#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:39:03 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179540 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/09/4500972.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_4500972
loop_
_publ_author_name
'Lu, Huijie'
'Zhu, Yanyan'
'Chen, Nan'
'Gao, Yongchao'
'Guo, Xiaofang'
'Li, Gang'
'Tang, Mingsheng'
_publ_section_title
;
 Ligand-Directed Assembly of a Series of Complexes Bearing Thiourea-Based
 Carboxylates
;
_journal_issue                   12
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5241
_journal_paper_doi               10.1021/cg200564d
_journal_volume                  11
_journal_year                    2011
_chemical_formula_sum            'C34 H34 Cu3 N4 O10 S2'
_chemical_formula_weight         913.39
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           154
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   11.1990(7)
_cell_length_b                   11.1990(7)
_cell_length_c                   26.231(4)
_cell_measurement_reflns_used    2724
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.28
_cell_measurement_theta_min      2.33
_cell_volume                     2849.1(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6901
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         2.33
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.834
_exptl_absorpt_correction_T_max  0.6183
_exptl_absorpt_correction_T_min  0.5348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1395
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.024(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0280
_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)+(0.0006P)²+0.4383P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0414
_refine_ls_wR_factor_ref         0.0426
_reflns_number_gt                2780
_reflns_number_total             3285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg200564d_si_006.cif
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P3(2)21
_cod_database_code               4500972
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'y, x, -z'
'x-y, -y, -z+1/3'
'-x, -x+y, -z+2/3'
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
Cu1 Cu 0.43395(5) 0.43395(5) 0.0000 0.03919(16) Uani 1 2 d S
Cu2 Cu 0.48734(4) 0.85360(4) 0.085715(14) 0.03852(11) Uani 1 1 d .
N1 N 0.3302(3) 0.6721(3) 0.07130(9) 0.0338(7) Uani 1 1 d .
N2 N 0.4579(3) 0.6188(3) 0.01199(9) 0.0344(7) Uani 1 1 d .
O1 O 0.3098(2) 0.7582(2) 0.22533(7) 0.0587(8) Uani 1 1 d .
O2 O 0.4423(2) 0.8336(2) 0.15730(7) 0.0452(7) Uani 1 1 d .
O3 O 0.5725(2) 0.8556(2) 0.02227(7) 0.0425(6) Uani 1 1 d .
O4 O 0.4057(3) 0.9933(2) 0.06120(8) 0.0609(8) Uani 1 1 d .
H4D H 0.4571 1.0701 0.0758 0.091 Uiso 1 1 d R
O5 O 0.6613(2) 1.0258(2) 0.10607(8) 0.0472(7) Uani 1 1 d .
H5D H 0.6443 1.0668 0.1298 0.071 Uiso 1 1 d R
S3 S 0.24774(9) 0.40383(9) 0.04515(3) 0.0433(2) Uani 1 1 d .
C1 C 0.2023(3) 0.6302(3) 0.09646(10) 0.0314(8) Uani 1 1 d .
C2 C 0.1988(3) 0.6759(3) 0.14613(10) 0.0347(8) Uani 1 1 d .
C3 C 0.0718(4) 0.6421(3) 0.16731(11) 0.0434(9) Uani 1 1 d .
H3 H 0.0691 0.6738 0.1998 0.052 Uiso 1 1 calc R
C4 C -0.0489(4) 0.5635(4) 0.14164(12) 0.0498(10) Uani 1 1 d .
H4 H -0.1328 0.5410 0.1567 0.060 Uiso 1 1 calc R
C5 C -0.0454(4) 0.5177(3) 0.09281(12) 0.0458(9) Uani 1 1 d .
H5 H -0.1272 0.4635 0.0752 0.055 Uiso 1 1 calc R
C6 C 0.0782(4) 0.5519(3) 0.07035(11) 0.0394(9) Uani 1 1 d .
H6 H 0.0794 0.5227 0.0373 0.047 Uiso 1 1 calc R
C7 C 0.3485(3) 0.5829(3) 0.04451(10) 0.0314(8) Uani 1 1 d .
C8 C 0.5550(4) 0.7498(4) -0.00047(11) 0.0346(8) Uani 1 1 d .
C9 C 0.6439(3) 0.7668(3) -0.04490(11) 0.0326(8) Uani 1 1 d .
C10 C 0.6010(3) 0.6742(3) -0.08460(11) 0.0402(9) Uani 1 1 d .
H10 H 0.5133 0.5968 -0.0838 0.048 Uiso 1 1 calc R
C11 C 0.6872(4) 0.6951(4) -0.12581(12) 0.0572(11) Uani 1 1 d .
H11 H 0.6576 0.6311 -0.1522 0.069 Uiso 1 1 calc R
C12 C 0.8153(4) 0.8092(4) -0.12754(14) 0.0649(12) Uani 1 1 d .
H12 H 0.8731 0.8225 -0.1550 0.078 Uiso 1 1 calc R
C13 C 0.8591(4) 0.9042(4) -0.08910(14) 0.0610(12) Uani 1 1 d .
H13 H 0.9460 0.9825 -0.0907 0.073 Uiso 1 1 calc R
C14 C 0.7734(4) 0.8837(4) -0.04762(12) 0.0458(10) Uani 1 1 d .
H14 H 0.8031 0.9487 -0.0216 0.055 Uiso 1 1 calc R
C15 C 0.3238(4) 0.7598(4) 0.17895(12) 0.0412(9) Uani 1 1 d .
C16 C 0.2707(4) 0.9651(5) 0.05915(18) 0.1024(17) Uani 1 1 d .
H16A H 0.2151 0.8789 0.0420 0.154 Uiso 1 1 calc R
H16B H 0.2667 1.0373 0.0409 0.154 Uiso 1 1 calc R
H16C H 0.2365 0.9594 0.0932 0.154 Uiso 1 1 calc R
C17 C 0.7636(4) 1.1215(4) 0.07209(12) 0.0722(12) Uani 1 1 d .
H17A H 0.8096 1.0789 0.0558 0.108 Uiso 1 1 calc R
H17B H 0.8295 1.2010 0.0908 0.108 Uiso 1 1 calc R
H17C H 0.7206 1.1492 0.0467 0.108 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'
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
N2 Cu1 N2 107.41(16) 4 .
N2 Cu1 S3 72.91(8) 4 4
N2 Cu1 S3 157.68(7) . 4
N2 Cu1 S3 157.68(7) 4 .
N2 Cu1 S3 72.91(8) . .
S3 Cu1 S3 115.56(5) 4 .
O3 Cu2 O2 161.57(10) . .
O3 Cu2 N1 91.62(10) . .
O2 Cu2 N1 91.18(10) . .
O3 Cu2 O5 88.93(9) . .
O2 Cu2 O5 85.67(8) . .
N1 Cu2 O5 171.47(11) . .
O3 Cu2 O4 96.65(9) . .
O2 Cu2 O4 100.63(9) . .
N1 Cu2 O4 101.53(10) . .
O5 Cu2 O4 86.85(9) . .
C7 N1 C1 120.6(3) . .
C7 N1 Cu2 119.5(2) . .
C1 N1 Cu2 119.17(19) . .
C8 N2 C7 125.4(3) . .
C8 N2 Cu1 135.2(2) . .
C7 N2 Cu1 99.1(2) . .
C15 O2 Cu2 128.9(2) . .
C8 O3 Cu2 124.2(2) . .
C16 O4 Cu2 128.8(2) . .
C16 O4 H4D 111.0 . .
Cu2 O4 H4D 105.6 . .
C17 O5 Cu2 125.78(19) . .
C17 O5 H5D 111.4 . .
Cu2 O5 H5D 109.9 . .
C7 S3 Cu1 78.80(11) . .
C6 C1 C2 118.8(3) . .
C6 C1 N1 120.0(3) . .
C2 C1 N1 121.0(3) . .
C3 C2 C1 118.8(3) . .
C3 C2 C15 116.5(3) . .
C1 C2 C15 124.7(3) . .
C4 C3 C2 121.8(3) . .
C4 C3 H3 119.1 . .
C2 C3 H3 119.1 . .
C3 C4 C5 119.4(3) . .
C3 C4 H4 120.3 . .
C5 C4 H4 120.3 . .
C6 C5 C4 120.3(3) . .
C6 C5 H5 119.8 . .
C4 C5 H5 119.8 . .
C5 C6 C1 120.9(3) . .
C5 C6 H6 119.6 . .
C1 C6 H6 119.6 . .
N1 C7 N2 124.1(3) . .
N1 C7 S3 127.6(2) . .
N2 C7 S3 108.2(2) . .
O3 C8 N2 124.7(3) . .
O3 C8 C9 118.4(3) . .
N2 C8 C9 116.8(3) . .
C10 C9 C14 118.6(3) . .
C10 C9 C8 122.7(3) . .
C14 C9 C8 118.7(3) . .
C9 C10 C11 120.7(3) . .
C9 C10 H10 119.6 . .
C11 C10 H10 119.6 . .
C12 C11 C10 120.0(3) . .
C12 C11 H11 120.0 . .
C10 C11 H11 120.0 . .
C11 C12 C13 120.4(4) . .
C11 C12 H12 119.8 . .
C13 C12 H12 119.8 . .
C12 C13 C14 119.9(4) . .
C12 C13 H13 120.0 . .
C14 C13 H13 120.0 . .
C9 C14 C13 120.4(3) . .
C9 C14 H14 119.8 . .
C13 C14 H14 119.8 . .
O1 C15 O2 121.9(3) . .
O1 C15 C2 119.1(3) . .
O2 C15 C2 119.0(3) . .
O4 C16 H16A 109.5 . .
O4 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
O4 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
O5 C17 H17A 109.5 . .
O5 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
O5 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N2 1.975(3) 4
Cu1 N2 1.975(3) .
Cu1 S3 2.2720(9) 4
Cu1 S3 2.2720(9) .
Cu2 O3 1.9126(19) .
Cu2 O2 1.928(2) .
Cu2 N1 1.948(3) .
Cu2 O5 2.011(2) .
Cu2 O4 2.264(2) .
N1 C7 1.318(3) .
N1 C1 1.427(4) .
N2 C8 1.359(4) .
N2 C7 1.378(3) .
O1 C15 1.226(3) .
O2 C15 1.293(4) .
O3 C8 1.251(4) .
O4 C16 1.382(4) .
O4 H4D 0.8501 .
O5 C17 1.423(3) .
O5 H5D 0.8500 .
S3 C7 1.741(3) .
C1 C6 1.397(4) .
C1 C2 1.407(4) .
C2 C3 1.391(4) .
C2 C15 1.507(4) .
C3 C4 1.366(4) .
C3 H3 0.9300 .
C4 C5 1.388(4) .
C4 H4 0.9300 .
C5 C6 1.371(4) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C8 C9 1.482(4) .
C9 C10 1.376(4) .
C9 C14 1.387(4) .
C10 C11 1.389(4) .
C10 H10 0.9300 .
C11 C12 1.364(5) .
C11 H11 0.9300 .
C12 C13 1.366(5) .
C12 H12 0.9300 .
C13 C14 1.392(4) .
C13 H13 0.9300 .
C14 H14 0.9300 .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5D O2 0.85 1.82 2.668(3) 174.5 5_675
O4 H4D O1 0.85 1.87 2.716(3) 173.1 5_675
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
O3 Cu2 N1 C7 32.4(2) .
O2 Cu2 N1 C7 -129.4(2) .
O5 Cu2 N1 C7 -61.2(7) .
O4 Cu2 N1 C7 129.5(2) .
O3 Cu2 N1 C1 -157.3(2) .
O2 Cu2 N1 C1 40.9(2) .
O5 Cu2 N1 C1 109.1(7) .
O4 Cu2 N1 C1 -60.2(2) .
N2 Cu1 N2 C8 23.7(2) 4
S3 Cu1 N2 C8 -63.6(4) 4
S3 Cu1 N2 C8 -179.7(3) .
N2 Cu1 N2 C7 -149.3(2) 4
S3 Cu1 N2 C7 123.4(2) 4
S3 Cu1 N2 C7 7.36(15) .
O3 Cu2 O2 C15 -125.0(3) .
N1 Cu2 O2 C15 -26.3(3) .
O5 Cu2 O2 C15 161.6(3) .
O4 Cu2 O2 C15 75.7(3) .
O2 Cu2 O3 C8 70.5(4) .
N1 Cu2 O3 C8 -28.2(3) .
O5 Cu2 O3 C8 143.3(3) .
O4 Cu2 O3 C8 -130.0(3) .
O3 Cu2 O4 C16 119.2(3) .
O2 Cu2 O4 C16 -67.2(3) .
N1 Cu2 O4 C16 26.2(3) .
O5 Cu2 O4 C16 -152.2(3) .
O3 Cu2 O5 C17 22.1(3) .
O2 Cu2 O5 C17 -175.5(3) .
N1 Cu2 O5 C17 115.9(7) .
O4 Cu2 O5 C17 -74.6(3) .
N2 Cu1 S3 C7 88.5(2) 4
N2 Cu1 S3 C7 -5.85(12) .
S3 Cu1 S3 C7 -163.64(10) 4
C7 N1 C1 C6 -47.0(4) .
Cu2 N1 C1 C6 142.8(2) .
C7 N1 C1 C2 138.2(3) .
Cu2 N1 C1 C2 -32.0(4) .
C6 C1 C2 C3 -0.4(4) .
N1 C1 C2 C3 174.5(3) .
C6 C1 C2 C15 179.4(3) .
N1 C1 C2 C15 -5.7(5) .
C1 C2 C3 C4 1.5(5) .
C15 C2 C3 C4 -178.4(3) .
C2 C3 C4 C5 -1.0(5) .
C3 C4 C5 C6 -0.6(5) .
C4 C5 C6 C1 1.7(5) .
C2 C1 C6 C5 -1.2(5) .
N1 C1 C6 C5 -176.1(3) .
C1 N1 C7 N2 168.0(3) .
Cu2 N1 C7 N2 -21.8(4) .
C1 N1 C7 S3 -14.8(4) .
Cu2 N1 C7 S3 155.32(18) .
C8 N2 C7 N1 -6.0(5) .
Cu1 N2 C7 N1 167.9(3) .
C8 N2 C7 S3 176.4(2) .
Cu1 N2 C7 S3 -9.7(2) .
Cu1 S3 C7 N1 -169.1(3) .
Cu1 S3 C7 N2 8.46(18) .
Cu2 O3 C8 N2 10.8(4) .
Cu2 O3 C8 C9 -170.45(19) .
C7 N2 C8 O3 12.9(5) .
Cu1 N2 C8 O3 -158.6(2) .
C7 N2 C8 C9 -165.8(3) .
Cu1 N2 C8 C9 22.7(4) .
O3 C8 C9 C10 -151.1(3) .
N2 C8 C9 C10 27.7(4) .
O3 C8 C9 C14 26.2(4) .
N2 C8 C9 C14 -155.0(3) .
C14 C9 C10 C11 2.0(5) .
C8 C9 C10 C11 179.3(3) .
C9 C10 C11 C12 -0.8(6) .
C10 C11 C12 C13 -0.6(6) .
C11 C12 C13 C14 0.8(6) .
C10 C9 C14 C13 -1.7(5) .
C8 C9 C14 C13 -179.1(3) .
C12 C13 C14 C9 0.3(6) .
Cu2 O2 C15 O1 -179.0(3) .
Cu2 O2 C15 C2 -0.5(5) .
C3 C2 C15 O1 22.4(5) .
C1 C2 C15 O1 -157.5(3) .
C3 C2 C15 O2 -156.2(3) .
C1 C2 C15 O2 24.0(5) .
