#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:20:30 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179838 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/34/7013402.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_7013402
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            'C22 H44 N8 O10 S4 Zn2'
_chemical_formula_weight         839.63
_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                77.79(2)
_cell_angle_beta                 77.94(2)
_cell_angle_gamma                85.63(2)
_cell_formula_units_Z            1
_cell_length_a                   9.011(2)
_cell_length_b                   9.701(2)
_cell_length_c                   11.141(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     930.3(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      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12787
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    1.570
_exptl_absorpt_correction_T_max  1.024
_exptl_absorpt_correction_T_min  0.974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sortav Blessing (1995)
multi-scan from symmetry-related measurements (Blessing 1995)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.030(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         4250
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0376
_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)+(0.0494P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0994
_reflns_number_gt                3083
_reflns_number_total             4250
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b307420j.txt
_cod_data_source_block           compound11_h01njb1
_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 'multiscan' 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_cell_volume        930.4(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7013402
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 0.16348(3) 0.13814(3) 0.26644(3) 0.03903(13) Uani 1 1 d . . .
S1 S 0.19813(10) 0.01015(8) 0.10865(6) 0.0511(2) Uani 1 1 d . . .
S2 S 0.31225(10) 0.33662(8) 0.18493(7) 0.0599(2) Uani 1 1 d . . .
O1 O 0.2479(2) 0.02273(18) 0.40966(16) 0.0431(4) Uani 1 1 d . . .
O2 O 0.2065(2) -0.17926(19) 0.35882(16) 0.0452(4) Uani 1 1 d . . .
O3 O 0.0987(3) -0.3024(2) 0.80878(18) 0.0690(7) Uani 1 1 d . . .
O4 O 0.0383(2) -0.1697(2) 0.63567(16) 0.0470(5) Uani 1 1 d . . .
O5 O 0.1166(3) 0.1574(2) 0.61930(19) 0.0500(5) Uani 1 1 d D . .
H5A H 0.170(6) 0.106(6) 0.568(5) 0.20(3) Uiso 1 1 d D . .
H5B H 0.018(2) 0.158(4) 0.625(4) 0.104(15) Uiso 1 1 d D . .
N1 N 0.0799(3) 0.2368(3) -0.0257(2) 0.0565(7) Uani 1 1 d D . .
H1 H 0.035(3) 0.263(3) 0.043(2) 0.063(10) Uiso 1 1 d D . .
N2 N 0.2280(3) 0.0856(3) -0.1366(2) 0.0553(7) Uani 1 1 d D . .
H2 H 0.191(3) 0.131(3) -0.198(2) 0.053(9) Uiso 1 1 d D . .
N3 N 0.1969(3) 0.4093(3) 0.4040(2) 0.0489(6) Uani 1 1 d D . .
H3 H 0.169(3) 0.319(2) 0.423(3) 0.063(10) Uiso 1 1 d D . .
N4 N 0.3233(3) 0.5786(3) 0.2532(2) 0.0574(7) Uani 1 1 d D . .
H4 H 0.293(3) 0.634(3) 0.308(2) 0.053(8) Uiso 1 1 d D . .
C1 C 0.1662(3) 0.1207(3) -0.0274(2) 0.0463(7) Uani 1 1 d . . .
C2 C 0.0513(5) 0.3362(4) -0.1357(3) 0.0819(12) Uani 1 1 d . . .
H2A H 0.1461 0.3622 -0.1912 0.123 Uiso 1 1 calc R . .
H2B H -0.0010 0.4188 -0.1111 0.123 Uiso 1 1 calc R . .
H2C H -0.0100 0.2934 -0.1777 0.123 Uiso 1 1 calc R . .
C3 C 0.3292(5) -0.0362(4) -0.1488(3) 0.0722(10) Uani 1 1 d . . .
H3A H 0.4128 -0.0319 -0.1087 0.108 Uiso 1 1 calc R . .
H3B H 0.3669 -0.0367 -0.2359 0.108 Uiso 1 1 calc R . .
H3C H 0.2750 -0.1207 -0.1098 0.108 Uiso 1 1 calc R . .
C4 C 0.2736(3) 0.4491(3) 0.2879(2) 0.0419(6) Uani 1 1 d . . .
C5 C 0.1879(5) 0.4895(3) 0.5019(3) 0.0707(10) Uani 1 1 d . . .
H5C H 0.2884 0.5105 0.5073 0.106 Uiso 1 1 calc R . .
H5D H 0.1388 0.4349 0.5806 0.106 Uiso 1 1 calc R . .
H5E H 0.1304 0.5759 0.4825 0.106 Uiso 1 1 calc R . .
C6 C 0.4116(5) 0.6361(4) 0.1291(4) 0.0957(15) Uani 1 1 d . . .
H6A H 0.5093 0.5884 0.1181 0.144 Uiso 1 1 calc R . .
H6B H 0.4243 0.7351 0.1216 0.144 Uiso 1 1 calc R . .
H6C H 0.3590 0.6225 0.0662 0.144 Uiso 1 1 calc R . .
C7 C 0.2577(3) -0.1115(3) 0.4235(2) 0.0376(6) Uani 1 1 d . . .
C8 C 0.3504(3) -0.1885(3) 0.5150(2) 0.0393(6) Uani 1 1 d . . .
C9 C 0.2949(3) -0.2476(3) 0.6336(2) 0.0441(6) Uani 1 1 d . . .
H9 H 0.3631 -0.2973 0.6803 0.053 Uiso 1 1 calc R . .
C10 C 0.5165(4) -0.1981(5) 0.4587(4) 0.0767(11) Uani 1 1 d . . .
H10A H 0.5692 -0.2549 0.5193 0.115 Uiso 1 1 calc R . .
H10B H 0.5566 -0.1051 0.4344 0.115 Uiso 1 1 calc R . .
H10C H 0.5301 -0.2403 0.3864 0.115 Uiso 1 1 calc R . .
C11 C 0.1334(3) -0.2409(3) 0.6976(2) 0.0440(6) 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'
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'
O O 0.0106 0.0060 '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
O4 Zn1 O1 95.87(7) 2_556 . ?
O4 Zn1 S1 121.24(6) 2_556 . ?
O1 Zn1 S1 108.30(5) . . ?
O4 Zn1 S2 116.49(6) 2_556 . ?
O1 Zn1 S2 107.67(6) . . ?
S1 Zn1 S2 105.91(3) . . ?
C1 S1 Zn1 109.01(9) . . ?
C4 S2 Zn1 108.89(9) . . ?
C7 O1 Zn1 119.74(17) . . ?
C11 O4 Zn1 115.60(16) . 2_556 ?
C1 N1 C2 125.0(3) . . ?
C1 N2 C3 123.6(3) . . ?
C4 N3 C5 123.9(3) . . ?
C4 N4 C6 124.1(2) . . ?
N1 C1 N2 119.4(3) . . ?
N1 C1 S1 121.9(2) . . ?
N2 C1 S1 118.7(2) . . ?
N4 C4 N3 118.1(2) . . ?
N4 C4 S2 119.9(2) . . ?
N3 C4 S2 122.0(2) . . ?
O2 C7 O1 124.2(2) . . ?
O2 C7 C8 118.8(2) . . ?
O1 C7 C8 116.7(2) . . ?
C9 C8 C7 125.0(2) . . ?
C9 C8 C10 121.9(3) . . ?
C7 C8 C10 113.1(2) . . ?
C8 C9 C11 125.6(2) . . ?
O3 C11 O4 123.8(3) . . ?
O3 C11 C9 118.1(3) . . ?
O4 C11 C9 118.1(2) . . ?
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 O4 1.9536(18) 2_556 ?
Zn1 O1 2.0000(18) . ?
Zn1 S1 2.3160(8) . ?
Zn1 S2 2.3399(9) . ?
S1 C1 1.725(3) . ?
S2 C4 1.713(3) . ?
O1 C7 1.276(3) . ?
O2 C7 1.245(3) . ?
O3 C11 1.242(3) . ?
O4 C11 1.282(3) . ?
O4 Zn1 1.9536(18) 2_556 ?
N1 C1 1.321(4) . ?
N1 C2 1.446(4) . ?
N2 C1 1.331(3) . ?
N2 C3 1.448(4) . ?
N3 C4 1.325(3) . ?
N3 C5 1.454(4) . ?
N4 C4 1.318(4) . ?
N4 C6 1.462(4) . ?
C7 C8 1.494(4) . ?
C8 C9 1.331(4) . ?
C8 C10 1.501(4) . ?
C9 C11 1.484(4) . ?
