#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:52:43 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180100 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/46/7054673.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_7054673
loop_
_publ_author_name
'Hazra, Susanta'
'Karmakar, Anirban'
'Guedes da Silva, Maria de Fátima C.'
'Dlháň, L'ubor'
'Boča, Roman'
'Pombeiro, Armando J. L.'
_publ_section_title
;
 Sulfonated Schiff base dinuclear and polymeric copper(ii) complexes:
 crystal structures, magnetic properties and catalytic application in
 Henry reaction
;
_journal_issue                   5
_journal_name_full               'New J. Chem.'
_journal_page_first              3424
_journal_paper_doi               10.1039/C5NJ00330J
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C24 H18 Cu2 N10 O6 S2'
_chemical_formula_sum            'C24 H18 Cu2 N10 O6 S2'
_chemical_formula_weight         733.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-10-23 deposited with the CCDC.
2015-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3215(10)
_cell_length_b                   12.3215(9)
_cell_length_c                   16.7717(12)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.33
_cell_measurement_theta_min      2.43
_cell_volume                     2752.9(3)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II PHOTON  100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32709
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    1.758
_exptl_absorpt_correction_T_max  0.8564
_exptl_absorpt_correction_T_min  0.6005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.953
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2518
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0366
_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)+(0.0578P)²+1.5300P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.0989
_reflns_number_gt                2083
_reflns_number_total             2518
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj00330j2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7054673--7054675.cif.'
_cod_database_code               7054673
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -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
C1 C 0.1297(2) 0.2830(2) 0.58619(17) 0.0333(6) Uani 1 1 d .
C2 C 0.1490(2) 0.3247(3) 0.51155(17) 0.0358(7) Uani 1 1 d .
C3 C 0.1427(3) 0.4362(3) 0.4989(2) 0.0426(8) Uani 1 1 d .
H3 H 0.1583 0.4643 0.4489 0.051 Uiso 1 1 calc R
C4 C 0.1138(3) 0.5053(3) 0.5589(2) 0.0522(9) Uani 1 1 d .
H4 H 0.1097 0.5796 0.5498 0.063 Uiso 1 1 calc R
C5 C 0.0910(3) 0.4628(3) 0.6331(2) 0.0520(9) Uani 1 1 d .
H5 H 0.0700 0.5090 0.6738 0.062 Uiso 1 1 calc R
C6 C 0.0989(2) 0.3535(3) 0.6476(2) 0.0464(8) Uani 1 1 d .
H6 H 0.0838 0.3260 0.6978 0.056 Uiso 1 1 calc R
C11 C 0.1530(2) 0.1295(3) 0.67054(17) 0.0379(7) Uani 1 1 d .
H11 H 0.1664 0.1751 0.7134 0.045 Uiso 1 1 calc R
C12 C 0.1491(2) 0.0117(3) 0.68078(16) 0.0325(6) Uani 1 1 d .
C13 C 0.1601(2) -0.0392(3) 0.75376(18) 0.0426(8) Uani 1 1 d .
H13 H 0.1754 0.0005 0.7994 0.051 Uiso 1 1 calc R
C14 C 0.1480(2) -0.1506(3) 0.75721(18) 0.0470(8) Uani 1 1 d .
H14 H 0.1537 -0.1869 0.8056 0.056 Uiso 1 1 calc R
C15 C 0.1274(2) -0.2068(3) 0.68869(19) 0.0442(8) Uani 1 1 d .
H15 H 0.1191 -0.2817 0.6903 0.053 Uiso 1 1 calc R
C16 C 0.1192(2) -0.1516(3) 0.61692(18) 0.0380(7) Uani 1 1 d .
H16 H 0.1063 -0.1904 0.5705 0.046 Uiso 1 1 calc R
N1 N 0.13749(18) 0.1681(2) 0.60034(13) 0.0321(5) Uani 1 1 d .
N3 N 0.12928(17) -0.04400(19) 0.61310(14) 0.0306(5) Uani 1 1 d .
N11 N 0.0703(2) -0.0718(2) 0.45105(14) 0.0345(6) Uani 1 1 d .
N12 N 0.08632(19) -0.0749(2) 0.38044(15) 0.0373(6) Uani 1 1 d .
N13 N 0.0974(3) -0.0827(3) 0.31305(17) 0.0665(10) Uani 1 1 d .
O11 O 0.10871(17) 0.15223(19) 0.42968(12) 0.0462(6) Uani 1 1 d .
O12 O 0.28419(18) 0.1981(2) 0.44922(15) 0.0541(6) Uani 1 1 d .
O13 O 0.1775(2) 0.30382(19) 0.35918(12) 0.0563(7) Uani 1 1 d .
S1 S 0.18528(6) 0.23982(6) 0.43052(4) 0.0377(2) Uani 1 1 d .
Cu1 Cu 0.10543(3) 0.05147(3) 0.519197(19) 0.03124(15) Uani 1 1 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'
S S 0.1246 0.1234 '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'
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
C2 C1 C6 119.3(3) .
C2 C1 N1 120.2(3) .
C6 C1 N1 120.5(3) .
C1 C2 C3 119.7(3) .
C1 C2 S1 121.7(2) .
C3 C2 S1 118.6(2) .
C4 C3 C2 121.1(3) .
C4 C3 H3 119.4 .
C2 C3 H3 119.4 .
C3 C4 C5 119.1(3) .
C3 C4 H4 120.5 .
C5 C4 H4 120.5 .
C6 C5 C4 120.8(3) .
C6 C5 H5 119.6 .
C4 C5 H5 119.6 .
C5 C6 C1 119.9(3) .
C5 C6 H6 120.0 .
C1 C6 H6 120.0 .
N1 C11 C12 117.9(3) .
N1 C11 H11 121.0 .
C12 C11 H11 121.0 .
N3 C12 C13 122.3(3) .
N3 C12 C11 114.3(2) .
C13 C12 C11 123.3(3) .
C12 C13 C14 118.3(3) .
C12 C13 H13 120.8 .
C14 C13 H13 120.8 .
C15 C14 C13 119.4(3) .
C15 C14 H14 120.3 .
C13 C14 H14 120.3 .
C14 C15 C16 119.7(3) .
C14 C15 H15 120.1 .
C16 C15 H15 120.1 .
N3 C16 C15 121.4(3) .
N3 C16 H16 119.3 .
C15 C16 H16 119.3 .
C11 N1 C1 121.7(2) .
C11 N1 Cu1 112.8(2) .
C1 N1 Cu1 124.89(18) .
C16 N3 C12 118.9(2) .
C16 N3 Cu1 127.5(2) .
C12 N3 Cu1 113.30(19) .
N12 N11 Cu1 123.8(2) .
N12 N11 Cu1 112.3(2) 5_556
Cu1 N11 Cu1 91.78(9) 5_556
N13 N12 N11 175.9(4) .
S1 O11 Cu1 118.11(12) .
O13 S1 O12 116.15(15) .
O13 S1 O11 109.97(14) .
O12 S1 O11 111.64(15) .
O13 S1 C2 107.07(14) .
O12 S1 C2 106.86(14) .
O11 S1 C2 104.32(13) .
O11 Cu1 N11 92.85(9) .
O11 Cu1 N3 169.16(9) .
N11 Cu1 N3 92.39(10) .
O11 Cu1 N1 93.50(10) .
N11 Cu1 N1 173.47(10) .
N3 Cu1 N1 81.60(10) .
O11 Cu1 N11 96.62(9) 5_556
N11 Cu1 N11 88.22(10) 5_556
N3 Cu1 N11 93.02(9) 5_556
N1 Cu1 N11 89.55(9) 5_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.377(4) .
C1 C6 1.408(4) .
C1 N1 1.439(4) .
C2 C3 1.393(4) .
C2 S1 1.781(3) .
C3 C4 1.374(5) .
C3 H3 0.9300 .
C4 C5 1.384(5) .
C4 H4 0.9300 .
C5 C6 1.373(5) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C11 N1 1.287(4) .
C11 C12 1.463(4) .
C11 H11 0.9300 .
C12 N3 1.352(4) .
C12 C13 1.383(4) .
C13 C14 1.383(5) .
C13 H13 0.9300 .
C14 C15 1.369(5) .
C14 H14 0.9300 .
C15 C16 1.387(4) .
C15 H15 0.9300 .
C16 N3 1.334(4) .
C16 H16 0.9300 .
N1 Cu1 2.024(2) .
N3 Cu1 1.991(2) .
N11 N12 1.204(3) .
N11 Cu1 1.957(2) .
N11 Cu1 2.406(3) 5_556
N12 N13 1.144(4) .
O11 S1 1.485(2) .
O11 Cu1 1.949(2) .
O12 S1 1.449(3) .
O13 S1 1.437(2) .
Cu1 N11 2.406(3) 5_556
