# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_JKM5
_database_code_depnum_ccdc_archive 'CCDC 1837111'
_audit_update_record             
;
2018-05-30 deposited with the CCDC.
2018-05-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 H11 K O'
_chemical_formula_weight         126.24

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_H-M_alt        'P -4 21 c'
_space_group_name_Hall           'P -4 2n'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   8.2509(4)
_cell_length_b                   8.2509(4)
_cell_length_c                   20.346(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1385.1(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5019
_cell_measurement_theta_min      2.4685
_cell_measurement_theta_max      27.8242

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_F_000             544
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.34
_exptl_absorpt_coefficient_mu    0.662
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6935
_exptl_absorpt_correction_T_max  1.0709
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Smart'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7105
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.002
_diffrn_reflns_theta_max         27.869
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1664
_reflns_number_gt                1629
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.721
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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.
;

_computing_data_collection       APEX2
_computing_cell_refinement       APEX2
_computing_data_reduction        APEX2
_computing_structure_solution    ShelXS
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ShelXP
_computing_publication_material  XCIF

_refine_special_details          'Refined as a 2-component inversion twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0274P)²+0.1681P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.30(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1664
_refine_ls_number_parameters     71
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0222
_refine_ls_wR_factor_ref         0.0571
_refine_ls_wR_factor_gt          0.0568
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_restrained_S_all      1.128
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
K1 K 0.36257(4) 0.32344(4) 0.06376(2) 0.02379(12) Uani 1 1 d . . . . .
O1 O 0.68036(14) 0.36232(14) 0.06413(6) 0.0248(3) Uani 1 1 d . . . . .
C10 C 0.7765(2) 0.2731(2) 0.10649(8) 0.0191(3) Uani 1 1 d . . . . .
C11 C 0.9466(2) 0.2478(2) 0.07659(10) 0.0292(4) Uani 1 1 d . . . . .
H11A H 1.0157(11) 0.1910(17) 0.1083(5) 0.044 Uiso 1 1 calc R U . . .
H11B H 0.9947(10) 0.3534(14) 0.0661(6) 0.044 Uiso 1 1 calc R U . . .
H11C H 0.9376(3) 0.1831(17) 0.0363(7) 0.044 Uiso 1 1 calc R U . . .
C12 C 0.7017(3) 0.1050(2) 0.11848(9) 0.0290(4) Uani 1 1 d . . . . .
H12A H 0.5987(16) 0.1172(3) 0.1401(7) 0.044 Uiso 1 1 calc R U . . .
H12B H 0.7731(13) 0.0419(11) 0.1457(7) 0.044 Uiso 1 1 calc R U . . .
H12C H 0.6864(17) 0.0508(11) 0.0771(6) 0.044 Uiso 1 1 calc R U . . .
C13 C 0.7916(2) 0.3641(2) 0.17279(8) 0.0282(4) Uani 1 1 d . . . . .
H13A H 0.8440 0.4672 0.1643 0.034 Uiso 1 1 calc R U . . .
H13B H 0.6829 0.3874 0.1883 0.034 Uiso 1 1 calc R U . . .
C14 C 0.8833(3) 0.2806(3) 0.22842(10) 0.0507(6) Uani 1 1 d . . . . .
H14A H 0.889(2) 0.3518(15) 0.2658(7) 0.076 Uiso 1 1 calc R U . . .
H14B H 0.991(2) 0.255(2) 0.2140(4) 0.076 Uiso 1 1 calc R U . . .
H14C H 0.8278(17) 0.182(2) 0.2405(7) 0.076 Uiso 1 1 calc R U . . .


_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
K1 O1 2.6023(12) 3_565 ?
K1 O1 2.6168(12) 2_665 ?
K1 O1 2.6416(12) . ?
K1 C11 3.498(2) 1_455 ?
K1 C12 3.509(2) . ?
K1 K1 3.6808(7) 3_565 ?
K1 K1 3.6808(7) 4_655 ?
K1 K1 3.6921(7) 2_665 ?
O1 C10 1.384(2) . ?
O1 K1 2.6024(12) 4_655 ?
O1 K1 2.6169(12) 2_665 ?
C10 C12 1.537(2) . ?
C10 C11 1.544(2) . ?
C10 C13 1.549(2) . ?
C11 K1 3.498(2) 1_655 ?
C13 C14 1.526(3) . ?

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 K1 O1 90.84(4) 3_565 2_665 ?
O1 K1 O1 90.29(4) 3_565 . ?
O1 K1 O1 90.80(4) 2_665 . ?
O1 K1 C11 94.11(4) 3_565 1_455 ?
O1 K1 C11 92.50(4) 2_665 1_455 ?
O1 K1 C11 174.45(4) . 1_455 ?
O1 K1 C12 108.16(4) 3_565 . ?
O1 K1 C12 128.01(4) 2_665 . ?
O1 K1 C12 43.12(4) . . ?
C11 K1 C12 131.84(5) 1_455 . ?
O1 K1 K1 45.86(3) 3_565 3_565 ?
O1 K1 K1 44.99(3) 2_665 3_565 ?
O1 K1 K1 90.21(3) . 3_565 ?
C11 K1 K1 95.28(3) 1_455 3_565 ?
C12 K1 K1 130.92(3) . 3_565 ?
O1 K1 K1 45.31(3) 3_565 4_655 ?
O1 K1 K1 90.60(3) 2_665 4_655 ?
O1 K1 K1 44.99(3) . 4_655 ?
C11 K1 K1 139.36(4) 1_455 4_655 ?
C12 K1 K1 72.99(3) . 4_655 ?
K1 K1 K1 60.203(13) 3_565 4_655 ?
O1 K1 K1 90.57(3) 3_565 2_665 ?
O1 K1 K1 45.68(3) 2_665 2_665 ?
O1 K1 K1 45.13(3) . 2_665 ?
C11 K1 K1 138.02(4) 1_455 2_665 ?
C12 K1 K1 85.15(3) . 2_665 ?
K1 K1 K1 59.899(7) 3_565 2_665 ?
K1 K1 K1 59.899(7) 4_655 2_665 ?
C10 O1 K1 129.06(10) . 4_655 ?
C10 O1 K1 127.35(9) . 2_665 ?
K1 O1 K1 89.70(4) 4_655 2_665 ?
C10 O1 K1 120.43(9) . . ?
K1 O1 K1 89.16(4) 4_655 . ?
K1 O1 K1 89.19(4) 2_665 . ?
O1 C10 C12 110.39(14) . . ?
O1 C10 C11 110.35(13) . . ?
C12 C10 C11 107.82(15) . . ?
O1 C10 C13 109.29(14) . . ?
C12 C10 C13 109.34(14) . . ?
C11 C10 C13 109.63(15) . . ?
C10 C11 K1 153.81(13) . 1_655 ?
C10 C12 K1 78.86(10) . . ?
C14 C13 C10 117.83(17) . . ?

_refine_diff_density_max         0.232
_refine_diff_density_min         -0.151
_refine_diff_density_rms         0.038

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: n-hexane'
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_jkm1
_database_code_depnum_ccdc_archive 'CCDC 1837112'
_audit_update_record             
;
2018-05-30 deposited with the CCDC.
2018-05-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 H11 K O'
_chemical_formula_weight         126.24

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   21.876(4)
_cell_length_b                   8.1807(17)
_cell_length_c                   16.896(3)
_cell_angle_alpha                90
_cell_angle_beta                 111.919(3)
_cell_angle_gamma                90
_cell_volume                     2805.2(10)
_cell_formula_units_Z            16
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3930
_cell_measurement_theta_min      2.5988
_cell_measurement_theta_max      26.0439

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_F_000             1088
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    0.654
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7568
_exptl_absorpt_correction_T_max  1.0032
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Smart'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29399
_diffrn_reflns_av_unetI/netI     0.0714
_diffrn_reflns_av_R_equivalents  0.0903
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.003
_diffrn_reflns_theta_max         27.899
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6662
_reflns_number_gt                4239
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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.
;

_computing_data_collection       APEX2
_computing_cell_refinement       APEX2
_computing_data_reduction        APEX2
_computing_structure_solution    ShelXS
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ShelXP
_computing_publication_material  XCIF

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0327P)²+4.8009P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6662
_refine_ls_number_parameters     289
_refine_ls_number_restraints     114
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0720
_refine_ls_wR_factor_ref         0.1596
_refine_ls_wR_factor_gt          0.1446
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_restrained_S_all      1.153
_refine_ls_shift/su_max          0.068
_refine_ls_shift/su_mean         0.001

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
K1 K 0.31773(4) 0.18003(10) 0.46691(6) 0.0315(2) Uani 1 1 d . . . . .
K2 K 0.19173(5) 0.14918(10) 0.55923(6) 0.0346(2) Uani 1 1 d . . . . .
K3 K 0.31732(5) -0.17469(11) 0.60212(6) 0.0335(2) Uani 1 1 d . . . . .
K4 K 0.19136(5) -0.13601(10) 0.38708(6) 0.0337(2) Uani 1 1 d . . . . .
O1 O 0.18898(14) -0.1683(3) 0.54009(19) 0.0367(7) Uani 1 1 d D . . . .
C10 C 0.139(2) -0.253(8) 0.555(4) 0.037(4) Uiso 0.046(3) 1 d D U P A 3
C11 C 0.066(3) -0.237(13) 0.498(6) 0.039(8) Uiso 0.046(3) 1 d D U P A 3
H11A H 0.0531 -0.1220 0.4948 0.058 Uiso 0.046(3) 1 calc R U P A 3
H11B H 0.0398 -0.3006 0.5235 0.058 Uiso 0.046(3) 1 calc R U P A 3
H11C H 0.0585 -0.2787 0.4411 0.058 Uiso 0.046(3) 1 calc R U P A 3
C12 C 0.159(5) -0.434(10) 0.560(6) 0.033(9) Uiso 0.046(3) 1 d D U P A 3
H12A H 0.2000 -0.4515 0.6087 0.049 Uiso 0.046(3) 1 calc R U P A 3
H12B H 0.1652 -0.4659 0.5072 0.049 Uiso 0.046(3) 1 calc R U P A 3
H12C H 0.1239 -0.5012 0.5661 0.049 Uiso 0.046(3) 1 calc R U P A 3
C13 C 0.151(5) -0.191(8) 0.645(4) 0.036(5) Uiso 0.046(3) 1 d D U P A 3
H13A H 0.1980 -0.1570 0.6727 0.044 Uiso 0.046(3) 1 calc R U P A 3
H13B H 0.1238 -0.0926 0.6407 0.044 Uiso 0.046(3) 1 calc R U P A 3
C14 C 0.136(5) -0.316(8) 0.703(4) 0.046(9) Uiso 0.046(3) 1 d D U P A 3
H14A H 0.1334 -0.2598 0.7531 0.068 Uiso 0.046(3) 1 calc R U P A 3
H14B H 0.1712 -0.3980 0.7221 0.068 Uiso 0.046(3) 1 calc R U P A 3
H14C H 0.0940 -0.3695 0.6716 0.068 Uiso 0.046(3) 1 calc R U P A 3
C10A C 0.1423(5) -0.2581(14) 0.5570(7) 0.032(3) Uiso 0.503(3) 1 d D U P A 1
C11A C 0.1276(7) -0.1694(16) 0.6277(7) 0.052(3) Uiso 0.503(3) 1 d D U P A 1
H11D H 0.1133 -0.0574 0.6094 0.078 Uiso 0.503(3) 1 calc R U P A 1
H11E H 0.1675 -0.1667 0.6796 0.078 Uiso 0.503(3) 1 calc R U P A 1
H11F H 0.0926 -0.2273 0.6392 0.078 Uiso 0.503(3) 1 calc R U P A 1
C12A C 0.1639(8) -0.4351(15) 0.5829(9) 0.039(3) Uiso 0.503(3) 1 d D U P A 1
H12D H 0.1742 -0.4884 0.5374 0.059 Uiso 0.503(3) 1 calc R U P A 1
H12E H 0.1282 -0.4945 0.5920 0.059 Uiso 0.503(3) 1 calc R U P A 1
H12F H 0.2031 -0.4354 0.6357 0.059 Uiso 0.503(3) 1 calc R U P A 1
C13A C 0.0810(5) -0.2648(15) 0.4736(6) 0.042(3) Uiso 0.503(3) 1 d D U P A 1
H13C H 0.0708 -0.1529 0.4500 0.051 Uiso 0.503(3) 1 calc R U P A 1
H13D H 0.0913 -0.3323 0.4314 0.051 Uiso 0.503(3) 1 calc R U P A 1
C14A C 0.0200(5) -0.3357(14) 0.4854(8) 0.067(3) Uiso 0.503(3) 1 d D U P A 1
H14D H -0.0162 -0.3442 0.4298 0.100 Uiso 0.503(3) 1 calc R U P A 1
H14E H 0.0070 -0.2637 0.5227 0.100 Uiso 0.503(3) 1 calc R U P A 1
H14F H 0.0304 -0.4445 0.5113 0.100 Uiso 0.503(3) 1 calc R U P A 1
C10B C 0.1480(5) -0.2658(14) 0.5671(7) 0.030(3) Uiso 0.451(3) 1 d D U P A 4
C11B C 0.1393(7) -0.1998(15) 0.6477(7) 0.036(3) Uiso 0.451(3) 1 d D U P A 4
H11G H 0.1179 -0.0925 0.6353 0.054 Uiso 0.451(3) 1 calc R U P A 4
H11H H 0.1825 -0.1893 0.6939 0.054 Uiso 0.451(3) 1 calc R U P A 4
H11I H 0.1119 -0.2756 0.6650 0.054 Uiso 0.451(3) 1 calc R U P A 4
C12B C 0.1803(7) -0.4339(14) 0.5907(10) 0.037(3) Uiso 0.451(3) 1 d D U P A 4
H12G H 0.1843 -0.4842 0.5401 0.055 Uiso 0.451(3) 1 calc R U P A 4
H12H H 0.1531 -0.5036 0.6116 0.055 Uiso 0.451(3) 1 calc R U P A 4
H12I H 0.2242 -0.4217 0.6353 0.055 Uiso 0.451(3) 1 calc R U P A 4
C13B C 0.0784(6) -0.2858(15) 0.4979(9) 0.046(3) Uiso 0.451(3) 1 d D U P A 4
H13E H 0.0823 -0.3374 0.4471 0.055 Uiso 0.451(3) 1 calc R U P A 4
H13F H 0.0527 -0.3609 0.5196 0.055 Uiso 0.451(3) 1 calc R U P A 4
C14B C 0.0400(6) -0.1251(15) 0.4707(9) 0.067(3) Uiso 0.451(3) 1 d D U P A 4
H14G H -0.0038 -0.1478 0.4277 0.100 Uiso 0.451(3) 1 calc R U P A 4
H14H H 0.0639 -0.0516 0.4465 0.100 Uiso 0.451(3) 1 calc R U P A 4
H14I H 0.0354 -0.0732 0.5205 0.100 Uiso 0.451(3) 1 calc R U P A 4
O2 O 0.32053(13) -0.1371(3) 0.44960(18) 0.0329(7) Uani 1 1 d D . . . .
C20 C 0.3597(2) -0.2286(4) 0.4182(2) 0.0270(9) Uani 1 1 d D . . . .
C21 C 0.3277(2) -0.2410(5) 0.3206(3) 0.0379(11) Uani 1 1 d . . . . .
H21A H 0.2868(13) -0.297(3) 0.3050(5) 0.057 Uiso 1 1 calc R U . . .
H21B H 0.3561(10) -0.300(3) 0.2997(6) 0.057 Uiso 1 1 calc R U . . .
H21C H 0.3205(13) -0.134(3) 0.2967(7) 0.057 Uiso 1 1 calc R U . . .
C22 C 0.3682(2) -0.4038(5) 0.4549(3) 0.0345(10) Uani 1 1 d . . . . .
H22A H 0.3932(14) -0.3998(6) 0.5172(15) 0.052 Uiso 1 1 calc R U . . .
H22B H 0.3926(14) -0.471(2) 0.4278(15) 0.052 Uiso 1 1 calc R U . . .
H22C H 0.3244(11) -0.4527(18) 0.4433(16) 0.052 Uiso 1 1 calc R U . . .
C23 C 0.4276(2) -0.1474(5) 0.4440(3) 0.0331(9) Uani 1 1 d . . . . .
H23A H 0.4212 -0.0380 0.4172 0.040 Uiso 1 1 calc R U . . .
H23B H 0.4447 -0.1304 0.5066 0.040 Uiso 1 1 calc R U . . .
C24 C 0.4810(2) -0.2357(7) 0.4222(4) 0.0563(15) Uani 1 1 d . . . . .
H24A H 0.5201(13) -0.172(3) 0.441(2) 0.084 Uiso 1 1 calc R U . . .
H24B H 0.4664(9) -0.250(4) 0.3623(18) 0.084 Uiso 1 1 calc R U . . .
H24C H 0.4896(13) -0.339(4) 0.449(2) 0.084 Uiso 1 1 calc R U . . .
O3 O 0.18938(13) 0.1827(3) 0.40430(18) 0.0344(7) Uani 1 1 d D . . . .
C30 C 0.1451(2) 0.2763(5) 0.3402(3) 0.0291(9) Uani 1 1 d D . . . .
C31 C 0.1334(2) 0.2027(6) 0.2520(3) 0.0431(12) Uani 1 1 d . . . . .
H31A H 0.1129(15) 0.098(3) 0.2474(8) 0.065 Uiso 1 1 calc R U . . .
H31B H 0.1746(11) 0.190(4) 0.2453(9) 0.065 Uiso 1 1 calc R U . . .
H31C H 0.1056(15) 0.274(3) 0.2087(12) 0.065 Uiso 1 1 calc R U . . .
C32 C 0.1731(2) 0.4496(5) 0.3428(3) 0.0401(11) Uani 1 1 d . . . . .
H32A H 0.2137(13) 0.4441(6) 0.3315(19) 0.060 Uiso 1 1 calc R U . . .
H32B H 0.1825(14) 0.4974(19) 0.3992(16) 0.060 Uiso 1 1 calc R U . . .
H32C H 0.1408(10) 0.517(2) 0.2994(17) 0.060 Uiso 1 1 calc R U . . .
C33 C 0.0795(2) 0.2872(6) 0.3534(3) 0.0423(11) Uani 1 1 d . . . . .
H33A H 0.0648 0.1742 0.3576 0.051 Uiso 1 1 calc R U . . .
H33B H 0.0884 0.3400 0.4094 0.051 Uiso 1 1 calc R U . . .
C34 C 0.0220(3) 0.3772(7) 0.2876(4) 0.0685(18) Uani 1 1 d D . . . .
H34A H -0.0153(14) 0.376(4) 0.3049(15) 0.103 Uiso 1 1 calc R U . . .
H34B H 0.0104(14) 0.324(4) 0.2329(19) 0.103 Uiso 1 1 calc R U . . .
H34C H 0.0345(8) 0.489(4) 0.283(2) 0.103 Uiso 1 1 calc R U . . .
O4 O 0.32018(14) 0.1431(3) 0.62302(17) 0.0343(7) Uani 1 1 d D . . . .
C40 C 0.36025(19) 0.2279(4) 0.6939(2) 0.0254(8) Uani 1 1 d D . . . .
C41 C 0.3251(2) 0.2473(5) 0.7565(3) 0.0372(10) Uani 1 1 d D . . . .
H41A H 0.3154(13) 0.139(3) 0.7737(15) 0.056 Uiso 1 1 calc R U . . .
H41B H 0.2839(12) 0.308(3) 0.7289(9) 0.056 Uiso 1 1 calc R U . . .
H41C H 0.3535(9) 0.308(3) 0.8068(15) 0.056 Uiso 1 1 calc R U . . .
C42 C 0.3747(2) 0.3981(5) 0.6675(3) 0.0370(10) Uani 1 1 d D . . . .
H42A H 0.4003(14) 0.3877(5) 0.6314(18) 0.056 Uiso 1 1 calc R U . . .
H42B H 0.3997(14) 0.461(2) 0.7181(13) 0.056 Uiso 1 1 calc R U . . .
H42C H 0.3335(10) 0.454(2) 0.6362(18) 0.056 Uiso 1 1 calc R U . . .
C43 C 0.4252(2) 0.1336(5) 0.7366(3) 0.0343(10) Uani 1 1 d D . . . .
H43A H 0.4145 0.0260 0.7550 0.041 Uiso 1 1 calc R U . . .
H43B H 0.4443 0.1128 0.6929 0.041 Uiso 1 1 calc R U . . .
C44 C 0.4784(2) 0.2134(7) 0.8134(3) 0.0585(16) Uani 1 1 d D . . . .
H44A H 0.5161(14) 0.140(3) 0.8361(16) 0.088 Uiso 1 1 calc R U . . .
H44B H 0.4607(8) 0.235(4) 0.8575(17) 0.088 Uiso 1 1 calc R U . . .
H44C H 0.4924(14) 0.316(4) 0.7958(8) 0.088 Uiso 1 1 calc R U . . .


_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
K1 O3 2.605(3) . ?
K1 O2 2.614(3) . ?
K1 O4 2.635(3) . ?
K1 K2 3.6476(15) . ?
K1 K4 3.6554(13) . ?
K1 K3 3.6952(13) . ?
K2 O4 2.608(3) . ?
K2 O3 2.613(3) . ?
K2 O1 2.615(3) . ?
K2 C13 3.40(5) . ?
K2 C12B 3.475(12) 1_565 ?
K2 C10 3.48(5) . ?
K2 C12 3.48(8) 1_565 ?
K2 C10A 3.499(11) . ?
K2 C12A 3.504(12) 1_565 ?
K2 K3 3.6888(14) . ?
K2 K4 3.7265(14) . ?
K3 O1 2.605(3) . ?
K3 O4 2.622(3) . ?
K3 O2 2.622(3) . ?
K3 K4 3.6632(14) . ?
K4 O1 2.619(3) . ?
K4 O2 2.621(3) . ?
K4 O3 2.625(3) . ?
K4 C13A 3.421(10) . ?
K4 C32 3.463(4) 1_545 ?
K4 C30 3.525(4) . ?
K4 C10 3.55(4) . ?
O1 C10A 1.371(9) . ?
O1 C10 1.384(16) . ?
O1 C10B 1.398(10) . ?
C10 C12 1.534(17) . ?
C10 C11 1.535(17) . ?
C10 C13 1.544(17) . ?
C13 C14 1.537(18) . ?
C14 K4 2.91(5) 4_556 ?
C10A C11A 1.531(11) . ?
C10A C12A 1.535(11) . ?
C10A C13A 1.542(11) . ?
C13A C14A 1.536(12) . ?
C10B C12B 1.529(11) . ?
C10B C11B 1.540(11) . ?
C10B C13B 1.545(11) . ?
C13B C14B 1.535(13) . ?
O2 C20 1.384(4) . ?
C20 C21 1.535(6) . ?
C20 C23 1.535(6) . ?
C20 C22 1.545(5) . ?
C23 C24 1.531(6) . ?
O3 C30 1.383(4) . ?
C30 C33 1.536(6) . ?
C30 C32 1.538(5) . ?
C30 C31 1.538(6) . ?
C33 C34 1.522(7) . ?
O4 C40 1.378(4) . ?
C40 C41 1.531(5) . ?
C40 C42 1.531(5) . ?
C40 C43 1.539(5) . ?
C43 C44 1.529(6) . ?

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
O3 K1 O2 91.69(9) . . ?
O3 K1 O4 91.35(9) . . ?
O2 K1 O4 90.33(9) . . ?
O3 K1 K2 45.75(7) . . ?
O2 K1 K2 91.85(7) . . ?
O4 K1 K2 45.60(6) . . ?
O3 K1 K4 45.89(6) . . ?
O2 K1 K4 45.80(6) . . ?
O4 K1 K4 91.05(6) . . ?
K2 K1 K4 61.36(3) . . ?
O3 K1 K3 90.37(7) . . ?
O2 K1 K3 45.20(7) . . ?
O4 K1 K3 45.19(6) . . ?
K2 K1 K3 60.31(3) . . ?
K4 K1 K3 59.78(3) . . ?
O4 K2 O3 91.79(9) . . ?
O4 K2 O1 90.21(9) . . ?
O3 K2 O1 89.38(9) . . ?
O4 K2 C13 102.7(19) . . ?
O3 K2 C13 127.0(10) . . ?
O1 K2 C13 40.9(14) . . ?
O4 K2 C12B 94.8(2) . 1_565 ?
O3 K2 C12B 94.3(3) . 1_565 ?
O1 K2 C12B 173.7(3) . 1_565 ?
O4 K2 C10 106.6(11) . . ?
O3 K2 C10 101.1(9) . . ?
O1 K2 C10 20.7(10) . . ?
C13 K2 C10 25.9(4) . . ?
O4 K2 C12 102.1(19) . 1_565 ?
O3 K2 C12 88.4(17) . 1_565 ?
O1 K2 C12 167.6(18) . 1_565 ?
C13 K2 C12 135(3) . 1_565 ?
C10 K2 C12 149(2) . 1_565 ?
O4 K2 C10A 105.49(19) . . ?
O3 K2 C10A 101.5(2) . . ?
O1 K2 C10A 19.97(19) . . ?
O4 K2 C12A 100.2(3) . 1_565 ?
O3 K2 C12A 94.2(2) . 1_565 ?
O1 K2 C12A 168.8(3) . 1_565 ?
C10A K2 C12A 149.3(3) . 1_565 ?
O4 K2 K1 46.23(7) . . ?
O3 K2 K1 45.56(6) . . ?
O1 K2 K1 90.11(7) . . ?
C13 K2 K1 126.7(18) . . ?
C12B K2 K1 96.1(2) 1_565 . ?
C10 K2 K1 110.5(9) . . ?
C12 K2 K1 97(2) 1_565 . ?
C10A K2 K1 109.94(18) . . ?
C12A K2 K1 99.9(3) 1_565 . ?
O4 K2 K3 45.29(6) . . ?
O3 K2 K3 90.39(7) . . ?
O1 K2 K3 44.93(7) . . ?
C13 K2 K3 67.8(19) . . ?
C12B K2 K3 140.0(2) 1_565 . ?
C10 K2 K3 62.5(10) . . ?
C12 K2 K3 147.3(19) 1_565 . ?
C10A K2 K3 61.47(18) . . ?
C12A K2 K3 145.4(3) 1_565 . ?
K1 K2 K3 60.48(3) . . ?
O4 K2 K4 89.93(7) . . ?
O3 K2 K4 44.78(6) . . ?
O1 K2 K4 44.64(7) . . ?
C13 K2 K4 84.1(12) . . ?
C12B K2 K4 139.0(3) 1_565 . ?
C10 K2 K4 59.0(9) . . ?
C12 K2 K4 132.3(17) 1_565 . ?
C10A K2 K4 58.99(19) . . ?
C12A K2 K4 138.3(2) 1_565 . ?
K1 K2 K4 59.42(3) . . ?
K3 K2 K4 59.21(3) . . ?
O1 K3 O4 90.13(9) . . ?
O1 K3 O2 91.29(9) . . ?
O4 K3 O2 90.46(9) . . ?
O1 K3 K4 45.62(7) . . ?
O4 K3 K4 91.10(6) . . ?
O2 K3 K4 45.68(6) . . ?
O1 K3 K2 45.15(6) . . ?
O4 K3 K2 44.98(6) . . ?
O2 K3 K2 90.80(6) . . ?
K4 K3 K2 60.91(3) . . ?
O1 K3 K1 89.23(7) . . ?
O4 K3 K1 45.49(7) . . ?
O2 K3 K1 45.02(6) . . ?
K4 K3 K1 59.57(3) . . ?
K2 K3 K1 59.21(3) . . ?
O1 K4 O2 91.01(9) . . ?
O1 K4 O3 89.05(9) . . ?
O2 K4 O3 91.07(9) . . ?
O1 K4 C14 152.5(17) . 4 ?
O2 K4 C14 112.7(19) . 4 ?
O3 K4 C14 103.6(15) . 4 ?
O1 K4 C13A 43.11(17) . . ?
O2 K4 C13A 130.77(19) . . ?
O3 K4 C13A 102.4(2) . . ?
O1 K4 C32 94.08(10) . 1_545 ?
O2 K4 C32 95.97(10) . 1_545 ?
O3 K4 C32 172.24(10) . 1_545 ?
C14 K4 C32 70.6(14) 4 1_545 ?
C13A K4 C32 75.4(2) . 1_545 ?
O1 K4 C30 102.03(10) . . ?
O2 K4 C30 105.63(9) . . ?
O3 K4 C30 19.88(8) . . ?
C14 K4 C30 85.4(15) 4 . ?
C13A K4 C30 101.6(2) . . ?
C32 K4 C30 152.62(10) 1_545 . ?
O1 K4 C10 19.3(8) . . ?
O2 K4 C10 107.2(9) . . ?
O3 K4 C10 99.0(12) . . ?
C14 K4 C10 133.2(14) 4 . ?
C32 K4 C10 82.1(11) 1_545 . ?
C30 K4 C10 106.7(13) . . ?
O1 K4 K1 89.89(7) . . ?
O2 K4 K1 45.63(6) . . ?
O3 K4 K1 45.43(6) . . ?
C14 K4 K1 116.4(15) 4 . ?
C13A K4 K1 128.11(18) . . ?
C32 K4 K1 141.51(9) 1_545 . ?
C30 K4 K1 61.33(7) . . ?
C10 K4 K1 108.7(8) . . ?
O1 K4 K3 45.32(7) . . ?
O2 K4 K3 45.69(7) . . ?
O3 K4 K3 90.76(6) . . ?
C14 K4 K3 155.0(19) 4 . ?
C13A K4 K3 86.51(17) . . ?
C32 K4 K3 96.50(8) 1_545 . ?
C30 K4 K3 110.60(7) . . ?
C10 K4 K3 62.1(9) . . ?
K1 K4 K3 60.65(2) . . ?
O1 K4 K2 44.57(6) . . ?
O2 K4 K2 89.98(7) . . ?
O3 K4 K2 44.53(7) . . ?
C14 K4 K2 142.9(17) 4 . ?
C13A K4 K2 69.86(19) . . ?
C32 K4 K2 138.42(8) 1_545 . ?
C30 K4 K2 59.54(7) . . ?
C10 K4 K2 57.0(11) . . ?
K1 K4 K2 59.22(3) . . ?
K3 K4 K2 59.88(3) . . ?
C10A O1 K3 132.8(5) . . ?
C10 O1 K3 136(3) . . ?
C10B O1 K3 125.7(5) . . ?
C10A O1 K2 119.4(6) . . ?
C10 O1 K2 117(3) . . ?
C10B O1 K2 121.0(5) . . ?
K3 O1 K2 89.92(9) . . ?
C10A O1 K4 123.4(5) . . ?
C10 O1 K4 122(2) . . ?
C10B O1 K4 129.2(5) . . ?
K3 O1 K4 89.06(9) . . ?
K2 O1 K4 90.80(9) . . ?
O1 C10 C12 106(7) . . ?
O1 C10 C11 124(6) . . ?
C12 C10 C11 109(2) . . ?
O1 C10 C13 99(4) . . ?
C12 C10 C13 109(2) . . ?
C11 C10 C13 110(2) . . ?
O1 C10 K2 42(2) . . ?
C12 C10 K2 146(5) . . ?
C11 C10 K2 101(5) . . ?
C13 C10 K2 74(2) . . ?
O1 C10 K4 38.7(17) . . ?
C12 C10 K4 98(5) . . ?
C11 C10 K4 93(5) . . ?
C13 C10 K4 136(3) . . ?
K2 C10 K4 64.0(6) . . ?
C14 C13 C10 115(2) . . ?
C14 C13 K2 166(3) . . ?
C10 C13 K2 80(2) . . ?
C13 C14 K4 132(5) . 4_556 ?
O1 C10A C11A 107.4(9) . . ?
O1 C10A C12A 113.0(10) . . ?
C11A C10A C12A 111.0(9) . . ?
O1 C10A C13A 106.8(8) . . ?
C11A C10A C13A 111.4(9) . . ?
C12A C10A C13A 107.3(9) . . ?
O1 C10A K2 40.6(4) . . ?
C11A C10A K2 72.2(7) . . ?
C12A C10A K2 146.5(8) . . ?
C13A C10A K2 101.7(6) . . ?
C14A C13A C10A 113.3(9) . . ?
C14A C13A K4 163.4(7) . . ?
C10A C13A K4 82.4(5) . . ?
O1 C10B C12B 107.9(9) . . ?
O1 C10B C11B 113.2(9) . . ?
C12B C10B C11B 106.4(9) . . ?
O1 C10B C13B 112.6(10) . . ?
C12B C10B C13B 109.3(9) . . ?
C11B C10B C13B 107.0(9) . . ?
C14B C13B C10B 114.3(10) . . ?
C20 O2 K1 128.6(2) . . ?
C20 O2 K4 125.1(2) . . ?
K1 O2 K4 88.57(9) . . ?
C20 O2 K3 124.1(2) . . ?
K1 O2 K3 89.77(9) . . ?
K4 O2 K3 88.63(9) . . ?
O2 C20 C21 110.4(3) . . ?
O2 C20 C23 109.2(3) . . ?
C21 C20 C23 109.8(3) . . ?
O2 C20 C22 110.3(3) . . ?
C21 C20 C22 108.0(3) . . ?
C23 C20 C22 109.1(3) . . ?
C24 C23 C20 118.2(4) . . ?
C30 O3 K1 131.0(2) . . ?
C30 O3 K2 126.0(2) . . ?
K1 O3 K2 88.69(9) . . ?
C30 O3 K4 119.9(2) . . ?
K1 O3 K4 88.68(9) . . ?
K2 O3 K4 90.69(9) . . ?
O3 C30 C33 109.7(4) . . ?
O3 C30 C32 109.5(3) . . ?
C33 C30 C32 109.0(4) . . ?
O3 C30 C31 110.9(3) . . ?
C33 C30 C31 109.7(4) . . ?
C32 C30 C31 108.0(4) . . ?
O3 C30 K4 40.19(16) . . ?
C33 C30 K4 103.2(2) . . ?
C32 C30 K4 142.9(3) . . ?
C31 C30 K4 76.9(2) . . ?
C34 C33 C30 119.0(4) . . ?
C40 O4 K2 126.0(2) . . ?
C40 O4 K3 126.3(2) . . ?
K2 O4 K3 89.73(9) . . ?
C40 O4 K1 125.5(2) . . ?
K2 O4 K1 88.16(8) . . ?
K3 O4 K1 89.32(9) . . ?
O4 C40 C41 109.4(3) . . ?
O4 C40 C42 109.8(3) . . ?
C41 C40 C42 108.6(3) . . ?
O4 C40 C43 109.4(3) . . ?
C41 C40 C43 110.0(3) . . ?
C42 C40 C43 109.7(3) . . ?
C44 C43 C40 117.5(4) . . ?

_refine_diff_density_max         0.561
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.079

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: n-hexane'
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_JKM2
_database_code_depnum_ccdc_archive 'CCDC 1837114'
_audit_update_record             
;
2018-05-30 deposited with the CCDC.
2018-05-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 H11 Cs O'
_chemical_formula_weight         220.05

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'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   19.114(3)
_cell_length_b                   8.8747(15)
_cell_length_c                   20.401(3)
_cell_angle_alpha                90
_cell_angle_beta                 117.105(4)
_cell_angle_gamma                90
_cell_volume                     3080.6(9)
_cell_formula_units_Z            16
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7726
_cell_measurement_theta_min      2.2429
_cell_measurement_theta_max      26.7328

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_F_000             1664
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    4.714
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6471
_exptl_absorpt_correction_T_max  0.8649
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Smart'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37696
_diffrn_reflns_av_unetI/netI     0.0731
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.121
_diffrn_reflns_theta_max         27.890
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.006
_diffrn_measured_fraction_theta_full 1.008
_diffrn_reflns_Laue_measured_fraction_max 1.006
_diffrn_reflns_Laue_measured_fraction_full 1.008
_diffrn_reflns_point_group_measured_fraction_max 1.006
_diffrn_reflns_point_group_measured_fraction_full 1.008
_reflns_number_total             7562
_reflns_number_gt                5474
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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.
;

_computing_data_collection       APEX2
_computing_cell_refinement       APEX2
_computing_data_reduction        APEX2
_computing_structure_solution    ShelXS
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ShelXP
_computing_publication_material  XCIF

_refine_special_details          'Refined as a 2-component twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1387P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7562
_refine_ls_number_parameters     280
_refine_ls_number_restraints     128
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0695
_refine_ls_wR_factor_ref         0.2364
_refine_ls_wR_factor_gt          0.2090
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_restrained_S_all      1.142
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000

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
Cs1 Cs 0.47909(6) 0.17064(11) 0.34366(5) 0.0298(2) Uani 1 1 d . . . . .
Cs2 Cs 0.37854(6) -0.16756(11) 0.18352(5) 0.0298(2) Uani 1 1 d . . . . .
Cs3 Cs 0.06266(5) -0.61574(10) 0.18747(5) 0.0277(2) Uani 1 1 d . . . . .
Cs4 Cs 0.10767(6) -0.27922(10) 0.34464(5) 0.0289(2) Uani 1 1 d . . . . .
O1 O 0.4824(6) -0.1555(11) 0.3424(5) 0.029(2) Uani 1 1 d D . . . .
C10 C 0.4760(9) -0.2483(16) 0.3935(8) 0.035(4) Uani 1 1 d D . . . .
C11 C 0.5563(10) -0.264(2) 0.4629(10) 0.051(5) Uani 1 1 d D . . . .
H11A H 0.5955 -0.3021 0.4485 0.076 Uiso 1 1 calc R U . . .
H11B H 0.5512 -0.3356 0.4972 0.076 Uiso 1 1 calc R U . . .
H11C H 0.5729 -0.1661 0.4868 0.076 Uiso 1 1 calc R U . . .
C12 C 0.4497(12) -0.4063(18) 0.3612(10) 0.046(5) Uani 1 1 d D . . . .
H12A H 0.3990 -0.3995 0.3169 0.069 Uiso 1 1 calc R U . . .
H12B H 0.4442 -0.4706 0.3977 0.069 Uiso 1 1 calc R U . . .
H12C H 0.4889 -0.4497 0.3483 0.069 Uiso 1 1 calc R U . . .
C13 C 0.4180(10) -0.184(2) 0.4207(10) 0.046(4) Uani 1 1 d D . . . .
H13A H 0.4118 -0.2585 0.4536 0.055 Uiso 1 1 calc R U . . .
H13B H 0.4416 -0.0919 0.4502 0.055 Uiso 1 1 calc R U . . .
C14 C 0.3377(10) -0.144(3) 0.3604(10) 0.057(6) Uani 1 1 d D . . . .
H14A H 0.3046 -0.1078 0.3822 0.086 Uiso 1 1 calc R U . . .
H14B H 0.3137 -0.2339 0.3305 0.086 Uiso 1 1 calc R U . . .
H14C H 0.3426 -0.0653 0.3291 0.086 Uiso 1 1 calc R U . . .
O2 O 0.3838(6) 0.1593(12) 0.1842(6) 0.032(2) Uani 1 1 d D . . . .
C20 C 0.3187(9) 0.2520(17) 0.1497(9) 0.034(3) Uani 0.88 1 d D U P A 1
C21 C 0.3431(14) 0.412(2) 0.1379(12) 0.041(4) Uani 0.88 1 d D U P A 1
H21A H 0.3822 0.4528 0.1851 0.062 Uiso 0.88 1 calc R U P A 1
H21B H 0.2968 0.4778 0.1176 0.062 Uiso 0.88 1 calc R U P A 1
H21C H 0.3658 0.4071 0.1035 0.062 Uiso 0.88 1 calc R U P A 1
C22 C 0.2781(12) 0.272(3) 0.1993(11) 0.051(5) Uani 0.88 1 d D U P A 1
H22A H 0.3161 0.3100 0.2475 0.077 Uiso 0.88 1 calc R U P A 1
H22B H 0.2578 0.1741 0.2055 0.077 Uiso 0.88 1 calc R U P A 1
H22C H 0.2346 0.3432 0.1765 0.077 Uiso 0.88 1 calc R U P A 1
C23 C 0.2597(11) 0.189(2) 0.0733(9) 0.039(3) Uani 0.88 1 d D U P A 1
H23A H 0.2341 0.0983 0.0812 0.047 Uiso 0.88 1 calc R U P A 1
H23B H 0.2181 0.2649 0.0482 0.047 Uiso 0.88 1 calc R U P A 1
C24 C 0.2944(12) 0.147(2) 0.0232(11) 0.045(4) Uani 0.88 1 d D U P A 1
H24A H 0.2529 0.1082 -0.0233 0.067 Uiso 0.88 1 calc R U P A 1
H24B H 0.3345 0.0690 0.0466 0.067 Uiso 0.88 1 calc R U P A 1
H24C H 0.3184 0.2361 0.0134 0.067 Uiso 0.88 1 calc R U P A 1
C20A C 0.315(3) 0.115(8) 0.124(3) 0.037(4) Uiso 0.12 1 d D U P A 3
C21A C 0.324(7) -0.019(10) 0.079(6) 0.040(8) Uiso 0.12 1 d D U P A 3
H21D H 0.3189 -0.1141 0.1012 0.059 Uiso 0.12 1 calc R U P A 3
H21E H 0.3756 -0.0145 0.0802 0.059 Uiso 0.12 1 calc R U P A 3
H21F H 0.2827 -0.0134 0.0281 0.059 Uiso 0.12 1 calc R U P A 3
C22A C 0.240(5) 0.082(13) 0.132(6) 0.038(10) Uiso 0.12 1 d D U P A 3
H22D H 0.2476 -0.0095 0.1608 0.057 Uiso 0.12 1 calc R U P A 3
H22E H 0.1954 0.0690 0.0828 0.057 Uiso 0.12 1 calc R U P A 3
H22F H 0.2295 0.1673 0.1567 0.057 Uiso 0.12 1 calc R U P A 3
C23A C 0.300(6) 0.257(9) 0.074(4) 0.036(4) Uiso 0.12 1 d D U P A 3
H23C H 0.3193 0.2357 0.0370 0.043 Uiso 0.12 1 calc R U P A 3
H23D H 0.2430 0.2753 0.0469 0.043 Uiso 0.12 1 calc R U P A 3
C24A C 0.340(10) 0.398(9) 0.115(7) 0.035(8) Uiso 0.12 1 d D U P A 3
H24D H 0.3266 0.4822 0.0801 0.053 Uiso 0.12 1 calc R U P A 3
H24E H 0.3967 0.3835 0.1398 0.053 Uiso 0.12 1 calc R U P A 3
H24F H 0.3212 0.4210 0.1515 0.053 Uiso 0.12 1 calc R U P A 3
O3 O 0.1020(6) -0.6034(12) 0.3432(6) 0.034(2) Uani 1 1 d D . . . .
C30 C 0.1566(10) -0.6991(17) 0.3957(8) 0.036(4) Uani 1 1 d D . . . .
C31 C 0.1171(13) -0.852(2) 0.3952(15) 0.068(7) Uani 1 1 d . . . . .
H31A H 0.0948 -0.8953 0.3456 0.102 Uiso 1 1 calc R U . . .
H31B H 0.0752 -0.8360 0.4095 0.102 Uiso 1 1 calc R U . . .
H31C H 0.1564 -0.9211 0.4301 0.102 Uiso 1 1 calc R U . . .
C32 C 0.1896(14) -0.640(3) 0.4720(11) 0.062(6) Uani 1 1 d . . . . .
H32A H 0.1466 -0.6145 0.4836 0.093 Uiso 1 1 calc R U . . .
H32B H 0.2208 -0.5495 0.4762 0.093 Uiso 1 1 calc R U . . .
H32C H 0.2231 -0.7167 0.5065 0.093 Uiso 1 1 calc R U . . .
C33 C 0.2252(12) -0.735(2) 0.3784(11) 0.046(4) Uani 1 1 d . . . . .
H33A H 0.2048 -0.7952 0.3326 0.055 Uiso 1 1 calc R U . . .
H33B H 0.2639 -0.7981 0.4187 0.055 Uiso 1 1 calc R U . . .
C34 C 0.2683(12) -0.594(3) 0.3690(12) 0.066(7) Uani 1 1 d . . . . .
H34A H 0.3111 -0.6259 0.3583 0.099 Uiso 1 1 calc R U . . .
H34B H 0.2899 -0.5343 0.4145 0.099 Uiso 1 1 calc R U . . .
H34C H 0.2310 -0.5318 0.3283 0.099 Uiso 1 1 calc R U . . .
O4 O 0.0567(6) -0.2910(11) 0.1857(5) 0.028(2) Uani 1 1 d D . . . .
C40 C 0.0880(10) -0.1978(17) 0.1512(9) 0.035(4) Uani 1 1 d D . . . .
C41 C 0.1582(12) -0.268(3) 0.1478(12) 0.055(5) Uani 1 1 d . . . . .
H41A H 0.1430 -0.3644 0.1218 0.082 Uiso 1 1 calc R U . . .
H41B H 0.2000 -0.2843 0.1979 0.082 Uiso 1 1 calc R U . . .
H41C H 0.1773 -0.2000 0.1215 0.082 Uiso 1 1 calc R U . . .
C42 C 0.1136(13) -0.048(2) 0.1913(12) 0.055(5) Uani 1 1 d . . . . .
H42A H 0.0688 -0.0002 0.1942 0.083 Uiso 1 1 calc R U . . .
H42B H 0.1325 0.0185 0.1643 0.083 Uiso 1 1 calc R U . . .
H42C H 0.1559 -0.0646 0.2411 0.083 Uiso 1 1 calc R U . . .
C43 C 0.0253(12) -0.157(2) 0.0715(10) 0.047(5) Uani 1 1 d . . . . .
H43A H -0.0167 -0.0967 0.0743 0.056 Uiso 1 1 calc R U . . .
H43B H 0.0503 -0.0942 0.0481 0.056 Uiso 1 1 calc R U . . .
C44 C -0.0124(11) -0.297(3) 0.0222(10) 0.056(6) Uani 1 1 d . . . . .
H44A H -0.0509 -0.2632 -0.0269 0.085 Uiso 1 1 calc R U . . .
H44B H -0.0387 -0.3584 0.0441 0.085 Uiso 1 1 calc R U . . .
H44C H 0.0286 -0.3563 0.0181 0.085 Uiso 1 1 calc R U . . .


_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
Cs1 O1 2.895(10) . ?
Cs1 O2 2.918(11) . ?
Cs1 O2 2.925(11) 2_655 ?
Cs1 C20A 3.71(6) 2_655 ?
Cs1 C21A 3.75(11) 2_655 ?
Cs1 C24A 3.76(17) 2_655 ?
Cs1 C20 3.810(15) . ?
Cs1 C12 3.838(16) 1_565 ?
Cs1 C23A 3.84(11) 2_655 ?
Cs1 C10 3.862(13) . ?
Cs1 C20 3.872(15) 2_655 ?
Cs1 C21 3.89(2) 2_655 ?
Cs2 C20A 2.81(7) . ?
Cs2 O2 2.902(10) . ?
Cs2 O1 2.932(10) . ?
Cs2 O1 2.938(10) 2_655 ?
Cs2 C11 3.821(19) 2_655 ?
Cs2 C21 3.830(18) 1_545 ?
Cs2 C10 3.834(13) 2_655 ?
Cs2 C20 3.864(15) . ?
Cs2 C10 3.882(14) . ?
Cs2 Cs2 4.176(2) 2_655 ?
Cs2 Cs1 4.2539(14) 2_655 ?
Cs3 O4 2.884(9) . ?
Cs3 O3 2.915(11) . ?
Cs3 O3 2.917(11) 2 ?
Cs3 C31 3.71(2) 2 ?
Cs3 C30 3.810(16) 2 ?
Cs3 C40 3.856(14) . ?
Cs3 C30 3.856(15) . ?
Cs3 C33 3.863(19) . ?
Cs3 Cs4 4.1746(14) . ?
Cs3 Cs3 4.2207(19) 2 ?
Cs3 Cs4 4.2432(14) 2 ?
Cs4 O3 2.879(11) . ?
Cs4 O4 2.914(10) 2 ?
Cs4 O4 2.932(10) . ?
Cs4 C43 3.810(19) 2 ?
Cs4 C40 3.847(15) 2 ?
Cs4 C40 3.858(14) . ?
Cs4 C30 3.868(14) . ?
Cs4 C44 3.903(18) 2 ?
Cs4 C31 3.91(2) 1_565 ?
Cs4 Cs4 4.168(2) 2 ?
Cs4 Cs3 4.2432(14) 2 ?
O1 C10 1.378(13) . ?
O1 Cs2 2.938(10) 2_655 ?
C10 C12 1.533(19) . ?
C10 C11 1.55(2) . ?
C10 C13 1.556(19) . ?
C10 Cs2 3.834(13) 2_655 ?
C13 C14 1.51(2) . ?
O2 C20 1.386(14) . ?
O2 C20A 1.389(18) . ?
O2 Cs1 2.925(11) 2_655 ?
C20 C22 1.54(2) . ?
C20 C21 1.55(2) . ?
C20 C23 1.56(2) . ?
C20 Cs1 3.873(15) 2_655 ?
C21 Cs1 3.89(2) 2_655 ?
C23 C24 1.50(2) . ?
C20A C22A 1.54(2) . ?
C20A C21A 1.55(2) . ?
C20A C23A 1.56(2) . ?
C20A Cs1 3.71(6) 2_655 ?
C21A Cs1 3.75(11) 2_655 ?
C23A C24A 1.50(3) . ?
C23A Cs1 3.84(11) 2_655 ?
O3 C30 1.393(14) . ?
O3 Cs3 2.917(11) 2 ?
C30 C32 1.48(3) . ?
C30 C33 1.54(3) . ?
C30 C31 1.55(3) . ?
C30 Cs3 3.810(16) 2 ?
C33 C34 1.56(3) . ?
O4 C40 1.386(13) . ?
O4 Cs4 2.914(10) 2 ?
C40 C41 1.51(2) . ?
C40 C42 1.52(3) . ?
C40 C43 1.56(2) . ?
C40 Cs4 3.847(15) 2 ?
C43 C44 1.55(3) . ?
C43 Cs4 3.810(19) 2 ?
C44 Cs4 3.903(18) 2 ?

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 Cs1 O2 87.7(3) . . ?
O1 Cs1 O2 86.5(3) . 2_655 ?
O2 Cs1 O2 86.7(3) . 2_655 ?
O1 Cs1 C20A 81.0(11) . 2_655 ?
O2 Cs1 C20A 105.6(9) . 2_655 ?
O2 Cs1 C20A 20.0(9) 2_655 2_655 ?
O1 Cs1 C21A 62.2(14) . 2_655 ?
O2 Cs1 C21A 116.7(17) . 2_655 ?
O2 Cs1 C21A 41.4(13) 2_655 2_655 ?
C20A Cs1 C21A 24.0(5) 2_655 2_655 ?
O1 Cs1 C24A 121.1(13) . 2_655 ?
O2 Cs1 C24A 108(2) . 2_655 ?
O2 Cs1 C24A 41.1(17) 2_655 2_655 ?
C20A Cs1 C24A 40.4(12) 2_655 2_655 ?
C21A Cs1 C24A 60.1(12) 2_655 2_655 ?
O1 Cs1 C20 101.0(3) . . ?
O2 Cs1 C20 18.3(3) . . ?
O2 Cs1 C20 100.0(3) 2_655 . ?
O1 Cs1 C12 169.6(3) . 1_565 ?
O2 Cs1 C12 95.4(4) . 1_565 ?
O2 Cs1 C12 103.5(3) 2_655 1_565 ?
C20A Cs1 C12 107.6(12) 2_655 1_565 ?
C21A Cs1 C12 124.2(15) 2_655 1_565 ?
C24A Cs1 C12 67.2(14) 2_655 1_565 ?
C20 Cs1 C12 80.1(4) . 1_565 ?
O1 Cs1 C23A 100.3(11) . 2_655 ?
O2 Cs1 C23A 119.9(13) . 2_655 ?
O2 Cs1 C23A 35.8(12) 2_655 2_655 ?
C20A Cs1 C23A 23.8(6) 2_655 2_655 ?
C21A Cs1 C23A 38.2(9) 2_655 2_655 ?
C24A Cs1 C23A 22.8(7) 2_655 2_655 ?
C12 Cs1 C23A 86.7(11) 1_565 2_655 ?
O1 Cs1 C10 16.9(3) . . ?
O2 Cs1 C10 100.6(3) . . ?
O2 Cs1 C10 98.1(3) 2_655 . ?
C20A Cs1 C10 88.1(11) 2_655 . ?
C21A Cs1 C10 65.8(12) 2_655 . ?
C24A Cs1 C10 125.5(13) 2_655 . ?
C20 Cs1 C10 110.8(4) . . ?
C12 Cs1 C10 153.7(3) 1_565 . ?
C23A Cs1 C10 102.9(12) 2_655 . ?
O1 Cs1 C20 99.3(3) . 2_655 ?
O2 Cs1 C20 98.7(3) . 2_655 ?
O2 Cs1 C20 17.3(3) 2_655 2_655 ?
C20 Cs1 C20 108.6(3) . 2_655 ?
C12 Cs1 C20 90.0(4) 1_565 2_655 ?
C10 Cs1 C20 107.8(3) . 2_655 ?
O1 Cs1 C21 122.0(3) . 2_655 ?
O2 Cs1 C21 101.6(4) . 2_655 ?
O2 Cs1 C21 38.5(3) 2_655 2_655 ?
C20 Cs1 C21 104.5(4) . 2_655 ?
C12 Cs1 C21 67.1(4) 1_565 2_655 ?
C10 Cs1 C21 128.5(4) . 2_655 ?
C20 Cs1 C21 23.0(3) 2_655 2_655 ?
C20A Cs2 O2 28.1(5) . . ?
C20A Cs2 O1 112.9(9) . . ?
O2 Cs2 O1 87.4(3) . . ?
C20A Cs2 O1 97.8(15) . 2_655 ?
O2 Cs2 O1 86.1(3) . 2_655 ?
O1 Cs2 O1 89.1(3) . 2_655 ?
C20A Cs2 C11 95.2(16) . 2_655 ?
O2 Cs2 C11 101.9(4) . 2_655 ?
O1 Cs2 C11 125.1(3) . 2_655 ?
O1 Cs2 C11 39.1(3) 2_655 2_655 ?
O2 Cs2 C21 167.6(4) . 1_545 ?
O1 Cs2 C21 105.1(4) . 1_545 ?
O1 Cs2 C21 93.8(4) 2_655 1_545 ?
C11 Cs2 C21 71.0(4) 2_655 1_545 ?
C20A Cs2 C10 103.8(16) . 2_655 ?
O2 Cs2 C10 99.1(3) . 2_655 ?
O1 Cs2 C10 102.0(3) . 2_655 ?
O1 Cs2 C10 18.0(3) 2_655 2_655 ?
C11 Cs2 C10 23.4(3) 2_655 2_655 ?
C21 Cs2 C10 78.4(4) 1_545 2_655 ?
O2 Cs2 C20 17.1(3) . . ?
O1 Cs2 C20 99.1(3) . . ?
O1 Cs2 C20 98.7(3) 2_655 . ?
C11 Cs2 C20 104.6(4) 2_655 . ?
C21 Cs2 C20 152.9(4) 1_545 . ?
C10 Cs2 C20 108.5(4) 2_655 . ?
C20A Cs2 C10 122.6(11) . . ?
O2 Cs2 C10 100.4(3) . . ?
O1 Cs2 C10 17.0(3) . . ?
O1 Cs2 C10 100.8(3) 2_655 . ?
C11 Cs2 C10 131.1(3) 2_655 . ?
C21 Cs2 C10 91.8(4) 1_545 . ?
C10 Cs2 C10 110.2(3) 2_655 . ?
C20 Cs2 C10 109.2(3) . . ?
C20A Cs2 Cs2 114.5(7) . 2_655 ?
O2 Cs2 Cs2 88.4(2) . 2_655 ?
O1 Cs2 Cs2 44.71(19) . 2_655 ?
O1 Cs2 Cs2 44.6(2) 2_655 2_655 ?
C11 Cs2 Cs2 81.1(2) 2_655 2_655 ?
C21 Cs2 Cs2 100.3(4) 1_545 2_655 ?
C10 Cs2 Cs2 57.8(2) 2_655 2_655 ?
C20 Cs2 Cs2 105.5(2) . 2_655 ?
C10 Cs2 Cs2 56.7(2) . 2_655 ?
C20A Cs2 Cs1 69.8(7) . . ?
O2 Cs2 Cs1 43.9(2) . . ?
O1 Cs2 Cs1 43.5(2) . . ?
O1 Cs2 Cs1 89.02(19) 2_655 . ?
C11 Cs2 Cs1 124.9(3) 2_655 . ?
C21 Cs2 Cs1 148.5(3) 1_545 . ?
C10 Cs2 Cs1 107.0(2) 2_655 . ?
C20 Cs2 Cs1 56.2(2) . . ?
C10 Cs2 Cs1 56.9(2) . . ?
Cs2 Cs2 Cs1 61.03(2) 2_655 . ?
C20A Cs2 Cs1 59.3(12) . 2_655 ?
O2 Cs2 Cs1 43.3(2) . 2_655 ?
O1 Cs2 Cs1 88.10(19) . 2_655 ?
O1 Cs2 Cs1 42.8(2) 2_655 2_655 ?
C11 Cs2 Cs1 66.5(3) 2_655 2_655 ?
C21 Cs2 Cs1 135.1(3) 1_545 2_655 ?
C10 Cs2 Cs1 56.8(2) 2_655 2_655 ?
C20 Cs2 Cs1 56.7(2) . 2_655 ?
C10 Cs2 Cs1 105.1(2) . 2_655 ?
Cs2 Cs2 Cs1 59.78(2) 2_655 2_655 ?
Cs1 Cs2 Cs1 60.27(3) . 2_655 ?
O4 Cs3 O3 88.0(3) . . ?
O4 Cs3 O3 85.8(3) . 2 ?
O3 Cs3 O3 87.1(3) . 2 ?
O4 Cs3 C31 122.4(4) . 2 ?
O3 Cs3 C31 104.0(5) . 2 ?
O3 Cs3 C31 40.4(4) 2 2 ?
O4 Cs3 C30 99.2(3) . 2 ?
O3 Cs3 C30 100.3(3) . 2 ?
O3 Cs3 C30 18.5(3) 2 2 ?
C31 Cs3 C30 23.7(4) 2 2 ?
O4 Cs3 C40 17.0(3) . . ?
O3 Cs3 C40 100.4(3) . . ?
O3 Cs3 C40 98.1(3) 2 . ?
C31 Cs3 C40 128.9(4) 2 . ?
C30 Cs3 C40 108.1(4) 2 . ?
O4 Cs3 C30 101.6(3) . . ?
O3 Cs3 C30 17.6(3) . . ?
O3 Cs3 C30 99.2(3) 2 . ?
C31 Cs3 C30 105.2(5) 2 . ?
C30 Cs3 C30 108.6(3) 2 . ?
C40 Cs3 C30 111.1(3) . . ?
O4 Cs3 C33 107.2(4) . . ?
O3 Cs3 C33 38.9(4) . . ?
O3 Cs3 C33 121.3(4) 2 . ?
C31 Cs3 C33 117.1(5) 2 . ?
C30 Cs3 C33 127.7(4) 2 . ?
C40 Cs3 C33 110.1(4) . . ?
C30 Cs3 C33 23.0(4) . . ?
O4 Cs3 Cs4 44.59(19) . . ?
O3 Cs3 Cs4 43.6(2) . . ?
O3 Cs3 Cs4 87.9(2) 2 . ?
C31 Cs3 Cs4 125.3(4) 2 . ?
C30 Cs3 Cs4 106.3(2) 2 . ?
C40 Cs3 Cs4 57.3(2) . . ?
C30 Cs3 Cs4 57.4(2) . . ?
C33 Cs3 Cs4 68.4(3) . . ?
O4 Cs3 Cs3 88.71(18) . 2 ?
O3 Cs3 Cs3 43.7(2) . 2 ?
O3 Cs3 Cs3 43.6(2) 2 2 ?
C31 Cs3 Cs3 67.1(4) 2 2 ?
C30 Cs3 Cs3 57.1(2) 2 2 ?
C40 Cs3 Cs3 105.7(2) . 2 ?
C30 Cs3 Cs3 56.1(3) . 2 ?
C33 Cs3 Cs3 78.9(3) . 2 ?
Cs4 Cs3 Cs3 60.72(2) . 2 ?
O4 Cs3 Cs4 43.2(2) . 2 ?
O3 Cs3 Cs4 86.6(2) . 2 ?
O3 Cs3 Cs4 42.6(2) 2 2 ?
C31 Cs3 Cs4 80.8(3) 2 2 ?
C30 Cs3 Cs4 57.1(2) 2 2 ?
C40 Cs3 Cs4 56.5(2) . 2 ?
C30 Cs3 Cs4 104.2(2) . 2 ?
C33 Cs3 Cs4 123.8(3) . 2 ?
Cs4 Cs3 Cs4 59.35(3) . 2 ?
Cs3 Cs3 Cs4 59.10(2) 2 2 ?
O3 Cs4 O4 86.0(3) . 2 ?
O3 Cs4 O4 87.8(3) . . ?
O4 Cs4 O4 88.9(3) 2 . ?
O3 Cs4 C43 105.0(4) . 2 ?
O4 Cs4 C43 39.7(3) 2 2 ?
O4 Cs4 C43 123.6(4) . 2 ?
O3 Cs4 C40 98.9(3) . 2 ?
O4 Cs4 C40 17.6(3) 2 2 ?
O4 Cs4 C40 101.2(3) . 2 ?
C43 Cs4 C40 23.5(4) 2 2 ?
O3 Cs4 C40 101.0(3) . . ?
O4 Cs4 C40 101.3(3) 2 . ?
O4 Cs4 C40 17.6(3) . . ?
C43 Cs4 C40 129.2(4) 2 . ?
C40 Cs4 C40 110.2(3) 2 . ?
O3 Cs4 C30 16.9(3) . . ?
O4 Cs4 C30 97.3(3) 2 . ?
O4 Cs4 C30 100.4(3) . . ?
C43 Cs4 C30 106.3(4) 2 . ?
C40 Cs4 C30 107.1(4) 2 . ?
C40 Cs4 C30 110.8(3) . . ?
O3 Cs4 C44 86.6(4) . 2 ?
O4 Cs4 C44 49.2(3) 2 2 ?
O4 Cs4 C44 138.0(3) . 2 ?
C43 Cs4 C44 23.1(5) 2 2 ?
C40 Cs4 C44 39.2(4) 2 2 ?
C40 Cs4 C44 149.4(4) . 2 ?
C30 Cs4 C44 84.6(4) . 2 ?
O3 Cs4 C31 165.5(5) . 1_565 ?
O4 Cs4 C31 90.4(4) 2 1_565 ?
O4 Cs4 C31 106.2(4) . 1_565 ?
C43 Cs4 C31 64.3(5) 2 1_565 ?
C40 Cs4 C31 75.0(4) 2 1_565 ?
C40 Cs4 C31 93.4(5) . 1_565 ?
C30 Cs4 C31 152.4(4) . 1_565 ?
C44 Cs4 C31 80.5(5) 2 1_565 ?
O3 Cs4 Cs4 88.5(2) . 2 ?
O4 Cs4 Cs4 44.70(19) 2 2 ?
O4 Cs4 Cs4 44.4(2) . 2 ?
C43 Cs4 Cs4 80.6(3) 2 2 ?
C40 Cs4 Cs4 57.4(2) 2 2 ?
C40 Cs4 Cs4 57.1(3) . 2 ?
C30 Cs4 Cs4 105.4(2) . 2 ?
C44 Cs4 Cs4 93.9(3) 2 2 ?
C31 Cs4 Cs4 98.7(3) 1_565 2 ?
O3 Cs4 Cs3 44.2(2) . . ?
O4 Cs4 Cs3 89.21(18) 2 . ?
O4 Cs4 Cs3 43.66(18) . . ?
C43 Cs4 Cs3 127.0(3) 2 . ?
C40 Cs4 Cs3 106.8(2) 2 . ?
C40 Cs4 Cs3 57.2(2) . . ?
C30 Cs4 Cs3 57.2(2) . . ?
C44 Cs4 Cs3 120.5(4) 2 . ?
C31 Cs4 Cs3 149.8(4) 1_565 . ?
Cs4 Cs4 Cs3 61.15(2) 2 . ?
O3 Cs4 Cs3 43.3(2) . 2 ?
O4 Cs4 Cs3 42.67(18) 2 2 ?
O4 Cs4 Cs3 87.65(18) . 2 ?
C43 Cs4 Cs3 69.4(3) 2 2 ?
C40 Cs4 Cs3 56.7(2) 2 2 ?
C40 Cs4 Cs3 105.3(2) . 2 ?
C30 Cs4 Cs3 55.8(3) . 2 ?
C44 Cs4 Cs3 60.7(3) 2 2 ?
C31 Cs4 Cs3 131.5(3) 1_565 2 ?
Cs4 Cs4 Cs3 59.51(2) 2 2 ?
Cs3 Cs4 Cs3 60.18(3) . 2 ?
C10 O1 Cs1 125.5(9) . . ?
C10 O1 Cs2 124.5(9) . . ?
Cs1 O1 Cs2 92.3(3) . . ?
C10 O1 Cs2 121.0(8) . 2_655 ?
Cs1 O1 Cs2 93.6(3) . 2_655 ?
Cs2 O1 Cs2 90.7(3) . 2_655 ?
O1 C10 C12 110.2(13) . . ?
O1 C10 C11 110.7(13) . . ?
C12 C10 C11 107.6(14) . . ?
O1 C10 C13 111.9(12) . . ?
C12 C10 C13 110.1(13) . . ?
C11 C10 C13 106.2(13) . . ?
O1 C10 Cs2 41.1(6) . 2_655 ?
C12 C10 Cs2 98.7(9) . 2_655 ?
C11 C10 Cs2 77.9(9) . 2_655 ?
C13 C10 Cs2 147.5(10) . 2_655 ?
O1 C10 Cs1 37.6(6) . . ?
C12 C10 Cs1 143.9(10) . . ?
C11 C10 Cs1 101.7(10) . . ?
C13 C10 Cs1 80.7(9) . . ?
Cs2 C10 Cs1 67.1(2) 2_655 . ?
O1 C10 Cs2 38.5(7) . . ?
C12 C10 Cs2 78.2(9) . . ?
C11 C10 Cs2 143.4(10) . . ?
C13 C10 Cs2 105.3(9) . . ?
Cs2 C10 Cs2 65.5(2) 2_655 . ?
Cs1 C10 Cs2 65.7(2) . . ?
C14 C13 C10 114.8(14) . . ?
C20 O2 Cs2 124.8(9) . . ?
C20A O2 Cs2 72(3) . . ?
C20 O2 Cs1 120.3(9) . . ?
C20A O2 Cs1 149(3) . . ?
Cs2 O2 Cs1 92.4(3) . . ?
C20 O2 Cs1 123.9(9) . 2_655 ?
C20A O2 Cs1 114(3) . 2_655 ?
Cs2 O2 Cs1 93.8(3) . 2_655 ?
Cs1 O2 Cs1 93.2(3) . 2_655 ?
O2 C20 C22 109.8(13) . . ?
O2 C20 C21 111.1(14) . . ?
C22 C20 C21 106.1(14) . . ?
O2 C20 C23 111.6(13) . . ?
C22 C20 C23 110.3(14) . . ?
C21 C20 C23 107.9(13) . . ?
O2 C20 Cs1 41.4(7) . . ?
C22 C20 Cs1 75.3(10) . . ?
C21 C20 Cs1 100.3(11) . . ?
C23 C20 Cs1 147.7(11) . . ?
O2 C20 Cs2 38.1(7) . . ?
C22 C20 Cs2 100.8(11) . . ?
C21 C20 Cs2 145.7(12) . . ?
C23 C20 Cs2 81.4(9) . . ?
Cs1 C20 Cs2 66.4(2) . . ?
O2 C20 Cs1 38.8(7) . 2_655 ?
C22 C20 Cs1 142.3(11) . 2_655 ?
C21 C20 Cs1 79.0(11) . 2_655 ?
C23 C20 Cs1 103.0(9) . 2_655 ?
Cs1 C20 Cs1 67.1(2) . 2_655 ?
Cs2 C20 Cs1 66.7(2) . 2_655 ?
C20 C21 Cs1 77.9(10) . 2_655 ?
C24 C23 C20 115.4(14) . . ?
O2 C20A C22A 120(7) . . ?
O2 C20A C21A 115(7) . . ?
C22A C20A C21A 106(3) . . ?
O2 C20A C23A 100(5) . . ?
C22A C20A C23A 109(3) . . ?
C21A C20A C23A 106(3) . . ?
O2 C20A Cs2 80(3) . . ?
C22A C20A Cs2 91(4) . . ?
C21A C20A Cs2 55(4) . . ?
C23A C20A Cs2 156(5) . . ?
O2 C20A Cs1 46(2) . 2_655 ?
C22A C20A Cs1 165(5) . 2_655 ?
C21A C20A Cs1 79(5) . 2_655 ?
C23A C20A Cs1 83(4) . 2_655 ?
Cs2 C20A Cs1 80.1(15) . 2_655 ?
C20A C21A Cs1 77(5) . 2_655 ?
C24A C23A C20A 115(3) . . ?
C24A C23A Cs1 76(7) . 2_655 ?
C20A C23A Cs1 74(4) . 2_655 ?
C30 O3 Cs4 126.2(9) . . ?
C30 O3 Cs3 123.1(9) . . ?
Cs4 O3 Cs3 92.2(3) . . ?
C30 O3 Cs3 120.0(9) . 2 ?
Cs4 O3 Cs3 94.1(3) . 2 ?
Cs3 O3 Cs3 92.7(3) . 2 ?
O3 C30 C32 113.7(15) . . ?
O3 C30 C33 111.6(13) . . ?
C32 C30 C33 108.4(16) . . ?
O3 C30 C31 109.6(14) . . ?
C32 C30 C31 106.9(17) . . ?
C33 C30 C31 106.3(15) . . ?
O3 C30 Cs3 41.6(7) . 2 ?
C32 C30 Cs3 104.7(12) . 2 ?
C33 C30 Cs3 144.8(11) . 2 ?
C31 C30 Cs3 74.5(10) . 2 ?
O3 C30 Cs3 39.3(7) . . ?
C32 C30 Cs3 148.2(12) . . ?
C33 C30 Cs3 78.7(9) . . ?
C31 C30 Cs3 100.3(12) . . ?
Cs3 C30 Cs3 66.8(2) 2 . ?
O3 C30 Cs4 36.9(7) . . ?
C32 C30 Cs4 82.9(11) . . ?
C33 C30 Cs4 105.4(10) . . ?
C31 C30 Cs4 141.6(11) . . ?
Cs3 C30 Cs4 67.1(2) 2 . ?
Cs3 C30 Cs4 65.4(2) . . ?
C30 C33 C34 114.5(16) . . ?
C30 C33 Cs3 78.3(9) . . ?
C34 C33 Cs3 83.2(11) . . ?
C40 O4 Cs3 125.4(9) . . ?
C40 O4 Cs4 122.9(9) . 2 ?
Cs3 O4 Cs4 94.1(3) . 2 ?
C40 O4 Cs4 122.5(9) . . ?
Cs3 O4 Cs4 91.7(3) . . ?
Cs4 O4 Cs4 90.9(3) 2 . ?
O4 C40 C41 112.1(14) . . ?
O4 C40 C42 111.0(13) . . ?
C41 C40 C42 108.0(16) . . ?
O4 C40 C43 111.2(14) . . ?
C41 C40 C43 108.9(14) . . ?
C42 C40 C43 105.3(14) . . ?
O4 C40 Cs4 39.5(7) . 2 ?
C41 C40 Cs4 144.8(12) . 2 ?
C42 C40 Cs4 103.3(11) . 2 ?
C43 C40 Cs4 76.9(9) . 2 ?
O4 C40 Cs3 37.6(6) . . ?
C41 C40 Cs3 78.8(10) . . ?
C42 C40 Cs3 141.0(11) . . ?
C43 C40 Cs3 108.5(10) . . ?
Cs4 C40 Cs3 66.8(2) 2 . ?
O4 C40 Cs4 39.9(7) . . ?
C41 C40 Cs4 107.2(11) . . ?
C42 C40 Cs4 75.9(10) . . ?
C43 C40 Cs4 141.3(11) . . ?
Cs4 C40 Cs4 65.5(2) 2 . ?
Cs3 C40 Cs4 65.5(2) . . ?
C44 C43 C40 113.7(16) . . ?
C44 C43 Cs4 81.8(10) . 2 ?
C40 C43 Cs4 79.6(9) . 2 ?
C43 C44 Cs4 75.1(10) . 2 ?

_refine_diff_density_max         3.191
_refine_diff_density_min         -1.993
_refine_diff_density_rms         0.314

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: n-hexane'
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_JKM42
_database_code_depnum_ccdc_archive 'CCDC 1837113'
_audit_update_record             
;
2018-05-30 deposited with the CCDC.
2018-05-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 H11 O Rb'
_chemical_formula_weight         172.61

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'I a'
_space_group_name_Hall           'I -2ya'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y, z'
'x+1/2, y+1/2, z+1/2'
'x+1, -y+1/2, z+1/2'

_cell_length_a                   19.509(16)
_cell_length_b                   8.686(6)
_cell_length_c                   20.161(17)
_cell_angle_alpha                90
_cell_angle_beta                 116.48(2)
_cell_angle_gamma                90
_cell_volume                     3058(4)
_cell_formula_units_Z            16
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    1528
_cell_measurement_theta_min      2.2571
_cell_measurement_theta_max      19.0342

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_F_000             1376
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    6.381
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8336
_exptl_absorpt_correction_T_max  1.1588
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker smart'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12649
_diffrn_reflns_av_unetI/netI     0.1368
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.257
_diffrn_reflns_theta_max         27.928
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5571
_reflns_number_gt                1683
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_max     0.989
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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.
;

_computing_data_collection       APEX2
_computing_cell_refinement       APEX2
_computing_data_reduction        APEX2
_computing_structure_solution    ShelXS
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ShelXP
_computing_publication_material  XCIF

_refine_special_details          'Refined as a 2-component inversion twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0423P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5571
_refine_ls_number_parameters     292
_refine_ls_number_restraints     1123
_refine_ls_R_factor_all          0.1737
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.1045
_refine_ls_wR_factor_gt          0.0818
_refine_ls_goodness_of_fit_ref   0.715
_refine_ls_restrained_S_all      0.751
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001

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 0.17187(11) 0.8845(3) 0.05511(11) 0.1008(12) Uani 1 1 d D U . . .
Rb2 Rb 0.03602(14) 0.5605(3) 0.06831(13) 0.1101(12) Uani 1 1 d D U . . .
Rb3 Rb 0.11781(12) 0.8839(3) 0.22136(11) 0.1034(12) Uani 1 1 d D U . . .
Rb4 Rb 0.25311(13) 0.5582(3) 0.20701(13) 0.1074(12) Uani 1 1 d D U . . .
O1 O 0.1176(6) 0.5647(10) 0.2209(5) 0.103(4) Uani 1 1 d D U . . .
O2 O 0.2547(5) 0.8732(11) 0.2098(5) 0.093(4) Uani 1 1 d D U . . .
O3 O 0.1699(6) 0.5679(11) 0.0532(5) 0.107(5) Uani 1 1 d D U . . .
O4 O 0.0382(6) 0.8801(11) 0.0702(6) 0.113(5) Uani 1 1 d D U . . .
C10 C 0.1137(11) 0.471(2) 0.2759(10) 0.1075(8) Uani 0.51 1 d D U P A 1
C11 C 0.1923(10) 0.446(3) 0.3423(10) 0.102(7) Uani 0.51 1 d D U P A 1
H11A H 0.2270 0.4004 0.3255 0.152 Uiso 0.51 1 calc R U P A 1
H11B H 0.1869 0.3787 0.3780 0.152 Uiso 0.51 1 calc R U P A 1
H11C H 0.2126 0.5448 0.3655 0.152 Uiso 0.51 1 calc R U P A 1
C12 C 0.0760(16) 0.3127(18) 0.2400(14) 0.100(9) Uani 0.51 1 d D U P A 1
H12A H 0.0255 0.3310 0.1998 0.150 Uiso 0.51 1 calc R U P A 1
H12B H 0.0717 0.2481 0.2771 0.150 Uiso 0.51 1 calc R U P A 1
H12C H 0.1077 0.2617 0.2208 0.150 Uiso 0.51 1 calc R U P A 1
C13 C 0.0601(12) 0.547(3) 0.3053(12) 0.1075(8) Uani 0.51 1 d D U P A 1
H13A H 0.0538 0.4765 0.3401 0.129 Uiso 0.51 1 calc R U P A 1
H13B H 0.0847 0.6409 0.3326 0.129 Uiso 0.51 1 calc R U P A 1
C14 C -0.0137(14) 0.586(4) 0.248(2) 0.1075(8) Uani 0.51 1 d D U P A 1
H14A H -0.0438 0.6342 0.2698 0.161 Uiso 0.51 1 calc R U P A 1
H14B H -0.0393 0.4932 0.2220 0.161 Uiso 0.51 1 calc R U P A 1
H14C H -0.0081 0.6567 0.2136 0.161 Uiso 0.51 1 calc R U P A 1
C10A C 0.0865(11) 0.481(3) 0.2614(11) 0.1075(8) Uiso 0.49 1 d D U P A 3
C11A C -0.0009(10) 0.498(3) 0.2313(15) 0.1075(8) Uiso 0.49 1 d D U P A 3
H11D H -0.0141 0.6062 0.2291 0.161 Uiso 0.49 1 calc R U P A 3
H11E H -0.0175 0.4444 0.2638 0.161 Uiso 0.49 1 calc R U P A 3
H11F H -0.0261 0.4539 0.1820 0.161 Uiso 0.49 1 calc R U P A 3
C12A C 0.1043(19) 0.305(2) 0.2608(19) 0.136(19) Uiso 0.49 1 d D . P A 3
H12D H 0.1592 0.2902 0.2826 0.204 Uiso 0.49 1 calc R U P A 3
H12E H 0.0811 0.2682 0.2101 0.204 Uiso 0.49 1 calc R U P A 3
H12F H 0.0834 0.2493 0.2892 0.204 Uiso 0.49 1 calc R U P A 3
C13A C 0.1250(14) 0.534(4) 0.3448(9) 0.1075(8) Uiso 0.49 1 d D U P A 3
H13C H 0.1092 0.6392 0.3485 0.129 Uiso 0.49 1 calc R U P A 3
H13D H 0.1079 0.4665 0.3735 0.129 Uiso 0.49 1 calc R U P A 3
C14A C 0.2052(12) 0.527(3) 0.3743(13) 0.099(11) Uiso 0.49 1 d D . P A 3
H14D H 0.2280 0.5697 0.4240 0.149 Uiso 0.49 1 calc R U P A 3
H14E H 0.2217 0.5863 0.3432 0.149 Uiso 0.49 1 calc R U P A 3
H14F H 0.2212 0.4208 0.3760 0.149 Uiso 0.49 1 calc R U P A 3
C20A C 0.3241(13) 0.945(3) 0.2552(15) 0.2169(13) Uiso 0.38 1 d D U P A 1
C21A C 0.340(3) 1.090(4) 0.220(3) 0.26(4) Uiso 0.38 1 d D . P A 1
H21A H 0.3227 1.0719 0.1672 0.394 Uiso 0.38 1 calc R U P A 1
H21B H 0.3940 1.1122 0.2433 0.394 Uiso 0.38 1 calc R U P A 1
H21C H 0.3118 1.1765 0.2262 0.394 Uiso 0.38 1 calc R U P A 1
C22A C 0.3935(12) 0.834(5) 0.276(2) 0.18(2) Uiso 0.38 1 d D . P A 1
H22A H 0.3989 0.8076 0.2319 0.276 Uiso 0.38 1 calc R U P A 1
H22B H 0.3849 0.7408 0.2979 0.276 Uiso 0.38 1 calc R U P A 1
H22C H 0.4399 0.8838 0.3115 0.276 Uiso 0.38 1 calc R U P A 1
C23A C 0.322(2) 0.997(7) 0.3286(19) 0.2169(13) Uiso 0.38 1 d D U P A 1
H23A H 0.2977 1.0984 0.3213 0.260 Uiso 0.38 1 calc R U P A 1
H23B H 0.2905 0.9240 0.3405 0.260 Uiso 0.38 1 calc R U P A 1
C24A C 0.396(2) 1.004(7) 0.3882(18) 0.2170(13) Uiso 0.38 1 d D U P A 1
H24D H 0.3915 1.0127 0.4343 0.325 Uiso 0.38 1 calc R U P A 1
H24E H 0.4225 1.0923 0.3823 0.325 Uiso 0.38 1 calc R U P A 1
H24F H 0.4235 0.9106 0.3892 0.325 Uiso 0.38 1 calc R U P A 1
C20 C 0.3179(12) 0.973(2) 0.2433(11) 0.2169(13) Uiso 0.62 1 d D U P A 3
C21 C 0.2961(14) 1.1350(18) 0.2065(14) 0.108(11) Uiso 0.62 1 d D . P A 3
H21D H 0.2917 1.1302 0.1567 0.163 Uiso 0.62 1 calc R U P A 3
H21E H 0.3354 1.2087 0.2356 0.163 Uiso 0.62 1 calc R U P A 3
H21F H 0.2475 1.1669 0.2044 0.163 Uiso 0.62 1 calc R U P A 3
C22 C 0.3896(10) 0.914(3) 0.2370(14) 0.133(10) Uiso 0.62 1 d D . P A 3
H22D H 0.3792 0.9113 0.1853 0.199 Uiso 0.62 1 calc R U P A 3
H22E H 0.4020 0.8110 0.2576 0.199 Uiso 0.62 1 calc R U P A 3
H22F H 0.4324 0.9820 0.2641 0.199 Uiso 0.62 1 calc R U P A 3
C23 C 0.3382(17) 0.999(3) 0.3259(10) 0.2170(13) Uiso 0.62 1 d D U P A 3
H23C H 0.3840 1.0637 0.3479 0.260 Uiso 0.62 1 calc R U P A 3
H23D H 0.2962 1.0562 0.3286 0.260 Uiso 0.62 1 calc R U P A 3
C24 C 0.351(3) 0.868(4) 0.3680(17) 0.2170(13) Uiso 0.62 1 d D U P A 3
H24A H 0.3401 0.8877 0.4095 0.325 Uiso 0.62 1 calc R U P A 3
H24B H 0.4045 0.8374 0.3864 0.325 Uiso 0.62 1 calc R U P A 3
H24C H 0.3185 0.7856 0.3379 0.325 Uiso 0.62 1 calc R U P A 3
C30 C 0.1819(9) 0.4730(15) 0.0028(8) 0.125(5) Uani 1 1 d D U . . .
C31 C 0.1488(12) 0.546(2) -0.0756(7) 0.195(8) Uani 1 1 d D U . . .
H31A H 0.0941 0.5610 -0.0942 0.293 Uiso 1 1 calc R U . . .
H31B H 0.1585 0.4784 -0.1088 0.293 Uiso 1 1 calc R U . . .
H31C H 0.1732 0.6448 -0.0729 0.293 Uiso 1 1 calc R U . . .
C32 C 0.1463(11) 0.3136(13) 0.0003(10) 0.154(7) Uani 1 1 d D U . . .
H32A H 0.0937 0.3259 -0.0081 0.231 Uiso 1 1 calc R U . . .
H32B H 0.1752 0.2610 0.0470 0.231 Uiso 1 1 calc R U . . .
H32C H 0.1477 0.2535 -0.0397 0.231 Uiso 1 1 calc R U . . .
C33 C 0.2686(9) 0.4450(19) 0.0275(12) 0.192(8) Uani 1 1 d D U . . .
H33A H 0.2878 0.3746 0.0699 0.230 Uiso 1 1 calc R U . . .
H33B H 0.2742 0.3931 -0.0130 0.230 Uiso 1 1 calc R U . . .
C34 C 0.3158(12) 0.578(3) 0.0476(16) 0.200(11) Uani 1 1 d D U . . .
H34A H 0.3645 0.5533 0.0480 0.301 Uiso 1 1 calc R U . . .
H34B H 0.3243 0.6117 0.0965 0.301 Uiso 1 1 calc R U . . .
H34C H 0.2908 0.6590 0.0119 0.301 Uiso 1 1 calc R U . . .
C40 C -0.0287(10) 0.976(2) 0.0379(10) 0.126(6) Uani 0.62 1 d D U P A 1
C41 C -0.0046(12) 1.1399(16) 0.0252(14) 0.115(8) Uani 0.62 1 d D U P A 1
H41A H 0.0207 1.1332 -0.0065 0.172 Uiso 0.62 1 calc R U P A 1
H41B H 0.0301 1.1844 0.0725 0.172 Uiso 0.62 1 calc R U P A 1
H41C H -0.0498 1.2043 0.0018 0.172 Uiso 0.62 1 calc R U P A 1
C42 C -0.0722(13) 0.984(3) 0.0856(13) 0.187(10) Uani 0.62 1 d D U P A 1
H42A H -0.0891 0.8816 0.0908 0.280 Uiso 0.62 1 calc R U P A 1
H42B H -0.1163 1.0509 0.0618 0.280 Uiso 0.62 1 calc R U P A 1
H42C H -0.0386 1.0246 0.1342 0.280 Uiso 0.62 1 calc R U P A 1
C43 C -0.0841(11) 0.910(3) -0.0393(10) 0.1760(15) Uani 0.62 1 d D U P A 1
H43A H -0.1022 0.8076 -0.0337 0.211 Uiso 0.62 1 calc R U P A 1
H43B H -0.1286 0.9775 -0.0635 0.211 Uiso 0.62 1 calc R U P A 1
C44 C -0.044(2) 0.899(4) -0.0835(15) 0.1760(15) Uani 0.62 1 d D U P A 1
H44A H -0.0775 0.8592 -0.1321 0.264 Uiso 0.62 1 calc R U P A 1
H44B H 0.0000 0.8310 -0.0596 0.264 Uiso 0.62 1 calc R U P A 1
H44C H -0.0258 1.0008 -0.0887 0.264 Uiso 0.62 1 calc R U P A 1
C40A C -0.0237(10) 0.963(2) 0.0210(10) 0.023(6) Uiso 0.38 1 d D . P A 3
C41A C -0.024(2) 1.131(2) 0.048(2) 0.11(2) Uiso 0.38 1 d D . P A 3
H41D H -0.0249 1.1289 0.0961 0.159 Uiso 0.38 1 calc R U P A 3
H41E H -0.0687 1.1852 0.0128 0.159 Uiso 0.38 1 calc R U P A 3
H41F H 0.0220 1.1843 0.0534 0.159 Uiso 0.38 1 calc R U P A 3
C42A C -0.0199(19) 0.978(4) -0.0544(11) 0.105(13) Uiso 0.38 1 d D . P A 3
H42D H 0.0275 1.0279 -0.0466 0.158 Uiso 0.38 1 calc R U P A 3
H42E H -0.0630 1.0382 -0.0885 0.158 Uiso 0.38 1 calc R U P A 3
H42F H -0.0219 0.8759 -0.0751 0.158 Uiso 0.38 1 calc R U P A 3
C43A C -0.0993(10) 0.884(4) 0.009(2) 0.1760(15) Uiso 0.38 1 d D U P A 3
H43C H -0.1111 0.8031 -0.0281 0.211 Uiso 0.38 1 calc R U P A 3
H43D H -0.0911 0.8335 0.0558 0.211 Uiso 0.38 1 calc R U P A 3
C44A C -0.1625(14) 0.978(5) -0.012(3) 0.1760(15) Uiso 0.38 1 d D U P A 3
H44D H -0.2057 0.9190 -0.0149 0.264 Uiso 0.38 1 calc R U P A 3
H44E H -0.1748 1.0214 -0.0608 0.264 Uiso 0.38 1 calc R U P A 3
H44F H -0.1514 1.0611 0.0233 0.264 Uiso 0.38 1 calc R U P A 3


_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 O3 2.751(9) . ?
Rb1 O4 2.758(11) . ?
Rb1 O2 2.802(10) . ?
Rb1 C40A 3.626(18) . ?
Rb1 C21 3.65(2) . ?
Rb1 C20 3.67(2) . ?
Rb1 Rb3 3.937(3) . ?
Rb1 Rb4 3.949(4) . ?
Rb1 Rb2 3.955(4) . ?
Rb2 O3 2.762(11) . ?
Rb2 O1 2.763(10) . ?
Rb2 O4 2.776(10) . ?
Rb2 C24A 3.47(3) 3_444 ?
Rb2 C10A 3.631(19) . ?
Rb2 C43A 3.67(3) . ?
Rb2 C40A 3.67(2) . ?
Rb2 C32 3.707(16) . ?
Rb2 C30 3.711(15) . ?
Rb2 Rb4 3.898(3) . ?
Rb2 Rb3 3.945(4) . ?
Rb3 O4 2.735(11) . ?
Rb3 O1 2.772(9) . ?
Rb3 O2 2.785(10) . ?
Rb3 C40 3.613(18) . ?
Rb3 C10A 3.70(2) . ?
Rb3 C23A 3.71(3) . ?
Rb3 Rb4 3.967(4) . ?
Rb4 O2 2.737(10) . ?
Rb4 O1 2.780(10) . ?
Rb4 O3 2.788(10) . ?
Rb4 C22A 3.43(4) . ?
Rb4 C20A 3.60(3) . ?
Rb4 C10 3.644(18) . ?
O1 C10 1.406(16) . ?
O1 C10A 1.415(16) . ?
O2 C20A 1.399(18) . ?
O2 C20 1.410(17) . ?
O3 C30 1.406(11) . ?
O4 C40A 1.37(2) . ?
O4 C40 1.434(16) . ?
C10 C11 1.536(15) . ?
C10 C13 1.560(15) . ?
C10 C12 1.574(16) . ?
C13 C14 1.427(19) . ?
C10A C11A 1.540(15) . ?
C10A C12A 1.569(16) . ?
C10A C13A 1.571(15) . ?
C13A C14A 1.405(19) . ?
C20A C21A 1.542(17) . ?
C20A C22A 1.561(17) . ?
C20A C23A 1.567(17) . ?
C23A C24A 1.41(2) . ?
C20 C23 1.546(15) . ?
C20 C22 1.549(16) . ?
C20 C21 1.556(16) . ?
C23 C24 1.38(2) . ?
C30 C32 1.539(12) . ?
C30 C31 1.553(14) . ?
C30 C33 1.556(14) . ?
C33 C34 1.416(16) . ?
C40 C42 1.542(15) . ?
C40 C43 1.556(15) . ?
C40 C41 1.558(15) . ?
C43 C44 1.43(2) . ?
C40A C43A 1.548(16) . ?
C40A C42A 1.561(16) . ?
C40A C41A 1.565(16) . ?
C43A C44A 1.38(2) . ?

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
O3 Rb1 O4 88.9(3) . . ?
O3 Rb1 O2 88.7(3) . . ?
O4 Rb1 O2 88.9(3) . . ?
O3 Rb1 C40A 100.3(4) . . ?
O4 Rb1 C40A 19.4(4) . . ?
O2 Rb1 C40A 104.7(4) . . ?
O3 Rb1 C21 127.4(4) . . ?
O4 Rb1 C21 102.9(5) . . ?
O2 Rb1 C21 41.6(3) . . ?
C40A Rb1 C21 107.2(5) . . ?
O3 Rb1 C20 103.0(4) . . ?
O4 Rb1 C20 103.0(4) . . ?
O2 Rb1 C20 20.0(3) . . ?
C40A Rb1 C20 115.0(5) . . ?
C21 Rb1 C20 24.5(3) . . ?
O3 Rb1 Rb3 90.2(2) . . ?
O4 Rb1 Rb3 44.0(2) . . ?
O2 Rb1 Rb3 45.0(2) . . ?
C40A Rb1 Rb3 60.2(3) . . ?
C21 Rb1 Rb3 67.6(4) . . ?
C20 Rb1 Rb3 59.9(3) . . ?
O3 Rb1 Rb4 44.9(2) . . ?
O4 Rb1 Rb4 88.7(2) . . ?
O2 Rb1 Rb4 43.9(2) . . ?
C40A Rb1 Rb4 107.8(3) . . ?
C21 Rb1 Rb4 83.8(3) . . ?
C20 Rb1 Rb4 59.4(3) . . ?
Rb3 Rb1 Rb4 60.40(8) . . ?
O3 Rb1 Rb2 44.3(2) . . ?
O4 Rb1 Rb2 44.6(2) . . ?
O2 Rb1 Rb2 88.4(2) . . ?
C40A Rb1 Rb2 57.7(3) . . ?
C21 Rb1 Rb2 125.6(4) . . ?
C20 Rb1 Rb2 108.3(3) . . ?
Rb3 Rb1 Rb2 59.99(8) . . ?
Rb4 Rb1 Rb2 59.10(7) . . ?
O3 Rb2 O1 91.1(3) . . ?
O3 Rb2 O4 88.2(3) . . ?
O1 Rb2 O4 88.5(3) . . ?
O3 Rb2 C24A 103.4(9) . 3_444 ?
O1 Rb2 C24A 163.8(10) . 3_444 ?
O4 Rb2 C24A 99.0(10) . 3_444 ?
O3 Rb2 C10A 107.8(4) . . ?
O1 Rb2 C10A 20.3(3) . . ?
O4 Rb2 C10A 100.3(4) . . ?
O3 Rb2 C43A 121.7(5) . . ?
O1 Rb2 C43A 108.9(7) . . ?
O4 Rb2 C43A 40.9(4) . . ?
C10A Rb2 C43A 107.7(8) . . ?
O3 Rb2 C40A 98.9(3) . . ?
O1 Rb2 C40A 103.6(4) . . ?
O4 Rb2 C40A 18.8(3) . . ?
C10A Rb2 C40A 111.2(5) . . ?
C43A Rb2 C40A 24.3(3) . . ?
O3 Rb2 C32 40.5(3) . . ?
O1 Rb2 C32 106.2(4) . . ?
O4 Rb2 C32 125.2(3) . . ?
C24A Rb2 C32 81.3(9) 3_444 . ?
C10A Rb2 C32 111.3(4) . . ?
C43A Rb2 C32 140.8(8) . . ?
C40A Rb2 C32 128.6(4) . . ?
O3 Rb2 C30 18.7(2) . . ?
O1 Rb2 C30 104.3(3) . . ?
O4 Rb2 C30 101.6(3) . . ?
C24A Rb2 C30 88.4(9) 3_444 . ?
C10A Rb2 C30 117.3(4) . . ?
C43A Rb2 C30 126.6(6) . . ?
C40A Rb2 C30 107.9(4) . . ?
C32 Rb2 C30 24.0(2) . . ?
O3 Rb2 Rb4 45.6(2) . . ?
O1 Rb2 Rb4 45.5(2) . . ?
O4 Rb2 Rb4 89.5(2) . . ?
C24A Rb2 Rb4 147.9(9) 3_444 . ?
C10A Rb2 Rb4 62.7(3) . . ?
C43A Rb2 Rb4 129.1(5) . . ?
C40A Rb2 Rb4 108.0(3) . . ?
C32 Rb2 Rb4 68.8(3) . . ?
C30 Rb2 Rb4 59.6(2) . . ?
O3 Rb2 Rb3 89.8(2) . . ?
O1 Rb2 Rb3 44.6(2) . . ?
O4 Rb2 Rb3 43.9(2) . . ?
C24A Rb2 Rb3 140.7(9) 3_444 . ?
C10A Rb2 Rb3 58.3(4) . . ?
C43A Rb2 Rb3 72.0(6) . . ?
C40A Rb2 Rb3 59.8(3) . . ?
C32 Rb2 Rb3 127.0(3) . . ?
C30 Rb2 Rb3 108.5(2) . . ?
Rb4 Rb2 Rb3 60.76(8) . . ?
O3 Rb2 Rb1 44.04(19) . . ?
O1 Rb2 Rb1 89.7(2) . . ?
O4 Rb2 Rb1 44.2(2) . . ?
C24A Rb2 Rb1 105.7(10) 3_444 . ?
C10A Rb2 Rb1 109.7(3) . . ?
C43A Rb2 Rb1 80.8(3) . . ?
C40A Rb2 Rb1 56.6(3) . . ?
C32 Rb2 Rb1 82.5(2) . . ?
C30 Rb2 Rb1 58.6(2) . . ?
Rb4 Rb2 Rb1 60.38(8) . . ?
Rb3 Rb2 Rb1 59.78(6) . . ?
O4 Rb3 O1 89.1(3) . . ?
O4 Rb3 O2 89.8(3) . . ?
O1 Rb3 O2 88.1(3) . . ?
O4 Rb3 C40 20.8(3) . . ?
O1 Rb3 C40 102.6(4) . . ?
O2 Rb3 C40 105.8(4) . . ?
O4 Rb3 C10A 99.5(4) . . ?
O1 Rb3 C10A 19.2(3) . . ?
O2 Rb3 C10A 104.2(4) . . ?
O4 Rb3 C23A 125.5(7) . . ?
O1 Rb3 C23A 105.4(10) . . ?
O2 Rb3 C23A 40.5(5) . . ?
C40 Rb3 C23A 133.7(10) . . ?
O4 Rb3 Rb1 44.5(2) . . ?
O1 Rb3 Rb1 89.9(2) . . ?
O2 Rb3 Rb1 45.4(2) . . ?
C40 Rb3 Rb1 61.2(3) . . ?
C10A Rb3 Rb1 108.7(3) . . ?
C23A Rb3 Rb1 82.6(6) . . ?
O4 Rb3 Rb2 44.7(2) . . ?
O1 Rb3 Rb2 44.4(2) . . ?
O2 Rb3 Rb2 88.8(2) . . ?
C40 Rb3 Rb2 59.8(3) . . ?
C10A Rb3 Rb2 56.6(3) . . ?
C23A Rb3 Rb2 126.7(6) . . ?
Rb1 Rb3 Rb2 60.23(8) . . ?
O4 Rb3 Rb4 88.6(2) . . ?
O1 Rb3 Rb4 44.5(2) . . ?
O2 Rb3 Rb4 43.6(2) . . ?
C40 Rb3 Rb4 109.3(3) . . ?
C10A Rb3 Rb4 61.4(3) . . ?
C23A Rb3 Rb4 69.9(7) . . ?
Rb1 Rb3 Rb4 59.96(8) . . ?
Rb2 Rb3 Rb4 59.03(6) . . ?
O2 Rb4 O1 88.9(3) . . ?
O2 Rb4 O3 89.3(3) . . ?
O1 Rb4 O3 90.2(3) . . ?
O2 Rb4 C22A 45.1(5) . . ?
O1 Rb4 C22A 124.6(7) . . ?
O3 Rb4 C22A 113.2(9) . . ?
O2 Rb4 C20A 20.2(4) . . ?
O1 Rb4 C20A 102.9(5) . . ?
O3 Rb4 C20A 103.6(5) . . ?
C22A Rb4 C20A 25.5(3) . . ?
O2 Rb4 C10 101.8(4) . . ?
O1 Rb4 C10 20.1(3) . . ?
O3 Rb4 C10 105.5(4) . . ?
C22A Rb4 C10 126.0(8) . . ?
C20A Rb4 C10 110.8(6) . . ?
O2 Rb4 Rb2 90.5(2) . . ?
O1 Rb4 Rb2 45.1(2) . . ?
O3 Rb4 Rb2 45.1(2) . . ?
C22A Rb4 Rb2 134.7(6) . . ?
C20A Rb4 Rb2 110.7(4) . . ?
C10 Rb4 Rb2 61.2(3) . . ?
O2 Rb4 Rb1 45.2(2) . . ?
O1 Rb4 Rb1 89.6(2) . . ?
O3 Rb4 Rb1 44.1(2) . . ?
C22A Rb4 Rb1 77.6(7) . . ?
C20A Rb4 Rb1 60.8(5) . . ?
C10 Rb4 Rb1 109.6(3) . . ?
Rb2 Rb4 Rb1 60.53(8) . . ?
O2 Rb4 Rb3 44.6(2) . . ?
O1 Rb4 Rb3 44.33(19) . . ?
O3 Rb4 Rb3 89.0(2) . . ?
C22A Rb4 Rb3 84.8(5) . . ?
C20A Rb4 Rb3 60.2(4) . . ?
C10 Rb4 Rb3 59.1(3) . . ?
Rb2 Rb4 Rb3 60.21(8) . . ?
Rb1 Rb4 Rb3 59.64(6) . . ?
C10 O1 Rb2 131.6(9) . . ?
C10A O1 Rb2 117.0(9) . . ?
C10 O1 Rb3 125.3(9) . . ?
C10A O1 Rb3 120.6(10) . . ?
Rb2 O1 Rb3 90.9(3) . . ?
C10 O1 Rb4 117.2(9) . . ?
C10A O1 Rb4 136.0(10) . . ?
Rb2 O1 Rb4 89.4(3) . . ?
Rb3 O1 Rb4 91.2(3) . . ?
C20A O2 Rb4 117.3(13) . . ?
C20 O2 Rb4 128.8(10) . . ?
C20A O2 Rb3 127.9(13) . . ?
C20 O2 Rb3 127.2(10) . . ?
Rb4 O2 Rb3 91.9(3) . . ?
C20A O2 Rb1 128.5(14) . . ?
C20 O2 Rb1 117.3(10) . . ?
Rb4 O2 Rb1 91.0(3) . . ?
Rb3 O2 Rb1 89.6(3) . . ?
C30 O3 Rb1 126.2(7) . . ?
C30 O3 Rb2 122.4(8) . . ?
Rb1 O3 Rb2 91.7(3) . . ?
C30 O3 Rb4 125.7(8) . . ?
Rb1 O3 Rb4 91.0(3) . . ?
Rb2 O3 Rb4 89.2(3) . . ?
C40A O4 Rb3 132.7(10) . . ?
C40 O4 Rb3 116.6(9) . . ?
C40A O4 Rb1 118.9(9) . . ?
C40 O4 Rb1 131.0(9) . . ?
Rb3 O4 Rb1 91.6(3) . . ?
C40A O4 Rb2 120.7(9) . . ?
C40 O4 Rb2 124.6(9) . . ?
Rb3 O4 Rb2 91.4(3) . . ?
Rb1 O4 Rb2 91.2(3) . . ?
O1 C10 C11 112.5(13) . . ?
O1 C10 C13 109.5(13) . . ?
C11 C10 C13 107.8(13) . . ?
O1 C10 C12 108.7(13) . . ?
C11 C10 C12 111.1(13) . . ?
C13 C10 C12 107.0(12) . . ?
O1 C10 Rb4 42.7(7) . . ?
C11 C10 Rb4 74.7(10) . . ?
C13 C10 Rb4 142.8(12) . . ?
C12 C10 Rb4 106.3(11) . . ?
C14 C13 C10 113.5(17) . . ?
O1 C10A C11A 114.1(14) . . ?
O1 C10A C12A 109.9(14) . . ?
C11A C10A C12A 107.3(13) . . ?
O1 C10A C13A 110.3(13) . . ?
C11A C10A C13A 108.2(13) . . ?
C12A C10A C13A 106.8(13) . . ?
O1 C10A Rb2 42.7(7) . . ?
C11A C10A Rb2 80.6(10) . . ?
C12A C10A Rb2 97.5(12) . . ?
C13A C10A Rb2 149.8(13) . . ?
O1 C10A Rb3 40.2(8) . . ?
C11A C10A Rb3 95.0(11) . . ?
C12A C10A Rb3 149.4(13) . . ?
C13A C10A Rb3 85.1(12) . . ?
Rb2 C10A Rb3 65.1(3) . . ?
C14A C13A C10A 110.6(15) . . ?
O2 C20A C21A 113.2(15) . . ?
O2 C20A C22A 111.7(15) . . ?
C21A C20A C22A 107.7(14) . . ?
O2 C20A C23A 108.6(15) . . ?
C21A C20A C23A 107.4(14) . . ?
C22A C20A C23A 108.0(14) . . ?
O2 C20A Rb4 42.5(10) . . ?
C21A C20A Rb4 140.1(19) . . ?
C22A C20A Rb4 71.2(13) . . ?
C23A C20A Rb4 110.6(18) . . ?
C20A C22A Rb4 83.3(12) . . ?
C24A C23A C20A 111.7(19) . . ?
C24A C23A Rb3 159(4) . . ?
C20A C23A Rb3 81.3(11) . . ?
O2 C20 C23 110.8(14) . . ?
O2 C20 C22 112.5(14) . . ?
C23 C20 C22 109.3(14) . . ?
O2 C20 C21 109.5(13) . . ?
C23 C20 C21 105.5(13) . . ?
C22 C20 C21 109.1(13) . . ?
O2 C20 Rb1 42.7(7) . . ?
C23 C20 Rb1 148.4(13) . . ?
C22 C20 Rb1 99.1(11) . . ?
C21 C20 Rb1 77.1(9) . . ?
C20 C21 Rb1 78.4(9) . . ?
C24 C23 C20 115.7(18) . . ?
O3 C30 C32 109.5(9) . . ?
O3 C30 C31 111.6(11) . . ?
C32 C30 C31 111.0(11) . . ?
O3 C30 C33 111.6(10) . . ?
C32 C30 C33 106.2(11) . . ?
C31 C30 C33 106.8(10) . . ?
O3 C30 Rb2 38.9(6) . . ?
C32 C30 Rb2 77.9(7) . . ?
C31 C30 Rb2 104.0(9) . . ?
C33 C30 Rb2 144.6(9) . . ?
C30 C32 Rb2 78.1(7) . . ?
C34 C33 C30 116.1(14) . . ?
O4 C40 C42 112.7(13) . . ?
O4 C40 C43 109.0(12) . . ?
C42 C40 C43 108.2(13) . . ?
O4 C40 C41 109.0(12) . . ?
C42 C40 C41 110.5(13) . . ?
C43 C40 C41 107.3(12) . . ?
O4 C40 Rb3 42.6(7) . . ?
C42 C40 Rb3 77.1(10) . . ?
C43 C40 Rb3 145.4(12) . . ?
C41 C40 Rb3 102.2(10) . . ?
C44 C43 C40 108.4(15) . . ?
O4 C40A C43A 110.5(13) . . ?
O4 C40A C42A 109.8(13) . . ?
C43A C40A C42A 110.1(14) . . ?
O4 C40A C41A 111.9(14) . . ?
C43A C40A C41A 108.4(13) . . ?
C42A C40A C41A 106.0(13) . . ?
O4 C40A Rb1 41.8(7) . . ?
C43A C40A Rb1 142.9(12) . . ?
C42A C40A Rb1 72.4(12) . . ?
C41A C40A Rb1 106.0(15) . . ?
O4 C40A Rb2 40.6(7) . . ?
C43A C40A Rb2 77.8(11) . . ?
C42A C40A Rb2 100.6(13) . . ?
C41A C40A Rb2 148.1(14) . . ?
Rb1 C40A Rb2 65.6(3) . . ?
C44A C43A C40A 116(2) . . ?
C44A C43A Rb2 165.9(18) . . ?
C40A C43A Rb2 77.9(10) . . ?

_refine_diff_density_max         0.394
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.058

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: n-hexane'
_chemical_properties_physical    Moisture-sensitive
