# Copyright The Royal Society of Chemistry, 1998 #============================================================================== data_global #============================================================================== _audit_creation_date 9-10-97 _audit_creation_method from_MolEN_master_file_using_cif_in _audit_update_record ; ? ; # 1. SUBMISSION DETAILS _publ_contact_author ; Ulli Englert Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str.1 52074 Aachen Germany ; _publ_contact_author_email 'ullrich.englert@ac.rwth-aachen.de' _publ_contact_author_fax '(0241) 8888288' _publ_contact_author_phone '(0241) 804666' _publ_requested_journal ? _publ_requested_coeditor_name ? _publ_contact_letter ; ?edit? ; # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; Electronic effects in the nickel-catalysed hydrocyanation of styrene applying chelating phosphorus ligands with large bite angles ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Goertz, Wolfgang' ; Institut fuer Technische Chemie und Petrolchemie RWTH Aachen Templergraben 55 52056 Aachen Germany ; 'Keim, Wilhelm' ; Institut fuer Technische Chemie und Petrolchemie RWTH Aachen Templergraben 55 52056 Aachen Germany ; 'Vogt, Dieter' ; Institut fuer Technische Chemie und Petrolchemie RWTH Aachen Templergraben 55 52056 Aachen Germany ; 'Englert, Ulli' ; Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str.1 52074 Aachen Germany ; 'Boele, Maarten D. K.' ; J. H. vant Hoff Research Institute Department of Inorganic Chemistry University of Amsterdam Nieuwe Achtergracht 166 1018 WV Amsterdam The Netherlands ; 'van der Veenc, Lars A. ' ; J. H. vant Hoff Research Institute Department of Inorganic Chemistry University of Amsterdam Nieuwe Achtergracht 166 1018 WV Amsterdam The Netherlands ; 'Kamerc, Paul C. J.' ; J. H. vant Hoff Research Institute Department of Inorganic Chemistry University of Amsterdam Nieuwe Achtergracht 166 1018 WV Amsterdam The Netherlands ; 'van Leeuwenc, Piet W. N. M.' ; J. H. vant Hoff Research Institute Department of Inorganic Chemistry University of Amsterdam Nieuwe Achtergracht 166 1018 WV Amsterdam The Netherlands ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_experimental ; Backgrounds were obtained from analysis of the scan profile (Blessing, Coppens _& Becker, 1974) ; _publ_section_references ; Blessing, R.H., Coppens, P. & Becker, P. (1974). J. Appl. Cryst., 7, 488-492. Enraf-Nonius, CAD4 Operations Manual, Delft, 1977. Fair, C.K. (1990). MolEN, An Interactive Intelligent System for Crystal Structure Analysis, User Manual, Enraf - Nonius, Delft, The Netherlands. International Tables for X-Ray Crystallography, T. Hahn E Vol. A, D. Reidel Publ. Comp., Dordrecht, (1983) Johnson, C.K. (1976). ORTEP. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ?none? ?none? ; data_DV1_220997 # 5. CRYSTAL DATA _chemical_compound_source 'see paper' _exptl_crystal_description 'irregular fragment' _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _chemical_name_common ; Complex 3 ; _chemical_formula_sum 'C56 H48 Cl2 Ni1 O1 P2 S1' _chemical_formula_weight 960.63 _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m 'P21/c' _cell_length_a 19.755(8) _cell_length_b 19.314(8) _cell_length_c 13.072(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.14(3) _cell_angle_gamma 90.00 _cell_volume 4857(3) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9 _cell_measurement_theta_max 13 _cell_formula_units_z 4.00 _exptl_crystal_density_diffrn 1.31 _exptl_crystal_density_meas none _diffrn_radiation_type Mo-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.655 _cell_measurement_temperature 203 _exptl_crystal_F_000 2000 # 6. DATA COLLECTION _diffrn_ambient_temperature 203 _diffrn_measurement_device Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.945 _exptl_absorpt_correction_T_max 1.000 _diffrn_reflns_number 12207 _reflns_number_total 8523 _reflns_number_observed 5601 _reflns_observed_criterion >1.0\s(I) _diffrn_reflns_av_R_equivalents 0.060 _diffrn_reflns_theta_min 2.0 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_max 22 _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% -2.72 # 7. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_R_factor_obs 0.085 _refine_ls_wR_factor_obs 0.065 _refine_ls_hydrogen_treatment riding _refine_ls_number_reflns 5601 _refine_ls_number_parameters 568 _refine_ls_number_restraints 192 _refine_ls_goodness_of_fit_obs 1.173 _refine_ls_weighting_scheme '4Fo^2^/ (\s^2^(Fo^2^) + 0.0016 Fo^4^)' _refine_ls_shift/esd_max 0.013 _refine_diff_density_max 0.5514 _refine_diff_density_min -0.6438 _refine_ls_extinction_method none _atom_type_scat_source International_Tables_for_Xray_Crystallography # 8. COMPUTING DATA _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_reduction PROCESS_MolEN_(Fair,_1990) _computing_structure_solution SHELXS86_(Sheldrick,_1986) _computing_structure_refinement LSFM_MolEN_(Fair,_1990) _computing_molecular_graphics ORTEP_(Johnson,_1976) _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Ni 0.73160(4) 0.59881(4) 0.06172(6) 0.0278(2) Ueq Cl1 0.62810(9) 0.64187(8) -0.0030(1) 0.0466(5) Ueq Cl2 0.83346(8) 0.64767(9) 0.1249(1) 0.0431(5) Ueq S 0.94629(9) 0.37835(9) 0.2242(1) 0.0423(5) Ueq P1 0.75411(8) 0.52484(8) -0.0652(1) 0.0283(4) Ueq P2 0.71522(8) 0.53543(8) 0.2034(1) 0.0263(4) Ueq O 0.8084(2) 0.4474(2) 0.1292(3) 0.028(1) Ueq C1 0.8556(3) 0.4462(3) 0.0654(4) 0.027(2) Ueq C2 0.8360(3) 0.4769(3) -0.0325(4) 0.028(2) Ueq C3 0.8801(3) 0.4718(3) -0.1015(4) 0.029(2) Ueq C4 0.9429(3) 0.4368(3) -0.0739(4) 0.031(2) Ueq C5 0.9632(3) 0.4096(3) 0.0275(5) 0.036(2) Ueq C6 0.9193(3) 0.4147(3) 0.0974(4) 0.033(2) Ueq C7 0.8973(3) 0.4312(3) 0.2897(4) 0.032(2) Ueq C8 0.9178(3) 0.4438(3) 0.3978(5) 0.038(2) Ueq C9 0.8776(3) 0.4833(3) 0.4491(4) 0.035(2) Ueq C10 0.8164(3) 0.5116(3) 0.3931(4) 0.033(2) Ueq C11 0.7949(3) 0.5008(3) 0.2855(4) 0.028(2) Ueq C12 0.8358(3) 0.4602(3) 0.2357(4) 0.027(2) Ueq C13 0.9892(3) 0.4290(3) -0.1494(5) 0.042(2) Ueq C14 0.9013(4) 0.4954(4) 0.5666(5) 0.055(2) Ueq C20 0.7628(3) 0.5764(3) -0.1785(4) 0.028(2) Ueq C21 0.7286(4) 0.5597(4) -0.2797(5) 0.048(2) Ueq C22 0.7353(4) 0.6027(4) -0.3625(5) 0.062(3) Ueq C23 0.7760(4) 0.6608(4) -0.3449(5) 0.060(2) Ueq C24 0.8109(4) 0.6768(4) -0.2442(5) 0.053(2) Ueq C25 0.8035(3) 0.6358(3) -0.1612(5) 0.042(2) Ueq C30 0.6874(3) 0.4610(3) -0.1182(4) 0.033(2) Ueq C31 0.6187(3) 0.4832(4) -0.1449(5) 0.047(2) Ueq C32 0.5671(4) 0.4360(4) -0.1883(5) 0.059(2) Ueq C33 0.5836(4) 0.3683(4) -0.2054(6) 0.073(3) Ueq C34 0.6508(5) 0.3475(4) -0.1791(7) 0.093(3) Ueq C35 0.7034(4) 0.3930(4) -0.1345(6) 0.063(3) Ueq C40 0.6560(3) 0.4624(3) 0.1826(4) 0.025(2) Ueq C41 0.5976(3) 0.4659(3) 0.1013(5) 0.043(2) Ueq C42 0.5488(4) 0.4130(4) 0.0868(5) 0.053(2) Ueq C43 0.5574(3) 0.3575(4) 0.1529(5) 0.047(2) Ueq C44 0.6149(4) 0.3534(3) 0.2341(6) 0.053(2) Ueq C45 0.6649(3) 0.4060(3) 0.2492(5) 0.044(2) Ueq C50 0.6803(3) 0.5931(3) 0.2881(4) 0.027(2) Ueq C51 0.6253(3) 0.5749(3) 0.3317(5) 0.037(2) Ueq C52 0.5975(3) 0.6220(4) 0.3906(5) 0.046(2) Ueq C53 0.6245(4) 0.6880(4) 0.4043(5) 0.050(2) Ueq C54 0.6799(4) 0.7062(3) 0.3617(5) 0.050(2) Ueq C55 0.7073(3) 0.6596(3) 0.3036(5) 0.042(2) Ueq C60 0.0140(4) 0.7389(4) 0.5647(6) 0.066(3) Ueq C61 -0.0521(4) 0.7165(4) 0.5513(6) 0.079(3) Ueq C62 -0.0837(5) 0.6854(5) 0.4583(8) 0.095(4) Ueq C63 -0.0473(5) 0.6761(5) 0.3827(7) 0.101(4) Ueq C64 0.0190(5) 0.6985(4) 0.3984(6) 0.082(3) Ueq C65 0.0496(4) 0.7302(4) 0.4888(6) 0.075(3) Ueq C70 0.1867(5) 0.7003(5) 0.2624(8) 0.094(4) Ueq C71 0.2099(5) 0.7645(5) 0.2963(7) 0.100(4) Ueq C72 0.2432(5) 0.7746(5) 0.3990(8) 0.107(4) Ueq C73 0.2517(5) 0.7219(5) 0.4679(7) 0.106(4) Ueq C74 0.2276(5) 0.6564(5) 0.4319(7) 0.098(4) Ueq C75 0.1964(5) 0.6475(5) 0.3297(7) 0.097(4) Ueq C80 0.4997(6) 0.5833(5) 0.6004(7) 0.166(4) Ueq C81 0.4461(5) 0.6010(8) 0.5250(7) 0.186(5) Ueq C82 0.4343(5) 0.6681(8) 0.5001(7) 0.159(5) Ueq C83 0.4761(6) 0.7145(6) 0.5537(6) 0.141(4) Ueq C84 0.5301(5) 0.6977(7) 0.6278(7) 0.144(5) Ueq C85 0.5399(5) 0.6302(6) 0.6493(7) 0.144(4) Ueq H3 0.8670 0.4940 -0.1706 0.0374 Uiso calc H5 1.0086 0.3870 0.0499 0.0468 Uiso calc H8 0.9619 0.4249 0.4382 0.0494 Uiso calc H10 0.7882 0.5410 0.4283 0.0424 Uiso calc H13a 1.0001 0.4685 -0.1898 0.0541 Uiso calc H13b 0.9680 0.3938 -0.2009 0.0541 Uiso calc H13c 1.0337 0.4118 -0.1080 0.0541 Uiso calc H14a 0.8603 0.4991 0.5968 0.0710 Uiso calc H14b 0.9284 0.5383 0.5796 0.0710 Uiso calc H14c 0.9301 0.4564 0.5989 0.0710 Uiso calc H21 0.6996 0.5180 -0.2931 0.0629 Uiso calc H22 0.7114 0.5909 -0.4346 0.0806 Uiso calc H23 0.7793 0.6914 -0.4034 0.0777 Uiso calc H24 0.8414 0.7174 -0.2317 0.0687 Uiso calc H25 0.8275 0.6480 -0.0894 0.0541 Uiso calc H31 0.6072 0.5316 -0.1337 0.0615 Uiso calc H32 0.5183 0.4504 -0.2072 0.0773 Uiso calc H33 0.5466 0.3354 -0.2355 0.0954 Uiso calc H34 0.6621 0.2995 -0.1928 0.1207 Uiso calc H35 0.7518 0.3775 -0.1149 0.0820 Uiso calc H41 0.5911 0.5056 0.0534 0.0552 Uiso calc H42 0.5078 0.4153 0.0284 0.0688 Uiso calc H43 0.5226 0.3206 0.1419 0.0616 Uiso calc H44 0.6200 0.3143 0.2831 0.0686 Uiso calc H45 0.7067 0.4026 0.3061 0.0577 Uiso calc H51 0.6057 0.5282 0.3201 0.0477 Uiso calc H52 0.5591 0.6088 0.4226 0.0590 Uiso calc H53 0.6034 0.7224 0.4425 0.0652 Uiso calc H54 0.7002 0.7525 0.3752 0.0654 Uiso calc H55 0.7463 0.6730 0.2730 0.0545 Uiso calc H60 0.0364 0.7622 0.6302 0.0852 Uiso calc H61 -0.0768 0.7227 0.6077 0.1029 Uiso calc H62 -0.1317 0.6687 0.4465 0.1230 Uiso calc H63 -0.0685 0.6540 0.3156 0.1318 Uiso calc H64 0.0453 0.6926 0.3437 0.1064 Uiso calc H65 0.0979 0.7462 0.5006 0.0971 Uiso calc H70 0.1628 0.6928 0.1889 0.1228 Uiso calc H71 0.2026 0.8037 0.2474 0.1304 Uiso calc H72 0.2620 0.8204 0.4223 0.1388 Uiso calc H73 0.2731 0.7297 0.5424 0.1376 Uiso calc H74 0.2346 0.6165 0.4795 0.1281 Uiso calc H75 0.1797 0.6014 0.3044 0.1268 Uiso calc H80 0.5152 0.5372 0.6273 0.2040 Uiso calc H81 0.4200 0.5600 0.4939 0.2295 Uiso calc H82 0.3923 0.6761 0.4449 0.2130 Uiso calc H83 0.4616 0.7614 0.5295 0.1877 Uiso calc H84 0.5585 0.7372 0.6591 0.1837 Uiso calc H85 0.5814 0.6220 0.7055 0.1801 Uiso calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni 0.0277(3) 0.0234(4) 0.0332(4) 0.0003(4) 0.0090(3) 0.0026(4) Cl1 0.0319(9) 0.0341(9) 0.070(1) 0.0071(8) 0.0049(8) 0.0125(9) Cl2 0.0342(8) 0.047(1) 0.0487(9) -0.0118(8) 0.0115(7) -0.0091(8) S 0.0390(9) 0.044(1) 0.0435(9) 0.0165(8) 0.0077(7) 0.0086(8) P1 0.0265(9) 0.0288(8) 0.0289(8) 0.0015(7) 0.0050(7) 0.0032(8) P2 0.0259(8) 0.0246(8) 0.0292(8) 0.0001(7) 0.0077(6) 0.0004(7) O 0.025(2) 0.030(2) 0.030(2) 0.002(2) 0.007(2) 0.004(2) C1 0.028(3) 0.026(3) 0.027(3) -0.001(3) 0.006(2) -0.007(3) C2 0.028(3) 0.021(3) 0.032(3) -0.003(3) 0.001(3) -0.008(3) C3 0.026(3) 0.030(3) 0.029(3) -0.004(3) 0.004(3) -0.006(3) C4 0.026(3) 0.030(3) 0.037(3) -0.005(3) 0.009(3) -0.011(3) C5 0.026(3) 0.028(3) 0.053(4) 0.003(3) 0.010(3) -0.015(3) C6 0.040(3) 0.024(3) 0.033(3) -0.004(3) 0.007(3) -0.008(3) C7 0.035(3) 0.034(3) 0.030(3) 0.001(3) 0.009(3) 0.012(3) C8 0.028(3) 0.040(4) 0.044(4) -0.003(3) 0.004(3) 0.011(3) C9 0.032(3) 0.044(4) 0.029(3) -0.005(3) 0.007(3) 0.010(3) C10 0.034(3) 0.032(3) 0.034(3) -0.008(3) 0.010(3) -0.000(3) C11 0.022(3) 0.026(3) 0.034(3) -0.005(3) 0.004(2) 0.007(3) C12 0.029(3) 0.023(3) 0.029(3) -0.002(3) 0.007(2) 0.006(3) C13 0.037(3) 0.045(4) 0.046(4) 0.004(3) 0.015(3) -0.014(3) C14 0.050(4) 0.082(5) 0.028(4) -0.007(4) -0.000(3) 0.003(4) C20 0.028(3) 0.032(3) 0.027(3) 0.005(3) 0.009(2) 0.004(3) C21 0.046(4) 0.064(5) 0.031(4) 0.003(4) -0.000(3) 0.009(4) C22 0.058(5) 0.092(6) 0.033(4) 0.005(5) 0.003(3) 0.007(4) C23 0.069(5) 0.066(5) 0.048(4) 0.002(4) 0.020(4) 0.017(4) C24 0.060(4) 0.038(4) 0.068(4) -0.002(4) 0.032(3) 0.008(4) C25 0.055(4) 0.032(4) 0.042(4) -0.003(3) 0.020(3) 0.000(3) C30 0.030(3) 0.043(4) 0.027(3) -0.000(3) 0.007(3) 0.002(3) C31 0.034(4) 0.061(5) 0.047(4) -0.009(4) 0.008(3) -0.006(4) C32 0.032(4) 0.086(6) 0.055(5) -0.022(4) 0.000(3) -0.014(4) C33 0.063(5) 0.065(5) 0.078(6) -0.025(5) -0.013(5) 0.003(5) C34 0.079(6) 0.040(5) 0.131(8) -0.007(5) -0.038(6) -0.004(5) C35 0.048(5) 0.034(4) 0.094(6) -0.002(4) -0.013(4) -0.008(4) C40 0.029(3) 0.022(3) 0.026(3) -0.001(3) 0.010(2) -0.000(3) C41 0.026(3) 0.043(4) 0.054(4) -0.014(3) 0.000(3) 0.006(4) C42 0.038(4) 0.062(5) 0.054(4) -0.011(4) -0.000(3) 0.008(4) C43 0.043(4) 0.042(4) 0.060(4) -0.018(3) 0.017(3) -0.010(4) C44 0.062(5) 0.027(4) 0.069(5) -0.010(4) 0.012(4) 0.007(4) C45 0.045(4) 0.036(4) 0.048(4) -0.007(4) 0.002(3) 0.002(4) C50 0.032(3) 0.021(3) 0.029(3) 0.009(3) 0.006(2) 0.001(3) C51 0.037(3) 0.033(4) 0.042(3) -0.005(3) 0.015(3) -0.005(3) C52 0.041(4) 0.055(4) 0.048(4) -0.004(3) 0.027(3) 0.004(4) C53 0.059(4) 0.048(4) 0.048(4) -0.001(4) 0.023(3) -0.013(4) C54 0.069(4) 0.028(4) 0.063(4) -0.009(3) 0.034(3) -0.007(3) C55 0.044(4) 0.029(4) 0.061(4) -0.005(3) 0.027(3) -0.006(3) C60 0.100(6) 0.037(4) 0.058(5) 0.003(5) 0.014(4) 0.004(4) C61 0.094(6) 0.065(5) 0.089(5) 0.026(5) 0.044(4) 0.018(5) C62 0.051(5) 0.097(7) 0.126(8) 0.014(5) -0.002(5) 0.016(7) C63 0.101(7) 0.111(8) 0.067(6) 0.018(7) -0.030(6) -0.013(6) C64 0.122(7) 0.077(6) 0.052(4) 0.035(5) 0.032(4) 0.011(5) C65 0.086(6) 0.052(5) 0.093(6) 0.002(5) 0.034(4) 0.010(5) C70 0.070(6) 0.100(7) 0.110(7) 0.006(6) 0.013(5) 0.011(7) C71 0.087(6) 0.082(6) 0.141(8) 0.037(5) 0.044(5) 0.036(6) C72 0.109(8) 0.069(6) 0.137(8) 0.015(6) 0.019(6) -0.016(6) C73 0.115(8) 0.095(7) 0.091(7) 0.006(7) -0.010(6) -0.023(6) C74 0.107(7) 0.087(7) 0.098(7) -0.009(6) 0.016(6) 0.015(6) C75 0.113(7) 0.086(7) 0.093(6) -0.028(6) 0.025(6) -0.017(6) C80 0.315(8) 0.067(7) 0.195(6) 0.033(6) 0.221(4) 0.016(6) C81 0.161(7) 0.30(2) 0.133(7) -0.118(9) 0.112(5) -0.088(9) C82 0.125(7) 0.30(1) 0.069(6) 0.109(8) 0.050(5) 0.033(8) C83 0.27(1) 0.092(7) 0.103(5) 0.050(7) 0.129(5) 0.035(5) C84 0.144(7) 0.22(1) 0.097(6) -0.072(8) 0.080(5) -0.045(8) C85 0.122(6) 0.22(1) 0.107(6) 0.112(6) 0.069(5) 0.084(7) # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Ni Cl1 2.191(2) ? Ni Cl2 2.206(2) ? Ni P1 2.307(2) ? Ni P2 2.304(2) ? S C6 1.767(6) ? S C7 1.758(6) ? P1 C2 1.829(6) ? P1 C20 1.826(6) ? P1 C30 1.823(6) ? P2 C11 1.819(6) ? P2 C40 1.813(6) ? P2 C50 1.813(6) ? O C1 1.386(6) ? O C12 1.397(6) ? C1 C2 1.384(8) ? C1 C6 1.373(8) ? C2 C3 1.391(8) ? C3 C4 1.387(8) ? C3 H3 0.9800 ? C4 C5 1.397(8) ? C4 C13 1.497(8) ? C5 C6 1.400(8) ? C5 H5 0.9800 ? C7 C8 1.400(8) ? C7 C12 1.378(8) ? C8 C9 1.380(8) ? C8 H8 0.9800 ? C9 C10 1.376(8) ? C9 C14 1.519(8) ? C10 C11 1.390(7) ? C10 H10 0.9800 ? C11 C12 1.389(8) ? C13 H13a 0.9800 ? C13 H13b 0.9800 ? C13 H13c 0.9800 ? C14 H14a 0.9800 ? C14 H14b 0.9800 ? C14 H14c 0.9800 ? C20 C21 1.380(8) ? C20 C25 1.389(8) ? C21 C22 1.395(9) ? C21 H21 0.9800 ? C22 C23 1.37(1) ? C22 H22 0.9800 ? C23 C24 1.37(1) ? C23 H23 0.9800 ? C24 C25 1.377(8) ? C24 H24 0.9800 ? C25 H25 0.9800 ? C30 C31 1.390(8) ? C30 C35 1.378(9) ? C31 C32 1.390(9) ? C31 H31 0.9800 ? C32 C33 1.38(1) ? C32 H32 0.9800 ? C33 C34 1.35(1) ? C33 H33 0.9800 ? C34 C35 1.38(1) ? C34 H34 0.9800 ? C35 H35 0.9800 ? C40 C41 1.382(8) ? C40 C45 1.381(8) ? C41 C42 1.388(9) ? C41 H41 0.9800 ? C42 C43 1.361(9) ? C42 H42 0.9800 ? C43 C44 1.369(9) ? C43 H43 0.9800 ? C44 C45 1.399(9) ? C44 H44 0.9800 ? C45 H45 0.9800 ? C50 C51 1.383(8) ? C50 C55 1.388(8) ? C51 C52 1.383(8) ? C51 H51 0.9800 ? C52 C53 1.377(9) ? C52 H52 0.9800 ? C53 C54 1.381(9) ? C53 H53 0.9800 ? C54 C55 1.367(8) ? C54 H54 0.9800 ? C55 H55 0.9800 ? C60 C61 1.35(1) ? C60 C65 1.35(1) ? C60 H60 0.9800 ? C61 C62 1.37(1) ? C61 H61 0.9800 ? C62 C63 1.36(1) ? C62 H62 0.9800 ? C63 C64 1.35(1) ? C63 H63 0.9800 ? C64 C65 1.35(1) ? C64 H64 0.9800 ? C65 H65 0.9800 ? C70 C71 1.36(1) ? C70 C75 1.33(1) ? C70 H70 0.9800 ? C71 C72 1.37(1) ? C71 H71 0.9800 ? C72 C73 1.35(1) ? C72 H72 0.9800 ? C73 C74 1.40(1) ? C73 H73 0.9800 ? C74 C75 1.35(1) ? C74 H74 0.9800 ? C75 H75 0.9800 ? C80 C81 1.32(3) ? C80 C85 1.28(2) ? C80 H80 0.9800 ? C81 C82 1.34(3) ? C81 H81 0.9800 ? C82 C83 1.31(2) ? C82 H82 0.9800 ? C83 C84 1.31(2) ? C83 H83 0.9800 ? C84 C85 1.34(2) ? C84 H84 0.9800 ? C85 H85 0.9800 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Cl1 Ni Cl2 132.37(7) ? Cl1 Ni P1 105.82(7) ? Cl1 Ni P2 102.88(7) ? Cl2 Ni P1 103.03(7) ? Cl2 Ni P2 102.08(7) ? P1 Ni P2 109.52(6) ? C6 S C7 98.2(3) ? Ni P1 C2 116.8(2) ? Ni P1 C20 108.3(2) ? Ni P1 C30 116.8(2) ? C2 P1 C20 103.0(3) ? C2 P1 C30 105.7(3) ? C20 P1 C30 104.7(3) ? Ni P2 C11 114.1(2) ? Ni P2 C40 119.8(2) ? Ni P2 C50 107.9(2) ? C11 P2 C40 104.1(3) ? C11 P2 C50 105.3(3) ? C40 P2 C50 104.3(3) ? C1 O C12 116.2(5) ? O C1 C2 117.7(5) ? O C1 C6 121.3(5) ? C2 C1 C6 121.1(6) ? P1 C2 C1 118.6(5) ? P1 C2 C3 122.4(5) ? C1 C2 C3 119.0(6) ? C2 C3 C4 121.4(6) ? C2 C3 H3 119.54 ? C4 C3 H3 119.07 ? C3 C4 C5 118.5(6) ? C3 C4 C13 121.4(6) ? C5 C4 C13 120.1(6) ? C4 C5 C6 120.4(6) ? C4 C5 H5 119.75 ? C6 C5 H5 119.88 ? S C6 C1 121.5(5) ? S C6 C5 118.9(5) ? C1 C6 C5 119.6(6) ? S C7 C8 121.8(5) ? S C7 C12 120.4(5) ? C8 C7 C12 117.8(6) ? C7 C8 C9 121.3(6) ? C7 C8 H8 119.81 ? C9 C8 H8 118.91 ? C8 C9 C10 119.7(6) ? C8 C9 C14 119.8(6) ? C10 C9 C14 120.5(6) ? C9 C10 C11 120.5(6) ? C9 C10 H10 120.36 ? C11 C10 H10 119.10 ? P2 C11 C10 124.5(5) ? P2 C11 C12 116.7(5) ? C10 C11 C12 118.8(6) ? O C12 C7 122.3(5) ? O C12 C11 115.6(5) ? C7 C12 C11 121.9(6) ? C4 C13 H13a 121.24 ? C4 C13 H13b 107.07 ? C4 C13 H13c 105.95 ? H13a C13 H13b 106.40 ? H13a C13 H13c 106.40 ? H13b C13 H13c 109.47 ? C9 C14 H14a 108.98 ? C9 C14 H14b 109.67 ? C9 C14 H14c 109.46 ? H14a C14 H14b 109.63 ? H14a C14 H14c 109.63 ? H14b C14 H14c 109.47 ? P1 C20 C21 122.3(5) ? P1 C20 C25 118.4(5) ? C21 C20 C25 119.2(6) ? C20 C21 C22 119.5(7) ? C20 C21 H21 120.16 ? C22 C21 H21 120.35 ? C21 C22 C23 120.9(7) ? C21 C22 H22 119.75 ? C23 C22 H22 119.37 ? C22 C23 C24 119.6(7) ? C22 C23 H23 120.18 ? C24 C23 H23 120.25 ? C23 C24 C25 120.3(7) ? C23 C24 H24 119.66 ? C25 C24 H24 120.03 ? C20 C25 C24 120.5(7) ? C20 C25 H25 119.37 ? C24 C25 H25 120.11 ? P1 C30 C31 117.8(5) ? P1 C30 C35 122.2(5) ? C31 C30 C35 120.0(6) ? C30 C31 C32 118.9(7) ? C30 C31 H31 120.27 ? C32 C31 H31 120.83 ? C31 C32 C33 120.6(8) ? C31 C32 H32 120.26 ? C33 C32 H32 119.09 ? C32 C33 C34 119.7(8) ? C32 C33 H33 119.71 ? C34 C33 H33 120.61 ? C33 C34 C35 121.2(8) ? C33 C34 H34 119.05 ? C35 C34 H34 119.76 ? C30 C35 C34 119.6(7) ? C30 C35 H35 119.65 ? C34 C35 H35 120.77 ? P2 C40 C41 118.3(5) ? P2 C40 C45 122.3(5) ? C41 C40 C45 119.2(6) ? C40 C41 C42 120.1(6) ? C40 C41 H41 119.69 ? C42 C41 H41 120.24 ? C41 C42 C43 120.7(7) ? C41 C42 H42 119.88 ? C43 C42 H42 119.45 ? C42 C43 C44 120.0(7) ? C42 C43 H43 119.84 ? C44 C43 H43 120.13 ? C43 C44 C45 120.0(7) ? C43 C44 H44 119.77 ? C45 C44 H44 120.18 ? C40 C45 C44 120.0(6) ? C40 C45 H45 119.68 ? C44 C45 H45 120.29 ? P2 C50 C51 122.7(5) ? P2 C50 C55 118.1(5) ? C51 C50 C55 119.1(6) ? C50 C51 C52 120.7(6) ? C50 C51 H51 119.30 ? C52 C51 H51 119.96 ? C51 C52 C53 119.4(6) ? C51 C52 H52 120.63 ? C53 C52 H52 120.02 ? C52 C53 C54 120.2(7) ? C52 C53 H53 119.88 ? C54 C53 H53 119.94 ? C53 C54 C55 120.4(6) ? C53 C54 H54 119.42 ? C55 C54 H54 120.12 ? C50 C55 C54 120.2(6) ? C50 C55 H55 119.82 ? C54 C55 H55 120.00 ? C61 C60 C65 121.0(9) ? C61 C60 H60 119.67 ? C65 C60 H60 119.34 ? C60 C61 C62 119.(1) ? C60 C61 H61 119.72 ? C62 C61 H61 121.01 ? C61 C62 C63 119(1) ? C61 C62 H62 120.86 ? C63 C62 H62 119.65 ? C62 C63 C64 120(1) ? C62 C63 H63 121.27 ? C64 C63 H63 118.57 ? C63 C64 C65 120.(1) ? C63 C64 H64 120.50 ? C65 C64 H64 119.15 ? C60 C65 C64 1191(1) ? C60 C65 H65 119.72 ? C64 C65 H65 120.52 ? C71 C70 C75 120(1) ? C71 C70 H70 120.40 ? C75 C70 H70 119.89 ? C70 C71 C72 120(1) ? C70 C71 H71 120.13 ? C72 C71 H71 119.75 ? C71 C72 C73 121(1) ? C71 C72 H72 119.91 ? C73 C72 H72 119.52 ? C72 C73 C74 119(1) ? C72 C73 H73 120.65 ? C74 C73 H73 120.73 ? C73 C74 C75 120(1) ? C73 C74 H74 120.59 ? C75 C74 H74 119.73 ? C70 C75 C74 121(1) ? C70 C75 H75 119.10 ? C74 C75 H75 119.55 ? C81 C80 C85 120(2) ? C81 C80 H80 129.51 ? C85 C80 H80 110.97 ? C80 C81 C82 120(2) ? C80 C81 H81 111.03 ? C82 C81 H81 129.18 ? C81 C82 C83 119(2) ? C81 C82 H82 113.61 ? C83 C82 H82 127.73 ? C82 C83 C84 122(2) ? C82 C83 H83 110.82 ? C84 C83 H83 126.83 ? C83 C84 C85 117(2) ? C83 C84 H84 114.09 ? C85 C84 H84 128.95 ? C80 C85 C84 123(2) ? C80 C85 H85 125.25 ? C84 C85 H85 111.93 ? #=END data_GW2_180997 # 5. CRYSTAL DATA _chemical_compound_source 'see paper' _exptl_crystal_description 'monoclinic rod' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _chemical_name_common ; Ligand 1d ; _chemical_formula_sum 'C38 H30 O1 P2 S1' _chemical_formula_weight 596.67 _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m 'P21/c' _cell_length_a 11.904(2) _cell_length_b 21.377(2) _cell_length_c 13.285(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.18(1) _cell_angle_gamma 90.00 _cell_volume 3130.4(7) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 21 _cell_measurement_theta_max 29 _cell_formula_units_z 4.00 _exptl_crystal_density_diffrn 1.27 _exptl_crystal_density_meas none _diffrn_radiation_type Cu-K\a _diffrn_radiation_wavelength 1.54184 _exptl_absorpt_coefficient_mu 2.094 _cell_measurement_temperature 293 _exptl_crystal_F_000 1248 # 6. DATA COLLECTION _diffrn_ambient_temperature 293 _diffrn_measurement_device Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.804 _exptl_absorpt_correction_T_max 0.999 _diffrn_reflns_number 9557 _reflns_number_total 6435 _reflns_number_observed 4989 _reflns_observed_criterion >1.0\s(I) _diffrn_reflns_av_R_equivalents 0.059 _diffrn_reflns_theta_min 5.5 _diffrn_reflns_theta_max 74.9 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_max 15 _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% -5.03 # 7. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_R_factor_obs 0.063 _refine_ls_wR_factor_obs 0.063 _refine_ls_hydrogen_treatment refined_isotropically _refine_ls_number_reflns 4989 _refine_ls_number_parameters 499 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_obs 1.280 _refine_ls_weighting_scheme '4Fo^2^/ (\s^2^(Fo^2^) + 0.0016 Fo^4^)' _refine_ls_shift/esd_max 0.021 _refine_diff_density_max 0.3444 _refine_diff_density_min -0.3601 _refine_ls_extinction_method none _atom_type_scat_source International_Tables_for_Xray_Crystallography # 8. COMPUTING DATA _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_reduction PROCESS_MolEN_(Fair,_1990) _computing_structure_solution SHELXS86_(Sheldrick,_1986) _computing_structure_refinement LSFM_MolEN_(Fair,_1990) _computing_molecular_graphics ORTEP_(Johnson,_1976) _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type S 0.89787(8) -0.09456(4) 0.48279(6) 0.0598(2) Ueq P1 0.76643(7) 0.15204(4) 0.51350(6) 0.0464(2) Ueq P2 0.70607(7) 0.10238(3) 0.20518(6) 0.0425(2) Ueq O 0.7862(2) 0.03800(9) 0.4039(1) 0.0613(7) Ueq C1 0.8311(2) 0.0267(1) 0.5136(2) 0.0417(8) Ueq C2 0.8244(2) 0.0761(1) 0.5786(2) 0.0423(8) Ueq C3 0.8627(3) 0.0660(1) 0.6902(2) 0.0506(9) Ueq C4 0.9094(3) 0.0090(1) 0.7377(2) 0.0522(9) Ueq C5 0.9201(3) -0.0382(1) 0.6708(2) 0.0495(9) Ueq C6 0.8809(2) -0.0305(1) 0.5595(2) 0.0426(8) Ueq C7 0.8364(2) -0.0641(1) 0.3499(2) 0.0424(8) Ueq C8 0.8342(3) -0.1023(1) 0.2655(2) 0.0544(9) Ueq C9 0.7912(3) -0.0813(1) 0.1594(2) 0.056(1) Ueq C10 0.7474(3) -0.0204(1) 0.1389(2) 0.0489(9) Ueq C11 0.7481(2) 0.0193(1) 0.2219(2) 0.0404(7) Ueq C12 0.7918(2) -0.0038(1) 0.3272(2) 0.0409(7) Ueq C13 0.9494(3) -0.0005(2) 0.8589(2) 0.074(1) Ueq C14 0.7913(4) -0.1241(2) 0.0682(3) 0.085(1) Ueq C20 0.8657(3) 0.2061(1) 0.6166(2) 0.0475(8) Ueq C21 0.8491(3) 0.2261(2) 0.7094(2) 0.065(1) Ueq C22 0.9362(4) 0.2659(2) 0.7828(3) 0.090(2) Ueq C23 1.0361(4) 0.2845(2) 0.7647(4) 0.096(2) Ueq C24 1.0515(3) 0.2665(2) 0.6731(4) 0.084(1) Ueq C25 0.9660(3) 0.2285(1) 0.5985(3) 0.060(1) Ueq C30 0.6233(3) 0.1570(1) 0.5333(2) 0.0524(9) Ueq C31 0.5674(3) 0.2155(2) 0.5237(3) 0.071(1) Ueq C32 0.4543(3) 0.2213(2) 0.5295(3) 0.092(2) Ueq C33 0.3942(3) 0.1692(2) 0.5429(4) 0.094(2) Ueq C34 0.4457(3) 0.1108(2) 0.5504(3) 0.085(1) Ueq C35 0.5598(3) 0.1048(2) 0.5453(3) 0.065(1) Ueq C40 0.5594(2) 0.1012(1) 0.2192(2) 0.0471(8) Ueq C41 0.4926(3) 0.0476(2) 0.2171(3) 0.067(1) Ueq C42 0.3845(3) 0.0509(2) 0.2336(3) 0.088(1) Ueq C43 0.3422(3) 0.1075(2) 0.2508(3) 0.092(2) Ueq C44 0.4034(3) 0.1606(2) 0.2509(3) 0.083(1) Ueq C45 0.5129(3) 0.1582(2) 0.2361(3) 0.066(1) Ueq C50 0.6661(3) 0.1135(1) 0.0596(2) 0.0437(8) Ueq C51 0.7602(3) 0.1341(2) 0.0290(2) 0.0556(9) Ueq C52 0.7389(3) 0.1472(2) -0.0790(2) 0.073(1) Ueq C53 0.6232(3) 0.1413(2) -0.1578(3) 0.075(1) Ueq C54 0.5305(3) 0.1211(2) -0.1281(3) 0.069(1) Ueq C55 0.5511(3) 0.1070(2) -0.0216(2) 0.056(1) Ueq H3 0.860(2) 0.100(1) 0.737(2) 0.025(8) Uiso H5 0.957(2) -0.077(1) 0.705(2) 0.031(9) Uiso H8 0.866(2) -0.143(1) 0.278(2) 0.022(8) Uiso H10 0.715(2) -0.005(1) 0.068(2) 0.020(8) Uiso H13a 0.892(4) -0.025(2) 0.867(3) 0.11(2) Uiso H13b 0.954(3) 0.039(2) 0.894(3) 0.09(2) Uiso H13c 1.000(4) -0.031(2) 0.872(3) 0.11(2) Uiso H14a 0.853(4) -0.109(2) 0.040(4) 0.12(2) Uiso H14b 0.722(4) -0.128(2) 0.011(4) 0.13(2) Uiso H14c 0.843(4) -0.161(2) 0.096(4) 0.14(2) Uiso H21 0.784(3) 0.210(1) 0.725(2) 0.04(1) Uiso H22 0.910(3) 0.272(2) 0.825(3) 0.06(1) Uiso H23 1.095(3) 0.309(2) 0.818(3) 0.07(1) Uiso H24 1.128(3) 0.286(2) 0.663(3) 0.09(1) Uiso H25 0.975(2) 0.216(1) 0.535(2) 0.030(9) Uiso H31 0.609(3) 0.255(2) 0.508(3) 0.06(1) Uiso H32 0.419(3) 0.262(2) 0.526(3) 0.09(2) Uiso H33 0.313(4) 0.172(3) 0.554(4) 0.16(2) Uiso H34 0.403(3) 0.071(2) 0.564(3) 0.07(1) Uiso H35 0.592(3) 0.063(2) 0.550(2) 0.06(1) Uiso H41 0.530(3) 0.004(2) 0.210(3) 0.07(1) Uiso H42 0.338(3) 0.010(2) 0.240(3) 0.06(1) Uiso H43 0.266(3) 0.110(2) 0.267(3) 0.08(1) Uiso H44 0.372(3) 0.201(2) 0.261(2) 0.05(1) Uiso H45 0.569(3) 0.194(1) 0.242(2) 0.04(1) Uiso H51 0.851(2) 0.141(1) 0.098(2) 0.031(9) Uiso H52 0.814(3) 0.160(2) -0.097(3) 0.06(1) Uiso H53 0.600(3) 0.150(2) -0.241(3) 0.06(1) Uiso H54 0.446(3) 0.117(1) -0.190(2) 0.04(1) Uiso H55 0.485(2) 0.091(1) 0.000(2) 0.016(7) Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S 0.0804(5) 0.0420(4) 0.0547(4) 0.0160(4) 0.0230(3) 0.0115(3) P1 0.0565(4) 0.0401(4) 0.0376(3) 0.0028(3) 0.0121(3) 0.0011(3) P2 0.0482(3) 0.0367(3) 0.0387(3) -0.0027(3) 0.0121(2) 0.0020(3) O 0.095(1) 0.043(1) 0.0366(9) 0.022(1) 0.0147(9) 0.0035(9) C1 0.044(1) 0.043(1) 0.035(1) -0.000(1) 0.011(1) 0.004(1) C2 0.046(1) 0.038(1) 0.039(1) 0.001(1) 0.012(1) 0.005(1) C3 0.060(2) 0.049(2) 0.038(1) -0.000(1) 0.013(1) 0.002(1) C4 0.054(2) 0.056(2) 0.042(1) -0.005(1) 0.013(1) 0.009(1) C5 0.047(1) 0.050(2) 0.047(1) 0.000(1) 0.013(1) 0.015(1) C6 0.038(1) 0.042(1) 0.044(1) -0.002(1) 0.011(1) 0.005(1) C7 0.038(1) 0.038(1) 0.047(1) -0.001(1) 0.011(1) 0.003(1) C8 0.056(2) 0.041(1) 0.057(2) 0.008(1) 0.012(1) -0.004(1) C9 0.056(2) 0.050(2) 0.056(2) 0.006(1) 0.014(1) -0.011(1) C10 0.048(2) 0.053(2) 0.040(1) 0.002(1) 0.010(1) -0.002(1) C11 0.036(1) 0.038(1) 0.042(1) -0.001(1) 0.009(1) -0.001(1) C12 0.041(1) 0.037(1) 0.041(1) 0.001(1) 0.011(1) -0.001(1) C13 0.100(2) 0.072(2) 0.043(1) 0.004(2) 0.019(1) 0.013(2) C14 0.104(3) 0.069(2) 0.065(2) 0.021(2) 0.012(2) -0.023(2) C20 0.053(2) 0.036(1) 0.048(1) 0.004(1) 0.013(1) 0.002(1) C21 0.088(2) 0.059(2) 0.045(1) -0.002(2) 0.021(1) -0.006(2) C22 0.129(3) 0.065(2) 0.054(2) 0.010(2) 0.008(2) -0.015(2) C23 0.089(3) 0.051(2) 0.100(3) -0.001(2) -0.020(2) -0.013(2) C24 0.064(2) 0.042(2) 0.122(3) -0.004(2) 0.009(2) -0.006(2) C25 0.058(2) 0.040(2) 0.080(2) 0.009(1) 0.022(1) 0.003(2) C30 0.051(2) 0.053(2) 0.045(1) -0.000(1) 0.009(1) -0.005(1) C31 0.059(2) 0.057(2) 0.090(2) 0.004(2) 0.019(2) -0.010(2) C32 0.062(2) 0.086(3) 0.116(3) 0.015(2) 0.021(2) -0.020(2) C33 0.054(2) 0.116(3) 0.108(3) -0.001(2) 0.025(2) -0.022(3) C34 0.061(2) 0.100(3) 0.092(2) -0.017(2) 0.025(2) -0.006(2) C35 0.059(2) 0.060(2) 0.068(2) -0.006(2) 0.014(1) -0.004(2) C40 0.053(1) 0.049(2) 0.038(1) 0.008(1) 0.016(1) 0.007(1) C41 0.055(2) 0.062(2) 0.086(2) 0.001(2) 0.030(1) 0.016(2) C42 0.062(2) 0.100(3) 0.105(2) 0.004(2) 0.033(2) 0.031(2) C43 0.059(2) 0.146(4) 0.073(2) 0.020(2) 0.028(1) 0.011(2) C44 0.067(2) 0.098(3) 0.074(2) 0.033(2) 0.017(2) -0.014(2) C45 0.067(2) 0.066(2) 0.060(2) 0.012(2) 0.018(1) -0.004(2) C50 0.051(1) 0.036(1) 0.040(1) -0.001(1) 0.013(1) 0.003(1) C51 0.058(2) 0.058(2) 0.053(1) -0.004(1) 0.023(1) 0.004(1) C52 0.086(2) 0.087(3) 0.057(2) -0.014(2) 0.039(1) -0.001(2) C53 0.094(2) 0.087(3) 0.042(1) -0.012(2) 0.023(1) 0.005(2) C54 0.075(2) 0.077(2) 0.043(2) -0.007(2) 0.007(1) 0.000(2) C55 0.056(2) 0.057(2) 0.048(1) -0.008(2) 0.013(1) 0.001(1) # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag S C6 1.763(3) ? S C7 1.760(3) ? P1 C2 1.846(3) ? P1 C20 1.841(3) ? P1 C30 1.823(3) ? P2 C11 1.836(3) ? P2 C40 1.824(3) ? P2 C50 1.824(3) ? O C1 1.371(3) ? O C12 1.375(3) ? C1 C2 1.387(3) ? C1 C6 1.395(3) ? C2 C3 1.394(4) ? C3 C4 1.387(4) ? C3 H3 0.97(3) ? C4 C5 1.383(4) ? C4 C13 1.510(4) ? C5 C6 1.382(4) ? C5 H5 0.97(3) ? C7 C8 1.380(4) ? C7 C12 1.385(3) ? C8 C9 1.381(4) ? C8 H8 0.93(3) ? C9 C10 1.390(4) ? C9 C14 1.518(5) ? C10 C11 1.388(4) ? C10 H10 0.94(3) ? C11 C12 1.386(3) ? C13 H13a 0.90(5) ? C13 H13b 0.96(5) ? C13 H13c 0.86(5) ? C14 H14a 1.00(5) ? C14 H14b 0.89(6) ? C14 H14c 0.98(6) ? C20 C21 1.387(4) ? C20 C25 1.389(4) ? C21 C22 1.410(6) ? C21 H21 0.95(3) ? C22 C23 1.359(7) ? C22 H22 0.75(4) ? C23 C24 1.353(6) ? C23 H23 0.95(4) ? C24 C25 1.384(5) ? C24 H24 1.06(4) ? C25 H25 0.93(3) ? C30 C31 1.398(4) ? C30 C35 1.392(4) ? C31 C32 1.383(5) ? C31 H31 1.04(4) ? C32 C33 1.372(6) ? C32 H32 0.96(4) ? C33 C34 1.378(6) ? C33 H33 1.03(6) ? C34 C35 1.390(5) ? C34 H34 1.03(4) ? C35 H35 0.97(4) ? C40 C41 1.389(4) ? C40 C45 1.392(4) ? C41 C42 1.386(5) ? C41 H41 1.05(4) ? C42 C43 1.363(6) ? C42 H42 1.04(4) ? C43 C44 1.348(6) ? C43 H43 1.01(4) ? C44 C45 1.391(5) ? C44 H44 0.98(4) ? C45 H45 0.99(3) ? C50 C51 1.400(4) ? C50 C55 1.393(4) ? C51 C52 1.387(4) ? C51 H51 1.13(3) ? C52 C53 1.385(5) ? C52 H52 1.05(4) ? C53 C54 1.374(5) ? C53 H53 1.05(4) ? C54 C55 1.375(4) ? C54 H54 1.04(3) ? C55 H55 1.00(3) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C6 S C7 101.4(1) ? C2 P1 C20 100.5(1) ? C2 P1 C30 100.8(1) ? C20 P1 C30 103.2(1) ? C11 P2 C40 101.6(1) ? C11 P2 C50 101.8(1) ? C40 P2 C50 103.5(1) ? C1 O C12 124.3(2) ? O C1 C2 115.9(2) ? O C1 C6 123.4(2) ? C2 C1 C6 120.7(2) ? P1 C2 C1 118.5(2) ? P1 C2 C3 123.3(2) ? C1 C2 C3 118.2(2) ? C2 C3 C4 122.2(3) ? C2 C3 H3 119(2) ? C4 C3 H3 118(2) ? C3 C4 C5 117.9(3) ? C3 C4 C13 120.9(3) ? C5 C4 C13 121.2(3) ? C4 C5 C6 121.6(3) ? C4 C5 H5 117(2) ? C6 C5 H5 121(2) ? S C6 C1 123.4(2) ? S C6 C5 117.3(2) ? C1 C6 C5 119.2(3) ? S C7 C8 118.0(2) ? S C7 C12 122.9(2) ? C8 C7 C12 119.1(3) ? C7 C8 C9 121.5(3) ? C7 C8 H8 121(2) ? C9 C8 H8 117(2) ? C8 C9 C10 118.1(3) ? C8 C9 C14 120.4(3) ? C10 C9 C14 121.5(3) ? C9 C10 C11 121.8(3) ? C9 C10 H10 121(2) ? C11 C10 H10 117(2) ? P2 C11 C10 125.1(2) ? P2 C11 C12 116.5(2) ? C10 C11 C12 118.2(2) ? O C12 C7 124.4(2) ? O C12 C11 114.4(2) ? C7 C12 C11 121.2(2) ? C4 C13 H13a 105(3) ? C4 C13 H13b 110(3) ? C4 C13 H13c 103(3) ? H13a C13 H13b 111(4) ? H13a C13 H13c 92(4) ? H13b C13 H13c 132(4) ? C9 C14 H14a 109(3) ? C9 C14 H14b 117(4) ? C9 C14 H14c 112(3) ? H14a C14 H14b 107(5) ? H14a C14 H14c 87(4) ? H14b C14 H14c 120(5) ? P1 C20 C21 126.0(3) ? P1 C20 C25 116.1(2) ? C21 C20 C25 117.9(3) ? C20 C21 C22 119.1(4) ? C20 C21 H21 120(2) ? C22 C21 H21 121(2) ? C21 C22 C23 121.2(4) ? C21 C22 H22 103(4) ? C23 C22 H22 136(4) ? C22 C23 C24 120.1(4) ? C22 C23 H23 119(3) ? C24 C23 H23 121(3) ? C23 C24 C25 119.8(4) ? C23 C24 H24 115(2) ? C25 C24 H24 125(2) ? C20 C25 C24 121.8(4) ? C20 C25 H25 117(2) ? C24 C25 H25 121(2) ? P1 C30 C31 118.5(3) ? P1 C30 C35 123.2(3) ? C31 C30 C35 117.9(3) ? C30 C31 C32 121.0(4) ? C30 C31 H31 120(2) ? C32 C31 H31 119(2) ? C31 C32 C33 120.0(4) ? C31 C32 H32 119(3) ? C33 C32 H32 121(3) ? C32 C33 C34 120.4(4) ? C32 C33 H33 122(3) ? C34 C33 H33 117(3) ? C33 C34 C35 119.8(4) ? C33 C34 H34 121(2) ? C35 C34 H34 119(2) ? C30 C35 C34 120.9(4) ? C30 C35 H35 122(2) ? C34 C35 H35 117(2) ? P2 C40 C41 124.9(2) ? P2 C40 C45 117.3(3) ? C41 C40 C45 117.7(3) ? C40 C41 C42 121.0(4) ? C40 C41 H41 118(2) ? C42 C41 H41 120(2) ? C41 C42 C43 119.6(4) ? C41 C42 H42 121(2) ? C43 C42 H42 119(2) ? C42 C43 C44 121.0(4) ? C42 C43 H43 120(2) ? C44 C43 H43 119(2) ? C43 C44 C45 120.2(4) ? C43 C44 H44 121(2) ? C45 C44 H44 119(2) ? C40 C45 C44 120.5(4) ? C40 C45 H45 113(2) ? C44 C45 H45 127(2) ? P2 C50 C51 115.6(2) ? P2 C50 C55 126.5(2) ? C51 C50 C55 117.8(3) ? C50 C51 C52 120.7(3) ? C50 C51 H51 116(1) ? C52 C51 H51 124(1) ? C51 C52 C53 120.3(3) ? C51 C52 H52 117(2) ? C53 C52 H52 123(2) ? C52 C53 C54 119.2(3) ? C52 C53 H53 125(2) ? C54 C53 H53 116(2) ? C53 C54 C55 120.9(3) ? C53 C54 H54 116(2) ? C55 C54 H54 123(2) ? C50 C55 C54 121.1(3) ? C50 C55 H55 118(2) ? C54 C55 H55 121(2) ? #=END data_GW4_081297 # 5. CRYSTAL DATA _chemical_compound_source 'see paper' _exptl_crystal_description 'irregular fragment' _exptl_crystal_colour red _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.28 _chemical_name_common ; Complex 4 ; _chemical_formula_sum 'C62 H66 N6 Ni1 O1 P2 S1' _chemical_formula_weight 1063.98 _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'P-1' _cell_length_a 11.436(5) _cell_length_b 12.496(3) _cell_length_c 21.699(8) _cell_angle_alpha 77.20(2) _cell_angle_beta 86.18(3) _cell_angle_gamma 65.86(2) _cell_volume 2758(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9 _cell_measurement_theta_max 12 _cell_formula_units_z 2.00 _exptl_crystal_density_diffrn 1.28 _exptl_crystal_density_meas none _diffrn_radiation_type Mo-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.491 _cell_measurement_temperature 203 _exptl_crystal_F_000 1124 # 6. DATA COLLECTION _diffrn_ambient_temperature 203 _diffrn_measurement_device Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.000 _exptl_absorpt_correction_T_max 0.000 _diffrn_reflns_number 10824 _reflns_number_total 9678 _reflns_number_observed 7164 _reflns_observed_criterion >1.0\s(I) _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_theta_min 2.1 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% -5.64 # 7. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_R_factor_obs 0.081 _refine_ls_wR_factor_obs 0.072 _refine_ls_hydrogen_treatment riding _refine_ls_number_reflns 7164 _refine_ls_number_parameters 658 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_obs 1.414 _refine_ls_weighting_scheme '4Fo^2^/ (\s^2^(Fo^2^) + 0.0016 Fo^4^)' _refine_ls_shift/esd_max 0.013 _refine_diff_density_max 0.7247 _refine_diff_density_min -0.5293 _refine_ls_extinction_method none _atom_type_scat_source International_Tables_for_Xray_Crystallography # 8. COMPUTING DATA _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_reduction PROCESS_MolEN_(Fair,_1990) _computing_structure_solution SHELXS86_(Sheldrick,_1986) _computing_structure_refinement LSFM_MolEN_(Fair,_1990) _computing_molecular_graphics ORTEP_(Johnson,_1976) _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Ni 0.06790(6) 0.15381(5) 0.22161(3) 0.0258(2) Ueq . S 0.5773(1) -0.1375(1) 0.30410(9) 0.0550(5) Ueq . P1 0.1517(1) 0.2864(1) 0.21615(6) 0.0267(4) Ueq . P2 0.0653(1) -0.0233(1) 0.26012(6) 0.0271(4) Ueq . O 0.2973(3) 0.0214(3) 0.2843(2) 0.031(1) Ueq . N1 0.2268(4) 0.0621(4) 0.1131(2) 0.050(2) Ueq . N2 -0.1735(4) 0.2835(4) 0.2855(2) 0.050(2) Ueq . N3 0.1441(4) 0.6506(4) -0.0193(2) 0.054(2) Ueq . N4 0.0153(5) 0.5677(4) 0.4215(2) 0.056(2) Ueq . N5 -0.1151(4) -0.1090(4) 0.5263(2) 0.044(2) Ueq . N6 -0.2071(4) -0.2046(4) 0.1088(2) 0.044(1) Ueq . C1 0.1717(4) 0.0933(4) 0.1568(2) 0.030(1) Ueq . C2 -0.0768(4) 0.2319(4) 0.2651(2) 0.033(2) Ueq . C10 0.3790(4) 0.0774(4) 0.2573(2) 0.031(1) Ueq . C11 0.3257(4) 0.1975(4) 0.2265(2) 0.027(1) Ueq . C12 0.4100(4) 0.2524(4) 0.2033(2) 0.034(2) Ueq . C13 0.5416(4) 0.1903(4) 0.2083(2) 0.035(2) Ueq . C14 0.5912(4) 0.0692(5) 0.2378(3) 0.039(2) Ueq . C15 0.5099(4) 0.0137(4) 0.2629(3) 0.036(2) Ueq . C16 0.4563(5) -0.1802(4) 0.2870(3) 0.039(2) Ueq . C17 0.4859(5) -0.2973(5) 0.2837(3) 0.047(2) Ueq . C18 0.3920(5) -0.3370(5) 0.2747(3) 0.047(2) Ueq . C19 0.2656(5) -0.2508(4) 0.2666(3) 0.038(2) Ueq . C20 0.2330(4) -0.1305(4) 0.2672(2) 0.032(2) Ueq . C21 0.3307(4) -0.0957(4) 0.2785(2) 0.032(2) Ueq . C22 0.6289(5) 0.2511(5) 0.1800(3) 0.050(2) Ueq . C23 0.4251(6) -0.4652(5) 0.2747(3) 0.062(2) Ueq . C30 0.1384(4) 0.4001(4) 0.1454(2) 0.028(1) Ueq . C31 0.1508(5) 0.3734(4) 0.0866(3) 0.038(2) Ueq . C32 0.1524(5) 0.4561(5) 0.0324(3) 0.041(2) Ueq . C33 0.1422(5) 0.5696(5) 0.0350(3) 0.040(2) Ueq . C34 0.1285(5) 0.5978(4) 0.0947(3) 0.043(2) Ueq . C35 0.1271(5) 0.5142(4) 0.1485(3) 0.035(2) Ueq . C36 0.1513(6) 0.7637(5) -0.0146(3) 0.068(2) Ueq . C37 0.1555(6) 0.6232(6) -0.0808(3) 0.061(2) Ueq . C40 0.1138(4) 0.3663(4) 0.2798(2) 0.030(1) Ueq . C41 -0.0135(5) 0.4461(4) 0.2859(2) 0.033(2) Ueq . C42 -0.0460(5) 0.5119(4) 0.3322(3) 0.042(2) Ueq . C43 0.0470(5) 0.5038(4) 0.3744(3) 0.039(2) Ueq . C44 0.1716(5) 0.4227(5) 0.3680(3) 0.049(2) Ueq . C45 0.2039(5) 0.3570(4) 0.3219(3) 0.037(2) Ueq . C46 -0.1101(7) 0.6635(5) 0.4218(3) 0.068(2) Ueq . C47 0.1160(7) 0.5731(5) 0.4558(3) 0.073(2) Ueq . C50 0.0135(4) -0.0503(4) 0.3404(2) 0.026(1) Ueq . C51 0.0995(5) -0.1140(4) 0.3915(2) 0.033(2) Ueq . C52 0.0576(5) -0.1305(4) 0.4527(2) 0.035(2) Ueq . C53 -0.0740(5) -0.0868(4) 0.4663(2) 0.036(2) Ueq . C54 -0.1606(5) -0.0196(4) 0.4146(2) 0.033(2) Ueq . C55 -0.1181(4) -0.0022(4) 0.3540(2) 0.033(2) Ueq . C56 -0.0254(6) -0.1771(5) 0.5787(3) 0.052(2) Ueq . C57 -0.2491(6) -0.0471(6) 0.5409(3) 0.072(2) Ueq . C60 -0.0160(4) -0.0789(4) 0.2157(2) 0.029(1) Ueq . C61 -0.0582(4) -0.1689(4) 0.2432(2) 0.034(2) Ueq . C62 -0.1192(4) -0.2114(4) 0.2084(3) 0.035(2) Ueq . C63 -0.1430(4) -0.1653(4) 0.1428(2) 0.035(2) Ueq . C64 -0.0993(5) -0.0754(4) 0.1157(3) 0.040(2) Ueq . C65 -0.0398(5) -0.0336(4) 0.1506(2) 0.035(2) Ueq . C66 -0.2079(6) -0.1776(5) 0.0401(3) 0.056(2) Ueq . C67 -0.2483(6) -0.2993(5) 0.1388(3) 0.066(2) Ueq . C70 0.4714(5) 0.8022(5) -0.0059(3) 0.050(2) Ueq . C71 0.5202(6) 0.6807(6) -0.0057(3) 0.073(2) Ueq . C72 0.5067(8) 0.6001(6) 0.0452(4) 0.099(3) Ueq . C73 0.4457(8) 0.6386(7) 0.0980(4) 0.096(3) Ueq . C74 0.3970(7) 0.7598(6) 0.0990(3) 0.076(3) Ueq . C75 0.4122(6) 0.8397(5) 0.0471(3) 0.054(2) Ueq . C76 0.4846(6) 0.8911(6) -0.0623(3) 0.073(3) Ueq . C80 0.3936(6) 0.6632(6) 0.5582(4) 0.085(3) Ueq . C81 0.4284(7) 0.7273(6) 0.5903(4) 0.087(3) Ueq . C82 0.5015(8) 0.7893(8) 0.5672(5) 0.132(5) Ueq . C83 0.5391(9) 0.7817(8) 0.5043(5) 0.126(5) Ueq . C84 0.5024(8) 0.7197(8) 0.4684(4) 0.107(4) Ueq . C85 0.4330(8) 0.6593(8) 0.4928(4) 0.100(4) Ueq . C86 0.3234(9) 0.5894(9) 0.5850(5) 0.133(5) Ueq . H12 0.3732 0.3372 0.1817 0.0447 Uiso calc H14 0.6845 0.0241 0.2405 0.0513 Uiso calc H17 0.5768 -0.3520 0.2889 0.0615 Uiso calc H19 0.1957 -0.2739 0.2606 0.0489 Uiso calc H22a 0.6904 0.2775 0.1941 0.0647 Uiso calc H22b 0.5681 0.3287 0.1565 0.0647 Uiso calc H22c 0.6770 0.2068 0.1481 0.0647 Uiso calc H23a 0.5152 -0.5220 0.2770 0.0802 Uiso calc H23b 0.3891 -0.4694 0.2361 0.0802 Uiso calc H23c 0.3841 -0.4982 0.3105 0.0802 Uiso calc H31 0.1630 0.2924 0.0836 0.0499 Uiso calc H32 0.1594 0.4350 -0.0090 0.0531 Uiso calc H34 0.1210 0.6774 0.0979 0.0559 Uiso calc H35 0.1181 0.5354 0.1899 0.0458 Uiso calc H36a 0.0652 0.8247 -0.0278 0.0885 Uiso calc H36b 0.2147 0.7787 -0.0438 0.0885 Uiso calc H36c 0.1767 0.7608 0.0282 0.0885 Uiso calc H37a 0.2017 0.5396 -0.0847 0.0794 Uiso calc H37b 0.1987 0.6701 -0.1069 0.0794 Uiso calc H37c 0.0678 0.6511 -0.0972 0.0794 Uiso calc H41 -0.0809 0.4555 0.2570 0.0432 Uiso calc H42 -0.1355 0.5670 0.3352 0.0540 Uiso calc H44 0.2392 0.4080 0.3982 0.0633 Uiso calc H45 0.2934 0.3023 0.3188 0.0484 Uiso calc H46a -0.1392 0.6960 0.4599 0.0885 Uiso calc H46b -0.1749 0.6361 0.4128 0.0885 Uiso calc H46c -0.1176 0.7321 0.3876 0.0885 Uiso calc H47a 0.1946 0.5004 0.4568 0.0950 Uiso calc H47b 0.0932 0.5758 0.5000 0.0950 Uiso calc H47c 0.1350 0.6430 0.4373 0.0950 Uiso calc H51 0.1918 -0.1460 0.3841 0.0433 Uiso calc H52 0.1209 -0.1732 0.4876 0.0448 Uiso calc H54 -0.2529 0.0148 0.4219 0.0429 Uiso calc H55 -0.1813 0.0448 0.3194 0.0435 Uiso calc H56a 0.0301 -0.2538 0.5677 0.0681 Uiso calc H56b -0.0675 -0.1963 0.6179 0.0681 Uiso calc H56c 0.0298 -0.1387 0.5867 0.0681 Uiso calc H57a -0.2799 0.0375 0.5433 0.0934 Uiso calc H57b -0.2693 -0.0872 0.5818 0.0934 Uiso calc H57c -0.3052 -0.0457 0.5083 0.0934 Uiso calc H61 -0.0427 -0.2030 0.2886 0.0437 Uiso calc H62 -0.1472 -0.2745 0.2293 0.0456 Uiso calc H64 -0.1120 -0.0416 0.0701 0.0524 Uiso calc H65 -0.0116 0.0298 0.1303 0.0455 Uiso calc H66a -0.2466 -0.0896 0.0301 0.0730 Uiso calc H66b -0.2595 -0.2090 0.0213 0.0730 Uiso calc H66c -0.1214 -0.2069 0.0233 0.0730 Uiso calc H67a -0.3291 -0.2672 0.1606 0.0857 Uiso calc H67b -0.1843 -0.3584 0.1707 0.0857 Uiso calc H67c -0.2600 -0.3405 0.1077 0.0857 Uiso calc H71 0.5692 0.6496 -0.0413 0.0950 Uiso calc H72 0.5344 0.5152 0.0444 0.1281 Uiso calc H73 0.4418 0.5809 0.1361 0.1253 Uiso calc H74 0.3487 0.7897 0.1351 0.0988 Uiso calc H75 0.3797 0.9249 0.0484 0.0698 Uiso calc H76a 0.4723 0.9752 -0.0685 0.0945 Uiso calc H76b 0.4261 0.8930 -0.0940 0.0945 Uiso calc H76c 0.5733 0.8517 -0.0749 0.0945 Uiso calc H81 0.3971 0.7359 0.6328 0.1133 Uiso calc H82 0.5337 0.8324 0.5895 0.1721 Uiso calc H83 0.5917 0.8226 0.4820 0.1642 Uiso calc H84 0.5314 0.7236 0.4247 0.1392 Uiso calc H85 0.4070 0.6169 0.4673 0.1295 Uiso calc H86a 0.3068 0.5479 0.5554 0.1734 Uiso calc H86b 0.3701 0.5250 0.6207 0.1734 Uiso calc H86c 0.2403 0.6336 0.6020 0.1734 Uiso calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni 0.0282(3) 0.0270(2) 0.0231(3) -0.0129(2) 0.0003(2) -0.0035(2) S 0.0322(6) 0.0465(8) 0.073(1) -0.0149(5) -0.0169(7) 0.0159(8) P1 0.0282(5) 0.0275(5) 0.0240(7) -0.0124(4) 0.0001(5) -0.0023(5) P2 0.0303(6) 0.0280(5) 0.0235(7) -0.0134(4) -0.0005(5) -0.0032(5) O 0.029(1) 0.031(1) 0.033(2) -0.016(1) -0.000(1) -0.000(1) N1 0.067(3) 0.046(2) 0.040(3) -0.026(2) 0.018(2) -0.014(2) N2 0.046(2) 0.050(2) 0.055(3) -0.018(2) 0.010(2) -0.020(2) N3 0.069(3) 0.049(2) 0.039(3) -0.031(2) -0.000(2) 0.013(2) N4 0.076(3) 0.053(2) 0.050(3) -0.030(2) 0.014(2) -0.029(2) N5 0.056(2) 0.051(2) 0.023(2) -0.023(2) 0.005(2) -0.004(2) N6 0.056(2) 0.045(2) 0.040(3) -0.029(1) -0.011(2) -0.008(2) C1 0.042(2) 0.023(2) 0.027(3) -0.017(2) -0.005(2) 0.002(2) C2 0.032(2) 0.033(2) 0.033(3) -0.014(2) -0.002(2) -0.006(2) C10 0.029(2) 0.040(2) 0.029(3) -0.020(2) 0.003(2) -0.009(2) C11 0.028(2) 0.031(2) 0.022(2) -0.011(2) 0.002(2) -0.007(2) C12 0.037(2) 0.040(2) 0.031(3) -0.021(2) 0.001(2) -0.010(2) C13 0.028(2) 0.042(2) 0.035(3) -0.015(2) -0.002(2) -0.007(2) C14 0.029(2) 0.047(3) 0.045(3) -0.017(2) -0.001(2) -0.010(2) C15 0.032(2) 0.035(2) 0.038(3) -0.016(2) -0.006(2) 0.004(2) C16 0.032(2) 0.038(3) 0.037(3) -0.013(2) -0.003(2) 0.011(2) C17 0.037(3) 0.036(3) 0.054(4) -0.006(2) -0.000(3) 0.004(3) C18 0.051(3) 0.032(3) 0.049(4) -0.012(2) 0.007(3) -0.002(3) C19 0.043(3) 0.027(2) 0.040(3) -0.014(2) 0.001(2) -0.002(2) C20 0.027(2) 0.033(2) 0.029(3) -0.008(2) 0.000(2) -0.000(2) C21 0.031(2) 0.029(2) 0.030(3) -0.009(2) -0.001(2) 0.001(2) C22 0.035(2) 0.052(3) 0.075(4) -0.031(2) 0.010(3) -0.015(3) C23 0.058(3) 0.032(3) 0.088(5) -0.011(2) -0.002(4) -0.010(3) C30 0.026(2) 0.026(2) 0.028(3) -0.011(2) 0.002(2) -0.000(2) C31 0.050(3) 0.033(2) 0.035(3) -0.021(2) 0.007(2) -0.004(2) C32 0.050(3) 0.045(3) 0.026(3) -0.023(2) -0.001(2) 0.002(2) C33 0.030(2) 0.045(3) 0.038(3) -0.015(2) -0.002(2) 0.006(3) C34 0.050(3) 0.027(2) 0.047(4) -0.018(2) 0.001(3) 0.005(2) C35 0.038(2) 0.031(2) 0.035(3) -0.015(2) -0.001(2) -0.001(2) C36 0.084(4) 0.056(3) 0.060(4) -0.039(2) -0.002(3) 0.020(3) C37 0.069(3) 0.080(4) 0.037(4) -0.043(2) -0.003(3) 0.010(3) C40 0.036(2) 0.029(2) 0.025(3) -0.017(2) 0.002(2) -0.000(2) C41 0.038(2) 0.027(2) 0.030(3) -0.009(2) -0.001(2) -0.003(2) C42 0.049(3) 0.033(3) 0.037(3) -0.013(2) 0.006(3) -0.003(2) C43 0.059(3) 0.032(2) 0.032(3) -0.024(2) 0.010(2) -0.010(2) C44 0.060(3) 0.063(3) 0.037(3) -0.032(2) -0.002(2) -0.021(2) C45 0.038(2) 0.043(2) 0.035(3) -0.022(2) -0.001(2) -0.007(2) C46 0.108(5) 0.045(3) 0.057(4) -0.033(3) 0.028(4) -0.027(3) C47 0.117(4) 0.071(3) 0.055(4) -0.055(3) 0.002(3) -0.027(3) C50 0.035(2) 0.030(2) 0.018(2) -0.018(2) 0.000(2) -0.004(2) C51 0.040(2) 0.037(2) 0.025(3) -0.017(2) -0.001(2) -0.007(2) C52 0.049(3) 0.029(2) 0.023(3) -0.015(2) -0.007(2) 0.001(2) C53 0.061(3) 0.032(2) 0.025(3) -0.030(2) 0.003(2) -0.006(2) C54 0.043(2) 0.039(2) 0.023(3) -0.023(2) 0.001(2) -0.007(2) C55 0.033(2) 0.041(2) 0.028(3) -0.018(2) 0.001(2) -0.006(2) C56 0.078(3) 0.057(3) 0.029(3) -0.038(2) 0.004(3) -0.001(3) C57 0.069(3) 0.127(5) 0.031(3) -0.056(3) 0.010(3) -0.009(3) C60 0.036(2) 0.028(2) 0.023(3) -0.014(2) -0.002(2) -0.004(2) C61 0.035(2) 0.035(2) 0.029(3) -0.016(2) -0.000(2) 0.000(2) C62 0.043(2) 0.038(2) 0.035(3) -0.028(2) -0.003(2) -0.006(2) C63 0.030(2) 0.034(2) 0.039(3) -0.009(2) -0.006(2) -0.011(2) C64 0.052(3) 0.041(2) 0.031(3) -0.024(2) -0.011(2) 0.001(2) C65 0.045(2) 0.032(2) 0.029(3) -0.019(2) -0.004(2) -0.001(2) C66 0.076(3) 0.067(3) 0.038(3) -0.037(2) -0.014(3) -0.015(2) C67 0.088(3) 0.072(3) 0.063(4) -0.060(2) -0.015(3) -0.005(3) C70 0.036(3) 0.062(3) 0.061(4) -0.019(2) -0.003(3) -0.030(2) C71 0.054(4) 0.072(4) 0.093(5) -0.009(3) -0.006(3) -0.049(3) C72 0.099(5) 0.054(4) 0.129(7) -0.011(3) -0.045(5) -0.018(4) C73 0.121(5) 0.078(4) 0.087(6) -0.050(3) -0.042(4) 0.019(4) C74 0.081(4) 0.078(4) 0.061(5) -0.030(3) -0.000(4) -0.005(4) C75 0.053(3) 0.057(3) 0.051(4) -0.019(2) 0.004(3) -0.020(3) C76 0.068(3) 0.105(4) 0.063(4) -0.048(3) 0.013(3) -0.030(3) C80 0.052(4) 0.056(4) 0.111(6) -0.007(3) -0.010(4) 0.027(4) C81 0.067(5) 0.047(4) 0.113(6) 0.007(4) -0.022(5) -0.002(4) C82 0.086(6) 0.093(6) 0.18(1) -0.012(5) -0.053(6) 0.016(7) C83 0.090(6) 0.094(6) 0.159(9) -0.017(5) -0.011(6) 0.006(7) C84 0.097(6) 0.093(6) 0.105(7) -0.023(5) 0.020(5) -0.006(5) C85 0.092(6) 0.086(6) 0.082(6) -0.009(5) 0.004(5) 0.005(5) C86 0.091(6) 0.119(7) 0.159(9) -0.013(6) 0.006(7) -0.030(7) # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Ni P1 2.208(1) ? Ni P2 2.197(1) ? Ni C1 1.863(5) ? Ni C2 1.861(5) ? S C15 1.764(5) ? S C16 1.760(5) ? P1 C11 1.840(4) ? P1 C30 1.813(4) ? P1 C40 1.808(5) ? P2 C20 1.829(4) ? P2 C50 1.806(4) ? P2 C60 1.795(4) ? O C10 1.410(5) ? O C21 1.385(5) ? N1 C1 1.154(6) ? N2 C2 1.145(6) ? N3 C33 1.379(6) ? N3 C36 1.475(7) ? N3 C37 1.434(7) ? N4 C43 1.375(6) ? N4 C46 1.445(7) ? N4 C47 1.443(7) ? N5 C53 1.363(6) ? N5 C56 1.442(6) ? N5 C57 1.457(7) ? N6 C63 1.359(6) ? N6 C66 1.454(6) ? N6 C67 1.456(6) ? C10 C11 1.389(6) ? C10 C15 1.378(6) ? C11 C12 1.406(6) ? C12 C13 1.382(6) ? C12 H12 0.9800 ? C13 C14 1.392(7) ? C13 C22 1.511(6) ? C14 C15 1.391(6) ? C14 H14 0.9801 ? C16 C17 1.377(7) ? C16 C21 1.386(6) ? C17 C18 1.394(7) ? C17 H17 0.9799 ? C18 C19 1.399(7) ? C18 C23 1.488(7) ? C19 C20 1.395(6) ? C19 H19 0.9800 ? C20 C21 1.408(6) ? C22 H22a 0.9800 ? C22 H22b 0.9801 ? C22 H22c 0.9798 ? C23 H23a 0.9800 ? C23 H23b 0.9801 ? C23 H23c 0.9800 ? C30 C31 1.373(6) ? C30 C35 1.395(6) ? C31 C32 1.389(6) ? C31 H31 0.9800 ? C32 C33 1.388(7) ? C32 H32 0.9800 ? C33 C34 1.400(7) ? C34 C35 1.387(6) ? C34 H34 0.9799 ? C35 H35 0.9800 ? C36 H36a 0.9797 ? C36 H36b 0.9802 ? C36 H36c 0.9801 ? C37 H37a 0.9801 ? C37 H37b 0.9800 ? C37 H37c 0.9799 ? C40 C41 1.405(6) ? C40 C45 1.375(6) ? C41 C42 1.375(6) ? C41 H41 0.9802 ? C42 C43 1.408(7) ? C42 H42 0.9802 ? C43 C44 1.389(7) ? C44 C45 1.370(7) ? C44 H44 0.9801 ? C45 H45 0.9798 ? C46 H46a 0.9800 ? C46 H46b 0.9799 ? C46 H46c 0.9800 ? C47 H47a 0.9797 ? C47 H47b 0.9802 ? C47 H47c 0.9800 ? C50 C51 1.394(6) ? C50 C55 1.412(6) ? C51 C52 1.382(6) ? C51 H51 0.9798 ? C52 C53 1.411(6) ? C52 H52 0.9801 ? C53 C54 1.412(6) ? C54 C55 1.375(6) ? C54 H54 0.9799 ? C55 H55 0.9801 ? C56 H56a 0.9800 ? C56 H56b 0.9800 ? C56 H56c 0.9799 ? C57 H57a 0.9798 ? C57 H57b 0.9801 ? C57 H57c 0.9800 ? C60 C61 1.401(6) ? C60 C65 1.401(6) ? C61 C62 1.374(6) ? C61 H61 0.9800 ? C62 C63 1.412(6) ? C62 H62 0.9800 ? C63 C64 1.409(6) ? C64 C65 1.358(6) ? C64 H64 0.9800 ? C65 H65 0.9799 ? C66 H66a 0.9800 ? C66 H66b 0.9799 ? C66 H66c 0.9801 ? C67 H67a 0.9802 ? C67 H67b 0.9800 ? C67 H67c 0.9800 ? C70 C71 1.385(8) ? C70 C75 1.369(7) ? C70 C76 1.506(8) ? C71 C72 1.37(1) ? C71 H71 0.9801 ? C72 C73 1.38(1) ? C72 H72 0.9801 ? C73 C74 1.39(1) ? C73 H73 0.9800 ? C74 C75 1.384(8) ? C74 H74 0.9800 ? C75 H75 0.9801 ? C76 H76a 0.9798 ? C76 H76b 0.9799 ? C76 H76c 0.9803 ? C80 C81 1.35(1) ? C80 C85 1.46(1) ? C80 C86 1.46(1) ? C81 C82 1.36(1) ? C81 H81 0.9801 ? C82 C83 1.42(1) ? C82 H82 0.9806 ? C83 C84 1.40(1) ? C83 H83 0.9799 ? C84 C85 1.32(1) ? C84 H84 0.9798 ? C85 H85 0.9799 ? C86 H86a 0.9801 ? C86 H86b 0.9803 ? C86 H86c 0.9798 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag P1 Ni P2 151.51(5) ? P1 Ni C1 90.5(1) ? P1 Ni C2 95.9(1) ? P2 Ni C1 89.8(1) ? P2 Ni C2 93.0(1) ? C1 Ni C2 161.0(2) ? C15 S C16 98.5(2) ? Ni P1 C11 105.2(1) ? Ni P1 C30 122.4(2) ? Ni P1 C40 115.9(1) ? C11 P1 C30 103.2(2) ? C11 P1 C40 103.3(2) ? C30 P1 C40 104.6(2) ? Ni P2 C20 105.9(2) ? Ni P2 C50 117.1(1) ? Ni P2 C60 118.9(2) ? C20 P2 C50 101.7(2) ? C20 P2 C60 106.0(2) ? C50 P2 C60 105.4(2) ? C10 O C21 117.3(3) ? C33 N3 C36 119.6(5) ? C33 N3 C37 122.3(5) ? C36 N3 C37 117.6(4) ? C43 N4 C46 120.6(5) ? C43 N4 C47 119.3(5) ? C46 N4 C47 116.0(5) ? C53 N5 C56 121.3(4) ? C53 N5 C57 120.3(4) ? C56 N5 C57 117.5(4) ? C63 N6 C66 121.1(4) ? C63 N6 C67 120.6(4) ? C66 N6 C67 116.4(4) ? Ni C1 N1 173.9(4) ? Ni C2 N2 172.1(4) ? O C10 C11 119.2(4) ? O C10 C15 119.8(4) ? C11 C10 C15 121.0(4) ? P1 C11 C10 123.0(3) ? P1 C11 C12 119.3(3) ? C10 C11 C12 117.7(4) ? C11 C12 C13 122.4(4) ? C11 C12 H12 118.26 ? C13 C12 H12 119.36 ? C12 C13 C14 118.2(4) ? C12 C13 C22 120.8(4) ? C14 C13 C22 121.0(4) ? C13 C14 C15 120.6(4) ? C13 C14 H14 118.60 ? C15 C14 H14 120.79 ? S C15 C10 120.9(4) ? S C15 C14 119.0(4) ? C10 C15 C14 120.1(4) ? S C16 C17 120.2(4) ? S C16 C21 119.3(4) ? C17 C16 C21 120.5(5) ? C16 C17 C18 122.1(5) ? C16 C17 H17 116.48 ? C18 C17 H17 121.41 ? C17 C18 C19 116.7(5) ? C17 C18 C23 121.3(5) ? C19 C18 C23 121.9(5) ? C18 C19 C20 122.5(5) ? C18 C19 H19 120.15 ? C20 C19 H19 117.31 ? P2 C20 C19 120.6(4) ? P2 C20 C21 120.6(4) ? C19 C20 C21 118.6(4) ? O C21 C16 121.8(4) ? O C21 C20 118.7(4) ? C16 C21 C20 119.5(4) ? C13 C22 H22a 138.93 ? C13 C22 H22b 102.14 ? C13 C22 H22c 105.25 ? H22a C22 H22b 98.96 ? H22a C22 H22c 102.17 ? H22b C22 H22c 105.94 ? C18 C23 H23a 119.86 ? C18 C23 H23b 108.65 ? C18 C23 H23c 108.87 ? H23a C23 H23b 105.64 ? H23a C23 H23c 105.98 ? H23b C23 H23c 107.18 ? P1 C30 C31 120.8(3) ? P1 C30 C35 121.7(3) ? C31 C30 C35 117.2(4) ? C30 C31 C32 121.6(4) ? C30 C31 H31 118.53 ? C32 C31 H31 119.82 ? C31 C32 C33 121.6(5) ? C31 C32 H32 119.67 ? C33 C32 H32 118.71 ? N3 C33 C32 120.9(5) ? N3 C33 C34 122.0(5) ? C32 C33 C34 117.1(4) ? C33 C34 C35 120.6(5) ? C33 C34 H34 118.82 ? C35 C34 H34 120.57 ? C30 C35 C34 121.8(4) ? C30 C35 H35 118.71 ? C34 C35 H35 119.46 ? N3 C36 H36a 103.69 ? N3 C36 H36b 109.88 ? N3 C36 H36c 111.63 ? H36a C36 H36b 110.02 ? H36a C36 H36c 113.48 ? H36b C36 H36c 108.09 ? N3 C37 H37a 118.88 ? N3 C37 H37b 106.68 ? N3 C37 H37c 106.23 ? H37a C37 H37b 107.60 ? H37a C37 H37c 107.60 ? H37b C37 H37c 109.65 ? P1 C40 C41 119.1(3) ? P1 C40 C45 123.6(4) ? C41 C40 C45 117.3(4) ? C40 C41 C42 121.1(4) ? C40 C41 H41 120.07 ? C42 C41 H41 118.81 ? C41 C42 C43 121.4(5) ? C41 C42 H42 119.27 ? C43 C42 H42 119.36 ? N4 C43 C42 121.9(5) ? N4 C43 C44 121.8(5) ? C42 C43 C44 116.2(4) ? C43 C44 C45 122.3(5) ? C43 C44 H44 120.07 ? C45 C44 H44 117.53 ? C40 C45 C44 121.6(5) ? C40 C45 H45 119.21 ? C44 C45 H45 119.17 ? N4 C46 H46a 120.04 ? N4 C46 H46b 108.83 ? N4 C46 H46c 109.61 ? H46a C46 H46b 104.86 ? H46a C46 H46c 106.06 ? H46b C46 H46c 106.63 ? N4 C47 H47a 110.09 ? N4 C47 H47b 110.92 ? N4 C47 H47c 112.73 ? H47a C47 H47b 106.33 ? H47a C47 H47c 108.45 ? H47b C47 H47c 108.08 ? P2 C50 C51 122.6(3) ? P2 C50 C55 120.3(3) ? C51 C50 C55 117.1(4) ? C50 C51 C52 121.5(4) ? C50 C51 H51 119.42 ? C52 C51 H51 119.08 ? C51 C52 C53 121.7(4) ? C51 C52 H52 119.23 ? C53 C52 H52 119.05 ? N5 C53 C52 121.5(4) ? N5 C53 C54 121.9(5) ? C52 C53 C54 116.6(4) ? C53 C54 C55 121.3(4) ? C53 C54 H54 119.61 ? C55 C54 H54 119.12 ? C50 C55 C54 121.8(4) ? C50 C55 H55 119.44 ? C54 C55 H55 118.74 ? N5 C56 H56a 106.76 ? N5 C56 H56b 112.67 ? N5 C56 H56c 113.62 ? H56a C56 H56b 106.75 ? H56a C56 H56c 107.52 ? H56b C56 H56c 109.15 ? N5 C57 H57a 118.02 ? N5 C57 H57b 110.89 ? N5 C57 H57c 110.36 ? H57a C57 H57b 105.15 ? H57a C57 H57c 103.37 ? H57b C57 H57c 108.44 ? P2 C60 C61 122.8(3) ? P2 C60 C65 120.8(3) ? C61 C60 C65 116.4(4) ? C60 C61 C62 122.1(4) ? C60 C61 H61 118.70 ? C62 C61 H61 119.20 ? C61 C62 C63 121.2(4) ? C61 C62 H62 119.80 ? C63 C62 H62 119.00 ? N6 C63 C62 121.2(4) ? N6 C63 C64 122.7(4) ? C62 C63 C64 116.1(4) ? C63 C64 C65 122.2(4) ? C63 C64 H64 119.31 ? C65 C64 H64 118.49 ? C60 C65 C64 122.0(4) ? C60 C65 H65 117.92 ? C64 C65 H65 120.12 ? N6 C66 H66a 102.05 ? N6 C66 H66b 113.02 ? N6 C66 H66c 112.47 ? H66a C66 H66b 110.49 ? H66a C66 H66c 109.80 ? H66b C66 H66c 108.85 ? N6 C67 H67a 111.27 ? N6 C67 H67b 110.08 ? N6 C67 H67c 111.12 ? H67a C67 H67b 106.98 ? H67a C67 H67c 108.61 ? H67b C67 H67c 108.66 ? C71 C70 C75 118.4(6) ? C71 C70 C76 121.2(6) ? C75 C70 C76 120.4(5) ? C70 C71 C72 121.2(7) ? C70 C71 H71 120.76 ? C72 C71 H71 117.96 ? C71 C72 C73 120.1(7) ? C71 C72 H72 121.82 ? C73 C72 H72 117.94 ? C72 C73 C74 119.6(7) ? C72 C73 H73 120.76 ? C74 C73 H73 119.52 ? C73 C74 C75 119.3(7) ? C73 C74 H74 120.88 ? C75 C74 H74 119.73 ? C70 C75 C74 121.3(6) ? C70 C75 H75 119.59 ? C74 C75 H75 119.07 ? C70 C76 H76a 132.86 ? C70 C76 H76b 103.18 ? C70 C76 H76c 103.78 ? H76a C76 H76b 103.56 ? H76a C76 H76c 102.93 ? H76b C76 H76c 109.38 ? C81 C80 C85 119.7(8) ? C81 C80 C86 1241(1) ? C85 C80 C86 115.5(9) ? C80 C81 C82 125.(1) ? C80 C81 H81 120.64 ? C82 C81 H81 114.09 ? C81 C82 C83 113(1) ? C81 C82 H82 127.98 ? C83 C82 H82 118.69 ? C82 C83 C84 124(1) ? C82 C83 H83 121.53 ? C84 C83 H83 114.61 ? C83 C84 C85 121.(1) ? C83 C84 H84 116.45 ? C85 C84 H84 122.54 ? C80 C85 C84 117.0(9) ? C80 C85 H85 122.47 ? C84 C85 H85 120.50 ? C80 C86 H86a 114.33 ? C80 C86 H86b 112.32 ? C80 C86 H86c 114.12 ? H86a C86 H86b 104.45 ? H86a C86 H86c 106.32 ? H86b C86 H86c 104.34 ?