.93 0.52 2 6 20 2.49 0.50 -3 -6 -20 3.58 0.47 3 6 20 3.68 0.55 -4 -6 -20 5.73 0.57 4 6 20 5.80 0.68 -5 -6 -20 2.72 0.56 5 6 20 2.25 0.46 6 6 20 2.95 0.58 2 7 20 4.91 0.60 -3 -7 -20 2.40 0.41 3 7 20 3.45 0.56 -4 -7 -20 3.46 0.41 4 7 20 4.23 0.61 -5 -7 -20 1.21 0.33 5 7 20 1.71 0.45 6 7 20 1.48 0.44 2 8 20 0.61 0.33 -3 -8 -20 3.29 0.45 3 8 20 2.20 0.47 -4 -8 -20 5.12 0.47 4 8 20 4.80 0.63 -5 -8 -20 2.71 0.37 5 8 20 3.15 0.53 -6 -8 -20 4.60 0.49 6 8 20 4.30 0.68 -3 -9 -20 1.44 0.48 3 9 20 1.40 0.42 -4 -9 -20 9.93 0.60 4 9 20 11.13 0.85 -5 -9 -20 8.12 0.53 5 9 20 6.44 0.70 -6 -9 -20 2.91 0.42 6 9 20 3.25 0.78 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 18917 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 0.42741(2) 0.46462(2) 0.60252(2) 0.00889(3) Uani 1 1 d . . . . . P1 P 0.31319(2) 0.37709(2) 0.78086(2) 0.00888(5) Uani 1 1 d . . . . . O1 O 0.5654(14) 0.2980(12) 0.6183(11) 0.0156(12) Uani 0.5 1 d D U P A 1 O2 O 0.6844(13) 0.3596(9) 0.4524(9) 0.0225(17) Uani 0.5 1 d D U P A 1 O3 O 0.33463(8) 0.42000(8) 0.51450(6) 0.01963(16) Uani 1 1 d . . . . . O4 O 0.45762(8) 0.47009(8) 0.34840(6) 0.01877(15) Uani 1 1 d . . . . . C1 C 0.21282(9) 0.28440(9) 0.77051(7) 0.01156(16) Uani 1 1 d . . . . . H1 H 0.1585 0.3421 0.7086 0.014 Uiso 1 1 calc R U . . . C2 C 0.29658(10) 0.16967(10) 0.73392(8) 0.01436(17) Uani 1 1 d . . . . . H2A H 0.3563 0.1981 0.6651 0.017 Uiso 1 1 calc R U . . . H2B H 0.3500 0.1074 0.7940 0.017 Uiso 1 1 calc R U . . . C3 C 0.21037(11) 0.10625(10) 0.71071(8) 0.01818(19) Uani 1 1 d . . . . . H3A H 0.1653 0.1655 0.6445 0.022 Uiso 1 1 calc R U . . . H3B H 0.2659 0.0296 0.6923 0.022 Uiso 1 1 calc R U . . . C4 C 0.10919(11) 0.06844(11) 0.81116(9) 0.0206(2) Uani 1 1 d . . . . . H4A H 0.1538 -0.0002 0.8741 0.025 Uiso 1 1 calc R U . . . H4B H 0.0507 0.0354 0.7899 0.025 Uiso 1 1 calc R U . . . C5 C 0.02863(11) 0.18121(11) 0.84982(10) 0.0218(2) Uani 1 1 d . . . . . H5A H -0.0313 0.1525 0.9184 0.026 Uiso 1 1 calc R U . . . H5B H -0.0245 0.2456 0.7903 0.026 Uiso 1 1 calc R U . . . C6 C 0.11700(10) 0.24089(10) 0.87500(8) 0.01691(18) Uani 1 1 d . . . . . H6A H 0.1661 0.1781 0.9377 0.020 Uiso 1 1 calc R U . . . H6B H 0.0631 0.3146 0.8986 0.020 Uiso 1 1 calc R U . . . C7 C 0.41475(9) 0.26730(9) 0.89551(7) 0.01176(16) Uani 1 1 d . . . . . H7 H 0.4363 0.1807 0.8901 0.014 Uiso 1 1 calc R U . . . C8 C 0.54530(9) 0.29686(10) 0.87827(7) 0.01526(18) Uani 1 1 d . . . . . H8A H 0.5907 0.2972 0.8025 0.018 Uiso 1 1 calc R U . . . H8B H 0.5290 0.3824 0.8824 0.018 Uiso 1 1 calc R U . . . C9 C 0.63219(10) 0.19873(11) 0.96748(8) 0.0185(2) Uani 1 1 d . . . . . H9A H 0.6552 0.1144 0.9587 0.022 Uiso 1 1 calc R U . . . H9B H 0.7138 0.2223 0.9561 0.022 Uiso 1 1 calc R U . . . C10 C 0.56369(10) 0.19095(11) 1.08602(8) 0.01742(19) Uani 1 1 d . . . . . H10A H 0.5472 0.2731 1.0972 0.021 Uiso 1 1 calc R U . . . H10B H 0.6203 0.1245 1.1420 0.021 Uiso 1 1 calc R U . . . C11 C 0.43481(10) 0.15960(10) 1.10362(8) 0.01746(19) Uani 1 1 d . . . . . H11A H 0.4522 0.0744 1.0984 0.021 Uiso 1 1 calc R U . . . H11B H 0.3899 0.1577 1.1799 0.021 Uiso 1 1 calc R U . . . C12 C 0.34678(9) 0.25756(10) 1.01583(7) 0.01459(17) Uani 1 1 d . . . . . H12A H 0.3232 0.3415 1.0254 0.018 Uiso 1 1 calc R U . . . H12B H 0.2655 0.2332 1.0275 0.018 Uiso 1 1 calc R U . . . C13 C 0.19542(9) 0.49968(9) 0.83682(7) 0.01113(16) Uani 1 1 d . . . . . H13 H 0.1596 0.4561 0.9153 0.013 Uiso 1 1 calc R U . . . C14 C 0.08118(9) 0.57307(9) 0.76658(7) 0.01246(16) Uani 1 1 d . . . . . H14A H 0.1147 0.6148 0.6877 0.015 Uiso 1 1 calc R U . . . H14B H 0.0366 0.5131 0.7666 0.015 Uiso 1 1 calc R U . . . C15 C -0.01599(9) 0.67341(10) 0.81461(8) 0.01563(18) Uani 1 1 d . . . . . H15A H -0.0858 0.7226 0.7655 0.019 Uiso 1 1 calc R U . . . H15B H -0.0566 0.6305 0.8902 0.019 Uiso 1 1 calc R U . . . C16 C 0.04842(10) 0.76394(10) 0.82368(9) 0.01758(19) Uani 1 1 d . . . . . H16A H -0.0160 0.8221 0.8613 0.021 Uiso 1 1 calc R U . . . H16B H 0.0780 0.8159 0.7472 0.021 Uiso 1 1 calc R U . . . C17 C 0.16475(10) 0.69158(10) 0.89048(9) 0.01777(19) Uani 1 1 d . . . . . H17A H 0.1334 0.6490 0.9698 0.021 Uiso 1 1 calc R U . . . H17B H 0.2088 0.7524 0.8895 0.021 Uiso 1 1 calc R U . . . C18 C 0.26262(9) 0.59196(10) 0.84154(8) 0.01436(17) Uani 1 1 d . . . . . H18A H 0.3342 0.5440 0.8889 0.017 Uiso 1 1 calc R U . . . H18B H 0.3006 0.6349 0.7648 0.017 Uiso 1 1 calc R U . . . C19 C 0.663(2) 0.2794(13) 0.5467(12) 0.0113(5) Uani 0.5 1 d D U P A 1 C20 C 0.7575(18) 0.1459(11) 0.5728(7) 0.0163(15) Uani 0.5 1 d D U P A 1 C21 C 0.7302(9) 0.0656(7) 0.6957(5) 0.0316(13) Uani 0.5 1 d D U P A 1 H21A H 0.6406 0.0595 0.7110 0.047 Uiso 0.5 1 calc R U P A 1 H21B H 0.7420 0.1055 0.7449 0.047 Uiso 0.5 1 calc R U P A 1 H21C H 0.7907 -0.0196 0.7100 0.047 Uiso 0.5 1 calc R U P A 1 C22 C 0.7411(10) 0.0833(10) 0.4958(7) 0.0250(11) Uani 0.5 1 d D U P A 1 H22A H 0.6516 0.0771 0.5102 0.038 Uiso 0.5 1 calc R U P A 1 H22B H 0.8017 -0.0019 0.5109 0.038 Uiso 0.5 1 calc R U P A 1 H22C H 0.7596 0.1345 0.4171 0.038 Uiso 0.5 1 calc R U P A 1 C23 C 0.8965(12) 0.1592(13) 0.5500(11) 0.0288(19) Uani 0.5 1 d D U P A 1 H23A H 0.9586 0.0747 0.5678 0.043 Uiso 0.5 1 calc R U P A 1 H23B H 0.9043 0.2035 0.5971 0.043 Uiso 0.5 1 calc R U P A 1 H23C H 0.9153 0.2078 0.4705 0.043 Uiso 0.5 1 calc R U P A 1 O1' O 0.5741(14) 0.3066(13) 0.6104(11) 0.0172(14) Uani 0.5 1 d D U P A 2 O2' O 0.6953(12) 0.3545(8) 0.4437(8) 0.0140(8) Uani 0.5 1 d D U P A 2 C19' C 0.671(2) 0.2803(13) 0.5407(12) 0.0113(5) Uani 0.5 1 d D U P A 2 C20' C 0.7676(18) 0.1486(11) 0.5778(7) 0.0163(15) Uani 0.5 1 d D U P A 2 C21' C 0.7491(9) 0.0850(8) 0.7055(5) 0.0316(13) Uani 0.5 1 d D U P A 2 H21D H 0.8034 -0.0031 0.7256 0.047 Uiso 0.5 1 calc R U P A 2 H21E H 0.6574 0.0863 0.7312 0.047 Uiso 0.5 1 calc R U P A 2 H21F H 0.7746 0.1310 0.7417 0.047 Uiso 0.5 1 calc R U P A 2 C22' C 0.9070(11) 0.1570(13) 0.5394(10) 0.0194(11) Uani 0.5 1 d D U P A 2 H22D H 0.9210 0.2178 0.5663 0.029 Uiso 0.5 1 calc R U P A 2 H22E H 0.9228 0.1853 0.4569 0.029 Uiso 0.5 1 calc R U P A 2 H22F H 0.9670 0.0732 0.5701 0.029 Uiso 0.5 1 calc R U P A 2 C23' C 0.7374(12) 0.0705(11) 0.5204(7) 0.0352(17) Uani 0.5 1 d D U P A 2 H23D H 0.7464 0.1129 0.4386 0.053 Uiso 0.5 1 calc R U P A 2 H23E H 0.6482 0.0634 0.5473 0.053 Uiso 0.5 1 calc R U P A 2 H23F H 0.7985 -0.0146 0.5388 0.053 Uiso 0.5 1 calc R U P A 2 C24 C 0.36435(9) 0.42992(9) 0.41204(7) 0.01153(16) Uani 1 1 d . . . . . C25 C 0.28322(10) 0.38440(10) 0.36303(7) 0.01543(18) Uani 1 1 d . . . . . C26 C 0.34562(14) 0.24130(12) 0.38854(10) 0.0259(2) Uani 1 1 d . . . . . H26A H 0.4355 0.2266 0.3515 0.039 Uiso 1 1 calc R U . . . H26B H 0.2960 0.2068 0.3603 0.039 Uiso 1 1 calc R U . . . H26C H 0.3452 0.1991 0.4701 0.039 Uiso 1 1 calc R U . . . C27 C 0.28642(12) 0.45128(12) 0.23541(8) 0.0219(2) Uani 1 1 d . . . . . H27A H 0.2513 0.5432 0.2192 0.033 Uiso 1 1 calc R U . . . H27B H 0.2335 0.4210 0.2062 0.033 Uiso 1 1 calc R U . . . H27C H 0.3764 0.4324 0.1992 0.033 Uiso 1 1 calc R U . . . C28 C 0.14249(11) 0.40891(14) 0.41990(9) 0.0249(2) Uani 1 1 d . . . . . H28A H 0.1415 0.3702 0.5018 0.037 Uiso 1 1 calc R U . . . H28B H 0.0935 0.3716 0.3939 0.037 Uiso 1 1 calc R U . . . H28C H 0.1023 0.5006 0.4005 0.037 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.00849(5) 0.00968(6) 0.00839(5) -0.00282(4) -0.00105(3) -0.00259(4) P1 0.00839(10) 0.00918(10) 0.00882(8) -0.00289(7) -0.00110(7) -0.00221(8) O1 0.0119(15) 0.014(2) 0.0132(19) -0.0038(18) 0.0062(11) 0.0002(17) O2 0.017(2) 0.0171(19) 0.019(2) -0.0031(13) 0.0075(14) 0.0033(12) O3 0.0219(4) 0.0326(5) 0.0117(3) -0.0080(3) -0.0012(3) -0.0162(3) O4 0.0186(3) 0.0293(4) 0.0157(3) -0.0099(3) 0.0018(3) -0.0154(3) C1 0.0109(4) 0.0108(4) 0.0135(3) -0.0040(3) -0.0013(3) -0.0037(3) C2 0.0157(4) 0.0122(4) 0.0165(4) -0.0063(3) -0.0010(3) -0.0044(3) C3 0.0230(5) 0.0145(5) 0.0207(4) -0.0068(4) -0.0052(4) -0.0069(4) C4 0.0209(5) 0.0159(5) 0.0280(5) -0.0059(4) -0.0035(4) -0.0101(4) C5 0.0154(5) 0.0206(5) 0.0323(5) -0.0097(4) 0.0006(4) -0.0097(4) C6 0.0153(4) 0.0172(5) 0.0199(4) -0.0076(3) 0.0037(3) -0.0088(4) C7 0.0116(4) 0.0127(4) 0.0101(3) -0.0031(3) -0.0027(3) -0.0022(3) C8 0.0113(4) 0.0203(5) 0.0122(3) -0.0025(3) -0.0026(3) -0.0044(4) C9 0.0135(4) 0.0236(5) 0.0156(4) -0.0044(4) -0.0053(3) -0.0017(4) C10 0.0177(4) 0.0197(5) 0.0134(4) -0.0037(3) -0.0058(3) -0.0028(4) C11 0.0197(5) 0.0184(5) 0.0112(3) 0.0000(3) -0.0040(3) -0.0057(4) C12 0.0137(4) 0.0180(5) 0.0101(3) -0.0027(3) -0.0018(3) -0.0041(3) C13 0.0104(4) 0.0120(4) 0.0110(3) -0.0048(3) -0.0006(3) -0.0026(3) C14 0.0109(4) 0.0124(4) 0.0148(3) -0.0055(3) -0.0027(3) -0.0021(3) C15 0.0111(4) 0.0143(4) 0.0209(4) -0.0077(3) -0.0020(3) -0.0006(3) C16 0.0169(4) 0.0131(5) 0.0239(4) -0.0094(4) -0.0021(3) -0.0020(4) C17 0.0168(4) 0.0182(5) 0.0235(4) -0.0137(4) -0.0019(3) -0.0038(4) C18 0.0123(4) 0.0157(5) 0.0185(4) -0.0094(3) -0.0017(3) -0.0040(3) C19 0.0099(18) 0.0101(4) 0.0128(11) -0.0036(5) -0.0004(6) -0.0022(7) C20 0.013(2) 0.0106(5) 0.0186(6) -0.0017(5) 0.0003(10) 0.0001(9) C21 0.032(2) 0.014(2) 0.0248(11) 0.0045(10) 0.0058(11) 0.0038(12) C22 0.0272(18) 0.011(2) 0.037(2) -0.0114(19) -0.0015(17) -0.0036(14) C23 0.017(3) 0.021(3) 0.035(3) -0.003(2) -0.005(2) 0.0056(18) O1' 0.016(2) 0.0110(15) 0.0136(16) 0.0025(10) 0.0036(13) -0.0015(14) O2' 0.0129(18) 0.0076(14) 0.0098(11) 0.0013(11) 0.0051(13) 0.0021(12) C19' 0.0099(18) 0.0101(4) 0.0128(11) -0.0036(5) -0.0004(6) -0.0022(7) C20' 0.013(2) 0.0106(5) 0.0186(6) -0.0017(5) 0.0003(10) 0.0001(9) C21' 0.032(2) 0.014(2) 0.0248(11) 0.0045(10) 0.0058(11) 0.0038(12) C22' 0.0083(16) 0.021(2) 0.0252(18) -0.0082(15) 0.0005(13) -0.0009(15) C23' 0.034(2) 0.017(2) 0.054(4) -0.014(3) -0.003(3) -0.0058(17) C24 0.0122(4) 0.0107(4) 0.0122(3) -0.0036(3) -0.0033(3) -0.0028(3) C25 0.0180(4) 0.0212(5) 0.0121(3) -0.0054(3) -0.0026(3) -0.0112(4) C26 0.0409(7) 0.0209(6) 0.0230(5) -0.0096(4) -0.0035(5) -0.0149(5) C27 0.0268(5) 0.0328(6) 0.0129(4) -0.0059(4) -0.0038(4) -0.0176(5) C28 0.0173(5) 0.0431(7) 0.0187(4) -0.0083(4) -0.0026(4) -0.0157(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O2 Ni1 O3 87.1(5) 2_666 . O3 Ni1 O1' 91.0(7) . . O2 Ni1 O4 88.9(5) 2_666 2_666 O3 Ni1 O4 165.35(3) . 2_666 O1' Ni1 O4 88.3(7) . 2_666 O2 Ni1 O1 165.30(17) 2_666 . O3 Ni1 O1 89.4(6) . . O4 Ni1 O1 90.9(6) 2_666 . O3 Ni1 O2' 88.4(4) . 2_666 O1' Ni1 O2' 165.32(17) . 2_666 O4 Ni1 O2' 88.6(4) 2_666 2_666 O2 Ni1 P1 102.8(3) 2_666 . O3 Ni1 P1 95.59(2) . . O1' Ni1 P1 95.6(3) . . O4 Ni1 P1 99.03(2) 2_666 . O1 Ni1 P1 91.7(3) . . O2' Ni1 P1 99.1(3) 2_666 . O2 Ni1 Ni1 83.6(3) 2_666 2_666 O3 Ni1 Ni1 81.87(2) . 2_666 O1' Ni1 Ni1 77.9(3) . 2_666 O4 Ni1 Ni1 83.68(2) 2_666 2_666 O1 Ni1 Ni1 81.7(3) . 2_666 O2' Ni1 Ni1 87.5(3) 2_666 2_666 P1 Ni1 Ni1 172.968(10) . 2_666 C13 P1 C1 104.53(4) . . C13 P1 C7 105.89(4) . . C1 P1 C7 105.36(4) . . C13 P1 Ni1 112.86(3) . . C1 P1 Ni1 110.92(3) . . C7 P1 Ni1 116.34(3) . . C19 O1 Ni1 124.9(7) . . C19 O2 Ni1 124.7(7) . 2_666 C24 O3 Ni1 125.83(7) . . C24 O4 Ni1 123.37(6) . 2_666 C6 C1 C2 109.43(8) . . C6 C1 P1 116.25(6) . . C2 C1 P1 112.11(6) . . C6 C1 H1 106.1 . . C2 C1 H1 106.1 . . P1 C1 H1 106.1 . . C3 C2 C1 110.66(8) . . C3 C2 H2A 109.5 . . C1 C2 H2A 109.5 . . C3 C2 H2B 109.5 . . C1 C2 H2B 109.5 . . H2A C2 H2B 108.1 . . C4 C3 C2 112.24(8) . . C4 C3 H3A 109.2 . . C2 C3 H3A 109.2 . . C4 C3 H3B 109.2 . . C2 C3 H3B 109.2 . . H3A C3 H3B 107.9 . . C3 C4 C5 111.31(9) . . C3 C4 H4A 109.4 . . C5 C4 H4A 109.4 . . C3 C4 H4B 109.4 . . C5 C4 H4B 109.4 . . H4A C4 H4B 108.0 . . C4 C5 C6 110.77(9) . . C4 C5 H5A 109.5 . . C6 C5 H5A 109.5 . . C4 C5 H5B 109.5 . . C6 C5 H5B 109.5 . . H5A C5 H5B 108.1 . . C5 C6 C1 110.69(8) . . C5 C6 H6A 109.5 . . C1 C6 H6A 109.5 . . C5 C6 H6B 109.5 . . C1 C6 H6B 109.5 . . H6A C6 H6B 108.1 . . C8 C7 C12 110.10(7) . . C8 C7 P1 112.09(6) . . C12 C7 P1 115.21(6) . . C8 C7 H7 106.3 . . C12 C7 H7 106.3 . . P1 C7 H7 106.3 . . C9 C8 C7 111.31(8) . . C9 C8 H8A 109.4 . . C7 C8 H8A 109.4 . . C9 C8 H8B 109.4 . . C7 C8 H8B 109.4 . . H8A C8 H8B 108.0 . . C10 C9 C8 111.20(8) . . C10 C9 H9A 109.4 . . C8 C9 H9A 109.4 . . C10 C9 H9B 109.4 . . C8 C9 H9B 109.4 . . H9A C9 H9B 108.0 . . C9 C10 C11 110.17(8) . . C9 C10 H10A 109.6 . . C11 C10 H10A 109.6 . . C9 C10 H10B 109.6 . . C11 C10 H10B 109.6 . . H10A C10 H10B 108.1 . . C12 C11 C10 111.16(8) . . C12 C11 H11A 109.4 . . C10 C11 H11A 109.4 . . C12 C11 H11B 109.4 . . C10 C11 H11B 109.4 . . H11A C11 H11B 108.0 . . C11 C12 C7 111.21(8) . . C11 C12 H12A 109.4 . . C7 C12 H12A 109.4 . . C11 C12 H12B 109.4 . . C7 C12 H12B 109.4 . . H12A C12 H12B 108.0 . . C14 C13 C18 110.26(8) . . C14 C13 P1 111.34(6) . . C18 C13 P1 110.89(6) . . C14 C13 H13 108.1 . . C18 C13 H13 108.1 . . P1 C13 H13 108.1 . . C15 C14 C13 110.67(7) . . C15 C14 H14A 109.5 . . C13 C14 H14A 109.5 . . C15 C14 H14B 109.5 . . C13 C14 H14B 109.5 . . H14A C14 H14B 108.1 . . C16 C15 C14 112.17(8) . . C16 C15 H15A 109.2 . . C14 C15 H15A 109.2 . . C16 C15 H15B 109.2 . . C14 C15 H15B 109.2 . . H15A C15 H15B 107.9 . . C15 C16 C17 111.26(9) . . C15 C16 H16A 109.4 . . C17 C16 H16A 109.4 . . C15 C16 H16B 109.4 . . C17 C16 H16B 109.4 . . H16A C16 H16B 108.0 . . C16 C17 C18 111.64(8) . . C16 C17 H17A 109.3 . . C18 C17 H17A 109.3 . . C16 C17 H17B 109.3 . . C18 C17 H17B 109.3 . . H17A C17 H17B 108.0 . . C17 C18 C13 110.50(8) . . C17 C18 H18A 109.5 . . C13 C18 H18A 109.5 . . C17 C18 H18B 109.5 . . C13 C18 H18B 109.5 . . H18A C18 H18B 108.1 . . O2 C19 O1 124.9(4) . . O2 C19 C20 117.3(4) . . O1 C19 C20 117.6(4) . . C22 C20 C21 109.7(13) . . C22 C20 C19 108.4(15) . . C21 C20 C19 111.0(3) . . C22 C20 C23 110.4(4) . . C21 C20 C23 109.4(12) . . C19 C20 C23 108.1(16) . . C20 C21 H21A 109.5 . . C20 C21 H21B 109.5 . . H21A C21 H21B 109.5 . . C20 C21 H21C 109.5 . . H21A C21 H21C 109.5 . . H21B C21 H21C 109.5 . . C20 C22 H22A 109.5 . . C20 C22 H22B 109.5 . . H22A C22 H22B 109.5 . . C20 C22 H22C 109.5 . . H22A C22 H22C 109.5 . . H22B C22 H22C 109.5 . . C20 C23 H23A 109.5 . . C20 C23 H23B 109.5 . . H23A C23 H23B 109.5 . . C20 C23 H23C 109.5 . . H23A C23 H23C 109.5 . . H23B C23 H23C 109.5 . . C19' O1' Ni1 132.0(7) . . C19' O2' Ni1 117.7(6) . 2_666 O2' C19' O1' 124.9(4) . . O2' C19' C20' 117.6(4) . . O1' C19' C20' 117.5(4) . . C22' C20' C21' 109.4(13) . . C22' C20' C19' 110.8(14) . . C21' C20' C19' 111.5(4) . . C22' C20' C23' 110.0(4) . . C21' C20' C23' 109.6(12) . . C19' C20' C23' 105.5(16) . . C20' C21' H21D 109.5 . . C20' C21' H21E 109.5 . . H21D C21' H21E 109.5 . . C20' C21' H21F 109.5 . . H21D C21' H21F 109.5 . . H21E C21' H21F 109.5 . . C20' C22' H22D 109.5 . . C20' C22' H22E 109.5 . . H22D C22' H22E 109.5 . . C20' C22' H22F 109.5 . . H22D C22' H22F 109.5 . . H22E C22' H22F 109.5 . . C20' C23' H23D 109.5 . . C20' C23' H23E 109.5 . . H23D C23' H23E 109.5 . . C20' C23' H23F 109.5 . . H23D C23' H23F 109.5 . . H23E C23' H23F 109.5 . . O4 C24 O3 125.11(9) . . O4 C24 C25 117.89(8) . . O3 C24 C25 116.95(8) . . C28 C25 C24 109.98(8) . . C28 C25 C27 109.91(9) . . C24 C25 C27 111.02(8) . . C28 C25 C26 110.07(10) . . C24 C25 C26 106.12(9) . . C27 C25 C26 109.68(9) . . C25 C26 H26A 109.5 . . C25 C26 H26B 109.5 . . H26A C26 H26B 109.5 . . C25 C26 H26C 109.5 . . H26A C26 H26C 109.5 . . H26B C26 H26C 109.5 . . C25 C27 H27A 109.5 . . C25 C27 H27B 109.5 . . H27A C27 H27B 109.5 . . C25 C27 H27C 109.5 . . H27A C27 H27C 109.5 . . H27B C27 H27C 109.5 . . C25 C28 H28A 109.5 . . C25 C28 H28B 109.5 . . H28A C28 H28B 109.5 . . C25 C28 H28C 109.5 . . H28A C28 H28C 109.5 . . H28B C28 H28C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ni1 O2 1.978(10) 2_666 Ni1 O3 2.0019(7) . Ni1 O1' 2.006(9) . Ni1 O4 2.0064(8) 2_666 Ni1 O1 2.017(9) . Ni1 O2' 2.057(9) 2_666 Ni1 P1 2.3773(3) . Ni1 Ni1 2.7364(2) 2_666 P1 C13 1.8480(9) . P1 C1 1.8568(10) . P1 C7 1.8638(9) . O1 C19 1.258(3) . O2 C19 1.255(3) . O2 Ni1 1.978(10) 2_666 O3 C24 1.2590(10) . O4 C24 1.2584(11) . O4 Ni1 2.0064(8) 2_666 C1 C6 1.5366(13) . C1 C2 1.5398(13) . C1 H1 1.0000 . C2 C3 1.5317(15) . C2 H2A 0.9900 . C2 H2B 0.9900 . C3 C4 1.5272(15) . C3 H3A 0.9900 . C3 H3B 0.9900 . C4 C5 1.5273(16) . C4 H4A 0.9900 . C4 H4B 0.9900 . C5 C6 1.5311(15) . C5 H5A 0.9900 . C5 H5B 0.9900 . C6 H6A 0.9900 . C6 H6B 0.9900 . C7 C8 1.5360(13) . C7 C12 1.5398(12) . C7 H7 1.0000 . C8 C9 1.5318(14) . C8 H8A 0.9900 . C8 H8B 0.9900 . C9 C10 1.5249(13) . C9 H9A 0.9900 . C9 H9B 0.9900 . C10 C11 1.5278(15) . C10 H10A 0.9900 . C10 H10B 0.9900 . C11 C12 1.5271(14) . C11 H11A 0.9900 . C11 H11B 0.9900 . C12 H12A 0.9900 . C12 H12B 0.9900 . C13 C14 1.5371(13) . C13 C18 1.5385(14) . C13 H13 1.0000 . C14 C15 1.5310(13) . C14 H14A 0.9900 . C14 H14B 0.9900 . C15 C16 1.5228(15) . C15 H15A 0.9900 . C15 H15B 0.9900 . C16 C17 1.5292(15) . C16 H16A 0.9900 . C16 H16B 0.9900 . C17 C18 1.5340(14) . C17 H17A 0.9900 . C17 H17B 0.9900 . C18 H18A 0.9900 . C18 H18B 0.9900 . C19 C20 1.532(3) . C20 C22 1.52(2) . C20 C21 1.528(4) . C20 C23 1.54(2) . C21 H21A 0.9800 . C21 H21B 0.9800 . C21 H21C 0.9800 . C22 H22A 0.9800 . C22 H22B 0.9800 . C22 H22C 0.9800 . C23 H23A 0.9800 . C23 H23B 0.9800 . C23 H23C 0.9800 . O1' C19' 1.258(3) . O2' C19' 1.256(3) . O2' Ni1 2.057(9) 2_666 C19' C20' 1.532(3) . C20' C22' 1.52(2) . C20' C21' 1.528(4) . C20' C23' 1.54(2) . C21' H21D 0.9800 . C21' H21E 0.9800 . C21' H21F 0.9800 . C22' H22D 0.9800 . C22' H22E 0.9800 . C22' H22F 0.9800 . C23' H23D 0.9800 . C23' H23E 0.9800 . C23' H23F 0.9800 . C24 C25 1.5330(14) . C25 C28 1.5301(15) . C25 C27 1.5331(13) . C25 C26 1.5343(17) . C26 H26A 0.9800 . C26 H26B 0.9800 . C26 H26C 0.9800 . C27 H27A 0.9800 . C27 H27B 0.9800 . C27 H27C 0.9800 . C28 H28A 0.9800 . C28 H28B 0.9800 . C28 H28C 0.9800 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 C13 P1 C1 C6 -48.45(8) . C7 P1 C1 C6 62.94(8) . Ni1 P1 C1 C6 -170.36(6) . C13 P1 C1 C2 -175.36(6) . C7 P1 C1 C2 -63.98(7) . Ni1 P1 C1 C2 62.73(7) . C6 C1 C2 C3 57.22(10) . P1 C1 C2 C3 -172.28(6) . C1 C2 C3 C4 -55.13(11) . C2 C3 C4 C5 53.75(12) . C3 C4 C5 C6 -54.84(12) . C4 C5 C6 C1 58.21(12) . C2 C1 C6 C5 -59.18(11) . P1 C1 C6 C5 172.59(7) . C13 P1 C7 C8 -98.60(7) . C1 P1 C7 C8 150.99(7) . Ni1 P1 C7 C8 27.67(8) . C13 P1 C7 C12 28.34(8) . C1 P1 C7 C12 -82.07(8) . Ni1 P1 C7 C12 154.61(6) . C12 C7 C8 C9 55.31(11) . P1 C7 C8 C9 -175.05(7) . C7 C8 C9 C10 -56.68(12) . C8 C9 C10 C11 56.90(12) . C9 C10 C11 C12 -57.17(11) . C10 C11 C12 C7 57.00(11) . C8 C7 C12 C11 -55.53(11) . P1 C7 C12 C11 176.52(7) . C1 P1 C13 C14 -52.32(7) . C7 P1 C13 C14 -163.32(7) . Ni1 P1 C13 C14 68.31(7) . C1 P1 C13 C18 -175.48(6) . C7 P1 C13 C18 73.52(7) . Ni1 P1 C13 C18 -54.85(7) . C18 C13 C14 C15 -56.96(10) . P1 C13 C14 C15 179.52(6) . C13 C14 C15 C16 55.60(11) . C14 C15 C16 C17 -54.02(11) . C15 C16 C17 C18 54.32(11) . C16 C17 C18 C13 -56.33(11) . C14 C13 C18 C17 57.45(10) . P1 C13 C18 C17 -178.77(7) . Ni1 O2 C19 O1 2(4) 2_666 Ni1 O2 C19 C20 177.6(16) 2_666 Ni1 O1 C19 O2 -4(5) . Ni1 O1 C19 C20 -179.7(18) . O2 C19 C20 C22 -68(3) . O1 C19 C20 C22 108(3) . O2 C19 C20 C21 172(2) . O1 C19 C20 C21 -12(3) . O2 C19 C20 C23 52(3) . O1 C19 C20 C23 -132(3) . Ni1 O2' C19' O1' 3(4) 2_666 Ni1 O2' C19' C20' -176.0(18) 2_666 Ni1 O1' C19' O2' -1(5) . Ni1 O1' C19' C20' 178.0(19) . O2' C19' C20' C22' 41(3) . O1' C19' C20' C22' -138(2) . O2' C19' C20' C21' 163(2) . O1' C19' C20' C21' -16(3) . O2' C19' C20' C23' -78(3) . O1' C19' C20' C23' 103(3) . Ni1 O4 C24 O3 -3.33(15) 2_666 Ni1 O4 C24 C25 179.19(7) 2_666 Ni1 O3 C24 O4 -0.19(16) . Ni1 O3 C24 C25 177.30(7) . O4 C24 C25 C28 -148.94(10) . O3 C24 C25 C28 33.38(13) . O4 C24 C25 C27 -27.08(13) . O3 C24 C25 C27 155.24(10) . O4 C24 C25 C26 92.04(11) . O3 C24 C25 C26 -85.64(11) .