#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:03:15 +0100 (vie 25 de mar de 2016) $
#$Revision: 179738 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/34/7003467.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_7003467
loop_
_publ_author_name
'Tangoulis, V.'
'Panagoulis, D.'
'Raptopoulou, C. P.'
'Dendrinou-Samara, C.'
_publ_section_title
;
 Low-dimensional copper(ii) complexes triply bridged with
 azide/carboxylate/DMSO showing very strong ferromagnetic interaction
 and influence of dipolar fields at low temperatures: a quantum Monte
 Carlo magnetic study
;
_journal_issue                   13
_journal_name_full               'Dalton Transactions'
_journal_page_first              1752
_journal_page_last               1760
_journal_paper_doi               10.1039/b716291j
_journal_year                    2008
_chemical_formula_sum            'C14 H18 Cu3 N12 O6 S4'
_chemical_formula_weight         769.26
_chemical_name_systematic
;
?
;
_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                103.69(2)
_cell_angle_beta                 115.89(3)
_cell_angle_gamma                98.88(2)
_cell_formula_units_Z            1
_cell_length_a                   8.331(5)
_cell_length_b                   10.657(6)
_cell_length_c                   9.147(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      27
_cell_measurement_theta_min      11
_cell_volume                     678.3(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'P21 Nicolet upgraded by Crystal Logic'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2190
_diffrn_reflns_theta_full        59.01
_diffrn_reflns_theta_max         59.01
_diffrn_reflns_theta_min         5.72
_diffrn_standards_decay_%        -2.9
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.113
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.54
_exptl_absorpt_correction_type   'psi-scan empirical'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.883
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parall
_exptl_crystal_F_000             385
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.842
_refine_diff_density_min         -1.079
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       0.013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         1945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0658
_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)+(0.1499P)²+0.5071P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1835
_refine_ls_wR_factor_ref         0.1855
_reflns_number_gt                1888
_reflns_number_total             1945
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b716291j.txt
_cod_data_source_block           keg1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7003467
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.0000 0.5000 0.0000 0.0393(4) Uani 1 2 d S . .
Cu2 Cu 0.31595(8) 0.45026(6) 0.32414(7) 0.0398(4) Uani 1 1 d . . .
O1 O -0.0036(4) 0.3147(3) -0.0907(4) 0.0481(9) Uani 1 1 d . . .
O2 O 0.2268(4) 0.2834(3) 0.1344(4) 0.0449(8) Uani 1 1 d . . .
N1 N 0.0672(5) 0.4839(4) 0.2310(5) 0.0408(9) Uani 1 1 d . . .
N4 N 0.4497(6) 0.5988(4) 0.5493(5) 0.0542(11) Uani 1 1 d . . .
C1 C 0.0988(6) 0.2477(4) -0.0208(5) 0.0390(10) Uani 1 1 d . C .
C2 C 0.0675(6) 0.1111(4) -0.1328(6) 0.0413(10) Uani 1 1 d . . .
C4 C -0.0538(10) -0.0850(7) -0.3722(8) 0.080(2) Uani 1 1 d . . .
H4 H -0.1259 -0.1464 -0.4845 0.105 Uiso 1 1 calc R A 1
C5 C 0.0810(9) -0.1135(6) -0.2482(8) 0.0637(15) Uani 1 1 d . C .
H5 H 0.1082 -0.1952 -0.2676 0.083 Uiso 1 1 calc R B 1
C3 C -0.0825(7) 0.0492(4) -0.3221(5) 0.0852(16) Uani 0.750(7) 1 d P C 1
S1 S 0.1941(2) 0.00799(16) -0.0591(2) 0.0530(7) Uani 0.750(7) 1 d P C 1
C3A C 0.1941(2) 0.00799(16) -0.0591(2) 0.0530(7) Uani 0.250(7) 1 d P C 2
S1A S -0.0825(7) 0.0492(4) -0.3221(5) 0.0852(16) Uani 0.250(7) 1 d P C 2
N2 N 0.0229(6) 0.5523(4) 0.3250(5) 0.0492(10) Uani 1 1 d . . .
N3 N -0.0285(8) 0.6119(6) 0.4078(7) 0.0750(15) Uani 1 1 d . . .
N5 N 0.4338(6) 0.7112(5) 0.5843(5) 0.0514(11) Uani 1 1 d . . .
N6 N 0.4197(8) 0.8175(6) 0.6217(7) 0.0799(16) Uani 1 1 d . . .
S2 S 0.50277(18) 0.67794(14) 0.15634(19) 0.0581(5) Uani 1 1 d . . .
O3 O 0.3571(5) 0.5644(4) 0.1444(5) 0.0605(10) Uani 1 1 d . . .
C6 C 0.4117(10) 0.6811(7) -0.0543(9) 0.0751(17) Uani 1 1 d . . .
H6A H 0.4054 0.5981 -0.1293 0.098 Uiso 1 1 calc R . .
H6B H 0.4910 0.7557 -0.0561 0.098 Uiso 1 1 calc R . .
H6C H 0.2887 0.6911 -0.0934 0.098 Uiso 1 1 calc R . .
C7 C 0.4726(11) 0.8309(7) 0.2517(10) 0.0818(19) Uani 1 1 d . . .
H7A H 0.5246 0.8490 0.3738 0.106 Uiso 1 1 calc R . .
H7B H 0.3418 0.8232 0.2009 0.106 Uiso 1 1 calc R . .
H7C H 0.5349 0.9034 0.2322 0.106 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 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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
O1 Cu1 O1 180.0 2_565 . ?
O1 Cu1 N1 91.14(14) 2_565 2_565 ?
O1 Cu1 N1 88.86(14) . 2_565 ?
O1 Cu1 N1 88.86(14) 2_565 . ?
O1 Cu1 N1 91.14(14) . . ?
N1 Cu1 N1 180.0(2) 2_565 . ?
O1 Cu1 O3 92.49(13) 2_565 . ?
O1 Cu1 O3 87.51(13) . . ?
N1 Cu1 O3 101.28(14) 2_565 . ?
N1 Cu1 O3 78.72(14) . . ?
O2 Cu2 N4 166.03(15) . . ?
O2 Cu2 N1 93.04(15) . . ?
N4 Cu2 N1 99.17(16) . . ?
O2 Cu2 N4 88.92(15) . 2_666 ?
N4 Cu2 N4 77.72(19) . 2_666 ?
N1 Cu2 N4 167.72(18) . 2_666 ?
O2 Cu2 O3 87.44(15) . . ?
N4 Cu2 O3 100.57(18) . . ?
N1 Cu2 O3 83.67(15) . . ?
N4 Cu2 O3 108.54(17) 2_666 . ?
C1 O1 Cu1 130.6(3) . . ?
C1 O2 Cu2 130.2(3) . . ?
N2 N1 Cu1 120.1(3) . . ?
N2 N1 Cu2 121.4(3) . . ?
Cu1 N1 Cu2 107.57(17) . . ?
N5 N4 Cu2 128.8(3) . . ?
N5 N4 Cu2 124.6(3) . 2_666 ?
Cu2 N4 Cu2 102.28(19) . 2_666 ?
O1 C1 O2 127.7(4) . . ?
O1 C1 C2 116.5(4) . . ?
O2 C1 C2 115.8(4) . . ?
C1 C2 C3 123.5(4) . . ?
C1 C2 S1 122.5(3) . . ?
C3 C2 S1 114.0(3) . . ?
C5 C4 C3 116.9(5) . . ?
C5 C4 H4 121.6 . . ?
C3 C4 H4 121.6 . . ?
C4 C5 S1 114.4(4) . . ?
C4 C5 H5 122.8 . . ?
S1 C5 H5 122.8 . . ?
C4 C3 C2 101.8(4) . . ?
C5 S1 C2 93.0(3) . . ?
N3 N2 N1 176.2(5) . . ?
N6 N5 N4 178.1(6) . . ?
O3 S2 C6 104.2(3) . . ?
O3 S2 C7 106.4(3) . . ?
C6 S2 C7 98.0(4) . . ?
S2 O3 Cu2 138.7(2) . . ?
S2 O3 Cu1 133.0(2) . . ?
Cu2 O3 Cu1 81.35(11) . . ?
S2 C6 H6A 109.5 . . ?
S2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
S2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
S2 C7 H7A 109.5 . . ?
S2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
S2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
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
Cu1 O1 1.943(3) 2_565 ?
Cu1 O1 1.943(3) . ?
Cu1 N1 1.994(4) 2_565 ?
Cu1 N1 1.994(4) . ?
Cu1 O3 2.564(4) . ?
Cu2 O2 1.931(3) . ?
Cu2 N4 1.974(4) . ?
Cu2 N1 1.995(4) . ?
Cu2 N4 2.013(4) 2_666 ?
Cu2 O3 2.369(4) . ?
O1 C1 1.255(5) . ?
O2 C1 1.262(5) . ?
N1 N2 1.212(5) . ?
N4 N5 1.208(6) . ?
N4 Cu2 2.013(4) 2_666 ?
C1 C2 1.476(6) . ?
C2 C3 1.520(6) . ?
C2 S1 1.691(5) . ?
C4 C5 1.340(9) . ?
C4 C3 1.484(7) . ?
C4 H4 0.9300 . ?
C5 S1 1.642(6) . ?
C5 H5 0.9300 . ?
N2 N3 1.140(6) . ?
N5 N6 1.143(7) . ?
S2 O3 1.522(4) . ?
S2 C6 1.747(7) . ?
S2 C7 1.768(7) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
