Pyridine dicarbanion-bonded Ag<sub>13</sub> organometallic nanoclusters: synthesis and on-surface oxidative coupling reaction.
Li, Cui-Cui; Zhang, Siqi; Tang, Jian; Jian, Ruijun; Xia, Yu; Zhao, Liang; Chemical science 13 (2022) 8095–8103; doi:10.1039/d2sc00989g

data_1567108
_publ_section_title
;
 Pyridine dicarbanion-bonded Ag<sub>13</sub> organometallic nanoclusters:
 synthesis and on-surface oxidative coupling reaction.
;
_journal_issue                   27
_journal_name_full               'Chemical science'
_journal_page_first              8095
_journal_page_last               8103
_journal_paper_doi               10.1039/d2sc00989g
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C41 H36 Ag13 F15 N6 O15 S5, C F3 O3 S'
_chemical_formula_sum            'C42 H36 Ag13 F18 N6 O18 S6'
_chemical_formula_weight         2849.44
_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   geom
_audit_creation_date             2020-03-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-11 deposited with the CCDC.	2022-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                82.805(4)
_cell_angle_beta                 84.350(3)
_cell_angle_gamma                88.156(4)
_cell_formula_units_Z            2
_cell_length_a                   14.0332(6)
_cell_length_b                   15.3545(7)
_cell_length_c                   22.4180(9)
_cell_measurement_reflns_used    10234
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.5520
_cell_measurement_theta_min      4.3770
_cell_volume                     4768.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.963
_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   -113.00 -16.00   1.00    1.77    --  -40.56 -57.00 -90.00   97
  2  \w    -66.00  28.00   1.00    1.77    --  -40.56  57.00  60.00   94
  3  \w    -51.00  33.00   1.00    1.77    --  -40.56  38.00-150.00   84
  4  \w      5.00  64.00   1.00    1.77    --   40.56 -99.00 120.00   59
  5  \w     26.00  80.00   1.00    1.77    --   40.56 -99.00-150.00   54
  6  \w    108.00 178.00   1.00    7.07    --  107.77  45.00-150.00   70
  7  \w     51.00 114.00   1.00    7.07    --  107.77 -61.00-120.00   63
  8  \w     63.00 132.00   1.00    7.07    --  107.77 -77.00  30.00   69
  9  \w     36.00  78.00   1.00    7.07    --  107.77-125.00  90.00   42
 10  \w    153.00 178.00   1.00    7.07    --  107.77  77.00-120.00   25
 11  \w     80.00 178.00   1.00    7.07    --  107.77  61.00  90.00   98
 12  \w     44.00 118.00   1.00    7.07    --  107.77 -45.00  90.00   74
 13  \w     75.00 132.00   1.00    7.07    --  107.77  77.00-120.00   57
 14  \w     39.00  65.00   1.00    7.07    --  107.77-125.00 -30.00   26
 15  \w     36.00  97.00   1.00    7.07    --  107.77 -45.00 -60.00   61
 16  \w     84.00 118.00   1.00    7.07    --  107.77-125.00 -30.00   34
 17  \w     74.00 101.00   1.00    7.07    --  107.77-125.00  60.00   27
 18  \w     69.00 117.00   1.00    7.07    --  107.77-125.00-120.00   48
 19  \w     26.00  82.00   1.00    7.07    --  107.77 -95.00-120.00   56
 20  \w     93.00 118.00   1.00    7.07    --  107.77-125.00  90.00   25
 21  \w     93.00 178.00   1.00    7.07    --  107.77   0.00-180.00   85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0317193000
_diffrn_orient_matrix_UB_12      -0.0549798000
_diffrn_orient_matrix_UB_13      0.0605833000
_diffrn_orient_matrix_UB_21      -0.0032979000
_diffrn_orient_matrix_UB_22      0.0833757000
_diffrn_orient_matrix_UB_23      0.0319483000
_diffrn_orient_matrix_UB_31      -0.1056291000
_diffrn_orient_matrix_UB_32      0.0160309000
_diffrn_orient_matrix_UB_33      -0.0122694000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0998
_diffrn_reflns_av_unetI/netI     0.1164
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            34811
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.763
_diffrn_reflns_theta_min         3.719
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.889
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light bronze'
_exptl_crystal_density_diffrn    1.985
_exptl_crystal_description       block
_exptl_crystal_F_000             2686
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.796
_refine_diff_density_min         -2.729
_refine_diff_density_rms         0.347
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     922
_refine_ls_number_reflns         18877
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.1665
_refine_ls_R_factor_gt           0.1234
_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^)+(0.2000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3387
_refine_ls_wR_factor_ref         0.3901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10652
_reflns_number_total             18877
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00989g2.cif
_cod_data_source_block           20191113-lcc-acecluster-acetone_sq
_cod_depositor_comments
'Adding full bibliography for 1567108--1567115.cif.'
_cod_database_code               1567108
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H O N S F Ag'
_chemical_oxdiff_usercomment     'C H O N Fe Cl'
_shelx_estimated_absorpt_t_max   0.208
_shelx_estimated_absorpt_t_min   0.055
_reflns_odcompleteness_completeness 99.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.79
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 S00F, C02K, F01R, F02J, F01D
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C73, F42, F32, F47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S00H, C58, F014, F021, F01U
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F02V, C59, F02M, F01T, S00J
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C02K \\sim F01R \\sim F02J \\sim F01D \\sim S00F: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
F42 \\sim C73 \\sim F32 \\sim F47: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
F014 \\sim C58 \\sim F01U \\sim F021 \\sim S00H: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
S00J \\sim C59 \\sim F02V \\sim F01T \\sim F02M: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
4.a Aromatic/amide H refined with riding coordinates:
 N00P(H00P), C025(H025), N01F(H01F), C029(H029), N00R(H00R), N00V(H00V),
 N00Z(H00Z), C010(H010), C018(H018), C01G(H01G), C01H(H01H), C01L(H01L),
 C01P(H01P), N01X(H01X), C022(H022), C027(H027), C02C(H02C), C02F(H02F)
4.b Fitted hexagon refined as free rotating group:
 C00Q(C01B,C025,C02G,N01F,C029)
4.c Idealised Me refined as rotating group:
 C01Q(H01A,H01B,H01C), C02D(H02A,H02B,H02D), C02O(H02E,H02G,H02H), C02R(H02I,
 H02J,H02K), C35(H35A,H35B,H35C), C0AA(H0AA,H0AB,H0AC)
;
_shelx_res_checksum              52490
_shelx_fab_checksum              11771
_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 4.609
_oxdiff_exptl_absorpt_empirical_full_min 0.346