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_1567113
_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         'C55 H53 Ag5 F3 N17 O3 S, 2(C F3 O3 S)'
_chemical_formula_sum            'C57 H53 Ag5 F9 N17 O9 S3'
_chemical_formula_weight         1926.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 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                 91.174(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.7535(5)
_cell_length_b                   24.5293(6)
_cell_length_c                   24.9163(4)
_cell_measurement_reflns_used    10929
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      70.8510
_cell_measurement_theta_min      4.2730
_cell_volume                     15736.7(6)
_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  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.966
_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    -72.00  19.00   1.00    5.00    --  -40.81  77.00-180.00   91
  2  \w   -114.00 -18.00   1.00    5.00    --  -40.81 -38.00-150.00   96
  3  \w     24.00  63.00   1.00    5.00    --   40.81-125.00  90.00   39
  4  \w     30.00  95.00   1.00   16.00    --  100.91 -95.00 -60.00   65
  5  \w    106.00 172.00   1.00   16.00    --  100.91 125.00-180.00   66
  6  \w     78.00 118.00   1.00   16.00    --  100.91-125.00  30.00   40
  7  \w     79.00 158.00   1.00   16.00    --  100.91  61.00-180.00   79
  8  \w     76.00 167.00   1.00   16.00    --  100.91  61.00-120.00   91
  9  \w     52.00 129.00   1.00   16.00    --  100.91 -61.00  90.00   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30754
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.599
_diffrn_reflns_theta_min         3.604
_exptl_absorpt_coefficient_mu    11.246
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40429
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_description       cylinder
_exptl_crystal_F_000             7600
_exptl_crystal_size_length       0.300
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_exptl_crystal_size_rad          0.060
_refine_diff_density_max         1.802
_refine_diff_density_min         -1.672
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     920
_refine_ls_number_reflns         14867
_refine_ls_number_restraints     380
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0728
_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^)+(0.1074P)^2^+199.4885P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1979
_refine_ls_wR_factor_ref         0.2182
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11488
_reflns_number_total             14867
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00989g2.cif
_cod_data_source_block           lcc-ca36_sq
_cod_depositor_comments
'Adding full bibliography for 1567108--1567115.cif.'
_cod_database_code               1567113
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.806
_shelx_estimated_absorpt_t_min   0.071
_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
 N-C31
 2.42 with sigma of 0.02
 C02F-C31
 2.6 with sigma of 0.02
 C31-N
 2.6 with sigma of 0.02
 C31-C02F
 2.4 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(F020) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F17A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F16A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F17A) \\sim Ueq, Uanis(F16A) \\sim Ueq, Uanis(F02U) \\sim Ueq,
Uanis(O01Y) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(S009)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(Ag)=1-FVAR(1)
 Sof(Ag04)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C00Z(H00Z), C012(H012), C013(H013), C016(H016), C019(H019), C01G(H01G),
 C01L(H01L), C01N(H01N), C01P(H01P), C01Q(H01Q), C01R(H01R), C01U(H01U),
 C01V(H01V), C01Z(H01Z), C021(H021), C023(H023), C024(H024), C026(H026),
 C027(H027), C028(H028), C02B(H02G), C02D(H02H), C02F(H02I), C02G(H02J),
 C02H(H02K), C02K(H02O)
6.b Idealised Me refined as rotating group:
 C01K(H01A,H01B,H01C), C01W(H01D,H01E,H01F), C025(H02A,H02B,H02C), C02A(H02D,
 H02E,H02F), C02J(H02L,H02M,H02N), C02L(H02P,H02Q,H02R), C02M(H02S,H02T,H02U),
 C02O(H02V,H02W,H02X), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              1932
_shelx_fab_checksum              25249
_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
;