On-Demand Degradation of Metal-Organic Framework Based on Photocleavable Dianthracene-Based Ligand.
Collet, Guillaume; Lathion, Timothée; Besnard, Céline; Piguet, Claude; Petoud, Stéphane; Journal of the American Chemical Society 140 (2018) 10820–10828; doi:10.1021/jacs.8b05047

data_4132601
_publ_section_title
;
 On-Demand Degradation of Metal-Organic Framework Based on Photocleavable
 Dianthracene-Based Ligand.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10820
_journal_page_last               10828
_journal_paper_doi               10.1021/jacs.8b05047
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         '2(C2 H6 O S), C30 H20 O4'
_chemical_formula_sum            'C34 H32 O6 S2'
_chemical_formula_weight         600.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.060(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.4209(3)
_cell_length_b                   7.9301(2)
_cell_length_c                   18.7758(5)
_cell_measurement_reflns_used    3380
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      73.4440
_cell_measurement_theta_min      4.3370
_cell_volume                     1505.13(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4679
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.971
_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    -76.00  20.00   1.00    1.00    --  -37.56 -19.00  30.00   96
  2  \w     56.00  94.00   1.00    1.00    --   37.56-126.00  25.00   38
  3  \w     40.00  68.00   1.00    2.00    --  110.40 -45.00 -90.00   28
  4  \w     83.00 109.00   1.00    2.00    --  110.40 -94.00 -90.00   26
  5  \w     34.00 107.00   1.00    2.00    --  110.40-111.00  60.00   73
  6  \w     93.00 124.00   1.00    2.00    --  110.40 -61.00  60.00   31
  7  \w     88.00 169.00   1.00    2.00    --  110.40  45.00   0.00   81
  8  \w    106.00 134.00   1.00    2.00    --  110.40 111.00-150.00   28
  9  \w     29.00 141.00   1.00    2.00    --  110.40 -30.00-180.00  112
 10  \w     32.00  85.00   1.00    2.00    --  110.40 -61.00  60.00   53
 11  \w   -115.00 -22.00   1.00    1.00    --  -37.56 -38.00   0.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1488213000
_diffrn_orient_matrix_UB_12      0.0141888000
_diffrn_orient_matrix_UB_13      -0.0370620000
_diffrn_orient_matrix_UB_21      0.0302895000
_diffrn_orient_matrix_UB_22      -0.0230298000
_diffrn_orient_matrix_UB_23      -0.0757257000
_diffrn_orient_matrix_UB_31      -0.0145071000
_diffrn_orient_matrix_UB_32      -0.1922280000
_diffrn_orient_matrix_UB_33      0.0063877000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            4930
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.339
_diffrn_reflns_theta_min         4.457
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.972
_exptl_absorpt_correction_T_max  0.625
_exptl_absorpt_correction_T_min  0.428
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       prism
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.634
_exptl_crystal_size_mid          0.513
_exptl_crystal_size_min          0.302
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.0195(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0772P)^2^+1.1093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1311
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2804
_reflns_number_total             2934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05047_si_003.cif
_cod_data_source_block           diant_b
_cod_database_code               4132601
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C17 H16 O3 S1'
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.29
_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, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C21(H21)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C24(H24), C25(H25), C26(H26), C30(H30), C31(H31), C32(H32), C33(H33)
2.c Idealised Me refined as rotating group:
 C3S(H3SA,H3SB,H3SC), C4S(H4SA,H4SB,H4SC)
;
_shelx_res_checksum              75346
_shelx_hkl_checksum              18674
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.455
_oxdiff_exptl_absorpt_empirical_full_min 0.618