# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_contact_author_name 'Jian-Fang Ma' _publ_contact_author_address ; Department of Chemistry Northeast Normal University Changchun 130024 P.R.China ; _publ_contact_author_email jianfangma@yahoo.com.cn _publ_contact_author_fax +86-431-85098620 _publ_contact_author_phone +86-431-85098620 _publ_author_name 'Jian-Fang Ma' #======================================== data_compound-L _database_code_depnum_ccdc_archive 'CCDC 852760' #TrackingRef 'Crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H13 O5 P' _chemical_formula_sum 'C14 H13 O5 P' _chemical_formula_weight 292.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.387(5) _cell_length_b 6.888(5) _cell_length_c 15.845(5) _cell_angle_alpha 79.079(5) _cell_angle_beta 85.111(5) _cell_angle_gamma 82.479(5) _cell_volume 677.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1646 _cell_measurement_theta_min 3.0269 _cell_measurement_theta_max 29.0867 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 304 _exptl_absorpt_coefficient_mu 0.219 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.93016 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4199 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.35 _reflns_number_total 2465 _reflns_number_gt 1869 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0708P)^2^+0.0667P] 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 2465 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1452 _refine_ls_wR_factor_gt 0.1278 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 P1 P 0.17418(10) -0.27069(10) 0.49193(5) 0.0484(3) Uani 1 1 d . . . C1 C 0.2999(5) -0.2566(5) 0.3863(2) 0.0649(9) Uani 1 1 d . . . H1A H 0.4514 -0.2610 0.3896 0.078 Uiso 1 1 calc R . . H1B H 0.2743 -0.3708 0.3627 0.078 Uiso 1 1 calc R . . C2 C 0.2186(4) -0.0673(4) 0.32679(18) 0.0523(7) Uani 1 1 d . . . C3 C 0.3097(4) 0.1067(4) 0.31932(19) 0.0556(7) Uani 1 1 d . . . H3 H 0.4295 0.1063 0.3489 0.067 Uiso 1 1 calc R . . C4 C 0.2273(4) 0.2800(4) 0.26925(18) 0.0526(7) Uani 1 1 d . . . H4 H 0.2935 0.3943 0.2648 0.063 Uiso 1 1 calc R . . C5 C 0.0471(4) 0.2881(4) 0.22500(16) 0.0427(6) Uani 1 1 d . . . C6 C -0.0418(4) 0.1129(4) 0.23109(19) 0.0519(7) Uani 1 1 d . . . H6 H -0.1609 0.1131 0.2011 0.062 Uiso 1 1 calc R . . C7 C 0.0422(4) -0.0618(4) 0.2806(2) 0.0561(7) Uani 1 1 d . . . H7 H -0.0201 -0.1777 0.2832 0.067 Uiso 1 1 calc R . . C8 C -0.0614(4) 0.4772(4) 0.17811(17) 0.0450(6) Uani 1 1 d . . . C9 C -0.2633(4) 0.5387(4) 0.21175(19) 0.0544(7) Uani 1 1 d . . . H9 H -0.3194 0.4613 0.2610 0.065 Uiso 1 1 calc R . . C10 C -0.3814(5) 0.7093(4) 0.1746(2) 0.0603(8) Uani 1 1 d . . . H10 H -0.5145 0.7468 0.1992 0.072 Uiso 1 1 calc R . . C11 C -0.3047(5) 0.8247(4) 0.1015(2) 0.0634(8) Uani 1 1 d . . . H11 H -0.3855 0.9395 0.0757 0.076 Uiso 1 1 calc R . . C12 C -0.1049(5) 0.7684(4) 0.0663(2) 0.0584(8) Uani 1 1 d . . . H12 H -0.0526 0.8465 0.0165 0.070 Uiso 1 1 calc R . . C13 C 0.0189(4) 0.5981(4) 0.10385(17) 0.0465(6) Uani 1 1 d . . . C14 C 0.2301(5) 0.5500(4) 0.05979(18) 0.0507(7) Uani 1 1 d . . . O1 O 0.2612(3) -0.1241(3) 0.53759(13) 0.0603(6) Uani 1 1 d . . . H1 H 0.2323 -0.0103 0.5114 0.090 Uiso 1 1 calc R . . O2 O 0.2518(3) -0.4753(3) 0.54613(14) 0.0602(6) Uani 1 1 d . . . H2 H 0.2180 -0.5645 0.5243 0.090 Uiso 1 1 calc R . . O3 O -0.0620(3) -0.2371(2) 0.48636(13) 0.0536(5) Uani 1 1 d . . . O4 O 0.3398(3) 0.3873(3) 0.08305(13) 0.0652(6) Uani 1 1 d . . . O5 O 0.2881(3) 0.6819(3) -0.00196(14) 0.0744(7) Uani 1 1 d . . . H5 H 0.4051 0.6432 -0.0222 0.112 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 P1 0.0450(4) 0.0431(4) 0.0519(5) 0.0003(3) -0.0114(3) 0.0066(3) C1 0.0605(18) 0.0639(19) 0.061(2) -0.0069(16) -0.0054(15) 0.0207(14) C2 0.0475(15) 0.0576(17) 0.0465(17) -0.0071(13) 0.0012(13) 0.0078(12) C3 0.0402(15) 0.078(2) 0.0452(17) -0.0022(15) -0.0073(12) -0.0036(13) C4 0.0484(15) 0.0609(17) 0.0478(17) -0.0012(14) -0.0059(13) -0.0151(13) C5 0.0425(13) 0.0528(15) 0.0311(14) -0.0025(11) -0.0019(11) -0.0068(11) C6 0.0519(15) 0.0541(16) 0.0514(17) -0.0066(13) -0.0170(13) -0.0079(12) C7 0.0638(18) 0.0469(16) 0.0584(19) -0.0082(14) -0.0118(15) -0.0057(13) C8 0.0475(14) 0.0478(15) 0.0421(15) -0.0078(12) -0.0087(12) -0.0113(11) C9 0.0500(15) 0.0597(17) 0.0521(18) -0.0069(14) -0.0018(13) -0.0072(13) C10 0.0509(16) 0.0608(18) 0.069(2) -0.0142(16) -0.0081(15) 0.0014(13) C11 0.0679(19) 0.0498(17) 0.071(2) -0.0058(15) -0.0170(16) -0.0017(14) C12 0.073(2) 0.0502(16) 0.0505(18) 0.0024(13) -0.0098(15) -0.0155(14) C13 0.0552(16) 0.0456(15) 0.0400(15) -0.0059(12) -0.0059(12) -0.0120(12) C14 0.0631(17) 0.0525(16) 0.0372(15) -0.0009(13) -0.0042(13) -0.0184(14) O1 0.0556(11) 0.0518(12) 0.0715(14) -0.0062(10) -0.0244(10) 0.0073(9) O2 0.0580(11) 0.0455(11) 0.0703(14) 0.0066(10) -0.0223(10) 0.0058(8) O3 0.0452(10) 0.0467(11) 0.0639(13) -0.0009(9) -0.0125(9) 0.0060(8) O4 0.0691(13) 0.0639(13) 0.0535(13) 0.0042(10) 0.0087(10) -0.0034(10) O5 0.0743(15) 0.0719(14) 0.0647(15) 0.0119(11) 0.0146(12) -0.0114(11) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 P1 O3 1.503(2) . ? P1 O1 1.531(2) . ? P1 O2 1.550(2) . ? P1 C1 1.785(3) . ? C1 C2 1.516(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.381(4) . ? C2 C7 1.387(4) . ? C3 C4 1.371(4) . ? C3 H3 0.9300 . ? C4 C5 1.388(4) . ? C4 H4 0.9300 . ? C5 C6 1.384(3) . ? C5 C8 1.488(4) . ? C6 C7 1.377(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.397(4) . ? C8 C13 1.407(4) . ? C9 C10 1.371(4) . ? C9 H9 0.9300 . ? C10 C11 1.368(4) . ? C10 H10 0.9300 . ? C11 C12 1.385(4) . ? C11 H11 0.9300 . ? C12 C13 1.389(4) . ? C12 H12 0.9300 . ? C13 C14 1.492(4) . ? C14 O4 1.251(3) . ? C14 O5 1.269(3) . ? O1 H1 0.8200 . ? O2 H2 0.8200 . ? O5 H5 0.8200 . ? 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 O3 P1 O1 113.93(11) . . ? O3 P1 O2 112.98(10) . . ? O1 P1 O2 102.68(12) . . ? O3 P1 C1 109.63(14) . . ? O1 P1 C1 109.00(14) . . ? O2 P1 C1 108.28(12) . . ? C2 C1 P1 111.63(18) . . ? C2 C1 H1A 109.3 . . ? P1 C1 H1A 109.3 . . ? C2 C1 H1B 109.3 . . ? P1 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? C3 C2 C7 117.7(3) . . ? C3 C2 C1 121.9(3) . . ? C7 C2 C1 120.4(3) . . ? C4 C3 C2 121.4(3) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 121.3(2) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C6 C5 C4 117.3(3) . . ? C6 C5 C8 119.5(2) . . ? C4 C5 C8 123.0(2) . . ? C7 C6 C5 121.4(3) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C2 120.9(3) . . ? C6 C7 H7 119.6 . . ? C2 C7 H7 119.6 . . ? C9 C8 C13 117.5(3) . . ? C9 C8 C5 116.1(2) . . ? C13 C8 C5 126.5(2) . . ? C10 C9 C8 122.1(3) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? C11 C10 C9 120.3(3) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 119.1(3) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C11 C12 C13 121.5(3) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C12 C13 C8 119.5(2) . . ? C12 C13 C14 116.9(2) . . ? C8 C13 C14 123.6(3) . . ? O4 C14 O5 123.1(3) . . ? O4 C14 C13 120.8(2) . . ? O5 C14 C13 116.1(3) . . ? P1 O1 H1 109.5 . . ? P1 O2 H2 109.5 . . ? C14 O5 H5 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 P1 C1 C2 51.6(3) . . . . ? O1 P1 C1 C2 -73.7(2) . . . . ? O2 P1 C1 C2 175.30(19) . . . . ? P1 C1 C2 C3 88.9(3) . . . . ? P1 C1 C2 C7 -88.2(3) . . . . ? C7 C2 C3 C4 1.0(4) . . . . ? C1 C2 C3 C4 -176.1(2) . . . . ? C2 C3 C4 C5 0.9(4) . . . . ? C3 C4 C5 C6 -2.2(4) . . . . ? C3 C4 C5 C8 172.9(2) . . . . ? C4 C5 C6 C7 1.4(4) . . . . ? C8 C5 C6 C7 -173.8(2) . . . . ? C5 C6 C7 C2 0.5(4) . . . . ? C3 C2 C7 C6 -1.8(4) . . . . ? C1 C2 C7 C6 175.4(2) . . . . ? C6 C5 C8 C9 61.9(3) . . . . ? C4 C5 C8 C9 -113.0(3) . . . . ? C6 C5 C8 C13 -117.9(3) . . . . ? C4 C5 C8 C13 67.2(4) . . . . ? C13 C8 C9 C10 0.2(4) . . . . ? C5 C8 C9 C10 -179.6(3) . . . . ? C8 C9 C10 C11 1.0(5) . . . . ? C9 C10 C11 C12 -1.0(5) . . . . ? C10 C11 C12 C13 -0.2(5) . . . . ? C11 C12 C13 C8 1.4(4) . . . . ? C11 C12 C13 C14 179.1(3) . . . . ? C9 C8 C13 C12 -1.4(4) . . . . ? C5 C8 C13 C12 178.4(2) . . . . ? C9 C8 C13 C14 -178.9(2) . . . . ? C5 C8 C13 C14 0.9(4) . . . . ? C12 C13 C14 O4 -171.0(3) . . . . ? C8 C13 C14 O4 6.5(4) . . . . ? C12 C13 C14 O5 8.3(4) . . . . ? C8 C13 C14 O5 -174.1(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O3 0.82 1.83 2.604(3) 156.1 2_546 O1 H1 O3 0.82 1.90 2.617(3) 145.0 2_556 O5 H5 O4 0.82 1.83 2.635(3) 167.0 2_665 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.317 _refine_diff_density_min -0.306 #================================ data_compound-1 _database_code_depnum_ccdc_archive 'CCDC 852761' #TrackingRef 'Crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_absolute_configuration unk _chemical_formula_moiety 'C14 H11 Cu O5 P, (H2 O)' _chemical_formula_sum 'C14 H13 Cu O6 P' _chemical_formula_weight 371.75 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' 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 monoclinic _symmetry_space_group_name_H-M p21 _symmetry_space_group_name_hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 5.1625(3) _cell_length_b 9.7839(6) _cell_length_c 14.7090(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.773(6) _cell_angle_gamma 90.00 _cell_volume 742.87(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1235 _cell_measurement_theta_min 3.4588 _cell_measurement_theta_max 29.1500 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 378 _exptl_absorpt_coefficient_mu 1.603 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.93356 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2700 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0712 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 25.35 _reflns_number_total 2079 _reflns_number_gt 1904 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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. For O1W, some anisotropic displacement ellipsoids were rather elongated which led us to use the ISOR restraints. ; _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^)+(0.0168P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.006(18) _refine_ls_number_reflns 2079 _refine_ls_number_parameters 208 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0709 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 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 1.17773(9) 0.19124(5) 0.46672(4) 0.02567(17) Uani 1 1 d . . . P1 P 1.3077(2) -0.10630(11) 0.55633(9) 0.0187(3) Uani 1 1 d . . . O1 O 1.3603(5) 0.0209(3) 0.4988(2) 0.0216(8) Uani 1 1 d . . . C5 C 0.9531(11) 0.2601(6) 0.8037(4) 0.0302(14) Uani 1 1 d . . . C2 C 1.2197(11) 0.0464(6) 0.7156(4) 0.0321(14) Uani 1 1 d . . . C3 C 1.2884(9) 0.1838(7) 0.7030(4) 0.0362(13) Uani 1 1 d . . . H3 H 1.4242 0.2055 0.6646 0.043 Uiso 1 1 calc R . . C8 C 0.8380(10) 0.3696(6) 0.8581(4) 0.0360(14) Uani 1 1 d . . . C7 C 1.0101(10) 0.0189(6) 0.7695(4) 0.0317(13) Uani 1 1 d . . . H7 H 0.9560 -0.0710 0.7774 0.038 Uiso 1 1 calc R . . C1 C 1.3718(10) -0.0681(6) 0.6734(4) 0.0329(13) Uani 1 1 d . . . H1A H 1.3409 -0.1504 0.7084 0.039 Uiso 1 1 calc R . . H1B H 1.5545 -0.0464 0.6799 0.039 Uiso 1 1 calc R . . C4 C 1.1596(10) 0.2855(6) 0.7458(4) 0.0347(15) Uani 1 1 d . . . H4 H 1.2108 0.3754 0.7363 0.042 Uiso 1 1 calc R . . C9 C 0.7664(11) 0.4993(6) 0.8246(4) 0.0380(14) Uani 1 1 d . . . C6 C 0.8785(11) 0.1245(6) 0.8123(4) 0.0365(15) Uani 1 1 d . . . H6 H 0.7360 0.1035 0.8477 0.044 Uiso 1 1 calc R . . C13 C 0.8123(11) 0.3496(6) 0.9509(5) 0.0473(16) Uani 1 1 d . . . H13 H 0.8547 0.2648 0.9755 0.057 Uiso 1 1 calc R . . C10 C 0.6875(13) 0.6021(7) 0.8828(5) 0.056(2) Uani 1 1 d . . . H10 H 0.6469 0.6880 0.8595 0.067 Uiso 1 1 calc R . . C11 C 0.6688(15) 0.5786(8) 0.9744(5) 0.067(2) Uani 1 1 d . . . H11 H 0.6178 0.6485 1.0131 0.080 Uiso 1 1 calc R . . C12 C 0.7252(13) 0.4523(8) 1.0085(5) 0.063(2) Uani 1 1 d . . . H12 H 0.7056 0.4347 1.0702 0.076 Uiso 1 1 calc R . . O2 O 1.4846(5) -0.2215(3) 0.5284(2) 0.0209(8) Uani 1 1 d . . . O4 O 0.6681(8) 0.4334(4) 0.6735(3) 0.0439(11) Uani 1 1 d . . . H4A H 0.6637 0.4589 0.6204 0.066 Uiso 1 1 calc R . . C14 C 0.7499(10) 0.5335(6) 0.7255(4) 0.0344(14) Uani 1 1 d . . . O5 O 0.7929(9) 0.6478(4) 0.6966(3) 0.0608(14) Uani 1 1 d . . . O3 O 1.0225(6) -0.1434(3) 0.5469(2) 0.0216(8) Uani 1 1 d . . . O1W O 0.8692(8) 0.0798(5) 0.4539(4) 0.0400(14) Uani 0.80 1 d P . . O1W' O 0.872(3) 0.1061(17) 0.5279(13) 0.021(4) Uani 0.20 1 d PU . . 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 0.0116(2) 0.0102(3) 0.0552(4) 0.0036(3) -0.0007(2) -0.0010(3) P1 0.0113(6) 0.0101(6) 0.0346(8) 0.0015(6) -0.0003(5) 0.0002(5) O1 0.0116(16) 0.0103(16) 0.043(2) 0.0014(16) 0.0015(14) 0.0016(14) C5 0.031(3) 0.030(3) 0.030(3) 0.004(3) 0.003(3) 0.003(3) C2 0.031(3) 0.028(3) 0.037(4) -0.002(3) -0.007(3) 0.002(3) C3 0.031(3) 0.035(3) 0.043(3) 0.003(4) 0.013(2) 0.003(3) C8 0.035(3) 0.040(3) 0.033(3) -0.003(3) 0.005(2) 0.002(3) C7 0.033(3) 0.026(3) 0.036(4) -0.003(3) -0.005(2) -0.002(3) C1 0.032(3) 0.034(3) 0.032(3) -0.007(3) -0.006(2) 0.007(3) C4 0.036(3) 0.027(3) 0.041(4) -0.006(3) 0.003(3) -0.006(3) C9 0.041(3) 0.029(3) 0.044(4) -0.003(3) 0.004(3) 0.002(3) C6 0.037(3) 0.042(4) 0.030(4) 0.005(3) 0.002(3) -0.003(3) C13 0.054(4) 0.039(4) 0.049(4) -0.007(3) 0.005(3) 0.006(3) C10 0.066(5) 0.045(4) 0.058(5) -0.008(4) 0.010(4) 0.006(3) C11 0.090(6) 0.052(5) 0.059(5) -0.019(4) 0.019(5) 0.010(4) C12 0.075(5) 0.075(6) 0.039(5) -0.014(4) 0.009(4) 0.004(4) O2 0.0119(16) 0.0081(15) 0.043(2) 0.0000(16) 0.0029(15) 0.0009(14) O4 0.068(3) 0.031(2) 0.032(3) -0.002(2) 0.007(2) -0.013(2) C14 0.038(3) 0.026(3) 0.039(4) 0.005(3) -0.001(3) 0.000(3) O5 0.100(4) 0.027(2) 0.055(3) 0.009(2) -0.016(3) -0.010(2) O3 0.0109(16) 0.0122(18) 0.042(2) -0.0022(16) 0.0038(15) -0.0013(14) O1W 0.018(2) 0.020(2) 0.082(5) 0.002(3) 0.000(3) -0.005(2) O1W' 0.014(5) 0.022(6) 0.027(6) 0.001(4) 0.005(4) -0.004(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O3 1.929(3) 2_756 ? Cu1 O1W 1.937(4) . ? Cu1 O2 1.942(3) 2_856 ? Cu1 O1 1.969(3) . ? Cu1 O1W' 2.007(14) . ? P1 O2 1.511(3) . ? P1 O3 1.521(3) . ? P1 O1 1.532(4) . ? P1 C1 1.789(6) . ? C5 C6 1.388(7) . ? C5 C4 1.396(8) . ? C5 C8 1.467(8) . ? C2 C7 1.377(7) . ? C2 C3 1.403(9) . ? C2 C1 1.507(7) . ? C3 C4 1.356(8) . ? C3 H3 0.9300 . ? C8 C13 1.387(8) . ? C8 C9 1.409(8) . ? C7 C6 1.391(8) . ? C7 H7 0.9300 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C4 H4 0.9300 . ? C9 C10 1.386(8) . ? C9 C14 1.498(8) . ? C6 H6 0.9300 . ? C13 C12 1.393(8) . ? C13 H13 0.9300 . ? C10 C11 1.372(9) . ? C10 H10 0.9300 . ? C11 C12 1.364(9) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? O2 Cu1 1.942(3) 2_846 ? O4 C14 1.309(7) . ? O4 H4A 0.8200 . ? C14 O5 1.217(7) . ? O3 Cu1 1.929(3) 2_746 ? O1W O1W' 1.119(18) . ? 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 O3 Cu1 O1W 91.31(18) 2_756 . ? O3 Cu1 O2 96.58(13) 2_756 2_856 ? O1W Cu1 O2 171.00(18) . 2_856 ? O3 Cu1 O1 171.50(15) 2_756 . ? O1W Cu1 O1 86.42(16) . . ? O2 Cu1 O1 86.37(12) 2_856 . ? O3 Cu1 O1W' 88.3(5) 2_756 . ? O1W Cu1 O1W' 32.9(5) . . ? O2 Cu1 O1W' 151.2(6) 2_856 . ? O1 Cu1 O1W' 85.3(5) . . ? O2 P1 O3 112.64(19) . . ? O2 P1 O1 110.09(17) . . ? O3 P1 O1 108.80(17) . . ? O2 P1 C1 108.2(2) . . ? O3 P1 C1 107.7(2) . . ? O1 P1 C1 109.3(2) . . ? P1 O1 Cu1 137.07(18) . . ? C6 C5 C4 116.2(5) . . ? C6 C5 C8 122.2(5) . . ? C4 C5 C8 121.4(5) . . ? C7 C2 C3 117.8(5) . . ? C7 C2 C1 120.7(5) . . ? C3 C2 C1 121.6(5) . . ? C4 C3 C2 121.0(5) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C13 C8 C9 116.2(5) . . ? C13 C8 C5 118.6(6) . . ? C9 C8 C5 125.0(5) . . ? C2 C7 C6 120.5(5) . . ? C2 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C2 C1 P1 117.5(4) . . ? C2 C1 H1A 107.9 . . ? P1 C1 H1A 107.9 . . ? C2 C1 H1B 107.9 . . ? P1 C1 H1B 107.9 . . ? H1A C1 H1B 107.2 . . ? C3 C4 C5 122.4(5) . . ? C3 C4 H4 118.8 . . ? C5 C4 H4 118.8 . . ? C10 C9 C8 121.1(6) . . ? C10 C9 C14 115.2(6) . . ? C8 C9 C14 123.6(5) . . ? C5 C6 C7 122.1(5) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C8 C13 C12 122.3(6) . . ? C8 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C11 C10 C9 120.7(7) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C12 C11 C10 119.7(7) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 119.9(7) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? P1 O2 Cu1 149.7(2) . 2_846 ? C14 O4 H4A 109.5 . . ? O5 C14 O4 122.9(6) . . ? O5 C14 C9 122.4(6) . . ? O4 C14 C9 114.5(5) . . ? P1 O3 Cu1 136.6(2) . 2_746 ? O1W' O1W Cu1 77.0(8) . . ? O1W O1W' Cu1 70.1(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 P1 O1 Cu1 160.8(3) . . . . ? O3 P1 O1 Cu1 36.9(4) . . . . ? C1 P1 O1 Cu1 -80.4(3) . . . . ? O3 Cu1 O1 P1 33.2(11) 2_756 . . . ? O1W Cu1 O1 P1 -41.5(4) . . . . ? O2 Cu1 O1 P1 143.9(3) 2_856 . . . ? O1W' Cu1 O1 P1 -8.5(6) . . . . ? C7 C2 C3 C4 3.0(8) . . . . ? C1 C2 C3 C4 -176.0(6) . . . . ? C6 C5 C8 C13 46.7(9) . . . . ? C4 C5 C8 C13 -127.9(7) . . . . ? C6 C5 C8 C9 -138.0(7) . . . . ? C4 C5 C8 C9 47.4(9) . . . . ? C3 C2 C7 C6 -2.3(8) . . . . ? C1 C2 C7 C6 176.6(6) . . . . ? C7 C2 C1 P1 100.7(6) . . . . ? C3 C2 C1 P1 -80.4(6) . . . . ? O2 P1 C1 C2 178.9(4) . . . . ? O3 P1 C1 C2 -59.1(5) . . . . ? O1 P1 C1 C2 59.0(5) . . . . ? C2 C3 C4 C5 -0.5(9) . . . . ? C6 C5 C4 C3 -2.6(9) . . . . ? C8 C5 C4 C3 172.2(6) . . . . ? C13 C8 C9 C10 3.1(9) . . . . ? C5 C8 C9 C10 -172.3(6) . . . . ? C13 C8 C9 C14 -172.2(5) . . . . ? C5 C8 C9 C14 12.5(9) . . . . ? C4 C5 C6 C7 3.3(10) . . . . ? C8 C5 C6 C7 -171.5(6) . . . . ? C2 C7 C6 C5 -0.8(10) . . . . ? C9 C8 C13 C12 -1.1(9) . . . . ? C5 C8 C13 C12 174.6(6) . . . . ? C8 C9 C10 C11 -2.2(10) . . . . ? C14 C9 C10 C11 173.4(6) . . . . ? C9 C10 C11 C12 -0.8(11) . . . . ? C10 C11 C12 C13 2.8(12) . . . . ? C8 C13 C12 C11 -1.8(11) . . . . ? O3 P1 O2 Cu1 -158.7(4) . . . 2_846 ? O1 P1 O2 Cu1 79.7(5) . . . 2_846 ? C1 P1 O2 Cu1 -39.7(5) . . . 2_846 ? C10 C9 C14 O5 35.2(8) . . . . ? C8 C9 C14 O5 -149.3(6) . . . . ? C10 C9 C14 O4 -140.2(6) . . . . ? C8 C9 C14 O4 35.3(8) . . . . ? O2 P1 O3 Cu1 16.4(4) . . . 2_746 ? O1 P1 O3 Cu1 138.7(3) . . . 2_746 ? C1 P1 O3 Cu1 -102.9(4) . . . 2_746 ? O3 Cu1 O1W O1W' -84.9(10) 2_756 . . . ? O2 Cu1 O1W O1W' 123.7(16) 2_856 . . . ? O1 Cu1 O1W O1W' 86.9(9) . . . . ? O3 Cu1 O1W' O1W 95.0(8) 2_756 . . . ? O2 Cu1 O1W' O1W -164.3(4) 2_856 . . . ? O1 Cu1 O1W' O1W -90.7(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4A O1 0.82 1.86 2.676(5) 177.4 2_756 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.323 _refine_diff_density_min -0.394 _refine_diff_density_rms 0.070 #=================================== data_compound-2 _database_code_depnum_ccdc_archive 'CCDC 852762' #TrackingRef 'Crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H23.9 Cu5 O14.2 P2, 0.8(H2 O)' _chemical_formula_sum 'C28 H25.50 Cu5 O15 P2' _chemical_formula_weight 981.62 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' 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 monoclinic _symmetry_space_group_name_H-M p21/c _symmetry_space_group_name_hall '-P 2ybc' 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 13.6470(10) _cell_length_b 12.2255(5) _cell_length_c 10.0282(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.675(5) _cell_angle_gamma 90.00 _cell_volume 1658.13(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1646 _cell_measurement_theta_min 2.8960 _cell_measurement_theta_max 29.1133 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.966 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 977 _exptl_absorpt_coefficient_mu 3.322 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.82844 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6471 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.1015 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3013 _reflns_number_gt 2134 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0528P)^2^+0.5484P] 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 3013 _refine_ls_number_parameters 233 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0917 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1539 _refine_ls_wR_factor_gt 0.1329 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _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 0.59762(7) 0.26811(7) 0.96986(8) 0.0275(3) Uani 1 1 d . . . Cu2 Cu 0.60496(8) 0.08914(7) 1.21665(8) 0.0317(3) Uani 1 1 d . . . Cu3 Cu 0.5000 0.0000 1.5000 0.0269(4) Uani 1 2 d S . . P1 P 0.54883(16) 0.65662(14) 0.77111(17) 0.0265(5) Uani 1 1 d . . . C1 C 0.6671(7) 0.7112(7) 0.8487(9) 0.054(3) Uani 1 1 d . . . H1A H 0.7068 0.7281 0.7780 0.065 Uiso 1 1 calc R . . H1B H 0.6550 0.7793 0.8933 0.065 Uiso 1 1 calc R . . C2 C 0.7269(7) 0.6366(7) 0.9503(8) 0.040(2) Uani 1 1 d . . . C3 C 0.8094(7) 0.5812(8) 0.9189(9) 0.049(2) Uani 1 1 d . . . H3 H 0.8307 0.5929 0.8358 0.059 Uiso 1 1 calc R . . C4 C 0.8613(7) 0.5085(7) 1.0091(8) 0.044(2) Uani 1 1 d . . . H4 H 0.9156 0.4705 0.9858 0.053 Uiso 1 1 calc R . . C5 C 0.8307(7) 0.4939(6) 1.1339(7) 0.038(2) Uani 1 1 d . . . C6 C 0.7508(7) 0.5489(6) 1.1704(7) 0.038(2) Uani 1 1 d . . . H6 H 0.7309 0.5382 1.2546 0.046 Uiso 1 1 calc R . . C7 C 0.6997(7) 0.6216(6) 1.0773(8) 0.043(2) Uani 1 1 d . . . H7 H 0.6464 0.6607 1.1015 0.052 Uiso 1 1 calc R . . C8 C 0.8869(7) 0.4147(6) 1.2334(8) 0.040(2) Uani 1 1 d . . . C9 C 0.9785(8) 0.4477(7) 1.2968(9) 0.055(3) Uani 1 1 d . . . H9 H 1.0039 0.5149 1.2748 0.066 Uiso 1 1 calc R . . C10 C 1.0317(8) 0.3839(9) 1.3901(11) 0.070(3) Uani 1 1 d . . . H10 H 1.0956 0.4043 1.4251 0.084 Uiso 1 1 calc R . . C11 C 0.9920(9) 0.2896(9) 1.4331(12) 0.083(4) Uani 1 1 d . . . H11 H 1.0261 0.2489 1.5028 0.099 Uiso 1 1 calc R . . C12 C 0.9008(8) 0.2557(9) 1.3719(10) 0.065(3) Uani 1 1 d . . . H12 H 0.8744 0.1903 1.3983 0.078 Uiso 1 1 calc R . . C13 C 0.8473(6) 0.3183(7) 1.2706(7) 0.0352(19) Uani 1 1 d . . . C14 C 0.7522(6) 0.2695(6) 1.2033(8) 0.0333(19) Uani 1 1 d . . . O1 O 0.4986(4) 0.7525(4) 0.6911(5) 0.0302(13) Uani 1 1 d . . . O2 O 0.5639(5) 0.5604(4) 0.6810(5) 0.0406(15) Uani 1 1 d . . . O3 O 0.4937(4) 0.6264(4) 0.8879(4) 0.0329(13) Uani 1 1 d . . . O4 O 0.7196(4) 0.3008(4) 1.0883(5) 0.0347(13) Uani 1 1 d . . . O5 O 0.7116(5) 0.1959(5) 1.2669(5) 0.0444(15) Uani 1 1 d . . . O6 O 0.5863(4) 0.1239(4) 1.0315(4) 0.0384(15) Uani 1 1 d . . . O7 O 0.6026(4) 0.0760(3) 1.4113(4) 0.0234(11) Uani 1 1 d . . . O1W O 1.242(3) 0.503(3) 1.481(3) 0.20(3) Uani 0.41(3) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0488(7) 0.0199(5) 0.0139(5) 0.0012(4) 0.0053(4) -0.0033(4) Cu2 0.0600(8) 0.0223(5) 0.0133(5) 0.0009(4) 0.0069(4) -0.0051(4) Cu3 0.0489(9) 0.0202(6) 0.0134(6) -0.0026(5) 0.0108(6) -0.0030(6) P1 0.0497(14) 0.0184(9) 0.0127(9) -0.0002(7) 0.0089(8) 0.0043(8) C1 0.069(7) 0.044(5) 0.045(5) 0.019(4) -0.007(5) -0.012(5) C2 0.033(5) 0.043(5) 0.040(5) 0.010(4) -0.009(4) -0.011(4) C3 0.032(6) 0.073(7) 0.040(5) 0.010(5) -0.001(4) -0.011(5) C4 0.041(6) 0.046(5) 0.048(5) 0.004(4) 0.017(4) -0.003(4) C5 0.052(6) 0.036(5) 0.027(4) -0.003(4) 0.007(4) -0.007(4) C6 0.056(6) 0.033(4) 0.024(4) -0.005(4) 0.000(4) 0.006(4) C7 0.063(7) 0.033(4) 0.030(5) -0.009(4) -0.008(4) 0.005(4) C8 0.041(6) 0.035(5) 0.039(5) -0.001(4) -0.005(4) 0.005(4) C9 0.063(7) 0.042(5) 0.057(6) 0.010(5) -0.001(5) -0.012(5) C10 0.048(7) 0.072(7) 0.084(8) 0.031(6) -0.015(6) -0.004(6) C11 0.077(9) 0.075(8) 0.084(8) 0.031(7) -0.034(7) 0.004(7) C12 0.056(7) 0.062(7) 0.071(7) 0.015(6) -0.011(6) -0.009(5) C13 0.029(5) 0.044(5) 0.029(4) -0.002(4) -0.008(4) 0.005(4) C14 0.039(5) 0.034(4) 0.028(4) 0.005(4) 0.011(4) 0.004(4) O1 0.050(4) 0.022(3) 0.018(3) 0.003(2) 0.005(2) 0.004(2) O2 0.071(4) 0.032(3) 0.019(3) -0.002(2) 0.005(3) 0.014(3) O3 0.053(4) 0.029(3) 0.021(3) 0.012(2) 0.020(2) 0.012(3) O4 0.046(4) 0.034(3) 0.024(3) 0.006(2) 0.003(3) -0.010(3) O5 0.057(4) 0.052(4) 0.024(3) 0.004(3) 0.001(3) -0.017(3) O6 0.082(5) 0.023(3) 0.011(2) 0.006(2) 0.010(3) -0.006(3) O7 0.045(3) 0.018(2) 0.009(2) 0.0000(19) 0.008(2) -0.002(2) O1W 0.23(4) 0.27(4) 0.13(2) -0.04(2) 0.10(2) -0.17(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O6 1.882(5) . ? Cu1 O1 1.950(5) 2_646 ? Cu1 O4 1.953(5) . ? Cu1 O7 1.998(4) 4_565 ? Cu1 O3 2.393(5) 3_667 ? Cu2 O6 1.888(4) . ? Cu2 O2 1.932(5) 4_566 ? Cu2 O7 1.963(4) . ? Cu2 O5 1.969(6) . ? Cu3 O3 1.906(5) 2_647 ? Cu3 O3 1.906(5) 4_566 ? Cu3 O7 1.987(5) 3_658 ? Cu3 O7 1.987(5) . ? P1 O2 1.514(5) . ? P1 O3 1.520(5) . ? P1 O1 1.530(5) . ? P1 C1 1.822(9) . ? C1 C2 1.521(11) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.386(13) . ? C2 C7 1.385(11) . ? C3 C4 1.392(12) . ? C3 H3 0.9300 . ? C4 C5 1.383(11) . ? C4 H4 0.9300 . ? C5 C6 1.372(12) . ? C5 C8 1.522(11) . ? C6 C7 1.406(11) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C13 1.370(11) . ? C8 C9 1.384(12) . ? C9 C10 1.352(13) . ? C9 H9 0.9300 . ? C10 C11 1.368(14) . ? C10 H10 0.9300 . ? C11 C12 1.376(14) . ? C11 H11 0.9300 . ? C12 C13 1.397(12) . ? C12 H12 0.9300 . ? C13 C14 1.503(11) . ? C14 O4 1.240(8) . ? C14 O5 1.273(9) . ? O1 Cu1 1.950(5) 2_656 ? O2 Cu2 1.932(5) 4_565 ? O3 Cu3 1.906(4) 2_657 ? O3 Cu1 2.393(5) 3_667 ? O7 Cu1 1.998(4) 4_566 ? 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 O6 Cu1 O1 96.0(2) . 2_646 ? O6 Cu1 O4 95.3(2) . . ? O1 Cu1 O4 161.6(2) 2_646 . ? O6 Cu1 O7 176.3(2) . 4_565 ? O1 Cu1 O7 83.98(19) 2_646 4_565 ? O4 Cu1 O7 85.6(2) . 4_565 ? O6 Cu1 O3 103.7(2) . 3_667 ? O1 Cu1 O3 101.5(2) 2_646 3_667 ? O4 Cu1 O3 89.8(2) . 3_667 ? O7 Cu1 O3 72.67(17) 4_565 3_667 ? O6 Cu2 O2 91.9(2) . 4_566 ? O6 Cu2 O7 167.9(2) . . ? O2 Cu2 O7 93.65(19) 4_566 . ? O6 Cu2 O5 95.8(2) . . ? O2 Cu2 O5 149.4(3) 4_566 . ? O7 Cu2 O5 84.8(2) . . ? O3 Cu3 O3 180.000(1) 2_647 4_566 ? O3 Cu3 O7 95.39(19) 2_647 3_658 ? O3 Cu3 O7 84.61(19) 4_566 3_658 ? O3 Cu3 O7 84.61(19) 2_647 . ? O3 Cu3 O7 95.39(19) 4_566 . ? O7 Cu3 O7 180.000(1) 3_658 . ? O2 P1 O3 113.1(3) . . ? O2 P1 O1 111.7(3) . . ? O3 P1 O1 110.9(3) . . ? O2 P1 C1 110.8(4) . . ? O3 P1 C1 105.2(4) . . ? O1 P1 C1 104.6(3) . . ? C2 C1 P1 115.6(6) . . ? C2 C1 H1A 108.4 . . ? P1 C1 H1A 108.4 . . ? C2 C1 H1B 108.4 . . ? P1 C1 H1B 108.4 . . ? H1A C1 H1B 107.4 . . ? C3 C2 C7 118.0(8) . . ? C3 C2 C1 121.3(8) . . ? C7 C2 C1 120.6(9) . . ? C2 C3 C4 121.5(8) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C5 C4 C3 118.8(9) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C6 C5 C4 121.7(8) . . ? C6 C5 C8 119.1(7) . . ? C4 C5 C8 119.3(8) . . ? C5 C6 C7 118.3(8) . . ? C5 C6 H6 120.8 . . ? C7 C6 H6 120.8 . . ? C2 C7 C6 121.6(8) . . ? C2 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C13 C8 C9 119.4(8) . . ? C13 C8 C5 122.9(8) . . ? C9 C8 C5 117.5(8) . . ? C10 C9 C8 121.3(9) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 120.3(10) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C12 119.0(10) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C11 C12 C13 120.9(9) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C8 C13 C12 118.8(8) . . ? C8 C13 C14 124.6(7) . . ? C12 C13 C14 116.5(8) . . ? O4 C14 O5 123.9(8) . . ? O4 C14 C13 118.5(7) . . ? O5 C14 C13 117.6(7) . . ? P1 O1 Cu1 135.5(3) . 2_656 ? P1 O2 Cu2 133.2(3) . 4_565 ? P1 O3 Cu3 131.6(3) . 2_657 ? P1 O3 Cu1 132.8(3) . 3_667 ? Cu3 O3 Cu1 94.09(18) 2_657 3_667 ? C14 O4 Cu1 132.3(5) . . ? C14 O5 Cu2 134.2(5) . . ? Cu1 O6 Cu2 121.9(2) . . ? Cu2 O7 Cu3 126.1(2) . . ? Cu2 O7 Cu1 102.72(19) . 4_566 ? Cu3 O7 Cu1 105.1(2) . 4_566 ? 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 C1 C2 -67.5(8) . . . . ? O3 P1 C1 C2 55.1(8) . . . . ? O1 P1 C1 C2 172.0(7) . . . . ? P1 C1 C2 C3 105.1(9) . . . . ? P1 C1 C2 C7 -74.6(10) . . . . ? C7 C2 C3 C4 3.1(13) . . . . ? C1 C2 C3 C4 -176.6(8) . . . . ? C2 C3 C4 C5 -1.7(13) . . . . ? C3 C4 C5 C6 0.2(13) . . . . ? C3 C4 C5 C8 -179.9(8) . . . . ? C4 C5 C6 C7 -0.1(13) . . . . ? C8 C5 C6 C7 -180.0(7) . . . . ? C3 C2 C7 C6 -3.0(13) . . . . ? C1 C2 C7 C6 176.7(7) . . . . ? C5 C6 C7 C2 1.5(12) . . . . ? C6 C5 C8 C13 68.3(11) . . . . ? C4 C5 C8 C13 -111.6(10) . . . . ? C6 C5 C8 C9 -105.9(10) . . . . ? C4 C5 C8 C9 74.2(11) . . . . ? C13 C8 C9 C10 3.3(15) . . . . ? C5 C8 C9 C10 177.6(9) . . . . ? C8 C9 C10 C11 -6.2(18) . . . . ? C9 C10 C11 C12 6(2) . . . . ? C10 C11 C12 C13 -2.4(19) . . . . ? C9 C8 C13 C12 0.0(13) . . . . ? C5 C8 C13 C12 -174.1(8) . . . . ? C9 C8 C13 C14 -175.5(8) . . . . ? C5 C8 C13 C14 10.5(13) . . . . ? C11 C12 C13 C8 -0.4(16) . . . . ? C11 C12 C13 C14 175.4(10) . . . . ? C8 C13 C14 O4 19.2(12) . . . . ? C12 C13 C14 O4 -156.3(8) . . . . ? C8 C13 C14 O5 -162.8(8) . . . . ? C12 C13 C14 O5 21.6(12) . . . . ? O2 P1 O1 Cu1 32.0(6) . . . 2_656 ? O3 P1 O1 Cu1 -95.2(5) . . . 2_656 ? C1 P1 O1 Cu1 151.9(5) . . . 2_656 ? O3 P1 O2 Cu2 -44.3(6) . . . 4_565 ? O1 P1 O2 Cu2 -170.3(4) . . . 4_565 ? C1 P1 O2 Cu2 73.5(6) . . . 4_565 ? O2 P1 O3 Cu3 38.7(6) . . . 2_657 ? O1 P1 O3 Cu3 165.1(4) . . . 2_657 ? C1 P1 O3 Cu3 -82.3(5) . . . 2_657 ? O2 P1 O3 Cu1 -159.3(4) . . . 3_667 ? O1 P1 O3 Cu1 -32.9(5) . . . 3_667 ? C1 P1 O3 Cu1 79.7(5) . . . 3_667 ? O5 C14 O4 Cu1 6.8(12) . . . . ? C13 C14 O4 Cu1 -175.4(5) . . . . ? O6 Cu1 O4 C14 -32.3(7) . . . . ? O1 Cu1 O4 C14 -160.1(7) 2_646 . . . ? O7 Cu1 O4 C14 144.1(7) 4_565 . . . ? O3 Cu1 O4 C14 71.5(7) 3_667 . . . ? O4 C14 O5 Cu2 11.0(13) . . . . ? C13 C14 O5 Cu2 -166.8(5) . . . . ? O6 Cu2 O5 C14 4.2(8) . . . . ? O2 Cu2 O5 C14 107.9(8) 4_566 . . . ? O7 Cu2 O5 C14 -163.7(8) . . . . ? O1 Cu1 O6 Cu2 -149.1(4) 2_646 . . . ? O4 Cu1 O6 Cu2 45.5(4) . . . . ? O7 Cu1 O6 Cu2 -59(3) 4_565 . . . ? O3 Cu1 O6 Cu2 -45.6(4) 3_667 . . . ? O2 Cu2 O6 Cu1 173.3(4) 4_566 . . . ? O7 Cu2 O6 Cu1 55.8(12) . . . . ? O5 Cu2 O6 Cu1 -36.4(4) . . . . ? O6 Cu2 O7 Cu3 75.6(11) . . . . ? O2 Cu2 O7 Cu3 -41.7(3) 4_566 . . . ? O5 Cu2 O7 Cu3 169.0(3) . . . . ? O6 Cu2 O7 Cu1 -44.1(11) . . . 4_566 ? O2 Cu2 O7 Cu1 -161.4(3) 4_566 . . 4_566 ? O5 Cu2 O7 Cu1 49.2(3) . . . 4_566 ? O3 Cu3 O7 Cu2 -135.2(3) 2_647 . . . ? O3 Cu3 O7 Cu2 44.8(3) 4_566 . . . ? O7 Cu3 O7 Cu2 155(100) 3_658 . . . ? O3 Cu3 O7 Cu1 -16.5(2) 2_647 . . 4_566 ? O3 Cu3 O7 Cu1 163.5(2) 4_566 . . 4_566 ? O7 Cu3 O7 Cu1 -86(100) 3_658 . . 4_566 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.773 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.143 #======================================== data_compound-3 _database_code_depnum_ccdc_archive 'CCDC 852763' #TrackingRef 'Crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H20 O10 P2 Zn3, (H2 O)' _chemical_formula_sum 'C28 H22 O11 P2 Zn3' _chemical_formula_weight 792.51 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' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_hall '-P 2ybc' 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 15.076(5) _cell_length_b 10.156(5) _cell_length_c 19.074(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 99.099(5) _cell_angle_gamma 90.000(5) _cell_volume 2883.7(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3025 _cell_measurement_theta_min 3.0984 _cell_measurement_theta_max 29.0609 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.825 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 2.648 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6062 _exptl_absorpt_correction_T_max 0.6766 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11778 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.0781 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5257 _reflns_number_gt 3845 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0373P)^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 5257 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1039 _refine_ls_wR_factor_gt 0.0910 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Zn1 Zn 0.63043(4) 0.03299(6) 0.94740(3) 0.02434(16) Uani 1 1 d . . . Zn2 Zn 0.53194(4) 0.32506(6) 0.92052(3) 0.02448(16) Uani 1 1 d . . . Zn3 Zn 0.58842(4) -0.18808(5) 0.80544(3) 0.02201(16) Uani 1 1 d . . . P1 P 0.59719(9) -0.23672(13) 0.46835(6) 0.0232(3) Uani 1 1 d . . . P2 P 0.52544(8) 0.58608(13) 0.67905(6) 0.0204(3) Uani 1 1 d . . . C1 C 0.7092(3) -0.1718(5) 0.4862(2) 0.0307(12) Uani 1 1 d . . . H1A H 0.7485 -0.2311 0.4656 0.037 Uiso 1 1 calc R . . H1B H 0.7099 -0.0881 0.4618 0.037 Uiso 1 1 calc R . . C2 C 0.7485(3) -0.1508(5) 0.5634(2) 0.0281(12) Uani 1 1 d . . . C3 C 0.8158(3) -0.2316(6) 0.5968(3) 0.0353(13) Uani 1 1 d . . . H3 H 0.8325 -0.3053 0.5730 0.042 Uiso 1 1 calc R . . C4 C 0.8590(3) -0.2055(6) 0.6648(3) 0.0352(13) Uani 1 1 d . . . H4 H 0.9053 -0.2604 0.6854 0.042 Uiso 1 1 calc R . . C5 C 0.8346(3) -0.0992(5) 0.7028(3) 0.0297(12) Uani 1 1 d . . . C6 C 0.7640(4) -0.0192(5) 0.6703(3) 0.0338(13) Uani 1 1 d . . . H6 H 0.7449 0.0518 0.6949 0.041 Uiso 1 1 calc R . . C7 C 0.7227(4) -0.0461(5) 0.6017(3) 0.0346(13) Uani 1 1 d . . . H7 H 0.6762 0.0080 0.5809 0.042 Uiso 1 1 calc R . . C8 C 0.8880(3) -0.0629(5) 0.7730(2) 0.0294(12) Uani 1 1 d . . . C9 C 0.9811(4) -0.0524(6) 0.7765(3) 0.0399(14) Uani 1 1 d . . . H9 H 1.0063 -0.0732 0.7364 0.048 Uiso 1 1 calc R . . C10 C 1.0367(4) -0.0129(6) 0.8366(3) 0.0423(15) Uani 1 1 d . . . H10 H 1.0985 -0.0095 0.8375 0.051 Uiso 1 1 calc R . . C11 C 1.0001(4) 0.0220(6) 0.8960(3) 0.0394(14) Uani 1 1 d . . . H11 H 1.0367 0.0534 0.9363 0.047 Uiso 1 1 calc R . . C12 C 0.9095(4) 0.0101(5) 0.8949(3) 0.0341(13) Uani 1 1 d . . . H12 H 0.8852 0.0334 0.9351 0.041 Uiso 1 1 calc R . . C13 C 0.8528(3) -0.0362(5) 0.8352(2) 0.0276(12) Uani 1 1 d . . . C14 C 0.7568(3) -0.0618(5) 0.8431(2) 0.0268(12) Uani 1 1 d . . . C15 C 0.6265(3) 0.5148(5) 0.6575(2) 0.0319(13) Uani 1 1 d . . . H15A H 0.6112 0.4406 0.6258 0.038 Uiso 1 1 calc R . . H15B H 0.6574 0.5795 0.6327 0.038 Uiso 1 1 calc R . . C16 C 0.6885(3) 0.4689(5) 0.7230(3) 0.0294(12) Uani 1 1 d . . . C17 C 0.7474(3) 0.5556(5) 0.7621(3) 0.0346(13) Uani 1 1 d . . . H17 H 0.7517 0.6412 0.7457 0.041 Uiso 1 1 calc R . . C18 C 0.8003(3) 0.5180(5) 0.8251(3) 0.0335(13) Uani 1 1 d . . . H18 H 0.8402 0.5781 0.8498 0.040 Uiso 1 1 calc R . . C19 C 0.7943(3) 0.3914(5) 0.8517(3) 0.0322(13) Uani 1 1 d . . . C20 C 0.7358(4) 0.3037(5) 0.8117(3) 0.0365(14) Uani 1 1 d . . . H20 H 0.7314 0.2178 0.8277 0.044 Uiso 1 1 calc R . . C21 C 0.6843(4) 0.3420(6) 0.7488(3) 0.0371(14) Uani 1 1 d . . . H21 H 0.6459 0.2813 0.7232 0.045 Uiso 1 1 calc R . . C22 C 0.8493(3) 0.3539(5) 0.9210(3) 0.0285(12) Uani 1 1 d . . . C23 C 0.9414(4) 0.3714(6) 0.9300(3) 0.0385(14) Uani 1 1 d . . . H23 H 0.9669 0.4058 0.8926 0.046 Uiso 1 1 calc R . . C24 C 0.9965(4) 0.3398(6) 0.9923(3) 0.0453(15) Uani 1 1 d . . . H24 H 1.0582 0.3522 0.9961 0.054 Uiso 1 1 calc R . . C25 C 0.9612(4) 0.2902(6) 1.0487(3) 0.0437(15) Uani 1 1 d . . . H25 H 0.9981 0.2715 1.0914 0.052 Uiso 1 1 calc R . . C26 C 0.8699(4) 0.2684(6) 1.0410(3) 0.0397(14) Uani 1 1 d . . . H26 H 0.8457 0.2314 1.0784 0.048 Uiso 1 1 calc R . . C27 C 0.8131(4) 0.3007(5) 0.9785(3) 0.0296(12) Uani 1 1 d . . . C28 C 0.7157(4) 0.2758(6) 0.9758(2) 0.0307(12) Uani 1 1 d . . . O1 O 0.5390(2) -0.1527(3) 0.50772(15) 0.0276(8) Uani 1 1 d . . . O2 O 0.5653(2) -0.2215(3) 0.38853(15) 0.0306(8) Uani 1 1 d . . . O3 O 0.5980(2) -0.3798(3) 0.49105(16) 0.0304(8) Uani 1 1 d . . . O4 O 0.7139(2) -0.1468(4) 0.80431(18) 0.0348(9) Uani 1 1 d . . . O5 O 0.7266(2) 0.0016(4) 0.89067(18) 0.0382(9) Uani 1 1 d . . . O6 O 0.4669(2) 0.6347(3) 0.60897(15) 0.0231(7) Uani 1 1 d . . . O7 O 0.4751(2) 0.4807(3) 0.71258(15) 0.0288(8) Uani 1 1 d . . . O8 O 0.5473(2) 0.7038(3) 0.72523(16) 0.0306(8) Uani 1 1 d . . . O9 O 0.6918(2) 0.1733(3) 1.00578(16) 0.0330(9) Uani 1 1 d . . . O10 O 0.6606(2) 0.3578(4) 0.94468(17) 0.0337(9) Uani 1 1 d . . . O1W O 0.4976(2) 0.4748(3) 0.85613(16) 0.0330(9) 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 Zn1 0.0333(4) 0.0166(3) 0.0227(3) 0.0006(2) 0.0034(2) -0.0017(3) Zn2 0.0302(4) 0.0190(3) 0.0252(3) 0.0006(2) 0.0072(2) -0.0019(3) Zn3 0.0293(3) 0.0185(3) 0.0179(3) -0.0011(2) 0.0029(2) -0.0026(3) P1 0.0357(8) 0.0169(7) 0.0177(6) -0.0010(5) 0.0068(5) 0.0027(6) P2 0.0286(7) 0.0157(7) 0.0163(6) -0.0005(5) 0.0021(5) 0.0002(6) C1 0.036(3) 0.026(3) 0.032(3) -0.002(2) 0.010(2) -0.001(3) C2 0.032(3) 0.026(3) 0.028(3) -0.001(2) 0.011(2) -0.008(3) C3 0.036(3) 0.033(3) 0.038(3) -0.007(3) 0.007(2) 0.006(3) C4 0.030(3) 0.039(4) 0.036(3) 0.002(3) 0.005(2) 0.011(3) C5 0.029(3) 0.028(3) 0.035(3) 0.003(2) 0.013(2) -0.001(3) C6 0.040(3) 0.031(3) 0.032(3) -0.006(2) 0.011(2) 0.004(3) C7 0.035(3) 0.036(3) 0.033(3) 0.003(3) 0.005(2) 0.010(3) C8 0.030(3) 0.028(3) 0.031(3) 0.004(2) 0.007(2) -0.002(3) C9 0.040(4) 0.048(4) 0.033(3) 0.001(3) 0.011(3) -0.003(3) C10 0.029(3) 0.045(4) 0.054(4) 0.003(3) 0.008(3) -0.008(3) C11 0.037(4) 0.039(4) 0.040(3) -0.003(3) -0.004(3) -0.012(3) C12 0.039(3) 0.030(3) 0.034(3) -0.008(3) 0.006(2) -0.002(3) C13 0.030(3) 0.024(3) 0.029(3) 0.001(2) 0.006(2) -0.005(2) C14 0.034(3) 0.024(3) 0.024(3) 0.005(2) 0.007(2) 0.005(3) C15 0.044(3) 0.032(3) 0.021(2) 0.003(2) 0.007(2) 0.011(3) C16 0.031(3) 0.029(3) 0.030(3) 0.000(2) 0.011(2) 0.010(3) C17 0.035(3) 0.026(3) 0.044(3) 0.009(3) 0.011(3) -0.003(3) C18 0.030(3) 0.026(3) 0.043(3) -0.001(3) 0.002(2) -0.004(3) C19 0.030(3) 0.032(3) 0.036(3) 0.004(3) 0.007(2) 0.000(3) C20 0.048(4) 0.023(3) 0.036(3) 0.008(3) 0.002(3) 0.002(3) C21 0.046(4) 0.027(3) 0.035(3) -0.008(3) -0.004(2) 0.002(3) C22 0.031(3) 0.019(3) 0.035(3) -0.003(2) 0.003(2) 0.001(2) C23 0.031(3) 0.039(4) 0.047(3) 0.005(3) 0.011(3) -0.004(3) C24 0.035(4) 0.042(4) 0.056(4) -0.001(3) -0.002(3) 0.001(3) C25 0.042(4) 0.039(4) 0.045(3) 0.004(3) -0.009(3) 0.002(3) C26 0.046(4) 0.036(4) 0.035(3) 0.006(3) 0.001(3) -0.005(3) C27 0.038(3) 0.017(3) 0.034(3) -0.002(2) 0.006(2) -0.001(2) C28 0.040(3) 0.029(3) 0.023(3) -0.004(2) 0.004(2) -0.002(3) O1 0.037(2) 0.023(2) 0.0258(17) -0.0023(15) 0.0160(14) 0.0033(17) O2 0.046(2) 0.029(2) 0.0171(16) -0.0029(15) 0.0069(14) 0.0084(18) O3 0.052(2) 0.0160(19) 0.0254(18) -0.0011(15) 0.0134(15) 0.0041(17) O4 0.029(2) 0.034(2) 0.042(2) -0.0151(18) 0.0105(16) -0.0087(18) O5 0.038(2) 0.042(2) 0.038(2) -0.0078(19) 0.0193(17) -0.0010(19) O6 0.033(2) 0.0151(18) 0.0204(16) 0.0026(14) 0.0022(13) 0.0001(15) O7 0.041(2) 0.0217(19) 0.0227(17) 0.0033(15) 0.0032(14) -0.0087(17) O8 0.041(2) 0.022(2) 0.0274(18) -0.0059(15) 0.0001(15) -0.0020(17) O9 0.047(2) 0.026(2) 0.0238(18) -0.0031(16) -0.0010(15) -0.0169(18) O10 0.028(2) 0.029(2) 0.043(2) 0.0008(18) 0.0025(16) -0.0042(18) O1W 0.051(2) 0.024(2) 0.0235(17) 0.0056(15) 0.0039(15) -0.0032(18) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Zn1 O3 1.866(3) 4_556 ? Zn1 O9 1.949(3) . ? Zn1 O5 1.968(3) . ? Zn1 O6 1.969(3) 2_646 ? Zn2 O1 1.879(3) 2_656 ? Zn2 O10 1.950(3) . ? Zn2 O1W 1.972(3) . ? Zn2 O6 2.014(3) 2_646 ? Zn3 O8 1.905(3) 1_545 ? Zn3 O2 1.911(3) 4_556 ? Zn3 O4 1.941(3) . ? Zn3 O7 1.968(3) 2_646 ? P1 O1 1.507(3) . ? P1 O3 1.516(4) . ? P1 O2 1.530(3) . ? P1 C1 1.795(5) . ? P2 O8 1.491(3) . ? P2 O7 1.511(3) . ? P2 O6 1.561(3) . ? P2 C15 1.792(5) . ? C1 C2 1.512(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.380(7) . ? C2 C7 1.381(7) . ? C3 C4 1.383(7) . ? C3 H3 0.9300 . ? C4 C5 1.382(7) . ? C4 H4 0.9300 . ? C5 C6 1.403(7) . ? C5 C8 1.495(7) . ? C6 C7 1.384(7) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.399(7) . ? C8 C13 1.401(7) . ? C9 C10 1.369(7) . ? C9 H9 0.9300 . ? C10 C11 1.382(7) . ? C10 H10 0.9300 . ? C11 C12 1.368(7) . ? C11 H11 0.9300 . ? C12 C13 1.393(7) . ? C12 H12 0.9300 . ? C13 C14 1.500(7) . ? C14 O4 1.249(6) . ? C14 O5 1.255(6) . ? C15 C16 1.511(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.382(7) . ? C16 C21 1.385(7) . ? C17 C18 1.387(7) . ? C17 H17 0.9300 . ? C18 C19 1.391(7) . ? C18 H18 0.9300 . ? C19 C20 1.394(7) . ? C19 C22 1.494(7) . ? C20 C21 1.377(7) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.382(7) . ? C22 C27 1.408(7) . ? C23 C24 1.377(7) . ? C23 H23 0.9300 . ? C24 C25 1.370(8) . ? C24 H24 0.9300 . ? C25 C26 1.378(8) . ? C25 H25 0.9300 . ? C26 C27 1.393(7) . ? C26 H26 0.9300 . ? C27 C28 1.484(7) . ? C28 O10 1.257(6) . ? C28 O9 1.267(6) . ? O1 Zn2 1.879(3) 2_646 ? O2 Zn3 1.911(3) 4 ? O3 Zn1 1.866(3) 4 ? O6 Zn1 1.969(3) 2_656 ? O6 Zn2 2.014(3) 2_656 ? O7 Zn3 1.968(3) 2_656 ? O8 Zn3 1.905(3) 1_565 ? 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 O3 Zn1 O9 119.26(14) 4_556 . ? O3 Zn1 O5 112.22(15) 4_556 . ? O9 Zn1 O5 96.20(15) . . ? O3 Zn1 O6 117.12(15) 4_556 2_646 ? O9 Zn1 O6 100.01(14) . 2_646 ? O5 Zn1 O6 109.58(14) . 2_646 ? O1 Zn2 O10 117.81(14) 2_656 . ? O1 Zn2 O1W 103.73(14) 2_656 . ? O10 Zn2 O1W 99.72(15) . . ? O1 Zn2 O6 110.50(14) 2_656 2_646 ? O10 Zn2 O6 100.21(14) . 2_646 ? O1W Zn2 O6 125.41(13) . 2_646 ? O8 Zn3 O2 108.08(15) 1_545 4_556 ? O8 Zn3 O4 108.00(14) 1_545 . ? O2 Zn3 O4 114.76(15) 4_556 . ? O8 Zn3 O7 105.94(14) 1_545 2_646 ? O2 Zn3 O7 114.58(14) 4_556 2_646 ? O4 Zn3 O7 104.97(15) . 2_646 ? O1 P1 O3 112.30(18) . . ? O1 P1 O2 108.83(19) . . ? O3 P1 O2 111.59(19) . . ? O1 P1 C1 107.6(2) . . ? O3 P1 C1 109.5(2) . . ? O2 P1 C1 106.8(2) . . ? O8 P2 O7 113.38(18) . . ? O8 P2 O6 107.14(19) . . ? O7 P2 O6 109.44(18) . . ? O8 P2 C15 110.0(2) . . ? O7 P2 C15 108.2(2) . . ? O6 P2 C15 108.51(19) . . ? C2 C1 P1 116.6(3) . . ? C2 C1 H1A 108.1 . . ? P1 C1 H1A 108.1 . . ? C2 C1 H1B 108.1 . . ? P1 C1 H1B 108.1 . . ? H1A C1 H1B 107.3 . . ? C3 C2 C7 117.5(5) . . ? C3 C2 C1 120.8(5) . . ? C7 C2 C1 121.7(5) . . ? C2 C3 C4 121.5(5) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C5 C4 C3 121.1(5) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 117.8(5) . . ? C4 C5 C8 120.8(5) . . ? C6 C5 C8 121.1(5) . . ? C7 C6 C5 120.0(5) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C2 C7 C6 122.1(5) . . ? C2 C7 H7 119.0 . . ? C6 C7 H7 119.0 . . ? C9 C8 C13 117.2(4) . . ? C9 C8 C5 117.1(4) . . ? C13 C8 C5 125.7(5) . . ? C10 C9 C8 122.6(5) . . ? C10 C9 H9 118.7 . . ? C8 C9 H9 118.7 . . ? C9 C10 C11 119.4(5) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C12 C11 C10 119.5(5) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C13 121.6(5) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C12 C13 C8 119.4(5) . . ? C12 C13 C14 117.0(4) . . ? C8 C13 C14 123.5(4) . . ? O4 C14 O5 124.7(5) . . ? O4 C14 C13 118.6(4) . . ? O5 C14 C13 116.7(4) . . ? C16 C15 P2 111.8(3) . . ? C16 C15 H15A 109.2 . . ? P2 C15 H15A 109.2 . . ? C16 C15 H15B 109.2 . . ? P2 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C17 C16 C21 117.5(5) . . ? C17 C16 C15 120.7(5) . . ? C21 C16 C15 121.7(5) . . ? C16 C17 C18 121.7(5) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C17 C18 C19 120.6(5) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C20 117.6(5) . . ? C18 C19 C22 119.9(5) . . ? C20 C19 C22 122.4(5) . . ? C21 C20 C19 121.1(5) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C16 121.5(5) . . ? C20 C21 H21 119.3 . . ? C16 C21 H21 119.3 . . ? C23 C22 C27 117.3(5) . . ? C23 C22 C19 118.9(4) . . ? C27 C22 C19 123.9(5) . . ? C24 C23 C22 122.3(5) . . ? C24 C23 H23 118.9 . . ? C22 C23 H23 118.9 . . ? C25 C24 C23 120.5(6) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 118.7(5) . . ? C24 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? C25 C26 C27 121.4(5) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C26 C27 C22 119.7(5) . . ? C26 C27 C28 117.4(4) . . ? C22 C27 C28 122.9(4) . . ? O10 C28 O9 123.0(5) . . ? O10 C28 C27 118.7(5) . . ? O9 C28 C27 118.3(5) . . ? P1 O1 Zn2 137.6(2) . 2_646 ? P1 O2 Zn3 135.0(2) . 4 ? P1 O3 Zn1 131.50(19) . 4 ? C14 O4 Zn3 123.9(3) . . ? C14 O5 Zn1 149.7(4) . . ? P2 O6 Zn1 124.97(19) . 2_656 ? P2 O6 Zn2 120.93(18) . 2_656 ? Zn1 O6 Zn2 112.95(14) 2_656 2_656 ? P2 O7 Zn3 143.74(19) . 2_656 ? P2 O8 Zn3 161.9(2) . 1_565 ? C28 O9 Zn1 119.1(3) . . ? C28 O10 Zn2 123.9(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 P1 C1 C2 51.4(4) . . . . ? O3 P1 C1 C2 -70.8(4) . . . . ? O2 P1 C1 C2 168.2(4) . . . . ? P1 C1 C2 C3 108.3(5) . . . . ? P1 C1 C2 C7 -75.7(6) . . . . ? C7 C2 C3 C4 -3.1(8) . . . . ? C1 C2 C3 C4 173.0(5) . . . . ? C2 C3 C4 C5 1.9(8) . . . . ? C3 C4 C5 C6 0.5(8) . . . . ? C3 C4 C5 C8 -173.2(5) . . . . ? C4 C5 C6 C7 -1.6(7) . . . . ? C8 C5 C6 C7 172.2(5) . . . . ? C3 C2 C7 C6 2.1(8) . . . . ? C1 C2 C7 C6 -174.1(5) . . . . ? C5 C6 C7 C2 0.3(8) . . . . ? C4 C5 C8 C9 49.5(7) . . . . ? C6 C5 C8 C9 -124.1(5) . . . . ? C4 C5 C8 C13 -131.8(6) . . . . ? C6 C5 C8 C13 54.6(7) . . . . ? C13 C8 C9 C10 -2.5(8) . . . . ? C5 C8 C9 C10 176.3(5) . . . . ? C8 C9 C10 C11 -1.9(9) . . . . ? C9 C10 C11 C12 3.3(9) . . . . ? C10 C11 C12 C13 -0.2(8) . . . . ? C11 C12 C13 C8 -4.3(8) . . . . ? C11 C12 C13 C14 172.3(5) . . . . ? C9 C8 C13 C12 5.6(8) . . . . ? C5 C8 C13 C12 -173.2(5) . . . . ? C9 C8 C13 C14 -170.8(5) . . . . ? C5 C8 C13 C14 10.4(8) . . . . ? C12 C13 C14 O4 -152.4(5) . . . . ? C8 C13 C14 O4 24.0(7) . . . . ? C12 C13 C14 O5 25.1(7) . . . . ? C8 C13 C14 O5 -158.5(5) . . . . ? O8 P2 C15 C16 61.3(4) . . . . ? O7 P2 C15 C16 -63.1(4) . . . . ? O6 P2 C15 C16 178.2(4) . . . . ? P2 C15 C16 C17 -84.7(5) . . . . ? P2 C15 C16 C21 90.8(5) . . . . ? C21 C16 C17 C18 -0.3(8) . . . . ? C15 C16 C17 C18 175.3(5) . . . . ? C16 C17 C18 C19 -1.2(8) . . . . ? C17 C18 C19 C20 2.0(8) . . . . ? C17 C18 C19 C22 -177.8(5) . . . . ? C18 C19 C20 C21 -1.3(8) . . . . ? C22 C19 C20 C21 178.4(5) . . . . ? C19 C20 C21 C16 -0.2(8) . . . . ? C17 C16 C21 C20 1.0(8) . . . . ? C15 C16 C21 C20 -174.6(5) . . . . ? C18 C19 C22 C23 -54.9(7) . . . . ? C20 C19 C22 C23 125.4(6) . . . . ? C18 C19 C22 C27 125.3(6) . . . . ? C20 C19 C22 C27 -54.4(7) . . . . ? C27 C22 C23 C24 -0.5(8) . . . . ? C19 C22 C23 C24 179.7(5) . . . . ? C22 C23 C24 C25 -0.6(9) . . . . ? C23 C24 C25 C26 2.2(9) . . . . ? C24 C25 C26 C27 -2.6(9) . . . . ? C25 C26 C27 C22 1.5(8) . . . . ? C25 C26 C27 C28 -178.9(5) . . . . ? C23 C22 C27 C26 0.0(7) . . . . ? C19 C22 C27 C26 179.8(5) . . . . ? C23 C22 C27 C28 -179.5(5) . . . . ? C19 C22 C27 C28 0.3(8) . . . . ? C26 C27 C28 O10 141.6(5) . . . . ? C22 C27 C28 O10 -38.9(7) . . . . ? C26 C27 C28 O9 -37.6(7) . . . . ? C22 C27 C28 O9 141.9(5) . . . . ? O3 P1 O1 Zn2 1.7(4) . . . 2_646 ? O2 P1 O1 Zn2 125.8(3) . . . 2_646 ? C1 P1 O1 Zn2 -118.8(3) . . . 2_646 ? O1 P1 O2 Zn3 -167.8(3) . . . 4 ? O3 P1 O2 Zn3 -43.4(4) . . . 4 ? C1 P1 O2 Zn3 76.3(4) . . . 4 ? O1 P1 O3 Zn1 161.6(3) . . . 4 ? O2 P1 O3 Zn1 39.1(3) . . . 4 ? C1 P1 O3 Zn1 -79.0(3) . . . 4 ? O5 C14 O4 Zn3 4.8(7) . . . . ? C13 C14 O4 Zn3 -177.9(3) . . . . ? O8 Zn3 O4 C14 168.5(4) 1_545 . . . ? O2 Zn3 O4 C14 -70.8(4) 4_556 . . . ? O7 Zn3 O4 C14 55.9(4) 2_646 . . . ? O4 C14 O5 Zn1 6.0(10) . . . . ? C13 C14 O5 Zn1 -171.3(5) . . . . ? O3 Zn1 O5 C14 53.0(7) 4_556 . . . ? O9 Zn1 O5 C14 178.1(7) . . . . ? O6 Zn1 O5 C14 -78.9(7) 2_646 . . . ? O8 P2 O6 Zn1 -146.2(2) . . . 2_656 ? O7 P2 O6 Zn1 -22.9(3) . . . 2_656 ? C15 P2 O6 Zn1 95.0(3) . . . 2_656 ? O8 P2 O6 Zn2 20.7(3) . . . 2_656 ? O7 P2 O6 Zn2 144.0(2) . . . 2_656 ? C15 P2 O6 Zn2 -98.1(3) . . . 2_656 ? O8 P2 O7 Zn3 172.5(3) . . . 2_656 ? O6 P2 O7 Zn3 53.0(4) . . . 2_656 ? C15 P2 O7 Zn3 -65.1(4) . . . 2_656 ? O7 P2 O8 Zn3 49.0(8) . . . 1_565 ? O6 P2 O8 Zn3 169.8(7) . . . 1_565 ? C15 P2 O8 Zn3 -72.4(8) . . . 1_565 ? O10 C28 O9 Zn1 68.5(6) . . . . ? C27 C28 O9 Zn1 -112.3(4) . . . . ? O3 Zn1 O9 C28 178.3(4) 4_556 . . . ? O5 Zn1 O9 C28 58.5(4) . . . . ? O6 Zn1 O9 C28 -52.7(4) 2_646 . . . ? O9 C28 O10 Zn2 -13.0(6) . . . . ? C27 C28 O10 Zn2 167.9(3) . . . . ? O1 Zn2 O10 C28 81.1(4) 2_656 . . . ? O1W Zn2 O10 C28 -167.7(4) . . . . ? O6 Zn2 O10 C28 -38.8(4) 2_646 . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.684 _refine_diff_density_min -0.571 _refine_diff_density_rms 0.111 #======================================== data_compound-4 _database_code_depnum_ccdc_archive 'CCDC 852764' #TrackingRef 'Crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_absolute_configuration unk _chemical_formula_moiety 'C52 H36 N4 O10 P2 Zn3, 2(H2 O)' _chemical_formula_sum 'C52 H40 N4 O12 P2 Zn3' _chemical_formula_weight 1170.93 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' 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' Zn Zn 0.2839 1.4301 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M p212121 _symmetry_space_group_name_hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.5652(2) _cell_length_b 17.5422(4) _cell_length_c 25.6946(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4762.16(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7196 _cell_measurement_theta_min 0.98167 _cell_measurement_theta_max 1.00000 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_absorpt_coefficient_mu 1.637 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.98167 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19208 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8709 _reflns_number_gt 7755 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0274P)^2^+0.2069P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.010(8) _refine_ls_number_reflns 8709 _refine_ls_number_parameters 658 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0712 _refine_ls_wR_factor_gt 0.0674 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 Zn1 Zn 1.12473(4) 0.34421(2) 0.604945(16) 0.02563(11) Uani 1 1 d . . . Zn2 Zn 1.49003(3) 0.33062(2) 0.511566(15) 0.02182(10) Uani 1 1 d . . . Zn3 Zn 1.67897(4) 0.04218(3) 0.878612(17) 0.02805(11) Uani 1 1 d . . . P1 P 1.40723(8) 0.36677(6) 0.63025(4) 0.0240(2) Uani 1 1 d . . . P2 P 1.70531(8) 0.19163(6) 0.51241(4) 0.0235(2) Uani 1 1 d . . . C1 C 1.5246(3) 0.3268(2) 0.67408(14) 0.0324(9) Uani 1 1 d . . . H1A H 1.5506 0.2778 0.6603 0.039 Uiso 1 1 calc R . . H1B H 1.5983 0.3598 0.6735 0.039 Uiso 1 1 calc R . . C2 C 1.4865(3) 0.3155(2) 0.73002(15) 0.0302(9) Uani 1 1 d . . . C3 C 1.4869(4) 0.3752(2) 0.76468(15) 0.0369(10) Uani 1 1 d . . . H3 H 1.5100 0.4234 0.7530 0.044 Uiso 1 1 calc R . . C4 C 1.4539(4) 0.3656(2) 0.81665(15) 0.0333(10) Uani 1 1 d . . . H4 H 1.4519 0.4076 0.8388 0.040 Uiso 1 1 calc R . . C5 C 1.4238(3) 0.2936(2) 0.83584(15) 0.0267(9) Uani 1 1 d . . . C6 C 1.4218(4) 0.2336(2) 0.80049(16) 0.0351(10) Uani 1 1 d . . . H6 H 1.4008 0.1849 0.8121 0.042 Uiso 1 1 calc R . . C7 C 1.4503(4) 0.2446(2) 0.74858(16) 0.0340(10) Uani 1 1 d . . . H7 H 1.4450 0.2037 0.7257 0.041 Uiso 1 1 calc R . . C8 C 1.3918(3) 0.2820(2) 0.89162(15) 0.0272(9) Uani 1 1 d . . . C9 C 1.3061(3) 0.3303(2) 0.91607(15) 0.0339(9) Uani 1 1 d . . . H9 H 1.2744 0.3720 0.8979 0.041 Uiso 1 1 calc R . . C10 C 1.2668(4) 0.3181(3) 0.96662(17) 0.0408(11) Uani 1 1 d . . . H10 H 1.2111 0.3521 0.9823 0.049 Uiso 1 1 calc R . . C11 C 1.3098(4) 0.2559(3) 0.99372(17) 0.0430(11) Uani 1 1 d . . . H11 H 1.2814 0.2464 1.0274 0.052 Uiso 1 1 calc R . . C12 C 1.3956(4) 0.2076(2) 0.97034(15) 0.0363(10) Uani 1 1 d . . . H12 H 1.4250 0.1655 0.9888 0.044 Uiso 1 1 calc R . . C13 C 1.4396(3) 0.2200(2) 0.91988(15) 0.0276(9) Uani 1 1 d . . . C14 C 1.5461(3) 0.1714(2) 0.90012(14) 0.0283(9) Uani 1 1 d . . . C15 C 1.9327(4) 0.0876(2) 0.93141(16) 0.0335(10) Uani 1 1 d . . . H15 H 1.9007 0.0647 0.9612 0.040 Uiso 1 1 calc R . . C16 C 2.0489(4) 0.1240(3) 0.93439(18) 0.0441(11) Uani 1 1 d . . . H16 H 2.0937 0.1245 0.9655 0.053 Uiso 1 1 calc R . . C17 C 2.0970(4) 0.1588(2) 0.89168(18) 0.0438(11) Uani 1 1 d . . . H17 H 2.1746 0.1836 0.8934 0.053 Uiso 1 1 calc R . . C18 C 2.0292(3) 0.1572(2) 0.84498(16) 0.0349(10) Uani 1 1 d . . . C19 C 2.0720(4) 0.1924(3) 0.7978(2) 0.0534(13) Uani 1 1 d . . . H19 H 2.1488 0.2183 0.7976 0.064 Uiso 1 1 calc R . . C20 C 2.0028(5) 0.1887(3) 0.7539(2) 0.0594(14) Uani 1 1 d . . . H20 H 2.0332 0.2116 0.7237 0.071 Uiso 1 1 calc R . . C21 C 1.8840(4) 0.1504(3) 0.75268(17) 0.0465(12) Uani 1 1 d . . . C22 C 1.8086(5) 0.1433(3) 0.70830(18) 0.0624(15) Uani 1 1 d . . . H22 H 1.8355 0.1639 0.6768 0.075 Uiso 1 1 calc R . . C23 C 1.6964(5) 0.1065(3) 0.71123(18) 0.0590(15) Uani 1 1 d . . . H23 H 1.6462 0.1012 0.6817 0.071 Uiso 1 1 calc R . . C24 C 1.6564(4) 0.0766(3) 0.75845(17) 0.0461(12) Uani 1 1 d . . . H24 H 1.5785 0.0521 0.7600 0.055 Uiso 1 1 calc R . . C25 C 1.8385(4) 0.1174(2) 0.79860(15) 0.0313(9) Uani 1 1 d . . . C26 C 1.9127(3) 0.1196(2) 0.84516(16) 0.0298(9) Uani 1 1 d . . . C27 C 1.6758(4) 0.1440(3) 0.57390(15) 0.0425(11) Uani 1 1 d . . . H27A H 1.7458 0.1095 0.5804 0.051 Uiso 1 1 calc R . . H27B H 1.6771 0.1822 0.6012 0.051 Uiso 1 1 calc R . . C28 C 1.5545(4) 0.0992(3) 0.57919(15) 0.0332(10) Uani 1 1 d . . . C29 C 1.5524(4) 0.0222(3) 0.56643(15) 0.0359(10) Uani 1 1 d . . . H29 H 1.6255 -0.0007 0.5538 0.043 Uiso 1 1 calc R . . C30 C 1.4445(3) -0.0209(2) 0.57209(15) 0.0334(10) Uani 1 1 d . . . H30 H 1.4459 -0.0719 0.5623 0.040 Uiso 1 1 calc R . . C31 C 1.3326(3) 0.0102(2) 0.59225(15) 0.0271(9) Uani 1 1 d . . . C32 C 1.3355(4) 0.0873(2) 0.60480(16) 0.0359(10) Uani 1 1 d . . . H32 H 1.2632 0.1102 0.6182 0.043 Uiso 1 1 calc R . . C33 C 1.4442(4) 0.1308(3) 0.59770(16) 0.0401(10) Uani 1 1 d . . . H33 H 1.4423 0.1825 0.6057 0.048 Uiso 1 1 calc R . . C34 C 1.2202(3) -0.0398(2) 0.59915(14) 0.0260(8) Uani 1 1 d . . . C35 C 1.2389(4) -0.1148(2) 0.61539(16) 0.0357(10) Uani 1 1 d . . . H35 H 1.3208 -0.1307 0.6230 0.043 Uiso 1 1 calc R . . C36 C 1.1410(3) -0.1663(2) 0.62069(16) 0.0385(10) Uani 1 1 d . . . H36 H 1.1568 -0.2155 0.6326 0.046 Uiso 1 1 calc R . . C37 C 1.0198(4) -0.1442(2) 0.60818(16) 0.0363(10) Uani 1 1 d . . . H37 H 0.9532 -0.1787 0.6105 0.044 Uiso 1 1 calc R . . C38 C 0.9983(4) -0.0710(2) 0.59228(15) 0.0320(9) Uani 1 1 d . . . H38 H 0.9162 -0.0566 0.5837 0.038 Uiso 1 1 calc R . . C39 C 1.0941(3) -0.0175(2) 0.58846(13) 0.0232(8) Uani 1 1 d . . . C40 C 1.0539(3) 0.0618(2) 0.57448(15) 0.0266(9) Uani 1 1 d . . . C41 C 0.8914(4) 0.4142(3) 0.54655(16) 0.0360(10) Uani 1 1 d . . . H41 H 0.9266 0.3921 0.5170 0.043 Uiso 1 1 calc R . . C42 C 0.7746(4) 0.4500(3) 0.54215(18) 0.0428(11) Uani 1 1 d . . . H42 H 0.7337 0.4519 0.5101 0.051 Uiso 1 1 calc R . . C43 C 0.7201(4) 0.4821(3) 0.58477(18) 0.0414(12) Uani 1 1 d . . . H43 H 0.6421 0.5064 0.5823 0.050 Uiso 1 1 calc R . . C44 C 0.7836(3) 0.4779(2) 0.63256(17) 0.0330(10) Uani 1 1 d . . . C45 C 0.7353(4) 0.5097(3) 0.6804(2) 0.0450(12) Uani 1 1 d . . . H45 H 0.6569 0.5338 0.6802 0.054 Uiso 1 1 calc R . . C46 C 0.7999(4) 0.5055(3) 0.72447(19) 0.0503(13) Uani 1 1 d . . . H46 H 0.7665 0.5275 0.7544 0.060 Uiso 1 1 calc R . . C47 C 0.9202(4) 0.4676(3) 0.72706(16) 0.0407(11) Uani 1 1 d . . . C48 C 0.9929(5) 0.4611(3) 0.77205(17) 0.0557(13) Uani 1 1 d . . . H48 H 0.9650 0.4830 0.8029 0.067 Uiso 1 1 calc R . . C49 C 1.1041(5) 0.4230(3) 0.77084(18) 0.0600(15) Uani 1 1 d . . . H49 H 1.1529 0.4187 0.8008 0.072 Uiso 1 1 calc R . . C50 C 1.1452(4) 0.3901(3) 0.72421(17) 0.0454(12) Uani 1 1 d . . . H50 H 1.2211 0.3633 0.7240 0.055 Uiso 1 1 calc R . . C51 C 0.9691(3) 0.4347(2) 0.68168(15) 0.0298(9) Uani 1 1 d . . . C52 C 0.9014(3) 0.4414(2) 0.63369(14) 0.0257(9) Uani 1 1 d . . . O1 O 1.2942(2) 0.31342(14) 0.62969(10) 0.0306(6) Uani 1 1 d . . . O2 O 1.3722(3) 0.44492(15) 0.65074(10) 0.0362(7) Uani 1 1 d . . . O3 O 1.4760(2) 0.37345(17) 0.57879(9) 0.0380(7) Uani 1 1 d . . . O4 O 1.6464(2) 0.20149(17) 0.88854(13) 0.0509(9) Uani 1 1 d . . . O5 O 1.5264(2) 0.09964(15) 0.89772(11) 0.0386(7) Uani 1 1 d . . . O6 O 1.6189(3) 0.25781(18) 0.50629(14) 0.0584(9) Uani 1 1 d . . . O7 O 1.8418(2) 0.21772(14) 0.51759(10) 0.0270(6) Uani 1 1 d . . . O8 O 1.6853(2) 0.13357(14) 0.46899(9) 0.0281(6) Uani 1 1 d . . . O9 O 1.0412(3) 0.10863(16) 0.60986(11) 0.0452(8) Uani 1 1 d . . . O10 O 1.0280(3) 0.07353(15) 0.52700(10) 0.0389(7) Uani 1 1 d . . . N1 N 1.7248(3) 0.0816(2) 0.80110(13) 0.0331(8) Uani 1 1 d . . . N2 N 1.8656(3) 0.08407(17) 0.88832(12) 0.0270(7) Uani 1 1 d . . . N3 N 0.9546(3) 0.41003(18) 0.59070(12) 0.0259(7) Uani 1 1 d . . . N4 N 1.0803(3) 0.39580(19) 0.68042(12) 0.0318(8) Uani 1 1 d . . . O1W O 1.6891(2) 0.00167(15) 0.96080(10) 0.0354(7) Uani 1 1 d . . . O2W O 1.0023(2) 0.25338(14) 0.60665(10) 0.0343(6) 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 Zn1 0.0231(2) 0.0279(2) 0.0258(2) 0.0010(2) 0.00270(18) 0.0015(2) Zn2 0.01932(19) 0.0243(2) 0.0219(2) 0.00107(19) 0.00013(17) 0.00147(19) Zn3 0.0300(2) 0.0241(2) 0.0300(2) -0.0001(2) -0.0007(2) -0.0013(2) P1 0.0262(5) 0.0254(5) 0.0204(5) -0.0007(4) 0.0002(4) 0.0019(4) P2 0.0146(4) 0.0289(5) 0.0270(5) -0.0022(5) 0.0003(4) 0.0015(4) C1 0.028(2) 0.037(2) 0.032(2) -0.0013(19) -0.0040(17) 0.005(2) C2 0.0245(19) 0.032(2) 0.034(2) -0.0001(18) -0.0095(17) 0.0016(19) C3 0.050(2) 0.025(2) 0.036(2) 0.0053(19) -0.009(2) -0.002(2) C4 0.044(2) 0.023(2) 0.033(2) -0.0043(18) -0.0077(19) 0.0043(19) C5 0.0230(18) 0.027(2) 0.030(2) 0.0010(18) -0.0038(16) 0.0022(18) C6 0.043(2) 0.020(2) 0.042(3) 0.0043(19) -0.003(2) -0.003(2) C7 0.044(2) 0.023(2) 0.034(2) -0.0027(19) -0.0057(19) 0.001(2) C8 0.0231(18) 0.023(2) 0.035(2) -0.0013(18) -0.0039(17) -0.0010(17) C9 0.034(2) 0.029(2) 0.039(2) 0.000(2) -0.0044(19) 0.001(2) C10 0.037(2) 0.045(3) 0.041(3) -0.010(2) -0.002(2) 0.010(2) C11 0.046(2) 0.051(3) 0.032(2) -0.002(2) 0.004(2) 0.003(2) C12 0.041(2) 0.039(2) 0.029(2) 0.0045(19) -0.0056(19) 0.010(2) C13 0.0277(19) 0.023(2) 0.032(2) -0.0023(18) -0.0060(17) 0.0010(18) C14 0.033(2) 0.028(2) 0.024(2) 0.0081(18) -0.0072(17) 0.0018(18) C15 0.031(2) 0.035(2) 0.035(2) -0.001(2) -0.0010(19) 0.003(2) C16 0.042(2) 0.050(3) 0.040(3) -0.005(2) -0.011(2) -0.003(2) C17 0.030(2) 0.039(3) 0.062(3) -0.007(3) -0.004(2) -0.006(2) C18 0.029(2) 0.027(2) 0.048(3) 0.002(2) 0.0029(19) 0.0023(19) C19 0.040(2) 0.054(3) 0.067(3) 0.015(3) 0.008(2) -0.014(2) C20 0.052(3) 0.068(4) 0.058(3) 0.027(3) 0.012(3) -0.010(3) C21 0.044(2) 0.053(3) 0.043(3) 0.016(2) 0.008(2) -0.005(2) C22 0.061(3) 0.088(4) 0.039(3) 0.029(3) 0.001(2) -0.008(3) C23 0.062(3) 0.082(4) 0.034(3) 0.013(3) -0.009(2) -0.009(3) C24 0.042(2) 0.056(3) 0.040(3) 0.005(2) -0.008(2) -0.005(2) C25 0.034(2) 0.027(2) 0.032(2) 0.0037(18) 0.0043(18) -0.0032(19) C26 0.030(2) 0.023(2) 0.036(2) 0.0007(19) 0.0013(18) 0.0001(18) C27 0.040(2) 0.065(3) 0.023(2) 0.000(2) -0.0007(18) -0.023(2) C28 0.034(2) 0.042(3) 0.024(2) 0.0016(19) 0.0001(17) -0.012(2) C29 0.0246(19) 0.052(3) 0.031(2) 0.009(2) 0.0040(17) 0.003(2) C30 0.035(2) 0.033(2) 0.032(2) 0.0041(19) 0.0010(18) 0.0019(19) C31 0.0257(18) 0.027(2) 0.028(2) 0.0041(18) 0.0005(17) 0.0008(17) C32 0.0286(19) 0.037(2) 0.042(2) -0.003(2) 0.0042(19) -0.002(2) C33 0.045(2) 0.035(2) 0.041(3) -0.007(2) 0.005(2) -0.012(2) C34 0.0259(18) 0.027(2) 0.025(2) 0.0041(18) -0.0006(16) 0.0008(17) C35 0.030(2) 0.033(2) 0.045(3) 0.007(2) -0.0046(19) 0.0036(19) C36 0.045(2) 0.020(2) 0.050(3) 0.010(2) 0.001(2) 0.001(2) C37 0.034(2) 0.024(2) 0.050(3) 0.005(2) -0.001(2) -0.0054(18) C38 0.0240(18) 0.033(2) 0.039(2) 0.0046(19) -0.0056(19) 0.000(2) C39 0.0301(19) 0.0202(19) 0.0194(19) 0.0030(16) 0.0027(15) -0.0010(17) C40 0.0222(18) 0.027(2) 0.031(2) 0.0080(19) -0.0003(17) -0.0012(17) C41 0.030(2) 0.044(3) 0.034(2) -0.003(2) 0.0034(19) 0.000(2) C42 0.033(2) 0.053(3) 0.042(3) -0.001(2) -0.010(2) 0.000(2) C43 0.024(2) 0.045(3) 0.055(3) 0.005(2) 0.001(2) 0.003(2) C44 0.0251(19) 0.028(2) 0.046(3) 0.001(2) 0.0057(18) -0.0001(18) C45 0.035(2) 0.042(3) 0.058(3) -0.005(2) 0.017(2) 0.009(2) C46 0.050(3) 0.056(3) 0.044(3) -0.011(3) 0.020(2) 0.008(3) C47 0.045(2) 0.047(3) 0.030(2) -0.003(2) 0.0088(19) -0.003(2) C48 0.061(3) 0.075(4) 0.032(2) -0.013(3) 0.013(2) 0.000(3) C49 0.055(3) 0.099(4) 0.026(3) 0.001(3) -0.001(2) 0.000(3) C50 0.037(2) 0.065(3) 0.035(3) 0.009(2) -0.003(2) 0.001(2) C51 0.029(2) 0.026(2) 0.034(2) 0.0006(18) 0.0062(18) -0.0017(18) C52 0.0245(18) 0.024(2) 0.029(2) 0.0010(17) 0.0068(16) -0.0029(16) O1 0.0243(12) 0.0300(15) 0.0375(16) 0.0014(13) -0.0007(12) 0.0018(12) O2 0.0580(17) 0.0238(15) 0.0268(15) 0.0025(12) 0.0019(13) 0.0040(14) O3 0.0366(15) 0.0571(19) 0.0202(14) -0.0078(13) 0.0055(12) -0.0067(15) O4 0.0312(15) 0.0384(17) 0.083(2) -0.0075(18) 0.0085(16) -0.0031(14) O5 0.0356(15) 0.0246(15) 0.0554(18) 0.0022(14) 0.0094(14) 0.0004(13) O6 0.0352(15) 0.0516(19) 0.088(3) -0.0147(19) -0.0085(17) 0.0234(16) O7 0.0193(11) 0.0304(14) 0.0314(14) -0.0045(12) 0.0022(11) -0.0008(11) O8 0.0294(13) 0.0301(15) 0.0247(14) 0.0023(12) -0.0042(11) -0.0028(13) O9 0.068(2) 0.0285(16) 0.0393(18) -0.0035(15) -0.0067(15) 0.0108(15) O10 0.0523(17) 0.0315(16) 0.0329(16) 0.0119(13) 0.0036(13) 0.0124(14) N1 0.0354(18) 0.032(2) 0.031(2) 0.0024(16) -0.0028(15) -0.0036(16) N2 0.0319(16) 0.0191(16) 0.0299(19) -0.0027(14) 0.0019(15) 0.0018(14) N3 0.0242(15) 0.0268(17) 0.0268(18) 0.0010(14) 0.0028(14) -0.0004(14) N4 0.0287(17) 0.039(2) 0.0274(18) 0.0023(16) 0.0014(14) -0.0012(16) O1W 0.0460(15) 0.0325(16) 0.0276(15) -0.0003(12) -0.0023(13) -0.0043(14) O2W 0.0352(13) 0.0266(14) 0.0410(16) 0.0012(13) 0.0058(14) -0.0044(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Zn1 O1 1.976(2) . ? Zn1 O8 2.042(2) 3_456 ? Zn1 O2W 2.053(2) . ? Zn1 N3 2.167(3) . ? Zn1 N4 2.191(3) . ? Zn2 O6 1.872(3) . ? Zn2 O3 1.889(2) . ? Zn2 O7 1.932(2) 3_456 ? Zn2 O10 1.993(3) 3_556 ? Zn3 O2 1.942(3) 4_846 ? Zn3 O5 1.963(3) . ? Zn3 N2 2.119(3) . ? Zn3 N1 2.163(3) . ? Zn3 O1W 2.231(3) . ? P1 O3 1.513(3) . ? P1 O2 1.515(3) . ? P1 O1 1.517(3) . ? P1 C1 1.816(4) . ? P2 O6 1.485(3) . ? P2 O7 1.519(2) . ? P2 O8 1.525(3) . ? P2 C27 1.814(4) . ? C1 C2 1.506(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.375(5) . ? C2 C7 1.385(5) . ? C3 C4 1.390(5) . ? C3 H3 0.9300 . ? C4 C5 1.393(5) . ? C4 H4 0.9300 . ? C5 C6 1.391(5) . ? C5 C8 1.486(5) . ? C6 C7 1.381(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.391(5) . ? C8 C13 1.402(5) . ? C9 C10 1.380(5) . ? C9 H9 0.9300 . ? C10 C11 1.372(6) . ? C10 H10 0.9300 . ? C11 C12 1.379(6) . ? C11 H11 0.9300 . ? C12 C13 1.394(5) . ? C12 H12 0.9300 . ? C13 C14 1.499(5) . ? C14 O4 1.221(4) . ? C14 O5 1.278(5) . ? C15 N2 1.316(5) . ? C15 C16 1.386(5) . ? C15 H15 0.9300 . ? C16 C17 1.354(6) . ? C16 H16 0.9300 . ? C17 C18 1.398(5) . ? C17 H17 0.9300 . ? C18 C26 1.396(5) . ? C18 C19 1.434(6) . ? C19 C20 1.346(7) . ? C19 H19 0.9300 . ? C20 C21 1.425(6) . ? C20 H20 0.9300 . ? C21 C22 1.396(6) . ? C21 C25 1.399(5) . ? C22 C23 1.352(7) . ? C22 H22 0.9300 . ? C23 C24 1.388(6) . ? C23 H23 0.9300 . ? C24 N1 1.316(5) . ? C24 H24 0.9300 . ? C25 N1 1.357(5) . ? C25 C26 1.431(5) . ? C26 N2 1.366(5) . ? C27 C28 1.509(5) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C33 1.375(5) . ? C28 C29 1.391(6) . ? C29 C30 1.375(5) . ? C29 H29 0.9300 . ? C30 C31 1.401(5) . ? C30 H30 0.9300 . ? C31 C32 1.390(5) . ? C31 C34 1.487(5) . ? C32 C33 1.391(5) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.394(5) . ? C34 C39 1.415(5) . ? C35 C36 1.381(5) . ? C35 H35 0.9300 . ? C36 C37 1.375(5) . ? C36 H36 0.9300 . ? C37 C38 1.367(5) . ? C37 H37 0.9300 . ? C38 C39 1.384(5) . ? C38 H38 0.9300 . ? C39 C40 1.499(5) . ? C40 O9 1.233(4) . ? C40 O10 1.267(4) . ? C41 N3 1.319(5) . ? C41 C42 1.389(5) . ? C41 H41 0.9300 . ? C42 C43 1.360(6) . ? C42 H42 0.9300 . ? C43 C44 1.401(6) . ? C43 H43 0.9300 . ? C44 C52 1.400(5) . ? C44 C45 1.443(6) . ? C45 C46 1.325(6) . ? C45 H45 0.9300 . ? C46 C47 1.435(6) . ? C46 H46 0.9300 . ? C47 C48 1.393(6) . ? C47 C51 1.400(5) . ? C48 C49 1.352(7) . ? C48 H48 0.9300 . ? C49 C50 1.399(6) . ? C49 H49 0.9300 . ? C50 N4 1.321(5) . ? C50 H50 0.9300 . ? C51 N4 1.360(5) . ? C51 C52 1.430(5) . ? C52 N3 1.356(4) . ? O2 Zn3 1.942(3) 4_856 ? O7 Zn2 1.932(2) 3_556 ? O8 Zn1 2.042(2) 3_556 ? O10 Zn2 1.993(3) 3_456 ? 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 Zn1 O8 93.86(10) . 3_456 ? O1 Zn1 O2W 110.61(11) . . ? O8 Zn1 O2W 111.44(10) 3_456 . ? O1 Zn1 N3 162.12(11) . . ? O8 Zn1 N3 90.07(10) 3_456 . ? O2W Zn1 N3 83.95(11) . . ? O1 Zn1 N4 91.27(11) . . ? O8 Zn1 N4 144.26(12) 3_456 . ? O2W Zn1 N4 99.61(11) . . ? N3 Zn1 N4 75.64(11) . . ? O6 Zn2 O3 113.24(14) . . ? O6 Zn2 O7 105.18(12) . 3_456 ? O3 Zn2 O7 117.75(11) . 3_456 ? O6 Zn2 O10 113.16(14) . 3_556 ? O3 Zn2 O10 97.75(12) . 3_556 ? O7 Zn2 O10 109.93(11) 3_456 3_556 ? O2 Zn3 O5 108.65(12) 4_846 . ? O2 Zn3 N2 127.53(12) 4_846 . ? O5 Zn3 N2 123.81(11) . . ? O2 Zn3 N1 89.18(12) 4_846 . ? O5 Zn3 N1 104.47(12) . . ? N2 Zn3 N1 77.82(12) . . ? O2 Zn3 O1W 95.80(10) 4_846 . ? O5 Zn3 O1W 88.06(11) . . ? N2 Zn3 O1W 87.40(11) . . ? N1 Zn3 O1W 164.31(11) . . ? O3 P1 O2 110.55(16) . . ? O3 P1 O1 114.67(15) . . ? O2 P1 O1 111.66(15) . . ? O3 P1 C1 104.12(16) . . ? O2 P1 C1 107.51(18) . . ? O1 P1 C1 107.77(16) . . ? O6 P2 O7 110.94(17) . . ? O6 P2 O8 111.06(16) . . ? O7 P2 O8 113.37(14) . . ? O6 P2 C27 110.3(2) . . ? O7 P2 C27 103.04(16) . . ? O8 P2 C27 107.80(18) . . ? C2 C1 P1 117.4(3) . . ? C2 C1 H1A 108.0 . . ? P1 C1 H1A 108.0 . . ? C2 C1 H1B 108.0 . . ? P1 C1 H1B 108.0 . . ? H1A C1 H1B 107.2 . . ? C3 C2 C7 117.5(4) . . ? C3 C2 C1 121.1(4) . . ? C7 C2 C1 121.4(4) . . ? C2 C3 C4 121.9(4) . . ? C2 C3 H3 119.0 . . ? C4 C3 H3 119.0 . . ? C3 C4 C5 120.5(4) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 117.3(4) . . ? C6 C5 C8 121.5(3) . . ? C4 C5 C8 121.2(4) . . ? C7 C6 C5 121.4(4) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C2 121.3(4) . . ? C6 C7 H7 119.4 . . ? C2 C7 H7 119.4 . . ? C9 C8 C13 118.3(4) . . ? C9 C8 C5 120.0(3) . . ? C13 C8 C5 121.6(3) . . ? C10 C9 C8 121.7(4) . . ? C10 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? C11 C10 C9 120.1(4) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 119.1(4) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C11 C12 C13 121.9(4) . . ? C11 C12 H12 119.1 . . ? C13 C12 H12 119.1 . . ? C12 C13 C8 118.9(4) . . ? C12 C13 C14 118.4(3) . . ? C8 C13 C14 122.4(3) . . ? O4 C14 O5 123.7(4) . . ? O4 C14 C13 119.3(3) . . ? O5 C14 C13 117.0(3) . . ? N2 C15 C16 123.1(4) . . ? N2 C15 H15 118.5 . . ? C16 C15 H15 118.5 . . ? C17 C16 C15 119.7(4) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 119.6(4) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C26 C18 C17 117.3(4) . . ? C26 C18 C19 119.0(4) . . ? C17 C18 C19 123.7(4) . . ? C20 C19 C18 121.1(4) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 121.3(4) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C22 C21 C25 117.2(4) . . ? C22 C21 C20 124.2(4) . . ? C25 C21 C20 118.6(4) . . ? C23 C22 C21 119.8(4) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 119.7(4) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? N1 C24 C23 122.4(4) . . ? N1 C24 H24 118.8 . . ? C23 C24 H24 118.8 . . ? N1 C25 C21 122.3(4) . . ? N1 C25 C26 117.2(3) . . ? C21 C25 C26 120.4(3) . . ? N2 C26 C18 122.6(4) . . ? N2 C26 C25 117.9(3) . . ? C18 C26 C25 119.5(4) . . ? C28 C27 P2 117.6(3) . . ? C28 C27 H27A 107.9 . . ? P2 C27 H27A 107.9 . . ? C28 C27 H27B 107.9 . . ? P2 C27 H27B 107.9 . . ? H27A C27 H27B 107.2 . . ? C33 C28 C29 117.3(4) . . ? C33 C28 C27 122.8(4) . . ? C29 C28 C27 119.9(4) . . ? C30 C29 C28 121.5(4) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C29 C30 C31 121.7(4) . . ? C29 C30 H30 119.2 . . ? C31 C30 H30 119.2 . . ? C32 C31 C30 116.4(3) . . ? C32 C31 C34 124.3(3) . . ? C30 C31 C34 119.3(3) . . ? C31 C32 C33 121.5(4) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? C28 C33 C32 121.6(4) . . ? C28 C33 H33 119.2 . . ? C32 C33 H33 119.2 . . ? C35 C34 C39 116.9(3) . . ? C35 C34 C31 118.6(3) . . ? C39 C34 C31 124.5(3) . . ? C36 C35 C34 122.8(3) . . ? C36 C35 H35 118.6 . . ? C34 C35 H35 118.6 . . ? C37 C36 C35 119.3(4) . . ? C37 C36 H36 120.4 . . ? C35 C36 H36 120.3 . . ? C38 C37 C36 119.3(4) . . ? C38 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? C37 C38 C39 122.5(4) . . ? C37 C38 H38 118.8 . . ? C39 C38 H38 118.8 . . ? C38 C39 C34 119.2(3) . . ? C38 C39 C40 116.1(3) . . ? C34 C39 C40 124.7(3) . . ? O9 C40 O10 125.3(4) . . ? O9 C40 C39 118.2(3) . . ? O10 C40 C39 116.3(3) . . ? N3 C41 C42 123.0(4) . . ? N3 C41 H41 118.5 . . ? C42 C41 H41 118.5 . . ? C43 C42 C41 119.9(4) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C42 C43 C44 118.8(4) . . ? C42 C43 H43 120.6 . . ? C44 C43 H43 120.6 . . ? C52 C44 C43 117.9(4) . . ? C52 C44 C45 118.3(4) . . ? C43 C44 C45 123.8(4) . . ? C46 C45 C44 121.6(4) . . ? C46 C45 H45 119.2 . . ? C44 C45 H45 119.2 . . ? C45 C46 C47 121.5(4) . . ? C45 C46 H46 119.3 . . ? C47 C46 H46 119.3 . . ? C48 C47 C51 117.0(4) . . ? C48 C47 C46 124.4(4) . . ? C51 C47 C46 118.6(4) . . ? C49 C48 C47 120.1(4) . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C48 C49 C50 119.6(4) . . ? C48 C49 H49 120.2 . . ? C50 C49 H49 120.2 . . ? N4 C50 C49 122.5(4) . . ? N4 C50 H50 118.8 . . ? C49 C50 H50 118.8 . . ? N4 C51 C47 123.1(4) . . ? N4 C51 C52 116.9(3) . . ? C47 C51 C52 120.0(3) . . ? N3 C52 C44 122.5(3) . . ? N3 C52 C51 117.5(3) . . ? C44 C52 C51 120.0(3) . . ? P1 O1 Zn1 123.21(15) . . ? P1 O2 Zn3 136.74(16) . 4_856 ? P1 O3 Zn2 143.67(18) . . ? C14 O5 Zn3 112.6(2) . . ? P2 O6 Zn2 166.6(3) . . ? P2 O7 Zn2 127.11(16) . 3_556 ? P2 O8 Zn1 126.61(15) . 3_556 ? C40 O10 Zn2 131.2(3) . 3_456 ? C24 N1 C25 118.5(3) . . ? C24 N1 Zn3 128.5(3) . . ? C25 N1 Zn3 112.9(2) . . ? C15 N2 C26 117.7(3) . . ? C15 N2 Zn3 128.1(3) . . ? C26 N2 Zn3 113.7(2) . . ? C41 N3 C52 117.9(3) . . ? C41 N3 Zn1 126.5(3) . . ? C52 N3 Zn1 115.0(2) . . ? C50 N4 C51 117.8(3) . . ? C50 N4 Zn1 127.7(3) . . ? C51 N4 Zn1 114.4(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 O3 P1 C1 C2 177.9(3) . . . . ? O2 P1 C1 C2 60.6(3) . . . . ? O1 P1 C1 C2 -59.9(3) . . . . ? P1 C1 C2 C3 -80.3(4) . . . . ? P1 C1 C2 C7 100.0(4) . . . . ? C7 C2 C3 C4 0.7(6) . . . . ? C1 C2 C3 C4 -179.0(4) . . . . ? C2 C3 C4 C5 2.6(6) . . . . ? C3 C4 C5 C6 -3.3(6) . . . . ? C3 C4 C5 C8 178.2(3) . . . . ? C4 C5 C6 C7 0.9(6) . . . . ? C8 C5 C6 C7 179.4(3) . . . . ? C5 C6 C7 C2 2.4(6) . . . . ? C3 C2 C7 C6 -3.1(6) . . . . ? C1 C2 C7 C6 176.5(3) . . . . ? C6 C5 C8 C9 -131.1(4) . . . . ? C4 C5 C8 C9 47.3(5) . . . . ? C6 C5 C8 C13 44.5(5) . . . . ? C4 C5 C8 C13 -137.1(4) . . . . ? C13 C8 C9 C10 -0.7(5) . . . . ? C5 C8 C9 C10 175.1(4) . . . . ? C8 C9 C10 C11 -1.7(6) . . . . ? C9 C10 C11 C12 2.2(6) . . . . ? C10 C11 C12 C13 -0.3(6) . . . . ? C11 C12 C13 C8 -2.1(6) . . . . ? C11 C12 C13 C14 171.4(4) . . . . ? C9 C8 C13 C12 2.6(5) . . . . ? C5 C8 C13 C12 -173.2(3) . . . . ? C9 C8 C13 C14 -170.8(3) . . . . ? C5 C8 C13 C14 13.5(5) . . . . ? C12 C13 C14 O4 -117.2(4) . . . . ? C8 C13 C14 O4 56.1(5) . . . . ? C12 C13 C14 O5 61.1(5) . . . . ? C8 C13 C14 O5 -125.6(4) . . . . ? N2 C15 C16 C17 0.9(6) . . . . ? C15 C16 C17 C18 -0.4(7) . . . . ? C16 C17 C18 C26 0.6(6) . . . . ? C16 C17 C18 C19 179.9(4) . . . . ? C26 C18 C19 C20 -1.1(7) . . . . ? C17 C18 C19 C20 179.7(5) . . . . ? C18 C19 C20 C21 0.7(8) . . . . ? C19 C20 C21 C22 -178.9(5) . . . . ? C19 C20 C21 C25 1.1(8) . . . . ? C25 C21 C22 C23 0.7(8) . . . . ? C20 C21 C22 C23 -179.3(5) . . . . ? C21 C22 C23 C24 0.6(8) . . . . ? C22 C23 C24 N1 -1.0(8) . . . . ? C22 C21 C25 N1 -1.7(7) . . . . ? C20 C21 C25 N1 178.2(4) . . . . ? C22 C21 C25 C26 177.5(4) . . . . ? C20 C21 C25 C26 -2.5(6) . . . . ? C17 C18 C26 N2 -1.3(6) . . . . ? C19 C18 C26 N2 179.5(4) . . . . ? C17 C18 C26 C25 178.9(4) . . . . ? C19 C18 C26 C25 -0.3(6) . . . . ? N1 C25 C26 N2 1.6(5) . . . . ? C21 C25 C26 N2 -177.7(4) . . . . ? N1 C25 C26 C18 -178.6(4) . . . . ? C21 C25 C26 C18 2.1(6) . . . . ? O6 P2 C27 C28 71.3(4) . . . . ? O7 P2 C27 C28 -170.3(3) . . . . ? O8 P2 C27 C28 -50.1(4) . . . . ? P2 C27 C28 C33 -90.8(5) . . . . ? P2 C27 C28 C29 91.0(4) . . . . ? C33 C28 C29 C30 -0.1(6) . . . . ? C27 C28 C29 C30 178.2(4) . . . . ? C28 C29 C30 C31 -1.7(6) . . . . ? C29 C30 C31 C32 1.7(6) . . . . ? C29 C30 C31 C34 -177.9(3) . . . . ? C30 C31 C32 C33 -0.1(6) . . . . ? C34 C31 C32 C33 179.5(4) . . . . ? C29 C28 C33 C32 1.7(6) . . . . ? C27 C28 C33 C32 -176.5(4) . . . . ? C31 C32 C33 C28 -1.6(7) . . . . ? C32 C31 C34 C35 -142.5(4) . . . . ? C30 C31 C34 C35 37.2(5) . . . . ? C32 C31 C34 C39 40.0(6) . . . . ? C30 C31 C34 C39 -140.3(4) . . . . ? C39 C34 C35 C36 0.6(6) . . . . ? C31 C34 C35 C36 -177.1(4) . . . . ? C34 C35 C36 C37 1.8(6) . . . . ? C35 C36 C37 C38 -1.9(6) . . . . ? C36 C37 C38 C39 -0.4(6) . . . . ? C37 C38 C39 C34 2.8(6) . . . . ? C37 C38 C39 C40 -175.4(4) . . . . ? C35 C34 C39 C38 -2.9(5) . . . . ? C31 C34 C39 C38 174.7(3) . . . . ? C35 C34 C39 C40 175.2(4) . . . . ? C31 C34 C39 C40 -7.2(6) . . . . ? C38 C39 C40 O9 98.1(4) . . . . ? C34 C39 C40 O9 -80.0(5) . . . . ? C38 C39 C40 O10 -77.5(4) . . . . ? C34 C39 C40 O10 104.3(4) . . . . ? N3 C41 C42 C43 -0.6(7) . . . . ? C41 C42 C43 C44 -0.3(7) . . . . ? C42 C43 C44 C52 0.7(6) . . . . ? C42 C43 C44 C45 -179.9(4) . . . . ? C52 C44 C45 C46 0.5(6) . . . . ? C43 C44 C45 C46 -178.8(5) . . . . ? C44 C45 C46 C47 -1.2(7) . . . . ? C45 C46 C47 C48 180.0(5) . . . . ? C45 C46 C47 C51 -0.1(7) . . . . ? C51 C47 C48 C49 -1.3(7) . . . . ? C46 C47 C48 C49 178.7(5) . . . . ? C47 C48 C49 C50 -0.1(8) . . . . ? C48 C49 C50 N4 1.2(8) . . . . ? C48 C47 C51 N4 1.8(6) . . . . ? C46 C47 C51 N4 -178.1(4) . . . . ? C48 C47 C51 C52 -178.0(4) . . . . ? C46 C47 C51 C52 2.1(6) . . . . ? C43 C44 C52 N3 -0.3(5) . . . . ? C45 C44 C52 N3 -179.7(4) . . . . ? C43 C44 C52 C51 -179.1(4) . . . . ? C45 C44 C52 C51 1.5(5) . . . . ? N4 C51 C52 N3 -1.4(5) . . . . ? C47 C51 C52 N3 178.3(4) . . . . ? N4 C51 C52 C44 177.4(3) . . . . ? C47 C51 C52 C44 -2.8(6) . . . . ? O3 P1 O1 Zn1 -82.8(2) . . . . ? O2 P1 O1 Zn1 44.0(2) . . . . ? C1 P1 O1 Zn1 161.82(18) . . . . ? O8 Zn1 O1 P1 61.95(19) 3_456 . . . ? O2W Zn1 O1 P1 176.59(16) . . . . ? N3 Zn1 O1 P1 -40.3(5) . . . . ? N4 Zn1 O1 P1 -82.65(19) . . . . ? O3 P1 O2 Zn3 34.4(3) . . . 4_856 ? O1 P1 O2 Zn3 -94.6(3) . . . 4_856 ? C1 P1 O2 Zn3 147.4(2) . . . 4_856 ? O2 P1 O3 Zn2 -138.3(3) . . . . ? O1 P1 O3 Zn2 -11.0(4) . . . . ? C1 P1 O3 Zn2 106.5(3) . . . . ? O6 Zn2 O3 P1 -94.4(3) . . . . ? O7 Zn2 O3 P1 28.8(4) 3_456 . . . ? O10 Zn2 O3 P1 146.2(3) 3_556 . . . ? O4 C14 O5 Zn3 4.5(5) . . . . ? C13 C14 O5 Zn3 -173.7(2) . . . . ? O2 Zn3 O5 C14 -157.3(3) 4_846 . . . ? N2 Zn3 O5 C14 21.7(3) . . . . ? N1 Zn3 O5 C14 -63.2(3) . . . . ? O1W Zn3 O5 C14 107.2(3) . . . . ? O7 P2 O6 Zn2 -127.3(9) . . . . ? O8 P2 O6 Zn2 105.6(10) . . . . ? C27 P2 O6 Zn2 -13.8(10) . . . . ? O3 Zn2 O6 P2 55.1(10) . . . . ? O7 Zn2 O6 P2 -74.8(10) 3_456 . . . ? O10 Zn2 O6 P2 165.2(9) 3_556 . . . ? O6 P2 O7 Zn2 -141.7(2) . . . 3_556 ? O8 P2 O7 Zn2 -15.9(2) . . . 3_556 ? C27 P2 O7 Zn2 100.3(2) . . . 3_556 ? O6 P2 O8 Zn1 29.1(2) . . . 3_556 ? O7 P2 O8 Zn1 -96.63(19) . . . 3_556 ? C27 P2 O8 Zn1 149.99(19) . . . 3_556 ? O9 C40 O10 Zn2 12.5(6) . . . 3_456 ? C39 C40 O10 Zn2 -172.2(2) . . . 3_456 ? C23 C24 N1 C25 0.0(7) . . . . ? C23 C24 N1 Zn3 178.1(4) . . . . ? C21 C25 N1 C24 1.4(6) . . . . ? C26 C25 N1 C24 -177.8(4) . . . . ? C21 C25 N1 Zn3 -177.0(3) . . . . ? C26 C25 N1 Zn3 3.7(4) . . . . ? O2 Zn3 N1 C24 47.7(4) 4_846 . . . ? O5 Zn3 N1 C24 -61.3(4) . . . . ? N2 Zn3 N1 C24 176.5(4) . . . . ? O1W Zn3 N1 C24 156.6(4) . . . . ? O2 Zn3 N1 C25 -134.0(3) 4_846 . . . ? O5 Zn3 N1 C25 116.9(3) . . . . ? N2 Zn3 N1 C25 -5.2(3) . . . . ? O1W Zn3 N1 C25 -25.2(6) . . . . ? C16 C15 N2 C26 -1.5(6) . . . . ? C16 C15 N2 Zn3 -172.5(3) . . . . ? C18 C26 N2 C15 1.7(5) . . . . ? C25 C26 N2 C15 -178.5(3) . . . . ? C18 C26 N2 Zn3 174.0(3) . . . . ? C25 C26 N2 Zn3 -6.2(4) . . . . ? O2 Zn3 N2 C15 -103.2(3) 4_846 . . . ? O5 Zn3 N2 C15 78.0(3) . . . . ? N1 Zn3 N2 C15 177.4(3) . . . . ? O1W Zn3 N2 C15 -7.9(3) . . . . ? O2 Zn3 N2 C26 85.4(3) 4_846 . . . ? O5 Zn3 N2 C26 -93.3(3) . . . . ? N1 Zn3 N2 C26 6.1(3) . . . . ? O1W Zn3 N2 C26 -179.2(3) . . . . ? C42 C41 N3 C52 1.0(6) . . . . ? C42 C41 N3 Zn1 171.7(3) . . . . ? C44 C52 N3 C41 -0.5(5) . . . . ? C51 C52 N3 C41 178.3(3) . . . . ? C44 C52 N3 Zn1 -172.3(3) . . . . ? C51 C52 N3 Zn1 6.5(4) . . . . ? O1 Zn1 N3 C41 138.6(4) . . . . ? O8 Zn1 N3 C41 35.7(3) 3_456 . . . ? O2W Zn1 N3 C41 -75.8(3) . . . . ? N4 Zn1 N3 C41 -177.4(3) . . . . ? O1 Zn1 N3 C52 -50.5(5) . . . . ? O8 Zn1 N3 C52 -153.3(3) 3_456 . . . ? O2W Zn1 N3 C52 95.1(3) . . . . ? N4 Zn1 N3 C52 -6.5(2) . . . . ? C49 C50 N4 C51 -0.6(7) . . . . ? C49 C50 N4 Zn1 -177.0(4) . . . . ? C47 C51 N4 C50 -0.9(6) . . . . ? C52 C51 N4 C50 178.9(4) . . . . ? C47 C51 N4 Zn1 175.9(3) . . . . ? C52 C51 N4 Zn1 -4.3(4) . . . . ? O1 Zn1 N4 C50 -10.2(4) . . . . ? O8 Zn1 N4 C50 -108.6(4) 3_456 . . . ? O2W Zn1 N4 C50 101.0(4) . . . . ? N3 Zn1 N4 C50 -177.9(4) . . . . ? O1 Zn1 N4 C51 173.4(3) . . . . ? O8 Zn1 N4 C51 75.0(3) 3_456 . . . ? O2W Zn1 N4 C51 -75.5(3) . . . . ? N3 Zn1 N4 C51 5.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.376 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.062 #======================================== data_compound-5 _database_code_depnum_ccdc_archive 'CCDC 852765' #TrackingRef 'Crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H20 Cd3 O10 P2, 2(H2 O)' _chemical_formula_sum 'C28 H24 Cd3 O12 P2' _chemical_formula_weight 951.61 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' 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 10.151(5) _cell_length_b 9.687(5) _cell_length_c 29.778(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 2928(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5410 _cell_measurement_theta_min 2.9801 _cell_measurement_theta_max 29.0450 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 2.334 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.76641 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10260 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.35 _reflns_number_total 2679 _reflns_number_gt 2443 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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. H atoms of water molecule were refined isotropically with distance restraints of O---H = 0.85+-0.01 \%A and H...H = 1.44+-0.01 \%A. ; _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^)+(0.0201P)^2^+5.6456P] 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 2679 _refine_ls_number_parameters 202 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0585 _refine_ls_wR_factor_gt 0.0564 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 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 Cd1 Cd 0.5000 -0.5000 0.0000 0.01824(10) Uani 1 2 d S . . Cd2 Cd 0.37812(2) 0.10954(3) 0.025113(9) 0.01845(9) Uani 1 1 d . . . P1 P 0.79105(9) -0.30432(9) 0.02195(3) 0.01525(19) Uani 1 1 d . . . C1 C 0.7697(4) -0.3349(4) 0.08092(12) 0.0232(8) Uani 1 1 d . . . H1A H 0.7288 -0.4247 0.0846 0.028 Uiso 1 1 calc R . . H1B H 0.8563 -0.3397 0.0946 0.028 Uiso 1 1 calc R . . C2 C 0.6891(4) -0.2308(4) 0.10663(12) 0.0232(8) Uani 1 1 d . . . C3 C 0.7422(4) -0.1565(4) 0.14195(12) 0.0278(9) Uani 1 1 d . . . H3 H 0.8305 -0.1687 0.1493 0.033 Uiso 1 1 calc R . . C4 C 0.6667(4) -0.0643(4) 0.16664(13) 0.0291(9) Uani 1 1 d . . . H4 H 0.7056 -0.0144 0.1898 0.035 Uiso 1 1 calc R . . C5 C 0.5342(4) -0.0454(4) 0.15734(12) 0.0263(9) Uani 1 1 d . . . C6 C 0.4810(4) -0.1207(4) 0.12191(13) 0.0277(9) Uani 1 1 d . . . H6 H 0.3922 -0.1103 0.1150 0.033 Uiso 1 1 calc R . . C7 C 0.5562(4) -0.2098(4) 0.09685(13) 0.0262(9) Uani 1 1 d . . . H7 H 0.5179 -0.2570 0.0730 0.031 Uiso 1 1 calc R . . C8 C 0.4516(4) 0.0503(4) 0.18479(13) 0.0292(9) Uani 1 1 d . . . C9 C 0.4680(5) 0.0559(5) 0.23129(14) 0.0406(11) Uani 1 1 d . . . H9 H 0.5321 0.0013 0.2449 0.049 Uiso 1 1 calc R . . C10 C 0.3907(5) 0.1412(5) 0.25750(15) 0.0461(12) Uani 1 1 d . . . H10 H 0.4051 0.1459 0.2883 0.055 Uiso 1 1 calc R . . C11 C 0.2929(5) 0.2189(5) 0.23829(14) 0.0487(13) Uani 1 1 d . . . H11 H 0.2395 0.2743 0.2561 0.058 Uiso 1 1 calc R . . C12 C 0.2739(5) 0.2148(5) 0.19257(14) 0.0419(11) Uani 1 1 d . . . H12 H 0.2069 0.2669 0.1796 0.050 Uiso 1 1 calc R . . C13 C 0.3542(4) 0.1332(4) 0.16556(13) 0.0270(9) Uani 1 1 d . . . C14 C 0.3421(4) 0.1411(4) 0.11554(13) 0.0252(9) Uani 1 1 d . . . O1 O 0.6571(2) -0.3316(2) -0.00050(8) 0.0204(5) Uani 1 1 d . . . O2 O 0.8992(2) -0.4040(2) 0.00585(8) 0.0200(5) Uani 1 1 d . . . O3 O 0.8273(2) -0.1541(2) 0.01174(8) 0.0191(5) Uani 1 1 d . . . O4 O 0.4333(3) 0.1983(3) 0.09406(9) 0.0321(7) Uani 1 1 d . . . O5 O 0.2483(2) 0.0868(2) 0.09500(7) 0.0463(8) Uani 1 1 d . . . O1W O 0.5128(2) -0.4783(2) -0.07681(7) 0.0305(6) Uani 1 1 d RD . . H1 H 0.5799 -0.5251 -0.0846 0.046 Uiso 1 1 d RD . . H1' H 0.5166 -0.3929 -0.0831 0.046 Uiso 1 1 d RD . . 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 Cd1 0.01280(18) 0.01311(19) 0.0288(2) 0.00019(15) -0.00098(16) -0.00090(14) Cd2 0.01678(15) 0.01509(14) 0.02347(15) -0.00154(11) -0.00129(11) 0.00226(10) P1 0.0131(4) 0.0110(4) 0.0216(4) -0.0002(3) -0.0010(4) 0.0006(4) C1 0.0210(19) 0.025(2) 0.0239(19) 0.0034(15) -0.0011(16) 0.0036(16) C2 0.024(2) 0.022(2) 0.0232(18) 0.0059(15) 0.0036(17) 0.0007(16) C3 0.025(2) 0.034(2) 0.0243(19) 0.0045(17) -0.0001(17) 0.0000(18) C4 0.033(2) 0.033(2) 0.022(2) -0.0021(17) -0.0025(19) -0.0043(19) C5 0.032(2) 0.025(2) 0.0227(19) 0.0021(16) 0.0052(18) -0.0007(18) C6 0.021(2) 0.028(2) 0.034(2) 0.0002(17) 0.0009(18) -0.0024(17) C7 0.027(2) 0.027(2) 0.025(2) -0.0025(16) 0.0004(18) -0.0014(18) C8 0.035(2) 0.028(2) 0.024(2) -0.0030(16) 0.0056(19) -0.0009(19) C9 0.047(3) 0.046(3) 0.029(2) 0.0006(19) 0.002(2) 0.008(2) C10 0.055(3) 0.059(3) 0.024(2) -0.007(2) 0.005(2) 0.005(3) C11 0.053(3) 0.061(3) 0.032(2) -0.017(2) 0.008(2) 0.012(3) C12 0.044(3) 0.049(3) 0.033(2) -0.009(2) 0.003(2) 0.017(2) C13 0.025(2) 0.031(2) 0.025(2) -0.0040(17) 0.0038(18) -0.0018(18) C14 0.024(2) 0.022(2) 0.029(2) -0.0044(16) -0.0009(18) 0.0059(17) O1 0.0141(12) 0.0143(12) 0.0329(14) 0.0006(10) -0.0019(11) -0.0019(10) O2 0.0165(12) 0.0137(13) 0.0297(14) -0.0041(10) -0.0006(11) 0.0023(10) O3 0.0164(12) 0.0121(12) 0.0287(13) -0.0011(10) -0.0007(11) -0.0017(10) O4 0.0315(15) 0.0360(17) 0.0288(15) 0.0022(12) 0.0022(13) 0.0004(14) O5 0.0418(18) 0.059(2) 0.0376(17) 0.0008(15) -0.0124(16) -0.0164(17) O1W 0.0286(15) 0.0269(15) 0.0358(15) -0.0029(12) 0.0025(13) 0.0021(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Cd1 O1 2.282(2) . ? Cd1 O1 2.282(2) 5_645 ? Cd1 O1W 2.301(2) . ? Cd1 O1W 2.301(2) 5_645 ? Cd1 O3 2.329(2) 3_445 ? Cd1 O3 2.329(2) 7_755 ? Cd2 O2 2.205(2) 3_445 ? Cd2 O4 2.295(3) . ? Cd2 O1 2.300(3) 5_655 ? Cd2 O2 2.335(3) 7_765 ? Cd2 O3 2.396(3) 5_655 ? Cd2 O5 2.473(2) . ? Cd2 C14 2.735(4) . ? Cd2 P1 2.9110(12) 5_655 ? P1 O3 1.531(3) . ? P1 O1 1.538(3) . ? P1 O2 1.539(2) . ? P1 C1 1.794(4) . ? P1 Cd2 2.9110(12) 5_655 ? C1 C2 1.507(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.384(5) . ? C2 C7 1.396(5) . ? C3 C4 1.388(5) . ? C3 H3 0.9300 . ? C4 C5 1.384(6) . ? C4 H4 0.9300 . ? C5 C6 1.392(5) . ? C5 C8 1.493(6) . ? C6 C7 1.373(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.396(5) . ? C8 C13 1.397(6) . ? C9 C10 1.381(6) . ? C9 H9 0.9300 . ? C10 C11 1.371(7) . ? C10 H10 0.9300 . ? C11 C12 1.376(6) . ? C11 H11 0.9300 . ? C12 C13 1.392(6) . ? C12 H12 0.9300 . ? C13 C14 1.496(5) . ? C14 O5 1.249(4) . ? C14 O4 1.254(5) . ? O1 Cd2 2.300(3) 5_655 ? O2 Cd2 2.205(2) 3_545 ? O2 Cd2 2.335(3) 7_755 ? O3 Cd1 2.329(2) 3_545 ? O3 Cd2 2.396(3) 5_655 ? O1W H1 0.8502 . ? O1W H1' 0.8493 . ? 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 Cd1 O1 180.0 . 5_645 ? O1 Cd1 O1W 83.60(8) . . ? O1 Cd1 O1W 96.40(8) 5_645 . ? O1 Cd1 O1W 96.40(8) . 5_645 ? O1 Cd1 O1W 83.60(8) 5_645 5_645 ? O1W Cd1 O1W 180.00(10) . 5_645 ? O1 Cd1 O3 93.83(9) . 3_445 ? O1 Cd1 O3 86.17(9) 5_645 3_445 ? O1W Cd1 O3 80.48(8) . 3_445 ? O1W Cd1 O3 99.52(8) 5_645 3_445 ? O1 Cd1 O3 86.17(9) . 7_755 ? O1 Cd1 O3 93.83(9) 5_645 7_755 ? O1W Cd1 O3 99.52(8) . 7_755 ? O1W Cd1 O3 80.48(8) 5_645 7_755 ? O3 Cd1 O3 180.0 3_445 7_755 ? O2 Cd2 O4 133.53(9) 3_445 . ? O2 Cd2 O1 136.58(9) 3_445 5_655 ? O4 Cd2 O1 88.42(9) . 5_655 ? O2 Cd2 O2 75.68(9) 3_445 7_765 ? O4 Cd2 O2 90.26(9) . 7_765 ? O1 Cd2 O2 97.16(8) 5_655 7_765 ? O2 Cd2 O3 93.20(8) 3_445 5_655 ? O4 Cd2 O3 123.68(9) . 5_655 ? O1 Cd2 O3 63.26(8) 5_655 5_655 ? O2 Cd2 O3 137.73(9) 7_765 5_655 ? O2 Cd2 O5 108.85(8) 3_445 . ? O4 Cd2 O5 53.90(9) . . ? O1 Cd2 O5 105.58(8) 5_655 . ? O2 Cd2 O5 135.84(8) 7_765 . ? O3 Cd2 O5 86.43(8) 5_655 . ? O2 Cd2 C14 121.72(10) 3_445 . ? O4 Cd2 C14 27.11(10) . . ? O1 Cd2 C14 100.86(10) 5_655 . ? O2 Cd2 C14 112.17(10) 7_765 . ? O3 Cd2 C14 108.34(10) 5_655 . ? O5 Cd2 C14 27.15(9) . . ? O2 Cd2 P1 116.19(7) 3_445 5_655 ? O4 Cd2 P1 109.37(7) . 5_655 ? O1 Cd2 P1 31.65(6) 5_655 5_655 ? O2 Cd2 P1 119.27(7) 7_765 5_655 ? O3 Cd2 P1 31.69(6) 5_655 5_655 ? O5 Cd2 P1 98.54(6) . 5_655 ? C14 Cd2 P1 108.83(8) . 5_655 ? O3 P1 O1 106.82(13) . . ? O3 P1 O2 111.26(14) . . ? O1 P1 O2 112.81(14) . . ? O3 P1 C1 112.35(16) . . ? O1 P1 C1 106.88(16) . . ? O2 P1 C1 106.72(15) . . ? O3 P1 Cd2 55.27(10) . 5_655 ? O1 P1 Cd2 51.72(9) . 5_655 ? O2 P1 Cd2 132.66(11) . 5_655 ? C1 P1 Cd2 120.46(12) . 5_655 ? C2 C1 P1 116.9(3) . . ? C2 C1 H1A 108.1 . . ? P1 C1 H1A 108.1 . . ? C2 C1 H1B 108.1 . . ? P1 C1 H1B 108.1 . . ? H1A C1 H1B 107.3 . . ? C3 C2 C7 117.4(4) . . ? C3 C2 C1 121.5(3) . . ? C7 C2 C1 121.1(3) . . ? C4 C3 C2 121.5(4) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 121.0(4) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 117.3(4) . . ? C4 C5 C8 121.2(4) . . ? C6 C5 C8 121.5(4) . . ? C7 C6 C5 121.7(4) . . ? C7 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C6 C7 C2 121.0(4) . . ? C6 C7 H7 119.5 . . ? C2 C7 H7 119.5 . . ? C9 C8 C13 117.9(4) . . ? C9 C8 C5 120.0(4) . . ? C13 C8 C5 122.0(3) . . ? C10 C9 C8 121.1(4) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C11 C10 C9 120.3(4) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 119.9(4) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C13 120.4(4) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C8 120.3(4) . . ? C12 C13 C14 119.9(4) . . ? C8 C13 C14 119.7(3) . . ? O5 C14 O4 120.0(3) . . ? O5 C14 C13 121.9(4) . . ? O4 C14 C13 118.0(3) . . ? O5 C14 Cd2 64.67(19) . . ? O4 C14 Cd2 56.54(19) . . ? C13 C14 Cd2 164.5(3) . . ? P1 O1 Cd1 137.56(14) . . ? P1 O1 Cd2 96.63(11) . 5_655 ? Cd1 O1 Cd2 124.19(11) . 5_655 ? P1 O2 Cd2 128.87(14) . 3_545 ? P1 O2 Cd2 125.38(13) . 7_755 ? Cd2 O2 Cd2 104.32(9) 3_545 7_755 ? P1 O3 Cd1 145.07(14) . 3_545 ? P1 O3 Cd2 93.04(11) . 5_655 ? Cd1 O3 Cd2 118.09(10) 3_545 5_655 ? C14 O4 Cd2 96.4(2) . . ? C14 O5 Cd2 88.2(2) . . ? Cd1 O1W H1 105.5 . . ? Cd1 O1W H1' 108.2 . . ? H1 O1W H1' 115.0 . . ? 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 O3 P1 C1 C2 45.7(3) . . . . ? O1 P1 C1 C2 -71.2(3) . . . . ? O2 P1 C1 C2 167.9(3) . . . . ? Cd2 P1 C1 C2 -16.1(3) 5_655 . . . ? P1 C1 C2 C3 -119.5(3) . . . . ? P1 C1 C2 C7 63.2(4) . . . . ? C7 C2 C3 C4 -0.3(5) . . . . ? C1 C2 C3 C4 -177.6(3) . . . . ? C2 C3 C4 C5 1.4(6) . . . . ? C3 C4 C5 C6 -1.0(6) . . . . ? C3 C4 C5 C8 178.0(4) . . . . ? C4 C5 C6 C7 -0.3(6) . . . . ? C8 C5 C6 C7 -179.3(4) . . . . ? C5 C6 C7 C2 1.4(6) . . . . ? C3 C2 C7 C6 -1.1(6) . . . . ? C1 C2 C7 C6 176.3(3) . . . . ? C4 C5 C8 C9 -39.9(6) . . . . ? C6 C5 C8 C9 139.0(4) . . . . ? C4 C5 C8 C13 141.9(4) . . . . ? C6 C5 C8 C13 -39.1(6) . . . . ? C13 C8 C9 C10 -0.2(7) . . . . ? C5 C8 C9 C10 -178.5(4) . . . . ? C8 C9 C10 C11 2.2(7) . . . . ? C9 C10 C11 C12 -1.7(8) . . . . ? C10 C11 C12 C13 -0.6(8) . . . . ? C11 C12 C13 C8 2.6(7) . . . . ? C11 C12 C13 C14 -173.4(4) . . . . ? C9 C8 C13 C12 -2.1(6) . . . . ? C5 C8 C13 C12 176.1(4) . . . . ? C9 C8 C13 C14 173.9(4) . . . . ? C5 C8 C13 C14 -7.9(6) . . . . ? C12 C13 C14 O5 -75.2(5) . . . . ? C8 C13 C14 O5 108.7(4) . . . . ? C12 C13 C14 O4 108.4(5) . . . . ? C8 C13 C14 O4 -67.6(5) . . . . ? C12 C13 C14 Cd2 173.8(8) . . . . ? C8 C13 C14 Cd2 -2.3(13) . . . . ? O2 Cd2 C14 O5 -68.1(2) 3_445 . . . ? O4 Cd2 C14 O5 167.2(4) . . . . ? O1 Cd2 C14 O5 103.02(19) 5_655 . . . ? O2 Cd2 C14 O5 -154.55(18) 7_765 . . . ? O3 Cd2 C14 O5 37.8(2) 5_655 . . . ? P1 Cd2 C14 O5 71.3(2) 5_655 . . . ? O2 Cd2 C14 O4 124.7(2) 3_445 . . . ? O1 Cd2 C14 O4 -64.2(2) 5_655 . . . ? O2 Cd2 C14 O4 38.3(2) 7_765 . . . ? O3 Cd2 C14 O4 -129.4(2) 5_655 . . . ? O5 Cd2 C14 O4 -167.2(4) . . . . ? P1 Cd2 C14 O4 -95.9(2) 5_655 . . . ? O2 Cd2 C14 C13 50.6(11) 3_445 . . . ? O4 Cd2 C14 C13 -74.1(10) . . . . ? O1 Cd2 C14 C13 -138.2(10) 5_655 . . . ? O2 Cd2 C14 C13 -35.8(11) 7_765 . . . ? O3 Cd2 C14 C13 156.5(10) 5_655 . . . ? O5 Cd2 C14 C13 118.7(11) . . . . ? P1 Cd2 C14 C13 -170.0(10) 5_655 . . . ? O3 P1 O1 Cd1 -169.51(19) . . . . ? O2 P1 O1 Cd1 67.9(2) . . . . ? C1 P1 O1 Cd1 -49.0(2) . . . . ? Cd2 P1 O1 Cd1 -164.9(3) 5_655 . . . ? O3 P1 O1 Cd2 -4.64(14) . . . 5_655 ? O2 P1 O1 Cd2 -127.20(13) . . . 5_655 ? C1 P1 O1 Cd2 115.81(14) . . . 5_655 ? O1 Cd1 O1 P1 49(100) 5_645 . . . ? O1W Cd1 O1 P1 -132.0(2) . . . . ? O1W Cd1 O1 P1 48.0(2) 5_645 . . . ? O3 Cd1 O1 P1 148.0(2) 3_445 . . . ? O3 Cd1 O1 P1 -32.0(2) 7_755 . . . ? O1 Cd1 O1 Cd2 -112(100) 5_645 . . 5_655 ? O1W Cd1 O1 Cd2 66.26(13) . . . 5_655 ? O1W Cd1 O1 Cd2 -113.74(13) 5_645 . . 5_655 ? O3 Cd1 O1 Cd2 -13.70(14) 3_445 . . 5_655 ? O3 Cd1 O1 Cd2 166.30(14) 7_755 . . 5_655 ? O3 P1 O2 Cd2 -141.89(17) . . . 3_545 ? O1 P1 O2 Cd2 -21.9(2) . . . 3_545 ? C1 P1 O2 Cd2 95.2(2) . . . 3_545 ? Cd2 P1 O2 Cd2 -80.1(2) 5_655 . . 3_545 ? O3 P1 O2 Cd2 54.0(2) . . . 7_755 ? O1 P1 O2 Cd2 174.00(14) . . . 7_755 ? C1 P1 O2 Cd2 -68.9(2) . . . 7_755 ? Cd2 P1 O2 Cd2 115.76(14) 5_655 . . 7_755 ? O1 P1 O3 Cd1 -149.6(2) . . . 3_545 ? O2 P1 O3 Cd1 -26.1(3) . . . 3_545 ? C1 P1 O3 Cd1 93.5(3) . . . 3_545 ? Cd2 P1 O3 Cd1 -154.1(3) 5_655 . . 3_545 ? O1 P1 O3 Cd2 4.43(14) . . . 5_655 ? O2 P1 O3 Cd2 127.95(12) . . . 5_655 ? C1 P1 O3 Cd2 -112.46(15) . . . 5_655 ? O5 C14 O4 Cd2 -13.4(4) . . . . ? C13 C14 O4 Cd2 163.0(3) . . . . ? O2 Cd2 O4 C14 -74.7(3) 3_445 . . . ? O1 Cd2 O4 C14 117.8(2) 5_655 . . . ? O2 Cd2 O4 C14 -145.0(2) 7_765 . . . ? O3 Cd2 O4 C14 61.8(2) 5_655 . . . ? O5 Cd2 O4 C14 7.2(2) . . . . ? P1 Cd2 O4 C14 93.7(2) 5_655 . . . ? O4 C14 O5 Cd2 12.3(3) . . . . ? C13 C14 O5 Cd2 -164.0(3) . . . . ? O2 Cd2 O5 C14 123.5(2) 3_445 . . . ? O4 Cd2 O5 C14 -7.2(2) . . . . ? O1 Cd2 O5 C14 -83.4(2) 5_655 . . . ? O2 Cd2 O5 C14 34.8(2) 7_765 . . . ? O3 Cd2 O5 C14 -144.4(2) 5_655 . . . ? P1 Cd2 O5 C14 -115.0(2) 5_655 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1 O5 0.85 1.84 2.667(2) 164.7 3_545 O1W H1' O4 0.85 1.98 2.814(4) 167.3 5_655 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.569 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.090 #======================================== data_compound-6 _database_code_depnum_ccdc_archive 'CCDC 852766' #TrackingRef 'Crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H11 Cd2 O6 P, 1.5(H2 O)' _chemical_formula_sum 'C14 H14 Cd2 O7.50 P' _chemical_formula_weight 558.02 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' 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_hall '-P 2ybc' 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 14.8874(7) _cell_length_b 10.9755(4) _cell_length_c 9.8754(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.096(4) _cell_angle_gamma 90.00 _cell_volume 1611.25(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2205 _cell_measurement_theta_min 3.1395 _cell_measurement_theta_max 29.1940 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1076 _exptl_absorpt_coefficient_mu 2.776 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.91997 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6005 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 25.03 _reflns_number_total 2827 _reflns_number_gt 2265 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0334P)^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 2827 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Cd1 Cd 0.58265(3) -0.08461(4) 0.81299(4) 0.02320(15) Uani 1 1 d . . . Cd2 Cd 0.50777(4) 0.34747(4) 1.04350(5) 0.03534(17) Uani 1 1 d . . . P1 P 0.40986(11) 0.11988(13) 0.83680(15) 0.0211(4) Uani 1 1 d . . . C1 C 0.2893(4) 0.1113(6) 0.8255(6) 0.0339(16) Uani 1 1 d . . . H1A H 0.2705 0.0603 0.8991 0.041 Uiso 1 1 calc R . . H1B H 0.2657 0.1924 0.8400 0.041 Uiso 1 1 calc R . . C2 C 0.2463(4) 0.0626(5) 0.6945(6) 0.0256(14) Uani 1 1 d . . . C3 C 0.2359(5) 0.1359(6) 0.5803(7) 0.0391(18) Uani 1 1 d . . . H3 H 0.2572 0.2155 0.5834 0.047 Uiso 1 1 calc R . . C4 C 0.1938(5) 0.0918(6) 0.4612(7) 0.0381(17) Uani 1 1 d . . . H4 H 0.1873 0.1431 0.3864 0.046 Uiso 1 1 calc R . . C5 C 0.1618(4) -0.0244(6) 0.4502(6) 0.0287(15) Uani 1 1 d . . . C6 C 0.1718(5) -0.0976(6) 0.5651(7) 0.0418(18) Uani 1 1 d . . . H6 H 0.1504 -0.1772 0.5621 0.050 Uiso 1 1 calc R . . C7 C 0.2133(5) -0.0533(6) 0.6837(7) 0.0396(17) Uani 1 1 d . . . H7 H 0.2190 -0.1044 0.7589 0.048 Uiso 1 1 calc R . . C8 C 0.1134(4) -0.0673(5) 0.3226(7) 0.0323(15) Uani 1 1 d . . . C9 C 0.1516(4) -0.0640(5) 0.1969(6) 0.0280(14) Uani 1 1 d . . . C10 C 0.1009(5) -0.0969(5) 0.0802(7) 0.0344(16) Uani 1 1 d . . . H10 H 0.1261 -0.0921 -0.0038 0.041 Uiso 1 1 calc R . . C11 C 0.0134(5) -0.1367(6) 0.0881(8) 0.0444(19) Uani 1 1 d . . . H11 H -0.0206 -0.1569 0.0094 0.053 Uiso 1 1 calc R . . C12 C -0.0233(5) -0.1466(7) 0.2114(9) 0.051(2) Uani 1 1 d . . . H12 H -0.0810 -0.1781 0.2172 0.061 Uiso 1 1 calc R . . C13 C 0.0253(5) -0.1095(7) 0.3280(8) 0.0470(19) Uani 1 1 d . . . H13 H -0.0013 -0.1128 0.4110 0.056 Uiso 1 1 calc R . . C14 C 0.2477(4) -0.0265(7) 0.1820(6) 0.0369(17) Uani 1 1 d . . . O1 O 0.4465(3) -0.0060(3) 0.8101(4) 0.0276(9) Uani 1 1 d . . . O2 O 0.4362(3) 0.1680(3) 0.9791(4) 0.0266(10) Uani 1 1 d . . . O3 O 0.4377(3) 0.2109(3) 0.7285(4) 0.0339(11) Uani 1 1 d . . . O4 O 0.2664(4) 0.0816(5) 0.1728(6) 0.0684(18) Uani 1 1 d . . . O5 O 0.3063(9) -0.0886(12) 0.1448(12) 0.040(3) Uani 0.50 1 d P . . O5' O 0.3053(8) -0.1174(11) 0.2236(16) 0.052(4) Uani 0.50 1 d P . . O6 O 0.4221(3) 0.4698(3) 0.9104(4) 0.0290(10) Uani 1 1 d . . . O1W O 0.6032(6) 0.3179(9) 0.8638(9) 0.045(3) Uani 0.50 1 d P . . O2W' O 0.6356(6) 0.2287(9) 1.1442(11) 0.044(3) Uani 0.50 1 d P . . O2W O 0.6349(7) 0.2693(11) 1.0308(13) 0.065(3) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0296(3) 0.0226(2) 0.0176(2) 0.00148(17) 0.00308(18) 0.00085(19) Cd2 0.0615(4) 0.0233(3) 0.0212(3) 0.00179(19) 0.0020(2) -0.0109(2) P1 0.0310(9) 0.0187(7) 0.0136(8) 0.0002(6) 0.0021(6) -0.0010(7) C1 0.035(4) 0.048(4) 0.019(3) -0.002(3) 0.002(3) 0.014(3) C2 0.019(3) 0.032(3) 0.026(3) -0.004(3) 0.000(3) -0.004(3) C3 0.060(5) 0.022(3) 0.033(4) 0.006(3) -0.012(3) -0.011(3) C4 0.048(4) 0.036(4) 0.029(4) 0.006(3) -0.008(3) -0.013(3) C5 0.022(3) 0.033(4) 0.030(4) -0.011(3) 0.004(3) -0.006(3) C6 0.043(4) 0.029(4) 0.052(5) 0.006(3) -0.008(4) -0.007(3) C7 0.046(4) 0.042(4) 0.030(4) 0.010(3) -0.003(3) -0.002(4) C8 0.033(4) 0.027(3) 0.036(4) -0.011(3) -0.001(3) 0.002(3) C9 0.027(3) 0.027(3) 0.030(4) -0.004(3) -0.002(3) 0.004(3) C10 0.037(4) 0.035(4) 0.031(4) -0.006(3) -0.005(3) 0.003(3) C11 0.037(4) 0.043(4) 0.051(5) -0.010(4) -0.014(4) 0.000(4) C12 0.028(4) 0.057(5) 0.067(6) -0.017(4) -0.003(4) -0.011(4) C13 0.035(4) 0.060(5) 0.047(5) -0.007(4) 0.010(4) -0.007(4) C14 0.028(4) 0.058(5) 0.024(4) -0.024(4) 0.001(3) 0.003(4) O1 0.031(2) 0.023(2) 0.029(2) -0.0034(18) 0.0021(18) -0.0001(19) O2 0.040(3) 0.026(2) 0.014(2) 0.0019(17) 0.0030(18) -0.015(2) O3 0.064(3) 0.023(2) 0.016(2) 0.0029(18) 0.010(2) 0.003(2) O4 0.044(3) 0.063(4) 0.097(5) 0.048(3) -0.008(3) -0.015(3) O5 0.036(6) 0.043(8) 0.040(7) -0.005(6) 0.002(6) -0.002(5) O5' 0.031(6) 0.035(7) 0.088(11) 0.004(7) -0.011(8) 0.010(5) O6 0.042(3) 0.025(2) 0.020(2) -0.0017(17) 0.0057(19) -0.005(2) O1W 0.043(6) 0.058(6) 0.034(6) 0.013(5) 0.020(5) 0.025(5) O2W' 0.038(6) 0.042(6) 0.051(7) 0.005(5) 0.001(5) 0.011(5) O2W 0.040(7) 0.072(8) 0.083(10) -0.044(7) 0.004(6) 0.003(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Cd1 O1 2.201(4) . ? Cd1 O4 2.245(5) 3_656 ? Cd1 O2 2.279(4) 3_657 ? Cd1 O6 2.282(4) 2_646 ? Cd1 O3 2.299(4) 2_646 ? Cd1 O5 2.539(12) 3_656 ? Cd2 O2W 2.088(10) . ? Cd2 O6 2.231(4) . ? Cd2 O3 2.245(4) 4_566 ? Cd2 O6 2.295(4) 3_667 ? Cd2 O2 2.312(4) . ? Cd2 O1W 2.354(9) . ? Cd2 O2W' 2.471(9) . ? Cd2 Cd2 3.4613(9) 3_667 ? P1 O1 1.514(4) . ? P1 O2 1.533(4) . ? P1 O3 1.537(4) . ? P1 C1 1.795(7) . ? C1 C2 1.510(8) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C7 1.366(9) . ? C2 C3 1.388(8) . ? C3 C4 1.389(9) . ? C3 H3 0.9300 . ? C4 C5 1.363(8) . ? C4 H4 0.9300 . ? C5 C6 1.392(9) . ? C5 C8 1.494(8) . ? C6 C7 1.383(9) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.394(9) . ? C8 C13 1.394(9) . ? C9 C10 1.391(8) . ? C9 C14 1.503(9) . ? C10 C11 1.380(10) . ? C10 H10 0.9300 . ? C11 C12 1.365(11) . ? C11 H11 0.9300 . ? C12 C13 1.388(10) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 O5 1.181(14) . ? C14 O4 1.223(8) . ? C14 O5' 1.364(14) . ? O2 Cd1 2.279(4) 3_657 ? O3 Cd2 2.245(4) 4_565 ? O3 Cd1 2.299(4) 2_656 ? O4 Cd1 2.245(5) 3_656 ? O5 O5' 0.840(13) . ? O5 Cd1 2.539(12) 3_656 ? O6 Cd1 2.282(4) 2_656 ? O6 Cd2 2.295(4) 3_667 ? O1W O2W 1.773(17) . ? O2W' O2W 1.205(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O4 155.93(18) . 3_656 ? O1 Cd1 O2 90.62(15) . 3_657 ? O4 Cd1 O2 96.98(17) 3_656 3_657 ? O1 Cd1 O6 84.51(14) . 2_646 ? O4 Cd1 O6 92.02(18) 3_656 2_646 ? O2 Cd1 O6 167.60(14) 3_657 2_646 ? O1 Cd1 O3 105.55(15) . 2_646 ? O4 Cd1 O3 98.5(2) 3_656 2_646 ? O2 Cd1 O3 75.33(14) 3_657 2_646 ? O6 Cd1 O3 94.96(14) 2_646 2_646 ? O1 Cd1 O5 107.4(3) . 3_656 ? O4 Cd1 O5 48.5(3) 3_656 3_656 ? O2 Cd1 O5 105.3(3) 3_657 3_656 ? O6 Cd1 O5 87.1(3) 2_646 3_656 ? O3 Cd1 O5 147.0(3) 2_646 3_656 ? O2W Cd2 O6 134.7(4) . . ? O2W Cd2 O3 113.2(4) . 4_566 ? O6 Cd2 O3 112.04(16) . 4_566 ? O2W Cd2 O6 88.1(3) . 3_667 ? O6 Cd2 O6 80.24(15) . 3_667 ? O3 Cd2 O6 108.30(14) 4_566 3_667 ? O2W Cd2 O2 92.2(3) . . ? O6 Cd2 O2 96.35(14) . . ? O3 Cd2 O2 75.71(14) 4_566 . ? O6 Cd2 O2 175.45(13) 3_667 . ? O2W Cd2 O1W 46.6(4) . . ? O6 Cd2 O1W 89.3(2) . . ? O3 Cd2 O1W 154.1(2) 4_566 . ? O6 Cd2 O1W 89.1(3) 3_667 . ? O2 Cd2 O1W 87.9(3) . . ? O2W Cd2 O2W' 29.1(4) . . ? O6 Cd2 O2W' 163.4(3) . . ? O3 Cd2 O2W' 84.5(3) 4_566 . ? O6 Cd2 O2W' 92.8(2) 3_667 . ? O2 Cd2 O2W' 89.7(2) . . ? O1W Cd2 O2W' 75.4(3) . . ? O2W Cd2 Cd2 115.5(4) . 3_667 ? O6 Cd2 Cd2 40.80(10) . 3_667 ? O3 Cd2 Cd2 116.75(10) 4_566 3_667 ? O6 Cd2 Cd2 39.43(10) 3_667 3_667 ? O2 Cd2 Cd2 137.07(10) . 3_667 ? O1W Cd2 Cd2 88.9(2) . 3_667 ? O2W' Cd2 Cd2 130.6(2) . 3_667 ? O1 P1 O2 113.4(2) . . ? O1 P1 O3 111.0(2) . . ? O2 P1 O3 110.4(2) . . ? O1 P1 C1 108.1(3) . . ? O2 P1 C1 106.3(3) . . ? O3 P1 C1 107.3(3) . . ? C2 C1 P1 116.6(4) . . ? C2 C1 H1A 108.1 . . ? P1 C1 H1A 108.1 . . ? C2 C1 H1B 108.1 . . ? P1 C1 H1B 108.1 . . ? H1A C1 H1B 107.3 . . ? C7 C2 C3 116.9(6) . . ? C7 C2 C1 122.0(6) . . ? C3 C2 C1 121.0(6) . . ? C2 C3 C4 120.8(6) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 122.2(6) . . ? C5 C4 H4 118.9 . . ? C3 C4 H4 118.9 . . ? C4 C5 C6 117.0(6) . . ? C4 C5 C8 120.8(6) . . ? C6 C5 C8 122.1(6) . . ? C7 C6 C5 120.7(6) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C2 C7 C6 122.4(6) . . ? C2 C7 H7 118.8 . . ? C6 C7 H7 118.8 . . ? C9 C8 C13 118.2(6) . . ? C9 C8 C5 122.8(6) . . ? C13 C8 C5 119.0(6) . . ? C10 C9 C8 120.1(6) . . ? C10 C9 C14 117.9(6) . . ? C8 C9 C14 122.0(5) . . ? C11 C10 C9 120.5(7) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C12 C11 C10 120.0(7) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 120.0(7) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C8 121.0(7) . . ? C12 C13 H13 119.5 . . ? C8 C13 H13 119.5 . . ? O5 C14 O4 111.2(9) . . ? O5 C14 O5' 37.7(7) . . ? O4 C14 O5' 126.1(8) . . ? O5 C14 C9 126.5(8) . . ? O4 C14 C9 119.6(6) . . ? O5' C14 C9 110.9(8) . . ? P1 O1 Cd1 134.1(2) . . ? P1 O2 Cd1 130.5(2) . 3_657 ? P1 O2 Cd2 129.6(2) . . ? Cd1 O2 Cd2 99.90(14) 3_657 . ? P1 O3 Cd2 122.4(2) . 4_565 ? P1 O3 Cd1 136.1(2) . 2_656 ? Cd2 O3 Cd1 101.30(15) 4_565 2_656 ? C14 O4 Cd1 103.9(5) . 3_656 ? O5' O5 C14 83.0(16) . . ? O5' O5 Cd1 100.0(15) . 3_656 ? C14 O5 Cd1 90.1(7) . 3_656 ? O5 O5' C14 59.3(13) . . ? Cd2 O6 Cd1 113.51(17) . 2_656 ? Cd2 O6 Cd2 99.76(15) . 3_667 ? Cd1 O6 Cd2 114.25(17) 2_656 3_667 ? O2W O1W Cd2 58.8(4) . . ? O2W O2W' Cd2 57.5(6) . . ? O2W' O2W O1W 164.6(10) . . ? O2W' O2W Cd2 93.3(8) . . ? O1W O2W Cd2 74.6(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 P1 C1 C2 -56.3(5) . . . . ? O2 P1 C1 C2 -178.4(5) . . . . ? O3 P1 C1 C2 63.4(5) . . . . ? P1 C1 C2 C7 103.0(7) . . . . ? P1 C1 C2 C3 -79.3(7) . . . . ? C7 C2 C3 C4 -0.2(11) . . . . ? C1 C2 C3 C4 -178.0(6) . . . . ? C2 C3 C4 C5 -0.5(12) . . . . ? C3 C4 C5 C6 0.9(11) . . . . ? C3 C4 C5 C8 177.3(7) . . . . ? C4 C5 C6 C7 -0.6(11) . . . . ? C8 C5 C6 C7 -176.9(6) . . . . ? C3 C2 C7 C6 0.5(11) . . . . ? C1 C2 C7 C6 178.3(6) . . . . ? C5 C6 C7 C2 -0.1(11) . . . . ? C4 C5 C8 C9 57.4(9) . . . . ? C6 C5 C8 C9 -126.3(7) . . . . ? C4 C5 C8 C13 -120.8(8) . . . . ? C6 C5 C8 C13 55.4(9) . . . . ? C13 C8 C9 C10 2.9(9) . . . . ? C5 C8 C9 C10 -175.4(6) . . . . ? C13 C8 C9 C14 -176.6(6) . . . . ? C5 C8 C9 C14 5.2(9) . . . . ? C8 C9 C10 C11 -2.0(9) . . . . ? C14 C9 C10 C11 177.4(6) . . . . ? C9 C10 C11 C12 -1.4(10) . . . . ? C10 C11 C12 C13 4.0(11) . . . . ? C11 C12 C13 C8 -3.1(12) . . . . ? C9 C8 C13 C12 -0.4(10) . . . . ? C5 C8 C13 C12 177.9(6) . . . . ? C10 C9 C14 O5 -64.2(12) . . . . ? C8 C9 C14 O5 115.2(10) . . . . ? C10 C9 C14 O4 95.6(8) . . . . ? C8 C9 C14 O4 -84.9(9) . . . . ? C10 C9 C14 O5' -103.8(9) . . . . ? C8 C9 C14 O5' 75.7(10) . . . . ? O2 P1 O1 Cd1 -58.6(4) . . . . ? O3 P1 O1 Cd1 66.4(4) . . . . ? C1 P1 O1 Cd1 -176.2(3) . . . . ? O4 Cd1 O1 P1 -7.6(7) 3_656 . . . ? O2 Cd1 O1 P1 101.2(3) 3_657 . . . ? O6 Cd1 O1 P1 -90.3(3) 2_646 . . . ? O3 Cd1 O1 P1 176.1(3) 2_646 . . . ? O5 Cd1 O1 P1 -5.1(4) 3_656 . . . ? O1 P1 O2 Cd1 -54.5(4) . . . 3_657 ? O3 P1 O2 Cd1 -179.9(3) . . . 3_657 ? C1 P1 O2 Cd1 64.1(4) . . . 3_657 ? O1 P1 O2 Cd2 125.1(3) . . . . ? O3 P1 O2 Cd2 -0.2(4) . . . . ? C1 P1 O2 Cd2 -116.3(3) . . . . ? O2W Cd2 O2 P1 -87.5(5) . . . . ? O6 Cd2 O2 P1 47.9(3) . . . . ? O3 Cd2 O2 P1 159.1(3) 4_566 . . . ? O6 Cd2 O2 P1 7(2) 3_667 . . . ? O1W Cd2 O2 P1 -41.1(4) . . . . ? O2W' Cd2 O2 P1 -116.5(4) . . . . ? Cd2 Cd2 O2 P1 45.0(4) 3_667 . . . ? O2W Cd2 O2 Cd1 92.2(4) . . . 3_657 ? O6 Cd2 O2 Cd1 -132.34(16) . . . 3_657 ? O3 Cd2 O2 Cd1 -21.16(16) 4_566 . . 3_657 ? O6 Cd2 O2 Cd1 -173.4(18) 3_667 . . 3_657 ? O1W Cd2 O2 Cd1 138.6(3) . . . 3_657 ? O2W' Cd2 O2 Cd1 63.2(3) . . . 3_657 ? Cd2 Cd2 O2 Cd1 -135.24(9) 3_667 . . 3_657 ? O1 P1 O3 Cd2 7.4(4) . . . 4_565 ? O2 P1 O3 Cd2 134.1(3) . . . 4_565 ? C1 P1 O3 Cd2 -110.5(3) . . . 4_565 ? O1 P1 O3 Cd1 -178.7(3) . . . 2_656 ? O2 P1 O3 Cd1 -52.0(4) . . . 2_656 ? C1 P1 O3 Cd1 63.4(4) . . . 2_656 ? O5 C14 O4 Cd1 -26.0(9) . . . 3_656 ? O5' C14 O4 Cd1 13.9(12) . . . 3_656 ? C9 C14 O4 Cd1 171.2(5) . . . 3_656 ? O4 C14 O5 O5' 122.1(15) . . . . ? C9 C14 O5 O5' -76.6(17) . . . . ? O4 C14 O5 Cd1 22.1(7) . . . 3_656 ? O5' C14 O5 Cd1 -100.0(15) . . . 3_656 ? C9 C14 O5 Cd1 -176.6(7) . . . 3_656 ? Cd1 O5 O5' C14 88.9(8) 3_656 . . . ? O4 C14 O5' O5 -77.8(18) . . . . ? C9 C14 O5' O5 123.2(14) . . . . ? O2W Cd2 O6 Cd1 44.5(5) . . . 2_656 ? O3 Cd2 O6 Cd1 -132.14(17) 4_566 . . 2_656 ? O6 Cd2 O6 Cd1 122.0(2) 3_667 . . 2_656 ? O2 Cd2 O6 Cd1 -55.01(19) . . . 2_656 ? O1W Cd2 O6 Cd1 32.8(3) . . . 2_656 ? O2W' Cd2 O6 Cd1 55.6(9) . . . 2_656 ? Cd2 Cd2 O6 Cd1 122.0(2) 3_667 . . 2_656 ? O2W Cd2 O6 Cd2 -77.4(4) . . . 3_667 ? O3 Cd2 O6 Cd2 105.90(16) 4_566 . . 3_667 ? O6 Cd2 O6 Cd2 0.0 3_667 . . 3_667 ? O2 Cd2 O6 Cd2 -176.97(15) . . . 3_667 ? O1W Cd2 O6 Cd2 -89.2(3) . . . 3_667 ? O2W' Cd2 O6 Cd2 -66.4(9) . . . 3_667 ? O6 Cd2 O1W O2W 168.5(5) . . . . ? O3 Cd2 O1W O2W -45.0(9) 4_566 . . . ? O6 Cd2 O1W O2W 88.3(5) 3_667 . . . ? O2 Cd2 O1W O2W -95.1(5) . . . . ? O2W' Cd2 O1W O2W -4.9(5) . . . . ? Cd2 Cd2 O1W O2W 127.7(5) 3_667 . . . ? O6 Cd2 O2W' O2W -16.3(14) . . . . ? O3 Cd2 O2W' O2W 170.9(8) 4_566 . . . ? O6 Cd2 O2W' O2W -81.0(8) 3_667 . . . ? O2 Cd2 O2W' O2W 95.2(8) . . . . ? O1W Cd2 O2W' O2W 7.3(8) . . . . ? Cd2 Cd2 O2W' O2W -68.3(8) 3_667 . . . ? Cd2 O2W' O2W O1W -38(4) . . . . ? Cd2 O1W O2W O2W' 40(4) . . . . ? O6 Cd2 O2W O2W' 173.5(6) . . . . ? O3 Cd2 O2W O2W' -9.9(8) 4_566 . . . ? O6 Cd2 O2W O2W' 99.2(7) 3_667 . . . ? O2 Cd2 O2W O2W' -85.3(7) . . . . ? O1W Cd2 O2W O2W' -170.2(10) . . . . ? Cd2 Cd2 O2W O2W' 128.5(7) 3_667 . . . ? O6 Cd2 O2W O1W -16.3(7) . . . . ? O3 Cd2 O2W O1W 160.4(4) 4_566 . . . ? O6 Cd2 O2W O1W -90.5(5) 3_667 . . . ? O2 Cd2 O2W O1W 84.9(5) . . . . ? O2W' Cd2 O2W O1W 170.2(10) . . . . ? Cd2 Cd2 O2W O1W -61.2(5) 3_667 . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.743 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.143 #======================================== data_compound-7 _database_code_depnum_ccdc_archive 'CCDC 852767' #TrackingRef 'Crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H27 Cd N4 O5 P, 2.5 (H2 O)' _chemical_formula_sum 'C38 H32 Cd N4 O7.50 P' _chemical_formula_weight 808.05 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' 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' Cd Cd -0.8075 1.2024 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 _symmetry_space_group_name_hall -p1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2243(17) _cell_length_b 12.7247(8) _cell_length_c 13.065(2) _cell_angle_alpha 95.695(9) _cell_angle_beta 102.674(13) _cell_angle_gamma 94.360(9) _cell_volume 1802.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3567 _cell_measurement_theta_min 2.9686 _cell_measurement_theta_max 29.1705 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 822 _exptl_absorpt_coefficient_mu 0.707 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8431 _exptl_absorpt_correction_T_max 0.8716 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11565 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0844 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6567 _reflns_number_gt 5063 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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. Because O1W O2W O3W and O4W are non-positive, we use 'isor' to refine them. ; _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^)+(0.0513P)^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 6567 _refine_ls_number_parameters 485 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1209 _refine_ls_wR_factor_gt 0.1070 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 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 Cd1 Cd 0.32292(3) 0.26954(2) 0.66614(2) 0.03417(13) Uani 1 1 d . . . P1 P 0.82892(11) 0.52754(9) 1.25377(9) 0.0348(3) Uani 1 1 d . . . C1 C 0.7591(6) 0.4750(4) 1.1187(4) 0.0573(15) Uani 1 1 d . . . H1A H 0.7252 0.5322 1.0816 0.069 Uiso 1 1 calc R . . H1B H 0.8228 0.4503 1.0854 0.069 Uiso 1 1 calc R . . C2 C 0.6595(5) 0.3856(4) 1.1047(4) 0.0483(13) Uani 1 1 d . . . C3 C 0.5376(5) 0.4046(4) 1.0880(4) 0.0506(13) Uani 1 1 d . . . H3 H 0.5173 0.4742 1.0906 0.061 Uiso 1 1 calc R . . C4 C 0.4451(5) 0.3216(4) 1.0675(4) 0.0478(13) Uani 1 1 d . . . H4 H 0.3637 0.3366 1.0558 0.057 Uiso 1 1 calc R . . C5 C 0.4713(5) 0.2159(4) 1.0639(3) 0.0428(12) Uani 1 1 d . . . C6 C 0.5938(5) 0.1970(4) 1.0856(4) 0.0502(13) Uani 1 1 d . . . H6 H 0.6145 0.1277 1.0873 0.060 Uiso 1 1 calc R . . C7 C 0.6865(5) 0.2812(4) 1.1051(4) 0.0541(14) Uani 1 1 d . . . H7 H 0.7681 0.2667 1.1185 0.065 Uiso 1 1 calc R . . C8 C 0.3717(5) 0.1272(4) 1.0447(4) 0.0469(12) Uani 1 1 d . . . C9 C 0.3782(6) 0.0551(5) 1.1195(4) 0.0668(17) Uani 1 1 d . . . H9 H 0.4454 0.0623 1.1767 0.080 Uiso 1 1 calc R . . C10 C 0.2864(6) -0.0265(5) 1.1098(5) 0.077(2) Uani 1 1 d . . . H10 H 0.2937 -0.0742 1.1598 0.092 Uiso 1 1 calc R . . C11 C 0.1856(6) -0.0382(4) 1.0282(5) 0.0657(16) Uani 1 1 d . . . H11 H 0.1233 -0.0922 1.0231 0.079 Uiso 1 1 calc R . . C12 C 0.1774(5) 0.0323(4) 0.9525(5) 0.0602(15) Uani 1 1 d . . . H12 H 0.1090 0.0245 0.8963 0.072 Uiso 1 1 calc R . . C13 C 0.2694(4) 0.1141(4) 0.9591(4) 0.0423(12) Uani 1 1 d . . . C14 C 0.2534(5) 0.1838(4) 0.8706(4) 0.0480(13) Uani 1 1 d . . . C15 C 0.4165(5) 0.0310(4) 0.6334(4) 0.0605(16) Uani 1 1 d . . . H15 H 0.4809 0.0605 0.6890 0.073 Uiso 1 1 calc R . . C16 C 0.4175(6) -0.0737(5) 0.5883(5) 0.0740(19) Uani 1 1 d . . . H16 H 0.4804 -0.1138 0.6155 0.089 Uiso 1 1 calc R . . C17 C 0.3268(6) -0.1157(4) 0.5054(5) 0.0682(18) Uani 1 1 d . . . H17 H 0.3283 -0.1843 0.4742 0.082 Uiso 1 1 calc R . . C18 C 0.2301(5) -0.0566(4) 0.4657(4) 0.0493(13) Uani 1 1 d . . . C19 C 0.1306(6) -0.0966(4) 0.3803(4) 0.0619(16) Uani 1 1 d . . . H19 H 0.1290 -0.1650 0.3472 0.074 Uiso 1 1 calc R . . C20 C 0.0383(6) -0.0380(4) 0.3460(4) 0.0600(15) Uani 1 1 d . . . H20 H -0.0263 -0.0666 0.2902 0.072 Uiso 1 1 calc R . . C21 C 0.0387(5) 0.0686(4) 0.3949(4) 0.0435(12) Uani 1 1 d . . . C22 C -0.0551(5) 0.1340(4) 0.3618(4) 0.0531(14) Uani 1 1 d . . . H22 H -0.1213 0.1087 0.3061 0.064 Uiso 1 1 calc R . . C23 C -0.0482(5) 0.2343(4) 0.4117(4) 0.0513(13) Uani 1 1 d . . . H23 H -0.1087 0.2783 0.3891 0.062 Uiso 1 1 calc R . . C24 C 0.0504(5) 0.2709(4) 0.4973(4) 0.0450(12) Uani 1 1 d . . . H24 H 0.0530 0.3390 0.5313 0.054 Uiso 1 1 calc R . . C25 C 0.1356(4) 0.1125(3) 0.4814(4) 0.0381(11) Uani 1 1 d . . . C26 C 0.2338(4) 0.0476(3) 0.5170(3) 0.0365(11) Uani 1 1 d . . . C27 C 0.3455(5) 0.3269(4) 0.4197(4) 0.0464(12) Uani 1 1 d . . . H27 H 0.2616 0.3060 0.4018 0.056 Uiso 1 1 calc R . . C28 C 0.4019(5) 0.3619(4) 0.3416(4) 0.0508(14) Uani 1 1 d . . . H28 H 0.3557 0.3645 0.2737 0.061 Uiso 1 1 calc R . . C29 C 0.5241(5) 0.3919(4) 0.3658(4) 0.0455(12) Uani 1 1 d . . . H29 H 0.5629 0.4142 0.3145 0.055 Uiso 1 1 calc R . . C30 C 0.5918(4) 0.3888(3) 0.4701(3) 0.0364(11) Uani 1 1 d . . . C31 C 0.7203(4) 0.4184(4) 0.5000(4) 0.0445(12) Uani 1 1 d . . . H31 H 0.7610 0.4415 0.4502 0.053 Uiso 1 1 calc R . . C32 C 0.7847(5) 0.4136(4) 0.5999(4) 0.0458(12) Uani 1 1 d . . . H32 H 0.8686 0.4344 0.6180 0.055 Uiso 1 1 calc R . . C33 C 0.7247(4) 0.3769(4) 0.6777(4) 0.0376(11) Uani 1 1 d . . . C34 C 0.7880(5) 0.3656(4) 0.7808(4) 0.0496(13) Uani 1 1 d . . . H34 H 0.8724 0.3836 0.8016 0.060 Uiso 1 1 calc R . . C35 C 0.7252(5) 0.3281(5) 0.8503(4) 0.0544(14) Uani 1 1 d . . . H35 H 0.7665 0.3199 0.9186 0.065 Uiso 1 1 calc R . . C36 C 0.6001(4) 0.3024(4) 0.8184(4) 0.0446(12) Uani 1 1 d . . . H36 H 0.5584 0.2788 0.8672 0.053 Uiso 1 1 calc R . . C37 C 0.5975(4) 0.3464(3) 0.6500(3) 0.0325(10) Uani 1 1 d . . . C38 C 0.5291(4) 0.3530(3) 0.5437(3) 0.0312(10) Uani 1 1 d . . . O1 O 0.8972(3) 0.4479(3) 1.3122(3) 0.0582(10) Uani 1 1 d . . . O2 O 0.7303(2) 0.57200(17) 1.30189(18) 0.0448(8) Uani 1 1 d . . . O3 O 0.9272(2) 0.62144(17) 1.24500(18) 0.0486(9) Uani 1 1 d R . . H3' H 0.8896 0.6708 1.2155 0.073 Uiso 1 1 d R . . O4 O 0.3387(4) 0.2015(3) 0.8267(3) 0.0626(11) Uani 1 1 d . . . O5 O 0.1500(4) 0.2172(3) 0.8443(4) 0.0908(16) Uani 1 1 d . . . O1W O 1.0762(5) 0.3599(5) 1.2325(4) 0.1111(17) Uani 1 1 d U . . O2W O 0.0084(10) 0.2533(10) 0.9733(9) 0.106(3) Uani 0.50 1 d PU . . O3W O 1.0860(12) 0.1631(10) 1.1630(10) 0.136(6) Uani 0.519(16) 1 d PU . . O4W O 0.0418(12) 0.4503(11) 1.0381(10) 0.047(3) Uani 0.25 1 d PU . . O5W O 0.0202(14) 0.3473(13) 1.0036(10) 0.056(4) Uani 0.25 1 d P . . N1 N 0.3263(4) 0.0889(3) 0.5986(3) 0.0432(10) Uani 1 1 d . . . N2 N 0.1408(3) 0.2113(3) 0.5320(3) 0.0354(9) Uani 1 1 d . . . N3 N 0.4069(3) 0.3224(3) 0.5184(3) 0.0358(9) Uani 1 1 d . . . N4 N 0.5360(3) 0.3098(3) 0.7212(3) 0.0363(9) 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 Cd1 0.0341(2) 0.0349(2) 0.0336(2) 0.00251(14) 0.00873(15) 0.00286(14) P1 0.0349(7) 0.0324(6) 0.0383(6) 0.0048(5) 0.0104(5) 0.0034(5) C1 0.076(4) 0.058(3) 0.036(3) 0.002(3) 0.016(3) -0.014(3) C2 0.060(4) 0.053(3) 0.026(2) -0.004(2) 0.006(2) -0.011(3) C3 0.070(4) 0.045(3) 0.035(3) 0.005(2) 0.008(3) 0.002(3) C4 0.058(4) 0.053(3) 0.032(3) 0.002(2) 0.008(2) 0.008(3) C5 0.049(3) 0.045(3) 0.031(2) 0.009(2) 0.001(2) 0.001(2) C6 0.051(4) 0.046(3) 0.048(3) 0.004(2) 0.002(3) 0.005(3) C7 0.046(3) 0.064(4) 0.050(3) 0.003(3) 0.009(3) 0.000(3) C8 0.049(3) 0.047(3) 0.044(3) 0.010(2) 0.008(2) 0.000(2) C9 0.069(4) 0.071(4) 0.056(3) 0.036(3) -0.003(3) -0.004(3) C10 0.088(5) 0.070(4) 0.076(4) 0.047(4) 0.011(4) 0.001(4) C11 0.061(4) 0.057(3) 0.082(4) 0.026(3) 0.021(4) -0.006(3) C12 0.051(4) 0.062(4) 0.063(4) 0.024(3) 0.003(3) -0.010(3) C13 0.041(3) 0.043(3) 0.042(3) 0.012(2) 0.007(2) -0.001(2) C14 0.056(4) 0.043(3) 0.035(3) 0.007(2) -0.005(3) -0.018(3) C15 0.058(4) 0.056(3) 0.063(4) 0.000(3) 0.002(3) 0.022(3) C16 0.080(5) 0.057(4) 0.082(4) 0.008(3) 0.001(4) 0.034(4) C17 0.089(5) 0.041(3) 0.073(4) -0.006(3) 0.013(4) 0.025(3) C18 0.067(4) 0.035(3) 0.047(3) -0.002(2) 0.017(3) 0.008(3) C19 0.084(5) 0.039(3) 0.056(3) -0.012(3) 0.010(3) 0.004(3) C20 0.076(4) 0.044(3) 0.046(3) -0.012(3) -0.005(3) -0.009(3) C21 0.048(3) 0.041(3) 0.037(3) 0.005(2) 0.004(2) -0.005(2) C22 0.047(3) 0.056(3) 0.047(3) 0.007(3) -0.005(3) -0.007(3) C23 0.042(3) 0.054(3) 0.057(3) 0.019(3) 0.004(3) 0.008(3) C24 0.043(3) 0.040(3) 0.053(3) 0.010(2) 0.011(3) 0.006(2) C25 0.044(3) 0.033(2) 0.039(3) 0.008(2) 0.012(2) -0.001(2) C26 0.043(3) 0.031(2) 0.035(2) 0.005(2) 0.009(2) 0.002(2) C27 0.041(3) 0.061(3) 0.037(3) 0.012(2) 0.004(2) 0.007(2) C28 0.052(4) 0.068(3) 0.037(3) 0.023(3) 0.013(3) 0.008(3) C29 0.049(3) 0.053(3) 0.042(3) 0.016(2) 0.020(2) 0.009(3) C30 0.040(3) 0.036(2) 0.040(3) 0.012(2) 0.016(2) 0.013(2) C31 0.039(3) 0.054(3) 0.049(3) 0.017(3) 0.022(2) 0.009(2) C32 0.032(3) 0.055(3) 0.053(3) 0.011(3) 0.015(2) 0.003(2) C33 0.033(3) 0.043(3) 0.038(3) 0.003(2) 0.010(2) 0.008(2) C34 0.034(3) 0.067(3) 0.046(3) 0.004(3) 0.005(2) 0.005(3) C35 0.038(3) 0.090(4) 0.036(3) 0.012(3) 0.007(2) 0.011(3) C36 0.038(3) 0.064(3) 0.031(3) 0.010(2) 0.006(2) 0.004(2) C37 0.031(3) 0.032(2) 0.038(2) 0.002(2) 0.013(2) 0.009(2) C38 0.031(3) 0.029(2) 0.036(2) 0.006(2) 0.012(2) 0.009(2) O1 0.056(2) 0.051(2) 0.072(2) 0.0237(19) 0.014(2) 0.0150(18) O2 0.047(2) 0.0315(16) 0.061(2) 0.0044(16) 0.0251(17) 0.0006(15) O3 0.035(2) 0.0478(19) 0.066(2) 0.0174(18) 0.0131(17) 0.0044(16) O4 0.087(3) 0.068(2) 0.038(2) 0.0163(19) 0.020(2) 0.005(2) O5 0.052(3) 0.090(3) 0.124(4) 0.073(3) -0.014(3) -0.009(2) O1W 0.097(3) 0.142(4) 0.105(3) 0.024(3) 0.034(3) 0.038(3) O2W 0.097(5) 0.120(5) 0.103(5) 0.031(4) 0.022(4) 0.006(4) O3W 0.151(8) 0.129(7) 0.134(7) 0.011(4) 0.048(5) 0.010(4) O4W 0.052(5) 0.055(5) 0.042(5) 0.006(4) 0.029(4) -0.002(4) O5W 0.067(10) 0.089(12) 0.027(7) 0.020(8) 0.024(7) 0.050(9) N1 0.050(3) 0.036(2) 0.043(2) 0.0062(19) 0.008(2) 0.009(2) N2 0.043(2) 0.0262(18) 0.037(2) 0.0028(17) 0.0102(18) 0.0014(17) N3 0.031(2) 0.043(2) 0.034(2) 0.0063(18) 0.0067(17) 0.0036(17) N4 0.035(2) 0.046(2) 0.033(2) 0.0084(18) 0.0142(18) 0.0106(18) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Cd1 O2 2.173(2) 2_667 ? Cd1 O4 2.324(3) . ? Cd1 N4 2.342(4) . ? Cd1 N1 2.384(4) . ? Cd1 N2 2.396(4) . ? Cd1 N3 2.455(3) . ? P1 O1 1.487(3) . ? P1 O2 1.506(2) . ? P1 O3 1.593(3) . ? P1 C1 1.804(5) . ? C1 C2 1.501(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.381(7) . ? C2 C7 1.386(7) . ? C3 C4 1.386(7) . ? C3 H3 0.9300 . ? C4 C5 1.396(6) . ? C4 H4 0.9300 . ? C5 C6 1.386(7) . ? C5 C8 1.489(7) . ? C6 C7 1.398(7) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.399(7) . ? C8 C13 1.402(7) . ? C9 C10 1.382(8) . ? C9 H9 0.9300 . ? C10 C11 1.361(8) . ? C10 H10 0.9300 . ? C11 C12 1.392(7) . ? C11 H11 0.9300 . ? C12 C13 1.392(7) . ? C12 H12 0.9300 . ? C13 C14 1.513(6) . ? C14 O4 1.238(6) . ? C14 O5 1.254(6) . ? C15 N1 1.324(6) . ? C15 C16 1.405(8) . ? C15 H15 0.9300 . ? C16 C17 1.346(8) . ? C16 H16 0.9300 . ? C17 C18 1.402(7) . ? C17 H17 0.9300 . ? C18 C19 1.416(8) . ? C18 C26 1.418(6) . ? C19 C20 1.346(7) . ? C19 H19 0.9300 . ? C20 C21 1.440(7) . ? C20 H20 0.9300 . ? C21 C22 1.411(7) . ? C21 C25 1.419(7) . ? C22 C23 1.364(7) . ? C22 H22 0.9300 . ? C23 C24 1.403(7) . ? C23 H23 0.9300 . ? C24 N2 1.339(5) . ? C24 H24 0.9300 . ? C25 N2 1.352(5) . ? C25 C26 1.451(6) . ? C26 N1 1.346(6) . ? C27 N3 1.330(5) . ? C27 C28 1.404(7) . ? C27 H27 0.9300 . ? C28 C29 1.353(7) . ? C28 H28 0.9300 . ? C29 C30 1.413(6) . ? C29 H29 0.9300 . ? C30 C38 1.401(6) . ? C30 C31 1.420(7) . ? C31 C32 1.355(6) . ? C31 H31 0.9300 . ? C32 C33 1.433(6) . ? C32 H32 0.9300 . ? C33 C37 1.407(6) . ? C33 C34 1.405(6) . ? C34 C35 1.366(7) . ? C34 H34 0.9300 . ? C35 C36 1.377(7) . ? C35 H35 0.9300 . ? C36 N4 1.331(5) . ? C36 H36 0.9300 . ? C37 N4 1.370(5) . ? C37 C38 1.446(6) . ? C38 N3 1.355(6) . ? O2 Cd1 2.173(2) 2_667 ? O3 H3' 0.8589 . ? O2W O5W 1.209(17) . ? O4W O5W 1.33(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cd1 O4 103.35(11) 2_667 . ? O2 Cd1 N4 98.24(11) 2_667 . ? O4 Cd1 N4 85.08(13) . . ? O2 Cd1 N1 164.03(12) 2_667 . ? O4 Cd1 N1 83.80(13) . . ? N4 Cd1 N1 96.58(13) . . ? O2 Cd1 N2 94.24(10) 2_667 . ? O4 Cd1 N2 116.80(13) . . ? N4 Cd1 N2 151.50(12) . . ? N1 Cd1 N2 69.82(12) . . ? O2 Cd1 N3 91.18(10) 2_667 . ? O4 Cd1 N3 152.82(13) . . ? N4 Cd1 N3 70.01(12) . . ? N1 Cd1 N3 88.30(13) . . ? N2 Cd1 N3 84.26(12) . . ? O1 P1 O2 115.37(18) . . ? O1 P1 O3 107.32(18) . . ? O2 P1 O3 109.75(15) . . ? O1 P1 C1 111.6(2) . . ? O2 P1 C1 107.6(2) . . ? O3 P1 C1 104.58(19) . . ? C2 C1 P1 115.3(3) . . ? C2 C1 H1A 108.5 . . ? P1 C1 H1A 108.5 . . ? C2 C1 H1B 108.5 . . ? P1 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? C3 C2 C7 117.8(5) . . ? C3 C2 C1 121.0(5) . . ? C7 C2 C1 121.1(5) . . ? C2 C3 C4 121.0(5) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C3 C4 C5 121.5(5) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C6 C5 C4 117.5(5) . . ? C6 C5 C8 121.2(4) . . ? C4 C5 C8 121.2(5) . . ? C5 C6 C7 120.6(5) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C2 C7 C6 121.5(5) . . ? C2 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C9 C8 C13 118.1(5) . . ? C9 C8 C5 117.6(5) . . ? C13 C8 C5 124.2(4) . . ? C10 C9 C8 121.1(5) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C11 C10 C9 121.0(5) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 118.9(6) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? C13 C12 C11 121.4(5) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C12 C13 C8 119.4(4) . . ? C12 C13 C14 117.1(4) . . ? C8 C13 C14 123.5(4) . . ? O4 C14 O5 124.1(5) . . ? O4 C14 C13 119.6(5) . . ? O5 C14 C13 116.2(5) . . ? N1 C15 C16 121.7(5) . . ? N1 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C17 C16 C15 119.5(5) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 120.5(5) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C19 123.4(5) . . ? C17 C18 C26 116.7(5) . . ? C19 C18 C26 119.8(5) . . ? C20 C19 C18 121.6(5) . . ? C20 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? C19 C20 C21 120.6(5) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C22 C21 C25 116.6(4) . . ? C22 C21 C20 123.1(5) . . ? C25 C21 C20 120.3(4) . . ? C23 C22 C21 119.8(5) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 119.8(5) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? N2 C24 C23 122.5(5) . . ? N2 C24 H24 118.7 . . ? C23 C24 H24 118.7 . . ? N2 C25 C21 123.4(4) . . ? N2 C25 C26 118.5(4) . . ? C21 C25 C26 118.0(4) . . ? N1 C26 C18 122.0(4) . . ? N1 C26 C25 118.3(4) . . ? C18 C26 C25 119.7(4) . . ? N3 C27 C28 122.8(5) . . ? N3 C27 H27 118.6 . . ? C28 C27 H27 118.6 . . ? C29 C28 C27 119.6(5) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C30 119.0(4) . . ? C28 C29 H29 120.5 . . ? C30 C29 H29 120.5 . . ? C38 C30 C29 118.1(4) . . ? C38 C30 C31 120.3(4) . . ? C29 C30 C31 121.6(4) . . ? C32 C31 C30 121.1(4) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C31 C32 C33 120.6(5) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C37 C33 C34 117.6(4) . . ? C37 C33 C32 119.5(4) . . ? C34 C33 C32 122.9(5) . . ? C35 C34 C33 119.7(5) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 119.4(4) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? N4 C36 C35 123.3(4) . . ? N4 C36 H36 118.3 . . ? C35 C36 H36 118.3 . . ? N4 C37 C33 121.8(4) . . ? N4 C37 C38 118.6(4) . . ? C33 C37 C38 119.6(4) . . ? N3 C38 C30 122.4(4) . . ? N3 C38 C37 118.7(4) . . ? C30 C38 C37 118.9(4) . . ? P1 O2 Cd1 134.50(13) . 2_667 ? P1 O3 H3' 109.2 . . ? C14 O4 Cd1 125.8(3) . . ? O2W O5W O4W 175.9(16) . . ? C15 N1 C26 119.6(4) . . ? C15 N1 Cd1 123.5(4) . . ? C26 N1 Cd1 116.8(3) . . ? C24 N2 C25 117.9(4) . . ? C24 N2 Cd1 125.8(3) . . ? C25 N2 Cd1 116.1(3) . . ? C27 N3 C38 118.1(4) . . ? C27 N3 Cd1 127.3(3) . . ? C38 N3 Cd1 114.6(3) . . ? C36 N4 C37 118.1(4) . . ? C36 N4 Cd1 123.9(3) . . ? C37 N4 Cd1 117.9(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 P1 C1 C2 65.6(5) . . . . ? O2 P1 C1 C2 -62.0(5) . . . . ? O3 P1 C1 C2 -178.6(4) . . . . ? P1 C1 C2 C3 94.5(5) . . . . ? P1 C1 C2 C7 -87.4(5) . . . . ? C7 C2 C3 C4 -2.9(7) . . . . ? C1 C2 C3 C4 175.2(4) . . . . ? C2 C3 C4 C5 0.7(7) . . . . ? C3 C4 C5 C6 2.4(7) . . . . ? C3 C4 C5 C8 178.3(4) . . . . ? C4 C5 C6 C7 -3.1(7) . . . . ? C8 C5 C6 C7 -179.1(5) . . . . ? C3 C2 C7 C6 2.1(7) . . . . ? C1 C2 C7 C6 -176.0(5) . . . . ? C5 C6 C7 C2 0.9(8) . . . . ? C6 C5 C8 C9 51.7(7) . . . . ? C4 C5 C8 C9 -124.1(5) . . . . ? C6 C5 C8 C13 -131.2(5) . . . . ? C4 C5 C8 C13 53.0(7) . . . . ? C13 C8 C9 C10 -0.2(9) . . . . ? C5 C8 C9 C10 177.0(6) . . . . ? C8 C9 C10 C11 -1.3(10) . . . . ? C9 C10 C11 C12 1.6(10) . . . . ? C10 C11 C12 C13 -0.4(9) . . . . ? C11 C12 C13 C8 -1.1(9) . . . . ? C11 C12 C13 C14 178.0(5) . . . . ? C9 C8 C13 C12 1.4(8) . . . . ? C5 C8 C13 C12 -175.7(5) . . . . ? C9 C8 C13 C14 -177.6(5) . . . . ? C5 C8 C13 C14 5.3(8) . . . . ? C12 C13 C14 O4 -130.3(5) . . . . ? C8 C13 C14 O4 48.7(7) . . . . ? C12 C13 C14 O5 47.3(7) . . . . ? C8 C13 C14 O5 -133.7(5) . . . . ? N1 C15 C16 C17 2.2(10) . . . . ? C15 C16 C17 C18 -1.7(10) . . . . ? C16 C17 C18 C19 -178.6(6) . . . . ? C16 C17 C18 C26 0.1(9) . . . . ? C17 C18 C19 C20 178.7(6) . . . . ? C26 C18 C19 C20 0.0(9) . . . . ? C18 C19 C20 C21 0.6(9) . . . . ? C19 C20 C21 C22 179.6(5) . . . . ? C19 C20 C21 C25 -1.2(8) . . . . ? C25 C21 C22 C23 0.9(7) . . . . ? C20 C21 C22 C23 -179.8(5) . . . . ? C21 C22 C23 C24 -1.6(8) . . . . ? C22 C23 C24 N2 1.1(8) . . . . ? C22 C21 C25 N2 0.3(7) . . . . ? C20 C21 C25 N2 -179.0(4) . . . . ? C22 C21 C25 C26 -179.7(4) . . . . ? C20 C21 C25 C26 1.0(7) . . . . ? C17 C18 C26 N1 1.0(7) . . . . ? C19 C18 C26 N1 179.8(5) . . . . ? C17 C18 C26 C25 -178.9(5) . . . . ? C19 C18 C26 C25 -0.1(7) . . . . ? N2 C25 C26 N1 -0.4(6) . . . . ? C21 C25 C26 N1 179.6(4) . . . . ? N2 C25 C26 C18 179.6(4) . . . . ? C21 C25 C26 C18 -0.4(6) . . . . ? N3 C27 C28 C29 0.5(8) . . . . ? C27 C28 C29 C30 -1.0(8) . . . . ? C28 C29 C30 C38 0.9(7) . . . . ? C28 C29 C30 C31 179.5(5) . . . . ? C38 C30 C31 C32 -0.5(7) . . . . ? C29 C30 C31 C32 -179.0(4) . . . . ? C30 C31 C32 C33 0.9(7) . . . . ? C31 C32 C33 C37 -0.5(7) . . . . ? C31 C32 C33 C34 176.9(5) . . . . ? C37 C33 C34 C35 -1.2(7) . . . . ? C32 C33 C34 C35 -178.7(5) . . . . ? C33 C34 C35 C36 -0.4(8) . . . . ? C34 C35 C36 N4 1.7(8) . . . . ? C34 C33 C37 N4 1.8(6) . . . . ? C32 C33 C37 N4 179.4(4) . . . . ? C34 C33 C37 C38 -177.8(4) . . . . ? C32 C33 C37 C38 -0.3(6) . . . . ? C29 C30 C38 N3 -0.4(6) . . . . ? C31 C30 C38 N3 -179.0(4) . . . . ? C29 C30 C38 C37 178.3(4) . . . . ? C31 C30 C38 C37 -0.3(6) . . . . ? N4 C37 C38 N3 -0.3(6) . . . . ? C33 C37 C38 N3 179.4(4) . . . . ? N4 C37 C38 C30 -179.0(4) . . . . ? C33 C37 C38 C30 0.7(6) . . . . ? O1 P1 O2 Cd1 134.4(2) . . . 2_667 ? O3 P1 O2 Cd1 13.0(3) . . . 2_667 ? C1 P1 O2 Cd1 -100.2(3) . . . 2_667 ? O5 C14 O4 Cd1 -13.2(8) . . . . ? C13 C14 O4 Cd1 164.2(3) . . . . ? O2 Cd1 O4 C14 64.5(4) 2_667 . . . ? N4 Cd1 O4 C14 161.8(4) . . . . ? N1 Cd1 O4 C14 -101.0(4) . . . . ? N2 Cd1 O4 C14 -37.4(5) . . . . ? N3 Cd1 O4 C14 -175.0(4) . . . . ? C16 C15 N1 C26 -1.1(8) . . . . ? C16 C15 N1 Cd1 -177.2(4) . . . . ? C18 C26 N1 C15 -0.6(7) . . . . ? C25 C26 N1 C15 179.4(4) . . . . ? C18 C26 N1 Cd1 175.8(3) . . . . ? C25 C26 N1 Cd1 -4.3(5) . . . . ? O2 Cd1 N1 C15 -175.2(4) 2_667 . . . ? O4 Cd1 N1 C15 -57.5(4) . . . . ? N4 Cd1 N1 C15 26.8(4) . . . . ? N2 Cd1 N1 C15 -179.0(4) . . . . ? N3 Cd1 N1 C15 96.4(4) . . . . ? O2 Cd1 N1 C26 8.6(6) 2_667 . . . ? O4 Cd1 N1 C26 126.3(3) . . . . ? N4 Cd1 N1 C26 -149.4(3) . . . . ? N2 Cd1 N1 C26 4.8(3) . . . . ? N3 Cd1 N1 C26 -79.7(3) . . . . ? C23 C24 N2 C25 0.2(7) . . . . ? C23 C24 N2 Cd1 173.9(4) . . . . ? C21 C25 N2 C24 -0.9(7) . . . . ? C26 C25 N2 C24 179.1(4) . . . . ? C21 C25 N2 Cd1 -175.3(3) . . . . ? C26 C25 N2 Cd1 4.8(5) . . . . ? O2 Cd1 N2 C24 2.3(4) 2_667 . . . ? O4 Cd1 N2 C24 109.6(4) . . . . ? N4 Cd1 N2 C24 -113.7(4) . . . . ? N1 Cd1 N2 C24 -178.8(4) . . . . ? N3 Cd1 N2 C24 -88.5(4) . . . . ? O2 Cd1 N2 C25 176.2(3) 2_667 . . . ? O4 Cd1 N2 C25 -76.6(3) . . . . ? N4 Cd1 N2 C25 60.2(4) . . . . ? N1 Cd1 N2 C25 -4.9(3) . . . . ? N3 Cd1 N2 C25 85.4(3) . . . . ? C28 C27 N3 C38 0.0(7) . . . . ? C28 C27 N3 Cd1 177.7(4) . . . . ? C30 C38 N3 C27 -0.1(6) . . . . ? C37 C38 N3 C27 -178.7(4) . . . . ? C30 C38 N3 Cd1 -178.0(3) . . . . ? C37 C38 N3 Cd1 3.3(5) . . . . ? O2 Cd1 N3 C27 -82.9(4) 2_667 . . . ? O4 Cd1 N3 C27 154.0(4) . . . . ? N4 Cd1 N3 C27 178.8(4) . . . . ? N1 Cd1 N3 C27 81.2(4) . . . . ? N2 Cd1 N3 C27 11.3(4) . . . . ? O2 Cd1 N3 C38 94.9(3) 2_667 . . . ? O4 Cd1 N3 C38 -28.2(5) . . . . ? N4 Cd1 N3 C38 -3.5(3) . . . . ? N1 Cd1 N3 C38 -101.1(3) . . . . ? N2 Cd1 N3 C38 -171.0(3) . . . . ? C35 C36 N4 C37 -1.1(7) . . . . ? C35 C36 N4 Cd1 -178.9(4) . . . . ? C33 C37 N4 C36 -0.7(6) . . . . ? C38 C37 N4 C36 179.0(4) . . . . ? C33 C37 N4 Cd1 177.2(3) . . . . ? C38 C37 N4 Cd1 -3.1(5) . . . . ? O2 Cd1 N4 C36 92.9(4) 2_667 . . . ? O4 Cd1 N4 C36 -9.9(4) . . . . ? N1 Cd1 N4 C36 -93.0(4) . . . . ? N2 Cd1 N4 C36 -152.0(3) . . . . ? N3 Cd1 N4 C36 -178.8(4) . . . . ? O2 Cd1 N4 C37 -84.8(3) 2_667 . . . ? O4 Cd1 N4 C37 172.4(3) . . . . ? N1 Cd1 N4 C37 89.2(3) . . . . ? N2 Cd1 N4 C37 30.2(4) . . . . ? N3 Cd1 N4 C37 3.4(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3' O5 0.86 1.73 2.575(4) 165.9 2_667 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.671 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.094 #========================================end