# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Yanxiang Cheng' _publ_contact_author_address ; State Key Laboratory of Polymer Physics and Chemistry Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun 130022, P. R. China ; _publ_contact_author_email yanxiang@ciac.jl.cn _publ_contact_author_phone +8643185262106 _publ_contact_author_fax +8643185684937 loop_ _publ_author_name _publ_author_address 'Xiaohui Liu' ;State Key Laboratory of Polymer Physics and Chemistry Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun 130022, P. R. China Graduate University of the Chinese Academy of Sciences Chinese Academy of Sciences Beijing, 100039, P. R. China ; 'Wei Sun' ;State Key Laboratory of Polymer Physics and Chemistry Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun 130022, P. R. China ; 'Luyi Zou' ;State Key Laboratory of Polymer Physics and Chemistry Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun 130022, P. R. China ; 'Zhiyuan Xie' ;State Key Laboratory of Polymer Physics and Chemistry Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun 130022, P. R. China ; 'Xiao Li' ;State Key Laboratory of Polymer Physics and Chemistry Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun 130022, P. R. China ; 'Canzhong Lu' ;State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou 350002, P.R. China ; ; lixiang Wang ; ;State Key Laboratory of Polymer Physics and Chemistry Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun 130022, P. R. China ; 'Yanxiang Cheng' ;State Key Laboratory of Polymer Physics and Chemistry Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun 130022, P. R. China ; data_s314 _database_code_depnum_ccdc_archive 'CCDC 828213' #TrackingRef 'S314.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H39 Cl2 Cu N2 O P2' _chemical_formula_weight 880.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.586(4) _cell_length_b 11.370(4) _cell_length_c 20.412(8) _cell_angle_alpha 96.330(7) _cell_angle_beta 93.891(7) _cell_angle_gamma 103.119(7) _cell_volume 2143.5(14) _cell_formula_units_Z 2 _cell_measurement_temperature 186(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 0.749 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8016 _exptl_absorpt_correction_T_max 0.9316 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 186(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12192 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0927 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 26.15 _reflns_number_total 8309 _reflns_number_gt 4745 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8309 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1275 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.1819 _refine_ls_wR_factor_gt 0.1498 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.86787(6) 0.83079(5) 0.71040(3) 0.0469(2) Uani 1 1 d . . . N1 N 0.9982(4) 0.9219(4) 0.64339(19) 0.0497(10) Uani 1 1 d . . . N2 N 0.9382(4) 0.6904(4) 0.66757(19) 0.0492(10) Uani 1 1 d . . . P1 P 0.62745(13) 0.79627(11) 0.67808(6) 0.0446(3) Uani 1 1 d . . . P2 P 0.91789(13) 0.89178(12) 0.81908(6) 0.0462(3) Uani 1 1 d . . . O1 O 0.6655(3) 0.6933(3) 0.80833(16) 0.0522(8) Uani 1 1 d . . . C1 C 1.0321(6) 1.0410(5) 0.6359(3) 0.0668(15) Uani 1 1 d . . . H1A H 0.9953 1.0955 0.6647 0.080 Uiso 1 1 calc R . . C2 C 1.1167(7) 1.0876(6) 0.5892(3) 0.0755(17) Uani 1 1 d . . . H2A H 1.1378 1.1722 0.5855 0.091 Uiso 1 1 calc R . . C3 C 1.1706(6) 1.0076(6) 0.5474(3) 0.0797(18) Uani 1 1 d . . . H3A H 1.2293 1.0367 0.5142 0.096 Uiso 1 1 calc R . . C4 C 1.1384(6) 0.8864(5) 0.5545(3) 0.0641(15) Uani 1 1 d . . . H4A H 1.1749 0.8309 0.5262 0.077 Uiso 1 1 calc R . . C5 C 1.0524(5) 0.8447(5) 0.6030(2) 0.0503(12) Uani 1 1 d . . . C6 C 1.0167(5) 0.7174(4) 0.6153(2) 0.0492(12) Uani 1 1 d . . . C7 C 1.0454(6) 0.6161(5) 0.5807(3) 0.0625(15) Uani 1 1 d . . . H7A H 1.0989 0.6137 0.5433 0.075 Uiso 1 1 calc R . . C8 C 0.9788(6) 0.5162(5) 0.6123(3) 0.0572(14) Uani 1 1 d . . . C9 C 0.9623(7) 0.3896(6) 0.6011(3) 0.0790(19) Uani 1 1 d . . . H9A H 1.0023 0.3541 0.5648 0.095 Uiso 1 1 calc R . . C10 C 0.8901(7) 0.3194(6) 0.6419(4) 0.085(2) Uani 1 1 d . . . H10A H 0.8788 0.2337 0.6339 0.102 Uiso 1 1 calc R . . C11 C 0.8310(7) 0.3688(5) 0.6957(4) 0.0799(18) Uani 1 1 d . . . H11A H 0.7827 0.3167 0.7245 0.096 Uiso 1 1 calc R . . C12 C 0.8416(6) 0.4925(5) 0.7077(3) 0.0658(15) Uani 1 1 d . . . H12A H 0.7996 0.5258 0.7440 0.079 Uiso 1 1 calc R . . C13 C 0.9150(5) 0.5671(5) 0.6657(2) 0.0521(13) Uani 1 1 d . . . C14 C 0.5861(5) 0.7647(5) 0.5883(2) 0.0513(13) Uani 1 1 d . . . C15 C 0.4954(6) 0.8180(6) 0.5523(3) 0.0803(18) Uani 1 1 d . . . H15A H 0.4533 0.8774 0.5743 0.096 Uiso 1 1 calc R . . C16 C 0.4653(7) 0.7857(8) 0.4846(3) 0.099(2) Uani 1 1 d . . . H16A H 0.4025 0.8226 0.4604 0.119 Uiso 1 1 calc R . . C17 C 0.5252(8) 0.7014(7) 0.4527(3) 0.095(2) Uani 1 1 d . . . H17A H 0.5023 0.6778 0.4064 0.114 Uiso 1 1 calc R . . C18 C 0.6192(7) 0.6499(6) 0.4871(3) 0.0808(18) Uani 1 1 d . . . H18A H 0.6626 0.5922 0.4644 0.097 Uiso 1 1 calc R . . C19 C 0.6502(6) 0.6816(5) 0.5542(3) 0.0640(15) Uani 1 1 d . . . H19A H 0.7161 0.6465 0.5776 0.077 Uiso 1 1 calc R . . C20 C 0.5245(5) 0.9073(4) 0.7024(2) 0.0453(11) Uani 1 1 d . . . C21 C 0.5865(6) 1.0298(5) 0.7009(4) 0.082(2) Uani 1 1 d . . . H21A H 0.6810 1.0540 0.6879 0.099 Uiso 1 1 calc R . . C22 C 0.5103(8) 1.1165(6) 0.7183(4) 0.107(3) Uani 1 1 d . . . H22A H 0.5522 1.2001 0.7165 0.128 Uiso 1 1 calc R . . C23 C 0.3758(7) 1.0829(6) 0.7381(4) 0.088(2) Uani 1 1 d . . . H23A H 0.3259 1.1434 0.7515 0.106 Uiso 1 1 calc R . . C24 C 0.3137(6) 0.9657(6) 0.7389(3) 0.0717(16) Uani 1 1 d . . . H24A H 0.2188 0.9428 0.7516 0.086 Uiso 1 1 calc R . . C25 C 0.3865(6) 0.8782(5) 0.7212(3) 0.0635(15) Uani 1 1 d . . . H25A H 0.3407 0.7950 0.7220 0.076 Uiso 1 1 calc R . . C26 C 0.5188(5) 0.6569(4) 0.7040(2) 0.0467(12) Uani 1 1 d . . . C27 C 0.4026(5) 0.5809(5) 0.6638(3) 0.0590(14) Uani 1 1 d . . . H27A H 0.3768 0.6021 0.6217 0.071 Uiso 1 1 calc R . . C28 C 0.3236(6) 0.4751(5) 0.6838(3) 0.0723(17) Uani 1 1 d . . . H28A H 0.2440 0.4258 0.6557 0.087 Uiso 1 1 calc R . . C29 C 0.3593(7) 0.4418(5) 0.7429(3) 0.0737(17) Uani 1 1 d . . . H29A H 0.3064 0.3683 0.7560 0.088 Uiso 1 1 calc R . . C30 C 0.4742(6) 0.5159(5) 0.7847(3) 0.0680(16) Uani 1 1 d . . . H30A H 0.5003 0.4928 0.8263 0.082 Uiso 1 1 calc R . . C31 C 0.5497(5) 0.6225(4) 0.7655(2) 0.0498(12) Uani 1 1 d . . . C32 C 0.6391(5) 0.7933(5) 0.8468(2) 0.0522(13) Uani 1 1 d . . . C33 C 0.5102(6) 0.7934(6) 0.8713(3) 0.0695(16) Uani 1 1 d . . . H33A H 0.4331 0.7231 0.8617 0.083 Uiso 1 1 calc R . . C34 C 0.4914(7) 0.8947(7) 0.9097(3) 0.093(2) Uani 1 1 d . . . H34A H 0.4008 0.8946 0.9260 0.112 Uiso 1 1 calc R . . C35 C 0.6030(8) 0.9958(7) 0.9247(3) 0.090(2) Uani 1 1 d . . . H35A H 0.5899 1.0658 0.9512 0.108 Uiso 1 1 calc R . . C36 C 0.7342(6) 0.9954(5) 0.9010(3) 0.0702(16) Uani 1 1 d . . . H36A H 0.8117 1.0651 0.9123 0.084 Uiso 1 1 calc R . . C37 C 0.7557(5) 0.8953(5) 0.8611(2) 0.0518(13) Uani 1 1 d . . . C38 C 1.0018(5) 0.7928(4) 0.8655(2) 0.0493(12) Uani 1 1 d . . . C39 C 0.9973(6) 0.7930(5) 0.9330(3) 0.0699(16) Uani 1 1 d . . . H39A H 0.9485 0.8451 0.9570 0.084 Uiso 1 1 calc R . . C40 C 1.0640(8) 0.7170(6) 0.9660(3) 0.091(2) Uani 1 1 d . . . H40A H 1.0631 0.7182 1.0125 0.109 Uiso 1 1 calc R . . C41 C 1.1308(7) 0.6404(6) 0.9306(4) 0.089(2) Uani 1 1 d . . . H41A H 1.1759 0.5880 0.9531 0.107 Uiso 1 1 calc R . . C42 C 1.1344(6) 0.6374(5) 0.8636(3) 0.0708(16) Uani 1 1 d . . . H42A H 1.1800 0.5826 0.8397 0.085 Uiso 1 1 calc R . . C43 C 1.0708(5) 0.7152(4) 0.8309(3) 0.0560(13) Uani 1 1 d . . . H43A H 1.0746 0.7151 0.7846 0.067 Uiso 1 1 calc R . . C44 C 1.0304(5) 1.0444(4) 0.8469(2) 0.0501(12) Uani 1 1 d . . . C45 C 0.9957(6) 1.1406(5) 0.8173(3) 0.0654(15) Uani 1 1 d . . . H45A H 0.9159 1.1246 0.7847 0.078 Uiso 1 1 calc R . . C46 C 1.0762(7) 1.2592(5) 0.8349(3) 0.0797(18) Uani 1 1 d . . . H46A H 1.0514 1.3238 0.8145 0.096 Uiso 1 1 calc R . . C47 C 1.1902(8) 1.2824(6) 0.8814(3) 0.084(2) Uani 1 1 d . . . H47A H 1.2445 1.3638 0.8936 0.101 Uiso 1 1 calc R . . C48 C 1.2286(7) 1.1899(6) 0.9111(3) 0.087(2) Uani 1 1 d . . . H48A H 1.3096 1.2071 0.9432 0.105 Uiso 1 1 calc R . . C49 C 1.1472(6) 1.0705(5) 0.8937(3) 0.0668(15) Uani 1 1 d . . . H49A H 1.1728 1.0065 0.9144 0.080 Uiso 1 1 calc R . . C50 C 0.7693(8) 1.4600(8) 0.8990(4) 0.129(3) Uani 1 1 d . . . H50A H 0.7821 1.5047 0.8601 0.155 Uiso 1 1 calc R . . H50B H 0.8652 1.4668 0.9224 0.155 Uiso 1 1 calc R . . Cl1 Cl 0.6539(4) 1.5251(3) 0.95507(14) 0.1949(14) Uani 1 1 d . . . Cl2 Cl 0.6912(4) 1.3188(3) 0.87572(16) 0.1854(12) 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 Cu 0.0427(4) 0.0537(4) 0.0464(4) 0.0056(3) 0.0093(3) 0.0143(3) N1 0.042(2) 0.057(3) 0.053(3) 0.014(2) 0.0088(19) 0.014(2) N2 0.050(3) 0.056(3) 0.045(2) 0.0065(19) 0.0091(19) 0.017(2) P1 0.0396(7) 0.0512(8) 0.0424(7) 0.0054(6) 0.0039(5) 0.0098(6) P2 0.0421(7) 0.0522(8) 0.0443(7) 0.0032(6) 0.0055(6) 0.0124(6) O1 0.044(2) 0.062(2) 0.051(2) 0.0098(17) 0.0063(15) 0.0097(17) C1 0.072(4) 0.058(4) 0.077(4) 0.018(3) 0.010(3) 0.021(3) C2 0.074(4) 0.072(4) 0.085(5) 0.033(4) 0.019(4) 0.012(3) C3 0.062(4) 0.102(5) 0.076(4) 0.035(4) 0.020(3) 0.007(4) C4 0.061(4) 0.080(4) 0.055(3) 0.011(3) 0.016(3) 0.020(3) C5 0.043(3) 0.068(4) 0.042(3) 0.009(3) 0.005(2) 0.018(3) C6 0.046(3) 0.053(3) 0.048(3) 0.000(2) 0.000(2) 0.017(2) C7 0.062(4) 0.082(4) 0.048(3) -0.006(3) 0.010(3) 0.033(3) C8 0.062(4) 0.057(3) 0.053(3) -0.003(3) -0.006(3) 0.023(3) C9 0.091(5) 0.066(4) 0.082(5) -0.014(3) -0.011(4) 0.037(4) C10 0.089(5) 0.050(4) 0.113(6) -0.004(4) -0.010(4) 0.021(4) C11 0.080(5) 0.057(4) 0.102(5) 0.018(4) -0.004(4) 0.016(3) C12 0.065(4) 0.058(4) 0.077(4) 0.013(3) 0.008(3) 0.017(3) C13 0.052(3) 0.054(3) 0.050(3) 0.003(3) -0.002(2) 0.013(3) C14 0.043(3) 0.069(3) 0.041(3) 0.011(3) 0.004(2) 0.008(3) C15 0.073(4) 0.126(6) 0.049(4) 0.010(4) 0.008(3) 0.037(4) C16 0.083(5) 0.173(8) 0.051(4) 0.015(4) -0.002(3) 0.054(5) C17 0.089(5) 0.143(7) 0.042(4) 0.001(4) -0.002(3) 0.014(5) C18 0.085(5) 0.093(5) 0.056(4) -0.014(3) 0.002(3) 0.017(4) C19 0.066(4) 0.075(4) 0.049(3) -0.001(3) 0.001(3) 0.016(3) C20 0.037(3) 0.052(3) 0.045(3) 0.006(2) 0.001(2) 0.008(2) C21 0.044(3) 0.059(4) 0.141(6) 0.011(4) 0.011(4) 0.005(3) C22 0.082(5) 0.044(4) 0.192(9) 0.001(4) -0.003(5) 0.022(4) C23 0.068(5) 0.076(5) 0.121(6) -0.013(4) -0.004(4) 0.036(4) C24 0.061(4) 0.082(5) 0.080(4) 0.006(3) 0.020(3) 0.032(4) C25 0.062(4) 0.060(3) 0.071(4) 0.012(3) 0.019(3) 0.015(3) C26 0.041(3) 0.049(3) 0.049(3) 0.003(2) 0.009(2) 0.008(2) C27 0.057(3) 0.062(3) 0.052(3) 0.003(3) 0.001(3) 0.007(3) C28 0.066(4) 0.064(4) 0.070(4) -0.009(3) 0.006(3) -0.013(3) C29 0.076(4) 0.055(4) 0.085(5) 0.010(3) 0.023(4) 0.001(3) C30 0.066(4) 0.067(4) 0.074(4) 0.029(3) 0.011(3) 0.011(3) C31 0.043(3) 0.051(3) 0.055(3) 0.005(2) 0.008(2) 0.009(2) C32 0.048(3) 0.070(4) 0.040(3) 0.008(3) 0.008(2) 0.014(3) C33 0.048(3) 0.103(5) 0.050(3) 0.001(3) 0.018(3) 0.003(3) C34 0.058(4) 0.145(7) 0.072(4) -0.013(4) 0.027(3) 0.021(4) C35 0.090(5) 0.101(5) 0.084(5) -0.010(4) 0.034(4) 0.036(4) C36 0.070(4) 0.079(4) 0.059(4) -0.008(3) 0.018(3) 0.019(3) C37 0.046(3) 0.070(3) 0.040(3) 0.007(2) 0.008(2) 0.014(3) C38 0.036(3) 0.056(3) 0.052(3) 0.003(2) -0.001(2) 0.004(2) C39 0.079(4) 0.074(4) 0.057(4) 0.009(3) 0.001(3) 0.022(3) C40 0.119(6) 0.102(5) 0.055(4) 0.024(4) -0.011(4) 0.030(5) C41 0.085(5) 0.092(5) 0.096(6) 0.033(4) -0.016(4) 0.029(4) C42 0.054(4) 0.070(4) 0.087(5) 0.010(3) -0.008(3) 0.017(3) C43 0.048(3) 0.055(3) 0.061(3) 0.005(3) -0.001(3) 0.008(3) C44 0.049(3) 0.052(3) 0.047(3) -0.001(2) 0.013(2) 0.009(2) C45 0.069(4) 0.063(4) 0.065(4) 0.006(3) 0.009(3) 0.017(3) C46 0.099(5) 0.058(4) 0.080(5) 0.008(3) 0.020(4) 0.011(4) C47 0.094(5) 0.061(4) 0.082(5) -0.011(4) 0.019(4) -0.004(4) C48 0.079(5) 0.085(5) 0.082(5) -0.008(4) -0.011(4) 0.002(4) C49 0.064(4) 0.059(4) 0.068(4) 0.000(3) -0.003(3) 0.003(3) C50 0.109(7) 0.158(8) 0.099(6) 0.057(6) -0.005(5) -0.028(6) Cl1 0.284(4) 0.208(3) 0.106(2) 0.0046(19) -0.032(2) 0.110(3) Cl2 0.245(4) 0.165(3) 0.161(3) 0.021(2) 0.002(2) 0.084(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N2 2.006(4) . ? Cu N1 2.112(4) . ? Cu P2 2.2355(16) . ? Cu P1 2.2862(16) . ? N1 C1 1.347(6) . ? N1 C5 1.351(6) . ? N2 C13 1.365(6) . ? N2 C6 1.370(6) . ? P1 C20 1.819(5) . ? P1 C14 1.826(5) . ? P1 C26 1.840(5) . ? P2 C44 1.830(5) . ? P2 C38 1.831(5) . ? P2 C37 1.832(5) . ? O1 C32 1.391(6) . ? O1 C31 1.398(5) . ? C1 C2 1.367(7) . ? C2 C3 1.387(8) . ? C3 C4 1.369(8) . ? C4 C5 1.386(7) . ? C5 C6 1.463(7) . ? C6 C7 1.374(6) . ? C7 C8 1.415(7) . ? C8 C9 1.403(7) . ? C8 C13 1.417(7) . ? C9 C10 1.335(9) . ? C10 C11 1.392(9) . ? C11 C12 1.380(7) . ? C12 C13 1.387(7) . ? C14 C15 1.383(7) . ? C14 C19 1.390(7) . ? C15 C16 1.384(8) . ? C16 C17 1.354(9) . ? C17 C18 1.375(8) . ? C18 C19 1.372(7) . ? C20 C25 1.380(7) . ? C20 C21 1.389(7) . ? C21 C22 1.385(8) . ? C22 C23 1.361(9) . ? C23 C24 1.333(8) . ? C24 C25 1.370(7) . ? C26 C31 1.388(6) . ? C26 C27 1.394(6) . ? C27 C28 1.387(7) . ? C28 C29 1.349(8) . ? C29 C30 1.394(7) . ? C30 C31 1.376(7) . ? C32 C33 1.364(7) . ? C32 C37 1.404(7) . ? C33 C34 1.375(8) . ? C34 C35 1.371(9) . ? C35 C36 1.379(8) . ? C36 C37 1.387(7) . ? C38 C43 1.380(7) . ? C38 C39 1.382(7) . ? C39 C40 1.388(8) . ? C40 C41 1.367(9) . ? C41 C42 1.368(9) . ? C42 C43 1.385(7) . ? C44 C49 1.376(7) . ? C44 C45 1.398(7) . ? C45 C46 1.387(7) . ? C46 C47 1.355(9) . ? C47 C48 1.378(9) . ? C48 C49 1.398(7) . ? C50 Cl2 1.612(8) . ? C50 Cl1 1.854(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu N1 80.83(16) . . ? N2 Cu P2 120.42(12) . . ? N1 Cu P2 119.41(12) . . ? N2 Cu P1 107.57(12) . . ? N1 Cu P1 112.81(11) . . ? P2 Cu P1 112.07(5) . . ? C1 N1 C5 118.1(5) . . ? C1 N1 Cu 129.8(4) . . ? C5 N1 Cu 112.1(3) . . ? C13 N2 C6 104.8(4) . . ? C13 N2 Cu 140.2(4) . . ? C6 N2 Cu 113.9(3) . . ? C20 P1 C14 103.5(2) . . ? C20 P1 C26 101.8(2) . . ? C14 P1 C26 100.8(2) . . ? C20 P1 Cu 121.46(16) . . ? C14 P1 Cu 113.00(16) . . ? C26 P1 Cu 113.77(16) . . ? C44 P2 C38 103.8(2) . . ? C44 P2 C37 101.8(2) . . ? C38 P2 C37 102.6(2) . . ? C44 P2 Cu 118.85(17) . . ? C38 P2 Cu 115.37(17) . . ? C37 P2 Cu 112.32(16) . . ? C32 O1 C31 116.2(4) . . ? N1 C1 C2 123.6(6) . . ? C1 C2 C3 118.0(6) . . ? C4 C3 C2 119.3(6) . . ? C3 C4 C5 120.0(6) . . ? N1 C5 C4 121.0(5) . . ? N1 C5 C6 115.6(4) . . ? C4 C5 C6 123.4(5) . . ? N2 C6 C7 112.8(5) . . ? N2 C6 C5 117.1(4) . . ? C7 C6 C5 130.1(5) . . ? C6 C7 C8 105.9(5) . . ? C9 C8 C7 135.3(6) . . ? C9 C8 C13 119.4(6) . . ? C7 C8 C13 105.3(5) . . ? C10 C9 C8 119.6(6) . . ? C9 C10 C11 121.5(6) . . ? C12 C11 C10 121.0(6) . . ? C11 C12 C13 118.5(6) . . ? N2 C13 C12 128.8(5) . . ? N2 C13 C8 111.2(5) . . ? C12 C13 C8 120.1(5) . . ? C15 C14 C19 118.1(5) . . ? C15 C14 P1 124.3(4) . . ? C19 C14 P1 117.6(4) . . ? C16 C15 C14 120.7(6) . . ? C17 C16 C15 120.1(6) . . ? C16 C17 C18 120.3(6) . . ? C19 C18 C17 120.1(6) . . ? C18 C19 C14 120.6(5) . . ? C25 C20 C21 117.2(5) . . ? C25 C20 P1 124.4(4) . . ? C21 C20 P1 118.4(4) . . ? C22 C21 C20 119.9(6) . . ? C23 C22 C21 120.5(6) . . ? C24 C23 C22 120.4(6) . . ? C23 C24 C25 120.1(6) . . ? C24 C25 C20 121.9(5) . . ? C31 C26 C27 116.6(5) . . ? C31 C26 P1 120.8(4) . . ? C27 C26 P1 122.6(4) . . ? C28 C27 C26 121.7(5) . . ? C29 C28 C27 120.4(5) . . ? C28 C29 C30 119.6(5) . . ? C31 C30 C29 119.8(5) . . ? C30 C31 C26 121.9(5) . . ? C30 C31 O1 118.0(5) . . ? C26 C31 O1 120.0(4) . . ? C33 C32 O1 123.1(5) . . ? C33 C32 C37 121.0(5) . . ? O1 C32 C37 115.8(4) . . ? C32 C33 C34 120.4(6) . . ? C35 C34 C33 120.1(6) . . ? C34 C35 C36 119.7(6) . . ? C35 C36 C37 121.5(6) . . ? C36 C37 C32 117.3(5) . . ? C36 C37 P2 124.9(4) . . ? C32 C37 P2 117.5(4) . . ? C43 C38 C39 119.6(5) . . ? C43 C38 P2 118.0(4) . . ? C39 C38 P2 122.4(4) . . ? C38 C39 C40 120.1(6) . . ? C41 C40 C39 119.3(6) . . ? C40 C41 C42 121.6(6) . . ? C41 C42 C43 119.2(6) . . ? C38 C43 C42 120.3(5) . . ? C49 C44 C45 118.2(5) . . ? C49 C44 P2 124.8(4) . . ? C45 C44 P2 117.1(4) . . ? C46 C45 C44 120.9(6) . . ? C47 C46 C45 119.7(6) . . ? C46 C47 C48 121.1(6) . . ? C47 C48 C49 119.3(6) . . ? C44 C49 C48 120.9(6) . . ? Cl2 C50 Cl1 107.9(4) . . ? 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 N2 Cu N1 C1 -175.4(4) . . . . ? P2 Cu N1 C1 -55.5(4) . . . . ? P1 Cu N1 C1 79.3(4) . . . . ? N2 Cu N1 C5 4.9(3) . . . . ? P2 Cu N1 C5 124.7(3) . . . . ? P1 Cu N1 C5 -100.4(3) . . . . ? N1 Cu N2 C13 -171.7(5) . . . . ? P2 Cu N2 C13 69.5(5) . . . . ? P1 Cu N2 C13 -60.5(5) . . . . ? N1 Cu N2 C6 -6.3(3) . . . . ? P2 Cu N2 C6 -125.1(3) . . . . ? P1 Cu N2 C6 104.8(3) . . . . ? N2 Cu P1 C20 -176.4(2) . . . . ? N1 Cu P1 C20 -89.1(2) . . . . ? P2 Cu P1 C20 49.06(19) . . . . ? N2 Cu P1 C14 -52.6(2) . . . . ? N1 Cu P1 C14 34.7(2) . . . . ? P2 Cu P1 C14 172.86(18) . . . . ? N2 Cu P1 C26 61.6(2) . . . . ? N1 Cu P1 C26 148.8(2) . . . . ? P2 Cu P1 C26 -73.00(17) . . . . ? N2 Cu P2 C44 115.9(2) . . . . ? N1 Cu P2 C44 19.1(2) . . . . ? P1 Cu P2 C44 -116.06(19) . . . . ? N2 Cu P2 C38 -8.3(2) . . . . ? N1 Cu P2 C38 -105.2(2) . . . . ? P1 Cu P2 C38 119.70(17) . . . . ? N2 Cu P2 C37 -125.5(2) . . . . ? N1 Cu P2 C37 137.7(2) . . . . ? P1 Cu P2 C37 2.56(19) . . . . ? C5 N1 C1 C2 0.9(8) . . . . ? Cu N1 C1 C2 -178.8(4) . . . . ? N1 C1 C2 C3 -0.2(9) . . . . ? C1 C2 C3 C4 -0.3(9) . . . . ? C2 C3 C4 C5 0.1(9) . . . . ? C1 N1 C5 C4 -1.2(7) . . . . ? Cu N1 C5 C4 178.6(4) . . . . ? C1 N1 C5 C6 177.6(4) . . . . ? Cu N1 C5 C6 -2.6(5) . . . . ? C3 C4 C5 N1 0.6(8) . . . . ? C3 C4 C5 C6 -178.0(5) . . . . ? C13 N2 C6 C7 -0.5(5) . . . . ? Cu N2 C6 C7 -170.9(3) . . . . ? C13 N2 C6 C5 177.3(4) . . . . ? Cu N2 C6 C5 6.9(5) . . . . ? N1 C5 C6 N2 -2.7(6) . . . . ? C4 C5 C6 N2 176.0(4) . . . . ? N1 C5 C6 C7 174.7(5) . . . . ? C4 C5 C6 C7 -6.6(8) . . . . ? N2 C6 C7 C8 0.9(6) . . . . ? C5 C6 C7 C8 -176.6(5) . . . . ? C6 C7 C8 C9 177.4(6) . . . . ? C6 C7 C8 C13 -0.9(5) . . . . ? C7 C8 C9 C10 -179.7(6) . . . . ? C13 C8 C9 C10 -1.7(8) . . . . ? C8 C9 C10 C11 -0.4(10) . . . . ? C9 C10 C11 C12 1.9(10) . . . . ? C10 C11 C12 C13 -1.2(9) . . . . ? C6 N2 C13 C12 179.6(5) . . . . ? Cu N2 C13 C12 -14.2(9) . . . . ? C6 N2 C13 C8 0.0(5) . . . . ? Cu N2 C13 C8 166.1(4) . . . . ? C11 C12 C13 N2 179.5(5) . . . . ? C11 C12 C13 C8 -0.8(8) . . . . ? C9 C8 C13 N2 -178.0(4) . . . . ? C7 C8 C13 N2 0.6(6) . . . . ? C9 C8 C13 C12 2.3(8) . . . . ? C7 C8 C13 C12 -179.1(5) . . . . ? C20 P1 C14 C15 -0.2(5) . . . . ? C26 P1 C14 C15 104.8(5) . . . . ? Cu P1 C14 C15 -133.4(4) . . . . ? C20 P1 C14 C19 179.8(4) . . . . ? C26 P1 C14 C19 -75.2(4) . . . . ? Cu P1 C14 C19 46.6(4) . . . . ? C19 C14 C15 C16 2.4(9) . . . . ? P1 C14 C15 C16 -177.5(5) . . . . ? C14 C15 C16 C17 -0.3(11) . . . . ? C15 C16 C17 C18 -1.7(11) . . . . ? C16 C17 C18 C19 1.4(11) . . . . ? C17 C18 C19 C14 0.8(9) . . . . ? C15 C14 C19 C18 -2.7(8) . . . . ? P1 C14 C19 C18 177.3(4) . . . . ? C14 P1 C20 C25 92.0(5) . . . . ? C26 P1 C20 C25 -12.2(5) . . . . ? Cu P1 C20 C25 -139.8(4) . . . . ? C14 P1 C20 C21 -86.5(5) . . . . ? C26 P1 C20 C21 169.2(4) . . . . ? Cu P1 C20 C21 41.6(5) . . . . ? C25 C20 C21 C22 0.5(9) . . . . ? P1 C20 C21 C22 179.2(5) . . . . ? C20 C21 C22 C23 1.1(11) . . . . ? C21 C22 C23 C24 -2.2(12) . . . . ? C22 C23 C24 C25 1.6(10) . . . . ? C23 C24 C25 C20 0.1(9) . . . . ? C21 C20 C25 C24 -1.1(8) . . . . ? P1 C20 C25 C24 -179.7(4) . . . . ? C20 P1 C26 C31 -94.0(4) . . . . ? C14 P1 C26 C31 159.6(4) . . . . ? Cu P1 C26 C31 38.4(4) . . . . ? C20 P1 C26 C27 85.9(4) . . . . ? C14 P1 C26 C27 -20.5(5) . . . . ? Cu P1 C26 C27 -141.7(4) . . . . ? C31 C26 C27 C28 -1.2(8) . . . . ? P1 C26 C27 C28 178.8(4) . . . . ? C26 C27 C28 C29 -1.0(9) . . . . ? C27 C28 C29 C30 1.5(9) . . . . ? C28 C29 C30 C31 0.4(9) . . . . ? C29 C30 C31 C26 -2.8(8) . . . . ? C29 C30 C31 O1 -179.1(5) . . . . ? C27 C26 C31 C30 3.1(7) . . . . ? P1 C26 C31 C30 -177.0(4) . . . . ? C27 C26 C31 O1 179.4(4) . . . . ? P1 C26 C31 O1 -0.7(6) . . . . ? C32 O1 C31 C30 -100.4(5) . . . . ? C32 O1 C31 C26 83.3(5) . . . . ? C31 O1 C32 C33 34.8(7) . . . . ? C31 O1 C32 C37 -147.0(4) . . . . ? O1 C32 C33 C34 179.2(5) . . . . ? C37 C32 C33 C34 1.0(9) . . . . ? C32 C33 C34 C35 -1.1(10) . . . . ? C33 C34 C35 C36 -0.1(11) . . . . ? C34 C35 C36 C37 1.3(10) . . . . ? C35 C36 C37 C32 -1.3(8) . . . . ? C35 C36 C37 P2 172.3(5) . . . . ? C33 C32 C37 C36 0.1(7) . . . . ? O1 C32 C37 C36 -178.1(4) . . . . ? C33 C32 C37 P2 -174.0(4) . . . . ? O1 C32 C37 P2 7.8(6) . . . . ? C44 P2 C37 C36 1.8(5) . . . . ? C38 P2 C37 C36 109.1(5) . . . . ? Cu P2 C37 C36 -126.4(4) . . . . ? C44 P2 C37 C32 175.4(4) . . . . ? C38 P2 C37 C32 -77.3(4) . . . . ? Cu P2 C37 C32 47.2(4) . . . . ? C44 P2 C38 C43 -110.7(4) . . . . ? C37 P2 C38 C43 143.6(4) . . . . ? Cu P2 C38 C43 21.1(4) . . . . ? C44 P2 C38 C39 69.8(5) . . . . ? C37 P2 C38 C39 -35.9(5) . . . . ? Cu P2 C38 C39 -158.4(4) . . . . ? C43 C38 C39 C40 1.1(8) . . . . ? P2 C38 C39 C40 -179.3(5) . . . . ? C38 C39 C40 C41 -1.5(10) . . . . ? C39 C40 C41 C42 0.4(11) . . . . ? C40 C41 C42 C43 1.0(10) . . . . ? C39 C38 C43 C42 0.3(8) . . . . ? P2 C38 C43 C42 -179.2(4) . . . . ? C41 C42 C43 C38 -1.4(8) . . . . ? C38 P2 C44 C49 -1.5(5) . . . . ? C37 P2 C44 C49 104.8(5) . . . . ? Cu P2 C44 C49 -131.2(4) . . . . ? C38 P2 C44 C45 177.3(4) . . . . ? C37 P2 C44 C45 -76.4(4) . . . . ? Cu P2 C44 C45 47.6(4) . . . . ? C49 C44 C45 C46 -0.4(8) . . . . ? P2 C44 C45 C46 -179.3(4) . . . . ? C44 C45 C46 C47 0.1(9) . . . . ? C45 C46 C47 C48 0.6(10) . . . . ? C46 C47 C48 C49 -0.9(10) . . . . ? C45 C44 C49 C48 0.1(8) . . . . ? P2 C44 C49 C48 178.9(5) . . . . ? C47 C48 C49 C44 0.5(10) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 26.15 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.509 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.067 # Attachment 'S326.CIF' data_s326 _database_code_depnum_ccdc_archive 'CCDC 828214' #TrackingRef 'S326.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H39 Cu N2 P2' _chemical_formula_weight 781.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 20.386(3) _cell_length_b 21.293(3) _cell_length_c 9.1912(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3989.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 186(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 0.664 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8808 _exptl_absorpt_correction_T_max 0.9414 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 186(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21912 _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_av_sigmaI/netI 0.0859 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 26.06 _reflns_number_total 7863 _reflns_number_gt 5091 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.013(18) _refine_ls_number_reflns 7863 _refine_ls_number_parameters 487 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1003 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1030 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.24870(3) 0.30784(2) 0.38793(9) 0.04800(14) Uani 1 1 d . . . N1 N 0.19982(19) 0.29881(19) 0.1865(4) 0.0544(11) Uani 1 1 d . . . N2 N 0.18639(17) 0.23777(17) 0.4400(4) 0.0467(10) Uani 1 1 d . . . P1 P 0.21822(6) 0.40408(6) 0.46629(15) 0.0460(3) Uani 1 1 d . . . P2 P 0.35679(5) 0.28858(5) 0.37624(16) 0.0452(3) Uani 1 1 d . . . C1 C 0.2068(3) 0.3323(3) 0.0665(6) 0.0656(15) Uani 1 1 d . . . H1A H 0.2425 0.3609 0.0616 0.079 Uiso 1 1 calc R . . C2 C 0.1657(3) 0.3283(3) -0.0516(6) 0.0784(17) Uani 1 1 d . . . H2A H 0.1721 0.3539 -0.1351 0.094 Uiso 1 1 calc R . . C3 C 0.1154(3) 0.2864(3) -0.0442(7) 0.088(2) Uani 1 1 d . . . H3A H 0.0859 0.2823 -0.1236 0.106 Uiso 1 1 calc R . . C4 C 0.1072(3) 0.2499(3) 0.0781(7) 0.0710(16) Uani 1 1 d . . . H4A H 0.0726 0.2201 0.0834 0.085 Uiso 1 1 calc R . . C5 C 0.1502(2) 0.2574(2) 0.1933(5) 0.0488(12) Uani 1 1 d . . . C6 C 0.1459(2) 0.2220(2) 0.3296(5) 0.0452(12) Uani 1 1 d . . . C7 C 0.1033(2) 0.1743(2) 0.3660(7) 0.0583(14) Uani 1 1 d . . . H7A H 0.0705 0.1561 0.3059 0.070 Uiso 1 1 calc R . . C8 C 0.1184(2) 0.1581(2) 0.5103(6) 0.0563(14) Uani 1 1 d . . . C9 C 0.0957(3) 0.1137(2) 0.6132(8) 0.0734(18) Uani 1 1 d . . . H9A H 0.0620 0.0850 0.5874 0.088 Uiso 1 1 calc R . . C10 C 0.1221(3) 0.1123(3) 0.7488(8) 0.0820(19) Uani 1 1 d . . . H10A H 0.1065 0.0822 0.8169 0.098 Uiso 1 1 calc R . . C11 C 0.1715(3) 0.1539(3) 0.7907(7) 0.0735(17) Uani 1 1 d . . . H11A H 0.1888 0.1519 0.8865 0.088 Uiso 1 1 calc R . . C12 C 0.1951(3) 0.1976(2) 0.6945(6) 0.0607(14) Uani 1 1 d . . . H12A H 0.2281 0.2264 0.7235 0.073 Uiso 1 1 calc R . . C13 C 0.1698(2) 0.1991(2) 0.5529(6) 0.0468(13) Uani 1 1 d . . . C14 C 0.1414(2) 0.4081(2) 0.5691(5) 0.0473(12) Uani 1 1 d . . . C15 C 0.1300(3) 0.4513(2) 0.6765(6) 0.0598(15) Uani 1 1 d . . . H15A H 0.1628 0.4814 0.6994 0.072 Uiso 1 1 calc R . . C16 C 0.0713(3) 0.4515(3) 0.7520(6) 0.0733(17) Uani 1 1 d . . . H16A H 0.0640 0.4818 0.8262 0.088 Uiso 1 1 calc R . . C17 C 0.0239(3) 0.4086(3) 0.7205(7) 0.0735(17) Uani 1 1 d . . . H17A H -0.0162 0.4088 0.7732 0.088 Uiso 1 1 calc R . . C18 C 0.0339(3) 0.3653(3) 0.6132(7) 0.0742(17) Uani 1 1 d . . . H18A H 0.0006 0.3358 0.5898 0.089 Uiso 1 1 calc R . . C19 C 0.0927(2) 0.3649(2) 0.5391(6) 0.0619(15) Uani 1 1 d . . . H19A H 0.0999 0.3342 0.4659 0.074 Uiso 1 1 calc R . . C20 C 0.2045(2) 0.4590(2) 0.3184(5) 0.0511(13) Uani 1 1 d . . . C21 C 0.2573(3) 0.4781(3) 0.2319(7) 0.0750(17) Uani 1 1 d . . . H21A H 0.3002 0.4640 0.2554 0.090 Uiso 1 1 calc R . . C22 C 0.2486(3) 0.5169(3) 0.1139(7) 0.0874(19) Uani 1 1 d . . . H22A H 0.2856 0.5312 0.0605 0.105 Uiso 1 1 calc R . . C23 C 0.1878(4) 0.5348(3) 0.0737(7) 0.099(2) Uani 1 1 d . . . H23A H 0.1818 0.5612 -0.0086 0.119 Uiso 1 1 calc R . . C24 C 0.1345(4) 0.5147(4) 0.1521(7) 0.111(3) Uani 1 1 d . . . H24A H 0.0916 0.5265 0.1228 0.133 Uiso 1 1 calc R . . C25 C 0.1430(3) 0.4774(3) 0.2732(6) 0.0809(19) Uani 1 1 d . . . H25A H 0.1056 0.4642 0.3268 0.097 Uiso 1 1 calc R . . C26 C 0.2748(2) 0.4441(2) 0.5876(5) 0.0490(13) Uani 1 1 d . . . C27 C 0.2903(3) 0.5072(3) 0.5817(7) 0.0661(15) Uani 1 1 d . . . H27A H 0.2720 0.5329 0.5077 0.079 Uiso 1 1 calc R . . C28 C 0.3325(3) 0.5331(3) 0.6834(9) 0.096(2) Uani 1 1 d . . . H28A H 0.3433 0.5764 0.6778 0.115 Uiso 1 1 calc R . . C29 C 0.3585(3) 0.4973(4) 0.7909(8) 0.100(3) Uani 1 1 d . . . H29A H 0.3868 0.5158 0.8610 0.120 Uiso 1 1 calc R . . C30 C 0.3440(3) 0.4343(4) 0.7984(7) 0.087(2) Uani 1 1 d . . . H30A H 0.3626 0.4091 0.8731 0.104 Uiso 1 1 calc R . . C31 C 0.3027(2) 0.4079(3) 0.6978(6) 0.0656(15) Uani 1 1 d . . . H31A H 0.2929 0.3644 0.7033 0.079 Uiso 1 1 calc R . . C32 C 0.3928(2) 0.2708(2) 0.5533(5) 0.0466(12) Uani 1 1 d . . . C33 C 0.4482(3) 0.2978(2) 0.6128(6) 0.0599(14) Uani 1 1 d . . . H33A H 0.4722 0.3281 0.5588 0.072 Uiso 1 1 calc R . . C34 C 0.4690(3) 0.2809(3) 0.7517(6) 0.0728(17) Uani 1 1 d . . . H34A H 0.5071 0.2998 0.7922 0.087 Uiso 1 1 calc R . . C35 C 0.4352(3) 0.2376(3) 0.8294(6) 0.0743(17) Uani 1 1 d . . . H35A H 0.4493 0.2268 0.9247 0.089 Uiso 1 1 calc R . . C36 C 0.3806(3) 0.2091(3) 0.7709(7) 0.0744(17) Uani 1 1 d . . . H36A H 0.3571 0.1782 0.8243 0.089 Uiso 1 1 calc R . . C37 C 0.3608(3) 0.2263(3) 0.6342(6) 0.0662(16) Uani 1 1 d . . . H37A H 0.3232 0.2065 0.5937 0.079 Uiso 1 1 calc R . . C38 C 0.3825(3) 0.2195(2) 0.2731(5) 0.0510(13) Uani 1 1 d . . . C39 C 0.4477(3) 0.2005(3) 0.2681(6) 0.0648(15) Uani 1 1 d . . . H39A H 0.4801 0.2245 0.3172 0.078 Uiso 1 1 calc R . . C40 C 0.4660(3) 0.1478(3) 0.1941(6) 0.0806(18) Uani 1 1 d . . . H40A H 0.5108 0.1360 0.1900 0.097 Uiso 1 1 calc R . . C41 C 0.4192(4) 0.1120(3) 0.1254(7) 0.088(2) Uani 1 1 d . . . H41A H 0.4317 0.0748 0.0757 0.105 Uiso 1 1 calc R . . C42 C 0.3549(4) 0.1297(3) 0.1283(7) 0.088(2) Uani 1 1 d . . . H42A H 0.3229 0.1055 0.0786 0.106 Uiso 1 1 calc R . . C43 C 0.3363(3) 0.1833(3) 0.2041(7) 0.0697(17) Uani 1 1 d . . . H43A H 0.2913 0.1949 0.2081 0.084 Uiso 1 1 calc R . . C44 C 0.4074(2) 0.3514(2) 0.2982(5) 0.0439(12) Uani 1 1 d . . . C45 C 0.41910(19) 0.40601(19) 0.3768(6) 0.0503(11) Uani 1 1 d . . . H45A H 0.4021 0.4100 0.4725 0.060 Uiso 1 1 calc R . . C46 C 0.4552(2) 0.4547(2) 0.3175(6) 0.0582(14) Uani 1 1 d . . . H46A H 0.4635 0.4915 0.3729 0.070 Uiso 1 1 calc R . . C47 C 0.4788(2) 0.4496(3) 0.1792(7) 0.0638(15) Uani 1 1 d . . . H47A H 0.5040 0.4828 0.1386 0.077 Uiso 1 1 calc R . . C48 C 0.4662(2) 0.3970(3) 0.0987(6) 0.0648(16) Uani 1 1 d . . . H48A H 0.4821 0.3941 0.0018 0.078 Uiso 1 1 calc R . . C49 C 0.4307(2) 0.3482(2) 0.1572(5) 0.0529(13) Uani 1 1 d . . . H49A H 0.4221 0.3119 0.1000 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0399(3) 0.0486(3) 0.0555(3) 0.0014(4) -0.0055(3) -0.0092(3) N1 0.052(3) 0.062(3) 0.049(3) -0.001(2) -0.004(2) -0.004(2) N2 0.039(2) 0.050(2) 0.051(3) -0.001(2) -0.0032(19) -0.0068(18) P1 0.0333(7) 0.0482(7) 0.0565(7) 0.0008(7) -0.0024(6) -0.0049(6) P2 0.0395(6) 0.0437(7) 0.0525(7) 0.0016(8) -0.0020(8) -0.0036(5) C1 0.067(4) 0.074(4) 0.056(4) 0.007(3) -0.006(3) -0.007(3) C2 0.088(5) 0.098(5) 0.049(4) 0.006(3) -0.015(3) 0.010(4) C3 0.065(4) 0.126(6) 0.073(5) -0.005(4) -0.028(3) 0.010(4) C4 0.054(4) 0.081(4) 0.078(4) -0.009(4) -0.017(3) -0.004(3) C5 0.037(3) 0.055(3) 0.055(3) -0.015(3) -0.004(3) 0.001(2) C6 0.035(3) 0.038(3) 0.063(3) -0.006(2) -0.002(2) -0.004(2) C7 0.040(3) 0.049(3) 0.087(5) -0.014(3) -0.007(3) -0.007(2) C8 0.041(3) 0.040(3) 0.087(4) -0.003(3) 0.014(3) -0.002(2) C9 0.060(4) 0.044(3) 0.117(6) 0.007(4) 0.018(4) -0.006(3) C10 0.073(5) 0.067(4) 0.107(5) 0.026(4) 0.035(4) 0.003(3) C11 0.073(4) 0.066(4) 0.081(4) 0.022(4) 0.015(3) 0.007(3) C12 0.062(4) 0.057(3) 0.063(4) 0.005(3) 0.005(3) 0.000(3) C13 0.038(3) 0.039(3) 0.064(4) -0.004(3) 0.013(3) 0.000(2) C14 0.040(3) 0.044(3) 0.057(3) 0.007(3) 0.002(2) 0.003(2) C15 0.052(3) 0.055(4) 0.072(4) -0.004(3) 0.003(3) -0.001(3) C16 0.072(4) 0.071(4) 0.077(4) -0.004(3) 0.020(3) 0.004(3) C17 0.050(4) 0.093(5) 0.078(4) 0.006(4) 0.018(3) -0.004(3) C18 0.054(4) 0.080(5) 0.088(5) 0.001(4) 0.004(3) -0.021(3) C19 0.043(3) 0.068(4) 0.075(4) -0.013(3) 0.010(3) -0.007(3) C20 0.047(3) 0.045(3) 0.061(3) -0.003(3) 0.001(3) -0.003(2) C21 0.056(4) 0.087(5) 0.082(4) 0.013(4) -0.005(3) -0.010(3) C22 0.088(5) 0.090(5) 0.084(5) 0.019(4) 0.008(4) -0.014(4) C23 0.134(7) 0.092(5) 0.070(5) 0.028(4) 0.008(5) 0.027(5) C24 0.096(6) 0.160(8) 0.075(5) 0.033(5) 0.002(4) 0.058(5) C25 0.061(4) 0.112(5) 0.070(4) 0.021(4) 0.011(3) 0.029(4) C26 0.035(3) 0.061(4) 0.051(3) -0.007(3) 0.004(2) -0.004(2) C27 0.054(4) 0.063(4) 0.082(4) -0.006(3) 0.001(3) -0.011(3) C28 0.078(5) 0.098(6) 0.111(6) -0.044(5) 0.014(4) -0.046(4) C29 0.064(5) 0.153(8) 0.082(5) -0.032(5) -0.007(4) -0.038(5) C30 0.053(4) 0.142(6) 0.065(4) -0.009(4) -0.010(3) 0.002(4) C31 0.052(3) 0.081(4) 0.064(4) -0.010(3) -0.008(3) -0.004(3) C32 0.044(3) 0.044(3) 0.052(3) 0.001(2) 0.005(3) 0.010(2) C33 0.058(4) 0.053(3) 0.069(4) 0.011(3) -0.006(3) -0.004(3) C34 0.078(4) 0.072(4) 0.069(4) 0.006(3) -0.030(3) -0.005(3) C35 0.096(5) 0.079(4) 0.048(4) 0.001(3) -0.007(3) 0.022(4) C36 0.070(4) 0.088(5) 0.065(4) 0.025(3) 0.002(3) -0.002(3) C37 0.056(4) 0.077(4) 0.066(4) 0.016(3) 0.004(3) -0.003(3) C38 0.054(3) 0.046(3) 0.053(3) 0.006(3) 0.000(3) 0.001(3) C39 0.072(4) 0.062(4) 0.060(4) -0.004(3) -0.003(3) 0.009(3) C40 0.099(5) 0.067(4) 0.075(4) 0.008(4) 0.021(4) 0.022(4) C41 0.130(7) 0.043(4) 0.091(5) -0.008(4) 0.025(5) 0.005(4) C42 0.109(6) 0.062(4) 0.094(5) -0.014(4) 0.005(5) -0.026(4) C43 0.074(4) 0.056(4) 0.078(4) -0.009(3) 0.003(3) -0.016(3) C44 0.031(3) 0.042(3) 0.059(3) 0.008(3) -0.008(2) 0.005(2) C45 0.045(3) 0.044(3) 0.061(3) 0.009(3) -0.003(3) 0.001(2) C46 0.057(3) 0.049(3) 0.069(4) 0.005(3) -0.011(3) 0.000(3) C47 0.049(3) 0.061(4) 0.082(5) 0.023(3) -0.013(3) -0.007(3) C48 0.059(4) 0.080(5) 0.056(4) 0.021(3) -0.001(3) -0.001(3) C49 0.057(3) 0.054(3) 0.048(3) 0.004(3) -0.004(3) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N2 2.017(4) . ? Cu N1 2.111(4) . ? Cu P2 2.2439(13) . ? Cu P1 2.2591(14) . ? N1 C1 1.321(6) . ? N1 C5 1.345(6) . ? N2 C6 1.350(5) . ? N2 C13 1.367(5) . ? P1 C20 1.815(5) . ? P1 C26 1.816(5) . ? P1 C14 1.831(5) . ? P2 C32 1.825(5) . ? P2 C38 1.826(5) . ? P2 C44 1.834(5) . ? C1 C2 1.374(7) . ? C2 C3 1.362(7) . ? C3 C4 1.376(8) . ? C4 C5 1.382(7) . ? C5 C6 1.464(6) . ? C6 C7 1.379(6) . ? C7 C8 1.405(8) . ? C8 C9 1.414(7) . ? C8 C13 1.419(6) . ? C9 C10 1.358(8) . ? C10 C11 1.395(8) . ? C11 C12 1.371(7) . ? C12 C13 1.401(7) . ? C14 C15 1.368(6) . ? C14 C19 1.381(6) . ? C15 C16 1.384(6) . ? C16 C17 1.361(7) . ? C17 C18 1.365(7) . ? C18 C19 1.379(7) . ? C20 C25 1.378(6) . ? C20 C21 1.398(7) . ? C21 C22 1.374(8) . ? C22 C23 1.349(8) . ? C23 C24 1.371(9) . ? C24 C25 1.377(8) . ? C26 C27 1.381(7) . ? C26 C31 1.394(7) . ? C27 C28 1.385(8) . ? C28 C29 1.356(9) . ? C29 C30 1.377(8) . ? C30 C31 1.371(7) . ? C32 C37 1.370(6) . ? C32 C33 1.380(6) . ? C33 C34 1.393(7) . ? C34 C35 1.354(7) . ? C35 C36 1.377(7) . ? C36 C37 1.369(7) . ? C38 C43 1.373(7) . ? C38 C39 1.392(6) . ? C39 C40 1.362(7) . ? C40 C41 1.375(8) . ? C41 C42 1.364(8) . ? C42 C43 1.388(8) . ? C44 C49 1.382(6) . ? C44 C45 1.390(6) . ? C45 C46 1.382(6) . ? C46 C47 1.364(7) . ? C47 C48 1.366(7) . ? C48 C49 1.376(6) . ? 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 N2 Cu N1 81.00(15) . . ? N2 Cu P2 119.64(11) . . ? N1 Cu P2 113.88(12) . . ? N2 Cu P1 114.96(11) . . ? N1 Cu P1 103.44(12) . . ? P2 Cu P1 116.82(5) . . ? C1 N1 C5 118.3(4) . . ? C1 N1 Cu 129.2(4) . . ? C5 N1 Cu 112.0(3) . . ? C6 N2 C13 105.6(4) . . ? C6 N2 Cu 112.9(3) . . ? C13 N2 Cu 141.4(3) . . ? C20 P1 C26 104.8(2) . . ? C20 P1 C14 103.0(2) . . ? C26 P1 C14 101.8(2) . . ? C20 P1 Cu 112.81(16) . . ? C26 P1 Cu 116.55(17) . . ? C14 P1 Cu 116.26(16) . . ? C32 P2 C38 100.4(2) . . ? C32 P2 C44 105.9(2) . . ? C38 P2 C44 102.9(2) . . ? C32 P2 Cu 112.98(16) . . ? C38 P2 Cu 116.98(17) . . ? C44 P2 Cu 115.95(14) . . ? N1 C1 C2 124.1(5) . . ? C3 C2 C1 117.4(6) . . ? C2 C3 C4 120.1(6) . . ? C3 C4 C5 119.0(5) . . ? N1 C5 C4 121.1(5) . . ? N1 C5 C6 114.9(4) . . ? C4 C5 C6 124.0(5) . . ? N2 C6 C7 112.7(5) . . ? N2 C6 C5 118.7(4) . . ? C7 C6 C5 128.6(5) . . ? C6 C7 C8 105.8(5) . . ? C7 C8 C9 136.4(5) . . ? C7 C8 C13 105.7(5) . . ? C9 C8 C13 117.9(5) . . ? C10 C9 C8 119.9(6) . . ? C9 C10 C11 121.7(6) . . ? C12 C11 C10 120.4(6) . . ? C11 C12 C13 119.1(5) . . ? N2 C13 C12 128.9(5) . . ? N2 C13 C8 110.1(5) . . ? C12 C13 C8 120.9(5) . . ? C15 C14 C19 118.0(5) . . ? C15 C14 P1 123.3(4) . . ? C19 C14 P1 118.7(4) . . ? C14 C15 C16 120.7(5) . . ? C17 C16 C15 120.3(5) . . ? C16 C17 C18 120.1(5) . . ? C17 C18 C19 119.4(5) . . ? C18 C19 C14 121.4(5) . . ? C25 C20 C21 116.5(5) . . ? C25 C20 P1 123.4(4) . . ? C21 C20 P1 119.7(4) . . ? C22 C21 C20 121.6(6) . . ? C23 C22 C21 120.3(6) . . ? C22 C23 C24 119.7(7) . . ? C23 C24 C25 120.4(7) . . ? C24 C25 C20 121.4(6) . . ? C27 C26 C31 118.2(5) . . ? C27 C26 P1 125.3(4) . . ? C31 C26 P1 116.5(4) . . ? C26 C27 C28 120.2(6) . . ? C29 C28 C27 120.8(7) . . ? C28 C29 C30 120.0(7) . . ? C31 C30 C29 119.8(6) . . ? C30 C31 C26 121.0(6) . . ? C37 C32 C33 117.6(5) . . ? C37 C32 P2 115.8(4) . . ? C33 C32 P2 126.6(4) . . ? C32 C33 C34 120.3(5) . . ? C35 C34 C33 120.3(5) . . ? C34 C35 C36 120.3(5) . . ? C37 C36 C35 118.7(6) . . ? C36 C37 C32 122.8(6) . . ? C43 C38 C39 118.4(5) . . ? C43 C38 P2 119.7(4) . . ? C39 C38 P2 121.7(4) . . ? C40 C39 C38 121.1(6) . . ? C39 C40 C41 119.8(6) . . ? C42 C41 C40 120.2(6) . . ? C41 C42 C43 120.0(6) . . ? C38 C43 C42 120.4(6) . . ? C49 C44 C45 118.0(5) . . ? C49 C44 P2 121.6(4) . . ? C45 C44 P2 120.2(4) . . ? C46 C45 C44 121.0(5) . . ? C47 C46 C45 119.7(5) . . ? C46 C47 C48 120.2(5) . . ? C47 C48 C49 120.4(5) . . ? C48 C49 C44 120.7(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Cu N1 C1 176.8(5) . . . . ? P2 Cu N1 C1 -64.7(5) . . . . ? P1 Cu N1 C1 63.1(4) . . . . ? N2 Cu N1 C5 5.2(3) . . . . ? P2 Cu N1 C5 123.7(3) . . . . ? P1 Cu N1 C5 -108.5(3) . . . . ? N1 Cu N2 C6 -1.6(3) . . . . ? P2 Cu N2 C6 -114.0(3) . . . . ? P1 Cu N2 C6 99.1(3) . . . . ? N1 Cu N2 C13 178.9(5) . . . . ? P2 Cu N2 C13 66.4(5) . . . . ? P1 Cu N2 C13 -80.4(5) . . . . ? N2 Cu P1 C20 -118.1(2) . . . . ? N1 Cu P1 C20 -31.9(2) . . . . ? P2 Cu P1 C20 94.09(18) . . . . ? N2 Cu P1 C26 120.6(2) . . . . ? N1 Cu P1 C26 -153.2(2) . . . . ? P2 Cu P1 C26 -27.25(19) . . . . ? N2 Cu P1 C14 0.5(2) . . . . ? N1 Cu P1 C14 86.7(2) . . . . ? P2 Cu P1 C14 -147.31(18) . . . . ? N2 Cu P2 C32 -67.6(2) . . . . ? N1 Cu P2 C32 -160.8(2) . . . . ? P1 Cu P2 C32 78.67(18) . . . . ? N2 Cu P2 C38 48.2(2) . . . . ? N1 Cu P2 C38 -44.9(2) . . . . ? P1 Cu P2 C38 -165.50(17) . . . . ? N2 Cu P2 C44 169.9(2) . . . . ? N1 Cu P2 C44 76.8(2) . . . . ? P1 Cu P2 C44 -43.8(2) . . . . ? C5 N1 C1 C2 1.2(8) . . . . ? Cu N1 C1 C2 -170.0(4) . . . . ? N1 C1 C2 C3 -1.1(9) . . . . ? C1 C2 C3 C4 0.0(9) . . . . ? C2 C3 C4 C5 1.0(9) . . . . ? C1 N1 C5 C4 -0.2(7) . . . . ? Cu N1 C5 C4 172.4(4) . . . . ? C1 N1 C5 C6 179.8(4) . . . . ? Cu N1 C5 C6 -7.5(5) . . . . ? C3 C4 C5 N1 -0.9(8) . . . . ? C3 C4 C5 C6 179.1(5) . . . . ? C13 N2 C6 C7 -0.1(5) . . . . ? Cu N2 C6 C7 -179.8(3) . . . . ? C13 N2 C6 C5 177.7(4) . . . . ? Cu N2 C6 C5 -2.0(5) . . . . ? N1 C5 C6 N2 6.7(6) . . . . ? C4 C5 C6 N2 -173.3(5) . . . . ? N1 C5 C6 C7 -176.0(5) . . . . ? C4 C5 C6 C7 4.0(8) . . . . ? N2 C6 C7 C8 -0.6(6) . . . . ? C5 C6 C7 C8 -178.1(4) . . . . ? C6 C7 C8 C9 -178.9(6) . . . . ? C6 C7 C8 C13 1.0(5) . . . . ? C7 C8 C9 C10 -178.7(6) . . . . ? C13 C8 C9 C10 1.4(8) . . . . ? C8 C9 C10 C11 0.2(9) . . . . ? C9 C10 C11 C12 -0.3(9) . . . . ? C10 C11 C12 C13 -1.1(8) . . . . ? C6 N2 C13 C12 -177.5(5) . . . . ? Cu N2 C13 C12 2.1(8) . . . . ? C6 N2 C13 C8 0.8(5) . . . . ? Cu N2 C13 C8 -179.7(4) . . . . ? C11 C12 C13 N2 -179.2(5) . . . . ? C11 C12 C13 C8 2.7(7) . . . . ? C7 C8 C13 N2 -1.1(5) . . . . ? C9 C8 C13 N2 178.8(4) . . . . ? C7 C8 C13 C12 177.3(4) . . . . ? C9 C8 C13 C12 -2.8(7) . . . . ? C20 P1 C14 C15 -87.1(4) . . . . ? C26 P1 C14 C15 21.3(5) . . . . ? Cu P1 C14 C15 149.1(4) . . . . ? C20 P1 C14 C19 94.1(4) . . . . ? C26 P1 C14 C19 -157.5(4) . . . . ? Cu P1 C14 C19 -29.8(5) . . . . ? C19 C14 C15 C16 -0.3(8) . . . . ? P1 C14 C15 C16 -179.1(4) . . . . ? C14 C15 C16 C17 0.1(8) . . . . ? C15 C16 C17 C18 -0.5(9) . . . . ? C16 C17 C18 C19 1.1(9) . . . . ? C17 C18 C19 C14 -1.3(9) . . . . ? C15 C14 C19 C18 0.8(8) . . . . ? P1 C14 C19 C18 179.7(4) . . . . ? C26 P1 C20 C25 -127.1(5) . . . . ? C14 P1 C20 C25 -21.0(5) . . . . ? Cu P1 C20 C25 105.1(4) . . . . ? C26 P1 C20 C21 61.3(4) . . . . ? C14 P1 C20 C21 167.4(4) . . . . ? Cu P1 C20 C21 -66.5(4) . . . . ? C25 C20 C21 C22 4.3(9) . . . . ? P1 C20 C21 C22 176.4(5) . . . . ? C20 C21 C22 C23 -3.7(10) . . . . ? C21 C22 C23 C24 0.8(11) . . . . ? C22 C23 C24 C25 1.3(12) . . . . ? C23 C24 C25 C20 -0.5(11) . . . . ? C21 C20 C25 C24 -2.2(9) . . . . ? P1 C20 C25 C24 -174.0(5) . . . . ? C20 P1 C26 C27 13.2(5) . . . . ? C14 P1 C26 C27 -93.8(5) . . . . ? Cu P1 C26 C27 138.7(4) . . . . ? C20 P1 C26 C31 -169.0(4) . . . . ? C14 P1 C26 C31 84.1(4) . . . . ? Cu P1 C26 C31 -43.5(4) . . . . ? C31 C26 C27 C28 0.0(8) . . . . ? P1 C26 C27 C28 177.7(4) . . . . ? C26 C27 C28 C29 -0.7(9) . . . . ? C27 C28 C29 C30 1.1(11) . . . . ? C28 C29 C30 C31 -0.6(10) . . . . ? C29 C30 C31 C26 -0.2(9) . . . . ? C27 C26 C31 C30 0.5(8) . . . . ? P1 C26 C31 C30 -177.5(4) . . . . ? C38 P2 C32 C37 -75.8(4) . . . . ? C44 P2 C32 C37 177.5(4) . . . . ? Cu P2 C32 C37 49.5(4) . . . . ? C38 P2 C32 C33 104.7(5) . . . . ? C44 P2 C32 C33 -2.1(5) . . . . ? Cu P2 C32 C33 -130.0(4) . . . . ? C37 C32 C33 C34 -1.5(8) . . . . ? P2 C32 C33 C34 178.1(4) . . . . ? C32 C33 C34 C35 0.2(8) . . . . ? C33 C34 C35 C36 1.1(9) . . . . ? C34 C35 C36 C37 -1.1(9) . . . . ? C35 C36 C37 C32 -0.3(9) . . . . ? C33 C32 C37 C36 1.5(8) . . . . ? P2 C32 C37 C36 -178.0(4) . . . . ? C32 P2 C38 C43 124.3(4) . . . . ? C44 P2 C38 C43 -126.6(4) . . . . ? Cu P2 C38 C43 1.7(5) . . . . ? C32 P2 C38 C39 -52.4(5) . . . . ? C44 P2 C38 C39 56.7(5) . . . . ? Cu P2 C38 C39 -175.0(4) . . . . ? C43 C38 C39 C40 1.4(8) . . . . ? P2 C38 C39 C40 178.1(4) . . . . ? C38 C39 C40 C41 -1.4(9) . . . . ? C39 C40 C41 C42 1.5(10) . . . . ? C40 C41 C42 C43 -1.7(10) . . . . ? C39 C38 C43 C42 -1.5(8) . . . . ? P2 C38 C43 C42 -178.4(5) . . . . ? C41 C42 C43 C38 1.7(10) . . . . ? C32 P2 C44 C49 131.6(4) . . . . ? C38 P2 C44 C49 26.7(4) . . . . ? Cu P2 C44 C49 -102.2(4) . . . . ? C32 P2 C44 C45 -53.3(4) . . . . ? C38 P2 C44 C45 -158.2(4) . . . . ? Cu P2 C44 C45 72.8(4) . . . . ? C49 C44 C45 C46 -2.5(6) . . . . ? P2 C44 C45 C46 -177.7(3) . . . . ? C44 C45 C46 C47 1.1(7) . . . . ? C45 C46 C47 C48 0.8(8) . . . . ? C46 C47 C48 C49 -1.2(8) . . . . ? C47 C48 C49 C44 -0.2(8) . . . . ? C45 C44 C49 C48 2.0(7) . . . . ? P2 C44 C49 C48 177.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.527 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.050 # Attachment 'T010.CIF' data_t010 _database_code_depnum_ccdc_archive 'CCDC 828215' #TrackingRef 'T010.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H43 Cl2 Cu N2 P2' _chemical_formula_weight 916.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9902(8) _cell_length_b 12.2055(8) _cell_length_c 19.3749(13) _cell_angle_alpha 75.6690(10) _cell_angle_beta 81.1440(10) _cell_angle_gamma 66.0970(10) _cell_volume 2297.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 186(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_absorpt_coefficient_mu 0.700 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8191 _exptl_absorpt_correction_T_max 0.9289 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 186(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12689 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.72 _reflns_number_total 8560 _reflns_number_gt 6829 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1050P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8560 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1595 _refine_ls_wR_factor_gt 0.1441 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.63613(4) 0.58711(3) 0.709032(19) 0.02766(14) Uani 1 1 d . . . N1 N 0.4870(3) 0.6085(2) 0.64312(13) 0.0317(6) Uani 1 1 d . . . N2 N 0.7106(3) 0.4185(2) 0.68711(14) 0.0331(6) Uani 1 1 d . . . P1 P 0.57129(8) 0.56151(7) 0.82606(4) 0.0289(2) Uani 1 1 d . . . P2 P 0.74578(8) 0.70922(7) 0.65709(4) 0.0291(2) Uani 1 1 d . . . C1 C 0.3807(3) 0.7125(3) 0.61612(16) 0.0325(7) Uani 1 1 d . . . C2 C 0.3573(3) 0.8237(3) 0.63529(18) 0.0375(8) Uani 1 1 d . . . H2A H 0.4126 0.8254 0.6678 0.045 Uiso 1 1 calc R . . C3 C 0.2561(3) 0.9288(3) 0.6076(2) 0.0460(9) Uani 1 1 d . . . H3A H 0.2412 1.0032 0.6211 0.055 Uiso 1 1 calc R . . C4 C 0.1736(4) 0.9278(4) 0.5593(2) 0.0550(11) Uani 1 1 d . . . H4A H 0.1035 1.0015 0.5401 0.066 Uiso 1 1 calc R . . C5 C 0.1939(4) 0.8222(4) 0.5401(2) 0.0488(10) Uani 1 1 d . . . H5A H 0.1381 0.8229 0.5070 0.059 Uiso 1 1 calc R . . C6 C 0.2968(3) 0.7104(4) 0.56848(18) 0.0408(8) Uani 1 1 d . . . C7 C 0.3201(4) 0.5981(4) 0.55108(19) 0.0473(9) Uani 1 1 d . . . H7A H 0.2632 0.5933 0.5206 0.057 Uiso 1 1 calc R . . C8 C 0.4238(4) 0.4973(4) 0.57809(19) 0.0468(9) Uani 1 1 d . . . H8A H 0.4395 0.4210 0.5669 0.056 Uiso 1 1 calc R . . C9 C 0.5097(3) 0.5040(3) 0.62304(17) 0.0360(7) Uani 1 1 d . . . C10 C 0.6293(4) 0.4004(3) 0.64796(18) 0.0385(8) Uani 1 1 d . . . C11 C 0.6778(4) 0.2790(3) 0.6395(2) 0.0507(10) Uani 1 1 d . . . H11A H 0.6389 0.2450 0.6143 0.061 Uiso 1 1 calc R . . C12 C 0.7959(4) 0.2176(3) 0.6762(2) 0.0495(10) Uani 1 1 d . . . C13 C 0.8954(5) 0.0969(4) 0.6876(2) 0.0689(14) Uani 1 1 d . . . H13A H 0.8882 0.0352 0.6687 0.083 Uiso 1 1 calc R . . C14 C 1.0011(5) 0.0710(4) 0.7261(3) 0.0771(16) Uani 1 1 d . . . H14A H 1.0684 -0.0092 0.7326 0.093 Uiso 1 1 calc R . . C15 C 1.0139(5) 0.1585(4) 0.7563(2) 0.0672(13) Uani 1 1 d . . . H15A H 1.0880 0.1361 0.7837 0.081 Uiso 1 1 calc R . . C16 C 0.9187(4) 0.2784(3) 0.7465(2) 0.0494(10) Uani 1 1 d . . . H16A H 0.9266 0.3380 0.7672 0.059 Uiso 1 1 calc R . . C17 C 0.8115(4) 0.3078(3) 0.70537(18) 0.0408(8) Uani 1 1 d . . . C18 C 0.4691(3) 0.4681(3) 0.85493(16) 0.0331(7) Uani 1 1 d . . . C19 C 0.3677(3) 0.4898(3) 0.90721(17) 0.0403(8) Uani 1 1 d . . . H19A H 0.3481 0.5556 0.9305 0.048 Uiso 1 1 calc R . . C20 C 0.2933(4) 0.4166(4) 0.9266(2) 0.0482(9) Uani 1 1 d . . . H20A H 0.2237 0.4327 0.9630 0.058 Uiso 1 1 calc R . . C21 C 0.3197(4) 0.3223(4) 0.8937(2) 0.0512(10) Uani 1 1 d . . . H21A H 0.2682 0.2731 0.9066 0.061 Uiso 1 1 calc R . . C22 C 0.4221(4) 0.2989(4) 0.8414(2) 0.0521(10) Uani 1 1 d . . . H22A H 0.4422 0.2320 0.8190 0.063 Uiso 1 1 calc R . . C23 C 0.4957(4) 0.3718(3) 0.82136(19) 0.0420(8) Uani 1 1 d . . . H23A H 0.5647 0.3560 0.7846 0.050 Uiso 1 1 calc R . . C24 C 0.4751(3) 0.6965(3) 0.86477(16) 0.0324(7) Uani 1 1 d . . . C25 C 0.3538(3) 0.7759(3) 0.8364(2) 0.0464(9) Uani 1 1 d . . . H25A H 0.3227 0.7579 0.7991 0.056 Uiso 1 1 calc R . . C26 C 0.2782(4) 0.8810(4) 0.8623(2) 0.0613(12) Uani 1 1 d . . . H26A H 0.1944 0.9337 0.8433 0.074 Uiso 1 1 calc R . . C27 C 0.3228(5) 0.9103(4) 0.9153(2) 0.0625(12) Uani 1 1 d . . . H27A H 0.2710 0.9834 0.9322 0.075 Uiso 1 1 calc R . . C28 C 0.4420(5) 0.8335(4) 0.9432(2) 0.0597(11) Uani 1 1 d . . . H28A H 0.4732 0.8531 0.9798 0.072 Uiso 1 1 calc R . . C29 C 0.5185(4) 0.7261(3) 0.91835(19) 0.0435(8) Uani 1 1 d . . . H29A H 0.6010 0.6729 0.9384 0.052 Uiso 1 1 calc R . . C30 C 0.7157(3) 0.4777(3) 0.88096(16) 0.0310(7) Uani 1 1 d . . . C31 C 0.8184(3) 0.5197(3) 0.86793(18) 0.0418(8) Uani 1 1 d . . . H31A H 0.8104 0.5919 0.8330 0.050 Uiso 1 1 calc R . . C32 C 0.9333(4) 0.4571(4) 0.9055(2) 0.0540(11) Uani 1 1 d . . . H32A H 1.0029 0.4871 0.8964 0.065 Uiso 1 1 calc R . . C33 C 0.9463(4) 0.3521(4) 0.9557(2) 0.0581(12) Uani 1 1 d . . . H33A H 1.0250 0.3092 0.9812 0.070 Uiso 1 1 calc R . . C34 C 0.8449(4) 0.3090(4) 0.9691(2) 0.0518(10) Uani 1 1 d . . . H34A H 0.8539 0.2363 1.0038 0.062 Uiso 1 1 calc R . . C35 C 0.7293(3) 0.3719(3) 0.93185(18) 0.0399(8) Uani 1 1 d . . . H35A H 0.6595 0.3421 0.9414 0.048 Uiso 1 1 calc R . . C36 C 0.8993(3) 0.6820(3) 0.69694(16) 0.0352(7) Uani 1 1 d . . . C37 C 0.9170(5) 0.7627(4) 0.7293(2) 0.0601(12) Uani 1 1 d . . . H37A H 0.8472 0.8401 0.7310 0.072 Uiso 1 1 calc R . . C38 C 1.0362(6) 0.7314(5) 0.7594(3) 0.0871(18) Uani 1 1 d . . . H38A H 1.0472 0.7867 0.7826 0.105 Uiso 1 1 calc R . . C39 C 1.1390(5) 0.6199(5) 0.7559(3) 0.0764(16) Uani 1 1 d . . . H39A H 1.2217 0.5996 0.7752 0.092 Uiso 1 1 calc R . . C40 C 1.1214(4) 0.5389(5) 0.7246(2) 0.0638(12) Uani 1 1 d . . . H40A H 1.1919 0.4621 0.7223 0.077 Uiso 1 1 calc R . . C41 C 1.0026(4) 0.5683(4) 0.6966(2) 0.0504(10) Uani 1 1 d . . . H41A H 0.9904 0.5103 0.6765 0.060 Uiso 1 1 calc R . . C42 C 0.6446(3) 0.8719(3) 0.65144(18) 0.0341(7) Uani 1 1 d . . . C43 C 0.6144(4) 0.9567(3) 0.5874(2) 0.0434(8) Uani 1 1 d . . . H43A H 0.6577 0.9326 0.5441 0.052 Uiso 1 1 calc R . . C44 C 0.5225(4) 1.0756(4) 0.5853(2) 0.0561(11) Uani 1 1 d . . . H44A H 0.5031 1.1321 0.5410 0.067 Uiso 1 1 calc R . . C45 C 0.4598(4) 1.1112(4) 0.6478(3) 0.0635(12) Uani 1 1 d . . . H45A H 0.3964 1.1924 0.6466 0.076 Uiso 1 1 calc R . . C46 C 0.4886(5) 1.0292(4) 0.7122(3) 0.0634(12) Uani 1 1 d . . . H46A H 0.4456 1.0544 0.7553 0.076 Uiso 1 1 calc R . . C47 C 0.5800(4) 0.9102(3) 0.7143(2) 0.0482(9) Uani 1 1 d . . . H47A H 0.5989 0.8543 0.7588 0.058 Uiso 1 1 calc R . . C48 C 0.8105(3) 0.6964(3) 0.56515(16) 0.0304(7) Uani 1 1 d . . . C49 C 0.9060(4) 0.7420(4) 0.53166(19) 0.0489(10) Uani 1 1 d . . . H49A H 0.9385 0.7818 0.5564 0.059 Uiso 1 1 calc R . . C50 C 0.9543(4) 0.7301(4) 0.4626(2) 0.0505(10) Uani 1 1 d . . . H50A H 1.0192 0.7625 0.4401 0.061 Uiso 1 1 calc R . . C51 C 0.9099(4) 0.6728(3) 0.42672(18) 0.0442(9) Uani 1 1 d . . . H51A H 0.9429 0.6656 0.3791 0.053 Uiso 1 1 calc R . . C52 C 0.8173(4) 0.6252(4) 0.45947(19) 0.0534(10) Uani 1 1 d . . . H52A H 0.7868 0.5843 0.4344 0.064 Uiso 1 1 calc R . . C53 C 0.7673(4) 0.6361(3) 0.52891(18) 0.0414(8) Uani 1 1 d . . . H53A H 0.7036 0.6022 0.5513 0.050 Uiso 1 1 calc R . . C54 C 0.7751(5) 1.0588(5) 0.8784(3) 0.0705(13) Uani 1 1 d . . . H54A H 0.7208 1.1379 0.8928 0.085 Uiso 1 1 calc R . . H54B H 0.8035 1.0766 0.8273 0.085 Uiso 1 1 calc R . . Cl1 Cl 0.6780(2) 0.97202(19) 0.89001(12) 0.1294(7) Uani 1 1 d . . . Cl2 Cl 0.91583(14) 0.98340(15) 0.92843(8) 0.0954(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 Cu 0.0279(2) 0.0269(2) 0.0277(2) -0.00321(15) -0.00148(15) -0.01150(16) N1 0.0310(14) 0.0370(15) 0.0306(14) -0.0070(11) 0.0000(11) -0.0172(12) N2 0.0323(15) 0.0262(14) 0.0378(15) -0.0064(11) 0.0052(12) -0.0109(11) P1 0.0251(4) 0.0320(4) 0.0268(4) -0.0019(3) -0.0020(3) -0.0102(3) P2 0.0326(4) 0.0309(4) 0.0267(4) -0.0033(3) -0.0022(3) -0.0163(4) C1 0.0273(16) 0.0414(19) 0.0281(16) -0.0015(14) 0.0000(13) -0.0163(14) C2 0.0326(18) 0.0405(19) 0.0380(18) -0.0051(15) -0.0034(14) -0.0137(15) C3 0.0350(19) 0.042(2) 0.056(2) -0.0084(17) -0.0003(17) -0.0119(16) C4 0.032(2) 0.058(3) 0.061(3) 0.005(2) -0.0083(18) -0.0111(18) C5 0.036(2) 0.069(3) 0.043(2) 0.0025(19) -0.0138(16) -0.0264(19) C6 0.0361(19) 0.058(2) 0.0341(18) -0.0048(16) 0.0000(14) -0.0277(17) C7 0.051(2) 0.068(3) 0.037(2) -0.0106(18) -0.0029(17) -0.038(2) C8 0.059(2) 0.057(2) 0.041(2) -0.0146(18) 0.0030(18) -0.038(2) C9 0.044(2) 0.0412(19) 0.0316(17) -0.0091(14) 0.0054(14) -0.0268(16) C10 0.048(2) 0.0368(19) 0.0362(18) -0.0104(15) 0.0099(15) -0.0243(16) C11 0.075(3) 0.040(2) 0.044(2) -0.0113(17) 0.0097(19) -0.032(2) C12 0.063(3) 0.0318(19) 0.042(2) -0.0061(16) 0.0196(18) -0.0156(18) C13 0.104(4) 0.027(2) 0.053(3) -0.0058(18) 0.023(3) -0.013(2) C14 0.081(4) 0.036(2) 0.063(3) 0.006(2) 0.021(3) 0.012(2) C15 0.055(3) 0.049(3) 0.060(3) 0.010(2) 0.008(2) 0.002(2) C16 0.042(2) 0.036(2) 0.051(2) 0.0029(16) 0.0052(17) -0.0062(16) C17 0.045(2) 0.0263(17) 0.0381(19) -0.0015(14) 0.0151(15) -0.0098(15) C18 0.0282(16) 0.0383(18) 0.0271(16) 0.0019(13) -0.0051(13) -0.0107(14) C19 0.0351(19) 0.054(2) 0.0289(17) -0.0028(15) -0.0032(14) -0.0174(16) C20 0.0334(19) 0.071(3) 0.039(2) -0.0028(19) 0.0014(15) -0.0260(19) C21 0.045(2) 0.060(3) 0.054(2) 0.003(2) -0.0045(18) -0.034(2) C22 0.054(2) 0.050(2) 0.060(3) -0.0125(19) 0.0022(19) -0.029(2) C23 0.041(2) 0.043(2) 0.042(2) -0.0069(16) 0.0083(16) -0.0215(17) C24 0.0312(17) 0.0315(17) 0.0278(16) -0.0013(13) 0.0040(13) -0.0103(14) C25 0.0344(19) 0.046(2) 0.043(2) -0.0003(16) -0.0032(16) -0.0041(16) C26 0.045(2) 0.042(2) 0.065(3) 0.004(2) 0.006(2) 0.0035(19) C27 0.068(3) 0.034(2) 0.066(3) -0.013(2) 0.022(2) -0.009(2) C28 0.070(3) 0.056(3) 0.058(3) -0.024(2) 0.016(2) -0.029(2) C29 0.041(2) 0.049(2) 0.0386(19) -0.0099(16) 0.0016(15) -0.0169(17) C30 0.0233(15) 0.0330(17) 0.0296(16) -0.0046(13) 0.0002(12) -0.0054(13) C31 0.0328(18) 0.049(2) 0.0369(19) 0.0036(16) -0.0045(15) -0.0157(16) C32 0.0311(19) 0.081(3) 0.046(2) 0.000(2) -0.0047(16) -0.024(2) C33 0.0290(19) 0.075(3) 0.048(2) 0.003(2) -0.0112(17) -0.0037(19) C34 0.042(2) 0.050(2) 0.044(2) 0.0103(17) -0.0089(17) -0.0073(18) C35 0.0335(18) 0.0395(19) 0.0379(19) -0.0015(15) -0.0018(14) -0.0089(15) C36 0.0367(18) 0.044(2) 0.0262(16) 0.0026(14) -0.0049(13) -0.0219(16) C37 0.072(3) 0.046(2) 0.072(3) 0.004(2) -0.035(2) -0.030(2) C38 0.101(4) 0.067(3) 0.115(4) 0.008(3) -0.066(4) -0.048(3) C39 0.070(3) 0.099(4) 0.069(3) 0.022(3) -0.035(3) -0.052(3) C40 0.039(2) 0.085(3) 0.050(2) -0.001(2) -0.0052(19) -0.012(2) C41 0.042(2) 0.059(2) 0.046(2) -0.0141(18) -0.0035(17) -0.0131(19) C42 0.0361(18) 0.0298(17) 0.0416(19) -0.0064(14) -0.0036(14) -0.0179(14) C43 0.048(2) 0.037(2) 0.045(2) -0.0019(16) -0.0043(17) -0.0192(17) C44 0.058(3) 0.039(2) 0.069(3) -0.0005(19) -0.014(2) -0.0182(19) C45 0.058(3) 0.032(2) 0.096(4) -0.012(2) -0.004(3) -0.0136(19) C46 0.074(3) 0.046(2) 0.078(3) -0.029(2) 0.013(2) -0.028(2) C47 0.063(3) 0.041(2) 0.046(2) -0.0101(17) 0.0038(18) -0.0270(19) C48 0.0324(17) 0.0309(17) 0.0272(16) -0.0024(13) -0.0015(13) -0.0138(14) C49 0.060(2) 0.070(3) 0.037(2) -0.0138(18) 0.0056(17) -0.047(2) C50 0.053(2) 0.069(3) 0.040(2) -0.0070(18) 0.0075(17) -0.040(2) C51 0.055(2) 0.048(2) 0.0315(18) -0.0102(16) 0.0071(16) -0.0235(18) C52 0.074(3) 0.072(3) 0.037(2) -0.0198(19) 0.0086(19) -0.050(2) C53 0.046(2) 0.054(2) 0.0364(19) -0.0090(16) 0.0021(15) -0.0337(18) C54 0.059(3) 0.071(3) 0.068(3) -0.001(2) -0.002(2) -0.018(2) Cl1 0.1280(16) 0.1249(15) 0.1589(19) -0.0256(13) -0.0233(13) -0.0691(13) Cl2 0.0637(8) 0.1071(11) 0.0815(9) 0.0085(8) -0.0107(7) -0.0123(7) _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 Cu N2 2.012(3) . ? Cu N1 2.125(2) . ? Cu P2 2.2419(9) . ? Cu P1 2.2536(9) . ? N1 C9 1.341(4) . ? N1 C1 1.381(4) . ? N2 C17 1.360(4) . ? N2 C10 1.369(4) . ? P1 C24 1.830(3) . ? P1 C30 1.833(3) . ? P1 C18 1.845(3) . ? P2 C42 1.825(3) . ? P2 C48 1.833(3) . ? P2 C36 1.837(3) . ? C1 C2 1.408(5) . ? C1 C6 1.413(4) . ? C2 C3 1.363(5) . ? C3 C4 1.406(5) . ? C4 C5 1.352(6) . ? C5 C6 1.419(5) . ? C6 C7 1.405(5) . ? C7 C8 1.348(5) . ? C8 C9 1.416(5) . ? C9 C10 1.452(5) . ? C10 C11 1.399(5) . ? C11 C12 1.409(6) . ? C12 C13 1.422(5) . ? C12 C17 1.432(5) . ? C13 C14 1.362(7) . ? C14 C15 1.400(7) . ? C15 C16 1.399(5) . ? C16 C17 1.399(5) . ? C18 C19 1.372(5) . ? C18 C23 1.390(5) . ? C19 C20 1.392(5) . ? C20 C21 1.361(6) . ? C21 C22 1.381(6) . ? C22 C23 1.383(5) . ? C24 C29 1.383(5) . ? C24 C25 1.391(4) . ? C25 C26 1.384(5) . ? C26 C27 1.379(6) . ? C27 C28 1.364(6) . ? C28 C29 1.397(5) . ? C30 C31 1.385(5) . ? C30 C35 1.386(5) . ? C31 C32 1.390(5) . ? C32 C33 1.374(6) . ? C33 C34 1.380(6) . ? C34 C35 1.394(5) . ? C36 C37 1.378(5) . ? C36 C41 1.393(5) . ? C37 C38 1.387(6) . ? C38 C39 1.382(7) . ? C39 C40 1.368(7) . ? C40 C41 1.368(5) . ? C42 C43 1.390(5) . ? C42 C47 1.398(5) . ? C43 C44 1.387(5) . ? C44 C45 1.374(6) . ? C45 C46 1.381(6) . ? C46 C47 1.386(6) . ? C48 C53 1.379(4) . ? C48 C49 1.384(5) . ? C49 C50 1.381(5) . ? C50 C51 1.353(5) . ? C51 C52 1.369(5) . ? C52 C53 1.390(5) . ? C54 Cl1 1.743(5) . ? C54 Cl2 1.745(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu N1 80.76(11) . . ? N2 Cu P2 116.53(8) . . ? N1 Cu P2 110.67(7) . . ? N2 Cu P1 105.38(8) . . ? N1 Cu P1 112.90(7) . . ? P2 Cu P1 122.90(3) . . ? C9 N1 C1 118.4(3) . . ? C9 N1 Cu 111.8(2) . . ? C1 N1 Cu 129.7(2) . . ? C17 N2 C10 106.1(3) . . ? C17 N2 Cu 140.1(3) . . ? C10 N2 Cu 113.3(2) . . ? C24 P1 C30 104.03(14) . . ? C24 P1 C18 102.61(15) . . ? C30 P1 C18 103.29(14) . . ? C24 P1 Cu 119.21(10) . . ? C30 P1 Cu 110.93(10) . . ? C18 P1 Cu 115.04(10) . . ? C42 P2 C48 104.57(15) . . ? C42 P2 C36 105.31(15) . . ? C48 P2 C36 100.06(15) . . ? C42 P2 Cu 113.70(11) . . ? C48 P2 Cu 114.60(11) . . ? C36 P2 Cu 116.96(11) . . ? N1 C1 C2 119.2(3) . . ? N1 C1 C6 121.5(3) . . ? C2 C1 C6 119.3(3) . . ? C3 C2 C1 120.7(3) . . ? C2 C3 C4 120.3(4) . . ? C5 C4 C3 120.1(3) . . ? C4 C5 C6 121.3(3) . . ? C7 C6 C1 118.5(3) . . ? C7 C6 C5 123.3(3) . . ? C1 C6 C5 118.2(3) . . ? C8 C7 C6 119.3(3) . . ? C7 C8 C9 120.6(3) . . ? N1 C9 C8 121.6(3) . . ? N1 C9 C10 116.0(3) . . ? C8 C9 C10 122.4(3) . . ? N2 C10 C11 111.8(3) . . ? N2 C10 C9 117.9(3) . . ? C11 C10 C9 130.3(3) . . ? C10 C11 C12 105.9(3) . . ? C11 C12 C13 135.8(4) . . ? C11 C12 C17 105.7(3) . . ? C13 C12 C17 118.4(4) . . ? C14 C13 C12 119.1(4) . . ? C13 C14 C15 122.3(4) . . ? C16 C15 C14 120.7(5) . . ? C15 C16 C17 117.9(4) . . ? N2 C17 C16 128.0(3) . . ? N2 C17 C12 110.5(3) . . ? C16 C17 C12 121.5(3) . . ? C19 C18 C23 118.7(3) . . ? C19 C18 P1 123.3(3) . . ? C23 C18 P1 118.0(3) . . ? C18 C19 C20 120.8(4) . . ? C21 C20 C19 120.4(4) . . ? C20 C21 C22 119.4(4) . . ? C21 C22 C23 120.6(4) . . ? C22 C23 C18 120.1(3) . . ? C29 C24 C25 118.5(3) . . ? C29 C24 P1 123.9(3) . . ? C25 C24 P1 117.6(3) . . ? C26 C25 C24 120.2(4) . . ? C27 C26 C25 120.8(4) . . ? C28 C27 C26 119.5(4) . . ? C27 C28 C29 120.3(4) . . ? C24 C29 C28 120.7(4) . . ? C31 C30 C35 119.0(3) . . ? C31 C30 P1 117.8(2) . . ? C35 C30 P1 123.2(3) . . ? C30 C31 C32 120.6(3) . . ? C33 C32 C31 120.1(4) . . ? C32 C33 C34 119.9(3) . . ? C33 C34 C35 120.1(4) . . ? C30 C35 C34 120.3(3) . . ? C37 C36 C41 118.4(3) . . ? C37 C36 P2 125.1(3) . . ? C41 C36 P2 116.4(3) . . ? C36 C37 C38 120.3(4) . . ? C39 C38 C37 120.1(5) . . ? C40 C39 C38 119.9(4) . . ? C39 C40 C41 120.1(4) . . ? C40 C41 C36 121.1(4) . . ? C43 C42 C47 117.9(3) . . ? C43 C42 P2 123.7(3) . . ? C47 C42 P2 117.9(3) . . ? C44 C43 C42 121.5(4) . . ? C45 C44 C43 119.6(4) . . ? C44 C45 C46 120.2(4) . . ? C45 C46 C47 120.3(4) . . ? C46 C47 C42 120.5(4) . . ? C53 C48 C49 118.7(3) . . ? C53 C48 P2 119.7(2) . . ? C49 C48 P2 121.6(2) . . ? C50 C49 C48 120.6(3) . . ? C51 C50 C49 120.6(3) . . ? C50 C51 C52 119.6(3) . . ? C51 C52 C53 120.8(3) . . ? C48 C53 C52 119.7(3) . . ? Cl1 C54 Cl2 111.9(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 N2 Cu N1 C9 3.0(2) . . . . ? P2 Cu N1 C9 118.0(2) . . . . ? P1 Cu N1 C9 -99.9(2) . . . . ? N2 Cu N1 C1 -172.5(3) . . . . ? P2 Cu N1 C1 -57.5(3) . . . . ? P1 Cu N1 C1 84.6(3) . . . . ? N1 Cu N2 C17 -174.1(4) . . . . ? P2 Cu N2 C17 77.4(4) . . . . ? P1 Cu N2 C17 -62.7(4) . . . . ? N1 Cu N2 C10 -4.2(2) . . . . ? P2 Cu N2 C10 -112.7(2) . . . . ? P1 Cu N2 C10 107.2(2) . . . . ? N2 Cu P1 C24 -171.09(14) . . . . ? N1 Cu P1 C24 -84.79(15) . . . . ? P2 Cu P1 C24 52.05(13) . . . . ? N2 Cu P1 C30 68.17(14) . . . . ? N1 Cu P1 C30 154.47(14) . . . . ? P2 Cu P1 C30 -68.68(12) . . . . ? N2 Cu P1 C18 -48.60(14) . . . . ? N1 Cu P1 C18 37.70(14) . . . . ? P2 Cu P1 C18 174.55(11) . . . . ? N2 Cu P2 C42 158.52(14) . . . . ? N1 Cu P2 C42 68.72(14) . . . . ? P1 Cu P2 C42 -68.95(12) . . . . ? N2 Cu P2 C48 38.32(14) . . . . ? N1 Cu P2 C48 -51.48(14) . . . . ? P1 Cu P2 C48 170.85(11) . . . . ? N2 Cu P2 C36 -78.32(15) . . . . ? N1 Cu P2 C36 -168.12(14) . . . . ? P1 Cu P2 C36 54.20(13) . . . . ? C9 N1 C1 C2 -178.5(3) . . . . ? Cu N1 C1 C2 -3.3(4) . . . . ? C9 N1 C1 C6 0.0(5) . . . . ? Cu N1 C1 C6 175.3(2) . . . . ? N1 C1 C2 C3 177.7(3) . . . . ? C6 C1 C2 C3 -0.9(5) . . . . ? C1 C2 C3 C4 -0.2(6) . . . . ? C2 C3 C4 C5 0.2(6) . . . . ? C3 C4 C5 C6 0.7(6) . . . . ? N1 C1 C6 C7 2.7(5) . . . . ? C2 C1 C6 C7 -178.7(3) . . . . ? N1 C1 C6 C5 -176.8(3) . . . . ? C2 C1 C6 C5 1.8(5) . . . . ? C4 C5 C6 C7 178.8(4) . . . . ? C4 C5 C6 C1 -1.7(5) . . . . ? C1 C6 C7 C8 -2.3(5) . . . . ? C5 C6 C7 C8 177.1(4) . . . . ? C6 C7 C8 C9 -0.6(6) . . . . ? C1 N1 C9 C8 -3.1(5) . . . . ? Cu N1 C9 C8 -179.2(3) . . . . ? C1 N1 C9 C10 174.8(3) . . . . ? Cu N1 C9 C10 -1.3(4) . . . . ? C7 C8 C9 N1 3.5(5) . . . . ? C7 C8 C9 C10 -174.3(3) . . . . ? C17 N2 C10 C11 -1.0(4) . . . . ? Cu N2 C10 C11 -174.3(2) . . . . ? C17 N2 C10 C9 178.1(3) . . . . ? Cu N2 C10 C9 4.9(4) . . . . ? N1 C9 C10 N2 -2.3(4) . . . . ? C8 C9 C10 N2 175.5(3) . . . . ? N1 C9 C10 C11 176.7(3) . . . . ? C8 C9 C10 C11 -5.5(6) . . . . ? N2 C10 C11 C12 0.5(4) . . . . ? C9 C10 C11 C12 -178.5(3) . . . . ? C10 C11 C12 C13 -178.0(4) . . . . ? C10 C11 C12 C17 0.2(4) . . . . ? C11 C12 C13 C14 178.4(4) . . . . ? C17 C12 C13 C14 0.4(6) . . . . ? C12 C13 C14 C15 1.5(7) . . . . ? C13 C14 C15 C16 -1.5(7) . . . . ? C14 C15 C16 C17 -0.4(6) . . . . ? C10 N2 C17 C16 -178.8(3) . . . . ? Cu N2 C17 C16 -8.4(6) . . . . ? C10 N2 C17 C12 1.2(4) . . . . ? Cu N2 C17 C12 171.5(3) . . . . ? C15 C16 C17 N2 -177.7(4) . . . . ? C15 C16 C17 C12 2.4(5) . . . . ? C11 C12 C17 N2 -0.9(4) . . . . ? C13 C12 C17 N2 177.7(3) . . . . ? C11 C12 C17 C16 179.1(3) . . . . ? C13 C12 C17 C16 -2.4(5) . . . . ? C24 P1 C18 C19 -14.2(3) . . . . ? C30 P1 C18 C19 93.7(3) . . . . ? Cu P1 C18 C19 -145.2(2) . . . . ? C24 P1 C18 C23 165.2(3) . . . . ? C30 P1 C18 C23 -86.9(3) . . . . ? Cu P1 C18 C23 34.1(3) . . . . ? C23 C18 C19 C20 0.3(5) . . . . ? P1 C18 C19 C20 179.7(2) . . . . ? C18 C19 C20 C21 -0.2(5) . . . . ? C19 C20 C21 C22 0.7(6) . . . . ? C20 C21 C22 C23 -1.3(6) . . . . ? C21 C22 C23 C18 1.4(6) . . . . ? C19 C18 C23 C22 -0.9(5) . . . . ? P1 C18 C23 C22 179.7(3) . . . . ? C30 P1 C24 C29 6.1(3) . . . . ? C18 P1 C24 C29 113.4(3) . . . . ? Cu P1 C24 C29 -118.1(3) . . . . ? C30 P1 C24 C25 -176.6(3) . . . . ? C18 P1 C24 C25 -69.2(3) . . . . ? Cu P1 C24 C25 59.3(3) . . . . ? C29 C24 C25 C26 -0.9(5) . . . . ? P1 C24 C25 C26 -178.4(3) . . . . ? C24 C25 C26 C27 1.5(6) . . . . ? C25 C26 C27 C28 -1.1(7) . . . . ? C26 C27 C28 C29 0.1(7) . . . . ? C25 C24 C29 C28 -0.1(5) . . . . ? P1 C24 C29 C28 177.3(3) . . . . ? C27 C28 C29 C24 0.5(6) . . . . ? C24 P1 C30 C31 -78.2(3) . . . . ? C18 P1 C30 C31 174.9(3) . . . . ? Cu P1 C30 C31 51.1(3) . . . . ? C24 P1 C30 C35 105.1(3) . . . . ? C18 P1 C30 C35 -1.7(3) . . . . ? Cu P1 C30 C35 -125.5(3) . . . . ? C35 C30 C31 C32 -0.3(5) . . . . ? P1 C30 C31 C32 -177.1(3) . . . . ? C30 C31 C32 C33 0.5(6) . . . . ? C31 C32 C33 C34 -0.3(7) . . . . ? C32 C33 C34 C35 -0.1(6) . . . . ? C31 C30 C35 C34 -0.1(5) . . . . ? P1 C30 C35 C34 176.6(3) . . . . ? C33 C34 C35 C30 0.3(6) . . . . ? C42 P2 C36 C37 12.8(4) . . . . ? C48 P2 C36 C37 121.1(3) . . . . ? Cu P2 C36 C37 -114.5(3) . . . . ? C42 P2 C36 C41 -170.1(3) . . . . ? C48 P2 C36 C41 -61.8(3) . . . . ? Cu P2 C36 C41 62.6(3) . . . . ? C41 C36 C37 C38 1.2(6) . . . . ? P2 C36 C37 C38 178.3(4) . . . . ? C36 C37 C38 C39 1.3(8) . . . . ? C37 C38 C39 C40 -2.1(8) . . . . ? C38 C39 C40 C41 0.3(7) . . . . ? C39 C40 C41 C36 2.2(6) . . . . ? C37 C36 C41 C40 -3.0(6) . . . . ? P2 C36 C41 C40 179.7(3) . . . . ? C48 P2 C42 C43 7.9(3) . . . . ? C36 P2 C42 C43 112.9(3) . . . . ? Cu P2 C42 C43 -117.8(3) . . . . ? C48 P2 C42 C47 179.3(3) . . . . ? C36 P2 C42 C47 -75.7(3) . . . . ? Cu P2 C42 C47 53.6(3) . . . . ? C47 C42 C43 C44 -0.4(5) . . . . ? P2 C42 C43 C44 171.0(3) . . . . ? C42 C43 C44 C45 0.2(6) . . . . ? C43 C44 C45 C46 0.4(7) . . . . ? C44 C45 C46 C47 -0.6(7) . . . . ? C45 C46 C47 C42 0.3(6) . . . . ? C43 C42 C47 C46 0.2(5) . . . . ? P2 C42 C47 C46 -171.7(3) . . . . ? C42 P2 C48 C53 -111.9(3) . . . . ? C36 P2 C48 C53 139.2(3) . . . . ? Cu P2 C48 C53 13.2(3) . . . . ? C42 P2 C48 C49 70.5(3) . . . . ? C36 P2 C48 C49 -38.3(3) . . . . ? Cu P2 C48 C49 -164.3(3) . . . . ? C53 C48 C49 C50 1.7(6) . . . . ? P2 C48 C49 C50 179.3(3) . . . . ? C48 C49 C50 C51 -0.6(6) . . . . ? C49 C50 C51 C52 -0.6(6) . . . . ? C50 C51 C52 C53 0.6(6) . . . . ? C49 C48 C53 C52 -1.7(5) . . . . ? P2 C48 C53 C52 -179.3(3) . . . . ? C51 C52 C53 C48 0.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.72 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.662 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.074 # Attachment 'T015.CIF' data_t015 _database_code_depnum_ccdc_archive 'CCDC 828216' #TrackingRef 'T015.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H43 Cu N2 O2 P2' _chemical_formula_weight 877.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7152(9) _cell_length_b 12.1017(9) _cell_length_c 16.7936(12) _cell_angle_alpha 74.3790(10) _cell_angle_beta 77.3600(10) _cell_angle_gamma 70.7180(10) _cell_volume 2142.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 186(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.630 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8832 _exptl_absorpt_correction_T_max 0.9316 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 186(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12056 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0733 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 26.05 _reflns_number_total 8233 _reflns_number_gt 6055 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+1.2131P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8233 _refine_ls_number_parameters 558 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1707 _refine_ls_wR_factor_gt 0.1519 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.61906(4) 0.84745(4) 0.71548(3) 0.02518(16) Uani 1 1 d . . . N1 N 0.6083(3) 0.7858(3) 0.6125(2) 0.0269(7) Uani 1 1 d . . . N2 N 0.4578(3) 0.9682(3) 0.6846(2) 0.0271(8) Uani 1 1 d . . . O1 O 0.8617(2) 0.6474(3) 0.79879(17) 0.0315(7) Uani 1 1 d . . . P1 P 0.78146(9) 0.89988(9) 0.72471(6) 0.0247(2) Uani 1 1 d . . . P2 P 0.58436(9) 0.69507(9) 0.82621(6) 0.0251(2) Uani 1 1 d . . . C1 C 0.6849(4) 0.6874(4) 0.5822(3) 0.0314(10) Uani 1 1 d . . . C2 C 0.7963(4) 0.6250(4) 0.6142(3) 0.0347(10) Uani 1 1 d . . . H2A H 0.8181 0.6522 0.6552 0.042 Uiso 1 1 calc R . . C3 C 0.8724(5) 0.5263(4) 0.5866(3) 0.0438(12) Uani 1 1 d . . . H3A H 0.9472 0.4855 0.6085 0.053 Uiso 1 1 calc R . . C4 C 0.8421(5) 0.4836(5) 0.5262(3) 0.0524(14) Uani 1 1 d . . . H4A H 0.8960 0.4146 0.5073 0.063 Uiso 1 1 calc R . . C5 C 0.7360(5) 0.5414(5) 0.4952(3) 0.0523(14) Uani 1 1 d . . . H5A H 0.7157 0.5119 0.4548 0.063 Uiso 1 1 calc R . . C6 C 0.6536(5) 0.6455(4) 0.5215(3) 0.0413(11) Uani 1 1 d . . . C7 C 0.5426(5) 0.7122(5) 0.4899(3) 0.0521(14) Uani 1 1 d . . . H7A H 0.5196 0.6884 0.4476 0.062 Uiso 1 1 calc R . . C8 C 0.4693(5) 0.8089(5) 0.5190(3) 0.0467(12) Uani 1 1 d . . . H8A H 0.3950 0.8535 0.4974 0.056 Uiso 1 1 calc R . . C9 C 0.5035(4) 0.8441(4) 0.5824(3) 0.0323(10) Uani 1 1 d . . . C10 C 0.4257(4) 0.9437(4) 0.6188(3) 0.0319(10) Uani 1 1 d . . . C11 C 0.3176(4) 1.0266(4) 0.5940(3) 0.0420(12) Uani 1 1 d . . . H11A H 0.2771 1.0270 0.5506 0.050 Uiso 1 1 calc R . . C12 C 0.2808(4) 1.1096(4) 0.6465(3) 0.0379(11) Uani 1 1 d . . . C13 C 0.1856(4) 1.2170(5) 0.6496(3) 0.0508(14) Uani 1 1 d . . . H13A H 0.1273 1.2450 0.6119 0.061 Uiso 1 1 calc R . . C14 C 0.1785(5) 1.2797(5) 0.7073(3) 0.0545(15) Uani 1 1 d . . . H14A H 0.1152 1.3525 0.7094 0.065 Uiso 1 1 calc R . . C15 C 0.2638(4) 1.2384(4) 0.7644(3) 0.0456(12) Uani 1 1 d . . . H15A H 0.2560 1.2834 0.8047 0.055 Uiso 1 1 calc R . . C16 C 0.3583(4) 1.1340(4) 0.7625(3) 0.0378(11) Uani 1 1 d . . . H16A H 0.4146 1.1065 0.8015 0.045 Uiso 1 1 calc R . . C17 C 0.3696(4) 1.0691(4) 0.7020(3) 0.0313(10) Uani 1 1 d . . . C18 C 0.9208(4) 0.8558(4) 0.6520(2) 0.0260(9) Uani 1 1 d . . . C19 C 1.0379(4) 0.8184(4) 0.6720(3) 0.0408(11) Uani 1 1 d . . . H19A H 1.0502 0.8082 0.7279 0.049 Uiso 1 1 calc R . . C20 C 1.1386(4) 0.7955(5) 0.6096(3) 0.0520(14) Uani 1 1 d . . . H20A H 1.2190 0.7698 0.6235 0.062 Uiso 1 1 calc R . . C21 C 1.1219(4) 0.8099(4) 0.5287(3) 0.0431(12) Uani 1 1 d . . . H21A H 1.1904 0.7948 0.4865 0.052 Uiso 1 1 calc R . . C22 C 1.0062(5) 0.8460(4) 0.5094(3) 0.0428(12) Uani 1 1 d . . . H22A H 0.9945 0.8557 0.4534 0.051 Uiso 1 1 calc R . . C23 C 0.9057(4) 0.8688(4) 0.5699(3) 0.0336(10) Uani 1 1 d . . . H23A H 0.8258 0.8934 0.5553 0.040 Uiso 1 1 calc R . . C24 C 0.7628(4) 1.0596(4) 0.7104(2) 0.0280(9) Uani 1 1 d . . . C25 C 0.8564(4) 1.1053(4) 0.7133(3) 0.0351(10) Uani 1 1 d . . . H25A H 0.9356 1.0522 0.7207 0.042 Uiso 1 1 calc R . . C26 C 0.8357(5) 1.2257(4) 0.7057(3) 0.0418(12) Uani 1 1 d . . . H26A H 0.9005 1.2553 0.7075 0.050 Uiso 1 1 calc R . . C27 C 0.7199(5) 1.3049(4) 0.6953(3) 0.0417(12) Uani 1 1 d . . . H27A H 0.7047 1.3880 0.6919 0.050 Uiso 1 1 calc R . . C28 C 0.6278(4) 1.2612(4) 0.6899(3) 0.0390(11) Uani 1 1 d . . . H28A H 0.5492 1.3147 0.6810 0.047 Uiso 1 1 calc R . . C29 C 0.6494(4) 1.1397(4) 0.6973(3) 0.0322(10) Uani 1 1 d . . . H29A H 0.5852 1.1106 0.6935 0.039 Uiso 1 1 calc R . . C30 C 0.8304(4) 0.8369(4) 0.8280(2) 0.0297(9) Uani 1 1 d . . . C31 C 0.8301(4) 0.9034(4) 0.8843(3) 0.0386(11) Uani 1 1 d . . . H31A H 0.8107 0.9882 0.8673 0.046 Uiso 1 1 calc R . . C32 C 0.8576(5) 0.8485(5) 0.9645(3) 0.0500(14) Uani 1 1 d . . . H32A H 0.8579 0.8951 1.0018 0.060 Uiso 1 1 calc R . . C33 C 0.8842(4) 0.7261(5) 0.9894(3) 0.0481(13) Uani 1 1 d . . . H33A H 0.9012 0.6888 1.0447 0.058 Uiso 1 1 calc R . . C34 C 0.8870(4) 0.6563(5) 0.9364(3) 0.0387(11) Uani 1 1 d . . . H34A H 0.9069 0.5715 0.9540 0.046 Uiso 1 1 calc R . . C35 C 0.8599(4) 0.7128(4) 0.8565(3) 0.0315(10) Uani 1 1 d . . . C36 C 0.8257(4) 0.5431(4) 0.8312(3) 0.0306(9) Uani 1 1 d . . . C37 C 0.9157(4) 0.4358(4) 0.8416(3) 0.0400(11) Uani 1 1 d . . . H37A H 0.9992 0.4342 0.8278 0.048 Uiso 1 1 calc R . . C38 C 0.8841(4) 0.3293(4) 0.8724(3) 0.0404(11) Uani 1 1 d . . . H38A H 0.9458 0.2546 0.8801 0.049 Uiso 1 1 calc R . . C39 C 0.7625(4) 0.3332(4) 0.8916(3) 0.0392(11) Uani 1 1 d . . . H39A H 0.7403 0.2609 0.9131 0.047 Uiso 1 1 calc R . . C40 C 0.6724(4) 0.4419(4) 0.8798(3) 0.0324(10) Uani 1 1 d . . . H40A H 0.5891 0.4430 0.8935 0.039 Uiso 1 1 calc R . . C41 C 0.7016(4) 0.5510(4) 0.8479(2) 0.0273(9) Uani 1 1 d . . . C42 C 0.5433(4) 0.7443(4) 0.9250(2) 0.0271(9) Uani 1 1 d . . . C43 C 0.5833(4) 0.6750(4) 0.9998(3) 0.0331(10) Uani 1 1 d . . . H43A H 0.6368 0.5961 1.0018 0.040 Uiso 1 1 calc R . . C44 C 0.5446(4) 0.7214(5) 1.0719(3) 0.0405(11) Uani 1 1 d . . . H44A H 0.5727 0.6741 1.1228 0.049 Uiso 1 1 calc R . . C45 C 0.4663(5) 0.8346(5) 1.0698(3) 0.0443(12) Uani 1 1 d . . . H45A H 0.4397 0.8650 1.1194 0.053 Uiso 1 1 calc R . . C46 C 0.4256(4) 0.9052(4) 0.9953(3) 0.0429(12) Uani 1 1 d . . . H46A H 0.3712 0.9837 0.9937 0.051 Uiso 1 1 calc R . . C47 C 0.4653(4) 0.8595(4) 0.9235(3) 0.0362(10) Uani 1 1 d . . . H47A H 0.4388 0.9078 0.8724 0.043 Uiso 1 1 calc R . . C48 C 0.4535(4) 0.6458(4) 0.8222(3) 0.0284(9) Uani 1 1 d . . . C49 C 0.3508(4) 0.6541(4) 0.8833(3) 0.0379(11) Uani 1 1 d . . . H49A H 0.3483 0.6824 0.9314 0.045 Uiso 1 1 calc R . . C50 C 0.2521(4) 0.6213(4) 0.8743(4) 0.0494(13) Uani 1 1 d . . . H50A H 0.1818 0.6292 0.9156 0.059 Uiso 1 1 calc R . . C51 C 0.2550(5) 0.5777(5) 0.8065(4) 0.0529(14) Uani 1 1 d . . . H51A H 0.1876 0.5543 0.8014 0.063 Uiso 1 1 calc R . . C52 C 0.3562(5) 0.5677(5) 0.7453(3) 0.0499(13) Uani 1 1 d . . . H52A H 0.3588 0.5371 0.6982 0.060 Uiso 1 1 calc R . . C53 C 0.4539(4) 0.6027(4) 0.7532(3) 0.0392(11) Uani 1 1 d . . . H53A H 0.5226 0.5971 0.7106 0.047 Uiso 1 1 calc R . . C54 C 0.1451(7) 0.9431(7) 0.8556(6) 0.090(2) Uani 1 1 d . . . O21 O 0.0816(5) 1.0586(5) 0.8479(4) 0.0591(17) Uani 0.60 1 d P . . O22 O 0.1606(18) 0.9097(18) 0.7865(13) 0.060(5) Uiso 0.20 1 d P . . O23 O 0.095(2) 0.948(2) 0.9446(16) 0.089(7) Uiso 0.20 1 d P . . 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 Cu 0.0226(3) 0.0286(3) 0.0207(3) -0.0003(2) -0.00687(19) -0.0043(2) N1 0.0305(19) 0.0287(18) 0.0202(17) -0.0018(14) -0.0030(14) -0.0101(15) N2 0.0252(18) 0.0289(18) 0.0237(18) 0.0010(14) -0.0073(14) -0.0061(15) O1 0.0285(16) 0.0349(17) 0.0254(16) 0.0039(13) -0.0084(12) -0.0071(13) P1 0.0229(5) 0.0286(6) 0.0195(5) -0.0010(4) -0.0049(4) -0.0054(4) P2 0.0215(5) 0.0268(5) 0.0214(5) 0.0017(4) -0.0049(4) -0.0037(4) C1 0.037(2) 0.034(2) 0.022(2) 0.0000(18) -0.0007(18) -0.016(2) C2 0.043(3) 0.031(2) 0.026(2) -0.0012(18) 0.0004(19) -0.013(2) C3 0.040(3) 0.035(3) 0.049(3) -0.004(2) 0.002(2) -0.010(2) C4 0.061(4) 0.033(3) 0.053(3) -0.013(2) 0.008(3) -0.008(3) C5 0.071(4) 0.050(3) 0.042(3) -0.022(3) 0.008(3) -0.027(3) C6 0.050(3) 0.045(3) 0.032(3) -0.010(2) -0.001(2) -0.019(2) C7 0.063(4) 0.071(4) 0.035(3) -0.019(3) -0.012(2) -0.026(3) C8 0.046(3) 0.064(3) 0.035(3) -0.013(2) -0.012(2) -0.015(3) C9 0.032(2) 0.040(3) 0.024(2) 0.0013(19) -0.0073(18) -0.014(2) C10 0.030(2) 0.039(2) 0.024(2) 0.0003(18) -0.0097(17) -0.0086(19) C11 0.035(3) 0.054(3) 0.033(3) -0.002(2) -0.017(2) -0.006(2) C12 0.028(2) 0.044(3) 0.034(3) 0.002(2) -0.0110(19) -0.004(2) C13 0.033(3) 0.057(3) 0.046(3) -0.002(3) -0.013(2) 0.005(2) C14 0.035(3) 0.046(3) 0.057(3) -0.006(3) -0.004(2) 0.016(2) C15 0.042(3) 0.042(3) 0.044(3) -0.013(2) 0.001(2) -0.002(2) C16 0.031(2) 0.043(3) 0.034(3) -0.004(2) 0.0003(19) -0.010(2) C17 0.026(2) 0.035(2) 0.027(2) 0.0001(18) -0.0050(17) -0.0050(19) C18 0.027(2) 0.025(2) 0.024(2) -0.0020(16) -0.0021(16) -0.0085(17) C19 0.029(2) 0.054(3) 0.029(2) -0.002(2) -0.0062(19) -0.004(2) C20 0.029(3) 0.067(4) 0.047(3) -0.006(3) -0.001(2) -0.005(2) C21 0.041(3) 0.041(3) 0.041(3) -0.012(2) 0.011(2) -0.012(2) C22 0.059(3) 0.050(3) 0.024(2) -0.011(2) 0.003(2) -0.024(3) C23 0.032(2) 0.044(3) 0.024(2) -0.0066(19) -0.0062(18) -0.009(2) C24 0.029(2) 0.036(2) 0.017(2) -0.0048(17) -0.0019(16) -0.0092(18) C25 0.032(2) 0.039(3) 0.034(2) -0.008(2) -0.0058(19) -0.008(2) C26 0.046(3) 0.048(3) 0.039(3) -0.015(2) 0.002(2) -0.025(2) C27 0.062(3) 0.031(2) 0.029(3) -0.006(2) 0.001(2) -0.015(2) C28 0.039(3) 0.037(3) 0.035(3) -0.002(2) -0.007(2) -0.005(2) C29 0.033(2) 0.033(2) 0.028(2) -0.0032(18) -0.0043(18) -0.0090(19) C30 0.026(2) 0.039(2) 0.019(2) -0.0019(18) -0.0031(16) -0.0072(19) C31 0.039(3) 0.046(3) 0.027(2) -0.007(2) -0.0053(19) -0.008(2) C32 0.045(3) 0.077(4) 0.029(3) -0.018(3) -0.011(2) -0.009(3) C33 0.041(3) 0.075(4) 0.023(2) -0.001(2) -0.013(2) -0.012(3) C34 0.028(2) 0.052(3) 0.030(2) 0.005(2) -0.0123(19) -0.009(2) C35 0.021(2) 0.046(3) 0.026(2) -0.0034(19) -0.0050(17) -0.0099(19) C36 0.031(2) 0.032(2) 0.023(2) 0.0020(18) -0.0053(17) -0.0074(19) C37 0.029(2) 0.040(3) 0.039(3) 0.000(2) -0.0097(19) 0.001(2) C38 0.042(3) 0.032(2) 0.038(3) -0.002(2) -0.016(2) 0.002(2) C39 0.046(3) 0.032(2) 0.036(3) -0.003(2) -0.012(2) -0.006(2) C40 0.029(2) 0.035(2) 0.029(2) -0.0035(19) -0.0051(18) -0.0072(19) C41 0.027(2) 0.029(2) 0.019(2) 0.0029(17) -0.0070(16) -0.0033(18) C42 0.024(2) 0.033(2) 0.022(2) -0.0008(17) -0.0032(16) -0.0099(18) C43 0.026(2) 0.039(3) 0.032(2) 0.0010(19) -0.0062(18) -0.0121(19) C44 0.047(3) 0.056(3) 0.022(2) -0.001(2) -0.009(2) -0.022(2) C45 0.048(3) 0.060(3) 0.035(3) -0.017(2) -0.002(2) -0.024(3) C46 0.042(3) 0.037(3) 0.049(3) -0.016(2) 0.000(2) -0.009(2) C47 0.041(3) 0.033(2) 0.031(2) -0.0014(19) -0.0053(19) -0.010(2) C48 0.025(2) 0.024(2) 0.032(2) 0.0024(17) -0.0099(17) -0.0057(17) C49 0.032(2) 0.038(3) 0.039(3) -0.002(2) -0.005(2) -0.009(2) C50 0.025(2) 0.044(3) 0.070(4) 0.002(3) -0.006(2) -0.010(2) C51 0.041(3) 0.047(3) 0.075(4) 0.005(3) -0.025(3) -0.020(3) C52 0.058(3) 0.044(3) 0.056(3) -0.003(2) -0.027(3) -0.019(3) C53 0.041(3) 0.041(3) 0.036(3) 0.000(2) -0.008(2) -0.017(2) C54 0.065(4) 0.075(5) 0.131(7) -0.013(5) -0.026(5) -0.019(4) O21 0.043(3) 0.028(3) 0.086(5) -0.005(3) 0.006(3) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N2 2.042(3) . ? Cu N1 2.101(3) . ? Cu P1 2.2418(12) . ? Cu P2 2.3112(11) . ? N1 C9 1.329(5) . ? N1 C1 1.379(5) . ? N2 C17 1.368(5) . ? N2 C10 1.372(5) . ? O1 C36 1.396(5) . ? O1 C35 1.400(5) . ? P1 C24 1.827(4) . ? P1 C18 1.828(4) . ? P1 C30 1.831(4) . ? P2 C42 1.826(4) . ? P2 C41 1.831(4) . ? P2 C48 1.839(4) . ? C1 C2 1.413(6) . ? C1 C6 1.413(6) . ? C2 C3 1.360(6) . ? C3 C4 1.410(7) . ? C4 C5 1.348(8) . ? C5 C6 1.422(7) . ? C6 C7 1.415(7) . ? C7 C8 1.345(7) . ? C8 C9 1.420(6) . ? C9 C10 1.444(6) . ? C10 C11 1.397(6) . ? C11 C12 1.414(7) . ? C12 C13 1.410(7) . ? C12 C17 1.426(6) . ? C13 C14 1.357(8) . ? C14 C15 1.413(7) . ? C15 C16 1.380(6) . ? C16 C17 1.403(6) . ? C18 C19 1.382(6) . ? C18 C23 1.388(6) . ? C19 C20 1.401(6) . ? C20 C21 1.372(7) . ? C21 C22 1.363(7) . ? C22 C23 1.382(6) . ? C24 C29 1.384(6) . ? C24 C25 1.396(6) . ? C25 C26 1.370(6) . ? C26 C27 1.394(7) . ? C27 C28 1.378(7) . ? C28 C29 1.383(6) . ? C30 C31 1.395(6) . ? C30 C35 1.395(6) . ? C31 C32 1.389(6) . ? C32 C33 1.372(8) . ? C33 C34 1.372(7) . ? C34 C35 1.385(6) . ? C36 C37 1.372(6) . ? C36 C41 1.395(6) . ? C37 C38 1.393(7) . ? C38 C39 1.378(7) . ? C39 C40 1.385(6) . ? C40 C41 1.408(6) . ? C42 C43 1.389(6) . ? C42 C47 1.389(6) . ? C43 C44 1.394(6) . ? C44 C45 1.370(7) . ? C45 C46 1.394(7) . ? C46 C47 1.384(6) . ? C48 C53 1.393(6) . ? C48 C49 1.394(6) . ? C49 C50 1.390(6) . ? C50 C51 1.367(8) . ? C51 C52 1.384(8) . ? C52 C53 1.386(6) . ? C54 O22 1.29(2) . ? C54 O21 1.335(9) . ? C54 O23 1.49(3) . ? O21 O23 1.81(3) . ? 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 N2 Cu N1 81.93(13) . . ? N2 Cu P1 123.58(10) . . ? N1 Cu P1 122.46(10) . . ? N2 Cu P2 110.74(10) . . ? N1 Cu P2 102.16(9) . . ? P1 Cu P2 111.48(4) . . ? C9 N1 C1 119.1(4) . . ? C9 N1 Cu 111.6(3) . . ? C1 N1 Cu 128.7(3) . . ? C17 N2 C10 105.7(3) . . ? C17 N2 Cu 144.2(3) . . ? C10 N2 Cu 110.0(3) . . ? C36 O1 C35 116.4(3) . . ? C24 P1 C18 101.08(18) . . ? C24 P1 C30 103.04(19) . . ? C18 P1 C30 104.16(19) . . ? C24 P1 Cu 117.24(14) . . ? C18 P1 Cu 117.63(14) . . ? C30 P1 Cu 111.81(14) . . ? C42 P2 C41 103.99(18) . . ? C42 P2 C48 103.12(19) . . ? C41 P2 C48 101.10(19) . . ? C42 P2 Cu 111.22(14) . . ? C41 P2 Cu 121.36(13) . . ? C48 P2 Cu 114.00(13) . . ? N1 C1 C2 119.2(4) . . ? N1 C1 C6 121.7(4) . . ? C2 C1 C6 119.1(4) . . ? C3 C2 C1 120.5(4) . . ? C2 C3 C4 121.0(5) . . ? C5 C4 C3 119.5(5) . . ? C4 C5 C6 121.7(5) . . ? C1 C6 C7 117.2(4) . . ? C1 C6 C5 118.3(5) . . ? C7 C6 C5 124.5(5) . . ? C8 C7 C6 120.6(5) . . ? C7 C8 C9 119.6(5) . . ? N1 C9 C8 121.8(4) . . ? N1 C9 C10 116.2(4) . . ? C8 C9 C10 122.0(4) . . ? N2 C10 C11 111.9(4) . . ? N2 C10 C9 119.9(4) . . ? C11 C10 C9 128.1(4) . . ? C10 C11 C12 106.0(4) . . ? C13 C12 C11 133.8(4) . . ? C13 C12 C17 120.5(4) . . ? C11 C12 C17 105.7(4) . . ? C14 C13 C12 118.9(5) . . ? C13 C14 C15 121.1(5) . . ? C16 C15 C14 121.2(5) . . ? C15 C16 C17 118.9(5) . . ? N2 C17 C16 129.8(4) . . ? N2 C17 C12 110.8(4) . . ? C16 C17 C12 119.4(4) . . ? C19 C18 C23 118.8(4) . . ? C19 C18 P1 124.7(3) . . ? C23 C18 P1 116.4(3) . . ? C18 C19 C20 119.9(4) . . ? C21 C20 C19 120.6(5) . . ? C22 C21 C20 119.3(4) . . ? C21 C22 C23 121.1(4) . . ? C22 C23 C18 120.4(4) . . ? C29 C24 C25 118.1(4) . . ? C29 C24 P1 118.4(3) . . ? C25 C24 P1 123.5(3) . . ? C26 C25 C24 120.9(4) . . ? C25 C26 C27 120.4(4) . . ? C28 C27 C26 119.2(4) . . ? C27 C28 C29 120.1(4) . . ? C24 C29 C28 121.2(4) . . ? C31 C30 C35 116.6(4) . . ? C31 C30 P1 125.3(3) . . ? C35 C30 P1 117.8(3) . . ? C32 C31 C30 121.5(5) . . ? C33 C32 C31 119.2(5) . . ? C32 C33 C34 121.7(5) . . ? C33 C34 C35 118.1(5) . . ? C34 C35 C30 122.9(4) . . ? C34 C35 O1 121.3(4) . . ? C30 C35 O1 115.8(4) . . ? C37 C36 C41 122.8(4) . . ? C37 C36 O1 117.7(4) . . ? C41 C36 O1 119.4(4) . . ? C36 C37 C38 119.7(4) . . ? C39 C38 C37 119.3(4) . . ? C38 C39 C40 120.4(4) . . ? C39 C40 C41 121.5(4) . . ? C36 C41 C40 116.2(4) . . ? C36 C41 P2 121.5(3) . . ? C40 C41 P2 122.3(3) . . ? C43 C42 C47 119.0(4) . . ? C43 C42 P2 124.9(3) . . ? C47 C42 P2 116.1(3) . . ? C42 C43 C44 119.9(4) . . ? C45 C44 C43 120.5(4) . . ? C44 C45 C46 120.2(4) . . ? C47 C46 C45 119.1(4) . . ? C46 C47 C42 121.2(4) . . ? C53 C48 C49 117.9(4) . . ? C53 C48 P2 118.7(3) . . ? C49 C48 P2 123.4(3) . . ? C50 C49 C48 120.5(5) . . ? C51 C50 C49 120.7(5) . . ? C50 C51 C52 120.0(5) . . ? C51 C52 C53 119.5(5) . . ? C52 C53 C48 121.4(5) . . ? O22 C54 O21 110.6(11) . . ? O22 C54 O23 156.1(15) . . ? O21 C54 O23 79.3(11) . . ? C54 O21 O23 54.1(9) . . ? C54 O23 O21 46.5(8) . . ? 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 N2 Cu N1 C9 -5.0(3) . . . . ? P1 Cu N1 C9 -129.9(3) . . . . ? P2 Cu N1 C9 104.6(3) . . . . ? N2 Cu N1 C1 -175.7(4) . . . . ? P1 Cu N1 C1 59.4(4) . . . . ? P2 Cu N1 C1 -66.1(3) . . . . ? N1 Cu N2 C17 -173.5(5) . . . . ? P1 Cu N2 C17 -49.6(5) . . . . ? P2 Cu N2 C17 86.5(5) . . . . ? N1 Cu N2 C10 2.7(3) . . . . ? P1 Cu N2 C10 126.5(3) . . . . ? P2 Cu N2 C10 -97.3(3) . . . . ? N2 Cu P1 C24 4.22(19) . . . . ? N1 Cu P1 C24 107.09(18) . . . . ? P2 Cu P1 C24 -131.67(14) . . . . ? N2 Cu P1 C18 -116.67(18) . . . . ? N1 Cu P1 C18 -13.81(19) . . . . ? P2 Cu P1 C18 107.44(15) . . . . ? N2 Cu P1 C30 122.87(18) . . . . ? N1 Cu P1 C30 -134.27(18) . . . . ? P2 Cu P1 C30 -13.03(16) . . . . ? N2 Cu P2 C42 -77.02(17) . . . . ? N1 Cu P2 C42 -162.90(17) . . . . ? P1 Cu P2 C42 64.66(14) . . . . ? N2 Cu P2 C41 160.26(19) . . . . ? N1 Cu P2 C41 74.39(19) . . . . ? P1 Cu P2 C41 -58.05(17) . . . . ? N2 Cu P2 C48 39.05(19) . . . . ? N1 Cu P2 C48 -46.83(18) . . . . ? P1 Cu P2 C48 -179.27(15) . . . . ? C9 N1 C1 C2 -179.9(4) . . . . ? Cu N1 C1 C2 -9.8(6) . . . . ? C9 N1 C1 C6 -1.5(6) . . . . ? Cu N1 C1 C6 168.6(3) . . . . ? N1 C1 C2 C3 178.7(4) . . . . ? C6 C1 C2 C3 0.2(6) . . . . ? C1 C2 C3 C4 -0.3(7) . . . . ? C2 C3 C4 C5 0.0(8) . . . . ? C3 C4 C5 C6 0.5(8) . . . . ? N1 C1 C6 C7 2.9(7) . . . . ? C2 C1 C6 C7 -178.6(4) . . . . ? N1 C1 C6 C5 -178.2(4) . . . . ? C2 C1 C6 C5 0.2(7) . . . . ? C4 C5 C6 C1 -0.6(8) . . . . ? C4 C5 C6 C7 178.2(5) . . . . ? C1 C6 C7 C8 -2.0(8) . . . . ? C5 C6 C7 C8 179.2(5) . . . . ? C6 C7 C8 C9 -0.3(8) . . . . ? C1 N1 C9 C8 -1.0(6) . . . . ? Cu N1 C9 C8 -172.7(4) . . . . ? C1 N1 C9 C10 178.0(4) . . . . ? Cu N1 C9 C10 6.3(5) . . . . ? C7 C8 C9 N1 1.9(8) . . . . ? C7 C8 C9 C10 -177.0(5) . . . . ? C17 N2 C10 C11 -0.5(5) . . . . ? Cu N2 C10 C11 -178.2(3) . . . . ? C17 N2 C10 C9 177.5(4) . . . . ? Cu N2 C10 C9 -0.2(5) . . . . ? N1 C9 C10 N2 -4.3(6) . . . . ? C8 C9 C10 N2 174.6(4) . . . . ? N1 C9 C10 C11 173.3(4) . . . . ? C8 C9 C10 C11 -7.8(7) . . . . ? N2 C10 C11 C12 1.1(5) . . . . ? C9 C10 C11 C12 -176.7(4) . . . . ? C10 C11 C12 C13 175.0(5) . . . . ? C10 C11 C12 C17 -1.2(5) . . . . ? C11 C12 C13 C14 -177.1(5) . . . . ? C17 C12 C13 C14 -1.3(8) . . . . ? C12 C13 C14 C15 -0.7(8) . . . . ? C13 C14 C15 C16 1.0(8) . . . . ? C14 C15 C16 C17 0.7(7) . . . . ? C10 N2 C17 C16 -179.0(4) . . . . ? Cu N2 C17 C16 -2.8(8) . . . . ? C10 N2 C17 C12 -0.3(5) . . . . ? Cu N2 C17 C12 175.9(4) . . . . ? C15 C16 C17 N2 176.0(4) . . . . ? C15 C16 C17 C12 -2.7(7) . . . . ? C13 C12 C17 N2 -175.9(4) . . . . ? C11 C12 C17 N2 1.0(5) . . . . ? C13 C12 C17 C16 3.0(7) . . . . ? C11 C12 C17 C16 179.8(4) . . . . ? C24 P1 C18 C19 88.7(4) . . . . ? C30 P1 C18 C19 -17.9(4) . . . . ? Cu P1 C18 C19 -142.3(4) . . . . ? C24 P1 C18 C23 -87.1(3) . . . . ? C30 P1 C18 C23 166.2(3) . . . . ? Cu P1 C18 C23 41.9(4) . . . . ? C23 C18 C19 C20 0.6(7) . . . . ? P1 C18 C19 C20 -175.1(4) . . . . ? C18 C19 C20 C21 0.0(8) . . . . ? C19 C20 C21 C22 -0.4(8) . . . . ? C20 C21 C22 C23 0.2(8) . . . . ? C21 C22 C23 C18 0.4(7) . . . . ? C19 C18 C23 C22 -0.8(7) . . . . ? P1 C18 C23 C22 175.3(4) . . . . ? C18 P1 C24 C29 131.3(3) . . . . ? C30 P1 C24 C29 -121.2(3) . . . . ? Cu P1 C24 C29 2.0(4) . . . . ? C18 P1 C24 C25 -49.9(4) . . . . ? C30 P1 C24 C25 57.7(4) . . . . ? Cu P1 C24 C25 -179.1(3) . . . . ? C29 C24 C25 C26 1.7(6) . . . . ? P1 C24 C25 C26 -177.2(3) . . . . ? C24 C25 C26 C27 0.3(7) . . . . ? C25 C26 C27 C28 -2.2(7) . . . . ? C26 C27 C28 C29 2.0(7) . . . . ? C25 C24 C29 C28 -1.9(6) . . . . ? P1 C24 C29 C28 177.0(3) . . . . ? C27 C28 C29 C24 0.1(7) . . . . ? C24 P1 C30 C31 9.9(4) . . . . ? C18 P1 C30 C31 115.1(4) . . . . ? Cu P1 C30 C31 -116.9(4) . . . . ? C24 P1 C30 C35 -176.4(3) . . . . ? C18 P1 C30 C35 -71.2(4) . . . . ? Cu P1 C30 C35 56.8(3) . . . . ? C35 C30 C31 C32 -0.1(6) . . . . ? P1 C30 C31 C32 173.7(4) . . . . ? C30 C31 C32 C33 -0.8(7) . . . . ? C31 C32 C33 C34 1.4(8) . . . . ? C32 C33 C34 C35 -1.1(7) . . . . ? C33 C34 C35 C30 0.1(6) . . . . ? C33 C34 C35 O1 179.6(4) . . . . ? C31 C30 C35 C34 0.5(6) . . . . ? P1 C30 C35 C34 -173.8(3) . . . . ? C31 C30 C35 O1 -179.0(3) . . . . ? P1 C30 C35 O1 6.7(5) . . . . ? C36 O1 C35 C34 33.8(5) . . . . ? C36 O1 C35 C30 -146.7(4) . . . . ? C35 O1 C36 C37 -100.5(4) . . . . ? C35 O1 C36 C41 82.5(5) . . . . ? C41 C36 C37 C38 -2.1(7) . . . . ? O1 C36 C37 C38 -178.9(4) . . . . ? C36 C37 C38 C39 0.4(7) . . . . ? C37 C38 C39 C40 0.5(7) . . . . ? C38 C39 C40 C41 0.1(7) . . . . ? C37 C36 C41 C40 2.6(6) . . . . ? O1 C36 C41 C40 179.5(4) . . . . ? C37 C36 C41 P2 -175.6(3) . . . . ? O1 C36 C41 P2 1.2(5) . . . . ? C39 C40 C41 C36 -1.7(6) . . . . ? C39 C40 C41 P2 176.5(3) . . . . ? C42 P2 C41 C36 -93.5(4) . . . . ? C48 P2 C41 C36 159.8(3) . . . . ? Cu P2 C41 C36 32.6(4) . . . . ? C42 P2 C41 C40 88.4(4) . . . . ? C48 P2 C41 C40 -18.3(4) . . . . ? Cu P2 C41 C40 -145.5(3) . . . . ? C41 P2 C42 C43 -8.1(4) . . . . ? C48 P2 C42 C43 97.1(4) . . . . ? Cu P2 C42 C43 -140.3(3) . . . . ? C41 P2 C42 C47 172.6(3) . . . . ? C48 P2 C42 C47 -82.2(4) . . . . ? Cu P2 C42 C47 40.3(4) . . . . ? C47 C42 C43 C44 0.2(6) . . . . ? P2 C42 C43 C44 -179.1(3) . . . . ? C42 C43 C44 C45 0.7(7) . . . . ? C43 C44 C45 C46 -0.8(7) . . . . ? C44 C45 C46 C47 0.0(7) . . . . ? C45 C46 C47 C42 1.0(7) . . . . ? C43 C42 C47 C46 -1.1(7) . . . . ? P2 C42 C47 C46 178.3(4) . . . . ? C42 P2 C48 C53 179.5(3) . . . . ? C41 P2 C48 C53 -73.1(4) . . . . ? Cu P2 C48 C53 58.8(4) . . . . ? C42 P2 C48 C49 2.3(4) . . . . ? C41 P2 C48 C49 109.7(4) . . . . ? Cu P2 C48 C49 -118.4(3) . . . . ? C53 C48 C49 C50 -0.7(6) . . . . ? P2 C48 C49 C50 176.5(3) . . . . ? C48 C49 C50 C51 1.6(7) . . . . ? C49 C50 C51 C52 -1.1(8) . . . . ? C50 C51 C52 C53 -0.3(8) . . . . ? C51 C52 C53 C48 1.2(7) . . . . ? C49 C48 C53 C52 -0.7(7) . . . . ? P2 C48 C53 C52 -178.0(4) . . . . ? O22 C54 O21 O23 157.4(15) . . . . ? O22 C54 O23 O21 -117(4) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.717 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.087