#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/80/7028069.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_7028069
loop_
_publ_author_name
'Chen, Zhong-Ning'
'Zhang, Hua-Xin'
'Yu, Kai-Bei'
'Zheng, Kang-Cheng'
'Cai, Hu'
'Kang, Bei-Sheng'
_publ_section_title
;
 Extended network via hydrogen bond linkages of zig-zag co-ordination
 chains [{Cu2(trans-oxen)(μ-OH)(μ-H2O)}n]n+ or
 [Cu2(trans-oxen)(μ-OCN)2]n
 [H2oxen = N,N′-bis(2-aminoethyl)oxamide]
;
_journal_issue                   7
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1133
_journal_paper_doi               10.1039/a708615f
_journal_year                    1998
_chemical_formula_sum            'C3 H9.5 Br0.5 Cu N2 O3'
_chemical_formula_weight         225.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            36
_cell_length_a                   14.873(2)
_cell_length_b                   14.873(2)
_cell_length_c                   34.872(7)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      18.27
_cell_measurement_theta_min      2.77
_cell_volume                     6680.4(18)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '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  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2733
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        2.55
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.582
_exptl_absorpt_correction_T_max  0.9923
_exptl_absorpt_correction_T_min  0.6269
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    2.015
_exptl_crystal_F_000             4032
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.00017(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.909
_refine_ls_goodness_of_fit_obs   1.020
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         1323
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.910
_refine_ls_restrained_S_obs      1.022
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_obs          0.0349
_refine_ls_shift/esd_max         0.008
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0540P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0866
_refine_ls_wR_factor_obs         0.0820
_reflns_number_observed          965
_reflns_number_total             1323
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            f708615sup1.cif
_cod_data_source_block           y475
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6680.2(19)
_cod_original_sg_symbol_H-M      R-3c
_cod_original_formula_sum        'C3 H9.50 Br0.50 Cu N2 O3'
_cod_database_code               7028069
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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
Cu 0.0285(4) 0.0313(4) 0.0277(3) 0.0091(3) 0.0115(2) 0.0189(3)
O1 0.030(2) 0.033(2) 0.030(2) 0.0124(15) 0.0115(15) 0.020(2)
O2 0.022(2) 0.022(2) 0.020(2) -0.0036(9) 0.0036(9) 0.008(2)
O3 0.162(6) 0.070(3) 0.079(4) 0.003(3) 0.007(3) 0.074(4)
O4 0.045(3) 0.045(3) 0.057(4) -0.005(2) 0.005(2) 0.015(3)
N1 0.029(2) 0.031(2) 0.030(2) 0.011(2) 0.010(2) 0.019(2)
N2 0.031(2) 0.039(3) 0.054(3) 0.006(2) 0.008(2) 0.024(2)
C1 0.019(2) 0.021(2) 0.022(2) 0.004(2) 0.003(2) 0.007(2)
C2 0.041(3) 0.053(3) 0.045(3) 0.027(3) 0.014(3) 0.029(3)
C3 0.189(10) 0.182(9) 0.055(5) 0.071(5) 0.066(5) 0.172(9)
Br1 0.0472(4) 0.0472(4) 0.0528(7) 0.000 0.000 0.0236(2)
Br2 0.1036(10) 0.1036(10) 0.0472(11) 0.000 0.000 0.0518(5)
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Cu Cu 0.51821(4) -0.16253(4) 0.87224(2) 0.0274(2) Uani 1 d .
O1 O 0.7305(2) -0.0984(2) 0.79112(9) 0.0291(7) Uani 1 d .
O2 O 0.4390(3) -0.2277(3) 0.9167 0.0231(10) Uani 1 d S
O3 O 0.6335(5) 0.1678(4) 0.90834(14) 0.097(2) Uani 1 d .
O4 O 0.6543(4) -0.0124(4) 0.9167 0.0527(14) Uani 1 d SD
N1 N 0.5978(3) -0.1028(3) 0.82704(11) 0.0287(9) Uani 1 d .
N2 N 0.4641(3) -0.0655(3) 0.86105(13) 0.0385(11) Uani 1 d .
H2C H 0.3942(3) -0.1008(3) 0.86173(13) 0.046 Uiso 1 calc R
H2D H 0.4869(3) -0.0155(3) 0.87906(13) 0.046 Uiso 1 calc R
C1 C 0.6661(3) -0.1290(3) 0.81883(12) 0.0225(10) Uani 1 d .
C2 C 0.5763(4) -0.0334(4) 0.80548(15) 0.0435(14) Uani 1 d .
H2E H 0.5523(4) -0.0613(4) 0.78000(15) 0.052 Uiso 1 calc R
H2F H 0.6392(4) 0.0335(4) 0.80288(15) 0.052 Uiso 1 calc R
C3 C 0.4978(7) -0.0207(7) 0.8250(2) 0.107(4) Uani 1 d .
H3A H 0.5238(7) 0.0532(7) 0.8276(2) 0.129 Uiso 1 calc R
H3B H 0.4375(7) -0.0480(7) 0.8084(2) 0.129 Uiso 1 calc R
Br1 Br 0.6667 0.3333 0.98338(3) 0.0491(3) Uani 1 d S
Br2 Br 0.6667 0.3333 0.8333 0.0848(6) Uani 1 d S
H4OA H 0.7202(30) 0.0046(51) 0.9201(23) 0.104(30) Uiso 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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
O2 Cu N1 177.38(13) . .
O2 Cu N2 98.97(12) . .
N1 Cu N2 83.3(2) . .
O2 Cu O1 94.26(8) . 31_646
N1 Cu O1 83.63(14) . 31_646
N2 Cu O1 165.82(15) . 31_646
C1 O1 Cu 108.8(3) . 31_646
Cu O2 Cu 110.9(2) 10_546 .
C1 N1 C2 126.4(4) . .
C1 N1 Cu 116.3(3) . .
C2 N1 Cu 117.3(3) . .
C3 N2 Cu 109.9(3) . .
O1 C1 N1 128.8(4) . .
O1 C1 C1 119.0(5) . 31_646
N1 C1 C1 112.2(5) . 31_646
N1 C2 C3 109.4(4) . .
N2 C3 C2 119.0(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu O2 1.894(2) .
Cu N1 1.903(4) .
Cu N2 2.011(4) .
Cu O1 2.028(3) 31_646
O1 C1 1.274(5) .
O1 Cu 2.028(3) 31_646
O2 Cu 1.894(2) 10_546
N1 C1 1.289(6) .
N1 C2 1.436(6) .
N2 C3 1.393(7) .
C1 C1 1.516(8) 31_646
C2 C3 1.444(7) .
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
N1 Cu O2 Cu 126.0(31) . 10_546
N2 Cu O2 Cu -85.05(13) . 10_546
O1 Cu O2 Cu 89.83(10) 31_646 10_546
O2 Cu N1 C1 -37.5(33) . .
N2 Cu N1 C1 173.3(4) . .
O1 Cu N1 C1 -1.3(3) 31_646 .
O2 Cu N1 C2 142.5(30) . .
N2 Cu N1 C2 -6.7(4) . .
O1 Cu N1 C2 178.8(4) 31_646 .
O2 Cu N2 C3 -169.4(5) . .
N1 Cu N2 C3 9.2(5) . .
O1 Cu N2 C3 31.9(10) 31_646 .
Cu O1 C1 N1 -179.4(4) 31_646 .
Cu O1 C1 C1 2.3(6) 31_646 31_646
C2 N1 C1 O1 2.0(8) . .
Cu N1 C1 O1 -178.0(4) . .
C2 N1 C1 C1 -179.7(5) . 31_646
Cu N1 C1 C1 0.4(6) . 31_646
C1 N1 C2 C3 -177.4(6) . .
Cu N1 C2 C3 2.5(7) . .
Cu N2 C3 C2 -10.9(10) . .
N1 C2 C3 N2 5.9(11) . .
