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_1567111
_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         'C59 H55 Ag5 N17, 3(C F3 O3 S)'
_chemical_formula_sum            'C62 H55 Ag5 F9 N17 O9 S3'
_chemical_formula_weight         1988.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-12-15 deposited with the CCDC.	2022-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 129.9700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.1353(5)
_cell_length_b                   21.9159(4)
_cell_length_c                   25.6721(3)
_cell_measurement_reflns_used    17073
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      71.3320
_cell_measurement_theta_min      4.2140
_cell_volume                     16443.4(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.969
_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    -64.00  26.00   1.00    6.00    --  -40.81  38.00  90.00   90
  2  \w    -65.00  29.00   1.00    6.00    --  -40.81  38.00-150.00   94
  3  \w     13.00  58.00   1.00    6.00    --   40.81 -99.00 -60.00   45
  4  \w     25.00 124.00   1.00   30.00    --  100.91 -77.00-120.00   99
  5  \w     69.00 120.00   1.00   30.00    --  100.91  77.00  90.00   51
  6  \w     92.00 173.00   1.00   30.00    --  100.91  45.00  60.00   81
  7  \w     79.00 170.00   1.00   30.00    --  100.91  61.00   0.00   91
  8  \w    152.00 177.00   1.00   30.00    --  100.91  77.00  90.00   25
  9  \w     78.00 137.00   1.00   30.00    --  100.91  61.00 -60.00   59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0559444000
_diffrn_orient_matrix_UB_12      -0.0235653000
_diffrn_orient_matrix_UB_13      -0.0098020000
_diffrn_orient_matrix_UB_21      -0.0217786000
_diffrn_orient_matrix_UB_22      0.0624557000
_diffrn_orient_matrix_UB_23      0.0138908000
_diffrn_orient_matrix_UB_31      0.0023800000
_diffrn_orient_matrix_UB_32      0.0220714000
_diffrn_orient_matrix_UB_33      -0.0498633000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            31666
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.438
_diffrn_reflns_theta_min         3.971
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.785
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       block
_exptl_crystal_F_000             7856
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.672
_refine_diff_density_min         -1.373
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     974
_refine_ls_number_reflns         15519
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0969P)^2^+84.9287P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1625
_refine_ls_wR_factor_ref         0.1656
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14304
_reflns_number_total             15519
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00989g2.cif
_cod_data_source_block           y_sq
_cod_depositor_comments
'Adding full bibliography for 1567108--1567115.cif.'
_cod_database_code               1567111
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.412
_shelx_estimated_absorpt_t_min   0.159
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_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. Restrained distances
 C9-C10
 1.4 with sigma of 0.02
 C10-C5
 1.4 with sigma of 0.02
 C9-C17
 1.4 with sigma of 0.02
 C17-C6
 1.4 with sigma of 0.02
3. Rigid bond restraints
 C9, C5, C17, C6, C10, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C136
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C4 \\sim C6 \\sim C17 \\sim C9 \\sim C10 \\sim C5: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(S7A)=1-FVAR(1)
 Sof(S7)=FVAR(1)
 Sof(F5A)=1-FVAR(2)
 Sof(F5)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C33(H33), C36(H36), C38(H38), C56(H56), C57(H57), C63(H63), C64(H64),
 C70(H70), C72(H72), C75(H75), C86(H86), C89(H89), C93(H93), C125(H125), C1(H1),
  C145(H145), C4AA(H4AA), C6AA(H6AA), C7AA(H7AA), C13(H13), C5AA(H5AA),
 C2AA(H2AA), C20(H20), C5BA(H5BA), C8BA(H8BA), C7BA(H7BA), C5(H5), C6(H6),
 C9(H9), C10(H10), C17(H17)
6.b Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C68(H68A,H68B,H68C), C127(H12A,H12B,H12C), C19(H19A,H19B,
 H19C), C24(H24A,H24B,H24C), C9AA(H9AA,H9AB,H9AC), C8(H8A,H8B,H8C), C18(H18A,
 H18B,H18C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              62277
_shelx_fab_checksum              30011
_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 2.070
_oxdiff_exptl_absorpt_empirical_full_min 0.719