#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:22:48 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179575 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/40/4504052.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_4504052
loop_
_publ_author_name
'Park, Hyunsoo'
'Krigsfeld, Gabriel'
'Parise, John B.'
_publ_section_title
;
 Solvothermal Synthesis and Structural Characterization of New
 Zn−Triazole−Sulfoisophthalate Frameworks
;
_journal_issue                   4
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              736
_journal_paper_doi               10.1021/cg060741x
_journal_volume                  7
_journal_year                    2007
_chemical_formula_sum            'C32 H30 N24 O21.06 S2 Zn7'
_chemical_formula_weight         1609.63
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.95(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.050(3)
_cell_length_b                   12.517(3)
_cell_length_c                   15.377(3)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      1.84
_cell_volume                     2678.3(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2000)'
_computing_structure_solution    'SHELXS (Sheldrick, 2000)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.826
_diffrn_measurement_device_type  'Bruker SMART 1K CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13853
_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.84
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker P4'
_exptl_absorpt_coefficient_mu    3.258
_exptl_absorpt_correction_T_max  0.521
_exptl_absorpt_correction_T_min  0.355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.996
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1601
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.325
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         4523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0424P)²+5.8969P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.0947
_reflns_number_gt                4261
_reflns_number_total             4523
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg060741xsi20061021_025917.cif
_cod_data_source_block           structure1
_cod_original_cell_volume        2678.3(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4504052
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Zn1 Zn -0.06008(4) 0.19899(4) 0.15288(4) 0.01985(14) Uani 1 1 d .
Zn2 Zn 0.0000 0.0000 0.0000 0.01782(17) Uani 1 2 d S
Zn3 Zn -0.19115(4) 0.31114(4) 0.31045(3) 0.01962(13) Uani 1 1 d .
Zn4 Zn 0.14007(4) 0.60807(4) 0.22061(4) 0.02173(14) Uani 1 1 d .
S1 S 0.25851(9) 0.43464(9) 0.07618(9) 0.0305(3) Uani 1 1 d .
O1 O -0.1011(3) 0.2606(3) 0.4117(2) 0.0321(8) Uani 1 1 d .
O2 O -0.0680(3) 0.1624(3) 0.3009(2) 0.0309(8) Uani 1 1 d .
O3 O -0.2470(2) 0.2918(3) 0.1861(2) 0.0304(8) Uani 1 1 d .
O4 O 0.3964(3) 0.7543(4) -0.1979(3) 0.0530(12) Uani 1 1 d .
O5 O 0.2041(3) 0.4946(3) 0.1273(3) 0.0582(14) Uani 1 1 d .
O6 O 0.3162(4) 0.3639(5) 0.1278(8) 0.192(5) Uani 1 1 d .
O7 O 0.1988(6) 0.3910(6) 0.0056(4) 0.155(4) Uani 1 1 d .
N1 N -0.0810(3) 0.3992(3) 0.2589(2) 0.0190(8) Uani 1 1 d .
N2 N -0.0440(3) 0.3504(3) 0.1917(3) 0.0222(9) Uani 1 1 d .
N3 N 0.0398(3) 0.4965(3) 0.2255(3) 0.0226(9) Uani 1 1 d .
N4 N 0.0775(3) 0.1475(3) 0.1656(3) 0.0209(8) Uani 1 1 d .
N5 N 0.1033(3) 0.0679(3) 0.1126(3) 0.0227(9) Uani 1 1 d .
N6 N 0.2299(3) 0.1101(3) 0.2076(3) 0.0221(8) Uani 1 1 d .
N7 N -0.1349(3) 0.0640(3) 0.1376(2) 0.0199(8) Uani 1 1 d .
N8 N -0.1117(3) -0.0097(3) 0.0786(3) 0.0211(8) Uani 1 1 d .
N9 N -0.2265(3) -0.0763(3) 0.1464(3) 0.0238(9) Uani 1 1 d .
N10 N 0.1057(3) 0.7058(3) 0.1180(3) 0.0256(9) Uani 1 1 d .
N11 N 0.0720(3) 0.7682(3) -0.0164(3) 0.0231(9) Uani 1 1 d .
N12 N 0.0493(3) 0.8449(3) 0.0406(3) 0.0218(8) Uani 1 1 d .
C1 C 0.0266(3) 0.4107(3) 0.1735(3) 0.0248(10) Uani 1 1 d .
H1 H 0.0634 0.3957 0.1292 0.030 Uiso 1 1 calc R
C2 C -0.0299(3) 0.4847(4) 0.2766(3) 0.0250(10) Uani 1 1 d .
H2 H -0.0404 0.5331 0.3202 0.030 Uiso 1 1 calc R
C3 C 0.1544(3) 0.1693(4) 0.2211(3) 0.0265(11) Uani 1 1 d .
H3 H 0.1561 0.2205 0.2651 0.032 Uiso 1 1 calc R
C4 C 0.1931(3) 0.0490(4) 0.1394(3) 0.0262(11) Uani 1 1 d .
H4 H 0.2287 -0.0021 0.1140 0.031 Uiso 1 1 calc R
C5 C -0.2024(3) 0.0219(4) 0.1772(3) 0.0241(10) Uani 1 1 d .
H5 H -0.2302 0.0557 0.2212 0.029 Uiso 1 1 calc R
C6 C -0.1677(3) -0.0911(4) 0.0859(3) 0.0264(11) Uani 1 1 d .
H6 H -0.1669 -0.1530 0.0527 0.032 Uiso 1 1 calc R
C7 C 0.1045(4) 0.6874(4) 0.0322(3) 0.0262(11) Uani 1 1 d .
H7 H 0.1247 0.6237 0.0097 0.031 Uiso 1 1 calc R
C8 C 0.0701(4) 0.8053(3) 0.1187(3) 0.0264(11) Uani 1 1 d .
H8 H 0.0614 0.8417 0.1697 0.032 Uiso 1 1 calc R
C9 C -0.0524(3) 0.1902(4) 0.3794(3) 0.0248(10) Uani 1 1 d .
C10 C 0.0280(3) 0.1424(4) 0.4392(3) 0.0247(10) Uani 1 1 d .
C11 C 0.0526(4) 0.1860(4) 0.5211(3) 0.0282(11) Uani 1 1 d .
H11 H 0.0137 0.2384 0.5407 0.034 Uiso 1 1 calc R
C12 C 0.3661(3) 0.6533(4) -0.0748(3) 0.0280(11) Uani 1 1 d .
C13 C 0.3094(4) 0.5739(4) -0.0459(3) 0.0282(11) Uani 1 1 d .
H13 H 0.2539 0.5517 -0.0814 0.034 Uiso 1 1 calc R
C14 C 0.3350(3) 0.5277(4) 0.0349(3) 0.0245(10) Uani 1 1 d .
C15 C 0.4159(3) 0.5620(4) 0.0888(3) 0.0251(10) Uani 1 1 d .
H15 H 0.4326 0.5312 0.1438 0.030 Uiso 1 1 calc R
C16 C 0.3358(4) 0.7091(4) -0.1595(3) 0.0324(12) Uani 1 1 d .
O1W O -0.2823(3) 0.1760(3) 0.3395(3) 0.0356(9) Uani 1 1 d .
O2W O 0.0830(3) 0.7037(3) 0.3129(3) 0.0358(10) Uani 1 1 d .
O3W O 0.9134(8) 0.4497(10) 0.5237(7) 0.216(6) Uani 1 1 d .
O4W O 0.8274(10) 0.6375(11) 0.5776(11) 0.142(6) Uani 0.53 1 d P
H2W H 0.122(5) 0.751(5) 0.334(4) 0.05(2) Uiso 1 1 d .
H22W H 0.036(4) 0.716(4) 0.316(4) 0.025(17) Uiso 1 1 d .
H11W H -0.293(5) 0.154(5) 0.387(5) 0.06(2) Uiso 1 1 d .
H1W H -0.332(5) 0.183(5) 0.311(4) 0.04(2) Uiso 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_1
_geom_angle_site_symmetry_3
N7 Zn1 N2 151.84(15) . .
N7 Zn1 N4 102.89(15) . .
N2 Zn1 N4 101.97(15) . .
N7 Zn1 N11 94.56(15) . 3_565
N2 Zn1 N11 95.89(15) . 3_565
N4 Zn1 N11 95.80(16) . 3_565
N7 Zn1 O2 81.56(14) . .
N2 Zn1 O2 85.02(14) . .
N4 Zn1 O2 90.95(14) . .
N11 Zn1 O2 172.84(14) 3_565 .
N8 Zn2 N8 180.0 . 3
N8 Zn2 N12 90.99(14) . 1_545
N8 Zn2 N12 89.01(14) 3 1_545
N8 Zn2 N12 89.02(14) . 3_565
N8 Zn2 N12 90.98(14) 3 3_565
N12 Zn2 N12 180.00(7) 1_545 3_565
N8 Zn2 N5 88.12(14) . 3
N8 Zn2 N5 91.87(14) 3 3
N12 Zn2 N5 91.73(14) 1_545 3
N12 Zn2 N5 88.27(14) 3_565 3
N8 Zn2 N5 91.88(14) . .
N8 Zn2 N5 88.12(14) 3 .
N12 Zn2 N5 88.27(14) 1_545 .
N12 Zn2 N5 91.73(14) 3_565 .
N5 Zn2 N5 180.0 3 .
O1 Zn3 O3 148.21(15) . .
O1 Zn3 N9 107.63(16) . 2_455
O3 Zn3 N9 103.72(16) . 2_455
O1 Zn3 N1 92.29(15) . .
O3 Zn3 N1 85.16(14) . .
N9 Zn3 N1 103.98(14) 2_455 .
O1 Zn3 O1W 85.48(16) . .
O3 Zn3 O1W 86.43(16) . .
N9 Zn3 O1W 95.45(15) 2_455 .
N1 Zn3 O1W 160.17(14) . .
O1 Zn3 C9 28.33(14) . .
O3 Zn3 C9 120.12(16) . .
N9 Zn3 C9 135.96(16) 2_455 .
N1 Zn3 C9 84.86(14) . .
O1W Zn3 C9 83.89(16) . .
N3 Zn4 N6 125.80(16) . 2
N3 Zn4 N10 111.30(17) . .
N6 Zn4 N10 121.98(16) 2 .
N3 Zn4 O2W 92.08(16) . .
N6 Zn4 O2W 91.41(17) 2 .
N10 Zn4 O2W 96.39(16) . .
N3 Zn4 O5 85.99(14) . .
N6 Zn4 O5 86.89(17) 2 .
N10 Zn4 O5 87.59(17) . .
O2W Zn4 O5 175.99(17) . .
O6 S1 O7 116.2(6) . .
O6 S1 O5 110.3(5) . .
O7 S1 O5 109.5(4) . .
O6 S1 C14 107.1(3) . .
O7 S1 C14 108.1(3) . .
O5 S1 C14 104.9(2) . .
C9 O1 Zn3 103.7(3) . .
C9 O2 Zn1 149.6(3) . .
C16 O3 Zn3 123.9(3) 3_565 .
S1 O5 Zn4 169.7(3) . .
C2 N1 N2 105.7(3) . .
C2 N1 Zn3 139.1(3) . .
N2 N1 Zn3 114.9(3) . .
C1 N2 N1 106.5(3) . .
C1 N2 Zn1 123.0(3) . .
N1 N2 Zn1 127.9(3) . .
C1 N3 C2 102.1(4) . .
C1 N3 Zn4 125.5(3) . .
C2 N3 Zn4 132.4(3) . .
C3 N4 N5 106.1(4) . .
C3 N4 Zn1 133.5(3) . .
N5 N4 Zn1 120.2(3) . .
C4 N5 N4 105.7(4) . .
C4 N5 Zn2 132.0(3) . .
N4 N5 Zn2 122.3(3) . .
C3 N6 C4 102.1(4) . .
C3 N6 Zn4 127.4(3) . 2_545
C4 N6 Zn4 130.3(3) . 2_545
C5 N7 N8 107.0(3) . .
C5 N7 Zn1 133.9(3) . .
N8 N7 Zn1 118.9(3) . .
C6 N8 N7 105.6(3) . .
C6 N8 Zn2 126.9(3) . .
N7 N8 Zn2 127.3(3) . .
C6 N9 C5 102.7(4) . .
C6 N9 Zn3 125.1(3) . 2_445
C5 N9 Zn3 131.3(3) . 2_445
C7 N10 C8 102.3(4) . .
C7 N10 Zn4 129.9(3) . .
C8 N10 Zn4 127.6(3) . .
C7 N11 N12 105.7(4) . .
C7 N11 Zn1 133.8(3) . 3_565
N12 N11 Zn1 120.3(3) . 3_565
C8 N12 N11 106.4(4) . .
C8 N12 Zn2 130.2(3) . 1_565
N11 N12 Zn2 123.2(3) . 1_565
N2 C1 N3 112.5(4) . .
N1 C2 N3 113.2(4) . .
N4 C3 N6 112.7(4) . .
N5 C4 N6 113.4(4) . .
N7 C5 N9 111.7(4) . .
N8 C6 N9 113.0(4) . .
N11 C7 N10 112.9(4) . .
N12 C8 N10 112.7(4) . .
O2 C9 O1 123.0(5) . .
O2 C9 C10 120.3(4) . .
O1 C9 C10 116.6(4) . .
O2 C9 Zn3 75.2(3) . .
O1 C9 Zn3 47.9(2) . .
C10 C9 Zn3 164.0(4) . .
C11 C10 C15 119.5(4) . 2_545
C11 C10 C9 118.9(4) . .
C15 C10 C9 121.4(4) 2_545 .
C12 C11 C10 121.0(4) 2_545 .
C11 C12 C13 119.3(5) 2 .
C11 C12 C16 119.9(4) 2 .
C13 C12 C16 120.6(4) . .
C14 C13 C12 120.1(5) . .
C13 C14 C15 120.2(4) . .
C13 C14 S1 120.5(4) . .
C15 C14 S1 118.9(4) . .
C14 C15 C10 119.9(4) . 2
O4 C16 O3 124.4(5) . 3_565
O4 C16 C12 120.0(5) . .
O3 C16 C12 115.6(4) 3_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N7 1.986(4) .
Zn1 N2 1.990(4) .
Zn1 N4 2.021(4) .
Zn1 N11 2.122(4) 3_565
Zn1 O2 2.339(3) .
Zn2 N8 2.113(4) .
Zn2 N8 2.113(4) 3
Zn2 N12 2.126(4) 1_545
Zn2 N12 2.126(4) 3_565
Zn2 N5 2.265(4) 3
Zn2 N5 2.265(4) .
Zn3 O1 1.970(4) .
Zn3 O3 1.979(3) .
Zn3 N9 1.993(4) 2_455
Zn3 N1 2.139(4) .
Zn3 O1W 2.204(4) .
Zn3 C9 2.578(5) .
Zn4 N3 1.993(4) .
Zn4 N6 2.000(4) 2
Zn4 N10 2.003(4) .
Zn4 O2W 2.099(4) .
Zn4 O5 2.290(4) .
S1 O6 1.376(6) .
S1 O7 1.389(6) .
S1 O5 1.389(4) .
S1 C14 1.762(5) .
O1 C9 1.259(6) .
O2 C9 1.247(6) .
O3 C16 1.258(6) 3_565
O4 C16 1.239(6) .
N1 C2 1.297(6) .
N1 N2 1.365(5) .
N2 C1 1.308(6) .
N3 C1 1.336(6) .
N3 C2 1.346(6) .
N4 C3 1.309(6) .
N4 N5 1.368(5) .
N5 C4 1.294(6) .
N6 C3 1.333(6) .
N6 C4 1.342(6) .
N6 Zn4 2.000(4) 2_545
N7 C5 1.307(5) .
N7 N8 1.364(5) .
N8 C6 1.301(5) .
N9 C6 1.340(6) .
N9 C5 1.344(6) .
N9 Zn3 1.993(4) 2_445
N10 C7 1.336(6) .
N10 C8 1.342(6) .
N11 C7 1.302(6) .
N11 N12 1.367(5) .
N11 Zn1 2.122(4) 3_565
N12 C8 1.294(6) .
N12 Zn2 2.126(4) 1_565
C9 C10 1.480(7) .
C10 C11 1.374(7) .
C10 C15 1.383(6) 2_545
C11 C12 1.375(7) 2_545
C12 C11 1.375(7) 2
C12 C13 1.385(7) .
C12 C16 1.487(7) .
C13 C14 1.373(7) .
C14 C15 1.378(7) .
C15 C10 1.383(6) 2
C16 O3 1.258(6) 3_565
