# Supplementary Information (SI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_PD-440_auto_a
_database_code_depnum_ccdc_archive 'CCDC 2362606'
loop_
_audit_author_name
_audit_author_address
'Kai-Stephan Feichtner'
;Ruhr Universitaet Bochum
Germany
;
_audit_update_record             
;
2024-07-31 deposited with the CCDC.	2024-08-01 downloaded from the CCDC.
;
#

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C70 H66 Li2 O2 P4 Se2'
_chemical_formula_sum            'C70 H66 Li2 O2 P4 Se2'
_chemical_formula_weight         1234.90
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'
Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

#

_cell_length_a                   15.72650(10)
_cell_length_b                   9.50190(10)
_cell_length_c                   20.4394(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.1570(10)
_cell_angle_gamma                90
_cell_volume                     3030.50(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    26409
_cell_measurement_theta_min      2.8200
_cell_measurement_theta_max      75.8840
_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_F_000             1272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    2.869
_shelx_estimated_absorpt_T_min   0.500
_shelx_estimated_absorpt_T_max   0.689
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.545
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            38788
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.832
_diffrn_reflns_theta_max         76.746
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6214
_reflns_number_gt                5859
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0422P)²+3.1317P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6214
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0893
_refine_ls_wR_factor_gt          0.0879
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Se1 Se 0.50961(2) 0.38873(2) 0.58926(2) 0.02309(8) Uani 1 1 d . . . . .
P1 P 0.63428(3) 0.49269(5) 0.61219(2) 0.01914(11) Uani 1 1 d . . . . .
O1 O 0.60016(10) 0.23751(16) 0.44241(8) 0.0324(3) Uani 1 1 d . . . . .
C1 C 0.68397(12) 0.5120(2) 0.54493(9) 0.0207(4) Uani 1 1 d . . . . .
Li1 Li 0.5804(2) 0.4173(4) 0.48049(18) 0.0289(7) Uani 1 1 d . . . . .
C2 C 0.61015(12) 0.6600(2) 0.64967(10) 0.0231(4) Uani 1 1 d . . . . .
C3 C 0.58274(13) 0.6656(3) 0.71211(10) 0.0295(4) Uani 1 1 d . . . . .
H3 H 0.578847 0.581496 0.736677 0.035 Uiso 1 1 calc R U . . .
C4 C 0.56112(14) 0.7940(3) 0.73844(11) 0.0362(5) Uani 1 1 d . . . . .
H4 H 0.542223 0.797323 0.780783 0.043 Uiso 1 1 calc R U . . .
C5 C 0.56713(15) 0.9165(3) 0.70305(13) 0.0376(5) Uani 1 1 d . . . . .
H5 H 0.553074 1.004095 0.721347 0.045 Uiso 1 1 calc R U . . .
C6 C 0.59356(15) 0.9122(2) 0.64101(13) 0.0361(5) Uani 1 1 d . . . . .
H6 H 0.596955 0.996615 0.616580 0.043 Uiso 1 1 calc R U . . .
C7 C 0.61521(13) 0.7839(2) 0.61433(11) 0.0278(4) Uani 1 1 d . . . . .
H7 H 0.633518 0.781260 0.571778 0.033 Uiso 1 1 calc R U . . .
C8 C 0.69358(13) 0.3974(2) 0.68177(10) 0.0230(4) Uani 1 1 d . . . . .
C9 C 0.67663(14) 0.2562(2) 0.69311(10) 0.0284(4) Uani 1 1 d . . . . .
H9 H 0.628973 0.211718 0.668314 0.034 Uiso 1 1 calc R U . . .
C10 C 0.72873(15) 0.1795(2) 0.74035(11) 0.0322(5) Uani 1 1 d . . . . .
H10 H 0.716917 0.082935 0.747251 0.039 Uiso 1 1 calc R U . . .
C11 C 0.79776(14) 0.2438(2) 0.77731(11) 0.0318(5) Uani 1 1 d . . . . .
H11 H 0.833650 0.191389 0.809329 0.038 Uiso 1 1 calc R U . . .
C12 C 0.81423(14) 0.3850(2) 0.76734(11) 0.0300(5) Uani 1 1 d . . . . .
H12 H 0.861127 0.429676 0.793000 0.036 Uiso 1 1 calc R U . . .
C13 C 0.76265(13) 0.4614(2) 0.72015(10) 0.0255(4) Uani 1 1 d . . . . .
H13 H 0.774342 0.558246 0.713831 0.031 Uiso 1 1 calc R U . . .
C14 C 0.86283(12) 0.5913(2) 0.59968(9) 0.0217(4) Uani 1 1 d . . . . .
C15 C 0.84530(13) 0.7260(2) 0.62205(10) 0.0265(4) Uani 1 1 d . . . . .
H15 H 0.796765 0.776118 0.601739 0.032 Uiso 1 1 calc R U . . .
C16 C 0.89828(15) 0.7872(2) 0.67371(11) 0.0315(5) Uani 1 1 d . . . . .
H16 H 0.885933 0.878927 0.688449 0.038 Uiso 1 1 calc R U . . .
C17 C 0.96921(14) 0.7148(3) 0.70391(11) 0.0337(5) Uani 1 1 d . . . . .
H17 H 1.004977 0.756252 0.739645 0.040 Uiso 1 1 calc R U . . .
C18 C 0.98755(14) 0.5821(3) 0.68172(11) 0.0326(5) Uani 1 1 d . . . . .
H18 H 1.036329 0.532638 0.702039 0.039 Uiso 1 1 calc R U . . .
C19 C 0.93482(13) 0.5206(2) 0.62969(10) 0.0270(4) Uani 1 1 d . . . . .
H19 H 0.948119 0.429642 0.614574 0.032 Uiso 1 1 calc R U . . .
C20 C 0.80630(12) 0.61325(19) 0.46179(9) 0.0208(4) Uani 1 1 d . . . . .
C21 C 0.88736(13) 0.6698(2) 0.45690(10) 0.0258(4) Uani 1 1 d . . . . .
H21 H 0.931746 0.659718 0.492624 0.031 Uiso 1 1 calc R U . . .
C22 C 0.90355(14) 0.7405(2) 0.40032(11) 0.0288(4) Uani 1 1 d . . . . .
H22 H 0.958611 0.779558 0.397620 0.035 Uiso 1 1 calc R U . . .
C23 C 0.83957(15) 0.7539(2) 0.34800(11) 0.0320(5) Uani 1 1 d . . . . .
H23 H 0.850925 0.800721 0.308936 0.038 Uiso 1 1 calc R U . . .
C24 C 0.75877(15) 0.6993(3) 0.35238(11) 0.0360(5) Uani 1 1 d . . . . .
H24 H 0.714777 0.709261 0.316371 0.043 Uiso 1 1 calc R U . . .
C25 C 0.74175(14) 0.6298(2) 0.40936(11) 0.0292(4) Uani 1 1 d . . . . .
H25 H 0.686031 0.593774 0.412376 0.035 Uiso 1 1 calc R U . . .
C26 C 0.83345(12) 0.3412(2) 0.52055(10) 0.0234(4) Uani 1 1 d . . . . .
C27 C 0.88004(13) 0.3113(2) 0.46848(10) 0.0276(4) Uani 1 1 d . . . . .
H27 H 0.891246 0.383897 0.438760 0.033 Uiso 1 1 calc R U . . .
C28 C 0.91019(15) 0.1758(2) 0.45981(12) 0.0350(5) Uani 1 1 d . . . . .
H28 H 0.941712 0.156143 0.424129 0.042 Uiso 1 1 calc R U . . .
C29 C 0.89442(15) 0.0697(2) 0.50294(14) 0.0389(6) Uani 1 1 d . . . . .
H29 H 0.914778 -0.022891 0.496826 0.047 Uiso 1 1 calc R U . . .
C30 C 0.84910(17) 0.0986(2) 0.55482(16) 0.0440(6) Uani 1 1 d . . . . .
H30 H 0.838951 0.026043 0.584850 0.053 Uiso 1 1 calc R U . . .
C31 C 0.81818(16) 0.2332(2) 0.56345(13) 0.0370(5) Uani 1 1 d . . . . .
H31 H 0.786268 0.251755 0.599023 0.044 Uiso 1 1 calc R U . . .
C32 C 0.64275(16) 0.2175(3) 0.38474(11) 0.0359(5) Uani 1 1 d . . . . .
H32A H 0.691336 0.283843 0.385065 0.043 Uiso 1 1 calc R U . . .
H32B H 0.602402 0.233950 0.344282 0.043 Uiso 1 1 calc R U . . .
C33 C 0.67441(19) 0.0683(3) 0.38679(14) 0.0465(6) Uani 1 1 d . . . . .
H33A H 0.736702 0.064614 0.401784 0.056 Uiso 1 1 calc R U . . .
H33B H 0.663333 0.024236 0.342647 0.056 Uiso 1 1 calc R U . . .
C34 C 0.62498(19) -0.0056(3) 0.43497(16) 0.0479(6) Uani 1 1 d . . . . .
H34A H 0.659922 -0.080293 0.458996 0.057 Uiso 1 1 calc R U . . .
H34B H 0.571716 -0.047767 0.412335 0.057 Uiso 1 1 calc R U . . .
P2 P 0.78609(3) 0.51389(5) 0.53458(2) 0.01823(11) Uani 1 1 d . . . . .
C35 C 0.60508(18) 0.1109(2) 0.48128(13) 0.0395(6) Uani 1 1 d . . . . .
H35A H 0.549965 0.092761 0.498463 0.047 Uiso 1 1 calc R U . . .
H35B H 0.650925 0.118548 0.518970 0.047 Uiso 1 1 calc R U . . .

#


#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Se1 P1 2.1933(5) . ?
Se1 Li1 2.622(4) . ?
Se1 Li1 2.632(4) 3_666 ?
P1 C1 1.6737(19) . ?
P1 C2 1.825(2) . ?
P1 C8 1.839(2) . ?
P1 Li1 2.812(4) . ?
O1 C35 1.438(3) . ?
O1 C32 1.439(3) . ?
O1 Li1 1.919(4) . ?
C1 P2 1.6459(19) . ?
C1 Li1 2.159(4) . ?
C2 C7 1.388(3) . ?
C2 C3 1.398(3) . ?
C3 C4 1.393(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.379(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.383(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.395(3) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.393(3) . ?
C8 C13 1.398(3) . ?
C9 C10 1.392(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.385(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.387(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.386(3) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C19 1.392(3) . ?
C14 C15 1.398(3) . ?
C14 P2 1.835(2) . ?
C15 C16 1.388(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.388(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.383(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.393(3) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C25 1.390(3) . ?
C20 C21 1.398(3) . ?
C20 P2 1.823(2) . ?
C21 C22 1.388(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.380(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.386(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.393(3) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C31 1.390(3) . ?
C26 C27 1.395(3) . ?
C26 P2 1.839(2) . ?
C27 C28 1.391(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.382(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.377(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.387(3) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 C33 1.502(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.502(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.514(4) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 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 Se1 Li1 70.84(8) . . ?
P1 Se1 Li1 101.92(8) . 3_666 ?
Li1 Se1 Li1 74.03(13) . 3_666 ?
C1 P1 C2 113.08(9) . . ?
C1 P1 C8 116.45(9) . . ?
C2 P1 C8 102.49(9) . . ?
C1 P1 Se1 111.73(7) . . ?
C2 P1 Se1 104.77(6) . . ?
C8 P1 Se1 107.29(7) . . ?
C1 P1 Li1 50.03(10) . . ?
C2 P1 Li1 124.75(10) . . ?
C8 P1 Li1 132.70(10) . . ?
Se1 P1 Li1 61.71(8) . . ?
C35 O1 C32 110.10(17) . . ?
C35 O1 Li1 121.38(17) . . ?
C32 O1 Li1 124.42(18) . . ?
P2 C1 P1 132.04(12) . . ?
P2 C1 Li1 126.87(14) . . ?
P1 C1 Li1 93.53(13) . . ?
O1 Li1 C1 118.06(19) . . ?
O1 Li1 Se1 111.04(17) . . ?
C1 Li1 Se1 83.89(13) . . ?
O1 Li1 Se1 120.47(17) . 3_666 ?
C1 Li1 Se1 110.65(16) . 3_666 ?
Se1 Li1 Se1 105.98(13) . 3_666 ?
C7 C2 C3 119.14(19) . . ?
C7 C2 P1 119.46(15) . . ?
C3 C2 P1 121.33(17) . . ?
C4 C3 C2 120.2(2) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C5 C4 C3 120.0(2) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.3(2) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C7 120.0(2) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C2 C7 C6 120.3(2) . . ?
C2 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C9 C8 C13 118.52(19) . . ?
C9 C8 P1 120.92(16) . . ?
C13 C8 P1 120.22(15) . . ?
C10 C9 C8 120.8(2) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C11 C10 C9 120.1(2) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C12 119.7(2) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C13 C12 C11 120.4(2) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C12 C13 C8 120.6(2) . . ?
C12 C13 H13 119.7 . . ?
C8 C13 H13 119.7 . . ?
C19 C14 C15 118.72(19) . . ?
C19 C14 P2 123.48(16) . . ?
C15 C14 P2 117.74(15) . . ?
C16 C15 C14 120.5(2) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C17 C16 C15 120.2(2) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C18 C17 C16 119.7(2) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C17 C18 C19 120.3(2) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C14 C19 C18 120.6(2) . . ?
C14 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
C25 C20 C21 119.08(18) . . ?
C25 C20 P2 120.19(15) . . ?
C21 C20 P2 120.69(15) . . ?
C22 C21 C20 120.59(19) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C23 C22 C21 119.9(2) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C24 120.1(2) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C23 C24 C25 120.3(2) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C20 C25 C24 120.0(2) . . ?
C20 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C31 C26 C27 118.64(19) . . ?
C31 C26 P2 117.08(16) . . ?
C27 C26 P2 124.22(16) . . ?
C28 C27 C26 120.4(2) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C29 C28 C27 120.2(2) . . ?
C29 C28 H28 119.9 . . ?
C27 C28 H28 119.9 . . ?
C30 C29 C28 119.8(2) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C29 C30 C31 120.3(2) . . ?
C29 C30 H30 119.8 . . ?
C31 C30 H30 119.8 . . ?
C30 C31 C26 120.6(2) . . ?
C30 C31 H31 119.7 . . ?
C26 C31 H31 119.7 . . ?
O1 C32 C33 106.8(2) . . ?
O1 C32 H32A 110.4 . . ?
C33 C32 H32A 110.4 . . ?
O1 C32 H32B 110.4 . . ?
C33 C32 H32B 110.4 . . ?
H32A C32 H32B 108.6 . . ?
C32 C33 C34 105.2(2) . . ?
C32 C33 H33A 110.7 . . ?
C34 C33 H33A 110.7 . . ?
C32 C33 H33B 110.7 . . ?
C34 C33 H33B 110.7 . . ?
H33A C33 H33B 108.8 . . ?
C33 C34 C35 103.5(2) . . ?
C33 C34 H34A 111.1 . . ?
C35 C34 H34A 111.1 . . ?
C33 C34 H34B 111.1 . . ?
C35 C34 H34B 111.1 . . ?
H34A C34 H34B 109.0 . . ?
C1 P2 C20 112.51(9) . . ?
C1 P2 C14 118.38(9) . . ?
C20 P2 C14 102.61(9) . . ?
C1 P2 C26 115.52(9) . . ?
C20 P2 C26 102.69(9) . . ?
C14 P2 C26 103.18(9) . . ?
O1 C35 C34 105.5(2) . . ?
O1 C35 H35A 110.6 . . ?
C34 C35 H35A 110.6 . . ?
O1 C35 H35B 110.6 . . ?
C34 C35 H35B 110.6 . . ?
H35A C35 H35B 108.8 . . ?

#

_refine_diff_density_max         1.184
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.064
######### additional information out of the cif_od #######  
_audit_creation_date             2023-10-22
_cell_oxdiff_length_a            15.7232(2)
_cell_oxdiff_length_b            9.50480(13)
_cell_oxdiff_length_c            20.4401(2)
_cell_oxdiff_angle_alpha         89.9348(11)
_cell_oxdiff_angle_beta          97.2173(11)
_cell_oxdiff_angle_gamma         89.9948(11)
_cell_oxdiff_volume              3030.49(7)
_cell_oxdiff_measurement_reflns_used 26409
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -6 3 0.0784
-2 -3 -11 0.0824
2 4 10 0.1067
0 6 -6 0.1275
-1 -5 6 0.0878
-2 5 8 0.1080
1 5 -6 0.1257
3 -4 -10 0.0723
10 0 0 0.0874
-10 0 0 0.0479
-1 6 6 0.1078
-2 0 13 0.1395
7 2 -9 0.1108

#

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
-0.7278 -6.0389 2.6319 0.0200 -0.1030 -0.9945
-1.9310 -3.2834 -10.5551 0.1760 -0.9448 -0.2765
1.9216 3.7819 9.7961 -0.1701 0.9131 0.3706
0.2597 5.5766 -5.6498 0.0259 -0.1435 0.9893
-1.1210 -5.4690 6.0883 0.0589 0.1703 -0.9836
-2.4684 4.8963 7.7636 0.2717 0.7665 0.5820
1.2216 5.3782 -6.4409 -0.0690 -0.1991 0.9775
2.9914 -3.8025 -10.1187 -0.3113 -0.8796 -0.3596
10.1109 0.0087 0.1432 -0.9915 0.1299 0.0126
-10.1101 0.0025 -0.1507 0.9915 -0.1299 -0.0107
-0.5098 5.5717 5.7119 0.0875 0.6724 0.7350
-2.4154 -0.4083 13.1527 0.2176 0.9076 -0.3590
7.3062 2.1812 -9.1140 -0.6879 -0.4728 0.5507

#

_oxdiff_exptl_absorpt_empirical_full_min 0.624
_oxdiff_exptl_absorpt_empirical_full_max 2.036
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_environment      N~2~
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0980477000
_diffrn_orient_matrix_UB_12      0.0079772000
_diffrn_orient_matrix_UB_13      -0.0012143000
_diffrn_orient_matrix_UB_21      0.0117756000
_diffrn_orient_matrix_UB_22      0.0473020000
_diffrn_orient_matrix_UB_23      0.0726384000
_diffrn_orient_matrix_UB_31      0.0014299000
_diffrn_orient_matrix_UB_32      0.1548215000
_diffrn_orient_matrix_UB_33      -0.0222225000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    108.00 178.00   0.50    0.44    --  105.91  45.00 -90.00  140
  2  ω     96.00 171.00   0.50    0.44    --  105.91 125.00 -90.00  150
  3  ω     96.00 132.00   0.50    0.44    --  105.91 125.00   0.00   72
  4  ω    135.00 169.00   0.50    0.44    --  105.91 125.00   0.00   68
  5  ω    118.00 143.00   0.50    0.44    --  105.91 102.00 142.00   50
  6  ω    -58.00  23.00   0.50    0.11    --  -47.28  57.00 120.00  162
  7  ω    -39.00  26.00   0.50    0.11    --  -47.28  38.00  60.00  130
  8  ω    -48.00 -22.00   0.50    0.44    --  -91.75  45.00   0.00   52
  9  ω    -47.00 -21.00   0.50    0.44    --  -91.75  45.00 -60.00   52
 10  ω    -48.00 -23.00   0.50    0.44    --  -91.75  45.00-120.00   50
 11  ω    -48.00 -21.00   0.50    0.44    --  -91.75  45.00-150.00   54
 12  ω    -14.00  11.00   0.50    0.11    --  -47.28  19.00-150.00   50
 13  ω    -48.00 -20.00   0.50    0.44    --  -91.75  45.00  90.00   56
 14  ω    -70.00  13.00   0.50    0.11    --  -47.28 102.00 142.00  166
 15  ω    -84.00 -43.00   0.50    0.44    --  -91.75 125.00 150.00   82
 16  ω    -74.00 -49.00   0.50    0.44    --  -91.75 102.00 142.00   50
 17  ω   -163.00 -78.00   0.50    0.44    --  -91.75 -15.00  30.00  170
 18  ω   -108.00 -82.00   0.50    0.11    --  -47.28 -19.00  90.00   52
 19  ω   -120.00 -76.00   0.50    0.44    --  -91.75 -61.00 150.00   88
 20  ω   -161.00-127.00   0.50    0.44    --  -91.75 -61.00 150.00   68
 21  ω   -160.00 -71.00   0.50    0.44    --  -91.75 -77.00 120.00  178
 22  ω   -164.00 -79.00   0.50    0.44    --  -91.75 -15.00   0.00  170
 23  ω   -138.00-111.00   0.50    0.44    --  -91.75-102.00  39.00   54
 24  ω   -119.00 -86.00   0.50    0.11    --  -47.28-125.00 150.00   66
 25  ω   -119.00 -91.00   0.50    0.11    --  -47.28-125.00  90.00   56
 26  ω   -118.00 -83.00   0.50    0.11    --  -47.28-125.00-120.00   70
 27  ω   -118.00 -87.00   0.50    0.11    --  -47.28-125.00-150.00   62
 28  ω     34.00  63.00   0.50    0.44    --  105.91 -94.00 -60.00   58
 29  ω     60.00 111.00   0.50    0.44    --  105.91-125.00-180.00  102
 30  ω     36.00 111.00   0.50    0.44    --  105.91-125.00 -90.00  150
 31  ω     83.00 110.00   0.50    0.44    --  105.91-125.00 -60.00   54
 32  ω     43.00 112.00   0.50    0.44    --  105.91-125.00  30.00  138
 33  ω     51.00 104.00   0.50    0.44    --  105.91-125.00  60.00  106
 34  ω     33.00  77.00   0.50    0.44    --  105.91 -94.00  60.00   88
 35  ω     81.00 106.00   0.50    0.44    --  105.91 -94.00  60.00   50
 36  ω     64.00 106.00   0.50    0.44    --  105.91-102.00  39.00   84
 37  ω     44.00 106.00   0.50    0.44    --  105.91 -94.00  90.00  124
 38  ω      9.00  70.00   0.50    0.11    --   47.28-102.00  39.00  122
 39  ω     74.00  99.00   0.50    0.44    --  105.91 -94.00 -60.00   50
 40  ω     42.00  73.00   0.50    0.44    --  105.91 -61.00 -90.00   62
 41  ω     35.00  63.00   0.50    0.44    --  105.91 -61.00 -60.00   56
 42  ω     49.00  74.00   0.50    0.44    --  105.91 -61.00 -30.00   50
;
_diffrn_oxdiff_digest_frames     
;
0106e17d3e74f56483180527d34abb82e2037126cc9
;
_diffrn_oxdiff_digest_hkl        
;
01d2fa598c6f1b9eacb9bc5f2c405cdc1a4689
;
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'C35 H34 P2 Li1 Se1 O1'
_chemical_oxdiff_usercomment     'vapor diffudion thf-hex'








####################################################################### 
# 
# 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_PD-499-3
_database_code_depnum_ccdc_archive 'CCDC 2362608'
loop_
_audit_author_name
_audit_author_address
'Kai-Stephan Feichtner'
;Ruhr Universitaet Bochum
Germany
;
_audit_update_record             
;
2024-07-31 deposited with the CCDC.	2024-08-01 downloaded from the CCDC.
;
#

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H66 Li2 N6 O2 P2 Se2'
_chemical_formula_sum            'C46 H66 Li2 N6 O2 P2 Se2'
_chemical_formula_weight         968.78
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'
N N 0.0311 0.0180 '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'
Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

#

_cell_length_a                   23.8320(7)
_cell_length_b                   9.4158(2)
_cell_length_c                   11.2461(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.328(3)
_cell_angle_gamma                90
_cell_volume                     2455.63(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7456
_cell_measurement_theta_min      4.8620
_cell_measurement_theta_max      75.3410
_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_F_000             1008
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    2.818
_shelx_estimated_absorpt_T_min   0.539
_shelx_estimated_absorpt_T_max   0.786
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.423
_exptl_absorpt_correction_T_max  0.694
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            13004
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.812
_diffrn_reflns_theta_max         76.898
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_point_group_measured_fraction_full 0.955
_reflns_number_total             4663
_reflns_number_gt                4394
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.750
_reflns_Friedel_fraction_max     0.820
_reflns_Friedel_fraction_full    0.904
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT (G.M. Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1285P)²+3.5312P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1766 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4663
_refine_ls_number_parameters     276
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0571
_refine_ls_wR_factor_ref         0.1781
_refine_ls_wR_factor_gt          0.1530
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.33738(7) 0.52103(19) 0.74786(15) 0.0305(4) Uani 1 1 d . . . . .
O1 O 0.4543(2) 0.5825(6) 0.5452(5) 0.0342(10) Uani 1 1 d . . . . .
N1 N 0.4765(3) 0.8070(8) 0.2667(6) 0.0397(14) Uani 1 1 d . . . . .
C1 C 0.3904(3) 0.4947(8) 0.6712(7) 0.0382(16) Uani 1 1 d . . . . .
Li1 Li 0.4592(5) 0.6144(13) 0.3661(11) 0.032(2) Uani 1 1 d . . . . .
N2 N 0.3681(3) 0.6733(6) 0.2825(6) 0.0349(13) Uani 1 1 d . . . . .
C2 C 0.4212(3) 0.5452(7) 0.6081(6) 0.0315(14) Uani 1 1 d . . . . .
N3 N 0.4358(3) 0.4194(8) 0.2642(7) 0.0456(16) Uani 1 1 d . . . . .
C3 C 0.2694(3) 0.5233(9) 0.6323(7) 0.0369(14) Uani 1 1 d . . . . .
C4 C 0.2635(4) 0.4411(10) 0.5269(8) 0.0430(18) Uani 1 1 d . . . . .
H4 H 0.294220 0.380648 0.517953 0.052 Uiso 1 1 calc R U . . .
C5 C 0.2146(4) 0.4464(11) 0.4370(8) 0.050(2) Uani 1 1 d . . . . .
H5 H 0.211784 0.392461 0.364457 0.059 Uiso 1 1 calc R U . . .
C6 C 0.1683(4) 0.5315(11) 0.4510(10) 0.058(2) Uani 1 1 d . . . . .
H6 H 0.134289 0.536904 0.387519 0.070 Uiso 1 1 calc R U . . .
C7 C 0.1725(4) 0.6065(10) 0.5567(11) 0.056(2) Uani 1 1 d . . . . .
H7 H 0.140375 0.659589 0.568479 0.067 Uiso 1 1 calc R U . . .
C8 C 0.2227(4) 0.6060(10) 0.6461(9) 0.0476(18) Uani 1 1 d . . . . .
H8 H 0.225608 0.662165 0.717462 0.057 Uiso 1 1 calc R U . . .
C9 C 0.3333(3) 0.3585(9) 0.8345(7) 0.0368(15) Uani 1 1 d . . . . .
C10 C 0.3678(3) 0.2408(8) 0.8229(7) 0.0374(16) Uani 1 1 d . . . . .
H10 H 0.394385 0.245908 0.771851 0.045 Uiso 1 1 calc R U . . .
C11 C 0.3628(4) 0.1182(9) 0.8859(8) 0.0448(18) Uani 1 1 d . . . . .
H11 H 0.386851 0.039338 0.879746 0.054 Uiso 1 1 calc R U . . .
C12 C 0.3228(4) 0.1084(9) 0.9588(8) 0.0447(18) Uani 1 1 d . . . . .
H12 H 0.318603 0.022001 0.999488 0.054 Uiso 1 1 calc R U . . .
C13 C 0.2893(3) 0.2251(9) 0.9714(7) 0.0412(18) Uani 1 1 d . . . . .
H13 H 0.262518 0.219540 1.022099 0.049 Uiso 1 1 calc R U . . .
C14 C 0.2949(3) 0.3502(9) 0.9101(7) 0.0388(16) Uani 1 1 d . . . . .
H14 H 0.272339 0.430580 0.919953 0.047 Uiso 1 1 calc R U . . .
C15 C 0.4622(5) 0.3018(11) 0.3413(11) 0.061(2) Uani 1 1 d . . . . .
H15A H 0.454536 0.212781 0.295250 0.092 Uiso 1 1 calc R U . . .
H15B H 0.445924 0.296504 0.413601 0.092 Uiso 1 1 calc R U . . .
H15C H 0.503946 0.317017 0.366848 0.092 Uiso 1 1 calc R U . . .
C16 C 0.4475(5) 0.4031(14) 0.1451(10) 0.067(3) Uani 1 1 d . . . . .
H16A H 0.432390 0.311560 0.110324 0.100 Uiso 1 1 calc R U . . .
H16B H 0.489198 0.406629 0.151937 0.100 Uiso 1 1 calc R U . . .
H16C H 0.428776 0.480092 0.091714 0.100 Uiso 1 1 calc R U . . .
C17 C 0.3726(4) 0.4180(11) 0.2601(9) 0.053(2) Uani 1 1 d . . . . .
H17A H 0.354507 0.336404 0.210026 0.064 Uiso 1 1 calc R U . . .
H17B H 0.366980 0.404574 0.343898 0.064 Uiso 1 1 calc R U . . .
C18 C 0.3434(4) 0.5501(10) 0.2085(9) 0.0480(19) Uani 1 1 d . . . . .
H18A H 0.347829 0.562639 0.123718 0.058 Uiso 1 1 calc R U . . .
H18B H 0.301751 0.543366 0.206189 0.058 Uiso 1 1 calc R U . . .
C19 C 0.3359(3) 0.7057(13) 0.3767(7) 0.0448(16) Uani 1 1 d . . . . .
H19A H 0.296697 0.736080 0.337061 0.067 Uiso 1 1 calc R U . . .
H19B H 0.355487 0.781871 0.429685 0.067 Uiso 1 1 calc R U . . .
H19C H 0.334037 0.620515 0.425724 0.067 Uiso 1 1 calc R U . . .
C20 C 0.3692(3) 0.8019(9) 0.2080(7) 0.0409(17) Uani 1 1 d . . . . .
H20A H 0.334527 0.859753 0.207638 0.049 Uiso 1 1 calc R U . . .
H20B H 0.368056 0.773537 0.122647 0.049 Uiso 1 1 calc R U . . .
C21 C 0.4225(4) 0.8906(9) 0.2561(9) 0.0477(19) Uani 1 1 d . . . . .
H21A H 0.422797 0.971966 0.200486 0.057 Uiso 1 1 calc R U . . .
H21B H 0.421224 0.928853 0.337371 0.057 Uiso 1 1 calc R U . . .
C22 C 0.4858(5) 0.7747(12) 0.1465(10) 0.058(2) Uani 1 1 d . . . . .
H22A H 0.454581 0.713518 0.102437 0.088 Uiso 1 1 calc R U . . .
H22B H 0.522767 0.725741 0.155130 0.088 Uiso 1 1 calc R U . . .
H22C H 0.486225 0.863170 0.100779 0.088 Uiso 1 1 calc R U . . .
C23 C 0.5247(5) 0.8925(12) 0.3311(10) 0.059(2) Uani 1 1 d . . . . .
H23A H 0.560647 0.839261 0.337967 0.089 Uiso 1 1 calc R U . . .
H23B H 0.519558 0.915165 0.412932 0.089 Uiso 1 1 calc R U . . .
H23C H 0.526421 0.980618 0.285724 0.089 Uiso 1 1 calc R U . . .
Se1 Se 0.34436(3) 0.70274(8) 0.86346(6) 0.0377(3) 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 1.704(7) . ?
P1 C9 1.828(8) . ?
P1 C3 1.829(8) . ?
P1 Se1 2.1320(18) . ?
O1 C2 1.225(8) . ?
O1 Li1 2.066(13) . ?
O1 Li1 2.095(14) 2_656 ?
N1 C22 1.451(12) . ?
N1 C23 1.452(12) . ?
N1 C21 1.488(11) . ?
N1 Li1 2.218(14) . ?
C1 C2 1.229(10) . ?
Li1 N3 2.169(13) . ?
N2 C18 1.469(10) . ?
N2 C20 1.476(10) . ?
N2 C19 1.477(8) . ?
N3 C16 1.438(13) . ?
N3 C15 1.457(14) . ?
N3 C17 1.498(12) . ?
C3 C8 1.396(11) . ?
C3 C4 1.396(12) . ?
C4 C5 1.356(13) . ?
C4 H4 0.9500 . ?
C5 C6 1.402(15) . ?
C5 H5 0.9500 . ?
C6 C7 1.367(16) . ?
C6 H6 0.9500 . ?
C7 C8 1.373(13) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C14 1.388(10) . ?
C9 C10 1.403(11) . ?
C10 C11 1.373(11) . ?
C10 H10 0.9500 . ?
C11 C12 1.396(12) . ?
C11 H11 0.9500 . ?
C12 C13 1.385(13) . ?
C12 H12 0.9500 . ?
C13 C14 1.386(12) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.477(13) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.512(13) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 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 C9 106.5(4) . . ?
C1 P1 C3 106.3(4) . . ?
C9 P1 C3 104.0(4) . . ?
C1 P1 Se1 117.6(3) . . ?
C9 P1 Se1 110.7(2) . . ?
C3 P1 Se1 110.8(3) . . ?
C2 O1 Li1 142.4(6) . . ?
C2 O1 Li1 117.4(6) . 2_656 ?
Li1 O1 Li1 99.9(5) . 2_656 ?
C22 N1 C23 107.9(7) . . ?
C22 N1 C21 110.5(7) . . ?
C23 N1 C21 108.5(8) . . ?
C22 N1 Li1 112.6(7) . . ?
C23 N1 Li1 114.8(7) . . ?
C21 N1 Li1 102.4(6) . . ?
C2 C1 P1 148.0(7) . . ?
O1 Li1 O1 77.7(5) . 2_656 ?
O1 Li1 N3 109.1(6) . . ?
O1 Li1 N3 103.6(6) 2_656 . ?
O1 Li1 N1 132.0(6) . . ?
O1 Li1 N1 94.6(5) 2_656 . ?
N3 Li1 N1 118.7(6) . . ?
C18 N2 C20 112.5(7) . . ?
C18 N2 C19 111.2(7) . . ?
C20 N2 C19 108.6(7) . . ?
C18 N2 Li1 105.5(5) . . ?
C20 N2 Li1 107.5(5) . . ?
C19 N2 Li1 111.5(5) . . ?
O1 C2 C1 173.7(8) . . ?
C16 N3 C15 108.9(8) . . ?
C16 N3 C17 112.3(8) . . ?
C15 N3 C17 107.8(8) . . ?
C16 N3 Li1 120.1(8) . . ?
C15 N3 Li1 107.8(6) . . ?
C17 N3 Li1 99.1(6) . . ?
C8 C3 C4 118.6(8) . . ?
C8 C3 P1 121.7(6) . . ?
C4 C3 P1 119.7(6) . . ?
C5 C4 C3 120.8(8) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 120.1(9) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C7 C6 C5 119.4(8) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C6 C7 C8 120.9(9) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 H7 119.6 . . ?
C7 C8 C3 120.1(9) . . ?
C7 C8 H8 119.9 . . ?
C3 C8 H8 119.9 . . ?
C14 C9 C10 119.6(7) . . ?
C14 C9 P1 119.8(6) . . ?
C10 C9 P1 120.5(5) . . ?
C11 C10 C9 119.6(7) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C10 C11 C12 120.6(8) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C13 C12 C11 119.7(8) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 C14 119.9(7) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 C9 120.4(8) . . ?
C13 C14 H14 119.8 . . ?
C9 C14 H14 119.8 . . ?
N3 C15 H15A 109.5 . . ?
N3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N3 C16 H16A 109.5 . . ?
N3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 N3 112.5(8) . . ?
C18 C17 H17A 109.1 . . ?
N3 C17 H17A 109.1 . . ?
C18 C17 H17B 109.1 . . ?
N3 C17 H17B 109.1 . . ?
H17A C17 H17B 107.8 . . ?
N2 C18 C17 110.6(7) . . ?
N2 C18 H18A 109.5 . . ?
C17 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
N2 C19 H19A 109.5 . . ?
N2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N2 C20 C21 111.9(6) . . ?
N2 C20 H20A 109.2 . . ?
C21 C20 H20A 109.2 . . ?
N2 C20 H20B 109.2 . . ?
C21 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
N1 C21 C20 112.1(7) . . ?
N1 C21 H21A 109.2 . . ?
C20 C21 H21A 109.2 . . ?
N1 C21 H21B 109.2 . . ?
C20 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
N1 C22 H22A 109.5 . . ?
N1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N1 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N1 C23 H23A 109.5 . . ?
N1 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N1 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 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
C9 P1 C1 C2 -171.2(13) . . . . ?
C3 P1 C1 C2 78.4(13) . . . . ?
Se1 P1 C1 C2 -46.5(14) . . . . ?
C1 P1 C3 C8 -148.0(7) . . . . ?
C9 P1 C3 C8 99.8(7) . . . . ?
Se1 P1 C3 C8 -19.2(7) . . . . ?
C1 P1 C3 C4 31.6(8) . . . . ?
C9 P1 C3 C4 -80.6(7) . . . . ?
Se1 P1 C3 C4 160.5(6) . . . . ?
C8 C3 C4 C5 3.1(13) . . . . ?
P1 C3 C4 C5 -176.6(6) . . . . ?
C3 C4 C5 C6 -2.2(13) . . . . ?
C4 C5 C6 C7 -1.2(14) . . . . ?
C5 C6 C7 C8 3.8(15) . . . . ?
C6 C7 C8 C3 -2.9(14) . . . . ?
C4 C3 C8 C7 -0.5(13) . . . . ?
P1 C3 C8 C7 179.1(7) . . . . ?
C1 P1 C9 C14 177.8(6) . . . . ?
C3 P1 C9 C14 -70.2(7) . . . . ?
Se1 P1 C9 C14 48.9(7) . . . . ?
C1 P1 C9 C10 -3.8(7) . . . . ?
C3 P1 C9 C10 108.3(7) . . . . ?
Se1 P1 C9 C10 -132.6(6) . . . . ?
C14 C9 C10 C11 0.5(12) . . . . ?
P1 C9 C10 C11 -178.0(7) . . . . ?
C9 C10 C11 C12 1.6(13) . . . . ?
C10 C11 C12 C13 -2.5(14) . . . . ?
C11 C12 C13 C14 1.1(13) . . . . ?
C12 C13 C14 C9 1.0(12) . . . . ?
C10 C9 C14 C13 -1.8(12) . . . . ?
P1 C9 C14 C13 176.7(6) . . . . ?
C16 N3 C17 C18 -73.2(10) . . . . ?
C15 N3 C17 C18 166.9(8) . . . . ?
Li1 N3 C17 C18 54.8(9) . . . . ?
C20 N2 C18 C17 145.3(7) . . . . ?
C19 N2 C18 C17 -92.6(9) . . . . ?
Li1 N2 C18 C17 28.4(9) . . . . ?
N3 C17 C18 N2 -60.3(10) . . . . ?
C18 N2 C20 C21 -143.6(7) . . . . ?
C19 N2 C20 C21 92.9(7) . . . . ?
Li1 N2 C20 C21 -27.9(8) . . . . ?
C22 N1 C21 C20 70.9(9) . . . . ?
C23 N1 C21 C20 -171.0(7) . . . . ?
Li1 N1 C21 C20 -49.3(8) . . . . ?
N2 C20 C21 N1 55.2(9) . . . . ?

#

_refine_diff_density_max         1.970
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.124
######### additional information out of the cif_od #######  
_audit_creation_date             2024-07-29
_cell_oxdiff_length_a            23.8364(10)
_cell_oxdiff_length_b            9.4161(3)
_cell_oxdiff_length_c            11.2436(3)
_cell_oxdiff_angle_alpha         89.983(2)
_cell_oxdiff_angle_beta          103.328(3)
_cell_oxdiff_angle_gamma         89.982(3)
_cell_oxdiff_volume              2455.63(13)
_cell_oxdiff_measurement_reflns_used 7456
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0883
-3 2 -6 0.0662
0 2 -7 0.0678
-2 -4 -5 0.0828
4 -4 4 0.0645
-2 -3 7 0.0775
10 -1 4 0.0378
-11 -1 6 0.0963
-12 3 5 0.0981
-3 6 3 0.1218
-12 -4 3 0.1272
-13 2 -2 0.0838
-14 3 1 0.1030
6 0 6 0.0425
-6 0 -6 0.0443
3 3 6 0.0467
-14 2 4 0.0935
0 6 0 0.1287
15 0 -4 0.0742

#

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
-0.0014 -0.9993 -0.0000 -0.0019 0.1476 -0.0703
-3.3762 1.9731 -6.1724 -0.9411 -0.2796 0.1901
0.2312 1.8978 -6.7743 -0.9035 -0.1685 0.3941
-2.4221 -4.4165 -4.5208 -0.6987 0.6626 -0.2698
4.4274 -4.4480 3.9426 0.6700 0.7066 -0.2275
-1.7615 -2.6389 6.5451 0.8206 0.2431 -0.5171
9.9363 -0.5992 4.3183 0.9098 0.2704 0.3148
-11.2539 -1.1655 5.9055 0.4239 -0.2030 -0.8827
-11.9665 2.6678 4.5656 0.2267 -0.7663 -0.6012
-2.9059 5.6367 2.7177 0.2818 -0.9484 0.1453
-11.6747 -3.5803 3.3722 0.0633 0.1830 -0.9811
-13.2955 1.6854 -1.6117 -0.6531 -0.5577 -0.5123
-13.9683 2.6244 1.3808 -0.2695 -0.7602 -0.5911
6.1569 -0.1052 5.8447 0.9921 0.0786 0.0974
-6.1087 0.1151 -5.8592 -0.9925 -0.0786 -0.0936
3.2197 2.8091 5.7832 0.8925 -0.4248 0.1519
-14.1478 1.5098 3.8155 0.0513 -0.6382 -0.7682
0.3208 6.1014 0.3616 0.0710 -0.8991 0.4319
14.6751 0.2791 -3.8229 -0.0315 0.3872 0.9214

#

_oxdiff_exptl_absorpt_empirical_full_min 0.530
_oxdiff_exptl_absorpt_empirical_full_max 2.191
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_environment      N~2~
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0329946000
_diffrn_orient_matrix_UB_12      0.0018979000
_diffrn_orient_matrix_UB_13      0.1350276000
_diffrn_orient_matrix_UB_21      0.0251163000
_diffrn_orient_matrix_UB_22      -0.1477543000
_diffrn_orient_matrix_UB_23      -0.0156663000
_diffrn_orient_matrix_UB_31      0.0518850000
_diffrn_orient_matrix_UB_32      0.0702360000
_diffrn_orient_matrix_UB_33      -0.0367312000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -118.00 -33.00   0.50    1.30    --  -46.90 -51.00 144.00  170
  2  ω     75.00 119.00   0.50    1.30    --   46.90  51.00 -69.00   88
  3  ω      0.00  26.00   0.50    1.30    --   46.90 -51.00 144.00   52
  4  ω     29.00  56.00   0.50    1.30    --   46.90 -51.00 144.00   54
  5  ω    -50.00 -25.00   0.50    5.50    --  -91.75  51.00 -69.00   50
  6  ω   -162.00 -79.00   0.50    5.50    --  -91.75 -51.00 144.00  166
  7  ω    149.00 175.00   0.50    5.50    --  105.91  51.00 -69.00   52
  8  ω     34.00  60.00   0.50    5.50    --  105.91 -51.00 144.00   52
  9  ω   -119.00 -93.00   0.50    1.30    --  -46.90-125.00   0.00   52
 10  ω    -54.00  25.00   0.50    1.30    --  -46.90  51.00 -69.00  158
 11  ω   -119.00 -73.00   0.50    1.30    --  -46.90-125.00  90.00   92
 12  ω   -112.00 -85.00   0.50    1.30    --  -46.90-125.00 120.00   54
 13  ω    -72.00 -13.00   0.50    1.30    --  -46.90 125.00 -30.00  118
 14  ω     56.00  85.00   0.50    1.30    --   46.90-125.00   0.00   58
 15  ω    -48.00 -23.00   0.50    5.50    --  -91.75  45.00  30.00   50
 16  ω    -46.00 -21.00   0.50    5.50    --  -91.75  45.00   0.00   50
 17  ω    -68.00 -37.00   0.50    5.50    --  -91.75  61.00 -90.00   62
 18  ω   -163.00 -85.00   0.50    5.50    --  -91.75 -45.00  30.00  156
 19  ω    -58.00 -24.00   0.50    5.50    --  -91.75  61.00  90.00   68
 20  ω    -67.00 -20.00   0.50    5.50    --  -91.75  61.00 120.00   94
 21  ω    -48.00 -21.00   0.50    5.50    --  -91.75  45.00 120.00   54
 22  ω     35.00  65.00   0.50    5.50    --  105.91 -94.00  30.00   60
 23  ω     93.00 141.00   0.50    5.50    --  105.91  30.00 -60.00   96
 24  ω     33.00 106.00   0.50    5.50    --  105.91 -94.00   0.00  146
 25  ω     76.00 104.00   0.50    5.50    --  105.91 -77.00 120.00   56
 26  ω     55.00 107.00   0.50    5.50    --  105.91-104.00 164.24  104
 27  ω     95.00 171.00   0.50    5.50    --  105.91  45.00-150.00  152
 28  ω     71.00  97.00   0.50    5.50    --  105.91-125.00 -90.00   52
 29  ω     54.00 111.00   0.50    5.50    --  105.91-125.00   0.00  114
 30  ω     48.00  89.00   0.50    5.50    --  105.91 -94.00  90.00   82
 31  ω     42.00  87.00   0.50    5.50    --  105.91 -94.00-120.00   90
 32  ω     95.00 155.00   0.50    5.50    --  105.91  77.00 -60.00  120
 33  ω     77.00 102.00   0.50    5.50    --  105.91 -77.00-120.00   50
 34  ω     34.00  62.00   0.50    5.50    --  105.91 -77.00-120.00   56
 35  ω     95.00 122.00   0.50    5.50    --  105.91 125.00  30.00   54
 36  ω     69.00 102.00   0.50    5.50    --  105.91 -94.00  30.00   66
 37  ω     38.00 111.00   0.50    5.50    --  105.91-125.00-180.00  146
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'C92 H132 Li4 N12 O4 P4 Se4'
_chemical_oxdiff_usercomment     'vapor diffusion tol-thf/hex in freezer'








####################################################################### 
# 
# 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_PD-447_auto_a
_database_code_depnum_ccdc_archive 'CCDC 2362607'
loop_
_audit_author_name
_audit_author_address
'Kai-Stephan Feichtner'
;Ruhr Universitaet Bochum
Germany
;
_audit_update_record             
;
2024-07-31 deposited with the CCDC.	2024-08-01 downloaded from the CCDC.
;
#

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C70 H66 Li2 O2 P4 S2'
_chemical_formula_sum            'C70 H66 Li2 O2 P4 S2'
_chemical_formula_weight         1141.10
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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

#

_cell_length_a                   14.7042(2)
_cell_length_b                   11.10570(10)
_cell_length_c                   18.8325(2)
_cell_angle_alpha                90
_cell_angle_beta                 106.0010(10)
_cell_angle_gamma                90
_cell_volume                     2956.21(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    21114
_cell_measurement_theta_min      4.6560
_cell_measurement_theta_max      76.4420
_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_F_000             1200
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    2.193
_shelx_estimated_absorpt_T_min   0.506
_shelx_estimated_absorpt_T_max   0.844
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.257
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            35590
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.127
_diffrn_reflns_theta_max         67.997
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5382
_reflns_number_gt                4961
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0524P)²+1.9154P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5382
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0922
_refine_ls_wR_factor_gt          0.0900
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.38430(3) 0.54020(3) 0.41395(2) 0.01799(11) Uani 1 1 d . . . . .
P1 P 0.29199(3) 0.56700(3) 0.47510(2) 0.01438(11) Uani 1 1 d . . . . .
O1 O 0.53622(9) 0.77432(11) 0.55332(7) 0.0268(3) Uani 1 1 d . . . . .
C1 C 0.34861(11) 0.59265(14) 0.56367(8) 0.0171(3) Uani 1 1 d . . . . .
Li1 Li 0.4816(2) 0.6142(3) 0.54078(16) 0.0231(6) Uani 1 1 d . . . . .
P2 P 0.31785(3) 0.63227(3) 0.63832(2) 0.01461(11) Uani 1 1 d . . . . .
C2 C 0.20903(11) 0.43956(14) 0.45690(9) 0.0173(3) Uani 1 1 d . . . . .
C3 C 0.20329(12) 0.36391(14) 0.51426(9) 0.0200(3) Uani 1 1 d . . . . .
H3 H 0.243607 0.376917 0.562566 0.024 Uiso 1 1 calc R U . . .
C4 C 0.13897(13) 0.26942(15) 0.50143(10) 0.0259(4) Uani 1 1 d . . . . .
H4 H 0.135493 0.218429 0.541100 0.031 Uiso 1 1 calc R U . . .
C5 C 0.08005(13) 0.24887(16) 0.43159(11) 0.0295(4) Uani 1 1 d . . . . .
H5 H 0.035820 0.184486 0.423232 0.035 Uiso 1 1 calc R U . . .
C6 C 0.08589(13) 0.32315(17) 0.37346(11) 0.0293(4) Uani 1 1 d . . . . .
H6 H 0.045764 0.309314 0.325192 0.035 Uiso 1 1 calc R U . . .
C7 C 0.15046(12) 0.41763(16) 0.38605(10) 0.0235(4) Uani 1 1 d . . . . .
H7 H 0.154722 0.467575 0.346137 0.028 Uiso 1 1 calc R U . . .
C8 C 0.21260(11) 0.68910(14) 0.42979(8) 0.0162(3) Uani 1 1 d . . . . .
C9 C 0.23942(11) 0.77382(14) 0.38481(9) 0.0183(3) Uani 1 1 d . . . . .
H9 H 0.298389 0.765517 0.373793 0.022 Uiso 1 1 calc R U . . .
C10 C 0.18057(12) 0.87054(15) 0.35588(9) 0.0216(3) Uani 1 1 d . . . . .
H10 H 0.199270 0.927171 0.324803 0.026 Uiso 1 1 calc R U . . .
C11 C 0.09503(12) 0.88456(16) 0.37216(10) 0.0241(4) Uani 1 1 d . . . . .
H11 H 0.055011 0.950663 0.352468 0.029 Uiso 1 1 calc R U . . .
C12 C 0.06806(12) 0.80126(16) 0.41753(10) 0.0250(4) Uani 1 1 d . . . . .
H12 H 0.009676 0.810964 0.429294 0.030 Uiso 1 1 calc R U . . .
C13 C 0.12589(11) 0.70405(15) 0.44573(9) 0.0206(3) Uani 1 1 d . . . . .
H13 H 0.106409 0.647026 0.476176 0.025 Uiso 1 1 calc R U . . .
C14 C 0.25478(11) 0.77489(14) 0.63833(9) 0.0169(3) Uani 1 1 d . . . . .
C15 C 0.20611(11) 0.80092(15) 0.69092(9) 0.0197(3) Uani 1 1 d . . . . .
H15 H 0.205151 0.743538 0.728119 0.024 Uiso 1 1 calc R U . . .
C16 C 0.15941(12) 0.90975(16) 0.68899(9) 0.0227(4) Uani 1 1 d . . . . .
H16 H 0.126945 0.926886 0.724996 0.027 Uiso 1 1 calc R U . . .
C17 C 0.15996(12) 0.99407(15) 0.63439(10) 0.0231(4) Uani 1 1 d . . . . .
H17 H 0.127992 1.068731 0.633052 0.028 Uiso 1 1 calc R U . . .
C18 C 0.20745(12) 0.96843(15) 0.58195(9) 0.0216(3) Uani 1 1 d . . . . .
H18 H 0.207344 1.025437 0.544320 0.026 Uiso 1 1 calc R U . . .
C19 C 0.25517(11) 0.85998(14) 0.58410(9) 0.0184(3) Uani 1 1 d . . . . .
H19 H 0.288255 0.843753 0.548366 0.022 Uiso 1 1 calc R U . . .
C20 C 0.42444(11) 0.64656(14) 0.71565(8) 0.0163(3) Uani 1 1 d . . . . .
C21 C 0.43351(12) 0.72908(14) 0.77320(9) 0.0187(3) Uani 1 1 d . . . . .
H21 H 0.382353 0.781202 0.773404 0.022 Uiso 1 1 calc R U . . .
C22 C 0.51674(12) 0.73546(15) 0.83007(9) 0.0217(3) Uani 1 1 d . . . . .
H22 H 0.522445 0.792300 0.868748 0.026 Uiso 1 1 calc R U . . .
C23 C 0.59152(12) 0.65920(15) 0.83062(9) 0.0222(3) Uani 1 1 d . . . . .
H23 H 0.648258 0.663536 0.869750 0.027 Uiso 1 1 calc R U . . .
C24 C 0.58351(12) 0.57652(15) 0.77400(10) 0.0222(3) Uani 1 1 d . . . . .
H24 H 0.634685 0.524081 0.774377 0.027 Uiso 1 1 calc R U . . .
C25 C 0.50056(11) 0.57051(14) 0.71676(9) 0.0188(3) Uani 1 1 d . . . . .
H25 H 0.495501 0.514096 0.677939 0.023 Uiso 1 1 calc R U . . .
C26 C 0.24416(11) 0.52479(14) 0.67197(8) 0.0169(3) Uani 1 1 d . . . . .
C27 C 0.28714(12) 0.42496(15) 0.71322(9) 0.0211(3) Uani 1 1 d . . . . .
H27 H 0.354189 0.419405 0.729000 0.025 Uiso 1 1 calc R U . . .
C28 C 0.23258(13) 0.33398(16) 0.73128(10) 0.0268(4) Uani 1 1 d . . . . .
H28 H 0.262378 0.266693 0.759375 0.032 Uiso 1 1 calc R U . . .
C29 C 0.13472(14) 0.34132(17) 0.70833(10) 0.0286(4) Uani 1 1 d . . . . .
H29 H 0.097432 0.279237 0.720825 0.034 Uiso 1 1 calc R U . . .
C30 C 0.09123(13) 0.43956(17) 0.66704(10) 0.0264(4) Uani 1 1 d . . . . .
H30 H 0.024160 0.444509 0.651200 0.032 Uiso 1 1 calc R U . . .
C31 C 0.14560(12) 0.53053(15) 0.64888(9) 0.0207(3) Uani 1 1 d . . . . .
H31 H 0.115407 0.597310 0.620466 0.025 Uiso 1 1 calc R U . . .
C32 C 0.62985(14) 0.78794(17) 0.54478(12) 0.0311(4) Uani 1 1 d . . . . .
H32A H 0.633431 0.753098 0.497238 0.037 Uiso 1 1 calc R U . . .
H32B H 0.676892 0.747026 0.585484 0.037 Uiso 1 1 calc R U . . .
C33 C 0.64803(16) 0.9198(2) 0.54658(14) 0.0424(5) Uani 1 1 d . . . . .
H33A H 0.628983 0.954196 0.496148 0.051 Uiso 1 1 calc R U . . .
H33B H 0.715833 0.937308 0.569359 0.051 Uiso 1 1 calc R U . . .
C34 C 0.58673(14) 0.97086(16) 0.59391(11) 0.0282(4) Uani 1 1 d . . . . .
H34A H 0.626698 0.999437 0.642251 0.034 Uiso 1 1 calc R U . . .
H34B H 0.547223 1.038531 0.568317 0.034 Uiso 1 1 calc R U . . .
C35 C 0.52525(14) 0.86501(17) 0.60378(12) 0.0333(4) Uani 1 1 d . . . . .
H35A H 0.545999 0.834549 0.655134 0.040 Uiso 1 1 calc R U . . .
H35B H 0.458171 0.889960 0.592875 0.040 Uiso 1 1 calc R U . . .

#


#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 P1 2.0296(5) . ?
S1 Li1 2.558(3) . ?
S1 Li1 2.574(3) 3_666 ?
P1 C1 1.6705(16) . ?
P1 C2 1.8379(16) . ?
P1 C8 1.8386(16) . ?
P1 Li1 2.770(3) . ?
O1 C35 1.424(2) . ?
O1 C32 1.438(2) . ?
O1 Li1 1.939(3) . ?
C1 P2 1.6508(15) . ?
C1 Li1 2.128(3) . ?
P2 C20 1.8287(16) . ?
P2 C14 1.8355(16) . ?
P2 C26 1.8381(16) . ?
C2 C3 1.389(2) . ?
C2 C7 1.396(2) . ?
C3 C4 1.389(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.392(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.391(3) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.394(2) . ?
C8 C13 1.398(2) . ?
C9 C10 1.393(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.383(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.389(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.386(2) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C19 1.393(2) . ?
C14 C15 1.403(2) . ?
C15 C16 1.386(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.392(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.387(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.389(2) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.397(2) . ?
C20 C25 1.398(2) . ?
C21 C22 1.388(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.386(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.387(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.389(2) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C31 1.395(2) . ?
C26 C27 1.401(2) . ?
C27 C28 1.389(2) . ?
C27 H27 0.9500 . ?
C28 C29 1.386(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.389(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.388(2) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 C33 1.487(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.540(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.525(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 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 S1 Li1 73.28(6) . . ?
P1 S1 Li1 118.74(7) . 3_666 ?
Li1 S1 Li1 74.00(10) . 3_666 ?
C1 P1 C2 116.11(8) . . ?
C1 P1 C8 114.55(7) . . ?
C2 P1 C8 100.23(7) . . ?
C1 P1 S1 111.37(6) . . ?
C2 P1 S1 107.13(5) . . ?
C8 P1 S1 106.45(5) . . ?
C1 P1 Li1 50.12(8) . . ?
C2 P1 Li1 139.75(8) . . ?
C8 P1 Li1 119.99(8) . . ?
S1 P1 Li1 62.16(6) . . ?
C35 O1 C32 106.76(13) . . ?
C35 O1 Li1 127.64(14) . . ?
C32 O1 Li1 117.40(13) . . ?
P2 C1 P1 135.86(10) . . ?
P2 C1 Li1 128.70(12) . . ?
P1 C1 Li1 92.85(11) . . ?
O1 Li1 C1 116.81(14) . . ?
O1 Li1 S1 120.97(14) . . ?
C1 Li1 S1 81.06(10) . . ?
O1 Li1 S1 108.45(13) . 3_666 ?
C1 Li1 S1 121.39(13) . 3_666 ?
S1 Li1 S1 106.00(10) . 3_666 ?
C1 P2 C20 109.00(8) . . ?
C1 P2 C14 119.15(8) . . ?
C20 P2 C14 104.31(7) . . ?
C1 P2 C26 116.51(8) . . ?
C20 P2 C26 103.84(7) . . ?
C14 P2 C26 102.38(7) . . ?
C3 C2 C7 118.95(15) . . ?
C3 C2 P1 120.00(13) . . ?
C7 C2 P1 121.04(13) . . ?
C4 C3 C2 120.40(16) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C5 C4 C3 120.63(17) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 119.52(16) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C7 C6 C5 120.02(17) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C2 120.46(16) . . ?
C6 C7 H7 119.8 . . ?
C2 C7 H7 119.8 . . ?
C9 C8 C13 118.56(15) . . ?
C9 C8 P1 122.01(12) . . ?
C13 C8 P1 119.20(12) . . ?
C10 C9 C8 120.59(15) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C11 C10 C9 120.34(15) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C10 C11 C12 119.51(16) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C13 C12 C11 120.34(16) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C12 C13 C8 120.65(15) . . ?
C12 C13 H13 119.7 . . ?
C8 C13 H13 119.7 . . ?
C19 C14 C15 118.95(14) . . ?
C19 C14 P2 118.77(12) . . ?
C15 C14 P2 122.28(12) . . ?
C16 C15 C14 120.45(15) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C17 120.16(15) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 H16 119.9 . . ?
C18 C17 C16 119.61(15) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C17 C18 C19 120.45(16) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C18 C19 C14 120.37(15) . . ?
C18 C19 H19 119.8 . . ?
C14 C19 H19 119.8 . . ?
C21 C20 C25 118.69(15) . . ?
C21 C20 P2 123.52(12) . . ?
C25 C20 P2 117.80(12) . . ?
C22 C21 C20 120.47(15) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C23 C22 C21 120.24(15) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C22 C23 C24 119.98(15) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C23 C24 C25 119.91(15) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C20 120.71(15) . . ?
C24 C25 H25 119.6 . . ?
C20 C25 H25 119.6 . . ?
C31 C26 C27 118.70(15) . . ?
C31 C26 P2 121.56(12) . . ?
C27 C26 P2 119.11(12) . . ?
C28 C27 C26 120.58(16) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C29 C28 C27 120.05(17) . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C28 C29 C30 119.92(16) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C31 C30 C29 120.13(17) . . ?
C31 C30 H30 119.9 . . ?
C29 C30 H30 119.9 . . ?
C30 C31 C26 120.62(16) . . ?
C30 C31 H31 119.7 . . ?
C26 C31 H31 119.7 . . ?
O1 C32 C33 105.83(15) . . ?
O1 C32 H32A 110.6 . . ?
C33 C32 H32A 110.6 . . ?
O1 C32 H32B 110.6 . . ?
C33 C32 H32B 110.6 . . ?
H32A C32 H32B 108.7 . . ?
C32 C33 C34 104.23(16) . . ?
C32 C33 H33A 110.9 . . ?
C34 C33 H33A 110.9 . . ?
C32 C33 H33B 110.9 . . ?
C34 C33 H33B 110.9 . . ?
H33A C33 H33B 108.9 . . ?
C35 C34 C33 104.34(15) . . ?
C35 C34 H34A 110.9 . . ?
C33 C34 H34A 110.9 . . ?
C35 C34 H34B 110.9 . . ?
C33 C34 H34B 110.9 . . ?
H34A C34 H34B 108.9 . . ?
O1 C35 C34 106.48(14) . . ?
O1 C35 H35A 110.4 . . ?
C34 C35 H35A 110.4 . . ?
O1 C35 H35B 110.4 . . ?
C34 C35 H35B 110.4 . . ?
H35A C35 H35B 108.6 . . ?

#

_refine_diff_density_max         0.486
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.053
######### additional information out of the cif_od #######  
_audit_creation_date             2023-11-04
_cell_oxdiff_length_a            14.7103(3)
_cell_oxdiff_length_b            11.10116(14)
_cell_oxdiff_length_c            18.8310(2)
_cell_oxdiff_angle_alpha         89.9966(10)
_cell_oxdiff_angle_beta          105.9858(14)
_cell_oxdiff_angle_gamma         90.0217(12)
_cell_oxdiff_volume              2956.22(7)
_cell_oxdiff_measurement_reflns_used 21114
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
9 0 -8 0.0706
3 -7 2 0.0839
-8 4 4 0.0537
3 -6 3 0.0718
7 3 -10 0.1195
9 -1 1 0.0412
-9 0 -2 0.0253
-2 1 -11 0.0816

#

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
8.8151 0.4437 -7.5654 0.1541 0.6409 -0.7520
2.6677 -6.7497 1.5462 -0.1549 -0.6495 -0.7444
-7.8918 3.9425 4.3549 -0.0109 -0.0420 0.9991
3.1217 -6.3782 2.7952 -0.0181 -0.6735 -0.7390
6.5667 2.7856 -9.5343 0.0229 0.9159 -0.4007
8.9166 -1.2408 0.5441 0.5758 0.0466 -0.8163
-8.6453 0.2482 -1.9251 -0.7111 -0.0572 0.7008
-1.5525 1.3661 -10.8313 -0.7198 0.6820 0.1293

#

_oxdiff_exptl_absorpt_empirical_full_min 0.706
_oxdiff_exptl_absorpt_empirical_full_max 1.394
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_environment      N~2~
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_reflns_av_sigmaI/netI    0.0532
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0697169000
_diffrn_orient_matrix_UB_12      0.0653211000
_diffrn_orient_matrix_UB_13      0.0647005000
_diffrn_orient_matrix_UB_21      0.0213730000
_diffrn_orient_matrix_UB_22      0.0922151000
_diffrn_orient_matrix_UB_23      -0.0544018000
_diffrn_orient_matrix_UB_31      -0.0809359000
_diffrn_orient_matrix_UB_32      0.0805478000
_diffrn_orient_matrix_UB_33      0.0098196000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -83.00 -45.00   0.50    0.40    --  -47.03 120.00-178.00   76
  2  ω    -79.00 -53.00   0.50    0.40    --  -47.03 154.00 -19.00   52
  3  ω    -86.00 -53.00   0.50    0.40    --  -47.03-154.00 -59.00   66
  4  ω     32.00  82.00   0.50    0.40    --   47.03-120.00  98.00  100
  5  ω     70.00 111.00   0.50    0.40    --   47.03-154.00 -59.00   82
  6  ω    -76.00 -51.00   0.50    1.60    --  -91.75 120.00-178.00   50
  7  ω    -91.00 -66.00   0.50    1.60    --  -91.75 154.00 -19.00   50
  8  ω   -126.00 -98.00   0.50    1.60    --  -91.75-120.00  98.00   56
  9  ω    132.00 158.00   0.50    1.60    --  105.91 154.00 -19.00   52
 10  ω     78.00 125.00   0.50    1.60    --  105.91 154.00 -19.00   94
 11  ω     66.00  91.00   0.50    1.60    --  105.91-154.00 -59.00   50
 12  ω    100.00 164.00   0.50    1.60    --  105.91 120.00-178.00  128
 13  ω     79.00 110.00   0.50    1.60    --  105.91-120.00  98.00   62
 14  ω   -119.00 -24.00   0.50    0.40    --  -47.03 -77.00 -60.00  190
 15  ω   -116.00 -49.00   0.50    0.40    --  -47.03 -57.00 -30.00  134
 16  ω   -115.00 -79.00   0.50    0.40    --  -47.03-125.00 -90.00   72
 17  ω    -18.00  25.00   0.50    0.40    --  -47.03  19.00-120.00   86
 18  ω    -23.00  27.00   0.50    0.40    --  -47.03  19.00  90.00  100
 19  ω    -83.00 -58.00   0.50    1.60    --  -91.75-154.00 -59.00   50
 20  ω   -163.00 -81.00   0.50    1.60    --  -91.75 -30.00 150.00  164
 21  ω    -48.00 -21.00   0.50    1.60    --  -91.75  45.00-120.00   54
 22  ω    -48.00 -23.00   0.50    1.60    --  -91.75  45.00  60.00   50
 23  ω    -81.00 -25.00   0.50    1.60    --  -91.75 125.00 -30.00  112
 24  ω    -80.00 -30.00   0.50    1.60    --  -91.75 125.00 -60.00  100
 25  ω   -133.00 -86.00   0.50    1.60    --  -91.75-154.00 -59.00   94
 26  ω    -48.00 -22.00   0.50    1.60    --  -91.75  45.00 -30.00   52
 27  ω   -160.00 -96.00   0.50    1.60    --  -91.75 -61.00 120.00  128
 28  ω    -46.00 -21.00   0.50    1.60    --  -91.75  45.00   0.00   50
 29  ω     54.00 104.00   0.50    1.60    --  105.91 -94.00-150.00  100
 30  ω     45.00 110.00   0.50    1.60    --  105.91-125.00-150.00  130
 31  ω     34.00  95.00   0.50    1.60    --  105.91 -77.00  90.00  122
 32  ω     52.00 110.00   0.50    1.60    --  105.91-125.00  60.00  116
 33  ω     39.00  67.00   0.50    1.60    --  105.91 -61.00 120.00   56
 34  ω     84.00 171.00   0.50    1.60    --  105.91  77.00-120.00  174
 35  ω     40.00  72.00   0.50    1.60    --  105.91 -61.00 150.00   64
 36  ω    150.00 175.00   0.50    1.60    --  105.91  45.00  90.00   50
 37  ω     95.00 122.00   0.50    1.60    --  105.91  45.00  90.00   54
 38  ω     94.00 168.00   0.50    1.60    --  105.91  30.00   0.00  148
 39  ω     50.00 105.00   0.50    1.60    --  105.91 -97.00 -42.34  110
 40  ω     85.00 112.00   0.50    1.60    --  105.91-125.00-180.00   54
 41  ω     34.00 106.00   0.50    1.60    --  105.91-102.00 -83.84  144
 42  ω     42.00  71.00   0.50    1.60    --  105.91 -61.00  90.00   58
 43  ω     34.00  64.00   0.50    1.60    --  105.91 -94.00 -60.00   60
;
_diffrn_oxdiff_digest_frames     
;
01e699fa046379967cdf69fa035e84b5990379488e4
;
_diffrn_oxdiff_digest_hkl        
;
010ca92a1077c4c513c016c5dc176396b8a6e8
;
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'C35 H33 Li1 S1 O1 P2'
_chemical_oxdiff_usercomment     'vapor diffusion tol-thf/hex'








####################################################################### 
# 
# 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_SMO-225
_database_code_depnum_ccdc_archive 'CCDC 2362609'
loop_
_audit_author_name
_audit_author_address
'Kai-Stephan Feichtner'
;Ruhr Universitaet Bochum
Germany
;
_audit_update_record             
;
2024-07-31 deposited with the CCDC.	2024-08-01 downloaded from the CCDC.
;
#

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H36 Li2 O6 P2'
_chemical_formula_sum            'C36 H36 Li2 O6 P2'
_chemical_formula_weight         640.47
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'

#

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

#

_cell_length_a                   14.2502(3)
_cell_length_b                   15.4854(3)
_cell_length_c                   15.5126(3)
_cell_angle_alpha                90.527(2)
_cell_angle_beta                 91.990(2)
_cell_angle_gamma                100.300(2)
_cell_volume                     3365.56(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    14366
_cell_measurement_theta_min      6.3130
_cell_measurement_theta_max      75.9510
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_F_000             1344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.136
_exptl_absorpt_coefficient_mu    1.528
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_T_max  0.848
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            22471
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.851
_diffrn_reflns_theta_max         76.831
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             22471
_reflns_number_gt                20188
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT (G.M. Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0673P)²+7.1882P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         22471
_refine_ls_number_parameters     830
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0660
_refine_ls_wR_factor_ref         0.2099
_refine_ls_wR_factor_gt          0.1834
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_restrained_S_all      1.157
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
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 . . . . .

#


#

_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 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_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_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 ?

#

_refine_diff_density_max         0.672
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.100
######### additional information out of the cif_od #######  
_audit_creation_date             2023-11-14
_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
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_
_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

#

_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
;
_diffrn_ambient_environment      N~2~
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_reflns_av_sigmaI/netI    0.0323
_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_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
;
_oxdiff_twin_items               2
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

#

_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)
;
_chemical_oxdiff_formula         'C72 H72 Li4 O12 P4'
_chemical_oxdiff_usercomment     'tHF toluene /pen'








