# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 918381' #TrackingRef 'Combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H26 Ce N O10' _chemical_formula_sum 'C27 H26 Ce N O10' _chemical_formula_weight 664.61 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' Ce Ce -0.2486 2.6331 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 13.7661(5) _cell_length_b 24.6948(11) _cell_length_c 8.3773(10) _cell_angle_alpha 90.000 _cell_angle_beta 105.686(5) _cell_angle_gamma 90.000 _cell_volume 2741.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4120 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.35 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 1.717 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6268 _exptl_absorpt_correction_T_max 0.8470 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f & \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8843 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.32 _reflns_number_total 2508 _reflns_number_gt 2189 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _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. The DMA molecule coordinated to the metal site resides on, and is disordered about the mirror plane. ; _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^)+(0.0422P)^2^+3.4534P] 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 2508 _refine_ls_number_parameters 193 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0856 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 Ce1 Ce 0.13679(2) 0.5000 0.34471(4) 0.02592(13) Uani 1 2 d S . . O2 O 0.0662(2) 0.42400(10) 0.4487(4) 0.0368(7) Uani 1 1 d . . . C3 C 0.0000 0.4003(2) 0.5000 0.0259(12) Uani 1 2 d S . . C4 C 0.0000 0.3392(2) 0.5000 0.0230(11) Uani 1 2 d S . . C5 C 0.0533(3) 0.31201(14) 0.4059(4) 0.0237(8) Uani 1 1 d . . . H5 H 0.0901 0.3314 0.3436 0.028 Uiso 1 1 calc R . . C6 C 0.0517(3) 0.25561(14) 0.4049(5) 0.0243(8) Uani 1 1 d . . . C7 C 0.0000 0.2276(2) 0.5000 0.0245(11) Uani 1 2 d S . . H7 H 0.0000 0.1892 0.5000 0.029 Uiso 1 2 calc SR . . O8 O 0.0996(2) 0.22385(10) 0.3151(3) 0.0280(6) Uani 1 1 d . . . C9 C 0.1514(3) 0.25100(15) 0.2095(5) 0.0303(9) Uani 1 1 d . . . H9A H 0.2090 0.2722 0.2771 0.036 Uiso 1 1 calc R . . H9B H 0.1049 0.2761 0.1332 0.036 Uiso 1 1 calc R . . C10 C 0.1881(3) 0.20818(15) 0.1130(5) 0.0282(9) Uani 1 1 d . . . C11 C 0.1277(3) 0.19124(16) -0.0404(5) 0.0327(9) Uani 1 1 d . . . H11 H 0.0636 0.2075 -0.0853 0.039 Uiso 1 1 calc R . . C12 C 0.1607(3) 0.15079(17) -0.1280(5) 0.0329(9) Uani 1 1 d . . . H12 H 0.1190 0.1395 -0.2326 0.039 Uiso 1 1 calc R . . C13 C 0.2540(3) 0.12663(15) -0.0643(5) 0.0275(8) Uani 1 1 d . . . C14 C 0.3151(3) 0.14412(16) 0.0885(5) 0.0338(9) Uani 1 1 d . . . H14 H 0.3796 0.1283 0.1334 0.041 Uiso 1 1 calc R . . C15 C 0.2811(3) 0.18472(17) 0.1744(5) 0.0361(10) Uani 1 1 d . . . H15 H 0.3231 0.1965 0.2780 0.043 Uiso 1 1 calc R . . C16 C 0.2891(3) 0.08285(16) -0.1595(5) 0.0309(9) Uani 1 1 d . . . O17 O 0.2326(2) 0.06706(12) -0.2958(4) 0.0400(7) Uani 1 1 d . . . O18 O 0.3767(2) 0.06342(12) -0.1010(4) 0.0420(7) Uani 1 1 d . . . O19 O -0.0435(3) 0.5000 0.1780(5) 0.0383(10) Uani 1 2 d S . . H19 H -0.0688 0.5260 0.1114 0.046 Uiso 0.50 1 d PR . . O20 O 0.2629(3) 0.5000 0.6103(5) 0.0389(10) Uani 1 2 d S . . C21 C 0.3532(8) 0.5172(3) 0.6731(11) 0.041(2) Uani 0.50 1 d P . . H21 H 0.3667 0.5550 0.6827 0.049 Uiso 0.50 1 d PR . . N22 N 0.4261(7) 0.4809(3) 0.7244(11) 0.051(2) Uani 0.50 1 d P . . C23 C 0.3887(5) 0.4224(2) 0.6996(8) 0.0746(18) Uani 0.50 1 d P . . H23A H 0.3867 0.4078 0.8075 0.112 Uiso 0.50 1 d PR . . H23B H 0.4342 0.4004 0.6543 0.112 Uiso 0.50 1 d PR . . H23C H 0.3208 0.4216 0.6234 0.112 Uiso 0.50 1 d PR . . C24 C 0.5320(6) 0.5000 0.7864(13) 0.089(3) Uani 1 2 d S . . H24A H 0.5347 0.5395 0.7774 0.134 Uiso 0.50 1 d PR . . H24B H 0.5739 0.4834 0.7218 0.134 Uiso 0.50 1 d PR . . H24C H 0.5574 0.4893 0.9029 0.134 Uiso 0.50 1 d PR . . C25 C 0.3887(5) 0.4224(2) 0.6996(8) 0.0746(18) Uani 0.50 1 d P . . H25A H 0.3867 0.4078 0.8075 0.112 Uiso 0.50 1 d PR . . H25B H 0.4342 0.4004 0.6543 0.112 Uiso 0.50 1 d PR . . H25C H 0.3208 0.4216 0.6234 0.112 Uiso 0.50 1 d PR . . 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 Ce1 0.0251(2) 0.02428(18) 0.0311(2) 0.000 0.01228(13) 0.000 O2 0.0392(18) 0.0219(13) 0.0558(19) 0.0028(12) 0.0240(15) -0.0031(12) C3 0.029(3) 0.022(3) 0.028(3) 0.000 0.011(2) 0.000 C4 0.024(3) 0.023(3) 0.023(3) 0.000 0.007(2) 0.000 C5 0.022(2) 0.0243(19) 0.0254(18) 0.0017(15) 0.0076(15) -0.0030(15) C6 0.023(2) 0.0253(19) 0.0253(19) -0.0024(15) 0.0079(16) 0.0036(15) C7 0.030(3) 0.019(2) 0.025(3) 0.000 0.007(2) 0.000 O8 0.0368(16) 0.0224(13) 0.0306(14) -0.0017(11) 0.0187(12) 0.0005(11) C9 0.034(2) 0.027(2) 0.036(2) -0.0011(16) 0.0193(18) 0.0005(17) C10 0.031(2) 0.0259(19) 0.032(2) 0.0024(15) 0.0168(18) 0.0022(16) C11 0.025(2) 0.038(2) 0.037(2) 0.0001(18) 0.0110(18) 0.0094(18) C12 0.033(2) 0.037(2) 0.031(2) -0.0025(17) 0.0127(18) 0.0028(18) C13 0.027(2) 0.0287(19) 0.029(2) -0.0006(16) 0.0115(17) 0.0028(16) C14 0.029(2) 0.037(2) 0.034(2) -0.0014(18) 0.0054(18) 0.0099(18) C15 0.037(3) 0.037(2) 0.031(2) -0.0072(17) 0.0031(19) 0.0040(19) C16 0.031(2) 0.031(2) 0.032(2) 0.0012(17) 0.0114(18) 0.0028(18) O17 0.0295(17) 0.0468(18) 0.0408(17) -0.0147(14) 0.0045(14) 0.0084(13) O18 0.0346(18) 0.0488(18) 0.0397(17) -0.0079(14) 0.0050(14) 0.0181(14) O19 0.037(3) 0.038(2) 0.040(2) 0.000 0.0100(19) 0.000 O20 0.034(3) 0.048(2) 0.033(2) 0.000 0.006(2) 0.000 C21 0.052(7) 0.027(5) 0.045(5) -0.004(3) 0.015(5) -0.004(4) N22 0.032(5) 0.047(5) 0.069(6) -0.005(3) 0.007(4) 0.004(3) C23 0.091(5) 0.033(3) 0.096(4) 0.011(3) 0.018(4) 0.013(3) C24 0.031(5) 0.128(9) 0.104(8) 0.000 0.009(5) 0.000 C25 0.091(5) 0.033(3) 0.096(4) 0.011(3) 0.018(4) 0.013(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 Ce1 O2 2.384(3) 6_565 ? Ce1 O2 2.384(3) . ? Ce1 O20 2.424(4) . ? Ce1 O19 2.498(4) . ? Ce1 O18 2.540(3) 7 ? Ce1 O18 2.540(3) 4 ? Ce1 O17 2.557(3) 7 ? Ce1 O17 2.557(3) 4 ? Ce1 C16 2.914(4) 7 ? Ce1 C16 2.914(4) 4 ? O2 C3 1.253(3) . ? C3 O2 1.253(3) 2_556 ? C3 C4 1.510(7) . ? C4 C5 1.386(4) . ? C4 C5 1.386(4) 2_556 ? C5 C6 1.393(5) . ? C5 H5 0.9500 . ? C6 O8 1.373(4) . ? C6 C7 1.387(4) . ? C7 C6 1.387(4) 2_556 ? C7 H7 0.9500 . ? O8 C9 1.443(4) . ? C9 C10 1.499(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C15 1.373(6) . ? C10 C11 1.393(6) . ? C11 C12 1.387(5) . ? C11 H11 0.9500 . ? C12 C13 1.386(6) . ? C12 H12 0.9500 . ? C13 C14 1.396(6) . ? C13 C16 1.499(5) . ? C14 C15 1.387(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 O17 1.257(5) . ? C16 O18 1.267(5) . ? C16 Ce1 2.914(4) 7 ? O17 Ce1 2.557(3) 7 ? O18 Ce1 2.540(3) 7 ? O19 H19 0.8596 . ? O20 C21 1.284(11) . ? O20 C21 1.284(11) 6_565 ? C21 N22 1.326(11) . ? C21 H21 0.9500 . ? N22 C24 1.486(12) . ? N22 C23 1.529(9) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? 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 Ce1 O2 103.86(13) 6_565 . ? O2 Ce1 O20 85.76(10) 6_565 . ? O2 Ce1 O20 85.76(10) . . ? O2 Ce1 O19 76.27(9) 6_565 . ? O2 Ce1 O19 76.28(9) . . ? O20 Ce1 O19 150.48(14) . . ? O2 Ce1 O18 146.19(10) 6_565 7 ? O2 Ce1 O18 81.96(10) . 7 ? O20 Ce1 O18 128.05(9) . 7 ? O19 Ce1 O18 72.85(10) . 7 ? O2 Ce1 O18 81.96(10) 6_565 4 ? O2 Ce1 O18 146.19(10) . 4 ? O20 Ce1 O18 128.05(9) . 4 ? O19 Ce1 O18 72.85(10) . 4 ? O18 Ce1 O18 76.13(14) 7 4 ? O2 Ce1 O17 160.37(10) 6_565 7 ? O2 Ce1 O17 85.54(10) . 7 ? O20 Ce1 O17 77.69(10) . 7 ? O19 Ce1 O17 123.09(9) . 7 ? O18 Ce1 O17 51.22(9) 7 7 ? O18 Ce1 O17 99.92(10) 4 7 ? O2 Ce1 O17 85.54(10) 6_565 4 ? O2 Ce1 O17 160.37(10) . 4 ? O20 Ce1 O17 77.69(10) . 4 ? O19 Ce1 O17 123.09(9) . 4 ? O18 Ce1 O17 99.92(10) 7 4 ? O18 Ce1 O17 51.22(9) 4 4 ? O17 Ce1 O17 80.71(14) 7 4 ? O2 Ce1 C16 169.54(11) 6_565 7 ? O2 Ce1 C16 82.99(10) . 7 ? O20 Ce1 C16 102.81(11) . 7 ? O19 Ce1 C16 98.08(11) . 7 ? O18 Ce1 C16 25.71(10) 7 7 ? O18 Ce1 C16 87.98(11) 4 7 ? O17 Ce1 C16 25.52(10) 7 7 ? O17 Ce1 C16 90.39(11) 4 7 ? O2 Ce1 C16 82.99(10) 6_565 4 ? O2 Ce1 C16 169.54(11) . 4 ? O20 Ce1 C16 102.81(11) . 4 ? O19 Ce1 C16 98.08(11) . 4 ? O18 Ce1 C16 87.98(11) 7 4 ? O18 Ce1 C16 25.71(10) 4 4 ? O17 Ce1 C16 90.39(11) 7 4 ? O17 Ce1 C16 25.52(10) 4 4 ? C16 Ce1 C16 89.19(15) 7 4 ? C3 O2 Ce1 154.0(3) . . ? O2 C3 O2 124.3(5) . 2_556 ? O2 C3 C4 117.8(2) . . ? O2 C3 C4 117.8(2) 2_556 . ? C5 C4 C5 122.2(5) . 2_556 ? C5 C4 C3 118.9(2) . . ? C5 C4 C3 118.9(2) 2_556 . ? C4 C5 C6 118.5(3) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? O8 C6 C7 115.3(3) . . ? O8 C6 C5 124.4(3) . . ? C7 C6 C5 120.3(3) . . ? C6 C7 C6 120.2(5) . 2_556 ? C6 C7 H7 119.9 . . ? C6 C7 H7 119.9 2_556 . ? C6 O8 C9 117.4(3) . . ? O8 C9 C10 107.3(3) . . ? O8 C9 H9A 110.3 . . ? C10 C9 H9A 110.3 . . ? O8 C9 H9B 110.3 . . ? C10 C9 H9B 110.3 . . ? H9A C9 H9B 108.5 . . ? C15 C10 C11 118.8(3) . . ? C15 C10 C9 120.8(4) . . ? C11 C10 C9 120.4(4) . . ? C12 C11 C10 120.4(4) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C13 C12 C11 120.6(4) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 119.0(4) . . ? C12 C13 C16 120.3(4) . . ? C14 C13 C16 120.7(4) . . ? C15 C14 C13 119.7(4) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C10 C15 C14 121.5(4) . . ? C10 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? O17 C16 O18 121.6(4) . . ? O17 C16 C13 119.9(4) . . ? O18 C16 C13 118.5(4) . . ? O17 C16 Ce1 61.2(2) . 7 ? O18 C16 Ce1 60.4(2) . 7 ? C13 C16 Ce1 178.0(3) . 7 ? C16 O17 Ce1 93.3(2) . 7 ? C16 O18 Ce1 93.9(2) . 7 ? Ce1 O19 H19 121.9 . . ? O20 C21 N22 118.2(7) . . ? O20 C21 H21 120.3 . . ? N22 C21 H21 121.5 . . ? C21 N22 C24 118.9(7) . . ? C21 N22 C23 113.4(7) . . ? C24 N22 C23 127.5(7) . . ? N22 C23 H23A 108.3 . . ? N22 C23 H23B 110.5 . . ? H23A C23 H23B 109.5 . . ? N22 C23 H23C 109.6 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N22 C24 H24A 110.1 . . ? N22 C24 H24B 110.0 . . ? H24A C24 H24B 109.5 . . ? N22 C24 H24C 108.3 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.32 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.248 _refine_diff_density_min -0.847 _refine_diff_density_rms 0.099 data_2 _database_code_depnum_ccdc_archive 'CCDC 918382' #TrackingRef 'Combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H26 N Nd O10' _chemical_formula_sum 'C27 H26 N Nd O10' _chemical_formula_weight 668.72 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' Nd Nd -0.2486 2.6331 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 13.6593(4) _cell_length_b 24.5441(11) _cell_length_c 8.4234(3) _cell_angle_alpha 90.000 _cell_angle_beta 105.445(3) _cell_angle_gamma 90.000 _cell_volume 2722.00(18) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2928 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.86 _exptl_crystal_description needles _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 1.965 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5902 _exptl_absorpt_correction_T_max 0.8277 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10937 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 27.86 _reflns_number_total 3241 _reflns_number_gt 2734 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _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. The DMA molecule coordinated to the metal site resides on, and is disordered about, the mirror plane. ; _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^)+(0.0580P)^2^+2.8163P] 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 3241 _refine_ls_number_parameters 193 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1005 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 Nd1 Nd 0.13519(2) 0.5000 0.34060(3) 0.02819(11) Uani 1 2 d S . . O2 O 0.0667(2) 0.42543(11) 0.4479(4) 0.0405(7) Uani 1 1 d . . . C3 C 0.0000 0.4019(2) 0.5000 0.0292(11) Uani 1 2 d S . . C4 C 0.0000 0.3403(2) 0.5000 0.0250(10) Uani 1 2 d S . . C5 C 0.0540(3) 0.31268(15) 0.4059(4) 0.0269(7) Uani 1 1 d . . . H5 H 0.0911 0.3322 0.3437 0.032 Uiso 1 1 calc R . . C6 C 0.0524(3) 0.25577(15) 0.4050(4) 0.0275(7) Uani 1 1 d . . . C7 C 0.0000 0.2275(2) 0.5000 0.0271(10) Uani 1 2 d S . . H7 H 0.0000 0.1888 0.5000 0.033 Uiso 1 2 calc SR . . O8 O 0.0999(2) 0.22380(11) 0.3151(3) 0.0306(6) Uani 1 1 d . . . C9 C 0.1519(3) 0.25149(16) 0.2097(5) 0.0319(8) Uani 1 1 d . . . H9A H 0.2101 0.2727 0.2766 0.038 Uiso 1 1 calc R . . H9B H 0.1051 0.2768 0.1344 0.038 Uiso 1 1 calc R . . C10 C 0.1884(3) 0.20797(16) 0.1131(5) 0.0302(8) Uani 1 1 d . . . C11 C 0.1279(3) 0.19139(17) -0.0392(5) 0.0340(8) Uani 1 1 d . . . H11 H 0.0635 0.2079 -0.0833 0.041 Uiso 1 1 calc R . . C12 C 0.1611(3) 0.15059(18) -0.1277(5) 0.0343(9) Uani 1 1 d . . . H12 H 0.1195 0.1395 -0.2318 0.041 Uiso 1 1 calc R . . C13 C 0.2551(3) 0.12622(16) -0.0635(4) 0.0303(8) Uani 1 1 d . . . C14 C 0.3165(3) 0.14374(18) 0.0873(5) 0.0368(9) Uani 1 1 d . . . H14 H 0.3814 0.1277 0.1309 0.044 Uiso 1 1 calc R . . C15 C 0.2834(3) 0.18440(18) 0.1737(5) 0.0379(9) Uani 1 1 d . . . H15 H 0.3262 0.1964 0.2760 0.046 Uiso 1 1 calc R . . C16 C 0.2910(3) 0.08263(17) -0.1593(5) 0.0328(8) Uani 1 1 d . . . O17 O 0.2337(2) 0.06639(13) -0.2944(3) 0.0420(7) Uani 1 1 d . . . O18 O 0.3788(2) 0.06280(15) -0.1023(4) 0.0508(9) Uani 1 1 d . . . O19 O -0.0452(3) 0.5000 0.1811(5) 0.0409(9) Uani 1 2 d S . . H19 H -0.0651 0.5265 0.1149 0.049 Uiso 0.50 1 d PR . . O20 O 0.2582(3) 0.5000 0.6036(5) 0.0418(10) Uani 1 2 d S . . C21 C 0.3476(7) 0.5171(3) 0.6660(10) 0.039(2) Uani 0.50 1 d P . . H21 H 0.3611 0.5548 0.6756 0.047 Uiso 0.50 1 d PR . . N22 N 0.4211(7) 0.4808(3) 0.7178(11) 0.053(2) Uani 0.50 1 d P . . C23 C 0.3850(5) 0.4218(2) 0.6923(9) 0.0801(19) Uani 0.50 1 d P. . . H23A H 0.3830 0.4072 0.8001 0.120 Uiso 0.50 1 d PR . . H23B H 0.4305 0.3998 0.6470 0.120 Uiso 0.50 1 d PR . . H23C H 0.3170 0.4210 0.6160 0.120 Uiso 0.50 1 d PR . . C24 C 0.5291(6) 0.5000 0.7848(14) 0.094(3) Uani 1 2 d S . . H24A H 0.5318 0.5395 0.7758 0.141 Uiso 0.50 1 d PR . . H24B H 0.5710 0.4834 0.7203 0.141 Uiso 0.50 1 d PR . . H24C H 0.5544 0.4893 0.9014 0.141 Uiso 0.50 1 d PR . . C25 C 0.3850(5) 0.4218(2) 0.6923(9) 0.0801(19) Uani 0.50 1 d P. . . H25A H 0.3830 0.4072 0.8001 0.120 Uiso 0.50 1 d PR . . H25B H 0.4305 0.3998 0.6470 0.120 Uiso 0.50 1 d PR . . H25C H 0.3170 0.4210 0.6160 0.120 Uiso 0.50 1 d PR . . 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 Nd1 0.02858(17) 0.02934(18) 0.02985(17) 0.000 0.01336(11) 0.000 O2 0.0442(17) 0.0274(15) 0.0570(19) 0.0027(13) 0.0261(14) -0.0022(12) C3 0.037(3) 0.026(3) 0.025(2) 0.000 0.009(2) 0.000 C4 0.028(2) 0.020(2) 0.026(2) 0.000 0.0050(18) 0.000 C5 0.0282(18) 0.028(2) 0.0255(17) 0.0035(14) 0.0084(13) -0.0001(14) C6 0.0310(18) 0.027(2) 0.0256(17) -0.0020(13) 0.0095(14) 0.0034(14) C7 0.033(3) 0.022(3) 0.027(2) 0.000 0.010(2) 0.000 O8 0.0401(14) 0.0247(14) 0.0320(13) 0.0001(10) 0.0185(11) 0.0024(11) C9 0.036(2) 0.033(2) 0.0317(19) -0.0011(15) 0.0172(15) -0.0004(16) C10 0.0329(19) 0.028(2) 0.0339(19) 0.0011(15) 0.0159(15) 0.0013(15) C11 0.0281(19) 0.040(2) 0.035(2) -0.0008(16) 0.0105(15) 0.0084(16) C12 0.034(2) 0.040(2) 0.0304(19) -0.0010(16) 0.0127(15) 0.0022(17) C13 0.0322(19) 0.033(2) 0.0286(18) -0.0002(15) 0.0136(14) 0.0028(16) C14 0.033(2) 0.043(2) 0.032(2) 0.0002(17) 0.0049(15) 0.0082(17) C15 0.038(2) 0.044(3) 0.030(2) -0.0069(16) 0.0053(16) 0.0068(18) C16 0.0315(19) 0.036(2) 0.033(2) 0.0004(16) 0.0135(15) 0.0033(16) O17 0.0346(15) 0.0513(19) 0.0384(16) -0.0145(13) 0.0067(12) 0.0095(13) O18 0.0409(17) 0.064(2) 0.0433(17) -0.0164(15) 0.0044(13) 0.0235(15) O19 0.032(2) 0.050(3) 0.039(2) 0.000 0.0071(16) 0.000 O20 0.041(2) 0.052(3) 0.032(2) 0.000 0.0070(17) 0.000 C21 0.054(6) 0.025(5) 0.036(4) -0.003(3) 0.010(4) -0.003(3) N22 0.039(4) 0.053(6) 0.065(5) 0.006(3) 0.007(4) 0.007(3) C23 0.104(5) 0.037(3) 0.099(5) 0.013(3) 0.027(4) 0.009(3) C24 0.034(4) 0.110(9) 0.132(9) 0.000 0.010(5) 0.000 C25 0.104(5) 0.037(3) 0.099(5) 0.013(3) 0.027(4) 0.009(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 Nd1 O2 2.343(3) . ? Nd1 O2 2.343(3) 6_565 ? Nd1 O20 2.398(4) . ? Nd1 O19 2.472(4) . ? Nd1 O18 2.497(3) 7 ? Nd1 O18 2.497(3) 4 ? Nd1 O17 2.527(3) 7 ? Nd1 O17 2.527(3) 4 ? Nd1 C16 2.878(4) 4 ? Nd1 C16 2.878(4) 7 ? O2 C3 1.253(4) . ? C3 O2 1.253(4) 2_556 ? C3 C4 1.511(7) . ? C4 C5 1.394(4) . ? C4 C5 1.394(4) 2_556 ? C5 C6 1.397(5) . ? C5 H5 0.9500 . ? C6 O8 1.368(4) . ? C6 C7 1.392(4) . ? C7 C6 1.392(4) 2_556 ? C7 H7 0.9500 . ? O8 C9 1.446(4) . ? C9 C10 1.506(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C15 1.387(6) . ? C10 C11 1.390(6) . ? C11 C12 1.394(5) . ? C11 H11 0.9500 . ? C12 C13 1.389(5) . ? C12 H12 0.9500 . ? C13 C14 1.391(6) . ? C13 C16 1.499(5) . ? C14 C15 1.381(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 O17 1.262(5) . ? C16 O18 1.265(5) . ? C16 Nd1 2.878(4) 7 ? O17 Nd1 2.527(3) 7 ? O18 Nd1 2.497(3) 7 ? O19 H19 0.8521 . ? O20 C21 1.265(9) 6_565 ? O20 C21 1.265(9) . ? C21 N22 1.326(11) . ? C21 H21 0.9442 . ? N22 C24 1.508(11) . ? N22 C23 1.525(10) . ? C23 H23A 0.9837 . ? C23 H23B 0.9747 . ? C23 H23C 0.9783 . ? C24 H24A 0.9741 . ? C24 H24B 0.9765 . ? C24 H24C 0.9856 . ? 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 Nd1 O2 102.72(14) . 6_565 ? O2 Nd1 O20 84.10(10) . . ? O2 Nd1 O20 84.10(10) 6_565 . ? O2 Nd1 O19 76.55(9) . . ? O2 Nd1 O19 76.55(9) 6_565 . ? O20 Nd1 O19 148.66(14) . . ? O2 Nd1 O18 82.82(11) . 7 ? O2 Nd1 O18 147.04(10) 6_565 7 ? O20 Nd1 O18 128.85(9) . 7 ? O19 Nd1 O18 73.22(10) . 7 ? O2 Nd1 O18 147.04(10) . 4 ? O2 Nd1 O18 82.82(11) 6_565 4 ? O20 Nd1 O18 128.85(9) . 4 ? O19 Nd1 O18 73.22(10) . 4 ? O18 Nd1 O18 76.22(17) 7 4 ? O2 Nd1 O17 85.84(10) . 7 ? O2 Nd1 O17 159.23(10) 6_565 7 ? O20 Nd1 O17 77.94(10) . 7 ? O19 Nd1 O17 124.11(9) . 7 ? O18 Nd1 O17 51.97(9) 7 7 ? O18 Nd1 O17 100.37(11) 4 7 ? O2 Nd1 O17 159.23(10) . 4 ? O2 Nd1 O17 85.84(10) 6_565 4 ? O20 Nd1 O17 77.94(10) . 4 ? O19 Nd1 O17 124.11(9) . 4 ? O18 Nd1 O17 100.37(11) 7 4 ? O18 Nd1 O17 51.97(9) 4 4 ? O17 Nd1 O17 80.33(15) 7 4 ? O2 Nd1 C16 170.85(11) . 4 ? O2 Nd1 C16 83.48(11) 6_565 4 ? O20 Nd1 C16 103.40(10) . 4 ? O19 Nd1 C16 98.68(10) . 4 ? O18 Nd1 C16 88.33(12) 7 4 ? O18 Nd1 C16 26.00(10) 4 4 ? O17 Nd1 C16 90.57(11) 7 4 ? O17 Nd1 C16 25.97(10) 4 4 ? O2 Nd1 C16 83.48(11) . 7 ? O2 Nd1 C16 170.85(11) 6_565 7 ? O20 Nd1 C16 103.40(10) . 7 ? O19 Nd1 C16 98.68(10) . 7 ? O18 Nd1 C16 26.00(10) 7 7 ? O18 Nd1 C16 88.34(12) 4 7 ? O17 Nd1 C16 25.97(10) 7 7 ? O17 Nd1 C16 90.57(11) 4 7 ? C16 Nd1 C16 89.60(16) 4 7 ? C3 O2 Nd1 153.8(3) . . ? O2 C3 O2 125.1(5) 2_556 . ? O2 C3 C4 117.4(3) 2_556 . ? O2 C3 C4 117.4(3) . . ? C5 C4 C5 121.7(5) . 2_556 ? C5 C4 C3 119.1(2) . . ? C5 C4 C3 119.1(2) 2_556 . ? C4 C5 C6 118.7(3) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? O8 C6 C7 115.1(3) . . ? O8 C6 C5 124.6(3) . . ? C7 C6 C5 120.3(3) . . ? C6 C7 C6 120.2(5) 2_556 . ? C6 C7 H7 119.9 2_556 . ? C6 C7 H7 119.9 . . ? C6 O8 C9 117.0(3) . . ? O8 C9 C10 106.6(3) . . ? O8 C9 H9A 110.4 . . ? C10 C9 H9A 110.4 . . ? O8 C9 H9B 110.4 . . ? C10 C9 H9B 110.4 . . ? H9A C9 H9B 108.6 . . ? C15 C10 C11 119.1(3) . . ? C15 C10 C9 120.6(4) . . ? C11 C10 C9 120.3(3) . . ? C10 C11 C12 120.4(4) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C13 C12 C11 120.0(4) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 119.5(4) . . ? C12 C13 C16 119.9(3) . . ? C14 C13 C16 120.6(3) . . ? C15 C14 C13 120.1(4) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C10 120.9(4) . . ? C14 C15 H15 119.6 . . ? C10 C15 H15 119.6 . . ? O17 C16 O18 121.2(4) . . ? O17 C16 C13 119.9(3) . . ? O18 C16 C13 118.9(3) . . ? O17 C16 Nd1 61.3(2) . 7 ? O18 C16 Nd1 59.9(2) . 7 ? C13 C16 Nd1 178.6(3) . 7 ? C16 O17 Nd1 92.8(2) . 7 ? C16 O18 Nd1 94.1(2) . 7 ? Nd1 O19 H19 117.0 . . ? C21 O20 Nd1 138.2(4) . . ? O20 C21 N22 118.4(7) . . ? O20 C21 H21 120.3 . . ? N22 C21 H21 121.2 . . ? C21 N22 C24 119.5(7) . . ? C21 N22 C23 113.8(7) . . ? C24 N22 C23 126.6(6) . . ? N22 C23 H23A 107.6 . . ? N22 C23 H23B 111.4 . . ? H23A C23 H23B 109.7 . . ? N22 C23 H23C 109.1 . . ? H23A C23 H23C 110.1 . . ? H23B C23 H23C 108.9 . . ? N22 C24 H24A 109.6 . . ? N22 C24 H24B 108.7 . . ? H24A C24 H24B 109.4 . . ? N22 C24 H24C 109.8 . . ? H24A C24 H24C 109.3 . . ? H24B C24 H24C 110.0 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 2.373 _refine_diff_density_min -1.233 _refine_diff_density_rms 0.123 data_3 _database_code_depnum_ccdc_archive 'CCDC 918383' #TrackingRef 'Combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H15 Cu2 O9, C4 H9 N O' _chemical_formula_sum 'C23 H15 Cu2 O9' _chemical_formula_weight 649.55 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.8091(4) _cell_length_b 25.5978(7) _cell_length_c 5.7377(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.1557(12) _cell_angle_gamma 90.00 _cell_volume 2589.21(13) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 3080 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 27.82 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 1.704 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5896 _exptl_absorpt_correction_T_max 0.7858 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14289 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 27.82 _reflns_number_total 3075 _reflns_number_gt 2675 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _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. The crystals contain residual DMA crystallization solvent in the interstitial voids, which could not be modeled reliably by discrete atoms. Its contribution to the diffraction pattern was thus subtracted by the SQUEEZE technique, using the PLATON software (Spek, 2009), The crystallization solvent is located on and disordered about crystallographic centers of inversion. ; _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^)+(0.0667P)^2^+1.4521P] 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 3075 _refine_ls_number_parameters 156 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1142 _refine_ls_wR_factor_gt 0.1101 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 -0.083534(16) 0.478207(11) 0.04994(5) 0.01487(13) Uani 1 1 d . . . O2 O 0.0000 0.50940(9) 0.2500 0.0115(5) Uani 1 2 d S . . O3 O -0.04079(10) 0.40820(6) 0.0808(3) 0.0161(4) Uani 1 1 d . . . C4 C 0.0000 0.38586(13) 0.2500 0.0127(6) Uani 1 2 d S . . C5 C 0.0000 0.32755(13) 0.2500 0.0127(6) Uani 1 2 d S . . C6 C 0.04429(13) 0.30094(9) 0.4341(5) 0.0150(5) Uani 1 1 d . . . H6 H 0.0735 0.3195 0.5588 0.018 Uiso 1 1 calc R . . C7 C 0.04441(13) 0.24653(10) 0.4293(4) 0.0155(5) Uani 1 1 d . . . C8 C 0.0000 0.21903(13) 0.2500 0.0157(7) Uani 1 2 d S . . H8 H 0.0000 0.1819 0.2500 0.019 Uiso 1 2 calc SR . . O9 O 0.08718(10) 0.21566(7) 0.5926(3) 0.0204(4) Uani 1 1 d . . . C10 C 0.13808(14) 0.24036(10) 0.7785(5) 0.0183(5) Uani 1 1 d . . . H10A H 0.1095 0.2553 0.8988 0.022 Uiso 1 1 calc R . . H10B H 0.1670 0.2687 0.7147 0.022 Uiso 1 1 calc R . . C11 C 0.19047(14) 0.19779(10) 0.8830(5) 0.0166(5) Uani 1 1 d . . . C12 C 0.18126(15) 0.17386(11) 1.0936(5) 0.0223(6) Uani 1 1 d . . . H12 H 0.1430 0.1859 1.1801 0.027 Uiso 1 1 calc R . . C13 C 0.22767(15) 0.13232(11) 1.1796(5) 0.0213(5) Uani 1 1 d . . . H13 H 0.2220 0.1168 1.3265 0.026 Uiso 1 1 calc R . . C14 C 0.28240(14) 0.11368(10) 1.0495(5) 0.0167(5) Uani 1 1 d . . . C15 C 0.29240(15) 0.13766(11) 0.8390(5) 0.0216(6) Uani 1 1 d . . . H15 H 0.3297 0.1251 0.7501 0.026 Uiso 1 1 calc R . . C16 C 0.24730(16) 0.18037(11) 0.7588(5) 0.0220(5) Uani 1 1 d . . . H16 H 0.2555 0.1977 0.6182 0.026 Uiso 1 1 calc R . . C17 C 0.33077(14) 0.06810(10) 1.1383(5) 0.0179(5) Uani 1 1 d . . . O18 O 0.36882(10) 0.04630(7) 0.9944(3) 0.0209(4) Uani 1 1 d . . . O19 O 0.33061(10) 0.05469(7) 1.3517(3) 0.0198(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01443(18) 0.00905(18) 0.01897(19) -0.00150(11) -0.00508(12) 0.00094(10) O2 0.0134(11) 0.0086(10) 0.0105(11) 0.000 -0.0049(9) 0.000 O3 0.0202(9) 0.0078(8) 0.0177(9) -0.0009(6) -0.0067(7) 0.0025(6) C4 0.0133(15) 0.0074(14) 0.0165(16) 0.000 -0.0013(12) 0.000 C5 0.0125(15) 0.0080(15) 0.0163(16) 0.000 -0.0029(12) 0.000 C6 0.0126(11) 0.0091(11) 0.0216(12) 0.0004(9) -0.0034(9) 0.0007(8) C7 0.0114(11) 0.0121(11) 0.0216(13) 0.0029(9) -0.0023(9) 0.0019(8) C8 0.0137(15) 0.0070(14) 0.0251(18) 0.000 -0.0017(13) 0.000 O9 0.0202(9) 0.0089(8) 0.0282(10) 0.0027(7) -0.0103(8) 0.0014(7) C10 0.0166(12) 0.0137(11) 0.0221(13) 0.0005(10) -0.0061(10) 0.0038(9) C11 0.0154(11) 0.0112(11) 0.0214(12) -0.0001(9) -0.0038(10) 0.0036(9) C12 0.0206(13) 0.0225(14) 0.0238(13) 0.0039(11) 0.0035(11) 0.0077(10) C13 0.0217(13) 0.0206(13) 0.0213(13) 0.0051(10) 0.0025(10) 0.0060(10) C14 0.0152(11) 0.0120(11) 0.0210(12) 0.0013(9) -0.0044(9) 0.0023(9) C15 0.0221(13) 0.0209(13) 0.0223(13) 0.0033(10) 0.0048(11) 0.0087(10) C16 0.0257(13) 0.0193(13) 0.0211(13) 0.0062(10) 0.0040(10) 0.0065(10) C17 0.0141(11) 0.0140(12) 0.0238(13) 0.0021(10) -0.0043(10) 0.0016(9) O18 0.0208(9) 0.0140(9) 0.0260(10) 0.0014(7) -0.0039(8) 0.0061(7) O19 0.0159(9) 0.0187(9) 0.0226(10) 0.0045(7) -0.0050(7) 0.0013(7) _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 1.9193(10) . ? Cu1 O18 1.9451(18) 3_454 ? Cu1 O3 1.9452(17) . ? Cu1 O19 1.9616(18) 8_454 ? O2 Cu1 1.9194(10) 2 ? O3 C4 1.264(2) . ? C4 O3 1.264(2) 2 ? C4 C5 1.493(4) . ? C5 C6 1.402(3) 2 ? C5 C6 1.402(3) . ? C6 C7 1.393(3) . ? C6 H6 0.9500 . ? C7 O9 1.371(3) . ? C7 C8 1.396(3) . ? C8 C7 1.396(3) 2 ? C8 H8 0.9500 . ? O9 C10 1.444(3) . ? C10 C11 1.503(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.385(4) . ? C11 C16 1.391(4) . ? C12 C13 1.394(4) . ? C12 H12 0.9500 . ? C13 C14 1.393(4) . ? C13 H13 0.9500 . ? C14 C15 1.389(4) . ? C14 C17 1.496(3) . ? C15 C16 1.395(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 O18 1.269(3) . ? C17 O19 1.272(3) . ? O18 Cu1 1.9451(18) 3_546 ? O19 Cu1 1.9616(18) 8_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 O2 Cu1 O18 90.48(8) . 3_454 ? O2 Cu1 O3 93.94(8) . . ? O18 Cu1 O3 175.19(8) 3_454 . ? O2 Cu1 O19 178.66(7) . 8_454 ? O18 Cu1 O19 90.21(8) 3_454 8_454 ? O3 Cu1 O19 85.41(8) . 8_454 ? Cu1 O2 Cu1 130.83(13) . 2 ? C4 O3 Cu1 131.43(17) . . ? O3 C4 O3 126.2(3) . 2 ? O3 C4 C5 116.91(15) . . ? O3 C4 C5 116.91(15) 2 . ? C6 C5 C6 121.9(3) 2 . ? C6 C5 C4 119.07(15) 2 . ? C6 C5 C4 119.07(15) . . ? C7 C6 C5 118.2(2) . . ? C7 C6 H6 120.9 . . ? C5 C6 H6 120.9 . . ? O9 C7 C6 124.4(2) . . ? O9 C7 C8 114.5(2) . . ? C6 C7 C8 121.1(2) . . ? C7 C8 C7 119.4(3) . 2 ? C7 C8 H8 120.3 . . ? C7 C8 H8 120.3 2 . ? C7 O9 C10 118.82(19) . . ? O9 C10 C11 105.4(2) . . ? O9 C10 H10A 110.7 . . ? C11 C10 H10A 110.7 . . ? O9 C10 H10B 110.7 . . ? C11 C10 H10B 110.7 . . ? H10A C10 H10B 108.8 . . ? C12 C11 C16 119.3(2) . . ? C12 C11 C10 121.7(2) . . ? C16 C11 C10 118.9(2) . . ? C11 C12 C13 120.6(2) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C14 C13 C12 119.8(2) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C15 C14 C13 120.0(2) . . ? C15 C14 C17 120.1(2) . . ? C13 C14 C17 119.8(2) . . ? C14 C15 C16 119.6(2) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C11 C16 C15 120.6(3) . . ? C11 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? O18 C17 O19 125.6(2) . . ? O18 C17 C14 117.1(2) . . ? O19 C17 C14 117.3(2) . . ? C17 O18 Cu1 123.23(17) . 3_546 ? C17 O19 Cu1 124.48(16) . 8_557 ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.043 342 46 ' ' 2 0.500 0.500 0.039 342 46 ' ' _platon_squeeze_details ; There are two molecules of the DMA solvent per unit-cell located on, and disordered about, crystallographic inversion centers at 0,0,0 and 0.5,0.5,0. ; # start Validation Reply Form _vrf_CHEMW01_3 ; PROBLEM: RESPONSE: The disordered DMA solvent (2 molecules per unit-cell) was included in the structural formula, but excluded from the structural model. ; _vrf_CHEMW03_3 ; PROBLEM: RESPONSE: The disordered DMA solvent (2 molecules per unit-cell) was included in the structural formula, but excluded from the structural model. ; # end Validation Reply Form _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.82 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.849 _refine_diff_density_min -0.754 _refine_diff_density_rms 0.107 data_4 _database_code_depnum_ccdc_archive 'CCDC 918384' #TrackingRef 'Combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H38 Cd2 N2 O16, 2(C2 H8 N), 4(C4 H9 N O)' _chemical_formula_sum 'C76 H90 Cd2 N8 O20' _chemical_formula_weight 1660.36 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' 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' 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 15.3997(9) _cell_length_b 15.4635(9) _cell_length_c 17.2247(10) _cell_angle_alpha 93.145(3) _cell_angle_beta 114.157(2) _cell_angle_gamma 100.775(3) _cell_volume 3636.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 12795 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 26.02 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1716 _exptl_absorpt_coefficient_mu 0.665 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8064 _exptl_absorpt_correction_T_max 0.8823 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28863 _diffrn_reflns_av_R_equivalents 0.0770 _diffrn_reflns_av_sigmaI/netI 0.0706 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.05 _reflns_number_total 12824 _reflns_number_gt 8927 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _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. The asymmetric unit contains also four severely disordered molecules of dimethylacetamide, which could not be reliably modeled by discrete atoms. Their contribution to the diffraction pattern was subtracted by the SQUEEZE procedure, using the PLATON software (Spek, 2009). ; _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^+1.4975P] 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 12824 _refine_ls_number_parameters 743 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0980 _refine_ls_R_factor_gt 0.0683 _refine_ls_wR_factor_ref 0.1600 _refine_ls_wR_factor_gt 0.1499 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.003 _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 0.77738(3) 0.06273(3) 0.59840(3) 0.03406(14) Uani 1 1 d . . . Cd2 Cd 0.21511(3) 0.25371(3) -0.02429(3) 0.03391(14) Uani 1 1 d . . . O3 O 0.2159(3) 0.0930(3) -0.0687(3) 0.0389(10) Uani 1 1 d . . . O4 O 0.3282(3) 0.2080(3) -0.0643(3) 0.0401(10) Uani 1 1 d . . . C5 C 0.2945(4) 0.1260(4) -0.0738(4) 0.0343(14) Uani 1 1 d . . . C6 C 0.3514(4) 0.0639(4) -0.0923(4) 0.0313(13) Uani 1 1 d . . . C7 C 0.4364(4) 0.1023(4) -0.1007(4) 0.0343(14) Uani 1 1 d . . . H7 H 0.4567 0.1649 -0.0967 0.041 Uiso 1 1 calc R . . C8 C 0.4900(4) 0.0452(4) -0.1153(4) 0.0340(14) Uani 1 1 d . . . C9 C 0.4602(4) -0.0457(4) -0.1226(4) 0.0353(14) Uani 1 1 d . . . H9 H 0.4963 -0.0833 -0.1352 0.042 Uiso 1 1 calc R . . C10 C 0.3774(4) -0.0824(4) -0.1115(4) 0.0340(14) Uani 1 1 d . . . C11 C 0.3222(4) -0.0277(4) -0.0963(4) 0.0349(14) Uani 1 1 d . . . H11 H 0.2653 -0.0524 -0.0888 0.042 Uiso 1 1 calc R . . O12 O 0.5763(3) 0.0739(3) -0.1230(3) 0.0419(11) Uani 1 1 d . . . C13 C 0.6240(4) 0.1671(4) -0.0947(4) 0.0371(14) Uani 1 1 d . . . H13A H 0.6210 0.1878 -0.0407 0.044 Uiso 1 1 calc R . . H13B H 0.5915 0.2031 -0.1390 0.044 Uiso 1 1 calc R . . C14 C 0.7290(4) 0.1766(4) -0.0804(4) 0.0357(14) Uani 1 1 d . . . C15 C 0.7491(4) 0.1462(4) -0.1464(4) 0.0340(14) Uani 1 1 d . . . H15 H 0.6973 0.1176 -0.1998 0.041 Uiso 1 1 calc R . . C16 C 0.8463(4) 0.1577(4) -0.1344(4) 0.0360(14) Uani 1 1 d . . . H16 H 0.8600 0.1371 -0.1802 0.043 Uiso 1 1 calc R . . C17 C 0.9227(4) 0.1988(4) -0.0567(4) 0.0342(14) Uani 1 1 d . . . C18 C 0.9012(5) 0.2289(5) 0.0097(5) 0.0519(19) Uani 1 1 d . . . H18 H 0.9527 0.2578 0.0632 0.062 Uiso 1 1 calc R . . C19 C 0.8051(5) 0.2169(5) -0.0023(4) 0.0499(18) Uani 1 1 d . . . H19 H 0.7911 0.2366 0.0436 0.060 Uiso 1 1 calc R . . C20 C 1.0261(4) 0.2162(4) -0.0458(4) 0.0376(15) Uani 1 1 d . . . O21` O 1.0438(3) 0.1953(3) -0.1094(3) 0.0415(11) Uani 1 1 d . . . O22 O 1.0938(3) 0.2501(4) 0.0260(3) 0.0636(15) Uani 1 1 d . . . O23 O 0.3443(3) -0.1711(3) -0.1131(3) 0.0416(11) Uani 1 1 d . . . C24 C 0.4019(4) -0.2307(4) -0.1238(4) 0.0412(15) Uani 1 1 d . . . H24A H 0.4717 -0.2072 -0.0839 0.049 Uiso 1 1 calc R . . H24B H 0.3961 -0.2353 -0.1834 0.049 Uiso 1 1 calc R . . C25 C 0.3667(5) -0.3186(4) -0.1059(4) 0.0420(16) Uani 1 1 d . . . C26 C 0.4283(5) -0.3567(5) -0.0388(5) 0.0520(18) Uani 1 1 d . . . H26 H 0.4939 -0.3250 -0.0048 0.062 Uiso 1 1 calc R . . C27 C 0.3955(5) -0.4392(5) -0.0214(5) 0.0515(18) Uani 1 1 d . . . H27 H 0.4385 -0.4634 0.0246 0.062 Uiso 1 1 calc R . . C28 C 0.2981(5) -0.4886(4) -0.0713(4) 0.0429(16) Uani 1 1 d . . . C29 C 0.2366(5) -0.4507(5) -0.1378(5) 0.0510(18) Uani 1 1 d . . . H29 H 0.1711 -0.4823 -0.1723 0.061 Uiso 1 1 calc R . . C30 C 0.2704(5) -0.3675(5) -0.1538(5) 0.0513(18) Uani 1 1 d . . . H30 H 0.2268 -0.3426 -0.1988 0.062 Uiso 1 1 calc R . . C31 C 0.2661(5) -0.5764(5) -0.0534(5) 0.0453(17) Uani 1 1 d . . . O32 O 0.3146(4) -0.6003(3) 0.0183(3) 0.0531(12) Uani 1 1 d . . . O33 O 0.1901(3) -0.6306(3) -0.1104(3) 0.0557(13) Uani 1 1 d . . . O34 O 0.6678(3) 0.1012(3) 0.6475(3) 0.0353(10) Uani 1 1 d . . . O35 O 0.7738(3) 0.2146(3) 0.6409(3) 0.0386(10) Uani 1 1 d . . . C36 C 0.6956(4) 0.1827(4) 0.6493(4) 0.0344(14) Uani 1 1 d . . . C37 C 0.6375(4) 0.2448(4) 0.6601(4) 0.0363(14) Uani 1 1 d . . . C38 C 0.6640(4) 0.3339(4) 0.6564(4) 0.0418(16) Uani 1 1 d . . . H38 H 0.7216 0.3570 0.6494 0.050 Uiso 1 1 calc R . . C39 C 0.6051(5) 0.3903(4) 0.6633(5) 0.0492(18) Uani 1 1 d . . . C40 C 0.5226(5) 0.3572(4) 0.6746(5) 0.0498(18) Uani 1 1 d . . . H40 H 0.4832 0.3958 0.6794 0.060 Uiso 1 1 calc R . . C41 C 0.4972(4) 0.2684(4) 0.6790(4) 0.0420(16) Uani 1 1 d . . . C42 C 0.5524(4) 0.2115(4) 0.6709(4) 0.0370(14) Uani 1 1 d . . . H42 H 0.5332 0.1498 0.6725 0.044 Uiso 1 1 calc R . . O43 O 0.4116(3) 0.2430(3) 0.6873(3) 0.0510(13) Uani 1 1 d . . . C44 C 0.3652(4) 0.1497(4) 0.6656(4) 0.0403(15) Uani 1 1 d . . . H44A H 0.4005 0.1168 0.7117 0.048 Uiso 1 1 calc R . . H44B H 0.3650 0.1250 0.6113 0.048 Uiso 1 1 calc R . . C45 C 0.2625(4) 0.1414(4) 0.6557(4) 0.0386(15) Uani 1 1 d . . . C46 C 0.2449(4) 0.1718(4) 0.7252(4) 0.0386(15) Uani 1 1 d . . . H46 H 0.2977 0.1987 0.7787 0.046 Uiso 1 1 calc R . . C47 C 0.1487(4) 0.1617(4) 0.7140(4) 0.0396(15) Uani 1 1 d . . . H47 H 0.1361 0.1796 0.7613 0.048 Uiso 1 1 calc R . . C48 C 0.0715(4) 0.1263(4) 0.6359(4) 0.0349(14) Uani 1 1 d . . . C49 C 0.0888(4) 0.1013(4) 0.5659(4) 0.0419(16) Uani 1 1 d . . . H49 H 0.0356 0.0801 0.5111 0.050 Uiso 1 1 calc R . . C50 C 0.1851(5) 0.1075(5) 0.5765(4) 0.0466(17) Uani 1 1 d . . . H50 H 0.1972 0.0885 0.5292 0.056 Uiso 1 1 calc R . . C51 C -0.0323(4) 0.1115(4) 0.6264(4) 0.0357(14) Uani 1 1 d . . . O52 O -0.0483(3) 0.1173(3) 0.6921(3) 0.0342(9) Uani 1 1 d . . . O53 O -0.1015(3) 0.0907(3) 0.5510(3) 0.0459(11) Uani 1 1 d . . . O54 O 0.6354(4) 0.4778(3) 0.6551(4) 0.0658(16) Uani 1 1 d . . . C55 C 0.5730(6) 0.5359(5) 0.6563(7) 0.072(3) Uani 1 1 d . . . H55A H 0.5695 0.5406 0.7124 0.086 Uiso 1 1 calc R . . H55B H 0.5061 0.5123 0.6104 0.086 Uiso 1 1 calc R . . C56 C 0.6161(6) 0.6259(5) 0.6416(6) 0.057(2) Uani 1 1 d . . . C57 C 0.7105(6) 0.6736(5) 0.7027(6) 0.067(2) Uani 1 1 d . . . H57 H 0.7479 0.6474 0.7501 0.081 Uiso 1 1 calc R . . C58 C 0.7469(5) 0.7582(5) 0.6923(5) 0.0546(19) Uani 1 1 d . . . H58 H 0.8093 0.7912 0.7332 0.066 Uiso 1 1 calc R . . C59 C 0.6921(5) 0.7953(4) 0.6217(5) 0.0433(16) Uani 1 1 d . . . C60 C 0.6020(5) 0.7474(5) 0.5609(5) 0.0515(18) Uani 1 1 d . . . H60 H 0.5669 0.7725 0.5117 0.062 Uiso 1 1 calc R . . C61 C 0.5625(6) 0.6633(5) 0.5711(5) 0.057(2) Uani 1 1 d . . . H61 H 0.4995 0.6315 0.5304 0.068 Uiso 1 1 calc R . . C62 C 0.7297(5) 0.8901(4) 0.6129(5) 0.0409(16) Uani 1 1 d . . . O63 O 0.6832(3) 0.9177(3) 0.5450(3) 0.0474(11) Uani 1 1 d . . . O64 O 0.8039(3) 0.9391(3) 0.6749(3) 0.0555(13) Uani 1 1 d . . . N65 N 0.3108(4) 0.2231(4) 0.1098(3) 0.0372(12) Uani 1 1 d . . . C66 C 0.2951(4) 0.1404(5) 0.1306(4) 0.0389(15) Uani 1 1 d . . . H66 H 0.2367 0.0984 0.0937 0.047 Uiso 1 1 calc R . . C67 C 0.3599(4) 0.1142(4) 0.2027(4) 0.0383(15) Uani 1 1 d . . . H67 H 0.3463 0.0554 0.2150 0.046 Uiso 1 1 calc R . . C68 C 0.4452(4) 0.1747(4) 0.2572(4) 0.0362(14) Uani 1 1 d . . . C69 C 0.4614(4) 0.2620(4) 0.2376(4) 0.0391(15) Uani 1 1 d . . . H69 H 0.5184 0.3058 0.2740 0.047 Uiso 1 1 calc R . . C70 C 0.3920(4) 0.2817(4) 0.1642(4) 0.0377(14) Uani 1 1 d . . . H70 H 0.4024 0.3407 0.1514 0.045 Uiso 1 1 calc R . . C71 C 0.5213(4) 0.1477(4) 0.3310(4) 0.0360(14) Uani 1 1 d . . . C72 C 0.4993(4) 0.0731(4) 0.3664(4) 0.0374(14) Uani 1 1 d . . . H72 H 0.4337 0.0396 0.3450 0.045 Uiso 1 1 calc R . . C73 C 0.5727(4) 0.0473(4) 0.4328(4) 0.0390(15) Uani 1 1 d . . . H73 H 0.5561 -0.0050 0.4551 0.047 Uiso 1 1 calc R . . N74 N 0.6656(4) 0.0921(4) 0.4671(3) 0.0407(13) Uani 1 1 d . . . C75 C 0.6877(5) 0.1650(5) 0.4354(4) 0.0517(18) Uani 1 1 d . . . H75 H 0.7536 0.1981 0.4597 0.062 Uiso 1 1 calc R . . C76 C 0.6189(4) 0.1948(5) 0.3686(4) 0.0474(17) Uani 1 1 d . . . H76 H 0.6380 0.2475 0.3481 0.057 Uiso 1 1 calc R . . N77 N 0.9710(4) -0.0115(4) 0.1816(4) 0.0471(14) Uani 1 1 d . . . H77A H 1.0044 -0.0487 0.2160 0.056 Uiso 1 1 calc R . . H77B H 0.9098 -0.0446 0.1448 0.056 Uiso 1 1 calc R . . C78 C 0.9609(5) 0.0602(5) 0.2362(5) 0.0520(18) Uani 1 1 d . . . H78A H 1.0259 0.0937 0.2776 0.078 Uiso 1 1 calc R . . H78B H 0.9241 0.0337 0.2674 0.078 Uiso 1 1 calc R . . H78C H 0.9259 0.1004 0.1999 0.078 Uiso 1 1 calc R . . C79 C 1.0232(5) 0.0244(5) 0.1308(5) 0.057(2) Uani 1 1 d . . . H79A H 0.9913 0.0683 0.0981 0.085 Uiso 1 1 calc R . . H79B H 1.0217 -0.0242 0.0910 0.085 Uiso 1 1 calc R . . H79C H 1.0912 0.0528 0.1696 0.085 Uiso 1 1 calc R . . N80 N 0.0210(6) 0.6912(4) 0.2452(4) 0.079(2) Uani 1 1 d . . . H80A H 0.0702 0.7420 0.2681 0.094 Uiso 1 1 calc R . . H80B H -0.0331 0.7075 0.2062 0.094 Uiso 1 1 calc R . . C81 C 0.0501(6) 0.6331(6) 0.1980(6) 0.072(2) Uani 1 1 d . . . H81A H 0.0717 0.5855 0.2311 0.108 Uiso 1 1 calc R . . H81B H 0.1040 0.6668 0.1877 0.108 Uiso 1 1 calc R . . H81C H -0.0054 0.6071 0.1428 0.108 Uiso 1 1 calc R . . C82 C -0.0021(7) 0.6624(6) 0.3136(7) 0.080(3) Uani 1 1 d . . . H82A H -0.0601 0.6130 0.2902 0.121 Uiso 1 1 calc R . . H82B H -0.0152 0.7119 0.3419 0.121 Uiso 1 1 calc R . . H82C H 0.0532 0.6426 0.3556 0.121 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 Cd1 0.0248(2) 0.0371(3) 0.0450(3) 0.0083(2) 0.0180(2) 0.0101(2) Cd2 0.0241(2) 0.0380(3) 0.0419(3) 0.0051(2) 0.0150(2) 0.0106(2) O3 0.026(2) 0.045(3) 0.048(3) 0.002(2) 0.0170(19) 0.0101(19) O4 0.032(2) 0.047(3) 0.051(3) 0.011(2) 0.025(2) 0.013(2) C5 0.021(3) 0.048(4) 0.034(3) 0.006(3) 0.012(3) 0.010(3) C6 0.018(3) 0.041(4) 0.037(3) 0.006(3) 0.011(2) 0.013(3) C7 0.028(3) 0.038(4) 0.043(3) 0.004(3) 0.018(3) 0.016(3) C8 0.018(3) 0.049(4) 0.036(3) 0.011(3) 0.013(2) 0.007(3) C9 0.032(3) 0.039(4) 0.042(3) 0.008(3) 0.019(3) 0.016(3) C10 0.031(3) 0.038(4) 0.040(3) 0.011(3) 0.019(3) 0.013(3) C11 0.025(3) 0.044(4) 0.043(3) 0.013(3) 0.020(3) 0.010(3) O12 0.032(2) 0.043(3) 0.066(3) 0.009(2) 0.034(2) 0.011(2) C13 0.026(3) 0.033(3) 0.060(4) 0.007(3) 0.026(3) 0.008(3) C14 0.027(3) 0.040(4) 0.046(4) 0.013(3) 0.019(3) 0.011(3) C15 0.021(3) 0.040(4) 0.042(3) 0.014(3) 0.012(3) 0.010(3) C16 0.033(3) 0.035(3) 0.056(4) 0.014(3) 0.031(3) 0.014(3) C17 0.028(3) 0.030(3) 0.047(4) 0.008(3) 0.019(3) 0.005(3) C18 0.028(3) 0.076(5) 0.052(4) -0.003(4) 0.018(3) 0.014(3) C19 0.035(4) 0.069(5) 0.053(4) 0.003(4) 0.027(3) 0.012(3) C20 0.028(3) 0.041(4) 0.048(4) 0.008(3) 0.020(3) 0.007(3) O21` 0.029(2) 0.043(3) 0.057(3) 0.003(2) 0.023(2) 0.0085(19) O22 0.029(2) 0.106(5) 0.052(3) -0.003(3) 0.016(2) 0.013(3) O23 0.034(2) 0.035(3) 0.068(3) 0.010(2) 0.031(2) 0.0113(19) C24 0.029(3) 0.039(4) 0.059(4) 0.003(3) 0.023(3) 0.008(3) C25 0.041(4) 0.032(4) 0.066(4) 0.007(3) 0.034(3) 0.013(3) C26 0.037(4) 0.043(4) 0.070(5) 0.011(4) 0.015(4) 0.013(3) C27 0.034(4) 0.043(4) 0.070(5) 0.010(4) 0.015(3) 0.008(3) C28 0.038(4) 0.039(4) 0.058(4) 0.006(3) 0.025(3) 0.013(3) C29 0.040(4) 0.044(4) 0.064(5) 0.011(4) 0.018(3) 0.007(3) C30 0.032(4) 0.068(5) 0.054(4) 0.020(4) 0.012(3) 0.022(4) C31 0.032(4) 0.043(4) 0.071(5) 0.009(4) 0.027(4) 0.016(3) O32 0.055(3) 0.046(3) 0.055(3) 0.012(2) 0.019(3) 0.012(2) O33 0.032(3) 0.044(3) 0.083(4) 0.016(3) 0.017(3) 0.006(2) O34 0.039(2) 0.023(2) 0.054(3) 0.0079(19) 0.028(2) 0.0113(18) O35 0.027(2) 0.035(2) 0.060(3) 0.009(2) 0.025(2) 0.0079(18) C36 0.026(3) 0.045(4) 0.032(3) 0.006(3) 0.009(3) 0.015(3) C37 0.029(3) 0.028(3) 0.049(4) 0.004(3) 0.015(3) 0.006(3) C38 0.033(3) 0.033(4) 0.073(5) 0.002(3) 0.036(3) 0.009(3) C39 0.047(4) 0.023(3) 0.089(5) 0.005(3) 0.042(4) 0.002(3) C40 0.041(4) 0.032(4) 0.094(6) 0.007(4) 0.046(4) 0.009(3) C41 0.034(3) 0.034(4) 0.069(4) 0.005(3) 0.032(3) 0.010(3) C42 0.028(3) 0.026(3) 0.057(4) 0.008(3) 0.018(3) 0.007(3) O43 0.035(2) 0.035(3) 0.095(4) 0.000(2) 0.042(3) 0.007(2) C44 0.029(3) 0.035(4) 0.062(4) 0.011(3) 0.023(3) 0.008(3) C45 0.021(3) 0.040(4) 0.059(4) 0.008(3) 0.022(3) 0.009(3) C46 0.031(3) 0.045(4) 0.040(3) 0.006(3) 0.016(3) 0.008(3) C47 0.031(3) 0.055(4) 0.038(3) 0.010(3) 0.017(3) 0.015(3) C48 0.025(3) 0.045(4) 0.045(4) 0.008(3) 0.023(3) 0.013(3) C49 0.029(3) 0.038(4) 0.052(4) -0.009(3) 0.016(3) 0.000(3) C50 0.035(4) 0.053(4) 0.053(4) -0.007(3) 0.024(3) 0.002(3) C51 0.031(3) 0.022(3) 0.055(4) 0.008(3) 0.018(3) 0.009(3) O52 0.027(2) 0.042(3) 0.042(2) 0.0094(19) 0.0205(19) 0.0132(18) O53 0.029(2) 0.062(3) 0.047(3) -0.003(2) 0.019(2) 0.006(2) O54 0.057(3) 0.035(3) 0.136(5) 0.015(3) 0.070(3) 0.013(2) C55 0.072(5) 0.030(4) 0.143(8) 0.015(5) 0.071(6) 0.018(4) C56 0.057(5) 0.032(4) 0.102(6) 0.012(4) 0.054(5) 0.009(4) C57 0.074(6) 0.032(4) 0.129(8) 0.032(5) 0.070(6) 0.019(4) C58 0.048(4) 0.050(5) 0.081(5) 0.014(4) 0.039(4) 0.016(4) C59 0.044(4) 0.034(4) 0.062(4) 0.009(3) 0.030(3) 0.014(3) C60 0.056(5) 0.047(4) 0.055(4) 0.005(3) 0.029(4) 0.007(4) C61 0.058(5) 0.038(4) 0.076(5) 0.001(4) 0.035(4) 0.000(4) C62 0.033(4) 0.032(4) 0.066(5) 0.008(3) 0.028(3) 0.011(3) O63 0.056(3) 0.040(3) 0.057(3) 0.011(2) 0.031(3) 0.019(2) O64 0.037(3) 0.048(3) 0.075(3) 0.023(3) 0.018(3) 0.006(2) N65 0.033(3) 0.043(3) 0.042(3) 0.007(2) 0.020(2) 0.013(2) C66 0.025(3) 0.053(4) 0.040(4) 0.004(3) 0.016(3) 0.008(3) C67 0.035(3) 0.033(3) 0.050(4) 0.005(3) 0.023(3) 0.002(3) C68 0.031(3) 0.047(4) 0.035(3) 0.004(3) 0.017(3) 0.011(3) C69 0.032(3) 0.043(4) 0.040(4) 0.002(3) 0.015(3) 0.007(3) C70 0.039(4) 0.026(3) 0.046(4) 0.004(3) 0.016(3) 0.006(3) C71 0.032(3) 0.043(4) 0.037(3) 0.004(3) 0.019(3) 0.008(3) C72 0.028(3) 0.037(4) 0.047(4) 0.007(3) 0.014(3) 0.011(3) C73 0.029(3) 0.038(4) 0.048(4) 0.000(3) 0.016(3) 0.006(3) N74 0.030(3) 0.050(4) 0.046(3) 0.011(3) 0.019(2) 0.010(3) C75 0.026(3) 0.063(5) 0.053(4) 0.015(4) 0.008(3) 0.001(3) C76 0.031(3) 0.066(5) 0.046(4) 0.028(3) 0.016(3) 0.005(3) N77 0.038(3) 0.043(3) 0.054(3) 0.011(3) 0.011(3) 0.011(3) C78 0.039(4) 0.054(5) 0.061(5) 0.002(4) 0.018(3) 0.018(3) C79 0.049(4) 0.044(4) 0.088(6) 0.005(4) 0.038(4) 0.013(3) N80 0.124(7) 0.038(4) 0.058(4) 0.006(3) 0.020(4) 0.029(4) C81 0.048(5) 0.071(6) 0.099(7) 0.019(5) 0.031(5) 0.021(4) C82 0.094(7) 0.052(5) 0.113(8) 0.017(5) 0.068(6) 0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O53 2.306(4) 1_655 ? Cd1 O34 2.325(4) . ? Cd1 O63 2.334(5) 1_545 ? Cd1 N74 2.346(5) . ? Cd1 O64 2.384(5) 1_545 ? Cd1 O35 2.439(4) . ? Cd1 O52 2.446(4) 1_655 ? Cd1 C62 2.687(7) 1_545 ? Cd1 C51 2.714(6) 1_655 ? Cd1 C36 2.719(6) . ? Cd2 N65 2.307(5) . ? Cd2 O4 2.323(4) . ? Cd2 O22 2.353(4) 1_455 ? Cd2 O32 2.364(5) 1_565 ? Cd2 O33 2.372(5) 1_565 ? Cd2 O21` 2.393(4) 1_455 ? Cd2 O3 2.564(4) . ? Cd2 C20 2.723(6) 1_455 ? Cd2 C31 2.732(7) 1_565 ? O3 C5 1.262(7) . ? O4 C5 1.250(7) . ? C5 C6 1.516(8) . ? C6 C11 1.392(8) . ? C6 C7 1.401(8) . ? C7 C8 1.394(8) . ? C7 H7 0.9500 . ? C8 C9 1.376(9) . ? C8 O12 1.382(6) . ? C9 C10 1.387(8) . ? C9 H9 0.9500 . ? C10 O23 1.365(7) . ? C10 C11 1.391(8) . ? C11 H11 0.9500 . ? O12 C13 1.445(7) . ? C13 C14 1.509(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.376(8) . ? C14 C19 1.384(9) . ? C15 C16 1.399(8) . ? C15 H15 0.9500 . ? C16 C17 1.385(8) . ? C16 H16 0.9500 . ? C17 C18 1.393(9) . ? C17 C20 1.493(8) . ? C18 C19 1.382(8) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 O22 1.249(7) . ? C20 O21` 1.272(7) . ? C20 Cd2 2.723(6) 1_655 ? O21` Cd2 2.393(4) 1_655 ? O22 Cd2 2.353(4) 1_655 ? O23 C24 1.447(7) . ? C24 C25 1.465(9) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C30 1.401(9) . ? C25 C26 1.404(9) . ? C26 C27 1.379(10) . ? C26 H26 0.9500 . ? C27 C28 1.419(9) . ? C27 H27 0.9500 . ? C28 C29 1.394(10) . ? C28 C31 1.450(10) . ? C29 C30 1.381(10) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 O32 1.272(8) . ? C31 O33 1.280(8) . ? C31 Cd2 2.732(7) 1_545 ? O32 Cd2 2.364(5) 1_545 ? O33 Cd2 2.372(5) 1_545 ? O34 C36 1.247(7) . ? O35 C36 1.281(7) . ? C36 C37 1.482(8) . ? C37 C38 1.374(9) . ? C37 C42 1.405(8) . ? C38 C39 1.404(8) . ? C38 H38 0.9500 . ? C39 C40 1.373(9) . ? C39 O54 1.381(8) . ? C40 C41 1.371(9) . ? C40 H40 0.9500 . ? C41 O43 1.371(7) . ? C41 C42 1.372(8) . ? C42 H42 0.9500 . ? O43 C44 1.438(7) . ? C44 C45 1.499(8) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C50 1.383(9) . ? C45 C46 1.407(8) . ? C46 C47 1.390(8) . ? C46 H46 0.9500 . ? C47 C48 1.374(8) . ? C47 H47 0.9500 . ? C48 C49 1.387(8) . ? C48 C51 1.511(8) . ? C49 C50 1.403(8) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 O52 1.255(7) . ? C51 O53 1.272(7) . ? C51 Cd1 2.714(6) 1_455 ? O52 Cd1 2.446(4) 1_455 ? O53 Cd1 2.306(4) 1_455 ? O54 C55 1.437(8) . ? C55 C56 1.508(10) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C61 1.387(11) . ? C56 C57 1.423(11) . ? C57 C58 1.374(10) . ? C57 H57 0.9500 . ? C58 C59 1.394(10) . ? C58 H58 0.9500 . ? C59 C60 1.382(9) . ? C59 C62 1.510(9) . ? C60 C61 1.381(10) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C62 O63 1.244(8) . ? C62 O64 1.268(8) . ? C62 Cd1 2.687(7) 1_565 ? O63 Cd1 2.334(5) 1_565 ? O64 Cd1 2.384(5) 1_565 ? N65 C70 1.337(8) . ? N65 C66 1.352(8) . ? C66 C67 1.376(9) . ? C66 H66 0.9500 . ? C67 C68 1.385(8) . ? C67 H67 0.9500 . ? C68 C69 1.410(9) . ? C68 C71 1.478(9) . ? C69 C70 1.376(9) . ? C69 H69 0.9500 . ? C70 H70 0.9500 . ? C71 C72 1.386(9) . ? C71 C76 1.397(9) . ? C72 C73 1.380(9) . ? C72 H72 0.9500 . ? C73 N74 1.330(8) . ? C73 H73 0.9500 . ? N74 C75 1.328(9) . ? C75 C76 1.378(9) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? N77 C79 1.477(9) . ? N77 C78 1.486(8) . ? N77 H77A 0.9200 . ? N77 H77B 0.9200 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? N80 C82 1.433(11) . ? N80 C81 1.428(10) . ? N80 H80A 0.9200 . ? N80 H80B 0.9200 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? 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 O53 Cd1 O34 154.91(16) 1_655 . ? O53 Cd1 O63 110.53(15) 1_655 1_545 ? O34 Cd1 O63 92.21(15) . 1_545 ? O53 Cd1 N74 89.61(17) 1_655 . ? O34 Cd1 N74 82.79(16) . . ? O63 Cd1 N74 82.51(18) 1_545 . ? O53 Cd1 O64 105.75(17) 1_655 1_545 ? O34 Cd1 O64 95.67(16) . 1_545 ? O63 Cd1 O64 55.66(17) 1_545 1_545 ? N74 Cd1 O64 138.11(18) . 1_545 ? O53 Cd1 O35 100.13(15) 1_655 . ? O34 Cd1 O35 55.05(13) . . ? O63 Cd1 O35 144.36(14) 1_545 . ? N74 Cd1 O35 79.90(17) . . ? O64 Cd1 O35 132.55(16) 1_545 . ? O53 Cd1 O52 55.33(14) 1_655 1_655 ? O34 Cd1 O52 117.23(14) . 1_655 ? O63 Cd1 O52 130.50(15) 1_545 1_655 ? N74 Cd1 O52 136.47(17) . 1_655 ? O64 Cd1 O52 81.16(15) 1_545 1_655 ? O35 Cd1 O52 81.94(13) . 1_655 ? O53 Cd1 C62 111.80(17) 1_655 1_545 ? O34 Cd1 C62 93.26(16) . 1_545 ? O63 Cd1 C62 27.55(18) 1_545 1_545 ? N74 Cd1 C62 110.0(2) . 1_545 ? O64 Cd1 C62 28.16(18) 1_545 1_545 ? O35 Cd1 C62 146.27(16) . 1_545 ? O52 Cd1 C62 107.08(17) 1_655 1_545 ? O53 Cd1 C51 27.87(17) 1_655 1_655 ? O34 Cd1 C51 141.07(17) . 1_655 ? O63 Cd1 C51 123.17(16) 1_545 1_655 ? N74 Cd1 C51 114.76(19) . 1_655 ? O64 Cd1 C51 92.51(17) 1_545 1_655 ? O35 Cd1 C51 92.39(15) . 1_655 ? O52 Cd1 C51 27.52(16) 1_655 1_655 ? C62 Cd1 C51 110.66(18) 1_545 1_655 ? O53 Cd1 C36 127.70(18) 1_655 . ? O34 Cd1 C36 27.23(16) . . ? O63 Cd1 C36 117.39(17) 1_545 . ? N74 Cd1 C36 77.40(17) . . ? O64 Cd1 C36 117.65(18) 1_545 . ? O35 Cd1 C36 28.09(16) . . ? O52 Cd1 C36 102.74(15) 1_655 . ? C62 Cd1 C36 120.31(19) 1_545 . ? C51 Cd1 C36 119.14(18) 1_655 . ? N65 Cd2 O4 84.63(16) . . ? N65 Cd2 O22 85.81(17) . 1_455 ? O4 Cd2 O22 160.50(19) . 1_455 ? N65 Cd2 O32 87.49(18) . 1_565 ? O4 Cd2 O32 89.42(16) . 1_565 ? O22 Cd2 O32 107.11(18) 1_455 1_565 ? N65 Cd2 O33 143.01(18) . 1_565 ? O4 Cd2 O33 96.13(16) . 1_565 ? O22 Cd2 O33 101.72(18) 1_455 1_565 ? O32 Cd2 O33 55.59(16) 1_565 1_565 ? N65 Cd2 O21` 127.70(17) . 1_455 ? O4 Cd2 O21` 120.15(14) . 1_455 ? O22 Cd2 O21` 55.10(15) 1_455 1_455 ? O32 Cd2 O21` 132.98(16) 1_565 1_455 ? O33 Cd2 O21` 83.65(16) 1_565 1_455 ? N65 Cd2 O3 81.64(16) . . ? O4 Cd2 O3 53.50(14) . . ? O22 Cd2 O3 108.24(17) 1_455 . ? O32 Cd2 O3 142.01(15) 1_565 . ? O33 Cd2 O3 127.93(16) 1_565 . ? O21` Cd2 O3 80.11(13) 1_455 . ? N65 Cd2 C20 107.89(18) . 1_455 ? O4 Cd2 C20 145.21(17) . 1_455 ? O22 Cd2 C20 27.26(17) 1_455 1_455 ? O32 Cd2 C20 122.64(18) 1_565 1_455 ? O33 Cd2 C20 92.43(18) 1_565 1_455 ? O21` Cd2 C20 27.85(16) 1_455 1_455 ? O3 Cd2 C20 95.32(16) . 1_455 ? N65 Cd2 C31 115.2(2) . 1_565 ? O4 Cd2 C31 92.15(17) . 1_565 ? O22 Cd2 C31 107.31(19) 1_455 1_565 ? O32 Cd2 C31 27.71(18) 1_565 1_565 ? O33 Cd2 C31 27.91(18) 1_565 1_565 ? O21` Cd2 C31 109.35(18) 1_455 1_565 ? O3 Cd2 C31 141.56(16) . 1_565 ? C20 Cd2 C31 110.06(18) 1_455 1_565 ? C5 O3 Cd2 85.8(4) . . ? C5 O4 Cd2 97.3(3) . . ? O4 C5 O3 123.2(5) . . ? O4 C5 C6 118.0(5) . . ? O3 C5 C6 118.8(6) . . ? C11 C6 C7 121.5(5) . . ? C11 C6 C5 120.7(5) . . ? C7 C6 C5 117.7(6) . . ? C8 C7 C6 117.5(6) . . ? C8 C7 H7 121.2 . . ? C6 C7 H7 121.2 . . ? C9 C8 O12 114.7(5) . . ? C9 C8 C7 121.6(5) . . ? O12 C8 C7 123.7(6) . . ? C8 C9 C10 120.1(5) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? O23 C10 C9 124.8(5) . . ? O23 C10 C11 115.1(5) . . ? C9 C10 C11 120.0(6) . . ? C10 C11 C6 119.1(5) . . ? C10 C11 H11 120.4 . . ? C6 C11 H11 120.4 . . ? C8 O12 C13 117.0(4) . . ? O12 C13 C14 107.2(4) . . ? O12 C13 H13A 110.3 . . ? C14 C13 H13A 110.3 . . ? O12 C13 H13B 110.3 . . ? C14 C13 H13B 110.3 . . ? H13A C13 H13B 108.5 . . ? C15 C14 C19 119.7(5) . . ? C15 C14 C13 119.5(5) . . ? C19 C14 C13 120.8(5) . . ? C14 C15 C16 119.7(6) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C17 C16 C15 120.9(6) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 118.8(5) . . ? C16 C17 C20 120.8(5) . . ? C18 C17 C20 120.3(6) . . ? C19 C18 C17 120.1(6) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C14 120.8(6) . . ? C18 C19 H19 119.6 . . ? C14 C19 H19 119.6 . . ? O22 C20 O21` 121.1(5) . . ? O22 C20 C17 119.4(5) . . ? O21` C20 C17 119.5(5) . . ? O22 C20 Cd2 59.7(3) . 1_655 ? O21` C20 Cd2 61.5(3) . 1_655 ? C17 C20 Cd2 178.1(4) . 1_655 ? C20 O21` Cd2 90.6(3) . 1_655 ? C20 O22 Cd2 93.1(4) . 1_655 ? C10 O23 C24 117.5(4) . . ? O23 C24 C25 109.1(5) . . ? O23 C24 H24A 109.9 . . ? C25 C24 H24A 109.9 . . ? O23 C24 H24B 109.9 . . ? C25 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? C30 C25 C26 117.3(6) . . ? C30 C25 C24 121.8(6) . . ? C26 C25 C24 120.9(6) . . ? C27 C26 C25 121.2(7) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C26 C27 C28 120.8(7) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C29 C28 C27 118.1(6) . . ? C29 C28 C31 122.1(6) . . ? C27 C28 C31 119.8(6) . . ? C30 C29 C28 120.4(6) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C25 122.2(6) . . ? C29 C30 H30 118.9 . . ? C25 C30 H30 118.9 . . ? O32 C31 O33 119.9(6) . . ? O32 C31 C28 120.1(6) . . ? O33 C31 C28 120.0(7) . . ? O32 C31 Cd2 59.8(4) . 1_545 ? O33 C31 Cd2 60.2(4) . 1_545 ? C28 C31 Cd2 175.6(4) . 1_545 ? C31 O32 Cd2 92.5(4) . 1_545 ? C31 O33 Cd2 91.9(4) . 1_545 ? C36 O34 Cd1 94.3(3) . . ? C36 O35 Cd1 88.2(3) . . ? O34 C36 O35 121.3(5) . . ? O34 C36 C37 120.2(5) . . ? O35 C36 C37 118.5(6) . . ? O34 C36 Cd1 58.5(3) . . ? O35 C36 Cd1 63.7(3) . . ? C37 C36 Cd1 169.3(4) . . ? C38 C37 C42 119.8(5) . . ? C38 C37 C36 120.6(6) . . ? C42 C37 C36 119.5(6) . . ? C37 C38 C39 119.2(6) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? C40 C39 O54 124.5(6) . . ? C40 C39 C38 120.5(6) . . ? O54 C39 C38 115.0(6) . . ? C41 C40 C39 119.9(6) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 O43 114.4(5) . . ? C40 C41 C42 120.8(6) . . ? O43 C41 C42 124.7(6) . . ? C41 C42 C37 119.7(6) . . ? C41 C42 H42 120.2 . . ? C37 C42 H42 120.2 . . ? C41 O43 C44 116.9(4) . . ? O43 C44 C45 106.9(5) . . ? O43 C44 H44A 110.3 . . ? C45 C44 H44A 110.3 . . ? O43 C44 H44B 110.3 . . ? C45 C44 H44B 110.3 . . ? H44A C44 H44B 108.6 . . ? C50 C45 C46 120.1(5) . . ? C50 C45 C44 119.5(6) . . ? C46 C45 C44 120.3(6) . . ? C47 C46 C45 118.7(6) . . ? C47 C46 H46 120.6 . . ? C45 C46 H46 120.6 . . ? C48 C47 C46 121.3(6) . . ? C48 C47 H47 119.4 . . ? C46 C47 H47 119.4 . . ? C47 C48 C49 120.1(5) . . ? C47 C48 C51 120.4(5) . . ? C49 C48 C51 119.5(5) . . ? C48 C49 C50 119.6(6) . . ? C48 C49 H49 120.2 . . ? C50 C49 H49 120.2 . . ? C45 C50 C49 120.0(6) . . ? C45 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? O52 C51 O53 122.0(5) . . ? O52 C51 C48 119.8(5) . . ? O53 C51 C48 118.1(6) . . ? O52 C51 Cd1 64.3(3) . 1_455 ? O53 C51 Cd1 57.9(3) . 1_455 ? C48 C51 Cd1 172.3(4) . 1_455 ? C51 O52 Cd1 88.2(3) . 1_455 ? C51 O53 Cd1 94.2(4) . 1_455 ? C39 O54 C55 116.2(5) . . ? O54 C55 C56 107.5(6) . . ? O54 C55 H55A 110.2 . . ? C56 C55 H55A 110.2 . . ? O54 C55 H55B 110.2 . . ? C56 C55 H55B 110.2 . . ? H55A C55 H55B 108.5 . . ? C61 C56 C57 120.4(7) . . ? C61 C56 C55 120.2(8) . . ? C57 C56 C55 119.3(8) . . ? C58 C57 C56 119.3(8) . . ? C58 C57 H57 120.4 . . ? C56 C57 H57 120.4 . . ? C57 C58 C59 119.8(8) . . ? C57 C58 H58 120.1 . . ? C59 C58 H58 120.1 . . ? C60 C59 C58 120.6(7) . . ? C60 C59 C62 119.6(6) . . ? C58 C59 C62 119.7(6) . . ? C61 C60 C59 120.7(7) . . ? C61 C60 H60 119.6 . . ? C59 C60 H60 119.6 . . ? C60 C61 C56 119.1(7) . . ? C60 C61 H61 120.4 . . ? C56 C61 H61 120.4 . . ? O63 C62 O64 122.6(6) . . ? O63 C62 C59 117.5(6) . . ? O64 C62 C59 119.9(6) . . ? O63 C62 Cd1 60.2(3) . 1_565 ? O64 C62 Cd1 62.5(3) . 1_565 ? C59 C62 Cd1 173.1(4) . 1_565 ? C62 O63 Cd1 92.2(4) . 1_565 ? C62 O64 Cd1 89.3(4) . 1_565 ? C70 N65 C66 117.3(5) . . ? C70 N65 Cd2 121.3(4) . . ? C66 N65 Cd2 120.7(4) . . ? N65 C66 C67 123.0(6) . . ? N65 C66 H66 118.5 . . ? C67 C66 H66 118.5 . . ? C66 C67 C68 119.2(6) . . ? C66 C67 H67 120.4 . . ? C68 C67 H67 120.4 . . ? C67 C68 C69 118.5(6) . . ? C67 C68 C71 121.2(6) . . ? C69 C68 C71 120.1(5) . . ? C70 C69 C68 117.9(6) . . ? C70 C69 H69 121.1 . . ? C68 C69 H69 121.1 . . ? N65 C70 C69 124.1(6) . . ? N65 C70 H70 117.9 . . ? C69 C70 H70 117.9 . . ? C72 C71 C76 116.1(6) . . ? C72 C71 C68 121.4(6) . . ? C76 C71 C68 122.5(6) . . ? C73 C72 C71 120.0(6) . . ? C73 C72 H72 120.0 . . ? C71 C72 H72 120.0 . . ? N74 C73 C72 123.1(6) . . ? N74 C73 H73 118.4 . . ? C72 C73 H73 118.4 . . ? C75 N74 C73 117.7(6) . . ? C75 N74 Cd1 120.5(4) . . ? C73 N74 Cd1 120.2(4) . . ? N74 C75 C76 122.7(6) . . ? N74 C75 H75 118.6 . . ? C76 C75 H75 118.6 . . ? C75 C76 C71 120.3(7) . . ? C75 C76 H76 119.9 . . ? C71 C76 H76 119.9 . . ? C79 N77 C78 112.1(6) . . ? C79 N77 H77A 109.2 . . ? C78 N77 H77A 109.2 . . ? C79 N77 H77B 109.2 . . ? C78 N77 H77B 109.2 . . ? H77A N77 H77B 107.9 . . ? N77 C78 H78A 109.5 . . ? N77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? N77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? N77 C79 H79A 109.5 . . ? N77 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? N77 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C82 N80 C81 120.4(7) . . ? C82 N80 H80A 107.2 . . ? C81 N80 H80A 107.2 . . ? C82 N80 H80B 107.2 . . ? C81 N80 H80B 107.2 . . ? H80A N80 H80B 106.9 . . ? N80 C81 H81A 109.5 . . ? N80 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? N80 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? N80 C82 H82A 109.5 . . ? N80 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? N80 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.007 0.500 0.421 1098 349 ' ' _platon_squeeze_details ; There are 8 disordered molecules of the dimethylacetamide solvent per unit-cell trapped in the large solvent-accessible void of the lattice. ; # start Validation Reply Form _vrf_CHEMW01_4 ; PROBLEM: RESPONSE: The disordered DMA solvent (8 molecules per unit-cell) was included in the structural formula, but excluded from the structural model. ; _vrf_CHEMW03_4 ; PROBLEM: RESPONSE: The disordered DMA solvent (8 molecules per unit-cell) was included in the structural formula, but excluded from the structural model. ; # end Validation Reply Form _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.964 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.100 #=========================END======================================