#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/52/7205274.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_7205274
loop_
_publ_author_name
'Zhao, Li-Min'
'Zhang, Zhen-Jie'
'Zhang, Shi-Yuan'
'Cui, Ping'
'Shi, Wei'
'Zhao, Bin'
'Cheng, Peng'
'Liao, Dai-Zheng'
'Yan, Shi-Ping'
_publ_section_title
;
 Metal--organic frameworks based on transition-metal carboxylate
 clusters as secondary building units: synthesis, structures and
 properties
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              907
_journal_paper_doi               10.1039/c0ce00315h
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C28 H19 N8 O11 S Zn1.5'
_chemical_formula_weight         773.63
_chemical_name_systematic
;
?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/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                90.00
_cell_angle_beta                 130.288(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.181(3)
_cell_length_b                   9.5978(11)
_cell_length_c                   24.677(3)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.38
_cell_volume                     3104.0(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0768
_diffrn_reflns_av_sigmaI/netI    0.1218
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            12517
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    1.311
_exptl_absorpt_correction_T_max  0.7795
_exptl_absorpt_correction_T_min  0.7353
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.571
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         5383
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1290
_refine_ls_R_factor_gt           0.0762
_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)+(0.1051P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.1950
_reflns_number_gt                3309
_reflns_number_total             5383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CE00315H.TXT
_cod_data_source_block           p090718z
_cod_original_cell_volume        3104.0(8)
_cod_original_sg_symbol_H-M      P2/c
_cod_original_formula_sum        'C28 H19 N8 O11 S Zn1.50'
_cod_database_code               7205274
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
O7 O 0.0956(4) 0.8555(6) -0.0058(2) 0.0244(13) Uani 1 1 d . . .
Zn1 Zn 0.45750(6) 0.30619(9) 0.32971(4) 0.0166(3) Uani 1 1 d . . .
Zn2 Zn 1.0000 0.0000 1.0000 0.0224(3) Uani 1 2 d S . .
C1 C 0.9038(5) -0.0090(9) 0.8479(4) 0.0212(18) Uani 1 1 d . . .
H1 H 0.9201 -0.1029 0.8585 0.025 Uiso 1 1 calc R . .
C2 C 0.8435(6) 0.0317(8) 0.7775(4) 0.0208(18) Uani 1 1 d . . .
H2 H 0.8184 -0.0326 0.7414 0.025 Uiso 1 1 calc R . .
C3 C 0.8222(5) 0.1726(8) 0.7633(3) 0.0179(17) Uani 1 1 d . . .
C4 C 0.8638(5) 0.2656(9) 0.8179(4) 0.0212(18) Uani 1 1 d . . .
H4 H 0.8528 0.3609 0.8091 0.025 Uiso 1 1 calc R . .
C5 C 0.9229(6) 0.2140(8) 0.8871(4) 0.0215(18) Uani 1 1 d . . .
H5 H 0.9516 0.2762 0.9246 0.026 Uiso 1 1 calc R . .
C6 C 0.6450(5) 0.1916(9) 0.5758(4) 0.0181(17) Uani 1 1 d . . .
C7 C 0.6277(5) 0.3303(8) 0.5567(4) 0.0210(18) Uani 1 1 d . . .
H7 H 0.6519 0.4004 0.5902 0.025 Uiso 1 1 calc R . .
C8 C 0.5727(6) 0.3609(8) 0.4856(4) 0.0213(18) Uani 1 1 d . . .
H8 H 0.5607 0.4540 0.4718 0.026 Uiso 1 1 calc R . .
C9 C 0.5515(6) 0.1319(9) 0.4546(4) 0.0222(18) Uani 1 1 d . . .
H9 H 0.5253 0.0644 0.4196 0.027 Uiso 1 1 calc R . .
C10 C 0.6050(6) 0.0894(9) 0.5243(4) 0.0244(19) Uani 1 1 d . . .
H10 H 0.6138 -0.0046 0.5361 0.029 Uiso 1 1 calc R . .
C11 C 0.4182(5) 0.5699(8) 0.2824(4) 0.0164(17) Uani 1 1 d . . .
C12 C 0.3777(5) 0.6903(8) 0.2311(4) 0.0174(16) Uani 1 1 d . . .
C13 C 0.3096(5) 0.6620(8) 0.1582(4) 0.0162(17) Uani 1 1 d . . .
H13 H 0.2934 0.5708 0.1416 0.019 Uiso 1 1 calc R . .
C14 C 0.2668(5) 0.7729(7) 0.1114(4) 0.0149(16) Uani 1 1 d . . .
C15 C 0.2899(6) 0.9082(8) 0.1350(4) 0.0183(17) Uani 1 1 d . . .
H15 H 0.2619 0.9812 0.1026 0.022 Uiso 1 1 calc R . .
C16 C 0.3556(5) 0.9358(8) 0.2076(4) 0.0179(17) Uani 1 1 d . . .
C17 C 0.3992(5) 0.8266(8) 0.2555(4) 0.0185(17) Uani 1 1 d . . .
H17 H 0.4429 0.8446 0.3041 0.022 Uiso 1 1 calc R . .
C18 C 0.3691(6) 1.0848(8) 0.2301(4) 0.0186(18) Uani 1 1 d . . .
C19 C 0.3077(6) 0.2906(8) 0.3658(4) 0.0266(19) Uani 1 1 d . . .
H19 H 0.3677 0.2707 0.4114 0.032 Uiso 1 1 calc R . .
C20 C 0.2181(7) 0.2932(10) 0.3543(5) 0.039(2) Uani 1 1 d . . .
H20 H 0.2178 0.2767 0.3913 0.047 Uiso 1 1 calc R . .
C21 C 0.1292(7) 0.3206(9) 0.2870(5) 0.037(2) Uani 1 1 d . . .
C22 C 0.1311(6) 0.3470(8) 0.2330(4) 0.032(2) Uani 1 1 d . . .
H22 H 0.0714 0.3669 0.1873 0.038 Uiso 1 1 calc R . .
C23 C 0.2259(6) 0.3429(9) 0.2488(4) 0.027(2) Uani 1 1 d . . .
H23 H 0.2275 0.3600 0.2125 0.032 Uiso 1 1 calc R . .
C24 C 0.1822(7) 0.6419(14) 0.4542(6) 0.057(3) Uani 1 1 d . . .
H24 H 0.2023 0.5582 0.4789 0.069 Uiso 1 1 calc R . .
C25 C 0.1153(7) 0.6368(12) 0.3809(5) 0.043(3) Uani 1 1 d . . .
H25 H 0.0914 0.5516 0.3575 0.052 Uiso 1 1 calc R . .
C26 C 0.0853(7) 0.7558(13) 0.3440(5) 0.045(3) Uani 1 1 d . . .
C27 C 0.1205(9) 0.8858(14) 0.3810(8) 0.066(4) Uani 1 1 d . . .
H27 H 0.1007 0.9715 0.3580 0.079 Uiso 1 1 calc R . .
C28 C 0.1873(10) 0.8729(16) 0.4551(8) 0.072(4) Uani 1 1 d . . .
H28 H 0.2114 0.9550 0.4814 0.087 Uiso 1 1 calc R . .
N1 N 0.5363(5) 0.2642(7) 0.4360(3) 0.0177(14) Uani 1 1 d . . .
N2 N 0.7026(5) 0.1405(7) 0.6472(3) 0.0228(16) Uani 1 1 d . . .
N3 N 0.7611(5) 0.2297(7) 0.6929(3) 0.0225(16) Uani 1 1 d . . .
N4 N 0.9394(4) 0.0780(7) 0.9010(3) 0.0164(14) Uani 1 1 d . . .
N5 N 0.3141(5) 0.3155(7) 0.3141(3) 0.0221(15) Uani 1 1 d . . .
N6 N 0.0366(6) 0.3200(8) 0.2800(3) 0.0396(19) Uani 1 1 d . . .
N7 N 0.2187(7) 0.7564(14) 0.4905(5) 0.064(3) Uani 1 1 d . . .
N8 N 0.0191(10) 0.7524(17) 0.2684(5) 0.148(6) Uani 1 1 d . . .
O1 O 0.4061(4) 0.4485(5) 0.2568(3) 0.0182(12) Uani 1 1 d . . .
O2 O 0.4587(4) 0.5903(6) 0.3454(3) 0.0262(13) Uani 1 1 d . . .
O3 O 0.4417(4) 1.1130(5) 0.2953(3) 0.0218(12) Uani 1 1 d . . .
O4 O 0.3070(4) 1.1713(5) 0.1846(3) 0.0254(13) Uani 1 1 d . . .
O5 O 0.1271(5) 0.6081(6) 0.0107(3) 0.0427(16) Uani 1 1 d . . .
O6 O 0.2168(4) 0.7533(7) -0.0128(3) 0.0402(16) Uani 1 1 d . . .
O8 O 0.6071(4) 0.3403(5) 0.3614(3) 0.0242(13) Uani 1 1 d . . .
O9 O 0.8856(4) -0.1599(6) 0.9466(3) 0.0269(13) Uani 1 1 d . . .
O10 O 0.5803(5) 0.7700(7) 0.4629(3) 0.0452(17) Uani 1 1 d . . .
O11 O 0.9194(5) 0.5736(8) 0.9214(4) 0.063(2) Uani 1 1 d . . .
S1 S 0.16933(15) 0.7449(2) 0.01807(10) 0.0227(5) 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
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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
_geom_angle_publ_flag
S1 O7 Zn2 156.2(3) . 1_464 ?
O1 Zn1 O3 113.8(2) . 1_545 ?
O1 Zn1 N1 146.9(2) . . ?
O3 Zn1 N1 99.0(2) 1_545 . ?
O1 Zn1 O8 87.21(19) . . ?
O3 Zn1 O8 95.6(2) 1_545 . ?
N1 Zn1 O8 85.5(2) . . ?
O1 Zn1 N5 91.3(2) . . ?
O3 Zn1 N5 97.7(2) 1_545 . ?
N1 Zn1 N5 88.3(2) . . ?
O8 Zn1 N5 166.1(2) . . ?
N4 Zn2 N4 180.0(2) . 3_757 ?
N4 Zn2 O9 91.6(2) . 3_757 ?
N4 Zn2 O9 88.4(2) 3_757 3_757 ?
N4 Zn2 O9 88.4(2) . . ?
N4 Zn2 O9 91.6(2) 3_757 . ?
O9 Zn2 O9 180.0(4) 3_757 . ?
N4 Zn2 O7 91.3(2) . 3_666 ?
N4 Zn2 O7 88.7(2) 3_757 3_666 ?
O9 Zn2 O7 86.3(2) 3_757 3_666 ?
O9 Zn2 O7 93.7(2) . 3_666 ?
N4 Zn2 O7 88.7(2) . 1_646 ?
N4 Zn2 O7 91.3(2) 3_757 1_646 ?
O9 Zn2 O7 93.7(2) 3_757 1_646 ?
O9 Zn2 O7 86.3(2) . 1_646 ?
O7 Zn2 O7 180.0(3) 3_666 1_646 ?
N4 C1 C2 123.8(8) . . ?
N4 C1 H1 118.1 . . ?
C2 C1 H1 118.1 . . ?
C1 C2 C3 117.0(7) . . ?
C1 C2 H2 121.5 . . ?
C3 C2 H2 121.5 . . ?
C4 C3 C2 120.1(7) . . ?
C4 C3 N3 116.7(7) . . ?
C2 C3 N3 123.1(7) . . ?
C3 C4 C5 118.4(7) . . ?
C3 C4 H4 120.8 . . ?
C5 C4 H4 120.8 . . ?
N4 C5 C4 121.8(7) . . ?
N4 C5 H5 119.1 . . ?
C4 C5 H5 119.1 . . ?
C7 C6 C10 120.0(7) . . ?
C7 C6 N2 125.0(7) . . ?
C10 C6 N2 115.0(7) . . ?
C6 C7 C8 117.3(7) . . ?
C6 C7 H7 121.4 . . ?
C8 C7 H7 121.4 . . ?
N1 C8 C7 123.3(8) . . ?
N1 C8 H8 118.4 . . ?
C7 C8 H8 118.4 . . ?
N1 C9 C10 122.6(7) . . ?
N1 C9 H9 118.7 . . ?
C10 C9 H9 118.7 . . ?
C6 C10 C9 117.8(8) . . ?
C6 C10 H10 121.1 . . ?
C9 C10 H10 121.1 . . ?
O2 C11 O1 123.0(7) . . ?
O2 C11 C12 120.7(7) . . ?
O1 C11 C12 116.3(6) . . ?
C17 C12 C13 120.5(7) . . ?
C17 C12 C11 120.6(7) . . ?
C13 C12 C11 118.6(7) . . ?
C14 C13 C12 118.4(7) . . ?
C14 C13 H13 120.8 . . ?
C12 C13 H13 120.8 . . ?
C15 C14 C13 121.5(7) . . ?
C15 C14 S1 117.5(5) . . ?
C13 C14 S1 120.7(6) . . ?
C14 C15 C16 119.8(7) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C17 C16 C15 119.8(7) . . ?
C17 C16 C18 122.6(7) . . ?
C15 C16 C18 117.5(7) . . ?
C16 C17 C12 119.9(7) . . ?
C16 C17 H17 120.0 . . ?
C12 C17 H17 120.0 . . ?
O4 C18 O3 124.6(7) . . ?
O4 C18 C16 117.8(7) . . ?
O3 C18 C16 117.5(7) . . ?
N5 C19 C20 124.0(8) . . ?
N5 C19 H19 118.0 . . ?
C20 C19 H19 118.0 . . ?
C21 C20 C19 118.4(8) . . ?
C21 C20 H20 120.8 . . ?
C19 C20 H20 120.8 . . ?
C20 C21 C22 120.1(8) . . ?
C20 C21 N6 114.3(7) . . ?
C22 C21 N6 125.6(8) . . ?
C21 C22 C23 118.3(8) . . ?
C21 C22 H22 120.9 . . ?
C23 C22 H22 120.9 . . ?
N5 C23 C22 122.9(7) . . ?
N5 C23 H23 118.5 . . ?
C22 C23 H23 118.5 . . ?
N7 C24 C25 123.9(11) . . ?
N7 C24 H24 118.1 . . ?
C25 C24 H24 118.1 . . ?
C26 C25 C24 119.3(11) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
C25 C26 N8 120.1(12) . . ?
C25 C26 C27 119.4(10) . . ?
N8 C26 C27 120.5(12) . . ?
C28 C27 C26 114.1(11) . . ?
C28 C27 H27 122.9 . . ?
C26 C27 H27 122.9 . . ?
N7 C28 C27 125.9(12) . . ?
N7 C28 H28 117.0 . . ?
C27 C28 H28 117.0 . . ?
C9 N1 C8 119.0(6) . . ?
C9 N1 Zn1 116.7(5) . . ?
C8 N1 Zn1 124.3(5) . . ?
N3 N2 C6 112.9(6) . . ?
N2 N3 C3 111.4(6) . . ?
C1 N4 C5 118.6(6) . . ?
C1 N4 Zn2 119.7(5) . . ?
C5 N4 Zn2 121.1(5) . . ?
C23 N5 C19 116.3(7) . . ?
C23 N5 Zn1 118.5(5) . . ?
C19 N5 Zn1 125.2(5) . . ?
N6 N6 C21 109.9(9) 2 . ?
C24 N7 C28 117.3(11) . . ?
N8 N8 C26 172(4) 2 . ?
C11 O1 Zn1 110.4(4) . . ?
C18 O3 Zn1 119.4(5) . 1_565 ?
O6 S1 O7 112.9(3) . . ?
O6 S1 O5 113.2(4) . . ?
O7 S1 O5 112.1(3) . . ?
O6 S1 C14 107.2(3) . . ?
O7 S1 C14 104.9(3) . . ?
O5 S1 C14 105.9(3) . . ?
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
O7 S1 1.453(5) . ?
O7 Zn2 2.225(5) 1_464 ?
Zn1 O1 1.957(5) . ?
Zn1 O3 1.984(5) 1_545 ?
Zn1 N1 2.070(6) . ?
Zn1 O8 2.174(5) . ?
Zn1 N5 2.235(6) . ?
Zn2 N4 2.080(5) . ?
Zn2 N4 2.080(5) 3_757 ?
Zn2 O9 2.146(5) 3_757 ?
Zn2 O9 2.146(5) . ?
Zn2 O7 2.225(5) 3_666 ?
Zn2 O7 2.225(5) 1_646 ?
C1 N4 1.322(9) . ?
C1 C2 1.385(10) . ?
C1 H1 0.9300 . ?
C2 C3 1.386(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.371(10) . ?
C3 N3 1.434(9) . ?
C4 C5 1.397(10) . ?
C4 H4 0.9300 . ?
C5 N4 1.332(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.379(11) . ?
C6 C10 1.386(11) . ?
C6 N2 1.439(9) . ?
C7 C8 1.383(9) . ?
C7 H7 0.9300 . ?
C8 N1 1.326(9) . ?
C8 H8 0.9300 . ?
C9 N1 1.317(9) . ?
C9 C10 1.387(10) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 O2 1.241(8) . ?
C11 O1 1.277(9) . ?
C11 C12 1.512(10) . ?
C12 C17 1.387(10) . ?
C12 C13 1.399(10) . ?
C13 C14 1.382(10) . ?
C13 H13 0.9300 . ?
C14 C15 1.372(10) . ?
C14 S1 1.787(7) . ?
C15 C16 1.394(9) . ?
C15 H15 0.9300 . ?
C16 C17 1.382(10) . ?
C16 C18 1.497(11) . ?
C17 H17 0.9300 . ?
C18 O4 1.242(9) . ?
C18 O3 1.273(8) . ?
C19 N5 1.370(9) . ?
C19 C20 1.374(11) . ?
C19 H19 0.9300 . ?
C20 C21 1.371(12) . ?
C20 H20 0.9300 . ?
C21 C22 1.379(12) . ?
C21 N6 1.485(11) . ?
C22 C23 1.409(11) . ?
C22 H22 0.9300 . ?
C23 N5 1.343(9) . ?
C23 H23 0.9300 . ?
C24 N7 1.296(14) . ?
C24 C25 1.380(13) . ?
C24 H24 0.9300 . ?
C25 C26 1.339(14) . ?
C25 H25 0.9300 . ?
C26 N8 1.423(13) . ?
C26 C27 1.430(16) . ?
C27 C28 1.400(16) . ?
C27 H27 0.9300 . ?
C28 N7 1.302(16) . ?
C28 H28 0.9300 . ?
N2 N3 1.245(9) . ?
N6 N6 1.168(13) 2 ?
N8 N8 0.698(18) 2 ?
O3 Zn1 1.984(5) 1_565 ?
O5 S1 1.453(6) . ?
O6 S1 1.434(6) . ?
