# Electronic Supplementary Material (ESI) for Chemical Communications # 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_1np _database_code_depnum_ccdc_archive 'CCDC 909973' #TrackingRef '15265_web_deposit_cif_file_0_AndreaIenco_1352302535.totale_ccdc_deposit.cif' _audit_creation_date 2012-11-07T12:46:09-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H36 Cu3 N6 O14 P4' _chemical_formula_sum 'C32 H36 Cu3 N6 O14 P4' _chemical_formula_weight 1043.17 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4686(9) _cell_length_b 11.8434(9) _cell_length_c 12.3923(10) _cell_angle_alpha 117.656(9) _cell_angle_beta 94.288(8) _cell_angle_gamma 97.946(7) _cell_volume 1203.70(18) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4019 _cell_measurement_theta_min 4.2702 _cell_measurement_theta_max 72.4615 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description parallelepiped _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 529 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.48664 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 8.1241 _diffrn_orient_matrix_ub_11 -0.0679099 _diffrn_orient_matrix_ub_12 0.0051738 _diffrn_orient_matrix_ub_13 -0.1141414 _diffrn_orient_matrix_ub_21 0.0220964 _diffrn_orient_matrix_ub_22 0.1491096 _diffrn_orient_matrix_ub_23 0.075811 _diffrn_orient_matrix_ub_31 0.1502718 _diffrn_orient_matrix_ub_32 0.0128753 _diffrn_orient_matrix_ub_33 -0.0378065 _diffrn_measurement_device_type 'Xcalibur, Onyx' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0728 _diffrn_reflns_av_unetI/netI 0.0636 _diffrn_reflns_number 15935 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.27 _diffrn_reflns_theta_max 72.61 _diffrn_reflns_theta_full 72.61 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 4723 _reflns_number_gt 3181 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1158P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4723 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0865 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1916 _refine_ls_wR_factor_gt 0.164 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.769 _refine_diff_density_min -0.887 _refine_diff_density_rms 0.112 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.022 0.081 0.081 339 98 ' ' _platon_squeeze_details ; ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5 0.5 0 0.0374(3) Uani 1 2 d S . . Cu2 Cu 0.84459(7) 0.27679(7) -0.02807(6) 0.0361(2) Uani 1 1 d . . . P1 P 0.60581(12) 0.32713(12) 0.11671(11) 0.0329(3) Uani 1 1 d . . . P2 P 1.14399(13) 0.43089(14) 0.06996(11) 0.0388(3) Uani 1 1 d . . . O1 O 0.6585(3) 0.2256(3) 0.0067(3) 0.0372(8) Uani 1 1 d . . . O2 O 0.4918(3) 0.3850(3) 0.0753(3) 0.0341(8) Uani 1 1 d . . . O3 O 0.5504(4) 0.2747(4) 0.1973(3) 0.0430(9) Uani 1 1 d . . . O4 O 1.0423(3) 0.3227(4) -0.0438(3) 0.0422(9) Uani 1 1 d . . . O5 O 1.2374(4) 0.5280(4) 0.0486(3) 0.0444(10) Uani 1 1 d . . . O6 O 1.2364(3) 0.3681(4) 0.1311(3) 0.0469(10) Uani 1 1 d . . . O7 O 0.9393(16) 0.0854(15) -0.0337(13) 0.222(6) Uani 1 1 d . . . N1 N 0.5621(4) 0.6571(4) 0.1709(4) 0.0366(9) Uani 1 1 d . . . N2 N 0.7833(4) 0.1550(4) -0.2117(4) 0.0368(10) Uani 1 1 d . . . N3 N 0.8990(4) 0.4052(4) 0.1625(3) 0.0330(9) Uani 1 1 d . . . C1 C 0.7669(5) 0.4577(5) 0.1960(4) 0.0362(11) Uani 1 1 d . . . H1A H 0.7619 0.5264 0.1724 0.043 Uiso 1 1 calc R . . H1B H 0.7697 0.4971 0.2864 0.043 Uiso 1 1 calc R . . C2 C 1.0220(5) 0.5050(5) 0.1767(4) 0.0401(12) Uani 1 1 d . . . H2A H 1.0743 0.5489 0.2624 0.048 Uiso 1 1 calc R . . H2B H 0.9859 0.5712 0.1607 0.048 Uiso 1 1 calc R . . C3 C 0.9358(6) 0.3338(6) 0.2321(5) 0.0416(12) Uani 1 1 d . . . H3A H 1.0198 0.2936 0.2026 0.05 Uiso 1 1 calc R . . H3B H 0.8532 0.263 0.2133 0.05 Uiso 1 1 calc R . . C4 C 0.9706(5) 0.4202(6) 0.3702(5) 0.0424(12) Uani 1 1 d . . . C5 C 0.8604(6) 0.4324(7) 0.4425(5) 0.0482(14) Uani 1 1 d . . . H5 H 0.7648 0.3858 0.4043 0.058 Uiso 1 1 calc R . . C6 C 1.1094(5) 0.4875(6) 0.4298(5) 0.0470(14) Uani 1 1 d . . . H6 H 1.1857 0.4787 0.3827 0.056 Uiso 1 1 calc R . . C10 C 0.5053(6) 0.6534(5) 0.2662(5) 0.0400(12) Uani 1 1 d . . . H10 H 0.4332 0.5807 0.25 0.048 Uiso 1 1 calc R . . C11 C 0.5485(6) 0.7519(5) 0.3869(5) 0.0426(12) Uani 1 1 d . . . H11 H 0.5081 0.7457 0.4523 0.051 Uiso 1 1 calc R . . C12 C 0.6518(5) 0.8600(5) 0.4111(4) 0.0374(11) Uani 1 1 d . . . C13 C 0.7075(6) 0.8629(5) 0.3130(5) 0.0405(12) Uani 1 1 d . . . H13 H 0.7788 0.9349 0.3265 0.049 Uiso 1 1 calc R . . C14 C 0.6597(5) 0.7603(5) 0.1938(4) 0.0365(11) Uani 1 1 d . . . H14 H 0.6982 0.7646 0.1269 0.044 Uiso 1 1 calc R . . C15 C 0.6958(6) 0.9675(5) 0.5410(4) 0.0394(12) Uani 1 1 d . . . C16 C 0.8299(6) 1.0520(5) 0.5829(5) 0.0458(14) Uani 1 1 d . . . H16 H 0.8949 1.0469 0.5268 0.055 Uiso 1 1 calc R . . C17 C 0.8674(6) 1.1427(5) 0.7058(5) 0.0435(13) Uani 1 1 d . . . H17 H 0.9591 1.1992 0.7322 0.052 Uiso 1 1 calc R . . C18 C 0.6511(6) 1.0804(6) 0.7471(5) 0.0453(13) Uani 1 1 d . . . H18 H 0.5854 1.0933 0.8041 0.054 Uiso 1 1 calc R . . C19 C 0.6055(6) 0.9861(6) 0.6267(5) 0.0450(13) Uani 1 1 d . . . H19 H 0.5114 0.9339 0.6028 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0400(6) 0.0369(6) 0.0223(5) 0.0061(4) -0.0069(4) 0.0043(4) Cu2 0.0282(4) 0.0442(4) 0.0206(4) 0.0062(3) 0.0012(3) -0.0034(3) P1 0.0247(6) 0.0411(7) 0.0259(6) 0.0112(5) 0.0021(4) 0.0041(5) P2 0.0232(6) 0.0567(8) 0.0234(6) 0.0103(6) 0.0005(5) 0.0032(5) O1 0.0250(16) 0.0444(19) 0.0305(18) 0.0092(15) 0.0051(13) 0.0041(14) O2 0.0190(14) 0.0462(19) 0.0286(17) 0.0134(15) 0.0003(12) -0.0011(13) O3 0.0365(19) 0.059(2) 0.0371(19) 0.0264(18) 0.0090(15) 0.0053(17) O4 0.0228(15) 0.061(2) 0.0265(17) 0.0099(16) -0.0013(13) 0.0038(16) O5 0.0246(16) 0.069(2) 0.0240(17) 0.0156(17) -0.0008(13) -0.0088(16) O6 0.0188(15) 0.074(3) 0.039(2) 0.0219(19) -0.0001(14) 0.0056(16) O7 0.244(15) 0.256(16) 0.222(14) 0.135(13) 0.091(12) 0.116(14) N1 0.036(2) 0.039(2) 0.0204(19) 0.0027(17) -0.0015(16) 0.0077(18) N2 0.0238(19) 0.041(2) 0.026(2) 0.0018(17) 0.0022(15) 0.0001(17) N3 0.031(2) 0.046(2) 0.0219(19) 0.0155(17) 0.0055(15) 0.0114(17) C1 0.028(2) 0.047(3) 0.025(2) 0.010(2) -0.0001(18) 0.010(2) C2 0.031(2) 0.051(3) 0.024(2) 0.010(2) -0.0055(19) -0.001(2) C3 0.032(2) 0.066(3) 0.036(3) 0.030(3) 0.012(2) 0.014(2) C4 0.030(2) 0.073(4) 0.028(2) 0.025(3) 0.009(2) 0.016(2) C5 0.027(2) 0.086(4) 0.034(3) 0.030(3) 0.005(2) 0.015(3) C6 0.024(2) 0.085(4) 0.030(3) 0.025(3) 0.0046(19) 0.015(3) C10 0.038(3) 0.038(3) 0.032(3) 0.010(2) 0.000(2) 0.002(2) C11 0.037(3) 0.046(3) 0.030(3) 0.008(2) 0.005(2) 0.005(2) C12 0.032(2) 0.038(3) 0.028(2) 0.004(2) 0.0053(19) 0.002(2) C13 0.035(3) 0.039(3) 0.032(3) 0.007(2) 0.004(2) 0.002(2) C14 0.030(2) 0.044(3) 0.027(2) 0.012(2) 0.0059(19) 0.001(2) C15 0.037(3) 0.040(3) 0.024(2) 0.002(2) 0.002(2) 0.003(2) C16 0.040(3) 0.048(3) 0.029(3) 0.006(2) 0.005(2) -0.010(2) C17 0.040(3) 0.040(3) 0.036(3) 0.008(2) 0.011(2) -0.001(2) C18 0.035(3) 0.050(3) 0.036(3) 0.009(2) 0.002(2) 0.007(2) C19 0.033(3) 0.051(3) 0.032(3) 0.007(2) 0.000(2) 0.001(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.974(4) . ? Cu1 O2 1.974(4) 2_665 ? Cu1 N1 2.036(4) 2_665 ? Cu1 N1 2.036(4) . ? Cu2 O4 1.926(3) . ? Cu2 O1 1.929(3) . ? Cu2 N2 2.030(4) . ? Cu2 N3 2.103(4) . ? P1 O3 1.491(4) . ? P1 O1 1.516(4) . ? P1 O2 1.531(4) . ? P1 C1 1.843(5) . ? P2 O5 1.488(4) . ? P2 O4 1.528(3) . ? P2 O6 1.580(4) . ? P2 C2 1.813(6) . ? N1 C14 1.324(7) . ? N1 C10 1.350(7) . ? N2 C17 1.310(7) 1_544 ? N2 C18 1.337(7) 1_544 ? N3 C1 1.475(6) . ? N3 C2 1.476(7) . ? N3 C3 1.515(7) . ? C3 C4 1.510(7) . ? C4 C6 1.388(7) . ? C4 C5 1.405(7) . ? C5 C6 1.396(8) 2_766 ? C6 C5 1.396(8) 2_766 ? C10 C11 1.386(7) . ? C11 C12 1.392(7) . ? C12 C13 1.373(7) . ? C12 C15 1.496(7) . ? C13 C14 1.395(7) . ? C15 C19 1.370(8) . ? C15 C16 1.397(7) . ? C16 C17 1.376(7) . ? C17 N2 1.310(7) 1_566 ? C18 N2 1.337(7) 1_566 ? C18 C19 1.372(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 O2 Cu1 O2 180 . 2_665 ? O2 Cu1 N1 90.44(16) . 2_665 ? O2 Cu1 N1 89.56(16) 2_665 2_665 ? O2 Cu1 N1 89.56(16) . . ? O2 Cu1 N1 90.44(16) 2_665 . ? N1 Cu1 N1 179.9990(10) 2_665 . ? O4 Cu2 O1 171.37(17) . . ? O4 Cu2 N2 93.79(15) . . ? O1 Cu2 N2 91.70(15) . . ? O4 Cu2 N3 88.33(15) . . ? O1 Cu2 N3 86.37(14) . . ? N2 Cu2 N3 177.44(16) . . ? O3 P1 O1 112.0(2) . . ? O3 P1 O2 111.0(2) . . ? O1 P1 O2 111.0(2) . . ? O3 P1 C1 112.4(2) . . ? O1 P1 C1 103.4(2) . . ? O2 P1 C1 106.7(2) . . ? O5 P2 O4 115.4(2) . . ? O5 P2 O6 111.4(2) . . ? O4 P2 O6 109.1(2) . . ? O5 P2 C2 111.7(3) . . ? O4 P2 C2 103.2(2) . . ? O6 P2 C2 105.4(2) . . ? P1 O1 Cu2 116.98(19) . . ? P1 O2 Cu1 133.32(19) . . ? P2 O4 Cu2 118.4(2) . . ? C14 N1 C10 118.5(4) . . ? C14 N1 Cu1 123.2(3) . . ? C10 N1 Cu1 118.2(3) . . ? C17 N2 C18 116.9(4) 1_544 1_544 ? C17 N2 Cu2 123.6(3) 1_544 . ? C18 N2 Cu2 119.4(4) 1_544 . ? C1 N3 C2 112.8(4) . . ? C1 N3 C3 110.9(4) . . ? C2 N3 C3 112.2(4) . . ? C1 N3 Cu2 103.6(3) . . ? C2 N3 Cu2 105.9(3) . . ? C3 N3 Cu2 111.0(3) . . ? N3 C1 P1 110.2(3) . . ? N3 C2 P2 110.2(4) . . ? N3 C3 C4 113.5(5) . . ? C6 C4 C5 118.0(5) . . ? C6 C4 C3 122.3(5) . . ? C5 C4 C3 119.7(5) . . ? C6 C5 C4 120.3(5) 2_766 . ? C4 C6 C5 121.6(5) . 2_766 ? N1 C10 C11 122.2(5) . . ? C10 C11 C12 119.2(5) . . ? C13 C12 C11 117.8(5) . . ? C13 C12 C15 123.1(5) . . ? C11 C12 C15 119.1(5) . . ? C12 C13 C14 120.1(5) . . ? N1 C14 C13 122.1(5) . . ? C19 C15 C16 116.3(5) . . ? C19 C15 C12 120.8(5) . . ? C16 C15 C12 122.9(5) . . ? C17 C16 C15 119.8(5) . . ? N2 C17 C16 123.4(5) 1_566 . ? N2 C18 C19 123.4(5) 1_566 . ? C18 C19 C15 119.9(5) . . ? data_2np _database_code_depnum_ccdc_archive 'CCDC 909974' #TrackingRef '15265_web_deposit_cif_file_0_AndreaIenco_1352302535.totale_ccdc_deposit.cif' _audit_creation_date 2012-11-07T12:56:35-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H38 Cu3 N6 O12 P4' _chemical_formula_sum 'C30 H38 Cu3 N6 O12 P4' _chemical_formula_weight 989.16 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5516(5) _cell_length_b 12.9047(7) _cell_length_c 13.982(2) _cell_angle_alpha 75.544(7) _cell_angle_beta 89.628(7) _cell_angle_gamma 75.697(5) _cell_volume 1614.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3952 _cell_measurement_theta_min 4.2334 _cell_measurement_theta_max 61.9882 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.017 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 503 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.437 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.83577 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 8.1241 _diffrn_orient_matrix_ub_11 0.015845 _diffrn_orient_matrix_ub_12 -0.0250182 _diffrn_orient_matrix_ub_13 0.1136108 _diffrn_orient_matrix_ub_21 -0.1282248 _diffrn_orient_matrix_ub_22 0.1002422 _diffrn_orient_matrix_ub_23 -0.0020565 _diffrn_orient_matrix_ub_31 -0.1053957 _diffrn_orient_matrix_ub_32 -0.0746162 _diffrn_orient_matrix_ub_33 0.0089789 _diffrn_measurement_device_type 'Xcalibur, Onyx' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_unetI/netI 0.0846 _diffrn_reflns_number 9346 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.24 _diffrn_reflns_theta_max 62.07 _diffrn_reflns_theta_full 62.07 _diffrn_measured_fraction_theta_full 0.965 _diffrn_measured_fraction_theta_max 0.965 _reflns_number_total 4899 _reflns_number_gt 3413 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4899 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1324 _refine_ls_R_factor_gt 0.1101 _refine_ls_wR_factor_ref 0.2774 _refine_ls_wR_factor_gt 0.2669 _refine_ls_goodness_of_fit_ref 1.352 _refine_ls_restrained_S_all 1.352 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.908 _refine_diff_density_min -0.999 _refine_diff_density_rms 0.174 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.035 -0.026 0.500 822 105 ' ' #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0 0.5 0 0.0330(5) Uani 1 2 d S . . Cu2 Cu -0.32501(12) 0.33969(10) 0.13123(10) 0.0296(4) Uani 1 1 d . . . P1 P -0.0929(2) 0.41032(19) 0.21613(18) 0.0292(6) Uani 1 1 d . . . P2 P -0.6344(2) 0.46840(19) 0.10745(17) 0.0267(6) Uani 1 1 d . . . O1 O -0.1352(6) 0.3120(5) 0.1937(5) 0.0336(15) Uani 1 1 d . . . O2 O 0.0178(6) 0.4517(5) 0.1409(5) 0.0335(15) Uani 1 1 d . . . O3 O -0.0362(7) 0.3886(6) 0.3202(5) 0.0446(17) Uani 1 1 d . . . O4 O -0.5284(6) 0.3636(5) 0.0958(5) 0.0328(15) Uani 1 1 d . . . O5 O -0.7242(6) 0.4391(5) 0.2013(4) 0.0352(15) Uani 1 1 d . . . O6 O -0.7319(6) 0.5333(5) 0.0173(4) 0.0337(15) Uani 1 1 d . . . N1 N -0.3868(7) 0.4703(6) 0.1972(5) 0.0312(17) Uani 1 1 d . . . N2 N -0.0650(7) 0.6572(6) 0.0113(6) 0.0309(17) Uani 1 1 d . . . N3 N -0.2694(8) 0.1960(6) 0.0923(6) 0.0343(18) Uani 1 1 d . . . C1 C -0.5192(8) 0.5484(7) 0.1408(6) 0.0256(19) Uani 1 1 d . . . H1A H -0.492 0.5964 0.0803 0.031 Uiso 1 1 calc R . . H1B H -0.5716 0.5961 0.1819 0.031 Uiso 1 1 calc R . . C2 C -0.2599(8) 0.5192(7) 0.1885(7) 0.026(2) Uani 1 1 d . . . H2A H -0.2663 0.5664 0.2351 0.032 Uiso 1 1 calc R . . H2B H -0.2605 0.5661 0.1206 0.032 Uiso 1 1 calc R . . C3 C -0.4111(9) 0.4229(8) 0.3040(6) 0.035(2) Uani 1 1 d . . . H3A H -0.3226 0.366 0.3351 0.042 Uiso 1 1 calc R . . H3B H -0.491 0.386 0.3071 0.042 Uiso 1 1 calc R . . C4 C -0.4484(13) 0.5111(9) 0.3637(8) 0.051(3) Uani 1 1 d . . . H4A H -0.5358 0.5694 0.333 0.061 Uiso 1 1 calc R . . H4B H -0.3672 0.5461 0.3645 0.061 Uiso 1 1 calc R . . C5 C -0.4759(12) 0.4524(10) 0.4708(8) 0.053(3) Uani 1 1 d . . . H5A H -0.3868 0.3974 0.5032 0.064 Uiso 1 1 calc R . . H5B H -0.5533 0.4138 0.47 0.064 Uiso 1 1 calc R . . C7 C -0.1649(10) 0.7372(7) -0.0483(7) 0.033(2) Uani 1 1 d . . . H7 H -0.2072 0.7196 -0.1015 0.04 Uiso 1 1 calc R . . C8 C -0.2120(10) 0.8443(7) -0.0386(8) 0.040(2) Uani 1 1 d . . . H8 H -0.2852 0.8972 -0.0833 0.048 Uiso 1 1 calc R . . C9 C -0.1507(10) 0.8730(8) 0.0374(8) 0.038(2) Uani 1 1 d . . . C10 C -0.0455(10) 0.7893(7) 0.1016(8) 0.040(2) Uani 1 1 d . . . H10 H -0.0007 0.8044 0.1553 0.048 Uiso 1 1 calc R . . C11 C -0.0084(10) 0.6859(8) 0.0857(8) 0.042(2) Uani 1 1 d . . . H11 H 0.0623 0.6304 0.1304 0.05 Uiso 1 1 calc R . . C12 C -0.3579(11) 0.1651(8) 0.0362(8) 0.046(3) Uani 1 1 d . . . H12 H -0.4473 0.216 0.0098 0.055 Uiso 1 1 calc R . . C13 C -0.3247(11) 0.0627(8) 0.0153(7) 0.041(2) Uani 1 1 d . . . H13 H -0.3907 0.044 -0.0241 0.049 Uiso 1 1 calc R . . C14 C -0.1939(10) -0.0125(8) 0.0525(7) 0.038(2) Uani 1 1 d . . . C15 C -0.1027(10) 0.0221(8) 0.1053(9) 0.047(3) Uani 1 1 d . . . H15 H -0.0108 -0.0258 0.13 0.056 Uiso 1 1 calc R . . C16 C -0.1423(10) 0.1260(7) 0.1234(8) 0.039(2) Uani 1 1 d . . . H16 H -0.0755 0.1477 0.1594 0.047 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0292(10) 0.0246(10) 0.0484(12) -0.0172(9) 0.0162(8) -0.0052(8) Cu2 0.0164(7) 0.0270(7) 0.0505(9) -0.0180(6) 0.0045(5) -0.0067(5) P1 0.0198(11) 0.0320(13) 0.0418(14) -0.0143(10) 0.0088(10) -0.0130(10) P2 0.0121(10) 0.0344(13) 0.0390(14) -0.0154(10) 0.0072(9) -0.0098(9) O1 0.025(3) 0.031(3) 0.049(4) -0.015(3) 0.008(3) -0.011(3) O2 0.011(3) 0.024(3) 0.071(5) -0.022(3) 0.008(3) -0.004(2) O3 0.047(4) 0.051(4) 0.040(4) -0.009(3) 0.002(3) -0.023(4) O4 0.020(3) 0.027(3) 0.062(4) -0.023(3) 0.013(3) -0.013(3) O5 0.021(3) 0.051(4) 0.038(4) -0.012(3) 0.017(3) -0.017(3) O6 0.033(3) 0.033(4) 0.034(4) -0.011(3) 0.002(3) -0.004(3) N1 0.017(4) 0.046(5) 0.033(4) -0.013(4) 0.001(3) -0.010(3) N2 0.020(4) 0.033(4) 0.044(5) -0.012(4) 0.010(3) -0.012(3) N3 0.025(4) 0.021(4) 0.057(5) -0.016(4) 0.009(4) 0.000(3) C1 0.010(4) 0.028(5) 0.041(5) -0.013(4) 0.008(3) -0.004(3) C2 0.017(4) 0.026(5) 0.046(6) -0.019(4) 0.007(4) -0.015(4) C3 0.016(4) 0.055(6) 0.032(5) -0.012(5) -0.004(4) -0.006(4) C4 0.058(7) 0.061(7) 0.043(6) -0.028(5) 0.012(5) -0.017(6) C5 0.036(6) 0.084(9) 0.046(7) -0.031(6) 0.011(5) -0.012(6) C7 0.027(5) 0.026(5) 0.048(6) -0.012(4) 0.002(4) -0.006(4) C8 0.025(5) 0.019(5) 0.073(7) -0.012(5) 0.007(5) 0.002(4) C9 0.024(5) 0.036(6) 0.060(7) -0.023(5) 0.007(4) -0.008(4) C10 0.037(6) 0.020(5) 0.064(7) -0.018(5) 0.005(5) -0.004(4) C11 0.028(5) 0.032(6) 0.061(7) -0.016(5) 0.006(5) 0.005(4) C12 0.038(6) 0.022(5) 0.076(8) -0.017(5) 0.001(5) 0.001(4) C13 0.041(6) 0.039(6) 0.050(6) -0.024(5) -0.004(5) -0.009(5) C14 0.025(5) 0.040(6) 0.052(6) -0.025(5) 0.002(4) -0.001(4) C15 0.016(5) 0.033(6) 0.097(9) -0.024(6) 0.005(5) -0.008(4) C16 0.022(5) 0.029(5) 0.077(7) -0.025(5) 0.006(5) -0.014(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.907(7) 2_565 ? Cu1 O2 1.907(7) . ? Cu1 N2 2.016(7) 2_565 ? Cu1 N2 2.016(7) . ? Cu2 O1 1.929(6) . ? Cu2 O4 1.938(6) . ? Cu2 N3 2.008(7) . ? Cu2 N1 2.077(8) . ? P1 O3 1.490(7) . ? P1 O1 1.525(6) . ? P1 O2 1.579(6) . ? P1 C2 1.816(8) . ? P2 O6 1.503(6) . ? P2 O4 1.520(6) . ? P2 O5 1.580(6) . ? P2 C1 1.817(8) . ? N1 C2 1.490(10) . ? N1 C1 1.491(11) . ? N1 C3 1.506(11) . ? N2 C7 1.328(11) . ? N2 C11 1.346(12) . ? N3 C16 1.322(11) . ? N3 C12 1.350(13) . ? C3 C4 1.546(13) . ? C4 C5 1.553(15) . ? C5 C5 1.61(2) 2_466 ? C7 C8 1.385(12) . ? C8 C9 1.386(14) . ? C9 C10 1.405(13) . ? C9 C14 1.500(13) 1_565 ? C10 C11 1.367(13) . ? C12 C13 1.384(13) . ? C13 C14 1.389(13) . ? C14 C15 1.367(13) . ? C14 C9 1.500(13) 1_545 ? C15 C16 1.386(13) . ? 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 Cu1 O2 180.0(3) 2_565 . ? O2 Cu1 N2 88.7(3) 2_565 2_565 ? O2 Cu1 N2 91.3(3) . 2_565 ? O2 Cu1 N2 91.3(3) 2_565 . ? O2 Cu1 N2 88.7(3) . . ? N2 Cu1 N2 179.9980(10) 2_565 . ? O1 Cu2 O4 168.3(3) . . ? O1 Cu2 N3 91.3(3) . . ? O4 Cu2 N3 93.1(3) . . ? O1 Cu2 N1 86.7(3) . . ? O4 Cu2 N1 87.0(2) . . ? N3 Cu2 N1 169.4(3) . . ? O3 P1 O1 113.5(4) . . ? O3 P1 O2 110.8(4) . . ? O1 P1 O2 111.1(3) . . ? O3 P1 C2 111.7(4) . . ? O1 P1 C2 103.4(3) . . ? O2 P1 C2 105.9(4) . . ? O6 P2 O4 115.0(4) . . ? O6 P2 O5 111.5(3) . . ? O4 P2 O5 109.4(4) . . ? O6 P2 C1 111.4(4) . . ? O4 P2 C1 103.9(3) . . ? O5 P2 C1 105.0(4) . . ? P1 O1 Cu2 117.1(4) . . ? P1 O2 Cu1 129.8(4) . . ? P2 O4 Cu2 118.9(3) . . ? C2 N1 C1 112.7(7) . . ? C2 N1 C3 110.9(7) . . ? C1 N1 C3 113.2(6) . . ? C2 N1 Cu2 104.1(5) . . ? C1 N1 Cu2 107.7(5) . . ? C3 N1 Cu2 107.8(5) . . ? C7 N2 C11 115.5(8) . . ? C7 N2 Cu1 125.1(6) . . ? C11 N2 Cu1 119.4(6) . . ? C16 N3 C12 117.1(8) . . ? C16 N3 Cu2 120.0(6) . . ? C12 N3 Cu2 122.9(6) . . ? N1 C1 P2 108.5(6) . . ? N1 C2 P1 110.2(6) . . ? N1 C3 C4 113.1(8) . . ? C3 C4 C5 107.8(9) . . ? C4 C5 C5 106.7(12) . 2_466 ? N2 C7 C8 124.8(9) . . ? C7 C8 C9 118.9(9) . . ? C8 C9 C10 117.0(9) . . ? C8 C9 C14 122.4(9) . 1_565 ? C10 C9 C14 120.5(9) . 1_565 ? C11 C10 C9 119.1(10) . . ? N2 C11 C10 124.6(10) . . ? N3 C12 C13 123.1(9) . . ? C12 C13 C14 119.3(9) . . ? C15 C14 C13 116.8(9) . . ? C15 C14 C9 120.0(9) . 1_545 ? C13 C14 C9 123.3(8) . 1_545 ? C14 C15 C16 121.1(9) . . ? N3 C16 C15 122.4(9) . . ? data_3lp _database_code_depnum_ccdc_archive 'CCDC 909975' #TrackingRef '15265_web_deposit_cif_file_0_AndreaIenco_1352302535.totale_ccdc_deposit.cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H40 Cu3 N6 O12 P4' _chemical_formula_sum 'C34 H40 Cu3 N6 O12 P4' _chemical_formula_weight 1039.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.9010(4) _cell_length_b 9.5384(3) _cell_length_c 26.6923(12) _cell_angle_alpha 90.00 _cell_angle_beta 96.326(3) _cell_angle_gamma 90.00 _cell_volume 3517.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 1937 _cell_measurement_theta_min 3.33 _cell_measurement_theta_max 53.64 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_max 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.981 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1058 _exptl_absorpt_coefficient_mu 1.029 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8345 _exptl_absorpt_correction_T_max 0.9137 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6431 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 21.93 _reflns_number_total 3816 _reflns_number_gt 2943 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Single crystal of 3 was collected at 200 K. Due to the small crystal, the diffraction was weak and the resolution was low. We have tried our best to obtain the best completeness (upto ~89.4%). PLATON reported alert_A on high Ueq on atoms C7,C9, C21, and C23 is due to the disorders. We cannot find the best model to fit into the data to avoid these errors. However, the structure here confirmed that these peaks are carbons ( based on the structure of the ligand) and it is belong to the H8L1. Squeeze found ~ 447 electons that can be accounted to disorder solvents molecules. ; _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^)+(0.1622P)^2^+2.1951P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3816 _refine_ls_number_parameters 258 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0774 _refine_ls_wR_factor_ref 0.2392 _refine_ls_wR_factor_gt 0.2284 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.002 -0.038 -0.002 1810 447 ' ' _platon_squeeze_details ; ; 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 C23 C 0.5145(14) 0.7194(13) 0.1708(6) 0.170(10) Uani 1 1 d . . . H23 H 0.4656 0.7863 0.1669 0.204 Uiso 1 1 calc R . . C21 C 0.5788(16) 0.7289(16) 0.2137(7) 0.190(11) Uani 1 1 d . . . H21 H 0.5742 0.8053 0.2349 0.228 Uiso 1 1 calc R . . C9 C 0.6518(15) 0.552(2) 0.1889(7) 0.171(8) Uiso 1 1 d D . . H9 H 0.6987 0.4819 0.1932 0.205 Uiso 1 1 calc R . . C22 C 0.5938(10) 0.5592(18) 0.1445(7) 0.132(6) Uiso 1 1 d D . . H22 H 0.6140 0.5090 0.1177 0.159 Uiso 1 1 calc R . . Cu1 Cu 0.42168(6) 0.62301(9) 0.07446(4) 0.0420(4) Uani 1 1 d . . . Cu2 Cu 0.5000 1.0000 0.0000 0.0460(5) Uani 1 2 d S . . P3 P 0.40144(12) 0.35908(16) 0.01348(8) 0.0302(6) Uani 1 1 d . . . P4 P 0.31482(12) 0.88331(17) 0.04526(8) 0.0282(5) Uani 1 1 d . . . N4 N 0.5153(4) 0.6272(6) 0.1356(2) 0.0358(15) Uani 1 1 d D . . O15 O 0.3157(3) 0.2596(5) 0.0242(2) 0.0517(16) Uani 1 1 d . . . O14 O 0.4705(3) 0.2850(5) -0.0161(2) 0.0362(13) Uani 1 1 d . . . O17 O 0.4464(3) 0.4237(5) 0.0629(2) 0.0368(13) Uani 1 1 d . . . O11 O 0.2187(4) 0.9341(6) 0.0565(2) 0.0485(15) Uani 1 1 d . . . N3 N 0.3126(4) 0.6102(5) 0.0163(2) 0.0289(14) Uani 1 1 d . . . O12 O 0.3727(3) 1.0048(4) 0.02737(19) 0.0371(13) Uani 1 1 d . . . N1 N 0.9286(5) 0.5167(6) 0.4304(2) 0.0356(15) Uani 1 1 d . . . O13 O 0.3710(3) 0.8063(4) 0.08944(18) 0.0303(11) Uani 1 1 d . . . C11 C 0.2193(4) 0.5667(7) 0.0372(3) 0.0349(18) Uani 1 1 d . . . H11A H 0.2028 0.6365 0.0612 0.042 Uiso 1 1 calc R . . H11B H 0.2297 0.4783 0.0549 0.042 Uiso 1 1 calc R . . C14 C 0.3052(5) 0.7534(6) -0.0057(3) 0.0308(17) Uani 1 1 d . . . H14A H 0.2437 0.7640 -0.0264 0.037 Uiso 1 1 calc R . . H14B H 0.3567 0.7679 -0.0269 0.037 Uiso 1 1 calc R . . C16 C 0.3443(5) 0.5061(7) -0.0207(3) 0.0319(17) Uani 1 1 d . . . C13 C 0.0426(4) 0.5074(8) 0.0199(3) 0.045(2) Uani 1 1 d . . . H13A H 0.0542 0.4190 0.0375 0.054 Uiso 1 1 calc R . . H13B H 0.0284 0.5778 0.0443 0.054 Uiso 1 1 calc R . . C12 C 0.1337(5) 0.5506(10) -0.0046(4) 0.060(3) Uani 1 1 d . . . H12A H 0.1222 0.6386 -0.0224 0.072 Uiso 1 1 calc R . . H12B H 0.1488 0.4797 -0.0286 0.072 Uiso 1 1 calc R . . C8 C 0.6434(8) 0.6392(14) 0.2254(4) 0.083(4) Uani 1 1 d D . . C6 C 0.7803(11) 0.5389(16) 0.2761(6) 0.121(5) Uani 1 1 d . . . H6A H 0.8267 0.5541 0.2521 0.145 Uiso 1 1 calc R . . H6B H 0.7456 0.4522 0.2680 0.145 Uiso 1 1 calc R . . C1 C 0.9623(6) 0.6000(9) 0.3935(3) 0.053(2) Uani 1 1 d . . . H1 H 1.0184 0.6516 0.4022 0.063 Uiso 1 1 calc R . . C7 C 0.7167(13) 0.6522(17) 0.2770(7) 0.153(8) Uani 1 1 d . . . H7A H 0.7517 0.7403 0.2778 0.184 Uiso 1 1 calc R . . H7B H 0.6813 0.6472 0.3063 0.184 Uiso 1 1 calc R . . C3 C 0.8333(10) 0.5374(15) 0.3341(5) 0.100(4) Uani 1 1 d . . . C5 C 0.8490(7) 0.4526(10) 0.4179(4) 0.060(3) Uani 1 1 d . . . H5 H 0.8248 0.3945 0.4415 0.072 Uiso 1 1 calc R . . C2 C 0.9208(9) 0.6108(13) 0.3478(4) 0.089(4) Uani 1 1 d . . . H2 H 0.9481 0.6659 0.3243 0.107 Uiso 1 1 calc R . . C4 C 0.7977(10) 0.4654(16) 0.3714(5) 0.108(5) Uani 1 1 d . . . H4 H 0.7371 0.4235 0.3653 0.130 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C23 0.26(2) 0.056(8) 0.156(14) -0.017(9) -0.165(15) 0.041(10) C21 0.29(2) 0.068(9) 0.172(17) -0.032(10) -0.145(18) 0.059(13) Cu1 0.0349(6) 0.0301(6) 0.0605(8) 0.0003(5) 0.0032(5) 0.0066(4) Cu2 0.0483(9) 0.0426(9) 0.0470(10) -0.0032(7) 0.0047(7) -0.0168(6) P3 0.0217(9) 0.0092(9) 0.0621(14) -0.0024(8) 0.0146(9) -0.0025(7) P4 0.0263(10) 0.0110(9) 0.0470(13) 0.0028(8) 0.0023(9) 0.0009(7) N4 0.031(3) 0.035(4) 0.041(4) 0.008(3) 0.002(3) 0.014(3) O15 0.039(3) 0.015(3) 0.107(5) -0.006(3) 0.037(3) -0.012(2) O14 0.020(2) 0.022(3) 0.069(4) -0.010(2) 0.018(2) 0.0025(19) O17 0.032(2) 0.023(3) 0.057(4) 0.009(2) 0.010(2) 0.007(2) O11 0.039(3) 0.039(3) 0.069(4) 0.002(3) 0.012(3) 0.016(2) N3 0.015(3) 0.012(3) 0.060(4) -0.008(3) 0.004(3) -0.001(2) O12 0.042(3) 0.012(2) 0.057(4) -0.005(2) 0.004(3) -0.003(2) N1 0.049(4) 0.019(3) 0.038(4) -0.002(3) 0.001(3) -0.003(3) O13 0.032(2) 0.017(2) 0.042(3) 0.001(2) 0.004(2) -0.002(2) C11 0.019(3) 0.020(4) 0.066(5) 0.008(4) 0.008(3) 0.001(3) C14 0.027(3) 0.011(3) 0.052(5) 0.001(3) -0.005(3) -0.005(3) C16 0.025(3) 0.024(4) 0.047(5) -0.005(3) 0.006(3) -0.002(3) C13 0.016(3) 0.029(4) 0.090(7) 0.000(4) 0.011(4) 0.000(3) C12 0.023(4) 0.067(6) 0.093(8) -0.001(5) 0.014(4) -0.019(4) C8 0.064(6) 0.126(11) 0.051(6) 0.009(7) -0.026(5) 0.017(7) C6 0.128(12) 0.091(10) 0.138(14) -0.008(9) -0.008(10) 0.038(9) C1 0.055(5) 0.051(5) 0.048(6) 0.005(4) -0.009(5) -0.006(4) C7 0.170(16) 0.108(12) 0.160(16) 0.046(11) -0.075(13) -0.004(12) C3 0.124(11) 0.105(10) 0.059(8) 0.034(7) -0.035(7) -0.028(8) C5 0.088(7) 0.044(5) 0.049(6) 0.006(5) 0.009(5) 0.003(5) C2 0.094(8) 0.105(10) 0.062(8) 0.031(7) -0.026(7) -0.016(7) C4 0.115(10) 0.129(12) 0.068(8) 0.007(8) -0.051(8) -0.037(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C23 N4 1.289(16) . ? C23 C21 1.374(17) . ? C21 C8 1.255(17) . ? C9 C8 1.298(15) . ? C9 C22 1.359(15) . ? C22 N4 1.269(13) . ? Cu1 O13 1.943(4) . ? Cu1 O17 1.963(5) . ? Cu1 N4 1.972(6) . ? Cu1 N3 2.051(6) . ? Cu2 O12 1.988(5) 3_675 ? Cu2 O12 1.988(5) . ? Cu2 N1 2.014(6) 4_575 ? Cu2 N1 2.014(6) 2_655 ? P3 O14 1.487(5) . ? P3 O17 1.527(6) . ? P3 O15 1.574(5) . ? P3 C16 1.809(7) . ? P4 O11 1.482(5) . ? P4 O12 1.517(5) . ? P4 O13 1.528(5) . ? P4 C14 1.834(7) . ? N3 C14 1.486(8) . ? N3 C16 1.501(9) . ? N3 C11 1.525(8) . ? N1 C5 1.276(11) . ? N1 C1 1.386(11) . ? N1 Cu2 2.014(6) 2_645 ? C11 C12 1.545(11) . ? C13 C13 1.508(15) 3_565 ? C13 C12 1.544(10) . ? C8 C7 1.624(17) . ? C6 C7 1.40(2) . ? C6 C3 1.639(17) . ? C1 C2 1.295(13) . ? C3 C4 1.347(17) . ? C3 C2 1.417(16) . ? C5 C4 1.368(14) . ? 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 N4 C23 C21 126.5(14) . . ? C8 C21 C23 123.0(15) . . ? C8 C9 C22 121.8(19) . . ? N4 C22 C9 127.3(17) . . ? O13 Cu1 O17 167.91(19) . . ? O13 Cu1 N4 91.9(2) . . ? O17 Cu1 N4 92.2(2) . . ? O13 Cu1 N3 87.41(19) . . ? O17 Cu1 N3 87.2(2) . . ? N4 Cu1 N3 173.2(2) . . ? O12 Cu2 O12 180.0 3_675 . ? O12 Cu2 N1 91.5(2) 3_675 4_575 ? O12 Cu2 N1 88.5(2) . 4_575 ? O12 Cu2 N1 88.5(2) 3_675 2_655 ? O12 Cu2 N1 91.5(2) . 2_655 ? N1 Cu2 N1 179.997(1) 4_575 2_655 ? O14 P3 O17 115.1(3) . . ? O14 P3 O15 110.8(3) . . ? O17 P3 O15 109.4(3) . . ? O14 P3 C16 111.9(3) . . ? O17 P3 C16 103.8(3) . . ? O15 P3 C16 105.1(3) . . ? O11 P4 O12 109.6(3) . . ? O11 P4 O13 113.4(3) . . ? O12 P4 O13 111.5(3) . . ? O11 P4 C14 112.2(3) . . ? O12 P4 C14 106.3(3) . . ? O13 P4 C14 103.7(3) . . ? C22 N4 C23 106.7(11) . . ? C22 N4 Cu1 128.3(9) . . ? C23 N4 Cu1 124.0(7) . . ? P3 O17 Cu1 117.7(3) . . ? C14 N3 C16 111.1(6) . . ? C14 N3 C11 111.7(5) . . ? C16 N3 C11 112.6(5) . . ? C14 N3 Cu1 104.9(4) . . ? C16 N3 Cu1 107.0(4) . . ? C11 N3 Cu1 109.1(5) . . ? P4 O12 Cu2 128.5(3) . . ? C5 N1 C1 116.1(7) . . ? C5 N1 Cu2 121.9(6) . 2_645 ? C1 N1 Cu2 122.0(5) . 2_645 ? P4 O13 Cu1 116.1(3) . . ? N3 C11 C12 112.5(6) . . ? N3 C14 P4 109.4(5) . . ? N3 C16 P3 109.0(5) . . ? C13 C13 C12 110.1(9) 3_565 . ? C13 C12 C11 108.9(7) . . ? C21 C8 C9 111.8(14) . . ? C21 C8 C7 121.6(13) . . ? C9 C8 C7 125.9(14) . . ? C7 C6 C3 102.2(13) . . ? C2 C1 N1 124.4(9) . . ? C6 C7 C8 105.4(15) . . ? C4 C3 C2 115.9(10) . . ? C4 C3 C6 122.6(12) . . ? C2 C3 C6 121.5(11) . . ? N1 C5 C4 123.0(10) . . ? C1 C2 C3 119.0(11) . . ? C3 C4 C5 121.2(12) . . ? _diffrn_measured_fraction_theta_max 0.893 _diffrn_reflns_theta_full 21.93 _diffrn_measured_fraction_theta_full 0.893 _refine_diff_density_max 0.876 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.115 data_3np _database_code_depnum_ccdc_archive 'CCDC 909976' #TrackingRef '15265_web_deposit_cif_file_0_AndreaIenco_1352302535.totale_ccdc_deposit.cif' _audit_creation_date 2012-11-07T15:51:11-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C34 H46 Cu3 N6 O13 P4' _chemical_formula_sum 'C34 H46 Cu3 N6 O13 P4' _chemical_formula_weight 1061.27 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.288(2) _cell_length_b 9.5700(7) _cell_length_c 24.207(2) _cell_angle_alpha 90 _cell_angle_beta 105.705(9) _cell_angle_gamma 90 _cell_volume 5193.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3222 _cell_measurement_theta_min 4.6166 _cell_measurement_theta_max 61.7919 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description parallelepiped _exptl_crystal_colour blue _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2172 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.081 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.18913 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 8.1241 _diffrn_orient_matrix_ub_11 0.0374969 _diffrn_orient_matrix_ub_12 -0.0052706 _diffrn_orient_matrix_ub_13 0.0630739 _diffrn_orient_matrix_ub_21 0.0574439 _diffrn_orient_matrix_ub_22 -0.0042626 _diffrn_orient_matrix_ub_23 -0.0199388 _diffrn_orient_matrix_ub_31 0.0027435 _diffrn_orient_matrix_ub_32 0.1607778 _diffrn_orient_matrix_ub_33 0.0017647 _diffrn_measurement_device_type 'Xcalibur, Onyx' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0653 _diffrn_reflns_av_unetI/netI 0.0931 _diffrn_reflns_number 17869 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 4.73 _diffrn_reflns_theta_max 61.88 _diffrn_reflns_theta_full 61.88 _diffrn_measured_fraction_theta_full 0.971 _diffrn_measured_fraction_theta_max 0.971 _reflns_number_total 7908 _reflns_number_gt 5196 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7908 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1316 _refine_ls_R_factor_gt 0.1024 _refine_ls_wR_factor_ref 0.2991 _refine_ls_wR_factor_gt 0.273 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.267 _refine_diff_density_min -0.964 _refine_diff_density_rms 0.175 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.006 -0.035 0.494 710 196 ' ' 2 0.051 0.066 0.052 710 199 ' ' 3 0.068 0.071 0.877 12 1 ' ' 4 0.068 0.429 0.377 11 1 ' ' 5 0.932 0.571 0.623 11 0 ' ' 6 0.932 0.929 0.123 10 1 ' ' _platon_squeeze_details ; ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.26226(5) -0.95725(13) 0.48279(5) 0.0303(4) Uani 1 1 d . . . Cu2 Cu 0.26191(5) -0.56352(13) 0.57542(5) 0.0303(4) Uani 1 1 d . . . Cu3 Cu 0.27396(5) -1.35362(14) 0.37970(5) 0.0320(4) Uani 1 1 d . . . P1 P 0.18923(10) -0.8193(3) 0.56402(10) 0.0326(6) Uani 1 1 d . . . P2 P 0.21636(10) -0.2941(3) 0.51479(9) 0.0310(6) Uani 1 1 d . . . P3 P 0.33838(10) -1.0815(2) 0.40345(9) 0.0307(6) Uani 1 1 d . . . P4 P 0.31044(9) -1.6030(2) 0.45502(9) 0.0281(5) Uani 1 1 d . . . N1 N 0.1734(3) -0.5506(7) 0.5306(3) 0.0273(16) Uani 1 1 d . . . N2 N 0.3595(3) -1.3518(8) 0.4388(3) 0.0327(17) Uani 1 1 d . . . N3 N 0.3341(3) -0.9788(7) 0.5533(3) 0.0294(16) Uani 1 1 d . . . N4 N 0.6535(3) -1.0598(7) 0.8737(3) 0.0326(18) Uani 1 1 d . . . N5 N 0.1909(3) -0.9245(7) 0.4149(3) 0.0270(16) Uani 1 1 d . . . N6 N 0.1893(3) -1.3599(8) 0.3342(3) 0.0336(18) Uani 1 1 d . . . O1 O 0.2420(2) -0.7393(6) 0.6037(2) 0.0288(13) Uani 1 1 d . . . O2 O 0.2093(3) -0.9435(6) 0.5336(2) 0.0310(14) Uani 1 1 d . . . O3 O 0.1454(3) -0.8698(6) 0.5944(3) 0.0391(16) Uani 1 1 d . . . O4 O 0.2670(2) -0.3646(6) 0.5627(2) 0.0294(14) Uani 1 1 d . . . O5 O 0.2368(2) -0.2130(6) 0.4712(2) 0.0330(14) Uani 1 1 d . . . O6 O 0.1788(2) -0.1988(6) 0.5457(3) 0.0319(14) Uani 1 1 d . . . O7 O 0.2847(2) -1.1623(6) 0.3633(2) 0.0332(14) Uani 1 1 d . . . O8 O 0.3166(2) -0.9559(6) 0.4335(2) 0.0306(14) Uani 1 1 d . . . O9 O 0.3846(3) -1.0388(6) 0.3750(3) 0.0391(15) Uani 1 1 d . . . O10 O 0.2634(2) -1.5428(6) 0.4032(2) 0.0326(14) Uani 1 1 d . . . O11 O 0.3534(3) -1.7064(6) 0.4340(2) 0.0322(14) Uani 1 1 d . . . O12 O 0.2865(2) -1.6704(6) 0.4998(2) 0.0301(14) Uani 1 1 d . . . O23 O 0.3021(3) -1.4129(8) 0.2940(3) 0.052(2) Uani 1 1 d . . . C1 C 0.1573(4) -0.6918(10) 0.5070(4) 0.037(2) Uani 1 1 d . . . H1A H 0.1734 -0.7077 0.4737 0.044 Uiso 1 1 calc R . . H1B H 0.1134 -0.7019 0.4942 0.044 Uiso 1 1 calc R . . C2 C 0.1698(4) -0.4424(10) 0.4839(4) 0.036(2) Uani 1 1 d . . . H2A H 0.128 -0.4117 0.4681 0.043 Uiso 1 1 calc R . . H2B H 0.1838 -0.4834 0.4523 0.043 Uiso 1 1 calc R . . C3 C 0.1384(4) -0.5041(10) 0.5736(4) 0.031(2) Uani 1 1 d . . . H3A H 0.1349 -0.5854 0.5978 0.037 Uiso 1 1 calc R . . H3B H 0.1622 -0.4321 0.5992 0.037 Uiso 1 1 calc R . . C4 C 0.0766(4) -0.4460(11) 0.5475(4) 0.042(2) Uani 1 1 d . . . H4A H 0.06 -0.4194 0.5795 0.05 Uiso 1 1 calc R . . H4B H 0.0814 -0.3585 0.5273 0.05 Uiso 1 1 calc R . . C5 C 0.0306(4) -0.5321(10) 0.5067(4) 0.040(2) Uani 1 1 d . . . H5A H 0.0293 -0.626 0.5235 0.048 Uiso 1 1 calc R . . H5B H 0.0423 -0.5438 0.4706 0.048 Uiso 1 1 calc R . . C6 C 0.3674(4) -1.2079(8) 0.4614(4) 0.0283(19) Uani 1 1 d . . . H6A H 0.4103 -1.1897 0.4791 0.034 Uiso 1 1 calc R . . H6B H 0.3461 -1.1969 0.4913 0.034 Uiso 1 1 calc R . . C7 C 0.3555(4) -1.4532(9) 0.4844(4) 0.029(2) Uani 1 1 d . . . H7A H 0.338 -1.4059 0.5124 0.035 Uiso 1 1 calc R . . H7B H 0.3961 -1.4848 0.5051 0.035 Uiso 1 1 calc R . . C8 C 0.4061(3) -1.3910(8) 0.4082(3) 0.0239(18) Uani 1 1 d . . . H8A H 0.3966 -1.3415 0.3709 0.029 Uiso 1 1 calc R . . H8B H 0.4027 -1.4924 0.3999 0.029 Uiso 1 1 calc R . . C9 C 0.4708(4) -1.3590(10) 0.4404(4) 0.033(2) Uani 1 1 d . . . H9A H 0.4958 -1.3889 0.4153 0.04 Uiso 1 1 calc R . . H9B H 0.4745 -1.2561 0.4439 0.04 Uiso 1 1 calc R . . C10 C 0.4987(4) -1.4198(9) 0.4996(4) 0.032(2) Uani 1 1 d . . . H10A H 0.4754 -1.3882 0.526 0.039 Uiso 1 1 calc R . . H10B H 0.5397 -1.3826 0.5142 0.039 Uiso 1 1 calc R . . C40 C 0.3884(4) -0.9388(9) 0.5541(4) 0.032(2) Uani 1 1 d . . . H40 H 0.3936 -0.8955 0.5204 0.039 Uiso 1 1 calc R . . C41 C 0.4378(4) -0.9546(9) 0.5990(4) 0.033(2) Uani 1 1 d . . . H41 H 0.4754 -0.9226 0.5958 0.039 Uiso 1 1 calc R . . C42 C 0.4337(4) -1.0163(10) 0.6491(4) 0.032(2) Uani 1 1 d . . . C43 C 0.3753(4) -1.0608(10) 0.6493(4) 0.032(2) Uani 1 1 d . . . H43 H 0.369 -1.104 0.6826 0.038 Uiso 1 1 calc R . . C44 C 0.3283(4) -1.0416(10) 0.6019(4) 0.036(2) Uani 1 1 d . . . H44 H 0.2899 -1.0734 0.6029 0.043 Uiso 1 1 calc R . . C45 C 0.6322(4) -1.1749(10) 0.8419(4) 0.035(2) Uani 1 1 d . . . H45 H 0.6565 -1.2555 0.844 0.043 Uiso 1 1 calc R . . C46 C 0.5740(4) -1.1736(10) 0.8058(4) 0.036(2) Uani 1 1 d . . . H46 H 0.5596 -1.2542 0.7835 0.044 Uiso 1 1 calc R . . C47 C 0.5381(4) -1.0639(9) 0.8016(4) 0.032(2) Uani 1 1 d . . . C48 C 0.5599(4) -0.9462(9) 0.8349(4) 0.033(2) Uani 1 1 d . . . H48 H 0.5362 -0.8648 0.8334 0.039 Uiso 1 1 calc R . . C49 C 0.6162(4) -0.9530(9) 0.8693(4) 0.032(2) Uani 1 1 d . . . H49 H 0.6304 -0.8737 0.8926 0.039 Uiso 1 1 calc R . . C50 C 0.4875(4) -1.0346(10) 0.6993(4) 0.036(2) Uani 1 1 d . . . H50A H 0.5125 -0.95 0.7019 0.044 Uiso 1 1 calc R . . H50B H 0.5108 -1.1142 0.6907 0.044 Uiso 1 1 calc R . . C51 C 0.4774(4) -1.0601(10) 0.7589(4) 0.038(2) Uani 1 1 d . . . H51A H 0.4529 -0.984 0.7686 0.046 Uiso 1 1 calc R . . H51B H 0.4563 -1.1498 0.7593 0.046 Uiso 1 1 calc R . . C60 C 0.1936(4) -0.8593(9) 0.3657(4) 0.034(2) Uani 1 1 d . . . H60 H 0.2318 -0.8333 0.3621 0.041 Uiso 1 1 calc R . . C61 C 0.1450(4) -0.8285(11) 0.3209(4) 0.040(2) Uani 1 1 d . . . H61 H 0.1502 -0.7924 0.286 0.048 Uiso 1 1 calc R . . C62 C 0.0877(4) -0.8510(10) 0.3273(4) 0.038(2) Uani 1 1 d . . . C63 C 0.0843(4) -0.9219(11) 0.3771(4) 0.045(3) Uani 1 1 d . . . H63 H 0.0462 -0.9442 0.382 0.054 Uiso 1 1 calc R . . C64 C 0.1347(4) -0.9600(10) 0.4191(4) 0.034(2) Uani 1 1 d . . . H64 H 0.1308 -1.0115 0.4514 0.04 Uiso 1 1 calc R . . C65 C -0.1474(5) -0.7689(11) 0.1615(4) 0.048(3) Uani 1 1 d . . . H65 H -0.1582 -0.688 0.1382 0.058 Uiso 1 1 calc R . . C66 C -0.0875(4) -0.7916(11) 0.1907(5) 0.050(3) Uani 1 1 d . . . H66 H -0.0582 -0.7278 0.1855 0.06 Uiso 1 1 calc R . . C67 C -0.0702(4) -0.9024(11) 0.2264(4) 0.044(2) Uani 1 1 d . . . C68 C -0.1141(4) -0.9912(10) 0.2309(4) 0.037(2) Uani 1 1 d . . . H68 H -0.1045 -1.0687 0.2563 0.045 Uiso 1 1 calc R . . C69 C -0.1711(4) -0.9719(10) 0.2001(4) 0.039(2) Uani 1 1 d . . . H69 H -0.1999 -1.0402 0.2026 0.047 Uiso 1 1 calc R . . C70 C -0.0058(4) -0.9375(11) 0.2597(4) 0.049(3) Uani 1 1 d . . . H70A H 0.0136 -0.989 0.2342 0.059 Uiso 1 1 calc R . . H70B H -0.0064 -0.9993 0.2924 0.059 Uiso 1 1 calc R . . C71 C 0.0309(4) -0.8067(11) 0.2826(4) 0.046(3) Uani 1 1 d . . . H71A H 0.0412 -0.7569 0.2507 0.055 Uiso 1 1 calc R . . H71B H 0.0075 -0.7427 0.3001 0.055 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0260(7) 0.0324(8) 0.0248(7) -0.0005(5) -0.0065(5) 0.0064(5) Cu2 0.0272(7) 0.0256(8) 0.0297(7) 0.0028(6) -0.0069(5) 0.0034(5) Cu3 0.0225(7) 0.0296(8) 0.0352(7) 0.0025(6) -0.0071(5) 0.0006(5) P1 0.0309(12) 0.0318(13) 0.0314(12) 0.0043(10) 0.0019(10) 0.0064(10) P2 0.0247(12) 0.0327(13) 0.0289(12) 0.0031(10) -0.0042(9) 0.0045(10) P3 0.0316(12) 0.0264(12) 0.0294(12) -0.0002(10) 0.0001(9) 0.0044(10) P4 0.0234(11) 0.0241(12) 0.0290(11) 0.0014(9) -0.0064(9) 0.0004(9) N1 0.029(4) 0.019(4) 0.029(4) 0.012(3) -0.002(3) 0.008(3) N2 0.024(4) 0.030(4) 0.036(4) 0.006(3) -0.006(3) 0.008(3) N3 0.032(4) 0.025(4) 0.029(4) 0.001(3) 0.003(3) 0.005(3) N4 0.043(4) 0.022(4) 0.024(4) 0.005(3) -0.006(3) -0.012(3) N5 0.022(4) 0.026(4) 0.029(4) 0.001(3) 0.000(3) 0.009(3) N6 0.037(4) 0.028(4) 0.026(4) 0.002(3) -0.010(3) 0.000(3) O1 0.029(3) 0.030(3) 0.020(3) 0.001(3) -0.006(2) 0.003(3) O2 0.030(3) 0.037(4) 0.019(3) 0.003(3) -0.007(2) -0.002(3) O3 0.044(4) 0.019(3) 0.047(4) 0.000(3) -0.001(3) 0.000(3) O4 0.021(3) 0.022(3) 0.034(3) 0.001(3) -0.011(2) 0.011(2) O5 0.026(3) 0.035(4) 0.034(3) -0.009(3) 0.000(3) 0.000(3) O6 0.027(3) 0.027(3) 0.040(3) -0.002(3) 0.007(3) 0.007(3) O7 0.030(3) 0.035(4) 0.025(3) -0.005(3) -0.008(2) -0.003(3) O8 0.027(3) 0.027(3) 0.031(3) -0.006(3) -0.005(2) 0.004(3) O9 0.048(4) 0.026(4) 0.045(4) -0.001(3) 0.016(3) 0.003(3) O10 0.020(3) 0.046(4) 0.027(3) 0.006(3) -0.003(2) -0.001(3) O11 0.029(3) 0.027(3) 0.039(3) -0.009(3) 0.007(3) 0.001(3) O12 0.028(3) 0.027(3) 0.028(3) -0.008(3) -0.006(2) -0.001(3) O23 0.050(4) 0.068(5) 0.030(3) -0.012(3) -0.001(3) 0.028(4) C1 0.034(5) 0.038(6) 0.029(5) 0.007(4) -0.005(4) 0.004(4) C2 0.030(5) 0.040(6) 0.029(5) 0.020(4) -0.005(4) 0.000(4) C3 0.026(5) 0.031(5) 0.033(5) 0.003(4) 0.004(4) 0.002(4) C4 0.027(5) 0.051(7) 0.045(5) 0.007(5) 0.002(4) 0.001(4) C5 0.035(5) 0.032(5) 0.046(5) 0.002(5) 0.000(4) 0.008(4) C6 0.020(4) 0.017(4) 0.043(5) 0.002(4) 0.000(4) -0.006(3) C7 0.017(4) 0.036(5) 0.033(5) 0.000(4) 0.006(3) 0.006(4) C8 0.024(4) 0.012(4) 0.030(4) 0.004(3) -0.002(3) 0.004(3) C9 0.024(4) 0.035(5) 0.036(5) -0.007(4) 0.003(4) -0.003(4) C10 0.022(4) 0.032(5) 0.039(5) 0.001(4) 0.002(4) 0.001(4) C40 0.032(5) 0.035(5) 0.026(4) -0.004(4) 0.002(4) 0.001(4) C41 0.026(5) 0.034(5) 0.030(5) 0.007(4) -0.007(4) -0.002(4) C42 0.032(5) 0.031(5) 0.030(5) 0.000(4) 0.002(4) -0.005(4) C43 0.025(5) 0.038(6) 0.028(4) 0.003(4) -0.003(4) 0.001(4) C44 0.034(5) 0.034(5) 0.041(5) 0.008(4) 0.012(4) 0.002(4) C45 0.047(6) 0.024(5) 0.034(5) 0.001(4) 0.007(4) 0.004(4) C46 0.031(5) 0.034(6) 0.036(5) 0.001(4) -0.004(4) -0.004(4) C47 0.043(5) 0.015(5) 0.034(5) 0.001(4) 0.005(4) 0.003(4) C48 0.042(5) 0.016(5) 0.037(5) 0.002(4) 0.004(4) 0.008(4) C49 0.035(5) 0.025(5) 0.031(5) 0.002(4) -0.001(4) -0.003(4) C50 0.025(5) 0.041(6) 0.036(5) 0.004(4) -0.003(4) -0.006(4) C51 0.030(5) 0.039(6) 0.035(5) -0.005(4) -0.008(4) -0.004(4) C60 0.028(5) 0.030(5) 0.038(5) 0.001(4) -0.003(4) -0.001(4) C61 0.024(5) 0.048(6) 0.042(5) -0.007(5) -0.002(4) 0.004(4) C62 0.030(5) 0.041(6) 0.034(5) 0.000(4) -0.005(4) 0.000(4) C63 0.035(5) 0.048(6) 0.050(6) 0.009(5) 0.005(5) 0.002(5) C64 0.021(4) 0.034(5) 0.039(5) 0.009(4) -0.005(4) 0.008(4) C65 0.054(7) 0.038(6) 0.047(6) 0.004(5) 0.003(5) -0.012(5) C66 0.021(5) 0.040(6) 0.076(8) 0.003(6) -0.008(5) 0.002(4) C67 0.041(6) 0.046(6) 0.042(6) 0.007(5) 0.006(5) 0.006(5) C68 0.036(5) 0.025(5) 0.044(5) 0.004(4) -0.002(4) 0.007(4) C69 0.032(5) 0.033(5) 0.044(5) -0.005(5) -0.003(4) -0.005(4) C70 0.036(6) 0.051(7) 0.045(6) 0.006(5) -0.015(5) 0.000(5) C71 0.039(6) 0.051(7) 0.040(5) 0.003(5) -0.001(4) -0.006(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O8 1.960(6) . ? Cu1 O2 1.968(6) . ? Cu1 N5 2.019(6) . ? Cu1 N3 2.052(7) . ? Cu2 O1 1.919(6) . ? Cu2 O4 1.937(6) . ? Cu2 N4 2.020(7) 2_656 ? Cu2 N1 2.056(7) . ? Cu2 O12 2.301(6) 1_565 ? Cu3 O7 1.905(6) . ? Cu3 O10 1.934(6) . ? Cu3 N6 1.983(7) . ? Cu3 N2 2.115(7) . ? Cu3 O23 2.407(6) . ? P1 O3 1.492(7) . ? P1 O2 1.536(6) . ? P1 O1 1.542(6) . ? P1 C1 1.841(9) . ? P2 O5 1.487(7) . ? P2 O4 1.565(5) . ? P2 O6 1.585(6) . ? P2 C2 1.819(9) . ? P3 O9 1.483(7) . ? P3 O8 1.559(6) . ? P3 O7 1.564(6) . ? P3 C6 1.837(8) . ? P4 O12 1.493(6) . ? P4 O10 1.536(6) . ? P4 O11 1.586(6) . ? P4 C7 1.805(9) . ? N1 C1 1.476(11) . ? N1 C2 1.518(10) . ? N1 C3 1.551(11) . ? N2 C6 1.474(11) . ? N2 C7 1.493(11) . ? N2 C8 1.516(11) . ? N3 C40 1.317(11) . ? N3 C44 1.358(11) . ? N4 C49 1.328(11) . ? N4 C45 1.359(11) . ? N4 Cu2 2.020(7) 2_646 ? N5 C60 1.361(11) . ? N5 C64 1.383(11) . ? N6 C65 1.333(12) 2_545 ? N6 C69 1.352(12) 2_545 ? O12 Cu2 2.301(6) 1_545 ? C3 C4 1.513(12) . ? C4 C5 1.493(13) . ? C5 C5 1.506(17) 3_546 ? C8 C9 1.529(10) . ? C9 C10 1.522(12) . ? C10 C10 1.537(17) 3_626 ? C40 C41 1.360(11) . ? C41 C42 1.375(12) . ? C42 C43 1.426(12) . ? C42 C50 1.500(11) . ? C43 C44 1.368(12) . ? C45 C46 1.399(12) . ? C46 C47 1.329(12) . ? C47 C48 1.398(12) . ? C47 C51 1.509(12) . ? C48 C49 1.351(12) . ? C50 C51 1.545(12) . ? C60 C61 1.370(12) . ? C61 C62 1.401(13) . ? C62 C63 1.405(13) . ? C62 C71 1.524(12) . ? C63 C64 1.377(12) . ? C65 N6 1.333(12) 2 ? C65 C66 1.399(13) . ? C66 C67 1.358(14) . ? C67 C68 1.358(14) . ? C67 C70 1.535(13) . ? C68 C69 1.347(12) . ? C69 N6 1.352(12) 2 ? C70 C71 1.532(14) . ? 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 O8 Cu1 O2 175.6(2) . . ? O8 Cu1 N5 91.6(3) . . ? O2 Cu1 N5 89.0(2) . . ? O8 Cu1 N3 89.6(3) . . ? O2 Cu1 N3 89.7(3) . . ? N5 Cu1 N3 176.6(3) . . ? O1 Cu2 O4 161.6(3) . . ? O1 Cu2 N4 95.0(3) . 2_656 ? O4 Cu2 N4 89.3(3) . 2_656 ? O1 Cu2 N1 86.4(2) . . ? O4 Cu2 N1 87.3(2) . . ? N4 Cu2 N1 173.0(3) 2_656 . ? O1 Cu2 O12 91.7(2) . 1_565 ? O4 Cu2 O12 105.7(2) . 1_565 ? N4 Cu2 O12 94.6(2) 2_656 1_565 ? N1 Cu2 O12 92.1(2) . 1_565 ? O7 Cu3 O10 174.9(3) . . ? O7 Cu3 N6 94.6(3) . . ? O10 Cu3 N6 87.1(3) . . ? O7 Cu3 N2 88.8(3) . . ? O10 Cu3 N2 88.9(3) . . ? N6 Cu3 N2 171.7(3) . . ? O7 Cu3 O23 88.0(3) . . ? O10 Cu3 O23 96.9(3) . . ? N6 Cu3 O23 88.6(3) . . ? N2 Cu3 O23 99.1(3) . . ? O3 P1 O2 108.9(4) . . ? O3 P1 O1 113.0(3) . . ? O2 P1 O1 112.8(3) . . ? O3 P1 C1 113.1(4) . . ? O2 P1 C1 105.5(4) . . ? O1 P1 C1 103.2(4) . . ? O5 P2 O4 115.4(3) . . ? O5 P2 O6 111.0(3) . . ? O4 P2 O6 107.5(3) . . ? O5 P2 C2 112.7(4) . . ? O4 P2 C2 102.3(4) . . ? O6 P2 C2 107.4(4) . . ? O9 P3 O8 112.0(4) . . ? O9 P3 O7 113.9(4) . . ? O8 P3 O7 111.4(3) . . ? O9 P3 C6 111.8(4) . . ? O8 P3 C6 104.5(4) . . ? O7 P3 C6 102.4(3) . . ? O12 P4 O10 115.5(3) . . ? O12 P4 O11 110.8(3) . . ? O10 P4 O11 110.2(3) . . ? O12 P4 C7 110.4(4) . . ? O10 P4 C7 103.5(4) . . ? O11 P4 C7 105.8(4) . . ? C1 N1 C2 112.3(7) . . ? C1 N1 C3 113.4(7) . . ? C2 N1 C3 111.7(6) . . ? C1 N1 Cu2 105.2(5) . . ? C2 N1 Cu2 106.3(5) . . ? C3 N1 Cu2 107.3(5) . . ? C6 N2 C7 111.0(7) . . ? C6 N2 C8 112.3(7) . . ? C7 N2 C8 113.4(6) . . ? C6 N2 Cu3 105.0(5) . . ? C7 N2 Cu3 105.0(5) . . ? C8 N2 Cu3 109.6(5) . . ? C40 N3 C44 115.9(7) . . ? C40 N3 Cu1 123.1(6) . . ? C44 N3 Cu1 120.9(6) . . ? C49 N4 C45 116.5(8) . . ? C49 N4 Cu2 124.9(6) . 2_646 ? C45 N4 Cu2 118.6(6) . 2_646 ? C60 N5 C64 116.4(7) . . ? C60 N5 Cu1 124.1(6) . . ? C64 N5 Cu1 119.3(6) . . ? C65 N6 C69 116.9(8) 2_545 2_545 ? C65 N6 Cu3 125.1(7) 2_545 . ? C69 N6 Cu3 117.7(6) 2_545 . ? P1 O1 Cu2 116.2(3) . . ? P1 O2 Cu1 132.5(4) . . ? P2 O4 Cu2 118.4(3) . . ? P3 O7 Cu3 118.3(3) . . ? P3 O8 Cu1 128.7(4) . . ? P4 O10 Cu3 118.2(3) . . ? P4 O12 Cu2 127.4(3) . 1_545 ? N1 C1 P1 108.0(5) . . ? N1 C2 P2 108.6(5) . . ? C4 C3 N1 116.0(7) . . ? C5 C4 C3 120.3(9) . . ? C4 C5 C5 112.7(10) . 3_546 ? N2 C6 P3 110.4(6) . . ? N2 C7 P4 111.8(6) . . ? N2 C8 C9 116.0(6) . . ? C10 C9 C8 120.9(8) . . ? C9 C10 C10 113.5(9) . 3_626 ? N3 C40 C41 125.4(8) . . ? C40 C41 C42 120.5(9) . . ? C41 C42 C43 115.2(8) . . ? C41 C42 C50 121.4(8) . . ? C43 C42 C50 123.4(8) . . ? C44 C43 C42 120.2(8) . . ? N3 C44 C43 122.8(9) . . ? N4 C45 C46 119.4(9) . . ? C47 C46 C45 122.6(9) . . ? C46 C47 C48 117.9(8) . . ? C46 C47 C51 121.7(8) . . ? C48 C47 C51 120.2(8) . . ? C49 C48 C47 117.2(8) . . ? N4 C49 C48 126.3(8) . . ? C42 C50 C51 118.0(7) . . ? C47 C51 C50 107.0(7) . . ? N5 C60 C61 124.5(9) . . ? C60 C61 C62 119.2(9) . . ? C61 C62 C63 116.4(9) . . ? C61 C62 C71 123.3(9) . . ? C63 C62 C71 120.3(9) . . ? C64 C63 C62 121.7(9) . . ? C63 C64 N5 121.1(9) . . ? N6 C65 C66 120.6(10) 2 . ? C67 C66 C65 121.9(10) . . ? C68 C67 C66 116.0(9) . . ? C68 C67 C70 118.1(9) . . ? C66 C67 C70 125.9(10) . . ? C69 C68 C67 121.4(9) . . ? C68 C69 N6 123.1(9) . 2 ? C67 C70 C71 112.4(9) . . ? C62 C71 C70 108.7(8) . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF