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_7121583
_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      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   25.2076(4)
_cell_length_b                   25.2076(4)
_cell_length_c                   15.3459(3)
_cell_measurement_reflns_used    10622
_cell_measurement_temperature    250.00(10)
_cell_measurement_theta_max      72.7810
_cell_measurement_theta_min      3.5030
_cell_volume                     8444.7(3)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      250.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.999
_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    -76.00 -51.00   0.50    0.50    --    0.00 -77.00 -30.00   50
  2  \w    -27.00  56.00   0.50    0.50    --    0.00  57.00 -90.00  166
  3  \w     -9.00  29.00   0.50    0.50    --    0.00 -77.00 -30.00   76
  4  \w     19.00 128.00   0.50    4.00    --   97.60 -82.00 -90.00  218
  5  \w     69.00 159.00   0.50    4.00    --   97.60  45.00 120.00  180
  6  \w     24.00 115.00   0.50    4.00    --   97.60 -61.00 -90.00  182
  7  \w     93.00 176.00   0.50    4.00    --   97.60  45.00  90.00  166
;
_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      -0.0567071000
_diffrn_orient_matrix_UB_12      -0.0562596000
_diffrn_orient_matrix_UB_13      0.0381011000
_diffrn_orient_matrix_UB_21      0.0390396000
_diffrn_orient_matrix_UB_22      -0.0299889000
_diffrn_orient_matrix_UB_23      0.0198757000
_diffrn_orient_matrix_UB_31      0.0152187000
_diffrn_orient_matrix_UB_32      0.0301598000
_diffrn_orient_matrix_UB_33      0.0907740000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26474
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.495
_diffrn_reflns_theta_min         2.024
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.113
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34820
_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    1.361
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.400
_refine_diff_density_min         -1.397
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       0.000038(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         2773
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0798
_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^)+(0.0808P)^2^+60.6256P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2080
_refine_ls_wR_factor_ref         0.2124
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2352
_reflns_number_total             2773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01559g3.cif
_cod_data_source_block           ab
_cod_database_code               7121583
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H O N Ag F S'
_chemical_oxdiff_usercomment     'C H O'
_reflns_odcompleteness_completeness 99.97
_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
 C3-C1 = C2-C1 = C4-C1
 1.53 with sigma of 0.01
 O1-C5 \\sim O2-C5
 with sigma of 0.01
 C10-C9 \\sim C11-C10 \\sim C12-C13 \\sim C12-C11 \\sim C13-N4
 with sigma of 0.01
 C10-C13 \\sim C12-C11_$1
 with sigma of 0.01
 C11_$1-C11 \\sim C12-C12_$1
 with sigma of 0.01
 F2-C6 \\sim F1-C6 \\sim F6-C6 \\sim F5-C6 \\sim F4-C6 \\sim F3-C6
 with sigma of 0.01
 C8-C7 \\sim C9-C8
 with sigma of 0.01
 C16-C15 \\sim C15-C14
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F1 \\sim F6 \\sim F5 \\sim F4 \\sim F3 \\sim F2: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
C5 \\sim C6: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq,
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(F3)
\\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq,
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: Ag3(0.5) S1(0.5) F1(0.25) F2(0.25) F3(0.25) F4(0.25) F5(0.25)
 F6(0.25) O1(0.5) O2(0.5) C1(0.5) C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) C3(0.5)
 H3A(0.5) H3B(0.5) H3C(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) C5(0.5) C6(0.5)
 C7(0.5) H7(0.5) C8(0.5) H8(0.5) C11(0.5) H11(0.5) C12(0.5) H12(0.5) C14(0.5)
 H14(0.5) C15(0.5) H15(0.5) C18(0.5) H18(0.5) C19(0.5) H19(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C11(H11), C12(H12), C14(H14), C15(H15), C18(H18), C19(H19)
5.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              68522
_shelx_hkl_checksum              26292
_shelx_fab_checksum              75346
_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 2.347
_oxdiff_exptl_absorpt_empirical_full_min 0.623