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_4132600
_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         'C70.78 H59.56 N2 O15 Yb2'
_chemical_formula_sum            'C70.77 H59.54 N2 O15 Yb2'
_chemical_formula_weight         1524.06
_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     direct
_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                84.612(3)
_cell_angle_beta                 80.119(3)
_cell_angle_gamma                64.846(3)
_cell_formula_units_Z            2
_cell_length_a                   16.6368(5)
_cell_length_b                   18.0871(6)
_cell_length_c                   19.3244(7)
_cell_measurement_reflns_used    11849
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      73.3730
_cell_measurement_theta_min      3.4890
_cell_volume                     5184.0(3)
_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    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_temperature      180.15
_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    100.00 158.00   1.00    5.00    --  110.40 111.00 -30.00   58
  2  \w    114.00 140.00   1.00    5.00    --  110.40 111.00  30.00   26
  3  \w    112.00 177.00   1.00    5.00    --  110.40 120.00  -8.00   65
  4  \w     94.00 129.00   1.00    1.50    --   37.69 178.00   0.00   35
  5  \w     63.00  89.00   1.00    1.50    --   37.69 178.00  30.00   26
  6  \w    146.00 172.00   1.00    5.00    --  110.40  61.00-180.00   26
  7  \w     96.00 133.00   1.00    5.00    --  110.40 -77.00-120.00   37
  8  \w     57.00 112.00   1.00    5.00    --  110.40-111.00 -60.00   55
  9  \w     50.00 115.00   1.00    5.00    --  110.40-111.00  60.00   65
 10  \w     79.00 105.00   1.00    5.00    --  110.40 -94.00 150.00   26
 11  \w     39.00 147.00   1.00    5.00    --  110.40 -30.00  30.00  108
 12  \w     29.00  54.00   1.00    5.00    --  110.40-111.00 -60.00   25
 13  \w     32.00 141.00   1.00    5.00    --  110.40 -45.00-120.00  109
 14  \w     27.00 144.00   1.00    5.00    --  110.40 -77.00  60.00  117
 15  \w     19.00 177.00   1.00    5.00    --  110.40   0.00 150.00  158
 16  \w    -28.00  65.00   1.00    1.50    --   37.69 -57.00  60.00   93
 17  \w    -67.00  37.00   1.00    1.50    --  -37.69  38.00-120.00  104
 18  \w    -68.00  35.00   1.00    1.50    --  -37.69  38.00 -30.00  103
 19  \w   -105.00 -34.00   1.00    1.50    --  -37.69 178.00 -90.00   71
 20  \w   -129.00 -97.00   1.00    1.50    --  -37.69 178.00   0.00   32
;
_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      -0.0380376000
_diffrn_orient_matrix_UB_12      0.0716320000
_diffrn_orient_matrix_UB_13      0.0508491000
_diffrn_orient_matrix_UB_21      0.0030882000
_diffrn_orient_matrix_UB_22      0.0589872000
_diffrn_orient_matrix_UB_23      -0.0622728000
_diffrn_orient_matrix_UB_31      -0.0961120000
_diffrn_orient_matrix_UB_32      0.0157711000
_diffrn_orient_matrix_UB_33      -0.0093990000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36773
_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         73.691
_diffrn_reflns_theta_min         2.966
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.6
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.740
_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    0.976
_exptl_crystal_description       plate
_exptl_crystal_F_000             1516
_exptl_crystal_size_max          0.126
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.036
_refine_diff_density_max         3.213
_refine_diff_density_min         -1.291
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     897
_refine_ls_number_reflns         20325
_refine_ls_number_restraints     170
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0590
_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^)+(0.1070P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1744
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14845
_reflns_number_total             20325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05047_si_004.cif
_cod_data_source_block           mofants1b
_cod_database_code               4132600
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Yb2 C80 H58 N4 O17'
_cell_oxdiff_angle_alpha         84.612(3)
_cell_oxdiff_angle_beta          80.119(3)
_cell_oxdiff_angle_gamma         64.846(3)
_cell_oxdiff_length_a            16.6368(5)
_cell_oxdiff_length_b            18.0871(6)
_cell_oxdiff_length_c            19.3244(7)
_cell_oxdiff_measurement_reflns_used 11849
_cell_oxdiff_volume              5184.0(3)
_reflns_odcompleteness_completeness 99.92
_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,H) groups
2. Restrained distances
 C53-C52
 1.5 with sigma of 0.02
 Yb2-O14B \\sim Yb2-O14A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C10B) = Uanis(C7A)
Uanis(C10A) = Uanis(C8B)
Uanis(N7B) = Uanis(N8A)
Uanis(O7A) = Uanis(O7B)
4. Rigid body (RIGU) restrains
 O14B, N3B, C4B, C1B, C5B, C2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O14A, N3A, C4A, C1A, C5A, C2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O7B, C6B, C10B, N7B, C9B, C8B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O7A, C6A, C7A, N8A, C9A, C10A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C51, C50, O9, O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O15, C52, O8, C53
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O7A)=Sof(C6A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(N8A)=Sof(C9A)=
 Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(O7B)=Sof(C6B)=Sof(C10B)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(N7B)=Sof(C9B)=
 Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(H8BC)=FVAR(1)
 Sof(O14A)=Sof(N3A)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(C1A)=Sof(C5A)=
 Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C2A)=Sof(H2AB)=Sof(H2AC)=Sof(H2AD)=Sof(H50)=
 1-FVAR(2)
 Sof(O14B)=Sof(N3B)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(H4BC)=Sof(C1B)=Sof(C5B)=
 Sof(H5BA)=Sof(H5BB)=Sof(H5BC)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(H2BC)=Sof(C51)=
 Sof(H51A)=Sof(H51B)=Sof(H51C)=FVAR(2)
 Sof(H52)=1-FVAR(3)
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=FVAR(3)
6.a Free rotating group:
 O7B(C6B,C10B,N7B,C9B,C8B), O7A(C6A,C7A,N8A,C9A,C10A)
6.b Rotating group:
 O13(H13A,H13B)
6.c Ternary CH refined with riding coordinates:
 C24(H24), C39(H39), C54(H54), C9(H9)
6.d Me refined with riding coordinates:
 C2B(H2BA,H2BB,H2BC)
6.e Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C44(H44), C41(H41), C35(H35), C36(H36), C14(H14), C29(H29),
 C34(H34), C5(H5), C42(H42), C37(H37), C59(H59), C6(H6), C58(H58), C52(H52),
 C28(H28), C13(H13), C2AA(H2AA), C12(H12), C43(H43), C0AA(H0AA), C22(H22),
 C11(H11), C49(H49), C57(H57), C1AA(H1AA), C56(H56), C26(H26), C19(H19),
 C27(H27), C20(H20), C21(H21), C50(H50)
6.f Idealised Me refined as rotating group:
 C10B(H10A,H10B,H10C), C9B(H9BA,H9BB,H9BC), C8B(H8BA,H8BB,H8BC), C7A(H7AA,H7AB,
 H7AC), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F), C4A(H4AA,H4AB,H4AC),
 C5A(H5AA,H5AB,H5AC), C2A(H2AB,H2AC,H2AD), C4B(H4BA,H4BB,H4BC), C5B(H5BA,H5BB,
 H5BC), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              52521
_shelx_hkl_checksum              73593
_shelx_fab_checksum              48849
_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 1.615
_oxdiff_exptl_absorpt_empirical_full_min 0.615