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_7708723
_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_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             2018-12-04
_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                   6.638(6)
_cell_length_b                   25.42(3)
_cell_length_c                   28.23(8)
_cell_measurement_reflns_used    211
_cell_measurement_temperature    571(2)
_cell_measurement_theta_max      10.8760
_cell_measurement_theta_min      3.8970
_cell_volume                     4763(15)
_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      571.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.077
_diffrn_measured_fraction_theta_max 0.674
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f    -35.00  19.40   0.80   28.00   0.00 -30.00   0.00    --    68
  2  \f    140.00 200.00   0.80   28.00   0.00 -30.00   0.00    --    75
  3  \f    160.00 216.80   0.80   28.00   0.00  30.00   0.00    --    71
  4  \f    -20.00  34.40   0.80   28.00   0.00  30.00   0.00    --    68
  5  \w    -24.00  24.00   0.80   28.00    --   30.00  39.46 -12.90   60
  6  \w    -24.00  24.00   0.80   28.00    --   30.00  39.46 167.10   60
  7  \w    -50.00  10.00   0.80   28.00    --  -30.00  39.46 167.10   75
  8  \w    -50.00  10.00   0.80   28.00    --  -30.00  39.46 -12.90   75
  9  \w    -64.00  -8.00   0.80   28.00    --  -30.00  81.40 -28.90   70
 10  \w    -64.00  -8.00   0.80   28.00    --  -30.00  81.40 151.10   70
 11  \w    -19.00   7.40   0.80   28.00    --   30.00  81.40 151.10   33
 12  \w    -19.00   7.40   0.80   28.00    --   30.00  81.40 -28.90   33
 13  \w    -43.00 -21.40   0.80   28.00    --   30.00 134.60 -56.90   27
 14  \w    -43.00 -21.40   0.80   28.00    --   30.00 134.60 123.10   27
 15  \w    -90.00 -36.40   0.80   28.00    --  -30.00 134.60 123.10   67
 16  \w    -90.00 -36.40   0.80   28.00    --  -30.00 134.60 -56.90   67
;
_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      0.0110045000
_diffrn_orient_matrix_UB_12      0.0156919000
_diffrn_orient_matrix_UB_13      -0.0204154000
_diffrn_orient_matrix_UB_21      0.0617696000
_diffrn_orient_matrix_UB_22      0.0178011000
_diffrn_orient_matrix_UB_23      0.0130571000
_diffrn_orient_matrix_UB_31      0.0868712000
_diffrn_orient_matrix_UB_32      -0.0146762000
_diffrn_orient_matrix_UB_33      -0.0062928000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3085
_diffrn_reflns_av_unetI/netI     0.1605
_diffrn_reflns_Laue_measured_fraction_full 0.077
_diffrn_reflns_Laue_measured_fraction_max 0.674
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4271
_diffrn_reflns_point_group_measured_fraction_full 0.072
_diffrn_reflns_point_group_measured_fraction_max 0.710
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         11.443
_diffrn_reflns_theta_min         4.085
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_T_max  0.435
_exptl_absorpt_correction_T_min  0.277
_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            pink
_exptl_crystal_density_diffrn    1.155
_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          0.216
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.153
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 124 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.14(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         622
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.1569
_refine_ls_R_factor_gt           0.1168
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.072
_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          0.2985
_refine_ls_wR_factor_ref         0.3456
_reflns_Friedel_coverage         0.646
_reflns_Friedel_fraction_full    0.066
_reflns_Friedel_fraction_max     0.775
_reflns_number_gt                422
_reflns_number_total             622
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01937f2.cif
_cod_data_source_block           DMOF_1_2_GPa_Gly
_cod_original_cell_volume        4762(16)
_cod_database_code               7708723
_shelx_shelxl_version_number     2017/1