#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:12:01 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179561 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/30/4503057.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_4503057
loop_
_publ_author_name
'Xue, Ming'
'Zhu, Guangshan'
'Zhang, Yujian'
'Fang, Qianrong'
'Hewitt, Ian J.'
'Qiu, Shilun'
_publ_section_title
;
 Rational Design and Control of the Dimensions of Channels in a Series of
 3D Pillared Metal−Organic Frameworks: Synthesis, Structures,
 Adsorption, and Luminescence Properties
;
_journal_issue                   2
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              427
_journal_paper_doi               10.1021/cg0701022
_journal_volume                  8
_journal_year                    2008
_chemical_formula_moiety         'C30 H22 N2 O13 Zn3'
_chemical_formula_sum            'C30 H22 N2 O13 Zn3'
_chemical_formula_weight         814.61
_chemical_melting_point          ?
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_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                95.64(3)
_cell_angle_beta                 97.68(3)
_cell_angle_gamma                118.25(3)
_cell_formula_units_Z            1
_cell_length_a                   8.9508(18)
_cell_length_b                   9.0892(18)
_cell_length_c                   19.802(4)
_cell_measurement_temperature    293(2)
_cell_volume                     1382.1(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7373
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.06
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.331
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.979
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             410
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.761
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.283
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         5887
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0708
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1980P)²+1.9021P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2300
_refine_ls_wR_factor_ref         0.2423
_reflns_number_gt                5126
_reflns_number_total             5887
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0701022-file001.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Triclinic' changed to 'triclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1382.0(5)
_cod_original_sg_symbol_H-M      P1
_cod_database_code               4503057
loop_
_symmetry_equiv_pos_as_xyz
'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 0.68612(10) 0.55708(9) 0.22914(5) 0.0372(4) Uani 1 1 d .
Zn2 Zn 0.5600(3) 0.3851(2) 0.06379(11) 0.0324(3) Uani 1 1 d .
Zn3 Zn 0.43368(10) 0.21375(9) -0.10176(5) 0.0371(4) Uani 1 1 d .
N1 N 0.7817(19) 0.6371(17) 0.3337(8) 0.054(4) Uani 1 1 d .
N2 N 1.3407(19) 1.137(2) 0.7962(7) 0.054(4) Uani 1 1 d .
O1 O 0.5497(17) 0.6623(17) 0.2069(6) 0.064(3) Uani 1 1 d .
O2 O 0.5078(18) 0.5802(13) 0.0931(6) 0.055(3) Uani 1 1 d .
O3 O 0.545(2) 1.2373(19) 0.2617(8) 0.107(5) Uani 1 1 d U
O4 O 0.5697(14) 1.3348(11) 0.1671(5) 0.042(3) Uani 1 1 d .
O5 O -0.0917(14) 0.6704(16) 0.1995(6) 0.056(3) Uani 1 1 d .
O6 O -0.1768(13) 0.5511(13) 0.0875(5) 0.046(3) Uani 1 1 d .
O7 O 0.2949(12) 0.2254(12) 0.0388(6) 0.046(3) Uani 1 1 d .
O8 O 0.2138(16) 0.0942(18) -0.0721(7) 0.062(4) Uani 1 1 d .
O9 O -0.3841(17) 0.1930(14) 0.0351(5) 0.049(3) Uani 1 1 d .
O10 O -0.446(2) 0.0909(19) -0.0759(6) 0.081(4) Uani 1 1 d .
O11 O -0.4479(16) -0.5633(13) -0.0395(6) 0.052(3) Uani 1 1 d .
O12 O -0.3489(14) -0.4780(9) -0.1292(4) 0.066(3) Uani 1 1 d .
O13A O 0.122(3) 0.530(3) 0.9295(16) 0.103(8) Uani 0.50 1 d P
O13 O 0.074(4) 0.477(3) 0.8569(19) 0.123(9) Uani 0.50 1 d PU
C1 C 0.4976(18) 0.6632(16) 0.1404(8) 0.039(3) Uani 1 1 d .
C2 C 0.4034(17) 0.7642(17) 0.1267(8) 0.040(4) Uani 1 1 d .
C3 C 0.4998(19) 0.9413(17) 0.1720(9) 0.042(4) Uani 1 1 d .
H3A H 0.6156 1.0046 0.1632 0.050 Uiso 1 1 calc R
H3B H 0.5092 0.9325 0.2207 0.050 Uiso 1 1 calc R
C4 C 0.394(2) 1.0338(16) 0.1536(8) 0.041(3) Uani 1 1 d .
C5 C 0.489(2) 1.2136(17) 0.1958(7) 0.038(3) Uani 1 1 d .
C6 C 0.2116(17) 0.9354(16) 0.1732(7) 0.030(3) Uani 1 1 d .
H6A H 0.2250 0.9267 0.2218 0.037 Uiso 1 1 calc R
H6B H 0.1469 0.9948 0.1648 0.037 Uiso 1 1 calc R
C7 C 0.1145(17) 0.7550(14) 0.1267(8) 0.035(3) Uani 1 1 d .
C8 C -0.0638(17) 0.6534(16) 0.1385(7) 0.031(3) Uani 1 1 d .
C9 C 0.2171(18) 0.6630(18) 0.1422(8) 0.037(3) Uani 1 1 d .
H9A H 0.1564 0.5500 0.1140 0.045 Uiso 1 1 calc R
H9B H 0.2262 0.6514 0.1906 0.045 Uiso 1 1 calc R
C10 C 0.188(2) 0.121(2) -0.0116(8) 0.043(4) Uani 1 1 d .
C11 C -0.0007(18) 0.0104(18) -0.0012(7) 0.035(3) Uani 1 1 d .
C12 C -0.0995(18) 0.1095(17) -0.0152(7) 0.035(3) Uani 1 1 d .
H12A H -0.0377 0.2206 0.0146 0.042 Uiso 1 1 calc R
H12B H -0.1062 0.1256 -0.0630 0.042 Uiso 1 1 calc R
C13 C -0.2802(19) 0.0114(18) -0.0014(7) 0.035(3) Uani 1 1 d .
C14 C -0.3763(18) 0.1063(18) -0.0166(7) 0.037(3) Uani 1 1 d .
C15 C -0.3772(18) -0.1754(17) -0.0449(8) 0.039(3) Uani 1 1 d .
H15A H -0.4898 -0.2388 -0.0331 0.047 Uiso 1 1 calc R
H15B H -0.3956 -0.1713 -0.0939 0.047 Uiso 1 1 calc R
C16 C -0.2749(19) -0.2653(17) -0.0309(7) 0.036(3) Uani 1 1 d .
C17 C -0.377(2) -0.4428(17) -0.0736(8) 0.052(4) Uani 1 1 d .
C18 C -0.099(2) -0.1644(18) -0.0437(8) 0.045(4) Uani 1 1 d .
H18A H -0.1068 -0.1561 -0.0924 0.054 Uiso 1 1 calc R
H18B H -0.0343 -0.2235 -0.0339 0.054 Uiso 1 1 calc R
C19 C 0.941(3) 0.762(2) 0.3557(11) 0.080(5) Uani 1 1 d U
H19 H 1.0206 0.7914 0.3269 0.096 Uiso 1 1 calc R
C20 C 0.987(3) 0.848(4) 0.4234(14) 0.101(8) Uani 1 1 d U
H20 H 1.0624 0.9646 0.4348 0.121 Uiso 1 1 calc R
C21 C 0.918(3) 0.755(3) 0.4734(10) 0.090(8) Uani 1 1 d .
C22 C 0.763(3) 0.618(3) 0.4506(9) 0.076(5) Uani 1 1 d U
H22 H 0.6991 0.5581 0.4818 0.091 Uiso 1 1 calc R
C23 C 0.697(3) 0.566(3) 0.3805(11) 0.085(7) Uani 1 1 d .
H23 H 0.5855 0.4737 0.3655 0.102 Uiso 1 1 calc R
C24 C 0.977(3) 0.812(3) 0.5473(11) 0.083(6) Uani 1 1 d U
H24 H 0.9034 0.7468 0.5744 0.100 Uiso 1 1 calc R
C25 C 1.109(4) 0.932(5) 0.5777(10) 0.130(11) Uani 1 1 d .
H25 H 1.1741 0.9961 0.5479 0.156 Uiso 1 1 calc R
C26 C 1.200(3) 1.007(4) 0.6543(12) 0.101(10) Uani 1 1 d .
C27 C 1.349(4) 1.165(4) 0.6780(15) 0.117(9) Uani 1 1 d U
H27 H 1.4040 1.2296 0.6462 0.140 Uiso 1 1 calc R
C28 C 1.414(3) 1.226(3) 0.7473(9) 0.075(6) Uani 1 1 d U
H28 H 1.5132 1.3318 0.7617 0.090 Uiso 1 1 calc R
C29 C 1.194(3) 0.977(3) 0.7742(11) 0.085(6) Uani 1 1 d U
H29 H 1.1558 0.8980 0.8035 0.102 Uiso 1 1 calc R
C30 C 1.103(3) 0.940(3) 0.7027(11) 0.092(7) Uani 1 1 d U
H30 H 0.9836 0.8730 0.6902 0.110 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
O1 Zn1 O5 111.4(6) . 1_655
O1 Zn1 O4 106.3(5) . 1_545
O5 Zn1 O4 101.5(4) 1_655 1_545
O1 Zn1 N1 104.9(6) . .
O5 Zn1 N1 97.4(5) 1_655 .
O4 Zn1 N1 134.1(5) 1_545 .
O6 Zn2 O7 178.0(6) 1_655 .
O6 Zn2 O9 87.6(5) 1_655 1_655
O7 Zn2 O9 94.0(5) . 1_655
O6 Zn2 O2 91.6(5) 1_655 .
O7 Zn2 O2 86.8(5) . .
O9 Zn2 O2 179.1(7) 1_655 .
O6 Zn2 O4 90.1(4) 1_655 1_545
O7 Zn2 O4 91.1(5) . 1_545
O9 Zn2 O4 89.3(4) 1_655 1_545
O2 Zn2 O4 90.6(4) . 1_545
O6 Zn2 O11 89.5(4) 1_655 1_665
O7 Zn2 O11 89.3(5) . 1_665
O9 Zn2 O11 90.7(5) 1_655 1_665
O2 Zn2 O11 89.4(5) . 1_665
O4 Zn2 O11 179.6(6) 1_545 1_665
O10 Zn3 O8 104.1(7) 1_655 .
O10 Zn3 O11 108.0(5) 1_655 1_665
O8 Zn3 O11 103.1(5) . 1_665
O10 Zn3 N2 106.0(6) 1_655 1_444
O8 Zn3 N2 97.5(6) . 1_444
O11 Zn3 N2 134.0(6) 1_665 1_444
C23 N1 C19 117.1(18) . .
C23 N1 Zn1 124.0(13) . .
C19 N1 Zn1 118.8(14) . .
C28 N2 C29 118.5(16) . .
C28 N2 Zn3 124.6(13) . 1_666
C29 N2 Zn3 116.9(14) . 1_666
C1 O1 Zn1 119.5(9) . .
C1 O2 Zn2 145.1(12) . .
C5 O4 Zn1 113.9(8) . 1_565
C5 O4 Zn2 136.7(9) . 1_565
Zn1 O4 Zn2 106.2(4) 1_565 1_565
C8 O5 Zn1 127.5(10) . 1_455
C8 O6 Zn2 138.4(9) . 1_455
C10 O7 Zn2 137.0(10) . .
C10 O8 Zn3 125.8(11) . .
C14 O9 Zn2 142.9(11) . 1_455
C14 O10 Zn3 122.9(9) . 1_455
C17 O11 Zn3 110.6(10) . 1_445
C17 O11 Zn2 141.6(10) . 1_445
Zn3 O11 Zn2 106.0(5) 1_445 1_445
O2 C1 O1 123.6(15) . .
O2 C1 C2 119.5(14) . .
O1 C1 C2 116.6(11) . .
C3 C2 C1 111.7(11) . .
C3 C2 C9 109.4(10) . .
C1 C2 C9 108.3(11) . .
C2 C3 C4 107.6(12) . .
C5 C4 C3 109.4(12) . .
C5 C4 C6 108.3(11) . .
C3 C4 C6 109.1(11) . .
O4 C5 O3 115.7(14) . .
O4 C5 C4 119.2(11) . .
O3 C5 C4 119.3(14) . .
C7 C6 C4 107.0(9) . .
C8 C7 C9 109.8(11) . .
C8 C7 C6 111.6(10) . .
C9 C7 C6 109.1(11) . .
O6 C8 O5 124.0(13) . .
O6 C8 C7 116.9(11) . .
O5 C8 C7 119.0(12) . .
C7 C9 C2 110.6(11) . .
O7 C10 O8 126.8(14) . .
O7 C10 C11 117.3(12) . .
O8 C10 C11 116.0(14) . .
C18 C11 C12 110.6(11) . .
C18 C11 C10 115.6(11) . .
C12 C11 C10 107.8(11) . .
C13 C12 C11 109.7(11) . .
C14 C13 C12 109.4(11) . .
C14 C13 C15 112.5(11) . .
C12 C13 C15 110.4(10) . .
O10 C14 O9 124.3(13) . .
O10 C14 C13 119.5(11) . .
O9 C14 C13 116.1(13) . .
C16 C15 C13 111.4(11) . .
C18 C16 C15 110.1(11) . .
C18 C16 C17 114.3(11) . .
C15 C16 C17 108.2(12) . .
O12 C17 O11 118.2(13) . .
O12 C17 C16 122.0(12) . .
O11 C17 C16 115.6(13) . .
C16 C18 C11 113.4(11) . .
N1 C19 C20 118(2) . .
C19 C20 C21 118(2) . .
C22 C21 C20 115(2) . .
C22 C21 C24 118(2) . .
C20 C21 C24 126(2) . .
C21 C22 C23 119(2) . .
N1 C23 C22 124(2) . .
C25 C24 C21 127.9(18) . .
C24 C25 C26 136(3) . .
C30 C26 C27 116(2) . .
C30 C26 C25 117(2) . .
C27 C26 C25 125(3) . .
C28 C27 C26 121(3) . .
N2 C28 C27 122(2) . .
N2 C29 C30 116(2) . .
C26 C30 C29 118(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 1.909(12) .
Zn1 O5 1.962(11) 1_655
Zn1 O4 1.963(9) 1_545
Zn1 N1 2.047(15) .
Zn2 O6 2.061(11) 1_655
Zn2 O7 2.065(9) .
Zn2 O9 2.082(10) 1_655
Zn2 O2 2.086(10) .
Zn2 O4 2.140(11) 1_545
Zn2 O11 2.142(12) 1_665
Zn3 O10 1.944(11) 1_655
Zn3 O8 1.952(12) .
Zn3 O11 1.969(11) 1_665
Zn3 N2 1.997(13) 1_444
N1 C23 1.30(3) .
N1 C19 1.31(2) .
N2 C28 1.36(2) .
N2 C29 1.40(3) .
N2 Zn3 1.997(13) 1_666
O1 C1 1.34(2) .
O2 C1 1.185(17) .
O3 C5 1.29(2) .
O4 C5 1.240(17) .
O4 Zn1 1.963(9) 1_565
O4 Zn2 2.140(11) 1_565
O5 C8 1.275(17) .
O5 Zn1 1.962(11) 1_455
O6 C8 1.249(16) .
O6 Zn2 2.061(11) 1_455
O7 C10 1.229(19) .
O8 C10 1.273(19) .
O9 C14 1.259(16) .
O9 Zn2 2.082(10) 1_455
O10 C14 1.215(19) .
O10 Zn3 1.944(11) 1_455
O11 C17 1.290(18) .
O11 Zn3 1.969(11) 1_445
O11 Zn2 2.142(12) 1_445
O12 C17 1.205(18) .
O13A O13 1.41(4) .
C1 C2 1.53(2) .
C2 C3 1.528(18) .
C2 C9 1.569(19) .
C3 C4 1.57(2) .
C4 C5 1.523(18) .
C4 C6 1.572(19) .
C6 C7 1.560(16) .
C7 C8 1.484(19) .
C7 C9 1.530(19) .
C10 C11 1.56(2) .
C11 C18 1.491(18) .
C11 C12 1.552(19) .
C12 C13 1.512(19) .
C13 C14 1.503(19) .
C13 C15 1.579(18) .
C15 C16 1.51(2) .
C16 C18 1.48(2) .
C16 C17 1.511(19) .
C19 C20 1.38(3) .
C20 C21 1.38(4) .
C21 C22 1.33(3) .
C21 C24 1.44(3) .
C22 C23 1.37(3) .
C24 C25 1.19(3) .
C25 C26 1.54(3) .
C26 C30 1.37(4) .
C26 C27 1.39(4) .
C27 C28 1.37(3) .
C29 C30 1.46(3) .
