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_7129267
_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(Cl O4), C48 H36 Cd N12, 0.75(C8 H6)'
_chemical_formula_sum            'C54 H40.5 Cd Cl2 N12 O8'
_chemical_formula_weight         1168.78
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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                   15.7006(2)
_cell_length_b                   16.1755(2)
_cell_length_c                   21.6748(3)
_cell_measurement_reflns_used    17472
_cell_measurement_temperature    159(14)
_cell_measurement_theta_max      70.8590
_cell_measurement_theta_min      4.0470
_cell_volume                     5504.64(12)
_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
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      159(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0793
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9881
_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    -20.00  56.00   1.00    1.00    --    0.00  57.00  30.00   76
  2  \w     29.00 120.00   1.00    1.00    --   54.00  77.00   0.00   91
  3  \w     79.00 105.00   1.00    1.00    --   54.00  57.00  90.00   26
  4  \w     47.00  95.00   1.00    1.00    --  108.00 -36.00 -26.00   48
  5  \w     53.00 118.00   1.00    1.00    --  108.00 -63.00 -60.00   65
  6  \w     72.00 117.00   1.00    1.00    --  108.00 -63.00-180.00   45
  7  \w     63.00 108.00   1.00    1.00    --  108.00-111.00-120.00   45
  8  \w     56.00 113.00   1.00    1.00    --  108.00-111.00 -30.00   57
  9  \w     91.00 116.00   1.00    1.00    --  108.00-111.00  90.00   25
 10  \w     67.00 126.00   1.00    1.00    --  108.00 -50.00 120.00   59
 11  \w     36.00 107.00   1.00    1.00    --   54.00-125.00 -30.00   71
 12  \w     42.00 133.00   1.00    1.00    --  108.00 -37.00-120.00   91
 13  \w     88.00 170.00   1.00    1.00    --  108.00  50.00 -90.00   82
 14  \w    124.00 176.00   1.00    1.00    --  108.00 111.00-120.00   52
 15  \w     67.00 151.00   1.00    1.00    --  108.00 178.00-180.00   84
 16  \w     36.00 175.00   1.00    1.00    --  108.00   0.00  60.00  139
 17  \w     56.00 101.00   1.00    1.00    --  108.00-111.00-180.00   45
 18  \w     11.00 121.00   1.00    1.00    --   54.00  19.00 -30.00  110
 19  \w     39.00 123.00   1.00    1.00    --  108.00 -37.00  90.00   84
 20  \w     23.00  76.00   1.00    1.00    --   54.00-125.00 150.00   53
 21  \w      7.00  62.00   1.00    1.00    --   54.00 -57.00  30.00   55
 22  \w    -14.00  71.00   1.00    1.00    --   54.00 -57.00 150.00   85
 23  \w    -71.00  14.00   1.00    1.00    --    0.00 -37.00-120.00   85
 24  \w     -7.00  25.00   1.00    1.00    --    0.00 -77.00-180.00   32
 25  \w    -38.00 -12.00   1.00    1.00    --    0.00 -77.00-180.00   26
;
_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      -0.0810425000
_diffrn_orient_matrix_UB_12      -0.0461657000
_diffrn_orient_matrix_UB_13      -0.0204351000
_diffrn_orient_matrix_UB_21      0.0551510000
_diffrn_orient_matrix_UB_22      -0.0710501000
_diffrn_orient_matrix_UB_23      -0.0254014000
_diffrn_orient_matrix_UB_31      -0.0040428000
_diffrn_orient_matrix_UB_32      -0.0435623000
_diffrn_orient_matrix_UB_33      0.0631390000
_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  0.0363
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39470
_diffrn_reflns_theta_full        71.00
_diffrn_reflns_theta_max         71.01
_diffrn_reflns_theta_min         3.41
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.605
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34530
_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 orange'
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2378
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.021
_refine_diff_density_min         -1.085
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.018(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         10522
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1081P)^2^+6.9170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1517
_refine_ls_wR_factor_ref         0.1573
_reflns_number_gt                9959
_reflns_number_total             10522
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1cc05316g2.cif
_cod_data_source_block           exp_3286
_cod_original_cell_volume        5504.65(13)
_cod_original_formula_sum        'C54 H40.50 Cd Cl2 N12 O8'
_cod_database_code               7129267
_chemical_oxdiff_formula         'C1 H1 O1 N1 Cd1'
_reflns_odcompleteness_completeness 99.95
_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 N(H,H) groups
2. Restrained distances
 H73-C73
 0.82 with sigma of 0.01
 H73-C72
 2.02 with sigma of 0.01
 C56-C52
 1.53 with sigma of 0.01
 O1-Cl2 = O2-Cl2 = O3-Cl2 = O4-Cl2
 1.43 with sigma of 0.01
 H55-C55 = H65-C65
 0.93 with sigma of 0.01
 H73-C66 \\sim H73-C68
 with sigma of 0.01
 C72-C66 \\sim C72-C68
 with sigma of 0.01
 O1-O2 \\sim O1-O3 \\sim O1-O4 \\sim O2-O3 \\sim O2-O4 \\sim O3-O4
 with sigma of 0.01
3. Restrained planarity
 C61, C62, C63, C64, C65, H65
 with sigma of 0.01
 C51, C52, C53, C55, C56, H55
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: O8(0.5) O9(0.5) C49(0.25) H49A(0.25) C50(0.25) H50A(0.25)
 C51(0.25) H51A(0.25) C52(0.25) C53(0.25) H53A(0.25) C54(0.25) H54A(0.25)
 C55(0.25) H55(0.25) C56(0.25) C58(0.25) H58A(0.25) C59(0.25) H59(0.25)
 C60(0.25) H60A(0.25) C61(0.25) H61A(0.25) C62(0.25) C63(0.25) H63A(0.25)
 C65(0.25) H65(0.25) C64(0.25) C66(0.25) H66A(0.25) C67(0.25) C68(0.25)
 H68A(0.25) C69(0.25) H69A(0.25) C70(0.25) H70A(0.25) C71(0.25) H71A(0.25)
 C72(0.25) C73(0.25) H73(0.25) Cl1(0.5) Cl1'(0.5)
6.a Riding coordinates:
 N5(H5B,H5C), N11(H11A,H11C), C49(H49A,C50), C49(H50A,C51), C49(H51A,C52,C53),
 C49(H53A,C54), C49(H54A), C55(H55), C58(H58A,C59), C58(H59,C60), C58(H60A,C61),
  C58(H61A,C62,C63), C58(H63A), C65(H65), C66(H66A,C67,C68), C66(H68A,C69),
 C66(H69A,C70), C66(H70A,C71), C66(H71A), C73(H73)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C11(H11), C15(H15),
 C16(H16), C17(H17), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25),
  C26(H26), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C35(H35),
 C39(H39), C40(H40), C41(H41), C43(H43), C45(H45), C46(H46), C47(H47), C48(H48)
6.c Fitted hexagon refined as free rotating group:
 C49(C55,C56), C58(C65,C64,Cl1'), C66(C72,C73,Cl2,O1,O2)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.681
_oxdiff_exptl_absorpt_empirical_full_min 0.671