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_1551430
_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                   17.34149(13)
_cell_length_b                   17.34149(13)
_cell_length_c                   20.1671(4)
_cell_measurement_reflns_used    4427
_cell_measurement_temperature    290.00(10)
_cell_measurement_theta_max      71.7250
_cell_measurement_theta_min      3.6020
_cell_volume                     6064.80(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      vacuum
_diffrn_ambient_temperature      290.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.984
_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      1.00  52.00   0.50    3.00    --   45.50  37.00 -60.00  102
  2  \w     85.00 131.00   0.50    3.00    --   45.50  37.00 -60.00   92
  3  \w     88.00 133.00   0.50    3.00    --   45.50  82.00 -90.00   90
  4  \w     88.00 157.00   0.50    9.00    --  100.10  82.00 -60.00  138
  5  \w    114.00 187.00   0.50    9.00    --  100.10  82.00  60.00  146
  6  \w     11.00 134.00   0.50    9.00    --  100.10 -61.00 120.00  246
;
_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      0.0118940000
_diffrn_orient_matrix_UB_12      0.0706183000
_diffrn_orient_matrix_UB_13      0.0451010000
_diffrn_orient_matrix_UB_21      0.0171696000
_diffrn_orient_matrix_UB_22      -0.0538312000
_diffrn_orient_matrix_UB_23      0.0589306000
_diffrn_orient_matrix_UB_31      0.0864249000
_diffrn_orient_matrix_UB_32      0.0009441000
_diffrn_orient_matrix_UB_33      -0.0179779000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7799
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        66.750
_diffrn_reflns_theta_max         72.695
_diffrn_reflns_theta_min         3.361
_diffrn_source                   MM007HF-DW
_diffrn_source_type              'Microfocus Rotating Anode X-ray Source'
_exptl_absorpt_coefficient_mu    16.990
_exptl_absorpt_correction_T_max  0.420
_exptl_absorpt_correction_T_min  0.145
_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    1.689
_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         0.669
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 1105 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.021(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2994
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0492P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0831
_reflns_Friedel_coverage         0.748
_reflns_Friedel_fraction_full    0.943
_reflns_Friedel_fraction_max     0.898
_reflns_number_gt                2736
_reflns_number_total             2994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nchem.2718-s7.cif
_cod_data_source_block           ag12bpy_vacuum_290k
_cod_original_cell_volume        6064.78(14)
_cod_database_code               1551430
_chemical_oxdiff_formula         'C80 H104 O8 N8 S8 Ag12'
_chemical_oxdiff_usercomment     st
_reflns_odcompleteness_completeness 99.75
_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
 C4-C5 \\sim C6-C4 \\sim C7-C4
 with sigma of 0.01
 F2-C9 \\sim F1B-C9 \\sim F2B-C9 \\sim F1-C9
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O1 \\sim C8: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F1B) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2B) \\sim Ueq, Uanis(F2)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
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 anion was highly disordered due 
to symmetry and rotation.The F1 and F2 were split over two parts with
fixed occupancies (0.45:0.55). Restraints such as 
"ISOR", "SIMU" and "SADI" were applied for the ADPs and geometry,
respectively. In addition, one t-butyl mercaptan was also found to 
be disordered, the symmetry for C5 and C7 was suppressed for chemical 
reasonability, and the ADPs were restrained using "ISOR 0.01 0.02". 
The C-C distances were also restrained to be similar using "SADI".
;
_shelx_res_checksum              38350
_shelx_hkl_checksum              68338