A new type of C2H2 binding site in a cis-bridging hexafluorosilicate ultramicroporous material that offers trace C2H2 capture
Song, Bai-Qiao; Gao, Mei-Yan; Mercene van Wyk, Lisa; Deng, Cheng-Hua; Eaby, Alan C.; Wang, Shi-Qiang; Darwish, Shaza; Li, Dan; Qin, Shao-Jie; Peng, Yun-Lei; Yang, Qing-Yuan; Barbour, Leonard J.; Zaworotko, Michael J.; Chemical Science 16 (2025) 9010–9019; doi:10.1039/D5SC00697J

data_1574479
_publ_section_title
;
 A new type of C2H2 binding site in a cis-bridging hexafluorosilicate
 ultramicroporous material that offers trace C2H2 capture
;
_journal_issue                   20
_journal_name_full               'Chemical Science'
_journal_page_first              9010
_journal_page_last               9019
_journal_paper_doi               10.1039/D5SC00697J
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C28 H26 Cu F6 N8 Si, 1.5(C2 H2)'
_chemical_formula_sum            'C31 H29 Cu F6 N8 Si'
_chemical_formula_weight         719.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-04-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-04-24 deposited with the CCDC.	2025-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                60.939(2)
_cell_angle_beta                 77.661(2)
_cell_angle_gamma                62.396(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5344(2)
_cell_length_b                   13.1083(3)
_cell_length_c                   13.4560(3)
_cell_measurement_reflns_used    18089
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      74.0740
_cell_measurement_theta_min      3.9750
_cell_volume                     1712.38(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.948
_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     68.00  99.00   0.50    0.05    --   55.73  45.00 120.00   62
  2  \w     64.00 107.00   0.50    0.05    --   55.73  45.00  30.00   86
  3  \w     93.00 129.00   0.50    0.05    --   87.28  30.00 -60.00   72
  4  \w     65.00 102.00   0.50    0.05    --   55.73  45.00 -90.00   74
  5  \w     75.00 114.00   0.50    0.05    --   66.80  45.00-180.00   78
  6  \w    110.00 135.00   0.50    0.05    --   87.28  30.00-180.00   50
  7  \w     93.00 136.00   0.50    0.05    --   87.28  30.00-150.00   86
  8  \w     95.00 132.00   0.50    0.05    --   87.28  30.00 -90.00   74
  9  \w     99.00 129.00   0.50    0.05    --   87.28  30.00  60.00   60
 10  \w     72.00 107.00   0.50    0.05    --   87.28  15.00  30.00   70
 11  \w   -109.00 -64.00   0.50    0.05    --  -56.42 -45.00 150.00   90
 12  \w   -133.00 -90.00   0.50    0.05    --  -82.00 -45.00  90.00   86
 13  \w   -134.00 -94.00   0.50    0.05    --  -82.00 -45.00  60.00   80
 14  \w   -110.00 -75.00   0.50    0.05    --  -67.86 -45.00  30.00   70
 15  \w   -130.00 -86.00   0.50    0.05    --  -77.48 -45.00   0.00   88
 16  \w   -134.00 -91.00   0.50    0.05    --  -82.00 -45.00 -30.00   86
 17  \w   -133.00 -97.00   0.50    0.05    --  -82.00 -45.00 -60.00   72
 18  \w   -137.00 -96.00   0.50    0.05    --  -82.00 -30.00-150.00   82
 19  \w   -101.00 -39.00   0.50    0.05    --  -77.48 -15.00  60.00  124
 20  \w    -54.00 -28.00   0.50    0.05    --  -77.48 112.00 150.00   52
 21  \w    -97.00 -56.00   0.50    0.05    --  -82.00 112.00 150.00   82
 22  \w    -90.00 -26.00   0.50    0.05    --  -77.48 112.00  60.00  128
 23  \w    -66.00 -26.00   0.50    0.05    --  -77.48 112.00   0.00   80
 24  \w    -82.00 -25.00   0.50    0.05    --  -77.48 112.00-120.00  114
 25  \w    -97.00 -33.00   0.50    0.05    --  -82.00 112.00-150.00  128
 26  \w    -97.00 -59.00   0.50    0.05    --  -82.00 112.00-180.00   76
 27  \w    -55.00 -30.00   0.50    0.05    --  -82.00 112.00-180.00   50
 28  \w    -31.00  -3.00   0.50    0.05    --  -56.42  45.00-150.00   56
 29  \w    -31.00  -3.00   0.50    0.05    --  -56.42  45.00 -90.00   56
 30  \w    -29.00  -3.00   0.50    0.05    --  -56.42  45.00 -30.00   52
 31  \w    -31.00  -6.00   0.50    0.05    --  -56.42  45.00   0.00   50
 32  \w    -29.00  -3.00   0.50    0.05    --  -56.42  45.00  90.00   52
 33  \w    -31.00  -5.00   0.50    0.05    --  -56.42  45.00 150.00   52
 34  \w     48.00  74.00   0.50    0.05    --   87.28 -81.00 -71.00   52
 35  \w     49.00  96.00   0.50    0.05    --   87.28-112.00-180.00   94
 36  \w     38.00  64.00   0.50    0.05    --   87.28-112.00 -30.00   52
 37  \w     71.00  96.00   0.50    0.05    --   87.28-112.00 -60.00   50
 38  \w     71.00  96.00   0.50    0.05    --   87.28-112.00 -30.00   50
 39  \w     68.00  93.00   0.50    0.05    --   87.28 -95.00 -60.00   50
 40  \w     59.00  96.00   0.50    0.05    --   87.28-112.00  30.00   74
 41  \w     71.00  96.00   0.50    0.05    --   87.28-112.00  60.00   50
 42  \w     53.00  96.00   0.50    0.05    --   87.28-112.00 120.00   86
 43  \w     24.00  79.00   0.50    0.05    --   66.80 -95.00 150.00  110
 44  \w     40.00  65.00   0.50    0.05    --   87.28 -95.00 150.00   50
 45  \w     57.00  93.00   0.50    0.05    --   87.28 -95.00 120.00   72
 46  \w     35.00  95.00   0.50    0.05    --   83.67-107.00  76.94  120
 47  \w     43.00  69.00   0.50    0.05    --   87.28 -95.00   0.00   52
 48  \w     39.00  92.00   0.50    0.05    --   80.06 -95.00 -30.00  106
 49  \w     37.00  62.00   0.50    0.05    --   80.06 -81.00 -71.00   50
 50  \w     21.00  49.00   0.50    0.05    --   66.80 -95.00-120.00   56
 51  \w     40.00  93.00   0.50    0.05    --   87.28 -95.00-150.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0502641000
_diffrn_orient_matrix_UB_12      -0.0781575000
_diffrn_orient_matrix_UB_13      0.1104156000
_diffrn_orient_matrix_UB_21      -0.0357437000
_diffrn_orient_matrix_UB_22      -0.0498866000
_diffrn_orient_matrix_UB_23      -0.0645772000
_diffrn_orient_matrix_UB_31      0.1242423000
_diffrn_orient_matrix_UB_32      -0.1156550000
_diffrn_orient_matrix_UB_33      0.0282376000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24859
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.720
_diffrn_reflns_theta_min         3.980
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.824
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6668
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0603P)^2^+2.3718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1259
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6096
_reflns_number_total             6668
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00697j2.cif
_cod_data_source_block           SIFSIX-bidmb-Cu_C2H2
_cod_depositor_comments
'Adding full bibliography for 1574477--1574483.cif.'
_cod_original_cell_volume        1712.38(7)
_cod_database_code               1574479
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.712
_shelx_estimated_absorpt_t_min   0.611
_diffrn_oxdiff_digest_frames
;
01cdac48d70e4c2bcca8413226d8b1f628037981360
;
_diffrn_oxdiff_digest_hkl
;
01804780460dbce05a234b7123c8e7a41272ab
;
_reflns_odcompleteness_completeness 99.48
_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
2. Others
 Fixed Sof: C16(0.5) H16A(0.5) H16B(0.5) H16C(0.5) C8(0.5) H8A(0.5) H8B(0.5)
 H8C(0.5) C6(0.5) H6A(0.5) H6B(0.5) H6C(0.5) C12(0.5) H12A(0.5) H12B(0.5)
 H12C(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C1(H1), C24(H24), C17(H17), C26(H26), C11(H11), C2(H2), C9(H9),
 C3(H3), C19(H19), C10(H10), C21(H21), C28(H28), C25(H25)
3.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C30(H30A,H30B,H30C), C16(H16A,H16B,H16C), C8(H8A,H8B,
 H8C), C6(H6A,H6B,H6C), C12(H12A,H12B,H12C)
3.c :
 C32(H32), C33(H33), C31(H31)
;
_shelx_res_checksum              73685
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.869
_oxdiff_exptl_absorpt_empirical_full_min 0.646