Cd-MOF: Specific adsorption selectivity for linear alkyne (propyne, 2-butyne and phenylacetylene) molecules
Jin, Guo-Xia; Wang, Teng; Yue, Tai-Xing; Wang, Xiaokang; Dai, Fangna; Wu, Xiang-Wen; Liu, Qi-Kui; Ma, Jian-ping; Chemical Communications  (2021) –; doi:10.1039/D1CC05316G

data_7129266
_publ_section_title
;
 Cd-MOF: Specific adsorption selectivity for linear alkyne (propyne,
 2-butyne and phenylacetylene) molecules
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05316G
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C4 H6), 0.25(C192 H144 Cd4 N48), 2(Cl O4)'
_chemical_formula_sum            'C56 H48 Cd Cl2 N12 O8'
_chemical_formula_weight         1200.36
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-11-02
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_audit_update_record
;
2021-11-05 deposited with the CCDC.	2021-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8898(3)
_cell_length_b                   15.8898(3)
_cell_length_c                   21.4310(7)
_cell_measurement_reflns_used    4232
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      69.9660
_cell_measurement_theta_min      4.4180
_cell_volume                     5411.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0793
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9986
_diffrn_measured_fraction_theta_max 0.9727
_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    -13.00  23.00   1.00    1.00    --    0.00  95.00 -62.00   36
  2  \w    -24.00   3.00   1.00    1.00    --    0.00  37.00-150.00   27
  3  \w     27.00  64.00   1.00    1.00    --    0.00  37.00-150.00   37
  4  \w     98.00 123.00   1.00    2.09    --   54.00  57.00-120.00   25
  5  \w     36.00 123.00   1.00    2.09    --   54.00  57.00 120.00   87
  6  \w     49.00  96.00   1.00    2.09    --   54.00-125.00-180.00   47
  7  \w     51.00 118.00   1.00    2.09    --  108.00 -50.00 -90.00   67
  8  \w     60.00  87.00   1.00    2.09    --  108.00 -63.00 -60.00   27
  9  \w     70.00 112.00   1.00    2.09    --  108.00-111.00-180.00   42
 10  \w     96.00 129.00   1.00    2.09    --  108.00 -63.00 -60.00   33
 11  \w     47.00 132.00   1.00    2.09    --  108.00 -37.00  60.00   85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0423457000
_diffrn_orient_matrix_UB_12      0.0741502000
_diffrn_orient_matrix_UB_13      0.0341028000
_diffrn_orient_matrix_UB_21      0.0800067000
_diffrn_orient_matrix_UB_22      -0.0533220000
_diffrn_orient_matrix_UB_23      0.0091579000
_diffrn_orient_matrix_UB_31      0.0346523000
_diffrn_orient_matrix_UB_32      0.0324683000
_diffrn_orient_matrix_UB_33      -0.0626541000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10897
_diffrn_reflns_theta_full        67.02
_diffrn_reflns_theta_max         67.03
_diffrn_reflns_theta_min         3.46
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.698
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.959
_refine_diff_density_min         -2.622
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         4833
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1175
_refine_ls_R_factor_gt           0.1094
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1373P)^2^+55.0740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2754
_refine_ls_wR_factor_ref         0.2835
_reflns_number_gt                4364
_reflns_number_total             4833
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1cc05316g2.cif
_cod_data_source_block           exp_3739
_cod_database_code               7129266
_chemical_oxdiff_formula         'C1 H1 N1 O1 Cd1 Cl1'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
C37 \\sim C40 \\sim C38 \\sim C39 \\sim O4 \\sim O5: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: O2(0.5) Cl1(0.5)
4.a Riding coordinates:
 N5(H5A,H5B)
4.b Me refined with riding coordinates:
 C40(H40A,H40B,H40C)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C7(H7), C9(H9), C11(H11), C17(H17), C19(H19), C20(H20), C21(H21),
 C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30)
4.d Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.101
_oxdiff_exptl_absorpt_empirical_full_min 0.822