A Flexible Fluorescent SCC-MOF for Switchable Molecule Identification and Temperature Display
Dong, Xi-Yan; Huang, Hui-Lin; Wang, Jia-Yin; Li, Hai-Yang; Zang, Shuang-Quan; Chemistry of Materials 30 (2018) 2160–; doi:10.1021/acs.chemmater.8b00611

data_4003124
_publ_section_title
;
 A Flexible Fluorescent SCC-MOF for Switchable Molecule Identification and
 Temperature Display
;
_journal_issue                   6
_journal_name_full               'Chemistry of Materials'
_journal_page_first              2160
_journal_paper_doi               10.1021/acs.chemmater.8b00611
_journal_volume                  30
_journal_year                    2018
_chemical_formula_moiety         'C60 H82 Ag10 F6 N4 O10 P2 S6, 8(C H2 Cl2)'
_chemical_formula_sum            'C68 H98 Ag10 Cl16 F6 N4 O10 P2 S6'
_chemical_formula_weight         3145.70
_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             2017-08-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_cell_angle_alpha                67.234(4)
_cell_angle_beta                 70.613(4)
_cell_angle_gamma                89.920(4)
_cell_formula_units_Z            1
_cell_length_a                   12.1375(6)
_cell_length_b                   14.2801(5)
_cell_length_c                   17.8065(8)
_cell_measurement_reflns_used    13780
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.8740
_cell_measurement_theta_min      3.4340
_cell_volume                     2655.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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     28.00  63.00   0.50    0.50    --    0.00  57.00 -60.00   70
  2  \w    -28.00  79.00   0.50    0.50    --    0.00  57.00-150.00  214
  3  \w      2.00  79.00   0.50    0.50    --    0.00  77.00-120.00  154
  4  \w    -28.00  88.00   0.50    0.50    --    0.00  38.00 150.00  232
  5  \w      8.00 157.00   0.50    0.90    --   97.60 -15.00  90.00  298
  6  \w      9.00 114.00   0.50    0.90    --   97.60 -30.00 120.00  210
  7  \w     12.00  43.00   0.50    0.90    --   97.60 -82.00  90.00   62
  8  \w     46.00  80.00   0.50    0.90    --   97.60 -82.00 -60.00   68
  9  \w     50.00 112.00   0.50    0.90    --   97.60 -82.00 -90.00  124
 10  \w     17.00  88.00   0.50    0.90    --   97.60 -30.00-150.00  142
 11  \w     97.00 125.00   0.50    0.90    --   97.60 -30.00-150.00   56
 12  \w      9.00 127.00   0.50    0.90    --   97.60 -61.00   0.00  236
 13  \w     11.00 135.00   0.50    0.90    --   97.60 -82.00   0.00  248
 14  \w     70.00  99.00   0.50    0.90    --   97.60  15.00 120.00   58
 15  \w     39.00 134.00   0.50    0.90    --   97.60 -82.00 120.00  190
 16  \w     79.00 106.00   0.50    0.90    --   97.60 -82.00  90.00   54
 17  \w    105.00 135.00   0.50    0.90    --   97.60  15.00 120.00   60
 18  \w    158.00 184.00   0.50    0.90    --   97.60  15.00 120.00   52
 19  \w    124.00 152.00   0.50    0.90    --   97.60 -15.00-120.00   56
 20  \w     83.00 108.00   0.50    0.90    --   97.60 -82.00 -60.00   50
 21  \w     87.00 132.00   0.50    0.90    --   97.60 -82.00  60.00   90
 22  \w     21.00 135.00   0.50    0.90    --   97.60 -82.00-150.00  228
 23  \w     55.00  82.00   0.50    0.90    --   97.60 -82.00 150.00   54
 24  \w     92.00 117.00   0.50    0.90    --   97.60 -82.00 150.00   50
 25  \w      8.00  84.00   0.50    0.90    --   97.60 -15.00-120.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0653411000
_diffrn_orient_matrix_UB_12      -0.0034790000
_diffrn_orient_matrix_UB_13      0.0916602000
_diffrn_orient_matrix_UB_21      -0.0598583000
_diffrn_orient_matrix_UB_22      -0.1100176000
_diffrn_orient_matrix_UB_23      0.0303697000
_diffrn_orient_matrix_UB_31      0.1031866000
_diffrn_orient_matrix_UB_32      -0.0432522000
_diffrn_orient_matrix_UB_33      0.0280263000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25680
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        64.999
_diffrn_reflns_theta_max         64.999
_diffrn_reflns_theta_min         2.884
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.044
_exptl_absorpt_correction_T_max  0.246
_exptl_absorpt_correction_T_min  0.067
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (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    1.967
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         4.978
_refine_diff_density_min         -1.666
_refine_diff_density_rms         0.359
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         8976
_refine_ls_number_restraints     290
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.1082
_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^)+(0.2900P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3166
_refine_ls_wR_factor_ref         0.3258
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8069
_reflns_number_total             8976
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm8b00611_si_004.cif
_cod_data_source_block           ag10bpy_ch2cl2_100k
_cod_database_code               4003124
_chemical_oxdiff_formula         'C68 H98 Ag10 Cl16 F6 N4 O10 P2 S6'
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C28B-C23B \\sim C27B-C28B \\sim C26B-C27B \\sim C26B-C25B \\sim C25B-C24B
\\sim C24B-C23B
 with sigma of 0.01
 C28-C23 \\sim C28-C27 \\sim C26-C27 \\sim C25-C26 \\sim C24-C25 \\sim C24-C23
 with sigma of 0.01
 P1-C23 \\sim P1-C23B
 with sigma of 0.01
 N2-C18B \\sim N2-C18 \\sim N2-C22 \\sim N2-C22B
 with sigma of 0.01
 C18B-C19B \\sim C18-C19 \\sim C19B-C20 \\sim C19-C20 \\sim C21-C22 \\sim
C21B-C22B \\sim C21-C20 ~
 C21B-C20
 with sigma of 0.01
 C11B-C9 \\sim C12-C9 \\sim C10B-C9 \\sim C11-C9 \\sim C12B-C9 \\sim C10-C9
 with sigma of 0.01
 Cl8-C34 \\sim Cl7-C34 \\sim Cl7B-C34B \\sim Cl8B-C34B
 with sigma of 0.01
 Cl7-Cl8 \\sim Cl8B-Cl7B
 with sigma of 0.01
3. Restrained planarity
 C23, C24, C25, C26, C27, C28
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Cl7 \\sim Cl8 \\sim Cl7B \\sim Cl8B: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C26B \\sim C27: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(N2) \\sim Ueq, Uanis(C22B) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21B)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19B) \\sim Ueq,
Uanis(C18B) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23B) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28B) \\sim Ueq, Uanis(C24B)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C24) \\sim Ueq,
Uanis(C28) \\sim Ueq, Uanis(C25B) \\sim Ueq, Uanis(C27B) \\sim Ueq, Uanis(C26B)
\\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C10) \\sim Ueq, Uanis(C11B) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C10B)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12B) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: C10(0.6) H10A(0.6) H10B(0.6) H10C(0.6) C10B(0.4) H10D(0.4)
 H10E(0.4) H10F(0.4) C11(0.6) H11A(0.6) H11B(0.6) H11C(0.6) C11B(0.4) H11D(0.4)
 H11E(0.4) H11F(0.4) C12(0.6) H12A(0.6) H12B(0.6) H12C(0.6) C12B(0.4) H12D(0.4)
 H12E(0.4) H12F(0.4) C18(0.5) H18(0.5) C18B(0.5) H18B(0.5) C19(0.5) H19(0.5)
 C19B(0.5) H19B(0.5) C21(0.5) H21(0.5) C21B(0.5) H21B(0.5) C22(0.5) H22(0.5)
 C22B(0.5) H22B(0.5) C23(0.5) C23B(0.5) C24(0.5) H24(0.5) C24B(0.5) H24B(0.5)
 C25(0.5) H25(0.5) C25B(0.5) H25B(0.5) C26(0.5) H26(0.5) C26B(0.5) H26B(0.5)
 C27(0.5) H27(0.5) C27B(0.5) H27B(0.5) C28(0.5) H28(0.5) C28B(0.5) H28B(0.5)
 Cl3B(0.5) Cl4B(0.5) C32B(0.5) H32A(0.5) H32B(0.5) Cl7(0.5) Cl8(0.5) C34(0.5)
 H34A(0.5) H34B(0.5) Cl3(0.5) Cl4(0.5) C32(0.5) H32C(0.5) H32D(0.5) Cl7B(0.5)
 Cl8B(0.5) C34B(0.5) H34C(0.5) H34D(0.5)
6.a Riding coordinates:
 C10(H10A,H10B,H10C), C11B(H11D,H11E,H11F), C12B(H12D,H12E,H12F)
6.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C32B(H32A,H32B), C31(H31A,H31B), C34(H34A,H34B), C32(H32C,
 H32D), C34B(H34C,H34D)
6.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C18B(H18B), C19(H19), C19B(H19B), C21(H21), C21B(H21B), C22(H22),
 C22B(H22B), C13(H13), C14(H14), C16(H16), C17(H17), C24(H24), C24B(H24B),
 C25(H25), C25B(H25B), C26(H26), C26B(H26B), C27(H27), C27B(H27B), C28(H28),
 C28B(H28B)
6.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10B(H10D,H10E,H10F), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C)
6.e Idealised tetrahedral OH refined as rotating group:
 O5(H5)
comments: The single-crystal X-ray diffraction data was collected at 100K. 
In the host framework, the PhPO3H anion, one pyridine ring and one t-butyl 
mercaptan anion were found to be disordered. For the pyridine ring and 
PhPO3H anion, they were disordered over two sites with the fixed occupancy 
of 0.5. The geometry restraints and displacement parameter restrains were 
restrained using the "FLAT" "SADI", "SIMU" and "ISOR"commands. 
For the t-butyl mercaptan anions, two unequal parts were assigned 
with fixed occupancies(0.6:0.4) according to the difference electron 
maps. Restraints such as "SADI 0.01" and "ISOR 0.01" were applied 
for the geometry and ADPs, respectively. Additionally, Four CH2Cl2 
molecules were assigned from a difference Fourier map. Two of them 
could be located easily and refined anisotropically. The other two 
are disordered due to the relatively small size of the molecule 
compared with the cavity and weak interactions with 
host framework. The disordered models obtained by splitting each CH2Cl2 
over two sites with fixed occupancy ratio of 0.5:0.5, and refined 
isotropically.
;
_shelx_res_checksum              66502
_shelx_hkl_checksum              46356
_shelx_shelxl_version_number     2016/6
_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 2.041
_oxdiff_exptl_absorpt_empirical_full_min 0.561