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_7708473
_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         'C78 H90 Ag12 N6 O18 S12, 4(H2 O)'
_chemical_formula_sum            'C78 H98 Ag12 N6 O22 S12'
_chemical_formula_weight         3150.78
_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             2021-08-27
_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                 94.1890(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.88620(10)
_cell_length_b                   12.60960(10)
_cell_length_c                   25.3661(2)
_cell_measurement_reflns_used    14409
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      73.4090
_cell_measurement_theta_min      3.5000
_cell_volume                     5067.73(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 0.992
_diffrn_measured_fraction_theta_max 0.965
_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    -82.00 -39.00   0.50    0.50    --    0.00   0.00   0.00   86
  2  \w     50.00  86.00   0.50    0.50    --    0.00  57.00-120.00   72
  3  \w    -18.00  25.00   0.50    0.50    --    0.00  57.00-120.00   86
  4  \w     20.00  66.00   0.50    0.60    --   97.20 -82.00  30.00   92
  5  \w     75.00 138.00   0.50    0.60    --   97.20  82.00 -30.00  126
  6  \w     33.00 119.00   0.50    0.60    --   97.20 -82.00  90.00  172
  7  \w     74.00 174.00   0.50    0.60    --   97.20  45.00 -60.00  200
  8  \w     38.00 115.00   0.50    0.60    --   97.20 -82.00 -30.00  154
  9  \w     28.00 111.00   0.50    0.60    --   97.20 -61.00  90.00  166
 10  \w     70.00 106.00   0.50    0.60    --   97.20 -82.00  30.00   72
 11  \w     85.00 183.00   0.50    0.60    --   97.20  45.00-150.00  196
;
_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      -0.0960799000
_diffrn_orient_matrix_UB_12      0.0158557000
_diffrn_orient_matrix_UB_13      -0.0092839000
_diffrn_orient_matrix_UB_21      -0.0126828000
_diffrn_orient_matrix_UB_22      -0.1211282000
_diffrn_orient_matrix_UB_23      -0.0001923000
_diffrn_orient_matrix_UB_31      -0.0076887000
_diffrn_orient_matrix_UB_32      0.0020796000
_diffrn_orient_matrix_UB_33      0.0601908000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26038
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.765
_diffrn_reflns_theta_min         3.494
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.029
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64438
_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    2.065
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             3080
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.770
_refine_diff_density_min         -1.637
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     825
_refine_ls_number_reflns         9910
_refine_ls_number_restraints     709
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0407P)^2^+4.9308P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0850
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8865
_reflns_number_total             9910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02505h2.cif
_cod_data_source_block           NC_a
_cod_database_code               7708473
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.743
_shelx_estimated_absorpt_t_min   0.571
_reflns_odcompleteness_completeness 99.07
_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
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C8-C4 \\sim C8-C20 \\sim C4-C18 \\sim C25-C18 \\sim C28-C20 \\sim C28-C25
\\sim C49-C4 \\sim C49-C50 ~
 C51-C50 \\sim C51-C52 \\sim C52-C53 \\sim C4-C53
 with sigma of 0.01
 C5-C13 \\sim C5-C32 \\sim C5-C41 \\sim C41-C40 \\sim C39-C32 \\sim C42-C39
\\sim C40-C33 \\sim C33-C30 ~
 C43-C42 \\sim C43-C13 \\sim C30-C13
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O7 \\sim O8 \\sim O9 \\sim O10 \\sim O11 \\sim O12: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C31 \\sim C34 \\sim C35 \\sim C36 \\sim C38 \\sim C44 \\sim C45 \\sim C46 \\sim
C47 \\sim C48: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C39 \\sim C42 \\sim C43: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C4 \\sim C8 \\sim C18 \\sim C20 \\sim C25 \\sim C28 \\sim C49 \\sim C50 \\sim
C51 \\sim C52 \\sim C53: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C13 \\sim C30 \\sim C32 \\sim C33 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim
C43: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C10 \\sim C22 \\sim C23 \\sim C24 \\sim C29 \\sim C54 \\sim C55 \\sim C56 \\sim
C57 \\sim C58: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Ag4 \\sim Ag8: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O15 \\sim O16: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O13 \\sim O14: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(Ag7)=1-FVAR(1)
 Sof(Ag5)=FVAR(1)
 Sof(Ag8)=1-FVAR(2)
 Sof(Ag4)=FVAR(2)
 Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=Sof(C47)=Sof(H47)=
 Sof(C48)=Sof(H48)=Sof(N4)=1-FVAR(3)
 Sof(C31)=Sof(H31)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36)=
 Sof(C38)=Sof(H38)=Sof(N3)=FVAR(3)
 Sof(C49)=Sof(H49)=Sof(C50)=Sof(H50)=Sof(C51)=Sof(H51)=Sof(C52)=Sof(H52)=
 Sof(C53)=Sof(H53)=1-FVAR(4)
 Sof(C8)=Sof(H8)=Sof(C18)=Sof(H18)=Sof(C20)=Sof(H20)=Sof(C25)=Sof(H25)=
 Sof(C28)=Sof(H28)=FVAR(4)
 Sof(C54)=Sof(H54)=Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56)=Sof(C57)=Sof(H57)=
 Sof(C58)=Sof(H58)=1-FVAR(5)
 Sof(C10)=Sof(H10)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=
 Sof(C29)=Sof(H29)=FVAR(5)
 Fixed Sof: H13A(0.5) H13(0.5) C30(0.5) H30(0.5) C32(0.5) H32(0.5) C33(0.5)
 H33(0.5) C39(0.5) H39(0.5) C40(0.5) H40(0.5) C41(0.5) H41(0.5) C42(0.5)
 H42(0.5) C43(0.5) H43(0.5) O7(0.6) O8(0.6) O9(0.6) O10(0.4) O11(0.4) O12(0.4)
 O13(0.75) H13B(0.75) H13C(0.75) O14(0.25) H14D(0.25) H14E(0.25) O15(0.75)
 H15A(0.75) H15B(0.75) O16(0.25) H16A(0.25) H16B(0.25)
5.a Everything fixed:
 O14, H14D, H14E, O16, H16A, H16B
5.b Free rotating group:
 O13(H13B,H13C), O15(H15A,H15B)
5.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B)
5.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13A), C13(H13),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
  C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
 C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54),
  C55(H55), C56(H56), C57(H57), C58(H58)
5.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C19(H19A,H19B,H19C), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              15981
_shelx_hkl_checksum              36437
_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 1.417
_oxdiff_exptl_absorpt_empirical_full_min 0.816