# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ad-mar13 #TrackingRef 'ad-mar13.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H47 Cu O5 P2' _chemical_formula_sum 'C45 H47 Cu O5 P2' _chemical_formula_weight 793.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0902(10) _cell_length_b 13.2571(9) _cell_length_c 13.3691(10) _cell_angle_alpha 86.456(6) _cell_angle_beta 89.537(7) _cell_angle_gamma 64.306(7) _cell_volume 1926.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 104.8(4) _cell_measurement_reflns_used 6161 _cell_measurement_theta_min 3.3101 _cell_measurement_theta_max 70.3856 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 1.954 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.97516 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 104.8(4) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini S' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time 10 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14265 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 66.98 _reflns_number_total 6810 _reflns_number_gt 6042 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0987P)^2^+0.8903P] 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 6810 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1482 _refine_ls_wR_factor_gt 0.1424 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 C1 C 0.8062(2) 0.1983(2) 0.58869(19) 0.0229(5) Uani 1 1 d . . . C2 C 0.8245(3) 0.2084(2) 0.4741(2) 0.0262(6) Uani 1 1 d . . . C3 C 0.7740(3) 0.1358(3) 0.4248(2) 0.0381(7) Uani 1 1 d . . . H3A H 0.6895 0.1596 0.4420 0.057 Uiso 1 1 calc R . . H3B H 0.8206 0.0588 0.4481 0.057 Uiso 1 1 calc R . . H3C H 0.7801 0.1433 0.3534 0.057 Uiso 1 1 calc R . . C4 C 0.9582(3) 0.1722(3) 0.4478(2) 0.0349(7) Uani 1 1 d . . . H4A H 0.9888 0.2185 0.4793 0.052 Uiso 1 1 calc R . . H4B H 0.9650 0.1798 0.3764 0.052 Uiso 1 1 calc R . . H4C H 1.0055 0.0953 0.4712 0.052 Uiso 1 1 calc R . . C5 C 0.7737(3) 0.4041(3) 0.4691(2) 0.0351(7) Uani 1 1 d . . . H5A H 0.8401 0.4099 0.4319 0.042 Uiso 1 1 calc R . . H5B H 0.7976 0.3882 0.5395 0.042 Uiso 1 1 calc R . . C6 C 0.6571(3) 0.5121(3) 0.4543(2) 0.0364(7) Uani 1 1 d . . . H6A H 0.6414 0.5333 0.3832 0.044 Uiso 1 1 calc R . . H6B H 0.5883 0.5007 0.4810 0.044 Uiso 1 1 calc R . . C7 C 0.5574(3) 0.6990(3) 0.4970(2) 0.0353(7) Uani 1 1 d . . . H7A H 0.5435 0.7320 0.5614 0.042 Uiso 1 1 calc R . . H7B H 0.4899 0.6805 0.4836 0.042 Uiso 1 1 calc R . . C8 C 0.5567(3) 0.7849(3) 0.4171(2) 0.0380(7) Uani 1 1 d . . . H8A H 0.5940 0.7481 0.3570 0.046 Uiso 1 1 calc R . . H8B H 0.4728 0.8384 0.4005 0.046 Uiso 1 1 calc R . . C9 C 0.6092(4) 0.9338(3) 0.3871(3) 0.0478(8) Uani 1 1 d . . . H9A H 0.6550 0.9705 0.4131 0.072 Uiso 1 1 calc R . . H9B H 0.5240 0.9857 0.3811 0.072 Uiso 1 1 calc R . . H9C H 0.6392 0.9080 0.3223 0.072 Uiso 1 1 calc R . . C10 C 0.6976(2) -0.0269(2) 0.7978(2) 0.0225(5) Uani 1 1 d . . . C11 C 0.7384(2) -0.0444(2) 0.7001(2) 0.0258(5) Uani 1 1 d . . . H11 H 0.7619 0.0062 0.6659 0.031 Uiso 1 1 calc R . . C12 C 0.7443(3) -0.1376(3) 0.6533(2) 0.0306(6) Uani 1 1 d . . . H12 H 0.7719 -0.1490 0.5880 0.037 Uiso 1 1 calc R . . C13 C 0.7095(3) -0.2128(2) 0.7035(2) 0.0319(6) Uani 1 1 d . . . H13 H 0.7109 -0.2735 0.6712 0.038 Uiso 1 1 calc R . . C14 C 0.6724(3) -0.1979(2) 0.8022(2) 0.0305(6) Uani 1 1 d . . . H14 H 0.6505 -0.2496 0.8366 0.037 Uiso 1 1 calc R . . C15 C 0.6678(3) -0.1060(2) 0.8496(2) 0.0273(6) Uani 1 1 d . . . H15 H 0.6448 -0.0971 0.9163 0.033 Uiso 1 1 calc R . . C16 C 0.5183(2) 0.1929(2) 0.85189(18) 0.0217(5) Uani 1 1 d . . . C17 C 0.4295(3) 0.1540(2) 0.8727(2) 0.0282(6) Uani 1 1 d . . . H17 H 0.4533 0.0777 0.8862 0.034 Uiso 1 1 calc R . . C18 C 0.3063(3) 0.2281(3) 0.8733(2) 0.0319(6) Uani 1 1 d . . . H18 H 0.2479 0.2015 0.8877 0.038 Uiso 1 1 calc R . . C19 C 0.2696(3) 0.3426(3) 0.8525(2) 0.0310(6) Uani 1 1 d . . . H19 H 0.1868 0.3924 0.8526 0.037 Uiso 1 1 calc R . . C20 C 0.3569(3) 0.3819(2) 0.8315(2) 0.0291(6) Uani 1 1 d . . . H20 H 0.3329 0.4582 0.8178 0.035 Uiso 1 1 calc R . . C21 C 0.4802(3) 0.3074(2) 0.83112(19) 0.0245(5) Uani 1 1 d . . . H21 H 0.5383 0.3343 0.8168 0.029 Uiso 1 1 calc R . . C22 C 0.7264(2) 0.0567(2) 0.98303(19) 0.0213(5) Uani 1 1 d . . . C23 C 0.6445(2) 0.0943(2) 1.0611(2) 0.0246(5) Uani 1 1 d . . . H23 H 0.5618 0.1398 1.0469 0.030 Uiso 1 1 calc R . . C24 C 0.6858(3) 0.0639(2) 1.1606(2) 0.0290(6) Uani 1 1 d . . . H24 H 0.6306 0.0888 1.2125 0.035 Uiso 1 1 calc R . . C25 C 0.8088(3) -0.0033(2) 1.1818(2) 0.0323(6) Uani 1 1 d . . . H25 H 0.8366 -0.0226 1.2481 0.039 Uiso 1 1 calc R . . C26 C 0.8907(3) -0.0419(2) 1.1046(2) 0.0300(6) Uani 1 1 d . . . H26 H 0.9733 -0.0878 1.1190 0.036 Uiso 1 1 calc R . . C27 C 0.8496(3) -0.0120(2) 1.0056(2) 0.0264(5) Uani 1 1 d . . . H27 H 0.9049 -0.0382 0.9540 0.032 Uiso 1 1 calc R . . C28 C 0.6762(2) 0.4610(2) 0.82903(19) 0.0204(5) Uani 1 1 d . . . C29 C 0.6082(2) 0.4980(2) 0.7395(2) 0.0253(5) Uani 1 1 d . . . H29 H 0.6398 0.4608 0.6817 0.030 Uiso 1 1 calc R . . C30 C 0.4936(3) 0.5901(2) 0.7356(2) 0.0268(6) Uani 1 1 d . . . H30 H 0.4494 0.6151 0.6753 0.032 Uiso 1 1 calc R . . C31 C 0.4461(3) 0.6439(2) 0.8220(2) 0.0280(6) Uani 1 1 d . . . H31 H 0.3689 0.7044 0.8202 0.034 Uiso 1 1 calc R . . C32 C 0.5131(3) 0.6080(2) 0.9115(2) 0.0299(6) Uani 1 1 d . . . H32 H 0.4810 0.6450 0.9693 0.036 Uiso 1 1 calc R . . C33 C 0.6280(3) 0.5170(2) 0.9148(2) 0.0256(5) Uani 1 1 d . . . H33 H 0.6729 0.4934 0.9748 0.031 Uiso 1 1 calc R . . C34 C 0.8868(2) 0.3188(2) 0.95423(19) 0.0225(5) Uani 1 1 d . . . C35 C 0.8522(3) 0.2631(2) 1.0313(2) 0.0265(6) Uani 1 1 d . . . H35 H 0.7956 0.2352 1.0185 0.032 Uiso 1 1 calc R . . C36 C 0.9020(3) 0.2494(3) 1.1270(2) 0.0313(6) Uani 1 1 d . . . H36 H 0.8778 0.2129 1.1781 0.038 Uiso 1 1 calc R . . C37 C 0.9871(3) 0.2893(3) 1.1471(2) 0.0343(6) Uani 1 1 d . . . H37 H 1.0211 0.2789 1.2113 0.041 Uiso 1 1 calc R . . C38 C 1.0217(3) 0.3452(3) 1.0710(2) 0.0343(7) Uani 1 1 d . . . H38 H 1.0788 0.3725 1.0842 0.041 Uiso 1 1 calc R . . C39 C 0.9710(3) 0.3604(2) 0.9751(2) 0.0287(6) Uani 1 1 d . . . H39 H 0.9936 0.3987 0.9245 0.034 Uiso 1 1 calc R . . C40 C 0.9171(2) 0.3724(2) 0.74644(18) 0.0207(5) Uani 1 1 d . . . C41 C 0.8998(3) 0.4829(2) 0.7275(2) 0.0273(6) Uani 1 1 d . . . H41 H 0.8375 0.5404 0.7591 0.033 Uiso 1 1 calc R . . C42 C 0.9751(3) 0.5071(3) 0.6618(2) 0.0333(6) Uani 1 1 d . . . H42 H 0.9624 0.5811 0.6485 0.040 Uiso 1 1 calc R . . C43 C 1.0698(3) 0.4214(3) 0.6156(2) 0.0312(6) Uani 1 1 d . . . H43 H 1.1209 0.4379 0.5720 0.037 Uiso 1 1 calc R . . C44 C 1.0877(2) 0.3122(3) 0.6342(2) 0.0282(6) Uani 1 1 d . . . H44 H 1.1514 0.2548 0.6036 0.034 Uiso 1 1 calc R . . C45 C 1.0109(2) 0.2872(2) 0.6989(2) 0.0248(5) Uani 1 1 d . . . H45 H 1.0223 0.2134 0.7103 0.030 Uiso 1 1 calc R . . O1 O 0.70536(18) 0.26342(17) 0.62376(14) 0.0280(4) Uani 1 1 d . . . O2 O 0.89157(18) 0.12384(16) 0.64198(14) 0.0271(4) Uani 1 1 d . . . O3 O 0.7474(2) 0.31876(17) 0.43328(15) 0.0341(5) Uani 1 1 d . . . O4 O 0.6680(2) 0.59899(18) 0.50314(17) 0.0370(5) Uani 1 1 d . . . O5 O 0.6230(2) 0.84150(18) 0.45282(16) 0.0359(5) Uani 1 1 d . . . P1 P 0.68372(6) 0.10179(5) 0.85139(4) 0.01955(17) Uani 1 1 d . . . P2 P 0.81949(5) 0.33263(5) 0.82905(4) 0.01865(16) Uani 1 1 d . . . Cu1 Cu 0.77971(3) 0.19385(3) 0.77491(3) 0.02035(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0255(13) 0.0236(12) 0.0228(13) -0.0003(10) 0.0010(10) -0.0138(11) C2 0.0262(14) 0.0234(13) 0.0230(13) 0.0021(10) 0.0023(10) -0.0056(11) C3 0.0355(16) 0.0499(19) 0.0254(14) -0.0047(13) -0.0020(12) -0.0150(14) C4 0.0287(15) 0.0399(16) 0.0295(14) 0.0005(12) 0.0067(12) -0.0092(13) C5 0.0306(15) 0.0324(15) 0.0409(16) 0.0049(12) 0.0044(12) -0.0133(13) C6 0.0350(16) 0.0342(16) 0.0354(16) 0.0024(12) -0.0053(13) -0.0113(13) C7 0.0309(15) 0.0327(15) 0.0436(17) 0.0035(13) -0.0035(13) -0.0156(13) C8 0.0331(16) 0.0396(17) 0.0398(17) 0.0019(13) -0.0108(13) -0.0149(14) C9 0.056(2) 0.0336(17) 0.053(2) 0.0144(15) -0.0095(17) -0.0201(16) C10 0.0183(12) 0.0212(12) 0.0256(13) 0.0012(10) -0.0030(10) -0.0067(10) C11 0.0256(13) 0.0261(13) 0.0240(13) 0.0047(10) -0.0024(10) -0.0103(11) C12 0.0304(14) 0.0332(14) 0.0251(13) -0.0042(11) -0.0014(11) -0.0106(12) C13 0.0277(14) 0.0238(13) 0.0418(16) -0.0035(12) -0.0068(12) -0.0088(11) C14 0.0264(14) 0.0246(13) 0.0401(16) 0.0049(11) -0.0014(12) -0.0114(11) C15 0.0243(13) 0.0265(13) 0.0306(14) 0.0029(11) 0.0031(11) -0.0112(11) C16 0.0201(12) 0.0255(13) 0.0183(11) 0.0021(9) -0.0011(9) -0.0092(10) C17 0.0255(14) 0.0280(13) 0.0307(14) 0.0046(11) 0.0008(11) -0.0120(12) C18 0.0225(14) 0.0378(16) 0.0361(15) 0.0028(12) 0.0017(11) -0.0146(12) C19 0.0201(13) 0.0361(15) 0.0308(14) 0.0011(12) 0.0004(11) -0.0069(12) C20 0.0274(14) 0.0254(13) 0.0306(14) 0.0011(11) -0.0011(11) -0.0081(12) C21 0.0242(13) 0.0262(13) 0.0237(12) 0.0021(10) -0.0019(10) -0.0120(11) C22 0.0244(12) 0.0186(11) 0.0221(12) 0.0027(9) -0.0001(10) -0.0110(10) C23 0.0241(13) 0.0218(12) 0.0250(13) 0.0029(10) 0.0028(10) -0.0080(10) C24 0.0358(15) 0.0249(13) 0.0215(13) 0.0012(10) 0.0060(11) -0.0091(12) C25 0.0430(17) 0.0250(13) 0.0237(13) 0.0048(11) -0.0028(12) -0.0108(13) C26 0.0260(14) 0.0282(14) 0.0278(14) 0.0056(11) -0.0060(11) -0.0052(11) C27 0.0230(13) 0.0265(13) 0.0267(13) 0.0014(10) 0.0041(10) -0.0085(11) C28 0.0185(12) 0.0198(12) 0.0234(12) 0.0019(9) 0.0027(10) -0.0092(10) C29 0.0229(13) 0.0256(13) 0.0227(12) -0.0019(10) 0.0014(10) -0.0061(11) C30 0.0237(13) 0.0249(13) 0.0281(13) 0.0042(10) -0.0045(11) -0.0078(11) C31 0.0211(13) 0.0226(13) 0.0349(15) 0.0008(11) 0.0041(11) -0.0049(11) C32 0.0299(14) 0.0274(13) 0.0259(13) -0.0050(11) 0.0075(11) -0.0059(12) C33 0.0267(13) 0.0267(13) 0.0212(12) 0.0003(10) 0.0002(10) -0.0099(11) C34 0.0167(11) 0.0216(12) 0.0247(12) 0.0018(10) -0.0001(9) -0.0044(10) C35 0.0248(13) 0.0308(14) 0.0249(13) 0.0014(11) 0.0007(10) -0.0134(11) C36 0.0337(15) 0.0366(15) 0.0227(13) 0.0054(11) 0.0007(11) -0.0153(13) C37 0.0330(15) 0.0388(16) 0.0266(14) 0.0054(12) -0.0106(12) -0.0123(13) C38 0.0338(16) 0.0396(16) 0.0332(15) 0.0035(12) -0.0090(12) -0.0200(14) C39 0.0253(13) 0.0326(14) 0.0293(14) 0.0066(11) -0.0040(11) -0.0147(12) C40 0.0192(12) 0.0262(12) 0.0172(11) 0.0026(9) -0.0009(9) -0.0109(10) C41 0.0251(13) 0.0248(13) 0.0297(14) -0.0004(11) 0.0048(11) -0.0089(11) C42 0.0360(16) 0.0289(14) 0.0372(15) 0.0075(12) 0.0017(12) -0.0175(13) C43 0.0271(14) 0.0417(16) 0.0289(14) 0.0040(12) 0.0037(11) -0.0196(13) C44 0.0200(13) 0.0380(15) 0.0255(13) -0.0027(11) 0.0031(10) -0.0115(11) C45 0.0214(12) 0.0250(13) 0.0250(13) 0.0025(10) -0.0011(10) -0.0076(11) O1 0.0252(10) 0.0338(10) 0.0212(9) 0.0002(7) 0.0027(7) -0.0096(8) O2 0.0296(10) 0.0267(9) 0.0226(9) 0.0030(7) 0.0008(8) -0.0106(8) O3 0.0349(11) 0.0307(11) 0.0284(10) 0.0052(8) -0.0005(8) -0.0074(9) O4 0.0280(11) 0.0341(11) 0.0487(13) 0.0008(9) -0.0014(9) -0.0139(9) O5 0.0379(12) 0.0344(11) 0.0374(11) 0.0028(9) -0.0030(9) -0.0181(10) P1 0.0185(3) 0.0210(3) 0.0190(3) 0.0028(2) 0.0008(2) -0.0089(3) P2 0.0161(3) 0.0189(3) 0.0189(3) 0.0023(2) 0.0006(2) -0.0062(2) Cu1 0.0198(2) 0.0215(2) 0.0196(2) 0.00231(14) 0.00189(14) -0.00924(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.257(3) . ? C1 O2 1.261(3) . ? C1 C2 1.552(4) . ? C1 Cu1 2.508(3) . ? C2 O3 1.426(3) . ? C2 C4 1.519(4) . ? C2 C3 1.526(4) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 O3 1.412(4) . ? C5 C6 1.515(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O4 1.414(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O4 1.416(4) . ? C7 C8 1.510(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O5 1.416(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O5 1.410(4) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.389(4) . ? C10 C15 1.394(4) . ? C10 P1 1.832(3) . ? C11 C12 1.393(4) . ? C11 H11 0.9300 . ? C12 C13 1.377(4) . ? C12 H12 0.9300 . ? C13 C14 1.389(4) . ? C13 H13 0.9300 . ? C14 C15 1.388(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C21 1.393(4) . ? C16 C17 1.397(4) . ? C16 P1 1.834(3) . ? C17 C18 1.384(4) . ? C17 H17 0.9300 . ? C18 C19 1.394(4) . ? C18 H18 0.9300 . ? C19 C20 1.385(4) . ? C19 H19 0.9300 . ? C20 C21 1.386(4) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C27 1.392(4) . ? C22 C23 1.392(4) . ? C22 P1 1.827(3) . ? C23 C24 1.397(4) . ? C23 H23 0.9300 . ? C24 C25 1.383(4) . ? C24 H24 0.9300 . ? C25 C26 1.385(4) . ? C25 H25 0.9300 . ? C26 C27 1.390(4) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C33 1.388(4) . ? C28 C29 1.393(4) . ? C28 P2 1.828(3) . ? C29 C30 1.393(4) . ? C29 H29 0.9300 . ? C30 C31 1.381(4) . ? C30 H30 0.9300 . ? C31 C32 1.387(4) . ? C31 H31 0.9300 . ? C32 C33 1.389(4) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C39 1.389(4) . ? C34 C35 1.396(4) . ? C34 P2 1.830(3) . ? C35 C36 1.385(4) . ? C35 H35 0.9300 . ? C36 C37 1.381(5) . ? C36 H36 0.9300 . ? C37 C38 1.388(4) . ? C37 H37 0.9300 . ? C38 C39 1.391(4) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C45 1.390(4) . ? C40 C41 1.393(4) . ? C40 P2 1.827(2) . ? C41 C42 1.381(4) . ? C41 H41 0.9300 . ? C42 C43 1.389(5) . ? C42 H42 0.9300 . ? C43 C44 1.375(4) . ? C43 H43 0.9300 . ? C44 C45 1.392(4) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? O1 Cu1 2.1959(19) . ? O2 Cu1 2.2193(19) . ? P1 Cu1 2.2218(7) . ? P2 Cu1 2.2533(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 123.0(2) . . ? O1 C1 C2 118.2(2) . . ? O2 C1 C2 118.8(2) . . ? O1 C1 Cu1 61.10(13) . . ? O2 C1 Cu1 62.15(13) . . ? C2 C1 Cu1 175.93(18) . . ? O3 C2 C4 112.2(2) . . ? O3 C2 C3 103.2(2) . . ? C4 C2 C3 110.4(2) . . ? O3 C2 C1 110.6(2) . . ? C4 C2 C1 112.5(2) . . ? C3 C2 C1 107.4(2) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 C6 106.4(3) . . ? O3 C5 H5A 110.4 . . ? C6 C5 H5A 110.4 . . ? O3 C5 H5B 110.4 . . ? C6 C5 H5B 110.4 . . ? H5A C5 H5B 108.6 . . ? O4 C6 C5 110.4(3) . . ? O4 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? O4 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? O4 C7 C8 113.8(3) . . ? O4 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? O4 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? O5 C8 C7 109.3(2) . . ? O5 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 . . ? O5 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 . . ? H8A C8 H8B 108.3 . . ? O5 C9 H9A 109.5 . . ? O5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 119.3(2) . . ? C11 C10 P1 117.5(2) . . ? C15 C10 P1 123.2(2) . . ? C10 C11 C12 120.2(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 120.2(3) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 120.0(3) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.0(3) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C10 120.3(3) . . ? C14 C15 H15 119.9 . . ? C10 C15 H15 119.9 . . ? C21 C16 C17 118.6(2) . . ? C21 C16 P1 117.5(2) . . ? C17 C16 P1 123.9(2) . . ? C18 C17 C16 120.6(3) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 120.1(3) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 C18 119.7(3) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 120.0(3) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C16 121.0(3) . . ? C20 C21 H21 119.5 . . ? C16 C21 H21 119.5 . . ? C27 C22 C23 119.0(2) . . ? C27 C22 P1 117.3(2) . . ? C23 C22 P1 123.5(2) . . ? C22 C23 C24 120.4(3) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C25 C24 C23 119.9(3) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.1(3) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C26 C27 120.0(3) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C22 120.6(3) . . ? C26 C27 H27 119.7 . . ? C22 C27 H27 119.7 . . ? C33 C28 C29 119.1(2) . . ? C33 C28 P2 123.2(2) . . ? C29 C28 P2 117.5(2) . . ? C30 C29 C28 120.8(2) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C31 C30 C29 119.4(2) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C30 C31 C32 120.3(2) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C31 C32 C33 120.1(3) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C28 C33 C32 120.3(2) . . ? C28 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C39 C34 C35 119.0(2) . . ? C39 C34 P2 122.8(2) . . ? C35 C34 P2 118.2(2) . . ? C36 C35 C34 120.2(3) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C37 C36 C35 120.7(3) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C36 C37 C38 119.5(3) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C37 C38 C39 120.0(3) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C34 C39 C38 120.5(3) . . ? C34 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C45 C40 C41 119.3(2) . . ? C45 C40 P2 117.3(2) . . ? C41 C40 P2 123.4(2) . . ? C42 C41 C40 120.2(3) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C43 120.3(3) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C44 C43 C42 119.9(3) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 120.2(3) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C40 C45 C44 120.1(3) . . ? C40 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C1 O1 Cu1 88.84(15) . . ? C1 O2 Cu1 87.69(16) . . ? C5 O3 C2 114.7(2) . . ? C6 O4 C7 111.9(2) . . ? C9 O5 C8 111.3(2) . . ? C22 P1 C10 102.79(11) . . ? C22 P1 C16 104.71(12) . . ? C10 P1 C16 105.09(12) . . ? C22 P1 Cu1 115.92(8) . . ? C10 P1 Cu1 117.51(9) . . ? C16 P1 Cu1 109.56(8) . . ? C40 P2 C28 103.39(11) . . ? C40 P2 C34 104.15(12) . . ? C28 P2 C34 104.40(12) . . ? C40 P2 Cu1 114.25(9) . . ? C28 P2 Cu1 108.91(8) . . ? C34 P2 Cu1 120.10(9) . . ? O1 Cu1 O2 60.13(7) . . ? O1 Cu1 P1 113.11(6) . . ? O2 Cu1 P1 119.12(5) . . ? O1 Cu1 P2 100.77(6) . . ? O2 Cu1 P2 109.88(5) . . ? P1 Cu1 P2 129.50(3) . . ? O1 Cu1 C1 30.06(8) . . ? O2 Cu1 C1 30.15(8) . . ? P1 Cu1 C1 122.22(6) . . ? P2 Cu1 C1 106.02(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 O3 25.4(3) . . . . ? O2 C1 C2 O3 -156.2(2) . . . . ? Cu1 C1 C2 O3 -54(3) . . . . ? O1 C1 C2 C4 151.8(3) . . . . ? O2 C1 C2 C4 -29.8(4) . . . . ? Cu1 C1 C2 C4 72(3) . . . . ? O1 C1 C2 C3 -86.5(3) . . . . ? O2 C1 C2 C3 91.9(3) . . . . ? Cu1 C1 C2 C3 -166(3) . . . . ? O3 C5 C6 O4 170.2(2) . . . . ? O4 C7 C8 O5 -79.0(3) . . . . ? C15 C10 C11 C12 2.8(4) . . . . ? P1 C10 C11 C12 -176.4(2) . . . . ? C10 C11 C12 C13 0.1(4) . . . . ? C11 C12 C13 C14 -2.2(4) . . . . ? C12 C13 C14 C15 1.4(4) . . . . ? C13 C14 C15 C10 1.6(4) . . . . ? C11 C10 C15 C14 -3.6(4) . . . . ? P1 C10 C15 C14 175.6(2) . . . . ? C21 C16 C17 C18 -0.5(4) . . . . ? P1 C16 C17 C18 178.9(2) . . . . ? C16 C17 C18 C19 0.4(4) . . . . ? C17 C18 C19 C20 -0.3(4) . . . . ? C18 C19 C20 C21 0.2(4) . . . . ? C19 C20 C21 C16 -0.2(4) . . . . ? C17 C16 C21 C20 0.4(4) . . . . ? P1 C16 C21 C20 -179.0(2) . . . . ? C27 C22 C23 C24 0.4(4) . . . . ? P1 C22 C23 C24 -174.5(2) . . . . ? C22 C23 C24 C25 0.4(4) . . . . ? C23 C24 C25 C26 -1.0(4) . . . . ? C24 C25 C26 C27 0.8(5) . . . . ? C25 C26 C27 C22 0.1(4) . . . . ? C23 C22 C27 C26 -0.7(4) . . . . ? P1 C22 C27 C26 174.5(2) . . . . ? C33 C28 C29 C30 0.1(4) . . . . ? P2 C28 C29 C30 175.0(2) . . . . ? C28 C29 C30 C31 -1.1(4) . . . . ? C29 C30 C31 C32 1.3(4) . . . . ? C30 C31 C32 C33 -0.6(4) . . . . ? C29 C28 C33 C32 0.6(4) . . . . ? P2 C28 C33 C32 -173.9(2) . . . . ? C31 C32 C33 C28 -0.4(4) . . . . ? C39 C34 C35 C36 -0.3(4) . . . . ? P2 C34 C35 C36 179.2(2) . . . . ? C34 C35 C36 C37 -0.7(5) . . . . ? C35 C36 C37 C38 0.9(5) . . . . ? C36 C37 C38 C39 -0.2(5) . . . . ? C35 C34 C39 C38 1.1(4) . . . . ? P2 C34 C39 C38 -178.4(2) . . . . ? C37 C38 C39 C34 -0.8(5) . . . . ? C45 C40 C41 C42 0.2(4) . . . . ? P2 C40 C41 C42 -178.1(2) . . . . ? C40 C41 C42 C43 -1.1(4) . . . . ? C41 C42 C43 C44 0.8(5) . . . . ? C42 C43 C44 C45 0.4(4) . . . . ? C41 C40 C45 C44 0.9(4) . . . . ? P2 C40 C45 C44 179.4(2) . . . . ? C43 C44 C45 C40 -1.2(4) . . . . ? O2 C1 O1 Cu1 6.3(3) . . . . ? C2 C1 O1 Cu1 -175.4(2) . . . . ? O1 C1 O2 Cu1 -6.2(3) . . . . ? C2 C1 O2 Cu1 175.5(2) . . . . ? C6 C5 O3 C2 -156.8(2) . . . . ? C4 C2 O3 C5 -62.4(3) . . . . ? C3 C2 O3 C5 178.7(2) . . . . ? C1 C2 O3 C5 64.1(3) . . . . ? C5 C6 O4 C7 -175.7(2) . . . . ? C8 C7 O4 C6 -100.2(3) . . . . ? C7 C8 O5 C9 -171.0(3) . . . . ? C27 C22 P1 C10 72.1(2) . . . . ? C23 C22 P1 C10 -112.9(2) . . . . ? C27 C22 P1 C16 -178.3(2) . . . . ? C23 C22 P1 C16 -3.3(3) . . . . ? C27 C22 P1 Cu1 -57.5(2) . . . . ? C23 C22 P1 Cu1 117.5(2) . . . . ? C11 C10 P1 C22 -145.1(2) . . . . ? C15 C10 P1 C22 35.7(2) . . . . ? C11 C10 P1 C16 105.6(2) . . . . ? C15 C10 P1 C16 -73.6(2) . . . . ? C11 C10 P1 Cu1 -16.5(2) . . . . ? C15 C10 P1 Cu1 164.31(19) . . . . ? C21 C16 P1 C22 108.9(2) . . . . ? C17 C16 P1 C22 -70.4(3) . . . . ? C21 C16 P1 C10 -143.1(2) . . . . ? C17 C16 P1 C10 37.5(3) . . . . ? C21 C16 P1 Cu1 -16.0(2) . . . . ? C17 C16 P1 Cu1 164.6(2) . . . . ? C45 C40 P2 C28 -155.0(2) . . . . ? C41 C40 P2 C28 23.4(2) . . . . ? C45 C40 P2 C34 96.2(2) . . . . ? C41 C40 P2 C34 -85.5(2) . . . . ? C45 C40 P2 Cu1 -36.8(2) . . . . ? C41 C40 P2 Cu1 141.6(2) . . . . ? C33 C28 P2 C40 -118.7(2) . . . . ? C29 C28 P2 C40 66.6(2) . . . . ? C33 C28 P2 C34 -10.0(2) . . . . ? C29 C28 P2 C34 175.3(2) . . . . ? C33 C28 P2 Cu1 119.4(2) . . . . ? C29 C28 P2 Cu1 -55.2(2) . . . . ? C39 C34 P2 C40 14.7(3) . . . . ? C35 C34 P2 C40 -164.7(2) . . . . ? C39 C34 P2 C28 -93.4(2) . . . . ? C35 C34 P2 C28 87.1(2) . . . . ? C39 C34 P2 Cu1 144.2(2) . . . . ? C35 C34 P2 Cu1 -35.3(2) . . . . ? C1 O1 Cu1 O2 -3.43(14) . . . . ? C1 O1 Cu1 P1 -114.84(14) . . . . ? C1 O1 Cu1 P2 103.43(14) . . . . ? C1 O2 Cu1 O1 3.42(14) . . . . ? C1 O2 Cu1 P1 104.85(14) . . . . ? C1 O2 Cu1 P2 -87.80(15) . . . . ? C22 P1 Cu1 O1 -172.44(11) . . . . ? C10 P1 Cu1 O1 65.51(11) . . . . ? C16 P1 Cu1 O1 -54.26(11) . . . . ? C22 P1 Cu1 O2 120.03(11) . . . . ? C10 P1 Cu1 O2 -2.02(11) . . . . ? C16 P1 Cu1 O2 -121.79(10) . . . . ? C22 P1 Cu1 P2 -44.49(10) . . . . ? C10 P1 Cu1 P2 -166.53(9) . . . . ? C16 P1 Cu1 P2 73.69(9) . . . . ? C22 P1 Cu1 C1 155.05(12) . . . . ? C10 P1 Cu1 C1 33.01(12) . . . . ? C16 P1 Cu1 C1 -86.77(12) . . . . ? C40 P2 Cu1 O1 -54.39(10) . . . . ? C28 P2 Cu1 O1 60.62(10) . . . . ? C34 P2 Cu1 O1 -179.22(11) . . . . ? C40 P2 Cu1 O2 7.55(10) . . . . ? C28 P2 Cu1 O2 122.56(10) . . . . ? C34 P2 Cu1 O2 -117.28(11) . . . . ? C40 P2 Cu1 P1 173.19(9) . . . . ? C28 P2 Cu1 P1 -71.80(9) . . . . ? C34 P2 Cu1 P1 48.36(10) . . . . ? C40 P2 Cu1 C1 -23.93(11) . . . . ? C28 P2 Cu1 C1 91.08(11) . . . . ? C34 P2 Cu1 C1 -148.76(11) . . . . ? O2 C1 Cu1 O1 -174.1(2) . . . . ? C2 C1 Cu1 O1 82(3) . . . . ? O1 C1 Cu1 O2 174.1(2) . . . . ? C2 C1 Cu1 O2 -104(3) . . . . ? O1 C1 Cu1 P1 80.63(15) . . . . ? O2 C1 Cu1 P1 -93.44(15) . . . . ? C2 C1 Cu1 P1 162(3) . . . . ? O1 C1 Cu1 P2 -83.80(15) . . . . ? O2 C1 Cu1 P2 102.13(14) . . . . ? C2 C1 Cu1 P2 -2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 66.98 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.070 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.094 _database_code_depnum_ccdc_archive 'CCDC 932855' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl3 #TrackingRef 'ad-peg.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H47 Cu O6 P2' _chemical_formula_sum 'C45 H47 Cu O6 P2' _chemical_formula_weight 809.31 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.9464(8) _cell_length_b 10.6978(3) _cell_length_c 23.2985(11) _cell_angle_alpha 90.00 _cell_angle_beta 91.701(4) _cell_angle_gamma 90.00 _cell_volume 3972.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 104(1) _cell_measurement_reflns_used 7528 _cell_measurement_theta_min 2.8785 _cell_measurement_theta_max 28.3550 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 0.679 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8762 _exptl_absorpt_correction_T_max 0.9352 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 104(1) _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 'oxford gemini s' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time 1 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19549 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7368 _reflns_number_gt 6034 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+0.7732P] 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 7368 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0863 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.51313(13) 0.02561(17) 0.74049(9) 0.0171(4) Uani 1 1 d . . . C2 C 0.56647(15) -0.04171(19) 0.78593(9) 0.0216(5) Uani 1 1 d . . . H2A H 0.5530 -0.1320 0.7840 0.026 Uiso 1 1 calc R . . H2B H 0.6262 -0.0322 0.7762 0.026 Uiso 1 1 calc R . . C3 C 0.59115(15) 0.12114(19) 0.85283(9) 0.0248(5) Uani 1 1 d . . . H3A H 0.5529 0.1848 0.8357 0.030 Uiso 1 1 calc R . . H3B H 0.6460 0.1281 0.8342 0.030 Uiso 1 1 calc R . . C4 C 0.60224(15) 0.1436(2) 0.91616(10) 0.0252(5) Uani 1 1 d . . . H4A H 0.6347 0.0741 0.9339 0.030 Uiso 1 1 calc R . . H4B H 0.6340 0.2220 0.9229 0.030 Uiso 1 1 calc R . . C5 C 0.53192(16) 0.1604(2) 1.00277(9) 0.0268(5) Uani 1 1 d . . . H5A H 0.5699 0.2304 1.0134 0.032 Uiso 1 1 calc R . . H5B H 0.5569 0.0821 1.0182 0.032 Uiso 1 1 calc R . . C6 C 0.44776(16) 0.18121(19) 1.02815(10) 0.0272(5) Uani 1 1 d . . . H6A H 0.4039 0.1375 1.0049 0.033 Uiso 1 1 calc R . . H6B H 0.4476 0.1471 1.0677 0.033 Uiso 1 1 calc R . . C7 C 0.35293(16) 0.3381(2) 1.05519(11) 0.0294(5) Uani 1 1 d . . . H7A H 0.3508 0.2949 1.0927 0.035 Uiso 1 1 calc R . . H7B H 0.3060 0.3067 1.0304 0.035 Uiso 1 1 calc R . . C8 C 0.34387(16) 0.4777(2) 1.06378(10) 0.0301(6) Uani 1 1 d . . . H8A H 0.3668 0.5212 1.0302 0.036 Uiso 1 1 calc R . . H8B H 0.2834 0.4983 1.0651 0.036 Uiso 1 1 calc R . . C9 C 0.47298(16) 0.5332(2) 1.11027(11) 0.0353(6) Uani 1 1 d . . . H9A H 0.4972 0.5644 1.1467 0.053 Uiso 1 1 calc R . . H9B H 0.4865 0.5910 1.0792 0.053 Uiso 1 1 calc R . . H9C H 0.4962 0.4505 1.1021 0.053 Uiso 1 1 calc R . . C10 C 0.64383(13) 0.28276(17) 0.69704(9) 0.0182(5) Uani 1 1 d . . . C11 C 0.70005(15) 0.19046(19) 0.68072(10) 0.0241(5) Uani 1 1 d . . . H11 H 0.6886 0.1429 0.6469 0.029 Uiso 1 1 calc R . . C12 C 0.77229(15) 0.1675(2) 0.71332(10) 0.0272(5) Uani 1 1 d . . . H12 H 0.8112 0.1064 0.7012 0.033 Uiso 1 1 calc R . . C13 C 0.78803(15) 0.2335(2) 0.76371(10) 0.0258(5) Uani 1 1 d . . . H13 H 0.8372 0.2168 0.7865 0.031 Uiso 1 1 calc R . . C14 C 0.73205(15) 0.3235(2) 0.78063(10) 0.0256(5) Uani 1 1 d . . . H14 H 0.7427 0.3685 0.8152 0.031 Uiso 1 1 calc R . . C15 C 0.66033(14) 0.34893(18) 0.74754(9) 0.0217(5) Uani 1 1 d . . . H15 H 0.6224 0.4117 0.7594 0.026 Uiso 1 1 calc R . . C16 C 0.50575(13) 0.45205(18) 0.68052(9) 0.0177(4) Uani 1 1 d . . . C17 C 0.45135(14) 0.44454(19) 0.72612(9) 0.0229(5) Uani 1 1 d . . . H17 H 0.4380 0.3652 0.7418 0.027 Uiso 1 1 calc R . . C18 C 0.41638(15) 0.5521(2) 0.74889(10) 0.0268(5) Uani 1 1 d . . . H18 H 0.3798 0.5463 0.7802 0.032 Uiso 1 1 calc R . . C19 C 0.43496(14) 0.66736(19) 0.72580(10) 0.0233(5) Uani 1 1 d . . . H19 H 0.4110 0.7408 0.7413 0.028 Uiso 1 1 calc R . . C20 C 0.48824(15) 0.67650(19) 0.68029(10) 0.0237(5) Uani 1 1 d . . . H20 H 0.5005 0.7561 0.6645 0.028 Uiso 1 1 calc R . . C21 C 0.52389(14) 0.56948(18) 0.65749(9) 0.0209(5) Uani 1 1 d . . . H21 H 0.5606 0.5761 0.6263 0.025 Uiso 1 1 calc R . . C22 C 0.58581(14) 0.34347(17) 0.58230(9) 0.0186(5) Uani 1 1 d . . . C23 C 0.66324(15) 0.39825(19) 0.57214(10) 0.0239(5) Uani 1 1 d . . . H23 H 0.7001 0.4197 0.6034 0.029 Uiso 1 1 calc R . . C24 C 0.68638(16) 0.4213(2) 0.51611(10) 0.0309(6) Uani 1 1 d . . . H24 H 0.7389 0.4598 0.5094 0.037 Uiso 1 1 calc R . . C25 C 0.63426(18) 0.3893(2) 0.47013(10) 0.0334(6) Uani 1 1 d . . . H25 H 0.6510 0.4046 0.4320 0.040 Uiso 1 1 calc R . . C26 C 0.55794(18) 0.3352(2) 0.47992(10) 0.0331(6) Uani 1 1 d . . . H26 H 0.5217 0.3133 0.4484 0.040 Uiso 1 1 calc R . . C27 C 0.53342(15) 0.31232(19) 0.53569(9) 0.0252(5) Uani 1 1 d . . . H27 H 0.4804 0.2751 0.5420 0.030 Uiso 1 1 calc R . . C28 C 0.25656(14) 0.24077(18) 0.62465(8) 0.0173(4) Uani 1 1 d . . . C29 C 0.28613(15) 0.36340(18) 0.63203(9) 0.0217(5) Uani 1 1 d . . . H29 H 0.3445 0.3801 0.6304 0.026 Uiso 1 1 calc R . . C30 C 0.23036(15) 0.46081(19) 0.64166(10) 0.0247(5) Uani 1 1 d . . . H30 H 0.2509 0.5437 0.6462 0.030 Uiso 1 1 calc R . . C31 C 0.14565(15) 0.43798(19) 0.64465(9) 0.0230(5) Uani 1 1 d . . . H31 H 0.1079 0.5047 0.6514 0.028 Uiso 1 1 calc R . . C32 C 0.11575(15) 0.3168(2) 0.63770(9) 0.0235(5) Uani 1 1 d . . . H32 H 0.0574 0.3005 0.6399 0.028 Uiso 1 1 calc R . . C33 C 0.17114(14) 0.21923(19) 0.62751(9) 0.0196(5) Uani 1 1 d . . . H33 H 0.1501 0.1368 0.6225 0.024 Uiso 1 1 calc R . . C34 C 0.33936(13) 0.11328(18) 0.53395(9) 0.0171(4) Uani 1 1 d . . . C35 C 0.31056(14) 0.21139(19) 0.49890(9) 0.0204(5) Uani 1 1 d . . . H35 H 0.2797 0.2780 0.5151 0.025 Uiso 1 1 calc R . . C36 C 0.32674(14) 0.21212(19) 0.44070(9) 0.0225(5) Uani 1 1 d . . . H36 H 0.3072 0.2796 0.4174 0.027 Uiso 1 1 calc R . . C37 C 0.37106(14) 0.1155(2) 0.41619(9) 0.0229(5) Uani 1 1 d . . . H37 H 0.3821 0.1166 0.3764 0.028 Uiso 1 1 calc R . . C38 C 0.39905(14) 0.0173(2) 0.45053(9) 0.0243(5) Uani 1 1 d . . . H38 H 0.4290 -0.0498 0.4340 0.029 Uiso 1 1 calc R . . C39 C 0.38373(14) 0.01597(19) 0.50860(9) 0.0209(5) Uani 1 1 d . . . H39 H 0.4036 -0.0518 0.5316 0.025 Uiso 1 1 calc R . . C40 C 0.27716(13) -0.02369(18) 0.63200(9) 0.0181(4) Uani 1 1 d . . . C41 C 0.21935(15) -0.08444(19) 0.59545(9) 0.0240(5) Uani 1 1 d . . . H41 H 0.2126 -0.0583 0.5566 0.029 Uiso 1 1 calc R . . C42 C 0.17156(15) -0.18316(19) 0.61568(10) 0.0255(5) Uani 1 1 d . . . H42 H 0.1320 -0.2238 0.5908 0.031 Uiso 1 1 calc R . . C43 C 0.18174(14) -0.22201(18) 0.67203(10) 0.0242(5) Uani 1 1 d . . . H43 H 0.1483 -0.2881 0.6861 0.029 Uiso 1 1 calc R . . C44 C 0.24091(15) -0.16444(18) 0.70800(10) 0.0236(5) Uani 1 1 d . . . H44 H 0.2489 -0.1929 0.7464 0.028 Uiso 1 1 calc R . . C45 C 0.28851(14) -0.06563(18) 0.68837(9) 0.0201(5) Uani 1 1 d . . . H45 H 0.3288 -0.0266 0.7133 0.024 Uiso 1 1 calc R . . O1 O 0.52461(10) -0.00717(12) 0.68934(6) 0.0213(3) Uani 1 1 d . . . O2 O 0.46251(9) 0.10991(13) 0.75393(6) 0.0211(3) Uani 1 1 d . . . O3 O 0.55698(10) -0.00082(13) 0.84332(6) 0.0218(3) Uani 1 1 d . . . O4 O 0.52281(10) 0.15240(13) 0.94184(6) 0.0254(4) Uani 1 1 d . . . O5 O 0.43059(11) 0.31184(13) 1.02916(6) 0.0283(4) Uani 1 1 d . . . O6 O 0.38478(11) 0.52411(15) 1.11431(7) 0.0336(4) Uani 1 1 d . . . P1 P 0.54816(4) 0.30609(5) 0.65337(2) 0.01634(13) Uani 1 1 d . . . P2 P 0.33312(4) 0.11783(5) 0.61204(2) 0.01582(13) Uani 1 1 d . . . Cu1 Cu 0.455332(17) 0.14771(2) 0.656673(10) 0.01729(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0165(11) 0.0136(10) 0.0214(11) 0.0020(8) 0.0035(9) -0.0040(8) C2 0.0262(13) 0.0184(11) 0.0205(11) 0.0014(8) 0.0034(10) 0.0039(9) C3 0.0269(14) 0.0201(11) 0.0276(12) 0.0024(9) 0.0044(10) -0.0049(10) C4 0.0252(13) 0.0226(11) 0.0277(12) -0.0016(9) 0.0003(10) -0.0031(10) C5 0.0346(15) 0.0244(12) 0.0213(12) -0.0037(9) -0.0034(11) 0.0019(10) C6 0.0378(15) 0.0202(11) 0.0236(12) 0.0010(9) 0.0020(11) -0.0009(10) C7 0.0274(14) 0.0289(13) 0.0323(13) 0.0006(10) 0.0061(11) -0.0036(10) C8 0.0245(14) 0.0315(13) 0.0345(14) -0.0027(10) 0.0019(11) 0.0027(10) C9 0.0321(15) 0.0322(13) 0.0412(15) -0.0060(11) -0.0034(12) 0.0010(11) C10 0.0179(12) 0.0137(10) 0.0232(11) 0.0029(8) 0.0030(9) -0.0041(8) C11 0.0264(14) 0.0180(11) 0.0280(12) -0.0019(9) 0.0000(10) 0.0015(9) C12 0.0241(13) 0.0218(12) 0.0359(14) 0.0044(10) 0.0048(11) 0.0031(10) C13 0.0191(13) 0.0272(12) 0.0308(13) 0.0085(10) -0.0029(10) -0.0027(10) C14 0.0260(14) 0.0251(12) 0.0254(12) 0.0004(9) -0.0030(10) -0.0049(10) C15 0.0220(12) 0.0162(10) 0.0271(12) 0.0000(9) 0.0016(10) -0.0016(9) C16 0.0163(11) 0.0175(10) 0.0192(11) 0.0000(8) -0.0027(9) 0.0003(9) C17 0.0239(13) 0.0190(11) 0.0260(12) -0.0003(9) 0.0047(10) -0.0021(9) C18 0.0249(14) 0.0264(12) 0.0294(13) -0.0068(9) 0.0078(10) -0.0020(10) C19 0.0216(13) 0.0180(11) 0.0302(12) -0.0081(9) -0.0016(10) 0.0052(9) C20 0.0261(13) 0.0156(11) 0.0292(12) 0.0025(9) -0.0037(10) 0.0010(9) C21 0.0214(12) 0.0180(11) 0.0234(11) 0.0011(8) 0.0019(10) -0.0012(9) C22 0.0227(12) 0.0118(10) 0.0214(11) 0.0020(8) 0.0039(9) 0.0020(9) C23 0.0225(13) 0.0215(11) 0.0280(12) 0.0020(9) 0.0034(10) 0.0004(9) C24 0.0281(14) 0.0263(12) 0.0390(14) 0.0075(10) 0.0113(12) -0.0003(10) C25 0.0483(18) 0.0286(13) 0.0241(13) 0.0082(10) 0.0137(12) 0.0023(12) C26 0.0484(18) 0.0305(13) 0.0202(12) 0.0050(10) -0.0002(12) -0.0057(12) C27 0.0266(14) 0.0233(11) 0.0258(12) 0.0047(9) 0.0012(10) -0.0049(10) C28 0.0227(12) 0.0176(10) 0.0115(10) -0.0003(8) 0.0024(9) -0.0012(9) C29 0.0204(12) 0.0175(11) 0.0275(12) -0.0028(9) 0.0063(10) -0.0028(9) C30 0.0274(14) 0.0154(11) 0.0318(13) -0.0022(9) 0.0065(11) 0.0010(9) C31 0.0264(13) 0.0211(11) 0.0217(11) -0.0015(9) 0.0058(10) 0.0070(10) C32 0.0184(12) 0.0294(12) 0.0227(12) -0.0002(9) 0.0025(10) -0.0005(10) C33 0.0217(12) 0.0167(11) 0.0206(11) -0.0002(8) 0.0029(9) -0.0008(9) C34 0.0159(11) 0.0167(10) 0.0188(11) -0.0028(8) 0.0016(9) -0.0036(8) C35 0.0219(12) 0.0167(10) 0.0229(11) -0.0011(8) 0.0035(10) 0.0010(9) C36 0.0263(13) 0.0211(11) 0.0201(11) 0.0037(9) 0.0005(10) -0.0012(9) C37 0.0215(12) 0.0301(12) 0.0174(11) -0.0039(9) 0.0039(9) -0.0047(10) C38 0.0208(13) 0.0252(12) 0.0270(12) -0.0086(9) 0.0047(10) 0.0027(10) C39 0.0206(12) 0.0184(11) 0.0235(12) -0.0008(9) -0.0001(10) 0.0018(9) C40 0.0161(11) 0.0159(10) 0.0225(11) -0.0007(8) 0.0039(9) 0.0004(8) C41 0.0277(13) 0.0189(11) 0.0252(12) -0.0008(9) -0.0004(10) -0.0007(10) C42 0.0247(13) 0.0165(11) 0.0354(13) -0.0062(9) 0.0043(11) -0.0032(9) C43 0.0245(13) 0.0118(10) 0.0369(13) -0.0009(9) 0.0128(11) -0.0001(9) C44 0.0276(13) 0.0185(11) 0.0253(12) 0.0048(9) 0.0104(10) 0.0033(9) C45 0.0196(12) 0.0170(10) 0.0239(11) -0.0001(8) 0.0019(9) 0.0010(9) O1 0.0276(9) 0.0170(7) 0.0193(8) -0.0005(6) 0.0024(7) 0.0016(6) O2 0.0231(9) 0.0194(7) 0.0212(8) 0.0010(6) 0.0046(7) 0.0053(6) O3 0.0297(9) 0.0183(7) 0.0177(8) 0.0009(6) 0.0036(7) -0.0029(6) O4 0.0263(9) 0.0294(8) 0.0205(8) -0.0018(6) -0.0010(7) 0.0009(7) O5 0.0349(10) 0.0193(8) 0.0314(9) -0.0008(6) 0.0112(8) 0.0007(7) O6 0.0332(11) 0.0353(9) 0.0325(9) -0.0089(7) 0.0063(8) -0.0019(8) P1 0.0175(3) 0.0128(3) 0.0188(3) 0.0004(2) 0.0024(2) -0.0011(2) P2 0.0178(3) 0.0132(3) 0.0166(3) 0.00036(19) 0.0020(2) -0.0009(2) Cu1 0.01869(15) 0.01398(14) 0.01923(14) 0.00135(9) 0.00090(11) -0.00138(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.256(2) . ? C1 O1 1.261(2) . ? C1 C2 1.520(3) . ? C1 Cu1 2.502(2) . ? C2 O3 1.419(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O3 1.429(2) . ? C3 C4 1.500(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O4 1.420(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 O4 1.425(3) . ? C5 C6 1.499(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O5 1.424(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O5 1.423(3) . ? C7 C8 1.515(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O6 1.419(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O6 1.416(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.392(3) . ? C10 C11 1.394(3) . ? C10 P1 1.825(2) . ? C11 C12 1.383(3) . ? C11 H11 0.9500 . ? C12 C13 1.386(3) . ? C12 H12 0.9500 . ? C13 C14 1.379(3) . ? C13 H13 0.9500 . ? C14 C15 1.387(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.394(3) . ? C16 C21 1.400(3) . ? C16 P1 1.822(2) . ? C17 C18 1.391(3) . ? C17 H17 0.9500 . ? C18 C19 1.381(3) . ? C18 H18 0.9500 . ? C19 C20 1.382(3) . ? C19 H19 0.9500 . ? C20 C21 1.391(3) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.391(3) . ? C22 C23 1.393(3) . ? C22 P1 1.822(2) . ? C23 C24 1.389(3) . ? C23 H23 0.9500 . ? C24 C25 1.379(3) . ? C24 H24 0.9500 . ? C25 C26 1.373(4) . ? C25 H25 0.9500 . ? C26 C27 1.390(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.385(3) . ? C28 C29 1.403(3) . ? C28 P2 1.824(2) . ? C29 C30 1.392(3) . ? C29 H29 0.9500 . ? C30 C31 1.376(3) . ? C30 H30 0.9500 . ? C31 C32 1.389(3) . ? C31 H31 0.9500 . ? C32 C33 1.392(3) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.399(3) . ? C34 C39 1.399(3) . ? C34 P2 1.826(2) . ? C35 C36 1.388(3) . ? C35 H35 0.9500 . ? C36 C37 1.385(3) . ? C36 H36 0.9500 . ? C37 C38 1.387(3) . ? C37 H37 0.9500 . ? C38 C39 1.382(3) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C45 1.395(3) . ? C40 C41 1.397(3) . ? C40 P2 1.825(2) . ? C41 C42 1.393(3) . ? C41 H41 0.9500 . ? C42 C43 1.382(3) . ? C42 H42 0.9500 . ? C43 C44 1.388(3) . ? C43 H43 0.9500 . ? C44 C45 1.387(3) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? O1 Cu1 2.1202(14) . ? O2 Cu1 2.3013(14) . ? P1 Cu1 2.2528(6) . ? P2 Cu1 2.2048(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 O2 C1 O1 123.22(19) . . ? O2 C1 C2 121.13(18) . . ? O1 C1 C2 115.64(18) . . ? O2 C1 Cu1 66.13(11) . . ? O1 C1 Cu1 57.87(10) . . ? C2 C1 Cu1 167.57(15) . . ? O3 C2 C1 115.92(17) . . ? O3 C2 H2A 108.3 . . ? C1 C2 H2A 108.3 . . ? O3 C2 H2B 108.3 . . ? C1 C2 H2B 108.3 . . ? H2A C2 H2B 107.4 . . ? O3 C3 C4 109.40(17) . . ? O3 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? O3 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? O4 C4 C3 110.15(19) . . ? O4 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? O4 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? O4 C5 C6 109.63(19) . . ? O4 C5 H5A 109.7 . . ? C6 C5 H5A 109.7 . . ? O4 C5 H5B 109.7 . . ? C6 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? O5 C6 C5 109.07(19) . . ? O5 C6 H6A 109.9 . . ? C5 C6 H6A 109.9 . . ? O5 C6 H6B 109.9 . . ? C5 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? O5 C7 C8 109.77(19) . . ? O5 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? O5 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? O6 C8 C7 114.28(19) . . ? O6 C8 H8A 108.7 . . ? C7 C8 H8A 108.7 . . ? O6 C8 H8B 108.7 . . ? C7 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? O6 C9 H9A 109.5 . . ? O6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 118.9(2) . . ? C15 C10 P1 122.38(16) . . ? C11 C10 P1 118.58(16) . . ? C12 C11 C10 120.5(2) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 120.1(2) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 119.7(2) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C15 120.5(2) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C14 C15 C10 120.2(2) . . ? C14 C15 H15 119.9 . . ? C10 C15 H15 119.9 . . ? C17 C16 C21 118.97(19) . . ? C17 C16 P1 117.45(15) . . ? C21 C16 P1 123.57(17) . . ? C18 C17 C16 120.6(2) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C19 C18 C17 119.8(2) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 120.40(19) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C19 C20 C21 120.17(19) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C16 120.1(2) . . ? C20 C21 H21 120.0 . . ? C16 C21 H21 120.0 . . ? C27 C22 C23 118.9(2) . . ? C27 C22 P1 116.77(17) . . ? C23 C22 P1 124.35(17) . . ? C24 C23 C22 119.7(2) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C25 C24 C23 121.0(2) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C26 C25 C24 119.5(2) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C25 C26 C27 120.3(2) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C26 C27 C22 120.6(2) . . ? C26 C27 H27 119.7 . . ? C22 C27 H27 119.7 . . ? C33 C28 C29 118.50(19) . . ? C33 C28 P2 123.48(15) . . ? C29 C28 P2 118.02(17) . . ? C30 C29 C28 120.4(2) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C31 C30 C29 120.5(2) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C30 C31 C32 119.6(2) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C31 C32 C33 120.2(2) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C28 C33 C32 120.87(19) . . ? C28 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C35 C34 C39 118.25(19) . . ? C35 C34 P2 122.35(16) . . ? C39 C34 P2 118.92(16) . . ? C36 C35 C34 120.48(19) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C37 C36 C35 120.7(2) . . ? C37 C36 H36 119.6 . . ? C35 C36 H36 119.6 . . ? C36 C37 C38 119.1(2) . . ? C36 C37 H37 120.4 . . ? C38 C37 H37 120.4 . . ? C39 C38 C37 120.6(2) . . ? C39 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? C38 C39 C34 120.78(19) . . ? C38 C39 H39 119.6 . . ? C34 C39 H39 119.6 . . ? C45 C40 C41 119.30(19) . . ? C45 C40 P2 117.15(15) . . ? C41 C40 P2 123.34(16) . . ? C42 C41 C40 120.3(2) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C43 C42 C41 120.0(2) . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C42 C43 C44 119.9(2) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C45 C44 C43 120.5(2) . . ? C45 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? C44 C45 C40 119.9(2) . . ? C44 C45 H45 120.0 . . ? C40 C45 H45 120.0 . . ? C1 O1 Cu1 91.90(12) . . ? C1 O2 Cu1 83.92(12) . . ? C2 O3 C3 112.13(16) . . ? C4 O4 C5 110.98(17) . . ? C7 O5 C6 111.75(17) . . ? C9 O6 C8 113.72(18) . . ? C22 P1 C16 105.25(9) . . ? C22 P1 C10 104.12(10) . . ? C16 P1 C10 103.67(9) . . ? C22 P1 Cu1 115.50(7) . . ? C16 P1 Cu1 112.43(7) . . ? C10 P1 Cu1 114.66(6) . . ? C28 P2 C40 102.85(10) . . ? C28 P2 C34 103.67(9) . . ? C40 P2 C34 105.87(9) . . ? C28 P2 Cu1 113.95(7) . . ? C40 P2 Cu1 115.60(7) . . ? C34 P2 Cu1 113.60(7) . . ? O1 Cu1 P2 119.99(4) . . ? O1 Cu1 P1 105.31(4) . . ? P2 Cu1 P1 131.72(2) . . ? O1 Cu1 O2 59.93(5) . . ? P2 Cu1 O2 117.16(4) . . ? P1 Cu1 O2 98.76(4) . . ? O1 Cu1 C1 30.23(6) . . ? P2 Cu1 C1 126.32(5) . . ? P1 Cu1 C1 101.07(5) . . ? O2 Cu1 C1 29.95(6) . . ? 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 O2 C1 C2 O3 -1.7(3) . . . . ? O1 C1 C2 O3 176.90(17) . . . . ? Cu1 C1 C2 O3 121.2(6) . . . . ? O3 C3 C4 O4 -68.2(2) . . . . ? O4 C5 C6 O5 -86.9(2) . . . . ? O5 C7 C8 O6 -83.2(2) . . . . ? C15 C10 C11 C12 -1.9(3) . . . . ? P1 C10 C11 C12 -178.41(17) . . . . ? C10 C11 C12 C13 2.2(3) . . . . ? C11 C12 C13 C14 -1.1(3) . . . . ? C12 C13 C14 C15 -0.3(3) . . . . ? C13 C14 C15 C10 0.6(3) . . . . ? C11 C10 C15 C14 0.5(3) . . . . ? P1 C10 C15 C14 176.90(16) . . . . ? C21 C16 C17 C18 -0.8(3) . . . . ? P1 C16 C17 C18 -179.78(17) . . . . ? C16 C17 C18 C19 0.7(3) . . . . ? C17 C18 C19 C20 -0.2(3) . . . . ? C18 C19 C20 C21 -0.2(3) . . . . ? C19 C20 C21 C16 0.1(3) . . . . ? C17 C16 C21 C20 0.4(3) . . . . ? P1 C16 C21 C20 179.31(17) . . . . ? C27 C22 C23 C24 0.4(3) . . . . ? P1 C22 C23 C24 179.13(16) . . . . ? C22 C23 C24 C25 -0.9(3) . . . . ? C23 C24 C25 C26 0.8(4) . . . . ? C24 C25 C26 C27 -0.3(4) . . . . ? C25 C26 C27 C22 -0.2(4) . . . . ? C23 C22 C27 C26 0.1(3) . . . . ? P1 C22 C27 C26 -178.71(17) . . . . ? C33 C28 C29 C30 -0.4(3) . . . . ? P2 C28 C29 C30 179.87(16) . . . . ? C28 C29 C30 C31 0.7(3) . . . . ? C29 C30 C31 C32 -0.3(3) . . . . ? C30 C31 C32 C33 -0.3(3) . . . . ? C29 C28 C33 C32 -0.3(3) . . . . ? P2 C28 C33 C32 179.51(15) . . . . ? C31 C32 C33 C28 0.6(3) . . . . ? C39 C34 C35 C36 -0.8(3) . . . . ? P2 C34 C35 C36 171.11(17) . . . . ? C34 C35 C36 C37 0.5(3) . . . . ? C35 C36 C37 C38 0.2(3) . . . . ? C36 C37 C38 C39 -0.6(3) . . . . ? C37 C38 C39 C34 0.3(3) . . . . ? C35 C34 C39 C38 0.4(3) . . . . ? P2 C34 C39 C38 -171.79(17) . . . . ? C45 C40 C41 C42 2.1(3) . . . . ? P2 C40 C41 C42 -172.33(17) . . . . ? C40 C41 C42 C43 -0.5(3) . . . . ? C41 C42 C43 C44 -1.5(3) . . . . ? C42 C43 C44 C45 1.8(3) . . . . ? C43 C44 C45 C40 -0.2(3) . . . . ? C41 C40 C45 C44 -1.8(3) . . . . ? P2 C40 C45 C44 173.01(16) . . . . ? O2 C1 O1 Cu1 10.7(2) . . . . ? C2 C1 O1 Cu1 -167.88(16) . . . . ? O1 C1 O2 Cu1 -9.92(19) . . . . ? C2 C1 O2 Cu1 168.61(18) . . . . ? C1 C2 O3 C3 -69.9(2) . . . . ? C4 C3 O3 C2 -163.59(18) . . . . ? C3 C4 O4 C5 173.81(16) . . . . ? C6 C5 O4 C4 174.92(17) . . . . ? C8 C7 O5 C6 171.13(18) . . . . ? C5 C6 O5 C7 -177.43(18) . . . . ? C7 C8 O6 C9 75.8(3) . . . . ? C27 C22 P1 C16 -99.17(17) . . . . ? C23 C22 P1 C16 82.06(19) . . . . ? C27 C22 P1 C10 152.10(16) . . . . ? C23 C22 P1 C10 -26.7(2) . . . . ? C27 C22 P1 Cu1 25.46(18) . . . . ? C23 C22 P1 Cu1 -153.31(16) . . . . ? C17 C16 P1 C22 161.80(17) . . . . ? C21 C16 P1 C22 -17.2(2) . . . . ? C17 C16 P1 C10 -89.15(18) . . . . ? C21 C16 P1 C10 91.90(19) . . . . ? C17 C16 P1 Cu1 35.26(19) . . . . ? C21 C16 P1 Cu1 -143.70(16) . . . . ? C15 C10 P1 C22 124.76(17) . . . . ? C11 C10 P1 C22 -58.82(18) . . . . ? C15 C10 P1 C16 14.86(19) . . . . ? C11 C10 P1 C16 -168.72(17) . . . . ? C15 C10 P1 Cu1 -108.08(16) . . . . ? C11 C10 P1 Cu1 68.34(18) . . . . ? C33 C28 P2 C40 -20.4(2) . . . . ? C29 C28 P2 C40 159.35(16) . . . . ? C33 C28 P2 C34 89.71(19) . . . . ? C29 C28 P2 C34 -90.53(17) . . . . ? C33 C28 P2 Cu1 -146.32(16) . . . . ? C29 C28 P2 Cu1 33.45(18) . . . . ? C45 C40 P2 C28 -93.14(17) . . . . ? C41 C40 P2 C28 81.4(2) . . . . ? C45 C40 P2 C34 158.39(16) . . . . ? C41 C40 P2 C34 -27.0(2) . . . . ? C45 C40 P2 Cu1 31.68(19) . . . . ? C41 C40 P2 Cu1 -153.75(16) . . . . ? C35 C34 P2 C28 17.5(2) . . . . ? C39 C34 P2 C28 -170.69(17) . . . . ? C35 C34 P2 C40 125.37(18) . . . . ? C39 C34 P2 C40 -62.81(19) . . . . ? C35 C34 P2 Cu1 -106.71(18) . . . . ? C39 C34 P2 Cu1 65.11(18) . . . . ? C1 O1 Cu1 P2 -111.58(11) . . . . ? C1 O1 Cu1 P1 85.73(12) . . . . ? C1 O1 Cu1 O2 -5.64(11) . . . . ? C28 P2 Cu1 O1 144.79(8) . . . . ? C40 P2 Cu1 O1 25.93(9) . . . . ? C34 P2 Cu1 O1 -96.77(8) . . . . ? C28 P2 Cu1 P1 -57.83(8) . . . . ? C40 P2 Cu1 P1 -176.69(7) . . . . ? C34 P2 Cu1 P1 60.61(8) . . . . ? C28 P2 Cu1 O2 75.53(8) . . . . ? C40 P2 Cu1 O2 -43.33(9) . . . . ? C34 P2 Cu1 O2 -166.04(8) . . . . ? C28 P2 Cu1 C1 109.26(9) . . . . ? C40 P2 Cu1 C1 -9.60(10) . . . . ? C34 P2 Cu1 C1 -132.30(9) . . . . ? C22 P1 Cu1 O1 103.40(9) . . . . ? C16 P1 Cu1 O1 -135.78(8) . . . . ? C10 P1 Cu1 O1 -17.69(9) . . . . ? C22 P1 Cu1 P2 -56.40(8) . . . . ? C16 P1 Cu1 P2 64.42(8) . . . . ? C10 P1 Cu1 P2 -177.49(8) . . . . ? C22 P1 Cu1 O2 164.49(8) . . . . ? C16 P1 Cu1 O2 -74.69(8) . . . . ? C10 P1 Cu1 O2 43.40(9) . . . . ? C22 P1 Cu1 C1 134.17(9) . . . . ? C16 P1 Cu1 C1 -105.01(9) . . . . ? C10 P1 Cu1 C1 13.08(9) . . . . ? C1 O2 Cu1 O1 5.68(11) . . . . ? C1 O2 Cu1 P2 116.31(11) . . . . ? C1 O2 Cu1 P1 -97.00(11) . . . . ? O2 C1 Cu1 O1 -170.20(19) . . . . ? C2 C1 Cu1 O1 61.6(6) . . . . ? O2 C1 Cu1 P2 -81.87(12) . . . . ? O1 C1 Cu1 P2 88.32(12) . . . . ? C2 C1 Cu1 P2 149.9(6) . . . . ? O2 C1 Cu1 P1 88.34(11) . . . . ? O1 C1 Cu1 P1 -101.46(11) . . . . ? C2 C1 Cu1 P1 -39.9(7) . . . . ? O1 C1 Cu1 O2 170.20(19) . . . . ? C2 C1 Cu1 O2 -128.2(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.424 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.057 _database_code_depnum_ccdc_archive 'CCDC 932856' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl4 #TrackingRef 'ad120305.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H35 Cu O3 P2' _chemical_formula_sum 'C39 H35 Cu O3 P2' _chemical_formula_weight 677.15 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4723(6) _cell_length_b 12.4970(7) _cell_length_c 12.7037(6) _cell_angle_alpha 67.651(5) _cell_angle_beta 75.301(4) _cell_angle_gamma 62.402(5) _cell_volume 1615.69(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100 _cell_measurement_reflns_used 4762 _cell_measurement_theta_min 2.9653 _cell_measurement_theta_max 28.3497 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 0.813 _exptl_absorpt_correction_T_min 0.87989 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _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 'oxford gemini s' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time 10 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12298 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.75 _reflns_number_total 6090 _reflns_number_gt 4734 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+0.2799P] 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 6090 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0805 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1383(2) 0.0867(3) 0.6001(2) 0.0230(6) Uani 1 1 d . . . C2 C 0.1546(3) 0.0230(3) 0.5110(2) 0.0377(8) Uani 1 1 d . . . H2A H 0.0850 0.0725 0.4666 0.045 Uiso 1 1 calc R . . H2B H 0.2260 0.0256 0.4591 0.045 Uiso 1 1 calc R . . C3 C 0.2819(3) -0.1861(3) 0.5986(3) 0.0415(8) Uani 1 1 d . . . H3A H 0.2869 -0.2712 0.6305 0.062 Uiso 1 1 calc R . . H3B H 0.2915 -0.1606 0.6568 0.062 Uiso 1 1 calc R . . H3C H 0.3450 -0.1828 0.5373 0.062 Uiso 1 1 calc R . . C4 C 0.4033(2) -0.0101(2) 0.7980(2) 0.0182(6) Uani 1 1 d . . . C5 C 0.4705(2) -0.1129(2) 0.8833(2) 0.0201(6) Uani 1 1 d . . . H5 H 0.4488 -0.1132 0.9590 0.024 Uiso 1 1 calc R . . C6 C 0.5692(2) -0.2149(2) 0.8569(2) 0.0238(6) Uani 1 1 d . . . H6 H 0.6130 -0.2830 0.9151 0.029 Uiso 1 1 calc R . . C7 C 0.6030(3) -0.2168(3) 0.7460(2) 0.0312(7) Uani 1 1 d . . . H7 H 0.6702 -0.2848 0.7284 0.037 Uiso 1 1 calc R . . C8 C 0.5352(3) -0.1155(3) 0.6603(2) 0.0392(8) Uani 1 1 d . . . H8 H 0.5570 -0.1161 0.5849 0.047 Uiso 1 1 calc R . . C9 C 0.4361(3) -0.0140(3) 0.6861(2) 0.0300(7) Uani 1 1 d . . . H9 H 0.3907 0.0524 0.6280 0.036 Uiso 1 1 calc R . . C10 C 0.2348(2) 0.0682(2) 0.9801(2) 0.0173(5) Uani 1 1 d . . . C11 C 0.2733(2) 0.0876(2) 1.0624(2) 0.0196(6) Uani 1 1 d . . . H11 H 0.3232 0.1308 1.0403 0.023 Uiso 1 1 calc R . . C12 C 0.2375(2) 0.0426(2) 1.1775(2) 0.0223(6) Uani 1 1 d . . . H12 H 0.2633 0.0560 1.2321 0.027 Uiso 1 1 calc R . . C13 C 0.1641(2) -0.0219(2) 1.2111(2) 0.0248(6) Uani 1 1 d . . . H13 H 0.1395 -0.0508 1.2882 0.030 Uiso 1 1 calc R . . C14 C 0.1268(2) -0.0438(2) 1.1301(2) 0.0237(6) Uani 1 1 d . . . H14 H 0.0779 -0.0883 1.1529 0.028 Uiso 1 1 calc R . . C15 C 0.1622(2) 0.0006(2) 1.0156(2) 0.0205(6) Uani 1 1 d . . . H15 H 0.1375 -0.0148 0.9616 0.025 Uiso 1 1 calc R . . C16 C 0.3399(2) 0.2349(2) 0.81794(19) 0.0171(5) Uani 1 1 d . . . C17 C 0.2618(2) 0.3524(2) 0.8332(2) 0.0209(6) Uani 1 1 d . . . H17 H 0.1785 0.3747 0.8462 0.025 Uiso 1 1 calc R . . C18 C 0.3070(3) 0.4365(2) 0.8293(2) 0.0244(6) Uani 1 1 d . . . H18 H 0.2541 0.5142 0.8409 0.029 Uiso 1 1 calc R . . C19 C 0.4300(3) 0.4053(3) 0.8083(2) 0.0255(6) Uani 1 1 d . . . H19 H 0.4602 0.4622 0.8047 0.031 Uiso 1 1 calc R . . C20 C 0.5090(3) 0.2888(3) 0.7925(2) 0.0257(6) Uani 1 1 d . . . H20 H 0.5922 0.2674 0.7786 0.031 Uiso 1 1 calc R . . C21 C 0.4638(2) 0.2042(2) 0.7975(2) 0.0218(6) Uani 1 1 d . . . H21 H 0.5171 0.1261 0.7870 0.026 Uiso 1 1 calc R . . C22 C -0.1599(2) 0.3447(2) 0.8784(2) 0.0187(6) Uani 1 1 d . . . C23 C -0.2851(2) 0.3942(2) 0.8826(2) 0.0229(6) Uani 1 1 d . . . H23 H -0.3235 0.4487 0.8166 0.028 Uiso 1 1 calc R . . C24 C -0.3543(3) 0.3633(3) 0.9848(2) 0.0269(6) Uani 1 1 d . . . H24 H -0.4385 0.3970 0.9868 0.032 Uiso 1 1 calc R . . C25 C -0.2978(2) 0.2826(2) 1.0832(2) 0.0230(6) Uani 1 1 d . . . H25 H -0.3440 0.2612 1.1513 0.028 Uiso 1 1 calc R . . C26 C -0.1736(2) 0.2337(2) 1.0808(2) 0.0212(6) Uani 1 1 d . . . H26 H -0.1359 0.1804 1.1475 0.025 Uiso 1 1 calc R . . C27 C -0.1045(2) 0.2636(2) 0.9792(2) 0.0196(6) Uani 1 1 d . . . H27 H -0.0204 0.2295 0.9779 0.024 Uiso 1 1 calc R . . C28 C -0.1680(2) 0.4464(2) 0.63769(19) 0.0191(6) Uani 1 1 d . . . C29 C -0.2154(2) 0.5745(2) 0.57301(19) 0.0191(6) Uani 1 1 d . . . H29 H -0.1907 0.6306 0.5809 0.023 Uiso 1 1 calc R . . C30 C -0.2998(2) 0.6172(3) 0.4967(2) 0.0250(6) Uani 1 1 d . . . H30 H -0.3308 0.7021 0.4531 0.030 Uiso 1 1 calc R . . C31 C -0.3381(2) 0.5360(3) 0.4847(2) 0.0267(7) Uani 1 1 d . . . H31 H -0.3961 0.5663 0.4347 0.032 Uiso 1 1 calc R . . C32 C -0.2900(3) 0.4084(3) 0.5476(2) 0.0282(7) Uani 1 1 d . . . H32 H -0.3155 0.3529 0.5396 0.034 Uiso 1 1 calc R . . C33 C -0.2039(2) 0.3639(2) 0.6220(2) 0.0236(6) Uani 1 1 d . . . H33 H -0.1698 0.2779 0.6620 0.028 Uiso 1 1 calc R . . C34 C -0.0430(2) 0.5123(2) 0.7508(2) 0.0176(6) Uani 1 1 d . . . C35 C 0.0185(2) 0.5714(2) 0.6569(2) 0.0208(6) Uani 1 1 d . . . H35 H 0.0444 0.5452 0.5919 0.025 Uiso 1 1 calc R . . C36 C 0.0414(2) 0.6684(2) 0.6594(2) 0.0245(6) Uani 1 1 d . . . H36 H 0.0803 0.7087 0.5953 0.029 Uiso 1 1 calc R . . C37 C 0.0068(2) 0.7060(2) 0.7564(2) 0.0259(6) Uani 1 1 d . . . H37 H 0.0231 0.7707 0.7581 0.031 Uiso 1 1 calc R . . C38 C -0.0519(2) 0.6469(2) 0.8506(2) 0.0253(6) Uani 1 1 d . . . H38 H -0.0743 0.6712 0.9163 0.030 Uiso 1 1 calc R . . C39 C -0.0781(2) 0.5516(2) 0.8483(2) 0.0208(6) Uani 1 1 d . . . H39 H -0.1191 0.5136 0.9119 0.025 Uiso 1 1 calc R . . O1 O 0.16170(18) 0.18263(16) 0.56406(14) 0.0266(4) Uani 1 1 d . . . O2 O 0.10243(18) 0.04375(18) 0.70113(15) 0.0304(5) Uani 1 1 d . . . O3 O 0.1673(2) -0.10326(18) 0.55617(16) 0.0372(5) Uani 1 1 d . . . P1 P 0.27323(6) 0.12797(6) 0.82698(5) 0.01684(15) Uani 1 1 d . . . P2 P -0.06274(6) 0.37844(6) 0.74650(5) 0.01731(15) Uani 1 1 d . . . Cu1 Cu 0.11403(3) 0.21667(3) 0.72381(2) 0.01891(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0250(16) 0.0227(15) 0.0202(15) -0.0035(12) -0.0075(12) -0.0087(13) C2 0.065(2) 0.0253(17) 0.0279(16) -0.0081(13) -0.0115(15) -0.0187(16) C3 0.053(2) 0.0322(19) 0.0409(19) -0.0169(15) -0.0107(16) -0.0106(17) C4 0.0196(15) 0.0191(14) 0.0189(13) -0.0078(11) -0.0009(10) -0.0093(12) C5 0.0183(15) 0.0236(15) 0.0207(14) -0.0090(11) -0.0023(11) -0.0085(12) C6 0.0217(16) 0.0214(15) 0.0280(15) -0.0078(12) -0.0055(12) -0.0068(12) C7 0.0260(17) 0.0270(17) 0.0339(17) -0.0157(13) -0.0013(13) -0.0013(13) C8 0.044(2) 0.0394(19) 0.0197(15) -0.0160(14) 0.0017(13) -0.0022(16) C9 0.0345(18) 0.0228(16) 0.0198(15) -0.0067(12) -0.0047(12) 0.0000(13) C10 0.0151(14) 0.0148(13) 0.0162(13) -0.0033(10) -0.0024(10) -0.0021(11) C11 0.0181(14) 0.0194(14) 0.0211(14) -0.0066(11) -0.0019(11) -0.0073(12) C12 0.0265(16) 0.0191(14) 0.0194(14) -0.0073(11) -0.0056(11) -0.0048(12) C13 0.0284(17) 0.0156(14) 0.0202(14) -0.0040(11) 0.0018(11) -0.0041(12) C14 0.0258(16) 0.0175(14) 0.0256(15) -0.0035(11) -0.0009(12) -0.0104(12) C15 0.0212(15) 0.0190(14) 0.0209(14) -0.0077(11) -0.0034(11) -0.0060(12) C16 0.0187(14) 0.0177(14) 0.0126(12) -0.0017(10) -0.0048(10) -0.0063(11) C17 0.0185(15) 0.0233(15) 0.0194(14) -0.0052(11) -0.0055(11) -0.0065(12) C18 0.0307(17) 0.0168(14) 0.0247(15) -0.0041(11) -0.0116(12) -0.0060(12) C19 0.0319(17) 0.0247(16) 0.0249(15) -0.0002(12) -0.0130(12) -0.0162(13) C20 0.0197(15) 0.0303(17) 0.0260(15) -0.0029(12) -0.0055(12) -0.0120(13) C21 0.0234(16) 0.0198(14) 0.0199(14) -0.0040(11) -0.0027(11) -0.0082(12) C22 0.0231(15) 0.0166(14) 0.0176(13) -0.0060(10) -0.0022(11) -0.0083(12) C23 0.0216(15) 0.0231(15) 0.0215(14) -0.0036(11) -0.0059(11) -0.0077(12) C24 0.0217(16) 0.0332(17) 0.0244(15) -0.0091(13) -0.0014(12) -0.0102(13) C25 0.0281(16) 0.0276(16) 0.0191(14) -0.0092(12) 0.0018(11) -0.0164(13) C26 0.0296(16) 0.0211(14) 0.0159(13) -0.0030(11) -0.0066(11) -0.0128(12) C27 0.0210(15) 0.0182(14) 0.0220(14) -0.0076(11) -0.0048(11) -0.0074(12) C28 0.0213(15) 0.0197(14) 0.0141(13) -0.0055(11) -0.0008(10) -0.0070(12) C29 0.0231(15) 0.0192(14) 0.0139(13) -0.0059(10) -0.0005(10) -0.0079(12) C30 0.0281(17) 0.0230(15) 0.0167(14) -0.0026(11) -0.0066(12) -0.0051(13) C31 0.0239(16) 0.0382(18) 0.0176(14) -0.0078(12) -0.0044(11) -0.0119(14) C32 0.0377(18) 0.0375(18) 0.0201(15) -0.0090(13) -0.0034(12) -0.0236(15) C33 0.0304(17) 0.0200(15) 0.0200(14) -0.0014(11) -0.0068(12) -0.0116(13) C34 0.0153(14) 0.0147(13) 0.0200(13) -0.0046(11) -0.0077(10) -0.0014(11) C35 0.0202(15) 0.0213(15) 0.0195(14) -0.0079(11) -0.0019(11) -0.0059(12) C36 0.0202(15) 0.0230(15) 0.0290(15) -0.0057(12) -0.0029(12) -0.0093(12) C37 0.0239(16) 0.0175(15) 0.0383(17) -0.0101(12) -0.0108(13) -0.0049(12) C38 0.0292(17) 0.0197(15) 0.0280(15) -0.0119(12) -0.0085(12) -0.0043(13) C39 0.0224(15) 0.0182(14) 0.0170(13) -0.0052(11) -0.0037(11) -0.0037(12) O1 0.0411(13) 0.0195(10) 0.0214(10) -0.0051(8) -0.0067(8) -0.0133(9) O2 0.0348(12) 0.0379(12) 0.0225(11) -0.0095(9) 0.0037(9) -0.0211(10) O3 0.0521(15) 0.0245(12) 0.0425(13) -0.0110(9) -0.0120(11) -0.0174(11) P1 0.0167(4) 0.0171(4) 0.0168(3) -0.0060(3) -0.0023(3) -0.0060(3) P2 0.0197(4) 0.0161(4) 0.0157(3) -0.0048(3) -0.0034(3) -0.0062(3) Cu1 0.01906(19) 0.01893(19) 0.01870(18) -0.00730(13) -0.00368(13) -0.00560(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.242(3) . ? C1 O1 1.254(3) . ? C1 C2 1.540(4) . ? C1 Cu1 2.539(3) . ? C2 O3 1.404(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 O3 1.415(3) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C9 1.390(3) . ? C4 C5 1.390(3) . ? C4 P1 1.825(3) . ? C5 C6 1.384(4) . ? C5 H5 0.9300 . ? C6 C7 1.371(4) . ? C6 H6 0.9300 . ? C7 C8 1.389(4) . ? C7 H7 0.9300 . ? C8 C9 1.379(4) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.392(3) . ? C10 C15 1.396(3) . ? C10 P1 1.824(2) . ? C11 C12 1.389(3) . ? C11 H11 0.9300 . ? C12 C13 1.376(4) . ? C12 H12 0.9300 . ? C13 C14 1.388(3) . ? C13 H13 0.9300 . ? C14 C15 1.380(3) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C21 1.388(3) . ? C16 C17 1.393(3) . ? C16 P1 1.831(2) . ? C17 C18 1.385(3) . ? C17 H17 0.9300 . ? C18 C19 1.377(4) . ? C18 H18 0.9300 . ? C19 C20 1.387(4) . ? C19 H19 0.9300 . ? C20 C21 1.387(4) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.383(3) . ? C22 C27 1.399(3) . ? C22 P2 1.833(3) . ? C23 C24 1.392(4) . ? C23 H23 0.9300 . ? C24 C25 1.381(3) . ? C24 H24 0.9300 . ? C25 C26 1.374(4) . ? C25 H25 0.9300 . ? C26 C27 1.384(3) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C33 1.390(3) . ? C28 C29 1.399(3) . ? C28 P2 1.831(2) . ? C29 C30 1.392(3) . ? C29 H29 0.9300 . ? C30 C31 1.373(4) . ? C30 H30 0.9300 . ? C31 C32 1.389(4) . ? C31 H31 0.9300 . ? C32 C33 1.385(3) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.396(3) . ? C34 C39 1.399(3) . ? C34 P2 1.822(2) . ? C35 C36 1.380(4) . ? C35 H35 0.9300 . ? C36 C37 1.382(4) . ? C36 H36 0.9300 . ? C37 C38 1.378(4) . ? C37 H37 0.9300 . ? C38 C39 1.383(4) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? O1 Cu1 2.1125(18) . ? O2 Cu1 2.3575(19) . ? P1 Cu1 2.2507(7) . ? P2 Cu1 2.2410(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O1 123.4(2) . . ? O2 C1 C2 120.3(2) . . ? O1 C1 C2 116.3(2) . . ? O2 C1 Cu1 67.33(14) . . ? O1 C1 Cu1 56.05(13) . . ? C2 C1 Cu1 172.16(19) . . ? O3 C2 C1 115.2(2) . . ? O3 C2 H2A 108.5 . . ? C1 C2 H2A 108.5 . . ? O3 C2 H2B 108.5 . . ? C1 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? O3 C3 H3A 109.5 . . ? O3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? O3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C9 C4 C5 118.2(2) . . ? C9 C4 P1 118.84(18) . . ? C5 C4 P1 122.95(19) . . ? C6 C5 C4 120.8(2) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C7 C6 C5 120.7(2) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C8 118.9(3) . . ? C6 C7 H7 120.5 . . ? C8 C7 H7 120.5 . . ? C9 C8 C7 120.7(3) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C4 120.6(2) . . ? C8 C9 H9 119.7 . . ? C4 C9 H9 119.7 . . ? C11 C10 C15 118.8(2) . . ? C11 C10 P1 123.36(19) . . ? C15 C10 P1 117.82(18) . . ? C12 C11 C10 120.3(2) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C13 C12 C11 120.3(2) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 120.1(2) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 119.9(2) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C10 120.7(2) . . ? C14 C15 H15 119.7 . . ? C10 C15 H15 119.7 . . ? C21 C16 C17 118.6(2) . . ? C21 C16 P1 123.3(2) . . ? C17 C16 P1 118.04(19) . . ? C18 C17 C16 120.7(3) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C19 C18 C17 120.0(3) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 120.0(2) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C19 C20 C21 119.9(3) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C20 C21 C16 120.7(3) . . ? C20 C21 H21 119.7 . . ? C16 C21 H21 119.7 . . ? C23 C22 C27 118.5(2) . . ? C23 C22 P2 123.10(18) . . ? C27 C22 P2 118.39(19) . . ? C22 C23 C24 120.7(2) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C25 C24 C23 119.9(3) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C26 C25 C24 120.2(2) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C27 120.0(2) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C22 120.7(2) . . ? C26 C27 H27 119.6 . . ? C22 C27 H27 119.6 . . ? C33 C28 C29 119.2(2) . . ? C33 C28 P2 116.59(18) . . ? C29 C28 P2 124.20(19) . . ? C30 C29 C28 119.3(2) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C31 C30 C29 121.1(2) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C30 C31 C32 119.7(2) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C33 C32 C31 119.9(2) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32 C33 C28 120.7(2) . . ? C32 C33 H33 119.6 . . ? C28 C33 H33 119.6 . . ? C35 C34 C39 118.3(2) . . ? C35 C34 P2 118.93(19) . . ? C39 C34 P2 122.5(2) . . ? C36 C35 C34 120.7(2) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C37 120.4(3) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C38 C37 C36 119.5(2) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C37 C38 C39 120.7(2) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C38 C39 C34 120.3(2) . . ? C38 C39 H39 119.9 . . ? C34 C39 H39 119.9 . . ? C1 O1 Cu1 94.46(16) . . ? C1 O2 Cu1 83.58(15) . . ? C2 O3 C3 111.5(2) . . ? C10 P1 C4 102.31(11) . . ? C10 P1 C16 103.12(11) . . ? C4 P1 C16 104.03(11) . . ? C10 P1 Cu1 113.15(8) . . ? C4 P1 Cu1 117.26(8) . . ? C16 P1 Cu1 115.19(8) . . ? C34 P2 C28 105.03(11) . . ? C34 P2 C22 103.05(12) . . ? C28 P2 C22 101.59(11) . . ? C34 P2 Cu1 112.92(8) . . ? C28 P2 Cu1 116.40(9) . . ? C22 P2 Cu1 116.20(8) . . ? O1 Cu1 P2 117.59(5) . . ? O1 Cu1 P1 113.37(6) . . ? P2 Cu1 P1 125.81(3) . . ? O1 Cu1 O2 58.58(6) . . ? P2 Cu1 O2 116.64(5) . . ? P1 Cu1 O2 104.54(5) . . ? O1 Cu1 C1 29.49(7) . . ? P2 Cu1 C1 121.19(6) . . ? P1 Cu1 C1 112.06(6) . . ? O2 Cu1 C1 29.09(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 O3 -20.7(4) . . . . ? O1 C1 C2 O3 160.1(3) . . . . ? Cu1 C1 C2 O3 172.4(13) . . . . ? C9 C4 C5 C6 1.7(4) . . . . ? P1 C4 C5 C6 -179.37(19) . . . . ? C4 C5 C6 C7 0.0(4) . . . . ? C5 C6 C7 C8 -1.1(4) . . . . ? C6 C7 C8 C9 0.5(5) . . . . ? C7 C8 C9 C4 1.2(5) . . . . ? C5 C4 C9 C8 -2.3(4) . . . . ? P1 C4 C9 C8 178.7(2) . . . . ? C15 C10 C11 C12 -1.4(4) . . . . ? P1 C10 C11 C12 178.06(19) . . . . ? C10 C11 C12 C13 0.2(4) . . . . ? C11 C12 C13 C14 0.9(4) . . . . ? C12 C13 C14 C15 -0.8(4) . . . . ? C13 C14 C15 C10 -0.5(4) . . . . ? C11 C10 C15 C14 1.6(4) . . . . ? P1 C10 C15 C14 -177.98(19) . . . . ? C21 C16 C17 C18 -0.7(3) . . . . ? P1 C16 C17 C18 178.89(18) . . . . ? C16 C17 C18 C19 1.1(4) . . . . ? C17 C18 C19 C20 -0.8(4) . . . . ? C18 C19 C20 C21 0.2(4) . . . . ? C19 C20 C21 C16 0.1(4) . . . . ? C17 C16 C21 C20 0.1(3) . . . . ? P1 C16 C21 C20 -179.46(18) . . . . ? C27 C22 C23 C24 -0.4(4) . . . . ? P2 C22 C23 C24 178.7(2) . . . . ? C22 C23 C24 C25 0.1(4) . . . . ? C23 C24 C25 C26 0.7(4) . . . . ? C24 C25 C26 C27 -1.1(4) . . . . ? C25 C26 C27 C22 0.7(4) . . . . ? C23 C22 C27 C26 0.0(4) . . . . ? P2 C22 C27 C26 -179.14(19) . . . . ? C33 C28 C29 C30 1.7(4) . . . . ? P2 C28 C29 C30 -176.7(2) . . . . ? C28 C29 C30 C31 0.6(4) . . . . ? C29 C30 C31 C32 -1.6(4) . . . . ? C30 C31 C32 C33 0.2(4) . . . . ? C31 C32 C33 C28 2.2(4) . . . . ? C29 C28 C33 C32 -3.1(4) . . . . ? P2 C28 C33 C32 175.4(2) . . . . ? C39 C34 C35 C36 -1.6(4) . . . . ? P2 C34 C35 C36 -176.31(18) . . . . ? C34 C35 C36 C37 1.9(4) . . . . ? C35 C36 C37 C38 -0.7(4) . . . . ? C36 C37 C38 C39 -0.9(4) . . . . ? C37 C38 C39 C34 1.2(4) . . . . ? C35 C34 C39 C38 0.0(4) . . . . ? P2 C34 C39 C38 174.55(19) . . . . ? O2 C1 O1 Cu1 -1.2(3) . . . . ? C2 C1 O1 Cu1 178.0(2) . . . . ? O1 C1 O2 Cu1 1.1(3) . . . . ? C2 C1 O2 Cu1 -178.1(2) . . . . ? C1 C2 O3 C3 -72.2(3) . . . . ? C11 C10 P1 C4 97.2(2) . . . . ? C15 C10 P1 C4 -83.3(2) . . . . ? C11 C10 P1 C16 -10.6(2) . . . . ? C15 C10 P1 C16 168.9(2) . . . . ? C11 C10 P1 Cu1 -135.67(19) . . . . ? C15 C10 P1 Cu1 43.8(2) . . . . ? C9 C4 P1 C10 161.2(2) . . . . ? C5 C4 P1 C10 -17.8(2) . . . . ? C9 C4 P1 C16 -91.7(2) . . . . ? C5 C4 P1 C16 89.3(2) . . . . ? C9 C4 P1 Cu1 36.8(2) . . . . ? C5 C4 P1 Cu1 -142.18(18) . . . . ? C21 C16 P1 C10 104.3(2) . . . . ? C17 C16 P1 C10 -75.22(19) . . . . ? C21 C16 P1 C4 -2.2(2) . . . . ? C17 C16 P1 C4 178.28(18) . . . . ? C21 C16 P1 Cu1 -131.91(18) . . . . ? C17 C16 P1 Cu1 48.5(2) . . . . ? C35 C34 P2 C28 -68.3(2) . . . . ? C39 C34 P2 C28 117.2(2) . . . . ? C35 C34 P2 C22 -174.34(19) . . . . ? C39 C34 P2 C22 11.2(2) . . . . ? C35 C34 P2 Cu1 59.5(2) . . . . ? C39 C34 P2 Cu1 -115.0(2) . . . . ? C33 C28 P2 C34 -176.5(2) . . . . ? C29 C28 P2 C34 1.9(3) . . . . ? C33 C28 P2 C22 -69.4(2) . . . . ? C29 C28 P2 C22 109.0(2) . . . . ? C33 C28 P2 Cu1 57.8(2) . . . . ? C29 C28 P2 Cu1 -123.8(2) . . . . ? C23 C22 P2 C34 94.1(2) . . . . ? C27 C22 P2 C34 -86.8(2) . . . . ? C23 C22 P2 C28 -14.5(2) . . . . ? C27 C22 P2 C28 164.6(2) . . . . ? C23 C22 P2 Cu1 -141.91(19) . . . . ? C27 C22 P2 Cu1 37.2(2) . . . . ? C1 O1 Cu1 P2 -105.26(15) . . . . ? C1 O1 Cu1 P1 93.86(15) . . . . ? C1 O1 Cu1 O2 0.62(15) . . . . ? C34 P2 Cu1 O1 -108.34(10) . . . . ? C28 P2 Cu1 O1 13.28(11) . . . . ? C22 P2 Cu1 O1 132.90(10) . . . . ? C34 P2 Cu1 P1 49.90(9) . . . . ? C28 P2 Cu1 P1 171.52(9) . . . . ? C22 P2 Cu1 P1 -68.86(9) . . . . ? C34 P2 Cu1 O2 -175.01(9) . . . . ? C28 P2 Cu1 O2 -53.39(11) . . . . ? C22 P2 Cu1 O2 66.23(10) . . . . ? C34 P2 Cu1 C1 -142.07(11) . . . . ? C28 P2 Cu1 C1 -20.45(12) . . . . ? C22 P2 Cu1 C1 99.18(11) . . . . ? C10 P1 Cu1 O1 -143.81(10) . . . . ? C4 P1 Cu1 O1 -25.04(11) . . . . ? C16 P1 Cu1 O1 97.90(11) . . . . ? C10 P1 Cu1 P2 57.16(10) . . . . ? C4 P1 Cu1 P2 175.93(9) . . . . ? C16 P1 Cu1 P2 -61.13(10) . . . . ? C10 P1 Cu1 O2 -82.15(10) . . . . ? C4 P1 Cu1 O2 36.62(11) . . . . ? C16 P1 Cu1 O2 159.56(10) . . . . ? C10 P1 Cu1 C1 -111.80(11) . . . . ? C4 P1 Cu1 C1 6.97(12) . . . . ? C16 P1 Cu1 C1 129.90(11) . . . . ? C1 O2 Cu1 O1 -0.63(15) . . . . ? C1 O2 Cu1 P2 106.87(15) . . . . ? C1 O2 Cu1 P1 -109.40(15) . . . . ? O2 C1 Cu1 O1 178.9(3) . . . . ? C2 C1 Cu1 O1 -13.4(14) . . . . ? O2 C1 Cu1 P2 -89.42(15) . . . . ? O1 C1 Cu1 P2 91.67(16) . . . . ? C2 C1 Cu1 P2 78.3(15) . . . . ? O2 C1 Cu1 P1 80.13(15) . . . . ? O1 C1 Cu1 P1 -98.78(15) . . . . ? C2 C1 Cu1 P1 -112.2(15) . . . . ? O1 C1 Cu1 O2 -178.9(3) . . . . ? C2 C1 Cu1 O2 167.7(16) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.75 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.440 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.064 _database_code_depnum_ccdc_archive 'CCDC 932857' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_adner1 #TrackingRef 'adner1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H39 Cu O4 P2' _chemical_formula_sum 'C41 H39 Cu O4 P2' _chemical_formula_weight 721.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 21.2391(2) _cell_length_b 10.7028(1) _cell_length_c 30.5782(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6950.97(11) _cell_formula_units_Z 8 _cell_measurement_temperature 115(2) _cell_measurement_reflns_used 8789 _cell_measurement_theta_min 3.5590 _cell_measurement_theta_max 62.8473 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 2.090 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET) (compiled Mar 22 2010,13:57:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.5729 _exptl_absorpt_correction_T_max 0.6800 _exptl_special_details ; ? ; _diffrn_ambient_temperature 115(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'oxford gemini s' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time 5 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13967 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 62.94 _reflns_number_total 5547 _reflns_number_gt 4614 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET) (compiled Mar 22 2010,13:57:49) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET) (compiled Mar 22 2010,13:57:49) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET) (compiled Mar 22 2010,13:57:49) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0718P)^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 5547 _refine_ls_number_parameters 455 _refine_ls_number_restraints 127 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0929 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.985 _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 C1 C -0.04753(11) 1.0093(2) 0.38694(7) 0.0237(5) Uani 1 1 d . . . C2 C -0.10244(12) 1.0866(2) 0.40469(8) 0.0348(6) Uani 1 1 d . . . H2A H -0.1059 1.0711 0.4365 0.042 Uiso 1 1 calc R . . H2B H -0.0923 1.1762 0.4007 0.042 Uiso 1 1 calc R . . C3 C -0.19018(12) 0.9526(3) 0.40163(8) 0.0410(7) Uani 1 1 d DU . . H3A H -0.1975 0.9588 0.4335 0.049 Uiso 1 1 calc R A 1 H3B H -0.1635 0.8787 0.3957 0.049 Uiso 1 1 calc R A 1 C6 C 0.10549(10) 1.05615(19) 0.28812(6) 0.0193(4) Uani 1 1 d . . . C7 C 0.04387(10) 1.0879(2) 0.27800(7) 0.0225(5) Uani 1 1 d . . . H7 H 0.0100 1.0404 0.2897 0.027 Uiso 1 1 calc R . . C8 C 0.03143(11) 1.1891(2) 0.25076(7) 0.0277(5) Uani 1 1 d . . . H8 H -0.0108 1.2102 0.2438 0.033 Uiso 1 1 calc R . . C9 C 0.08044(12) 1.2589(2) 0.23381(7) 0.0301(5) Uani 1 1 d . . . H9 H 0.0719 1.3273 0.2149 0.036 Uiso 1 1 calc R . . C10 C 0.14201(12) 1.2289(2) 0.24442(7) 0.0299(5) Uani 1 1 d . . . H10 H 0.1756 1.2779 0.2332 0.036 Uiso 1 1 calc R . . C11 C 0.15493(11) 1.1274(2) 0.27148(7) 0.0234(5) Uani 1 1 d . . . H11 H 0.1972 1.1069 0.2786 0.028 Uiso 1 1 calc R . . C12 C 0.19382(10) 0.94841(19) 0.34820(6) 0.0178(4) Uani 1 1 d . . . C13 C 0.19562(11) 1.0473(2) 0.37776(7) 0.0249(5) Uani 1 1 d . . . H13 H 0.1593 1.0980 0.3818 0.030 Uiso 1 1 calc R . . C14 C 0.24989(11) 1.0724(2) 0.40124(7) 0.0306(5) Uani 1 1 d . . . H14 H 0.2512 1.1415 0.4208 0.037 Uiso 1 1 calc R . . C15 C 0.30214(11) 0.9969(2) 0.39624(8) 0.0316(5) Uani 1 1 d . . . H15 H 0.3389 1.0124 0.4131 0.038 Uiso 1 1 calc R . . C16 C 0.30119(12) 0.8993(2) 0.36691(8) 0.0322(6) Uani 1 1 d . . . H16 H 0.3375 0.8486 0.3631 0.039 Uiso 1 1 calc R . . C17 C 0.24662(10) 0.8749(2) 0.34276(7) 0.0249(5) Uani 1 1 d . . . H17 H 0.2459 0.8076 0.3225 0.030 Uiso 1 1 calc R . . C18 C 0.13467(10) 0.7942(2) 0.28188(7) 0.0201(4) Uani 1 1 d . . . C19 C 0.14070(11) 0.8168(2) 0.23724(7) 0.0262(5) Uani 1 1 d . . . H19 H 0.1399 0.9001 0.2265 0.031 Uiso 1 1 calc R . . C20 C 0.14786(12) 0.7178(2) 0.20834(7) 0.0326(6) Uani 1 1 d . . . H20 H 0.1522 0.7338 0.1779 0.039 Uiso 1 1 calc R . . C21 C 0.14878(12) 0.5962(2) 0.22349(8) 0.0314(5) Uani 1 1 d . . . H21 H 0.1526 0.5288 0.2035 0.038 Uiso 1 1 calc R . . C22 C 0.14413(12) 0.5730(2) 0.26785(8) 0.0310(5) Uani 1 1 d . . . H22 H 0.1460 0.4896 0.2784 0.037 Uiso 1 1 calc R . . C23 C 0.13680(11) 0.6716(2) 0.29692(7) 0.0243(5) Uani 1 1 d . . . H23 H 0.1332 0.6552 0.3274 0.029 Uiso 1 1 calc R . . C24 C 0.02676(9) 0.5642(2) 0.39846(6) 0.0175(4) Uani 1 1 d . . . C25 C 0.00923(11) 0.5566(2) 0.35459(7) 0.0256(5) Uani 1 1 d . . . H25 H 0.0037 0.6310 0.3381 0.031 Uiso 1 1 calc R . . C26 C -0.00013(13) 0.4420(2) 0.33494(8) 0.0337(6) Uani 1 1 d . . . H26 H -0.0125 0.4380 0.3051 0.040 Uiso 1 1 calc R . . C27 C 0.00830(12) 0.3335(2) 0.35833(7) 0.0292(5) Uani 1 1 d . . . H27 H 0.0024 0.2548 0.3446 0.035 Uiso 1 1 calc R . . C28 C 0.02551(11) 0.3393(2) 0.40205(7) 0.0260(5) Uani 1 1 d . . . H28 H 0.0308 0.2645 0.4184 0.031 Uiso 1 1 calc R . . C29 C 0.03506(10) 0.4543(2) 0.42192(7) 0.0219(5) Uani 1 1 d . . . H29 H 0.0474 0.4579 0.4518 0.026 Uiso 1 1 calc R . . C30 C -0.03458(9) 0.7381(2) 0.45557(6) 0.0181(4) Uani 1 1 d . . . C31 C -0.03636(10) 0.8370(2) 0.48532(7) 0.0240(5) Uani 1 1 d . . . H31 H -0.0012 0.8914 0.4879 0.029 Uiso 1 1 calc R . . C32 C -0.08891(11) 0.8566(2) 0.51112(7) 0.0259(5) Uani 1 1 d . . . H32 H -0.0898 0.9242 0.5312 0.031 Uiso 1 1 calc R . . C33 C -0.14013(11) 0.7777(2) 0.50760(7) 0.0279(5) Uani 1 1 d . . . H33 H -0.1763 0.7913 0.5252 0.033 Uiso 1 1 calc R . . C34 C -0.13871(11) 0.6790(2) 0.47841(8) 0.0293(5) Uani 1 1 d . . . H34 H -0.1739 0.6244 0.4763 0.035 Uiso 1 1 calc R . . C35 C -0.08646(10) 0.6593(2) 0.45238(7) 0.0217(5) Uani 1 1 d . . . H35 H -0.0860 0.5917 0.4322 0.026 Uiso 1 1 calc R . . C36 C 0.09829(9) 0.72310(19) 0.46109(6) 0.0178(4) Uani 1 1 d . . . C37 C 0.14806(10) 0.8045(2) 0.45363(7) 0.0211(5) Uani 1 1 d . . . H37 H 0.1495 0.8518 0.4274 0.025 Uiso 1 1 calc R . . C38 C 0.19587(10) 0.8169(2) 0.48449(7) 0.0246(5) Uani 1 1 d . . . H38 H 0.2293 0.8742 0.4795 0.029 Uiso 1 1 calc R . . C39 C 0.19491(10) 0.7464(2) 0.52224(7) 0.0248(5) Uani 1 1 d . . . H39 H 0.2279 0.7539 0.5430 0.030 Uiso 1 1 calc R . . C40 C 0.14533(11) 0.6641(2) 0.52975(7) 0.0243(5) Uani 1 1 d . . . H40 H 0.1447 0.6147 0.5555 0.029 Uiso 1 1 calc R . . C41 C 0.09686(10) 0.6543(2) 0.49966(7) 0.0215(5) Uani 1 1 d . . . H41 H 0.0624 0.6002 0.5054 0.026 Uiso 1 1 calc R . . O1 O -0.05599(7) 0.92892(15) 0.35788(5) 0.0268(4) Uani 1 1 d . . . O2 O 0.00521(8) 1.03213(14) 0.40380(5) 0.0278(4) Uani 1 1 d . . . O3 O -0.16135(8) 1.06308(18) 0.38544(6) 0.0401(5) Uani 1 1 d DU B . O4 O -0.29108(18) 1.0448(6) 0.38815(10) 0.0481(15) Uani 0.652(10) 1 d PDU B 1 C4 C -0.2500(3) 0.9435(7) 0.3780(2) 0.0432(15) Uani 0.652(10) 1 d PDU B 1 H4A H -0.2416 0.9427 0.3462 0.052 Uiso 0.652(10) 1 calc PR B 1 H4B H -0.2709 0.8638 0.3857 0.052 Uiso 0.652(10) 1 calc PR B 1 C5 C -0.3124(5) 1.0815(7) 0.3533(2) 0.063(2) Uani 0.652(10) 1 d PDU B 1 H5A H -0.3364 1.1586 0.3580 0.095 Uiso 0.652(10) 1 calc PR B 1 H5B H -0.3403 1.0174 0.3410 0.095 Uiso 0.652(10) 1 calc PR B 1 H5C H -0.2778 1.0978 0.3329 0.095 Uiso 0.652(10) 1 calc PR B 1 O4' O -0.3035(2) 0.9628(10) 0.3783(2) 0.038(2) Uani 0.348(10) 1 d PDU B 2 C4' C -0.2451(5) 0.8925(13) 0.3718(4) 0.0432(15) Uani 0.348(10) 1 d PDU B 2 H4'1 H -0.2327 0.8957 0.3406 0.052 Uiso 0.348(10) 1 calc PR B 2 H4'2 H -0.2516 0.8040 0.3800 0.052 Uiso 0.348(10) 1 calc PR B 2 C5' C -0.3407(5) 1.0623(13) 0.3591(4) 0.047(3) Uani 0.348(10) 1 d PDU B 2 H5'1 H -0.3815 1.0674 0.3740 0.071 Uiso 0.348(10) 1 calc PR B 2 H5'2 H -0.3475 1.0448 0.3280 0.071 Uiso 0.348(10) 1 calc PR B 2 H5'3 H -0.3183 1.1418 0.3623 0.071 Uiso 0.348(10) 1 calc PR B 2 P1 P 0.11831(2) 0.91728(5) 0.321641(16) 0.01649(14) Uani 1 1 d . . . P2 P 0.03471(2) 0.72195(5) 0.420601(16) 0.01624(13) Uani 1 1 d . . . Cu1 Cu 0.045018(14) 0.87493(3) 0.370627(9) 0.01862(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0299(13) 0.0177(11) 0.0235(11) 0.0053(10) 0.0071(10) 0.0055(10) C2 0.0403(15) 0.0295(13) 0.0348(13) 0.0034(11) 0.0111(11) 0.0136(12) C3 0.0313(13) 0.0582(17) 0.0336(13) 0.0179(13) 0.0055(11) 0.0090(13) C6 0.0250(11) 0.0156(10) 0.0172(9) -0.0037(8) 0.0004(8) 0.0000(9) C7 0.0277(12) 0.0200(11) 0.0199(11) -0.0027(9) -0.0003(9) 0.0014(9) C8 0.0352(13) 0.0253(12) 0.0226(11) -0.0023(10) -0.0071(10) 0.0098(10) C9 0.0529(15) 0.0178(11) 0.0198(10) 0.0013(9) -0.0051(10) 0.0034(11) C10 0.0442(14) 0.0183(11) 0.0270(11) 0.0025(9) 0.0044(10) -0.0055(11) C11 0.0279(12) 0.0187(11) 0.0237(11) -0.0009(9) -0.0011(9) -0.0006(9) C12 0.0208(11) 0.0153(10) 0.0173(10) 0.0034(8) 0.0007(8) -0.0036(8) C13 0.0237(12) 0.0241(12) 0.0268(11) -0.0039(9) 0.0035(9) -0.0033(10) C14 0.0297(13) 0.0338(13) 0.0283(11) -0.0077(10) 0.0024(10) -0.0119(11) C15 0.0253(12) 0.0380(14) 0.0316(12) 0.0037(11) -0.0063(10) -0.0119(11) C16 0.0216(12) 0.0302(13) 0.0447(14) 0.0028(11) -0.0037(11) 0.0009(10) C17 0.0235(12) 0.0212(11) 0.0300(11) -0.0023(9) -0.0010(10) -0.0008(9) C18 0.0179(10) 0.0189(11) 0.0234(10) -0.0012(9) 0.0000(8) -0.0020(9) C19 0.0347(13) 0.0190(11) 0.0251(11) 0.0001(9) 0.0021(10) -0.0020(10) C20 0.0458(15) 0.0302(14) 0.0217(11) -0.0063(10) 0.0051(10) -0.0055(12) C21 0.0385(14) 0.0244(12) 0.0313(12) -0.0108(10) 0.0062(11) -0.0027(11) C22 0.0397(14) 0.0186(12) 0.0347(13) -0.0037(10) 0.0035(11) 0.0016(11) C23 0.0296(12) 0.0196(11) 0.0237(11) -0.0015(9) 0.0007(9) -0.0007(10) C24 0.0146(10) 0.0177(11) 0.0201(10) -0.0004(8) 0.0031(8) -0.0004(8) C25 0.0334(12) 0.0205(11) 0.0229(11) 0.0023(9) -0.0014(10) -0.0015(10) C26 0.0500(16) 0.0289(13) 0.0222(11) -0.0037(10) -0.0049(11) -0.0053(12) C27 0.0414(14) 0.0188(11) 0.0273(11) -0.0046(10) 0.0035(10) -0.0054(11) C28 0.0319(12) 0.0166(11) 0.0296(11) 0.0022(10) 0.0021(10) -0.0002(10) C29 0.0256(11) 0.0202(11) 0.0199(10) -0.0002(9) -0.0011(9) 0.0000(9) C30 0.0188(10) 0.0162(10) 0.0192(10) 0.0038(8) 0.0001(8) 0.0020(9) C31 0.0233(11) 0.0224(11) 0.0263(11) -0.0027(10) 0.0014(9) -0.0021(9) C32 0.0282(12) 0.0257(12) 0.0237(11) -0.0047(9) 0.0031(9) 0.0050(10) C33 0.0223(11) 0.0341(13) 0.0272(11) -0.0005(10) 0.0060(9) 0.0060(10) C34 0.0191(11) 0.0303(13) 0.0384(13) 0.0001(11) 0.0039(10) -0.0019(10) C35 0.0197(11) 0.0191(11) 0.0263(11) -0.0021(9) -0.0004(9) 0.0004(9) C36 0.0171(10) 0.0152(10) 0.0210(10) -0.0028(8) 0.0015(8) 0.0016(8) C37 0.0199(10) 0.0212(11) 0.0223(10) -0.0001(9) 0.0028(9) 0.0007(9) C38 0.0187(11) 0.0261(12) 0.0288(11) -0.0013(10) 0.0007(9) -0.0042(9) C39 0.0209(11) 0.0281(12) 0.0254(11) -0.0048(9) -0.0041(9) 0.0022(10) C40 0.0305(12) 0.0229(11) 0.0194(10) 0.0015(9) -0.0010(9) 0.0005(10) C41 0.0233(11) 0.0184(11) 0.0229(10) -0.0011(9) 0.0013(9) -0.0022(9) O1 0.0263(8) 0.0300(9) 0.0242(8) -0.0019(7) -0.0008(6) 0.0058(7) O2 0.0331(9) 0.0170(8) 0.0335(8) -0.0046(7) 0.0035(7) 0.0007(7) O3 0.0343(10) 0.0481(11) 0.0380(9) 0.0208(8) 0.0096(8) 0.0173(8) O4 0.0342(18) 0.081(4) 0.0294(16) -0.0039(18) -0.0005(13) 0.019(2) C4 0.0339(19) 0.071(5) 0.025(2) 0.001(3) 0.0102(16) 0.009(3) C5 0.089(6) 0.062(4) 0.038(3) 0.013(3) 0.023(4) 0.003(4) O4' 0.024(3) 0.057(6) 0.033(3) 0.020(3) 0.004(2) -0.005(3) C4' 0.0339(19) 0.071(5) 0.025(2) 0.001(3) 0.0102(16) 0.009(3) C5' 0.032(5) 0.098(9) 0.013(4) 0.005(4) 0.011(4) 0.008(6) P1 0.0179(3) 0.0140(3) 0.0176(3) 0.0003(2) 0.0006(2) -0.0005(2) P2 0.0169(3) 0.0137(3) 0.0181(3) 0.0010(2) 0.00113(19) -0.0009(2) Cu1 0.01939(18) 0.01600(18) 0.02046(18) 0.00200(12) 0.00237(12) 0.00044(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.250(3) . ? C1 O2 1.257(3) . ? C1 C2 1.530(3) . ? C1 Cu1 2.486(2) . ? C2 O3 1.405(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O3 1.421(3) . ? C3 C4 1.464(6) . ? C3 C4' 1.614(12) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C6 C7 1.387(3) . ? C6 C11 1.394(3) . ? C6 P1 1.826(2) . ? C7 C8 1.392(3) . ? C7 H7 0.9500 . ? C8 C9 1.382(4) . ? C8 H8 0.9500 . ? C9 C10 1.385(4) . ? C9 H9 0.9500 . ? C10 C11 1.393(3) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C17 1.380(3) . ? C12 C13 1.393(3) . ? C12 P1 1.828(2) . ? C13 C14 1.384(3) . ? C13 H13 0.9500 . ? C14 C15 1.381(4) . ? C14 H14 0.9500 . ? C15 C16 1.378(4) . ? C15 H15 0.9500 . ? C16 C17 1.399(3) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.391(3) . ? C18 C19 1.392(3) . ? C18 P1 1.826(2) . ? C19 C20 1.388(3) . ? C19 H19 0.9500 . ? C20 C21 1.381(4) . ? C20 H20 0.9500 . ? C21 C22 1.383(4) . ? C21 H21 0.9500 . ? C22 C23 1.389(3) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C29 1.389(3) . ? C24 C25 1.395(3) . ? C24 P2 1.827(2) . ? C25 C26 1.381(3) . ? C25 H25 0.9500 . ? C26 C27 1.376(4) . ? C26 H26 0.9500 . ? C27 C28 1.387(3) . ? C27 H27 0.9500 . ? C28 C29 1.388(3) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C35 1.391(3) . ? C30 C31 1.396(3) . ? C30 P2 1.827(2) . ? C31 C32 1.383(3) . ? C31 H31 0.9500 . ? C32 C33 1.381(3) . ? C32 H32 0.9500 . ? C33 C34 1.384(3) . ? C33 H33 0.9500 . ? C34 C35 1.382(3) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.388(3) . ? C36 C41 1.391(3) . ? C36 P2 1.832(2) . ? C37 C38 1.393(3) . ? C37 H37 0.9500 . ? C38 C39 1.379(3) . ? C38 H38 0.9500 . ? C39 C40 1.392(3) . ? C39 H39 0.9500 . ? C40 C41 1.385(3) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? O1 Cu1 2.2556(16) . ? O2 Cu1 2.1388(15) . ? O4 C5 1.224(7) . ? O4 C4 1.426(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? O4' C5' 1.450(11) . ? O4' C4' 1.464(11) . ? C4' H4'1 0.9900 . ? C4' H4'2 0.9900 . ? C5' H5'1 0.9800 . ? C5' H5'2 0.9800 . ? C5' H5'3 0.9800 . ? P1 Cu1 2.2074(6) . ? P2 Cu1 2.2504(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 O1 C1 O2 123.6(2) . . ? O1 C1 C2 121.0(2) . . ? O2 C1 C2 115.4(2) . . ? O1 C1 Cu1 64.71(12) . . ? O2 C1 Cu1 59.35(11) . . ? C2 C1 Cu1 170.75(16) . . ? O3 C2 C1 115.7(2) . . ? O3 C2 H2A 108.4 . . ? C1 C2 H2A 108.4 . . ? O3 C2 H2B 108.4 . . ? C1 C2 H2B 108.4 . . ? H2A C2 H2B 107.4 . . ? O3 C3 C4 104.9(4) . . ? O3 C3 C4' 116.5(6) . . ? C4 C3 C4' 21.3(4) . . ? O3 C3 H3A 110.8 . . ? C4 C3 H3A 110.8 . . ? C4' C3 H3A 118.1 . . ? O3 C3 H3B 110.8 . . ? C4 C3 H3B 110.8 . . ? C4' C3 H3B 89.6 . . ? H3A C3 H3B 108.8 . . ? C7 C6 C11 119.7(2) . . ? C7 C6 P1 117.74(16) . . ? C11 C6 P1 122.55(16) . . ? C6 C7 C8 120.2(2) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C9 C8 C7 120.1(2) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 119.9(2) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C10 C11 120.4(2) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C6 119.7(2) . . ? C10 C11 H11 120.2 . . ? C6 C11 H11 120.2 . . ? C17 C12 C13 119.3(2) . . ? C17 C12 P1 123.74(16) . . ? C13 C12 P1 116.80(16) . . ? C14 C13 C12 120.5(2) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C15 C14 C13 119.9(2) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C16 C15 C14 120.3(2) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 119.8(2) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C12 C17 C16 120.2(2) . . ? C12 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C23 C18 C19 119.0(2) . . ? C23 C18 P1 117.79(16) . . ? C19 C18 P1 123.05(17) . . ? C20 C19 C18 120.1(2) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C21 C20 C19 120.5(2) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 119.8(2) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 C23 120.0(2) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C18 120.6(2) . . ? C22 C23 H23 119.7 . . ? C18 C23 H23 119.7 . . ? C29 C24 C25 118.8(2) . . ? C29 C24 P2 125.42(16) . . ? C25 C24 P2 115.77(16) . . ? C26 C25 C24 120.6(2) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C27 C26 C25 120.4(2) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C26 C27 C28 119.8(2) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C27 C28 C29 120.0(2) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C28 C29 C24 120.5(2) . . ? C28 C29 H29 119.8 . . ? C24 C29 H29 119.8 . . ? C35 C30 C31 118.95(19) . . ? C35 C30 P2 122.64(16) . . ? C31 C30 P2 118.35(16) . . ? C32 C31 C30 120.5(2) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C33 C32 C31 119.9(2) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 120.0(2) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 120.4(2) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C30 120.2(2) . . ? C34 C35 H35 119.9 . . ? C30 C35 H35 119.9 . . ? C37 C36 C41 119.23(19) . . ? C37 C36 P2 117.01(15) . . ? C41 C36 P2 123.60(16) . . ? C36 C37 C38 120.24(19) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C39 C38 C37 120.3(2) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C38 C39 C40 119.7(2) . . ? C38 C39 H39 120.1 . . ? C40 C39 H39 120.1 . . ? C41 C40 C39 120.1(2) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C36 120.5(2) . . ? C40 C41 H41 119.8 . . ? C36 C41 H41 119.8 . . ? C1 O1 Cu1 85.23(13) . . ? C1 O2 Cu1 90.27(13) . . ? C2 O3 C3 112.76(18) . . ? C5 O4 C4 106.4(6) . . ? O4 C4 C3 112.0(4) . . ? O4 C4 H4A 109.2 . . ? C3 C4 H4A 109.2 . . ? O4 C4 H4B 109.2 . . ? C3 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? O4 C5 H5A 109.5 . . ? O4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C5' O4' C4' 141.5(9) . . ? O4' C4' C3 109.3(7) . . ? O4' C4' H4'1 109.8 . . ? C3 C4' H4'1 109.8 . . ? O4' C4' H4'2 109.8 . . ? C3 C4' H4'2 109.8 . . ? H4'1 C4' H4'2 108.3 . . ? O4' C5' H5'1 109.5 . . ? O4' C5' H5'2 109.5 . . ? H5'1 C5' H5'2 109.5 . . ? O4' C5' H5'3 109.5 . . ? H5'1 C5' H5'3 109.5 . . ? H5'2 C5' H5'3 109.5 . . ? C18 P1 C6 103.98(9) . . ? C18 P1 C12 105.09(9) . . ? C6 P1 C12 103.41(9) . . ? C18 P1 Cu1 115.97(7) . . ? C6 P1 Cu1 116.29(7) . . ? C12 P1 Cu1 110.77(7) . . ? C24 P2 C30 103.29(9) . . ? C24 P2 C36 108.95(9) . . ? C30 P2 C36 101.39(9) . . ? C24 P2 Cu1 115.45(7) . . ? C30 P2 Cu1 114.01(7) . . ? C36 P2 Cu1 112.47(7) . . ? O2 Cu1 P1 116.05(5) . . ? O2 Cu1 P2 102.23(5) . . ? P1 Cu1 P2 132.75(2) . . ? O2 Cu1 O1 60.30(6) . . ? P1 Cu1 O1 120.06(4) . . ? P2 Cu1 O1 102.19(4) . . ? O2 Cu1 C1 30.38(7) . . ? P1 Cu1 C1 125.09(5) . . ? P2 Cu1 C1 101.99(5) . . ? O1 Cu1 C1 30.06(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 O3 -1.6(3) . . . . ? O2 C1 C2 O3 178.95(19) . . . . ? Cu1 C1 C2 O3 -127.7(10) . . . . ? C11 C6 C7 C8 1.1(3) . . . . ? P1 C6 C7 C8 -176.77(16) . . . . ? C6 C7 C8 C9 -0.3(3) . . . . ? C7 C8 C9 C10 -0.8(3) . . . . ? C8 C9 C10 C11 1.1(3) . . . . ? C9 C10 C11 C6 -0.3(3) . . . . ? C7 C6 C11 C10 -0.8(3) . . . . ? P1 C6 C11 C10 176.99(16) . . . . ? C17 C12 C13 C14 0.5(3) . . . . ? P1 C12 C13 C14 176.09(17) . . . . ? C12 C13 C14 C15 -1.7(3) . . . . ? C13 C14 C15 C16 2.2(4) . . . . ? C14 C15 C16 C17 -1.3(4) . . . . ? C13 C12 C17 C16 0.4(3) . . . . ? P1 C12 C17 C16 -174.92(17) . . . . ? C15 C16 C17 C12 0.0(4) . . . . ? C23 C18 C19 C20 0.9(3) . . . . ? P1 C18 C19 C20 -174.56(18) . . . . ? C18 C19 C20 C21 0.3(4) . . . . ? C19 C20 C21 C22 -1.6(4) . . . . ? C20 C21 C22 C23 1.8(4) . . . . ? C21 C22 C23 C18 -0.6(4) . . . . ? C19 C18 C23 C22 -0.7(3) . . . . ? P1 C18 C23 C22 174.96(18) . . . . ? C29 C24 C25 C26 0.5(3) . . . . ? P2 C24 C25 C26 -177.87(19) . . . . ? C24 C25 C26 C27 -0.6(4) . . . . ? C25 C26 C27 C28 0.8(4) . . . . ? C26 C27 C28 C29 -0.9(4) . . . . ? C27 C28 C29 C24 0.8(3) . . . . ? C25 C24 C29 C28 -0.6(3) . . . . ? P2 C24 C29 C28 177.60(17) . . . . ? C35 C30 C31 C32 -0.2(3) . . . . ? P2 C30 C31 C32 177.09(17) . . . . ? C30 C31 C32 C33 0.1(3) . . . . ? C31 C32 C33 C34 0.3(3) . . . . ? C32 C33 C34 C35 -0.6(3) . . . . ? C33 C34 C35 C30 0.5(3) . . . . ? C31 C30 C35 C34 -0.1(3) . . . . ? P2 C30 C35 C34 -177.29(17) . . . . ? C41 C36 C37 C38 -0.1(3) . . . . ? P2 C36 C37 C38 175.47(16) . . . . ? C36 C37 C38 C39 1.5(3) . . . . ? C37 C38 C39 C40 -1.1(3) . . . . ? C38 C39 C40 C41 -0.7(3) . . . . ? C39 C40 C41 C36 2.2(3) . . . . ? C37 C36 C41 C40 -1.8(3) . . . . ? P2 C36 C41 C40 -177.01(16) . . . . ? O2 C1 O1 Cu1 7.7(2) . . . . ? C2 C1 O1 Cu1 -171.74(19) . . . . ? O1 C1 O2 Cu1 -8.1(2) . . . . ? C2 C1 O2 Cu1 171.38(17) . . . . ? C1 C2 O3 C3 78.5(3) . . . . ? C4 C3 O3 C2 -179.8(3) . . . . ? C4' C3 O3 C2 -160.7(5) . . . . ? C5 O4 C4 C3 134.6(6) . . . . ? O3 C3 C4 O4 -64.2(5) . . . . ? C4' C3 C4 O4 170(2) . . . . ? C5' O4' C4' C3 97.0(16) . . . . ? O3 C3 C4' O4' -78.9(9) . . . . ? C4 C3 C4' O4' -18.0(13) . . . . ? C23 C18 P1 C6 -170.07(17) . . . . ? C19 C18 P1 C6 5.4(2) . . . . ? C23 C18 P1 C12 81.58(18) . . . . ? C19 C18 P1 C12 -102.94(19) . . . . ? C23 C18 P1 Cu1 -41.10(19) . . . . ? C19 C18 P1 Cu1 134.38(17) . . . . ? C7 C6 P1 C18 96.36(17) . . . . ? C11 C6 P1 C18 -81.45(18) . . . . ? C7 C6 P1 C12 -154.05(16) . . . . ? C11 C6 P1 C12 28.14(19) . . . . ? C7 C6 P1 Cu1 -32.42(18) . . . . ? C11 C6 P1 Cu1 149.76(15) . . . . ? C17 C12 P1 C18 -10.0(2) . . . . ? C13 C12 P1 C18 174.62(16) . . . . ? C17 C12 P1 C6 -118.72(18) . . . . ? C13 C12 P1 C6 65.86(17) . . . . ? C17 C12 P1 Cu1 116.02(17) . . . . ? C13 C12 P1 Cu1 -59.41(17) . . . . ? C29 C24 P2 C30 -71.4(2) . . . . ? C25 C24 P2 C30 106.82(17) . . . . ? C29 C24 P2 C36 35.8(2) . . . . ? C25 C24 P2 C36 -145.99(16) . . . . ? C29 C24 P2 Cu1 163.47(16) . . . . ? C25 C24 P2 Cu1 -18.32(18) . . . . ? C35 C30 P2 C24 -17.0(2) . . . . ? C31 C30 P2 C24 165.84(17) . . . . ? C35 C30 P2 C36 -129.83(18) . . . . ? C31 C30 P2 C36 53.00(19) . . . . ? C35 C30 P2 Cu1 109.06(17) . . . . ? C31 C30 P2 Cu1 -68.10(18) . . . . ? C37 C36 P2 C24 121.60(16) . . . . ? C41 C36 P2 C24 -63.07(19) . . . . ? C37 C36 P2 C30 -129.91(16) . . . . ? C41 C36 P2 C30 45.43(19) . . . . ? C37 C36 P2 Cu1 -7.73(18) . . . . ? C41 C36 P2 Cu1 167.60(15) . . . . ? C1 O2 Cu1 P1 115.57(12) . . . . ? C1 O2 Cu1 P2 -92.91(12) . . . . ? C1 O2 Cu1 O1 4.28(12) . . . . ? C18 P1 Cu1 O2 -161.55(9) . . . . ? C6 P1 Cu1 O2 -38.83(9) . . . . ? C12 P1 Cu1 O2 78.81(9) . . . . ? C18 P1 Cu1 P2 57.84(8) . . . . ? C6 P1 Cu1 P2 -179.45(7) . . . . ? C12 P1 Cu1 P2 -61.80(8) . . . . ? C18 P1 Cu1 O1 -92.30(9) . . . . ? C6 P1 Cu1 O1 30.41(9) . . . . ? C12 P1 Cu1 O1 148.06(9) . . . . ? C18 P1 Cu1 C1 -127.67(10) . . . . ? C6 P1 Cu1 C1 -4.95(10) . . . . ? C12 P1 Cu1 C1 112.69(10) . . . . ? C24 P2 Cu1 O2 151.46(8) . . . . ? C30 P2 Cu1 O2 32.07(9) . . . . ? C36 P2 Cu1 O2 -82.65(8) . . . . ? C24 P2 Cu1 P1 -64.23(8) . . . . ? C30 P2 Cu1 P1 176.38(8) . . . . ? C36 P2 Cu1 P1 61.66(8) . . . . ? C24 P2 Cu1 O1 89.62(8) . . . . ? C30 P2 Cu1 O1 -29.78(9) . . . . ? C36 P2 Cu1 O1 -144.50(8) . . . . ? C24 P2 Cu1 C1 120.38(9) . . . . ? C30 P2 Cu1 C1 0.98(10) . . . . ? C36 P2 Cu1 C1 -113.74(9) . . . . ? C1 O1 Cu1 O2 -4.32(12) . . . . ? C1 O1 Cu1 P1 -109.03(12) . . . . ? C1 O1 Cu1 P2 92.93(12) . . . . ? O1 C1 Cu1 O2 172.6(2) . . . . ? C2 C1 Cu1 O2 -57.4(11) . . . . ? O1 C1 Cu1 P1 90.47(13) . . . . ? O2 C1 Cu1 P1 -82.10(13) . . . . ? C2 C1 Cu1 P1 -139.5(11) . . . . ? O1 C1 Cu1 P2 -93.66(12) . . . . ? O2 C1 Cu1 P2 93.77(12) . . . . ? C2 C1 Cu1 P2 36.3(11) . . . . ? O2 C1 Cu1 O1 -172.6(2) . . . . ? C2 C1 Cu1 O1 130.0(11) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 62.94 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.400 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.062 _database_code_depnum_ccdc_archive 'CCDC 933501'