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_7708476
_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
'0.5(C128 H170.67 Ag24 N8 O48 S28), 0.66(C36 H36 N24 O12), 0.34(C36 H32 N24 O12)'
_chemical_formula_sum            'C100 H119.96 Ag12 N28 O36 S14'
_chemical_formula_weight         4033.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-04
_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                 92.988(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.7785(17)
_cell_length_b                   15.0645(13)
_cell_length_c                   29.008(3)
_cell_measurement_reflns_used    11644
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      72.5920
_cell_measurement_theta_min      2.9580
_cell_volume                     6449.3(11)
_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 0.999
_diffrn_measured_fraction_theta_max 0.956
_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    -28.00  88.00   0.50    0.50    --    0.00  38.00 -60.00  232
  2  \w    -21.00  30.00   0.50    0.50    --    0.00  38.00-150.00  102
  3  \w     -7.00  28.00   0.50    0.50    --    0.00 -57.00   0.00   70
  4  \w    -45.00 -12.00   0.50    0.50    --    0.00 -57.00   0.00   66
  5  \w     60.00  86.00   0.50    0.50    --    0.00  38.00-150.00   52
  6  \w    135.00 161.00   0.50    5.00    --   97.60  30.00 150.00   52
  7  \w      8.00 106.00   0.50    5.00    --   97.60 -61.00-120.00  196
  8  \w      9.00 104.00   0.50    5.00    --   97.60 -45.00-120.00  190
  9  \w     70.00 176.00   0.50    5.00    --   97.60  45.00 120.00  212
 10  \w     65.00 187.00   0.50    5.00    --   97.60  82.00   0.00  244
 11  \w     69.00 165.00   0.50    5.00    --   97.60  45.00  90.00  192
 12  \w    123.00 149.00   0.50    5.00    --   97.60 -15.00  90.00   52
 13  \w     92.00 118.00   0.50    5.00    --   97.60 -61.00-180.00   52
 14  \w      9.00  50.00   0.50    5.00    --   97.60 -15.00  90.00   82
;
_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      -0.0561100000
_diffrn_orient_matrix_UB_12      -0.0335495000
_diffrn_orient_matrix_UB_13      -0.0431545000
_diffrn_orient_matrix_UB_21      -0.0615565000
_diffrn_orient_matrix_UB_22      0.0816298000
_diffrn_orient_matrix_UB_23      0.0027780000
_diffrn_orient_matrix_UB_31      0.0634815000
_diffrn_orient_matrix_UB_32      0.0518587000
_diffrn_orient_matrix_UB_33      -0.0306041000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_av_unetI/netI     0.0725
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            34606
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.792
_diffrn_reflns_theta_min         2.933
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.144
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51829
_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    2.077
_exptl_crystal_description       block
_exptl_crystal_F_000             3984
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.156
_refine_diff_density_min         -3.246
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1331
_refine_ls_number_reflns         12669
_refine_ls_number_restraints     1083
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1558
_refine_ls_R_factor_gt           0.1317
_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^)+(0.1683P)^2^+180.7074P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3430
_refine_ls_wR_factor_ref         0.3621
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9020
_reflns_number_total             12669
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02505h2.cif
_cod_data_source_block           SCM_1
_cod_database_code               7708476
_shelxl_version_number           2013-2
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.726
_shelx_estimated_absorpt_t_min   0.627
_reflns_odcompleteness_completeness 99.90
_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
2. Restrained distances
 S8-C70
 1.7 with sigma of 0.01
 N9-C51 \\sim N8-C46 \\sim N8-C43 \\sim N12-C48 \\sim N6-C48 \\sim N14-C40
\\sim N7-C40 \\sim N4-C36 \\sim N3-
 C36 \\sim N11-C42 \\sim N10-C42
 with sigma of 0.01
 N9-C47 \\sim N11-C46 \\sim N13-C49 \\sim N12-C38
 with sigma of 0.01
 O27-C70 \\sim C70-O26
 with sigma of 0.01
 S6-C31 \\sim S8-C70
 with sigma of 0.01
 O26-C70 \\sim C70-O25
 with sigma of 0.01
 S5-C71 \\sim S5-C26
 with sigma of 0.01
 N15-C63 \\sim N24-C63 \\sim N13-C43 \\sim N8-C43
 with sigma of 0.01
 C77-C76 \\sim C74-C78
 with sigma of 0.01
 C75-C78 \\sim C74-C75 \\sim C74-C76 \\sim C73-C76 \\sim C77-C73 \\sim C78-C77
 with sigma of 0.01
 N18-C57 \\sim N21-C57 \\sim N14-C39 \\sim N4-C39
 with sigma of 0.01
 N21-O20 \\sim O20-N18
 with sigma of 0.01
 O24-C69 \\sim O16-C35 \\sim O17-C37 \\sim O23-C67 \\sim O21-C59 \\sim O18-C41
\\sim O22-C61 \\sim O15-C44
 \\sim O13-C34 \\sim O19-C52 \\sim O14-C39 \\sim O20-C57
 with sigma of 0.01
 O12-C31 \\sim C31-O9
 with sigma of 0.01
 O9-C31 \\sim C31-O10
 with sigma of 0.01
 S8-O27 \\sim S6-O12 \\sim S6-O10 \\sim S8-O25 \\sim S8-O26 \\sim S6-O9
 with sigma of 0.01
3. Restrained planarity
 C73, C74, C75, C76, C77, C78
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C28 \\sim C33: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
N1 \\sim N2 \\sim N3 \\sim N4 \\sim N5 \\sim N6 \\sim N7 \\sim N8 \\sim N9
\\sim N10 \\sim N11 \\sim N12 \\sim N13 \\sim N14 \\sim N15 \\sim N16 \\sim N17
\\sim N18 \\sim N19 \\sim N20 \\sim N21 \\sim N22 \\sim N23 \\sim N24 \\sim N25
\\sim N26: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C31 \\sim C70: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C26 \\sim C71: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim
C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim
C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim
C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim
C66 \\sim C67 \\sim C68 \\sim C69: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C19 \\sim C22 \\sim C25 \\sim C27 \\sim C30 \\sim C32: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
O6 \\sim O8 \\sim O11 \\sim O28 \\sim O29 \\sim O30: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C72 \\sim C73
\\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
O13 \\sim O15 \\sim O16 \\sim O17 \\sim O18 \\sim O19 \\sim O21 \\sim O22 \\sim
O23 \\sim O24: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O9 \\sim O10 \\sim O12: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O9 \\sim O10 \\sim O12 \\sim O25 \\sim O26 \\sim O27: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(O13) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O20)
\\sim Ueq, Uanis(S6) \\sim Ueq, Uanis(S8) \\sim Ueq, Uanis(O22) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C26) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C12) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O26) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(O25)
\\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O23) \\sim Ueq, Uanis(O21) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(C52)=Sof(C53)=Sof(H53)=Sof(C54)=Sof(H54)=Sof(C55)=Sof(H55A)=Sof(H55B)=
 Sof(C56)=Sof(H56)=Sof(C57)=Sof(C58)=Sof(H58)=Sof(C59)=Sof(C60)=Sof(H60)=
 Sof(C61)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(C64)=Sof(H64)=
 Sof(C65)=Sof(H65)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(C67)=Sof(C68)=Sof(H68A)=
 Sof(H68B)=Sof(C69)=Sof(N15)=Sof(N16)=Sof(N17)=Sof(N18)=Sof(N19)=Sof(N20)=
 Sof(N21)=Sof(N22)=Sof(N23)=Sof(N24)=Sof(N25)=Sof(N26)=Sof(O19)=Sof(O20)=
 Sof(O21)=Sof(O22)=Sof(O23)=Sof(O24)=1-FVAR(1)
 Sof(C34)=Sof(C35)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(C38)=Sof(H38)=
 Sof(C39)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(C42)=Sof(H42A)=Sof(H42B)=
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=
 Sof(C47)=Sof(H47)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C49)=Sof(H49)=Sof(C50)=
 Sof(H50)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(N3)=Sof(N4)=Sof(N5)=Sof(N6)=Sof(N7)=
 Sof(N8)=Sof(N9)=Sof(N10)=Sof(N11)=Sof(N12)=Sof(N13)=Sof(N14)=Sof(O13)=Sof(O14)=
 Sof(O15)=Sof(O16)=Sof(O17)=Sof(O18)=FVAR(1)
 Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(O25)=Sof(O26)=Sof(O27)=Sof(S8)=1-FVAR(2)
 Sof(C31)=Sof(H31B)=Sof(H31C)=Sof(H31A)=Sof(O9)=Sof(O10)=Sof(O12)=Sof(S6)=
 FVAR(2)
 Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=Sof(O28)=Sof(O29)=Sof(O30)=1-FVAR(3)
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(O6)=Sof(O8)=Sof(O11)=FVAR(3)
 Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(C73)=Sof(C74)=Sof(H74)=Sof(C75)=Sof(H75)=
 Sof(C76)=Sof(H76)=Sof(C77)=Sof(H77)=Sof(C78)=Sof(H78)=1-FVAR(4)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C7)=
 Sof(H7)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=FVAR(4)
 Fixed Sof: H24A(0.5) H24B(0.5) H24C(0.5) H24D(0.5) C28(0.5) H28A(0.5)
 H28B(0.5) C33(0.5) H33A(0.5) H33B(0.5)
6.a Ternary CH refined with riding coordinates:
 C38(H38), C45(H45), C46(H46), C47(H47), C49(H49), C50(H50), C54(H54),
 C56(H56), C58(H58), C62(H62), C64(H64), C65(H65)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C15(H15A,H15B), C16(H16A,H16B), C24(H24A,H24B),
 C24(H24C,H24D), C28(H28A,H28B), C33(H33A,H33B), C72(H72A,H72B), C36(H36A,H36B),
  C40(H40A,H40B), C42(H42A,H42B), C43(H43A,H43B), C48(H48A,H48B), C51(H51A,
 H51B), C55(H55A,H55B), C63(H63A,H63B), C66(H66A,H66B), C68(H68A,H68B),
 C70(H70A,H70B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C25(H25), C27(H27),
  C30(H30), C32(H32), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78),
 C53(H53), C60(H60)
6.d Fitted hexagon refined as free rotating group:
 C4(C5,C6,C7,C8,C9)
6.e Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), C29(H29A,H29C,H29B), C31(H31B,H31C,
 H31A), C71(H71A,H71B,H71C)
;
_shelx_res_checksum              7843
_shelx_hkl_checksum              18666
_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 1.691
_oxdiff_exptl_absorpt_empirical_full_min 0.531