#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:44:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179732 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/28/7002876.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_7002876
loop_
_publ_author_name
'Maldonado, Carmen R.'
'Quirós, Miguel'
'Salas, Juan M.'
'Rodríguez-Diéguez, Antonio'
_publ_section_title
;
 Versatile binding behaviour of
 4,6-dimethyl-1,2,3-triazolo[4,5-d]-pyrimidin-5,7-dionato in the
 presence of bipyrimidine. Supramolecular H-bond architectures
;
_journal_issue                   46
_journal_name_full               'Dalton Transactions'
_journal_page_first              10311
_journal_page_last               10317
_journal_paper_doi               10.1039/b913541c
_journal_year                    2009
_chemical_formula_moiety         'C32 H38 Cd2 N24 O12, 6(H2 O)'
_chemical_formula_sum            'C32 H50 Cd2 N24 O18'
_chemical_formula_weight         1283.76
_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                90.286(1)
_cell_angle_beta                 105.216(1)
_cell_angle_gamma                114.417(1)
_cell_formula_units_Z            1
_cell_length_a                   10.5968(5)
_cell_length_b                   10.7757(5)
_cell_length_c                   11.7018(6)
_cell_measurement_reflns_used    8224
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.4
_cell_measurement_theta_min      2.2
_cell_volume                     1164.21(10)
_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      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.907
_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  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13738
_diffrn_reflns_theta_full        26.80
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        -0.0
_diffrn_standards_number         309
_exptl_absorpt_coefficient_mu    1.015
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             650
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.535
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5279
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.001
_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+1.7000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0783
_reflns_number_gt                5044
_reflns_number_total             5279
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b913541c.txt
_cod_data_source_block           cdaxbpir
_cod_database_code               7002876
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd Cd 0.28417(2) 0.498981(19) 0.255354(16) 0.01423(7) Uani 1 1 d . . .
N1A N 0.2491(2) 0.2087(2) 0.1519(2) 0.0169(5) Uani 1 1 d . . .
N2A N 0.1827(2) 0.2644(2) 0.2004(2) 0.0171(5) Uani 1 1 d . . .
N3A N 0.0571(2) 0.1690(2) 0.2179(2) 0.0170(5) Uani 1 1 d . . .
C3AA C 0.0479(3) 0.0488(3) 0.1767(2) 0.0150(5) Uani 1 1 d . . .
N4A N -0.0608(2) -0.0805(2) 0.1706(2) 0.0159(4) Uani 1 1 d . . .
C4A C -0.1924(3) -0.1026(3) 0.2034(3) 0.0203(6) Uani 1 1 d . . .
H41A H -0.2779 -0.1624 0.1388 0.024 Uiso 1 1 d R . .
H42A H -0.1953 -0.0141 0.2166 0.024 Uiso 1 1 d R . .
H43A H -0.1919 -0.1461 0.2768 0.024 Uiso 1 1 d R . .
C5A C -0.0508(3) -0.1923(3) 0.1244(2) 0.0162(5) Uani 1 1 d . . .
O5A O -0.1455(2) -0.30847(19) 0.11740(17) 0.0189(4) Uani 1 1 d . . .
N6A N 0.0717(2) -0.1690(2) 0.0866(2) 0.0165(4) Uani 1 1 d . . .
C6A C 0.0821(3) -0.2896(3) 0.0384(3) 0.0206(6) Uani 1 1 d . . .
H61A H 0.0192 -0.3723 0.0654 0.025 Uiso 1 1 d R . .
H62A H 0.1825 -0.2778 0.0667 0.025 Uiso 1 1 d R . .
H63A H 0.0514 -0.2991 -0.0491 0.025 Uiso 1 1 d R . .
C7A C 0.1844(3) -0.0402(3) 0.0880(2) 0.0168(5) Uani 1 1 d . . .
O7A O 0.2863(2) -0.0291(2) 0.05110(18) 0.0225(4) Uani 1 1 d . . .
C7AA C 0.1650(3) 0.0705(3) 0.1359(2) 0.0158(5) Uani 1 1 d . . .
N1B N 0.3672(2) 0.7346(2) 0.2822(2) 0.0162(4) Uani 1 1 d . . .
N2B N 0.4870(2) 0.8002(2) 0.2492(2) 0.0179(5) Uani 1 1 d . . .
N3B N 0.5392(2) 0.9379(2) 0.2750(2) 0.0174(5) Uani 1 1 d . . .
C3AB C 0.4491(3) 0.9579(3) 0.3270(2) 0.0150(5) Uani 1 1 d . . .
N4B N 0.4580(2) 1.0807(2) 0.3695(2) 0.0169(5) Uani 1 1 d . . .
C4B C 0.5754(3) 1.2116(3) 0.3633(3) 0.0197(6) Uani 1 1 d . . .
H41B H 0.6603 1.1970 0.3616 0.024 Uiso 1 1 d R . .
H42B H 0.6007 1.2767 0.4334 0.024 Uiso 1 1 d R . .
H43B H 0.5438 1.2488 0.2907 0.024 Uiso 1 1 d R . .
C5B C 0.3540(3) 1.0824(3) 0.4181(2) 0.0178(5) Uani 1 1 d . . .
O5B O 0.3564(2) 1.1894(2) 0.45682(18) 0.0230(4) Uani 1 1 d . . .
N6B N 0.2427(2) 0.9543(2) 0.4214(2) 0.0174(5) Uani 1 1 d . . .
C6B C 0.1342(3) 0.9590(3) 0.4756(3) 0.0235(6) Uani 1 1 d . . .
H61B H 0.1778 0.9859 0.5620 0.028 Uiso 1 1 d R . .
H62B H 0.0521 0.8681 0.4600 0.028 Uiso 1 1 d R . .
H63B H 0.1003 1.0263 0.4409 0.028 Uiso 1 1 d R . .
C7B C 0.2254(3) 0.8258(3) 0.3778(2) 0.0168(5) Uani 1 1 d . . .
O7B O 0.1180(2) 0.7201(2) 0.38117(18) 0.0227(4) Uani 1 1 d . . .
C7AB C 0.3402(3) 0.8330(3) 0.3317(2) 0.0150(5) Uani 1 1 d . . .
N1P N 0.3104(2) 0.4634(2) 0.4637(2) 0.0149(4) Uani 1 1 d . . .
C2P C 0.4423(3) 0.4829(3) 0.5306(2) 0.0136(5) Uani 1 1 d . . .
N3P N 0.4786(2) 0.4739(2) 0.6474(2) 0.0140(4) Uani 1 1 d . . .
C4P C 0.3743(3) 0.4412(3) 0.7017(2) 0.0175(5) Uani 1 1 d . . .
H4P H 0.3969 0.4344 0.7849 0.021 Uiso 1 1 d R . .
C5P C 0.2344(3) 0.4172(3) 0.6391(3) 0.0197(6) Uani 1 1 d . . .
H5P H 0.1602 0.3926 0.6773 0.024 Uiso 1 1 d R . .
C6P C 0.2067(3) 0.4303(3) 0.5189(3) 0.0184(5) Uani 1 1 d . . .
H6P H 0.1118 0.4155 0.4740 0.022 Uiso 1 1 d R . .
O1W O 0.3256(2) 0.5131(2) 0.07310(19) 0.0257(5) Uani 1 1 d D . .
H11W H 0.268(3) 0.453(3) 0.016(2) 0.031 Uiso 1 1 d D . .
H12W H 0.380(3) 0.578(3) 0.045(3) 0.031 Uiso 1 1 d D . .
O2W O 0.0647(2) 0.4966(2) 0.23839(19) 0.0219(4) Uani 1 1 d D . .
H21W H 0.000(3) 0.424(2) 0.252(3) 0.026 Uiso 1 1 d D . .
H22W H 0.074(4) 0.566(2) 0.280(3) 0.026 Uiso 1 1 d D . .
O3W O 0.6298(2) 0.1324(2) 0.1121(2) 0.0282(5) Uani 1 1 d D . .
H31W H 0.645(4) 0.093(3) 0.058(2) 0.034 Uiso 1 1 d D . .
H32W H 0.594(4) 0.069(3) 0.152(3) 0.034 Uiso 1 1 d D . .
O4W O -0.1182(2) 0.2680(2) 0.2914(2) 0.0295(5) Uani 1 1 d D . .
H41W H -0.192(3) 0.238(4) 0.230(2) 0.035 Uiso 1 1 d D . .
H42W H -0.071(4) 0.226(3) 0.274(3) 0.035 Uiso 1 1 d D . .
O5W O 0.5066(3) 0.3150(2) 0.0511(2) 0.0330(5) Uani 1 1 d D . .
H51W H 0.537(4) 0.254(3) 0.061(4) 0.040 Uiso 1 1 d D . .
H52W H 0.429(2) 0.294(4) 0.070(3) 0.040 Uiso 1 1 d 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'
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
_geom_angle_publ_flag
O2W Cd O1W 109.49(8) . . ?
O2W Cd N1B 84.33(7) . . ?
O1W Cd N1B 89.24(8) . . ?
O2W Cd N2A 92.18(8) . . ?
O1W Cd N2A 84.71(8) . . ?
N1B Cd N2A 171.60(8) . . ?
O2W Cd N3P 157.12(8) . 2_666 ?
O1W Cd N3P 92.27(8) . 2_666 ?
N1B Cd N3P 89.14(7) . 2_666 ?
N2A Cd N3P 96.91(8) . 2_666 ?
O2W Cd N1P 89.83(7) . . ?
O1W Cd N1P 160.13(8) . . ?
N1B Cd N1P 97.48(8) . . ?
N2A Cd N1P 90.13(8) . . ?
N3P Cd N1P 69.27(7) 2_666 . ?
N2A N1A C7AA 105.6(2) . . ?
N1A N2A N3A 112.9(2) . . ?
N1A N2A Cd 120.51(17) . . ?
N3A N2A Cd 126.47(17) . . ?
C3AA N3A N2A 104.0(2) . . ?
N3A C3AA C7AA 109.8(2) . . ?
N3A C3AA N4A 127.7(2) . . ?
C7AA C3AA N4A 122.4(2) . . ?
C5A N4A C3AA 119.0(2) . . ?
C5A N4A C4A 118.4(2) . . ?
C3AA N4A C4A 122.4(2) . . ?
N4A C4A H41A 109.5 . . ?
N4A C4A H42A 109.4 . . ?
H41A C4A H42A 109.5 . . ?
N4A C4A H43A 109.5 . . ?
H41A C4A H43A 109.5 . . ?
H42A C4A H43A 109.5 . . ?
O5A C5A N4A 120.7(2) . . ?
O5A C5A N6A 121.4(2) . . ?
N4A C5A N6A 117.9(2) . . ?
C7A N6A C5A 126.0(2) . . ?
C7A N6A C6A 116.5(2) . . ?
C5A N6A C6A 117.5(2) . . ?
N6A C6A H61A 109.4 . . ?
N6A C6A H62A 109.5 . . ?
H61A C6A H62A 109.5 . . ?
N6A C6A H63A 109.5 . . ?
H61A C6A H63A 109.5 . . ?
H62A C6A H63A 109.5 . . ?
O7A C7A N6A 121.7(2) . . ?
O7A C7A C7AA 125.8(3) . . ?
N6A C7A C7AA 112.5(2) . . ?
N1A C7AA C3AA 107.6(2) . . ?
N1A C7AA C7A 130.3(2) . . ?
C3AA C7AA C7A 122.1(2) . . ?
N2B N1B C7AB 106.9(2) . . ?
N2B N1B Cd 112.74(16) . . ?
C7AB N1B Cd 140.01(18) . . ?
N1B N2B N3B 111.2(2) . . ?
C3AB N3B N2B 105.9(2) . . ?
N3B C3AB N4B 127.5(2) . . ?
N3B C3AB C7AB 109.5(2) . . ?
N4B C3AB C7AB 123.0(2) . . ?
C3AB N4B C5B 119.7(2) . . ?
C3AB N4B C4B 121.6(2) . . ?
C5B N4B C4B 118.7(2) . . ?
N4B C4B H41B 109.5 . . ?
N4B C4B H42B 109.5 . . ?
H41B C4B H42B 109.5 . . ?
N4B C4B H43B 109.5 . . ?
H41B C4B H43B 109.5 . . ?
H42B C4B H43B 109.5 . . ?
O5B C5B N4B 122.3(3) . . ?
O5B C5B N6B 120.9(3) . . ?
N4B C5B N6B 116.8(2) . . ?
C7B N6B C5B 126.5(2) . . ?
C7B N6B C6B 117.8(2) . . ?
C5B N6B C6B 115.6(2) . . ?
N6B C6B H61B 109.5 . . ?
N6B C6B H62B 109.5 . . ?
H61B C6B H62B 109.5 . . ?
N6B C6B H63B 109.5 . . ?
H61B C6B H63B 109.5 . . ?
H62B C6B H63B 109.5 . . ?
O7B C7B N6B 120.3(2) . . ?
O7B C7B C7AB 126.7(3) . . ?
N6B C7B C7AB 113.0(2) . . ?
N1B C7AB C3AB 106.5(2) . . ?
N1B C7AB C7B 132.6(2) . . ?
C3AB C7AB C7B 120.9(2) . . ?
C2P N1P C6P 116.9(2) . . ?
C2P N1P Cd 116.70(17) . . ?
C6P N1P Cd 126.35(18) . . ?
N3P C2P N1P 125.1(2) . . ?
N3P C2P C2P 117.6(3) . 2_666 ?
N1P C2P C2P 117.3(3) . 2_666 ?
C2P N3P C4P 117.4(2) . . ?
C2P N3P Cd 119.02(17) . 2_666 ?
C4P N3P Cd 123.41(18) . 2_666 ?
N3P C4P C5P 121.3(2) . . ?
N3P C4P H4P 119.4 . . ?
C5P C4P H4P 119.4 . . ?
C6P C5P C4P 117.5(3) . . ?
C6P C5P H5P 121.3 . . ?
C4P C5P H5P 121.2 . . ?
N1P C6P C5P 121.7(2) . . ?
N1P C6P H6P 119.1 . . ?
C5P C6P H6P 119.1 . . ?
Cd O1W H11W 120(3) . . ?
Cd O1W H12W 132(3) . . ?
H11W O1W H12W 107(3) . . ?
Cd O2W H21W 117(2) . . ?
Cd O2W H22W 111(2) . . ?
H21W O2W H22W 110(3) . . ?
H31W O3W H32W 104(4) . . ?
H41W O4W H42W 100(4) . . ?
H51W O5W H52W 113(4) . . ?
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
Cd O2W 2.271(2) . ?
Cd O1W 2.281(2) . ?
Cd N1B 2.306(2) . ?
Cd N2A 2.309(2) . ?
Cd N3P 2.364(2) 2_666 ?
Cd N1P 2.431(2) . ?
N1A N2A 1.317(3) . ?
N1A C7AA 1.364(3) . ?
N2A N3A 1.373(3) . ?
N3A C3AA 1.335(3) . ?
C3AA C7AA 1.377(4) . ?
C3AA N4A 1.379(3) . ?
N4A C5A 1.373(3) . ?
N4A C4A 1.469(3) . ?
C4A H41A 0.9800 . ?
C4A H42A 0.9800 . ?
C4A H43A 0.9800 . ?
C5A O5A 1.224(3) . ?
C5A N6A 1.406(3) . ?
N6A C7A 1.405(3) . ?
N6A C6A 1.471(3) . ?
C6A H61A 0.9800 . ?
C6A H62A 0.9800 . ?
C6A H63A 0.9800 . ?
C7A O7A 1.226(3) . ?
C7A C7AA 1.426(4) . ?
N1B N2B 1.334(3) . ?
N1B C7AB 1.369(3) . ?
N2B N3B 1.352(3) . ?
N3B C3AB 1.343(3) . ?
C3AB N4B 1.368(3) . ?
C3AB C7AB 1.377(4) . ?
N4B C5B 1.372(3) . ?
N4B C4B 1.463(3) . ?
C4B H41B 0.9800 . ?
C4B H42B 0.9800 . ?
C4B H43B 0.9800 . ?
C5B O5B 1.225(3) . ?
C5B N6B 1.406(4) . ?
N6B C7B 1.395(4) . ?
N6B C6B 1.468(3) . ?
C6B H61B 0.9800 . ?
C6B H62B 0.9800 . ?
C6B H63B 0.9800 . ?
C7B O7B 1.243(3) . ?
C7B C7AB 1.429(4) . ?
N1P C2P 1.339(3) . ?
N1P C6P 1.343(3) . ?
C2P N3P 1.334(3) . ?
C2P C2P 1.494(5) 2_666 ?
N3P C4P 1.342(3) . ?
N3P Cd 2.364(2) 2_666 ?
C4P C5P 1.383(4) . ?
C4P H4P 0.9500 . ?
C5P C6P 1.380(4) . ?
C5P H5P 0.9500 . ?
C6P H6P 0.9500 . ?
O1W H11W 0.836(10) . ?
O1W H12W 0.837(10) . ?
O2W H21W 0.847(10) . ?
O2W H22W 0.848(10) . ?
O3W H31W 0.850(10) . ?
O3W H32W 0.847(10) . ?
O4W H41W 0.850(10) . ?
O4W H42W 0.853(10) . ?
O5W H51W 0.846(10) . ?
O5W H52W 0.843(10) . ?
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 O5A 0.836(10) 1.943(11) 2.777(3) 176(4) 2
O1W H12W O5W 0.837(10) 1.900(14) 2.714(3) 164(4) 2_665
O2W H22W O7B 0.848(10) 1.851(11) 2.693(3) 172(3) .
O2W H21W O4W 0.847(10) 1.786(11) 2.629(3) 173(4) .
O3W H31W O7A 0.850(10) 1.875(13) 2.715(3) 169(4) 2_655
O3W H32W N3B 0.847(10) 2.042(13) 2.879(3) 169(4) 1_545
O4W H42W N3A 0.853(10) 1.954(13) 2.792(3) 167(4) .
O4W H41W O3W 0.850(10) 1.901(14) 2.733(3) 166(4) 1_455
O5W H52W N1A 0.843(10) 2.222(14) 3.044(3) 165(4) .
O5W H51W O3W 0.846(10) 1.944(13) 2.781(3) 170(4) .
