#------------------------------------------------------------------------------
#$Date: 2019-11-24 06:15:34 +0200 (Sun, 24 Nov 2019) $
#$Revision: 236921 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/98/4349882.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_4349882
loop_
_publ_author_name
'He, Chun-Ting'
'Ye, Zi-Ming'
'Xu, Yan-Tong'
'Xie, Yi'
'Lian, Xin-Lu'
'Zhang, Jie-Peng'
'Chen, Xiao-Ming'
_publ_section_title
;
 A flexible metal--organic framework with adaptive pores for high
 column-capacity gas chromatographic separation
;
_journal_issue                   11
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              2777
_journal_paper_doi               10.1039/C8QI00684A
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         '0.25(C144 H128 N24 O24 Zn8), 2(C6 H6)'
_chemical_formula_sum            'C48 H44 N6 O6 Zn2'
_chemical_formula_weight         931.63
_space_group_crystal_system      orthorhombic
_space_group_IT_number           73
_space_group_name_Hall           '-I 2b 2c'
_space_group_name_H-M_alt        'I b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-11 deposited with the CCDC.
2018-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.2385(11)
_cell_length_b                   22.5360(14)
_cell_length_c                   23.4694(15)
_cell_measurement_reflns_used    3705
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.689
_cell_measurement_theta_min      2.286
_cell_volume                     9117.6(10)
_computing_cell_refinement       'SAINT V6.36A (?, 2016)'
_computing_data_reduction        'SAINT V6.36A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      153.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            17687
_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         25.996
_diffrn_reflns_theta_min         1.807
_exptl_absorpt_coefficient_mu    1.107
_exptl_absorpt_correction_T_max  0.8090
_exptl_absorpt_correction_T_min  0.7325
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3856
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4469
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0570
_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)+(0.0696P)²+40.3113P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3430
_reflns_number_total             4469
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8qi00684a2.cif
_cod_data_source_block           1C6H6
_cod_database_code               4349882
_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.
;
_shelx_estimated_absorpt_t_max   0.809
_shelx_estimated_absorpt_t_min   0.732
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C25-C24
 1.36 with sigma of 0.001
 C26-C25
 1.36 with sigma of 0.001
 C27-C26
 1.36 with sigma of 0.001
 C27-C26_$1
 1.36 with sigma of 0.001
 C26_$1-C25_$1
 1.36 with sigma of 0.001
 C25_$1-C24
 1.36 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C27) = Uanis(C26) = Uanis(C25) = Uanis(C24) = Uanis(C25) = Uanis(C26)
4.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C4(H4), C6(H6), C7(H7), C17(H17), C18(H18), C23(H23),
 C22(H22), C21(H21), C24(H24), C25(H25), C26(H26), C27(H27)
4.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'x+1/2, -y, z'
'-x, y, 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
Zn1 Zn 0.60098(2) 0.72890(2) 0.86697(2) 0.02250(16) Uani 1 1 d . . .
N1 N 0.76471(19) 0.29412(14) 0.91111(16) 0.0328(8) Uani 1 1 d . . .
H1 H 0.7439 0.2600 0.9209 0.039 Uiso 1 1 calc R . .
N2 N 0.8353(2) 0.30018(14) 0.88637(16) 0.0302(8) Uani 1 1 d . . .
N3 N 0.53860(18) 0.74203(14) 0.79788(13) 0.0241(7) Uani 1 1 d . . .
O1 O 0.65926(18) 0.65638(12) 0.85954(13) 0.0361(7) Uani 1 1 d . . .
O2 O 0.7590(2) 0.67598(13) 0.91702(17) 0.0505(9) Uani 1 1 d . . .
O3 O 0.54154(18) 0.78786(12) 0.43670(12) 0.0331(7) Uani 1 1 d . . .
C1 C 0.7177(2) 0.64165(17) 0.8895(2) 0.0309(9) Uani 1 1 d . . .
C2 C 0.7358(2) 0.57592(17) 0.8909(2) 0.0308(9) Uani 1 1 d . . .
C3 C 0.6938(3) 0.53705(19) 0.8578(2) 0.0402(11) Uani 1 1 d . . .
H3 H 0.6541 0.5516 0.8334 0.048 Uiso 1 1 calc R . .
C4 C 0.7093(3) 0.47661(19) 0.8600(2) 0.0440(12) Uani 1 1 d . . .
H4 H 0.6803 0.4501 0.8368 0.053 Uiso 1 1 calc R . .
C5 C 0.7668(2) 0.45432(16) 0.8955(2) 0.0310(9) Uani 1 1 d . . .
C6 C 0.8085(3) 0.49418(19) 0.9284(2) 0.0435(12) Uani 1 1 d . . .
H6 H 0.8479 0.4800 0.9532 0.052 Uiso 1 1 calc R . .
C7 C 0.7936(3) 0.55465(18) 0.9255(2) 0.0432(12) Uani 1 1 d . . .
H7 H 0.8236 0.5815 0.9477 0.052 Uiso 1 1 calc R . .
C8 C 0.7810(2) 0.38921(18) 0.8982(2) 0.0312(9) Uani 1 1 d . . .
C9 C 0.7309(2) 0.34715(17) 0.9187(2) 0.0329(10) Uani 1 1 d . . .
C10 C 0.8460(2) 0.35886(17) 0.87877(19) 0.0313(10) Uani 1 1 d . . .
C11 C 0.6528(3) 0.3537(2) 0.9463(3) 0.0501(14) Uani 1 1 d . . .
H11A H 0.6505 0.3289 0.9805 0.075 Uiso 1 1 calc GR . .
H11B H 0.6123 0.3411 0.9195 0.075 Uiso 1 1 calc GR . .
H11C H 0.6445 0.3953 0.9568 0.075 Uiso 1 1 calc GR . .
C12 C 0.9202(3) 0.38210(19) 0.8537(2) 0.0444(12) Uani 1 1 d . . .
H12A H 0.9288 0.3639 0.8163 0.067 Uiso 1 1 calc GR . .
H12B H 0.9636 0.3723 0.8790 0.067 Uiso 1 1 calc GR . .
H12C H 0.9167 0.4253 0.8494 0.067 Uiso 1 1 calc GR . .
C13 C 0.5619(2) 0.73781(18) 0.74335(17) 0.0290(9) Uani 1 1 d . . .
C14 C 0.6441(3) 0.7210(3) 0.7289(2) 0.0548(15) Uani 1 1 d . . .
H14A H 0.6655 0.6962 0.7594 0.082 Uiso 1 1 calc GR . .
H14B H 0.6755 0.7570 0.7250 0.082 Uiso 1 1 calc GR . .
H14C H 0.6448 0.6989 0.6929 0.082 Uiso 1 1 calc GR . .
C15 C 0.5000 0.7500 0.7075(2) 0.0270(12) Uani 1 2 d S T P
C16 C 0.5000 0.7500 0.6444(2) 0.0276(12) Uani 1 2 d S T P
C17 C 0.4450(2) 0.71744(18) 0.61378(18) 0.0311(9) Uani 1 1 d . . .
H17 H 0.4068 0.6953 0.6338 0.037 Uiso 1 1 calc R . .
C18 C 0.4452(2) 0.71684(18) 0.55502(18) 0.0289(9) Uani 1 1 d . . .
H18 H 0.4080 0.6938 0.5349 0.035 Uiso 1 1 calc R . .
C19 C 0.5000 0.7500 0.5252(2) 0.0242(11) Uani 1 2 d S T P
C20 C 0.5000 0.7500 0.4617(2) 0.0284(13) Uani 1 2 d S T P
C23 C 0.5254(4) 0.4994(4) 0.9454(3) 0.0766(19) Uani 1 1 d . . .
H23 H 0.5433 0.4988 0.9071 0.092 Uiso 1 1 calc R . .
C22 C 0.5319(3) 0.5499(3) 0.9769(4) 0.0702(19) Uani 1 1 d . . .
H22 H 0.5540 0.5847 0.9607 0.084 Uiso 1 1 calc R . .
C21 C 0.5064(4) 0.5502(3) 1.0317(4) 0.0731(19) Uani 1 1 d . . .
H21 H 0.5109 0.5852 1.0540 0.088 Uiso 1 1 calc R . .
C24 C 0.8670(10) 0.5000 0.7500 0.179(3) Uani 1 2 d DS TU P
H24 H 0.8119 0.5000 0.7500 0.215 Uiso 1 2 calc RS T P
C25 C 0.9098(5) 0.5384(6) 0.7818(6) 0.179(3) Uani 1 1 d D U .
H25 H 0.8824 0.5653 0.8056 0.215 Uiso 1 1 calc R . .
C26 C 0.9886(5) 0.5415(5) 0.7823(5) 0.179(3) Uani 1 1 d D U .
H26 H 1.0160 0.5705 0.8036 0.215 Uiso 1 1 calc R . .
C27 C 1.0253(11) 0.5000 0.7500 0.179(3) Uani 1 2 d DS TU P
H27 H 1.0804 0.5000 0.7500 0.215 Uiso 1 2 calc RS T 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'
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
N3 Zn1 N2 111.54(14) . 12_765
O1 Zn1 N2 114.57(14) . 12_765
O1 Zn1 N3 109.75(13) . .
O1 Zn1 O3 100.60(13) . 11_576
O3 Zn1 N2 104.54(14) 11_576 12_765
O3 Zn1 N3 115.45(13) 11_576 .
N2 N1 H1 124.5 . .
C9 N1 H1 124.5 . .
C9 N1 N2 110.9(3) . .
N1 N2 Zn1 120.7(2) . 12_755
C10 N2 Zn1 133.1(3) . 12_755
C10 N2 N1 106.2(3) . .
N3 N3 Zn1 124.52(9) 6_564 .
C13 N3 Zn1 127.6(3) . .
C13 N3 N3 107.9(2) . 6_564
C1 O1 Zn1 125.7(3) . .
C20 O3 Zn1 123.6(3) . 11_575
O1 C1 C2 115.5(4) . .
O2 C1 O1 125.6(4) . .
O2 C1 C2 118.8(4) . .
C3 C2 C1 120.0(4) . .
C7 C2 C1 120.3(4) . .
C7 C2 C3 119.6(4) . .
C2 C3 H3 120.0 . .
C2 C3 C4 120.1(4) . .
C4 C3 H3 120.0 . .
C3 C4 H4 119.5 . .
C3 C4 C5 120.9(4) . .
C5 C4 H4 119.5 . .
C4 C5 C8 119.9(4) . .
C6 C5 C4 118.1(4) . .
C6 C5 C8 122.0(4) . .
C5 C6 H6 119.6 . .
C5 C6 C7 120.9(4) . .
C7 C6 H6 119.6 . .
C2 C7 C6 120.4(4) . .
C2 C7 H7 119.8 . .
C6 C7 H7 119.8 . .
C9 C8 C5 126.3(4) . .
C9 C8 C10 106.4(4) . .
C10 C8 C5 127.2(4) . .
N1 C9 C8 107.2(4) . .
N1 C9 C11 122.3(4) . .
C8 C9 C11 130.5(4) . .
N2 C10 C8 109.3(4) . .
N2 C10 C12 120.7(4) . .
C8 C10 C12 130.1(4) . .
C9 C11 H11A 109.5 . .
C9 C11 H11B 109.5 . .
C9 C11 H11C 109.5 . .
H11A C11 H11B 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C10 C12 H12A 109.5 . .
C10 C12 H12B 109.5 . .
C10 C12 H12C 109.5 . .
H12A C12 H12B 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
N3 C13 C14 120.9(4) . .
N3 C13 C15 109.5(4) . .
C15 C13 C14 129.6(4) . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14B 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C13 C15 C13 105.3(5) 6_564 .
C13 C15 C16 127.4(2) . .
C13 C15 C16 127.4(2) 6_564 .
C17 C16 C15 120.9(3) 6_564 .
C17 C16 C15 120.9(3) . .
C17 C16 C17 118.2(5) 6_564 .
C16 C17 H17 119.4 . .
C18 C17 C16 121.1(4) . .
C18 C17 H17 119.4 . .
C17 C18 H18 120.0 . .
C17 C18 C19 119.9(4) . .
C19 C18 H18 120.0 . .
C18 C19 C18 119.7(5) 6_564 .
C18 C19 C20 120.2(3) 6_564 .
C18 C19 C20 120.2(3) . .
O3 C20 O3 124.4(5) 6_564 .
O3 C20 C19 117.8(3) . .
O3 C20 C19 117.8(3) 6_564 .
C22 C23 H23 119.7 . .
C21 C23 H23 119.7 9_667 .
C21 C23 C22 120.5(7) 9_667 .
C23 C22 H22 120.4 . .
C21 C22 C23 119.3(6) . .
C21 C22 H22 120.4 . .
C23 C21 C22 120.2(6) 9_667 .
C23 C21 H21 119.9 9_667 .
C22 C21 H21 119.9 . .
C25 C24 H24 122.8 . .
C25 C24 H24 122.8 8_456 .
C25 C24 C25 114.4(19) . 8_456
C24 C25 H25 117.3 . .
C26 C25 C24 125.3(16) . .
C26 C25 H25 117.3 . .
C25 C26 H26 122.4 . .
C25 C26 C27 115.2(16) . .
C27 C26 H26 122.4 . .
C26 C27 C26 124.5(19) 8_456 .
C26 C27 H27 117.8 8_456 .
C26 C27 H27 117.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N2 1.999(3) 12_765
Zn1 N3 1.968(3) .
Zn1 O1 1.926(3) .
Zn1 O3 1.967(3) 11_576
N1 H1 0.8800 .
N1 N2 1.355(5) .
N1 C9 1.342(5) .
N2 Zn1 1.999(3) 12_755
N2 C10 1.347(5) .
N3 N3 1.378(6) 6_564
N3 C13 1.345(5) .
O1 C1 1.273(5) .
O2 C1 1.234(5) .
O3 Zn1 1.967(3) 11_575
O3 C20 1.259(4) .
C1 C2 1.514(5) .
C2 C3 1.378(6) .
C2 C7 1.371(6) .
C3 H3 0.9500 .
C3 C4 1.389(6) .
C4 H4 0.9500 .
C4 C5 1.389(6) .
C5 C6 1.385(6) .
C5 C8 1.489(5) .
C6 H6 0.9500 .
C6 C7 1.388(6) .
C7 H7 0.9500 .
C8 C9 1.370(6) .
C8 C10 1.389(6) .
C9 C11 1.501(6) .
C10 C12 1.503(6) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 C14 1.505(6) .
C13 C15 1.386(5) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 C13 1.386(5) 6_564
C15 C16 1.482(8) .
C16 C17 1.398(5) .
C16 C17 1.398(5) 6_564
C17 H17 0.9500 .
C17 C18 1.379(6) .
C18 H18 0.9500 .
C18 C19 1.393(5) .
C19 C18 1.393(5) 6_564
C19 C20 1.490(7) .
C20 O3 1.259(4) 6_564
C23 H23 0.9500 .
C23 C22 1.363(10) .
C23 C21 1.354(9) 9_667
C22 H22 0.9500 .
C22 C21 1.359(10) .
C21 C23 1.354(9) 9_667
C21 H21 0.9500 .
C24 H24 0.9500 .
C24 C25 1.3601(7) 8_456
C24 C25 1.3601(7) .
C25 H25 0.9500 .
C25 C26 1.3599(7) .
C26 H26 0.9500 .
C26 C27 1.3600(7) .
C27 C26 1.3600(7) 8_456
C27 H27 0.9500 .
