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#$Date: 2016-03-24 01:32:20 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179534 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/03/4500301.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_4500301
loop_
_publ_author_name
'Su, Zhi'
'Fan, Jian'
'Chen, Min'
'Okamura, Taka-aki'
'Sun, Wei-Yin'
_publ_section_title
;
 Syntheses, Characterization, and Properties of Three-Dimensional Pillared
 Frameworks with Entanglement
;
_journal_issue                   4
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1159
_journal_paper_doi               10.1021/cg101365v
_journal_volume                  11
_journal_year                    2011
_chemical_formula_moiety         'C17 H14 Cd N4 O4'
_chemical_formula_sum            'C17 H14 Cd N4 O4'
_chemical_formula_weight         450.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.591(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.0110(8)
_cell_length_b                   17.257(2)
_cell_length_c                   14.755(2)
_cell_measurement_reflns_used    2664
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.85
_cell_measurement_theta_min      2.73
_cell_volume                     1530.5(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7658
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    1.462
_exptl_absorpt_correction_T_max  0.8676
_exptl_absorpt_correction_T_min  0.7587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs,bruker(2000)
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.956
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.867
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0427
_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)+(0.0278P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0723
_reflns_number_gt                2259
_reflns_number_total             2759
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg101365v_si_002.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4500301
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
C1 C 1.0182(6) 0.9730(2) 0.6406(3) 0.0231(9) Uani 1 1 d .
C2 C 1.1195(6) 0.9344(2) 0.5704(3) 0.0253(9) Uani 1 1 d .
H2 H 1.2512 0.9533 0.5463 0.030 Uiso 1 1 calc R
C3 C 1.0252(6) 0.8681(2) 0.5362(3) 0.0240(9) Uani 1 1 d .
C4 C 0.8304(6) 0.8389(2) 0.5708(3) 0.0264(9) Uani 1 1 d .
H4 H 0.7659 0.7945 0.5464 0.032 Uiso 1 1 calc R
C5 C 0.7324(6) 0.8773(2) 0.6429(3) 0.0241(9) Uani 1 1 d .
C6 C 0.8221(6) 0.9448(2) 0.6772(3) 0.0246(9) Uani 1 1 d .
H6 H 0.7526 0.9710 0.7241 0.030 Uiso 1 1 calc R
C7 C 1.1348(6) 1.0420(2) 0.6826(3) 0.0276(10) Uani 1 1 d .
C8 C 1.1079(7) 0.7523(2) 0.4396(3) 0.0338(11) Uani 1 1 d .
H8 H 1.0165 0.7159 0.4671 0.041 Uiso 1 1 calc R
C9 C 1.2411(7) 0.7407(2) 0.3682(3) 0.0327(10) Uani 1 1 d .
H9 H 1.2554 0.6940 0.3374 0.039 Uiso 1 1 calc R
C10 C 1.2818(7) 0.8584(2) 0.4067(3) 0.0316(10) Uani 1 1 d .
H10 H 1.3290 0.9097 0.4090 0.038 Uiso 1 1 calc R
C11 C 0.4077(6) 0.8791(2) 0.7473(3) 0.0278(10) Uani 1 1 d .
H11 H 0.4232 0.9289 0.7706 0.033 Uiso 1 1 calc R
C12 C 0.2529(7) 0.8263(2) 0.7694(3) 0.0296(10) Uani 1 1 d .
H12 H 0.1410 0.8343 0.8115 0.035 Uiso 1 1 calc R
C13 C 0.4575(6) 0.7720(2) 0.6713(3) 0.0290(10) Uani 1 1 d .
H13 H 0.5187 0.7358 0.6322 0.035 Uiso 1 1 calc R
C14 C -0.3125(8) 0.5412(2) 0.5388(3) 0.0442(12) Uani 1 1 d .
H14 H -0.2249 0.5402 0.4832 0.053 Uiso 1 1 calc R
C15 C -0.3473(7) 0.4575(2) 0.5604(3) 0.0441(12) Uani 1 1 d .
H15A H -0.4221 0.4531 0.6181 0.053 Uiso 1 1 calc R
H15B H -0.2041 0.4320 0.5660 0.053 Uiso 1 1 calc R
C16 C -0.5141(8) 0.5829(2) 0.5127(3) 0.0487(13) Uani 1 1 d .
H16A H -0.4729 0.6340 0.4911 0.058 Uiso 1 1 calc R
H16B H -0.6051 0.5899 0.5660 0.058 Uiso 1 1 calc R
C17 C -0.1635(7) 0.5831(2) 0.6063(3) 0.0295(10) Uani 1 1 d .
Cd1 Cd 0.09308(4) 0.648586(15) 0.73839(2) 0.02237(11) Uani 1 1 d .
N1 N 1.3528(5) 0.80749(18) 0.3474(2) 0.0287(8) Uani 1 1 d .
N2 N 1.1332(5) 0.82763(18) 0.4636(2) 0.0248(8) Uani 1 1 d .
N3 N 0.2828(5) 0.75915(17) 0.7215(2) 0.0274(8) Uani 1 1 d .
N4 N 0.5379(5) 0.84454(17) 0.6833(2) 0.0231(7) Uani 1 1 d .
O1 O 1.3143(5) 1.06254(17) 0.6465(2) 0.0427(8) Uani 1 1 d .
O2 O 1.0590(5) 1.07380(17) 0.7502(2) 0.0388(8) Uani 1 1 d .
O3 O -0.1517(5) 0.65560(14) 0.6053(2) 0.0365(7) Uani 1 1 d .
O4 O -0.0470(4) 0.54477(16) 0.6613(2) 0.0376(7) 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'
Cd Cd -0.8075 1.2024 '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
C2 C1 C6 120.4(4) . .
C2 C1 C7 118.8(3) . .
C6 C1 C7 120.5(4) . .
C3 C2 C1 119.7(4) . .
C3 C2 H2 120.2 . .
C1 C2 H2 120.2 . .
C2 C3 C4 121.3(4) . .
C2 C3 N2 119.4(3) . .
C4 C3 N2 119.3(3) . .
C3 C4 C5 118.5(4) . .
C3 C4 H4 120.7 . .
C5 C4 H4 120.7 . .
C6 C5 C4 121.1(4) . .
C6 C5 N4 119.8(4) . .
C4 C5 N4 119.0(3) . .
C5 C6 C1 118.9(4) . .
C5 C6 H6 120.5 . .
C1 C6 H6 120.5 . .
O2 C7 O1 122.9(4) . .
O2 C7 C1 120.7(4) . .
O1 C7 C1 116.4(4) . .
O2 C7 Cd1 64.9(2) . 2_656
O1 C7 Cd1 58.4(2) . 2_656
C1 C7 Cd1 169.8(3) . 2_656
C9 C8 N2 106.4(4) . .
C9 C8 H8 126.8 . .
N2 C8 H8 126.8 . .
C8 C9 N1 110.3(4) . .
C8 C9 H9 124.9 . .
N1 C9 H9 124.9 . .
N1 C10 N2 112.0(3) . .
N1 C10 H10 124.0 . .
N2 C10 H10 124.0 . .
C12 C11 N4 105.9(3) . .
C12 C11 H11 127.0 . .
N4 C11 H11 127.0 . .
C11 C12 N3 110.6(3) . .
C11 C12 H12 124.7 . .
N3 C12 H12 124.7 . .
N3 C13 N4 111.8(3) . .
N3 C13 H13 124.1 . .
N4 C13 H13 124.1 . .
C16 C14 C15 114.6(4) . .
C16 C14 C17 114.9(4) . .
C15 C14 C17 113.9(4) . .
C16 C14 H14 103.9 . .
C15 C14 H14 103.9 . .
C17 C14 H14 103.9 . .
C14 C15 C16 111.6(4) . 3_466
C14 C15 H15A 109.3 . .
C16 C15 H15A 109.3 3_466 .
C14 C15 H15B 109.3 . .
C16 C15 H15B 109.3 3_466 .
H15A C15 H15B 108.0 . .
C14 C16 C15 114.0(4) . 3_466
C14 C16 H16A 108.7 . .
C15 C16 H16A 108.7 3_466 .
C14 C16 H16B 108.7 . .
C15 C16 H16B 108.7 3_466 .
H16A C16 H16B 107.6 . .
O3 C17 O4 120.1(4) . .
O3 C17 C14 120.1(4) . .
O4 C17 C14 119.7(4) . .
N3 Cd1 O4 143.19(12) . .
N3 Cd1 N1 96.98(11) . 4_476
O4 Cd1 N1 112.11(11) . 4_476
N3 Cd1 O1 120.58(12) . 2_646
O4 Cd1 O1 86.95(11) . 2_646
N1 Cd1 O1 81.17(11) 4_476 2_646
N3 Cd1 O3 99.86(11) . .
O4 Cd1 O3 54.67(9) . .
N1 Cd1 O3 99.70(11) 4_476 .
O1 Cd1 O3 139.28(10) 2_646 .
N3 Cd1 O2 91.21(10) . 2_646
O4 Cd1 O2 86.05(10) . 2_646
N1 Cd1 O2 131.58(11) 4_476 2_646
O1 Cd1 O2 54.34(9) 2_646 2_646
O3 Cd1 O2 125.78(10) . 2_646
N3 Cd1 C7 108.66(12) . 2_646
O4 Cd1 C7 84.23(11) . 2_646
N1 Cd1 C7 107.61(12) 4_476 2_646
O1 Cd1 C7 27.55(11) 2_646 2_646
O3 Cd1 C7 137.14(10) . 2_646
O2 Cd1 C7 26.91(10) 2_646 2_646
C10 N1 C9 104.5(3) . .
C10 N1 Cd1 117.1(3) . 4_775
C9 N1 Cd1 138.2(3) . 4_775
C10 N2 C8 106.9(3) . .
C10 N2 C3 125.6(3) . .
C8 N2 C3 127.5(3) . .
C13 N3 C12 105.0(3) . .
C13 N3 Cd1 128.3(3) . .
C12 N3 Cd1 126.4(3) . .
C13 N4 C11 106.7(3) . .
C13 N4 C5 127.0(3) . .
C11 N4 C5 126.1(3) . .
C7 O1 Cd1 94.0(2) . 2_656
C7 O2 Cd1 88.2(2) . 2_656
C17 O3 Cd1 88.5(3) . .
C17 O4 Cd1 96.3(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.379(5) .
C1 C6 1.390(5) .
C1 C7 1.511(5) .
C2 C3 1.371(5) .
C2 H2 0.9300 .
C3 C4 1.377(5) .
C3 N2 1.440(5) .
C4 C5 1.389(5) .
C4 H4 0.9300 .
C5 C6 1.378(5) .
C5 N4 1.435(5) .
C6 H6 0.9300 .
C7 O2 1.230(5) .
C7 O1 1.259(4) .
C7 Cd1 2.716(4) 2_656
C8 C9 1.345(5) .
C8 N2 1.355(5) .
C8 H8 0.9300 .
C9 N1 1.371(5) .
C9 H9 0.9300 .
C10 N1 1.314(5) .
C10 N2 1.341(5) .
C10 H10 0.9300 .
C11 C12 1.345(5) .
C11 N4 1.368(5) .
C11 H11 0.9300 .
C12 N3 1.371(5) .
C12 H12 0.9300 .
C13 N3 1.309(5) .
C13 N4 1.352(4) .
C13 H13 0.9300 .
C14 C16 1.458(6) .
C14 C15 1.494(5) .
C14 C17 1.515(6) .
C14 H14 0.9800 .
C15 C16 1.525(6) 3_466
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C16 C15 1.525(6) 3_466
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C17 O3 1.254(4) .
C17 O4 1.255(5) .
Cd1 N3 2.238(3) .
Cd1 O4 2.279(3) .
Cd1 N1 2.301(3) 4_476
Cd1 O1 2.320(3) 2_646
Cd1 O3 2.445(3) .
Cd1 O2 2.462(3) 2_646
Cd1 C7 2.716(4) 2_646
N1 Cd1 2.301(3) 4_775
O1 Cd1 2.320(3) 2_656
O2 Cd1 2.462(3) 2_656
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C6 C1 C2 C3 0.4(6) . .
C7 C1 C2 C3 174.8(4) . .
C1 C2 C3 C4 -0.1(6) . .
C1 C2 C3 N2 -179.3(3) . .
C2 C3 C4 C5 -1.3(6) . .
N2 C3 C4 C5 177.9(4) . .
C3 C4 C5 C6 2.5(6) . .
C3 C4 C5 N4 -175.9(3) . .
C4 C5 C6 C1 -2.2(6) . .
N4 C5 C6 C1 176.1(3) . .
C2 C1 C6 C5 0.7(6) . .
C7 C1 C6 C5 -173.6(4) . .
C2 C1 C7 O2 -173.8(4) . .
C6 C1 C7 O2 0.6(6) . .
C2 C1 C7 O1 3.9(5) . .
C6 C1 C7 O1 178.3(4) . .
C2 C1 C7 Cd1 -53.0(18) . 2_656
C6 C1 C7 Cd1 121.4(16) . 2_656
N2 C8 C9 N1 0.8(5) . .
N4 C11 C12 N3 0.4(5) . .
C16 C14 C15 C16 48.5(7) . 3_466
C17 C14 C15 C16 -176.3(4) . 3_466
C15 C14 C16 C15 -49.7(7) . 3_466
C17 C14 C16 C15 175.6(4) . 3_466
C16 C14 C17 O3 -32.6(6) . .
C15 C14 C17 O3 -167.6(4) . .
C16 C14 C17 O4 149.5(4) . .
C15 C14 C17 O4 14.5(6) . .
N2 C10 N1 C9 0.2(5) . .
N2 C10 N1 Cd1 176.4(3) . 4_775
C8 C9 N1 C10 -0.6(5) . .
C8 C9 N1 Cd1 -175.5(3) . 4_775
N1 C10 N2 C8 0.3(5) . .
N1 C10 N2 C3 179.8(4) . .
C9 C8 N2 C10 -0.6(5) . .
C9 C8 N2 C3 179.9(4) . .
C2 C3 N2 C10 -21.0(6) . .
C4 C3 N2 C10 159.8(4) . .
C2 C3 N2 C8 158.4(4) . .
C4 C3 N2 C8 -20.8(6) . .
N4 C13 N3 C12 -1.3(5) . .
N4 C13 N3 Cd1 -175.3(3) . .
C11 C12 N3 C13 0.6(5) . .
C11 C12 N3 Cd1 174.7(3) . .
O4 Cd1 N3 C13 -41.7(4) . .
N1 Cd1 N3 C13 175.5(4) 4_476 .
O1 Cd1 N3 C13 91.6(4) 2_646 .
O3 Cd1 N3 C13 -83.4(4) . .
O2 Cd1 N3 C13 43.3(4) 2_646 .
C7 Cd1 N3 C13 64.2(4) 2_646 .
O4 Cd1 N3 C12 145.5(3) . .
N1 Cd1 N3 C12 2.7(3) 4_476 .
O1 Cd1 N3 C12 -81.1(3) 2_646 .
O3 Cd1 N3 C12 103.9(3) . .
O2 Cd1 N3 C12 -129.4(3) 2_646 .
C7 Cd1 N3 C12 -108.6(3) 2_646 .
N3 C13 N4 C11 1.6(5) . .
N3 C13 N4 C5 176.9(4) . .
C12 C11 N4 C13 -1.1(4) . .
C12 C11 N4 C5 -176.5(4) . .
C6 C5 N4 C13 -164.9(4) . .
C4 C5 N4 C13 13.5(6) . .
C6 C5 N4 C11 9.6(6) . .
C4 C5 N4 C11 -172.0(4) . .
O2 C7 O1 Cd1 7.7(4) . 2_656
C1 C7 O1 Cd1 -170.0(3) . 2_656
O1 C7 O2 Cd1 -7.2(4) . 2_656
C1 C7 O2 Cd1 170.3(3) . 2_656
O4 C17 O3 Cd1 -5.6(4) . .
C14 C17 O3 Cd1 176.5(4) . .
N3 Cd1 O3 C17 154.0(2) . .
O4 Cd1 O3 C17 3.2(2) . .
N1 Cd1 O3 C17 -107.1(2) 4_476 .
O1 Cd1 O3 C17 -19.4(3) 2_646 .
O2 Cd1 O3 C17 55.3(3) 2_646 .
C7 Cd1 O3 C17 22.4(3) 2_646 .
O3 C17 O4 Cd1 6.0(4) . .
C14 C17 O4 Cd1 -176.1(3) . .
N3 Cd1 O4 C17 -56.6(3) . .
N1 Cd1 O4 C17 83.0(3) 4_476 .
O1 Cd1 O4 C17 162.2(3) 2_646 .
O3 Cd1 O4 C17 -3.3(2) . .
O2 Cd1 O4 C17 -143.4(3) 2_646 .
C7 Cd1 O4 C17 -170.3(3) 2_646 .
