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_1567114
_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), C16 H22 N2'
_chemical_formula_sum            'C18 H22 F6 N2 O6 S2'
_chemical_formula_weight         540.51
_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_Int_Tables_number      2
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-02-03 deposited with the CCDC.	2022-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                85.714(2)
_cell_angle_beta                 87.099(3)
_cell_angle_gamma                87.475(3)
_cell_formula_units_Z            3
_cell_length_a                   9.0344(3)
_cell_length_b                   12.9270(4)
_cell_length_c                   15.4280(5)
_cell_measurement_reflns_used    7752
_cell_measurement_temperature    173
_cell_measurement_theta_max      65.1340
_cell_measurement_theta_min      4.2830
_cell_volume                     1792.99(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.9824
_diffrn_measured_fraction_theta_max 0.9824
_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    -70.00  31.00   1.00    1.00    --  -42.06  57.00 120.00  101
  2  \w   -115.00 -14.00   1.00    1.00    --  -42.06 -57.00 -30.00  101
  3  \w    -87.00  -6.00   1.00    1.00    --  -42.06 125.00-150.00   81
  4  \w    103.00 166.00   1.00    1.00    --   89.35  77.00-120.00   63
  5  \w     97.00 163.00   1.00    1.00    --   89.35 125.00-180.00   66
  6  \w      8.00 142.00   1.00    1.00    --   89.35 -15.00-150.00  134
  7  \w    103.00 166.00   1.00    1.00    --   89.35  77.00-180.00   63
  8  \w     17.00 118.00   1.00    1.00    --   89.35 -61.00-120.00  101
  9  \w     27.00 112.00   1.00    1.00    --   89.35-125.00-180.00   85
 10  \w     97.00 163.00   1.00    1.00    --   89.35 125.00-150.00   66
 11  \w     13.00 122.00   1.00    1.00    --   89.35 -77.00 150.00  109
 12  \w     27.00 112.00   1.00    1.00    --   89.35-125.00 -30.00   85
 13  \w     27.00 112.00   1.00    1.00    --   89.35-125.00  60.00   85
 14  \w     13.00 118.00   1.00    1.00    --   89.35 -30.00 120.00  105
 15  \w   -115.00 -14.00   1.00    1.00    --  -42.06 -57.00-150.00  101
 16  \w   -115.00 -74.00   1.00    1.00    --  -42.06 -57.00 -90.00   41
 17  \w   -115.00 -14.00   1.00    1.00    --  -42.06 -57.00  90.00  101
;
_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      -0.0011007000
_diffrn_orient_matrix_UB_12      0.0918926000
_diffrn_orient_matrix_UB_13      -0.0695915000
_diffrn_orient_matrix_UB_21      -0.1415712000
_diffrn_orient_matrix_UB_22      -0.0392898000
_diffrn_orient_matrix_UB_23      -0.0359857000
_diffrn_orient_matrix_UB_31      -0.0956890000
_diffrn_orient_matrix_UB_32      0.0657090000
_diffrn_orient_matrix_UB_33      0.0625439000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17157
_diffrn_reflns_theta_full        65.2307
_diffrn_reflns_theta_max         65.23
_diffrn_reflns_theta_min         3.43
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.799
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.5016
_exptl_crystal_description       block
_exptl_crystal_F_000             839.4592
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.9051
_refine_diff_density_min         -0.5638
_refine_diff_density_rms         0.0733
_refine_ls_d_res_high            0.8490
_refine_ls_d_res_low             12.8803
_refine_ls_goodness_of_fit_ref   1.0569
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    54
_refine_ls_number_parameters     463
_refine_ls_number_reflns         6033
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0569
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+2.0130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1682
_refine_ls_wR_factor_ref         0.1791
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                4852
_reflns_number_total             6033
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2sc00989g2.cif
_cod_data_source_block           20201105-Pr-coupling
_cod_depositor_comments
'Adding full bibliography for 1567108--1567115.cif.'
_cod_database_code               1567114
_chemical_oxdiff_formula         CHONSF
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00V(H00b,H00c), C00X(H00d,H00e), C011(H01a,H01b), C015(H01m,H01n), C016(H01c,
 H01d), C018(H01e,H01f)
2.b Aromatic/amide H refined with riding coordinates:
 N007(H007), N009(H009), N00A(H00A), C00I(H00I), C00J(H00J), C00L(H00L),
 C00O(H00O), C00Q(H00Q), C00R(H00R), C00S(H00S), C00Y(H00Y), C00Z(H00Z)
2.c Idealised Me refined as rotating group:
 C01B(H01o,H01p,H01q), C01E(H01g,H01h,H01i), C01F(H01j,H01k,H01l)
;
_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 1.407
_oxdiff_exptl_absorpt_empirical_full_min 0.639