#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/88/2218808.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2218808
loop_
_publ_author_name
'Kurawa, Mukhtar A.'
'Adams, Christopher J.'
'Orpen, A. Guy'
_publ_section_title
;2-Oxo-1,2-dihydropyrimidin-3-ium
 di-μ-chlorido-bis{dichloridobis[pyrimidin-2(1H)-one-κN³]cuprate(II)}
 dihydrate
;
_journal_coeditor_code           SG2250
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m924
_journal_page_last               m925
_journal_paper_doi               10.1107/S1600536808017455
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac
'(C4 H5 N2 O)2 [Cu2 Cl6 (C4 H4 N2 O)2], 2H2 O'
_chemical_formula_moiety
'2(C4 H5 N2 O +), C8 H8 Cl6 Cu2 N4 O2 2-, 2(H2 O)'
_chemical_formula_sum            'C16 H22 Cl6 Cu2 N8 O6'
_chemical_formula_weight         762.22
_chemical_name_systematic
;
2-Oxo-1,2-dihydropyrimidin-3-ium
di-μ-chlorido-bis{dichloridobis[pyrimidin-2(1H)-one-\kN³]cuprate(II)}
dihydrate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.032(3)
_cell_angle_beta                 100.508(4)
_cell_angle_gamma                102.035(4)
_cell_formula_units_Z            1
_cell_length_a                   7.5924(4)
_cell_length_b                   8.6401(3)
_cell_length_c                   10.6349(4)
_cell_measurement_reflns_used    10481
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.9994
_cell_measurement_theta_min      2.430
_cell_volume                     663.39(5)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2007)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2007)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2007)
;
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Gemini-R Ultra'
_diffrn_measurement_method       'ω (1° width)'
_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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14528
_diffrn_reflns_theta_full        30.12
_diffrn_reflns_theta_max         30.12
_diffrn_reflns_theta_min         2.44
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.258
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.433167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2007)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             382
_exptl_crystal_size_max          0.413
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.155
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.572
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         3902
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0238
_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)+(0.0422P)²+0.0753P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0693
_reflns_number_gt                3269
_reflns_number_total             3902
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sg2250.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2218808
_cod_database_fobs_code          2218808
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Cu Cu1 0.07237(3) 0.45037(2) 0.848449(17) 0.01007(6) Uani d . 1
Cl Cl1 -0.06435(5) 0.63425(4) 0.75599(3) 0.01291(8) Uani d . 1
Cl Cl2 0.19396(5) 0.64570(4) 1.06611(3) 0.01065(8) Uani d . 1
Cl Cl3 0.26769(6) 0.45986(5) 0.70847(4) 0.01557(9) Uani d . 1
N N1 0.18231(18) 0.28152(15) 0.92487(12) 0.0099(2) Uani d . 1
N N2 0.15847(19) 0.00585(15) 0.91842(13) 0.0122(3) Uani d . 1
H H2B 0.1020 -0.0912 0.8865 0.015 Uiso calc R 1
N N3 0.69462(19) 0.93935(16) 0.46681(12) 0.0124(3) Uani d . 1
H H3A 0.7819 1.0237 0.4760 0.015 Uiso calc R 1
N N4 0.43187(19) 0.76169(16) 0.34665(13) 0.0137(3) Uani d . 1
H H2A 0.3488 0.7298 0.2768 0.016 Uiso calc R 1
O O1 0.58355(18) 0.96484(15) 0.25699(12) 0.0204(3) Uani d . 1
O O2 -0.02211(17) 0.10178(14) 0.76366(11) 0.0176(2) Uani d . 1
O O3 0.93114(18) 0.22792(15) 0.49005(12) 0.0198(3) Uani d D 1
C C1 0.0983(2) 0.12810(17) 0.86166(15) 0.0116(3) Uani d . 1
C C2 0.3215(2) 0.30666(18) 1.02403(14) 0.0119(3) Uani d . 1
H H2C 0.3773 0.4116 1.0619 0.014 Uiso calc R 1
C C3 0.3900(2) 0.18275(18) 1.07546(15) 0.0132(3) Uani d . 1
H H3B 0.4917 0.2036 1.1436 0.016 Uiso calc R 1
C C4 0.3004(2) 0.03050(18) 1.02078(15) 0.0129(3) Uani d . 1
H H4A 0.3368 -0.0560 1.0538 0.016 Uiso calc R 1
C C5 0.5717(2) 0.89360(19) 0.34849(15) 0.0135(3) Uani d . 1
C C6 0.6850(2) 0.85959(19) 0.56744(15) 0.0134(3) Uani d . 1
H H6A 0.7744 0.8941 0.6433 0.016 Uiso calc R 1
C C7 0.5451(2) 0.72742(19) 0.56028(15) 0.0141(3) Uani d . 1
H H7A 0.5372 0.6718 0.6301 0.017 Uiso calc R 1
C C8 0.4167(2) 0.68029(19) 0.44567(15) 0.0139(3) Uani d . 1
H H8A 0.3194 0.5917 0.4373 0.017 Uiso calc R 1
H H1 0.947(3) 0.268(3) 0.4257(19) 0.037(7) Uiso d D 1
H H2 1.024(3) 0.267(3) 0.551(2) 0.044(8) Uiso d D 1
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'
Cl Cl 0.1484 0.1585 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 Cu1 Cl3 . . 88.53(4)
N1 Cu1 Cl1 . . 177.38(4)
Cl3 Cu1 Cl1 . . 91.956(15)
N1 Cu1 Cl2 . 2_567 88.05(4)
Cl3 Cu1 Cl2 . 2_567 157.928(16)
Cl1 Cu1 Cl2 . 2_567 90.538(15)
N1 Cu1 Cl2 . . 91.12(4)
Cl3 Cu1 Cl2 . . 115.984(15)
Cl1 Cu1 Cl2 . . 90.982(14)
Cl2 Cu1 Cl2 2_567 . 85.883(14)
Cu1 Cl2 Cu1 2_567 . 94.117(14)
C2 N1 C1 . . 120.92(13)
C2 N1 Cu1 . . 125.69(10)
C1 N1 Cu1 . . 113.38(10)
C4 N2 C1 . . 123.75(13)
C4 N2 H2B . . 118.1
C1 N2 H2B . . 118.1
C6 N3 C5 . . 123.65(14)
C6 N3 H3A . . 118.2
C5 N3 H3A . . 118.2
C8 N4 C5 . . 124.63(14)
C8 N4 H2A . . 117.7
C5 N4 H2A . . 117.7
H1 O3 H2 . . 109(2)
O2 C1 N1 . . 122.46(14)
O2 C1 N2 . . 122.11(14)
N1 C1 N2 . . 115.42(13)
N1 C2 C3 . . 123.13(14)
N1 C2 H2C . . 118.4
C3 C2 H2C . . 118.4
C4 C3 C2 . . 116.78(15)
C4 C3 H3B . . 121.6
C2 C3 H3B . . 121.6
N2 C4 C3 . . 119.63(14)
N2 C4 H4A . . 120.2
C3 C4 H4A . . 120.2
O1 C5 N4 . . 123.48(15)
O1 C5 N3 . . 123.19(15)
N4 C5 N3 . . 113.30(13)
N3 C6 C7 . . 120.87(15)
N3 C6 H6A . . 119.6
C7 C6 H6A . . 119.6
C6 C7 C8 . . 117.45(15)
C6 C7 H7A . . 121.3
C8 C7 H7A . . 121.3
N4 C8 C7 . . 120.03(15)
N4 C8 H8A . . 120.0
C7 C8 H8A . . 120.0
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 N1 . 1.9989(12) yes
Cu1 Cl3 . 2.2809(4) yes
Cu1 Cl1 . 2.2830(4) yes
Cu1 Cl2 2_567 2.3942(4) yes
Cu1 Cl2 . 2.6093(4) yes
Cl2 Cu1 2_567 2.3942(4) ?
N1 C2 . 1.314(2) ?
N1 C1 . 1.3854(19) ?
N2 C4 . 1.349(2) ?
N2 C1 . 1.3868(19) ?
N2 H2B . 0.8600 ?
N3 C6 . 1.337(2) ?
N3 C5 . 1.387(2) ?
N3 H3A . 0.8600 ?
N4 C8 . 1.335(2) ?
N4 C5 . 1.382(2) ?
N4 H2A . 0.8600 ?
O1 C5 . 1.2119(19) ?
O2 C1 . 1.221(2) ?
O3 H1 . 0.815(16) ?
O3 H2 . 0.844(17) ?
C2 C3 . 1.403(2) ?
C2 H2C . 0.9300 ?
C3 C4 . 1.361(2) ?
C3 H3B . 0.9300 ?
C4 H4A . 0.9300 ?
C6 C7 . 1.373(2) ?
C6 H6A . 0.9300 ?
C7 C8 . 1.378(2) ?
C7 H7A . 0.9300 ?
C8 H8A . 0.9300 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N2 H2B Cl1 1_545 0.86 2.56 3.4143(14) 170.8
N3 H3A O3 1_565 0.86 1.86 2.7099(18) 168.1
N4 H2A Cl2 1_554 0.86 2.30 3.1336(14) 164.7
O3 H1 Cl1 2_666 0.815(16) 2.428(17) 3.2258(13) 166(2)
O3 H2 Cl3 1_655 0.844(17) 2.454(18) 3.2653(13) 162(2)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
N1 Cu1 Cl2 Cu1 . 2_567 -87.97(4)
Cl3 Cu1 Cl2 Cu1 . 2_567 -176.875(16)
Cl1 Cu1 Cl2 Cu1 . 2_567 90.469(15)
Cl2 Cu1 Cl2 Cu1 2_567 2_567 0.0
Cl3 Cu1 N1 C2 . . 92.08(13)
Cl2 Cu1 N1 C2 2_567 . -109.72(13)
Cl2 Cu1 N1 C2 . . -23.88(13)
Cl3 Cu1 N1 C1 . . -87.19(10)
Cl2 Cu1 N1 C1 2_567 . 71.00(10)
Cl2 Cu1 N1 C1 . . 156.84(10)
C2 N1 C1 O2 . . -174.50(15)
Cu1 N1 C1 O2 . . 4.8(2)
C2 N1 C1 N2 . . 6.4(2)
Cu1 N1 C1 N2 . . -174.26(10)
C4 N2 C1 O2 . . 174.79(15)
C4 N2 C1 N1 . . -6.1(2)
C1 N1 C2 C3 . . -2.4(2)
Cu1 N1 C2 C3 . . 178.41(11)
N1 C2 C3 C4 . . -2.5(2)
C1 N2 C4 C3 . . 1.5(2)
C2 C3 C4 N2 . . 2.9(2)
C8 N4 C5 O1 . . 179.35(16)
C8 N4 C5 N3 . . -2.3(2)
C6 N3 C5 O1 . . -178.50(16)
C6 N3 C5 N4 . . 3.2(2)
C5 N3 C6 C7 . . -2.4(2)
N3 C6 C7 C8 . . 0.4(2)
C5 N4 C8 C7 . . 0.7(2)
C6 C7 C8 N4 . . 0.4(2)
