#------------------------------------------------------------------------------
#$Date: 2019-11-24 00:29:10 +0200 (Sun, 24 Nov 2019) $
#$Revision: 235765 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/97/4349720.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_4349720
loop_
_publ_author_name
'Liu, Yu-Ling'
'Zhang, Wen'
_publ_section_title
;
 Cation-templated cyanometallate-based supramolecular rectangular cage
 compounds showing dielectric transitions
;
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1304
_journal_paper_doi               10.1039/C7QI00218A
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety         'C6 H Cd Cl2 Co N6, 2(C H5 N2 S)'
_chemical_formula_sum            'C8 H11 Cd Cl2 Co N10 S2'
_chemical_formula_weight         553.63
_space_group_crystal_system      tetragonal
_space_group_IT_number           130
_space_group_name_Hall           '-P 4a 2ac'
_space_group_name_H-M_alt        'P 4/n c c :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-02-20 deposited with the CCDC.
2017-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.026(6)
_cell_length_b                   15.026(6)
_cell_length_c                   17.267(10)
_cell_measurement_reflns_used    8097
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.4778
_cell_measurement_theta_min      2.9554
_cell_volume                     3899(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39003
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.463
_diffrn_reflns_theta_min         2.711
_exptl_absorpt_coefficient_mu    2.443
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_description       plate
_exptl_crystal_F_000             2072
_refine_diff_density_max         3.959
_refine_diff_density_min         -2.616
_refine_diff_density_rms         0.332
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         2236
_refine_ls_number_restraints     113
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.1389
_refine_ls_R_factor_gt           0.1381
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0233P)²+291.8011P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2312
_refine_ls_wR_factor_ref         0.2315
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2215
_reflns_number_total             2236
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7qi00218a2.cif
_cod_data_source_block           4-113K
_cod_original_cell_volume        3899(4)
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_database_code               4349720
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x, z'
'-x+1/2, -y+1/2, z'
'y, -x+1/2, z'
'x+1/2, -y, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-x, y+1/2, -z+1/2'
'-y, -x, -z+1/2'
'-x, -y, -z'
'y-1/2, -x, -z'
'x-1/2, y-1/2, -z'
'-y, x-1/2, -z'
'-x-1/2, y, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'x, -y-1/2, z-1/2'
'y, x, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cd1 Cd 0.5000 1.0000 0.5000 0.0127(3) Uani 1 2 d S . P
Co1 Co 0.7500 1.2500 0.5000 0.0096(6) Uani 1 4 d DS TU P
Co2 Co 0.7500 0.7500 0.53896(15) 0.0092(6) Uani 1 4 d DS TU P
Cl1 Cl 0.4659(3) 1.0491(2) 0.64213(18) 0.0280(8) Uani 1 1 d . . .
N3 N 0.6172(7) 1.0977(7) 0.4978(7) 0.0149(13) Uani 1 1 d . U .
N2 N 0.5978(7) 0.8840(7) 0.5383(6) 0.0182(18) Uani 1 1 d . U .
N5 N 0.7500 0.7500 0.3626(3) 0.021(4) Uani 1 4 d DS TU P
N1 N 0.7500 0.7500 0.7163(12) 0.020(4) Uani 1 4 d S TU P
N4 N 0.7500 1.2500 0.6740(3) 0.019(2) Uani 1 2 d DS TU P
C1 C 0.7500 0.7500 0.6490(12) 0.013(2) Uani 1 4 d S TU P
C2 C 0.6587(8) 0.8374(9) 0.5397(6) 0.0162(16) Uani 1 1 d . U .
C3 C 0.6637(9) 1.1588(8) 0.4947(8) 0.0148(13) Uani 1 1 d . U .
C4 C 0.7500 1.2500 0.6101(3) 0.0150(18) Uani 1 2 d DS TU P
C5 C 0.7500 0.7500 0.4291(2) 0.011(2) Uani 1 4 d DS TU P
S1 S 0.8264(4) 0.4819(4) 0.6892(3) 0.0514(13) Uani 1 1 d D U .
N6 N 0.6734(10) 0.4902(11) 0.7033(8) 0.054(4) Uani 1 1 d D U .
H6A H 0.6189 0.4948 0.7180 0.065 Uiso 1 1 calc R U .
H6B H 0.6856 0.4818 0.6552 0.065 Uiso 1 1 calc R U .
N7 N 0.7470(13) 0.5079(10) 0.8294(4) 0.054(3) Uani 1 1 d D U .
H7A H 0.7003 0.5144 0.8576 0.065 Uiso 1 1 calc R U .
H7B H 0.7989 0.5093 0.8504 0.065 Uiso 1 1 calc R U .
C6 C 0.7392(6) 0.4961(6) 0.7552(3) 0.054(3) Uani 1 1 d D U .
H2 H 0.7501 0.7500 0.3115 0.065 Uiso 1 4 d DR U P
H1 H 0.7501 1.2500 0.7500 0.065 Uiso 1 4 d DR U P
H3 H 0.8793 0.4867 0.7283 0.065 Uiso 1 1 d R U .
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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'
S S 0.1246 0.1234 '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
N3 Cd1 N3 180.0 9_676 .
N3 Cd1 N2 90.0(4) 9_676 .
N3 Cd1 N2 90.0(4) . .
N3 Cd1 N2 90.0(4) 9_676 9_676
N3 Cd1 N2 90.0(4) . 9_676
N2 Cd1 N2 180.0 . 9_676
N3 Cd1 Cl1 90.8(3) 9_676 .
N3 Cd1 Cl1 89.2(3) . .
N2 Cd1 Cl1 93.9(3) . .
N2 Cd1 Cl1 86.1(3) 9_676 .
N3 Cd1 Cl1 89.2(3) 9_676 9_676
N3 Cd1 Cl1 90.8(3) . 9_676
N2 Cd1 Cl1 86.1(3) . 9_676
N2 Cd1 Cl1 93.9(3) 9_676 9_676
Cl1 Cd1 Cl1 180.0 . 9_676
C3 Co1 C3 90.14(4) 3_675 12_766
C3 Co1 C3 90.14(4) 3_675 10_576
C3 Co1 C3 174.4(8) 12_766 10_576
C3 Co1 C3 174.4(8) 3_675 .
C3 Co1 C3 90.14(4) 12_766 .
C3 Co1 C3 90.14(4) 10_576 .
C3 Co1 C4 87.2(4) 3_675 10_576
C3 Co1 C4 92.8(4) 12_766 10_576
C3 Co1 C4 92.8(4) 10_576 10_576
C3 Co1 C4 87.2(4) . 10_576
C3 Co1 C4 92.8(4) 3_675 .
C3 Co1 C4 87.2(4) 12_766 .
C3 Co1 C4 87.2(4) 10_576 .
C3 Co1 C4 92.8(4) . .
C4 Co1 C4 180.0 10_576 .
C5 Co2 C2 90.4(3) . 4_565
C5 Co2 C2 90.4(3) . 2_655
C2 Co2 C2 179.3(7) 4_565 2_655
C5 Co2 C2 90.4(3) . 3_665
C2 Co2 C2 89.998(8) 4_565 3_665
C2 Co2 C2 89.998(6) 2_655 3_665
C5 Co2 C2 90.4(3) . .
C2 Co2 C2 89.997(6) 4_565 .
C2 Co2 C2 89.998(7) 2_655 .
C2 Co2 C2 179.3(7) 3_665 .
C5 Co2 C1 180.0 . .
C2 Co2 C1 89.6(3) 4_565 .
C2 Co2 C1 89.6(3) 2_655 .
C2 Co2 C1 89.6(3) 3_665 .
C2 Co2 C1 89.6(3) . .
C3 N3 Cd1 167.0(11) . .
C2 N2 Cd1 160.6(10) . .
C5 N5 H2 179.9 . .
C4 N4 H1 179.9 . .
C4 N4 H1 179.9 . .
H1 N4 H1 0.0 . .
N1 C1 Co2 180.0 . .
N2 C2 Co2 173.5(13) . .
N3 C3 Co1 171.8(13) . .
N4 C4 Co1 180.0 . .
N5 C5 Co2 180.0 . .
C6 S1 H3 98.0 . .
C6 N6 H6A 120.0 . .
C6 N6 H6B 120.0 . .
H6A N6 H6B 120.0 . .
C6 N7 H7A 120.0 . .
C6 N7 H7B 120.0 . .
H7A N7 H7B 120.0 . .
N7 C6 N6 137.4(13) . .
N7 C6 S1 126.3(11) . .
N6 C6 S1 96.2(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 N3 2.293(10) 9_676
Cd1 N3 2.293(10) .
Cd1 N2 2.373(10) .
Cd1 N2 2.373(10) 9_676
Cd1 Cl1 2.614(3) .
Cd1 Cl1 2.614(3) 9_676
Co1 C3 1.889(11) 3_675
Co1 C3 1.889(11) 12_766
Co1 C3 1.889(11) 10_576
Co1 C3 1.889(11) .
Co1 C4 1.902(5) 10_576
Co1 C4 1.902(5) .
Co2 C5 1.897(3) .
Co2 C2 1.899(11) 4_565
Co2 C2 1.899(11) 2_655
Co2 C2 1.899(11) 3_665
Co2 C2 1.899(11) .
Co2 C1 1.90(2) .
N3 C3 1.155(15) .
N2 C2 1.153(15) .
N5 C5 1.148(4) .
N5 H2 0.8820 .
N1 C1 1.16(3) .
N4 C4 1.103(5) .
N4 H1 1.3124 .
N4 H1 1.3124 .
S1 C6 1.749(5) .
S1 H3 1.0462 .
N6 C6 1.338(5) .
N6 H6A 0.8600 .
N6 H6B 0.8600 .
N7 C6 1.300(5) .
N7 H7A 0.8600 .
N7 H7B 0.8600 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
S1 H3 Cl1 1.05 2.58 3.550(7) 153.5 8_766
N5 H2 N1 0.88 1.64 2.53(2) 179.9 13_755
N7 H7B Cl1 0.86 2.32 3.13(2) 157.0 8_766
N7 H7A Cl1 0.86 2.55 3.30(2) 145.5 7_646
N6 H6A Cl1 0.86 2.85 3.506(19) 134.4 7_646
N6 H6A Cl1 0.86 2.88 3.525(12) 133.5 2_655
