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_7121585
_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         '0.33(C306 H306 Ag36 F54 N24 O36 S18)'
_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           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-05
_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            3
_cell_length_a                   43.8008(6)
_cell_length_b                   43.8008(6)
_cell_length_c                   11.1753(4)
_cell_measurement_reflns_used    12420
_cell_measurement_temperature    250.00(10)
_cell_measurement_theta_max      67.1680
_cell_measurement_theta_min      3.4840
_cell_volume                     18567.5(8)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      250.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.875
_diffrn_measured_fraction_theta_max 0.932
_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    135.00 178.00   0.25    2.50    --  100.10  82.00 -30.00  172
  2  \w    160.00 189.00   0.25    2.50    --  100.10  82.00 150.00  116
  3  \w     99.00 131.00   0.25    0.50    --   45.50  77.00  30.00  128
  4  \w     88.00 134.00   0.25    0.50    --   45.50  82.00 -30.00  184
  5  \w    103.00 132.00   0.25    0.50    --   45.50  82.00-120.00  116
  6  \w     89.00 117.00   0.25    0.50    --   45.50  82.00 150.00  112
  7  \w     45.00 162.00   0.25    2.50    --  100.10  15.00   0.00  468
  8  \w     92.00 134.00   0.25    2.50    --  100.10 -77.00  30.00  168
  9  \w     72.00  98.00   0.25    2.50    --  100.10 -82.00   0.00  104
 10  \w     -6.00  38.00   0.25    0.50    --   45.50 -82.00 150.00  176
;
_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      0.0311618000
_diffrn_orient_matrix_UB_12      -0.0069519000
_diffrn_orient_matrix_UB_13      -0.0050214000
_diffrn_orient_matrix_UB_21      0.0259736000
_diffrn_orient_matrix_UB_22      0.0397032000
_diffrn_orient_matrix_UB_23      0.0161146000
_diffrn_orient_matrix_UB_31      -0.0019366000
_diffrn_orient_matrix_UB_32      -0.0049295000
_diffrn_orient_matrix_UB_33      0.1368184000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_unetI/netI     0.0918
_diffrn_reflns_Laue_measured_fraction_full 0.875
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            46480
_diffrn_reflns_point_group_measured_fraction_full 0.875
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         64.992
_diffrn_reflns_theta_min         2.330
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.264
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7b (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    0.929
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             5064
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.252
_refine_diff_density_min         -3.012
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1367
_refine_ls_number_reflns         19616
_refine_ls_number_restraints     2242
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1564
_refine_ls_R_factor_gt           0.1378
_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^)+(0.3500P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4309
_refine_ls_wR_factor_ref         0.4506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13373
_reflns_number_total             19616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01559g2.cif
_cod_data_source_block           aa
_cod_database_code               7121585
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H O N S Ag'
_shelx_estimated_absorpt_t_max   0.637
_shelx_estimated_absorpt_t_min   0.492
_reflns_odcompleteness_completeness 97.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.94
_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
{O5, C88}
{C91, O8}
{O10, C69}
{O11, C68}
3. Restrained distances
 O2-C85
 1.3 with sigma of 0.01
 C90-C89 = C92-C93 = C97-C91 = C71-C69
 1.53 with sigma of 0.01
 C80-C78 = C84-C81 = C86-C21 = C87-C85
 1.53 with sigma of 0.01
 F2-C87 = F1-C87 = F3-C87 = C50-C51 = F9-C90
 1.39 with sigma of 0.01
 F19-C98
 1.39 with sigma of 0.01
 C101-C91 = C102-C91 = C97-C91 = C99-C100 = C74-C68
 1.53 with sigma of 0.01
 C95-C88 = C88-C96 = C94-C88 = C73-C98
 1.53 with sigma of 0.01
 S3B-C81 \\sim S3-C78
 with sigma of 0.01
 O1-C21 \\sim O3-C85 \\sim O2-C85 \\sim O4-C21
 with sigma of 0.01
 C62-C34 \\sim C59-C34 \\sim C59-C61 \\sim C46-C61 \\sim C58-C53 \\sim C53-C54
\\sim C54-C55 \\sim C62-C60
 \\sim C56-C55 \\sim C57-C56 \\sim C58-C57 \\sim C46-C60
 with sigma of 0.01
 F12-C90 \\sim F10-C90 \\sim F7-C90 \\sim F11-C90 \\sim F8-C90 \\sim F9-C90
 with sigma of 0.01
 O6-C89 \\sim O5-C89
 with sigma of 0.01
 O7-C92 \\sim O8-C92
 with sigma of 0.01
 F13-C93 \\sim F18-C93 \\sim F14-C93 \\sim F16-C93 \\sim F15-C93 \\sim F17-C93
 with sigma of 0.01
 C72-C69 \\sim C70-C69 \\sim C71-C69
 with sigma of 0.01
 O10-C73 \\sim O9-C73
 with sigma of 0.01
 F27-C100 \\sim F23-C100 \\sim F26-C100 \\sim F24-C100 \\sim F22-C100 \\sim
F25-C100
 with sigma of 0.01
 F20-C98 \\sim F21-C98 \\sim F19-C98
 with sigma of 0.01
 C80-C78 \\sim C84-C81 \\sim C83-C81 \\sim C79-C78 \\sim C78-C77 \\sim C82-C81
 with sigma of 0.01
 C28-C29 \\sim C47-C48 \\sim C47-C52 \\sim C28-C32 \\sim C51-C52 \\sim C32-C31
\\sim C50-C51 \\sim C33-C31
 \\sim C33-C30 \\sim C50-C49 \\sim C49-C48 \\sim C30-C29
 with sigma of 0.01
 F4-C86 \\sim F6-C86 \\sim F1-C87 \\sim F5-C86
 with sigma of 0.01
 F2-F3 \\sim F3-F1
 with sigma of 0.01
 F23-C99 \\sim C99-F27
 with sigma of 0.01
 O12-C99 \\sim O11-C99
 with sigma of 0.01
 C33-C12 \\sim C50-C19 \\sim C46-C43 \\sim C58-C1 \\sim C67-C25 \\sim C9-C38
 with sigma of 0.01
 N5-C34 \\sim N6-C55 \\sim N6-C22 \\sim N5-C35 \\sim N6-C47 \\sim N5-C28
 with sigma of 0.01
 C102-C101 \\sim C101-C97 \\sim C97-C102
 with sigma of 0.01
 C95-C96 \\sim C96-C94 \\sim C94-C95
 with sigma of 0.01
 C74-C68 \\sim C75-C68 \\sim C76-C68
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
S3 \\sim S3B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C86 \\sim F4 \\sim F5 \\sim F6: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C34 \\sim C46 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim
C59 \\sim C60 \\sim C61 \\sim C62: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim O9 \\sim O10 \\sim F19 \\sim
F20 \\sim F21 \\sim C98: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C29 \\sim C47 \\sim C32 \\sim C31 \\sim C33 \\sim C30 \\sim C48 \\sim C28 \\sim
C52 \\sim C51 \\sim C50 \\sim C49: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C78 \\sim C79 \\sim C80 \\sim C84 \\sim C81 \\sim C83 \\sim C82 \\sim C77:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O1 \\sim C21 \\sim O2 \\sim O3 \\sim C85 \\sim O4 \\sim C86 \\sim C87: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C87 \\sim F1 \\sim F2 \\sim F3: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C5 \\sim C6 \\sim N2 \\sim C7 \\sim C8 \\sim C9 \\sim C25 \\sim C38 \\sim N8
\\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
C24 \\sim C25 \\sim C26 \\sim C37 \\sim C38 \\sim C39: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C22 \\sim C23 \\sim C27 \\sim C35 \\sim C36 \\sim C40: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
N1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C10 \\sim N7 \\sim C41 \\sim C42
\\sim C43 \\sim C44 \\sim C45: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
O7 \\sim C91 \\sim C92 \\sim O8 \\sim C93 \\sim F13 \\sim F14 \\sim F15 \\sim
F16 \\sim F17 \\sim F18 \\sim C97 \\sim C101 \\sim C102: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C88 \\sim O5 \\sim O6 \\sim C89 \\sim F7 \\sim C90 \\sim F8 \\sim F9 \\sim F10
\\sim F11 \\sim F12 \\sim C94 \\sim C95 \\sim C96: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
C68 \\sim C74 \\sim C75 \\sim C76 \\sim O11 \\sim O12 \\sim C99 \\sim C100
\\sim F22 \\sim F23 \\sim F24 \\sim F25 \\sim F26 \\sim F27: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S3B) \\sim Ueq, Uanis(S3) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C40) \\sim Ueq,
Uanis(C86) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C98)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C92)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(N6) \\sim Ueq,
Uanis(C17) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C57) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C80) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O5) = Uanis(C88)
Uanis(C91) = Uanis(O8)
Uanis(O10) = Uanis(C69)
Uanis(O11) = Uanis(C68)
5. Others
 Fixed Sof: Ag3(0.65) Ag6(0.5) Ag4(0.65) Ag5(0.5) Ag4B(0.35) Ag3B(0.35)
 Ag5B(0.5) Ag6B(0.5) S3(0.5) S3B(0.5) S1(0.65) S1B(0.35) S2(0.65) S2B(0.35)
 N1(0.5) C1(0.5) C2(0.5) H2(0.5) C3(0.5) H3(0.5) C4(0.5) H4(0.5) C5(0.5)
 H5(0.5) C6(0.5) H6(0.5) N2(0.5) C7(0.5) H7(0.5) C8(0.5) H8(0.5) C9(0.5)
 C10(0.5) H10(0.5) C11(0.5) H11(0.5) C12(0.5) C13(0.5) H13(0.5) C14(0.5)
 H14(0.5) N3(0.5) C15(0.5) H15(0.5) C16(0.5) H16(0.5) N4(0.5) C17(0.5) H17(0.5)
 C18(0.5) H18(0.5) C19(0.5) C20(0.5) H20(0.5) N5(0.5) O1(0.5) C21(0.5) C22(0.5)
 C23(0.5) H23(0.5) C24(0.5) H24(0.5) C25(0.5) C26(0.5) H26(0.5) C27(0.5)
 H27(0.5) C29(0.5) H29(0.5) C47(0.5) C32(0.5) H32(0.5) C31(0.5) H31(0.5)
 C33(0.5) C30(0.5) H30(0.5) N6(0.5) C34(0.5) C35(0.5) C36(0.5) H36(0.5)
 C37(0.5) H37(0.5) C38(0.5) C39(0.5) H39(0.5) C40(0.5) H40(0.5) N7(0.5)
 C41(0.5) H41(0.5) C42(0.5) H42(0.5) C43(0.5) C44(0.5) H44(0.5) C45(0.5)
 H45(0.5) C46(0.5) C48(0.5) H48(0.5) C28(0.5) C52(0.5) H52(0.5) C51(0.5)
 H51(0.5) C50(0.5) C49(0.5) H49(0.5) C53(0.5) H53(0.5) C54(0.5) H54(0.5)
 C55(0.5) C56(0.5) H56(0.5) C57(0.5) H57(0.5) C58(0.5) C59(0.5) H59(0.5)
 C60(0.5) H60(0.5) C61(0.5) H61(0.5) C62(0.5) H62(0.5) N8(0.5) C63(0.5)
 H63(0.5) C64(0.5) H64(0.5) C65(0.5) H65(0.5) C66(0.5) H66(0.5) C67(0.5)
 C68(0.65) C69(0.65) C70(0.65) H70A(0.65) H70B(0.65) H70C(0.65) C71(0.65)
 H71A(0.65) H71B(0.65) H71C(0.65) C72(0.65) H72A(0.65) H72B(0.65) H72C(0.65)
 C73(0.35) C74(0.65) H74A(0.65) H74B(0.65) H74C(0.65) C75(0.65) H75A(0.65)
 H75B(0.65) H75C(0.65) C76(0.65) H76A(0.65) H76B(0.65) H76C(0.65) C77(0.5)
 H77A(0.5) H77B(0.5) H77C(0.5) C78(0.5) C79(0.5) H79A(0.5) H79B(0.5) H79C(0.5)
 C80(0.5) H80A(0.5) H80B(0.5) H80C(0.5) C81(0.5) C82(0.5) H82A(0.5) H82B(0.5)
 H82C(0.5) C83(0.5) H83A(0.5) H83B(0.5) H83C(0.5) C84(0.5) H84A(0.5) H84B(0.5)
 H84C(0.5) O2(0.5) O3(0.5) C85(0.5) O4(0.5) C86(0.5) C87(0.5) F1(0.5) F2(0.5)
 F3(0.5) F4(0.5) F5(0.5) F6(0.5) C88(0.35) O5(0.65) O6(0.65) C89(0.65)
 F7(0.325) C90(0.65) F8(0.325) F9(0.325) F10(0.325) F11(0.325) F12(0.325)
 O7(0.65) C91(0.35) C92(0.65) O8(0.65) C93(0.65) F13(0.325) F14(0.325)
 F15(0.325) F16(0.325) F17(0.325) F18(0.325) O9(0.35) C94(0.35) H94A(0.35)
 H94B(0.35) H94C(0.35) C95(0.35) H95A(0.35) H95B(0.35) H95C(0.35) C96(0.35)
 H96A(0.35) H96B(0.35) H96C(0.35) C97(0.35) H97A(0.35) H97B(0.35) H97C(0.35)
 O10(0.35) F19(0.35) F20(0.35) F21(0.35) C98(0.35) O11(0.35) O12(0.35)
 C99(0.35) C100(0.35) F22(0.175) F23(0.175) F24(0.175) F25(0.175) F26(0.175)
 F27(0.175) C101(0.35) H10A(0.35) H10B(0.35) H10C(0.35) C102(0.35) H10D(0.35)
 H10E(0.35) H10F(0.35)
6.a Riding coordinates:
 C76(H76A,H76B,H76C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C), C101(H10A,H10B,
 H10C), C102(H10D,H10E,H10F)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C23(H23),
  C24(H24), C26(H26), C27(H27), C29(H29), C32(H32), C31(H31), C30(H30),
 C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45),
  C48(H48), C52(H52), C51(H51), C49(H49), C53(H53), C54(H54), C56(H56),
 C57(H57), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65),
  C66(H66)
6.c Fitted hexagon refined as free rotating group:
 C5(C6,N2,C7,C8,C9), C11(C12,C13,C14,N3,C15), C22(C23,C24,C25,C26,C27),
 C29(C47,C32,C31,C33,C30), C35(C36,C37,C38,C39,C40), N7(C41,C42,C43,C44,C45),
 C48(C28,C52,C51,C50,C49), C53(C54,C55,C56,C57,C58)
6.d Idealised Me refined as rotating group:
 C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C74(H74A,H74B,
 H74C), C75(H75A,H75B,H75C), C77(H77A,H77B,H77C), C79(H79A,H79B,H79C), C80(H80A,
 H80B,H80C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C),
 C94(H94A,H94B,H94C), C97(H97A,H97B,H97C)
;
_shelx_res_checksum              29573
_shelx_hkl_checksum              20158
_shelx_fab_checksum              31240
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.300
_oxdiff_exptl_absorpt_empirical_full_min 0.527