#------------------------------------------------------------------------------ #$Date: 2016-02-18 10:40:55 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176722 $ #$URL: file:///home/coder/svn-repositories/cod/cif/3/00/00/3000007.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_3000007 loop_ _publ_author_name 'Carmen R. Maldonado' 'Miguel Quiros' 'Juan M. Salas' _publ_section_title ; H-bond superstructures built by aquacomplexes and an azapurine derivative: A case of molecular recognition ; _journal_name_full 'Dalton Transactions' _journal_page_first 10390 _journal_page_last 10395 _journal_paper_doi 10.1039/c2dt30992k _journal_year 2012 _chemical_formula_moiety 'C20 H24 N4 O4 S2 Zn 2+, 2(C6 H6 N5 O2 1-)' _chemical_formula_sum 'C32 H36 N14 O8 S2 Zn' _chemical_formula_weight 874.24 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 100.431(1) _cell_angle_beta 97.247(2) _cell_angle_gamma 94.369(1) _cell_formula_units_Z 1 _cell_length_a 8.3460(8) _cell_length_b 10.1959(10) _cell_length_c 11.7050(11) _cell_measurement_reflns_used 5301 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 27.9 _cell_measurement_theta_min 2.4 _cell_volume 966.73(16) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT (Bruker, 1999)' _computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)' _computing_publication_material SHELXL-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 298(2) _diffrn_detector_area_resol_mean 8.26 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.920 _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 11323 _diffrn_reflns_theta_full 26.80 _diffrn_reflns_theta_max 28.21 _diffrn_reflns_theta_min 1.79 _diffrn_standards_decay_% -0.2 _diffrn_standards_number 216 _exptl_absorpt_coefficient_mu 0.812 _exptl_absorpt_correction_T_max 0.902 _exptl_absorpt_correction_T_min 0.791 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 452 _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _refine_diff_density_max 0.437 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.056 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 273 _refine_ls_number_reflns 4383 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0368 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0994 _refine_ls_wR_factor_ref 0.1017 _reflns_number_gt 4013 _reflns_number_total 4383 _reflns_threshold_expression I>2\s(I) _cod_data_source_file znaxss.cif _cod_data_source_block znaxss _cod_depositor_comments ;Extending hold period by 9 months (from 2011-12-03 to 2012-09-03) Also changing journal name to Dalton Transactions Adding Fobs data. Releasing structure 3000007 into public domain as published material. ; _cod_database_code 3000007 _cod_database_fobs_code 3000007 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 Zn Zn 0.5000 0.5000 0.5000 0.03322(10) Uani 1 2 d S O1W O 0.24590(14) 0.46875(13) 0.46191(13) 0.0402(3) Uani 1 1 d D H11W H 0.191(2) 0.5322(17) 0.480(2) 0.048 Uiso 1 1 d D H12W H 0.198(2) 0.4060(17) 0.4850(19) 0.048 Uiso 1 1 d D O2W O 0.49865(15) 0.30196(13) 0.53214(14) 0.0444(3) Uani 1 1 d D H21W H 0.5897(16) 0.272(2) 0.538(2) 0.053 Uiso 1 1 d D H22W H 0.437(2) 0.259(2) 0.5664(18) 0.053 Uiso 1 1 d D N1P N 0.51543(18) 0.42066(15) 0.31925(14) 0.0401(3) Uani 1 1 d . C2P C 0.4081(2) 0.31927(19) 0.25813(18) 0.0424(4) Uani 1 1 d . H2P H 0.3198 0.2897 0.2914 0.051 Uiso 1 1 d R C3P C 0.4175(2) 0.2570(2) 0.14639(19) 0.0494(5) Uani 1 1 d . H3P H 0.3391 0.1833 0.1043 0.059 Uiso 1 1 d R C4P C 0.5438(3) 0.2996(2) 0.09016(18) 0.0538(5) Uani 1 1 d . C5P C 0.6522(3) 0.4058(2) 0.15034(19) 0.0537(5) Uani 1 1 d . H5P H 0.7382 0.4405 0.1174 0.064 Uiso 1 1 d R C6P C 0.6347(2) 0.4620(2) 0.26290(18) 0.0460(4) Uani 1 1 d . H6P H 0.7114 0.5359 0.3067 0.055 Uiso 1 1 d R S S 0.55145(11) 0.21488(11) -0.05327(6) 0.1029(4) Uani 1 1 d . N1Q N 1.0287(3) 0.3841(3) -0.1417(2) 0.0835(7) Uani 1 1 d . C2Q C 0.8907(4) 0.4189(3) -0.1828(3) 0.0826(9) Uani 1 1 d . H2Q H 0.8885 0.4817 -0.2334 0.099 Uiso 1 1 d R C3Q C 0.7427(4) 0.3724(3) -0.1574(2) 0.0692(7) Uani 1 1 d . H3Q H 0.6428 0.3977 -0.1926 0.083 Uiso 1 1 d R C4Q C 0.7406(3) 0.2831(3) -0.08425(19) 0.0588(6) Uani 1 1 d . C5Q C 0.8841(4) 0.2423(3) -0.0405(3) 0.0785(8) Uani 1 1 d . H5Q H 0.8899 0.1799 0.0105 0.094 Uiso 1 1 d R C6Q C 1.0252(4) 0.2967(4) -0.0725(3) 0.0874(9) Uani 1 1 d . H6Q H 1.1268 0.2730 -0.0389 0.105 Uiso 1 1 d R N1 N 0.05956(18) 0.27227(15) 0.53431(15) 0.0414(4) Uani 1 1 d . N2 N -0.09247(19) 0.29654(16) 0.50877(17) 0.0477(4) Uani 1 1 d . N3 N -0.19704(18) 0.21281(16) 0.54980(16) 0.0432(4) Uani 1 1 d . C3A C -0.1037(2) 0.13507(16) 0.60234(16) 0.0347(4) Uani 1 1 d . N4 N -0.15071(17) 0.03717(15) 0.66119(14) 0.0382(3) Uani 1 1 d . C4 C -0.3224(2) 0.0057(2) 0.6692(2) 0.0497(5) Uani 1 1 d . H41 H -0.3713 -0.0800 0.6159 0.060 Uiso 1 1 d R H42 H -0.3837 0.0791 0.6497 0.060 Uiso 1 1 d R H43 H -0.3251 -0.0016 0.7506 0.060 Uiso 1 1 d R C5 C -0.0358(2) -0.02791(19) 0.71575(17) 0.0409(4) Uani 1 1 d . O5 O -0.07024(18) -0.11075(16) 0.77385(15) 0.0588(4) Uani 1 1 d . N6 N 0.12710(17) 0.00532(16) 0.70240(15) 0.0406(3) Uani 1 1 d . C6 C 0.2469(3) -0.0725(2) 0.7551(2) 0.0576(6) Uani 1 1 d . H61 H 0.3384 -0.0731 0.7135 0.069 Uiso 1 1 d R H62 H 0.1946 -0.1655 0.7452 0.069 Uiso 1 1 d R H63 H 0.2869 -0.0343 0.8387 0.069 Uiso 1 1 d R C7 C 0.1836(2) 0.10492(18) 0.64499(17) 0.0379(4) Uani 1 1 d . O7 O 0.32954(15) 0.12901(15) 0.64310(15) 0.0533(4) Uani 1 1 d . C7A C 0.05620(19) 0.16917(17) 0.59338(16) 0.0353(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 Zn 0.02514(15) 0.03221(16) 0.04552(18) 0.01308(11) 0.00948(11) 0.00232(10) O1W 0.0274(6) 0.0347(6) 0.0639(8) 0.0189(6) 0.0131(5) 0.0039(5) O2W 0.0302(6) 0.0382(7) 0.0733(9) 0.0265(6) 0.0154(6) 0.0068(5) N1P 0.0347(7) 0.0386(8) 0.0494(9) 0.0120(7) 0.0119(6) 0.0003(6) C2P 0.0362(9) 0.0402(9) 0.0535(11) 0.0158(8) 0.0103(8) -0.0024(7) C3P 0.0441(10) 0.0473(11) 0.0537(11) 0.0087(9) 0.0061(9) -0.0102(8) C4P 0.0509(11) 0.0628(13) 0.0447(11) 0.0057(9) 0.0106(9) -0.0077(10) C5P 0.0480(11) 0.0601(13) 0.0522(12) 0.0090(10) 0.0172(9) -0.0123(9) C6P 0.0414(10) 0.0453(10) 0.0508(11) 0.0095(8) 0.0124(8) -0.0082(8) S 0.0936(6) 0.1334(8) 0.0585(4) -0.0276(4) 0.0309(4) -0.0568(5) N1Q 0.0722(16) 0.0990(19) 0.0750(15) 0.0038(14) 0.0239(13) -0.0107(14) C2Q 0.102(2) 0.083(2) 0.0651(16) 0.0233(15) 0.0193(16) -0.0094(17) C3Q 0.0719(16) 0.0788(17) 0.0578(14) 0.0173(12) 0.0048(12) 0.0109(13) C4Q 0.0662(14) 0.0647(14) 0.0410(11) 0.0002(10) 0.0133(10) -0.0073(11) C5Q 0.093(2) 0.0799(19) 0.0661(16) 0.0262(14) 0.0076(15) 0.0078(16) C6Q 0.0608(17) 0.105(2) 0.093(2) 0.0126(19) 0.0040(15) 0.0156(16) N1 0.0310(7) 0.0368(8) 0.0632(10) 0.0215(7) 0.0135(7) 0.0060(6) N2 0.0349(8) 0.0404(8) 0.0767(12) 0.0273(8) 0.0152(8) 0.0093(6) N3 0.0302(7) 0.0378(8) 0.0680(10) 0.0210(7) 0.0138(7) 0.0071(6) C3A 0.0283(8) 0.0286(8) 0.0492(10) 0.0091(7) 0.0113(7) 0.0024(6) N4 0.0279(7) 0.0350(7) 0.0566(9) 0.0169(7) 0.0144(6) 0.0012(5) C4 0.0301(9) 0.0477(11) 0.0753(14) 0.0182(10) 0.0174(9) -0.0016(7) C5 0.0340(9) 0.0388(9) 0.0535(11) 0.0163(8) 0.0113(8) -0.0007(7) O5 0.0452(8) 0.0611(9) 0.0825(11) 0.0439(8) 0.0153(7) -0.0003(7) N6 0.0296(7) 0.0418(8) 0.0562(9) 0.0233(7) 0.0079(6) 0.0037(6) C6 0.0379(10) 0.0652(14) 0.0787(15) 0.0415(12) 0.0016(10) 0.0064(9) C7 0.0297(8) 0.0373(9) 0.0505(10) 0.0156(8) 0.0103(7) 0.0022(7) O7 0.0246(6) 0.0635(9) 0.0819(10) 0.0381(8) 0.0117(6) 0.0037(6) C7A 0.0267(8) 0.0334(8) 0.0498(10) 0.0131(7) 0.0125(7) 0.0036(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' 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 O1W Zn O1W 179.999(1) 2_666 . O1W Zn O2W 91.70(5) 2_666 . O1W Zn O2W 88.30(5) . . O1W Zn O2W 88.30(5) 2_666 2_666 O1W Zn O2W 91.70(5) . 2_666 O2W Zn O2W 180.0 . 2_666 O1W Zn N1P 89.31(6) 2_666 2_666 O1W Zn N1P 90.69(6) . 2_666 O2W Zn N1P 91.61(6) . 2_666 O2W Zn N1P 88.39(6) 2_666 2_666 O1W Zn N1P 90.69(6) 2_666 . O1W Zn N1P 89.31(6) . . O2W Zn N1P 88.39(6) . . O2W Zn N1P 91.61(6) 2_666 . N1P Zn N1P 179.999(2) 2_666 . Zn O1W H11W 119.5(16) . . Zn O1W H12W 118.5(16) . . H11W O1W H12W 103(2) . . Zn O2W H21W 115.3(16) . . Zn O2W H22W 131.3(17) . . H21W O2W H22W 108(2) . . C6P N1P C2P 116.31(17) . . C6P N1P Zn 123.23(13) . . C2P N1P Zn 120.36(12) . . N1P C2P C3P 123.72(17) . . N1P C2P H2P 119.9 . . C3P C2P H2P 116.3 . . C2P C3P C4P 119.12(18) . . C2P C3P H3P 122.2 . . C4P C3P H3P 118.7 . . C5P C4P C3P 117.90(19) . . C5P C4P S 124.80(16) . . C3P C4P S 117.29(16) . . C6P C5P C4P 119.18(18) . . C6P C5P H5P 118.5 . . C4P C5P H5P 122.3 . . N1P C6P C5P 123.74(18) . . N1P C6P H6P 116.3 . . C5P C6P H6P 120.0 . . C4P S C4Q 102.96(10) . . C2Q N1Q C6Q 116.8(3) . . N1Q C2Q C3Q 124.6(3) . . N1Q C2Q H2Q 119.2 . . C3Q C2Q H2Q 116.2 . . C4Q C3Q C2Q 118.0(3) . . C4Q C3Q H3Q 120.0 . . C2Q C3Q H3Q 122.0 . . C3Q C4Q C5Q 118.9(3) . . C3Q C4Q S 119.7(2) . . C5Q C4Q S 121.3(2) . . C4Q C5Q C6Q 117.6(3) . . C4Q C5Q H5Q 122.6 . . C6Q C5Q H5Q 119.9 . . N1Q C6Q C5Q 124.0(3) . . N1Q C6Q H6Q 117.6 . . C5Q C6Q H6Q 118.4 . . N2 N1 C7A 106.55(14) . . N1 N2 N3 111.61(14) . . C3A N3 N2 105.19(14) . . N3 C3A N4 127.84(15) . . N3 C3A C7A 109.60(15) . . N4 C3A C7A 122.53(16) . . C5 N4 C3A 119.60(14) . . C5 N4 C4 119.99(15) . . C3A N4 C4 120.37(15) . . N4 C4 H41 113.0 . . N4 C4 H42 109.5 . . H41 C4 H42 108.8 . . N4 C4 H43 104.9 . . H41 C4 H43 110.1 . . H42 C4 H43 110.5 . . O5 C5 N4 122.25(16) . . O5 C5 N6 120.74(17) . . N4 C5 N6 117.01(15) . . C7 N6 C5 126.23(15) . . C7 N6 C6 117.87(15) . . C5 N6 C6 115.89(15) . . N6 C6 H61 108.6 . . N6 C6 H62 107.1 . . H61 C6 H62 109.4 . . N6 C6 H63 113.0 . . H61 C6 H63 107.5 . . H62 C6 H63 111.2 . . O7 C7 N6 120.56(16) . . O7 C7 C7A 126.76(16) . . N6 C7 C7A 112.68(14) . . N1 C7A C3A 107.05(15) . . N1 C7A C7 131.07(15) . . C3A C7A C7 121.81(16) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Zn O1W 2.0988(12) 2_666 Zn O1W 2.0988(12) . Zn O2W 2.1192(13) . Zn O2W 2.1193(13) 2_666 Zn N1P 2.1475(16) 2_666 Zn N1P 2.1475(16) . O1W H11W 0.831(10) . O1W H12W 0.833(9) . O2W H21W 0.839(10) . O2W H22W 0.837(10) . N1P C6P 1.344(2) . N1P C2P 1.346(2) . C2P C3P 1.361(3) . C2P H2P 0.9307 . C3P C4P 1.394(3) . C3P H3P 0.9715 . C4P C5P 1.379(3) . C4P S 1.755(2) . C5P C6P 1.369(3) . C5P H5P 0.9319 . C6P H6P 0.9719 . S C4Q 1.782(2) . N1Q C2Q 1.292(4) . N1Q C6Q 1.309(4) . C2Q C3Q 1.377(4) . C2Q H2Q 0.9474 . C3Q C4Q 1.359(4) . C3Q H3Q 0.9567 . C4Q C5Q 1.367(4) . C5Q C6Q 1.386(4) . C5Q H5Q 0.9480 . C6Q H6Q 0.9562 . N1 N2 1.319(2) . N1 C7A 1.359(2) . N2 N3 1.365(2) . N3 C3A 1.328(2) . C3A N4 1.372(2) . C3A C7A 1.375(2) . N4 C5 1.366(2) . N4 C4 1.463(2) . C4 H41 1.0010 . C4 H42 0.9820 . C4 H43 0.9720 . C5 O5 1.216(2) . C5 N6 1.410(2) . N6 C7 1.400(2) . N6 C6 1.467(2) . C6 H61 0.9563 . C6 H62 0.9934 . C6 H63 0.9897 . C7 O7 1.228(2) . C7 C7A 1.418(2) . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H11W N2 0.831(10) 1.977(11) 2.786(2) 164(2) 2_566 O1W H12W N1 0.833(9) 1.933(10) 2.7609(19) 172(2) . O2W H21W N3 0.839(10) 1.920(10) 2.758(2) 177(2) 1_655 O2W H22W O7 0.837(10) 1.953(11) 2.7751(18) 167(2) .