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_1574481
_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'
_chemical_formula_sum            'C28 H26 Cu F6 N8 Si'
_chemical_formula_weight         680.20
_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             2024-06-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-06-13 deposited with the CCDC.	2025-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                61.138(2)
_cell_angle_beta                 77.6840(10)
_cell_angle_gamma                62.477(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5027(2)
_cell_length_b                   13.1215(2)
_cell_length_c                   13.3760(2)
_cell_measurement_reflns_used    17125
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.8170
_cell_measurement_theta_min      3.9910
_cell_volume                     1704.18(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_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                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.950
_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     54.00  80.00   0.50    0.05    --  104.67-125.00-150.00   52
  2  \w     64.00  99.00   0.50    0.05    --  104.67-125.00   0.00   70
  3  \w     35.00  65.00   0.50    0.05    --  104.67-125.00  30.00   60
  4  \w     43.00  92.00   0.50    0.05    --  104.67-125.00  90.00   98
  5  \w     66.00 111.00   0.50    0.05    --  104.67-125.00 150.00   90
  6  \w     38.00  65.00   0.50    0.05    --  104.67-125.00 150.00   54
  7  \w     79.00 104.00   0.50    0.05    --  104.67 -94.00 120.00   50
  8  \w     41.00  94.00   0.50    0.05    --  104.67-125.00 -90.00  106
  9  \w     36.00 107.00   0.50    0.05    --  104.67-106.00 -87.20  142
 10  \w     68.00 100.00   0.50    0.05    --  104.67 -94.00 -90.00   64
 11  \w     35.00  62.00   0.50    0.05    --  104.67 -94.00 -90.00   54
 12  \w     -4.00  69.00   0.50    0.05    --   46.39 -77.00 150.00  146
 13  \w     -1.00  25.00   0.50    0.05    --   46.39 -48.00 159.00   52
 14  \w     39.00  68.00   0.50    0.05    --  104.67 -61.00 150.00   58
 15  \w    129.00 171.00   0.50    0.05    --  104.67  77.00  60.00   84
 16  \w     84.00 123.00   0.50    0.05    --  104.67  77.00  60.00   78
 17  \w    102.00 175.00   0.50    0.05    --  104.67  48.00 -52.00  146
 18  \w     93.00 169.00   0.50    0.05    --  104.67  30.00-120.00  152
 19  \w     99.00 174.00   0.50    0.05    --  104.67  45.00-150.00  150
 20  \w     45.00 119.00   0.50    0.05    --   46.39  48.00 -52.00  148
 21  \w   -171.00 -84.00   0.50    0.05    -- -100.00 -30.00  30.00  174
 22  \w   -139.00 -88.00   0.50    0.05    -- -100.00 -94.00  60.00  102
 23  \w   -165.00 -89.00   0.50    0.05    -- -100.00 -48.00 159.00  152
 24  \w   -118.00 -33.00   0.50    0.05    --  -46.39 -48.00 159.00  170
 25  \w   -120.00 -34.00   0.50    0.05    --  -46.39 -37.00  60.00  172
 26  \w    -54.00 -29.00   0.50    0.05    -- -100.00  45.00 150.00   50
 27  \w    -55.00 -27.00   0.50    0.05    -- -100.00  61.00 150.00   56
 28  \w    -70.00 -27.00   0.50    0.05    -- -100.00  61.00  30.00   86
 29  \w    -69.00 -38.00   0.50    0.05    -- -100.00  61.00   0.00   62
 30  \w    -73.00 -47.00   0.50    0.05    -- -100.00  61.00 -30.00   52
 31  \w    -53.00 -27.00   0.50    0.05    -- -100.00  45.00  30.00   52
 32  \w    -57.00 -31.00   0.50    0.05    -- -100.00  48.00 -52.00   52
 33  \w    -69.00 -43.00   0.50    0.05    -- -100.00  61.00-180.00   52
 34  \w    -57.00 -13.00   0.50    0.05    --  -46.39  48.00 -52.00   88
 35  \w    -10.00  17.00   0.50    0.05    --  -46.39  48.00 -52.00   54
 36  \w   -124.00 -36.00   0.50    0.05    -- -100.00 143.00  39.47  176
 37  \w    -93.00 -30.00   0.50    0.05    --  -46.39 125.00 -90.00  126
 38  \w   -111.00 -56.00   0.50    0.05    -- -100.00 125.00-180.00  110
 39  \w   -112.00 -61.00   0.50    0.05    -- -100.00 125.00 -30.00  102
 40  \w   -112.00 -41.00   0.50    0.05    -- -100.00 125.00   0.00  142
 41  \w   -108.00 -60.00   0.50    0.05    -- -100.00 110.00 179.40   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0876447000
_diffrn_orient_matrix_UB_12      -0.0410253000
_diffrn_orient_matrix_UB_13      -0.0200956000
_diffrn_orient_matrix_UB_21      0.0297771000
_diffrn_orient_matrix_UB_22      -0.1134410000
_diffrn_orient_matrix_UB_23      0.1202484000
_diffrn_orient_matrix_UB_31      -0.1036350000
_diffrn_orient_matrix_UB_32      0.0852262000
_diffrn_orient_matrix_UB_33      0.0493322000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22113
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.666
_diffrn_reflns_theta_min         3.987
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.801
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023) 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    1.326
_exptl_crystal_description       block
_exptl_crystal_F_000             694
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         6739
_refine_ls_number_restraints     323
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0487P)^2^+2.0677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1078
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6457
_reflns_number_total             6739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00697j2.cif
_cod_data_source_block           CO2@SIFSIX-bidmb-Cu_act
_cod_depositor_comments
'Adding full bibliography for 1574477--1574483.cif.'
_cod_database_code               1574481
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.652
_shelx_estimated_absorpt_t_min   0.605
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C23B, C23A, C22B, C22A, C21B, C21A, C20A, C20B, N6B, N6A, C19B, C19A, C17, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N7, C25B, C25A, C26A, C26B, N8A, N8B, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C23B \\sim C23A \\sim C22B \\sim C22A \\sim C21A \\sim C21B \\sim C20A \\sim
C20B \\sim N6B \\sim N6A \\sim C19B \\sim C19A \\sim C18 \\sim C17: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08
N7 \\sim C25A \\sim C25B \\sim C26A \\sim C26B \\sim N8B \\sim N8A \\sim C24:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(H18A)=Sof(C19B)=Sof(H19B)=1-FVAR(1)
 Sof(H18)=Sof(C19A)=Sof(H19A)=FVAR(1)
 Sof(N6B)=1-FVAR(2)
 Sof(N6A)=FVAR(2)
 Sof(C20B)=1-FVAR(3)
 Sof(C20A)=FVAR(3)
 Sof(C22B)=Sof(C23B)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C21B)=Sof(H21B)=1-FVAR(4)
 Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=FVAR(4)
 Sof(C25B)=Sof(H25B)=1-FVAR(5)
 Sof(C25A)=Sof(H25A)=FVAR(5)
 Sof(C26B)=Sof(H26B)=1-FVAR(6)
 Sof(C26A)=Sof(H26A)=FVAR(6)
 Sof(N8B)=Sof(C28B)=Sof(C27B)=Sof(H27B)=Sof(C29B)=Sof(C30B)=Sof(H30A)=
 Sof(H30B)=Sof(H30C)=1-FVAR(7)
 Sof(N8A)=Sof(C28A)=Sof(C27A)=Sof(H27A)=Sof(C29A)=Sof(C30A)=Sof(H30D)=
 Sof(H30E)=Sof(H30F)=FVAR(7)
 Fixed Sof: C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5) C12(0.5) H12A(0.5) H12B(0.5)
 H12C(0.5) C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5) C16(0.5) H16A(0.5) H16B(0.5)
 H16C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C17(H17), C24(H24), C9(H9), C18(H18A), C18(H18), C1(H1), C10(H10), C11(H11),
 C2(H2), C25B(H25B), C3(H3), C19B(H19B), C27B(H27B), C21B(H21B), C26B(H26B),
 C19A(H19A), C21A(H21A), C25A(H25A), C26A(H26A), C27A(H27A)
5.b Idealised Me refined as rotating group:
 C23B(H23A,H23B,H23C), C30B(H30A,H30B,H30C), C8(H8A,H8B,H8C), C12(H12A,H12B,
 H12C), C5(H5A,H5B,H5C), C16(H16A,H16B,H16C), C23A(H23D,H23E,H23F), C30A(H30D,
 H30E,H30F)
;
_shelx_res_checksum              55229
_shelx_fab_checksum              93452
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.624
_oxdiff_exptl_absorpt_empirical_full_min 0.571