Bistable Dithienylethene-Based Metal-Organic Framework Illustrating Optically Induced Changes in Chemical Separations.
Furlong, Brandon J.; Katz, Michael J.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b07856

data_4126414
_publ_section_title
;
 Bistable Dithienylethene-Based Metal-Organic Framework Illustrating
 Optically Induced Changes in Chemical Separations.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b07856
_journal_year                    2017
_chemical_formula_moiety         'C9.69 H8.32 N7.43 O2.86 S0.09 Zn1.50'
_chemical_formula_sum            'C9.69 H8.32 N7.43 O2.86 S0.09 Zn1.5'
_chemical_formula_weight         375.69
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            16
_cell_length_a                   27.2188(5)
_cell_length_b                   27.2188(5)
_cell_length_c                   17.0357(8)
_cell_measurement_reflns_used    13383
_cell_measurement_temperature    250.00(10)
_cell_measurement_theta_max      74.9520
_cell_measurement_theta_min      3.7120
_cell_volume                     10930.2(6)
_computing_cell_refinement       'CrystAlis Pro'
_computing_data_collection       'Rigaku Crystal Clear Expert 2.1 SM'
_computing_data_reduction        'CrystAlis Pro'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      250.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9989
_diffrn_measured_fraction_theta_max 0.9906
_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    -60.00  26.00   0.50   17.50    --  -47.45  37.00   0.00  172
  2  \w    -99.00 -13.00   0.50   63.00    --  -86.25  37.00 -60.00  172
  3  \w   -120.00 -87.00   0.50   17.50    --  -47.45 -77.00   0.00   66
  4  \w   -120.00 -70.00   0.50   17.50    --  -47.45-125.00 -60.00  100
  5  \w   -120.00 -70.00   0.50   17.50    --  -47.45-125.00 -30.00  100
  6  \w     36.00 110.00   0.50   63.00    --  107.75 -99.00 150.00  148
  7  \w     95.00 178.00   0.50   63.00    --  107.75  19.00  90.00  166
  8  \w     92.00 178.00   0.50   63.00    --  107.75 125.00-120.00  172
  9  \w     36.00 110.00   0.50   63.00    --  107.75 -99.00-180.00  148
 10  \w     35.00 121.00   0.50   63.00    --  107.75-125.00 -30.00  172
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0510601000
_diffrn_orient_matrix_UB_12      -0.0487766000
_diffrn_orient_matrix_UB_13      0.0424589000
_diffrn_orient_matrix_UB_21      -0.0122294000
_diffrn_orient_matrix_UB_22      -0.0381285000
_diffrn_orient_matrix_UB_23      -0.0726612000
_diffrn_orient_matrix_UB_31      0.0389101000
_diffrn_orient_matrix_UB_32      -0.0210910000
_diffrn_orient_matrix_UB_33      0.0328915000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            57181
_diffrn_reflns_theta_full        66.4915
_diffrn_reflns_theta_max         77.7792
_diffrn_reflns_theta_min         3.7509
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.893
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.913
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             3005.685
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.49
_refine_diff_density_min         -0.59
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3394
_refine_ls_number_restraints     347
_refine_ls_R_factor_all          0.1379
_refine_ls_R_factor_gt           0.1143
_refine_ls_shift/su_max          0.6778872
_refine_ls_shift/su_mean         0.0381631
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 12.2 19.7 12.0 5.21 1.41 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1974
_refine_ls_wR_factor_gt          0.1393
_refine_ls_wR_factor_ref         0.1581
_reflns_limit_h_max              0
_reflns_limit_h_min              -17
_reflns_limit_k_max              34
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                2518
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.1274
_oxford_refine_ls_scale          0.387(2)
_oxford_reflns_number_all        4211
_oxford_reflns_threshold_expression_ref I>0.5\s(I)
_cod_data_source_file            ja7b07856_si_002.cif
_cod_data_source_block           PSZ-1_anisotropic
_cod_original_formula_sum        'C9.69 H8.32 N7.43 O2.86 S0.09 Zn1.50'
_cod_database_code               4126414
_cell_oxdiff_length_a            27.2168(6)
_cell_oxdiff_length_b            27.1942(7)
_cell_oxdiff_length_c            17.0499(4)
_cell_oxdiff_angle_alpha         90.062(2)
_cell_oxdiff_angle_beta          89.973(2)
_cell_oxdiff_angle_gamma         119.985(2)
_cell_oxdiff_volume              10930.2(4)
_cell_oxdiff_measurement_reflns_used 13383
_oxdiff_exptl_absorpt_empirical_full_min 0.748
_oxdiff_exptl_absorpt_empirical_full_max 1.700
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_ac3_digest_frames
;
010a05eeebc61c3b61b2e16166c56a50c701416da94
;
_diffrn_oxdiff_ac3_digest_hkl
;
0133d96d2333189eb5eddd101e5ae39350442e
;
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_theta     66.49
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         ZnN9C24H24O2S2