#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/18/7211899.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_7211899
loop_
_publ_author_name
'Poplaukhin, Pavel'
'Tiekink, Edward R. T.'
_publ_section_title
;
 Interwoven coordination polymers sustained by tautomeric forms of the
 bridging ligand
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              1302
_journal_paper_doi               10.1039/b916585a
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         'C30 H46 N8 O6 S8 Zn2'
_chemical_formula_sum            'C30 H46 N8 O6 S8 Zn2'
_chemical_formula_weight         1001.97
_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                82.811(17)
_cell_angle_beta                 78.712(13)
_cell_angle_gamma                89.077(17)
_cell_formula_units_Z            1
_cell_length_a                   8.460(4)
_cell_length_b                   9.438(4)
_cell_length_c                   13.305(5)
_cell_measurement_reflns_used    4033
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      40.5
_cell_measurement_theta_min      2.5
_cell_volume                     1033.6(8)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics
'ORTEPII (Johnson, 1976) & DIAMOND (Crystal Impact, 2006)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHEXLS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      98(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  AFC12Κ/SATURN724
_diffrn_measurement_method       ω
_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  0.043
_diffrn_reflns_av_sigmaI/netI    0.058
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7700
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.5
_diffrn_standards_decay_%        '< 1'
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.616
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             518
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.89
_refine_diff_density_min         -0.74
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.09
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.09
_refine_ls_R_factor_all          0.071
_refine_ls_R_factor_gt           0.057
_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)+(0.0460P)²+2.2398P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.123
_refine_ls_wR_factor_ref         0.131
_reflns_number_gt                3946
_reflns_number_total             4721
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b916585a.txt
_cod_data_source_block           CSD699066
_cod_original_cell_volume        1033.7(7)
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_database_code               7211899
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
Zn Zn 0.70591(6) 0.42847(5) 0.28582(3) 0.02173(14) Uani 1 1 d .
S1 S 0.90606(12) 0.27711(10) 0.33781(7) 0.0217(2) Uani 1 1 d .
S2 S 0.69026(12) 0.45517(11) 0.47310(7) 0.0229(2) Uani 1 1 d .
S3 S 0.45094(12) 0.37810(10) 0.25890(7) 0.0228(2) Uani 1 1 d .
S4 S 0.74064(13) 0.35737(11) 0.09361(7) 0.0244(2) Uani 1 1 d .
O1 O 0.7861(4) 0.1383(4) 0.7237(2) 0.0378(8) Uani 1 1 d .
H1O H 0.7501 0.0987 0.6796 0.057 Uiso 1 1 calc R
O2 O 0.2601(4) 0.0497(3) 0.0941(2) 0.0380(8) Uani 1 1 d .
H2O H 0.2597 -0.0279 0.1326 0.057 Uiso 1 1 calc R
O3 O 0.3557(4) 0.9475(3) 0.4331(2) 0.0287(6) Uani 1 1 d .
N1 N 0.9342(4) 0.3034(4) 0.5307(2) 0.0229(7) Uani 1 1 d .
N2 N 0.4409(5) 0.3115(4) 0.0713(3) 0.0275(8) Uani 1 1 d .
N3 N 0.7819(4) 0.6370(3) 0.2272(2) 0.0203(7) Uani 1 1 d .
N4 N 0.6198(4) 1.0149(3) 0.3737(2) 0.0225(7) Uani 1 1 d .
H4n H 0.7087 1.0369 0.3935 0.027 Uiso 1 1 calc R
C1 C 0.8517(5) 0.3411(4) 0.4566(3) 0.0204(7) Uani 1 1 d .
C2 C 0.8992(5) 0.3644(5) 0.6289(3) 0.0259(8) Uani 1 1 d .
H2A H 0.8709 0.4662 0.6152 0.031 Uiso 1 1 calc R
H2B H 0.9976 0.3600 0.6590 0.031 Uiso 1 1 calc R
C3 C 0.7638(5) 0.2883(5) 0.7061(3) 0.0308(9) Uani 1 1 d .
H3A H 0.7536 0.3282 0.7724 0.037 Uiso 1 1 calc R
H3B H 0.6617 0.3068 0.6811 0.037 Uiso 1 1 calc R
C4 C 1.0698(5) 0.2031(5) 0.5170(3) 0.0282(9) Uani 1 1 d .
H4A H 1.0556 0.1405 0.4660 0.042 Uiso 1 1 calc R
H4B H 1.0730 0.1453 0.5831 0.042 Uiso 1 1 calc R
H4C H 1.1711 0.2569 0.4929 0.042 Uiso 1 1 calc R
C5 C 0.5351(5) 0.3460(4) 0.1334(3) 0.0208(8) Uani 1 1 d .
C6 C 0.2648(5) 0.3056(5) 0.1016(4) 0.0315(10) Uani 1 1 d .
H6A H 0.2176 0.3279 0.0390 0.038 Uiso 1 1 calc R
H6B H 0.2291 0.3798 0.1473 0.038 Uiso 1 1 calc R
C7 C 0.2019(6) 0.1630(5) 0.1564(3) 0.0346(10) Uani 1 1 d .
H7A H 0.2376 0.1451 0.2234 0.041 Uiso 1 1 calc R
H7B H 0.0826 0.1633 0.1705 0.041 Uiso 1 1 calc R
C8 C 0.5082(6) 0.2747(5) -0.0330(3) 0.0365(11) Uani 1 1 d .
H8A H 0.5033 0.3582 -0.0841 0.055 Uiso 1 1 calc R
H8B H 0.4455 0.1961 -0.0477 0.055 Uiso 1 1 calc R
H8C H 0.6207 0.2454 -0.0366 0.055 Uiso 1 1 calc R
C9 C 0.9092(5) 0.6654(4) 0.1496(3) 0.0211(8) Uani 1 1 d .
H9 H 0.9694 0.5879 0.1229 0.025 Uiso 1 1 calc R
C10 C 0.9560(5) 0.8026(4) 0.1074(3) 0.0250(8) Uani 1 1 d .
H10 H 1.0489 0.8194 0.0542 0.030 Uiso 1 1 calc R
C11 C 0.8656(5) 0.9159(4) 0.1436(3) 0.0246(8) Uani 1 1 d .
H11 H 0.8944 1.0111 0.1141 0.030 Uiso 1 1 calc R
C12 C 0.7324(4) 0.8893(4) 0.2237(3) 0.0176(7) Uani 1 1 d .
C13 C 0.6965(4) 0.7477(4) 0.2638(3) 0.0192(7) Uani 1 1 d .
H13 H 0.6075 0.7281 0.3195 0.023 Uiso 1 1 calc R
C14 C 0.6268(5) 1.0096(4) 0.2641(3) 0.0231(8) Uani 1 1 d .
H14A H 0.6695 1.1017 0.2250 0.028 Uiso 1 1 calc R
H14B H 0.5164 0.9966 0.2521 0.028 Uiso 1 1 calc R
C15 C 0.4879(5) 0.9885(4) 0.4457(3) 0.0226(8) 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'
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'
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_3
N3 Zn S3 112.75(9) .
N3 Zn S1 115.18(10) .
S3 Zn S1 130.94(5) .
N3 Zn S2 96.70(9) .
S3 Zn S2 109.39(4) .
S1 Zn S2 74.95(4) .
N3 Zn S4 90.67(9) .
S3 Zn S4 72.59(4) .
S1 Zn S4 96.80(4) .
S2 Zn S4 170.70(4) .
C1 S1 Zn 85.94(13) .
C1 S2 Zn 81.22(13) .
C5 S3 Zn 89.70(14) .
C5 S4 Zn 78.94(13) .
C3 O1 H1O 109.5 .
C7 O2 H2O 109.5 .
C1 N1 C2 121.5(3) .
C1 N1 C4 121.8(3) .
C2 N1 C4 116.7(3) .
C5 N2 C6 122.6(4) .
C5 N2 C8 121.6(4) .
C6 N2 C8 115.8(3) .
C9 N3 C13 118.2(3) .
C9 N3 Zn 122.0(3) .
C13 N3 Zn 119.6(3) .
C15 N4 C14 124.1(3) .
C15 N4 H4n 118.0 .
C14 N4 H4n 118.0 .
N1 C1 S2 122.0(3) .
N1 C1 S1 120.3(3) .
S2 C1 S1 117.7(2) .
N1 C2 C3 113.0(3) .
N1 C2 H2A 109.0 .
C3 C2 H2A 109.0 .
N1 C2 H2B 109.0 .
C3 C2 H2B 109.0 .
H2A C2 H2B 107.8 .
O1 C3 C2 113.3(4) .
O1 C3 H3A 108.9 .
C2 C3 H3A 108.9 .
O1 C3 H3B 108.9 .
C2 C3 H3B 108.9 .
H3A C3 H3B 107.7 .
N1 C4 H4A 109.5 .
N1 C4 H4B 109.5 .
H4A C4 H4B 109.5 .
N1 C4 H4C 109.5 .
H4A C4 H4C 109.5 .
H4B C4 H4C 109.5 .
N2 C5 S4 121.3(3) .
N2 C5 S3 120.0(3) .
S4 C5 S3 118.7(2) .
N2 C6 C7 113.2(4) .
N2 C6 H6A 108.9 .
C7 C6 H6A 108.9 .
N2 C6 H6B 108.9 .
C7 C6 H6B 108.9 .
H6A C6 H6B 107.7 .
O2 C7 C6 110.6(4) .
O2 C7 H7A 109.5 .
C6 C7 H7A 109.5 .
O2 C7 H7B 109.5 .
C6 C7 H7B 109.5 .
H7A C7 H7B 108.1 .
N2 C8 H8A 109.5 .
N2 C8 H8B 109.5 .
H8A C8 H8B 109.5 .
N2 C8 H8C 109.5 .
H8A C8 H8C 109.5 .
H8B C8 H8C 109.5 .
N3 C9 C10 122.5(4) .
N3 C9 H9 118.8 .
C10 C9 H9 118.8 .
C9 C10 C11 119.1(4) .
C9 C10 H10 120.5 .
C11 C10 H10 120.5 .
C10 C11 C12 119.6(4) .
C10 C11 H11 120.2 .
C12 C11 H11 120.2 .
C13 C12 C11 117.5(3) .
C13 C12 C14 120.9(3) .
C11 C12 C14 121.6(3) .
N3 C13 C12 123.1(3) .
N3 C13 H13 118.5 .
C12 C13 H13 118.5 .
N4 C14 C12 112.4(3) .
N4 C14 H14A 109.1 .
C12 C14 H14A 109.1 .
N4 C14 H14B 109.1 .
C12 C14 H14B 109.1 .
H14A C14 H14B 107.9 .
O3 C15 N4 126.8(4) .
O3 C15 C15 120.1(5) 2_676
N4 C15 C15 113.1(4) 2_676
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn N3 2.087(3) .
Zn S3 2.3207(14) .
Zn S1 2.3495(13) .
Zn S2 2.5132(14) .
Zn S4 2.6844(14) .
S1 C1 1.738(4) .
S2 C1 1.723(4) .
S3 C5 1.744(4) .
S4 C5 1.717(4) .
O1 C3 1.422(5) .
O1 H1O 0.8400 .
O2 C7 1.456(5) .
O2 H2O 0.8400 .
O3 C15 1.238(5) .
N1 C1 1.326(5) .
N1 C2 1.469(5) .
N1 C4 1.474(5) .
N2 C5 1.326(5) .
N2 C6 1.465(6) .
N2 C8 1.475(6) .
N3 C9 1.343(5) .
N3 C13 1.347(5) .
N4 C15 1.325(5) .
N4 C14 1.456(5) .
N4 H4n 0.8800 .
C2 C3 1.505(6) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C6 C7 1.501(6) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 C10 1.377(6) .
C9 H9 0.9500 .
C10 C11 1.385(6) .
C10 H10 0.9500 .
C11 C12 1.393(5) .
C11 H11 0.9500 .
C12 C13 1.391(5) .
C12 C14 1.519(5) .
C13 H13 0.9500 .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 C15 1.541(8) 2_676
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_4
N3 Zn S1 C1 87.53(16) .
S3 Zn S1 C1 -105.69(13) .
S2 Zn S1 C1 -2.87(13) .
S4 Zn S1 C1 -178.51(13) .
N3 Zn S2 C1 -111.41(16) .
S3 Zn S2 C1 131.58(13) .
S1 Zn S2 C1 2.93(13) .
S4 Zn S2 C1 30.8(3) .
N3 Zn S3 C5 81.86(16) .
S1 Zn S3 C5 -85.17(13) .
S2 Zn S3 C5 -171.78(12) .
S4 Zn S3 C5 -1.35(12) .
N3 Zn S4 C5 -112.28(16) .
S3 Zn S4 C5 1.40(13) .
S1 Zn S4 C5 132.26(13) .
S2 Zn S4 C5 105.2(3) .
S3 Zn N3 C9 -115.6(3) .
S1 Zn N3 C9 53.6(3) .
S2 Zn N3 C9 130.1(3) .
S4 Zn N3 C9 -44.2(3) .
S3 Zn N3 C13 60.8(3) .
S1 Zn N3 C13 -130.0(3) .
S2 Zn N3 C13 -53.5(3) .
S4 Zn N3 C13 132.1(3) .
C2 N1 C1 S2 -4.1(5) .
C4 N1 C1 S2 178.5(3) .
C2 N1 C1 S1 175.1(3) .
C4 N1 C1 S1 -2.2(5) .
Zn S2 C1 N1 174.9(3) .
Zn S2 C1 S1 -4.31(19) .
Zn S1 C1 N1 -174.7(3) .
Zn S1 C1 S2 4.6(2) .
C1 N1 C2 C3 84.2(5) .
C4 N1 C2 C3 -98.3(4) .
N1 C2 C3 O1 53.1(5) .
C6 N2 C5 S4 -177.9(3) .
C8 N2 C5 S4 2.9(5) .
C6 N2 C5 S3 3.1(5) .
C8 N2 C5 S3 -176.1(3) .
Zn S4 C5 N2 179.0(3) .
Zn S4 C5 S3 -2.03(18) .
Zn S3 C5 N2 -178.7(3) .
Zn S3 C5 S4 2.3(2) .
C5 N2 C6 C7 -87.7(5) .
C8 N2 C6 C7 91.6(4) .
N2 C6 C7 O2 -55.2(5) .
C13 N3 C9 C10 0.7(5) .
Zn N3 C9 C10 177.1(3) .
N3 C9 C10 C11 -2.2(6) .
C9 C10 C11 C12 1.7(6) .
C10 C11 C12 C13 0.0(6) .
C10 C11 C12 C14 -178.3(4) .
C9 N3 C13 C12 1.2(5) .
Zn N3 C13 C12 -175.3(3) .
C11 C12 C13 N3 -1.6(5) .
C14 C12 C13 N3 176.8(3) .
C15 N4 C14 C12 -113.6(4) .
C13 C12 C14 N4 60.4(5) .
C11 C12 C14 N4 -121.3(4) .
C14 N4 C15 O3 4.9(6) .
C14 N4 C15 C15 -176.2(4) 2_676
