# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Sue Berners-Price' _publ_contact_author_email SUE.BERNERS-PRICE@UWA.EDU.AU _publ_section_title ; 1:2 Adducts of copper(I) halides with 1,2-bis(di-2-pyridylphosphino)ethane: Solid state and solution structural studies and antitumour activity ; loop_ _publ_author_name 'Sue Berners-Price' 'Richard J. Bowen' 'Aleksandra Filipovska' 'Peter Healy' 'Maribel Navarro' ; A.-M.J.Shearwood ; 'Brian W Skelton' # Attachment 'mn2_mn6_217bp07.cif' data_mn2 #===END _database_code_depnum_ccdc_archive 'CCDC 717471' _audit_creation_date 2008-12-05T11:45:52-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C94 H89 Cl2 Cu2 N19 P8' _chemical_formula_moiety 'C88 H80 Cu2 N16 P8, 3(C2 H3 N), 2(Cl)' _chemical_formula_weight 1930.58 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6804(6) _cell_length_b 12.8005(2) _cell_length_c 15.5405(6) _cell_angle_alpha 83.820(2) _cell_angle_beta 66.951(4) _cell_angle_gamma 81.930(2) _cell_volume 2294.26(16) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7291 _cell_measurement_theta_min 3.5938 _cell_measurement_theta_max 37.3721 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.36 _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 998 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.646 _exptl_absorpt_correction_T_max 0.77 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 -0.0402886949 _diffrn_orient_matrix_ub_12 -0.0054584117 _diffrn_orient_matrix_ub_13 0.0467569394 _diffrn_orient_matrix_ub_21 0.045279337 _diffrn_orient_matrix_ub_22 -0.0028335872 _diffrn_orient_matrix_ub_23 0.0165097302 _diffrn_orient_matrix_ub_31 -0.0082664506 _diffrn_orient_matrix_ub_32 0.0557264658 _diffrn_orient_matrix_ub_33 0.0024836377 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_unetI/netI 0.0367 _diffrn_reflns_number 50222 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 37.47 _diffrn_reflns_theta_full 35.75 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.938 _diffrn_measurement_device_type ; Oxford Diffraction Gemini diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 22591 _reflns_number_gt 16620 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1677P)^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_number_reflns 22591 _refine_ls_number_parameters 573 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.082 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.2325 _refine_ls_wR_factor_gt 0.2176 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.142 _refine_diff_density_min -2.128 _refine_diff_density_rms 0.184 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cu1 Cu 0.572802(12) 0.459114(11) 0.285053(10) 0.01435(3) Uani 1 1 d . . . P1 P 0.39979(3) 0.41837(3) 0.28617(2) 0.01764(6) Uani 1 1 d . . . C111 C 0.31339(11) 0.32073(11) 0.36911(11) 0.0235(3) Uani 1 1 d . . . N112 N 0.28355(12) 0.34321(12) 0.45831(10) 0.0298(3) Uani 1 1 d . . . C113 C 0.21354(17) 0.28038(16) 0.52542(14) 0.0390(4) Uani 1 1 d . . . H113 H 0.1904 0.2954 0.5892 0.047 Uiso 1 1 calc R . . C114 C 0.17441(16) 0.19505(14) 0.50448(16) 0.0429(5) Uani 1 1 d . . . H114 H 0.1257 0.1523 0.5537 0.052 Uiso 1 1 calc R . . C115 C 0.20482(16) 0.17159(14) 0.41428(17) 0.0423(5) Uani 1 1 d . . . H115 H 0.1773 0.1133 0.3997 0.051 Uiso 1 1 calc R . . C116 C 0.27752(14) 0.23508(13) 0.34354(14) 0.0319(3) Uani 1 1 d . . . H116 H 0.302 0.2203 0.2796 0.038 Uiso 1 1 calc R . . C121 C 0.28342(11) 0.52467(10) 0.29068(10) 0.0199(2) Uani 1 1 d . . . N122 N 0.25973(10) 0.54484(11) 0.21327(9) 0.0255(3) Uani 1 1 d . . . C123 C 0.17754(14) 0.62473(14) 0.21522(13) 0.0326(4) Uani 1 1 d . . . H123 H 0.1601 0.641 0.1608 0.039 Uiso 1 1 calc R . . C124 C 0.11735(15) 0.68426(14) 0.29196(14) 0.0347(4) Uani 1 1 d . . . H124 H 0.0608 0.7405 0.2898 0.042 Uiso 1 1 calc R . . C125 C 0.14074(15) 0.66076(14) 0.37222(14) 0.0341(4) Uani 1 1 d . . . H125 H 0.0993 0.6996 0.4264 0.041 Uiso 1 1 calc R . . C126 C 0.22586(13) 0.57933(12) 0.37222(11) 0.0265(3) Uani 1 1 d . . . H126 H 0.2443 0.5615 0.426 0.032 Uiso 1 1 calc R . . C10 C 0.43804(12) 0.36671(12) 0.17095(10) 0.0239(3) Uani 1 1 d . . . H10A H 0.4713 0.292 0.1712 0.029 Uiso 1 1 calc R . . H10B H 0.3681 0.3699 0.1566 0.029 Uiso 1 1 calc R . . C20 C 0.52592(12) 0.43273(12) 0.09627(9) 0.0239(3) Uani 1 1 d . . . H20A H 0.4896 0.5057 0.0917 0.029 Uiso 1 1 calc R . . H20B H 0.5504 0.4022 0.0347 0.029 Uiso 1 1 calc R . . P2 P 0.65232(3) 0.43593(3) 0.12522(2) 0.01839(6) Uani 1 1 d . . . C211 C 0.73769(12) 0.30945(11) 0.08516(9) 0.0205(2) Uani 1 1 d . . . N212 N 0.72211(12) 0.26525(11) 0.01725(9) 0.0268(3) Uani 1 1 d . . . C213 C 0.78205(15) 0.17139(13) -0.00905(12) 0.0316(3) Uani 1 1 d . . . H213 H 0.7708 0.1384 -0.0563 0.038 Uiso 1 1 calc R . . C214 C 0.85897(16) 0.11964(13) 0.02802(13) 0.0324(4) Uani 1 1 d . . . H214 H 0.8993 0.0531 0.0067 0.039 Uiso 1 1 calc R . . C215 C 0.87645(15) 0.16651(15) 0.09715(13) 0.0340(4) Uani 1 1 d . . . H215 H 0.9292 0.1334 0.124 0.041 Uiso 1 1 calc R . . C216 C 0.81401(14) 0.26371(14) 0.12585(11) 0.0305(3) Uani 1 1 d . . . H216 H 0.8237 0.2984 0.1729 0.037 Uiso 1 1 calc R . . C221 C 0.73608(12) 0.53171(11) 0.03682(9) 0.0217(3) Uani 1 1 d . . . N222 N 0.84972(13) 0.50989(13) 0.00780(12) 0.0353(4) Uani 1 1 d . . . C223 C 0.91487(18) 0.58309(17) -0.05010(15) 0.0433(5) Uani 1 1 d . . . H223 H 0.9963 0.5686 -0.0713 0.052 Uiso 1 1 calc R . . C224 C 0.86972(17) 0.67826(15) -0.08036(12) 0.0335(4) Uani 1 1 d . . . H224 H 0.9187 0.7281 -0.1202 0.04 Uiso 1 1 calc R . . C225 C 0.75149(16) 0.69825(12) -0.05078(11) 0.0299(3) Uani 1 1 d . . . H225 H 0.7177 0.7616 -0.0717 0.036 Uiso 1 1 calc R . . C226 C 0.68200(15) 0.62473(12) 0.01000(11) 0.0269(3) Uani 1 1 d . . . H226 H 0.6003 0.6375 0.0325 0.032 Uiso 1 1 calc R . . P3 P 0.64157(3) 0.34849(2) 0.38102(2) 0.01379(5) Uani 1 1 d . . . C311 C 0.79456(10) 0.35417(10) 0.35699(8) 0.0171(2) Uani 1 1 d . . . N312 N 0.81273(10) 0.44942(10) 0.37427(10) 0.0251(3) Uani 1 1 d . . . C313 C 0.92021(14) 0.46230(14) 0.36389(14) 0.0345(4) Uani 1 1 d . . . H313 H 0.934 0.5287 0.3771 0.041 Uiso 1 1 calc R . . C314 C 1.01279(14) 0.38398(16) 0.33484(14) 0.0363(4) Uani 1 1 d . . . H314 H 1.0877 0.3967 0.3282 0.044 Uiso 1 1 calc R . . C315 C 0.99293(13) 0.28750(14) 0.31595(12) 0.0296(3) Uani 1 1 d . . . H315 H 1.0543 0.2326 0.2955 0.035 Uiso 1 1 calc R . . C316 C 0.88130(11) 0.27138(12) 0.32722(9) 0.0215(3) Uani 1 1 d . . . H316 H 0.8653 0.2055 0.3148 0.026 Uiso 1 1 calc R . . C321 C 0.63159(11) 0.20645(10) 0.38366(9) 0.0176(2) Uani 1 1 d . . . N322 N 0.66513(11) 0.14459(9) 0.44683(9) 0.0236(2) Uani 1 1 d . . . C323 C 0.65791(16) 0.04079(11) 0.45058(13) 0.0313(4) Uani 1 1 d . . . H323 H 0.6818 -0.0039 0.494 0.038 Uiso 1 1 calc R . . C324 C 0.61688(18) -0.00516(12) 0.39354(14) 0.0362(4) Uani 1 1 d . . . H324 H 0.6122 -0.0792 0.3989 0.043 Uiso 1 1 calc R . . C325 C 0.58385(17) 0.05797(13) 0.33036(14) 0.0367(4) Uani 1 1 d . . . H325 H 0.5564 0.0286 0.2905 0.044 Uiso 1 1 calc R . . C326 C 0.59089(13) 0.16674(12) 0.32494(11) 0.0257(3) Uani 1 1 d . . . H326 H 0.568 0.2125 0.2815 0.031 Uiso 1 1 calc R . . C30 C 0.58663(10) 0.36902(9) 0.50791(8) 0.0156(2) Uani 1 1 d . . . H30A H 0.639 0.3257 0.5344 0.019 Uiso 1 1 calc R . . H30B H 0.5902 0.444 0.5157 0.019 Uiso 1 1 calc R . . C40 C 0.46427(10) 0.34221(9) 0.56497(8) 0.0162(2) Uani 1 1 d . . . H40A H 0.4596 0.2665 0.5607 0.019 Uiso 1 1 calc R . . H40B H 0.4103 0.3846 0.5395 0.019 Uiso 1 1 calc R . . P4 P 0.42335(3) 0.37057(2) 0.68811(2) 0.01529(6) Uani 1 1 d . . . C411 C 0.28627(11) 0.31202(10) 0.74448(9) 0.0193(2) Uani 1 1 d . . . N412 N 0.28808(12) 0.21101(11) 0.72865(11) 0.0309(3) Uani 1 1 d . . . C413 C 0.18947(15) 0.16640(14) 0.76844(15) 0.0365(4) Uani 1 1 d . . . H413 H 0.1897 0.0955 0.7554 0.044 Uiso 1 1 calc R . . C414 C 0.08745(15) 0.21767(17) 0.82738(14) 0.0369(4) Uani 1 1 d . . . H414 H 0.0199 0.1823 0.8554 0.044 Uiso 1 1 calc R . . C415 C 0.08590(14) 0.32127(16) 0.84459(14) 0.0355(4) Uani 1 1 d . . . H415 H 0.0171 0.3586 0.8851 0.043 Uiso 1 1 calc R . . C416 C 0.18729(13) 0.37098(13) 0.80156(11) 0.0267(3) Uani 1 1 d . . . H416 H 0.1884 0.4428 0.8111 0.032 Uiso 1 1 calc R . . C421 C 0.51827(11) 0.27410(10) 0.72825(8) 0.0169(2) Uani 1 1 d . . . N422 N 0.53466(11) 0.30336(10) 0.80245(8) 0.0219(2) Uani 1 1 d . . . C423 C 0.60221(13) 0.23634(12) 0.83683(10) 0.0263(3) Uani 1 1 d . . . H423 H 0.6142 0.2562 0.8892 0.032 Uiso 1 1 calc R . . C424 C 0.65544(14) 0.13960(12) 0.79992(11) 0.0275(3) Uani 1 1 d . . . H424 H 0.7021 0.0944 0.8267 0.033 Uiso 1 1 calc R . . C425 C 0.63889(14) 0.11100(12) 0.72361(11) 0.0273(3) Uani 1 1 d . . . H425 H 0.6752 0.0459 0.6962 0.033 Uiso 1 1 calc R . . C426 C 0.56860(13) 0.17820(10) 0.68707(9) 0.0221(3) Uani 1 1 d . . . H426 H 0.555 0.1593 0.6351 0.026 Uiso 1 1 calc R . . Cl1 Cl 1.11300(5) 0.04571(4) 0.16417(3) 0.04183(14) Uani 0.8878(14) 1 d P . . Cl1' Cl 1.0792(4) 0.0064(4) 0.1704(3) 0.0374(9) Uiso 0.1122(14) 1 d P . . N101 N 0.5090(3) -0.1044(2) 0.8868(3) 0.1041(14) Uani 1 1 d . . . C101 C 0.4460(3) -0.0316(2) 0.9078(2) 0.0658(8) Uani 1 1 d . . . C102 C 0.3662(3) 0.0621(2) 0.9352(2) 0.0620(8) Uani 1 1 d . . . H10C H 0.4086 0.1218 0.9316 0.093 Uiso 1 1 calc R . . H10D H 0.311 0.0507 0.9995 0.093 Uiso 1 1 calc R . . H10E H 0.3246 0.0775 0.893 0.093 Uiso 1 1 calc R . . N201 N 1.1367(2) -0.1003(2) 0.48290(15) 0.0257(3) Uani 0.5 1 d PD A -3 C201 C 1.0680(2) -0.0509(3) 0.54777(17) 0.0257(3) Uani 0.5 1 d PD A -3 C202 C 0.9888(2) 0.0174(2) 0.62548(17) 0.0257(3) Uani 0.5 1 d PD A -3 H20C H 0.9236 -0.0209 0.6662 0.039 Uiso 0.5 1 calc PR A -3 H20D H 0.9601 0.0826 0.5987 0.039 Uiso 0.5 1 calc PRD A -3 H20E H 1.0309 0.0348 0.6622 0.039 Uiso 0.5 1 calc PRD A -3 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 Cu1 0.01405(5) 0.01384(6) 0.01563(5) -0.00031(4) -0.00669(4) -0.00036(4) P1 0.01574(11) 0.01715(12) 0.02243(12) 0.00089(10) -0.01016(9) -0.00253(10) C111 0.0174(4) 0.0202(5) 0.0350(6) 0.0069(4) -0.0139(4) -0.0040(4) N112 0.0272(5) 0.0322(6) 0.0295(5) 0.0089(5) -0.0110(4) -0.0096(5) C113 0.0324(7) 0.0390(8) 0.0403(8) 0.0192(7) -0.0122(6) -0.0086(7) C114 0.0259(7) 0.0288(7) 0.0650(11) 0.0211(7) -0.0125(7) -0.0062(6) C115 0.0297(6) 0.0219(6) 0.0770(12) 0.0132(7) -0.0239(7) -0.0103(5) C116 0.0277(6) 0.0228(6) 0.0483(8) 0.0040(6) -0.0180(6) -0.0073(5) C121 0.0152(4) 0.0187(5) 0.0276(5) 0.0020(4) -0.0103(4) -0.0031(4) N122 0.0196(4) 0.0289(5) 0.0285(5) 0.0057(4) -0.0122(4) -0.0010(4) C123 0.0248(6) 0.0327(7) 0.0399(7) 0.0095(6) -0.0164(5) 0.0013(5) C124 0.0242(6) 0.0297(7) 0.0472(8) 0.0063(6) -0.0143(6) 0.0026(6) C125 0.0252(6) 0.0301(7) 0.0448(8) -0.0073(6) -0.0123(6) 0.0053(6) C126 0.0224(5) 0.0262(6) 0.0326(6) -0.0060(5) -0.0125(4) 0.0009(5) C10 0.0238(5) 0.0243(5) 0.0289(5) -0.0046(4) -0.0156(4) -0.0009(4) C20 0.0261(5) 0.0272(6) 0.0216(5) -0.0012(4) -0.0141(4) 0.0015(5) P2 0.01870(12) 0.02142(13) 0.01529(11) -0.00037(10) -0.00763(9) 0.00000(11) C211 0.0211(5) 0.0224(5) 0.0168(4) -0.0001(4) -0.0066(4) -0.0009(4) N212 0.0289(5) 0.0252(5) 0.0287(5) -0.0049(4) -0.0139(4) 0.0009(4) C213 0.0325(7) 0.0278(6) 0.0351(7) -0.0089(5) -0.0131(5) 0.0009(6) C214 0.0275(7) 0.0254(6) 0.0356(7) -0.0012(6) -0.0050(6) 0.0034(6) C215 0.0293(7) 0.0356(8) 0.0335(7) -0.0020(6) -0.0124(5) 0.0090(6) C216 0.0328(6) 0.0335(7) 0.0260(5) -0.0037(5) -0.0156(5) 0.0083(6) C221 0.0242(5) 0.0234(5) 0.0157(4) -0.0003(4) -0.0066(4) -0.0002(4) N222 0.0232(6) 0.0348(7) 0.0390(7) 0.0124(6) -0.0068(5) -0.0010(5) C223 0.0271(7) 0.0446(9) 0.0452(9) 0.0179(8) -0.0049(7) -0.0044(7) C224 0.0366(8) 0.0335(7) 0.0250(6) 0.0080(5) -0.0074(6) -0.0073(6) C225 0.0372(7) 0.0216(6) 0.0271(6) 0.0012(5) -0.0096(5) -0.0006(6) C226 0.0313(6) 0.0220(6) 0.0247(5) -0.0009(4) -0.0096(5) 0.0020(5) P3 0.01347(10) 0.01252(11) 0.01537(10) 0.00008(8) -0.00597(8) -0.00064(9) C311 0.0143(4) 0.0198(5) 0.0162(4) 0.0008(4) -0.0055(3) -0.0014(4) N312 0.0184(4) 0.0216(5) 0.0357(6) -0.0012(4) -0.0096(4) -0.0060(4) C313 0.0211(5) 0.0309(7) 0.0522(9) -0.0030(6) -0.0120(6) -0.0100(5) C314 0.0170(5) 0.0452(9) 0.0473(9) 0.0010(7) -0.0125(5) -0.0069(6) C315 0.0163(5) 0.0360(7) 0.0343(7) -0.0007(6) -0.0096(5) 0.0025(5) C316 0.0169(4) 0.0245(5) 0.0219(5) -0.0001(4) -0.0076(4) 0.0014(4) C321 0.0164(4) 0.0144(4) 0.0207(4) -0.0020(4) -0.0060(4) -0.0003(4) N322 0.0288(5) 0.0148(4) 0.0271(5) 0.0019(4) -0.0121(4) -0.0002(4) C323 0.0368(7) 0.0138(5) 0.0384(7) 0.0008(5) -0.0107(6) 0.0002(5) C324 0.0408(8) 0.0175(5) 0.0444(9) -0.0059(6) -0.0076(7) -0.0071(6) C325 0.0402(7) 0.0271(6) 0.0463(8) -0.0131(6) -0.0160(6) -0.0087(6) C326 0.0262(5) 0.0250(6) 0.0293(6) -0.0054(5) -0.0127(4) -0.0046(5) C30 0.0155(4) 0.0153(4) 0.0163(4) 0.0005(3) -0.0066(3) -0.0024(3) C40 0.0152(4) 0.0153(4) 0.0182(4) -0.0005(3) -0.0062(3) -0.0026(3) P4 0.01419(11) 0.01326(11) 0.01641(11) -0.00044(9) -0.00388(9) -0.00123(9) C411 0.0158(4) 0.0195(5) 0.0192(5) 0.0003(4) -0.0032(4) -0.0026(4) N412 0.0224(5) 0.0236(5) 0.0392(7) -0.0028(5) -0.0012(5) -0.0091(4) C413 0.0273(6) 0.0292(7) 0.0468(9) 0.0020(6) -0.0051(6) -0.0138(6) C414 0.0218(6) 0.0466(9) 0.0375(8) 0.0052(7) -0.0041(6) -0.0162(6) C415 0.0164(6) 0.0460(9) 0.0359(8) -0.0046(7) -0.0005(5) -0.0033(6) C416 0.0181(5) 0.0307(6) 0.0275(6) -0.0053(5) -0.0040(4) -0.0013(5) C421 0.0159(4) 0.0156(4) 0.0170(4) 0.0009(3) -0.0043(3) -0.0016(4) N422 0.0248(4) 0.0200(4) 0.0220(4) -0.0017(4) -0.0105(4) -0.0007(4) C423 0.0291(5) 0.0264(6) 0.0267(5) -0.0005(5) -0.0156(4) 0.0004(5) C424 0.0274(6) 0.0245(6) 0.0306(6) 0.0024(5) -0.0140(5) 0.0024(5) C425 0.0280(6) 0.0206(5) 0.0295(6) -0.0005(5) -0.0095(5) 0.0053(5) C426 0.0272(5) 0.0167(5) 0.0213(5) -0.0023(4) -0.0093(4) 0.0018(4) Cl1 0.0460(3) 0.0394(2) 0.02736(18) 0.00145(16) -0.00904(17) 0.0190(2) N101 0.083(2) 0.0444(11) 0.139(3) -0.0167(15) 0.015(2) -0.0223(13) C101 0.0661(15) 0.0478(11) 0.0631(15) -0.0166(10) 0.0074(12) -0.0268(11) C102 0.0677(16) 0.0399(10) 0.0552(14) -0.0049(10) 0.0050(12) -0.0152(11) N201 0.0205(5) 0.0381(8) 0.0153(5) 0.0040(5) -0.0069(4) 0.0026(6) C201 0.0205(5) 0.0381(8) 0.0153(5) 0.0040(5) -0.0069(4) 0.0026(6) C202 0.0205(5) 0.0381(8) 0.0153(5) 0.0040(5) -0.0069(4) 0.0026(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Cu1 P4 2.2740(4) 2_666 ? Cu1 P3 2.2818(4) . ? Cu1 P1 2.3184(4) . ? Cu1 P2 2.3212(4) . ? P1 C111 1.8318(14) . ? P1 C10 1.8340(15) . ? P1 C121 1.8465(13) . ? C111 N112 1.339(2) . ? C111 C116 1.394(2) . ? N112 C113 1.348(2) . ? C113 C114 1.378(3) . ? C113 H113 0.95 . ? C114 C115 1.356(4) . ? C114 H114 0.95 . ? C115 C116 1.394(3) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 N122 1.341(2) . ? C121 C126 1.397(2) . ? N122 C123 1.347(2) . ? C123 C124 1.380(3) . ? C123 H123 0.95 . ? C124 C125 1.385(3) . ? C124 H124 0.95 . ? C125 C126 1.391(2) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C10 C20 1.531(2) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C20 P2 1.8332(16) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? P2 C211 1.8379(14) . ? P2 C221 1.8382(14) . ? C211 N212 1.340(2) . ? C211 C216 1.385(2) . ? N212 C213 1.339(2) . ? C213 C214 1.378(3) . ? C213 H213 0.95 . ? C214 C215 1.388(3) . ? C214 H214 0.95 . ? C215 C216 1.393(2) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 N222 1.328(2) . ? C221 C226 1.396(2) . ? N222 C223 1.351(3) . ? C223 C224 1.387(3) . ? C223 H223 0.95 . ? C224 C225 1.379(3) . ? C224 H224 0.95 . ? C225 C226 1.394(2) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? P3 C321 1.8352(13) . ? P3 C311 1.8371(13) . ? P3 C30 1.8513(12) . ? C311 N312 1.3453(19) . ? C311 C316 1.3880(18) . ? N312 C313 1.340(2) . ? C313 C314 1.393(2) . ? C313 H313 0.95 . ? C314 C315 1.378(3) . ? C314 H314 0.95 . ? C315 C316 1.399(2) . ? C315 H315 0.95 . ? C316 H316 0.95 . ? C321 N322 1.3553(19) . ? C321 C326 1.378(2) . ? N322 C323 1.3381(19) . ? C323 C324 1.401(3) . ? C323 H323 0.95 . ? C324 C325 1.360(3) . ? C324 H324 0.95 . ? C325 C326 1.399(2) . ? C325 H325 0.95 . ? C326 H326 0.95 . ? C30 C40 1.5225(16) . ? C30 H30A 0.99 . ? C30 H30B 0.99 . ? C40 P4 1.8392(13) . ? C40 H40A 0.99 . ? C40 H40B 0.99 . ? P4 C421 1.8350(13) . ? P4 C411 1.8392(13) . ? P4 Cu1 2.2740(4) 2_666 ? C411 N412 1.337(2) . ? C411 C416 1.3921(19) . ? N412 C413 1.338(2) . ? C413 C414 1.381(3) . ? C413 H413 0.95 . ? C414 C415 1.377(3) . ? C414 H414 0.95 . ? C415 C416 1.404(2) . ? C415 H415 0.95 . ? C416 H416 0.95 . ? C421 N422 1.3475(19) . ? C421 C426 1.3976(18) . ? N422 C423 1.345(2) . ? C423 C424 1.390(2) . ? C423 H423 0.95 . ? C424 C425 1.376(3) . ? C424 H424 0.95 . ? C425 C426 1.390(2) . ? C425 H425 0.95 . ? C426 H426 0.95 . ? N101 C101 1.125(4) . ? C101 C102 1.441(4) . ? C102 H10C 0.98 . ? C102 H10D 0.98 . ? C102 H10E 0.98 . ? N201 C201 1.212(3) . ? C201 C202 1.504(4) . ? C202 H20C 0.98 . ? C202 H20D 0.98 . ? C202 H20E 0.98 . ? 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 P4 Cu1 P3 109.222(14) 2_666 . ? P4 Cu1 P1 115.734(13) 2_666 . ? P3 Cu1 P1 113.835(13) . . ? P4 Cu1 P2 110.009(13) 2_666 . ? P3 Cu1 P2 119.026(13) . . ? P1 Cu1 P2 87.911(14) . . ? C111 P1 C10 104.38(7) . . ? C111 P1 C121 99.17(6) . . ? C10 P1 C121 102.46(7) . . ? C111 P1 Cu1 123.66(5) . . ? C10 P1 Cu1 104.41(5) . . ? C121 P1 Cu1 120.09(5) . . ? N112 C111 C116 123.08(14) . . ? N112 C111 P1 112.32(11) . . ? C116 C111 P1 124.53(13) . . ? C111 N112 C113 117.49(17) . . ? N112 C113 C114 122.1(2) . . ? N112 C113 H113 118.9 . . ? C114 C113 H113 118.9 . . ? C115 C114 C113 120.66(17) . . ? C115 C114 H114 119.7 . . ? C113 C114 H114 119.7 . . ? C114 C115 C116 118.39(19) . . ? C114 C115 H115 120.8 . . ? C116 C115 H115 120.8 . . ? C111 C116 C115 118.26(19) . . ? C111 C116 H116 120.9 . . ? C115 C116 H116 120.9 . . ? N122 C121 C126 123.76(13) . . ? N122 C121 P1 116.68(10) . . ? C126 C121 P1 119.56(11) . . ? C121 N122 C123 116.82(14) . . ? N122 C123 C124 123.56(17) . . ? N122 C123 H123 118.2 . . ? C124 C123 H123 118.2 . . ? C123 C124 C125 118.95(16) . . ? C123 C124 H124 120.5 . . ? C125 C124 H124 120.5 . . ? C124 C125 C126 118.93(16) . . ? C124 C125 H125 120.5 . . ? C126 C125 H125 120.5 . . ? C125 C126 C121 117.96(16) . . ? C125 C126 H126 121 . . ? C121 C126 H126 121 . . ? C20 C10 P1 109.39(10) . . ? C20 C10 H10A 109.8 . . ? P1 C10 H10A 109.8 . . ? C20 C10 H10B 109.8 . . ? P1 C10 H10B 109.8 . . ? H10A C10 H10B 108.2 . . ? C10 C20 P2 110.85(10) . . ? C10 C20 H20A 109.5 . . ? P2 C20 H20A 109.5 . . ? C10 C20 H20B 109.5 . . ? P2 C20 H20B 109.5 . . ? H20A C20 H20B 108.1 . . ? C20 P2 C211 102.85(7) . . ? C20 P2 C221 103.64(7) . . ? C211 P2 C221 102.29(6) . . ? C20 P2 Cu1 103.33(4) . . ? C211 P2 Cu1 117.93(4) . . ? C221 P2 Cu1 124.06(5) . . ? N212 C211 C216 122.90(13) . . ? N212 C211 P2 117.59(11) . . ? C216 C211 P2 119.50(12) . . ? C213 N212 C211 116.92(15) . . ? N212 C213 C214 124.17(18) . . ? N212 C213 H213 117.9 . . ? C214 C213 H213 117.9 . . ? C213 C214 C215 118.76(15) . . ? C213 C214 H214 120.6 . . ? C215 C214 H214 120.6 . . ? C214 C215 C216 117.77(17) . . ? C214 C215 H215 121.1 . . ? C216 C215 H215 121.1 . . ? C211 C216 C215 119.46(17) . . ? C211 C216 H216 120.3 . . ? C215 C216 H216 120.3 . . ? N222 C221 C226 123.55(14) . . ? N222 C221 P2 115.04(11) . . ? C226 C221 P2 121.16(11) . . ? C221 N222 C223 117.19(15) . . ? N222 C223 C224 123.79(18) . . ? N222 C223 H223 118.1 . . ? C224 C223 H223 118.1 . . ? C225 C224 C223 117.96(16) . . ? C225 C224 H224 121 . . ? C223 C224 H224 121 . . ? C224 C225 C226 119.51(15) . . ? C224 C225 H225 120.2 . . ? C226 C225 H225 120.2 . . ? C225 C226 C221 117.97(15) . . ? C225 C226 H226 121 . . ? C221 C226 H226 121 . . ? C321 P3 C311 103.14(6) . . ? C321 P3 C30 100.67(6) . . ? C311 P3 C30 96.76(6) . . ? C321 P3 Cu1 118.06(5) . . ? C311 P3 Cu1 114.36(4) . . ? C30 P3 Cu1 120.44(4) . . ? N312 C311 C316 123.35(13) . . ? N312 C311 P3 111.18(9) . . ? C316 C311 P3 125.45(11) . . ? C313 N312 C311 117.15(13) . . ? N312 C313 C314 123.76(17) . . ? N312 C313 H313 118.1 . . ? C314 C313 H313 118.1 . . ? C315 C314 C313 118.26(16) . . ? C315 C314 H314 120.9 . . ? C313 C314 H314 120.9 . . ? C314 C315 C316 119.24(14) . . ? C314 C315 H315 120.4 . . ? C316 C315 H315 120.4 . . ? C311 C316 C315 118.22(14) . . ? C311 C316 H316 120.9 . . ? C315 C316 H316 120.9 . . ? N322 C321 C326 122.81(12) . . ? N322 C321 P3 116.10(11) . . ? C326 C321 P3 121.09(11) . . ? C323 N322 C321 117.25(15) . . ? N322 C323 C324 123.15(17) . . ? N322 C323 H323 118.4 . . ? C324 C323 H323 118.4 . . ? C325 C324 C323 118.85(15) . . ? C325 C324 H324 120.6 . . ? C323 C324 H324 120.6 . . ? C324 C325 C326 119.05(18) . . ? C324 C325 H325 120.5 . . ? C326 C325 H325 120.5 . . ? C321 C326 C325 118.88(16) . . ? C321 C326 H326 120.6 . . ? C325 C326 H326 120.6 . . ? C40 C30 P3 115.83(9) . . ? C40 C30 H30A 108.3 . . ? P3 C30 H30A 108.3 . . ? C40 C30 H30B 108.3 . . ? P3 C30 H30B 108.3 . . ? H30A C30 H30B 107.4 . . ? C30 C40 P4 109.72(9) . . ? C30 C40 H40A 109.7 . . ? P4 C40 H40A 109.7 . . ? C30 C40 H40B 109.7 . . ? P4 C40 H40B 109.7 . . ? H40A C40 H40B 108.2 . . ? C421 P4 C40 104.02(6) . . ? C421 P4 C411 100.66(6) . . ? C40 P4 C411 101.45(6) . . ? C421 P4 Cu1 114.25(5) . 2_666 ? C40 P4 Cu1 115.87(4) . 2_666 ? C411 P4 Cu1 118.34(4) . 2_666 ? N412 C411 C416 122.75(13) . . ? N412 C411 P4 116.56(10) . . ? C416 C411 P4 120.68(11) . . ? C411 N412 C413 117.90(14) . . ? N412 C413 C414 123.64(17) . . ? N412 C413 H413 118.2 . . ? C414 C413 H413 118.2 . . ? C415 C414 C413 118.44(16) . . ? C415 C414 H414 120.8 . . ? C413 C414 H414 120.8 . . ? C414 C415 C416 119.10(15) . . ? C414 C415 H415 120.5 . . ? C416 C415 H415 120.5 . . ? C411 C416 C415 118.12(15) . . ? C411 C416 H416 120.9 . . ? C415 C416 H416 120.9 . . ? N422 C421 C426 122.42(13) . . ? N422 C421 P4 113.86(9) . . ? C426 C421 P4 123.72(11) . . ? C423 N422 C421 117.54(12) . . ? N422 C423 C424 123.59(15) . . ? N422 C423 H423 118.2 . . ? C424 C423 H423 118.2 . . ? C425 C424 C423 118.33(15) . . ? C425 C424 H424 120.8 . . ? C423 C424 H424 120.8 . . ? C424 C425 C426 119.39(14) . . ? C424 C425 H425 120.3 . . ? C426 C425 H425 120.3 . . ? C425 C426 C421 118.72(14) . . ? C425 C426 H426 120.6 . . ? C421 C426 H426 120.6 . . ? N101 C101 C102 179.3(5) . . ? C101 C102 H10C 109.5 . . ? C101 C102 H10D 109.5 . . ? H10C C102 H10D 109.5 . . ? C101 C102 H10E 109.5 . . ? H10C C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? N201 C201 C202 175.5(3) . . ? 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 P4 Cu1 P1 C111 -118.50(6) 2_666 . . . ? P3 Cu1 P1 C111 9.27(6) . . . . ? P2 Cu1 P1 C111 130.25(6) . . . . ? P4 Cu1 P1 C10 122.87(5) 2_666 . . . ? P3 Cu1 P1 C10 -109.36(5) . . . . ? P2 Cu1 P1 C10 11.62(5) . . . . ? P4 Cu1 P1 C121 8.89(5) 2_666 . . . ? P3 Cu1 P1 C121 136.66(5) . . . . ? P2 Cu1 P1 C121 -102.36(5) . . . . ? C10 P1 C111 N112 176.23(11) . . . . ? C121 P1 C111 N112 -78.28(12) . . . . ? Cu1 P1 C111 N112 57.59(12) . . . . ? C10 P1 C111 C116 -6.55(14) . . . . ? C121 P1 C111 C116 98.94(13) . . . . ? Cu1 P1 C111 C116 -125.20(12) . . . . ? C116 C111 N112 C113 -1.4(2) . . . . ? P1 C111 N112 C113 175.85(13) . . . . ? C111 N112 C113 C114 0.8(3) . . . . ? N112 C113 C114 C115 -0.5(3) . . . . ? C113 C114 C115 C116 0.7(3) . . . . ? N112 C111 C116 C115 1.7(2) . . . . ? P1 C111 C116 C115 -175.26(13) . . . . ? C114 C115 C116 C111 -1.3(3) . . . . ? C111 P1 C121 N122 -111.47(12) . . . . ? C10 P1 C121 N122 -4.42(12) . . . . ? Cu1 P1 C121 N122 110.58(11) . . . . ? C111 P1 C121 C126 68.80(13) . . . . ? C10 P1 C121 C126 175.85(12) . . . . ? Cu1 P1 C121 C126 -69.14(12) . . . . ? C126 C121 N122 C123 1.9(2) . . . . ? P1 C121 N122 C123 -177.82(12) . . . . ? C121 N122 C123 C124 -0.8(2) . . . . ? N122 C123 C124 C125 -0.8(3) . . . . ? C123 C124 C125 C126 1.3(3) . . . . ? C124 C125 C126 C121 -0.3(2) . . . . ? N122 C121 C126 C125 -1.4(2) . . . . ? P1 C121 C126 C125 178.34(12) . . . . ? C111 P1 C10 C20 -171.44(10) . . . . ? C121 P1 C10 C20 85.55(10) . . . . ? Cu1 P1 C10 C20 -40.39(10) . . . . ? P1 C10 C20 P2 55.54(11) . . . . ? C10 C20 P2 C211 80.91(10) . . . . ? C10 C20 P2 C221 -172.83(10) . . . . ? C10 C20 P2 Cu1 -42.30(10) . . . . ? P4 Cu1 P2 C20 -103.58(5) 2_666 . . . ? P3 Cu1 P2 C20 129.35(5) . . . . ? P1 Cu1 P2 C20 13.10(5) . . . . ? P4 Cu1 P2 C211 143.82(6) 2_666 . . . ? P3 Cu1 P2 C211 16.75(6) . . . . ? P1 Cu1 P2 C211 -99.50(6) . . . . ? P4 Cu1 P2 C221 13.34(6) 2_666 . . . ? P3 Cu1 P2 C221 -113.73(6) . . . . ? P1 Cu1 P2 C221 130.03(6) . . . . ? C20 P2 C211 N212 24.91(12) . . . . ? C221 P2 C211 N212 -82.39(12) . . . . ? Cu1 P2 C211 N212 137.77(9) . . . . ? C20 P2 C211 C216 -154.74(12) . . . . ? C221 P2 C211 C216 97.96(13) . . . . ? Cu1 P2 C211 C216 -41.87(13) . . . . ? C216 C211 N212 C213 1.8(2) . . . . ? P2 C211 N212 C213 -177.83(12) . . . . ? C211 N212 C213 C214 -1.2(2) . . . . ? N212 C213 C214 C215 0.1(3) . . . . ? C213 C214 C215 C216 0.5(3) . . . . ? N212 C211 C216 C215 -1.3(2) . . . . ? P2 C211 C216 C215 178.33(13) . . . . ? C214 C215 C216 C211 0.1(3) . . . . ? C20 P2 C221 N222 -144.89(13) . . . . ? C211 P2 C221 N222 -38.21(15) . . . . ? Cu1 P2 C221 N222 98.34(13) . . . . ? C20 P2 C221 C226 40.73(14) . . . . ? C211 P2 C221 C226 147.42(13) . . . . ? Cu1 P2 C221 C226 -76.04(14) . . . . ? C226 C221 N222 C223 0.6(3) . . . . ? P2 C221 N222 C223 -173.65(16) . . . . ? C221 N222 C223 C224 -0.1(3) . . . . ? N222 C223 C224 C225 -1.2(3) . . . . ? C223 C224 C225 C226 1.9(3) . . . . ? C224 C225 C226 C221 -1.5(3) . . . . ? N222 C221 C226 C225 0.2(3) . . . . ? P2 C221 C226 C225 174.10(13) . . . . ? P4 Cu1 P3 C321 172.78(4) 2_666 . . . ? P1 Cu1 P3 C321 41.73(5) . . . . ? P2 Cu1 P3 C321 -59.78(5) . . . . ? P4 Cu1 P3 C311 -65.61(5) 2_666 . . . ? P1 Cu1 P3 C311 163.34(5) . . . . ? P2 Cu1 P3 C311 61.83(5) . . . . ? P4 Cu1 P3 C30 48.96(5) 2_666 . . . ? P1 Cu1 P3 C30 -82.09(5) . . . . ? P2 Cu1 P3 C30 176.40(5) . . . . ? C321 P3 C311 N312 -165.42(10) . . . . ? C30 P3 C311 N312 -62.76(11) . . . . ? Cu1 P3 C311 N312 65.09(11) . . . . ? C321 P3 C311 C316 13.00(13) . . . . ? C30 P3 C311 C316 115.66(12) . . . . ? Cu1 P3 C311 C316 -116.49(11) . . . . ? C316 C311 N312 C313 -1.7(2) . . . . ? P3 C311 N312 C313 176.81(13) . . . . ? C311 N312 C313 C314 1.3(3) . . . . ? N312 C313 C314 C315 -0.2(3) . . . . ? C313 C314 C315 C316 -0.5(3) . . . . ? N312 C311 C316 C315 1.0(2) . . . . ? P3 C311 C316 C315 -177.28(11) . . . . ? C314 C315 C316 C311 0.2(2) . . . . ? C311 P3 C321 N322 57.75(11) . . . . ? C30 P3 C321 N322 -41.85(11) . . . . ? Cu1 P3 C321 N322 -175.06(8) . . . . ? C311 P3 C321 C326 -122.94(11) . . . . ? C30 P3 C321 C326 137.45(11) . . . . ? Cu1 P3 C321 C326 4.25(12) . . . . ? C326 C321 N322 C323 0.3(2) . . . . ? P3 C321 N322 C323 179.54(11) . . . . ? C321 N322 C323 C324 -0.6(2) . . . . ? N322 C323 C324 C325 0.8(3) . . . . ? C323 C324 C325 C326 -0.6(3) . . . . ? N322 C321 C326 C325 -0.1(2) . . . . ? P3 C321 C326 C325 -179.35(12) . . . . ? C324 C325 C326 C321 0.3(2) . . . . ? C321 P3 C30 C40 -59.87(10) . . . . ? C311 P3 C30 C40 -164.66(9) . . . . ? Cu1 P3 C30 C40 71.88(9) . . . . ? P3 C30 C40 P4 -178.57(6) . . . . ? C30 C40 P4 C421 -66.69(9) . . . . ? C30 C40 P4 C411 -170.87(8) . . . . ? C30 C40 P4 Cu1 59.59(9) . . . 2_666 ? C421 P4 C411 N412 -53.38(14) . . . . ? C40 P4 C411 N412 53.45(14) . . . . ? Cu1 P4 C411 N412 -178.58(11) 2_666 . . . ? C421 P4 C411 C416 125.66(13) . . . . ? C40 P4 C411 C416 -127.50(13) . . . . ? Cu1 P4 C411 C416 0.46(15) 2_666 . . . ? C416 C411 N412 C413 1.3(3) . . . . ? P4 C411 N412 C413 -179.73(15) . . . . ? C411 N412 C413 C414 -2.4(3) . . . . ? N412 C413 C414 C415 1.7(3) . . . . ? C413 C414 C415 C416 0.3(3) . . . . ? N412 C411 C416 C415 0.6(3) . . . . ? P4 C411 C416 C415 -178.41(14) . . . . ? C414 C415 C416 C411 -1.3(3) . . . . ? C40 P4 C421 N422 156.67(9) . . . . ? C411 P4 C421 N422 -98.54(10) . . . . ? Cu1 P4 C421 N422 29.38(10) 2_666 . . . ? C40 P4 C421 C426 -24.00(12) . . . . ? C411 P4 C421 C426 80.78(12) . . . . ? Cu1 P4 C421 C426 -151.29(10) 2_666 . . . ? C426 C421 N422 C423 -0.07(19) . . . . ? P4 C421 N422 C423 179.27(10) . . . . ? C421 N422 C423 C424 0.1(2) . . . . ? N422 C423 C424 C425 0.5(2) . . . . ? C423 C424 C425 C426 -1.1(2) . . . . ? C424 C425 C426 C421 1.1(2) . . . . ? N422 C421 C426 C425 -0.5(2) . . . . ? P4 C421 C426 C425 -179.81(11) . . . . ? data_mn6 #===END _database_code_depnum_ccdc_archive 'CCDC 717472' _audit_creation_date 2008-12-08T14:30:04-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C94 H89 Br2 Cu2 N19 P8' _chemical_formula_moiety 'C88 H80 Cu2 N16 P8, 3(C2 H3 N), 2(Br)' _chemical_formula_weight 2019.5 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7223(6) _cell_length_b 12.7701(8) _cell_length_c 15.1170(9) _cell_angle_alpha 84.684(5) _cell_angle_beta 67.697(5) _cell_angle_gamma 84.046(4) _cell_volume 2256.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 19330 _cell_measurement_theta_min 2.7743 _cell_measurement_theta_max 34.7156 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1034 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.558 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.91029 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0009 _diffrn_orient_matrix_ub_11 -0.0066293897 _diffrn_orient_matrix_ub_12 -0.0290464221 _diffrn_orient_matrix_ub_13 -0.035088733 _diffrn_orient_matrix_ub_21 -0.0226448608 _diffrn_orient_matrix_ub_22 0.046383183 _diffrn_orient_matrix_ub_23 -0.0178887287 _diffrn_orient_matrix_ub_31 0.0555605164 _diffrn_orient_matrix_ub_32 0.0110312982 _diffrn_orient_matrix_ub_33 -0.032011735 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_unetI/netI 0.0648 _diffrn_reflns_number 44238 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 34.84 _diffrn_reflns_theta_full 32 _diffrn_measured_fraction_theta_full 0.98 _diffrn_measured_fraction_theta_max 0.93 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 18283 _reflns_number_gt 11497 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0814P)^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_number_reflns 18283 _refine_ls_number_parameters 573 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0824 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.15 _refine_ls_wR_factor_gt 0.1431 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.116 _refine_diff_density_min -1.251 _refine_diff_density_rms 0.099 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cu1 Cu 0.57832(2) 0.464678(19) 0.279235(17) 0.01603(6) Uani 1 1 d . . . P1 P 0.41105(5) 0.41408(5) 0.27507(4) 0.02300(12) Uani 1 1 d . . . C111 C 0.32275(19) 0.31451(19) 0.3565(2) 0.0290(5) Uani 1 1 d . . . N112 N 0.29408(19) 0.33227(17) 0.44880(17) 0.0343(5) Uani 1 1 d . . . C113 C 0.2249(2) 0.2670(2) 0.5147(2) 0.0421(7) Uani 1 1 d . . . H113 H 0.2042 0.2796 0.5804 0.051 Uiso 1 1 calc R . . C114 C 0.1819(3) 0.1820(2) 0.4921(3) 0.0455(7) Uani 1 1 d . . . H114 H 0.1326 0.1377 0.5409 0.055 Uiso 1 1 calc R . . C115 C 0.2133(2) 0.1639(2) 0.3960(2) 0.0417(7) Uani 1 1 d . . . H115 H 0.1866 0.1058 0.3778 0.05 Uiso 1 1 calc R . . C116 C 0.2838(2) 0.2313(2) 0.3270(2) 0.0342(6) Uani 1 1 d . . . H116 H 0.3052 0.221 0.2608 0.041 Uiso 1 1 calc R . . C121 C 0.29716(18) 0.51734(18) 0.28003(16) 0.0223(4) Uani 1 1 d . . . N122 N 0.27430(17) 0.54198(17) 0.20088(14) 0.0279(4) Uani 1 1 d . . . C123 C 0.1936(2) 0.6199(2) 0.20603(19) 0.0334(5) Uani 1 1 d . . . H123 H 0.1761 0.6382 0.1506 0.04 Uiso 1 1 calc R . . C124 C 0.1343(2) 0.6753(2) 0.2866(2) 0.0331(5) Uani 1 1 d . . . H124 H 0.0791 0.731 0.2856 0.04 Uiso 1 1 calc R . . C125 C 0.1567(2) 0.6479(2) 0.36895(19) 0.0309(5) Uani 1 1 d . . . H125 H 0.1166 0.6837 0.4259 0.037 Uiso 1 1 calc R . . C126 C 0.23884(19) 0.56748(19) 0.36598(17) 0.0264(5) Uani 1 1 d . . . H126 H 0.2558 0.5462 0.4213 0.032 Uiso 1 1 calc R . . C10 C 0.4519(2) 0.3625(2) 0.15693(19) 0.0322(5) Uani 1 1 d . . . H10A H 0.4789 0.2871 0.1593 0.039 Uiso 1 1 calc R . . H10B H 0.3848 0.3678 0.1383 0.039 Uiso 1 1 calc R . . C20 C 0.5459(2) 0.4241(2) 0.08273(17) 0.0316(5) Uani 1 1 d . . . H20A H 0.515 0.4968 0.0732 0.038 Uiso 1 1 calc R . . H20B H 0.5728 0.3904 0.0208 0.038 Uiso 1 1 calc R . . P2 P 0.66564(5) 0.42905(5) 0.12028(4) 0.02201(12) Uani 1 1 d . . . C211 C 0.74883(19) 0.30311(18) 0.08542(16) 0.0243(4) Uani 1 1 d . . . N212 N 0.73921(19) 0.25545(18) 0.01302(16) 0.0341(5) Uani 1 1 d . . . C213 C 0.7996(2) 0.1633(2) -0.0111(2) 0.0420(7) Uani 1 1 d . . . H213 H 0.7949 0.1297 -0.0628 0.05 Uiso 1 1 calc R . . C214 C 0.8665(2) 0.1153(2) 0.0334(2) 0.0447(7) Uani 1 1 d . . . H214 H 0.9056 0.0487 0.0143 0.054 Uiso 1 1 calc R . . C215 C 0.8781(2) 0.1625(3) 0.1059(2) 0.0485(8) Uani 1 1 d . . . H215 H 0.926 0.13 0.1375 0.058 Uiso 1 1 calc R . . C216 C 0.8172(2) 0.2614(2) 0.13355(19) 0.0381(6) Uani 1 1 d . . . H216 H 0.8236 0.2972 0.1834 0.046 Uiso 1 1 calc R . . C221 C 0.7511(2) 0.52449(19) 0.03053(15) 0.0266(5) Uani 1 1 d . . . N222 N 0.6930(2) 0.6162(2) 0.01921(18) 0.0460(6) Uani 1 1 d . . . C223 C 0.7552(3) 0.6930(2) -0.0431(2) 0.0512(8) Uani 1 1 d . . . H223 H 0.7166 0.7583 -0.0528 0.061 Uiso 1 1 calc R . . C224 C 0.8703(3) 0.6788(3) -0.0915(2) 0.0518(8) Uani 1 1 d . . . H224 H 0.9117 0.7335 -0.1328 0.062 Uiso 1 1 calc R . . C225 C 0.9241(3) 0.5836(3) -0.0788(2) 0.0530(8) Uani 1 1 d . . . H225 H 1.0037 0.5716 -0.1132 0.064 Uiso 1 1 calc R . . C226 C 0.8651(2) 0.5045(2) -0.01707(18) 0.0330(5) Uani 1 1 d . . . H226 H 0.9027 0.4385 -0.0081 0.04 Uiso 1 1 calc R . . P3 P 0.64047(4) 0.35733(4) 0.38029(4) 0.01553(10) Uani 1 1 d . . . C311 C 0.79058(17) 0.36549(17) 0.36265(14) 0.0185(4) Uani 1 1 d . A . N312 N 0.80948(16) 0.46264(16) 0.37791(15) 0.0267(4) Uani 1 1 d . . . C313 C 0.9149(2) 0.4778(2) 0.37187(19) 0.0336(6) Uani 1 1 d . A . H313 H 0.9294 0.5459 0.3831 0.04 Uiso 1 1 calc R . . C314 C 1.0031(2) 0.4007(2) 0.35040(18) 0.0348(6) Uani 1 1 d . . . H314 H 1.0764 0.4154 0.3468 0.042 Uiso 1 1 calc R A . C315 C 0.9830(2) 0.3021(2) 0.33421(18) 0.0313(5) Uani 1 1 d . A . H315 H 1.0425 0.2473 0.3192 0.038 Uiso 1 1 calc R . . C316 C 0.87505(18) 0.28298(19) 0.34002(16) 0.0242(4) Uani 1 1 d . . . H316 H 0.8593 0.2154 0.3288 0.029 Uiso 1 1 calc R A . C321 C 0.6288(5) 0.2119(5) 0.3830(5) 0.0218(16) Uiso 0.5 1 d P A 1 N322 N 0.5791(5) 0.1844(5) 0.3200(5) 0.0408(16) Uiso 0.5 1 d P A 1 C323 C 0.5702(7) 0.0682(8) 0.3249(7) 0.063(2) Uiso 0.5 1 d P A 1 H323 H 0.5442 0.0384 0.2823 0.076 Uiso 0.5 1 calc PR A 1 C324 C 0.5983(8) 0.0077(7) 0.3880(7) 0.065(2) Uiso 0.5 1 d P A 1 H324 H 0.5851 -0.065 0.3948 0.077 Uiso 0.5 1 calc PR A 1 C325 C 0.6446(7) 0.0443(6) 0.4426(6) 0.053(2) Uiso 0.5 1 d P A 1 H325 H 0.6679 -0.004 0.4846 0.063 Uiso 0.5 1 calc PR A 1 C326 C 0.6600(5) 0.1463(5) 0.4415(5) 0.0256(15) Uiso 0.5 1 d P A 1 H326 H 0.6929 0.1704 0.4821 0.031 Uiso 0.5 1 calc PR A 1 C331 C 0.6225(4) 0.2218(4) 0.3694(4) 0.0111(11) Uiso 0.5 1 d P A 2 N332 N 0.5714(4) 0.2093(4) 0.3085(3) 0.0230(10) Uiso 0.5 1 d P A 2 C333 C 0.5513(4) 0.1067(4) 0.3054(3) 0.0199(8) Uiso 0.5 1 d P A 2 H333 H 0.5127 0.0936 0.2651 0.024 Uiso 0.5 1 calc PR A 2 C334 C 0.5814(4) 0.0211(4) 0.3546(4) 0.0235(9) Uiso 0.5 1 d P A 2 H334 H 0.5648 -0.0475 0.3469 0.028 Uiso 0.5 1 calc PR A 2 C335 C 0.6350(4) 0.0347(4) 0.4145(4) 0.0223(9) Uiso 0.5 1 d P A 2 H335 H 0.6594 -0.0235 0.4478 0.027 Uiso 0.5 1 calc PR A 2 C336 C 0.6528(5) 0.1385(5) 0.4251(4) 0.0219(13) Uiso 0.5 1 d P A 2 H336 H 0.6851 0.1526 0.4696 0.026 Uiso 0.5 1 calc PR A 2 C30 C 0.58246(16) 0.37352(15) 0.51113(14) 0.0157(3) Uani 1 1 d . A . H30A H 0.6342 0.3324 0.5388 0.019 Uiso 1 1 calc R . . H30B H 0.5834 0.4487 0.5217 0.019 Uiso 1 1 calc R . . C40 C 0.46223(16) 0.33988(16) 0.56593(14) 0.0169(4) Uani 1 1 d . . . H40A H 0.4598 0.264 0.5587 0.02 Uiso 1 1 calc R A . H40B H 0.4086 0.3804 0.5399 0.02 Uiso 1 1 calc R . . P4 P 0.42031(4) 0.36411(4) 0.69278(4) 0.01646(10) Uani 1 1 d . . . C411 C 0.28497(17) 0.30105(17) 0.74530(15) 0.0197(4) Uani 1 1 d . . . N412 N 0.28882(18) 0.19986(17) 0.72824(17) 0.0346(5) Uani 1 1 d . A . C413 C 0.1912(2) 0.1523(2) 0.7614(2) 0.0357(6) Uani 1 1 d . . . H413 H 0.1936 0.0809 0.7475 0.043 Uiso 1 1 calc R A . C414 C 0.0872(2) 0.2015(2) 0.81468(19) 0.0343(6) Uani 1 1 d . A . H414 H 0.0198 0.1648 0.838 0.041 Uiso 1 1 calc R . . C415 C 0.0845(2) 0.3061(3) 0.8330(2) 0.0478(8) Uani 1 1 d . . . H415 H 0.0146 0.3428 0.8692 0.057 Uiso 1 1 calc R A . C416 C 0.1856(2) 0.3572(2) 0.79777(19) 0.0334(6) Uani 1 1 d . A . H416 H 0.1858 0.4289 0.8097 0.04 Uiso 1 1 calc R . . C421 C 0.51590(17) 0.26827(16) 0.72964(15) 0.0192(4) Uani 1 1 d . . . N422 N 0.53269(19) 0.2866(2) 0.81192(16) 0.0390(5) Uani 1 1 d . A . C423 C 0.6031(3) 0.2139(3) 0.8404(2) 0.0498(9) Uani 1 1 d . . . H423 H 0.6143 0.2226 0.8979 0.06 Uiso 1 1 calc R A . C424 C 0.6577(3) 0.1289(3) 0.7869(3) 0.0539(9) Uani 1 1 d . A . H424 H 0.7076 0.0799 0.8061 0.065 Uiso 1 1 calc R . . C425 C 0.6385(2) 0.1165(2) 0.7056(3) 0.0499(8) Uani 1 1 d . . . H425 H 0.6756 0.0575 0.6689 0.06 Uiso 1 1 calc R A . C426 C 0.56821(19) 0.18517(16) 0.67488(18) 0.0241(4) Uani 1 1 d . A . H426 H 0.5564 0.1755 0.6179 0.029 Uiso 1 1 calc R . . Br1 Br 1.08106(8) 0.03288(4) 0.21497(7) 0.0637(3) Uani 0.833(2) 1 d P B 1 Br1' Br 1.0268(3) 0.0115(2) 0.2886(4) 0.0675(15) Uani 0.167(2) 1 d PD B 2 N101 N 0.5166(4) -0.1073(3) 0.9154(3) 0.0745(10) Uani 1 1 d . . . C101 C 0.4486(4) -0.0377(3) 0.9207(3) 0.0594(10) Uani 1 1 d . . . C102 C 0.3641(4) 0.0508(3) 0.9314(4) 0.0777(13) Uani 1 1 d . . . H10C H 0.4024 0.1149 0.9013 0.117 Uiso 1 1 calc R . . H10D H 0.3207 0.0603 0.9996 0.117 Uiso 1 1 calc R . . H10E H 0.3122 0.0369 0.9005 0.117 Uiso 1 1 calc R . . N201 N 1.1074(6) -0.0940(6) 0.4929(6) 0.080(3) Uani 0.5 1 d PD C -3 C201 C 1.0342(7) -0.0287(7) 0.4969(7) 0.070(2) Uiso 0.5 1 d PD C -3 C202 C 0.9344(10) 0.0706(10) 0.5227(9) 0.091(4) Uiso 0.5 1 d PD C -3 H20C H 0.8937 0.0737 0.4788 0.136 Uiso 0.5 1 calc PR C -3 H20D H 0.97 0.137 0.5156 0.136 Uiso 0.5 1 calc PR C -3 H20E H 0.8806 0.0599 0.5887 0.136 Uiso 0.5 1 calc PR C -3 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 Cu1 0.01449(11) 0.01860(12) 0.01597(12) -0.00304(9) -0.00683(9) 0.00085(8) P1 0.0189(3) 0.0248(3) 0.0294(3) -0.0070(2) -0.0128(2) 0.0001(2) C111 0.0224(10) 0.0223(11) 0.0496(15) -0.0008(10) -0.0228(10) 0.0010(8) N112 0.0358(11) 0.0309(11) 0.0447(13) 0.0061(9) -0.0246(10) -0.0097(9) C113 0.0412(15) 0.0409(16) 0.0521(17) 0.0164(13) -0.0281(13) -0.0137(12) C114 0.0373(15) 0.0351(15) 0.068(2) 0.0140(14) -0.0263(15) -0.0101(12) C115 0.0324(13) 0.0212(12) 0.076(2) -0.0008(13) -0.0245(14) -0.0044(10) C116 0.0256(11) 0.0263(12) 0.0543(16) -0.0076(11) -0.0188(11) 0.0015(9) C121 0.0171(9) 0.0258(11) 0.0262(10) 0.0004(8) -0.0104(8) -0.0036(8) N122 0.0239(9) 0.0339(11) 0.0264(10) 0.0013(8) -0.0106(8) -0.0024(8) C123 0.0302(12) 0.0385(14) 0.0328(13) 0.0071(11) -0.0158(10) -0.0012(10) C124 0.0256(11) 0.0286(12) 0.0445(15) 0.0022(11) -0.0148(11) 0.0033(9) C125 0.0264(11) 0.0305(13) 0.0360(13) -0.0075(10) -0.0116(10) 0.0027(9) C126 0.0254(11) 0.0287(12) 0.0306(12) -0.0050(9) -0.0163(9) -0.0004(9) C10 0.0297(12) 0.0338(13) 0.0420(14) -0.0168(11) -0.0221(11) 0.0058(10) C20 0.0326(12) 0.0409(14) 0.0263(11) -0.0124(10) -0.0172(10) 0.0085(10) P2 0.0227(3) 0.0260(3) 0.0171(2) -0.0051(2) -0.0077(2) 0.0040(2) C211 0.0203(10) 0.0264(11) 0.0209(10) -0.0014(8) -0.0026(8) 0.0012(8) N212 0.0338(11) 0.0321(11) 0.0330(11) -0.0125(9) -0.0065(9) -0.0011(9) C213 0.0416(15) 0.0339(15) 0.0459(16) -0.0171(12) -0.0077(13) -0.0029(12) C214 0.0353(14) 0.0284(14) 0.0568(18) -0.0037(12) -0.0025(13) 0.0021(11) C215 0.0261(13) 0.060(2) 0.0535(18) 0.0189(15) -0.0147(13) 0.0041(12) C216 0.0297(13) 0.0521(17) 0.0305(13) 0.0000(12) -0.0119(11) 0.0073(12) C221 0.0347(12) 0.0274(11) 0.0157(9) -0.0041(8) -0.0080(9) 0.0034(9) N222 0.0569(16) 0.0385(14) 0.0392(13) -0.0080(11) -0.0167(12) 0.0114(12) C223 0.085(3) 0.0302(15) 0.0452(17) -0.0070(13) -0.0345(18) 0.0096(15) C224 0.078(2) 0.0421(18) 0.0344(15) 0.0090(13) -0.0190(16) -0.0192(17) C225 0.0357(16) 0.061(2) 0.0491(18) 0.0032(16) -0.0008(14) -0.0081(15) C226 0.0288(12) 0.0349(14) 0.0304(12) 0.0021(10) -0.0080(10) 0.0039(10) P3 0.0145(2) 0.0160(2) 0.0163(2) -0.00225(17) -0.00583(18) -0.00014(17) C311 0.0151(8) 0.0236(10) 0.0158(9) -0.0007(7) -0.0051(7) -0.0008(7) N312 0.0182(8) 0.0271(10) 0.0323(10) -0.0048(8) -0.0053(8) -0.0047(7) C313 0.0236(11) 0.0381(14) 0.0397(14) -0.0051(11) -0.0093(10) -0.0119(10) C314 0.0175(10) 0.0527(17) 0.0335(13) -0.0035(12) -0.0075(9) -0.0069(10) C315 0.0178(10) 0.0425(14) 0.0329(12) 0.0004(10) -0.0104(9) 0.0027(9) C316 0.0197(10) 0.0282(11) 0.0248(10) -0.0009(8) -0.0093(8) 0.0012(8) C30 0.0162(8) 0.0148(8) 0.0174(8) -0.0006(7) -0.0077(7) -0.0013(7) C40 0.0168(9) 0.0168(9) 0.0174(9) -0.0018(7) -0.0068(7) -0.0006(7) P4 0.0159(2) 0.0161(2) 0.0165(2) -0.00147(18) -0.00545(18) 0.00090(18) C411 0.0178(9) 0.0221(10) 0.0185(9) 0.0017(7) -0.0068(7) -0.0006(7) N412 0.0255(10) 0.0253(10) 0.0451(13) -0.0050(9) -0.0026(9) -0.0067(8) C413 0.0284(12) 0.0289(13) 0.0440(15) 0.0019(11) -0.0063(11) -0.0091(10) C414 0.0213(11) 0.0449(15) 0.0352(13) 0.0071(11) -0.0091(10) -0.0105(10) C415 0.0179(11) 0.0556(19) 0.0610(19) -0.0126(15) -0.0026(12) -0.0029(12) C416 0.0188(10) 0.0356(14) 0.0430(14) -0.0122(11) -0.0071(10) 0.0015(9) C421 0.0163(9) 0.0189(9) 0.0206(9) 0.0022(7) -0.0058(7) -0.0010(7) N422 0.0320(11) 0.0591(16) 0.0291(11) 0.0022(10) -0.0141(9) -0.0111(11) C423 0.0374(15) 0.086(3) 0.0342(14) 0.0218(15) -0.0240(13) -0.0229(16) C424 0.0393(16) 0.0493(19) 0.079(2) 0.0349(18) -0.0361(17) -0.0082(14) C425 0.0341(14) 0.0197(12) 0.092(3) -0.0053(14) -0.0208(16) 0.0083(10) C426 0.0232(10) 0.0144(9) 0.0356(12) -0.0058(8) -0.0124(9) 0.0042(7) Br1 0.0868(5) 0.0381(2) 0.0937(6) -0.0248(3) -0.0669(5) 0.0234(2) Br1' 0.0487(15) 0.0480(13) 0.119(4) -0.0308(17) -0.044(2) 0.0101(10) N101 0.108(3) 0.0350(16) 0.076(2) -0.0106(15) -0.026(2) -0.0075(18) C101 0.088(3) 0.0378(18) 0.053(2) -0.0054(15) -0.0216(19) -0.0235(19) C102 0.075(3) 0.052(2) 0.112(4) 0.013(2) -0.042(3) -0.021(2) N201 0.063(4) 0.075(5) 0.119(6) 0.069(4) -0.060(4) -0.040(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Cu1 P3 2.2677(6) . ? Cu1 P4 2.2681(6) 2_666 ? Cu1 P2 2.2994(6) . ? Cu1 P1 2.3118(6) . ? P1 C10 1.827(3) . ? P1 C111 1.830(3) . ? P1 C121 1.839(2) . ? C111 N112 1.337(4) . ? C111 C116 1.392(3) . ? N112 C113 1.339(3) . ? C113 C114 1.389(4) . ? C113 H113 0.95 . ? C114 C115 1.388(5) . ? C114 H114 0.95 . ? C115 C116 1.385(4) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 N122 1.338(3) . ? C121 C126 1.404(3) . ? N122 C123 1.338(3) . ? C123 C124 1.380(4) . ? C123 H123 0.95 . ? C124 C125 1.387(4) . ? C124 H124 0.95 . ? C125 C126 1.378(3) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C10 C20 1.524(4) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C20 P2 1.825(3) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? P2 C221 1.832(2) . ? P2 C211 1.834(2) . ? C211 N212 1.350(3) . ? C211 C216 1.372(3) . ? N212 C213 1.337(3) . ? C213 C214 1.341(5) . ? C213 H213 0.95 . ? C214 C215 1.361(5) . ? C214 H214 0.95 . ? C215 C216 1.421(4) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 N222 1.352(3) . ? C221 C226 1.361(3) . ? N222 C223 1.378(4) . ? C223 C224 1.368(5) . ? C223 H223 0.95 . ? C224 C225 1.366(5) . ? C224 H224 0.95 . ? C225 C226 1.380(4) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? P3 C331 1.799(5) . ? P3 C311 1.838(2) . ? P3 C30 1.854(2) . ? P3 C321 1.874(7) . ? C311 N312 1.344(3) . ? C311 C316 1.391(3) . ? N312 C313 1.343(3) . ? C313 C314 1.374(4) . ? C313 H313 0.95 . ? C314 C315 1.373(4) . ? C314 H314 0.95 . ? C315 C316 1.389(3) . ? C315 H315 0.95 . ? C316 H316 0.95 . ? C321 C326 1.305(9) . ? C321 N322 1.413(9) . ? N322 C323 1.493(11) . ? C323 C324 1.303(13) . ? C323 H323 0.95 . ? C324 C325 1.322(12) . ? C324 H324 0.95 . ? C325 C326 1.334(10) . ? C325 H325 0.95 . ? C326 H326 0.95 . ? C331 N332 1.342(7) . ? C331 C336 1.409(8) . ? N332 C333 1.369(7) . ? C333 C334 1.369(7) . ? C333 H333 0.95 . ? C334 C335 1.356(8) . ? C334 H334 0.95 . ? C335 C336 1.400(8) . ? C335 H335 0.95 . ? C336 H336 0.95 . ? C30 C40 1.523(3) . ? C30 H30A 0.99 . ? C30 H30B 0.99 . ? C40 P4 1.832(2) . ? C40 H40A 0.99 . ? C40 H40B 0.99 . ? P4 C421 1.835(2) . ? P4 C411 1.837(2) . ? P4 Cu1 2.2681(6) 2_666 ? C411 N412 1.333(3) . ? C411 C416 1.378(3) . ? N412 C413 1.337(3) . ? C413 C414 1.381(4) . ? C413 H413 0.95 . ? C414 C415 1.383(4) . ? C414 H414 0.95 . ? C415 C416 1.398(4) . ? C415 H415 0.95 . ? C416 H416 0.95 . ? C421 C426 1.361(3) . ? C421 N422 1.383(3) . ? N422 C423 1.377(4) . ? C423 C424 1.376(5) . ? C423 H423 0.95 . ? C424 C425 1.367(5) . ? C424 H424 0.95 . ? C425 C426 1.364(4) . ? C425 H425 0.95 . ? C426 H426 0.95 . ? N101 C101 1.159(5) . ? C101 C102 1.453(6) . ? C102 H10C 0.98 . ? C102 H10D 0.98 . ? C102 H10E 0.98 . ? N201 C201 1.171(9) . ? C201 C202 1.660(12) . ? C202 H20C 0.98 . ? C202 H20D 0.98 . ? C202 H20E 0.98 . ? 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 P3 Cu1 P4 110.10(2) . 2_666 ? P3 Cu1 P2 114.96(2) . . ? P4 Cu1 P2 113.54(2) 2_666 . ? P3 Cu1 P1 112.18(2) . . ? P4 Cu1 P1 116.51(2) 2_666 . ? P2 Cu1 P1 88.19(2) . . ? C10 P1 C111 103.77(12) . . ? C10 P1 C121 103.97(11) . . ? C111 P1 C121 98.31(10) . . ? C10 P1 Cu1 104.87(8) . . ? C111 P1 Cu1 125.51(8) . . ? C121 P1 Cu1 117.97(7) . . ? N112 C111 C116 122.5(2) . . ? N112 C111 P1 113.01(18) . . ? C116 C111 P1 124.4(2) . . ? C111 N112 C113 118.1(2) . . ? N112 C113 C114 123.4(3) . . ? N112 C113 H113 118.3 . . ? C114 C113 H113 118.3 . . ? C115 C114 C113 117.9(3) . . ? C115 C114 H114 121.1 . . ? C113 C114 H114 121.1 . . ? C116 C115 C114 119.3(3) . . ? C116 C115 H115 120.3 . . ? C114 C115 H115 120.3 . . ? C115 C116 C111 118.7(3) . . ? C115 C116 H116 120.6 . . ? C111 C116 H116 120.6 . . ? N122 C121 C126 122.9(2) . . ? N122 C121 P1 118.26(17) . . ? C126 C121 P1 118.85(17) . . ? C123 N122 C121 116.7(2) . . ? N122 C123 C124 124.3(2) . . ? N122 C123 H123 117.8 . . ? C124 C123 H123 117.8 . . ? C123 C124 C125 118.7(2) . . ? C123 C124 H124 120.7 . . ? C125 C124 H124 120.7 . . ? C126 C125 C124 118.3(2) . . ? C126 C125 H125 120.9 . . ? C124 C125 H125 120.9 . . ? C125 C126 C121 119.1(2) . . ? C125 C126 H126 120.4 . . ? C121 C126 H126 120.4 . . ? C20 C10 P1 110.47(17) . . ? C20 C10 H10A 109.6 . . ? P1 C10 H10A 109.6 . . ? C20 C10 H10B 109.6 . . ? P1 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C10 C20 P2 111.32(17) . . ? C10 C20 H20A 109.4 . . ? P2 C20 H20A 109.4 . . ? C10 C20 H20B 109.4 . . ? P2 C20 H20B 109.4 . . ? H20A C20 H20B 108 . . ? C20 P2 C221 101.52(12) . . ? C20 P2 C211 103.84(11) . . ? C221 P2 C211 103.11(10) . . ? C20 P2 Cu1 103.12(8) . . ? C221 P2 Cu1 121.88(8) . . ? C211 P2 Cu1 120.35(8) . . ? N212 C211 C216 123.0(2) . . ? N212 C211 P2 117.85(18) . . ? C216 C211 P2 119.2(2) . . ? C213 N212 C211 117.2(2) . . ? N212 C213 C214 124.0(3) . . ? N212 C213 H213 118 . . ? C214 C213 H213 118 . . ? C213 C214 C215 119.7(3) . . ? C213 C214 H214 120.1 . . ? C215 C214 H214 120.1 . . ? C214 C215 C216 118.7(3) . . ? C214 C215 H215 120.7 . . ? C216 C215 H215 120.7 . . ? C211 C216 C215 117.4(3) . . ? C211 C216 H216 121.3 . . ? C215 C216 H216 121.3 . . ? N222 C221 C226 123.6(2) . . ? N222 C221 P2 114.80(19) . . ? C226 C221 P2 121.53(19) . . ? C221 N222 C223 116.8(3) . . ? C224 C223 N222 122.4(3) . . ? C224 C223 H223 118.8 . . ? N222 C223 H223 118.8 . . ? C225 C224 C223 118.1(3) . . ? C225 C224 H224 120.9 . . ? C223 C224 H224 120.9 . . ? C224 C225 C226 121.3(3) . . ? C224 C225 H225 119.3 . . ? C226 C225 H225 119.3 . . ? C221 C226 C225 117.6(3) . . ? C221 C226 H226 121.2 . . ? C225 C226 H226 121.2 . . ? C331 P3 C311 107.10(18) . . ? C331 P3 C30 104.46(18) . . ? C311 P3 C30 96.07(9) . . ? C311 P3 C321 102.9(2) . . ? C30 P3 C321 98.6(2) . . ? C331 P3 Cu1 110.44(18) . . ? C311 P3 Cu1 115.16(7) . . ? C30 P3 Cu1 121.88(6) . . ? C321 P3 Cu1 118.4(2) . . ? N312 C311 C316 122.86(19) . . ? N312 C311 P3 111.11(15) . . ? C316 C311 P3 126.00(17) . . ? C313 N312 C311 117.1(2) . . ? N312 C313 C314 123.8(2) . . ? N312 C313 H313 118.1 . . ? C314 C313 H313 118.1 . . ? C315 C314 C313 118.5(2) . . ? C315 C314 H314 120.7 . . ? C313 C314 H314 120.7 . . ? C314 C315 C316 119.4(2) . . ? C314 C315 H315 120.3 . . ? C316 C315 H315 120.3 . . ? C315 C316 C311 118.2(2) . . ? C315 C316 H316 120.9 . . ? C311 C316 H316 120.9 . . ? C326 C321 N322 125.5(6) . . ? C326 C321 P3 121.3(5) . . ? N322 C321 P3 113.1(5) . . ? C321 N322 C323 111.5(6) . . ? C324 C323 N322 119.7(8) . . ? C324 C323 H323 120.1 . . ? N322 C323 H323 120.1 . . ? C323 C324 C325 122.1(9) . . ? C323 C324 H324 119 . . ? C325 C324 H324 119 . . ? C324 C325 C326 122.8(8) . . ? C324 C325 H325 118.6 . . ? C326 C325 H325 118.6 . . ? C321 C326 C325 118.1(7) . . ? C321 C326 H326 120.9 . . ? C325 C326 H326 120.9 . . ? N332 C331 C336 123.8(5) . . ? N332 C331 P3 113.7(4) . . ? C336 C331 P3 122.4(4) . . ? C331 N332 C333 113.3(5) . . ? C334 C333 N332 126.4(5) . . ? C334 C333 H333 116.8 . . ? N332 C333 H333 116.8 . . ? C335 C334 C333 119.7(5) . . ? C335 C334 H334 120.1 . . ? C333 C334 H334 120.1 . . ? C334 C335 C336 116.9(5) . . ? C334 C335 H335 121.6 . . ? C336 C335 H335 121.6 . . ? C335 C336 C331 119.7(6) . . ? C335 C336 H336 120.1 . . ? C331 C336 H336 120.1 . . ? C40 C30 P3 115.96(14) . . ? C40 C30 H30A 108.3 . . ? P3 C30 H30A 108.3 . . ? C40 C30 H30B 108.3 . . ? P3 C30 H30B 108.3 . . ? H30A C30 H30B 107.4 . . ? C30 C40 P4 109.09(14) . . ? C30 C40 H40A 109.9 . . ? P4 C40 H40A 109.9 . . ? C30 C40 H40B 109.9 . . ? P4 C40 H40B 109.9 . . ? H40A C40 H40B 108.3 . . ? C40 P4 C421 102.35(9) . . ? C40 P4 C411 101.08(9) . . ? C421 P4 C411 101.60(9) . . ? C40 P4 Cu1 113.93(7) . 2_666 ? C421 P4 Cu1 116.88(7) . 2_666 ? C411 P4 Cu1 118.51(7) . 2_666 ? N412 C411 C416 122.8(2) . . ? N412 C411 P4 116.31(16) . . ? C416 C411 P4 120.91(18) . . ? C411 N412 C413 118.2(2) . . ? N412 C413 C414 123.6(3) . . ? N412 C413 H413 118.2 . . ? C414 C413 H413 118.2 . . ? C413 C414 C415 117.7(2) . . ? C413 C414 H414 121.2 . . ? C415 C414 H414 121.2 . . ? C414 C415 C416 119.4(2) . . ? C414 C415 H415 120.3 . . ? C416 C415 H415 120.3 . . ? C411 C416 C415 118.3(2) . . ? C411 C416 H416 120.8 . . ? C415 C416 H416 120.8 . . ? C426 C421 N422 123.4(2) . . ? C426 C421 P4 119.41(17) . . ? N422 C421 P4 117.18(17) . . ? C423 N422 C421 117.3(3) . . ? C424 C423 N422 121.0(3) . . ? C424 C423 H423 119.5 . . ? N422 C423 H423 119.5 . . ? C425 C424 C423 118.6(3) . . ? C425 C424 H424 120.7 . . ? C423 C424 H424 120.7 . . ? C426 C425 C424 122.8(3) . . ? C426 C425 H425 118.6 . . ? C424 C425 H425 118.6 . . ? C421 C426 C425 116.9(3) . . ? C421 C426 H426 121.5 . . ? C425 C426 H426 121.5 . . ? N101 C101 C102 177.3(4) . . ? C101 C102 H10C 109.5 . . ? C101 C102 H10D 109.5 . . ? H10C C102 H10D 109.5 . . ? C101 C102 H10E 109.5 . . ? H10C C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? N201 C201 C202 168.0(10) . . ? 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 P3 Cu1 P1 C10 -109.57(9) . . . . ? P4 Cu1 P1 C10 122.25(9) 2_666 . . . ? P2 Cu1 P1 C10 6.73(9) . . . . ? P3 Cu1 P1 C111 9.90(11) . . . . ? P4 Cu1 P1 C111 -118.28(10) 2_666 . . . ? P2 Cu1 P1 C111 126.20(10) . . . . ? P3 Cu1 P1 C121 135.34(8) . . . . ? P4 Cu1 P1 C121 7.16(9) 2_666 . . . ? P2 Cu1 P1 C121 -108.36(9) . . . . ? C10 P1 C111 N112 173.11(18) . . . . ? C121 P1 C111 N112 -80.20(18) . . . . ? Cu1 P1 C111 N112 53.1(2) . . . . ? C10 P1 C111 C116 -9.9(2) . . . . ? C121 P1 C111 C116 96.8(2) . . . . ? Cu1 P1 C111 C116 -129.87(18) . . . . ? C116 C111 N112 C113 -0.2(4) . . . . ? P1 C111 N112 C113 176.9(2) . . . . ? C111 N112 C113 C114 0.2(4) . . . . ? N112 C113 C114 C115 0.4(4) . . . . ? C113 C114 C115 C116 -1.1(4) . . . . ? C114 C115 C116 C111 1.1(4) . . . . ? N112 C111 C116 C115 -0.5(4) . . . . ? P1 C111 C116 C115 -177.17(19) . . . . ? C10 P1 C121 N122 -6.2(2) . . . . ? C111 P1 C121 N122 -112.74(19) . . . . ? Cu1 P1 C121 N122 109.35(17) . . . . ? C10 P1 C121 C126 174.35(18) . . . . ? C111 P1 C121 C126 67.8(2) . . . . ? Cu1 P1 C121 C126 -70.07(19) . . . . ? C126 C121 N122 C123 1.6(3) . . . . ? P1 C121 N122 C123 -177.80(18) . . . . ? C121 N122 C123 C124 0.2(4) . . . . ? N122 C123 C124 C125 -1.5(4) . . . . ? C123 C124 C125 C126 1.0(4) . . . . ? C124 C125 C126 C121 0.7(4) . . . . ? N122 C121 C126 C125 -2.1(3) . . . . ? P1 C121 C126 C125 177.31(18) . . . . ? C111 P1 C10 C20 -168.14(17) . . . . ? C121 P1 C10 C20 89.49(18) . . . . ? Cu1 P1 C10 C20 -34.99(18) . . . . ? P1 C10 C20 P2 52.9(2) . . . . ? C10 C20 P2 C221 -170.64(17) . . . . ? C10 C20 P2 C211 82.58(18) . . . . ? C10 C20 P2 Cu1 -43.70(18) . . . . ? P3 Cu1 P2 C20 130.40(9) . . . . ? P4 Cu1 P2 C20 -101.56(10) 2_666 . . . ? P1 Cu1 P2 C20 16.70(10) . . . . ? P3 Cu1 P2 C221 -116.86(10) . . . . ? P4 Cu1 P2 C221 11.18(10) 2_666 . . . ? P1 Cu1 P2 C221 129.44(10) . . . . ? P3 Cu1 P2 C211 15.49(9) . . . . ? P4 Cu1 P2 C211 143.54(9) 2_666 . . . ? P1 Cu1 P2 C211 -98.21(9) . . . . ? C20 P2 C211 N212 25.1(2) . . . . ? C221 P2 C211 N212 -80.5(2) . . . . ? Cu1 P2 C211 N212 139.64(16) . . . . ? C20 P2 C211 C216 -154.7(2) . . . . ? C221 P2 C211 C216 99.8(2) . . . . ? Cu1 P2 C211 C216 -40.1(2) . . . . ? C216 C211 N212 C213 0.3(4) . . . . ? P2 C211 N212 C213 -179.45(19) . . . . ? C211 N212 C213 C214 1.3(4) . . . . ? N212 C213 C214 C215 -2.0(5) . . . . ? C213 C214 C215 C216 0.9(4) . . . . ? N212 C211 C216 C215 -1.3(4) . . . . ? P2 C211 C216 C215 178.5(2) . . . . ? C214 C215 C216 C211 0.6(4) . . . . ? C20 P2 C221 N222 51.2(2) . . . . ? C211 P2 C221 N222 158.6(2) . . . . ? Cu1 P2 C221 N222 -62.3(2) . . . . ? C20 P2 C221 C226 -131.5(2) . . . . ? C211 P2 C221 C226 -24.1(2) . . . . ? Cu1 P2 C221 C226 115.0(2) . . . . ? C226 C221 N222 C223 -1.2(4) . . . . ? P2 C221 N222 C223 176.0(2) . . . . ? C221 N222 C223 C224 -0.3(4) . . . . ? N222 C223 C224 C225 1.7(5) . . . . ? C223 C224 C225 C226 -1.7(5) . . . . ? N222 C221 C226 C225 1.2(4) . . . . ? P2 C221 C226 C225 -175.8(2) . . . . ? C224 C225 C226 C221 0.3(5) . . . . ? P4 Cu1 P3 C331 172.62(18) 2_666 . . . ? P2 Cu1 P3 C331 -57.63(18) . . . . ? P1 Cu1 P3 C331 41.12(18) . . . . ? P4 Cu1 P3 C311 -65.92(8) 2_666 . . . ? P2 Cu1 P3 C311 63.83(8) . . . . ? P1 Cu1 P3 C311 162.59(8) . . . . ? P4 Cu1 P3 C30 49.54(8) 2_666 . . . ? P2 Cu1 P3 C30 179.29(7) . . . . ? P1 Cu1 P3 C30 -81.95(8) . . . . ? P4 Cu1 P3 C321 171.9(2) 2_666 . . . ? P2 Cu1 P3 C321 -58.4(2) . . . . ? P1 Cu1 P3 C321 40.4(2) . . . . ? C331 P3 C311 N312 -174.6(2) . . . . ? C30 P3 C311 N312 -67.41(16) . . . . ? C321 P3 C311 N312 -167.6(2) . . . . ? Cu1 P3 C311 N312 62.15(16) . . . . ? C331 P3 C311 C316 3.1(3) . . . . ? C30 P3 C311 C316 110.34(19) . . . . ? C321 P3 C311 C316 10.1(3) . . . . ? Cu1 P3 C311 C316 -120.11(17) . . . . ? C316 C311 N312 C313 -1.0(3) . . . . ? P3 C311 N312 C313 176.87(18) . . . . ? C311 N312 C313 C314 0.6(4) . . . . ? N312 C313 C314 C315 -0.1(4) . . . . ? C313 C314 C315 C316 -0.1(4) . . . . ? C314 C315 C316 C311 -0.3(3) . . . . ? N312 C311 C316 C315 0.8(3) . . . . ? P3 C311 C316 C315 -176.69(18) . . . . ? C331 P3 C321 C326 177(3) . . . . ? C311 P3 C321 C326 53.7(6) . . . . ? C30 P3 C321 C326 -44.6(6) . . . . ? Cu1 P3 C321 C326 -178.0(5) . . . . ? C331 P3 C321 N322 -6(2) . . . . ? C311 P3 C321 N322 -129.0(4) . . . . ? C30 P3 C321 N322 132.7(4) . . . . ? Cu1 P3 C321 N322 -0.8(5) . . . . ? C326 C321 N322 C323 -2.3(10) . . . . ? P3 C321 N322 C323 -179.4(5) . . . . ? C321 N322 C323 C324 5.3(10) . . . . ? N322 C323 C324 C325 -6.3(13) . . . . ? C323 C324 C325 C326 3.9(13) . . . . ? N322 C321 C326 C325 0.2(10) . . . . ? P3 C321 C326 C325 177.0(5) . . . . ? C324 C325 C326 C321 -0.6(11) . . . . ? C311 P3 C331 N332 -129.3(4) . . . . ? C30 P3 C331 N332 129.5(4) . . . . ? C321 P3 C331 N332 172(3) . . . . ? Cu1 P3 C331 N332 -3.2(4) . . . . ? C311 P3 C331 C336 54.8(5) . . . . ? C30 P3 C331 C336 -46.4(5) . . . . ? C321 P3 C331 C336 -4(2) . . . . ? Cu1 P3 C331 C336 -179.1(4) . . . . ? C336 C331 N332 C333 -0.1(7) . . . . ? P3 C331 N332 C333 -175.9(3) . . . . ? C331 N332 C333 C334 -2.2(7) . . . . ? N332 C333 C334 C335 1.1(7) . . . . ? C333 C334 C335 C336 2.4(7) . . . . ? C334 C335 C336 C331 -4.4(8) . . . . ? N332 C331 C336 C335 3.4(8) . . . . ? P3 C331 C336 C335 178.9(4) . . . . ? C331 P3 C30 C40 -52.9(2) . . . . ? C311 P3 C30 C40 -162.37(15) . . . . ? C321 P3 C30 C40 -58.3(2) . . . . ? Cu1 P3 C30 C40 72.89(15) . . . . ? P3 C30 C40 P4 -179.08(10) . . . . ? C30 C40 P4 C421 -67.54(15) . . . . ? C30 C40 P4 C411 -172.18(14) . . . . ? C30 C40 P4 Cu1 59.58(14) . . . 2_666 ? C40 P4 C411 N412 55.9(2) . . . . ? C421 P4 C411 N412 -49.3(2) . . . . ? Cu1 P4 C411 N412 -178.87(16) 2_666 . . . ? C40 P4 C411 C416 -123.0(2) . . . . ? C421 P4 C411 C416 131.8(2) . . . . ? Cu1 P4 C411 C416 2.2(2) 2_666 . . . ? C416 C411 N412 C413 2.0(4) . . . . ? P4 C411 N412 C413 -176.9(2) . . . . ? C411 N412 C413 C414 -2.0(4) . . . . ? N412 C413 C414 C415 1.1(5) . . . . ? C413 C414 C415 C416 -0.2(5) . . . . ? N412 C411 C416 C415 -1.2(4) . . . . ? P4 C411 C416 C415 177.7(2) . . . . ? C414 C415 C416 C411 0.3(5) . . . . ? C40 P4 C421 C426 -18.46(19) . . . . ? C411 P4 C421 C426 85.76(19) . . . . ? Cu1 P4 C421 C426 -143.67(16) 2_666 . . . ? C40 P4 C421 N422 160.11(17) . . . . ? C411 P4 C421 N422 -95.67(18) . . . . ? Cu1 P4 C421 N422 34.90(19) 2_666 . . . ? C426 C421 N422 C423 -2.4(3) . . . . ? P4 C421 N422 C423 179.10(19) . . . . ? C421 N422 C423 C424 2.4(4) . . . . ? N422 C423 C424 C425 -1.5(5) . . . . ? C423 C424 C425 C426 0.5(5) . . . . ? N422 C421 C426 C425 1.4(3) . . . . ? P4 C421 C426 C425 179.92(19) . . . . ? C424 C425 C426 C421 -0.5(4) . . . . ? data_217bp07 _database_code_depnum_ccdc_archive 'CCDC 717473' _audit_creation_date 2008-12-08T11:52:59-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C88 H82 Cu2 I2 N16 O P8' _chemical_formula_moiety 'C88 H80 Cu2 N16 P8,2(I), (H2 O)' _chemical_formula_weight 2008.34 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6523(8) _cell_length_b 12.6343(12) _cell_length_c 14.9936(10) _cell_angle_alpha 83.640(7) _cell_angle_beta 68.207(6) _cell_angle_gamma 86.633(7) _cell_volume 2211.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6501 _cell_measurement_theta_min 3.4895 _cell_measurement_theta_max 66.9129 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description slab _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.025 _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1014 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 7.887 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.59034 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 -0.0523727569 _diffrn_orient_matrix_ub_12 0.0127040647 _diffrn_orient_matrix_ub_13 0.1093732466 _diffrn_orient_matrix_ub_21 -0.0440732199 _diffrn_orient_matrix_ub_22 -0.1141881301 _diffrn_orient_matrix_ub_23 0.0196586609 _diffrn_orient_matrix_ub_31 0.112024915 _diffrn_orient_matrix_ub_32 -0.0415671263 _diffrn_orient_matrix_ub_33 0.0108343074 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_unetI/netI 0.0414 _diffrn_reflns_number 19001 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 69.3 _diffrn_reflns_theta_full 66.5 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.937 _diffrn_measurement_device_type ; Oxford Diffraction Gemini diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 7746 _reflns_number_gt 5882 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1432P)^2^+23.8255P] 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_number_reflns 7746 _refine_ls_number_parameters 533 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1291 _refine_ls_R_factor_gt 0.1064 _refine_ls_wR_factor_ref 0.2955 _refine_ls_wR_factor_gt 0.2757 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.933 _refine_diff_density_min -2.248 _refine_diff_density_rms 0.163 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 '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' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cu1 Cu 0.57270(12) 0.46250(12) 0.28072(9) 0.0445(4) Uani 1 1 d . . . P1 P 0.4029(2) 0.4077(2) 0.28025(18) 0.0477(7) Uani 1 1 d . . . C111 C 0.3095(8) 0.3091(9) 0.3697(7) 0.048(2) Uani 1 1 d . . . N112 N 0.2843(8) 0.3305(8) 0.4610(6) 0.056(2) Uani 1 1 d . . . C113 C 0.2118(11) 0.2657(12) 0.5314(9) 0.069(4) Uani 1 1 d . . . H113 H 0.1909 0.2827 0.596 0.083 Uiso 1 1 calc R . . C114 C 0.1654(10) 0.1759(11) 0.5164(9) 0.065(3) Uani 1 1 d . . . H114 H 0.1175 0.1302 0.5685 0.078 Uiso 1 1 calc R . . C115 C 0.1926(11) 0.1562(12) 0.4208(11) 0.072(4) Uani 1 1 d . . . H115 H 0.1609 0.0968 0.4065 0.087 Uiso 1 1 calc R . . C116 C 0.2647(10) 0.2217(10) 0.3471(8) 0.056(3) Uani 1 1 d . . . H116 H 0.2839 0.208 0.2819 0.067 Uiso 1 1 calc R . . C121 C 0.2991(8) 0.5156(9) 0.2782(7) 0.047(2) Uani 1 1 d . . . N122 N 0.2900(9) 0.5480(9) 0.1930(7) 0.064(3) Uani 1 1 d . . . C123 C 0.2202(12) 0.6324(12) 0.1911(9) 0.074(4) Uani 1 1 d . . . H123 H 0.211 0.656 0.1319 0.089 Uiso 1 1 calc R . . C124 C 0.1615(11) 0.6862(11) 0.2706(10) 0.070(4) Uani 1 1 d . . . H124 H 0.1144 0.7462 0.2656 0.083 Uiso 1 1 calc R . . C125 C 0.1719(9) 0.6521(10) 0.3568(8) 0.058(3) Uani 1 1 d . . . H125 H 0.1323 0.6882 0.4124 0.069 Uiso 1 1 calc R . . C126 C 0.2407(9) 0.5643(10) 0.3620(8) 0.055(3) Uani 1 1 d . . . H126 H 0.2479 0.538 0.4213 0.066 Uiso 1 1 calc R . . C10 C 0.4379(9) 0.3526(10) 0.1636(8) 0.057(3) Uani 1 1 d . . . H10A H 0.4597 0.2763 0.1695 0.069 Uiso 1 1 calc R . . H10B H 0.3705 0.3584 0.1448 0.069 Uiso 1 1 calc R . . C20 C 0.5356(9) 0.4135(9) 0.0872(7) 0.051(3) Uani 1 1 d . . . H20A H 0.5094 0.4871 0.0746 0.061 Uiso 1 1 calc R . . H20B H 0.5596 0.379 0.0264 0.061 Uiso 1 1 calc R . . P2 P 0.6572(2) 0.4181(2) 0.12474(17) 0.0484(7) Uani 1 1 d . . . C211 C 0.7316(9) 0.2888(9) 0.0953(7) 0.052(3) Uani 1 1 d . . . N212 N 0.6982(10) 0.2298(9) 0.0413(8) 0.072(3) Uani 1 1 d . . . C213 C 0.7500(12) 0.1337(11) 0.0238(9) 0.071(4) Uani 1 1 d . . . H213 H 0.7249 0.0889 -0.011 0.085 Uiso 1 1 calc R . . C214 C 0.8373(11) 0.0973(11) 0.0537(9) 0.068(3) Uani 1 1 d . . . H214 H 0.8738 0.0307 0.0366 0.082 Uiso 1 1 calc R . . C215 C 0.8712(10) 0.1578(10) 0.1086(8) 0.062(3) Uani 1 1 d . . . H215 H 0.9301 0.1335 0.1311 0.074 Uiso 1 1 calc R . . C216 C 0.8164(9) 0.2562(10) 0.1302(7) 0.053(3) Uani 1 1 d . . . H216 H 0.8371 0.3001 0.1684 0.064 Uiso 1 1 calc R . . C221 C 0.7506(8) 0.5139(9) 0.0312(6) 0.047(2) Uani 1 1 d . . . N222 N 0.7035(9) 0.6104(9) 0.0214(7) 0.064(3) Uani 1 1 d . . . C223 C 0.7697(11) 0.6874(11) -0.0420(9) 0.066(3) Uani 1 1 d . . . H223 H 0.7364 0.7557 -0.0491 0.079 Uiso 1 1 calc R . . C224 C 0.8804(11) 0.6708(11) -0.0953(8) 0.063(3) Uani 1 1 d . . . H224 H 0.9247 0.7263 -0.1387 0.075 Uiso 1 1 calc R . . C225 C 0.9280(11) 0.5709(12) -0.0851(9) 0.071(4) Uani 1 1 d . . . H225 H 1.0053 0.5568 -0.1232 0.086 Uiso 1 1 calc R . . C226 C 0.8653(10) 0.4935(10) -0.0214(8) 0.057(3) Uani 1 1 d . . . H226 H 0.8988 0.4258 -0.0124 0.068 Uiso 1 1 calc R . . P3 P 0.6348(2) 0.3590(2) 0.38581(17) 0.0437(6) Uani 1 1 d . . . C311 C 0.7861(8) 0.3701(8) 0.3655(7) 0.044(2) Uani 1 1 d . . . N312 N 0.8106(7) 0.4686(8) 0.3778(6) 0.054(2) Uani 1 1 d . . . C313 C 0.9156(10) 0.4869(10) 0.3724(8) 0.060(3) Uani 1 1 d . . . H313 H 0.9333 0.5562 0.3809 0.072 Uiso 1 1 calc R . . C314 C 0.9999(9) 0.4079(11) 0.3550(8) 0.059(3) Uani 1 1 d . . . H314 H 1.0735 0.4227 0.353 0.071 Uiso 1 1 calc R . . C315 C 0.9757(9) 0.3085(11) 0.3406(8) 0.061(3) Uani 1 1 d . . . H315 H 1.0332 0.2543 0.3269 0.073 Uiso 1 1 calc R . . C316 C 0.8675(10) 0.2872(10) 0.3461(8) 0.058(3) Uani 1 1 d . . . H316 H 0.8489 0.2184 0.337 0.07 Uiso 1 1 calc R . . C321 C 0.6167(8) 0.2182(9) 0.3797(7) 0.048(2) Uani 1 1 d . . . N322 N 0.5721(7) 0.2005(8) 0.3134(6) 0.053(2) Uani 1 1 d . . . C323 C 0.5597(11) 0.1002(10) 0.3032(8) 0.062(3) Uani 1 1 d . . . H323 H 0.5273 0.0867 0.2578 0.075 Uiso 1 1 calc R . . C324 C 0.5900(11) 0.0141(11) 0.3530(9) 0.069(3) Uani 1 1 d . . . H324 H 0.5815 -0.0562 0.3402 0.083 Uiso 1 1 calc R . . C325 C 0.6331(11) 0.0313(11) 0.4222(10) 0.071(4) Uani 1 1 d . . . H325 H 0.6542 -0.0267 0.4586 0.086 Uiso 1 1 calc R . . C326 C 0.6450(10) 0.1373(10) 0.4370(8) 0.058(3) Uani 1 1 d . . . H326 H 0.6718 0.1527 0.4853 0.07 Uiso 1 1 calc R . . C30 C 0.5822(8) 0.3736(9) 0.5159(6) 0.044(2) Uani 1 1 d . . . H30A H 0.6334 0.3321 0.5436 0.053 Uiso 1 1 calc R . . H30B H 0.5875 0.4495 0.5244 0.053 Uiso 1 1 calc R . . C40 C 0.4621(8) 0.3388(8) 0.5726(6) 0.044(2) Uani 1 1 d . . . H40A H 0.456 0.262 0.5676 0.053 Uiso 1 1 calc R . . H40B H 0.4096 0.3789 0.5454 0.053 Uiso 1 1 calc R . . P4 P 0.4211(2) 0.3625(2) 0.70072(17) 0.0455(6) Uani 1 1 d . . . C411 C 0.2833(9) 0.2993(9) 0.7542(7) 0.050(3) Uani 1 1 d . . . N412 N 0.2794(7) 0.1951(7) 0.7441(7) 0.052(2) Uani 1 1 d . . . C413 C 0.1809(10) 0.1474(11) 0.7762(8) 0.063(3) Uani 1 1 d . . . H413 H 0.1808 0.0744 0.7664 0.075 Uiso 1 1 calc R . . C414 C 0.0766(11) 0.1966(12) 0.8236(9) 0.068(3) Uani 1 1 d . . . H414 H 0.0071 0.1592 0.8472 0.081 Uiso 1 1 calc R . . C415 C 0.0811(10) 0.3043(11) 0.8342(9) 0.069(3) Uani 1 1 d . . . H415 H 0.0124 0.3428 0.8641 0.083 Uiso 1 1 calc R . . C416 C 0.1826(9) 0.3553(10) 0.8023(8) 0.054(3) Uani 1 1 d . . . H416 H 0.1851 0.4278 0.8126 0.065 Uiso 1 1 calc R . . C421 C 0.5091(9) 0.2625(9) 0.7432(7) 0.050(3) Uani 1 1 d . . . N422 N 0.5095(12) 0.2652(14) 0.8345(9) 0.111(6) Uani 1 1 d . . . C423 C 0.5675(14) 0.1838(17) 0.8676(11) 0.108(7) Uani 1 1 d . . . H423 H 0.5666 0.1817 0.9315 0.13 Uiso 1 1 calc R . . C424 C 0.6265(12) 0.1059(12) 0.8105(10) 0.078(4) Uani 1 1 d . . . H424 H 0.6664 0.0502 0.8333 0.093 Uiso 1 1 calc R . . C425 C 0.6251(10) 0.1122(10) 0.7202(9) 0.064(3) Uani 1 1 d . . . H425 H 0.6686 0.0612 0.6784 0.076 Uiso 1 1 calc R . . C426 C 0.5655(8) 0.1867(7) 0.6866(7) 0.041(2) Uani 1 1 d . . . H426 H 0.5634 0.1857 0.624 0.049 Uiso 1 1 calc R . . O1 O 0.884(2) 0.1100(18) 0.5195(17) 0.098(7) Uani 0.5 1 d P . . I1 I 1.06954(9) 0.02592(7) 0.25032(9) 0.0948(5) 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 Cu1 0.0454(8) 0.0620(9) 0.0367(7) -0.0237(6) -0.0255(6) 0.0225(6) P1 0.0444(13) 0.0682(17) 0.0422(13) -0.0269(12) -0.0271(11) 0.0225(12) C111 0.040(5) 0.067(6) 0.044(5) -0.019(5) -0.021(4) 0.016(5) N112 0.054(5) 0.079(6) 0.043(5) -0.020(5) -0.026(4) 0.016(5) C113 0.066(8) 0.102(10) 0.050(7) -0.025(7) -0.030(6) 0.023(7) C114 0.049(6) 0.088(9) 0.059(7) -0.007(6) -0.023(5) 0.014(6) C115 0.063(8) 0.086(9) 0.090(10) -0.039(8) -0.049(8) 0.033(7) C116 0.051(6) 0.078(8) 0.047(6) -0.019(6) -0.028(5) 0.016(6) C121 0.042(5) 0.064(6) 0.042(5) -0.019(5) -0.024(4) 0.020(5) N122 0.070(6) 0.084(7) 0.051(5) -0.024(5) -0.038(5) 0.033(5) C123 0.080(8) 0.104(10) 0.052(7) -0.030(7) -0.040(6) 0.045(8) C124 0.064(7) 0.085(9) 0.078(8) -0.035(7) -0.045(7) 0.034(6) C125 0.052(6) 0.072(7) 0.058(7) -0.031(6) -0.026(5) 0.019(5) C126 0.055(6) 0.077(7) 0.048(6) -0.027(5) -0.034(5) 0.023(5) C10 0.058(6) 0.080(7) 0.051(6) -0.040(6) -0.037(5) 0.034(6) C20 0.049(6) 0.077(7) 0.038(5) -0.026(5) -0.028(5) 0.023(5) P2 0.0494(14) 0.0696(17) 0.0361(13) -0.0258(12) -0.0251(11) 0.0244(12) C211 0.050(6) 0.068(7) 0.045(5) -0.030(5) -0.022(5) 0.029(5) N212 0.094(8) 0.076(6) 0.079(7) -0.047(6) -0.066(6) 0.044(6) C213 0.087(9) 0.077(8) 0.069(8) -0.036(7) -0.049(7) 0.034(7) C214 0.070(8) 0.076(8) 0.064(7) -0.031(6) -0.031(6) 0.033(6) C215 0.061(7) 0.078(8) 0.057(7) -0.019(6) -0.034(6) 0.030(6) C216 0.051(6) 0.074(7) 0.037(5) -0.014(5) -0.020(5) 0.018(5) C221 0.048(5) 0.073(7) 0.024(4) -0.017(4) -0.018(4) 0.014(5) N222 0.065(6) 0.083(7) 0.053(6) -0.029(5) -0.030(5) 0.026(6) C223 0.064(7) 0.077(8) 0.066(8) -0.025(7) -0.033(6) 0.024(7) C224 0.064(7) 0.085(8) 0.043(6) -0.013(6) -0.023(5) 0.004(6) C225 0.058(7) 0.100(10) 0.051(7) -0.026(7) -0.013(6) 0.021(7) C226 0.053(6) 0.075(7) 0.044(6) -0.020(5) -0.021(5) 0.024(6) P3 0.0435(13) 0.0601(15) 0.0372(12) -0.0219(11) -0.0244(10) 0.0213(11) C311 0.039(5) 0.064(6) 0.037(5) -0.024(4) -0.020(4) 0.020(4) N312 0.043(5) 0.074(6) 0.050(5) -0.027(4) -0.020(4) 0.017(4) C313 0.054(6) 0.077(8) 0.058(7) -0.029(6) -0.026(5) 0.010(6) C314 0.038(5) 0.093(9) 0.050(6) -0.016(6) -0.018(5) 0.006(5) C315 0.048(6) 0.093(9) 0.047(6) -0.032(6) -0.022(5) 0.030(6) C316 0.059(7) 0.079(8) 0.049(6) -0.029(5) -0.033(5) 0.033(6) C321 0.038(5) 0.073(7) 0.036(5) -0.026(5) -0.015(4) 0.022(5) N322 0.050(5) 0.073(6) 0.042(5) -0.026(4) -0.020(4) 0.006(4) C323 0.071(7) 0.075(8) 0.050(6) -0.029(6) -0.029(6) 0.017(6) C324 0.072(8) 0.071(8) 0.067(8) -0.036(6) -0.023(6) 0.014(6) C325 0.074(8) 0.069(8) 0.069(8) -0.017(6) -0.026(7) 0.030(6) C326 0.062(7) 0.067(7) 0.052(6) -0.018(5) -0.027(5) 0.021(5) C30 0.044(5) 0.064(6) 0.034(5) -0.023(4) -0.024(4) 0.017(4) C40 0.048(5) 0.058(6) 0.033(5) -0.025(4) -0.021(4) 0.018(4) P4 0.0459(13) 0.0615(15) 0.0378(13) -0.0247(11) -0.0230(11) 0.0208(11) C411 0.059(6) 0.067(7) 0.035(5) -0.027(5) -0.028(5) 0.031(5) N412 0.044(5) 0.060(5) 0.057(5) -0.016(4) -0.022(4) 0.013(4) C413 0.062(7) 0.077(8) 0.055(7) -0.022(6) -0.028(6) 0.021(6) C414 0.054(7) 0.093(9) 0.066(8) -0.026(7) -0.031(6) 0.015(6) C415 0.049(7) 0.090(9) 0.068(8) -0.034(7) -0.019(6) 0.020(6) C416 0.043(6) 0.068(7) 0.056(6) -0.030(5) -0.021(5) 0.022(5) C421 0.049(6) 0.070(7) 0.043(5) -0.020(5) -0.029(5) 0.023(5) N422 0.113(10) 0.170(14) 0.086(8) -0.081(9) -0.072(8) 0.086(10) C423 0.099(11) 0.180(18) 0.079(10) -0.070(11) -0.068(9) 0.080(12) C424 0.078(9) 0.104(10) 0.067(8) -0.031(7) -0.046(7) 0.046(8) C425 0.064(7) 0.072(7) 0.068(8) -0.030(6) -0.038(6) 0.028(6) C426 0.047(5) 0.046(5) 0.038(5) -0.021(4) -0.023(4) 0.024(4) O1 0.108(16) 0.093(14) 0.111(17) -0.024(12) -0.062(14) 0.030(12) I1 0.1041(8) 0.0725(6) 0.1560(11) -0.0484(6) -0.0997(8) 0.0427(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Cu1 P4 2.269(3) 2_666 ? Cu1 P3 2.269(3) . ? Cu1 P1 2.299(3) . ? Cu1 P2 2.300(3) . ? P1 C111 1.837(12) . ? P1 C121 1.843(9) . ? P1 C10 1.843(9) . ? C111 N112 1.340(13) . ? C111 C116 1.397(16) . ? N112 C113 1.344(18) . ? C113 C114 1.384(19) . ? C113 H113 0.95 . ? C114 C115 1.392(18) . ? C114 H114 0.95 . ? C115 C116 1.37(2) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 N122 1.342(13) . ? C121 C126 1.389(13) . ? N122 C123 1.349(15) . ? C123 C124 1.378(16) . ? C123 H123 0.95 . ? C124 C125 1.367(17) . ? C124 H124 0.95 . ? C125 C126 1.383(15) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C10 C20 1.516(17) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C20 P2 1.831(10) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? P2 C221 1.841(11) . ? P2 C211 1.848(10) . ? C211 N212 1.348(14) . ? C211 C216 1.383(14) . ? N212 C213 1.349(15) . ? C213 C214 1.377(17) . ? C213 H213 0.95 . ? C214 C215 1.372(17) . ? C214 H214 0.95 . ? C215 C216 1.398(15) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 N222 1.343(14) . ? C221 C226 1.395(14) . ? N222 C223 1.361(18) . ? C223 C224 1.348(17) . ? C223 H223 0.95 . ? C224 C225 1.384(19) . ? C224 H224 0.95 . ? C225 C226 1.350(19) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? P3 C321 1.823(11) . ? P3 C311 1.835(10) . ? P3 C30 1.839(9) . ? C311 N312 1.348(14) . ? C311 C316 1.401(13) . ? N312 C313 1.334(14) . ? C313 C314 1.388(16) . ? C313 H313 0.95 . ? C314 C315 1.367(18) . ? C314 H314 0.95 . ? C315 C316 1.382(17) . ? C315 H315 0.95 . ? C316 H316 0.95 . ? C321 N322 1.355(12) . ? C321 C326 1.379(15) . ? N322 C323 1.319(15) . ? C323 C324 1.367(18) . ? C323 H323 0.95 . ? C324 C325 1.380(18) . ? C324 H324 0.95 . ? C325 C326 1.407(18) . ? C325 H325 0.95 . ? C326 H326 0.95 . ? C30 C40 1.505(14) . ? C30 H30A 0.99 . ? C30 H30B 0.99 . ? C40 P4 1.849(8) . ? C40 H40A 0.99 . ? C40 H40B 0.99 . ? P4 C411 1.817(13) . ? P4 C421 1.851(10) . ? P4 Cu1 2.269(3) 2_666 ? C411 N412 1.348(14) . ? C411 C416 1.403(13) . ? N412 C413 1.314(16) . ? C413 C414 1.391(16) . ? C413 H413 0.95 . ? C414 C415 1.394(19) . ? C414 H414 0.95 . ? C415 C416 1.367(18) . ? C415 H415 0.95 . ? C416 H416 0.95 . ? C421 C426 1.341(13) . ? C421 N422 1.374(14) . ? N422 C423 1.38(2) . ? C423 C424 1.372(18) . ? C423 H423 0.95 . ? C424 C425 1.354(17) . ? C424 H424 0.95 . ? C425 C426 1.341(14) . ? C425 H425 0.95 . ? C426 H426 0.95 . ? 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 P4 Cu1 P3 110.73(10) 2_666 . ? P4 Cu1 P1 115.31(10) 2_666 . ? P3 Cu1 P1 113.01(12) . . ? P4 Cu1 P2 115.17(12) 2_666 . ? P3 Cu1 P2 112.94(10) . . ? P1 Cu1 P2 88.08(10) . . ? C111 P1 C121 100.5(5) . . ? C111 P1 C10 104.7(5) . . ? C121 P1 C10 103.7(4) . . ? C111 P1 Cu1 125.1(3) . . ? C121 P1 Cu1 115.0(4) . . ? C10 P1 Cu1 105.6(4) . . ? N112 C111 C116 122.1(11) . . ? N112 C111 P1 113.2(8) . . ? C116 C111 P1 124.6(8) . . ? C111 N112 C113 117.6(10) . . ? N112 C113 C114 124.5(11) . . ? N112 C113 H113 117.8 . . ? C114 C113 H113 117.8 . . ? C113 C114 C115 116.5(13) . . ? C113 C114 H114 121.7 . . ? C115 C114 H114 121.7 . . ? C116 C115 C114 120.4(13) . . ? C116 C115 H115 119.8 . . ? C114 C115 H115 119.8 . . ? C115 C116 C111 118.8(10) . . ? C115 C116 H116 120.6 . . ? C111 C116 H116 120.6 . . ? N122 C121 C126 123.3(9) . . ? N122 C121 P1 117.3(7) . . ? C126 C121 P1 119.2(7) . . ? C121 N122 C123 116.7(9) . . ? N122 C123 C124 123.3(11) . . ? N122 C123 H123 118.4 . . ? C124 C123 H123 118.4 . . ? C125 C124 C123 119.1(11) . . ? C125 C124 H124 120.4 . . ? C123 C124 H124 120.4 . . ? C124 C125 C126 119.2(10) . . ? C124 C125 H125 120.4 . . ? C126 C125 H125 120.4 . . ? C125 C126 C121 118.3(10) . . ? C125 C126 H126 120.8 . . ? C121 C126 H126 120.8 . . ? C20 C10 P1 109.5(7) . . ? C20 C10 H10A 109.8 . . ? P1 C10 H10A 109.8 . . ? C20 C10 H10B 109.8 . . ? P1 C10 H10B 109.8 . . ? H10A C10 H10B 108.2 . . ? C10 C20 P2 111.6(7) . . ? C10 C20 H20A 109.3 . . ? P2 C20 H20A 109.3 . . ? C10 C20 H20B 109.3 . . ? P2 C20 H20B 109.3 . . ? H20A C20 H20B 108 . . ? C20 P2 C221 102.4(5) . . ? C20 P2 C211 103.7(5) . . ? C221 P2 C211 103.3(5) . . ? C20 P2 Cu1 102.5(3) . . ? C221 P2 Cu1 119.6(3) . . ? C211 P2 Cu1 122.4(4) . . ? N212 C211 C216 123.1(9) . . ? N212 C211 P2 117.4(7) . . ? C216 C211 P2 119.5(8) . . ? C211 N212 C213 116.8(9) . . ? N212 C213 C214 123.3(11) . . ? N212 C213 H213 118.3 . . ? C214 C213 H213 118.3 . . ? C215 C214 C213 119.6(11) . . ? C215 C214 H214 120.2 . . ? C213 C214 H214 120.2 . . ? C214 C215 C216 118.0(10) . . ? C214 C215 H215 121 . . ? C216 C215 H215 121 . . ? C211 C216 C215 119.1(10) . . ? C211 C216 H216 120.5 . . ? C215 C216 H216 120.5 . . ? N222 C221 C226 120.7(11) . . ? N222 C221 P2 115.3(8) . . ? C226 C221 P2 123.7(9) . . ? C221 N222 C223 118.6(10) . . ? C224 C223 N222 122.7(12) . . ? C224 C223 H223 118.6 . . ? N222 C223 H223 118.6 . . ? C223 C224 C225 118.3(13) . . ? C223 C224 H224 120.8 . . ? C225 C224 H224 120.8 . . ? C226 C225 C224 120.4(11) . . ? C226 C225 H225 119.8 . . ? C224 C225 H225 119.8 . . ? C225 C226 C221 119.2(11) . . ? C225 C226 H226 120.4 . . ? C221 C226 H226 120.4 . . ? C321 P3 C311 104.6(4) . . ? C321 P3 C30 104.1(5) . . ? C311 P3 C30 95.8(4) . . ? C321 P3 Cu1 111.0(3) . . ? C311 P3 Cu1 115.6(4) . . ? C30 P3 Cu1 123.4(3) . . ? N312 C311 C316 122.2(10) . . ? N312 C311 P3 111.6(6) . . ? C316 C311 P3 126.0(9) . . ? C313 N312 C311 118.6(9) . . ? N312 C313 C314 122.1(11) . . ? N312 C313 H313 118.9 . . ? C314 C313 H313 118.9 . . ? C315 C314 C313 119.3(10) . . ? C315 C314 H314 120.4 . . ? C313 C314 H314 120.4 . . ? C314 C315 C316 119.8(10) . . ? C314 C315 H315 120.1 . . ? C316 C315 H315 120.1 . . ? C315 C316 C311 117.9(11) . . ? C315 C316 H316 121.1 . . ? C311 C316 H316 121.1 . . ? N322 C321 C326 123.0(11) . . ? N322 C321 P3 113.4(8) . . ? C326 C321 P3 123.7(8) . . ? C323 N322 C321 116.6(10) . . ? N322 C323 C324 125.0(11) . . ? N322 C323 H323 117.5 . . ? C324 C323 H323 117.5 . . ? C323 C324 C325 118.8(12) . . ? C323 C324 H324 120.6 . . ? C325 C324 H324 120.6 . . ? C324 C325 C326 117.9(12) . . ? C324 C325 H325 121.1 . . ? C326 C325 H325 121.1 . . ? C321 C326 C325 118.6(11) . . ? C321 C326 H326 120.7 . . ? C325 C326 H326 120.7 . . ? C40 C30 P3 115.7(6) . . ? C40 C30 H30A 108.4 . . ? P3 C30 H30A 108.4 . . ? C40 C30 H30B 108.4 . . ? P3 C30 H30B 108.4 . . ? H30A C30 H30B 107.4 . . ? C30 C40 P4 110.3(6) . . ? C30 C40 H40A 109.6 . . ? P4 C40 H40A 109.6 . . ? C30 C40 H40B 109.6 . . ? P4 C40 H40B 109.6 . . ? H40A C40 H40B 108.1 . . ? C411 P4 C40 101.3(4) . . ? C411 P4 C421 100.2(5) . . ? C40 P4 C421 102.6(4) . . ? C411 P4 Cu1 117.3(3) . 2_666 ? C40 P4 Cu1 112.0(4) . 2_666 ? C421 P4 Cu1 120.6(4) . 2_666 ? N412 C411 C416 119.8(11) . . ? N412 C411 P4 117.6(7) . . ? C416 C411 P4 122.6(9) . . ? C413 N412 C411 119.8(9) . . ? N412 C413 C414 124.5(12) . . ? N412 C413 H413 117.8 . . ? C414 C413 H413 117.8 . . ? C413 C414 C415 115.5(13) . . ? C413 C414 H414 122.2 . . ? C415 C414 H414 122.2 . . ? C416 C415 C414 121.1(11) . . ? C416 C415 H415 119.5 . . ? C414 C415 H415 119.5 . . ? C415 C416 C411 119.2(11) . . ? C415 C416 H416 120.4 . . ? C411 C416 H416 120.4 . . ? C426 C421 N422 122.0(10) . . ? C426 C421 P4 119.4(7) . . ? N422 C421 P4 118.5(8) . . ? C421 N422 C423 117.2(11) . . ? C424 C423 N422 121.5(12) . . ? C424 C423 H423 119.2 . . ? N422 C423 H423 119.2 . . ? C425 C424 C423 117.0(12) . . ? C425 C424 H424 121.5 . . ? C423 C424 H424 121.5 . . ? C426 C425 C424 123.5(10) . . ? C426 C425 H425 118.3 . . ? C424 C425 H425 118.3 . . ? C421 C426 C425 118.6(9) . . ? C421 C426 H426 120.7 . . ? C425 C426 H426 120.7 . . ? 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 P4 Cu1 P1 C111 -117.1(4) 2_666 . . . ? P3 Cu1 P1 C111 11.7(4) . . . . ? P2 Cu1 P1 C111 125.9(4) . . . . ? P4 Cu1 P1 C121 8.0(4) 2_666 . . . ? P3 Cu1 P1 C121 136.8(4) . . . . ? P2 Cu1 P1 C121 -109.0(4) . . . . ? P4 Cu1 P1 C10 121.7(4) 2_666 . . . ? P3 Cu1 P1 C10 -109.6(4) . . . . ? P2 Cu1 P1 C10 4.6(4) . . . . ? C121 P1 C111 N112 -79.2(8) . . . . ? C10 P1 C111 N112 173.5(7) . . . . ? Cu1 P1 C111 N112 51.8(8) . . . . ? C121 P1 C111 C116 98.8(9) . . . . ? C10 P1 C111 C116 -8.5(10) . . . . ? Cu1 P1 C111 C116 -130.1(8) . . . . ? C116 C111 N112 C113 -1.3(15) . . . . ? P1 C111 N112 C113 176.7(8) . . . . ? C111 N112 C113 C114 3.0(17) . . . . ? N112 C113 C114 C115 -3.3(18) . . . . ? C113 C114 C115 C116 2.0(16) . . . . ? C114 C115 C116 C111 -0.6(16) . . . . ? N112 C111 C116 C115 0.2(15) . . . . ? P1 C111 C116 C115 -177.6(8) . . . . ? C111 P1 C121 N122 -122.6(9) . . . . ? C10 P1 C121 N122 -14.5(11) . . . . ? Cu1 P1 C121 N122 100.3(9) . . . . ? C111 P1 C121 C126 62.0(10) . . . . ? C10 P1 C121 C126 170.1(10) . . . . ? Cu1 P1 C121 C126 -75.1(10) . . . . ? C126 C121 N122 C123 0.1(19) . . . . ? P1 C121 N122 C123 -175.1(10) . . . . ? C121 N122 C123 C124 1(2) . . . . ? N122 C123 C124 C125 -1(2) . . . . ? C123 C124 C125 C126 0(2) . . . . ? C124 C125 C126 C121 1.5(18) . . . . ? N122 C121 C126 C125 -1.5(18) . . . . ? P1 C121 C126 C125 173.6(9) . . . . ? C111 P1 C10 C20 -167.1(7) . . . . ? C121 P1 C10 C20 88.0(8) . . . . ? Cu1 P1 C10 C20 -33.3(7) . . . . ? P1 C10 C20 P2 53.0(8) . . . . ? C10 C20 P2 C221 -170.5(7) . . . . ? C10 C20 P2 C211 82.2(8) . . . . ? C10 C20 P2 Cu1 -46.0(7) . . . . ? P4 Cu1 P2 C20 -98.4(4) 2_666 . . . ? P3 Cu1 P2 C20 133.0(4) . . . . ? P1 Cu1 P2 C20 18.8(4) . . . . ? P4 Cu1 P2 C221 13.9(4) 2_666 . . . ? P3 Cu1 P2 C221 -114.7(4) . . . . ? P1 Cu1 P2 C221 131.1(4) . . . . ? P4 Cu1 P2 C211 146.2(4) 2_666 . . . ? P3 Cu1 P2 C211 17.6(5) . . . . ? P1 Cu1 P2 C211 -96.6(5) . . . . ? C20 P2 C211 N212 10.8(11) . . . . ? C221 P2 C211 N212 -95.7(10) . . . . ? Cu1 P2 C211 N212 125.6(9) . . . . ? C20 P2 C211 C216 -168.1(10) . . . . ? C221 P2 C211 C216 85.3(10) . . . . ? Cu1 P2 C211 C216 -53.3(11) . . . . ? C216 C211 N212 C213 2(2) . . . . ? P2 C211 N212 C213 -177.3(10) . . . . ? C211 N212 C213 C214 -4(2) . . . . ? N212 C213 C214 C215 3(2) . . . . ? C213 C214 C215 C216 -1(2) . . . . ? N212 C211 C216 C215 0.4(19) . . . . ? P2 C211 C216 C215 179.3(9) . . . . ? C214 C215 C216 C211 -0.5(18) . . . . ? C20 P2 C221 N222 57.0(8) . . . . ? C211 P2 C221 N222 164.6(7) . . . . ? Cu1 P2 C221 N222 -55.3(8) . . . . ? C20 P2 C221 C226 -128.2(9) . . . . ? C211 P2 C221 C226 -20.7(9) . . . . ? Cu1 P2 C221 C226 119.5(8) . . . . ? C226 C221 N222 C223 0.9(14) . . . . ? P2 C221 N222 C223 175.9(8) . . . . ? C221 N222 C223 C224 -0.1(17) . . . . ? N222 C223 C224 C225 0.5(18) . . . . ? C223 C224 C225 C226 -1.8(18) . . . . ? C224 C225 C226 C221 2.7(18) . . . . ? N222 C221 C226 C225 -2.3(15) . . . . ? P2 C221 C226 C225 -176.8(9) . . . . ? P4 Cu1 P3 C321 174.3(3) 2_666 . . . ? P1 Cu1 P3 C321 43.2(3) . . . . ? P2 Cu1 P3 C321 -54.8(4) . . . . ? P4 Cu1 P3 C311 -66.8(3) 2_666 . . . ? P1 Cu1 P3 C311 162.1(3) . . . . ? P2 Cu1 P3 C311 64.0(3) . . . . ? P4 Cu1 P3 C30 49.9(4) 2_666 . . . ? P1 Cu1 P3 C30 -81.2(4) . . . . ? P2 Cu1 P3 C30 -179.3(4) . . . . ? C321 P3 C311 N312 -173.6(7) . . . . ? C30 P3 C311 N312 -67.4(8) . . . . ? Cu1 P3 C311 N312 64.1(7) . . . . ? C321 P3 C311 C316 2.2(10) . . . . ? C30 P3 C311 C316 108.4(9) . . . . ? Cu1 P3 C311 C316 -120.1(9) . . . . ? C316 C311 N312 C313 -0.9(15) . . . . ? P3 C311 N312 C313 175.1(8) . . . . ? C311 N312 C313 C314 -0.1(17) . . . . ? N312 C313 C314 C315 1.4(18) . . . . ? C313 C314 C315 C316 -1.6(17) . . . . ? C314 C315 C316 C311 0.7(16) . . . . ? N312 C311 C316 C315 0.6(16) . . . . ? P3 C311 C316 C315 -174.8(8) . . . . ? C311 P3 C321 N322 -124.2(7) . . . . ? C30 P3 C321 N322 135.9(7) . . . . ? Cu1 P3 C321 N322 1.1(8) . . . . ? C311 P3 C321 C326 56.1(10) . . . . ? C30 P3 C321 C326 -43.8(10) . . . . ? Cu1 P3 C321 C326 -178.6(8) . . . . ? C326 C321 N322 C323 -2.1(15) . . . . ? P3 C321 N322 C323 178.2(8) . . . . ? C321 N322 C323 C324 -1.1(17) . . . . ? N322 C323 C324 C325 3(2) . . . . ? C323 C324 C325 C326 -0.8(19) . . . . ? N322 C321 C326 C325 3.7(16) . . . . ? P3 C321 C326 C325 -176.5(9) . . . . ? C324 C325 C326 C321 -2.2(18) . . . . ? C321 P3 C30 C40 -56.5(8) . . . . ? C311 P3 C30 C40 -163.1(8) . . . . ? Cu1 P3 C30 C40 71.0(8) . . . . ? P3 C30 C40 P4 -178.2(5) . . . . ? C30 C40 P4 C411 -173.1(7) . . . . ? C30 C40 P4 C421 -69.8(8) . . . . ? C30 C40 P4 Cu1 61.0(7) . . . 2_666 ? C40 P4 C411 N412 58.3(8) . . . . ? C421 P4 C411 N412 -46.9(8) . . . . ? Cu1 P4 C411 N412 -179.4(6) 2_666 . . . ? C40 P4 C411 C416 -119.9(9) . . . . ? C421 P4 C411 C416 134.8(9) . . . . ? Cu1 P4 C411 C416 2.3(9) 2_666 . . . ? C416 C411 N412 C413 2.5(15) . . . . ? P4 C411 N412 C413 -175.8(8) . . . . ? C411 N412 C413 C414 -1.7(17) . . . . ? N412 C413 C414 C415 1.4(19) . . . . ? C413 C414 C415 C416 -2.1(19) . . . . ? C414 C415 C416 C411 3.0(18) . . . . ? N412 C411 C416 C415 -3.2(16) . . . . ? P4 C411 C416 C415 175.1(9) . . . . ? C411 P4 C421 C426 93.6(10) . . . . ? C40 P4 C421 C426 -10.5(11) . . . . ? Cu1 P4 C421 C426 -135.9(8) 2_666 . . . ? C411 P4 C421 N422 -82.9(13) . . . . ? C40 P4 C421 N422 172.9(12) . . . . ? Cu1 P4 C421 N422 47.5(13) 2_666 . . . ? C426 C421 N422 C423 -2(2) . . . . ? P4 C421 N422 C423 174.2(14) . . . . ? C421 N422 C423 C424 3(3) . . . . ? N422 C423 C424 C425 0(3) . . . . ? C423 C424 C425 C426 -3(2) . . . . ? N422 C421 C426 C425 -1(2) . . . . ? P4 C421 C426 C425 -177.3(9) . . . . ? C424 C425 C426 C421 4(2) . . . . ? #===END