#------------------------------------------------------------------------------ #$Date: 2014-07-23 12:49:31 +0300 (Wed, 23 Jul 2014) $ #$Revision: 120677 $ #$URL: file:///home/coder/svn-repositories/cod/cif/3/00/00/3000003.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_3000003 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_year 2012 _chemical_formula_moiety 'C20 H24 Cd N4 O4 S2 2+, 2(C6 H6 N5 O2 1-)' _chemical_formula_sum 'C32 H36 Cd N14 O8 S2' _chemical_formula_weight 921.27 _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 100.942(1) _cell_angle_beta 99.816(1) _cell_angle_gamma 94.821(1) _cell_formula_units_Z 1 _cell_length_a 8.4223(6) _cell_length_b 10.1249(7) _cell_length_c 11.7854(8) _cell_measurement_reflns_used 7611 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.2 _cell_measurement_theta_min 2.4 _cell_volume 965.22(12) _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, 1997a)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997b)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 8.26 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.909 _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 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 11246 _diffrn_reflns_theta_full 26.70 _diffrn_reflns_theta_max 28.25 _diffrn_reflns_theta_min 1.79 _diffrn_standards_decay_% 0.1 _diffrn_standards_number 280 _exptl_absorpt_coefficient_mu 0.743 _exptl_absorpt_correction_T_max 0.957 _exptl_absorpt_correction_T_min 0.743 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_description laminae _exptl_crystal_F_000 470 _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.06 _refine_diff_density_max 1.228 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.087 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 273 _refine_ls_number_reflns 4355 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0311 _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^)+(0.0500P)^2^+0.6000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0821 _refine_ls_wR_factor_ref 0.0827 _reflns_number_gt 4228 _reflns_number_total 4355 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file cdaxss.cif _[local]_cod_data_source_block cdaxss _cod_depositor_comments ;Extending hold period by 9 months (from 2011-12-03 to 2012-09-03) Also changing journal name to Dalton Transactions Releasing structure 3000003 into public domain as published material. ; _cod_database_code 3000003 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 Cd Cd 0.5000 0.5000 0.5000 0.01387(8) Uani 1 2 d S O1W O 0.22244(17) 0.45967(15) 0.44931(14) 0.0181(3) Uani 1 1 d D H11W H 0.177(3) 0.5259(18) 0.473(2) 0.022 Uiso 1 1 d D H12W H 0.180(3) 0.402(2) 0.480(2) 0.022 Uiso 1 1 d D O2W O 0.49681(18) 0.28203(15) 0.52953(14) 0.0196(3) Uani 1 1 d D H21W H 0.5874(18) 0.254(3) 0.541(2) 0.023 Uiso 1 1 d D H22W H 0.438(3) 0.247(3) 0.569(2) 0.023 Uiso 1 1 d D N1P N 0.5148(2) 0.41641(17) 0.30690(16) 0.0182(3) Uani 1 1 d . C2P C 0.4056(3) 0.3130(2) 0.24269(19) 0.0191(4) Uani 1 1 d . H2P H 0.3173 0.2835 0.2760 0.023 Uiso 1 1 d R C3P C 0.4161(3) 0.2485(2) 0.13089(19) 0.0213(4) Uani 1 1 d . H3P H 0.3377 0.1748 0.0888 0.026 Uiso 1 1 d R C4P C 0.5434(3) 0.2924(2) 0.08013(19) 0.0229(4) Uani 1 1 d . C5P C 0.6534(3) 0.4021(2) 0.14405(19) 0.0221(4) Uani 1 1 d . H5P H 0.7394 0.4367 0.1112 0.026 Uiso 1 1 d R C6P C 0.6354(3) 0.4593(2) 0.25622(19) 0.0195(4) Uani 1 1 d . H6P H 0.7122 0.5332 0.3001 0.023 Uiso 1 1 d R S S 0.55248(9) 0.20445(8) -0.06205(6) 0.04056(18) Uani 1 1 d . N1Q N 1.0248(3) 0.3924(2) -0.1360(2) 0.0347(5) Uani 1 1 d . C2Q C 0.8822(3) 0.4245(3) -0.1822(2) 0.0325(5) Uani 1 1 d . H2Q H 0.8801 0.4873 -0.2328 0.039 Uiso 1 1 d R C3Q C 0.7350(3) 0.3707(2) -0.1606(2) 0.0298(5) Uani 1 1 d . H3Q H 0.6351 0.3960 -0.1958 0.036 Uiso 1 1 d R C4Q C 0.7387(3) 0.2805(2) -0.0873(2) 0.0260(5) Uani 1 1 d . C5Q C 0.8859(3) 0.2449(3) -0.0377(2) 0.0323(5) Uani 1 1 d . H5Q H 0.8916 0.1825 0.0134 0.039 Uiso 1 1 d R C6Q C 1.0251(3) 0.3044(3) -0.0654(2) 0.0364(6) Uani 1 1 d . H6Q H 1.1268 0.2807 -0.0318 0.044 Uiso 1 1 d R N1 N 0.0605(2) 0.26743(17) 0.54071(16) 0.0176(3) Uani 1 1 d . N2 N -0.0913(2) 0.29462(17) 0.51868(17) 0.0194(4) Uani 1 1 d . N3 N -0.1932(2) 0.21145(17) 0.56012(16) 0.0180(3) Uani 1 1 d . C3A C -0.0982(2) 0.13079(19) 0.60988(17) 0.0152(4) Uani 1 1 d . N4 N -0.1425(2) 0.03203(17) 0.66792(16) 0.0169(3) Uani 1 1 d . C4 C -0.3110(2) 0.0029(2) 0.6807(2) 0.0209(4) Uani 1 1 d . H41 H -0.3602 -0.0821 0.6266 0.025 Uiso 1 1 d R H42 H -0.3719 0.0769 0.6622 0.025 Uiso 1 1 d R H43 H -0.3135 -0.0055 0.7619 0.025 Uiso 1 1 d R C5 C -0.0256(2) -0.0368(2) 0.71831(18) 0.0182(4) Uani 1 1 d . O5 O -0.05697(18) -0.12111(16) 0.77554(15) 0.0242(3) Uani 1 1 d . N6 N 0.1340(2) -0.00652(17) 0.70155(16) 0.0172(3) Uani 1 1 d . C6 C 0.2534(3) -0.0891(2) 0.7499(2) 0.0231(4) Uani 1 1 d . H61 H 0.3492 -0.0824 0.7134 0.028 Uiso 1 1 d R H62 H 0.2051 -0.1838 0.7332 0.028 Uiso 1 1 d R H63 H 0.2855 -0.0560 0.8352 0.028 Uiso 1 1 d R C7 C 0.1888(2) 0.0941(2) 0.64530(18) 0.0166(4) Uani 1 1 d . O7 O 0.33266(17) 0.11534(15) 0.64023(14) 0.0215(3) Uani 1 1 d . C7A C 0.0594(2) 0.16294(19) 0.59840(18) 0.0153(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 Cd 0.01380(11) 0.01060(11) 0.01926(12) 0.00551(7) 0.00578(7) 0.00230(7) O1W 0.0173(7) 0.0128(7) 0.0281(8) 0.0096(6) 0.0084(6) 0.0033(5) O2W 0.0156(7) 0.0152(7) 0.0326(8) 0.0124(6) 0.0079(6) 0.0041(5) N1P 0.0193(8) 0.0140(8) 0.0231(9) 0.0059(7) 0.0065(7) 0.0020(6) C2P 0.0188(10) 0.0152(9) 0.0259(11) 0.0087(8) 0.0059(8) 0.0026(7) C3P 0.0223(10) 0.0169(10) 0.0236(11) 0.0057(8) 0.0020(8) -0.0028(8) C4P 0.0265(11) 0.0224(11) 0.0193(10) 0.0034(8) 0.0059(8) -0.0003(9) C5P 0.0239(10) 0.0198(10) 0.0235(11) 0.0055(8) 0.0085(8) -0.0026(8) C6P 0.0196(10) 0.0154(9) 0.0232(10) 0.0047(8) 0.0047(8) -0.0012(8) S 0.0420(4) 0.0461(4) 0.0254(3) -0.0088(3) 0.0139(3) -0.0189(3) N1Q 0.0334(11) 0.0361(12) 0.0334(12) 0.0016(9) 0.0130(9) -0.0026(9) C2Q 0.0448(15) 0.0287(12) 0.0250(12) 0.0080(10) 0.0085(10) -0.0001(11) C3Q 0.0362(13) 0.0272(12) 0.0243(11) 0.0048(9) -0.0002(10) 0.0072(10) C4Q 0.0329(12) 0.0233(11) 0.0195(10) -0.0004(9) 0.0075(9) -0.0030(9) C5Q 0.0404(14) 0.0285(12) 0.0283(12) 0.0100(10) 0.0027(10) 0.0040(10) C6Q 0.0290(13) 0.0361(14) 0.0416(15) 0.0049(12) 0.0013(11) 0.0074(11) N1 0.0163(8) 0.0131(8) 0.0258(9) 0.0081(7) 0.0063(7) 0.0025(6) N2 0.0176(8) 0.0141(8) 0.0302(10) 0.0100(7) 0.0083(7) 0.0035(6) N3 0.0173(8) 0.0130(8) 0.0267(9) 0.0084(7) 0.0070(7) 0.0030(6) C3A 0.0165(9) 0.0106(8) 0.0197(9) 0.0045(7) 0.0057(7) 0.0017(7) N4 0.0151(8) 0.0131(8) 0.0255(9) 0.0085(7) 0.0071(6) 0.0013(6) C4 0.0160(9) 0.0169(10) 0.0325(11) 0.0080(8) 0.0097(8) 0.0000(7) C5 0.0186(10) 0.0148(9) 0.0224(10) 0.0061(8) 0.0054(8) 0.0007(7) O5 0.0214(7) 0.0222(8) 0.0346(9) 0.0177(7) 0.0080(6) 0.0017(6) N6 0.0149(8) 0.0146(8) 0.0252(9) 0.0106(7) 0.0043(7) 0.0032(6) C6 0.0183(10) 0.0205(10) 0.0339(12) 0.0150(9) 0.0030(8) 0.0043(8) C7 0.0179(9) 0.0130(9) 0.0203(10) 0.0057(7) 0.0048(7) 0.0014(7) O7 0.0149(7) 0.0218(8) 0.0316(8) 0.0137(6) 0.0060(6) 0.0028(6) C7A 0.0152(9) 0.0110(9) 0.0213(10) 0.0061(7) 0.0047(7) 0.0013(7) 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' Cd Cd -0.8075 1.2024 '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 Cd O1W 180.0 . 2_666 O1W Cd O2W 92.55(5) . 2_666 O1W Cd O2W 87.45(5) 2_666 2_666 O1W Cd O2W 87.45(5) . . O1W Cd O2W 92.55(5) 2_666 . O2W Cd O2W 180.0 2_666 . O1W Cd N1P 89.07(6) . . O1W Cd N1P 90.93(6) 2_666 . O2W Cd N1P 91.93(6) 2_666 . O2W Cd N1P 88.07(6) . . O1W Cd N1P 90.93(6) . 2_666 O1W Cd N1P 89.07(6) 2_666 2_666 O2W Cd N1P 88.07(6) 2_666 2_666 O2W Cd N1P 91.93(6) . 2_666 N1P Cd N1P 180.0 . 2_666 Cd O1W H11W 113.1(18) . . Cd O1W H12W 114.9(18) . . H11W O1W H12W 101(3) . . Cd O2W H21W 115.6(18) . . Cd O2W H22W 125.2(19) . . H21W O2W H22W 109(3) . . C6P N1P C2P 117.38(19) . . C6P N1P Cd 122.96(14) . . C2P N1P Cd 119.48(14) . . N1P C2P C3P 122.9(2) . . N1P C2P H2P 118.6 . . C3P C2P H2P 118.5 . . C2P C3P C4P 119.1(2) . . C2P C3P H3P 120.5 . . C4P C3P H3P 120.4 . . C5P C4P C3P 118.4(2) . . C5P C4P S 124.44(17) . . C3P C4P S 117.16(17) . . C6P C5P C4P 118.6(2) . . C6P C5P H5P 120.7 . . C4P C5P H5P 120.7 . . N1P C6P C5P 123.50(19) . . N1P C6P H6P 118.2 . . C5P C6P H6P 118.3 . . C4P S C4Q 102.75(11) . . C2Q N1Q C6Q 117.3(2) . . N1Q C2Q C3Q 123.4(2) . . N1Q C2Q H2Q 118.3 . . C3Q C2Q H2Q 118.3 . . C4Q C3Q C2Q 118.1(2) . . C4Q C3Q H3Q 121.1 . . C2Q C3Q H3Q 120.9 . . C3Q C4Q C5Q 119.9(2) . . C3Q C4Q S 119.39(19) . . C5Q C4Q S 120.65(19) . . C4Q C5Q C6Q 117.2(2) . . C4Q C5Q H5Q 121.5 . . C6Q C5Q H5Q 121.3 . . N1Q C6Q C5Q 124.1(2) . . N1Q C6Q H6Q 118.0 . . C5Q C6Q H6Q 117.9 . . N2 N1 C7A 106.41(16) . . N1 N2 N3 111.77(16) . . C3A N3 N2 105.07(16) . . N3 C3A N4 127.71(18) . . N3 C3A C7A 109.55(17) . . N4 C3A C7A 122.71(18) . . C5 N4 C3A 119.33(17) . . C5 N4 C4 119.54(17) . . C3A N4 C4 121.09(17) . . N4 C4 H41 109.5 . . N4 C4 H42 109.5 . . H41 C4 H42 109.5 . . N4 C4 H43 109.4 . . H41 C4 H43 109.5 . . H42 C4 H43 109.5 . . O5 C5 N4 122.05(19) . . O5 C5 N6 120.76(19) . . N4 C5 N6 117.19(17) . . C7 N6 C5 126.61(17) . . C7 N6 C6 117.89(17) . . C5 N6 C6 115.49(16) . . N6 C6 H61 109.5 . . N6 C6 H62 109.4 . . H61 C6 H62 109.5 . . N6 C6 H63 109.5 . . H61 C6 H63 109.5 . . H62 C6 H63 109.5 . . O7 C7 N6 120.93(18) . . O7 C7 C7A 126.99(19) . . N6 C7 C7A 112.08(17) . . N1 C7A C3A 107.18(17) . . N1 C7A C7 130.85(18) . . C3A C7A C7 121.94(18) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cd O1W 2.2933(15) . Cd O1W 2.2933(15) 2_666 Cd O2W 2.2972(14) 2_666 Cd O2W 2.2973(14) . Cd N1P 2.3009(18) . Cd N1P 2.3009(18) 2_666 O1W H11W 0.828(10) . O1W H12W 0.831(10) . O2W H21W 0.836(10) . O2W H22W 0.836(10) . N1P C6P 1.345(3) . N1P C2P 1.347(3) . C2P C3P 1.376(3) . C2P H2P 0.9500 . C3P C4P 1.395(3) . C3P H3P 0.9500 . C4P C5P 1.389(3) . C4P S 1.759(2) . C5P C6P 1.378(3) . C5P H5P 0.9500 . C6P H6P 0.9500 . S C4Q 1.785(2) . N1Q C2Q 1.325(4) . N1Q C6Q 1.329(4) . C2Q C3Q 1.395(4) . C2Q H2Q 0.9500 . C3Q C4Q 1.369(3) . C3Q H3Q 0.9500 . C4Q C5Q 1.384(4) . C5Q C6Q 1.390(4) . C5Q H5Q 0.9500 . C6Q H6Q 0.9500 . N1 N2 1.323(2) . N1 C7A 1.362(3) . N2 N3 1.365(2) . N3 C3A 1.335(3) . C3A N4 1.375(3) . C3A C7A 1.376(3) . N4 C5 1.371(3) . N4 C4 1.464(3) . C4 H41 0.9800 . C4 H42 0.9800 . C4 H43 0.9800 . C5 O5 1.223(3) . C5 N6 1.409(3) . N6 C7 1.404(3) . N6 C6 1.470(2) . C6 H61 0.9800 . C6 H62 0.9800 . C6 H63 0.9800 . C7 O7 1.226(2) . C7 C7A 1.431(3) . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H11W N2 0.828(10) 2.002(13) 2.793(2) 159(3) 2_566 O1W H12W N1 0.831(10) 1.939(10) 2.767(2) 174(3) . O2W H21W N3 0.836(10) 1.917(11) 2.747(2) 172(3) 1_655 O2W H22W O7 0.836(10) 1.938(13) 2.742(2) 161(3) . _journal_paper_doi 10.1039/c2dt30992k