# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_yulr_1104_3
_database_code_depnum_ccdc_archive 'CCDC 1544757'
_audit_update_record             
;
2017-07-06 deposited with the CCDC.
2017-08-09 downloaded from the CCDC.
;
_audit_creation_date             2017-06-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H64 K2 O14, 2(C4 H8 O), C54 H54 B2'
_chemical_formula_sum            'C94 H134 B2 K2 O16'
_chemical_formula_weight         1619.82
_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'
B B 0.0013 0.0007 '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'
O O 0.0106 0.0060 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.0148(10)
_cell_length_b                   12.4531(11)
_cell_length_c                   15.4631(15)
_cell_angle_alpha                95.007(8)
_cell_angle_beta                 105.069(8)
_cell_angle_gamma                93.255(7)
_cell_volume                     2217.9(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1202
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.2310
_cell_measurement_theta_min      3.5190
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             874
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0998
_diffrn_reflns_av_unetI/netI     0.2432
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12982
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.344
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -40.00   14.00   1.2000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3492  -77.0000  -90.0000 45

#__ type_ start__ end____ width___ exp.time_
  2 omega  -16.00   10.40   1.2000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3492  -99.0000 -180.0000 22

#__ type_ start__ end____ width___ exp.time_
  3 omega  -47.00   46.60   1.2000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305  -57.0000    0.0000 78

#__ type_ start__ end____ width___ exp.time_
  4 omega   -1.00   92.60   1.2000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305   57.0000  150.0000 78

#__ type_ start__ end____ width___ exp.time_
  5 omega   35.00   65.00   1.2000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305  178.0000   30.0000 25

#__ type_ start__ end____ width___ exp.time_
  6 omega    5.00   92.60   1.2000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305   57.0000 -120.0000 73
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0419141000
_diffrn_orient_matrix_UB_12      -0.0444272000
_diffrn_orient_matrix_UB_13      -0.0061142000
_diffrn_orient_matrix_UB_21      -0.0056552000
_diffrn_orient_matrix_UB_22      -0.0048439000
_diffrn_orient_matrix_UB_23      -0.0470210000
_diffrn_orient_matrix_UB_31      0.0444382000
_diffrn_orient_matrix_UB_32      -0.0359763000
_diffrn_orient_matrix_UB_33      0.0058176000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3003
_reflns_number_total             7780
_reflns_odcompleteness_completeness 99.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         7780
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2134
_refine_ls_R_factor_gt           0.0926
_refine_ls_restrained_S_all      0.995
_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)+(0.0331P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.2156
_refine_special_details          ?

# start Validation Reply Form
_vrf_PLAT026_yulr_1104_3         
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low .....    39 %    
RESPONSE: due to the disordered solvent of THF
;

_vrf_PLAT241_yulr_1104_3         
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of.....  C41 Check    
RESPONSE: due to the disordered solvent of THF
;

_vrf_PLAT910_yulr_1104_3         
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).....       18 Note  
RESPONSE: Theta min = 3.519 deg. The theta value of the missing reflections
are less than 3.519 deg. and therefore reflections were excluded
;
# end Validation Reply Form

_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 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), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),
  C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,
 H46B), C47(H47A,H47B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C12(H12), C14(H14), C21(H21), C23(H23)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.88329(11) 0.44881(11) 0.38088(9) 0.0336(4) Uani 1 1 d . . . . .
O1 O 0.7773(3) 0.6025(3) 0.4590(3) 0.0361(11) Uani 1 1 d . . . . .
O2 O 0.6782(3) 0.3868(3) 0.4182(3) 0.0343(11) Uani 1 1 d . . . . .
O3 O 0.7614(4) 0.2478(4) 0.3011(3) 0.0564(14) Uani 1 1 d . . . . .
O4 O 0.9545(4) 0.3208(4) 0.2607(3) 0.0512(13) Uani 1 1 d . . . . .
O5 O 1.0624(3) 0.5292(3) 0.3126(3) 0.0375(11) Uani 1 1 d . . . . .
O6 O 1.0128(3) 0.6543(3) 0.4636(3) 0.0355(11) Uani 1 1 d . . . . .
O7 O 0.7526(4) 0.5335(4) 0.2370(3) 0.0649(17) Uani 1 1 d . . . . .
C28 C 0.9102(6) 0.2133(5) 0.2296(5) 0.060(2) Uani 1 1 d . . . . .
H28A H 0.9733 0.1675 0.2315 0.072 Uiso 1 1 calc R . . . .
H28B H 0.8635 0.2093 0.1678 0.072 Uiso 1 1 calc R . . . .
C29 C 0.8375(5) 0.1748(5) 0.2889(5) 0.057(2) Uani 1 1 d . . . . .
H29A H 0.7952 0.1063 0.2615 0.068 Uiso 1 1 calc R . . . .
H29B H 0.8876 0.1632 0.3469 0.068 Uiso 1 1 calc R . . . .
C30 C 0.6860(6) 0.2096(5) 0.3525(5) 0.056(2) Uani 1 1 d . . . . .
H30A H 0.7310 0.1945 0.4114 0.067 Uiso 1 1 calc R . . . .
H30B H 0.6411 0.1436 0.3218 0.067 Uiso 1 1 calc R . . . .
C31 C 0.6080(5) 0.2959(5) 0.3622(4) 0.0461(19) Uani 1 1 d . . . . .
H31A H 0.5698 0.3171 0.3036 0.055 Uiso 1 1 calc R . . . .
H31B H 0.5493 0.2699 0.3899 0.055 Uiso 1 1 calc R . . . .
C32 C 0.6120(5) 0.4774(5) 0.4267(4) 0.0389(17) Uani 1 1 d . . . . .
H32A H 0.5447 0.4551 0.4463 0.047 Uiso 1 1 calc R . . . .
H32B H 0.5857 0.5054 0.3688 0.047 Uiso 1 1 calc R . . . .
C33 C 0.6863(5) 0.5630(5) 0.4939(4) 0.0401(17) Uani 1 1 d . . . . .
H33A H 0.6405 0.6216 0.5054 0.048 Uiso 1 1 calc R . . . .
H33B H 0.7181 0.5332 0.5502 0.048 Uiso 1 1 calc R . . . .
C34 C 0.8444(5) 0.6950(5) 0.5116(4) 0.0428(18) Uani 1 1 d . . . . .
H34A H 0.8843 0.6765 0.5708 0.051 Uiso 1 1 calc R . . . .
H34B H 0.7948 0.7519 0.5190 0.051 Uiso 1 1 calc R . . . .
C35 C 0.9295(5) 0.7321(5) 0.4638(5) 0.0445(18) Uani 1 1 d . . . . .
H35A H 0.8896 0.7423 0.4023 0.053 Uiso 1 1 calc R . . . .
H35B H 0.9687 0.8011 0.4934 0.053 Uiso 1 1 calc R . . . .
C36 C 1.0973(5) 0.6867(5) 0.4167(4) 0.0376(17) Uani 1 1 d . . . . .
H36A H 1.1710 0.6605 0.4454 0.045 Uiso 1 1 calc R . . . .
H36B H 1.1076 0.7650 0.4221 0.045 Uiso 1 1 calc R . . . .
C37 C 1.0634(5) 0.6450(5) 0.3199(4) 0.0378(16) Uani 1 1 d . . . . .
H37A H 0.9873 0.6662 0.2912 0.045 Uiso 1 1 calc R . . . .
H37B H 1.1180 0.6748 0.2901 0.045 Uiso 1 1 calc R . . . .
C38 C 1.0317(6) 0.4836(5) 0.2212(4) 0.0477(18) Uani 1 1 d . . . . .
H38A H 1.0853 0.5132 0.1904 0.057 Uiso 1 1 calc R . . . .
H38B H 0.9546 0.5013 0.1911 0.057 Uiso 1 1 calc R . . . .
C39 C 1.0353(6) 0.3627(5) 0.2178(5) 0.0515(19) Uani 1 1 d . . . . .
H39A H 1.0165 0.3310 0.1557 0.062 Uiso 1 1 calc R . . . .
H39B H 1.1123 0.3448 0.2480 0.062 Uiso 1 1 calc R . . . .
C40 C 0.7040(7) 0.4547(7) 0.1619(6) 0.091(3) Uani 1 1 d . . . . .
H40A H 0.7557 0.4489 0.1231 0.109 Uiso 1 1 calc R . . . .
H40B H 0.6928 0.3846 0.1825 0.109 Uiso 1 1 calc R . . . .
C41 C 0.6022(9) 0.4861(7) 0.1164(7) 0.157(6) Uani 1 1 d . . . . .
H41A H 0.5398 0.4481 0.1334 0.188 Uiso 1 1 calc R . . . .
H41B H 0.5915 0.4684 0.0522 0.188 Uiso 1 1 calc R . . . .
C42 C 0.5992(6) 0.6039(5) 0.1365(5) 0.053(2) Uani 1 1 d . . . . .
H42A H 0.5233 0.6222 0.1407 0.064 Uiso 1 1 calc R . . . .
H42B H 0.6212 0.6435 0.0914 0.064 Uiso 1 1 calc R . . . .
C43 C 0.6871(5) 0.6257(5) 0.2257(4) 0.0424(18) Uani 1 1 d . . . . .
H43A H 0.7372 0.6900 0.2270 0.051 Uiso 1 1 calc R . . . .
H43B H 0.6492 0.6366 0.2737 0.051 Uiso 1 1 calc R . . . .
O8 O 0.9457(7) 0.7611(8) -0.0144(6) 0.141(3) Uani 1 1 d . . . . .
C44 C 0.9196(13) 0.7343(9) 0.0687(9) 0.140(7) Uani 1 1 d . . . . .
H44A H 0.9874 0.7512 0.1193 0.168 Uiso 1 1 calc R . . . .
H44B H 0.8962 0.6577 0.0643 0.168 Uiso 1 1 calc R . . . .
C45 C 0.8248(10) 0.7989(14) 0.0817(9) 0.150(7) Uani 1 1 d . . . . .
H45A H 0.8279 0.8139 0.1450 0.180 Uiso 1 1 calc R . . . .
H45B H 0.7496 0.7636 0.0495 0.180 Uiso 1 1 calc R . . . .
C46 C 0.8518(10) 0.8991(9) 0.0420(8) 0.108(4) Uani 1 1 d . . . . .
H46A H 0.7821 0.9341 0.0174 0.130 Uiso 1 1 calc R . . . .
H46B H 0.9057 0.9498 0.0867 0.130 Uiso 1 1 calc R . . . .
C47 C 0.9032(10) 0.8597(10) -0.0283(9) 0.119(5) Uani 1 1 d . . . . .
H47A H 0.8454 0.8536 -0.0859 0.142 Uiso 1 1 calc R . . . .
H47B H 0.9654 0.9115 -0.0308 0.142 Uiso 1 1 calc R . . . .
C1 C 0.7591(4) 0.0513(4) 0.6729(4) 0.0289(15) Uani 1 1 d . . . . .
C2 C 0.8733(5) 0.0702(5) 0.7273(4) 0.0307(15) Uani 1 1 d . . . . .
H2 H 0.8874 0.0964 0.7876 0.037 Uiso 1 1 calc R . . . .
C3 C 0.9655(4) 0.0496(4) 0.6906(4) 0.0297(15) Uani 1 1 d . . . . .
H3 H 1.0407 0.0612 0.7274 0.036 Uiso 1 1 calc R . . . .
C4 C 0.9474(5) 0.0123(5) 0.6010(4) 0.0308(15) Uani 1 1 d . . . . .
H4 H 1.0092 -0.0036 0.5775 0.037 Uiso 1 1 calc R . . . .
C5 C 0.8342(4) -0.0010(4) 0.5465(4) 0.0293(14) Uani 1 1 d . . . . .
H5 H 0.8211 -0.0237 0.4855 0.035 Uiso 1 1 calc R . . . .
C6 C 0.7409(4) 0.0188(4) 0.5806(4) 0.0217(13) Uani 1 1 d . . . . .
C7 C 0.6169(4) 0.0073(4) 0.5346(4) 0.0263(14) Uani 1 1 d . . . . .
C8 C 0.5502(4) 0.0422(4) 0.5938(4) 0.0256(14) Uani 1 1 d . . . . .
C9 C 0.4303(4) 0.0312(4) 0.5564(4) 0.0276(14) Uani 1 1 d . . . . .
H9 H 0.3815 0.0495 0.5922 0.033 Uiso 1 1 calc R . . . .
C10 C 0.5821(4) -0.0093(4) 0.7580(4) 0.0250(14) Uani 1 1 d . . . . .
C11 C 0.6191(4) -0.1128(4) 0.7742(4) 0.0264(14) Uani 1 1 d . . . . .
C12 C 0.5783(5) -0.1730(5) 0.8354(4) 0.0323(16) Uani 1 1 d . . . . .
H12 H 0.6043 -0.2411 0.8447 0.039 Uiso 1 1 calc R . . . .
C13 C 0.5029(5) -0.1359(5) 0.8813(4) 0.0380(17) Uani 1 1 d . . . . .
C14 C 0.4575(5) -0.0393(5) 0.8589(4) 0.0348(16) Uani 1 1 d . . . . .
H14 H 0.4012 -0.0141 0.8851 0.042 Uiso 1 1 calc R . . . .
C15 C 0.4943(5) 0.0219(4) 0.7977(3) 0.0241(13) Uani 1 1 d . . . . .
C16 C 0.6991(5) -0.1677(5) 0.7252(4) 0.0385(16) Uani 1 1 d . . . . .
H16A H 0.6758 -0.1565 0.6626 0.058 Uiso 1 1 calc GR . . . .
H16B H 0.6946 -0.2439 0.7310 0.058 Uiso 1 1 calc GR . . . .
H16C H 0.7772 -0.1374 0.7512 0.058 Uiso 1 1 calc GR . . . .
C17 C 0.4663(6) -0.1968(5) 0.9512(4) 0.052(2) Uani 1 1 d . . . . .
H17A H 0.4897 -0.1538 1.0085 0.078 Uiso 1 1 calc GR . . . .
H17B H 0.5023 -0.2637 0.9557 0.078 Uiso 1 1 calc GR . . . .
H17C H 0.3838 -0.2116 0.9338 0.078 Uiso 1 1 calc GR . . . .
C18 C 0.4315(5) 0.1246(5) 0.7802(4) 0.0374(16) Uani 1 1 d . . . . .
H18A H 0.4665 0.1810 0.8276 0.056 Uiso 1 1 calc GR . . . .
H18B H 0.3516 0.1102 0.7785 0.056 Uiso 1 1 calc GR . . . .
H18C H 0.4371 0.1472 0.7236 0.056 Uiso 1 1 calc GR . . . .
C19 C 0.6566(4) 0.1993(4) 0.7457(4) 0.0248(13) Uani 1 1 d . . . . .
C20 C 0.6328(5) 0.2911(5) 0.6976(4) 0.0325(15) Uani 1 1 d . . . . .
C21 C 0.6542(5) 0.3958(5) 0.7420(5) 0.0363(16) Uani 1 1 d . . . . .
H21 H 0.6359 0.4534 0.7078 0.044 Uiso 1 1 calc R . . . .
C22 C 0.7005(5) 0.4184(5) 0.8332(5) 0.0402(17) Uani 1 1 d . . . . .
C23 C 0.7300(5) 0.3284(5) 0.8806(4) 0.0401(17) Uani 1 1 d . . . . .
H23 H 0.7649 0.3399 0.9422 0.048 Uiso 1 1 calc R . . . .
C24 C 0.7091(5) 0.2229(5) 0.8392(4) 0.0302(15) Uani 1 1 d . . . . .
C25 C 0.7473(5) 0.1356(5) 0.9014(4) 0.0402(17) Uani 1 1 d . . . . .
H25A H 0.6858 0.1145 0.9271 0.060 Uiso 1 1 calc GR . . . .
H25B H 0.8144 0.1634 0.9486 0.060 Uiso 1 1 calc GR . . . .
H25C H 0.7656 0.0739 0.8675 0.060 Uiso 1 1 calc GR . . . .
C26 C 0.5857(5) 0.2809(5) 0.5964(4) 0.0474(19) Uani 1 1 d . . . . .
H26A H 0.5070 0.2501 0.5800 0.071 Uiso 1 1 calc GR . . . .
H26B H 0.6315 0.2348 0.5693 0.071 Uiso 1 1 calc GR . . . .
H26C H 0.5886 0.3511 0.5756 0.071 Uiso 1 1 calc GR . . . .
C27 C 0.7213(8) 0.5305(5) 0.8832(6) 0.065(2) Uani 1 1 d . . . . .
H27A H 0.7252 0.5830 0.8419 0.08(3) Uiso 1 1 calc GR . . . .
H27B H 0.7929 0.5360 0.9295 0.19(6) Uiso 1 1 calc GR . . . .
H27C H 0.6591 0.5438 0.9100 0.10(3) Uiso 1 1 calc GR . . . .
B1 B 0.6329(5) 0.0732(5) 0.6962(4) 0.0213(15) Uani 1 1 d . . . . .


_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 K1 4.058(3) 2_766 ?
K1 O1 2.724(4) . ?
K1 O2 2.758(4) . ?
K1 O3 2.835(5) . ?
K1 O4 2.681(5) . ?
K1 O5 2.805(4) . ?
K1 O6 2.855(4) 2_766 ?
K1 O6 2.924(4) . ?
K1 O7 2.704(4) . ?
K1 C29 3.536(7) . ?
K1 C37 3.522(6) . ?
K1 C38 3.443(7) . ?
O1 C33 1.421(7) . ?
O1 C34 1.425(7) . ?
O2 C31 1.443(6) . ?
O2 C32 1.432(6) . ?
O3 C29 1.361(7) . ?
O3 C30 1.439(8) . ?
O4 C28 1.407(7) . ?
O4 C39 1.412(7) . ?
O5 C37 1.435(6) . ?
O5 C38 1.422(7) . ?
O6 K1 2.855(4) 2_766 ?
O6 C35 1.432(6) . ?
O6 C36 1.452(7) . ?
O7 C40 1.427(8) . ?
O7 C43 1.425(6) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.509(10) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.489(8) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.493(8) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C35 1.485(8) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 C37 1.483(8) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 C39 1.506(8) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 C41 1.341(9) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 C42 1.477(9) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C42 C43 1.496(7) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
O8 C44 1.462(14) . ?
O8 C47 1.369(11) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C44 C45 1.477(16) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C45 C46 1.493(14) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C46 C47 1.447(14) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C1 C2 1.405(7) . ?
C1 C6 1.406(7) . ?
C1 B1 1.678(8) . ?
C2 H2 0.9300 . ?
C2 C3 1.396(8) . ?
C3 H3 0.9300 . ?
C3 C4 1.380(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.393(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.383(8) . ?
C6 C7 1.467(7) . ?
C7 C8 1.422(8) . ?
C7 C9 1.403(7) 2_656 ?
C8 C9 1.400(6) . ?
C8 B1 1.635(8) . ?
C9 C7 1.403(7) 2_656 ?
C9 H9 0.9300 . ?
C10 C11 1.408(7) . ?
C10 C15 1.408(8) . ?
C10 B1 1.657(8) . ?
C11 C12 1.422(8) . ?
C11 C16 1.526(8) . ?
C12 H12 0.9300 . ?
C12 C13 1.365(8) . ?
C13 C14 1.383(8) . ?
C13 C17 1.513(8) . ?
C14 H14 0.9300 . ?
C14 C15 1.407(8) . ?
C15 C18 1.531(7) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C20 1.421(7) . ?
C19 C24 1.416(7) . ?
C19 B1 1.661(8) . ?
C20 C21 1.397(8) . ?
C20 C26 1.511(8) . ?
C21 H21 0.9300 . ?
C21 C22 1.372(8) . ?
C22 C23 1.404(8) . ?
C22 C27 1.510(8) . ?
C23 H23 0.9300 . ?
C23 C24 1.390(8) . ?
C24 C25 1.525(7) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?

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 K1 75.89(9) . 2_766 ?
O1 K1 O2 62.05(12) . . ?
O1 K1 O3 120.47(14) . . ?
O1 K1 O5 114.89(13) . . ?
O1 K1 O6 99.13(12) . 2_766 ?
O1 K1 O6 60.43(11) . . ?
O1 K1 C29 140.55(15) . . ?
O1 K1 C37 92.22(13) . . ?
O1 K1 C38 126.66(14) . . ?
O2 K1 K1 107.40(10) . 2_766 ?
O2 K1 O3 60.17(14) . . ?
O2 K1 O5 168.20(12) . . ?
O2 K1 O6 120.59(13) . . ?
O2 K1 O6 84.48(11) . 2_766 ?
O2 K1 C29 78.66(15) . . ?
O2 K1 C37 150.39(13) . . ?
O2 K1 C38 148.02(14) . . ?
O3 K1 K1 134.73(11) . 2_766 ?
O3 K1 O6 179.02(13) . . ?
O3 K1 O6 88.65(13) . 2_766 ?
O3 K1 C29 21.24(13) . . ?
O3 K1 C37 136.29(16) . . ?
O3 K1 C38 97.18(16) . . ?
O4 K1 K1 117.55(10) . 2_766 ?
O4 K1 O1 163.41(13) . . ?
O4 K1 O2 118.23(13) . . ?
O4 K1 O3 58.17(14) . . ?
O4 K1 O5 61.05(13) . . ?
O4 K1 O6 97.37(13) . 2_766 ?
O4 K1 O6 121.10(13) . . ?
O4 K1 O7 85.94(15) . . ?
O4 K1 C29 42.15(16) . . ?
O4 K1 C37 82.05(15) . . ?
O4 K1 C38 43.47(14) . . ?
O5 K1 K1 81.86(9) . 2_766 ?
O5 K1 O3 118.55(15) . . ?
O5 K1 O6 60.85(12) . . ?
O5 K1 O6 107.31(12) . 2_766 ?
O5 K1 C29 102.79(15) . . ?
O5 K1 C37 22.81(12) . . ?
O5 K1 C38 23.59(12) . . ?
O6 K1 K1 44.72(7) . 2_766 ?
O6 K1 K1 46.09(8) 2_766 2_766 ?
O6 K1 O6 90.82(11) 2_766 . ?
O6 K1 C29 79.51(14) 2_766 . ?
O6 K1 C29 157.79(13) . . ?
O6 K1 C37 43.39(13) . . ?
O6 K1 C37 115.84(13) 2_766 . ?
O6 K1 C38 119.56(14) 2_766 . ?
O6 K1 C38 82.37(14) . . ?
O7 K1 K1 138.96(12) . 2_766 ?
O7 K1 O1 77.49(14) . . ?
O7 K1 O2 86.49(14) . . ?
O7 K1 O3 85.91(14) . . ?
O7 K1 O5 81.72(15) . . ?
O7 K1 O6 94.73(13) . . ?
O7 K1 O6 170.90(15) . 2_766 ?
O7 K1 C29 97.64(15) . . ?
O7 K1 C37 72.94(15) . . ?
O7 K1 C38 68.46(16) . . ?
C29 K1 K1 122.61(11) . 2_766 ?
C37 K1 K1 77.48(10) . 2_766 ?
C37 K1 C29 124.20(17) . . ?
C38 K1 K1 104.56(12) . 2_766 ?
C38 K1 C29 85.11(17) . . ?
C38 K1 C37 39.66(15) . . ?
C33 O1 K1 115.6(3) . . ?
C33 O1 C34 113.8(5) . . ?
C34 O1 K1 119.5(3) . . ?
C31 O2 K1 117.4(4) . . ?
C32 O2 K1 111.4(3) . . ?
C32 O2 C31 111.9(4) . . ?
C29 O3 K1 109.8(4) . . ?
C29 O3 C30 112.4(5) . . ?
C30 O3 K1 111.6(4) . . ?
C28 O4 K1 124.9(4) . . ?
C28 O4 C39 114.7(6) . . ?
C39 O4 K1 120.2(4) . . ?
C37 O5 K1 107.9(3) . . ?
C38 O5 K1 104.3(3) . . ?
C38 O5 C37 111.7(4) . . ?
K1 O6 K1 89.19(11) 2_766 . ?
C35 O6 K1 122.6(4) . 2_766 ?
C35 O6 K1 106.8(3) . . ?
C35 O6 C36 112.3(4) . . ?
C36 O6 K1 111.7(3) . . ?
C36 O6 K1 111.4(3) . 2_766 ?
C40 O7 K1 113.2(4) . . ?
C43 O7 K1 134.4(4) . . ?
C43 O7 C40 108.1(5) . . ?
O4 C28 H28A 109.9 . . ?
O4 C28 H28B 109.9 . . ?
O4 C28 C29 108.9(6) . . ?
H28A C28 H28B 108.3 . . ?
C29 C28 H28A 109.9 . . ?
C29 C28 H28B 109.9 . . ?
K1 C29 H29A 158.3 . . ?
K1 C29 H29B 83.3 . . ?
O3 C29 K1 49.0(3) . . ?
O3 C29 C28 111.5(5) . . ?
O3 C29 H29A 109.3 . . ?
O3 C29 H29B 109.3 . . ?
C28 C29 K1 83.0(4) . . ?
C28 C29 H29A 109.3 . . ?
C28 C29 H29B 109.3 . . ?
H29A C29 H29B 108.0 . . ?
O3 C30 H30A 110.2 . . ?
O3 C30 H30B 110.2 . . ?
O3 C30 C31 107.6(5) . . ?
H30A C30 H30B 108.5 . . ?
C31 C30 H30A 110.2 . . ?
C31 C30 H30B 110.2 . . ?
O2 C31 C30 107.5(5) . . ?
O2 C31 H31A 110.2 . . ?
O2 C31 H31B 110.2 . . ?
C30 C31 H31A 110.2 . . ?
C30 C31 H31B 110.2 . . ?
H31A C31 H31B 108.5 . . ?
O2 C32 H32A 109.9 . . ?
O2 C32 H32B 109.9 . . ?
O2 C32 C33 108.9(4) . . ?
H32A C32 H32B 108.3 . . ?
C33 C32 H32A 109.9 . . ?
C33 C32 H32B 109.9 . . ?
O1 C33 C32 108.8(5) . . ?
O1 C33 H33A 109.9 . . ?
O1 C33 H33B 109.9 . . ?
C32 C33 H33A 109.9 . . ?
C32 C33 H33B 109.9 . . ?
H33A C33 H33B 108.3 . . ?
O1 C34 H34A 110.1 . . ?
O1 C34 H34B 110.1 . . ?
O1 C34 C35 107.9(5) . . ?
H34A C34 H34B 108.4 . . ?
C35 C34 H34A 110.1 . . ?
C35 C34 H34B 110.1 . . ?
O6 C35 C34 110.3(5) . . ?
O6 C35 H35A 109.6 . . ?
O6 C35 H35B 109.6 . . ?
C34 C35 H35A 109.6 . . ?
C34 C35 H35B 109.6 . . ?
H35A C35 H35B 108.1 . . ?
O6 C36 H36A 109.0 . . ?
O6 C36 H36B 109.0 . . ?
O6 C36 C37 112.9(5) . . ?
H36A C36 H36B 107.8 . . ?
C37 C36 H36A 109.0 . . ?
C37 C36 H36B 109.0 . . ?
K1 C37 H37A 78.5 . . ?
K1 C37 H37B 158.4 . . ?
O5 C37 K1 49.3(3) . . ?
O5 C37 C36 108.6(5) . . ?
O5 C37 H37A 110.0 . . ?
O5 C37 H37B 110.0 . . ?
C36 C37 K1 85.6(3) . . ?
C36 C37 H37A 110.0 . . ?
C36 C37 H37B 110.0 . . ?
H37A C37 H37B 108.3 . . ?
K1 C38 H38A 161.3 . . ?
K1 C38 H38B 77.5 . . ?
O5 C38 K1 52.2(3) . . ?
O5 C38 H38A 109.8 . . ?
O5 C38 H38B 109.8 . . ?
O5 C38 C39 109.3(5) . . ?
H38A C38 H38B 108.3 . . ?
C39 C38 K1 83.7(4) . . ?
C39 C38 H38A 109.8 . . ?
C39 C38 H38B 109.8 . . ?
O4 C39 C38 109.0(6) . . ?
O4 C39 H39A 109.9 . . ?
O4 C39 H39B 109.9 . . ?
C38 C39 H39A 109.9 . . ?
C38 C39 H39B 109.9 . . ?
H39A C39 H39B 108.3 . . ?
O7 C40 H40A 110.1 . . ?
O7 C40 H40B 110.1 . . ?
H40A C40 H40B 108.4 . . ?
C41 C40 O7 108.1(7) . . ?
C41 C40 H40A 110.1 . . ?
C41 C40 H40B 110.1 . . ?
C40 C41 H41A 109.7 . . ?
C40 C41 H41B 109.7 . . ?
C40 C41 C42 109.9(7) . . ?
H41A C41 H41B 108.2 . . ?
C42 C41 H41A 109.7 . . ?
C42 C41 H41B 109.7 . . ?
C41 C42 H42A 111.4 . . ?
C41 C42 H42B 111.4 . . ?
C41 C42 C43 101.6(5) . . ?
H42A C42 H42B 109.3 . . ?
C43 C42 H42A 111.4 . . ?
C43 C42 H42B 111.4 . . ?
O7 C43 C42 106.9(5) . . ?
O7 C43 H43A 110.3 . . ?
O7 C43 H43B 110.3 . . ?
C42 C43 H43A 110.3 . . ?
C42 C43 H43B 110.3 . . ?
H43A C43 H43B 108.6 . . ?
C47 O8 C44 104.6(10) . . ?
O8 C44 H44A 110.2 . . ?
O8 C44 H44B 110.2 . . ?
O8 C44 C45 107.6(10) . . ?
H44A C44 H44B 108.5 . . ?
C45 C44 H44A 110.2 . . ?
C45 C44 H44B 110.2 . . ?
C44 C45 H45A 111.7 . . ?
C44 C45 H45B 111.7 . . ?
C44 C45 C46 100.4(10) . . ?
H45A C45 H45B 109.5 . . ?
C46 C45 H45A 111.7 . . ?
C46 C45 H45B 111.7 . . ?
C45 C46 H46A 111.1 . . ?
C45 C46 H46B 111.1 . . ?
H46A C46 H46B 109.0 . . ?
C47 C46 C45 103.5(11) . . ?
C47 C46 H46A 111.1 . . ?
C47 C46 H46B 111.1 . . ?
O8 C47 C46 112.0(11) . . ?
O8 C47 H47A 109.2 . . ?
O8 C47 H47B 109.2 . . ?
C46 C47 H47A 109.2 . . ?
C46 C47 H47B 109.2 . . ?
H47A C47 H47B 107.9 . . ?
C2 C1 C6 118.6(5) . . ?
C2 C1 B1 130.8(6) . . ?
C6 C1 B1 110.3(4) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 C1 120.0(6) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 H3 119.3 . . ?
C4 C3 C2 121.4(5) . . ?
C4 C3 H3 119.3 . . ?
C3 C4 H4 120.9 . . ?
C3 C4 C5 118.3(6) . . ?
C5 C4 H4 120.9 . . ?
C4 C5 H5 119.1 . . ?
C6 C5 C4 121.8(6) . . ?
C6 C5 H5 119.1 . . ?
C1 C6 C7 110.6(5) . . ?
C5 C6 C1 119.9(5) . . ?
C5 C6 C7 129.5(5) . . ?
C8 C7 C6 111.2(5) . . ?
C9 C7 C6 124.7(6) 2_656 . ?
C9 C7 C8 124.1(5) 2_656 . ?
C7 C8 B1 110.5(4) . . ?
C9 C8 C7 115.3(5) . . ?
C9 C8 B1 133.7(5) . . ?
C7 C9 H9 119.7 2_656 . ?
C8 C9 C7 120.6(6) . 2_656 ?
C8 C9 H9 119.7 . . ?
C11 C10 C15 115.2(5) . . ?
C11 C10 B1 124.8(5) . . ?
C15 C10 B1 120.0(5) . . ?
C10 C11 C12 120.4(6) . . ?
C10 C11 C16 122.7(5) . . ?
C12 C11 C16 116.8(5) . . ?
C11 C12 H12 118.4 . . ?
C13 C12 C11 123.3(6) . . ?
C13 C12 H12 118.4 . . ?
C12 C13 C14 116.4(6) . . ?
C12 C13 C17 123.0(6) . . ?
C14 C13 C17 120.5(6) . . ?
C13 C14 H14 119.1 . . ?
C13 C14 C15 121.8(6) . . ?
C15 C14 H14 119.1 . . ?
C10 C15 C18 124.1(5) . . ?
C14 C15 C10 122.2(5) . . ?
C14 C15 C18 113.7(5) . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C17 H17A 109.5 . . ?
C13 C17 H17B 109.5 . . ?
C13 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 B1 123.2(5) . . ?
C24 C19 C20 115.0(5) . . ?
C24 C19 B1 121.7(5) . . ?
C19 C20 C26 121.9(5) . . ?
C21 C20 C19 121.2(6) . . ?
C21 C20 C26 116.8(5) . . ?
C20 C21 H21 118.2 . . ?
C22 C21 C20 123.6(6) . . ?
C22 C21 H21 118.2 . . ?
C21 C22 C23 115.5(6) . . ?
C21 C22 C27 124.7(7) . . ?
C23 C22 C27 119.8(7) . . ?
C22 C23 H23 118.7 . . ?
C24 C23 C22 122.7(6) . . ?
C24 C23 H23 118.7 . . ?
C19 C24 C25 122.9(5) . . ?
C23 C24 C19 121.8(5) . . ?
C23 C24 C25 115.3(5) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C20 C26 H26A 109.5 . . ?
C20 C26 H26B 109.5 . . ?
C20 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C8 B1 C1 97.0(4) . . ?
C8 B1 C10 104.9(4) . . ?
C8 B1 C19 122.2(4) . . ?
C10 B1 C1 119.2(4) . . ?
C10 B1 C19 111.2(5) . . ?
C19 B1 C1 102.6(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
K1 O1 C33 C32 -44.4(5) . . . . ?
K1 O1 C34 C35 41.9(6) . . . . ?
K1 O2 C31 C30 45.5(6) . . . . ?
K1 O2 C32 C33 -53.2(6) . . . . ?
K1 O3 C29 C28 -59.0(7) . . . . ?
K1 O3 C30 C31 55.7(6) . . . . ?
K1 O4 C28 C29 -12.4(7) . . . . ?
K1 O4 C39 C38 -22.3(7) . . . . ?
K1 O5 C37 C36 66.7(5) . . . . ?
K1 O5 C38 C39 -65.3(5) . . . . ?
K1 O6 C35 C34 56.5(5) . . . . ?
K1 O6 C35 C34 -43.6(6) 2_766 . . . ?
K1 O6 C36 C37 126.3(4) 2_766 . . . ?
K1 O6 C36 C37 28.3(5) . . . . ?
K1 O7 C40 C41 148.7(8) . . . . ?
K1 O7 C43 C42 -157.7(5) . . . . ?
K1 C38 C39 O4 14.9(5) . . . . ?
O1 C34 C35 O6 -67.7(6) . . . . ?
O2 C32 C33 O1 65.9(6) . . . . ?
O3 C30 C31 O2 -67.1(7) . . . . ?
O4 C28 C29 K1 7.8(4) . . . . ?
O4 C28 C29 O3 48.4(8) . . . . ?
O5 C38 C39 O4 61.1(7) . . . . ?
O6 C36 C37 K1 -21.5(4) . . . . ?
O6 C36 C37 O5 -65.7(6) . . . . ?
O7 C40 C41 C42 22.2(13) . . . . ?
C28 O4 C39 C38 152.7(5) . . . . ?
C29 O3 C30 C31 179.5(5) . . . . ?
C30 O3 C29 K1 -124.8(6) . . . . ?
C30 O3 C29 C28 176.2(6) . . . . ?
C31 O2 C32 C33 173.2(5) . . . . ?
C32 O2 C31 C30 176.1(5) . . . . ?
C33 O1 C34 C35 -175.7(4) . . . . ?
C34 O1 C33 C32 171.7(5) . . . . ?
C35 O6 C36 C37 -91.8(6) . . . . ?
C36 O6 C35 C34 179.4(5) . . . . ?
C37 O5 C38 K1 -116.3(5) . . . . ?
C37 O5 C38 C39 178.4(5) . . . . ?
C38 O5 C37 K1 114.0(5) . . . . ?
C38 O5 C37 C36 -179.3(5) . . . . ?
C39 O4 C28 C29 172.9(5) . . . . ?
C40 O7 C43 C42 -3.6(8) . . . . ?
C40 C41 C42 C43 -23.3(12) . . . . ?
C41 C42 C43 O7 15.5(9) . . . . ?
C43 O7 C40 C41 -11.4(11) . . . . ?
O8 C44 C45 C46 -33.0(12) . . . . ?
C44 O8 C47 C46 0.7(13) . . . . ?
C44 C45 C46 C47 31.9(12) . . . . ?
C45 C46 C47 O8 -21.4(13) . . . . ?
C47 O8 C44 C45 21.0(12) . . . . ?
C1 C2 C3 C4 1.1(9) . . . . ?
C1 C6 C7 C8 5.6(6) . . . . ?
C1 C6 C7 C9 -175.4(5) . . . 2_656 ?
C2 C1 C6 C5 4.3(8) . . . . ?
C2 C1 C6 C7 -177.7(5) . . . . ?
C2 C1 B1 C8 173.8(5) . . . . ?
C2 C1 B1 C10 -74.9(8) . . . . ?
C2 C1 B1 C19 48.5(7) . . . . ?
C2 C3 C4 C5 2.2(9) . . . . ?
C3 C4 C5 C6 -2.2(8) . . . . ?
C4 C5 C6 C1 -1.1(8) . . . . ?
C4 C5 C6 C7 -178.6(5) . . . . ?
C5 C6 C7 C8 -176.6(6) . . . . ?
C5 C6 C7 C9 2.3(9) . . . 2_656 ?
C6 C1 C2 C3 -4.3(8) . . . . ?
C6 C1 B1 C8 0.6(6) . . . . ?
C6 C1 B1 C10 112.0(5) . . . . ?
C6 C1 B1 C19 -124.7(5) . . . . ?
C6 C7 C8 C9 -178.1(4) . . . . ?
C6 C7 C8 B1 -5.2(6) . . . . ?
C7 C8 C9 C7 -2.8(8) . . . 2_656 ?
C7 C8 B1 C1 2.7(6) . . . . ?
C7 C8 B1 C10 -120.0(5) . . . . ?
C7 C8 B1 C19 112.5(6) . . . . ?
C9 C7 C8 C9 2.9(9) 2_656 . . . ?
C9 C7 C8 B1 175.8(5) 2_656 . . . ?
C9 C8 B1 C1 173.9(6) . . . . ?
C9 C8 B1 C10 51.2(8) . . . . ?
C9 C8 B1 C19 -76.4(8) . . . . ?
C10 C11 C12 C13 0.0(9) . . . . ?
C11 C10 C15 C14 8.3(8) . . . . ?
C11 C10 C15 C18 -172.6(5) . . . . ?
C11 C10 B1 C1 -17.3(8) . . . . ?
C11 C10 B1 C8 89.6(6) . . . . ?
C11 C10 B1 C19 -136.4(5) . . . . ?
C11 C12 C13 C14 6.2(9) . . . . ?
C11 C12 C13 C17 -175.5(5) . . . . ?
C12 C13 C14 C15 -5.1(8) . . . . ?
C13 C14 C15 C10 -2.3(9) . . . . ?
C13 C14 C15 C18 178.6(5) . . . . ?
C15 C10 C11 C12 -7.2(8) . . . . ?
C15 C10 C11 C16 170.1(5) . . . . ?
C15 C10 B1 C1 163.6(5) . . . . ?
C15 C10 B1 C8 -89.4(6) . . . . ?
C15 C10 B1 C19 44.6(7) . . . . ?
C16 C11 C12 C13 -177.4(5) . . . . ?
C17 C13 C14 C15 176.7(5) . . . . ?
C19 C20 C21 C22 1.1(10) . . . . ?
C20 C19 C24 C23 3.1(8) . . . . ?
C20 C19 C24 C25 -176.6(5) . . . . ?
C20 C19 B1 C1 90.3(6) . . . . ?
C20 C19 B1 C8 -16.4(8) . . . . ?
C20 C19 B1 C10 -141.2(5) . . . . ?
C20 C21 C22 C23 2.2(9) . . . . ?
C20 C21 C22 C27 -178.2(7) . . . . ?
C21 C22 C23 C24 -2.8(9) . . . . ?
C22 C23 C24 C19 0.2(10) . . . . ?
C22 C23 C24 C25 179.9(6) . . . . ?
C24 C19 C20 C21 -3.7(8) . . . . ?
C24 C19 C20 C26 175.1(5) . . . . ?
C24 C19 B1 C1 -85.7(6) . . . . ?
C24 C19 B1 C8 167.5(5) . . . . ?
C24 C19 B1 C10 42.8(7) . . . . ?
C26 C20 C21 C22 -177.7(6) . . . . ?
C27 C22 C23 C24 177.5(7) . . . . ?
B1 C1 C2 C3 -177.0(5) . . . . ?
B1 C1 C6 C5 178.4(5) . . . . ?
B1 C1 C6 C7 -3.6(6) . . . . ?
B1 C8 C9 C7 -173.6(5) . . . 2_656 ?
B1 C10 C11 C12 173.8(5) . . . . ?
B1 C10 C11 C16 -9.0(8) . . . . ?
B1 C10 C15 C14 -172.5(5) . . . . ?
B1 C10 C15 C18 6.5(8) . . . . ?
B1 C19 C20 C21 -179.9(5) . . . . ?
B1 C19 C20 C26 -1.2(8) . . . . ?
B1 C19 C24 C23 179.4(6) . . . . ?
B1 C19 C24 C25 -0.3(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_panxb_0518
_database_code_depnum_ccdc_archive 'CCDC 1544754'
_audit_update_record             
;
2017-07-06 deposited with the CCDC.
2017-08-09 downloaded from the CCDC.
;
_audit_creation_date             2017-06-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C54 H56 B2, 2(C H Cl3)'
_chemical_formula_sum            'C56 H58 B2 Cl6'
_chemical_formula_weight         965.34
_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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   15.3919(7)
_cell_length_b                   8.1281(4)
_cell_length_c                   20.3055(13)
_cell_angle_alpha                90
_cell_angle_beta                 92.736(5)
_cell_angle_gamma                90
_cell_volume                     2537.4(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2187
_cell_measurement_temperature    290.56(10)
_cell_measurement_theta_max      27.1150
_cell_measurement_theta_min      3.7450
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10772
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.731
_diffrn_reflns_theta_min         3.401
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      290.56(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -28.00   -2.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -38.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
  2 omega  -46.00   65.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -19.0000   60.0000 111

#__ type_ start__ end____ width___ exp.time_
  3 omega  -48.00   35.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -57.0000    0.0000 83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0242653000
_diffrn_orient_matrix_UB_12      0.0289219000
_diffrn_orient_matrix_UB_13      0.0264800000
_diffrn_orient_matrix_UB_21      0.0241440000
_diffrn_orient_matrix_UB_22      -0.0524288000
_diffrn_orient_matrix_UB_23      0.0219582000
_diffrn_orient_matrix_UB_31      0.0309875000
_diffrn_orient_matrix_UB_32      0.0635115000
_diffrn_orient_matrix_UB_33      0.0060810000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3832
_reflns_number_total             5767
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.901
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         5767
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0602
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0502P)²+1.5526P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1554
_refine_special_details          ?

# start Validation Reply Form
_vrf_PLAT910_panxb_0518          
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).....       12 Note  
RESPONSE: Theta min = 3.401 deg. The theta value of the missing reflections
are less than 3.401 deg. and therefore reflections were excluded
;
# end Validation Reply Form

_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C28(H28)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C12(H12), C14(H14), C21(H21),
 C23(H23)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
C1 C 0.82845(16) 0.2253(3) 0.07954(12) 0.0229(5) Uani 1 1 d . . . . .
C2 C 0.79910(18) 0.0902(3) 0.11601(13) 0.0284(6) Uani 1 1 d . . . . .
H2 H 0.7400 0.0814 0.1230 0.034 Uiso 1 1 calc R . . . .
C3 C 0.85494(19) -0.0297(3) 0.14173(14) 0.0331(7) Uani 1 1 d . . . . .
H3 H 0.8331 -0.1191 0.1643 0.040 Uiso 1 1 calc R . . . .
C4 C 0.94364(19) -0.0156(3) 0.13367(14) 0.0339(7) Uani 1 1 d . . . . .
H4 H 0.9817 -0.0947 0.1513 0.041 Uiso 1 1 calc R . . . .
C5 C 0.97512(18) 0.1172(3) 0.09923(14) 0.0305(6) Uani 1 1 d . . . . .
H5 H 1.0347 0.1265 0.0943 0.037 Uiso 1 1 calc R . . . .
C6 C 0.91959(16) 0.2374(3) 0.07173(13) 0.0241(6) Uani 1 1 d . . . . .
C7 C 0.96006(15) 0.3727(3) 0.03520(13) 0.0232(5) Uani 1 1 d . . . . .
C8 C 0.94163(16) 0.5381(3) 0.04736(13) 0.0258(6) Uani 1 1 d . . . . .
H8 H 0.9029 0.5650 0.0794 0.031 Uiso 1 1 calc R . . . .
C9 C 1.01981(16) 0.3379(3) -0.01244(13) 0.0254(6) Uani 1 1 d . . . . .
H9 H 1.0340 0.2290 -0.0209 0.031 Uiso 1 1 calc R . . . .
C10 C 0.66932(16) 0.3669(3) 0.08669(13) 0.0234(5) Uani 1 1 d . . . . .
C11 C 0.58608(16) 0.3352(3) 0.05574(13) 0.0253(6) Uani 1 1 d . . . . .
C12 C 0.51103(16) 0.3834(3) 0.08620(14) 0.0278(6) Uani 1 1 d . . . . .
H12 H 0.4572 0.3640 0.0648 0.033 Uiso 1 1 calc R . . . .
C13 C 0.51391(17) 0.4595(3) 0.14754(14) 0.0290(6) Uani 1 1 d . . . . .
C14 C 0.59533(17) 0.4812(3) 0.17931(14) 0.0280(6) Uani 1 1 d . . . . .
H14 H 0.5985 0.5273 0.2213 0.034 Uiso 1 1 calc R . . . .
C15 C 0.67198(16) 0.4365(3) 0.15058(13) 0.0254(6) Uani 1 1 d . . . . .
C16 C 0.57734(18) 0.2433(4) -0.00856(14) 0.0337(7) Uani 1 1 d . . . . .
H16A H 0.5994 0.1336 -0.0025 0.051 Uiso 1 1 calc GR . . . .
H16B H 0.6099 0.2991 -0.0410 0.051 Uiso 1 1 calc GR . . . .
H16C H 0.5172 0.2386 -0.0232 0.051 Uiso 1 1 calc GR . . . .
C17 C 0.43218(19) 0.5136(4) 0.17968(17) 0.0424(8) Uani 1 1 d . . . . .
H17A H 0.3830 0.4989 0.1493 0.064 Uiso 1 1 calc GR . . . .
H17B H 0.4371 0.6276 0.1916 0.064 Uiso 1 1 calc GR . . . .
H17C H 0.4244 0.4488 0.2185 0.064 Uiso 1 1 calc GR . . . .
C18 C 0.75712(17) 0.4724(4) 0.18844(14) 0.0352(7) Uani 1 1 d . . . . .
H18A H 0.7460 0.5362 0.2269 0.053 Uiso 1 1 calc GR . . . .
H18B H 0.7947 0.5330 0.1609 0.053 Uiso 1 1 calc GR . . . .
H18C H 0.7846 0.3707 0.2015 0.053 Uiso 1 1 calc GR . . . .
C19 C 0.76465(15) 0.4317(3) -0.02026(13) 0.0222(5) Uani 1 1 d . . . . .
C20 C 0.79330(16) 0.3492(3) -0.07651(13) 0.0243(5) Uani 1 1 d . . . . .
C21 C 0.80572(17) 0.4339(3) -0.13477(14) 0.0295(6) Uani 1 1 d . . . . .
H21 H 0.8239 0.3762 -0.1712 0.035 Uiso 1 1 calc R . . . .
C22 C 0.79168(17) 0.6027(4) -0.14004(14) 0.0319(6) Uani 1 1 d . . . . .
C23 C 0.76247(16) 0.6829(3) -0.08534(14) 0.0295(6) Uani 1 1 d . . . . .
H23 H 0.7529 0.7957 -0.0878 0.035 Uiso 1 1 calc R . . . .
C24 C 0.74683(16) 0.6023(3) -0.02690(13) 0.0260(6) Uani 1 1 d . . . . .
C25 C 0.71445(19) 0.7071(3) 0.02894(14) 0.0353(7) Uani 1 1 d . . . . .
H25A H 0.7137 0.8206 0.0159 0.053 Uiso 1 1 calc GR . . . .
H25B H 0.7525 0.6935 0.0674 0.053 Uiso 1 1 calc GR . . . .
H25C H 0.6567 0.6732 0.0387 0.053 Uiso 1 1 calc GR . . . .
C26 C 0.80899(19) 0.1644(3) -0.07654(14) 0.0331(6) Uani 1 1 d . . . . .
H26A H 0.8031 0.1236 -0.1209 0.050 Uiso 1 1 calc GR . . . .
H26B H 0.7672 0.1113 -0.0501 0.050 Uiso 1 1 calc GR . . . .
H26C H 0.8666 0.1417 -0.0586 0.050 Uiso 1 1 calc GR . . . .
C27 C 0.8057(2) 0.6941(4) -0.20337(17) 0.0526(9) Uani 1 1 d . . . . .
H27A H 0.7776 0.7994 -0.2021 0.079 Uiso 1 1 calc GR . . . .
H27B H 0.7814 0.6317 -0.2400 0.079 Uiso 1 1 calc GR . . . .
H27C H 0.8668 0.7093 -0.2083 0.079 Uiso 1 1 calc GR . . . .
B1 B 0.75546(18) 0.3414(3) 0.04809(15) 0.0229(6) Uani 1 1 d . . . . .
Cl1 Cl 0.58142(6) -0.11206(10) 0.16280(5) 0.0553(3) Uani 1 1 d . . . . .
Cl2 Cl 0.41148(5) 0.03688(12) 0.15316(5) 0.0538(3) Uani 1 1 d . . . . .
Cl3 Cl 0.51543(6) 0.05779(15) 0.27473(5) 0.0683(3) Uani 1 1 d . . . . .
C28 C 0.51806(19) 0.0520(4) 0.18858(15) 0.0364(7) Uani 1 1 d . . . . .
H28 H 0.5439 0.1548 0.1736 0.044 Uiso 1 1 calc R . . . .


_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
C1 C2 1.410(4) . ?
C1 C6 1.423(3) . ?
C1 B1 1.579(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.385(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.387(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.386(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.397(4) . ?
C6 C7 1.481(3) . ?
C7 C8 1.398(3) . ?
C7 C9 1.395(3) . ?
C8 H8 0.9300 . ?
C8 C9 1.382(4) 3_765 ?
C9 C8 1.382(4) 3_765 ?
C9 H9 0.9300 . ?
C10 C11 1.423(3) . ?
C10 C15 1.414(4) . ?
C10 B1 1.586(4) . ?
C11 C12 1.392(4) . ?
C11 C16 1.505(4) . ?
C12 H12 0.9300 . ?
C12 C13 1.390(4) . ?
C13 C14 1.393(4) . ?
C13 C17 1.510(4) . ?
C14 H14 0.9300 . ?
C14 C15 1.389(4) . ?
C15 C18 1.516(4) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C20 1.413(3) . ?
C19 C24 1.419(3) . ?
C19 B1 1.582(4) . ?
C20 C21 1.390(4) . ?
C20 C26 1.521(4) . ?
C21 H21 0.9300 . ?
C21 C22 1.393(4) . ?
C22 C23 1.381(4) . ?
C22 C27 1.509(4) . ?
C23 H23 0.9300 . ?
C23 C24 1.387(4) . ?
C24 C25 1.521(4) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
Cl1 C28 1.747(3) . ?
Cl2 C28 1.764(3) . ?
Cl3 C28 1.752(3) . ?
C28 H28 0.9800 . ?

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
C2 C1 C6 117.0(2) . . ?
C2 C1 B1 116.0(2) . . ?
C6 C1 B1 126.9(2) . . ?
C1 C2 H2 118.8 . . ?
C3 C2 C1 122.5(3) . . ?
C3 C2 H2 118.8 . . ?
C2 C3 H3 120.2 . . ?
C2 C3 C4 119.6(3) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 H4 120.2 . . ?
C5 C4 C3 119.6(3) . . ?
C5 C4 H4 120.2 . . ?
C4 C5 H5 119.2 . . ?
C4 C5 C6 121.6(3) . . ?
C6 C5 H5 119.2 . . ?
C1 C6 C7 123.2(2) . . ?
C5 C6 C1 119.7(2) . . ?
C5 C6 C7 117.1(2) . . ?
C8 C7 C6 122.1(2) . . ?
C9 C7 C6 120.3(2) . . ?
C9 C7 C8 117.6(2) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 C7 121.0(2) 3_765 . ?
C9 C8 H8 119.5 3_765 . ?
C7 C9 H9 119.3 . . ?
C8 C9 C7 121.4(2) 3_765 . ?
C8 C9 H9 119.3 3_765 . ?
C11 C10 B1 121.0(2) . . ?
C15 C10 C11 117.6(2) . . ?
C15 C10 B1 121.2(2) . . ?
C10 C11 C16 120.9(2) . . ?
C12 C11 C10 120.1(2) . . ?
C12 C11 C16 118.9(2) . . ?
C11 C12 H12 118.9 . . ?
C13 C12 C11 122.1(2) . . ?
C13 C12 H12 118.9 . . ?
C12 C13 C14 117.5(2) . . ?
C12 C13 C17 121.7(3) . . ?
C14 C13 C17 120.8(3) . . ?
C13 C14 H14 118.8 . . ?
C15 C14 C13 122.4(3) . . ?
C15 C14 H14 118.8 . . ?
C10 C15 C18 121.9(2) . . ?
C14 C15 C10 120.1(2) . . ?
C14 C15 C18 117.9(2) . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C17 H17A 109.5 . . ?
C13 C17 H17B 109.5 . . ?
C13 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C24 117.0(2) . . ?
C20 C19 B1 122.2(2) . . ?
C24 C19 B1 120.8(2) . . ?
C19 C20 C26 121.6(2) . . ?
C21 C20 C19 120.9(2) . . ?
C21 C20 C26 117.4(2) . . ?
C20 C21 H21 119.1 . . ?
C20 C21 C22 121.8(3) . . ?
C22 C21 H21 119.1 . . ?
C21 C22 C27 121.5(3) . . ?
C23 C22 C21 117.3(3) . . ?
C23 C22 C27 121.2(3) . . ?
C22 C23 H23 118.6 . . ?
C22 C23 C24 122.8(2) . . ?
C24 C23 H23 118.6 . . ?
C19 C24 C25 123.0(2) . . ?
C23 C24 C19 120.2(2) . . ?
C23 C24 C25 116.7(2) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C20 C26 H26A 109.5 . . ?
C20 C26 H26B 109.5 . . ?
C20 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C1 B1 C10 118.3(2) . . ?
C1 B1 C19 122.7(2) . . ?
C19 B1 C10 119.0(2) . . ?
Cl1 C28 Cl2 110.25(16) . . ?
Cl1 C28 Cl3 111.06(17) . . ?
Cl1 C28 H28 108.5 . . ?
Cl2 C28 H28 108.5 . . ?
Cl3 C28 Cl2 110.10(17) . . ?
Cl3 C28 H28 108.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 2.2(4) . . . . ?
C1 C6 C7 C8 50.1(4) . . . . ?
C1 C6 C7 C9 -130.9(3) . . . . ?
C2 C1 C6 C5 0.6(4) . . . . ?
C2 C1 C6 C7 -179.6(2) . . . . ?
C2 C1 B1 C10 33.3(3) . . . . ?
C2 C1 B1 C19 -146.3(2) . . . . ?
C2 C3 C4 C5 -0.8(4) . . . . ?
C3 C4 C5 C6 -0.6(4) . . . . ?
C4 C5 C6 C1 0.7(4) . . . . ?
C4 C5 C6 C7 -179.2(2) . . . . ?
C5 C6 C7 C8 -130.0(3) . . . . ?
C5 C6 C7 C9 48.9(3) . . . . ?
C6 C1 C2 C3 -2.0(4) . . . . ?
C6 C1 B1 C10 -150.6(2) . . . . ?
C6 C1 B1 C19 29.8(4) . . . . ?
C6 C7 C8 C9 -179.9(2) . . . 3_765 ?
C6 C7 C9 C8 179.8(2) . . . 3_765 ?
C8 C7 C9 C8 -1.2(4) . . . 3_765 ?
C9 C7 C8 C9 1.2(4) . . . 3_765 ?
C10 C11 C12 C13 -1.5(4) . . . . ?
C11 C10 C15 C14 -4.0(4) . . . . ?
C11 C10 C15 C18 178.9(2) . . . . ?
C11 C10 B1 C1 -125.2(3) . . . . ?
C11 C10 B1 C19 54.4(3) . . . . ?
C11 C12 C13 C14 -2.3(4) . . . . ?
C11 C12 C13 C17 179.0(3) . . . . ?
C12 C13 C14 C15 2.9(4) . . . . ?
C13 C14 C15 C10 0.3(4) . . . . ?
C13 C14 C15 C18 177.5(3) . . . . ?
C15 C10 C11 C12 4.6(4) . . . . ?
C15 C10 C11 C16 -172.7(2) . . . . ?
C15 C10 B1 C1 61.0(3) . . . . ?
C15 C10 B1 C19 -119.5(3) . . . . ?
C16 C11 C12 C13 175.9(2) . . . . ?
C17 C13 C14 C15 -178.4(3) . . . . ?
C19 C20 C21 C22 0.8(4) . . . . ?
C20 C19 C24 C23 -3.7(4) . . . . ?
C20 C19 C24 C25 179.2(2) . . . . ?
C20 C19 B1 C1 46.7(3) . . . . ?
C20 C19 B1 C10 -132.9(2) . . . . ?
C20 C21 C22 C23 -1.7(4) . . . . ?
C20 C21 C22 C27 179.7(3) . . . . ?
C21 C22 C23 C24 -0.2(4) . . . . ?
C22 C23 C24 C19 3.0(4) . . . . ?
C22 C23 C24 C25 -179.8(2) . . . . ?
C24 C19 C20 C21 1.9(4) . . . . ?
C24 C19 C20 C26 -176.1(2) . . . . ?
C24 C19 B1 C1 -131.3(3) . . . . ?
C24 C19 B1 C10 49.2(3) . . . . ?
C26 C20 C21 C22 179.0(2) . . . . ?
C27 C22 C23 C24 178.3(3) . . . . ?
B1 C1 C2 C3 174.4(2) . . . . ?
B1 C1 C6 C5 -175.4(2) . . . . ?
B1 C1 C6 C7 4.4(4) . . . . ?
B1 C10 C11 C12 -169.5(2) . . . . ?
B1 C10 C11 C16 13.2(4) . . . . ?
B1 C10 C15 C14 170.0(2) . . . . ?
B1 C10 C15 C18 -7.0(4) . . . . ?
B1 C19 C20 C21 -176.1(2) . . . . ?
B1 C19 C20 C26 5.8(4) . . . . ?
B1 C19 C24 C23 174.3(2) . . . . ?
B1 C19 C24 C25 -2.8(4) . . . . ?

_olex2_date_sample_data_collection 2016-05-18
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_yulr_1213_2
_database_code_depnum_ccdc_archive 'CCDC 1544755'
_audit_update_record             
;
2017-07-06 deposited with the CCDC.
2017-08-09 downloaded from the CCDC.
;
_audit_creation_date             2017-06-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C20 H40 K O8), C54 H56 B2, 2(C4 H8 O)'
_chemical_formula_sum            'C102 H152 B2 K2 O18'
_chemical_formula_weight         1766.05
_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'
B B 0.0013 0.0007 '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'
O O 0.0106 0.0060 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.8138(5)
_cell_length_b                   13.8501(6)
_cell_length_c                   16.3243(7)
_cell_angle_alpha                104.712(4)
_cell_angle_beta                 107.141(4)
_cell_angle_gamma                103.546(4)
_cell_volume                     2523.5(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    3489
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.424
_cell_measurement_theta_min      3.780
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0713
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18549
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         3.325
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -18.00   25.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5055  -99.0000   60.0000 43

#__ type_ start__ end____ width___ exp.time_
  2 omega -102.00  -77.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5055  178.0000   90.0000 25

#__ type_ start__ end____ width___ exp.time_
  3 omega  -47.00   54.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867  -38.0000    0.0000 101

#__ type_ start__ end____ width___ exp.time_
  4 omega  -45.00   53.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867  -38.0000   90.0000 98

#__ type_ start__ end____ width___ exp.time_
  5 omega    1.00   86.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867   77.0000 -120.0000 85

#__ type_ start__ end____ width___ exp.time_
  6 omega   16.00   77.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867   77.0000  -60.0000 61

#__ type_ start__ end____ width___ exp.time_
  7 omega   17.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867   57.0000   30.0000 27
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0518472000
_diffrn_orient_matrix_UB_12      0.0105950000
_diffrn_orient_matrix_UB_13      0.0372133000
_diffrn_orient_matrix_UB_21      0.0228659000
_diffrn_orient_matrix_UB_22      0.0502374000
_diffrn_orient_matrix_UB_23      -0.0030460000
_diffrn_orient_matrix_UB_31      -0.0238130000
_diffrn_orient_matrix_UB_32      0.0228138000
_diffrn_orient_matrix_UB_33      0.0309466000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6178
_reflns_number_total             9906
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     610
_refine_ls_number_reflns         9906
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.1337
_refine_ls_R_factor_gt           0.0894
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1349P)²+2.2114P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2362
_refine_ls_wR_factor_ref         0.2779
_refine_special_details          ?


# start Validation Reply Form
_vrf_PLAT242_yulr_1213_2         
;
PROBLEM: Low 'MainMol' Ueq as Compared to Neighbors of.....     C52 Check   
RESPONSE: due to the disordered solvent of THF
;

_vrf_PLAT910_yulr_1213_2         
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).....       22 Note  
RESPONSE: Theta min = 3.780 deg. The theta value of the missing reflections
are less than 3.780 deg. and therefore reflections were excluded
;
# end Validation Reply Form

_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C55) \\sim Ueq, Uanis(C54) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C47) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C49)
\\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C48) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Fixed Sof: H44C(0.4) H44D(0.4) H44A(0.6) H44B(0.6) H51C(0.5) H51D(0.5)
 H51A(0.5) H51B(0.5) H53A(0.5) H53B(0.5) H53C(0.5) H53D(0.5) O10(0.5) C48(0.6)
 H48A(0.6) H48B(0.6) C49(0.6) H49A(0.6) H49B(0.6) C50(0.6) H50A(0.6) H50B(0.6)
 C54(0.65) H54A(0.65) H54B(0.65) O9(0.5) C45(0.4) H45A(0.4) H45B(0.4) C46(0.4)
 H46A(0.4) H46B(0.4) C47(0.4) H47A(0.4) H47B(0.4) C55(0.35) H55A(0.35)
 H55B(0.35)
4.a Ternary CH refined with riding coordinates:
 C8(H8)
4.b Secondary CH2 refined with riding coordinates:
 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), C39(H39A,H39B), C44(H44C,H44D), C44(H44A,H44B),
  C51(H51C,H51D), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C53(H53C,
 H53D), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C54(H54A,H54B),
 C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C55(H55A,H55B), C40(H40A,H40B),
  C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C12(H12), C14(H14), C21(H21), C23(H23)
4.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.03185(7) 0.72587(6) 0.28634(5) 0.0369(2) Uani 1 1 d . . . . .
O1 O 0.2364(3) 0.8371(2) 0.2710(2) 0.0603(9) Uani 1 1 d . . . . .
O2 O 0.0177(3) 0.7821(3) 0.1306(2) 0.0631(9) Uani 1 1 d . . . . .
O3 O -0.1847(3) 0.7123(3) 0.1669(2) 0.0658(9) Uani 1 1 d . . . . .
O4 O -0.1699(3) 0.6163(3) 0.3019(2) 0.0595(8) Uani 1 1 d . . . . .
O5 O 0.0463(3) 0.6721(2) 0.4444(2) 0.0556(8) Uani 1 1 d . . . . .
O6 O 0.2435(3) 0.7368(3) 0.4034(2) 0.0619(9) Uani 1 1 d . . . . .
O7 O 0.0358(3) 0.9214(3) 0.3805(3) 0.0704(10) Uani 1 1 d . . . . .
C28 C 0.2236(5) 0.8320(4) 0.1831(4) 0.0736(16) Uani 1 1 d . . . . .
H28A H 0.2157 0.7597 0.1467 0.088 Uiso 1 1 calc R . . . .
H28B H 0.2936 0.8822 0.1842 0.088 Uiso 1 1 calc R . . . .
C29 C 0.1182(5) 0.8588(4) 0.1386(3) 0.0651(14) Uani 1 1 d . . . . .
H29A H 0.1240 0.9298 0.1761 0.078 Uiso 1 1 calc R . . . .
H29B H 0.1137 0.8600 0.0773 0.078 Uiso 1 1 calc R . . . .
C30 C -0.0847(6) 0.8014(5) 0.0895(4) 0.0795(18) Uani 1 1 d . . . . .
H30A H -0.0903 0.8052 0.0287 0.095 Uiso 1 1 calc R . . . .
H30B H -0.0837 0.8700 0.1278 0.095 Uiso 1 1 calc R . . . .
C31 C -0.1873(5) 0.7135(5) 0.0795(3) 0.0732(15) Uani 1 1 d . . . . .
H31A H -0.2597 0.7236 0.0461 0.088 Uiso 1 1 calc R . . . .
H31B H -0.1860 0.6448 0.0435 0.088 Uiso 1 1 calc R . . . .
C32 C -0.2760(4) 0.6295(5) 0.1606(4) 0.0756(16) Uani 1 1 d . . . . .
H32A H -0.2718 0.5608 0.1276 0.091 Uiso 1 1 calc R . . . .
H32B H -0.3509 0.6352 0.1263 0.091 Uiso 1 1 calc R . . . .
C33 C -0.2678(4) 0.6355(5) 0.2563(4) 0.0716(15) Uani 1 1 d . . . . .
H33A H -0.2652 0.7067 0.2906 0.086 Uiso 1 1 calc R . . . .
H33B H -0.3374 0.5827 0.2530 0.086 Uiso 1 1 calc R . . . .
C34 C -0.1592(5) 0.6242(4) 0.3903(4) 0.0690(15) Uani 1 1 d . . . . .
H34A H -0.2290 0.5743 0.3896 0.083 Uiso 1 1 calc R . . . .
H34B H -0.1515 0.6969 0.4255 0.083 Uiso 1 1 calc R . . . .
C35 C -0.0520(5) 0.5979(4) 0.4352(4) 0.0627(13) Uani 1 1 d . . . . .
H35A H -0.0481 0.5957 0.4961 0.075 Uiso 1 1 calc R . . . .
H35B H -0.0576 0.5271 0.3974 0.075 Uiso 1 1 calc R . . . .
C36 C 0.1456(5) 0.6481(5) 0.4809(3) 0.0685(14) Uani 1 1 d . . . . .
H36A H 0.1403 0.5790 0.4402 0.082 Uiso 1 1 calc R . . . .
H36B H 0.1524 0.6424 0.5414 0.082 Uiso 1 1 calc R . . . .
C37 C 0.2498(5) 0.7322(5) 0.4909(3) 0.0702(15) Uani 1 1 d . . . . .
H37A H 0.2543 0.8015 0.5306 0.084 Uiso 1 1 calc R . . . .
H37B H 0.3205 0.7169 0.5200 0.084 Uiso 1 1 calc R . . . .
C38 C 0.3392(4) 0.8092(4) 0.4058(4) 0.0688(14) Uani 1 1 d . . . . .
H38A H 0.4097 0.7943 0.4363 0.083 Uiso 1 1 calc R . . . .
H38B H 0.3462 0.8813 0.4419 0.083 Uiso 1 1 calc R . . . .
C39 C 0.3305(4) 0.8046(4) 0.3119(4) 0.0645(13) Uani 1 1 d . . . . .
H39A H 0.4037 0.8517 0.3147 0.077 Uiso 1 1 calc R . . . .
H39B H 0.3181 0.7314 0.2744 0.077 Uiso 1 1 calc R . . . .
C44 C 0.1473(6) 0.9786(5) 0.4463(5) 0.103(2) Uani 1 1 d . . . . .
H44C H 0.2096 0.9654 0.4256 0.124 Uiso 0.4 1 calc R . P A 2
H44D H 0.1585 0.9697 0.5063 0.124 Uiso 0.4 1 calc R . P A 2
H44A H 0.2036 0.9829 0.4157 0.124 Uiso 0.6 1 calc R . P B 1
H44B H 0.1671 0.9402 0.4891 0.124 Uiso 0.6 1 calc R . P B 1
C51 C 0.1294(7) 0.5000(5) 0.2053(6) 0.111(3) Uani 1 1 d . . . . .
H51C H 0.2058 0.5500 0.2169 0.134 Uiso 0.5 1 calc R . P C 2
H51D H 0.1335 0.4790 0.2594 0.134 Uiso 0.5 1 calc R . P C 2
H51A H 0.1731 0.4843 0.2584 0.134 Uiso 0.5 1 calc R . P D 1
H51B H 0.1829 0.5604 0.2000 0.134 Uiso 0.5 1 calc R . P D 1
C52 C 0.0919(6) 0.4086(5) 0.1234(4) 0.0772(16) Uani 1 1 d . . . . .
H52A H 0.1153 0.3499 0.1382 0.093 Uiso 1 1 calc R . . . .
H52B H 0.1246 0.4267 0.0792 0.093 Uiso 1 1 calc R . . . .
C53 C -0.0361(8) 0.3799(7) 0.0866(6) 0.149(4) Uani 1 1 d . . . . .
H53A H -0.0747 0.3028 0.0690 0.179 Uiso 0.5 1 calc R . P E 1
H53B H -0.0633 0.4018 0.0332 0.179 Uiso 0.5 1 calc R . P E 1
H53C H -0.0727 0.3421 0.1203 0.179 Uiso 0.5 1 calc R . P F 2
H53D H -0.0717 0.3381 0.0204 0.179 Uiso 0.5 1 calc R . P F 2
O10 O 0.0422(9) 0.5290(9) 0.2213(7) 0.085(3) Uani 0.5 1 d . U P G 1
C48 C 0.1580(9) 1.0858(7) 0.4983(7) 0.062(2) Uani 0.6 1 d . U P H 1
H48A H 0.2370 1.1365 0.5182 0.075 Uiso 0.6 1 calc R . P H 1
H48B H 0.1362 1.0880 0.5519 0.075 Uiso 0.6 1 calc R . P H 1
C49 C 0.0697(13) 1.1051(9) 0.4244(8) 0.064(3) Uani 0.6 1 d . U P H 1
H49A H 0.0094 1.1231 0.4454 0.077 Uiso 0.6 1 calc R . P H 1
H49B H 0.1077 1.1636 0.4073 0.077 Uiso 0.6 1 calc R . P H 1
C50 C 0.0180(11) 1.0021(8) 0.3449(6) 0.069(2) Uani 0.6 1 d . U P H 1
H50A H -0.0658 0.9874 0.3132 0.082 Uiso 0.6 1 calc R . P H 1
H50B H 0.0562 1.0055 0.3006 0.082 Uiso 0.6 1 calc R . P H 1
C54 C -0.0576(11) 0.4425(10) 0.1676(10) 0.121(4) Uani 0.65 1 d . U P G 1
H54A H -0.1242 0.4667 0.1458 0.146 Uiso 0.65 1 calc R . P G 1
H54B H -0.0755 0.3976 0.2034 0.146 Uiso 0.65 1 calc R . P G 1
O9 O 0.0365(12) 0.5463(8) 0.1817(7) 0.083(3) Uani 0.5 1 d . U P G 2
C45 C 0.126(2) 1.1029(16) 0.4429(18) 0.088(6) Uani 0.4 1 d . U P H 2
H45A H 0.1594 1.1561 0.5054 0.105 Uiso 0.4 1 calc R . P H 2
H45B H 0.1640 1.1307 0.4051 0.105 Uiso 0.4 1 calc R . P H 2
C46 C 0.0033(17) 1.0828(14) 0.4040(13) 0.073(5) Uani 0.4 1 d . U P H 2
H46A H -0.0131 1.1275 0.3665 0.088 Uiso 0.4 1 calc R . P H 2
H46B H -0.0274 1.0991 0.4530 0.088 Uiso 0.4 1 calc R . P H 2
C47 C -0.0528(18) 0.9664(15) 0.3450(13) 0.093(5) Uani 0.4 1 d . U P H 2
H47A H -0.1255 0.9343 0.3524 0.111 Uiso 0.4 1 calc R . P H 2
H47B H -0.0695 0.9563 0.2796 0.111 Uiso 0.4 1 calc R . P H 2
C55 C -0.0387(18) 0.4948(15) 0.1075(15) 0.097(6) Uani 0.35 1 d . U P G 2
H55A H -0.0237 0.5231 0.0606 0.116 Uiso 0.35 1 calc R . P G 2
H55B H -0.1152 0.4968 0.1081 0.116 Uiso 0.35 1 calc R . P G 2
C1 C 0.4313(3) 1.4223(3) 0.2617(2) 0.0311(8) Uani 1 1 d . . . . .
C2 C 0.3983(3) 1.4155(3) 0.1695(2) 0.0389(9) Uani 1 1 d . . . . .
H2 H 0.3699 1.3478 0.1231 0.047 Uiso 1 1 calc R . . . .
C3 C 0.4058(3) 1.5044(3) 0.1445(2) 0.0411(9) Uani 1 1 d . . . . .
H3 H 0.3843 1.4967 0.0817 0.049 Uiso 1 1 calc R . . . .
C4 C 0.4445(3) 1.6048(3) 0.2100(2) 0.0393(9) Uani 1 1 d . . . . .
H4 H 0.4493 1.6656 0.1925 0.047 Uiso 1 1 calc R . . . .
C5 C 0.4757(3) 1.6147(3) 0.3012(2) 0.0340(8) Uani 1 1 d . . . . .
H5 H 0.5030 1.6828 0.3469 0.041 Uiso 1 1 calc R . . . .
C6 C 0.4674(3) 1.5251(3) 0.3265(2) 0.0291(7) Uani 1 1 d . . . . .
C7 C 0.4919(3) 1.5240(2) 0.4204(2) 0.0261(7) Uani 1 1 d . . . . .
C8 C 0.4979(3) 1.4160(3) 0.4187(2) 0.0280(7) Uani 1 1 d . . . . .
H8 H 0.5790 1.4240 0.4226 0.034 Uiso 1 1 calc R . . . .
C9 C 0.5025(3) 1.4008(3) 0.5076(2) 0.0285(7) Uani 1 1 d . . . . .
H9 H 0.5014 1.3337 0.5125 0.034 Uiso 1 1 calc R . . . .
C10 C 0.2748(3) 1.2676(3) 0.2658(2) 0.0294(7) Uani 1 1 d . . . . .
C11 C 0.2220(3) 1.1841(3) 0.1797(2) 0.0341(8) Uani 1 1 d . . . . .
C12 C 0.1020(3) 1.1323(3) 0.1393(2) 0.0357(8) Uani 1 1 d . . . . .
H12 H 0.0710 1.0761 0.0822 0.043 Uiso 1 1 calc R . . . .
C13 C 0.0268(3) 1.1597(3) 0.1792(3) 0.0394(9) Uani 1 1 d . . . . .
C14 C 0.0777(3) 1.2424(3) 0.2637(2) 0.0365(8) Uani 1 1 d . . . . .
H14 H 0.0291 1.2632 0.2937 0.044 Uiso 1 1 calc R . . . .
C15 C 0.1967(3) 1.2956(3) 0.3056(2) 0.0310(8) Uani 1 1 d . . . . .
C16 C 0.2889(4) 1.1413(3) 0.1253(2) 0.0411(9) Uani 1 1 d . . . . .
H16A H 0.3599 1.1980 0.1379 0.062 Uiso 1 1 calc GR . . . .
H16B H 0.2410 1.1148 0.0599 0.062 Uiso 1 1 calc GR . . . .
H16C H 0.3090 1.0835 0.1428 0.062 Uiso 1 1 calc GR . . . .
C17 C -0.1027(4) 1.1039(4) 0.1344(3) 0.0564(12) Uani 1 1 d . . . . .
H17A H -0.1236 1.0653 0.0694 0.085 Uiso 1 1 calc GR . . . .
H17B H -0.1424 1.1562 0.1407 0.085 Uiso 1 1 calc GR . . . .
H17C H -0.1261 1.0539 0.1640 0.085 Uiso 1 1 calc GR . . . .
C18 C 0.2361(3) 1.3840(3) 0.3954(2) 0.0404(9) Uani 1 1 d . . . . .
H18A H 0.2869 1.3677 0.4439 0.061 Uiso 1 1 calc GR . . . .
H18B H 0.1685 1.3917 0.4093 0.061 Uiso 1 1 calc GR . . . .
H18C H 0.2785 1.4503 0.3913 0.061 Uiso 1 1 calc GR . . . .
C19 C 0.4873(3) 1.2423(3) 0.2995(2) 0.0347(8) Uani 1 1 d . . . . .
C20 C 0.5836(4) 1.2519(3) 0.2718(2) 0.0451(10) Uani 1 1 d . . . . .
C21 C 0.6373(4) 1.1747(4) 0.2662(3) 0.0601(13) Uani 1 1 d . . . . .
H21 H 0.7002 1.1832 0.2460 0.072 Uiso 1 1 calc R . . . .
C22 C 0.6020(5) 1.0863(4) 0.2891(3) 0.0675(15) Uani 1 1 d . . . . .
C23 C 0.5146(4) 1.0795(3) 0.3207(3) 0.0556(12) Uani 1 1 d . . . . .
H23 H 0.4913 1.0212 0.3395 0.067 Uiso 1 1 calc R . . . .
C24 C 0.4570(3) 1.1537(3) 0.3270(2) 0.0409(9) Uani 1 1 d . . . . .
C25 C 0.3626(4) 1.1339(3) 0.3646(3) 0.0459(10) Uani 1 1 d . . . . .
H25A H 0.3584 1.2017 0.3976 0.069 Uiso 1 1 calc GR . . . .
H25B H 0.3801 1.0950 0.4065 0.069 Uiso 1 1 calc GR . . . .
H25C H 0.2882 1.0920 0.3141 0.069 Uiso 1 1 calc GR . . . .
C26 C 0.6635(7) 1.0044(6) 0.2844(5) 0.105(2) Uani 1 1 d . . . . .
H26A H 0.6518 0.9689 0.2206 0.157 Uiso 1 1 calc GR . . . .
H26B H 0.6318 0.9519 0.3090 0.157 Uiso 1 1 calc GR . . . .
H26C H 0.7466 1.0398 0.3206 0.157 Uiso 1 1 calc GR . . . .
C27 C 0.6334(4) 1.3461(4) 0.2485(3) 0.0591(12) Uani 1 1 d . . . . .
H27A H 0.5811 1.3412 0.1889 0.089 Uiso 1 1 calc GR . . . .
H27B H 0.7092 1.3474 0.2460 0.089 Uiso 1 1 calc GR . . . .
H27C H 0.6425 1.4112 0.2954 0.089 Uiso 1 1 calc GR . . . .
B1 B 0.4189(4) 1.3296(3) 0.3094(2) 0.0293(8) Uani 1 1 d . . . . .
O8 O -0.3269(7) 0.2013(7) -0.0164(7) 0.186(3) Uani 1 1 d . . . . .
C40 C -0.3635(9) 0.2872(7) -0.0016(6) 0.119(3) Uani 1 1 d . . . . .
H40A H -0.3422 0.3296 -0.0384 0.143 Uiso 1 1 calc R . . . .
H40B H -0.3251 0.3326 0.0637 0.143 Uiso 1 1 calc R . . . .
C41 C -0.4908(10) 0.2513(11) -0.0276(7) 0.149(4) Uani 1 1 d . . . . .
H41A H -0.5324 0.2423 -0.0921 0.179 Uiso 1 1 calc R . . . .
H41B H -0.5151 0.2999 0.0129 0.179 Uiso 1 1 calc R . . . .
C42 C -0.5081(9) 0.1415(10) -0.0120(6) 0.142(4) Uani 1 1 d . . . . .
H42A H -0.5083 0.1485 0.0498 0.170 Uiso 1 1 calc R . . . .
H42B H -0.5814 0.0872 -0.0582 0.170 Uiso 1 1 calc R . . . .
C43 C -0.4088(9) 0.1153(9) -0.0223(8) 0.142(3) Uani 1 1 d . . . . .
H43A H -0.3759 0.0875 0.0260 0.171 Uiso 1 1 calc R . . . .
H43B H -0.4336 0.0591 -0.0823 0.171 Uiso 1 1 calc R . . . .


_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 2.828(3) . ?
K1 O2 2.810(3) . ?
K1 O3 2.813(3) . ?
K1 O4 2.792(3) . ?
K1 O5 2.829(3) . ?
K1 O6 2.764(3) . ?
K1 O7 2.734(3) . ?
K1 O10 2.713(11) . ?
K1 O9 2.661(10) . ?
O1 C28 1.376(6) . ?
O1 C39 1.426(6) . ?
O2 C29 1.412(6) . ?
O2 C30 1.408(7) . ?
O3 C31 1.423(6) . ?
O3 C32 1.391(6) . ?
O4 C33 1.379(6) . ?
O4 C34 1.383(6) . ?
O5 C35 1.367(6) . ?
O5 C36 1.392(6) . ?
O6 C37 1.425(6) . ?
O6 C38 1.373(6) . ?
O7 C44 1.399(8) . ?
O7 C50 1.418(10) . ?
O7 C47 1.463(17) . ?
C28 C29 1.512(8) . ?
C30 C31 1.503(9) . ?
C32 C33 1.514(8) . ?
C34 C35 1.527(8) . ?
C36 C37 1.487(8) . ?
C38 C39 1.487(8) . ?
C44 C48 1.462(10) . ?
C44 C45 1.82(2) . ?
C51 C52 1.448(8) . ?
C51 O10 1.345(12) . ?
C51 O9 1.479(13) . ?
C52 C53 1.484(10) . ?
C53 C54 1.522(14) . ?
C53 C55 1.551(19) . ?
O10 C54 1.388(15) . ?
C48 C49 1.519(15) . ?
C49 C50 1.507(15) . ?
O9 C55 1.21(2) . ?
C45 C46 1.43(2) . ?
C46 C47 1.52(2) . ?
C1 C2 1.410(5) . ?
C1 C6 1.413(5) . ?
C1 B1 1.662(5) . ?
C2 C3 1.383(5) . ?
C3 C4 1.390(5) . ?
C4 C5 1.384(5) . ?
C5 C6 1.395(5) . ?
C6 C7 1.477(4) . ?
C7 C8 1.510(5) . ?
C7 C9 1.329(4) 2_686 ?
C8 C9 1.504(4) . ?
C8 B1 1.710(5) . ?
C9 C7 1.329(4) 2_686 ?
C10 C11 1.420(5) . ?
C10 C15 1.419(5) . ?
C10 B1 1.681(5) . ?
C11 C12 1.399(5) . ?
C11 C16 1.515(5) . ?
C12 C13 1.383(6) . ?
C13 C14 1.399(5) . ?
C13 C17 1.511(5) . ?
C14 C15 1.392(5) . ?
C15 C18 1.505(5) . ?
C19 C20 1.424(6) . ?
C19 C24 1.420(5) . ?
C19 B1 1.655(5) . ?
C20 C21 1.400(6) . ?
C20 C27 1.504(7) . ?
C21 C22 1.384(8) . ?
C22 C23 1.358(7) . ?
C22 C26 1.524(7) . ?
C23 C24 1.400(6) . ?
C24 C25 1.510(6) . ?
O8 C40 1.370(10) . ?
O8 C43 1.351(11) . ?
C40 C41 1.480(13) . ?
C41 C42 1.580(14) . ?
C42 C43 1.446(12) . ?

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 O5 119.63(10) . . ?
O2 K1 O1 60.26(11) . . ?
O2 K1 O3 60.52(11) . . ?
O2 K1 O5 179.23(9) . . ?
O3 K1 O1 119.39(11) . . ?
O3 K1 O5 119.41(10) . . ?
O4 K1 O1 179.89(11) . . ?
O4 K1 O2 119.82(11) . . ?
O4 K1 O3 60.67(10) . . ?
O4 K1 O5 60.29(10) . . ?
O6 K1 O1 61.10(10) . . ?
O6 K1 O2 119.85(11) . . ?
O6 K1 O3 179.35(11) . . ?
O6 K1 O4 118.84(10) . . ?
O6 K1 O5 60.23(10) . . ?
O7 K1 O1 85.38(11) . . ?
O7 K1 O2 91.04(11) . . ?
O7 K1 O3 83.90(11) . . ?
O7 K1 O4 94.55(11) . . ?
O7 K1 O5 88.20(10) . . ?
O7 K1 O6 96.60(11) . . ?
O10 K1 O1 96.7(2) . . ?
O10 K1 O2 98.3(3) . . ?
O10 K1 O3 103.2(2) . . ?
O10 K1 O4 83.4(2) . . ?
O10 K1 O5 82.5(3) . . ?
O10 K1 O6 76.2(2) . . ?
O10 K1 O7 170.2(3) . . ?
O9 K1 O1 89.3(3) . . ?
O9 K1 O2 82.6(2) . . ?
O9 K1 O3 95.0(3) . . ?
O9 K1 O4 90.8(3) . . ?
O9 K1 O5 98.2(2) . . ?
O9 K1 O6 84.5(3) . . ?
O9 K1 O7 173.2(2) . . ?
C28 O1 K1 113.9(3) . . ?
C28 O1 C39 111.9(4) . . ?
C39 O1 K1 110.7(3) . . ?
C29 O2 K1 115.4(3) . . ?
C30 O2 K1 115.3(3) . . ?
C30 O2 C29 112.7(4) . . ?
C31 O3 K1 114.1(3) . . ?
C32 O3 K1 113.2(3) . . ?
C32 O3 C31 112.1(4) . . ?
C33 O4 K1 114.4(3) . . ?
C33 O4 C34 111.8(4) . . ?
C34 O4 K1 114.5(3) . . ?
C35 O5 K1 114.1(3) . . ?
C35 O5 C36 112.3(4) . . ?
C36 O5 K1 113.8(3) . . ?
C37 O6 K1 116.6(3) . . ?
C38 O6 K1 116.0(3) . . ?
C38 O6 C37 113.8(4) . . ?
C44 O7 K1 108.9(3) . . ?
C44 O7 C50 97.8(6) . . ?
C44 O7 C47 125.9(9) . . ?
C50 O7 K1 126.9(4) . . ?
C47 O7 K1 122.2(7) . . ?
O1 C28 C29 111.0(4) . . ?
O2 C29 C28 109.2(4) . . ?
O2 C30 C31 109.2(4) . . ?
O3 C31 C30 110.3(4) . . ?
O3 C32 C33 108.5(4) . . ?
O4 C33 C32 110.9(4) . . ?
O4 C34 C35 108.9(4) . . ?
O5 C35 C34 110.5(4) . . ?
O5 C36 C37 110.0(4) . . ?
O6 C37 C36 109.9(4) . . ?
O6 C38 C39 111.0(5) . . ?
O1 C39 C38 109.9(4) . . ?
O7 C44 C48 112.5(7) . . ?
O7 C44 C45 90.8(9) . . ?
C52 C51 O9 101.7(6) . . ?
O10 C51 C52 114.0(7) . . ?
C51 C52 C53 103.5(5) . . ?
C52 C53 C54 102.2(7) . . ?
C52 C53 C55 96.5(10) . . ?
C51 O10 K1 129.4(7) . . ?
C51 O10 C54 105.7(9) . . ?
C54 O10 K1 121.2(8) . . ?
C44 C48 C49 98.7(8) . . ?
C50 C49 C48 104.6(9) . . ?
O7 C50 C49 107.3(8) . . ?
O10 C54 C53 107.7(10) . . ?
C51 O9 K1 125.2(7) . . ?
C55 O9 K1 121.9(10) . . ?
C55 O9 C51 113.0(11) . . ?
C46 C45 C44 107.9(15) . . ?
C45 C46 C47 107.1(16) . . ?
O7 C47 C46 102.6(14) . . ?
O9 C55 C53 106.3(13) . . ?
C2 C1 C6 115.7(3) . . ?
C2 C1 B1 131.7(3) . . ?
C6 C1 B1 112.0(3) . . ?
C3 C2 C1 122.0(3) . . ?
C2 C3 C4 120.9(3) . . ?
C5 C4 C3 118.9(3) . . ?
C4 C5 C6 120.3(3) . . ?
C1 C6 C7 112.1(3) . . ?
C5 C6 C1 122.2(3) . . ?
C5 C6 C7 125.7(3) . . ?
C6 C7 C8 107.3(3) . . ?
C9 C7 C6 127.3(3) 2_686 . ?
C9 C7 C8 125.1(3) 2_686 . ?
C7 C8 B1 107.4(3) . . ?
C9 C8 C7 111.2(3) . . ?
C9 C8 B1 129.1(3) . . ?
C7 C9 C8 123.6(3) 2_686 . ?
C11 C10 B1 119.8(3) . . ?
C15 C10 C11 114.9(3) . . ?
C15 C10 B1 125.2(3) . . ?
C10 C11 C16 123.8(3) . . ?
C12 C11 C10 121.8(3) . . ?
C12 C11 C16 114.4(3) . . ?
C13 C12 C11 122.7(3) . . ?
C12 C13 C14 116.0(3) . . ?
C12 C13 C17 122.1(4) . . ?
C14 C13 C17 121.9(4) . . ?
C15 C14 C13 122.7(4) . . ?
C10 C15 C18 122.7(3) . . ?
C14 C15 C10 121.8(3) . . ?
C14 C15 C18 115.5(3) . . ?
C20 C19 B1 125.2(3) . . ?
C24 C19 C20 114.9(4) . . ?
C24 C19 B1 119.8(3) . . ?
C19 C20 C27 121.7(4) . . ?
C21 C20 C19 121.5(4) . . ?
C21 C20 C27 116.8(4) . . ?
C22 C21 C20 122.2(5) . . ?
C21 C22 C26 121.3(6) . . ?
C23 C22 C21 116.7(4) . . ?
C23 C22 C26 121.9(6) . . ?
C22 C23 C24 123.6(5) . . ?
C19 C24 C25 122.8(3) . . ?
C23 C24 C19 120.9(4) . . ?
C23 C24 C25 116.2(4) . . ?
C1 B1 C8 94.8(3) . . ?
C1 B1 C10 102.1(3) . . ?
C10 B1 C8 125.2(3) . . ?
C19 B1 C1 122.7(3) . . ?
C19 B1 C8 102.7(3) . . ?
C19 B1 C10 110.4(3) . . ?
C43 O8 C40 109.7(8) . . ?
O8 C40 C41 109.8(9) . . ?
C40 C41 C42 99.1(7) . . ?
C43 C42 C41 103.0(8) . . ?
O8 C43 C42 110.8(10) . . ?

_olex2_date_sample_data_collection 2016-12-13
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_yulr_1114
_database_code_depnum_ccdc_archive 'CCDC 1544756'
_audit_update_record             
;
2017-07-06 deposited with the CCDC.
2017-08-09 downloaded from the CCDC.
;
_audit_creation_date             2017-06-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C70 H88 B2 K2 O4, 2(C4 H8 O)'
_chemical_formula_sum            'C78 H104 B2 K2 O6'
_chemical_formula_weight         1237.43
_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'
B B 0.0013 0.0007 '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'
O O 0.0106 0.0060 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.2166(9)
_cell_length_b                   12.8705(12)
_cell_length_c                   13.0567(12)
_cell_angle_alpha                72.277(8)
_cell_angle_beta                 70.112(7)
_cell_angle_gamma                67.341(8)
_cell_volume                     1745.6(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1792
_cell_measurement_temperature    291.43(10)
_cell_measurement_theta_max      22.6460
_cell_measurement_theta_min      3.7310
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.1001
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12129
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.245
_diffrn_ambient_temperature      291.43(10)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -102.00  -72.00   1.5000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5055  178.0000  -30.0000 20

#__ type_ start__ end____ width___ exp.time_
  2 omega   -4.00   26.00   1.5000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5055  -99.0000  -60.0000 20

#__ type_ start__ end____ width___ exp.time_
  3 omega    3.00   81.00   1.5000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867   57.0000 -180.0000 52

#__ type_ start__ end____ width___ exp.time_
  4 omega   36.00  105.00   1.5000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867 -178.0000  -60.0000 46

#__ type_ start__ end____ width___ exp.time_
  5 omega    5.00   89.00   1.5000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867   77.0000  -60.0000 56

#__ type_ start__ end____ width___ exp.time_
  6 omega  -38.00   89.50   1.5000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867  -19.0000  -30.0000 85
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0135847000
_diffrn_orient_matrix_UB_12      -0.0497917000
_diffrn_orient_matrix_UB_13      -0.0205917000
_diffrn_orient_matrix_UB_21      -0.0017344000
_diffrn_orient_matrix_UB_22      -0.0337301000
_diffrn_orient_matrix_UB_23      0.0544386000
_diffrn_orient_matrix_UB_31      -0.0635847000
_diffrn_orient_matrix_UB_32      0.0098891000
_diffrn_orient_matrix_UB_33      0.0094099000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3901
_reflns_number_total             6847
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         6847
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1273
_refine_ls_R_factor_gt           0.0673
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0633P)²+0.5256P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1830
_refine_special_details          ?

# start Validation Reply Form

_vrf_PLAT910_yulr_1114           
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).....       12 Note  
RESPONSE: Theta min = 3.73 deg. The theta value of the missing reflections
are less than 3.73 deg. and therefore reflections were excluded
;
# end Validation Reply Form

_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 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), C39(H39A,H39B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C12(H12), C14(H14), C21(H21), C23(H23)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.96798(7) -0.14796(7) 0.85683(7) 0.0423(2) Uani 1 1 d . . . . .
H8 H 0.978(2) 0.185(3) 0.951(2) 0.025(8) Uiso 1 1 d . . . . .
O1 O 0.8591(2) -0.3080(2) 0.9525(2) 0.0580(7) Uani 1 1 d . . . . .
O2 O 1.1184(2) -0.2881(2) 0.7204(2) 0.0582(8) Uani 1 1 d . . . . .
C1 C 0.7371(3) 0.2413(3) 0.9995(3) 0.0259(7) Uani 1 1 d . . . . .
C2 C 0.6302(3) 0.3333(3) 1.0238(3) 0.0307(7) Uani 1 1 d . . . . .
H2 H 0.6058 0.3920 0.9658 0.037 Uiso 1 1 calc R . . . .
C3 C 0.5600(3) 0.3393(3) 1.1315(3) 0.0369(8) Uani 1 1 d . . . . .
H3 H 0.4886 0.4007 1.1447 0.044 Uiso 1 1 calc R . . . .
C4 C 0.5953(3) 0.2542(3) 1.2200(3) 0.0367(8) Uani 1 1 d . . . . .
H4 H 0.5462 0.2569 1.2920 0.044 Uiso 1 1 calc R . . . .
C5 C 0.7043(3) 0.1650(3) 1.2004(3) 0.0338(8) Uani 1 1 d . . . . .
H5 H 0.7306 0.1093 1.2594 0.041 Uiso 1 1 calc R . . . .
C6 C 0.7741(3) 0.1597(3) 1.0917(3) 0.0260(7) Uani 1 1 d . . . . .
C7 C 0.8915(2) 0.0719(3) 1.0540(2) 0.0254(7) Uani 1 1 d . . . . .
C8 C 0.9552(3) 0.1250(3) 0.9401(3) 0.0261(7) Uani 1 1 d . . . . .
C9 C 0.9304(3) -0.0368(3) 1.1075(3) 0.0263(7) Uani 1 1 d . . . . .
H9 H 0.8704 -0.0651 1.1706 0.032 Uiso 1 1 calc R . . . .
C10 C 0.8352(3) 0.3295(3) 0.7880(2) 0.0262(7) Uani 1 1 d . . . . .
C11 C 0.9269(3) 0.3841(3) 0.7511(3) 0.0291(7) Uani 1 1 d . . . . .
C12 C 0.9162(3) 0.4864(3) 0.6711(3) 0.0355(8) Uani 1 1 d . . . . .
H12 H 0.9793 0.5184 0.6473 0.043 Uiso 1 1 calc R . . . .
C13 C 0.8165(3) 0.5416(3) 0.6261(3) 0.0344(8) Uani 1 1 d . . . . .
C14 C 0.7258(3) 0.4911(3) 0.6637(3) 0.0345(8) Uani 1 1 d . . . . .
H14 H 0.6563 0.5274 0.6365 0.041 Uiso 1 1 calc R . . . .
C15 C 0.7333(3) 0.3881(3) 0.7405(3) 0.0292(7) Uani 1 1 d . . . . .
C16 C 1.0421(3) 0.3374(3) 0.7917(3) 0.0389(8) Uani 1 1 d . . . . .
H16A H 1.0211 0.3425 0.8682 0.058 Uiso 1 1 calc GR . . . .
H16B H 1.0962 0.3816 0.7479 0.058 Uiso 1 1 calc GR . . . .
H16C H 1.0822 0.2586 0.7846 0.058 Uiso 1 1 calc GR . . . .
C17 C 0.8078(4) 0.6519(3) 0.5392(3) 0.0481(10) Uani 1 1 d . . . . .
H17A H 0.8059 0.6391 0.4712 0.072 Uiso 1 1 calc GR . . . .
H17B H 0.8777 0.6755 0.5263 0.072 Uiso 1 1 calc GR . . . .
H17C H 0.7342 0.7108 0.5650 0.072 Uiso 1 1 calc GR . . . .
C18 C 0.6279(3) 0.3420(3) 0.7648(3) 0.0368(8) Uani 1 1 d . . . . .
H18A H 0.6513 0.2861 0.7202 0.055 Uiso 1 1 calc GR . . . .
H18B H 0.5574 0.4040 0.7477 0.055 Uiso 1 1 calc GR . . . .
H18C H 0.6083 0.3066 0.8421 0.055 Uiso 1 1 calc GR . . . .
C19 C 0.8095(3) 0.1192(3) 0.8262(3) 0.0270(7) Uani 1 1 d . . . . .
C20 C 0.8819(3) 0.1001(3) 0.7176(3) 0.0286(7) Uani 1 1 d . . . . .
C21 C 0.8632(3) 0.0311(3) 0.6649(3) 0.0366(8) Uani 1 1 d . . . . .
H21 H 0.9126 0.0215 0.5942 0.044 Uiso 1 1 calc R . . . .
C22 C 0.7751(3) -0.0235(3) 0.7127(3) 0.0394(9) Uani 1 1 d . . . . .
C23 C 0.7051(3) -0.0084(3) 0.8195(3) 0.0374(8) Uani 1 1 d . . . . .
H23 H 0.6458 -0.0450 0.8551 0.045 Uiso 1 1 calc R . . . .
C24 C 0.7209(3) 0.0602(3) 0.8756(3) 0.0305(7) Uani 1 1 d . . . . .
C25 C 0.9813(3) 0.1540(3) 0.6504(3) 0.0355(8) Uani 1 1 d . . . . .
H25A H 1.0162 0.1663 0.6997 0.053 Uiso 1 1 calc GR . . . .
H25B H 0.9469 0.2263 0.6053 0.053 Uiso 1 1 calc GR . . . .
H25C H 1.0441 0.1038 0.6034 0.053 Uiso 1 1 calc GR . . . .
C26 C 0.7562(4) -0.0974(4) 0.6537(4) 0.0641(12) Uani 1 1 d . . . . .
H26A H 0.8328 -0.1542 0.6297 0.096 Uiso 1 1 calc GR . . . .
H26B H 0.7258 -0.0501 0.5904 0.096 Uiso 1 1 calc GR . . . .
H26C H 0.6979 -0.1349 0.7037 0.096 Uiso 1 1 calc GR . . . .
C27 C 0.6365(3) 0.0662(3) 0.9911(3) 0.0385(8) Uani 1 1 d . . . . .
H27A H 0.5827 0.0221 1.0069 0.058 Uiso 1 1 calc GR . . . .
H27B H 0.5888 0.1448 0.9950 0.058 Uiso 1 1 calc GR . . . .
H27C H 0.6845 0.0356 1.0447 0.058 Uiso 1 1 calc GR . . . .
C28 C 0.8746(4) -0.3945(5) 0.8983(5) 0.0878(18) Uani 1 1 d . . . . .
H28A H 0.9362 -0.4646 0.9218 0.105 Uiso 1 1 calc R . . . .
H28B H 0.9016 -0.3700 0.8184 0.105 Uiso 1 1 calc R . . . .
C29 C 0.7594(4) -0.4148(6) 0.9264(5) 0.110(2) Uani 1 1 d . . . . .
H29A H 0.7299 -0.3940 0.8604 0.132 Uiso 1 1 calc R . . . .
H29B H 0.7691 -0.4956 0.9578 0.132 Uiso 1 1 calc R . . . .
C30 C 0.6741(4) -0.3468(5) 1.0054(4) 0.0812(16) Uani 1 1 d . . . . .
H30A H 0.6362 -0.3941 1.0705 0.097 Uiso 1 1 calc R . . . .
H30B H 0.6102 -0.2871 0.9732 0.097 Uiso 1 1 calc R . . . .
C31 C 0.7463(4) -0.2952(4) 1.0361(3) 0.0568(11) Uani 1 1 d . . . . .
H31A H 0.7026 -0.2147 1.0380 0.068 Uiso 1 1 calc R . . . .
H31B H 0.7611 -0.3350 1.1086 0.068 Uiso 1 1 calc R . . . .
C32 C 1.1463(6) -0.2658(6) 0.6054(4) 0.111(2) Uani 1 1 d . . . . .
H32A H 1.1800 -0.2025 0.5745 0.133 Uiso 1 1 calc R . . . .
H32B H 1.0731 -0.2455 0.5805 0.133 Uiso 1 1 calc R . . . .
C33 C 1.2370(6) -0.3713(7) 0.5693(5) 0.120(3) Uani 1 1 d . . . . .
H33A H 1.1971 -0.4206 0.5632 0.144 Uiso 1 1 calc R . . . .
H33B H 1.2930 -0.3534 0.4983 0.144 Uiso 1 1 calc R . . . .
C34 C 1.3011(5) -0.4253(5) 0.6578(6) 0.104(2) Uani 1 1 d . . . . .
H34A H 1.3684 -0.3963 0.6438 0.124 Uiso 1 1 calc R . . . .
H34B H 1.3328 -0.5081 0.6649 0.124 Uiso 1 1 calc R . . . .
C35 C 1.2046(4) -0.3924(4) 0.7588(4) 0.0664(13) Uani 1 1 d . . . . .
H35A H 1.1657 -0.4515 0.7969 0.080 Uiso 1 1 calc R . . . .
H35B H 1.2394 -0.3811 0.8096 0.080 Uiso 1 1 calc R . . . .
B1 B 0.8340(3) 0.2074(3) 0.8808(3) 0.0258(8) Uani 1 1 d . . . . .
O3 O 0.4877(4) 0.1461(4) 0.5280(3) 0.1259(15) Uani 1 1 d . . . . .
C36 C 0.4067(6) 0.0877(5) 0.6124(5) 0.1014(18) Uani 1 1 d . . . . .
H36A H 0.3266 0.1161 0.5976 0.122 Uiso 1 1 calc R . . . .
H36B H 0.4398 0.0057 0.6144 0.122 Uiso 1 1 calc R . . . .
C37 C 0.3980(5) 0.1113(6) 0.7155(5) 0.0975(18) Uani 1 1 d . . . . .
H37A H 0.4587 0.0516 0.7516 0.117 Uiso 1 1 calc R . . . .
H37B H 0.3171 0.1164 0.7651 0.117 Uiso 1 1 calc R . . . .
C38 C 0.4208(6) 0.2216(6) 0.6859(5) 0.106(2) Uani 1 1 d . . . . .
H38A H 0.3450 0.2849 0.6855 0.127 Uiso 1 1 calc R . . . .
H38B H 0.4588 0.2264 0.7378 0.127 Uiso 1 1 calc R . . . .
C39 C 0.5026(6) 0.2233(6) 0.5757(5) 0.107(2) Uani 1 1 d . . . . .
H39A H 0.4828 0.3002 0.5308 0.128 Uiso 1 1 calc R . . . .
H39B H 0.5868 0.1998 0.5798 0.128 Uiso 1 1 calc R . . . .


_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 2.643(3) . ?
K1 O2 2.641(3) . ?
K1 C6 3.379(3) 2_757 ?
K1 C7 2.934(3) 2_757 ?
K1 C8 3.222(3) 2_757 ?
K1 C9 3.280(3) 2_757 ?
K1 C19 3.208(3) . ?
K1 C20 3.128(3) . ?
K1 C21 3.102(3) . ?
K1 C22 3.152(3) . ?
K1 C23 3.140(3) . ?
K1 C24 3.164(3) . ?
O1 C28 1.416(5) . ?
O1 C31 1.424(4) . ?
O2 C32 1.386(5) . ?
O2 C35 1.422(4) . ?
C1 C2 1.401(4) . ?
C1 C6 1.411(4) . ?
C1 B1 1.661(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.384(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.387(5) . ?
C4 H4 0.9300 . ?
C4 C5 1.388(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.392(4) . ?
C6 K1 3.379(3) 2_757 ?
C6 C7 1.478(4) . ?
C7 K1 2.934(3) 2_757 ?
C7 C8 1.513(4) . ?
C7 C9 1.339(4) . ?
C8 K1 3.222(3) 2_757 ?
C8 H8 0.97(3) . ?
C8 C9 1.498(4) 2_757 ?
C8 B1 1.728(4) . ?
C9 K1 3.280(3) 2_757 ?
C9 C8 1.498(4) 2_757 ?
C9 H9 0.9800 . ?
C10 C11 1.419(4) . ?
C10 C15 1.422(4) . ?
C10 B1 1.668(5) . ?
C11 C12 1.401(4) . ?
C11 C16 1.511(4) . ?
C12 H12 0.9300 . ?
C12 C13 1.378(4) . ?
C13 C14 1.372(5) . ?
C13 C17 1.516(4) . ?
C14 H14 0.9300 . ?
C14 C15 1.389(4) . ?
C15 C18 1.519(4) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C20 1.430(4) . ?
C19 C24 1.423(4) . ?
C19 B1 1.670(4) . ?
C20 C21 1.396(4) . ?
C20 C25 1.510(4) . ?
C21 H21 0.9300 . ?
C21 C22 1.379(5) . ?
C22 C23 1.393(5) . ?
C22 C26 1.513(5) . ?
C23 H23 0.9300 . ?
C23 C24 1.403(4) . ?
C24 C27 1.516(4) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.434(6) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.426(6) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.495(6) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.472(8) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.463(8) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C35 1.486(6) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
O3 C36 1.444(6) . ?
O3 C39 1.415(6) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 C37 1.428(7) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 C38 1.462(8) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 C39 1.446(7) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?

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 C6 123.33(8) . 2_757 ?
O1 K1 C7 128.84(9) . 2_757 ?
O1 K1 C8 102.14(9) . 2_757 ?
O1 K1 C9 146.67(8) . 2_757 ?
O1 K1 C19 120.58(8) . . ?
O1 K1 C20 131.88(9) . . ?
O1 K1 C21 113.76(9) . . ?
O1 K1 C22 88.81(9) . . ?
O1 K1 C23 80.05(9) . . ?
O1 K1 C24 94.81(9) . . ?
O2 K1 O1 85.66(9) . . ?
O2 K1 C6 84.89(8) . 2_757 ?
O2 K1 C7 110.11(8) . 2_757 ?
O2 K1 C8 121.91(8) . 2_757 ?
O2 K1 C9 117.65(9) . 2_757 ?
O2 K1 C19 134.98(8) . . ?
O2 K1 C20 109.04(8) . . ?
O2 K1 C21 91.33(8) . . ?
O2 K1 C22 94.69(8) . . ?
O2 K1 C23 117.56(8) . . ?
O2 K1 C24 140.24(8) . . ?
C7 K1 C6 25.88(7) 2_757 2_757 ?
C7 K1 C8 27.95(8) 2_757 2_757 ?
C7 K1 C9 24.06(7) 2_757 2_757 ?
C7 K1 C19 82.57(8) 2_757 . ?
C7 K1 C20 89.82(8) 2_757 . ?
C7 K1 C21 114.11(9) 2_757 . ?
C7 K1 C22 134.86(9) 2_757 . ?
C7 K1 C23 125.94(9) 2_757 . ?
C7 K1 C24 100.38(8) 2_757 . ?
C8 K1 C6 42.75(7) 2_757 2_757 ?
C8 K1 C9 46.07(8) 2_757 2_757 ?
C9 K1 C6 44.32(7) 2_757 2_757 ?
C19 K1 C6 104.72(8) . 2_757 ?
C19 K1 C8 89.87(8) . 2_757 ?
C19 K1 C9 60.51(7) . 2_757 ?
C20 K1 C6 103.87(8) . 2_757 ?
C20 K1 C8 106.99(8) . 2_757 ?
C20 K1 C9 65.79(8) . 2_757 ?
C20 K1 C19 26.04(7) . . ?
C20 K1 C22 45.74(9) . . ?
C20 K1 C23 52.25(9) . . ?
C20 K1 C24 44.84(8) . . ?
C21 K1 C6 122.20(9) . 2_757 ?
C21 K1 C8 132.85(9) . 2_757 ?
C21 K1 C9 90.52(8) . 2_757 ?
C21 K1 C19 46.01(8) . . ?
C21 K1 C20 25.89(8) . . ?
C21 K1 C22 25.46(9) . . ?
C21 K1 C23 44.31(9) . . ?
C21 K1 C24 52.19(8) . . ?
C22 K1 C6 147.61(9) . 2_757 ?
C22 K1 C8 142.16(8) . 2_757 ?
C22 K1 C9 110.90(8) . 2_757 ?
C22 K1 C19 54.28(8) . . ?
C22 K1 C24 45.66(8) . . ?
C23 K1 C6 150.28(8) . 2_757 ?
C23 K1 C8 120.50(8) . 2_757 ?
C23 K1 C9 105.97(8) . 2_757 ?
C23 K1 C19 45.78(8) . . ?
C23 K1 C22 25.58(8) . . ?
C23 K1 C24 25.72(8) . . ?
C24 K1 C6 125.55(8) . 2_757 ?
C24 K1 C8 96.93(8) . 2_757 ?
C24 K1 C9 82.06(8) . 2_757 ?
C24 K1 C19 25.79(8) . . ?
C28 O1 K1 122.3(3) . . ?
C28 O1 C31 107.8(3) . . ?
C31 O1 K1 125.1(2) . . ?
C32 O2 K1 128.4(3) . . ?
C32 O2 C35 109.6(4) . . ?
C35 O2 K1 120.6(2) . . ?
C2 C1 C6 116.2(3) . . ?
C2 C1 B1 132.7(3) . . ?
C6 C1 B1 111.1(2) . . ?
C1 C2 H2 119.1 . . ?
C3 C2 C1 121.9(3) . . ?
C3 C2 H2 119.1 . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.4(3) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 120.2 . . ?
C3 C4 C5 119.6(3) . . ?
C5 C4 H4 120.2 . . ?
C4 C5 H5 120.3 . . ?
C4 C5 C6 119.4(3) . . ?
C6 C5 H5 120.3 . . ?
C1 C6 K1 117.66(19) . 2_757 ?
C1 C6 C7 110.2(3) . . ?
C5 C6 K1 94.07(18) . 2_757 ?
C5 C6 C1 122.3(3) . . ?
C5 C6 C7 127.5(3) . . ?
C7 C6 K1 60.03(14) . 2_757 ?
C6 C7 K1 94.09(17) . 2_757 ?
C6 C7 C8 107.4(3) . . ?
C8 C7 K1 86.65(16) . 2_757 ?
C9 C7 K1 92.59(18) . 2_757 ?
C9 C7 C6 126.2(3) . . ?
C9 C7 C8 126.2(3) . . ?
K1 C8 H8 47.7(17) 2_757 . ?
C7 C8 K1 65.40(15) . 2_757 ?
C7 C8 H8 106.1(17) . . ?
C7 C8 B1 102.2(2) . . ?
C9 C8 K1 99.93(17) 2_757 2_757 ?
C9 C8 H8 108.8(16) 2_757 . ?
C9 C8 C7 110.0(3) 2_757 . ?
C9 C8 B1 127.1(3) 2_757 . ?
B1 C8 K1 131.80(18) . 2_757 ?
B1 C8 H8 100.7(16) . . ?
K1 C9 H9 117.0 2_757 . ?
C7 C9 K1 63.35(17) . 2_757 ?
C7 C9 C8 123.7(3) . 2_757 ?
C7 C9 H9 117.0 . . ?
C8 C9 K1 103.76(18) 2_757 2_757 ?
C8 C9 H9 117.0 2_757 . ?
C11 C10 C15 115.0(3) . . ?
C11 C10 B1 127.3(3) . . ?
C15 C10 B1 117.7(3) . . ?
C10 C11 C16 123.8(3) . . ?
C12 C11 C10 120.9(3) . . ?
C12 C11 C16 115.3(3) . . ?
C11 C12 H12 118.5 . . ?
C13 C12 C11 123.0(3) . . ?
C13 C12 H12 118.5 . . ?
C12 C13 C17 121.9(3) . . ?
C14 C13 C12 116.4(3) . . ?
C14 C13 C17 121.7(3) . . ?
C13 C14 H14 118.5 . . ?
C13 C14 C15 123.0(3) . . ?
C15 C14 H14 118.5 . . ?
C10 C15 C18 123.5(3) . . ?
C14 C15 C10 121.7(3) . . ?
C14 C15 C18 114.8(3) . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C17 H17A 109.5 . . ?
C13 C17 H17B 109.5 . . ?
C13 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 K1 73.87(17) . . ?
C20 C19 B1 118.5(3) . . ?
C24 C19 K1 75.40(17) . . ?
C24 C19 C20 114.6(3) . . ?
C24 C19 B1 126.9(3) . . ?
B1 C19 K1 120.12(17) . . ?
C19 C20 K1 80.09(17) . . ?
C19 C20 C25 123.3(3) . . ?
C21 C20 K1 76.01(19) . . ?
C21 C20 C19 121.7(3) . . ?
C21 C20 C25 115.0(3) . . ?
C25 C20 K1 116.01(19) . . ?
K1 C21 H21 114.3 . . ?
C20 C21 K1 78.10(18) . . ?
C20 C21 H21 118.4 . . ?
C22 C21 K1 79.3(2) . . ?
C22 C21 C20 123.1(3) . . ?
C22 C21 H21 118.4 . . ?
C21 C22 K1 75.3(2) . . ?
C21 C22 C23 116.3(3) . . ?
C21 C22 C26 122.2(3) . . ?
C23 C22 K1 76.75(19) . . ?
C23 C22 C26 121.5(3) . . ?
C26 C22 K1 116.5(2) . . ?
K1 C23 H23 115.9 . . ?
C22 C23 K1 77.66(19) . . ?
C22 C23 H23 118.8 . . ?
C22 C23 C24 122.4(3) . . ?
C24 C23 K1 78.10(18) . . ?
C24 C23 H23 118.8 . . ?
C19 C24 K1 78.81(17) . . ?
C19 C24 C27 123.3(3) . . ?
C23 C24 K1 76.19(18) . . ?
C23 C24 C19 121.9(3) . . ?
C23 C24 C27 114.9(3) . . ?
C27 C24 K1 116.5(2) . . ?
C20 C25 H25A 109.5 . . ?
C20 C25 H25B 109.5 . . ?
C20 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C26 H26A 109.5 . . ?
C22 C26 H26B 109.5 . . ?
C22 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O1 C28 H28A 110.0 . . ?
O1 C28 H28B 110.0 . . ?
O1 C28 C29 108.5(4) . . ?
H28A C28 H28B 108.4 . . ?
C29 C28 H28A 110.0 . . ?
C29 C28 H28B 110.0 . . ?
C28 C29 H29A 110.1 . . ?
C28 C29 H29B 110.1 . . ?
H29A C29 H29B 108.4 . . ?
C30 C29 C28 108.2(4) . . ?
C30 C29 H29A 110.1 . . ?
C30 C29 H29B 110.1 . . ?
C29 C30 H30A 110.5 . . ?
C29 C30 H30B 110.5 . . ?
C29 C30 C31 106.0(3) . . ?
H30A C30 H30B 108.7 . . ?
C31 C30 H30A 110.5 . . ?
C31 C30 H30B 110.5 . . ?
O1 C31 C30 106.0(3) . . ?
O1 C31 H31A 110.5 . . ?
O1 C31 H31B 110.5 . . ?
C30 C31 H31A 110.5 . . ?
C30 C31 H31B 110.5 . . ?
H31A C31 H31B 108.7 . . ?
O2 C32 H32A 110.3 . . ?
O2 C32 H32B 110.3 . . ?
O2 C32 C33 107.1(5) . . ?
H32A C32 H32B 108.6 . . ?
C33 C32 H32A 110.3 . . ?
C33 C32 H32B 110.3 . . ?
C32 C33 H33A 111.1 . . ?
C32 C33 H33B 111.1 . . ?
H33A C33 H33B 109.1 . . ?
C34 C33 C32 103.3(4) . . ?
C34 C33 H33A 111.1 . . ?
C34 C33 H33B 111.1 . . ?
C33 C34 H34A 111.1 . . ?
C33 C34 H34B 111.1 . . ?
C33 C34 C35 103.5(4) . . ?
H34A C34 H34B 109.0 . . ?
C35 C34 H34A 111.1 . . ?
C35 C34 H34B 111.1 . . ?
O2 C35 C34 105.7(4) . . ?
O2 C35 H35A 110.6 . . ?
O2 C35 H35B 110.6 . . ?
C34 C35 H35A 110.6 . . ?
C34 C35 H35B 110.6 . . ?
H35A C35 H35B 108.7 . . ?
C1 B1 C8 94.2(2) . . ?
C1 B1 C10 107.8(2) . . ?
C1 B1 C19 117.5(2) . . ?
C10 B1 C8 122.2(2) . . ?
C10 B1 C19 109.2(2) . . ?
C19 B1 C8 105.9(2) . . ?
C39 O3 C36 107.7(4) . . ?
O3 C36 H36A 110.5 . . ?
O3 C36 H36B 110.5 . . ?
H36A C36 H36B 108.7 . . ?
C37 C36 O3 106.3(5) . . ?
C37 C36 H36A 110.5 . . ?
C37 C36 H36B 110.5 . . ?
C36 C37 H37A 110.7 . . ?
C36 C37 H37B 110.7 . . ?
C36 C37 C38 105.1(5) . . ?
H37A C37 H37B 108.8 . . ?
C38 C37 H37A 110.7 . . ?
C38 C37 H37B 110.7 . . ?
C37 C38 H38A 110.9 . . ?
C37 C38 H38B 110.9 . . ?
H38A C38 H38B 108.9 . . ?
C39 C38 C37 104.3(5) . . ?
C39 C38 H38A 110.9 . . ?
C39 C38 H38B 110.9 . . ?
O3 C39 C38 107.5(4) . . ?
O3 C39 H39A 110.2 . . ?
O3 C39 H39B 110.2 . . ?
C38 C39 H39A 110.2 . . ?
C38 C39 H39B 110.2 . . ?
H39A C39 H39B 108.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
K1 O1 C28 C29 -141.7(4) . . . . ?
K1 O1 C31 C30 136.7(3) . . . . ?
K1 O2 C32 C33 178.7(3) . . . . ?
K1 O2 C35 C34 -159.0(3) . . . . ?
K1 C6 C7 C8 -87.8(2) 2_757 . . . ?
K1 C6 C7 C9 96.2(3) 2_757 . . . ?
K1 C7 C8 C9 92.0(2) 2_757 . . 2_757 ?
K1 C7 C8 B1 -130.60(18) 2_757 . . . ?
K1 C7 C9 C8 -89.2(3) 2_757 . . 2_757 ?
K1 C8 B1 C1 -33.1(3) 2_757 . . . ?
K1 C8 B1 C10 81.0(3) 2_757 . . . ?
K1 C8 B1 C19 -153.3(2) 2_757 . . . ?
K1 C19 C20 C21 66.7(3) . . . . ?
K1 C19 C20 C25 -114.7(3) . . . . ?
K1 C19 C24 C23 -65.8(3) . . . . ?
K1 C19 C24 C27 114.4(3) . . . . ?
K1 C19 B1 C1 -100.6(2) . . . . ?
K1 C19 B1 C8 2.9(3) . . . . ?
K1 C19 B1 C10 136.25(19) . . . . ?
K1 C20 C21 C22 68.6(3) . . . . ?
K1 C21 C22 C23 66.8(3) . . . . ?
K1 C21 C22 C26 -112.3(3) . . . . ?
K1 C22 C23 C24 67.1(3) . . . . ?
K1 C23 C24 C19 67.2(3) . . . . ?
K1 C23 C24 C27 -113.1(3) . . . . ?
O1 C28 C29 C30 -4.4(8) . . . . ?
O2 C32 C33 C34 -28.5(7) . . . . ?
C1 C2 C3 C4 1.3(5) . . . . ?
C1 C6 C7 K1 111.0(2) . . . 2_757 ?
C1 C6 C7 C8 23.3(3) . . . . ?
C1 C6 C7 C9 -152.7(3) . . . . ?
C2 C1 C6 K1 -110.7(3) . . . 2_757 ?
C2 C1 C6 C5 4.5(4) . . . . ?
C2 C1 C6 C7 -176.6(3) . . . . ?
C2 C1 B1 C8 156.1(3) . . . . ?
C2 C1 B1 C10 30.3(4) . . . . ?
C2 C1 B1 C19 -93.6(4) . . . . ?
C2 C3 C4 C5 2.5(5) . . . . ?
C3 C4 C5 C6 -2.7(5) . . . . ?
C4 C5 C6 K1 125.6(3) . . . 2_757 ?
C4 C5 C6 C1 -0.9(5) . . . . ?
C4 C5 C6 C7 -179.6(3) . . . . ?
C5 C6 C7 K1 -70.2(3) . . . 2_757 ?
C5 C6 C7 C8 -157.9(3) . . . . ?
C5 C6 C7 C9 26.1(5) . . . . ?
C6 C1 C2 C3 -4.7(4) . . . . ?
C6 C1 B1 C8 -23.2(3) . . . . ?
C6 C1 B1 C10 -149.0(2) . . . . ?
C6 C1 B1 C19 87.2(3) . . . . ?
C6 C7 C8 K1 93.2(2) . . . 2_757 ?
C6 C7 C8 C9 -174.8(2) . . . 2_757 ?
C6 C7 C8 B1 -37.4(3) . . . . ?
C6 C7 C9 K1 -97.0(3) . . . 2_757 ?
C6 C7 C9 C8 173.9(3) . . . 2_757 ?
C7 C8 B1 C1 34.7(3) . . . . ?
C7 C8 B1 C10 148.8(3) . . . . ?
C7 C8 B1 C19 -85.4(3) . . . . ?
C8 C7 C9 K1 87.8(3) . . . 2_757 ?
C8 C7 C9 C8 -1.4(5) . . . 2_757 ?
C9 C7 C8 K1 -90.8(3) . . . 2_757 ?
C9 C7 C8 C9 1.2(5) . . . 2_757 ?
C9 C7 C8 B1 138.6(3) . . . . ?
C9 C8 B1 C1 161.8(3) 2_757 . . . ?
C9 C8 B1 C10 -84.0(4) 2_757 . . . ?
C9 C8 B1 C19 41.7(4) 2_757 . . . ?
C10 C11 C12 C13 1.9(5) . . . . ?
C11 C10 C15 C14 0.1(4) . . . . ?
C11 C10 C15 C18 177.3(3) . . . . ?
C11 C10 B1 C1 103.2(3) . . . . ?
C11 C10 B1 C8 -3.8(5) . . . . ?
C11 C10 B1 C19 -128.1(3) . . . . ?
C11 C12 C13 C14 -0.1(5) . . . . ?
C11 C12 C13 C17 -179.7(3) . . . . ?
C12 C13 C14 C15 -1.8(5) . . . . ?
C13 C14 C15 C10 1.8(5) . . . . ?
C13 C14 C15 C18 -175.6(3) . . . . ?
C15 C10 C11 C12 -1.8(4) . . . . ?
C15 C10 C11 C16 179.3(3) . . . . ?
C15 C10 B1 C1 -75.7(3) . . . . ?
C15 C10 B1 C8 177.2(3) . . . . ?
C15 C10 B1 C19 53.0(3) . . . . ?
C16 C11 C12 C13 -179.2(3) . . . . ?
C17 C13 C14 C15 177.8(3) . . . . ?
C19 C20 C21 K1 -68.8(3) . . . . ?
C19 C20 C21 C22 -0.1(5) . . . . ?
C20 C19 C24 K1 64.2(2) . . . . ?
C20 C19 C24 C23 -1.6(4) . . . . ?
C20 C19 C24 C27 178.6(3) . . . . ?
C20 C19 B1 C1 172.3(3) . . . . ?
C20 C19 B1 C8 -84.2(3) . . . . ?
C20 C19 B1 C10 49.2(3) . . . . ?
C20 C21 C22 K1 -68.0(3) . . . . ?
C20 C21 C22 C23 -1.2(5) . . . . ?
C20 C21 C22 C26 179.7(3) . . . . ?
C21 C22 C23 K1 -65.9(3) . . . . ?
C21 C22 C23 C24 1.2(5) . . . . ?
C22 C23 C24 K1 -66.9(3) . . . . ?
C22 C23 C24 C19 0.3(5) . . . . ?
C22 C23 C24 C27 -179.9(3) . . . . ?
C24 C19 C20 K1 -65.1(2) . . . . ?
C24 C19 C20 C21 1.5(4) . . . . ?
C24 C19 C20 C25 -179.8(3) . . . . ?
C24 C19 B1 C1 -6.5(4) . . . . ?
C24 C19 B1 C8 97.0(3) . . . . ?
C24 C19 B1 C10 -129.6(3) . . . . ?
C25 C20 C21 K1 112.5(2) . . . . ?
C25 C20 C21 C22 -178.9(3) . . . . ?
C26 C22 C23 K1 113.1(3) . . . . ?
C26 C22 C23 C24 -179.8(3) . . . . ?
C28 O1 C31 C30 -19.1(5) . . . . ?
C28 C29 C30 C31 -7.3(7) . . . . ?
C29 C30 C31 O1 16.2(6) . . . . ?
C31 O1 C28 C29 15.0(6) . . . . ?
C32 O2 C35 C34 8.6(6) . . . . ?
C32 C33 C34 C35 32.6(6) . . . . ?
C33 C34 C35 O2 -26.0(6) . . . . ?
C35 O2 C32 C33 12.4(6) . . . . ?
B1 C1 C2 C3 176.1(3) . . . . ?
B1 C1 C6 K1 68.7(3) . . . 2_757 ?
B1 C1 C6 C5 -176.1(3) . . . . ?
B1 C1 C6 C7 2.8(3) . . . . ?
B1 C10 C11 C12 179.2(3) . . . . ?
B1 C10 C11 C16 0.4(5) . . . . ?
B1 C10 C15 C14 179.1(3) . . . . ?
B1 C10 C15 C18 -3.6(4) . . . . ?
B1 C19 C20 K1 115.9(2) . . . . ?
B1 C19 C20 C21 -177.4(3) . . . . ?
B1 C19 C20 C25 1.2(4) . . . . ?
B1 C19 C24 K1 -116.9(3) . . . . ?
B1 C19 C24 C23 177.2(3) . . . . ?
B1 C19 C24 C27 -2.5(5) . . . . ?
O3 C36 C37 C38 27.0(7) . . . . ?
C36 O3 C39 C38 -5.9(7) . . . . ?
C36 C37 C38 C39 -30.4(7) . . . . ?
C37 C38 C39 O3 22.3(7) . . . . ?
C39 O3 C36 C37 -13.3(7) . . . . ?

_olex2_date_sample_data_collection 2016-11-14
_olex2_submission_special_instructions 'No special instructions were received'
