# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 2007818'
loop_
_audit_author_name
_audit_author_address
'Zheng Wei'
;University at Albany, State University of New York
United States of America
;
_audit_update_record             
;
2020-06-03 deposited with the CCDC.	2020-07-15 downloaded from the CCDC.
;

#=====================================================================
# start Validation Reply Form

_vrf_PLAT910_4                   
;
RESPONSE: 
Data completeness is 99.6% and data redundancy is higher than 7, which are 
good enough to guarantee a reliable structure refinement.
;


_vrf_PLAT906_4                   
;
RESPONSE: 
The K value is large only for weak reflections with
Fc/Fcmax lower than 0.038.
;

_vrf_FORMU01_4                   
;
RESPONSE: 
In each unit cell, 8 severely disordered THF molecules
were removed by PLATON?s SQUEEZE subroutine so they do not include in
the structure model and _atom_site_* section of cif file. But the reported
formula includes the solvents, which causes the atom counts discrepancy.
;


_vrf_CELLZ01_4                   
;
RESPONSE: 
In each unit cell, 8 severely disordered THF molecules
were removed by PLATON?s SQUEEZE subroutine so they do not include in
the structure model and _atom_site_* section of cif file. But the reported
formula includes the solvents, which causes the formula discrepancy
between the one calculated from atom_site data and the reported one.
;

_vrf_PLAT041_4                   
;
RESPONSE: 
In each unit cell, 8 severely disordered THF molecules
were removed by PLATON?s SQUEEZE subroutine so they do not include in
the structure model and _atom_site_* section of cif file. But the reported
formula includes the solvents, which causes the discrepancy between the
calculated SumFormula and the reported SumFormula.
;

_vrf_PLAT042_4                   
;
RESPONSE: 
In each unit cell, 8 severely disordered THF molecules
were removed by PLATON?s SQUEEZE subroutine so they do not include in
the structure model and _atom_site_* section of cif file. But the reported
Reported MoietyFormula includes the solvents, which causes the discrepancy 
between the calculated and the reported MoietyFormula.
;

_vrf_PLAT068_4                   
;
RESPONSE: 
In each unit cell, 8 severely disordered THF molecules
were removed by PLATON?s SQUEEZE subroutine so they do not include in
the structure model and _atom_site_* section of cif file. The reported F000
counts these solvent molecules while the calculated F000 does not,
which causes the discrepancy between these two.
;




_vrf_PLAT606_4                   
;
RESPONSE: 
SQUEEZE was applied to remove 8 severely disordered THF molecules in 
the unit cell, thus leaving large voids.
;

_vrf_PLAT868_4                   
;
RESPONSE: 
It was applied to remove 8 severely disordered THF molecules in 
the unit cell.
;

# end Validation Reply Form 
#=====================================================================

_audit_creation_date             2019-07-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C76 H72 O12 Rb2, 4(C4 H8 O)'
_chemical_formula_sum            'C92 H104 O16 Rb2'
_chemical_formula_weight         1636.69
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   27.646(2)
_cell_length_b                   14.0025(11)
_cell_length_c                   24.309(2)
_cell_angle_alpha                90
_cell_angle_beta                 123.6520(10)
_cell_angle_gamma                90
_cell_volume                     7833.3(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.91
_shelx_estimated_absorpt_T_max   0.949
_shelx_estimated_absorpt_T_min   0.902
_exptl_absorpt_coefficient_mu    1.320
_exptl_absorpt_correction_T_max  0.6736
_exptl_absorpt_correction_T_min  0.5486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0829 before and 0.0706 after correction. The Ratio of minimum to maximum transmission is 0.8144. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3432
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1045
_diffrn_reflns_av_unetI/netI     0.0682
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            53718
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.415
_diffrn_reflns_theta_min         2.909
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5089
_reflns_number_total             7199
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (bruker, 2016)'
_computing_data_collection       'APEX3 v.2017.3-0 (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         7199
_refine_ls_number_restraints     206
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0559
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0324P)²+28.8782P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1112
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C40-C39 = C42-C41 = C41-C40 = C42A-C41A
 1.54 with sigma of 0.02
 O7-C42 = O7-C39 = O7A-C42A = O7A-C39A
 1.43 with sigma of 0.02
 C41-C42 \\sim C41A-C42A
 with sigma of 0.02
 O7-C42 \\sim O7A-C42A
 with sigma of 0.02
 O7-C39 \\sim O7A-C39A
 with sigma of 0.02
 C41-O7 \\sim C41A-O7A
 with sigma of 0.04
 C41-C39 \\sim C41A-C39A
 with sigma of 0.04
 C42-C39 \\sim C42A-C39A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C41 \\sim C40 \\sim O7 \\sim C42 \\sim C39 \\sim C39A \\sim O7A \\sim C42A
\\sim C41A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C41, C40, O7, C42, C39, C39A, O7A, C42A, C41A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H41C)=Sof(H41D)=Sof(C39A)=Sof(H39C)=Sof(H39D)=Sof(O7A)=Sof(C42A)=
 Sof(H42C)=Sof(H42D)=Sof(C41A)=Sof(H41E)=Sof(H41F)=1-FVAR(1)
 Sof(H41A)=Sof(H41B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(O7)=Sof(C42)=Sof(H42A)=
 Sof(H42B)=Sof(C39)=Sof(H39A)=Sof(H39B)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C16(H16)
6.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,
 H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B),
 C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C41(H41A,H41B), C41(H41C,H41D),
  C40(H40A,H40B), C42(H42A,H42B), C39(H39A,H39B), C39A(H39C,H39D), C42A(H42C,
 H42D), C41A(H41E,H41F)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C19(H19), C20(H20)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rb1 Rb 0.21424(2) 0.40357(2) 0.61738(2) 0.02642(11) Uani 1 1 d . . . . .
O1 O 0.11577(11) 0.36391(19) 0.62873(13) 0.0351(7) Uani 1 1 d . . . . .
O2 O 0.18330(11) 0.20962(18) 0.63513(13) 0.0307(6) Uani 1 1 d . . . . .
O3 O 0.28670(11) 0.23876(17) 0.64168(12) 0.0280(6) Uani 1 1 d . . . . .
O4 O 0.34313(11) 0.41700(17) 0.68984(13) 0.0310(6) Uani 1 1 d . . . . .
O5 O 0.27678(12) 0.57402(17) 0.67740(13) 0.0324(7) Uani 1 1 d . . . . .
O6 O 0.17582(12) 0.53865(18) 0.67966(13) 0.0329(7) Uani 1 1 d . . . . .
C1 C 0.17049(19) 0.3479(3) 0.4658(2) 0.0350(10) Uani 1 1 d . . . . .
H1 H 0.162521 0.281405 0.459136 0.042 Uiso 1 1 calc R . . . .
C2 C 0.12772(18) 0.4103(3) 0.45463(18) 0.0318(9) Uani 1 1 d . . . . .
H2 H 0.090187 0.387049 0.440190 0.038 Uiso 1 1 calc R . . . .
C3 C 0.13935(17) 0.5087(3) 0.46451(18) 0.0277(9) Uani 1 1 d . . . . .
C4 C 0.10471(16) 0.5881(3) 0.46164(17) 0.0288(9) Uani 1 1 d . . . . .
C5 C 0.05793(16) 0.5950(3) 0.46853(18) 0.0337(9) Uani 1 1 d . . . . .
H5 H 0.032870 0.541787 0.457592 0.040 Uiso 1 1 calc R . . . .
C6 C 0.04718(16) 0.6806(3) 0.49167(19) 0.0308(9) Uani 1 1 d . . . . .
C7 C 0.01879(17) 0.6866(3) 0.5267(2) 0.0377(10) Uani 1 1 d . . . . .
H7 H -0.011602 0.642923 0.515629 0.045 Uiso 1 1 calc R . . . .
C8 C 0.03405(18) 0.7531(3) 0.5753(2) 0.0398(11) Uani 1 1 d . . . . .
H8 H 0.013547 0.754514 0.596295 0.048 Uiso 1 1 calc R . . . .
C9 C 0.08029(18) 0.8206(3) 0.5953(2) 0.0349(10) Uani 1 1 d . . . . .
C10 C 0.11605(19) 0.8695(3) 0.6571(2) 0.0374(11) Uani 1 1 d . . . . .
H10 H 0.101497 0.879025 0.684040 0.045 Uiso 1 1 calc R . . . .
C11 C 0.17077(19) 0.9035(3) 0.6789(2) 0.0363(10) Uani 1 1 d . . . . .
H11 H 0.192752 0.935678 0.720142 0.044 Uiso 1 1 calc R . . . .
C12 C 0.19486(18) 0.8909(2) 0.64021(19) 0.0315(9) Uani 1 1 d . . . . .
C13 C 0.25434(18) 0.8878(2) 0.66134(19) 0.0326(10) Uani 1 1 d . . . . .
H13 H 0.282709 0.918723 0.701324 0.039 Uiso 1 1 calc R . . . .
C14 C 0.27172(18) 0.8409(3) 0.62501(19) 0.0304(9) Uani 1 1 d . . . . .
H14 H 0.312061 0.837545 0.642375 0.036 Uiso 1 1 calc R . . . .
C15 C 0.23169(16) 0.7970(2) 0.56241(18) 0.0247(9) Uani 1 1 d . . . . .
C16 C 0.24576(17) 0.7233(2) 0.52539(18) 0.0266(9) Uani 1 1 d . . . . .
H16 H 0.283068 0.690728 0.558522 0.032 Uiso 1 1 calc R . . . .
C17 C 0.19721(17) 0.6472(2) 0.49263(18) 0.0272(9) Uani 1 1 d . . . . .
C18 C 0.19619(17) 0.5452(2) 0.48553(18) 0.0254(9) Uani 1 1 d . . . . .
C19 C 0.23867(18) 0.4787(3) 0.49616(18) 0.0304(9) Uani 1 1 d . . . . .
H19 H 0.276322 0.500074 0.509642 0.036 Uiso 1 1 calc R . . . .
C20 C 0.22579(18) 0.3818(3) 0.48701(19) 0.0318(10) Uani 1 1 d . . . . .
H20 H 0.255184 0.337558 0.495331 0.038 Uiso 1 1 calc R . . . .
C21 C 0.14130(17) 0.6703(3) 0.47449(18) 0.0260(9) Uani 1 1 d . . . . .
C22 C 0.12724(17) 0.7566(3) 0.48976(18) 0.0289(9) Uani 1 1 d . . . . .
C23 C 0.08281(16) 0.7587(3) 0.50180(18) 0.0285(9) Uani 1 1 d . . . . .
C24 C 0.10051(17) 0.8238(3) 0.55445(19) 0.0315(10) Uani 1 1 d . . . . .
C25 C 0.15680(17) 0.8580(2) 0.57651(18) 0.0279(9) Uani 1 1 d . . . . .
C26 C 0.17447(17) 0.8153(2) 0.53786(19) 0.0281(9) Uani 1 1 d . . . . .
C27 C 0.10536(18) 0.2681(3) 0.6390(2) 0.0407(11) Uani 1 1 d . . . . .
H27A H 0.063661 0.259697 0.621470 0.049 Uiso 1 1 calc R . . . .
H27B H 0.128142 0.253933 0.686934 0.049 Uiso 1 1 calc R . . . .
C28 C 0.12228(17) 0.2020(3) 0.6052(2) 0.0401(11) Uani 1 1 d . . . . .
H28A H 0.112076 0.135642 0.609080 0.048 Uiso 1 1 calc R . . . .
H28B H 0.101269 0.218384 0.557717 0.048 Uiso 1 1 calc R . . . .
C29 C 0.20385(17) 0.1437(3) 0.60836(19) 0.0310(10) Uani 1 1 d . . . . .
H29A H 0.188563 0.160691 0.561941 0.037 Uiso 1 1 calc R . . . .
H29B H 0.190260 0.078560 0.609034 0.037 Uiso 1 1 calc R . . . .
C30 C 0.26875(18) 0.1463(3) 0.6486(2) 0.0317(10) Uani 1 1 d . . . . .
H30A H 0.284078 0.133706 0.695654 0.038 Uiso 1 1 calc R . . . .
H30B H 0.283951 0.096576 0.633074 0.038 Uiso 1 1 calc R . . . .
C31 C 0.34785(17) 0.2481(3) 0.6804(2) 0.0345(10) Uani 1 1 d . . . . .
H31A H 0.365543 0.196851 0.669048 0.041 Uiso 1 1 calc R . . . .
H31B H 0.362776 0.242340 0.727853 0.041 Uiso 1 1 calc R . . . .
C32 C 0.36367(18) 0.3440(3) 0.6671(2) 0.0380(10) Uani 1 1 d . . . . .
H32A H 0.406388 0.348862 0.690160 0.046 Uiso 1 1 calc R . . . .
H32B H 0.346047 0.351623 0.619123 0.046 Uiso 1 1 calc R . . . .
C33 C 0.35709(19) 0.5101(3) 0.6795(2) 0.0377(10) Uani 1 1 d . . . . .
H33A H 0.337227 0.522625 0.631628 0.045 Uiso 1 1 calc R . . . .
H33B H 0.399521 0.515627 0.700371 0.045 Uiso 1 1 calc R . . . .
C34 C 0.3377(2) 0.5808(3) 0.7097(2) 0.0383(11) Uani 1 1 d . . . . .
H34A H 0.356959 0.567314 0.757373 0.046 Uiso 1 1 calc R . . . .
H34B H 0.348419 0.646199 0.704778 0.046 Uiso 1 1 calc R . . . .
C35 C 0.2549(2) 0.6375(3) 0.7041(2) 0.0393(11) Uani 1 1 d . . . . .
H35A H 0.265804 0.703887 0.701452 0.047 Uiso 1 1 calc R . . . .
H35B H 0.272275 0.622004 0.751244 0.047 Uiso 1 1 calc R . . . .
C36 C 0.1906(2) 0.6292(3) 0.6668(2) 0.0424(11) Uani 1 1 d . . . . .
H36A H 0.174801 0.680507 0.680583 0.051 Uiso 1 1 calc R . . . .
H36B H 0.173489 0.636222 0.618886 0.051 Uiso 1 1 calc R . . . .
C37 C 0.11461(18) 0.5287(3) 0.6484(2) 0.0404(11) Uani 1 1 d . . . . .
H37A H 0.094544 0.539615 0.600295 0.048 Uiso 1 1 calc R . . . .
H37B H 0.100585 0.576910 0.666211 0.048 Uiso 1 1 calc R . . . .
C38 C 0.10099(18) 0.4317(3) 0.6603(2) 0.0402(11) Uani 1 1 d . . . . .
H38A H 0.123271 0.418812 0.708394 0.048 Uiso 1 1 calc R . . . .
H38B H 0.059068 0.427044 0.642617 0.048 Uiso 1 1 calc R . . . .
C41 C 0.54659(19) 0.4703(3) 0.9574(2) 0.0486(11) Uani 1 1 d D U . . .
H41A H 0.577232 0.506177 0.996423 0.058 Uiso 0.653(6) 1 calc R . P A 1
H41B H 0.527447 0.426413 0.971586 0.058 Uiso 0.653(6) 1 calc R . P A 1
H41C H 0.534946 0.403850 0.958493 0.058 Uiso 0.347(6) 1 calc R . P A 2
H41D H 0.573235 0.494892 1.002818 0.058 Uiso 0.347(6) 1 calc R . P A 2
C40 C 0.5026(6) 0.5384(12) 0.9051(5) 0.058(2) Uani 0.653(6) 1 d D U P A 1
H40A H 0.462224 0.519085 0.888311 0.070 Uiso 0.653(6) 1 calc R . P A 1
H40B H 0.509068 0.604911 0.921595 0.070 Uiso 0.653(6) 1 calc R . P A 1
O7 O 0.5355(3) 0.4301(5) 0.8597(3) 0.0736(17) Uani 0.653(6) 1 d D U P A 1
C42 C 0.5724(3) 0.4151(6) 0.9265(4) 0.0537(17) Uani 0.653(6) 1 d D U P A 1
H42A H 0.611949 0.438690 0.942780 0.064 Uiso 0.653(6) 1 calc R . P A 1
H42B H 0.574792 0.346240 0.937046 0.064 Uiso 0.653(6) 1 calc R . P A 1
C39 C 0.5161(5) 0.5264(6) 0.8535(5) 0.071(2) Uani 0.653(6) 1 d D U P A 1
H39A H 0.480990 0.537951 0.808756 0.085 Uiso 0.653(6) 1 calc R . P A 1
H39B H 0.546820 0.571686 0.861282 0.085 Uiso 0.653(6) 1 calc R . P A 1
C39A C 0.4967(11) 0.534(2) 0.9159(8) 0.055(3) Uani 0.347(6) 1 d D U P A 2
H39C H 0.464693 0.515766 0.920925 0.066 Uiso 0.347(6) 1 calc R . P A 2
H39D H 0.508113 0.600193 0.931662 0.066 Uiso 0.347(6) 1 calc R . P A 2
O7A O 0.4761(5) 0.5293(7) 0.8474(5) 0.064(2) Uani 0.347(6) 1 d D U P A 2
C42A C 0.5157(6) 0.4771(14) 0.8424(8) 0.065(3) Uani 0.347(6) 1 d D U P A 2
H42C H 0.521467 0.505268 0.809059 0.077 Uiso 0.347(6) 1 calc R . P A 2
H42D H 0.502714 0.410103 0.830005 0.077 Uiso 0.347(6) 1 calc R . P A 2
C41A C 0.5720(6) 0.4825(13) 0.9119(7) 0.063(2) Uani 0.347(6) 1 d D U P A 2
H41E H 0.591841 0.544700 0.919691 0.075 Uiso 0.347(6) 1 calc R . P A 2
H41F H 0.599168 0.430231 0.919492 0.075 Uiso 0.347(6) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rb1 O1 2.938(3) . ?
Rb1 O2 2.950(2) . ?
Rb1 O3 2.894(2) . ?
Rb1 O4 2.980(3) . ?
Rb1 O5 2.832(2) . ?
Rb1 O6 2.963(3) . ?
Rb1 C1 3.272(4) . ?
Rb1 C2 3.301(4) . ?
Rb1 C3 3.426(4) . ?
Rb1 C18 3.561(4) . ?
Rb1 C19 3.529(4) . ?
Rb1 C20 3.370(4) . ?
O1 C27 1.422(5) . ?
O1 C38 1.416(5) . ?
O2 C28 1.424(5) . ?
O2 C29 1.417(4) . ?
O3 C30 1.430(4) . ?
O3 C31 1.413(5) . ?
O4 C32 1.421(5) . ?
O4 C33 1.420(4) . ?
O5 C34 1.412(5) . ?
O5 C35 1.418(5) . ?
O6 C36 1.419(5) . ?
O6 C37 1.427(5) . ?
C1 H1 0.9500 . ?
C1 C2 1.371(5) . ?
C1 C20 1.398(6) . ?
C2 H2 0.9500 . ?
C2 C3 1.404(5) . ?
C3 C4 1.443(5) . ?
C3 C18 1.450(5) . ?
C4 C5 1.396(5) . ?
C4 C21 1.448(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.423(5) . ?
C6 C7 1.444(6) . ?
C6 C23 1.399(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.375(6) . ?
C8 H8 0.9500 . ?
C8 C9 1.441(6) . ?
C9 C10 1.434(6) . ?
C9 C24 1.385(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.381(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.433(6) . ?
C12 C13 1.426(6) . ?
C12 C25 1.382(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.383(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.432(5) . ?
C15 C16 1.554(5) . ?
C15 C26 1.370(5) . ?
C16 C16 1.568(7) 7_566 ?
C16 H16 1.0000 . ?
C16 C17 1.545(5) . ?
C17 C18 1.437(5) . ?
C17 C21 1.390(5) . ?
C18 C19 1.406(5) . ?
C19 H19 0.9500 . ?
C19 C20 1.389(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.382(5) . ?
C22 C23 1.412(5) . ?
C22 C26 1.433(5) . ?
C23 C24 1.419(5) . ?
C24 C25 1.419(5) . ?
C25 C26 1.410(5) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.476(6) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.494(5) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.501(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.497(5) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.488(6) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.479(6) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 H41C 0.9900 . ?
C41 H41D 0.9900 . ?
C41 C40 1.514(12) . ?
C41 C42 1.505(7) . ?
C41 C39A 1.47(2) . ?
C41 C41A 1.613(16) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C39 1.503(12) . ?
O7 C42 1.374(8) . ?
O7 C39 1.429(9) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39A H39C 0.9900 . ?
C39A H39D 0.9900 . ?
C39A O7A 1.432(13) . ?
O7A C42A 1.377(12) . ?
C42A H42C 0.9900 . ?
C42A H42D 0.9900 . ?
C42A C41A 1.539(13) . ?
C41A H41E 0.9900 . ?
C41A H41F 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Rb1 O2 56.86(7) . . ?
O1 Rb1 O4 145.42(7) . . ?
O1 Rb1 O6 57.27(7) . . ?
O1 Rb1 C1 106.09(9) . . ?
O1 Rb1 C2 91.39(9) . . ?
O1 Rb1 C3 98.55(8) . . ?
O1 Rb1 C18 120.99(8) . . ?
O1 Rb1 C19 138.68(9) . . ?
O1 Rb1 C20 130.30(9) . . ?
O2 Rb1 O4 108.68(7) . . ?
O2 Rb1 O6 107.33(7) . . ?
O2 Rb1 C1 89.38(8) . . ?
O2 Rb1 C2 97.21(8) . . ?
O2 Rb1 C3 120.28(8) . . ?
O2 Rb1 C18 137.47(8) . . ?
O2 Rb1 C19 126.99(8) . . ?
O2 Rb1 C20 103.91(8) . . ?
O3 Rb1 O1 113.75(7) . . ?
O3 Rb1 O2 57.32(7) . . ?
O3 Rb1 O4 57.59(7) . . ?
O3 Rb1 O6 143.92(7) . . ?
O3 Rb1 C1 79.75(9) . . ?
O3 Rb1 C2 103.15(9) . . ?
O3 Rb1 C3 119.87(8) . . ?
O3 Rb1 C18 111.33(8) . . ?
O3 Rb1 C19 88.68(8) . . ?
O3 Rb1 C20 72.80(8) . . ?
O4 Rb1 C1 104.80(9) . . ?
O4 Rb1 C2 122.80(9) . . ?
O4 Rb1 C3 114.84(8) . . ?
O4 Rb1 C18 91.27(8) . . ?
O4 Rb1 C19 75.84(8) . . ?
O4 Rb1 C20 81.74(9) . . ?
O5 Rb1 O1 116.36(8) . . ?
O5 Rb1 O2 147.60(7) . . ?
O5 Rb1 O3 114.27(7) . . ?
O5 Rb1 O4 56.88(7) . . ?
O5 Rb1 O6 59.21(8) . . ?
O5 Rb1 C1 121.34(9) . . ?
O5 Rb1 C2 115.05(9) . . ?
O5 Rb1 C3 91.50(8) . . ?
O5 Rb1 C18 74.66(8) . . ?
O5 Rb1 C19 80.47(8) . . ?
O5 Rb1 C20 102.24(8) . . ?
O6 Rb1 O4 107.91(7) . . ?
O6 Rb1 C1 135.55(9) . . ?
O6 Rb1 C2 111.54(9) . . ?
O6 Rb1 C3 96.18(8) . . ?
O6 Rb1 C18 101.15(8) . . ?
O6 Rb1 C19 121.68(8) . . ?
O6 Rb1 C20 141.79(8) . . ?
C1 Rb1 C2 24.08(10) . . ?
C1 Rb1 C3 42.00(9) . . ?
C1 Rb1 C18 48.64(9) . . ?
C1 Rb1 C19 41.67(10) . . ?
C1 Rb1 C20 24.24(10) . . ?
C2 Rb1 C3 24.01(9) . . ?
C2 Rb1 C18 42.11(9) . . ?
C2 Rb1 C19 48.50(10) . . ?
C2 Rb1 C20 42.17(10) . . ?
C3 Rb1 C18 23.85(9) . . ?
C3 Rb1 C19 41.09(9) . . ?
C19 Rb1 C18 22.87(8) . . ?
C20 Rb1 C3 48.25(9) . . ?
C20 Rb1 C18 40.81(8) . . ?
C20 Rb1 C19 23.08(9) . . ?
C27 O1 Rb1 118.9(2) . . ?
C38 O1 Rb1 119.0(2) . . ?
C38 O1 C27 112.9(3) . . ?
C28 O2 Rb1 110.6(2) . . ?
C29 O2 Rb1 108.07(19) . . ?
C29 O2 C28 112.3(3) . . ?
C30 O3 Rb1 120.0(2) . . ?
C31 O3 Rb1 120.0(2) . . ?
C31 O3 C30 111.8(3) . . ?
C32 O4 Rb1 109.2(2) . . ?
C33 O4 Rb1 107.8(2) . . ?
C33 O4 C32 112.7(3) . . ?
C34 O5 Rb1 122.8(2) . . ?
C34 O5 C35 112.5(3) . . ?
C35 O5 Rb1 118.1(2) . . ?
C36 O6 Rb1 103.3(2) . . ?
C36 O6 C37 111.8(3) . . ?
C37 O6 Rb1 108.7(2) . . ?
Rb1 C1 H1 109.4 . . ?
C2 C1 Rb1 79.1(2) . . ?
C2 C1 H1 119.9 . . ?
C2 C1 C20 120.2(4) . . ?
C20 C1 Rb1 81.8(2) . . ?
C20 C1 H1 119.9 . . ?
Rb1 C2 H2 110.5 . . ?
C1 C2 Rb1 76.8(2) . . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 120.0(4) . . ?
C3 C2 Rb1 83.0(2) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 Rb1 73.0(2) . . ?
C2 C3 C4 131.6(4) . . ?
C2 C3 C18 120.4(3) . . ?
C4 C3 Rb1 111.7(2) . . ?
C4 C3 C18 107.8(3) . . ?
C18 C3 Rb1 83.3(2) . . ?
C3 C4 C21 103.7(3) . . ?
C5 C4 C3 133.0(4) . . ?
C5 C4 C21 120.1(4) . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 121.1(4) . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C7 125.6(4) . . ?
C23 C6 C5 116.5(4) . . ?
C23 C6 C7 114.2(4) . . ?
C6 C7 H7 118.7 . . ?
C8 C7 C6 122.6(4) . . ?
C8 C7 H7 118.7 . . ?
C7 C8 H8 119.1 . . ?
C7 C8 C9 121.8(4) . . ?
C9 C8 H8 119.1 . . ?
C10 C9 C8 129.4(4) . . ?
C24 C9 C8 114.5(4) . . ?
C24 C9 C10 114.7(4) . . ?
C9 C10 H10 118.6 . . ?
C11 C10 C9 122.7(4) . . ?
C11 C10 H10 118.6 . . ?
C10 C11 H11 119.5 . . ?
C10 C11 C12 120.9(4) . . ?
C12 C11 H11 119.5 . . ?
C13 C12 C11 129.0(4) . . ?
C25 C12 C11 115.7(4) . . ?
C25 C12 C13 113.8(4) . . ?
C12 C13 H13 119.2 . . ?
C14 C13 C12 121.6(4) . . ?
C14 C13 H13 119.2 . . ?
C13 C14 H14 118.5 . . ?
C13 C14 C15 123.0(4) . . ?
C15 C14 H14 118.5 . . ?
C14 C15 C16 127.3(3) . . ?
C26 C15 C14 114.1(3) . . ?
C26 C15 C16 118.1(3) . . ?
C15 C16 C16 109.5(3) . 7_566 ?
C15 C16 H16 108.3 . . ?
C16 C16 H16 108.3 7_566 . ?
C17 C16 C15 109.4(3) . . ?
C17 C16 C16 112.9(4) . 7_566 ?
C17 C16 H16 108.3 . . ?
C18 C17 C16 134.5(4) . . ?
C21 C17 C16 119.9(3) . . ?
C21 C17 C18 104.4(3) . . ?
C3 C18 Rb1 72.8(2) . . ?
C17 C18 Rb1 117.5(2) . . ?
C17 C18 C3 109.7(3) . . ?
C19 C18 Rb1 77.3(2) . . ?
C19 C18 C3 117.6(3) . . ?
C19 C18 C17 132.6(4) . . ?
Rb1 C19 H19 119.1 . . ?
C18 C19 Rb1 79.9(2) . . ?
C18 C19 H19 119.9 . . ?
C20 C19 Rb1 72.1(2) . . ?
C20 C19 C18 120.2(4) . . ?
C20 C19 H19 119.9 . . ?
Rb1 C20 H20 112.0 . . ?
C1 C20 Rb1 73.9(2) . . ?
C1 C20 H20 119.3 . . ?
C19 C20 Rb1 84.9(2) . . ?
C19 C20 C1 121.4(4) . . ?
C19 C20 H20 119.3 . . ?
C17 C21 C4 113.9(3) . . ?
C22 C21 C4 119.1(4) . . ?
C22 C21 C17 123.2(4) . . ?
C21 C22 C23 118.7(3) . . ?
C21 C22 C26 117.1(4) . . ?
C23 C22 C26 108.9(3) . . ?
C6 C23 C22 123.8(3) . . ?
C6 C23 C24 121.2(4) . . ?
C22 C23 C24 107.2(3) . . ?
C9 C24 C23 123.5(4) . . ?
C9 C24 C25 122.3(4) . . ?
C25 C24 C23 108.4(4) . . ?
C12 C25 C24 122.0(4) . . ?
C12 C25 C26 123.9(4) . . ?
C26 C25 C24 108.5(3) . . ?
C15 C26 C22 124.0(3) . . ?
C15 C26 C25 122.1(4) . . ?
C25 C26 C22 106.9(3) . . ?
O1 C27 H27A 109.7 . . ?
O1 C27 H27B 109.7 . . ?
O1 C27 C28 109.7(3) . . ?
H27A C27 H27B 108.2 . . ?
C28 C27 H27A 109.7 . . ?
C28 C27 H27B 109.7 . . ?
Rb1 C28 H28A 158.0 . . ?
Rb1 C28 H28B 81.3 . . ?
O2 C28 Rb1 48.27(17) . . ?
O2 C28 C27 108.6(3) . . ?
O2 C28 H28A 110.0 . . ?
O2 C28 H28B 110.0 . . ?
C27 C28 Rb1 83.8(2) . . ?
C27 C28 H28A 110.0 . . ?
C27 C28 H28B 110.0 . . ?
H28A C28 H28B 108.3 . . ?
Rb1 C29 H29A 78.4 . . ?
Rb1 C29 H29B 159.4 . . ?
O2 C29 Rb1 50.26(15) . . ?
O2 C29 H29A 109.9 . . ?
O2 C29 H29B 109.9 . . ?
O2 C29 C30 109.0(3) . . ?
H29A C29 H29B 108.3 . . ?
C30 C29 Rb1 84.9(2) . . ?
C30 C29 H29A 109.9 . . ?
C30 C29 H29B 109.9 . . ?
O3 C30 C29 108.3(3) . . ?
O3 C30 H30A 110.0 . . ?
O3 C30 H30B 110.0 . . ?
C29 C30 H30A 110.0 . . ?
C29 C30 H30B 110.0 . . ?
H30A C30 H30B 108.4 . . ?
O3 C31 H31A 109.9 . . ?
O3 C31 H31B 109.9 . . ?
O3 C31 C32 108.9(3) . . ?
H31A C31 H31B 108.3 . . ?
C32 C31 H31A 109.9 . . ?
C32 C31 H31B 109.9 . . ?
Rb1 C32 H32A 159.3 . . ?
Rb1 C32 H32B 81.9 . . ?
O4 C32 Rb1 49.51(17) . . ?
O4 C32 C31 109.5(3) . . ?
O4 C32 H32A 109.8 . . ?
O4 C32 H32B 109.8 . . ?
C31 C32 Rb1 82.3(2) . . ?
C31 C32 H32A 109.8 . . ?
C31 C32 H32B 109.8 . . ?
H32A C32 H32B 108.2 . . ?
Rb1 C33 H33A 79.6 . . ?
Rb1 C33 H33B 160.3 . . ?
O4 C33 Rb1 50.56(17) . . ?
O4 C33 H33A 110.0 . . ?
O4 C33 H33B 110.0 . . ?
O4 C33 C34 108.3(3) . . ?
H33A C33 H33B 108.4 . . ?
C34 C33 Rb1 82.8(2) . . ?
C34 C33 H33A 110.0 . . ?
C34 C33 H33B 110.0 . . ?
O5 C34 C33 108.9(3) . . ?
O5 C34 H34A 109.9 . . ?
O5 C34 H34B 109.9 . . ?
C33 C34 H34A 109.9 . . ?
C33 C34 H34B 109.9 . . ?
H34A C34 H34B 108.3 . . ?
Rb1 C35 H35A 142.9 . . ?
Rb1 C35 H35B 105.3 . . ?
O5 C35 H35A 109.7 . . ?
O5 C35 H35B 109.7 . . ?
O5 C35 C36 109.9(3) . . ?
H35A C35 H35B 108.2 . . ?
C36 C35 Rb1 72.6(2) . . ?
C36 C35 H35A 109.7 . . ?
C36 C35 H35B 109.7 . . ?
Rb1 C36 H36A 162.5 . . ?
Rb1 C36 H36B 75.4 . . ?
O6 C36 Rb1 53.94(17) . . ?
O6 C36 C35 109.2(3) . . ?
O6 C36 H36A 109.8 . . ?
O6 C36 H36B 109.8 . . ?
C35 C36 Rb1 83.9(2) . . ?
C35 C36 H36A 109.8 . . ?
C35 C36 H36B 109.8 . . ?
H36A C36 H36B 108.3 . . ?
Rb1 C37 H37A 79.9 . . ?
Rb1 C37 H37B 159.1 . . ?
O6 C37 Rb1 49.74(17) . . ?
O6 C37 H37A 109.7 . . ?
O6 C37 H37B 109.7 . . ?
O6 C37 C38 109.9(3) . . ?
H37A C37 H37B 108.2 . . ?
C38 C37 Rb1 84.5(2) . . ?
C38 C37 H37A 109.7 . . ?
C38 C37 H37B 109.7 . . ?
O1 C38 C37 109.1(3) . . ?
O1 C38 H38A 109.9 . . ?
O1 C38 H38B 109.9 . . ?
C37 C38 H38A 109.9 . . ?
C37 C38 H38B 109.9 . . ?
H38A C38 H38B 108.3 . . ?
H41A C41 H41B 108.6 . . ?
H41C C41 H41D 110.4 . . ?
C40 C41 H41A 110.4 . . ?
C40 C41 H41B 110.4 . . ?
C42 C41 H41A 110.4 . . ?
C42 C41 H41B 110.4 . . ?
C42 C41 C40 106.7(6) . . ?
C39A C41 H41C 113.0 . . ?
C39A C41 H41D 113.0 . . ?
C39A C41 C41A 93.8(10) . . ?
C41A C41 H41C 113.0 . . ?
C41A C41 H41D 113.0 . . ?
C41 C40 H40A 111.8 . . ?
C41 C40 H40B 111.8 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 C41 100.0(8) . . ?
C39 C40 H40A 111.8 . . ?
C39 C40 H40B 111.8 . . ?
C42 O7 C39 105.0(6) . . ?
C41 C42 H42A 110.7 . . ?
C41 C42 H42B 110.7 . . ?
O7 C42 C41 105.3(5) . . ?
O7 C42 H42A 110.7 . . ?
O7 C42 H42B 110.7 . . ?
H42A C42 H42B 108.8 . . ?
C40 C39 H39A 110.6 . . ?
C40 C39 H39B 110.6 . . ?
O7 C39 C40 105.6(8) . . ?
O7 C39 H39A 110.6 . . ?
O7 C39 H39B 110.6 . . ?
H39A C39 H39B 108.7 . . ?
C41 C39A H39C 109.0 . . ?
C41 C39A H39D 109.0 . . ?
H39C C39A H39D 107.8 . . ?
O7A C39A C41 112.8(15) . . ?
O7A C39A H39C 109.0 . . ?
O7A C39A H39D 109.0 . . ?
C42A O7A C39A 107.6(13) . . ?
O7A C42A H42C 110.9 . . ?
O7A C42A H42D 110.9 . . ?
O7A C42A C41A 104.2(11) . . ?
H42C C42A H42D 108.9 . . ?
C41A C42A H42C 110.9 . . ?
C41A C42A H42D 110.9 . . ?
C41 C41A H41E 111.6 . . ?
C41 C41A H41F 111.6 . . ?
C42A C41A C41 100.8(10) . . ?
C42A C41A H41E 111.6 . . ?
C42A C41A H41F 111.6 . . ?
H41E C41A H41F 109.4 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.448 0.750 318.3 75.4 2(C4H8O)
2 0.000 0.552 0.250 318.3 75.4 2(C4H8O)
3 0.500 0.052 0.250 318.3 75.4 2(C4H8O)
4 0.500 -0.052 0.750 318.3 75.4 2(C4H8O)

_olex2_submission_special_instructions 'No special instructions were received'
