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_7708474
_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
'C40 H84 Ag12 N4 O24 S14, C36 H36 N24 O12, 4(C3 H7 N O)'
_chemical_formula_sum            'C88 H148 Ag12 N32 O40 S14'
_chemical_formula_weight         4037.66
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-03
_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                79.5070(10)
_cell_angle_beta                 80.7700(10)
_cell_angle_gamma                79.2250(10)
_cell_formula_units_Z            1
_cell_length_a                   13.9198(2)
_cell_length_b                   14.8144(2)
_cell_length_c                   18.0353(2)
_cell_measurement_reflns_used    20240
_cell_measurement_temperature    199.99(10)
_cell_measurement_theta_max      72.6450
_cell_measurement_theta_min      3.3380
_cell_volume                     3561.59(8)
_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 0.993
_diffrn_measured_fraction_theta_max 0.966
_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     43.00  75.00   0.50    1.14    --    0.00  57.00  60.00   64
  2  \w      0.00  87.00   0.50    1.14    --    0.00  77.00  90.00  174
  3  \w      1.00  79.00   0.50    1.14    --    0.00  38.00-180.00  156
  4  \w    -28.00  35.00   0.50    1.14    --    0.00  57.00  60.00  126
  5  \w    -69.00  29.00   0.50    1.14    --    0.00 -38.00-180.00  196
  6  \w      8.00 127.00   0.50    4.56    --   97.60 -61.00-120.00  238
  7  \w      8.00 124.00   0.50    4.56    --   97.60 -61.00  60.00  232
  8  \w     27.00 133.00   0.50    4.56    --   97.60 -82.00  60.00  212
  9  \w     20.00 106.00   0.50    4.56    --   97.60 -82.00   0.00  172
 10  \w    130.00 156.00   0.50    4.56    --   97.60  77.00-150.00   52
 11  \w      9.00 158.00   0.50    4.56    --   97.60 -15.00-120.00  298
 12  \w     63.00 102.00   0.50    4.56    --   97.60  77.00-150.00   78
 13  \w     38.00  87.00   0.50    4.56    --   97.60  15.00 120.00   98
 14  \w    104.00 187.00   0.50    4.56    --   97.60  15.00 120.00  166
 15  \w     96.00 123.00   0.50    4.56    --   97.60 -82.00 -90.00   54
 16  \w     20.00  46.00   0.50    4.56    --   97.60 -82.00 -90.00   52
 17  \w     16.00  70.00   0.50    4.56    --   97.60 -82.00-180.00  108
 18  \w     89.00 120.00   0.50    4.56    --   97.60 -82.00-180.00   62
 19  \w     13.00 131.00   0.50    4.56    --   97.60 -82.00-120.00  236
 20  \w     84.00 120.00   0.50    4.56    --   97.60 -82.00 120.00   72
 21  \w     77.00 103.00   0.50    4.56    --   97.60 -61.00 -30.00   52
 22  \w     84.00 109.00   0.50    4.56    --   97.60 -82.00 -30.00   50
 23  \w     17.00 155.00   0.50    4.56    --   97.60 -15.00  30.00  276
;
_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      -0.0287784000
_diffrn_orient_matrix_UB_12      0.0079491000
_diffrn_orient_matrix_UB_13      0.0849590000
_diffrn_orient_matrix_UB_21      -0.0571674000
_diffrn_orient_matrix_UB_22      0.0985625000
_diffrn_orient_matrix_UB_23      -0.0214322000
_diffrn_orient_matrix_UB_31      -0.0938990000
_diffrn_orient_matrix_UB_32      -0.0413615000
_diffrn_orient_matrix_UB_33      0.0008817000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37672
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.303
_diffrn_reflns_theta_min         2.513
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.546
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56220
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.883
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.320
_refine_diff_density_min         -1.159
_refine_diff_density_rms         0.184
_refine_ls_extinction_coef       0.00036(4)
_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   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     956
_refine_ls_number_reflns         13836
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0631
_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^)+(0.0963P)^2^+15.8741P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1750
_refine_ls_wR_factor_ref         0.1808
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11938
_reflns_number_total             13836
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02505h2.cif
_cod_data_source_block           SCM_3
_cod_database_code               7708474
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H O F N P Ag'
_shelx_estimated_absorpt_t_max   0.746
_shelx_estimated_absorpt_t_min   0.653
_reflns_odcompleteness_completeness 96.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     73.15
_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
 N17-C48 \\sim N17-C49
 with sigma of 0.01
 N16-C45 \\sim N16-C44
 with sigma of 0.01
 N15-C43 \\sim N15-C42
 with sigma of 0.01
3. Rigid bond restraints
 O14, S7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C2 \\sim C13 \\sim C20 \\sim C22: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
O5 \\sim O10 \\sim O12 \\sim O13 \\sim O14: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O11) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Sof(Ag7)=1-FVAR(1)
 Sof(Ag6)=FVAR(1)
 Sof(Ag8)=1-FVAR(2)
 Sof(Ag5)=FVAR(2)
 Fixed Sof: C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C20(0.75) H20A(0.75)
 H20B(0.75) H20C(0.75) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C22(0.25)
 H22A(0.25) H22B(0.25) H22C(0.25) O10(0.75) O12(0.75) O13(0.25) O14(0.25)
 C44(0.5) H44(0.5) C45(0.5) H45A(0.5) H45B(0.5) H45C(0.5) C46(0.5) H46A(0.5)
 H46B(0.5) H46C(0.5) N16(0.5) O22(0.5) C47(0.5) H47(0.5) C48(0.5) H48A(0.5)
 H48B(0.5) H48C(0.5) C49(0.5) H49A(0.5) H49B(0.5) H49C(0.5) N17(0.5) O23(0.5)
6.a Riding coordinates:
 C21(H21A,H21B,H21C), C45(H45A,H45B,H45C)
6.b Ternary CH refined with riding coordinates:
 C1(H1), C5(H5), C27(H27), C30(H30), C31(H31), C32(H32), C38(H38), C40(H40)
6.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B), C28(H28A,H28B), C29(H29A,H29B),
 C33(H33A,H33B), C36(H36A,H36B), C37(H37A,H37B), C39(H39A,H39B)
6.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C10(H10), C16(H16), C41(H41), C44(H44), C47(H47)
6.e Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,
 H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C),
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C46(H46A,H46B,H46C), C48(H48A,H48B,
 H48C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              59996
_shelx_hkl_checksum              85985
_shelx_fab_checksum              59240
_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 1.836
_oxdiff_exptl_absorpt_empirical_full_min 0.275