#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/33/7013397.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_7013397
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            'C14 H21 N4 O4.5 S2 Zn'
_chemical_formula_weight         446.84
_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                98.2960(10)
_cell_angle_beta                 106.8340(10)
_cell_angle_gamma                100.0610(10)
_cell_formula_units_Z            2
_cell_length_a                   8.55500(10)
_cell_length_b                   9.6180(2)
_cell_length_c                   13.0360(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     989.03(3)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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     0.71070
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20647
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.60
_exptl_absorpt_coefficient_mu    1.481
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             462
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.042(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4510
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0303
_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
[1.00000+0.00000exp(0.00(sinθ/λ)²)]/
[σ²(Fo²)+0.0000+0.4018*P+(0.0437P)²+0.0000sinθ/λ]
where P = 0.00000Fo² + 1.00000Fc²
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0854
_reflns_number_gt                4116
_reflns_number_total             4510
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b307420j.txt
_cod_data_source_block           compound6_h01rwh1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 'Multi-Scan' changed
to 'multi-scan' 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      P-1
_cod_original_formula_sum        'C14 H21 N4 O4.50 S2 Zn'
_cod_database_code               7013397
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
Zn1 Zn 0.83398(2) 0.75647(2) 0.241636(16) 0.03241(10) Uani 1 1 d . . .
S1 S 0.69901(6) 0.92073(5) 0.15435(4) 0.03966(13) Uani 1 1 d . . .
S2 S 0.80369(8) 0.55496(6) 0.11038(5) 0.04838(15) Uani 1 1 d . . .
O1 O 0.71089(16) 0.69871(14) 0.34066(11) 0.0355(3) Uani 1 1 d . . .
O2 O 0.7771(2) 0.48586(17) 0.33108(15) 0.0562(4) Uani 1 1 d . . .
O3 O 1.05535(16) 0.85392(16) 0.34913(12) 0.0422(3) Uani 1 1 d . . .
O4 O 1.1847(2) 0.8868(2) 0.22586(13) 0.0609(5) Uani 1 1 d . . .
O5 O 0.8593(4) 0.4871(4) -0.3015(3) 0.0558(8) Uani 0.50 1 d P . .
N1 N 0.6984(2) 1.19275(19) 0.22565(15) 0.0452(4) Uani 1 1 d D . .
H1 H 0.738(3) 1.276(2) 0.2706(18) 0.048(7) Uiso 1 1 d D . .
N2 N 0.9164(2) 1.1113(2) 0.32654(15) 0.0451(4) Uani 1 1 d D . .
H2 H 0.965(3) 1.037(2) 0.334(2) 0.052(7) Uiso 1 1 d D . .
N3 N 0.7806(3) 0.5323(2) -0.09788(16) 0.0551(5) Uani 1 1 d D . .
H3 H 0.817(3) 0.557(3) -0.1482(19) 0.060(8) Uiso 1 1 d D . .
N4 N 0.9617(3) 0.7367(2) 0.01766(16) 0.0502(5) Uani 1 1 d D . .
H4 H 1.013(3) 0.780(3) 0.0843(15) 0.050(7) Uiso 1 1 d D . .
C1 C 0.7775(2) 1.0873(2) 0.24206(15) 0.0343(4) Uani 1 1 d . . .
C2 C 0.5426(4) 1.1787(3) 0.1387(3) 0.0788(9) Uani 1 1 d . . .
H2A H 0.5547 1.1424 0.0696 0.118 Uiso 1 1 calc R . .
H2B H 0.5155 1.2714 0.1385 0.118 Uiso 1 1 calc R . .
H2C H 0.4544 1.1130 0.1506 0.118 Uiso 1 1 calc R . .
C3 C 0.9920(3) 1.2451(3) 0.4075(2) 0.0653(7) Uani 1 1 d . . .
H3A H 1.0339 1.3189 0.3735 0.098 Uiso 1 1 calc R . .
H3B H 1.0829 1.2307 0.4655 0.098 Uiso 1 1 calc R . .
H3C H 0.9093 1.2741 0.4370 0.098 Uiso 1 1 calc R . .
C4 C 0.8523(2) 0.6141(2) 0.00228(17) 0.0414(4) Uani 1 1 d . . .
C5 C 0.6556(3) 0.3964(3) -0.1249(2) 0.0679(7) Uani 1 1 d . . .
H5C H 0.7084 0.3238 -0.0961 0.102 Uiso 1 1 calc R . .
H5D H 0.6068 0.3665 -0.2031 0.102 Uiso 1 1 calc R . .
H5E H 0.5694 0.4097 -0.0934 0.102 Uiso 1 1 calc R . .
C6 C 1.0040(4) 0.7954(3) -0.0701(2) 0.0733(8) Uani 1 1 d . . .
H6A H 1.0495 0.7285 -0.1083 0.110 Uiso 1 1 calc R . .
H6B H 1.0855 0.8853 -0.0398 0.110 Uiso 1 1 calc R . .
H6C H 0.9048 0.8112 -0.1201 0.110 Uiso 1 1 calc R . .
C7 C 0.7017(2) 0.57346(19) 0.36188(14) 0.0326(4) Uani 1 1 d . . .
C8 C 0.5959(2) 0.53524(18) 0.43269(15) 0.0322(4) Uani 1 1 d . . .
C9 C 0.5338(3) 0.6381(2) 0.4834(2) 0.0497(5) Uani 1 1 d . . .
H9 H 0.5559 0.7322 0.4729 0.060 Uiso 1 1 calc R . .
C10 C 0.5609(3) 0.3964(2) 0.4501(2) 0.0532(6) Uani 1 1 d . . .
H10 H 0.6017 0.3253 0.4168 0.064 Uiso 1 1 calc R . .
C11 C 1.1865(2) 0.8923(2) 0.32069(16) 0.0366(4) Uani 1 1 d . . .
C12 C 1.3486(2) 0.94871(18) 0.41410(15) 0.0317(4) Uani 1 1 d . . .
C13 C 1.3510(2) 0.9731(2) 0.52253(16) 0.0358(4) Uani 1 1 d . . .
H13 H 1.2506 0.9548 0.5378 0.043 Uiso 1 1 calc R . .
C14 C 1.4999(2) 0.9759(2) 0.39245(16) 0.0359(4) Uani 1 1 d . . .
H14 H 1.5005 0.9597 0.3205 0.043 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'
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
O1 Zn1 O3 100.28(6) . . ?
O1 Zn1 S2 108.45(4) . . ?
O3 Zn1 S2 121.02(5) . . ?
O1 Zn1 S1 105.72(4) . . ?
O3 Zn1 S1 111.61(5) . . ?
S2 Zn1 S1 108.44(2) . . ?
C1 S1 Zn1 107.20(7) . . ?
C4 S2 Zn1 107.71(7) . . ?
C7 O1 Zn1 119.77(12) . . ?
C11 O3 Zn1 122.49(13) . . ?
C1 N1 C2 124.5(2) . . ?
C1 N2 C3 125.9(2) . . ?
C4 N3 C5 124.6(2) . . ?
C4 N4 C6 124.1(2) . . ?
N1 C1 N2 119.15(18) . . ?
N1 C1 S1 120.09(15) . . ?
N2 C1 S1 120.76(15) . . ?
N4 C4 N3 119.8(2) . . ?
N4 C4 S2 121.22(16) . . ?
N3 C4 S2 118.92(17) . . ?
O2 C7 O1 124.15(17) . . ?
O2 C7 C8 119.69(16) . . ?
O1 C7 C8 116.12(16) . . ?
C9 C8 C10 118.09(18) . . ?
C9 C8 C7 121.00(16) . . ?
C10 C8 C7 120.89(17) . . ?
C8 C9 C10 121.01(18) . 2_666 ?
C8 C10 C9 120.90(19) . 2_666 ?
O4 C11 O3 124.47(18) . . ?
O4 C11 C12 120.39(17) . . ?
O3 C11 C12 115.14(17) . . ?
C13 C12 C14 118.89(17) . . ?
C13 C12 C11 121.37(16) . . ?
C14 C12 C11 119.74(17) . . ?
C14 C13 C12 120.97(16) 2_876 . ?
C13 C14 C12 120.14(17) 2_876 . ?
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
Zn1 O1 1.9682(12) . ?
Zn1 O3 1.9729(13) . ?
Zn1 S2 2.3156(5) . ?
Zn1 S1 2.3493(5) . ?
S1 C1 1.7248(19) . ?
S2 C4 1.723(2) . ?
O1 C7 1.269(2) . ?
O2 C7 1.236(2) . ?
O3 C11 1.292(2) . ?
O4 C11 1.225(3) . ?
N1 C1 1.323(3) . ?
N1 C2 1.448(3) . ?
N2 C1 1.324(3) . ?
N2 C3 1.452(3) . ?
N3 C4 1.331(3) . ?
N3 C5 1.461(3) . ?
N4 C4 1.321(3) . ?
N4 C6 1.454(3) . ?
C7 C8 1.508(2) . ?
C8 C9 1.377(3) . ?
C8 C10 1.383(3) . ?
C9 C10 1.383(3) 2_666 ?
C10 C9 1.383(3) 2_666 ?
C11 C12 1.506(3) . ?
C12 C13 1.392(3) . ?
C12 C14 1.393(2) . ?
C13 C14 1.379(3) 2_876 ?
C14 C13 1.379(3) 2_876 ?
