Ensembles from Silver Clusters and Cucurbit[6]urils-contained Linkers
Li, Na-Na; Yang, Ming; Xu, Xiao-Jie; Dong, Xi-Yan; Li, Si; Zang, Shuang-Quan; Dalton Transactions  (2021) –; doi:10.1039/D1DT02505H

data_7708475
_publ_section_title
;
 Ensembles from Silver Clusters and Cucurbit[6]urils-contained Linkers
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02505H
_journal_year                    2021
_chemical_formula_moiety
'C80.5 H82.5 Ag12 F24 N6.5 O19 S6, 0.5(C H4 O), C36 H36 N24 O12, 2(C7 H8), 2(C3 H7 N O)'
_chemical_formula_sum            'C137 H150.5 Ag12 F24 N32.5 O33.5 S6'
_chemical_formula_weight         4731.19
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-27 deposited with the CCDC.	2021-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.4025(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.29384(8)
_cell_length_b                   25.34019(12)
_cell_length_c                   21.44672(10)
_cell_measurement_reflns_used    40718
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      73.4130
_cell_measurement_theta_min      2.7800
_cell_volume                     8311.45(7)
_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      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_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    -35.00  22.00   0.50    0.50    --    0.00  77.00-150.00  114
  2  \w     11.00  37.00   0.50    0.50    --    0.00  57.00  60.00   52
  3  \w      5.00  88.00   0.50    0.50    --    0.00  38.00 150.00  166
  4  \w     30.00  89.00   0.50    0.50    --    0.00  77.00-150.00  118
  5  \w    -27.00   2.00   0.50    0.50    --    0.00  38.00 150.00   58
  6  \w     49.00  75.00   0.50    0.50    --    0.00  57.00  60.00   52
  7  \w    -24.00  80.00   0.50    0.50    --    0.00  57.00 -60.00  208
  8  \w      9.00 134.00   0.50    1.00    --   98.80 -82.00  90.00  250
  9  \w     11.00 132.00   0.50    1.00    --   98.80 -30.00-180.00  242
 10  \w     15.00  41.00   0.50    1.00    --   98.80 -61.00-180.00   52
 11  \w    101.00 127.00   0.50    1.00    --   98.80 -45.00  30.00   52
 12  \w     73.00 104.00   0.50    1.00    --   98.80 -82.00-180.00   62
 13  \w    110.00 136.00   0.50    1.00    --   98.80 -82.00-180.00   52
 14  \w     10.00 138.00   0.50    1.00    --   98.80 -15.00-180.00  256
 15  \w     17.00  53.00   0.50    1.00    --   98.80 -45.00  30.00   72
 16  \w     14.00 126.00   0.50    1.00    --   98.80 -61.00  90.00  224
 17  \w      9.00 103.00   0.50    1.00    --   98.80 -61.00 -30.00  188
 18  \w     71.00 187.00   0.50    1.00    --   98.80  30.00-180.00  232
 19  \w     51.00 109.00   0.50    1.00    --   98.80 -82.00-120.00  116
 20  \w     40.00 122.00   0.50    1.00    --   98.80 -82.00 -30.00  164
 21  \w     56.00 126.00   0.50    1.00    --   98.80 -61.00-180.00  140
 22  \w     87.00 112.00   0.50    1.00    --   98.80 -82.00 -60.00   50
 23  \w     77.00 102.00   0.50    1.00    --   98.80 -82.00  60.00   50
 24  \w     84.00 109.00   0.50    1.00    --   98.80 -82.00 150.00   50
 25  \w     96.00 121.00   0.50    1.00    --   98.80 -82.00   0.00   50
 26  \w     90.00 182.00   0.50    1.00    --   98.80  45.00 150.00  184
;
_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      0.0463728000
_diffrn_orient_matrix_UB_12      0.0539545000
_diffrn_orient_matrix_UB_13      -0.0011451000
_diffrn_orient_matrix_UB_21      0.0762889000
_diffrn_orient_matrix_UB_22      -0.0232070000
_diffrn_orient_matrix_UB_23      0.0384490000
_diffrn_orient_matrix_UB_31      0.0466491000
_diffrn_orient_matrix_UB_32      -0.0156774000
_diffrn_orient_matrix_UB_33      -0.0606766000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            89844
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.804
_diffrn_reflns_theta_min         3.375
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.715
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26724
_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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_description       block
_exptl_crystal_F_000             4688
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.096
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1405
_refine_ls_number_reflns         16623
_refine_ls_number_restraints     660
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+21.6554P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1033
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14714
_reflns_number_total             16623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02505h2.cif
_cod_data_source_block           SCM_2
_cod_original_cell_volume        8311.44(7)
_cod_original_formula_sum        'C137 H150.50 Ag12 F24 N32.50 O33.50 S6'
_cod_database_code               7708475
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.785
_shelx_estimated_absorpt_t_min   0.702
_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, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O18-C79
 1.4 with sigma of 0.01
 F9-C43 \\sim F16-C43 \\sim F17-C43 \\sim F10-C43 \\sim F18-C43 \\sim F5-C43
 with sigma of 0.01
 F20-C38 \\sim F2-C38 \\sim F21-C38 \\sim F4-C38 \\sim F19-C38 \\sim F6-C38
 with sigma of 0.01
 F1-C48 \\sim F22-C48 \\sim F8-C48 \\sim F23-C48 \\sim F24-C48 \\sim F11-C48
 with sigma of 0.01
 C65-C59 \\sim C59-C37 \\sim C69-C68 \\sim C73-C68 \\sim C73-C72 \\sim C72-C71
\\sim C71-C70 \\sim C69-C70
 \\sim C65-C63
 with sigma of 0.01
 C77-C31 \\sim C50-C31 \\sim C77-C78 \\sim C76-C31 \\sim C44-C31 \\sim C75-C76
\\sim C57-C44
 with sigma of 0.01
 C69-C32 \\sim C37-C32
 with sigma of 0.01
 C69-C68 \\sim C73-C68 \\sim C73-C72 \\sim C72-C71 \\sim C71-C70 \\sim C69-C70
 with sigma of 0.01
 C68-C71 \\sim C72-C69 \\sim C70-C73
 with sigma of 0.01
 C70-C68 \\sim C71-C73
 with sigma of 0.01
 N18-C84 \\sim N18-C85 \\sim N16-C66 \\sim N16-C83
 with sigma of 0.01
 F12-C41 \\sim F15-C41 \\sim F3-C41 \\sim F14-C41 \\sim F7-C41 \\sim F13-C41
 with sigma of 0.01
 N17-C82 \\sim N17-C81 \\sim N17-C80
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F5 \\sim F9 \\sim F10 \\sim F16 \\sim F17 \\sim F18: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
F2 \\sim F4 \\sim F6 \\sim F19 \\sim F20 \\sim F21: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
F1 \\sim F8 \\sim F11 \\sim F22 \\sim F23 \\sim F24: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C37 \\sim C47 \\sim C59 \\sim C61 \\sim C63 \\sim C65 \\sim C68 \\sim C69 \\sim
C70 \\sim C71 \\sim C72 \\sim C73: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C31 \\sim C44 \\sim C50 \\sim C57 \\sim C58 \\sim C60 \\sim C74 \\sim C75 \\sim
C76 \\sim C77 \\sim C78: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
N16 \\sim N18: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C66 \\sim C84 \\sim C85: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
F3 \\sim F7 \\sim F12 \\sim F13 \\sim F14 \\sim F15: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(F8) \\sim Ueq, Uanis(N17) \\sim Ueq, Uanis(C80) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(F7) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(F15) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(F13)=Sof(F14)=Sof(F15)=1-FVAR(1)
 Sof(F3)=Sof(F7)=Sof(F12)=FVAR(1)
 Sof(F16)=Sof(F17)=Sof(F18)=1-FVAR(2)
 Sof(F5)=Sof(F9)=Sof(F10)=FVAR(2)
 Sof(F19)=Sof(F20)=Sof(F21)=1-FVAR(3)
 Sof(F2)=Sof(F4)=Sof(F6)=FVAR(3)
 Sof(F22)=Sof(F23)=Sof(F24)=1-FVAR(4)
 Sof(F1)=Sof(F8)=Sof(F11)=FVAR(4)
 Sof(H32C)=Sof(H32D)=Sof(C68)=Sof(H68)=Sof(C69)=Sof(C70)=Sof(H70)=Sof(C71)=
 Sof(H71)=Sof(C72)=Sof(H72)=Sof(C73)=Sof(H73)=1-FVAR(5)
 Sof(H32A)=Sof(H32B)=Sof(C37)=Sof(C47)=Sof(H47)=Sof(C59)=Sof(H59)=Sof(C61)=
 Sof(H61)=Sof(C63)=Sof(H63)=Sof(C65)=Sof(H65)=FVAR(5)
 Sof(C74)=Sof(H74)=Sof(C75)=Sof(H75)=Sof(C76)=Sof(H76)=Sof(C77)=Sof(H77)=
 Sof(C78)=Sof(H78)=1-FVAR(6)
 Sof(C44)=Sof(H44)=Sof(C50)=Sof(H50)=Sof(C57)=Sof(H57)=Sof(C58)=Sof(H58)=
 Sof(C60)=Sof(H60)=FVAR(6)
 Sof(H54A)=Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(H84C)=Sof(C85)=Sof(H85A)=Sof(H85B)=
 Sof(H85C)=Sof(N18)=1-FVAR(7)
 Sof(H54)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=Sof(C83)=Sof(H83A)=Sof(H83B)=
 Sof(H83C)=Sof(N16)=FVAR(7)
 Fixed Sof: C67(0.5) H67A(0.5) H67B(0.5) H67C(0.5) C79(0.25) H79A(0.25)
 H79B(0.25) H79C(0.25) C80(0.25) H80(0.25) C81(0.25) H81A(0.25) H81B(0.25)
 H81C(0.25) C82(0.25) H82A(0.25) H82B(0.25) H82C(0.25) N17(0.25) O17(0.5)
 O18(0.25) H18(0.25)
5.a Everything fixed:
 H18
5.b Ternary CH refined with riding coordinates:
 C2(H2), C4(H4), C8(H8), C17(H17), C20(H20), C23(H23)
5.c Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C14(H14A,H14B), C16(H16A,H16B), C32(H32A,H32B), C32(H32C,
 H32D), C35(H35A,H35B), C42(H42A,H42B), C5(H5A,H5B), C7(H7A,H7B), C13(H13A,
 H13B), C15(H15A,H15B), C21(H21A,H21B), C26(H26A,H26B)
5.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C22(H22), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30), C34(H34),
 C36(H36), C44(H44), C47(H47), C50(H50), C54(H54), C54(H54A), C57(H57),
 C58(H58), C59(H59), C60(H60), C61(H61), C63(H63), C65(H65), C68(H68), C70(H70),
  C71(H71), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C77(H77),
 C78(H78), C80(H80), C45(H45), C49(H49), C51(H51), C52(H52), C53(H53), C46(H46)
5.e Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C79(H79A,H79B,H79C), C81(H81A,H81B,
 H81C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C85(H85A,
 H85B,H85C), C64(H64A,H64B,H64C), C55(H55A,H55B,H55C), C62(H62A,H62B,H62C)
;
_shelx_res_checksum              59723
_shelx_hkl_checksum              47727
_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 2.434
_oxdiff_exptl_absorpt_empirical_full_min 0.690