#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500026.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_1500026
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quirós'
'Juan M. Salas'
'Antonio Rodríguez-Diéguez'
_publ_contact_author_address
;
     Departamento de Química Inorgánica
     Facultad de Ciencias
     Universidad de Granada
     18071 Granada
     SPAIN
;
_publ_contact_author_email       mquiros@ugr.es
_publ_contact_author_fax         34-58-248526
_publ_contact_author_name        'Miguel Quirós'
_publ_contact_author_phone       34-58-240441
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              1553
_journal_page_last               1558
_journal_paper_doi               10.1016/j.ica.2008.07.029
_journal_volume                  362
_journal_year                    2009
_chemical_formula_moiety         'Cd H12 O6 2+, 2 (C5 H4 N5 O2 1-)'
_chemical_formula_sum            'C10 H20 Cd N10 O10'
_chemical_formula_weight         552.76
_chemical_name_systematic
; 
 Hexaacua cadmium(II) 4,5,6,7-tetrahydro-4-methyl-5,7-dioxo-
 -1,2,3-triazolo-[4,5-d]-pyrimidinate 
;
_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                86.413(2)
_cell_angle_beta                 67.813(2)
_cell_angle_gamma                87.315(2)
_cell_formula_units_Z            1
_cell_length_a                   6.8110(8)
_cell_length_b                   8.7316(10)
_cell_length_c                   8.9234(10)
_cell_measurement_reflns_used    3487
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      2.5
_cell_volume                     490.27(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, 1997a)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.906
_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  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5761
_diffrn_reflns_theta_full        26.70
_diffrn_reflns_theta_max         28.40
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        0.1
_diffrn_standards_number         135
_exptl_absorpt_coefficient_mu    1.189
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.872
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             278
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         2223
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0250
_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)+(0.0400P)²+0.0800P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0640
_reflns_number_gt                2177
_reflns_number_total             2223
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cd4max.cif
_cod_data_source_block           cd4max
_cod_database_code               1500026
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 0.5000 0.5000 0.5000 0.03147(9) Uani 1 2 d S . .
O1W O 0.5169(3) 0.49348(19) 0.2430(2) 0.0390(4) Uani 1 1 d D . .
H11W H 0.419(3) 0.533(3) 0.223(4) 0.047 Uiso 1 1 d D . .
H12W H 0.546(5) 0.4125(19) 0.199(3) 0.047 Uiso 1 1 d D . .
O2W O 0.1457(3) 0.5407(2) 0.5922(2) 0.0473(4) Uani 1 1 d D . .
H21W H 0.104(5) 0.6293(16) 0.605(4) 0.057 Uiso 1 1 d D . .
H22W H 0.057(4) 0.475(3) 0.624(4) 0.057 Uiso 1 1 d D . .
O3W O 0.4458(4) 0.2441(2) 0.5400(2) 0.0576(6) Uani 1 1 d D . .
H31W H 0.408(5) 0.191(3) 0.623(2) 0.069 Uiso 1 1 d D . .
H32W H 0.478(5) 0.179(3) 0.473(3) 0.069 Uiso 1 1 d D . .
N1 N 0.6416(3) 0.2053(2) 0.1255(2) 0.0321(4) Uani 1 1 d . . .
N2 N 0.5961(3) 0.0954(2) 0.2412(2) 0.0358(4) Uani 1 1 d . . .
N3 N 0.6582(3) -0.0454(2) 0.1794(2) 0.0317(4) Uani 1 1 d . . .
C3A C 0.7441(3) -0.0190(2) 0.0194(2) 0.0250(4) Uani 1 1 d . . .
N4 N 0.8296(3) -0.12565(19) -0.09825(19) 0.0268(3) Uani 1 1 d . . .
C4 C 0.8318(4) -0.2901(2) -0.0542(3) 0.0364(5) Uani 1 1 d . . .
H41 H 0.7500 -0.3433 -0.1006 0.044 Uiso 1 1 d R . .
H42 H 0.7718 -0.3053 0.0617 0.044 Uiso 1 1 d R . .
H43 H 0.9754 -0.3293 -0.0944 0.044 Uiso 1 1 d R . .
C5 C 0.9034(3) -0.0748(2) -0.2565(2) 0.0281(4) Uani 1 1 d . . .
O5 O 0.9745(3) -0.16261(18) -0.36857(18) 0.0386(4) Uani 1 1 d . . .
N6 N 0.8983(3) 0.0817(2) -0.2887(2) 0.0299(4) Uani 1 1 d . . .
H6 H 0.9505 0.1116 -0.3893 0.036 Uiso 1 1 d R . .
C7 C 0.8199(3) 0.1968(2) -0.1800(2) 0.0278(4) Uani 1 1 d . . .
O7 O 0.8286(3) 0.33242(17) -0.22786(19) 0.0395(4) Uani 1 1 d . . .
C7A C 0.7360(3) 0.1360(2) -0.0169(2) 0.0262(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'
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 O2W 180.0 . 2_666 ?
O2W Cd O1W 91.18(7) . . ?
O2W Cd O1W 88.82(7) 2_666 . ?
O2W Cd O1W 88.82(7) . 2_666 ?
O2W Cd O1W 91.18(7) 2_666 2_666 ?
O1W Cd O1W 180.0 . 2_666 ?
O2W Cd O3W 91.02(8) . 2_666 ?
O2W Cd O3W 88.98(8) 2_666 2_666 ?
O1W Cd O3W 88.99(6) . 2_666 ?
O1W Cd O3W 91.01(6) 2_666 2_666 ?
O2W Cd O3W 88.98(8) . . ?
O2W Cd O3W 91.02(8) 2_666 . ?
O1W Cd O3W 91.01(6) . . ?
O1W Cd O3W 88.99(6) 2_666 . ?
O3W Cd O3W 180.0 2_666 . ?
Cd O1W H11W 117(2) . . ?
Cd O1W H12W 119(2) . . ?
H11W O1W H12W 107(3) . . ?
Cd O2W H21W 116(2) . . ?
Cd O2W H22W 126(2) . . ?
H21W O2W H22W 118(3) . . ?
Cd O3W H31W 130(2) . . ?
Cd O3W H32W 128(3) . . ?
H31W O3W H32W 101(3) . . ?
N2 N1 C7A 106.67(17) . . ?
N1 N2 N3 111.58(16) . . ?
C3A N3 N2 105.17(16) . . ?
N3 C3A C7A 109.51(17) . . ?
N3 C3A N4 127.71(18) . . ?
C7A C3A N4 122.79(17) . . ?
C5 N4 C3A 118.39(16) . . ?
C5 N4 C4 120.58(16) . . ?
C3A N4 C4 120.97(16) . . ?
N4 C4 H41 109.7 . . ?
N4 C4 H42 109.4 . . ?
H41 C4 H42 109.5 . . ?
N4 C4 H43 109.4 . . ?
H41 C4 H43 109.5 . . ?
H42 C4 H43 109.5 . . ?
O5 C5 N4 122.44(19) . . ?
O5 C5 N6 120.26(18) . . ?
N4 C5 N6 117.29(17) . . ?
C5 N6 C7 128.44(17) . . ?
C5 N6 H6 115.8 . . ?
C7 N6 H6 115.8 . . ?
O7 C7 N6 120.72(18) . . ?
O7 C7 C7A 127.68(19) . . ?
N6 C7 C7A 111.61(17) . . ?
N1 C7A C3A 107.08(17) . . ?
N1 C7A C7 131.54(19) . . ?
C3A C7A C7 121.38(17) . . ?
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 2.2545(18) . ?
Cd O2W 2.2546(18) 2_666 ?
Cd O1W 2.2566(16) . ?
Cd O1W 2.2566(16) 2_666 ?
Cd O3W 2.2658(18) 2_666 ?
Cd O3W 2.2658(18) . ?
O1W H11W 0.812(10) . ?
O1W H12W 0.811(10) . ?
O2W H21W 0.811(10) . ?
O2W H22W 0.811(10) . ?
O3W H31W 0.811(10) . ?
O3W H32W 0.811(10) . ?
N1 N2 1.321(2) . ?
N1 C7A 1.355(2) . ?
N2 N3 1.362(2) . ?
N3 C3A 1.331(2) . ?
C3A C7A 1.376(3) . ?
C3A N4 1.385(2) . ?
N4 C5 1.361(2) . ?
N4 C4 1.466(3) . ?
C4 H41 0.9601 . ?
C4 H42 0.9601 . ?
C4 H43 0.9601 . ?
C5 O5 1.232(2) . ?
C5 N6 1.380(3) . ?
N6 C7 1.384(3) . ?
N6 H6 0.8600 . ?
C7 O7 1.230(3) . ?
C7 C7A 1.424(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 H12W N1 0.811(10) 1.960(12) 2.758(2) 168(3) .
O1W H11W O7 0.812(10) 1.995(13) 2.783(2) 163(3) 2_665
O2W H21W O5 0.811(10) 1.971(11) 2.778(2) 173(3) 1_466
O2W H22W O7 0.811(10) 2.035(14) 2.817(2) 162(3) 1_456
O3W H32W N2 0.811(10) 2.084(17) 2.845(2) 156(3) .
O3W H31W N3 0.811(10) 2.024(11) 2.831(3) 174(3) 2_656
N6 H6 O5 0.86 2.05 2.896(2) 168.9 2_754
