# 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 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Xiao-Yang Yu' _publ_contact_author_email 'yangyangyu_0@yahoo.com.cn ' _publ_author_name 'Xiao-Yang Yu' # Attachment '- 2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 742273' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H18 Fe3 N4 O18' _chemical_formula_weight 769.93 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.4427(13) _cell_length_b 9.5515(19) _cell_length_c 10.224(2) _cell_angle_alpha 107.45(3) _cell_angle_beta 91.15(3) _cell_angle_gamma 101.70(3) _cell_volume 585.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 388 _exptl_absorpt_coefficient_mu 1.943 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7463 _exptl_absorpt_correction_T_max 0.9351 _exptl_absorpt_process_details sadabs _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4630 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2047 _reflns_number_gt 1531 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1488P)^2^+4.3218P] 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 2047 _refine_ls_number_parameters 206 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1030 _refine_ls_R_factor_gt 0.0792 _refine_ls_wR_factor_ref 0.2358 _refine_ls_wR_factor_gt 0.2211 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.035 _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 Fe1 Fe 0.29908(19) 0.19578(13) 0.66368(11) 0.0173(4) Uani 1 1 d . . . Fe2 Fe 0.5000 0.5000 0.5000 0.0193(5) Uani 1 2 d S . . C1 C 0.2680(13) 0.0728(10) 0.8574(9) 0.0179(18) Uani 1 1 d . . . C2 C 0.2520(13) 0.0108(10) 0.9752(8) 0.0172(17) Uani 1 1 d . . . C3 C 0.2935(13) 0.1039(9) 1.1074(8) 0.0156(17) Uani 1 1 d . . . H3 H 0.3345 0.2073 1.1244 0.019 Uiso 1 1 calc R . . C4 C 0.2748(13) 0.0454(9) 1.2181(8) 0.0159(17) Uani 1 1 d . . . C5 C 0.2185(12) -0.1115(9) 1.1920(8) 0.0139(16) Uani 1 1 d D . . C6 C 0.1823(13) -0.2037(9) 1.0573(9) 0.0165(17) Uani 1 1 d . . . H6 H 0.1496 -0.3074 1.0396 0.020 Uiso 1 1 calc R . . C7 C 0.1936(13) -0.1454(10) 0.9459(8) 0.0178(18) Uani 1 1 d . . . C8 C 0.1462(13) -0.2420(10) 0.8046(9) 0.0222(19) Uani 1 1 d . . . C9 C 0.3141(13) 0.1526(10) 1.3606(9) 0.0206(19) Uani 1 1 d . . . C10 C 0.1991(12) -0.1870(8) 1.3087(8) 0.0124(16) Uani 1 1 d DU . . N1 N 0.2326(12) -0.0149(8) 0.7304(7) 0.0211(16) Uani 1 1 d . . . N2 N 0.1702(13) -0.1713(10) 0.7089(8) 0.0284(18) Uani 1 1 d . . . H2 H 0.1446 -0.2276 0.6246 0.034 Uiso 1 1 calc R . . O1 O 0.3184(10) 0.2135(7) 0.8754(6) 0.0227(14) Uani 1 1 d . . . O2 O 0.0856(11) -0.3829(8) 0.7721(7) 0.0327(16) Uani 1 1 d . . . O3 O 0.3861(12) 0.2890(6) 1.3734(7) 0.0314(16) Uani 1 1 d . . . O4 O 0.2688(11) 0.0983(7) 1.4579(6) 0.0291(15) Uani 1 1 d . . . O5 O 0.3637(9) -0.2141(6) 1.3455(6) 0.0193(13) Uani 1 1 d . . . O6 O 0.0193(10) -0.2246(7) 1.3396(6) 0.0229(14) Uani 1 1 d . . . O1W O 0.3082(12) 0.4662(8) 0.1020(7) 0.0360(17) Uani 1 1 d . . . H1WB H 0.1784 0.4576 0.1188 0.054 Uiso 1 1 d R . . H1WA H 0.3281 0.3987 0.0304 0.054 Uiso 1 1 d R . . O2W O 0.7856(10) 0.4363(7) 0.5442(6) 0.0267(14) Uani 1 1 d . . . H2WB H 0.7514 0.3624 0.5760 0.032 Uiso 1 1 d R . . H2WA H 0.9146 0.4338 0.5591 0.032 Uiso 1 1 d R . . O3W O 0.3847(9) 0.4407(7) 0.6910(6) 0.0215(13) Uani 1 1 d . . . H3WA H 0.2530 0.4411 0.6859 0.032 Uiso 1 1 d R . . H3WB H 0.4719 0.4578 0.7606 0.032 Uiso 1 1 d 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 Fe1 0.0221(7) 0.0197(7) 0.0108(6) 0.0064(5) 0.0008(5) 0.0036(5) Fe2 0.0253(10) 0.0133(9) 0.0160(9) 0.0020(7) -0.0024(7) 0.0014(7) C1 0.017(4) 0.024(5) 0.018(4) 0.009(4) 0.004(3) 0.009(4) C2 0.017(4) 0.022(5) 0.010(4) 0.003(3) -0.002(3) 0.002(3) C3 0.023(4) 0.010(4) 0.015(4) 0.007(3) -0.001(3) 0.003(3) C4 0.018(4) 0.019(4) 0.013(4) 0.007(3) 0.003(3) 0.007(3) C5 0.011(4) 0.014(4) 0.019(4) 0.012(3) -0.003(3) -0.001(3) C6 0.018(4) 0.010(4) 0.021(4) 0.004(3) 0.002(3) 0.002(3) C7 0.018(4) 0.022(4) 0.017(4) 0.008(4) 0.003(3) 0.010(3) C8 0.014(4) 0.025(5) 0.021(4) -0.002(4) 0.001(3) 0.005(4) C9 0.014(4) 0.022(5) 0.021(4) 0.001(4) -0.006(3) 0.004(3) C10 0.013(3) 0.007(3) 0.015(3) 0.000(2) 0.000(2) 0.001(2) N1 0.025(4) 0.021(4) 0.015(4) 0.003(3) 0.000(3) 0.003(3) N2 0.033(5) 0.037(5) 0.014(4) 0.003(3) 0.000(3) 0.013(4) O1 0.029(4) 0.019(3) 0.020(3) 0.008(3) -0.002(3) 0.001(3) O2 0.035(4) 0.026(4) 0.029(4) -0.001(3) 0.002(3) 0.004(3) O3 0.058(5) 0.007(3) 0.023(3) 0.003(3) -0.002(3) -0.003(3) O4 0.049(4) 0.023(3) 0.013(3) 0.006(3) 0.000(3) 0.004(3) O5 0.025(3) 0.018(3) 0.014(3) 0.005(2) -0.001(2) 0.002(3) O6 0.033(4) 0.024(3) 0.015(3) 0.012(3) 0.003(3) 0.005(3) O1W 0.043(4) 0.029(4) 0.028(4) 0.002(3) -0.002(3) 0.001(3) O2W 0.023(3) 0.034(4) 0.026(3) 0.014(3) -0.001(3) 0.007(3) O3W 0.019(3) 0.020(3) 0.025(3) 0.006(3) 0.002(3) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O4 2.017(6) 1_554 ? Fe1 O1 2.120(6) . ? Fe1 O6 2.125(6) 2_557 ? Fe1 O5 2.150(6) 2_657 ? Fe1 O3W 2.221(6) . ? Fe1 N1 2.277(7) . ? Fe2 O3 2.018(6) 2_667 ? Fe2 O3 2.018(6) 1_554 ? Fe2 O2W 2.132(6) 2_666 ? Fe2 O2W 2.132(6) . ? Fe2 O3W 2.289(6) 2_666 ? Fe2 O3W 2.289(6) . ? C1 O1 1.271(11) . ? C1 N1 1.303(11) . ? C1 C2 1.491(11) . ? C2 C3 1.363(12) . ? C2 C7 1.398(12) . ? C3 C4 1.402(11) . ? C4 C5 1.408(12) . ? C4 C9 1.490(12) . ? C5 C6 1.379(12) . ? C5 C10 1.564(9) . ? C6 C7 1.407(11) . ? C7 C8 1.449(12) . ? C8 O2 1.260(11) . ? C8 N2 1.342(12) . ? C9 O3 1.257(11) . ? C9 O4 1.266(11) . ? C10 O6 1.218(9) . ? C10 O5 1.219(10) . ? N1 N2 1.413(11) . ? O3 Fe2 2.018(6) 1_556 ? O4 Fe1 2.017(6) 1_556 ? O5 Fe1 2.150(6) 2_657 ? O6 Fe1 2.125(6) 2_557 ? 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 O4 Fe1 O1 158.7(3) 1_554 . ? O4 Fe1 O6 91.1(3) 1_554 2_557 ? O1 Fe1 O6 93.9(2) . 2_557 ? O4 Fe1 O5 87.3(3) 1_554 2_657 ? O1 Fe1 O5 92.3(2) . 2_657 ? O6 Fe1 O5 166.7(2) 2_557 2_657 ? O4 Fe1 O3W 104.2(2) 1_554 . ? O1 Fe1 O3W 96.9(2) . . ? O6 Fe1 O3W 84.4(2) 2_557 . ? O5 Fe1 O3W 83.1(2) 2_657 . ? O4 Fe1 N1 99.2(3) 1_554 . ? O1 Fe1 N1 59.7(2) . . ? O6 Fe1 N1 96.6(2) 2_557 . ? O5 Fe1 N1 96.7(2) 2_657 . ? O3W Fe1 N1 156.6(3) . . ? O3 Fe2 O3 180.000(1) 2_667 1_554 ? O3 Fe2 O2W 89.4(3) 2_667 2_666 ? O3 Fe2 O2W 90.6(3) 1_554 2_666 ? O3 Fe2 O2W 90.6(3) 2_667 . ? O3 Fe2 O2W 89.4(3) 1_554 . ? O2W Fe2 O2W 180.000(1) 2_666 . ? O3 Fe2 O3W 93.2(2) 2_667 2_666 ? O3 Fe2 O3W 86.8(2) 1_554 2_666 ? O2W Fe2 O3W 85.9(2) 2_666 2_666 ? O2W Fe2 O3W 94.1(2) . 2_666 ? O3 Fe2 O3W 86.8(2) 2_667 . ? O3 Fe2 O3W 93.2(2) 1_554 . ? O2W Fe2 O3W 94.1(2) 2_666 . ? O2W Fe2 O3W 85.9(2) . . ? O3W Fe2 O3W 180.000(2) 2_666 . ? O1 C1 N1 116.7(8) . . ? O1 C1 C2 121.8(8) . . ? N1 C1 C2 121.5(8) . . ? C3 C2 C7 121.2(8) . . ? C3 C2 C1 120.8(8) . . ? C7 C2 C1 118.0(7) . . ? C2 C3 C4 120.6(8) . . ? C3 C4 C5 119.5(7) . . ? C3 C4 C9 118.4(8) . . ? C5 C4 C9 122.1(7) . . ? C6 C5 C4 118.8(7) . . ? C6 C5 C10 118.1(7) . . ? C4 C5 C10 123.1(7) . . ? C5 C6 C7 121.9(8) . . ? C2 C7 C6 117.9(8) . . ? C2 C7 C8 120.2(8) . . ? C6 C7 C8 121.9(8) . . ? O2 C8 N2 121.5(8) . . ? O2 C8 C7 123.1(8) . . ? N2 C8 C7 115.4(8) . . ? O3 C9 O4 125.8(8) . . ? O3 C9 C4 117.2(8) . . ? O4 C9 C4 117.0(8) . . ? O6 C10 O5 129.0(7) . . ? O6 C10 C5 115.7(7) . . ? O5 C10 C5 114.8(7) . . ? C1 N1 N2 117.3(7) . . ? C1 N1 Fe1 87.8(5) . . ? N2 N1 Fe1 154.8(6) . . ? C8 N2 N1 127.5(8) . . ? C1 O1 Fe1 95.8(5) . . ? C9 O3 Fe2 148.1(6) . 1_556 ? C9 O4 Fe1 131.4(6) . 1_556 ? C10 O5 Fe1 149.5(5) . 2_657 ? C10 O6 Fe1 146.8(5) . 2_557 ? Fe1 O3W Fe2 114.6(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 N2 H2 O2W 0.86 2.34 3.095(10) 146.4 2_656 O1W H1WB O2 0.85 2.17 2.942(10) 151.0 2_556 O1W H1WA O1 0.85 1.98 2.813(9) 167.1 1_554 O2W H2WB O5 0.85 1.87 2.711(9) 170.4 2_657 O2W H2WB O6 0.85 2.47 3.081(9) 129.6 2_657 O2W H2WA O2 0.85 2.42 2.863(10) 113.3 1_665 O2W H2WA O2W 0.85 2.51 3.054(13) 123.2 2_766 O2W H2WB O6 0.85 2.47 3.081(9) 129.6 2_657 O3W H3WA O2 0.85 2.16 2.789(9) 131.1 1_565 O3W H3WA O6 0.85 2.37 2.921(9) 123.1 2_557 O3W H3WB O1W 0.85 1.84 2.678(10) 166.1 2_666 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.628 _refine_diff_density_min -0.760 _refine_diff_density_rms 0.237 data_1 _database_code_depnum_ccdc_archive 'CCDC 742939' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H18 Cu2 N4 O16' _chemical_formula_weight 697.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.6226(13) _cell_length_b 9.6570(19) _cell_length_c 9.752(2) _cell_angle_alpha 95.92(3) _cell_angle_beta 108.90(3) _cell_angle_gamma 94.26(3) _cell_volume 583.1(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.986 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 352 _exptl_absorpt_coefficient_mu 1.921 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8461 _exptl_absorpt_correction_T_max 0.8935 _exptl_absorpt_process_details sadabs _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5796 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2658 _reflns_number_gt 1940 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+0.5629P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2658 _refine_ls_number_parameters 204 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1242 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 1.42629(7) -0.13297(5) 0.45630(5) 0.02640(18) Uani 1 1 d U . . C1 C 0.7757(6) -0.1339(4) 0.2343(4) 0.0224(8) Uani 1 1 d . . . C2 C 0.7427(6) 0.0164(4) 0.2427(4) 0.0193(7) Uani 1 1 d . . . C3 C 0.5414(6) 0.0603(4) 0.1833(4) 0.0216(8) Uani 1 1 d . . . H3 H 0.4225 -0.0057 0.1370 0.026 Uiso 1 1 calc R . . C4 C 0.5166(6) 0.2012(4) 0.1925(4) 0.0208(8) Uani 1 1 d . . . C5 C 0.6998(6) 0.3006(4) 0.2624(4) 0.0196(7) Uani 1 1 d . . . C6 C 0.8971(6) 0.2561(4) 0.3239(4) 0.0214(8) Uani 1 1 d . . . H6 H 1.0154 0.3217 0.3731 0.026 Uiso 1 1 calc R . . C7 C 0.9228(5) 0.1140(4) 0.3137(4) 0.0182(7) Uani 1 1 d . . . C8 C 1.1330(6) 0.0688(4) 0.3777(4) 0.0195(7) Uani 1 1 d . . . C9 C 0.3025(6) 0.2532(4) 0.1348(4) 0.0263(8) Uani 1 1 d . . . C10 C 0.6888(6) 0.4564(4) 0.2751(4) 0.0245(8) Uani 1 1 d . . . N1 N 0.9756(5) -0.1618(3) 0.2987(4) 0.0251(7) Uani 1 1 d . . . N2 N 1.1594(5) -0.0658(3) 0.3705(3) 0.0207(6) Uani 1 1 d . . . O1 O 0.6272(4) -0.2295(3) 0.1698(3) 0.0317(7) Uani 1 1 d . . . O2 O 1.2922(4) 0.1626(3) 0.4435(3) 0.0288(6) Uani 1 1 d . . . O3 O 0.2757(5) 0.3759(3) 0.1553(4) 0.0421(8) Uani 1 1 d . . . O4 O 0.1463(5) 0.1542(3) 0.0609(3) 0.0361(7) Uani 1 1 d . . . H4 H 0.0363 0.1898 0.0234 0.054 Uiso 1 1 calc R . . O5 O 0.6873(5) 0.5067(3) 0.1545(3) 0.0339(7) Uani 1 1 d . . . H5 H 0.6589 0.5879 0.1591 0.051 Uiso 1 1 calc R . . O6 O 0.6987(6) 0.5255(3) 0.3862(3) 0.0479(9) Uani 1 1 d . . . O1W O 1.2365(5) -0.3776(3) 0.3712(4) 0.0428(7) Uani 1 1 d U . . H1WA H 1.2357 -0.3952 0.2838 0.051 Uiso 1 1 d R . . H1WB H 1.2627 -0.4503 0.4133 0.051 Uiso 1 1 d R . . O2W O 0.1858(6) 0.7078(5) 0.0553(4) 0.0481(9) Uani 1 1 d . . . H1 H 0.984(10) -0.257(7) 0.305(7) 0.072(19) Uiso 1 1 d . . . H2WA H 0.164(9) 0.618(6) 0.017(6) 0.051(17) Uiso 1 1 d . . . H2WB H 0.317(13) 0.740(8) 0.105(8) 0.10(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0162(2) 0.0268(3) 0.0327(3) 0.0058(2) 0.00174(19) 0.00793(18) C1 0.0222(18) 0.0181(18) 0.0250(19) 0.0060(16) 0.0043(15) 0.0024(14) C2 0.0191(17) 0.0163(17) 0.0219(18) 0.0047(15) 0.0053(15) 0.0027(14) C3 0.0180(17) 0.0184(17) 0.0240(18) 0.0028(15) 0.0018(15) -0.0020(14) C4 0.0188(18) 0.0212(18) 0.0233(18) 0.0048(16) 0.0070(15) 0.0053(14) C5 0.0190(18) 0.0141(16) 0.0254(19) 0.0036(15) 0.0065(15) 0.0037(13) C6 0.0160(17) 0.0168(17) 0.027(2) -0.0011(15) 0.0027(15) 0.0012(14) C7 0.0148(16) 0.0175(17) 0.0211(17) 0.0033(15) 0.0035(14) 0.0043(13) C8 0.0172(17) 0.0177(17) 0.0204(18) 0.0000(15) 0.0021(14) 0.0050(14) C9 0.0190(18) 0.031(2) 0.028(2) 0.0063(18) 0.0054(16) 0.0071(16) C10 0.0210(18) 0.0155(17) 0.032(2) 0.0027(17) 0.0018(16) 0.0067(14) N1 0.0188(16) 0.0158(15) 0.0350(19) 0.0037(14) 0.0011(14) 0.0028(12) N2 0.0134(14) 0.0165(15) 0.0279(17) 0.0039(13) 0.0003(12) 0.0033(11) O1 0.0217(14) 0.0168(13) 0.0475(18) 0.0025(13) 0.0001(13) 0.0009(11) O2 0.0154(13) 0.0169(13) 0.0438(17) -0.0010(12) -0.0026(12) 0.0019(10) O3 0.0287(16) 0.0285(16) 0.062(2) 0.0034(16) 0.0048(15) 0.0136(13) O4 0.0162(13) 0.0401(17) 0.0446(18) 0.0030(15) 0.0005(13) 0.0047(12) O5 0.0471(19) 0.0183(14) 0.0365(17) 0.0062(13) 0.0122(14) 0.0094(13) O6 0.081(3) 0.0265(16) 0.0333(18) -0.0029(14) 0.0146(18) 0.0205(17) O1W 0.061(2) 0.0223(11) 0.047(2) 0.0055(13) 0.0190(17) 0.0141(11) O2W 0.0238(18) 0.057(2) 0.054(2) 0.000(2) 0.0012(16) 0.0118(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.862(3) 2_856 ? Cu1 N2 1.889(3) . ? Cu1 O1W 2.516(3) . ? Cu1 Cu1 2.6291(13) 2_856 ? C1 O1 1.249(5) . ? C1 N1 1.330(5) . ? C1 C2 1.482(5) . ? C2 C3 1.388(5) . ? C2 C7 1.398(5) . ? C3 C4 1.380(5) . ? C3 H3 0.9300 . ? C4 C5 1.419(5) . ? C4 C9 1.492(5) . ? C5 C6 1.372(5) . ? C5 C10 1.507(5) . ? C6 C7 1.393(5) . ? C6 H6 0.9300 . ? C7 C8 1.450(5) . ? C8 O2 1.282(4) . ? C8 N2 1.322(4) . ? C9 O3 1.217(5) . ? C9 O4 1.316(5) . ? C10 O6 1.193(5) . ? C10 O5 1.315(5) . ? N1 N2 1.406(4) . ? N1 H1 0.94(6) . ? O2 Cu1 1.862(3) 2_856 ? O4 H4 0.8200 . ? O5 H5 0.8200 . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8499 . ? O2W H2WA 0.89(6) . ? O2W H2WB 0.86(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 N2 168.75(12) 2_856 . ? O2 Cu1 O1W 103.15(12) 2_856 . ? N2 Cu1 O1W 87.94(12) . . ? O2 Cu1 Cu1 83.83(9) 2_856 2_856 ? N2 Cu1 Cu1 84.99(10) . 2_856 ? O1W Cu1 Cu1 172.26(8) . 2_856 ? O1 C1 N1 121.4(3) . . ? O1 C1 C2 122.8(3) . . ? N1 C1 C2 115.9(3) . . ? C3 C2 C7 120.6(3) . . ? C3 C2 C1 121.9(3) . . ? C7 C2 C1 117.5(3) . . ? C4 C3 C2 120.4(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 119.1(3) . . ? C3 C4 C9 122.3(3) . . ? C5 C4 C9 118.5(3) . . ? C6 C5 C4 120.0(3) . . ? C6 C5 C10 117.1(3) . . ? C4 C5 C10 122.9(3) . . ? C5 C6 C7 120.9(3) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C6 C7 C2 118.9(3) . . ? C6 C7 C8 120.2(3) . . ? C2 C7 C8 120.9(3) . . ? O2 C8 N2 120.8(3) . . ? O2 C8 C7 118.3(3) . . ? N2 C8 C7 120.8(3) . . ? O3 C9 O4 123.4(4) . . ? O3 C9 C4 122.8(4) . . ? O4 C9 C4 113.8(3) . . ? O6 C10 O5 124.9(3) . . ? O6 C10 C5 122.9(3) . . ? O5 C10 C5 111.9(3) . . ? C1 N1 N2 127.8(3) . . ? C1 N1 H1 112(4) . . ? N2 N1 H1 119(4) . . ? C8 N2 N1 117.1(3) . . ? C8 N2 Cu1 123.3(3) . . ? N1 N2 Cu1 119.5(2) . . ? C8 O2 Cu1 127.0(2) . 2_856 ? C9 O4 H4 109.5 . . ? C10 O5 H5 109.5 . . ? Cu1 O1W H1WA 104.2 . . ? Cu1 O1W H1WB 128.0 . . ? H1WA O1W H1WB 109.1 . . ? H2WA O2W H2WB 116(6) . . ? 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 O2W H2WB O1 0.86(8) 1.93(8) 2.764(5) 162(8) 1_565 O2W H2WA O5 0.89(6) 2.46(6) 3.111(5) 130(4) 2_665 O1W H1WB O6 0.85 2.10 2.820(4) 142.1 2_756 O1W H1WA O3 0.85 2.50 3.094(5) 127.6 1_645 O1W H1WA O2W 0.85 2.47 3.190(5) 143.3 1_645 O5 H5 O1 0.82 1.79 2.604(4) 173.6 1_565 O4 H4 O2W 0.82 1.84 2.651(5) 172.2 2_565 N1 H1 O1W 0.94(6) 2.08(6) 2.807(4) 134(5) . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.703 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.133 # Attachment '- 4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 802479' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H44 Cd2 N12 O20' _chemical_formula_weight 1429.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 18.683(11) _cell_length_b 7.826(5) _cell_length_c 37.85(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5534(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 0.861 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.8817 _exptl_absorpt_correction_T_max 0.9501 _exptl_absorpt_process_details SADABS _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33927 _diffrn_reflns_av_R_equivalents 0.1062 _diffrn_reflns_av_sigmaI/netI 0.1207 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12231 _reflns_number_gt 8100 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1244P)^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 0.52(4) _refine_ls_number_reflns 12231 _refine_ls_number_parameters 812 _refine_ls_number_restraints 2834 _refine_ls_R_factor_all 0.1097 _refine_ls_R_factor_gt 0.0779 _refine_ls_wR_factor_ref 0.2439 _refine_ls_wR_factor_gt 0.1874 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 0.968 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.002 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 0.15243(3) 0.64658(9) 0.391358(19) 0.02899(17) Uani 1 1 d U . . Cd2 Cd 1.09766(4) 0.10192(10) 0.058511(18) 0.02997(18) Uani 1 1 d . . . C1 C 0.0476(6) 0.7471(14) 0.3213(3) 0.032(2) Uani 1 1 d U . . C2 C -0.0215(6) 0.8140(16) 0.3073(3) 0.0339(19) Uani 1 1 d U . . C3 C -0.0842(5) 0.8082(16) 0.3276(3) 0.0317(19) Uani 1 1 d U . . H3B H -0.0824 0.7621 0.3502 0.038 Uiso 1 1 calc R . . C4 C -0.1492(6) 0.8698(14) 0.3147(3) 0.035(2) Uani 1 1 d U . . C5 C -0.2202(6) 0.8562(16) 0.3344(3) 0.038(2) Uani 1 1 d U . . C6 C -0.1525(6) 0.9377(16) 0.2800(3) 0.038(2) Uani 1 1 d U . . H6B H -0.1962 0.9738 0.2708 0.046 Uiso 1 1 calc R . . C7 C -0.0879(6) 0.9514(17) 0.2586(3) 0.042(2) Uani 1 1 d U . . H7B H -0.0883 1.0047 0.2366 0.050 Uiso 1 1 calc R . . C8 C -0.0252(6) 0.8807(14) 0.2726(3) 0.0304(19) Uani 1 1 d U . . C9 C 0.0431(6) 0.8798(15) 0.2517(3) 0.035(2) Uani 1 1 d U . . C10 C 0.5383(7) 0.7626(15) 0.3261(3) 0.034(2) Uani 1 1 d U . . C11 C 0.4683(5) 0.6961(15) 0.3143(2) 0.0290(18) Uani 1 1 d U . . C12 C 0.4074(5) 0.7023(16) 0.3360(3) 0.0336(19) Uani 1 1 d U . . H12A H 0.4108 0.7529 0.3581 0.040 Uiso 1 1 calc R . . C13 C 0.3413(5) 0.6340(14) 0.3251(3) 0.0296(19) Uani 1 1 d U . . C14 C 0.2769(6) 0.6458(15) 0.3486(3) 0.037(2) Uani 1 1 d U . . C15 C 0.3357(5) 0.5654(15) 0.2899(3) 0.0335(19) Uani 1 1 d U . . H15A H 0.2916 0.5294 0.2813 0.040 Uiso 1 1 calc R . . C16 C 0.3953(5) 0.5531(15) 0.2689(3) 0.0315(19) Uani 1 1 d U . . H16A H 0.3916 0.4975 0.2473 0.038 Uiso 1 1 calc R . . C17 C 0.4620(5) 0.6220(14) 0.2791(3) 0.0305(19) Uani 1 1 d U . . C18 C 0.5263(6) 0.6221(15) 0.2576(3) 0.0334(19) Uani 1 1 d U . . C19 C 0.7146(6) 0.0019(14) 0.1253(3) 0.032(2) Uani 1 1 d U . . C20 C 0.7841(5) 0.0672(15) 0.1369(2) 0.0292(18) Uani 1 1 d U . . C21 C 0.8435(5) 0.0604(15) 0.1149(3) 0.0298(18) Uani 1 1 d U . . H21A H 0.8393 0.0191 0.0920 0.036 Uiso 1 1 calc R . . C22 C 0.9115(6) 0.1180(14) 0.1280(3) 0.0321(19) Uani 1 1 d U . . C23 C 0.9770(5) 0.1070(13) 0.1038(3) 0.030(2) Uani 1 1 d U . . C24 C 0.9163(6) 0.1927(15) 0.1614(3) 0.0336(19) Uani 1 1 d U . . H24A H 0.9594 0.2393 0.1690 0.040 Uiso 1 1 calc R . . C25 C 0.8562(5) 0.1975(14) 0.1835(2) 0.0293(17) Uani 1 1 d U . . H25A H 0.8609 0.2379 0.2065 0.035 Uiso 1 1 calc R . . C26 C 0.7898(6) 0.1430(15) 0.1716(3) 0.0327(19) Uani 1 1 d U . . C27 C 0.7252(5) 0.1425(14) 0.1935(2) 0.0294(18) Uani 1 1 d U . . C28 C 0.7037(7) 0.4884(15) 0.1262(4) 0.036(2) Uani 1 1 d U . . C29 C 0.7700(5) 0.5607(15) 0.1409(3) 0.0328(19) Uani 1 1 d U . . C30 C 0.8335(5) 0.5600(15) 0.1183(3) 0.0320(18) Uani 1 1 d U . . H30A H 0.8314 0.5229 0.0950 0.038 Uiso 1 1 calc R . . C31 C 0.8977(5) 0.6175(14) 0.1333(3) 0.032(2) Uani 1 1 d DU . . C32 C 0.9660(5) 0.6081(15) 0.1104(3) 0.036(2) Uani 1 1 d DU . . C33 C 0.8982(6) 0.6864(15) 0.1670(3) 0.035(2) Uani 1 1 d U . . H33A H 0.9409 0.7292 0.1760 0.042 Uiso 1 1 calc R . . C34 C 0.8363(6) 0.6939(15) 0.1882(3) 0.037(2) Uani 1 1 d U . . H34A H 0.8379 0.7383 0.2109 0.044 Uiso 1 1 calc R . . C35 C 0.7712(6) 0.6311(14) 0.1735(3) 0.0333(19) Uani 1 1 d U . . C36 C 0.7062(6) 0.6288(15) 0.1962(3) 0.038(2) Uani 1 1 d U . . C37 C 0.2487(7) 0.7298(16) 0.4632(3) 0.042(2) Uani 1 1 d U . . H37A H 0.2846 0.7469 0.4465 0.051 Uiso 1 1 calc R . . C38 C 0.2636(7) 0.7551(16) 0.4992(3) 0.046(3) Uani 1 1 d U . . H38 H 0.3099 0.7813 0.5065 0.055 Uiso 1 1 calc R . . C39 C 0.2106(7) 0.7410(16) 0.5229(4) 0.045(3) Uani 1 1 d U . . H39A H 0.2197 0.7634 0.5466 0.055 Uiso 1 1 calc R . . C40 C 0.1410(6) 0.6926(17) 0.5122(3) 0.041(2) Uani 1 1 d U . . H40A H 0.1039 0.6847 0.5285 0.050 Uiso 1 1 calc R . . C41 C 0.1295(6) 0.6566(14) 0.4764(3) 0.0336(19) Uani 1 1 d U . . C42 C 0.0591(6) 0.5912(14) 0.4638(3) 0.0334(19) Uani 1 1 d U . . C43 C 0.0020(7) 0.5288(17) 0.4866(3) 0.042(2) Uani 1 1 d U . . H43 H 0.0087 0.5306 0.5109 0.051 Uiso 1 1 calc R . . C44 C -0.0588(6) 0.4698(18) 0.4738(3) 0.047(3) Uani 1 1 d U . . H44 H -0.0943 0.4295 0.4889 0.056 Uiso 1 1 calc R . . C45 C -0.0694(7) 0.4685(17) 0.4367(3) 0.044(2) Uani 1 1 d U . . H45A H -0.1127 0.4352 0.4267 0.053 Uiso 1 1 calc R . . C46 C -0.0118(6) 0.5197(16) 0.4161(3) 0.040(2) Uani 1 1 d U . . H46A H -0.0171 0.5118 0.3917 0.048 Uiso 1 1 calc R . . C47 C 1.2603(6) 0.2252(16) 0.0308(3) 0.039(2) Uani 1 1 d U . . H47A H 1.2679 0.2325 0.0551 0.047 Uiso 1 1 calc R . . C48 C 1.3168(6) 0.2724(16) 0.0087(3) 0.040(2) Uani 1 1 d U . . H48A H 1.3609 0.3080 0.0175 0.049 Uiso 1 1 calc R . . C49 C 1.3026(7) 0.2623(16) -0.0273(3) 0.044(2) Uani 1 1 d U . . H49A H 1.3380 0.2951 -0.0432 0.053 Uiso 1 1 calc R . . C50 C 1.2375(6) 0.2051(17) -0.0403(3) 0.042(2) Uani 1 1 d U . . H50A H 1.2294 0.1958 -0.0645 0.051 Uiso 1 1 calc R . . C51 C 1.1852(6) 0.1621(15) -0.0161(3) 0.036(2) Uani 1 1 d U . . C52 C 1.1129(6) 0.0901(14) -0.0281(3) 0.0341(19) Uani 1 1 d U . . C53 C 1.0969(6) 0.0678(19) -0.0635(3) 0.046(2) Uani 1 1 d U . . H53A H 1.1310 0.0951 -0.0805 0.055 Uiso 1 1 calc R . . C54 C 1.0302(7) 0.0047(17) -0.0740(3) 0.048(3) Uani 1 1 d U . . H54A H 1.0185 -0.0126 -0.0976 0.058 Uiso 1 1 calc R . . C55 C 0.9799(7) -0.0322(17) -0.0454(3) 0.045(2) Uani 1 1 d U . . H55A H 0.9344 -0.0740 -0.0504 0.054 Uiso 1 1 calc R . . C56 C 1.0002(7) -0.0049(16) -0.0118(4) 0.043(2) Uani 1 1 d U . . H56A H 0.9672 -0.0294 0.0059 0.052 Uiso 1 1 calc R . . N1 N 0.1044(5) 0.7574(14) 0.2988(3) 0.040(2) Uani 1 1 d U . . H1A H 0.1449 0.7207 0.3066 0.048 Uiso 1 1 calc R . . N2 N 0.1034(4) 0.8221(15) 0.2643(2) 0.0354(18) Uani 1 1 d U . . N3 N 0.5920(6) 0.7575(13) 0.3022(3) 0.038(2) Uani 1 1 d U . . H3A H 0.6319 0.8042 0.3081 0.045 Uiso 1 1 calc R . . N4 N 0.5883(5) 0.6824(15) 0.2685(2) 0.0370(18) Uani 1 1 d U . . N5 N 0.6637(5) 0.0827(15) 0.1831(2) 0.0392(19) Uani 1 1 d U . . N6 N 0.6581(5) 0.0166(14) 0.1473(3) 0.038(2) Uani 1 1 d U . . H6A H 0.6167 -0.0148 0.1398 0.046 Uiso 1 1 calc R . . N7 N 0.6452(5) 0.5658(16) 0.1833(3) 0.0416(19) Uani 1 1 d U . . N8 N 0.6468(5) 0.4940(14) 0.1495(3) 0.041(2) Uani 1 1 d U . . H8A H 0.6077 0.4476 0.1423 0.050 Uiso 1 1 calc R . . N9 N 0.1806(5) 0.6792(12) 0.4522(2) 0.0311(16) Uani 1 1 d U . . N10 N 0.0503(5) 0.5791(13) 0.4280(2) 0.0330(17) Uani 1 1 d U . . N11 N 1.1968(5) 0.1708(13) 0.0200(2) 0.0331(17) Uani 1 1 d U . . N12 N 1.0646(5) 0.0553(13) -0.0017(2) 0.0373(18) Uani 1 1 d U . . O1 O 0.0522(4) 0.6863(13) 0.3526(2) 0.0439(17) Uani 1 1 d U . . O2 O 0.0381(4) 0.9413(13) 0.2196(2) 0.046(2) Uani 1 1 d U . . H2 H 0.0774 0.9365 0.2099 0.070 Uiso 1 1 calc R . . O3 O -0.2157(5) 0.8088(16) 0.3663(2) 0.063(2) Uani 1 1 d U . . O4 O -0.2762(4) 0.9021(13) 0.3206(3) 0.057(2) Uani 1 1 d U . . O5 O 0.5475(4) 0.8259(11) 0.35719(18) 0.0371(17) Uani 1 1 d U . . O6 O 0.5209(4) 0.5576(13) 0.2248(2) 0.0477(19) Uani 1 1 d U . . H6 H 0.5598 0.5639 0.2149 0.072 Uiso 1 1 calc R . . O7 O 0.2861(4) 0.6715(12) 0.38135(19) 0.0439(18) Uani 1 1 d U . . O8 O 0.2155(4) 0.6135(11) 0.3348(2) 0.0383(16) Uani 1 1 d U . . O9 O 0.7310(4) 0.2055(12) 0.2261(2) 0.0449(19) Uani 1 1 d U . . H9 H 0.6922 0.1991 0.2362 0.067 Uiso 1 1 calc R . . O10 O 0.7029(4) -0.0533(14) 0.0934(2) 0.0462(18) Uani 1 1 d U . . O11 O 1.0390(4) 0.1343(11) 0.1179(2) 0.0437(18) Uani 1 1 d U . . O12 O 0.9695(4) 0.0783(12) 0.07147(18) 0.0405(17) Uani 1 1 d U . . O13 O 0.7079(5) 0.6955(14) 0.2271(2) 0.054(2) Uani 1 1 d U . . H13 H 0.6687 0.6849 0.2365 0.081 Uiso 1 1 calc R . . O14 O 0.6965(4) 0.4223(12) 0.0964(2) 0.0432(19) Uani 1 1 d U . . O15 O 1.0221(5) 0.6631(13) 0.1256(3) 0.055(2) Uani 1 1 d U . . O16 O 0.9623(5) 0.5417(16) 0.0804(3) 0.064(2) Uani 1 1 d U . . O17 O 0.1550(4) 0.9460(11) 0.3867(3) 0.048(2) Uani 1 1 d U . . H17A H 0.1930 1.0020 0.3824 0.057 Uiso 1 1 d R . . H17B H 0.1197 1.0031 0.3789 0.057 Uiso 1 1 d R . . O18 O 0.1620(3) 0.3547(9) 0.3905(3) 0.0316(14) Uani 1 1 d U . . H18A H 0.2003 0.3075 0.3833 0.038 Uiso 1 1 d R . . H18B H 0.1268 0.3042 0.3809 0.038 Uiso 1 1 d R . . O19 O 1.0885(4) 0.4019(9) 0.0573(3) 0.0347(14) Uani 1 1 d U . . H19A H 1.1218 0.4534 0.0683 0.042 Uiso 1 1 d R . . H19B H 1.0487 0.4444 0.0636 0.042 Uiso 1 1 d R . . O20 O 1.0974(4) -0.2018(11) 0.0630(3) 0.046(2) Uani 1 1 d U . . H20A H 1.0561 -0.1631 0.0580 0.055 Uiso 1 1 d R . . H20B H 1.0941 -0.2560 0.0824 0.055 Uiso 1 1 d 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 Cd1 0.0269(3) 0.0366(4) 0.0235(3) 0.0026(3) 0.0015(3) -0.0002(3) Cd2 0.0278(3) 0.0385(4) 0.0236(3) 0.0017(3) 0.0030(3) 0.0016(3) C1 0.026(4) 0.045(4) 0.025(4) 0.001(3) 0.006(3) 0.001(3) C2 0.031(4) 0.042(4) 0.029(4) 0.001(3) 0.000(3) -0.001(3) C3 0.025(4) 0.048(4) 0.022(3) 0.005(3) 0.001(3) -0.003(3) C4 0.032(4) 0.042(4) 0.030(4) -0.005(3) 0.001(4) -0.001(4) C5 0.028(4) 0.052(5) 0.034(4) 0.001(4) 0.004(4) -0.006(4) C6 0.032(4) 0.049(5) 0.033(4) 0.007(4) -0.003(4) 0.004(4) C7 0.035(4) 0.049(5) 0.040(4) 0.009(4) 0.001(4) 0.004(4) C8 0.026(4) 0.046(4) 0.020(3) 0.003(3) 0.008(3) -0.001(3) C9 0.031(4) 0.049(5) 0.024(4) 0.002(3) 0.000(3) 0.001(4) C10 0.030(4) 0.045(5) 0.026(4) 0.003(4) -0.002(4) -0.002(4) C11 0.028(4) 0.040(4) 0.018(3) -0.006(3) 0.003(3) 0.002(3) C12 0.028(4) 0.045(4) 0.027(3) 0.007(3) 0.000(3) 0.001(3) C13 0.028(4) 0.044(4) 0.017(3) 0.005(3) 0.001(3) 0.004(3) C14 0.024(4) 0.047(5) 0.039(4) 0.007(4) -0.002(4) 0.004(4) C15 0.024(4) 0.041(4) 0.035(4) 0.001(3) -0.001(3) -0.002(3) C16 0.031(4) 0.043(4) 0.021(3) 0.005(3) -0.002(3) 0.000(4) C17 0.026(4) 0.043(4) 0.022(3) -0.001(3) 0.000(3) 0.000(3) C18 0.031(4) 0.048(4) 0.022(3) -0.004(3) 0.005(3) -0.007(3) C19 0.031(4) 0.045(4) 0.020(4) -0.006(3) 0.003(3) -0.001(3) C20 0.027(3) 0.042(4) 0.018(3) 0.000(3) 0.000(3) 0.002(3) C21 0.023(3) 0.044(4) 0.022(3) -0.003(3) 0.002(3) 0.005(3) C22 0.028(4) 0.044(4) 0.024(3) 0.001(3) 0.005(3) 0.000(3) C23 0.017(4) 0.038(4) 0.035(4) 0.007(3) 0.009(3) 0.002(3) C24 0.031(4) 0.041(4) 0.029(4) -0.001(3) -0.003(3) 0.001(3) C25 0.029(4) 0.038(4) 0.021(3) -0.004(3) 0.001(3) 0.001(3) C26 0.027(3) 0.043(4) 0.029(4) 0.000(3) 0.005(3) 0.002(3) C27 0.029(4) 0.041(4) 0.018(3) -0.003(3) 0.002(3) -0.004(3) C28 0.029(4) 0.043(4) 0.036(4) -0.003(3) 0.002(4) 0.001(3) C29 0.028(4) 0.037(4) 0.033(4) 0.004(3) 0.002(3) 0.003(3) C30 0.028(4) 0.040(4) 0.028(3) -0.001(3) 0.001(3) 0.003(3) C31 0.025(4) 0.039(4) 0.033(4) 0.003(3) 0.004(3) 0.005(3) C32 0.028(4) 0.047(5) 0.032(4) 0.006(4) 0.005(4) 0.003(4) C33 0.026(4) 0.046(4) 0.033(4) 0.004(4) -0.007(3) -0.002(4) C34 0.036(4) 0.043(4) 0.031(4) -0.003(4) 0.002(3) -0.003(4) C35 0.026(4) 0.041(4) 0.033(4) -0.001(3) 0.002(3) 0.002(3) C36 0.032(4) 0.047(4) 0.034(4) -0.003(3) 0.003(3) 0.001(3) C37 0.041(4) 0.052(5) 0.034(4) 0.004(4) 0.002(4) -0.001(4) C38 0.045(5) 0.054(5) 0.037(5) -0.002(4) -0.014(4) 0.000(4) C39 0.048(5) 0.050(5) 0.038(4) -0.009(4) -0.006(4) 0.001(4) C40 0.043(4) 0.050(5) 0.030(4) -0.001(4) -0.002(4) -0.004(4) C41 0.033(4) 0.038(4) 0.029(4) 0.000(3) -0.002(3) 0.003(3) C42 0.036(4) 0.036(4) 0.028(4) 0.003(3) 0.006(3) 0.000(3) C43 0.045(4) 0.053(5) 0.029(4) -0.003(4) 0.009(4) -0.004(4) C44 0.038(5) 0.053(5) 0.049(5) -0.001(4) 0.015(4) -0.012(4) C45 0.043(5) 0.050(5) 0.040(4) 0.002(4) 0.011(4) -0.014(4) C46 0.039(4) 0.046(5) 0.034(4) -0.004(4) 0.001(4) -0.005(4) C47 0.036(4) 0.050(5) 0.030(4) 0.002(4) 0.004(4) -0.003(4) C48 0.037(4) 0.047(5) 0.037(4) 0.001(4) 0.002(4) -0.005(4) C49 0.043(5) 0.056(5) 0.034(4) 0.010(4) 0.018(4) -0.004(4) C50 0.043(4) 0.052(5) 0.032(4) 0.004(4) 0.009(4) -0.010(4) C51 0.034(4) 0.043(4) 0.032(4) 0.007(3) 0.007(3) 0.004(3) C52 0.037(4) 0.039(4) 0.026(4) 0.002(3) 0.002(3) 0.000(3) C53 0.045(4) 0.055(5) 0.038(4) 0.000(4) -0.001(4) -0.003(4) C54 0.052(5) 0.055(5) 0.038(5) -0.002(4) -0.012(4) -0.001(4) C55 0.044(5) 0.053(5) 0.037(4) -0.004(4) -0.005(4) 0.001(4) C56 0.042(5) 0.047(5) 0.040(4) -0.001(4) 0.001(4) -0.005(4) N1 0.028(4) 0.066(5) 0.026(4) 0.006(4) 0.009(3) 0.011(4) N2 0.022(4) 0.062(5) 0.022(4) 0.007(4) 0.002(3) 0.001(3) N3 0.029(4) 0.055(5) 0.029(4) -0.007(4) 0.006(4) -0.006(3) N4 0.032(4) 0.063(5) 0.016(3) -0.001(3) 0.002(3) 0.003(4) N5 0.032(4) 0.063(5) 0.023(4) -0.008(4) 0.007(3) -0.002(4) N6 0.027(4) 0.065(5) 0.024(4) -0.009(3) -0.002(3) -0.004(4) N7 0.032(4) 0.057(4) 0.036(4) -0.005(4) 0.002(3) -0.001(3) N8 0.032(4) 0.058(5) 0.034(4) -0.007(4) 0.000(4) -0.004(4) N9 0.035(4) 0.041(4) 0.017(3) -0.001(3) -0.004(3) 0.002(3) N10 0.029(4) 0.046(4) 0.024(3) -0.005(3) 0.003(3) 0.002(3) N11 0.027(4) 0.049(4) 0.023(3) -0.002(3) 0.004(3) -0.004(3) N12 0.041(4) 0.046(4) 0.024(3) 0.002(3) 0.004(3) -0.004(4) O1 0.027(3) 0.069(4) 0.036(3) 0.014(3) 0.001(3) 0.006(3) O2 0.029(4) 0.073(5) 0.037(4) 0.020(4) 0.013(3) 0.006(4) O3 0.045(4) 0.107(6) 0.038(4) 0.007(4) 0.007(4) -0.015(4) O4 0.020(3) 0.074(5) 0.075(5) 0.010(4) 0.004(4) 0.001(3) O5 0.032(3) 0.060(5) 0.020(3) -0.010(3) -0.002(3) -0.003(3) O6 0.047(4) 0.068(5) 0.028(3) -0.015(3) 0.010(3) -0.002(4) O7 0.039(3) 0.063(4) 0.029(3) -0.003(3) 0.013(3) -0.002(3) O8 0.030(3) 0.052(4) 0.033(3) 0.012(3) -0.001(3) -0.001(3) O9 0.040(4) 0.068(5) 0.026(3) -0.014(3) 0.005(3) 0.000(4) O10 0.031(3) 0.072(4) 0.036(3) -0.009(3) 0.004(3) -0.003(3) O11 0.028(3) 0.056(4) 0.048(4) 0.007(3) 0.000(3) 0.002(3) O12 0.042(3) 0.058(4) 0.021(3) -0.003(3) 0.017(3) 0.001(3) O13 0.045(4) 0.079(5) 0.039(4) -0.017(4) 0.007(4) -0.006(4) O14 0.034(4) 0.061(5) 0.035(4) -0.006(3) 0.004(3) -0.001(3) O15 0.036(4) 0.065(5) 0.063(5) -0.001(4) 0.002(4) 0.000(4) O16 0.041(4) 0.090(6) 0.061(5) -0.008(4) 0.007(4) 0.009(4) O17 0.040(4) 0.044(4) 0.058(5) 0.008(4) 0.006(3) 0.000(3) O18 0.031(3) 0.040(3) 0.024(3) -0.005(3) 0.005(3) 0.001(3) O19 0.037(3) 0.041(4) 0.026(3) -0.008(3) -0.006(3) 0.005(3) O20 0.036(4) 0.047(4) 0.054(5) 0.012(4) 0.007(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O18 2.292(7) . ? Cd1 O17 2.350(9) . ? Cd1 N9 2.378(8) . ? Cd1 O1 2.400(8) . ? Cd1 N10 2.418(8) . ? Cd1 O8 2.456(8) . ? Cd1 O7 2.534(8) . ? Cd2 O19 2.354(8) . ? Cd2 O20 2.383(9) . ? Cd2 N12 2.391(9) . ? Cd2 O10 2.399(8) 3 ? Cd2 N11 2.418(8) . ? Cd2 O12 2.452(8) . ? Cd2 O11 2.514(9) . ? C1 O1 1.279(15) . ? C1 N1 1.363(15) . ? C1 C2 1.490(17) . ? C2 C3 1.400(14) . ? C2 C8 1.416(14) . ? C3 C4 1.396(15) . ? C4 C6 1.417(15) . ? C4 C5 1.527(15) . ? C5 O4 1.223(14) . ? C5 O3 1.266(14) . ? C6 C7 1.459(15) . ? C7 C8 1.400(16) . ? C8 C9 1.503(14) . ? C9 N2 1.304(14) . ? C9 O2 1.309(13) . ? C10 O5 1.289(15) . ? C10 N3 1.351(16) . ? C10 C11 1.476(16) . ? C11 C12 1.402(14) . ? C11 C17 1.460(13) . ? C12 C13 1.408(15) . ? C13 C15 1.440(14) . ? C13 C14 1.499(15) . ? C14 O7 1.268(14) . ? C14 O8 1.285(13) . ? C15 C16 1.370(14) . ? C16 C17 1.412(14) . ? C17 C18 1.449(14) . ? C18 N4 1.317(14) . ? C18 O6 1.346(12) . ? C19 O10 1.303(14) . ? C19 N6 1.349(15) . ? C19 C20 1.462(16) . ? C20 C21 1.387(13) . ? C20 C26 1.446(14) . ? C21 C22 1.438(14) . ? C22 C24 1.395(15) . ? C22 C23 1.530(14) . ? C23 O12 1.253(13) . ? C23 O11 1.293(13) . ? C24 C25 1.399(14) . ? C25 C26 1.387(15) . ? C26 C27 1.465(14) . ? C27 N5 1.302(14) . ? C27 O9 1.336(12) . ? C28 O14 1.247(16) . ? C28 N8 1.383(17) . ? C28 C29 1.472(17) . ? C29 C35 1.353(15) . ? C29 C30 1.461(14) . ? C30 C31 1.400(15) . ? C31 C33 1.385(15) . ? C31 C32 1.546(12) . ? C32 O16 1.248(15) . ? C32 O15 1.271(14) . ? C33 C34 1.407(15) . ? C34 C35 1.424(15) . ? C35 C36 1.488(15) . ? C36 O13 1.281(14) . ? C36 N7 1.334(15) . ? C37 N9 1.395(16) . ? C37 C38 1.407(18) . ? C38 C39 1.342(18) . ? C39 C40 1.413(17) . ? C40 C41 1.403(15) . ? C41 N9 1.333(14) . ? C41 C42 1.490(16) . ? C42 N10 1.366(13) . ? C42 C43 1.456(16) . ? C43 C44 1.319(17) . ? C44 C45 1.418(17) . ? C45 C46 1.389(16) . ? C46 N10 1.329(14) . ? C47 N11 1.327(15) . ? C47 C48 1.397(16) . ? C48 C49 1.391(17) . ? C49 C50 1.386(17) . ? C50 C51 1.382(15) . ? C51 N11 1.384(14) . ? C51 C52 1.532(17) . ? C52 N12 1.373(14) . ? C52 C53 1.382(16) . ? C53 C54 1.400(18) . ? C54 C55 1.463(18) . ? C55 C56 1.344(17) . ? C56 N12 1.348(16) . ? N1 N2 1.404(14) . ? N3 N4 1.406(14) . ? N5 N6 1.452(14) . ? N7 N8 1.398(15) . ? O10 Cd2 2.399(8) 3_455 ? 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 O18 Cd1 O17 172.4(3) . . ? O18 Cd1 N9 96.0(3) . . ? O17 Cd1 N9 87.8(4) . . ? O18 Cd1 O1 100.4(3) . . ? O17 Cd1 O1 80.9(3) . . ? N9 Cd1 O1 138.7(3) . . ? O18 Cd1 N10 81.5(3) . . ? O17 Cd1 N10 106.1(3) . . ? N9 Cd1 N10 69.0(3) . . ? O1 Cd1 N10 76.3(3) . . ? O18 Cd1 O8 81.1(3) . . ? O17 Cd1 O8 91.7(3) . . ? N9 Cd1 O8 138.5(3) . . ? O1 Cd1 O8 81.7(3) . . ? N10 Cd1 O8 148.8(3) . . ? O18 Cd1 O7 89.9(3) . . ? O17 Cd1 O7 83.8(3) . . ? N9 Cd1 O7 85.3(3) . . ? O1 Cd1 O7 131.9(3) . . ? N10 Cd1 O7 151.7(3) . . ? O8 Cd1 O7 53.5(2) . . ? O19 Cd2 O20 174.8(3) . . ? O19 Cd2 N12 96.6(3) . . ? O20 Cd2 N12 85.1(4) . . ? O19 Cd2 O10 103.2(3) . 3 ? O20 Cd2 O10 78.7(3) . 3 ? N12 Cd2 O10 135.4(3) . 3 ? O19 Cd2 N11 79.7(3) . . ? O20 Cd2 N11 105.5(3) . . ? N12 Cd2 N11 69.9(3) . . ? O10 Cd2 N11 74.9(3) 3 . ? O19 Cd2 O12 90.5(3) . . ? O20 Cd2 O12 84.7(3) . . ? N12 Cd2 O12 85.8(3) . . ? O10 Cd2 O12 132.8(3) 3 . ? N11 Cd2 O12 152.3(3) . . ? O19 Cd2 O11 83.4(3) . . ? O20 Cd2 O11 92.1(3) . . ? N12 Cd2 O11 139.1(3) . . ? O10 Cd2 O11 83.2(3) 3 . ? N11 Cd2 O11 148.3(3) . . ? O12 Cd2 O11 53.3(2) . . ? O1 C1 N1 123.2(11) . . ? O1 C1 C2 121.2(10) . . ? N1 C1 C2 115.6(10) . . ? C3 C2 C8 118.6(10) . . ? C3 C2 C1 121.2(9) . . ? C8 C2 C1 120.1(10) . . ? C4 C3 C2 121.6(9) . . ? C3 C4 C6 119.5(10) . . ? C3 C4 C5 124.1(10) . . ? C6 C4 C5 116.2(10) . . ? O4 C5 O3 123.4(11) . . ? O4 C5 C4 120.9(10) . . ? O3 C5 C4 115.4(10) . . ? C4 C6 C7 120.4(10) . . ? C8 C7 C6 116.9(10) . . ? C7 C8 C2 122.7(10) . . ? C7 C8 C9 120.8(9) . . ? C2 C8 C9 116.5(10) . . ? N2 C9 O2 121.8(10) . . ? N2 C9 C8 122.9(9) . . ? O2 C9 C8 115.3(9) . . ? O5 C10 N3 121.7(11) . . ? O5 C10 C11 121.9(11) . . ? N3 C10 C11 116.4(11) . . ? C12 C11 C17 118.8(9) . . ? C12 C11 C10 122.1(9) . . ? C17 C11 C10 119.1(9) . . ? C11 C12 C13 121.9(10) . . ? C12 C13 C15 118.4(9) . . ? C12 C13 C14 120.5(9) . . ? C15 C13 C14 121.0(9) . . ? O7 C14 O8 123.3(10) . . ? O7 C14 C13 118.8(9) . . ? O8 C14 C13 117.6(10) . . ? C16 C15 C13 120.3(9) . . ? C15 C16 C17 122.2(10) . . ? C16 C17 C18 125.4(9) . . ? C16 C17 C11 118.2(9) . . ? C18 C17 C11 116.5(9) . . ? N4 C18 O6 119.2(9) . . ? N4 C18 C17 123.6(9) . . ? O6 C18 C17 117.1(9) . . ? O10 C19 N6 118.1(11) . . ? O10 C19 C20 122.8(10) . . ? N6 C19 C20 118.7(10) . . ? C21 C20 C26 120.0(10) . . ? C21 C20 C19 121.2(9) . . ? C26 C20 C19 118.8(9) . . ? C20 C21 C22 119.3(9) . . ? C24 C22 C21 120.0(9) . . ? C24 C22 C23 121.0(9) . . ? C21 C22 C23 118.8(9) . . ? O12 C23 O11 122.2(9) . . ? O12 C23 C22 120.4(9) . . ? O11 C23 C22 117.4(10) . . ? C22 C24 C25 120.1(10) . . ? C26 C25 C24 121.0(9) . . ? C25 C26 C20 119.2(9) . . ? C25 C26 C27 123.6(9) . . ? C20 C26 C27 116.9(9) . . ? N5 C27 O9 119.0(9) . . ? N5 C27 C26 123.9(9) . . ? O9 C27 C26 117.1(9) . . ? O14 C28 N8 120.5(12) . . ? O14 C28 C29 126.3(11) . . ? N8 C28 C29 113.1(11) . . ? C35 C29 C30 121.5(10) . . ? C35 C29 C28 121.1(10) . . ? C30 C29 C28 117.4(10) . . ? C31 C30 C29 117.2(9) . . ? C33 C31 C30 120.3(9) . . ? C33 C31 C32 122.1(10) . . ? C30 C31 C32 117.6(9) . . ? O16 C32 O15 126.7(10) . . ? O16 C32 C31 119.0(10) . . ? O15 C32 C31 114.2(10) . . ? C31 C33 C34 122.3(10) . . ? C33 C34 C35 117.8(10) . . ? C29 C35 C34 120.6(10) . . ? C29 C35 C36 120.6(10) . . ? C34 C35 C36 118.5(10) . . ? O13 C36 N7 120.4(10) . . ? O13 C36 C35 120.1(10) . . ? N7 C36 C35 119.4(10) . . ? N9 C37 C38 120.5(12) . . ? C39 C38 C37 119.4(12) . . ? C38 C39 C40 120.6(12) . . ? C41 C40 C39 118.2(11) . . ? N9 C41 C40 121.8(10) . . ? N9 C41 C42 117.3(9) . . ? C40 C41 C42 120.9(10) . . ? N10 C42 C43 118.4(10) . . ? N10 C42 C41 116.5(9) . . ? C43 C42 C41 124.9(10) . . ? C44 C43 C42 122.0(11) . . ? C43 C44 C45 119.1(11) . . ? C46 C45 C44 116.4(12) . . ? N10 C46 C45 126.0(11) . . ? N11 C47 C48 125.2(11) . . ? C49 C48 C47 115.3(11) . . ? C50 C49 C48 122.3(11) . . ? C51 C50 C49 117.6(11) . . ? C50 C51 N11 122.1(11) . . ? C50 C51 C52 121.0(10) . . ? N11 C51 C52 116.7(9) . . ? N12 C52 C53 122.5(11) . . ? N12 C52 C51 115.8(9) . . ? C53 C52 C51 121.7(10) . . ? C52 C53 C54 120.9(12) . . ? C53 C54 C55 115.5(12) . . ? C56 C55 C54 119.2(12) . . ? C55 C56 N12 125.1(12) . . ? C1 N1 N2 126.3(10) . . ? C9 N2 N1 118.5(9) . . ? C10 N3 N4 125.7(10) . . ? C18 N4 N3 118.4(9) . . ? C27 N5 N6 118.2(9) . . ? C19 N6 N5 123.3(10) . . ? C36 N7 N8 117.7(9) . . ? C28 N8 N7 127.9(11) . . ? C41 N9 C37 119.2(9) . . ? C41 N9 Cd1 119.4(7) . . ? C37 N9 Cd1 121.3(7) . . ? C46 N10 C42 117.8(9) . . ? C46 N10 Cd1 124.7(7) . . ? C42 N10 Cd1 117.3(7) . . ? C47 N11 C51 117.4(9) . . ? C47 N11 Cd2 124.8(7) . . ? C51 N11 Cd2 117.7(7) . . ? C56 N12 C52 116.8(10) . . ? C56 N12 Cd2 123.6(8) . . ? C52 N12 Cd2 119.6(7) . . ? C1 O1 Cd1 131.8(8) . . ? C14 O7 Cd1 90.0(7) . . ? C14 O8 Cd1 93.1(7) . . ? C19 O10 Cd2 134.4(7) . 3_455 ? C23 O11 Cd2 90.3(6) . . ? C23 O12 Cd2 94.2(6) . . ? 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 O13 H13 N4 0.82 1.93 2.730(12) 166.1 . N1 H1A O8 0.86 1.89 2.726(13) 162.3 . O6 H6 N7 0.82 1.99 2.803(12) 169.9 . O19 H19B O16 0.85 1.89 2.744(12) 176.7 . O2 H2 N5 0.82 1.91 2.729(12) 174.0 3_465 O18 H18B O5 0.85 2.01 2.856(11) 176.6 3_465 N8 H8A O15 0.86 1.93 2.786(14) 177.8 3_465 O18 H18A O3 0.85 1.93 2.775(12) 177.1 3_565 O9 H9 N2 0.82 1.98 2.795(11) 174.7 3_565 O19 H19A O14 0.85 2.01 2.856(12) 177.0 3_565 O17 H17A O3 0.85 2.34 3.181(14) 170.2 3_575 O17 H17B O5 0.85 2.07 2.910(12) 169.6 3_475 N3 H3A O4 0.86 1.94 2.799(14) 177.8 1_655 N6 H6A O11 0.86 1.92 2.754(13) 164.6 3_455 O20 H20B O15 0.85 2.21 2.951(14) 145.8 1_545 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.012 _refine_diff_density_min -2.188 _refine_diff_density_rms 0.312 # Attachment '- 3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 802480' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H12 N5 O7 Zn' _chemical_formula_weight 379.62 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.4252(16) _cell_length_b 20.219(3) _cell_length_c 7.0187(12) _cell_angle_alpha 90.00 _cell_angle_beta 108.742(2) _cell_angle_gamma 90.00 _cell_volume 1266.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.991 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 1.992 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6914 _exptl_absorpt_correction_T_max 0.9246 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7233 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 26.92 _reflns_number_total 2739 _reflns_number_gt 1863 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^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 2739 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1016 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.963 _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 0.77013(5) 0.98878(2) 0.55455(7) 0.02800(16) Uani 1 1 d . . . C1 C 0.8819(4) 0.86439(16) 0.5831(5) 0.0197(8) Uani 1 1 d . . . C2 C 0.9716(4) 0.80526(16) 0.6574(5) 0.0194(8) Uani 1 1 d . . . C3 C 0.9067(4) 0.74305(16) 0.5894(5) 0.0178(7) Uani 1 1 d . . . C4 C 0.7557(4) 0.74092(17) 0.4416(5) 0.0213(8) Uani 1 1 d . . . C5 C 1.2135(4) 0.62693(16) 0.8713(5) 0.0210(8) Uani 1 1 d . . . C6 C 1.1281(4) 0.68748(16) 0.7973(5) 0.0185(7) Uani 1 1 d . . . C7 C 1.1927(4) 0.74946(16) 0.8662(5) 0.0168(7) Uani 1 1 d . . . C8 C 1.3421(4) 0.75067(17) 1.0175(5) 0.0208(8) Uani 1 1 d . . . C9 C 0.9853(4) 0.68465(16) 0.6604(5) 0.0196(8) Uani 1 1 d . . . H9 H 0.9415 0.6439 0.6154 0.024 Uiso 1 1 calc R . . C10 C 1.1142(4) 0.80742(16) 0.7976(5) 0.0202(8) Uani 1 1 d . . . H10 H 1.1573 0.8480 0.8459 0.024 Uiso 1 1 calc R . . N1 N 0.7479(3) 0.86132(13) 0.4521(4) 0.0236(7) Uani 1 1 d . . . N2 N 0.6914(3) 0.79943(13) 0.3873(4) 0.0247(7) Uani 1 1 d . . . H2 H 0.6030 0.7986 0.3004 0.030 Uiso 1 1 calc R . . N3 N 1.3468(3) 0.62912(14) 1.0095(4) 0.0241(7) Uani 1 1 d . . . N4 N 1.4028(3) 0.69144(14) 1.0757(4) 0.0238(7) Uani 1 1 d . . . H4 H 1.4890 0.6919 1.1676 0.029 Uiso 1 1 calc R . . N5 N 0.5424(3) 0.97881(13) 0.4552(4) 0.0238(7) Uani 1 1 d . . . H5A H 0.5099 0.9859 0.3215 0.029 Uiso 1 1 calc R . . H5B H 0.5206 0.9366 0.4752 0.029 Uiso 1 1 calc R . . O1 O 0.9333(3) 0.92301(11) 0.6496(4) 0.0245(6) Uani 1 1 d . . . O2 O 0.6911(3) 0.68820(12) 0.3705(4) 0.0292(6) Uani 1 1 d . . . O3 O 1.1550(3) 0.57057(11) 0.8014(4) 0.0303(6) Uani 1 1 d . . . O4 O 1.4076(3) 0.80281(11) 1.0938(4) 0.0292(6) Uani 1 1 d . . . O1W O 0.8012(3) 1.01295(12) 0.2793(4) 0.0317(6) Uani 1 1 d . . . H1WB H 0.8675 1.0403 0.2709 0.038 Uiso 1 1 d R . . H1WA H 0.7281 1.0303 0.1885 0.038 Uiso 1 1 d R . . O2W O 0.4384(3) 0.93109(13) 0.9985(4) 0.0393(7) Uani 1 1 d . . . H2WA H 0.4246 0.8916 1.0301 0.047 Uiso 1 1 d R . . H2WB H 0.5191 0.9316 0.9691 0.047 Uiso 1 1 d R . . O3W O 0.7052(3) 0.94610(13) 0.8683(4) 0.0421(8) Uani 1 1 d . . . H3WA H 0.7612 0.9607 0.9809 0.050 Uiso 1 1 d R . . H3WB H 0.7137 0.9048 0.8950 0.050 Uiso 1 1 d 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 Zn1 0.0143(2) 0.0192(2) 0.0442(3) -0.0028(2) 0.00071(19) 0.00139(18) C1 0.0167(18) 0.0194(17) 0.0226(19) 0.0038(14) 0.0057(15) 0.0041(14) C2 0.0171(18) 0.0193(17) 0.021(2) 0.0025(14) 0.0045(15) 0.0019(14) C3 0.0134(17) 0.0195(17) 0.0176(18) -0.0011(14) 0.0008(15) 0.0004(14) C4 0.0124(18) 0.0261(18) 0.022(2) -0.0009(16) 0.0010(15) 0.0010(15) C5 0.0204(19) 0.0206(18) 0.0195(19) 0.0003(14) 0.0029(16) 0.0025(15) C6 0.0149(17) 0.0184(17) 0.020(2) 0.0026(14) 0.0022(15) 0.0008(14) C7 0.0126(17) 0.0208(17) 0.0153(18) -0.0009(13) 0.0022(14) -0.0004(14) C8 0.0138(17) 0.0266(19) 0.021(2) 0.0038(15) 0.0046(15) 0.0005(15) C9 0.0166(18) 0.0195(17) 0.020(2) -0.0031(14) 0.0023(15) 0.0005(14) C10 0.0184(18) 0.0181(17) 0.022(2) -0.0006(14) 0.0033(16) -0.0002(14) N1 0.0156(16) 0.0169(14) 0.0325(18) 0.0014(13) -0.0003(14) 0.0029(12) N2 0.0150(15) 0.0235(16) 0.0268(18) -0.0014(13) -0.0055(13) 0.0013(12) N3 0.0131(15) 0.0206(15) 0.0318(18) -0.0012(13) -0.0021(13) 0.0008(12) N4 0.0140(15) 0.0244(16) 0.0245(17) -0.0002(13) -0.0058(13) -0.0014(13) N5 0.0166(15) 0.0202(15) 0.0325(18) -0.0002(13) 0.0049(13) 0.0017(12) O1 0.0149(13) 0.0188(12) 0.0350(16) -0.0016(11) 0.0013(11) -0.0005(10) O2 0.0203(14) 0.0232(13) 0.0332(16) -0.0014(11) -0.0063(12) 0.0016(11) O3 0.0252(14) 0.0165(12) 0.0371(16) -0.0002(11) -0.0070(12) 0.0002(11) O4 0.0203(14) 0.0207(13) 0.0360(16) -0.0013(11) -0.0059(12) -0.0021(11) O1W 0.0183(13) 0.0316(14) 0.0408(17) 0.0052(12) 0.0031(12) -0.0025(11) O2W 0.0325(16) 0.0309(15) 0.0492(19) 0.0072(13) 0.0056(14) -0.0003(13) O3W 0.0404(18) 0.0257(14) 0.0467(19) -0.0046(13) -0.0049(15) 0.0036(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.948(2) 2_756 ? Zn1 O1 1.980(2) . ? Zn1 N5 2.042(3) . ? Zn1 O1W 2.103(3) . ? C1 N1 1.303(4) . ? C1 O1 1.309(4) . ? C1 C2 1.461(4) . ? C2 C10 1.388(5) . ? C2 C3 1.413(4) . ? C3 C9 1.398(4) . ? C3 C4 1.468(4) . ? C4 O2 1.249(4) . ? C4 N2 1.328(4) . ? C5 O3 1.292(4) . ? C5 N3 1.318(4) . ? C5 C6 1.466(4) . ? C6 C9 1.381(5) . ? C6 C7 1.409(4) . ? C7 C10 1.387(4) . ? C7 C8 1.467(5) . ? C8 O4 1.252(4) . ? C8 N4 1.333(4) . ? N1 N2 1.379(4) . ? N3 N4 1.387(4) . ? N5 N5 1.446(5) 3_676 ? O3 Zn1 1.948(2) 2_746 ? 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 O1 106.41(10) 2_756 . ? O3 Zn1 N5 115.25(11) 2_756 . ? O1 Zn1 N5 131.76(10) . . ? O3 Zn1 O1W 98.36(10) 2_756 . ? O1 Zn1 O1W 98.26(10) . . ? N5 Zn1 O1W 98.65(11) . . ? N1 C1 O1 117.3(3) . . ? N1 C1 C2 122.1(3) . . ? O1 C1 C2 120.6(3) . . ? C10 C2 C3 118.9(3) . . ? C10 C2 C1 123.0(3) . . ? C3 C2 C1 118.0(3) . . ? C9 C3 C2 120.6(3) . . ? C9 C3 C4 120.6(3) . . ? C2 C3 C4 118.7(3) . . ? O2 C4 N2 121.8(3) . . ? O2 C4 C3 123.0(3) . . ? N2 C4 C3 115.2(3) . . ? O3 C5 N3 119.9(3) . . ? O3 C5 C6 118.9(3) . . ? N3 C5 C6 121.2(3) . . ? C9 C6 C7 119.5(3) . . ? C9 C6 C5 120.9(3) . . ? C7 C6 C5 119.6(3) . . ? C10 C7 C6 120.6(3) . . ? C10 C7 C8 121.2(3) . . ? C6 C7 C8 118.2(3) . . ? O4 C8 N4 121.4(3) . . ? O4 C8 C7 123.4(3) . . ? N4 C8 C7 115.1(3) . . ? C6 C9 C3 120.0(3) . . ? C7 C10 C2 120.4(3) . . ? C1 N1 N2 117.4(3) . . ? C4 N2 N1 128.4(3) . . ? C5 N3 N4 116.5(3) . . ? C8 N4 N3 129.3(3) . . ? N5 N5 Zn1 117.4(3) 3_676 . ? C1 O1 Zn1 109.3(2) . . ? C5 O3 Zn1 120.8(2) . 2_746 ? 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 O2W H2WB O3W 0.85 2.11 2.954(4) 170.9 . O2W H2WA O4 0.85 1.87 2.717(3) 175.4 1_455 O3W H3WB O2 0.85 1.89 2.719(3) 162.0 4_576 O1W H1WB O1 0.85 1.93 2.718(3) 154.1 3_776 O3W H3WA O1W 0.85 2.27 3.048(4) 152.9 1_556 N5 H5B N3 0.90 2.18 2.959(4) 144.3 4_475 O1W H1WA O2W 0.85 1.86 2.711(4) 176.3 3_676 N5 H5A O3W 0.90 2.46 3.082(4) 126.8 3_676 N5 H5A O2W 0.90 2.42 3.186(4) 143.5 1_554 N4 H4 O2 0.86 1.98 2.838(4) 176.3 1_656 N2 H2 O4 0.86 1.95 2.804(4) 175.5 1_454 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.92 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.408 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.097