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#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100148.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_1100148
loop_
_publ_author_name
'Mohammad Abul-Haj'
'Miguel Quiros'
'Juan M. Salas'
_publ_section_title
;
Diaquabis(nitrato-O)bis(4,7-dihydro-1,2,4-triazolo
[1,5-a]pyrimidine-7-one-N³)copper(II).
;
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m903
_journal_page_last               m905
_journal_paper_doi               10.1107/S1600536803019974
_journal_volume                  59
_journal_year                    2003
_chemical_formula_moiety         'C10 H12 Cu N10 O10'
_chemical_formula_sum            'C10 H12 Cu N10 O10'
_chemical_formula_weight         495.84
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4717(5)
_cell_length_b                   6.4247(2)
_cell_length_c                   18.4846(6)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.6
_cell_measurement_theta_min      12.7
_cell_volume                     1718.63(10)
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE STADI4 4-circle-diffractometer'
_diffrn_measurement_method
;
 Scan width (ω) = 1.05 - 1.25, scan ratio 2\q:\w = 1.00
;
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3096
_diffrn_reflns_theta_full        32.45
_diffrn_reflns_theta_max         32.45
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        4.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.355
_exptl_absorpt_correction_T_max  0.7036
_exptl_absorpt_correction_T_min  0.5692
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'X-RED (Stoe, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brick-shaped
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.383
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.0078(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_gt    1.113
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         3092
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.088
_refine_ls_restrained_S_gt       1.113
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0650P)²+3.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.1658
_reflns_number_gt                2141
_reflns_number_total             3096
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             2202376
_cod_database_code               1100148
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cu Cu 0.5000 0.5000 0.5000 0.0276(2) Uani 1 d S .
N1 N 0.5490(2) 0.0712(4) 0.33448(14) 0.0393(6) Uani 1 d . .
C2 C 0.5189(2) 0.1410(5) 0.3969(2) 0.0375(6) Uani 1 d . .
H2 H 0.4894 0.0560 0.4304 0.045 Uiso 1 calc RT .
N3 N 0.5341(2) 0.3490(4) 0.40906(12) 0.0307(5) Uani 1 d . .
C3A C 0.5769(2) 0.4102(4) 0.34914(15) 0.0311(5) Uani 1 d . .
N4 N 0.6091(2) 0.5978(4) 0.3301(2) 0.0415(6) Uani 1 d . .
H4 H 0.6048 0.7019 0.3592 0.050 Uiso 1 calc RT .
C5 C 0.6487(2) 0.6202(6) 0.2636(2) 0.0456(8) Uani 1 d . .
H5 H 0.6712 0.7502 0.2502 0.055 Uiso 1 calc RT .
C6 C 0.6564(3) 0.4609(6) 0.2165(2) 0.0451(7) Uani 1 d . .
H6 H 0.6849 0.4838 0.1721 0.054 Uiso 1 calc RT .
C7 C 0.6220(2) 0.2581(5) 0.2329(2) 0.0354(6) Uani 1 d . .
O7 O 0.6210(2) 0.1020(4) 0.19453(12) 0.0458(6) Uani 1 d . .
N8 N 0.5860(2) 0.2468(4) 0.30352(12) 0.0317(5) Uani 1 d . .
N1N N 0.3085(2) 0.2281(5) 0.5033(2) 0.0455(7) Uani 1 d . .
O1N O 0.3890(2) 0.2359(4) 0.53173(13) 0.0403(5) Uani 1 d . .
O2N O 0.2998(2) 0.2337(6) 0.4369(2) 0.0764(10) Uani 1 d . .
O3N O 0.2405(2) 0.2160(6) 0.5432(2) 0.0724(10) Uani 1 d . .
O1W O 0.59055(15) 0.3231(4) 0.55131(12) 0.0359(5) Uani 1 d D .
H11W H 0.6388(19) 0.2951(66) 0.5275(19) 0.043 Uiso 1 d DT .
H12W H 0.6026(27) 0.3639(60) 0.5942(12) 0.043 Uiso 1 d DT .
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'
Cu Cu 0.3201 1.2651 '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
O1W Cu N3 87.75(9) . . y
O1W Cu O1N 85.44(9) . . y
N3 Cu O1N 91.59(9) . . y
C2 N1 N8 102.4(2) . . n
N1 C2 N3 115.1(3) . . n
N1 C2 H2 122.5 . . n
N3 C2 H2 122.4 . . n
C3A N3 C2 103.1(2) . . n
C3A N3 Cu 132.2(2) . . n
C2 N3 Cu 124.7(2) . . n
N3 C3A N4 130.4(3) . . n
N3 C3A N8 109.6(2) . . n
N4 C3A N8 120.0(3) . . n
C3A N4 C5 118.6(3) . . n
C3A N4 H4 120.7 . . n
C5 N4 H4 120.7 . . n
C6 C5 N4 122.4(3) . . n
C6 C5 H5 118.7 . . n
N4 C5 H5 118.8 . . n
C5 C6 C7 121.8(3) . . n
C5 C6 H6 119.1 . . n
C7 C6 H6 119.0 . . n
O7 C7 N8 119.3(3) . . n
O7 C7 C6 128.9(3) . . n
N8 C7 C6 111.9(3) . . n
C3A N8 N1 109.9(2) . . n
C3A N8 C7 125.0(3) . . n
N1 N8 C7 125.0(2) . . n
O3N N1N O2N 121.0(3) . . n
O3N N1N O1N 119.0(3) . . n
O2N N1N O1N 120.1(3) . . n
N1N O1N Cu 122.3(2) . . y
Cu O1W H11W 115(3) . . n
Cu O1W H12W 114(3) . . n
H11W O1W H12W 113(4) . . n
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
Cu O1W 1.977(2) . y
Cu N3 2.003(2) . y
Cu O1N 2.410(2) . y
N1 C2 1.312(4) . n
N1 N8 1.374(4) . n
C2 N3 1.373(4) . n
C2 H2 0.9300 . n
N3 C3A 1.328(4) . n
C3A N4 1.339(4) . n
C3A N8 1.353(4) . n
N4 C5 1.364(4) . n
N4 H4 0.8600 . n
C5 C6 1.348(5) . n
C5 H5 0.9300 . n
C6 C7 1.427(5) . n
C6 H6 0.9300 . n
C7 O7 1.228(4) . n
C7 N8 1.408(4) . n
N1N O3N 1.232(4) . n
N1N O2N 1.234(4) . n
N1N O1N 1.278(4) . n
O1W H11W 0.844(18) . n
O1W H12W 0.853(18) . n
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
_geom_hbond_publ_flag
N4 H4 O1N 0.86 2.06 2.769(4) 139.5(2) 5_666 n
O1W H11W O3N 0.84(2) 1.97(2) 2.797(4) 166(3) 4_556 n
O1W H12W O7 0.85(2) 1.89(1) 2.727(3) 168(4) 7_566 n
