Size disproportionation among nanocluster transformations.
Zhu, Chen; Lu, Luyao; Li, Fei; Kang, Xi; Zhu, Manzhou; Chemical science 15 (2024) 16637–16644; doi:10.1039/d4sc04884a

data_1572629
_publ_section_title
;
 Size disproportionation among nanocluster transformations.
;
_journal_issue                   40
_journal_name_full               'Chemical science'
_journal_page_first              16637
_journal_page_last               16644
_journal_paper_doi               10.1039/d4sc04884a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety
'C134.416 H91.048 Ag11 Au0.5 Cu5 F34.964 P3 S13, C129.814 H86.064 Ag9 Au0.5 Cu7 F33.149 P2.75 S13'
_chemical_formula_sum            'C264.23 H177.12 Ag20 Au Cu12 F68.11 P5.75 S26'
_chemical_formula_weight         8774.59
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-14
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-07-12 deposited with the CCDC.	2024-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                82.015(3)
_cell_angle_beta                 84.918(3)
_cell_angle_gamma                83.158(3)
_cell_formula_units_Z            2
_cell_length_a                   20.3056(8)
_cell_length_b                   22.3996(9)
_cell_length_c                   37.5185(12)
_cell_measurement_reflns_used    2711
_cell_measurement_temperature    120
_cell_measurement_theta_max      67.22
_cell_measurement_theta_min      1.92
_cell_volume                     16733.9(11)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)
;
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details      '546 frames, detector distance = 60 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_unetI/netI     0.0966
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            139460
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        62.499
_diffrn_reflns_theta_max         62.499
_diffrn_reflns_theta_min         4.336
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    13.217
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            'metallic blackish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             8490
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.393
_refine_diff_density_min         -3.203
_refine_diff_density_rms         0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3314
_refine_ls_number_reflns         52150
_refine_ls_number_restraints     3998
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1303
_refine_ls_R_factor_gt           0.0997
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2746
_refine_ls_wR_factor_ref         0.3009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                31851
_reflns_number_total             52150
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04884a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1572629--1572632.cif.'
_cod_database_code               1572629
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.352
_shelx_estimated_absorpt_t_min   0.352
_olex2_refinement_description
;
1. Restrained distances
 C0A9-F07L
 1.38 with sigma of 0.01
 F09R-C0A9
 1.38 with sigma of 0.01
 C0A9-F070
 1.38 with sigma of 0.01
 C78-F0AG
 1.38 with sigma of 0.01
 F09O-C311
 1.38 with sigma of 0.01
 F0AN-C311
 1.38 with sigma of 0.01
 F09F-C311
 1.38 with sigma of 0.01
 F8-C07Z
 1.38 with sigma of 0.01
 C07Z-F3
 1.38 with sigma of 0.01
 F4-C07Z
 1.38 with sigma of 0.01
 C78-F04R
 1.38 with sigma of 0.01
 F0AG-C78
 1.38 with sigma of 0.01
 F99-C78
 1.38 with sigma of 0.01
 C371-C132
 3.6 with sigma of 0.02
 C371-C179
 3.6 with sigma of 0.02
 F13-C3
 1.36 with sigma of 0.01
 C3-C085
 1.44 with sigma of 0.01
 F7-C3
 1.36 with sigma of 0.01
 F26-C3
 1.36 with sigma of 0.01
 F27-C3
 1.36 with sigma of 0.01
 F1-C3
 1.36 with sigma of 0.01
 F556-C3
 1.36 with sigma of 0.04
 C371-P1B
 1.8 with sigma of 0.04
 P1B-C171
 1.8 with sigma of 0.04
 C124-C177
 1.4 with sigma of 0.01
 C177-C123
 2.5 with sigma of 0.01
 C125-C177
 2.5 with sigma of 0.01
 C177-F49
 1.35 with sigma of 0.01
 F31-F52
 2 with sigma of 0.01
 F49-F31
 2 with sigma of 0.01
 F52-F49
 2 with sigma of 0.01
 F31-C177
 1.35 with sigma of 0.01
 C177-F52
 1.35 with sigma of 0.01
 C33-C85
 1.4 with sigma of 0.04
 C85-F671
 1.3 with sigma of 0.01
 C85-F683
 1.3 with sigma of 0.01
 C33-F671
 2.3 with sigma of 0.01
 C33-F683
 2.3 with sigma of 0.01
 P1B-C169
 2.8 with sigma of 0.04
 P1B-C172
 2.8 with sigma of 0.04
 C176-P1B
 2.8 with sigma of 0.04
 P1B-C173
 2.8 with sigma of 0.04
 P1B-C193
 1.8 with sigma of 0.04
 P1B-C132
 2.8 with sigma of 0.04
 C179-P1B
 2.8 with sigma of 0.04
 F671-F683
 2 with sigma of 0.04
 F248-F671
 2 with sigma of 0.04
 F683-C33
 2.3 with sigma of 0.04
 F683-F248
 2 with sigma of 0.04
 F248-C85
 1.3 with sigma of 0.04
 F671-C33
 2.3 with sigma of 0.04
 F248-C33
 2.3 with sigma of 0.04
2. Restrained planarity
 P1B, C371, C176, C225, C175, C174, C173
 with sigma of 0.1
 P1B, C171, C95, C111, C170, C172
 with sigma of 0.1
 C121, C124, C123, C122, C125, C126, S01K, C177
 with sigma of 0.1
 P1B, C193, C179, C273, C142, C138, C132
 with sigma of 0.01
3. Rigid bond restraints
 P1B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 F683, F671
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
F01U \\sim F01V \\sim F01X \\sim F01Y \\sim F021 \\sim F024 \\sim F028 \\sim
F029 \\sim F02C \\sim F02E \\sim F02J \\sim F02K \\sim F02Q \\sim F02V \\sim
F02W \\sim F036 \\sim F03C \\sim F03D \\sim F03F \\sim F03G \\sim F03N \\sim
F03T \\sim F03U \\sim F03V \\sim F049 \\sim F04C \\sim F04H \\sim F04I \\sim
F04Q \\sim F04R \\sim F056 \\sim F05N \\sim F05O \\sim F05W \\sim F062 \\sim
F06G \\sim F06K \\sim F06M \\sim F06T \\sim F070 \\sim F071 \\sim F072 \\sim
F075 \\sim F078 \\sim F07H \\sim F07I \\sim F07L \\sim F07O \\sim F07P \\sim
F08K \\sim F08L \\sim F09D \\sim F09F \\sim F09O \\sim F09R \\sim F0A0 \\sim
F0AG \\sim F0AN \\sim F3 \\sim F4 \\sim F8 \\sim F25 \\sim F99 \\sim F33 \\sim
F143 \\sim F7 \\sim F1 \\sim F13 \\sim F26 \\sim F27 \\sim F556 \\sim F31 \\sim
F49 \\sim F52 \\sim F671 \\sim F683: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C01Z \\sim C022 \\sim C027 \\sim C025 \\sim C047 \\sim C05L \\sim C04U \\sim
C02L \\sim C02H \\sim C02M \\sim C02X \\sim C03A \\sim C039 \\sim C05I \\sim
C03M \\sim C02Y \\sim C033 \\sim C04B \\sim C04E \\sim C04K \\sim C04T \\sim
C04X \\sim C055 \\sim C031 \\sim C02N \\sim C032 \\sim C061 \\sim C06P \\sim
C058 \\sim C05A \\sim C06L \\sim C06E \\sim C03J \\sim C020 \\sim C03Z \\sim
C05B \\sim C05K \\sim C02Z \\sim C03R \\sim C02O \\sim C05H \\sim C05D \\sim
C08V \\sim C09A \\sim C04Z \\sim C053 \\sim C03O \\sim C05G \\sim C05U \\sim
C05Z \\sim C05Y \\sim C05M \\sim C077 \\sim C05R \\sim C07R \\sim C063 \\sim
C066 \\sim C03X \\sim C034 \\sim C04N \\sim C057 \\sim C04G \\sim C06B \\sim
C06H \\sim C03P \\sim C07M \\sim C06S \\sim C08O \\sim C09V \\sim C06W \\sim
C076 \\sim C07B \\sim C07C \\sim C07U \\sim C07Z \\sim C080 \\sim C081 \\sim
C082 \\sim C083 \\sim C084 \\sim C08D \\sim C094 \\sim C099 \\sim C09B \\sim
C09Q \\sim C085 \\sim C073 \\sim C09M \\sim C02P \\sim C0A6 \\sim C0A9 \\sim
C0AC \\sim C1 \\sim C31 \\sim C75 \\sim C2 \\sim C8 \\sim C9 \\sim C4 \\sim C17
\\sim C18 \\sim C12 \\sim C5 \\sim C6 \\sim C13 \\sim C15 \\sim C16 \\sim C20
\\sim C19 \\sim C14 \\sim C11 \\sim C7 \\sim C10 \\sim C22 \\sim C23 \\sim C24
\\sim C30 \\sim C32 \\sim C38 \\sim C51 \\sim C80 \\sim C154 \\sim C27 \\sim
C28 \\sim C29 \\sim C40 \\sim C39 \\sim C34 \\sim C37 \\sim C62 \\sim C90 \\sim
C44 \\sim C35 \\sim C36 \\sim C41 \\sim C42 \\sim C43 \\sim C45 \\sim C46 \\sim
C47 \\sim C72 \\sim C55 \\sim C61 \\sim C60 \\sim C59 \\sim C57 \\sim C56 \\sim
C48 \\sim C49 \\sim C50 \\sim C52 \\sim C54 \\sim C53 \\sim C63 \\sim C129
\\sim C65 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C73 \\sim C74
\\sim C76 \\sim C77 \\sim C78 \\sim C86 \\sim C84 \\sim C83 \\sim C82 \\sim C81
\\sim C79 \\sim C113 \\sim C87 \\sim C93 \\sim C92 \\sim C91 \\sim C89 \\sim
C88 \\sim C94 \\sim C96 \\sim C97 \\sim C98 \\sim C99 \\sim C100 \\sim C107
\\sim C106 \\sim C109 \\sim C117 \\sim C118 \\sim C108 \\sim C102 \\sim C105
\\sim C104 \\sim C119 \\sim C120 \\sim C103 \\sim C112 \\sim C110 \\sim C101
\\sim C116 \\sim C115 \\sim C114 \\sim C121 \\sim C126 \\sim C125 \\sim C124
\\sim C123 \\sim C122 \\sim C127 \\sim C130 \\sim C134 \\sim C135 \\sim C131
\\sim C133 \\sim C128 \\sim C136 \\sim C143 \\sim C141 \\sim C140 \\sim C139
\\sim C137 \\sim C148 \\sim C150 \\sim C151 \\sim C152 \\sim C157 \\sim C149
\\sim C144 \\sim C147 \\sim C146 \\sim C178 \\sim C166 \\sim C145 \\sim C153
\\sim C155 \\sim C156 \\sim C160 \\sim C159 \\sim C158 \\sim C161 \\sim C162
\\sim C168 \\sim C167 \\sim C165 \\sim C164 \\sim C163 \\sim C311 \\sim C66
\\sim C3 \\sim C21 \\sim C25 \\sim C26 \\sim C33 \\sim C58 \\sim C64 \\sim C85
\\sim C173 \\sim C174 \\sim C175 \\sim C225 \\sim C176 \\sim C371 \\sim C171
\\sim C172 \\sim C170 \\sim C111 \\sim C95 \\sim C169 \\sim C177: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C138 \\sim C142 \\sim C273 \\sim C179 \\sim C193 \\sim C132 \\sim F248: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(F01U) \\sim Ueq, Uanis(F01V) \\sim Ueq, Uanis(F01X) \\sim Ueq,
Uanis(F01Y) \\sim Ueq, Uanis(F021) \\sim Ueq, Uanis(F024) \\sim Ueq,
Uanis(F028) \\sim Ueq, Uanis(F029) \\sim Ueq, Uanis(F02C) \\sim Ueq,
Uanis(F02E) \\sim Ueq, Uanis(F02J) \\sim Ueq, Uanis(F02K) \\sim Ueq,
Uanis(F02Q) \\sim Ueq, Uanis(F02V) \\sim Ueq, Uanis(F02W) \\sim Ueq,
Uanis(F036) \\sim Ueq, Uanis(F03C) \\sim Ueq, Uanis(F03D) \\sim Ueq,
Uanis(F03F) \\sim Ueq, Uanis(F03G) \\sim Ueq, Uanis(F03N) \\sim Ueq,
Uanis(F03T) \\sim Ueq, Uanis(F03U) \\sim Ueq, Uanis(F03V) \\sim Ueq,
Uanis(F049) \\sim Ueq, Uanis(F04C) \\sim Ueq, Uanis(F04H) \\sim Ueq,
Uanis(F04I) \\sim Ueq, Uanis(F04Q) \\sim Ueq, Uanis(F04R) \\sim Ueq,
Uanis(F056) \\sim Ueq, Uanis(F05N) \\sim Ueq, Uanis(F05O) \\sim Ueq,
Uanis(F05W) \\sim Ueq, Uanis(F062) \\sim Ueq, Uanis(F06G) \\sim Ueq,
Uanis(F06K) \\sim Ueq, Uanis(F06M) \\sim Ueq, Uanis(F06T) \\sim Ueq,
Uanis(F070) \\sim Ueq, Uanis(F071) \\sim Ueq, Uanis(F072) \\sim Ueq,
Uanis(F075) \\sim Ueq, Uanis(F078) \\sim Ueq, Uanis(F07H) \\sim Ueq,
Uanis(F07I) \\sim Ueq, Uanis(F07L) \\sim Ueq, Uanis(F07O) \\sim Ueq,
Uanis(F07P) \\sim Ueq, Uanis(F08K) \\sim Ueq, Uanis(F08L) \\sim Ueq,
Uanis(F09D) \\sim Ueq, Uanis(F09F) \\sim Ueq, Uanis(F09O) \\sim Ueq,
Uanis(F09R) \\sim Ueq, Uanis(F0A0) \\sim Ueq, Uanis(F0AG) \\sim Ueq,
Uanis(F0AN) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F8)
\\sim Ueq, Uanis(F25) \\sim Ueq, Uanis(F99) \\sim Ueq, Uanis(F33) \\sim Ueq,
Uanis(F143) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F13)
\\sim Ueq, Uanis(F26) \\sim Ueq, Uanis(F27) \\sim Ueq, Uanis(F556) \\sim Ueq,
Uanis(F31) \\sim Ueq, Uanis(F49) \\sim Ueq, Uanis(F52) \\sim Ueq, Uanis(F671)
\\sim Ueq, Uanis(F683) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(F671) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C01Z) \\sim Ueq, Uanis(C022) \\sim Ueq, Uanis(C027) \\sim Ueq,
Uanis(C025) \\sim Ueq, Uanis(C047) \\sim Ueq, Uanis(C05L) \\sim Ueq,
Uanis(C04U) \\sim Ueq, Uanis(C02L) \\sim Ueq, Uanis(C02H) \\sim Ueq,
Uanis(C02M) \\sim Ueq, Uanis(C02X) \\sim Ueq, Uanis(C03A) \\sim Ueq,
Uanis(C039) \\sim Ueq, Uanis(C05I) \\sim Ueq, Uanis(C03M) \\sim Ueq,
Uanis(C02Y) \\sim Ueq, Uanis(C033) \\sim Ueq, Uanis(C04B) \\sim Ueq,
Uanis(C04E) \\sim Ueq, Uanis(C04K) \\sim Ueq, Uanis(C04T) \\sim Ueq,
Uanis(C04X) \\sim Ueq, Uanis(C055) \\sim Ueq, Uanis(C031) \\sim Ueq,
Uanis(C02N) \\sim Ueq, Uanis(C032) \\sim Ueq, Uanis(C061) \\sim Ueq,
Uanis(C06P) \\sim Ueq, Uanis(C058) \\sim Ueq, Uanis(C05A) \\sim Ueq,
Uanis(C06L) \\sim Ueq, Uanis(C06E) \\sim Ueq, Uanis(C03J) \\sim Ueq,
Uanis(C020) \\sim Ueq, Uanis(C03Z) \\sim Ueq, Uanis(C05B) \\sim Ueq,
Uanis(C05K) \\sim Ueq, Uanis(C02Z) \\sim Ueq, Uanis(C03R) \\sim Ueq,
Uanis(C02O) \\sim Ueq, Uanis(C05H) \\sim Ueq, Uanis(C05D) \\sim Ueq,
Uanis(C08V) \\sim Ueq, Uanis(C09A) \\sim Ueq, Uanis(C04Z) \\sim Ueq,
Uanis(C053) \\sim Ueq, Uanis(C03O) \\sim Ueq, Uanis(C05G) \\sim Ueq,
Uanis(C05U) \\sim Ueq, Uanis(C05Z) \\sim Ueq, Uanis(C05Y) \\sim Ueq,
Uanis(C05M) \\sim Ueq, Uanis(C077) \\sim Ueq, Uanis(C05R) \\sim Ueq,
Uanis(C07R) \\sim Ueq, Uanis(C063) \\sim Ueq, Uanis(C066) \\sim Ueq,
Uanis(C03X) \\sim Ueq, Uanis(C034) \\sim Ueq, Uanis(C04N) \\sim Ueq,
Uanis(C057) \\sim Ueq, Uanis(C04G) \\sim Ueq, Uanis(C06B) \\sim Ueq,
Uanis(C06H) \\sim Ueq, Uanis(C03P) \\sim Ueq, Uanis(C07M) \\sim Ueq,
Uanis(C06S) \\sim Ueq, Uanis(C08O) \\sim Ueq, Uanis(C09V) \\sim Ueq,
Uanis(C06W) \\sim Ueq, Uanis(C076) \\sim Ueq, Uanis(C07B) \\sim Ueq,
Uanis(C07C) \\sim Ueq, Uanis(C07U) \\sim Ueq, Uanis(C07Z) \\sim Ueq,
Uanis(C080) \\sim Ueq, Uanis(C081) \\sim Ueq, Uanis(C082) \\sim Ueq,
Uanis(C083) \\sim Ueq, Uanis(C084) \\sim Ueq, Uanis(C08D) \\sim Ueq,
Uanis(C094) \\sim Ueq, Uanis(C099) \\sim Ueq, Uanis(C09B) \\sim Ueq,
Uanis(C09Q) \\sim Ueq, Uanis(C085) \\sim Ueq, Uanis(C073) \\sim Ueq,
Uanis(C09M) \\sim Ueq, Uanis(C02P) \\sim Ueq, Uanis(C0A6) \\sim Ueq,
Uanis(C0A9) \\sim Ueq, Uanis(C0AC) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C31)
\\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C8) \\sim Ueq,
Uanis(C9) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq,
Uanis(C13) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C7) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C32) \\sim Ueq,
Uanis(C38) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C154)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq,
Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C37)
\\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C44) \\sim Ueq,
Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42)
\\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq,
Uanis(C47) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C61)
\\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C57) \\sim Ueq,
Uanis(C56) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50)
\\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C53) \\sim Ueq,
Uanis(C63) \\sim Ueq, Uanis(C129) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C67)
\\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq,
Uanis(C71) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C76)
\\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C86) \\sim Ueq,
Uanis(C84) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C81)
\\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C87) \\sim Ueq,
Uanis(C93) \\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C89)
\\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C96) \\sim Ueq,
Uanis(C97) \\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(C99) \\sim Ueq, Uanis(C100)
\\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(C106) \\sim Ueq, Uanis(C109) \\sim Ueq,
Uanis(C117) \\sim Ueq, Uanis(C118) \\sim Ueq, Uanis(C108) \\sim Ueq,
Uanis(C102) \\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(C104) \\sim Ueq,
Uanis(C119) \\sim Ueq, Uanis(C120) \\sim Ueq, Uanis(C103) \\sim Ueq,
Uanis(C112) \\sim Ueq, Uanis(C110) \\sim Ueq, Uanis(C101) \\sim Ueq,
Uanis(C116) \\sim Ueq, Uanis(C115) \\sim Ueq, Uanis(C114) \\sim Ueq,
Uanis(C121) \\sim Ueq, Uanis(C126) \\sim Ueq, Uanis(C125) \\sim Ueq,
Uanis(C124) \\sim Ueq, Uanis(C123) \\sim Ueq, Uanis(C122) \\sim Ueq,
Uanis(C127) \\sim Ueq, Uanis(C130) \\sim Ueq, Uanis(C134) \\sim Ueq,
Uanis(C135) \\sim Ueq, Uanis(C131) \\sim Ueq, Uanis(C133) \\sim Ueq,
Uanis(C128) \\sim Ueq, Uanis(C136) \\sim Ueq, Uanis(C143) \\sim Ueq,
Uanis(C141) \\sim Ueq, Uanis(C140) \\sim Ueq, Uanis(C139) \\sim Ueq,
Uanis(C137) \\sim Ueq, Uanis(C148) \\sim Ueq, Uanis(C150) \\sim Ueq,
Uanis(C151) \\sim Ueq, Uanis(C152) \\sim Ueq, Uanis(C157) \\sim Ueq,
Uanis(C149) \\sim Ueq, Uanis(C144) \\sim Ueq, Uanis(C147) \\sim Ueq,
Uanis(C146) \\sim Ueq, Uanis(C178) \\sim Ueq, Uanis(C166) \\sim Ueq,
Uanis(C145) \\sim Ueq, Uanis(C153) \\sim Ueq, Uanis(C155) \\sim Ueq,
Uanis(C156) \\sim Ueq, Uanis(C160) \\sim Ueq, Uanis(C159) \\sim Ueq,
Uanis(C158) \\sim Ueq, Uanis(C161) \\sim Ueq, Uanis(C162) \\sim Ueq,
Uanis(C168) \\sim Ueq, Uanis(C167) \\sim Ueq, Uanis(C165) \\sim Ueq,
Uanis(C164) \\sim Ueq, Uanis(C163) \\sim Ueq, Uanis(C311) \\sim Ueq, Uanis(C66)
\\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C173) \\sim Ueq, Uanis(C174) \\sim Ueq,
Uanis(C175) \\sim Ueq, Uanis(C225) \\sim Ueq, Uanis(C176) \\sim Ueq,
Uanis(C371) \\sim Ueq, Uanis(C171) \\sim Ueq, Uanis(C172) \\sim Ueq,
Uanis(C170) \\sim Ueq, Uanis(C111) \\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C169)
\\sim Ueq, Uanis(C177) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(F248) \\sim Ueq, Uanis(C132) \\sim Ueq, Uanis(C193) \\sim Ueq,
Uanis(C273) \\sim Ueq, Uanis(C179) \\sim Ueq, Uanis(C142) \\sim Ueq,
Uanis(C138) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C225)=Sof(H225)=FVAR(1)
 Sof(C175)=Sof(H175)=FVAR(2)
 Sof(C174)=Sof(H174)=FVAR(3)
 Sof(C169)=Sof(H169)=FVAR(4)
 Sof(C95)=Sof(H95)=FVAR(5)
 Sof(C170)=Sof(H170)=FVAR(6)
 Sof(C172)=Sof(H172)=FVAR(7)
 Sof(C125)=Sof(H125)=FVAR(8)
 Sof(C126)=Sof(H126)=FVAR(9)
 Sof(C122)=Sof(H122)=FVAR(10)
 Sof(C123)=Sof(H123)=FVAR(11)
 Fixed Sof: F07P(0.7) F09F(0.7) F0A0(0.8) F0AN(0.8) P1B(0.75) F33(0.5)
 F143(0.4) F7(0.3) F1(0.7) F13(0.55) F26(0.6) F27(0.45) F556(0.4) C171(0.5)
 F49(0.45) F671(0.15) F683(0.25) C193(0.25) C179(0.25) H179(0.25) C273(0.25)
 H273(0.25) C142(0.25) H142(0.25) C138(0.25) H138(0.25) C132(0.25) H132(0.25)
 F248(0.1)
6.a Aromatic/amide H refined with riding coordinates:
 C022(H022), C027(H027), C047(H047), C05L(H05L), C02L(H02L), C02H(H02H),
 C02M(H02M), C03A(H03A), C05I(H05I), C03M(H03M), C033(H033), C04K(H04K),
 C04X(H04X), C031(H031), C02N(H02N), C061(H061), C06P(H06P), C058(H058),
 C05A(H05A), C06E(H06E), C03J(H03J), C03Z(H03Z), C05B(H05B), C02Z(H02Z),
 C03R(H03R), C05H(H05H), C05D(H05D), C08V(H08V), C09A(H09A), C053(H053),
 C03O(H03O), C05Z(H05Z), C05M(H05M), C077(H077), C07R(H07R), C063(H063),
 C066(H066), C034(H034), C04N(H04N), C04G(H04G), C06H(H06H), C07M(H07M),
 C06S(H06S), C08O(H08O), C09V(H09V), C07C(H07C), C080(H080), C084(H084),
 C09B(H09B), C09Q(H09Q), C073(H073), C09M(H09M), C0A6(H0A6), C0AC(H0AC),
 C31(H31), C75(H75), C8(H8), C9(H9), C17(H17), C18(H18), C12(H12), C5(H5),
 C6(H6), C15(H15), C16(H16), C20(H20), C19(H19), C14(H14), C11(H11), C10(H10),
 C22(H22), C23(H23), C24(H24), C32(H32), C38(H38), C51(H51), C80(H80),
 C154(H154), C28(H28), C29(H29), C40(H40), C39(H39), C34(H34), C37(H37),
 C62(H62), C90(H90), C44(H44), C36(H36), C42(H42), C43(H43), C46(H46), C47(H47),
  C61(H61), C60(H60), C57(H57), C56(H56), C48(H48), C50(H50), C52(H52),
 C53(H53), C63(H63), C65(H65), C67(H67), C69(H69), C70(H70), C73(H73), C74(H74),
  C77(H77), C84(H84), C83(H83), C81(H81), C79(H79), C87(H87), C93(H93),
 C91(H91), C89(H89), C96(H96), C97(H97), C99(H99), C100(H100), C106(H106),
 C109(H109), C117(H117), C118(H118), C108(H108), C105(H105), C104(H104),
 C119(H119), C120(H120), C103(H103), C112(H112), C101(H101), C116(H116),
 C115(H115), C114(H114), C126(H126), C125(H125), C123(H123), C122(H122),
 C130(H130), C134(H134), C135(H135), C131(H131), C133(H133), C143(H143),
 C141(H141), C139(H139), C137(H137), C150(H150), C151(H151), C152(H152),
 C157(H157), C149(H149), C147(H147), C146(H146), C178(H178), C166(H166),
 C145(H145), C153(H153), C156(H156), C160(H160), C159(H159), C158(H158),
 C162(H162), C167(H167), C165(H165), C163(H163), C25(H25), C26(H26), C58(H58),
 C64(H64), C173(H173), C174(H174), C175(H175), C225(H225), C176(H176),
 C172(H172), C170(H170), C111(H111), C95(H95), C169(H169), C179(H179),
 C273(H273), C142(H142), C138(H138), C132(H132)
6.b Fitted hexagon refined as free rotating group:
 C027(C025,C047,C05L,C04U,C02L), C03A(C039,C05I,C03M,C02Y,C033), C055(C031,
 C02N,C032,C061,C06P), C05A(C06L,C06E,C03J,C020,C03Z), C05B(C05K,C02Z,C03R,C02O,
 C05H), C05D(C08V,C09A,C04Z,C053,C03O), C05Z(C05Y,C05M,C077,C05R,C07R),
 C066(C03X,C034,C04N,C057,C04G), C06H(C03P,C07M,C06S,C08O,C09V), C09Q(C085,C073,
 C09M,C02P,C0A6), C1(C31,C75,C2,C8,C9), C4(C17,C18,C12,C5,C6), C13(C15,C16,C20,
 C19,C14), C11(C7,C10,C22,C23,C24), C30(C32,C38,C51,C80,C154), C27(C28,C29,C40,
 C39,C34), C37(C62,C90,C44,C35,C36), C41(C42,C43,C45,C46,C47), C55(C61,C60,C59,
 C57,C56), C48(C49,C50,C52,C54,C53), C63(C129,C65,C67,C68,C69), C70(C71,C73,C74,
 C76,C77), C86(C84,C83,C82,C81,C79), C87(C93,C92,C91,C89,C88), C94(C96,C97,C98,
 C99,C100), C107(C106,C109,C117,C118,C108), C102(C105,C104,C119,C120,C103),
 C112(C110,C101,C116,C115,C114), C121(C126,C125,C124,C123,C122), C130(C134,C135,
 C131,C133,C128), C136(C143,C141,C140,C139,C137), C148(C150,C151,C152,C157,
 C149), C144(C147,C146,C178,C166,C145), C153(C155,C156,C160,C159,C158),
 C162(C168,C167,C165,C164,C163), C21(C25,C26,C33,C58,C64), C173(C174,C175,C225,
 C176,C371), C171(C172,C170,C111,C95,C169), C193(C179,C273,C142,C138,C132)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              28758
_shelx_hkl_checksum              72614
_shelx_fab_checksum              25359
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '60.0 mm'
_stoe_detector_pixelsize_x       '0.172 mm'
_stoe_detector_pixelsize_y       '0.172 mm'
_stoe_detector_size_x            '8.4 cm'
_stoe_detector_size_y            '10.6 cm'
_stoe_evaluation_integration_a   5.5
_stoe_evaluation_integration_b   -0.6
_stoe_evaluation_integration_ems 0.010
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 93.8
_stoe_evaluation_lana_dxs_max_order 3
_stoe_evaluation_lana_dys_max_order 3
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 140.3
_stoe_evaluation_lana_max_2theta_desired 140.3
_stoe_evaluation_lana_mean_redundancy 2.6
_stoe_evaluation_lana_number_refls_after_or 156108
_stoe_evaluation_lana_number_refls_outliers 15491
_stoe_evaluation_lana_number_refls_total 171599
_stoe_evaluation_lana_number_refls_unique 59668
_stoe_evaluation_lana_number_refls_written 156108
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group -1
_stoe_evaluation_lana_table
;
2Theta          15.2   30.0   44.8   59.6   74.4   89.2  104.0  118.8  133.6
<Resolution>    4.82   2.86   2.00   1.54   1.26   1.10   0.98   0.90   0.85
N(total)        1210   5453  10369  13344  33624  32964  31509  27415  15711
<Redundancy>     2.0    2.2    2.1    1.9    3.5    3.0    2.7    2.4    2.2
Complet. [%%]    90.3   98.7   99.5   98.3   98.4   99.2   97.4   95.3   71.3
<I/sigma>       32.3   25.1   19.6    6.7    4.7    3.0    1.8    1.7    0.9
R(int)         0.076  0.054  0.055  0.083  0.079  0.090  0.155  0.165  0.300
;
_stoe_measurement_identifier     1
_stoe_measurement_max_exposure_per_frame '6.0 s'
_stoe_measurement_mean_exposure_per_frame '4.7 s'
_stoe_measurement_min_exposure_per_frame '1.0 s'
_stoe_measurement_total_exposure_time '2.7 h'
_stoe_measurement_total_frame_number 2070
_stoe_measurement_total_run_number 32
_stoe_measurement_tube_power     '30.0 W'