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_4126412
_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         'C12 H11 N9 O2 Zn2'
_chemical_formula_sum            'C12 H11 N9 O2 Zn2'
_chemical_formula_weight         444.08
_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            12
_cell_length_a                   27.0265(8)
_cell_length_b                   27.0265(8)
_cell_length_c                   17.8985(9)
_cell_measurement_reflns_used    13189
_cell_measurement_temperature    250
_cell_measurement_theta_max      24.1360
_cell_measurement_theta_min      2.0820
_cell_volume                     11322.1(7)
_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_temperature      250
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9840
_diffrn_measured_fraction_theta_max 0.9840
_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    -70.00 110.00   0.50    5.00    --   20.00  54.00   0.00  360
  2  \w    -70.00 110.00   0.50    5.00    --   20.00  54.00  90.00  360
  3  \w    -70.00 110.00   0.50    5.00    --   20.00  54.00 180.00  360
  4  \w    -70.00 110.00   0.50    5.00    --   20.00  54.00 270.00  360
;
_diffrn_measurement_device       'Rigaku Saturn 70 AFC8'
_diffrn_measurement_device_type
;
dtrek-CrysAlisPro-abstract goniometer 
imported rigaku-d*trek images
;
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0295731000
_diffrn_orient_matrix_UB_12      0.0160799000
_diffrn_orient_matrix_UB_13      0.0083489000
_diffrn_orient_matrix_UB_21      -0.0065647000
_diffrn_orient_matrix_UB_22      0.0025510000
_diffrn_orient_matrix_UB_23      0.0377099000
_diffrn_orient_matrix_UB_31      0.0000093000
_diffrn_orient_matrix_UB_32      -0.0255443000
_diffrn_orient_matrix_UB_33      0.0089842000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1291
_diffrn_reflns_av_sigmaI/netI    0.1346
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            173404
_diffrn_reflns_theta_full        29.4729
_diffrn_reflns_theta_max         29.5382
_diffrn_reflns_theta_min         1.7401
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.283
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41o (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.781
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             2664.001
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         8.48
_refine_diff_density_min         -7.95
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8295
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2498
_refine_ls_number_restraints     128
_refine_ls_R_factor_all          0.2066
_refine_ls_R_factor_gt           0.1464
_refine_ls_shift/su_max          0.0147975
_refine_ls_shift/su_mean         0.0015604
_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: 
 0.385E+04 0.645E+04 0.409E+04 0.183E+04 482. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3549
_refine_ls_wR_factor_gt          0.3125
_refine_ls_wR_factor_ref         0.3030
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              6
_reflns_limit_k_min              0
_reflns_limit_l_max              44
_reflns_limit_l_min              0
_reflns_number_gt                2933
_reflns_number_total             5676
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.1364
_oxford_refine_ls_scale          1.048(13)
_oxford_reflns_number_all        5652
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ja7b07856_si_002.cif
_cod_data_source_block           ZIF-70_250K
_cod_original_cell_volume        11322.1(8)
_cod_database_code               4126412
_cell_oxdiff_length_a            27.0320(10)
_cell_oxdiff_length_b            27.0328(12)
_cell_oxdiff_length_c            17.8873(9)
_cell_oxdiff_angle_alpha         90.066(4)
_cell_oxdiff_angle_beta          89.940(4)
_cell_oxdiff_angle_gamma         119.981(4)
_cell_oxdiff_volume              11322.1(8)
_cell_oxdiff_measurement_reflns_used 13191
_oxdiff_exptl_absorpt_empirical_full_min 0.894
_oxdiff_exptl_absorpt_empirical_full_max 1.225
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_reflns_odcompleteness_completeness 98.40
_reflns_odcompleteness_theta     29.47
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         Zn(N2C3H3)0.5(N2C3NO2H2)1.5