Crystal engineering of a new platform of hybrid ultramicroporous materials and their C<sub>2</sub>H<sub>2</sub>/CO<sub>2</sub> separation properties.
O'Hearn, Daniel J; Sensharma, Debobroto; Raza, Asif; Bezrukov, Andrey A.; Vandichel, Matthias; Mukherjee, Soumya; Zaworotko, Michael J.; Chemical science 15 (2024) 17937–17943; doi:10.1039/d4sc03029j

data_1572699
_publ_section_title
;
 Crystal engineering of a new platform of hybrid ultramicroporous
 materials and their C<sub>2</sub>H<sub>2</sub>/CO<sub>2</sub> separation
 properties.
;
_journal_issue                   43
_journal_name_full               'Chemical science'
_journal_page_first              17937
_journal_page_last               17943
_journal_paper_doi               10.1039/d4sc03029j
_journal_volume                  15
_journal_year                    2024
_chemical_absolute_configuration Unknown
_chemical_formula_moiety         'C14 H18 F6 N4 Si Zn'
_chemical_formula_sum            'C14 H18 F6 N4 Si Zn'
_chemical_formula_weight         449.78
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-09
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-05-03 deposited with the CCDC.	2024-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.704(4)
_cell_length_b                   13.535(4)
_cell_length_c                   14.921(3)
_cell_measurement_reflns_used    1361
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      51.928
_cell_measurement_theta_min      4.771
_cell_volume                     2565.6(12)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1245
_diffrn_reflns_av_unetI/netI     0.1074
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6541
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        59.042
_diffrn_reflns_theta_max         59.042
_diffrn_reflns_theta_min         4.774
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.216
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1014 before and 0.0820 after correction.
The Ratio of minimum to maximum transmission is 0.7145.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.055
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.5(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1805
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0709
_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^)+(0.1129P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1692
_refine_ls_wR_factor_ref         0.1914
_reflns_Friedel_coverage         0.722
_reflns_Friedel_fraction_full    0.955
_reflns_Friedel_fraction_max     0.953
_reflns_number_gt                1210
_reflns_number_total             1805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03029j2.cif
_cod_data_source_block           SIFSIX-24-Zn
_cod_depositor_comments          'Adding full bibliography for 1572699.cif.'
_cod_original_cell_volume        2565.5(12)
_cod_database_code               1572699
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.888
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.53427
 0.46573
2. Restrained distances
 H2-N2
 1 with sigma of 0.02
 C2-N2
 1.46 with sigma of 0.01
 H2-H1B = H2-H2B
 2.1 with sigma of 0.04
 C2-C7 \\sim C2-C4
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 N1, C3, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C7(H7), C6(H6)
4.c Fitted hexagon refined as free rotating group:
 C5(C4,C3,C7,C6,N1)
;
_shelx_res_checksum              49389
_shelx_hkl_checksum              89590
_shelx_fab_checksum              7451
_olex2_submission_special_instructions 'No special instructions were received'