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#$Date: 2022-10-12 01:41:50 +0300 (Wed, 12 Oct 2022) $
#$Revision: 278531 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/56/7245648.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_7245648
loop_
_publ_author_name
'Ju, Huiyeong'
'Kim, Seulgi'
'Jung, Jong Hwa'
'Lee, Shim Sung'
_publ_section_title
;
 A series of entangled MOFs constructed from flexible dipyridyl piperazine
 and rigid dicarboxylate: interpenetration, self-penetration and
 polycatenation
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00745B
_journal_year                    2022
_chemical_formula_moiety         'C30 H28 Cd N4 O6, 2(C4 H9 N O) '
_chemical_formula_sum            'C38 H50 Cd N6 O8'
_chemical_formula_weight         831.24
_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   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-09-01 deposited with the CCDC.	2022-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                114.880(18)
_cell_angle_beta                 99.231(18)
_cell_angle_gamma                97.47(2)
_cell_formula_units_Z            1
_cell_length_a                   7.664(4)
_cell_length_b                   10.968(6)
_cell_length_c                   12.971(6)
_cell_measurement_reflns_used    6058
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.04
_cell_measurement_theta_min      2.76
_cell_volume                     952.3(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.909
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9842
_diffrn_reflns_point_group_measured_fraction_full 0.909
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.782
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       block
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.185
_refine_diff_density_max         3.275
_refine_diff_density_min         -4.679
_refine_diff_density_rms         0.247
_refine_ls_extinction_coef       0.022(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3413
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.1353
_refine_ls_R_factor_gt           0.0882
_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)+(0.1328P)²+13.6342P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2321
_refine_ls_wR_factor_ref         0.3098
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2748
_reflns_number_total             3413
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ce00745b2.cif
_cod_data_source_block           3
_cod_database_code               7245648
_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. 
;
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
Cd1 Cd 1.000000 1.000000 0.000000 0.0376(5) Uani 1 2 d S . P . .
O1 O 0.8665(10) 1.0309(9) 0.1520(7) 0.048(2) Uani 1 1 d . . . . .
O1W O 1.1578(11) 0.8483(9) 0.0346(8) 0.051(2) Uani 1 1 d . U . . .
O2 O 1.0467(11) 0.9366(11) 0.2336(8) 0.057(2) Uani 1 1 d . . . . .
N1 N 0.7329(11) 0.8305(9) -0.1237(8) 0.039(2) Uani 1 1 d . . . . .
N2 N 0.1753(11) 0.5026(10) -0.4372(9) 0.043(2) Uani 1 1 d . . . . .
C1 C 0.7399(15) 0.7406(13) -0.2312(10) 0.047(3) Uani 1 1 d . . . . .
H1A H 0.846820 0.753347 -0.257155 0.057 Uiso 1 1 calc R U . . .
C2 C 0.5987(15) 0.6302(15) -0.3058(12) 0.054(3) Uani 1 1 d . . . . .
H2A H 0.607355 0.570253 -0.382211 0.065 Uiso 1 1 calc R U . . .
C3 C 0.4435(13) 0.6084(13) -0.2673(12) 0.047(3) Uani 1 1 d . . . . .
C4 C 0.4352(14) 0.7029(14) -0.1570(11) 0.050(3) Uani 1 1 d . . . . .
H4A H 0.329248 0.693618 -0.129197 0.061 Uiso 1 1 calc R U . . .
C5 C 0.5810(14) 0.8096(14) -0.0885(11) 0.050(3) Uani 1 1 d . . . . .
H5A H 0.574452 0.871998 -0.012348 0.060 Uiso 1 1 calc R U . . .
C6 C 0.2898(15) 0.4817(14) -0.3460(12) 0.054(3) Uani 1 1 d . . . . .
H6A H 0.342436 0.400779 -0.383615 0.065 Uiso 1 1 calc R U . . .
H6B H 0.214025 0.462159 -0.297422 0.065 Uiso 1 1 calc R U . . .
C7 C 0.0755(14) 0.6085(14) -0.3871(12) 0.052(3) Uani 1 1 d . . . . .
H7A H 0.162028 0.696800 -0.333434 0.062 Uiso 1 1 calc R U . . .
H7B H 0.000380 0.582665 -0.340943 0.062 Uiso 1 1 calc R U . . .
C8 C 0.0455(14) 0.3733(13) -0.5180(11) 0.047(3) Uani 1 1 d . . . . .
H8A H -0.030040 0.343342 -0.474125 0.057 Uiso 1 1 calc R U . . .
H8B H 0.111878 0.300800 -0.554289 0.057 Uiso 1 1 calc R U . . .
C9 C 0.9106(12) 0.9852(13) 0.2237(10) 0.042(3) Uani 1 1 d . . . . .
C10 C 0.7845(13) 0.9871(12) 0.3036(10) 0.040(2) Uani 1 1 d . . . . .
C11 C 0.8226(15) 0.9366(16) 0.3830(12) 0.055(3) Uani 1 1 d . . . . .
H11A H 0.925744 0.897454 0.385889 0.066 Uiso 1 1 calc R U . . .
C12 C 0.7122(16) 0.9420(17) 0.4593(12) 0.059(4) Uani 1 1 d . . . . .
H12A H 0.742061 0.905806 0.513073 0.071 Uiso 1 1 calc R U . . .
C13 C 0.5585(13) 0.9987(13) 0.4598(10) 0.041(3) Uani 1 1 d . . . . .
C14 C 0.5181(15) 1.0431(14) 0.3743(12) 0.052(3) Uani 1 1 d . . . . .
H14A H 0.410192 1.075644 0.366501 0.062 Uiso 1 1 calc R U . . .
C15 C 0.6307(15) 1.0410(13) 0.3007(11) 0.047(3) Uani 1 1 d . . . . .
H15A H 0.602121 1.077278 0.246799 0.057 Uiso 1 1 calc R U . . .
N3 N 0.2472(15) 0.6007(14) 0.1749(12) 0.068(3) Uani 1 1 d D . . . .
O3 O 0.0118(13) 0.4188(11) 0.1107(10) 0.068(3) Uani 1 1 d . U . . .
C16 C 0.195(2) 0.6685(18) 0.2792(15) 0.083(5) Uani 1 1 d D . . . .
H16A H 0.081126 0.613707 0.277149 0.125 Uiso 1 1 calc R U . . .
H16B H 0.176322 0.758992 0.288374 0.125 Uiso 1 1 calc R U . . .
H16C H 0.289229 0.680462 0.345351 0.125 Uiso 1 1 calc R U . . .
C17 C 0.4089(19) 0.666(2) 0.1609(18) 0.087(5) Uani 1 1 d D . . . .
H17A H 0.513669 0.641661 0.195358 0.131 Uiso 1 1 calc R U . . .
H17B H 0.422038 0.766481 0.200400 0.131 Uiso 1 1 calc R U . . .
H17C H 0.402057 0.635926 0.077420 0.131 Uiso 1 1 calc R U . . .
C18 C 0.218(2) 0.4024(18) -0.0137(15) 0.072(4) Uani 1 1 d . . . . .
H18A H 0.335762 0.383082 0.008414 0.109 Uiso 1 1 calc R U . . .
H18B H 0.231020 0.461957 -0.052189 0.109 Uiso 1 1 calc R U . . .
H18C H 0.131395 0.315675 -0.067514 0.109 Uiso 1 1 calc R U . . .
C19 C 0.1494(17) 0.4740(16) 0.0947(14) 0.059(4) 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'
Cd Cd -0.8075 1.2024 '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'
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 Cd1 O1 180.0 . 2_775 ?
O1 Cd1 O1W 92.0(3) . . ?
O1 Cd1 O1W 88.0(3) 2_775 . ?
O1 Cd1 O1W 88.0(3) . 2_775 ?
O1 Cd1 O1W 92.0(3) 2_775 2_775 ?
O1W Cd1 O1W 180.0 . 2_775 ?
O1 Cd1 N1 86.9(3) . . ?
O1 Cd1 N1 93.1(3) 2_775 . ?
O1W Cd1 N1 95.9(3) . . ?
O1W Cd1 N1 84.1(3) 2_775 . ?
O1 Cd1 N1 93.1(3) . 2_775 ?
O1 Cd1 N1 86.9(3) 2_775 2_775 ?
O1W Cd1 N1 84.1(3) . 2_775 ?
O1W Cd1 N1 95.9(3) 2_775 2_775 ?
N1 Cd1 N1 180.0(5) . 2_775 ?
C9 O1 Cd1 123.2(7) . . ?
C1 N1 C5 117.4(10) . . ?
C1 N1 Cd1 118.2(6) . . ?
C5 N1 Cd1 124.0(8) . . ?
C7 N2 C8 108.7(9) . . ?
C7 N2 C6 111.5(11) . . ?
C8 N2 C6 109.4(9) . . ?
N1 C1 C2 123.0(10) . . ?
N1 C1 H1A 118.5 . . ?
C2 C1 H1A 118.5 . . ?
C1 C2 C3 118.9(13) . . ?
C1 C2 H2A 120.5 . . ?
C3 C2 H2A 120.5 . . ?
C4 C3 C2 118.0(11) . . ?
C4 C3 C6 122.3(11) . . ?
C2 C3 C6 119.7(13) . . ?
C5 C4 C3 119.4(10) . . ?
C5 C4 H4A 120.3 . . ?
C3 C4 H4A 120.3 . . ?
N1 C5 C4 123.2(12) . . ?
N1 C5 H5A 118.4 . . ?
C4 C5 H5A 118.4 . . ?
N2 C6 C3 111.8(9) . . ?
N2 C6 H6A 109.3 . . ?
C3 C6 H6A 109.3 . . ?
N2 C6 H6B 109.3 . . ?
C3 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
N2 C7 C8 111.1(11) . 2_564 ?
N2 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 2_564 . ?
N2 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 2_564 . ?
H7A C7 H7B 108.0 . . ?
N2 C8 C7 110.7(10) . 2_564 ?
N2 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 2_564 . ?
N2 C8 H8B 109.5 . . ?
C7 C8 H8B 109.5 2_564 . ?
H8A C8 H8B 108.1 . . ?
O2 C9 O1 125.5(10) . . ?
O2 C9 C10 117.6(10) . . ?
O1 C9 C10 116.8(9) . . ?
C11 C10 C15 117.8(9) . . ?
C11 C10 C9 120.1(10) . . ?
C15 C10 C9 122.1(9) . . ?
C10 C11 C12 120.7(11) . . ?
C10 C11 H11A 119.6 . . ?
C12 C11 H11A 119.6 . . ?
C11 C12 C13 122.5(10) . . ?
C11 C12 H12A 118.7 . . ?
C13 C12 H12A 118.7 . . ?
C14 C13 C12 115.4(10) . . ?
C14 C13 C13 122.9(12) . 2_676 ?
C12 C13 C13 121.6(11) . 2_676 ?
C15 C14 C13 121.9(10) . . ?
C15 C14 H14A 119.1 . . ?
C13 C14 H14A 119.1 . . ?
C14 C15 C10 121.5(10) . . ?
C14 C15 H15A 119.2 . . ?
C10 C15 H15A 119.2 . . ?
C19 N3 C16 119.3(12) . . ?
C19 N3 C17 123.0(14) . . ?
C16 N3 C17 117.6(14) . . ?
N3 C16 H16A 109.5 . . ?
N3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C17 H17A 109.5 . . ?
N3 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N3 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C19 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O3 C19 N3 121.3(14) . . ?
O3 C19 C18 121.6(15) . . ?
N3 C19 C18 117.0(12) . . ?
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 O1 2.286(7) . ?
Cd1 O1 2.286(7) 2_775 ?
Cd1 O1W 2.326(8) . ?
Cd1 O1W 2.326(8) 2_775 ?
Cd1 N1 2.381(9) . ?
Cd1 N1 2.381(9) 2_775 ?
O1 C9 1.251(13) . ?
O2 C9 1.244(14) . ?
N1 C1 1.342(14) . ?
N1 C5 1.343(13) . ?
N2 C7 1.453(16) . ?
N2 C8 1.465(14) . ?
N2 C6 1.472(14) . ?
C1 C2 1.383(17) . ?
C1 H1A 0.9500 . ?
C2 C3 1.392(16) . ?
C2 H2A 0.9500 . ?
C3 C4 1.387(18) . ?
C3 C6 1.535(16) . ?
C4 C5 1.369(17) . ?
C4 H4A 0.9500 . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.519(16) 2_564 ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.522(13) . ?
C10 C11 1.371(15) . ?
C10 C15 1.387(16) . ?
C11 C12 1.390(16) . ?
C11 H11A 0.9500 . ?
C12 C13 1.402(16) . ?
C12 H12A 0.9500 . ?
C13 C14 1.395(14) . ?
C13 C13 1.473(19) 2_676 ?
C14 C15 1.381(15) . ?
C14 H14A 0.9500 . ?
C15 H15A 0.9500 . ?
N3 C19 1.355(19) . ?
N3 C16 1.398(15) . ?
N3 C17 1.428(13) . ?
O3 C19 1.238(15) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.51(2) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 0.6(18) . . . . ?
Cd1 N1 C1 C2 173.6(10) . . . . ?
N1 C1 C2 C3 -1.8(19) . . . . ?
C1 C2 C3 C4 2.9(18) . . . . ?
C1 C2 C3 C6 -176.4(11) . . . . ?
C2 C3 C4 C5 -2.8(17) . . . . ?
C6 C3 C4 C5 176.4(11) . . . . ?
C1 N1 C5 C4 -0.5(17) . . . . ?
Cd1 N1 C5 C4 -173.2(9) . . . . ?
C3 C4 C5 N1 1.7(18) . . . . ?
C7 N2 C6 C3 -66.6(13) . . . . ?
C8 N2 C6 C3 173.1(11) . . . . ?
C4 C3 C6 N2 101.0(14) . . . . ?
C2 C3 C6 N2 -79.8(14) . . . . ?
C8 N2 C7 C8 -58.0(12) . . . 2_564 ?
C6 N2 C7 C8 -178.6(9) . . . 2_564 ?
C7 N2 C8 C7 57.8(14) . . . 2_564 ?
C6 N2 C8 C7 179.7(10) . . . 2_564 ?
Cd1 O1 C9 O2 11.5(17) . . . . ?
Cd1 O1 C9 C10 -167.4(7) . . . . ?
O2 C9 C10 C11 0.0(18) . . . . ?
O1 C9 C10 C11 179.0(12) . . . . ?
O2 C9 C10 C15 179.0(12) . . . . ?
O1 C9 C10 C15 -2.1(17) . . . . ?
C15 C10 C11 C12 -1(2) . . . . ?
C9 C10 C11 C12 177.8(13) . . . . ?
C10 C11 C12 C13 0(2) . . . . ?
C11 C12 C13 C14 3(2) . . . . ?
C11 C12 C13 C13 179.0(16) . . . 2_676 ?
C12 C13 C14 C15 -5(2) . . . . ?
C13 C13 C14 C15 179.4(15) 2_676 . . . ?
C13 C14 C15 C10 4(2) . . . . ?
C11 C10 C15 C14 -1(2) . . . . ?
C9 C10 C15 C14 -179.5(12) . . . . ?
C16 N3 C19 O3 2(2) . . . . ?
C17 N3 C19 O3 178.4(14) . . . . ?
C16 N3 C19 C18 -177.0(14) . . . . ?
C17 N3 C19 C18 0(2) . . . . ?
