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_4132603
_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         'C30 H20 O4, 2(C4 H9 N O)'
_chemical_formula_sum            'C38 H38 N2 O6'
_chemical_formula_weight         618.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-09 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.716(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6198(3)
_cell_length_b                   12.0108(3)
_cell_length_c                   12.5761(3)
_cell_measurement_reflns_used    3011
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      73.5940
_cell_measurement_theta_min      5.0850
_cell_volume                     1593.10(7)
_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      180.01(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 0.969
_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    -26.00  30.00   1.00    3.10    --  -37.69  57.00  90.00   56
  2  \w     25.00  71.00   1.00    3.10    --   37.69  38.00 -90.00   46
  3  \w    105.00 143.00   1.00   15.00    --  110.40 111.00 -60.00   38
  4  \w    109.00 134.00   1.00   15.00    --  110.40  61.00-150.00   25
  5  \w    110.00 175.00   1.00   15.00    --  110.40  99.00-159.00   65
  6  \w     72.00 115.00   1.00    3.10    --   37.69 178.00-120.00   43
  7  \w    100.00 158.00   1.00   15.00    --  110.40 111.00  90.00   58
  8  \w    100.00 178.00   1.00   15.00    --  110.40 111.00 150.00   78
  9  \w    107.00 139.00   1.00   15.00    --  110.40 -45.00  90.00   32
 10  \w     72.00 138.00   1.00   15.00    --  110.40 -77.00 150.00   66
 11  \w     56.00 106.00   1.00   15.00    --  110.40 -94.00 120.00   50
 12  \w     36.00  89.00   1.00   15.00    --  110.40 -45.00  90.00   53
 13  \w    -73.00  34.00   1.00    3.10    --  -37.69  77.00 -30.00  107
;
_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      -0.0762622000
_diffrn_orient_matrix_UB_12      0.1015684000
_diffrn_orient_matrix_UB_13      -0.0461458000
_diffrn_orient_matrix_UB_21      -0.1241862000
_diffrn_orient_matrix_UB_22      -0.0662886000
_diffrn_orient_matrix_UB_23      0.0015041000
_diffrn_orient_matrix_UB_31      -0.0107628000
_diffrn_orient_matrix_UB_32      0.0417816000
_diffrn_orient_matrix_UB_33      0.1143014000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5834
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.563
_diffrn_reflns_theta_min         4.192
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.704
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.885
_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    1.290
_exptl_crystal_description       prism
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.114
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.039
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         3122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0538P)^2^+0.2851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1082
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2581
_reflns_number_total             3122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05047_si_002.cif
_cod_data_source_block           batch3_2b
_cod_database_code               4132603
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C38H38N2O6
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.924
_reflns_odcompleteness_completeness 99.90
_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:
 C5(H5)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C8(H8), C9(H9), C10(H10), C14(H14)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              4330
_shelx_hkl_checksum              49318
_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 2.825
_oxdiff_exptl_absorpt_empirical_full_min 0.807