Photochromism, photoluminescence modulation and selective recognition of small molecules of two highly stable dynamic metal‒organic frameworks
Gong, Yun-Nan; Wei, Xue-Wen; Deng, Ji-Hua; Zhong, Di-Chang; Pan, Chun-Yang; Dalton Trans.  (2017) –; doi:10.1039/C7DT03783J

data_7044493
_publ_section_title
;
 Photochromism, photoluminescence modulation and selective recognition of
 small molecules of two highly stable dynamic metal--organic frameworks
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03783J
_journal_year                    2017
_chemical_formula_moiety
'[C29.75 H20.5 O8 Tb, C7 H8 O],(C7H8O),2(C4H9NO),2(H2O)'
_chemical_formula_sum            'C51.75 H58.5 N2 O14 Tb'
_chemical_formula_weight         1091.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-09-29
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-09-29 deposited with the CCDC.
2017-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.459(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.3408(9)
_cell_length_b                   14.8489(5)
_cell_length_c                   27.2678(14)
_cell_measurement_reflns_used    7538
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      66.5780
_cell_measurement_theta_min      3.4840
_cell_volume                     9783.8(8)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            19818
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        66.819
_diffrn_reflns_theta_max         66.819
_diffrn_reflns_theta_min         3.493
_exptl_absorpt_coefficient_mu    7.446
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.448
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.160
_refine_ls_extinction_coef       0.000053(16)
_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   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         8516
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0639
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1401P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1872
_refine_ls_wR_factor_ref         0.1955
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6806
_reflns_number_total             8516
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03783j2.cif
_cod_data_source_block           1e
_cod_original_formula_sum        'C51.75 H58.50 O14 N2 Tb'
_cod_database_code               7044493
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.401
_shelx_estimated_absorpt_t_min   0.199
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 C26-C27
 1.4 with sigma of 0.02
 C26-C25
 1.4 with sigma of 0.02
 C23-C24
 1.4 with sigma of 0.02
 C24-C25
 1.4 with sigma of 0.02
 C28-C27
 1.4 with sigma of 0.02
 C28-C23
 1.4 with sigma of 0.02
 C8AA-C4AA
 1.53 with sigma of 0.01
 C22-C23
 1.53 with sigma of 0.01
 O7-H7A
 0.85 with sigma of 0.01
 O1AA-H1AA
 0.85 with sigma of 0.01
 O0AA-C4AA
 1.43 with sigma of 0.01
 C22-H7A
 1.851243 with sigma of 0.02
 Tb1-H7A
 2.928422 with sigma of 0.02
 C1AA-H1AA
 2.128357 with sigma of 0.02
 Tb1-H1AA
 3.097777 with sigma of 0.02
 C5AA-C4AA \\sim C4AA-C6AA
 with sigma of 0.01
 C24-C22 \\sim C22-C28
 with sigma of 0.01
3. Others
 Fixed Sof: O1AA(0.25) H1AA(0.25) H22A(0.75) H22B(0.75) H22C(0.25) H22D(0.25)
 C24(0.75) H24(0.75) C23(0.75) C28(0.75) H28(0.75) C27(0.75) H27(0.75)
 C26(0.75) H26(0.75) C1AA(0.25) H1AB(0.25) H1AC(0.25) C0AA(0.25) H0AA(0.25)
 C7AA(0.25) H7AA(0.25) C2AA(0.25) C2BA(0.25) H2BA(0.25) C42(0.25) H42(0.25)
 C3AA(0.25) H3AA(0.25) O1AB(0.75) H1AD(0.75) H1AE(0.75) C7BA(0.25) H7BA(0.25)
 H25(0.75) H25A(0.25) C6BA(0.25) H6BA(0.25) C5BA(0.25) H5BA(0.25) C4BA(0.25)
 H4BA(0.25) C3BA(0.25)
4.a Riding coordinates:
 O1W(H1WA,H1WB), O0AA(H0AB)
4.b Rotating group:
 O1AB(H1AD,H1AE)
4.c Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C22(H22C,H22D), C1AA(H1AB,H1AC), C4AA(H4AA,H4AB)
4.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C13(H13), C17(H17), C10(H10), C14(H14), C7(H7), C20(H20), C6(H6),
 C21(H21), C24(H24), C28(H28), C27(H27), C26(H26), C6AA(H6AA), C9AA(H9AA),
 C0BA(H0BA), C1BA(H1BA), C5AA(H5AA), C0AA(H0AA), C7AA(H7AA), C2BA(H2BA),
 C42(H42), C3AA(H3AA), C7BA(H7BA), C25(H25), C25(H25A), C6BA(H6BA), C5BA(H5BA),
 C4BA(H4BA)
4.e Fitted hexagon refined as free rotating group:
 C8AA(C6AA,C9AA,C0BA,C1BA,C5AA), C0AA(C7AA,C2AA,C2BA,C42,C3AA), C7BA(C25,C6BA,
 C5BA,C4BA,C3BA)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              24429
_shelx_fab_checksum              9704
_olex2_submission_special_instructions 'No special instructions were received'