#------------------------------------------------------------------------------
#$Date: 2016-02-18 10:40:55 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176722 $
#$URL: svn://www.crystallography.net/cod/cif/3/00/00/3000002.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_3000002
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         'C10 H8 N2, Cd H12 O6 2+, 2(C6 H6 N5 O2 1-)'
_chemical_formula_sum            'C22 H32 Cd N12 O10'
_chemical_formula_weight         737.00
_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                109.292(1)
_cell_angle_beta                 107.638(1)
_cell_angle_gamma                101.821(1)
_cell_formula_units_Z            1
_cell_length_a                   8.5931(4)
_cell_length_b                   9.0396(4)
_cell_length_c                   10.9308(5)
_cell_measurement_reflns_used    6828
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      2.5
_cell_volume                     718.50(6)
_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 0.911
_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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8412
_diffrn_reflns_theta_full        26.70
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0.1
_diffrn_standards_number         255
_exptl_absorpt_coefficient_mu    0.837
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       laminae
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3265
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0231
_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)+(0.0300P)²+0.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0591
_refine_ls_wR_factor_ref         0.0592
_reflns_number_gt                3249
_reflns_number_total             3265
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cdax44.cif
_cod_data_source_block           cdax44
_cod_depositor_comments
;Changing journal name to Dalton Transactions
 Adding Fobs data.

 Requested journal is now Dalton Transactions

 Releasing structure 3000002 into public domain as published material.
;
_cod_database_code               3000002
_cod_database_fobs_code          3000002
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 0.01314(6) Uani 1 2 d S
O1W O 0.46315(16) 0.61624(16) 0.33923(13) 0.0181(2) Uani 1 1 d D
H11W H 0.453(3) 0.547(2) 0.2634(15) 0.022 Uiso 1 1 d D
H12W H 0.3710(18) 0.635(3) 0.324(2) 0.022 Uiso 1 1 d D
O2W O 0.40275(16) 0.24307(16) 0.31931(14) 0.0221(3) Uani 1 1 d D
H21W H 0.2999(16) 0.180(2) 0.271(2) 0.027 Uiso 1 1 d D
H22W H 0.466(3) 0.197(3) 0.287(2) 0.027 Uiso 1 1 d D
O3W O 0.76846(16) 0.52666(16) 0.51070(14) 0.0216(3) Uani 1 1 d D
H31W H 0.8601(19) 0.599(2) 0.5728(19) 0.026 Uiso 1 1 d D
H32W H 0.795(3) 0.452(2) 0.461(2) 0.026 Uiso 1 1 d D
N1 N 0.92618(18) 0.22141(18) 0.28711(15) 0.0167(3) Uani 1 1 d .
N2 N 0.79603(18) 0.25600(18) 0.31636(15) 0.0178(3) Uani 1 1 d .
N3 N 0.64619(18) 0.12198(18) 0.24361(15) 0.0170(3) Uani 1 1 d .
C3A C 0.6884(2) 0.0002(2) 0.16681(17) 0.0140(3) Uani 1 1 d .
N4 N 0.58234(18) -0.16017(18) 0.07393(15) 0.0150(3) Uani 1 1 d .
C4 C 0.3989(2) -0.2203(2) 0.0488(2) 0.0192(3) Uani 1 1 d .
H41 H 0.3284 -0.2785 -0.0532 0.023 Uiso 1 1 d R
H42 H 0.3637 -0.1257 0.0899 0.023 Uiso 1 1 d R
H43 H 0.3819 -0.2972 0.0930 0.023 Uiso 1 1 d R
C5 C 0.6499(2) -0.2665(2) 0.00167(17) 0.0141(3) Uani 1 1 d .
O5 O 0.55900(16) -0.40869(15) -0.08491(13) 0.0179(2) Uani 1 1 d .
N6 N 0.82737(18) -0.20628(17) 0.03219(15) 0.0143(3) Uani 1 1 d .
C6 C 0.8967(2) -0.3253(2) -0.04288(19) 0.0189(3) Uani 1 1 d .
H61 H 0.8483 -0.4343 -0.0444 0.023 Uiso 1 1 d R
H62 H 1.0235 -0.2853 0.0059 0.023 Uiso 1 1 d R
H63 H 0.8647 -0.3358 -0.1401 0.023 Uiso 1 1 d R
C7 C 0.9433(2) -0.0447(2) 0.12453(17) 0.0143(3) Uani 1 1 d .
O7 O 1.09625(15) -0.00578(15) 0.14063(13) 0.0177(2) Uani 1 1 d .
C7A C 0.8616(2) 0.0591(2) 0.19210(17) 0.0147(3) Uani 1 1 d .
N1P N 0.1852(2) 0.7336(2) 0.31515(17) 0.0228(3) Uani 1 1 d .
C2P C 0.2687(3) 0.8977(2) 0.3896(2) 0.0234(4) Uani 1 1 d .
H2P H 0.3801 0.9426 0.3917 0.028 Uiso 1 1 d R
C3P C 0.2026(2) 1.0062(2) 0.4640(2) 0.0209(4) Uani 1 1 d .
H3P H 0.2689 1.1214 0.5168 0.025 Uiso 1 1 d R
C4P C 0.0380(2) 0.9443(2) 0.46034(18) 0.0171(3) Uani 1 1 d .
C5P C -0.0518(2) 0.7742(2) 0.3793(2) 0.0212(4) Uani 1 1 d .
H5P H -0.1660 0.7264 0.3708 0.025 Uiso 1 1 d R
C6P C 0.0268(3) 0.6752(2) 0.3110(2) 0.0241(4) Uani 1 1 d .
H6P H -0.0356 0.5592 0.2582 0.029 Uiso 1 1 d R
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'
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
O3W Cd O3W 180.0 . 2_666
O3W Cd O2W 89.13(5) . .
O3W Cd O2W 90.87(5) 2_666 .
O3W Cd O2W 90.87(5) . 2_666
O3W Cd O2W 89.12(5) 2_666 2_666
O2W Cd O2W 180.0 . 2_666
O3W Cd O1W 91.95(5) . 2_666
O3W Cd O1W 88.05(5) 2_666 2_666
O2W Cd O1W 90.29(5) . 2_666
O2W Cd O1W 89.71(5) 2_666 2_666
O3W Cd O1W 88.05(5) . .
O3W Cd O1W 91.95(5) 2_666 .
O2W Cd O1W 89.70(5) . .
O2W Cd O1W 90.29(5) 2_666 .
O1W Cd O1W 179.999(2) 2_666 .
Cd O1W H11W 108.7(16) . .
Cd O1W H12W 109.5(16) . .
H11W O1W H12W 106(2) . .
Cd O2W H21W 127.3(17) . .
Cd O2W H22W 124.9(17) . .
H21W O2W H22W 108(2) . .
Cd O3W H31W 127.5(17) . .
Cd O3W H32W 124.3(17) . .
H31W O3W H32W 107(2) . .
N2 N1 C7A 106.37(13) . .
N1 N2 N3 112.07(13) . .
C3A N3 N2 104.90(13) . .
N3 C3A N4 127.93(15) . .
N3 C3A C7A 109.45(15) . .
N4 C3A C7A 122.61(15) . .
C3A N4 C5 119.12(14) . .
C3A N4 C4 121.76(14) . .
C5 N4 C4 119.12(14) . .
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 121.27(15) . .
O5 C5 N6 121.25(15) . .
N4 C5 N6 117.47(14) . .
C7 N6 C5 126.68(14) . .
C7 N6 C6 117.28(14) . .
C5 N6 C6 116.03(14) . .
N6 C6 H61 109.4 . .
N6 C6 H62 109.5 . .
H61 C6 H62 109.5 . .
N6 C6 H63 109.5 . .
H61 C6 H63 109.5 . .
H62 C6 H63 109.5 . .
O7 C7 N6 120.65(15) . .
O7 C7 C7A 127.16(15) . .
N6 C7 C7A 112.20(14) . .
N1 C7A C3A 107.21(14) . .
N1 C7A C7 130.96(15) . .
C3A C7A C7 121.84(15) . .
C6P N1P C2P 116.47(16) . .
N1P C2P C3P 123.99(18) . .
N1P C2P H2P 118.0 . .
C3P C2P H2P 118.0 . .
C2P C3P C4P 119.27(17) . .
C2P C3P H3P 120.4 . .
C4P C3P H3P 120.4 . .
C3P C4P C5P 116.96(16) . .
C3P C4P C4P 121.3(2) . 2_576
C5P C4P C4P 121.8(2) . 2_576
C6P C5P C4P 119.48(17) . .
C6P C5P H5P 120.2 . .
C4P C5P H5P 120.3 . .
N1P C6P C5P 123.77(17) . .
N1P C6P H6P 118.1 . .
C5P C6P H6P 118.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd O3W 2.2324(12) .
Cd O3W 2.2325(12) 2_666
Cd O2W 2.2731(13) .
Cd O2W 2.2731(13) 2_666
Cd O1W 2.3047(13) 2_666
Cd O1W 2.3047(13) .
O1W H11W 0.823(10) .
O1W H12W 0.823(10) .
O2W H21W 0.835(10) .
O2W H22W 0.839(10) .
O3W H31W 0.825(10) .
O3W H32W 0.834(10) .
N1 N2 1.321(2) .
N1 C7A 1.360(2) .
N2 N3 1.365(2) .
N3 C3A 1.336(2) .
C3A N4 1.374(2) .
C3A C7A 1.380(2) .
N4 C5 1.374(2) .
N4 C4 1.464(2) .
C4 H41 0.9800 .
C4 H42 0.9800 .
C4 H43 0.9800 .
C5 O5 1.223(2) .
C5 N6 1.402(2) .
N6 C7 1.402(2) .
N6 C6 1.471(2) .
C6 H61 0.9800 .
C6 H62 0.9800 .
C6 H63 0.9800 .
C7 O7 1.229(2) .
C7 C7A 1.430(2) .
N1P C6P 1.336(3) .
N1P C2P 1.337(3) .
C2P C3P 1.388(3) .
C2P H2P 0.9500 .
C3P C4P 1.393(3) .
C3P H3P 0.9500 .
C4P C5P 1.394(3) .
C4P C4P 1.494(3) 2_576
C5P C6P 1.388(3) .
C5P H5P 0.9500 .
C6P H6P 0.9500 .
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 H12W N1P 0.823(10) 1.974(11) 2.783(2) 167(2) .
O1W H11W O5 0.823(10) 1.895(10) 2.7149(17) 174(2) 2_655
O2W H21W O7 0.835(10) 1.901(12) 2.7136(17) 164(2) 1_455
O2W H22W N3 0.839(10) 1.936(11) 2.7654(19) 170(2) .
O3W H31W N1 0.825(10) 1.945(10) 2.7690(19) 176(2) 2_766
O3W H32W N2 0.834(10) 1.952(11) 2.7682(19) 166(2) .
