#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/09/7050931.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_7050931
loop_
_publ_author_name
'Gao, En-Qing'
'Wang, Zhe-Ming'
'Liao, Chun-Sheng'
'Yan, Chun-Hua'
_publ_section_title
;
 Topological isomerism in the formation of a novel three-dimensional
 metal-organic polycatenane
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1096
_journal_paper_doi               10.1039/b204324f
_journal_volume                  26
_journal_year                    2002
_chemical_formula_sum            'C17 H14 Cd N8'
_chemical_formula_weight         442.76
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   13.2140(2)
_cell_length_b                   21.7332(4)
_cell_length_c                   28.7125(5)
_cell_measurement_reflns_used    20254
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     8245.7(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.76
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'NONIUS KappaCCD Diffractometer'
_diffrn_measurement_method       CCD
_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  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            36198
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.61
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.075
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3520
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.00037(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         2346
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0925P)²+10.3993P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1493
_reflns_number_gt                1692
_reflns_number_total             2346
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b204324f.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      Fddd
_cod_database_code               7050931
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'
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 0.3750 0.3750 0.074184(15) 0.0630(2) Uani 1 2 d S . .
N1 N 0.4278(3) 0.30524(15) 0.13099(12) 0.0636(8) Uani 1 1 d . . .
N2 N 0.2166(3) 0.32710(19) 0.07226(15) 0.0817(10) Uani 1 1 d . . .
N3 N 0.0693(4) 0.1942(2) -0.01741(18) 0.1041(15) Uani 1 1 d . . .
N4 N 0.0766(5) 0.2833(4) 0.0309(4) 0.186(4) Uani 1 1 d . . .
C1 C 0.6250 0.1250 0.1895(2) 0.0797(18) Uani 1 2 d S . .
H1A H 0.6713 0.1471 0.1699 0.096 Uiso 1 1 d R . .
C2 C 0.5660(4) 0.1709(2) 0.22038(15) 0.0777(12) Uani 1 1 d . . .
H2A H 0.5154 0.1490 0.2384 0.093 Uiso 1 1 calc R . .
H2B H 0.6121 0.1908 0.2419 0.093 Uiso 1 1 calc R . .
C3 C 0.5157(3) 0.21834(18) 0.19075(15) 0.0660(10) Uani 1 1 d . . .
C4 C 0.5584(3) 0.2749(2) 0.18328(15) 0.0736(11) Uani 1 1 d . . .
H4A H 0.6189 0.2851 0.1980 0.088 Uiso 1 1 calc R . .
C5 C 0.5131(3) 0.31660(19) 0.15442(14) 0.0684(10) Uani 1 1 d . . .
H5A H 0.5433 0.3550 0.1509 0.082 Uiso 1 1 calc R . .
C6 C 0.3851(4) 0.2510(2) 0.1383(2) 0.0852(15) Uani 1 1 d . . .
H6A H 0.3248 0.2419 0.1231 0.102 Uiso 1 1 calc R . .
C7 C 0.4266(4) 0.2072(2) 0.1678(2) 0.0920(15) Uani 1 1 d . . .
H7A H 0.3937 0.1698 0.1721 0.110 Uiso 1 1 calc R . .
C8 C 0.0805(4) 0.2346(3) 0.0057(2) 0.0941(16) Uani 1 1 d . . .
C9 C 0.1561(4) 0.3030(2) 0.0527(2) 0.0881(15) 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'
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
_geom_angle_publ_flag
N1 Cd1 N1 91.31(16) 2 . ?
N1 Cd1 N3 179.01(14) 2 29 ?
N1 Cd1 N3 88.58(17) . 29 ?
N1 Cd1 N3 88.58(17) 2 18_665 ?
N1 Cd1 N3 179.01(14) . 18_665 ?
N3 Cd1 N3 91.5(3) 29 18_665 ?
N1 Cd1 N2 89.70(13) 2 2 ?
N1 Cd1 N2 92.19(13) . 2 ?
N3 Cd1 N2 89.33(16) 29 2 ?
N3 Cd1 N2 88.79(16) 18_665 2 ?
N1 Cd1 N2 92.19(13) 2 . ?
N1 Cd1 N2 89.70(13) . . ?
N3 Cd1 N2 88.79(16) 29 . ?
N3 Cd1 N2 89.33(16) 18_665 . ?
N2 Cd1 N2 177.3(2) 2 . ?
C6 N1 C5 116.4(4) . . ?
C6 N1 Cd1 124.2(3) . . ?
C5 N1 Cd1 118.9(3) . . ?
C9 N2 Cd1 150.2(4) . . ?
C8 N3 Cd1 152.2(5) . 29 ?
C8 N4 C9 120.8(6) . . ?
C2 C1 C2 110.1(5) 14_545 . ?
C3 C2 C1 110.1(4) . . ?
C7 C3 C4 116.0(4) . . ?
C7 C3 C2 122.3(4) . . ?
C4 C3 C2 121.7(4) . . ?
C5 C4 C3 120.6(4) . . ?
N1 C5 C4 123.6(4) . . ?
N1 C6 C7 122.6(4) . . ?
C3 C7 C6 120.8(4) . . ?
N3 C8 N4 169.7(6) . . ?
N2 C9 N4 170.2(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N1 2.333(3) 2 ?
Cd1 N1 2.333(3) . ?
Cd1 N3 2.337(4) 29 ?
Cd1 N3 2.337(4) 18_665 ?
Cd1 N2 2.339(4) 2 ?
Cd1 N2 2.339(4) . ?
N1 C6 1.324(5) . ?
N1 C5 1.336(5) . ?
N2 C9 1.109(6) . ?
N3 C8 1.110(6) . ?
N3 Cd1 2.337(4) 29 ?
N4 C8 1.283(7) . ?
N4 C9 1.295(8) . ?
C1 C2 1.546(6) 14_545 ?
C1 C2 1.546(6) . ?
C2 C3 1.492(6) . ?
C3 C7 1.370(7) . ?
C3 C4 1.371(6) . ?
C4 C5 1.366(6) . ?
C6 C7 1.388(7) . ?
