A microporous zinc‒organic framework with Lewis basic pyridyl sites for highly selective C2H2/CH4 and C2H2/CO2 gas separation
Yan, Peng; Yang, Jucai; Hao, Xiangying; Chen, Zhisheng; Shen, Guanhua; Zhao, Yanhua; Ma, Deyun; Zhu, Jiaxin; CrystEngComm 22 (2020) 275–282; doi:10.1039/C9CE01481K

data_7238042
_publ_section_title
;
 A microporous zinc--organic framework with Lewis basic pyridyl sites for
 highly selective C2H2/CH4 and C2H2/CO2 gas separation
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              275
_journal_page_last               282
_journal_paper_doi               10.1039/C9CE01481K
_journal_volume                  22
_journal_year                    2020
_chemical_formula_moiety         '0.5(C102 H66 N10 O24 Zn6)'
_chemical_formula_sum            'C51 H33 N5 O12 Zn3'
_chemical_formula_weight         1103.99
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-12-26
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.12.08 svn.r3473 for OlexSys, GUI svn.r5433)
;
_audit_update_record
;
2019-09-20 deposited with the CCDC.	2019-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3343(12)
_cell_length_b                   25.123(2)
_cell_length_c                   18.1924(14)
_cell_measurement_reflns_used    2512
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      21.715
_cell_measurement_theta_min      2.429
_cell_volume                     6551.5(9)
_computing_cell_refinement       'SAINT V8.32B (?, 2016)'
_computing_data_reduction        'SAINT V8.32B (?, 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      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1790
_diffrn_reflns_av_unetI/netI     0.1524
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33327
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.517
_diffrn_reflns_theta_min         1.621
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.140
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       block
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
TITL t         P b c n      R = 0.12
CELL   14.3343   25.1230   18.1924     90.00     90.00     90.00
SPGR Pbcn
C101 0.215 0.319 0.470 !       5.40 eA-3
C102 0.919 0.688 0.473 !       4.20 eA-3
C103 0.139 0.296 0.486 !       3.81 eA-3
Q104 0.092 0.098 0.185 !       3.03 eA-3
C105 0.252 0.642 0.017 !       2.94 eA-3
C106 0.642 0.503 0.113 !       2.82 eA-3
Q107 0.407 0.684 0.183 !       2.58 eA-3
C108 0.762 0.801 0.111 !       2.55 eA-3
Q109 0.112 0.162 0.320 !       2.39 eA-3
Q110 0.500 0.709 0.316 !       2.36 eA-3
C111 0.174 0.494 0.371 !       1.98 eA-3
C112 0.769 0.461 0.115 !       1.90 eA-3
C113 0.324 0.967 0.378 !       1.86 eA-3
C114 0.594 0.958 0.160 !       1.85 eA-3
C115 0.288 0.297 0.422 !       1.81 eA-3
C116 0.080 0.552 0.872 !       1.54 eA-3
Q117 0.484 0.568 0.187 !       1.48 eA-3
C118 0.524 0.994 0.092 !       1.47 eA-3
C119 0.534 0.997 0.156 !       1.36 eA-3
Q120 0.874 0.107 0.209 !       1.35 eA-3
C121 0.310 0.184 0.030 !       1.35 eA-3
C122 0.643 0.032 0.084 !       1.31 eA-3
C123 0.968 0.481 0.924 !       1.31 eA-3
C124 0.880 0.410 0.140 !       1.29 eA-3
C125 0.949 0.417 0.121 !       1.26 eA-3
Q126 0.455 0.341 0.962 !       1.26 eA-3
Q127 0.534 0.620 0.049 !       1.25 eA-3
C128 0.750 0.157 0.598 !       1.25 eA-3
C129 0.188 0.578 0.904 !       1.24 eA-3
C130 0.665 0.020 0.106 !       1.24 eA-3
C131 0.904 0.522 0.110 !       1.22 eA-3
C132 0.464 0.966 0.349 !       1.20 eA-3
C133 0.920 0.534 0.087 !       1.20 eA-3
C134 0.222 0.391 0.474 !       1.19 eA-3
Q135 0.558 0.676 0.890 !       1.17 eA-3
C136 0.017 0.515 0.376 !       1.16 eA-3
Q137 0.530 0.647 0.801 !       1.15 eA-3
Q138 0.541 0.339 0.403 !       1.15 eA-3
Q139 0.406 0.444 0.313 !       1.15 eA-3
Q140 0.592 0.809 0.312 !       1.14 eA-3
C141 0.213 0.419 0.379 !       1.13 eA-3
C142 0.092 0.504 0.315 !       1.12 eA-3
C143 0.141 0.317 0.415 !       1.10 eA-3
C144 0.687 0.021 0.078 !       1.08 eA-3
C145 0.468 0.978 0.299 !       1.07 eA-3
Q146 0.613 0.521 0.361 !       1.05 eA-3
C147 0.970 0.419 0.097 !       1.05 eA-3
Q148 0.218 0.369 0.766 !       1.03 eA-3
Q149 0.463 0.352 0.910 !       1.03 eA-3
C150 0.421 0.045 0.079 !       1.02 eA-3
Q151 0.262 0.563 0.609 !       1.01 eA-3
C152 0.982 0.492 0.703 !       1.01 eA-3
C153 0.521 0.034 0.060 !       1.00 eA-3
C154 0.990 0.451 0.091 !       1.00 eA-3
Q155 0.660 0.132 0.847 !       0.99 eA-3
C156 0.500 0.977 0.253 !       0.99 eA-3
C157 0.913 0.569 0.467 !       0.99 eA-3
C158 0.060 0.530 0.956 !       0.99 eA-3
C159 0.021 0.529 0.150 !       0.98 eA-3
Q160 0.663 0.792 0.300 !       0.97 eA-3
Q161 0.487 0.364 0.541 !       0.97 eA-3
Q162 0.972 0.093 0.455 !       0.97 eA-3
C163 0.190 0.820 0.453 !       0.96 eA-3
Q164 0.596 0.377 0.653 !       0.96 eA-3
C165 0.936 0.464 0.894 !       0.95 eA-3
C166 0.860 0.287 0.113 !       0.95 eA-3
Q167 0.954 0.187 0.441 !       0.95 eA-3
Q168 0.907 0.769 0.302 !       0.95 eA-3
C169 0.781 0.261 0.035 !       0.94 eA-3
Q170 0.721 0.616 0.435 !       0.93 eA-3
C171 0.265 0.374 0.436 !       0.93 eA-3
Q172 0.341 0.124 0.235 !       0.93 eA-3
C173 0.480 0.036 0.094 !       0.93 eA-3
C174 0.907 0.531 0.047 !       0.93 eA-3
Q175 0.815 0.388 0.155 !       0.92 eA-3
C176 0.487 0.970 0.208 !       0.90 eA-3
C177 0.410 0.008 0.564 !       0.90 eA-3
C178 0.960 0.513 0.856 !       0.90 eA-3
Q179 0.010 0.884 0.419 !       0.90 eA-3
C180 0.237 0.114 0.876 !       0.89 eA-3
Q181 0.126 0.006 0.610 !       0.88 eA-3
C182 0.694 0.897 0.981 !       0.88 eA-3
C183 0.779 0.677 0.648 !       0.87 eA-3
C184 0.489 1.001 0.472 !       0.86 eA-3
Q185 0.153 0.987 0.047 !       0.86 eA-3
C186 0.609 0.008 0.013 !       0.86 eA-3
C187 0.205 0.598 0.876 !       0.85 eA-3
Q188 0.224 0.665 0.328 !       0.84 eA-3
Q189 0.357 0.740 0.467 !       0.84 eA-3
Q190 0.216 0.155 0.347 !       0.84 eA-3
C191 0.480 0.927 0.438 !       0.82 eA-3
Q192 0.568 0.297 0.919 !       0.81 eA-3
Q193 0.863 0.100 0.127 !       0.81 eA-3
Q194 0.892 0.286 0.349 !       0.81 eA-3
C195 0.021 0.467 0.968 !       0.81 eA-3
Q196 0.526 0.569 0.412 !       0.81 eA-3
Q197 1.000 0.195 0.250 !       0.80 eA-3
Q198 0.283 0.848 0.078 !       0.80 eA-3
C199 0.654 0.776 0.063 !       0.80 eA-3
;
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.800
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         7527
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      0.800
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.0519
_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/[\s^2^(Fo^2^)+(0.0370P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1145
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3356
_reflns_number_total             7527
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01481k2.cif
_cod_data_source_block           mm_sq_s
_cod_depositor_comments
;Adding full bibliography for 7238042.cif.

 Adding full bibliography for 7238042.cif.
;
_cod_database_code               7238042
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{N3, C18}
3. Restrained distances
 O4A-C13 \\sim C13-O4
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C3)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N3) = Uanis(C18)
5. Rigid body (RIGU) restrains
 O4, C13, O4A, Zn2, O3, O3A, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2, N2, C5, N2A, C6A, C7, C7A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2, C3, N2, C5, C6, C7, C3A, C6A, C7A, N2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O2(0.5) O3(0.5) O4(0.5) C3(0.5) H3(0.5) N2(0.5) C6(0.5) H6(0.5)
 C7(0.5) H7(0.5) C18(0.5) H18(0.5) H19A(0.5) H19(0.5) O2A(0.5) O4A(0.5)
 O3A(0.5) C3A(0.5) H3A(0.5) N2A(0.5) C6A(0.5) H6A(0.5) C7A(0.5) H7A(0.5) N3(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C9(H9), C10(H10), C15(H15), C16(H16), C18(H18),
 C19(H19A), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26),
 C3A(H3A), C6A(H6A), C7A(H7A)
7.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'