#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:09:54 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180126 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/24/7102463.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_7102463
loop_
_publ_author_name
'Wang, Xinlong'
'Qin, Chao'
'Wang, Enbo'
'Li, Yangguang'
'Hu, Changwen'
'Xu, Lin'
_publ_section_title
;
 Designed double layer assembly: a three-dimensional open framework
 with two types of cavities by connection of infinite two-dimensional
 bilayer.
;
_journal_issue                   4
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              378
_journal_page_last               379
_journal_paper_doi               10.1039/b313364h
_journal_year                    2004
_chemical_formula_sum            'C24 H16 N4 O9 Zn2'
_chemical_formula_weight         635.15
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 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                 111.60(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.069(3)
_cell_length_b                   13.635(3)
_cell_length_c                   11.508(2)
_cell_measurement_reflns_used    5113
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.41
_cell_volume                     2344.3(8)
_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_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku RAXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotation anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5113
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    2.112
_exptl_absorpt_correction_T_max  0.497
_exptl_absorpt_correction_T_min  0.426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.423
_exptl_crystal_size_mid          0.374
_exptl_crystal_size_min          0.331
_refine_diff_density_max         1.028
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2673
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0333
_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)+(0.0830P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1068
_reflns_number_gt                2342
_reflns_number_total             2673
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b313364h.txt
_cod_data_source_block           qc22
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7102463
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Zn1 Zn 0.396833(16) 0.209235(18) 0.96353(2) 0.02603(13) Uani 1 1 d .
N1 N 0.52688(13) 0.22364(15) 0.98376(19) 0.0284(4) Uani 1 1 d .
N2 N 0.33189(12) 0.12067(14) 0.81228(17) 0.0265(4) Uani 1 1 d .
C1 C 0.54939(17) 0.2935(2) 0.9197(3) 0.0444(7) Uani 1 1 d .
H1A H 0.5051 0.3358 0.8703 0.053 Uiso 1 1 calc R
C6 C 0.36923(14) 0.05759(17) 0.7563(2) 0.0273(4) Uani 1 1 d .
H6A H 0.4307 0.0611 0.7761 0.033 Uiso 1 1 calc R
C10 C 0.24214(15) 0.11759(18) 0.7794(2) 0.0305(5) Uani 1 1 d .
H10A H 0.2149 0.1633 0.8137 0.037 Uiso 1 1 calc R
C9 C 0.18943(14) 0.04922(18) 0.6967(2) 0.0311(5) Uani 1 1 d .
H9A H 0.1279 0.0487 0.6770 0.037 Uiso 1 1 calc R
O1W O 0.5000 0.4867(3) 0.7500 0.0656(9) Uani 1 2 d SD
H1 H 0.5493 0.5195 0.8201 0.098 Uiso 1 1 d RD
C2 C 0.63551(18) 0.3058(2) 0.9235(3) 0.0459(7) Uani 1 1 d .
H2A H 0.6481 0.3553 0.8768 0.055 Uiso 1 1 calc R
C5 C 0.59144(17) 0.1645(2) 1.0540(3) 0.0491(8) Uani 1 1 d .
H5A H 0.5769 0.1154 1.0992 0.059 Uiso 1 1 calc R
C4 C 0.67925(17) 0.1727(3) 1.0629(3) 0.0504(8) Uani 1 1 d .
H4A H 0.7223 0.1298 1.1137 0.060 Uiso 1 1 calc R
C8 C 0.22870(14) -0.01903(15) 0.64297(19) 0.0242(4) Uani 1 1 d .
C7 C 0.32126(14) -0.01268(16) 0.6707(2) 0.0256(4) Uani 1 1 d .
C12 C 0.16945(14) -0.09659(17) 0.5602(2) 0.0291(4) Uani 1 1 d .
O1 O 0.15870(12) -0.16975(13) 0.62136(17) 0.0365(4) Uani 1 1 d .
O2 O 0.13327(15) -0.08272(17) 0.44747(17) 0.0516(5) Uani 1 1 d .
C11 C 0.37006(15) -0.07739(18) 0.6103(2) 0.0312(5) Uani 1 1 d .
O3 O 0.33785(12) -0.16216(13) 0.57535(16) 0.0354(4) Uani 1 1 d .
O4 O 0.43610(14) -0.04495(17) 0.5948(2) 0.0531(6) Uani 1 1 d .
C3 C 0.70307(13) 0.24460(17) 0.99650(19) 0.0254(4) 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
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 O3 111.15(7) 4_556 6_556
O1 Zn1 N1 103.72(8) 4_556 .
O3 Zn1 N1 133.01(8) 6_556 .
O1 Zn1 N2 94.38(8) 4_556 .
O3 Zn1 N2 98.37(8) 6_556 .
N1 Zn1 N2 109.54(8) . .
C5 N1 C1 117.4(2) . .
C5 N1 Zn1 123.59(17) . .
C1 N1 Zn1 118.95(16) . .
C6 N2 C10 117.75(19) . .
C6 N2 Zn1 127.22(15) . .
C10 N2 Zn1 114.33(15) . .
N1 C1 C2 122.9(2) . .
N2 C6 C7 123.7(2) . .
N2 C10 C9 122.5(2) . .
C10 C9 C8 119.7(2) . .
C1 C2 C3 120.1(2) . .
N1 C5 C4 123.0(2) . .
C3 C4 C5 120.0(2) . .
C9 C8 C7 118.3(2) . .
C9 C8 C12 117.83(19) . .
C7 C8 C12 123.88(19) . .
C6 C7 C8 117.96(19) . .
C6 C7 C11 118.94(19) . .
C8 C7 C11 123.1(2) . .
O2 C12 O1 126.9(2) . .
O2 C12 C8 120.3(2) . .
O1 C12 C8 112.66(19) . .
C12 O1 Zn1 121.08(16) . 4_546
O4 C11 O3 123.9(2) . .
O4 C11 C7 118.8(2) . .
O3 C11 C7 117.3(2) . .
C11 O3 Zn1 105.44(15) . 6
C4 C3 C2 116.7(2) . .
C4 C3 C3 121.5(3) . 7_657
C2 C3 C3 121.8(3) . 7_657
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 1.9573(18) 4_556
Zn1 O3 1.9659(17) 6_556
Zn1 N1 2.025(2) .
Zn1 N2 2.0590(19) .
N1 C5 1.327(3) .
N1 C1 1.334(3) .
N2 C6 1.341(3) .
N2 C10 1.350(3) .
C1 C2 1.379(4) .
C6 C7 1.387(3) .
C10 C9 1.377(3) .
C9 C8 1.391(3) .
C2 C3 1.382(3) .
C5 C4 1.381(3) .
C4 C3 1.381(3) .
C8 C7 1.404(3) .
C8 C12 1.505(3) .
C7 C11 1.509(3) .
C12 O2 1.226(3) .
C12 O1 1.269(3) .
O1 Zn1 1.9573(18) 4_546
C11 O4 1.222(3) .
C11 O3 1.270(3) .
O3 Zn1 1.9659(17) 6
C3 C3 1.488(4) 7_657
