data_12080_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H60 Cr N4 Ni1P3, 0.5(C4 H10 O)' _chemical_formula_sum 'C41 H65 Cr N4 Ni O0.5 P3' _chemical_formula_weight 825.62 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 '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' 'O' 'O' 0.0106 0.0060 '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 11.1205(16) _cell_length_b 14.167(2) _cell_length_c 14.256(2) _cell_angle_alpha 71.694(2) _cell_angle_beta 83.745(2) _cell_angle_gamma 81.854(2) _cell_volume 2105.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9577 _cell_measurement_theta_min 2.2625 _cell_measurement_theta_max 27.520 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.302 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.853 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7265 _exptl_absorpt_correction_T_max 0.7838 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_measurement_method 'area detector, omega scans per phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24583 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_sigmaI/netI 0.0771 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.52 _reflns_number_total 9577 _reflns_number_gt 6867 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL, Bruker' _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^)+(0.1128P)^2^+0.0000P] 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 9577 _refine_ls_number_parameters 490 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1835 _refine_ls_wR_factor_gt 0.1611 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 Ni1 Ni 0.28046(4) 0.17414(3) 0.16167(3) 0.02183(14) Uani 1 1 d . . . Cr1 Cr 0.19996(5) 0.26676(4) 0.27488(4) 0.02076(15) Uani 1 1 d . . . P1 P 0.19482(9) 0.30150(7) 0.04454(7) 0.0251(2) Uani 1 1 d . . . P2 P 0.46332(8) 0.18140(7) 0.20639(7) 0.0261(2) Uani 1 1 d . . . P3 P 0.17550(8) 0.04885(7) 0.25222(7) 0.0250(2) Uani 1 1 d . . . N1 N 0.1286(2) 0.3467(2) 0.3726(2) 0.0203(6) Uani 1 1 d . . . N2 N 0.1769(3) 0.3992(2) 0.1782(2) 0.0241(6) Uani 1 1 d . . . N3 N 0.3398(3) 0.2380(3) 0.3548(2) 0.0330(8) Uani 1 1 d . . . N4 N 0.0702(3) 0.1836(2) 0.3436(2) 0.0298(7) Uani 1 1 d . . . C1 C 0.1514(3) 0.4514(3) 0.3229(3) 0.0228(7) Uani 1 1 d . . . C2 C 0.1528(3) 0.5201(3) 0.3718(3) 0.0285(8) Uani 1 1 d . . . H2A H 0.1424 0.5008 0.4406 0.034 Uiso 1 1 calc R . . C3 C 0.1699(4) 0.6191(3) 0.3191(3) 0.0325(9) Uani 1 1 d . . . H3A H 0.1709 0.6660 0.3523 0.039 Uiso 1 1 calc R . . C4 C 0.1853(4) 0.6466(3) 0.2172(3) 0.0319(8) Uani 1 1 d . . . H4A H 0.1959 0.7125 0.1816 0.038 Uiso 1 1 calc R . . C5 C 0.1852(3) 0.5766(3) 0.1668(3) 0.0277(8) Uani 1 1 d . . . H5A H 0.1950 0.5967 0.0980 0.033 Uiso 1 1 calc R . . C6 C 0.1704(3) 0.4766(3) 0.2183(3) 0.0228(7) Uani 1 1 d . . . C7 C 0.1902(4) 0.4219(3) 0.0713(3) 0.0279(8) Uani 1 1 d . . . H7A H 0.2648 0.4520 0.0451 0.034 Uiso 1 1 calc R . . H7B H 0.1220 0.4682 0.0413 0.034 Uiso 1 1 calc R . . C8 C 0.0342(4) 0.3096(3) 0.0149(3) 0.0328(9) Uani 1 1 d . . . H8A H 0.0159 0.3740 -0.0356 0.039 Uiso 1 1 calc R . . C9 C -0.0530(4) 0.3092(3) 0.1053(3) 0.0419(10) Uani 1 1 d . . . H9A H -0.1355 0.3190 0.0870 0.063 Uiso 1 1 calc R . . H9B H -0.0395 0.3623 0.1300 0.063 Uiso 1 1 calc R . . H9C H -0.0391 0.2462 0.1559 0.063 Uiso 1 1 calc R . . C10 C 0.0149(5) 0.2279(3) -0.0288(4) 0.0487(12) Uani 1 1 d . . . H10A H -0.0686 0.2352 -0.0439 0.073 Uiso 1 1 calc R . . H10B H 0.0344 0.1634 0.0182 0.073 Uiso 1 1 calc R . . H10C H 0.0667 0.2336 -0.0883 0.073 Uiso 1 1 calc R . . C11 C 0.2806(4) 0.3308(3) -0.0789(3) 0.0368(9) Uani 1 1 d . . . H11A H 0.3531 0.3591 -0.0713 0.044 Uiso 1 1 calc R . . C12 C 0.2134(5) 0.4112(3) -0.1625(3) 0.0521(13) Uani 1 1 d . . . H12A H 0.2659 0.4254 -0.2221 0.078 Uiso 1 1 calc R . . H12B H 0.1910 0.4711 -0.1439 0.078 Uiso 1 1 calc R . . H12C H 0.1414 0.3871 -0.1736 0.078 Uiso 1 1 calc R . . C13 C 0.3277(5) 0.2362(3) -0.1073(3) 0.0499(12) Uani 1 1 d . . . H13A H 0.3793 0.2532 -0.1673 0.075 Uiso 1 1 calc R . . H13B H 0.2602 0.2060 -0.1174 0.075 Uiso 1 1 calc R . . H13C H 0.3734 0.1900 -0.0552 0.075 Uiso 1 1 calc R . . C14 C 0.1948(3) 0.2982(3) 0.4632(2) 0.0235(7) Uani 1 1 d . . . C15 C 0.1495(3) 0.3050(3) 0.5556(3) 0.0291(8) Uani 1 1 d . . . H15A H 0.0728 0.3387 0.5633 0.035 Uiso 1 1 calc R . . C16 C 0.2190(4) 0.2614(3) 0.6361(3) 0.0375(9) Uani 1 1 d . . . H16A H 0.1889 0.2650 0.6985 0.045 Uiso 1 1 calc R . . C17 C 0.3330(4) 0.2127(3) 0.6237(3) 0.0433(11) Uani 1 1 d . . . H17A H 0.3808 0.1860 0.6775 0.052 Uiso 1 1 calc R . . C18 C 0.3779(4) 0.2027(3) 0.5316(3) 0.0392(10) Uani 1 1 d . . . H18A H 0.4539 0.1673 0.5252 0.047 Uiso 1 1 calc R . . C19 C 0.3091(3) 0.2458(3) 0.4486(3) 0.0285(8) Uani 1 1 d . . . C20 C 0.4581(3) 0.1877(3) 0.3346(3) 0.0336(9) Uani 1 1 d . . . H20A H 0.4692 0.1208 0.3810 0.040 Uiso 1 1 calc R . . H20B H 0.5222 0.2246 0.3410 0.040 Uiso 1 1 calc R . . C21 C 0.5619(4) 0.2811(3) 0.1418(4) 0.0466(11) Uani 1 1 d . . . H21A H 0.6375 0.2653 0.1758 0.056 Uiso 1 1 calc R . . C22 C 0.5957(5) 0.2858(5) 0.0350(4) 0.0726(18) Uani 1 1 d . . . H22A H 0.6270 0.3481 0.0003 0.109 Uiso 1 1 calc R . . H22B H 0.5248 0.2809 0.0047 0.109 Uiso 1 1 calc R . . H22C H 0.6566 0.2313 0.0322 0.109 Uiso 1 1 calc R . . C23 C 0.5013(5) 0.3821(4) 0.1507(6) 0.077(2) Uani 1 1 d . . . H23A H 0.5537 0.4328 0.1183 0.116 Uiso 1 1 calc R . . H23B H 0.4869 0.3782 0.2194 0.116 Uiso 1 1 calc R . . H23C H 0.4252 0.3987 0.1200 0.116 Uiso 1 1 calc R . . C24 C 0.5673(3) 0.0641(3) 0.2143(3) 0.0334(9) Uani 1 1 d . . . H24A H 0.5337 0.0124 0.2704 0.040 Uiso 1 1 calc R . . C25 C 0.5621(5) 0.0296(4) 0.1228(4) 0.0532(13) Uani 1 1 d . . . H25A H 0.6155 -0.0313 0.1291 0.080 Uiso 1 1 calc R . . H25B H 0.5874 0.0804 0.0643 0.080 Uiso 1 1 calc R . . H25C H 0.4803 0.0181 0.1180 0.080 Uiso 1 1 calc R . . C26 C 0.6985(4) 0.0651(4) 0.2369(4) 0.0574(14) Uani 1 1 d . . . H26A H 0.7422 -0.0002 0.2456 0.086 Uiso 1 1 calc R . . H26B H 0.6982 0.0833 0.2963 0.086 Uiso 1 1 calc R . . H26C H 0.7373 0.1129 0.1828 0.086 Uiso 1 1 calc R . . C27 C -0.0010(3) 0.3319(3) 0.3862(2) 0.0226(7) Uani 1 1 d . . . C28 C -0.0916(3) 0.4013(3) 0.4073(3) 0.0270(8) Uani 1 1 d . . . H28A H -0.0719 0.4616 0.4110 0.032 Uiso 1 1 calc R . . C29 C -0.2123(3) 0.3808(3) 0.4229(3) 0.0343(9) Uani 1 1 d . . . H29A H -0.2740 0.4266 0.4377 0.041 Uiso 1 1 calc R . . C30 C -0.2380(3) 0.2909(3) 0.4160(3) 0.0349(9) Uani 1 1 d . . . H30A H -0.3183 0.2765 0.4270 0.042 Uiso 1 1 calc R . . C31 C -0.1483(3) 0.2214(3) 0.3933(3) 0.0325(9) Uani 1 1 d . . . H31A H -0.1690 0.1613 0.3899 0.039 Uiso 1 1 calc R . . C32 C -0.0265(3) 0.2413(3) 0.3755(3) 0.0246(7) Uani 1 1 d . . . C33 C 0.0443(3) 0.0942(3) 0.3247(3) 0.0302(8) Uani 1 1 d . . . H33A H -0.0282 0.1089 0.2881 0.036 Uiso 1 1 calc R . . H33B H 0.0294 0.0428 0.3869 0.036 Uiso 1 1 calc R . . C34 C 0.2390(4) -0.0609(3) 0.3519(3) 0.0348(9) Uani 1 1 d . . . H34A H 0.1713 -0.0989 0.3854 0.042 Uiso 1 1 calc R . . C35 C 0.2901(4) -0.0252(3) 0.4286(3) 0.0449(11) Uani 1 1 d . . . H35A H 0.3143 -0.0818 0.4837 0.067 Uiso 1 1 calc R . . H35B H 0.2286 0.0191 0.4513 0.067 Uiso 1 1 calc R . . H35C H 0.3593 0.0097 0.3990 0.067 Uiso 1 1 calc R . . C36 C 0.3335(4) -0.1316(3) 0.3132(4) 0.0443(11) Uani 1 1 d . . . H36A H 0.3694 -0.1824 0.3681 0.066 Uiso 1 1 calc R . . H36B H 0.3957 -0.0945 0.2720 0.066 Uiso 1 1 calc R . . H36C H 0.2947 -0.1625 0.2754 0.066 Uiso 1 1 calc R . . C37 C 0.0948(4) -0.0078(3) 0.1792(3) 0.0326(9) Uani 1 1 d . . . H37A H 0.0324 0.0452 0.1470 0.039 Uiso 1 1 calc R . . C38 C 0.0254(4) -0.0951(3) 0.2385(4) 0.0433(10) Uani 1 1 d . . . H38A H -0.0221 -0.1124 0.1953 0.065 Uiso 1 1 calc R . . H38B H -0.0275 -0.0764 0.2892 0.065 Uiso 1 1 calc R . . H38C H 0.0820 -0.1516 0.2686 0.065 Uiso 1 1 calc R . . C39 C 0.1782(4) -0.0315(3) 0.0935(3) 0.0447(11) Uani 1 1 d . . . H39A H 0.1313 -0.0541 0.0537 0.067 Uiso 1 1 calc R . . H39B H 0.2423 -0.0830 0.1202 0.067 Uiso 1 1 calc R . . H39C H 0.2128 0.0277 0.0534 0.067 Uiso 1 1 calc R . . C43 C -0.474(2) 0.4376(18) 0.6527(15) 0.095(7) Uani 0.50 1 d PD A -1 H43A H -0.4353 0.4482 0.7051 0.143 Uiso 0.50 1 calc PR A -1 H43B H -0.4358 0.3770 0.6404 0.143 Uiso 0.50 1 calc PR A -1 H43C H -0.5586 0.4323 0.6716 0.143 Uiso 0.50 1 calc PR A -1 C42 C -0.4596(12) 0.5272(12) 0.5572(12) 0.088(6) Uani 0.50 1 d PD A -1 H42A H -0.5127 0.5861 0.5626 0.105 Uiso 0.50 1 calc PR A -1 H42B H -0.3762 0.5431 0.5447 0.105 Uiso 0.50 1 calc PR A -1 O1 O -0.4940(18) 0.4932(15) 0.4800(12) 0.074(5) Uani 0.50 1 d PD A -1 C41 C -0.4954(16) 0.5691(13) 0.3874(13) 0.081(6) Uani 0.50 1 d PD A -1 H41A H -0.4190 0.5980 0.3733 0.098 Uiso 0.50 1 calc PR A -1 H41B H -0.5606 0.6217 0.3899 0.098 Uiso 0.50 1 calc PR A -1 C40 C -0.5141(16) 0.5260(16) 0.3062(15) 0.100(6) Uani 0.50 1 d PD A -1 H40A H -0.5089 0.5768 0.2432 0.150 Uiso 0.50 1 calc PR A -1 H40B H -0.5929 0.5026 0.3172 0.150 Uiso 0.50 1 calc PR A -1 H40C H -0.4524 0.4711 0.3065 0.150 Uiso 0.50 1 calc PR A -1 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 0.0256(2) 0.0202(2) 0.0223(2) -0.01194(19) -0.00124(17) 0.00135(17) Cr1 0.0235(3) 0.0205(3) 0.0209(3) -0.0116(2) -0.0013(2) 0.0009(2) P1 0.0352(5) 0.0217(4) 0.0208(4) -0.0115(4) -0.0047(4) 0.0025(4) P2 0.0226(5) 0.0268(5) 0.0312(5) -0.0143(4) 0.0015(4) -0.0004(4) P3 0.0277(5) 0.0192(4) 0.0302(5) -0.0110(4) -0.0021(4) -0.0009(4) N1 0.0224(14) 0.0205(14) 0.0199(14) -0.0100(12) -0.0006(11) -0.0005(11) N2 0.0336(16) 0.0200(14) 0.0202(14) -0.0095(12) -0.0004(12) -0.0009(12) N3 0.0236(15) 0.049(2) 0.0333(17) -0.0258(16) -0.0063(13) 0.0092(14) N4 0.0331(17) 0.0248(16) 0.0367(17) -0.0182(14) 0.0081(14) -0.0080(13) C1 0.0232(17) 0.0197(16) 0.0270(18) -0.0110(15) -0.0028(14) 0.0029(13) C2 0.034(2) 0.0300(19) 0.0247(18) -0.0156(16) -0.0021(15) 0.0006(16) C3 0.042(2) 0.0238(18) 0.039(2) -0.0207(17) -0.0038(18) -0.0008(16) C4 0.042(2) 0.0200(17) 0.035(2) -0.0108(16) -0.0049(17) -0.0018(16) C5 0.0322(19) 0.0259(18) 0.0269(18) -0.0115(16) -0.0034(15) -0.0006(15) C6 0.0249(17) 0.0227(17) 0.0232(17) -0.0106(14) -0.0028(14) -0.0015(14) C7 0.041(2) 0.0238(18) 0.0215(17) -0.0117(15) -0.0040(15) 0.0010(16) C8 0.040(2) 0.0280(19) 0.033(2) -0.0113(17) -0.0170(17) 0.0048(16) C9 0.034(2) 0.046(3) 0.045(2) -0.010(2) -0.0114(19) -0.0009(19) C10 0.068(3) 0.029(2) 0.054(3) -0.013(2) -0.035(2) 0.002(2) C11 0.054(3) 0.032(2) 0.0240(19) -0.0141(17) 0.0008(18) 0.0053(19) C12 0.083(4) 0.040(3) 0.024(2) -0.0063(19) 0.001(2) 0.012(2) C13 0.066(3) 0.047(3) 0.035(2) -0.021(2) -0.005(2) 0.021(2) C14 0.0257(17) 0.0254(18) 0.0214(17) -0.0094(15) -0.0034(14) -0.0031(14) C15 0.034(2) 0.0288(19) 0.0291(19) -0.0169(16) -0.0010(16) 0.0007(15) C16 0.047(2) 0.044(2) 0.0250(19) -0.0170(18) -0.0078(17) 0.0021(19) C17 0.052(3) 0.049(3) 0.033(2) -0.020(2) -0.0217(19) 0.010(2) C18 0.037(2) 0.047(3) 0.039(2) -0.025(2) -0.0141(18) 0.0127(19) C19 0.0299(19) 0.0303(19) 0.0306(19) -0.0182(17) -0.0053(15) 0.0024(15) C20 0.0233(18) 0.044(2) 0.041(2) -0.027(2) -0.0045(16) 0.0041(16) C21 0.030(2) 0.043(3) 0.063(3) -0.010(2) 0.001(2) -0.0102(19) C22 0.053(3) 0.087(4) 0.060(4) 0.005(3) 0.014(3) -0.027(3) C23 0.046(3) 0.033(3) 0.141(6) -0.011(3) -0.001(3) -0.006(2) C24 0.0260(19) 0.033(2) 0.046(2) -0.0235(19) -0.0002(17) 0.0050(16) C25 0.058(3) 0.055(3) 0.059(3) -0.042(3) 0.006(2) 0.006(2) C26 0.030(2) 0.053(3) 0.091(4) -0.032(3) -0.008(2) 0.015(2) C27 0.0262(17) 0.0242(17) 0.0189(16) -0.0100(14) -0.0027(13) 0.0012(14) C28 0.0293(18) 0.0257(18) 0.0295(19) -0.0166(16) -0.0008(15) 0.0034(15) C29 0.0258(19) 0.039(2) 0.041(2) -0.0189(19) -0.0018(16) 0.0046(16) C30 0.0242(19) 0.046(2) 0.038(2) -0.0172(19) 0.0010(16) -0.0049(17) C31 0.032(2) 0.034(2) 0.037(2) -0.0191(18) 0.0048(17) -0.0088(16) C32 0.0274(18) 0.0265(18) 0.0219(17) -0.0119(15) 0.0010(14) -0.0011(14) C33 0.034(2) 0.0229(18) 0.037(2) -0.0158(17) 0.0043(16) -0.0034(15) C34 0.036(2) 0.0232(19) 0.041(2) -0.0031(17) -0.0038(17) -0.0047(16) C35 0.048(3) 0.045(3) 0.037(2) 0.000(2) -0.011(2) -0.012(2) C36 0.042(2) 0.027(2) 0.059(3) -0.007(2) -0.010(2) 0.0038(18) C37 0.037(2) 0.0254(19) 0.042(2) -0.0200(18) -0.0061(17) 0.0001(16) C38 0.041(2) 0.035(2) 0.064(3) -0.026(2) -0.004(2) -0.0092(18) C39 0.063(3) 0.038(2) 0.044(2) -0.030(2) -0.002(2) -0.004(2) C43 0.050(12) 0.13(2) 0.104(18) -0.038(15) 0.016(10) -0.020(12) C42 0.026(6) 0.118(13) 0.154(16) -0.095(13) -0.012(7) 0.005(7) O1 0.031(5) 0.060(7) 0.120(14) -0.029(8) 0.027(8) 0.005(4) C41 0.039(9) 0.065(9) 0.123(17) -0.020(10) 0.004(8) 0.023(7) C40 0.056(9) 0.126(15) 0.136(17) -0.077(13) -0.009(10) 0.015(9) _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 P1 2.2176(10) . ? Ni1 P2 2.2215(10) . ? Ni1 P3 2.2357(11) . ? Ni1 Cr1 2.4105(7) . ? Cr1 N3 1.948(3) . ? Cr1 N2 1.950(3) . ? Cr1 N4 1.970(3) . ? Cr1 N1 2.086(3) . ? P1 C7 1.855(4) . ? P1 C8 1.859(4) . ? P1 C11 1.862(4) . ? P2 C20 1.852(4) . ? P2 C21 1.856(4) . ? P2 C24 1.865(4) . ? P3 C33 1.853(4) . ? P3 C34 1.859(4) . ? P3 C37 1.862(4) . ? N1 C27 1.470(4) . ? N1 C1 1.474(4) . ? N1 C14 1.478(4) . ? N2 C6 1.378(4) . ? N2 C7 1.450(4) . ? N3 C19 1.378(5) . ? N3 C20 1.450(4) . ? N4 C32 1.382(4) . ? N4 C33 1.447(5) . ? C1 C2 1.366(5) . ? C1 C6 1.419(5) . ? C2 C3 1.397(5) . ? C2 H2A 0.9300 . ? C3 C4 1.379(5) . ? C3 H3A 0.9300 . ? C4 C5 1.395(5) . ? C4 H4A 0.9300 . ? C5 C6 1.399(5) . ? C5 H5A 0.9300 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.525(6) . ? C8 C10 1.526(5) . ? C8 H8A 0.9800 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C13 1.527(5) . ? C11 C12 1.541(6) . ? C11 H11A 0.9800 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.385(5) . ? C14 C19 1.408(5) . ? C15 C16 1.382(5) . ? C15 H15A 0.9300 . ? C16 C17 1.377(6) . ? C16 H16A 0.9300 . ? C17 C18 1.396(6) . ? C17 H17A 0.9300 . ? C18 C19 1.404(5) . ? C18 H18A 0.9300 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.510(7) . ? C21 C23 1.530(7) . ? C21 H21A 0.9800 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C26 1.531(6) . ? C24 C25 1.538(6) . ? C24 H24A 0.9800 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.381(5) . ? C27 C32 1.409(5) . ? C28 C29 1.393(5) . ? C28 H28A 0.9300 . ? C29 C30 1.378(6) . ? C29 H29A 0.9300 . ? C30 C31 1.387(5) . ? C30 H30A 0.9300 . ? C31 C32 1.403(5) . ? C31 H31A 0.9300 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C36 1.528(6) . ? C34 C35 1.529(6) . ? C34 H34A 0.9800 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.520(6) . ? C37 C39 1.546(6) . ? C37 H37A 0.9800 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C43 C42 1.553(17) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C42 O1 1.438(18) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? O1 C41 1.417(17) . ? C41 C40 1.513(16) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? 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 P1 Ni1 P2 119.66(4) . . ? P1 Ni1 P3 121.15(4) . . ? P2 Ni1 P3 118.51(4) . . ? P1 Ni1 Cr1 86.34(3) . . ? P2 Ni1 Cr1 86.59(3) . . ? P3 Ni1 Cr1 88.85(3) . . ? N3 Cr1 N2 116.97(14) . . ? N3 Cr1 N4 111.14(14) . . ? N2 Cr1 N4 125.95(13) . . ? N3 Cr1 N1 82.17(12) . . ? N2 Cr1 N1 81.98(11) . . ? N4 Cr1 N1 81.53(12) . . ? N3 Cr1 Ni1 98.31(9) . . ? N2 Cr1 Ni1 98.00(8) . . ? N4 Cr1 Ni1 98.06(9) . . ? N1 Cr1 Ni1 179.46(8) . . ? C7 P1 C8 99.88(17) . . ? C7 P1 C11 100.47(18) . . ? C8 P1 C11 103.74(19) . . ? C7 P1 Ni1 111.96(12) . . ? C8 P1 Ni1 122.40(13) . . ? C11 P1 Ni1 115.26(13) . . ? C20 P2 C21 100.2(2) . . ? C20 P2 C24 101.74(18) . . ? C21 P2 C24 103.08(19) . . ? C20 P2 Ni1 112.26(12) . . ? C21 P2 Ni1 124.48(16) . . ? C24 P2 Ni1 112.19(13) . . ? C33 P3 C34 99.01(18) . . ? C33 P3 C37 100.07(18) . . ? C34 P3 C37 103.67(18) . . ? C33 P3 Ni1 111.31(12) . . ? C34 P3 Ni1 124.35(13) . . ? C37 P3 Ni1 114.83(13) . . ? C27 N1 C1 113.7(3) . . ? C27 N1 C14 113.4(3) . . ? C1 N1 C14 114.0(3) . . ? C27 N1 Cr1 103.37(19) . . ? C1 N1 Cr1 106.3(2) . . ? C14 N1 Cr1 104.85(19) . . ? C6 N2 C7 118.6(3) . . ? C6 N2 Cr1 113.8(2) . . ? C7 N2 Cr1 126.4(2) . . ? C19 N3 C20 118.9(3) . . ? C19 N3 Cr1 112.9(2) . . ? C20 N3 Cr1 126.3(2) . . ? C32 N4 C33 117.5(3) . . ? C32 N4 Cr1 110.3(2) . . ? C33 N4 Cr1 125.9(2) . . ? C2 C1 C6 121.9(3) . . ? C2 C1 N1 123.6(3) . . ? C6 C1 N1 114.5(3) . . ? C1 C2 C3 120.3(3) . . ? C1 C2 H2A 119.8 . . ? C3 C2 H2A 119.8 . . ? C4 C3 C2 119.2(3) . . ? C4 C3 H3A 120.4 . . ? C2 C3 H3A 120.4 . . ? C3 C4 C5 120.8(4) . . ? C3 C4 H4A 119.6 . . ? C5 C4 H4A 119.6 . . ? C4 C5 C6 120.9(3) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? N2 C6 C5 126.6(3) . . ? N2 C6 C1 116.5(3) . . ? C5 C6 C1 116.8(3) . . ? N2 C7 P1 106.6(2) . . ? N2 C7 H7A 110.4 . . ? P1 C7 H7A 110.4 . . ? N2 C7 H7B 110.4 . . ? P1 C7 H7B 110.4 . . ? H7A C7 H7B 108.6 . . ? C9 C8 C10 111.7(4) . . ? C9 C8 P1 111.0(3) . . ? C10 C8 P1 112.1(3) . . ? C9 C8 H8A 107.2 . . ? C10 C8 H8A 107.2 . . ? P1 C8 H8A 107.2 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C12 112.1(3) . . ? C13 C11 P1 111.7(3) . . ? C12 C11 P1 114.8(3) . . ? C13 C11 H11A 105.8 . . ? C12 C11 H11A 105.8 . . ? P1 C11 H11A 105.8 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 122.0(3) . . ? C15 C14 N1 122.9(3) . . ? C19 C14 N1 115.1(3) . . ? C16 C15 C14 119.6(3) . . ? C16 C15 H15A 120.2 . . ? C14 C15 H15A 120.2 . . ? C17 C16 C15 119.8(4) . . ? C17 C16 H16A 120.1 . . ? C15 C16 H16A 120.1 . . ? C16 C17 C18 121.1(4) . . ? C16 C17 H17A 119.5 . . ? C18 C17 H17A 119.5 . . ? C17 C18 C19 120.3(4) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? N3 C19 C18 126.4(3) . . ? N3 C19 C14 116.5(3) . . ? C18 C19 C14 117.1(3) . . ? N3 C20 P2 107.3(3) . . ? N3 C20 H20A 110.3 . . ? P2 C20 H20A 110.3 . . ? N3 C20 H20B 110.3 . . ? P2 C20 H20B 110.3 . . ? H20A C20 H20B 108.5 . . ? C22 C21 C23 111.5(5) . . ? C22 C21 P2 112.6(4) . . ? C23 C21 P2 110.2(3) . . ? C22 C21 H21A 107.4 . . ? C23 C21 H21A 107.4 . . ? P2 C21 H21A 107.4 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C26 C24 C25 111.8(4) . . ? C26 C24 P2 115.9(3) . . ? C25 C24 P2 111.1(3) . . ? C26 C24 H24A 105.7 . . ? C25 C24 H24A 105.7 . . ? P2 C24 H24A 105.7 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 122.2(3) . . ? C28 C27 N1 123.0(3) . . ? C32 C27 N1 114.8(3) . . ? C27 C28 C29 120.0(3) . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C30 C29 C28 118.4(3) . . ? C30 C29 H29A 120.8 . . ? C28 C29 H29A 120.8 . . ? C29 C30 C31 122.2(4) . . ? C29 C30 H30A 118.9 . . ? C31 C30 H30A 118.9 . . ? C30 C31 C32 120.3(4) . . ? C30 C31 H31A 119.9 . . ? C32 C31 H31A 119.9 . . ? N4 C32 C31 126.5(3) . . ? N4 C32 C27 116.6(3) . . ? C31 C32 C27 116.8(3) . . ? N4 C33 P3 109.4(3) . . ? N4 C33 H33A 109.8 . . ? P3 C33 H33A 109.8 . . ? N4 C33 H33B 109.8 . . ? P3 C33 H33B 109.8 . . ? H33A C33 H33B 108.2 . . ? C36 C34 C35 111.6(4) . . ? C36 C34 P3 113.4(3) . . ? C35 C34 P3 109.7(3) . . ? C36 C34 H34A 107.3 . . ? C35 C34 H34A 107.3 . . ? P3 C34 H34A 107.3 . . ? 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 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C39 112.1(3) . . ? C38 C37 P3 116.1(3) . . ? C39 C37 P3 112.0(3) . . ? C38 C37 H37A 105.1 . . ? C39 C37 H37A 105.1 . . ? P3 C37 H37A 105.1 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O1 C42 C43 104.3(16) . . ? O1 C42 H42A 110.9 . . ? C43 C42 H42A 110.9 . . ? O1 C42 H42B 110.9 . . ? C43 C42 H42B 110.9 . . ? H42A C42 H42B 108.9 . . ? C41 O1 C42 112.2(17) . . ? O1 C41 C40 110.2(16) . . ? O1 C41 H41A 109.6 . . ? C40 C41 H41A 109.6 . . ? O1 C41 H41B 109.6 . . ? C40 C41 H41B 109.6 . . ? H41A C41 H41B 108.1 . . ? 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 P1 Ni1 Cr1 N3 -139.55(11) . . . . ? P2 Ni1 Cr1 N3 -19.51(11) . . . . ? P3 Ni1 Cr1 N3 99.14(11) . . . . ? P1 Ni1 Cr1 N2 -20.65(10) . . . . ? P2 Ni1 Cr1 N2 99.39(9) . . . . ? P3 Ni1 Cr1 N2 -141.96(9) . . . . ? P1 Ni1 Cr1 N4 107.57(10) . . . . ? P2 Ni1 Cr1 N4 -132.39(10) . . . . ? P3 Ni1 Cr1 N4 -13.74(10) . . . . ? P1 Ni1 Cr1 N1 67(9) . . . . ? P2 Ni1 Cr1 N1 -173(93) . . . . ? P3 Ni1 Cr1 N1 -54(9) . . . . ? P2 Ni1 P1 C7 -52.89(14) . . . . ? P3 Ni1 P1 C7 117.51(14) . . . . ? Cr1 Ni1 P1 C7 31.07(14) . . . . ? P2 Ni1 P1 C8 -171.25(15) . . . . ? P3 Ni1 P1 C8 -0.85(16) . . . . ? Cr1 Ni1 P1 C8 -87.28(15) . . . . ? P2 Ni1 P1 C11 61.12(16) . . . . ? P3 Ni1 P1 C11 -128.48(16) . . . . ? Cr1 Ni1 P1 C11 145.09(16) . . . . ? P1 Ni1 P2 C20 112.87(15) . . . . ? P3 Ni1 P2 C20 -57.79(16) . . . . ? Cr1 Ni1 P2 C20 29.04(15) . . . . ? P1 Ni1 P2 C21 -8.1(2) . . . . ? P3 Ni1 P2 C21 -178.72(19) . . . . ? Cr1 Ni1 P2 C21 -91.89(19) . . . . ? P1 Ni1 P2 C24 -133.28(15) . . . . ? P3 Ni1 P2 C24 56.07(16) . . . . ? Cr1 Ni1 P2 C24 142.89(15) . . . . ? P1 Ni1 P3 C33 -61.90(15) . . . . ? P2 Ni1 P3 C33 108.61(14) . . . . ? Cr1 Ni1 P3 C33 23.13(14) . . . . ? P1 Ni1 P3 C34 -179.95(17) . . . . ? P2 Ni1 P3 C34 -9.43(17) . . . . ? Cr1 Ni1 P3 C34 -94.92(17) . . . . ? P1 Ni1 P3 C37 50.88(14) . . . . ? P2 Ni1 P3 C37 -138.60(14) . . . . ? Cr1 Ni1 P3 C37 135.91(14) . . . . ? N3 Cr1 N1 C27 -144.1(2) . . . . ? N2 Cr1 N1 C27 97.1(2) . . . . ? N4 Cr1 N1 C27 -31.2(2) . . . . ? Ni1 Cr1 N1 C27 9(9) . . . . ? N3 Cr1 N1 C1 95.9(2) . . . . ? N2 Cr1 N1 C1 -22.8(2) . . . . ? N4 Cr1 N1 C1 -151.2(2) . . . . ? Ni1 Cr1 N1 C1 -111(9) . . . . ? N3 Cr1 N1 C14 -25.1(2) . . . . ? N2 Cr1 N1 C14 -143.9(2) . . . . ? N4 Cr1 N1 C14 87.8(2) . . . . ? Ni1 Cr1 N1 C14 128(9) . . . . ? N3 Cr1 N2 C6 -55.5(3) . . . . ? N4 Cr1 N2 C6 94.8(3) . . . . ? N1 Cr1 N2 C6 21.4(2) . . . . ? Ni1 Cr1 N2 C6 -159.1(2) . . . . ? N3 Cr1 N2 C7 111.5(3) . . . . ? N4 Cr1 N2 C7 -98.2(3) . . . . ? N1 Cr1 N2 C7 -171.6(3) . . . . ? Ni1 Cr1 N2 C7 7.9(3) . . . . ? N2 Cr1 N3 C19 100.9(3) . . . . ? N4 Cr1 N3 C19 -53.7(3) . . . . ? N1 Cr1 N3 C19 24.0(3) . . . . ? Ni1 Cr1 N3 C19 -155.7(3) . . . . ? N2 Cr1 N3 C20 -95.5(4) . . . . ? N4 Cr1 N3 C20 109.9(3) . . . . ? N1 Cr1 N3 C20 -172.3(4) . . . . ? Ni1 Cr1 N3 C20 7.9(4) . . . . ? N3 Cr1 N4 C32 108.1(3) . . . . ? N2 Cr1 N4 C32 -43.7(3) . . . . ? N1 Cr1 N4 C32 29.9(2) . . . . ? Ni1 Cr1 N4 C32 -149.8(2) . . . . ? N3 Cr1 N4 C33 -101.0(3) . . . . ? N2 Cr1 N4 C33 107.2(3) . . . . ? N1 Cr1 N4 C33 -179.1(3) . . . . ? Ni1 Cr1 N4 C33 1.2(3) . . . . ? C27 N1 C1 C2 87.7(4) . . . . ? C14 N1 C1 C2 -44.3(4) . . . . ? Cr1 N1 C1 C2 -159.2(3) . . . . ? C27 N1 C1 C6 -91.4(3) . . . . ? C14 N1 C1 C6 136.6(3) . . . . ? Cr1 N1 C1 C6 21.6(3) . . . . ? C6 C1 C2 C3 1.8(5) . . . . ? N1 C1 C2 C3 -177.2(3) . . . . ? C1 C2 C3 C4 0.0(6) . . . . ? C2 C3 C4 C5 -0.7(6) . . . . ? C3 C4 C5 C6 -0.5(6) . . . . ? C7 N2 C6 C5 -5.5(5) . . . . ? Cr1 N2 C6 C5 162.6(3) . . . . ? C7 N2 C6 C1 177.0(3) . . . . ? Cr1 N2 C6 C1 -14.9(4) . . . . ? C4 C5 C6 N2 -175.3(3) . . . . ? C4 C5 C6 C1 2.2(5) . . . . ? C2 C1 C6 N2 174.9(3) . . . . ? N1 C1 C6 N2 -6.0(4) . . . . ? C2 C1 C6 C5 -2.9(5) . . . . ? N1 C1 C6 C5 176.3(3) . . . . ? C6 N2 C7 P1 -179.7(3) . . . . ? Cr1 N2 C7 P1 13.8(4) . . . . ? C8 P1 C7 N2 98.9(3) . . . . ? C11 P1 C7 N2 -155.0(3) . . . . ? Ni1 P1 C7 N2 -32.1(3) . . . . ? C7 P1 C8 C9 -64.6(3) . . . . ? C11 P1 C8 C9 -168.1(3) . . . . ? Ni1 P1 C8 C9 59.4(3) . . . . ? C7 P1 C8 C10 169.6(3) . . . . ? C11 P1 C8 C10 66.2(3) . . . . ? Ni1 P1 C8 C10 -66.3(3) . . . . ? C7 P1 C11 C13 164.7(3) . . . . ? C8 P1 C11 C13 -92.3(3) . . . . ? Ni1 P1 C11 C13 44.2(4) . . . . ? C7 P1 C11 C12 -66.3(4) . . . . ? C8 P1 C11 C12 36.7(4) . . . . ? Ni1 P1 C11 C12 173.2(3) . . . . ? C27 N1 C14 C15 -45.7(4) . . . . ? C1 N1 C14 C15 86.5(4) . . . . ? Cr1 N1 C14 C15 -157.7(3) . . . . ? C27 N1 C14 C19 135.5(3) . . . . ? C1 N1 C14 C19 -92.3(4) . . . . ? Cr1 N1 C14 C19 23.5(3) . . . . ? C19 C14 C15 C16 1.6(6) . . . . ? N1 C14 C15 C16 -177.0(3) . . . . ? C14 C15 C16 C17 0.7(6) . . . . ? C15 C16 C17 C18 -2.8(7) . . . . ? C16 C17 C18 C19 2.5(7) . . . . ? C20 N3 C19 C18 -5.2(6) . . . . ? Cr1 N3 C19 C18 159.8(4) . . . . ? C20 N3 C19 C14 178.0(4) . . . . ? Cr1 N3 C19 C14 -17.1(4) . . . . ? C17 C18 C19 N3 -176.9(4) . . . . ? C17 C18 C19 C14 -0.1(6) . . . . ? C15 C14 C19 N3 175.2(4) . . . . ? N1 C14 C19 N3 -6.0(5) . . . . ? C15 C14 C19 C18 -1.9(6) . . . . ? N1 C14 C19 C18 176.9(3) . . . . ? C19 N3 C20 P2 175.2(3) . . . . ? Cr1 N3 C20 P2 12.5(4) . . . . ? C21 P2 C20 N3 104.2(3) . . . . ? C24 P2 C20 N3 -150.0(3) . . . . ? Ni1 P2 C20 N3 -29.8(3) . . . . ? C20 P2 C21 C22 173.2(4) . . . . ? C24 P2 C21 C22 68.4(4) . . . . ? Ni1 P2 C21 C22 -60.6(4) . . . . ? C20 P2 C21 C23 -61.7(4) . . . . ? C24 P2 C21 C23 -166.4(4) . . . . ? Ni1 P2 C21 C23 64.6(5) . . . . ? C20 P2 C24 C26 -64.3(4) . . . . ? C21 P2 C24 C26 39.2(4) . . . . ? Ni1 P2 C24 C26 175.5(3) . . . . ? C20 P2 C24 C25 166.6(3) . . . . ? C21 P2 C24 C25 -89.9(3) . . . . ? Ni1 P2 C24 C25 46.4(3) . . . . ? C1 N1 C27 C28 -36.0(4) . . . . ? C14 N1 C27 C28 96.3(4) . . . . ? Cr1 N1 C27 C28 -150.8(3) . . . . ? C1 N1 C27 C32 143.6(3) . . . . ? C14 N1 C27 C32 -84.1(4) . . . . ? Cr1 N1 C27 C32 28.8(3) . . . . ? C32 C27 C28 C29 2.8(5) . . . . ? N1 C27 C28 C29 -177.6(3) . . . . ? C27 C28 C29 C30 -0.5(6) . . . . ? C28 C29 C30 C31 -0.6(6) . . . . ? C29 C30 C31 C32 -0.6(6) . . . . ? C33 N4 C32 C31 1.2(6) . . . . ? Cr1 N4 C32 C31 154.9(3) . . . . ? C33 N4 C32 C27 -175.3(3) . . . . ? Cr1 N4 C32 C27 -21.6(4) . . . . ? C30 C31 C32 N4 -173.8(4) . . . . ? C30 C31 C32 C27 2.7(5) . . . . ? C28 C27 C32 N4 173.0(3) . . . . ? N1 C27 C32 N4 -6.7(4) . . . . ? C28 C27 C32 C31 -3.9(5) . . . . ? N1 C27 C32 C31 176.5(3) . . . . ? C32 N4 C33 P3 164.9(3) . . . . ? Cr1 N4 C33 P3 15.8(4) . . . . ? C34 P3 C33 N4 105.7(3) . . . . ? C37 P3 C33 N4 -148.5(3) . . . . ? Ni1 P3 C33 N4 -26.7(3) . . . . ? C33 P3 C34 C36 166.8(3) . . . . ? C37 P3 C34 C36 64.0(3) . . . . ? Ni1 P3 C34 C36 -69.6(3) . . . . ? C33 P3 C34 C35 -67.7(3) . . . . ? C37 P3 C34 C35 -170.5(3) . . . . ? Ni1 P3 C34 C35 55.9(3) . . . . ? C33 P3 C37 C38 -62.4(3) . . . . ? C34 P3 C37 C38 39.6(3) . . . . ? Ni1 P3 C37 C38 178.4(2) . . . . ? C33 P3 C37 C39 167.0(3) . . . . ? C34 P3 C37 C39 -91.0(3) . . . . ? Ni1 P3 C37 C39 47.8(3) . . . . ? C43 C42 O1 C41 175.6(19) . . . . ? C42 O1 C41 C40 171.8(12) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.656 _refine_diff_density_min -0.985 _refine_diff_density_rms 0.140 _iucr_refine_instructions_details ; TITL 12080_0m in P-1 CELL 0.71073 11.1205 14.1669 14.2565 71.694 83.745 81.854 ZERR 2.00 0.0016 0.0020 0.0020 0.002 0.002 0.002 LATT 1 SFAC C H N P CR NI O UNIT 82 120 8 6 2 2 2 TEMP 23.000 L.S. 16 BOND $H FMAP 2 PLAN 20 ACTA CONF LIST 4 HTAB SPEC 0.0001 DFIX O1 C42 1.42 DFIX O1 C41 1.42 DFIX C42 C43 1.52 DFIX C41 C40 1.52 WGHT 0.112800 FVAR 0.16128 NI1 6 0.280458 0.174137 0.161674 11.00000 0.02560 0.02019 = 0.02226 -0.01194 -0.00124 0.00135 CR1 5 0.199959 0.266760 0.274877 11.00000 0.02354 0.02047 = 0.02090 -0.01160 -0.00129 0.00094 P1 4 0.194823 0.301494 0.044546 11.00000 0.03521 0.02173 = 0.02076 -0.01154 -0.00471 0.00251 P2 4 0.463321 0.181405 0.206387 11.00000 0.02256 0.02684 = 0.03125 -0.01426 0.00152 -0.00042 P3 4 0.175497 0.048851 0.252218 11.00000 0.02770 0.01918 = 0.03023 -0.01103 -0.00214 -0.00093 N1 3 0.128639 0.346742 0.372640 11.00000 0.02239 0.02055 = 0.01989 -0.01004 -0.00061 -0.00046 N2 3 0.176860 0.399214 0.178180 11.00000 0.03355 0.01999 = 0.02017 -0.00950 -0.00043 -0.00088 N3 3 0.339767 0.238021 0.354776 11.00000 0.02356 0.04854 = 0.03335 -0.02575 -0.00632 0.00923 N4 3 0.070165 0.183562 0.343636 11.00000 0.03309 0.02483 = 0.03664 -0.01813 0.00810 -0.00804 C1 1 0.151413 0.451448 0.322873 11.00000 0.02317 0.01975 = 0.02699 -0.01102 -0.00283 0.00286 C2 1 0.152814 0.520091 0.371828 11.00000 0.03449 0.03005 = 0.02475 -0.01563 -0.00210 0.00059 AFIX 43 H2A 2 0.142350 0.500801 0.440582 11.00000 -1.20000 AFIX 0 C3 1 0.169892 0.619125 0.319105 11.00000 0.04238 0.02382 = 0.03853 -0.02070 -0.00385 -0.00076 AFIX 43 H3A 2 0.170864 0.665953 0.352318 11.00000 -1.20000 AFIX 0 C4 1 0.185292 0.646572 0.217161 11.00000 0.04221 0.02002 = 0.03511 -0.01076 -0.00495 -0.00181 AFIX 43 H4A 2 0.195876 0.712534 0.181566 11.00000 -1.20000 AFIX 0 C5 1 0.185186 0.576589 0.166794 11.00000 0.03220 0.02589 = 0.02690 -0.01150 -0.00342 -0.00062 AFIX 43 H5A 2 0.195052 0.596661 0.098003 11.00000 -1.20000 AFIX 0 C6 1 0.170444 0.476617 0.218313 11.00000 0.02494 0.02271 = 0.02316 -0.01063 -0.00282 -0.00144 C7 1 0.190213 0.421939 0.071296 11.00000 0.04091 0.02378 = 0.02150 -0.01172 -0.00397 0.00101 AFIX 23 H7A 2 0.264760 0.452017 0.045115 11.00000 -1.20000 H7B 2 0.122031 0.468216 0.041340 11.00000 -1.20000 AFIX 0 C8 1 0.034208 0.309556 0.014946 11.00000 0.03981 0.02797 = 0.03272 -0.01125 -0.01704 0.00478 AFIX 13 H8A 2 0.015916 0.373993 -0.035626 11.00000 -1.20000 AFIX 0 C9 1 -0.053038 0.309214 0.105335 11.00000 0.03352 0.04562 = 0.04496 -0.01004 -0.01142 -0.00086 AFIX 137 H9A 2 -0.135466 0.318961 0.086966 11.00000 -1.50000 H9B 2 -0.039493 0.362273 0.130033 11.00000 -1.50000 H9C 2 -0.039063 0.246194 0.155891 11.00000 -1.50000 AFIX 0 C10 1 0.014873 0.227870 -0.028822 11.00000 0.06842 0.02869 = 0.05442 -0.01344 -0.03499 0.00207 AFIX 33 H10A 2 -0.068643 0.235218 -0.043892 11.00000 -1.50000 H10B 2 0.034434 0.163419 0.018218 11.00000 -1.50000 H10C 2 0.066665 0.233578 -0.088329 11.00000 -1.50000 AFIX 0 C11 1 0.280574 0.330819 -0.078884 11.00000 0.05402 0.03238 = 0.02403 -0.01415 0.00076 0.00530 AFIX 13 H11A 2 0.353079 0.359147 -0.071344 11.00000 -1.20000 AFIX 0 C12 1 0.213396 0.411167 -0.162505 11.00000 0.08265 0.04015 = 0.02432 -0.00631 0.00087 0.01167 AFIX 137 H12A 2 0.265899 0.425376 -0.222127 11.00000 -1.50000 H12B 2 0.191024 0.471117 -0.143846 11.00000 -1.50000 H12C 2 0.141423 0.387053 -0.173624 11.00000 -1.50000 AFIX 0 C13 1 0.327753 0.236212 -0.107339 11.00000 0.06646 0.04653 = 0.03491 -0.02109 -0.00479 0.02083 AFIX 137 H13A 2 0.379351 0.253241 -0.167331 11.00000 -1.50000 H13B 2 0.260192 0.205979 -0.117384 11.00000 -1.50000 H13C 2 0.373376 0.189943 -0.055191 11.00000 -1.50000 AFIX 0 C14 1 0.194777 0.298207 0.463167 11.00000 0.02572 0.02542 = 0.02140 -0.00943 -0.00336 -0.00306 C15 1 0.149511 0.305000 0.555567 11.00000 0.03371 0.02882 = 0.02907 -0.01691 -0.00106 0.00071 AFIX 43 H15A 2 0.072799 0.338677 0.563336 11.00000 -1.20000 AFIX 0 C16 1 0.219005 0.261441 0.636147 11.00000 0.04737 0.04374 = 0.02501 -0.01703 -0.00782 0.00215 AFIX 43 H16A 2 0.188867 0.265047 0.698540 11.00000 -1.20000 AFIX 0 C17 1 0.332990 0.212702 0.623691 11.00000 0.05207 0.04934 = 0.03337 -0.02006 -0.02172 0.01013 AFIX 43 H17A 2 0.380836 0.186004 0.677530 11.00000 -1.20000 AFIX 0 C18 1 0.377926 0.202700 0.531587 11.00000 0.03677 0.04724 = 0.03921 -0.02474 -0.01408 0.01270 AFIX 43 H18A 2 0.453871 0.167317 0.525172 11.00000 -1.20000 AFIX 0 C19 1 0.309062 0.245783 0.448571 11.00000 0.02988 0.03034 = 0.03058 -0.01820 -0.00528 0.00241 C20 1 0.458096 0.187665 0.334579 11.00000 0.02328 0.04428 = 0.04130 -0.02695 -0.00451 0.00412 AFIX 23 H20A 2 0.469213 0.120809 0.380968 11.00000 -1.20000 H20B 2 0.522231 0.224581 0.341034 11.00000 -1.20000 AFIX 0 C21 1 0.561859 0.281102 0.141780 11.00000 0.03002 0.04273 = 0.06335 -0.00971 0.00138 -0.01014 AFIX 13 H21A 2 0.637504 0.265250 0.175811 11.00000 -1.20000 AFIX 0 C22 1 0.595653 0.285801 0.035037 11.00000 0.05303 0.08691 = 0.06031 0.00488 0.01392 -0.02701 AFIX 137 H22A 2 0.626975 0.348148 0.000293 11.00000 -1.50000 H22B 2 0.524790 0.280859 0.004718 11.00000 -1.50000 H22C 2 0.656677 0.231383 0.032242 11.00000 -1.50000 AFIX 0 C23 1 0.501311 0.382099 0.150693 11.00000 0.04613 0.03321 = 0.14088 -0.01108 -0.00106 -0.00560 AFIX 137 H23A 2 0.553759 0.432825 0.118275 11.00000 -1.50000 H23B 2 0.486926 0.378186 0.219371 11.00000 -1.50000 H23C 2 0.425246 0.398678 0.120028 11.00000 -1.50000 AFIX 0 C24 1 0.567262 0.064067 0.214273 11.00000 0.02604 0.03341 = 0.04583 -0.02350 -0.00023 0.00496 AFIX 13 H24A 2 0.533661 0.012414 0.270434 11.00000 -1.20000 AFIX 0 C25 1 0.562133 0.029576 0.122831 11.00000 0.05751 0.05453 = 0.05911 -0.04247 0.00642 0.00577 AFIX 33 H25A 2 0.615464 -0.031291 0.129066 11.00000 -1.50000 H25B 2 0.587419 0.080390 0.064353 11.00000 -1.50000 H25C 2 0.480315 0.018103 0.118000 11.00000 -1.50000 AFIX 0 C26 1 0.698488 0.065118 0.236866 11.00000 0.03002 0.05283 = 0.09114 -0.03159 -0.00800 0.01469 AFIX 137 H26A 2 0.742250 -0.000189 0.245596 11.00000 -1.50000 H26B 2 0.698189 0.083260 0.296362 11.00000 -1.50000 H26C 2 0.737288 0.112944 0.182804 11.00000 -1.50000 AFIX 0 C27 1 -0.001033 0.331909 0.386234 11.00000 0.02618 0.02417 = 0.01886 -0.00996 -0.00269 0.00125 C28 1 -0.091563 0.401264 0.407260 11.00000 0.02930 0.02570 = 0.02952 -0.01664 -0.00082 0.00344 AFIX 43 H28A 2 -0.071937 0.461607 0.410955 11.00000 -1.20000 AFIX 0 C29 1 -0.212265 0.380788 0.422927 11.00000 0.02580 0.03858 = 0.04057 -0.01884 -0.00179 0.00464 AFIX 43 H29A 2 -0.273977 0.426626 0.437675 11.00000 -1.20000 AFIX 0 C30 1 -0.238027 0.290943 0.416044 11.00000 0.02417 0.04556 = 0.03784 -0.01716 0.00097 -0.00492 AFIX 43 H30A 2 -0.318314 0.276477 0.427015 11.00000 -1.20000 AFIX 0 C31 1 -0.148317 0.221391 0.393318 11.00000 0.03248 0.03356 = 0.03717 -0.01912 0.00474 -0.00883 AFIX 43 H31A 2 -0.168989 0.161277 0.389858 11.00000 -1.20000 AFIX 0 C32 1 -0.026522 0.241336 0.375529 11.00000 0.02742 0.02653 = 0.02185 -0.01195 0.00101 -0.00110 C33 1 0.044266 0.094200 0.324692 11.00000 0.03350 0.02296 = 0.03736 -0.01579 0.00430 -0.00335 AFIX 23 H33A 2 -0.028188 0.108912 0.288073 11.00000 -1.20000 H33B 2 0.029409 0.042801 0.386919 11.00000 -1.20000 AFIX 0 C34 1 0.239009 -0.060898 0.351931 11.00000 0.03581 0.02317 = 0.04140 -0.00314 -0.00384 -0.00468 AFIX 13 H34A 2 0.171255 -0.098902 0.385386 11.00000 -1.20000 AFIX 0 C35 1 0.290052 -0.025166 0.428594 11.00000 0.04823 0.04466 = 0.03699 -0.00012 -0.01092 -0.01203 AFIX 137 H35A 2 0.314252 -0.081804 0.483654 11.00000 -1.50000 H35B 2 0.228617 0.019059 0.451270 11.00000 -1.50000 H35C 2 0.359339 0.009686 0.398999 11.00000 -1.50000 AFIX 0 C36 1 0.333472 -0.131621 0.313247 11.00000 0.04182 0.02696 = 0.05893 -0.00686 -0.00992 0.00378 AFIX 137 H36A 2 0.369387 -0.182377 0.368104 11.00000 -1.50000 H36B 2 0.395691 -0.094471 0.272004 11.00000 -1.50000 H36C 2 0.294695 -0.162456 0.275324 11.00000 -1.50000 AFIX 0 C37 1 0.094777 -0.007790 0.179198 11.00000 0.03662 0.02543 = 0.04222 -0.02005 -0.00614 0.00008 AFIX 13 H37A 2 0.032411 0.045161 0.146961 11.00000 -1.20000 AFIX 0 C38 1 0.025395 -0.095072 0.238527 11.00000 0.04050 0.03466 = 0.06385 -0.02575 -0.00392 -0.00925 AFIX 137 H38A 2 -0.022142 -0.112370 0.195312 11.00000 -1.50000 H38B 2 -0.027523 -0.076372 0.289191 11.00000 -1.50000 H38C 2 0.082035 -0.151594 0.268545 11.00000 -1.50000 AFIX 0 C39 1 0.178169 -0.031520 0.093497 11.00000 0.06304 0.03828 = 0.04411 -0.03003 -0.00213 -0.00409 AFIX 137 H39A 2 0.131278 -0.054085 0.053703 11.00000 -1.50000 H39B 2 0.242280 -0.082946 0.120180 11.00000 -1.50000 H39C 2 0.212748 0.027732 0.053375 11.00000 -1.50000 AFIX 0 SAME C40 C41 O1 C42 C43 SAME C43 C42 O1 C41 C40 PART -1 C43 1 -0.473798 0.438397 0.652717 10.50000 0.05000 0.12853 = 0.10611 -0.04148 0.01681 -0.02191 AFIX 137 H43A 2 -0.436011 0.449785 0.705017 10.50000 -1.50000 H43B 2 -0.435435 0.377560 0.641166 10.50000 -1.50000 H43C 2 -0.558719 0.432886 0.671331 10.50000 -1.50000 AFIX 0 C42 1 -0.459714 0.526658 0.557386 10.50000 0.02504 0.11878 = 0.15317 -0.09487 -0.01233 0.00585 AFIX 23 H42A 2 -0.512509 0.585740 0.562573 10.50000 -1.20000 H42B 2 -0.376213 0.542342 0.544954 10.50000 -1.20000 AFIX 0 O1 7 -0.493972 0.493443 0.479884 10.50000 0.03121 0.06149 = 0.11792 -0.02782 0.02622 0.00444 C41 1 -0.495313 0.569913 0.387213 10.50000 0.03877 0.06455 = 0.12354 -0.02199 0.00448 0.02079 AFIX 23 H41A 2 -0.418823 0.598788 0.372986 10.50000 -1.20000 H41B 2 -0.560529 0.622568 0.389611 10.50000 -1.20000 AFIX 0 C40 1 -0.514212 0.525516 0.306284 10.50000 0.05707 0.12603 = 0.13738 -0.07824 -0.00938 0.01577 AFIX 137 H40A 2 -0.508815 0.575792 0.242996 10.50000 -1.50000 H40B 2 -0.593108 0.502298 0.317598 10.50000 -1.50000 H40C 2 -0.452631 0.470460 0.307219 10.50000 -1.50000 PART 0 HKLF 4 REM 12080_0m in P-1 REM R1 = 0.0592 for 6867 Fo > 4sig(Fo) and 0.0852 for all 9577 data REM 490 parameters refined using 7 restraints END WGHT 0.1127 0.0000 REM Highest difference peak 1.656, deepest hole -0.985, 1-sigma level 0.140 Q1 1 0.2657 0.2415 0.0957 11.00000 0.05 1.66 Q2 1 0.2018 0.2017 0.1387 11.00000 0.05 1.52 Q3 1 0.1933 0.1775 0.1612 11.00000 0.05 1.51 Q4 1 0.2813 0.1198 0.2245 11.00000 0.05 1.43 Q5 1 0.3581 0.1576 0.1760 11.00000 0.05 1.33 Q6 1 0.3246 0.1342 0.2104 11.00000 0.05 1.30 Q7 1 0.2246 0.1334 0.2055 11.00000 0.05 1.22 Q8 1 0.2793 0.2456 0.3106 11.00000 0.05 1.22 Q9 1 0.3583 0.2028 0.1273 11.00000 0.05 1.13 Q10 1 0.1850 0.3254 0.2136 11.00000 0.05 1.11 Q11 1 0.1143 0.2452 0.3099 11.00000 0.05 1.08 Q12 1 0.2254 0.2155 0.3345 11.00000 0.05 1.03 Q13 1 0.1187 0.3222 0.0197 11.00000 0.05 1.01 Q14 1 0.1441 0.2172 0.3286 11.00000 0.05 0.99 Q15 1 0.1229 0.2977 0.2409 11.00000 0.05 0.93 Q16 1 0.1330 0.3366 -0.0010 11.00000 0.05 0.89 Q17 1 0.2145 0.0033 0.3073 11.00000 0.05 0.79 Q18 1 0.2327 0.3446 -0.0084 11.00000 0.05 0.71 Q19 1 0.4805 0.2379 0.1473 11.00000 0.05 0.66 Q20 1 0.4537 0.1341 0.2570 11.00000 0.05 0.64 ;