Efficient separation of C<sub>2</sub>H<sub>2</sub> from C<sub>2</sub>H<sub>2</sub>/CO<sub>2</sub> mixtures in an acid-base resistant metal-organic framework.
Zhang, Ling; Jiang, Ke; Li, Libo; Xia, Yu-Pei; Hu, Tong-Liang; Yang, Yu; Cui, Yuanjing; Li, Bin; Chen, Banglin; Qian, Guodong; Chemical communications (Cambridge, England) 54 (2018) 4846–4849; doi:10.1039/c8cc02235f

data_7121491
_publ_section_title
;
 Efficient separation of C<sub>2</sub>H<sub>2</sub> from
 C<sub>2</sub>H<sub>2</sub>/CO<sub>2</sub> mixtures in an acid-base
 resistant metal-organic framework.
;
_journal_issue                   38
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4846
_journal_page_last               4849
_journal_paper_doi               10.1039/c8cc02235f
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C7 H4 N O3 Zn'
_chemical_formula_sum            'C7 H4 N O3 Zn'
_chemical_formula_weight         215.48
_space_group_crystal_system      tetragonal
_space_group_IT_number           91
_space_group_name_Hall           'P 4w 2c'
_space_group_name_H-M_alt        'P 41 2 2'
_symmetry_space_group_name_Hall  'P 4w 2c'
_symmetry_space_group_name_H-M   'P 41 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-04-09
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-04-12 deposited with the CCDC.
2018-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.88630(10)
_cell_length_b                   12.88630(10)
_cell_length_c                   13.2102(3)
_cell_measurement_reflns_used    3996
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.5780
_cell_measurement_theta_min      5.8630
_cell_volume                     2193.64(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9d (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      1.00  27.00   0.50    1.00    --    0.00  82.00 -90.00   52
  2  \w    -33.00  32.00   0.50    1.00    --    0.00  82.00  60.00  130
  3  \w     66.00 172.00   0.50    2.00    --   95.20  15.00  30.00  212
  4  \w    144.00 185.00   0.50    2.00    --   95.20  82.00 -90.00   82
  5  \w    143.00 185.00   0.50    2.00    --   95.20  82.00 -60.00   84
  6  \w    154.00 179.00   0.50    2.00    --   95.20  82.00 150.00   50
  7  \w     76.00 110.00   0.50    2.00    --   95.20 -77.00  60.00   68
  8  \w     43.00  73.00   0.50    2.00    --   95.20 -77.00  60.00   60
  9  \w    121.00 146.00   0.50   20.00    --   95.80  82.00  60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1152398000
_diffrn_orient_matrix_UB_12      -0.0010428000
_diffrn_orient_matrix_UB_13      0.0308684000
_diffrn_orient_matrix_UB_21      -0.0031383000
_diffrn_orient_matrix_UB_22      0.1192115000
_diffrn_orient_matrix_UB_23      -0.0074050000
_diffrn_orient_matrix_UB_31      -0.0316693000
_diffrn_orient_matrix_UB_32      -0.0081856000
_diffrn_orient_matrix_UB_33      -0.1122665000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6476
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.240
_diffrn_reflns_theta_min         3.430
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.920
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9d (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.48(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         2022
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0355
_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/[\s^2^(Fo^2^)+(0.0527P)^2^+1.6343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.0968
_reflns_Friedel_coverage         0.661
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1934
_reflns_number_total             2022
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc02235f2.cif
_cod_data_source_block           zhangl_pl_sq
_cod_depositor_comments          'Adding full bibliography for 7121491.cif.'
_cod_database_code               7121491
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.566
_shelx_estimated_absorpt_t_min   0.506
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.52(8)
 0.48(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(Zn2A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 Zn2A, Zn2, N1, C6, C1, O1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H1BC)=Sof(H1BD)=Sof(Zn2A)=0.5*(1-FVAR(2))
 Sof(Zn2)=Sof(H1AA)=Sof(H1AB)=0.5*FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 N1(H1AA,H1AB), N1(H1BC,H1BD)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C2(H2)
;
_shelx_res_checksum              78066
_shelx_fab_checksum              57807
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.296
_oxdiff_exptl_absorpt_empirical_full_min 0.778