#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/22/7032224.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_7032224
loop_
_publ_author_name
'Selvakumaran, Nagamani'
'Bhuvanesh, Nattamai S. P.'
'Karvembu, Ramasamy'
_publ_section_title
;
 Self-assembled Cu(ii) and Ni(ii) metallamacrocycles formed from
 3,3,3',3'-tetrabenzyl-1,1'-aroylbis(thiourea) ligands: DNA and protein
 binding studies, and cytotoxicity of trinuclear complexes.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16395
_journal_page_last               16410
_journal_paper_doi               10.1039/c4dt01859a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C44 H49 N6 O4.5 S2'
_chemical_formula_weight         798.01
_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                81.433(5)
_cell_angle_beta                 68.491(5)
_cell_angle_gamma                84.688(5)
_cell_formula_units_Z            1
_cell_length_a                   9.660(4)
_cell_length_b                   10.747(5)
_cell_length_c                   10.981(5)
_cell_measurement_reflns_used    6824
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.41
_cell_measurement_theta_min      2.27
_cell_volume                     1047.9(8)
_computing_cell_refinement
; 
  APEX-II(BRUKER-NONIUS, 2003) 
;
_computing_data_collection       'APEX-II (BRUKER-NONIUS, 2003)'
_computing_data_reduction        APEX-II
_computing_molecular_graphics    Olex2
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'APEX II'
_diffrn_measurement_method       '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  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12107
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  0.9653
_exptl_absorpt_correction_T_min  0.9163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             423
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0394
_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)+(0.0519P)²+0.4046P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1089
_reflns_number_gt                4150
_reflns_number_total             4726
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01859a2.cif
_cod_data_source_block           tp3u
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7032224--7032227.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C44 H49 N6 O4.50 S2'
_cod_database_code               7032224
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
S1 S 0.68415(4) 0.93596(3) 0.79705(4) 0.03407(12) Uani 1 1 d . . .
O1 O 0.76883(10) 0.55836(9) 0.83517(8) 0.0246(2) Uani 1 1 d . . .
N1 N 0.51063(11) 0.73729(10) 0.89674(10) 0.0195(2) Uani 1 1 d . . .
N2 N 0.71095(11) 0.71945(10) 0.69986(10) 0.0199(2) Uani 1 1 d . . .
H2 H 0.7397 0.7633 0.6188 0.030 Uiso 1 1 d R . .
C1 C 0.43971(13) 0.62726(11) 0.88152(12) 0.0218(3) Uani 1 1 d . . .
H1A H 0.4055 0.5712 0.9661 0.026 Uiso 1 1 calc R . .
H1B H 0.5129 0.5789 0.8142 0.026 Uiso 1 1 calc R . .
C2 C 0.30841(14) 0.67172(12) 0.83996(13) 0.0225(3) Uani 1 1 d . . .
C3 C 0.33072(16) 0.74430(14) 0.71847(14) 0.0293(3) Uani 1 1 d . . .
H3 H 0.4288 0.7637 0.6603 0.035 Uiso 1 1 calc R . .
C4 C 0.20961(19) 0.78817(15) 0.68248(16) 0.0367(3) Uani 1 1 d . . .
H4 H 0.2249 0.8385 0.6002 0.044 Uiso 1 1 calc R . .
C5 C 0.06676(18) 0.75876(15) 0.76614(18) 0.0399(4) Uani 1 1 d . . .
H5 H -0.0159 0.7892 0.7414 0.048 Uiso 1 1 calc R . .
C6 C 0.04425(17) 0.68550(16) 0.88519(18) 0.0408(4) Uani 1 1 d . . .
H6 H -0.0539 0.6644 0.9418 0.049 Uiso 1 1 calc R . .
C7 C 0.16445(15) 0.64207(14) 0.92322(15) 0.0306(3) Uani 1 1 d . . .
H7 H 0.1482 0.5922 1.0059 0.037 Uiso 1 1 calc R . .
C8 C 0.42811(14) 0.79405(13) 1.01866(12) 0.0248(3) Uani 1 1 d . . .
H8A H 0.3199 0.7897 1.0387 0.030 Uiso 1 1 calc R . .
H8B H 0.4516 0.8840 1.0045 0.030 Uiso 1 1 calc R . .
C9 C 0.46540(15) 0.72911(12) 1.13507(12) 0.0245(3) Uani 1 1 d . . .
C10 C 0.35528(19) 0.71204(15) 1.25953(14) 0.0377(4) Uani 1 1 d . . .
H10 H 0.2547 0.7365 1.2706 0.045 Uiso 1 1 calc R . .
C11 C 0.3921(2) 0.65900(18) 1.36849(15) 0.0510(5) Uani 1 1 d . . .
H11 H 0.3163 0.6475 1.4534 0.061 Uiso 1 1 calc R . .
C12 C 0.5371(2) 0.62335(16) 1.35363(17) 0.0485(5) Uani 1 1 d . . .
H12 H 0.5616 0.5889 1.4283 0.058 Uiso 1 1 calc R . .
C13 C 0.6466(2) 0.63760(15) 1.23064(17) 0.0418(4) Uani 1 1 d . . .
H13 H 0.7466 0.6118 1.2201 0.050 Uiso 1 1 calc R . .
C14 C 0.61103(17) 0.68981(14) 1.12158(14) 0.0313(3) Uani 1 1 d . . .
H14 H 0.6872 0.6988 1.0367 0.038 Uiso 1 1 calc R . .
C15 C 0.62779(13) 0.79194(11) 0.80348(12) 0.0200(2) Uani 1 1 d . . .
C16 C 0.78714(13) 0.60985(11) 0.72384(11) 0.0185(2) Uani 1 1 d . . .
C17 C 0.89640(13) 0.55605(11) 0.60512(11) 0.0186(2) Uani 1 1 d . . .
C18 C 0.88969(14) 0.58428(12) 0.47939(12) 0.0231(3) Uani 1 1 d . . .
H18 H 0.8147 0.6417 0.4651 0.028 Uiso 1 1 calc R . .
C19 C 0.99318(14) 0.52818(12) 0.37497(12) 0.0236(3) Uani 1 1 d . . .
H19 H 0.9885 0.5475 0.2892 0.028 Uiso 1 1 calc R . .
O1D O 0.68682(17) 0.85693(13) 0.46789(12) 0.0554(4) Uani 1 1 d . . .
N3D N 0.79360(15) 0.91740(12) 0.24750(13) 0.0354(3) Uani 1 1 d . . .
C2D C 0.6792(2) 0.90100(14) 0.36130(16) 0.0393(4) Uani 1 1 d . . .
H2D H 0.5830 0.9258 0.3594 0.047 Uiso 1 1 calc R . .
C4D C 0.7704(2) 0.97188(17) 0.12708(17) 0.0486(4) Uani 1 1 d . . .
H4DA H 0.6634 0.9860 0.1450 0.073 Uiso 1 1 calc R . .
H4DB H 0.8124 0.9141 0.0602 0.073 Uiso 1 1 calc R . .
H4DC H 0.8197 1.0523 0.0947 0.073 Uiso 1 1 calc R . .
C5D C 0.9453(2) 0.8868(2) 0.2391(2) 0.0574(5) Uani 1 1 d . . .
H5DA H 0.9475 0.8620 0.3280 0.086 Uiso 1 1 calc R . .
H5DB H 1.0057 0.9605 0.1974 0.086 Uiso 1 1 calc R . .
H5DC H 0.9856 0.8170 0.1863 0.086 Uiso 1 1 calc R . .
O2 O 1.0177(10) 0.9321(8) 0.4991(8) 0.098(3) Uani 0.25 1 d P A -1
H2A H 1.0405 0.9979 0.5106 0.147 Uiso 0.25 1 d PR A -1
H2B H 0.9424 0.9148 0.4920 0.147 Uiso 0.25 1 d PR A -1
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'
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
C15 N1 C8 121.21(11) . .
C15 N1 C1 124.22(10) . .
C8 N1 C1 114.07(10) . .
C16 N2 C15 121.04(10) . .
C16 N2 H2 120.2 . .
C15 N2 H2 114.4 . .
N1 C1 C2 109.55(10) . .
N1 C1 H1A 109.8 . .
C2 C1 H1A 109.8 . .
N1 C1 H1B 109.8 . .
C2 C1 H1B 109.8 . .
H1A C1 H1B 108.2 . .
C7 C2 C3 119.42(12) . .
C7 C2 C1 120.36(12) . .
C3 C2 C1 120.21(12) . .
C4 C3 C2 120.03(14) . .
C4 C3 H3 120.0 . .
C2 C3 H3 120.0 . .
C5 C4 C3 120.17(15) . .
C5 C4 H4 119.9 . .
C3 C4 H4 119.9 . .
C6 C5 C4 120.06(14) . .
C6 C5 H5 120.0 . .
C4 C5 H5 120.0 . .
C5 C6 C7 120.40(14) . .
C5 C6 H6 119.8 . .
C7 C6 H6 119.8 . .
C2 C7 C6 119.91(14) . .
C2 C7 H7 120.0 . .
C6 C7 H7 120.0 . .
N1 C8 C9 112.50(11) . .
N1 C8 H8A 109.1 . .
C9 C8 H8A 109.1 . .
N1 C8 H8B 109.1 . .
C9 C8 H8B 109.1 . .
H8A C8 H8B 107.8 . .
C10 C9 C14 118.54(14) . .
C10 C9 C8 120.38(13) . .
C14 C9 C8 121.03(12) . .
C9 C10 C11 120.14(16) . .
C9 C10 H10 119.9 . .
C11 C10 H10 119.9 . .
C12 C11 C10 120.45(16) . .
C12 C11 H11 119.8 . .
C10 C11 H11 119.8 . .
C11 C12 C13 119.96(15) . .
C11 C12 H12 120.0 . .
C13 C12 H12 120.0 . .
C12 C13 C14 120.01(17) . .
C12 C13 H13 120.0 . .
C14 C13 H13 120.0 . .
C13 C14 C9 120.87(15) . .
C13 C14 H14 119.6 . .
C9 C14 H14 119.6 . .
N1 C15 N2 115.83(11) . .
N1 C15 S1 126.23(9) . .
N2 C15 S1 117.95(9) . .
O1 C16 N2 122.53(11) . .
O1 C16 C17 121.08(11) . .
N2 C16 C17 116.39(10) . .
C19 C17 C18 119.66(11) 2_766 .
C19 C17 C16 117.06(11) 2_766 .
C18 C17 C16 123.26(11) . .
C19 C18 C17 119.74(11) . .
C19 C18 H18 120.1 . .
C17 C18 H18 120.1 . .
C18 C19 C17 120.60(12) . 2_766
C18 C19 H19 119.7 . .
C17 C19 H19 119.7 2_766 .
C2D N3D C5D 121.92(15) . .
C2D N3D C4D 120.77(15) . .
C5D N3D C4D 117.26(15) . .
O1D C2D N3D 125.91(17) . .
O1D C2D H2D 117.0 . .
N3D C2D H2D 117.0 . .
N3D C4D H4DA 109.5 . .
N3D C4D H4DB 109.5 . .
H4DA C4D H4DB 109.5 . .
N3D C4D H4DC 109.5 . .
H4DA C4D H4DC 109.5 . .
H4DB C4D H4DC 109.5 . .
N3D C5D H5DA 109.5 . .
N3D C5D H5DB 109.5 . .
H5DA C5D H5DB 109.5 . .
N3D C5D H5DC 109.5 . .
H5DA C5D H5DC 109.5 . .
H5DB C5D H5DC 109.5 . .
H2A O2 H2B 129.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 C15 1.6710(14) .
O1 C16 1.2207(15) .
N1 C15 1.3299(17) .
N1 C8 1.4734(15) .
N1 C1 1.4793(16) .
N2 C16 1.3740(16) .
N2 C15 1.4230(15) .
N2 H2 0.9000 .
C1 C2 1.5142(18) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 C7 1.3908(19) .
C2 C3 1.3946(19) .
C3 C4 1.389(2) .
C3 H3 0.9500 .
C4 C5 1.383(2) .
C4 H4 0.9500 .
C5 C6 1.376(3) .
C5 H5 0.9500 .
C6 C7 1.392(2) .
C6 H6 0.9500 .
C7 H7 0.9500 .
C8 C9 1.5087(19) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 C10 1.389(2) .
C9 C14 1.391(2) .
C10 C11 1.398(2) .
C10 H10 0.9500 .
C11 C12 1.374(3) .
C11 H11 0.9500 .
C12 C13 1.374(3) .
C12 H12 0.9500 .
C13 C14 1.390(2) .
C13 H13 0.9500 .
C14 H14 0.9500 .
C16 C17 1.5002(16) .
C17 C19 1.3922(17) 2_766
C17 C18 1.3927(18) .
C18 C19 1.3898(17) .
C18 H18 0.9500 .
C19 C17 1.3922(17) 2_766
C19 H19 0.9500 .
O1D C2D 1.221(2) .
N3D C2D 1.331(2) .
N3D C5D 1.444(2) .
N3D C4D 1.451(2) .
C2D H2D 0.9500 .
C4D H4DA 0.9800 .
C4D H4DB 0.9800 .
C4D H4DC 0.9800 .
C5D H5DA 0.9800 .
C5D H5DB 0.9800 .
C5D H5DC 0.9800 .
O2 H2A 0.8000 .
O2 H2B 0.8000 .
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
_geom_torsion_site_symmetry_4
C15 N1 C1 C2 -95.61(13) . .
C8 N1 C1 C2 76.33(13) . .
N1 C1 C2 C7 -114.88(13) . .
N1 C1 C2 C3 64.25(15) . .
C7 C2 C3 C4 1.1(2) . .
C1 C2 C3 C4 -178.00(12) . .
C2 C3 C4 C5 -0.8(2) . .
C3 C4 C5 C6 -0.2(2) . .
C4 C5 C6 C7 1.0(2) . .
C3 C2 C7 C6 -0.4(2) . .
C1 C2 C7 C6 178.73(13) . .
C5 C6 C7 C2 -0.6(2) . .
C15 N1 C8 C9 -102.88(14) . .
C1 N1 C8 C9 84.90(13) . .
N1 C8 C9 C10 -142.25(13) . .
N1 C8 C9 C14 40.45(17) . .
C14 C9 C10 C11 1.4(2) . .
C8 C9 C10 C11 -175.96(14) . .
C9 C10 C11 C12 0.0(2) . .
C10 C11 C12 C13 -1.2(3) . .
C11 C12 C13 C14 1.0(2) . .
C12 C13 C14 C9 0.5(2) . .
C10 C9 C14 C13 -1.7(2) . .
C8 C9 C14 C13 175.68(13) . .
C8 N1 C15 N2 171.14(10) . .
C1 N1 C15 N2 -17.46(16) . .
C8 N1 C15 S1 -9.27(17) . .
C1 N1 C15 S1 162.13(9) . .
C16 N2 C15 N1 -65.40(15) . .
C16 N2 C15 S1 114.97(12) . .
C15 N2 C16 O1 12.26(18) . .
C15 N2 C16 C17 -167.30(11) . .
O1 C16 C17 C19 -19.74(18) . 2_766
N2 C16 C17 C19 159.82(11) . 2_766
O1 C16 C17 C18 158.80(12) . .
N2 C16 C17 C18 -21.64(17) . .
C19 C17 C18 C19 0.0(2) 2_766 .
C16 C17 C18 C19 -178.50(12) . .
C17 C18 C19 C17 0.0(2) . 2_766
C5D N3D C2D O1D -2.0(3) . .
C4D N3D C2D O1D -179.51(16) . .
