#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:07:15 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178769 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/23/4102345.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_4102345
loop_
_publ_author_name
'Hai-Long Jiang'
'Yoshiro Tatsu'
'Zhang-Hui Lu'
'Qiang Xu'
_publ_section_title
;
 Non-, Micro-, and Mesoporous Metal-Organic Framework Isomers: Reversible
 Transformation, Fluorescence Sensing, and Large Molecule Separation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5586
_journal_page_last               5587
_journal_paper_doi               10.1021/ja101541s
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C18 H13 Cd N3 O4'
_chemical_formula_weight         447.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 112.77(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.950(3)
_cell_length_b                   11.700(2)
_cell_length_c                   10.210(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1756.8(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0670
_diffrn_reflns_av_sigmaI/netI    0.0612
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8503
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.46
_exptl_absorpt_coefficient_mu    1.271
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7262
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.982
_refine_diff_density_min         -1.314
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2100
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.070
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0743P)²+3.4701P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1411
_reflns_number_gt                1434
_reflns_number_total             2100
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja101541s_si_002.cif
_cod_data_source_block           a
_cod_original_cell_volume        1756.8(6)
_cod_database_code               4102345
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.13085(4) 0.0000 0.10509(7) 0.0397(2) Uani 1 2 d SU . .
N3 N 0.1244(4) 0.1972(4) 0.1156(6) 0.0513(13) Uani 1 1 d U . .
C11 C 0.1372(7) 0.2584(6) 0.0173(11) 0.085(3) Uani 1 1 d U . .
H11A H 0.1469 0.2203 -0.0555 0.103 Uiso 1 1 calc R . .
C12 C 0.1371(7) 0.3765(6) 0.0162(10) 0.080(2) Uani 1 1 d U . .
H12A H 0.1460 0.4151 -0.0570 0.096 Uiso 1 1 calc R . .
C13 C 0.1243(5) 0.4364(5) 0.1196(8) 0.0575(16) Uani 1 1 d U . .
C14 C 0.1118(8) 0.3740(6) 0.2215(10) 0.089(2) Uani 1 1 d U . .
H14A H 0.1040 0.4104 0.2969 0.107 Uiso 1 1 calc R . .
C15 C 0.1107(9) 0.2551(7) 0.2143(11) 0.098(3) Uani 1 1 d U . .
H15A H 0.0995 0.2146 0.2843 0.118 Uiso 1 1 calc R . .
C1 C 0.0636(6) 0.0000 -0.1941(9) 0.0426(17) Uani 1 2 d SU . .
C2 C 0.0329(6) 0.0000 -0.3497(9) 0.0387(16) Uani 1 2 d SU B .
C3 C 0.0929(6) 0.0000 -0.4203(10) 0.052(2) Uani 1 2 d SDU . .
H3A H 0.1573 0.0000 -0.3662 0.062 Uiso 0.50 2 d SPR A 1
N1 N 0.1808(7) 0.0000 -0.3540(18) 0.105(9) Uani 0.50 2 d SPDU B 2
H1A H 0.2151 0.0000 -0.4014 0.126 Uiso 0.50 2 calc SPR B 2
H1B H 0.2046 0.0000 -0.2627 0.126 Uiso 0.50 2 calc SPR B 2
C4 C -0.0601(6) 0.0000 -0.4342(10) 0.051(2) Uani 1 2 d SU . .
H4A H -0.1013 0.0000 -0.3900 0.061 Uiso 1 2 calc SR B .
C5 C 0.3070(7) 0.0000 0.3292(13) 0.072(3) Uani 1 2 d SU . .
C6 C 0.4069(6) 0.0000 0.4197(10) 0.050(2) Uani 1 2 d SU . .
C7 C 0.4530(5) 0.1006(6) 0.4587(10) 0.075(2) Uani 1 1 d DU . .
H7A H 0.4221 0.1695 0.4306 0.090 Uiso 0.75 1 calc PR C 1
N2 N 0.418(3) 0.2026(16) 0.413(5) 0.152(18) Uani 0.25 1 d PDU D 2
H2A H 0.3620 0.2084 0.3542 0.183 Uiso 0.25 1 calc PR D 2
H2B H 0.4504 0.2630 0.4414 0.183 Uiso 0.25 1 calc PR D 2
O1 O 0.1466(4) 0.0000 -0.1173(7) 0.0559(15) Uani 1 2 d SU . .
O2 O 0.0059(4) 0.0000 -0.1371(6) 0.0475(14) Uani 1 2 d SU . .
O3 O 0.2506(6) 0.0000 0.3777(11) 0.136(4) Uani 1 2 d SU . .
O4 O 0.2830(6) 0.0000 0.2023(9) 0.098(3) Uani 1 2 d SU . .
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'
Cd Cd -0.8075 1.2024 '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'
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 Cd1 N3 92.25(14) . .
O4 Cd1 N3 92.25(14) . 6
N3 Cd1 N3 171.4(2) . 6
O4 Cd1 O2 148.4(3) . 5
N3 Cd1 O2 86.15(12) . 5
N3 Cd1 O2 86.15(12) 6 5
O4 Cd1 O1 85.8(3) . .
N3 Cd1 O1 93.84(14) . .
N3 Cd1 O1 93.84(14) 6 .
O2 Cd1 O1 125.8(2) 5 .
O4 Cd1 O2 138.6(3) . .
N3 Cd1 O2 90.75(15) . .
N3 Cd1 O2 90.75(15) 6 .
O2 Cd1 O2 73.0(2) 5 .
O1 Cd1 O2 52.77(19) . .
C15 N3 C11 115.5(6) . .
C15 N3 Cd1 125.3(5) . .
C11 N3 Cd1 119.1(5) . .
N3 C11 C12 123.6(7) . .
N3 C11 H11A 118.2 . .
C12 C11 H11A 118.2 . .
C13 C12 C11 120.9(7) . .
C13 C12 H12A 119.6 . .
C11 C12 H12A 119.6 . .
C12 C13 C14 115.8(6) . .
C12 C13 C13 121.3(4) . 6_565
C14 C13 C13 122.8(4) . 6_565
C13 C14 C15 120.3(7) . .
C13 C14 H14A 119.9 . .
C15 C14 H14A 119.9 . .
N3 C15 C14 123.9(7) . .
N3 C15 H15A 118.1 . .
C14 C15 H15A 118.1 . .
O1 C1 O2 119.5(8) . .
O1 C1 C2 120.5(7) . .
O2 C1 C2 120.0(8) . .
C4 C2 C3 117.0(8) . .
C4 C2 C1 119.8(7) . .
C3 C2 C1 123.2(8) . .
N1 C3 C4 116.6(11) . 5_554
N1 C3 C2 123.0(11) . .
C4 C3 C2 120.4(8) 5_554 .
N1 C3 H3A 3.3 . .
C4 C3 H3A 119.9 5_554 .
C2 C3 H3A 119.7 . .
C3 N1 H3A 9.3 . .
C3 N1 H1A 120.0 . .
H3A N1 H1A 129.3 . .
C3 N1 H1B 120.0 . .
H3A N1 H1B 110.7 . .
H1A N1 H1B 120.0 . .
C3 C4 C2 122.6(7) 5_554 .
C3 C4 H4A 118.7 5_554 .
C2 C4 H4A 118.7 . .
O3 C5 O4 118.4(12) . .
O3 C5 C6 122.7(12) . .
O4 C5 C6 118.9(10) . .
C7 C6 C7 119.4(10) . 6
C7 C6 C5 120.3(5) . .
C7 C6 C5 120.3(5) 6 .
N2 C7 C6 124.5(18) . .
N2 C7 C7 114.9(17) . 2_656
C6 C7 C7 120.3(5) . 2_656
N2 C7 H7A 7.6 . .
C6 C7 H7A 119.9 . .
C7 C7 H7A 119.9 2_656 .
C7 N2 H2A 120.0 . .
C7 N2 H2B 120.0 . .
H2A N2 H2B 120.0 . .
C1 O1 Cd1 97.0(5) . .
C1 O2 Cd1 162.3(6) . 5
C1 O2 Cd1 90.7(5) . .
Cd1 O2 Cd1 107.0(2) 5 .
C5 O4 Cd1 108.5(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 O4 2.239(8) .
Cd1 N3 2.314(5) .
Cd1 N3 2.314(5) 6
Cd1 O2 2.328(5) 5
Cd1 O1 2.379(6) .
Cd1 O2 2.504(6) .
N3 C15 1.301(10) .
N3 C11 1.311(9) .
C11 C12 1.382(10) .
C11 H11A 0.9300 .
C12 C13 1.347(10) .
C12 H12A 0.9300 .
C13 C14 1.347(10) .
C13 C13 1.488(11) 6_565
C14 C15 1.393(10) .
C14 H14A 0.9300 .
C15 H15A 0.9300 .
C1 O1 1.250(11) .
C1 O2 1.265(9) .
C1 C2 1.470(12) .
C2 C4 1.398(13) .
C2 C3 1.404(10) .
C3 N1 1.299(9) .
C3 C4 1.371(13) 5_554
C3 H3A 0.9600 .
N1 H3A 0.3453 .
N1 H1A 0.8600 .
N1 H1B 0.8600 .
C4 C3 1.371(13) 5_554
C4 H4A 0.9300 .
C5 O3 1.183(13) .
C5 O4 1.200(13) .
C5 C6 1.500(15) .
C6 C7 1.363(9) .
C6 C7 1.363(9) 6
C7 N2 1.326(10) .
C7 C7 1.409(15) 2_656
C7 H7A 0.9300 .
N2 H2A 0.8600 .
N2 H2B 0.8600 .
O2 Cd1 2.328(5) 5
