Epitaxial Coordination Assembly of Semi-conductive Silver-chalcogenide Layer-based MOF
Gong, Chun-Hua; Hu, Xiaozong; Han, Zhen; Liu, Xiao-Fei; Yang, Min-Zi; Zang, Shuang-Quan; Chemical Communications  (2022) –; doi:10.1039/D1CC07160B

data_7129510
_publ_section_title
;
 Epitaxial Coordination Assembly of Semi-conductive Silver-chalcogenide
 Layer-based MOF
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC07160B
_journal_year                    2022
_chemical_formula_moiety         'C17 H29 Ag6 O4 S4'
_chemical_formula_sum            'C17 H29 Ag6 O4 S4'
_chemical_formula_weight         1072.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-20
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2021-09-27 deposited with the CCDC.	2022-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.191(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2510(4)
_cell_length_b                   19.6897(6)
_cell_length_c                   12.4126(5)
_cell_measurement_reflns_used    9489
_cell_measurement_temperature    199.99(10)
_cell_measurement_theta_max      28.6700
_cell_measurement_theta_min      2.7490
_cell_volume                     2596.94(17)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      199.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.863
_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    -92.00 -30.00   0.50    1.00    --   -3.60 -57.00-180.00  124
  2  \w     63.00  93.00   0.50    1.00    --    3.60  19.00 -90.00   60
  3  \w    -24.00  92.00   0.50    1.00    --    3.60  82.00-120.00  232
  4  \w    -21.00  24.00   0.50    1.00    --    3.60  57.00   0.00   90
  5  \w    -41.00  21.00   0.50    1.00    --    3.60  19.00 -90.00  124
;
_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      0.0185513000
_diffrn_orient_matrix_UB_12      -0.0242752000
_diffrn_orient_matrix_UB_13      -0.0335930000
_diffrn_orient_matrix_UB_21      0.0206000000
_diffrn_orient_matrix_UB_22      -0.0220545000
_diffrn_orient_matrix_UB_23      0.0477291000
_diffrn_orient_matrix_UB_31      -0.0607271000
_diffrn_orient_matrix_UB_32      -0.0149043000
_diffrn_orient_matrix_UB_33      -0.0159492000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.863
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23921
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.863
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.159
_diffrn_reflns_theta_min         2.022
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.780
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64870
_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            color
_exptl_crystal_density_diffrn    2.744
_exptl_crystal_description       block
_exptl_crystal_F_000             2036
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.823
_refine_diff_density_min         -1.818
_refine_diff_density_rms         0.374
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         6039
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0935
_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^)+(0.0415P)^2^+396.5911P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2321
_refine_ls_wR_factor_ref         0.2413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5369
_reflns_number_total             6039
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc07160b2.cif
_cod_data_source_block           3D_MOF
_cod_database_code               7129510
_shelxl_version_number           2013-2
_chemical_oxdiff_usercomment     ' '
_reflns_odcompleteness_completeness 99.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13-C12
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H13A)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=1-FVAR(1)
 Sof(H13)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
 Sof(H2B)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=1-FVAR(2)
 Sof(H2A)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C13(H13A), C2(H2A), C2(H2B), C9(H9), C6(H6)
5.b Aromatic/amide H refined with riding coordinates:
 C15(H15)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C1(H1A,H1B,H1C), C7(H7A,H7B,H7C), C5(H5A,H5B,H5C),
 C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C4(H4A,H4B,H4C),
 C11(H11A,H11B,H11C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              84908
_shelx_hkl_checksum              61481
_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 2.352
_oxdiff_exptl_absorpt_empirical_full_min 0.788