#------------------------------------------------------------------------------
#$Date: 2024-09-06 01:08:12 +0200 (Fri 06 de Sep de 2024) $
#$Revision: 294410 $
#$URL: svn://www.crystallography.net/cod/cif/7/13/34/7133443.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7133443
loop_
_publ_author_name
'Duari, Prakash'
'Mondal, Sunita'
'Jörges, Mike'
'Gessner, Viktoria H.'
_publ_section_title
;
 The lithium effect in ketenyl anion chemistry.
;
_journal_issue                   70
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9372
_journal_page_last               9375
_journal_paper_doi               10.1039/d4cc03167a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C36 H36 Li2 O6 P2'
_chemical_formula_sum            'C36 H36 Li2 O6 P2'
_chemical_formula_weight         640.47
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-14
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-07-31 deposited with the CCDC.	2024-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90.527(2)
_cell_angle_beta                 91.990(2)
_cell_angle_gamma                100.300(2)
_cell_formula_units_Z            4
_cell_length_a                   14.2502(3)
_cell_length_b                   15.4854(3)
_cell_length_c                   15.5126(3)
_cell_measurement_reflns_used    14366
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.9510
_cell_measurement_theta_min      6.3130
_cell_volume                     3365.56(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT (G.M. Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     90.00 168.00   0.50    1.00    --  105.91  62.00-125.00  156
  2  ω    111.00 173.00   0.50    1.00    --  105.91  30.00 -60.00  124
  3  ω     53.00 117.00   0.50    0.25    --   47.03  62.00-125.00  128
  4  ω     93.00 174.00   0.50    1.00    --  105.91  30.00 -30.00  162
  5  ω     96.00 178.00   0.50    1.00    --  105.91  15.00  30.00  164
  6  ω     75.00 105.00   0.50    1.00    --  105.91 -94.00  30.00   60
  7  ω     80.00 109.00   0.50    1.00    --  105.91-117.00  40.16   58
  8  ω     35.00  89.00   0.50    0.25    --   47.03-125.00 -30.00  108
  9  ω     36.00  70.00   0.50    1.00    --  105.91-125.00-150.00   68
 10  ω     85.00 112.00   0.50    1.00    --  105.91-125.00-150.00   54
 11  ω     79.00 106.00   0.50    1.00    --  105.91 -94.00-150.00   54
 12  ω     39.00  65.00   0.50    1.00    --  105.91 -94.00-150.00   52
 13  ω     69.00 106.00   0.50    1.00    --  105.91-125.00 -60.00   74
 14  ω     36.00  95.00   0.50    1.00    --  105.91 -94.00 -30.00  118
 15  ω     78.00 103.00   0.50    1.00    --  105.91 -94.00 -90.00   50
 16  ω     46.00  72.00   0.50    1.00    --  105.91-117.00  40.16   52
 17  ω     34.00  60.00   0.50    1.00    --  105.91 -94.00  60.00   52
 18  ω     69.00 106.00   0.50    1.00    --  105.91 -94.00  60.00   74
 19  ω     74.00 101.00   0.50    1.00    --  105.91 -94.00  90.00   54
 20  ω     73.00 104.00   0.50    1.00    --  105.91 -94.00 150.00   62
 21  ω     44.00  71.00   0.50    1.00    --  105.91 -94.00 150.00   54
 22  ω     35.00  68.00   0.50    1.00    --  105.91 -94.00  90.00   66
 23  ω     46.00  71.00   0.50    1.00    --  105.91 -94.00  30.00   50
 24  ω     40.00  92.00   0.50    1.00    --  105.91 -77.00 -30.00  104
 25  ω     40.00  73.00   0.50    1.00    --  105.91 -61.00-120.00   66
 26  ω     13.00  45.00   0.50    0.25    --   47.03 -62.00  96.00   64
 27  ω    -18.00  12.00   0.50    0.25    --   47.03 -62.00  96.00   60
 28  ω     34.00  75.00   0.50    1.00    --  105.91 -62.00  96.00   82
 29  ω     96.00 171.00   0.50    1.00    --  105.91 125.00 -30.00  150
 30  ω    110.00 136.00   0.50    1.00    --  105.91 125.00 -60.00   52
 31  ω    143.00 171.00   0.50    1.00    --  105.91 125.00 -60.00   56
 32  ω    -64.00  24.00   0.50    0.25    --  -47.03  62.00-125.00  176
 33  ω    -50.00 -24.00   0.50    1.00    --  -91.75  62.00-125.00   52
 34  ω    -68.00 -21.00   0.50    1.00    --  -91.75  61.00 -60.00   94
 35  ω    -48.00 -23.00   0.50    1.00    --  -91.75  45.00 -60.00   50
 36  ω    -46.00 -21.00   0.50    1.00    --  -91.75  45.00-120.00   50
 37  ω    -48.00 -23.00   0.50    1.00    --  -91.75  45.00 -30.00   50
 38  ω    -21.00   6.00   0.50    0.25    --  -47.03  19.00-180.00   54
 39  ω    -57.00 -31.00   0.50    1.00    --  -91.75  61.00  60.00   52
 40  ω    -48.00 -22.00   0.50    1.00    --  -91.75  45.00  90.00   52
 41  ω    -60.00 -25.00   0.50    1.00    --  -91.75  61.00 150.00   70
 42  ω    -61.00 -14.00   0.50    0.25    --  -47.03 125.00 150.00   94
 43  ω   -143.00-112.00   0.50    1.00    --  -91.75 -45.00-150.00   62
 44  ω   -118.00 -78.00   0.50    0.25    --  -47.03-125.00-180.00   80
 45  ω   -116.00 -81.00   0.50    0.25    --  -47.03-125.00-150.00   70
 46  ω   -114.00 -30.00   0.50    0.25    --  -47.03 -62.00  96.00  168
 47  ω   -163.00 -86.00   0.50    1.00    --  -91.75 -62.00  96.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0715940000
_diffrn_orient_matrix_UB_12      -0.0213103000
_diffrn_orient_matrix_UB_13      0.0698271000
_diffrn_orient_matrix_UB_21      0.0669280000
_diffrn_orient_matrix_UB_22      0.0872238000
_diffrn_orient_matrix_UB_23      -0.0176587000
_diffrn_orient_matrix_UB_31      -0.0498470000
_diffrn_orient_matrix_UB_32      0.0465237000
_diffrn_orient_matrix_UB_33      0.0684778000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22471
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.831
_diffrn_reflns_theta_min         2.851
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.528
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.136
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     830
_refine_ls_number_reflns         22471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0660
_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)+(0.0673P)²+7.1882P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1834
_refine_ls_wR_factor_ref         0.2099
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20188
_reflns_number_total             22471
_reflns_threshold_expression     'I > 2σ(I)'
_twin_special_details
;
Component 2 rotated by -179.9596° 
 around [-0.00 -0.00 1.00] (reciprocal) or [0.04 0.02 1.00] (direct)
;
_cod_data_source_file            d4cc03167a2.cif
_cod_data_source_block           SMO-225
_cod_depositor_comments
'Adding full bibliography for 7133440--7133443.cif.'
_cod_database_code               7133443
_shelx_shelxl_version_number     2019/3
_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.
;
_cell_oxdiff_length_a            14.2502(3)
_cell_oxdiff_length_b            15.4854(3)
_cell_oxdiff_length_c            15.5126(3)
_cell_oxdiff_angle_alpha         90.5275(15)
_cell_oxdiff_angle_beta          91.9898(16)
_cell_oxdiff_angle_gamma         100.2998(15)
_cell_oxdiff_volume              3365.57(11)
_cell_oxdiff_measurement_reflns_used 14366
_oxdiff_exptl_absorpt_empirical_full_min 0.584
_oxdiff_exptl_absorpt_empirical_full_max 1.737
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_twin_items               2
_chemical_oxdiff_formula         'C72 H72 Li4 O12 P4'
_chemical_oxdiff_usercomment     'tHF toluene /pen'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 0.65025(7) 0.14894(6) 0.53976(6) 0.0224(2) Uani 1 1 d . . . . .
O1 O 0.5662(2) 0.3518(2) 0.4099(2) 0.0330(7) Uani 1 1 d . . . . .
C1 C 0.6355(3) 0.2373(3) 0.4827(3) 0.0303(9) Uani 1 1 d . . . . .
C12 C 0.9521(3) 0.1032(4) 0.4865(3) 0.0420(12) Uani 1 1 d . . . . .
H12 H 1.013186 0.094549 0.474196 0.050 Uiso 1 1 calc R U . . .
C13 C 0.9397(3) 0.1789(3) 0.5287(3) 0.0374(10) Uani 1 1 d . . . . .
H13 H 0.992576 0.220935 0.545204 0.045 Uiso 1 1 calc R U . . .
C14 C 0.8487(3) 0.1926(3) 0.5465(3) 0.0316(9) Uani 1 1 d . . . . .
H14 H 0.840526 0.243747 0.574934 0.038 Uiso 1 1 calc R U . . .
C15 C 0.6481(3) 0.1767(3) 0.6528(3) 0.0241(8) Uani 1 1 d . . . . .
C16 C 0.5894(3) 0.2337(3) 0.6805(3) 0.0342(10) Uani 1 1 d . . . . .
H16 H 0.552642 0.258671 0.640397 0.041 Uiso 1 1 calc R U . . .
C17 C 0.5855(4) 0.2532(3) 0.7670(3) 0.0420(11) Uani 1 1 d . . . . .
H17 H 0.545311 0.290510 0.784869 0.050 Uiso 1 1 calc R U . . .
C18 C 0.6403(4) 0.2183(3) 0.8269(3) 0.0403(11) Uani 1 1 d . . . . .
H18 H 0.638418 0.233151 0.884979 0.048 Uiso 1 1 calc R U . . .
C29 C 0.9154(4) 0.6190(4) 0.5516(4) 0.0444(12) Uani 1 1 d . . . . .
H29 H 0.968479 0.659676 0.570506 0.053 Uiso 1 1 calc R U . . .
C30 C 0.9133(3) 0.5305(3) 0.5637(3) 0.0388(11) Uani 1 1 d . . . . .
H30 H 0.965409 0.511341 0.589889 0.047 Uiso 1 1 calc R U . . .
C31 C 0.8340(4) 0.4706(3) 0.5369(3) 0.0375(10) Uani 1 1 d . . . . .
H31 H 0.832114 0.411049 0.545904 0.045 Uiso 1 1 calc R U . . .
C32 C 0.7569(3) 0.4990(3) 0.4964(3) 0.0349(10) Uani 1 1 d . . . . .
H32 H 0.703835 0.458114 0.477917 0.042 Uiso 1 1 calc R U . . .
C33 C 0.8254(3) 0.8682(3) 0.8346(3) 0.0263(8) Uani 1 1 d . . . . .
C19 C 0.6982(4) 0.1612(3) 0.8012(3) 0.0390(11) Uani 1 1 d . . . . .
H19 H 0.734720 0.136741 0.841931 0.047 Uiso 1 1 calc R U . . .
C21 C 0.6663(3) 0.6159(3) 0.3183(3) 0.0264(8) Uani 1 1 d . . . . .
C22 C 0.6934(3) 0.6901(3) 0.2688(3) 0.0327(9) Uani 1 1 d . . . . .
H22 H 0.705322 0.745155 0.295632 0.039 Uiso 1 1 calc R U . . .
C23 C 0.7028(3) 0.6838(3) 0.1811(3) 0.0360(10) Uani 1 1 d . . . . .
H23 H 0.720811 0.734278 0.149291 0.043 Uiso 1 1 calc R U . . .
C24 C 0.6857(3) 0.6023(3) 0.1401(3) 0.0346(10) Uani 1 1 d . . . . .
H24 H 0.693748 0.597733 0.081072 0.042 Uiso 1 1 calc R U . . .
C20 C 0.7019(3) 0.1403(3) 0.7147(3) 0.0322(9) Uani 1 1 d . . . . .
H20 H 0.740770 0.101422 0.697629 0.039 Uiso 1 1 calc R U . . .
Li1 Li 0.4950(5) 0.4426(5) 0.4340(5) 0.0297(15) Uani 1 1 d . . . . .
P2 P 0.65446(8) 0.62288(7) 0.43322(7) 0.0247(2) Uani 1 1 d . . . . .
O2 O 0.6207(2) 0.8681(2) 0.5067(3) 0.0443(9) Uani 1 1 d . . . . .
C2 C 0.5986(3) 0.2942(3) 0.4471(3) 0.0248(8) Uani 1 1 d . . . . .
C25 C 0.6564(3) 0.5276(3) 0.1879(3) 0.0321(9) Uani 1 1 d . . . . .
H25 H 0.642613 0.472948 0.160472 0.038 Uiso 1 1 calc R U . . .
C26 C 0.6475(3) 0.5340(3) 0.2756(3) 0.0313(9) Uani 1 1 d . . . . .
H26 H 0.628846 0.483320 0.307052 0.038 Uiso 1 1 calc R U . . .
C27 C 0.7579(3) 0.5882(3) 0.4833(3) 0.0283(9) Uani 1 1 d . . . . .
C28 C 0.8383(3) 0.6472(3) 0.5111(3) 0.0391(11) Uani 1 1 d . . . . .
H28 H 0.840549 0.706917 0.502576 0.047 Uiso 1 1 calc R U . . .
C34 C 0.8834(3) 0.8210(3) 0.7911(3) 0.0381(10) Uani 1 1 d . . . . .
H34 H 0.924009 0.791068 0.822224 0.046 Uiso 1 1 calc R U . . .
C35 C 0.8817(4) 0.8178(4) 0.7021(3) 0.0438(12) Uani 1 1 d . . . . .
H35 H 0.921963 0.786774 0.673923 0.053 Uiso 1 1 calc R U . . .
C36 C 0.8202(3) 0.8607(4) 0.6544(3) 0.0404(11) Uani 1 1 d . . . . .
H36 H 0.818175 0.857475 0.594471 0.049 Uiso 1 1 calc R U . . .
C37 C 0.7629(4) 0.9075(3) 0.6964(3) 0.0403(11) Uani 1 1 d . . . . .
H37 H 0.721953 0.936767 0.664847 0.048 Uiso 1 1 calc R U . . .
C38 C 0.7649(3) 0.9118(3) 0.7870(3) 0.0353(10) Uani 1 1 d . . . . .
H38 H 0.725631 0.944096 0.814993 0.042 Uiso 1 1 calc R U . . .
C39 C 0.7306(3) 0.9105(3) 0.9890(3) 0.0273(8) Uani 1 1 d . . . . .
C40 C 0.6522(3) 0.8527(3) 1.0189(3) 0.0372(10) Uani 1 1 d . . . . .
H40 H 0.650183 0.792514 1.014009 0.045 Uiso 1 1 calc R U . . .
C41 C 0.5777(3) 0.8840(4) 1.0556(3) 0.0424(11) Uani 1 1 d . . . . .
H41 H 0.525619 0.844936 1.074836 0.051 Uiso 1 1 calc R U . . .
C42 C 0.5805(4) 0.9732(4) 1.0637(3) 0.0419(12) Uani 1 1 d . . . . .
H42 H 0.530714 0.993923 1.089447 0.050 Uiso 1 1 calc R U . . .
C43 C 0.6566(3) 1.0320(3) 1.0339(3) 0.0386(11) Uani 1 1 d . . . . .
H43 H 0.657678 1.092084 1.038634 0.046 Uiso 1 1 calc R U . . .
C44 C 0.7318(3) 1.0005(3) 0.9967(3) 0.0341(10) Uani 1 1 d . . . . .
H44 H 0.783319 1.039940 0.976799 0.041 Uiso 1 1 calc R U . . .
C45 C 0.7345(3) 1.3608(3) 1.0268(3) 0.0261(8) Uani 1 1 d . . . . .
C46 C 0.6616(3) 1.3013(3) 1.0645(3) 0.0288(9) Uani 1 1 d . . . . .
H46 H 0.676795 1.257519 1.100198 0.035 Uiso 1 1 calc R U . . .
C47 C 0.5672(3) 1.3082(3) 1.0484(3) 0.0372(10) Uani 1 1 d . . . . .
H47 H 0.519113 1.268964 1.073459 0.045 Uiso 1 1 calc R U . . .
C55 C 0.8601(4) 1.2486(3) 1.2924(3) 0.0408(11) Uani 1 1 d . . . . .
H55 H 0.866030 1.195653 1.318006 0.049 Uiso 1 1 calc R U . . .
C56 C 0.8689(3) 1.2574(3) 1.2035(3) 0.0360(10) Uani 1 1 d . . . . .
H56 H 0.880105 1.210211 1.170339 0.043 Uiso 1 1 calc R U . . .
C48 C 0.5435(3) 1.3732(3) 0.9951(3) 0.0366(10) Uani 1 1 d . . . . .
H48 H 0.479816 1.376878 0.983825 0.044 Uiso 1 1 calc R U . . .
C54 C 0.8429(3) 1.3165(3) 1.3422(3) 0.0383(11) Uani 1 1 d . . . . .
H54 H 0.835745 1.309561 1.401205 0.046 Uiso 1 1 calc R U . . .
C49 C 0.6152(3) 1.4323(3) 0.9589(3) 0.0343(10) Uani 1 1 d . . . . .
H49 H 0.599525 1.476251 0.923629 0.041 Uiso 1 1 calc R U . . .
C53 C 0.8361(4) 1.3966(4) 1.3043(3) 0.0402(11) Uani 1 1 d . . . . .
H53 H 0.825856 1.443578 1.338312 0.048 Uiso 1 1 calc R U . . .
C50 C 0.7103(3) 1.4266(3) 0.9750(3) 0.0297(9) Uani 1 1 d . . . . .
H50 H 0.758087 1.467078 0.950906 0.036 Uiso 1 1 calc R U . . .
C51 C 0.8611(3) 1.3367(3) 1.1638(3) 0.0255(8) Uani 1 1 d . . . . .
C52 C 0.8444(3) 1.4064(3) 1.2165(3) 0.0338(10) Uani 1 1 d . . . . .
H52 H 0.838948 1.459834 1.191807 0.041 Uiso 1 1 calc R U . . .
C57 C 0.3755(6) 0.3536(4) 0.2873(4) 0.069(2) Uani 1 1 d . . . . .
H57A H 0.338033 0.311494 0.324182 0.083 Uiso 1 1 calc R U . . .
H57B H 0.428012 0.328141 0.266254 0.083 Uiso 1 1 calc R U . . .
C58 C 0.3147(6) 0.3770(5) 0.2133(4) 0.075(2) Uani 1 1 d . . . . .
H58A H 0.260648 0.330501 0.200409 0.090 Uiso 1 1 calc R U . . .
H58B H 0.351319 0.389507 0.161928 0.090 Uiso 1 1 calc R U . . .
C59 C 0.2829(4) 0.4587(6) 0.2479(4) 0.076(2) Uani 1 1 d . . . . .
H59A H 0.265735 0.495048 0.201491 0.091 Uiso 1 1 calc R U . . .
H59B H 0.229186 0.443737 0.285070 0.091 Uiso 1 1 calc R U . . .
C60 C 0.3708(4) 0.5036(4) 0.2981(4) 0.0518(14) Uani 1 1 d . . . . .
H60A H 0.415105 0.538379 0.260286 0.062 Uiso 1 1 calc R U . . .
H60B H 0.354220 0.541633 0.342924 0.062 Uiso 1 1 calc R U . . .
C61 C 0.5107(4) 0.8559(3) 0.7136(3) 0.0398(11) Uani 1 1 d . . . . .
H61A H 0.561783 0.856329 0.756647 0.048 Uiso 1 1 calc R U . . .
H61B H 0.511157 0.807641 0.673390 0.048 Uiso 1 1 calc R U . . .
C62 C 0.4152(4) 0.8456(4) 0.7563(3) 0.0445(12) Uani 1 1 d . . . . .
H62A H 0.423892 0.849908 0.818586 0.053 Uiso 1 1 calc R U . . .
H62B H 0.375687 0.789550 0.740837 0.053 Uiso 1 1 calc R U . . .
C63 C 0.3700(4) 0.9220(4) 0.7212(3) 0.0450(12) Uani 1 1 d . . . . .
H63A H 0.329671 0.904121 0.670166 0.054 Uiso 1 1 calc R U . . .
H63B H 0.332731 0.944574 0.764387 0.054 Uiso 1 1 calc R U . . .
C64 C 0.4562(4) 0.9891(3) 0.6998(3) 0.0370(10) Uani 1 1 d . . . . .
H64A H 0.439845 1.028658 0.655859 0.044 Uiso 1 1 calc R U . . .
H64B H 0.482037 1.023257 0.750670 0.044 Uiso 1 1 calc R U . . .
C65 C 1.0629(4) 0.5554(4) 1.1958(3) 0.0417(11) Uani 1 1 d . . . . .
H65A H 1.099215 0.530031 1.153642 0.050 Uiso 1 1 calc R U . . .
H65B H 1.041924 0.511617 1.238678 0.050 Uiso 1 1 calc R U . . .
C66 C 1.1207(4) 0.6338(4) 1.2364(5) 0.0636(18) Uani 1 1 d . . . . .
H66A H 1.159992 0.668659 1.195059 0.076 Uiso 1 1 calc R U . . .
H66B H 1.160984 0.618758 1.283580 0.076 Uiso 1 1 calc R U . . .
C67 C 1.0446(6) 0.6806(4) 1.2684(5) 0.072(2) Uani 1 1 d . . . . .
H67A H 1.067829 0.743383 1.272767 0.087 Uiso 1 1 calc R U . . .
H67B H 1.024188 0.659388 1.324604 0.087 Uiso 1 1 calc R U . . .
C68 C 0.9629(4) 0.6597(3) 1.2012(3) 0.0408(11) Uani 1 1 d . . . . .
H68A H 0.901949 0.646085 1.228574 0.049 Uiso 1 1 calc R U . . .
H68B H 0.961938 0.708751 1.162923 0.049 Uiso 1 1 calc R U . . .
C69 C 1.1168(4) 0.9953(3) 0.7976(3) 0.0391(11) Uani 1 1 d . . . . .
H69A H 1.105716 0.944931 0.758486 0.047 Uiso 1 1 calc R U . . .
H69B H 1.146419 0.979153 0.850841 0.047 Uiso 1 1 calc R U . . .
C70 C 1.1802(4) 1.0737(3) 0.7566(4) 0.0435(12) Uani 1 1 d . . . . .
H70A H 1.215738 1.054559 0.710018 0.052 Uiso 1 1 calc R U . . .
H70B H 1.224656 1.106240 0.799071 0.052 Uiso 1 1 calc R U . . .
C71 C 1.1080(4) 1.1295(3) 0.7224(4) 0.0407(11) Uani 1 1 d . . . . .
H71A H 1.116413 1.185469 0.752890 0.049 Uiso 1 1 calc R U . . .
H71B H 1.114922 1.140062 0.661162 0.049 Uiso 1 1 calc R U . . .
C72 C 1.0117(3) 1.0742(3) 0.7395(3) 0.0369(10) Uani 1 1 d . . . . .
H72A H 0.965063 1.110964 0.751258 0.044 Uiso 1 1 calc R U . . .
H72B H 0.988587 1.035803 0.690628 0.044 Uiso 1 1 calc R U . . .
P3 P 0.83391(8) 0.87236(7) 0.95045(7) 0.0256(2) Uani 1 1 d . . . . .
O3 O 0.8667(2) 0.6218(2) 0.9828(2) 0.0371(7) Uani 1 1 d . . . . .
C3 C 0.6598(3) 0.7285(3) 0.4604(3) 0.0352(10) Uani 1 1 d . . . . .
Li3 Li 0.9561(5) 0.5593(5) 1.0335(5) 0.0290(15) Uani 1 1 d . . . . .
P4 P 0.85761(7) 1.34990(7) 1.04879(7) 0.0240(2) Uani 1 1 d . . . . .
O4 O 0.9211(2) 1.14273(19) 0.91021(19) 0.0315(7) Uani 1 1 d . . . . .
C4 C 0.6376(3) 0.7980(3) 0.4839(3) 0.0283(9) Uani 1 1 d . . . . .
Li4 Li 0.9882(5) 1.0462(5) 0.9293(5) 0.0310(15) Uani 1 1 d . . . . .
O5 O 0.5808(2) 0.06538(18) 0.51759(18) 0.0254(6) Uani 1 1 d . . . . .
C5 C 0.8311(3) 0.7705(3) 0.9873(3) 0.0377(10) Uani 1 1 d . . . . .
O6 O 0.5669(2) 0.55856(19) 0.45691(18) 0.0269(6) Uani 1 1 d . . . . .
C6 C 0.8517(3) 0.6965(3) 0.9828(3) 0.0295(9) Uani 1 1 d . . . . .
O7 O 0.9200(2) 0.94057(19) 0.97778(19) 0.0293(6) Uani 1 1 d . . . . .
C7 C 0.8760(3) 1.2564(3) 1.0025(3) 0.0336(10) Uani 1 1 d . . . . .
O8 O 0.9219(2) 1.43315(18) 1.02282(19) 0.0264(6) Uani 1 1 d . . . . .
C8 C 0.9001(3) 1.2006(3) 0.9556(3) 0.0255(8) Uani 1 1 d . . . . .
O9 O 0.4111(2) 0.4344(2) 0.3342(2) 0.0400(8) Uani 1 1 d . . . . .
C9 C 0.7698(3) 0.1297(3) 0.5219(3) 0.0259(8) Uani 1 1 d . . . . .
O10 O 0.5237(2) 0.9382(2) 0.6684(2) 0.0331(7) Uani 1 1 d . . . . .
C10 C 0.7829(3) 0.0531(3) 0.4810(3) 0.0302(9) Uani 1 1 d . . . . .
H10 H 0.730417 0.010073 0.465932 0.036 Uiso 1 1 calc R U . . .
O11 O 0.9825(2) 0.5845(2) 1.15465(19) 0.0326(7) Uani 1 1 d . . . . .
C11 C 0.8739(3) 0.0401(4) 0.4625(3) 0.0383(11) Uani 1 1 d . . . . .
H11 H 0.882325 -0.010873 0.433989 0.046 Uiso 1 1 calc R U . . .
O12 O 1.0296(2) 1.0243(2) 0.8138(2) 0.0380(7) Uani 1 1 d . . . . .
Li2 Li 0.5409(5) 0.9434(4) 0.5450(5) 0.0263(14) Uani 1 1 d . . . . .
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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 -2 0.0738
-8 4 -4 0.1272
3 2 9 0.0540
8 -2 5 0.0522
-7 -2 -6 0.0845
-6 0 8 0.0671
6 4 6 0.0606
6 0 -8 0.0750
0 -9 4 0.1137
-2 10 -1 0.1498
-1 0 2 0.0644
-3 -8 5 0.1078
6 2 6 0.0496
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
O5 P1 C1 115.9(2) . . ?
O5 P1 C15 111.03(18) . . ?
C1 P1 C15 108.1(2) . . ?
O5 P1 C9 108.23(18) . . ?
C1 P1 C9 107.2(2) . . ?
C15 P1 C9 105.93(19) . . ?
O5 P1 Li2 30.48(16) . 2_666 ?
C1 P1 Li2 86.6(2) . 2_666 ?
C15 P1 Li2 116.04(19) . 2_666 ?
C9 P1 Li2 128.98(19) . 2_666 ?
C2 O1 Li1 139.5(4) . . ?
C2 C1 P1 161.9(4) . . ?
C13 C12 C11 120.1(4) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C14 120.3(5) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C13 C14 C9 119.8(5) . . ?
C13 C14 H14 120.1 . . ?
C9 C14 H14 120.1 . . ?
C20 C15 C16 118.3(4) . . ?
C20 C15 P1 121.5(3) . . ?
C16 C15 P1 120.1(3) . . ?
C17 C16 C15 120.3(5) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C18 C17 C16 120.7(5) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 C19 120.0(4) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C30 C29 C28 119.8(5) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C31 C30 C29 119.9(4) . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
C30 C31 C32 120.1(5) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C31 C32 C27 120.8(4) . . ?
C31 C32 H32 119.6 . . ?
C27 C32 H32 119.6 . . ?
C34 C33 C38 118.6(4) . . ?
C34 C33 P3 118.6(3) . . ?
C38 C33 P3 122.8(3) . . ?
C18 C19 C20 119.8(5) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
C22 C21 C26 117.8(4) . . ?
C22 C21 P2 122.0(3) . . ?
C26 C21 P2 120.3(3) . . ?
C23 C22 C21 121.4(4) . . ?
C23 C22 H22 119.3 . . ?
C21 C22 H22 119.3 . . ?
C22 C23 C24 120.2(4) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C23 C24 C25 119.3(4) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
C19 C20 C15 120.8(4) . . ?
C19 C20 H20 119.6 . . ?
C15 C20 H20 119.6 . . ?
O9 Li1 O1 101.3(4) . . ?
O9 Li1 O6 114.0(4) . . ?
O1 Li1 O6 117.0(4) . . ?
O9 Li1 O6 115.0(4) . 2_666 ?
O1 Li1 O6 118.5(4) . 2_666 ?
O6 Li1 O6 91.9(3) . 2_666 ?
O6 P2 C3 117.7(2) . . ?
O6 P2 C21 108.14(18) . . ?
C3 P2 C21 108.1(2) . . ?
O6 P2 C27 108.19(18) . . ?
C3 P2 C27 107.2(2) . . ?
C21 P2 C27 107.02(19) . . ?
O6 P2 Li1 31.12(18) . 2_666 ?
C3 P2 Li1 93.5(2) . 2_666 ?
C21 P2 Li1 137.9(2) . 2_666 ?
C27 P2 Li1 100.03(19) . 2_666 ?
C4 O2 Li2 154.0(4) . . ?
O1 C2 C1 176.7(5) . . ?
C26 C25 C24 120.4(4) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C21 120.9(4) . . ?
C25 C26 H26 119.6 . . ?
C21 C26 H26 119.6 . . ?
C28 C27 C32 118.1(4) . . ?
C28 C27 P2 122.4(3) . . ?
C32 C27 P2 119.4(3) . . ?
C27 C28 C29 121.2(5) . . ?
C27 C28 H28 119.4 . . ?
C29 C28 H28 119.4 . . ?
C35 C34 C33 120.9(5) . . ?
C35 C34 H34 119.5 . . ?
C33 C34 H34 119.5 . . ?
C34 C35 C36 120.4(5) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
C37 C36 C35 119.2(5) . . ?
C37 C36 H36 120.4 . . ?
C35 C36 H36 120.4 . . ?
C36 C37 C38 120.7(5) . . ?
C36 C37 H37 119.7 . . ?
C38 C37 H37 119.7 . . ?
C33 C38 C37 120.1(4) . . ?
C33 C38 H38 119.9 . . ?
C37 C38 H38 119.9 . . ?
C44 C39 C40 118.6(4) . . ?
C44 C39 P3 119.4(3) . . ?
C40 C39 P3 121.8(3) . . ?
C41 C40 C39 120.7(5) . . ?
C41 C40 H40 119.6 . . ?
C39 C40 H40 119.6 . . ?
C42 C41 C40 120.0(5) . . ?
C42 C41 H41 120.0 . . ?
C40 C41 H41 120.0 . . ?
C41 C42 C43 120.6(5) . . ?
C41 C42 H42 119.7 . . ?
C43 C42 H42 119.7 . . ?
C42 C43 C44 119.4(5) . . ?
C42 C43 H43 120.3 . . ?
C44 C43 H43 120.3 . . ?
C43 C44 C39 120.6(4) . . ?
C43 C44 H44 119.7 . . ?
C39 C44 H44 119.7 . . ?
C50 C45 C46 119.2(4) . . ?
C50 C45 P4 122.0(3) . . ?
C46 C45 P4 118.9(3) . . ?
C47 C46 C45 119.8(4) . . ?
C47 C46 H46 120.1 . . ?
C45 C46 H46 120.1 . . ?
C46 C47 C48 120.7(4) . . ?
C46 C47 H47 119.7 . . ?
C48 C47 H47 119.7 . . ?
C54 C55 C56 120.8(5) . . ?
C54 C55 H55 119.6 . . ?
C56 C55 H55 119.6 . . ?
C55 C56 C51 120.6(5) . . ?
C55 C56 H56 119.7 . . ?
C51 C56 H56 119.7 . . ?
C49 C48 C47 119.5(4) . . ?
C49 C48 H48 120.2 . . ?
C47 C48 H48 120.2 . . ?
C55 C54 C53 119.7(4) . . ?
C55 C54 H54 120.1 . . ?
C53 C54 H54 120.1 . . ?
C48 C49 C50 120.5(5) . . ?
C48 C49 H49 119.8 . . ?
C50 C49 H49 119.8 . . ?
C52 C53 C54 120.2(5) . . ?
C52 C53 H53 119.9 . . ?
C54 C53 H53 119.9 . . ?
C45 C50 C49 120.3(4) . . ?
C45 C50 H50 119.8 . . ?
C49 C50 H50 119.8 . . ?
C56 C51 C52 117.7(4) . . ?
C56 C51 P4 123.4(3) . . ?
C52 C51 P4 118.5(3) . . ?
C53 C52 C51 121.0(4) . . ?
C53 C52 H52 119.5 . . ?
C51 C52 H52 119.5 . . ?
O9 C57 C58 106.2(5) . . ?
O9 C57 H57A 110.5 . . ?
C58 C57 H57A 110.5 . . ?
O9 C57 H57B 110.5 . . ?
C58 C57 H57B 110.5 . . ?
H57A C57 H57B 108.7 . . ?
C57 C58 C59 101.9(5) . . ?
C57 C58 H58A 111.4 . . ?
C59 C58 H58A 111.4 . . ?
C57 C58 H58B 111.4 . . ?
C59 C58 H58B 111.4 . . ?
H58A C58 H58B 109.2 . . ?
C60 C59 C58 102.1(5) . . ?
C60 C59 H59A 111.4 . . ?
C58 C59 H59A 111.3 . . ?
C60 C59 H59B 111.4 . . ?
C58 C59 H59B 111.4 . . ?
H59A C59 H59B 109.2 . . ?
O9 C60 C59 104.7(5) . . ?
O9 C60 H60A 110.8 . . ?
C59 C60 H60A 110.8 . . ?
O9 C60 H60B 110.8 . . ?
C59 C60 H60B 110.8 . . ?
H60A C60 H60B 108.9 . . ?
O10 C61 C62 107.2(4) . . ?
O10 C61 H61A 110.3 . . ?
C62 C61 H61A 110.3 . . ?
O10 C61 H61B 110.3 . . ?
C62 C61 H61B 110.3 . . ?
H61A C61 H61B 108.5 . . ?
C61 C62 C63 104.3(4) . . ?
C61 C62 H62A 110.9 . . ?
C63 C62 H62A 110.9 . . ?
C61 C62 H62B 110.9 . . ?
C63 C62 H62B 110.9 . . ?
H62A C62 H62B 108.9 . . ?
C64 C63 C62 102.5(4) . . ?
C64 C63 H63A 111.3 . . ?
C62 C63 H63A 111.3 . . ?
C64 C63 H63B 111.3 . . ?
C62 C63 H63B 111.3 . . ?
H63A C63 H63B 109.2 . . ?
O10 C64 C63 104.7(4) . . ?
O10 C64 H64A 110.8 . . ?
C63 C64 H64A 110.8 . . ?
O10 C64 H64B 110.8 . . ?
C63 C64 H64B 110.8 . . ?
H64A C64 H64B 108.9 . . ?
O11 C65 C66 105.7(4) . . ?
O11 C65 H65A 110.6 . . ?
C66 C65 H65A 110.6 . . ?
O11 C65 H65B 110.6 . . ?
C66 C65 H65B 110.6 . . ?
H65A C65 H65B 108.7 . . ?
C65 C66 C67 101.3(5) . . ?
C65 C66 H66A 111.5 . . ?
C67 C66 H66A 111.5 . . ?
C65 C66 H66B 111.5 . . ?
C67 C66 H66B 111.5 . . ?
H66A C66 H66B 109.3 . . ?
C66 C67 C68 104.8(5) . . ?
C66 C67 H67A 110.8 . . ?
C68 C67 H67A 110.8 . . ?
C66 C67 H67B 110.8 . . ?
C68 C67 H67B 110.8 . . ?
H67A C67 H67B 108.9 . . ?
O11 C68 C67 104.4(4) . . ?
O11 C68 H68A 110.9 . . ?
C67 C68 H68A 110.9 . . ?
O11 C68 H68B 110.9 . . ?
C67 C68 H68B 110.9 . . ?
H68A C68 H68B 108.9 . . ?
O12 C69 C70 105.3(4) . . ?
O12 C69 H69A 110.7 . . ?
C70 C69 H69A 110.7 . . ?
O12 C69 H69B 110.7 . . ?
C70 C69 H69B 110.7 . . ?
H69A C69 H69B 108.8 . . ?
C69 C70 C71 103.4(4) . . ?
C69 C70 H70A 111.1 . . ?
C71 C70 H70A 111.1 . . ?
C69 C70 H70B 111.1 . . ?
C71 C70 H70B 111.1 . . ?
H70A C70 H70B 109.1 . . ?
C72 C71 C70 103.9(4) . . ?
C72 C71 H71A 111.0 . . ?
C70 C71 H71A 111.0 . . ?
C72 C71 H71B 111.0 . . ?
C70 C71 H71B 111.0 . . ?
H71A C71 H71B 109.0 . . ?
O12 C72 C71 104.1(4) . . ?
O12 C72 H72A 110.9 . . ?
C71 C72 H72A 110.9 . . ?
O12 C72 H72B 110.9 . . ?
C71 C72 H72B 110.9 . . ?
H72A C72 H72B 109.0 . . ?
O7 P3 C5 116.7(2) . . ?
O7 P3 C33 108.11(18) . . ?
C5 P3 C33 109.0(2) . . ?
O7 P3 C39 106.88(19) . . ?
C5 P3 C39 107.5(2) . . ?
C33 P3 C39 108.34(19) . . ?
C6 O3 Li3 137.8(4) . . ?
C4 C3 P2 162.4(4) . . ?
O3 Li3 O11 113.9(4) . . ?
O3 Li3 O8 114.9(4) . 1_545 ?
O11 Li3 O8 106.0(4) . 1_545 ?
O3 Li3 O8 116.9(4) . 2_777 ?
O11 Li3 O8 108.1(4) . 2_777 ?
O8 Li3 O8 95.0(3) 1_545 2_777 ?
O8 P4 C7 116.5(2) . . ?
O8 P4 C51 111.49(18) . . ?
C7 P4 C51 108.2(2) . . ?
O8 P4 C45 108.89(18) . . ?
C7 P4 C45 108.5(2) . . ?
C51 P4 C45 102.21(19) . . ?
O8 P4 Li3 30.73(17) . 2_777 ?
C7 P4 Li3 87.1(2) . 2_777 ?
C51 P4 Li3 117.1(2) . 2_777 ?
C45 P4 Li3 130.73(19) . 2_777 ?
C8 O4 Li4 134.8(4) . . ?
O2 C4 C3 176.7(5) . . ?
O7 Li4 O7 91.1(3) 2_777 . ?
O7 Li4 O4 116.7(4) 2_777 . ?
O7 Li4 O4 118.3(4) . . ?
O7 Li4 O12 118.4(4) 2_777 . ?
O7 Li4 O12 111.2(4) . . ?
O4 Li4 O12 102.0(4) . . ?
P1 O5 Li2 145.5(3) . 1_545 ?
P1 O5 Li2 126.3(3) . 2_666 ?
Li2 O5 Li2 86.6(3) 1_545 2_666 ?
C6 C5 P3 152.1(5) . . ?
P2 O6 Li1 144.1(3) . . ?
P2 O6 Li1 125.1(3) . 2_666 ?
Li1 O6 Li1 88.1(3) . 2_666 ?
O3 C6 C5 175.0(5) . . ?
P3 O7 Li4 135.4(3) . 2_777 ?
P3 O7 Li4 135.6(3) . . ?
Li4 O7 Li4 88.9(3) 2_777 . ?
C8 C7 P4 165.7(4) . . ?
P4 O8 Li3 148.0(3) . 1_565 ?
P4 O8 Li3 126.1(3) . 2_777 ?
Li3 O8 Li3 85.0(3) 1_565 2_777 ?
O4 C8 C7 177.4(5) . . ?
C60 O9 C57 110.0(4) . . ?
C60 O9 Li1 126.2(4) . . ?
C57 O9 Li1 123.8(4) . . ?
C10 C9 C14 119.6(4) . . ?
C10 C9 P1 120.0(3) . . ?
C14 C9 P1 120.4(3) . . ?
C64 O10 C61 108.2(3) . . ?
C64 O10 Li2 114.9(3) . . ?
C61 O10 Li2 121.7(3) . . ?
C9 C10 C11 120.3(4) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
C65 O11 C68 109.0(4) . . ?
C65 O11 Li3 118.6(3) . . ?
C68 O11 Li3 126.1(4) . . ?
C12 C11 C10 119.8(5) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C69 O12 C72 104.8(3) . . ?
C69 O12 Li4 123.5(4) . . ?
C72 O12 Li4 124.2(3) . . ?
O2 Li2 O5 115.1(4) . 1_565 ?
O2 Li2 O10 113.0(4) . . ?
O5 Li2 O10 106.9(3) 1_565 . ?
O2 Li2 O5 115.7(4) . 2_666 ?
O5 Li2 O5 93.4(3) 1_565 2_666 ?
O10 Li2 O5 110.9(4) . 2_666 ?
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 O5 1.510(3) . ?
P1 C1 1.677(4) . ?
P1 C15 1.804(4) . ?
P1 C9 1.812(4) . ?
P1 Li2 3.085(7) 2_666 ?
O1 C2 1.216(5) . ?
O1 Li1 1.916(8) . ?
C1 C2 1.230(6) . ?
C12 C13 1.379(8) . ?
C12 C11 1.381(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.388(6) . ?
C13 H13 0.9300 . ?
C14 C9 1.389(6) . ?
C14 H14 0.9300 . ?
C15 C20 1.394(6) . ?
C15 C16 1.395(6) . ?
C16 C17 1.377(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.369(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.379(8) . ?
C18 H18 0.9300 . ?
C29 C30 1.381(7) . ?
C29 C28 1.386(7) . ?
C29 H29 0.9300 . ?
C30 C31 1.377(7) . ?
C30 H30 0.9300 . ?
C31 C32 1.387(6) . ?
C31 H31 0.9300 . ?
C32 C27 1.396(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.385(6) . ?
C33 C38 1.386(6) . ?
C33 P3 1.796(4) . ?
C19 C20 1.382(6) . ?
C19 H19 0.9300 . ?
C21 C22 1.392(6) . ?
C21 C26 1.403(6) . ?
C21 P2 1.800(4) . ?
C22 C23 1.377(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.385(7) . ?
C23 H23 0.9300 . ?
C24 C25 1.389(6) . ?
C24 H24 0.9300 . ?
C20 H20 0.9300 . ?
Li1 O9 1.912(8) . ?
Li1 O6 1.925(8) . ?
Li1 O6 1.935(8) 2_666 ?
P2 O6 1.509(3) . ?
P2 C3 1.673(4) . ?
P2 C27 1.810(5) . ?
O2 C4 1.206(5) . ?
O2 Li2 1.873(8) . ?
C25 C26 1.375(6) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C28 1.385(6) . ?
C28 H28 0.9300 . ?
C34 C35 1.380(7) . ?
C34 H34 0.9300 . ?
C35 C36 1.388(7) . ?
C35 H35 0.9300 . ?
C36 C37 1.363(7) . ?
C36 H36 0.9300 . ?
C37 C38 1.405(7) . ?
C37 H37 0.9300 . ?
C38 H38 0.9300 . ?
C39 C44 1.395(6) . ?
C39 C40 1.396(6) . ?
C39 P3 1.800(4) . ?
C40 C41 1.381(7) . ?
C40 H40 0.9300 . ?
C41 C42 1.378(8) . ?
C41 H41 0.9300 . ?
C42 C43 1.382(7) . ?
C42 H42 0.9300 . ?
C43 C44 1.394(6) . ?
C43 H43 0.9300 . ?
C44 H44 0.9300 . ?
C45 C50 1.387(6) . ?
C45 C46 1.407(6) . ?
C45 P4 1.813(4) . ?
C46 C47 1.382(6) . ?
C46 H46 0.9300 . ?
C47 C48 1.387(7) . ?
C47 H47 0.9300 . ?
C55 C54 1.361(7) . ?
C55 C56 1.396(7) . ?
C55 H55 0.9300 . ?
C56 C51 1.399(6) . ?
C56 H56 0.9300 . ?
C48 C49 1.383(7) . ?
C48 H48 0.9300 . ?
C54 C53 1.396(7) . ?
C54 H54 0.9300 . ?
C49 C50 1.389(6) . ?
C49 H49 0.9300 . ?
C53 C52 1.377(6) . ?
C53 H53 0.9300 . ?
C50 H50 0.9300 . ?
C51 C52 1.408(6) . ?
C51 P4 1.797(4) . ?
C52 H52 0.9300 . ?
C57 O9 1.444(7) . ?
C57 C58 1.500(9) . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C58 C59 1.517(11) . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C59 C60 1.506(9) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C60 O9 1.414(6) . ?
C60 H60A 0.9700 . ?
C60 H60B 0.9700 . ?
C61 O10 1.445(5) . ?
C61 C62 1.518(7) . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C62 C63 1.540(7) . ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?
C63 C64 1.508(7) . ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
C64 O10 1.443(5) . ?
C64 H64A 0.9700 . ?
C64 H64B 0.9700 . ?
C65 O11 1.436(5) . ?
C65 C66 1.464(8) . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
C66 C67 1.502(10) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
C67 C68 1.525(8) . ?
C67 H67A 0.9700 . ?
C67 H67B 0.9700 . ?
C68 O11 1.438(5) . ?
C68 H68A 0.9700 . ?
C68 H68B 0.9700 . ?
C69 O12 1.424(6) . ?
C69 C70 1.535(7) . ?
C69 H69A 0.9700 . ?
C69 H69B 0.9700 . ?
C70 C71 1.542(7) . ?
C70 H70A 0.9700 . ?
C70 H70B 0.9700 . ?
C71 C72 1.516(7) . ?
C71 H71A 0.9700 . ?
C71 H71B 0.9700 . ?
C72 O12 1.434(5) . ?
C72 H72A 0.9700 . ?
C72 H72B 0.9700 . ?
P3 O7 1.514(3) . ?
P3 C5 1.676(5) . ?
O3 C6 1.214(5) . ?
O3 Li3 1.887(8) . ?
C3 C4 1.231(6) . ?
Li3 O11 1.926(8) . ?
Li3 O8 1.931(8) 1_545 ?
Li3 O8 1.958(8) 2_777 ?
P4 O8 1.509(3) . ?
P4 C7 1.676(4) . ?
O4 C8 1.219(5) . ?
O4 Li4 1.932(8) . ?
Li4 O7 1.897(8) 2_777 ?
Li4 O7 1.921(8) . ?
Li4 O12 1.951(8) . ?
O5 Li2 1.929(7) 1_545 ?
O5 Li2 1.941(7) 2_666 ?
C5 C6 1.235(6) . ?
C7 C8 1.228(6) . ?
C9 C10 1.385(6) . ?
O10 Li2 1.939(8) . ?
C10 C11 1.386(6) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
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
O5 P1 C1 C2 48.3(14) . . . . ?
C15 P1 C1 C2 -77.0(13) . . . . ?
C9 P1 C1 C2 169.2(13) . . . . ?
Li2 P1 C1 C2 39.3(13) 2_666 . . . ?
C11 C12 C13 C14 -0.6(7) . . . . ?
C12 C13 C14 C9 0.1(7) . . . . ?
O5 P1 C15 C20 84.3(4) . . . . ?
C1 P1 C15 C20 -147.6(4) . . . . ?
C9 P1 C15 C20 -33.0(4) . . . . ?
Li2 P1 C15 C20 117.2(4) 2_666 . . . ?
O5 P1 C15 C16 -93.6(4) . . . . ?
C1 P1 C15 C16 34.5(4) . . . . ?
C9 P1 C15 C16 149.1(3) . . . . ?
Li2 P1 C15 C16 -60.7(4) 2_666 . . . ?
C20 C15 C16 C17 0.2(7) . . . . ?
P1 C15 C16 C17 178.2(4) . . . . ?
C15 C16 C17 C18 1.1(7) . . . . ?
C16 C17 C18 C19 -1.7(8) . . . . ?
C28 C29 C30 C31 -1.1(8) . . . . ?
C29 C30 C31 C32 1.1(8) . . . . ?
C30 C31 C32 C27 -0.8(7) . . . . ?
C17 C18 C19 C20 1.0(7) . . . . ?
C26 C21 C22 C23 -0.9(7) . . . . ?
P2 C21 C22 C23 179.5(4) . . . . ?
C21 C22 C23 C24 -0.2(7) . . . . ?
C22 C23 C24 C25 1.8(7) . . . . ?
C18 C19 C20 C15 0.4(7) . . . . ?
C16 C15 C20 C19 -1.0(7) . . . . ?
P1 C15 C20 C19 -178.9(3) . . . . ?
C22 C21 P2 O6 139.4(4) . . . . ?
C26 C21 P2 O6 -40.2(4) . . . . ?
C22 C21 P2 C3 11.0(4) . . . . ?
C26 C21 P2 C3 -168.7(4) . . . . ?
C22 C21 P2 C27 -104.2(4) . . . . ?
C26 C21 P2 C27 76.1(4) . . . . ?
C22 C21 P2 Li1 128.2(4) . . . 2_666 ?
C26 C21 P2 Li1 -51.5(5) . . . 2_666 ?
C23 C24 C25 C26 -2.2(7) . . . . ?
C24 C25 C26 C21 1.1(7) . . . . ?
C22 C21 C26 C25 0.4(6) . . . . ?
P2 C21 C26 C25 -179.9(3) . . . . ?
C31 C32 C27 C28 0.4(7) . . . . ?
C31 C32 C27 P2 -178.1(4) . . . . ?
O6 P2 C27 C28 -147.8(4) . . . . ?
C3 P2 C27 C28 -19.9(5) . . . . ?
C21 P2 C27 C28 95.9(4) . . . . ?
Li1 P2 C27 C28 -116.7(4) 2_666 . . . ?
O6 P2 C27 C32 30.7(4) . . . . ?
C3 P2 C27 C32 158.6(4) . . . . ?
C21 P2 C27 C32 -85.6(4) . . . . ?
Li1 P2 C27 C32 61.8(4) 2_666 . . . ?
C32 C27 C28 C29 -0.4(7) . . . . ?
P2 C27 C28 C29 178.1(4) . . . . ?
C30 C29 C28 C27 0.8(8) . . . . ?
C38 C33 C34 C35 0.4(7) . . . . ?
P3 C33 C34 C35 -178.1(4) . . . . ?
C33 C34 C35 C36 -1.2(8) . . . . ?
C34 C35 C36 C37 1.3(8) . . . . ?
C35 C36 C37 C38 -0.6(8) . . . . ?
C34 C33 C38 C37 0.3(7) . . . . ?
P3 C33 C38 C37 178.7(4) . . . . ?
C36 C37 C38 C33 -0.2(8) . . . . ?
C44 C39 C40 C41 -0.3(7) . . . . ?
P3 C39 C40 C41 173.9(4) . . . . ?
C39 C40 C41 C42 -0.5(8) . . . . ?
C40 C41 C42 C43 1.2(8) . . . . ?
C41 C42 C43 C44 -1.1(8) . . . . ?
C42 C43 C44 C39 0.3(7) . . . . ?
C40 C39 C44 C43 0.4(7) . . . . ?
P3 C39 C44 C43 -173.9(4) . . . . ?
C50 C45 C46 C47 1.1(6) . . . . ?
P4 C45 C46 C47 -179.8(3) . . . . ?
C45 C46 C47 C48 0.1(7) . . . . ?
C54 C55 C56 C51 0.6(7) . . . . ?
C46 C47 C48 C49 -1.0(7) . . . . ?
C56 C55 C54 C53 -1.4(8) . . . . ?
C47 C48 C49 C50 0.6(7) . . . . ?
C55 C54 C53 C52 1.5(7) . . . . ?
C46 C45 C50 C49 -1.6(6) . . . . ?
P4 C45 C50 C49 179.4(3) . . . . ?
C48 C49 C50 C45 0.7(7) . . . . ?
C55 C56 C51 C52 0.2(7) . . . . ?
C55 C56 C51 P4 -172.5(4) . . . . ?
C54 C53 C52 C51 -0.8(7) . . . . ?
C56 C51 C52 C53 -0.1(7) . . . . ?
P4 C51 C52 C53 173.0(4) . . . . ?
O9 C57 C58 C59 -26.3(8) . . . . ?
C57 C58 C59 C60 37.4(7) . . . . ?
C58 C59 C60 O9 -35.7(6) . . . . ?
O10 C61 C62 C63 7.6(5) . . . . ?
C61 C62 C63 C64 -26.3(5) . . . . ?
C62 C63 C64 O10 36.1(5) . . . . ?
O11 C65 C66 C67 38.3(6) . . . . ?
C65 C66 C67 C68 -34.0(7) . . . . ?
C66 C67 C68 O11 17.8(7) . . . . ?
O12 C69 C70 C71 -20.8(5) . . . . ?
C69 C70 C71 C72 -5.0(5) . . . . ?
C70 C71 C72 O12 28.9(5) . . . . ?
C34 C33 P3 O7 80.2(4) . . . . ?
C38 C33 P3 O7 -98.2(4) . . . . ?
C34 C33 P3 C5 -47.6(4) . . . . ?
C38 C33 P3 C5 133.9(4) . . . . ?
C34 C33 P3 C39 -164.3(4) . . . . ?
C38 C33 P3 C39 17.2(4) . . . . ?
C44 C39 P3 O7 30.0(4) . . . . ?
C40 C39 P3 O7 -144.1(4) . . . . ?
C44 C39 P3 C5 156.1(4) . . . . ?
C40 C39 P3 C5 -18.0(4) . . . . ?
C44 C39 P3 C33 -86.3(4) . . . . ?
C40 C39 P3 C33 99.6(4) . . . . ?
O6 P2 C3 C4 -14.0(16) . . . . ?
C21 P2 C3 C4 108.8(15) . . . . ?
C27 P2 C3 C4 -136.2(15) . . . . ?
Li1 P2 C3 C4 -34.5(15) 2_666 . . . ?
C6 O3 Li3 O11 45.7(7) . . . . ?
C6 O3 Li3 O8 168.3(5) . . . 1_545 ?
C6 O3 Li3 O8 -81.6(7) . . . 2_777 ?
C56 C51 P4 O8 -134.9(4) . . . . ?
C52 C51 P4 O8 52.5(4) . . . . ?
C56 C51 P4 C7 -5.4(4) . . . . ?
C52 C51 P4 C7 -178.1(3) . . . . ?
C56 C51 P4 C45 109.0(4) . . . . ?
C52 C51 P4 C45 -63.7(4) . . . . ?
C56 C51 P4 Li3 -101.6(4) . . . 2_777 ?
C52 C51 P4 Li3 85.7(4) . . . 2_777 ?
C50 C45 P4 O8 14.5(4) . . . . ?
C46 C45 P4 O8 -164.6(3) . . . . ?
C50 C45 P4 C7 -113.3(4) . . . . ?
C46 C45 P4 C7 67.6(4) . . . . ?
C50 C45 P4 C51 132.5(4) . . . . ?
C46 C45 P4 C51 -46.6(4) . . . . ?
C50 C45 P4 Li3 -10.8(5) . . . 2_777 ?
C46 C45 P4 Li3 170.1(3) . . . 2_777 ?
C1 P1 O5 Li2 -177.9(5) . . . 1_545 ?
C15 P1 O5 Li2 -54.1(5) . . . 1_545 ?
C9 P1 O5 Li2 61.8(5) . . . 1_545 ?
Li2 P1 O5 Li2 -160.0(5) 2_666 . . 1_545 ?
C1 P1 O5 Li2 -17.9(4) . . . 2_666 ?
C15 P1 O5 Li2 105.9(3) . . . 2_666 ?
C9 P1 O5 Li2 -138.3(3) . . . 2_666 ?
O7 P3 C5 C6 -85.4(10) . . . . ?
C33 P3 C5 C6 37.4(10) . . . . ?
C39 P3 C5 C6 154.6(9) . . . . ?
C3 P2 O6 Li1 163.0(5) . . . . ?
C21 P2 O6 Li1 40.3(5) . . . . ?
C27 P2 O6 Li1 -75.3(5) . . . . ?
Li1 P2 O6 Li1 -154.4(5) 2_666 . . . ?
C3 P2 O6 Li1 -42.6(4) . . . 2_666 ?
C21 P2 O6 Li1 -165.3(3) . . . 2_666 ?
C27 P2 O6 Li1 79.1(4) . . . 2_666 ?
C5 P3 O7 Li4 -23.2(5) . . . 2_777 ?
C33 P3 O7 Li4 -146.4(4) . . . 2_777 ?
C39 P3 O7 Li4 97.2(4) . . . 2_777 ?
C5 P3 O7 Li4 151.4(4) . . . . ?
C33 P3 O7 Li4 28.2(5) . . . . ?
C39 P3 O7 Li4 -88.3(4) . . . . ?
O8 P4 C7 C8 -17.5(19) . . . . ?
C51 P4 C7 C8 -144.1(17) . . . . ?
C45 P4 C7 C8 105.7(18) . . . . ?
Li3 P4 C7 C8 -26.5(18) 2_777 . . . ?
C7 P4 O8 Li3 178.3(5) . . . 1_565 ?
C51 P4 O8 Li3 -56.8(6) . . . 1_565 ?
C45 P4 O8 Li3 55.2(6) . . . 1_565 ?
Li3 P4 O8 Li3 -164.1(6) 2_777 . . 1_565 ?
C7 P4 O8 Li3 -17.7(4) . . . 2_777 ?
C51 P4 O8 Li3 107.3(4) . . . 2_777 ?
C45 P4 O8 Li3 -140.7(3) . . . 2_777 ?
C59 C60 O9 C57 19.9(6) . . . . ?
C59 C60 O9 Li1 -157.0(5) . . . . ?
C58 C57 O9 C60 4.3(8) . . . . ?
C58 C57 O9 Li1 -178.7(5) . . . . ?
C13 C14 C9 C10 1.1(6) . . . . ?
C13 C14 C9 P1 -176.8(3) . . . . ?
O5 P1 C9 C10 9.4(4) . . . . ?
C1 P1 C9 C10 -116.2(4) . . . . ?
C15 P1 C9 C10 128.5(3) . . . . ?
Li2 P1 C9 C10 -16.4(5) 2_666 . . . ?
O5 P1 C9 C14 -172.7(3) . . . . ?
C1 P1 C9 C14 61.7(4) . . . . ?
C15 P1 C9 C14 -53.5(4) . . . . ?
Li2 P1 C9 C14 161.6(3) 2_666 . . . ?
C63 C64 O10 C61 -32.7(5) . . . . ?
C63 C64 O10 Li2 106.9(4) . . . . ?
C62 C61 O10 C64 15.4(5) . . . . ?
C62 C61 O10 Li2 -120.9(4) . . . . ?
C14 C9 C10 C11 -1.8(6) . . . . ?
P1 C9 C10 C11 176.1(3) . . . . ?
C66 C65 O11 C68 -28.5(6) . . . . ?
C66 C65 O11 Li3 125.4(5) . . . . ?
C67 C68 O11 C65 6.1(6) . . . . ?
C67 C68 O11 Li3 -145.4(5) . . . . ?
C13 C12 C11 C10 -0.1(7) . . . . ?
C9 C10 C11 C12 1.3(7) . . . . ?
C70 C69 O12 C72 40.3(5) . . . . ?
C70 C69 O12 Li4 -110.4(5) . . . . ?
C71 C72 O12 C69 -43.6(5) . . . . ?
C71 C72 O12 Li4 106.9(5) . . . . ?
C4 O2 Li2 O5 -154.4(8) . . . 1_565 ?
C4 O2 Li2 O10 82.4(10) . . . . ?
C4 O2 Li2 O5 -47.1(11) . . . 2_666 ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.6076 23361 22773 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.3924 23342 22773 nmt -0.9996 0.0001 -0.0006 -0.0008 -1.0004 -0.0002 0.0793
0.0313 0.9999
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
0.9997 -0.0005 -1.9991 -0.0680 0.1022 -0.1867
-8.2507 3.5680 -3.8057 -0.9325 -0.1738 0.3167
3.4969 1.8958 8.7661 0.8221 0.2446 0.5142
7.9490 -1.8969 4.8383 0.9474 0.2811 -0.1532
-6.6685 -1.5205 -6.0605 -0.8682 -0.4719 -0.1533
-5.7142 0.2407 8.0928 0.1509 -0.5044 0.8502
5.5139 4.0335 5.8985 0.7207 0.6167 0.3167
5.7279 -0.4391 -8.0983 -0.1460 0.4881 -0.8605
-0.2078 -8.9807 4.2694 0.4746 -0.8726 -0.1151
-1.9996 10.0206 -0.7686 -0.4104 0.7538 0.5132
-0.9997 0.0005 1.9991 0.0680 -0.1022 0.1867
-2.8651 -7.8073 4.6141 0.2834 -0.9542 0.0956
6.4987 1.6592 6.2219 0.8644 0.4698 0.1793
