#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:19:12 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179837 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/33/7013394.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_7013394
loop_
_publ_author_name
'Burke, Nichola J.'
'Burrows, Andrew D.'
'Donovan, Adele S.'
'Harrington, Ross W.'
'Mahon, Mary F.'
'Price, Caroline E.'
_publ_section_title
;
 Zinc dicarboxylate polymers and dimers: thiourea substitution as a
 tool in supramolecular synthesis
;
_journal_issue                   20
_journal_name_full               'Dalton Transactions'
_journal_page_first              3840
_journal_paper_doi               10.1039/b307420j
_journal_year                    2003
_chemical_formula_sum            'C12 H18 N4 O5 S2 Zn'
_chemical_formula_weight         427.79
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 94.1980(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3830(3)
_cell_length_b                   10.4260(3)
_cell_length_c                   16.5870(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     1790.78(8)
_computing_data_reduction
'Denzo and Scalepack (otwinowski & Minor, 1997'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       KappaCCD
_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  0.0923
_diffrn_reflns_av_sigmaI/netI    0.0664
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19197
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.80
_exptl_absorpt_coefficient_mu    1.634
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.0049(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         4086
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0392
_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
[1.00000+0.00000exp(0.00(sinθ/λ)²)]/
[σ²(Fo²)+0.0000+1.1923*P+(0.0328P)²+0.0000sinθ/λ]
where P = 0.00000Fo² + 1.00000Fc²
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0941
_reflns_number_gt                2873
_reflns_number_total             4086
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b307420j.txt
_cod_data_source_block           compound3_k01rwh6
_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 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' 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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7013394
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0621(3) 0.6598(3) 0.33701(18) 0.0244(7) Uani 1 1 d . . .
C2 C 0.0215(4) 0.8559(3) 0.4130(2) 0.0343(8) Uani 1 1 d . . .
H2A H -0.0099 0.9424 0.3995 0.041 Uiso 1 1 calc R . .
H2B H 0.1077 0.8613 0.4412 0.041 Uiso 1 1 calc R . .
H2C H -0.0377 0.8140 0.4482 0.041 Uiso 1 1 calc R . .
C3 C 0.5359(3) 0.4510(3) 0.34526(17) 0.0226(6) Uani 1 1 d . . .
C4 C 0.6815(4) 0.6097(4) 0.4152(3) 0.0491(11) Uani 1 1 d . . .
H4A H 0.7692 0.6083 0.4414 0.059 Uiso 1 1 calc R . .
H4B H 0.6204 0.6343 0.4549 0.059 Uiso 1 1 calc R . .
H4C H 0.6770 0.6720 0.3709 0.059 Uiso 1 1 calc R . .
C5 C 0.2125(3) 0.2604(3) 0.35364(17) 0.0206(6) Uani 1 1 d . . .
C6 C 0.2650(3) 0.1359(3) 0.38692(17) 0.0204(6) Uani 1 1 d . . .
C7 C 0.2656(3) 0.1126(3) 0.46981(17) 0.0198(6) Uani 1 1 d . . .
H7 H 0.2328 0.1758 0.5042 0.024 Uiso 1 1 calc R . .
C8 C 0.3136(3) -0.0021(3) 0.50263(17) 0.0203(6) Uani 1 1 d . . .
C9 C 0.3626(3) -0.0945(3) 0.45256(18) 0.0248(7) Uani 1 1 d . . .
H9 H 0.3941 -0.1735 0.4746 0.030 Uiso 1 1 calc R . .
C10 C 0.3654(3) -0.0710(3) 0.37028(19) 0.0291(7) Uani 1 1 d . . .
H10 H 0.4010 -0.1331 0.3363 0.035 Uiso 1 1 calc R . .
C11 C 0.3163(3) 0.0435(3) 0.33746(18) 0.0257(7) Uani 1 1 d . . .
H11 H 0.3176 0.0588 0.2811 0.031 Uiso 1 1 calc R . .
C12 C 0.3040(3) -0.0295(3) 0.59123(17) 0.0205(6) Uani 1 1 d . . .
N1 N 0.0955(3) 0.5971(3) 0.40391(16) 0.0279(6) Uani 1 1 d D . .
H1A H 0.107(4) 0.633(4) 0.4525(15) 0.050(12) Uiso 1 1 d D . .
H1B H 0.108(4) 0.5137(19) 0.399(2) 0.039(11) Uiso 1 1 d D . .
N2 N 0.0282(3) 0.7813(3) 0.33904(17) 0.0321(7) Uani 1 1 d D . .
H2 H 0.004(4) 0.815(4) 0.2933(17) 0.060(14) Uiso 1 1 d D . .
N3 N 0.5199(3) 0.3314(3) 0.31841(17) 0.0262(6) Uani 1 1 d D . .
H3A H 0.577(3) 0.273(3) 0.333(2) 0.042(11) Uiso 1 1 d D . .
H3B H 0.442(2) 0.306(3) 0.2990(18) 0.019(8) Uiso 1 1 d D . .
N4 N 0.6482(3) 0.4820(3) 0.38324(18) 0.0316(6) Uani 1 1 d D . .
H4 H 0.705(3) 0.421(3) 0.394(2) 0.050(12) Uiso 1 1 d D . .
O1 O 0.2458(2) 0.29153(19) 0.28320(12) 0.0230(5) Uani 1 1 d . . .
O2 O 0.1442(2) 0.3277(2) 0.39575(12) 0.0261(5) Uani 1 1 d . . .
O3 O 0.2879(2) 0.06756(19) 0.63658(12) 0.0244(5) Uani 1 1 d . . .
O4 O 0.3079(2) -0.14262(19) 0.61550(12) 0.0259(5) Uani 1 1 d . . .
O5 O 0.1229(3) 0.6759(2) 0.57438(14) 0.0298(5) Uani 1 1 d D . .
H5A H 0.043(2) 0.677(5) 0.588(3) 0.075(17) Uiso 1 1 d D . .
H5B H 0.161(4) 0.748(3) 0.585(2) 0.051(13) Uiso 1 1 d D . .
S1 S 0.05821(8) 0.58621(8) 0.24256(5) 0.0291(2) Uani 1 1 d . . .
S2 S 0.41840(8) 0.56750(7) 0.33061(5) 0.0276(2) Uani 1 1 d . . .
Zn1 Zn 0.25269(4) 0.47469(3) 0.24858(2) 0.02083(12) 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'
O O 0.0106 0.0060 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
N1 C1 N2 120.8(3) . . ?
N1 C1 S1 121.9(2) . . ?
N2 C1 S1 117.3(2) . . ?
N4 C3 N3 118.2(3) . . ?
N4 C3 S2 118.9(2) . . ?
N3 C3 S2 122.9(2) . . ?
O2 C5 O1 124.7(3) . . ?
O2 C5 C6 119.2(3) . . ?
O1 C5 C6 116.0(3) . . ?
C7 C6 C11 119.0(3) . . ?
C7 C6 C5 119.2(3) . . ?
C11 C6 C5 121.7(3) . . ?
C8 C7 C6 120.7(3) . . ?
C7 C8 C9 119.8(3) . . ?
C7 C8 C12 119.8(3) . . ?
C9 C8 C12 120.2(3) . . ?
C10 C9 C8 119.9(3) . . ?
C9 C10 C11 120.1(3) . . ?
C10 C11 C6 120.4(3) . . ?
O4 C12 O3 124.1(3) . . ?
O4 C12 C8 119.4(3) . . ?
O3 C12 C8 116.4(2) . . ?
C1 N2 C2 124.3(3) . . ?
C3 N4 C4 124.8(3) . . ?
C5 O1 Zn1 121.38(19) . . ?
C12 O3 Zn1 114.79(18) . 4_566 ?
C1 S1 Zn1 102.62(11) . . ?
C3 S2 Zn1 105.93(11) . . ?
O3 Zn1 O1 94.04(8) 4_565 . ?
O3 Zn1 S2 117.70(7) 4_565 . ?
O1 Zn1 S2 105.68(7) . . ?
O3 Zn1 S1 106.96(7) 4_565 . ?
O1 Zn1 S1 116.18(7) . . ?
S2 Zn1 S1 114.84(3) . . ?
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
C1 N1 1.312(4) . ?
C1 N2 1.317(4) . ?
C1 S1 1.742(3) . ?
C2 N2 1.459(4) . ?
C3 N4 1.324(4) . ?
C3 N3 1.330(4) . ?
C3 S2 1.726(3) . ?
C4 N4 1.465(4) . ?
C5 O2 1.247(4) . ?
C5 O1 1.284(3) . ?
C5 C6 1.498(4) . ?
C6 C7 1.396(4) . ?
C6 C11 1.396(4) . ?
C7 C8 1.391(4) . ?
C8 C9 1.392(4) . ?
C8 C12 1.507(4) . ?
C9 C10 1.389(4) . ?
C10 C11 1.393(4) . ?
C12 O4 1.246(3) . ?
C12 O3 1.279(3) . ?
O1 Zn1 1.997(2) . ?
O3 Zn1 1.969(2) 4_566 ?
S1 Zn1 2.3259(9) . ?
S2 Zn1 2.3249(9) . ?
Zn1 O3 1.969(2) 4_565 ?
