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_7129265
_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         '0.25(C192 H144 Cd4 N48), Cl2 O8, 2(C3 H4)'
_chemical_formula_sum            'C54 H44 Cd Cl2 N12 O8'
_chemical_formula_weight         1172.31
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-11-14
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_audit_update_record
;
2021-09-18 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                   15.8548(3)
_cell_length_b                   15.8548(3)
_cell_length_c                   21.4208(5)
_cell_measurement_reflns_used    4901
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      70.8520
_cell_measurement_theta_min      5.7040
_cell_volume                     5384.65(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0793
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9989
_diffrn_measured_fraction_theta_max 0.9542
_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    -16.00  13.00   1.00    1.00    --    0.00  57.00 -90.00   29
  2  \w     34.00  68.00   1.00    1.00    --    0.00  57.00 -90.00   34
  3  \w     61.00 105.00   1.00    1.00    --   54.00  57.00  60.00   44
  4  \w    103.00 135.00   1.00    1.00    --  108.00 111.00 -30.00   32
  5  \w    152.00 178.00   1.00    1.00    --  108.00 111.00-150.00   26
  6  \w    100.00 138.00   1.00    1.00    --  108.00 111.00-150.00   38
  7  \w     78.00 151.00   1.00    1.00    --  108.00 178.00-120.00   73
  8  \w     47.00 110.00   1.00    1.00    --  108.00-111.00-150.00   63
  9  \w     74.00 108.00   1.00    1.00    --   54.00-125.00-120.00   34
 10  \w     23.00  85.00   1.00    1.00    --   54.00-125.00-150.00   62
 11  \w    -64.00 -39.00   1.00    1.00    --    0.00 147.00-156.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0071617000
_diffrn_orient_matrix_UB_12      -0.0966516000
_diffrn_orient_matrix_UB_13      -0.0031424000
_diffrn_orient_matrix_UB_21      -0.0347356000
_diffrn_orient_matrix_UB_22      0.0013247000
_diffrn_orient_matrix_UB_23      -0.0672027000
_diffrn_orient_matrix_UB_31      0.0906109000
_diffrn_orient_matrix_UB_32      0.0082264000
_diffrn_orient_matrix_UB_33      -0.0254629000
_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  0.0283
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            10200
_diffrn_reflns_theta_full        70.85
_diffrn_reflns_theta_max         70.86
_diffrn_reflns_theta_min         3.47
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.708
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.029(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         4955
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0543P)^2^+4.8376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.1014
_reflns_number_gt                4520
_reflns_number_total             4955
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1cc05316g2.cif
_cod_data_source_block           exp_3305
_cod_original_cell_volume        5384.63(19)
_cod_database_code               7129265
_chemical_oxdiff_formula         'C1 H1 O1 N1 Cd1 Cl1'
_reflns_odcompleteness_completeness 99.89
_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. Restrained distances
 O4-Cl2 \\sim O5-Cl2 \\sim O6-Cl2 \\sim O7-Cl2
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C25 \\sim C26 \\sim C27: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O4(0.5) O2(0.5) Cl3(0.5) O5(0.5) O6(0.5) O7(0.5)
5.a Riding coordinates:
 N5(H5A,H5B)
5.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C22(H22), C4(H4), C11(H11), C2(H2), C21(H21), C24(H24), C8(H8),
 C9(H9), C5(H5), C7(H7), C17(H17), C23(H23), C1(H1), C15(H15), C16(H16)
5.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C)
5.d :
 C25(H25)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.158
_oxdiff_exptl_absorpt_empirical_full_min 0.855