#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/84/7208414.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_7208414
loop_
_publ_author_name
'Guo, Min'
'Sun, Zhong-Ming'
_publ_section_title
;
 Solvents control over the degree of interpenetration in metal-organic
 frameworks and their high sensitivities for detecting nitrobenzene at ppm
 level
;
_journal_issue                   31
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              15939
_journal_paper_doi               10.1039/c2jm32066e
_journal_volume                  22
_journal_year                    2012
_chemical_formula_sum            'C32 H26 N2 O9 Zn1.5'
_chemical_formula_weight         680.60
_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                99.783(2)
_cell_angle_beta                 102.396(2)
_cell_angle_gamma                101.834(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6549(12)
_cell_length_b                   14.5638(16)
_cell_length_c                   16.0435(17)
_cell_measurement_reflns_used    2184
_cell_measurement_temperature    571(2)
_cell_measurement_theta_max      20.62
_cell_measurement_theta_min      2.45
_cell_volume                     2319.5(4)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      571(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0712
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12256
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.975
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shuttle-like
_exptl_crystal_F_000             698
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.447
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         8390
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.1274
_refine_ls_R_factor_gt           0.0931
_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2923
_refine_ls_wR_factor_ref         0.3245
_reflns_number_gt                5492
_reflns_number_total             8390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2jm32066e.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C32 H26 N2 O9 Zn1.50'
_cod_database_code               7208414
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 0.0000 -0.5000 -0.5000 0.0351(3) Uani 1 2 d S
Zn2 Zn 0.77570(8) 0.62490(5) 0.52481(5) 0.0424(3) Uani 1 1 d .
O1 O 0.7386(6) 0.5409(4) -0.3985(4) 0.0646(15) Uani 1 1 d .
O2 O 0.6376(6) 0.5284(5) 0.4011(4) 0.0866(18) Uani 1 1 d U
O3 O 0.8492(5) 0.5571(3) 0.4263(3) 0.0497(12) Uani 1 1 d .
O4 O 0.0810(5) -0.3655(3) -0.4189(3) 0.0552(13) Uani 1 1 d .
O5 O 0.8840(5) 0.4556(4) -0.4187(4) 0.0591(14) Uani 1 1 d .
O6 O 0.6819(7) 0.2941(5) 0.0443(4) 0.096(2) Uani 1 1 d .
O7 O 0.5926(6) 0.2483(5) -0.1713(4) 0.0808(18) Uani 1 1 d .
O8 O 0.4686(6) 0.0095(4) -0.1714(4) 0.087(2) Uani 1 1 d .
O14 O -0.0631(5) -0.2746(4) -0.4163(4) 0.0640(14) Uani 1 1 d .
N1 N 0.6448(6) 0.7062(4) 0.5276(4) 0.0530(15) Uani 1 1 d .
N2 N 0.5408(7) 0.8185(5) 0.5177(5) 0.071(2) Uani 1 1 d .
C4 C 0.7935(7) 0.4741(5) -0.3874(5) 0.0490(17) Uani 1 1 d .
C5 C 0.7445(7) 0.4126(5) -0.3280(5) 0.0504(17) Uani 1 1 d .
C6 C 0.8178(8) 0.3578(6) -0.2893(6) 0.069(2) Uani 1 1 d .
H6 H 0.9010 0.3581 -0.2988 0.083 Uiso 1 1 calc R
C8 C 0.6225(8) 0.4111(6) -0.3126(5) 0.064(2) Uani 1 1 d .
H8 H 0.5722 0.4497 -0.3370 0.077 Uiso 1 1 calc R
C9 C 0.7388(9) 0.5199(7) 0.3748(5) 0.071(2) Uani 1 1 d U
C10 C 0.7220(8) 0.4643(5) 0.2868(5) 0.060(2) Uani 1 1 d .
C11 C 0.8317(8) 0.4556(6) 0.2563(5) 0.063(2) Uani 1 1 d .
H11 H 0.9162 0.4876 0.2912 0.075 Uiso 1 1 calc R
C12 C 0.8165(9) 0.3991(6) 0.1734(5) 0.073(2) Uani 1 1 d .
H12 H 0.8900 0.3941 0.1522 0.087 Uiso 1 1 calc R
C13 C 0.6879(10) 0.3500(6) 0.1230(5) 0.073(3) Uani 1 1 d .
C14 C 0.5751(10) 0.3614(7) 0.1508(6) 0.085(3) Uani 1 1 d .
H14 H 0.4902 0.3337 0.1146 0.102 Uiso 1 1 calc R
C15 C 0.5948(9) 0.4160(7) 0.2349(5) 0.071(2) Uani 1 1 d .
H15 H 0.5217 0.4203 0.2569 0.085 Uiso 1 1 calc R
C16 C 0.4477(12) 1.0506(7) 0.5563(7) 0.101(4) Uani 1 1 d .
H16 H 0.4105 1.0842 0.5950 0.122 Uiso 1 1 calc R
C17 C 0.4711(13) 0.9616(8) 0.5671(8) 0.112(4) Uani 1 1 d .
H17 H 0.4521 0.9364 0.6138 0.134 Uiso 1 1 calc R
C18 C 0.5212(10) 0.9135(6) 0.5088(6) 0.075(3) Uani 1 1 d .
C19 C 0.4564(10) 0.7447(7) 0.5333(6) 0.078(3) Uani 1 1 d .
H19 H 0.3712 0.7428 0.5395 0.094 Uiso 1 1 calc R
C20 C 0.6537(9) 0.7906(6) 0.5156(6) 0.071(2) Uani 1 1 d .
H20 H 0.7287 0.8288 0.5065 0.085 Uiso 1 1 calc R
C21 C 0.5197(9) 0.6752(6) 0.5381(6) 0.067(2) Uani 1 1 d .
H21 H 0.4846 0.6149 0.5471 0.080 Uiso 1 1 calc R
C23 C 0.5738(8) 0.3538(7) -0.2618(6) 0.070(2) Uani 1 1 d .
H23 H 0.4889 0.3508 -0.2546 0.084 Uiso 1 1 calc R
C24 C 0.3611(8) -0.0579(5) -0.2236(5) 0.061(2) Uani 1 1 d .
C25 C 0.2402(10) -0.0448(6) -0.2532(7) 0.084(3) Uani 1 1 d .
H25 H 0.2235 0.0145 -0.2348 0.100 Uiso 1 1 calc R
C26 C 0.3827(9) -0.1491(6) -0.2477(6) 0.073(2) Uani 1 1 d .
H26 H 0.4650 -0.1602 -0.2254 0.088 Uiso 1 1 calc R
C27 C 0.0526(7) -0.2902(5) -0.3950(4) 0.0463(16) Uani 1 1 d .
C28 C 0.1614(7) -0.2088(5) -0.3354(5) 0.0503(17) Uani 1 1 d .
C29 C 0.1406(9) -0.1175(6) -0.3102(6) 0.078(3) Uani 1 1 d .
H29 H 0.0585 -0.1061 -0.3322 0.093 Uiso 1 1 calc R
C30 C 0.2831(8) -0.2222(5) -0.3042(5) 0.062(2) Uani 1 1 d .
H30 H 0.2994 -0.2819 -0.3214 0.074 Uiso 1 1 calc R
C36 C 0.4514(9) 0.0900(6) -0.1237(5) 0.071(3) Uani 1 1 d .
H36A H 0.3945 0.0726 -0.0862 0.086 Uiso 1 1 calc R
H36B H 0.4094 0.1256 -0.1625 0.086 Uiso 1 1 calc R
C37 C 0.5864(9) 0.1522(6) -0.0683(5) 0.066(2) Uani 1 1 d .
C39 C 0.6644(9) 0.1933(6) -0.1264(5) 0.061(2) Uani 1 1 d .
H39A H 0.7504 0.2333 -0.0917 0.074 Uiso 1 1 calc R
H39B H 0.6783 0.1419 -0.1677 0.074 Uiso 1 1 calc R
C41 C 0.6480(8) 0.3019(6) -0.2223(5) 0.061(2) Uani 1 1 d .
C42 C 0.7710(9) 0.3025(6) -0.2366(6) 0.076(3) Uani 1 1 d .
H42 H 0.8220 0.2653 -0.2105 0.091 Uiso 1 1 calc R
C46 C 0.5553(10) 0.2317(7) -0.0040(5) 0.079(3) Uani 1 1 d .
H46A H 0.5009 0.2668 -0.0358 0.095 Uiso 1 1 calc R
H46B H 0.5088 0.2038 0.0351 0.095 Uiso 1 1 calc R
C48 C 0.6696(12) 0.0941(7) -0.0145(7) 0.105(4) Uani 1 1 d .
H48A H 0.6675 0.0347 -0.0521 0.158 Uiso 1 1 calc R
H48B H 0.6323 0.0806 0.0329 0.158 Uiso 1 1 calc R
H48C H 0.7598 0.1316 0.0087 0.158 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
O4 Zn1 O4 180.00(17) . 2_544
O4 Zn1 O5 87.2(2) . 2_654
O4 Zn1 O5 92.8(2) 2_544 2_654
O4 Zn1 O5 92.8(2) . 1_445
O4 Zn1 O5 87.2(2) 2_544 1_445
O5 Zn1 O5 180.000(1) 2_654 1_445
O4 Zn1 O3 91.03(18) . 2_655
O4 Zn1 O3 88.97(18) 2_544 2_655
O5 Zn1 O3 93.48(19) 2_654 2_655
O5 Zn1 O3 86.52(19) 1_445 2_655
O4 Zn1 O3 88.97(18) . 1_444
O4 Zn1 O3 91.03(18) 2_544 1_444
O5 Zn1 O3 86.52(19) 2_654 1_444
O5 Zn1 O3 93.48(19) 1_445 1_444
O3 Zn1 O3 180.000(1) 2_655 1_444
O1 Zn2 O14 109.4(3) 1_556 1_666
O1 Zn2 N1 104.4(3) 1_556 .
O14 Zn2 N1 98.1(2) 1_666 .
O1 Zn2 O3 110.2(2) 1_556 .
O14 Zn2 O3 97.1(2) 1_666 .
N1 Zn2 O3 134.6(2) . .
O1 Zn2 O2 97.0(3) 1_556 .
O14 Zn2 O2 149.8(3) 1_666 .
N1 Zn2 O2 88.9(2) . .
O3 Zn2 O2 59.0(2) . .
O1 Zn2 C9 107.2(3) 1_556 .
O14 Zn2 C9 123.6(3) 1_666 .
N1 Zn2 C9 112.4(3) . .
O3 Zn2 C9 29.2(2) . .
O2 Zn2 C9 29.9(3) . .
C4 O1 Zn2 124.0(5) . 1_554
C9 O2 Zn2 87.6(5) . .
C9 O3 Zn2 94.9(5) . .
C9 O3 Zn1 133.8(5) . 1_666
Zn2 O3 Zn1 102.55(18) . 1_666
C27 O4 Zn1 141.3(5) . .
C4 O5 Zn1 141.8(5) . 1_665
C13 O6 C46 117.1(8) . .
C41 O7 C39 119.9(7) . .
C24 O8 C36 119.2(8) . .
C27 O14 Zn2 123.9(5) . 1_444
C20 N1 C21 105.9(7) . .
C20 N1 Zn2 129.5(6) . .
C21 N1 Zn2 124.5(5) . .
C19 N2 C20 106.6(7) . .
C19 N2 C18 128.4(8) . .
C20 N2 C18 124.9(8) . .
O5 C4 O1 126.3(7) . .
O5 C4 C5 118.0(6) . .
O1 C4 C5 115.7(7) . .
C6 C5 C8 118.4(7) . .
C6 C5 C4 122.0(7) . .
C8 C5 C4 119.6(7) . .
C5 C6 C42 120.8(8) . .
C23 C8 C5 120.9(8) . .
O3 C9 O2 118.1(7) . .
O3 C9 C10 122.5(8) . .
O2 C9 C10 119.4(8) . .
O3 C9 Zn2 55.8(4) . .
O2 C9 Zn2 62.5(4) . .
C10 C9 Zn2 176.6(8) . .
C11 C10 C15 119.9(7) . .
C11 C10 C9 120.2(7) . .
C15 C10 C9 119.8(9) . .
C10 C11 C12 120.5(8) . .
C11 C12 C13 118.5(9) . .
O6 C13 C14 123.1(8) . .
O6 C13 C12 114.9(9) . .
C14 C13 C12 121.9(8) . .
C15 C14 C13 117.5(9) . .
C14 C15 C10 121.4(9) . .
C18 C16 C17 119.7(10) 2_676 .
C18 C17 C16 118.8(10) . .
C16 C18 C17 121.5(8) 2_676 .
C16 C18 N2 119.5(8) 2_676 .
C17 C18 N2 119.0(8) . .
C21 C19 N2 106.1(8) . .
N1 C20 N2 111.7(8) . .
C19 C21 N1 109.6(8) . .
C41 C23 C8 120.2(8) . .
C25 C24 O8 126.3(8) . .
C25 C24 C26 118.9(7) . .
O8 C24 C26 114.8(8) . .
C24 C25 C29 121.0(8) . .
C30 C26 C24 120.2(8) . .
O4 C27 O14 125.6(6) . .
O4 C27 C28 117.5(7) . .
O14 C27 C28 116.9(6) . .
C30 C28 C29 118.3(7) . .
C30 C28 C27 120.3(7) . .
C29 C28 C27 121.4(7) . .
C25 C29 C28 120.5(8) . .
C28 C30 C26 121.1(8) . .
O8 C36 C37 108.9(8) . .
C39 C37 C36 109.5(6) . .
C39 C37 C46 112.0(7) . .
C36 C37 C46 105.2(8) . .
C39 C37 C48 108.3(8) . .
C36 C37 C48 112.6(7) . .
C46 C37 C48 109.2(7) . .
O7 C39 C37 108.1(7) . .
C23 C41 O7 116.3(8) . .
C23 C41 C42 119.7(7) . .
O7 C41 C42 124.0(8) . .
C6 C42 C41 119.8(8) . .
O6 C46 C37 105.4(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O4 2.057(4) .
Zn1 O4 2.057(4) 2_544
Zn1 O5 2.074(5) 2_654
Zn1 O5 2.074(5) 1_445
Zn1 O3 2.177(4) 2_655
Zn1 O3 2.177(4) 1_444
Zn2 O1 1.921(5) 1_556
Zn2 O14 1.946(5) 1_666
Zn2 N1 2.008(6) .
Zn2 O3 2.098(5) .
Zn2 O2 2.242(6) .
Zn2 C9 2.526(8) .
O1 C4 1.251(9) .
O1 Zn2 1.921(5) 1_554
O2 C9 1.261(11) .
O3 C9 1.237(9) .
O3 Zn1 2.177(4) 1_666
O4 C27 1.219(8) .
O5 C4 1.233(9) .
O5 Zn1 2.074(5) 1_665
O6 C13 1.363(10) .
O6 C46 1.433(9) .
O7 C41 1.363(9) .
O7 C39 1.399(9) .
O8 C24 1.351(9) .
O8 C36 1.356(10) .
O14 C27 1.285(9) .
O14 Zn2 1.946(5) 1_444
N1 C20 1.264(9) .
N1 C21 1.372(11) .
N2 C19 1.349(12) .
N2 C20 1.352(10) .
N2 C18 1.466(9) .
C4 C5 1.516(9) .
C5 C6 1.360(10) .
C5 C8 1.371(10) .
C6 C42 1.363(11) .
C8 C23 1.366(11) .
C9 C10 1.457(11) .
C10 C11 1.381(12) .
C10 C15 1.397(11) .
C11 C12 1.397(11) .
C12 C13 1.403(12) .
C13 C14 1.400(14) .
C14 C15 1.392(12) .
C16 C18 1.318(12) 2_676
C16 C17 1.400(12) .
C17 C18 1.340(14) .
C18 C16 1.318(12) 2_676
C19 C21 1.330(12) .
C23 C41 1.338(11) .
C24 C25 1.339(12) .
C24 C26 1.398(12) .
C25 C29 1.370(11) .
C26 C30 1.370(10) .
C27 C28 1.496(9) .
C28 C30 1.352(11) .
C28 C29 1.398(10) .
C36 C37 1.523(11) .
C37 C39 1.496(11) .
C37 C46 1.554(13) .
C37 C48 1.573(13) .
C41 C42 1.377(12) .
