#------------------------------------------------------------------------------
#$Date: 2016-02-18 09:40:55 +0100 (jue 18 de feb de 2016) $
#$Revision: 176722 $
#$URL: svn://www.crystallography.net/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_paper_doi               10.1039/c2dt30992k
_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       'φ and ω 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/[σ²(Fo²)+(0.0500P)²+0.6000P] where P=(Fo²+2Fc²)/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>2σ(I)
_cod_data_source_file            cdaxss.cif
_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_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) .
