Structure, optical properties, and catalytic applications of alkynyl-protected M<sub>4</sub>Rh<sub>2</sub> (M = Ag/Au) nanoclusters with atomic precision: a comparative study.
Chen, Leyi; Sun, Fang; Shen, Quanli; Wang, Lei; Liu, Yonggang; Fan, Hao; Tang, Qing; Tang, Zhenghua; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt01326j

data_7713232
_publ_section_title
;
 Structure, optical properties, and catalytic applications of
 alkynyl-protected M<sub>4</sub>Rh<sub>2</sub> (M = Ag/Au) nanoclusters
 with atomic precision: a comparative study.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt01326j
_journal_year                    2023
_chemical_formula_moiety
'C115 H54 Ag4 F49 P2 Rh2, C116 H54 Ag4 F48 P2 Rh2, 5(C7 H8)'
_chemical_formula_sum            'C266 H148 Ag8 F97 P4 Rh4'
_chemical_formula_weight         6585.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-27
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-06-27 deposited with the CCDC.	2023-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.6840(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.0491(3)
_cell_length_b                   29.5409(3)
_cell_length_c                   34.5184(4)
_cell_measurement_reflns_used    32661
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      74.0120
_cell_measurement_theta_min      2.9640
_cell_volume                     25630.3(5)
_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 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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.968
_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    -62.00  35.00   1.00    6.50    --  -41.14  77.00-120.00   97
  2  \w   -109.00 -20.00   1.00    6.50    --  -41.14 -57.00 120.00   89
  3  \w    -33.00  14.00   1.00    9.00    --   41.14 -38.00   0.00   47
  4  \w     41.00 107.00   1.00   30.00    --  107.79-125.00   0.00   66
  5  \w     53.00 118.00   1.00   30.00    --  107.79-125.00-150.00   65
  6  \w     95.00 178.00   1.00   30.00    --  107.79  30.00  60.00   83
  7  \w    142.00 169.00   1.00   30.00    --  107.79 125.00 120.00   27
  8  \w     96.00 121.00   1.00   30.00    --  107.79 125.00 120.00   25
  9  \w     44.00  99.00   1.00   30.00    --  107.79-125.00 -60.00   55
 10  \w    106.00 174.00   1.00   30.00    --  107.79 125.00-150.00   68
 11  \w     37.00 123.00   1.00   30.00    --  107.79 -45.00 -60.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0107613000
_diffrn_orient_matrix_UB_12      -0.0508832000
_diffrn_orient_matrix_UB_13      -0.0027183000
_diffrn_orient_matrix_UB_21      0.0090806000
_diffrn_orient_matrix_UB_22      -0.0055086000
_diffrn_orient_matrix_UB_23      0.0465100000
_diffrn_orient_matrix_UB_31      -0.0596634000
_diffrn_orient_matrix_UB_32      -0.0100356000
_diffrn_orient_matrix_UB_33      -0.0116905000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            108374
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.302
_diffrn_reflns_theta_min         3.003
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.157
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20232
_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            'dark red'
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_description       prism
_exptl_crystal_F_000             12932
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.070
_refine_diff_density_min         -1.573
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3624
_refine_ls_number_reflns         50559
_refine_ls_number_restraints     8282
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0730
_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^)+(0.0656P)^2^+289.6361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1707
_refine_ls_wR_factor_ref         0.1984
_reflns_Friedel_coverage         0.000
_reflns_number_gt                35690
_reflns_number_total             50559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01326j2.cif
_cod_data_source_block           2206b0019
_cod_database_code               7713232
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         AgRhCHFP
_chemical_oxdiff_usercomment     CLY-0518.4
_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
 C215-C27
 1.53 with sigma of 0.02
 C7-F87
 1.35 with sigma of 0.02
 C27-F73
 1.36 with sigma of 0.02
 C27-F37
 1.37 with sigma of 0.02
 C27-F75
 1.35 with sigma of 0.02
 C217-C109
 1.53 with sigma of 0.02
 C109-F19
 1.36 with sigma of 0.02
 C109-F77
 1.37 with sigma of 0.02
 C109-F39
 1.35 with sigma of 0.02
 C219-C55
 1.53 with sigma of 0.02
 C55-F79
 1.36 with sigma of 0.02
 C55-F5
 1.37 with sigma of 0.02
 C55-F81
 1.35 with sigma of 0.02
 C221-C111
 1.53 with sigma of 0.02
 C111-F41
 1.36 with sigma of 0.02
 C111-F83
 1.37 with sigma of 0.02
 C111-F21
 1.35 with sigma of 0.02
 C223-C7
 1.53 with sigma of 0.02
 C7-F85
 1.36 with sigma of 0.02
 C7-F43
 1.37 with sigma of 0.02
 C225-C113
 1.53 with sigma of 0.02
 C113-F11
 1.36 with sigma of 0.02
 C113-F89
 1.37 with sigma of 0.02
 C113-F45
 1.35 with sigma of 0.02
 C227-C57
 1.53 with sigma of 0.02
 C57-F91
 1.36 with sigma of 0.02
 C57-F23
 1.37 with sigma of 0.02
 C57-F93
 1.35 with sigma of 0.02
 C229-C115
 1.53 with sigma of 0.02
 C115-F47
 1.36 with sigma of 0.02
 C115-F95
 1.37 with sigma of 0.02
 C115-F3
 1.35 with sigma of 0.02
 C231-C29
 1.51 with sigma of 0.02
 C29-C233 = C29-C237 = C117-C235
 1.39 with sigma of 0.02
 C233-C117 = C235-C59 = C59-C237
 1.38 with sigma of 0.02
 C119-C239
 1.51 with sigma of 0.02
 C239-C15 = C239-C61 = C241-C121
 1.39 with sigma of 0.02
 C15-C241 = C121-C243 = C243-C61
 1.38 with sigma of 0.02
 C245-C123
 1.51 with sigma of 0.02
 C123-C247 = C123-C251 = C31-C249
 1.39 with sigma of 0.02
 C247-C31 = C249-C125 = C125-C251
 1.38 with sigma of 0.02
 C63-C253
 1.51 with sigma of 0.02
 C253-C127 = C253-C129 = C255-C2
 1.39 with sigma of 0.02
 C127-C255 = C2-C257 = C257-C129
 1.38 with sigma of 0.02
 C259-C65
 1.51 with sigma of 0.02
 C65-C261 = C65-C265 = C131-C263
 1.39 with sigma of 0.02
 C261-C131 = C263-C33 = C33-C265
 1.38 with sigma of 0.02
 C247-C249
 2.39 with sigma of 0.04
 C223-F85 = C223-F87
 2.4 with sigma of 0.04
 C227-F23
 2.38 with sigma of 0.04
 C219-F5
 2.38 with sigma of 0.04
 C119-C15 = C119-C61
 2.52 with sigma of 0.04
 C65-C131
 2.42 with sigma of 0.04
 C215-F37
 2.38 with sigma of 0.04
 C223-F43
 2.38 with sigma of 0.04
 C29-C117
 2.42 with sigma of 0.04
 C241-C243 = C121-C61
 2.4 with sigma of 0.04
 C253-C257
 2.41 with sigma of 0.04
 C217-F77
 2.38 with sigma of 0.04
 C221-F83
 2.38 with sigma of 0.04
 C225-F89
 2.38 with sigma of 0.04
 C229-F95
 2.38 with sigma of 0.04
 C233-C235
 2.39 with sigma of 0.04
 C239-C243
 2.41 with sigma of 0.04
 C123-C31
 2.42 with sigma of 0.04
 C63-C127 = C63-C129
 2.52 with sigma of 0.04
 C255-C257 = C2-C129
 2.4 with sigma of 0.04
 C261-C263
 2.39 with sigma of 0.04
 C215-F73 = C215-F75
 2.4 with sigma of 0.04
 C217-F19 = C217-F39
 2.4 with sigma of 0.04
 C219-F79 = C219-F81
 2.4 with sigma of 0.04
 C221-F41 = C221-F21
 2.4 with sigma of 0.04
 C225-F11 = C225-F45
 2.4 with sigma of 0.04
 C227-F91 = C227-F93
 2.4 with sigma of 0.04
 C229-F47 = C229-F3
 2.4 with sigma of 0.04
 C231-C233 = C231-C237
 2.52 with sigma of 0.04
 C29-C59
 2.41 with sigma of 0.04
 C117-C59 = C235-C237
 2.4 with sigma of 0.04
 C239-C241
 2.42 with sigma of 0.04
 C15-C121
 2.39 with sigma of 0.04
 C245-C247 = C245-C251
 2.52 with sigma of 0.04
 C123-C125
 2.41 with sigma of 0.04
 C31-C125 = C249-C251
 2.4 with sigma of 0.04
 C253-C255
 2.42 with sigma of 0.04
 C127-C2
 2.39 with sigma of 0.04
 C259-C261 = C259-C265
 2.52 with sigma of 0.04
 C65-C33
 2.41 with sigma of 0.04
 C131-C33 = C263-C265
 2.4 with sigma of 0.04
 C65-C33 \\sim C65-C131 \\sim C265-C263 \\sim C261-C265 \\sim C131-C33 \\sim
C261-C263
 with sigma of 0.04
 F85-C7 \\sim F43-C7 \\sim F87-C7
 with sigma of 0.02
 F85-F43 \\sim F43-F87 \\sim F87-F85
 with sigma of 0.04
 F85-C223 \\sim F43-C223 \\sim F87-C223
 with sigma of 0.04
 C223-F87 \\sim C223-F87A
 with sigma of 0.04
 C7-F87 \\sim C7A-F87A
 with sigma of 0.02
 F85-F87 \\sim F85A-F87A
 with sigma of 0.04
 F43-F87 \\sim F43A-F87A
 with sigma of 0.04
 C123-C125 \\sim C123-C31 \\sim C251-C249 \\sim C247-C251 \\sim C31-C125 \\sim
C247-C249
 with sigma of 0.04
 C253-C257 \\sim C253-C255 \\sim C129-C2 \\sim C127-C129 \\sim C255-C257 \\sim
C127-C2
 with sigma of 0.04
 C119-C61 \\sim C119-C15
 with sigma of 0.04
 C245-C251 \\sim C245-C247
 with sigma of 0.04
 C63-C129 \\sim C63-C127
 with sigma of 0.04
 C259-C265 \\sim C259-C261
 with sigma of 0.04
 C123-C247 \\sim C247-C31 \\sim C31-C249 \\sim C249-C125 \\sim C125-C251 \\sim
C251-C123
 with sigma of 0.02
 C253-C127 \\sim C127-C255 \\sim C255-C2 \\sim C2-C257 \\sim C257-C129 \\sim
C129-C253
 with sigma of 0.02
 C65-C261 \\sim C261-C131 \\sim C131-C263 \\sim C263-C33 \\sim C33-C265 \\sim
C265-C65
 with sigma of 0.02
 F73-C27 \\sim F37-C27 \\sim F75-C27
 with sigma of 0.02
 F73-F37 \\sim F37-F75 \\sim F75-F73
 with sigma of 0.04
 F73-C215 \\sim F37-C215 \\sim F75-C215
 with sigma of 0.04
 F19-C109 \\sim F77-C109 \\sim F39-C109
 with sigma of 0.02
 F19-F77 \\sim F77-F39 \\sim F39-F19
 with sigma of 0.04
 F19-C217 \\sim F77-C217 \\sim F39-C217
 with sigma of 0.04
 F79-C55 \\sim F5-C55 \\sim F81-C55
 with sigma of 0.02
 F79-F5 \\sim F5-F81 \\sim F81-F79
 with sigma of 0.04
 F79-C219 \\sim F5-C219 \\sim F81-C219
 with sigma of 0.04
 F41-C111 \\sim F83-C111 \\sim F21-C111
 with sigma of 0.02
 F41-F83 \\sim F83-F21 \\sim F21-F41
 with sigma of 0.04
 F41-C221 \\sim F83-C221 \\sim F21-C221
 with sigma of 0.04
 F11-C113 \\sim F89-C113 \\sim F45-C113
 with sigma of 0.02
 F11-F89 \\sim F89-F45 \\sim F45-F11
 with sigma of 0.04
 F11-C225 \\sim F89-C225 \\sim F45-C225
 with sigma of 0.04
 F91-C57 \\sim F23-C57 \\sim F93-C57
 with sigma of 0.02
 F91-F23 \\sim F23-F93 \\sim F93-F91
 with sigma of 0.04
 F91-C227 \\sim F23-C227 \\sim F93-C227
 with sigma of 0.04
 F47-C115 \\sim F95-C115 \\sim F3-C115
 with sigma of 0.02
 F47-F95 \\sim F95-F3 \\sim F3-F47
 with sigma of 0.04
 F47-C229 \\sim F95-C229 \\sim F3-C229
 with sigma of 0.04
 C29-C233 \\sim C233-C117 \\sim C117-C235 \\sim C235-C59 \\sim C59-C237 \\sim
C237-C29
 with sigma of 0.02
 C29-C59 \\sim C29-C117 \\sim C237-C235 \\sim C233-C237 \\sim C117-C59 \\sim
C233-C235
 with sigma of 0.04
 C231-C237 \\sim C231-C233
 with sigma of 0.04
 C239-C15 \\sim C15-C241 \\sim C241-C121 \\sim C121-C243 \\sim C243-C61 \\sim
C61-C239
 with sigma of 0.02
 C239-C243 \\sim C239-C241 \\sim C61-C121 \\sim C15-C61 \\sim C241-C243 \\sim
C15-C121
 with sigma of 0.04
 C109-F39 \\sim C275-F39A
 with sigma of 0.02
 C217-C109 \\sim C217-C275
 with sigma of 0.02
 C225-C113 \\sim C225-C274
 with sigma of 0.02
 F5-F81 \\sim F5A-F81A
 with sigma of 0.04
 C109-F19 \\sim C275-F19A
 with sigma of 0.02
 C55-F79 \\sim C55A-F79A
 with sigma of 0.02
 C109-F77 \\sim C275-F77A
 with sigma of 0.02
 C113-F45 \\sim C274-F45A
 with sigma of 0.02
 C225-F89 \\sim C225-F89A
 with sigma of 0.04
 C219-F81 \\sim C219-F81A
 with sigma of 0.04
 C225-F11 \\sim C225-F11A
 with sigma of 0.04
 C113-F89 \\sim C274-F89A
 with sigma of 0.02
 F77-F39 \\sim F77A-F39A
 with sigma of 0.04
 C55-F81 \\sim C55A-F81A
 with sigma of 0.02
 C223-C7 \\sim C223-C7A
 with sigma of 0.02
 C225-F45 \\sim C225-F45A
 with sigma of 0.04
 F85-F43 \\sim F85A-F43A
 with sigma of 0.04
 C223-F43 \\sim C223-F43A
 with sigma of 0.04
 F79-F5 \\sim F79A-F5A
 with sigma of 0.04
 C7-F43 \\sim C7A-F43A
 with sigma of 0.02
 F25-C201 \\sim F25A-C276
 with sigma of 0.02
 F19-F39 \\sim F19A-F39A
 with sigma of 0.04
 F11-F45 \\sim F11A-F45A
 with sigma of 0.04
 F11-F89 \\sim F11A-F89A
 with sigma of 0.04
 C217-F39 \\sim C217-F39A
 with sigma of 0.04
 F89-F45 \\sim F89A-F45A
 with sigma of 0.04
 C143-C201 \\sim C143-C276
 with sigma of 0.02
 F19-F77 \\sim F19A-F77A
 with sigma of 0.04
 F69-C201 \\sim F69A-C276
 with sigma of 0.02
 C113-F11 \\sim C274-F11A
 with sigma of 0.02
 F9-C201 \\sim F9A-C276
 with sigma of 0.02
 C219-C55 \\sim C219-C55A
 with sigma of 0.02
 F25-C143 \\sim F25A-C143
 with sigma of 0.04
 C55-F5 \\sim C55A-F5A
 with sigma of 0.02
 F25-F69 \\sim F25A-F69A
 with sigma of 0.04
 F25-F9 \\sim F25A-F9A
 with sigma of 0.04
 C143-F69 \\sim C143-F69A
 with sigma of 0.04
 C219-F79 \\sim C219-F79A
 with sigma of 0.04
 C143-F9 \\sim C143-F9A
 with sigma of 0.04
 C223-F85 \\sim C223-F85A
 with sigma of 0.04
 F69-F9 \\sim F69A-F9A
 with sigma of 0.04
 C219-F5 \\sim C219-F5A
 with sigma of 0.04
 F34-C169 \\sim F34A-C169
 with sigma of 0.02
 F63-C169 \\sim F63A-C169
 with sigma of 0.02
 F79-F81 \\sim F79A-F81A
 with sigma of 0.04
 C169-F65 \\sim C169-F65A
 with sigma of 0.02
 C217-F19 \\sim C217-F19A
 with sigma of 0.04
 C7-F85 \\sim C7A-F85A
 with sigma of 0.02
 C217-F77 \\sim C217-F77A
 with sigma of 0.04
3. Restrained planarity
 C259, C65, C261, C131, C263, C33, C265
 with sigma of 0.1
 C231, C29, C233, C117, C235, C59, C237
 with sigma of 0.1
 C245, C123, C247, C31, C249, C125, C251
 with sigma of 0.1
 C119, C239, C15, C241, C121, C243, C61
 with sigma of 0.1
 C63, C253, C127, C255, C2, C257, C129
 with sigma of 0.1
4. Rigid bond restraints
 C7, F85, F43, F87, C7A, F43A, F87A, F85A, C223
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 C55, F5, F81, C55A, F79A, F5A, F81A, F79, C219
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 C113, F11, F89, F45, C274, F11A, F89A, F45A, C225
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 F25, F69, F9, C201, F25A, F69A, F9A, C276, C143
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 F73, F75, C27, F37
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 F23, C57, F91, F93, C227
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 F75, F73, F37, C27, C215
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 F97, F94, F13, C179, C42
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C223 \\sim C7 \\sim F85 \\sim F43 \\sim F87: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C223 \\sim C7 \\sim F85 \\sim F43 \\sim F87 \\sim C7A \\sim F43A \\sim F87A
\\sim F85A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 1.7A
C229 \\sim C115 \\sim F47 \\sim F95 \\sim F3: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C221 \\sim C111 \\sim F41 \\sim F83 \\sim F21: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C63 \\sim C253 \\sim C127 \\sim C255 \\sim C2 \\sim C257 \\sim C129: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C217 \\sim C109 \\sim F19 \\sim F77 \\sim F39: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C225 \\sim C113 \\sim F11 \\sim F89 \\sim F45: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C119 \\sim C239 \\sim C15 \\sim C241 \\sim C121 \\sim C243 \\sim C61: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C215 \\sim C27 \\sim F73 \\sim F37 \\sim F75: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C219 \\sim C55 \\sim F79 \\sim F5 \\sim F81: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C227 \\sim C57 \\sim F91 \\sim F23 \\sim F93: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C231 \\sim C29 \\sim C233 \\sim C117 \\sim C235 \\sim C59 \\sim C237: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C245 \\sim C123 \\sim C247 \\sim C31 \\sim C249 \\sim C125 \\sim C251: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C259 \\sim C65 \\sim C261 \\sim C131 \\sim C263 \\sim C33 \\sim C265: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C109 \\sim F19 \\sim F77 \\sim C275 \\sim F19A \\sim F39A \\sim F77A \\sim F39
\\sim C217: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 1.7A
C113 \\sim F11 \\sim F89 \\sim F45 \\sim C274 \\sim F11A \\sim F89A \\sim F45A
\\sim C225: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 1.7A
F34 \\sim F63 \\sim C169 \\sim F65 \\sim F34A \\sim F63A \\sim F65A \\sim C100:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
F69 \\sim F9 \\sim C201 \\sim F69A \\sim F9A \\sim C276 \\sim F25 \\sim F25A
\\sim C143: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 1.7A
C55 \\sim F79 \\sim F5 \\sim F81 \\sim C55A \\sim F79A \\sim F5A \\sim F81A
\\sim C219: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 1.7A
C1 \\sim C4 \\sim C6 \\sim C8 \\sim C10 \\sim C12 \\sim C14 \\sim C16 \\sim C18
\\sim C20 \\sim C22 \\sim C24 \\sim C26 \\sim C28 \\sim C30 \\sim C32 \\sim C34
\\sim C36 \\sim C38 \\sim C40 \\sim C42 \\sim C44 \\sim C46 \\sim C48 \\sim C50
\\sim C52 \\sim C54 \\sim C56 \\sim C58 \\sim C60 \\sim C62 \\sim C64 \\sim C66
\\sim C68 \\sim C70 \\sim C72 \\sim C74 \\sim C76 \\sim C78 \\sim C80 \\sim C82
\\sim C84 \\sim C86 \\sim C88 \\sim C90 \\sim C92 \\sim C94 \\sim C96 \\sim C98
\\sim C100 \\sim C102 \\sim C104 \\sim C106 \\sim C108 \\sim C110 \\sim C112
\\sim C114 \\sim C116 \\sim C118 \\sim C120 \\sim C122 \\sim C124 \\sim C126
\\sim C128 \\sim C130 \\sim C132 \\sim C134 \\sim C136 \\sim C138 \\sim C140
\\sim C142 \\sim C144 \\sim C146 \\sim C148 \\sim C150 \\sim C152 \\sim C154
\\sim C156 \\sim C158 \\sim C160 \\sim C162 \\sim C164 \\sim C166 \\sim C168
\\sim C170 \\sim C172 \\sim C174 \\sim C176 \\sim C178 \\sim C180 \\sim C182
\\sim C184 \\sim C186 \\sim C188 \\sim C190 \\sim C192 \\sim C194 \\sim C196
\\sim C198 \\sim C200 \\sim C202 \\sim C204 \\sim C206 \\sim C208 \\sim C210
\\sim C212 \\sim C214 \\sim C216 \\sim C218 \\sim C220 \\sim C222 \\sim C224
\\sim C226 \\sim C228 \\sim C230 \\sim C232 \\sim C234 \\sim C236 \\sim C238
\\sim C240 \\sim C242 \\sim C244 \\sim C246 \\sim C248 \\sim C250 \\sim C252
\\sim C254 \\sim C256 \\sim C258 \\sim C260 \\sim C262 \\sim C264 \\sim C266
\\sim C268 \\sim C270 \\sim C272 \\sim C273 \\sim C137 \\sim C69 \\sim C139
\\sim C35 \\sim C141 \\sim C71 \\sim C143 \\sim C9 \\sim C145 \\sim C73 \\sim
C147 \\sim C37 \\sim C149 \\sim C75 \\sim C151 \\sim C19 \\sim C153 \\sim C77
\\sim C155 \\sim C39 \\sim C157 \\sim C79 \\sim C159 \\sim C5 \\sim C161 \\sim
C81 \\sim C163 \\sim C41 \\sim C165 \\sim C83 \\sim C167 \\sim C21 \\sim C169
\\sim C85 \\sim C171 \\sim C43 \\sim C173 \\sim C87 \\sim C175 \\sim C11 \\sim
C177 \\sim C89 \\sim C179 \\sim C45 \\sim C181 \\sim C91 \\sim C183 \\sim C23
\\sim C185 \\sim C93 \\sim C187 \\sim C47 \\sim C189 \\sim C95 \\sim C191 \\sim
C3 \\sim C193 \\sim C97 \\sim C195 \\sim C49 \\sim C197 \\sim C99 \\sim C199
\\sim C25 \\sim C201 \\sim C101 \\sim C203 \\sim C51 \\sim C205 \\sim C103
\\sim C207 \\sim C13 \\sim C209 \\sim C105 \\sim C211 \\sim C53 \\sim C213
\\sim C107 \\sim C215 \\sim C27 \\sim C217 \\sim C109 \\sim C219 \\sim C55
\\sim C221 \\sim C111 \\sim C223 \\sim C7 \\sim C225 \\sim C113 \\sim C227
\\sim C57 \\sim C229 \\sim C115 \\sim C231 \\sim C29 \\sim C233 \\sim C117
\\sim C235 \\sim C59 \\sim C237 \\sim C119 \\sim C239 \\sim C15 \\sim C241
\\sim C121 \\sim C243 \\sim C61 \\sim C245 \\sim C123 \\sim C247 \\sim C31
\\sim C249 \\sim C125 \\sim C251 \\sim C63 \\sim C253 \\sim C127 \\sim C255
\\sim C2 \\sim C257 \\sim C129 \\sim C259 \\sim C65 \\sim C261 \\sim C131 \\sim
C263 \\sim C33 \\sim C265 \\sim C274 \\sim C55A \\sim C275 \\sim C7A \\sim
C276: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 3.8A
F23 \\sim F93 \\sim F91 \\sim C227 \\sim C57: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 1.7A
F73 \\sim F75 \\sim C27 \\sim F37 \\sim C215: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 1.7A
F94 \\sim F97 \\sim F13 \\sim C179 \\sim C42: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 1.7A
Uanis(F87A) = Uanis(F87)
6. Rigid body (RIGU) restrains
 C223, C7, F85, F43, F87
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C219, C55, F79, F5, F81
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, F85, F43, F87, C7A, F43A, F87A, F85A, C223
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C245, C123, C247, C31, C249, C125, C251
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C227, C57, F91, F23, F93
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C215, C27, F73, F37, F75
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C231, C29, C233, C117, C235, C59, C237
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C259, C65, C261, C131, C263, C33, C265
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C217, C109, F19, F77, F39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C221, C111, F41, F83, F21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C225, C113, F11, F89, F45
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C229, C115, F47, F95, F3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C119, C239, C15, C241, C121, C243, C61
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C63, C253, C127, C255, C2, C257, C129
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C109, F19, F77, F39, C275, F19A, F39A, F77A, C217
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 F11, F89, F45, C274, F11A, F89A, F45A, C113, C225
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 F34, F63, C169, F65, F34A, F63A, F65A, C100
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 F27, F57, C5, F35, C105
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 C57, F91, F93, F23, C227
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 F94, F97, F13, C179, C42
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 F75, C27, F37, F73, C215
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
7. Others
 Sof(C274)=Sof(F11A)=Sof(F89A)=Sof(F45A)=1-FVAR(1)
 Sof(C113)=Sof(F11)=Sof(F89)=Sof(F45)=FVAR(1)
 Sof(C55A)=Sof(F79A)=Sof(F5A)=Sof(F81A)=1-FVAR(2)
 Sof(C55)=Sof(F79)=Sof(F5)=Sof(F81)=FVAR(2)
 Sof(C275)=Sof(F19A)=Sof(F39A)=Sof(F77A)=1-FVAR(3)
 Sof(C109)=Sof(F19)=Sof(F77)=Sof(F39)=FVAR(3)
 Sof(C7A)=Sof(F43A)=Sof(F87A)=Sof(F85A)=1-FVAR(4)
 Sof(C7)=Sof(F85)=Sof(F43)=Sof(F87)=FVAR(4)
 Sof(F25A)=Sof(F69A)=Sof(F9A)=Sof(C276)=1-FVAR(5)
 Sof(F25)=Sof(F69)=Sof(F9)=Sof(C201)=FVAR(5)
 Sof(F34A)=Sof(F63A)=Sof(F65A)=1-FVAR(6)
 Sof(F34)=Sof(F63)=Sof(F65)=FVAR(6)
8.a Aromatic/amide H refined with riding coordinates:
 C38(H38), C50(H50), C54(H54), C56(H56), C86(H86), C88(H88), C94(H94),
 C98(H98), C102(H102), C104(H104), C106(H106), C108(H108), C110(H110),
 C112(H112), C114(H114), C118(H118), C120(H120), C122(H122), C126(H126),
 C128(H128), C130(H130), C132(H132), C140(H140), C144(H144), C146(H146),
 C148(H148), C150(H150), C152(H152), C156(H156), C158(H158), C162(H162),
 C164(H164), C166(H166), C168(H168), C172(H172), C174(H174), C180(H180),
 C182(H182), C184(H184), C186(H186), C188(H188), C196(H196), C202(H202),
 C204(H204), C210(H210), C212(H212), C216(H216), C220(H220), C222(H222),
 C224(H224), C226(H226), C228(H228), C230(H230), C232(H232), C234(H234),
 C236(H236), C238(H238), C240(H240), C242(H242), C244(H244), C246(H246),
 C248(H248), C250(H250), C252(H252), C258(H258), C260(H260), C262(H262),
 C264(H264), C266(H266), C270(H270), C69(H69), C139(H139), C71(H71), C9(H9),
 C145(H145), C37(H37), C151(H151), C19(H19), C153(H153), C39(H39), C79(H79),
 C161(H161), C165(H165), C83(H83), C167(H167), C21(H21), C171(H171), C43(H43),
 C173(H173), C87(H87), C11(H11), C177(H177), C89(H89), C45(H45), C181(H181),
 C91(H91), C23(H23), C185(H185), C187(H187), C47(H47), C189(H189), C97(H97),
 C99(H99), C25(H25), C101(H101), C103(H103), C13(H13), C107(H107), C233(H233),
 C117(H117), C235(H235), C59(H59), C237(H237), C15(H15), C241(H241), C121(H121),
  C243(H243), C61(H61), C247(H247), C31(H31), C249(H249), C125(H125),
 C251(H251), C127(H127), C255(H255), C2(H2), C257(H257), C129(H129), C261(H261),
  C131(H131), C263(H263), C33(H33), C265(H265)
8.b Idealised Me refined as rotating group:
 C231(H23A,H23B,H23C), C119(H11A,H11B,H11C), C245(H24A,H24B,H24C), C63(H63A,
 H63B,H63C), C259(H25A,H25B,H25C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              2497
_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 2.446
_oxdiff_exptl_absorpt_empirical_full_min 0.532