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_1551431
_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                   17.29649(13)
_cell_length_b                   17.29649(13)
_cell_length_c                   19.8753(3)
_cell_measurement_reflns_used    6384
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      72.1320
_cell_measurement_theta_min      3.3820
_cell_volume                     5946.07(11)
_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      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.985
_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  87.00   0.50    2.00    --   45.50 -82.00-180.00  236
  2  \w     29.00 136.00   0.50    7.00    --  100.10 -61.00 120.00  214
  3  \w    114.00 145.00   0.50    7.00    --  100.10  82.00 -60.00   62
  4  \w    116.00 180.00   0.50    7.00    --  100.10  82.00  60.00  128
  5  \w    104.00 186.00   0.50    7.00    --  100.10  82.00  90.00  164
;
_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      -0.0700519000
_diffrn_orient_matrix_UB_12      -0.0123693000
_diffrn_orient_matrix_UB_13      -0.0465463000
_diffrn_orient_matrix_UB_21      0.0549372000
_diffrn_orient_matrix_UB_22      -0.0169135000
_diffrn_orient_matrix_UB_23      -0.0591969000
_diffrn_orient_matrix_UB_31      -0.0007289000
_diffrn_orient_matrix_UB_32      -0.0866351000
_diffrn_orient_matrix_UB_33      0.0182720000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7576
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        66.750
_diffrn_reflns_theta_max         72.606
_diffrn_reflns_theta_min         3.387
_diffrn_source                   MM007HF-DW
_diffrn_source_type              'Microfocus Rotating Anode X-ray Source'
_exptl_absorpt_coefficient_mu    17.330
_exptl_absorpt_correction_T_max  0.411
_exptl_absorpt_correction_T_min  0.129
_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    1.723
_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         1.331
_refine_diff_density_min         -2.014
_refine_diff_density_rms         0.224
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.04(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2965
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.229
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0650
_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^)+275.4369P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1584
_refine_ls_wR_factor_ref         0.1589
_reflns_Friedel_coverage         0.824
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                2952
_reflns_number_total             2965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nchem.2718-s8.cif
_cod_data_source_block           ag12bpy_vacuum_100k
_cod_original_cell_volume        5946.06(12)
_cod_database_code               1551431
_chemical_oxdiff_formula         'C80 H104 O8 N8 S8 Ag12'
_chemical_oxdiff_usercomment     st
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.96(5) 0.04(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C3-C1 = C2-C1 = C5-C4 = C6-C4
 1.53 with sigma of 0.02
 F1-C8 \\sim F2-C8
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(F2) \\sim
Ueq, Uanis(F1) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Fixed Sof: Ag3(0.25) H3A(0.5) H3B(0.5) H3C(0.5) H5A(0.5) H5B(0.5) H5C(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C12(H12), C13(H13)
6.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
Comments: The trifluoroacetate and t-butyl mercaptan anions 
were observed to be disordered, however, the related atoms 
were not split but rather had strong restraints applied. 
The geometry and ADPs of the trifluoroacetate were restrained 
using "SADI" and "ISOR", respectively. For the t-butyl mercaptan, 
ADP restraints "ISOR 0.01 0.02" were applied to C4, C5 and C6. 
The C-C distance was restrained by "DFIX 1.53 0.01". The structure 
is slightly twinned. So "TWIN" command was used with a refined BASF
parameter of 0.038.
;
_shelx_res_checksum              83704
_shelx_hkl_checksum              46816