Monitoring the Growth of Ag-S Clusters through Crystallization of Intermediate Clusters
Nan, Zi-Ang; Xiao, Ying; Liu, Xiyan; Wang, Tan; Cheng, Xiaoling; Yang, Yang; Lei, Zhen; Wang, Quan-Ming; Chemical Communications  (2019) –; doi:10.1039/C9CC03533H

data_7123459
_publ_section_title
;
 Monitoring the Growth of Ag-S Clusters through Crystallization of
 Intermediate Clusters
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03533H
_journal_year                    2019
_chemical_formula_moiety
'Ag30.95 C64 S22.5, Ag31.05 C66 F3 O2 S22.5, 2(C2 F3 O2)'
_chemical_formula_sum            'C136 H288 Ag62 F12 O8 S45'
_chemical_formula_weight         10410.29
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2019-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-31 deposited with the CCDC.    2019-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                88.2810(10)
_cell_angle_beta                 86.5500(10)
_cell_angle_gamma                85.8780(10)
_cell_formula_units_Z            2
_cell_length_a                   20.9287(3)
_cell_length_b                   25.7382(4)
_cell_length_c                   27.9899(4)
_cell_measurement_reflns_used    35259
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.1436
_cell_measurement_theta_min      2.7541
_cell_volume                     15006.0(4)
_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      173.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0700
_diffrn_reflns_av_unetI/netI     0.1110
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            121836
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.760
_exptl_absorpt_coefficient_mu    4.287
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.304
_exptl_crystal_description       block
_exptl_crystal_F_000             9820
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.622
_refine_diff_density_min         -1.362
_refine_diff_density_rms         0.266
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2714
_refine_ls_number_reflns         52746
_refine_ls_number_restraints     597
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1223
_refine_ls_R_factor_gt           0.0762
_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^)+(0.1054P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2037
_refine_ls_wR_factor_ref         0.2262
_reflns_Friedel_coverage         0.000
_reflns_number_gt                32808
_reflns_number_total             52746
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03533h2.cif
_cod_data_source_block           x649a_sq
_cod_database_code               7123459
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.674
_shelx_estimated_absorpt_t_min   0.566
_olex2_refinement_description
;
1. Restrained distances
 F2-C5HA
 1.35 with sigma of 0.02
 F7-C5HA
 1.35 with sigma of 0.02
 F8-C5HA
 1.35 with sigma of 0.02
 F7-F2
 2.2 with sigma of 0.02
 F8-F2
 2.2 with sigma of 0.02
 F7-F8
 2.2 with sigma of 0.02
 C42-O11
 1.43 with sigma of 0.02
 C38-C4GA
 1.54 with sigma of 0.02
 C4GA-C17
 1.54 with sigma of 0.02
 C4GA-C14
 1.54 with sigma of 0.02
 C38-C17
 2.51 with sigma of 0.02
 C17-C14
 2.51 with sigma of 0.02
 C38-C14
 2.51 with sigma of 0.02
 C4GA-C26
 1.54 with sigma of 0.02
 C4GA-C30
 1.54 with sigma of 0.02
 C30-C26
 2.51 with sigma of 0.02
 C4GA-C34
 1.54 with sigma of 0.02
 C30-C34
 2.51 with sigma of 0.02
 C34-C26
 2.51 with sigma of 0.02
 C26-C30
 2.51 with sigma of 0.02
 C5HA-O11
 2.46 with sigma of 0.02
 C8IA-C41A
 1.54 with sigma of 0.02
 C8IA-C41B
 1.54 with sigma of 0.02
 C8IA-C8B
 1.54 with sigma of 0.02
 C8IA-C8A
 1.54 with sigma of 0.02
 C8IA-C10A
 1.54 with sigma of 0.02
 C8IA-C10B
 1.54 with sigma of 0.02
 C41B-C8A
 2.51 with sigma of 0.02
 C8A-C10B
 2.51 with sigma of 0.02
 C10B-C41B
 2.51 with sigma of 0.02
 C41A-C8B
 2.51 with sigma of 0.02
 C8B-C10A
 2.51 with sigma of 0.02
 C10A-C41A
 2.51 with sigma of 0.02
 C7DA-C5GA
 1.54 with sigma of 0.02
 C5GA-F106
 1.35 with sigma of 0.02
 C5GA-F34
 1.35 with sigma of 0.02
 C5GA-F11
 1.35 with sigma of 0.02
 O1-C7DA
 1.3 with sigma of 0.02
 C5GA-O1
 2.46 with sigma of 0.02
 C7DA-F11
 2.36 with sigma of 0.02
 C7DA-F106
 2.36 with sigma of 0.02
 C7DA-F34
 2.36 with sigma of 0.02
 F106-F11
 2.2 with sigma of 0.02
 F11-F34
 2.2 with sigma of 0.02
 F34-F106
 2.2 with sigma of 0.02
 O1AA-C7DA
 1.3 with sigma of 0.02
 O1AA-C5GA
 2.46 with sigma of 0.02
 O1-O1AA
 2.25 with sigma of 0.02
 O37-C42
 1.26 with sigma of 0.02
 O37-O11
 2.33 with sigma of 0.02
 O37-C5HA
 2.46 with sigma of 0.02
 C5EA-C32
 1.54 with sigma of 0.02
 C5EA-C44
 1.54 with sigma of 0.02
 C8JA-C5EA
 1.54 with sigma of 0.02
 C8JA-C32
 2.51 with sigma of 0.02
 C32-C44
 2.51 with sigma of 0.02
 C44-C8JA
 2.51 with sigma of 0.02
2. Restrained atomic chiral volume
 C42
 fixed at 0 with sigma of 0.01
 C7DA
 fixed at 0 with sigma of 0.01
3. Rigid bond restraints
 F1, F1CA, F7DA, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C0BA, S84, C0FA, C4HA, C1GA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1AA, C7DA, O1, F34, C5GA, F11, F106
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Ag56 \\sim O0AA \\sim O5HA \\sim C6JA: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
F1 \\sim F1CA \\sim F7DA \\sim O0AA \\sim O5HA \\sim C6JA \\sim C22: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
C38 \\sim C34 \\sim C14 \\sim C30 \\sim C17 \\sim C26: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C32 \\sim C8JA \\sim C5EA \\sim C44: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
S2A \\sim S79 \\sim Ag2B: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Ag2H \\sim Ag25 \\sim Ag2G \\sim Ag17: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C8A \\sim C8B \\sim C41B \\sim C41A \\sim C10B \\sim C10A \\sim C8IA: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
C1IA \\sim C5DA \\sim C9 \\sim C4IA: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
O1 \\sim C7DA \\sim O1AA \\sim C5GA \\sim F11 \\sim F34 \\sim F106: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
C42 \\sim C5HA \\sim F2 \\sim F7 \\sim O11 \\sim O37 \\sim F8: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Ag1L \\sim O37: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C8JA \\sim C5EA \\sim C32 \\sim C44: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
S75 \\sim S102 \\sim Ag1C \\sim Ag1I \\sim Ag3E: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002
Ag41 \\sim Ag5A \\sim Ag21: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
S22A \\sim S104 \\sim Ag1H: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
S109 \\sim C0AA \\sim C9HA \\sim C8GA \\sim C4: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
C1AA \\sim S93 \\sim S1 \\sim C2FA \\sim C7IA \\sim C4JA: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C2AA \\sim C23 \\sim C11 \\sim C15 \\sim S85: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C2CA \\sim C6HA \\sim C2GA \\sim C0JA \\sim S87: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
C3DA \\sim C5IA \\sim C7JA \\sim C2JA \\sim S79 \\sim S2A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C2HA \\sim C7AA \\sim C5FA \\sim C8CA \\sim S90: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
C9JA \\sim C0EA \\sim C24 \\sim C12 \\sim S77: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C13 \\sim C20 \\sim C0GA \\sim C45 \\sim S106: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C3BA \\sim C2BA \\sim C2EA \\sim C3EA \\sim S89: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
Uanis(Ag3E) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Ag2G) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Ag2H) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Ag2F) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Ag1I) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: Ag4(0.9) Ag7(0.95) Ag10(0.85) Ag17(0.9) Ag19(0.95) Ag21(0.95)
 Ag23(0.85) Ag25(0.9) Ag30(0.93) Ag32(0.75) Ag33(0.9) Ag35(0.65) Ag36(0.88)
 Ag37(0.8) Ag38(0.75) Ag42(0.9) Ag44(0.9) Ag45(0.95) Ag51(0.85) Ag52(0.82)
 Ag53(0.9) Ag54(0.85) Ag55(0.5) Ag56(0.8) Ag57(0.8) Ag58(0.9) Ag60(0.75)
 Ag61(0.65) Ag78(0.55) S79(0.75) S88(0.88) S90(0.85) S93(0.75) S104(0.85)
 Ag2A(0.15) Ag2(0.15) Ag1B(0.15) Ag1C(0.1) Ag1D(0.1) Ag1E(0.12) Ag1F(0.1)
 Ag1G(0.25) Ag1H(0.1) Ag1J(0.1) Ag1K(0.35) Ag1L(0.35) Ag1M(0.35) Ag1N(0.1)
 Ag1O(0.25) Ag1P(0.1) Ag1I(0.1) Ag1Q(0.1) Ag1R(0.1) Ag1S(0.1) Ag1(0.1)
 Ag1T(0.1) Ag2B(0.08) Ag1U(0.1) Ag1V(0.07) Ag1W(0.05) Ag2E(0.05) S1(0.25)
 Ag2F(0.05) Ag2G(0.05) S22A(0.15) Ag2H(0.05) Ag3A(0.5) Ag3B(0.25) Ag3C(0.05)
 C8B(0.5) C10B(0.5) C14(0.5) C17(0.5) C26(0.5) C30(0.5) C41B(0.5) Ag4G(0.05)
 S0AA(0.15) Ag3E(0.05) Ag3G(0.05) S2A(0.25) Ag4A(0.05) C38(0.5) S2C(0.12)
 Ag5A(0.05) C34(0.5) C8A(0.5) C41A(0.5) C10A(0.5)
;
_shelx_res_checksum              13863
_shelx_fab_checksum              46928
_olex2_submission_special_instructions 'No special instructions were received'