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_1567110
_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         'C48 H50 Ag N16, 3(C F3 O3 S)'
_chemical_formula_sum            'C51 H50 Ag F9 N16 O9 S3'
_chemical_formula_weight         1406.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-05-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-26 deposited with the CCDC.	2022-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.122(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6223(2)
_cell_length_b                   29.4112(4)
_cell_length_c                   17.5734(3)
_cell_measurement_reflns_used    13265
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      73.6380
_cell_measurement_theta_min      4.5690
_cell_volume                     6567.72(19)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_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    'olex2.solve (Bourhis et al., 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 0.970
_diffrn_measured_fraction_theta_max 0.939
_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    -63.00  17.00   1.00    7.50    --  -41.81  38.00   0.00   80
  2  \w    -65.00   9.00   1.00    7.50    --  -41.81  38.00-120.00   74
  3  \w     61.00  94.00   1.00    7.50    --   41.81-125.00-150.00   33
  4  \w      1.00  65.00   1.00    7.50    --   41.81 -77.00 -30.00   64
  5  \w    111.00 175.00   1.00   30.91    --  107.37  77.00  60.00   64
  6  \w     34.00 100.00   1.00   30.91    --  107.37 -95.00 150.00   66
  7  \w    105.00 159.00   1.00   30.91    --  107.37  77.00-180.00   54
  8  \w     28.00  63.00   1.00   30.91    --  107.37 -95.00 120.00   35
  9  \w    103.00 175.00   1.00   30.91    --  107.37  77.00-150.00   72
 10  \w     34.00 116.00   1.00   30.91    --  107.37 -45.00 150.00   82
 11  \w     38.00 104.00   1.00   30.91    --  107.37 -95.00  60.00   66
;
_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      0.1090843000
_diffrn_orient_matrix_UB_12      0.0210638000
_diffrn_orient_matrix_UB_13      0.0456203000
_diffrn_orient_matrix_UB_21      0.0510798000
_diffrn_orient_matrix_UB_22      -0.0472278000
_diffrn_orient_matrix_UB_23      0.0058037000
_diffrn_orient_matrix_UB_31      0.0141831000
_diffrn_orient_matrix_UB_32      0.0083597000
_diffrn_orient_matrix_UB_33      -0.0819273000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26666
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.322
_diffrn_reflns_theta_min         4.038
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.124
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
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    1.422
_exptl_crystal_description       block
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.328
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     810
_refine_ls_number_reflns         12564
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1058P)^2^+5.1946P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1602
_refine_ls_wR_factor_ref         0.1672
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10845
_reflns_number_total             12564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00989g2.cif
_cod_data_source_block           20220419-t-49-rt_auto
_cod_depositor_comments
'Adding full bibliography for 1567108--1567115.cif.'
_cod_database_code               1567110
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H O N Ag S F'
_shelx_estimated_absorpt_t_max   0.734
_shelx_estimated_absorpt_t_min   0.425
_reflns_odcompleteness_completeness 99.87
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
S004 \\sim O029 \\sim O02J \\sim O1: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 N00B(H00B), N00K(H00K), C00O(H00O), C00Z(H00Z), C011(H011), C015(H015),
 C016(H016), C01C(H01M), C01D(H01N), C01E(H01O), C01F(H01P), C01H(H01Q),
 C01I(H01R), C01L(H01S), C01M(H01T), C01N(H01U), C01O(H01V), C01P(H01W),
 C01R(H01X), C01S(H01Y), C01T(H01Z), C01U(H01), C01W(H0AA), C01X(H1AA),
 C01Y(H2AA), C021(H021)
3.b Idealised Me refined as rotating group:
 C010(H01A,H01B,H01C), C018(H01D,H01E,H01F), C019(H01G,H01H,H01I), C01A(H01J,
 H01K,H01L), C01Z(H3AA,H,HA), C022(H02A,H02B,H02C), C023(H02D,H02E,H02F),
 C024(H02G,H02H,H02I)
;
_shelx_res_checksum              23249
_shelx_fab_checksum              38089
_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 1.435
_oxdiff_exptl_absorpt_empirical_full_min 0.613