Snapshots of key intermediates unveiling the growth from silver ions to Ag70 nanoclusters
Luo, Xi-Ming; Huang, Shuo; Luo, Peng; Ma, Kai; Wang, Zhao-Yang; Dong, Xi-Yan; Zang, Shuang-Quan; Chemical Science 13 (2022) 11110–11118; doi:10.1039/D2SC04204E

data_1567541
_publ_section_title
;
 Snapshots of key intermediates unveiling the growth from silver ions to
 Ag70 nanoclusters
;
_journal_issue                   37
_journal_name_full               'Chemical Science'
_journal_page_first              11110
_journal_page_last               11118
_journal_paper_doi               10.1039/D2SC04204E
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C62 H77 Ag24 F50 N5 O25 S9'
_chemical_formula_sum            'C62 H77 Ag24 F50 N5 O25 S9'
_chemical_formula_weight         5119.70
_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   mixed
_audit_creation_date             2022-03-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-06-28 deposited with the CCDC.	2022-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                97.0910(10)
_cell_angle_beta                 112.841(2)
_cell_angle_gamma                104.1620(10)
_cell_formula_units_Z            1
_cell_length_a                   14.9116(3)
_cell_length_b                   16.3962(2)
_cell_length_c                   18.2438(3)
_cell_measurement_reflns_used    11547
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      73.9910
_cell_measurement_theta_min      2.9990
_cell_volume                     3864.89(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.947
_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    -89.00  15.00   0.50    0.50    --    0.00 -38.00  90.00  208
  2  \w    -23.00  88.00   0.50    0.50    --    0.00  57.00  60.00  222
  3  \w      7.00 121.00   0.50    3.00    --   95.80 -82.00-150.00  228
  4  \w     36.00 123.00   0.50    3.00    --   95.80 -15.00  60.00  174
  5  \w     78.00 105.00   0.50    3.00    --   95.80  30.00  60.00   54
  6  \w      8.00  34.00   0.50    3.00    --   95.80 -82.00  60.00   52
  7  \w      6.00 108.00   0.50    3.00    --   95.80 -61.00-150.00  204
  8  \w     47.00 125.00   0.50    3.00    --   95.80 -82.00  60.00  156
  9  \w     43.00 119.00   0.50    3.00    --   95.80 -61.00  60.00  152
 10  \w     17.00  93.00   0.50    3.00    --   95.80 -61.00 -30.00  152
 11  \w     16.00 117.00   0.50    3.00    --   95.80 -82.00 -30.00  202
 12  \w    127.00 185.00   0.50    3.00    --   95.80  30.00  60.00  116
 13  \w     76.00 184.00   0.50    3.00    --   95.80  30.00  90.00  216
 14  \w     63.00 114.00   0.50    3.00    --   95.80 -30.00  60.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0810409000
_diffrn_orient_matrix_UB_12      0.0095156000
_diffrn_orient_matrix_UB_13      -0.0337599000
_diffrn_orient_matrix_UB_21      0.0700380000
_diffrn_orient_matrix_UB_22      -0.0259329000
_diffrn_orient_matrix_UB_23      0.0744047000
_diffrn_orient_matrix_UB_31      -0.0502711000
_diffrn_orient_matrix_UB_32      -0.0960413000
_diffrn_orient_matrix_UB_33      -0.0474693000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33822
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.584
_diffrn_reflns_theta_min         2.710
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    25.887
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.200
_exptl_crystal_description       block
_exptl_crystal_F_000             2406
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.899
_refine_diff_density_min         -1.589
_refine_diff_density_rms         0.340
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1424
_refine_ls_number_reflns         15003
_refine_ls_number_restraints     5120
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.1286
_refine_ls_R_factor_gt           0.0995
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1960P)^2^+35.8638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3071
_refine_ls_wR_factor_ref         0.3306
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10588
_reflns_number_total             15003
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04204e4.cif
_cod_data_source_block           ag24-c2f5
_cod_depositor_comments
'Adding full bibliography for 1567539--1567541.cif.'
_cod_original_cell_volume        3864.89(12)
_cod_database_code               1567541
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.306
_shelx_estimated_absorpt_t_min   0.231
_reflns_odcompleteness_completeness 98.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O6-C7 = O5-C7
 1.2 with sigma of 0.02
 C8-C7
 1.51 with sigma of 0.01
 C8-C9
 1.51 with sigma of 0.01
 S1-C1AA
 1.85 with sigma of 0.02
 S5-C50
 1.85 with sigma of 0.02
 C69-C50 = C92-C50
 1.53 with sigma of 0.01
 C39-C2AA = C79-C2AA
 1.53 with sigma of 0.01
 N10-C0AA = N10-C55
 1.45 with sigma of 0.02
 C7AA-N10
 1.4 with sigma of 0.02
 C7AA-O0AA
 1.2 with sigma of 0.02
 C31-O4AA
 1.2 with sigma of 0.02
 N8-C44 = N8-C53
 1.45 with sigma of 0.02
 O9-C13 = O10-C13
 1.2 with sigma of 0.02
 C14-C13
 1.5 with sigma of 0.01
 C15-C14
 1.5 with sigma of 0.02
 O3AA-C54
 1.2 with sigma of 0.02
 C54-N38
 1.45 with sigma of 0.02
 O4-C4 = O3-C4
 1.2 with sigma of 0.02
 C4-C5
 1.51 with sigma of 0.01
 N2-C4AA
 1.4 with sigma of 0.02
 O23-C4AA
 1.2 with sigma of 0.02
 O23-Ag7
 2.5 with sigma of 0.02
 S3-C48
 1.85 with sigma of 0.01
 C80-C48
 1.53 with sigma of 0.01
 S3-C48 = S3-C100
 1.85 with sigma of 0.02
 C77-C48 = C6AA-C100 = C63-C48 = C80-C100
 1.53 with sigma of 0.01
 C1AA-C5AA = C1AA-C34
 1.53 with sigma of 0.01
 C8AA-C1AA = C9AA-C1AA
 1.53 with sigma of 0.01
 O16-C22 = O15-C22
 1.2 with sigma of 0.02
 C23-C22
 1.51 with sigma of 0.01
 O18-Ag8_$1
 2.3 with sigma of 0.02
 O2-C1 = O1-C1
 1.2 with sigma of 0.02
 C3-F4 = C3-F5 = C3-F3 = C3-C2
 1.51 with sigma of 0.01
 F2-C2 = F1-C2 = F3-C3 = F4-C3 = F5-C3
 1.4 with sigma of 0.01
 C35-O43
 1.2 with sigma of 0.02
 N38-C66
 1.45 with sigma of 0.02
 N38-C1BA
 1.45 with sigma of 0.02
 H66C-F3
 2 with sigma of 0.02
 N2-C3AA = N2-C29
 1.45 with sigma of 0.02
 N33-C116 = N33-C35 = N33-C56
 1.45 with sigma of 0.01
 C63-C77
 2.4 with sigma of 0.04
 C7AA-C55
 2.4 with sigma of 0.04
 C0AA-C55
 2.4 with sigma of 0.04
 C0AA-C7AA
 2.4 with sigma of 0.04
 O10-O9
 2.2 with sigma of 0.04
 F21-F22
 2.2 with sigma of 0.04
 N2-O23
 2.2 with sigma of 0.04
 F4-C2
 2.5 with sigma of 0.04
 C54-C66
 2.4 with sigma of 0.04
 C1BA-C66
 2.4 with sigma of 0.04
 C54-C1BA
 2.4 with sigma of 0.04
 C116-C35
 2.4 with sigma of 0.04
 O23-C29
 2.4 with sigma of 0.04
 C56-C35
 2.4 with sigma of 0.04
 C116-C56
 2.4 with sigma of 0.04
 C14-O9 \\sim C14-O10
 with sigma of 0.02
 C14-F25 \\sim C14-F24 \\sim C14-F23
 with sigma of 0.02
 F25-F24 \\sim F25-F23 \\sim F24-F23
 with sigma of 0.02
 O5-C7 \\sim O6-C7 \\sim O8-C10 \\sim O7-C10
 with sigma of 0.02
 C3-F1 \\sim C3-F2 \\sim F1-F2
 with sigma of 0.02
 F4-F5 \\sim F4-F3 \\sim F5-F3
 with sigma of 0.02
 C2-F5 \\sim F3-C2 \\sim C2-F4
 with sigma of 0.02
3. Restrained planarity
 O0AA, N10, C0AA, C7AA, C55
 with sigma of 0.1
 O9, O10, C13, C14
 with sigma of 0.1
 O4AA, N8, C31, C44, C53
 with sigma of 0.1
 O18, C25, O17, C26
 with sigma of 0.1
 O3AA, N38, C1BA, C54, C66
 with sigma of 0.1
 O23, N2, C3AA, C4AA, C29
 with sigma of 0.1
 O43, C35, N33, C56, C116
 with sigma of 0.1
4. Rigid bond restraints
 F21, F22, F23, F24, F25, O9, O10, C13, C14, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S3, C6AA, C48, C63, C77, C80, C100
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1AA, C5AA, C8AA, C9AA, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C50 \\sim C69 \\sim C92: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01
S2 \\sim C2AA \\sim C39 \\sim C79: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.01
Ag5 \\sim O0AA \\sim N10 \\sim C0AA \\sim C7AA \\sim C55: within 3A with sigma
of 0.01 and sigma for terminal atoms of 0.01
Ag9 \\sim O4AA \\sim N8 \\sim C31 \\sim C44 \\sim C53: within 3A with sigma of
0.01 and sigma for terminal atoms of 0.01
Ag6 \\sim F16 \\sim F17 \\sim F18 \\sim F19 \\sim F20 \\sim O7 \\sim O8 \\sim
C10 \\sim C11 \\sim C12: within 3A with sigma of 0.01 and sigma for terminal
atoms of 0.01
Ag2 \\sim F11 \\sim F12 \\sim F13 \\sim F14 \\sim F15 \\sim O5 \\sim C7 \\sim
C8 \\sim C9: within 3A with sigma of 0.01 and sigma for terminal atoms of 0.01
F6 \\sim F7 \\sim F8 \\sim F9 \\sim F10 \\sim O3 \\sim O4 \\sim C4 \\sim C5
\\sim C6: within 3A with sigma of 0.01 and sigma for terminal atoms of 0.01
Ag2 \\sim Ag6 \\sim F11 \\sim F12 \\sim F13 \\sim F14 \\sim F15 \\sim O5 \\sim
O6 \\sim C7 \\sim C8 \\sim C9 \\sim F16 \\sim F17 \\sim F18 \\sim F19 \\sim F20
\\sim O7 \\sim O8 \\sim C10 \\sim C11 \\sim C12: within 3A with sigma of 0.01
and sigma for terminal atoms of 0.01
Ag7 \\sim F26 \\sim F27 \\sim F28 \\sim F29 \\sim F30 \\sim O11 \\sim O12 \\sim
C16 \\sim C17 \\sim C18: within 3A with sigma of 0.01 and sigma for terminal
atoms of 0.01
Ag7 \\sim F26 \\sim F27 \\sim F28 \\sim F29 \\sim F30 \\sim O11 \\sim O12 \\sim
C16 \\sim C17 \\sim C18 \\sim F31 \\sim F32 \\sim F33 \\sim F34 \\sim F35 \\sim
O13 \\sim O14 \\sim C19 \\sim C20 \\sim C21: within 3A with sigma of 0.01 and
sigma for terminal atoms of 0.01
Ag4 \\sim O4 \\sim F10 \\sim C6 \\sim F8 \\sim F9 \\sim F7 \\sim C5 \\sim F6
\\sim C4 \\sim O3 \\sim Ag2: within 3A with sigma of 0.01 and sigma for
terminal atoms of 0.01
F36 \\sim F37 \\sim F38 \\sim F39 \\sim F40 \\sim O16 \\sim C22 \\sim C23 \\sim
C24 \\sim F41 \\sim F42 \\sim F43 \\sim F44 \\sim F45 \\sim O18 \\sim C25 \\sim
C26 \\sim C27 \\sim O15 \\sim O17 \\sim Ag10: within 3A with sigma of 0.01 and
sigma for terminal atoms of 0.01
Ag2 \\sim Ag3 \\sim F1 \\sim F3 \\sim F2 \\sim F4 \\sim F5 \\sim O1 \\sim O2
\\sim C1 \\sim C2 \\sim C3: within 3A with sigma of 0.01 and sigma for terminal
atoms of 0.01
Ag10 \\sim O3AA \\sim N38 \\sim C1BA \\sim C54 \\sim C66: within 3A with sigma
of 0.01 and sigma for terminal atoms of 0.01
Ag7 \\sim O23 \\sim N2 \\sim C3AA \\sim C4AA \\sim C29: within 3A with sigma of
0.01 and sigma for terminal atoms of 0.01
C116 \\sim N33 \\sim C56 \\sim C35 \\sim O43 \\sim Ag8: within 3A with sigma of
0.01 and sigma for terminal atoms of 0.01
Uanis(Ag19) \\sim Ueq, Uanis(Ag12) \\sim Ueq, Uanis(Ag18) \\sim Ueq,
Uanis(Ag15) \\sim Ueq, Uanis(Ag14) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Ag15) \\sim Ueq, Uanis(Ag14) \\sim Ueq, Uanis(Ag16) \\sim Ueq,
Uanis(Ag12) \\sim Ueq, Uanis(Ag13) \\sim Ueq, Uanis(Ag11) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(Ag16) \\sim Ueq, Uanis(Ag11) \\sim Ueq, Uanis(Ag13) \\sim Ueq,
Uanis(Ag17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C0AA) \\sim Ueq, Uanis(N10) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C7AA)
\\sim Ueq, Uanis(O0AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C14) \\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(F24)
\\sim Ueq, Uanis(F25) \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F22) \\sim Ueq,
Uanis(O9) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(F11) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14)
\\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq,
Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(F16) \\sim
Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F19) \\sim Ueq,
Uanis(F20) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C6) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F9)
\\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F8) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C6) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8)
\\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C69) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C92) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C2AA) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C39) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6AA) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C48)
\\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C80) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C5AA) \\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C8AA) \\sim Ueq, Uanis(C9AA) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F26) \\sim Ueq, Uanis(F27) \\sim Ueq, Uanis(F28) \\sim Ueq, Uanis(F29)
\\sim Ueq, Uanis(F30) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O12) \\sim Ueq,
Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(F31)
\\sim Ueq, Uanis(F32) \\sim Ueq, Uanis(F33) \\sim Ueq, Uanis(F34) \\sim Ueq,
Uanis(F35) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(F36) \\sim Ueq, Uanis(F37) \\sim Ueq, Uanis(F38) \\sim Ueq, Uanis(F39)
\\sim Ueq, Uanis(F40) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O16) \\sim Ueq,
Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(F41)
\\sim Ueq, Uanis(F42) \\sim Ueq, Uanis(F43) \\sim Ueq, Uanis(F44) \\sim Ueq,
Uanis(F45) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(F1) \\sim
Ueq, Uanis(F2) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(F4) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C29) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C3AA) \\sim Ueq, Uanis(C4AA)
\\sim Ueq, Uanis(O23) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
6. Same fragment restrains
{F1, F2, F3, F4, F5, O1, O2, C1, C2, C3} sigma for 1-2: 0.02, 1-3: 0.04
as
{F21, F22, F23, F24, F25, O9, O10, C13, C14, C15}
{F1, F2, F3, F4, F5, O1, O2, C1, C2, C3} sigma for 1-2: 0.02, 1-3: 0.04
as
{F6, F7, F8, F9, F10, O3, O4, C4, C5, C6}
{F1, F2, F3, F4, F5, O1, O2, C1, C2, C3} sigma for 1-2: 0.02, 1-3: 0.04
as
{F11, F12, F13, F14, F15, O5, O6, C7, C8, C9}
{F1, F2, F3, F4, F5, O1, O2, C1, C2, C3} sigma for 1-2: 0.02, 1-3: 0.04
as
{F16, F17, F18, F19, F20, O7, O8, C10, C11, C12}
{F1, F2, F3, F4, F5, O1, O2, C1, C2, C3} sigma for 1-2: 0.02, 1-3: 0.04
as
{F26, F27, F28, F29, F30, O11, O12, C16, C17, C18}
{F1, F2, F3, F4, F5, O1, O2, C1, C2, C3} sigma for 1-2: 0.02, 1-3: 0.04
as
{F31, F32, F33, F34, F35, O13, O14, C19, C20, C21}
{F1, F2, F3, F4, F5, O1, O2, C1, C2, C3} sigma for 1-2: 0.02, 1-3: 0.04
as
{F36, F37, F38, F39, F40, O15, O16, C22, C23, C24}
{F1, F2, F3, F4, F5, O1, O2, C1, C2, C3} sigma for 1-2: 0.02, 1-3: 0.04
as
{F41, F42, F43, F44, F45, O17, O18, C25, C26, C27}
7. Others
 Sof(F16)=Sof(F17)=Sof(F18)=Sof(F19)=Sof(F20)=Sof(O7)=Sof(O8)=Sof(C10)=
 Sof(C11)=Sof(C12)=1-FVAR(1)
 Sof(F11)=Sof(F12)=Sof(F13)=Sof(F14)=Sof(F15)=Sof(O5)=Sof(O6)=Sof(C7)=Sof(C8)=
 Sof(C9)=FVAR(1)
 Sof(C6AA)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C80)=Sof(H80A)=Sof(H80B)=
 Sof(H80C)=Sof(C100)=Sof(H100)=1-FVAR(2)
 Sof(C48)=Sof(H48)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=Sof(C77)=Sof(H77A)=
 Sof(H77B)=Sof(H77C)=FVAR(2)
 Sof(H1AB)=Sof(C9AA)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C34)=Sof(H34A)=
 Sof(H34B)=Sof(H34C)=1-FVAR(3)
 Sof(H1AA)=Sof(C5AA)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C8AA)=Sof(H8AA)=
 Sof(H8AB)=Sof(H8AC)=FVAR(3)
 Sof(F41)=Sof(F42)=Sof(F43)=Sof(F44)=Sof(F45)=Sof(O17)=Sof(O18)=Sof(C25)=
 Sof(C26)=Sof(C27)=1-FVAR(4)
 Sof(F36)=Sof(F37)=Sof(F38)=Sof(F39)=Sof(F40)=Sof(O15)=Sof(O16)=Sof(C22)=
 Sof(C23)=Sof(C24)=FVAR(4)
 Sof(F31)=Sof(F32)=Sof(F33)=Sof(F34)=Sof(F35)=Sof(O13)=Sof(O14)=Sof(C19)=
 Sof(C20)=Sof(C21)=1-FVAR(5)
 Sof(F26)=Sof(F27)=Sof(F28)=Sof(F29)=Sof(F30)=Sof(O11)=Sof(O12)=Sof(C16)=
 Sof(C17)=Sof(C18)=FVAR(5)
 Fixed Sof: Ag11(0.35) Ag12(0.35) Ag13(0.35) Ag14(0.15) Ag15(0.2) Ag16(0.1)
 Ag17(0.2) Ag18(0.2) Ag19(0.1) F21(0.5) F22(0.5) F23(0.5) F24(0.5) F25(0.5)
 O9(0.5) O10(0.5) C13(0.5) C14(0.5) C15(0.5) F1(0.75) F3(0.75) F2(0.75)
 F4(0.75) F5(0.75) F6(0.75) F7(0.75) F8(0.75) F9(0.75) F10(0.75) O3(0.75)
 O4(0.75) C4(0.75) C5(0.75) C6(0.75) O0AA(0.5) O1(0.75) O2(0.75) O3AA(0.5)
 O4AA(0.5) O23(0.5) N2(0.5) N8(0.5) N10(0.5) N38(0.5) C0AA(0.5) H0AA(0.5)
 H0AB(0.5) H0AC(0.5) C1(0.75) C1AA(0.5) C1BA(0.5) H1BA(0.5) H1BB(0.5) H1BC(0.5)
 C2(0.75) C2AA(0.5) H2AA(0.5) C3(0.75) C3AA(0.5) H3AA(0.5) H3AB(0.5) H3AC(0.5)
 C4AA(0.5) H4AA(0.5) C7AA(0.5) H7AA(0.5) C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5)
 C31(0.5) H31(0.5) C39(0.5) H39A(0.5) H39B(0.5) H39C(0.5) C44(0.5) H44A(0.5)
 H44B(0.5) H44C(0.5) C50(0.5) H50(0.5) C53(0.5) H53A(0.5) H53B(0.5) H53C(0.5)
 C54(0.5) H54(0.5) C55(0.5) H55A(0.5) H55B(0.5) H55C(0.5) C66(0.5) H66A(0.5)
 H66B(0.5) H66C(0.5) C69(0.5) H69A(0.5) H69B(0.5) H69C(0.5) C79(0.5) H79A(0.5)
 H79B(0.5) H79C(0.5) C92(0.5) H92A(0.5) H92B(0.5) H92C(0.5) N33(0.5) C35(0.5)
 H35(0.5) O43(0.5) C56(0.5) H56A(0.5) H56B(0.5) H56C(0.5) C116(0.5) H11A(0.5)
 H11B(0.5) H11C(0.5)
8.a Riding coordinates:
 C1BA(H1BA,H1BB,H1BC), C29(H29A,H29B,H29C), C66(H66A,H66B,H66C), C56(H56A,H56B,
 H56C), C116(H11A,H11B,H11C)
8.b Ternary CH refined with riding coordinates:
 C1AA(H1AA), C1AA(H1AB), C2AA(H2AA), C48(H48), C50(H50), C100(H100)
8.c Aromatic/amide H refined with riding coordinates:
 C4AA(H4AA), C7AA(H7AA), C31(H31), C54(H54), C35(H35)
8.d Idealised Me refined as rotating group:
 C0AA(H0AA,H0AB,H0AC), C3AA(H3AA,H3AB,H3AC), C5AA(H5AA,H5AB,H5AC), C6AA(H6AA,
 H6AB,H6AC), C8AA(H8AA,H8AB,H8AC), C9AA(H9AA,H9AB,H9AC), C34(H34A,H34B,H34C),
 C39(H39A,H39B,H39C), C44(H44A,H44B,H44C), C53(H53A,H53B,H53C), C55(H55A,H55B,
 H55C), C63(H63A,H63B,H63C), C69(H69A,H69B,H69C), C77(H77A,H77B,H77C), C79(H79A,
 H79B,H79C), C80(H80A,H80B,H80C), C92(H92A,H92B,H92C)
;
_shelx_res_checksum              36527
_shelx_fab_checksum              11104
_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 3.501
_oxdiff_exptl_absorpt_empirical_full_min 0.483