#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/19/7211900.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_7211900
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         1002.09
_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
_cell_angle_beta                 94.743(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.7471(14)
_cell_length_b                   16.151(2)
_cell_length_c                   13.210(2)
_cell_measurement_reflns_used    6446
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      40.6
_cell_measurement_theta_min      2.0
_cell_volume                     2072.5(5)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.027
_diffrn_reflns_av_sigmaI/netI    0.039
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8301
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        '< 1'
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.612
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.18
_refine_diff_density_min         -0.78
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4694
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.048
_refine_ls_R_factor_gt           0.046
_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)+(0.0588P)²+3.8048P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.117
_refine_ls_wR_factor_ref         0.120
_reflns_number_gt                4397
_reflns_number_total             4694
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b916585a.txt
_cod_data_source_block           CSD699067
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C30 H46 N8 O6 S8 Zn2 '
_cod_database_code               7211900
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
Zn Zn 0.52761(3) 0.03016(2) 0.71629(3) 0.02213(12) Uani 1 1 d .
S1 S 0.64829(8) -0.09289(5) 0.70264(5) 0.02500(17) Uani 1 1 d .
S2 S 0.48482(7) -0.05975(5) 0.87790(6) 0.02413(17) Uani 1 1 d .
S3 S 0.60105(7) 0.14868(5) 0.80803(5) 0.02347(16) Uani 1 1 d .
S4 S 0.65410(7) 0.12309(5) 0.59303(5) 0.02351(16) Uani 1 1 d .
O1 O 0.8329(2) -0.18755(16) 1.0607(2) 0.0353(5) Uani 1 1 d .
H1O H 0.8714 -0.1416 1.0538 0.053 Uiso 1 1 calc R
O2 O 0.9941(2) 0.2996(2) 0.8242(2) 0.0434(6) Uani 1 1 d .
H2O H 1.0565 0.2719 0.8562 0.065 Uiso 1 1 calc R
O3 O -0.1720(3) 0.0157(2) 0.9428(2) 0.0481(7) Uani 1 1 d .
H3O H -0.2021 0.0330 0.8853 0.072 Uiso 1 1 calc R
N1 N 0.6569(3) -0.18712(15) 0.86854(19) 0.0233(5) Uani 1 1 d .
N2 N 0.7376(3) 0.25632(16) 0.7017(2) 0.0251(5) Uani 1 1 d .
N3 N 0.3248(2) 0.04151(15) 0.66013(18) 0.0199(5) Uani 1 1 d .
N4 N 0.0471(3) 0.02717(17) 0.87798(19) 0.0266(5) Uani 1 1 d .
C1 C 0.6001(3) -0.12070(18) 0.8220(2) 0.0212(5) Uani 1 1 d .
C2 C 0.6132(3) -0.21727(19) 0.9661(2) 0.0245(6) Uani 1 1 d .
H2A H 0.6295 -0.2777 0.9707 0.029 Uiso 1 1 calc R
H2B H 0.5131 -0.2078 0.9675 0.029 Uiso 1 1 calc R
C3 C 0.6871(3) -0.1760(2) 1.0574(2) 0.0287(6) Uani 1 1 d .
H3A H 0.6662 -0.1160 1.0555 0.034 Uiso 1 1 calc R
H3B H 0.6527 -0.1992 1.1199 0.034 Uiso 1 1 calc R
C4 C 0.7680(4) -0.2338(2) 0.8261(3) 0.0361(8) Uani 1 1 d .
H4A H 0.7283 -0.2779 0.7819 0.054 Uiso 1 1 calc R
H4B H 0.8278 -0.2582 0.8815 0.054 Uiso 1 1 calc R
H4C H 0.8221 -0.1964 0.7866 0.054 Uiso 1 1 calc R
C5 C 0.6714(3) 0.18428(18) 0.6998(2) 0.0223(6) Uani 1 1 d .
C6 C 0.7485(3) 0.3098(2) 0.7927(3) 0.0287(6) Uani 1 1 d .
H6A H 0.6622 0.3056 0.8269 0.034 Uiso 1 1 calc R
H6B H 0.7588 0.3681 0.7712 0.034 Uiso 1 1 calc R
C7 C 0.8691(3) 0.2872(2) 0.8680(3) 0.0343(7) Uani 1 1 d .
H7A H 0.8670 0.3218 0.9297 0.041 Uiso 1 1 calc R
H7B H 0.8613 0.2285 0.8884 0.041 Uiso 1 1 calc R
C8 C 0.8065(3) 0.2856(2) 0.6133(3) 0.0311(7) Uani 1 1 d .
H8A H 0.8837 0.2488 0.6020 0.047 Uiso 1 1 calc R
H8B H 0.8409 0.3419 0.6261 0.047 Uiso 1 1 calc R
H8C H 0.7408 0.2854 0.5530 0.047 Uiso 1 1 calc R
C9 C 0.2860(3) 0.05854(18) 0.5628(2) 0.0212(5) Uani 1 1 d .
H9 H 0.3540 0.0603 0.5154 0.025 Uiso 1 1 calc R
C10 C 0.1495(3) 0.07372(18) 0.5287(2) 0.0218(5) Uani 1 1 d .
H10 H 0.1247 0.0858 0.4592 0.026 Uiso 1 1 calc R
C11 C 0.0498(3) 0.07080(18) 0.5984(2) 0.0209(5) Uani 1 1 d .
H11 H -0.0440 0.0812 0.5768 0.025 Uiso 1 1 calc R
C12 C 0.0882(3) 0.05254(17) 0.6997(2) 0.0196(5) Uani 1 1 d .
C13 C 0.2272(3) 0.03833(17) 0.7267(2) 0.0199(5) Uani 1 1 d .
H13 H 0.2549 0.0257 0.7956 0.024 Uiso 1 1 calc R
C14 C -0.0181(3) 0.0475(2) 0.7770(2) 0.0257(6) Uani 1 1 d .
H14A H -0.0665 0.1012 0.7799 0.031 Uiso 1 1 calc R
H14B H -0.0870 0.0045 0.7558 0.031 Uiso 1 1 calc R
C15 C -0.0329(3) 0.01216(19) 0.9479(2) 0.0228(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'
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 S1 121.64(7) .
N3 Zn S3 110.86(7) .
S1 Zn S3 127.10(3) .
N3 Zn S4 102.33(7) .
S1 Zn S4 100.13(3) .
S3 Zn S4 73.27(3) .
N3 Zn S2 97.41(7) .
S1 Zn S2 72.99(3) .
S3 Zn S2 95.33(3) .
S4 Zn S2 159.69(3) .
C1 S1 Zn 88.53(10) .
C1 S2 Zn 79.27(10) .
C5 S3 Zn 88.25(10) .
C5 S4 Zn 80.64(10) .
C3 O1 H1O 109.5 .
C7 O2 H2O 109.5 .
C15 O3 H3O 109.5 .
C1 N1 C4 121.9(3) .
C1 N1 C2 122.0(2) .
C4 N1 C2 116.1(2) .
C5 N2 C8 121.2(3) .
C5 N2 C6 121.9(3) .
C8 N2 C6 116.8(3) .
C9 N3 C13 118.4(2) .
C9 N3 Zn 123.41(19) .
C13 N3 Zn 117.96(19) .
C15 N4 C14 117.1(2) .
N1 C1 S2 121.8(2) .
N1 C1 S1 119.5(2) .
S2 C1 S1 118.66(17) .
N1 C2 C3 113.6(2) .
N1 C2 H2A 108.8 .
C3 C2 H2A 108.8 .
N1 C2 H2B 108.8 .
C3 C2 H2B 108.8 .
H2A C2 H2B 107.7 .
O1 C3 C2 112.0(3) .
O1 C3 H3A 109.2 .
C2 C3 H3A 109.2 .
O1 C3 H3B 109.2 .
C2 C3 H3B 109.2 .
H3A C3 H3B 107.9 .
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 122.2(2) .
N2 C5 S3 120.0(2) .
S4 C5 S3 117.85(17) .
N2 C6 C7 113.1(3) .
N2 C6 H6A 109.0 .
C7 C6 H6A 109.0 .
N2 C6 H6B 109.0 .
C7 C6 H6B 109.0 .
H6A C6 H6B 107.8 .
O2 C7 C6 110.2(3) .
O2 C7 H7A 109.6 .
C6 C7 H7A 109.6 .
O2 C7 H7B 109.6 .
C6 C7 H7B 109.6 .
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 122.3(3) .
N3 C9 H9 118.9 .
C10 C9 H9 118.9 .
C9 C10 C11 118.8(3) .
C9 C10 H10 120.6 .
C11 C10 H10 120.6 .
C12 C11 C10 119.7(2) .
C12 C11 H11 120.1 .
C10 C11 H11 120.1 .
C11 C12 C13 117.4(3) .
C11 C12 C14 121.0(2) .
C13 C12 C14 121.6(2) .
N3 C13 C12 123.4(3) .
N3 C13 H13 118.3 .
C12 C13 H13 118.3 .
N4 C14 C12 110.9(2) .
N4 C14 H14A 109.5 .
C12 C14 H14A 109.5 .
N4 C14 H14B 109.5 .
C12 C14 H14B 109.5 .
H14A C14 H14B 108.1 .
N4 C15 O3 128.6(3) .
N4 C15 C15 117.7(3) 3_557
O3 C15 C15 113.7(3) 3_557
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn N3 2.061(2) .
Zn S1 2.3241(8) .
Zn S3 2.3456(8) .
Zn S4 2.5993(8) .
Zn S2 2.6435(9) .
S1 C1 1.741(3) .
S2 C1 1.707(3) .
S3 C5 1.734(3) .
S4 C5 1.719(3) .
O1 C3 1.431(4) .
O1 H1O 0.8400 .
O2 C7 1.406(4) .
O2 H2O 0.8400 .
O3 C15 1.353(4) .
O3 H3O 0.8400 .
N1 C1 1.334(4) .
N1 C4 1.468(4) .
N1 C2 1.473(4) .
N2 C5 1.330(4) .
N2 C8 1.472(4) .
N2 C6 1.477(4) .
N3 C9 1.338(4) .
N3 C13 1.349(4) .
N4 C15 1.281(4) .
N4 C14 1.466(4) .
C2 C3 1.507(4) .
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 1.520(4) .
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 1.390(4) .
C9 H9 0.9500 .
C10 C11 1.394(4) .
C10 H10 0.9500 .
C11 C12 1.391(4) .
C11 H11 0.9500 .
C12 C13 1.392(4) .
C12 C14 1.515(4) .
C13 H13 0.9500 .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 C15 1.521(5) 3_557
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 -92.70(12) .
S3 Zn S1 C1 79.29(10) .
S4 Zn S1 C1 155.90(9) .
S2 Zn S1 C1 -4.42(9) .
N3 Zn S2 C1 125.48(11) .
S1 Zn S2 C1 4.59(9) .
S3 Zn S2 C1 -122.64(9) .
S4 Zn S2 C1 -68.17(12) .
N3 Zn S3 C5 -97.24(12) .
S1 Zn S3 C5 90.06(9) .
S4 Zn S3 C5 -0.11(9) .
S2 Zn S3 C5 162.74(9) .
N3 Zn S4 C5 108.46(11) .
S1 Zn S4 C5 -125.77(9) .
S3 Zn S4 C5 0.11(9) .
S2 Zn S4 C5 -57.68(12) .
S1 Zn N3 C9 -83.3(2) .
S3 Zn N3 C9 103.5(2) .
S4 Zn N3 C9 27.0(2) .
S2 Zn N3 C9 -157.9(2) .
S1 Zn N3 C13 102.3(2) .
S3 Zn N3 C13 -70.8(2) .
S4 Zn N3 C13 -147.40(19) .
S2 Zn N3 C13 27.8(2) .
C4 N1 C1 S2 -172.5(2) .
C2 N1 C1 S2 6.6(4) .
C4 N1 C1 S1 5.3(4) .
C2 N1 C1 S1 -175.5(2) .
Zn S2 C1 N1 171.2(2) .
Zn S2 C1 S1 -6.68(14) .
Zn S1 C1 N1 -170.5(2) .
Zn S1 C1 S2 7.48(15) .
C1 N1 C2 C3 -86.6(3) .
C4 N1 C2 C3 92.6(3) .
N1 C2 C3 O1 -58.9(3) .
C8 N2 C5 S4 -3.3(4) .
C6 N2 C5 S4 178.1(2) .
C8 N2 C5 S3 175.8(2) .
C6 N2 C5 S3 -2.7(4) .
Zn S4 C5 N2 179.0(2) .
Zn S4 C5 S3 -0.16(13) .
Zn S3 C5 N2 -179.0(2) .
Zn S3 C5 S4 0.18(14) .
C5 N2 C6 C7 85.7(3) .
C8 N2 C6 C7 -92.9(3) .
N2 C6 C7 O2 63.8(4) .
C13 N3 C9 C10 0.6(4) .
Zn N3 C9 C10 -173.7(2) .
N3 C9 C10 C11 -0.2(4) .
C9 C10 C11 C12 -0.3(4) .
C10 C11 C12 C13 0.4(4) .
C10 C11 C12 C14 -179.0(3) .
C9 N3 C13 C12 -0.6(4) .
Zn N3 C13 C12 174.1(2) .
C11 C12 C13 N3 0.1(4) .
C14 C12 C13 N3 179.4(3) .
C15 N4 C14 C12 -172.6(3) .
C11 C12 C14 N4 179.8(3) .
C13 C12 C14 N4 0.5(4) .
C14 N4 C15 O3 -3.0(5) .
C14 N4 C15 C15 177.8(3) 3_557
