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_4132602
_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(C15 H10 O2), 2(C4 H9 N O)'
_chemical_formula_sum            'C38 H38 N2 O6'
_chemical_formula_weight         618.70
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-04-09 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                66.913(5)
_cell_angle_beta                 74.315(5)
_cell_angle_gamma                74.609(4)
_cell_formula_units_Z            2
_cell_length_a                   9.2901(5)
_cell_length_b                   13.6758(7)
_cell_length_c                   14.4243(8)
_cell_measurement_reflns_used    5207
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      73.5480
_cell_measurement_theta_min      3.3690
_cell_volume                     1596.55(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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 0.998
_diffrn_measured_fraction_theta_max 0.966
_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     46.00 148.00   1.00    2.00    --  110.40 -30.00 150.00  102
  2  \w     54.00 103.00   1.00    2.00    --  110.40 -94.00 -30.00   49
  3  \w     83.00 113.00   1.00    2.00    --  110.40-111.00 -90.00   30
  4  \w     37.00 143.00   1.00    2.00    --  110.40 -30.00  30.00  106
  5  \w     80.00 171.00   1.00    2.00    --  110.40  45.00-150.00   91
  6  \w     93.00 124.00   1.00    2.00    --  110.40 178.00-150.00   31
  7  \w    121.00 150.00   1.00    2.00    --  110.40 178.00-120.00   29
  8  \w     60.00  87.00   1.00    2.00    --  110.40 178.00-120.00   27
  9  \w    128.00 169.00   1.00    2.00    --  110.40 111.00  60.00   41
 10  \w    132.00 158.00   1.00    2.00    --  110.40 111.00 120.00   26
 11  \w    101.00 169.00   1.00    2.00    --  110.40 111.00 150.00   68
 12  \w     29.00  80.00   1.00    2.00    --  110.40 -30.00 -90.00   51
 13  \w      1.00  61.00   1.00    1.00    --   39.06 -99.00   0.00   60
 14  \w     38.00  92.00   1.00    1.00    --   39.06-125.00 120.00   54
 15  \w     36.00 111.00   1.00    2.00    --  110.40-111.00  90.00   75
 16  \w     30.00 131.00   1.00    2.00    --  110.40 -77.00 150.00  101
 17  \w   -101.00  -8.00   1.00    1.00    --  -39.06 -57.00 120.00   93
 18  \w   -112.00 -86.00   1.00    1.00    --  -39.06 -99.00 150.00   26
 19  \w   -118.00 -75.00   1.00    1.00    --  -39.06-125.00 -60.00   43
 20  \w   -121.00 -12.00   1.00    1.00    --  -39.06 -77.00-120.00  109
 21  \w   -117.00 -82.00   1.00    1.00    --  -39.06 -99.00-150.00   35
;
_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      0.0861106000
_diffrn_orient_matrix_UB_12      0.0274467000
_diffrn_orient_matrix_UB_13      0.0615362000
_diffrn_orient_matrix_UB_21      -0.1354949000
_diffrn_orient_matrix_UB_22      0.0890086000
_diffrn_orient_matrix_UB_23      0.0163692000
_diffrn_orient_matrix_UB_31      -0.0699053000
_diffrn_orient_matrix_UB_32      -0.0825927000
_diffrn_orient_matrix_UB_33      0.0995784000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10783
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.784
_diffrn_reflns_theta_min         3.391
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.802
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.287
_exptl_crystal_description       plate
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         6235
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+0.3704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1132
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4970
_reflns_number_total             6235
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05047_si_001.cif
_cod_data_source_block           ligand_dma
_cod_database_code               4132602
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C38 H38 N2 O6'
_reflns_odcompleteness_completeness 99.86
_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. Restrained distances
 O1-H1
 0.85 with sigma of 0.02
 O18-H18
 0.85 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C11(H11), C28(H28)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C9(H9), C33(H33), C13(H13), C8(H8), C7(H7), C26(H26), C30(H30),
 C16(H16), C32(H32), C23(H23), C31(H31), C14(H14), C25(H25), C15(H15), C24(H24)
3.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C43(H43A,H43B,
 H43C), C46(H46A,H46B,H46C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              67479
_shelx_hkl_checksum              96545
_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 1.187
_oxdiff_exptl_absorpt_empirical_full_min 0.898