Atom-precise Modification of Silver(I) Thiolate Cluster by Shell Ligand Substitution: A New Approach to Generation of Cluster Functionality and Chirality.
Li, Si; Du, Xiang-Sha; Li, Bing; Wang, Jia-Yin; Li, Guo-Ping; Gao, Guang-Gang; Zang, Shuang-Quan; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b12136

data_4126971
_publ_section_title
;
 Atom-precise Modification of Silver(I) Thiolate Cluster by Shell Ligand
 Substitution: A New Approach to Generation of Cluster Functionality and
 Chirality.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b12136
_journal_year                    2017
_chemical_formula_moiety         'C105 H148 Ag20 N2 O21 S10, 2(C2 H3 N)'
_chemical_formula_sum            'C109 H154 Ag20 N4 O21 S10'
_chemical_formula_weight         4334.35
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                68.069(2)
_cell_angle_beta                 76.262(2)
_cell_angle_gamma                76.778(2)
_cell_formula_units_Z            1
_cell_length_a                   13.3254(2)
_cell_length_b                   17.0097(3)
_cell_length_c                   17.0989(3)
_cell_measurement_reflns_used    20829
_cell_measurement_temperature    220.00(10)
_cell_measurement_theta_max      73.8030
_cell_measurement_theta_min      4.0860
_cell_volume                     3449.91(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7b (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      220.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.993
_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    -19.00  22.00   0.50    0.50    --    0.00  38.00  90.00   82
  2  \w    -83.00  16.00   0.50    0.50    --    0.00 -57.00-150.00  198
  3  \w    -18.00  50.00   0.50    0.50    --    0.00  19.00-150.00  136
  4  \w     56.00  87.00   0.50    0.50    --    0.00  38.00  90.00   62
  5  \w     82.00 185.00   0.50    1.20    --   95.20  30.00 -30.00  206
  6  \w      7.00 108.00   0.50    1.20    --   95.20 -82.00  90.00  202
  7  \w     32.00 123.00   0.50    1.20    --   95.20 -82.00 -30.00  182
  8  \w     85.00 111.00   0.50    1.20    --   95.20 -30.00   0.00   52
  9  \w     78.00 185.00   0.50    1.20    --   95.20  30.00 -60.00  214
 10  \w     10.00  88.00   0.50    1.20    --   95.20 -61.00  90.00  156
 11  \w     76.00 184.00   0.50    1.20    --   95.20  15.00  60.00  216
 12  \w     48.00 127.00   0.50    1.20    --   95.20 -82.00-180.00  158
 13  \w     10.00  63.00   0.50    1.20    --   95.20 -30.00   0.00  106
 14  \w     18.00 120.00   0.50    1.20    --   95.20 -61.00-180.00  204
 15  \w     16.00 107.00   0.50    1.20    --   95.20 -61.00 -30.00  182
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0658041000
_diffrn_orient_matrix_UB_12      0.0901833000
_diffrn_orient_matrix_UB_13      -0.0225171000
_diffrn_orient_matrix_UB_21      -0.0241346000
_diffrn_orient_matrix_UB_22      -0.0081944000
_diffrn_orient_matrix_UB_23      0.0951628000
_diffrn_orient_matrix_UB_31      0.0979948000
_diffrn_orient_matrix_UB_32      0.0396852000
_diffrn_orient_matrix_UB_33      -0.0121056000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_Laue_measured_fraction_full 0.933
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28927
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         64.995
_diffrn_reflns_theta_min         3.259
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    24.078
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.086
_exptl_crystal_description       block
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.156
_refine_diff_density_min         -2.382
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     802
_refine_ls_number_reflns         11656
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0798
_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^)+(0.0381P)^2^+114.8201P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2014
_refine_ls_wR_factor_ref         0.2024
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11106
_reflns_number_total             11656
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b12136_si_003.cif
_cod_data_source_block           222
_cod_original_cell_volume        3449.92(12)
_cod_database_code               4126971
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 98.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C30, C33
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Ag10 \\sim Ag8: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Ag9A \\sim Ag9B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Ag8A \\sim Ag8B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C1 \\sim O1 \\sim O2: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(C47) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C54) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C52)
\\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C50) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C33) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(Ag9B)=1-FVAR(1)
 Sof(Ag9A)=FVAR(1)
 Sof(Ag8)=1-FVAR(2)
 Sof(Ag10)=FVAR(2)
 Sof(Ag8B)=1-FVAR(3)
 Sof(Ag8A)=FVAR(3)
 Fixed Sof: O1(0.5) O3(0.5) O2(0.5)
5.a Riding coordinates:
 C33(H33a,H33b,H33c)
5.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C4(H4), C25(H25), C26(H26), C18(H18), C22(H22), C8(H8), C7(H7),
 C28(H28), C21(H21), C6(H6), C14(H14), C12(H12), C20(H20), C27(H27), C11(H11),
 C19(H19), C15(H15), C13(H13), C5(H5)
5.c Idealised Me refined as rotating group:
 C43(H43a,H43b,H43c), C45(H45a,H45b,H45c), C35(H35a,H35b,H35c), C44(H44a,H44b,
 H44c), C40(H40a,H40b,H40c), C39(H39a,H39b,H39c), C37(H37a,H37b,H37c), C41(H41a,
 H41b,H41c), C49(H49a,H49b,H49c), C36(H36a,H36b,H36c), C31(H31a,H31b,H31c),
 C48(H48a,H48b,H48c), C47(H47a,H47b,H47c), C51(H51a,H51b,H51c), C52(H52a,H52b,
 H52c), C53(H53a,H53b,H53c), C32(H32a,H32b,H32c), C55(H55a,H55b,H55c)
;
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.987
_oxdiff_exptl_absorpt_empirical_full_min 0.661