#------------------------------------------------------------------------------
#$Date: 2019-09-25 12:31:03 +0200 (Wed 25 de Sep de 2019) $
#$Revision: 218848 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/12/7701250.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_7701250
loop_
_publ_author_name
'Tom, Lincy'
'Kurup, M. R. Prathapachandra'
_publ_section_title
;
 Stimuli Responsive Multifunctional ZMOF based on an Unorthodox Polytopic
 ligand: Reversible Thermochromism and Anion Triggered Metallogelation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT02820J
_journal_year                    2019
_chemical_formula_moiety         'C16 H16 Cd N6 O3, 0.724(H2 O)'
_chemical_formula_sum            'C16 H17.45 Cd N6 O3.72'
_chemical_formula_weight         465.80
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-04-21 deposited with the CCDC.    2019-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   35.013(2)
_cell_length_b                   35.013(2)
_cell_length_c                   14.6617(7)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      2.33
_cell_volume                     15565.9(15)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker AXS Kappa Apex2 diffractometer'
_diffrn_measurement_method       'ω and φ scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            64515
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.457
_diffrn_reflns_theta_min         1.163
_diffrn_source                   'Sealed tube'
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruer, 1999)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    0.891
_exptl_crystal_description       block
_exptl_crystal_F_000             4198
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         2.750
_refine_diff_density_min         -0.916
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.611
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         8590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.611
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1991P)²+189.4098P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1682
_refine_ls_wR_factor_ref         0.1937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5887
_reflns_number_total             8720
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt02820j2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        15565.6(19)
_cod_database_code               7701250
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_min   0.737
_shelx_estimated_absorpt_t_max   0.829
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.78897(19) 0.95697(15) 0.3853(3) 0.0715(13) Uani 1 1 d . . . . .
H1 H 0.789656 0.949963 0.324378 0.086 Uiso 1 1 calc R U . . .
C2 C 0.77768(19) 0.92455(13) 0.4493(3) 0.0691(13) Uani 1 1 d . . . . .
H2 H 0.770717 0.896295 0.431536 0.083 Uiso 1 1 calc R U . . .
C3 C 0.77669(12) 0.93410(11) 0.5404(2) 0.0440(8) Uani 1 1 d . . . . .
C4 C 0.78625(16) 0.97625(13) 0.5611(3) 0.0607(11) Uani 1 1 d . . . . .
H4 H 0.785200 0.984112 0.621266 0.073 Uiso 1 1 calc R U . . .
C5 C 0.79738(17) 1.00673(13) 0.4924(3) 0.0626(12) Uani 1 1 d . . . . .
H5 H 0.804135 1.035189 0.507918 0.075 Uiso 1 1 calc R U . . .
C6 C 0.76715(12) 0.89967(11) 0.6109(2) 0.0437(8) Uani 1 1 d . . . . .
C7 C 0.73317(14) 0.87266(12) 0.8311(3) 0.0531(9) Uani 1 1 d . . . . .
C8 C 0.7226(2) 0.90704(17) 0.8659(4) 0.0848(14) Uani 1 1 d . . . . .
H8A H 0.742586 0.935104 0.839119 0.127 Uiso 1 1 calc R U . . .
H8B H 0.725707 0.909114 0.931083 0.127 Uiso 1 1 calc R U . . .
H8C H 0.692895 0.898718 0.849707 0.127 Uiso 1 1 calc R U . . .
C9 C 0.7105(2) 0.83247(19) 0.9857(3) 0.1011(16) Uani 1 1 d . . . A 1
H9A H 0.682221 0.830633 0.983521 0.152 Uiso 1 1 calc R U . A 1
H9B H 0.730523 0.857743 1.020990 0.152 Uiso 1 1 calc R U . A 1
H9C H 0.707487 0.806266 1.013435 0.152 Uiso 1 1 calc R U . A 1
C10 C 0.72803(15) 0.83680(13) 0.8911(3) 0.0533(9) Uani 1 1 d . . . . .
C11 C 0.75361(11) 0.75542(11) 0.8670(2) 0.0420(7) Uani 1 1 d . . . . .
C12 C 0.74705(12) 0.71416(12) 0.9118(2) 0.0420(7) Uani 1 1 d . . . . .
C13 C 0.76859(14) 0.69343(13) 0.8769(3) 0.0523(9) Uani 1 1 d . . . . .
H13 H 0.787844 0.705701 0.827885 0.063 Uiso 1 1 calc R U . . .
C14 C 0.76132(13) 0.65437(12) 0.9152(3) 0.0520(9) Uani 1 1 d . . . . .
H14 H 0.776352 0.640952 0.891546 0.062 Uiso 1 1 calc R U . . .
C15 C 0.71408(14) 0.65595(14) 1.0198(3) 0.0574(9) Uani 1 1 d . . . . .
H15 H 0.695339 0.643296 1.069430 0.069 Uiso 1 1 calc R U . . .
C16 C 0.72031(15) 0.69554(14) 0.9861(3) 0.0591(10) Uani 1 1 d . . . . .
H16 H 0.706502 0.709389 1.013557 0.071 Uiso 1 1 calc R U . . .
N1 N 0.79897(12) 0.99777(9) 0.4057(2) 0.0493(8) Uani 1 1 d . . . . .
N2 N 0.75359(12) 0.90618(10) 0.6901(2) 0.0549(8) Uani 1 1 d . . . . .
N3 N 0.74718(11) 0.87291(9) 0.7503(2) 0.0489(7) Uani 1 1 d . . . . .
N4 N 0.73934(10) 0.81041(9) 0.8583(2) 0.0448(7) Uani 1 1 d . . . . .
N5 N 0.73391(11) 0.77460(10) 0.9086(2) 0.0493(7) Uani 1 1 d . . . . .
N6 N 0.73374(10) 0.63508(10) 0.9845(2) 0.0432(6) Uani 1 1 d . . . . .
O1 O 0.84142(14) 0.87362(16) 0.7545(4) 0.1179(18) Uani 1 1 d . . . . .
H1A H 0.851380 0.896231 0.787981 0.177 Uiso 1 1 d R U . . .
H1B H 0.841804 0.853665 0.785666 0.177 Uiso 1 1 d R U . . .
O2 O 0.77217(12) 0.86824(9) 0.58741(19) 0.0650(8) Uani 1 1 d . . . . .
O3 O 0.77563(10) 0.76714(10) 0.79471(19) 0.0629(7) Uani 1 1 d . . . . .
O4 O 0.6406(2) 0.7228(2) 0.9929(6) 0.146(3) Uani 0.724(12) 1 d . . P . .
H4A H 0.624431 0.734732 0.984562 0.220 Uiso 0.724(12) 1 d R U P . .
H4B H 0.665481 0.739742 0.968133 0.220 Uiso 0.724(12) 1 d R U P . .
Cd1 Cd 0.76832(2) 0.82093(2) 0.70829(2) 0.03780(8) 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
N1 C1 C2 123.4(4) . .
N1 C1 H1 118.3 . .
C2 C1 H1 118.3 . .
C1 C2 C3 119.6(4) . .
C1 C2 H2 120.2 . .
C3 C2 H2 120.2 . .
C4 C3 C2 116.9(3) . .
C4 C3 C6 123.3(3) . .
C2 C3 C6 119.8(3) . .
C3 C4 C5 119.6(4) . .
C3 C4 H4 120.2 . .
C5 C4 H4 120.2 . .
N1 C5 C4 123.5(4) . .
N1 C5 H5 118.3 . .
C4 C5 H5 118.3 . .
O2 C6 N2 128.2(3) . .
O2 C6 C3 116.6(3) . .
N2 C6 C3 115.2(3) . .
N3 C7 C10 116.3(3) . .
N3 C7 C8 123.5(4) . .
C10 C7 C8 120.2(4) . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C10 C9 H9A 109.5 . .
C10 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C10 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
N4 C10 C7 116.5(3) . .
N4 C10 C9 122.7(4) . .
C7 C10 C9 120.8(4) . .
O3 C11 N5 127.8(3) . .
O3 C11 C12 117.4(3) . .
N5 C11 C12 114.8(3) . .
C16 C12 C13 117.9(4) . .
C16 C12 C11 123.1(4) . .
C13 C12 C11 119.0(3) . .
C14 C13 C12 119.5(4) . .
C14 C13 H13 120.3 . .
C12 C13 H13 120.3 . .
N6 C14 C13 122.8(4) . .
N6 C14 H14 118.6 . .
C13 C14 H14 118.6 . .
N6 C15 C16 123.0(4) . .
N6 C15 H15 118.5 . .
C16 C15 H15 118.5 . .
C12 C16 C15 119.3(4) . .
C12 C16 H16 120.4 . .
C15 C16 H16 120.4 . .
C5 N1 C1 117.1(3) . .
C5 N1 Cd1 121.6(2) . 11_566
C1 N1 Cd1 121.3(3) . 11_566
C6 N2 N3 109.6(3) . .
C7 N3 N2 119.6(3) . .
C7 N3 Cd1 120.1(2) . .
N2 N3 Cd1 120.0(2) . .
C10 N4 N5 120.4(3) . .
C10 N4 Cd1 120.2(2) . .
N5 N4 Cd1 119.3(2) . .
C11 N5 N4 110.0(3) . .
C14 N6 C15 117.5(3) . .
C14 N6 Cd1 121.0(2) . 6_565
C15 N6 Cd1 121.5(2) . 6_565
Cd1 O1 H1A 132.1 . .
Cd1 O1 H1B 88.2 . .
H1A O1 H1B 107.1 . .
C6 O2 Cd1 115.1(2) . .
C11 O3 Cd1 114.6(2) . .
H4A O4 H4B 107.1 . .
N1 Cd1 N3 145.58(11) 12_656 .
N1 Cd1 N4 147.62(11) 12_656 .
N3 Cd1 N4 66.67(10) . .
N1 Cd1 O1 86.79(16) 12_656 .
N3 Cd1 O1 87.62(16) . .
N4 Cd1 O1 93.83(16) . .
N1 Cd1 O2 80.37(11) 12_656 .
N3 Cd1 O2 65.74(10) . .
N4 Cd1 O2 131.95(10) . .
O1 Cd1 O2 90.46(17) . .
N1 Cd1 O3 81.78(10) 12_656 .
N3 Cd1 O3 131.89(10) . .
N4 Cd1 O3 65.91(10) . .
O1 Cd1 O3 87.85(16) . .
O2 Cd1 O3 162.14(10) . .
N1 Cd1 N6 87.46(11) 12_656 8_654
N3 Cd1 N6 97.42(11) . 8_654
N4 Cd1 N6 90.76(11) . 8_654
O1 Cd1 N6 174.23(15) . 8_654
O2 Cd1 N6 89.07(11) . 8_654
O3 Cd1 N6 90.84(11) . 8_654
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.324(5) .
C1 C2 1.370(6) .
C1 H1 0.9300 .
C2 C3 1.381(6) .
C2 H2 0.9300 .
C3 C4 1.374(5) .
C3 C6 1.494(5) .
C4 C5 1.375(6) .
C4 H4 0.9300 .
C5 N1 1.316(5) .
C5 H5 0.9300 .
C6 O2 1.247(5) .
C6 N2 1.317(5) .
C7 N3 1.280(5) .
C7 C10 1.469(5) .
C7 C8 1.514(6) .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 C10 1.494(6) .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 N4 1.268(5) .
C11 O3 1.253(4) .
C11 N5 1.327(5) .
C11 C12 1.496(5) .
C12 C16 1.371(5) .
C12 C13 1.380(6) .
C13 C14 1.380(5) .
C13 H13 0.9300 .
C14 N6 1.330(5) .
C14 H14 0.9300 .
C15 N6 1.334(5) .
C15 C16 1.382(6) .
C15 H15 0.9300 .
C16 H16 0.9300 .
N1 Cd1 2.366(3) 11_566
N2 N3 1.386(4) .
N3 Cd1 2.364(3) .
N4 N5 1.384(4) .
N4 Cd1 2.372(3) .
N6 Cd1 2.395(3) 6_565
O1 Cd1 2.386(4) .
O1 H1A 0.8440 .
O1 H1B 0.8403 .
O2 Cd1 2.383(3) .
O3 Cd1 2.388(3) .
O4 H4A 0.8632 .
O4 H4B 0.8516 .
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
_geom_hbond_publ_flag
C1 H1 O3 0.93 2.63 3.152(5) 115.9 11_566 yes
C5 H5 O2 0.93 2.60 3.090(5) 113.6 11_566 yes
C9^a H9C^a O4 0.96 2.70 3.368(10) 127.5 . yes
C14 H14 O2 0.93 2.62 3.289(5) 129.0 6_565 yes
C16 H16 O4 0.93 2.59 3.373(9) 141.8 . yes
O4 H4A N2 0.86 2.16 3.024(8) 173.7 16_666 yes
O4 H4B N5 0.85 2.25 3.092(8) 169.6 . yes
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_4
N1 C1 C2 C3 -0.4(9) .
C1 C2 C3 C4 1.6(7) .
C1 C2 C3 C6 -176.2(5) .
C2 C3 C4 C5 -1.9(7) .
C6 C3 C4 C5 175.9(4) .
C3 C4 C5 N1 0.9(8) .
C4 C3 C6 O2 -158.9(4) .
C2 C3 C6 O2 18.8(6) .
C4 C3 C6 N2 22.3(6) .
C2 C3 C6 N2 -160.0(4) .
N3 C7 C10 N4 2.3(6) .
C8 C7 C10 N4 -177.0(4) .
N3 C7 C10 C9 -178.0(5) .
C8 C7 C10 C9 2.7(7) .
O3 C11 C12 C16 -173.7(4) .
N5 C11 C12 C16 4.5(5) .
O3 C11 C12 C13 5.9(5) .
N5 C11 C12 C13 -175.9(3) .
C16 C12 C13 C14 2.4(6) .
C11 C12 C13 C14 -177.2(4) .
C12 C13 C14 N6 0.9(6) .
C13 C12 C16 C15 -3.5(6) .
C11 C12 C16 C15 176.1(4) .
N6 C15 C16 C12 1.4(7) .
C4 C5 N1 C1 0.4(8) .
C4 C5 N1 Cd1 -177.7(4) 11_566
C2 C1 N1 C5 -0.6(8) .
C2 C1 N1 Cd1 177.5(4) 11_566
O2 C6 N2 N3 3.2(6) .
C3 C6 N2 N3 -178.2(3) .
C10 C7 N3 N2 -178.9(4) .
C8 C7 N3 N2 0.4(7) .
C10 C7 N3 Cd1 -4.6(5) .
C8 C7 N3 Cd1 174.7(4) .
C6 N2 N3 C7 -178.8(4) .
C6 N2 N3 Cd1 7.0(4) .
C7 C10 N4 N5 -177.3(3) .
C9 C10 N4 N5 3.0(7) .
C7 C10 N4 Cd1 1.1(5) .
C9 C10 N4 Cd1 -178.6(4) .
O3 C11 N5 N4 2.4(5) .
C12 C11 N5 N4 -175.7(3) .
C10 N4 N5 C11 -171.0(4) .
Cd1 N4 N5 C11 10.6(4) .
C13 C14 N6 C15 -2.9(6) .
C13 C14 N6 Cd1 176.1(3) 6_565
C16 C15 N6 C14 1.8(6) .
C16 C15 N6 Cd1 -177.3(3) 6_565
N2 C6 O2 Cd1 -11.2(6) .
C3 C6 O2 Cd1 170.2(3) .
N5 C11 O3 Cd1 -13.5(5) .
C12 C11 O3 Cd1 164.4(2) .
