#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:08:50 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179615 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/79/4507980.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_4507980
loop_
_publ_author_name
'Li, Ting'
'Wang, Feng-Lan'
'Wu, Shu-Ting'
'Huang, Xi-He'
'Chen, Shu-Mei'
'Huang, Chang-Cang'
_publ_section_title
;
 A Highly Chemical and Thermal Stable Porous Metal--Organic Framework with
 Unusual 5-ConnectedzfyTopology
;
_journal_issue                   8
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3271
_journal_paper_doi               10.1021/cg400587j
_journal_volume                  13
_journal_year                    2013
_chemical_formula_moiety         'C31 H25 N4 O6 Zn2'
_chemical_formula_sum            'C31 H25 N4 O6 Zn2'
_chemical_formula_weight         680.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                90.00
_cell_formula_units_Z            16
_cell_length_a                   43.719(6)
_cell_length_b                   43.719(6)
_cell_length_c                   8.5159(17)
_cell_measurement_reflns_used    26490
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.07
_cell_volume                     16277(5)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.893
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotation anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0962
_diffrn_reflns_av_sigmaI/netI    0.1131
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -56
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            26490
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.07
_diffrn_standards_decay_%        None
_diffrn_standards_interval_count None
_diffrn_standards_interval_time  None
_diffrn_standards_number         None
_exptl_absorpt_coefficient_mu    1.216
_exptl_absorpt_correction_T_max  0.9090
_exptl_absorpt_correction_T_min  0.8779
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       light-yellow
_exptl_crystal_F_000             5552
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         8313
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1226
_refine_ls_R_factor_gt           0.0613
_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)+(0.0000P)²+76.6163P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1269
_reflns_number_gt                4961
_reflns_number_total             8313
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg400587j_si_002.cif
_cod_data_source_block           a
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4507980
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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 0.345943(11) 0.197710(11) 0.43989(7) 0.02265(14) Uani 1 1 d .
Zn2 Zn 0.380932(11) 0.175517(11) 0.75533(7) 0.02308(14) Uani 1 1 d .
C1 C 0.35985(14) 0.27606(11) 0.4171(7) 0.0562(19) Uani 1 1 d .
H1A H 0.3463 0.2630 0.3589 0.084 Uiso 1 1 calc R
H1B H 0.3740 0.2857 0.3464 0.084 Uiso 1 1 calc R
H1C H 0.3482 0.2915 0.4708 0.084 Uiso 1 1 calc R
C2 C 0.37716(11) 0.25732(9) 0.5347(6) 0.0292(12) Uani 1 1 d .
C3 C 0.39884(10) 0.26642(10) 0.6424(6) 0.0268(11) Uani 1 1 d .
C4 C 0.40716(11) 0.24032(10) 0.7261(6) 0.0316(12) Uani 1 1 d .
C5 C 0.42994(13) 0.23726(12) 0.8546(8) 0.061(2) Uani 1 1 d .
H5A H 0.4306 0.2164 0.8896 0.091 Uiso 1 1 calc R
H5B H 0.4242 0.2503 0.9406 0.091 Uiso 1 1 calc R
H5C H 0.4498 0.2431 0.8167 0.091 Uiso 1 1 calc R
C6 C 0.38206(15) 0.30388(13) 0.9482(7) 0.064(2) Uani 1 1 d .
H6A H 0.3812 0.3196 1.0268 0.096 Uiso 1 1 calc R
H6B H 0.3903 0.2855 0.9935 0.096 Uiso 1 1 calc R
H6C H 0.3618 0.2999 0.9093 0.096 Uiso 1 1 calc R
C7 C 0.40195(11) 0.31411(10) 0.8167(6) 0.0306(12) Uani 1 1 d .
C8 C 0.40909(11) 0.29797(10) 0.6798(6) 0.0287(11) Uani 1 1 d .
C9 C 0.42725(12) 0.31744(10) 0.5920(6) 0.0329(12) Uani 1 1 d .
C10 C 0.44270(15) 0.31309(12) 0.4373(7) 0.0585(18) Uani 1 1 d .
H10A H 0.4535 0.3314 0.4096 0.088 Uiso 1 1 calc R
H10B H 0.4277 0.3087 0.3584 0.088 Uiso 1 1 calc R
H10C H 0.4569 0.2964 0.4444 0.088 Uiso 1 1 calc R
C11 C 0.31589(10) 0.17221(12) 0.7313(7) 0.0377(14) Uani 1 1 d .
C12 C 0.28518(10) 0.16502(12) 0.7988(7) 0.0382(14) Uani 1 1 d .
C13 C 0.28255(12) 0.15391(14) 0.9486(8) 0.0541(17) Uani 1 1 d .
H13A H 0.3001 0.1503 1.0075 0.065 Uiso 1 1 calc R
C14 C 0.25405(12) 0.14802(14) 1.0135(7) 0.0547(18) Uani 1 1 d .
H14A H 0.2526 0.1404 1.1153 0.066 Uiso 1 1 calc R
C15 C 0.22742(11) 0.15350(14) 0.9255(7) 0.0469(16) Uani 1 1 d .
C16 C 0.23061(12) 0.16484(14) 0.7754(8) 0.0548(18) Uani 1 1 d .
H16A H 0.2132 0.1688 0.7160 0.066 Uiso 1 1 calc R
C17 C 0.25906(11) 0.17051(13) 0.7110(7) 0.0504(17) Uani 1 1 d .
H17A H 0.2607 0.1780 0.6091 0.060 Uiso 1 1 calc R
C18 C 0.10953(10) 0.12918(10) 1.2056(7) 0.0322(13) Uani 1 1 d .
C19 C 0.13974(11) 0.13573(11) 1.1310(7) 0.0359(13) Uani 1 1 d .
C20 C 0.14475(12) 0.13066(13) 0.9734(7) 0.0486(16) Uani 1 1 d .
H20A H 0.1290 0.1231 0.9113 0.058 Uiso 1 1 calc R
C21 C 0.17282(12) 0.13665(15) 0.9068(8) 0.0554(18) Uani 1 1 d .
H21A H 0.1757 0.1332 0.8001 0.066 Uiso 1 1 calc R
C22 C 0.19696(12) 0.14781(14) 0.9959(8) 0.0467(15) Uani 1 1 d .
C23 C 0.19188(12) 0.15304(14) 1.1542(8) 0.0528(17) Uani 1 1 d .
H23A H 0.2077 0.1605 1.2165 0.063 Uiso 1 1 calc R
C24 C 0.16331(11) 0.14732(13) 1.2215(7) 0.0468(15) Uani 1 1 d .
H24A H 0.1601 0.1513 1.3275 0.056 Uiso 1 1 calc R
C25 C 0.33075(12) 0.22098(11) 0.1476(7) 0.0370(14) Uani 1 1 d .
C26 C 0.30741(11) 0.23218(12) 0.0316(7) 0.0393(14) Uani 1 1 d .
C27 C 0.27684(13) 0.23221(17) 0.0709(8) 0.068(2) Uani 1 1 d .
H27A H 0.2710 0.2270 0.1725 0.081 Uiso 1 1 calc R
C28 C 0.25454(13) 0.23982(18) -0.0385(8) 0.076(3) Uani 1 1 d .
H28A H 0.2341 0.2400 -0.0078 0.091 Uiso 1 1 calc R
C29 C 0.26186(11) 0.24702(13) -0.1899(6) 0.0408(14) Uani 1 1 d .
C30 C 0.29289(11) 0.24777(12) -0.2282(7) 0.0405(14) Uani 1 1 d .
H30A H 0.2987 0.2533 -0.3293 0.049 Uiso 1 1 calc R
C31 C 0.31517(11) 0.24050(12) -0.1185(7) 0.0377(13) Uani 1 1 d .
H31A H 0.3357 0.2413 -0.1472 0.045 Uiso 1 1 calc R
N1 N 0.37239(8) 0.22704(8) 0.5498(5) 0.0252(9) Uani 1 1 d .
N2 N 0.39090(8) 0.21652(8) 0.6700(5) 0.0256(9) Uani 1 1 d .
N3 N 0.41507(9) 0.34185(8) 0.8138(5) 0.0272(9) Uani 1 1 d .
N4 N 0.43023(9) 0.34325(8) 0.6743(5) 0.0289(10) Uani 1 1 d .
O1 O 0.31650(7) 0.18102(9) 0.5903(5) 0.0424(10) Uani 1 1 d .
O2 O 0.33897(7) 0.16924(8) 0.8191(5) 0.0405(9) Uani 1 1 d .
O3 O 0.10634(7) 0.13702(8) 1.3456(5) 0.0402(10) Uani 1 1 d .
O4 O 0.08934(7) 0.11702(8) 1.1210(4) 0.0384(9) Uani 1 1 d .
O5 O 0.31998(8) 0.21331(8) 0.2809(5) 0.0445(10) Uani 1 1 d .
O6 O 0.35816(8) 0.21978(8) 0.1105(5) 0.0468(11) Uani 1 1 d .
H4 H 0.4429(13) 0.3599(13) 0.651(7) 0.07(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'
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
O5 Zn1 O4 111.51(16) . 8_443
O5 Zn1 O1 102.01(16) . .
O4 Zn1 O1 101.39(15) 8_443 .
O5 Zn1 N1 117.29(15) . .
O4 Zn1 N1 114.00(15) 8_443 .
O1 Zn1 N1 108.58(16) . .
O2 Zn2 O3 102.85(15) . 8_443
O2 Zn2 N2 116.11(15) . .
O3 Zn2 N2 110.93(16) 8_443 .
O2 Zn2 N3 108.43(16) . 16_657
O3 Zn2 N3 106.90(15) 8_443 16_657
N2 Zn2 N3 110.98(15) . 16_657
C2 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
N1 C2 C3 109.1(4) . .
N1 C2 C1 121.5(4) . .
C3 C2 C1 129.4(4) . .
C2 C3 C4 106.5(4) . .
C2 C3 C8 128.2(4) . .
C4 C3 C8 124.9(4) . .
N2 C4 C3 108.3(4) . .
N2 C4 C5 123.0(4) . .
C3 C4 C5 128.7(4) . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C7 C6 H6A 109.5 . .
C7 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C7 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
N3 C7 C8 110.2(4) . .
N3 C7 C6 122.4(5) . .
C8 C7 C6 127.4(4) . .
C9 C8 C7 105.5(4) . .
C9 C8 C3 129.0(5) . .
C7 C8 C3 125.5(5) . .
N4 C9 C8 107.0(5) . .
N4 C9 C10 121.8(4) . .
C8 C9 C10 131.2(5) . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
O1 C11 O2 125.3(5) . .
O1 C11 C12 116.7(5) . .
O2 C11 C12 118.0(5) . .
C13 C12 C17 119.7(5) . .
C13 C12 C11 120.5(5) . .
C17 C12 C11 119.8(5) . .
C12 C13 C14 120.8(5) . .
C12 C13 H13A 119.6 . .
C14 C13 H13A 119.6 . .
C13 C14 C15 120.0(6) . .
C13 C14 H14A 120.0 . .
C15 C14 H14A 120.0 . .
C16 C15 C14 118.2(5) . .
C16 C15 C22 121.8(5) . .
C14 C15 C22 120.0(5) . .
C15 C16 C17 121.6(5) . .
C15 C16 H16A 119.2 . .
C17 C16 H16A 119.2 . .
C16 C17 C12 119.8(6) . .
C16 C17 H17A 120.1 . .
C12 C17 H17A 120.1 . .
O3 C18 O4 125.8(4) . .
O3 C18 C19 116.9(5) . .
O4 C18 C19 117.3(5) . .
C20 C19 C24 118.9(5) . .
C20 C19 C18 121.6(5) . .
C24 C19 C18 119.5(5) . .
C21 C20 C19 120.8(6) . .
C21 C20 H20A 119.6 . .
C19 C20 H20A 119.6 . .
C20 C21 C22 121.3(6) . .
C20 C21 H21A 119.4 . .
C22 C21 H21A 119.4 . .
C23 C22 C21 117.9(5) . .
C23 C22 C15 120.7(5) . .
C21 C22 C15 121.4(6) . .
C22 C23 C24 120.9(6) . .
C22 C23 H23A 119.6 . .
C24 C23 H23A 119.6 . .
C19 C24 C23 120.2(6) . .
C19 C24 H24A 119.9 . .
C23 C24 H24A 119.9 . .
O6 C25 O5 125.0(5) . .
O6 C25 C26 120.2(5) . .
O5 C25 C26 114.9(5) . .
C31 C26 C27 117.8(5) . .
C31 C26 C25 122.1(5) . .
C27 C26 C25 120.0(6) . .
C26 C27 C28 121.3(6) . .
C26 C27 H27A 119.4 . .
C28 C27 H27A 119.4 . .
C29 C28 C27 121.6(5) . .
C29 C28 H28A 119.2 . .
C27 C28 H28A 119.2 . .
C28 C29 C30 117.0(5) . .
C28 C29 C29 122.0(6) . 13_554
C30 C29 C29 121.0(7) . 13_554
C31 C30 C29 121.4(5) . .
C31 C30 H30A 119.3 . .
C29 C30 H30A 119.3 . .
C26 C31 C30 121.0(5) . .
C26 C31 H31A 119.5 . .
C30 C31 H31A 119.5 . .
C2 N1 N2 107.9(4) . .
C2 N1 Zn1 133.4(3) . .
N2 N1 Zn1 118.7(3) . .
C4 N2 N1 108.3(4) . .
C4 N2 Zn2 133.2(3) . .
N1 N2 Zn2 116.3(3) . .
C7 N3 N4 105.3(4) . .
C7 N3 Zn2 128.4(4) . 11_667
N4 N3 Zn2 122.3(3) . 11_667
C9 N4 N3 111.9(4) . .
C9 N4 H4 127(4) . .
N3 N4 H4 120(4) . .
C11 O1 Zn1 138.6(3) . .
C11 O2 Zn2 125.3(4) . .
C18 O3 Zn2 134.7(3) . 7_445
C18 O4 Zn1 127.6(4) . 7_445
C25 O5 Zn1 120.7(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O5 1.894(3) .
Zn1 O4 1.954(3) 8_443
Zn1 O1 1.957(4) .
Zn1 N1 1.964(3) .
Zn2 O2 1.933(3) .
Zn2 O3 1.965(3) 8_443
Zn2 N2 1.983(4) .
Zn2 N3 1.999(4) 16_657
C1 C2 1.499(7) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 N1 1.346(5) .
C2 C3 1.377(6) .
C3 C4 1.394(6) .
C3 C8 1.485(6) .
C4 N2 1.348(5) .
C4 C5 1.486(7) .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C6 C7 1.487(7) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 N3 1.342(5) .
C7 C8 1.398(7) .
C8 C9 1.384(7) .
C9 N4 1.334(6) .
C9 C10 1.493(7) .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 O1 1.262(6) .
C11 O2 1.262(6) .
C11 C12 1.494(6) .
C12 C13 1.369(7) .
C12 C17 1.386(7) .
C13 C14 1.387(7) .
C13 H13A 0.9300 .
C14 C15 1.405(7) .
C14 H14A 0.9300 .
C15 C16 1.378(8) .
C15 C22 1.481(7) .
C16 C17 1.382(7) .
C16 H16A 0.9300 .
C17 H17A 0.9300 .
C18 O3 1.248(6) .
C18 O4 1.257(6) .
C18 C19 1.493(6) .
C19 C20 1.378(7) .
C19 C24 1.383(7) .
C20 C21 1.377(7) .
C20 H20A 0.9300 .
C21 C22 1.389(8) .
C21 H21A 0.9300 .
C22 C23 1.385(8) .
C23 C24 1.396(7) .
C23 H23A 0.9300 .
C24 H24A 0.9300 .
C25 O6 1.240(6) .
C25 O5 1.274(6) .
C25 C26 1.502(7) .
C26 C31 1.372(7) .
C26 C27 1.378(7) .
C27 C28 1.389(7) .
C27 H27A 0.9300 .
C28 C29 1.366(8) .
C28 H28A 0.9300 .
C29 C30 1.396(7) .
C29 C29 1.480(9) 13_554
C30 C31 1.386(7) .
C30 H30A 0.9300 .
C31 H31A 0.9300 .
N1 N2 1.383(5) .
N3 N4 1.362(5) .
N3 Zn2 1.999(4) 11_667
N4 H4 0.94(6) .
O3 Zn2 1.965(3) 7_445
O4 Zn1 1.954(3) 7_445
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N4 H4 O6 0.94(6) 1.83(6) 2.755(5) 171(6) 11_666
C5 H5A N3 0.96 2.48 3.369(6) 153.9 16_657
C5 H5A N4 0.96 2.47 3.285(7) 142.7 16_657
C1 H1A O5 0.96 2.55 3.451(6) 156.8 .
