#------------------------------------------------------------------------------
#$Date: 2016-03-25 22:57:40 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180020 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/14/7031489.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_7031489
loop_
_publ_author_name
'Zilić, Dijana'
'Rakvin, Boris'
'Milić, Dalibor'
'Pajić, Damir'
'Dilović, Ivica'
'Cametti, Massimo'
'Džolić, Zoran'
_publ_section_title
;
 Crystal structures and magnetic properties of a set of dihalo-bridged
 oxalamidato copper(ii) dimers.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11877
_journal_page_last               11887
_journal_paper_doi               10.1039/c4dt00925h
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C30 H28 Br2 Cu2 N6 O4'
_chemical_formula_sum            'C30 H28 Br2 Cu2 N6 O4'
_chemical_formula_weight         823.48
_chemical_name_systematic
;
bis(μ-Bromo)-bis(N-benzyl-N'-((2-pyridin-2-yl)methyl)oxalamidato-N,N'',O)-
di-copper(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                93.172(5)
_cell_angle_beta                 90.749(5)
_cell_angle_gamma                94.721(5)
_cell_formula_units_Z            1
_cell_length_a                   8.0988(6)
_cell_length_b                   9.6585(6)
_cell_length_c                   10.1449(6)
_cell_measurement_reflns_used    1949
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.0328
_cell_measurement_theta_min      4.2327
_cell_volume                     789.53(9)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 16.3426
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0841
_diffrn_reflns_av_sigmaI/netI    0.0956
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9243
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.24
_exptl_absorpt_coefficient_mu    3.923
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             410
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0245P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0902
_reflns_number_gt                1927
_reflns_number_total             2771
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c4dt00925h2.cif
_cod_data_source_block           L2-Br
_cod_depositor_comments
'Adding full bibliography for 7031487--7031489.cif.'
_cod_database_code               7031489
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
C1 C 0.9535(6) 0.7051(6) -0.0147(5) 0.0197(13) Uani 1 1 d .
C2 C 1.0468(7) 0.7887(6) -0.0979(6) 0.0273(15) Uani 1 1 d .
H2 H 1.1383 0.8485 -0.0639 0.033 Uiso 1 1 calc R
C3 C 1.0057(7) 0.7841(6) -0.2292(6) 0.0295(15) Uani 1 1 d .
H3 H 1.0670 0.8424 -0.2868 0.035 Uiso 1 1 calc R
C4 C 0.8761(7) 0.6953(6) -0.2775(6) 0.0278(15) Uani 1 1 d .
H4 H 0.8469 0.6901 -0.3687 0.033 Uiso 1 1 calc R
C5 C 0.7880(7) 0.6129(6) -0.1904(5) 0.0243(14) Uani 1 1 d .
H5 H 0.6976 0.5513 -0.2235 0.029 Uiso 1 1 calc R
C6 C 0.9890(6) 0.7058(6) 0.1311(5) 0.0223(13) Uani 1 1 d .
H6A H 1.1026 0.6790 0.1472 0.027 Uiso 1 1 calc R
H6B H 0.9802 0.8001 0.1726 0.027 Uiso 1 1 calc R
C7 C 0.8790(6) 0.5759(5) 0.3113(6) 0.0197(13) Uani 1 1 d .
C8 C 0.7348(6) 0.4703(5) 0.3387(5) 0.0188(13) Uani 1 1 d .
C9 C 0.6069(7) 0.3118(5) 0.4956(5) 0.0245(14) Uani 1 1 d .
H9A H 0.4959 0.3365 0.4677 0.029 Uiso 1 1 calc R
H9B H 0.6085 0.3094 0.5930 0.029 Uiso 1 1 calc R
C10 C 0.6356(7) 0.1694(6) 0.4357(6) 0.0217(13) Uani 1 1 d .
C11 C 0.7366(7) 0.0848(6) 0.4986(6) 0.0323(16) Uani 1 1 d .
H11 H 0.7859 0.1150 0.5819 0.039 Uiso 1 1 calc R
C12 C 0.7669(8) -0.0440(6) 0.4410(7) 0.0405(18) Uani 1 1 d .
H12 H 0.8396 -0.1005 0.4835 0.049 Uiso 1 1 calc R
C13 C 0.6919(8) -0.0898(7) 0.3230(7) 0.0428(19) Uani 1 1 d .
H13 H 0.7099 -0.1794 0.2854 0.051 Uiso 1 1 calc R
C14 C 0.5911(8) -0.0072(6) 0.2588(7) 0.0368(17) Uani 1 1 d .
H14 H 0.5407 -0.0386 0.1762 0.044 Uiso 1 1 calc R
C15 C 0.5632(7) 0.1225(6) 0.3153(6) 0.0262(14) Uani 1 1 d .
H15 H 0.4935 0.1800 0.2709 0.031 Uiso 1 1 calc R
O1 O 0.9809(5) 0.6217(4) 0.3979(4) 0.0274(10) Uani 1 1 d .
O2 O 0.6256(4) 0.4382(4) 0.2505(3) 0.0244(9) Uani 1 1 d .
Cu1 Cu 0.69895(8) 0.51341(7) 0.07628(6) 0.0209(2) Uani 1 1 d .
Br1 Br 0.56223(7) 0.32384(6) -0.05807(6) 0.02422(18) Uani 1 1 d .
N1 N 0.8260(5) 0.6171(4) -0.0612(4) 0.0199(11) Uani 1 1 d .
N2 N 0.8681(5) 0.6068(4) 0.1870(4) 0.0192(11) Uani 1 1 d .
N3 N 0.7332(5) 0.4195(4) 0.4558(4) 0.0214(11) Uani 1 1 d .
H3N H 0.8113 0.4512 0.5135 0.026 Uiso 1 1 calc R
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'
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'
N N 0.0061 0.0033 '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_3
N1 C1 C2 121.4(5) .
N1 C1 C6 116.1(4) .
C2 C1 C6 122.5(5) .
C3 C2 C1 119.3(5) .
C3 C2 H2 120.3 .
C1 C2 H2 120.3 .
C2 C3 C4 119.8(5) .
C2 C3 H3 120.1 .
C4 C3 H3 120.1 .
C3 C4 C5 118.6(6) .
C3 C4 H4 120.7 .
C5 C4 H4 120.7 .
N1 C5 C4 122.4(5) .
N1 C5 H5 118.8 .
C4 C5 H5 118.8 .
N2 C6 C1 107.8(4) .
N2 C6 H6A 110.1 .
C1 C6 H6A 110.1 .
N2 C6 H6B 110.1 .
C1 C6 H6B 110.1 .
H6A C6 H6B 108.5 .
O1 C7 N2 129.5(5) .
O1 C7 C8 122.3(5) .
N2 C7 C8 108.2(5) .
O2 C8 N3 124.2(5) .
O2 C8 C7 119.3(5) .
N3 C8 C7 116.5(5) .
N3 C9 C10 112.1(4) .
N3 C9 H9A 109.2 .
C10 C9 H9A 109.2 .
N3 C9 H9B 109.2 .
C10 C9 H9B 109.2 .
H9A C9 H9B 107.9 .
C11 C10 C15 118.8(6) .
C11 C10 C9 120.6(5) .
C15 C10 C9 120.5(5) .
C10 C11 C12 120.4(6) .
C10 C11 H11 119.8 .
C12 C11 H11 119.8 .
C13 C12 C11 120.0(6) .
C13 C12 H12 120.0 .
C11 C12 H12 120.0 .
C12 C13 C14 120.5(6) .
C12 C13 H13 119.8 .
C14 C13 H13 119.8 .
C13 C14 C15 119.4(7) .
C13 C14 H14 120.3 .
C15 C14 H14 120.3 .
C10 C15 C14 120.8(6) .
C10 C15 H15 119.6 .
C14 C15 H15 119.6 .
C8 O2 Cu1 110.5(3) .
N2 Cu1 N1 81.32(18) .
N2 Cu1 O2 81.38(16) .
N1 Cu1 O2 162.69(16) .
N2 Cu1 Br1 156.64(14) .
N1 Cu1 Br1 100.66(12) .
O2 Cu1 Br1 95.16(10) .
N2 Cu1 Br1 109.77(14) 2_665
N1 Cu1 Br1 92.16(13) 2_665
O2 Cu1 Br1 93.86(11) 2_665
Br1 Cu1 Br1 93.47(3) 2_665
Cu1 Br1 Cu1 86.53(3) 2_665
C5 N1 C1 118.6(4) .
C5 N1 Cu1 126.0(4) .
C1 N1 Cu1 115.2(4) .
C7 N2 C6 121.1(4) .
C7 N2 Cu1 119.5(3) .
C6 N2 Cu1 119.4(3) .
C8 N3 C9 123.1(5) .
C8 N3 H3N 118.4 .
C9 N3 H3N 118.4 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.345(6) .
C1 C2 1.388(7) .
C1 C6 1.503(7) .
C2 C3 1.366(7) .
C2 H2 0.9500 .
C3 C4 1.368(7) .
C3 H3 0.9500 .
C4 C5 1.387(7) .
C4 H4 0.9500 .
C5 N1 1.340(6) .
C5 H5 0.9500 .
C6 N2 1.454(6) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 O1 1.236(6) .
C7 N2 1.316(6) .
C7 C8 1.525(7) .
C8 O2 1.258(6) .
C8 N3 1.310(6) .
C9 N3 1.475(6) .
C9 C10 1.510(7) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C11 1.377(8) .
C10 C15 1.385(7) .
C11 C12 1.387(8) .
C11 H11 0.9500 .
C12 C13 1.370(9) .
C12 H12 0.9500 .
C13 C14 1.371(9) .
C13 H13 0.9500 .
C14 C15 1.385(7) .
C14 H14 0.9500 .
C15 H15 0.9500 .
O2 Cu1 2.025(3) .
Cu1 N2 1.896(4) .
Cu1 N1 2.007(4) .
Cu1 Br1 2.4056(8) .
Cu1 Br1 2.7476(9) 2_665
Br1 Cu1 2.7476(9) 2_665
N3 H3N 0.8800 .
