Stepwise reduction of an asymmetric π-expanded pyracylene towards the crystalline radical trianion.
Zhu, Yikun; Borstelmann, Jan; Neiss, Christian; Wei, Zheng; Görling, Andreas; Kivala, Milan; Petrukhina, Marina A.; Chemical science 16 (2025) 3211–3217; doi:10.1039/d4sc08255a

data_1573688
_publ_section_title
;
 Stepwise reduction of an asymmetric &#x3c0;-expanded pyracylene towards
 the crystalline radical trianion.
;
_journal_issue                   7
_journal_name_full               'Chemical science'
_journal_page_first              3211
_journal_page_last               3217
_journal_paper_doi               10.1039/d4sc08255a
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C126 H150 O12 Rb2, 2.5(C4 H8 O)'
_chemical_formula_sum            'C136 H170 O14.5 Rb2'
_chemical_formula_weight         2207.65
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-12-13
_audit_creation_method
;
Olex2 1.5-ac6-012
(compiled 2023.08.24 svn.re1ec1418 for Rigaku Oxford Diffraction, GUI svn.r6817)
;
_audit_update_record
;
2024-10-18 deposited with the CCDC.	2025-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   27.49950(10)
_cell_length_b                   27.49950(10)
_cell_length_c                   70.8136(5)
_cell_measurement_reflns_used    33472
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      78.6370
_cell_measurement_theta_min      2.4570
_cell_volume                     53550.8(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.100a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.100a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.100a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac6-012 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-012 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.967
_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    -76.00  16.72   0.38   10.00    --  -49.93 101.00 -72.00  244
  2  \w    109.00 168.66   0.38   40.00    --  111.50 101.00 -72.00  157
  3  \w    107.00 131.70   0.38   40.00    --  111.50  61.00 -90.00   65
  4  \w    140.00 166.22   0.38   40.00    --  111.50  61.00 -90.00   69
  5  \w    -19.00  16.72   0.38   10.00    --  -49.93  19.00 -60.00   94
  6  \w    104.00 175.82   0.38   40.00    --  111.50  15.00-150.00  189
  7  \w     48.00  74.22   0.38   40.00    --  111.50 -61.00 -90.00   69
  8  \w     41.00  66.08   0.38   40.00    --  111.50 -61.00 -60.00   66
  9  \w     42.00  67.08   0.38   40.00    --  111.50 -61.00 -30.00   66
 10  \w     62.00  87.08   0.38   40.00    --  111.50 -77.00-180.00   66
 11  \w     56.00  94.00   0.38   40.00    --  111.50-140.00 116.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0077212000
_diffrn_orient_matrix_UB_12      -0.0464832000
_diffrn_orient_matrix_UB_13      -0.0117997000
_diffrn_orient_matrix_UB_21      -0.0149203000
_diffrn_orient_matrix_UB_22      0.0312657000
_diffrn_orient_matrix_UB_23      -0.0170859000
_diffrn_orient_matrix_UB_31      0.0534418000
_diffrn_orient_matrix_UB_32      0.0020149000
_diffrn_orient_matrix_UB_33      -0.0065014000
_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  0.0330
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       90
_diffrn_reflns_limit_l_min       -71
_diffrn_reflns_number            105590
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.714
_diffrn_reflns_theta_min         2.592
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.385
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.100a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             18816
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1890
_refine_ls_number_reflns         28218
_refine_ls_number_restraints     2226
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0771P)^2^+35.8776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1452
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21953
_reflns_number_total             28218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08255a2.cif
_cod_data_source_block           Rb_1_2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1573686--1573688.cif.
;
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'C136 H170 O14.50 Rb2'
_cod_database_code               1573688
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C H O Rb'
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.809
_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
 C54-C79 = C80-C79 = C79-C42
 1.54 with sigma of 0.02
 C52-C167 = C148-C37 = C148-C150 = C124-C167 = C89-C148 = C130-C167
 1.54 with sigma of 0.02
 C135-C132 = C132-C55 = C81-C132
 1.54 with sigma of 0.02
 C129-C35 = C129-C133 = C134-C129
 1.54 with sigma of 0.02
 C129-C133 = C166-C64 = C166-C99 = C168-C166 = C129-C35 = C134-C129
 1.54 with sigma of 0.02
 C141-C139 = C85-C141 = C56-C141 = C80-C79 = C79-C54 = C79-C42
 1.54 with sigma of 0.02
 C128-C158 \\sim C128-C136
 with sigma of 0.02
 C158-C27 \\sim C136-C84
 with sigma of 0.02
 C158-C69 \\sim C136-C82
 with sigma of 0.02
 C27-C71 \\sim C84-C138
 with sigma of 0.02
 C69-C122 \\sim C82-C137
 with sigma of 0.02
 C71-C50 \\sim C138-C31
 with sigma of 0.02
 C50-C122 \\sim C31-C137
 with sigma of 0.02
 C50-C79 \\sim C31-C141
 with sigma of 0.02
 C79-C54 \\sim C141-C85
 with sigma of 0.02
 C79-C80 \\sim C141-C139
 with sigma of 0.02
 C79-C42 \\sim C141-C56
 with sigma of 0.02
 C128-C27 \\sim C128-C84
 with sigma of 0.04
 C128-C69 \\sim C128-C82
 with sigma of 0.04
 C158-C71 \\sim C136-C138
 with sigma of 0.04
 C158-C122 \\sim C136-C137
 with sigma of 0.04
 C27-C69 \\sim C84-C82
 with sigma of 0.04
 C27-C50 \\sim C84-C31
 with sigma of 0.04
 C69-C50 \\sim C82-C31
 with sigma of 0.04
 C71-C122 \\sim C138-C137
 with sigma of 0.04
 C71-C79 \\sim C138-C141
 with sigma of 0.04
 C50-C54 \\sim C31-C85
 with sigma of 0.04
 C50-C80 \\sim C31-C139
 with sigma of 0.04
 C50-C42 \\sim C31-C56
 with sigma of 0.04
 C122-C79 \\sim C137-C141
 with sigma of 0.04
 C54-C80 \\sim C85-C139
 with sigma of 0.04
 C54-C42 \\sim C85-C56
 with sigma of 0.04
 C80-C42 \\sim C139-C56
 with sigma of 0.04
 C74-C106 \\sim C74-C58
 with sigma of 0.02
 C94-C1 \\sim C87-C146
 with sigma of 0.02
 C94-C3 \\sim C87-C144
 with sigma of 0.02
 C106-C1 \\sim C58-C146
 with sigma of 0.02
 C106-C12 \\sim C58-C143
 with sigma of 0.02
 C3-C167 \\sim C144-C148
 with sigma of 0.02
 C3-C73 \\sim C144-C43
 with sigma of 0.02
 C167-C124 \\sim C148-C150
 with sigma of 0.02
 C167-C52 \\sim C148-C37
 with sigma of 0.02
 C167-C130 \\sim C148-C89
 with sigma of 0.02
 C12-C73 \\sim C143-C43
 with sigma of 0.02
 C74-C1 \\sim C74-C146
 with sigma of 0.04
 C74-C12 \\sim C74-C143
 with sigma of 0.04
 C94-C106 \\sim C87-C58
 with sigma of 0.04
 C94-C167 \\sim C87-C148
 with sigma of 0.04
 C94-C73 \\sim C87-C43
 with sigma of 0.04
 C106-C73 \\sim C58-C43
 with sigma of 0.04
 C1-C3 \\sim C146-C144
 with sigma of 0.04
 C1-C12 \\sim C146-C143
 with sigma of 0.04
 C3-C12 \\sim C144-C143
 with sigma of 0.04
 C3-C124 \\sim C144-C150
 with sigma of 0.04
 C3-C52 \\sim C144-C37
 with sigma of 0.04
 C3-C130 \\sim C144-C89
 with sigma of 0.04
 C167-C73 \\sim C148-C43
 with sigma of 0.04
 C124-C52 \\sim C150-C37
 with sigma of 0.04
 C124-C130 \\sim C150-C89
 with sigma of 0.04
 C52-C130 \\sim C37-C89
 with sigma of 0.04
 C116-C77 \\sim C91-C153
 with sigma of 0.02
 C118-C75 \\sim C60-C155
 with sigma of 0.02
 C118-C77 \\sim C60-C153
 with sigma of 0.02
 C118-C132 \\sim C60-C157
 with sigma of 0.02
 C75-C126 \\sim C155-C93
 with sigma of 0.02
 C132-C81 \\sim C157-C159
 with sigma of 0.02
 C132-C135 \\sim C157-C95
 with sigma of 0.02
 C132-C55 \\sim C157-C44
 with sigma of 0.02
 C127-C116 \\sim C127-C91
 with sigma of 0.04
 C127-C126 \\sim C127-C93
 with sigma of 0.04
 C116-C118 \\sim C91-C60
 with sigma of 0.04
 C116-C126 \\sim C91-C93
 with sigma of 0.04
 C118-C126 \\sim C60-C93
 with sigma of 0.04
 C118-C81 \\sim C60-C159
 with sigma of 0.04
 C118-C135 \\sim C60-C95
 with sigma of 0.04
 C118-C55 \\sim C60-C44
 with sigma of 0.04
 C75-C77 \\sim C155-C153
 with sigma of 0.04
 C75-C132 \\sim C155-C157
 with sigma of 0.04
 C77-C132 \\sim C153-C157
 with sigma of 0.04
 C81-C135 \\sim C159-C95
 with sigma of 0.04
 C81-C55 \\sim C159-C44
 with sigma of 0.04
 C135-C55 \\sim C95-C44
 with sigma of 0.04
 C133-C134 \\sim C134-C35 \\sim C35-C133
 with sigma of 0.02
 C83-C109 \\sim C161-C109
 with sigma of 0.02
 C83-C151 \\sim C161-C33
 with sigma of 0.02
 C83-C175 \\sim C161-C62
 with sigma of 0.02
 C151-C165 \\sim C33-C164
 with sigma of 0.02
 C165-C22 \\sim C164-C97
 with sigma of 0.02
 C22-C185 \\sim C97-C162
 with sigma of 0.02
 C22-C129 \\sim C97-C166
 with sigma of 0.02
 C175-C185 \\sim C62-C162
 with sigma of 0.02
 C129-C35 \\sim C166-C168
 with sigma of 0.02
 C129-C133 \\sim C166-C64
 with sigma of 0.02
 C129-C134 \\sim C166-C99
 with sigma of 0.02
 C83-C165 \\sim C161-C164
 with sigma of 0.04
 C83-C185 \\sim C161-C162
 with sigma of 0.04
 C109-C151 \\sim C109-C33
 with sigma of 0.04
 C109-C175 \\sim C109-C62
 with sigma of 0.04
 C151-C22 \\sim C33-C97
 with sigma of 0.04
 C151-C175 \\sim C33-C62
 with sigma of 0.04
 C165-C185 \\sim C164-C162
 with sigma of 0.04
 C165-C129 \\sim C164-C166
 with sigma of 0.04
 C22-C175 \\sim C97-C62
 with sigma of 0.04
 C22-C35 \\sim C97-C168
 with sigma of 0.04
 C22-C133 \\sim C97-C64
 with sigma of 0.04
 C22-C134 \\sim C97-C99
 with sigma of 0.04
 C185-C129 \\sim C162-C166
 with sigma of 0.04
 C35-C133 \\sim C168-C64
 with sigma of 0.04
 C35-C134 \\sim C168-C99
 with sigma of 0.04
 C133-C134 \\sim C64-C99
 with sigma of 0.04
 C10-C156 \\sim C10-C170
 with sigma of 0.02
 C156-C114 \\sim C170-C171
 with sigma of 0.02
 C156-C120 \\sim C170-C101
 with sigma of 0.02
 C156-C131 \\sim C170-C46
 with sigma of 0.02
 C10-C114 \\sim C10-C171
 with sigma of 0.04
 C10-C120 \\sim C10-C101
 with sigma of 0.04
 C10-C131 \\sim C10-C46
 with sigma of 0.04
 C114-C120 \\sim C171-C101
 with sigma of 0.04
 C114-C131 \\sim C171-C46
 with sigma of 0.04
 C120-C131 \\sim C101-C46
 with sigma of 0.04
 O1-C9 \\sim O2-C173
 with sigma of 0.02
 O1-C20 \\sim O2-C103
 with sigma of 0.02
 O17-C21 \\sim O15-C66
 with sigma of 0.02
 O17-C179 \\sim O15-C39
 with sigma of 0.02
 O3-C172 \\sim O9-C105
 with sigma of 0.02
 O3-C177 \\sim O9-C178
 with sigma of 0.02
 O11-C163 \\sim O16-C176
 with sigma of 0.02
 O11-C25 \\sim O16-C180
 with sigma of 0.02
 O7-C184 \\sim O5-C107
 with sigma of 0.02
 O7-C40 \\sim O5-C68
 with sigma of 0.02
 O13-C160 \\sim O18-C174
 with sigma of 0.02
 O13-C112 \\sim O18-C181
 with sigma of 0.02
 C9-C177 \\sim C173-C178
 with sigma of 0.02
 C20-C21 \\sim C103-C66
 with sigma of 0.02
 C160-C25 \\sim C174-C180
 with sigma of 0.02
 C163-C179 \\sim C176-C39
 with sigma of 0.02
 C172-C184 \\sim C105-C107
 with sigma of 0.02
 C112-C40 \\sim C181-C68
 with sigma of 0.02
 O1-O17 \\sim O2-O15
 with sigma of 0.04
 O1-O3 \\sim O2-O9
 with sigma of 0.04
 O1-O11 \\sim O2-O16
 with sigma of 0.04
 O1-C59 \\sim O2-C59
 with sigma of 0.04
 O1-O7 \\sim O2-O5
 with sigma of 0.04
 O1-O13 \\sim O2-O18
 with sigma of 0.04
 O1-C76 \\sim O2-C76
 with sigma of 0.04
 O1-C86 \\sim O2-C86
 with sigma of 0.04
 O1-C90 \\sim O2-C90
 with sigma of 0.04
 O1-C26 \\sim O2-C26
 with sigma of 0.04
 O1-C111 \\sim O2-C111
 with sigma of 0.04
 O1-C21 \\sim O2-C66
 with sigma of 0.04
 O1-C177 \\sim O2-C178
 with sigma of 0.04
 O17-O3 \\sim O15-O9
 with sigma of 0.04
 O17-O11 \\sim O15-O16
 with sigma of 0.04
 O17-C59 \\sim O15-C59
 with sigma of 0.04
 O17-O7 \\sim O15-O5
 with sigma of 0.04
 O17-O13 \\sim O15-O18
 with sigma of 0.04
 O17-C76 \\sim O15-C76
 with sigma of 0.04
 O17-C86 \\sim O15-C86
 with sigma of 0.04
 O17-C90 \\sim O15-C90
 with sigma of 0.04
 O17-C26 \\sim O15-C26
 with sigma of 0.04
 O17-C111 \\sim O15-C111
 with sigma of 0.04
 O17-C20 \\sim O15-C103
 with sigma of 0.04
 O17-C163 \\sim O15-C176
 with sigma of 0.04
 O3-O11 \\sim O9-O16
 with sigma of 0.04
 O3-C59 \\sim O9-C59
 with sigma of 0.04
 O3-O7 \\sim O9-O5
 with sigma of 0.04
 O3-O13 \\sim O9-O18
 with sigma of 0.04
 O3-C76 \\sim O9-C76
 with sigma of 0.04
 O3-C86 \\sim O9-C86
 with sigma of 0.04
 O3-C90 \\sim O9-C90
 with sigma of 0.04
 O3-C26 \\sim O9-C26
 with sigma of 0.04
 O3-C111 \\sim O9-C111
 with sigma of 0.04
 O3-C9 \\sim O9-C173
 with sigma of 0.04
 O3-C184 \\sim O9-C107
 with sigma of 0.04
 O11-C59 \\sim O16-C59
 with sigma of 0.04
 O11-O7 \\sim O16-O5
 with sigma of 0.04
 O11-O13 \\sim O16-O18
 with sigma of 0.04
 O11-C76 \\sim O16-C76
 with sigma of 0.04
 O11-C86 \\sim O16-C86
 with sigma of 0.04
 O11-C90 \\sim O16-C90
 with sigma of 0.04
 O11-C26 \\sim O16-C26
 with sigma of 0.04
 O11-C111 \\sim O16-C111
 with sigma of 0.04
 O11-C160 \\sim O16-C174
 with sigma of 0.04
 O11-C179 \\sim O16-C39
 with sigma of 0.04
 C59-O7 \\sim C59-O5
 with sigma of 0.04
 C59-O13 \\sim C59-O18
 with sigma of 0.04
 O7-O13 \\sim O5-O18
 with sigma of 0.04
 O7-C76 \\sim O5-C76
 with sigma of 0.04
 O7-C86 \\sim O5-C86
 with sigma of 0.04
 O7-C90 \\sim O5-C90
 with sigma of 0.04
 O7-C26 \\sim O5-C26
 with sigma of 0.04
 O7-C111 \\sim O5-C111
 with sigma of 0.04
 O7-C172 \\sim O5-C105
 with sigma of 0.04
 O7-C112 \\sim O5-C181
 with sigma of 0.04
 O13-C76 \\sim O18-C76
 with sigma of 0.04
 O13-C86 \\sim O18-C86
 with sigma of 0.04
 O13-C90 \\sim O18-C90
 with sigma of 0.04
 O13-C26 \\sim O18-C26
 with sigma of 0.04
 O13-C111 \\sim O18-C111
 with sigma of 0.04
 O13-C25 \\sim O18-C180
 with sigma of 0.04
 O13-C40 \\sim O18-C68
 with sigma of 0.04
 C9-C20 \\sim C173-C103
 with sigma of 0.04
 C160-C112 \\sim C174-C181
 with sigma of 0.04
 C21-C179 \\sim C66-C39
 with sigma of 0.04
 C163-C25 \\sim C176-C180
 with sigma of 0.04
 C172-C177 \\sim C105-C178
 with sigma of 0.04
 C184-C40 \\sim C107-C68
 with sigma of 0.04
 C125-C154 \\sim C125-C108
 with sigma of 0.02
 C154-C23 \\sim C108-C182
 with sigma of 0.02
 C154-C29 \\sim C108-C48
 with sigma of 0.02
 C154-C110 \\sim C108-C183
 with sigma of 0.02
 C125-C23 \\sim C125-C182
 with sigma of 0.04
 C125-C29 \\sim C125-C48
 with sigma of 0.04
 C125-C110 \\sim C125-C183
 with sigma of 0.04
 C23-C29 \\sim C182-C48
 with sigma of 0.04
 C23-C110 \\sim C182-C183
 with sigma of 0.04
 C29-C110 \\sim C48-C183
 with sigma of 0.04
 Rb2-O1 \\sim Rb2X-O1
 with sigma of 0.02
 Rb2-O17 \\sim Rb2X-O17
 with sigma of 0.02
 Rb2-O3 \\sim Rb2X-O3
 with sigma of 0.02
 Rb2-O11 \\sim Rb2X-O11
 with sigma of 0.02
 Rb2-O7 \\sim Rb2X-O7
 with sigma of 0.02
 Rb2-O13 \\sim Rb2X-O13
 with sigma of 0.02
 Rb2-O2 \\sim Rb2X-O2
 with sigma of 0.02
 Rb2-O15 \\sim Rb2X-O15
 with sigma of 0.02
 Rb2-O9 \\sim Rb2X-O9
 with sigma of 0.02
 Rb2-O16 \\sim Rb2X-O16
 with sigma of 0.02
 Rb2-O5 \\sim Rb2X-O5
 with sigma of 0.02
 Rb2-O18 \\sim Rb2X-O18
 with sigma of 0.02
 Rb2-H39A \\sim Rb2X-H39A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C158 \\sim C27 \\sim C69 \\sim C71 \\sim C50 \\sim C122 \\sim C79 \\sim C54
\\sim C80 \\sim C42 \\sim C136 \\sim C82 \\sim C137 \\sim C31 \\sim C138 \\sim
C84 \\sim C139 \\sim C56 \\sim C141 \\sim C85: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C94 \\sim C106 \\sim C1 \\sim C3 \\sim C167 \\sim C12 \\sim C73 \\sim C124
\\sim C52 \\sim C130 \\sim C143 \\sim C43 \\sim C144 \\sim C87 \\sim C146 \\sim
C58 \\sim C148 \\sim C89 \\sim C150 \\sim C37: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C116 \\sim C118 \\sim C75 \\sim C126 \\sim C77 \\sim C132 \\sim C81 \\sim C135
\\sim C55 \\sim C152 \\sim C91 \\sim C153 \\sim C60 \\sim C155 \\sim C93 \\sim
C157 \\sim C44 \\sim C159 \\sim C95: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C83 \\sim C151 \\sim C165 \\sim C22 \\sim C175 \\sim C185 \\sim C129 \\sim C35
\\sim C133 \\sim C134 \\sim C161 \\sim C62 \\sim C162 \\sim C97 \\sim C164
\\sim C33 \\sim C166 \\sim C99 \\sim C168 \\sim C64: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C156 \\sim C114 \\sim C120 \\sim C131 \\sim C170 \\sim C101 \\sim C171 \\sim
C46: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O1 \\sim O17 \\sim O3 \\sim O11 \\sim O7 \\sim O13 \\sim C9 \\sim C20 \\sim
C160 \\sim C21 \\sim C163 \\sim C172 \\sim C177 \\sim C179 \\sim C25 \\sim C184
\\sim C112 \\sim C40 \\sim O2 \\sim O15 \\sim O9 \\sim O16 \\sim O5 \\sim O18
\\sim C173 \\sim C103 \\sim C174 \\sim C66 \\sim C176 \\sim C105 \\sim C178
\\sim C39 \\sim C180 \\sim C107 \\sim C181 \\sim C68: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C154 \\sim C23 \\sim C29 \\sim C110 \\sim C182 \\sim C108 \\sim C183 \\sim C48:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(Rb2X) = Uanis(Rb2)
Uanis(C168) = Uanis(C133)
4. Others
 Sof(C136)=Sof(C82)=Sof(H82)=Sof(C137)=Sof(H137)=Sof(C31)=Sof(C138)=Sof(H138)=
 Sof(C84)=Sof(H84)=Sof(C139)=Sof(H13R)=Sof(H13S)=Sof(H13T)=Sof(C56)=Sof(H56A)=
 Sof(H56B)=Sof(H56C)=Sof(C141)=Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(H85C)=1-FVAR(1)
 Sof(C158)=Sof(C27)=Sof(H27)=Sof(C69)=Sof(H69)=Sof(C71)=Sof(H71)=Sof(C50)=
 Sof(C122)=Sof(H122)=Sof(C79)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=Sof(C80)=
 Sof(H80A)=Sof(H80B)=Sof(H80C)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(1)
 Sof(C143)=Sof(H143)=Sof(C43)=Sof(H43)=Sof(C144)=Sof(C87)=Sof(H87)=Sof(C146)=
 Sof(H146)=Sof(C58)=Sof(C148)=Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(H89C)=Sof(C150)=
 Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=1-FVAR(2)
 Sof(C94)=Sof(H94)=Sof(C106)=Sof(C1)=Sof(H1)=Sof(C3)=Sof(C167)=Sof(C12)=
 Sof(H12)=Sof(C73)=Sof(H73)=Sof(C124)=Sof(H12F)=Sof(H12G)=Sof(H12H)=Sof(C52)=
 Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C130)=Sof(H13C)=Sof(H13D)=Sof(H13E)=FVAR(2)
 Sof(C91)=Sof(H91)=Sof(C153)=Sof(H153)=Sof(C60)=Sof(C155)=Sof(H155)=Sof(C93)=
 Sof(H93)=Sof(C157)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C159)=Sof(H15D)=
 Sof(H15E)=Sof(H15F)=Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(H95C)=1-FVAR(3)
 Sof(C116)=Sof(H116)=Sof(C118)=Sof(C75)=Sof(H75)=Sof(C126)=Sof(H126)=Sof(C77)=
 Sof(H77)=Sof(C132)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=Sof(C135)=Sof(H13O)=
 Sof(H13P)=Sof(H13Q)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=FVAR(3)
 Sof(C161)=Sof(C62)=Sof(H62)=Sof(C162)=Sof(H162)=Sof(C97)=Sof(C164)=Sof(H164)=
 Sof(C33)=Sof(H33)=Sof(C166)=Sof(C99)=Sof(H99A)=Sof(H99B)=Sof(H99C)=Sof(C168)=
 Sof(H16H)=Sof(H16I)=Sof(H16J)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=1-FVAR(4)
 Sof(C83)=Sof(C151)=Sof(H151)=Sof(C165)=Sof(H165)=Sof(C22)=Sof(C175)=Sof(H175)=
 Sof(C185)=Sof(H185)=Sof(C129)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C133)=
 Sof(H13I)=Sof(H13J)=Sof(H13K)=Sof(C134)=Sof(H13L)=Sof(H13M)=Sof(H13N)=FVAR(4)
 Sof(C170)=Sof(C101)=Sof(H10G)=Sof(H10H)=Sof(H10I)=Sof(C171)=Sof(H17G)=
 Sof(H17H)=Sof(H17I)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=1-FVAR(5)
 Sof(C156)=Sof(C114)=Sof(H11H)=Sof(H11I)=Sof(H11J)=Sof(C120)=Sof(H12C)=
 Sof(H12D)=Sof(H12E)=Sof(C131)=Sof(H13F)=Sof(H13G)=Sof(H13H)=FVAR(5)
 Sof(O2)=Sof(O15)=Sof(O9)=Sof(O16)=Sof(O5)=Sof(O18)=Sof(C173)=Sof(H17J)=
 Sof(H17K)=Sof(C103)=Sof(H10J)=Sof(H10K)=Sof(C174)=Sof(H17L)=Sof(H17M)=Sof(C66)=
 Sof(H66A)=Sof(H66B)=Sof(C176)=Sof(H17N)=Sof(H17O)=Sof(C105)=Sof(H10L)=
 Sof(H10M)=Sof(C178)=Sof(H17P)=Sof(H17Q)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C180)=
 Sof(H18C)=Sof(H18D)=Sof(C107)=Sof(H10N)=Sof(H10O)=Sof(C181)=Sof(H18E)=
 Sof(H18F)=Sof(C68)=Sof(H68A)=Sof(H68B)=1-FVAR(6)
 Sof(O1)=Sof(O17)=Sof(O3)=Sof(O11)=Sof(O7)=Sof(O13)=Sof(C9)=Sof(H9A)=Sof(H9B)=
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C160)=Sof(H16A)=Sof(H16B)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(C163)=Sof(H16C)=Sof(H16D)=Sof(C172)=Sof(H17A)=Sof(H17B)=
 Sof(C177)=Sof(H17C)=Sof(H17D)=Sof(C179)=Sof(H17E)=Sof(H17F)=Sof(C25)=Sof(H25A)=
 Sof(H25B)=Sof(C184)=Sof(H18A)=Sof(H18B)=Sof(C112)=Sof(H11F)=Sof(H11G)=Sof(C40)=
 Sof(H40A)=Sof(H40B)=FVAR(6)
 Sof(C182)=Sof(H18G)=Sof(H18H)=Sof(H18I)=Sof(C108)=Sof(C183)=Sof(H18J)=
 Sof(H18K)=Sof(H18L)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=1-FVAR(7)
 Sof(C154)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C29)=Sof(H29A)=Sof(H29B)=
 Sof(H29C)=Sof(C110)=Sof(H11C)=Sof(H11D)=Sof(H11E)=FVAR(7)
 Sof(Rb2X)=1-FVAR(8)
 Sof(Rb2)=FVAR(8)
5.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C7(H7A,H7B), C92(H92A,H92B), C96(H96A,H96B), C100(H10A,H10B),
 C102(H10C,H10D), C104(H10E,H10F), C115(H11A,H11B), C121(H12A,H12B), C8(H8A,
 H8B), C9(H9A,H9B), C13(H13A,H13B), C142(H14D,H14E), C20(H20A,H20B), C160(H16A,
 H16B), C21(H21A,H21B), C163(H16C,H16D), C172(H17A,H17B), C177(H17C,H17D),
 C179(H17E,H17F), C25(H25A,H25B), C184(H18A,H18B), C112(H11F,H11G), C40(H40A,
 H40B), C173(H17J,H17K), C103(H10J,H10K), C174(H17L,H17M), C66(H66A,H66B),
 C176(H17N,H17O), C105(H10L,H10M), C178(H17P,H17Q), C39(H39A,H39B), C180(H18C,
 H18D), C107(H10N,H10O), C181(H18E,H18F), C68(H68A,H68B)
5.b Me refined with riding coordinates:
 C23(H23A,H23B,H23C), C29(H29A,H29B,H29C), C110(H11C,H11D,H11E)
5.c Aromatic/amide H refined with riding coordinates:
 C34(H34), C17(H17), C19(H19), C47(H47), C61(H61), C65(H65), C14(H14),
 C88(H88), C90(H90), C94(H94), C111(H111), C117(H117), C123(H123), C1(H1),
 C18(H18), C11(H11), C151(H151), C165(H165), C175(H175), C27(H27), C185(H185),
 C69(H69), C12(H12), C71(H71), C116(H116), C73(H73), C122(H122), C75(H75),
 C126(H126), C77(H77), C82(H82), C137(H137), C138(H138), C84(H84), C143(H143),
 C43(H43), C87(H87), C146(H146), C91(H91), C153(H153), C155(H155), C93(H93),
 C62(H62), C162(H162), C164(H164), C33(H33)
5.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C140(H14A,H14B,H14C), C145(H14F,H14G,H14H), C147(H14I,H14J,
 H14K), C149(H14L,H14M,H14N), C169(H16E,H16F,H16G), C114(H11H,H11I,H11J),
 C120(H12C,H12D,H12E), C124(H12F,H12G,H12H), C52(H52A,H52B,H52C), C35(H35A,H35B,
 H35C), C130(H13C,H13D,H13E), C131(H13F,H13G,H13H), C54(H54A,H54B,H54C),
 C80(H80A,H80B,H80C), C133(H13I,H13J,H13K), C42(H42A,H42B,H42C), C134(H13L,H13M,
 H13N), C81(H81A,H81B,H81C), C135(H13O,H13P,H13Q), C55(H55A,H55B,H55C),
 C139(H13R,H13S,H13T), C56(H56A,H56B,H56C), C85(H85A,H85B,H85C), C89(H89A,H89B,
 H89C), C150(H15A,H15B,H15C), C37(H37A,H37B,H37C), C44(H44A,H44B,H44C),
 C159(H15D,H15E,H15F), C95(H95A,H95B,H95C), C99(H99A,H99B,H99C), C168(H16H,H16I,
 H16J), C64(H64A,H64B,H64C), C101(H10G,H10H,H10I), C171(H17G,H17H,H17I),
 C46(H46A,H46B,H46C), C182(H18G,H18H,H18I), C183(H18J,H18K,H18L), C48(H48A,H48B,
 H48C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              39109
_shelx_fab_checksum              35608
_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 1.336
_oxdiff_exptl_absorpt_empirical_full_min 0.824