# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name P.Sathyadevi _publ_contact_author_email sakthikpt@rediffmail.com loop_ _publ_author_name S.Palanisamy K.Paramasivam R.Butorac A.Cowley N.Bhuvanesh D.Nallasamy data_rrmur301 _database_code_depnum_ccdc_archive 'CCDC 751231' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Ni hydrozone complex ; _chemical_name_common 'Ni hydrozone complex' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H27 N2 Ni O2 P' _chemical_formula_weight 573.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5980(3) _cell_length_b 15.2119(4) _cell_length_c 17.2447(5) _cell_angle_alpha 106.718(2) _cell_angle_beta 99.364(2) _cell_angle_gamma 104.284(2) _cell_volume 2732.79(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15259 _cell_measurement_theta_min 1.3 _cell_measurement_theta_max 29.6 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.120 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 0.802 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.843 _exptl_absorpt_correction_T_max 0.910 _exptl_absorpt_process_details '(SADABS; Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker SMART APEX II CCD area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59792 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 29.61 _reflns_number_total 15259 _reflns_number_gt 9357 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II (Bruker, 2008)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0543P)^2^+1.3465P] 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 15259 _refine_ls_number_parameters 705 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0924 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1302 _refine_ls_wR_factor_gt 0.1054 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.002 _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 0.77966(3) 0.04142(2) 0.709873(19) 0.03445(9) Uani 1 1 d . . . Ni2 Ni 0.23636(3) 0.43260(2) 0.79072(2) 0.03817(9) Uani 1 1 d . . . P2 P 0.38767(5) 0.44564(4) 0.72637(4) 0.03407(14) Uani 1 1 d . . . P1 P 0.62861(5) 0.01399(4) 0.77434(4) 0.03276(14) Uani 1 1 d . . . O1A O 0.75554(16) 0.15216(13) 0.70397(12) 0.0488(5) Uani 1 1 d . . . O1B O 0.25087(17) 0.31782(13) 0.79094(13) 0.0534(5) Uani 1 1 d . . . O2B O 0.23213(16) 0.55401(13) 0.79912(12) 0.0487(5) Uani 1 1 d . . . O2A O 0.79571(15) -0.07586(12) 0.70790(11) 0.0419(4) Uani 1 1 d . . . N2A N 0.94500(17) -0.03511(14) 0.64061(12) 0.0368(4) Uani 1 1 d . . . N2B N 0.07683(18) 0.51341(15) 0.86258(13) 0.0409(5) Uani 1 1 d . . . N1A N 0.90692(16) 0.04770(13) 0.65560(11) 0.0313(4) Uani 1 1 d . . . N1B N 0.10993(17) 0.42845(14) 0.84444(12) 0.0350(4) Uani 1 1 d . . . C6B C 0.0821(2) 0.27035(18) 0.85182(14) 0.0371(5) Uani 1 1 d . . . C28A C 0.6111(2) 0.11091(18) 0.85748(15) 0.0396(6) Uani 1 1 d . . . C6A C 0.9252(2) 0.20295(17) 0.64458(14) 0.0339(5) Uani 1 1 d . . . C10A C 0.8970(2) -0.19022(17) 0.65842(16) 0.0389(5) Uani 1 1 d . . . C7A C 0.9655(2) 0.11846(16) 0.63478(14) 0.0329(5) Uani 1 1 d . . . C16B C 0.3955(2) 0.52195(18) 0.66187(16) 0.0424(6) Uani 1 1 d . . . C10B C 0.1350(2) 0.67153(19) 0.85226(17) 0.0461(6) Uani 1 1 d . . . C22B C 0.5335(2) 0.49091(16) 0.80524(15) 0.0365(5) Uani 1 1 d . . . C16A C 0.6385(2) -0.07693(18) 0.82209(16) 0.0401(6) Uani 1 1 d . . . C1A C 0.8212(2) 0.21379(18) 0.67542(15) 0.0381(5) Uani 1 1 d . . . C28B C 0.3911(2) 0.33127(17) 0.65719(15) 0.0353(5) Uani 1 1 d . . . C7B C 0.0466(2) 0.35713(18) 0.86283(14) 0.0360(5) Uani 1 1 d . . . C9A C 0.8797(2) -0.09455(17) 0.66985(15) 0.0370(5) Uani 1 1 d . . . C9B C 0.1476(2) 0.57442(18) 0.83716(16) 0.0412(6) Uani 1 1 d . . . C27A C 0.3728(2) -0.0226(2) 0.71873(17) 0.0492(7) Uani 1 1 d . . . H27A H 0.3742 0.0087 0.7740 0.059 Uiso 1 1 calc R . . C5A C 0.9891(2) 0.27896(18) 0.62102(16) 0.0436(6) Uani 1 1 d . . . H5A H 1.0591 0.2747 0.6024 0.052 Uiso 1 1 calc R . . C27B C 0.6443(2) 0.48470(19) 0.78512(17) 0.0448(6) Uani 1 1 d . . . H27B H 0.6453 0.4575 0.7296 0.054 Uiso 1 1 calc R . . C5B C 0.0162(2) 0.19429(19) 0.87454(16) 0.0458(6) Uani 1 1 d . . . H5B H -0.0526 0.2000 0.8943 0.055 Uiso 1 1 calc R . . C8B C -0.0616(2) 0.3678(2) 0.89808(18) 0.0491(7) Uani 1 1 d . . . H8B1 H -0.0336 0.4011 0.9574 0.074 Uiso 1 1 calc R . . H8B2 H -0.1181 0.3051 0.8868 0.074 Uiso 1 1 calc R . . H8B3 H -0.1021 0.4041 0.8725 0.074 Uiso 1 1 calc R . . C8A C 1.0744(2) 0.11161(19) 0.59898(17) 0.0445(6) Uani 1 1 d . . . H8A1 H 1.0971 0.0569 0.6050 0.067 Uiso 1 1 calc R . . H8A2 H 1.1422 0.1694 0.6283 0.067 Uiso 1 1 calc R . . H8A3 H 1.0532 0.1041 0.5408 0.067 Uiso 1 1 calc R . . C23B C 0.5337(3) 0.52972(19) 0.88801(16) 0.0454(6) Uani 1 1 d . . . H23B H 0.4607 0.5337 0.9023 0.055 Uiso 1 1 calc R . . C22A C 0.4805(2) -0.03413(17) 0.69803(15) 0.0368(5) Uani 1 1 d . . . C33B C 0.3450(2) 0.3014(2) 0.57122(16) 0.0461(6) Uani 1 1 d . . . H33B H 0.3165 0.3422 0.5475 0.055 Uiso 1 1 calc R . . C11B C 0.0619(3) 0.7043(2) 0.90184(18) 0.0540(7) Uani 1 1 d . . . H11B H 0.0186 0.6642 0.9262 0.065 Uiso 1 1 calc R . . C1B C 0.1838(2) 0.25749(19) 0.81982(16) 0.0430(6) Uani 1 1 d . . . C4B C 0.0490(3) 0.1128(2) 0.86880(18) 0.0539(7) Uani 1 1 d . . . H4B H 0.0030 0.0643 0.8842 0.065 Uiso 1 1 calc R . . C2B C 0.2173(3) 0.1738(2) 0.8162(2) 0.0572(8) Uani 1 1 d . . . H2B H 0.2863 0.1667 0.7973 0.069 Uiso 1 1 calc R . . C21A C 0.5549(3) -0.1683(2) 0.79350(19) 0.0594(8) Uani 1 1 d . . . H21A H 0.4867 -0.1854 0.7492 0.071 Uiso 1 1 calc R . . C11A C 0.9606(3) -0.2270(2) 0.60233(18) 0.0513(7) Uani 1 1 d . . . H11A H 0.9940 -0.1910 0.5714 0.062 Uiso 1 1 calc R . . C4A C 0.9524(3) 0.3584(2) 0.62450(18) 0.0531(7) Uani 1 1 d . . . H4A H 0.9970 0.4071 0.6086 0.064 Uiso 1 1 calc R . . C31B C 0.3825(3) 0.1508(2) 0.55486(19) 0.0568(8) Uani 1 1 d . . . H31B H 0.3786 0.0899 0.5206 0.068 Uiso 1 1 calc R . . C23A C 0.4761(3) -0.0806(2) 0.61624(18) 0.0623(9) Uani 1 1 d . . . H23A H 0.5476 -0.0886 0.6017 0.075 Uiso 1 1 calc R . . C17A C 0.7385(3) -0.0534(2) 0.8883(2) 0.0584(8) Uani 1 1 d . . . H17A H 0.7958 0.0079 0.9080 0.070 Uiso 1 1 calc R . . C24B C 0.6421(3) 0.5629(2) 0.95005(18) 0.0584(8) Uani 1 1 d . . . H24B H 0.6419 0.5890 1.0058 0.070 Uiso 1 1 calc R . . C32B C 0.3413(3) 0.2114(2) 0.52076(19) 0.0581(8) Uani 1 1 d . . . H32B H 0.3105 0.1920 0.4632 0.070 Uiso 1 1 calc R . . C33A C 0.6305(3) 0.2014(2) 0.85141(19) 0.0550(7) Uani 1 1 d . . . H33A H 0.6550 0.2129 0.8055 0.066 Uiso 1 1 calc R . . C15B C 0.1975(3) 0.7326(2) 0.8156(2) 0.0716(10) Uani 1 1 d . . . H15B H 0.2467 0.7121 0.7814 0.086 Uiso 1 1 calc R . . C3A C 0.8479(3) 0.3659(2) 0.65202(19) 0.0551(7) Uani 1 1 d . . . H3A H 0.8213 0.4191 0.6536 0.066 Uiso 1 1 calc R . . C29B C 0.4331(2) 0.26900(19) 0.69070(17) 0.0451(6) Uani 1 1 d . . . H29B H 0.4639 0.2876 0.7482 0.054 Uiso 1 1 calc R . . C2A C 0.7846(3) 0.2951(2) 0.67664(19) 0.0515(7) Uani 1 1 d . . . H2A H 0.7147 0.3010 0.6948 0.062 Uiso 1 1 calc R . . C26B C 0.7512(3) 0.5187(2) 0.84714(19) 0.0549(7) Uani 1 1 d . . . H26B H 0.8248 0.5157 0.8334 0.066 Uiso 1 1 calc R . . C3B C 0.1516(3) 0.1030(2) 0.83982(19) 0.0587(8) Uani 1 1 d . . . H3B H 0.1754 0.0482 0.8365 0.070 Uiso 1 1 calc R . . C30B C 0.4295(3) 0.1796(2) 0.6393(2) 0.0554(7) Uani 1 1 d . . . H30B H 0.4592 0.1387 0.6623 0.066 Uiso 1 1 calc R . . C21B C 0.5004(3) 0.5603(3) 0.6412(2) 0.0823(12) Uani 1 1 d . . . H21B H 0.5728 0.5499 0.6627 0.099 Uiso 1 1 calc R . . C12A C 0.9745(3) -0.3165(2) 0.5921(2) 0.0698(9) Uani 1 1 d . . . H12A H 1.0163 -0.3410 0.5536 0.084 Uiso 1 1 calc R . . C15A C 0.8486(3) -0.2453(2) 0.7038(2) 0.0560(8) Uani 1 1 d . . . H15A H 0.8051 -0.2220 0.7415 0.067 Uiso 1 1 calc R . . C25B C 0.7501(3) 0.5571(2) 0.9289(2) 0.0620(8) Uani 1 1 d . . . H25B H 0.8229 0.5795 0.9706 0.074 Uiso 1 1 calc R . . C18A C 0.7538(4) -0.1202(3) 0.9252(2) 0.0762(10) Uani 1 1 d . . . H18A H 0.8207 -0.1036 0.9704 0.091 Uiso 1 1 calc R . . C26A C 0.2639(3) -0.0577(2) 0.6574(2) 0.0626(8) Uani 1 1 d . . . H26A H 0.1921 -0.0496 0.6714 0.075 Uiso 1 1 calc R . . C24A C 0.3668(3) -0.1157(3) 0.5551(2) 0.0745(10) Uani 1 1 d . . . H24A H 0.3648 -0.1471 0.4998 0.089 Uiso 1 1 calc R . . C14A C 0.8644(3) -0.3341(2) 0.6935(2) 0.0728(10) Uani 1 1 d . . . H14A H 0.8319 -0.3704 0.7245 0.087 Uiso 1 1 calc R . . C20A C 0.5729(4) -0.2346(2) 0.8310(3) 0.0845(12) Uani 1 1 d . . . H20A H 0.5166 -0.2963 0.8113 0.101 Uiso 1 1 calc R . . C13A C 0.9277(3) -0.3695(2) 0.6379(2) 0.0729(10) Uani 1 1 d . . . H13A H 0.9387 -0.4295 0.6315 0.087 Uiso 1 1 calc R . . C25A C 0.2616(3) -0.1040(3) 0.5764(2) 0.0718(10) Uani 1 1 d . . . H25A H 0.1879 -0.1279 0.5354 0.086 Uiso 1 1 calc R . . C29A C 0.5734(4) 0.0952(3) 0.9255(2) 0.0727(10) Uani 1 1 d . . . H29A H 0.5591 0.0344 0.9304 0.087 Uiso 1 1 calc R . . C17B C 0.2913(3) 0.5405(3) 0.6302(2) 0.0815(12) Uani 1 1 d . . . H17B H 0.2185 0.5166 0.6439 0.098 Uiso 1 1 calc R . . C12B C 0.0520(4) 0.7958(2) 0.9159(2) 0.0739(10) Uani 1 1 d . . . H12B H 0.0030 0.8171 0.9500 0.089 Uiso 1 1 calc R . . C32A C 0.6140(3) 0.2758(2) 0.9132(2) 0.0748(10) Uani 1 1 d . . . H32A H 0.6272 0.3368 0.9087 0.090 Uiso 1 1 calc R . . C19B C 0.3985(4) 0.6305(3) 0.5572(2) 0.0849(12) Uani 1 1 d . . . H19B H 0.3993 0.6661 0.5214 0.102 Uiso 1 1 calc R . . C13B C 0.1136(4) 0.8550(3) 0.8802(3) 0.0882(12) Uani 1 1 d . . . H13B H 0.1067 0.9166 0.8896 0.106 Uiso 1 1 calc R . . C19A C 0.6708(5) -0.2113(3) 0.8956(3) 0.0855(13) Uani 1 1 d . . . H19A H 0.6820 -0.2568 0.9200 0.103 Uiso 1 1 calc R . . C20B C 0.5014(4) 0.6139(3) 0.5893(3) 0.1014(15) Uani 1 1 d . . . H20B H 0.5743 0.6392 0.5762 0.122 Uiso 1 1 calc R . . C14B C 0.1860(4) 0.8234(3) 0.8305(3) 0.0947(14) Uani 1 1 d . . . H14B H 0.2282 0.8641 0.8061 0.114 Uiso 1 1 calc R . . C31A C 0.5783(4) 0.2588(3) 0.9802(2) 0.0860(12) Uani 1 1 d . . . H31A H 0.5685 0.3087 1.0221 0.103 Uiso 1 1 calc R . . C18B C 0.2938(4) 0.5944(4) 0.5780(3) 0.1108(17) Uani 1 1 d . . . H18B H 0.2223 0.6061 0.5567 0.133 Uiso 1 1 calc R . . C30A C 0.5567(5) 0.1694(3) 0.9866(2) 0.0999(15) Uani 1 1 d . . . H30A H 0.5307 0.1582 1.0321 0.120 Uiso 1 1 calc R . . 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 0.03239(16) 0.03365(17) 0.04329(18) 0.01668(13) 0.01701(13) 0.01162(13) Ni2 0.03641(17) 0.03619(18) 0.04766(19) 0.01660(14) 0.01874(14) 0.01329(14) P2 0.0332(3) 0.0336(3) 0.0381(3) 0.0134(3) 0.0133(3) 0.0111(3) P1 0.0307(3) 0.0328(3) 0.0380(3) 0.0131(2) 0.0139(2) 0.0109(2) O1A 0.0504(10) 0.0470(11) 0.0738(13) 0.0375(10) 0.0367(10) 0.0250(9) O1B 0.0576(11) 0.0474(11) 0.0810(14) 0.0362(10) 0.0448(11) 0.0261(9) O2B 0.0475(10) 0.0416(10) 0.0676(12) 0.0232(9) 0.0297(9) 0.0167(8) O2A 0.0439(9) 0.0365(9) 0.0559(11) 0.0209(8) 0.0279(8) 0.0150(8) N2A 0.0345(10) 0.0339(11) 0.0451(11) 0.0148(9) 0.0152(9) 0.0112(9) N2B 0.0399(11) 0.0359(11) 0.0535(13) 0.0171(10) 0.0183(10) 0.0171(9) N1A 0.0313(9) 0.0295(10) 0.0325(10) 0.0085(8) 0.0071(8) 0.0114(8) N1B 0.0334(10) 0.0341(11) 0.0366(10) 0.0095(8) 0.0091(8) 0.0114(8) C6B 0.0361(12) 0.0396(13) 0.0330(12) 0.0127(10) 0.0058(10) 0.0089(10) C28A 0.0367(12) 0.0389(14) 0.0428(13) 0.0086(11) 0.0129(11) 0.0155(11) C6A 0.0350(12) 0.0325(12) 0.0340(12) 0.0119(10) 0.0097(10) 0.0086(10) C10A 0.0355(12) 0.0341(13) 0.0484(14) 0.0151(11) 0.0120(11) 0.0112(10) C7A 0.0326(11) 0.0331(12) 0.0324(12) 0.0126(9) 0.0100(9) 0.0064(10) C16B 0.0478(14) 0.0363(13) 0.0485(15) 0.0201(11) 0.0154(12) 0.0139(11) C10B 0.0481(15) 0.0390(14) 0.0556(16) 0.0185(12) 0.0173(13) 0.0159(12) C22B 0.0391(12) 0.0297(12) 0.0409(13) 0.0128(10) 0.0116(10) 0.0093(10) C16A 0.0433(13) 0.0391(14) 0.0484(15) 0.0189(11) 0.0236(12) 0.0186(11) C1A 0.0375(12) 0.0387(13) 0.0422(13) 0.0173(11) 0.0143(11) 0.0120(11) C28B 0.0325(11) 0.0338(12) 0.0394(13) 0.0114(10) 0.0135(10) 0.0083(10) C7B 0.0324(11) 0.0388(13) 0.0349(12) 0.0123(10) 0.0063(10) 0.0099(10) C9A 0.0348(12) 0.0346(13) 0.0428(13) 0.0140(10) 0.0123(10) 0.0104(10) C9B 0.0392(13) 0.0364(13) 0.0492(15) 0.0142(11) 0.0122(11) 0.0140(11) C27A 0.0402(14) 0.0572(17) 0.0488(15) 0.0172(13) 0.0151(12) 0.0117(13) C5A 0.0453(14) 0.0379(14) 0.0503(15) 0.0181(12) 0.0194(12) 0.0089(11) C27B 0.0400(14) 0.0474(15) 0.0468(15) 0.0145(12) 0.0120(12) 0.0142(12) C5B 0.0440(14) 0.0466(16) 0.0478(15) 0.0216(12) 0.0124(12) 0.0089(12) C8B 0.0416(14) 0.0573(17) 0.0620(17) 0.0292(14) 0.0262(13) 0.0199(13) C8A 0.0406(13) 0.0433(15) 0.0584(16) 0.0229(12) 0.0255(12) 0.0133(11) C23B 0.0507(15) 0.0414(15) 0.0442(15) 0.0130(12) 0.0149(12) 0.0145(12) C22A 0.0326(12) 0.0380(13) 0.0410(13) 0.0145(10) 0.0119(10) 0.0100(10) C33B 0.0467(14) 0.0469(16) 0.0447(15) 0.0162(12) 0.0115(12) 0.0140(12) C11B 0.0681(19) 0.0476(16) 0.0595(18) 0.0233(14) 0.0265(15) 0.0282(15) C1B 0.0481(14) 0.0402(14) 0.0460(14) 0.0185(11) 0.0167(12) 0.0152(12) C4B 0.0598(18) 0.0492(17) 0.0595(17) 0.0304(14) 0.0192(14) 0.0118(14) C2B 0.0658(19) 0.0501(17) 0.077(2) 0.0333(15) 0.0355(16) 0.0305(15) C21A 0.077(2) 0.0418(16) 0.0587(18) 0.0202(14) 0.0218(16) 0.0109(15) C11A 0.0608(17) 0.0461(16) 0.0624(18) 0.0255(14) 0.0307(14) 0.0255(14) C4A 0.0636(18) 0.0375(15) 0.0627(18) 0.0238(13) 0.0248(15) 0.0097(13) C31B 0.0664(19) 0.0393(15) 0.0627(19) 0.0077(14) 0.0321(16) 0.0144(14) C23A 0.0451(16) 0.084(2) 0.0463(16) 0.0055(15) 0.0131(13) 0.0193(16) C17A 0.0511(17) 0.069(2) 0.071(2) 0.0406(17) 0.0189(15) 0.0246(15) C24B 0.072(2) 0.0540(18) 0.0376(15) 0.0100(13) 0.0067(14) 0.0106(15) C32B 0.0591(18) 0.0565(19) 0.0473(16) 0.0051(14) 0.0152(14) 0.0119(15) C33A 0.0571(17) 0.0427(16) 0.0665(19) 0.0140(14) 0.0256(15) 0.0165(14) C15B 0.084(2) 0.0538(19) 0.098(3) 0.0374(19) 0.048(2) 0.0270(18) C3A 0.0660(19) 0.0416(15) 0.075(2) 0.0307(14) 0.0294(16) 0.0268(14) C29B 0.0506(15) 0.0435(15) 0.0457(15) 0.0165(12) 0.0177(12) 0.0172(12) C2A 0.0530(16) 0.0461(16) 0.0715(19) 0.0297(14) 0.0282(15) 0.0240(13) C26B 0.0406(15) 0.0605(19) 0.0649(19) 0.0246(15) 0.0098(14) 0.0164(14) C3B 0.077(2) 0.0474(17) 0.071(2) 0.0332(15) 0.0307(17) 0.0296(16) C30B 0.0669(19) 0.0452(16) 0.070(2) 0.0266(15) 0.0302(16) 0.0273(14) C21B 0.063(2) 0.117(3) 0.107(3) 0.085(3) 0.035(2) 0.033(2) C12A 0.086(2) 0.0538(19) 0.089(2) 0.0258(18) 0.045(2) 0.0394(18) C15A 0.0669(19) 0.0460(16) 0.073(2) 0.0315(15) 0.0378(16) 0.0226(14) C25B 0.0503(17) 0.063(2) 0.0592(19) 0.0205(16) -0.0058(15) 0.0067(15) C18A 0.079(2) 0.104(3) 0.082(2) 0.057(2) 0.029(2) 0.054(2) C26A 0.0354(15) 0.079(2) 0.070(2) 0.0259(18) 0.0122(14) 0.0133(15) C24A 0.060(2) 0.099(3) 0.0426(17) 0.0048(17) 0.0071(15) 0.0152(19) C14A 0.082(2) 0.055(2) 0.105(3) 0.050(2) 0.041(2) 0.0253(18) C20A 0.137(4) 0.0430(19) 0.083(3) 0.0310(18) 0.043(3) 0.023(2) C13A 0.088(2) 0.0438(18) 0.106(3) 0.0335(18) 0.039(2) 0.0356(18) C25A 0.0466(17) 0.093(3) 0.060(2) 0.0242(19) -0.0003(15) 0.0058(17) C29A 0.115(3) 0.065(2) 0.064(2) 0.0290(17) 0.047(2) 0.050(2) C17B 0.061(2) 0.122(3) 0.100(3) 0.076(3) 0.029(2) 0.044(2) C12B 0.103(3) 0.060(2) 0.081(2) 0.0281(18) 0.040(2) 0.049(2) C32A 0.083(2) 0.0407(17) 0.095(3) 0.0064(17) 0.033(2) 0.0217(17) C19B 0.120(3) 0.078(3) 0.084(3) 0.056(2) 0.035(3) 0.039(2) C13B 0.133(4) 0.047(2) 0.111(3) 0.040(2) 0.052(3) 0.045(2) C19A 0.142(4) 0.075(3) 0.094(3) 0.062(2) 0.064(3) 0.067(3) C20B 0.088(3) 0.127(4) 0.119(3) 0.095(3) 0.035(3) 0.019(3) C14B 0.128(4) 0.054(2) 0.133(4) 0.053(2) 0.068(3) 0.035(2) C31A 0.110(3) 0.075(3) 0.072(2) 0.002(2) 0.031(2) 0.050(2) C18B 0.105(3) 0.164(5) 0.133(4) 0.112(4) 0.042(3) 0.082(3) C30A 0.167(4) 0.102(3) 0.067(2) 0.030(2) 0.066(3) 0.079(3) _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 O1A 1.8023(18) . ? Ni1 O2A 1.8303(17) . ? Ni1 N1A 1.8696(18) . ? Ni1 P1 2.2403(6) . ? Ni2 O1B 1.7961(18) . ? Ni2 O2B 1.8241(18) . ? Ni2 N1B 1.8554(19) . ? Ni2 P2 2.2224(6) . ? P2 C28B 1.819(2) . ? P2 C16B 1.821(3) . ? P2 C22B 1.823(3) . ? P1 C28A 1.816(2) . ? P1 C22A 1.818(2) . ? P1 C16A 1.818(3) . ? O1A C1A 1.318(3) . ? O1B C1B 1.316(3) . ? O2B C9B 1.316(3) . ? O2A C9A 1.303(3) . ? N2A C9A 1.301(3) . ? N2A N1A 1.405(3) . ? N2B C9B 1.305(3) . ? N2B N1B 1.402(3) . ? N1A C7A 1.300(3) . ? N1B C7B 1.303(3) . ? C6B C1B 1.413(3) . ? C6B C5B 1.414(3) . ? C6B C7B 1.448(3) . ? C28A C33A 1.376(4) . ? C28A C29A 1.379(4) . ? C6A C5A 1.413(3) . ? C6A C1A 1.422(3) . ? C6A C7A 1.448(3) . ? C10A C11A 1.384(3) . ? C10A C15A 1.385(3) . ? C10A C9A 1.479(3) . ? C7A C8A 1.506(3) . ? C16B C21B 1.363(4) . ? C16B C17B 1.371(4) . ? C10B C11B 1.378(4) . ? C10B C15B 1.393(4) . ? C10B C9B 1.473(4) . ? C22B C23B 1.378(3) . ? C22B C27B 1.402(3) . ? C16A C21A 1.379(4) . ? C16A C17A 1.380(4) . ? C1A C2A 1.399(4) . ? C28B C29B 1.385(4) . ? C28B C33B 1.387(3) . ? C7B C8B 1.504(3) . ? C27A C26A 1.381(4) . ? C27A C22A 1.391(3) . ? C5A C4A 1.366(4) . ? C27B C26B 1.372(4) . ? C5B C4B 1.366(4) . ? C23B C24B 1.385(4) . ? C22A C23A 1.370(4) . ? C33B C32B 1.381(4) . ? C11B C12B 1.380(4) . ? C1B C2B 1.408(4) . ? C4B C3B 1.388(4) . ? C2B C3B 1.362(4) . ? C21A C20A 1.382(4) . ? C11A C12A 1.374(4) . ? C4A C3A 1.389(4) . ? C31B C32B 1.365(4) . ? C31B C30B 1.366(4) . ? C23A C24A 1.382(4) . ? C17A C18A 1.378(4) . ? C24B C25B 1.377(4) . ? C33A C32A 1.391(4) . ? C15B C14B 1.375(5) . ? C3A C2A 1.362(4) . ? C29B C30B 1.380(4) . ? C26B C25B 1.366(4) . ? C21B C20B 1.373(5) . ? C12A C13A 1.365(5) . ? C15A C14A 1.372(4) . ? C18A C19A 1.372(6) . ? C26A C25A 1.364(4) . ? C24A C25A 1.369(4) . ? C14A C13A 1.370(5) . ? C20A C19A 1.349(6) . ? C29A C30A 1.382(4) . ? C17B C18B 1.381(5) . ? C12B C13B 1.358(5) . ? C32A C31A 1.360(5) . ? C19B C20B 1.345(6) . ? C19B C18B 1.353(6) . ? C13B C14B 1.366(5) . ? C31A C30A 1.359(5) . ? 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 O1A Ni1 O2A 175.56(9) . . ? O1A Ni1 N1A 95.54(8) . . ? O2A Ni1 N1A 84.32(7) . . ? O1A Ni1 P1 92.21(5) . . ? O2A Ni1 P1 87.88(5) . . ? N1A Ni1 P1 172.20(6) . . ? O1B Ni2 O2B 174.96(9) . . ? O1B Ni2 N1B 95.53(8) . . ? O2B Ni2 N1B 84.76(8) . . ? O1B Ni2 P2 87.64(6) . . ? O2B Ni2 P2 92.07(6) . . ? N1B Ni2 P2 176.83(7) . . ? C28B P2 C16B 103.89(11) . . ? C28B P2 C22B 103.92(11) . . ? C16B P2 C22B 107.67(11) . . ? C28B P2 Ni2 114.26(7) . . ? C16B P2 Ni2 117.75(9) . . ? C22B P2 Ni2 108.32(8) . . ? C28A P1 C22A 104.23(11) . . ? C28A P1 C16A 103.50(12) . . ? C22A P1 C16A 106.30(12) . . ? C28A P1 Ni1 121.04(8) . . ? C22A P1 Ni1 109.65(8) . . ? C16A P1 Ni1 111.03(8) . . ? C1A O1A Ni1 126.73(16) . . ? C1B O1B Ni2 126.74(16) . . ? C9B O2B Ni2 110.33(16) . . ? C9A O2A Ni1 110.59(15) . . ? C9A N2A N1A 108.68(18) . . ? C9B N2B N1B 108.61(19) . . ? C7A N1A N2A 118.27(18) . . ? C7A N1A Ni1 128.81(16) . . ? N2A N1A Ni1 112.83(13) . . ? C7B N1B N2B 117.83(19) . . ? C7B N1B Ni2 128.85(17) . . ? N2B N1B Ni2 113.23(14) . . ? C1B C6B C5B 116.7(2) . . ? C1B C6B C7B 122.7(2) . . ? C5B C6B C7B 120.6(2) . . ? C33A C28A C29A 118.7(3) . . ? C33A C28A P1 119.8(2) . . ? C29A C28A P1 121.5(2) . . ? C5A C6A C1A 116.8(2) . . ? C5A C6A C7A 119.6(2) . . ? C1A C6A C7A 123.5(2) . . ? C11A C10A C15A 118.5(2) . . ? C11A C10A C9A 121.3(2) . . ? C15A C10A C9A 120.2(2) . . ? N1A C7A C6A 120.3(2) . . ? N1A C7A C8A 119.8(2) . . ? C6A C7A C8A 120.0(2) . . ? C21B C16B C17B 117.5(3) . . ? C21B C16B P2 123.0(2) . . ? C17B C16B P2 119.4(2) . . ? C11B C10B C15B 118.3(3) . . ? C11B C10B C9B 121.7(2) . . ? C15B C10B C9B 120.0(2) . . ? C23B C22B C27B 118.9(2) . . ? C23B C22B P2 118.50(19) . . ? C27B C22B P2 122.52(19) . . ? C21A C16A C17A 118.9(3) . . ? C21A C16A P1 123.6(2) . . ? C17A C16A P1 117.4(2) . . ? O1A C1A C2A 116.5(2) . . ? O1A C1A C6A 124.5(2) . . ? C2A C1A C6A 119.0(2) . . ? C29B C28B C33B 118.5(2) . . ? C29B C28B P2 119.78(19) . . ? C33B C28B P2 121.6(2) . . ? N1B C7B C6B 120.5(2) . . ? N1B C7B C8B 118.8(2) . . ? C6B C7B C8B 120.7(2) . . ? N2A C9A O2A 123.5(2) . . ? N2A C9A C10A 119.8(2) . . ? O2A C9A C10A 116.6(2) . . ? N2B C9B O2B 123.0(2) . . ? N2B C9B C10B 119.4(2) . . ? O2B C9B C10B 117.5(2) . . ? C26A C27A C22A 120.1(3) . . ? C4A C5A C6A 122.7(2) . . ? C26B C27B C22B 120.1(2) . . ? C4B C5B C6B 122.9(3) . . ? C22B C23B C24B 120.3(3) . . ? C23A C22A C27A 118.8(2) . . ? C23A C22A P1 118.35(19) . . ? C27A C22A P1 122.78(19) . . ? C32B C33B C28B 120.3(3) . . ? C10B C11B C12B 120.9(3) . . ? O1B C1B C2B 115.7(2) . . ? O1B C1B C6B 125.0(2) . . ? C2B C1B C6B 119.3(2) . . ? C5B C4B C3B 119.5(3) . . ? C3B C2B C1B 121.8(3) . . ? C16A C21A C20A 119.7(3) . . ? C12A C11A C10A 120.4(3) . . ? C5A C4A C3A 119.5(2) . . ? C32B C31B C30B 120.0(3) . . ? C22A C23A C24A 120.8(3) . . ? C18A C17A C16A 120.3(3) . . ? C25B C24B C23B 119.8(3) . . ? C31B C32B C33B 120.4(3) . . ? C28A C33A C32A 120.6(3) . . ? C14B C15B C10B 119.7(3) . . ? C2A C3A C4A 119.8(3) . . ? C30B C29B C28B 120.4(3) . . ? C3A C2A C1A 122.1(3) . . ? C25B C26B C27B 120.3(3) . . ? C2B C3B C4B 119.8(3) . . ? C31B C30B C29B 120.4(3) . . ? C16B C21B C20B 121.3(3) . . ? C13A C12A C11A 120.6(3) . . ? C14A C15A C10A 120.4(3) . . ? C26B C25B C24B 120.5(3) . . ? C19A C18A C17A 120.2(4) . . ? C25A C26A C27A 120.0(3) . . ? C25A C24A C23A 119.7(3) . . ? C13A C14A C15A 120.5(3) . . ? C19A C20A C21A 121.2(4) . . ? C12A C13A C14A 119.7(3) . . ? C26A C25A C24A 120.5(3) . . ? C28A C29A C30A 120.4(3) . . ? C16B C17B C18B 120.4(3) . . ? C13B C12B C11B 120.3(3) . . ? C31A C32A C33A 119.5(3) . . ? C20B C19B C18B 118.6(3) . . ? C12B C13B C14B 119.6(3) . . ? C20A C19A C18A 119.6(3) . . ? C19B C20B C21B 121.0(4) . . ? C13B C14B C15B 121.2(3) . . ? C30A C31A C32A 120.6(3) . . ? C19B C18B C17B 121.1(4) . . ? C31A C30A C29A 120.1(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 29.61 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.675 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.064 data_shelxl _database_code_depnum_ccdc_archive 'CCDC 780528' #TrackingRef 'Niths.cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H27 N2 Ni O2 P' _chemical_formula_sum 'C33 H27 N2 Ni O2 P' _chemical_formula_weight 573.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2703(10) _cell_length_b 11.8729(11) _cell_length_c 11.9851(11) _cell_angle_alpha 81.516(2) _cell_angle_beta 68.128(2) _cell_angle_gamma 89.718(2) _cell_volume 1339.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3761 _cell_measurement_theta_min 1.7388 _cell_measurement_theta_max 30.8261 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.542 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; Abscor. T. Higashi. (2001). Rigaku Corp. Tokyo, Japan ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC-12 with Saturn 724+ CCD' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14449 _diffrn_reflns_av_R_equivalents 0.0991 _diffrn_reflns_av_sigmaI/netI 0.0905 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4696 _reflns_number_gt 4020 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. An Integrated System of Windows Programs for the Solution, Refinement and Analysis of Single Crystal X-ray Diffraction Data. Sheldrick, G. M. (2008). SHELXL-97. Acat Cryst., A64, 112-122. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _publ_section_acknowledgements ; The data were collected using instrumentation purchased with funds provided by the National Science Foundation Grant No. 0741973. ; _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _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^)+(0.0405P)^2^+1.1436P] 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 4696 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1248 _refine_ls_wR_factor_gt 0.1179 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.000 _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 C1 C 0.9743(3) 0.2520(3) 0.2746(3) 0.0265(7) Uani 1 1 d . . . C2 C 1.0738(3) 0.3459(3) 0.2298(3) 0.0286(7) Uani 1 1 d . . . H2 H 1.0849 0.3916 0.1566 0.034 Uiso 1 1 calc R . . C3 C 1.1546(3) 0.3704(3) 0.2939(3) 0.0308(7) Uani 1 1 d . . . H3 H 1.2191 0.4328 0.2633 0.037 Uiso 1 1 calc R . . C4 C 1.1411(3) 0.3024(3) 0.4050(3) 0.0294(7) Uani 1 1 d . . . H4 H 1.1954 0.3195 0.4481 0.035 Uiso 1 1 calc R . . C5 C 1.0458(3) 0.2102(3) 0.4481(3) 0.0270(7) Uani 1 1 d . . . H5 H 1.0366 0.1646 0.5210 0.032 Uiso 1 1 calc R . . C6 C 0.9612(3) 0.1828(3) 0.3848(3) 0.0252(7) Uani 1 1 d . . . C7 C 0.8654(3) 0.0836(3) 0.4352(3) 0.0241(6) Uani 1 1 d . . . H7 H 0.8631 0.0403 0.5073 0.029 Uiso 1 1 calc R . . C8 C 0.6163(3) -0.0601(3) 0.3817(3) 0.0238(7) Uani 1 1 d . . . C9 C 0.5167(3) -0.1610(3) 0.4202(3) 0.0241(6) Uani 1 1 d . . . C10 C 0.5151(3) -0.2477(3) 0.5137(3) 0.0267(7) Uani 1 1 d . . . H10 H 0.5762 -0.2415 0.5538 0.032 Uiso 1 1 calc R . . C11 C 0.4224(3) -0.3432(3) 0.5471(3) 0.0289(7) Uani 1 1 d . . . H11 H 0.4228 -0.4004 0.6090 0.035 Uiso 1 1 calc R . . C12 C 0.3288(3) -0.3541(3) 0.4889(3) 0.0294(7) Uani 1 1 d . . . C13 C 0.3308(3) -0.2667(3) 0.3969(3) 0.0288(7) Uani 1 1 d . . . H13 H 0.2694 -0.2728 0.3572 0.035 Uiso 1 1 calc R . . C14 C 0.4219(3) -0.1709(3) 0.3628(3) 0.0255(7) Uani 1 1 d . . . H14 H 0.4200 -0.1133 0.3018 0.031 Uiso 1 1 calc R . . C15 C 0.2291(4) -0.4579(3) 0.5269(3) 0.0394(8) Uani 1 1 d . . . H15A H 0.1776 -0.4550 0.4742 0.059 Uiso 1 1 calc R . . H15B H 0.1646 -0.4593 0.6093 0.059 Uiso 1 1 calc R . . H15C H 0.2814 -0.5255 0.5215 0.059 Uiso 1 1 calc R . . C16 C 0.5423(3) 0.1713(2) 0.0853(3) 0.0213(6) Uani 1 1 d . . . C17 C 0.4241(3) 0.1394(3) 0.1927(3) 0.0256(7) Uani 1 1 d . . . H17 H 0.4295 0.1437 0.2678 0.031 Uiso 1 1 calc R . . C18 C 0.2994(3) 0.1016(3) 0.1875(3) 0.0284(7) Uani 1 1 d . . . H18 H 0.2211 0.0820 0.2590 0.034 Uiso 1 1 calc R . . C19 C 0.2903(3) 0.0929(3) 0.0769(3) 0.0292(7) Uani 1 1 d . . . H19 H 0.2062 0.0677 0.0740 0.035 Uiso 1 1 calc R . . C20 C 0.4079(3) 0.1220(3) -0.0303(3) 0.0288(7) Uani 1 1 d . . . H20 H 0.4026 0.1146 -0.1048 0.035 Uiso 1 1 calc R . . C21 C 0.5329(3) 0.1619(3) -0.0264(3) 0.0261(7) Uani 1 1 d . . . H21 H 0.6105 0.1825 -0.0983 0.031 Uiso 1 1 calc R . . C22 C 0.8464(3) 0.2288(3) -0.0458(3) 0.0218(6) Uani 1 1 d . . . C23 C 0.9517(3) 0.1515(3) -0.0555(3) 0.0261(7) Uani 1 1 d . . . H23 H 0.9452 0.0977 0.0114 0.031 Uiso 1 1 calc R . . C24 C 1.0662(3) 0.1542(3) -0.1647(3) 0.0294(7) Uani 1 1 d . . . H24 H 1.1361 0.1028 -0.1705 0.035 Uiso 1 1 calc R . . C25 C 1.0757(3) 0.2342(3) -0.2651(3) 0.0276(7) Uani 1 1 d . . . H25 H 1.1516 0.2358 -0.3384 0.033 Uiso 1 1 calc R . . C26 C 0.9720(3) 0.3116(3) -0.2560(3) 0.0276(7) Uani 1 1 d . . . H26 H 0.9787 0.3652 -0.3231 0.033 Uiso 1 1 calc R . . C27 C 0.8576(3) 0.3091(3) -0.1465(3) 0.0250(7) Uani 1 1 d . . . H27 H 0.7885 0.3613 -0.1407 0.030 Uiso 1 1 calc R . . C28 C 0.6760(3) 0.3738(3) 0.1162(3) 0.0223(6) Uani 1 1 d . . . C29 C 0.7909(3) 0.4437(3) 0.1041(3) 0.0271(7) Uani 1 1 d . . . H29 H 0.8800 0.4149 0.0799 0.032 Uiso 1 1 calc R . . C30 C 0.7752(3) 0.5549(3) 0.1272(3) 0.0300(7) Uani 1 1 d . . . H30 H 0.8531 0.6003 0.1180 0.036 Uiso 1 1 calc R . . C31 C 0.6425(4) 0.5981(3) 0.1643(3) 0.0379(8) Uani 1 1 d . . . H31 H 0.6310 0.6722 0.1815 0.045 Uiso 1 1 calc R . . C32 C 0.5269(4) 0.5306(3) 0.1755(4) 0.0410(9) Uani 1 1 d . . . H32 H 0.4384 0.5602 0.1991 0.049 Uiso 1 1 calc R . . C33 C 0.5424(3) 0.4194(3) 0.1520(3) 0.0327(8) Uani 1 1 d . . . H33 H 0.4644 0.3748 0.1598 0.039 Uiso 1 1 calc R . . N1 N 0.7826(2) 0.0518(2) 0.3856(2) 0.0218(5) Uani 1 1 d . . . N2 N 0.6961(2) -0.0481(2) 0.4436(2) 0.0237(5) Uani 1 1 d . . . O1 O 0.8975(2) 0.23560(18) 0.20940(18) 0.0280(5) Uani 1 1 d . . . O2 O 0.6219(2) 0.01087(17) 0.28528(18) 0.0236(5) Uani 1 1 d . . . P1 P 0.70054(7) 0.22372(6) 0.10057(7) 0.02083(19) Uani 1 1 d . . . Ni1 Ni 0.75423(4) 0.12858(3) 0.25083(3) 0.02177(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0247(15) 0.0284(17) 0.0255(17) -0.0045(14) -0.0084(13) 0.0044(13) C2 0.0281(16) 0.0281(17) 0.0285(17) 0.0024(14) -0.0121(13) -0.0011(13) C3 0.0281(16) 0.0268(18) 0.0378(19) -0.0060(15) -0.0123(14) 0.0015(13) C4 0.0311(17) 0.0280(18) 0.0343(18) -0.0065(14) -0.0177(14) 0.0041(13) C5 0.0293(16) 0.0274(17) 0.0288(17) -0.0093(14) -0.0143(13) 0.0076(13) C6 0.0255(15) 0.0244(16) 0.0275(17) -0.0070(14) -0.0110(13) 0.0059(12) C7 0.0252(15) 0.0267(17) 0.0212(16) -0.0034(13) -0.0100(12) 0.0089(13) C8 0.0234(15) 0.0244(16) 0.0210(16) -0.0062(13) -0.0045(12) 0.0048(12) C9 0.0235(15) 0.0240(16) 0.0218(15) -0.0053(13) -0.0043(12) 0.0027(12) C10 0.0275(16) 0.0268(17) 0.0249(16) -0.0025(14) -0.0095(13) 0.0026(13) C11 0.0325(17) 0.0264(17) 0.0237(16) 0.0002(14) -0.0075(13) 0.0021(13) C12 0.0289(16) 0.0263(17) 0.0270(17) -0.0090(14) -0.0020(13) 0.0003(13) C13 0.0233(15) 0.0343(19) 0.0291(17) -0.0106(15) -0.0083(13) 0.0016(13) C14 0.0281(16) 0.0254(17) 0.0226(16) -0.0073(13) -0.0076(13) 0.0036(13) C15 0.0357(19) 0.034(2) 0.046(2) -0.0105(17) -0.0115(16) -0.0045(15) C16 0.0224(14) 0.0179(15) 0.0243(16) -0.0032(12) -0.0096(12) 0.0044(12) C17 0.0289(16) 0.0261(17) 0.0226(16) -0.0064(13) -0.0098(13) 0.0055(13) C18 0.0234(15) 0.0274(17) 0.0300(17) -0.0036(14) -0.0054(13) 0.0019(13) C19 0.0269(16) 0.0265(17) 0.0370(19) -0.0036(14) -0.0158(14) 0.0009(13) C20 0.0339(17) 0.0301(18) 0.0256(17) -0.0046(14) -0.0147(14) 0.0018(14) C21 0.0286(16) 0.0220(16) 0.0267(17) -0.0006(13) -0.0105(13) 0.0031(13) C22 0.0232(14) 0.0225(15) 0.0201(15) -0.0045(12) -0.0082(12) -0.0002(12) C23 0.0329(16) 0.0211(16) 0.0246(16) -0.0013(13) -0.0121(13) 0.0031(13) C24 0.0272(16) 0.0285(17) 0.0305(18) -0.0080(15) -0.0075(13) 0.0078(13) C25 0.0264(16) 0.0331(18) 0.0204(16) -0.0073(14) -0.0044(12) 0.0008(13) C26 0.0291(16) 0.0315(18) 0.0210(16) -0.0003(14) -0.0094(13) -0.0024(13) C27 0.0235(15) 0.0261(16) 0.0267(17) -0.0009(13) -0.0122(13) 0.0025(12) C28 0.0293(15) 0.0209(15) 0.0183(15) -0.0010(12) -0.0115(12) 0.0050(12) C29 0.0253(15) 0.0265(17) 0.0285(17) -0.0027(14) -0.0097(13) 0.0028(13) C30 0.0297(16) 0.0271(17) 0.0348(18) -0.0038(14) -0.0144(14) -0.0025(13) C31 0.044(2) 0.0238(18) 0.051(2) -0.0103(16) -0.0215(17) 0.0061(15) C32 0.0307(18) 0.032(2) 0.061(2) -0.0127(18) -0.0166(17) 0.0101(15) C33 0.0263(16) 0.0269(18) 0.044(2) -0.0078(16) -0.0116(14) 0.0039(13) N1 0.0226(12) 0.0210(13) 0.0195(13) -0.0047(11) -0.0047(10) 0.0045(10) N2 0.0249(13) 0.0227(13) 0.0236(13) -0.0024(11) -0.0096(10) 0.0016(10) O1 0.0327(11) 0.0304(12) 0.0236(11) 0.0015(9) -0.0158(9) -0.0028(9) O2 0.0278(11) 0.0239(11) 0.0184(11) -0.0010(9) -0.0087(8) 0.0019(9) P1 0.0218(4) 0.0207(4) 0.0197(4) -0.0026(3) -0.0078(3) 0.0030(3) Ni1 0.0233(2) 0.0224(2) 0.0192(2) -0.00063(16) -0.00853(16) 0.00182(15) _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 C1 O1 1.333(4) . ? C1 C6 1.410(4) . ? C1 C2 1.415(4) . ? C2 C3 1.381(4) . ? C2 H2 0.9300 . ? C3 C4 1.411(5) . ? C3 H3 0.9300 . ? C4 C5 1.375(4) . ? C4 H4 0.9300 . ? C5 C6 1.415(4) . ? C5 H5 0.9300 . ? C6 C7 1.441(4) . ? C7 N1 1.291(4) . ? C7 H7 0.9300 . ? C8 O2 1.308(4) . ? C8 N2 1.315(4) . ? C8 C9 1.480(4) . ? C9 C14 1.399(4) . ? C9 C10 1.401(4) . ? C10 C11 1.394(4) . ? C10 H10 0.9300 . ? C11 C12 1.398(4) . ? C11 H11 0.9300 . ? C12 C13 1.391(5) . ? C12 C15 1.509(4) . ? C13 C14 1.388(4) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C21 1.398(4) . ? C16 C17 1.404(4) . ? C16 P1 1.824(3) . ? C17 C18 1.385(4) . ? C17 H17 0.9300 . ? C18 C19 1.382(4) . ? C18 H18 0.9300 . ? C19 C20 1.395(4) . ? C19 H19 0.9300 . ? C20 C21 1.391(4) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C27 1.391(4) . ? C22 C23 1.398(4) . ? C22 P1 1.827(3) . ? C23 C24 1.392(4) . ? C23 H23 0.9300 . ? C24 C25 1.391(5) . ? C24 H24 0.9300 . ? C25 C26 1.387(4) . ? C25 H25 0.9300 . ? C26 C27 1.394(4) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.396(4) . ? C28 C33 1.407(4) . ? C28 P1 1.826(3) . ? C29 C30 1.385(4) . ? C29 H29 0.9300 . ? C30 C31 1.388(5) . ? C30 H30 0.9300 . ? C31 C32 1.388(5) . ? C31 H31 0.9300 . ? C32 C33 1.387(5) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? N1 N2 1.409(3) . ? N1 Ni1 1.854(2) . ? O1 Ni1 1.820(2) . ? O2 Ni1 1.844(2) . ? P1 Ni1 2.2264(8) . ? 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 O1 C1 C6 124.2(3) . . ? O1 C1 C2 117.2(3) . . ? C6 C1 C2 118.6(3) . . ? C3 C2 C1 120.7(3) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 121.1(3) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 118.4(3) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C4 C5 C6 121.9(3) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C1 C6 C5 119.3(3) . . ? C1 C6 C7 122.3(3) . . ? C5 C6 C7 118.5(3) . . ? N1 C7 C6 123.5(3) . . ? N1 C7 H7 118.3 . . ? C6 C7 H7 118.3 . . ? O2 C8 N2 123.7(3) . . ? O2 C8 C9 117.5(2) . . ? N2 C8 C9 118.8(3) . . ? C14 C9 C10 118.9(3) . . ? C14 C9 C8 120.0(3) . . ? C10 C9 C8 121.2(3) . . ? C11 C10 C9 120.4(3) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 120.9(3) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C13 C12 C11 118.0(3) . . ? C13 C12 C15 122.0(3) . . ? C11 C12 C15 120.0(3) . . ? C14 C13 C12 121.9(3) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C9 119.9(3) . . ? C13 C14 H14 120.0 . . ? C9 C14 H14 120.0 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 119.0(3) . . ? C21 C16 P1 123.7(2) . . ? C17 C16 P1 117.3(2) . . ? C18 C17 C16 120.3(3) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C19 C18 C17 120.6(3) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 119.7(3) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? C21 C20 C19 120.3(3) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C16 120.1(3) . . ? C20 C21 H21 119.9 . . ? C16 C21 H21 119.9 . . ? C27 C22 C23 119.2(3) . . ? C27 C22 P1 122.0(2) . . ? C23 C22 P1 118.7(2) . . ? C24 C23 C22 120.5(3) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C23 119.8(3) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C26 C25 C24 120.1(3) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 120.1(3) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C22 C27 C26 120.3(3) . . ? C22 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C29 C28 C33 118.3(3) . . ? C29 C28 P1 119.2(2) . . ? C33 C28 P1 122.2(2) . . ? C30 C29 C28 121.4(3) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C29 C30 C31 119.7(3) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C32 C31 C30 119.9(3) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C33 C32 C31 120.6(3) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C28 120.2(3) . . ? C32 C33 H33 119.9 . . ? C28 C33 H33 119.9 . . ? C7 N1 N2 117.5(2) . . ? C7 N1 Ni1 127.2(2) . . ? N2 N1 Ni1 115.20(17) . . ? C8 N2 N1 106.8(2) . . ? C1 O1 Ni1 126.4(2) . . ? C8 O2 Ni1 110.80(17) . . ? C16 P1 C28 105.85(13) . . ? C16 P1 C22 108.13(13) . . ? C28 P1 C22 103.44(13) . . ? C16 P1 Ni1 115.97(10) . . ? C28 P1 Ni1 111.60(9) . . ? C22 P1 Ni1 110.99(10) . . ? O1 Ni1 O2 174.47(9) . . ? O1 Ni1 N1 95.71(10) . . ? O2 Ni1 N1 83.48(9) . . ? O1 Ni1 P1 86.93(7) . . ? O2 Ni1 P1 94.33(7) . . ? N1 Ni1 P1 174.75(7) . . ? 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 O1 C1 C2 C3 178.2(3) . . . . ? C6 C1 C2 C3 -1.1(5) . . . . ? C1 C2 C3 C4 0.4(5) . . . . ? C2 C3 C4 C5 0.4(5) . . . . ? C3 C4 C5 C6 -0.4(5) . . . . ? O1 C1 C6 C5 -178.2(3) . . . . ? C2 C1 C6 C5 1.0(4) . . . . ? O1 C1 C6 C7 2.5(5) . . . . ? C2 C1 C6 C7 -178.3(3) . . . . ? C4 C5 C6 C1 -0.3(5) . . . . ? C4 C5 C6 C7 179.1(3) . . . . ? C1 C6 C7 N1 -1.5(5) . . . . ? C5 C6 C7 N1 179.2(3) . . . . ? O2 C8 C9 C14 -7.3(4) . . . . ? N2 C8 C9 C14 174.4(3) . . . . ? O2 C8 C9 C10 172.7(3) . . . . ? N2 C8 C9 C10 -5.6(4) . . . . ? C14 C9 C10 C11 1.3(4) . . . . ? C8 C9 C10 C11 -178.7(3) . . . . ? C9 C10 C11 C12 -0.4(5) . . . . ? C10 C11 C12 C13 -0.1(5) . . . . ? C10 C11 C12 C15 -179.7(3) . . . . ? C11 C12 C13 C14 -0.1(5) . . . . ? C15 C12 C13 C14 179.5(3) . . . . ? C12 C13 C14 C9 1.0(5) . . . . ? C10 C9 C14 C13 -1.5(4) . . . . ? C8 C9 C14 C13 178.5(3) . . . . ? C21 C16 C17 C18 -1.3(4) . . . . ? P1 C16 C17 C18 178.4(2) . . . . ? C16 C17 C18 C19 1.1(5) . . . . ? C17 C18 C19 C20 0.2(5) . . . . ? C18 C19 C20 C21 -1.3(5) . . . . ? C19 C20 C21 C16 1.1(5) . . . . ? C17 C16 C21 C20 0.2(4) . . . . ? P1 C16 C21 C20 -179.5(2) . . . . ? C27 C22 C23 C24 -0.3(4) . . . . ? P1 C22 C23 C24 -178.6(2) . . . . ? C22 C23 C24 C25 -0.3(4) . . . . ? C23 C24 C25 C26 0.6(4) . . . . ? C24 C25 C26 C27 -0.3(4) . . . . ? C23 C22 C27 C26 0.5(4) . . . . ? P1 C22 C27 C26 178.8(2) . . . . ? C25 C26 C27 C22 -0.2(4) . . . . ? C33 C28 C29 C30 0.5(5) . . . . ? P1 C28 C29 C30 -173.4(2) . . . . ? C28 C29 C30 C31 0.5(5) . . . . ? C29 C30 C31 C32 -1.3(5) . . . . ? C30 C31 C32 C33 1.0(6) . . . . ? C31 C32 C33 C28 0.0(6) . . . . ? C29 C28 C33 C32 -0.7(5) . . . . ? P1 C28 C33 C32 172.9(3) . . . . ? C6 C7 N1 N2 178.8(2) . . . . ? C6 C7 N1 Ni1 -5.9(4) . . . . ? O2 C8 N2 N1 0.0(4) . . . . ? C9 C8 N2 N1 178.2(2) . . . . ? C7 N1 N2 C8 176.5(3) . . . . ? Ni1 N1 N2 C8 0.7(3) . . . . ? C6 C1 O1 Ni1 4.0(4) . . . . ? C2 C1 O1 Ni1 -175.2(2) . . . . ? N2 C8 O2 Ni1 -0.6(4) . . . . ? C9 C8 O2 Ni1 -178.85(19) . . . . ? C21 C16 P1 C28 97.7(3) . . . . ? C17 C16 P1 C28 -82.0(2) . . . . ? C21 C16 P1 C22 -12.6(3) . . . . ? C17 C16 P1 C22 167.7(2) . . . . ? C21 C16 P1 Ni1 -138.0(2) . . . . ? C17 C16 P1 Ni1 42.4(3) . . . . ? C29 C28 P1 C16 -166.7(2) . . . . ? C33 C28 P1 C16 19.7(3) . . . . ? C29 C28 P1 C22 -53.1(3) . . . . ? C33 C28 P1 C22 133.3(3) . . . . ? C29 C28 P1 Ni1 66.3(2) . . . . ? C33 C28 P1 Ni1 -107.3(2) . . . . ? C27 C22 P1 C16 71.2(3) . . . . ? C23 C22 P1 C16 -110.6(2) . . . . ? C27 C22 P1 C28 -40.8(3) . . . . ? C23 C22 P1 C28 137.5(2) . . . . ? C27 C22 P1 Ni1 -160.6(2) . . . . ? C23 C22 P1 Ni1 17.7(2) . . . . ? C1 O1 Ni1 N1 -8.3(3) . . . . ? C1 O1 Ni1 P1 167.2(2) . . . . ? C8 O2 Ni1 N1 0.77(19) . . . . ? C8 O2 Ni1 P1 -174.44(18) . . . . ? C7 N1 Ni1 O1 9.3(3) . . . . ? N2 N1 Ni1 O1 -175.32(18) . . . . ? C7 N1 Ni1 O2 -176.2(3) . . . . ? N2 N1 Ni1 O2 -0.83(18) . . . . ? C16 P1 Ni1 O1 -175.61(12) . . . . ? C28 P1 Ni1 O1 -54.31(12) . . . . ? C22 P1 Ni1 O1 60.51(12) . . . . ? C16 P1 Ni1 O2 9.79(12) . . . . ? C28 P1 Ni1 O2 131.09(12) . . . . ? C22 P1 Ni1 O2 -114.09(12) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.016 _refine_diff_density_min -0.616 _refine_diff_density_rms 0.079 data_ndb _database_code_depnum_ccdc_archive 'CCDC 822887' #TrackingRef 'niohnb.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H27 N2 Ni O2 P' _chemical_formula_weight 609.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.778(2) _cell_length_b 8.8459(14) _cell_length_c 20.488(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.896(9) _cell_angle_gamma 90.00 _cell_volume 2825.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 943 _cell_measurement_theta_min 3.30 _cell_measurement_theta_max 60.73 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 1.819 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8681 _exptl_absorpt_correction_T_max 0.9474 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER GADDS D8 Discover' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16630 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 59.99 _reflns_number_total 4125 _reflns_number_gt 3037 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'FRAMBO (BRUKER-NONIUS, 2003)' _computing_cell_refinement ; CELL-NOW (Sheldrick, 2003) and SAINT (BRUKER-NONIUS, 2003) ; _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'X-SEED (Barbour, 2001)' _computing_publication_material 'Bruker SHELXTL' _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 [0.00000+1.00000exp(1.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0529P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _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 4125 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0960 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.000 _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 C24 C 0.45423(19) 0.7211(3) 0.26999(15) 0.0223(7) Uani 1 1 d . . . H24A H 0.4078 0.7325 0.2348 0.027 Uiso 1 1 calc R . . C19 C 0.50377(17) 0.5897(3) 0.27449(14) 0.0189(6) Uani 1 1 d . . . C9 C 0.56209(19) 1.0088(3) -0.12102(14) 0.0222(7) Uani 1 1 d . . . H9A H 0.5343 1.0379 -0.1636 0.027 Uiso 1 1 calc R . . C15 C 0.09473(19) 0.2845(3) -0.06802(15) 0.0278(7) Uani 1 1 d . . . H15A H 0.0659 0.2898 -0.1123 0.033 Uiso 1 1 calc R . . C23 C 0.4723(2) 0.8351(3) 0.31648(15) 0.0280(7) Uani 1 1 d . . . H23A H 0.4376 0.9233 0.3136 0.034 Uiso 1 1 calc R . . C33 C 0.63966(19) 0.0828(3) 0.25130(15) 0.0256(7) Uani 1 1 d . . . H33A H 0.6414 -0.0129 0.2725 0.031 Uiso 1 1 calc R . . C14 C 0.16939(18) 0.3675(3) -0.04915(15) 0.0238(7) Uani 1 1 d . . . H14A H 0.1917 0.4283 -0.0807 0.029 Uiso 1 1 calc R . . C20 C 0.57265(18) 0.5759(3) 0.32560(14) 0.0219(7) Uani 1 1 d . . . H20A H 0.6072 0.4874 0.3289 0.026 Uiso 1 1 calc R . . C21 C 0.5910(2) 0.6909(4) 0.37162(15) 0.0296(8) Uani 1 1 d . . . H21A H 0.6380 0.6809 0.4064 0.036 Uiso 1 1 calc R . . C32 C 0.56891(18) 0.1753(3) 0.25079(14) 0.0208(6) Uani 1 1 d . . . H32A H 0.5222 0.1423 0.2714 0.025 Uiso 1 1 calc R . . C34 C 0.70809(19) 0.1286(3) 0.22112(15) 0.0272(7) Uani 1 1 d . . . H34A H 0.7565 0.0646 0.2215 0.033 Uiso 1 1 calc R . . C25 C 0.39609(17) 0.3273(3) 0.25460(14) 0.0182(6) Uani 1 1 d . . . C4 C 0.64210(18) 0.9270(3) 0.00487(14) 0.0199(6) Uani 1 1 d . . . C28 C 0.28797(18) 0.1377(3) 0.31280(15) 0.0263(7) Uani 1 1 d . . . H28A H 0.2515 0.0726 0.3327 0.032 Uiso 1 1 calc R . . C11 C 0.44293(18) 0.6842(3) -0.00594(14) 0.0187(6) Uani 1 1 d . . . H11A H 0.4182 0.7067 -0.0501 0.022 Uiso 1 1 calc R . . C8 C 0.64206(19) 1.0706(3) -0.09579(15) 0.0247(7) Uani 1 1 d . . . H8A H 0.6690 1.1403 -0.1213 0.030 Uiso 1 1 calc R . . C3 C 0.68055(18) 0.8904(3) 0.07018(15) 0.0226(7) Uani 1 1 d . . . H3A H 0.7344 0.9341 0.0874 0.027 Uiso 1 1 calc R . . C10 C 0.52334(18) 0.9063(3) -0.08464(14) 0.0195(6) Uani 1 1 d . . . H10A H 0.4691 0.8655 -0.1029 0.023 Uiso 1 1 calc R . . C16 C 0.06226(19) 0.1943(3) -0.02263(16) 0.0273(7) Uani 1 1 d . . . H16A H 0.0116 0.1369 -0.0357 0.033 Uiso 1 1 calc R . . C22 C 0.5408(2) 0.8205(3) 0.36700(16) 0.0301(7) Uani 1 1 d . . . H22A H 0.5536 0.8992 0.3986 0.036 Uiso 1 1 calc R . . C35 C 0.70534(18) 0.2690(3) 0.19032(15) 0.0250(7) Uani 1 1 d . . . H35A H 0.7522 0.3013 0.1697 0.030 Uiso 1 1 calc R . . C1 C 0.56275(18) 0.7246(3) 0.08420(14) 0.0194(6) Uani 1 1 d . . . C7 C 0.68118(18) 1.0296(3) -0.03405(15) 0.0227(7) Uani 1 1 d . . . H7A H 0.7357 1.0710 -0.0170 0.027 Uiso 1 1 calc R . . C30 C 0.39246(18) 0.3376(3) 0.32181(14) 0.0227(7) Uani 1 1 d . . . H30A H 0.4269 0.4099 0.3480 0.027 Uiso 1 1 calc R . . C36 C 0.63455(17) 0.3620(3) 0.18958(14) 0.0214(7) Uani 1 1 d . . . H36A H 0.6328 0.4573 0.1681 0.026 Uiso 1 1 calc R . . C18 C 0.17765(18) 0.2724(3) 0.06099(14) 0.0215(7) Uani 1 1 d . . . H18A H 0.2053 0.2691 0.1056 0.026 Uiso 1 1 calc R . . C2 C 0.64307(18) 0.7953(3) 0.10871(15) 0.0223(7) Uani 1 1 d . . . H2A H 0.6703 0.7752 0.1525 0.027 Uiso 1 1 calc R . . C12 C 0.29271(17) 0.4458(3) 0.03620(13) 0.0163(6) Uani 1 1 d . . . C29 C 0.33869(19) 0.2428(3) 0.35090(16) 0.0266(7) Uani 1 1 d . . . H29A H 0.3367 0.2500 0.3969 0.032 Uiso 1 1 calc R . . C26 C 0.34394(17) 0.2225(3) 0.21634(15) 0.0203(6) Uani 1 1 d . . . H26A H 0.3449 0.2160 0.1702 0.024 Uiso 1 1 calc R . . C27 C 0.29057(18) 0.1276(3) 0.24581(16) 0.0264(7) Uani 1 1 d . . . H27A H 0.2557 0.0555 0.2198 0.032 Uiso 1 1 calc R . . C13 C 0.21139(17) 0.3619(3) 0.01533(14) 0.0181(6) Uani 1 1 d . . . C17 C 0.10381(19) 0.1881(3) 0.04170(15) 0.0256(7) Uani 1 1 d . . . H17A H 0.0818 0.1258 0.0730 0.031 Uiso 1 1 calc R . . C6 C 0.52229(18) 0.7544(3) 0.01954(14) 0.0175(6) Uani 1 1 d . . . C31 C 0.56560(17) 0.3163(3) 0.22031(13) 0.0174(6) Uani 1 1 d . . . C5 C 0.56184(17) 0.8600(3) -0.02104(14) 0.0175(6) Uani 1 1 d . . . N2 N 0.32352(14) 0.5331(2) -0.00539(11) 0.0197(5) Uani 1 1 d . . . N1 N 0.40177(14) 0.5910(2) 0.02727(11) 0.0175(5) Uani 1 1 d . . . O1 O 0.53154(12) 0.6366(2) 0.12664(9) 0.0210(5) Uani 1 1 d . . . O2 O 0.33106(12) 0.4235(2) 0.09732(9) 0.0189(4) Uani 1 1 d . . . Ni1 Ni 0.43290(3) 0.52755(5) 0.11278(2) 0.01764(15) Uani 1 1 d . . . P1 P 0.47150(4) 0.43914(8) 0.21528(4) 0.01725(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C24 0.0259(16) 0.0198(15) 0.0215(17) 0.0038(12) 0.0048(12) -0.0042(13) C19 0.0191(14) 0.0193(14) 0.0194(16) 0.0038(12) 0.0068(11) -0.0023(12) C9 0.0277(16) 0.0203(15) 0.0198(16) -0.0021(12) 0.0076(13) 0.0019(13) C15 0.0263(16) 0.0337(17) 0.0208(18) 0.0019(14) -0.0043(13) -0.0059(15) C23 0.0371(18) 0.0168(15) 0.0323(19) 0.0002(13) 0.0126(15) -0.0011(14) C33 0.0304(17) 0.0221(15) 0.0240(18) 0.0031(13) 0.0033(13) 0.0045(14) C14 0.0244(16) 0.0265(16) 0.0203(17) 0.0034(13) 0.0032(12) -0.0025(14) C20 0.0182(15) 0.0245(15) 0.0238(17) -0.0008(13) 0.0058(12) 0.0006(13) C21 0.0267(17) 0.0389(19) 0.0231(18) -0.0054(14) 0.0038(13) -0.0086(15) C32 0.0219(15) 0.0229(15) 0.0182(16) 0.0001(12) 0.0044(12) 0.0004(13) C34 0.0217(16) 0.0298(17) 0.0297(18) -0.0032(14) 0.0031(13) 0.0073(14) C25 0.0179(14) 0.0155(14) 0.0209(17) 0.0024(12) 0.0019(12) 0.0055(12) C4 0.0197(15) 0.0156(14) 0.0260(17) -0.0028(12) 0.0080(12) 0.0033(12) C28 0.0194(15) 0.0272(17) 0.034(2) 0.0062(14) 0.0104(13) -0.0005(14) C11 0.0208(15) 0.0173(14) 0.0187(16) -0.0043(12) 0.0053(12) 0.0046(13) C8 0.0283(16) 0.0185(15) 0.0304(18) -0.0015(13) 0.0147(13) -0.0013(13) C3 0.0191(15) 0.0199(15) 0.0290(18) -0.0009(13) 0.0047(12) -0.0043(13) C10 0.0236(15) 0.0158(14) 0.0198(16) -0.0035(12) 0.0056(12) 0.0007(13) C16 0.0235(16) 0.0272(16) 0.0297(19) -0.0009(14) -0.0003(13) -0.0074(14) C22 0.0360(18) 0.0272(17) 0.0291(19) -0.0091(14) 0.0114(14) -0.0103(15) C35 0.0203(15) 0.0278(17) 0.0279(18) -0.0040(13) 0.0073(13) -0.0006(14) C1 0.0204(15) 0.0150(14) 0.0238(17) -0.0011(12) 0.0061(12) 0.0022(13) C7 0.0189(15) 0.0205(15) 0.0303(18) -0.0032(13) 0.0084(13) -0.0025(13) C30 0.0221(15) 0.0246(16) 0.0223(17) 0.0005(13) 0.0058(12) 0.0007(13) C36 0.0190(15) 0.0234(15) 0.0216(16) 0.0018(12) 0.0023(12) -0.0003(13) C18 0.0207(15) 0.0284(16) 0.0151(16) 0.0008(12) 0.0021(12) 0.0006(13) C2 0.0235(16) 0.0202(15) 0.0216(17) -0.0014(12) -0.0013(13) 0.0000(13) C12 0.0177(14) 0.0170(14) 0.0138(15) -0.0026(11) 0.0013(11) 0.0050(12) C29 0.0270(16) 0.0327(17) 0.0226(17) 0.0057(14) 0.0115(13) 0.0065(15) C26 0.0204(15) 0.0192(15) 0.0216(16) 0.0011(12) 0.0036(12) 0.0009(13) C27 0.0218(16) 0.0226(16) 0.034(2) 0.0059(13) 0.0005(13) -0.0048(14) C13 0.0176(14) 0.0159(14) 0.0207(16) -0.0008(12) 0.0031(12) 0.0024(12) C17 0.0284(17) 0.0247(16) 0.0247(18) 0.0017(13) 0.0074(13) -0.0011(14) C6 0.0217(14) 0.0145(14) 0.0171(16) -0.0033(11) 0.0057(11) 0.0033(12) C31 0.0194(15) 0.0208(15) 0.0114(15) -0.0029(11) 0.0003(11) 0.0008(12) C5 0.0209(15) 0.0141(13) 0.0187(16) -0.0029(11) 0.0075(12) 0.0029(12) N2 0.0193(12) 0.0205(12) 0.0184(13) -0.0010(10) 0.0004(10) -0.0031(11) N1 0.0139(11) 0.0162(11) 0.0219(14) -0.0009(10) 0.0014(10) 0.0007(10) O1 0.0226(10) 0.0227(10) 0.0174(11) 0.0028(8) 0.0021(8) -0.0023(9) O2 0.0196(10) 0.0218(10) 0.0160(11) -0.0006(8) 0.0042(8) 0.0008(9) Ni1 0.0183(3) 0.0188(3) 0.0156(3) 0.00027(19) 0.00202(19) -0.0008(2) P1 0.0172(4) 0.0180(4) 0.0165(4) 0.0002(3) 0.0025(3) -0.0002(3) _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 C24 C23 1.386(4) . ? C24 C19 1.396(4) . ? C24 H24A 0.9500 . ? C19 C20 1.393(4) . ? C19 P1 1.820(3) . ? C9 C10 1.376(4) . ? C9 C8 1.399(4) . ? C9 H9A 0.9500 . ? C15 C16 1.382(4) . ? C15 C14 1.391(4) . ? C15 H15A 0.9500 . ? C23 C22 1.382(4) . ? C23 H23A 0.9500 . ? C33 C32 1.383(4) . ? C33 C34 1.385(4) . ? C33 H33A 0.9500 . ? C14 C13 1.384(4) . ? C14 H14A 0.9500 . ? C20 C21 1.387(4) . ? C20 H20A 0.9500 . ? C21 C22 1.388(5) . ? C21 H21A 0.9500 . ? C32 C31 1.393(4) . ? C32 H32A 0.9500 . ? C34 C35 1.391(4) . ? C34 H34A 0.9500 . ? C25 C30 1.390(4) . ? C25 C26 1.397(4) . ? C25 P1 1.828(3) . ? C4 C7 1.411(4) . ? C4 C3 1.419(4) . ? C4 C5 1.424(4) . ? C28 C27 1.382(4) . ? C28 C29 1.386(4) . ? C28 H28A 0.9500 . ? C11 N1 1.304(4) . ? C11 C6 1.423(4) . ? C11 H11A 0.9500 . ? C8 C7 1.368(4) . ? C8 H8A 0.9500 . ? C3 C2 1.351(4) . ? C3 H3A 0.9500 . ? C10 C5 1.411(4) . ? C10 H10A 0.9500 . ? C16 C17 1.379(4) . ? C16 H16A 0.9500 . ? C22 H22A 0.9500 . ? C35 C36 1.385(4) . ? C35 H35A 0.9500 . ? C1 O1 1.318(3) . ? C1 C6 1.404(4) . ? C1 C2 1.433(4) . ? C7 H7A 0.9500 . ? C30 C29 1.391(4) . ? C30 H30A 0.9500 . ? C36 C31 1.398(4) . ? C36 H36A 0.9500 . ? C18 C17 1.389(4) . ? C18 C13 1.392(4) . ? C18 H18A 0.9500 . ? C2 H2A 0.9500 . ? C12 N2 1.299(4) . ? C12 O2 1.319(3) . ? C12 C13 1.487(4) . ? C29 H29A 0.9500 . ? C26 C27 1.391(4) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C17 H17A 0.9500 . ? C6 C5 1.454(4) . ? C31 P1 1.830(3) . ? N2 N1 1.407(3) . ? N1 Ni1 1.833(2) . ? O1 Ni1 1.8157(19) . ? O2 Ni1 1.8365(19) . ? Ni1 P1 2.2354(9) . ? 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 C23 C24 C19 120.5(3) . . ? C23 C24 H24A 119.8 . . ? C19 C24 H24A 119.8 . . ? C20 C19 C24 119.1(3) . . ? C20 C19 P1 122.8(2) . . ? C24 C19 P1 118.0(2) . . ? C10 C9 C8 120.6(3) . . ? C10 C9 H9A 119.7 . . ? C8 C9 H9A 119.7 . . ? C16 C15 C14 120.2(3) . . ? C16 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? C22 C23 C24 120.0(3) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C32 C33 C34 120.5(3) . . ? C32 C33 H33A 119.7 . . ? C34 C33 H33A 119.7 . . ? C13 C14 C15 120.4(3) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C21 C20 C19 120.2(3) . . ? C21 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? C20 C21 C22 120.2(3) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C33 C32 C31 120.5(3) . . ? C33 C32 H32A 119.7 . . ? C31 C32 H32A 119.7 . . ? C33 C34 C35 119.5(3) . . ? C33 C34 H34A 120.3 . . ? C35 C34 H34A 120.3 . . ? C30 C25 C26 119.3(3) . . ? C30 C25 P1 122.0(2) . . ? C26 C25 P1 118.6(2) . . ? C7 C4 C3 121.3(3) . . ? C7 C4 C5 119.9(3) . . ? C3 C4 C5 118.8(3) . . ? C27 C28 C29 119.9(3) . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? N1 C11 C6 124.4(3) . . ? N1 C11 H11A 117.8 . . ? C6 C11 H11A 117.8 . . ? C7 C8 C9 119.4(3) . . ? C7 C8 H8A 120.3 . . ? C9 C8 H8A 120.3 . . ? C2 C3 C4 122.1(3) . . ? C2 C3 H3A 118.9 . . ? C4 C3 H3A 118.9 . . ? C9 C10 C5 121.9(3) . . ? C9 C10 H10A 119.1 . . ? C5 C10 H10A 119.1 . . ? C17 C16 C15 119.7(3) . . ? C17 C16 H16A 120.2 . . ? C15 C16 H16A 120.2 . . ? C23 C22 C21 120.0(3) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C36 C35 C34 120.2(3) . . ? C36 C35 H35A 119.9 . . ? C34 C35 H35A 119.9 . . ? O1 C1 C6 124.9(3) . . ? O1 C1 C2 115.3(3) . . ? C6 C1 C2 119.8(3) . . ? C8 C7 C4 121.3(3) . . ? C8 C7 H7A 119.4 . . ? C4 C7 H7A 119.4 . . ? C25 C30 C29 120.4(3) . . ? C25 C30 H30A 119.8 . . ? C29 C30 H30A 119.8 . . ? C35 C36 C31 120.4(3) . . ? C35 C36 H36A 119.8 . . ? C31 C36 H36A 119.8 . . ? C17 C18 C13 120.4(3) . . ? C17 C18 H18A 119.8 . . ? C13 C18 H18A 119.8 . . ? C3 C2 C1 120.7(3) . . ? C3 C2 H2A 119.7 . . ? C1 C2 H2A 119.7 . . ? N2 C12 O2 123.3(2) . . ? N2 C12 C13 120.1(2) . . ? O2 C12 C13 116.6(2) . . ? C28 C29 C30 120.0(3) . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C27 C26 C25 120.0(3) . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C28 C27 C26 120.3(3) . . ? C28 C27 H27A 119.8 . . ? C26 C27 H27A 119.8 . . ? C14 C13 C18 119.0(3) . . ? C14 C13 C12 121.4(3) . . ? C18 C13 C12 119.5(2) . . ? C16 C17 C18 120.3(3) . . ? C16 C17 H17A 119.9 . . ? C18 C17 H17A 119.9 . . ? C1 C6 C11 120.7(3) . . ? C1 C6 C5 119.2(2) . . ? C11 C6 C5 120.1(3) . . ? C32 C31 C36 118.9(3) . . ? C32 C31 P1 122.1(2) . . ? C36 C31 P1 119.0(2) . . ? C10 C5 C4 117.0(3) . . ? C10 C5 C6 123.6(3) . . ? C4 C5 C6 119.3(3) . . ? C12 N2 N1 107.1(2) . . ? C11 N1 N2 116.9(2) . . ? C11 N1 Ni1 127.65(19) . . ? N2 N1 Ni1 115.41(17) . . ? C1 O1 Ni1 127.53(18) . . ? C12 O2 Ni1 110.46(17) . . ? O1 Ni1 N1 94.78(9) . . ? O1 Ni1 O2 177.87(9) . . ? N1 Ni1 O2 83.72(9) . . ? O1 Ni1 P1 86.36(6) . . ? N1 Ni1 P1 177.30(8) . . ? O2 Ni1 P1 95.20(6) . . ? C19 P1 C25 103.67(13) . . ? C19 P1 C31 104.83(12) . . ? C25 P1 C31 103.39(13) . . ? C19 P1 Ni1 112.19(9) . . ? C25 P1 Ni1 120.14(9) . . ? C31 P1 Ni1 111.19(9) . . ? 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 C23 C24 C19 C20 -1.3(4) . . . . ? C23 C24 C19 P1 175.6(2) . . . . ? C19 C24 C23 C22 1.3(5) . . . . ? C16 C15 C14 C13 -0.7(5) . . . . ? C24 C19 C20 C21 0.6(4) . . . . ? P1 C19 C20 C21 -176.0(2) . . . . ? C19 C20 C21 C22 -0.1(5) . . . . ? C34 C33 C32 C31 -0.4(4) . . . . ? C32 C33 C34 C35 0.2(4) . . . . ? C10 C9 C8 C7 -0.8(4) . . . . ? C7 C4 C3 C2 178.3(3) . . . . ? C5 C4 C3 C2 -0.7(4) . . . . ? C8 C9 C10 C5 0.3(4) . . . . ? C14 C15 C16 C17 0.6(5) . . . . ? C24 C23 C22 C21 -0.7(5) . . . . ? C20 C21 C22 C23 0.1(5) . . . . ? C33 C34 C35 C36 -0.3(4) . . . . ? C9 C8 C7 C4 -0.5(4) . . . . ? C3 C4 C7 C8 -176.7(3) . . . . ? C5 C4 C7 C8 2.3(4) . . . . ? C26 C25 C30 C29 1.2(4) . . . . ? P1 C25 C30 C29 -175.3(2) . . . . ? C34 C35 C36 C31 0.6(4) . . . . ? C4 C3 C2 C1 1.3(4) . . . . ? O1 C1 C2 C3 -178.7(3) . . . . ? C6 C1 C2 C3 -0.2(4) . . . . ? C27 C28 C29 C30 -0.3(4) . . . . ? C25 C30 C29 C28 -0.3(4) . . . . ? C30 C25 C26 C27 -1.4(4) . . . . ? P1 C25 C26 C27 175.1(2) . . . . ? C29 C28 C27 C26 0.0(4) . . . . ? C25 C26 C27 C28 0.8(4) . . . . ? C15 C14 C13 C18 -0.2(4) . . . . ? C15 C14 C13 C12 178.1(3) . . . . ? C17 C18 C13 C14 1.1(4) . . . . ? C17 C18 C13 C12 -177.2(3) . . . . ? N2 C12 C13 C14 3.8(4) . . . . ? O2 C12 C13 C14 -174.8(2) . . . . ? N2 C12 C13 C18 -178.0(2) . . . . ? O2 C12 C13 C18 3.5(4) . . . . ? C15 C16 C17 C18 0.3(5) . . . . ? C13 C18 C17 C16 -1.2(4) . . . . ? O1 C1 C6 C11 -2.2(4) . . . . ? C2 C1 C6 C11 179.4(2) . . . . ? O1 C1 C6 C5 176.9(2) . . . . ? C2 C1 C6 C5 -1.5(4) . . . . ? N1 C11 C6 C1 0.8(4) . . . . ? N1 C11 C6 C5 -178.3(2) . . . . ? C33 C32 C31 C36 0.8(4) . . . . ? C33 C32 C31 P1 177.3(2) . . . . ? C35 C36 C31 C32 -0.9(4) . . . . ? C35 C36 C31 P1 -177.5(2) . . . . ? C9 C10 C5 C4 1.5(4) . . . . ? C9 C10 C5 C6 178.7(3) . . . . ? C7 C4 C5 C10 -2.7(4) . . . . ? C3 C4 C5 C10 176.3(3) . . . . ? C7 C4 C5 C6 180.0(2) . . . . ? C3 C4 C5 C6 -1.0(4) . . . . ? C1 C6 C5 C10 -175.1(3) . . . . ? C11 C6 C5 C10 4.1(4) . . . . ? C1 C6 C5 C4 2.1(4) . . . . ? C11 C6 C5 C4 -178.8(2) . . . . ? O2 C12 N2 N1 1.0(3) . . . . ? C13 C12 N2 N1 -177.5(2) . . . . ? C6 C11 N1 N2 179.3(2) . . . . ? C6 C11 N1 Ni1 0.4(4) . . . . ? C12 N2 N1 C11 -179.0(2) . . . . ? C12 N2 N1 Ni1 0.1(3) . . . . ? C6 C1 O1 Ni1 2.4(4) . . . . ? C2 C1 O1 Ni1 -179.10(18) . . . . ? N2 C12 O2 Ni1 -1.6(3) . . . . ? C13 C12 O2 Ni1 176.90(18) . . . . ? C1 O1 Ni1 N1 -1.1(2) . . . . ? C1 O1 Ni1 O2 -46(3) . . . . ? C1 O1 Ni1 P1 176.4(2) . . . . ? C11 N1 Ni1 O1 -0.3(2) . . . . ? N2 N1 Ni1 O1 -179.23(17) . . . . ? C11 N1 Ni1 O2 178.2(2) . . . . ? N2 N1 Ni1 O2 -0.75(17) . . . . ? C11 N1 Ni1 P1 -115.2(16) . . . . ? N2 N1 Ni1 P1 65.9(17) . . . . ? C12 O2 Ni1 O1 47(3) . . . . ? C12 O2 Ni1 N1 1.19(17) . . . . ? C12 O2 Ni1 P1 -176.33(16) . . . . ? C20 C19 P1 C25 88.5(3) . . . . ? C24 C19 P1 C25 -88.2(2) . . . . ? C20 C19 P1 C31 -19.6(3) . . . . ? C24 C19 P1 C31 163.7(2) . . . . ? C20 C19 P1 Ni1 -140.4(2) . . . . ? C24 C19 P1 Ni1 42.9(2) . . . . ? C30 C25 P1 C19 -17.9(3) . . . . ? C26 C25 P1 C19 165.6(2) . . . . ? C30 C25 P1 C31 91.2(2) . . . . ? C26 C25 P1 C31 -85.2(2) . . . . ? C30 C25 P1 Ni1 -144.2(2) . . . . ? C26 C25 P1 Ni1 39.4(2) . . . . ? C32 C31 P1 C19 106.6(2) . . . . ? C36 C31 P1 C19 -76.9(2) . . . . ? C32 C31 P1 C25 -1.8(3) . . . . ? C36 C31 P1 C25 174.8(2) . . . . ? C32 C31 P1 Ni1 -132.0(2) . . . . ? C36 C31 P1 Ni1 44.6(2) . . . . ? O1 Ni1 P1 C19 48.39(11) . . . . ? N1 Ni1 P1 C19 163.5(16) . . . . ? O2 Ni1 P1 C19 -130.15(11) . . . . ? O1 Ni1 P1 C25 170.54(12) . . . . ? N1 Ni1 P1 C25 -74.4(16) . . . . ? O2 Ni1 P1 C25 -8.01(12) . . . . ? O1 Ni1 P1 C31 -68.64(11) . . . . ? N1 Ni1 P1 C31 46.4(16) . . . . ? O2 Ni1 P1 C31 112.82(11) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 59.99 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.494 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.063