#------------------------------------------------------------------------------
#$Date: 2023-03-04 20:18:56 +0200 (Sat, 04 Mar 2023) $
#$Revision: 281450 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/60/7246087.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_7246087
loop_
_publ_author_name
'Dinda, Susanta'
'Pahari, Goutam'
'Maiti, Anupam'
'Ghoshal, Debajyoti'
_publ_section_title
;
 Solvent induced reversible single-crystal-to-single-crystal structural
 transformation in dynamic metal organic frameworks: a case of enhanced
 hydrogen sorption in polycatenated framework
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              1116
_journal_page_last               1125
_journal_paper_doi               10.1039/D2CE01559E
_journal_volume                  25
_journal_year                    2023
_chemical_formula_sum            'C23 H18 N8 O10 Zn2'
_chemical_formula_weight         697.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2022-09-22 deposited with the CCDC.	2023-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                87.618(2)
_cell_angle_beta                 72.671(2)
_cell_angle_gamma                77.004(3)
_cell_formula_units_Z            2
_cell_length_a                   8.7683(7)
_cell_length_b                   12.2482(9)
_cell_length_c                   14.4310(9)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      1.8
_cell_volume                     1441.05(18)
_computing_cell_refinement       'SMART APEX II'
_computing_data_collection       'SMART APEX II (Bruker,2010)'
_computing_data_reduction        'SAINT (Bruker,2000)'
_computing_molecular_graphics    'Ortep-3v2 for windows (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0911
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14385
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.525
_diffrn_reflns_theta_min         2.228
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.732
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'XPREP' - A PROGRAM DATA PREPARATION & RECIPROCAL 
SPACE EXPLORATION,
Bruker Analytical X-ray Systems, 1997
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.998
_refine_diff_density_min         -2.194
_refine_diff_density_rms         0.251
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         6504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0899
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1946P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2400
_refine_ls_wR_factor_ref         0.2565
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5100
_reflns_number_total             6504
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ce01559e2.cif
_cod_data_source_block           DG3
_cod_depositor_comments
'Adding full bibliography for 7246084--7246089.cif.'
_cod_database_code               7246087
_shelx_shelxl_version_number     2016/6
_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.
;
_exptl_absorpt_special_details
;
?
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 1.12504(6) 0.30439(4) 0.01891(3) 0.0192(2) Uani 1 1 d . . . . .
Zn2 Zn 0.32119(6) 0.70515(4) 0.45767(4) 0.0196(2) Uani 1 1 d . . . . .
O3 O 0.5026(4) 0.5920(3) 0.3795(3) 0.0291(8) Uani 1 1 d . . . . .
O8 O 1.2653(4) 0.3999(3) 0.0424(2) 0.0225(7) Uani 1 1 d . . . . .
O7 O 1.4617(4) 0.2895(3) -0.0720(3) 0.0271(8) Uani 1 1 d . . . . .
O4 O 0.3516(4) 0.4806(3) 0.3481(3) 0.0271(8) Uani 1 1 d . . . . .
O2 O 0.8001(4) 0.2447(3) 0.0694(3) 0.0338(9) Uani 1 1 d . . . . .
O6 O 0.2046(4) 0.9059(3) 0.5518(3) 0.0371(9) Uani 1 1 d . . . . .
O1 O 0.9095(4) 0.3836(3) 0.0997(2) 0.0273(8) Uani 1 1 d . . . . .
O5 O 0.4557(4) 0.8071(3) 0.4779(3) 0.0249(8) Uani 1 1 d . . . . .
N5 N 0.1672(4) 0.6472(3) 0.5685(3) 0.0230(9) Uani 1 1 d . . . . .
N8 N 0.1240(4) 0.3092(3) 0.8809(3) 0.0197(8) Uani 1 1 d . . . . .
N4 N 1.2019(4) -0.2168(3) 0.3649(3) 0.0222(8) Uani 1 1 d . . . . .
N7 N 0.0616(4) 0.3644(3) 0.7477(3) 0.0208(8) Uani 1 1 d . . . . .
N6 N 0.0278(5) 0.5300(4) 0.6532(3) 0.0228(9) Uani 1 1 d . . . . .
N1 N 1.1933(5) 0.1509(4) 0.0664(3) 0.0260(9) Uani 1 1 d . . . . .
N3 N 1.1428(5) -0.1546(3) 0.2320(3) 0.0244(9) Uani 1 1 d . . . . .
O1W O 0.7344(6) 0.7079(4) 0.5388(3) 0.0506(12) Uani 1 1 d . . . . .
N2 N 1.2089(5) -0.0257(4) 0.1056(3) 0.0295(10) Uani 1 1 d . . . . .
C4 C 0.4819(5) 0.5124(4) 0.3323(3) 0.0216(10) Uani 1 1 d . . . . .
C13 C 0.0190(5) 0.3776(4) 0.8450(3) 0.0191(9) Uani 1 1 d . . . . .
H13 H -0.072755 0.428456 0.881822 0.023 Uiso 1 1 calc R U . . .
C16 C 1.1174(5) 0.0683(4) 0.0802(3) 0.0230(10) Uani 1 1 d . . . . .
H16 H 1.013792 0.073657 0.073487 0.028 Uiso 1 1 calc R U . . .
C19 C 1.1630(7) -0.1319(4) 0.1301(4) 0.0303(11) Uani 1 1 d . . . . .
H19A H 1.246919 -0.191393 0.090563 0.036 Uiso 1 1 calc R U . . .
H19B H 1.061147 -0.130527 0.115915 0.036 Uiso 1 1 calc R U . . .
C10 C -0.0355(6) 0.6324(4) 0.7026(3) 0.0258(10) Uani 1 1 d . . . . .
H10 H -0.120780 0.648561 0.760104 0.031 Uiso 1 1 calc R U . . .
C3 C 0.6322(5) 0.4602(4) 0.2525(3) 0.0217(10) Uani 1 1 d . . . . .
C2 C 0.6387(5) 0.3802(4) 0.1931(3) 0.0239(10) Uani 1 1 d . . . . .
C1 C 0.7927(5) 0.3317(4) 0.1148(3) 0.0248(11) Uani 1 1 d . . . . .
C22 C 1.2519(5) -0.2243(4) 0.2693(3) 0.0222(10) Uani 1 1 d . . . . .
H22 H 1.348566 -0.270905 0.232610 0.027 Uiso 1 1 calc R U . . .
C21 C 1.0548(6) -0.1367(4) 0.3897(4) 0.0276(11) Uani 1 1 d . . . . .
H21 H 0.991694 -0.113786 0.452809 0.033 Uiso 1 1 calc R U . . .
C9 C 0.0516(6) 0.7046(4) 0.6502(3) 0.0258(11) Uani 1 1 d . . . . .
H9 H 0.036737 0.779820 0.666087 0.031 Uiso 1 1 calc R U . . .
O1S O 0.7025(7) 0.0549(5) 0.1451(4) 0.0720(17) Uani 1 1 d . . . . .
C14 C 0.2033(6) 0.2825(4) 0.7200(4) 0.0262(11) Uani 1 1 d . . . . .
H14 H 0.262096 0.256282 0.657062 0.031 Uiso 1 1 calc R U . . .
C15 C 0.2403(6) 0.2477(4) 0.8021(4) 0.0271(11) Uani 1 1 d . . . . .
H15 H 0.329413 0.191500 0.805578 0.033 Uiso 1 1 calc R U . . .
C11 C 0.1489(5) 0.5441(4) 0.5735(3) 0.0234(10) Uani 1 1 d . . . . .
H11 H 0.211326 0.487522 0.527993 0.028 Uiso 1 1 calc R U . . .
C6 C 1.5201(5) 0.4524(4) -0.0253(4) 0.0268(11) Uani 1 1 d . . . . .
C12 C -0.0240(6) 0.4269(5) 0.6829(4) 0.0297(11) Uani 1 1 d . . . . .
H12A H -0.004094 0.380592 0.625740 0.036 Uiso 1 1 calc R U . . .
H12B H -0.140950 0.443908 0.715534 0.036 Uiso 1 1 calc R U . . .
C5 C 1.4099(5) 0.3749(4) -0.0178(3) 0.0225(10) Uani 1 1 d . . . . .
C20 C 1.0177(6) -0.0974(4) 0.3090(4) 0.0270(11) Uani 1 1 d . . . . .
H20 H 0.926776 -0.042979 0.305422 0.032 Uiso 1 1 calc R U . . .
C7 C 0.3545(6) 0.8992(4) 0.5180(4) 0.0271(11) Uani 1 1 d . . . . .
C17 C 1.3404(7) 0.1086(6) 0.0865(6) 0.0515(19) Uani 1 1 d . . . . .
H17 H 1.419939 0.148883 0.083205 0.062 Uiso 1 1 calc R U . . .
C18 C 1.3509(7) 0.0015(6) 0.1114(6) 0.058(2) Uani 1 1 d . . . . .
H18 H 1.436322 -0.045422 0.129122 0.069 Uiso 1 1 calc R U . . .
C1S C 0.624(2) 0.0766(11) 0.2408(8) 0.121(5) Uani 1 1 d . . . . .
C23 C 0.4234(6) 0.9978(4) 0.5206(4) 0.0318(12) Uani 1 1 d . . . . .
H3 H 0.711(7) 0.500(5) 0.254(4) 0.027(15) Uiso 1 1 d . . . . .
H2 H 0.551(7) 0.343(5) 0.196(4) 0.020(13) Uiso 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'
Zn Zn 0.2839 1.4301 '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
O1 Zn1 O8 100.64(14) . . ?
O1 Zn1 N8 108.45(14) . 1_654 ?
O8 Zn1 N8 111.24(15) . 1_654 ?
O1 Zn1 N1 112.05(16) . . ?
O8 Zn1 N1 108.78(16) . . ?
N8 Zn1 N1 114.79(16) 1_654 . ?
O3 Zn2 O5 96.50(14) . . ?
O3 Zn2 N5 115.25(16) . . ?
O5 Zn2 N5 121.60(16) . . ?
O3 Zn2 N4 105.62(15) . 1_465 ?
O5 Zn2 N4 105.79(16) . 1_465 ?
N5 Zn2 N4 110.28(16) . 1_465 ?
C4 O3 Zn2 122.9(3) . . ?
C5 O8 Zn1 111.2(3) . . ?
C1 O1 Zn1 116.5(3) . . ?
C7 O5 Zn2 106.9(3) . . ?
C11 N5 C9 106.4(4) . . ?
C11 N5 Zn2 124.0(3) . . ?
C9 N5 Zn2 129.4(4) . . ?
C13 N8 C15 106.0(4) . . ?
C13 N8 Zn1 126.4(3) . 1_456 ?
C15 N8 Zn1 127.4(3) . 1_456 ?
C22 N4 C21 106.1(4) . . ?
C22 N4 Zn2 127.6(3) . 1_645 ?
C21 N4 Zn2 126.2(3) . 1_645 ?
C13 N7 C14 107.5(4) . . ?
C13 N7 C12 126.6(4) . . ?
C14 N7 C12 125.9(4) . . ?
C11 N6 C10 107.3(4) . . ?
C11 N6 C12 126.5(4) . . ?
C10 N6 C12 126.2(4) . . ?
C16 N1 C17 105.6(4) . . ?
C16 N1 Zn1 128.8(3) . . ?
C17 N1 Zn1 125.4(4) . . ?
C22 N3 C20 107.7(4) . . ?
C22 N3 C19 126.4(4) . . ?
C20 N3 C19 125.4(4) . . ?
C16 N2 C18 106.7(5) . . ?
C16 N2 C19 127.1(4) . . ?
C18 N2 C19 126.0(5) . . ?
O4 C4 O3 125.1(4) . . ?
O4 C4 C3 121.6(4) . . ?
O3 C4 C3 113.4(4) . . ?
N8 C13 N7 111.0(4) . . ?
N1 C16 N2 111.4(4) . . ?
N2 C19 N3 111.0(4) . . ?
C9 C10 N6 106.2(4) . . ?
C2 C3 C4 124.2(4) . . ?
C3 C2 C1 121.6(4) . . ?
O2 C1 O1 124.7(4) . . ?
O2 C1 C2 119.0(5) . . ?
O1 C1 C2 116.3(4) . . ?
N4 C22 N3 110.5(4) . . ?
C20 C21 N4 109.8(4) . . ?
C10 C9 N5 108.7(4) . . ?
C15 C14 N7 106.4(4) . . ?
C14 C15 N8 109.1(4) . . ?
N5 C11 N6 111.4(4) . . ?
C6 C6 C5 124.6(5) 2_865 . ?
N6 C12 N7 112.3(4) . . ?
O7 C5 O8 123.4(5) . . ?
O7 C5 C6 118.0(4) . . ?
O8 C5 C6 118.6(4) . . ?
C21 C20 N3 105.9(4) . . ?
O6 C7 O5 122.2(5) . . ?
O6 C7 C23 120.3(4) . . ?
O5 C7 C23 117.5(4) . . ?
C18 C17 N1 110.0(5) . . ?
C17 C18 N2 106.2(5) . . ?
C23 C23 C7 124.9(6) 2_676 . ?
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
Zn1 O1 1.957(3) . ?
Zn1 O8 1.981(3) . ?
Zn1 N8 1.993(4) 1_654 ?
Zn1 N1 1.998(4) . ?
Zn2 O3 1.947(3) . ?
Zn2 O5 1.983(4) . ?
Zn2 N5 1.984(4) . ?
Zn2 N4 2.020(4) 1_465 ?
O3 C4 1.287(6) . ?
O8 C5 1.284(5) . ?
O7 C5 1.247(5) . ?
O4 C4 1.244(6) . ?
O2 C1 1.253(6) . ?
O6 C7 1.243(6) . ?
O1 C1 1.284(6) . ?
O5 C7 1.301(5) . ?
N5 C11 1.304(7) . ?
N5 C9 1.396(5) . ?
N8 C13 1.311(6) . ?
N8 C15 1.391(5) . ?
N4 C22 1.317(6) . ?
N4 C21 1.393(5) . ?
N7 C13 1.347(6) . ?
N7 C14 1.374(6) . ?
N7 C12 1.458(6) . ?
N6 C11 1.348(6) . ?
N6 C10 1.384(6) . ?
N6 C12 1.443(7) . ?
N1 C16 1.309(7) . ?
N1 C17 1.388(6) . ?
N3 C22 1.355(6) . ?
N3 C20 1.386(6) . ?
N3 C19 1.452(6) . ?
N2 C16 1.352(6) . ?
N2 C18 1.386(7) . ?
N2 C19 1.446(7) . ?
C4 C3 1.500(6) . ?
C10 C9 1.356(7) . ?
C3 C2 1.309(7) . ?
C2 C1 1.496(6) . ?
C21 C20 1.343(7) . ?
O1S C1S 1.355(12) . ?
C14 C15 1.347(7) . ?
C6 C6 1.323(9) 2_865 ?
C6 C5 1.479(7) . ?
C7 C23 1.474(8) . ?
C17 C18 1.336(9) . ?
C23 C23 1.309(10) 2_676 ?
