#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:10:53 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179470 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/67/4336742.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_4336742
loop_
_publ_author_name
'Suresh Sanda'
'Srinivasulu Parshamoni'
'Sanjit Konar'
_publ_section_title
;
 Third-Generation Breathing Metal-Organic Framework with Selective,
 Stepwise, Reversible, and Hysteretic Adsorption Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12866
_journal_page_last               12868
_journal_paper_doi               10.1021/ic402095u
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C15 H9 N2 O4 S2 Zn, 5(O)'
_chemical_formula_sum            'C15 H9 N2 O9 S2 Zn'
_chemical_formula_weight         490.77
_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                92.538(10)
_cell_angle_beta                 107.026(9)
_cell_angle_gamma                104.393(9)
_cell_formula_units_Z            2
_cell_length_a                   9.042(2)
_cell_length_b                   10.886(3)
_cell_length_c                   11.504(3)
_cell_measurement_reflns_used    7398
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      33.79
_cell_measurement_theta_min      2.45
_cell_volume                     1040.3(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0072
_diffrn_reflns_av_sigmaI/netI    0.0076
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9502
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    1.429
_exptl_absorpt_correction_T_max  0.690
_exptl_absorpt_correction_T_min  0.554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       block
_exptl_crystal_F_000             494
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.807
_refine_diff_density_min         -1.467
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.430
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.430
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.090
_refine_ls_shift/su_mean         0.029
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.1510
_reflns_number_gt                4593
_reflns_number_total             4751
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402095u_si_001.cif
_cod_data_source_block           compound_1
_cod_database_code               4336742
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
Zn1 Zn 0.66362(2) 0.663637(18) 0.110923(17) 0.01505(13) Uani 1 1 d .
S3 S 0.93649(6) 0.18938(4) 0.50169(4) 0.01749(15) Uani 1 1 d .
S4 S 1.09344(5) 0.32394(4) 0.44648(4) 0.01792(15) Uani 1 1 d .
O1 O 0.73030(16) 0.71362(13) -0.03015(13) 0.0183(3) Uani 1 1 d .
O2 O 0.7346(2) 0.65095(16) -0.21580(14) 0.0256(3) Uani 1 1 d .
O3 O 0.43783(16) 0.57072(15) 0.07643(14) 0.0205(3) Uani 1 1 d .
O5 O 0.37798(18) 0.75512(16) 0.09642(18) 0.0305(4) Uani 1 1 d .
N1 N 0.79001(18) 0.55399(15) 0.21224(14) 0.0145(3) Uani 1 1 d .
N3 N 0.74911(18) -0.16784(16) 0.22308(15) 0.0170(3) Uani 1 1 d .
C7 C 0.1643(2) 0.56333(17) 0.03857(16) 0.0148(3) Uani 1 1 d .
C8 C 1.0453(2) 0.52531(18) 0.32620(16) 0.0151(3) Uani 1 1 d .
H8 H 1.1568 0.5561 0.3543 0.018 Uiso 1 1 calc R
C10 C 0.8684(2) 0.05664(17) 0.38719(17) 0.0153(3) Uani 1 1 d .
C15 C 0.1153(2) 0.43351(17) 0.04836(16) 0.0139(3) Uani 1 1 d .
C16 C 0.9518(2) 0.59476(18) 0.25510(16) 0.0154(3) Uani 1 1 d .
H16 H 1.0031 0.6729 0.2362 0.018 Uiso 1 1 calc R
C18 C 0.9680(2) 0.40775(17) 0.35472(17) 0.0150(3) Uani 1 1 d .
C20 C 0.3398(2) 0.63763(19) 0.07447(16) 0.0170(3) Uani 1 1 d .
C22 C 0.7156(2) 0.4402(2) 0.23945(19) 0.0196(4) Uani 1 1 d .
H22 H 0.6039 0.4117 0.2100 0.023 Uiso 1 1 calc R
C26 C 0.7445(2) -0.04448(19) 0.39956(17) 0.0181(4) Uani 1 1 d .
H26 H 0.7002 -0.0376 0.4622 0.022 Uiso 1 1 calc R
C27 C 0.7722(2) 0.64650(18) -0.10303(17) 0.0149(3) Uani 1 1 d .
C30 C 0.0493(2) 0.62912(18) -0.00993(16) 0.0152(3) Uani 1 1 d .
H30 H 0.0830 0.7157 -0.0166 0.018 Uiso 1 1 calc R
C31 C 0.8001(2) 0.3640(2) 0.30993(19) 0.0209(4) Uani 1 1 d .
H31 H 0.7460 0.2858 0.3268 0.025 Uiso 1 1 calc R
C35 C 0.8666(2) -0.07013(19) 0.21082(18) 0.0196(4) Uani 1 1 d .
H35 H 0.9073 -0.0793 0.1464 0.024 Uiso 1 1 calc R
C38 C 0.9298(2) 0.04368(19) 0.29007(18) 0.0196(4) Uani 1 1 d .
H38 H 1.0105 0.1094 0.2789 0.023 Uiso 1 1 calc R
C39 C 0.6899(2) -0.1545(2) 0.31640(18) 0.0191(4) Uani 1 1 d .
H39 H 0.6092 -0.2218 0.3253 0.023 Uiso 1 1 calc R
O9 O 0.7484(3) 0.1218(2) 0.7441(2) 0.0418(4) Uani 1 1 d .
O10 O 0.5839(3) 0.2257(4) 0.5424(3) 0.0722(10) Uani 1 1 d .
O11 O 0.4736(3) 0.5540(4) 0.3911(2) 0.0716(10) Uani 1 1 d .
O16 O 0.3997(5) 0.1471(3) 0.2981(4) 0.0754(9) Uani 1 1 d .
O18 O 0.5279(7) 0.0634(6) 0.0899(7) 0.146(3) 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_1
_geom_angle_site_symmetry_3
O1 Zn1 O3 116.14(6) . .
O1 Zn1 N1 114.01(6) . .
O3 Zn1 N1 105.32(7) . .
O1 Zn1 N3 101.22(6) . 1_565
O3 Zn1 N3 118.11(6) . 1_565
N1 Zn1 N3 101.43(7) . 1_565
C10 S3 S4 105.21(6) . .
C18 S4 S3 103.01(7) . .
C27 O1 Zn1 128.23(12) . .
C20 O3 Zn1 116.83(13) . .
C22 N1 C16 118.55(17) . .
C22 N1 Zn1 121.50(12) . .
C16 N1 Zn1 119.95(13) . .
C39 N3 C35 118.47(18) . .
C39 N3 Zn1 118.73(13) . 1_545
C35 N3 Zn1 122.76(13) . 1_545
C15 C7 C30 120.00(16) . .
C15 C7 C20 122.42(16) . .
C30 C7 C20 117.55(16) . .
C16 C8 C18 118.53(16) . .
C16 C8 H8 120.7 . .
C18 C8 H8 120.7 . .
C38 C10 C26 118.99(17) . .
C38 C10 S3 125.73(14) . .
C26 C10 S3 115.26(13) . .
C7 C15 C30 118.92(16) . 2_565
C7 C15 C27 124.76(15) . 2_665
C30 C15 C27 116.27(16) 2_565 2_665
N1 C16 C8 122.85(17) . .
N1 C16 H16 118.6 . .
C8 C16 H16 118.6 . .
C31 C18 C8 119.10(17) . .
C31 C18 S4 124.42(15) . .
C8 C18 S4 116.47(13) . .
O5 C20 O3 124.90(17) . .
O5 C20 C7 119.59(17) . .
O3 C20 C7 115.48(17) . .
N1 C22 C31 122.41(17) . .
N1 C22 H22 118.8 . .
C31 C22 H22 118.8 . .
C39 C26 C10 118.60(16) . .
C39 C26 H26 120.7 . .
C10 C26 H26 120.7 . .
O2 C27 O1 123.22(17) . .
O2 C27 C15 118.10(16) . 2_665
O1 C27 C15 118.46(16) . 2_665
C7 C30 C15 121.07(17) . 2_565
C7 C30 H30 119.5 . .
C15 C30 H30 119.5 2_565 .
C22 C31 C18 118.55(18) . .
C22 C31 H31 120.7 . .
C18 C31 H31 120.7 . .
N3 C35 C38 123.02(18) . .
N3 C35 H35 118.5 . .
C38 C35 H35 118.5 . .
C35 C38 C10 118.22(17) . .
C35 C38 H38 120.9 . .
C10 C38 H38 120.9 . .
N3 C39 C26 122.70(17) . .
N3 C39 H39 118.6 . .
C26 C39 H39 118.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 1.9445(15) .
Zn1 O3 1.9525(15) .
Zn1 N1 2.0274(17) .
Zn1 N3 2.0320(18) 1_565
S3 C10 1.7653(19) .
S3 S4 2.0347(7) .
S4 C18 1.7695(19) .
O1 C27 1.284(2) .
O2 C27 1.248(2) .
O3 C20 1.276(3) .
O5 C20 1.233(3) .
N1 C22 1.352(2) .
N1 C16 1.348(2) .
N3 C39 1.350(2) .
N3 C35 1.349(2) .
N3 Zn1 2.0320(18) 1_545
C7 C15 1.392(3) .
C7 C30 1.404(2) .
C7 C20 1.514(2) .
C8 C16 1.386(3) .
C8 C18 1.400(2) .
C8 H8 0.9300 .
C10 C38 1.401(2) .
C10 C26 1.408(2) .
C15 C30 1.400(2) 2_565
C15 C27 1.518(2) 2_665
C16 H16 0.9300 .
C18 C31 1.400(3) .
C22 C31 1.393(3) .
C22 H22 0.9300 .
C26 C39 1.386(3) .
C26 H26 0.9300 .
C27 C15 1.518(2) 2_665
C30 C15 1.400(2) 2_565
C30 H30 0.9300 .
C31 H31 0.9300 .
C35 C38 1.391(3) .
C35 H35 0.9300 .
C38 H38 0.9300 .
C39 H39 0.9300 .
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_1
_geom_torsion_site_symmetry_4
C10 S3 S4 C18 89.13(9) . .
O3 Zn1 O1 C27 -83.53(16) . .
N1 Zn1 O1 C27 39.21(17) . .
N3 Zn1 O1 C27 147.24(15) 1_565 .
O1 Zn1 O3 C20 -88.90(15) . .
N1 Zn1 O3 C20 143.91(14) . .
N3 Zn1 O3 C20 31.62(16) 1_565 .
O1 Zn1 N1 C22 -126.68(15) . .
O3 Zn1 N1 C22 1.79(17) . .
N3 Zn1 N1 C22 125.42(15) 1_565 .
O1 Zn1 N1 C16 53.99(15) . .
O3 Zn1 N1 C16 -177.54(14) . .
N3 Zn1 N1 C16 -53.91(15) 1_565 .
S4 S3 C10 C38 8.23(19) . .
S4 S3 C10 C26 -173.56(13) . .
C30 C7 C15 C30 -0.4(3) . 2_565
C20 C7 C15 C30 -178.18(16) . 2_565
C30 C7 C15 C27 -177.84(16) . 2_665
C20 C7 C15 C27 4.4(3) . 2_665
C22 N1 C16 C8 -0.2(3) . .
Zn1 N1 C16 C8 179.12(14) . .
C18 C8 C16 N1 0.0(3) . .
C16 C8 C18 C31 0.5(3) . .
C16 C8 C18 S4 -179.64(14) . .
S3 S4 C18 C31 -14.60(18) . .
S3 S4 C18 C8 165.55(13) . .
Zn1 O3 C20 O5 -2.4(3) . .
Zn1 O3 C20 C7 175.79(11) . .
C15 C7 C20 O5 -160.13(18) . .
C30 C7 C20 O5 22.0(3) . .
C15 C7 C20 O3 21.6(2) . .
C30 C7 C20 O3 -156.30(17) . .
C16 N1 C22 C31 0.0(3) . .
Zn1 N1 C22 C31 -179.34(16) . .
C38 C10 C26 C39 1.3(3) . .
S3 C10 C26 C39 -177.03(15) . .
Zn1 O1 C27 O2 141.38(16) . .
Zn1 O1 C27 C15 -44.1(2) . 2_665
C15 C7 C30 C15 0.4(3) . 2_565
C20 C7 C30 C15 178.30(16) . 2_565
N1 C22 C31 C18 0.5(3) . .
C8 C18 C31 C22 -0.7(3) . .
S4 C18 C31 C22 179.44(16) . .
C39 N3 C35 C38 0.1(3) . .
Zn1 N3 C35 C38 -177.55(15) 1_545 .
N3 C35 C38 C10 0.3(3) . .
C26 C10 C38 C35 -1.0(3) . .
S3 C10 C38 C35 177.18(15) . .
C35 N3 C39 C26 0.2(3) . .
Zn1 N3 C39 C26 178.01(15) 1_545 .
C10 C26 C39 N3 -1.0(3) . .
