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_1567109
_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         '2(C F3 O3 S), C12 H14 N2'
_chemical_formula_sum            'C14 H14 F6 N2 O6 S2'
_chemical_formula_weight         484.39
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-04-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-07 deposited with the CCDC.	2022-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                77.250(9)
_cell_angle_beta                 88.991(8)
_cell_angle_gamma                75.454(9)
_cell_formula_units_Z            1
_cell_length_a                   6.8729(7)
_cell_length_b                   8.3071(9)
_cell_length_c                   8.8774(8)
_cell_measurement_reflns_used    1313
_cell_measurement_temperature    172.97(10)
_cell_measurement_theta_max      75.5790
_cell_measurement_theta_min      5.0980
_cell_volume                     478.12(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.97(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_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    -71.00  38.00   1.00    1.00    --  -40.56  19.00 150.00  109
  2  \w   -115.00 -34.00   1.00    1.00    --  -40.56 -38.00 -30.00   81
  3  \w      1.00  30.00   1.00    1.00    --   40.56 -99.00-150.00   29
  4  \w     23.00  94.00   1.00    1.00    --   40.56-125.00 -60.00   71
  5  \w     46.00  92.00   1.00    1.00    --   40.56-125.00 150.00   46
  6  \w     40.00  91.00   1.00    1.00    --  111.52 -61.00 150.00   51
  7  \w     82.00 108.00   1.00    1.00    --  111.52  77.00  90.00   26
  8  \w     78.00 144.00   1.00    1.00    --  111.52 -77.00-120.00   66
  9  \w     49.00 112.00   1.00    1.00    --  111.52-125.00 -90.00   63
 10  \w     87.00 174.00   1.00    1.00    --  111.52  45.00 150.00   87
 11  \w     27.00 160.00   1.00    1.00    --  111.52   0.00 120.00  133
 12  \w    130.00 173.00   1.00    1.00    --  111.52  77.00  90.00   43
 13  \w     78.00 118.00   1.00    1.00    --  111.52-125.00  90.00   40
 14  \w     99.00 124.00   1.00    1.00    --  111.52 125.00-180.00   25
 15  \w     42.00  77.00   1.00    1.00    --  111.52-125.00  90.00   35
 16  \w     36.00 128.00   1.00    1.00    --  111.52 -77.00  60.00   92
 17  \w     40.00  79.00   1.00    1.00    --  111.52-125.00 -30.00   39
 18  \w     42.00  69.00   1.00    1.00    --  111.52 -77.00-120.00   27
;
_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      0.1074569000
_diffrn_orient_matrix_UB_12      -0.1856851000
_diffrn_orient_matrix_UB_13      0.0771863000
_diffrn_orient_matrix_UB_21      0.0491345000
_diffrn_orient_matrix_UB_22      0.0581829000
_diffrn_orient_matrix_UB_23      0.1448729000
_diffrn_orient_matrix_UB_31      -0.1993753000
_diffrn_orient_matrix_UB_32      -0.0278046000
_diffrn_orient_matrix_UB_33      0.0690116000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3064
_diffrn_reflns_theta_full        75.83
_diffrn_reflns_theta_max         75.83
_diffrn_reflns_theta_min         5.11
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.423
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cylinder
_exptl_crystal_F_000             246
_exptl_crystal_size_length       0.500
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_exptl_crystal_size_rad          0.070
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0804P)^2^+0.2105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1496
_refine_ls_wR_factor_ref         0.1583
_reflns_number_gt                1659
_reflns_number_total             1908
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d2sc00989g2.cif
_cod_data_source_block           20190421-lcc-ca170-white
_cod_depositor_comments
'Adding full bibliography for 1567108--1567115.cif.'
_cod_original_cell_volume        478.12(8)
_cod_database_code               1567109
_chemical_oxdiff_formula         'C N O H S F Ag '
_chemical_oxdiff_usercomment     'pink needle'
_reflns_odcompleteness_completeness 100.00
_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.a Aromatic/amide H refined with riding coordinates:
 N005(H005), C7(H7), C9(H9), C10(H10)
2.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
;
_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 1.711
_oxdiff_exptl_absorpt_empirical_full_min 0.475