# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_8a
_database_code_depnum_ccdc_archive 'CCDC 1557235'
_audit_update_record             
;
2017-06-20 deposited with the CCDC.
2017-07-20 downloaded from the CCDC.
;
_audit_creation_date             2016-03-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C48 H70 Li2 O3 P2'
_chemical_formula_sum            'C48 H70 Li2 O3 P2'
_chemical_formula_weight         770.86
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H70 Li2 O3 P2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.0982(2)
_cell_length_b                   15.7006(3)
_cell_length_c                   24.9514(6)
_cell_angle_alpha                90
_cell_angle_beta                 102.271(2)
_cell_angle_gamma                90
_cell_volume                     4631.21(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7258
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      66.5870
_cell_measurement_theta_min      3.2930
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.127
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 -1 0.0341
1 0 -1 0.1116
-1 -1 2 0.1045
-1 1 1 0.1163
1 -1 -1 0.1003
0 0 -1 0.0404
1 0 2 0.0909
-1 0 -2 0.1059
1 1 -2 0.0975
0 -1 2 0.0453
0 1 -2 0.0453
0 1 1 0.0451
0 0 1 0.0404

_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0029 -1.0015 -0.9994 0.0980 0.0580 0.0263
1.0011 -0.0025 -1.0058 -0.0147 0.0039 0.1315
-1.0021 -0.9991 2.0093 0.1119 -0.0687 -0.1359
-0.9992 1.0040 1.0037 -0.0830 -0.0005 -0.1424
0.9992 -1.0040 -1.0037 0.0830 0.0005 0.1424
-0.0009 0.0000 -1.0015 0.0004 0.0614 0.0154
1.0040 -0.0026 1.9987 -0.0157 -0.1804 0.0854
-1.0040 0.0026 -1.9987 0.0157 0.1804 -0.0854
1.0021 0.9991 -2.0093 -0.1119 0.0687 0.1359
-0.0001 -1.0016 2.0050 0.0969 -0.1262 -0.0198
0.0001 1.0016 -2.0050 -0.0969 0.1262 0.0198
0.0029 1.0015 0.9994 -0.0980 -0.0580 -0.0263
0.0009 -0.0000 1.0015 -0.0004 -0.0614 -0.0154

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            33402
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.944
_diffrn_reflns_theta_min         3.348
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3968
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     12.00 116.00   1.00   10.00    --   41.59  57.00-150.00  104
  2  ω     15.00 117.00   1.00   10.00    --   41.59  38.00 -30.00  102
  3  ω     -3.00  96.00   1.00   10.00    --   41.59-125.00-180.00   99
  4  ω      9.00 133.00   1.00   40.00    --   93.50 -92.00  42.36  124
  5  ω     29.00  82.00   1.00   40.00    --   93.50 -94.00 -30.00   53
  6  ω     24.00  63.00   1.00   40.00    --   93.50 -30.00 -60.00   39
  7  ω     70.00 124.00   1.00   40.00    --   93.50 -92.00 105.03   54
  8  ω     12.00  38.00   1.00   40.00    --   93.50 -94.00 -60.00   26
  9  ω     54.00  80.00   1.00   40.00    --   93.50 -94.00 -60.00   26
 10  ω     49.00  95.00   1.00   40.00    --   93.50-125.00 120.00   46
 11  ω     29.00  66.00   1.00   40.00    --   93.50 -94.00 -90.00   37
 12  ω     88.00 114.00   1.00   40.00    --   93.50 -30.00 -60.00   26
 13  ω     10.00  82.00   1.00   40.00    --   93.50 -94.00 150.00   72
 14  ω     64.00 170.00   1.00   40.00    --   93.50  30.00-120.00  106
 15  ω     23.00  58.00   1.00   40.00    --   93.50 -92.00 105.03   35
 16  ω     27.00  72.00   1.00   40.00    --   93.50 -45.00 120.00   45
 17  ω     86.00 121.00   1.00   40.00    --   93.50 -45.00 120.00   35
 18  ω     46.00  72.00   1.00   40.00    --   93.50  15.00 -30.00   26
 19  ω    122.00 152.00   1.00   40.00    --   93.50  15.00 -30.00   30
 20  ω     50.00 128.00   1.00   40.00    --   93.50 -93.00 179.27   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0152333000
_diffrn_orient_matrix_UB_12      -0.0974509000
_diffrn_orient_matrix_UB_13      -0.0003497000
_diffrn_orient_matrix_UB_21      -0.0577001000
_diffrn_orient_matrix_UB_22      0.0033611000
_diffrn_orient_matrix_UB_23      -0.0612840000
_diffrn_orient_matrix_UB_31      0.1157980000
_diffrn_orient_matrix_UB_32      -0.0111601000
_diffrn_orient_matrix_UB_33      -0.0154364000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6035
_reflns_number_total             8211
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         8211
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0442
_refine_ls_restrained_S_all      1.012
_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)+(0.0499P)²+0.5205P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1141
_refine_special_details          
;
One of the tetrahydrofuran molecules has been 
modelled with one atom disordered over two sites. 
The occupancies of the two parts were allowed to 
refine with isotropic atom treatment. Upon 
convergence, the occupancies were fixed before 
anisotropy was introduced into the model. The ADPs 
of the disordered atoms were constrained using the 
EADP card and the geometry was restrained to be 
consistent with THF using the SADI card. The 
hydrogen atoms of one methyl group have also been 
modelled as disordered as disordered over two parts. 
As all hydrogen atoms were refined isotropically, it 
was not necessary to fix the occupancies of these 
two parts.
;
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C39B-C38 \\sim C39A-C38
 with sigma of 0.02
 C40-C39B \\sim C40-C39A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C39A) = Uanis(C39B)
4. Others
 Sof(H8BD)=Sof(H8BE)=Sof(H8BF)=1-FVAR(1)
 Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=FVAR(1)
 Fixed Sof: H38A(0.81767) H38B(0.81767) H38C(0.18233) H38D(0.18233)
 C39A(0.81767) H39A(0.81767) H39B(0.81767) C39B(0.18233) H39C(0.18233)
 H39D(0.18233) H40A(0.81767) H40B(0.81767) H40C(0.18233) H40D(0.18233)
5.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C38(H38C,H38D), C39A(H39A,H39B), C39B(H39C,
 H39D), C40(H40A,H40B), C40(H40C,H40D), C41(H41A,H41B), C42(H42A,H42B),
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C47(H47A,H47B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C14(H14), C21(H21), C23(H23), C30(H30), C32(H32)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8AA,H8AB,H8AC), C8(H8BD,H8BE,H8BF), C9(H9A,H9B,H9C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C)
;
_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
P1 P 0.66903(4) 0.42792(3) 0.37666(2) 0.02822(13) Uani 1 1 d . . . . .
P2 P 0.76339(4) 0.18478(3) 0.39102(2) 0.02924(13) Uani 1 1 d . . . . .
O1 O 0.54000(11) 0.28983(10) 0.25775(6) 0.0415(4) Uani 1 1 d . . . . .
O2 O 0.79158(12) 0.28953(10) 0.26405(6) 0.0401(4) Uani 1 1 d . . . . .
O3 O 0.77744(14) 0.32185(11) 0.52514(7) 0.0486(4) Uani 1 1 d . . . . .
C1 C 0.51484(15) 0.43888(12) 0.36646(8) 0.0280(4) Uani 1 1 d . . . . .
C2 C 0.45333(16) 0.50178(13) 0.33211(8) 0.0315(4) Uani 1 1 d . . . . .
C3 C 0.33544(17) 0.50145(15) 0.32134(9) 0.0373(5) Uani 1 1 d . . . . .
H3 H 0.2966 0.5436 0.2987 0.045 Uiso 1 1 calc R . . . .
C4 C 0.27376(16) 0.44116(15) 0.34280(9) 0.0376(5) Uani 1 1 d . . . . .
C5 C 0.33431(16) 0.38047(14) 0.37741(9) 0.0347(5) Uani 1 1 d . . . . .
H5 H 0.2949 0.3400 0.3931 0.042 Uiso 1 1 calc R . . . .
C6 C 0.45228(16) 0.37794(13) 0.38957(8) 0.0298(4) Uani 1 1 d . . . . .
C7 C 0.51018(18) 0.56974(15) 0.30514(10) 0.0406(5) Uani 1 1 d . . . . .
H7A H 0.5421 0.6119 0.3318 0.061 Uiso 1 1 calc GR . . . .
H7B H 0.4556 0.5961 0.2764 0.061 Uiso 1 1 calc GR . . . .
H7C H 0.5691 0.5446 0.2900 0.061 Uiso 1 1 calc GR . . . .
C8 C 0.14602(18) 0.44076(19) 0.32838(12) 0.0535(7) Uani 1 1 d . . . . .
H8AA H 0.1180 0.4934 0.3399 0.080 Uiso 0.47(3) 1 calc GR . P A 1
H8AB H 0.1183 0.3942 0.3467 0.080 Uiso 0.47(3) 1 calc GR . P A 1
H8AC H 0.1206 0.4344 0.2894 0.080 Uiso 0.47(3) 1 calc GR . P A 1
H8BD H 0.1173 0.4487 0.3611 0.080 Uiso 0.53(3) 1 calc GR . P A 2
H8BE H 0.1199 0.3872 0.3119 0.080 Uiso 0.53(3) 1 calc GR . P A 2
H8BF H 0.1197 0.4861 0.3031 0.080 Uiso 0.53(3) 1 calc GR . P A 2
C9 C 0.50945(18) 0.31018(14) 0.42763(10) 0.0385(5) Uani 1 1 d . . . . .
H9A H 0.5526 0.2742 0.4087 0.058 Uiso 1 1 calc GR . . . .
H9B H 0.4535 0.2767 0.4402 0.058 Uiso 1 1 calc GR . . . .
H9C H 0.5589 0.3361 0.4585 0.058 Uiso 1 1 calc GR . . . .
C10 C 0.72357(15) 0.53554(13) 0.39485(8) 0.0291(4) Uani 1 1 d . . . . .
C11 C 0.80290(15) 0.57312(14) 0.36783(9) 0.0338(5) Uani 1 1 d . . . . .
C12 C 0.84330(16) 0.65507(15) 0.38227(10) 0.0410(5) Uani 1 1 d . . . . .
H12 H 0.8944 0.6792 0.3636 0.049 Uiso 1 1 calc R . . . .
C13 C 0.81031(18) 0.70204(15) 0.42331(11) 0.0443(6) Uani 1 1 d . . . . .
C14 C 0.73477(17) 0.66379(15) 0.45055(10) 0.0413(5) Uani 1 1 d . . . . .
H14 H 0.7122 0.6937 0.4786 0.050 Uiso 1 1 calc R . . . .
C15 C 0.69136(16) 0.58245(13) 0.43763(9) 0.0333(5) Uani 1 1 d . . . . .
C16 C 0.84359(18) 0.52702(16) 0.32296(11) 0.0459(6) Uani 1 1 d . . . . .
H16A H 0.8866 0.4779 0.3379 0.069 Uiso 1 1 calc GR . . . .
H16B H 0.8904 0.5643 0.3069 0.069 Uiso 1 1 calc GR . . . .
H16C H 0.7798 0.5093 0.2954 0.069 Uiso 1 1 calc GR . . . .
C17 C 0.8528(2) 0.79099(17) 0.43712(14) 0.0618(8) Uani 1 1 d . . . . .
H17A H 0.9101 0.8043 0.4171 0.093 Uiso 1 1 calc GR . . . .
H17B H 0.8842 0.7949 0.4758 0.093 Uiso 1 1 calc GR . . . .
H17C H 0.7913 0.8305 0.4274 0.093 Uiso 1 1 calc GR . . . .
C18 C 0.61194(18) 0.54582(16) 0.47077(10) 0.0430(5) Uani 1 1 d . . . . .
H18A H 0.5356 0.5491 0.4499 0.064 Uiso 1 1 calc GR . . . .
H18B H 0.6183 0.5777 0.5041 0.064 Uiso 1 1 calc GR . . . .
H18C H 0.6313 0.4874 0.4794 0.064 Uiso 1 1 calc GR . . . .
C19 C 0.90281(15) 0.15204(13) 0.37998(8) 0.0300(4) Uani 1 1 d . . . . .
C20 C 0.92111(16) 0.07258(14) 0.35632(9) 0.0337(5) Uani 1 1 d . . . . .
C21 C 1.02732(17) 0.05359(16) 0.34597(10) 0.0424(5) Uani 1 1 d . . . . .
H21 H 1.0384 0.0007 0.3311 0.051 Uiso 1 1 calc R . . . .
C22 C 1.11675(17) 0.11033(18) 0.35692(10) 0.0480(6) Uani 1 1 d . . . . .
C23 C 1.09790(17) 0.18781(17) 0.37964(10) 0.0457(6) Uani 1 1 d . . . . .
H23 H 1.1569 0.2269 0.3872 0.055 Uiso 1 1 calc R . . . .
C24 C 0.99414(16) 0.20991(14) 0.39169(9) 0.0357(5) Uani 1 1 d . . . . .
C25 C 0.82915(18) 0.00691(15) 0.34069(10) 0.0417(5) Uani 1 1 d . . . . .
H25A H 0.8172 -0.0214 0.3731 0.062 Uiso 1 1 calc GR . . . .
H25B H 0.8512 -0.0341 0.3164 0.062 Uiso 1 1 calc GR . . . .
H25C H 0.7604 0.0343 0.3226 0.062 Uiso 1 1 calc GR . . . .
C26 C 1.2298(2) 0.0880(2) 0.34386(14) 0.0718(9) Uani 1 1 d . . . . .
H26A H 1.2655 0.0442 0.3684 0.108 Uiso 1 1 calc GR . . . .
H26B H 1.2771 0.1376 0.3481 0.108 Uiso 1 1 calc GR . . . .
H26C H 1.2184 0.0679 0.3067 0.108 Uiso 1 1 calc GR . . . .
C27 C 0.98321(19) 0.29429(15) 0.41812(11) 0.0464(6) Uani 1 1 d . . . . .
H27A H 0.9285 0.3286 0.3940 0.070 Uiso 1 1 calc GR . . . .
H27B H 1.0551 0.3227 0.4254 0.070 Uiso 1 1 calc GR . . . .
H27C H 0.9590 0.2856 0.4520 0.070 Uiso 1 1 calc GR . . . .
C28 C 0.71453(15) 0.09252(12) 0.42515(9) 0.0295(4) Uani 1 1 d . . . . .
C29 C 0.60678(15) 0.05618(13) 0.40463(9) 0.0323(5) Uani 1 1 d . . . . .
C30 C 0.57118(18) -0.01298(14) 0.43156(10) 0.0396(5) Uani 1 1 d . . . . .
H30 H 0.4995 -0.0353 0.4181 0.048 Uiso 1 1 calc R . . . .
C31 C 0.63795(19) -0.04976(14) 0.47751(10) 0.0412(5) Uani 1 1 d . . . . .
C32 C 0.74257(19) -0.01353(14) 0.49784(10) 0.0399(5) Uani 1 1 d . . . . .
H32 H 0.7886 -0.0369 0.5290 0.048 Uiso 1 1 calc R . . . .
C33 C 0.78153(17) 0.05683(13) 0.47328(9) 0.0333(5) Uani 1 1 d . . . . .
C34 C 0.53050(16) 0.08934(16) 0.35363(10) 0.0414(5) Uani 1 1 d . . . . .
H34A H 0.4964 0.1417 0.3617 0.062 Uiso 1 1 calc GR . . . .
H34B H 0.4725 0.0482 0.3403 0.062 Uiso 1 1 calc GR . . . .
H34C H 0.5738 0.0994 0.3261 0.062 Uiso 1 1 calc GR . . . .
C35 C 0.5980(2) -0.12692(16) 0.50396(12) 0.0560(7) Uani 1 1 d . . . . .
H35A H 0.5307 -0.1129 0.5167 0.084 Uiso 1 1 calc GR . . . .
H35B H 0.6559 -0.1448 0.5344 0.084 Uiso 1 1 calc GR . . . .
H35C H 0.5818 -0.1722 0.4776 0.084 Uiso 1 1 calc GR . . . .
C36 C 0.89607(18) 0.09198(15) 0.49949(10) 0.0431(5) Uani 1 1 d . . . . .
H36A H 0.9502 0.0751 0.4784 0.065 Uiso 1 1 calc GR . . . .
H36B H 0.9187 0.0702 0.5361 0.065 Uiso 1 1 calc GR . . . .
H36C H 0.8923 0.1530 0.5006 0.065 Uiso 1 1 calc GR . . . .
C37 C 0.42812(17) 0.26252(16) 0.26318(10) 0.0407(5) Uani 1 1 d . . . . .
H37A H 0.4161 0.2762 0.2994 0.049 Uiso 1 1 calc R . . . .
H37B H 0.4198 0.2015 0.2576 0.049 Uiso 1 1 calc R . . . .
C38 C 0.3451(2) 0.30922(19) 0.22027(13) 0.0604(7) Uani 1 1 d D . . . .
H38A H 0.2817 0.2730 0.2044 0.072 Uiso 0.8177 1 calc R . P B 1
H38B H 0.3170 0.3595 0.2355 0.072 Uiso 0.8177 1 calc R . P B 1
H38C H 0.3057 0.2699 0.1927 0.072 Uiso 0.1823 1 calc R . P C 2
H38D H 0.2899 0.3385 0.2366 0.072 Uiso 0.1823 1 calc R . P C 2
C39A C 0.4108(3) 0.3329(2) 0.17859(14) 0.0551(9) Uani 0.8177 1 d D . P D 1
H39A H 0.3798 0.3832 0.1583 0.066 Uiso 0.8177 1 calc R . P D 1
H39B H 0.4129 0.2865 0.1531 0.066 Uiso 0.8177 1 calc R . P D 1
C39B C 0.4117(10) 0.3713(10) 0.1953(7) 0.0551(9) Uani 0.1823 1 d D . P D 2
H39C H 0.3909 0.3679 0.1556 0.066 Uiso 0.1823 1 calc R . P D 2
H39D H 0.3974 0.4288 0.2063 0.066 Uiso 0.1823 1 calc R . P D 2
C40 C 0.5273(2) 0.3503(2) 0.21390(12) 0.0592(7) Uani 1 1 d D . . . .
H40A H 0.5855 0.3423 0.1929 0.071 Uiso 0.8177 1 calc R . P D 1
H40B H 0.5320 0.4080 0.2280 0.071 Uiso 0.8177 1 calc R . P D 1
H40C H 0.5701 0.4013 0.2266 0.071 Uiso 0.1823 1 calc R . P D 2
H40D H 0.5568 0.3264 0.1839 0.071 Uiso 0.1823 1 calc R . P D 2
C41 C 0.7916(2) 0.20650(15) 0.23977(10) 0.0444(5) Uani 1 1 d . . . . .
H41A H 0.7319 0.2021 0.2071 0.053 Uiso 1 1 calc R . . . .
H41B H 0.7803 0.1627 0.2655 0.053 Uiso 1 1 calc R . . . .
C42 C 0.9057(2) 0.19695(19) 0.22551(12) 0.0602(7) Uani 1 1 d . . . . .
H42A H 0.9599 0.1719 0.2557 0.072 Uiso 1 1 calc R . . . .
H42B H 0.9010 0.1619 0.1931 0.072 Uiso 1 1 calc R . . . .
C43 C 0.9375(3) 0.2869(2) 0.21508(14) 0.0702(9) Uani 1 1 d . . . . .
H43A H 1.0189 0.2945 0.2237 0.084 Uiso 1 1 calc R . . . .
H43B H 0.9081 0.3032 0.1772 0.084 Uiso 1 1 calc R . . . .
C44 C 0.8827(3) 0.3368(2) 0.25316(16) 0.0795(11) Uani 1 1 d . . . . .
H44A H 0.9370 0.3481 0.2871 0.095 Uiso 1 1 calc R . . . .
H44B H 0.8560 0.3910 0.2366 0.095 Uiso 1 1 calc R . . . .
C45 C 0.8340(2) 0.3870(2) 0.56036(11) 0.0614(7) Uani 1 1 d . . . . .
H45A H 0.8840 0.3615 0.5918 0.074 Uiso 1 1 calc R . . . .
H45B H 0.7789 0.4217 0.5735 0.074 Uiso 1 1 calc R . . . .
C46 C 0.9010(2) 0.44163(19) 0.52989(12) 0.0586(7) Uani 1 1 d . . . . .
H46A H 0.8523 0.4634 0.4973 0.088 Uiso 1 1 calc GR . . . .
H46B H 0.9601 0.4083 0.5200 0.088 Uiso 1 1 calc GR . . . .
H46C H 0.9337 0.4882 0.5528 0.088 Uiso 1 1 calc GR . . . .
C47 C 0.7331(3) 0.2537(2) 0.55306(12) 0.0622(7) Uani 1 1 d . . . . .
H47A H 0.7943 0.2296 0.5804 0.075 Uiso 1 1 calc R . . . .
H47B H 0.7045 0.2093 0.5268 0.075 Uiso 1 1 calc R . . . .
C48 C 0.6399(3) 0.2812(2) 0.58079(12) 0.0715(9) Uani 1 1 d . . . . .
H48A H 0.5782 0.3040 0.5539 0.107 Uiso 1 1 calc GR . . . .
H48B H 0.6681 0.3241 0.6077 0.107 Uiso 1 1 calc GR . . . .
H48C H 0.6141 0.2331 0.5984 0.107 Uiso 1 1 calc GR . . . .
Li1 Li 0.6829(3) 0.2990(2) 0.31238(15) 0.0365(8) Uani 1 1 d . . . . .
Li2 Li 0.7539(3) 0.3177(2) 0.44636(15) 0.0387(8) 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
P1 C1 1.8365(18) . ?
P1 C10 1.836(2) . ?
P1 Li1 2.609(4) . ?
P1 Li2 2.513(4) . ?
P2 C19 1.8391(19) . ?
P2 C28 1.840(2) . ?
P2 Li1 2.684(4) . ?
P2 Li2 2.518(4) . ?
O1 C37 1.453(3) . ?
O1 C40 1.432(3) . ?
O1 Li1 1.966(4) . ?
O2 C41 1.438(3) . ?
O2 C44 1.403(3) . ?
O2 Li1 1.970(4) . ?
O3 C45 1.426(3) . ?
O3 C47 1.441(3) . ?
O3 Li2 1.926(4) . ?
C1 C2 1.412(3) . ?
C1 C6 1.416(3) . ?
C2 C3 1.394(3) . ?
C2 C7 1.504(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.382(3) . ?
C4 C5 1.386(3) . ?
C4 C8 1.510(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.395(3) . ?
C6 C9 1.494(3) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8AA 0.9600 . ?
C8 H8AB 0.9600 . ?
C8 H8AC 0.9600 . ?
C8 H8BD 0.9600 . ?
C8 H8BE 0.9600 . ?
C8 H8BF 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.414(3) . ?
C10 C15 1.418(3) . ?
C11 C12 1.396(3) . ?
C11 C16 1.501(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.388(4) . ?
C13 C14 1.386(3) . ?
C13 C17 1.503(3) . ?
C14 H14 0.9300 . ?
C14 C15 1.392(3) . ?
C15 C18 1.508(3) . ?
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 1.418(3) . ?
C19 C24 1.412(3) . ?
C20 C21 1.396(3) . ?
C20 C25 1.506(3) . ?
C21 H21 0.9300 . ?
C21 C22 1.383(3) . ?
C22 C23 1.381(4) . ?
C22 C26 1.513(3) . ?
C23 H23 0.9300 . ?
C23 C24 1.395(3) . ?
C24 C27 1.498(3) . ?
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 C29 1.415(3) . ?
C28 C33 1.414(3) . ?
C29 C30 1.393(3) . ?
C29 C34 1.498(3) . ?
C30 H30 0.9300 . ?
C30 C31 1.381(3) . ?
C31 C32 1.382(3) . ?
C31 C35 1.508(3) . ?
C32 H32 0.9300 . ?
C32 C33 1.393(3) . ?
C33 C36 1.506(3) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 C38 1.495(3) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 H38C 0.9700 . ?
C38 H38D 0.9700 . ?
C38 C39A 1.484(5) . ?
C38 C39B 1.484(14) . ?
C39A H39A 0.9700 . ?
C39A H39B 0.9700 . ?
C39A C40 1.520(4) . ?
C39B H39C 0.9700 . ?
C39B H39D 0.9700 . ?
C39B C40 1.416(13) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 H40C 0.9700 . ?
C40 H40D 0.9700 . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 C42 1.504(3) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C42 C43 1.501(4) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C43 C44 1.491(4) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C45 C46 1.494(4) . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C47 C48 1.506(4) . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
Li1 Li2 3.283(5) . ?

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
C1 P1 Li1 100.57(9) . . ?
C1 P1 Li2 114.45(10) . . ?
C10 P1 C1 104.43(9) . . ?
C10 P1 Li1 143.05(10) . . ?
C10 P1 Li2 112.98(11) . . ?
Li2 P1 Li1 79.69(12) . . ?
C19 P2 C28 104.14(9) . . ?
C19 P2 Li1 106.22(10) . . ?
C19 P2 Li2 117.64(11) . . ?
C28 P2 Li1 139.64(10) . . ?
C28 P2 Li2 109.99(11) . . ?
Li2 P2 Li1 78.18(12) . . ?
C37 O1 Li1 131.00(17) . . ?
C40 O1 C37 108.43(16) . . ?
C40 O1 Li1 114.62(17) . . ?
C41 O2 Li1 112.77(17) . . ?
C44 O2 C41 109.12(18) . . ?
C44 O2 Li1 137.1(2) . . ?
C45 O3 C47 114.5(2) . . ?
C45 O3 Li2 126.92(19) . . ?
C47 O3 Li2 118.6(2) . . ?
C2 C1 P1 122.58(14) . . ?
C2 C1 C6 117.48(17) . . ?
C6 C1 P1 119.69(15) . . ?
C1 C2 C7 122.41(17) . . ?
C3 C2 C1 120.01(19) . . ?
C3 C2 C7 117.57(19) . . ?
C2 C3 H3 118.6 . . ?
C4 C3 C2 122.9(2) . . ?
C4 C3 H3 118.6 . . ?
C3 C4 C5 117.06(18) . . ?
C3 C4 C8 121.3(2) . . ?
C5 C4 C8 121.6(2) . . ?
C4 C5 H5 118.8 . . ?
C4 C5 C6 122.39(19) . . ?
C6 C5 H5 118.8 . . ?
C1 C6 C9 121.63(17) . . ?
C5 C6 C1 120.18(19) . . ?
C5 C6 C9 118.19(18) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8AA 109.5 . . ?
C4 C8 H8AB 109.5 . . ?
C4 C8 H8AC 109.5 . . ?
C4 C8 H8BD 109.5 . . ?
C4 C8 H8BE 109.5 . . ?
C4 C8 H8BF 109.5 . . ?
H8AA C8 H8AB 109.5 . . ?
H8AA C8 H8AC 109.5 . . ?
H8AB C8 H8AC 109.5 . . ?
H8BD C8 H8BE 109.5 . . ?
H8BD C8 H8BF 109.5 . . ?
H8BE C8 H8BF 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 P1 120.73(16) . . ?
C11 C10 C15 117.73(19) . . ?
C15 C10 P1 121.50(15) . . ?
C10 C11 C16 121.19(19) . . ?
C12 C11 C10 119.8(2) . . ?
C12 C11 C16 118.98(19) . . ?
C11 C12 H12 118.6 . . ?
C13 C12 C11 122.7(2) . . ?
C13 C12 H12 118.6 . . ?
C12 C13 C17 121.7(2) . . ?
C14 C13 C12 117.0(2) . . ?
C14 C13 C17 121.3(2) . . ?
C13 C14 H14 118.7 . . ?
C13 C14 C15 122.6(2) . . ?
C15 C14 H14 118.7 . . ?
C10 C15 C18 121.58(19) . . ?
C14 C15 C10 120.0(2) . . ?
C14 C15 C18 118.4(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 P2 122.53(14) . . ?
C24 C19 P2 119.43(16) . . ?
C24 C19 C20 117.89(17) . . ?
C19 C20 C25 122.56(17) . . ?
C21 C20 C19 119.77(19) . . ?
C21 C20 C25 117.7(2) . . ?
C20 C21 H21 118.7 . . ?
C22 C21 C20 122.6(2) . . ?
C22 C21 H21 118.7 . . ?
C21 C22 C26 120.9(3) . . ?
C23 C22 C21 117.25(19) . . ?
C23 C22 C26 121.9(2) . . ?
C22 C23 H23 118.6 . . ?
C22 C23 C24 122.8(2) . . ?
C24 C23 H23 118.6 . . ?
C19 C24 C27 121.44(18) . . ?
C23 C24 C19 119.7(2) . . ?
C23 C24 C27 118.84(19) . . ?
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 . . ?
C29 C28 P2 120.77(16) . . ?
C33 C28 P2 121.50(15) . . ?
C33 C28 C29 117.72(18) . . ?
C28 C29 C34 121.41(18) . . ?
C30 C29 C28 119.7(2) . . ?
C30 C29 C34 118.90(18) . . ?
C29 C30 H30 118.6 . . ?
C31 C30 C29 122.7(2) . . ?
C31 C30 H30 118.6 . . ?
C30 C31 C32 117.5(2) . . ?
C30 C31 C35 120.9(2) . . ?
C32 C31 C35 121.6(2) . . ?
C31 C32 H32 118.9 . . ?
C31 C32 C33 122.3(2) . . ?
C33 C32 H32 118.9 . . ?
C28 C33 C36 122.15(18) . . ?
C32 C33 C28 120.09(19) . . ?
C32 C33 C36 117.8(2) . . ?
C29 C34 H34A 109.5 . . ?
C29 C34 H34B 109.5 . . ?
C29 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C31 C35 H35A 109.5 . . ?
C31 C35 H35B 109.5 . . ?
C31 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O1 C37 H37A 110.4 . . ?
O1 C37 H37B 110.4 . . ?
O1 C37 C38 106.6(2) . . ?
H37A C37 H37B 108.6 . . ?
C38 C37 H37A 110.4 . . ?
C38 C37 H37B 110.4 . . ?
C37 C38 H38A 110.9 . . ?
C37 C38 H38B 110.9 . . ?
C37 C38 H38C 110.5 . . ?
C37 C38 H38D 110.5 . . ?
H38A C38 H38B 108.9 . . ?
H38C C38 H38D 108.7 . . ?
C39A C38 C37 104.3(2) . . ?
C39A C38 H38A 110.9 . . ?
C39A C38 H38B 110.9 . . ?
C39B C38 C37 106.3(5) . . ?
C39B C38 H38C 110.5 . . ?
C39B C38 H38D 110.5 . . ?
C38 C39A H39A 111.4 . . ?
C38 C39A H39B 111.4 . . ?
C38 C39A C40 102.0(2) . . ?
H39A C39A H39B 109.2 . . ?
C40 C39A H39A 111.4 . . ?
C40 C39A H39B 111.4 . . ?
C38 C39B H39C 110.3 . . ?
C38 C39B H39D 110.3 . . ?
H39C C39B H39D 108.5 . . ?
C40 C39B C38 107.2(9) . . ?
C40 C39B H39C 110.3 . . ?
C40 C39B H39D 110.3 . . ?
O1 C40 C39A 105.0(2) . . ?
O1 C40 H40A 110.7 . . ?
O1 C40 H40B 110.7 . . ?
O1 C40 H40C 109.6 . . ?
O1 C40 H40D 109.6 . . ?
C39A C40 H40A 110.7 . . ?
C39A C40 H40B 110.7 . . ?
C39B C40 O1 110.1(6) . . ?
C39B C40 H40C 109.6 . . ?
C39B C40 H40D 109.6 . . ?
H40A C40 H40B 108.8 . . ?
H40C C40 H40D 108.2 . . ?
O2 C41 H41A 110.6 . . ?
O2 C41 H41B 110.6 . . ?
O2 C41 C42 105.84(19) . . ?
H41A C41 H41B 108.7 . . ?
C42 C41 H41A 110.6 . . ?
C42 C41 H41B 110.6 . . ?
C41 C42 H42A 111.1 . . ?
C41 C42 H42B 111.1 . . ?
H42A C42 H42B 109.1 . . ?
C43 C42 C41 103.2(2) . . ?
C43 C42 H42A 111.1 . . ?
C43 C42 H42B 111.1 . . ?
C42 C43 H43A 111.2 . . ?
C42 C43 H43B 111.2 . . ?
H43A C43 H43B 109.1 . . ?
C44 C43 C42 102.7(2) . . ?
C44 C43 H43A 111.2 . . ?
C44 C43 H43B 111.2 . . ?
O2 C44 C43 108.6(2) . . ?
O2 C44 H44A 110.0 . . ?
O2 C44 H44B 110.0 . . ?
C43 C44 H44A 110.0 . . ?
C43 C44 H44B 110.0 . . ?
H44A C44 H44B 108.4 . . ?
O3 C45 H45A 109.7 . . ?
O3 C45 H45B 109.7 . . ?
O3 C45 C46 109.9(2) . . ?
H45A C45 H45B 108.2 . . ?
C46 C45 H45A 109.7 . . ?
C46 C45 H45B 109.7 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
O3 C47 H47A 108.8 . . ?
O3 C47 H47B 108.8 . . ?
O3 C47 C48 113.6(3) . . ?
H47A C47 H47B 107.7 . . ?
C48 C47 H47A 108.8 . . ?
C48 C47 H47B 108.8 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
P1 Li1 P2 97.46(12) . . ?
P1 Li1 Li2 48.86(9) . . ?
P2 Li1 Li2 48.66(9) . . ?
O1 Li1 P1 108.75(15) . . ?
O1 Li1 P2 125.92(17) . . ?
O1 Li1 O2 99.96(17) . . ?
O1 Li1 Li2 135.55(16) . . ?
O2 Li1 P1 124.99(17) . . ?
O2 Li1 P2 102.18(14) . . ?
O2 Li1 Li2 124.46(15) . . ?
P1 Li2 P2 104.53(13) . . ?
P1 Li2 Li1 51.44(9) . . ?
P2 Li2 Li1 53.16(10) . . ?
O3 Li2 P1 129.26(18) . . ?
O3 Li2 P2 125.00(18) . . ?
O3 Li2 Li1 172.72(19) . . ?

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
P1 C1 C2 C3 173.19(17) . . . . ?
P1 C1 C2 C7 -5.6(3) . . . . ?
P1 C1 C6 C5 -173.31(16) . . . . ?
P1 C1 C6 C9 7.2(3) . . . . ?
P1 C10 C11 C12 179.97(16) . . . . ?
P1 C10 C11 C16 1.0(3) . . . . ?
P1 C10 C15 C14 179.68(16) . . . . ?
P1 C10 C15 C18 0.8(3) . . . . ?
P2 C19 C20 C21 176.13(17) . . . . ?
P2 C19 C20 C25 -2.9(3) . . . . ?
P2 C19 C24 C23 -175.31(17) . . . . ?
P2 C19 C24 C27 6.1(3) . . . . ?
P2 C28 C29 C30 -179.24(15) . . . . ?
P2 C28 C29 C34 2.1(3) . . . . ?
P2 C28 C33 C32 -179.38(16) . . . . ?
P2 C28 C33 C36 0.2(3) . . . . ?
O1 C37 C38 C39A 22.6(3) . . . . ?
O1 C37 C38 C39B -7.0(8) . . . . ?
O2 C41 C42 C43 -28.9(3) . . . . ?
C1 P1 C10 C11 -130.45(16) . . . . ?
C1 P1 C10 C15 52.01(18) . . . . ?
C1 C2 C3 C4 -0.3(3) . . . . ?
C2 C1 C6 C5 1.1(3) . . . . ?
C2 C1 C6 C9 -178.36(19) . . . . ?
C2 C3 C4 C5 1.5(3) . . . . ?
C2 C3 C4 C8 -177.5(2) . . . . ?
C3 C4 C5 C6 -1.5(3) . . . . ?
C4 C5 C6 C1 0.2(3) . . . . ?
C4 C5 C6 C9 179.7(2) . . . . ?
C6 C1 C2 C3 -1.0(3) . . . . ?
C6 C1 C2 C7 -179.9(2) . . . . ?
C7 C2 C3 C4 178.6(2) . . . . ?
C8 C4 C5 C6 177.6(2) . . . . ?
C10 P1 C1 C2 51.08(18) . . . . ?
C10 P1 C1 C6 -134.81(16) . . . . ?
C10 C11 C12 C13 1.1(3) . . . . ?
C11 C10 C15 C14 2.1(3) . . . . ?
C11 C10 C15 C18 -176.80(19) . . . . ?
C11 C12 C13 C14 0.5(3) . . . . ?
C11 C12 C13 C17 -178.5(2) . . . . ?
C12 C13 C14 C15 -0.9(3) . . . . ?
C13 C14 C15 C10 -0.4(3) . . . . ?
C13 C14 C15 C18 178.5(2) . . . . ?
C15 C10 C11 C12 -2.4(3) . . . . ?
C15 C10 C11 C16 178.61(19) . . . . ?
C16 C11 C12 C13 -179.9(2) . . . . ?
C17 C13 C14 C15 178.1(2) . . . . ?
C19 P2 C28 C29 -127.88(16) . . . . ?
C19 P2 C28 C33 53.69(18) . . . . ?
C19 C20 C21 C22 -1.3(4) . . . . ?
C20 C19 C24 C23 0.3(3) . . . . ?
C20 C19 C24 C27 -178.3(2) . . . . ?
C20 C21 C22 C23 0.9(4) . . . . ?
C20 C21 C22 C26 -178.6(2) . . . . ?
C21 C22 C23 C24 0.2(4) . . . . ?
C22 C23 C24 C19 -0.7(4) . . . . ?
C22 C23 C24 C27 177.9(2) . . . . ?
C24 C19 C20 C21 0.7(3) . . . . ?
C24 C19 C20 C25 -178.3(2) . . . . ?
C25 C20 C21 C22 177.7(2) . . . . ?
C26 C22 C23 C24 179.6(2) . . . . ?
C28 P2 C19 C20 48.91(19) . . . . ?
C28 P2 C19 C24 -135.72(17) . . . . ?
C28 C29 C30 C31 -1.5(3) . . . . ?
C29 C28 C33 C32 2.1(3) . . . . ?
C29 C28 C33 C36 -178.33(19) . . . . ?
C29 C30 C31 C32 2.2(3) . . . . ?
C29 C30 C31 C35 -177.4(2) . . . . ?
C30 C31 C32 C33 -0.7(3) . . . . ?
C31 C32 C33 C28 -1.5(3) . . . . ?
C31 C32 C33 C36 179.0(2) . . . . ?
C33 C28 C29 C30 -0.7(3) . . . . ?
C33 C28 C29 C34 -179.46(19) . . . . ?
C34 C29 C30 C31 177.3(2) . . . . ?
C35 C31 C32 C33 178.8(2) . . . . ?
C37 O1 C40 C39A -22.2(3) . . . . ?
C37 O1 C40 C39B 7.4(9) . . . . ?
C37 C38 C39A C40 -35.0(3) . . . . ?
C37 C38 C39B C40 11.4(13) . . . . ?
C38 C39A C40 O1 35.5(3) . . . . ?
C38 C39B C40 O1 -11.7(13) . . . . ?
C40 O1 C37 C38 0.1(3) . . . . ?
C41 O2 C44 C43 6.5(4) . . . . ?
C41 C42 C43 C44 31.8(3) . . . . ?
C42 C43 C44 O2 -24.4(4) . . . . ?
C44 O2 C41 C42 14.3(3) . . . . ?
C45 O3 C47 C48 65.4(3) . . . . ?
C47 O3 C45 C46 165.6(2) . . . . ?
Li1 P1 C1 C2 -101.48(18) . . . . ?
Li1 P1 C1 C6 72.63(18) . . . . ?
Li1 P1 C10 C11 0.7(3) . . . . ?
Li1 P1 C10 C15 -176.89(17) . . . . ?
Li1 P2 C19 C20 -104.17(19) . . . . ?
Li1 P2 C19 C24 71.20(19) . . . . ?
Li1 P2 C28 C29 10.0(2) . . . . ?
Li1 P2 C28 C33 -168.48(17) . . . . ?
Li1 O1 C37 C38 150.7(2) . . . . ?
Li1 O1 C40 C39A -178.2(2) . . . . ?
Li1 O1 C40 C39B -148.6(8) . . . . ?
Li1 O2 C41 C42 -156.3(2) . . . . ?
Li1 O2 C44 C43 173.7(3) . . . . ?
Li2 P1 C1 C2 175.12(17) . . . . ?
Li2 P1 C1 C6 -10.8(2) . . . . ?
Li2 P1 C10 C11 104.57(18) . . . . ?
Li2 P1 C10 C15 -72.97(18) . . . . ?
Li2 P2 C19 C20 170.91(17) . . . . ?
Li2 P2 C19 C24 -13.7(2) . . . . ?
Li2 P2 C28 C29 105.20(18) . . . . ?
Li2 P2 C28 C33 -73.23(18) . . . . ?
Li2 O3 C45 C46 -15.3(3) . . . . ?
Li2 O3 C47 C48 -113.7(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.466
_oxdiff_exptl_absorpt_empirical_full_min 0.747
####################################################################### 
# 
# 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_3c
_database_code_depnum_ccdc_archive 'CCDC 1557232'
_audit_update_record             
;
2017-06-20 deposited with the CCDC.
2017-07-20 downloaded from the CCDC.
;
_audit_creation_date             2016-11-10
_audit_creation_method           
;
Olex2 1.2
(compiled Sep  9 2016 16:03:45 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C33 H57 N3 Na P'
_chemical_formula_sum            'C33 H57 N3 Na P'
_chemical_formula_weight         549.77
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C32 H54 N3 Na1 P1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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      tetragonal
_space_group_IT_number           96
_space_group_name_H-M_alt        'P 43 21 2'
_space_group_name_Hall           'P 4nw 2abw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+3/4'
'y+1/2, -x+1/2, z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'x+1/2, -y+1/2, -z+1/4'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   12.67110(10)
_cell_length_b                   12.67110(10)
_cell_length_c                   42.8676(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6882.68(14)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    14842
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      66.6280
_cell_measurement_theta_min      3.5970
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.993
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            52251
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.892
_diffrn_reflns_theta_min         3.637
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3968
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     19.00  84.00   1.00   20.00    --   41.59 -99.00   0.00   65
  2  ω     21.00  53.00   1.00   20.00    --   41.59  38.00-180.00   32
  3  ω     15.00 116.00   1.00   20.00    --   41.59  57.00-150.00  101
  4  ω     75.00 110.00   1.00   80.00    --   93.50 -93.00-139.00   35
  5  ω     66.00 114.00   1.00   80.00    --   93.50  45.00-150.00   48
  6  ω     15.00 100.00   1.00   80.00    --   93.50 -77.00 -60.00   85
  7  ω     24.00 121.00   1.00   80.00    --   93.50 -45.00  30.00   97
  8  ω     55.00 124.00   1.00   80.00    --   93.50 -61.00 -60.00   69
  9  ω     63.00 157.00   1.00   80.00    --   93.50  30.00 150.00   94
 10  ω      8.00 129.00   1.00   80.00    --   93.50 -91.00 -63.99  121
 11  ω     32.00  94.00   1.00   80.00    --   93.50 -45.00 -60.00   62
 12  ω     17.00  91.00   1.00   80.00    --   93.50-115.00 -73.00   74
 13  ω     94.00 170.00   1.00   80.00    --   93.50  30.00-150.00   76
 14  ω     20.00  51.00   1.00   80.00    --   93.50 -61.00 -60.00   31
 15  ω     37.00  63.00   1.00   80.00    --   93.50 -93.00-139.00   26
 16  ω     66.00 104.00   1.00   80.00    --   93.50 -92.00 -24.17   38
 17  ω    122.00 150.00   1.00   80.00    --   93.50 125.00   0.00   28
 18  ω     11.00  37.00   1.00   80.00    --   93.50 -94.00  30.00   26
 19  ω     98.00 124.00   1.00   80.00    --   93.50 -93.00-102.10   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0572504000
_diffrn_orient_matrix_UB_12      -0.1054559000
_diffrn_orient_matrix_UB_13      0.0057567000
_diffrn_orient_matrix_UB_21      0.1072751000
_diffrn_orient_matrix_UB_22      0.0568153000
_diffrn_orient_matrix_UB_23      -0.0021129000
_diffrn_orient_matrix_UB_31      -0.0029468000
_diffrn_orient_matrix_UB_32      0.0205720000
_diffrn_orient_matrix_UB_33      0.0354075000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage         0.698
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                5571
_reflns_number_total             6116
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details 
;
 Flack x determined using 2136 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         6116
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0394
_refine_ls_restrained_S_all      1.015
_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)+(0.0536P)²+1.7582P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1035
_refine_special_details          
;
The pentamethylethylenetriamine (PMDETA) 
moiety has been modelled as disordered 
over two positions. The occupancies of the 
two sites were allowed to refine with 
isotropic atom treatment. Upon convergence 
of the refinement, the occupancies were 
fixed before anisotropy was introduced into 
the model. The geometry of the PMDETA 
moiety was restrained using the SADI and 
SAME cards and the displacement 
parameters of all partially occupied atoms 
were constrained using the EADP card.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1A-C25A \\sim N1-C25
 with sigma of 0.02
 C27A-C25A \\sim C27-C25
 with sigma of 0.02
 Na1-N1 \\sim Na1-N1A
 with sigma of 0.02
 Na1-N2 \\sim Na1-N2A
 with sigma of 0.02
 Na1-N3 \\sim Na1-N3A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C26) = Uanis(C26A)
Uanis(C25) = Uanis(C25A)
Uanis(N1) = Uanis(N1A)
Uanis(C27) = Uanis(C27A)
Uanis(C28) = Uanis(C28A)
Uanis(C29) = Uanis(C29A)
Uanis(C30) = Uanis(C30A)
Uanis(C31) = Uanis(C31A)
Uanis(N3) = Uanis(N3A)
Uanis(N2) = Uanis(N2A)
Uanis(C32) = Uanis(C32A)
Uanis(C33) = Uanis(C33A)
4. Same fragment restrains
{N1A, C27A, C28A, N2A, C30A, C31A, N3A, C25A, C26A, C29A, C33A, C32A} sigma for
1-2: 0.02, 1-3: 0.02
as
{N1, C27, C28, N2, C30, C31, N3, C25, C26, C29, C33, C32}
5. Others
 Fixed Sof: N1(0.61026) C27(0.61026) H27A(0.61026) H27B(0.61026) C28(0.61026)
 H28A(0.61026) H28B(0.61026) N2(0.61026) C30(0.61026) H30A(0.61026)
 H30B(0.61026) C31(0.61026) H31A(0.61026) H31B(0.61026) N3(0.61026)
 C25(0.61026) H25A(0.61026) H25B(0.61026) H25C(0.61026) C26(0.61026)
 H26A(0.61026) H26B(0.61026) H26C(0.61026) C29(0.61026) H29A(0.61026)
 H29B(0.61026) H29C(0.61026) C33(0.61026) H33A(0.61026) H33B(0.61026)
 H33C(0.61026) C32(0.61026) H32A(0.61026) H32B(0.61026) H32C(0.61026)
 N1A(0.38974) C27A(0.38974) H27C(0.38974) H27D(0.38974) C28A(0.38974)
 H28C(0.38974) H28D(0.38974) N2A(0.38974) C30A(0.38974) H30C(0.38974)
 H30D(0.38974) C31A(0.38974) H31C(0.38974) H31D(0.38974) N3A(0.38974)
 C25A(0.38974) H25D(0.38974) H25E(0.38974) H25F(0.38974) C26A(0.38974)
 H26D(0.38974) H26E(0.38974) H26F(0.38974) C29A(0.38974) H29D(0.38974)
 H29E(0.38974) H29F(0.38974) C33A(0.38974) H33D(0.38974) H33E(0.38974)
 H33F(0.38974) C32A(0.38974) H32D(0.38974) H32E(0.38974) H32F(0.38974)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22)
6.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28A,H28B), C30(H30A,H30B), C31(H31A,H31B), C27A(H27C,
 H27D), C28A(H28C,H28D), C30A(H30C,H30D), C31A(H31C,H31D)
6.c Me refined with riding coordinates:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C33(H33A,H33B,
 H33C), C32(H32A,H32B,H32C), C25A(H25D,H25E,H25F), C26A(H26D,H26E,H26F),
 C29A(H29D,H29E,H29F), C33A(H33D,H33E,H33F), C32A(H32D,H32E,H32F)
6.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17)
6.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
P1 P 0.57873(6) 0.95091(5) 0.32833(2) 0.03433(16) Uani 1 1 d . . . . .
Na1 Na 0.55834(9) 0.74080(8) 0.35289(2) 0.0417(3) Uani 1 1 d D . . . .
N1 N 0.5644(13) 0.5762(9) 0.3204(2) 0.0527(12) Uani 0.6103 1 d D . P A 1
C27 C 0.4984(12) 0.4977(11) 0.3362(2) 0.071(3) Uani 0.6103 1 d D . P A 1
H27A H 0.5140 0.4272 0.3273 0.086 Uiso 0.6103 1 calc R . P A 1
H27B H 0.4234 0.5137 0.3318 0.086 Uiso 0.6103 1 calc R . P A 1
C28 C 0.514(3) 0.4938(12) 0.3707(3) 0.070(3) Uani 0.6103 1 d D . P A 1
H28A H 0.4688 0.4375 0.3794 0.084 Uiso 0.6103 1 calc R . P A 1
H28B H 0.5886 0.4742 0.3750 0.084 Uiso 0.6103 1 calc R . P A 1
N2 N 0.4910(16) 0.5923(11) 0.3867(2) 0.0497(14) Uani 0.6103 1 d D . P A 1
C30 C 0.543(2) 0.5993(17) 0.4170(3) 0.066(3) Uani 0.6103 1 d D . P A 1
H30A H 0.5381 0.5298 0.4274 0.080 Uiso 0.6103 1 calc R . P A 1
H30B H 0.5045 0.6509 0.4300 0.080 Uiso 0.6103 1 calc R . P A 1
C31 C 0.6556(19) 0.6306(19) 0.4161(6) 0.060(2) Uani 0.6103 1 d D . P A 1
H31A H 0.6814 0.6391 0.4377 0.072 Uiso 0.6103 1 calc R . P A 1
H31B H 0.6968 0.5731 0.4063 0.072 Uiso 0.6103 1 calc R . P A 1
N3 N 0.6752(14) 0.7289(15) 0.3989(3) 0.0487(18) Uani 0.6103 1 d D . P A 1
C25 C 0.6768(11) 0.5420(13) 0.3239(4) 0.080(3) Uani 0.6103 1 d D . P A 1
H25A H 0.6952 0.5395 0.3461 0.119 Uiso 0.6103 1 calc R . P A 1
H25B H 0.6859 0.4718 0.3147 0.119 Uiso 0.6103 1 calc R . P A 1
H25C H 0.7231 0.5924 0.3132 0.119 Uiso 0.6103 1 calc R . P A 1
C26 C 0.5399(10) 0.5791(13) 0.2871(2) 0.076(3) Uani 0.6103 1 d D . P A 1
H26A H 0.5845 0.6318 0.2768 0.114 Uiso 0.6103 1 calc R . P A 1
H26B H 0.5533 0.5095 0.2779 0.114 Uiso 0.6103 1 calc R . P A 1
H26C H 0.4655 0.5977 0.2842 0.114 Uiso 0.6103 1 calc R . P A 1
C29 C 0.3760(19) 0.604(4) 0.3906(8) 0.094(4) Uani 0.6103 1 d D . P A 1
H29A H 0.3606 0.6699 0.4014 0.142 Uiso 0.6103 1 calc R . P A 1
H29B H 0.3421 0.6039 0.3700 0.142 Uiso 0.6103 1 calc R . P A 1
H29C H 0.3488 0.5443 0.4029 0.142 Uiso 0.6103 1 calc R . P A 1
C33 C 0.787(2) 0.735(3) 0.3910(10) 0.070(3) Uani 0.6103 1 d D . P A 1
H33A H 0.8076 0.6730 0.3789 0.105 Uiso 0.6103 1 calc R . P A 1
H33B H 0.8000 0.7991 0.3786 0.105 Uiso 0.6103 1 calc R . P A 1
H33C H 0.8292 0.7385 0.4102 0.105 Uiso 0.6103 1 calc R . P A 1
C32 C 0.645(2) 0.8211(18) 0.4168(5) 0.073(4) Uani 0.6103 1 d D . P A 1
H32A H 0.5695 0.8165 0.4221 0.109 Uiso 0.6103 1 calc R . P A 1
H32B H 0.6864 0.8243 0.4360 0.109 Uiso 0.6103 1 calc R . P A 1
H32C H 0.6572 0.8849 0.4044 0.109 Uiso 0.6103 1 calc R . P A 1
C1 C 0.5508(2) 0.8902(2) 0.28979(6) 0.0390(6) Uani 1 1 d . . . . .
C2 C 0.4475(3) 0.8592(2) 0.28056(6) 0.0469(7) Uani 1 1 d . . . . .
C3 C 0.4333(3) 0.8076(3) 0.25208(7) 0.0609(9) Uani 1 1 d . . . . .
H3 H 0.3643 0.7867 0.2460 0.073 Uiso 1 1 calc R . . . .
C4 C 0.5170(4) 0.7863(3) 0.23262(7) 0.0673(11) Uani 1 1 d . . . . .
H4 H 0.5054 0.7514 0.2133 0.081 Uiso 1 1 calc R . . . .
C5 C 0.6179(4) 0.8157(3) 0.24122(7) 0.0610(10) Uani 1 1 d . . . . .
H5 H 0.6753 0.8001 0.2277 0.073 Uiso 1 1 calc R . . . .
C6 C 0.6372(3) 0.8680(2) 0.26935(6) 0.0453(7) Uani 1 1 d . . . . .
C7 C 0.3500(3) 0.8776(3) 0.30064(7) 0.0559(8) Uani 1 1 d . . . . .
H7 H 0.3723 0.9223 0.3187 0.067 Uiso 1 1 calc R . . . .
C8 C 0.3077(3) 0.7746(3) 0.31394(8) 0.0706(11) Uani 1 1 d . . . . .
H8A H 0.2809 0.7304 0.2969 0.106 Uiso 1 1 calc GR . . . .
H8B H 0.2504 0.7897 0.3286 0.106 Uiso 1 1 calc GR . . . .
H8C H 0.3645 0.7373 0.3248 0.106 Uiso 1 1 calc GR . . . .
C9 C 0.2634(4) 0.9368(4) 0.28379(10) 0.0812(12) Uani 1 1 d . . . . .
H9A H 0.2872 1.0088 0.2793 0.122 Uiso 1 1 calc GR . . . .
H9B H 0.2003 0.9394 0.2970 0.122 Uiso 1 1 calc GR . . . .
H9C H 0.2467 0.9006 0.2642 0.122 Uiso 1 1 calc GR . . . .
C10 C 0.7476(3) 0.9034(3) 0.27703(7) 0.0522(8) Uani 1 1 d . . . . .
H10 H 0.7403 0.9648 0.2915 0.063 Uiso 1 1 calc R . . . .
C11 C 0.8095(4) 0.9435(4) 0.24864(10) 0.0868(14) Uani 1 1 d . . . . .
H11A H 0.8241 0.8844 0.2345 0.130 Uiso 1 1 calc GR . . . .
H11B H 0.8762 0.9748 0.2556 0.130 Uiso 1 1 calc GR . . . .
H11C H 0.7676 0.9969 0.2377 0.130 Uiso 1 1 calc GR . . . .
C12 C 0.8105(4) 0.8205(4) 0.29447(11) 0.0797(12) Uani 1 1 d . . . . .
H12A H 0.7717 0.7990 0.3132 0.120 Uiso 1 1 calc GR . . . .
H12B H 0.8791 0.8498 0.3005 0.120 Uiso 1 1 calc GR . . . .
H12C H 0.8214 0.7590 0.2810 0.120 Uiso 1 1 calc GR . . . .
C13 C 0.49195(19) 1.06794(19) 0.32966(5) 0.0312(5) Uani 1 1 d . . . . .
C14 C 0.4447(2) 1.0973(2) 0.35819(6) 0.0357(6) Uani 1 1 d . . . . .
C15 C 0.3783(3) 1.1846(3) 0.35949(8) 0.0501(8) Uani 1 1 d . . . . .
H15 H 0.3471 1.2034 0.3788 0.060 Uiso 1 1 calc R . . . .
C16 C 0.3566(3) 1.2446(3) 0.33340(8) 0.0573(9) Uani 1 1 d . . . . .
H16 H 0.3075 1.3011 0.3344 0.069 Uiso 1 1 calc R . . . .
C17 C 0.4074(3) 1.2208(2) 0.30608(7) 0.0489(7) Uani 1 1 d . . . . .
H17 H 0.3949 1.2634 0.2882 0.059 Uiso 1 1 calc R . . . .
C18 C 0.4762(2) 1.1366(2) 0.30370(6) 0.0381(6) Uani 1 1 d . . . . .
C19 C 0.4633(2) 1.0331(2) 0.38790(6) 0.0436(7) Uani 1 1 d . . . . .
H19 H 0.5285 0.9901 0.3845 0.052 Uiso 1 1 calc R . . . .
C20 C 0.3737(3) 0.9569(3) 0.39396(8) 0.0628(9) Uani 1 1 d . . . . .
H20A H 0.3079 0.9964 0.3968 0.094 Uiso 1 1 calc GR . . . .
H20B H 0.3888 0.9161 0.4129 0.094 Uiso 1 1 calc GR . . . .
H20C H 0.3665 0.9089 0.3762 0.094 Uiso 1 1 calc GR . . . .
C21 C 0.4826(3) 1.1027(4) 0.41659(7) 0.0692(11) Uani 1 1 d . . . . .
H21A H 0.5403 1.1521 0.4122 0.104 Uiso 1 1 calc GR . . . .
H21B H 0.5015 1.0582 0.4344 0.104 Uiso 1 1 calc GR . . . .
H21C H 0.4183 1.1424 0.4215 0.104 Uiso 1 1 calc GR . . . .
C22 C 0.5407(3) 1.1286(2) 0.27360(6) 0.0482(7) Uani 1 1 d . . . . .
H22 H 0.5917 1.0691 0.2763 0.058 Uiso 1 1 calc R . . . .
C23 C 0.6053(3) 1.2281(3) 0.26820(7) 0.0580(9) Uani 1 1 d . . . . .
H23A H 0.5577 1.2877 0.2644 0.087 Uiso 1 1 calc GR . . . .
H23B H 0.6512 1.2181 0.2500 0.087 Uiso 1 1 calc GR . . . .
H23C H 0.6486 1.2426 0.2867 0.087 Uiso 1 1 calc GR . . . .
C24 C 0.4764(4) 1.1051(3) 0.24459(7) 0.0749(12) Uani 1 1 d . . . . .
H24A H 0.4434 1.0355 0.2466 0.112 Uiso 1 1 calc GR . . . .
H24B H 0.5227 1.1057 0.2263 0.112 Uiso 1 1 calc GR . . . .
H24C H 0.4215 1.1589 0.2421 0.112 Uiso 1 1 calc GR . . . .
N1A N 0.556(2) 0.5723(14) 0.3231(4) 0.0527(12) Uani 0.3897 1 d D . P A 2
C27A C 0.521(2) 0.4899(18) 0.3431(4) 0.071(3) Uani 0.3897 1 d D . P A 2
H27C H 0.5646 0.4271 0.3381 0.086 Uiso 0.3897 1 calc R . P A 2
H27D H 0.4479 0.4727 0.3370 0.086 Uiso 0.3897 1 calc R . P A 2
C28A C 0.522(5) 0.501(2) 0.3768(5) 0.070(3) Uani 0.3897 1 d D . P A 2
H28C H 0.4710 0.4494 0.3853 0.084 Uiso 0.3897 1 calc R . P A 2
H28D H 0.5928 0.4798 0.3842 0.084 Uiso 0.3897 1 calc R . P A 2
N2A N 0.498(3) 0.6018(18) 0.3906(4) 0.0497(14) Uani 0.3897 1 d D . P A 2
C30A C 0.554(4) 0.618(3) 0.4202(5) 0.066(3) Uani 0.3897 1 d D . P A 2
H30C H 0.5474 0.5534 0.4330 0.080 Uiso 0.3897 1 calc R . P A 2
H30D H 0.5197 0.6763 0.4316 0.080 Uiso 0.3897 1 calc R . P A 2
C31A C 0.667(3) 0.643(3) 0.4166(10) 0.060(2) Uani 0.3897 1 d D . P A 2
H31C H 0.7039 0.5813 0.4076 0.072 Uiso 0.3897 1 calc R . P A 2
H31D H 0.6980 0.6562 0.4375 0.072 Uiso 0.3897 1 calc R . P A 2
N3A N 0.687(2) 0.736(2) 0.3967(6) 0.0487(18) Uani 0.3897 1 d D . P A 2
C25A C 0.6714(18) 0.567(2) 0.3176(8) 0.080(3) Uani 0.3897 1 d D . P A 2
H25D H 0.6928 0.6243 0.3038 0.119 Uiso 0.3897 1 calc R . P A 2
H25E H 0.7088 0.5727 0.3375 0.119 Uiso 0.3897 1 calc R . P A 2
H25F H 0.6888 0.4988 0.3078 0.119 Uiso 0.3897 1 calc R . P A 2
C26A C 0.5032(16) 0.576(2) 0.2930(4) 0.076(3) Uani 0.3897 1 d D . P A 2
H26D H 0.5314 0.6347 0.2808 0.114 Uiso 0.3897 1 calc R . P A 2
H26E H 0.5158 0.5095 0.2819 0.114 Uiso 0.3897 1 calc R . P A 2
H26F H 0.4272 0.5856 0.2961 0.114 Uiso 0.3897 1 calc R . P A 2
C29A C 0.384(3) 0.614(7) 0.3958(13) 0.094(4) Uani 0.3897 1 d D . P A 2
H29D H 0.3705 0.6835 0.4052 0.142 Uiso 0.3897 1 calc R . P A 2
H29E H 0.3470 0.6093 0.3758 0.142 Uiso 0.3897 1 calc R . P A 2
H29F H 0.3592 0.5586 0.4098 0.142 Uiso 0.3897 1 calc R . P A 2
C33A C 0.797(3) 0.735(5) 0.3871(16) 0.070(3) Uani 0.3897 1 d D . P A 2
H33D H 0.8128 0.6693 0.3760 0.105 Uiso 0.3897 1 calc R . P A 2
H33E H 0.8110 0.7953 0.3732 0.105 Uiso 0.3897 1 calc R . P A 2
H33F H 0.8427 0.7406 0.4055 0.105 Uiso 0.3897 1 calc R . P A 2
C32A C 0.664(3) 0.834(3) 0.4130(9) 0.073(4) Uani 0.3897 1 d D . P A 2
H32D H 0.5897 0.8342 0.4194 0.109 Uiso 0.3897 1 calc R . P A 2
H32E H 0.7091 0.8391 0.4315 0.109 Uiso 0.3897 1 calc R . P A 2
H32F H 0.6775 0.8938 0.3992 0.109 Uiso 0.3897 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 Na1 2.8745(12) . ?
P1 C1 1.856(3) . ?
P1 C13 1.847(3) . ?
Na1 N1 2.509(9) . ?
Na1 N2 2.525(10) . ?
Na1 N3 2.472(10) . ?
Na1 C32 3.121(17) . ?
Na1 N1A 2.487(15) . ?
Na1 N2A 2.508(15) . ?
Na1 N3A 2.485(16) . ?
Na1 C25A 3.04(4) . ?
N1 C27 1.465(11) . ?
N1 C25 1.497(12) . ?
N1 C26 1.462(9) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.494(10) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 N2 1.455(11) . ?
N2 C30 1.460(10) . ?
N2 C29 1.474(11) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.477(11) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 N3 1.468(11) . ?
N3 C33 1.462(12) . ?
N3 C32 1.451(11) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C1 C2 1.423(4) . ?
C1 C6 1.430(4) . ?
C2 C3 1.396(4) . ?
C2 C7 1.524(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.375(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.382(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.398(4) . ?
C6 C10 1.505(5) . ?
C7 H7 1.0000 . ?
C7 C8 1.522(5) . ?
C7 C9 1.512(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 1.0000 . ?
C10 C11 1.534(5) . ?
C10 C12 1.516(6) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.412(4) . ?
C13 C18 1.426(4) . ?
C14 C15 1.391(4) . ?
C14 C19 1.529(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.380(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.370(5) . ?
C17 H17 0.9500 . ?
C17 C18 1.382(4) . ?
C18 C22 1.531(4) . ?
C19 H19 1.0000 . ?
C19 C20 1.512(5) . ?
C19 C21 1.533(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22 1.0000 . ?
C22 C23 1.521(5) . ?
C22 C24 1.516(4) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
N1A C27A 1.418(16) . ?
N1A C25A 1.489(17) . ?
N1A C26A 1.453(16) . ?
C27A H27C 0.9900 . ?
C27A H27D 0.9900 . ?
C27A C28A 1.451(15) . ?
C28A H28C 0.9900 . ?
C28A H28D 0.9900 . ?
C28A N2A 1.438(17) . ?
N2A C30A 1.467(16) . ?
N2A C29A 1.471(17) . ?
C30A H30C 0.9900 . ?
C30A H30D 0.9900 . ?
C30A C31A 1.475(17) . ?
C31A H31C 0.9900 . ?
C31A H31D 0.9900 . ?
C31A N3A 1.479(17) . ?
N3A C33A 1.460(16) . ?
N3A C32A 1.451(16) . ?
C25A H25D 0.9800 . ?
C25A H25E 0.9800 . ?
C25A H25F 0.9800 . ?
C26A H26D 0.9800 . ?
C26A H26E 0.9800 . ?
C26A H26F 0.9800 . ?
C29A H29D 0.9800 . ?
C29A H29E 0.9800 . ?
C29A H29F 0.9800 . ?
C33A H33D 0.9800 . ?
C33A H33E 0.9800 . ?
C33A H33F 0.9800 . ?
C32A H32D 0.9800 . ?
C32A H32E 0.9800 . ?
C32A H32F 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
C1 P1 Na1 85.70(8) . . ?
C13 P1 Na1 132.75(9) . . ?
C13 P1 C1 104.28(12) . . ?
P1 Na1 C32 89.3(5) . . ?
P1 Na1 C25A 116.6(4) . . ?
N1 Na1 P1 124.3(3) . . ?
N1 Na1 N2 73.1(3) . . ?
N1 Na1 C32 138.4(6) . . ?
N2 Na1 P1 158.6(4) . . ?
N2 Na1 C32 81.8(4) . . ?
N3 Na1 P1 107.2(4) . . ?
N3 Na1 N1 112.0(5) . . ?
N3 Na1 N2 72.4(4) . . ?
N3 Na1 C32 27.0(4) . . ?
N1A Na1 P1 127.5(4) . . ?
N1A Na1 N2A 74.0(5) . . ?
N1A Na1 C25A 29.2(6) . . ?
N2A Na1 P1 156.0(6) . . ?
N2A Na1 C25A 87.4(7) . . ?
N3A Na1 P1 103.8(7) . . ?
N3A Na1 N1A 112.1(8) . . ?
N3A Na1 N2A 72.3(6) . . ?
N3A Na1 C25A 92.9(9) . . ?
C27 N1 Na1 106.9(6) . . ?
C27 N1 C25 107.5(9) . . ?
C25 N1 Na1 102.3(10) . . ?
C26 N1 Na1 121.0(9) . . ?
C26 N1 C27 110.3(8) . . ?
C26 N1 C25 107.9(9) . . ?
N1 C27 H27A 108.8 . . ?
N1 C27 H27B 108.8 . . ?
N1 C27 C28 113.8(11) . . ?
H27A C27 H27B 107.7 . . ?
C28 C27 H27A 108.8 . . ?
C28 C27 H27B 108.8 . . ?
C27 C28 H28A 108.7 . . ?
C27 C28 H28B 108.7 . . ?
H28A C28 H28B 107.6 . . ?
N2 C28 C27 114.4(11) . . ?
N2 C28 H28A 108.7 . . ?
N2 C28 H28B 108.7 . . ?
C28 N2 Na1 107.4(8) . . ?
C28 N2 C30 112.4(10) . . ?
C28 N2 C29 109.7(11) . . ?
C30 N2 Na1 108.2(7) . . ?
C30 N2 C29 110.1(10) . . ?
C29 N2 Na1 109(2) . . ?
N2 C30 H30A 108.4 . . ?
N2 C30 H30B 108.4 . . ?
N2 C30 C31 115.5(10) . . ?
H30A C30 H30B 107.5 . . ?
C31 C30 H30A 108.4 . . ?
C31 C30 H30B 108.4 . . ?
C30 C31 H31A 108.8 . . ?
C30 C31 H31B 108.8 . . ?
H31A C31 H31B 107.7 . . ?
N3 C31 C30 113.9(9) . . ?
N3 C31 H31A 108.8 . . ?
N3 C31 H31B 108.8 . . ?
C31 N3 Na1 110.5(8) . . ?
C33 N3 Na1 113.1(18) . . ?
C33 N3 C31 109.2(10) . . ?
C32 N3 Na1 102.3(9) . . ?
C32 N3 C31 111.8(10) . . ?
C32 N3 C33 109.7(10) . . ?
N1 C25 H25A 109.5 . . ?
N1 C25 H25B 109.5 . . ?
N1 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N1 C26 H26A 109.5 . . ?
N1 C26 H26B 109.5 . . ?
N1 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N2 C29 H29A 109.5 . . ?
N2 C29 H29B 109.5 . . ?
N2 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C33 H33A 109.5 . . ?
N3 C33 H33B 109.5 . . ?
N3 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
Na1 C32 H32A 80.9 . . ?
Na1 C32 H32B 160.2 . . ?
Na1 C32 H32C 81.4 . . ?
N3 C32 Na1 50.7(7) . . ?
N3 C32 H32A 109.5 . . ?
N3 C32 H32B 109.5 . . ?
N3 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C2 C1 P1 122.5(2) . . ?
C2 C1 C6 118.6(2) . . ?
C6 C1 P1 118.7(2) . . ?
C1 C2 C7 123.1(2) . . ?
C3 C2 C1 119.4(3) . . ?
C3 C2 C7 117.5(3) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 C2 121.5(4) . . ?
C4 C3 H3 119.2 . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.9(3) . . ?
C5 C4 H4 120.1 . . ?
C4 C5 H5 119.3 . . ?
C4 C5 C6 121.3(3) . . ?
C6 C5 H5 119.3 . . ?
C1 C6 C10 121.3(2) . . ?
C5 C6 C1 119.2(3) . . ?
C5 C6 C10 119.5(3) . . ?
C2 C7 H7 107.1 . . ?
C8 C7 C2 111.4(3) . . ?
C8 C7 H7 107.1 . . ?
C9 C7 C2 113.2(3) . . ?
C9 C7 H7 107.1 . . ?
C9 C7 C8 110.4(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 H10 106.4 . . ?
C6 C10 C11 113.6(3) . . ?
C6 C10 C12 112.9(3) . . ?
C11 C10 H10 106.4 . . ?
C12 C10 H10 106.4 . . ?
C12 C10 C11 110.6(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 P1 119.38(18) . . ?
C14 C13 C18 117.1(2) . . ?
C18 C13 P1 123.29(19) . . ?
C13 C14 C19 121.1(2) . . ?
C15 C14 C13 120.0(2) . . ?
C15 C14 C19 118.9(2) . . ?
C14 C15 H15 119.1 . . ?
C16 C15 C14 121.8(3) . . ?
C16 C15 H15 119.1 . . ?
C15 C16 H16 120.7 . . ?
C17 C16 C15 118.5(3) . . ?
C17 C16 H16 120.7 . . ?
C16 C17 H17 119.0 . . ?
C16 C17 C18 122.0(3) . . ?
C18 C17 H17 119.0 . . ?
C13 C18 C22 122.9(2) . . ?
C17 C18 C13 120.1(3) . . ?
C17 C18 C22 116.7(2) . . ?
C14 C19 H19 107.3 . . ?
C14 C19 C21 112.7(3) . . ?
C20 C19 C14 111.5(2) . . ?
C20 C19 H19 107.3 . . ?
C20 C19 C21 110.4(3) . . ?
C21 C19 H19 107.3 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22 H22 107.2 . . ?
C23 C22 C18 111.2(3) . . ?
C23 C22 H22 107.2 . . ?
C24 C22 C18 114.7(3) . . ?
C24 C22 H22 107.2 . . ?
C24 C22 C23 109.1(2) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C27A N1A Na1 109.1(9) . . ?
C27A N1A C25A 111.3(15) . . ?
C27A N1A C26A 114.7(14) . . ?
C25A N1A Na1 96.3(17) . . ?
C26A N1A Na1 115.9(16) . . ?
C26A N1A C25A 108.0(13) . . ?
N1A C27A H27C 106.9 . . ?
N1A C27A H27D 106.9 . . ?
N1A C27A C28A 121.7(15) . . ?
H27C C27A H27D 106.7 . . ?
C28A C27A H27C 106.9 . . ?
C28A C27A H27D 106.9 . . ?
C27A C28A H28C 107.4 . . ?
C27A C28A H28D 107.4 . . ?
H28C C28A H28D 106.9 . . ?
N2A C28A C27A 119.8(16) . . ?
N2A C28A H28C 107.4 . . ?
N2A C28A H28D 107.4 . . ?
C28A N2A Na1 107.1(12) . . ?
C28A N2A C30A 112.3(16) . . ?
C28A N2A C29A 111.3(18) . . ?
C30A N2A Na1 108.2(11) . . ?
C30A N2A C29A 109.2(16) . . ?
C29A N2A Na1 109(4) . . ?
N2A C30A H30C 108.7 . . ?
N2A C30A H30D 108.7 . . ?
N2A C30A C31A 114.3(16) . . ?
H30C C30A H30D 107.6 . . ?
C31A C30A H30C 108.7 . . ?
C31A C30A H30D 108.7 . . ?
C30A C31A H31C 108.9 . . ?
C30A C31A H31D 108.9 . . ?
C30A C31A N3A 113.2(15) . . ?
H31C C31A H31D 107.8 . . ?
N3A C31A H31C 108.9 . . ?
N3A C31A H31D 108.9 . . ?
C31A N3A Na1 110.3(12) . . ?
C33A N3A Na1 115(3) . . ?
C33A N3A C31A 108.5(16) . . ?
C32A N3A Na1 102.3(15) . . ?
C32A N3A C31A 111.5(15) . . ?
C32A N3A C33A 109.6(16) . . ?
Na1 C25A H25D 83.6 . . ?
Na1 C25A H25E 74.7 . . ?
Na1 C25A H25F 163.0 . . ?
N1A C25A Na1 54.5(13) . . ?
N1A C25A H25D 109.5 . . ?
N1A C25A H25E 109.5 . . ?
N1A C25A H25F 109.5 . . ?
H25D C25A H25E 109.5 . . ?
H25D C25A H25F 109.5 . . ?
H25E C25A H25F 109.5 . . ?
N1A C26A H26D 109.5 . . ?
N1A C26A H26E 109.5 . . ?
N1A C26A H26F 109.5 . . ?
H26D C26A H26E 109.5 . . ?
H26D C26A H26F 109.5 . . ?
H26E C26A H26F 109.5 . . ?
N2A C29A H29D 109.5 . . ?
N2A C29A H29E 109.5 . . ?
N2A C29A H29F 109.5 . . ?
H29D C29A H29E 109.5 . . ?
H29D C29A H29F 109.5 . . ?
H29E C29A H29F 109.5 . . ?
N3A C33A H33D 109.5 . . ?
N3A C33A H33E 109.5 . . ?
N3A C33A H33F 109.5 . . ?
H33D C33A H33E 109.5 . . ?
H33D C33A H33F 109.5 . . ?
H33E C33A H33F 109.5 . . ?
N3A C32A H32D 109.5 . . ?
N3A C32A H32E 109.5 . . ?
N3A C32A H32F 109.5 . . ?
H32D C32A H32E 109.5 . . ?
H32D C32A H32F 109.5 . . ?
H32E C32A H32F 109.5 . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.353
_oxdiff_exptl_absorpt_empirical_full_min 0.737
####################################################################### 
# 
# 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_7a
_database_code_depnum_ccdc_archive 'CCDC 1557234'
_audit_update_record             
;
2017-06-20 deposited with the CCDC.
2017-07-20 downloaded from the CCDC.
;
_audit_creation_date             2016-04-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C33 H52 Li O3 P'
_chemical_formula_sum            'C33 H52 Li O3 P'
_chemical_formula_weight         534.65
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C21 H28 Li1 P1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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                   9.5265(4)
_cell_length_b                   9.5469(5)
_cell_length_c                   19.4340(10)
_cell_angle_alpha                82.213(4)
_cell_angle_beta                 89.691(4)
_cell_angle_gamma                65.484(5)
_cell_volume                     1590.76(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4999
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      66.4700
_cell_measurement_theta_min      4.5710
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.980
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22353
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.058
_diffrn_reflns_theta_min         4.600
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3968
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -99.00 -18.00   1.00    4.00    --  -41.59 125.00-150.00   81
  2  ω    -40.00  88.00   1.00    4.00    --   41.59 -19.00   0.00  128
  3  ω     15.00 117.00   1.00    4.00    --   41.59  38.00-180.00  102
  4  ω     -3.00  96.00   1.00    4.00    --   41.59-125.00 -60.00   99
  5  ω      9.00 133.00   1.00   16.00    --   93.50 -93.00-168.95  124
  6  ω      9.00 133.00   1.00   16.00    --   93.50 -93.00  23.20  124
  7  ω      9.00 133.00   1.00   16.00    --   93.50 -93.00  72.15  124
  8  ω      9.00 133.00   1.00   16.00    --   93.50 -92.00-141.57  124
  9  ω      9.00 133.00   1.00   16.00    --   93.50 -93.00 -52.40  124
 10  ω     63.00 168.00   1.00   16.00    --   93.50  61.00  60.00  105
 11  ω     66.00 168.00   1.00   16.00    --   93.50  45.00 -30.00  102
 12  ω      9.00  83.00   1.00   16.00    --   93.50 -94.00 -30.00   74
 13  ω     32.00 174.00   1.00   16.00    --   93.50  15.00  90.00  142
 14  ω     64.00 140.00   1.00   16.00    --   93.50  61.00 120.00   76
 15  ω     18.00 100.00   1.00   16.00    --   93.50 -90.00 134.38   82
 16  ω    120.00 167.00   1.00   16.00    --   93.50 125.00   0.00   47
 17  ω     67.00 168.00   1.00   16.00    --   93.50  61.00   0.00  101
 18  ω     68.00 135.00   1.00   16.00    --   93.50  77.00 -90.00   67
 19  ω    118.00 169.00   1.00   16.00    --   93.50  69.00  35.35   51
 20  ω     46.00 123.00   1.00   16.00    --   93.50 -30.00 -30.00   77
 21  ω      9.00  41.00   1.00   16.00    --   93.50 -94.00   0.00   32
 22  ω     48.00  73.00   1.00   16.00    --   93.50 -94.00   0.00   25
 23  ω    110.00 147.00   1.00   16.00    --   93.50 125.00 -90.00   37
 24  ω     10.00  68.00   1.00   16.00    --   93.50 -94.00-150.00   58
 25  ω    116.00 158.00   1.00   16.00    --   93.50 125.00 150.00   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0840968000
_diffrn_orient_matrix_UB_12      -0.1741949000
_diffrn_orient_matrix_UB_13      -0.0064851000
_diffrn_orient_matrix_UB_21      -0.0387267000
_diffrn_orient_matrix_UB_22      -0.0423897000
_diffrn_orient_matrix_UB_23      0.0748300000
_diffrn_orient_matrix_UB_31      -0.1520518000
_diffrn_orient_matrix_UB_32      0.0022150000
_diffrn_orient_matrix_UB_33      -0.0279355000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4366
_reflns_number_total             5634
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         5634
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0483
_refine_ls_restrained_S_all      1.021
_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)+(0.0592P)²+0.4357P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1306
_refine_special_details          ?
_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:
 C7(H7), C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,
 H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C17(H17)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_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
P1 P 0.84722(5) 0.51293(6) 0.76152(3) 0.03080(15) Uani 1 1 d . . . . .
O1 O 0.42826(17) 0.53885(18) 0.78506(8) 0.0430(4) Uani 1 1 d . . . . .
O2 O 0.42818(16) 0.77032(17) 0.66725(7) 0.0393(3) Uani 1 1 d . . . . .
O3 O 0.49779(16) 0.81578(19) 0.81636(8) 0.0413(4) Uani 1 1 d . . . . .
C1 C 0.8691(2) 0.3124(2) 0.79308(10) 0.0295(4) Uani 1 1 d . . . . .
C2 C 0.8978(2) 0.2562(2) 0.86583(10) 0.0324(4) Uani 1 1 d . . . . .
C3 C 0.9129(3) 0.1073(3) 0.89089(11) 0.0403(5) Uani 1 1 d . . . . .
H3 H 0.9312 0.0715 0.9394 0.048 Uiso 1 1 calc R . . . .
C4 C 0.9019(3) 0.0092(3) 0.84666(12) 0.0443(5) Uani 1 1 d . . . . .
H4 H 0.9158 -0.0937 0.8644 0.053 Uiso 1 1 calc R . . . .
C5 C 0.8704(2) 0.0640(3) 0.77644(12) 0.0395(5) Uani 1 1 d . . . . .
H5 H 0.8622 -0.0025 0.7460 0.047 Uiso 1 1 calc R . . . .
C6 C 0.8502(2) 0.2140(2) 0.74901(10) 0.0326(4) Uani 1 1 d . . . . .
C7 C 0.9106(2) 0.3584(3) 0.91674(10) 0.0373(5) Uani 1 1 d . . . . .
H7 H 0.9507 0.4310 0.8909 0.045 Uiso 1 1 calc R . . . .
C8 C 0.7525(3) 0.4583(3) 0.94050(14) 0.0547(6) Uani 1 1 d . . . . .
H8A H 0.6833 0.5193 0.8998 0.082 Uiso 1 1 calc GR . . . .
H8B H 0.7624 0.5288 0.9704 0.082 Uiso 1 1 calc GR . . . .
H8C H 0.7097 0.3912 0.9666 0.082 Uiso 1 1 calc GR . . . .
C9 C 1.0211(3) 0.2714(3) 0.97980(14) 0.0564(7) Uani 1 1 d . . . . .
H9A H 0.9792 0.2082 1.0095 0.085 Uiso 1 1 calc GR . . . .
H9B H 1.0338 0.3464 1.0062 0.085 Uiso 1 1 calc GR . . . .
H9C H 1.1216 0.2037 0.9644 0.085 Uiso 1 1 calc GR . . . .
C10 C 0.8049(2) 0.2655(3) 0.67121(10) 0.0340(4) Uani 1 1 d . . . . .
H10 H 0.7954 0.3744 0.6593 0.041 Uiso 1 1 calc R . . . .
C11 C 0.9256(3) 0.1645(3) 0.62616(12) 0.0464(6) Uani 1 1 d . . . . .
H11A H 1.0247 0.1685 0.6356 0.070 Uiso 1 1 calc GR . . . .
H11B H 0.8925 0.2031 0.5770 0.070 Uiso 1 1 calc GR . . . .
H11C H 0.9373 0.0567 0.6369 0.070 Uiso 1 1 calc GR . . . .
C12 C 0.6469(2) 0.2669(3) 0.65474(12) 0.0425(5) Uani 1 1 d . . . . .
H12A H 0.6540 0.1606 0.6644 0.064 Uiso 1 1 calc GR . . . .
H12B H 0.6158 0.3078 0.6055 0.064 Uiso 1 1 calc GR . . . .
H12C H 0.5701 0.3330 0.6837 0.064 Uiso 1 1 calc GR . . . .
C13 C 0.9790(2) 0.4902(2) 0.69064(10) 0.0292(4) Uani 1 1 d . . . . .
C14 C 1.1272(2) 0.3641(2) 0.69256(10) 0.0314(4) Uani 1 1 d . . . . .
C15 C 1.2205(2) 0.3564(2) 0.63605(11) 0.0338(4) Uani 1 1 d . . . . .
H15 H 1.3184 0.2703 0.6380 0.041 Uiso 1 1 calc R . . . .
C16 C 1.1767(2) 0.4680(3) 0.57759(11) 0.0363(5) Uani 1 1 d . . . . .
C17 C 1.0369(2) 0.5968(3) 0.57819(11) 0.0368(5) Uani 1 1 d . . . . .
H17 H 1.0065 0.6783 0.5398 0.044 Uiso 1 1 calc R . . . .
C18 C 0.9399(2) 0.6103(2) 0.63318(10) 0.0334(4) Uani 1 1 d . . . . .
C19 C 1.1924(2) 0.2417(2) 0.75526(11) 0.0364(5) Uani 1 1 d . . . . .
H19A H 1.1676 0.2907 0.7975 0.055 Uiso 1 1 calc GR . . . .
H19B H 1.3049 0.1884 0.7533 0.055 Uiso 1 1 calc GR . . . .
H19C H 1.1474 0.1660 0.7559 0.055 Uiso 1 1 calc GR . . . .
C20 C 1.2785(3) 0.4520(3) 0.51657(12) 0.0441(5) Uani 1 1 d . . . . .
H20A H 1.3327 0.5193 0.5178 0.066 Uiso 1 1 calc GR . . . .
H20B H 1.2146 0.4827 0.4731 0.066 Uiso 1 1 calc GR . . . .
H20C H 1.3541 0.3436 0.5193 0.066 Uiso 1 1 calc GR . . . .
C21 C 0.7920(2) 0.7550(3) 0.63013(12) 0.0429(5) Uani 1 1 d . . . . .
H21A H 0.7039 0.7271 0.6301 0.064 Uiso 1 1 calc GR . . . .
H21B H 0.7850 0.8261 0.5876 0.064 Uiso 1 1 calc GR . . . .
H21C H 0.7906 0.8062 0.6707 0.064 Uiso 1 1 calc GR . . . .
C22 C 0.2615(3) 0.6129(3) 0.78055(14) 0.0502(6) Uani 1 1 d . . . . .
H22A H 0.2195 0.5774 0.7433 0.060 Uiso 1 1 calc R . . . .
H22B H 0.2237 0.7275 0.7707 0.060 Uiso 1 1 calc R . . . .
C23 C 0.2143(3) 0.5639(3) 0.85124(15) 0.0573(7) Uani 1 1 d . . . . .
H23A H 0.1251 0.5374 0.8463 0.069 Uiso 1 1 calc R . . . .
H23B H 0.1861 0.6481 0.8804 0.069 Uiso 1 1 calc R . . . .
C24 C 0.3589(3) 0.4192(3) 0.88356(15) 0.0573(7) Uani 1 1 d . . . . .
H24A H 0.4036 0.4410 0.9245 0.069 Uiso 1 1 calc R . . . .
H24B H 0.3334 0.3293 0.8978 0.069 Uiso 1 1 calc R . . . .
C25 C 0.4692(3) 0.3884(3) 0.82527(13) 0.0457(5) Uani 1 1 d . . . . .
H25A H 0.5778 0.3436 0.8440 0.055 Uiso 1 1 calc R . . . .
H25B H 0.4557 0.3160 0.7968 0.055 Uiso 1 1 calc R . . . .
C26 C 0.3931(3) 0.7027(3) 0.61128(12) 0.0471(6) Uani 1 1 d . . . . .
H26A H 0.3380 0.6379 0.6284 0.057 Uiso 1 1 calc R . . . .
H26B H 0.4890 0.6370 0.5905 0.057 Uiso 1 1 calc R . . . .
C27 C 0.2918(3) 0.8389(4) 0.55868(13) 0.0597(7) Uani 1 1 d . . . . .
H27A H 0.1812 0.8709 0.5676 0.072 Uiso 1 1 calc R . . . .
H27B H 0.3090 0.8136 0.5107 0.072 Uiso 1 1 calc R . . . .
C28 C 0.3435(3) 0.9645(3) 0.56988(13) 0.0578(7) Uani 1 1 d . . . . .
H28A H 0.4371 0.9534 0.5446 0.069 Uiso 1 1 calc R . . . .
H28B H 0.2607 1.0695 0.5548 0.069 Uiso 1 1 calc R . . . .
C29 C 0.3769(3) 0.9351(3) 0.64701(13) 0.0463(5) Uani 1 1 d . . . . .
H29A H 0.4583 0.9682 0.6590 0.056 Uiso 1 1 calc R . . . .
H29B H 0.2827 0.9932 0.6709 0.056 Uiso 1 1 calc R . . . .
C30 C 0.6008(3) 0.8865(3) 0.82935(13) 0.0468(6) Uani 1 1 d . . . . .
H30A H 0.5755 0.9831 0.7962 0.056 Uiso 1 1 calc R . . . .
H30B H 0.7094 0.8142 0.8245 0.056 Uiso 1 1 calc R . . . .
C31 C 0.5771(3) 0.9219(4) 0.90230(15) 0.0646(8) Uani 1 1 d . . . . .
H31A H 0.6493 0.8338 0.9358 0.078 Uiso 1 1 calc R . . . .
H31B H 0.5921 1.0166 0.9075 0.078 Uiso 1 1 calc R . . . .
C32 C 0.4150(4) 0.9464(4) 0.91286(16) 0.0715(8) Uani 1 1 d . . . . .
H32A H 0.3433 1.0565 0.8977 0.086 Uiso 1 1 calc R . . . .
H32B H 0.4007 0.9174 0.9624 0.086 Uiso 1 1 calc R . . . .
C33 C 0.3874(3) 0.8421(3) 0.86878(13) 0.0465(5) Uani 1 1 d . . . . .
H33A H 0.4019 0.7424 0.8972 0.056 Uiso 1 1 calc R . . . .
H33B H 0.2810 0.8924 0.8473 0.056 Uiso 1 1 calc R . . . .
Li1 Li 0.5505(4) 0.6550(4) 0.75290(18) 0.0368(7) 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
P1 C1 1.854(2) . ?
P1 C13 1.832(2) . ?
P1 Li1 2.572(3) . ?
O1 C22 1.444(3) . ?
O1 C25 1.435(3) . ?
O1 Li1 1.963(4) . ?
O2 C26 1.444(3) . ?
O2 C29 1.437(3) . ?
O2 Li1 1.950(4) . ?
O3 C30 1.442(3) . ?
O3 C33 1.430(3) . ?
O3 Li1 1.999(4) . ?
C1 C2 1.428(3) . ?
C1 C6 1.417(3) . ?
C2 C3 1.387(3) . ?
C2 C7 1.519(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.388(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.381(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.391(3) . ?
C6 C10 1.531(3) . ?
C7 H7 1.0000 . ?
C7 C8 1.520(3) . ?
C7 C9 1.521(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 1.0000 . ?
C10 C11 1.522(3) . ?
C10 C12 1.535(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.422(3) . ?
C13 C18 1.416(3) . ?
C14 C15 1.399(3) . ?
C14 C19 1.502(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.381(3) . ?
C16 C17 1.389(3) . ?
C16 C20 1.511(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.393(3) . ?
C18 C21 1.504(3) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.517(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.548(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.515(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.509(4) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.513(4) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.498(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.496(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.481(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.498(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 Li1 99.42(10) . . ?
C13 P1 C1 104.34(9) . . ?
C13 P1 Li1 127.65(10) . . ?
C22 O1 Li1 121.23(18) . . ?
C25 O1 C22 105.63(17) . . ?
C25 O1 Li1 132.35(16) . . ?
C26 O2 Li1 125.69(17) . . ?
C29 O2 C26 109.90(16) . . ?
C29 O2 Li1 123.96(16) . . ?
C30 O3 Li1 121.58(16) . . ?
C33 O3 C30 109.58(16) . . ?
C33 O3 Li1 126.31(17) . . ?
C2 C1 P1 118.88(15) . . ?
C6 C1 P1 123.24(15) . . ?
C6 C1 C2 117.78(18) . . ?
C1 C2 C7 120.77(18) . . ?
C3 C2 C1 120.04(19) . . ?
C3 C2 C7 119.19(18) . . ?
C2 C3 H3 119.2 . . ?
C2 C3 C4 121.5(2) . . ?
C4 C3 H3 119.2 . . ?
C3 C4 H4 120.6 . . ?
C5 C4 C3 118.8(2) . . ?
C5 C4 H4 120.6 . . ?
C4 C5 H5 119.1 . . ?
C4 C5 C6 121.9(2) . . ?
C6 C5 H5 119.1 . . ?
C1 C6 C10 122.98(18) . . ?
C5 C6 C1 119.89(18) . . ?
C5 C6 C10 117.13(18) . . ?
C2 C7 H7 107.0 . . ?
C2 C7 C8 110.90(18) . . ?
C2 C7 C9 114.86(19) . . ?
C8 C7 H7 107.0 . . ?
C8 C7 C9 109.7(2) . . ?
C9 C7 H7 107.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 H10 107.8 . . ?
C6 C10 C12 110.43(17) . . ?
C11 C10 C6 112.49(17) . . ?
C11 C10 H10 107.8 . . ?
C11 C10 C12 110.28(17) . . ?
C12 C10 H10 107.8 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 P1 123.61(15) . . ?
C18 C13 P1 119.23(15) . . ?
C18 C13 C14 116.89(18) . . ?
C13 C14 C19 122.22(18) . . ?
C15 C14 C13 119.72(18) . . ?
C15 C14 C19 117.97(17) . . ?
C14 C15 H15 118.5 . . ?
C16 C15 C14 123.04(19) . . ?
C16 C15 H15 118.5 . . ?
C15 C16 C17 116.99(19) . . ?
C15 C16 C20 121.31(19) . . ?
C17 C16 C20 121.7(2) . . ?
C16 C17 H17 118.9 . . ?
C16 C17 C18 122.1(2) . . ?
C18 C17 H17 118.9 . . ?
C13 C18 C21 120.54(18) . . ?
C17 C18 C13 120.84(19) . . ?
C17 C18 C21 118.62(19) . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C16 C20 H20A 109.5 . . ?
C16 C20 H20B 109.5 . . ?
C16 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O1 C22 H22A 110.8 . . ?
O1 C22 H22B 110.8 . . ?
O1 C22 C23 105.0(2) . . ?
H22A C22 H22B 108.8 . . ?
C23 C22 H22A 110.8 . . ?
C23 C22 H22B 110.8 . . ?
C22 C23 H23A 110.8 . . ?
C22 C23 H23B 110.8 . . ?
C22 C23 C24 104.6(2) . . ?
H23A C23 H23B 108.9 . . ?
C24 C23 H23A 110.8 . . ?
C24 C23 H23B 110.8 . . ?
C23 C24 H24A 111.0 . . ?
C23 C24 H24B 111.0 . . ?
H24A C24 H24B 109.0 . . ?
C25 C24 C23 103.7(2) . . ?
C25 C24 H24A 111.0 . . ?
C25 C24 H24B 111.0 . . ?
O1 C25 C24 104.3(2) . . ?
O1 C25 H25A 110.9 . . ?
O1 C25 H25B 110.9 . . ?
C24 C25 H25A 110.9 . . ?
C24 C25 H25B 110.9 . . ?
H25A C25 H25B 108.9 . . ?
O2 C26 H26A 110.7 . . ?
O2 C26 H26B 110.7 . . ?
O2 C26 C27 105.4(2) . . ?
H26A C26 H26B 108.8 . . ?
C27 C26 H26A 110.7 . . ?
C27 C26 H26B 110.7 . . ?
C26 C27 H27A 111.2 . . ?
C26 C27 H27B 111.2 . . ?
C26 C27 C28 103.1(2) . . ?
H27A C27 H27B 109.1 . . ?
C28 C27 H27A 111.2 . . ?
C28 C27 H27B 111.2 . . ?
C27 C28 H28A 111.3 . . ?
C27 C28 H28B 111.3 . . ?
H28A C28 H28B 109.2 . . ?
C29 C28 C27 102.4(2) . . ?
C29 C28 H28A 111.3 . . ?
C29 C28 H28B 111.3 . . ?
O2 C29 C28 105.95(19) . . ?
O2 C29 H29A 110.5 . . ?
O2 C29 H29B 110.5 . . ?
C28 C29 H29A 110.5 . . ?
C28 C29 H29B 110.5 . . ?
H29A C29 H29B 108.7 . . ?
O3 C30 H30A 110.6 . . ?
O3 C30 H30B 110.6 . . ?
O3 C30 C31 105.8(2) . . ?
H30A C30 H30B 108.7 . . ?
C31 C30 H30A 110.6 . . ?
C31 C30 H30B 110.6 . . ?
C30 C31 H31A 111.0 . . ?
C30 C31 H31B 111.0 . . ?
H31A C31 H31B 109.0 . . ?
C32 C31 C30 103.6(2) . . ?
C32 C31 H31A 111.0 . . ?
C32 C31 H31B 111.0 . . ?
C31 C32 H32A 110.8 . . ?
C31 C32 H32B 110.8 . . ?
C31 C32 C33 104.7(2) . . ?
H32A C32 H32B 108.9 . . ?
C33 C32 H32A 110.8 . . ?
C33 C32 H32B 110.8 . . ?
O3 C33 C32 106.4(2) . . ?
O3 C33 H33A 110.5 . . ?
O3 C33 H33B 110.5 . . ?
C32 C33 H33A 110.5 . . ?
C32 C33 H33B 110.5 . . ?
H33A C33 H33B 108.6 . . ?
O1 Li1 P1 119.14(16) . . ?
O1 Li1 O3 103.58(17) . . ?
O2 Li1 P1 124.15(17) . . ?
O2 Li1 O1 98.24(16) . . ?
O2 Li1 O3 103.59(17) . . ?
O3 Li1 P1 105.65(14) . . ?

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
P1 C1 C2 C3 179.26(15) . . . . ?
P1 C1 C2 C7 -0.1(2) . . . . ?
P1 C1 C6 C5 179.23(15) . . . . ?
P1 C1 C6 C10 -1.9(3) . . . . ?
P1 C13 C14 C15 -179.81(14) . . . . ?
P1 C13 C14 C19 -3.2(3) . . . . ?
P1 C13 C18 C17 -179.71(15) . . . . ?
P1 C13 C18 C21 -0.1(3) . . . . ?
O1 C22 C23 C24 -18.6(3) . . . . ?
O2 C26 C27 C28 28.5(3) . . . . ?
O3 C30 C31 C32 -28.5(3) . . . . ?
C1 P1 C13 C14 -39.06(17) . . . . ?
C1 P1 C13 C18 147.12(15) . . . . ?
C1 C2 C3 C4 0.5(3) . . . . ?
C1 C2 C7 C8 87.2(2) . . . . ?
C1 C2 C7 C9 -147.8(2) . . . . ?
C1 C6 C10 C11 120.2(2) . . . . ?
C1 C6 C10 C12 -116.1(2) . . . . ?
C2 C1 C6 C5 -4.4(3) . . . . ?
C2 C1 C6 C10 174.43(17) . . . . ?
C2 C3 C4 C5 -2.1(3) . . . . ?
C3 C2 C7 C8 -92.1(2) . . . . ?
C3 C2 C7 C9 32.9(3) . . . . ?
C3 C4 C5 C6 0.3(3) . . . . ?
C4 C5 C6 C1 3.0(3) . . . . ?
C4 C5 C6 C10 -175.93(19) . . . . ?
C5 C6 C10 C11 -60.9(2) . . . . ?
C5 C6 C10 C12 62.8(2) . . . . ?
C6 C1 C2 C3 2.7(3) . . . . ?
C6 C1 C2 C7 -176.62(17) . . . . ?
C7 C2 C3 C4 179.8(2) . . . . ?
C13 P1 C1 C2 129.55(14) . . . . ?
C13 P1 C1 C6 -54.13(17) . . . . ?
C13 C14 C15 C16 1.1(3) . . . . ?
C14 C13 C18 C17 6.1(3) . . . . ?
C14 C13 C18 C21 -174.29(18) . . . . ?
C14 C15 C16 C17 3.7(3) . . . . ?
C14 C15 C16 C20 -177.67(19) . . . . ?
C15 C16 C17 C18 -3.5(3) . . . . ?
C16 C17 C18 C13 -1.4(3) . . . . ?
C16 C17 C18 C21 178.92(19) . . . . ?
C18 C13 C14 C15 -5.8(3) . . . . ?
C18 C13 C14 C19 170.72(18) . . . . ?
C19 C14 C15 C16 -175.66(18) . . . . ?
C20 C16 C17 C18 177.85(19) . . . . ?
C22 O1 C25 C24 -42.0(2) . . . . ?
C22 C23 C24 C25 -6.0(3) . . . . ?
C23 C24 C25 O1 28.6(2) . . . . ?
C25 O1 C22 C23 37.9(2) . . . . ?
C26 O2 C29 C28 -13.8(3) . . . . ?
C26 C27 C28 C29 -36.1(3) . . . . ?
C27 C28 C29 O2 31.1(3) . . . . ?
C29 O2 C26 C27 -9.4(3) . . . . ?
C30 O3 C33 C32 5.1(3) . . . . ?
C30 C31 C32 C33 31.3(3) . . . . ?
C31 C32 C33 O3 -23.0(3) . . . . ?
C33 O3 C30 C31 14.7(3) . . . . ?
Li1 P1 C1 C2 -97.50(16) . . . . ?
Li1 P1 C1 C6 78.83(17) . . . . ?
Li1 P1 C13 C14 -153.29(16) . . . . ?
Li1 P1 C13 C18 32.9(2) . . . . ?
Li1 O1 C22 C23 -133.0(2) . . . . ?
Li1 O1 C25 C24 127.6(2) . . . . ?
Li1 O2 C26 C27 178.1(2) . . . . ?
Li1 O2 C29 C28 158.8(2) . . . . ?
Li1 O3 C30 C31 -148.3(2) . . . . ?
Li1 O3 C33 C32 167.1(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.046
_oxdiff_exptl_absorpt_empirical_full_min 0.741
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1557229'
_audit_update_record             
;
2017-06-20 deposited with the CCDC.
2017-07-20 downloaded from the CCDC.
;
_audit_creation_date             2015-05-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H35 P'
_chemical_formula_sum            'C24 H35 P'
_chemical_formula_weight         354.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C24 H35 P1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
P P 0.2955 0.4335 '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                   7.75472(8)
_cell_length_b                   19.0684(2)
_cell_length_c                   14.79343(17)
_cell_angle_alpha                90
_cell_angle_beta                 90.1101(10)
_cell_angle_gamma                90
_cell_volume                     2187.51(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14016
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      66.6290
_cell_measurement_theta_min      3.7640
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.108
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.870
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31461
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.936
_diffrn_reflns_theta_min         2.317
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -86.00  -48.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.5905  138.0000  -48.0000 38

#__ type_ start__ end____ width___ exp.time_
  2 omega   69.00  116.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5905  131.0000  136.0000 47

#__ type_ start__ end____ width___ exp.time_
  3 omega   14.00  106.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   57.0000 -120.0000 92

#__ type_ start__ end____ width___ exp.time_
  4 omega   51.00   85.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5905 -138.0000 -109.0000 34

#__ type_ start__ end____ width___ exp.time_
  5 omega   15.00  113.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   38.0000  150.0000 98

#__ type_ start__ end____ width___ exp.time_
  6 omega   60.00  132.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000 -110.4725 72

#__ type_ start__ end____ width___ exp.time_
  7 omega   78.00  118.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000   -2.8723 40

#__ type_ start__ end____ width___ exp.time_
  8 omega   15.00   41.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  167.1857 26

#__ type_ start__ end____ width___ exp.time_
  9 omega   51.00  118.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000 -120.0000 67

#__ type_ start__ end____ width___ exp.time_
 10 omega   21.00   77.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -180.0000 56

#__ type_ start__ end____ width___ exp.time_
 11 omega   25.00   75.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -120.0000 50

#__ type_ start__ end____ width___ exp.time_
 12 omega  106.00  165.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000    0.0000 59

#__ type_ start__ end____ width___ exp.time_
 13 omega   65.00   95.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000  -90.0000 30

#__ type_ start__ end____ width___ exp.time_
 14 omega   38.00   67.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -30.0000 29

#__ type_ start__ end____ width___ exp.time_
 15 omega   10.00   41.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000   -2.8723 31

#__ type_ start__ end____ width___ exp.time_
 16 omega   51.00  103.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000   90.0000 52

#__ type_ start__ end____ width___ exp.time_
 17 omega   57.00   87.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000   90.0000 30

#__ type_ start__ end____ width___ exp.time_
 18 omega   43.00   68.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  -30.0000 25

#__ type_ start__ end____ width___ exp.time_
 19 omega   26.00   51.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000   90.0000 25

#__ type_ start__ end____ width___ exp.time_
 20 omega   21.00   57.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -90.0000 36

#__ type_ start__ end____ width___ exp.time_
 21 omega   23.00   49.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
 22 omega   29.00   72.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000 -150.0000 43

#__ type_ start__ end____ width___ exp.time_
 23 omega   17.00   82.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  150.0000 65

#__ type_ start__ end____ width___ exp.time_
 24 omega   71.00   97.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
 25 omega   55.00  175.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000  -60.0000 120

#__ type_ start__ end____ width___ exp.time_
 26 omega   80.00  107.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  167.1857 27

#__ type_ start__ end____ width___ exp.time_
 27 omega   87.00  123.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  107.4598 36

#__ type_ start__ end____ width___ exp.time_
 28 omega   15.00   41.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 29 omega   42.00   68.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 30 omega  103.00  141.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000 -180.0000 38

#__ type_ start__ end____ width___ exp.time_
 31 omega   47.00   74.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -60.0000 27

#__ type_ start__ end____ width___ exp.time_
 32 omega   48.00   77.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000  120.0000 29

#__ type_ start__ end____ width___ exp.time_
 33 omega   52.00   96.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000  150.0000 44

#__ type_ start__ end____ width___ exp.time_
 34 omega   10.00   59.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  107.4598 49

#__ type_ start__ end____ width___ exp.time_
 35 omega    8.00  120.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   77.0000    0.0000 112

#__ type_ start__ end____ width___ exp.time_
 36 omega   65.00  115.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5905  138.0000  -48.0000 50

#__ type_ start__ end____ width___ exp.time_
 37 omega    8.00  120.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   77.0000  -90.0000 112

#__ type_ start__ end____ width___ exp.time_
 38 omega    8.00  120.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   77.0000 -180.0000 112

#__ type_ start__ end____ width___ exp.time_
 39 omega    8.00  120.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   77.0000   90.0000 112

#__ type_ start__ end____ width___ exp.time_
 40 omega   66.00  168.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000 -180.0000 102

#__ type_ start__ end____ width___ exp.time_
 41 omega   66.00  168.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000   90.0000 102

#__ type_ start__ end____ width___ exp.time_
 42 omega   63.00  145.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000   30.0000 82
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.1915362000
_diffrn_orient_matrix_UB_12      0.0153843000
_diffrn_orient_matrix_UB_13      -0.0191953000
_diffrn_orient_matrix_UB_21      0.0360488000
_diffrn_orient_matrix_UB_22      -0.0792880000
_diffrn_orient_matrix_UB_23      -0.0065862000
_diffrn_orient_matrix_UB_31      -0.0386268000
_diffrn_orient_matrix_UB_32      0.0021732000
_diffrn_orient_matrix_UB_33      -0.1021205000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3578
_reflns_number_total             3874
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.124
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3874
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0337
_refine_ls_restrained_S_all      1.035
_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)+(0.0442P)²+0.4735P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0866
_refine_special_details          
'The crystal is twinned but psuedo-merohedry. One isopropyl group and the hydrogen bound to phosphorus have been modelled as disordered over two positions. The occupancies of the two parts were allowed to refine with isotropc atom treatment. Upon convergence, the occupancies were fixed before anisotropy was introduced to the model. Restraints were applied as appropriate.'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.8158(11) 0.1842(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All P(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C23B-C22 \\sim C23A-C22
 with sigma of 0.02
 C24B-C22 \\sim C24A-C22
 with sigma of 0.02
 C24A-C23A \\sim C24B-C23B
 with sigma of 0.02
 P1-H1B \\sim P1-H1A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C23B) = Uanis(C23A)
Uanis(C24B) = Uanis(C24A)
5. Others
 Fixed Sof: H1A(0.52006) H1B(0.47994) H22(0.52006) H22A(0.47994) C23A(0.52006)
 H23A(0.52006) H23B(0.52006) H23C(0.52006) C24A(0.52006) H24A(0.52006)
 H24B(0.52006) H24C(0.52006) C23B(0.47994) H23D(0.47994) H23E(0.47994)
 H23F(0.47994) C24B(0.47994) H24D(0.47994) H24E(0.47994) H24F(0.47994)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22), C22(H22A)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23A(H23A,H23B,H23C), C24A(H24A,H24B,
 H24C), C23B(H23D,H23E,H23F), C24B(H24D,H24E,H24F)
;
_atom_sites_solution_hydrogens   mixed
_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
P1 P 0.49586(6) 0.68172(2) 0.39493(3) 0.03236(12) Uani 1 1 d D . . . .
H1A H 0.544(4) 0.6395(17) 0.454(2) 0.039 Uiso 0.5201 1 d DR . P A 1
H1B H 0.361(4) 0.7193(18) 0.391(3) 0.039 Uiso 0.4799 1 d DR . P B 2
C1 C 0.49420(19) 0.63250(7) 0.28689(9) 0.0258(3) Uani 1 1 d . . . . .
C2 C 0.4805(2) 0.66998(8) 0.20492(10) 0.0312(3) Uani 1 1 d . . . . .
C3 C 0.4793(3) 0.63345(9) 0.12339(11) 0.0450(4) Uani 1 1 d . . . . .
H3 H 0.4721 0.6587 0.0682 0.054 Uiso 1 1 calc R . . . .
C4 C 0.4883(3) 0.56148(9) 0.12143(12) 0.0530(5) Uani 1 1 d . . . . .
H4 H 0.4885 0.5373 0.0653 0.064 Uiso 1 1 calc R . . . .
C5 C 0.4970(3) 0.52445(8) 0.20146(11) 0.0429(4) Uani 1 1 d . . . . .
H5 H 0.5014 0.4747 0.1996 0.052 Uiso 1 1 calc R . . . .
C6 C 0.4994(2) 0.55819(7) 0.28472(10) 0.0301(3) Uani 1 1 d . . . . .
C7 C 0.4647(2) 0.74935(8) 0.19970(11) 0.0358(4) Uani 1 1 d . . . . .
H7 H 0.4559 0.7675 0.2629 0.043 Uiso 1 1 calc R . . . .
C8 C 0.6242(3) 0.78222(11) 0.15697(14) 0.0498(5) Uani 1 1 d . . . . .
H8A H 0.7266 0.7691 0.1920 0.075 Uiso 1 1 calc GR . . . .
H8B H 0.6120 0.8334 0.1567 0.075 Uiso 1 1 calc GR . . . .
H8C H 0.6363 0.7653 0.0948 0.075 Uiso 1 1 calc GR . . . .
C9 C 0.3005(3) 0.77122(10) 0.14937(13) 0.0444(4) Uani 1 1 d . . . . .
H9A H 0.3077 0.7559 0.0862 0.067 Uiso 1 1 calc GR . . . .
H9B H 0.2885 0.8224 0.1516 0.067 Uiso 1 1 calc GR . . . .
H9C H 0.2002 0.7494 0.1781 0.067 Uiso 1 1 calc GR . . . .
C10 C 0.5024(2) 0.51094(7) 0.36805(10) 0.0336(3) Uani 1 1 d . . . . .
H10 H 0.5123 0.5415 0.4228 0.040 Uiso 1 1 calc R . . . .
C11 C 0.3349(2) 0.46983(10) 0.37475(16) 0.0501(5) Uani 1 1 d . . . . .
H11A H 0.3215 0.4402 0.3211 0.075 Uiso 1 1 calc GR . . . .
H11B H 0.2377 0.5025 0.3786 0.075 Uiso 1 1 calc GR . . . .
H11C H 0.3375 0.4403 0.4289 0.075 Uiso 1 1 calc GR . . . .
C12 C 0.6545(2) 0.46014(10) 0.36807(15) 0.0490(5) Uani 1 1 d . . . . .
H12A H 0.6425 0.4273 0.3175 0.073 Uiso 1 1 calc GR . . . .
H12B H 0.6563 0.4340 0.4251 0.073 Uiso 1 1 calc GR . . . .
H12C H 0.7622 0.4865 0.3616 0.073 Uiso 1 1 calc GR . . . .
C13 C 0.68508(18) 0.74069(7) 0.38681(9) 0.0245(3) Uani 1 1 d . . . . .
C14 C 0.85125(19) 0.71257(8) 0.37314(10) 0.0271(3) Uani 1 1 d . . . . .
C15 C 0.9917(2) 0.75798(8) 0.36698(10) 0.0332(3) Uani 1 1 d . . . . .
H15 H 1.1036 0.7393 0.3570 0.040 Uiso 1 1 calc R . . . .
C16 C 0.9711(2) 0.82968(8) 0.37507(11) 0.0355(4) Uani 1 1 d . . . . .
H16 H 1.0679 0.8599 0.3702 0.043 Uiso 1 1 calc R . . . .
C17 C 0.8090(2) 0.85718(8) 0.39031(11) 0.0321(3) Uani 1 1 d . . . . .
H17 H 0.7959 0.9065 0.3964 0.039 Uiso 1 1 calc R . . . .
C18 C 0.66390(19) 0.81421(7) 0.39693(10) 0.0262(3) Uani 1 1 d . . . . .
C19 C 0.8867(2) 0.63428(8) 0.36729(11) 0.0297(3) Uani 1 1 d . . . . .
H19 H 0.7735 0.6096 0.3728 0.036 Uiso 1 1 calc R . . . .
C20 C 0.9650(3) 0.61349(9) 0.27639(12) 0.0434(4) Uani 1 1 d . . . . .
H20A H 1.0770 0.6366 0.2691 0.065 Uiso 1 1 calc GR . . . .
H20B H 0.8876 0.6280 0.2274 0.065 Uiso 1 1 calc GR . . . .
H20C H 0.9807 0.5625 0.2744 0.065 Uiso 1 1 calc GR . . . .
C21 C 0.9997(2) 0.61031(8) 0.44615(11) 0.0368(3) Uani 1 1 d . . . . .
H21A H 1.1154 0.6303 0.4397 0.055 Uiso 1 1 calc GR . . . .
H21B H 1.0073 0.5590 0.4462 0.055 Uiso 1 1 calc GR . . . .
H21C H 0.9488 0.6263 0.5032 0.055 Uiso 1 1 calc GR . . . .
C22 C 0.4911(2) 0.84864(8) 0.41851(10) 0.0325(3) Uani 1 1 d D . . . .
H22 H 0.3986 0.8140 0.4034 0.039 Uiso 0.5201 1 calc R . P C 1
H22A H 0.3990 0.8201 0.3886 0.039 Uiso 0.4799 1 calc R . P D 2
C23A C 0.477(4) 0.8646(8) 0.5195(6) 0.059(3) Uani 0.5201 1 d D . P E 1
H23A H 0.3647 0.8855 0.5323 0.088 Uiso 0.5201 1 calc GR . P E 1
H23B H 0.5688 0.8974 0.5369 0.088 Uiso 0.5201 1 calc GR . P E 1
H23C H 0.4902 0.8210 0.5540 0.088 Uiso 0.5201 1 calc GR . P E 1
C24A C 0.457(3) 0.9149(5) 0.3615(8) 0.052(2) Uani 0.5201 1 d D . P E 1
H24A H 0.5463 0.9500 0.3747 0.077 Uiso 0.5201 1 calc GR . P E 1
H24B H 0.3438 0.9341 0.3765 0.077 Uiso 0.5201 1 calc GR . P E 1
H24C H 0.4609 0.9029 0.2972 0.077 Uiso 0.5201 1 calc GR . P E 1
C23B C 0.460(4) 0.8454(9) 0.5205(7) 0.059(3) Uani 0.4799 1 d D . P E 2
H23D H 0.3498 0.8680 0.5347 0.088 Uiso 0.4799 1 calc GR . P E 2
H23E H 0.5535 0.8698 0.5521 0.088 Uiso 0.4799 1 calc GR . P E 2
H23F H 0.4566 0.7963 0.5400 0.088 Uiso 0.4799 1 calc GR . P E 2
C24B C 0.475(3) 0.9240(6) 0.3830(10) 0.052(2) Uani 0.4799 1 d D . P E 2
H24D H 0.5460 0.9553 0.4201 0.077 Uiso 0.4799 1 calc GR . P E 2
H24E H 0.3541 0.9389 0.3861 0.077 Uiso 0.4799 1 calc GR . P E 2
H24F H 0.5141 0.9259 0.3201 0.077 Uiso 0.4799 1 calc GR . P E 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 H1A 1.24(3) . ?
P1 H1B 1.27(3) . ?
P1 C1 1.8536(14) . ?
P1 C13 1.8527(15) . ?
C1 C2 1.411(2) . ?
C1 C6 1.418(2) . ?
C2 C3 1.393(2) . ?
C2 C7 1.520(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.374(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.380(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.390(2) . ?
C6 C10 1.527(2) . ?
C7 H7 1.0000 . ?
C7 C8 1.525(3) . ?
C7 C9 1.532(2) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 1.0000 . ?
C10 C11 1.521(3) . ?
C10 C12 1.526(2) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.411(2) . ?
C13 C18 1.420(2) . ?
C14 C15 1.394(2) . ?
C14 C19 1.521(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.382(2) . ?
C16 H16 0.9500 . ?
C16 C17 1.381(2) . ?
C17 H17 0.9500 . ?
C17 C18 1.395(2) . ?
C18 C22 1.527(2) . ?
C19 H19 1.0000 . ?
C19 C20 1.529(2) . ?
C19 C21 1.528(2) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22 1.0000 . ?
C22 H22A 1.0000 . ?
C22 C23A 1.528(10) . ?
C22 C24A 1.542(9) . ?
C22 C23B 1.529(10) . ?
C22 C24B 1.535(10) . ?
C23A H23A 0.9800 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C24A H24A 0.9800 . ?
C24A H24B 0.9800 . ?
C24A H24C 0.9800 . ?
C23B H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C24B H24D 0.9800 . ?
C24B H24E 0.9800 . ?
C24B H24F 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
C1 P1 H1A 106.2(16) . . ?
C1 P1 H1B 103.9(17) . . ?
C13 P1 H1A 101.6(16) . . ?
C13 P1 H1B 108.0(17) . . ?
C13 P1 C1 104.81(7) . . ?
C2 C1 P1 119.00(10) . . ?
C2 C1 C6 119.26(12) . . ?
C6 C1 P1 121.69(10) . . ?
C1 C2 C7 123.62(13) . . ?
C3 C2 C1 119.41(14) . . ?
C3 C2 C7 116.97(13) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 C2 121.16(15) . . ?
C4 C3 H3 119.4 . . ?
C3 C4 H4 120.2 . . ?
C3 C4 C5 119.68(15) . . ?
C5 C4 H4 120.2 . . ?
C4 C5 H5 119.2 . . ?
C4 C5 C6 121.60(15) . . ?
C6 C5 H5 119.2 . . ?
C1 C6 C10 124.88(12) . . ?
C5 C6 C1 118.84(13) . . ?
C5 C6 C10 116.26(13) . . ?
C2 C7 H7 107.6 . . ?
C2 C7 C8 111.43(15) . . ?
C2 C7 C9 111.23(14) . . ?
C8 C7 H7 107.6 . . ?
C8 C7 C9 111.14(14) . . ?
C9 C7 H7 107.6 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 H10 108.1 . . ?
C11 C10 C6 110.17(15) . . ?
C11 C10 H10 108.1 . . ?
C11 C10 C12 109.45(13) . . ?
C12 C10 C6 112.68(14) . . ?
C12 C10 H10 108.1 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 P1 120.16(11) . . ?
C14 C13 C18 119.76(13) . . ?
C18 C13 P1 120.05(11) . . ?
C13 C14 C19 123.14(13) . . ?
C15 C14 C13 119.15(14) . . ?
C15 C14 C19 117.69(13) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 C14 121.23(15) . . ?
C16 C15 H15 119.4 . . ?
C15 C16 H16 120.2 . . ?
C17 C16 C15 119.69(15) . . ?
C17 C16 H16 120.2 . . ?
C16 C17 H17 119.2 . . ?
C16 C17 C18 121.52(14) . . ?
C18 C17 H17 119.2 . . ?
C13 C18 C22 123.27(13) . . ?
C17 C18 C13 118.63(13) . . ?
C17 C18 C22 118.06(13) . . ?
C14 C19 H19 107.4 . . ?
C14 C19 C20 112.14(13) . . ?
C14 C19 C21 110.72(12) . . ?
C20 C19 H19 107.4 . . ?
C21 C19 H19 107.4 . . ?
C21 C19 C20 111.48(13) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22 H22 107.4 . . ?
C18 C22 H22A 107.5 . . ?
C18 C22 C23A 110.6(11) . . ?
C18 C22 C24A 112.7(9) . . ?
C18 C22 C23B 109.2(12) . . ?
C18 C22 C24B 113.7(10) . . ?
C23A C22 H22 107.4 . . ?
C23A C22 C24A 111.1(7) . . ?
C24A C22 H22 107.4 . . ?
C23B C22 H22A 107.5 . . ?
C23B C22 C24B 111.2(8) . . ?
C24B C22 H22A 107.5 . . ?
C22 C23A H23A 109.5 . . ?
C22 C23A H23B 109.5 . . ?
C22 C23A H23C 109.5 . . ?
H23A C23A H23B 109.5 . . ?
H23A C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C22 C24A H24A 109.5 . . ?
C22 C24A H24B 109.5 . . ?
C22 C24A H24C 109.5 . . ?
H24A C24A H24B 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C22 C23B H23D 109.5 . . ?
C22 C23B H23E 109.5 . . ?
C22 C23B H23F 109.5 . . ?
H23D C23B H23E 109.5 . . ?
H23D C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C22 C24B H24D 109.5 . . ?
C22 C24B H24E 109.5 . . ?
C22 C24B H24F 109.5 . . ?
H24D C24B H24E 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?

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
P1 C1 C2 C3 179.94(14) . . . . ?
P1 C1 C2 C7 -0.7(2) . . . . ?
P1 C1 C6 C5 179.70(14) . . . . ?
P1 C1 C6 C10 1.5(2) . . . . ?
P1 C13 C14 C15 179.81(11) . . . . ?
P1 C13 C14 C19 -2.0(2) . . . . ?
P1 C13 C18 C17 -179.91(11) . . . . ?
P1 C13 C18 C22 2.6(2) . . . . ?
C1 P1 C13 C14 -58.26(13) . . . . ?
C1 P1 C13 C18 123.55(12) . . . . ?
C1 C2 C3 C4 1.1(3) . . . . ?
C1 C2 C7 C8 112.95(18) . . . . ?
C1 C2 C7 C9 -122.43(18) . . . . ?
C1 C6 C10 C11 112.31(18) . . . . ?
C1 C6 C10 C12 -125.14(18) . . . . ?
C2 C1 C6 C5 2.3(2) . . . . ?
C2 C1 C6 C10 -175.90(16) . . . . ?
C2 C3 C4 C5 0.6(3) . . . . ?
C3 C2 C7 C8 -67.7(2) . . . . ?
C3 C2 C7 C9 56.9(2) . . . . ?
C3 C4 C5 C6 -0.9(3) . . . . ?
C4 C5 C6 C1 -0.6(3) . . . . ?
C4 C5 C6 C10 177.81(19) . . . . ?
C5 C6 C10 C11 -65.9(2) . . . . ?
C5 C6 C10 C12 56.6(2) . . . . ?
C6 C1 C2 C3 -2.6(2) . . . . ?
C6 C1 C2 C7 176.78(15) . . . . ?
C7 C2 C3 C4 -178.28(19) . . . . ?
C13 P1 C1 C2 -59.56(14) . . . . ?
C13 P1 C1 C6 123.03(13) . . . . ?
C13 C14 C15 C16 0.8(2) . . . . ?
C13 C14 C19 C20 119.59(16) . . . . ?
C13 C14 C19 C21 -115.20(16) . . . . ?
C13 C18 C22 C23A 98.4(6) . . . . ?
C13 C18 C22 C24A -136.6(5) . . . . ?
C13 C18 C22 C23B 82.9(8) . . . . ?
C13 C18 C22 C24B -152.2(6) . . . . ?
C14 C13 C18 C17 1.9(2) . . . . ?
C14 C13 C18 C22 -175.57(14) . . . . ?
C14 C15 C16 C17 0.6(2) . . . . ?
C15 C14 C19 C20 -62.16(19) . . . . ?
C15 C14 C19 C21 63.04(19) . . . . ?
C15 C16 C17 C18 -0.6(2) . . . . ?
C16 C17 C18 C13 -0.6(2) . . . . ?
C16 C17 C18 C22 177.02(15) . . . . ?
C17 C18 C22 C23A -79.1(6) . . . . ?
C17 C18 C22 C24A 45.9(5) . . . . ?
C17 C18 C22 C23B -94.6(8) . . . . ?
C17 C18 C22 C24B 30.3(6) . . . . ?
C18 C13 C14 C15 -2.0(2) . . . . ?
C18 C13 C14 C19 176.23(14) . . . . ?
C19 C14 C15 C16 -177.54(14) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1 0 0 0.0456 -1.0000 -0.0000 0.0000 -0.1915 -0.0360 0.0386
0 -2 1 0.0606 -0.0000 -2.0000 1.0000 -0.0500 0.1520 -0.1065
0 2 -1 0.0646 0.0000 2.0000 -1.0000 0.0500 -0.1520 0.1065
0 -1 0 0.0365 0.0000 -1.0000 -0.0000 -0.0154 0.0793 -0.0022
0 1 0 0.0585 -0.0000 1.0000 0.0000 0.0154 -0.0793 0.0022
0 0 1 0.0783 -0.0000 -0.0000 1.0000 -0.0192 -0.0066 -0.1021
0 0 -1 0.0573 0.0000 0.0000 -1.0000 0.0192 0.0066 0.1021
1 0 0 0.0786 1.0000 0.0000 -0.0000 0.1915 0.0360 -0.0386

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.8158(11)
2 0.1842(11)
####################################################################### 
# 
# 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_4a
_database_code_depnum_ccdc_archive 'CCDC 1557233'
_audit_update_record             
;
2017-06-20 deposited with the CCDC.
2017-07-20 downloaded from the CCDC.
;
_audit_creation_date             2015-03-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H66 K O4 P'
_chemical_formula_sum            'C40 H66 K O4 P'
_chemical_formula_weight         680.99
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C40 H66 O4 P1 K1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.7963(5)
_cell_length_b                   14.4308(3)
_cell_length_c                   16.6968(5)
_cell_angle_alpha                90
_cell_angle_beta                 91.061(3)
_cell_angle_gamma                90
_cell_volume                     4046.36(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    18381
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      66.7750
_cell_measurement_theta_min      2.6150
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.793
_exptl_absorpt_correction_T_max  0.716
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            56946
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.124
_diffrn_reflns_theta_min         2.631
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3968
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   15.00  110.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   38.0000 -180.0000 95

#__ type_ start__ end____ width___ exp.time_
  2 omega  -31.00   68.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5905  -38.0000    0.0000 99

#__ type_ start__ end____ width___ exp.time_
  3 omega   -2.00   87.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5905 -125.0000  -60.0000 89

#__ type_ start__ end____ width___ exp.time_
  4 omega   10.00   47.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000   28.2599 37

#__ type_ start__ end____ width___ exp.time_
  5 omega   83.00  110.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000 -101.2745 27

#__ type_ start__ end____ width___ exp.time_
  6 omega    9.00   76.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000   42.4033 67

#__ type_ start__ end____ width___ exp.time_
  7 omega   22.00   49.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000 -101.2745 27

#__ type_ start__ end____ width___ exp.time_
  8 omega   64.00  128.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  142.9780 64

#__ type_ start__ end____ width___ exp.time_
  9 omega   16.00  155.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000  120.0000 139

#__ type_ start__ end____ width___ exp.time_
 10 omega   20.00   47.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000   30.0000 27

#__ type_ start__ end____ width___ exp.time_
 11 omega   22.00   74.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -150.0000 52

#__ type_ start__ end____ width___ exp.time_
 12 omega   24.00   76.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   30.0000 52

#__ type_ start__ end____ width___ exp.time_
 13 omega   27.00   66.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000   90.0000 39

#__ type_ start__ end____ width___ exp.time_
 14 omega   20.00   70.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  150.0000 50

#__ type_ start__ end____ width___ exp.time_
 15 omega   45.00   79.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000   90.0000 34

#__ type_ start__ end____ width___ exp.time_
 16 omega   62.00   92.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000 -180.0000 30

#__ type_ start__ end____ width___ exp.time_
 17 omega   24.00   63.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  -60.0000 39

#__ type_ start__ end____ width___ exp.time_
 18 omega   80.00  107.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000  -30.0000 27

#__ type_ start__ end____ width___ exp.time_
 19 omega   12.00   90.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000    0.0000 78

#__ type_ start__ end____ width___ exp.time_
 20 omega   93.00  140.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000    0.0000 47

#__ type_ start__ end____ width___ exp.time_
 21 omega   23.00   50.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000   30.0000 27

#__ type_ start__ end____ width___ exp.time_
 22 omega   80.00  121.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000   30.0000 41

#__ type_ start__ end____ width___ exp.time_
 23 omega   88.00  115.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000   42.4033 27

#__ type_ start__ end____ width___ exp.time_
 24 omega   20.00   72.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -90.0000 52

#__ type_ start__ end____ width___ exp.time_
 25 omega   51.00   82.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  120.0000 31

#__ type_ start__ end____ width___ exp.time_
 26 omega   51.00   78.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000 -150.0000 27

#__ type_ start__ end____ width___ exp.time_
 27 omega   62.00  123.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000  -60.0000 61

#__ type_ start__ end____ width___ exp.time_
 28 omega   25.00   52.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000    0.0000 27

#__ type_ start__ end____ width___ exp.time_
 29 omega   63.00   95.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000    0.0000 32

#__ type_ start__ end____ width___ exp.time_
 30 omega   28.00   83.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  -90.0000 55

#__ type_ start__ end____ width___ exp.time_
 31 omega   67.00  100.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000   28.2599 33

#__ type_ start__ end____ width___ exp.time_
 32 omega  124.00  151.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000 -180.0000 27

#__ type_ start__ end____ width___ exp.time_
 33 omega   38.00   94.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000 -122.7409 56

#__ type_ start__ end____ width___ exp.time_
 34 omega   86.00  113.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000 -120.0000 27

#__ type_ start__ end____ width___ exp.time_
 35 omega  125.00  152.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000 -120.0000 27

#__ type_ start__ end____ width___ exp.time_
 36 omega   27.00   67.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000  -30.0000 40

#__ type_ start__ end____ width___ exp.time_
 37 omega   65.00  130.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000  -34.9578 65

#__ type_ start__ end____ width___ exp.time_
 38 omega   42.00   67.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   60.0000 25

#__ type_ start__ end____ width___ exp.time_
 39 omega   20.00   74.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   90.0000 54

#__ type_ start__ end____ width___ exp.time_
 40 omega   10.00   35.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000  -34.9578 25

#__ type_ start__ end____ width___ exp.time_
 41 omega -120.00  -24.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5905  -77.0000  150.0000 96

#__ type_ start__ end____ width___ exp.time_
 42 omega  -99.00  -18.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5905  125.0000  150.0000 81

#__ type_ start__ end____ width___ exp.time_
 43 omega    8.00  120.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   77.0000   90.0000 112

#__ type_ start__ end____ width___ exp.time_
 44 omega   12.00  116.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   57.0000  -90.0000 104

#__ type_ start__ end____ width___ exp.time_
 45 omega    8.00  120.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5905   77.0000    0.0000 112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0004529000
_diffrn_orient_matrix_UB_12      0.0704998000
_diffrn_orient_matrix_UB_13      -0.0693055000
_diffrn_orient_matrix_UB_21      0.0320911000
_diffrn_orient_matrix_UB_22      0.0750327000
_diffrn_orient_matrix_UB_23      0.0577916000
_diffrn_orient_matrix_UB_31      0.0859150000
_diffrn_orient_matrix_UB_32      -0.0282920000
_diffrn_orient_matrix_UB_33      -0.0193478000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6116
_reflns_number_total             7175
_reflns_odcompleteness_completeness 99.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         7175
_refine_ls_number_restraints     669
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0847
_refine_ls_restrained_S_all      1.038
_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)+(0.0598P)²+9.0929P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1995
_refine_ls_wR_factor_ref         0.2058
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 K1A-O2A \\sim K1-O2
 with sigma of 0.02
 K1-O4 \\sim K1A-O4A
 with sigma of 0.02
 K1A-P1 \\sim K1-P1
 with sigma of 0.02
 K1-O3 \\sim K1A-O3A
 with sigma of 0.02
 K1-O1 \\sim K1A-O1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(K1) = Uanis(K1A)
Uanis(O1) = Uanis(O1A)
Uanis(C28) = Uanis(C28A)
Uanis(C27) = Uanis(C27A)
Uanis(C26) = Uanis(C26A)
Uanis(C25) = Uanis(C25A)
Uanis(O3) = Uanis(O3A)
Uanis(C36) = Uanis(C36A)
Uanis(C35) = Uanis(C35A)
Uanis(C34) = Uanis(C34A)
Uanis(C33) = Uanis(C33A)
Uanis(O4) = Uanis(O4A)
Uanis(C37) = Uanis(C37A)
Uanis(C40) = Uanis(C40A)
Uanis(C38) = Uanis(C38A)
Uanis(C39) = Uanis(C39A)
Uanis(O2) = Uanis(O2A)
Uanis(C29) = Uanis(C29A)
Uanis(C30) = Uanis(C30A)
Uanis(C31) = Uanis(C31A)
Uanis(C32) = Uanis(C32A)
4. Rigid body (RIGU) restrains
 C39A, K1, O1, O2, O3, O4, P1, C39, C38, C37, K1A, O4A, C40A, C37A, C28, C25,
 C29, C32, C33, C36, C40, C11, C1, C13, O1A, O2A, O3A, C38A, C27, C26, C30, C31,
  C34, C35, C10, C2, C6, C14, C18, C28A, C25A, C29A, C32A, C33A, C36A, C26A,
 C12, C3, C7, C5, C15, C19, C17, C22, C27A, C30A, C31A, C34A, C35A, C4, C8, C9,
 C16, C20, C21, C23, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O1A, C28A, C27A, C26A, C25A} sigma for 1-2: 0.02, 1-3: 0.02
as
{O1, C28, C27, C26, C25}
{O2A, C29A, C30A, C31A, C32A} sigma for 1-2: 0.02, 1-3: 0.02
as
{O2, C29, C30, C31, C32}
{O3A, C33A, C34A, C35A, C36A} sigma for 1-2: 0.02, 1-3: 0.02
as
{O3, C33, C34, C35, C36}
{O4A, C40A, C39A, C38A, C37A} sigma for 1-2: 0.02, 1-3: 0.02
as
{O4, C40, C39, C38, C37}
6. Others
 Fixed Sof: K1(0.61606) O1(0.61606) C28(0.61606) H28A(0.61606) H28B(0.61606)
 C27(0.61606) H27A(0.61606) H27B(0.61606) C26(0.61606) H26A(0.61606)
 H26B(0.61606) C25(0.61606) H25A(0.61606) H25B(0.61606) O2(0.61606)
 C29(0.61606) H29A(0.61606) H29B(0.61606) C30(0.61606) H30A(0.61606)
 H30B(0.61606) C31(0.61606) H31A(0.61606) H31B(0.61606) C32(0.61606)
 H32A(0.61606) H32B(0.61606) O3(0.61606) C33(0.61606) H33A(0.61606)
 H33B(0.61606) C34(0.61606) H34A(0.61606) H34B(0.61606) C35(0.61606)
 H35A(0.61606) H35B(0.61606) C36(0.61606) H36A(0.61606) H36B(0.61606)
 O4(0.61606) C40(0.61606) H40A(0.61606) H40B(0.61606) C39(0.61606)
 H39A(0.61606) H39B(0.61606) C38(0.61606) H38A(0.61606) H38B(0.61606)
 C37(0.61606) H37A(0.61606) H37B(0.61606) K1A(0.38394) O1A(0.38394)
 C28A(0.38394) H28C(0.38394) H28D(0.38394) C27A(0.38394) H27C(0.38394)
 H27D(0.38394) C26A(0.38394) H26C(0.38394) H26D(0.38394) C25A(0.38394)
 H25C(0.38394) H25D(0.38394) O3A(0.38394) C33A(0.38394) H33C(0.38394)
 H33D(0.38394) C34A(0.38394) H34C(0.38394) H34D(0.38394) C35A(0.38394)
 H35C(0.38394) H35D(0.38394) C36A(0.38394) H36C(0.38394) H36D(0.38394)
 O4A(0.38394) C40A(0.38394) H40C(0.38394) H40D(0.38394) C39A(0.38394)
 H39C(0.38394) H39D(0.38394) C38A(0.38394) H38C(0.38394) H38D(0.38394)
 C37A(0.38394) H37C(0.38394) H37D(0.38394) O2A(0.38394) C29A(0.38394)
 H29C(0.38394) H29D(0.38394) C30A(0.38394) H30C(0.38394) H30D(0.38394)
 C31A(0.38394) H31C(0.38394) H31D(0.38394) C32A(0.38394) H32C(0.38394)
 H32D(0.38394)
7.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22)
7.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C27(H27A,H27B), C26(H26A,H26B), C25(H25A,H25B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C40(H40A,H40B), C39(H39A,H39B),
  C38(H38A,H38B), C37(H37A,H37B), C28A(H28C,H28D), C27A(H27C,H27D), C26A(H26C,
 H26D), C25A(H25C,H25D), C33A(H33C,H33D), C34A(H34C,H34D), C35A(H35C,H35D),
 C36A(H36C,H36D), C40A(H40C,H40D), C39A(H39C,H39D), C38A(H38C,H38D), C37A(H37C,
 H37D), C29A(H29C,H29D), C30A(H30C,H30D), C31A(H31C,H31D), C32A(H32C,H32D)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17)
7.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C)
;
_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
K1 K 0.26499(11) 0.76905(13) 0.77104(9) 0.0426(4) Uani 0.6161 1 d D U P A 1
P1 P 0.25722(5) 0.54696(6) 0.75342(5) 0.0369(2) Uani 1 1 d D U . . .
O1 O 0.3814(4) 0.7668(9) 0.6621(5) 0.068(2) Uani 0.6161 1 d D U P A 1
C28 C 0.4607(7) 0.7496(11) 0.6914(8) 0.070(2) Uani 0.6161 1 d D U P A 1
H28A H 0.4602 0.7320 0.7487 0.084 Uiso 0.6161 1 calc R . P A 1
H28B H 0.4942 0.8055 0.6855 0.084 Uiso 0.6161 1 calc R . P A 1
C27 C 0.4927(12) 0.670(2) 0.6407(14) 0.0750(17) Uani 0.6161 1 d D U P A 1
H27A H 0.5508 0.6755 0.6334 0.090 Uiso 0.6161 1 calc R . P A 1
H27B H 0.4810 0.6090 0.6653 0.090 Uiso 0.6161 1 calc R . P A 1
C26 C 0.4480(11) 0.682(2) 0.5625(11) 0.072(2) Uani 0.6161 1 d D U P A 1
H26A H 0.4458 0.6230 0.5318 0.086 Uiso 0.6161 1 calc R . P A 1
H26B H 0.4721 0.7306 0.5293 0.086 Uiso 0.6161 1 calc R . P A 1
C25 C 0.3661(8) 0.7099(13) 0.5912(9) 0.071(2) Uani 0.6161 1 d D U P A 1
H25A H 0.3372 0.7458 0.5494 0.085 Uiso 0.6161 1 calc R . P A 1
H25B H 0.3342 0.6547 0.6049 0.085 Uiso 0.6161 1 calc R . P A 1
O2 O 0.1340(5) 0.7609(10) 0.8619(8) 0.0659(17) Uani 0.6161 1 d D U P A 1
C29 C 0.1397(6) 0.6880(7) 0.9213(8) 0.055(2) Uani 0.6161 1 d D U P A 1
H29A H 0.1668 0.7105 0.9707 0.066 Uiso 0.6161 1 calc R . P A 1
H29B H 0.1692 0.6341 0.9004 0.066 Uiso 0.6161 1 calc R . P A 1
C30 C 0.0551(6) 0.6631(6) 0.9371(6) 0.071(3) Uani 0.6161 1 d D U P A 1
H30A H 0.0424 0.6023 0.9125 0.085 Uiso 0.6161 1 calc R . P A 1
H30B H 0.0471 0.6582 0.9956 0.085 Uiso 0.6161 1 calc R . P A 1
C31 C 0.0067(4) 0.7285(6) 0.9061(6) 0.073(2) Uani 0.6161 1 d D U P A 1
H31A H -0.0216 0.7609 0.9494 0.087 Uiso 0.6161 1 calc R . P A 1
H31B H -0.0334 0.6999 0.8696 0.087 Uiso 0.6161 1 calc R . P A 1
C32 C 0.0568(6) 0.7950(6) 0.8615(6) 0.072(3) Uani 0.6161 1 d D U P A 1
H32A H 0.0365 0.8015 0.8058 0.087 Uiso 0.6161 1 calc R . P A 1
H32B H 0.0556 0.8566 0.8875 0.087 Uiso 0.6161 1 calc R . P A 1
O3 O 0.2195(4) 0.9047(4) 0.6681(4) 0.0719(17) Uani 0.6161 1 d D U P A 1
C33 C 0.1426(5) 0.9435(6) 0.6562(9) 0.073(2) Uani 0.6161 1 d D U P A 1
H33A H 0.1132 0.9447 0.7071 0.088 Uiso 0.6161 1 calc R . P A 1
H33B H 0.1115 0.9071 0.6163 0.088 Uiso 0.6161 1 calc R . P A 1
C34 C 0.1567(5) 1.0399(7) 0.6264(9) 0.091(3) Uani 0.6161 1 d D U P A 1
H34A H 0.1167 1.0573 0.5847 0.109 Uiso 0.6161 1 calc R . P A 1
H34B H 0.1548 1.0854 0.6707 0.109 Uiso 0.6161 1 calc R . P A 1
C35 C 0.2380(6) 1.0345(8) 0.5925(13) 0.123(4) Uani 0.6161 1 d D U P A 1
H35A H 0.2352 1.0427 0.5337 0.147 Uiso 0.6161 1 calc R . P A 1
H35B H 0.2721 1.0842 0.6155 0.147 Uiso 0.6161 1 calc R . P A 1
C36 C 0.2697(8) 0.9493(8) 0.6110(9) 0.102(4) Uani 0.6161 1 d D U P A 1
H36A H 0.3241 0.9568 0.6339 0.122 Uiso 0.6161 1 calc R . P A 1
H36B H 0.2729 0.9110 0.5620 0.122 Uiso 0.6161 1 calc R . P A 1
O4 O 0.3152(4) 0.8943(4) 0.8911(4) 0.0789(16) Uani 0.6161 1 d D U P A 1
C40 C 0.2488(7) 0.9487(6) 0.9257(7) 0.081(2) Uani 0.6161 1 d D U P A 1
H40A H 0.2005 0.9100 0.9304 0.097 Uiso 0.6161 1 calc R . P A 1
H40B H 0.2639 0.9726 0.9795 0.097 Uiso 0.6161 1 calc R . P A 1
C39 C 0.2350(6) 1.0249(7) 0.8697(9) 0.094(3) Uani 0.6161 1 d D U P A 1
H39A H 0.2024 1.0046 0.8229 0.113 Uiso 0.6161 1 calc R . P A 1
H39B H 0.2082 1.0776 0.8960 0.113 Uiso 0.6161 1 calc R . P A 1
C38 C 0.3147(7) 1.0493(7) 0.8465(12) 0.098(3) Uani 0.6161 1 d D U P A 1
H38A H 0.3364 1.0985 0.8820 0.117 Uiso 0.6161 1 calc R . P A 1
H38B H 0.3145 1.0722 0.7906 0.117 Uiso 0.6161 1 calc R . P A 1
C37 C 0.3633(5) 0.9645(7) 0.8539(8) 0.082(3) Uani 0.6161 1 d D U P A 1
H37A H 0.3800 0.9435 0.8003 0.098 Uiso 0.6161 1 calc R . P A 1
H37B H 0.4116 0.9769 0.8870 0.098 Uiso 0.6161 1 calc R . P A 1
C1 C 0.29096(19) 0.4612(2) 0.82857(17) 0.0317(6) Uani 1 1 d . U . . .
C2 C 0.2433(2) 0.3862(2) 0.85368(18) 0.0359(7) Uani 1 1 d . U . . .
C3 C 0.2746(2) 0.3207(2) 0.9075(2) 0.0438(8) Uani 1 1 d . U . . .
H3 H 0.2428 0.2692 0.9221 0.053 Uiso 1 1 calc R . . . .
C4 C 0.3498(2) 0.3291(3) 0.9397(2) 0.0506(9) Uani 1 1 d . U . . .
H4 H 0.3706 0.2828 0.9747 0.061 Uiso 1 1 calc R . . . .
C5 C 0.3949(2) 0.4055(3) 0.9207(2) 0.0449(8) Uani 1 1 d . U . . .
H5 H 0.4457 0.4133 0.9457 0.054 Uiso 1 1 calc R . . . .
C6 C 0.3677(2) 0.4716(2) 0.86590(18) 0.0365(7) Uani 1 1 d . U . . .
C7 C 0.1562(2) 0.3750(3) 0.8285(2) 0.0454(8) Uani 1 1 d . U . . .
H7 H 0.1428 0.4266 0.7906 0.054 Uiso 1 1 calc R . . . .
C8 C 0.1385(3) 0.2849(3) 0.7853(3) 0.0707(13) Uani 1 1 d . U . . .
H8A H 0.1709 0.2809 0.7373 0.106 Uiso 1 1 calc GR . . . .
H8B H 0.0820 0.2827 0.7699 0.106 Uiso 1 1 calc GR . . . .
H8C H 0.1512 0.2327 0.8209 0.106 Uiso 1 1 calc GR . . . .
C9 C 0.1023(2) 0.3855(3) 0.9011(2) 0.0587(10) Uani 1 1 d . U . . .
H9A H 0.1129 0.3349 0.9390 0.088 Uiso 1 1 calc GR . . . .
H9B H 0.0464 0.3833 0.8833 0.088 Uiso 1 1 calc GR . . . .
H9C H 0.1131 0.4450 0.9274 0.088 Uiso 1 1 calc GR . . . .
C10 C 0.4189(2) 0.5551(2) 0.8479(2) 0.0439(8) Uani 1 1 d . U . . .
H10 H 0.4054 0.5752 0.7920 0.053 Uiso 1 1 calc R . . . .
C11 C 0.3974(3) 0.6355(3) 0.9039(3) 0.0598(11) Uani 1 1 d . U . . .
H11A H 0.3401 0.6477 0.8996 0.090 Uiso 1 1 calc GR . . . .
H11B H 0.4269 0.6911 0.8884 0.090 Uiso 1 1 calc GR . . . .
H11C H 0.4116 0.6190 0.9592 0.090 Uiso 1 1 calc GR . . . .
C12 C 0.5083(2) 0.5371(3) 0.8519(3) 0.0616(11) Uani 1 1 d . U . . .
H12A H 0.5247 0.5239 0.9074 0.092 Uiso 1 1 calc GR . . . .
H12B H 0.5367 0.5919 0.8329 0.092 Uiso 1 1 calc GR . . . .
H12C H 0.5210 0.4839 0.8180 0.092 Uiso 1 1 calc GR . . . .
C13 C 0.2166(2) 0.4750(2) 0.67124(17) 0.0345(7) Uani 1 1 d . U . . .
C14 C 0.1410(2) 0.4959(2) 0.63651(19) 0.0385(7) Uani 1 1 d . U . . .
C15 C 0.1104(2) 0.4426(3) 0.5736(2) 0.0518(9) Uani 1 1 d . U . . .
H15 H 0.0601 0.4582 0.5504 0.062 Uiso 1 1 calc R . . . .
C16 C 0.1518(3) 0.3675(3) 0.5441(2) 0.0576(10) Uani 1 1 d . U . . .
H16 H 0.1294 0.3299 0.5027 0.069 Uiso 1 1 calc R . . . .
C17 C 0.2265(3) 0.3483(3) 0.5760(2) 0.0518(9) Uani 1 1 d . U . . .
H17 H 0.2555 0.2974 0.5554 0.062 Uiso 1 1 calc R . . . .
C18 C 0.2605(2) 0.4011(2) 0.63756(19) 0.0410(8) Uani 1 1 d . U . . .
C19 C 0.0924(2) 0.5774(3) 0.6657(2) 0.0469(9) Uani 1 1 d . U . . .
H19 H 0.1106 0.5912 0.7219 0.056 Uiso 1 1 calc R . . . .
C20 C 0.1095(4) 0.6630(3) 0.6155(3) 0.0844(15) Uani 1 1 d . U . . .
H20A H 0.1672 0.6728 0.6136 0.127 Uiso 1 1 calc GR . . A .
H20B H 0.0843 0.7172 0.6396 0.127 Uiso 1 1 calc GR . . A .
H20C H 0.0882 0.6539 0.5611 0.127 Uiso 1 1 calc GR . . A .
C21 C 0.0029(3) 0.5588(4) 0.6678(3) 0.0822(15) Uani 1 1 d . U . . .
H21A H -0.0183 0.5534 0.6129 0.123 Uiso 1 1 calc GR . . . .
H21B H -0.0236 0.6101 0.6950 0.123 Uiso 1 1 calc GR . . . .
H21C H -0.0068 0.5010 0.6968 0.123 Uiso 1 1 calc GR . . . .
C22 C 0.3457(2) 0.3784(3) 0.6623(2) 0.0539(10) Uani 1 1 d . U . . .
H22 H 0.3600 0.4185 0.7092 0.065 Uiso 1 1 calc R . . . .
C23 C 0.3575(3) 0.2784(4) 0.6882(3) 0.0844(16) Uani 1 1 d . U . . .
H23A H 0.3246 0.2655 0.7347 0.127 Uiso 1 1 calc GR . . . .
H23B H 0.4137 0.2680 0.7024 0.127 Uiso 1 1 calc GR . . . .
H23C H 0.3418 0.2370 0.6441 0.127 Uiso 1 1 calc GR . . . .
C24 C 0.4029(3) 0.4026(3) 0.5950(3) 0.0608(11) Uani 1 1 d . U . . .
H24A H 0.3894 0.3659 0.5473 0.091 Uiso 1 1 calc GR . . . .
H24B H 0.4577 0.3887 0.6125 0.091 Uiso 1 1 calc GR . . . .
H24C H 0.3983 0.4687 0.5822 0.091 Uiso 1 1 calc GR . . . .
K1A K 0.24405(19) 0.7685(2) 0.74129(16) 0.0426(4) Uani 0.3839 1 d D U P A 2
O1A O 0.3662(8) 0.7616(16) 0.6387(9) 0.068(2) Uani 0.3839 1 d D U P A 2
C28A C 0.4405(12) 0.758(2) 0.6821(14) 0.070(2) Uani 0.3839 1 d D U P A 2
H28C H 0.4314 0.7449 0.7395 0.084 Uiso 0.3839 1 calc R . P A 2
H28D H 0.4692 0.8175 0.6777 0.084 Uiso 0.3839 1 calc R . P A 2
C27A C 0.489(2) 0.680(3) 0.645(2) 0.0750(17) Uani 0.3839 1 d D U P A 2
H27C H 0.5457 0.6964 0.6422 0.090 Uiso 0.3839 1 calc R . P A 2
H27D H 0.4832 0.6215 0.6754 0.090 Uiso 0.3839 1 calc R . P A 2
C26A C 0.4528(18) 0.670(4) 0.5624(19) 0.072(2) Uani 0.3839 1 d D U P A 2
H26C H 0.4597 0.6064 0.5414 0.086 Uiso 0.3839 1 calc R . P A 2
H26D H 0.4764 0.7147 0.5246 0.086 Uiso 0.3839 1 calc R . P A 2
C25A C 0.3655(14) 0.692(2) 0.5767(16) 0.071(2) Uani 0.3839 1 d D U P A 2
H25C H 0.3393 0.7153 0.5271 0.085 Uiso 0.3839 1 calc R . P A 2
H25D H 0.3368 0.6355 0.5945 0.085 Uiso 0.3839 1 calc R . P A 2
O3A O 0.1979(7) 0.9041(7) 0.6357(7) 0.0719(17) Uani 0.3839 1 d D U P A 2
C33A C 0.1436(9) 0.9777(10) 0.6514(15) 0.073(2) Uani 0.3839 1 d D U P A 2
H33C H 0.1274 0.9764 0.7081 0.088 Uiso 0.3839 1 calc R . P A 2
H33D H 0.0953 0.9719 0.6169 0.088 Uiso 0.3839 1 calc R . P A 2
C34A C 0.1866(10) 1.0663(9) 0.6335(16) 0.091(3) Uani 0.3839 1 d D U P A 2
H34C H 0.1576 1.1025 0.5919 0.109 Uiso 0.3839 1 calc R . P A 2
H34D H 0.1927 1.1048 0.6824 0.109 Uiso 0.3839 1 calc R . P A 2
C35A C 0.2651(11) 1.0358(11) 0.605(2) 0.123(4) Uani 0.3839 1 d D U P A 2
H35C H 0.2811 1.0732 0.5579 0.147 Uiso 0.3839 1 calc R . P A 2
H35D H 0.3063 1.0422 0.6474 0.147 Uiso 0.3839 1 calc R . P A 2
C36A C 0.2556(13) 0.9452(12) 0.5836(17) 0.102(4) Uani 0.3839 1 d D U P A 2
H36C H 0.3071 0.9121 0.5890 0.122 Uiso 0.3839 1 calc R . P A 2
H36D H 0.2369 0.9406 0.5272 0.122 Uiso 0.3839 1 calc R . P A 2
O4A O 0.3176(7) 0.8881(7) 0.8546(6) 0.0789(16) Uani 0.3839 1 d D U P A 2
C40A C 0.2636(12) 0.9191(11) 0.9245(11) 0.081(2) Uani 0.3839 1 d D U P A 2
H40C H 0.2277 0.8688 0.9421 0.097 Uiso 0.3839 1 calc R . P A 2
H40D H 0.2949 0.9428 0.9710 0.097 Uiso 0.3839 1 calc R . P A 2
C39A C 0.2208(10) 0.9923(13) 0.8824(15) 0.094(3) Uani 0.3839 1 d D U P A 2
H39C H 0.1845 1.0267 0.9178 0.113 Uiso 0.3839 1 calc R . P A 2
H39D H 0.1909 0.9690 0.8349 0.113 Uiso 0.3839 1 calc R . P A 2
C38A C 0.2915(13) 1.0481(10) 0.8602(19) 0.098(3) Uani 0.3839 1 d D U P A 2
H38C H 0.3143 1.0809 0.9074 0.117 Uiso 0.3839 1 calc R . P A 2
H38D H 0.2776 1.0941 0.8182 0.117 Uiso 0.3839 1 calc R . P A 2
C37A C 0.3482(10) 0.9767(12) 0.8295(14) 0.082(3) Uani 0.3839 1 d D U P A 2
H37C H 0.3507 0.9797 0.7704 0.098 Uiso 0.3839 1 calc R . P A 2
H37D H 0.4023 0.9870 0.8523 0.098 Uiso 0.3839 1 calc R . P A 2
O2A O 0.1388(8) 0.7453(17) 0.8615(13) 0.0659(17) Uani 0.3839 1 d D U P A 2
C29A C 0.1358(9) 0.6644(14) 0.9132(16) 0.055(2) Uani 0.3839 1 d D U P A 2
H29C H 0.1535 0.6803 0.9684 0.066 Uiso 0.3839 1 calc R . P A 2
H29D H 0.1703 0.6144 0.8927 0.066 Uiso 0.3839 1 calc R . P A 2
C30A C 0.0511(10) 0.6353(11) 0.9116(11) 0.071(3) Uani 0.3839 1 d D U P A 2
H30C H 0.0469 0.5704 0.8927 0.085 Uiso 0.3839 1 calc R . P A 2
H30D H 0.0296 0.6385 0.9663 0.085 Uiso 0.3839 1 calc R . P A 2
C31A C 0.0093(7) 0.6899(10) 0.8633(9) 0.073(2) Uani 0.3839 1 d D U P A 2
H31C H -0.0363 0.7162 0.8923 0.087 Uiso 0.3839 1 calc R . P A 2
H31D H -0.0118 0.6537 0.8172 0.087 Uiso 0.3839 1 calc R . P A 2
C32A C 0.0609(9) 0.7657(9) 0.8344(10) 0.072(3) Uani 0.3839 1 d D U P A 2
H32C H 0.0586 0.7689 0.7751 0.087 Uiso 0.3839 1 calc R . P A 2
H32D H 0.0432 0.8260 0.8561 0.087 Uiso 0.3839 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 P1 3.221(2) . ?
K1 O1 2.696(7) . ?
K1 O2 2.698(7) . ?
K1 C29 3.505(13) . ?
K1 O3 2.706(5) . ?
K1 O4 2.817(6) . ?
P1 C1 1.844(3) . ?
P1 C13 1.841(3) . ?
P1 K1A 3.211(3) . ?
O1 C28 1.432(9) . ?
O1 C25 1.460(9) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C27 1.534(10) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C26 1.502(12) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C25 1.520(10) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
O2 C29 1.447(9) . ?
O2 C32 1.387(9) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.494(9) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.343(9) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.486(9) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
O3 C33 1.418(9) . ?
O3 C36 1.436(9) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.498(10) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.491(11) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.372(13) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
O4 C40 1.488(9) . ?
O4 C37 1.444(9) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C39 1.459(12) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C38 1.444(11) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C37 1.475(11) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C1 C2 1.414(4) . ?
C1 C6 1.429(5) . ?
C2 C3 1.400(5) . ?
C2 C7 1.524(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.369(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.377(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.394(5) . ?
C6 C10 1.513(5) . ?
C7 H7 1.0000 . ?
C7 C8 1.515(6) . ?
C7 C9 1.534(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 1.0000 . ?
C10 C11 1.536(5) . ?
C10 C12 1.525(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.419(5) . ?
C13 C18 1.419(4) . ?
C14 C15 1.393(5) . ?
C14 C19 1.518(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.384(6) . ?
C16 H16 0.9500 . ?
C16 C17 1.381(6) . ?
C17 H17 0.9500 . ?
C17 C18 1.394(5) . ?
C18 C22 1.518(5) . ?
C19 H19 1.0000 . ?
C19 C20 1.523(6) . ?
C19 C21 1.528(6) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C20 K1A 3.414(7) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22 1.0000 . ?
C22 C23 1.519(6) . ?
C22 C24 1.532(6) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
K1A O1A 2.700(11) . ?
K1A O3A 2.736(9) . ?
K1A O4A 2.829(10) . ?
K1A O2A 2.720(13) . ?
O1A C28A 1.433(13) . ?
O1A C25A 1.446(13) . ?
C28A H28C 0.9900 . ?
C28A H28D 0.9900 . ?
C28A C27A 1.528(13) . ?
C27A H27C 0.9900 . ?
C27A H27D 0.9900 . ?
C27A C26A 1.496(14) . ?
C26A H26C 0.9900 . ?
C26A H26D 0.9900 . ?
C26A C25A 1.523(14) . ?
C25A H25C 0.9900 . ?
C25A H25D 0.9900 . ?
O3A C33A 1.428(13) . ?
O3A C36A 1.442(12) . ?
C33A H33C 0.9900 . ?
C33A H33D 0.9900 . ?
C33A C34A 1.501(14) . ?
C34A H34C 0.9900 . ?
C34A H34D 0.9900 . ?
C34A C35A 1.479(15) . ?
C35A H35C 0.9900 . ?
C35A H35D 0.9900 . ?
C35A C36A 1.36(2) . ?
C36A H36C 0.9900 . ?
C36A H36D 0.9900 . ?
O4A C40A 1.557(13) . ?
O4A C37A 1.443(13) . ?
C40A H40C 0.9900 . ?
C40A H40D 0.9900 . ?
C40A C39A 1.453(15) . ?
C39A H39C 0.9900 . ?
C39A H39D 0.9900 . ?
C39A C38A 1.487(15) . ?
C38A H38C 0.9900 . ?
C38A H38D 0.9900 . ?
C38A C37A 1.500(15) . ?
C37A H37C 0.9900 . ?
C37A H37D 0.9900 . ?
O2A C29A 1.453(12) . ?
O2A C32A 1.408(13) . ?
C29A H29C 0.9900 . ?
C29A H29D 0.9900 . ?
C29A C30A 1.483(13) . ?
C30A H30C 0.9900 . ?
C30A H30D 0.9900 . ?
C30A C31A 1.320(13) . ?
C31A H31C 0.9900 . ?
C31A H31D 0.9900 . ?
C31A C32A 1.482(13) . ?
C32A H32C 0.9900 . ?
C32A H32D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 K1 C29 73.12(19) . . ?
O1 K1 P1 87.4(3) . . ?
O1 K1 O2 171.2(4) . . ?
O1 K1 C29 158.7(3) . . ?
O1 K1 O3 77.3(3) . . ?
O1 K1 O4 106.1(3) . . ?
O2 K1 P1 88.6(3) . . ?
O2 K1 C29 22.5(2) . . ?
O2 K1 O3 99.5(3) . . ?
O2 K1 O4 82.2(4) . . ?
O3 K1 P1 130.67(17) . . ?
O3 K1 C29 122.0(2) . . ?
O3 K1 O4 93.7(2) . . ?
O4 K1 P1 135.61(15) . . ?
O4 K1 C29 83.1(2) . . ?
C1 P1 K1 126.47(10) . . ?
C1 P1 K1A 136.99(11) . . ?
C13 P1 K1 130.00(10) . . ?
C13 P1 C1 103.50(14) . . ?
C13 P1 K1A 119.35(11) . . ?
C28 O1 K1 116.9(7) . . ?
C28 O1 C25 109.2(5) . . ?
C25 O1 K1 115.8(7) . . ?
O1 C28 H28A 110.6 . . ?
O1 C28 H28B 110.6 . . ?
O1 C28 C27 105.9(6) . . ?
H28A C28 H28B 108.7 . . ?
C27 C28 H28A 110.6 . . ?
C27 C28 H28B 110.6 . . ?
C28 C27 H27A 111.2 . . ?
C28 C27 H27B 111.2 . . ?
H27A C27 H27B 109.1 . . ?
C26 C27 C28 102.7(8) . . ?
C26 C27 H27A 111.2 . . ?
C26 C27 H27B 111.2 . . ?
C27 C26 H26A 111.5 . . ?
C27 C26 H26B 111.5 . . ?
C27 C26 C25 101.4(8) . . ?
H26A C26 H26B 109.3 . . ?
C25 C26 H26A 111.5 . . ?
C25 C26 H26B 111.5 . . ?
O1 C25 C26 105.0(7) . . ?
O1 C25 H25A 110.7 . . ?
O1 C25 H25B 110.7 . . ?
C26 C25 H25A 110.7 . . ?
C26 C25 H25B 110.7 . . ?
H25A C25 H25B 108.8 . . ?
C29 O2 K1 111.9(7) . . ?
C32 O2 K1 138.9(7) . . ?
C32 O2 C29 108.1(6) . . ?
K1 C29 H29A 102.3 . . ?
K1 C29 H29B 72.5 . . ?
O2 C29 K1 45.5(5) . . ?
O2 C29 H29A 110.9 . . ?
O2 C29 H29B 110.9 . . ?
O2 C29 C30 104.2(5) . . ?
H29A C29 H29B 108.9 . . ?
C30 C29 K1 142.4(7) . . ?
C30 C29 H29A 110.9 . . ?
C30 C29 H29B 110.9 . . ?
C29 C30 H30A 109.8 . . ?
C29 C30 H30B 109.8 . . ?
H30A C30 H30B 108.2 . . ?
C31 C30 C29 109.5(6) . . ?
C31 C30 H30A 109.8 . . ?
C31 C30 H30B 109.8 . . ?
C30 C31 H31A 110.2 . . ?
C30 C31 H31B 110.2 . . ?
C30 C31 C32 107.6(6) . . ?
H31A C31 H31B 108.5 . . ?
C32 C31 H31A 110.2 . . ?
C32 C31 H31B 110.2 . . ?
O2 C32 C31 107.9(6) . . ?
O2 C32 H32A 110.1 . . ?
O2 C32 H32B 110.1 . . ?
C31 C32 H32A 110.1 . . ?
C31 C32 H32B 110.1 . . ?
H32A C32 H32B 108.4 . . ?
C33 O3 K1 128.3(5) . . ?
C33 O3 C36 105.9(6) . . ?
C36 O3 K1 125.7(6) . . ?
O3 C33 H33A 110.7 . . ?
O3 C33 H33B 110.7 . . ?
O3 C33 C34 105.3(6) . . ?
H33A C33 H33B 108.8 . . ?
C34 C33 H33A 110.7 . . ?
C34 C33 H33B 110.7 . . ?
C33 C34 H34A 111.1 . . ?
C33 C34 H34B 111.1 . . ?
H34A C34 H34B 109.1 . . ?
C35 C34 C33 103.2(6) . . ?
C35 C34 H34A 111.1 . . ?
C35 C34 H34B 111.1 . . ?
C34 C35 H35A 110.0 . . ?
C34 C35 H35B 110.0 . . ?
H35A C35 H35B 108.4 . . ?
C36 C35 C34 108.4(8) . . ?
C36 C35 H35A 110.0 . . ?
C36 C35 H35B 110.0 . . ?
O3 C36 H36A 109.9 . . ?
O3 C36 H36B 109.9 . . ?
C35 C36 O3 108.7(7) . . ?
C35 C36 H36A 109.9 . . ?
C35 C36 H36B 109.9 . . ?
H36A C36 H36B 108.3 . . ?
C40 O4 K1 113.5(7) . . ?
C37 O4 K1 107.8(7) . . ?
C37 O4 C40 103.1(6) . . ?
O4 C40 H40A 110.7 . . ?
O4 C40 H40B 110.7 . . ?
H40A C40 H40B 108.8 . . ?
C39 C40 O4 105.1(6) . . ?
C39 C40 H40A 110.7 . . ?
C39 C40 H40B 110.7 . . ?
C40 C39 H39A 111.2 . . ?
C40 C39 H39B 111.2 . . ?
H39A C39 H39B 109.2 . . ?
C38 C39 C40 102.6(8) . . ?
C38 C39 H39A 111.2 . . ?
C38 C39 H39B 111.2 . . ?
C39 C38 H38A 110.3 . . ?
C39 C38 H38B 110.3 . . ?
C39 C38 C37 106.9(7) . . ?
H38A C38 H38B 108.6 . . ?
C37 C38 H38A 110.3 . . ?
C37 C38 H38B 110.3 . . ?
K1 C37 H37A 62.7 . . ?
K1 C37 H37B 137.2 . . ?
O4 C37 K1 49.3(5) . . ?
O4 C37 C38 107.7(6) . . ?
O4 C37 H37A 110.2 . . ?
O4 C37 H37B 110.2 . . ?
C38 C37 K1 112.0(8) . . ?
C38 C37 H37A 110.2 . . ?
C38 C37 H37B 110.2 . . ?
H37A C37 H37B 108.5 . . ?
C2 C1 P1 123.1(2) . . ?
C2 C1 C6 117.5(3) . . ?
C6 C1 P1 119.3(2) . . ?
C1 C2 C7 123.1(3) . . ?
C3 C2 C1 120.0(3) . . ?
C3 C2 C7 116.9(3) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 C2 121.6(3) . . ?
C4 C3 H3 119.2 . . ?
C3 C4 H4 120.4 . . ?
C3 C4 C5 119.2(3) . . ?
C5 C4 H4 120.4 . . ?
C4 C5 H5 119.2 . . ?
C4 C5 C6 121.6(3) . . ?
C6 C5 H5 119.2 . . ?
C1 C6 C10 120.6(3) . . ?
C5 C6 C1 119.7(3) . . ?
C5 C6 C10 119.7(3) . . ?
C2 C7 H7 107.4 . . ?
C2 C7 C9 110.5(3) . . ?
C8 C7 C2 113.7(3) . . ?
C8 C7 H7 107.4 . . ?
C8 C7 C9 110.3(3) . . ?
C9 C7 H7 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 H10 107.2 . . ?
C6 C10 C11 109.9(3) . . ?
C6 C10 C12 114.7(3) . . ?
C11 C10 H10 107.2 . . ?
C12 C10 H10 107.2 . . ?
C12 C10 C11 110.1(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 P1 120.1(2) . . ?
C18 C13 P1 122.1(3) . . ?
C18 C13 C14 117.8(3) . . ?
C13 C14 C19 121.1(3) . . ?
C15 C14 C13 120.4(3) . . ?
C15 C14 C19 118.5(3) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 C14 121.3(4) . . ?
C16 C15 H15 119.3 . . ?
C15 C16 H16 120.7 . . ?
C17 C16 C15 118.6(4) . . ?
C17 C16 H16 120.7 . . ?
C16 C17 H17 118.9 . . ?
C16 C17 C18 122.1(4) . . ?
C18 C17 H17 118.9 . . ?
C13 C18 C22 123.3(3) . . ?
C17 C18 C13 119.6(3) . . ?
C17 C18 C22 117.0(3) . . ?
C14 C19 H19 107.3 . . ?
C14 C19 C20 110.0(3) . . ?
C14 C19 C21 113.9(3) . . ?
C20 C19 H19 107.3 . . ?
C20 C19 C21 110.6(4) . . ?
C21 C19 H19 107.3 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
C19 C20 K1A 98.8(3) . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
K1A C20 H20A 46.6 . . ?
K1A C20 H20B 71.2 . . ?
K1A C20 H20C 148.9 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22 H22 107.4 . . ?
C18 C22 C23 113.5(4) . . ?
C18 C22 C24 110.7(3) . . ?
C23 C22 H22 107.4 . . ?
C23 C22 C24 110.2(3) . . ?
C24 C22 H22 107.4 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
P1 K1A C20 68.82(10) . . ?
O1A K1A P1 87.2(5) . . ?
O1A K1A C20 95.5(4) . . ?
O1A K1A O3A 80.0(5) . . ?
O1A K1A O4A 96.8(5) . . ?
O1A K1A O2A 167.4(6) . . ?
O3A K1A P1 140.4(3) . . ?
O3A K1A C20 75.3(3) . . ?
O3A K1A O4A 96.3(4) . . ?
O4A K1A P1 122.5(3) . . ?
O4A K1A C20 163.7(3) . . ?
O2A K1A P1 82.9(5) . . ?
O2A K1A C20 88.1(5) . . ?
O2A K1A O3A 112.5(5) . . ?
O2A K1A O4A 82.2(6) . . ?
C28A O1A K1A 110.2(11) . . ?
C28A O1A C25A 109.4(8) . . ?
C25A O1A K1A 118.9(13) . . ?
K1A C28A H28C 64.4 . . ?
K1A C28A H28D 116.7 . . ?
O1A C28A K1A 47.0(8) . . ?
O1A C28A H28C 110.4 . . ?
O1A C28A H28D 110.4 . . ?
O1A C28A C27A 106.4(9) . . ?
H28C C28A H28D 108.6 . . ?
C27A C28A K1A 132(2) . . ?
C27A C28A H28C 110.4 . . ?
C27A C28A H28D 110.4 . . ?
C28A C27A H27C 111.0 . . ?
C28A C27A H27D 111.0 . . ?
H27C C27A H27D 109.0 . . ?
C26A C27A C28A 103.8(10) . . ?
C26A C27A H27C 111.0 . . ?
C26A C27A H27D 111.0 . . ?
C27A C26A H26C 111.4 . . ?
C27A C26A H26D 111.4 . . ?
C27A C26A C25A 102.1(11) . . ?
H26C C26A H26D 109.2 . . ?
C25A C26A H26C 111.4 . . ?
C25A C26A H26D 111.4 . . ?
O1A C25A C26A 105.0(10) . . ?
O1A C25A H25C 110.7 . . ?
O1A C25A H25D 110.7 . . ?
C26A C25A H25C 110.7 . . ?
C26A C25A H25D 110.7 . . ?
H25C C25A H25D 108.8 . . ?
C33A O3A K1A 126.0(11) . . ?
C33A O3A C36A 104.1(8) . . ?
C36A O3A K1A 119.8(11) . . ?
O3A C33A H33C 110.4 . . ?
O3A C33A H33D 110.4 . . ?
O3A C33A C34A 106.7(8) . . ?
H33C C33A H33D 108.6 . . ?
C34A C33A H33C 110.4 . . ?
C34A C33A H33D 110.4 . . ?
C33A C34A H34C 110.9 . . ?
C33A C34A H34D 110.9 . . ?
H34C C34A H34D 108.9 . . ?
C35A C34A C33A 104.2(8) . . ?
C35A C34A H34C 110.9 . . ?
C35A C34A H34D 110.9 . . ?
C34A C35A H35C 110.6 . . ?
C34A C35A H35D 110.6 . . ?
H35C C35A H35D 108.7 . . ?
C36A C35A C34A 105.6(12) . . ?
C36A C35A H35C 110.6 . . ?
C36A C35A H35D 110.6 . . ?
O3A C36A H36C 110.0 . . ?
O3A C36A H36D 110.0 . . ?
C35A C36A O3A 108.4(13) . . ?
C35A C36A H36C 110.0 . . ?
C35A C36A H36D 110.0 . . ?
H36C C36A H36D 108.4 . . ?
C40A O4A K1A 115.0(10) . . ?
C37A O4A K1A 120.0(12) . . ?
C37A O4A C40A 100.3(8) . . ?
O4A C40A H40C 112.2 . . ?
O4A C40A H40D 112.2 . . ?
H40C C40A H40D 109.8 . . ?
C39A C40A O4A 97.8(10) . . ?
C39A C40A H40C 112.2 . . ?
C39A C40A H40D 112.2 . . ?
C40A C39A H39C 112.3 . . ?
C40A C39A H39D 112.3 . . ?
C40A C39A C38A 97.1(11) . . ?
H39C C39A H39D 109.9 . . ?
C38A C39A H39C 112.3 . . ?
C38A C39A H39D 112.3 . . ?
C39A C38A H38C 111.1 . . ?
C39A C38A H38D 111.1 . . ?
C39A C38A C37A 103.2(10) . . ?
H38C C38A H38D 109.1 . . ?
C37A C38A H38C 111.1 . . ?
C37A C38A H38D 111.1 . . ?
O4A C37A C38A 106.2(8) . . ?
O4A C37A H37C 110.5 . . ?
O4A C37A H37D 110.5 . . ?
C38A C37A H37C 110.5 . . ?
C38A C37A H37D 110.5 . . ?
H37C C37A H37D 108.7 . . ?
C29A O2A K1A 124.5(15) . . ?
C32A O2A K1A 110.5(11) . . ?
C32A O2A C29A 108.5(8) . . ?
O2A C29A H29C 110.7 . . ?
O2A C29A H29D 110.7 . . ?
O2A C29A C30A 105.1(8) . . ?
H29C C29A H29D 108.8 . . ?
C30A C29A H29C 110.7 . . ?
C30A C29A H29D 110.7 . . ?
C29A C30A H30C 109.7 . . ?
C29A C30A H30D 109.7 . . ?
H30C C30A H30D 108.2 . . ?
C31A C30A C29A 109.9(9) . . ?
C31A C30A H30C 109.7 . . ?
C31A C30A H30D 109.7 . . ?
C30A C31A H31C 109.8 . . ?
C30A C31A H31D 109.8 . . ?
C30A C31A C32A 109.4(9) . . ?
H31C C31A H31D 108.2 . . ?
C32A C31A H31C 109.8 . . ?
C32A C31A H31D 109.8 . . ?
K1A C32A H32C 64.5 . . ?
K1A C32A H32D 115.3 . . ?
O2A C32A K1A 47.2(8) . . ?
O2A C32A C31A 106.6(8) . . ?
O2A C32A H32C 110.4 . . ?
O2A C32A H32D 110.4 . . ?
C31A C32A K1A 133.0(9) . . ?
C31A C32A H32C 110.4 . . ?
C31A C32A H32D 110.4 . . ?
H32C C32A H32D 108.6 . . ?

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 P1 C1 C2 129.8(2) . . . . ?
K1 P1 C1 C6 -47.9(3) . . . . ?
K1 P1 C13 C14 -45.8(3) . . . . ?
K1 P1 C13 C18 130.6(2) . . . . ?
K1 O1 C28 C27 127.7(15) . . . . ?
K1 O1 C25 C26 -153.0(13) . . . . ?
K1 O2 C29 C30 -153.7(8) . . . . ?
K1 O2 C32 C31 152.4(11) . . . . ?
K1 C29 C30 C31 -44.9(15) . . . . ?
K1 O3 C33 C34 153.2(7) . . . . ?
K1 O3 C36 C35 -156.9(12) . . . . ?
K1 O4 C40 C39 -82.3(9) . . . . ?
K1 O4 C37 C38 104.2(11) . . . . ?
P1 C1 C2 C3 176.3(2) . . . . ?
P1 C1 C2 C7 -7.2(4) . . . . ?
P1 C1 C6 C5 -177.8(2) . . . . ?
P1 C1 C6 C10 3.7(4) . . . . ?
P1 C13 C14 C15 179.1(3) . . . . ?
P1 C13 C14 C19 0.2(4) . . . . ?
P1 C13 C18 C17 179.3(3) . . . . ?
P1 C13 C18 C22 -3.8(5) . . . . ?
O1 C28 C27 C26 28.6(19) . . . . ?
C28 O1 C25 C26 -18.5(17) . . . . ?
C28 C27 C26 C25 -38.6(18) . . . . ?
C27 C26 C25 O1 35.7(17) . . . . ?
C25 O1 C28 C27 -6.2(18) . . . . ?
O2 C29 C30 C31 -13.7(13) . . . . ?
C29 O2 C32 C31 -14.1(14) . . . . ?
C29 C30 C31 C32 5.4(12) . . . . ?
C30 C31 C32 O2 5.4(13) . . . . ?
C32 O2 C29 K1 170.5(16) . . . . ?
C32 O2 C29 C30 16.8(14) . . . . ?
O3 C33 C34 C35 22.6(15) . . . . ?
C33 O3 C36 C35 25.7(17) . . . . ?
C33 C34 C35 C36 -7.3(19) . . . . ?
C34 C35 C36 O3 -11(2) . . . . ?
C36 O3 C33 C34 -29.5(13) . . . . ?
O4 C40 C39 C38 -38.5(12) . . . . ?
C40 O4 C37 K1 -120.3(8) . . . . ?
C40 O4 C37 C38 -16.1(13) . . . . ?
C40 C39 C38 C37 28.2(15) . . . . ?
C39 C38 C37 K1 45.1(14) . . . . ?
C39 C38 C37 O4 -7.4(16) . . . . ?
C37 O4 C40 C39 34.0(11) . . . . ?
C1 P1 C13 C14 132.2(3) . . . . ?
C1 P1 C13 C18 -51.4(3) . . . . ?
C1 C2 C3 C4 2.8(5) . . . . ?
C1 C2 C7 C8 121.8(4) . . . . ?
C1 C2 C7 C9 -113.6(4) . . . . ?
C1 C6 C10 C11 86.6(4) . . . . ?
C1 C6 C10 C12 -148.7(3) . . . . ?
C2 C1 C6 C5 4.3(4) . . . . ?
C2 C1 C6 C10 -174.2(3) . . . . ?
C2 C3 C4 C5 2.2(6) . . . . ?
C3 C2 C7 C8 -61.6(4) . . . . ?
C3 C2 C7 C9 63.0(4) . . . . ?
C3 C4 C5 C6 -3.9(6) . . . . ?
C4 C5 C6 C1 0.6(5) . . . . ?
C4 C5 C6 C10 179.1(3) . . . . ?
C5 C6 C10 C11 -91.9(4) . . . . ?
C5 C6 C10 C12 32.8(5) . . . . ?
C6 C1 C2 C3 -5.9(4) . . . . ?
C6 C1 C2 C7 170.5(3) . . . . ?
C7 C2 C3 C4 -173.9(3) . . . . ?
C13 P1 C1 C2 -48.3(3) . . . . ?
C13 P1 C1 C6 134.0(2) . . . . ?
C13 C14 C15 C16 1.1(6) . . . . ?
C13 C14 C19 C20 93.1(4) . . . . ?
C13 C14 C19 C21 -142.1(4) . . . . ?
C13 C18 C22 C23 125.8(4) . . . . ?
C13 C18 C22 C24 -109.7(4) . . . . ?
C14 C13 C18 C17 -4.2(5) . . . . ?
C14 C13 C18 C22 172.7(3) . . . . ?
C14 C15 C16 C17 -2.8(6) . . . . ?
C14 C19 C20 K1A -98.5(3) . . . . ?
C15 C14 C19 C20 -85.8(5) . . . . ?
C15 C14 C19 C21 39.1(5) . . . . ?
C15 C16 C17 C18 1.0(6) . . . . ?
C16 C17 C18 C13 2.5(6) . . . . ?
C16 C17 C18 C22 -174.6(4) . . . . ?
C17 C18 C22 C23 -57.2(5) . . . . ?
C17 C18 C22 C24 67.3(5) . . . . ?
C18 C13 C14 C15 2.5(5) . . . . ?
C18 C13 C14 C19 -176.4(3) . . . . ?
C19 C14 C15 C16 179.9(4) . . . . ?
C21 C19 C20 K1A 134.7(3) . . . . ?
K1A P1 C1 C2 126.8(2) . . . . ?
K1A P1 C1 C6 -51.0(3) . . . . ?
K1A P1 C13 C14 -43.9(3) . . . . ?
K1A P1 C13 C18 132.5(3) . . . . ?
K1A O1A C28A C27A 132(2) . . . . ?
K1A O1A C25A C26A -149(2) . . . . ?
K1A C28A C27A C26A 69(3) . . . . ?
K1A O3A C33A C34A 124.4(14) . . . . ?
K1A O3A C36A C35A -114(2) . . . . ?
K1A O4A C40A C39A -80.8(13) . . . . ?
K1A O4A C37A C38A 106.5(18) . . . . ?
K1A O2A C29A C30A -129.9(16) . . . . ?
K1A O2A C32A C31A 134.0(11) . . . . ?
O1A C28A C27A C26A 22(3) . . . . ?
C28A O1A C25A C26A -22(3) . . . . ?
C28A C27A C26A C25A -34(3) . . . . ?
C27A C26A C25A O1A 35(3) . . . . ?
C25A O1A C28A K1A -132(2) . . . . ?
C25A O1A C28A C27A 0(3) . . . . ?
O3A C33A C34A C35A 2(3) . . . . ?
C33A O3A C36A C35A 34(3) . . . . ?
C33A C34A C35A C36A 18(3) . . . . ?
C34A C35A C36A O3A -32(3) . . . . ?
C36A O3A C33A C34A -20(2) . . . . ?
O4A C40A C39A C38A -57.6(15) . . . . ?
C40A O4A C37A C38A -20(2) . . . . ?
C40A C39A C38A C37A 46(2) . . . . ?
C39A C38A C37A O4A -14(2) . . . . ?
C37A O4A C40A C39A 49.4(16) . . . . ?
O2A C29A C30A C31A 2(3) . . . . ?
C29A O2A C32A K1A -140(3) . . . . ?
C29A O2A C32A C31A -6(2) . . . . ?
C29A C30A C31A C32A -5(2) . . . . ?
C30A C31A C32A K1A 53(2) . . . . ?
C30A C31A C32A O2A 7(2) . . . . ?
C32A O2A C29A C30A 3(3) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1 0 -2 0.1127 1.0020 0.0007 -2.0000 0.1391 -0.0834 0.1248
0 -1 1 0.0899 0.0008 -0.9999 1.0000 -0.1398 -0.0172 0.0090
-1 0 2 0.1317 -1.0020 -0.0007 2.0000 -0.1391 0.0834 -0.1248
1 3 -1 0.1216 0.9964 3.0015 -0.9975 0.2812 0.1995 0.0200
3 -2 1 0.1257 3.0034 -1.9961 1.0034 -0.2089 0.0046 0.2951
-3 2 -1 0.1257 -3.0034 1.9961 -1.0034 0.2089 -0.0046 -0.2951
2 1 2 0.1093 1.9974 1.0035 2.0045 -0.0673 0.2552 0.1044
-2 -1 -2 0.1253 -1.9974 -1.0035 -2.0045 0.0673 -0.2552 -0.1044
0 0 -1 0.1380 0.0008 -0.0003 -1.0007 0.0693 -0.0578 0.0194
0 0 1 0.0990 -0.0008 0.0003 1.0007 -0.0693 0.0578 -0.0194
0 -1 -1 0.0979 0.0024 -1.0005 -1.0013 -0.0011 -0.1329 0.0479
0 1 -1 0.1139 -0.0008 0.9999 -1.0000 0.1398 0.0172 -0.0090
1 0 0 0.1290 1.0003 0.0013 0.0013 0.0005 0.0323 0.0859
-1 0 0 0.1120 -1.0003 -0.0013 -0.0013 -0.0005 -0.0323 -0.0859
1 0 2 0.0848 0.9987 0.0020 2.0026 -0.1382 0.1479 0.0470
-2 -1 -1 0.1132 -1.9982 -1.0031 -1.0039 -0.0021 -0.1974 -0.1239
2 1 1 0.1232 1.9982 1.0031 1.0039 0.0021 0.1974 0.1239
1 2 2 0.1235 0.9954 2.0023 2.0038 0.0027 0.2980 -0.0099

_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_8b
_database_code_depnum_ccdc_archive 'CCDC 1557236'
_audit_update_record             
;
2017-06-20 deposited with the CCDC.
2017-07-20 downloaded from the CCDC.
;
_audit_creation_date             2017-03-28
_audit_creation_method           
;
Olex2 1.2
(compiled Mar  2 2017 14:00:58 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H46 Li O3 P'
_chemical_formula_sum            'C30 H46 Li O3 P'
_chemical_formula_weight         492.58
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H46 Li1 O3 P1'
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'
Li Li -0.0003 0.0001 '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'
P P 0.1023 0.0942 '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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.0626(3)
_cell_length_b                   17.2694(7)
_cell_length_c                   19.2321(6)
_cell_angle_alpha                90
_cell_angle_beta                 102.935(4)
_cell_angle_gamma                90
_cell_volume                     2933.56(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6490
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      26.5410
_cell_measurement_theta_min      3.7060
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.120
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 2 0.1088
0 -1 0 0.1347
-1 2 -1 0.1237
0 0 1 0.1006
-1 -1 1 0.1636
1 1 -1 0.1396
0 1 0 0.0813
0 -1 1 0.0846
0 1 -1 0.0936
1 0 0 0.1647
-1 0 0 0.1597
0 -1 -2 0.1148

_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0004 0.9989 2.0001 -0.0029 -0.0667 0.0543
0.0002 -0.9998 -0.0001 -0.0345 0.0109 -0.0195
-0.9998 1.9996 -1.0002 0.0786 0.0680 0.0719
-0.0001 -0.0005 1.0000 -0.0187 -0.0279 0.0174
-0.9996 -1.0008 0.9995 -0.0621 0.0448 0.0484
0.9996 1.0008 -0.9995 0.0621 -0.0448 -0.0484
-0.0002 0.9998 0.0001 0.0345 -0.0109 0.0195
0.0000 -1.0003 0.9999 -0.0532 -0.0170 -0.0020
-0.0000 1.0003 -0.9999 0.0532 0.0170 0.0020
0.9996 0.0006 0.0004 0.0090 -0.0618 -0.0504
-0.9996 -0.0006 -0.0004 -0.0090 0.0618 0.0504
0.0004 -0.9989 -2.0001 0.0029 0.0667 -0.0543

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.856
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23834
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.856
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.835
_diffrn_reflns_theta_min         3.308
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3968
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -71.00  56.00   1.00   12.50    --   10.16 -19.00-150.00  127
  2  ω    -66.00  37.00   1.00   12.50    --   10.16 -38.00 150.00  103
  3  ω    -23.00  26.00   1.00   12.50    --   -9.14 -84.00 102.00   49
  4  ω    -16.00  25.00   1.00   12.50    --   10.16  38.00 -60.00   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0089832000
_diffrn_orient_matrix_UB_12      0.0344926000
_diffrn_orient_matrix_UB_13      -0.0186558000
_diffrn_orient_matrix_UB_21      -0.0618333000
_diffrn_orient_matrix_UB_22      -0.0108821000
_diffrn_orient_matrix_UB_23      -0.0279278000
_diffrn_orient_matrix_UB_31      -0.0504356000
_diffrn_orient_matrix_UB_32      0.0194692000
_diffrn_orient_matrix_UB_33      0.0174338000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4288
_reflns_number_total             6573
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         6573
_refine_ls_number_restraints     160
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0533
_refine_ls_restrained_S_all      1.027
_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)+(0.0652P)²+0.7813P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1489
_refine_special_details          
;
One tetrahydrofuran molecule coordinated to 
lithium has been modelled as disordered over 
two positions. The occupancies of the two 
sites were allowed to refine with isotropic 
atom treatment. Upon convergence of the 
refinement, the occupancies were fixed 
before anisotropy was introduced into the 
model. The displacement parameters of allo 
disordered atoms were restrained using the 
SIMU card and the geometry of the 
tetrahydrofuran moieties was restrained using 
the SAME card.
;
_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. Uiso/Uaniso restraints and constraints
C30A \\sim O3A \\sim O3B \\sim C27B \\sim C29A \\sim C28B \\sim C28A \\sim C29B
\\sim C27A \\sim C30B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
3. Same fragment restrains
{O3A, C27A, C28A, C29A, C30A} sigma for 1-2: 0.02, 1-3: 0.02
as
{O3B, C30B, C29B, C28B, C27B}
4. Others
 Fixed Sof: O3A(0.47312) C27A(0.47312) H27A(0.47312) H27B(0.47312)
 C28A(0.47312) H28A(0.47312) H28B(0.47312) C29A(0.47312) H29A(0.47312)
 H29B(0.47312) C30A(0.47312) H30A(0.47312) H30B(0.47312) O3B(0.52688)
 C30B(0.52688) H30C(0.52688) H30D(0.52688) C29B(0.52688) H29C(0.52688)
 H29D(0.52688) C28B(0.52688) H28C(0.52688) H28D(0.52688) C27B(0.52688)
 H27C(0.52688) H27D(0.52688)
5.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,
 H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27A(H27A,H27B),
 C28A(H28A,H28B), C29A(H29A,H29B), C30A(H30A,H30B), C30B(H30C,H30D), C29B(H29C,
 H29D), C28B(H28C,H28D), C27B(H27C,H27D)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C14(H14)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
P1 P 0.56667(6) 0.28352(3) 0.32368(3) 0.03994(16) Uani 1 1 d . . . . .
O1 O 0.39652(16) 0.41386(8) 0.18239(7) 0.0476(4) Uani 1 1 d . . . . .
O2 O 0.15976(16) 0.34106(10) 0.24953(7) 0.0560(4) Uani 1 1 d . . . . .
C1 C 0.7300(2) 0.30461(11) 0.39510(9) 0.0365(4) Uani 1 1 d . . . . .
C2 C 0.8106(2) 0.24927(12) 0.44371(10) 0.0400(4) Uani 1 1 d . . . . .
C3 C 0.9408(2) 0.27095(12) 0.49296(10) 0.0438(5) Uani 1 1 d . . . . .
H3 H 0.9903 0.2340 0.5250 0.053 Uiso 1 1 calc R . . . .
C4 C 1.0000(2) 0.34474(13) 0.49639(10) 0.0448(5) Uani 1 1 d . . . . .
C5 C 0.9268(2) 0.39738(12) 0.44611(10) 0.0446(5) Uani 1 1 d . . . . .
H5 H 0.9664 0.4471 0.4461 0.053 Uiso 1 1 calc R . . . .
C6 C 0.7967(2) 0.37876(12) 0.39577(10) 0.0400(4) Uani 1 1 d . . . . .
C7 C 0.7644(2) 0.16551(12) 0.43995(12) 0.0517(5) Uani 1 1 d . . . . .
H7A H 0.6718 0.1600 0.4559 0.077 Uiso 1 1 calc GR . . . .
H7B H 0.8424 0.1354 0.4699 0.077 Uiso 1 1 calc GR . . . .
H7C H 0.7493 0.1477 0.3916 0.077 Uiso 1 1 calc GR . . . .
C8 C 1.1396(3) 0.36680(15) 0.55189(12) 0.0604(6) Uani 1 1 d . . . . .
H8A H 1.1104 0.3853 0.5939 0.091 Uiso 1 1 calc GR . . . .
H8B H 1.1935 0.4068 0.5333 0.091 Uiso 1 1 calc GR . . . .
H8C H 1.2038 0.3223 0.5638 0.091 Uiso 1 1 calc GR . . . .
C9 C 0.7332(3) 0.43785(13) 0.33945(12) 0.0536(6) Uani 1 1 d . . . . .
H9A H 0.7298 0.4163 0.2931 0.080 Uiso 1 1 calc GR . . . .
H9B H 0.7965 0.4830 0.3462 0.080 Uiso 1 1 calc GR . . . .
H9C H 0.6327 0.4519 0.3432 0.080 Uiso 1 1 calc GR . . . .
C10 C 0.4446(2) 0.21230(11) 0.35328(10) 0.0391(4) Uani 1 1 d . . . . .
C11 C 0.3721(2) 0.15781(12) 0.30192(11) 0.0436(5) Uani 1 1 d . . . . .
C12 C 0.2639(2) 0.10770(13) 0.31738(13) 0.0539(6) Uani 1 1 d . . . . .
H12 H 0.2182 0.0723 0.2828 0.065 Uiso 1 1 calc R . . . .
C13 C 0.2214(2) 0.10832(15) 0.38189(14) 0.0595(6) Uani 1 1 d . . . . .
C14 C 0.2909(2) 0.16201(14) 0.43190(13) 0.0553(6) Uani 1 1 d . . . . .
H14 H 0.2633 0.1638 0.4756 0.066 Uiso 1 1 calc R . . . .
C15 C 0.4004(2) 0.21347(12) 0.41961(11) 0.0458(5) Uani 1 1 d . . . . .
C16 C 0.4090(3) 0.15362(14) 0.22948(11) 0.0565(6) Uani 1 1 d . . . . .
H16A H 0.3705 0.1989 0.2024 0.085 Uiso 1 1 calc GR . . . .
H16B H 0.3633 0.1082 0.2049 0.085 Uiso 1 1 calc GR . . . .
H16C H 0.5168 0.1511 0.2349 0.085 Uiso 1 1 calc GR . . . .
C17 C 0.1018(3) 0.05288(19) 0.39687(18) 0.0879(9) Uani 1 1 d . . . . .
H17A H 0.0042 0.0677 0.3690 0.132 Uiso 1 1 calc GR . . . .
H17B H 0.1008 0.0548 0.4466 0.132 Uiso 1 1 calc GR . . . .
H17C H 0.1249 0.0012 0.3844 0.132 Uiso 1 1 calc GR . . . .
C18 C 0.4630(3) 0.27267(13) 0.47572(12) 0.0571(6) Uani 1 1 d . . . . .
H18A H 0.5674 0.2612 0.4961 0.086 Uiso 1 1 calc GR . . . .
H18B H 0.4065 0.2713 0.5124 0.086 Uiso 1 1 calc GR . . . .
H18C H 0.4552 0.3232 0.4545 0.086 Uiso 1 1 calc GR . . . .
C19 C 0.4692(3) 0.36426(13) 0.14060(11) 0.0534(6) Uani 1 1 d . . . . .
H19A H 0.3954 0.3327 0.1085 0.064 Uiso 1 1 calc R . . . .
H19B H 0.5416 0.3305 0.1710 0.064 Uiso 1 1 calc R . . . .
C20 C 0.5473(3) 0.41838(14) 0.09975(12) 0.0582(6) Uani 1 1 d . . . . .
H20A H 0.5627 0.3944 0.0563 0.070 Uiso 1 1 calc R . . . .
H20B H 0.6443 0.4350 0.1284 0.070 Uiso 1 1 calc R . . . .
C21 C 0.4377(3) 0.48535(13) 0.08339(11) 0.0508(5) Uani 1 1 d . . . . .
H21A H 0.4898 0.5333 0.0781 0.061 Uiso 1 1 calc R . . . .
H21B H 0.3608 0.4759 0.0403 0.061 Uiso 1 1 calc R . . . .
C22 C 0.3698(3) 0.48762(13) 0.14815(12) 0.0522(5) Uani 1 1 d . . . . .
H22A H 0.4168 0.5283 0.1804 0.063 Uiso 1 1 calc R . . . .
H22B H 0.2620 0.4978 0.1341 0.063 Uiso 1 1 calc R . . . .
C23 C 0.0757(3) 0.32743(17) 0.17930(12) 0.0650(7) Uani 1 1 d . . . . .
H23A H 0.1253 0.2886 0.1561 0.078 Uiso 1 1 calc R . . . .
H23B H 0.0663 0.3747 0.1514 0.078 Uiso 1 1 calc R . . . .
C24 C -0.0774(3) 0.29945(17) 0.18597(14) 0.0686(7) Uani 1 1 d . . . . .
H24A H -0.1468 0.3423 0.1854 0.082 Uiso 1 1 calc R . . . .
H24B H -0.1203 0.2637 0.1479 0.082 Uiso 1 1 calc R . . . .
C25 C -0.0429(3) 0.25965(19) 0.25705(14) 0.0736(8) Uani 1 1 d . . . . .
H25A H -0.1312 0.2580 0.2777 0.088 Uiso 1 1 calc R . . . .
H25B H -0.0067 0.2073 0.2532 0.088 Uiso 1 1 calc R . . . .
C26 C 0.0777(3) 0.3096(2) 0.29969(13) 0.0737(8) Uani 1 1 d . . . . .
H26A H 0.0336 0.3509 0.3226 0.088 Uiso 1 1 calc R . . . .
H26B H 0.1446 0.2795 0.3362 0.088 Uiso 1 1 calc R . . . .
Li1 Li 0.3638(4) 0.3844(2) 0.27533(17) 0.0460(8) Uani 1 1 d . . . . .
O3A O 0.337(3) 0.4850(13) 0.3258(6) 0.055(3) Uani 0.4731 1 d D U P A 1
C27A C 0.1920(19) 0.5278(10) 0.3068(6) 0.085(5) Uani 0.4731 1 d D U P A 1
H27A H 0.1081 0.4977 0.3162 0.102 Uiso 0.4731 1 calc R . P A 1
H27B H 0.1691 0.5446 0.2574 0.102 Uiso 0.4731 1 calc R . P A 1
C28A C 0.2328(9) 0.5960(4) 0.3588(5) 0.076(2) Uani 0.4731 1 d D U P A 1
H28A H 0.1449 0.6261 0.3631 0.091 Uiso 0.4731 1 calc R . P A 1
H28B H 0.3091 0.6296 0.3467 0.091 Uiso 0.4731 1 calc R . P A 1
C29A C 0.2976(11) 0.5444(7) 0.4279(4) 0.099(3) Uani 0.4731 1 d D U P A 1
H29A H 0.3412 0.5751 0.4697 0.119 Uiso 0.4731 1 calc R . P A 1
H29B H 0.2236 0.5084 0.4386 0.119 Uiso 0.4731 1 calc R . P A 1
C30A C 0.4100(8) 0.5075(5) 0.3971(4) 0.068(2) Uani 0.4731 1 d D U P A 1
H30A H 0.4924 0.5431 0.3961 0.082 Uiso 0.4731 1 calc R . P A 1
H30B H 0.4509 0.4624 0.4249 0.082 Uiso 0.4731 1 calc R . P A 1
O3B O 0.322(3) 0.4734(12) 0.3298(6) 0.064(5) Uani 0.5269 1 d D U P A 2
C30B C 0.2166(16) 0.5335(9) 0.2983(5) 0.066(3) Uani 0.5269 1 d D U P A 2
H30C H 0.1294 0.5119 0.2653 0.079 Uiso 0.5269 1 calc R . P A 2
H30D H 0.2646 0.5716 0.2735 0.079 Uiso 0.5269 1 calc R . P A 2
C29B C 0.1725(9) 0.5684(4) 0.3633(4) 0.085(2) Uani 0.5269 1 d D U P A 2
H29C H 0.1028 0.5358 0.3817 0.102 Uiso 0.5269 1 calc R . P A 2
H29D H 0.1309 0.6202 0.3543 0.102 Uiso 0.5269 1 calc R . P A 2
C28B C 0.3418(10) 0.5687(4) 0.4148(4) 0.088(3) Uani 0.5269 1 d D U P A 2
H28C H 0.4147 0.5980 0.3955 0.105 Uiso 0.5269 1 calc R . P A 2
H28D H 0.3439 0.5844 0.4634 0.105 Uiso 0.5269 1 calc R . P A 2
C27B C 0.3549(8) 0.4815(4) 0.4060(3) 0.0619(18) Uani 0.5269 1 d D U P A 2
H27C H 0.4559 0.4631 0.4276 0.074 Uiso 0.5269 1 calc R . P A 2
H27D H 0.2818 0.4538 0.4266 0.074 Uiso 0.5269 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C1 1.8164(19) . ?
P1 C10 1.829(2) . ?
P1 Li1 2.552(3) . ?
O1 C19 1.432(2) . ?
O1 C22 1.429(3) . ?
O1 Li1 1.944(3) . ?
O2 C23 1.414(3) . ?
O2 C26 1.449(3) . ?
O2 Li1 1.954(4) . ?
C1 C2 1.420(3) . ?
C1 C6 1.415(3) . ?
C2 C3 1.389(3) . ?
C2 C7 1.503(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.378(3) . ?
C4 C5 1.384(3) . ?
C4 C8 1.510(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.386(3) . ?
C6 C9 1.505(3) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.415(3) . ?
C10 C15 1.420(3) . ?
C11 C12 1.389(3) . ?
C11 C16 1.505(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.379(3) . ?
C13 C14 1.382(3) . ?
C13 C17 1.521(3) . ?
C14 H14 0.9300 . ?
C14 C15 1.391(3) . ?
C15 C18 1.503(3) . ?
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 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.497(3) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.511(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.508(3) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.502(3) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.499(4) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.487(4) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
Li1 O3A 2.032(13) . ?
Li1 O3B 1.944(10) . ?
O3A C27A 1.477(12) . ?
O3A C30A 1.437(10) . ?
C27A H27A 0.9700 . ?
C27A H27B 0.9700 . ?
C27A C28A 1.536(13) . ?
C28A H28A 0.9700 . ?
C28A H28B 0.9700 . ?
C28A C29A 1.600(10) . ?
C29A H29A 0.9700 . ?
C29A H29B 0.9700 . ?
C29A C30A 1.437(9) . ?
C30A H30A 0.9700 . ?
C30A H30B 0.9700 . ?
O3B C30B 1.448(11) . ?
O3B C27B 1.436(11) . ?
C30B H30C 0.9700 . ?
C30B H30D 0.9700 . ?
C30B C29B 1.521(11) . ?
C29B H29C 0.9700 . ?
C29B H29D 0.9700 . ?
C29B C28B 1.629(10) . ?
C28B H28C 0.9700 . ?
C28B H28D 0.9700 . ?
C28B C27B 1.523(9) . ?
C27B H27C 0.9700 . ?
C27B H27D 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
C1 P1 C10 110.29(9) . . ?
C1 P1 Li1 122.48(10) . . ?
C10 P1 Li1 97.81(10) . . ?
C19 O1 Li1 122.92(16) . . ?
C22 O1 C19 109.03(15) . . ?
C22 O1 Li1 127.73(16) . . ?
C23 O2 C26 109.06(18) . . ?
C23 O2 Li1 125.68(17) . . ?
C26 O2 Li1 124.92(16) . . ?
C2 C1 P1 125.10(15) . . ?
C6 C1 P1 117.55(14) . . ?
C6 C1 C2 116.58(17) . . ?
C1 C2 C7 121.30(17) . . ?
C3 C2 C1 120.05(19) . . ?
C3 C2 C7 118.51(18) . . ?
C2 C3 H3 118.5 . . ?
C4 C3 C2 122.96(19) . . ?
C4 C3 H3 118.5 . . ?
C3 C4 C5 116.96(18) . . ?
C3 C4 C8 121.5(2) . . ?
C5 C4 C8 121.5(2) . . ?
C4 C5 H5 118.8 . . ?
C4 C5 C6 122.4(2) . . ?
C6 C5 H5 118.8 . . ?
C1 C6 C9 120.88(17) . . ?
C5 C6 C1 120.76(18) . . ?
C5 C6 C9 118.28(18) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 P1 116.65(15) . . ?
C11 C10 C15 117.16(18) . . ?
C15 C10 P1 125.60(15) . . ?
C10 C11 C16 120.90(19) . . ?
C12 C11 C10 120.3(2) . . ?
C12 C11 C16 118.81(19) . . ?
C11 C12 H12 118.6 . . ?
C13 C12 C11 122.7(2) . . ?
C13 C12 H12 118.6 . . ?
C12 C13 C14 117.1(2) . . ?
C12 C13 C17 121.3(2) . . ?
C14 C13 C17 121.6(2) . . ?
C13 C14 H14 118.6 . . ?
C13 C14 C15 122.8(2) . . ?
C15 C14 H14 118.6 . . ?
C10 C15 C18 121.16(19) . . ?
C14 C15 C10 119.9(2) . . ?
C14 C15 C18 118.82(19) . . ?
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 . . ?
O1 C19 H19A 110.8 . . ?
O1 C19 H19B 110.8 . . ?
O1 C19 C20 104.60(17) . . ?
H19A C19 H19B 108.9 . . ?
C20 C19 H19A 110.8 . . ?
C20 C19 H19B 110.8 . . ?
C19 C20 H20A 111.2 . . ?
C19 C20 H20B 111.2 . . ?
C19 C20 C21 102.76(18) . . ?
H20A C20 H20B 109.1 . . ?
C21 C20 H20A 111.2 . . ?
C21 C20 H20B 111.2 . . ?
C20 C21 H21A 111.2 . . ?
C20 C21 H21B 111.2 . . ?
H21A C21 H21B 109.2 . . ?
C22 C21 C20 102.62(17) . . ?
C22 C21 H21A 111.2 . . ?
C22 C21 H21B 111.2 . . ?
O1 C22 C21 107.41(17) . . ?
O1 C22 H22A 110.2 . . ?
O1 C22 H22B 110.2 . . ?
C21 C22 H22A 110.2 . . ?
C21 C22 H22B 110.2 . . ?
H22A C22 H22B 108.5 . . ?
O2 C23 H23A 110.4 . . ?
O2 C23 H23B 110.4 . . ?
O2 C23 C24 106.41(19) . . ?
H23A C23 H23B 108.6 . . ?
C24 C23 H23A 110.4 . . ?
C24 C23 H23B 110.4 . . ?
C23 C24 H24A 111.3 . . ?
C23 C24 H24B 111.3 . . ?
H24A C24 H24B 109.2 . . ?
C25 C24 C23 102.54(19) . . ?
C25 C24 H24A 111.3 . . ?
C25 C24 H24B 111.3 . . ?
C24 C25 H25A 111.3 . . ?
C24 C25 H25B 111.3 . . ?
H25A C25 H25B 109.2 . . ?
C26 C25 C24 102.4(2) . . ?
C26 C25 H25A 111.3 . . ?
C26 C25 H25B 111.3 . . ?
O2 C26 C25 105.89(19) . . ?
O2 C26 H26A 110.6 . . ?
O2 C26 H26B 110.6 . . ?
C25 C26 H26A 110.6 . . ?
C25 C26 H26B 110.6 . . ?
H26A C26 H26B 108.7 . . ?
O1 Li1 P1 105.55(14) . . ?
O1 Li1 O2 101.37(16) . . ?
O1 Li1 O3A 106.0(8) . . ?
O1 Li1 O3B 112.1(7) . . ?
O2 Li1 P1 113.24(17) . . ?
O2 Li1 O3A 103.9(8) . . ?
O3A Li1 P1 124.4(4) . . ?
O3B Li1 P1 123.7(4) . . ?
O3B Li1 O2 98.8(8) . . ?
C27A O3A Li1 120.4(13) . . ?
C30A O3A Li1 127.4(8) . . ?
C30A O3A C27A 107.2(6) . . ?
O3A C27A H27A 112.0 . . ?
O3A C27A H27B 112.0 . . ?
O3A C27A C28A 98.7(10) . . ?
H27A C27A H27B 109.7 . . ?
C28A C27A H27A 112.0 . . ?
C28A C27A H27B 112.0 . . ?
C27A C28A H28A 112.6 . . ?
C27A C28A H28B 112.6 . . ?
C27A C28A C29A 96.0(7) . . ?
H28A C28A H28B 110.1 . . ?
C29A C28A H28A 112.6 . . ?
C29A C28A H28B 112.6 . . ?
C28A C29A H29A 113.0 . . ?
C28A C29A H29B 113.0 . . ?
H29A C29A H29B 110.4 . . ?
C30A C29A C28A 93.8(5) . . ?
C30A C29A H29A 113.0 . . ?
C30A C29A H29B 113.0 . . ?
O3A C30A C29A 107.1(8) . . ?
O3A C30A H30A 110.3 . . ?
O3A C30A H30B 110.3 . . ?
C29A C30A H30A 110.3 . . ?
C29A C30A H30B 110.3 . . ?
H30A C30A H30B 108.5 . . ?
C30B O3B Li1 122.1(7) . . ?
C27B O3B Li1 127.3(10) . . ?
C27B O3B C30B 108.9(6) . . ?
O3B C30B H30C 111.3 . . ?
O3B C30B H30D 111.3 . . ?
O3B C30B C29B 102.2(8) . . ?
H30C C30B H30D 109.2 . . ?
C29B C30B H30C 111.3 . . ?
C29B C30B H30D 111.3 . . ?
C30B C29B H29C 112.4 . . ?
C30B C29B H29D 112.4 . . ?
C30B C29B C28B 96.6(6) . . ?
H29C C29B H29D 110.0 . . ?
C28B C29B H29C 112.4 . . ?
C28B C29B H29D 112.4 . . ?
C29B C28B H28C 113.5 . . ?
C29B C28B H28D 113.5 . . ?
H28C C28B H28D 110.8 . . ?
C27B C28B C29B 90.9(5) . . ?
C27B C28B H28C 113.5 . . ?
C27B C28B H28D 113.5 . . ?
O3B C27B C28B 101.8(8) . . ?
O3B C27B H27C 111.4 . . ?
O3B C27B H27D 111.4 . . ?
C28B C27B H27C 111.4 . . ?
C28B C27B H27D 111.4 . . ?
H27C C27B H27D 109.3 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.038
_oxdiff_exptl_absorpt_empirical_full_min 0.969

#===END
####################################################################### 
# 
# 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_3a
_database_code_depnum_ccdc_archive 'CCDC 1557231'
_audit_update_record             
;
2017-06-20 deposited with the CCDC.
2017-07-20 downloaded from the CCDC.
;
_audit_creation_date             2017-04-13
_audit_creation_method           
;
Olex2 1.2
(compiled Mar 28 2017 19:34:44 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C64 H100 Na2 O4 P2'
_chemical_formula_sum            'C64 H100 Na2 O4 P2'
_chemical_formula_weight         1041.35
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C32 H50 Na1 O2 P1'
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'
Na Na 0.0362 0.0249 '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'
P P 0.1023 0.0942 '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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   18.7669(6)
_cell_length_b                   16.8927(5)
_cell_length_c                   19.9516(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6325.2(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7591
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      27.4950
_cell_measurement_theta_min      3.5920
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.967
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.094
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             2272
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 1 1 0.1147
1 1 -1 0.1270
-2 0 -1 0.1630
-2 -1 2 0.1331
1 1 1 0.1297
-1 -1 -1 0.1417
1 -1 1 0.1511
-1 1 -1 0.1541
1 -1 -1 0.0837
0 0 -1 0.1663

_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.2
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.0002 0.9990 1.0003 0.0203 0.0521 -0.0364
0.9998 1.0003 -0.9995 -0.0143 0.0286 0.0585
-2.0013 -0.0005 -1.0004 0.0833 -0.0050 -0.0044
-1.9997 -1.0010 1.9994 0.0316 -0.0169 -0.1060
1.0006 0.9998 1.0006 -0.0468 0.0476 -0.0018
-1.0006 -0.9998 -1.0006 0.0468 -0.0476 0.0018
1.0011 -0.9995 0.9998 -0.0528 -0.0331 -0.0239
-1.0011 0.9995 -0.9998 0.0528 0.0331 0.0239
1.0002 -0.9990 -1.0003 -0.0203 -0.0521 0.0364
-0.0005 0.0003 -1.0001 0.0162 -0.0095 0.0302

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28208
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.773
_diffrn_reflns_theta_min         3.402
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3968
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -55.00  28.00   1.00   10.00    --   10.16 -38.00-150.00   83
  2  ω    -19.00  43.00   1.00   10.00    --   10.16 -19.00  60.00   62
  3  ω      4.00  43.00   1.00   10.00    --   10.16 -99.00 -30.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0335365000
_diffrn_orient_matrix_UB_12      0.0030141000
_diffrn_orient_matrix_UB_13      -0.0162140000
_diffrn_orient_matrix_UB_21      -0.0022546000
_diffrn_orient_matrix_UB_22      0.0403758000
_diffrn_orient_matrix_UB_23      0.0095116000
_diffrn_orient_matrix_UB_31      0.0172928000
_diffrn_orient_matrix_UB_32      0.0110927000
_diffrn_orient_matrix_UB_33      -0.0301779000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4969
_reflns_number_total             7244
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         7244
_refine_ls_number_restraints     161
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0499
_refine_ls_restrained_S_all      1.028
_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)+(0.0505P)²+2.1441P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1268
_refine_special_details          
;
One tetrahydrofuran molecule coordinated to 
sodium has been modelled as disordered 
over two positions. The occupancies of the 
disordered parts were refined independently 
of the atomic displacement parameters. The 
geometry of the partially-occupied moieties 
was restrained using the SAME card and the 
displacement parameters of the partially- 
occupied atoms were restrained using the 
SIMU card.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Na1-O1B \\sim Na1-O1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1A \\sim C29A \\sim C30A \\sim C31A \\sim C32A \\sim O1B \\sim C29B \\sim C30B
\\sim C31B \\sim C32B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Same fragment restrains
{O1A, C29A, C30A, C31A, C32A} sigma for 1-2: 0.02, 1-3: 0.02
as
{O1B, C29B, C30B, C31B, C32B}
5. Others
 Fixed Sof: O1A(0.62679) C29A(0.62679) H29A(0.62679) H29B(0.62679)
 C30A(0.62679) H30A(0.62679) H30B(0.62679) C31A(0.62679) H31A(0.62679)
 H31B(0.62679) C32A(0.62679) H32A(0.62679) H32B(0.62679) O1B(0.37321)
 C29B(0.37321) H29C(0.37321) H29D(0.37321) C30B(0.37321) H30C(0.37321)
 H30D(0.37321) C31B(0.37321) H31C(0.37321) H31D(0.37321) C32B(0.37321)
 H32C(0.37321) H32D(0.37321)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22)
6.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29A(H29A,
 H29B), C30A(H30A,H30B), C31A(H31A,H31B), C32A(H32A,H32B), C29B(H29C,H29D),
 C30B(H30C,H30D), C31B(H31C,H31D), C32B(H32C,H32D)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17)
6.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
P1 P 0.46740(2) 0.60433(2) 0.42627(2) 0.02301(12) Uani 1 1 d . . . . .
Na1 Na 0.58984(4) 0.51222(4) 0.47253(3) 0.03591(19) Uani 1 1 d D . . . .
O1 O 0.70662(7) 0.55783(9) 0.47190(8) 0.0552(4) Uani 1 1 d . . . . .
C1 C 0.43656(9) 0.70898(10) 0.41819(8) 0.0253(4) Uani 1 1 d . . . . .
C2 C 0.37129(9) 0.72633(10) 0.38501(9) 0.0307(4) Uani 1 1 d . . . . .
C3 C 0.35123(11) 0.80450(12) 0.37394(10) 0.0411(5) Uani 1 1 d . . . . .
H3 H 0.3079 0.8151 0.3510 0.049 Uiso 1 1 calc R . . . .
C4 C 0.39246(12) 0.86700(12) 0.39541(11) 0.0480(5) Uani 1 1 d . . . . .
H4 H 0.3789 0.9200 0.3858 0.058 Uiso 1 1 calc R . . . .
C5 C 0.45333(11) 0.85142(11) 0.43088(10) 0.0429(5) Uani 1 1 d . . . . .
H5 H 0.4807 0.8944 0.4477 0.051 Uiso 1 1 calc R . . . .
C6 C 0.47632(10) 0.77404(10) 0.44305(9) 0.0320(4) Uani 1 1 d . . . . .
C7 C 0.31979(9) 0.66325(11) 0.36078(9) 0.0336(4) Uani 1 1 d . . . . .
H7 H 0.3395 0.6106 0.3744 0.040 Uiso 1 1 calc R . . . .
C8 C 0.31219(11) 0.66309(13) 0.28455(10) 0.0439(5) Uani 1 1 d . . . . .
H8A H 0.2912 0.7133 0.2699 0.066 Uiso 1 1 calc GR . . . .
H8B H 0.2812 0.6192 0.2709 0.066 Uiso 1 1 calc GR . . . .
H8C H 0.3592 0.6566 0.2640 0.066 Uiso 1 1 calc GR . . . .
C9 C 0.24652(10) 0.67253(14) 0.39429(11) 0.0485(5) Uani 1 1 d . . . . .
H9A H 0.2524 0.6733 0.4431 0.073 Uiso 1 1 calc GR . . . .
H9B H 0.2159 0.6280 0.3815 0.073 Uiso 1 1 calc GR . . . .
H9C H 0.2246 0.7222 0.3796 0.073 Uiso 1 1 calc GR . . . .
C10 C 0.54473(10) 0.76547(11) 0.48306(10) 0.0383(5) Uani 1 1 d . . . . .
H10 H 0.5566 0.7078 0.4854 0.046 Uiso 1 1 calc R . . . .
C11 C 0.53501(13) 0.79559(14) 0.55482(11) 0.0560(6) Uani 1 1 d . . . . .
H11A H 0.5239 0.8523 0.5539 0.084 Uiso 1 1 calc GR . . . .
H11B H 0.5791 0.7870 0.5802 0.084 Uiso 1 1 calc GR . . . .
H11C H 0.4959 0.7668 0.5763 0.084 Uiso 1 1 calc GR . . . .
C12 C 0.60778(12) 0.80817(14) 0.45024(13) 0.0569(6) Uani 1 1 d . . . . .
H12A H 0.6139 0.7889 0.4043 0.085 Uiso 1 1 calc GR . . . .
H12B H 0.6512 0.7977 0.4760 0.085 Uiso 1 1 calc GR . . . .
H12C H 0.5985 0.8653 0.4495 0.085 Uiso 1 1 calc GR . . . .
C13 C 0.46624(8) 0.57239(10) 0.33695(8) 0.0243(3) Uani 1 1 d . . . . .
C14 C 0.42523(9) 0.50609(10) 0.31612(8) 0.0297(4) Uani 1 1 d . . . . .
C15 C 0.42770(11) 0.48107(12) 0.24954(9) 0.0411(5) Uani 1 1 d . . . . .
H15 H 0.4006 0.4363 0.2363 0.049 Uiso 1 1 calc R . . . .
C16 C 0.46856(12) 0.51984(13) 0.20272(10) 0.0482(5) Uani 1 1 d . . . . .
H16 H 0.4697 0.5020 0.1576 0.058 Uiso 1 1 calc R . . . .
C17 C 0.50799(11) 0.58505(12) 0.22195(9) 0.0423(5) Uani 1 1 d . . . . .
H17 H 0.5355 0.6125 0.1894 0.051 Uiso 1 1 calc R . . . .
C18 C 0.50824(9) 0.61132(10) 0.28779(9) 0.0305(4) Uani 1 1 d . . . . .
C19 C 0.37848(10) 0.46026(11) 0.36423(9) 0.0352(4) Uani 1 1 d . . . . .
H19 H 0.3678 0.4961 0.4029 0.042 Uiso 1 1 calc R . . . .
C20 C 0.41731(13) 0.38878(12) 0.39216(10) 0.0501(6) Uani 1 1 d . . . . .
H20A H 0.4294 0.3526 0.3555 0.075 Uiso 1 1 calc GR . . . .
H20B H 0.3866 0.3614 0.4244 0.075 Uiso 1 1 calc GR . . . .
H20C H 0.4610 0.4061 0.4147 0.075 Uiso 1 1 calc GR . . . .
C21 C 0.30686(13) 0.43505(16) 0.33417(12) 0.0629(7) Uani 1 1 d . . . . .
H21A H 0.2846 0.4805 0.3120 0.094 Uiso 1 1 calc GR . . . .
H21B H 0.2756 0.4158 0.3699 0.094 Uiso 1 1 calc GR . . . .
H21C H 0.3146 0.3928 0.3014 0.094 Uiso 1 1 calc GR . . . .
C22 C 0.55440(10) 0.68241(12) 0.30385(10) 0.0410(5) Uani 1 1 d . . . . .
H22 H 0.5537 0.6898 0.3536 0.049 Uiso 1 1 calc R . . . .
C23 C 0.52412(15) 0.75773(13) 0.27207(12) 0.0621(7) Uani 1 1 d . . . . .
H23A H 0.5265 0.7534 0.2231 0.093 Uiso 1 1 calc GR . . . .
H23B H 0.5521 0.8035 0.2868 0.093 Uiso 1 1 calc GR . . . .
H23C H 0.4744 0.7645 0.2860 0.093 Uiso 1 1 calc GR . . . .
C24 C 0.63211(13) 0.66999(18) 0.28285(15) 0.0748(8) Uani 1 1 d . . . . .
H24A H 0.6506 0.6217 0.3038 0.112 Uiso 1 1 calc GR . . . .
H24B H 0.6607 0.7155 0.2973 0.112 Uiso 1 1 calc GR . . . .
H24C H 0.6348 0.6649 0.2340 0.112 Uiso 1 1 calc GR . . . .
C25 C 0.73571(14) 0.63327(15) 0.45730(15) 0.0685(7) Uani 1 1 d . . . . .
H25A H 0.7413 0.6646 0.4989 0.082 Uiso 1 1 calc R . . . .
H25B H 0.7041 0.6626 0.4263 0.082 Uiso 1 1 calc R . . . .
C26 C 0.80680(15) 0.61892(19) 0.42542(16) 0.0834(9) Uani 1 1 d . . . . .
H26A H 0.8044 0.6284 0.3765 0.100 Uiso 1 1 calc R . . . .
H26B H 0.8434 0.6543 0.4450 0.100 Uiso 1 1 calc R . . . .
C27 C 0.82403(15) 0.53428(17) 0.43972(16) 0.0765(8) Uani 1 1 d . . . . .
H27A H 0.8249 0.5028 0.3979 0.092 Uiso 1 1 calc R . . . .
H27B H 0.8708 0.5295 0.4622 0.092 Uiso 1 1 calc R . . . .
C28 C 0.76562(12) 0.50745(15) 0.48454(14) 0.0635(7) Uani 1 1 d . . . . .
H28A H 0.7530 0.4517 0.4748 0.076 Uiso 1 1 calc R . . . .
H28B H 0.7804 0.5114 0.5320 0.076 Uiso 1 1 calc R . . . .
O1A O 0.6033(2) 0.4107(3) 0.3935(2) 0.0424(10) Uani 0.6268 1 d D U P A 1
C29A C 0.6385(7) 0.3378(5) 0.4041(4) 0.054(2) Uani 0.6268 1 d D U P A 1
H29A H 0.6068 0.2929 0.3928 0.064 Uiso 0.6268 1 calc R . P A 1
H29B H 0.6536 0.3327 0.4514 0.064 Uiso 0.6268 1 calc R . P A 1
C30A C 0.7027(2) 0.3394(3) 0.3579(3) 0.0712(15) Uani 0.6268 1 d D U P A 1
H30A H 0.7464 0.3542 0.3828 0.085 Uiso 0.6268 1 calc R . P A 1
H30B H 0.7101 0.2872 0.3365 0.085 Uiso 0.6268 1 calc R . P A 1
C31A C 0.6842(3) 0.4006(4) 0.3073(3) 0.082(2) Uani 0.6268 1 d D U P A 1
H31A H 0.6896 0.3795 0.2613 0.098 Uiso 0.6268 1 calc R . P A 1
H31B H 0.7149 0.4478 0.3123 0.098 Uiso 0.6268 1 calc R . P A 1
C32A C 0.6071(3) 0.4207(3) 0.3217(3) 0.0542(14) Uani 0.6268 1 d D U P A 1
H32A H 0.5959 0.4758 0.3085 0.065 Uiso 0.6268 1 calc R . P A 1
H32B H 0.5743 0.3841 0.2983 0.065 Uiso 0.6268 1 calc R . P A 1
O1B O 0.6288(4) 0.4269(5) 0.3978(4) 0.052(2) Uani 0.3732 1 d D U P A 2
C29B C 0.6484(14) 0.3496(9) 0.4107(6) 0.072(6) Uani 0.3732 1 d D U P A 2
H29C H 0.6112 0.3227 0.4375 0.086 Uiso 0.3732 1 calc R . P A 2
H29D H 0.6938 0.3481 0.4359 0.086 Uiso 0.3732 1 calc R . P A 2
C30B C 0.6568(8) 0.3102(5) 0.3451(5) 0.118(4) Uani 0.3732 1 d D U P A 2
H30C H 0.7024 0.2808 0.3433 0.142 Uiso 0.3732 1 calc R . P A 2
H30D H 0.6173 0.2725 0.3372 0.142 Uiso 0.3732 1 calc R . P A 2
C31B C 0.6559(8) 0.3728(6) 0.2951(4) 0.091(4) Uani 0.3732 1 d D U P A 2
H31C H 0.6201 0.3610 0.2600 0.109 Uiso 0.3732 1 calc R . P A 2
H31D H 0.7032 0.3776 0.2736 0.109 Uiso 0.3732 1 calc R . P A 2
C32B C 0.6374(6) 0.4472(5) 0.3300(4) 0.066(3) Uani 0.3732 1 d D U P A 2
H32C H 0.6760 0.4867 0.3247 0.079 Uiso 0.3732 1 calc R . P A 2
H32D H 0.5928 0.4697 0.3117 0.079 Uiso 0.3732 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 Na1 3.0178(8) 5_666 ?
P1 Na1 2.9246(8) . ?
P1 C1 1.8672(17) . ?
P1 C13 1.8622(16) . ?
Na1 P1 3.0178(8) 5_666 ?
Na1 Na1 3.5698(14) 5_666 ?
Na1 O1 2.3231(16) . ?
Na1 O1A 2.343(4) . ?
Na1 O1B 2.199(7) . ?
O1 C25 1.417(3) . ?
O1 C28 1.419(3) . ?
C1 C2 1.423(2) . ?
C1 C6 1.418(2) . ?
C2 C3 1.391(3) . ?
C2 C7 1.518(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.377(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.369(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.398(3) . ?
C6 C10 1.519(3) . ?
C7 H7 1.0000 . ?
C7 C8 1.528(3) . ?
C7 C9 1.537(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 1.0000 . ?
C10 C11 1.530(3) . ?
C10 C12 1.533(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.421(2) . ?
C13 C18 1.420(2) . ?
C14 C15 1.395(2) . ?
C14 C19 1.513(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.375(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.381(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.387(3) . ?
C18 C22 1.515(3) . ?
C19 H19 1.0000 . ?
C19 C20 1.516(3) . ?
C19 C21 1.532(3) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22 1.0000 . ?
C22 C23 1.531(3) . ?
C22 C24 1.532(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.498(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.493(4) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.485(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
O1A C29A 1.414(7) . ?
O1A C32A 1.443(6) . ?
C29A H29A 0.9900 . ?
C29A H29B 0.9900 . ?
C29A C30A 1.517(10) . ?
C30A H30A 0.9900 . ?
C30A H30B 0.9900 . ?
C30A C31A 1.486(7) . ?
C31A H31A 0.9900 . ?
C31A H31B 0.9900 . ?
C31A C32A 1.514(7) . ?
C32A H32A 0.9900 . ?
C32A H32B 0.9900 . ?
O1B C29B 1.381(11) . ?
O1B C32B 1.404(9) . ?
C29B H29C 0.9900 . ?
C29B H29D 0.9900 . ?
C29B C30B 1.477(13) . ?
C30B H30C 0.9900 . ?
C30B H30D 0.9900 . ?
C30B C31B 1.454(10) . ?
C31B H31C 0.9900 . ?
C31B H31D 0.9900 . ?
C31B C32B 1.477(10) . ?
C32B H32C 0.9900 . ?
C32B H32D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Na1 P1 Na1 73.83(2) . 5_666 ?
C1 P1 Na1 140.76(6) . . ?
C1 P1 Na1 124.41(5) . 5_666 ?
C13 P1 Na1 116.56(6) . 5_666 ?
C13 P1 Na1 99.03(5) . . ?
C13 P1 C1 100.84(7) . . ?
P1 Na1 P1 106.17(2) . 5_666 ?
P1 Na1 Na1 54.28(2) . 5_666 ?
P1 Na1 Na1 51.89(2) 5_666 5_666 ?
O1 Na1 P1 123.76(5) . 5_666 ?
O1 Na1 P1 124.27(5) . . ?
O1 Na1 Na1 158.62(6) . 5_666 ?
O1 Na1 O1A 97.90(11) . . ?
O1A Na1 P1 105.15(13) . . ?
O1A Na1 P1 90.65(13) . 5_666 ?
O1A Na1 Na1 102.93(10) . 5_666 ?
O1B Na1 P1 113.3(2) . . ?
O1B Na1 P1 98.3(2) . 5_666 ?
O1B Na1 Na1 116.54(19) . 5_666 ?
O1B Na1 O1 84.2(2) . . ?
C25 O1 Na1 131.53(14) . . ?
C25 O1 C28 105.98(17) . . ?
C28 O1 Na1 122.43(13) . . ?
C2 C1 P1 120.13(13) . . ?
C6 C1 P1 122.72(13) . . ?
C6 C1 C2 117.14(15) . . ?
C1 C2 C7 123.49(15) . . ?
C3 C2 C1 120.17(17) . . ?
C3 C2 C7 116.33(16) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 C2 121.76(18) . . ?
C4 C3 H3 119.1 . . ?
C3 C4 H4 120.6 . . ?
C5 C4 C3 118.81(18) . . ?
C5 C4 H4 120.6 . . ?
C4 C5 H5 119.1 . . ?
C4 C5 C6 121.81(19) . . ?
C6 C5 H5 119.1 . . ?
C1 C6 C10 123.70(15) . . ?
C5 C6 C1 120.11(17) . . ?
C5 C6 C10 116.19(16) . . ?
C2 C7 H7 107.6 . . ?
C2 C7 C8 112.20(16) . . ?
C2 C7 C9 111.08(16) . . ?
C8 C7 H7 107.6 . . ?
C8 C7 C9 110.48(15) . . ?
C9 C7 H7 107.6 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 H10 107.8 . . ?
C6 C10 C11 111.05(17) . . ?
C6 C10 C12 112.53(17) . . ?
C11 C10 H10 107.8 . . ?
C11 C10 C12 109.59(17) . . ?
C12 C10 H10 107.8 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 P1 120.97(12) . . ?
C18 C13 P1 121.36(13) . . ?
C18 C13 C14 117.63(15) . . ?
C13 C14 C19 122.12(15) . . ?
C15 C14 C13 119.95(16) . . ?
C15 C14 C19 117.92(16) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 C14 121.43(19) . . ?
C16 C15 H15 119.3 . . ?
C15 C16 H16 120.3 . . ?
C15 C16 C17 119.34(18) . . ?
C17 C16 H16 120.3 . . ?
C16 C17 H17 119.3 . . ?
C16 C17 C18 121.34(18) . . ?
C18 C17 H17 119.3 . . ?
C13 C18 C22 122.59(16) . . ?
C17 C18 C13 120.28(17) . . ?
C17 C18 C22 117.13(16) . . ?
C14 C19 H19 107.1 . . ?
C14 C19 C20 111.21(16) . . ?
C14 C19 C21 113.73(16) . . ?
C20 C19 H19 107.1 . . ?
C20 C19 C21 110.13(17) . . ?
C21 C19 H19 107.1 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22 H22 107.5 . . ?
C18 C22 C23 111.04(18) . . ?
C18 C22 C24 112.21(18) . . ?
C23 C22 H22 107.5 . . ?
C23 C22 C24 110.73(19) . . ?
C24 C22 H22 107.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O1 C25 H25A 110.4 . . ?
O1 C25 H25B 110.4 . . ?
O1 C25 C26 106.6(2) . . ?
H25A C25 H25B 108.6 . . ?
C26 C25 H25A 110.4 . . ?
C26 C25 H25B 110.4 . . ?
C25 C26 H26A 110.6 . . ?
C25 C26 H26B 110.6 . . ?
H26A C26 H26B 108.8 . . ?
C27 C26 C25 105.5(2) . . ?
C27 C26 H26A 110.6 . . ?
C27 C26 H26B 110.6 . . ?
C26 C27 H27A 110.9 . . ?
C26 C27 H27B 110.9 . . ?
H27A C27 H27B 108.9 . . ?
C28 C27 C26 104.3(2) . . ?
C28 C27 H27A 110.9 . . ?
C28 C27 H27B 110.9 . . ?
O1 C28 C27 106.6(2) . . ?
O1 C28 H28A 110.4 . . ?
O1 C28 H28B 110.4 . . ?
C27 C28 H28A 110.4 . . ?
C27 C28 H28B 110.4 . . ?
H28A C28 H28B 108.6 . . ?
C29A O1A Na1 125.9(5) . . ?
C29A O1A C32A 103.1(4) . . ?
C32A O1A Na1 126.0(4) . . ?
O1A C29A H29A 110.7 . . ?
O1A C29A H29B 110.7 . . ?
O1A C29A C30A 105.4(5) . . ?
H29A C29A H29B 108.8 . . ?
C30A C29A H29A 110.7 . . ?
C30A C29A H29B 110.7 . . ?
C29A C30A H30A 111.0 . . ?
C29A C30A H30B 111.0 . . ?
H30A C30A H30B 109.0 . . ?
C31A C30A C29A 103.8(4) . . ?
C31A C30A H30A 111.0 . . ?
C31A C30A H30B 111.0 . . ?
C30A C31A H31A 110.8 . . ?
C30A C31A H31B 110.8 . . ?
C30A C31A C32A 104.5(4) . . ?
H31A C31A H31B 108.9 . . ?
C32A C31A H31A 110.8 . . ?
C32A C31A H31B 110.8 . . ?
O1A C32A C31A 102.1(4) . . ?
O1A C32A H32A 111.4 . . ?
O1A C32A H32B 111.4 . . ?
C31A C32A H32A 111.4 . . ?
C31A C32A H32B 111.4 . . ?
H32A C32A H32B 109.2 . . ?
C29B O1B Na1 125.6(7) . . ?
C29B O1B C32B 112.3(7) . . ?
C32B O1B Na1 122.1(6) . . ?
O1B C29B H29C 110.3 . . ?
O1B C29B H29D 110.3 . . ?
O1B C29B C30B 106.9(8) . . ?
H29C C29B H29D 108.6 . . ?
C30B C29B H29C 110.3 . . ?
C30B C29B H29D 110.3 . . ?
C29B C30B H30C 110.5 . . ?
C29B C30B H30D 110.5 . . ?
H30C C30B H30D 108.7 . . ?
C31B C30B C29B 106.1(7) . . ?
C31B C30B H30C 110.5 . . ?
C31B C30B H30D 110.5 . . ?
C30B C31B H31C 110.2 . . ?
C30B C31B H31D 110.2 . . ?
C30B C31B C32B 107.4(6) . . ?
H31C C31B H31D 108.5 . . ?
C32B C31B H31C 110.2 . . ?
C32B C31B H31D 110.2 . . ?
O1B C32B C31B 105.9(6) . . ?
O1B C32B H32C 110.6 . . ?
O1B C32B H32D 110.6 . . ?
C31B C32B H32C 110.6 . . ?
C31B C32B H32D 110.6 . . ?
H32C C32B H32D 108.7 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.019
_oxdiff_exptl_absorpt_empirical_full_min 0.981
####################################################################### 
# 
# 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_2a
_database_code_depnum_ccdc_archive 'CCDC 1557230'
_audit_update_record             
;
2017-06-20 deposited with the CCDC.
2017-07-20 downloaded from the CCDC.
;
_audit_creation_date             2015-03-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H58 Li O3 P, C36.02 H58.62 Li O3.01 P'
_chemical_formula_sum            'C72.02 H116.62 Li2 O6.01 P2'
_chemical_formula_weight         1154.41
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C72 H102 P3 As1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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                   11.32606(19)
_cell_length_b                   17.4145(5)
_cell_length_c                   19.3933(5)
_cell_angle_alpha                68.346(3)
_cell_angle_beta                 80.5527(18)
_cell_angle_gamma                89.5652(18)
_cell_volume                     3501.06(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    22496
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      66.8490
_cell_measurement_theta_min      3.9560
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.922
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95066
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1266
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49842
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.966
_diffrn_reflns_theta_min         2.489
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   13.00  113.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7155   57.0000  -60.0000 100

#__ type_ start__ end____ width___ exp.time_
  2 omega  -25.00   69.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7155  -57.0000  150.0000 94

#__ type_ start__ end____ width___ exp.time_
  3 omega   -1.00   71.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7155 -125.0000   90.0000 72

#__ type_ start__ end____ width___ exp.time_
  4 omega   36.00   62.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7155   38.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
  5 omega   11.00  106.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000 -171.9710 95

#__ type_ start__ end____ width___ exp.time_
  6 omega   18.00  133.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000 -136.6496 115

#__ type_ start__ end____ width___ exp.time_
  7 omega   30.00   74.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  -60.3306 44

#__ type_ start__ end____ width___ exp.time_
  8 omega   49.00   77.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000  120.0000 28

#__ type_ start__ end____ width___ exp.time_
  9 omega   97.00  123.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000   59.3439 26

#__ type_ start__ end____ width___ exp.time_
 10 omega   87.00  151.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000  -90.0000 64

#__ type_ start__ end____ width___ exp.time_
 11 omega  143.00  168.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000 -150.0000 25

#__ type_ start__ end____ width___ exp.time_
 12 omega  108.00  164.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000 -150.0000 56

#__ type_ start__ end____ width___ exp.time_
 13 omega   66.00   91.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000  -90.0000 25

#__ type_ start__ end____ width___ exp.time_
 14 omega  122.00  167.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000  -90.0000 45

#__ type_ start__ end____ width___ exp.time_
 15 omega   24.00   70.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   30.0000 46

#__ type_ start__ end____ width___ exp.time_
 16 omega   58.00  107.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  122.4333 49

#__ type_ start__ end____ width___ exp.time_
 17 omega   21.00   76.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -90.0000 55

#__ type_ start__ end____ width___ exp.time_
 18 omega   12.00   38.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
 19 omega   51.00   83.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  -90.0000 32

#__ type_ start__ end____ width___ exp.time_
 20 omega   23.00   57.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -30.0000 34

#__ type_ start__ end____ width___ exp.time_
 21 omega   26.00   75.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   90.0000 49

#__ type_ start__ end____ width___ exp.time_
 22 omega   83.00  120.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000 -150.0000 37

#__ type_ start__ end____ width___ exp.time_
 23 omega   98.00  177.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000    0.0000 79

#__ type_ start__ end____ width___ exp.time_
 24 omega   77.00  103.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 25 omega   36.00   62.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
 26 omega  119.00  145.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
 27 omega   20.00   68.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000    0.0000 48

#__ type_ start__ end____ width___ exp.time_
 28 omega   31.00   68.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  -90.0000 37

#__ type_ start__ end____ width___ exp.time_
 29 omega   51.00   83.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000   30.0000 32

#__ type_ start__ end____ width___ exp.time_
 30 omega   22.00   77.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -150.0000 55

#__ type_ start__ end____ width___ exp.time_
 31 omega    9.00   39.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  122.4333 30

#__ type_ start__ end____ width___ exp.time_
 32 omega   87.00  130.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  -60.3306 43

#__ type_ start__ end____ width___ exp.time_
 33 omega   34.00   60.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 34 omega   46.00   88.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000  -90.0000 42

#__ type_ start__ end____ width___ exp.time_
 35 omega    9.00   55.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000 -180.0000 46

#__ type_ start__ end____ width___ exp.time_
 36 omega   78.00  104.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 37 omega   62.00   88.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
 38 omega   98.00  123.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000    0.0000 25

#__ type_ start__ end____ width___ exp.time_
 39 omega   14.00   57.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000 -150.0000 43

#__ type_ start__ end____ width___ exp.time_
 40 omega   24.00   49.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000 -180.0000 25

#__ type_ start__ end____ width___ exp.time_
 41 omega   96.00  123.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000    4.5345 27

#__ type_ start__ end____ width___ exp.time_
 42 omega   39.00   75.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000    4.5345 36

#__ type_ start__ end____ width___ exp.time_
 43 omega  -71.00   25.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.7155   57.0000  -30.0000 96

#__ type_ start__ end____ width___ exp.time_
 44 omega    8.00  120.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7155   77.0000 -180.0000 112

#__ type_ start__ end____ width___ exp.time_
 45 omega    8.00  120.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7155   77.0000   30.0000 112

#__ type_ start__ end____ width___ exp.time_
 46 omega   12.00  116.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7155   57.0000  120.0000 104
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0013714000
_diffrn_orient_matrix_UB_12      0.0772535000
_diffrn_orient_matrix_UB_13      -0.0721901000
_diffrn_orient_matrix_UB_21      -0.0156316000
_diffrn_orient_matrix_UB_22      -0.0558501000
_diffrn_orient_matrix_UB_23      -0.0440667000
_diffrn_orient_matrix_UB_31      -0.1372260000
_diffrn_orient_matrix_UB_32      0.0015887000
_diffrn_orient_matrix_UB_33      0.0194624000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9868
_reflns_number_total             12397
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.038
_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     856
_refine_ls_number_reflns         12397
_refine_ls_number_restraints     169
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0390
_refine_ls_restrained_S_all      1.029
_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)+(0.0522P)²+0.7854P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1047
_refine_special_details          
;
There is disorder in this structure involving two 
orientations of a THF molecule and one of a diethyl 
ether molecule coordinating to a lithium centre. The 
occupancies of these three parts were allowed to 
refine with isotropic atom treatment. Upon 
convergence, the occupancies were fixed before 
anisotropy was introduced to the model. Restraints 
were applied a appropriate to model this disorder.
;
_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. Restrained distances
 O6C-C69C \\sim O6C-C71C
 with sigma of 0.02
 C36-C35B \\sim C35A-C36
 with sigma of 0.02
 C35A-C34 \\sim C34-C35B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C71A \\sim C72A \\sim C71C: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O6A \\sim O6B \\sim O6C: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C69A \\sim C69B \\sim C69C: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C71A \\sim C71C: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C71A \\sim C71B \\sim C72C: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C70A \\sim C70B \\sim C70C: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C35A \\sim C35B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
4. Rigid body (RIGU) restrains
 O6A, C69A, C70A, C71A, C71A, C72A, O6B, C69B, C70B, C71B, O6C, C69C, C70C,
 C71C, C72C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O6A, C69A, C70A, C71A, C72A} sigma for 1-2: 0.02, 1-3: 0.02
as
{O6B, C69B, C70B, C71B, C72B}
6. Others
 Fixed Sof: H34A(0.72735) H34B(0.72735) H34C(0.27265) H34D(0.27265)
 H36A(0.72735) H36B(0.72735) H36C(0.27265) H36D(0.27265) O6A(0.39127)
 C69A(0.39127) H69A(0.39127) H69B(0.39127) C70A(0.39127) H70A(0.39127)
 H70B(0.39127) C71A(0.39127) H71A(0.39127) H71B(0.39127) C72A(0.39127)
 H72A(0.39127) H72B(0.39127) C35A(0.72735) H35A(0.72735) H35B(0.72735)
 O6B(0.32268) C69B(0.32268) H69C(0.32268) H69D(0.32268) C70B(0.32268)
 H70C(0.32268) H70D(0.32268) C71B(0.32268) H71C(0.32268) H71D(0.32268)
 C72B(0.32268) H72C(0.32268) H72D(0.32268) C35B(0.27265) H35C(0.27265)
 H35D(0.27265) O6C(0.2913) C69C(0.2913) H69E(0.2913) H69F(0.2913) C70C(0.2913)
 H70E(0.2913) H70F(0.2913) H70G(0.2913) C71C(0.2913) H71E(0.2913) H71F(0.2913)
 C72C(0.2913) H72E(0.2913) H72F(0.2913) H72G(0.2913)
7.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22), C43(H43), C46(H46), C55(H55), C58(H58)
7.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B), C34(H34C,H34D), C36(H36A,H36B), C36(H36C,H36D), C61(H61A,H61B),
  C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C66(H66A,
 H66B), C67(H67A,H67B), C68(H68A,H68B), C69A(H69A,H69B), C70A(H70A,H70B),
 C71A(H71A,H71B), C72A(H72A,H72B), C35A(H35A,H35B), C69B(H69C,H69D), C70B(H70C,
 H70D), C71B(H71C,H71D), C72B(H72C,H72D), C35B(H35C,H35D), C69C(H69E,H69F),
 C71C(H71E,H71F)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C39(H39), C40(H40),
 C41(H41), C51(H51), C52(H52), C53(H53)
7.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C),
 C60(H60A,H60B,H60C), C70C(H70E,H70F,H70G), C72C(H72E,H72F,H72G)
;
_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
P1 P 0.18238(3) 0.96281(2) 0.25678(2) 0.02446(9) Uani 1 1 d . . . . .
P2 P 0.44621(3) 0.45219(2) 0.27237(2) 0.02296(9) Uani 1 1 d . . . . .
O1 O 0.47035(10) 0.86638(7) 0.25221(7) 0.0367(3) Uani 1 1 d . . . . .
O2 O 0.44883(10) 1.02058(7) 0.31076(6) 0.0340(3) Uani 1 1 d . . . . .
O3 O 0.51014(10) 1.04183(7) 0.14679(6) 0.0356(3) Uani 1 1 d . . . . .
O4 O 0.15370(10) 0.52401(7) 0.31118(7) 0.0375(3) Uani 1 1 d . . . . .
O5 O 0.16137(10) 0.36192(7) 0.26492(7) 0.0342(3) Uani 1 1 d . . . . .
C1 C 0.09345(12) 0.86338(9) 0.29082(8) 0.0226(3) Uani 1 1 d . . . . .
C2 C 0.03287(13) 0.83933(9) 0.24263(9) 0.0257(3) Uani 1 1 d . . . . .
C3 C -0.03766(14) 0.76526(10) 0.27174(10) 0.0319(4) Uani 1 1 d . . . . .
H3 H -0.0797 0.7511 0.2403 0.038 Uiso 1 1 calc R . . . .
C4 C -0.04649(15) 0.71254(10) 0.34592(10) 0.0345(4) Uani 1 1 d . . . . .
H4 H -0.0942 0.6636 0.3644 0.041 Uiso 1 1 calc R . . . .
C5 C 0.01623(14) 0.73330(10) 0.39242(9) 0.0314(4) Uani 1 1 d . . . . .
H5 H 0.0123 0.6970 0.4420 0.038 Uiso 1 1 calc R . . . .
C6 C 0.08533(13) 0.80745(9) 0.36680(9) 0.0252(3) Uani 1 1 d . . . . .
C7 C 0.04214(14) 0.89122(10) 0.15930(9) 0.0302(3) Uani 1 1 d . . . . .
H7 H 0.1019 0.9368 0.1469 0.036 Uiso 1 1 calc R . . . .
C8 C 0.08661(18) 0.84126(13) 0.11046(11) 0.0457(5) Uani 1 1 d . . . . .
H8A H 0.1611 0.8182 0.1229 0.069 Uiso 1 1 calc GR . . . .
H8B H 0.0983 0.8769 0.0582 0.069 Uiso 1 1 calc GR . . . .
H8C H 0.0282 0.7974 0.1197 0.069 Uiso 1 1 calc GR . . . .
C9 C -0.07550(16) 0.92937(12) 0.13950(10) 0.0408(4) Uani 1 1 d . . . . .
H9A H -0.1356 0.8861 0.1498 0.061 Uiso 1 1 calc GR . . . .
H9B H -0.0637 0.9641 0.0870 0.061 Uiso 1 1 calc GR . . . .
H9C H -0.1012 0.9619 0.1693 0.061 Uiso 1 1 calc GR . . . .
C10 C 0.14886(14) 0.82692(10) 0.42230(9) 0.0288(3) Uani 1 1 d . . . . .
H10 H 0.1694 0.8866 0.4013 0.035 Uiso 1 1 calc R . . . .
C11 C 0.0710(2) 0.80673(16) 0.49978(11) 0.0564(6) Uani 1 1 d . . . . .
H11A H -0.0035 0.8329 0.4940 0.085 Uiso 1 1 calc GR . . . .
H11B H 0.1122 0.8267 0.5299 0.085 Uiso 1 1 calc GR . . . .
H11C H 0.0556 0.7479 0.5241 0.085 Uiso 1 1 calc GR . . . .
C12 C 0.26564(18) 0.78346(14) 0.43063(12) 0.0490(5) Uani 1 1 d . . . . .
H12A H 0.2494 0.7248 0.4473 0.074 Uiso 1 1 calc GR . . . .
H12B H 0.3025 0.7955 0.4669 0.074 Uiso 1 1 calc GR . . . .
H12C H 0.3187 0.8026 0.3829 0.074 Uiso 1 1 calc GR . . . .
C13 C 0.07267(13) 1.03958(9) 0.21968(9) 0.0242(3) Uani 1 1 d . . . . .
C14 C 0.09935(14) 1.10176(10) 0.14642(9) 0.0292(3) Uani 1 1 d . . . . .
C15 C 0.01570(16) 1.16001(11) 0.11999(10) 0.0380(4) Uani 1 1 d . . . . .
H15 H 0.0345 1.2007 0.0720 0.046 Uiso 1 1 calc R . . . .
C16 C -0.09403(16) 1.15845(11) 0.16353(11) 0.0407(4) Uani 1 1 d . . . . .
H16 H -0.1495 1.1968 0.1446 0.049 Uiso 1 1 calc R . . . .
C17 C -0.12068(15) 1.09941(11) 0.23532(10) 0.0349(4) Uani 1 1 d . . . . .
H17 H -0.1948 1.0984 0.2646 0.042 Uiso 1 1 calc R . . . .
C18 C -0.03933(13) 1.04120(9) 0.26508(9) 0.0273(3) Uani 1 1 d . . . . .
C19 C 0.21863(15) 1.10925(11) 0.09486(9) 0.0354(4) Uani 1 1 d . . . . .
H19 H 0.2609 1.0592 0.1174 0.043 Uiso 1 1 calc R . . . .
C20 C 0.2052(2) 1.11503(14) 0.01598(11) 0.0526(5) Uani 1 1 d . . . . .
H20A H 0.1586 1.0674 0.0197 0.079 Uiso 1 1 calc GR . . . .
H20B H 0.2831 1.1170 -0.0132 0.079 Uiso 1 1 calc GR . . . .
H20C H 0.1656 1.1643 -0.0081 0.079 Uiso 1 1 calc GR . . . .
C21 C 0.29535(18) 1.18301(12) 0.09081(11) 0.0468(5) Uani 1 1 d . . . . .
H21A H 0.2543 1.2328 0.0713 0.070 Uiso 1 1 calc GR . . . .
H21B H 0.3706 1.1871 0.0582 0.070 Uiso 1 1 calc GR . . . .
H21C H 0.3094 1.1755 0.1403 0.070 Uiso 1 1 calc GR . . . .
C22 C -0.07410(14) 0.98313(10) 0.34689(10) 0.0320(4) Uani 1 1 d . . . . .
H22 H -0.0062 0.9487 0.3600 0.038 Uiso 1 1 calc R . . . .
C23 C -0.09562(18) 1.03065(12) 0.40009(11) 0.0445(4) Uani 1 1 d . . . . .
H23A H -0.0246 1.0638 0.3941 0.067 Uiso 1 1 calc GR . . . .
H23B H -0.1147 0.9921 0.4512 0.067 Uiso 1 1 calc GR . . . .
H23C H -0.1611 1.0658 0.3883 0.067 Uiso 1 1 calc GR . . . .
C24 C -0.18213(17) 0.92487(13) 0.35892(13) 0.0498(5) Uani 1 1 d . . . . .
H24A H -0.2500 0.9567 0.3452 0.075 Uiso 1 1 calc GR . . . .
H24B H -0.2002 0.8888 0.4110 0.075 Uiso 1 1 calc GR . . . .
H24C H -0.1641 0.8925 0.3282 0.075 Uiso 1 1 calc GR . . . .
C25 C 0.59141(16) 0.85218(12) 0.26692(12) 0.0436(4) Uani 1 1 d . . . . .
H25A H 0.5952 0.8468 0.3181 0.052 Uiso 1 1 calc R . . . .
H25B H 0.6459 0.8979 0.2325 0.052 Uiso 1 1 calc R . . . .
C26 C 0.62445(18) 0.77395(13) 0.25565(14) 0.0527(5) Uani 1 1 d . . . . .
H26A H 0.6749 0.7426 0.2909 0.063 Uiso 1 1 calc R . . . .
H26B H 0.6658 0.7852 0.2047 0.063 Uiso 1 1 calc R . . . .
C27 C 0.50468(18) 0.72856(12) 0.27039(14) 0.0523(5) Uani 1 1 d . . . . .
H27A H 0.4770 0.6993 0.3239 0.063 Uiso 1 1 calc R . . . .
H27B H 0.5083 0.6896 0.2451 0.063 Uiso 1 1 calc R . . . .
C28 C 0.42432(17) 0.79849(11) 0.23733(11) 0.0419(4) Uani 1 1 d . . . . .
H28A H 0.4297 0.8123 0.1836 0.050 Uiso 1 1 calc R . . . .
H28B H 0.3414 0.7834 0.2617 0.050 Uiso 1 1 calc R . . . .
C29 C 0.46941(19) 0.97812(14) 0.38572(11) 0.0494(5) Uani 1 1 d . . . . .
H29A H 0.5485 0.9942 0.3905 0.059 Uiso 1 1 calc R . . . .
H29B H 0.4648 0.9188 0.3981 0.059 Uiso 1 1 calc R . . . .
C30 C 0.37541(18) 1.00061(14) 0.43776(11) 0.0485(5) Uani 1 1 d . . . . .
H30A H 0.4119 1.0222 0.4692 0.058 Uiso 1 1 calc R . . . .
H30B H 0.3229 0.9527 0.4699 0.058 Uiso 1 1 calc R . . . .
C31 C 0.30640(18) 1.06598(12) 0.38714(11) 0.0450(4) Uani 1 1 d . . . . .
H31A H 0.2291 1.0432 0.3862 0.054 Uiso 1 1 calc R . . . .
H31B H 0.2942 1.1121 0.4037 0.054 Uiso 1 1 calc R . . . .
C32 C 0.38544(18) 1.09269(11) 0.31081(11) 0.0411(4) Uani 1 1 d . . . . .
H32A H 0.3376 1.1101 0.2711 0.049 Uiso 1 1 calc R . . . .
H32B H 0.4411 1.1382 0.3036 0.049 Uiso 1 1 calc R . . . .
C33 C 0.60339(19) 1.10057(14) 0.13962(12) 0.0546(6) Uani 1 1 d . . . . .
H33A H 0.6513 1.0771 0.1788 0.066 Uiso 1 1 calc R . . . .
H33B H 0.5691 1.1498 0.1447 0.066 Uiso 1 1 calc R . . . .
C34 C 0.6784(2) 1.12177(16) 0.06513(12) 0.0595(6) Uani 1 1 d D . . . .
H34A H 0.7564 1.0990 0.0700 0.071 Uiso 0.7274 1 calc R . P A 1
H34B H 0.6897 1.1814 0.0396 0.071 Uiso 0.7274 1 calc R . P A 1
H34C H 0.6552 1.1726 0.0291 0.071 Uiso 0.2726 1 calc R . P B 2
H34D H 0.7625 1.1276 0.0675 0.071 Uiso 0.2726 1 calc R . P B 2
C36 C 0.53126(19) 1.01880(13) 0.08250(11) 0.0479(5) Uani 1 1 d D . . . .
H36A H 0.4563 1.0141 0.0659 0.057 Uiso 0.7274 1 calc R . P C 1
H36B H 0.5677 0.9659 0.0948 0.057 Uiso 0.7274 1 calc R . P C 1
H36C H 0.4747 1.0434 0.0491 0.057 Uiso 0.2726 1 calc R . P D 2
H36D H 0.5238 0.9591 0.0977 0.057 Uiso 0.2726 1 calc R . P D 2
C37 C 0.57880(13) 0.52613(9) 0.23231(8) 0.0221(3) Uani 1 1 d . . . . .
C38 C 0.59616(13) 0.58416(9) 0.15715(9) 0.0255(3) Uani 1 1 d . . . . .
C39 C 0.69556(15) 0.64070(10) 0.12919(9) 0.0319(4) Uani 1 1 d . . . . .
H39 H 0.7051 0.6790 0.0800 0.038 Uiso 1 1 calc R . . . .
C40 C 0.77974(15) 0.64099(10) 0.17300(10) 0.0341(4) Uani 1 1 d . . . . .
H40 H 0.8465 0.6780 0.1532 0.041 Uiso 1 1 calc R . . . .
C41 C 0.76363(14) 0.58561(10) 0.24656(9) 0.0312(4) Uani 1 1 d . . . . .
H41 H 0.8204 0.5857 0.2762 0.037 Uiso 1 1 calc R . . . .
C42 C 0.66439(13) 0.52953(9) 0.27761(9) 0.0249(3) Uani 1 1 d . . . . .
C43 C 0.51021(15) 0.58829(10) 0.10349(9) 0.0321(4) Uani 1 1 d . . . . .
H43 H 0.4516 0.5411 0.1286 0.038 Uiso 1 1 calc R . . . .
C44 C 0.44138(17) 0.66701(12) 0.08635(11) 0.0433(4) Uani 1 1 d . . . . .
H44A H 0.3956 0.6680 0.1323 0.065 Uiso 1 1 calc GR . . . .
H44B H 0.3883 0.6681 0.0522 0.065 Uiso 1 1 calc GR . . . .
H44C H 0.4970 0.7145 0.0638 0.065 Uiso 1 1 calc GR . . . .
C45 C 0.57399(17) 0.58110(11) 0.03050(10) 0.0401(4) Uani 1 1 d . . . . .
H45A H 0.6271 0.6291 0.0024 0.060 Uiso 1 1 calc GR . . . .
H45B H 0.5157 0.5772 0.0010 0.060 Uiso 1 1 calc GR . . . .
H45C H 0.6192 0.5324 0.0422 0.060 Uiso 1 1 calc GR . . . .
C46 C 0.65050(14) 0.47588(10) 0.36098(9) 0.0293(3) Uani 1 1 d . . . . .
H46 H 0.5747 0.4428 0.3748 0.035 Uiso 1 1 calc R . . . .
C47 C 0.74991(18) 0.41572(12) 0.37800(11) 0.0454(4) Uani 1 1 d . . . . .
H47A H 0.7498 0.3807 0.3497 0.068 Uiso 1 1 calc GR . . . .
H47B H 0.7366 0.3824 0.4308 0.068 Uiso 1 1 calc GR . . . .
H47C H 0.8259 0.4462 0.3642 0.068 Uiso 1 1 calc GR . . . .
C48 C 0.64150(18) 0.52897(12) 0.40903(10) 0.0409(4) Uani 1 1 d . . . . .
H48A H 0.7151 0.5617 0.3975 0.061 Uiso 1 1 calc GR . . . .
H48B H 0.6272 0.4938 0.4614 0.061 Uiso 1 1 calc GR . . . .
H48C H 0.5766 0.5648 0.3984 0.061 Uiso 1 1 calc GR . . . .
C49 C 0.51391(12) 0.35147(9) 0.30929(8) 0.0213(3) Uani 1 1 d . . . . .
C50 C 0.60186(13) 0.32483(9) 0.26300(8) 0.0230(3) Uani 1 1 d . . . . .
C51 C 0.65562(14) 0.25016(9) 0.29362(9) 0.0287(3) Uani 1 1 d . . . . .
H51 H 0.7155 0.2346 0.2632 0.034 Uiso 1 1 calc R . . . .
C52 C 0.62152(15) 0.19912(10) 0.36807(10) 0.0327(4) Uani 1 1 d . . . . .
H52 H 0.6584 0.1497 0.3879 0.039 Uiso 1 1 calc R . . . .
C53 C 0.53206(14) 0.22210(10) 0.41296(9) 0.0302(3) Uani 1 1 d . . . . .
H53 H 0.5069 0.1866 0.4626 0.036 Uiso 1 1 calc R . . . .
C54 C 0.47852(13) 0.29731(9) 0.38566(8) 0.0238(3) Uani 1 1 d . . . . .
C55 C 0.63948(14) 0.37378(9) 0.17914(8) 0.0266(3) Uani 1 1 d . . . . .
H55 H 0.5898 0.4216 0.1657 0.032 Uiso 1 1 calc R . . . .
C56 C 0.77014(15) 0.40694(11) 0.15842(10) 0.0363(4) Uani 1 1 d . . . . .
H56A H 0.7832 0.4393 0.1875 0.055 Uiso 1 1 calc GR . . . .
H56B H 0.7878 0.4409 0.1058 0.055 Uiso 1 1 calc GR . . . .
H56C H 0.8216 0.3614 0.1689 0.055 Uiso 1 1 calc GR . . . .
C57 C 0.61529(17) 0.32272(11) 0.13306(10) 0.0376(4) Uani 1 1 d . . . . .
H57A H 0.6627 0.2751 0.1450 0.056 Uiso 1 1 calc GR . . . .
H57B H 0.6362 0.3559 0.0803 0.056 Uiso 1 1 calc GR . . . .
H57C H 0.5318 0.3051 0.1448 0.056 Uiso 1 1 calc GR . . . .
C58 C 0.38389(14) 0.31930(10) 0.43956(9) 0.0291(3) Uani 1 1 d . . . . .
H58 H 0.3785 0.3795 0.4187 0.035 Uiso 1 1 calc R . . . .
C59 C 0.26117(17) 0.28055(15) 0.44446(12) 0.0512(5) Uani 1 1 d . . . . .
H59A H 0.2383 0.3010 0.3956 0.077 Uiso 1 1 calc GR . . . .
H59B H 0.2032 0.2947 0.4792 0.077 Uiso 1 1 calc GR . . . .
H59C H 0.2647 0.2215 0.4616 0.077 Uiso 1 1 calc GR . . . .
C60 C 0.4139(2) 0.29628(14) 0.51818(11) 0.0505(5) Uani 1 1 d . . . . .
H60A H 0.4922 0.3197 0.5146 0.076 Uiso 1 1 calc GR . . . .
H60B H 0.4127 0.2371 0.5421 0.076 Uiso 1 1 calc GR . . . .
H60C H 0.3557 0.3175 0.5475 0.076 Uiso 1 1 calc GR . . . .
C61 C 0.0935(2) 0.48478(15) 0.38688(12) 0.0570(6) Uani 1 1 d . . . . .
H61A H 0.0952 0.4252 0.4022 0.068 Uiso 1 1 calc R . . . .
H61B H 0.0105 0.4992 0.3910 0.068 Uiso 1 1 calc R . . . .
C62 C 0.1550(2) 0.51290(15) 0.43639(12) 0.0550(5) Uani 1 1 d . . . . .
H62A H 0.1838 0.4662 0.4743 0.066 Uiso 1 1 calc R . . . .
H62B H 0.1009 0.5417 0.4615 0.066 Uiso 1 1 calc R . . . .
C63 C 0.25818(19) 0.57035(14) 0.38464(13) 0.0559(6) Uani 1 1 d . . . . .
H63A H 0.2676 0.6181 0.3980 0.067 Uiso 1 1 calc R . . . .
H63B H 0.3325 0.5422 0.3862 0.067 Uiso 1 1 calc R . . . .
C64 C 0.22326(18) 0.59527(12) 0.30852(12) 0.0490(5) Uani 1 1 d . . . . .
H64A H 0.1755 0.6434 0.2986 0.059 Uiso 1 1 calc R . . . .
H64B H 0.2938 0.6081 0.2695 0.059 Uiso 1 1 calc R . . . .
C65 C 0.03282(15) 0.34685(11) 0.28468(11) 0.0383(4) Uani 1 1 d . . . . .
H65A H -0.0067 0.3923 0.2523 0.046 Uiso 1 1 calc R . . . .
H65B H 0.0057 0.3411 0.3366 0.046 Uiso 1 1 calc R . . . .
C66 C 0.00529(17) 0.26792(12) 0.27419(13) 0.0487(5) Uani 1 1 d . . . . .
H66A H -0.0089 0.2789 0.2235 0.058 Uiso 1 1 calc R . . . .
H66B H -0.0641 0.2371 0.3101 0.058 Uiso 1 1 calc R . . . .
C67 C 0.11779(18) 0.22211(12) 0.28849(14) 0.0503(5) Uani 1 1 d . . . . .
H67A H 0.1274 0.1821 0.2643 0.060 Uiso 1 1 calc R . . . .
H67B H 0.1175 0.1940 0.3420 0.060 Uiso 1 1 calc R . . . .
C68 C 0.21549(16) 0.29137(11) 0.25320(12) 0.0414(4) Uani 1 1 d . . . . .
H68A H 0.2851 0.2771 0.2776 0.050 Uiso 1 1 calc R . . . .
H68B H 0.2397 0.3027 0.1999 0.050 Uiso 1 1 calc R . . . .
Li1 Li 0.4045(2) 0.97256(16) 0.23969(15) 0.0293(6) Uani 1 1 d . . . . .
Li2 Li 0.2370(2) 0.46863(17) 0.24601(16) 0.0307(6) Uani 1 1 d . . . . .
O6A O 0.2023(19) 0.5390(14) 0.1496(12) 0.036(3) Uani 0.3913 1 d D U P E 1
C69A C 0.0950(17) 0.5868(13) 0.1387(10) 0.052(4) Uani 0.3913 1 d D U P E 1
H69A H 0.1144 0.6449 0.1273 0.063 Uiso 0.3913 1 calc R . P E 1
H69B H 0.0339 0.5662 0.1836 0.063 Uiso 0.3913 1 calc R . P E 1
C70A C 0.0517(10) 0.5749(9) 0.0717(6) 0.067(3) Uani 0.3913 1 d D U P E 1
H70A H -0.0351 0.5697 0.0795 0.080 Uiso 0.3913 1 calc R . P E 1
H70B H 0.0804 0.6210 0.0250 0.080 Uiso 0.3913 1 calc R . P E 1
C71A C 0.1050(6) 0.4963(6) 0.0705(3) 0.0569(15) Uani 0.3913 1 d D U P E 1
H71A H 0.1145 0.4941 0.0206 0.068 Uiso 0.3913 1 calc R . P E 1
H71B H 0.0566 0.4481 0.1064 0.068 Uiso 0.3913 1 calc R . P E 1
C72A C 0.2242(16) 0.5032(15) 0.0929(14) 0.047(4) Uani 0.3913 1 d D U P E 1
H72A H 0.2560 0.4490 0.1130 0.056 Uiso 0.3913 1 calc R . P E 1
H72B H 0.2813 0.5382 0.0498 0.056 Uiso 0.3913 1 calc R . P E 1
C35A C 0.6140(3) 1.0852(2) 0.02161(17) 0.0429(7) Uani 0.7274 1 d D U P F 1
H35A H 0.6696 1.0621 -0.0082 0.051 Uiso 0.7274 1 calc R . P F 1
H35B H 0.5693 1.1264 -0.0114 0.051 Uiso 0.7274 1 calc R . P F 1
O6B O 0.181(2) 0.5385(14) 0.1559(11) 0.035(4) Uani 0.3227 1 d D U P E 2
C69B C 0.1169(10) 0.6147(6) 0.1446(6) 0.047(2) Uani 0.3227 1 d D U P E 2
H69C H 0.1683 0.6580 0.1463 0.056 Uiso 0.3227 1 calc R . P E 2
H69D H 0.0459 0.6050 0.1829 0.056 Uiso 0.3227 1 calc R . P E 2
C70B C 0.083(2) 0.6385(10) 0.0656(10) 0.055(4) Uani 0.3227 1 d D U P E 2
H70C H 0.0046 0.6619 0.0643 0.066 Uiso 0.3227 1 calc R . P E 2
H70D H 0.1416 0.6783 0.0274 0.066 Uiso 0.3227 1 calc R . P E 2
C71B C 0.0803(12) 0.5592(10) 0.0539(7) 0.063(3) Uani 0.3227 1 d D U P E 2
H71C H 0.0956 0.5683 0.0007 0.076 Uiso 0.3227 1 calc R . P E 2
H71D H 0.0038 0.5283 0.0770 0.076 Uiso 0.3227 1 calc R . P E 2
C72B C 0.1793(11) 0.5152(9) 0.0921(8) 0.052(3) Uani 0.3227 1 d D . P E 2
H72C H 0.1651 0.4558 0.1085 0.063 Uiso 0.3227 1 calc R . P E 2
H72D H 0.2555 0.5314 0.0579 0.063 Uiso 0.3227 1 calc R . P E 2
C35B C 0.6539(8) 1.0506(6) 0.0454(5) 0.053(2) Uani 0.2726 1 d D U P F 2
H35C H 0.6612 1.0674 -0.0087 0.063 Uiso 0.2726 1 calc R . P F 2
H35D H 0.7101 1.0083 0.0629 0.063 Uiso 0.2726 1 calc R . P F 2
O6C O 0.1831(19) 0.5272(13) 0.1426(12) 0.028(3) Uani 0.2913 1 d D U P E 3
C69C C 0.084(2) 0.5783(13) 0.1283(11) 0.043(3) Uani 0.2913 1 d D U P E 3
H69E H 0.0619 0.5967 0.1700 0.051 Uiso 0.2913 1 calc R . P E 3
H69F H 0.0168 0.5452 0.1272 0.051 Uiso 0.2913 1 calc R . P E 3
C70C C 0.107(2) 0.6517(9) 0.0576(12) 0.046(4) Uani 0.2913 1 d . U P E 3
H70E H 0.1190 0.6344 0.0155 0.069 Uiso 0.2913 1 calc GR . P E 3
H70F H 0.1767 0.6832 0.0565 0.069 Uiso 0.2913 1 calc GR . P E 3
H70G H 0.0388 0.6854 0.0548 0.069 Uiso 0.2913 1 calc GR . P E 3
C71C C 0.2234(18) 0.4918(16) 0.0881(14) 0.034(3) Uani 0.2913 1 d D U P E 3
H71E H 0.2886 0.4569 0.1041 0.041 Uiso 0.2913 1 calc R . P E 3
H71F H 0.2553 0.5361 0.0407 0.041 Uiso 0.2913 1 calc R . P E 3
C72C C 0.1282(7) 0.4406(6) 0.0744(4) 0.0512(18) Uani 0.2913 1 d . U P E 3
H72E H 0.1649 0.4138 0.0417 0.077 Uiso 0.2913 1 calc GR . P E 3
H72F H 0.0690 0.4762 0.0512 0.077 Uiso 0.2913 1 calc GR . P E 3
H72G H 0.0906 0.3997 0.1215 0.077 Uiso 0.2913 1 calc GR . P E 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C1 1.8474(15) . ?
P1 C13 1.8459(15) . ?
P1 Li1 2.482(3) . ?
P2 C37 1.8506(15) . ?
P2 C49 1.8467(15) . ?
P2 Li2 2.498(3) . ?
O1 C25 1.447(2) . ?
O1 C28 1.436(2) . ?
O1 Li1 1.934(3) . ?
O2 C29 1.425(2) . ?
O2 C32 1.442(2) . ?
O2 Li1 1.984(3) . ?
O3 C33 1.430(2) . ?
O3 C36 1.429(2) . ?
O3 Li1 1.960(3) . ?
O4 C61 1.423(2) . ?
O4 C64 1.455(2) . ?
O4 Li2 1.978(3) . ?
O5 C65 1.444(2) . ?
O5 C68 1.444(2) . ?
O5 Li2 1.934(3) . ?
C1 C2 1.423(2) . ?
C1 C6 1.423(2) . ?
C2 C3 1.397(2) . ?
C2 C7 1.519(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.379(2) . ?
C4 H4 0.9300 . ?
C4 C5 1.380(2) . ?
C5 H5 0.9300 . ?
C5 C6 1.393(2) . ?
C6 C10 1.523(2) . ?
C7 H7 0.9800 . ?
C7 C8 1.534(2) . ?
C7 C9 1.527(2) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10 0.9800 . ?
C10 C11 1.529(2) . ?
C10 C12 1.521(2) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.418(2) . ?
C13 C18 1.427(2) . ?
C14 C15 1.397(2) . ?
C14 C19 1.518(2) . ?
C15 H15 0.9300 . ?
C15 C16 1.377(3) . ?
C16 H16 0.9300 . ?
C16 C17 1.377(3) . ?
C17 H17 0.9300 . ?
C17 C18 1.392(2) . ?
C18 C22 1.520(2) . ?
C19 H19 0.9800 . ?
C19 C20 1.528(3) . ?
C19 C21 1.527(3) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22 0.9800 . ?
C22 C23 1.534(2) . ?
C22 C24 1.527(2) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.493(3) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C27 1.506(3) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.523(3) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.496(3) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.511(3) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.507(3) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.467(3) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 H34C 0.9700 . ?
C34 H34D 0.9700 . ?
C34 C35A 1.502(4) . ?
C34 C35B 1.466(9) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 H36C 0.9700 . ?
C36 H36D 0.9700 . ?
C36 C35A 1.502(3) . ?
C36 C35B 1.464(8) . ?
C37 C38 1.416(2) . ?
C37 C42 1.426(2) . ?
C38 C39 1.398(2) . ?
C38 C43 1.521(2) . ?
C39 H39 0.9300 . ?
C39 C40 1.378(2) . ?
C40 H40 0.9300 . ?
C40 C41 1.379(2) . ?
C41 H41 0.9300 . ?
C41 C42 1.393(2) . ?
C42 C46 1.522(2) . ?
C43 H43 0.9800 . ?
C43 C44 1.526(2) . ?
C43 C45 1.528(2) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46 0.9800 . ?
C46 C47 1.524(2) . ?
C46 C48 1.529(2) . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 C50 1.421(2) . ?
C49 C54 1.423(2) . ?
C50 C51 1.397(2) . ?
C50 C55 1.519(2) . ?
C51 H51 0.9300 . ?
C51 C52 1.378(2) . ?
C52 H52 0.9300 . ?
C52 C53 1.381(2) . ?
C53 H53 0.9300 . ?
C53 C54 1.395(2) . ?
C54 C58 1.520(2) . ?
C55 H55 0.9800 . ?
C55 C56 1.527(2) . ?
C55 C57 1.528(2) . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C57 H57A 0.9600 . ?
C57 H57B 0.9600 . ?
C57 H57C 0.9600 . ?
C58 H58 0.9800 . ?
C58 C59 1.523(2) . ?
C58 C60 1.522(2) . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C61 C62 1.490(3) . ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?
C62 C63 1.505(3) . ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
C63 C64 1.497(3) . ?
C64 H64A 0.9700 . ?
C64 H64B 0.9700 . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
C65 C66 1.504(3) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
C66 C67 1.508(3) . ?
C67 H67A 0.9700 . ?
C67 H67B 0.9700 . ?
C67 C68 1.520(3) . ?
C68 H68A 0.9700 . ?
C68 H68B 0.9700 . ?
Li2 O6A 1.922(18) . ?
Li2 O6B 1.930(15) . ?
Li2 O6C 2.079(19) . ?
O6A C69A 1.468(12) . ?
O6A C72A 1.441(12) . ?
C69A H69A 0.9700 . ?
C69A H69B 0.9700 . ?
C69A C70A 1.544(14) . ?
C70A H70A 0.9700 . ?
C70A H70B 0.9700 . ?
C70A C71A 1.498(13) . ?
C71A H71A 0.9700 . ?
C71A H71B 0.9700 . ?
C71A C72A 1.504(17) . ?
C72A H72A 0.9700 . ?
C72A H72B 0.9700 . ?
C35A H35A 0.9700 . ?
C35A H35B 0.9700 . ?
O6B C69B 1.467(13) . ?
O6B C72B 1.440(10) . ?
C69B H69C 0.9700 . ?
C69B H69D 0.9700 . ?
C69B C70B 1.548(17) . ?
C70B H70C 0.9700 . ?
C70B H70D 0.9700 . ?
C70B C71B 1.482(19) . ?
C71B H71C 0.9700 . ?
C71B H71D 0.9700 . ?
C71B C72B 1.495(15) . ?
C72B H72C 0.9700 . ?
C72B H72D 0.9700 . ?
C35B H35C 0.9700 . ?
C35B H35D 0.9700 . ?
O6C C69C 1.422(16) . ?
O6C C71C 1.422(14) . ?
C69C H69E 0.9700 . ?
C69C H69F 0.9700 . ?
C69C C70C 1.48(3) . ?
C70C H70E 0.9600 . ?
C70C H70F 0.9600 . ?
C70C H70G 0.9600 . ?
C71C H71E 0.9700 . ?
C71C H71F 0.9700 . ?
C71C C72C 1.52(2) . ?
C72C H72E 0.9600 . ?
C72C H72F 0.9600 . ?
C72C H72G 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
C1 P1 Li1 123.05(8) . . ?
C13 P1 C1 102.92(6) . . ?
C13 P1 Li1 132.16(8) . . ?
C37 P2 Li2 129.85(8) . . ?
C49 P2 C37 102.74(6) . . ?
C49 P2 Li2 124.14(8) . . ?
C25 O1 Li1 120.05(12) . . ?
C28 O1 C25 109.78(13) . . ?
C28 O1 Li1 129.37(13) . . ?
C29 O2 C32 106.58(13) . . ?
C29 O2 Li1 128.16(14) . . ?
C32 O2 Li1 114.08(12) . . ?
C33 O3 Li1 126.97(13) . . ?
C36 O3 C33 108.76(13) . . ?
C36 O3 Li1 121.01(13) . . ?
C61 O4 C64 106.56(14) . . ?
C61 O4 Li2 126.52(15) . . ?
C64 O4 Li2 112.85(13) . . ?
C65 O5 C68 109.72(12) . . ?
C65 O5 Li2 121.47(12) . . ?
C68 O5 Li2 128.35(13) . . ?
C2 C1 P1 121.85(11) . . ?
C2 C1 C6 117.81(13) . . ?
C6 C1 P1 120.34(11) . . ?
C1 C2 C7 122.43(13) . . ?
C3 C2 C1 119.77(14) . . ?
C3 C2 C7 117.80(14) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 C2 121.59(15) . . ?
C4 C3 H3 119.2 . . ?
C3 C4 H4 120.4 . . ?
C3 C4 C5 119.21(14) . . ?
C5 C4 H4 120.4 . . ?
C4 C5 H5 119.2 . . ?
C4 C5 C6 121.54(15) . . ?
C6 C5 H5 119.2 . . ?
C1 C6 C10 121.72(13) . . ?
C5 C6 C1 119.98(14) . . ?
C5 C6 C10 118.30(14) . . ?
C2 C7 H7 107.4 . . ?
C2 C7 C8 111.48(14) . . ?
C2 C7 C9 112.70(13) . . ?
C8 C7 H7 107.4 . . ?
C9 C7 H7 107.4 . . ?
C9 C7 C8 110.18(14) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 H10 107.3 . . ?
C6 C10 C11 113.54(14) . . ?
C11 C10 H10 107.3 . . ?
C12 C10 C6 111.29(13) . . ?
C12 C10 H10 107.3 . . ?
C12 C10 C11 109.94(16) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 P1 121.12(11) . . ?
C14 C13 C18 117.60(14) . . ?
C18 C13 P1 121.19(12) . . ?
C13 C14 C19 122.25(14) . . ?
C15 C14 C13 120.12(15) . . ?
C15 C14 C19 117.61(15) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 C14 121.40(17) . . ?
C16 C15 H15 119.3 . . ?
C15 C16 H16 120.4 . . ?
C17 C16 C15 119.29(16) . . ?
C17 C16 H16 120.4 . . ?
C16 C17 H17 119.2 . . ?
C16 C17 C18 121.61(16) . . ?
C18 C17 H17 119.2 . . ?
C13 C18 C22 122.89(14) . . ?
C17 C18 C13 119.88(15) . . ?
C17 C18 C22 117.20(14) . . ?
C14 C19 H19 107.5 . . ?
C14 C19 C20 113.19(15) . . ?
C14 C19 C21 110.09(15) . . ?
C20 C19 H19 107.5 . . ?
C21 C19 H19 107.5 . . ?
C21 C19 C20 110.77(15) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22 H22 107.2 . . ?
C18 C22 C23 111.76(14) . . ?
C18 C22 C24 112.17(15) . . ?
C23 C22 H22 107.2 . . ?
C24 C22 H22 107.2 . . ?
C24 C22 C23 110.96(15) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O1 C25 H25A 110.4 . . ?
O1 C25 H25B 110.4 . . ?
O1 C25 C26 106.61(15) . . ?
H25A C25 H25B 108.6 . . ?
C26 C25 H25A 110.4 . . ?
C26 C25 H25B 110.4 . . ?
C25 C26 H26A 111.2 . . ?
C25 C26 H26B 111.2 . . ?
C25 C26 C27 102.97(15) . . ?
H26A C26 H26B 109.1 . . ?
C27 C26 H26A 111.2 . . ?
C27 C26 H26B 111.2 . . ?
C26 C27 H27A 111.3 . . ?
C26 C27 H27B 111.3 . . ?
C26 C27 C28 102.52(16) . . ?
H27A C27 H27B 109.2 . . ?
C28 C27 H27A 111.3 . . ?
C28 C27 H27B 111.3 . . ?
O1 C28 C27 103.99(15) . . ?
O1 C28 H28A 111.0 . . ?
O1 C28 H28B 111.0 . . ?
C27 C28 H28A 111.0 . . ?
C27 C28 H28B 111.0 . . ?
H28A C28 H28B 109.0 . . ?
O2 C29 H29A 110.1 . . ?
O2 C29 H29B 110.1 . . ?
O2 C29 C30 107.91(15) . . ?
H29A C29 H29B 108.4 . . ?
C30 C29 H29A 110.1 . . ?
C30 C29 H29B 110.1 . . ?
C29 C30 H30A 110.7 . . ?
C29 C30 H30B 110.7 . . ?
C29 C30 C31 105.39(16) . . ?
H30A C30 H30B 108.8 . . ?
C31 C30 H30A 110.7 . . ?
C31 C30 H30B 110.7 . . ?
C30 C31 H31A 111.0 . . ?
C30 C31 H31B 111.0 . . ?
H31A C31 H31B 109.0 . . ?
C32 C31 C30 103.80(15) . . ?
C32 C31 H31A 111.0 . . ?
C32 C31 H31B 111.0 . . ?
O2 C32 C31 105.07(14) . . ?
O2 C32 H32A 110.7 . . ?
O2 C32 H32B 110.7 . . ?
C31 C32 H32A 110.7 . . ?
C31 C32 H32B 110.7 . . ?
H32A C32 H32B 108.8 . . ?
O3 C33 H33A 110.1 . . ?
O3 C33 H33B 110.1 . . ?
O3 C33 C34 108.07(15) . . ?
H33A C33 H33B 108.4 . . ?
C34 C33 H33A 110.1 . . ?
C34 C33 H33B 110.1 . . ?
C33 C34 H34A 110.4 . . ?
C33 C34 H34B 110.4 . . ?
C33 C34 H34C 111.2 . . ?
C33 C34 H34D 111.2 . . ?
C33 C34 C35A 106.84(18) . . ?
H34A C34 H34B 108.6 . . ?
H34C C34 H34D 109.1 . . ?
C35A C34 H34A 110.4 . . ?
C35A C34 H34B 110.4 . . ?
C35B C34 C33 102.7(4) . . ?
C35B C34 H34C 111.2 . . ?
C35B C34 H34D 111.2 . . ?
O3 C36 H36A 110.3 . . ?
O3 C36 H36B 110.3 . . ?
O3 C36 H36C 110.7 . . ?
O3 C36 H36D 110.7 . . ?
O3 C36 C35A 107.24(17) . . ?
O3 C36 C35B 105.0(3) . . ?
H36A C36 H36B 108.5 . . ?
H36C C36 H36D 108.8 . . ?
C35A C36 H36A 110.3 . . ?
C35A C36 H36B 110.3 . . ?
C35B C36 H36C 110.7 . . ?
C35B C36 H36D 110.7 . . ?
C38 C37 P2 121.65(11) . . ?
C38 C37 C42 117.43(13) . . ?
C42 C37 P2 120.84(11) . . ?
C37 C38 C43 122.70(13) . . ?
C39 C38 C37 120.27(14) . . ?
C39 C38 C43 117.03(14) . . ?
C38 C39 H39 119.3 . . ?
C40 C39 C38 121.44(15) . . ?
C40 C39 H39 119.3 . . ?
C39 C40 H40 120.4 . . ?
C39 C40 C41 119.11(14) . . ?
C41 C40 H40 120.4 . . ?
C40 C41 H41 119.2 . . ?
C40 C41 C42 121.58(15) . . ?
C42 C41 H41 119.2 . . ?
C37 C42 C46 122.71(13) . . ?
C41 C42 C37 120.09(14) . . ?
C41 C42 C46 117.16(13) . . ?
C38 C43 H43 107.6 . . ?
C38 C43 C44 111.32(14) . . ?
C38 C43 C45 112.14(14) . . ?
C44 C43 H43 107.6 . . ?
C44 C43 C45 110.45(14) . . ?
C45 C43 H43 107.6 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C42 C46 H46 107.3 . . ?
C42 C46 C47 112.30(14) . . ?
C42 C46 C48 111.11(13) . . ?
C47 C46 H46 107.3 . . ?
C47 C46 C48 111.34(14) . . ?
C48 C46 H46 107.3 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C50 C49 P2 121.76(11) . . ?
C50 C49 C54 117.60(13) . . ?
C54 C49 P2 120.64(11) . . ?
C49 C50 C55 122.54(13) . . ?
C51 C50 C49 120.29(14) . . ?
C51 C50 C55 117.16(13) . . ?
C50 C51 H51 119.4 . . ?
C52 C51 C50 121.18(14) . . ?
C52 C51 H51 119.4 . . ?
C51 C52 H52 120.4 . . ?
C51 C52 C53 119.28(14) . . ?
C53 C52 H52 120.4 . . ?
C52 C53 H53 119.2 . . ?
C52 C53 C54 121.63(15) . . ?
C54 C53 H53 119.2 . . ?
C49 C54 C58 121.80(13) . . ?
C53 C54 C49 119.88(14) . . ?
C53 C54 C58 118.32(13) . . ?
C50 C55 H55 107.3 . . ?
C50 C55 C56 112.60(13) . . ?
C50 C55 C57 111.14(13) . . ?
C56 C55 H55 107.3 . . ?
C56 C55 C57 110.80(13) . . ?
C57 C55 H55 107.3 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C55 C57 H57A 109.5 . . ?
C55 C57 H57B 109.5 . . ?
C55 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C54 C58 H58 107.3 . . ?
C54 C58 C59 111.01(13) . . ?
C54 C58 C60 113.74(14) . . ?
C59 C58 H58 107.3 . . ?
C60 C58 H58 107.3 . . ?
C60 C58 C59 109.92(15) . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C58 C60 H60A 109.5 . . ?
C58 C60 H60B 109.5 . . ?
C58 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
O4 C61 H61A 110.0 . . ?
O4 C61 H61B 110.0 . . ?
O4 C61 C62 108.66(16) . . ?
H61A C61 H61B 108.3 . . ?
C62 C61 H61A 110.0 . . ?
C62 C61 H61B 110.0 . . ?
C61 C62 H62A 110.7 . . ?
C61 C62 H62B 110.7 . . ?
C61 C62 C63 105.31(17) . . ?
H62A C62 H62B 108.8 . . ?
C63 C62 H62A 110.7 . . ?
C63 C62 H62B 110.7 . . ?
C62 C63 H63A 111.0 . . ?
C62 C63 H63B 111.0 . . ?
H63A C63 H63B 109.0 . . ?
C64 C63 C62 103.64(17) . . ?
C64 C63 H63A 111.0 . . ?
C64 C63 H63B 111.0 . . ?
O4 C64 C63 105.16(15) . . ?
O4 C64 H64A 110.7 . . ?
O4 C64 H64B 110.7 . . ?
C63 C64 H64A 110.7 . . ?
C63 C64 H64B 110.7 . . ?
H64A C64 H64B 108.8 . . ?
O5 C65 H65A 110.5 . . ?
O5 C65 H65B 110.5 . . ?
O5 C65 C66 106.24(14) . . ?
H65A C65 H65B 108.7 . . ?
C66 C65 H65A 110.5 . . ?
C66 C65 H65B 110.5 . . ?
C65 C66 H66A 111.2 . . ?
C65 C66 H66B 111.2 . . ?
C65 C66 C67 102.58(15) . . ?
H66A C66 H66B 109.2 . . ?
C67 C66 H66A 111.2 . . ?
C67 C66 H66B 111.2 . . ?
C66 C67 H67A 111.3 . . ?
C66 C67 H67B 111.3 . . ?
C66 C67 C68 102.47(16) . . ?
H67A C67 H67B 109.2 . . ?
C68 C67 H67A 111.3 . . ?
C68 C67 H67B 111.3 . . ?
O5 C68 C67 104.62(14) . . ?
O5 C68 H68A 110.8 . . ?
O5 C68 H68B 110.8 . . ?
C67 C68 H68A 110.8 . . ?
C67 C68 H68B 110.8 . . ?
H68A C68 H68B 108.9 . . ?
O1 Li1 P1 111.37(12) . . ?
O1 Li1 O2 113.27(14) . . ?
O1 Li1 O3 99.42(13) . . ?
O2 Li1 P1 107.63(12) . . ?
O3 Li1 P1 124.68(13) . . ?
O3 Li1 O2 100.09(12) . . ?
O4 Li2 P2 106.27(12) . . ?
O4 Li2 O6C 104.7(5) . . ?
O5 Li2 P2 110.09(12) . . ?
O5 Li2 O4 112.85(14) . . ?
O5 Li2 O6C 94.9(6) . . ?
O6A Li2 P2 122.0(7) . . ?
O6A Li2 O4 100.8(5) . . ?
O6A Li2 O5 104.7(7) . . ?
O6B Li2 P2 129.2(8) . . ?
O6B Li2 O4 95.5(4) . . ?
O6B Li2 O5 102.2(7) . . ?
O6C Li2 P2 127.7(6) . . ?
C69A O6A Li2 124.4(15) . . ?
C72A O6A Li2 114.0(14) . . ?
C72A O6A C69A 108.2(9) . . ?
O6A C69A H69A 110.7 . . ?
O6A C69A H69B 110.7 . . ?
O6A C69A C70A 105.0(9) . . ?
H69A C69A H69B 108.8 . . ?
C70A C69A H69A 110.7 . . ?
C70A C69A H69B 110.7 . . ?
C69A C70A H70A 111.0 . . ?
C69A C70A H70B 111.0 . . ?
H70A C70A H70B 109.0 . . ?
C71A C70A C69A 103.9(9) . . ?
C71A C70A H70A 111.0 . . ?
C71A C70A H70B 111.0 . . ?
C70A C71A H71A 111.5 . . ?
C70A C71A H71B 111.5 . . ?
C70A C71A C72A 101.4(9) . . ?
H71A C71A H71B 109.3 . . ?
C72A C71A H71A 111.5 . . ?
C72A C71A H71B 111.5 . . ?
O6A C72A C71A 106.0(12) . . ?
O6A C72A H72A 110.5 . . ?
O6A C72A H72B 110.5 . . ?
C71A C72A H72A 110.5 . . ?
C71A C72A H72B 110.5 . . ?
H72A C72A H72B 108.7 . . ?
C34 C35A C36 102.9(2) . . ?
C34 C35A H35A 111.2 . . ?
C34 C35A H35B 111.2 . . ?
C36 C35A H35A 111.2 . . ?
C36 C35A H35B 111.2 . . ?
H35A C35A H35B 109.1 . . ?
C69B O6B Li2 127.4(9) . . ?
C72B O6B Li2 123.2(10) . . ?
C72B O6B C69B 108.7(9) . . ?
O6B C69B H69C 110.8 . . ?
O6B C69B H69D 110.8 . . ?
O6B C69B C70B 104.7(9) . . ?
H69C C69B H69D 108.9 . . ?
C70B C69B H69C 110.8 . . ?
C70B C69B H69D 110.8 . . ?
C69B C70B H70C 111.0 . . ?
C69B C70B H70D 111.0 . . ?
H70C C70B H70D 109.0 . . ?
C71B C70B C69B 104.0(10) . . ?
C71B C70B H70C 111.0 . . ?
C71B C70B H70D 111.0 . . ?
C70B C71B H71C 111.2 . . ?
C70B C71B H71D 111.2 . . ?
C70B C71B C72B 102.8(11) . . ?
H71C C71B H71D 109.1 . . ?
C72B C71B H71C 111.2 . . ?
C72B C71B H71D 111.2 . . ?
O6B C72B C71B 106.7(9) . . ?
O6B C72B H72C 110.4 . . ?
O6B C72B H72D 110.4 . . ?
C71B C72B H72C 110.4 . . ?
C71B C72B H72D 110.4 . . ?
H72C C72B H72D 108.6 . . ?
C34 C35B H35C 110.4 . . ?
C34 C35B H35D 110.4 . . ?
C36 C35B C34 106.6(5) . . ?
C36 C35B H35C 110.4 . . ?
C36 C35B H35D 110.4 . . ?
H35C C35B H35D 108.6 . . ?
C69C O6C Li2 126.6(13) . . ?
C71C O6C Li2 114.7(14) . . ?
C71C O6C C69C 115.5(14) . . ?
O6C C69C H69E 108.5 . . ?
O6C C69C H69F 108.5 . . ?
O6C C69C C70C 114.9(19) . . ?
H69E C69C H69F 107.5 . . ?
C70C C69C H69E 108.5 . . ?
C70C C69C H69F 108.5 . . ?
C69C C70C H70E 109.5 . . ?
C69C C70C H70F 109.5 . . ?
C69C C70C H70G 109.5 . . ?
H70E C70C H70F 109.5 . . ?
H70E C70C H70G 109.5 . . ?
H70F C70C H70G 109.5 . . ?
O6C C71C H71E 108.5 . . ?
O6C C71C H71F 108.5 . . ?
O6C C71C C72C 115.0(15) . . ?
H71E C71C H71F 107.5 . . ?
C72C C71C H71E 108.5 . . ?
C72C C71C H71F 108.5 . . ?
C71C C72C H72E 109.5 . . ?
C71C C72C H72F 109.5 . . ?
C71C C72C H72G 109.5 . . ?
H72E C72C H72F 109.5 . . ?
H72E C72C H72G 109.5 . . ?
H72F C72C H72G 109.5 . . ?

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
P1 C1 C2 C3 -177.14(11) . . . . ?
P1 C1 C2 C7 3.2(2) . . . . ?
P1 C1 C6 C5 178.78(11) . . . . ?
P1 C1 C6 C10 -0.10(19) . . . . ?
P1 C13 C14 C15 -178.96(12) . . . . ?
P1 C13 C14 C19 -0.4(2) . . . . ?
P1 C13 C18 C17 -179.46(11) . . . . ?
P1 C13 C18 C22 2.4(2) . . . . ?
P2 C37 C38 C39 178.25(12) . . . . ?
P2 C37 C38 C43 -2.0(2) . . . . ?
P2 C37 C42 C41 -179.95(12) . . . . ?
P2 C37 C42 C46 -2.25(19) . . . . ?
P2 C49 C50 C51 176.79(11) . . . . ?
P2 C49 C50 C55 -4.70(19) . . . . ?
P2 C49 C54 C53 -178.89(11) . . . . ?
P2 C49 C54 C58 0.44(19) . . . . ?
O1 C25 C26 C27 -25.5(2) . . . . ?
O2 C29 C30 C31 -5.7(2) . . . . ?
O3 C33 C34 C35A 10.1(3) . . . . ?
O3 C33 C34 C35B -22.0(5) . . . . ?
O3 C36 C35A C34 25.0(3) . . . . ?
O3 C36 C35B C34 -26.8(7) . . . . ?
O4 C61 C62 C63 -1.3(3) . . . . ?
O5 C65 C66 C67 28.6(2) . . . . ?
C1 P1 C13 C14 -129.40(12) . . . . ?
C1 P1 C13 C18 53.96(13) . . . . ?
C1 C2 C3 C4 -2.7(2) . . . . ?
C1 C2 C7 C8 123.85(16) . . . . ?
C1 C2 C7 C9 -111.65(16) . . . . ?
C1 C6 C10 C11 135.96(17) . . . . ?
C1 C6 C10 C12 -99.36(18) . . . . ?
C2 C1 C6 C5 -2.2(2) . . . . ?
C2 C1 C6 C10 178.88(13) . . . . ?
C2 C3 C4 C5 -0.3(2) . . . . ?
C3 C2 C7 C8 -55.78(19) . . . . ?
C3 C2 C7 C9 68.73(19) . . . . ?
C3 C4 C5 C6 2.0(2) . . . . ?
C4 C5 C6 C1 -0.7(2) . . . . ?
C4 C5 C6 C10 178.22(15) . . . . ?
C5 C6 C10 C11 -42.9(2) . . . . ?
C5 C6 C10 C12 81.74(18) . . . . ?
C6 C1 C2 C3 3.9(2) . . . . ?
C6 C1 C2 C7 -175.72(13) . . . . ?
C7 C2 C3 C4 176.92(15) . . . . ?
C13 P1 C1 C2 56.70(13) . . . . ?
C13 P1 C1 C6 -124.36(12) . . . . ?
C13 C14 C15 C16 -0.5(3) . . . . ?
C13 C14 C19 C20 129.68(17) . . . . ?
C13 C14 C19 C21 -105.75(17) . . . . ?
C13 C18 C22 C23 118.78(16) . . . . ?
C13 C18 C22 C24 -115.87(17) . . . . ?
C14 C13 C18 C17 3.8(2) . . . . ?
C14 C13 C18 C22 -174.31(14) . . . . ?
C14 C15 C16 C17 1.6(3) . . . . ?
C15 C14 C19 C20 -51.7(2) . . . . ?
C15 C14 C19 C21 72.83(19) . . . . ?
C15 C16 C17 C18 0.1(3) . . . . ?
C16 C17 C18 C13 -2.8(2) . . . . ?
C16 C17 C18 C22 175.42(15) . . . . ?
C17 C18 C22 C23 -59.36(19) . . . . ?
C17 C18 C22 C24 65.98(19) . . . . ?
C18 C13 C14 C15 -2.2(2) . . . . ?
C18 C13 C14 C19 176.34(14) . . . . ?
C19 C14 C15 C16 -179.07(16) . . . . ?
C25 O1 C28 C27 19.4(2) . . . . ?
C25 C26 C27 C28 36.5(2) . . . . ?
C26 C27 C28 O1 -34.6(2) . . . . ?
C28 O1 C25 C26 3.7(2) . . . . ?
C29 O2 C32 C31 -34.37(18) . . . . ?
C29 C30 C31 C32 -14.7(2) . . . . ?
C30 C31 C32 O2 29.85(19) . . . . ?
C32 O2 C29 C30 25.0(2) . . . . ?
C33 O3 C36 C35A -19.8(3) . . . . ?
C33 O3 C36 C35B 12.7(5) . . . . ?
C33 C34 C35A C36 -21.1(3) . . . . ?
C33 C34 C35B C36 29.8(7) . . . . ?
C36 O3 C33 C34 6.0(3) . . . . ?
C37 P2 C49 C50 -54.60(12) . . . . ?
C37 P2 C49 C54 125.90(11) . . . . ?
C37 C38 C39 C40 0.9(2) . . . . ?
C37 C38 C43 C44 110.82(16) . . . . ?
C37 C38 C43 C45 -124.87(16) . . . . ?
C37 C42 C46 C47 116.28(16) . . . . ?
C37 C42 C46 C48 -118.27(16) . . . . ?
C38 C37 C42 C41 -3.1(2) . . . . ?
C38 C37 C42 C46 174.58(13) . . . . ?
C38 C39 C40 C41 -1.7(3) . . . . ?
C39 C38 C43 C44 -69.38(19) . . . . ?
C39 C38 C43 C45 54.93(19) . . . . ?
C39 C40 C41 C42 -0.1(3) . . . . ?
C40 C41 C42 C37 2.5(2) . . . . ?
C40 C41 C42 C46 -175.33(15) . . . . ?
C41 C42 C46 C47 -65.95(19) . . . . ?
C41 C42 C46 C48 59.49(19) . . . . ?
C42 C37 C38 C39 1.5(2) . . . . ?
C42 C37 C38 C43 -178.76(14) . . . . ?
C43 C38 C39 C40 -178.86(15) . . . . ?
C49 P2 C37 C38 127.07(12) . . . . ?
C49 P2 C37 C42 -56.24(13) . . . . ?
C49 C50 C51 C52 2.8(2) . . . . ?
C49 C50 C55 C56 114.90(15) . . . . ?
C49 C50 C55 C57 -120.11(15) . . . . ?
C49 C54 C58 C59 96.38(18) . . . . ?
C49 C54 C58 C60 -139.03(16) . . . . ?
C50 C49 C54 C53 1.6(2) . . . . ?
C50 C49 C54 C58 -179.09(13) . . . . ?
C50 C51 C52 C53 0.4(2) . . . . ?
C51 C50 C55 C56 -66.55(18) . . . . ?
C51 C50 C55 C57 58.45(18) . . . . ?
C51 C52 C53 C54 -2.6(2) . . . . ?
C52 C53 C54 C49 1.6(2) . . . . ?
C52 C53 C54 C58 -177.80(14) . . . . ?
C53 C54 C58 C59 -84.27(18) . . . . ?
C53 C54 C58 C60 40.3(2) . . . . ?
C54 C49 C50 C51 -3.7(2) . . . . ?
C54 C49 C50 C55 174.82(13) . . . . ?
C55 C50 C51 C52 -175.82(14) . . . . ?
C61 O4 C64 C63 31.7(2) . . . . ?
C61 C62 C63 C64 20.1(2) . . . . ?
C62 C63 C64 O4 -31.7(2) . . . . ?
C64 O4 C61 C62 -18.9(2) . . . . ?
C65 O5 C68 C67 -15.9(2) . . . . ?
C65 C66 C67 C68 -37.4(2) . . . . ?
C66 C67 C68 O5 33.1(2) . . . . ?
C68 O5 C65 C66 -8.0(2) . . . . ?
Li1 P1 C1 C2 -109.43(14) . . . . ?
Li1 P1 C1 C6 69.52(14) . . . . ?
Li1 P1 C13 C14 34.87(17) . . . . ?
Li1 P1 C13 C18 -141.77(13) . . . . ?
Li1 O1 C25 C26 -166.99(16) . . . . ?
Li1 O1 C28 C27 -170.97(16) . . . . ?
Li1 O2 C29 C30 -115.83(19) . . . . ?
Li1 O2 C32 C31 112.69(15) . . . . ?
Li1 O3 C33 C34 165.51(18) . . . . ?
Li1 O3 C36 C35A 179.2(2) . . . . ?
Li1 O3 C36 C35B -148.2(5) . . . . ?
Li2 P2 C37 C38 -32.68(17) . . . . ?
Li2 P2 C37 C42 144.01(12) . . . . ?
Li2 P2 C49 C50 106.68(13) . . . . ?
Li2 P2 C49 C54 -72.82(14) . . . . ?
Li2 O4 C61 C62 117.5(2) . . . . ?
Li2 O4 C64 C63 -111.30(16) . . . . ?
Li2 O5 C65 C66 164.88(15) . . . . ?
Li2 O5 C68 C67 171.89(16) . . . . ?
Li2 O6A C69A C70A -136.7(14) . . . . ?
Li2 O6A C72A C71A 117.9(16) . . . . ?
Li2 O6B C69B C70B -174.0(18) . . . . ?
Li2 O6B C72B C71B 152.2(16) . . . . ?
Li2 O6C C69C C70C 140.3(18) . . . . ?
Li2 O6C C71C C72C 104.8(18) . . . . ?
O6A C69A C70A C71A 22.4(19) . . . . ?
C69A O6A C72A C71A -25(3) . . . . ?
C69A C70A C71A C72A -36.4(15) . . . . ?
C70A C71A C72A O6A 38.4(19) . . . . ?
C72A O6A C69A C70A 1(3) . . . . ?
O6B C69B C70B C71B 24.2(19) . . . . ?
C69B O6B C72B C71B -19(2) . . . . ?
C69B C70B C71B C72B -35.1(16) . . . . ?
C70B C71B C72B O6B 34.2(19) . . . . ?
C72B O6B C69B C70B -3(2) . . . . ?
C69C O6C C71C C72C -56(3) . . . . ?
C71C O6C C69C C70C -61(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
