Solvent-controlled elongation and mechanochemical strain in a metal-organic framework
Półrolniczak, Aleksandra; Sobczak, Szymon; Nikolayenko, Varvara; Barbour, Len; Katrusiak, Andrzej; Dalton Transactions  (2021) –; doi:10.1039/D1DT01937F

data_7708718
_publ_section_title
;
 Solvent-controlled elongation and mechanochemical strain in a
 metal-organic framework
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT01937F
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C39 H24 F6 N2 O4 S2 Zn'
_chemical_formula_sum            'C39 H24 F6 N2 O4 S2 Zn'
_chemical_formula_weight         828.09
_chemical_name_common            DMOF
_chemical_name_systematic
1,2-bis(2-ethyl-5-phenyl-3-thienyl)perfluorocyclopentene
_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
_audit_creation_date             2018-11-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-30 deposited with the CCDC.	2021-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.9346(16)
_cell_length_b                   25.153(13)
_cell_length_c                   28.98(2)
_cell_measurement_reflns_used    781
_cell_measurement_temperature    293
_cell_measurement_theta_max      15.2620
_cell_measurement_theta_min      3.9300
_cell_volume                     5055(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.731
_diffrn_measured_fraction_theta_max 0.730
_diffrn_measurement_details
;
 Data were collected at room temperature and pressure of 0.40(2) GPa
 (400000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  \f    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  \f    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  \f    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  \w    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  \w    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  \w    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  \w    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  \w    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  \w    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  \w    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  \w    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  \w    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  \w    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  \w    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  \w    -90.00 -72.00   0.75   35.00    --  -30.00 134.60 -56.90   24
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0105084000
_diffrn_orient_matrix_UB_12      -0.0186997000
_diffrn_orient_matrix_UB_13      -0.0180937000
_diffrn_orient_matrix_UB_21      -0.0598238000
_diffrn_orient_matrix_UB_22      -0.0158472000
_diffrn_orient_matrix_UB_23      0.0143440000
_diffrn_orient_matrix_UB_31      -0.0824748000
_diffrn_orient_matrix_UB_32      0.0139130000
_diffrn_orient_matrix_UB_33      -0.0080538000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2726
_diffrn_reflns_av_unetI/netI     0.1455
_diffrn_reflns_Laue_measured_fraction_full 0.731
_diffrn_reflns_Laue_measured_fraction_max 0.730
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8705
_diffrn_reflns_point_group_measured_fraction_full 0.758
_diffrn_reflns_point_group_measured_fraction_max 0.758
_diffrn_reflns_theta_full        13.583
_diffrn_reflns_theta_max         13.583
_diffrn_reflns_theta_min         4.065
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_T_max  0.435
_exptl_absorpt_correction_T_min  0.257
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model (Absorb Angel (2004) J. Appl. Cryst. 37:486-492)
;
_exptl_crystal_colour            'clear light pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_description       plate
_exptl_crystal_F_000             1680
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 220 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.397
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         1171
_refine_ls_number_restraints     485
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.1125
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2978
_refine_ls_wR_factor_ref         0.3413
_reflns_Friedel_coverage         0.682
_reflns_Friedel_fraction_full    0.802
_reflns_Friedel_fraction_max     0.802
_reflns_number_gt                814
_reflns_number_total             1171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01937f2.cif
_cod_data_source_block           DMOF_0_40_GPa_Gly
_cod_database_code               7708718
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C39H25F6N2O4S2Zn
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.746
_exptl_oxdiff_absorpt_process_details
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.385     0.454
         range of gasket transmission (min-max)           0.665     1.000
         range of P media transmission (min-max)          0.997     0.998

 thickness of diamond anvil 1: 19.500 mm, mu =  0.0202 mm-1
       thickness of platten 1:  0.000 mm, mu =  0.0000 mm-1

 thickness of diamond anvil 2: 19.500 mm, mu =  0.0202 mm-1
       thickness of platten 2:  0.000 mm, mu =  0.0000 mm-1

    Gasket shadowing corrections were made based upon
    Gasket thickness = 280.0 microns, radius = 230.0 microns
    Gasket absorption coeff =        21.00 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.00

    Absorption coeff of pressure medium =   0.01 mm-1
;
_reflns_odcompleteness_completeness 65.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     15.83
_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. Restrained distances
 C8-C11
 1.42 with sigma of 0.01
 C15-C16
 1.43 with sigma of 0.01
 C26-C27
 1.45 with sigma of 0.01
 O2-C27 \\sim C27-O1
 with sigma of 0.02
 C36-O4 \\sim O4-O3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C14) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C14) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(O1)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C37) \\sim Ueq,
Uanis(C2) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C36)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C33)
\\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C30) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C29) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C34) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Zn01) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C15) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C18) \\sim Ueq, Uanis(Zn01) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C24, N2, C23, C22, C21, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19, C16, C17, C18, S2, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14, C13, C12, C11, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8, C7, C6, S1, C9, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2, C1, N1, C5, C4, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, C31, C30, C29, C28, C27, C26, O2, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C39, C38, C36, C35, C34, C33, C37, O4, O3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C17(H17), C7(H7), C32(H32), C31(H31), C29(H29), C28(H28), C2(H2), C1(H1),
 C5(H5), C4(H4), C22(H22), C25(H25), C24(H24), C23(H23), C35(H35), C34(H34),
 C39(H39), C38(H38)
5.b Fitted pentagon refined as free rotating group:
 S2(C18,C17,C16,C19), C15(C14,C13,C12,C11), C9(C8,C7,C6,S1)
5.c Fitted hexagon refined as free rotating group:
 C27(C32,C31,C30,C29,C28), C3(C2,C1,N1,C5,C4), C22(C21,C25,C24,N2,C23),
 C36(C35,C34,C33,C39,C38)
5.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              71875
_shelx_fab_checksum              69536
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 4.226
_oxdiff_exptl_absorpt_empirical_full_min 0.533