Electronic Supplementary Material for CrystEngComm This Journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Prof Jon Zubieta' _publ_contact_author_address ; Department of Chemistry Syracuse University Syracuse New York 13244 UNITED STATES OF AMERICA ; _publ_contact_author_email JAZUBIET@SYR.EDU _publ_contact_author_phone '315 443 2547' _publ_contact_author_fax '315 443 4070' _publ_section_title ; Secondary Metal-Ligand Cationic Subunits {ML}n+ as Structural Determinants in the Oxovanadium/Phenylphosphonate/{ML}n+ System, where {ML} is a Cu2+/Organonitrogen Moiety. ; loop_ _publ_author_name 'Jon Zubieta' "Charles O'Connor" 'Ming Hui Yu' 'Gundog Yucesan' data_2 _database_code_depnum_ccdc_archive 'CCDC 270525' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H24 Cu2 N5 O11 P3 V' _chemical_formula_weight 901.47 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' V V 0.3005 0.5294 '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/c 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 13.4837(13) _cell_length_b 13.7172(13) _cell_length_c 18.9414(18) _cell_angle_alpha 90.00 _cell_angle_beta 87.155(3) _cell_angle_gamma 90.00 _cell_volume 3499.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 8334 _cell_measurement_theta_min 1.51 _cell_measurement_theta_max 28 _exptl_crystal_description plate _exptl_crystal_colour Green _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1812 _exptl_absorpt_coefficient_mu 1.670 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS SHELX-97 (shledrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 35794 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 28.00 _reflns_number_total 8434 _reflns_number_gt 5393 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0562P)^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 8434 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1291 _refine_ls_wR_factor_gt 0.1098 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.037999(8) 0.905740(8) 0.229110(6) 0.00751(3) Uani 1 1 d . . . Cu2 Cu -0.036900(8) 0.409941(8) 0.044128(6) 0.00740(3) Uani 1 1 d . . . V1 V -0.026879(11) 0.833499(11) -0.037660(8) 0.00685(4) Uani 1 1 d . . . P1 P -0.079591(16) 0.970662(16) 0.097280(11) 0.00484(5) Uani 1 1 d . . . P2 P -0.106471(17) 0.665047(17) 0.071370(12) 0.00788(5) Uani 1 1 d . . . P3 P 0.107051(17) 0.325658(17) 0.147362(12) 0.00744(5) Uani 1 1 d . . . O1 O -0.03650(5) 0.89061(5) 0.14301(3) 0.00626(12) Uani 1 1 d . . . O2 O -0.01902(5) 1.06311(4) 0.10410(3) 0.00660(12) Uani 1 1 d . . . O3 O -0.08560(5) 0.93671(5) 0.02120(3) 0.00695(12) Uani 1 1 d . . . O4 O 0.07671(5) 0.79469(5) -0.01250(4) 0.01157(13) Uani 1 1 d . . . O5 O -0.11981(5) 0.74549(5) 0.01810(3) 0.00968(12) Uani 1 1 d . . . O6 O -0.05300(5) 0.70510(5) 0.13751(3) 0.01257(13) Uani 1 1 d . . . O7 O -0.04832(5) 0.57700(5) 0.04360(3) 0.01098(14) Uani 1 1 d . . . O8 O 0.08040(5) 0.40752(5) 0.09781(4) 0.00995(13) Uani 1 1 d . . . O9 O 0.07559(5) 0.34620(5) 0.22360(3) 0.01034(13) Uani 1 1 d . . . O10 O 0.06689(5) 0.22700(5) 0.12400(3) 0.01331(14) Uani 1 1 d . . . O90 O 0.01578(7) 1.06759(6) 0.24490(4) 0.02090(16) Uani 1 1 d . . . N1 N 0.17221(6) 0.91011(6) 0.17018(4) 0.01070(16) Uani 1 1 d . . . N2 N 0.13327(6) 0.89448(6) 0.30450(4) 0.01071(15) Uani 1 1 d . . . N3 N 0.13142(6) 0.88659(6) 0.37591(4) 0.00801(14) Uani 1 1 d . . . N4 N 0.16301(6) 0.89078(5) 0.50929(4) 0.00588(13) Uani 1 1 d . . . N10 N 0.29003(6) 0.86988(6) 0.33647(5) 0.01324(16) Uani 1 1 d . . . C1 C 0.18622(8) 0.92388(8) 0.10031(5) 0.01517(19) Uani 1 1 d . . . H1 H 0.1307 0.9325 0.0738 0.018 Uiso 1 1 calc R . . C2 C 0.27855(8) 0.92599(10) 0.06570(5) 0.0230(2) Uani 1 1 d . . . H2 H 0.2854 0.9368 0.0172 0.028 Uiso 1 1 calc R . . C3 C 0.36071(8) 0.91145(10) 0.10541(6) 0.0258(3) Uani 1 1 d . . . H3 H 0.4241 0.9133 0.0838 0.031 Uiso 1 1 calc R . . C4 C 0.34842(8) 0.89414(9) 0.17727(6) 0.0213(2) Uani 1 1 d . . . H4 H 0.4027 0.8821 0.2044 0.026 Uiso 1 1 calc R . . C5 C 0.25321(7) 0.89530(7) 0.20760(5) 0.01226(18) Uani 1 1 d . . . C6 C 0.22922(7) 0.88330(7) 0.28353(5) 0.01068(18) Uani 1 1 d . . . C7 C 0.22530(7) 0.87248(7) 0.39239(5) 0.01023(17) Uani 1 1 d . . . C8 C 0.24434(7) 0.86780(7) 0.46751(5) 0.01130(17) Uani 1 1 d . . . C9 C 0.33299(7) 0.84285(8) 0.49551(6) 0.01557(19) Uani 1 1 d . . . H9 H 0.3878 0.8275 0.4659 0.019 Uiso 1 1 calc R . . C10 C 0.34009(7) 0.84079(8) 0.56772(6) 0.0179(2) Uani 1 1 d . . . H10 H 0.3991 0.8227 0.5875 0.022 Uiso 1 1 calc R . . C11 C 0.25788(7) 0.86609(8) 0.61018(5) 0.01512(19) Uani 1 1 d . . . H11 H 0.2614 0.8668 0.6591 0.018 Uiso 1 1 calc R . . C12 C 0.17085(7) 0.89018(6) 0.57970(5) 0.01010(17) Uani 1 1 d . . . H12 H 0.1157 0.9066 0.6087 0.012 Uiso 1 1 calc R . . C13 C -0.20460(7) 0.99760(7) 0.12610(5) 0.00935(17) Uani 1 1 d . . . C14 C -0.23549(8) 1.08869(7) 0.15099(6) 0.0189(2) Uani 1 1 d . . . H14 H -0.1885 1.1375 0.1559 0.023 Uiso 1 1 calc R . . C15 C -0.33383(10) 1.10853(10) 0.16850(8) 0.0317(3) Uani 1 1 d . . . H15 H -0.3532 1.1705 0.1835 0.038 Uiso 1 1 calc R . . C16 C -0.40252(9) 1.03609(11) 0.16350(9) 0.0364(3) Uani 1 1 d . . . H16 H -0.4688 1.0487 0.1760 0.044 Uiso 1 1 calc R . . C17 C -0.37456(9) 0.94370(10) 0.13994(9) 0.0354(3) Uani 1 1 d . . . H17 H -0.4218 0.8947 0.1367 0.043 Uiso 1 1 calc R . . C18 C -0.27737(8) 0.92543(9) 0.12170(7) 0.0237(2) Uani 1 1 d . . . H18 H -0.2589 0.8635 0.1059 0.028 Uiso 1 1 calc R . . C19 C -0.22859(7) 0.63120(7) 0.10408(5) 0.01007(17) Uani 1 1 d . . . C20 C -0.25790(8) 0.64370(8) 0.17578(6) 0.0179(2) Uani 1 1 d . . . H20 H -0.2122 0.6647 0.2077 0.021 Uiso 1 1 calc R . . C21 C -0.35423(9) 0.62482(10) 0.19857(7) 0.0293(3) Uani 1 1 d . . . H21 H -0.3736 0.6337 0.2460 0.035 Uiso 1 1 calc R . . C22 C -0.42259(10) 0.59290(10) 0.15204(8) 0.0333(3) Uani 1 1 d . . . H22 H -0.4875 0.5799 0.1681 0.040 Uiso 1 1 calc R . . C23 C -0.39459(9) 0.58020(9) 0.08151(7) 0.0268(3) Uani 1 1 d . . . H23 H -0.4406 0.5580 0.0502 0.032 Uiso 1 1 calc R . . C24 C -0.29702(8) 0.60068(7) 0.05709(6) 0.0169(2) Uani 1 1 d . . . H24 H -0.2785 0.5937 0.0094 0.020 Uiso 1 1 calc R . . C25 C 0.24080(6) 0.31399(7) 0.14560(5) 0.01122(17) Uani 1 1 d . . . C26 C 0.29650(8) 0.37792(9) 0.18265(7) 0.0256(2) Uani 1 1 d . . . H26 H 0.2649 0.4270 0.2092 0.031 Uiso 1 1 calc R . . C27 C 0.39990(9) 0.37069(11) 0.18130(9) 0.0382(4) Uani 1 1 d . . . H27 H 0.4366 0.4138 0.2075 0.046 Uiso 1 1 calc R . . C28 C 0.44715(9) 0.29970(13) 0.14120(7) 0.0387(4) Uani 1 1 d . . . H28 H 0.5161 0.2956 0.1392 0.046 Uiso 1 1 calc R . . C29 C 0.39294(12) 0.23532(15) 0.10444(7) 0.0465(4) Uani 1 1 d . . . H29 H 0.4249 0.1861 0.0783 0.056 Uiso 1 1 calc R . . C30 C 0.28955(9) 0.24277(11) 0.10579(6) 0.0275(3) Uani 1 1 d . . . H30 H 0.2532 0.1993 0.0796 0.033 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 0.00547(6) 0.01189(6) 0.00519(6) 0.00030(4) -0.00049(4) -0.00150(4) Cu2 0.00637(6) 0.01089(6) 0.00489(6) 0.00000(4) 0.00021(4) -0.00070(4) V1 0.00997(7) 0.00659(7) 0.00400(7) 0.00060(5) -0.00029(5) -0.00160(5) P1 0.00440(9) 0.00577(10) 0.00428(10) 0.00030(7) 0.00041(7) -0.00021(7) P2 0.00908(10) 0.00889(11) 0.00548(10) -0.00030(8) 0.00142(8) -0.00221(8) P3 0.00639(10) 0.01028(11) 0.00569(10) -0.00180(8) -0.00050(8) -0.00001(8) O1 0.0060(3) 0.0100(3) 0.0030(3) 0.0040(2) -0.0020(2) -0.0003(2) O2 0.0109(3) 0.0040(3) 0.0050(3) 0.0020(2) -0.0017(2) -0.0042(2) O3 0.0090(3) 0.0070(3) 0.0050(3) 0.0012(2) -0.0014(2) -0.0027(2) O4 0.0088(3) 0.0131(3) 0.0130(3) 0.0028(2) -0.0019(2) 0.0002(2) O5 0.0099(3) 0.0100(3) 0.0090(3) 0.0055(2) 0.0010(2) -0.0022(2) O6 0.0189(3) 0.0160(3) 0.0030(3) -0.0017(2) -0.0030(2) 0.0020(3) O7 0.0150(4) 0.0144(3) 0.0035(3) 0.0001(2) -0.0002(3) 0.0010(3) O8 0.0089(3) 0.0110(3) 0.0101(3) -0.0003(2) -0.0020(2) 0.0000(2) O9 0.0070(3) 0.0180(3) 0.0060(3) -0.0039(2) 0.0000(2) 0.0070(2) O10 0.0220(4) 0.0130(3) 0.0050(3) -0.0017(2) -0.0010(2) -0.0040(3) O90 0.0378(5) 0.0150(3) 0.0101(3) -0.0010(3) -0.0030(3) 0.0000(3) N1 0.0099(4) 0.0160(4) 0.0060(4) -0.0030(3) 0.0010(3) -0.0040(3) N2 0.0102(4) 0.0179(4) 0.0039(3) 0.0020(3) 0.0001(3) 0.0020(3) N3 0.0081(3) 0.0079(3) 0.0080(3) 0.0010(3) -0.0001(3) -0.0001(3) N4 0.0109(3) 0.0010(3) 0.0060(3) 0.0000(2) -0.0030(3) -0.0010(3) N10 0.0043(3) 0.0193(4) 0.0164(4) 0.0030(3) -0.0031(3) 0.0047(3) C1 0.0139(5) 0.0200(5) 0.0121(4) 0.0050(4) -0.0052(4) -0.0040(4) C2 0.0151(5) 0.0462(7) 0.0069(4) 0.0071(4) 0.0061(4) 0.0001(5) C3 0.0102(5) 0.0492(8) 0.0174(5) 0.0012(5) 0.0061(4) -0.0031(4) C4 0.0069(4) 0.0419(7) 0.0150(5) -0.0009(4) 0.0020(4) 0.0050(4) C5 0.0128(4) 0.0150(4) 0.0091(4) -0.0050(3) -0.0020(3) -0.0040(3) C6 0.0089(4) 0.0141(4) 0.0090(4) -0.0038(3) 0.0003(3) -0.0030(4) C7 0.0068(4) 0.0120(4) 0.0120(4) 0.0020(3) -0.0019(3) -0.0030(3) C8 0.0139(4) 0.0140(4) 0.0060(4) -0.0020(3) -0.0010(3) -0.0010(3) C9 0.0050(4) 0.0250(5) 0.0169(5) 0.0030(4) -0.0019(3) 0.0041(4) C10 0.0102(4) 0.0293(6) 0.0152(5) 0.0042(4) -0.0090(4) 0.0018(4) C11 0.0151(5) 0.0252(5) 0.0058(4) 0.0020(4) -0.0070(3) 0.0050(4) C12 0.0138(4) 0.0050(4) 0.0111(4) -0.0011(3) 0.0041(3) -0.0040(3) C13 0.0090(4) 0.0150(4) 0.0039(4) 0.0020(3) 0.0010(3) 0.0050(3) C14 0.0147(5) 0.0140(5) 0.0270(6) -0.0011(4) 0.0090(4) -0.0011(4) C15 0.0229(6) 0.0261(6) 0.0450(8) -0.0020(5) 0.0083(5) 0.0052(5) C16 0.0102(5) 0.0391(7) 0.0587(9) 0.0010(6) 0.0112(5) 0.0062(5) C17 0.0120(5) 0.0280(6) 0.0650(10) -0.0109(6) 0.0113(5) -0.0041(5) C18 0.0121(5) 0.0248(5) 0.0343(6) -0.0051(5) -0.0001(4) 0.0061(4) C19 0.0078(4) 0.0089(4) 0.0130(4) 0.0010(3) 0.0040(3) 0.0000(3) C20 0.0180(5) 0.0189(5) 0.0160(5) 0.0069(4) 0.0068(4) 0.0039(4) C21 0.0238(6) 0.0382(7) 0.0250(6) 0.0059(5) 0.0071(5) 0.0059(5) C22 0.0171(6) 0.0330(7) 0.0478(8) 0.0158(6) 0.0191(5) 0.0050(5) C23 0.0150(5) 0.0269(6) 0.0389(7) 0.0039(5) -0.0051(5) -0.0041(4) C24 0.0190(5) 0.0109(4) 0.0199(5) 0.0008(4) 0.0079(4) 0.0069(4) C25 0.0038(4) 0.0179(4) 0.0122(4) 0.0059(4) -0.0020(3) 0.0008(3) C26 0.0163(5) 0.0170(5) 0.0444(7) 0.0037(5) -0.0103(5) 0.0010(4) C27 0.0161(6) 0.0370(7) 0.0632(10) 0.0191(7) -0.0200(6) -0.0131(5) C28 0.0090(5) 0.0810(11) 0.0248(6) 0.0188(7) 0.0109(4) 0.0169(6) C29 0.0381(8) 0.0803(12) 0.0200(6) -0.0019(7) 0.0091(5) 0.0338(8) C30 0.0210(5) 0.0469(7) 0.0150(5) -0.0060(5) -0.0031(4) 0.0129(5) _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 O9 1.9181(7) 2 ? Cu1 O1 1.9684(6) . ? Cu1 N2 1.9736(8) . ? Cu1 N1 2.0794(8) . ? Cu1 O90 2.2581(8) . ? Cu2 O8 1.9225(7) . ? Cu2 N3 1.9567(8) 2_545 ? Cu2 O7 1.9809(7) 3_565 ? Cu2 N4 2.0385(8) 2_545 ? Cu2 O7 2.2968(8) . ? V1 O4 1.5897(7) . ? V1 O10 1.9345(7) 3_565 ? V1 O3 1.9459(7) . ? V1 O2 1.9751(6) 3_575 ? V1 O5 2.0029(7) . ? P1 O2 1.5173(6) . ? P1 O3 1.5204(6) . ? P1 O1 1.5309(6) . ? P1 C13 1.7844(9) . ? P2 O5 1.5120(7) . ? P2 O7 1.5197(7) . ? P2 O6 1.5751(7) . ? P2 C19 1.7915(9) . ? P3 O9 1.5113(7) . ? P3 O8 1.5181(7) . ? P3 O10 1.5311(7) . ? P3 C25 1.8092(9) . ? O2 V1 1.9751(6) 3_575 ? O7 Cu2 1.9809(7) 3_565 ? O9 Cu1 1.9181(7) 2_545 ? O10 V1 1.9344(7) 3_565 ? N1 C1 1.3409(13) . ? N1 C5 1.3466(13) . ? N2 C6 1.3432(13) . ? N2 N3 1.3560(11) . ? N3 C7 1.3328(12) . ? N3 Cu2 1.9568(8) 2 ? N4 C12 1.3430(12) . ? N4 C8 1.3572(12) . ? N4 Cu2 2.0384(8) 2 ? N10 C7 1.3391(13) . ? N10 C6 1.3392(12) . ? C1 C2 1.3783(14) . ? C2 C3 1.3842(16) . ? C3 C4 1.3835(16) . ? C4 C5 1.3802(14) . ? C5 C6 1.4677(13) . ? C7 C8 1.4598(12) . ? C8 C9 1.3749(13) . ? C9 C10 1.3761(14) . ? C10 C11 1.3811(15) . ? C11 C12 1.3735(13) . ? C13 C14 1.3919(14) . ? C13 C18 1.3993(15) . ? C14 C15 1.3780(16) . ? C15 C16 1.365(2) . ? C16 C17 1.3894(19) . ? C17 C18 1.3619(16) . ? C19 C24 1.3786(15) . ? C19 C20 1.4059(13) . ? C20 C21 1.3729(16) . ? C21 C22 1.378(2) . ? C22 C23 1.381(2) . ? C23 C24 1.4012(16) . ? C25 C26 1.3704(15) . ? C25 C30 1.3807(15) . ? C26 C27 1.3967(16) . ? C27 C28 1.372(2) . ? C28 C29 1.360(3) . ? C29 C30 1.3968(19) . ? 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 O9 Cu1 O1 85.04(3) 2 . ? O9 Cu1 N2 99.33(3) 2 . ? O1 Cu1 N2 165.57(3) . . ? O9 Cu1 N1 156.41(3) 2 . ? O1 Cu1 N1 91.41(3) . . ? N2 Cu1 N1 79.06(3) . . ? O9 Cu1 O90 105.02(3) 2 . ? O1 Cu1 O90 98.26(3) . . ? N2 Cu1 O90 93.90(3) . . ? N1 Cu1 O90 98.57(3) . . ? O8 Cu2 N3 96.26(3) . 2_545 ? O8 Cu2 O7 89.25(3) . 3_565 ? N3 Cu2 O7 172.95(3) 2_545 3_565 ? O8 Cu2 N4 171.39(3) . 2_545 ? N3 Cu2 N4 80.55(3) 2_545 2_545 ? O7 Cu2 N4 93.37(3) 3_565 2_545 ? O8 Cu2 O7 94.39(3) . . ? N3 Cu2 O7 97.21(3) 2_545 . ? O7 Cu2 O7 86.69(3) 3_565 . ? N4 Cu2 O7 93.94(3) 2_545 . ? O4 V1 O10 113.32(3) . 3_565 ? O4 V1 O3 114.23(3) . . ? O10 V1 O3 132.37(3) 3_565 . ? O4 V1 O2 100.33(3) . 3_575 ? O10 V1 O2 82.02(3) 3_565 3_575 ? O3 V1 O2 87.04(3) . 3_575 ? O4 V1 O5 100.14(3) . . ? O10 V1 O5 89.64(3) 3_565 . ? O3 V1 O5 84.85(3) . . ? O2 V1 O5 159.53(3) 3_575 . ? O2 P1 O3 113.02(4) . . ? O2 P1 O1 109.28(4) . . ? O3 P1 O1 110.86(4) . . ? O2 P1 C13 107.77(4) . . ? O3 P1 C13 105.03(4) . . ? O1 P1 C13 110.78(4) . . ? O5 P2 O7 115.18(4) . . ? O5 P2 O6 110.52(4) . . ? O7 P2 O6 107.69(4) . . ? O5 P2 C19 106.39(4) . . ? O7 P2 C19 111.31(4) . . ? O6 P2 C19 105.33(4) . . ? O9 P3 O8 112.89(4) . . ? O9 P3 O10 110.76(4) . . ? O8 P3 O10 112.16(4) . . ? O9 P3 C25 105.45(4) . . ? O8 P3 C25 108.69(4) . . ? O10 P3 C25 106.44(4) . . ? P1 O1 Cu1 128.08(4) . . ? P1 O2 V1 134.33(4) . 3_575 ? P1 O3 V1 136.60(4) . . ? P2 O5 V1 134.41(4) . . ? P2 O7 Cu2 119.10(4) . 3_565 ? P2 O7 Cu2 145.59(4) . . ? Cu2 O7 Cu2 93.31(3) 3_565 . ? P3 O8 Cu2 124.47(4) . . ? P3 O9 Cu1 134.86(4) . 2_545 ? P3 O10 V1 137.82(4) . 3_565 ? C1 N1 C5 117.55(9) . . ? C1 N1 Cu1 127.59(7) . . ? C5 N1 Cu1 114.85(6) . . ? C6 N2 N3 104.81(7) . . ? C6 N2 Cu1 116.55(6) . . ? N3 N2 Cu1 138.38(6) . . ? C7 N3 N2 105.93(7) . . ? C7 N3 Cu2 115.60(6) . 2 ? N2 N3 Cu2 137.57(6) . 2 ? C12 N4 C8 118.45(8) . . ? C12 N4 Cu2 127.04(6) . 2 ? C8 N4 Cu2 114.22(6) . 2 ? C7 N10 C6 100.91(8) . . ? N1 C1 C2 123.51(9) . . ? C1 C2 C3 117.83(10) . . ? C4 C3 C2 119.96(10) . . ? C5 C4 C3 118.10(10) . . ? N1 C5 C4 123.00(9) . . ? N1 C5 C6 112.80(9) . . ? C4 C5 C6 124.18(9) . . ? N10 C6 N2 114.26(8) . . ? N10 C6 C5 129.48(9) . . ? N2 C6 C5 116.06(9) . . ? N3 C7 N10 114.08(8) . . ? N3 C7 C8 116.72(8) . . ? N10 C7 C8 129.09(8) . . ? N4 C8 C9 121.71(9) . . ? N4 C8 C7 112.46(8) . . ? C9 C8 C7 125.82(9) . . ? C8 C9 C10 119.55(9) . . ? C9 C10 C11 118.70(9) . . ? C12 C11 C10 119.57(9) . . ? N4 C12 C11 121.99(9) . . ? C14 C13 C18 117.15(9) . . ? C14 C13 P1 123.49(8) . . ? C18 C13 P1 119.33(8) . . ? C15 C14 C13 121.81(11) . . ? C16 C15 C14 119.19(12) . . ? C15 C16 C17 120.81(11) . . ? C18 C17 C16 119.45(12) . . ? C17 C18 C13 121.56(11) . . ? C24 C19 C20 119.71(9) . . ? C24 C19 P2 119.24(7) . . ? C20 C19 P2 120.79(8) . . ? C21 C20 C19 119.80(11) . . ? C20 C21 C22 120.74(12) . . ? C21 C22 C23 119.96(11) . . ? C22 C23 C24 120.07(12) . . ? C19 C24 C23 119.69(10) . . ? C26 C25 C30 118.32(10) . . ? C26 C25 P3 120.34(8) . . ? C30 C25 P3 121.32(8) . . ? C25 C26 C27 121.14(13) . . ? C28 C27 C26 119.75(13) . . ? C29 C28 C27 119.84(11) . . ? C28 C29 C30 120.29(13) . . ? C25 C30 C29 120.63(13) . . ? 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 P1 O1 Cu1 27.10(6) . . . . ? O3 P1 O1 Cu1 152.32(4) . . . . ? C13 P1 O1 Cu1 -91.48(5) . . . . ? O9 Cu1 O1 P1 112.99(5) 2 . . . ? N2 Cu1 O1 P1 -138.60(11) . . . . ? N1 Cu1 O1 P1 -90.37(5) . . . . ? O90 Cu1 O1 P1 8.50(5) . . . . ? O3 P1 O2 V1 17.64(7) . . . 3_575 ? O1 P1 O2 V1 141.59(5) . . . 3_575 ? C13 P1 O2 V1 -97.96(6) . . . 3_575 ? O2 P1 O3 V1 105.34(6) . . . . ? O1 P1 O3 V1 -17.74(7) . . . . ? C13 P1 O3 V1 -137.44(6) . . . . ? O4 V1 O3 P1 -24.82(7) . . . . ? O10 V1 O3 P1 158.80(5) 3_565 . . . ? O2 V1 O3 P1 -124.81(6) 3_575 . . . ? O5 V1 O3 P1 74.00(6) . . . . ? O7 P2 O5 V1 -62.37(7) . . . . ? O6 P2 O5 V1 59.94(7) . . . . ? C19 P2 O5 V1 173.80(5) . . . . ? O4 V1 O5 P2 1.44(7) . . . . ? O10 V1 O5 P2 115.08(6) 3_565 . . . ? O3 V1 O5 P2 -112.30(6) . . . . ? O2 V1 O5 P2 -179.37(6) 3_575 . . . ? O5 P2 O7 Cu2 18.59(6) . . . 3_565 ? O6 P2 O7 Cu2 -105.22(5) . . . 3_565 ? C19 P2 O7 Cu2 139.80(5) . . . 3_565 ? O5 P2 O7 Cu2 -139.74(6) . . . . ? O6 P2 O7 Cu2 96.44(7) . . . . ? C19 P2 O7 Cu2 -18.54(9) . . . . ? O8 Cu2 O7 P2 -109.85(7) . . . . ? N3 Cu2 O7 P2 -12.96(8) 2_545 . . . ? O7 Cu2 O7 P2 161.15(9) 3_565 . . . ? N4 Cu2 O7 P2 68.00(7) 2_545 . . . ? O8 Cu2 O7 Cu2 89.00(3) . . . 3_565 ? N3 Cu2 O7 Cu2 -174.11(3) 2_545 . . 3_565 ? O7 Cu2 O7 Cu2 0.0 3_565 . . 3_565 ? N4 Cu2 O7 Cu2 -93.15(3) 2_545 . . 3_565 ? O9 P3 O8 Cu2 -96.25(5) . . . . ? O10 P3 O8 Cu2 29.72(6) . . . . ? C25 P3 O8 Cu2 147.13(5) . . . . ? N3 Cu2 O8 P3 52.72(5) 2_545 . . . ? O7 Cu2 O8 P3 -122.89(5) 3_565 . . . ? N4 Cu2 O8 P3 -15.0(2) 2_545 . . . ? O7 Cu2 O8 P3 150.49(5) . . . . ? O8 P3 O9 Cu1 38.83(7) . . . 2_545 ? O10 P3 O9 Cu1 -87.89(7) . . . 2_545 ? C25 P3 O9 Cu1 157.36(6) . . . 2_545 ? O9 P3 O10 V1 150.85(6) . . . 3_565 ? O8 P3 O10 V1 23.72(8) . . . 3_565 ? C25 P3 O10 V1 -95.02(7) . . . 3_565 ? O9 Cu1 N1 C1 95.77(11) 2 . . . ? O1 Cu1 N1 C1 14.97(9) . . . . ? N2 Cu1 N1 C1 -175.94(9) . . . . ? O90 Cu1 N1 C1 -83.59(9) . . . . ? O9 Cu1 N1 C5 -82.83(10) 2 . . . ? O1 Cu1 N1 C5 -163.64(7) . . . . ? N2 Cu1 N1 C5 5.46(7) . . . . ? O90 Cu1 N1 C5 97.80(7) . . . . ? O9 Cu1 N2 C6 148.43(7) 2 . . . ? O1 Cu1 N2 C6 41.76(17) . . . . ? N1 Cu1 N2 C6 -7.65(7) . . . . ? O90 Cu1 N2 C6 -105.64(7) . . . . ? O9 Cu1 N2 N3 -24.62(10) 2 . . . ? O1 Cu1 N2 N3 -131.29(11) . . . . ? N1 Cu1 N2 N3 179.29(10) . . . . ? O90 Cu1 N2 N3 81.31(10) . . . . ? C6 N2 N3 C7 0.64(10) . . . . ? Cu1 N2 N3 C7 174.22(8) . . . . ? C6 N2 N3 Cu2 168.70(8) . . . 2 ? Cu1 N2 N3 Cu2 -17.72(16) . . . 2 ? C5 N1 C1 C2 -1.66(16) . . . . ? Cu1 N1 C1 C2 179.76(9) . . . . ? N1 C1 C2 C3 1.11(19) . . . . ? C1 C2 C3 C4 0.9(2) . . . . ? C2 C3 C4 C5 -2.2(2) . . . . ? C1 N1 C5 C4 0.23(15) . . . . ? Cu1 N1 C5 C4 178.99(9) . . . . ? C1 N1 C5 C6 178.72(9) . . . . ? Cu1 N1 C5 C6 -2.52(10) . . . . ? C3 C4 C5 N1 1.66(18) . . . . ? C3 C4 C5 C6 -176.66(11) . . . . ? C7 N10 C6 N2 0.56(11) . . . . ? C7 N10 C6 C5 175.04(10) . . . . ? N3 N2 C6 N10 -0.78(11) . . . . ? Cu1 N2 C6 N10 -176.02(7) . . . . ? N3 N2 C6 C5 -176.04(8) . . . . ? Cu1 N2 C6 C5 8.72(11) . . . . ? N1 C5 C6 N10 -178.22(10) . . . . ? C4 C5 C6 N10 0.25(18) . . . . ? N1 C5 C6 N2 -3.82(13) . . . . ? C4 C5 C6 N2 174.66(10) . . . . ? N2 N3 C7 N10 -0.34(11) . . . . ? Cu2 N3 C7 N10 -171.44(7) 2 . . . ? N2 N3 C7 C8 176.21(8) . . . . ? Cu2 N3 C7 C8 5.12(11) 2 . . . ? C6 N10 C7 N3 -0.11(11) . . . . ? C6 N10 C7 C8 -176.15(10) . . . . ? C12 N4 C8 C9 0.97(14) . . . . ? Cu2 N4 C8 C9 -173.36(8) 2 . . . ? C12 N4 C8 C7 -179.35(8) . . . . ? Cu2 N4 C8 C7 6.32(10) 2 . . . ? N3 C7 C8 N4 -7.58(12) . . . . ? N10 C7 C8 N4 168.37(9) . . . . ? N3 C7 C8 C9 172.09(10) . . . . ? N10 C7 C8 C9 -11.97(17) . . . . ? N4 C8 C9 C10 0.10(16) . . . . ? C7 C8 C9 C10 -179.53(10) . . . . ? C8 C9 C10 C11 -1.39(16) . . . . ? C9 C10 C11 C12 1.61(17) . . . . ? C8 N4 C12 C11 -0.74(13) . . . . ? Cu2 N4 C12 C11 172.78(7) 2 . . . ? C10 C11 C12 N4 -0.56(15) . . . . ? O2 P1 C13 C14 -1.00(10) . . . . ? O3 P1 C13 C14 -121.74(9) . . . . ? O1 P1 C13 C14 118.50(9) . . . . ? O2 P1 C13 C18 176.75(8) . . . . ? O3 P1 C13 C18 56.00(9) . . . . ? O1 P1 C13 C18 -63.75(9) . . . . ? C18 C13 C14 C15 -2.05(17) . . . . ? P1 C13 C14 C15 175.74(10) . . . . ? C13 C14 C15 C16 2.1(2) . . . . ? C14 C15 C16 C17 -1.1(2) . . . . ? C15 C16 C17 C18 0.0(3) . . . . ? C16 C17 C18 C13 0.0(2) . . . . ? C14 C13 C18 C17 0.95(18) . . . . ? P1 C13 C18 C17 -176.93(11) . . . . ? O5 P2 C19 C24 57.26(9) . . . . ? O7 P2 C19 C24 -68.95(9) . . . . ? O6 P2 C19 C24 174.62(7) . . . . ? O5 P2 C19 C20 -116.99(8) . . . . ? O7 P2 C19 C20 116.80(8) . . . . ? O6 P2 C19 C20 0.37(9) . . . . ? C24 C19 C20 C21 0.44(16) . . . . ? P2 C19 C20 C21 174.66(9) . . . . ? C19 C20 C21 C22 0.54(18) . . . . ? C20 C21 C22 C23 -0.4(2) . . . . ? C21 C22 C23 C24 -0.65(19) . . . . ? C20 C19 C24 C23 -1.49(15) . . . . ? P2 C19 C24 C23 -175.81(8) . . . . ? C22 C23 C24 C19 1.61(17) . . . . ? O9 P3 C25 C26 -43.02(10) . . . . ? O8 P3 C25 C26 78.28(9) . . . . ? O10 P3 C25 C26 -160.73(9) . . . . ? O9 P3 C25 C30 138.73(9) . . . . ? O8 P3 C25 C30 -99.97(9) . . . . ? O10 P3 C25 C30 21.02(10) . . . . ? C30 C25 C26 C27 -0.99(18) . . . . ? P3 C25 C26 C27 -179.30(10) . . . . ? C25 C26 C27 C28 1.3(2) . . . . ? C26 C27 C28 C29 -1.6(2) . . . . ? C27 C28 C29 C30 1.7(2) . . . . ? C26 C25 C30 C29 1.08(18) . . . . ? P3 C25 C30 C29 179.36(11) . . . . ? C28 C29 C30 C25 -1.5(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.833 _refine_diff_density_min -1.294 _refine_diff_density_rms 0.279 data_3 _database_code_depnum_ccdc_archive 'CCDC 270526' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H9 Cu0.50 N O5 P V' _chemical_formula_weight 348.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 17.2481(12) _cell_length_b 26.2681(19) _cell_length_c 11.0818(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5020.9(6) _cell_formula_units_Z 16 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2792 _exptl_absorpt_coefficient_mu 1.757 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6678 _exptl_absorpt_correction_T_max 0.8439 _exptl_absorpt_process_details 'SADABS (Sheldrick, 97)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 87(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 'APEX CCD detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 16266 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 32.75 _reflns_number_total 4408 _reflns_number_gt 4238 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+33.2314P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.495(12) _refine_ls_number_reflns 4408 _refine_ls_number_parameters 179 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0816 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 Cu1 Cu 0.5000 0.0000 -0.00539(3) 0.00845(8) Uani 1 2 d S . . V1 V 0.52148(2) 0.137287(15) 0.03421(4) 0.00917(8) Uani 1 1 d . . . P1 P 0.35919(3) 0.08060(2) 0.02815(6) 0.00896(10) Uani 1 1 d . . . O1 O 0.39812(10) 0.03203(7) -0.00836(17) 0.0117(3) Uani 1 1 d . . . O2 O 0.29144(11) 0.09354(7) -0.05672(17) 0.0126(3) Uani 1 1 d . . . O3 O 0.41481(10) 0.12695(6) 0.02868(19) 0.0121(3) Uani 1 1 d . . . O4 O 0.56370(11) 0.08384(7) -0.00012(18) 0.0139(3) Uani 1 1 d . . . O5 O 0.54862(13) 0.17966(7) -0.06146(18) 0.0182(4) Uani 1 1 d . . . N1 N 0.5000 0.0000 0.1766(3) 0.0101(5) Uani 1 2 d S . . N2 N 0.5000 0.0000 0.8133(3) 0.0099(5) Uani 1 2 d S . . C1 C 0.55609(14) 0.02430(9) 0.2384(2) 0.0116(4) Uani 1 1 d . . . H1 H 0.5964 0.0408 0.1949 0.014 Uiso 1 1 calc R . . C2 C 0.55697(16) 0.02601(10) 0.3630(2) 0.0124(4) Uani 1 1 d . . . H2 H 0.5960 0.0447 0.4042 0.015 Uiso 1 1 calc R . . C3 C 0.5000 0.0000 0.4277(3) 0.0106(6) Uani 1 2 d S . . C4 C 0.5000 0.0000 0.5613(3) 0.0118(6) Uani 1 2 d S . . C5 C 0.49381(17) 0.04530(10) 0.6257(2) 0.0151(5) Uani 1 1 d . . . H5 H 0.4900 0.0769 0.5846 0.018 Uiso 1 1 calc R . . C6 C 0.49328(16) 0.04351(10) 0.7510(2) 0.0150(5) Uani 1 1 d . . . H6 H 0.4879 0.0745 0.7944 0.018 Uiso 1 1 calc R . . C7 C 0.31801(15) 0.07583(10) 0.1760(2) 0.0117(4) Uani 1 1 d . . . C8 C 0.35864(15) 0.09304(10) 0.2773(3) 0.0147(4) Uani 1 1 d . . . H8 H 0.4070 0.1099 0.2678 0.018 Uiso 1 1 calc R . . C9 C 0.32803(18) 0.08539(11) 0.3925(2) 0.0181(5) Uani 1 1 d . . . H9 H 0.3556 0.0969 0.4615 0.022 Uiso 1 1 calc R . . C10 C 0.25710(18) 0.06086(11) 0.4059(3) 0.0194(5) Uani 1 1 d . . . H10 H 0.2362 0.0557 0.4843 0.023 Uiso 1 1 calc R . . C11 C 0.21679(19) 0.04393(12) 0.3060(2) 0.0215(6) Uani 1 1 d . . . H11 H 0.1682 0.0274 0.3159 0.026 Uiso 1 1 calc R . . C12 C 0.24711(17) 0.05102(12) 0.1906(3) 0.0180(5) Uani 1 1 d . . . H12 H 0.2196 0.0390 0.1221 0.022 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 0.01088(17) 0.01000(17) 0.00447(15) 0.000 0.000 0.00160(16) V1 0.01077(16) 0.00959(16) 0.00714(15) -0.00011(14) -0.00043(14) -0.00077(14) P1 0.0098(2) 0.0101(2) 0.0070(2) 0.0003(2) -0.0004(2) 0.00087(19) O1 0.0131(8) 0.0118(7) 0.0102(7) -0.0020(6) 0.0005(6) 0.0011(6) O2 0.0117(8) 0.0159(8) 0.0102(8) 0.0024(6) -0.0014(7) 0.0007(7) O3 0.0116(7) 0.0105(7) 0.0143(8) -0.0003(7) -0.0016(7) -0.0004(6) O4 0.0146(8) 0.0134(7) 0.0136(8) -0.0010(7) 0.0002(6) 0.0008(6) O5 0.0245(10) 0.0166(9) 0.0135(9) 0.0041(7) 0.0002(7) -0.0034(8) N1 0.0119(13) 0.0101(12) 0.0083(13) 0.000 0.000 0.0004(10) N2 0.0119(13) 0.0111(13) 0.0067(13) 0.000 0.000 -0.0002(10) C1 0.0140(10) 0.0117(9) 0.0092(9) 0.0011(8) 0.0013(8) -0.0022(8) C2 0.0170(11) 0.0135(10) 0.0068(10) 0.0000(8) -0.0017(8) -0.0026(9) C3 0.0141(15) 0.0101(14) 0.0078(15) 0.000 0.000 -0.0008(11) C4 0.0151(15) 0.0132(15) 0.0069(15) 0.000 0.000 -0.0010(12) C5 0.0260(13) 0.0115(10) 0.0078(10) 0.0011(8) -0.0015(9) 0.0000(10) C6 0.0238(12) 0.0129(10) 0.0084(10) -0.0016(8) -0.0013(9) 0.0005(9) C7 0.0140(10) 0.0127(10) 0.0083(9) 0.0001(8) 0.0007(8) 0.0039(8) C8 0.0166(11) 0.0171(10) 0.0105(10) -0.0009(9) -0.0002(9) 0.0017(8) C9 0.0223(13) 0.0220(13) 0.0101(11) -0.0004(10) -0.0003(10) 0.0035(11) C10 0.0255(14) 0.0211(12) 0.0117(11) 0.0019(10) 0.0047(10) 0.0047(11) C11 0.0250(14) 0.0253(13) 0.0143(13) 0.0010(10) 0.0056(10) -0.0063(11) C12 0.0196(13) 0.0219(13) 0.0124(12) -0.0003(9) 0.0013(10) -0.0048(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 Cu1 O1 1.9486(18) 2_655 ? Cu1 O1 1.9486(18) . ? Cu1 N2 2.009(3) 1_554 ? Cu1 N1 2.017(3) . ? V1 O5 1.607(2) . ? V1 O4 1.6268(19) . ? V1 O3 1.8607(18) . ? V1 O2 1.8654(19) 3 ? P1 O1 1.4975(19) . ? P1 O2 1.5380(19) . ? P1 O3 1.5502(18) . ? P1 C7 1.790(3) . ? O2 V1 1.8654(19) 11_454 ? N1 C1 1.346(3) 2_655 ? N1 C1 1.346(3) . ? N2 C6 1.341(3) 2_655 ? N2 C6 1.341(3) . ? N2 Cu1 2.009(3) 1_556 ? C1 C2 1.382(4) . ? C2 C3 1.395(3) . ? C3 C2 1.395(3) 2_655 ? C3 C4 1.480(4) . ? C4 C5 1.392(3) . ? C4 C5 1.392(3) 2_655 ? C5 C6 1.389(4) . ? C7 C12 1.395(4) . ? C7 C8 1.399(4) . ? C8 C9 1.395(4) . ? C9 C10 1.391(4) . ? C10 C11 1.381(4) . ? C11 C12 1.394(4) . ? 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 Cu1 O1 178.06(11) 2_655 . ? O1 Cu1 N2 89.03(6) 2_655 1_554 ? O1 Cu1 N2 89.03(6) . 1_554 ? O1 Cu1 N1 90.97(6) 2_655 . ? O1 Cu1 N1 90.97(6) . . ? N2 Cu1 N1 180.0 1_554 . ? O5 V1 O4 108.25(10) . . ? O5 V1 O3 111.56(10) . . ? O4 V1 O3 108.00(9) . . ? O5 V1 O2 112.50(10) . 3 ? O4 V1 O2 111.81(9) . 3 ? O3 V1 O2 104.66(9) . 3 ? O1 P1 O2 111.33(11) . . ? O1 P1 O3 113.12(10) . . ? O2 P1 O3 107.40(11) . . ? O1 P1 C7 111.44(11) . . ? O2 P1 C7 105.88(11) . . ? O3 P1 C7 107.28(12) . . ? P1 O1 Cu1 140.15(12) . . ? P1 O2 V1 141.06(12) . 11_454 ? P1 O3 V1 136.61(11) . . ? C1 N1 C1 118.8(3) 2_655 . ? C1 N1 Cu1 120.58(16) 2_655 . ? C1 N1 Cu1 120.58(16) . . ? C6 N2 C6 117.9(3) 2_655 . ? C6 N2 Cu1 121.03(16) 2_655 1_556 ? C6 N2 Cu1 121.03(16) . 1_556 ? N1 C1 C2 122.1(3) . . ? C1 C2 C3 119.3(3) . . ? C2 C3 C2 118.1(3) 2_655 . ? C2 C3 C4 120.93(16) 2_655 . ? C2 C3 C4 120.94(16) . . ? C5 C4 C5 118.3(3) . 2_655 ? C5 C4 C3 120.85(16) . . ? C5 C4 C3 120.85(16) 2_655 . ? C6 C5 C4 118.9(3) . . ? N2 C6 C5 122.9(2) . . ? C12 C7 C8 119.8(2) . . ? C12 C7 P1 119.1(2) . . ? C8 C7 P1 120.9(2) . . ? C9 C8 C7 119.9(2) . . ? C10 C9 C8 119.8(3) . . ? C11 C10 C9 120.4(3) . . ? C10 C11 C12 120.2(3) . . ? C11 C12 C7 119.9(3) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 32.75 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.609 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.096 data_4 _database_code_depnum_ccdc_archive 'CCDC 270527' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H13 Cu N2 O8 P2 V' _chemical_formula_weight 537.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.0833(7) _cell_length_b 11.5444(10) _cell_length_c 10.5565(9) _cell_angle_alpha 90.00 _cell_angle_beta 108.335(2) _cell_angle_gamma 90.00 _cell_volume 935.09(14) _cell_formula_units_Z 2 _cell_measurement_temperature 87(2) _cell_measurement_reflns_used 3973 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 28.20 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.910 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 538 _exptl_absorpt_coefficient_mu 1.859 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8505 _exptl_absorpt_correction_T_max 0.9128 _exptl_absorpt_process_details 'SADABS (Sheldrick, 97)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 87(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 'APEX CCD detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 9942 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 28.32 _reflns_number_total 4576 _reflns_number_gt 4412 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0521P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(4) _refine_ls_number_reflns 4576 _refine_ls_number_parameters 273 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.60758(4) 0.33336(3) 1.05187(3) 0.01038(9) Uani 1 1 d . . . V1 V 0.89275(6) 0.16316(4) 0.92352(5) 0.00997(11) Uani 1 1 d . . . P1 P 0.86191(9) 0.44769(6) 0.91367(7) 0.00907(14) Uani 1 1 d . . . P2 P 0.71667(9) 0.73007(6) 0.87102(7) 0.01053(15) Uani 1 1 d . . . O1 O 0.7351(3) 0.17708(18) 0.9881(2) 0.0165(5) Uani 1 1 d . . . O2 O 0.8147(3) 0.11475(19) 0.7727(2) 0.0192(5) Uani 1 1 d . . . O3 O 0.9003(2) 0.32587(18) 0.87524(19) 0.0129(4) Uani 1 1 d . . . O4 O 1.0371(3) 0.50452(17) 0.9930(2) 0.0131(4) Uani 1 1 d . . . O5 O 0.7314(3) 0.45122(18) 0.9905(2) 0.0107(4) Uani 1 1 d . . . O6 O 0.8545(3) 0.68934(17) 0.9959(2) 0.0129(4) Uani 1 1 d . . . O7 O 0.5354(3) 0.7308(2) 0.8813(2) 0.0164(4) Uani 1 1 d . . . O8 O 0.7646(3) 0.85111(19) 0.8255(2) 0.0238(5) Uani 1 1 d . . . H8 H 0.8480 0.8798 0.8865 0.036 Uiso 1 1 calc R . . N1 N 0.4169(3) 0.3402(2) 0.8768(2) 0.0120(4) Uani 1 1 d . . . N2 N -0.2157(3) 0.3398(2) 0.2382(2) 0.0120(4) Uani 1 1 d . . . C1 C 0.3525(4) 0.2404(3) 0.8163(3) 0.0176(6) Uani 1 1 d . . . H1 H 0.3949 0.1695 0.8601 0.021 Uiso 1 1 calc R . . C2 C 0.2259(4) 0.2371(3) 0.6917(3) 0.0155(6) Uani 1 1 d . . . H2 H 0.1839 0.1650 0.6508 0.019 Uiso 1 1 calc R . . C3 C 0.1617(3) 0.3402(3) 0.6279(3) 0.0137(5) Uani 1 1 d . . . C4 C 0.2249(4) 0.4437(3) 0.6940(3) 0.0195(7) Uani 1 1 d . . . H4 H 0.1803 0.5159 0.6548 0.023 Uiso 1 1 calc R . . C5 C 0.3530(4) 0.4404(3) 0.8173(3) 0.0178(6) Uani 1 1 d . . . H5 H 0.3967 0.5111 0.8609 0.021 Uiso 1 1 calc R . . C6 C -0.2172(4) 0.2583(2) 0.3298(3) 0.0146(6) Uani 1 1 d . . . H6 H -0.3045 0.1999 0.3059 0.018 Uiso 1 1 calc R . . C7 C -0.0984(4) 0.2559(3) 0.4556(3) 0.0144(6) Uani 1 1 d . . . H7 H -0.1041 0.1967 0.5166 0.017 Uiso 1 1 calc R . . C8 C 0.0308(3) 0.3410(3) 0.4936(3) 0.0119(5) Uani 1 1 d . . . C9 C 0.0333(4) 0.4246(3) 0.3995(3) 0.0152(6) Uani 1 1 d . . . H9 H 0.1200 0.4834 0.4208 0.018 Uiso 1 1 calc R . . C10 C -0.0908(4) 0.4218(3) 0.2749(3) 0.0148(6) Uani 1 1 d . . . H10 H -0.0881 0.4803 0.2123 0.018 Uiso 1 1 calc R . . C11 C 0.7052(4) 0.6348(2) 0.7341(3) 0.0105(5) Uani 1 1 d . . . C12 C 0.6147(4) 0.6746(3) 0.6062(3) 0.0155(6) Uani 1 1 d . . . H12 H 0.5815 0.7537 0.5942 0.019 Uiso 1 1 calc R . . C13 C 0.5720(5) 0.6020(3) 0.4969(3) 0.0222(7) Uani 1 1 d . . . H13 H 0.5058 0.6298 0.4112 0.027 Uiso 1 1 calc R . . C14 C 0.6282(5) 0.4867(3) 0.5147(3) 0.0221(7) Uani 1 1 d . . . H14 H 0.6019 0.4356 0.4405 0.027 Uiso 1 1 calc R . . C15 C 0.7216(4) 0.4474(3) 0.6402(3) 0.0176(6) Uani 1 1 d . . . H15 H 0.7598 0.3691 0.6504 0.021 Uiso 1 1 calc R . . C16 C 0.7619(4) 0.5187(2) 0.7529(3) 0.0105(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.00759(16) 0.01403(17) 0.00766(15) 0.00209(13) -0.00026(11) -0.00276(13) V1 0.0076(2) 0.0075(2) 0.0125(2) -0.00078(18) -0.00012(17) 0.00017(17) P1 0.0082(3) 0.0074(3) 0.0102(3) 0.0007(3) 0.0010(3) -0.0001(3) P2 0.0088(3) 0.0080(3) 0.0133(3) -0.0011(3) 0.0014(3) 0.0008(3) O1 0.0138(10) 0.0085(9) 0.0283(12) 0.0029(9) 0.0083(9) 0.0014(8) O2 0.0226(12) 0.0122(10) 0.0175(12) -0.0027(9) -0.0013(10) -0.0008(9) O3 0.0136(9) 0.0077(9) 0.0165(9) 0.0004(8) 0.0036(7) 0.0020(8) O4 0.0084(10) 0.0110(10) 0.0173(11) -0.0028(8) 0.0002(8) -0.0004(8) O5 0.0120(9) 0.0087(9) 0.0103(10) 0.0026(8) 0.0018(8) -0.0008(8) O6 0.0095(10) 0.0124(10) 0.0149(10) -0.0024(8) 0.0011(8) 0.0010(7) O7 0.0077(10) 0.0258(11) 0.0134(10) -0.0055(9) 0.0001(8) 0.0056(9) O8 0.0319(13) 0.0122(11) 0.0204(11) -0.0002(9) -0.0017(10) -0.0070(10) N1 0.0121(10) 0.0132(11) 0.0079(10) 0.0011(10) -0.0008(8) -0.0015(10) N2 0.0130(10) 0.0112(10) 0.0092(10) -0.0009(10) -0.0003(8) -0.0004(10) C1 0.0207(16) 0.0149(14) 0.0127(15) 0.0012(12) -0.0014(12) -0.0014(12) C2 0.0174(15) 0.0124(13) 0.0141(15) -0.0009(11) 0.0010(12) -0.0031(12) C3 0.0108(12) 0.0185(14) 0.0098(12) -0.0012(13) 0.0007(10) -0.0042(13) C4 0.0216(16) 0.0100(13) 0.0176(16) 0.0026(13) -0.0070(13) -0.0015(13) C5 0.0200(16) 0.0152(14) 0.0133(15) -0.0047(12) -0.0020(13) -0.0037(13) C6 0.0141(14) 0.0128(13) 0.0152(14) -0.0013(11) 0.0021(11) -0.0037(11) C7 0.0171(15) 0.0120(13) 0.0117(14) 0.0035(10) 0.0011(12) -0.0024(11) C8 0.0111(12) 0.0142(13) 0.0082(11) 0.0004(12) -0.0001(9) 0.0009(12) C9 0.0112(14) 0.0168(15) 0.0144(14) -0.0002(11) -0.0005(11) -0.0065(11) C10 0.0137(14) 0.0174(14) 0.0117(14) 0.0014(11) 0.0016(11) -0.0036(11) C11 0.0093(12) 0.0106(12) 0.0131(14) -0.0003(10) 0.0058(11) -0.0001(10) C12 0.0181(15) 0.0142(14) 0.0150(14) 0.0035(12) 0.0065(12) 0.0039(12) C13 0.0287(17) 0.0261(17) 0.0104(14) 0.0033(13) 0.0043(13) 0.0035(14) C14 0.034(2) 0.0218(16) 0.0116(15) -0.0033(12) 0.0079(14) -0.0001(14) C15 0.0263(17) 0.0131(13) 0.0150(15) 0.0012(12) 0.0089(13) 0.0034(13) C16 0.0098(13) 0.0125(13) 0.0106(13) 0.0020(10) 0.0054(11) 0.0004(11) _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 O5 1.919(2) . ? Cu1 O7 1.936(2) 2_647 ? Cu1 N1 2.001(2) . ? Cu1 N2 2.037(2) 1_656 ? Cu1 O1 2.282(2) . ? V1 O2 1.617(2) . ? V1 O1 1.631(2) . ? V1 O3 1.952(2) . ? V1 O6 1.974(2) 2_747 ? V1 O4 2.034(2) 2_747 ? P1 O5 1.520(2) . ? P1 O3 1.523(2) . ? P1 O4 1.546(2) . ? P1 C16 1.829(3) . ? P2 O7 1.503(2) . ? P2 O6 1.509(2) . ? P2 O8 1.566(2) . ? P2 C11 1.795(3) . ? O4 V1 2.034(2) 2_757 ? O6 V1 1.974(2) 2_757 ? O7 Cu1 1.936(2) 2_657 ? N1 C5 1.340(4) . ? N1 C1 1.340(4) . ? N2 C10 1.349(4) . ? N2 C6 1.352(4) . ? N2 Cu1 2.037(2) 1_454 ? C1 C2 1.390(4) . ? C2 C3 1.386(4) . ? C3 C4 1.397(4) . ? C3 C8 1.478(4) . ? C4 C5 1.385(4) . ? C6 C7 1.373(4) . ? C7 C8 1.398(4) . ? C8 C9 1.390(4) . ? C9 C10 1.381(4) . ? C11 C12 1.395(4) . ? C11 C16 1.410(4) . ? C12 C13 1.379(5) . ? C13 C14 1.400(5) . ? C14 C15 1.378(4) . ? C15 C16 1.399(4) . ? 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 O5 Cu1 O7 172.50(9) . 2_647 ? O5 Cu1 N1 89.57(9) . . ? O7 Cu1 N1 89.20(9) 2_647 . ? O5 Cu1 N2 91.05(9) . 1_656 ? O7 Cu1 N2 89.31(9) 2_647 1_656 ? N1 Cu1 N2 173.19(10) . 1_656 ? O5 Cu1 O1 97.41(8) . . ? O7 Cu1 O1 90.04(9) 2_647 . ? N1 Cu1 O1 92.70(10) . . ? N2 Cu1 O1 93.95(9) 1_656 . ? O2 V1 O1 109.37(12) . . ? O2 V1 O3 96.32(10) . . ? O1 V1 O3 96.16(9) . . ? O2 V1 O6 120.51(11) . 2_747 ? O1 V1 O6 130.06(10) . 2_747 ? O3 V1 O6 81.48(8) . 2_747 ? O2 V1 O4 94.85(10) . 2_747 ? O1 V1 O4 93.18(9) . 2_747 ? O3 V1 O4 162.17(8) . 2_747 ? O6 V1 O4 80.88(8) 2_747 2_747 ? O5 P1 O3 113.64(12) . . ? O5 P1 O4 111.76(12) . . ? O3 P1 O4 107.90(11) . . ? O5 P1 C16 107.76(12) . . ? O3 P1 C16 103.56(12) . . ? O4 P1 C16 111.99(13) . . ? O7 P2 O6 114.05(12) . . ? O7 P2 O8 110.99(14) . . ? O6 P2 O8 111.12(12) . . ? O7 P2 C11 104.89(13) . . ? O6 P2 C11 110.46(12) . . ? O8 P2 C11 104.75(13) . . ? V1 O1 Cu1 133.30(12) . . ? P1 O3 V1 142.50(13) . . ? P1 O4 V1 134.39(12) . 2_757 ? P1 O5 Cu1 133.20(13) . . ? P2 O6 V1 143.51(14) . 2_757 ? P2 O7 Cu1 137.46(15) . 2_657 ? C5 N1 C1 118.9(2) . . ? C5 N1 Cu1 122.6(2) . . ? C1 N1 Cu1 118.5(2) . . ? C10 N2 C6 117.2(2) . . ? C10 N2 Cu1 122.49(19) . 1_454 ? C6 N2 Cu1 120.2(2) . 1_454 ? N1 C1 C2 122.3(3) . . ? C3 C2 C1 119.2(3) . . ? C2 C3 C4 118.0(2) . . ? C2 C3 C8 121.2(3) . . ? C4 C3 C8 120.9(3) . . ? C5 C4 C3 119.6(3) . . ? N1 C5 C4 121.9(3) . . ? N2 C6 C7 123.0(3) . . ? C6 C7 C8 119.7(3) . . ? C9 C8 C7 117.4(2) . . ? C9 C8 C3 121.5(3) . . ? C7 C8 C3 121.0(3) . . ? C10 C9 C8 119.7(3) . . ? N2 C10 C9 122.9(3) . . ? C12 C11 C16 119.8(3) . . ? C12 C11 P2 117.1(2) . . ? C16 C11 P2 122.5(2) . . ? C13 C12 C11 121.8(3) . . ? C12 C13 C14 118.7(3) . . ? C15 C14 C13 119.9(3) . . ? C14 C15 C16 122.3(3) . . ? C15 C16 C11 117.5(3) . . ? C15 C16 P1 116.2(2) . . ? C11 C16 P1 125.9(2) . . ? 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 V1 O1 Cu1 -112.59(17) . . . . ? O3 V1 O1 Cu1 -13.66(17) . . . . ? O6 V1 O1 Cu1 70.4(2) 2_747 . . . ? O4 V1 O1 Cu1 151.13(16) 2_747 . . . ? O5 Cu1 O1 V1 4.95(17) . . . . ? O7 Cu1 O1 V1 -175.94(17) 2_647 . . . ? N1 Cu1 O1 V1 94.86(18) . . . . ? N2 Cu1 O1 V1 -86.63(18) 1_656 . . . ? O5 P1 O3 V1 -22.4(2) . . . . ? O4 P1 O3 V1 102.1(2) . . . . ? C16 P1 O3 V1 -139.02(19) . . . . ? O2 V1 O3 P1 137.4(2) . . . . ? O1 V1 O3 P1 27.0(2) . . . . ? O6 V1 O3 P1 -102.6(2) 2_747 . . . ? O4 V1 O3 P1 -94.1(3) 2_747 . . . ? O5 P1 O4 V1 -56.2(2) . . . 2_757 ? O3 P1 O4 V1 178.15(16) . . . 2_757 ? C16 P1 O4 V1 64.8(2) . . . 2_757 ? O3 P1 O5 Cu1 1.2(2) . . . . ? O4 P1 O5 Cu1 -121.17(16) . . . . ? C16 P1 O5 Cu1 115.37(17) . . . . ? O7 Cu1 O5 P1 -168.6(6) 2_647 . . . ? N1 Cu1 O5 P1 -88.10(18) . . . . ? N2 Cu1 O5 P1 98.69(18) 1_656 . . . ? O1 Cu1 O5 P1 4.57(17) . . . . ? O7 P2 O6 V1 -178.12(19) . . . 2_757 ? O8 P2 O6 V1 -51.8(2) . . . 2_757 ? C11 P2 O6 V1 64.0(2) . . . 2_757 ? O6 P2 O7 Cu1 83.8(2) . . . 2_657 ? O8 P2 O7 Cu1 -42.6(2) . . . 2_657 ? C11 P2 O7 Cu1 -155.24(19) . . . 2_657 ? O5 Cu1 N1 C5 -44.5(2) . . . . ? O7 Cu1 N1 C5 128.1(3) 2_647 . . . ? N2 Cu1 N1 C5 50.8(10) 1_656 . . . ? O1 Cu1 N1 C5 -141.9(2) . . . . ? O5 Cu1 N1 C1 134.7(2) . . . . ? O7 Cu1 N1 C1 -52.7(2) 2_647 . . . ? N2 Cu1 N1 C1 -130.1(9) 1_656 . . . ? O1 Cu1 N1 C1 37.3(2) . . . . ? C5 N1 C1 C2 2.3(4) . . . . ? Cu1 N1 C1 C2 -176.9(2) . . . . ? N1 C1 C2 C3 -0.8(5) . . . . ? C1 C2 C3 C4 -1.6(4) . . . . ? C1 C2 C3 C8 178.2(3) . . . . ? C2 C3 C4 C5 2.5(5) . . . . ? C8 C3 C4 C5 -177.2(3) . . . . ? C1 N1 C5 C4 -1.3(5) . . . . ? Cu1 N1 C5 C4 177.8(3) . . . . ? C3 C4 C5 N1 -1.1(5) . . . . ? C10 N2 C6 C7 -0.3(4) . . . . ? Cu1 N2 C6 C7 178.0(2) 1_454 . . . ? N2 C6 C7 C8 0.3(5) . . . . ? C6 C7 C8 C9 -0.6(4) . . . . ? C6 C7 C8 C3 -179.4(3) . . . . ? C2 C3 C8 C9 -143.5(3) . . . . ? C4 C3 C8 C9 36.2(4) . . . . ? C2 C3 C8 C7 35.2(4) . . . . ? C4 C3 C8 C7 -145.0(3) . . . . ? C7 C8 C9 C10 0.9(4) . . . . ? C3 C8 C9 C10 179.6(3) . . . . ? C6 N2 C10 C9 0.5(4) . . . . ? Cu1 N2 C10 C9 -177.7(2) 1_454 . . . ? C8 C9 C10 N2 -0.8(5) . . . . ? O7 P2 C11 C12 71.3(3) . . . . ? O6 P2 C11 C12 -165.4(2) . . . . ? O8 P2 C11 C12 -45.7(3) . . . . ? O7 P2 C11 C16 -99.8(2) . . . . ? O6 P2 C11 C16 23.6(3) . . . . ? O8 P2 C11 C16 143.3(2) . . . . ? C16 C11 C12 C13 2.7(5) . . . . ? P2 C11 C12 C13 -168.6(3) . . . . ? C11 C12 C13 C14 -2.8(5) . . . . ? C12 C13 C14 C15 1.1(5) . . . . ? C13 C14 C15 C16 0.7(5) . . . . ? C14 C15 C16 C11 -0.8(5) . . . . ? C14 C15 C16 P1 172.4(3) . . . . ? C12 C11 C16 C15 -0.9(4) . . . . ? P2 C11 C16 C15 170.0(2) . . . . ? C12 C11 C16 P1 -173.4(2) . . . . ? P2 C11 C16 P1 -2.5(4) . . . . ? O5 P1 C16 C15 -112.0(2) . . . . ? O3 P1 C16 C15 8.7(3) . . . . ? O4 P1 C16 C15 124.7(2) . . . . ? O5 P1 C16 C11 60.6(3) . . . . ? O3 P1 C16 C11 -178.7(2) . . . . ? O4 P1 C16 C11 -62.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.452 _refine_diff_density_min -0.369 _refine_diff_density_rms 0.097 data_5 _database_code_depnum_ccdc_archive 'CCDC 270528' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H12 Cu2 N O8 P2' _chemical_formula_weight 475.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 20.7505(10) _cell_length_b 45.726(2) _cell_length_c 6.0304(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5721.9(5) _cell_formula_units_Z 16 _cell_measurement_temperature 101(2) _cell_measurement_reflns_used 2933 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 27.43 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3792 _exptl_absorpt_coefficient_mu 3.242 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6970 _exptl_absorpt_correction_T_max 0.9380 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 101(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 15012 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -60 _diffrn_reflns_limit_k_max 60 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.30 _reflns_number_total 3568 _reflns_number_gt 3380 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.034(13) _refine_ls_number_reflns 3568 _refine_ls_number_parameters 230 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0727 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.096 _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 Cu1 Cu 0.17743(2) 0.091545(10) 0.91129(7) 0.00541(10) Uani 1 1 d . . . Cu2 Cu 0.10860(2) 0.139940(10) 0.19623(8) 0.00630(10) Uani 1 1 d . . . P1 P 0.22155(4) 0.09152(2) 0.40086(17) 0.00571(18) Uani 1 1 d . . . P2 P 0.32091(4) 0.10303(2) -0.03848(16) 0.00578(19) Uani 1 1 d . . . O1 O 0.19350(13) 0.07867(6) 0.6131(4) 0.0081(6) Uani 1 1 d . . . O2 O 0.26590(11) 0.11760(5) 0.4365(5) 0.0064(5) Uani 1 1 d . . . O3 O 0.16676(12) 0.09782(6) 0.2353(4) 0.0069(5) Uani 1 1 d . . . O4 O 0.36223(12) 0.12016(6) 0.1300(4) 0.0077(6) Uani 1 1 d . . . O5 O 0.35909(13) 0.09812(6) -0.2493(4) 0.0092(6) Uani 1 1 d . . . O6 O 0.25476(12) 0.11693(5) -0.0717(5) 0.0058(5) Uani 1 1 d . . . O91 O 0.23886(16) 0.17308(8) 0.5783(6) 0.0201(7) Uani 1 1 d . . . O90 O 0.19164(14) 0.16142(7) 0.1502(6) 0.0119(6) Uani 1 1 d . . . H90B H 0.2043 0.1683 0.2716 0.018 Uiso 1 1 calc R . . N1 N 0.10958(14) 0.05952(7) 0.9269(6) 0.0073(6) Uani 1 1 d . . . C1 C 0.10296(19) 0.04182(9) 1.1036(7) 0.0102(8) Uani 1 1 d . . . H1 H 0.1281 0.0456 1.2321 0.012 Uiso 1 1 calc R . . C2 C 0.06107(18) 0.01842(9) 1.1049(6) 0.0109(8) Uani 1 1 d . . . H2 H 0.0584 0.0062 1.2321 0.013 Uiso 1 1 calc R . . C3 C 0.02296(17) 0.01263(8) 0.9219(7) 0.0093(7) Uani 1 1 d . . . C4 C 0.02807(18) 0.03144(8) 0.7421(6) 0.0092(8) Uani 1 1 d . . . H4 H 0.0015 0.0287 0.6154 0.011 Uiso 1 1 calc R . . C5 C 0.07195(19) 0.05408(9) 0.7488(7) 0.0100(8) Uani 1 1 d . . . H5 H 0.0759 0.0664 0.6226 0.012 Uiso 1 1 calc R . . C6 C 0.27028(18) 0.06256(8) 0.2760(6) 0.0070(7) Uani 1 1 d . . . C7 C 0.26905(19) 0.03516(8) 0.3765(6) 0.0100(8) Uani 1 1 d . . . H7 H 0.2451 0.0324 0.5092 0.012 Uiso 1 1 calc R . . C8 C 0.30241(19) 0.01176(9) 0.2848(7) 0.0119(8) Uani 1 1 d . . . H8 H 0.3013 -0.0069 0.3547 0.014 Uiso 1 1 calc R . . C9 C 0.3373(2) 0.01565(9) 0.0909(7) 0.0147(9) Uani 1 1 d . . . H9 H 0.3591 -0.0004 0.0254 0.018 Uiso 1 1 calc R . . C10 C 0.34034(19) 0.04309(8) -0.0077(7) 0.0100(8) Uani 1 1 d . . . H10 H 0.3644 0.0456 -0.1403 0.012 Uiso 1 1 calc R . . C11 C 0.30860(18) 0.06693(8) 0.0849(6) 0.0070(7) Uani 1 1 d . . . H90A H 0.214(3) 0.1501(11) 0.115(10) 0.029(18) Uiso 1 1 d . . . H91A H 0.256(3) 0.1535(15) 0.558(12) 0.07(2) Uiso 1 1 d . . . H91B H 0.210(3) 0.1664(15) 0.689(15) 0.07(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0050(2) 0.0075(2) 0.0037(2) -0.00055(17) 0.00029(18) -0.00138(17) Cu2 0.0050(2) 0.0100(2) 0.0039(2) -0.00068(18) 0.00008(18) 0.00052(17) P1 0.0054(4) 0.0073(4) 0.0045(4) -0.0007(3) 0.0006(4) -0.0002(4) P2 0.0052(4) 0.0081(4) 0.0040(5) 0.0005(4) 0.0002(4) -0.0001(3) O1 0.0070(13) 0.0121(14) 0.0051(14) -0.0005(10) 0.0007(10) 0.0009(11) O2 0.0042(12) 0.0081(13) 0.0068(12) 0.0010(11) -0.0004(12) -0.0010(10) O3 0.0052(13) 0.0100(13) 0.0053(14) -0.0004(11) 0.0013(10) 0.0001(10) O4 0.0069(13) 0.0112(14) 0.0048(13) 0.0005(11) -0.0009(10) -0.0028(10) O5 0.0071(13) 0.0149(14) 0.0055(14) 0.0018(11) 0.0028(10) 0.0011(11) O6 0.0054(12) 0.0067(13) 0.0052(12) -0.0018(11) 0.0009(11) -0.0011(9) O91 0.0168(16) 0.0232(18) 0.0205(17) -0.0027(14) 0.0014(14) -0.0032(14) O90 0.0117(14) 0.0138(15) 0.0103(14) -0.0009(13) 0.0023(12) -0.0023(12) N1 0.0056(14) 0.0082(15) 0.0082(15) -0.0011(13) 0.0031(14) 0.0008(11) C1 0.0098(19) 0.013(2) 0.0078(17) -0.0014(15) -0.0035(15) -0.0012(15) C2 0.0118(19) 0.012(2) 0.0085(18) 0.0044(15) 0.0009(15) -0.0022(15) C3 0.0067(16) 0.0086(17) 0.0124(18) -0.0024(15) 0.0039(16) -0.0012(14) C4 0.0069(18) 0.0130(19) 0.0076(19) -0.0017(15) -0.0012(14) -0.0032(15) C5 0.0104(18) 0.0109(19) 0.0087(19) 0.0011(15) 0.0032(14) -0.0036(15) C6 0.0072(18) 0.0074(18) 0.0065(17) 0.0010(14) -0.0012(14) -0.0004(14) C7 0.0116(19) 0.0105(18) 0.0077(18) 0.0008(14) -0.0001(15) 0.0005(15) C8 0.014(2) 0.009(2) 0.0128(19) 0.0045(16) -0.0028(16) 0.0010(16) C9 0.014(2) 0.012(2) 0.018(2) -0.0033(17) -0.0011(16) 0.0026(16) C10 0.0086(18) 0.0117(19) 0.0096(19) 0.0005(15) 0.0007(14) -0.0020(14) C11 0.0056(17) 0.0103(19) 0.0050(17) -0.0007(14) -0.0013(14) 0.0008(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 Cu1 O1 1.921(3) . ? Cu1 O6 1.983(2) 1_556 ? Cu1 O3 1.987(3) 1_556 ? Cu1 N1 2.034(3) . ? Cu1 O4 2.221(3) 11_455 ? Cu2 O5 1.916(3) 11_455 ? Cu2 O2 1.955(2) 11_454 ? Cu2 O4 1.964(3) 11_454 ? Cu2 O90 2.003(3) . ? Cu2 O3 2.285(3) . ? P1 O2 1.522(3) . ? P1 O1 1.524(3) . ? P1 O3 1.540(3) . ? P1 C6 1.828(4) . ? P2 O5 1.514(3) . ? P2 O6 1.526(3) . ? P2 O4 1.543(3) . ? P2 C11 1.828(4) . ? O2 Cu2 1.955(2) 3 ? O3 Cu1 1.987(3) 1_554 ? O4 Cu2 1.964(3) 3 ? O4 Cu1 2.221(3) 3_554 ? O5 Cu2 1.916(3) 3_554 ? O6 Cu1 1.983(2) 1_554 ? N1 C1 1.345(5) . ? N1 C5 1.351(5) . ? C1 C2 1.379(5) . ? C2 C3 1.383(6) . ? C3 C4 1.388(5) . ? C3 C3 1.497(7) 2 ? C4 C5 1.379(5) . ? C6 C7 1.392(5) . ? C6 C11 1.414(5) . ? C7 C8 1.389(5) . ? C8 C9 1.387(6) . ? C9 C10 1.390(6) . ? C10 C11 1.391(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O6 95.02(11) . 1_556 ? O1 Cu1 O3 169.68(11) . 1_556 ? O6 Cu1 O3 87.40(11) 1_556 1_556 ? O1 Cu1 N1 86.72(12) . . ? O6 Cu1 N1 168.32(12) 1_556 . ? O3 Cu1 N1 88.93(12) 1_556 . ? O1 Cu1 O4 105.52(11) . 11_455 ? O6 Cu1 O4 92.06(10) 1_556 11_455 ? O3 Cu1 O4 84.37(10) 1_556 11_455 ? N1 Cu1 O4 98.61(11) . 11_455 ? O5 Cu2 O2 94.83(12) 11_455 11_454 ? O5 Cu2 O4 176.14(12) 11_455 11_454 ? O2 Cu2 O4 88.12(11) 11_454 11_454 ? O5 Cu2 O90 89.35(13) 11_455 . ? O2 Cu2 O90 158.25(12) 11_454 . ? O4 Cu2 O90 87.00(12) 11_454 . ? O5 Cu2 O3 97.96(11) 11_455 . ? O2 Cu2 O3 111.98(10) 11_454 . ? O4 Cu2 O3 83.20(10) 11_454 . ? O90 Cu2 O3 88.46(11) . . ? O2 P1 O1 114.49(16) . . ? O2 P1 O3 113.04(15) . . ? O1 P1 O3 109.55(15) . . ? O2 P1 C6 106.93(16) . . ? O1 P1 C6 106.15(17) . . ? O3 P1 C6 106.07(16) . . ? O5 P2 O6 114.97(16) . . ? O5 P2 O4 109.70(15) . . ? O6 P2 O4 112.00(15) . . ? O5 P2 C11 106.32(17) . . ? O6 P2 C11 107.68(16) . . ? O4 P2 C11 105.55(16) . . ? P1 O1 Cu1 137.25(17) . . ? P1 O2 Cu2 117.47(14) . 3 ? P1 O3 Cu1 121.88(16) . 1_554 ? P1 O3 Cu2 127.91(15) . . ? Cu1 O3 Cu2 94.54(11) 1_554 . ? P2 O4 Cu2 119.91(15) . 3 ? P2 O4 Cu1 142.64(16) . 3_554 ? Cu2 O4 Cu1 97.25(11) 3 3_554 ? P2 O5 Cu2 139.42(18) . 3_554 ? P2 O6 Cu1 119.40(14) . 1_554 ? C1 N1 C5 117.4(3) . . ? C1 N1 Cu1 122.7(3) . . ? C5 N1 Cu1 119.7(3) . . ? N1 C1 C2 122.4(4) . . ? C1 C2 C3 120.3(4) . . ? C2 C3 C4 117.4(3) . . ? C2 C3 C3 120.8(3) . 2 ? C4 C3 C3 121.8(3) . 2 ? C5 C4 C3 119.5(3) . . ? N1 C5 C4 122.9(4) . . ? C7 C6 C11 119.5(4) . . ? C7 C6 P1 117.5(3) . . ? C11 C6 P1 123.0(3) . . ? C8 C7 C6 120.7(4) . . ? C9 C8 C7 119.8(4) . . ? C8 C9 C10 120.0(4) . . ? C9 C10 C11 120.9(4) . . ? C10 C11 C6 118.9(4) . . ? C10 C11 P2 118.5(3) . . ? C6 C11 P2 122.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 P1 O1 Cu1 22.2(3) . . . . ? O3 P1 O1 Cu1 -105.9(2) . . . . ? C6 P1 O1 Cu1 140.0(2) . . . . ? O6 Cu1 O1 P1 -34.8(3) 1_556 . . . ? O3 Cu1 O1 P1 -138.0(5) 1_556 . . . ? N1 Cu1 O1 P1 156.8(3) . . . . ? O4 Cu1 O1 P1 58.8(3) 11_455 . . . ? O1 P1 O2 Cu2 96.5(2) . . . 3 ? O3 P1 O2 Cu2 -137.10(17) . . . 3 ? C6 P1 O2 Cu2 -20.8(2) . . . 3 ? O2 P1 O3 Cu1 88.4(2) . . . 1_554 ? O1 P1 O3 Cu1 -142.64(17) . . . 1_554 ? C6 P1 O3 Cu1 -28.5(2) . . . 1_554 ? O2 P1 O3 Cu2 -38.7(2) . . . . ? O1 P1 O3 Cu2 90.3(2) . . . . ? C6 P1 O3 Cu2 -155.51(18) . . . . ? O5 Cu2 O3 P1 -32.8(2) 11_455 . . . ? O2 Cu2 O3 P1 -131.29(19) 11_454 . . . ? O4 Cu2 O3 P1 143.5(2) 11_454 . . . ? O90 Cu2 O3 P1 56.4(2) . . . . ? O5 Cu2 O3 Cu1 -169.93(11) 11_455 . . 1_554 ? O2 Cu2 O3 Cu1 91.56(12) 11_454 . . 1_554 ? O4 Cu2 O3 Cu1 6.36(11) 11_454 . . 1_554 ? O90 Cu2 O3 Cu1 -80.80(13) . . . 1_554 ? O5 P2 O4 Cu2 -140.79(17) . . . 3 ? O6 P2 O4 Cu2 90.28(19) . . . 3 ? C11 P2 O4 Cu2 -26.6(2) . . . 3 ? O5 P2 O4 Cu1 45.8(3) . . . 3_554 ? O6 P2 O4 Cu1 -83.2(3) . . . 3_554 ? C11 P2 O4 Cu1 159.9(3) . . . 3_554 ? O6 P2 O5 Cu2 14.9(3) . . . 3_554 ? O4 P2 O5 Cu2 -112.4(3) . . . 3_554 ? C11 P2 O5 Cu2 133.9(3) . . . 3_554 ? O5 P2 O6 Cu1 96.2(2) . . . 1_554 ? O4 P2 O6 Cu1 -137.65(17) . . . 1_554 ? C11 P2 O6 Cu1 -22.0(2) . . . 1_554 ? O1 Cu1 N1 C1 136.1(3) . . . . ? O6 Cu1 N1 C1 37.2(8) 1_556 . . . ? O3 Cu1 N1 C1 -34.5(3) 1_556 . . . ? O4 Cu1 N1 C1 -118.6(3) 11_455 . . . ? O1 Cu1 N1 C5 -39.2(3) . . . . ? O6 Cu1 N1 C5 -138.2(6) 1_556 . . . ? O3 Cu1 N1 C5 150.2(3) 1_556 . . . ? O4 Cu1 N1 C5 66.0(3) 11_455 . . . ? C5 N1 C1 C2 1.7(6) . . . . ? Cu1 N1 C1 C2 -173.7(3) . . . . ? N1 C1 C2 C3 -1.1(6) . . . . ? C1 C2 C3 C4 -1.1(6) . . . . ? C1 C2 C3 C3 -179.7(4) . . . 2 ? C2 C3 C4 C5 2.5(6) . . . . ? C3 C3 C4 C5 -178.8(4) 2 . . . ? C1 N1 C5 C4 -0.1(6) . . . . ? Cu1 N1 C5 C4 175.4(3) . . . . ? C3 C4 C5 N1 -2.0(6) . . . . ? O2 P1 C6 C7 127.8(3) . . . . ? O1 P1 C6 C7 5.2(3) . . . . ? O3 P1 C6 C7 -111.3(3) . . . . ? O2 P1 C6 C11 -52.0(3) . . . . ? O1 P1 C6 C11 -174.6(3) . . . . ? O3 P1 C6 C11 68.9(3) . . . . ? C11 C6 C7 C8 -3.3(6) . . . . ? P1 C6 C7 C8 176.9(3) . . . . ? C6 C7 C8 C9 -0.1(6) . . . . ? C7 C8 C9 C10 1.8(6) . . . . ? C8 C9 C10 C11 -0.2(6) . . . . ? C9 C10 C11 C6 -3.2(6) . . . . ? C9 C10 C11 P2 174.3(3) . . . . ? C7 C6 C11 C10 4.8(5) . . . . ? P1 C6 C11 C10 -175.3(3) . . . . ? C7 C6 C11 P2 -172.5(3) . . . . ? P1 C6 C11 P2 7.4(5) . . . . ? O5 P2 C11 C10 7.8(4) . . . . ? O6 P2 C11 C10 131.5(3) . . . . ? O4 P2 C11 C10 -108.7(3) . . . . ? O5 P2 C11 C6 -174.9(3) . . . . ? O6 P2 C11 C6 -51.2(3) . . . . ? O4 P2 C11 C6 68.6(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.620 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.114 data_1 _database_code_depnum_ccdc_archive 'CCDC 271060' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H38 Cu2 N4 O15 P4 V2' _chemical_formula_weight 1263.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7559(9) _cell_length_b 13.8997(13) _cell_length_c 19.7171(18) _cell_angle_alpha 101.657(2) _cell_angle_beta 93.949(2) _cell_angle_gamma 110.477(2) _cell_volume 2424.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 91(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.731 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1276 _exptl_absorpt_coefficient_mu 1.447 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5315 _exptl_absorpt_correction_T_max 0.9312 _exptl_absorpt_process_details 'SADABS SHELXL-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 91(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 'APEX CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 31638 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0682 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 32.92 _reflns_number_total 16286 _reflns_number_gt 14140 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+24.5342P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16286 _refine_ls_number_parameters 676 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1885 _refine_ls_wR_factor_gt 0.1846 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.07132(5) 0.48511(4) 0.08206(3) 0.00881(10) Uani 1 1 d . . . Cu2 Cu 0.56349(5) 0.37959(4) 0.39430(3) 0.00945(10) Uani 1 1 d . . . V1 V 0.21581(7) 0.48405(5) 0.24060(4) 0.00831(12) Uani 1 1 d . . . V2 V 0.71256(7) 0.47508(5) 0.26240(4) 0.00813(12) Uani 1 1 d . . . P1 P 0.03604(11) 0.62859(8) 0.22461(5) 0.00798(17) Uani 1 1 d . . . P2 P 0.53340(11) 0.58613(8) 0.35292(5) 0.00816(17) Uani 1 1 d . . . P3 P 0.36733(11) 0.31873(8) 0.25379(5) 0.00785(17) Uani 1 1 d . . . P4 P 0.87307(11) 0.34707(8) 0.16687(5) 0.00747(17) Uani 1 1 d . . . O1 O -0.1106(3) 0.5863(2) 0.25162(17) 0.0125(5) Uani 1 1 d . . . O2 O 0.0239(3) 0.5912(3) 0.14529(16) 0.0128(5) Uani 1 1 d . . . O3 O 0.1620(3) 0.6101(2) 0.26413(16) 0.0110(5) Uani 1 1 d . . . O4 O 0.2575(3) 0.4849(3) 0.16325(16) 0.0122(5) Uani 1 1 d . . . O5 O 0.2391(3) 0.3570(2) 0.26009(16) 0.0105(5) Uani 1 1 d . . . O6 O 0.3889(3) 0.5722(2) 0.31012(16) 0.0110(5) Uani 1 1 d . . . O7 O 0.5192(3) 0.5053(2) 0.39633(16) 0.0114(5) Uani 1 1 d . . . O8 O 0.6586(3) 0.5960(2) 0.30851(16) 0.0096(5) Uani 1 1 d . . . O9 O 0.4082(3) 0.2864(2) 0.31939(17) 0.0135(6) Uani 1 1 d . . . O10 O 0.5006(3) 0.3982(2) 0.23327(16) 0.0108(5) Uani 1 1 d . . . O11 O 0.7515(3) 0.4323(3) 0.32825(16) 0.0122(5) Uani 1 1 d . . . O12 O 0.7403(3) 0.3773(2) 0.18241(16) 0.0112(5) Uani 1 1 d . . . O13 O 1.0029(3) 0.4019(2) 0.22660(16) 0.0110(5) Uani 1 1 d . . . O14 O 0.9166(3) 0.3618(2) 0.09600(16) 0.0115(5) Uani 1 1 d . . . O90 O 0.5627(7) 0.7475(4) 0.2358(3) 0.0440(12) Uani 1 1 d . . . N1 N 0.6215(4) 0.2564(3) 0.40271(19) 0.0125(6) Uani 1 1 d . . . N2 N 0.7050(4) 0.4474(3) 0.48434(18) 0.0118(6) Uani 1 1 d . . . N3 N 0.2199(4) 0.5977(3) 0.04664(18) 0.0108(6) Uani 1 1 d . . . N4 N 0.1251(4) 0.3911(3) 0.00487(19) 0.0109(6) Uani 1 1 d . . . C1 C 0.5701(5) 0.1596(4) 0.3621(3) 0.0174(8) Uani 1 1 d . . . H1 H 0.4916 0.1409 0.3247 0.021 Uiso 1 1 calc R . . C2 C 0.6277(5) 0.0830(4) 0.3723(3) 0.0188(8) Uani 1 1 d . . . H2 H 0.5882 0.0139 0.3422 0.023 Uiso 1 1 calc R . . C3 C 0.7410(5) 0.1087(4) 0.4259(3) 0.0190(9) Uani 1 1 d . . . H3 H 0.7818 0.0580 0.4327 0.023 Uiso 1 1 calc R . . C4 C 0.7967(5) 0.2112(4) 0.4708(2) 0.0155(8) Uani 1 1 d . . . C5 C 0.9086(5) 0.2455(4) 0.5314(3) 0.0200(9) Uani 1 1 d . . . H5 H 0.9526 0.1981 0.5419 0.024 Uiso 1 1 calc R . . C6 C 0.9527(5) 0.3450(4) 0.5740(3) 0.0197(9) Uani 1 1 d . . . H6 H 1.0272 0.3658 0.6136 0.024 Uiso 1 1 calc R . . C7 C 0.8878(5) 0.4182(4) 0.5599(2) 0.0155(8) Uani 1 1 d . . . C8 C 0.9229(5) 0.5207(4) 0.6026(2) 0.0179(8) Uani 1 1 d . . . H8 H 0.9980 0.5470 0.6424 0.021 Uiso 1 1 calc R . . C9 C 0.8480(5) 0.5823(4) 0.5865(2) 0.0166(8) Uani 1 1 d . . . H9 H 0.8697 0.6510 0.6154 0.020 Uiso 1 1 calc R . . C10 C 0.7385(5) 0.5429(4) 0.5265(2) 0.0138(7) Uani 1 1 d . . . H10 H 0.6868 0.5859 0.5159 0.017 Uiso 1 1 calc R . . C11 C 0.7779(5) 0.3859(4) 0.5010(2) 0.0126(7) Uani 1 1 d . . . C12 C 0.7325(5) 0.2823(4) 0.4569(2) 0.0133(7) Uani 1 1 d . . . C13 C 0.8130(4) 0.2072(3) 0.1633(2) 0.0116(7) Uani 1 1 d . . . C14 C 0.8258(6) 0.1745(4) 0.2251(3) 0.0187(8) Uani 1 1 d . . . H14 H 0.8663 0.2259 0.2683 0.022 Uiso 1 1 calc R . . C15 C 0.7799(7) 0.0676(4) 0.2240(3) 0.0261(11) Uani 1 1 d . . . H15 H 0.7896 0.0462 0.2664 0.031 Uiso 1 1 calc R . . C16 C 0.7198(6) -0.0082(4) 0.1611(3) 0.0238(10) Uani 1 1 d . . . H16 H 0.6879 -0.0813 0.1603 0.029 Uiso 1 1 calc R . . C17 C 0.7066(5) 0.0237(4) 0.0994(3) 0.0201(9) Uani 1 1 d . . . H17 H 0.6655 -0.0279 0.0563 0.024 Uiso 1 1 calc R . . C18 C 0.7532(5) 0.1303(3) 0.1005(2) 0.0149(8) Uani 1 1 d . . . H18 H 0.7443 0.1513 0.0579 0.018 Uiso 1 1 calc R . . C19 C 0.5849(4) 0.7133(3) 0.4143(2) 0.0109(7) Uani 1 1 d . . . C20 C 0.4920(5) 0.7707(3) 0.4173(2) 0.0154(8) Uani 1 1 d . . . H20 H 0.4018 0.7442 0.3858 0.018 Uiso 1 1 calc R . . C21 C 0.5323(6) 0.8671(4) 0.4668(3) 0.0197(9) Uani 1 1 d . . . H21 H 0.4694 0.9062 0.4685 0.024 Uiso 1 1 calc R . . C22 C 0.6621(6) 0.9059(4) 0.5132(3) 0.0235(10) Uani 1 1 d . . . H22 H 0.6868 0.9706 0.5475 0.028 Uiso 1 1 calc R . . C23 C 0.7570(6) 0.8510(4) 0.5101(3) 0.0240(10) Uani 1 1 d . . . H23 H 0.8473 0.8783 0.5417 0.029 Uiso 1 1 calc R . . C24 C 0.7189(5) 0.7552(4) 0.4600(3) 0.0181(8) Uani 1 1 d . . . H24 H 0.7847 0.7183 0.4571 0.022 Uiso 1 1 calc R . . C25 C 0.3036(4) 0.2019(3) 0.1827(2) 0.0104(7) Uani 1 1 d . . . C26 C 0.4033(5) 0.1555(3) 0.1586(2) 0.0135(7) Uani 1 1 d . . . H26 H 0.5045 0.1862 0.1793 0.016 Uiso 1 1 calc R . . C27 C 0.3537(5) 0.0643(4) 0.1044(3) 0.0183(8) Uani 1 1 d . . . H27 H 0.4211 0.0324 0.0885 0.022 Uiso 1 1 calc R . . C28 C 0.2060(6) 0.0195(4) 0.0733(3) 0.0209(9) Uani 1 1 d . . . H28 H 0.1724 -0.0432 0.0367 0.025 Uiso 1 1 calc R . . C29 C 0.1070(5) 0.0668(4) 0.0961(3) 0.0213(9) Uani 1 1 d . . . H29 H 0.0064 0.0369 0.0745 0.026 Uiso 1 1 calc R . . C30 C 0.1560(5) 0.1581(4) 0.1506(2) 0.0165(8) Uani 1 1 d . . . H30 H 0.0888 0.1905 0.1659 0.020 Uiso 1 1 calc R . . C31 C 0.0846(5) 0.7700(3) 0.2467(2) 0.0123(7) Uani 1 1 d . . . C32 C 0.2229(6) 0.8379(4) 0.2373(3) 0.0224(10) Uani 1 1 d . . . H32 H 0.2932 0.8096 0.2205 0.027 Uiso 1 1 calc R . . C33 C 0.2577(8) 0.9465(4) 0.2523(3) 0.0345(14) Uani 1 1 d . . . H33 H 0.3503 0.9920 0.2441 0.041 Uiso 1 1 calc R . . C34 C 0.1581(9) 0.9888(5) 0.2791(4) 0.0414(17) Uani 1 1 d . . . H34 H 0.1822 1.0631 0.2888 0.050 Uiso 1 1 calc R . . C35 C 0.0240(8) 0.9236(5) 0.2917(4) 0.0395(16) Uani 1 1 d . . . H35 H -0.0420 0.9533 0.3122 0.047 Uiso 1 1 calc R . . C36 C -0.0149(6) 0.8133(4) 0.2745(3) 0.0239(10) Uani 1 1 d . . . H36 H -0.1087 0.7683 0.2817 0.029 Uiso 1 1 calc R . . C37 C 0.2646(5) 0.7022(3) 0.0697(2) 0.0139(7) Uani 1 1 d . . . H37 H 0.2140 0.7306 0.1028 0.017 Uiso 1 1 calc R . . C38 C 0.3840(5) 0.7716(4) 0.0466(3) 0.0172(8) Uani 1 1 d . . . H38 H 0.4147 0.8458 0.0647 0.021 Uiso 1 1 calc R . . C39 C 0.4567(5) 0.7322(4) -0.0024(3) 0.0169(8) Uani 1 1 d . . . H39 H 0.5375 0.7789 -0.0185 0.020 Uiso 1 1 calc R . . C40 C 0.4105(5) 0.6221(4) -0.0285(2) 0.0137(7) Uani 1 1 d . . . C41 C 0.4777(5) 0.5717(4) -0.0798(2) 0.0156(8) Uani 1 1 d . . . H41 H 0.5601 0.6139 -0.0975 0.019 Uiso 1 1 calc R . . C42 C 0.4251(5) 0.4652(4) -0.1033(2) 0.0148(8) Uani 1 1 d . . . H42 H 0.4704 0.4337 -0.1376 0.018 Uiso 1 1 calc R . . C43 C 0.3019(5) 0.3988(3) -0.0771(2) 0.0131(7) Uani 1 1 d . . . C44 C 0.2403(5) 0.2872(4) -0.0995(3) 0.0179(8) Uani 1 1 d . . . H44 H 0.2781 0.2510 -0.1350 0.022 Uiso 1 1 calc R . . C45 C 0.1252(6) 0.2318(4) -0.0693(3) 0.0196(9) Uani 1 1 d . . . H45 H 0.0823 0.1567 -0.0842 0.024 Uiso 1 1 calc R . . C46 C 0.0707(5) 0.2860(4) -0.0164(2) 0.0172(8) Uani 1 1 d . . . H46 H -0.0074 0.2464 0.0048 0.021 Uiso 1 1 calc R . . C47 C 0.2381(4) 0.4463(3) -0.0256(2) 0.0106(7) Uani 1 1 d . . . C48 C 0.2912(4) 0.5590(3) -0.0018(2) 0.0103(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0075(2) 0.0107(2) 0.0077(2) 0.00182(16) 0.00224(16) 0.00282(16) Cu2 0.0080(2) 0.0113(2) 0.0083(2) 0.00250(17) -0.00022(16) 0.00285(17) V1 0.0053(3) 0.0096(3) 0.0090(3) 0.0012(2) 0.0006(2) 0.0023(2) V2 0.0055(3) 0.0089(3) 0.0090(3) 0.0010(2) 0.0015(2) 0.0020(2) P1 0.0057(4) 0.0079(4) 0.0091(4) 0.0014(3) 0.0009(3) 0.0014(3) P2 0.0056(4) 0.0088(4) 0.0087(4) 0.0001(3) 0.0008(3) 0.0021(3) P3 0.0055(4) 0.0087(4) 0.0086(4) 0.0013(3) 0.0010(3) 0.0022(3) P4 0.0050(4) 0.0084(4) 0.0080(4) 0.0007(3) 0.0012(3) 0.0021(3) O1 0.0079(12) 0.0110(13) 0.0160(14) 0.0035(11) 0.0038(10) -0.0001(10) O2 0.0131(13) 0.0158(14) 0.0103(13) 0.0025(11) 0.0034(10) 0.0063(11) O3 0.0105(13) 0.0127(13) 0.0098(13) 0.0013(10) 0.0007(10) 0.0053(10) O4 0.0088(12) 0.0165(14) 0.0110(13) 0.0033(11) 0.0029(10) 0.0039(11) O5 0.0091(12) 0.0116(13) 0.0107(13) 0.0010(10) 0.0030(10) 0.0044(10) O6 0.0045(11) 0.0139(13) 0.0104(13) -0.0017(10) -0.0022(9) 0.0017(10) O7 0.0091(12) 0.0147(14) 0.0107(13) 0.0035(11) 0.0024(10) 0.0046(10) O8 0.0062(11) 0.0112(13) 0.0112(13) 0.0017(10) 0.0044(10) 0.0029(10) O9 0.0127(13) 0.0144(14) 0.0127(14) 0.0044(11) -0.0011(11) 0.0040(11) O10 0.0064(12) 0.0120(13) 0.0122(13) 0.0015(10) 0.0012(10) 0.0020(10) O11 0.0098(13) 0.0166(14) 0.0112(13) 0.0043(11) 0.0019(10) 0.0055(11) O12 0.0084(12) 0.0117(13) 0.0125(13) 0.0004(10) 0.0016(10) 0.0038(10) O13 0.0081(12) 0.0127(13) 0.0099(13) 0.0012(10) 0.0004(10) 0.0023(10) O14 0.0094(12) 0.0129(13) 0.0106(13) -0.0002(10) 0.0029(10) 0.0036(10) O90 0.067(4) 0.038(3) 0.034(3) 0.019(2) 0.020(2) 0.021(2) N1 0.0114(15) 0.0147(16) 0.0117(15) 0.0058(13) 0.0025(12) 0.0039(12) N2 0.0095(14) 0.0165(16) 0.0083(14) 0.0043(12) 0.0026(11) 0.0027(12) N3 0.0112(15) 0.0150(16) 0.0078(14) 0.0049(12) 0.0036(11) 0.0051(12) N4 0.0080(14) 0.0143(16) 0.0099(15) 0.0030(12) 0.0029(11) 0.0032(12) C1 0.018(2) 0.016(2) 0.018(2) 0.0047(16) -0.0007(16) 0.0070(16) C2 0.020(2) 0.015(2) 0.022(2) 0.0050(17) 0.0008(17) 0.0070(16) C3 0.019(2) 0.019(2) 0.024(2) 0.0101(18) 0.0039(17) 0.0107(17) C4 0.0107(17) 0.022(2) 0.017(2) 0.0098(16) 0.0035(15) 0.0072(15) C5 0.017(2) 0.028(2) 0.019(2) 0.0106(18) 0.0031(16) 0.0102(18) C6 0.0141(19) 0.033(3) 0.015(2) 0.0106(18) 0.0009(15) 0.0102(18) C7 0.0089(17) 0.026(2) 0.0113(18) 0.0042(16) 0.0010(14) 0.0064(15) C8 0.0130(18) 0.029(2) 0.0079(17) 0.0028(16) 0.0015(14) 0.0043(17) C9 0.0126(18) 0.024(2) 0.0093(17) -0.0004(15) -0.0001(14) 0.0047(16) C10 0.0096(16) 0.019(2) 0.0107(17) 0.0029(15) 0.0027(13) 0.0031(14) C11 0.0096(16) 0.0192(19) 0.0083(16) 0.0045(14) 0.0006(13) 0.0040(14) C12 0.0096(16) 0.0171(19) 0.0138(18) 0.0073(15) 0.0003(14) 0.0039(14) C13 0.0076(15) 0.0117(17) 0.0162(18) 0.0033(14) 0.0046(13) 0.0040(13) C14 0.023(2) 0.016(2) 0.017(2) 0.0051(16) 0.0026(17) 0.0063(17) C15 0.036(3) 0.023(2) 0.028(3) 0.015(2) 0.013(2) 0.015(2) C16 0.026(2) 0.014(2) 0.036(3) 0.0094(19) 0.015(2) 0.0089(18) C17 0.019(2) 0.0112(18) 0.027(2) -0.0006(17) 0.0075(18) 0.0039(16) C18 0.0118(17) 0.0126(18) 0.0171(19) 0.0008(15) 0.0039(15) 0.0019(14) C19 0.0107(16) 0.0110(16) 0.0097(16) 0.0006(13) -0.0003(13) 0.0038(13) C20 0.0133(18) 0.0132(18) 0.020(2) 0.0029(15) 0.0046(15) 0.0055(15) C21 0.021(2) 0.0109(18) 0.026(2) 0.0019(17) 0.0113(18) 0.0057(16) C22 0.032(3) 0.014(2) 0.018(2) -0.0027(16) 0.0070(19) 0.0030(18) C23 0.025(2) 0.016(2) 0.021(2) -0.0038(17) -0.0041(18) 0.0022(18) C24 0.0147(19) 0.0157(19) 0.018(2) -0.0023(16) -0.0051(15) 0.0034(15) C25 0.0095(16) 0.0099(16) 0.0085(16) -0.0009(13) -0.0006(13) 0.0019(13) C26 0.0121(17) 0.0105(17) 0.0164(19) 0.0005(14) 0.0034(14) 0.0035(14) C27 0.0161(19) 0.0144(19) 0.024(2) 0.0002(16) 0.0069(17) 0.0065(16) C28 0.020(2) 0.015(2) 0.020(2) -0.0044(16) 0.0076(17) 0.0011(16) C29 0.0113(18) 0.022(2) 0.020(2) -0.0080(17) -0.0028(16) 0.0011(16) C30 0.0081(17) 0.0167(19) 0.018(2) -0.0054(16) -0.0018(14) 0.0026(14) C31 0.0146(18) 0.0098(16) 0.0105(17) 0.0012(13) -0.0008(14) 0.0032(14) C32 0.026(2) 0.017(2) 0.016(2) 0.0019(17) 0.0039(18) -0.0019(18) C33 0.048(4) 0.015(2) 0.024(3) 0.005(2) 0.000(2) -0.008(2) C34 0.064(5) 0.014(2) 0.040(4) 0.005(2) -0.008(3) 0.011(3) C35 0.049(4) 0.022(3) 0.047(4) -0.003(3) -0.006(3) 0.021(3) C36 0.020(2) 0.019(2) 0.034(3) 0.001(2) 0.0010(19) 0.0113(18) C37 0.0142(18) 0.0133(18) 0.0146(18) 0.0042(15) 0.0023(14) 0.0054(14) C38 0.0169(19) 0.0118(18) 0.020(2) 0.0036(16) 0.0032(16) 0.0018(15) C39 0.0129(18) 0.017(2) 0.020(2) 0.0062(16) 0.0030(15) 0.0032(15) C40 0.0096(16) 0.0162(19) 0.0142(18) 0.0065(15) 0.0018(14) 0.0021(14) C41 0.0079(16) 0.028(2) 0.0123(18) 0.0079(16) 0.0030(14) 0.0063(15) C42 0.0132(18) 0.025(2) 0.0130(18) 0.0087(16) 0.0079(14) 0.0115(16) C43 0.0113(17) 0.0157(18) 0.0131(18) 0.0028(14) 0.0026(14) 0.0063(14) C44 0.020(2) 0.018(2) 0.017(2) 0.0015(16) 0.0078(16) 0.0090(17) C45 0.023(2) 0.0144(19) 0.019(2) 0.0001(16) 0.0070(17) 0.0057(17) C46 0.0151(19) 0.0137(19) 0.018(2) 0.0022(15) 0.0065(16) -0.0007(15) C47 0.0074(15) 0.0165(18) 0.0088(16) 0.0040(14) 0.0008(12) 0.0052(13) C48 0.0081(15) 0.0143(17) 0.0081(16) 0.0030(13) 0.0010(12) 0.0037(13) _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 O14 1.931(3) 1_455 ? Cu1 O2 1.939(3) . ? Cu1 N3 2.008(4) . ? Cu1 N4 2.021(4) . ? Cu1 O4 2.338(3) . ? Cu2 O9 1.924(3) . ? Cu2 O7 1.935(3) . ? Cu2 N2 2.006(4) . ? Cu2 N1 2.015(4) . ? Cu2 O11 2.318(3) . ? V1 O4 1.606(3) . ? V1 O6 1.946(3) . ? V1 O13 1.957(3) 1_455 ? V1 O5 1.965(3) . ? V1 O3 1.978(3) . ? V2 O11 1.608(3) . ? V2 O1 1.931(3) 1_655 ? V2 O10 1.947(3) . ? V2 O12 1.964(3) . ? V2 O8 1.999(3) . ? P1 O1 1.523(3) . ? P1 O2 1.527(3) . ? P1 O3 1.533(3) . ? P1 C31 1.803(4) . ? P2 O7 1.519(3) . ? P2 O6 1.522(3) . ? P2 O8 1.535(3) . ? P2 C19 1.809(4) . ? P3 O10 1.524(3) . ? P3 O9 1.524(3) . ? P3 O5 1.524(3) . ? P3 C25 1.800(4) . ? P4 O14 1.520(3) . ? P4 O13 1.526(3) . ? P4 O12 1.527(3) . ? P4 C13 1.808(4) . ? O1 V2 1.931(3) 1_455 ? O13 V1 1.957(3) 1_655 ? O14 Cu1 1.931(3) 1_655 ? N1 C1 1.320(6) . ? N1 C12 1.362(5) . ? N2 C10 1.331(6) . ? N2 C11 1.361(6) . ? N3 C37 1.330(6) . ? N3 C48 1.353(5) . ? N4 C46 1.330(6) . ? N4 C47 1.360(5) . ? C1 C2 1.406(6) . ? C2 C3 1.369(7) . ? C3 C4 1.412(7) . ? C4 C12 1.401(6) . ? C4 C5 1.439(6) . ? C5 C6 1.367(8) . ? C6 C7 1.434(7) . ? C7 C11 1.407(6) . ? C7 C8 1.411(7) . ? C8 C9 1.373(7) . ? C9 C10 1.412(6) . ? C11 C12 1.422(6) . ? C13 C18 1.396(6) . ? C13 C14 1.396(6) . ? C14 C15 1.389(7) . ? C15 C16 1.390(8) . ? C16 C17 1.389(8) . ? C17 C18 1.385(6) . ? C19 C24 1.397(6) . ? C19 C20 1.398(6) . ? C20 C21 1.397(6) . ? C21 C22 1.376(8) . ? C22 C23 1.389(8) . ? C23 C24 1.399(7) . ? C25 C30 1.396(6) . ? C25 C26 1.403(6) . ? C26 C27 1.391(6) . ? C27 C28 1.392(7) . ? C28 C29 1.397(7) . ? C29 C30 1.395(6) . ? C31 C36 1.398(7) . ? C31 C32 1.400(6) . ? C32 C33 1.389(7) . ? C33 C34 1.383(11) . ? C34 C35 1.379(11) . ? C35 C36 1.405(8) . ? C37 C38 1.400(6) . ? C38 C39 1.374(7) . ? C39 C40 1.406(6) . ? C40 C48 1.399(6) . ? C40 C41 1.439(6) . ? C41 C42 1.352(7) . ? C42 C43 1.437(6) . ? C43 C47 1.400(6) . ? C43 C44 1.413(6) . ? C44 C45 1.371(7) . ? C45 C46 1.408(7) . ? C47 C48 1.430(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 O14 Cu1 O2 97.63(13) 1_455 . ? O14 Cu1 N3 168.20(14) 1_455 . ? O2 Cu1 N3 90.89(14) . . ? O14 Cu1 N4 89.53(13) 1_455 . ? O2 Cu1 N4 170.19(14) . . ? N3 Cu1 N4 81.12(15) . . ? O14 Cu1 O4 96.64(12) 1_455 . ? O2 Cu1 O4 94.66(12) . . ? N3 Cu1 O4 90.76(13) . . ? N4 Cu1 O4 91.15(13) . . ? O9 Cu2 O7 96.88(13) . . ? O9 Cu2 N2 165.68(14) . . ? O7 Cu2 N2 92.44(14) . . ? O9 Cu2 N1 88.93(14) . . ? O7 Cu2 N1 173.83(14) . . ? N2 Cu2 N1 81.46(15) . . ? O9 Cu2 O11 98.47(12) . . ? O7 Cu2 O11 92.10(12) . . ? N2 Cu2 O11 91.99(13) . . ? N1 Cu2 O11 89.06(13) . . ? O4 V1 O6 109.77(15) . . ? O4 V1 O13 105.27(14) . 1_455 ? O6 V1 O13 144.69(13) . 1_455 ? O4 V1 O5 104.61(15) . . ? O6 V1 O5 89.69(13) . . ? O13 V1 O5 85.58(13) 1_455 . ? O4 V1 O3 102.30(15) . . ? O6 V1 O3 82.82(13) . . ? O13 V1 O3 85.76(13) 1_455 . ? O5 V1 O3 153.03(13) . . ? O11 V2 O1 108.12(15) . 1_655 ? O11 V2 O10 104.31(15) . . ? O1 V2 O10 147.26(14) 1_655 . ? O11 V2 O12 103.12(15) . . ? O1 V2 O12 90.00(13) 1_655 . ? O10 V2 O12 86.94(13) . . ? O11 V2 O8 101.84(15) . . ? O1 V2 O8 83.44(13) 1_655 . ? O10 V2 O8 85.73(12) . . ? O12 V2 O8 155.01(13) . . ? O1 P1 O2 113.35(18) . . ? O1 P1 O3 113.10(18) . . ? O2 P1 O3 112.06(17) . . ? O1 P1 C31 103.77(19) . . ? O2 P1 C31 108.39(19) . . ? O3 P1 C31 105.38(18) . . ? O7 P2 O6 114.40(17) . . ? O7 P2 O8 112.40(17) . . ? O6 P2 O8 112.24(17) . . ? O7 P2 C19 106.58(18) . . ? O6 P2 C19 104.11(18) . . ? O8 P2 C19 106.22(18) . . ? O10 P3 O9 112.30(17) . . ? O10 P3 O5 112.19(17) . . ? O9 P3 O5 111.94(18) . . ? O10 P3 C25 106.27(18) . . ? O9 P3 C25 107.17(19) . . ? O5 P3 C25 106.49(18) . . ? O14 P4 O13 112.90(17) . . ? O14 P4 O12 112.51(17) . . ? O13 P4 O12 111.90(17) . . ? O14 P4 C13 107.33(19) . . ? O13 P4 C13 106.01(19) . . ? O12 P4 C13 105.59(18) . . ? P1 O1 V2 153.7(2) . 1_455 ? P1 O2 Cu1 135.9(2) . . ? P1 O3 V1 126.32(18) . . ? V1 O4 Cu1 114.69(15) . . ? P3 O5 V1 130.79(18) . . ? P2 O6 V1 149.9(2) . . ? P2 O7 Cu2 139.05(19) . . ? P2 O8 V2 124.49(17) . . ? P3 O9 Cu2 123.28(19) . . ? P3 O10 V2 141.3(2) . . ? V2 O11 Cu2 115.83(16) . . ? P4 O12 V2 131.54(19) . . ? P4 O13 V1 139.17(19) . 1_655 ? P4 O14 Cu1 124.48(18) . 1_655 ? C1 N1 C12 118.7(4) . . ? C1 N1 Cu2 128.6(3) . . ? C12 N1 Cu2 112.6(3) . . ? C10 N2 C11 118.1(4) . . ? C10 N2 Cu2 128.9(3) . . ? C11 N2 Cu2 112.9(3) . . ? C37 N3 C48 118.1(4) . . ? C37 N3 Cu1 128.1(3) . . ? C48 N3 Cu1 113.4(3) . . ? C46 N4 C47 118.0(4) . . ? C46 N4 Cu1 129.0(3) . . ? C47 N4 Cu1 112.8(3) . . ? N1 C1 C2 122.2(4) . . ? C3 C2 C1 119.6(5) . . ? C2 C3 C4 119.5(4) . . ? C12 C4 C3 117.0(4) . . ? C12 C4 C5 118.3(4) . . ? C3 C4 C5 124.7(4) . . ? C6 C5 C4 121.2(4) . . ? C5 C6 C7 120.8(4) . . ? C11 C7 C8 116.9(4) . . ? C11 C7 C6 118.7(4) . . ? C8 C7 C6 124.3(4) . . ? C9 C8 C7 119.6(4) . . ? C8 C9 C10 119.5(4) . . ? N2 C10 C9 122.3(4) . . ? N2 C11 C7 123.5(4) . . ? N2 C11 C12 116.2(4) . . ? C7 C11 C12 120.2(4) . . ? N1 C12 C4 123.0(4) . . ? N1 C12 C11 116.2(4) . . ? C4 C12 C11 120.8(4) . . ? C18 C13 C14 118.6(4) . . ? C18 C13 P4 122.0(3) . . ? C14 C13 P4 119.4(3) . . ? C15 C14 C13 120.7(5) . . ? C14 C15 C16 120.1(5) . . ? C17 C16 C15 119.6(4) . . ? C18 C17 C16 120.3(5) . . ? C17 C18 C13 120.7(4) . . ? C24 C19 C20 119.0(4) . . ? C24 C19 P2 119.9(3) . . ? C20 C19 P2 121.0(3) . . ? C21 C20 C19 119.8(4) . . ? C22 C21 C20 120.8(5) . . ? C21 C22 C23 120.2(4) . . ? C22 C23 C24 119.5(5) . . ? C19 C24 C23 120.6(5) . . ? C30 C25 C26 119.7(4) . . ? C30 C25 P3 120.5(3) . . ? C26 C25 P3 119.8(3) . . ? C27 C26 C25 119.9(4) . . ? C26 C27 C28 120.4(4) . . ? C27 C28 C29 119.9(4) . . ? C30 C29 C28 119.9(4) . . ? C29 C30 C25 120.2(4) . . ? C36 C31 C32 119.1(4) . . ? C36 C31 P1 120.3(4) . . ? C32 C31 P1 120.7(4) . . ? C33 C32 C31 120.3(6) . . ? C34 C33 C32 120.3(6) . . ? C35 C34 C33 120.3(5) . . ? C34 C35 C36 120.0(6) . . ? C31 C36 C35 119.9(5) . . ? N3 C37 C38 121.9(4) . . ? C39 C38 C37 119.9(4) . . ? C38 C39 C40 119.4(4) . . ? C48 C40 C39 116.6(4) . . ? C48 C40 C41 119.0(4) . . ? C39 C40 C41 124.4(4) . . ? C42 C41 C40 120.9(4) . . ? C41 C42 C43 121.2(4) . . ? C47 C43 C44 117.0(4) . . ? C47 C43 C42 118.7(4) . . ? C44 C43 C42 124.3(4) . . ? C45 C44 C43 119.2(4) . . ? C44 C45 C46 120.0(4) . . ? N4 C46 C45 122.1(4) . . ? N4 C47 C43 123.7(4) . . ? N4 C47 C48 116.0(4) . . ? C43 C47 C48 120.3(4) . . ? N3 C48 C40 124.0(4) . . ? N3 C48 C47 116.1(4) . . ? C40 C48 C47 119.9(4) . . ? _diffrn_measured_fraction_theta_max 0.898 _diffrn_reflns_theta_full 32.92 _diffrn_measured_fraction_theta_full 0.898 _refine_diff_density_max 1.381 _refine_diff_density_min -1.077 _refine_diff_density_rms 0.188