#------------------------------------------------------------------------------
#$Date: 2019-11-24 00:29:10 +0200 (Sun, 24 Nov 2019) $
#$Revision: 235765 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/97/4349724.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_4349724
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
'2(C3 H0.50 Cd0.50 Cl Co0.50 N3), 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           129
_space_group_name_Hall           '-P 4a 2a'
_space_group_name_H-M_alt        'P 4/n m m :2'
_atom_sites_solution_hydrogens   difmap
_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            4
_cell_length_a                   15.0723(16)
_cell_length_b                   15.0723(16)
_cell_length_c                   8.6294(9)
_cell_measurement_reflns_used    5463
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.5281
_cell_measurement_theta_min      3.0201
_cell_volume                     1960.4(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_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  0.0473
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            20779
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         2.720
_exptl_absorpt_coefficient_mu    2.429
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_description       plate
_exptl_crystal_F_000             1104
_refine_diff_density_max         1.882
_refine_diff_density_min         -3.584
_refine_diff_density_rms         0.275
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         1271
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0943
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1110P)²+53.6323P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2432
_refine_ls_wR_factor_ref         0.2447
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1227
_reflns_number_total             1271
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7qi00218a2.cif
_cod_data_source_block           4-273K
_cod_original_cell_volume        1960.4(5)
_cod_original_sg_symbol_H-M      'P 4/n m m'
_cod_database_code               4349724
_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'
'y+1/2, x+1/2, -z'
'-x, y+1/2, -z'
'-y, -x, -z'
'-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'
'-y-1/2, -x-1/2, z'
'x, -y-1/2, z'
'y, x, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.1601(6) 0.1601(6) 1.0730(15) 0.030(2) Uani 1 2 d S TU P
C2 C 0.2500 0.2500 1.293(3) 0.026(4) Uani 1 8 d S TU P
C3 C 0.2500 0.2500 0.854(3) 0.035(4) Uani 1 8 d S TU P
C4 C 0.1607(6) -0.1607(6) 1.0000 0.028(2) Uani 1 2 d S TU P
C5 C 0.2500 -0.2500 0.7775(5) 0.028(3) Uani 1 4 d DS TU P
C6 C 0.5073(4) 0.2500 0.4886(7) 0.069(7) Uani 1 2 d DS TU P
Cd1 Cd 0.0000 0.0000 1.0000 0.0197(4) Uani 1 4 d S T P
Cl1 Cl 0.0405(2) 0.0405(2) 0.7137(5) 0.0481(10) Uani 1 2 d S T P
Co1 Co 0.2500 0.2500 1.0736(3) 0.0137(6) Uani 1 8 d S T P
Co2 Co 0.2500 -0.2500 1.0000 0.0131(6) Uani 1 8 d DS T P
H1 H 0.2500 0.2500 0.621(3) 0.016 Uiso 1 8 d DS U P
H2 H 0.2500 -0.2500 0.5000 0.016 Uiso 1 8 d DS U P
N1 N 0.1071(6) 0.1071(6) 1.0714(15) 0.036(2) Uani 1 2 d S TU P
N2 N 0.2500 0.2500 1.425(3) 0.033(4) Uani 1 8 d S TU P
N3 N 0.2500 0.2500 0.723(2) 0.036(4) Uani 1 8 d DS TU P
N4 N 0.1078(5) -0.1078(5) 1.0000 0.034(2) Uani 1 2 d S TU P
N5 N 0.2500 -0.2500 0.6473(6) 0.035(3) Uani 1 4 d DS TU P
N6 N 0.5148 0.1752 0.4116(6) 0.095(2) Uani 0.5 1 d DR U P
H6A H 0.5230 0.1840 0.3143 0.114 Uiso 0.5 1 d R U P
H6B H 0.5095 0.1259 0.4615 0.114 Uiso 0.5 1 d R U P
N7 N 0.4941(6) 0.2500 0.6397(8) 0.095(2) Uani 1 2 d DS TU P
H7A H 0.4903 0.2983 0.6924 0.114 Uiso 1 1 d R U .
S1 S 0.5154(6) 0.3497 0.3877(8) 0.095(2) Uani 0.5 1 d DR U P
H3 H 0.5067 0.4000 0.4782 0.114 Uiso 0.5 1 d R U P
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'
O O 0.0106 0.0060 '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
N1 C1 Co1 179.4(13) . .
N2 C2 Co1 180.0 . .
N3 C3 Co1 180.0 . .
N4 C4 Co2 180.0(10) . .
N5 C5 Co2 180.0 . .
N6 C6 N6 118.3(4) 15_565 .
N6 C6 N7 120.9(2) 15_565 .
N6 C6 N7 120.8(2) . .
N6 C6 S1 1.0(3) 15_565 .
N6 C6 S1 118.9(2) . .
N7 C6 S1 120.29(8) . .
N6 C6 S1 118.9(2) 15_565 15_565
N6 C6 S1 1.0(3) . 15_565
N7 C6 S1 120.29(8) . 15_565
S1 C6 S1 119.41(17) . 15_565
N4 Cd1 N4 180.0 . 9_557
N4 Cd1 N1 90.000(2) . .
N4 Cd1 N1 90.000(2) 9_557 .
N4 Cd1 N1 90.000(2) . 9_557
N4 Cd1 N1 90.000(2) 9_557 9_557
N1 Cd1 N1 180.0(6) . 9_557
N4 Cd1 Cl1 90.0 . 9_557
N4 Cd1 Cl1 90.0 9_557 9_557
N1 Cd1 Cl1 94.1(3) . 9_557
N1 Cd1 Cl1 85.9(3) 9_557 9_557
N4 Cd1 Cl1 90.0 . .
N4 Cd1 Cl1 90.0 9_557 .
N1 Cd1 Cl1 85.9(3) . .
N1 Cd1 Cl1 94.1(3) 9_557 .
Cl1 Cd1 Cl1 180.0 9_557 .
C2 Co1 C3 180.000(11) . .
C2 Co1 C1 90.1(4) . .
C3 Co1 C1 89.9(4) . .
C2 Co1 C1 90.1(4) . 3
C3 Co1 C1 89.9(4) . 3
C1 Co1 C1 179.7(8) . 3
C2 Co1 C1 90.1(4) . 4
C3 Co1 C1 89.9(4) . 4
C1 Co1 C1 90.000(5) . 4
C1 Co1 C1 90.000(5) 3 4
C2 Co1 C1 90.1(4) . 2
C3 Co1 C1 89.9(4) . 2
C1 Co1 C1 90.000(4) . 2
C1 Co1 C1 90.000(5) 3 2
C1 Co1 C1 179.7(8) 4 2
C4 Co2 C4 90.000(1) . 12_557
C4 Co2 C4 90.000(1) . 10_657
C4 Co2 C4 180.0(4) 12_557 10_657
C4 Co2 C4 180.0 . 3_545
C4 Co2 C4 90.000(1) 12_557 3_545
C4 Co2 C4 90.000(1) 10_657 3_545
C4 Co2 C5 90.0 . 10_657
C4 Co2 C5 90.000(1) 12_557 10_657
C4 Co2 C5 90.000(1) 10_657 10_657
C4 Co2 C5 90.0 3_545 10_657
C4 Co2 C5 90.0 . .
C4 Co2 C5 90.000(1) 12_557 .
C4 Co2 C5 90.000(1) 10_657 .
C4 Co2 C5 90.0 3_545 .
C5 Co2 C5 180.0 10_657 .
C1 N1 Cd1 165.6(12) . .
C3 N3 H1 180.000(14) . .
C4 N4 Cd1 180.0(9) . .
C5 N5 H2 180.0 . .
S1 N6 C6 175.8(13) 15_565 .
S1 N6 H6A 70.3 15_565 .
C6 N6 H6A 112.0 . .
S1 N6 H6B 59.1 15_565 .
C6 N6 H6B 118.6 . .
H6A N6 H6B 129.4 . .
C6 N7 H7A 122.2 . .
N6 S1 C6 3.2(9) 15_565 .
N6 S1 H3 105.2 15_565 .
C6 S1 H3 103.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.130(17) .
C1 Co1 1.916(13) .
C2 N2 1.14(3) .
C2 Co1 1.89(2) .
C3 N3 1.13(3) .
C3 Co1 1.90(3) .
C4 N4 1.127(17) .
C4 Co2 1.904(12) .
C5 N5 1.123(4) .
C5 Co2 1.920(4) .
C6 N6 1.313(3) 15_565
C6 N6 1.313(3) .
C6 N7 1.320(3) .
C6 S1 1.7412(15) .
C6 S1 1.7412(15) 15_565
Cd1 N4 2.298(12) .
Cd1 N4 2.298(12) 9_557
Cd1 N1 2.364(12) .
Cd1 N1 2.364(12) 9_557
Cd1 Cl1 2.617(4) 9_557
Cd1 Cl1 2.617(4) .
Co1 C1 1.916(13) 3
Co1 C1 1.916(13) 4
Co1 C1 1.916(13) 2
Co2 C4 1.904(12) 12_557
Co2 C4 1.904(12) 10_657
Co2 C4 1.904(12) 3_545
Co2 C5 1.920(4) 10_657
N3 H1 0.880(10) .
N5 H2 1.271(5) .
N6 S1 0.429(3) 15_565
N6 H6A 0.8593 .
N6 H6B 0.8624 .
N7 H7A 0.8597 .
S1 N6 0.429(3) 15_565
S1 H3 1.0956 .
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 S1 1.10 2.76 3.467(13) 121.6 8_666
S1 H3 Cl1 1.10 2.33 3.370(7) 157.4 3
N7 H7A Cl1 0.86 2.48 3.264(3) 151.7 3
N6 H6B S1 0.86 2.99 3.601(8) 129.1 12_656
N6 H6B Cl1 0.86 2.96 3.447(4) 117.4 10_656
N6 H6B Cl1 0.86 2.64 3.408(5) 149.1 2
N5 H2 N5 1.271(5) 1.271(5) 2.542(10) 180.000(0) 10_656
N3 H1 N2 0.880(10) 1.69(3) 2.57(3) 180.000(9) 1_554
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
N6 C6 S1 N6 -57(15) . 15_565
N7 C6 S1 N6 123(15) . 15_565
S1 C6 S1 N6 -58(16) 15_565 15_565
