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_4002898
_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 H Cl3)'
_chemical_formula_sum            'C68 H90 Ag10 Cl24 F6 N4 O10 P2 S6'
_chemical_formula_weight         3421.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-08-12
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_cell_angle_alpha                68.060(2)
_cell_angle_beta                 74.7730(10)
_cell_angle_gamma                89.5690(10)
_cell_formula_units_Z            1
_cell_length_a                   12.0828(2)
_cell_length_b                   14.3610(2)
_cell_length_c                   18.2826(3)
_cell_measurement_reflns_used    17767
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      72.6130
_cell_measurement_theta_min      3.3260
_cell_volume                     2824.76(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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    -35.00  58.00   0.25    0.25    --   45.20 -57.00  30.00  372
  2  \w    -23.00  74.00   0.25    0.25    --   45.20 -57.00 120.00  388
  3  \w      7.00  74.00   0.25    0.25    --   45.20 -57.00-120.00  268
  4  \w    -39.00 -14.00   0.25    0.25    --   45.20 -57.00-120.00  100
  5  \w    -44.00 132.00   0.25    0.25    --   45.20   0.00   0.00  704
  6  \w     52.00 136.00   0.25    0.35    --  100.80 -45.00-120.00  336
  7  \w     47.00 111.00   0.25    0.35    --  100.80 -82.00-180.00  256
  8  \w     26.00 121.00   0.25    0.35    --  100.80 -82.00-120.00  380
  9  \w     16.00  42.00   0.25    0.35    --  100.80 -82.00-180.00  104
 10  \w     16.00 130.00   0.25    0.35    --  100.80 -61.00  60.00  456
 11  \w     11.00 111.00   0.25    0.35    --  100.80 -61.00-120.00  400
 12  \w     23.00 188.00   0.25    0.35    --  100.80  15.00 -60.00  660
 13  \w     11.00  46.00   0.25    0.35    --  100.80 -82.00   0.00  140
 14  \w     55.00 105.00   0.25    0.35    --  100.80 -82.00   0.00  200
 15  \w     27.00 134.00   0.25    0.35    --  100.80 -82.00  60.00  428
 16  \w    131.00 189.00   0.25    0.35    --  100.80 -15.00  30.00  232
 17  \w     92.00 123.00   0.25    0.35    --  100.80  82.00 150.00  124
 18  \w    146.00 177.00   0.25    0.35    --  100.80  82.00 150.00  124
 19  \w     31.00 112.00   0.25    0.35    --  100.80 -15.00  30.00  324
;
_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      -0.0438927000
_diffrn_orient_matrix_UB_12      0.0815981000
_diffrn_orient_matrix_UB_13      0.0652104000
_diffrn_orient_matrix_UB_21      -0.1035494000
_diffrn_orient_matrix_UB_22      -0.0757392000
_diffrn_orient_matrix_UB_23      -0.0166433000
_diffrn_orient_matrix_UB_31      0.0711224000
_diffrn_orient_matrix_UB_32      -0.0341925000
_diffrn_orient_matrix_UB_33      0.0667772000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24233
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        64.993
_diffrn_reflns_theta_max         64.993
_diffrn_reflns_theta_min         2.714
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.612
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
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    2.011
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.13
_refine_diff_density_max         3.062
_refine_diff_density_min         -2.257
_refine_diff_density_rms         0.273
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         9524
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0789
_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^)+(0.1180P)^2^+53.3395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2118
_refine_ls_wR_factor_ref         0.2141
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8850
_reflns_number_total             9524
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm8b00611_si_005.cif
_cod_data_source_block           ag10bpy_chcl3_100k
_cod_depositor_comments
'Adding full bibliography for 4002893--4002902.cif.'
_cod_database_code               4002898
_chemical_oxdiff_formula         'C H O N S Ag'
_reflns_odcompleteness_completeness 98.98
_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
 Cl5-C33 \\sim Cl5B-C33 \\sim Cl6-C33 \\sim Cl6B-C33 \\sim Cl4-C33
 with sigma of 0.01
 Cl1-C34 \\sim Cl3-C34 \\sim Cl2-C34
 with sigma of 0.01
 Cl1-C34 \\sim Cl3-C34 \\sim Cl2-C34 \\sim Cl1B-C34B \\sim Cl2B-C34B \\sim
Cl3B-C34B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl2B \\sim Cl1B \\sim Cl3B \\sim Cl3 \\sim Cl2 \\sim Cl1: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C34B \\sim C34: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Others
 Fixed Sof: Cl1(0.75) Cl1B(0.25) Cl2(0.75) Cl2B(0.25) Cl3(0.75) Cl3B(0.25)
 C34(0.75) H34(0.75) C34B(0.25) H34B(0.25) Cl5(0.5) Cl5B(0.5) Cl6(0.5)
 Cl6B(0.5) H33A(0.5) H33(0.5)
5.a Ternary CH refined with riding coordinates:
 C34(H34), C34B(H34B), C33(H33A), C33(H33), C32(H32), C31(H31)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21),
 C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28)
5.c 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), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C)
5.d Idealised tetrahedral OH refined as rotating group:
 O5(H5)
comments: Four CHCl3 molecules were assigned from a difference Fourier map. 
Two of them could be located easily due to the strong hydrogen bond and 
lone pair electrons interaction with the host framework, and refined 
anisotropically. The other two are highly disordered in the cavity. 
The disordered models obtained by splitting each CHCl3 over two sites 
with fixed occupancy ratio of 0.75:0.25 and 0.5:0.5, respectively. 
The disordered CHCl3 molecules were kept isotropic, and restrained 
using "SADI" and "SIMU" commands.
;
_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 3.070
_oxdiff_exptl_absorpt_empirical_full_min 0.507