Layer-sliding-driven crystal size and photoluminescence change in a novel SCC-MOF
Zang, Shuang-Quan; Du, Xiang-Sha; Yan, Bing-Jie; Wang, Jia-Yin; Xi, Xiao-Juan; Wang, Zhao-Yang; Chemical Communications  (2018) –; doi:10.1039/C8CC01559G

data_7121584
_publ_section_title
;
 Layer-sliding-driven crystal size and photoluminescence change in a novel
 SCC-MOF
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC01559G
_journal_year                    2018
_chemical_formula_moiety         'C102 H102 Ag12 F18 N8 O12 S6'
_chemical_formula_sum            'C102 H102 Ag12 F18 N8 O12 S6'
_chemical_formula_weight         3460.71
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m'
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   25.140(3)
_cell_length_b                   25.140(3)
_cell_length_c                   20.039(4)
_cell_measurement_reflns_used    1489
_cell_measurement_temperature    250.00(10)
_cell_measurement_theta_max      71.7840
_cell_measurement_theta_min      4.5950
_cell_volume                     10968(3)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      250.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.991
_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     36.00  81.00   0.50    2.00    --    0.00  57.00  60.00   90
  2  \w    -24.00  11.00   0.50    2.00    --    0.00  57.00  60.00   70
  3  \w     98.00 183.00   0.50   25.00    --   97.60  45.00 150.00  170
  4  \w     84.00 156.00   0.50   25.00    --   97.60  45.00  90.00  144
  5  \w      8.00 102.50   0.50   25.00    --   97.60 -61.00-150.00  189
;
_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      0.0297943000
_diffrn_orient_matrix_UB_12      0.0028791000
_diffrn_orient_matrix_UB_13      0.0679738000
_diffrn_orient_matrix_UB_21      -0.0328020000
_diffrn_orient_matrix_UB_22      0.0320897000
_diffrn_orient_matrix_UB_23      0.0306810000
_diffrn_orient_matrix_UB_31      -0.0551322000
_diffrn_orient_matrix_UB_32      -0.0632698000
_diffrn_orient_matrix_UB_33      0.0182174000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0932
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7657
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.493
_diffrn_reflns_theta_min         3.516
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.989
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (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    1.572
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             5064
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.104
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         2359
_refine_ls_number_restraints     170
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.1601
_refine_ls_R_factor_gt           0.1233
_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^)+(0.2000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3267
_refine_ls_wR_factor_ref         0.3459
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1256
_reflns_number_total             2359
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01559g5.cif
_cod_data_source_block           abc_250k
_cod_original_cell_volume        10969(3)
_cod_database_code               7121584
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H O N Ag S F'
_chemical_oxdiff_usercomment     'C H O'
_shelx_estimated_absorpt_t_max   0.401
_shelx_estimated_absorpt_t_min   0.285
_reflns_odcompleteness_completeness 99.69
_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. Shared sites
{C12, O1}
3. Restrained distances
 C12-C13
 1.53 with sigma of 0.01
 C16-C17
 1.53 with sigma of 0.01
 F3B-F1B \\sim F1B-F2B \\sim F2B-F3B
 with sigma of 0.01
 F1A-C17 \\sim F3B-C17 \\sim F2A-C17 \\sim F1B-C17 \\sim F3A-C17 \\sim F2B-C17
 with sigma of 0.01
 F2A-F3A \\sim F3A-F1A \\sim F1A-F2A
 with sigma of 0.01
 C12-C15 \\sim C12-C13 \\sim C12-C14
 with sigma of 0.01
 C12-C14 \\sim C12-C15 \\sim C12-C13
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
F3A \\sim F1A \\sim F2B \\sim F2A \\sim F3B \\sim F1B: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
C16 \\sim C17: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(F3B) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F1B) \\sim Ueq, Uanis(F3A)
\\sim Ueq, Uanis(F2B) \\sim Ueq, Uanis(F1A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C13) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C12) = Uanis(O1)
5. Others
 Fixed Sof: C12(0.5) C2(0.5) H2(0.5) C11(0.5) H11(0.5) C7(0.5) H7(0.5)
 C10(0.5) H10(0.5) C8(0.5) H8(0.5) Ag1(0.5) C13(0.5) H13A(0.5) H13B(0.5)
 H13C(0.5) C16(0.5) S1(0.5) C1(0.5) H1(0.5) C15(0.5) H15A(0.5) H15B(0.5)
 H15C(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5) F3A(0.25) O2(0.5) C17(0.5)
 O1(0.5) F1A(0.25) C5(0.5) H5(0.5) C4(0.5) H4(0.5) F2B(0.25) F2A(0.25)
 F3B(0.25) F1B(0.25)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C11(H11), C7(H7), C10(H10), C8(H8), C1(H1), C5(H5), C4(H4)
6.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C14(H14A,H14B,H14C)
;
_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 2.137
_oxdiff_exptl_absorpt_empirical_full_min 0.485