Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_date 10-05-05 _publ_contact_author_name 'Dominique Matt' _publ_contact_author_address ; Institut de Chimie, 1 rue Blaise Pascal, 67008 STRASBOURG, FRANCE ; _publ_contact_author_phone 0390241719 _publ_contact_author_fax 0390241719 _publ_contact_author_email dmatt@chimie.u-strasbg.fr _publ_contact_letter ; ; _publ_requested_category FM _publ_section_title ; Catalytic applications of keto-stabilised phosphorus ylides based on a macrocyclic scaffold: calixarenes with one or two pendant Ni(P,O)-subunits as ethylene oligomerisation and polymerisation catalysts ; loop_ _publ_author_name _publ_author_address P.Kuhn ; Laboratoire de Chimie Inorganique Moleculaire, UMR CNRS 7513 Universite Louis Pasteur, 1 rue Blaise Pascal 67000 STRASBOURG France ; D.Semeril ; Laboratoire de Chimie Inorganique Moleculaire, UMR CNRS 7513 Universite Louis Pasteur, 1 rue Blaise Pascal 67000 STRASBOURG France ; C.Jeunesse ; Laboratoire de Chimie Inorganique Moleculaire, UMR CNRS 7513 Universite Louis Pasteur, 1, rue Blaise Pascal 67000 STRASBOURG France ; D.Matt ; Laboratoire de Chimie Inorganique Moleculaire, UMR CNRS 7513 Universite Louis Pasteur, 1, rue Blaise Pascal 67000 STRASBOURG France ; P.J.Lutz ; Institut Charles Sadron, UPR 22 CNRS, 6 rue Boussingault, 67083 Strasbourg Cedex France ; R.Louis ; Institut de Chimie, LC 3 CNRS-ULP, Universite Louis Pasteur, 1, rue Blaise Pascal 67000 STRASBOURG France ; ; M.Neuburger ; ; Laboratory of Chemical Crystallography, Basel Universitat Spitalstrasse 51 4056 BASEL Switzerland ; _publ_section_references ; Blessing, R.H. (1987). Crystallogr. Rev. 1, 3-58. Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. A.L. Spek, PLATON 98, Utrecht University, The Netherland, 1998. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Sheldrick, G.M. (1997). SHELXL97. Program for the refinement of crystal structures. University of Gottingen. Germany. ; data_welt8 _database_code_depnum_ccdc_archive 'CCDC 294726' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C76.50 H75 Cl O8 P2' _chemical_formula_sum 'C76.50 H75 Cl O8 P2' _chemical_formula_weight 1219.75 _chemical_absolute_configuration . 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.127(2) _cell_length_b 16.167(2) _cell_length_c 20.818(4) _cell_angle_alpha 86.82(5) _cell_angle_beta 83.22(5) _cell_angle_gamma 78.40(5) _cell_volume 3313.6(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 37021 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1290 _exptl_absorpt_coefficient_mu 0.162 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19356 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1884 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 30.06 _reflns_number_total 19355 _reflns_number_gt 10532 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+7.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19355 _refine_ls_number_parameters 767 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2185 _refine_ls_R_factor_gt 0.0927 _refine_ls_wR_factor_ref 0.2343 _refine_ls_wR_factor_gt 0.1949 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.54300(12) 0.02653(7) 0.29799(5) 0.0411(3) Uani 1 1 d . . . P2 P 1.03166(12) -0.77845(7) -0.07155(5) 0.0380(3) Uani 1 1 d . . . O1 O 0.3718(3) -0.09686(17) 0.34246(14) 0.0441(7) Uani 1 1 d . . . O2 O 0.6487(3) -0.47932(16) 0.38803(13) 0.0369(6) Uani 1 1 d . . . H2 H 0.5848 -0.5031 0.3822 0.055 Uiso 1 1 calc . . . O3 O 0.9224(2) -0.56197(16) 0.38263(11) 0.0321(6) Uani 1 1 d . . . O4 O 0.7928(3) -0.63947(18) 0.30101(12) 0.0418(7) Uani 1 1 d . . . HO4 H 0.8510 -0.6284 0.3231 0.063 Uiso 1 1 calc . . . O5 O 0.5107(3) -0.59096(17) 0.33544(13) 0.0386(7) Uani 1 1 d . . . O6 O 1.1533(3) -0.73486(18) 0.03475(12) 0.0426(7) Uani 1 1 d . . . C1 C 0.5940(4) -0.0805(2) 0.3122(2) 0.0396(10) Uani 1 1 d . . . H1 H 0.6870 -0.1065 0.3043 0.048 Uiso 1 1 calc . . . C2 C 0.4982(4) -0.1285(2) 0.33529(18) 0.0343(9) Uani 1 1 d . . . C3 C 0.5413(4) -0.2212(2) 0.35064(17) 0.0301(8) Uani 1 1 d . . . C4 C 0.6686(4) -0.2575(2) 0.36882(18) 0.0315(8) Uani 1 1 d . . . H4 H 0.7318 -0.2223 0.3725 0.038 Uiso 1 1 calc . . . C5 C 0.7056(4) -0.3437(2) 0.38173(17) 0.0303(8) Uani 1 1 d . . . C6 C 0.6125(4) -0.3946(2) 0.37479(17) 0.0302(8) Uani 1 1 d . . . C7 C 0.4840(4) -0.3610(2) 0.35551(17) 0.0283(8) Uani 1 1 d . . . C8 C 0.4507(4) -0.2741(2) 0.34551(17) 0.0303(8) Uani 1 1 d . . . H8 H 0.3623 -0.2498 0.3347 0.036 Uiso 1 1 calc . . . C9 C 0.8449(4) -0.3827(2) 0.40176(19) 0.0370(9) Uani 1 1 d . . . H9A H 0.8355 -0.4269 0.4359 0.044 Uiso 1 1 calc . . . H9B H 0.8829 -0.3386 0.4202 0.044 Uiso 1 1 calc . . . C10 C 0.9432(4) -0.4218(2) 0.34513(18) 0.0310(8) Uani 1 1 d . . . C11 C 0.9985(4) -0.3697(3) 0.2985(2) 0.0416(10) Uani 1 1 d . . . H11 H 0.9793 -0.3104 0.3039 0.050 Uiso 1 1 calc . . . C12 C 1.0800(4) -0.4025(3) 0.2451(2) 0.0463(11) Uani 1 1 d . . . H12 H 1.1175 -0.3661 0.2139 0.056 Uiso 1 1 calc . . . C13 C 1.1075(4) -0.4883(3) 0.23660(19) 0.0433(11) Uani 1 1 d . . . H13 H 1.1636 -0.5103 0.1991 0.052 Uiso 1 1 calc . . . C14 C 1.0553(4) -0.5439(3) 0.28155(18) 0.0342(9) Uani 1 1 d . . . C15 C 0.9768(4) -0.5083(2) 0.33647(16) 0.0286(8) Uani 1 1 d . . . C16 C 1.0118(4) -0.6015(3) 0.42947(18) 0.0383(10) Uani 1 1 d . . . H16A H 1.0311 -0.5583 0.4570 0.046 Uiso 1 1 calc . . . H16B H 1.0988 -0.6312 0.4071 0.046 Uiso 1 1 calc . . . C17 C 0.9416(5) -0.6638(3) 0.4706(2) 0.0455(11) Uani 1 1 d . . . H17A H 0.9088 -0.7003 0.4419 0.055 Uiso 1 1 calc . . . H17B H 1.0077 -0.7003 0.4965 0.055 Uiso 1 1 calc . . . C18 C 0.8253(5) -0.6202(3) 0.5147(2) 0.0577(13) Uani 1 1 d . . . H18A H 0.8579 -0.5853 0.5440 0.087 Uiso 1 1 calc . . . H18B H 0.7820 -0.6624 0.5400 0.087 Uiso 1 1 calc . . . H18C H 0.7593 -0.5843 0.4892 0.087 Uiso 1 1 calc . . . C19 C 1.0782(4) -0.6370(3) 0.26904(19) 0.0436(11) Uani 1 1 d . . . H19A H 1.0607 -0.6681 0.3105 0.052 Uiso 1 1 calc . . . H19B H 1.1744 -0.6569 0.2523 0.052 Uiso 1 1 calc . . . C20 C 0.9883(4) -0.6582(2) 0.22096(18) 0.0330(9) Uani 1 1 d . . . C21 C 1.0408(4) -0.6801(2) 0.15871(18) 0.0346(9) Uani 1 1 d . . . H21 H 1.1342 -0.6808 0.1458 0.042 Uiso 1 1 calc . . . C22 C 0.9615(4) -0.7015(2) 0.11385(17) 0.0318(8) Uani 1 1 d . . . C23 C 0.8254(4) -0.6994(3) 0.1338(2) 0.0398(10) Uani 1 1 d . . . H23 H 0.7696 -0.7134 0.1041 0.048 Uiso 1 1 calc . . . C24 C 0.7681(4) -0.6772(2) 0.1962(2) 0.0388(10) Uani 1 1 d . . . C25 C 0.8513(4) -0.6572(2) 0.23945(18) 0.0372(9) Uani 1 1 d . . . C26 C 0.6181(5) -0.6753(3) 0.2168(2) 0.0508(12) Uani 1 1 d . . . H26A H 0.5822 -0.7073 0.1859 0.061 Uiso 1 1 calc . . . H26B H 0.6073 -0.7032 0.2601 0.061 Uiso 1 1 calc . . . C27 C 0.5371(4) -0.5855(3) 0.2190(2) 0.0399(10) Uani 1 1 d . . . C28 C 0.5136(5) -0.5384(3) 0.1622(2) 0.0496(12) Uani 1 1 d . . . H28 H 0.5421 -0.5646 0.1218 0.060 Uiso 1 1 calc . . . C29 C 0.4499(5) -0.4546(3) 0.1631(2) 0.0489(11) Uani 1 1 d . . . H29 H 0.4335 -0.4236 0.1238 0.059 Uiso 1 1 calc . . . C30 C 0.4101(4) -0.4158(3) 0.2219(2) 0.0402(10) Uani 1 1 d . . . H30 H 0.3692 -0.3576 0.2224 0.048 Uiso 1 1 calc . . . C31 C 0.4291(4) -0.4606(2) 0.27994(18) 0.0321(8) Uani 1 1 d . . . C32 C 0.4894(4) -0.5460(2) 0.27731(19) 0.0335(9) Uani 1 1 d . . . C33 C 0.3975(4) -0.6275(3) 0.3651(2) 0.0530(12) Uani 1 1 d . . . H33A H 0.3992 -0.6824 0.3459 0.064 Uiso 1 1 calc . . . H33B H 0.3105 -0.5893 0.3581 0.064 Uiso 1 1 calc . . . C34 C 0.4126(5) -0.6401(3) 0.4398(3) 0.0642(15) Uani 1 1 d . . . H34A H 0.4112 -0.5847 0.4581 0.077 Uiso 1 1 calc . . . H34B H 0.3344 -0.6624 0.4618 0.077 Uiso 1 1 calc . . . C35 C 0.5385(7) -0.6982(4) 0.4524(3) 0.0818(18) Uani 1 1 d . . . H35A H 0.5465 -0.7503 0.4290 0.123 Uiso 1 1 calc . . . H35B H 0.5371 -0.7117 0.4989 0.123 Uiso 1 1 calc . . . H35C H 0.6161 -0.6716 0.4376 0.123 Uiso 1 1 calc . . . C36 C 0.3879(4) -0.4164(2) 0.3433(2) 0.0369(9) Uani 1 1 d . . . H36A H 0.2957 -0.3815 0.3427 0.044 Uiso 1 1 calc . . . H36B H 0.3849 -0.4591 0.3791 0.044 Uiso 1 1 calc . . . C37 C 1.0262(4) -0.7281(2) 0.04743(18) 0.0338(9) Uani 1 1 d . . . C38 C 0.9472(4) -0.7454(3) 0.00153(19) 0.0398(10) Uani 1 1 d . . . H38 H 0.8516 -0.7393 0.0102 0.048 Uiso 1 1 calc . . . C39 C 0.4516(5) 0.0583(3) 0.2284(2) 0.0462(11) Uani 1 1 d . . . C40 C 0.3790(6) 0.0058(3) 0.2054(2) 0.0675(15) Uani 1 1 d . . . H40 H 0.3803 -0.0489 0.2247 0.081 Uiso 1 1 calc . . . C41 C 0.3030(6) 0.0322(4) 0.1535(3) 0.0783(17) Uani 1 1 d . . . H41 H 0.2544 -0.0050 0.1371 0.094 Uiso 1 1 calc . . . C42 C 0.2986(6) 0.1111(4) 0.1266(3) 0.0744(17) Uani 1 1 d . . . H42 H 0.2451 0.1294 0.0920 0.089 Uiso 1 1 calc . . . C43 C 0.3698(6) 0.1636(4) 0.1488(3) 0.0785(18) Uani 1 1 d . . . H43 H 0.3680 0.2182 0.1290 0.094 Uiso 1 1 calc . . . C44 C 0.4458(6) 0.1381(3) 0.2004(3) 0.0663(15) Uani 1 1 d . . . H44 H 0.4940 0.1759 0.2164 0.080 Uiso 1 1 calc . . . C45 C 0.4360(5) 0.0783(2) 0.3658(2) 0.0439(10) Uani 1 1 d . . . C46 C 0.4817(5) 0.0713(3) 0.4261(2) 0.0577(13) Uani 1 1 d . . . H46 H 0.5700 0.0400 0.4314 0.069 Uiso 1 1 calc . . . C47 C 0.4001(6) 0.1095(3) 0.4794(2) 0.0670(15) Uani 1 1 d . . . H47 H 0.4336 0.1058 0.5204 0.080 Uiso 1 1 calc . . . C48 C 0.2725(6) 0.1520(3) 0.4722(3) 0.0682(15) Uani 1 1 d . . . H48 H 0.2159 0.1772 0.5085 0.082 Uiso 1 1 calc . . . C49 C 0.2247(6) 0.1586(4) 0.4126(3) 0.0748(17) Uani 1 1 d . . . H49 H 0.1349 0.1878 0.4080 0.090 Uiso 1 1 calc . . . C50 C 0.3069(5) 0.1229(3) 0.3593(3) 0.0613(14) Uani 1 1 d . . . H50 H 0.2742 0.1291 0.3180 0.074 Uiso 1 1 calc . . . C51 C 0.6964(5) 0.0682(3) 0.2822(2) 0.0452(11) Uani 1 1 d . . . C52 C 0.7317(5) 0.1235(3) 0.3219(2) 0.0536(12) Uani 1 1 d . . . H52 H 0.6711 0.1445 0.3583 0.064 Uiso 1 1 calc . . . C53 C 0.8566(6) 0.1489(3) 0.3088(3) 0.0644(14) Uani 1 1 d . . . H53 H 0.8811 0.1861 0.3370 0.077 Uiso 1 1 calc . . . C54 C 0.9440(5) 0.1205(3) 0.2556(3) 0.0639(14) Uani 1 1 d . . . H54 H 1.0290 0.1375 0.2469 0.077 Uiso 1 1 calc . . . C55 C 0.9071(6) 0.0673(4) 0.2151(3) 0.0773(17) Uani 1 1 d . . . H55 H 0.9663 0.0481 0.1777 0.093 Uiso 1 1 calc . . . C56 C 0.7837(6) 0.0412(4) 0.2283(3) 0.0711(16) Uani 1 1 d . . . H56 H 0.7592 0.0043 0.1997 0.085 Uiso 1 1 calc . . . C57 C 1.1201(4) -0.7027(3) -0.11522(18) 0.0369(9) Uani 1 1 d . . . C58 C 1.0798(4) -0.6183(3) -0.09930(19) 0.0428(10) Uani 1 1 d . . . H58 H 1.0129 -0.6026 -0.0638 0.051 Uiso 1 1 calc . . . C59 C 1.1379(5) -0.5567(3) -0.1356(2) 0.0494(11) Uani 1 1 d . . . H59 H 1.1106 -0.4991 -0.1245 0.059 Uiso 1 1 calc . . . C60 C 1.2340(5) -0.5791(3) -0.1870(2) 0.0487(11) Uani 1 1 d . . . H60 H 1.2721 -0.5368 -0.2118 0.058 Uiso 1 1 calc . . . C61 C 1.2755(4) -0.6627(3) -0.2027(2) 0.0509(12) Uani 1 1 d . . . H61 H 1.3432 -0.6781 -0.2379 0.061 Uiso 1 1 calc . . . C62 C 1.2184(5) -0.7240(3) -0.1673(2) 0.0458(11) Uani 1 1 d . . . H62 H 1.2468 -0.7815 -0.1786 0.055 Uiso 1 1 calc . . . C63 C 1.1507(5) -0.8781(3) -0.06685(18) 0.0489(12) Uani 1 1 d . . . C64 C 1.2867(6) -0.8813(3) -0.0628(2) 0.0653(15) Uani 1 1 d . . . H64 H 1.3206 -0.8304 -0.0646 0.078 Uiso 1 1 calc . . . C65 C 1.3745(7) -0.9588(5) -0.0561(3) 0.087(2) Uani 1 1 d . . . H65 H 1.4683 -0.9610 -0.0537 0.104 Uiso 1 1 calc . . . C66 C 1.3240(9) -1.0325(4) -0.0528(3) 0.097(3) Uani 1 1 d . . . H66 H 1.3837 -1.0855 -0.0487 0.116 Uiso 1 1 calc . . . C67 C 1.1887(9) -1.0298(3) -0.0555(3) 0.089(2) Uani 1 1 d . . . H67 H 1.1545 -1.0806 -0.0525 0.107 Uiso 1 1 calc . . . C68 C 1.1013(6) -0.9519(3) -0.0627(2) 0.0653(15) Uani 1 1 d . . . H68 H 1.0075 -0.9498 -0.0648 0.078 Uiso 1 1 calc . . . C69 C 0.9083(6) -0.7968(3) -0.1229(2) 0.0517(12) Uani 1 1 d . . . C70 C 0.9495(8) -0.8224(4) -0.1852(3) 0.088(2) Uani 1 1 d . . . H70 H 1.0434 -0.8330 -0.2004 0.106 Uiso 1 1 calc . . . C71 C 0.8554(12) -0.8331(5) -0.2264(3) 0.121(4) Uani 1 1 d . . . H71 H 0.8842 -0.8501 -0.2696 0.145 Uiso 1 1 calc . . . C72 C 0.7225(13) -0.8187(5) -0.2037(5) 0.135(5) Uani 1 1 d . . . H72 H 0.6581 -0.8265 -0.2313 0.162 Uiso 1 1 calc . . . C73 C 0.6798(8) -0.7939(5) -0.1440(5) 0.124(3) Uani 1 1 d . . . H73 H 0.5856 -0.7838 -0.1294 0.149 Uiso 1 1 calc . . . C74 C 0.7732(7) -0.7825(4) -0.1021(3) 0.0841(19) Uani 1 1 d . . . H74 H 0.7422 -0.7649 -0.0593 0.101 Uiso 1 1 calc . . . Cl1 Cl 0.4997(3) -0.6761(2) 0.01492(16) 0.0855(9) Uiso 0.50 1 d P . . Cl2 Cl 0.2873(4) -0.5221(3) 0.0216(2) 0.1174(13) Uiso 0.50 1 d P . . C75 C 0.3413(11) -0.6209(7) -0.0035(5) 0.068(3) Uiso 0.50 1 d P . . H75A H 0.3421 -0.6191 -0.0511 0.082 Uiso 0.50 1 calc P . . H75B H 0.2730 -0.6543 0.0146 0.082 Uiso 0.50 1 calc P . . O7 O 0.2033(4) -0.1534(3) 0.4360(2) 0.0886(12) Uiso 1 1 d . . . H7 H 0.2270 -0.1231 0.4044 0.133 Uiso 1 1 calc . . . C76 C 0.1843(7) -0.1074(4) 0.4935(3) 0.093(2) Uiso 1 1 d . . . H76A H 0.2700 -0.0920 0.5009 0.139 Uiso 1 1 calc . . . H76B H 0.1544 -0.1423 0.5302 0.139 Uiso 1 1 calc . . . H76C H 0.1153 -0.0560 0.4892 0.139 Uiso 1 1 calc . . . O8 O -0.0288(4) -0.1648(3) 0.3934(2) 0.0900(13) Uiso 1 1 d . . . H8A H 0.0531 -0.1744 0.4002 0.135 Uiso 1 1 calc . . . C77 C -0.0754(8) -0.0775(5) 0.3860(4) 0.118(3) Uiso 1 1 d . . . H77A H -0.1590 -0.0604 0.4149 0.176 Uiso 1 1 calc . . . H77B H -0.0935 -0.0635 0.3411 0.176 Uiso 1 1 calc . . . H77C H -0.0062 -0.0477 0.3968 0.176 Uiso 1 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0509(7) 0.0281(6) 0.0420(6) -0.0023(5) -0.0025(5) -0.0034(5) P2 0.0517(7) 0.0364(6) 0.0252(5) -0.0049(4) -0.0086(5) -0.0038(5) O1 0.0401(17) 0.0329(15) 0.0569(19) -0.0058(13) -0.0118(14) 0.0035(13) O2 0.0328(15) 0.0296(15) 0.0502(17) 0.0019(12) -0.0116(13) -0.0078(12) O3 0.0322(14) 0.0395(15) 0.0254(13) 0.0036(11) -0.0077(11) -0.0074(12) O4 0.0391(16) 0.0564(18) 0.0318(15) -0.0159(13) 0.0023(12) -0.0134(14) O5 0.0292(15) 0.0427(16) 0.0455(17) 0.0033(13) 0.0010(12) -0.0148(12) O6 0.0372(17) 0.0573(19) 0.0298(14) -0.0080(13) -0.0027(12) 0.0001(14) C1 0.045(3) 0.027(2) 0.044(2) -0.0048(18) -0.0059(19) 0.0015(18) C2 0.041(2) 0.032(2) 0.029(2) -0.0081(16) -0.0075(17) -0.0010(18) C3 0.035(2) 0.028(2) 0.0262(18) -0.0037(15) -0.0051(16) -0.0019(16) C4 0.033(2) 0.032(2) 0.032(2) -0.0084(16) -0.0069(16) -0.0071(17) C5 0.031(2) 0.034(2) 0.0265(18) -0.0064(15) -0.0083(15) -0.0026(16) C6 0.035(2) 0.028(2) 0.0245(18) -0.0045(15) 0.0001(16) -0.0020(16) C7 0.028(2) 0.029(2) 0.0264(18) -0.0070(15) -0.0006(15) -0.0020(16) C8 0.0249(19) 0.039(2) 0.0251(18) -0.0045(16) -0.0020(15) -0.0005(16) C9 0.039(2) 0.037(2) 0.036(2) -0.0101(17) -0.0177(18) 0.0005(18) C10 0.027(2) 0.035(2) 0.034(2) -0.0016(16) -0.0143(16) -0.0064(16) C11 0.032(2) 0.041(2) 0.056(3) 0.011(2) -0.023(2) -0.0116(19) C12 0.033(2) 0.063(3) 0.048(3) 0.021(2) -0.013(2) -0.022(2) C13 0.025(2) 0.075(3) 0.027(2) 0.004(2) -0.0025(16) -0.006(2) C14 0.026(2) 0.045(2) 0.030(2) -0.0036(17) -0.0076(16) 0.0003(17) C15 0.0259(19) 0.038(2) 0.0232(18) 0.0014(15) -0.0068(15) -0.0064(16) C16 0.039(2) 0.048(2) 0.030(2) 0.0046(18) -0.0122(17) -0.0080(19) C17 0.053(3) 0.048(3) 0.034(2) 0.0003(19) -0.006(2) -0.004(2) C18 0.064(3) 0.062(3) 0.046(3) -0.002(2) -0.004(2) -0.010(3) C19 0.044(3) 0.050(3) 0.030(2) -0.0090(18) -0.0074(18) 0.010(2) C20 0.033(2) 0.032(2) 0.0296(19) -0.0044(16) -0.0030(16) 0.0041(17) C21 0.032(2) 0.036(2) 0.033(2) -0.0059(17) 0.0004(17) 0.0009(17) C22 0.035(2) 0.030(2) 0.0277(19) -0.0037(15) -0.0007(16) -0.0021(17) C23 0.042(2) 0.037(2) 0.043(2) -0.0118(18) -0.0048(19) -0.0088(19) C24 0.043(2) 0.032(2) 0.041(2) -0.0118(18) 0.0082(19) -0.0125(18) C25 0.052(3) 0.029(2) 0.029(2) -0.0059(16) -0.0007(18) -0.0044(18) C26 0.050(3) 0.045(3) 0.060(3) -0.021(2) 0.012(2) -0.020(2) C27 0.030(2) 0.047(3) 0.046(2) -0.016(2) 0.0047(18) -0.0182(19) C28 0.047(3) 0.069(3) 0.040(2) -0.019(2) -0.001(2) -0.025(2) C29 0.042(3) 0.071(3) 0.040(2) 0.006(2) -0.013(2) -0.022(2) C30 0.026(2) 0.046(2) 0.051(3) -0.002(2) -0.0070(18) -0.0099(18) C31 0.0211(19) 0.042(2) 0.036(2) -0.0070(17) 0.0004(16) -0.0122(17) C32 0.0210(19) 0.043(2) 0.040(2) -0.0076(18) -0.0001(16) -0.0146(17) C33 0.036(2) 0.061(3) 0.065(3) 0.004(2) 0.000(2) -0.022(2) C34 0.050(3) 0.068(3) 0.068(3) 0.027(3) 0.010(3) -0.014(3) C35 0.093(5) 0.090(4) 0.063(4) 0.008(3) -0.004(3) -0.026(4) C36 0.028(2) 0.036(2) 0.045(2) -0.0077(18) 0.0043(18) -0.0061(17) C37 0.039(2) 0.032(2) 0.0281(19) -0.0050(16) -0.0024(17) -0.0015(17) C38 0.042(2) 0.044(2) 0.033(2) -0.0088(18) -0.0009(18) -0.0061(19) C39 0.054(3) 0.036(2) 0.045(3) -0.0001(19) -0.005(2) 0.000(2) C40 0.102(4) 0.048(3) 0.055(3) 0.007(2) -0.034(3) -0.009(3) C41 0.102(5) 0.076(4) 0.058(3) 0.007(3) -0.035(3) -0.007(3) C42 0.068(4) 0.087(4) 0.052(3) 0.013(3) -0.005(3) 0.019(3) C43 0.073(4) 0.064(4) 0.088(4) 0.035(3) -0.017(3) 0.006(3) C44 0.075(4) 0.047(3) 0.077(4) 0.016(3) -0.014(3) -0.014(3) C45 0.053(3) 0.029(2) 0.049(3) -0.0048(19) -0.001(2) -0.006(2) C46 0.072(4) 0.046(3) 0.048(3) 0.003(2) -0.006(3) 0.003(2) C47 0.097(4) 0.053(3) 0.045(3) -0.001(2) -0.001(3) -0.004(3) C48 0.081(4) 0.052(3) 0.064(4) -0.015(3) 0.016(3) -0.004(3) C49 0.064(4) 0.076(4) 0.077(4) -0.027(3) 0.000(3) 0.007(3) C50 0.055(3) 0.060(3) 0.065(3) -0.020(3) -0.005(3) 0.001(3) C51 0.057(3) 0.032(2) 0.045(3) -0.0015(19) -0.002(2) -0.006(2) C52 0.055(3) 0.047(3) 0.058(3) -0.004(2) -0.007(2) -0.007(2) C53 0.068(4) 0.052(3) 0.078(4) -0.002(3) -0.020(3) -0.017(3) C54 0.060(3) 0.050(3) 0.082(4) 0.005(3) 0.001(3) -0.020(3) C55 0.070(4) 0.087(4) 0.076(4) -0.015(3) 0.019(3) -0.030(3) C56 0.075(4) 0.078(4) 0.064(3) -0.018(3) 0.010(3) -0.030(3) C57 0.043(2) 0.042(2) 0.0266(19) 0.0021(17) -0.0134(17) -0.0056(19) C58 0.048(3) 0.045(3) 0.036(2) -0.0034(19) -0.0111(19) -0.006(2) C59 0.053(3) 0.044(3) 0.055(3) 0.002(2) -0.021(2) -0.011(2) C60 0.043(3) 0.062(3) 0.046(3) 0.011(2) -0.015(2) -0.021(2) C61 0.039(3) 0.080(4) 0.036(2) 0.001(2) -0.008(2) -0.016(2) C62 0.049(3) 0.055(3) 0.033(2) -0.004(2) -0.007(2) -0.006(2) C63 0.071(3) 0.045(3) 0.0209(19) 0.0002(18) 0.002(2) 0.008(2) C64 0.075(4) 0.066(3) 0.041(3) 0.003(2) -0.007(3) 0.015(3) C65 0.091(5) 0.091(5) 0.055(3) -0.001(3) -0.007(3) 0.036(4) C66 0.133(7) 0.066(4) 0.060(4) 0.003(3) 0.008(4) 0.045(4) C67 0.133(6) 0.045(3) 0.067(4) 0.006(3) 0.015(4) 0.015(4) C68 0.097(4) 0.045(3) 0.042(3) 0.001(2) 0.010(3) 0.005(3) C69 0.087(4) 0.036(2) 0.039(2) 0.0068(19) -0.029(3) -0.021(2) C70 0.154(6) 0.081(4) 0.046(3) -0.007(3) -0.028(4) -0.050(4) C71 0.240(11) 0.109(6) 0.052(4) 0.013(4) -0.056(6) -0.107(8) C72 0.271(13) 0.093(6) 0.096(6) 0.060(5) -0.130(8) -0.119(8) C73 0.127(7) 0.124(6) 0.152(8) 0.037(6) -0.102(6) -0.057(5) C74 0.092(5) 0.088(4) 0.087(4) -0.001(3) -0.056(4) -0.027(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C1 1.723(4) . ? P1 C51 1.803(5) . ? P1 C39 1.806(5) . ? P1 C45 1.809(4) . ? P2 C38 1.712(4) . ? P2 C57 1.803(4) . ? P2 C63 1.813(5) . ? P2 C69 1.815(5) . ? O1 C2 1.274(5) . ? O2 C6 1.366(4) . ? O2 H2 0.8400 . ? O3 C15 1.399(4) . ? O3 C16 1.445(4) . ? O4 C25 1.367(4) . ? O4 HO4 0.8400 . ? O5 C32 1.393(5) . ? O5 C33 1.452(5) . ? O6 C37 1.267(5) . ? C1 C2 1.388(6) . ? C1 H1 0.9500 . ? C2 C3 1.502(5) . ? C3 C8 1.391(5) . ? C3 C4 1.391(5) . ? C4 C5 1.389(5) . ? C4 H4 0.9500 . ? C5 C6 1.394(5) . ? C5 C9 1.521(5) . ? C6 C7 1.401(5) . ? C7 C8 1.386(5) . ? C7 C36 1.500(5) . ? C8 H8 0.9500 . ? C9 C10 1.527(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C15 1.388(5) . ? C10 C11 1.390(6) . ? C11 C12 1.368(6) . ? C11 H11 0.9500 . ? C12 C13 1.376(6) . ? C12 H12 0.9500 . ? C13 C14 1.394(6) . ? C13 H13 0.9500 . ? C14 C15 1.395(5) . ? C14 C19 1.509(6) . ? C16 C17 1.516(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.487(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.525(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.379(5) . ? C20 C25 1.393(6) . ? C21 C22 1.401(5) . ? C21 H21 0.9500 . ? C22 C23 1.386(5) . ? C22 C37 1.505(5) . ? C23 C24 1.394(5) . ? C23 H23 0.9500 . ? C24 C25 1.395(6) . ? C24 C26 1.524(6) . ? C26 C27 1.517(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.388(6) . ? C27 C32 1.393(5) . ? C28 C29 1.380(6) . ? C28 H28 0.9500 . ? C29 C30 1.384(6) . ? C29 H29 0.9500 . ? C30 C31 1.388(6) . ? C30 H30 0.9500 . ? C31 C32 1.393(5) . ? C31 C36 1.510(5) . ? C33 C34 1.579(7) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.466(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.389(5) . ? C38 H38 0.9500 . ? C39 C40 1.367(7) . ? C39 C44 1.380(6) . ? C40 C41 1.398(7) . ? C40 H40 0.9500 . ? C41 C42 1.359(8) . ? C41 H41 0.9500 . ? C42 C43 1.349(8) . ? C42 H42 0.9500 . ? C43 C44 1.391(8) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C50 1.378(6) . ? C45 C46 1.380(6) . ? C46 C47 1.397(7) . ? C46 H46 0.9500 . ? C47 C48 1.357(8) . ? C47 H47 0.9500 . ? C48 C49 1.374(8) . ? C48 H48 0.9500 . ? C49 C50 1.385(7) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.375(6) . ? C51 C56 1.376(6) . ? C52 C53 1.399(7) . ? C52 H52 0.9500 . ? C53 C54 1.372(7) . ? C53 H53 0.9500 . ? C54 C55 1.369(8) . ? C54 H54 0.9500 . ? C55 C56 1.391(7) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C58 1.390(6) . ? C57 C62 1.390(6) . ? C58 C59 1.399(6) . ? C58 H58 0.9500 . ? C59 C60 1.371(6) . ? C59 H59 0.9500 . ? C60 C61 1.377(7) . ? C60 H60 0.9500 . ? C61 C62 1.382(6) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 C68 1.378(7) . ? C63 C64 1.381(7) . ? C64 C65 1.394(7) . ? C64 H64 0.9500 . ? C65 C66 1.384(10) . ? C65 H65 0.9500 . ? C66 C67 1.369(10) . ? C66 H66 0.9500 . ? C67 C68 1.398(7) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C74 1.362(8) . ? C69 C70 1.374(7) . ? C70 C71 1.396(10) . ? C70 H70 0.9500 . ? C71 C72 1.350(13) . ? C71 H71 0.9500 . ? C72 C73 1.324(13) . ? C72 H72 0.9500 . ? C73 C74 1.404(8) . ? C73 H73 0.9499 . ? C74 H74 0.9500 . ? Cl1 C75 1.746(11) . ? Cl2 C75 1.672(11) . ? C75 H75A 0.9899 . ? C75 H75B 0.9901 . ? O7 C76 1.418(7) . ? O7 H7 0.8400 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? O8 C77 1.401(8) . ? O8 H8A 0.8400 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P1 C51 106.0(2) . . ? C1 P1 C39 116.6(2) . . ? C51 P1 C39 105.5(2) . . ? C1 P1 C45 112.6(2) . . ? C51 P1 C45 110.3(2) . . ? C39 P1 C45 105.6(2) . . ? C38 P2 C57 114.5(2) . . ? C38 P2 C63 114.0(2) . . ? C57 P2 C63 107.9(2) . . ? C38 P2 C69 108.3(2) . . ? C57 P2 C69 106.08(19) . . ? C63 P2 C69 105.4(2) . . ? C6 O2 H2 109.5 . . ? C15 O3 C16 115.3(3) . . ? C25 O4 HO4 109.5 . . ? C32 O5 C33 115.1(3) . . ? C2 C1 P1 119.5(3) . . ? C2 C1 H1 120.2 . . ? P1 C1 H1 120.2 . . ? O1 C2 C1 121.9(4) . . ? O1 C2 C3 117.8(4) . . ? C1 C2 C3 120.3(4) . . ? C8 C3 C4 118.0(3) . . ? C8 C3 C2 118.7(3) . . ? C4 C3 C2 123.3(3) . . ? C5 C4 C3 121.7(3) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C4 C5 C6 118.4(3) . . ? C4 C5 C9 121.3(3) . . ? C6 C5 C9 120.3(3) . . ? O2 C6 C5 118.2(3) . . ? O2 C6 C7 120.0(3) . . ? C5 C6 C7 121.8(3) . . ? C8 C7 C6 117.4(3) . . ? C8 C7 C36 120.8(3) . . ? C6 C7 C36 121.8(3) . . ? C7 C8 C3 122.7(3) . . ? C7 C8 H8 118.7 . . ? C3 C8 H8 118.7 . . ? C5 C9 C10 112.4(3) . . ? C5 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? C5 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? C15 C10 C11 117.6(4) . . ? C15 C10 C9 122.6(3) . . ? C11 C10 C9 119.8(4) . . ? C12 C11 C10 121.1(4) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C13 119.9(4) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C14 121.7(4) . . ? C12 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C13 C14 C15 116.5(4) . . ? C13 C14 C19 120.9(4) . . ? C15 C14 C19 122.5(4) . . ? C10 C15 C14 122.9(4) . . ? C10 C15 O3 118.7(3) . . ? C14 C15 O3 118.2(3) . . ? O3 C16 C17 107.7(3) . . ? O3 C16 H16A 110.2 . . ? C17 C16 H16A 110.2 . . ? O3 C16 H16B 110.2 . . ? C17 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? C18 C17 C16 111.9(4) . . ? C18 C17 H17A 109.2 . . ? C16 C17 H17A 109.2 . . ? C18 C17 H17B 109.2 . . ? C16 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 C20 113.4(3) . . ? C14 C19 H19A 108.9 . . ? C20 C19 H19A 108.9 . . ? C14 C19 H19B 108.9 . . ? C20 C19 H19B 108.9 . . ? H19A C19 H19B 107.7 . . ? C21 C20 C25 118.4(4) . . ? C21 C20 C19 121.0(4) . . ? C25 C20 C19 120.6(3) . . ? C20 C21 C22 122.3(4) . . ? C20 C21 H21 118.8 . . ? C22 C21 H21 118.8 . . ? C23 C22 C21 117.7(3) . . ? C23 C22 C37 122.6(4) . . ? C21 C22 C37 119.7(3) . . ? C22 C23 C24 121.8(4) . . ? C22 C23 H23 119.1 . . ? C24 C23 H23 119.1 . . ? C23 C24 C25 118.6(4) . . ? C23 C24 C26 120.7(4) . . ? C25 C24 C26 120.7(4) . . ? O4 C25 C20 121.9(4) . . ? O4 C25 C24 116.9(4) . . ? C20 C25 C24 121.2(4) . . ? C27 C26 C24 111.4(3) . . ? C27 C26 H26A 109.3 . . ? C24 C26 H26A 109.3 . . ? C27 C26 H26B 109.3 . . ? C24 C26 H26B 109.3 . . ? H26A C26 H26B 108.0 . . ? C28 C27 C32 117.6(4) . . ? C28 C27 C26 120.5(4) . . ? C32 C27 C26 121.8(4) . . ? C29 C28 C27 121.5(4) . . ? C29 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C28 C29 C30 119.5(4) . . ? C28 C29 H29 120.3 . . ? C30 C29 H29 120.3 . . ? C29 C30 C31 121.1(4) . . ? C29 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C30 C31 C32 117.9(4) . . ? C30 C31 C36 120.1(4) . . ? C32 C31 C36 122.1(4) . . ? C27 C32 O5 119.5(4) . . ? C27 C32 C31 122.2(4) . . ? O5 C32 C31 118.1(3) . . ? O5 C33 C34 107.1(4) . . ? O5 C33 H33A 110.3 . . ? C34 C33 H33A 110.3 . . ? O5 C33 H33B 110.3 . . ? C34 C33 H33B 110.3 . . ? H33A C33 H33B 108.5 . . ? C35 C34 C33 112.0(4) . . ? C35 C34 H34A 109.2 . . ? C33 C34 H34A 109.2 . . ? C35 C34 H34B 109.2 . . ? C33 C34 H34B 109.2 . . ? H34A C34 H34B 107.9 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C7 C36 C31 112.1(3) . . ? C7 C36 H36A 109.2 . . ? C31 C36 H36A 109.2 . . ? C7 C36 H36B 109.2 . . ? C31 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? O6 C37 C38 121.2(4) . . ? O6 C37 C22 118.6(3) . . ? C38 C37 C22 120.2(4) . . ? C37 C38 P2 116.4(3) . . ? C37 C38 H38 121.8 . . ? P2 C38 H38 121.8 . . ? C40 C39 C44 118.7(5) . . ? C40 C39 P1 120.5(3) . . ? C44 C39 P1 120.7(4) . . ? C39 C40 C41 120.4(5) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C42 C41 C40 120.0(6) . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C43 C42 C41 120.3(5) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C42 C43 C44 120.2(5) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C39 C44 C43 120.4(5) . . ? C39 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C50 C45 C46 118.6(4) . . ? C50 C45 P1 121.4(4) . . ? C46 C45 P1 119.9(4) . . ? C45 C46 C47 120.9(5) . . ? C45 C46 H46 119.5 . . ? C47 C46 H46 119.5 . . ? C48 C47 C46 119.5(5) . . ? C48 C47 H47 120.3 . . ? C46 C47 H47 120.3 . . ? C47 C48 C49 120.3(5) . . ? C47 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? C48 C49 C50 120.3(5) . . ? C48 C49 H49 119.8 . . ? C50 C49 H49 119.8 . . ? C45 C50 C49 120.3(5) . . ? C45 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C52 C51 C56 118.8(5) . . ? C52 C51 P1 123.4(4) . . ? C56 C51 P1 117.8(4) . . ? C51 C52 C53 120.2(5) . . ? C51 C52 H52 119.9 . . ? C53 C52 H52 119.9 . . ? C54 C53 C52 120.6(5) . . ? C54 C53 H53 119.7 . . ? C52 C53 H53 119.7 . . ? C55 C54 C53 119.2(5) . . ? C55 C54 H54 120.4 . . ? C53 C54 H54 120.4 . . ? C54 C55 C56 120.4(5) . . ? C54 C55 H55 119.8 . . ? C56 C55 H55 119.8 . . ? C51 C56 C55 120.8(5) . . ? C51 C56 H56 119.6 . . ? C55 C56 H56 119.6 . . ? C58 C57 C62 118.8(4) . . ? C58 C57 P2 118.1(3) . . ? C62 C57 P2 122.9(3) . . ? C57 C58 C59 119.9(4) . . ? C57 C58 H58 120.0 . . ? C59 C58 H58 120.0 . . ? C60 C59 C58 120.3(4) . . ? C60 C59 H59 119.8 . . ? C58 C59 H59 119.8 . . ? C59 C60 C61 120.1(4) . . ? C59 C60 H60 119.9 . . ? C61 C60 H60 119.9 . . ? C60 C61 C62 120.0(4) . . ? C60 C61 H61 120.0 . . ? C62 C61 H61 120.0 . . ? C61 C62 C57 120.9(4) . . ? C61 C62 H62 119.6 . . ? C57 C62 H62 119.6 . . ? C68 C63 C64 119.7(5) . . ? C68 C63 P2 118.5(4) . . ? C64 C63 P2 121.6(4) . . ? C63 C64 C65 120.3(6) . . ? C63 C64 H64 119.9 . . ? C65 C64 H64 119.9 . . ? C66 C65 C64 119.4(7) . . ? C66 C65 H65 120.3 . . ? C64 C65 H65 120.3 . . ? C67 C66 C65 120.7(6) . . ? C67 C66 H66 119.7 . . ? C65 C66 H66 119.7 . . ? C66 C67 C68 119.6(6) . . ? C66 C67 H67 120.2 . . ? C68 C67 H67 120.2 . . ? C63 C68 C67 120.3(6) . . ? C63 C68 H68 119.8 . . ? C67 C68 H68 119.8 . . ? C74 C69 C70 118.4(5) . . ? C74 C69 P2 121.4(4) . . ? C70 C69 P2 120.1(5) . . ? C69 C70 C71 120.9(7) . . ? C69 C70 H70 119.5 . . ? C71 C70 H70 119.5 . . ? C72 C71 C70 118.7(8) . . ? C72 C71 H71 120.6 . . ? C70 C71 H71 120.6 . . ? C73 C72 C71 121.7(8) . . ? C73 C72 H72 119.2 . . ? C71 C72 H72 119.1 . . ? C72 C73 C74 120.2(9) . . ? C72 C73 H73 119.9 . . ? C74 C73 H73 119.9 . . ? C69 C74 C73 120.0(7) . . ? C69 C74 H74 120.0 . . ? C73 C74 H74 120.0 . . ? Cl2 C75 Cl1 118.9(7) . . ? Cl2 C75 H75A 107.6 . . ? Cl1 C75 H75A 107.6 . . ? Cl2 C75 H75B 107.6 . . ? Cl1 C75 H75B 107.6 . . ? H75A C75 H75B 107.0 . . ? C76 O7 H7 109.5 . . ? O7 C76 H76A 109.5 . . ? O7 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? O7 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C77 O8 H8A 109.5 . . ? O8 C77 H77A 109.5 . . ? O8 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? O8 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? 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 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C51 P1 C1 C2 170.6(3) . . . . ? C39 P1 C1 C2 -72.4(4) . . . . ? C45 P1 C1 C2 49.9(4) . . . . ? P1 C1 C2 O1 4.6(5) . . . . ? P1 C1 C2 C3 -177.4(3) . . . . ? O1 C2 C3 C8 26.3(5) . . . . ? C1 C2 C3 C8 -151.8(4) . . . . ? O1 C2 C3 C4 -154.8(4) . . . . ? C1 C2 C3 C4 27.2(5) . . . . ? C8 C3 C4 C5 -0.1(5) . . . . ? C2 C3 C4 C5 -179.0(3) . . . . ? C3 C4 C5 C6 1.3(5) . . . . ? C3 C4 C5 C9 -179.8(3) . . . . ? C4 C5 C6 O2 -179.5(3) . . . . ? C9 C5 C6 O2 1.7(5) . . . . ? C4 C5 C6 C7 -0.2(5) . . . . ? C9 C5 C6 C7 -179.0(3) . . . . ? O2 C6 C7 C8 177.2(3) . . . . ? C5 C6 C7 C8 -2.1(5) . . . . ? O2 C6 C7 C36 -5.3(5) . . . . ? C5 C6 C7 C36 175.4(3) . . . . ? C6 C7 C8 C3 3.4(5) . . . . ? C36 C7 C8 C3 -174.1(3) . . . . ? C4 C3 C8 C7 -2.3(5) . . . . ? C2 C3 C8 C7 176.6(3) . . . . ? C4 C5 C9 C10 -98.6(4) . . . . ? C6 C5 C9 C10 80.2(4) . . . . ? C5 C9 C10 C15 -103.2(4) . . . . ? C5 C9 C10 C11 74.3(4) . . . . ? C15 C10 C11 C12 1.8(5) . . . . ? C9 C10 C11 C12 -175.8(4) . . . . ? C10 C11 C12 C13 0.5(6) . . . . ? C11 C12 C13 C14 -0.6(6) . . . . ? C12 C13 C14 C15 -1.7(6) . . . . ? C12 C13 C14 C19 175.5(4) . . . . ? C11 C10 C15 C14 -4.3(5) . . . . ? C9 C10 C15 C14 173.2(3) . . . . ? C11 C10 C15 O3 -179.9(3) . . . . ? C9 C10 C15 O3 -2.3(5) . . . . ? C13 C14 C15 C10 4.2(5) . . . . ? C19 C14 C15 C10 -172.9(3) . . . . ? C13 C14 C15 O3 179.8(3) . . . . ? C19 C14 C15 O3 2.7(5) . . . . ? C16 O3 C15 C10 -99.7(4) . . . . ? C16 O3 C15 C14 84.6(4) . . . . ? C15 O3 C16 C17 -174.1(3) . . . . ? O3 C16 C17 C18 -71.1(4) . . . . ? C13 C14 C19 C20 -76.6(5) . . . . ? C15 C14 C19 C20 100.4(4) . . . . ? C14 C19 C20 C21 106.1(4) . . . . ? C14 C19 C20 C25 -75.1(5) . . . . ? C25 C20 C21 C22 -0.1(6) . . . . ? C19 C20 C21 C22 178.7(4) . . . . ? C20 C21 C22 C23 0.5(6) . . . . ? C20 C21 C22 C37 -177.7(3) . . . . ? C21 C22 C23 C24 -0.2(6) . . . . ? C37 C22 C23 C24 177.9(4) . . . . ? C22 C23 C24 C25 -0.5(6) . . . . ? C22 C23 C24 C26 180.0(4) . . . . ? C21 C20 C25 O4 177.3(3) . . . . ? C19 C20 C25 O4 -1.5(6) . . . . ? C21 C20 C25 C24 -0.6(6) . . . . ? C19 C20 C25 C24 -179.4(4) . . . . ? C23 C24 C25 O4 -177.1(3) . . . . ? C26 C24 C25 O4 2.4(6) . . . . ? C23 C24 C25 C20 0.9(6) . . . . ? C26 C24 C25 C20 -179.6(4) . . . . ? C23 C24 C26 C27 -104.0(4) . . . . ? C25 C24 C26 C27 76.4(5) . . . . ? C24 C26 C27 C28 71.7(5) . . . . ? C24 C26 C27 C32 -105.3(4) . . . . ? C32 C27 C28 C29 2.4(6) . . . . ? C26 C27 C28 C29 -174.7(4) . . . . ? C27 C28 C29 C30 1.0(7) . . . . ? C28 C29 C30 C31 -2.2(6) . . . . ? C29 C30 C31 C32 -0.1(6) . . . . ? C29 C30 C31 C36 178.5(4) . . . . ? C28 C27 C32 O5 179.9(3) . . . . ? C26 C27 C32 O5 -3.0(5) . . . . ? C28 C27 C32 C31 -4.8(6) . . . . ? C26 C27 C32 C31 172.3(4) . . . . ? C33 O5 C32 C27 -97.1(4) . . . . ? C33 O5 C32 C31 87.5(4) . . . . ? C30 C31 C32 C27 3.7(5) . . . . ? C36 C31 C32 C27 -174.9(3) . . . . ? C30 C31 C32 O5 179.0(3) . . . . ? C36 C31 C32 O5 0.5(5) . . . . ? C32 O5 C33 C34 -156.2(4) . . . . ? O5 C33 C34 C35 -61.5(5) . . . . ? C8 C7 C36 C31 102.3(4) . . . . ? C6 C7 C36 C31 -75.1(5) . . . . ? C30 C31 C36 C7 -74.1(5) . . . . ? C32 C31 C36 C7 104.4(4) . . . . ? C23 C22 C37 O6 -174.4(4) . . . . ? C21 C22 C37 O6 3.7(5) . . . . ? C23 C22 C37 C38 5.0(6) . . . . ? C21 C22 C37 C38 -176.8(4) . . . . ? O6 C37 C38 P2 1.5(5) . . . . ? C22 C37 C38 P2 -177.9(3) . . . . ? C57 P2 C38 C37 -61.8(4) . . . . ? C63 P2 C38 C37 63.2(4) . . . . ? C69 P2 C38 C37 -179.9(3) . . . . ? C1 P1 C39 C40 26.3(5) . . . . ? C51 P1 C39 C40 143.6(4) . . . . ? C45 P1 C39 C40 -99.6(4) . . . . ? C1 P1 C39 C44 -158.4(4) . . . . ? C51 P1 C39 C44 -41.1(5) . . . . ? C45 P1 C39 C44 75.8(4) . . . . ? C44 C39 C40 C41 1.4(8) . . . . ? P1 C39 C40 C41 176.8(4) . . . . ? C39 C40 C41 C42 -1.4(9) . . . . ? C40 C41 C42 C43 1.5(10) . . . . ? C41 C42 C43 C44 -1.5(10) . . . . ? C40 C39 C44 C43 -1.4(8) . . . . ? P1 C39 C44 C43 -176.9(4) . . . . ? C42 C43 C44 C39 1.5(9) . . . . ? C1 P1 C45 C50 -121.8(4) . . . . ? C51 P1 C45 C50 120.1(4) . . . . ? C39 P1 C45 C50 6.5(5) . . . . ? C1 P1 C45 C46 56.1(4) . . . . ? C51 P1 C45 C46 -62.0(4) . . . . ? C39 P1 C45 C46 -175.6(4) . . . . ? C50 C45 C46 C47 -0.9(7) . . . . ? P1 C45 C46 C47 -178.9(4) . . . . ? C45 C46 C47 C48 2.0(8) . . . . ? C46 C47 C48 C49 -1.2(9) . . . . ? C47 C48 C49 C50 -0.8(9) . . . . ? C46 C45 C50 C49 -1.0(8) . . . . ? P1 C45 C50 C49 177.0(4) . . . . ? C48 C49 C50 C45 1.9(9) . . . . ? C1 P1 C51 C52 -114.6(4) . . . . ? C39 P1 C51 C52 121.1(4) . . . . ? C45 P1 C51 C52 7.5(5) . . . . ? C1 P1 C51 C56 63.7(4) . . . . ? C39 P1 C51 C56 -60.5(4) . . . . ? C45 P1 C51 C56 -174.1(4) . . . . ? C56 C51 C52 C53 -2.5(7) . . . . ? P1 C51 C52 C53 175.8(4) . . . . ? C51 C52 C53 C54 1.4(8) . . . . ? C52 C53 C54 C55 0.4(8) . . . . ? C53 C54 C55 C56 -1.1(9) . . . . ? C52 C51 C56 C55 1.9(8) . . . . ? P1 C51 C56 C55 -176.6(5) . . . . ? C54 C55 C56 C51 -0.1(10) . . . . ? C38 P2 C57 C58 -20.7(4) . . . . ? C63 P2 C57 C58 -148.8(3) . . . . ? C69 P2 C57 C58 98.7(3) . . . . ? C38 P2 C57 C62 164.8(3) . . . . ? C63 P2 C57 C62 36.6(4) . . . . ? C69 P2 C57 C62 -75.9(4) . . . . ? C62 C57 C58 C59 0.2(6) . . . . ? P2 C57 C58 C59 -174.6(3) . . . . ? C57 C58 C59 C60 0.3(6) . . . . ? C58 C59 C60 C61 -0.9(7) . . . . ? C59 C60 C61 C62 1.1(7) . . . . ? C60 C61 C62 C57 -0.6(6) . . . . ? C58 C57 C62 C61 0.0(6) . . . . ? P2 C57 C62 C61 174.6(3) . . . . ? C38 P2 C63 C68 79.8(4) . . . . ? C57 P2 C63 C68 -151.8(3) . . . . ? C69 P2 C63 C68 -38.7(4) . . . . ? C38 P2 C63 C64 -95.6(4) . . . . ? C57 P2 C63 C64 32.8(4) . . . . ? C69 P2 C63 C64 145.8(4) . . . . ? C68 C63 C64 C65 1.5(7) . . . . ? P2 C63 C64 C65 176.9(4) . . . . ? C63 C64 C65 C66 -0.7(8) . . . . ? C64 C65 C66 C67 -0.6(9) . . . . ? C65 C66 C67 C68 1.1(10) . . . . ? C64 C63 C68 C67 -1.0(7) . . . . ? P2 C63 C68 C67 -176.5(4) . . . . ? C66 C67 C68 C63 -0.3(8) . . . . ? C38 P2 C69 C74 1.4(5) . . . . ? C57 P2 C69 C74 -122.0(4) . . . . ? C63 P2 C69 C74 123.7(4) . . . . ? C38 P2 C69 C70 178.8(4) . . . . ? C57 P2 C69 C70 55.4(5) . . . . ? C63 P2 C69 C70 -58.9(5) . . . . ? C74 C69 C70 C71 0.5(9) . . . . ? P2 C69 C70 C71 -177.0(5) . . . . ? C69 C70 C71 C72 -0.8(11) . . . . ? C70 C71 C72 C73 0.8(13) . . . . ? C71 C72 C73 C74 -0.5(13) . . . . ? C70 C69 C74 C73 -0.1(9) . . . . ? P2 C69 C74 C73 177.3(5) . . . . ? C72 C73 C74 C69 0.2(11) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.094 _refine_diff_density_min -0.990 _refine_diff_density_rms 0.077 data_shelxl _database_code_depnum_ccdc_archive 'CCDC 294727' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C116 H108 Ni2 O6 P4' _chemical_formula_sum 'C116 H108 Ni2 O6 P4' _chemical_formula_weight 1839.32 _chemical_absolute_configuration ? 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' Ni Ni 0.3393 1.1124 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/C' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.498(2) _cell_length_b 28.088(2) _cell_length_c 18.725(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.181(3) _cell_angle_gamma 90.00 _cell_volume 9630.0(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22595 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3872 _exptl_absorpt_coefficient_mu 0.514 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28035 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 30.05 _reflns_number_total 28035 _reflns_number_gt 17204 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1373P)^2^+17.6089P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 28035 _refine_ls_number_parameters 1137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1394 _refine_ls_R_factor_gt 0.0839 _refine_ls_wR_factor_ref 0.2572 _refine_ls_wR_factor_gt 0.2162 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.943 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.46256(2) 0.156919(14) 0.68496(2) 0.02618(11) Uani 1 1 d . . . Ni2 Ni -0.01033(3) 0.162596(19) 0.66838(3) 0.04179(14) Uani 1 1 d . . . P1 P 0.44476(5) 0.21135(3) 0.76306(4) 0.02673(18) Uani 1 1 d . . . P2 P 0.47552(5) 0.09892(3) 0.60681(5) 0.03085(19) Uani 1 1 d . . . P3 P -0.03246(6) 0.20950(4) 0.75439(5) 0.0411(2) Uani 1 1 d . . . P4 P 0.00298(6) 0.11075(4) 0.58319(5) 0.0431(2) Uani 1 1 d . . . O1 O 0.36194(14) -0.01166(9) 1.01909(15) 0.0417(6) Uani 1 1 d . . . O2 O 0.14027(13) -0.00811(9) 1.01494(15) 0.0403(6) Uani 1 1 d . . . O3 O 0.25244(14) 0.11035(9) 1.00664(12) 0.0352(5) Uani 1 1 d . . . O4 O 0.23344(19) 0.00736(11) 0.8712(3) 0.0836(14) Uani 1 1 d . . . O6 O 0.44443(13) 0.11141(8) 0.75679(12) 0.0305(5) Uani 1 1 d . . . O5 O 0.02332(15) 0.11763(10) 0.74221(14) 0.0413(6) Uani 1 1 d . . . C1 C 0.43225(19) 0.17462(12) 0.83603(17) 0.0299(7) Uani 1 1 d . . . H1 H 0.4258 0.1865 0.8822 0.036 Uiso 1 1 calc . . . C2 C 0.43272(16) 0.12702(11) 0.81997(17) 0.0258(6) Uani 1 1 d . . . C3 C 0.41784(17) 0.09014(11) 0.87320(18) 0.0280(6) Uani 1 1 d . . . C4 C 0.41474(18) 0.10180(12) 0.94534(18) 0.0310(7) Uani 1 1 d . . . H4 H 0.4248 0.1336 0.9608 0.037 Uiso 1 1 calc . . . C5 C 0.39753(18) 0.06861(13) 0.99511(19) 0.0326(7) Uani 1 1 d . . . C6 C 0.38297(18) 0.02198(13) 0.9719(2) 0.0358(8) Uani 1 1 d . . . C7 C 0.38564(19) 0.00880(12) 0.9005(2) 0.0367(8) Uani 1 1 d . . . C8 C 0.40378(18) 0.04301(12) 0.8516(2) 0.0325(7) Uani 1 1 d . . . H8 H 0.4066 0.0341 0.8032 0.039 Uiso 1 1 calc . . . C9 C 0.3727(2) -0.04209(13) 0.8760(3) 0.0512(11) Uani 1 1 d . . . H9A H 0.4110 -0.0618 0.9042 0.061 Uiso 1 1 calc . . . H9B H 0.3809 -0.0438 0.8250 0.061 Uiso 1 1 calc . . . C10 C 0.2994(2) -0.06565(12) 0.8810(2) 0.0370(8) Uani 1 1 d . . . C11 C 0.2979(2) -0.11484(13) 0.8910(3) 0.0449(9) Uani 1 1 d . . . H11 H 0.3421 -0.1325 0.8940 0.054 Uiso 1 1 calc . . . C12 C 0.2338(2) -0.13812(13) 0.8966(3) 0.0593(13) Uani 1 1 d . . . H12 H 0.2341 -0.1715 0.9044 0.071 Uiso 1 1 calc . . . C13 C 0.1691(2) -0.11353(14) 0.8910(3) 0.0510(11) Uani 1 1 d . . . H13 H 0.1252 -0.1302 0.8953 0.061 Uiso 1 1 calc . . . C14 C 0.1669(2) -0.06468(12) 0.8793(2) 0.0370(8) Uani 1 1 d . . . C15 C 0.2331(2) -0.04157(12) 0.8752(2) 0.0386(8) Uani 1 1 d . . . C16 C 0.0935(2) -0.03965(14) 0.8696(3) 0.0519(11) Uani 1 1 d . . . H16A H 0.0601 -0.0590 0.8947 0.062 Uiso 1 1 calc . . . H16B H 0.0742 -0.0406 0.8175 0.062 Uiso 1 1 calc . . . C17 C 0.08759(18) 0.01157(12) 0.8945(2) 0.0361(8) Uani 1 1 d . . . C18 C 0.05880(19) 0.04587(13) 0.8448(2) 0.0343(7) Uani 1 1 d . . . H18 H 0.0440 0.0367 0.7960 0.041 Uiso 1 1 calc . . . C19 C 0.05114(18) 0.09321(12) 0.86459(19) 0.0314(7) Uani 1 1 d . . . C20 C 0.07280(19) 0.10557(12) 0.93658(19) 0.0327(7) Uani 1 1 d . . . H20 H 0.0680 0.1377 0.9509 0.039 Uiso 1 1 calc . . . C21 C 0.10115(18) 0.07239(13) 0.9880(2) 0.0335(7) Uani 1 1 d . . . C22 C 0.10832(17) 0.02518(13) 0.9658(2) 0.0337(7) Uani 1 1 d . . . C23 C 0.1210(2) 0.08801(15) 1.0656(2) 0.0420(9) Uani 1 1 d . . . H23A H 0.1145 0.1230 1.0674 0.050 Uiso 1 1 calc . . . H23B H 0.0854 0.0735 1.0939 0.050 Uiso 1 1 calc . . . C24 C 0.1968(2) 0.07636(13) 1.10292(18) 0.0352(7) Uani 1 1 d . . . C25 C 0.2058(2) 0.05489(14) 1.17113(19) 0.0394(8) Uani 1 1 d . . . H25 H 0.1640 0.0482 1.1935 0.047 Uiso 1 1 calc . . . C26 C 0.2735(2) 0.04331(14) 1.20631(18) 0.0403(8) Uani 1 1 d . . . H26 H 0.2783 0.0294 1.2530 0.048 Uiso 1 1 calc . . . C27 C 0.3352(2) 0.05197(14) 1.17370(18) 0.0374(8) Uani 1 1 d . . . H27 H 0.3820 0.0430 1.1975 0.045 Uiso 1 1 calc . . . C28 C 0.3286(2) 0.07384(13) 1.10582(18) 0.0357(8) Uani 1 1 d . . . C29 C 0.2594(2) 0.08708(12) 1.07274(17) 0.0331(7) Uani 1 1 d . . . C30 C 0.3963(2) 0.08505(16) 1.0724(2) 0.0441(9) Uani 1 1 d . . . H30A H 0.4387 0.0706 1.1030 0.053 Uiso 1 1 calc . . . H30B H 0.4035 0.1200 1.0740 0.053 Uiso 1 1 calc . . . C31 C 0.02271(19) 0.12962(13) 0.80937(19) 0.0344(7) Uani 1 1 d . . . C32 C -0.0025(2) 0.17285(14) 0.8285(2) 0.0422(9) Uani 1 1 d . . . H32 H -0.0037 0.1821 0.8771 0.051 Uiso 1 1 calc . . . C33 C 0.35947(19) 0.24463(12) 0.73962(18) 0.0324(7) Uani 1 1 d . . . C34 C 0.3537(2) 0.29287(13) 0.7245(2) 0.0415(9) Uani 1 1 d . . . H34 H 0.3965 0.3118 0.7265 0.050 Uiso 1 1 calc . . . C35 C 0.2847(3) 0.31389(15) 0.7063(2) 0.0511(11) Uani 1 1 d . . . H35 H 0.2812 0.3470 0.6959 0.061 Uiso 1 1 calc . . . C36 C 0.2225(2) 0.28707(18) 0.7033(3) 0.0562(12) Uani 1 1 d . . . H36 H 0.1760 0.3015 0.6905 0.067 Uiso 1 1 calc . . . C37 C 0.2275(3) 0.2393(2) 0.7190(4) 0.0708(15) Uani 1 1 d . . . H37 H 0.1844 0.2207 0.7174 0.085 Uiso 1 1 calc . . . C38 C 0.2956(2) 0.21805(16) 0.7372(3) 0.0571(12) Uani 1 1 d . . . H38 H 0.2986 0.1850 0.7480 0.069 Uiso 1 1 calc . . . C39 C 0.51370(19) 0.25622(12) 0.79324(19) 0.0311(7) Uani 1 1 d . . . C40 C 0.5327(2) 0.29216(12) 0.7477(2) 0.0374(8) Uani 1 1 d . . . H40 H 0.5103 0.2934 0.6988 0.045 Uiso 1 1 calc . . . C41 C 0.5846(2) 0.32622(14) 0.7740(2) 0.0461(9) Uani 1 1 d . . . H41 H 0.5971 0.3507 0.7431 0.055 Uiso 1 1 calc . . . C42 C 0.6176(3) 0.32453(16) 0.8447(3) 0.0550(11) Uani 1 1 d . . . H42 H 0.6527 0.3479 0.8624 0.066 Uiso 1 1 calc . . . C43 C 0.5998(3) 0.28902(17) 0.8895(3) 0.0562(11) Uani 1 1 d . . . H43 H 0.6230 0.2878 0.9381 0.067 Uiso 1 1 calc . . . C44 C 0.5483(2) 0.25511(14) 0.8643(2) 0.0430(9) Uani 1 1 d . . . H44 H 0.5363 0.2308 0.8958 0.052 Uiso 1 1 calc . . . C45 C 0.4888(2) 0.20575(12) 0.62385(17) 0.0316(7) Uani 1 1 d . . . C46 C 0.5622(2) 0.21440(14) 0.6191(2) 0.0422(9) Uani 1 1 d . . . H46 H 0.5983 0.1937 0.6432 0.051 Uiso 1 1 calc . . . C47 C 0.5838(3) 0.25293(18) 0.5797(2) 0.0566(12) Uani 1 1 d . . . H47 H 0.6340 0.2586 0.5775 0.068 Uiso 1 1 calc . . . C48 C 0.5308(4) 0.28284(16) 0.5439(2) 0.0621(14) Uani 1 1 d . . . H48 H 0.5451 0.3094 0.5179 0.075 Uiso 1 1 calc . . . C49 C 0.4584(3) 0.27439(16) 0.5457(2) 0.0571(12) Uani 1 1 d . . . H49 H 0.4224 0.2944 0.5198 0.069 Uiso 1 1 calc . . . C50 C 0.4375(2) 0.23636(14) 0.5857(2) 0.0419(9) Uani 1 1 d . . . H50 H 0.3870 0.2310 0.5871 0.050 Uiso 1 1 calc . . . C51 C 0.4389(2) 0.10299(13) 0.51074(19) 0.0346(7) Uani 1 1 d . . . C52 C 0.4011(2) 0.06553(14) 0.4741(2) 0.0444(9) Uani 1 1 d . . . H52 H 0.3949 0.0367 0.4989 0.053 Uiso 1 1 calc . . . C53 C 0.3724(3) 0.06964(16) 0.4018(2) 0.0497(10) Uani 1 1 d . . . H53 H 0.3468 0.0436 0.3775 0.060 Uiso 1 1 calc . . . C54 C 0.3809(3) 0.11106(18) 0.3651(2) 0.0587(12) Uani 1 1 d . . . H54 H 0.3601 0.1142 0.3160 0.070 Uiso 1 1 calc . . . C55 C 0.4195(4) 0.14787(17) 0.3999(2) 0.0678(15) Uani 1 1 d . . . H55 H 0.4264 0.1763 0.3744 0.081 Uiso 1 1 calc . . . C56 C 0.4489(3) 0.14400(16) 0.4725(2) 0.0566(12) Uani 1 1 d . . . H56 H 0.4760 0.1697 0.4959 0.068 Uiso 1 1 calc . . . C57 C 0.5713(2) 0.08469(14) 0.6076(2) 0.0418(9) Uani 1 1 d . . . C58 C 0.6013(3) 0.0723(2) 0.5464(3) 0.0597(12) Uani 1 1 d . . . H58 H 0.5719 0.0722 0.5005 0.072 Uiso 1 1 calc . . . C59 C 0.6741(3) 0.0600(3) 0.5526(4) 0.0832(18) Uani 1 1 d . . . H59 H 0.6941 0.0508 0.5108 0.100 Uiso 1 1 calc . . . C60 C 0.7175(3) 0.0609(3) 0.6173(4) 0.088(2) Uani 1 1 d . . . H60 H 0.7679 0.0532 0.6204 0.105 Uiso 1 1 calc . . . C61 C 0.6886(3) 0.0729(2) 0.6784(3) 0.0750(16) Uani 1 1 d . . . H61 H 0.7187 0.0728 0.7240 0.090 Uiso 1 1 calc . . . C62 C 0.6161(3) 0.08511(18) 0.6738(3) 0.0579(12) Uani 1 1 d . . . H62 H 0.5965 0.0939 0.7161 0.069 Uiso 1 1 calc . . . C63 C -0.1289(2) 0.22168(15) 0.7565(2) 0.0431(9) Uani 1 1 d . . . C64 C -0.1638(3) 0.26457(18) 0.7358(3) 0.0649(14) Uani 1 1 d . . . H64 H -0.1368 0.2903 0.7198 0.078 Uiso 1 1 calc . . . C65 C -0.2383(3) 0.26981(19) 0.7383(3) 0.0699(15) Uani 1 1 d . . . H65 H -0.2615 0.2991 0.7240 0.084 Uiso 1 1 calc . . . C66 C -0.2785(3) 0.23356(19) 0.7611(3) 0.0646(13) Uani 1 1 d . . . H66 H -0.3285 0.2377 0.7662 0.078 Uiso 1 1 calc . . . C67 C -0.2446(4) 0.1922(3) 0.7760(7) 0.135(4) Uani 1 1 d . . . H67 H -0.2723 0.1657 0.7885 0.162 Uiso 1 1 calc . . . C68 C -0.1709(3) 0.1861(2) 0.7739(5) 0.112(3) Uani 1 1 d . . . H68 H -0.1495 0.1558 0.7852 0.135 Uiso 1 1 calc . . . C69 C 0.0142(2) 0.26636(15) 0.7680(2) 0.0476(10) Uani 1 1 d . . . C70 C 0.0657(3) 0.27388(17) 0.8289(3) 0.0587(12) Uani 1 1 d . . . H70 H 0.0752 0.2492 0.8636 0.070 Uiso 1 1 calc . . . C71 C 0.1027(3) 0.3158(2) 0.8400(4) 0.0737(16) Uani 1 1 d . . . H71 H 0.1361 0.3202 0.8829 0.088 Uiso 1 1 calc . . . C72 C 0.0921(3) 0.35186(19) 0.7895(4) 0.0750(16) Uani 1 1 d . . . H72 H 0.1191 0.3806 0.7969 0.090 Uiso 1 1 calc . . . C73 C 0.0420(3) 0.34575(17) 0.7283(4) 0.0692(15) Uani 1 1 d . . . H73 H 0.0339 0.3706 0.6937 0.083 Uiso 1 1 calc . . . C74 C 0.0032(3) 0.30350(17) 0.7170(3) 0.0554(11) Uani 1 1 d . . . H74 H -0.0310 0.2996 0.6746 0.066 Uiso 1 1 calc . . . C75 C -0.0406(4) 0.20972(19) 0.5984(2) 0.0716(16) Uani 1 1 d . . . C76 C 0.0112(5) 0.2386(2) 0.5715(3) 0.096(2) Uani 1 1 d . . . H76 H 0.0615 0.2342 0.5889 0.115 Uiso 1 1 calc . . . C77 C -0.0093(9) 0.2731(3) 0.5203(5) 0.166(6) Uani 1 1 d . . . H77 H 0.0266 0.2918 0.5021 0.199 Uiso 1 1 calc . . . C78 C -0.0812(10) 0.2801(4) 0.4961(5) 0.208(9) Uani 1 1 d . . . H78 H -0.0949 0.3045 0.4617 0.249 Uiso 1 1 calc . . . C79 C -0.1355(7) 0.2526(5) 0.5199(4) 0.182(7) Uani 1 1 d . . . H79 H -0.1856 0.2574 0.5016 0.219 Uiso 1 1 calc . . . C80 C -0.1135(4) 0.2167(3) 0.5731(3) 0.115(3) Uani 1 1 d . . . H80 H -0.1494 0.1976 0.5910 0.138 Uiso 1 1 calc . . . C81 C -0.0628(3) 0.1144(2) 0.5010(3) 0.0723(16) Uani 1 1 d . . . C82 C -0.0505(3) 0.1470(2) 0.4475(2) 0.0588(12) Uani 1 1 d . . . H82 H -0.0059 0.1643 0.4527 0.071 Uiso 1 1 calc . . . C83 C -0.1013(4) 0.1545(3) 0.3876(3) 0.096(2) Uani 1 1 d . . . H83 H -0.0913 0.1759 0.3510 0.116 Uiso 1 1 calc . . . C84 C -0.1662(5) 0.1309(7) 0.3812(5) 0.218(8) Uani 1 1 d . . . H84 H -0.2018 0.1359 0.3401 0.262 Uiso 1 1 calc . . . C85 C -0.1801(6) 0.1001(8) 0.4336(6) 0.297(13) Uani 1 1 d . . . H85 H -0.2264 0.0851 0.4297 0.357 Uiso 1 1 calc . . . C86 C -0.1272(5) 0.0901(6) 0.4936(4) 0.212(8) Uani 1 1 d . . . H86 H -0.1363 0.0669 0.5281 0.254 Uiso 1 1 calc . . . C87 C -0.0059(3) 0.05166(16) 0.6180(2) 0.099(3) Uani 1 1 d G . . C88 C -0.0634(3) 0.0438(2) 0.6569(2) 0.158(5) Uani 1 1 d G . . H88 H -0.0979 0.0684 0.6610 0.190 Uiso 1 1 calc . . . C89 C -0.0705(4) 0.0001(3) 0.6898(3) 0.296(13) Uani 1 1 d G . . H89 H -0.1098 -0.0053 0.7164 0.355 Uiso 1 1 calc . . . C90 C -0.0201(5) -0.0359(2) 0.6838(3) 0.309(15) Uani 1 1 d G . . H90 H -0.0249 -0.0658 0.7063 0.371 Uiso 1 1 calc . . . C91 C 0.0374(5) -0.02803(17) 0.6449(3) 0.273(12) Uani 1 1 d G . . H91 H 0.0719 -0.0526 0.6408 0.328 Uiso 1 1 calc . . . C92 C 0.0445(4) 0.01572(17) 0.6120(2) 0.156(5) Uani 1 1 d G . . H92 H 0.0838 0.0211 0.5854 0.188 Uiso 1 1 calc . . . C93 C 0.0904(2) 0.11335(16) 0.5493(2) 0.0468(10) Uani 1 1 d . . . C94 C 0.1061(3) 0.0866(2) 0.4911(3) 0.0766(17) Uani 1 1 d . . . H94 H 0.0705 0.0658 0.4665 0.092 Uiso 1 1 calc . . . C95 C 0.1743(5) 0.0906(4) 0.4692(3) 0.115(3) Uani 1 1 d . . . H95 H 0.1852 0.0719 0.4298 0.138 Uiso 1 1 calc . . . C96 C 0.2262(4) 0.1207(4) 0.5029(4) 0.125(4) Uani 1 1 d . . . H96 H 0.2726 0.1229 0.4869 0.150 Uiso 1 1 calc . . . C97 C 0.2113(3) 0.1476(3) 0.5593(4) 0.097(2) Uani 1 1 d . . . H97 H 0.2469 0.1690 0.5824 0.117 Uiso 1 1 calc . . . C98 C 0.1434(3) 0.1434(2) 0.5832(3) 0.0608(12) Uani 1 1 d . . . H98 H 0.1335 0.1617 0.6235 0.073 Uiso 1 1 calc . . . C99 C 0.4352(2) 0.04310(13) 0.6317(2) 0.0407(9) Uani 1 1 d . . . C100 C 0.3603(3) 0.04275(15) 0.6345(3) 0.0509(10) Uani 1 1 d . . . H100 H 0.3332 0.0715 0.6262 0.061 Uiso 1 1 calc . . . C101 C 0.3247(3) 0.0014(2) 0.6493(3) 0.0715(15) Uani 1 1 d . . . H101 H 0.2733 0.0015 0.6494 0.086 Uiso 1 1 calc . . . C102 C 0.3638(4) -0.04014(19) 0.6637(3) 0.0763(16) Uani 1 1 d . . . H102 H 0.3396 -0.0684 0.6750 0.092 Uiso 1 1 calc . . . C103 C 0.4366(4) -0.04068(17) 0.6619(3) 0.0724(16) Uani 1 1 d . . . H103 H 0.4631 -0.0695 0.6714 0.087 Uiso 1 1 calc . . . C104 C 0.4739(3) 0.00107(15) 0.6461(3) 0.0550(11) Uani 1 1 d . . . H104 H 0.5252 0.0004 0.6453 0.066 Uiso 1 1 calc . . . C105 C 0.4229(3) -0.0300(2) 1.0699(3) 0.0714(16) Uani 1 1 d . . . H10A H 0.4477 -0.0034 1.0982 0.086 Uiso 1 1 calc . . . H10B H 0.4588 -0.0457 1.0432 0.086 Uiso 1 1 calc . . . C106 C 0.3938(3) -0.0659(2) 1.1207(3) 0.0674(14) Uani 1 1 d . . . H10C H 0.4311 -0.0713 1.1633 0.081 Uiso 1 1 calc . . . H10D H 0.3496 -0.0528 1.1378 0.081 Uiso 1 1 calc . . . C107 C 0.3759(4) -0.1109(2) 1.0840(4) 0.096(2) Uani 1 1 d . . . H10E H 0.3382 -0.1056 1.0423 0.144 Uiso 1 1 calc . . . H10F H 0.3577 -0.1333 1.1173 0.144 Uiso 1 1 calc . . . H10G H 0.4198 -0.1240 1.0675 0.144 Uiso 1 1 calc . . . C108 C 0.0922(3) -0.0327(3) 1.0544(5) 0.119(3) Uani 1 1 d . . . H10H H 0.0569 -0.0517 1.0212 0.143 Uiso 1 1 calc . . . H10I H 0.0645 -0.0097 1.0801 0.143 Uiso 1 1 calc . . . C109 C 0.1376(4) -0.0659(3) 1.1091(7) 0.151(5) Uani 1 1 d . . . H10J H 0.1758 -0.0471 1.1392 0.181 Uiso 1 1 calc . . . H10K H 0.1055 -0.0802 1.1414 0.181 Uiso 1 1 calc . . . C110 C 0.1670(9) -0.0983(6) 1.0771(9) 0.196(6) Uiso 1 1 d . . . H11A H 0.1346 -0.1074 1.0332 0.294 Uiso 1 1 calc . . . H11B H 0.1760 -0.1260 1.1089 0.294 Uiso 1 1 calc . . . H11C H 0.2135 -0.0868 1.0642 0.294 Uiso 1 1 calc . . . C111 C 0.2522(3) 0.16139(15) 1.0134(2) 0.0491(10) Uani 1 1 d . . . H11D H 0.2979 0.1722 1.0430 0.059 Uiso 1 1 calc . . . H11E H 0.2105 0.1716 1.0375 0.059 Uiso 1 1 calc . . . C112 C 0.2459(2) 0.18279(15) 0.9385(2) 0.0487(10) Uani 1 1 d . . . H11F H 0.2866 0.1712 0.9141 0.058 Uiso 1 1 calc . . . H11G H 0.1995 0.1724 0.9098 0.058 Uiso 1 1 calc . . . C113 C 0.2480(4) 0.23667(19) 0.9421(3) 0.0753(17) Uani 1 1 d . . . H11H H 0.2057 0.2483 0.9631 0.113 Uiso 1 1 calc . . . H11I H 0.2465 0.2497 0.8934 0.113 Uiso 1 1 calc . . . H11J H 0.2930 0.2469 0.9722 0.113 Uiso 1 1 calc . . . C114 C 0.2270(3) 0.0253(3) 0.8026(5) 0.109(3) Uani 1 1 d . . . H11K H 0.1814 0.0143 0.7732 0.131 Uiso 1 1 calc . . . H11L H 0.2691 0.0160 0.7785 0.131 Uiso 1 1 calc . . . C115 C 0.2255(3) 0.0833(2) 0.8157(4) 0.0778(18) Uani 1 1 d . . . H11M H 0.1888 0.0914 0.8473 0.093 Uiso 1 1 calc . . . H11N H 0.2739 0.0944 0.8390 0.093 Uiso 1 1 calc . . . C116 C 0.2080(5) 0.1043(3) 0.7498(5) 0.109(3) Uani 1 1 d . . . H11O H 0.2449 0.0962 0.7191 0.164 Uiso 1 1 calc . . . H11P H 0.2064 0.1390 0.7558 0.164 Uiso 1 1 calc . . . H11Q H 0.1600 0.0930 0.7272 0.164 Uiso 1 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0338(2) 0.0237(2) 0.0211(2) 0.00069(15) 0.00407(16) 0.00229(16) Ni2 0.0480(3) 0.0492(3) 0.0298(2) 0.0061(2) 0.0109(2) 0.0101(2) P1 0.0351(4) 0.0222(4) 0.0232(4) 0.0016(3) 0.0055(3) 0.0018(3) P2 0.0393(5) 0.0287(4) 0.0246(4) -0.0022(3) 0.0047(3) 0.0039(4) P3 0.0484(6) 0.0429(5) 0.0330(5) 0.0068(4) 0.0095(4) 0.0150(4) P4 0.0523(6) 0.0477(6) 0.0283(5) 0.0017(4) 0.0025(4) -0.0144(5) O1 0.0348(13) 0.0387(14) 0.0543(17) 0.0222(12) 0.0158(12) 0.0029(11) O2 0.0298(12) 0.0387(14) 0.0530(16) 0.0133(12) 0.0076(11) 0.0028(11) O3 0.0426(13) 0.0404(14) 0.0221(11) 0.0095(10) 0.0029(10) -0.0025(11) O4 0.058(2) 0.0272(15) 0.177(4) 0.034(2) 0.056(2) 0.0124(14) O6 0.0423(13) 0.0249(11) 0.0253(11) 0.0007(9) 0.0080(10) 0.0005(10) O5 0.0516(15) 0.0433(15) 0.0286(13) -0.0001(11) 0.0045(11) 0.0121(12) C1 0.0391(17) 0.0286(16) 0.0226(15) 0.0011(12) 0.0070(13) 0.0015(14) C2 0.0249(14) 0.0273(15) 0.0247(15) 0.0014(12) 0.0013(11) -0.0008(12) C3 0.0274(15) 0.0262(15) 0.0304(16) 0.0045(12) 0.0046(12) 0.0009(12) C4 0.0305(16) 0.0316(17) 0.0307(17) 0.0057(13) 0.0037(13) 0.0003(13) C5 0.0259(15) 0.0397(19) 0.0319(17) 0.0123(14) 0.0033(13) -0.0006(14) C6 0.0245(15) 0.0372(19) 0.047(2) 0.0143(16) 0.0113(14) 0.0045(14) C7 0.0287(16) 0.0280(17) 0.056(2) 0.0082(16) 0.0137(15) 0.0031(13) C8 0.0305(16) 0.0273(16) 0.0416(19) 0.0035(14) 0.0112(14) 0.0024(13) C9 0.048(2) 0.0253(18) 0.087(3) 0.0038(19) 0.033(2) 0.0032(16) C10 0.0425(19) 0.0243(16) 0.047(2) 0.0026(14) 0.0141(16) 0.0018(14) C11 0.046(2) 0.0234(17) 0.065(3) 0.0001(17) 0.0090(19) 0.0044(16) C12 0.052(2) 0.0187(17) 0.106(4) 0.003(2) 0.006(2) -0.0030(17) C13 0.044(2) 0.0246(18) 0.084(3) -0.0066(19) 0.007(2) -0.0093(16) C14 0.0399(19) 0.0266(17) 0.043(2) -0.0040(14) 0.0012(15) -0.0014(14) C15 0.046(2) 0.0229(16) 0.050(2) 0.0065(15) 0.0177(17) 0.0012(15) C16 0.0332(19) 0.0305(19) 0.088(3) -0.006(2) -0.004(2) -0.0040(16) C17 0.0236(15) 0.0279(17) 0.057(2) -0.0016(15) 0.0060(15) -0.0021(13) C18 0.0291(16) 0.0345(18) 0.0379(19) -0.0064(14) 0.0001(14) -0.0022(14) C19 0.0277(15) 0.0318(17) 0.0349(18) -0.0012(14) 0.0050(13) -0.0005(13) C20 0.0361(17) 0.0303(17) 0.0319(17) 0.0004(13) 0.0059(14) 0.0009(14) C21 0.0264(15) 0.0386(19) 0.0371(18) 0.0044(14) 0.0099(13) 0.0007(14) C22 0.0208(14) 0.0333(18) 0.047(2) 0.0079(15) 0.0058(13) 0.0000(13) C23 0.043(2) 0.054(2) 0.0300(18) 0.0076(16) 0.0115(15) 0.0103(18) C24 0.0436(19) 0.0370(19) 0.0253(16) 0.0024(14) 0.0053(14) -0.0006(15) C25 0.050(2) 0.045(2) 0.0245(17) 0.0047(15) 0.0107(15) -0.0024(17) C26 0.057(2) 0.043(2) 0.0194(15) 0.0058(14) 0.0026(15) -0.0041(17) C27 0.046(2) 0.043(2) 0.0213(16) 0.0066(14) -0.0017(14) -0.0053(16) C28 0.0420(19) 0.0401(19) 0.0230(16) 0.0022(14) -0.0019(14) -0.0079(16) C29 0.0450(19) 0.0332(17) 0.0208(15) 0.0044(13) 0.0041(13) -0.0037(15) C30 0.0382(19) 0.063(3) 0.0290(18) 0.0152(17) -0.0019(15) -0.0164(18) C31 0.0318(17) 0.0391(19) 0.0324(18) 0.0015(14) 0.0046(14) 0.0060(14) C32 0.056(2) 0.040(2) 0.0309(18) 0.0049(15) 0.0052(16) 0.0142(18) C33 0.0382(17) 0.0318(17) 0.0264(16) -0.0004(13) 0.0019(13) 0.0072(14) C34 0.053(2) 0.0322(18) 0.038(2) 0.0031(15) 0.0010(17) 0.0062(16) C35 0.066(3) 0.043(2) 0.042(2) 0.0011(18) -0.003(2) 0.024(2) C36 0.048(2) 0.059(3) 0.058(3) -0.004(2) -0.004(2) 0.023(2) C37 0.043(2) 0.068(3) 0.097(4) 0.001(3) -0.003(3) 0.005(2) C38 0.046(2) 0.039(2) 0.082(4) 0.001(2) -0.003(2) 0.0049(19) C39 0.0384(17) 0.0246(15) 0.0309(17) -0.0014(13) 0.0068(14) -0.0003(13) C40 0.054(2) 0.0273(17) 0.0320(18) -0.0018(13) 0.0098(16) -0.0027(16) C41 0.060(3) 0.0305(19) 0.050(2) 0.0011(17) 0.015(2) -0.0070(18) C42 0.055(3) 0.043(2) 0.066(3) -0.002(2) 0.004(2) -0.016(2) C43 0.064(3) 0.053(3) 0.046(2) 0.001(2) -0.009(2) -0.014(2) C44 0.054(2) 0.0346(19) 0.039(2) 0.0055(16) 0.0007(17) -0.0063(17) C45 0.0452(19) 0.0280(16) 0.0224(15) -0.0005(12) 0.0077(13) -0.0015(14) C46 0.051(2) 0.043(2) 0.0330(19) -0.0052(16) 0.0089(16) -0.0068(18) C47 0.071(3) 0.060(3) 0.044(2) -0.009(2) 0.023(2) -0.022(2) C48 0.115(4) 0.041(2) 0.034(2) 0.0051(18) 0.024(2) -0.015(3) C49 0.098(4) 0.042(2) 0.032(2) 0.0115(17) 0.013(2) 0.007(2) C50 0.060(2) 0.039(2) 0.0270(17) 0.0047(15) 0.0066(16) 0.0068(18) C51 0.0403(18) 0.0357(18) 0.0277(17) -0.0046(14) 0.0042(14) 0.0030(15) C52 0.055(2) 0.037(2) 0.038(2) -0.0024(16) -0.0035(17) -0.0004(18) C53 0.060(3) 0.048(2) 0.037(2) -0.0075(18) -0.0061(18) -0.008(2) C54 0.083(3) 0.061(3) 0.028(2) -0.0023(19) -0.005(2) 0.000(3) C55 0.124(5) 0.046(2) 0.029(2) 0.0030(18) -0.001(2) -0.017(3) C56 0.094(4) 0.044(2) 0.030(2) -0.0038(17) 0.002(2) -0.019(2) C57 0.043(2) 0.042(2) 0.040(2) -0.0017(16) 0.0027(16) 0.0063(17) C58 0.046(2) 0.084(4) 0.051(3) -0.012(2) 0.013(2) 0.005(2) C59 0.051(3) 0.117(5) 0.086(4) -0.014(4) 0.027(3) 0.010(3) C60 0.043(3) 0.113(5) 0.108(5) -0.007(4) 0.011(3) 0.017(3) C61 0.058(3) 0.082(4) 0.076(4) -0.008(3) -0.017(3) 0.014(3) C62 0.055(3) 0.066(3) 0.049(3) -0.008(2) -0.005(2) 0.017(2) C63 0.049(2) 0.043(2) 0.038(2) 0.0000(16) 0.0061(17) 0.0104(18) C64 0.058(3) 0.050(3) 0.090(4) 0.016(3) 0.022(3) 0.012(2) C65 0.056(3) 0.056(3) 0.097(4) 0.010(3) 0.011(3) 0.019(2) C66 0.042(2) 0.061(3) 0.090(4) -0.001(3) 0.007(2) 0.004(2) C67 0.060(4) 0.072(4) 0.277(12) 0.064(6) 0.039(5) 0.005(3) C68 0.066(4) 0.054(3) 0.222(10) 0.056(5) 0.036(5) 0.019(3) C69 0.049(2) 0.044(2) 0.052(2) 0.0077(18) 0.0150(19) 0.0164(18) C70 0.053(3) 0.050(3) 0.070(3) 0.007(2) 0.000(2) 0.011(2) C71 0.064(3) 0.060(3) 0.091(4) -0.003(3) -0.005(3) 0.013(3) C72 0.072(3) 0.047(3) 0.104(5) -0.007(3) 0.004(3) 0.008(3) C73 0.080(4) 0.041(3) 0.091(4) 0.014(3) 0.027(3) 0.017(2) C74 0.061(3) 0.049(3) 0.058(3) 0.008(2) 0.014(2) 0.016(2) C75 0.118(5) 0.067(3) 0.033(2) 0.018(2) 0.022(3) 0.038(3) C76 0.180(7) 0.058(3) 0.061(4) 0.017(3) 0.057(4) 0.018(4) C77 0.338(17) 0.081(5) 0.103(7) 0.050(5) 0.121(9) 0.074(8) C78 0.38(2) 0.176(11) 0.089(6) 0.080(7) 0.125(10) 0.196(13) C79 0.248(13) 0.244(13) 0.064(5) 0.053(6) 0.056(6) 0.194(11) C80 0.131(6) 0.171(8) 0.043(3) 0.027(4) 0.015(3) 0.099(6) C81 0.061(3) 0.119(5) 0.035(2) 0.009(3) 0.002(2) -0.033(3) C82 0.055(3) 0.084(4) 0.035(2) 0.005(2) 0.0029(19) 0.004(2) C83 0.067(4) 0.169(7) 0.050(3) 0.029(4) 0.000(3) 0.002(4) C84 0.091(6) 0.48(2) 0.072(5) 0.099(10) -0.031(4) -0.094(10) C85 0.130(8) 0.62(3) 0.119(8) 0.160(13) -0.070(6) -0.230(14) C86 0.142(8) 0.416(19) 0.061(4) 0.079(8) -0.040(5) -0.191(11) C87 0.190(7) 0.059(3) 0.035(3) 0.011(2) -0.032(3) -0.069(4) C88 0.221(10) 0.194(9) 0.044(3) 0.041(4) -0.032(4) -0.174(8) C89 0.45(2) 0.304(18) 0.090(7) 0.099(9) -0.122(10) -0.34(2) C90 0.65(4) 0.126(9) 0.090(7) 0.066(6) -0.167(13) -0.233(15) C91 0.63(3) 0.049(4) 0.087(7) 0.019(4) -0.123(12) -0.073(10) C92 0.353(15) 0.039(3) 0.053(4) 0.006(3) -0.054(6) -0.025(6) C93 0.053(2) 0.054(2) 0.032(2) 0.0035(17) 0.0044(17) 0.014(2) C94 0.091(4) 0.096(4) 0.041(3) -0.007(3) 0.004(3) 0.046(3) C95 0.116(6) 0.186(9) 0.045(3) 0.008(4) 0.016(4) 0.103(6) C96 0.071(4) 0.248(11) 0.060(4) 0.044(5) 0.021(3) 0.080(6) C97 0.048(3) 0.160(7) 0.084(5) 0.034(5) 0.009(3) 0.005(4) C98 0.053(3) 0.079(3) 0.051(3) 0.008(2) 0.011(2) 0.002(2) C99 0.061(2) 0.0308(18) 0.0287(18) -0.0046(14) 0.0022(16) -0.0002(17) C100 0.058(3) 0.037(2) 0.058(3) -0.0033(19) 0.011(2) -0.0102(19) C101 0.077(3) 0.059(3) 0.078(4) -0.008(3) 0.009(3) -0.028(3) C102 0.101(5) 0.047(3) 0.079(4) -0.003(3) 0.007(3) -0.026(3) C103 0.112(5) 0.031(2) 0.072(4) 0.004(2) 0.007(3) 0.000(3) C104 0.078(3) 0.032(2) 0.054(3) 0.0024(18) 0.007(2) 0.007(2) C105 0.049(3) 0.077(4) 0.091(4) 0.047(3) 0.020(3) 0.019(2) C106 0.079(3) 0.064(3) 0.061(3) 0.021(3) 0.018(3) 0.021(3) C107 0.090(5) 0.074(4) 0.120(6) -0.008(4) 0.004(4) -0.003(4) C108 0.043(3) 0.127(6) 0.194(8) 0.126(6) 0.037(4) 0.021(3) C109 0.099(5) 0.116(6) 0.261(12) 0.126(8) 0.106(7) 0.048(5) C111 0.068(3) 0.040(2) 0.037(2) 0.0107(17) 0.0002(19) -0.006(2) C112 0.059(3) 0.044(2) 0.040(2) 0.0148(18) -0.0014(18) -0.0063(19) C113 0.103(4) 0.049(3) 0.065(3) 0.022(2) -0.015(3) -0.012(3) C114 0.049(3) 0.101(5) 0.174(8) 0.096(5) 0.006(4) 0.003(3) C115 0.047(3) 0.056(3) 0.128(6) 0.003(3) 0.005(3) 0.004(2) C116 0.105(5) 0.088(5) 0.143(7) 0.028(5) 0.045(5) -0.017(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C45 1.893(3) . ? Ni1 O6 1.919(2) . ? Ni1 P1 2.1730(9) . ? Ni1 P2 2.2255(9) . ? Ni2 C75 1.890(5) . ? Ni2 O5 1.910(3) . ? Ni2 P3 2.1645(12) . ? Ni2 P4 2.1995(12) . ? P1 C1 1.754(3) . ? P1 C39 1.824(4) . ? P1 C33 1.833(3) . ? P2 C57 1.815(4) . ? P2 C99 1.825(4) . ? P2 C51 1.834(4) . ? P3 C32 1.754(4) . ? P3 C69 1.816(5) . ? P3 C63 1.822(4) . ? P4 C87 1.799(4) . ? P4 C93 1.821(5) . ? P4 C81 1.824(5) . ? O1 C6 1.386(4) . ? O1 C105 1.462(6) . ? O2 C22 1.384(4) . ? O2 C108 1.416(6) . ? O3 C29 1.389(4) . ? O3 C111 1.439(5) . ? O4 C114 1.370(8) . ? O4 C15 1.376(4) . ? O6 C2 1.308(4) . ? O5 C31 1.304(4) . ? C1 C2 1.371(5) . ? C1 H1 0.9500 . ? C2 C3 1.490(4) . ? C3 C8 1.398(5) . ? C3 C4 1.399(5) . ? C4 C5 1.387(5) . ? C4 H4 0.9500 . ? C5 C6 1.394(5) . ? C5 C30 1.522(5) . ? C6 C7 1.396(6) . ? C7 C8 1.400(5) . ? C7 C9 1.509(5) . ? C8 H8 0.9500 . ? C9 C10 1.524(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C15 1.391(5) . ? C10 C11 1.395(5) . ? C11 C12 1.372(6) . ? C11 H11 0.9500 . ? C12 C13 1.373(6) . ? C12 H12 0.9500 . ? C13 C14 1.389(5) . ? C13 H13 0.9500 . ? C14 C15 1.399(5) . ? C14 C16 1.516(5) . ? C16 C17 1.521(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C22 1.389(5) . ? C17 C18 1.392(5) . ? C18 C19 1.393(5) . ? C18 H18 0.9500 . ? C19 C20 1.395(5) . ? C19 C31 1.496(5) . ? C20 C21 1.388(5) . ? C20 H20 0.9500 . ? C21 C22 1.401(5) . ? C21 C23 1.512(5) . ? C23 C24 1.511(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C29 1.392(5) . ? C24 C25 1.401(5) . ? C25 C26 1.368(6) . ? C25 H25 0.9500 . ? C26 C27 1.391(5) . ? C26 H26 0.9500 . ? C27 C28 1.401(5) . ? C27 H27 0.9500 . ? C28 C29 1.391(5) . ? C28 C30 1.511(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.367(5) . ? C32 H32 0.9500 . ? C33 C34 1.385(5) . ? C33 C38 1.392(6) . ? C34 C35 1.403(6) . ? C34 H34 0.9500 . ? C35 C36 1.371(7) . ? C35 H35 0.9500 . ? C36 C37 1.373(7) . ? C36 H36 0.9500 . ? C37 C38 1.392(6) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C44 1.392(5) . ? C39 C40 1.398(5) . ? C40 C41 1.394(6) . ? C40 H40 0.9500 . ? C41 C42 1.377(7) . ? C41 H41 0.9500 . ? C42 C43 1.373(7) . ? C42 H42 0.9500 . ? C43 C44 1.382(6) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.395(5) . ? C45 C50 1.398(5) . ? C46 C47 1.400(6) . ? C46 H46 0.9500 . ? C47 C48 1.389(8) . ? C47 H47 0.9500 . ? C48 C49 1.366(8) . ? C48 H48 0.9500 . ? C49 C50 1.390(6) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C56 1.382(6) . ? C51 C52 1.389(5) . ? C52 C53 1.387(6) . ? C52 H52 0.9500 . ? C53 C54 1.371(7) . ? C53 H53 0.9500 . ? C54 C55 1.368(7) . ? C54 H54 0.9500 . ? C55 C56 1.394(6) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C58 1.387(6) . ? C57 C62 1.388(6) . ? C58 C59 1.378(7) . ? C58 H58 0.9500 . ? C59 C60 1.355(9) . ? C59 H59 0.9500 . ? C60 C61 1.373(9) . ? C60 H60 0.9500 . ? C61 C62 1.374(7) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 C68 1.334(7) . ? C63 C64 1.396(6) . ? C64 C65 1.393(7) . ? C64 H64 0.9500 . ? C65 C66 1.365(8) . ? C65 H65 0.9500 . ? C66 C67 1.332(8) . ? C66 H66 0.9500 . ? C67 C68 1.380(9) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C70 1.394(7) . ? C69 C74 1.409(6) . ? C70 C71 1.363(8) . ? C70 H70 0.9500 . ? C71 C72 1.380(9) . ? C71 H71 0.9500 . ? C72 C73 1.378(9) . ? C72 H72 0.9500 . ? C73 C74 1.387(7) . ? C73 H73 0.9500 . ? C74 H74 0.9500 . ? C75 C80 1.378(9) . ? C75 C76 1.402(9) . ? C76 C77 1.377(10) . ? C76 H76 0.9500 . ? C77 C78 1.36(2) . ? C77 H77 0.9500 . ? C78 C79 1.39(2) . ? C78 H78 0.9500 . ? C79 C80 1.436(11) . ? C79 H79 0.9500 . ? C80 H80 0.9500 . ? C81 C86 1.363(8) . ? C81 C82 1.400(7) . ? C82 C83 1.373(7) . ? C82 H82 0.9500 . ? C83 C84 1.362(11) . ? C83 H83 0.9500 . ? C84 C85 1.358(15) . ? C84 H84 0.9500 . ? C85 C86 1.408(12) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? C87 C88 1.389(3) . ? C87 C92 1.389(3) . ? C88 C89 1.389(3) . ? C88 H88 0.9500 . ? C89 C90 1.389(3) . ? C89 H89 0.9500 . ? C90 C91 1.389(3) . ? C90 H90 0.9500 . ? C91 C92 1.389(3) . ? C91 H91 0.9500 . ? C92 H92 0.9500 . ? C93 C98 1.379(7) . ? C93 C94 1.387(6) . ? C94 C95 1.386(10) . ? C94 H94 0.9500 . ? C95 C96 1.364(14) . ? C95 H95 0.9500 . ? C96 C97 1.358(12) . ? C96 H96 0.9500 . ? C97 C98 1.398(8) . ? C97 H97 0.9500 . ? C98 H98 0.9500 . ? C99 C104 1.387(6) . ? C99 C100 1.394(6) . ? C100 C101 1.383(7) . ? C100 H100 0.9500 . ? C101 C102 1.379(9) . ? C101 H101 0.9500 . ? C102 C103 1.353(9) . ? C102 H102 0.9500 . ? C103 C104 1.413(7) . ? C103 H103 0.9500 . ? C104 H104 0.9500 . ? C105 C106 1.536(7) . ? C105 H10A 0.9900 . ? C105 H10B 0.9900 . ? C106 C107 1.453(9) . ? C106 H10C 0.9900 . ? C106 H10D 0.9900 . ? C107 H10E 0.9800 . ? C107 H10F 0.9800 . ? C107 H10G 0.9800 . ? C108 C109 1.541(10) . ? C108 H10H 0.9900 . ? C108 H10I 0.9900 . ? C109 C110 1.256(17) . ? C109 H10J 0.9900 . ? C109 H10K 0.9900 . ? C110 H11A 0.9800 . ? C110 H11B 0.9800 . ? C110 H11C 0.9800 . ? C111 C112 1.515(6) . ? C111 H11D 0.9900 . ? C111 H11E 0.9900 . ? C112 C113 1.515(7) . ? C112 H11F 0.9900 . ? C112 H11G 0.9900 . ? C113 H11H 0.9800 . ? C113 H11I 0.9800 . ? C113 H11J 0.9800 . ? C114 C115 1.647(10) . ? C114 H11K 0.9900 . ? C114 H11L 0.9900 . ? C115 C116 1.365(10) . ? C115 H11M 0.9900 . ? C115 H11N 0.9900 . ? C116 H11O 0.9800 . ? C116 H11P 0.9800 . ? C116 H11Q 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C45 Ni1 O6 172.51(13) . . ? C45 Ni1 P1 88.47(10) . . ? O6 Ni1 P1 86.48(7) . . ? C45 Ni1 P2 94.14(10) . . ? O6 Ni1 P2 91.10(7) . . ? P1 Ni1 P2 176.78(4) . . ? C75 Ni2 O5 176.8(2) . . ? C75 Ni2 P3 91.18(16) . . ? O5 Ni2 P3 86.60(8) . . ? C75 Ni2 P4 90.79(16) . . ? O5 Ni2 P4 91.63(8) . . ? P3 Ni2 P4 174.39(5) . . ? C1 P1 C39 109.21(16) . . ? C1 P1 C33 106.38(16) . . ? C39 P1 C33 105.18(16) . . ? C1 P1 Ni1 99.20(11) . . ? C39 P1 Ni1 121.89(12) . . ? C33 P1 Ni1 113.92(11) . . ? C57 P2 C99 104.06(19) . . ? C57 P2 C51 104.27(17) . . ? C99 P2 C51 101.37(17) . . ? C57 P2 Ni1 110.61(13) . . ? C99 P2 Ni1 111.99(13) . . ? C51 P2 Ni1 122.69(12) . . ? C32 P3 C69 108.3(2) . . ? C32 P3 C63 107.1(2) . . ? C69 P3 C63 106.23(19) . . ? C32 P3 Ni2 99.19(14) . . ? C69 P3 Ni2 120.20(14) . . ? C63 P3 Ni2 114.81(14) . . ? C87 P4 C93 107.2(2) . . ? C87 P4 C81 105.8(2) . . ? C93 P4 C81 102.9(2) . . ? C87 P4 Ni2 108.82(15) . . ? C93 P4 Ni2 115.03(15) . . ? C81 P4 Ni2 116.4(2) . . ? C6 O1 C105 113.2(3) . . ? C22 O2 C108 115.9(3) . . ? C29 O3 C111 113.0(3) . . ? C114 O4 C15 114.7(5) . . ? C2 O6 Ni1 118.6(2) . . ? C31 O5 Ni2 118.7(2) . . ? C2 C1 P1 113.4(2) . . ? C2 C1 H1 123.3 . . ? P1 C1 H1 123.3 . . ? O6 C2 C1 122.2(3) . . ? O6 C2 C3 116.2(3) . . ? C1 C2 C3 121.6(3) . . ? C8 C3 C4 118.0(3) . . ? C8 C3 C2 120.6(3) . . ? C4 C3 C2 121.3(3) . . ? C5 C4 C3 122.4(3) . . ? C5 C4 H4 118.8 . . ? C3 C4 H4 118.8 . . ? C4 C5 C6 118.4(3) . . ? C4 C5 C30 118.1(3) . . ? C6 C5 C30 123.6(3) . . ? O1 C6 C5 120.1(3) . . ? O1 C6 C7 118.8(3) . . ? C5 C6 C7 121.1(3) . . ? C6 C7 C8 119.3(3) . . ? C6 C7 C9 121.1(3) . . ? C8 C7 C9 119.6(4) . . ? C3 C8 C7 120.9(3) . . ? C3 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C7 C9 C10 119.8(3) . . ? C7 C9 H9A 107.4 . . ? C10 C9 H9A 107.4 . . ? C7 C9 H9B 107.4 . . ? C10 C9 H9B 107.4 . . ? H9A C9 H9B 106.9 . . ? C15 C10 C11 117.3(3) . . ? C15 C10 C9 124.5(3) . . ? C11 C10 C9 118.2(3) . . ? C12 C11 C10 121.1(4) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C13 120.5(4) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C14 121.0(4) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C13 C14 C15 117.4(3) . . ? C13 C14 C16 118.9(3) . . ? C15 C14 C16 123.7(3) . . ? O4 C15 C10 118.7(3) . . ? O4 C15 C14 118.5(3) . . ? C10 C15 C14 122.6(3) . . ? C14 C16 C17 120.2(3) . . ? C14 C16 H16A 107.3 . . ? C17 C16 H16A 107.3 . . ? C14 C16 H16B 107.3 . . ? C17 C16 H16B 107.3 . . ? H16A C16 H16B 106.9 . . ? C22 C17 C18 118.7(3) . . ? C22 C17 C16 122.2(4) . . ? C18 C17 C16 119.1(4) . . ? C17 C18 C19 121.7(3) . . ? C17 C18 H18 119.1 . . ? C19 C18 H18 119.1 . . ? C18 C19 C20 118.0(3) . . ? C18 C19 C31 120.5(3) . . ? C20 C19 C31 121.5(3) . . ? C21 C20 C19 122.1(3) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C20 C21 C22 118.2(3) . . ? C20 C21 C23 119.2(3) . . ? C22 C21 C23 122.6(3) . . ? O2 C22 C17 119.1(3) . . ? O2 C22 C21 119.5(3) . . ? C17 C22 C21 121.3(3) . . ? C24 C23 C21 117.7(3) . . ? C24 C23 H23A 107.9 . . ? C21 C23 H23A 107.9 . . ? C24 C23 H23B 107.9 . . ? C21 C23 H23B 107.9 . . ? H23A C23 H23B 107.2 . . ? C29 C24 C25 117.7(3) . . ? C29 C24 C23 122.4(3) . . ? C25 C24 C23 119.9(3) . . ? C26 C25 C24 121.6(3) . . ? C26 C25 H25 119.2 . . ? C24 C25 H25 119.2 . . ? C25 C26 C27 119.9(3) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C28 120.3(3) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C27 118.5(3) . . ? C29 C28 C30 121.6(3) . . ? C27 C28 C30 119.8(3) . . ? O3 C29 C28 119.0(3) . . ? O3 C29 C24 119.1(3) . . ? C28 C29 C24 121.8(3) . . ? C28 C30 C5 117.1(3) . . ? C28 C30 H30A 108.0 . . ? C5 C30 H30A 108.0 . . ? C28 C30 H30B 108.0 . . ? C5 C30 H30B 108.0 . . ? H30A C30 H30B 107.3 . . ? O5 C31 C32 122.2(3) . . ? O5 C31 C19 116.1(3) . . ? C32 C31 C19 121.7(3) . . ? C31 C32 P3 113.3(3) . . ? C31 C32 H32 123.4 . . ? P3 C32 H32 123.4 . . ? C34 C33 C38 118.5(3) . . ? C34 C33 P1 125.9(3) . . ? C38 C33 P1 115.6(3) . . ? C33 C34 C35 120.1(4) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 120.5(4) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C37 119.8(4) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C36 C37 C38 120.2(5) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C33 C38 C37 120.8(4) . . ? C33 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C44 C39 C40 118.5(3) . . ? C44 C39 P1 119.1(3) . . ? C40 C39 P1 122.4(3) . . ? C41 C40 C39 120.0(4) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C42 C41 C40 120.3(4) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C43 C42 C41 120.0(4) . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C42 C43 C44 120.3(4) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C43 C44 C39 120.8(4) . . ? C43 C44 H44 119.6 . . ? C39 C44 H44 119.6 . . ? C46 C45 C50 117.2(3) . . ? C46 C45 Ni1 120.0(3) . . ? C50 C45 Ni1 122.7(3) . . ? C45 C46 C47 121.4(4) . . ? C45 C46 H46 119.3 . . ? C47 C46 H46 119.3 . . ? C48 C47 C46 119.2(4) . . ? C48 C47 H47 120.4 . . ? C46 C47 H47 120.4 . . ? C49 C48 C47 120.6(4) . . ? C49 C48 H48 119.7 . . ? C47 C48 H48 119.7 . . ? C48 C49 C50 119.7(4) . . ? C48 C49 H49 120.1 . . ? C50 C49 H49 120.1 . . ? C49 C50 C45 121.8(4) . . ? C49 C50 H50 119.1 . . ? C45 C50 H50 119.1 . . ? C56 C51 C52 118.0(4) . . ? C56 C51 P2 120.1(3) . . ? C52 C51 P2 121.8(3) . . ? C53 C52 C51 121.0(4) . . ? C53 C52 H52 119.5 . . ? C51 C52 H52 119.5 . . ? C54 C53 C52 120.3(4) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C55 C54 C53 119.5(4) . . ? C55 C54 H54 120.3 . . ? C53 C54 H54 120.3 . . ? C54 C55 C56 120.7(4) . . ? C54 C55 H55 119.7 . . ? C56 C55 H55 119.7 . . ? C51 C56 C55 120.5(4) . . ? C51 C56 H56 119.8 . . ? C55 C56 H56 119.8 . . ? C58 C57 C62 118.8(4) . . ? C58 C57 P2 123.6(3) . . ? C62 C57 P2 117.6(3) . . ? C59 C58 C57 119.6(5) . . ? C59 C58 H58 120.2 . . ? C57 C58 H58 120.2 . . ? C60 C59 C58 121.3(5) . . ? C60 C59 H59 119.4 . . ? C58 C59 H59 119.4 . . ? C59 C60 C61 119.8(5) . . ? C59 C60 H60 120.1 . . ? C61 C60 H60 120.1 . . ? C60 C61 C62 120.1(5) . . ? C60 C61 H61 120.0 . . ? C62 C61 H61 120.0 . . ? C61 C62 C57 120.5(5) . . ? C61 C62 H62 119.8 . . ? C57 C62 H62 119.8 . . ? C68 C63 C64 116.8(4) . . ? C68 C63 P3 118.1(4) . . ? C64 C63 P3 124.9(4) . . ? C65 C64 C63 120.2(5) . . ? C65 C64 H64 119.9 . . ? C63 C64 H64 119.9 . . ? C66 C65 C64 121.2(5) . . ? C66 C65 H65 119.4 . . ? C64 C65 H65 119.4 . . ? C67 C66 C65 117.1(5) . . ? C67 C66 H66 121.5 . . ? C65 C66 H66 121.5 . . ? C66 C67 C68 122.6(6) . . ? C66 C67 H67 118.7 . . ? C68 C67 H67 118.7 . . ? C63 C68 C67 121.8(5) . . ? C63 C68 H68 119.1 . . ? C67 C68 H68 119.1 . . ? C70 C69 C74 117.3(4) . . ? C70 C69 P3 120.2(3) . . ? C74 C69 P3 122.4(4) . . ? C71 C70 C69 121.7(5) . . ? C71 C70 H70 119.2 . . ? C69 C70 H70 119.2 . . ? C70 C71 C72 120.7(5) . . ? C70 C71 H71 119.7 . . ? C72 C71 H71 119.7 . . ? C73 C72 C71 119.4(5) . . ? C73 C72 H72 120.3 . . ? C71 C72 H72 120.3 . . ? C72 C73 C74 120.3(5) . . ? C72 C73 H73 119.8 . . ? C74 C73 H73 119.8 . . ? C73 C74 C69 120.6(5) . . ? C73 C74 H74 119.7 . . ? C69 C74 H74 119.7 . . ? C80 C75 C76 118.6(6) . . ? C80 C75 Ni2 121.1(5) . . ? C76 C75 Ni2 120.2(5) . . ? C77 C76 C75 121.5(10) . . ? C77 C76 H76 119.3 . . ? C75 C76 H76 119.3 . . ? C78 C77 C76 119.6(11) . . ? C78 C77 H77 120.2 . . ? C76 C77 H77 120.2 . . ? C77 C78 C79 122.1(8) . . ? C77 C78 H78 119.0 . . ? C79 C78 H78 119.0 . . ? C78 C79 C80 117.8(10) . . ? C78 C79 H79 121.1 . . ? C80 C79 H79 121.1 . . ? C75 C80 C79 120.4(10) . . ? C75 C80 H80 119.8 . . ? C79 C80 H80 119.8 . . ? C86 C81 C82 118.9(6) . . ? C86 C81 P4 121.9(5) . . ? C82 C81 P4 118.9(4) . . ? C83 C82 C81 121.5(5) . . ? C83 C82 H82 119.3 . . ? C81 C82 H82 119.3 . . ? C84 C83 C82 119.3(7) . . ? C84 C83 H83 120.3 . . ? C82 C83 H83 120.3 . . ? C85 C84 C83 120.0(7) . . ? C85 C84 H84 120.0 . . ? C83 C84 H84 120.0 . . ? C84 C85 C86 121.5(7) . . ? C84 C85 H85 119.3 . . ? C86 C85 H85 119.3 . . ? C81 C86 C85 118.6(8) . . ? C81 C86 H86 120.7 . . ? C85 C86 H86 120.7 . . ? C88 C87 C92 120.0 . . ? C88 C87 P4 116.9(3) . . ? C92 C87 P4 122.9(3) . . ? C87 C88 C89 120.0 . . ? C87 C88 H88 120.0 . . ? C89 C88 H88 120.0 . . ? C90 C89 C88 120.0 . . ? C90 C89 H89 120.0 . . ? C88 C89 H89 120.0 . . ? C89 C90 C91 120.0 . . ? C89 C90 H90 120.0 . . ? C91 C90 H90 120.0 . . ? C92 C91 C90 120.0 . . ? C92 C91 H91 120.0 . . ? C90 C91 H91 120.0 . . ? C91 C92 C87 120.0 . . ? C91 C92 H92 120.0 . . ? C87 C92 H92 120.0 . . ? C98 C93 C94 118.6(5) . . ? C98 C93 P4 118.1(3) . . ? C94 C93 P4 123.3(4) . . ? C95 C94 C93 119.4(7) . . ? C95 C94 H94 120.3 . . ? C93 C94 H94 120.3 . . ? C96 C95 C94 121.5(6) . . ? C96 C95 H95 119.3 . . ? C94 C95 H95 119.3 . . ? C97 C96 C95 119.9(6) . . ? C97 C96 H96 120.1 . . ? C95 C96 H96 120.1 . . ? C96 C97 C98 119.6(8) . . ? C96 C97 H97 120.2 . . ? C98 C97 H97 120.2 . . ? C93 C98 C97 121.0(6) . . ? C93 C98 H98 119.5 . . ? C97 C98 H98 119.5 . . ? C104 C99 C100 118.4(4) . . ? C104 C99 P2 124.2(4) . . ? C100 C99 P2 117.4(3) . . ? C101 C100 C99 121.2(5) . . ? C101 C100 H100 119.4 . . ? C99 C100 H100 119.4 . . ? C102 C101 C100 119.9(5) . . ? C102 C101 H101 120.1 . . ? C100 C101 H101 120.1 . . ? C103 C102 C101 120.1(5) . . ? C103 C102 H102 119.9 . . ? C101 C102 H102 119.9 . . ? C102 C103 C104 120.9(5) . . ? C102 C103 H103 119.6 . . ? C104 C103 H103 119.6 . . ? C99 C104 C103 119.5(5) . . ? C99 C104 H104 120.2 . . ? C103 C104 H104 120.2 . . ? O1 C105 C106 109.1(4) . . ? O1 C105 H10A 109.9 . . ? C106 C105 H10A 109.9 . . ? O1 C105 H10B 109.9 . . ? C106 C105 H10B 109.9 . . ? H10A C105 H10B 108.3 . . ? C107 C106 C105 110.7(6) . . ? C107 C106 H10C 109.5 . . ? C105 C106 H10C 109.5 . . ? C107 C106 H10D 109.5 . . ? C105 C106 H10D 109.5 . . ? H10C C106 H10D 108.1 . . ? C106 C107 H10E 109.5 . . ? C106 C107 H10F 109.5 . . ? H10E C107 H10F 109.5 . . ? C106 C107 H10G 109.5 . . ? H10E C107 H10G 109.5 . . ? H10F C107 H10G 109.5 . . ? O2 C108 C109 108.6(4) . . ? O2 C108 H10H 110.0 . . ? C109 C108 H10H 110.0 . . ? O2 C108 H10I 110.0 . . ? C109 C108 H10I 110.0 . . ? H10H C108 H10I 108.4 . . ? C110 C109 C108 110.6(13) . . ? C110 C109 H10J 109.5 . . ? C108 C109 H10J 109.5 . . ? C110 C109 H10K 109.5 . . ? C108 C109 H10K 109.5 . . ? H10J C109 H10K 108.1 . . ? C109 C110 H11A 109.5 . . ? C109 C110 H11B 109.5 . . ? H11A C110 H11B 109.5 . . ? C109 C110 H11C 109.5 . . ? H11A C110 H11C 109.5 . . ? H11B C110 H11C 109.5 . . ? O3 C111 C112 108.3(3) . . ? O3 C111 H11D 110.0 . . ? C112 C111 H11D 110.0 . . ? O3 C111 H11E 110.0 . . ? C112 C111 H11E 110.0 . . ? H11D C111 H11E 108.4 . . ? C113 C112 C111 110.9(4) . . ? C113 C112 H11F 109.5 . . ? C111 C112 H11F 109.5 . . ? C113 C112 H11G 109.5 . . ? C111 C112 H11G 109.5 . . ? H11F C112 H11G 108.0 . . ? C112 C113 H11H 109.5 . . ? C112 C113 H11I 109.5 . . ? H11H C113 H11I 109.5 . . ? C112 C113 H11J 109.5 . . ? H11H C113 H11J 109.5 . . ? H11I C113 H11J 109.5 . . ? O4 C114 C115 103.0(7) . . ? O4 C114 H11K 111.2 . . ? C115 C114 H11K 111.2 . . ? O4 C114 H11L 111.2 . . ? C115 C114 H11L 111.2 . . ? H11K C114 H11L 109.1 . . ? C116 C115 C114 107.5(7) . . ? C116 C115 H11M 110.2 . . ? C114 C115 H11M 110.2 . . ? C116 C115 H11N 110.2 . . ? C114 C115 H11N 110.2 . . ? H11M C115 H11N 108.5 . . ? C115 C116 H11O 109.5 . . ? C115 C116 H11P 109.5 . . ? H11O C116 H11P 109.5 . . ? C115 C116 H11Q 109.5 . . ? H11O C116 H11Q 109.5 . . ? H11P C116 H11Q 109.5 . . ? 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 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C45 Ni1 P1 C1 -171.18(16) . . . . ? O6 Ni1 P1 C1 3.28(14) . . . . ? P2 Ni1 P1 C1 44.6(7) . . . . ? C45 Ni1 P1 C39 -51.62(17) . . . . ? O6 Ni1 P1 C39 122.84(15) . . . . ? P2 Ni1 P1 C39 164.2(7) . . . . ? C45 Ni1 P1 C33 76.21(17) . . . . ? O6 Ni1 P1 C33 -109.33(15) . . . . ? P2 Ni1 P1 C33 -68.0(7) . . . . ? C45 Ni1 P2 C57 77.98(18) . . . . ? O6 Ni1 P2 C57 -96.66(16) . . . . ? P1 Ni1 P2 C57 -137.9(7) . . . . ? C45 Ni1 P2 C99 -166.43(18) . . . . ? O6 Ni1 P2 C99 18.92(16) . . . . ? P1 Ni1 P2 C99 -22.3(7) . . . . ? C45 Ni1 P2 C51 -45.67(18) . . . . ? O6 Ni1 P2 C51 139.69(16) . . . . ? P1 Ni1 P2 C51 98.4(7) . . . . ? C75 Ni2 P3 C32 -176.9(3) . . . . ? O5 Ni2 P3 C32 0.81(18) . . . . ? P4 Ni2 P3 C32 72.5(5) . . . . ? C75 Ni2 P3 C69 -59.3(3) . . . . ? O5 Ni2 P3 C69 118.39(18) . . . . ? P4 Ni2 P3 C69 -169.9(5) . . . . ? C75 Ni2 P3 C63 69.4(3) . . . . ? O5 Ni2 P3 C63 -112.90(18) . . . . ? P4 Ni2 P3 C63 -41.2(5) . . . . ? C75 Ni2 P4 C87 -155.2(3) . . . . ? O5 Ni2 P4 C87 26.9(2) . . . . ? P3 Ni2 P4 C87 -44.6(5) . . . . ? C75 Ni2 P4 C93 84.6(3) . . . . ? O5 Ni2 P4 C93 -93.36(17) . . . . ? P3 Ni2 P4 C93 -164.8(5) . . . . ? C75 Ni2 P4 C81 -35.8(3) . . . . ? O5 Ni2 P4 C81 146.2(2) . . . . ? P3 Ni2 P4 C81 74.8(5) . . . . ? C45 Ni1 O6 C2 45.0(11) . . . . ? P1 Ni1 O6 C2 -2.8(2) . . . . ? P2 Ni1 O6 C2 179.4(2) . . . . ? C75 Ni2 O5 C31 44(4) . . . . ? P3 Ni2 O5 C31 -1.2(3) . . . . ? P4 Ni2 O5 C31 -175.9(3) . . . . ? C39 P1 C1 C2 -132.5(3) . . . . ? C33 P1 C1 C2 114.5(3) . . . . ? Ni1 P1 C1 C2 -3.9(3) . . . . ? Ni1 O6 C2 C1 0.7(4) . . . . ? Ni1 O6 C2 C3 179.1(2) . . . . ? P1 C1 C2 O6 2.6(4) . . . . ? P1 C1 C2 C3 -175.7(2) . . . . ? O6 C2 C3 C8 -11.6(4) . . . . ? C1 C2 C3 C8 166.8(3) . . . . ? O6 C2 C3 C4 170.9(3) . . . . ? C1 C2 C3 C4 -10.7(5) . . . . ? C8 C3 C4 C5 -0.8(5) . . . . ? C2 C3 C4 C5 176.8(3) . . . . ? C3 C4 C5 C6 0.1(5) . . . . ? C3 C4 C5 C30 179.5(3) . . . . ? C105 O1 C6 C5 -77.9(5) . . . . ? C105 O1 C6 C7 105.2(4) . . . . ? C4 C5 C6 O1 -176.7(3) . . . . ? C30 C5 C6 O1 3.9(5) . . . . ? C4 C5 C6 C7 0.1(5) . . . . ? C30 C5 C6 C7 -179.3(3) . . . . ? O1 C6 C7 C8 177.3(3) . . . . ? C5 C6 C7 C8 0.5(5) . . . . ? O1 C6 C7 C9 -5.5(5) . . . . ? C5 C6 C7 C9 177.6(3) . . . . ? C4 C3 C8 C7 1.3(5) . . . . ? C2 C3 C8 C7 -176.3(3) . . . . ? C6 C7 C8 C3 -1.2(5) . . . . ? C9 C7 C8 C3 -178.4(3) . . . . ? C6 C7 C9 C10 61.6(6) . . . . ? C8 C7 C9 C10 -121.2(4) . . . . ? C7 C9 C10 C15 30.2(7) . . . . ? C7 C9 C10 C11 -150.8(4) . . . . ? C15 C10 C11 C12 -1.6(7) . . . . ? C9 C10 C11 C12 179.4(5) . . . . ? C10 C11 C12 C13 1.3(8) . . . . ? C11 C12 C13 C14 0.3(8) . . . . ? C12 C13 C14 C15 -1.5(7) . . . . ? C12 C13 C14 C16 176.8(5) . . . . ? C114 O4 C15 C10 90.7(5) . . . . ? C114 O4 C15 C14 -94.6(5) . . . . ? C11 C10 C15 O4 174.8(4) . . . . ? C9 C10 C15 O4 -6.2(6) . . . . ? C11 C10 C15 C14 0.3(6) . . . . ? C9 C10 C15 C14 179.3(4) . . . . ? C13 C14 C15 O4 -173.3(4) . . . . ? C16 C14 C15 O4 8.6(6) . . . . ? C13 C14 C15 C10 1.2(6) . . . . ? C16 C14 C15 C10 -177.0(4) . . . . ? C13 C14 C16 C17 148.4(4) . . . . ? C15 C14 C16 C17 -33.5(7) . . . . ? C14 C16 C17 C22 -59.0(6) . . . . ? C14 C16 C17 C18 122.6(4) . . . . ? C22 C17 C18 C19 0.7(5) . . . . ? C16 C17 C18 C19 179.1(3) . . . . ? C17 C18 C19 C20 -0.4(5) . . . . ? C17 C18 C19 C31 177.6(3) . . . . ? C18 C19 C20 C21 -0.1(5) . . . . ? C31 C19 C20 C21 -178.2(3) . . . . ? C19 C20 C21 C22 0.4(5) . . . . ? C19 C20 C21 C23 -177.8(3) . . . . ? C108 O2 C22 C17 -93.4(6) . . . . ? C108 O2 C22 C21 90.0(6) . . . . ? C18 C17 C22 O2 -176.9(3) . . . . ? C16 C17 C22 O2 4.7(5) . . . . ? C18 C17 C22 C21 -0.4(5) . . . . ? C16 C17 C22 C21 -178.8(3) . . . . ? C20 C21 C22 O2 176.3(3) . . . . ? C23 C21 C22 O2 -5.5(5) . . . . ? C20 C21 C22 C17 -0.2(5) . . . . ? C23 C21 C22 C17 178.0(3) . . . . ? C20 C21 C23 C24 -127.8(4) . . . . ? C22 C21 C23 C24 54.0(5) . . . . ? C21 C23 C24 C29 50.6(5) . . . . ? C21 C23 C24 C25 -130.7(4) . . . . ? C29 C24 C25 C26 -2.1(6) . . . . ? C23 C24 C25 C26 179.2(4) . . . . ? C24 C25 C26 C27 -1.3(6) . . . . ? C25 C26 C27 C28 1.9(6) . . . . ? C26 C27 C28 C29 0.8(6) . . . . ? C26 C27 C28 C30 177.3(4) . . . . ? C111 O3 C29 C28 -93.7(4) . . . . ? C111 O3 C29 C24 88.3(4) . . . . ? C27 C28 C29 O3 177.7(3) . . . . ? C30 C28 C29 O3 1.3(5) . . . . ? C27 C28 C29 C24 -4.4(6) . . . . ? C30 C28 C29 C24 179.3(4) . . . . ? C25 C24 C29 O3 -177.1(3) . . . . ? C23 C24 C29 O3 1.6(5) . . . . ? C25 C24 C29 C28 4.9(5) . . . . ? C23 C24 C29 C28 -176.4(4) . . . . ? C29 C28 C30 C5 -54.1(5) . . . . ? C27 C28 C30 C5 129.5(4) . . . . ? C4 C5 C30 C28 128.3(4) . . . . ? C6 C5 C30 C28 -52.3(5) . . . . ? Ni2 O5 C31 C32 1.3(5) . . . . ? Ni2 O5 C31 C19 -178.8(2) . . . . ? C18 C19 C31 O5 -16.5(5) . . . . ? C20 C19 C31 O5 161.6(3) . . . . ? C18 C19 C31 C32 163.4(4) . . . . ? C20 C19 C31 C32 -18.6(5) . . . . ? O5 C31 C32 P3 -0.4(5) . . . . ? C19 C31 C32 P3 179.7(3) . . . . ? C69 P3 C32 C31 -126.6(3) . . . . ? C63 P3 C32 C31 119.2(3) . . . . ? Ni2 P3 C32 C31 -0.5(3) . . . . ? C1 P1 C33 C34 135.5(3) . . . . ? C39 P1 C33 C34 19.7(4) . . . . ? Ni1 P1 C33 C34 -116.3(3) . . . . ? C1 P1 C33 C38 -44.5(4) . . . . ? C39 P1 C33 C38 -160.3(3) . . . . ? Ni1 P1 C33 C38 63.7(3) . . . . ? C38 C33 C34 C35 -0.9(6) . . . . ? P1 C33 C34 C35 179.1(3) . . . . ? C33 C34 C35 C36 0.1(6) . . . . ? C34 C35 C36 C37 0.6(8) . . . . ? C35 C36 C37 C38 -0.6(9) . . . . ? C34 C33 C38 C37 0.9(7) . . . . ? P1 C33 C38 C37 -179.1(4) . . . . ? C36 C37 C38 C33 -0.1(9) . . . . ? C1 P1 C39 C44 2.6(4) . . . . ? C33 P1 C39 C44 116.5(3) . . . . ? Ni1 P1 C39 C44 -112.0(3) . . . . ? C1 P1 C39 C40 -176.7(3) . . . . ? C33 P1 C39 C40 -62.9(3) . . . . ? Ni1 P1 C39 C40 68.7(3) . . . . ? C44 C39 C40 C41 -0.9(6) . . . . ? P1 C39 C40 C41 178.5(3) . . . . ? C39 C40 C41 C42 0.4(6) . . . . ? C40 C41 C42 C43 0.3(7) . . . . ? C41 C42 C43 C44 -0.6(8) . . . . ? C42 C43 C44 C39 0.1(7) . . . . ? C40 C39 C44 C43 0.6(6) . . . . ? P1 C39 C44 C43 -178.8(4) . . . . ? O6 Ni1 C45 C46 54.1(11) . . . . ? P1 Ni1 C45 C46 101.7(3) . . . . ? P2 Ni1 C45 C46 -80.2(3) . . . . ? O6 Ni1 C45 C50 -121.7(9) . . . . ? P1 Ni1 C45 C50 -74.1(3) . . . . ? P2 Ni1 C45 C50 104.1(3) . . . . ? C50 C45 C46 C47 1.9(5) . . . . ? Ni1 C45 C46 C47 -174.1(3) . . . . ? C45 C46 C47 C48 -0.7(6) . . . . ? C46 C47 C48 C49 -1.3(7) . . . . ? C47 C48 C49 C50 2.0(7) . . . . ? C48 C49 C50 C45 -0.8(7) . . . . ? C46 C45 C50 C49 -1.2(6) . . . . ? Ni1 C45 C50 C49 174.7(3) . . . . ? C57 P2 C51 C56 -80.5(4) . . . . ? C99 P2 C51 C56 171.6(4) . . . . ? Ni1 P2 C51 C56 46.0(4) . . . . ? C57 P2 C51 C52 99.0(4) . . . . ? C99 P2 C51 C52 -8.8(4) . . . . ? Ni1 P2 C51 C52 -134.5(3) . . . . ? C56 C51 C52 C53 -1.9(6) . . . . ? P2 C51 C52 C53 178.6(3) . . . . ? C51 C52 C53 C54 0.0(7) . . . . ? C52 C53 C54 C55 1.7(8) . . . . ? C53 C54 C55 C56 -1.4(9) . . . . ? C52 C51 C56 C55 2.2(7) . . . . ? P2 C51 C56 C55 -178.3(4) . . . . ? C54 C55 C56 C51 -0.5(9) . . . . ? C99 P2 C57 C58 96.2(4) . . . . ? C51 P2 C57 C58 -9.7(5) . . . . ? Ni1 P2 C57 C58 -143.4(4) . . . . ? C99 P2 C57 C62 -82.0(4) . . . . ? C51 P2 C57 C62 172.2(4) . . . . ? Ni1 P2 C57 C62 38.5(4) . . . . ? C62 C57 C58 C59 0.9(8) . . . . ? P2 C57 C58 C59 -177.2(5) . . . . ? C57 C58 C59 C60 -1.5(10) . . . . ? C58 C59 C60 C61 1.8(12) . . . . ? C59 C60 C61 C62 -1.5(11) . . . . ? C60 C61 C62 C57 0.9(9) . . . . ? C58 C57 C62 C61 -0.7(8) . . . . ? P2 C57 C62 C61 177.6(4) . . . . ? C32 P3 C63 C68 -40.5(6) . . . . ? C69 P3 C63 C68 -156.1(6) . . . . ? Ni2 P3 C63 C68 68.5(6) . . . . ? C32 P3 C63 C64 144.8(4) . . . . ? C69 P3 C63 C64 29.2(5) . . . . ? Ni2 P3 C63 C64 -106.2(4) . . . . ? C68 C63 C64 C65 4.1(9) . . . . ? P3 C63 C64 C65 178.9(4) . . . . ? C63 C64 C65 C66 0.2(10) . . . . ? C64 C65 C66 C67 -4.5(11) . . . . ? C65 C66 C67 C68 4.6(15) . . . . ? C64 C63 C68 C67 -4.1(13) . . . . ? P3 C63 C68 C67 -179.3(8) . . . . ? C66 C67 C68 C63 -0.3(17) . . . . ? C32 P3 C69 C70 1.7(4) . . . . ? C63 P3 C69 C70 116.4(4) . . . . ? Ni2 P3 C69 C70 -111.1(4) . . . . ? C32 P3 C69 C74 178.7(4) . . . . ? C63 P3 C69 C74 -66.6(4) . . . . ? Ni2 P3 C69 C74 65.9(4) . . . . ? C74 C69 C70 C71 1.6(7) . . . . ? P3 C69 C70 C71 178.7(4) . . . . ? C69 C70 C71 C72 -2.2(9) . . . . ? C70 C71 C72 C73 1.8(9) . . . . ? C71 C72 C73 C74 -0.9(9) . . . . ? C72 C73 C74 C69 0.3(8) . . . . ? C70 C69 C74 C73 -0.6(7) . . . . ? P3 C69 C74 C73 -177.7(4) . . . . ? O5 Ni2 C75 C80 -127(3) . . . . ? P3 Ni2 C75 C80 -81.9(5) . . . . ? P4 Ni2 C75 C80 92.9(5) . . . . ? O5 Ni2 C75 C76 52(4) . . . . ? P3 Ni2 C75 C76 97.8(5) . . . . ? P4 Ni2 C75 C76 -87.5(5) . . . . ? C80 C75 C76 C77 -0.6(10) . . . . ? Ni2 C75 C76 C77 179.8(6) . . . . ? C75 C76 C77 C78 1.1(13) . . . . ? C76 C77 C78 C79 -1.6(17) . . . . ? C77 C78 C79 C80 1.5(17) . . . . ? C76 C75 C80 C79 0.5(11) . . . . ? Ni2 C75 C80 C79 -179.9(6) . . . . ? C78 C79 C80 C75 -0.9(14) . . . . ? C87 P4 C81 C86 32.2(10) . . . . ? C93 P4 C81 C86 144.5(10) . . . . ? Ni2 P4 C81 C86 -88.8(10) . . . . ? C87 P4 C81 C82 -155.0(5) . . . . ? C93 P4 C81 C82 -42.8(6) . . . . ? Ni2 P4 C81 C82 84.0(5) . . . . ? C86 C81 C82 C83 -0.9(12) . . . . ? P4 C81 C82 C83 -173.8(6) . . . . ? C81 C82 C83 C84 2.2(14) . . . . ? C82 C83 C84 C85 0(2) . . . . ? C83 C84 C85 C86 -3(3) . . . . ? C82 C81 C86 C85 -2(2) . . . . ? P4 C81 C86 C85 170.4(13) . . . . ? C84 C85 C86 C81 4(3) . . . . ? C93 P4 C87 C88 170.2(2) . . . . ? C81 P4 C87 C88 -80.5(3) . . . . ? Ni2 P4 C87 C88 45.3(2) . . . . ? C93 P4 C87 C92 -5.0(3) . . . . ? C81 P4 C87 C92 104.3(3) . . . . ? Ni2 P4 C87 C92 -129.9(2) . . . . ? C92 C87 C88 C89 0.0 . . . . ? P4 C87 C88 C89 -175.3(3) . . . . ? C87 C88 C89 C90 0.0 . . . . ? C88 C89 C90 C91 0.0 . . . . ? C89 C90 C91 C92 0.0 . . . . ? C90 C91 C92 C87 0.0 . . . . ? C88 C87 C92 C91 0.0 . . . . ? P4 C87 C92 C91 175.0(3) . . . . ? C87 P4 C93 C98 -114.9(4) . . . . ? C81 P4 C93 C98 133.8(4) . . . . ? Ni2 P4 C93 C98 6.2(4) . . . . ? C87 P4 C93 C94 65.1(4) . . . . ? C81 P4 C93 C94 -46.2(5) . . . . ? Ni2 P4 C93 C94 -173.8(4) . . . . ? C98 C93 C94 C95 0.5(8) . . . . ? P4 C93 C94 C95 -179.6(5) . . . . ? C93 C94 C95 C96 -0.9(10) . . . . ? C94 C95 C96 C97 0.1(12) . . . . ? C95 C96 C97 C98 1.2(12) . . . . ? C94 C93 C98 C97 0.8(8) . . . . ? P4 C93 C98 C97 -179.2(5) . . . . ? C96 C97 C98 C93 -1.6(10) . . . . ? C57 P2 C99 C104 -0.7(4) . . . . ? C51 P2 C99 C104 107.3(4) . . . . ? Ni1 P2 C99 C104 -120.3(3) . . . . ? C57 P2 C99 C100 -179.0(3) . . . . ? C51 P2 C99 C100 -70.9(3) . . . . ? Ni1 P2 C99 C100 61.5(3) . . . . ? C104 C99 C100 C101 -1.8(7) . . . . ? P2 C99 C100 C101 176.6(4) . . . . ? C99 C100 C101 C102 2.1(8) . . . . ? C100 C101 C102 C103 -1.5(9) . . . . ? C101 C102 C103 C104 0.7(9) . . . . ? C100 C99 C104 C103 0.9(7) . . . . ? P2 C99 C104 C103 -177.3(4) . . . . ? C102 C103 C104 C99 -0.4(8) . . . . ? C6 O1 C105 C106 178.6(4) . . . . ? O1 C105 C106 C107 75.6(6) . . . . ? C22 O2 C108 C109 -176.7(7) . . . . ? O2 C108 C109 C110 -66.4(13) . . . . ? C29 O3 C111 C112 178.9(3) . . . . ? O3 C111 C112 C113 -178.0(4) . . . . ? C15 O4 C114 C115 177.6(3) . . . . ? O4 C114 C115 C116 -170.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.051 _refine_diff_density_min -1.094 _refine_diff_density_rms 0.129 # Attachment 'trans-NiPOP.cif' data_Ni-pop_173k _database_code_depnum_ccdc_archive 'CCDC 294728' _audit_creation_date 05-10-26 _audit_creation_method CRYSTALS_ver_12.24 _oxford_structure_analysis_title 'Ni POP' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 17.548(7) _cell_length_b 19.597(6) _cell_length_c 18.816(8) _cell_angle_alpha 90 _cell_angle_beta 104.88(3) _cell_angle_gamma 90 _cell_volume 6254(4) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421 1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C74 H74 Ni O6 P2' _chemical_formula_moiety 'C74 H74 Ni O6 P2' _chemical_compound_source ? _chemical_formula_weight 1180.06 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 173 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.15 _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 0.415 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 0.97 # Sheldrick geometric definitions 0.95 0.97 _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'IPDS (Stoe & Cie, 1996)' _computing_data_reduction 'XRED (Stoe & Cie 1996)' _computing_cell_refinement 'IPDS (Stoe & Cie, 1996)' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al 1996)' _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_ambient_temperature 173 _diffrn_reflns_number 48066 _reflns_number_total 13324 _diffrn_reflns_av_R_equivalents 0.069 # Number of reflections with Friedels Law is 13324 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 13563 _diffrn_reflns_theta_min 1.528 _diffrn_reflns_theta_max 26.935 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.396 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -22 _reflns_limit_h_max 21 _reflns_limit_k_min 0 _reflns_limit_k_max 24 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.05 _refine_diff_density_max 1.35 _refine_ls_number_reflns 7863 _refine_ls_number_restraints 46 _refine_ls_number_parameters 775 #_refine_ls_R_factor_ref 0.0678 _refine_ls_wR_factor_ref 0.0482 _refine_ls_goodness_of_fit_ref 1.1964 #_reflns_number_all 13269 _refine_ls_R_factor_all 0.1236 _refine_ls_wR_factor_all 0.0547 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>1.40u(I) _reflns_number_gt 7863 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_gt 0.0482 _refine_ls_shift/su_max 0.004492 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.63 -1.03 1.24 ; # Check this file using the IUCr facility at: # http://journals.iucr.org/services/cif/checking/checkfull.html # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_section_abstract # Text of the abstract ; ? ; _publ_section_comment # Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen ; H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Stoe & Cie (1996), IPDS Software Stoe & Cie (1996), XRED V1.08 Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ni1 Ni 0.40626(2) 0.13244(2) 0.81060(2) 0.0271 1.0000 Uani . . . . . . P1 P 0.46536(5) 0.22930(4) 0.83586(5) 0.0281 1.0000 Uani . . . . . . P2 P 0.35024(5) 0.03464(4) 0.77144(5) 0.0264 1.0000 Uani . . . . . . O1 O 0.50933(13) 0.09240(11) 0.82063(14) 0.0307 1.0000 Uani . . . . . . O2 O 0.87922(12) 0.04753(12) 0.85163(13) 0.0308 1.0000 Uani . . . . . . O3 O 0.67632(13) 0.12462(12) 0.62270(13) 0.0324 1.0000 Uani . . . . . . O4 O 0.68012(14) -0.12820(13) 0.57571(13) 0.0362 1.0000 Uani . U . . . . O5 O 0.64591(13) -0.11818(12) 0.83638(13) 0.0314 1.0000 Uani . . . . . . O6 O 0.42162(14) 0.06915(12) 0.64720(14) 0.0355 1.0000 Uani . . . . . . C1 C 0.44280(19) 0.29128(18) 0.76089(19) 0.0307 1.0000 Uani . . . . . . C2 C 0.4446(2) 0.2674(2) 0.6914(2) 0.0388 1.0000 Uani . . . . . . C3 C 0.4351(2) 0.3105(2) 0.6333(2) 0.0470 1.0000 Uani . . . . . . C4 C 0.4227(3) 0.3797(3) 0.6424(3) 0.0549 1.0000 Uani . . . . . . C5 C 0.4200(3) 0.4038(2) 0.7099(3) 0.0536 1.0000 Uani . . . . . . C6 C 0.4302(2) 0.35944(19) 0.7692(2) 0.0411 1.0000 Uani . . . . . . C7 C 0.4606(2) 0.27687(17) 0.9179(2) 0.0319 1.0000 Uani . . . . . . C8 C 0.5285(2) 0.2853(2) 0.9753(2) 0.0441 1.0000 Uani . . . . . . C9 C 0.5247(3) 0.3188(2) 1.0385(2) 0.0561 1.0000 Uani . . . . . . C10 C 0.4540(3) 0.3432(2) 1.0466(3) 0.0554 1.0000 Uani . . . . . . C11 C 0.3868(3) 0.3343(2) 0.9912(3) 0.0521 1.0000 Uani . . . . . . C12 C 0.3895(2) 0.30213(19) 0.9260(2) 0.0421 1.0000 Uani . . . . . . C13 C 0.56249(19) 0.20259(18) 0.8428(2) 0.0320 1.0000 Uani . . . . . . C14 C 0.56809(17) 0.13494(17) 0.82984(17) 0.0250 1.0000 Uani . . . . . . C15 C 0.64600(18) 0.10596(17) 0.82704(18) 0.0261 1.0000 Uani . . . . . . C16 C 0.69292(18) 0.13978(16) 0.78918(18) 0.0260 1.0000 Uani . . . . . . C17 C 0.76905(17) 0.11837(16) 0.79281(17) 0.0241 1.0000 Uani . . . . . . C18 C 0.79976(17) 0.06391(17) 0.83913(17) 0.0249 1.0000 Uani . . . . . . C19 C 0.75207(18) 0.02462(17) 0.87251(17) 0.0259 1.0000 Uani . . . . . . C20 C 0.67444(18) 0.04596(17) 0.86443(18) 0.0258 1.0000 Uani . . . . . . C21 C 0.9257(2) 0.0852(2) 0.9127(2) 0.0419 1.0000 Uani . . . . . . C22 C 1.0102(2) 0.0613(2) 0.9284(2) 0.0491 1.0000 Uani . . . . . . C23 C 1.0490(3) 0.0763(3) 0.8691(3) 0.0663 1.0000 Uani . . . . . . C24 C 0.81409(19) 0.14747(16) 0.74055(19) 0.0289 1.0000 Uani . . . . . . C25 C 0.81098(19) 0.09493(17) 0.67974(19) 0.0277 1.0000 Uani . . . . . . C26 C 0.87587(19) 0.05343(19) 0.68137(19) 0.0321 1.0000 Uani . . . . . . C27 C 0.8697(2) 0.00045(19) 0.6316(2) 0.0359 1.0000 Uani . . . . . . C28 C 0.7992(2) -0.01222(18) 0.58187(19) 0.0324 1.0000 Uani . . . . . . C29 C 0.7328(2) 0.02775(18) 0.57836(18) 0.0293 1.0000 Uani . . . . . . C30 C 0.74131(19) 0.08336(17) 0.62601(18) 0.0267 1.0000 Uani . . . . . . C31 C 0.6682(3) 0.1798(2) 0.5732(2) 0.0488 1.0000 Uani . . . . . . C32 C 0.5888(3) 0.2124(3) 0.5647(3) 0.0665 1.0000 Uani . . . . . . C33 C 0.5724(3) 0.2669(3) 0.5091(3) 0.0771 1.0000 Uani . . . . . . C34 C 0.6520(2) 0.00837(19) 0.52957(19) 0.0332 1.0000 Uani . . . . . . C35 C 0.60532(19) -0.02673(18) 0.57617(18) 0.0280 1.0000 Uani . . . . . . C36 C 0.54701(19) 0.00784(16) 0.60040(17) 0.0250 1.0000 Uani . . . . . . C37 C 0.51097(19) -0.02233(17) 0.65069(17) 0.0254 1.0000 Uani . . . . . . C38 C 0.53789(19) -0.08599(17) 0.67996(18) 0.0287 1.0000 Uani . . . . . . C39 C 0.59553(19) -0.12116(16) 0.65724(18) 0.0271 1.0000 Uani . . . . . . C40 C 0.62539(19) -0.09216(18) 0.60211(18) 0.0290 1.0000 Uani . . . . . . C41 C 0.6421(5) -0.1612(4) 0.5073(5) 0.0422 0.5000 Uani D U . . . . C42 C 0.7088(5) -0.2027(5) 0.4909(5) 0.0513 0.5000 Uani D U . . . . C43 C 0.7464(6) -0.1648(5) 0.4419(6) 0.0574 0.5000 Uani D U . . . . C410 C 0.6501(6) -0.1844(5) 0.5246(5) 0.0440 0.5000 Uani D U . . . . C420 C 0.7178(6) -0.2285(5) 0.5110(5) 0.0528 0.5000 Uani D U . . . . C430 C 0.7573(6) -0.1920(5) 0.4621(6) 0.0578 0.5000 Uani D U . . . . C44 C 0.6329(2) -0.18425(17) 0.6988(2) 0.0342 1.0000 Uani . . . . . . C45 C 0.7112(2) -0.16395(17) 0.7494(2) 0.0313 1.0000 Uani . . . . . . C46 C 0.7814(2) -0.17488(18) 0.7296(2) 0.0377 1.0000 Uani . . . . . . C47 C 0.8522(2) -0.14872(19) 0.7720(2) 0.0387 1.0000 Uani . . . . . . C48 C 0.8531(2) -0.10763(19) 0.8315(2) 0.0375 1.0000 Uani . . . . . . C49 C 0.78398(19) -0.09495(16) 0.85294(19) 0.0285 1.0000 Uani . . . . . . C50 C 0.71476(19) -0.12638(17) 0.81381(19) 0.0302 1.0000 Uani . . . . . . C51 C 0.7821(2) -0.04113(19) 0.91053(19) 0.0326 1.0000 Uani . . . . . . C52 C 0.6416(2) -0.1668(2) 0.8934(2) 0.0422 1.0000 Uani . . . . . . C53 C 0.5682(2) -0.1538(2) 0.9181(2) 0.0470 1.0000 Uani . . . . . . C54 C 0.4936(3) -0.1728(3) 0.8601(3) 0.0589 1.0000 Uani . . . . . . C55 C 0.4485(2) 0.01501(17) 0.67449(19) 0.0283 1.0000 Uani . . . . . . C56 C 0.4164(2) -0.01811(17) 0.73407(19) 0.0291 1.0000 Uani . . . . . . C57 C 0.3419(2) -0.02045(19) 0.84672(19) 0.0324 1.0000 Uani . . . . . . C58 C 0.3929(2) -0.0103(2) 0.9158(2) 0.0435 1.0000 Uani . . . . . . C59 C 0.3929(2) -0.0546(3) 0.9734(2) 0.0508 1.0000 Uani . . . . . . C60 C 0.3409(3) -0.1080(3) 0.9636(2) 0.0534 1.0000 Uani . . . . . . C61 C 0.2890(2) -0.1189(2) 0.8951(2) 0.0472 1.0000 Uani . . . . . . C62 C 0.2895(2) -0.0755(2) 0.8372(2) 0.0376 1.0000 Uani . . . . . . C63 C 0.2526(2) 0.02926(17) 0.70688(19) 0.0297 1.0000 Uani . . . . . . C64 C 0.2404(2) -0.0003(2) 0.6378(2) 0.0398 1.0000 Uani . . . . . . C65 C 0.1645(3) -0.0050(2) 0.5917(2) 0.0456 1.0000 Uani . . . . . . C66 C 0.1010(2) 0.0198(2) 0.6134(2) 0.0475 1.0000 Uani . . . . . . C67 C 0.1123(2) 0.0499(2) 0.6811(2) 0.0453 1.0000 Uani . . . . . . C68 C 0.1883(2) 0.0548(2) 0.7275(2) 0.0371 1.0000 Uani . . . . . . C69 C 0.3092(2) 0.17358(18) 0.8126(2) 0.0340 1.0000 Uani . . . . . . C70 C 0.2645(2) 0.2137(2) 0.7569(3) 0.0489 1.0000 Uani . . . . . . C71 C 0.1956(3) 0.2451(3) 0.7636(3) 0.0642 1.0000 Uani . . . . . . C72 C 0.1701(3) 0.2362(3) 0.8266(4) 0.0732 1.0000 Uani . . . . . . C73 C 0.2134(3) 0.1953(3) 0.8818(3) 0.0604 1.0000 Uani . . . . . . C74 C 0.2822(2) 0.1649(2) 0.8756(2) 0.0419 1.0000 Uani . . . . . . H21 H 0.4528 0.2197 0.6847 0.0469 1.0000 Uiso . . . . . . H31 H 0.4369 0.2933 0.5860 0.0565 1.0000 Uiso . . . . . . H41 H 0.4160 0.4104 0.6014 0.0667 1.0000 Uiso . . . . . . H51 H 0.4111 0.4514 0.7164 0.0661 1.0000 Uiso . . . . . . H61 H 0.4284 0.3767 0.8165 0.0513 1.0000 Uiso . . . . . . H81 H 0.5780 0.2677 0.9705 0.0533 1.0000 Uiso . . . . . . H91 H 0.5718 0.3253 1.0773 0.0664 1.0000 Uiso . . . . . . H101 H 0.4518 0.3663 1.0911 0.0697 1.0000 Uiso . . . . . . H111 H 0.3373 0.3505 0.9974 0.0681 1.0000 Uiso . . . . . . H121 H 0.3424 0.2974 0.8868 0.0532 1.0000 Uiso . . . . . . H131 H 0.6070 0.2328 0.8545 0.0390 1.0000 Uiso . . . . . . H161 H 0.6722 0.1789 0.7598 0.0306 1.0000 Uiso . . . . . . H201 H 0.6399 0.0188 0.8850 0.0317 1.0000 Uiso . . . . . . H211 H 0.9061 0.0777 0.9552 0.0477 1.0000 Uiso . . . . . . H212 H 0.9230 0.1329 0.9009 0.0477 1.0000 Uiso . . . . . . H221 H 1.0397 0.0833 0.9726 0.0573 1.0000 Uiso . . . . . . H222 H 1.0111 0.0129 0.9358 0.0573 1.0000 Uiso . . . . . . H231 H 1.1022 0.0597 0.8829 0.0792 1.0000 Uiso . . . . . . H232 H 1.0493 0.1247 0.8612 0.0792 1.0000 Uiso . . . . . . H233 H 1.0207 0.0542 0.8245 0.0792 1.0000 Uiso . . . . . . H241 H 0.8678 0.1559 0.7667 0.0349 1.0000 Uiso . . . . . . H242 H 0.7901 0.1893 0.7195 0.0349 1.0000 Uiso . . . . . . H261 H 0.9249 0.0617 0.7171 0.0390 1.0000 Uiso . . . . . . H271 H 0.9148 -0.0274 0.6320 0.0455 1.0000 Uiso . . . . . . H281 H 0.7954 -0.0498 0.5484 0.0406 1.0000 Uiso . . . . . . H311 H 0.7088 0.2128 0.5921 0.0591 1.0000 Uiso . . . . . . H312 H 0.6726 0.1637 0.5262 0.0591 1.0000 Uiso . . . . . . H321 H 0.5868 0.2315 0.6113 0.0819 1.0000 Uiso . . . . . . H322 H 0.5490 0.1779 0.5505 0.0819 1.0000 Uiso . . . . . . H331 H 0.5212 0.2858 0.5059 0.0955 1.0000 Uiso . . . . . . H332 H 0.6115 0.3020 0.5229 0.0955 1.0000 Uiso . . . . . . H333 H 0.5737 0.2484 0.4621 0.0955 1.0000 Uiso . . . . . . H341 H 0.6583 -0.0219 0.4914 0.0409 1.0000 Uiso . . . . . . H342 H 0.6247 0.0487 0.5078 0.0409 1.0000 Uiso . . . . . . H361 H 0.5316 0.0528 0.5823 0.0295 1.0000 Uiso . . . . . . H381 H 0.5157 -0.1058 0.7168 0.0352 1.0000 Uiso . . . . . . H411 H 0.6000 -0.1902 0.5130 0.0515 0.5000 Uiso . . . . . . H412 H 0.6220 -0.1284 0.4692 0.0515 0.5000 Uiso . . . . . . H414 H 0.6165 -0.2126 0.5452 0.0525 0.5000 Uiso . . . . . . H415 H 0.6204 -0.1659 0.4786 0.0525 0.5000 Uiso . . . . . . H421 H 0.7472 -0.2124 0.5362 0.0615 0.5000 Uiso . . . . . . H422 H 0.6879 -0.2447 0.4676 0.0615 0.5000 Uiso . . . . . . H424 H 0.7552 -0.2377 0.5571 0.0618 0.5000 Uiso . . . . . . H425 H 0.6968 -0.2707 0.4883 0.0618 0.5000 Uiso . . . . . . H431 H 0.7882 -0.1917 0.4321 0.0681 0.5000 Uiso . . . . . . H432 H 0.7674 -0.1228 0.4651 0.0681 0.5000 Uiso . . . . . . H433 H 0.7081 -0.1551 0.3965 0.0681 0.5000 Uiso . . . . . . H434 H 0.7994 -0.2196 0.4538 0.0678 0.5000 Uiso . . . . . . H435 H 0.7785 -0.1498 0.4848 0.0678 0.5000 Uiso . . . . . . H436 H 0.7201 -0.1828 0.4160 0.0678 0.5000 Uiso . . . . . . H441 H 0.5992 -0.2023 0.7271 0.0421 1.0000 Uiso . . . . . . H442 H 0.6409 -0.2182 0.6645 0.0421 1.0000 Uiso . . . . . . H461 H 0.7809 -0.2008 0.6861 0.0465 1.0000 Uiso . . . . . . H471 H 0.9006 -0.1594 0.7597 0.0485 1.0000 Uiso . . . . . . H481 H 0.9017 -0.0874 0.8586 0.0440 1.0000 Uiso . . . . . . H511 H 0.8342 -0.0345 0.9416 0.0388 1.0000 Uiso . . . . . . H512 H 0.7478 -0.0558 0.9399 0.0388 1.0000 Uiso . . . . . . H521 H 0.6869 -0.1616 0.9345 0.0513 1.0000 Uiso . . . . . . H522 H 0.6403 -0.2122 0.8743 0.0513 1.0000 Uiso . . . . . . H531 H 0.5707 -0.1802 0.9617 0.0589 1.0000 Uiso . . . . . . H532 H 0.5660 -0.1062 0.9293 0.0589 1.0000 Uiso . . . . . . H541 H 0.4485 -0.1635 0.8786 0.0721 1.0000 Uiso . . . . . . H542 H 0.4948 -0.2204 0.8487 0.0721 1.0000 Uiso . . . . . . H543 H 0.4902 -0.1464 0.8164 0.0721 1.0000 Uiso . . . . . . H561 H 0.4604 -0.0305 0.7740 0.0356 1.0000 Uiso . . . . . . H562 H 0.3881 -0.0584 0.7136 0.0356 1.0000 Uiso . . . . . . H581 H 0.4285 0.0278 0.9238 0.0524 1.0000 Uiso . . . . . . H591 H 0.4296 -0.0478 1.0205 0.0607 1.0000 Uiso . . . . . . H601 H 0.3404 -0.1378 1.0040 0.0658 1.0000 Uiso . . . . . . H611 H 0.2529 -0.1565 0.8880 0.0579 1.0000 Uiso . . . . . . H621 H 0.2535 -0.0833 0.7900 0.0451 1.0000 Uiso . . . . . . H641 H 0.2843 -0.0176 0.6217 0.0490 1.0000 Uiso . . . . . . H651 H 0.1565 -0.0259 0.5441 0.0539 1.0000 Uiso . . . . . . H661 H 0.0489 0.0161 0.5813 0.0548 1.0000 Uiso . . . . . . H671 H 0.0682 0.0677 0.6966 0.0539 1.0000 Uiso . . . . . . H681 H 0.1959 0.0763 0.7747 0.0440 1.0000 Uiso . . . . . . H701 H 0.2814 0.2201 0.7126 0.0590 1.0000 Uiso . . . . . . H711 H 0.1657 0.2730 0.7243 0.0773 1.0000 Uiso . . . . . . H721 H 0.1230 0.2581 0.8317 0.0919 1.0000 Uiso . . . . . . H731 H 0.1955 0.1879 0.9254 0.0773 1.0000 Uiso . . . . . . H741 H 0.3120 0.1373 0.9152 0.0523 1.0000 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0224(2) 0.0260(2) 0.0350(2) -0.0037(2) 0.01125(17) 0.00061(18) P1 0.0255(4) 0.0246(4) 0.0369(5) -0.0050(4) 0.0129(4) 0.0011(3) P2 0.0256(4) 0.0267(5) 0.0289(5) -0.0005(4) 0.0109(4) -0.0008(3) O1 0.0231(11) 0.0260(12) 0.0460(15) -0.0047(11) 0.0142(10) 0.0018(10) O2 0.0206(11) 0.0371(13) 0.0338(13) -0.0085(11) 0.0056(10) 0.0021(10) O3 0.0331(12) 0.0325(13) 0.0328(13) 0.0017(11) 0.0109(10) 0.0041(11) O4 0.0378(12) 0.0352(13) 0.0386(13) -0.0142(11) 0.0155(10) -0.0001(10) O5 0.0297(12) 0.0332(14) 0.0342(13) 0.0098(10) 0.0137(10) 0.0057(10) O6 0.0367(13) 0.0337(14) 0.0390(14) 0.0065(12) 0.0148(11) 0.0096(11) C1 0.0268(18) 0.0329(19) 0.035(2) -0.0022(15) 0.0116(15) 0.0017(14) C2 0.037(2) 0.040(2) 0.040(2) -0.0097(18) 0.0116(17) -0.0005(17) C3 0.040(2) 0.061(3) 0.040(2) -0.002(2) 0.0109(18) -0.006(2) C4 0.048(2) 0.065(3) 0.053(3) 0.019(2) 0.017(2) 0.002(2) C5 0.062(3) 0.038(2) 0.065(3) 0.012(2) 0.024(2) 0.011(2) C6 0.047(2) 0.031(2) 0.050(2) 0.0015(18) 0.0214(18) 0.0075(17) C7 0.0378(19) 0.0228(17) 0.039(2) -0.0010(15) 0.0166(16) 0.0021(15) C8 0.044(2) 0.045(2) 0.045(2) -0.0112(19) 0.0131(19) 0.0003(18) C9 0.069(3) 0.054(3) 0.043(2) -0.014(2) 0.010(2) 0.003(2) C10 0.081(3) 0.041(2) 0.052(3) -0.017(2) 0.032(3) -0.003(2) C11 0.063(3) 0.040(2) 0.067(3) -0.015(2) 0.042(3) 0.000(2) C12 0.045(2) 0.030(2) 0.058(3) -0.0023(18) 0.025(2) -0.0004(17) C13 0.0248(17) 0.0310(19) 0.042(2) -0.0054(16) 0.0108(15) -0.0025(14) C14 0.0200(15) 0.0280(16) 0.0281(16) 0.0009(15) 0.0080(12) 0.0018(14) C15 0.0252(16) 0.0274(17) 0.0267(17) -0.0081(14) 0.0085(13) 0.0021(14) C16 0.0262(16) 0.0203(16) 0.0299(17) -0.0030(14) 0.0045(13) 0.0013(13) C17 0.0200(14) 0.0235(17) 0.0297(17) -0.0062(13) 0.0079(13) -0.0020(12) C18 0.0181(14) 0.0316(18) 0.0250(16) -0.0087(14) 0.0056(12) 0.0012(13) C19 0.0251(16) 0.0286(17) 0.0247(17) -0.0037(14) 0.0077(13) 0.0017(13) C20 0.0252(16) 0.0268(17) 0.0271(17) -0.0035(14) 0.0098(13) -0.0008(13) C21 0.0260(18) 0.053(2) 0.040(2) -0.0086(19) -0.0030(15) 0.0000(17) C22 0.030(2) 0.055(3) 0.058(3) -0.009(2) 0.0037(18) -0.0034(18) C23 0.039(2) 0.080(4) 0.079(4) 0.004(3) 0.014(2) -0.006(2) C24 0.0260(16) 0.0272(18) 0.0340(18) -0.0046(14) 0.0088(14) -0.0063(13) C25 0.0313(17) 0.0257(17) 0.0306(18) 0.0007(14) 0.0160(14) -0.0038(14) C26 0.0239(16) 0.040(2) 0.0335(19) 0.0005(16) 0.0093(14) -0.0025(15) C27 0.0342(19) 0.040(2) 0.039(2) -0.0046(17) 0.0200(17) 0.0034(16) C28 0.0357(19) 0.0315(19) 0.0341(19) -0.0075(15) 0.0164(16) -0.0031(15) C29 0.0327(18) 0.0335(18) 0.0252(17) 0.0041(15) 0.0141(14) -0.0026(15) C30 0.0310(17) 0.0290(17) 0.0236(17) 0.0052(14) 0.0131(13) -0.0010(14) C31 0.054(2) 0.045(2) 0.049(3) 0.013(2) 0.016(2) 0.009(2) C32 0.073(3) 0.057(3) 0.075(3) 0.027(3) 0.028(3) 0.024(3) C33 0.067(3) 0.078(4) 0.093(4) 0.037(3) 0.034(3) 0.024(3) C34 0.0372(19) 0.038(2) 0.0272(18) 0.0015(15) 0.0134(15) -0.0028(16) C35 0.0280(17) 0.0348(19) 0.0216(16) -0.0014(14) 0.0071(13) -0.0007(14) C36 0.0269(16) 0.0254(17) 0.0214(16) -0.0014(13) 0.0038(13) -0.0015(13) C37 0.0305(17) 0.0260(17) 0.0188(16) -0.0014(13) 0.0045(13) 0.0016(14) C38 0.0333(17) 0.0283(18) 0.0264(18) 0.0012(14) 0.0110(14) -0.0002(14) C39 0.0304(17) 0.0215(17) 0.0291(17) -0.0018(14) 0.0071(14) -0.0005(13) C40 0.0267(16) 0.0334(19) 0.0282(18) -0.0083(15) 0.0093(14) -0.0009(14) C41 0.0428(19) 0.042(2) 0.044(2) -0.0162(18) 0.0148(18) -0.0003(19) C42 0.051(2) 0.051(3) 0.052(3) -0.016(2) 0.013(2) 0.001(2) C43 0.058(3) 0.055(3) 0.057(3) -0.010(3) 0.011(3) 0.003(3) C410 0.0464(19) 0.040(2) 0.045(2) -0.0137(18) 0.0106(18) -0.0006(19) C420 0.056(2) 0.045(3) 0.053(3) -0.012(2) 0.007(2) 0.001(2) C430 0.061(3) 0.050(3) 0.059(3) -0.009(3) 0.008(3) 0.002(3) C44 0.0344(18) 0.0236(18) 0.047(2) 0.0003(16) 0.0151(17) 0.0051(15) C45 0.0331(18) 0.0238(17) 0.037(2) 0.0065(15) 0.0100(15) 0.0085(15) C46 0.041(2) 0.031(2) 0.045(2) 0.0073(17) 0.0169(18) 0.0108(16) C47 0.0342(19) 0.035(2) 0.052(2) 0.0052(17) 0.0206(17) 0.0116(15) C48 0.0322(18) 0.0332(19) 0.045(2) 0.0047(17) 0.0053(16) 0.0089(15) C49 0.0315(17) 0.0240(17) 0.0319(18) 0.0102(14) 0.0114(14) 0.0105(14) C50 0.0327(17) 0.0236(17) 0.0362(19) 0.0142(15) 0.0121(14) 0.0100(15) C51 0.0299(18) 0.038(2) 0.0294(18) 0.0046(16) 0.0063(15) 0.0065(15) C52 0.041(2) 0.041(2) 0.047(2) 0.0159(19) 0.0141(18) -0.0034(18) C53 0.049(2) 0.050(2) 0.048(2) 0.0115(19) 0.024(2) -0.0045(19) C54 0.055(3) 0.072(3) 0.053(3) 0.024(2) 0.020(2) 0.005(2) C55 0.0280(17) 0.0264(18) 0.0309(18) 0.0029(15) 0.0084(14) 0.0011(14) C56 0.0294(17) 0.0261(17) 0.0336(19) 0.0006(15) 0.0113(15) 0.0010(14) C57 0.0284(17) 0.039(2) 0.0314(19) -0.0010(16) 0.0115(15) 0.0009(15) C58 0.039(2) 0.057(3) 0.035(2) -0.0026(19) 0.0105(17) -0.0053(19) C59 0.041(2) 0.088(3) 0.0233(19) 0.007(2) 0.0071(17) -0.002(2) C60 0.055(3) 0.073(3) 0.036(2) 0.024(2) 0.0196(19) 0.005(2) C61 0.048(2) 0.047(3) 0.050(2) 0.008(2) 0.0183(19) -0.0053(19) C62 0.038(2) 0.044(2) 0.0306(19) 0.0066(17) 0.0087(16) -0.0100(17) C63 0.0334(18) 0.0264(17) 0.0300(18) 0.0039(15) 0.0096(15) -0.0040(14) C64 0.038(2) 0.044(2) 0.040(2) -0.0027(18) 0.0160(17) -0.0084(17) C65 0.053(2) 0.048(2) 0.034(2) -0.0042(18) 0.0073(19) -0.015(2) C66 0.041(2) 0.057(3) 0.040(2) 0.013(2) 0.0004(18) -0.014(2) C67 0.030(2) 0.051(2) 0.053(3) 0.007(2) 0.0085(18) -0.0012(17) C68 0.0315(19) 0.044(2) 0.034(2) -0.0006(17) 0.0061(15) -0.0013(16) C69 0.0289(18) 0.0297(19) 0.046(2) -0.0059(16) 0.0145(16) -0.0009(15) C70 0.035(2) 0.048(2) 0.065(3) 0.008(2) 0.014(2) 0.0024(18) C71 0.036(2) 0.058(3) 0.099(4) 0.018(3) 0.019(2) 0.015(2) C72 0.033(2) 0.073(3) 0.124(5) -0.007(3) 0.038(3) 0.009(2) C73 0.043(2) 0.067(3) 0.083(4) -0.011(3) 0.038(3) 0.000(2) C74 0.0313(19) 0.051(2) 0.048(2) -0.012(2) 0.0192(17) -0.0068(18) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2513(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ni1 . P1 . 2.1566(12) yes Ni1 . P2 . 2.1933(12) yes Ni1 . O1 . 1.936(2) yes Ni1 . C69 . 1.893(3) yes P1 . C1 . 1.826(4) yes P1 . C7 . 1.823(4) yes P1 . C13 . 1.756(3) yes P2 . C56 . 1.825(3) yes P2 . C57 . 1.817(4) yes P2 . C63 . 1.831(4) yes O1 . C14 . 1.302(4) yes O2 . C18 . 1.391(4) yes O2 . C21 . 1.431(4) yes O3 . C30 . 1.386(4) yes O3 . C31 . 1.410(5) yes O4 . C40 . 1.383(4) yes O4 . C41 . 1.442(10) yes O4 . C410 . 1.468(10) yes O5 . C50 . 1.389(4) yes O5 . C52 . 1.451(4) yes O6 . C55 . 1.219(4) yes C1 . C2 . 1.396(5) yes C1 . C6 . 1.369(5) yes C2 . C3 . 1.357(6) yes C2 . H21 . 0.959 no C3 . C4 . 1.391(6) yes C3 . H31 . 0.961 no C4 . C5 . 1.368(6) yes C4 . H41 . 0.961 no C5 . C6 . 1.389(6) yes C5 . H51 . 0.959 no C6 . H61 . 0.961 no C7 . C8 . 1.398(5) yes C7 . C12 . 1.386(5) yes C8 . C9 . 1.375(6) yes C8 . H81 . 0.959 no C9 . C10 . 1.374(7) yes C9 . H91 . 0.961 no C10 . C11 . 1.370(7) yes C10 . H101 . 0.961 no C11 . C12 . 1.390(6) yes C11 . H111 . 0.959 no C12 . H121 . 0.961 no C13 . C14 . 1.356(5) yes C13 . H131 . 0.959 no C14 . C15 . 1.494(4) yes C15 . C16 . 1.388(5) yes C15 . C20 . 1.395(5) yes C16 . C17 . 1.385(4) yes C16 . H161 . 0.960 no C17 . C18 . 1.396(5) yes C17 . C24 . 1.522(4) yes C18 . C19 . 1.399(5) yes C19 . C20 . 1.396(4) yes C19 . C51 . 1.502(5) yes C20 . H201 . 0.960 no C21 . C22 . 1.510(5) yes C21 . H211 . 0.961 no C21 . H212 . 0.959 no C22 . C23 . 1.477(7) yes C22 . H221 . 0.961 no C22 . H222 . 0.959 no C23 . H231 . 0.959 no C23 . H232 . 0.959 no C23 . H233 . 0.961 no C24 . C25 . 1.530(5) yes C24 . H241 . 0.960 no C24 . H242 . 0.960 no C25 . C26 . 1.393(5) yes C25 . C30 . 1.390(5) yes C26 . C27 . 1.383(5) yes C26 . H261 . 0.960 no C27 . C28 . 1.370(5) yes C27 . H271 . 0.959 no C28 . C29 . 1.392(5) yes C28 . H281 . 0.960 no C29 . C30 . 1.395(5) yes C29 . C34 . 1.525(5) yes C31 . C32 . 1.503(6) yes C31 . H311 . 0.960 no C31 . H312 . 0.961 no C32 . C33 . 1.471(7) yes C32 . H321 . 0.961 no C32 . H322 . 0.959 no C33 . H331 . 0.959 no C33 . H332 . 0.959 no C33 . H333 . 0.961 no C34 . C35 . 1.511(5) yes C34 . H341 . 0.960 no C34 . H342 . 0.960 no C35 . C36 . 1.398(5) yes C35 . C40 . 1.385(5) yes C36 . C37 . 1.397(5) yes C36 . H361 . 0.959 no C37 . C38 . 1.396(5) yes C37 . C55 . 1.480(5) yes C38 . C39 . 1.380(4) yes C38 . H381 . 0.960 no C39 . C40 . 1.397(5) yes C39 . C44 . 1.518(5) yes C41 . C42 . 1.519(8) yes C41 . H411 . 0.960 no C41 . H412 . 0.960 no C42 . C43 . 1.466(8) yes C42 . H421 . 0.961 no C42 . H422 . 0.960 no C43 . H431 . 0.959 no C43 . H432 . 0.960 no C43 . H433 . 0.961 no C410 . C420 . 1.542(8) yes C410 . H414 . 0.959 no C410 . H415 . 0.961 no C420 . C430 . 1.471(8) yes C420 . H424 . 0.961 no C420 . H425 . 0.960 no C430 . H434 . 0.959 no C430 . H435 . 0.960 no C430 . H436 . 0.961 no C44 . C45 . 1.510(5) yes C44 . H441 . 0.960 no C44 . H442 . 0.960 no C45 . C46 . 1.393(5) yes C45 . C50 . 1.406(5) yes C46 . C47 . 1.390(6) yes C46 . H461 . 0.961 no C47 . C48 . 1.376(5) yes C47 . H471 . 0.959 no C48 . C49 . 1.395(5) yes C48 . H481 . 0.960 no C49 . C50 . 1.392(5) yes C49 . C51 . 1.519(5) yes C51 . H511 . 0.960 no C51 . H512 . 0.960 no C52 . C53 . 1.498(5) yes C52 . H521 . 0.961 no C52 . H522 . 0.959 no C53 . C54 . 1.521(7) yes C53 . H531 . 0.961 no C53 . H532 . 0.959 no C54 . H541 . 0.959 no C54 . H542 . 0.959 no C54 . H543 . 0.961 no C55 . C56 . 1.523(5) yes C56 . H561 . 0.961 no C56 . H562 . 0.960 no C57 . C58 . 1.391(5) yes C57 . C62 . 1.399(5) yes C58 . C59 . 1.389(6) yes C58 . H581 . 0.959 no C59 . C60 . 1.369(6) yes C59 . H591 . 0.961 no C60 . C61 . 1.390(6) yes C60 . H601 . 0.961 no C61 . C62 . 1.384(5) yes C61 . H611 . 0.959 no C62 . H621 . 0.961 no C63 . C64 . 1.389(5) yes C63 . C68 . 1.378(5) yes C64 . C65 . 1.394(6) yes C64 . H641 . 0.959 no C65 . C66 . 1.369(6) yes C65 . H651 . 0.961 no C66 . C67 . 1.372(6) yes C66 . H661 . 0.960 no C67 . C68 . 1.396(5) yes C67 . H671 . 0.959 no C68 . H681 . 0.961 no C69 . C70 . 1.382(6) yes C69 . C74 . 1.395(5) yes C70 . C71 . 1.392(6) yes C70 . H701 . 0.961 no C71 . C72 . 1.381(8) yes C71 . H711 . 0.961 no C72 . C73 . 1.376(8) yes C72 . H721 . 0.959 no C73 . C74 . 1.379(6) yes C73 . H731 . 0.961 no C74 . H741 . 0.961 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P1 . Ni1 . P2 . 172.66(4) yes P1 . Ni1 . O1 . 87.19(8) yes P2 . Ni1 . O1 . 90.31(8) yes P1 . Ni1 . C69 . 90.28(12) yes P2 . Ni1 . C69 . 92.91(11) yes O1 . Ni1 . C69 . 173.40(14) yes Ni1 . P1 . C1 . 114.74(12) yes Ni1 . P1 . C7 . 120.83(12) yes C1 . P1 . C7 . 105.41(16) yes Ni1 . P1 . C13 . 99.01(13) yes C1 . P1 . C13 . 105.61(17) yes C7 . P1 . C13 . 110.18(17) yes Ni1 . P2 . C56 . 110.49(11) yes Ni1 . P2 . C57 . 112.11(13) yes C56 . P2 . C57 . 98.65(16) yes Ni1 . P2 . C63 . 122.38(12) yes C56 . P2 . C63 . 106.91(16) yes C57 . P2 . C63 . 103.53(16) yes Ni1 . O1 . C14 . 116.2(2) yes C18 . O2 . C21 . 110.9(2) yes C30 . O3 . C31 . 114.8(3) yes C40 . O4 . C41 . 110.2(4) yes C40 . O4 . C410 . 116.9(4) yes C50 . O5 . C52 . 111.4(3) yes P1 . C1 . C2 . 116.6(3) yes P1 . C1 . C6 . 124.8(3) yes C2 . C1 . C6 . 118.5(4) yes C1 . C2 . C3 . 121.2(4) yes C1 . C2 . H21 . 119.414 no C3 . C2 . H21 . 119.361 no C2 . C3 . C4 . 119.9(4) yes C2 . C3 . H31 . 120.123 no C4 . C3 . H31 . 119.969 no C3 . C4 . C5 . 119.6(4) yes C3 . C4 . H41 . 120.122 no C5 . C4 . H41 . 120.314 no C4 . C5 . C6 . 120.2(4) yes C4 . C5 . H51 . 119.947 no C6 . C5 . H51 . 119.895 no C5 . C6 . C1 . 120.7(4) yes C5 . C6 . H61 . 119.732 no C1 . C6 . H61 . 119.582 no P1 . C7 . C8 . 119.9(3) yes P1 . C7 . C12 . 121.0(3) yes C8 . C7 . C12 . 119.0(3) yes C7 . C8 . C9 . 120.2(4) yes C7 . C8 . H81 . 119.888 no C9 . C8 . H81 . 119.916 no C8 . C9 . C10 . 120.6(4) yes C8 . C9 . H91 . 119.792 no C10 . C9 . H91 . 119.626 no C9 . C10 . C11 . 119.8(4) yes C9 . C10 . H101 . 120.042 no C11 . C10 . H101 . 120.203 no C10 . C11 . C12 . 120.7(4) yes C10 . C11 . H111 . 119.629 no C12 . C11 . H111 . 119.650 no C11 . C12 . C7 . 119.7(4) yes C11 . C12 . H121 . 120.242 no C7 . C12 . H121 . 120.057 no P1 . C13 . C14 . 113.1(3) yes P1 . C13 . H131 . 123.461 no C14 . C13 . H131 . 123.461 no C13 . C14 . O1 . 123.9(3) yes C13 . C14 . C15 . 119.2(3) yes O1 . C14 . C15 . 116.9(3) yes C14 . C15 . C16 . 120.4(3) yes C14 . C15 . C20 . 121.0(3) yes C16 . C15 . C20 . 118.6(3) yes C15 . C16 . C17 . 121.5(3) yes C15 . C16 . H161 . 119.298 no C17 . C16 . H161 . 119.247 no C16 . C17 . C18 . 118.4(3) yes C16 . C17 . C24 . 120.6(3) yes C18 . C17 . C24 . 120.6(3) yes C17 . C18 . O2 . 119.5(3) yes C17 . C18 . C19 . 121.4(3) yes O2 . C18 . C19 . 119.1(3) yes C18 . C19 . C20 . 117.8(3) yes C18 . C19 . C51 . 120.6(3) yes C20 . C19 . C51 . 121.4(3) yes C19 . C20 . C15 . 121.3(3) yes C19 . C20 . H201 . 119.297 no C15 . C20 . H201 . 119.355 no O2 . C21 . C22 . 109.0(3) yes O2 . C21 . H211 . 109.715 no C22 . C21 . H211 . 109.498 no O2 . C21 . H212 . 109.491 no C22 . C21 . H212 . 109.597 no H211 . C21 . H212 . 109.487 no C21 . C22 . C23 . 114.2(4) yes C21 . C22 . H221 . 108.268 no C23 . C22 . H221 . 108.379 no C21 . C22 . H222 . 108.255 no C23 . C22 . H222 . 108.262 no H221 . C22 . H222 . 109.399 no C22 . C23 . H231 . 109.363 no C22 . C23 . H232 . 109.476 no H231 . C23 . H232 . 109.477 no C22 . C23 . H233 . 109.594 no H231 . C23 . H233 . 109.512 no H232 . C23 . H233 . 109.404 no C17 . C24 . C25 . 107.8(3) yes C17 . C24 . H241 . 109.768 no C25 . C24 . H241 . 109.978 no C17 . C24 . H242 . 109.949 no C25 . C24 . H242 . 109.770 no H241 . C24 . H242 . 109.517 no C24 . C25 . C26 . 120.3(3) yes C24 . C25 . C30 . 120.6(3) yes C26 . C25 . C30 . 118.8(3) yes C25 . C26 . C27 . 120.1(3) yes C25 . C26 . H261 . 119.875 no C27 . C26 . H261 . 119.981 no C26 . C27 . C28 . 119.9(3) yes C26 . C27 . H271 . 120.056 no C28 . C27 . H271 . 120.073 no C27 . C28 . C29 . 122.0(3) yes C27 . C28 . H281 . 119.081 no C29 . C28 . H281 . 118.952 no C28 . C29 . C30 . 117.3(3) yes C28 . C29 . C34 . 121.7(3) yes C30 . C29 . C34 . 120.8(3) yes C29 . C30 . C25 . 121.6(3) yes C29 . C30 . O3 . 118.4(3) yes C25 . C30 . O3 . 119.8(3) yes O3 . C31 . C32 . 109.3(4) yes O3 . C31 . H311 . 109.408 no C32 . C31 . H311 . 109.534 no O3 . C31 . H312 . 109.636 no C32 . C31 . H312 . 109.448 no H311 . C31 . H312 . 109.516 no C31 . C32 . C33 . 113.0(4) yes C31 . C32 . H321 . 108.505 no C33 . C32 . H321 . 108.706 no C31 . C32 . H322 . 108.594 no C33 . C32 . H322 . 108.495 no H321 . C32 . H322 . 109.501 no C32 . C33 . H331 . 109.460 no C32 . C33 . H332 . 109.379 no H331 . C33 . H332 . 109.476 no C32 . C33 . H333 . 109.593 no H331 . C33 . H333 . 109.408 no H332 . C33 . H333 . 109.512 no C29 . C34 . C35 . 108.8(3) yes C29 . C34 . H341 . 109.689 no C35 . C34 . H341 . 109.681 no C29 . C34 . H342 . 109.655 no C35 . C34 . H342 . 109.650 no H341 . C34 . H342 . 109.333 no C34 . C35 . C36 . 121.4(3) yes C34 . C35 . C40 . 119.9(3) yes C36 . C35 . C40 . 118.4(3) yes C35 . C36 . C37 . 120.8(3) yes C35 . C36 . H361 . 119.541 no C37 . C36 . H361 . 119.626 no C36 . C37 . C38 . 118.6(3) yes C36 . C37 . C55 . 119.7(3) yes C38 . C37 . C55 . 121.6(3) yes C37 . C38 . C39 . 121.7(3) yes C37 . C38 . H381 . 119.177 no C39 . C38 . H381 . 119.152 no C38 . C39 . C40 . 118.1(3) yes C38 . C39 . C44 . 120.1(3) yes C40 . C39 . C44 . 121.2(3) yes C39 . C40 . C35 . 121.9(3) yes C39 . C40 . O4 . 119.1(3) yes C35 . C40 . O4 . 118.9(3) yes O4 . C41 . C42 . 102.6(7) yes O4 . C41 . H411 . 111.077 no C42 . C41 . H411 . 111.155 no O4 . C41 . H412 . 111.324 no C42 . C41 . H412 . 111.134 no H411 . C41 . H412 . 109.434 no C41 . C42 . C43 . 110.6(7) yes C41 . C42 . H421 . 109.119 no C43 . C42 . H421 . 109.301 no C41 . C42 . H422 . 109.214 no C43 . C42 . H422 . 109.084 no H421 . C42 . H422 . 109.548 no C42 . C43 . H431 . 109.496 no C42 . C43 . H432 . 109.354 no H431 . C43 . H432 . 109.498 no C42 . C43 . H433 . 109.563 no H431 . C43 . H433 . 109.395 no H432 . C43 . H433 . 109.522 no O4 . C410 . C420 . 111.5(7) yes O4 . C410 . H414 . 108.858 no C420 . C410 . H414 . 108.966 no O4 . C410 . H415 . 109.054 no C420 . C410 . H415 . 108.877 no H414 . C410 . H415 . 109.536 no C410 . C420 . C430 . 109.9(8) yes C410 . C420 . H424 . 109.327 no C430 . C420 . H424 . 109.505 no C410 . C420 . H425 . 109.362 no C430 . C420 . H425 . 109.229 no H424 . C420 . H425 . 109.547 no C420 . C430 . H434 . 109.481 no C420 . C430 . H435 . 109.343 no H434 . C430 . H435 . 109.435 no C420 . C430 . H436 . 109.619 no H434 . C430 . H436 . 109.407 no H435 . C430 . H436 . 109.543 no C39 . C44 . C45 . 108.2(3) yes C39 . C44 . H441 . 109.850 no C45 . C44 . H441 . 109.669 no C39 . C44 . H442 . 109.660 no C45 . C44 . H442 . 109.885 no H441 . C44 . H442 . 109.537 no C44 . C45 . C46 . 121.0(3) yes C44 . C45 . C50 . 120.9(3) yes C46 . C45 . C50 . 117.7(3) yes C45 . C46 . C47 . 120.7(3) yes C45 . C46 . H461 . 119.613 no C47 . C46 . H461 . 119.694 no C46 . C47 . C48 . 120.4(3) yes C46 . C47 . H471 . 119.791 no C48 . C47 . H471 . 119.857 no C47 . C48 . C49 . 120.7(3) yes C47 . C48 . H481 . 119.721 no C49 . C48 . H481 . 119.587 no C48 . C49 . C50 . 118.3(3) yes C48 . C49 . C51 . 120.7(3) yes C50 . C49 . C51 . 120.6(3) yes C45 . C50 . C49 . 121.9(3) yes C45 . C50 . O5 . 118.3(3) yes C49 . C50 . O5 . 119.8(3) yes C49 . C51 . C19 . 109.0(3) yes C49 . C51 . H511 . 109.647 no C19 . C51 . H511 . 109.622 no C49 . C51 . H512 . 109.638 no C19 . C51 . H512 . 109.618 no H511 . C51 . H512 . 109.330 no O5 . C52 . C53 . 109.3(3) yes O5 . C52 . H521 . 109.643 no C53 . C52 . H521 . 109.430 no O5 . C52 . H522 . 109.415 no C53 . C52 . H522 . 109.552 no H521 . C52 . H522 . 109.515 no C52 . C53 . C54 . 112.8(4) yes C52 . C53 . H531 . 108.651 no C54 . C53 . H531 . 108.748 no C52 . C53 . H532 . 108.636 no C54 . C53 . H532 . 108.641 no H531 . C53 . H532 . 109.372 no C53 . C54 . H541 . 109.371 no C53 . C54 . H542 . 109.485 no H541 . C54 . H542 . 109.482 no C53 . C54 . H543 . 109.594 no H541 . C54 . H543 . 109.519 no H542 . C54 . H543 . 109.377 no C37 . C55 . O6 . 122.6(3) yes C37 . C55 . C56 . 117.0(3) yes O6 . C55 . C56 . 120.3(3) yes C55 . C56 . P2 . 115.7(2) yes C55 . C56 . H561 . 108.004 no P2 . C56 . H561 . 107.779 no C55 . C56 . H562 . 107.775 no P2 . C56 . H562 . 107.922 no H561 . C56 . H562 . 109.530 no P2 . C57 . C58 . 118.8(3) yes P2 . C57 . C62 . 122.8(3) yes C58 . C57 . C62 . 118.3(3) yes C57 . C58 . C59 . 120.7(4) yes C57 . C58 . H581 . 119.703 no C59 . C58 . H581 . 119.629 no C58 . C59 . C60 . 120.5(4) yes C58 . C59 . H591 . 119.824 no C60 . C59 . H591 . 119.693 no C59 . C60 . C61 . 119.8(4) yes C59 . C60 . H601 . 119.991 no C61 . C60 . H601 . 120.203 no C60 . C61 . C62 . 120.0(4) yes C60 . C61 . H611 . 120.022 no C62 . C61 . H611 . 119.959 no C57 . C62 . C61 . 120.7(4) yes C57 . C62 . H621 . 119.586 no C61 . C62 . H621 . 119.717 no P2 . C63 . C64 . 122.6(3) yes P2 . C63 . C68 . 119.1(3) yes C64 . C63 . C68 . 118.3(3) yes C63 . C64 . C65 . 120.2(4) yes C63 . C64 . H641 . 119.966 no C65 . C64 . H641 . 119.855 no C64 . C65 . C66 . 120.8(4) yes C64 . C65 . H651 . 119.637 no C66 . C65 . H651 . 119.549 no C65 . C66 . C67 . 119.6(4) yes C65 . C66 . H661 . 120.090 no C67 . C66 . H661 . 120.262 no C66 . C67 . C68 . 119.8(4) yes C66 . C67 . H671 . 120.167 no C68 . C67 . H671 . 120.069 no C67 . C68 . C63 . 121.3(4) yes C67 . C68 . H681 . 119.393 no C63 . C68 . H681 . 119.306 no Ni1 . C69 . C70 . 124.4(3) yes Ni1 . C69 . C74 . 117.9(3) yes C70 . C69 . C74 . 117.6(3) yes C69 . C70 . C71 . 121.3(4) yes C69 . C70 . H701 . 119.410 no C71 . C70 . H701 . 119.270 no C70 . C71 . C72 . 120.2(5) yes C70 . C71 . H711 . 119.840 no C72 . C71 . H711 . 119.992 no C71 . C72 . C73 . 119.0(4) yes C71 . C72 . H721 . 120.516 no C73 . C72 . H721 . 120.477 no C72 . C73 . C74 . 120.8(4) yes C72 . C73 . H731 . 119.669 no C74 . C73 . H731 . 119.520 no C69 . C74 . C73 . 121.1(4) yes C69 . C74 . H741 . 119.542 no C73 . C74 . H741 . 119.371 no