#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/13/7011365.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_7011365
loop_
_publ_author_name
'Yoshikawa, Hirofumi'
'Nishikiori, Shin-ichi'
'Watanabe, Tokuko'
'Ishida, Toshimasa'
'Watanabe, Go'
'Murakami, Makoto'
'Suwinska, Kinga'
'Luboradzki, Roman'
'Lipkowski, Janusz'
_publ_section_title
;
 Polycyano--polycadmate host clathrates including a methylviologen
 dication. Syntheses, crystal structures and photo-induced reduction of
 methylviologen dication
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1907
_journal_paper_doi               10.1039/b111059d
_journal_year                    2002
_chemical_formula_structural     'Cd5 (C12 N12)(C12 N2 H14)(C7 H8)'
_chemical_formula_sum            'C31 H22 Cd5 N14'
_chemical_formula_weight         1152.67
_space_group_IT_number           74
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2 2b'
_symmetry_space_group_name_H-M   'I c m m'
_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            4
_cell_length_a                   11.4002(4)
_cell_length_b                   23.4038(11)
_cell_length_c                   15.6457(4)
_cell_measurement_temperature    293(2)
_cell_volume                     4174.4(3)
_computing_molecular_graphics    'ORTEP 3 for windows'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       ω
_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  0.035
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            34097
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    2.526
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.840
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.605
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.896
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         3229
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.896
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0276
_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)+(0.0453P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0741
_reflns_number_gt                2559
_reflns_number_total             3229
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b111059d.txt
_cod_data_source_block           III-2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_sg_symbol_H-M      Icmm
_cod_database_code               7011365
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y+1/2, -z'
'-x, -y, z'
'-x, y+1/2, -z'
'x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1, -z+1/2'
'-x, -y, -z'
'-x, y-1/2, z'
'x, y, -z'
'x, -y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.0000 0.0000 0.0000 0.03618(8) Uani 1 4 d S . .
Cd2 Cd 0.2500 0.130897(10) 0.2500 0.03824(7) Uani 1 2 d S . .
Cd3 Cd 0.40354(2) -0.134988(15) 0.0000 0.05712(10) Uani 1 2 d S . .
C1 C 0.1477(2) 0.08241(11) 0.15107(15) 0.0463(5) Uani 1 1 d . . .
N1 N 0.0925(2) 0.05613(10) 0.10555(14) 0.0532(5) Uani 1 1 d . . .
C2 C 0.2412(3) -0.08602(19) 0.0000 0.0543(9) Uani 1 2 d S . .
N2 N 0.1586(3) -0.06008(16) 0.0000 0.0586(8) Uani 1 2 d S . .
C3 C 0.4904(3) 0.12616(18) 0.1147(2) 0.0753(10) Uani 1 1 d . . .
N3 N 0.4263(3) 0.12695(18) 0.1659(2) 0.0949(12) Uani 1 1 d . . .
CN1 C 0.2500 0.22587(15) 0.2500 0.0553(9) Uani 1 2 d S . .
CN2 C 0.3513(4) -0.2259(2) 0.0000 0.0975(18) Uani 1 2 d S . .
N101 N 0.7500 0.10166(16) 0.2500 0.0755(13) Uani 1 2 d S . .
C101 C 0.6683(4) 0.12915(15) 0.2903(3) 0.0844(12) Uani 1 1 d . . .
H101 H 0.6109 0.1086 0.3192 0.101 Uiso 1 1 calc R . .
C102 C 0.6638(3) 0.18796(13) 0.2916(2) 0.0669(8) Uani 1 1 d . . .
H102 H 0.6035 0.2067 0.3201 0.080 Uiso 1 1 calc R . .
C103 C 0.7500 0.21882(16) 0.2500 0.0438(7) Uani 1 2 d S . .
C111 C 0.7500 0.0384(3) 0.2500 0.171(6) Uani 1 2 d S . .
H111 H 0.7269 0.0247 0.1947 0.257 Uiso 0.50 1 calc PR . .
H121 H 0.6958 0.0247 0.2923 0.257 Uiso 0.50 1 calc PR . .
H131 H 0.8273 0.0247 0.2631 0.257 Uiso 0.50 1 calc PR . .
C201 C 0.3056(7) 0.2500 0.5000 0.0640(15) Uani 1 4 d S . .
C202 C 0.3617(7) 0.2015(2) 0.5000 0.0825(16) Uani 1 2 d S . .
H202 H 0.3188 0.1676 0.5000 0.099 Uiso 1 2 calc SR . .
C203 C 0.4784(7) 0.1987(4) 0.5000 0.114(3) Uani 1 2 d S . .
H203 H 0.5158 0.1634 0.5000 0.136 Uiso 1 2 calc SR . .
C204 C 0.5458(7) 0.2500 0.5000 0.166(8) Uani 1 4 d S . .
H204 H 0.6274 0.2500 0.5000 0.199 Uiso 1 4 calc SR . .
C205 C 0.1683(9) 0.2500 0.5000 0.144(6) Uani 1 4 d S . .
H215 H 0.1403 0.2478 0.4422 0.217 Uiso 0.25 1 calc PR . .
H225 H 0.1403 0.2845 0.5260 0.217 Uiso 0.25 1 calc PR . .
H235 H 0.1403 0.2177 0.5318 0.217 Uiso 0.25 1 calc PR . .
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
_geom_angle_publ_flag
N2 Cd1 N2 180.0 9 . ?
N2 Cd1 N1 90.64(9) 9 . ?
N2 Cd1 N1 89.36(9) . . ?
N2 Cd1 N1 90.64(9) 9 11 ?
N2 Cd1 N1 89.36(9) . 11 ?
N1 Cd1 N1 88.85(12) . 11 ?
N2 Cd1 N1 89.36(9) 9 9 ?
N2 Cd1 N1 90.64(9) . 9 ?
N1 Cd1 N1 180.0 . 9 ?
N1 Cd1 N1 91.15(12) 11 9 ?
N2 Cd1 N1 89.36(9) 9 3 ?
N2 Cd1 N1 90.64(9) . 3 ?
N1 Cd1 N1 91.15(12) . 3 ?
N1 Cd1 N1 180.0 11 3 ?
N1 Cd1 N1 88.85(12) 9 3 ?
CN1 Cd2 C1 120.35(6) . . ?
CN1 Cd2 C1 120.35(6) . 8_545 ?
C1 Cd2 C1 119.29(13) . 8_545 ?
CN1 Cd2 N3 92.20(10) . . ?
C1 Cd2 N3 92.12(12) . . ?
C1 Cd2 N3 85.65(11) 8_545 . ?
CN1 Cd2 N3 92.20(10) . 8_545 ?
C1 Cd2 N3 85.65(11) . 8_545 ?
C1 Cd2 N3 92.12(12) 8_545 8_545 ?
N3 Cd2 N3 175.6(2) . 8_545 ?
C3 Cd3 C3 111.30(19) 3_655 9_655 ?
C3 Cd3 C2 115.02(11) 3_655 . ?
C3 Cd3 C2 115.02(11) 9_655 . ?
C3 Cd3 CN2 103.97(13) 3_655 . ?
C3 Cd3 CN2 103.97(13) 9_655 . ?
C2 Cd3 CN2 106.14(17) . . ?
N1 C1 Cd2 175.4(2) . . ?
C1 N1 Cd1 172.5(2) . . ?
N2 C2 Cd3 179.0(4) . . ?
C2 N2 Cd1 174.9(4) . . ?
N3 C3 Cd3 169.4(4) . 9_655 ?
C3 N3 Cd2 165.6(3) . . ?
CN1 CN1 Cd2 180.0 13 . ?
CN2 CN2 Cd3 164.37(12) 2_545 . ?
C101 N101 C101 120.5(4) 8_645 . ?
C101 N101 C111 119.8(2) 8_645 . ?
C101 N101 C111 119.8(2) . . ?
N101 C101 C102 122.0(4) . . ?
C101 C102 C103 119.3(3) . . ?
C102 C103 C102 117.0(4) . 8_645 ?
C102 C103 C103 121.51(19) . 12_565 ?
C102 C103 C103 121.51(19) 8_645 12_565 ?
C202 C201 C202 121.2(9) 12_565 . ?
C202 C201 C205 119.4(4) 12_565 . ?
C202 C201 C205 119.4(4) . . ?
C201 C202 C203 122.2(7) . . ?
C202 C203 C204 119.8(6) . . ?
C203 C204 C203 114.7(7) . 12_565 ?
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 N2 2.290(3) 9 ?
Cd1 N2 2.290(3) . ?
Cd1 N1 2.359(2) . ?
Cd1 N1 2.359(2) 11 ?
Cd1 N1 2.359(2) 9 ?
Cd1 N1 2.359(2) 3 ?
Cd2 CN1 2.223(4) . ?
Cd2 C1 2.245(2) . ?
Cd2 C1 2.245(2) 8_545 ?
Cd2 N3 2.404(3) . ?
Cd2 N3 2.404(3) 8_545 ?
Cd3 C3 2.174(4) 3_655 ?
Cd3 C3 2.174(4) 9_655 ?
Cd3 C2 2.177(4) . ?
Cd3 CN2 2.208(6) . ?
C1 N1 1.132(3) . ?
C2 N2 1.121(5) . ?
C3 N3 1.084(4) . ?
C3 Cd3 2.174(4) 9_655 ?
CN1 CN1 1.129(7) 13 ?
CN2 CN2 1.130(11) 2_545 ?
N101 C101 1.296(5) 8_645 ?
N101 C101 1.296(5) . ?
N101 C111 1.481(7) . ?
C101 C102 1.377(5) . ?
C102 C103 1.382(4) . ?
C103 C102 1.382(4) 8_645 ?
C103 C103 1.459(7) 12_565 ?
C201 C202 1.304(7) 12_565 ?
C201 C202 1.304(7) . ?
C201 C205 1.564(12) . ?
C202 C203 1.332(11) . ?
C203 C204 1.426(11) . ?
C204 C203 1.426(11) 12_565 ?
