Reversible switching between nonporous and porous phases of a new SIFSIX coordination network induced by a flexible linker ligand.
Song, Bai-Qiao; Yang, Qing-Yuan; Wang, Shi-Qiang; Vandichel, Matthias; Kumar, Amrit; Crowley, Clare M.; Kumar, Naveen; Deng, Cheng-Hua; Gascon Perez, Victoria; Lusi, Matteo; Wu, Hui; Zhou, Wei; Zaworotko, Michael J.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c01314

data_4134606
_publ_section_title
;
 Reversible switching between nonporous and porous phases of a new SIFSIX
 coordination network induced by a flexible linker ligand.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c01314
_journal_year                    2020
_chemical_formula_moiety         'C24 H20 Cu F6 N8 Si, H2 O'
_chemical_formula_sum            'C24 H22 Cu F6 N8 O Si'
_chemical_formula_weight         644.12
_chemical_name_systematic        SIFSIX-23-Cu-beta1
_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   mixed
_audit_creation_date             2019-10-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                64.535(4)
_cell_angle_beta                 71.549(5)
_cell_angle_gamma                74.498(3)
_cell_formula_units_Z            2
_cell_length_a                   10.4165(8)
_cell_length_b                   11.6479(8)
_cell_length_c                   12.2390(12)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      57.99
_cell_measurement_theta_min      2.63
_cell_volume                     1256.77(19)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1164
_diffrn_reflns_av_unetI/netI     0.1610
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17000
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        58.241
_diffrn_reflns_theta_max         58.241
_diffrn_reflns_theta_min         4.113
_exptl_absorpt_coefficient_mu    2.433
_exptl_absorpt_correction_T_max  0.7507
_exptl_absorpt_correction_T_min  0.0886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1657 before and 0.1048 after correction. The Ratio of minimum to maximum transmission is 0.1180. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'light blue'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_description       needle
_exptl_crystal_F_000             654
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.939
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         17000
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1821
_refine_ls_R_factor_gt           0.1333
_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^)+(0.1135P)^2^+11.3661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3287
_refine_ls_wR_factor_ref         0.3600
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11441
_reflns_number_total             17000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01314_si_003.cif
_cod_data_source_block           oo
_cod_database_code               4134606
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.793
_shelx_estimated_absorpt_t_min   0.642
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.655(12)
 0.345(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 H1A-H15_$1
 2.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.2
5.a Free rotating group:
 O1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20),
  C21(H21), C23(H23), C24(H24)
;
_shelx_res_checksum              63974
_shelx_hkl_checksum              51343
_olex2_submission_original_sample_id SIFSIX-23-Cu-beta1
_olex2_submission_special_instructions 'No special instructions were received'