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_1567115
_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         'C72 H48 Ag13 F18 N6 O18 S6'
_chemical_formula_sum            'C72 H48 Ag13 F18 N6 O18 S6'
_chemical_formula_weight         3221.83
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-11-04
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.1557(9)
_cell_length_b                   30.2077(17)
_cell_length_c                   58.888(4)
_cell_measurement_reflns_used    9521
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.67
_cell_measurement_theta_min      2.24
_cell_volume                     28739(3)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0882
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       77
_diffrn_reflns_limit_l_min       -78
_diffrn_reflns_number            70758
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.181
_diffrn_reflns_theta_min         1.383
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.881
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       plate
_exptl_crystal_F_000             12280
_platon_squeeze_details
;
TITL 1_a.res in Fddd
CELL   16.1557   30.2077   58.8880     90.00     90.00     90.00
SPGR Fddd
C101 0.340 0.476 0.376 !       4.15 eA-3
Q102 0.451 0.216 0.344 !       3.57 eA-3
C103 0.792 0.235 0.056 !       3.53 eA-3
Q104 0.277 0.234 0.055 !       3.49 eA-3
C105 0.715 0.263 0.085 !       3.48 eA-3
Q106 0.519 0.282 0.090 !       3.38 eA-3
Q107 0.453 0.219 0.055 !       3.36 eA-3
Q108 0.934 0.227 0.125 !       3.17 eA-3
Q109 0.817 0.375 0.375 !       3.06 eA-3
C110 0.298 0.237 0.431 !       2.96 eA-3
C111 0.319 0.423 0.271 !       2.92 eA-3
Q112 0.514 0.274 0.375 !       2.69 eA-3
Q113 0.646 0.336 0.195 !       2.63 eA-3
Q114 0.419 0.124 0.054 !       2.50 eA-3
Q115 0.361 0.468 0.160 !       2.49 eA-3
C116 0.676 0.240 0.101 !       2.43 eA-3
Q117 0.254 0.186 0.089 !       2.39 eA-3
C118 0.589 0.267 0.168 !       2.39 eA-3
Q119 0.115 0.064 0.087 !       2.39 eA-3
Q120 0.117 0.014 0.195 !       2.39 eA-3
Q121 0.892 0.125 0.125 !       2.38 eA-3
Q122 0.044 0.279 0.161 !       2.37 eA-3
C123 0.625 0.195 0.126 !       2.33 eA-3
Q124 0.395 0.163 0.075 !       2.32 eA-3
Q125 0.968 0.079 0.161 !       2.24 eA-3
Q126 0.728 0.171 0.231 !       2.20 eA-3
Q127 0.850 0.264 0.238 !       2.20 eA-3
Q128 0.826 0.288 0.246 !       2.19 eA-3
Q129 0.554 0.381 0.161 !       2.18 eA-3
Q130 0.417 0.024 0.125 !       2.17 eA-3
Q131 0.798 0.150 0.220 !       2.17 eA-3
Q132 0.168 0.164 0.165 !       2.11 eA-3
C133 0.481 0.265 0.195 !       2.10 eA-3
Q134 0.894 0.283 0.226 !       2.10 eA-3
C135 0.353 0.266 0.239 !       2.05 eA-3
Q136 0.958 0.221 0.054 !       2.04 eA-3
Q137 0.034 0.459 0.235 !       2.01 eA-3
Q138 0.014 0.284 0.090 !       2.00 eA-3
Q139 0.606 0.225 0.059 !       1.99 eA-3
Q140 0.259 0.470 0.163 !       1.99 eA-3
Q141 0.607 0.421 0.266 !       1.96 eA-3
Q142 0.348 0.382 0.446 !       1.93 eA-3
Q143 0.343 0.028 0.044 !       1.93 eA-3
C144 0.333 0.036 0.027 !       1.92 eA-3
Q145 0.016 0.186 0.449 !       1.91 eA-3
Q146 0.154 0.117 0.055 !       1.88 eA-3
C147 0.475 0.140 0.269 !       1.88 eA-3
Q148 0.529 0.032 0.407 !       1.86 eA-3
Q149 0.488 0.126 0.050 !       1.86 eA-3
Q150 0.827 0.490 0.237 !       1.85 eA-3
Q151 0.941 0.439 0.051 !       1.85 eA-3
Q152 0.752 0.739 0.257 !       1.85 eA-3
Q153 0.752 0.239 0.757 !       1.85 eA-3
Q154 0.252 0.239 0.257 !       1.85 eA-3
Q155 0.248 0.261 0.743 !       1.85 eA-3
Q156 0.795 0.140 0.126 !       1.85 eA-3
Q157 0.997 0.289 0.237 !       1.84 eA-3
Q158 0.718 0.274 0.256 !       1.82 eA-3
Q159 0.903 0.162 0.446 !       1.82 eA-3
C160 0.881 0.062 0.444 !       1.80 eA-3
C161 0.477 0.352 0.246 !       1.80 eA-3
C162 0.396 0.484 0.255 !       1.80 eA-3
Q163 1.001 0.045 0.255 !       1.79 eA-3
Q164 0.010 0.375 0.305 !       1.78 eA-3
Q165 0.264 0.037 0.481 !       1.78 eA-3
Q166 0.569 0.327 0.200 !       1.77 eA-3
Q167 0.695 0.086 0.445 !       1.77 eA-3
C168 0.311 0.477 0.309 !       1.77 eA-3
Q169 0.465 0.272 0.005 !       1.76 eA-3
Q170 0.092 0.086 0.454 !       1.74 eA-3
Q171 0.089 0.468 0.160 !       1.73 eA-3
C172 0.168 0.392 0.235 !       1.69 eA-3
Q173 0.688 0.468 0.226 !       1.68 eA-3
C174 0.629 0.251 0.195 !       1.67 eA-3
C175 0.403 0.438 0.268 !       1.66 eA-3
C176 0.068 0.483 0.237 !       1.65 eA-3
Q177 0.330 0.330 0.406 !       1.65 eA-3
Q178 0.533 0.485 0.012 !       1.65 eA-3
Q179 0.827 0.460 0.015 !       1.65 eA-3
C180 0.231 0.180 0.497 !       1.63 eA-3
C181 0.275 0.157 0.488 !       1.63 eA-3
C182 0.133 0.469 0.196 !       1.63 eA-3
Q183 0.227 0.360 0.090 !       1.63 eA-3
Q184 0.268 0.066 0.045 !       1.62 eA-3
Q185 0.391 0.171 0.090 !       1.62 eA-3
Q186 0.554 0.095 0.159 !       1.61 eA-3
Q187 0.581 0.110 0.056 !       1.60 eA-3
Q188 0.557 0.383 0.016 !       1.60 eA-3
Q189 0.347 0.085 0.493 !       1.58 eA-3
Q190 0.007 0.235 0.486 !       1.58 eA-3
Q191 0.247 0.493 0.997 !       1.57 eA-3
Q192 0.738 0.312 0.050 !       1.57 eA-3
Q193 0.189 0.461 0.298 !       1.55 eA-3
C194 0.227 0.503 0.285 !       1.55 eA-3
C195 0.179 0.170 0.494 !       1.54 eA-3
C196 0.660 0.149 0.011 !       1.53 eA-3
Q197 0.414 0.103 0.152 !       1.53 eA-3
Q198 0.079 0.350 0.169 !       1.53 eA-3
Q199 0.851 0.466 0.160 !       1.52 eA-3
;
_refine_diff_density_max         2.883
_refine_diff_density_min         -2.824
_refine_diff_density_rms         0.485
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         8802
_refine_ls_number_restraints     501
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1873
_refine_ls_R_factor_gt           0.1340
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1489P)^2^+7230.0088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3601
_refine_ls_wR_factor_ref         0.4086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5651
_reflns_number_total             8802
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00989g2.cif
_cod_data_source_block           1_sq
_cod_depositor_comments
'Adding full bibliography for 1567108--1567115.cif.'
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               1567115
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Shared sites
{C00R, N00R}
3. Restrained distances
 H00R-N00R
 0.9 with sigma of 0.02
 C00F-H00R_$1
 3.7 with sigma of 0.02
 O1-S1 = O1-S2
 1.44 with sigma of 0.02
 S1-O2 = S1-O3 = S2-O4 = S2-O5
 1.4 with sigma of 0.02
 C1-F1 = C1-F2 = C1-F3 = C2-F4 = C2-F5 = C2-F6
 1.2 with sigma of 0.02
 C1-S1 = C2-S2
 1.8 with sigma of 0.02
 S2-F4 = S2-F5 = S2-F6 = S1-F3 = S1-F2 = S1-F1
 2.4 with sigma of 0.02
 O1-O2 \\sim O1-O3 \\sim O1-O4 \\sim O1-O5 \\sim O2-O3 \\sim O4-O5
 with sigma of 0.02
 C2-O4 \\sim C2-O5 \\sim C1-O2 \\sim C1-O3 \\sim C1-O1 \\sim C2-O1
 with sigma of 0.02
 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F4-F5 \\sim F5-F6 \\sim F6-F4
 with sigma of 0.02
4. Rigid bond restraints
 C4, C3, C7, C15, C5, C0AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C00H, C00X, C00Q, C00G, C00Y, C00T
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4, F5, F4, F6, C2, S2, O1, C1, F3, F2, F1, O5, S1, O3, O2
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.04
5. Uiso/Uaniso restraints and constraints
O4 \\sim F5 \\sim F4 \\sim F6 \\sim C2 \\sim S2 \\sim O1 \\sim C1 \\sim F3
\\sim F2 \\sim F1 \\sim O5 \\sim S1 \\sim O3 \\sim O2: within 2A with sigma of
0.4 and sigma for terminal atoms of 0.8
C4 \\sim C3 \\sim C7 \\sim C15 \\sim C5 \\sim C0AA: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C00H \\sim C00X \\sim C00Q \\sim C00G \\sim C00Y \\sim C00T: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C00G) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F4)
\\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(S2) \\sim Ueq,
Uanis(O1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F2) \\sim
Ueq, Uanis(F1) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(S1) \\sim Ueq, Uanis(O3)
\\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.08 and sigma for terminal atoms
of 0.16
Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O4) \\sim Ueq, Uanis(F6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C00R) = Uanis(N00R)
6. Others
 Fixed Sof: H00E(0.5) H00A(0.5) O1(0.5) C00R(0.5) C4(0.5) C0AA(0.5) H0AA(0.5)
 C5(0.5) H5(0.5) C15(0.5) H15(0.5) C7(0.5) H7(0.5) C3(0.5) H3(0.5) N00R(0.5)
 H00R(0.5) S1(0.33333) S2(0.16667) O3(0.33333) F4(0.16667) O2(0.33333)
 F3(0.33333) F2(0.33333) O5(0.16667) O4(0.16667) F5(0.16667) F6(0.16667)
 F1(0.33333) C2(0.16667) C1(0.33333)
 Fixed Uiso: H00R(0.05)
 Fixed X: H00R(0.83492)
 Fixed Y: H00R(0.41299)
 Fixed Z: H00R(0.489659)
7.a Aromatic/amide H refined with riding coordinates:
 N009(H009), C00E(H00E), C00E(H00A), C00T(H00T), C00Y(H00Y), C00G(H00G),
 C00Q(H00Q), C00X(H00X), C00L(H00L), C00M(H00M), C0AA(H0AA), C5(H5), C15(H15),
 C7(H7), C3(H3)
7.b Fitted hexagon refined as free rotating group:
 C00H(C00T,C00Y,C00G,C00Q,C00X), C4(C0AA,C5,C15,C7,C3)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'