#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/38/1513864.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_1513864
loop_
_publ_author_name
'Shen, Ping'
'He, Wen-Wen'
'Du, Dong-Ying'
'Jiang, Hai-Long'
'Li, Shun-Li'
'Lang, Zhong-Ling'
'Su, Zhong-Min'
'Fu, Qiang'
'Lan, Ya-Qian'
_publ_section_title
;
 Solid-state structural transformation doubly triggered by reaction
 temperature and time in 3D metal-organic frameworks: great enhancement of
 stability and gas adsorption
;
_journal_issue                   4
_journal_name_full               'Chemical Science'
_journal_page_first              1368
_journal_paper_doi               10.1039/c3sc52666f
_journal_volume                  5
_journal_year                    2014
_chemical_formula_sum            'C49.5 H36 N0 O19 Zn4'
_chemical_formula_weight         1196.26
_chemical_name_systematic
;
?
;
_space_group_IT_number           167
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   26.669(3)
_cell_length_b                   26.669(3)
_cell_length_c                   86.622(4)
_cell_measurement_temperature    293(2)
_cell_volume                     53355(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1222
_diffrn_reflns_av_sigmaI/netI    0.1243
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       102
_diffrn_reflns_limit_l_min       -91
_diffrn_reflns_number            86379
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    0.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7260
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.177
_refine_diff_density_rms         0.026
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.700
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         10440
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.700
_refine_ls_R_factor_all          0.1675
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0422P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0941
_reflns_number_gt                3636
_reflns_number_total             10440
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc52666f.txt
_cod_data_source_block           mm
_cod_original_formula_sum        'C49.50 H36 N0 O19 Zn4'
_cod_database_code               1513864
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'
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
O7 O 0.3333 0.6667 0.50668(3) 0.0819(9) Uani 1 3 d S
O5 O 0.31741(9) 0.37293(9) 0.56540(2) 0.1050(7) Uani 1 1 d .
O2 O 0.33200(10) 0.59867(11) 0.53763(3) 0.1222(8) Uani 1 1 d .
C2 C 0.31893(15) 0.50529(19) 0.54008(4) 0.1070(11) Uani 1 1 d .
C5 C 0.31841(14) 0.41770(18) 0.55808(4) 0.0962(10) Uani 1 1 d .
C15 C 0.10683(18) 0.5120(2) 0.45101(4) 0.1515(16) Uani 1 1 d .
H15 H 0.0822 0.5224 0.4462 0.182 Uiso 1 1 calc R
C11 C 0.18028(18) 0.53060(19) 0.46953(4) 0.1227(12) Uani 1 1 d .
C12 C 0.17837(16) 0.4789(2) 0.46493(4) 0.1252(12) Uani 1 1 d .
H12 H 0.2025 0.4677 0.4696 0.150 Uiso 1 1 calc R
C7 C 0.33518(15) 0.51492(15) 0.55555(4) 0.1213(12) Uani 1 1 d .
H7 H 0.3457 0.5505 0.5600 0.146 Uiso 1 1 calc R
C14 C 0.10540(17) 0.4611(2) 0.44676(4) 0.1160(12) Uani 1 1 d .
C6 C 0.33568(15) 0.4716(2) 0.56425(3) 0.1140(11) Uani 1 1 d .
H6 H 0.3479 0.4791 0.5745 0.137 Uiso 1 1 calc R
C13 C 0.14087(19) 0.44512(15) 0.45350(4) 0.1248(13) Uani 1 1 d .
H13 H 0.1400 0.4113 0.4504 0.150 Uiso 1 1 calc R
C16 C 0.14422(19) 0.54693(16) 0.46220(5) 0.1464(15) Uani 1 1 d .
H16 H 0.1455 0.5813 0.4649 0.176 Uiso 1 1 calc R
C3 C 0.30127(16) 0.4520(2) 0.53411(4) 0.1372(15) Uani 1 1 d .
H3 H 0.2903 0.4451 0.5238 0.165 Uiso 1 1 calc R
C4 C 0.29900(15) 0.40813(15) 0.54274(4) 0.1332(14) Uani 1 1 d .
H4 H 0.2844 0.3715 0.5384 0.160 Uiso 1 1 calc R
C1 C 0.31947(17) 0.55263(18) 0.53081(5) 0.1300(15) Uani 1 1 d .
O3 O 0.38755(12) 0.60967(13) 0.48524(3) 0.1517(10) Uani 1 1 d .
C10 C 0.22257(19) 0.5682(2) 0.48122(4) 0.1197(13) Uani 1 1 d .
O6 O 0.06695(10) 0.43110(11) 0.43523(2) 0.1177(7) Uani 1 1 d .
O4 O 0.25617(10) 0.55246(10) 0.48678(2) 0.1241(9) Uani 1 1 d .
O1 O 0.31344(11) 0.54333(10) 0.51634(3) 0.1488(10) Uani 1 1 d .
Zn1 Zn 0.3333 0.6667 0.529185(5) 0.0849(2) Uani 1 3 d S
Zn2 Zn 0.325064(14) 0.594246(15) 0.499366(3) 0.08797(15) Uani 1 1 d .
C9 C 0.35569(16) 0.3333 0.5833 0.0804(12) Uani 1 2 d S
C8 C 0.35011(12) 0.38605(12) 0.57925(3) 0.0919(9) Uani 1 1 d .
H8A H 0.3306 0.3942 0.5875 0.110 Uiso 1 1 calc R
H8B H 0.3881 0.4198 0.5778 0.110 Uiso 1 1 calc R
C17 C 0.06412(12) 0.37883(14) 0.43056(3) 0.0955(10) Uani 1 1 d .
H17A H 0.0498 0.3509 0.4389 0.115 Uiso 1 1 calc R
H17B H 0.1022 0.3859 0.4276 0.115 Uiso 1 1 calc R
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'
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
Zn2 O7 Zn2 109.85(6) 3_565 2_665
Zn2 O7 Zn2 109.85(6) 3_565 .
Zn2 O7 Zn2 109.85(6) 2_665 .
Zn2 O7 Zn1 109.09(6) 3_565 .
Zn2 O7 Zn1 109.09(6) 2_665 .
Zn2 O7 Zn1 109.09(6) . .
C5 O5 C8 116.4(3) . .
C1 O2 Zn1 127.7(3) . .
C3 C2 C7 118.3(3) . .
C3 C2 C1 122.2(4) . .
C7 C2 C1 119.5(4) . .
O5 C5 C6 126.4(3) . .
O5 C5 C4 116.4(4) . .
C6 C5 C4 117.2(3) . .
C16 C15 C14 120.5(4) . .
C16 C15 H15 119.7 . .
C14 C15 H15 119.7 . .
C16 C11 C12 118.9(3) . .
C16 C11 C10 120.9(4) . .
C12 C11 C10 120.0(5) . .
C13 C12 C11 120.2(4) . .
C13 C12 H12 119.9 . .
C11 C12 H12 119.9 . .
C6 C7 C2 120.1(3) . .
C6 C7 H7 119.9 . .
C2 C7 H7 119.9 . .
C13 C14 O6 124.8(4) . .
C13 C14 C15 120.9(4) . .
O6 C14 C15 114.3(4) . .
C5 C6 C7 121.4(3) . .
C5 C6 H6 119.3 . .
C7 C6 H6 119.3 . .
C14 C13 C12 120.0(4) . .
C14 C13 H13 120.0 . .
C12 C13 H13 120.0 . .
C15 C16 C11 119.5(4) . .
C15 C16 H16 120.3 . .
C11 C16 H16 120.3 . .
C2 C3 C4 122.2(3) . .
C2 C3 H3 118.9 . .
C4 C3 H3 118.9 . .
C3 C4 C5 120.6(3) . .
C3 C4 H4 119.7 . .
C5 C4 H4 119.7 . .
O2 C1 O1 127.1(4) . .
O2 C1 C2 117.6(4) . .
O1 C1 C2 114.8(4) . .
C10 O3 Zn2 133.4(3) 2_665 .
O3 C10 O4 124.0(4) 3_565 .
O3 C10 C11 118.3(4) 3_565 .
O4 C10 C11 117.7(4) . .
C14 O6 C17 116.0(3) . .
C10 O4 Zn2 130.6(3) . .
C1 O1 Zn2 131.1(3) . .
O2 Zn1 O2 106.65(8) 3_565 2_665
O2 Zn1 O2 106.65(8) 3_565 .
O2 Zn1 O2 106.65(8) 2_665 .
O2 Zn1 O7 112.17(7) 3_565 .
O2 Zn1 O7 112.17(7) 2_665 .
O2 Zn1 O7 112.17(7) . .
O1 Zn2 O3 116.84(12) . .
O1 Zn2 O7 110.63(10) . .
O3 Zn2 O7 109.73(10) . .
O1 Zn2 O4 104.65(10) . .
O3 Zn2 O4 103.54(11) . .
O7 Zn2 O4 111.08(9) . .
C8 C9 C8 112.2(3) 16 .
C8 C9 C17 110.75(14) 16 35
C8 C9 C17 105.73(16) . 35
C8 C9 C17 105.72(17) 16 20_556
C8 C9 C17 110.74(14) . 20_556
C17 C9 C17 111.8(3) 35 20_556
O5 C8 C9 107.4(2) . .
O5 C8 H8A 110.2 . .
C9 C8 H8A 110.2 . .
O5 C8 H8B 110.2 . .
C9 C8 H8B 110.2 . .
H8A C8 H8B 108.5 . .
O6 C17 C9 106.8(2) . 21_556
O6 C17 H17A 110.4 . .
C9 C17 H17A 110.4 21_556 .
O6 C17 H17B 110.4 . .
C9 C17 H17B 110.4 21_556 .
H17A C17 H17B 108.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O7 Zn2 1.9377(8) 3_565
O7 Zn2 1.9377(8) 2_665
O7 Zn2 1.9377(8) .
O7 Zn1 1.949(2) .
O5 C5 1.340(3) .
O5 C8 1.420(3) .
O2 C1 1.248(4) .
O2 Zn1 1.939(2) .
C2 C3 1.357(4) .
C2 C7 1.392(4) .
C2 C1 1.490(5) .
C5 C6 1.380(4) .
C5 C4 1.402(4) .
C15 C16 1.369(4) .
C15 C14 1.389(4) .
C15 H15 0.9300 .
C11 C16 1.391(4) .
C11 C12 1.411(4) .
C11 C10 1.474(5) .
C12 C13 1.376(4) .
C12 H12 0.9300 .
C7 C6 1.384(4) .
C7 H7 0.9300 .
C14 C13 1.348(4) .
C14 O6 1.367(4) .
C6 H6 0.9300 .
C13 H13 0.9300 .
C16 H16 0.9300 .
C3 C4 1.364(4) .
C3 H3 0.9300 .
C4 H4 0.9300 .
C1 O1 1.272(4) .
O3 C10 1.236(4) 2_665
O3 Zn2 1.938(2) .
C10 O3 1.236(4) 3_565
C10 O4 1.260(4) .
O6 C17 1.417(3) .
O4 Zn2 1.939(2) .
O1 Zn2 1.919(2) .
Zn1 O2 1.939(2) 3_565
Zn1 O2 1.939(2) 2_665
C9 C8 1.527(3) 16
C9 C8 1.527(3) .
C9 C17 1.544(3) 35
C9 C17 1.544(3) 20_556
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C17 C9 1.544(3) 21_556
C17 H17A 0.9700 .
C17 H17B 0.9700 .
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
C8 O5 C5 C6 -16.8(4) . .
C8 O5 C5 C4 164.4(3) . .
C16 C11 C12 C13 -0.7(6) . .
C10 C11 C12 C13 -176.9(3) . .
C3 C2 C7 C6 3.0(5) . .
C1 C2 C7 C6 -179.1(3) . .
C16 C15 C14 C13 -0.3(6) . .
C16 C15 C14 O6 -178.7(3) . .
O5 C5 C6 C7 179.7(3) . .
C4 C5 C6 C7 -1.5(5) . .
C2 C7 C6 C5 -2.2(5) . .
O6 C14 C13 C12 179.4(3) . .
C15 C14 C13 C12 1.2(6) . .
C11 C12 C13 C14 -0.7(6) . .
C14 C15 C16 C11 -1.1(6) . .
C12 C11 C16 C15 1.6(6) . .
C10 C11 C16 C15 177.7(4) . .
C7 C2 C3 C4 0.0(6) . .
C1 C2 C3 C4 -177.8(4) . .
C2 C3 C4 C5 -3.9(6) . .
O5 C5 C4 C3 -176.5(3) . .
C6 C5 C4 C3 4.5(5) . .
Zn1 O2 C1 O1 11.7(7) . .
Zn1 O2 C1 C2 -177.2(2) . .
C3 C2 C1 O2 174.4(4) . .
C7 C2 C1 O2 -3.4(6) . .
C3 C2 C1 O1 -13.4(6) . .
C7 C2 C1 O1 168.8(3) . .
C16 C11 C10 O3 5.6(6) . 3_565
C12 C11 C10 O3 -178.3(4) . 3_565
C16 C11 C10 O4 -176.0(4) . .
C12 C11 C10 O4 0.1(5) . .
C13 C14 O6 C17 1.7(5) . .
C15 C14 O6 C17 -180.0(3) . .
O3 C10 O4 Zn2 -13.7(6) 3_565 .
C11 C10 O4 Zn2 168.1(2) . .
O2 C1 O1 Zn2 4.3(7) . .
C2 C1 O1 Zn2 -167.0(2) . .
C1 O2 Zn1 O2 107.2(4) . 3_565
C1 O2 Zn1 O2 -139.1(4) . 2_665
C1 O2 Zn1 O7 -16.0(4) . .
Zn2 O7 Zn1 O2 5.01(8) 3_565 3_565
Zn2 O7 Zn1 O2 125.01(8) 2_665 3_565
Zn2 O7 Zn1 O2 -114.99(8) . 3_565
Zn2 O7 Zn1 O2 -114.99(8) 3_565 2_665
Zn2 O7 Zn1 O2 5.01(8) 2_665 2_665
Zn2 O7 Zn1 O2 125.01(8) . 2_665
Zn2 O7 Zn1 O2 125.01(8) 3_565 .
Zn2 O7 Zn1 O2 -114.99(8) 2_665 .
Zn2 O7 Zn1 O2 5.01(8) . .
C1 O1 Zn2 O3 113.9(4) . .
C1 O1 Zn2 O7 -12.6(4) . .
C1 O1 Zn2 O4 -132.3(3) . .
C10 O3 Zn2 O1 -120.3(4) 2_665 .
C10 O3 Zn2 O7 6.7(4) 2_665 .
C10 O3 Zn2 O4 125.3(4) 2_665 .
Zn2 O7 Zn2 O1 -115.01(12) 3_565 .
Zn2 O7 Zn2 O1 124.05(11) 2_665 .
Zn1 O7 Zn2 O1 4.52(8) . .
Zn2 O7 Zn2 O3 114.64(11) 3_565 .
Zn2 O7 Zn2 O3 -6.30(13) 2_665 .
Zn1 O7 Zn2 O3 -125.83(9) . .
Zn2 O7 Zn2 O4 0.76(12) 3_565 .
Zn2 O7 Zn2 O4 -120.18(9) 2_665 .
Zn1 O7 Zn2 O4 120.29(7) . .
C10 O4 Zn2 O1 130.2(3) . .
C10 O4 Zn2 O3 -106.9(3) . .
C10 O4 Zn2 O7 10.8(3) . .
C5 O5 C8 C9 -165.8(2) . .
C8 C9 C8 O5 -65.84(17) 16 .
C17 C9 C8 O5 173.3(2) 35 .
C17 C9 C8 O5 52.0(3) 20_556 .
C14 O6 C17 C9 -175.2(3) . 21_556
