#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:20:05 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180422 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/91/7209135.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_7209135
loop_
_publ_author_name
'Lago, Ana Belén'
'Carballo, Rosa'
'Rodríguez-Hermida, Sabina'
'Vázquez-López, Ezequiel M.'
_publ_section_title
;
 Control over the preparation of two pH-dependent Cu(ii) supramolecular
 isomers based on 1,3,5-benzenetricarboxylic acid and the
 bis(4-pyridylthio)methane ligand
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              1563
_journal_paper_doi               10.1039/c2ce26652k
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C29 H20 Cu N2 O12 S2'
_chemical_formula_weight         716.16
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 117.73(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.540(5)
_cell_length_b                   5.1400(10)
_cell_length_c                   22.306(5)
_cell_measurement_temperature    173(2)
_cell_volume                     2591.9(12)
_computing_cell_refinement       HKL2000
_computing_data_collection       HKL2000
_computing_data_reduction        HKL2000
_computing_molecular_graphics    Mercury
_computing_publication_material  Mercury
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'ADSC Q210r CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.78900
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21431
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.41
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    1.435
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.601
_refine_diff_density_min         -1.698
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         2668
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0900P)²+5.1263P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1281
_reflns_number_gt                2590
_reflns_number_total             2668
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26652k.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_sg_symbol_H-M      c2/c
_cod_database_code               7209135
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
H7 H 0.1102(15) 0.706(7) 0.2387(18) 0.029(9) Uiso 1 1 d .
H9 H -0.0288(13) 0.242(6) 0.1205(16) 0.021(8) Uiso 1 1 d .
H6 H 0.0921(14) 0.966(6) 0.1470(17) 0.016(8) Uiso 1 1 d .
H8 H -0.0446(14) 0.513(5) 0.0341(18) 0.014(8) Uiso 1 1 d .
C2 C 0.24158(10) 1.4996(4) 0.14492(13) 0.0126(5) Uani 1 1 d .
C9 C 0.11969(10) 1.0330(4) 0.03407(12) 0.0127(4) Uani 1 1 d .
C8 C 0.33216(9) 1.1224(4) 0.08135(12) 0.0145(4) Uani 1 1 d .
C12 C 0.24810(9) 1.7107(4) 0.19317(12) 0.0132(4) Uani 1 1 d .
C4 C 0.28061(9) 1.2097(4) 0.09108(12) 0.0128(4) Uani 1 1 d .
C3 C 0.28804(9) 1.4226(4) 0.13298(11) 0.0128(4) Uani 1 1 d .
C5 C 0.22641(9) 1.0792(4) 0.05994(11) 0.0130(4) Uani 1 1 d .
C7 C 0.18691(9) 1.3727(4) 0.11274(12) 0.0130(4) Uani 1 1 d .
C6 C 0.17887(9) 1.1643(4) 0.06948(12) 0.0129(4) Uani 1 1 d .
Cu1 Cu 0.0000 1.0000 0.0000 0.01100(17) Uani 1 2 d S
O1 O 0.07884(6) 1.1429(3) 0.04366(8) 0.0139(3) Uani 1 1 d .
O2 O 0.11201(7) 0.8345(3) -0.00033(9) 0.0177(4) Uani 1 1 d .
O3 O 0.32115(7) 0.8984(3) 0.04825(10) 0.0202(4) Uani 1 1 d .
O5 O 0.29814(7) 1.8437(3) 0.21539(9) 0.0177(4) Uani 1 1 d .
O6 O 0.21114(7) 1.7554(3) 0.21205(9) 0.0154(4) Uani 1 1 d .
O4 O 0.37796(7) 1.2434(3) 0.10188(10) 0.0203(4) Uani 1 1 d .
N1 N 0.02130(8) 0.7598(3) 0.08073(10) 0.0124(4) Uani 1 1 d .
C11 C -0.01229(10) 0.5517(5) 0.07559(12) 0.0136(4) Uani 1 1 d .
C41 C -0.00206(9) 0.3901(4) 0.12949(12) 0.0146(4) Uani 1 1 d .
C21 C 0.06791(9) 0.8089(4) 0.14214(12) 0.0135(4) Uani 1 1 d .
C31 C 0.08060(9) 0.6591(4) 0.19833(12) 0.0143(4) Uani 1 1 d .
S1 S 0.06517(2) 0.26413(11) 0.26731(3) 0.01493(18) Uani 1 1 d .
C51 C 0.04521(9) 0.4449(5) 0.19310(12) 0.0135(4) Uani 1 1 d .
C61 C 0.0000 0.0755(6) 0.2500 0.0154(6) Uani 1 2 d S
H61A H 0.0088 -0.0361 0.2886 0.019 Uiso 0.50 1 calc PR
H61B H -0.0088 -0.0361 0.2114 0.019 Uiso 0.50 1 calc PR
H5 H 0.2206(12) 0.949(6) 0.0294(15) 0.008(6) Uiso 1 1 d .
H3 H 0.3218(13) 1.515(5) 0.1534(15) 0.008(7) Uiso 1 1 d .
H4 H 0.1546(14) 1.440(6) 0.1190(17) 0.021(7) Uiso 1 1 d .
H2 H 0.2971(18) 1.973(8) 0.243(2) 0.044(12) Uiso 1 1 d .
H1 H 0.350(2) 0.853(9) 0.040(2) 0.057(13) Uiso 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_1
_geom_angle_site_symmetry_3
C3 C2 C7 120.4(2) . .
C3 C2 C12 122.0(2) . .
C7 C2 C12 117.5(2) . .
O2 C9 O1 123.9(2) . .
O2 C9 C6 121.9(2) . .
O1 C9 C6 114.2(2) . .
O4 C8 O3 125.0(2) . .
O4 C8 C4 123.4(2) . .
O3 C8 C4 111.57(18) . .
O6 C12 O5 122.7(2) . .
O6 C12 C2 123.0(2) . .
O5 C12 C2 114.34(19) . .
C3 C4 C5 120.30(19) . .
C3 C4 C8 118.53(19) . .
C5 C4 C8 121.2(2) . .
C2 C3 C4 119.4(2) . .
C6 C5 C4 120.3(2) . .
C6 C7 C2 120.3(2) . .
C7 C6 C5 119.24(19) . .
C7 C6 C9 119.90(19) . .
C5 C6 C9 120.9(2) . .
O1 Cu1 O1 180.0 5_575 .
O1 Cu1 N1 90.12(7) 5_575 .
O1 Cu1 N1 89.88(7) . .
O1 Cu1 N1 89.88(7) 5_575 5_575
O1 Cu1 N1 90.12(7) . 5_575
N1 Cu1 N1 180.00(8) . 5_575
C9 O1 Cu1 119.01(15) . .
C11 N1 C21 117.4(2) . .
C11 N1 Cu1 120.68(16) . .
C21 N1 Cu1 121.86(15) . .
N1 C11 C41 123.4(2) . .
C11 C41 C51 119.1(2) . .
N1 C21 C31 122.7(2) . .
C21 C31 C51 119.8(2) . .
C51 S1 C61 104.38(9) . .
C31 C51 C41 117.6(2) . .
C31 C51 S1 116.53(18) . .
C41 C51 S1 125.82(18) . .
S1 C61 S1 115.05(18) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C2 C3 1.389(3) .
C2 C7 1.399(3) .
C2 C12 1.482(3) .
C9 O2 1.236(3) .
C9 O1 1.289(3) .
C9 C6 1.501(3) .
C8 O4 1.211(3) .
C8 O3 1.325(3) .
C8 C4 1.499(3) .
C12 O6 1.221(3) .
C12 O5 1.325(3) .
C4 C3 1.393(3) .
C4 C5 1.398(3) .
C5 C6 1.397(3) .
C7 C6 1.392(3) .
Cu1 O1 1.9282(15) 5_575
Cu1 O1 1.9282(16) .
Cu1 N1 2.037(2) .
Cu1 N1 2.037(2) 5_575
N1 C11 1.342(3) .
N1 C21 1.356(3) .
C11 C41 1.382(3) .
C41 C51 1.399(3) .
C21 C31 1.375(3) .
C31 C51 1.394(3) .
S1 C51 1.755(2) .
S1 C61 1.8060(19) .
C61 S1 1.8060(18) 2
