Hypersensitive dual-function luminescence switching of a silver-chalcogenolate cluster-based metal-organic framework
Ren-Wu Huang; Yong-Sheng Wei; Xi-Yan Dong; Xiao-Hui Wu; Chen-Xia Du; Shuang-Quan Zang; Thomas C. W. Mak; Nature Chemistry 9 (2017) 689–697; doi:10.1038/nchem.2718

data_1551432
_publ_section_title
;
 Hypersensitive dual-function luminescence switching of a
 silver-chalcogenolate cluster-based metal-organic framework
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              689
_journal_page_last               697
_journal_paper_doi               10.1038/nchem.2718
_journal_volume                  9
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C80 H104 Ag12 F12 N8 O8 S8'
_chemical_formula_sum            'C80 H104 Ag12 F12 N8 O8 S8'
_chemical_formula_weight         3084.63
_space_group_crystal_system      tetragonal
_space_group_IT_number           121
_space_group_name_Hall           'I -4 2'
_space_group_name_H-M_alt        'I -4 2 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.33048(14)
_cell_length_b                   17.33048(14)
_cell_length_c                   20.2510(4)
_cell_measurement_reflns_used    4473
_cell_measurement_temperature    289.96(15)
_cell_measurement_theta_max      71.8050
_cell_measurement_theta_min      3.6110
_cell_volume                     6082.30(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7b (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      oxygen
_diffrn_ambient_temperature      289.96(15)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.982
_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    -31.00  83.00   0.50    5.00    --   45.70 -57.00  90.00  228
  2  \w     59.00 104.00   0.50   11.00    --  100.10  45.00 120.00   90
  3  \w     76.00 178.00   0.50   11.00    --  100.10  61.00  30.00  204
  4  \w    148.00 187.00   0.50   11.00    --  100.10  45.00 120.00   78
  5  \w    111.00 180.00   0.50   11.00    --  100.10  61.00 -90.00  138
  6  \w     69.00  97.00   0.50   11.00    --  100.10  61.00 -90.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0052376000
_diffrn_orient_matrix_UB_12      -0.0024875000
_diffrn_orient_matrix_UB_13      -0.0758309000
_diffrn_orient_matrix_UB_21      0.0027981000
_diffrn_orient_matrix_UB_22      -0.0887978000
_diffrn_orient_matrix_UB_23      0.0023285000
_diffrn_orient_matrix_UB_31      -0.0888052000
_diffrn_orient_matrix_UB_32      -0.0029346000
_diffrn_orient_matrix_UB_33      -0.0043190000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7808
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        66.750
_diffrn_reflns_theta_max         72.743
_diffrn_reflns_theta_min         3.357
_diffrn_source                   MM007HF-DW
_diffrn_source_type              'Microfocus Rotating Anode X-ray Source'
_exptl_absorpt_coefficient_mu    16.941
_exptl_absorpt_correction_T_max  0.444
_exptl_absorpt_correction_T_min  0.120
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7b (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    1.684
_exptl_crystal_description       block
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Flack x determined using 1070 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.016(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2910
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0552P)^2^+0.1002P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0861
_reflns_Friedel_coverage         0.696
_reflns_Friedel_fraction_full    0.892
_reflns_Friedel_fraction_max     0.834
_reflns_number_gt                2729
_reflns_number_total             2910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nchem.2718-s9.cif
_cod_data_source_block           ag12bpy_o2_290k
_cod_original_cell_volume        6082.30(15)
_cod_database_code               1551432
_chemical_oxdiff_formula         C80H104O8N8S8Ag12F12
_chemical_oxdiff_usercomment     st
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2. Restrained distances
 F2-C9 \\sim F1B-C9 \\sim F2B-C9 \\sim F1-C9
 with sigma of 0.01
 C4-C5 \\sim C6-C4 \\sim C7-C4
 with sigma of 0.01
 C3-C1 \\sim C2-C1
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C8 \\sim O1: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C9) \\sim Ueq, Uanis(F1B) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2B)
\\sim Ueq, Uanis(F2) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
4. Others
 Fixed Sof: Ag3(0.25) H3A(0.5) H3B(0.5) H3C(0.5) C7(0.5) H7A(0.5) H7B(0.5)
 H7C(0.5) H6A(0.5) H6B(0.5) H6C(0.5) F1(0.225) F2(0.45) F1B(0.275) F2B(0.55)
 C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C13(H13), C14(H14)
5.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C5(H5A,
 H5B,H5C)
Comments:The trifluoroacetate and t-butyl mercaptan anions were disordered.
For the trifluoroacetate anion, the F1 and F2 were split over two parts
with fixed occupancies (0.45:0.55). A similar C-F distance refinement
was applied for all C-F bonds with the "SADI" command, and the thermal
vibration parameters were restrained with "ISOR" and "SIMU". 
For the t-butyl mercaptan, the symmetry for C5 and C7 was suppressed
for chemical reasonability, and the C-C distances were also
restrained using "SADI". In addition, the guest oxygen molecules
were unable to be modelled due to the serious disorder and weak 
adsorption ability of the crystal at 290 K.
;
_shelx_res_checksum              92597
_shelx_hkl_checksum              43649