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#$Date: 2016-03-23 16:37:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179386 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/83/4328305.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_4328305
loop_
_publ_author_name
'John A. Schlueter'
'Hyunsoo Park'
'Gregory J. Halder'
'William R. Armand'
'Cortney Dunmars'
'Karena W. Chapman'
'Jamie L. Manson'
'John Singleton'
'Ross McDonald'
'Alex Plonczak'
'Jinhee Kang'
'Chaghoon Lee'
'Myung-Hwan Whangbo'
'Tom Lancaster'
'Andrew J. Steele'
'Isabel Franke'
'Jack D. Wright'
'Stephen J. Blundell'
'Francis L. Pratt'
'Josepth deGeorge'
'Mark M. Turnbull'
'Christopher P. Landee'
_publ_contact_author_address
;
Materials Science Division
Argonne National Laboratory
Argonne, IL 60439-4831, USA
;
_publ_contact_author_email       JASchlueter@anl.gov
_publ_contact_author_fax         '(630) 252-9151'
_publ_contact_author_name        'Dr. John Schlueter'
_publ_contact_author_phone       '(630) 252-3588'
_publ_section_title
;
 Importance of Halogen...Halogen Contacts for the Structural and Magnetic
 Properties of CuX2(pyrazine-N,N'-dioxide)(H2O)2 (X = Cl and Br)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2121
_journal_page_last               2129
_journal_paper_doi               10.1021/ic201924q
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'Cu 2+, C4 H4 N2 O2, 2(Cl 1-), 2(H2 O)'
_chemical_formula_sum            'C4 H8 Cl2 Cu N2 O4'
_chemical_formula_weight         282.56
_chemical_name_common
; 
Copper(II) pyrazine dioxide dibromide dihydrate 
;
_chemical_name_systematic
; 
catena-((μ₂-pyrazine N,N'dioxide)-diaqua-dichloro-copper) 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL-97 cif file'
_cell_angle_alpha                90.00
_cell_angle_beta                 115.400(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.0515(7)
_cell_length_b                   5.5560(2)
_cell_length_c                   10.4254(5)
_cell_measurement_reflns_used    896
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.64
_cell_volume                     892.21(7)
_computing_cell_refinement       'Bruker APEX II Suite (2006)'
_computing_data_collection       'Bruker APEX II Suite (2006)'
_computing_data_reduction        'Bruker APEX II Suite (2006)'
_computing_molecular_graphics    'Diamond 3.1a (Crystal Impact, 2005)'
_computing_publication_material  'SHELXTL (Bruker, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'area detector ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5494
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.64
_diffrn_source_type              'Bruker APEX II'
_exptl_absorpt_coefficient_mu    3.029
_exptl_absorpt_correction_T_max  0.739
_exptl_absorpt_correction_T_min  0.378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; R. Blessing (1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.104
_exptl_crystal_description       needle
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       0.0115(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         1340
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0287P)²+1.0492P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0590
_reflns_number_gt                1328
_reflns_number_total             1340
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201924q_si_001_1.cif
_cod_data_source_block           CuCl2H2O2PyzNO
_cod_original_cell_volume        892.21(6)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4328305
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Cl1 Cl 0.379013(19) 0.13784(5) 0.17543(3) 0.01304(10) Uani 1 1 d .
Cu1 Cu 0.2500 0.2500 0.0000 0.00979(10) Uani 1 2 d S
O11 O 0.23319(7) 0.47710(18) 0.12920(11) 0.0163(2) Uani 1 1 d D
H11B H 0.2634(12) 0.472(4) 0.2146(17) 0.020 Uiso 1 1 d D
H11A H 0.2159(13) 0.610(3) 0.104(2) 0.020 Uiso 1 1 d D
O1 O 0.17081(6) -0.06260(16) 0.08257(10) 0.01169(18) Uani 1 1 d .
N1 N 0.08684(7) -0.03220(18) 0.04130(11) 0.0095(2) Uani 1 1 d .
C2 C 0.02920(8) -0.1881(2) -0.04988(14) 0.0131(2) Uani 1 1 d .
H2 H 0.0491 -0.3203 -0.0856 0.016 Uiso 1 1 calc R
C1 C 0.05823(8) 0.1564(2) 0.09133(14) 0.0135(2) Uani 1 1 d .
H1 H 0.0986 0.2671 0.1552 0.016 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.01380(15) 0.01489(15) 0.01002(16) 0.00101(9) 0.00472(11) 0.00456(9)
Cu1 0.01211(14) 0.01019(13) 0.00749(14) 0.00018(6) 0.00461(9) 0.00358(6)
O11 0.0226(5) 0.0150(4) 0.0090(4) -0.0005(3) 0.0045(4) 0.0089(4)
O1 0.0096(4) 0.0128(4) 0.0127(4) 0.0016(3) 0.0048(3) 0.0021(3)
N1 0.0107(4) 0.0099(4) 0.0087(5) 0.0010(3) 0.0049(4) 0.0009(3)
C2 0.0142(5) 0.0113(5) 0.0140(6) -0.0036(5) 0.0061(4) 0.0009(5)
C1 0.0140(6) 0.0115(5) 0.0142(6) -0.0049(4) 0.0054(5) -0.0005(4)
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O11 Cu1 O11 180.0 . 7
O11 Cu1 Cl1 90.01(3) . 7
O11 Cu1 Cl1 89.99(3) . .
Cl1 Cu1 Cl1 180.0 7 .
O11 Cu1 O1 87.24(4) . .
O11 Cu1 O1 92.76(4) 7 .
Cl1 Cu1 O1 89.34(2) 7 .
Cl1 Cu1 O1 90.66(2) . .
O1 Cu1 O1 180.00(4) 7 .
Cu1 O11 H11B 121.2(15) . .
Cu1 O11 H11A 121.2(15) . .
H11B O11 H11A 111(2) . .
N1 O1 Cu1 117.29(7) . .
O1 N1 C2 120.63(10) . .
O1 N1 C1 119.68(10) . .
C2 N1 C1 119.70(10) . .
N1 C2 C1 120.25(11) . 5
N1 C2 H2 119.9 . .
C1 C2 H2 119.9 5 .
N1 C1 C2 120.05(11) . 5
N1 C1 H1 120.0 . .
C2 C1 H1 120.0 5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cl1 Cu1 2.2630(3) .
Cu1 O11 1.9544(10) .
Cu1 O1 2.5647(9) .
O11 H11B 0.815(15) .
O11 H11A 0.796(15) .
O1 N1 1.3174(13) .
N1 C2 1.3484(16) .
N1 C1 1.3513(15) .
C2 C1 1.3738(17) 5
C2 H2 0.9500 .
C1 C2 1.3738(17) 5
C1 H1 0.9500 .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O11 Cu1 O1 N1 70.53(8) . .
O11 Cu1 O1 N1 -109.47(8) 7 .
Cl1 Cu1 O1 N1 -19.50(8) 7 .
Cl1 Cu1 O1 N1 160.50(8) . .
Cu1 O1 N1 C2 112.63(11) . .
Cu1 O1 N1 C1 -67.67(12) . .
O1 N1 C2 C1 179.38(12) . 5
C1 N1 C2 C1 -0.3(2) . 5
O1 N1 C1 C2 -179.38(12) . 5
C2 N1 C1 C2 0.3(2) . 5
