# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 1145 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Furman, Joshua' 'Burwood, Ryan' 'Tang, Min' 'Mikhailovsky, Alexander' 'Cheetham, Tony' _publ_contact_author_name 'Furman, Joshua' _publ_contact_author_email akc30@cam.ac.uk _publ_section_title ; Understanding ligand-centred photoluminescence through flexibility and bonding of anthraquinone inorganic-organic frameworks ; # Attachment '- caaqdc.cif' data_CaAQDC _database_code_depnum_ccdc_archive 'CCDC 801096' #TrackingRef '- caaqdc.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H14 Ca O10' _chemical_formula_weight 406.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 '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 5.960(2) _cell_length_b 7.634(3) _cell_length_c 18.603(7) _cell_angle_alpha 90.145(6) _cell_angle_beta 95.804(6) _cell_angle_gamma 97.105(6) _cell_volume 835.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 80 _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max .5 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 420 _exptl_absorpt_coefficient_mu 0.433 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.856 _exptl_absorpt_correction_T_max 0.878 _exptl_absorpt_process_details ? _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 'Bruker P4' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6129 _diffrn_reflns_av_R_equivalents 0.0684 _diffrn_reflns_av_sigmaI/netI 0.1070 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 26.02 _reflns_number_total 3224 _reflns_number_gt 2131 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3224 _refine_ls_number_parameters 268 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0885 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1015 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 0.912 _refine_ls_restrained_S_all 0.909 _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 Ca1 Ca 0.01213(10) 0.26769(7) 1.04132(3) 0.01654(18) Uani 1 1 d . . . C1 C 0.6884(5) 0.3306(4) 0.78485(17) 0.0226(7) Uani 1 1 d . . . H1 H 0.8315 0.3957 0.7927 0.027 Uiso 1 1 calc R . . C2 C 0.5723(5) 0.2767(3) 0.84306(16) 0.0170(7) Uani 1 1 d . . . C3 C 0.3530(5) 0.1825(4) 0.83117(17) 0.0180(7) Uani 1 1 d . . . C4 C 0.2585(5) 0.1416(4) 0.76142(17) 0.0231(7) Uani 1 1 d . . . H4 H 0.1142 0.0785 0.7536 0.028 Uiso 1 1 calc R . . C5 C 0.3768(5) 0.1938(4) 0.70275(17) 0.0240(7) Uani 1 1 d . . . C6 C 0.2704(6) 0.1454(4) 0.62827(18) 0.0316(8) Uani 1 1 d . . . C7 C 0.3997(6) 0.2041(4) 0.56716(18) 0.0315(8) Uani 1 1 d . . . C8 C 0.3061(6) 0.1657(5) 0.49654(19) 0.0404(9) Uani 1 1 d . . . H8 H 0.1591 0.1075 0.4879 0.049 Uiso 1 1 calc R . . C9 C 0.4297(7) 0.2134(5) 0.4390(2) 0.0505(11) Uani 1 1 d . . . H9 H 0.3654 0.1874 0.3920 0.061 Uiso 1 1 calc R . . C10 C 0.6455(8) 0.2985(5) 0.4511(2) 0.0537(12) Uani 1 1 d . . . H10 H 0.7287 0.3284 0.4123 0.064 Uiso 1 1 calc R . . C11 C 0.7407(7) 0.3403(5) 0.5206(2) 0.0463(10) Uani 1 1 d . . . H11 H 0.8872 0.3997 0.5283 0.056 Uiso 1 1 calc R . . C12 C 0.6196(6) 0.2944(4) 0.57910(18) 0.0320(8) Uani 1 1 d . . . C13 C 0.7244(6) 0.3457(5) 0.65262(19) 0.0350(9) Uani 1 1 d . . . C14 C 0.5935(5) 0.2885(4) 0.71416(17) 0.0244(8) Uani 1 1 d . . . C15 C 0.6889(5) 0.3018(4) 0.91869(17) 0.0168(7) Uani 1 1 d . . . C16 C 0.2163(5) 0.1346(4) 0.89378(16) 0.0176(7) Uani 1 1 d . . . O1 O 0.0841(4) 0.0587(4) 0.61889(14) 0.0555(8) Uani 1 1 d . . . O2 O 0.9125(4) 0.4300(4) 0.66229(14) 0.0578(8) Uani 1 1 d . . . O3 O 0.6881(3) 0.1670(2) 0.95728(11) 0.0231(5) Uani 1 1 d . . . O4 O 0.7935(3) 0.4496(2) 0.93883(11) 0.0232(5) Uani 1 1 d . . . O5 O 0.2042(3) 0.2595(3) 0.93706(11) 0.0261(5) Uani 1 1 d . . . O6 O 0.1237(3) -0.0191(3) 0.89812(12) 0.0290(6) Uani 1 1 d . . . O7 O -0.2439(4) 0.3960(3) 1.10960(14) 0.0285(6) Uani 1 1 d D . . H7A H -0.251(5) 0.497(4) 1.0962(17) 0.034 Uiso 1 1 d D . . H7B H -0.214(5) 0.385(4) 1.1575(19) 0.034 Uiso 1 1 d D . . O8 O 0.3471(4) 0.1697(3) 1.09909(13) 0.0292(6) Uani 1 1 d D . . H8A H 0.472(6) 0.228(4) 1.0913(18) 0.035 Uiso 1 1 d D . . H8B H 0.350(6) 0.073(4) 1.0879(18) 0.035 Uiso 1 1 d D . . O9 O 0.2223(7) 0.6670(5) 0.7472(2) 0.0962(16) Uani 1 1 d D . . H9A H 0.161(9) 0.582(7) 0.716(3) 0.115 Uiso 1 1 d D . . H9B H 0.348(9) 0.692(8) 0.744(3) 0.115 Uiso 1 1 d D . . O10 O 0.6948(8) 0.8097(6) 0.7490(2) 0.0966(14) Uani 1 1 d D . . H10A H 0.690(10) 0.831(8) 0.790(3) 0.116 Uiso 1 1 d D . . H10B H 0.825(9) 0.765(8) 0.753(3) 0.116 Uiso 1 1 d 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 Ca1 0.0188(3) 0.0138(3) 0.0161(4) -0.0009(2) 0.0016(3) -0.0014(2) C1 0.0214(17) 0.0228(16) 0.022(2) 0.0011(14) 0.0020(15) -0.0035(13) C2 0.0194(16) 0.0149(14) 0.0163(18) -0.0005(13) 0.0025(14) -0.0004(12) C3 0.0210(17) 0.0146(14) 0.0180(19) -0.0006(13) 0.0032(14) 0.0001(12) C4 0.0187(17) 0.0261(17) 0.022(2) -0.0023(14) -0.0020(15) -0.0054(13) C5 0.0258(18) 0.0289(17) 0.0158(19) -0.0040(14) 0.0012(15) -0.0016(14) C6 0.037(2) 0.0362(19) 0.019(2) -0.0021(16) 0.0017(17) -0.0041(17) C7 0.039(2) 0.0349(19) 0.019(2) -0.0044(16) 0.0003(17) 0.0000(16) C8 0.049(2) 0.047(2) 0.022(2) -0.0017(18) -0.0033(19) -0.0008(18) C9 0.074(3) 0.058(3) 0.018(2) 0.0016(19) 0.005(2) 0.003(2) C10 0.074(3) 0.062(3) 0.024(2) 0.006(2) 0.020(2) -0.006(2) C11 0.054(3) 0.061(3) 0.021(2) 0.0003(19) 0.012(2) -0.008(2) C12 0.044(2) 0.0335(19) 0.017(2) 0.0007(15) 0.0055(17) -0.0016(17) C13 0.037(2) 0.044(2) 0.022(2) 0.0006(17) 0.0054(17) -0.0042(18) C14 0.0295(19) 0.0265(17) 0.0156(19) -0.0011(14) 0.0017(15) -0.0027(14) C15 0.0114(16) 0.0189(16) 0.0199(19) 0.0000(14) 0.0013(13) 0.0014(12) C16 0.0116(15) 0.0232(16) 0.0170(18) 0.0059(14) -0.0032(13) 0.0014(13) O1 0.0434(17) 0.084(2) 0.0285(17) -0.0115(14) -0.0019(13) -0.0285(16) O2 0.0439(17) 0.086(2) 0.0336(18) -0.0059(15) 0.0104(14) -0.0361(15) O3 0.0278(12) 0.0184(11) 0.0212(13) 0.0041(10) -0.0024(10) -0.0009(9) O4 0.0251(12) 0.0179(11) 0.0237(14) -0.0039(9) -0.0013(10) -0.0057(9) O5 0.0305(13) 0.0268(12) 0.0214(14) -0.0045(10) 0.0079(10) 0.0014(10) O6 0.0313(13) 0.0207(12) 0.0332(15) 0.0072(10) 0.0042(11) -0.0054(10) O7 0.0368(14) 0.0213(12) 0.0284(15) 0.0012(12) 0.0095(12) 0.0022(11) O8 0.0237(13) 0.0200(12) 0.0416(17) -0.0012(11) -0.0010(12) -0.0026(10) O9 0.150(4) 0.081(3) 0.041(2) -0.0071(18) -0.004(3) -0.041(3) O10 0.128(4) 0.113(3) 0.045(2) -0.001(2) 0.010(3) 0.000(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 Ca1 O6 2.311(2) 2_557 ? Ca1 O4 2.329(2) 2_667 ? Ca1 O5 2.354(2) . ? Ca1 O8 2.374(2) . ? Ca1 O7 2.378(2) . ? Ca1 O3 2.405(2) 1_455 ? Ca1 O4 2.687(2) 1_455 ? Ca1 C15 2.867(3) 1_455 ? Ca1 Ca1 3.8826(17) 2_567 ? Ca1 Ca1 4.3434(19) 2_557 ? Ca1 H7A 2.75(3) . ? Ca1 H8B 2.72(3) . ? C1 C2 1.380(4) . ? C1 C14 1.398(4) . ? C1 H1 0.9300 . ? C2 C3 1.408(4) . ? C2 C15 1.506(4) . ? C3 C4 1.380(4) . ? C3 C16 1.508(4) . ? C4 C5 1.391(4) . ? C4 H4 0.9300 . ? C5 C14 1.396(4) . ? C5 C6 1.490(4) . ? C6 O1 1.217(4) . ? C6 C7 1.477(5) . ? C7 C8 1.390(5) . ? C7 C12 1.399(5) . ? C8 C9 1.384(5) . ? C8 H8 0.9300 . ? C9 C10 1.364(5) . ? C9 H9 0.9300 . ? C10 C11 1.377(5) . ? C10 H10 0.9300 . ? C11 C12 1.388(5) . ? C11 H11 0.9300 . ? C12 C13 1.476(5) . ? C13 O2 1.218(4) . ? C13 C14 1.486(4) . ? C15 O3 1.256(3) . ? C15 O4 1.257(3) . ? C15 Ca1 2.867(3) 1_655 ? C16 O6 1.240(3) . ? C16 O5 1.260(3) . ? O3 Ca1 2.405(2) 1_655 ? O4 Ca1 2.329(2) 2_667 ? O4 Ca1 2.687(2) 1_655 ? O6 Ca1 2.311(2) 2_557 ? O7 H7A 0.82(3) . ? O7 H7B 0.90(3) . ? O8 H8A 0.84(3) . ? O8 H8B 0.77(3) . ? O9 H9A 0.88(5) . ? O9 H9B 0.76(5) . ? O10 H10A 0.78(5) . ? O10 H10B 0.88(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Ca1 O4 141.88(8) 2_557 2_667 ? O6 Ca1 O5 123.82(8) 2_557 . ? O4 Ca1 O5 86.09(7) 2_667 . ? O6 Ca1 O8 76.57(8) 2_557 . ? O4 Ca1 O8 85.18(8) 2_667 . ? O5 Ca1 O8 83.50(8) . . ? O6 Ca1 O7 81.33(8) 2_557 . ? O4 Ca1 O7 79.80(8) 2_667 . ? O5 Ca1 O7 150.30(8) . . ? O8 Ca1 O7 120.75(9) . . ? O6 Ca1 O3 81.54(8) 2_557 1_455 ? O4 Ca1 O3 129.78(7) 2_667 1_455 ? O5 Ca1 O3 82.27(8) . 1_455 ? O8 Ca1 O3 140.81(8) . 1_455 ? O7 Ca1 O3 86.89(8) . 1_455 ? O6 Ca1 O4 129.09(8) 2_557 1_455 ? O4 Ca1 O4 78.82(8) 2_667 1_455 ? O5 Ca1 O4 72.68(7) . 1_455 ? O8 Ca1 O4 151.99(8) . 1_455 ? O7 Ca1 O4 78.99(8) . 1_455 ? O3 Ca1 O4 51.06(6) 1_455 1_455 ? O6 Ca1 C15 106.75(8) 2_557 1_455 ? O4 Ca1 C15 104.60(8) 2_667 1_455 ? O5 Ca1 C15 72.43(8) . 1_455 ? O8 Ca1 C15 153.06(8) . 1_455 ? O7 Ca1 C15 85.96(9) . 1_455 ? O3 Ca1 C15 25.70(7) 1_455 1_455 ? O4 Ca1 C15 25.89(7) 1_455 1_455 ? O6 Ca1 Ca1 155.29(6) 2_557 2_567 ? O4 Ca1 Ca1 42.77(5) 2_667 2_567 ? O5 Ca1 Ca1 75.70(5) . 2_567 ? O8 Ca1 Ca1 124.10(6) . 2_567 ? O7 Ca1 Ca1 76.21(6) . 2_567 ? O3 Ca1 Ca1 87.07(5) 1_455 2_567 ? O4 Ca1 Ca1 36.05(4) 1_455 2_567 ? C15 Ca1 Ca1 61.87(6) 1_455 2_567 ? O6 Ca1 Ca1 56.14(6) 2_557 2_557 ? O4 Ca1 Ca1 149.67(6) 2_667 2_557 ? O5 Ca1 Ca1 68.31(5) . 2_557 ? O8 Ca1 Ca1 76.29(6) . 2_557 ? O7 Ca1 Ca1 130.36(6) . 2_557 ? O3 Ca1 Ca1 64.52(5) 1_455 2_557 ? O4 Ca1 Ca1 107.12(5) 1_455 2_557 ? C15 Ca1 Ca1 83.56(6) 1_455 2_557 ? Ca1 Ca1 Ca1 136.18(4) 2_567 2_557 ? O6 Ca1 H7A 97.6(7) 2_557 . ? O4 Ca1 H7A 67.6(7) 2_667 . ? O5 Ca1 H7A 134.8(7) . . ? O8 Ca1 H7A 127.3(7) . . ? O7 Ca1 H7A 16.4(6) . . ? O3 Ca1 H7A 87.3(7) 1_455 . ? O4 Ca1 H7A 66.7(7) 1_455 . ? C15 Ca1 H7A 79.3(7) 1_455 . ? Ca1 Ca1 H7A 59.9(7) 2_567 . ? Ca1 Ca1 H7A 142.5(7) 2_557 . ? O6 Ca1 H8B 68.2(7) 2_557 . ? O4 Ca1 H8B 99.6(7) 2_667 . ? O5 Ca1 H8B 78.9(7) . . ? O8 Ca1 H8B 15.5(7) . . ? O7 Ca1 H8B 129.0(7) . . ? O3 Ca1 H8B 125.3(7) 1_455 . ? O4 Ca1 H8B 151.6(7) 1_455 . ? C15 Ca1 H8B 140.7(7) 1_455 . ? Ca1 Ca1 H8B 135.1(7) 2_567 . ? Ca1 Ca1 H8B 60.8(7) 2_557 . ? H7A Ca1 H8B 139.2(10) . . ? C2 C1 C14 120.8(3) . . ? C2 C1 H1 119.6 . . ? C14 C1 H1 119.6 . . ? C1 C2 C3 119.7(3) . . ? C1 C2 C15 120.0(3) . . ? C3 C2 C15 120.0(3) . . ? C4 C3 C2 119.6(3) . . ? C4 C3 C16 119.9(3) . . ? C2 C3 C16 120.5(3) . . ? C3 C4 C5 120.7(3) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C14 119.9(3) . . ? C4 C5 C6 119.2(3) . . ? C14 C5 C6 120.9(3) . . ? O1 C6 C7 121.7(3) . . ? O1 C6 C5 120.5(3) . . ? C7 C6 C5 117.8(3) . . ? C8 C7 C12 118.9(3) . . ? C8 C7 C6 120.1(3) . . ? C12 C7 C6 121.0(3) . . ? C9 C8 C7 120.5(4) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C10 C9 C8 120.2(4) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 120.3(4) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C12 120.5(4) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C7 119.5(3) . . ? C11 C12 C13 119.0(3) . . ? C7 C12 C13 121.5(3) . . ? O2 C13 C12 121.0(3) . . ? O2 C13 C14 121.4(3) . . ? C12 C13 C14 117.6(3) . . ? C5 C14 C1 119.2(3) . . ? C5 C14 C13 121.2(3) . . ? C1 C14 C13 119.5(3) . . ? O3 C15 O4 123.1(3) . . ? O3 C15 C2 116.7(2) . . ? O4 C15 C2 120.0(3) . . ? O3 C15 Ca1 56.10(15) . 1_655 ? O4 C15 Ca1 69.02(16) . 1_655 ? C2 C15 Ca1 159.36(18) . 1_655 ? O6 C16 O5 125.7(3) . . ? O6 C16 C3 118.9(3) . . ? O5 C16 C3 115.4(3) . . ? C15 O3 Ca1 98.20(17) . 1_655 ? C15 O4 Ca1 171.8(2) . 2_667 ? C15 O4 Ca1 85.09(17) . 1_655 ? Ca1 O4 Ca1 101.18(8) 2_667 1_655 ? C16 O5 Ca1 130.90(19) . . ? C16 O6 Ca1 154.7(2) . 2_557 ? Ca1 O7 H7A 108(2) . . ? Ca1 O7 H7B 113(2) . . ? H7A O7 H7B 115(3) . . ? Ca1 O8 H8A 117(2) . . ? Ca1 O8 H8B 109(3) . . ? H8A O8 H8B 108(3) . . ? H9A O9 H9B 112(6) . . ? H10A O10 H10B 97(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 C1 C2 C3 -1.8(4) . . . . ? C14 C1 C2 C15 171.9(3) . . . . ? C1 C2 C3 C4 1.5(4) . . . . ? C15 C2 C3 C4 -172.2(3) . . . . ? C1 C2 C3 C16 -175.3(3) . . . . ? C15 C2 C3 C16 11.0(4) . . . . ? C2 C3 C4 C5 -0.6(4) . . . . ? C16 C3 C4 C5 176.2(3) . . . . ? C3 C4 C5 C14 0.0(5) . . . . ? C3 C4 C5 C6 179.3(3) . . . . ? C4 C5 C6 O1 -1.3(5) . . . . ? C14 C5 C6 O1 178.0(3) . . . . ? C4 C5 C6 C7 179.5(3) . . . . ? C14 C5 C6 C7 -1.2(5) . . . . ? O1 C6 C7 C8 2.2(5) . . . . ? C5 C6 C7 C8 -178.6(3) . . . . ? O1 C6 C7 C12 -176.0(3) . . . . ? C5 C6 C7 C12 3.2(5) . . . . ? C12 C7 C8 C9 1.1(5) . . . . ? C6 C7 C8 C9 -177.2(3) . . . . ? C7 C8 C9 C10 0.1(6) . . . . ? C8 C9 C10 C11 -1.1(6) . . . . ? C9 C10 C11 C12 0.9(6) . . . . ? C10 C11 C12 C7 0.4(6) . . . . ? C10 C11 C12 C13 -178.3(3) . . . . ? C8 C7 C12 C11 -1.3(5) . . . . ? C6 C7 C12 C11 176.9(3) . . . . ? C8 C7 C12 C13 177.3(3) . . . . ? C6 C7 C12 C13 -4.5(5) . . . . ? C11 C12 C13 O2 1.4(5) . . . . ? C7 C12 C13 O2 -177.3(3) . . . . ? C11 C12 C13 C14 -177.7(3) . . . . ? C7 C12 C13 C14 3.6(5) . . . . ? C4 C5 C14 C1 -0.3(4) . . . . ? C6 C5 C14 C1 -179.6(3) . . . . ? C4 C5 C14 C13 179.8(3) . . . . ? C6 C5 C14 C13 0.5(5) . . . . ? C2 C1 C14 C5 1.2(4) . . . . ? C2 C1 C14 C13 -178.9(3) . . . . ? O2 C13 C14 C5 179.2(3) . . . . ? C12 C13 C14 C5 -1.6(5) . . . . ? O2 C13 C14 C1 -0.6(5) . . . . ? C12 C13 C14 C1 178.5(3) . . . . ? C1 C2 C15 O3 -125.6(3) . . . . ? C3 C2 C15 O3 48.1(3) . . . . ? C1 C2 C15 O4 49.8(4) . . . . ? C3 C2 C15 O4 -136.6(3) . . . . ? C1 C2 C15 Ca1 -61.4(6) . . . 1_655 ? C3 C2 C15 Ca1 112.3(5) . . . 1_655 ? C4 C3 C16 O6 51.5(4) . . . . ? C2 C3 C16 O6 -131.8(3) . . . . ? C4 C3 C16 O5 -127.4(3) . . . . ? C2 C3 C16 O5 49.4(4) . . . . ? O4 C15 O3 Ca1 -17.7(3) . . . 1_655 ? C2 C15 O3 Ca1 157.5(2) . . . 1_655 ? O3 C15 O4 Ca1 156.0(11) . . . 2_667 ? C2 C15 O4 Ca1 -19.1(15) . . . 2_667 ? Ca1 C15 O4 Ca1 140.3(13) 1_655 . . 2_667 ? O3 C15 O4 Ca1 15.7(3) . . . 1_655 ? C2 C15 O4 Ca1 -159.4(2) . . . 1_655 ? O6 C16 O5 Ca1 -0.4(4) . . . . ? C3 C16 O5 Ca1 178.40(18) . . . . ? O6 Ca1 O5 C16 16.7(3) 2_557 . . . ? O4 Ca1 O5 C16 171.3(3) 2_667 . . . ? O8 Ca1 O5 C16 85.8(3) . . . . ? O7 Ca1 O5 C16 -127.2(3) . . . . ? O3 Ca1 O5 C16 -57.6(3) 1_455 . . . ? O4 Ca1 O5 C16 -109.2(3) 1_455 . . . ? C15 Ca1 O5 C16 -82.0(3) 1_455 . . . ? Ca1 Ca1 O5 C16 -146.6(3) 2_567 . . . ? Ca1 Ca1 O5 C16 8.0(2) 2_557 . . . ? O5 C16 O6 Ca1 -33.0(6) . . . 2_557 ? C3 C16 O6 Ca1 148.2(3) . . . 2_557 ? 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 O7 H7A O5 0.82(3) 1.96(3) 2.762(3) 169(3) 2_567 O7 H7B O9 0.90(3) 1.82(4) 2.702(5) 166(3) 2_567 O8 H8A O7 0.84(3) 1.99(3) 2.797(3) 159(3) 1_655 O8 H8B O3 0.77(3) 1.99(3) 2.749(3) 168(4) 2_657 O9 H9A O2 0.88(5) 1.95(5) 2.784(4) 155(5) 1_455 O9 H9B O10 0.76(5) 2.14(5) 2.887(6) 168(7) . O10 H10A O8 0.78(5) 2.10(5) 2.868(5) 168(6) 2_667 O10 H10B O9 0.88(5) 2.58(5) 3.456(7) 170(5) 1_655 _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.366 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.077 # Attachment '- cdaqdc_lowtemp.cif' data_CdAQDC _database_code_depnum_ccdc_archive 'CCDC 801097' #TrackingRef '- cdaqdc_lowtemp.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Cadmium anthraquinone-2,3-dicarboxylate' _chemical_melting_point ? _chemical_formula_moiety 'C16 H10 Cd O8, 2(H2 O)' _chemical_formula_sum 'C16 H14 Cd O10' _chemical_formula_weight 478.67 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' 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' _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.81330(10) _cell_length_b 7.4885(2) _cell_length_c 18.6076(6) _cell_angle_alpha 90.4040(10) _cell_angle_beta 95.523(2) _cell_angle_gamma 95.088(2) _cell_volume 803.01(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120 _cell_measurement_reflns_used 16567 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.980 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 1.419 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.750 _exptl_absorpt_correction_T_max 0.932 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type ; Bruker-Nonius APEX II CCD camera on \k-goniostat ; _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3649 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 27.61 _reflns_number_total 3649 _reflns_number_gt 3559 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement ; DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998 ; _computing_data_reduction ; DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1015P)^2^+2.9673P] 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 3649 _refine_ls_number_parameters 264 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1425 _refine_ls_wR_factor_gt 0.1409 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2451(9) 0.3545(7) 0.2399(3) 0.0086(10) Uani 1 1 d . . . H1 H 0.3925 0.4211 0.2475 0.010 Uiso 1 1 calc R . . C2 C 0.1479(10) 0.3110(7) 0.1701(3) 0.0059(10) Uani 1 1 d . . . C3 C -0.0710(10) 0.2155(8) 0.1580(3) 0.0067(10) Uani 1 1 d . . . C4 C -0.1879(10) 0.1615(8) 0.2176(3) 0.0101(11) Uani 1 1 d . . . H4 H -0.3346 0.0939 0.2101 0.012 Uiso 1 1 calc R . . C5 C -0.0935(9) 0.2049(8) 0.2875(3) 0.0089(10) Uani 1 1 d . . . C6 C -0.2248(10) 0.1506(8) 0.3493(3) 0.0105(11) Uani 1 1 d . . . C7 C -0.1178(10) 0.2030(8) 0.4233(3) 0.0109(11) Uani 1 1 d . . . C8 C -0.2464(11) 0.1602(9) 0.4820(3) 0.0160(12) Uani 1 1 d . . . H8 H -0.3988 0.1021 0.4740 0.019 Uiso 1 1 calc R . . C9 C -0.1489(12) 0.2037(9) 0.5522(3) 0.0154(13) Uani 1 1 d . . . H9 H -0.2352 0.1747 0.5920 0.019 Uiso 1 1 calc R . . C10 C 0.0750(11) 0.2895(8) 0.5641(3) 0.0144(11) Uani 1 1 d . . . H10 H 0.1420 0.3169 0.6119 0.017 Uiso 1 1 calc R . . C11 C 0.1999(11) 0.3348(8) 0.5054(3) 0.0127(11) Uani 1 1 d . . . H11 H 0.3518 0.3940 0.5132 0.015 Uiso 1 1 calc R . . C12 C 0.1023(10) 0.2933(8) 0.4352(3) 0.0106(11) Uani 1 1 d . . . C13 C 0.2359(10) 0.3522(8) 0.3735(3) 0.0099(11) Uani 1 1 d . . . C14 C 0.1266(10) 0.3005(7) 0.2990(3) 0.0087(11) Uani 1 1 d . . . C15 C -0.1923(9) 0.1884(7) 0.0840(3) 0.0055(9) Uiso 1 1 d . . . C16 C 0.2818(9) 0.3608(7) 0.1058(3) 0.0068(10) Uani 1 1 d . . . Cd1 Cd 0.51077(6) 0.75432(5) 0.038627(16) 0.00503(15) Uani 1 1 d . . . O5 O -0.4139(8) 0.0636(7) 0.3407(2) 0.0176(9) Uani 1 1 d . . . O1 O -0.2870(7) 0.0361(5) 0.0638(2) 0.0119(8) Uani 1 1 d . . . O2 O -0.2016(7) 0.3272(5) 0.0451(2) 0.0093(8) Uani 1 1 d . . . O6 O 0.4228(7) 0.4392(7) 0.3822(2) 0.0169(9) Uani 1 1 d . . . O1W O 0.8131(10) 0.6946(8) 0.2489(3) 0.0290(12) Uani 1 1 d D . . O3 O 0.2899(7) 0.2353(6) 0.0603(2) 0.0099(8) Uani 1 1 d . . . O2W O 0.2927(9) 0.8333(7) 0.2473(3) 0.0225(11) Uani 1 1 d D . . O4 O 0.3769(7) 0.5170(5) 0.1046(2) 0.0106(8) Uani 1 1 d . . . O3W O 0.8407(7) 0.6631(6) 0.0977(2) 0.0090(8) Uani 1 1 d D . . O4W O 0.2534(7) 0.8844(5) 0.1025(2) 0.0089(8) Uani 1 1 d D . . H1O1 H 0.815(13) 0.666(10) 0.2049(13) 0.011 Uiso 1 1 d D . . H1O2 H 0.164(7) 0.780(9) 0.256(4) 0.011 Uiso 1 1 d D . . H1O3 H 0.962(8) 0.733(8) 0.093(4) 0.011 Uiso 1 1 d D . . H1O4 H 0.260(13) 0.893(10) 0.1481(7) 0.011 Uiso 1 1 d D . . H2O1 H 0.686(7) 0.742(10) 0.250(4) 0.011 Uiso 1 1 d D . . H2O2 H 0.360(12) 0.920(7) 0.273(4) 0.011 Uiso 1 1 d D . . H2O3 H 0.857(13) 0.572(6) 0.072(3) 0.011 Uiso 1 1 d D . . H2O4 H 0.255(13) 0.980(6) 0.078(3) 0.011 Uiso 1 1 d 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 C1 0.006(2) 0.006(2) 0.014(3) 0.000(2) 0.002(2) -0.0005(19) C2 0.009(2) 0.002(2) 0.008(2) 0.0008(19) 0.004(2) 0.0020(19) C3 0.010(2) 0.008(3) 0.004(2) 0.0009(19) 0.0045(19) 0.003(2) C4 0.010(3) 0.007(3) 0.014(3) 0.001(2) 0.007(2) -0.0003(19) C5 0.009(3) 0.008(3) 0.010(3) -0.001(2) 0.001(2) 0.003(2) C6 0.012(3) 0.012(3) 0.008(3) 0.001(2) 0.004(2) 0.001(2) C7 0.010(3) 0.009(3) 0.013(3) 0.002(2) 0.002(2) -0.001(2) C8 0.017(3) 0.017(3) 0.014(3) 0.002(2) 0.004(2) -0.002(2) C9 0.021(3) 0.020(3) 0.006(2) 0.003(2) 0.004(2) 0.001(3) C10 0.019(3) 0.014(3) 0.010(3) -0.002(2) 0.002(2) 0.002(2) C11 0.014(3) 0.012(3) 0.011(3) 0.000(2) -0.001(2) 0.000(2) C12 0.011(3) 0.012(3) 0.010(2) 0.000(2) 0.005(2) 0.002(2) C13 0.009(2) 0.010(3) 0.011(3) 0.000(2) 0.005(2) 0.000(2) C14 0.011(3) 0.006(3) 0.009(2) 0.0016(18) 0.001(2) 0.006(2) C16 0.004(2) 0.006(2) 0.010(2) 0.0033(19) 0.0008(19) 0.0023(18) Cd1 0.0040(2) 0.0047(2) 0.0066(2) -0.00121(19) 0.00160(18) -0.00003(13) O5 0.011(2) 0.027(3) 0.013(2) -0.0010(18) 0.0023(16) -0.0082(17) O1 0.0089(18) 0.0059(19) 0.020(2) -0.0025(16) 0.0019(16) -0.0044(15) O2 0.0080(18) 0.0089(19) 0.0105(19) 0.0019(15) -0.0024(15) 0.0006(15) O6 0.011(2) 0.027(3) 0.011(2) -0.0031(18) 0.0000(16) -0.0055(18) O1W 0.031(3) 0.033(3) 0.022(3) -0.002(2) 0.003(2) 0.001(2) O3 0.0104(18) 0.0098(19) 0.0099(19) 0.0009(14) 0.0033(15) 0.0008(15) O2W 0.030(3) 0.023(3) 0.013(2) -0.0060(19) 0.004(2) -0.010(2) O4 0.0134(19) 0.0057(18) 0.0128(19) -0.0004(15) 0.0045(15) -0.0018(15) O3W 0.0052(17) 0.0066(19) 0.015(2) -0.0022(15) -0.0002(15) 0.0006(14) O4W 0.0094(18) 0.0059(18) 0.013(2) -0.0020(15) 0.0067(15) 0.0018(15) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.391(8) . ? C1 C14 1.397(8) . ? C2 C3 1.401(7) . ? C2 C16 1.519(7) . ? C3 C4 1.400(7) . ? C3 C15 1.489(7) . ? C4 C5 1.387(8) . ? C5 C14 1.406(8) . ? C5 C6 1.479(8) . ? C6 O5 1.223(7) . ? C6 C7 1.490(8) . ? C7 C12 1.390(8) . ? C7 C8 1.404(8) . ? C8 C9 1.397(9) . ? C9 C10 1.396(9) . ? C10 C11 1.396(8) . ? C11 C12 1.394(8) . ? C12 C13 1.495(7) . ? C13 O6 1.213(7) . ? C13 C14 1.500(8) . ? C15 O1 1.260(7) . ? C15 O2 1.272(7) . ? C16 O4 1.250(7) . ? C16 O3 1.268(7) . ? Cd1 O3 2.266(4) 2_665 ? Cd1 O4W 2.277(4) . ? Cd1 O3W 2.278(4) . ? Cd1 O4 2.289(4) . ? Cd1 O2 2.299(4) 2_565 ? Cd1 O1 2.344(4) 1_665 ? O1 Cd1 2.344(4) 1_445 ? O2 Cd1 2.299(4) 2_565 ? O3 Cd1 2.266(4) 2_665 ? 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 C2 C1 C14 120.2(5) . . ? C1 C2 C3 120.7(5) . . ? C1 C2 C16 120.3(5) . . ? C3 C2 C16 119.0(5) . . ? C4 C3 C2 118.7(5) . . ? C4 C3 C15 119.4(5) . . ? C2 C3 C15 121.6(5) . . ? C5 C4 C3 121.3(5) . . ? C4 C5 C14 119.6(5) . . ? C4 C5 C6 119.9(5) . . ? C14 C5 C6 120.6(5) . . ? O5 C6 C5 121.7(5) . . ? O5 C6 C7 120.5(5) . . ? C5 C6 C7 117.9(5) . . ? C12 C7 C8 119.9(5) . . ? C12 C7 C6 121.9(5) . . ? C8 C7 C6 118.2(5) . . ? C9 C8 C7 119.7(6) . . ? C10 C9 C8 120.3(6) . . ? C9 C10 C11 119.7(5) . . ? C12 C11 C10 120.1(6) . . ? C7 C12 C11 120.3(5) . . ? C7 C12 C13 121.0(5) . . ? C11 C12 C13 118.7(5) . . ? O6 C13 C12 122.4(5) . . ? O6 C13 C14 120.8(5) . . ? C12 C13 C14 116.8(5) . . ? C1 C14 C5 119.7(5) . . ? C1 C14 C13 118.5(5) . . ? C5 C14 C13 121.8(5) . . ? O1 C15 O2 123.4(5) . . ? O1 C15 C3 120.2(5) . . ? O2 C15 C3 116.3(5) . . ? O4 C16 O3 127.3(5) . . ? O4 C16 C2 117.3(5) . . ? O3 C16 C2 115.4(5) . . ? O3 Cd1 O4W 146.89(15) 2_665 . ? O3 Cd1 O3W 85.43(15) 2_665 . ? O4W Cd1 O3W 119.42(14) . . ? O3 Cd1 O4 131.11(14) 2_665 . ? O4W Cd1 O4 78.98(14) . . ? O3W Cd1 O4 76.69(15) . . ? O3 Cd1 O2 82.69(16) 2_665 2_565 ? O4W Cd1 O2 86.58(15) . 2_565 ? O3W Cd1 O2 144.67(15) . 2_565 ? O4 Cd1 O2 86.44(15) . 2_565 ? O3 Cd1 O1 83.26(15) 2_665 1_665 ? O4W Cd1 O1 79.81(15) . 1_665 ? O3W Cd1 O1 81.22(15) . 1_665 ? O4 Cd1 O1 136.25(16) . 1_665 ? O2 Cd1 O1 129.78(15) 2_565 1_665 ? C15 O1 Cd1 173.0(4) . 1_445 ? C15 O2 Cd1 102.4(3) . 2_565 ? C16 O3 Cd1 127.0(4) . 2_665 ? C16 O4 Cd1 148.8(4) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.61 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.552 _refine_diff_density_min -2.215 _refine_diff_density_rms 0.250 # Attachment '- cdaqdc_roomtemp.cif' data_CdAQDC2 _database_code_depnum_ccdc_archive 'CCDC 801098' #TrackingRef '- cdaqdc_roomtemp.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Cadmium anthraquinone-2,3-dicarboxylate' _chemical_melting_point ? _chemical_formula_moiety 'C16 Cd H10 O8, 2(H2 O)' _chemical_formula_sum 'C16 H14 Cd O10' _chemical_formula_weight 478.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.8534(17) _cell_length_b 7.504(2) _cell_length_c 18.599(5) _cell_angle_alpha 91.10(2) _cell_angle_beta 95.03(2) _cell_angle_gamma 95.97(2) _cell_volume 809.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298.1 _cell_measurement_reflns_used 1522 _cell_measurement_theta_min 2.9766 _cell_measurement_theta_max 26.3541 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.965 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 1.408 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.88662 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298.1 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_detector_area_resol_mean 16.1183 _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4197 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1056 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 26.53 _reflns_number_total 4197 _reflns_number_gt 3200 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0931P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4197 _refine_ls_number_parameters 268 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0775 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1659 _refine_ls_wR_factor_gt 0.1302 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.833 _refine_ls_shift/su_mean 0.056 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 Cd01 Cd 0.99053(19) -0.25420(12) 0.96143(3) 0.01586(18) Uani 1 1 d . . . C1 C 1.7450(19) -0.1492(13) 1.2392(5) 0.021(2) Uani 1 1 d . . . C2 C 1.642(2) -0.1890(14) 1.1690(5) 0.016(2) Uani 1 1 d . . . C3 C 1.4224(19) -0.2841(13) 1.1579(6) 0.015(2) Uani 1 1 d . . . C4 C 1.308(2) -0.3366(12) 1.2164(5) 0.022(2) Uani 1 1 d . . . C5 C 1.4053(19) -0.2937(13) 1.2865(5) 0.022(2) Uani 1 1 d . . . C6 C 1.2777(19) -0.3489(14) 1.3491(6) 0.025(2) Uani 1 1 d . . . C7 C 1.3809(19) -0.3006(15) 1.4221(5) 0.028(3) Uani 1 1 d . . . C8 C 1.261(2) -0.3407(16) 1.4811(7) 0.044(3) Uani 1 1 d . . . C9 C 1.350(3) -0.2960(18) 1.5500(5) 0.041(3) Uani 1 1 d . . . C10 C 1.576(3) -0.2115(18) 1.5613(7) 0.046(3) Uani 1 1 d . . . C11 C 1.699(2) -0.1663(15) 1.5044(5) 0.036(3) Uani 1 1 d . . . C12 C 1.607(2) -0.2052(16) 1.4337(5) 0.030(2) Uani 1 1 d . . . C13 C 1.7355(19) -0.1462(14) 1.3717(6) 0.027(2) Uani 1 1 d . . . C14 C 1.6241(18) -0.1980(13) 1.2969(5) 0.025(2) Uani 1 1 d . . . C15 C 1.7791(18) -0.1422(12) 1.1054(6) 0.017(2) Uani 1 1 d . . . C16 C 1.3046(18) -0.3126(15) 1.0832(6) 0.021(2) Uani 1 1 d . . . O1 O 1.2113(13) -0.4655(9) 1.0641(4) 0.0243(16) Uani 1 1 d . . . O2 O 1.2934(13) -0.1787(10) 1.0457(4) 0.0191(14) Uani 1 1 d . . . O3 O 1.7889(14) -0.2673(10) 1.0593(4) 0.0267(19) Uani 1 1 d . . . O4 O 1.8691(13) 0.0153(9) 1.1005(4) 0.0286(18) Uani 1 1 d . . . O5 O 1.0931(15) -0.4391(11) 1.3408(4) 0.044(2) Uani 1 1 d . . . O6 O 1.9180(16) -0.0616(12) 1.3799(4) 0.047(2) Uani 1 1 d . . . H1 H 1.8966 -0.0892 1.2467 0.025 Uiso 1 1 calc R . . H4 H 1.1605 -0.4033 1.2091 0.027 Uiso 1 1 calc R . . H8 H 1.1100 -0.4019 1.4736 0.052 Uiso 1 1 calc R . . H9 H 1.2609 -0.3213 1.5896 0.049 Uiso 1 1 calc R . . H11 H 1.8512 -0.1072 1.5131 0.044 Uiso 1 1 calc R . . H10 H 1.6443 -0.1857 1.6091 0.055 Uiso 1 1 calc R . . O1W O 1.2476(16) -0.3863(10) 0.8968(5) 0.0270(19) Uani 1 1 d D . . H1O1 H 1.211(19) -0.496(6) 0.907(6) 0.025 Uiso 1 1 d D . . H2O1 H 1.348(14) -0.298(10) 0.909(6) 0.025 Uiso 1 1 d D . . O2W O 0.6661(14) -0.1619(10) 0.9025(5) 0.0217(18) Uani 1 1 d D . . H1O2 H 0.631(19) -0.056(6) 0.910(6) 0.025 Uiso 1 1 d D . . H2O2 H 0.649(19) -0.212(13) 0.861(2) 0.025 Uiso 1 1 d D . . O3W O 1.313(3) 0.192(2) 1.2479(6) 0.075(4) Uani 1 1 d D . . H1O3 H 1.221(16) 0.100(9) 1.254(6) 0.025 Uiso 1 1 d D . . H2O3 H 1.419(14) 0.248(14) 1.276(5) 0.025 Uiso 1 1 d D . . O4W O 1.790(3) 0.3314(18) 1.2490(6) 0.079(4) Uani 1 1 d D . . H1O4 H 1.829(19) 0.430(8) 1.272(5) 0.025 Uiso 1 1 d D . . H2O4 H 1.78(2) 0.362(13) 1.2051(19) 0.025 Uiso 1 1 d 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 Cd01 0.0145(3) 0.0175(3) 0.0147(3) 0.0004(4) 0.0015(5) -0.00233(19) O1W 0.025(5) 0.030(4) 0.025(4) -0.004(3) 0.007(4) -0.008(4) O2W 0.019(5) 0.016(3) 0.028(4) -0.004(3) 0.000(3) -0.004(3) C3 0.008(5) 0.011(4) 0.026(6) -0.004(4) 0.002(4) -0.004(4) C7 0.032(7) 0.033(6) 0.019(5) 0.007(5) 0.006(4) -0.006(5) C2 0.012(5) 0.024(5) 0.011(5) -0.001(4) 0.003(4) -0.003(4) O3 0.023(5) 0.025(4) 0.031(4) -0.016(3) 0.002(3) -0.003(3) O4 0.026(4) 0.026(4) 0.031(4) 0.010(3) -0.001(3) -0.010(3) C11 0.046(8) 0.045(7) 0.016(5) -0.003(5) 0.004(5) -0.007(6) C15 0.009(5) 0.015(5) 0.027(6) 0.006(4) -0.001(4) 0.006(4) C10 0.064(10) 0.052(7) 0.021(6) 0.004(6) 0.002(6) 0.006(7) C12 0.034(6) 0.032(6) 0.020(5) -0.004(5) -0.003(6) -0.003(5) O6 0.040(5) 0.067(6) 0.024(4) -0.009(4) -0.002(4) -0.027(5) C6 0.024(6) 0.032(5) 0.019(5) 0.001(4) 0.008(4) -0.005(4) C13 0.027(6) 0.032(5) 0.020(5) 0.001(4) 0.001(4) -0.004(5) C9 0.049(9) 0.058(8) 0.013(5) 0.006(6) 0.010(6) -0.010(6) C14 0.025(7) 0.032(6) 0.017(5) -0.010(4) 0.000(4) -0.004(5) C1 0.024(6) 0.018(5) 0.018(6) -0.003(4) -0.002(4) -0.002(4) C4 0.033(7) 0.017(5) 0.015(5) 0.001(4) 0.011(5) -0.011(4) O5 0.038(5) 0.062(5) 0.028(5) 0.003(4) 0.010(4) -0.023(4) C5 0.024(6) 0.029(5) 0.012(5) -0.001(4) 0.000(4) 0.005(4) C8 0.045(8) 0.045(7) 0.041(7) 0.001(6) 0.016(6) -0.008(6) O2 0.015(3) 0.021(3) 0.019(4) 0.000(3) -0.003(3) -0.006(3) O1 0.028(4) 0.023(4) 0.021(4) -0.012(3) 0.005(3) -0.003(3) O3W 0.096(11) 0.084(8) 0.044(6) 0.002(8) 0.024(8) -0.018(7) O4W 0.141(14) 0.059(6) 0.034(6) -0.005(7) 0.020(8) -0.020(8) C16 0.013(6) 0.022(5) 0.024(6) -0.012(5) 0.003(4) -0.009(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd01 O3 2.253(8) 1_455 ? Cd01 O4 2.271(7) 2_857 ? Cd01 O2 2.278(7) . ? Cd01 O2W 2.286(8) . ? Cd01 O1W 2.296(9) . ? Cd01 O1 2.322(7) 2_747 ? C3 C4 1.370(14) . ? C3 C2 1.400(12) . ? C3 C16 1.496(15) . ? C7 C8 1.376(15) . ? C7 C12 1.434(17) . ? C7 C6 1.461(14) . ? C2 C1 1.404(14) . ? C2 C15 1.513(14) . ? O3 C15 1.269(11) . ? O3 Cd01 2.253(8) 1_655 ? O4 C15 1.251(11) . ? O4 Cd01 2.271(7) 2_857 ? C11 C10 1.359(16) . ? C11 C12 1.391(14) . ? C10 C9 1.405(19) . ? C12 C13 1.481(15) . ? O6 C13 1.181(13) . ? C6 O5 1.210(13) . ? C6 C5 1.481(14) . ? C13 C14 1.510(14) . ? C9 C8 1.362(16) . ? C14 C1 1.371(14) . ? C14 C5 1.397(15) . ? C4 C5 1.393(13) . ? O2 C16 1.239(14) . ? O1 C16 1.250(12) . ? O1 Cd01 2.322(7) 2_747 ? 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 Cd01 O4 130.6(3) 1_455 2_857 ? O3 Cd01 O2 82.7(3) 1_455 . ? O4 Cd01 O2 86.5(3) 2_857 . ? O3 Cd01 O2W 85.5(3) 1_455 . ? O4 Cd01 O2W 76.9(3) 2_857 . ? O2 Cd01 O2W 145.4(3) . . ? O3 Cd01 O1W 146.3(3) 1_455 . ? O4 Cd01 O1W 80.0(3) 2_857 . ? O2 Cd01 O1W 86.3(3) . . ? O2W Cd01 O1W 119.6(3) . . ? O3 Cd01 O1 82.6(3) 1_455 2_747 ? O4 Cd01 O1 137.8(3) 2_857 2_747 ? O2 Cd01 O1 128.2(3) . 2_747 ? O2W Cd01 O1 81.9(3) . 2_747 ? O1W Cd01 O1 79.6(3) . 2_747 ? C4 C3 C2 119.2(10) . . ? C4 C3 C16 120.2(10) . . ? C2 C3 C16 120.3(10) . . ? C8 C7 C12 118.5(10) . . ? C8 C7 C6 120.8(11) . . ? C12 C7 C6 120.6(9) . . ? C3 C2 C1 120.5(10) . . ? C3 C2 C15 120.2(10) . . ? C1 C2 C15 119.1(10) . . ? C15 O3 Cd01 127.0(7) . 1_655 ? C15 O4 Cd01 153.7(8) . 2_857 ? C10 C11 C12 121.1(12) . . ? O4 C15 O3 124.5(10) . . ? O4 C15 C2 119.0(9) . . ? O3 C15 C2 116.5(9) . . ? C11 C10 C9 120.7(12) . . ? C11 C12 C7 118.3(10) . . ? C11 C12 C13 121.1(12) . . ? C7 C12 C13 120.6(9) . . ? O5 C6 C7 119.4(10) . . ? O5 C6 C5 121.0(10) . . ? C7 C6 C5 119.5(9) . . ? O6 C13 C12 121.7(10) . . ? O6 C13 C14 120.8(10) . . ? C12 C13 C14 117.4(9) . . ? C8 C9 C10 118.6(11) . . ? C1 C14 C5 120.8(9) . . ? C1 C14 C13 117.9(9) . . ? C5 C14 C13 121.3(9) . . ? C14 C1 C2 119.1(10) . . ? C3 C4 C5 121.0(10) . . ? C4 C5 C14 119.3(10) . . ? C4 C5 C6 120.2(10) . . ? C14 C5 C6 120.5(9) . . ? C9 C8 C7 122.6(12) . . ? C16 O2 Cd01 105.0(6) . . ? C16 O1 Cd01 173.5(7) . 2_747 ? O2 C16 O1 123.9(10) . . ? O2 C16 C3 117.1(9) . . ? O1 C16 C3 118.8(10) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.53 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.497 _refine_diff_density_min -1.244 _refine_diff_density_rms 0.220 # Attachment '- mnaqdc.cif' data_MnAQDCC _database_code_depnum_ccdc_archive 'CCDC 801099' #TrackingRef '- mnaqdc.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Manganese anthraquinone-2,3-dicarboxylate' _chemical_melting_point ? _chemical_formula_moiety 'C16 H10 Mn O8, 2(H2 O)' _chemical_formula_sum 'C16 H14 Mn O10' _chemical_formula_weight 421.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.799(2) _cell_length_b 7.477(3) _cell_length_c 18.493(7) _cell_angle_alpha 89.639(6) _cell_angle_beta 85.173(6) _cell_angle_gamma 83.485(7) _cell_volume 793.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 85 _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 24.06 _exptl_crystal_description 'square plate' _exptl_crystal_colour 'transparent yellow' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.762 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 430 _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.918 _exptl_absorpt_correction_T_max 0.982 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6413 _diffrn_reflns_av_R_equivalents 0.0777 _diffrn_reflns_av_sigmaI/netI 0.1325 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.68 _reflns_number_total 2965 _reflns_number_gt 1810 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1068P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2965 _refine_ls_number_parameters 274 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1359 _refine_ls_R_factor_gt 0.0806 _refine_ls_wR_factor_ref 0.2093 _refine_ls_wR_factor_gt 0.1826 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Mn1 Mn 0.48607(17) 0.75368(14) 1.04047(6) 0.0157(3) Uani 1 1 d . . . C1 C -0.1858(12) 0.8437(10) 0.7845(4) 0.0238(17) Uani 1 1 d . . . H1 H -0.3318 0.9100 0.7907 0.029 Uiso 1 1 calc R . . C2 C -0.0732(10) 0.7944(8) 0.8436(3) 0.0130(14) Uani 1 1 d . . . C3 C 0.1443(11) 0.6930(9) 0.8355(4) 0.0167(15) Uani 1 1 d . . . C4 C 0.2459(12) 0.6461(9) 0.7671(4) 0.0219(16) Uani 1 1 d . . . H4 H 0.3920 0.5797 0.7617 0.026 Uiso 1 1 calc R . . C5 C 0.1272(12) 0.6992(10) 0.7050(4) 0.0232(16) Uani 1 1 d . . . C6 C 0.2343(12) 0.6450(10) 0.6314(4) 0.0266(17) Uani 1 1 d . . . C7 C 0.1067(13) 0.7054(10) 0.5682(4) 0.0274(18) Uani 1 1 d . . . C8 C 0.2026(15) 0.6631(12) 0.4990(4) 0.040(2) Uani 1 1 d . . . H8 H 0.3522 0.6031 0.4919 0.048 Uiso 1 1 calc R . . C9 C 0.0753(17) 0.7102(12) 0.4391(4) 0.044(2) Uani 1 1 d . . . H9 H 0.1408 0.6829 0.3922 0.053 Uiso 1 1 calc R . . C10 C -0.1457(16) 0.7964(12) 0.4501(4) 0.044(2) Uani 1 1 d . . . H10 H -0.2318 0.8257 0.4106 0.053 Uiso 1 1 calc R . . C11 C -0.2430(15) 0.8408(12) 0.5200(4) 0.040(2) Uani 1 1 d . . . H11 H -0.3932 0.8998 0.5271 0.048 Uiso 1 1 calc R . . C12 C -0.1170(14) 0.7975(11) 0.5787(4) 0.0303(18) Uani 1 1 d . . . C13 C -0.2257(12) 0.8534(10) 0.6513(4) 0.0284(18) Uani 1 1 d . . . C14 C -0.0919(12) 0.7991(10) 0.7148(4) 0.0228(16) Uani 1 1 d . . . C15 C -0.1978(11) 0.8308(9) 0.9189(4) 0.0208(16) Uani 1 1 d . . . C16 C 0.2806(11) 0.6410(9) 0.9002(4) 0.0177(15) Uani 1 1 d . . . O1 O -0.4161(9) 0.9432(9) 0.6593(3) 0.0493(17) Uani 1 1 d . . . O2 O 0.4233(9) 0.5537(9) 0.6248(3) 0.0514(18) Uani 1 1 d . . . O3 O -0.2845(8) 0.9862(7) 0.9338(3) 0.0301(13) Uani 1 1 d . . . O4 O -0.2148(8) 0.6984(6) 0.9577(3) 0.0231(12) Uani 1 1 d . . . O5 O 0.2932(8) 0.7686(6) 0.9444(2) 0.0220(11) Uani 1 1 d . . . O6 O 0.3677(8) 0.4840(7) 0.9050(3) 0.0286(12) Uani 1 1 d . . . H7A H 0.741(14) 0.992(3) 1.095(4) 0.040(12) Uiso 1 1 d D . . H7B H 0.718(13) 0.890(9) 1.1482(12) 0.040(12) Uiso 1 1 d D . . O7 O 0.7431(9) 0.8749(7) 1.1006(3) 0.0245(12) Uani 1 1 d D . . H8A H 0.056(10) 0.699(8) 1.067(3) 0.040(12) Uiso 1 1 d D . . H8B H 0.164(12) 0.541(4) 1.077(4) 0.040(12) Uiso 1 1 d D . . O8 O 0.1720(8) 0.6512(7) 1.0946(3) 0.0281(13) Uani 1 1 d D . . H9A H 0.608(16) 0.882(13) 0.281(5) 0.12(5) Uiso 1 1 d D . . H9B H 0.637(17) 0.728(9) 0.257(6) 0.09(5) Uiso 1 1 d D . . O9 O 0.7141(14) 0.8246(11) 0.2474(4) 0.064(2) Uani 1 1 d D . . H10A H 0.18(2) 0.564(5) 0.242(8) 0.14(6) Uiso 1 1 d D . . H10B H 0.040(7) 0.69(2) 0.259(11) 0.24(10) Uiso 1 1 d D . . O10 O 0.1933(14) 0.6813(12) 0.2471(4) 0.065(2) Uani 1 1 d 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 Mn1 0.0152(6) 0.0141(6) 0.0174(6) -0.0010(4) -0.0031(4) 0.0017(4) C1 0.017(4) 0.021(4) 0.032(4) -0.003(3) -0.005(3) 0.007(3) C2 0.013(3) 0.011(3) 0.015(3) 0.002(3) -0.002(3) 0.002(3) C3 0.018(3) 0.015(4) 0.017(4) -0.001(3) -0.001(3) -0.002(3) C4 0.021(4) 0.016(4) 0.026(4) 0.003(3) 0.005(3) 0.006(3) C5 0.030(4) 0.024(4) 0.017(4) 0.001(3) -0.003(3) -0.006(3) C6 0.022(4) 0.026(4) 0.030(4) -0.003(3) 0.001(3) 0.002(3) C7 0.030(4) 0.032(5) 0.020(4) 0.006(3) -0.005(3) 0.001(4) C8 0.046(5) 0.053(6) 0.020(4) -0.002(4) 0.004(4) -0.011(4) C9 0.064(6) 0.041(5) 0.023(5) 0.005(4) -0.001(4) 0.007(5) C10 0.057(6) 0.050(6) 0.023(5) 0.004(4) -0.010(4) 0.007(5) C11 0.037(5) 0.044(6) 0.038(5) 0.002(4) -0.008(4) 0.001(4) C12 0.035(4) 0.035(5) 0.020(4) -0.001(3) -0.004(3) -0.001(4) C13 0.021(4) 0.034(5) 0.028(4) -0.008(4) -0.004(3) 0.009(3) C14 0.027(4) 0.023(4) 0.020(4) 0.001(3) -0.010(3) 0.000(3) C15 0.012(3) 0.016(4) 0.033(4) -0.005(3) -0.006(3) 0.007(3) C16 0.008(3) 0.021(4) 0.023(4) 0.007(3) -0.001(3) 0.001(3) O1 0.034(3) 0.074(5) 0.033(3) -0.003(3) -0.009(3) 0.027(3) O2 0.034(3) 0.080(5) 0.033(3) -0.008(3) -0.003(3) 0.026(3) O3 0.017(3) 0.022(3) 0.048(3) -0.015(2) 0.003(2) 0.006(2) O4 0.021(3) 0.022(3) 0.025(3) 0.000(2) 0.002(2) 0.001(2) O5 0.025(3) 0.025(3) 0.018(3) -0.001(2) -0.009(2) -0.002(2) O6 0.026(3) 0.024(3) 0.035(3) 0.004(2) -0.010(2) 0.004(2) O7 0.030(3) 0.022(3) 0.022(3) 0.000(2) -0.007(2) 0.000(2) O8 0.021(3) 0.025(3) 0.037(3) -0.002(2) 0.000(2) 0.004(2) O9 0.085(5) 0.062(5) 0.038(4) -0.003(4) 0.004(4) 0.012(5) O10 0.073(5) 0.074(6) 0.046(4) -0.009(4) -0.006(4) 0.000(4) _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 Mn1 O6 2.162(5) 2_667 ? Mn1 O5 2.174(5) . ? Mn1 O3 2.185(5) 2_577 ? Mn1 O7 2.208(5) . ? Mn1 O8 2.215(5) . ? Mn1 O4 2.218(5) 1_655 ? C1 C2 1.348(9) . ? C1 C14 1.383(9) . ? C1 H1 0.9300 . ? C2 C3 1.393(9) . ? C2 C15 1.526(9) . ? C3 C4 1.380(9) . ? C3 C16 1.513(9) . ? C4 C5 1.420(9) . ? C4 H4 0.9300 . ? C5 C14 1.397(10) . ? C5 C6 1.486(10) . ? C6 O2 1.221(8) . ? C6 C7 1.477(10) . ? C7 C8 1.376(10) . ? C7 C12 1.397(10) . ? C8 C9 1.403(11) . ? C8 H8 0.9300 . ? C9 C10 1.368(12) . ? C9 H9 0.9300 . ? C10 C11 1.393(11) . ? C10 H10 0.9300 . ? C11 C12 1.375(11) . ? C11 H11 0.9300 . ? C12 C13 1.476(10) . ? C13 O1 1.224(8) . ? C13 C14 1.492(10) . ? C15 O4 1.227(8) . ? C15 O3 1.236(8) . ? C16 O6 1.229(8) . ? C16 O5 1.272(8) . ? O3 Mn1 2.185(5) 2_577 ? O4 Mn1 2.218(5) 1_455 ? O6 Mn1 2.162(5) 2_667 ? O7 H7A 0.88(2) . ? O7 H7B 0.89(2) . ? O8 H8A 0.91(2) . ? O8 H8B 0.89(2) . ? O9 H9A 0.90(2) . ? O9 H9B 0.90(2) . ? O10 H10A 0.89(2) . ? O10 H10B 0.89(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Mn1 O5 128.19(19) 2_667 . ? O6 Mn1 O3 139.7(2) 2_667 2_577 ? O5 Mn1 O3 83.62(19) . 2_577 ? O6 Mn1 O7 80.82(19) 2_667 . ? O5 Mn1 O7 145.88(19) . . ? O3 Mn1 O7 81.38(19) 2_577 . ? O6 Mn1 O8 77.69(19) 2_667 . ? O5 Mn1 O8 84.82(19) . . ? O3 Mn1 O8 82.25(19) 2_577 . ? O7 Mn1 O8 122.9(2) . . ? O6 Mn1 O4 86.14(18) 2_667 1_655 ? O5 Mn1 O4 81.69(18) . 1_655 ? O3 Mn1 O4 127.04(19) 2_577 1_655 ? O7 Mn1 O4 83.24(18) . 1_655 ? O8 Mn1 O4 145.60(19) . 1_655 ? C2 C1 C14 122.3(6) . . ? C2 C1 H1 118.9 . . ? C14 C1 H1 118.9 . . ? C1 C2 C3 119.9(6) . . ? C1 C2 C15 119.4(6) . . ? C3 C2 C15 120.3(6) . . ? C4 C3 C2 120.0(6) . . ? C4 C3 C16 118.4(6) . . ? C2 C3 C16 121.5(6) . . ? C3 C4 C5 119.9(6) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C14 C5 C4 118.7(6) . . ? C14 C5 C6 121.3(6) . . ? C4 C5 C6 119.9(6) . . ? O2 C6 C7 122.1(7) . . ? O2 C6 C5 119.7(7) . . ? C7 C6 C5 118.2(6) . . ? C8 C7 C12 119.8(7) . . ? C8 C7 C6 120.2(7) . . ? C12 C7 C6 119.9(6) . . ? C7 C8 C9 120.2(8) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C10 C9 C8 119.5(8) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 120.5(8) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 120.0(8) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C7 119.9(7) . . ? C11 C12 C13 117.7(7) . . ? C7 C12 C13 122.4(7) . . ? O1 C13 C12 121.7(7) . . ? O1 C13 C14 121.0(6) . . ? C12 C13 C14 117.3(6) . . ? C1 C14 C5 119.2(6) . . ? C1 C14 C13 120.3(6) . . ? C5 C14 C13 120.5(6) . . ? O4 C15 O3 125.9(7) . . ? O4 C15 C2 115.9(6) . . ? O3 C15 C2 118.1(6) . . ? O6 C16 O5 126.8(6) . . ? O6 C16 C3 118.3(6) . . ? O5 C16 C3 114.9(6) . . ? C15 O3 Mn1 171.8(5) . 2_577 ? C15 O4 Mn1 109.9(4) . 1_455 ? C16 O5 Mn1 126.5(4) . . ? C16 O6 Mn1 156.0(5) . 2_667 ? Mn1 O7 H7A 114(5) . . ? Mn1 O7 H7B 120(5) . . ? H7A O7 H7B 90(4) . . ? Mn1 O8 H8A 103(5) . . ? Mn1 O8 H8B 108(5) . . ? H8A O8 H8B 91(4) . . ? H9A O9 H9B 85(4) . . ? H10A O10 H10B 86(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 C1 C2 C3 -0.8(11) . . . . ? C14 C1 C2 C15 -173.5(7) . . . . ? C1 C2 C3 C4 1.2(10) . . . . ? C15 C2 C3 C4 173.8(6) . . . . ? C1 C2 C3 C16 177.6(6) . . . . ? C15 C2 C3 C16 -9.7(10) . . . . ? C2 C3 C4 C5 -0.8(10) . . . . ? C16 C3 C4 C5 -177.4(6) . . . . ? C3 C4 C5 C14 0.1(11) . . . . ? C3 C4 C5 C6 -178.6(7) . . . . ? C14 C5 C6 O2 -178.1(8) . . . . ? C4 C5 C6 O2 0.6(11) . . . . ? C14 C5 C6 C7 2.2(11) . . . . ? C4 C5 C6 C7 -179.1(7) . . . . ? O2 C6 C7 C8 -1.7(12) . . . . ? C5 C6 C7 C8 178.0(7) . . . . ? O2 C6 C7 C12 174.9(8) . . . . ? C5 C6 C7 C12 -5.4(11) . . . . ? C12 C7 C8 C9 -0.8(13) . . . . ? C6 C7 C8 C9 175.9(8) . . . . ? C7 C8 C9 C10 -0.8(13) . . . . ? C8 C9 C10 C11 1.3(14) . . . . ? C9 C10 C11 C12 -0.2(14) . . . . ? C10 C11 C12 C7 -1.4(13) . . . . ? C10 C11 C12 C13 177.9(8) . . . . ? C8 C7 C12 C11 1.9(12) . . . . ? C6 C7 C12 C11 -174.8(7) . . . . ? C8 C7 C12 C13 -177.4(8) . . . . ? C6 C7 C12 C13 6.0(12) . . . . ? C11 C12 C13 O1 -3.7(13) . . . . ? C7 C12 C13 O1 175.6(8) . . . . ? C11 C12 C13 C14 177.5(7) . . . . ? C7 C12 C13 C14 -3.2(12) . . . . ? C2 C1 C14 C5 0.1(11) . . . . ? C2 C1 C14 C13 178.7(7) . . . . ? C4 C5 C14 C1 0.2(11) . . . . ? C6 C5 C14 C1 178.9(7) . . . . ? C4 C5 C14 C13 -178.3(7) . . . . ? C6 C5 C14 C13 0.4(11) . . . . ? O1 C13 C14 C1 2.6(12) . . . . ? C12 C13 C14 C1 -178.6(7) . . . . ? O1 C13 C14 C5 -178.9(8) . . . . ? C12 C13 C14 C5 -0.1(11) . . . . ? C1 C2 C15 O4 121.8(7) . . . . ? C3 C2 C15 O4 -50.9(9) . . . . ? C1 C2 C15 O3 -53.7(9) . . . . ? C3 C2 C15 O3 133.6(7) . . . . ? C4 C3 C16 O6 -50.2(9) . . . . ? C2 C3 C16 O6 133.3(7) . . . . ? C4 C3 C16 O5 129.4(7) . . . . ? C2 C3 C16 O5 -47.1(9) . . . . ? O4 C15 O3 Mn1 -66(4) . . . 2_577 ? C2 C15 O3 Mn1 109(4) . . . 2_577 ? O3 C15 O4 Mn1 19.0(9) . . . 1_455 ? C2 C15 O4 Mn1 -156.1(4) . . . 1_455 ? O6 C16 O5 Mn1 2.9(10) . . . . ? C3 C16 O5 Mn1 -176.7(4) . . . . ? O6 Mn1 O5 C16 -14.6(6) 2_667 . . . ? O3 Mn1 O5 C16 -167.2(5) 2_577 . . . ? O7 Mn1 O5 C16 128.5(5) . . . . ? O8 Mn1 O5 C16 -84.5(5) . . . . ? O4 Mn1 O5 C16 63.8(5) 1_655 . . . ? O5 C16 O6 Mn1 21.7(16) . . . 2_667 ? C3 C16 O6 Mn1 -158.8(8) . . . 2_667 ? 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 O7 H7A O5 0.88(2) 1.92(3) 2.777(7) 164(7) 2_677 O7 H7B O9 0.89(2) 1.90(3) 2.733(9) 157(6) 1_556 O8 H8A O7 0.91(2) 2.16(6) 2.830(7) 129(6) 1_455 O8 H8B O4 0.89(2) 1.89(2) 2.770(7) 168(7) 2_567 O9 H9A O1 0.90(2) 1.92(3) 2.798(9) 165(10) 2_576 O9 H9B O10 0.90(2) 2.66(9) 3.318(12) 131(9) . O10 H10B O9 0.89(2) 2.06(9) 2.862(12) 149(16) 1_455 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.242 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.132 # Attachment '- niaqdc.cif' data_NiAQDC _database_code_depnum_ccdc_archive 'CCDC 801100' #TrackingRef '- niaqdc.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Ni(II) Anthraquinone-2,3-Dicarboxylic Acid' _chemical_melting_point ? _chemical_formula_moiety 'C16 H16 Ni O11, 2(H2 O)' _chemical_formula_sum 'C16 H20 Ni O13' _chemical_formula_weight 479.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.308(3) _cell_length_b 7.4101(15) _cell_length_c 16.183(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.064(4) _cell_angle_gamma 90.00 _cell_volume 1879.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 12.12 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max .4 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.693 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 1.104 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.648 _exptl_absorpt_correction_T_max 0.758 _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13851 _diffrn_reflns_av_R_equivalents 0.0809 _diffrn_reflns_av_sigmaI/netI 0.0845 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 26.02 _reflns_number_total 3675 _reflns_number_gt 2430 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+0.2922P] 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 3675 _refine_ls_number_parameters 313 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1131 _refine_ls_R_factor_gt 0.0622 _refine_ls_wR_factor_ref 0.1587 _refine_ls_wR_factor_gt 0.1284 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.086 _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 O3 O 0.3620(2) 1.0703(5) 0.5594(2) 0.0339(9) Uani 1 1 d . . . C6 C -0.0149(3) 0.7478(8) 0.3714(3) 0.0266(12) Uani 1 1 d . . . Ni1 Ni 0.41465(4) 1.08704(9) 0.28644(4) 0.0211(2) Uani 1 1 d . . . C1 C 0.1960(3) 0.8873(7) 0.5244(3) 0.0228(12) Uani 1 1 d . . . H1 H 0.2192 0.9086 0.5829 0.027 Uiso 1 1 calc R . . C2 C 0.2458(3) 0.9082(7) 0.4685(3) 0.0223(11) Uani 1 1 d . . . C3 C 0.2102(3) 0.8826(7) 0.3801(3) 0.0217(11) Uani 1 1 d . . . C4 C 0.1257(3) 0.8320(7) 0.3496(3) 0.0223(11) Uani 1 1 d . . . H4 H 0.1022 0.8152 0.2909 0.027 Uiso 1 1 calc R . . C5 C 0.0751(3) 0.8057(7) 0.4051(3) 0.0218(12) Uani 1 1 d . . . C7 C -0.0637(3) 0.7056(7) 0.4348(3) 0.0242(12) Uani 1 1 d . . . C8 C -0.1458(3) 0.6364(7) 0.4058(4) 0.0297(13) Uani 1 1 d . . . H8 H -0.1691 0.6108 0.3478 0.036 Uiso 1 1 calc R . . C9 C -0.1925(3) 0.6058(8) 0.4637(4) 0.0370(15) Uani 1 1 d . . . H9 H -0.2477 0.5604 0.4442 0.044 Uiso 1 1 calc R . . C10 C -0.1584(3) 0.6419(8) 0.5503(4) 0.0366(15) Uani 1 1 d . . . H10 H -0.1907 0.6222 0.5886 0.044 Uiso 1 1 calc R . . C11 C -0.0758(3) 0.7074(8) 0.5798(4) 0.0320(14) Uani 1 1 d . . . H11 H -0.0522 0.7301 0.6381 0.038 Uiso 1 1 calc R . . C12 C -0.0284(3) 0.7389(7) 0.5218(3) 0.0219(11) Uani 1 1 d . . . C13 C 0.0593(3) 0.8127(7) 0.5559(3) 0.0239(12) Uani 1 1 d . . . C14 C 0.1112(3) 0.8343(7) 0.4934(3) 0.0217(11) Uani 1 1 d . . . C15 C 0.3405(3) 0.9430(7) 0.5080(3) 0.0235(12) Uani 1 1 d . . . C16 C 0.2631(3) 0.9131(7) 0.3180(3) 0.0223(11) Uani 1 1 d . . . O1 O -0.0493(2) 0.7385(7) 0.2946(2) 0.0484(12) Uani 1 1 d . . . O2 O 0.0881(2) 0.8531(6) 0.6308(2) 0.0399(11) Uani 1 1 d . . . O4 O 0.3915(2) 0.8319(5) 0.4891(2) 0.0277(9) Uani 1 1 d . . . O5 O 0.3129(2) 1.0467(5) 0.3335(2) 0.0245(8) Uani 1 1 d . . . O6 O 0.2528(2) 0.8092(5) 0.2562(3) 0.0407(11) Uani 1 1 d . . . O7 O 0.5246(2) 1.1090(5) 0.2472(3) 0.0307(9) Uani 1 1 d D . . H7A H 0.537(3) 1.171(6) 0.206(3) 0.037 Uiso 1 1 d D . . H7B H 0.556(3) 1.020(5) 0.236(3) 0.037 Uiso 1 1 d D . . O8 O 0.3649(2) 0.9207(6) 0.1827(2) 0.0325(9) Uani 1 1 d D . . H8A H 0.384(3) 0.965(6) 0.142(3) 0.039 Uiso 1 1 d D . . H8B H 0.396(3) 0.825(4) 0.181(3) 0.039 Uiso 1 1 d D . . O9 O 0.4747(2) 0.8762(5) 0.3663(2) 0.0236(8) Uani 1 1 d D . . H9A H 0.457(3) 0.880(7) 0.411(2) 0.028 Uiso 1 1 d D . . H9B H 0.5268(13) 0.889(7) 0.395(3) 0.028 Uiso 1 1 d D . . O10 O 0.4699(2) 1.2703(5) 0.3803(2) 0.0311(9) Uani 1 1 d D . . H10A H 0.505(3) 1.247(7) 0.4305(19) 0.037 Uiso 1 1 d D . . H10B H 0.438(3) 1.334(7) 0.405(3) 0.037 Uiso 1 1 d D . . O11 O 0.3562(2) 1.3107(5) 0.2178(2) 0.0283(9) Uani 1 1 d D . . H11A H 0.307(2) 1.347(7) 0.224(3) 0.034 Uiso 1 1 d D . . H11B H 0.335(3) 1.309(8) 0.1631(13) 0.034 Uiso 1 1 d D . . O12 O 0.2201(2) 1.4402(6) 0.2615(3) 0.0405(10) Uani 1 1 d D . . H12A H 0.203(3) 1.550(4) 0.245(4) 0.049 Uiso 1 1 d D . . H12B H 0.1655(17) 1.407(7) 0.245(4) 0.049 Uiso 1 1 d D . . O13 O 0.3566(4) 1.4826(9) 0.4210(5) 0.095(2) Uani 1 1 d D . . H13A H 0.385(6) 1.446(11) 0.475(3) 0.114 Uiso 1 1 d D . . H13B H 0.362(6) 1.592(5) 0.445(5) 0.114 Uiso 1 1 d 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 O3 0.0202(18) 0.047(2) 0.034(2) -0.019(2) 0.0062(16) -0.0078(18) C6 0.022(3) 0.033(3) 0.024(3) -0.006(3) 0.005(2) -0.003(2) Ni1 0.0197(3) 0.0237(4) 0.0216(4) 0.0018(3) 0.0084(3) 0.0009(3) C1 0.019(2) 0.028(3) 0.020(3) -0.003(2) 0.003(2) 0.001(2) C2 0.016(2) 0.022(3) 0.026(3) -0.004(2) 0.002(2) 0.000(2) C3 0.019(2) 0.024(3) 0.022(3) 0.001(2) 0.006(2) 0.002(2) C4 0.019(2) 0.031(3) 0.016(3) 0.000(2) 0.004(2) -0.002(2) C5 0.018(2) 0.023(3) 0.022(3) 0.000(2) 0.002(2) 0.001(2) C7 0.021(3) 0.027(3) 0.025(3) -0.001(2) 0.007(2) -0.001(2) C8 0.026(3) 0.040(4) 0.025(3) -0.003(3) 0.010(2) -0.006(2) C9 0.025(3) 0.040(4) 0.045(4) -0.003(3) 0.008(3) -0.010(3) C10 0.026(3) 0.048(4) 0.040(4) 0.005(3) 0.016(3) -0.006(3) C11 0.026(3) 0.047(4) 0.023(3) 0.002(3) 0.008(2) 0.004(3) C12 0.017(2) 0.020(3) 0.029(3) 0.001(2) 0.007(2) 0.002(2) C13 0.019(2) 0.032(3) 0.020(3) 0.002(2) 0.003(2) 0.000(2) C14 0.019(2) 0.026(3) 0.021(3) 0.001(2) 0.007(2) 0.002(2) C15 0.021(2) 0.035(3) 0.015(3) 0.001(3) 0.005(2) -0.001(2) C16 0.019(2) 0.028(3) 0.020(3) 0.005(3) 0.006(2) -0.001(2) O1 0.028(2) 0.095(4) 0.021(2) -0.005(2) 0.0060(18) -0.017(2) O2 0.029(2) 0.067(3) 0.023(2) -0.007(2) 0.0075(18) -0.014(2) O4 0.0182(17) 0.038(2) 0.027(2) 0.0031(18) 0.0062(16) 0.0058(16) O5 0.0236(18) 0.026(2) 0.027(2) -0.0031(16) 0.0119(16) -0.0047(15) O6 0.049(3) 0.046(3) 0.035(2) -0.017(2) 0.027(2) -0.024(2) O7 0.030(2) 0.028(2) 0.040(2) 0.0080(19) 0.0214(18) 0.0029(17) O8 0.032(2) 0.043(2) 0.024(2) -0.001(2) 0.0110(16) 0.0072(19) O9 0.0191(17) 0.032(2) 0.0195(19) -0.0019(17) 0.0059(15) 0.0014(16) O10 0.030(2) 0.035(2) 0.025(2) -0.0061(19) 0.0032(17) 0.0016(18) O11 0.0252(19) 0.036(2) 0.025(2) 0.0085(19) 0.0097(17) 0.0088(17) O12 0.032(2) 0.043(3) 0.047(3) 0.008(2) 0.013(2) 0.0079(19) O13 0.071(4) 0.066(4) 0.146(6) -0.052(4) 0.027(4) 0.004(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 O3 C15 1.243(6) . ? C6 O1 1.217(6) . ? C6 C5 1.481(7) . ? C6 C7 1.494(7) . ? Ni1 O5 2.031(3) . ? Ni1 O10 2.050(4) . ? Ni1 O8 2.060(4) . ? Ni1 O7 2.068(3) . ? Ni1 O11 2.074(4) . ? Ni1 O9 2.090(4) . ? C1 C2 1.382(7) . ? C1 C14 1.391(6) . ? C1 H1 0.9300 . ? C2 C3 1.401(7) . ? C2 C15 1.521(6) . ? C3 C4 1.381(6) . ? C3 C16 1.512(6) . ? C4 C5 1.391(7) . ? C4 H4 0.9300 . ? C5 C14 1.402(7) . ? C7 C12 1.388(7) . ? C7 C8 1.389(7) . ? C8 C9 1.380(7) . ? C8 H8 0.9300 . ? C9 C10 1.383(8) . ? C9 H9 0.9300 . ? C10 C11 1.386(7) . ? C10 H10 0.9300 . ? C11 C12 1.390(7) . ? C11 H11 0.9300 . ? C12 C13 1.488(7) . ? C13 O2 1.209(6) . ? C13 C14 1.496(7) . ? C15 O4 1.266(6) . ? C16 O6 1.236(6) . ? C16 O5 1.260(6) . ? O7 H7A 0.878(19) . ? O7 H7B 0.877(19) . ? O8 H8A 0.866(19) . ? O8 H8B 0.877(19) . ? O9 H9A 0.855(19) . ? O9 H9B 0.856(19) . ? O10 H10A 0.871(19) . ? O10 H10B 0.873(19) . ? O11 H11A 0.874(19) . ? O11 H11B 0.858(19) . ? O12 H12A 0.88(2) . ? O12 H12B 0.89(2) . ? O13 H13A 0.91(2) . ? O13 H13B 0.89(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C6 C5 121.5(5) . . ? O1 C6 C7 120.5(4) . . ? C5 C6 C7 118.0(4) . . ? O5 Ni1 O10 93.29(14) . . ? O5 Ni1 O8 92.22(14) . . ? O10 Ni1 O8 173.33(16) . . ? O5 Ni1 O7 174.29(15) . . ? O10 Ni1 O7 86.24(15) . . ? O8 Ni1 O7 88.65(15) . . ? O5 Ni1 O11 90.91(14) . . ? O10 Ni1 O11 84.84(16) . . ? O8 Ni1 O11 91.30(16) . . ? O7 Ni1 O11 94.72(14) . . ? O5 Ni1 O9 87.12(13) . . ? O10 Ni1 O9 90.13(15) . . ? O8 Ni1 O9 93.92(15) . . ? O7 Ni1 O9 87.19(14) . . ? O11 Ni1 O9 174.49(14) . . ? C2 C1 C14 120.1(5) . . ? C2 C1 H1 120.0 . . ? C14 C1 H1 120.0 . . ? C1 C2 C3 120.1(4) . . ? C1 C2 C15 117.2(4) . . ? C3 C2 C15 122.5(4) . . ? C4 C3 C2 119.4(4) . . ? C4 C3 C16 120.0(4) . . ? C2 C3 C16 120.5(4) . . ? C3 C4 C5 121.3(5) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C4 C5 C14 118.7(4) . . ? C4 C5 C6 120.5(5) . . ? C14 C5 C6 120.8(4) . . ? C12 C7 C8 119.9(5) . . ? C12 C7 C6 120.6(4) . . ? C8 C7 C6 119.4(5) . . ? C9 C8 C7 119.6(5) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 120.8(5) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C9 C10 C11 119.8(5) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C12 119.7(5) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C7 C12 C11 120.2(4) . . ? C7 C12 C13 121.8(4) . . ? C11 C12 C13 118.0(5) . . ? O2 C13 C12 121.9(5) . . ? O2 C13 C14 121.1(4) . . ? C12 C13 C14 117.0(5) . . ? C1 C14 C5 120.4(4) . . ? C1 C14 C13 118.5(5) . . ? C5 C14 C13 121.1(4) . . ? O3 C15 O4 125.0(5) . . ? O3 C15 C2 118.3(4) . . ? O4 C15 C2 116.5(5) . . ? O6 C16 O5 125.9(4) . . ? O6 C16 C3 118.0(4) . . ? O5 C16 C3 116.0(5) . . ? C16 O5 Ni1 126.1(3) . . ? Ni1 O7 H7A 132(3) . . ? Ni1 O7 H7B 127(3) . . ? H7A O7 H7B 89(2) . . ? Ni1 O8 H8A 104(4) . . ? Ni1 O8 H8B 114(4) . . ? H8A O8 H8B 88(2) . . ? Ni1 O9 H9A 107(3) . . ? Ni1 O9 H9B 119(4) . . ? H9A O9 H9B 93(2) . . ? Ni1 O10 H10A 127(4) . . ? Ni1 O10 H10B 120(4) . . ? H10A O10 H10B 90(2) . . ? Ni1 O11 H11A 119(3) . . ? Ni1 O11 H11B 123(4) . . ? H11A O11 H11B 90(2) . . ? H12A O12 H12B 87(2) . . ? H13A O13 H13B 84(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 C1 C2 C3 2.3(8) . . . . ? C14 C1 C2 C15 -172.4(5) . . . . ? C1 C2 C3 C4 -1.6(8) . . . . ? C15 C2 C3 C4 172.9(5) . . . . ? C1 C2 C3 C16 177.3(5) . . . . ? C15 C2 C3 C16 -8.2(8) . . . . ? C2 C3 C4 C5 -0.1(8) . . . . ? C16 C3 C4 C5 -179.0(5) . . . . ? C3 C4 C5 C14 1.0(8) . . . . ? C3 C4 C5 C6 -178.7(5) . . . . ? O1 C6 C5 C4 -7.1(8) . . . . ? C7 C6 C5 C4 174.5(5) . . . . ? O1 C6 C5 C14 173.2(6) . . . . ? C7 C6 C5 C14 -5.2(7) . . . . ? O1 C6 C7 C12 -171.4(5) . . . . ? C5 C6 C7 C12 7.0(8) . . . . ? O1 C6 C7 C8 7.1(8) . . . . ? C5 C6 C7 C8 -174.6(5) . . . . ? C12 C7 C8 C9 1.7(8) . . . . ? C6 C7 C8 C9 -176.8(5) . . . . ? C7 C8 C9 C10 -0.5(9) . . . . ? C8 C9 C10 C11 -0.8(9) . . . . ? C9 C10 C11 C12 1.0(9) . . . . ? C8 C7 C12 C11 -1.6(8) . . . . ? C6 C7 C12 C11 176.9(5) . . . . ? C8 C7 C12 C13 179.9(5) . . . . ? C6 C7 C12 C13 -1.7(8) . . . . ? C10 C11 C12 C7 0.2(8) . . . . ? C10 C11 C12 C13 178.8(5) . . . . ? C7 C12 C13 O2 175.0(5) . . . . ? C11 C12 C13 O2 -3.6(8) . . . . ? C7 C12 C13 C14 -5.3(7) . . . . ? C11 C12 C13 C14 176.1(5) . . . . ? C2 C1 C14 C5 -1.4(8) . . . . ? C2 C1 C14 C13 179.9(5) . . . . ? C4 C5 C14 C1 -0.2(8) . . . . ? C6 C5 C14 C1 179.5(5) . . . . ? C4 C5 C14 C13 178.4(5) . . . . ? C6 C5 C14 C13 -1.9(8) . . . . ? O2 C13 C14 C1 5.5(8) . . . . ? C12 C13 C14 C1 -174.3(5) . . . . ? O2 C13 C14 C5 -173.2(5) . . . . ? C12 C13 C14 C5 7.1(7) . . . . ? C1 C2 C15 O3 -53.8(7) . . . . ? C3 C2 C15 O3 131.6(5) . . . . ? C1 C2 C15 O4 122.3(5) . . . . ? C3 C2 C15 O4 -52.3(7) . . . . ? C4 C3 C16 O6 -39.3(7) . . . . ? C2 C3 C16 O6 141.8(5) . . . . ? C4 C3 C16 O5 139.1(5) . . . . ? C2 C3 C16 O5 -39.8(7) . . . . ? O6 C16 O5 Ni1 -20.2(7) . . . . ? C3 C16 O5 Ni1 161.5(3) . . . . ? O10 Ni1 O5 C16 -160.5(4) . . . . ? O8 Ni1 O5 C16 23.3(4) . . . . ? O11 Ni1 O5 C16 114.6(4) . . . . ? O9 Ni1 O5 C16 -70.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.625 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.108 # Attachment '- znaqdc.cif' data_ZnAQDC _database_code_depnum_ccdc_archive 'CCDC 801101' #TrackingRef '- znaqdc.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Zinc(II) Anthraquinone-2,3-dicarboxylate' _chemical_melting_point ? _chemical_formula_moiety 'C16 H10 O8 Zn, 2(H2 O)' _chemical_formula_sum 'C16 H14 O10 Zn' _chemical_formula_weight 431.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.629(2) _cell_length_b 7.843(2) _cell_length_c 15.045(5) _cell_angle_alpha 91.409(6) _cell_angle_beta 95.784(5) _cell_angle_gamma 115.160(5) _cell_volume 808.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 67 _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 26.02 _exptl_crystal_description 'square plate' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.773 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 1.578 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.572 _exptl_absorpt_correction_T_max 0.969 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6709 _diffrn_reflns_av_R_equivalents 0.0977 _diffrn_reflns_av_sigmaI/netI 0.1859 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 26.02 _reflns_number_total 3124 _reflns_number_gt 1520 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3124 _refine_ls_number_parameters 269 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1681 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.1345 _refine_ls_wR_factor_gt 0.1036 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.946 _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 1.00224(13) 0.71567(12) 0.43583(6) 0.0321(3) Uani 1 1 d . . . C1 C 0.9008(9) 0.8656(9) 0.8297(4) 0.0265(16) Uani 1 1 d . . . H1 H 0.9023 0.9774 0.8528 0.032 Uiso 1 1 calc R . . C2 C 0.9614(9) 0.8605(8) 0.7463(4) 0.0231(15) Uani 1 1 d . . . C3 C 0.9515(9) 0.6901(9) 0.7100(4) 0.0213(15) Uani 1 1 d . . . C4 C 0.8839(9) 0.5326(8) 0.7589(4) 0.0237(16) Uani 1 1 d . . . H4 H 0.8754 0.4186 0.7348 0.028 Uiso 1 1 calc R . . C5 C 0.8286(9) 0.5414(8) 0.8433(4) 0.0215(15) Uani 1 1 d . . . C6 C 0.7657(9) 0.3700(9) 0.8928(5) 0.0278(17) Uani 1 1 d . . . C7 C 0.7333(9) 0.3876(9) 0.9880(4) 0.0247(16) Uani 1 1 d . . . C8 C 0.6905(9) 0.2335(10) 1.0390(5) 0.0341(18) Uani 1 1 d . . . H8 H 0.6864 0.1217 1.0144 0.041 Uiso 1 1 calc R . . C9 C 0.6546(10) 0.2457(11) 1.1248(5) 0.046(2) Uani 1 1 d . . . H9 H 0.6227 0.1414 1.1588 0.055 Uiso 1 1 calc R . . C10 C 0.6657(10) 0.4132(11) 1.1617(5) 0.043(2) Uani 1 1 d . . . H10 H 0.6451 0.4215 1.2212 0.051 Uiso 1 1 calc R . . C11 C 0.7061(10) 0.5670(10) 1.1129(4) 0.0349(18) Uani 1 1 d . . . H11 H 0.7094 0.6777 1.1385 0.042 Uiso 1 1 calc R . . C12 C 0.7425(9) 0.5566(9) 1.0243(4) 0.0257(16) Uani 1 1 d . . . C13 C 0.7850(9) 0.7212(9) 0.9703(4) 0.0270(17) Uani 1 1 d . . . C14 C 0.8382(9) 0.7101(9) 0.8794(4) 0.0227(15) Uani 1 1 d . . . C15 C 1.0529(11) 1.0406(9) 0.6994(4) 0.0250(16) Uani 1 1 d . . . C16 C 1.0076(9) 0.6701(9) 0.6195(4) 0.0277(17) Uani 1 1 d . . . O1 O 0.7815(7) 0.8645(6) 1.0010(3) 0.0408(13) Uani 1 1 d . . . O2 O 0.7409(7) 0.2174(6) 0.8583(3) 0.0422(13) Uani 1 1 d . . . O3 O 1.2329(7) 1.1150(6) 0.7064(3) 0.0396(13) Uani 1 1 d . . . O4 O 0.9402(6) 1.1011(6) 0.6594(3) 0.0331(12) Uani 1 1 d . . . O5 O 0.9934(8) 0.7791(7) 0.5631(3) 0.0486(14) Uani 1 1 d . . . O6 O 1.0715(7) 0.5510(6) 0.6052(3) 0.0426(13) Uani 1 1 d . . . O7 O 1.2913(8) 0.7768(8) 0.4467(4) 0.0586(16) Uani 1 1 d D . . H7A H 1.368(9) 0.845(8) 0.408(3) 0.070 Uiso 1 1 d D . . H7B H 1.331(11) 0.884(6) 0.480(4) 0.070 Uiso 1 1 d D . . O8 O 0.7033(8) 0.6485(7) 0.4203(3) 0.0468(14) Uani 1 1 d D . . H8A H 0.628(9) 0.538(4) 0.392(4) 0.056 Uiso 1 1 d D . . H8B H 0.706(10) 0.698(7) 0.368(2) 0.056 Uiso 1 1 d D . . O9 O 0.5294(8) 0.0157(7) 0.6885(3) 0.0468(14) Uani 1 1 d D . . H9A H 0.429(6) 0.040(9) 0.697(4) 0.056 Uiso 1 1 d D . . H9B H 0.587(8) 0.079(9) 0.739(3) 0.056 Uiso 1 1 d D . . O10 O 0.5388(7) 0.7237(6) 0.5788(4) 0.0462(14) Uani 1 1 d D . . H10A H 0.649(6) 0.782(8) 0.556(4) 0.055 Uiso 1 1 d D . . H10B H 0.579(9) 0.822(6) 0.618(3) 0.055 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0492(6) 0.0271(5) 0.0274(5) 0.0090(4) 0.0155(4) 0.0207(4) C1 0.031(4) 0.022(4) 0.027(4) 0.002(3) 0.002(3) 0.011(3) C2 0.020(4) 0.019(4) 0.026(4) 0.004(3) -0.002(3) 0.006(3) C3 0.035(4) 0.025(4) 0.013(4) 0.006(3) 0.002(3) 0.022(3) C4 0.028(4) 0.022(4) 0.022(4) -0.004(3) 0.003(3) 0.011(3) C5 0.019(4) 0.021(4) 0.019(4) 0.003(3) 0.003(3) 0.002(3) C6 0.020(4) 0.018(4) 0.043(5) 0.006(4) 0.005(3) 0.006(3) C7 0.022(4) 0.027(4) 0.025(4) 0.011(3) 0.012(3) 0.008(3) C8 0.032(4) 0.036(5) 0.033(5) 0.010(4) 0.001(4) 0.014(4) C9 0.046(5) 0.045(6) 0.045(5) 0.034(4) 0.010(4) 0.015(4) C10 0.036(5) 0.060(6) 0.024(4) 0.015(4) 0.003(4) 0.012(4) C11 0.045(5) 0.045(5) 0.020(4) 0.004(4) 0.008(4) 0.022(4) C12 0.022(4) 0.030(4) 0.024(4) -0.005(3) 0.003(3) 0.010(3) C13 0.030(4) 0.029(4) 0.026(4) 0.001(3) 0.001(3) 0.017(4) C14 0.027(4) 0.023(4) 0.018(4) -0.004(3) 0.003(3) 0.011(3) C15 0.037(5) 0.026(4) 0.019(4) 0.009(3) 0.013(4) 0.018(4) C16 0.026(4) 0.019(4) 0.032(4) 0.004(3) 0.009(3) 0.003(3) O1 0.062(4) 0.035(3) 0.033(3) 0.003(2) 0.017(3) 0.025(3) O2 0.067(4) 0.023(3) 0.036(3) 0.002(2) 0.012(3) 0.018(3) O3 0.025(3) 0.038(3) 0.055(4) 0.019(3) 0.013(3) 0.010(3) O4 0.034(3) 0.031(3) 0.046(3) 0.014(2) 0.011(2) 0.023(3) O5 0.091(4) 0.052(3) 0.032(3) 0.015(2) 0.023(3) 0.054(3) O6 0.059(4) 0.038(3) 0.042(3) 0.006(2) 0.028(3) 0.027(3) O7 0.046(4) 0.077(4) 0.052(4) 0.039(3) 0.018(3) 0.022(3) O8 0.050(4) 0.047(3) 0.049(4) 0.017(3) 0.022(3) 0.021(3) O9 0.044(3) 0.059(4) 0.043(3) 0.003(3) 0.014(3) 0.026(3) O10 0.037(3) 0.037(3) 0.057(4) 0.004(3) 0.007(3) 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 Zn1 O5 1.982(5) . ? Zn1 O6 1.984(5) 2_766 ? Zn1 O4 2.000(4) 2_776 ? Zn1 O7 2.036(6) . ? Zn1 O8 2.097(5) . ? C1 C14 1.377(8) . ? C1 C2 1.385(8) . ? C1 H1 0.9300 . ? C2 C3 1.400(8) . ? C2 C15 1.514(8) . ? C3 C4 1.383(8) . ? C3 C16 1.492(8) . ? C4 C5 1.387(8) . ? C4 H4 0.9300 . ? C5 C14 1.387(8) . ? C5 C6 1.471(8) . ? C6 O2 1.222(7) . ? C6 C7 1.491(8) . ? C7 C8 1.384(8) . ? C7 C12 1.392(8) . ? C8 C9 1.357(9) . ? C8 H8 0.9300 . ? C9 C10 1.378(10) . ? C9 H9 0.9300 . ? C10 C11 1.364(9) . ? C10 H10 0.9300 . ? C11 C12 1.396(8) . ? C11 H11 0.9300 . ? C12 C13 1.476(8) . ? C13 O1 1.217(7) . ? C13 C14 1.477(8) . ? C15 O3 1.234(7) . ? C15 O4 1.258(7) . ? C16 O6 1.247(7) . ? C16 O5 1.248(7) . ? O4 Zn1 2.000(4) 2_776 ? O6 Zn1 1.984(5) 2_766 ? O7 H7A 0.89(2) . ? O7 H7B 0.88(2) . ? O8 H8A 0.88(2) . ? O8 H8B 0.89(2) . ? O9 H9A 0.88(2) . ? O9 H9B 0.87(2) . ? O10 H10A 0.88(2) . ? O10 H10B 0.88(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zn1 O6 119.16(19) . 2_766 ? O5 Zn1 O4 124.67(19) . 2_776 ? O6 Zn1 O4 115.98(18) 2_766 2_776 ? O5 Zn1 O7 97.1(2) . . ? O6 Zn1 O7 91.5(2) 2_766 . ? O4 Zn1 O7 85.67(19) 2_776 . ? O5 Zn1 O8 84.8(2) . . ? O6 Zn1 O8 87.24(19) 2_766 . ? O4 Zn1 O8 93.55(18) 2_776 . ? O7 Zn1 O8 178.1(2) . . ? C14 C1 C2 122.0(6) . . ? C14 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C1 C2 C3 119.0(6) . . ? C1 C2 C15 120.1(5) . . ? C3 C2 C15 120.7(6) . . ? C4 C3 C2 119.1(6) . . ? C4 C3 C16 118.3(5) . . ? C2 C3 C16 122.6(6) . . ? C3 C4 C5 121.2(6) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C4 C5 C14 119.8(6) . . ? C4 C5 C6 118.1(6) . . ? C14 C5 C6 122.1(6) . . ? O2 C6 C5 122.1(6) . . ? O2 C6 C7 120.3(6) . . ? C5 C6 C7 117.6(5) . . ? C8 C7 C12 120.7(6) . . ? C8 C7 C6 119.3(6) . . ? C12 C7 C6 120.0(6) . . ? C9 C8 C7 120.0(7) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 119.8(7) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C11 C10 C9 121.6(7) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C12 119.4(7) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C7 C12 C11 118.6(6) . . ? C7 C12 C13 121.2(6) . . ? C11 C12 C13 120.1(6) . . ? O1 C13 C12 120.7(6) . . ? O1 C13 C14 120.8(6) . . ? C12 C13 C14 118.5(5) . . ? C1 C14 C5 118.9(6) . . ? C1 C14 C13 121.2(5) . . ? C5 C14 C13 119.8(6) . . ? O3 C15 O4 126.8(6) . . ? O3 C15 C2 115.6(6) . . ? O4 C15 C2 117.5(6) . . ? O6 C16 O5 123.8(6) . . ? O6 C16 C3 118.7(6) . . ? O5 C16 C3 117.5(6) . . ? C15 O4 Zn1 127.8(4) . 2_776 ? C16 O5 Zn1 117.9(4) . . ? C16 O6 Zn1 144.5(5) . 2_766 ? Zn1 O7 H7A 122(5) . . ? Zn1 O7 H7B 96(5) . . ? H7A O7 H7B 86(2) . . ? Zn1 O8 H8A 115(5) . . ? Zn1 O8 H8B 94(5) . . ? H8A O8 H8B 88(2) . . ? H9A O9 H9B 88(2) . . ? H10A O10 H10B 87(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 C1 C2 C3 2.6(9) . . . . ? C14 C1 C2 C15 -172.2(6) . . . . ? C1 C2 C3 C4 -0.8(9) . . . . ? C15 C2 C3 C4 173.9(6) . . . . ? C1 C2 C3 C16 178.0(6) . . . . ? C15 C2 C3 C16 -7.3(9) . . . . ? C2 C3 C4 C5 -0.9(9) . . . . ? C16 C3 C4 C5 -179.7(5) . . . . ? C3 C4 C5 C14 0.9(9) . . . . ? C3 C4 C5 C6 -177.6(6) . . . . ? C4 C5 C6 O2 -8.1(9) . . . . ? C14 C5 C6 O2 173.5(6) . . . . ? C4 C5 C6 C7 171.7(5) . . . . ? C14 C5 C6 C7 -6.8(9) . . . . ? O2 C6 C7 C8 5.3(9) . . . . ? C5 C6 C7 C8 -174.5(6) . . . . ? O2 C6 C7 C12 -173.5(6) . . . . ? C5 C6 C7 C12 6.8(9) . . . . ? C12 C7 C8 C9 0.8(10) . . . . ? C6 C7 C8 C9 -177.9(6) . . . . ? C7 C8 C9 C10 -1.6(11) . . . . ? C8 C9 C10 C11 2.1(11) . . . . ? C9 C10 C11 C12 -1.8(11) . . . . ? C8 C7 C12 C11 -0.5(9) . . . . ? C6 C7 C12 C11 178.3(6) . . . . ? C8 C7 C12 C13 -179.1(6) . . . . ? C6 C7 C12 C13 -0.3(9) . . . . ? C10 C11 C12 C7 1.0(10) . . . . ? C10 C11 C12 C13 179.5(6) . . . . ? C7 C12 C13 O1 175.7(6) . . . . ? C11 C12 C13 O1 -2.8(10) . . . . ? C7 C12 C13 C14 -6.3(9) . . . . ? C11 C12 C13 C14 175.2(6) . . . . ? C2 C1 C14 C5 -2.5(9) . . . . ? C2 C1 C14 C13 176.4(6) . . . . ? C4 C5 C14 C1 0.8(9) . . . . ? C6 C5 C14 C1 179.2(6) . . . . ? C4 C5 C14 C13 -178.2(5) . . . . ? C6 C5 C14 C13 0.3(9) . . . . ? O1 C13 C14 C1 5.4(10) . . . . ? C12 C13 C14 C1 -172.6(6) . . . . ? O1 C13 C14 C5 -175.7(6) . . . . ? C12 C13 C14 C5 6.3(9) . . . . ? C1 C2 C15 O3 98.8(7) . . . . ? C3 C2 C15 O3 -75.9(8) . . . . ? C1 C2 C15 O4 -79.6(8) . . . . ? C3 C2 C15 O4 105.7(7) . . . . ? C4 C3 C16 O6 -30.1(9) . . . . ? C2 C3 C16 O6 151.1(6) . . . . ? C4 C3 C16 O5 152.3(6) . . . . ? C2 C3 C16 O5 -26.5(9) . . . . ? O3 C15 O4 Zn1 20.7(9) . . . 2_776 ? C2 C15 O4 Zn1 -161.1(4) . . . 2_776 ? O6 C16 O5 Zn1 17.4(9) . . . . ? C3 C16 O5 Zn1 -165.0(4) . . . . ? O6 Zn1 O5 C16 24.0(6) 2_766 . . . ? O4 Zn1 O5 C16 -161.4(5) 2_776 . . . ? O7 Zn1 O5 C16 -71.7(5) . . . . ? O8 Zn1 O5 C16 107.9(5) . . . . ? O5 C16 O6 Zn1 -92.8(9) . . . 2_766 ? C3 C16 O6 Zn1 89.6(9) . . . 2_766 ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.532 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.112