# Electronic Supplementary Material (ESI) 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 
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data_230220_yxf_a2
_database_code_depnum_ccdc_archive 'CCDC 2271317'
loop_
_audit_author_name
_audit_author_address
'Xiaofan Yang'
;Zhejiang University
China
;
_audit_update_record             
;
2024-03-31 deposited with the CCDC.	2024-04-04 downloaded from the CCDC.
;
_audit_creation_date             2024-03-31
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C28 H26 N3 O7 P2 U), 0.5(H4 O2), 2(C3 H6 O)'
_chemical_formula_sum            'C62 H66 N6 O17 P4 U2'
_chemical_formula_weight         1767.14
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0137 0.0067 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2543 0.3332 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -3.9641 10.8496 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   31.0258(11)
_cell_length_b                   12.8733(5)
_cell_length_c                   16.8307(6)
_cell_angle_alpha                90
_cell_angle_beta                 114.1570(10)
_cell_angle_gamma                90
_cell_volume                     6133.6(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      60.624
_cell_measurement_theta_min      2.842
_shelx_estimated_absorpt_T_max   0.570
_shelx_estimated_absorpt_T_min   0.338
_exptl_absorpt_coefficient_mu    12.167
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.5598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1018 before and 0.0843 after correction.
The Ratio of minimum to maximum transmission is 0.7445.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.114
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.052
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5502
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.902
_diffrn_reflns_theta_min         2.716
_diffrn_ambient_temperature      170.00
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           3.57
_diffrn_source_power             0.24954300000000001
_diffrn_source_target            Mo
_diffrn_source_voltage           69.9
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5299
_reflns_number_total             5502
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         3.308
_refine_diff_density_min         -2.140
_refine_diff_density_rms         0.218
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         5502
_refine_ls_number_restraints     96
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0470
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0334P)²+44.3724P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1121
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.50(2)
 0.50(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Restrained distances
 O11-C1G
 1.21 with sigma of 0.02
 C1G-C1H = C1G-C1I
 1.5 with sigma of 0.02
 O12-C1J
 1.21 with sigma of 0.02
 C1J-C1K = C1J-C1L
 1.5 with sigma of 0.02
 C1H-C1G = C1G-C1I
 1.52 with sigma of 0.02
 C1L-C1J = C1J-C1K
 1.52 with sigma of 0.02
 O12-C1J = O11-C1G
 1.2 with sigma of 0.005
 O11-C1H = O11-C1I
 2.38 with sigma of 0.04
 O12-C1K = O12-C1L
 2.38 with sigma of 0.04
 C1H-C1I
 2.564 with sigma of 0.04
 C1L-C1K
 2.564 with sigma of 0.04
 C1G-C1H \\sim C1G-C1I
 with sigma of 0.02
 C1H-O11 \\sim C1I-O11
 with sigma of 0.04
 C1J-C1K \\sim C1J-C1L
 with sigma of 0.02
 C1K-O12 \\sim C1L-O12
 with sigma of 0.04
4. Restrained planarity
 O11, C1G, C1H, C1I
 with sigma of 0.05
 O12, C1J, C1K, C1L
 with sigma of 0.05
5. Uiso/Uaniso restraints and constraints
O11 \\sim C1G \\sim C1H \\sim C1I: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C1G \\sim O11 \\sim C1H \\sim C1I: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
O12 \\sim C1J \\sim C1K \\sim C1L: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6. Rigid body (RIGU) restrains
 O11, C1G, C1H, C1I
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O12, C1J, C1K, C1L
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(O12)=Sof(C1J)=Sof(C1K)=Sof(H1KA)=Sof(H1KB)=Sof(H1KC)=Sof(C1L)=Sof(H1LA)=
 Sof(H1LB)=Sof(H1LC)=1-FVAR(1)
 Sof(O11)=Sof(C1G)=Sof(C1H)=Sof(H1HA)=Sof(H1HB)=Sof(H1HC)=Sof(C1I)=Sof(H1IA)=
 Sof(H1IB)=Sof(H1IC)=FVAR(1)
 Fixed Sof: H9A(0.5) H9B(0.5)
8.a Everything fixed:
 O9, H9A, H9B
8.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C21(H21A,H21B)
8.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C16(H16),
 C17(H17), C18(H18), C19(H19), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28)
8.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C22(H22A,H22B,H22C), C1H(H1HA,H1HB,H1HC), C1I(H1IA,H1IB,
 H1IC), C1K(H1KA,H1KB,H1KC), C1L(H1LA,H1LB,H1LC)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.72936(2) 0.41764(2) 0.59623(2) 0.02844(11) Uani 1 1 d . . . . .
P1 P 0.84937(6) 0.48221(14) 0.72758(11) 0.0319(4) Uani 1 1 d . . . . .
P2 P 0.61697(6) 0.47073(16) 0.42277(12) 0.0364(4) Uani 1 1 d . . . . .
O1 O 0.80924(18) 0.4054(4) 0.6985(4) 0.0360(11) Uani 1 1 d . . . . .
O2 O 0.6521(2) 0.3981(5) 0.4875(4) 0.0468(13) Uani 1 1 d . . . . .
O6 O 0.7496(2) 0.3951(5) 0.5141(3) 0.0422(12) Uani 1 1 d . . . . .
O7 O 0.70863(18) 0.4488(4) 0.6765(3) 0.0369(11) Uani 1 1 d . . . . .
N1 N 0.7765(2) 0.6036(4) 0.6403(4) 0.0284(11) Uani 1 1 d . . . . .
N2 N 0.6847(2) 0.5978(5) 0.5197(4) 0.0331(13) Uani 1 1 d . . . . .
C1 C 0.8854(3) 0.4821(7) 0.8423(5) 0.0428(18) Uani 1 1 d . . . . .
H1A H 0.908058 0.540501 0.856710 0.051 Uiso 1 1 calc R U . . .
H1B H 0.865083 0.492740 0.874224 0.051 Uiso 1 1 calc R U . . .
C2 C 0.9127(4) 0.3794(9) 0.8721(6) 0.065(3) Uani 1 1 d . . . . .
H2A H 0.939790 0.379235 0.856219 0.098 Uiso 1 1 calc R U . . .
H2B H 0.891833 0.321040 0.843563 0.098 Uiso 1 1 calc R U . . .
H2C H 0.923922 0.372651 0.935370 0.098 Uiso 1 1 calc R U . . .
C3 C 0.8862(2) 0.4677(6) 0.6704(4) 0.0355(15) Uani 1 1 d . . . . .
C4 C 0.8724(3) 0.3986(7) 0.5995(5) 0.0414(17) Uani 1 1 d . . . . .
H4 H 0.844223 0.358963 0.583434 0.050 Uiso 1 1 calc R U . . .
C5 C 0.9008(3) 0.3893(9) 0.5526(6) 0.054(2) Uani 1 1 d . . . . .
H5 H 0.892081 0.342462 0.504956 0.065 Uiso 1 1 calc R U . . .
C6 C 0.9410(3) 0.4472(9) 0.5757(6) 0.055(2) Uani 1 1 d . . . . .
H6 H 0.960046 0.440085 0.543960 0.066 Uiso 1 1 calc R U . . .
C7 C 0.9543(3) 0.5166(8) 0.6448(6) 0.054(2) Uani 1 1 d . . . . .
H7 H 0.981977 0.557377 0.659395 0.065 Uiso 1 1 calc R U . . .
C8 C 0.9272(2) 0.5265(7) 0.6927(5) 0.0422(17) Uani 1 1 d . . . . .
H8 H 0.936627 0.573240 0.740551 0.051 Uiso 1 1 calc R U . . .
C9 C 0.8217(2) 0.6069(6) 0.6974(4) 0.0292(13) Uani 1 1 d . . . . .
C10 C 0.8453(3) 0.7015(6) 0.7341(5) 0.0353(15) Uani 1 1 d . . . . .
H10 H 0.877128 0.700953 0.776162 0.042 Uiso 1 1 calc R U . . .
C11 C 0.8216(3) 0.7920(7) 0.7080(5) 0.0422(17) Uani 1 1 d . . . . .
H11 H 0.836951 0.855708 0.731622 0.051 Uiso 1 1 calc R U . . .
C12 C 0.7746(3) 0.7926(6) 0.6464(5) 0.0351(15) Uani 1 1 d . . . . .
C13 C 0.7530(2) 0.6941(5) 0.6138(4) 0.0282(13) Uani 1 1 d . . . . .
C14 C 0.7057(2) 0.6927(6) 0.5514(4) 0.0308(14) Uani 1 1 d . . . . .
C15 C 0.6805(3) 0.7875(6) 0.5221(5) 0.0369(16) Uani 1 1 d . . . . .
C16 C 0.7039(3) 0.8826(7) 0.5579(5) 0.0434(18) Uani 1 1 d . . . . .
H16 H 0.687251 0.946119 0.539409 0.052 Uiso 1 1 calc R U . . .
C17 C 0.7483(3) 0.8848(6) 0.6163(5) 0.0397(16) Uani 1 1 d . . . . .
H17 H 0.762738 0.949823 0.638385 0.048 Uiso 1 1 calc R U . . .
C18 C 0.6334(3) 0.7839(7) 0.4616(5) 0.0431(18) Uani 1 1 d . . . . .
H18 H 0.615548 0.845980 0.443241 0.052 Uiso 1 1 calc R U . . .
C19 C 0.6132(3) 0.6891(7) 0.4290(5) 0.0423(17) Uani 1 1 d . . . . .
H19 H 0.581676 0.684751 0.386232 0.051 Uiso 1 1 calc R U . . .
C20 C 0.6407(3) 0.5986(6) 0.4608(5) 0.0337(15) Uani 1 1 d . . . . .
C21 C 0.5575(3) 0.4605(8) 0.4169(5) 0.050(2) Uani 1 1 d . . . . .
H21A H 0.558120 0.473478 0.475282 0.060 Uiso 1 1 calc R U . . .
H21B H 0.537481 0.514476 0.376897 0.060 Uiso 1 1 calc R U . . .
C22 C 0.5365(4) 0.3564(9) 0.3857(11) 0.092(4) Uani 1 1 d . . . . .
H22A H 0.503992 0.354861 0.381350 0.138 Uiso 1 1 calc R U . . .
H22B H 0.555209 0.303011 0.426859 0.138 Uiso 1 1 calc R U . . .
H22C H 0.536314 0.342680 0.328282 0.138 Uiso 1 1 calc R U . . .
C23 C 0.6144(2) 0.4528(6) 0.3157(5) 0.0373(15) Uani 1 1 d . . . . .
C24 C 0.5804(3) 0.5032(7) 0.2447(5) 0.0462(19) Uani 1 1 d . . . . .
H24 H 0.558691 0.548928 0.253321 0.055 Uiso 1 1 calc R U . . .
C25 C 0.5780(3) 0.4878(9) 0.1625(6) 0.056(2) Uani 1 1 d . . . . .
H25 H 0.554378 0.521634 0.114011 0.067 Uiso 1 1 calc R U . . .
C26 C 0.6103(4) 0.4224(8) 0.1512(7) 0.061(3) Uani 1 1 d . . . . .
H26 H 0.608409 0.409995 0.094228 0.073 Uiso 1 1 calc R U . . .
C27 C 0.6453(3) 0.3746(9) 0.2216(6) 0.056(2) Uani 1 1 d . . . . .
H27 H 0.667893 0.331386 0.213148 0.067 Uiso 1 1 calc R U . . .
C28 C 0.6474(3) 0.3897(7) 0.3037(6) 0.0468(19) Uani 1 1 d . . . . .
H28 H 0.671493 0.357032 0.352259 0.056 Uiso 1 1 calc R U . . .
O3 O 0.75839(19) 0.2483(4) 0.6748(4) 0.0459(13) Uani 1 1 d . . . . .
O4 O 0.6888(2) 0.2438(4) 0.5769(4) 0.0475(14) Uani 1 1 d . . . . .
O5 O 0.7172(2) 0.1068(4) 0.6560(4) 0.0427(12) Uani 1 1 d . . . . .
N3 N 0.7213(2) 0.1963(5) 0.6369(4) 0.0340(13) Uani 1 1 d . . . . .
O9 O 0.500000 0.665110 0.250000 0.050 Uani 1 2 d S T P . .
H9A H 0.483860 0.701090 0.272370 0.075 Uiso 0.5 1 d . U P A -1
H9B H 0.528440 0.685300 0.259440 0.075 Uiso 0.5 1 d . U P B -1
O11 O 0.9595(4) 0.7252(11) 0.8282(8) 0.058(3) Uani 0.514(17) 1 d D U P C 1
C1G C 0.9783(5) 0.7328(10) 0.9056(8) 0.060(3) Uani 0.514(17) 1 d D U P C 1
C1H C 1.0038(8) 0.8267(13) 0.9428(16) 0.060(3) Uani 0.514(17) 1 d D U P C 1
H1HA H 1.011722 0.828187 1.005410 0.091 Uiso 0.514(17) 1 calc R U P C 1
H1HB H 0.984196 0.887033 0.914847 0.091 Uiso 0.514(17) 1 calc R U P C 1
H1HC H 1.032973 0.828929 0.933333 0.091 Uiso 0.514(17) 1 calc R U P C 1
C1I C 0.9733(6) 0.6478(13) 0.9557(11) 0.062(3) Uani 0.514(17) 1 d D U P C 1
H1IA H 0.941679 0.617734 0.926380 0.093 Uiso 0.514(17) 1 calc R U P C 1
H1IB H 0.977748 0.672521 1.013628 0.093 Uiso 0.514(17) 1 calc R U P C 1
H1IC H 0.997097 0.594775 0.961549 0.093 Uiso 0.514(17) 1 calc R U P C 1
O12 O 1.0107(6) 0.7936(14) 0.9477(11) 0.079(4) Uani 0.486(17) 1 d D U P C 2
C1J C 0.9737(5) 0.7495(12) 0.9143(10) 0.079(4) Uani 0.486(17) 1 d D U P C 2
C1K C 0.9327(6) 0.7651(18) 0.9341(14) 0.078(4) Uani 0.486(17) 1 d D U P C 2
H1KA H 0.942848 0.768321 0.997322 0.117 Uiso 0.486(17) 1 calc R U P C 2
H1KB H 0.910638 0.707246 0.910383 0.117 Uiso 0.486(17) 1 calc R U P C 2
H1KC H 0.917101 0.830360 0.907799 0.117 Uiso 0.486(17) 1 calc R U P C 2
C1L C 0.9688(9) 0.6748(18) 0.8466(14) 0.080(4) Uani 0.486(17) 1 d D U P C 2
H1LA H 0.937374 0.681456 0.799024 0.120 Uiso 0.486(17) 1 calc R U P C 2
H1LB H 0.972803 0.604385 0.870641 0.120 Uiso 0.486(17) 1 calc R U P C 2
H1LC H 0.992948 0.688145 0.824287 0.120 Uiso 0.486(17) 1 calc R U P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 2.375(5) . ?
U1 O2 2.360(6) . ?
U1 O6 1.760(5) . ?
U1 O7 1.764(5) . ?
U1 N1 2.745(6) . ?
U1 N2 2.738(6) . ?
U1 O3 2.518(5) . ?
U1 O4 2.521(5) . ?
P1 O1 1.506(5) . ?
P1 C1 1.792(7) . ?
P1 C3 1.781(7) . ?
P1 C9 1.794(7) . ?
P2 O2 1.509(6) . ?
P2 C20 1.810(8) . ?
P2 C21 1.810(8) . ?
P2 C23 1.786(8) . ?
N1 C9 1.336(9) . ?
N1 C13 1.350(9) . ?
N2 C14 1.384(10) . ?
N2 C20 1.320(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.539(13) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.406(11) . ?
C3 C8 1.394(11) . ?
C4 H4 0.9500 . ?
C4 C5 1.410(12) . ?
C5 H5 0.9500 . ?
C5 C6 1.365(15) . ?
C6 H6 0.9500 . ?
C6 C7 1.389(15) . ?
C7 H7 0.9500 . ?
C7 C8 1.386(12) . ?
C8 H8 0.9500 . ?
C9 C10 1.425(11) . ?
C10 H10 0.9500 . ?
C10 C11 1.351(12) . ?
C11 H11 0.9500 . ?
C11 C12 1.403(12) . ?
C12 C13 1.433(10) . ?
C12 C17 1.411(11) . ?
C13 C14 1.413(10) . ?
C14 C15 1.425(10) . ?
C15 C16 1.425(12) . ?
C15 C18 1.398(11) . ?
C16 H16 0.9500 . ?
C16 C17 1.325(13) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C18 C19 1.379(13) . ?
C19 H19 0.9500 . ?
C19 C20 1.412(11) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.490(16) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.389(11) . ?
C23 C28 1.385(12) . ?
C24 H24 0.9500 . ?
C24 C25 1.368(12) . ?
C25 H25 0.9500 . ?
C25 C26 1.382(14) . ?
C26 H26 0.9500 . ?
C26 C27 1.382(14) . ?
C27 H27 0.9500 . ?
C27 C28 1.369(13) . ?
C28 H28 0.9500 . ?
O3 N3 1.256(8) . ?
O4 N3 1.254(8) . ?
O5 N3 1.218(8) . ?
O9 H9A 0.8726 . ?
O9 H9B 0.8698 . ?
O11 C1G 1.194(5) . ?
C1G C1H 1.441(11) . ?
C1G C1I 1.428(11) . ?
C1H H1HA 0.9800 . ?
C1H H1HB 0.9800 . ?
C1H H1HC 0.9800 . ?
C1I H1IA 0.9800 . ?
C1I H1IB 0.9800 . ?
C1I H1IC 0.9800 . ?
O12 C1J 1.194(5) . ?
C1J C1K 1.455(11) . ?
C1J C1L 1.450(11) . ?
C1K H1KA 0.9800 . ?
C1K H1KB 0.9800 . ?
C1K H1KC 0.9800 . ?
C1L H1LA 0.9800 . ?
C1L H1LB 0.9800 . ?
C1L H1LC 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
O1 U1 N1 65.11(17) . . ?
O1 U1 N2 125.05(17) . . ?
O1 U1 O3 61.24(17) . . ?
O1 U1 O4 110.60(17) . . ?
O2 U1 O1 169.4(2) . . ?
O2 U1 N1 124.25(18) . . ?
O2 U1 N2 64.39(19) . . ?
O2 U1 O3 110.26(18) . . ?
O2 U1 O4 60.70(18) . . ?
O6 U1 O1 87.5(2) . . ?
O6 U1 O2 87.1(2) . . ?
O6 U1 O7 176.3(2) . . ?
O6 U1 N1 92.0(2) . . ?
O6 U1 N2 92.6(2) . . ?
O6 U1 O3 96.0(2) . . ?
O6 U1 O4 94.1(2) . . ?
O7 U1 O1 93.4(2) . . ?
O7 U1 O2 92.6(2) . . ?
O7 U1 N1 85.2(2) . . ?
O7 U1 N2 84.0(2) . . ?
O7 U1 O3 87.6(2) . . ?
O7 U1 O4 88.9(2) . . ?
N2 U1 N1 59.97(18) . . ?
O3 U1 N1 125.22(17) . . ?
O3 U1 N2 169.73(18) . . ?
O3 U1 O4 49.57(17) . . ?
O4 U1 N1 172.42(18) . . ?
O4 U1 N2 124.16(18) . . ?
O1 P1 C1 114.7(4) . . ?
O1 P1 C3 112.6(3) . . ?
O1 P1 C9 105.0(3) . . ?
C1 P1 C9 108.7(4) . . ?
C3 P1 C1 109.1(4) . . ?
C3 P1 C9 106.3(3) . . ?
O2 P2 C20 103.9(3) . . ?
O2 P2 C21 114.3(4) . . ?
O2 P2 C23 111.7(4) . . ?
C20 P2 C21 110.1(4) . . ?
C23 P2 C20 108.6(4) . . ?
C23 P2 C21 108.2(4) . . ?
P1 O1 U1 132.1(3) . . ?
P2 O2 U1 134.2(3) . . ?
C9 N1 U1 120.5(5) . . ?
C9 N1 C13 118.4(6) . . ?
C13 N1 U1 120.5(4) . . ?
C14 N2 U1 119.9(4) . . ?
C20 N2 U1 121.9(5) . . ?
C20 N2 C14 117.5(6) . . ?
P1 C1 H1A 109.3 . . ?
P1 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
C2 C1 P1 111.6(6) . . ?
C2 C1 H1A 109.3 . . ?
C2 C1 H1B 109.3 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 P1 118.9(6) . . ?
C8 C3 P1 120.9(6) . . ?
C8 C3 C4 120.1(7) . . ?
C3 C4 H4 120.5 . . ?
C3 C4 C5 119.0(8) . . ?
C5 C4 H4 120.5 . . ?
C4 C5 H5 119.9 . . ?
C6 C5 C4 120.1(9) . . ?
C6 C5 H5 119.9 . . ?
C5 C6 H6 119.6 . . ?
C5 C6 C7 120.9(8) . . ?
C7 C6 H6 119.6 . . ?
C6 C7 H7 119.9 . . ?
C8 C7 C6 120.2(8) . . ?
C8 C7 H7 119.9 . . ?
C3 C8 H8 120.2 . . ?
C7 C8 C3 119.7(8) . . ?
C7 C8 H8 120.2 . . ?
N1 C9 P1 114.5(5) . . ?
N1 C9 C10 122.8(7) . . ?
C10 C9 P1 122.7(5) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 C9 118.7(7) . . ?
C11 C10 H10 120.7 . . ?
C10 C11 H11 119.7 . . ?
C10 C11 C12 120.6(7) . . ?
C12 C11 H11 119.7 . . ?
C11 C12 C13 117.3(7) . . ?
C11 C12 C17 122.9(7) . . ?
C17 C12 C13 119.8(7) . . ?
N1 C13 C12 122.2(6) . . ?
N1 C13 C14 119.4(6) . . ?
C14 C13 C12 118.4(6) . . ?
N2 C14 C13 118.7(6) . . ?
N2 C14 C15 121.1(6) . . ?
C13 C14 C15 120.1(7) . . ?
C14 C15 C16 118.5(7) . . ?
C18 C15 C14 119.0(7) . . ?
C18 C15 C16 122.5(7) . . ?
C15 C16 H16 119.1 . . ?
C17 C16 C15 121.9(7) . . ?
C17 C16 H16 119.1 . . ?
C12 C17 H17 119.3 . . ?
C16 C17 C12 121.3(7) . . ?
C16 C17 H17 119.3 . . ?
C15 C18 H18 120.4 . . ?
C19 C18 C15 119.3(7) . . ?
C19 C18 H18 120.4 . . ?
C18 C19 H19 120.9 . . ?
C18 C19 C20 118.3(7) . . ?
C20 C19 H19 120.9 . . ?
N2 C20 P2 113.9(5) . . ?
N2 C20 C19 124.7(7) . . ?
C19 C20 P2 121.4(6) . . ?
P2 C21 H21A 109.2 . . ?
P2 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
C22 C21 P2 112.0(7) . . ?
C22 C21 H21A 109.2 . . ?
C22 C21 H21B 109.2 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 P2 120.8(6) . . ?
C28 C23 P2 119.5(6) . . ?
C28 C23 C24 119.7(7) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 C23 120.7(8) . . ?
C25 C24 H24 119.6 . . ?
C24 C25 H25 120.5 . . ?
C24 C25 C26 119.0(8) . . ?
C26 C25 H25 120.5 . . ?
C25 C26 H26 119.6 . . ?
C25 C26 C27 120.9(9) . . ?
C27 C26 H26 119.6 . . ?
C26 C27 H27 120.1 . . ?
C28 C27 C26 119.9(9) . . ?
C28 C27 H27 120.1 . . ?
C23 C28 H28 120.1 . . ?
C27 C28 C23 119.8(8) . . ?
C27 C28 H28 120.1 . . ?
N3 O3 U1 97.9(4) . . ?
N3 O4 U1 97.8(4) . . ?
O4 N3 O3 114.6(6) . . ?
O5 N3 O3 122.9(6) . . ?
O5 N3 O4 122.6(6) . . ?
H9A O9 H9B 118.7 . . ?
O11 C1G C1H 118.6(14) . . ?
O11 C1G C1I 117.3(13) . . ?
C1I C1G C1H 124.1(14) . . ?
C1G C1H H1HA 109.5 . . ?
C1G C1H H1HB 109.5 . . ?
C1G C1H H1HC 109.5 . . ?
H1HA C1H H1HB 109.5 . . ?
H1HA C1H H1HC 109.5 . . ?
H1HB C1H H1HC 109.5 . . ?
C1G C1I H1IA 109.5 . . ?
C1G C1I H1IB 109.5 . . ?
C1G C1I H1IC 109.5 . . ?
H1IA C1I H1IB 109.5 . . ?
H1IA C1I H1IC 109.5 . . ?
H1IB C1I H1IC 109.5 . . ?
O12 C1J C1K 125.9(15) . . ?
O12 C1J C1L 117.3(14) . . ?
C1L C1J C1K 116.8(15) . . ?
C1J C1K H1KA 109.5 . . ?
C1J C1K H1KB 109.5 . . ?
C1J C1K H1KC 109.5 . . ?
H1KA C1K H1KB 109.5 . . ?
H1KA C1K H1KC 109.5 . . ?
H1KB C1K H1KC 109.5 . . ?
C1J C1L H1LA 109.5 . . ?
C1J C1L H1LB 109.5 . . ?
C1J C1L H1LC 109.5 . . ?
H1LA C1L H1LB 109.5 . . ?
H1LA C1L H1LC 109.5 . . ?
H1LB C1L H1LC 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
U1 N1 C9 P1 8.8(6) . . . . ?
U1 N1 C9 C10 -168.7(5) . . . . ?
U1 N1 C13 C12 169.9(5) . . . . ?
U1 N1 C13 C14 -10.5(7) . . . . ?
U1 N2 C14 C13 9.7(8) . . . . ?
U1 N2 C14 C15 -170.3(5) . . . . ?
U1 N2 C20 P2 -10.0(7) . . . . ?
U1 N2 C20 C19 169.6(6) . . . . ?
U1 O3 N3 O4 4.0(7) . . . . ?
U1 O3 N3 O5 -176.7(5) . . . . ?
U1 O4 N3 O3 -4.0(7) . . . . ?
U1 O4 N3 O5 176.7(5) . . . . ?
P1 C3 C4 C5 178.2(6) . . . . ?
P1 C3 C8 C7 -177.4(6) . . . . ?
P1 C9 C10 C11 -179.5(6) . . . . ?
P2 C23 C24 C25 -178.7(7) . . . . ?
P2 C23 C28 C27 179.2(8) . . . . ?
O1 P1 C1 C2 66.3(8) . . . . ?
O1 P1 C3 C4 7.5(7) . . . . ?
O1 P1 C3 C8 -175.1(6) . . . . ?
O1 P1 C9 N1 -15.7(5) . . . . ?
O1 P1 C9 C10 161.7(5) . . . . ?
O2 P2 C20 N2 13.4(6) . . . . ?
O2 P2 C20 C19 -166.2(6) . . . . ?
O2 P2 C21 C22 -63.7(9) . . . . ?
O2 P2 C23 C24 172.4(7) . . . . ?
O2 P2 C23 C28 -9.2(8) . . . . ?
N1 C9 C10 C11 -2.3(10) . . . . ?
N1 C13 C14 N2 0.5(9) . . . . ?
N1 C13 C14 C15 -179.5(6) . . . . ?
N2 C14 C15 C16 179.3(7) . . . . ?
N2 C14 C15 C18 1.3(10) . . . . ?
C1 P1 O1 U1 138.7(4) . . . . ?
C1 P1 C3 C4 136.0(6) . . . . ?
C1 P1 C3 C8 -46.6(7) . . . . ?
C1 P1 C9 N1 -138.9(5) . . . . ?
C1 P1 C9 C10 38.6(6) . . . . ?
C3 P1 O1 U1 -95.7(5) . . . . ?
C3 P1 C1 C2 -61.0(8) . . . . ?
C3 P1 C9 N1 103.8(5) . . . . ?
C3 P1 C9 C10 -78.8(6) . . . . ?
C3 C4 C5 C6 -0.6(13) . . . . ?
C4 C3 C8 C7 -0.1(11) . . . . ?
C4 C5 C6 C7 -0.4(14) . . . . ?
C5 C6 C7 C8 1.2(14) . . . . ?
C6 C7 C8 C3 -0.9(13) . . . . ?
C8 C3 C4 C5 0.8(12) . . . . ?
C9 P1 O1 U1 19.5(5) . . . . ?
C9 P1 C1 C2 -176.5(7) . . . . ?
C9 P1 C3 C4 -106.9(6) . . . . ?
C9 P1 C3 C8 70.4(7) . . . . ?
C9 N1 C13 C12 -1.5(9) . . . . ?
C9 N1 C13 C14 178.0(6) . . . . ?
C9 C10 C11 C12 0.4(11) . . . . ?
C10 C11 C12 C13 0.7(10) . . . . ?
C10 C11 C12 C17 -179.4(7) . . . . ?
C11 C12 C13 N1 -0.2(10) . . . . ?
C11 C12 C13 C14 -179.7(6) . . . . ?
C11 C12 C17 C16 179.9(8) . . . . ?
C12 C13 C14 N2 -179.9(6) . . . . ?
C12 C13 C14 C15 0.1(9) . . . . ?
C13 N1 C9 P1 -179.7(4) . . . . ?
C13 N1 C9 C10 2.8(9) . . . . ?
C13 C12 C17 C16 -0.3(11) . . . . ?
C13 C14 C15 C16 -0.7(10) . . . . ?
C13 C14 C15 C18 -178.7(6) . . . . ?
C14 N2 C20 P2 179.2(5) . . . . ?
C14 N2 C20 C19 -1.3(10) . . . . ?
C14 C15 C16 C17 0.9(12) . . . . ?
C14 C15 C18 C19 -2.8(11) . . . . ?
C15 C16 C17 C12 -0.4(13) . . . . ?
C15 C18 C19 C20 2.3(11) . . . . ?
C16 C15 C18 C19 179.2(7) . . . . ?
C17 C12 C13 N1 180.0(6) . . . . ?
C17 C12 C13 C14 0.4(9) . . . . ?
C18 C15 C16 C17 178.8(8) . . . . ?
C18 C19 C20 P2 179.3(6) . . . . ?
C18 C19 C20 N2 -0.3(12) . . . . ?
C20 P2 O2 U1 -13.9(6) . . . . ?
C20 P2 C21 C22 179.9(8) . . . . ?
C20 P2 C23 C24 -73.7(7) . . . . ?
C20 P2 C23 C28 104.8(7) . . . . ?
C20 N2 C14 C13 -179.2(6) . . . . ?
C20 N2 C14 C15 0.7(9) . . . . ?
C21 P2 O2 U1 -133.8(5) . . . . ?
C21 P2 C20 N2 136.2(6) . . . . ?
C21 P2 C20 C19 -43.4(7) . . . . ?
C21 P2 C23 C24 45.7(8) . . . . ?
C21 P2 C23 C28 -135.8(7) . . . . ?
C23 P2 O2 U1 102.9(5) . . . . ?
C23 P2 C20 N2 -105.6(6) . . . . ?
C23 P2 C20 C19 74.8(7) . . . . ?
C23 P2 C21 C22 61.5(9) . . . . ?
C23 C24 C25 C26 -1.0(15) . . . . ?
C24 C23 C28 C27 -2.3(14) . . . . ?
C24 C25 C26 C27 -1.4(16) . . . . ?
C25 C26 C27 C28 1.9(17) . . . . ?
C26 C27 C28 C23 0.0(16) . . . . ?
C28 C23 C24 C25 2.8(14) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.50(2)
2 0.50(2)

####################################################################### 
# 
# 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_230904_et_ph_rs
_database_code_depnum_ccdc_archive 'CCDC 2293650'
loop_
_audit_author_name
_audit_author_address
'Xiaofan Yang'
;Zhejiang University
China
;
_audit_update_record             
;
2023-09-07 deposited with the CCDC.	2024-04-04 downloaded from the CCDC.
;
_audit_creation_date             2023-09-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H26 N2 O2 P2'
_chemical_formula_sum            'C28 H26 N2 O2 P2'
_chemical_formula_weight         484.45
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0137 0.0067 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2543 0.3332 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.1143(4)
_cell_length_b                   28.2649(12)
_cell_length_c                   8.4249(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.202(2)
_cell_angle_gamma                90
_cell_volume                     2383.87(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9794
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      60.890
_cell_measurement_theta_min      4.075
_shelx_estimated_absorpt_T_max   0.919
_shelx_estimated_absorpt_T_min   0.809
_exptl_absorpt_coefficient_mu    1.232
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.6352
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1722 before and 0.1062 after correction.
The Ratio of minimum to maximum transmission is 0.8448.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            59219
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.891
_diffrn_reflns_theta_min         3.842
_diffrn_ambient_temperature      170.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'zju Bruker D8 Venture'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   ?
_diffrn_source_current           3.57
_diffrn_source_power             0.24954300000000001
_diffrn_source_voltage           69.9
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4903
_reflns_number_total             5466
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker Instrument Service vV6.2.14'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5466
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0387
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0480P)²+1.1381P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1009
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C21(H21A,H21B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C16(H16),
 C17(H17), C18(H18), C19(H19), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C22(H22A,H22B,H22C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.62026(4) 0.58040(2) 0.72328(4) 0.01954(10) Uani 1 1 d . . . . .
O1 O 0.71326(11) 0.56183(4) 0.86201(12) 0.0288(2) Uani 1 1 d . . . . .
N1 N 0.49348(12) 0.66306(4) 0.64901(14) 0.0209(2) Uani 1 1 d . . . . .
C1 C 0.67716(14) 0.56858(5) 0.53382(16) 0.0198(3) Uani 1 1 d . . . . .
P2 P 0.01859(4) 0.68307(2) 0.33298(5) 0.02410(10) Uani 1 1 d . . . . .
O2 O -0.08225(11) 0.70794(4) 0.21628(15) 0.0367(3) Uani 1 1 d . . . . .
N2 N 0.26374(12) 0.70297(4) 0.49363(14) 0.0224(2) Uani 1 1 d . . . . .
C2 C 0.78700(15) 0.53913(5) 0.53096(17) 0.0252(3) Uani 1 1 d . . . . .
H2 H 0.832224 0.526355 0.628105 0.030 Uiso 1 1 calc R U . . .
C3 C 0.83061(16) 0.52838(6) 0.38592(19) 0.0304(3) Uani 1 1 d . . . . .
H3 H 0.905144 0.508044 0.383926 0.037 Uiso 1 1 calc R U . . .
C4 C 0.76555(16) 0.54728(6) 0.24453(18) 0.0281(3) Uani 1 1 d . . . . .
H4 H 0.795474 0.539826 0.145607 0.034 Uiso 1 1 calc R U . . .
C5 C 0.65724(17) 0.57695(6) 0.24654(17) 0.0277(3) Uani 1 1 d . . . . .
H5 H 0.613351 0.590003 0.149143 0.033 Uiso 1 1 calc R U . . .
C6 C 0.61235(15) 0.58775(5) 0.39055(17) 0.0242(3) Uani 1 1 d . . . . .
H6 H 0.537775 0.608122 0.391710 0.029 Uiso 1 1 calc R U . . .
C7 C 0.45255(15) 0.55751(5) 0.70157(18) 0.0258(3) Uani 1 1 d . . . . .
H7A H 0.399510 0.572253 0.606530 0.031 Uiso 1 1 calc R U . . .
H7B H 0.455062 0.522995 0.682179 0.031 Uiso 1 1 calc R U . . .
C8 C 0.38343(19) 0.56656(7) 0.8476(2) 0.0415(4) Uani 1 1 d . . . . .
H8A H 0.290710 0.555579 0.825782 0.062 Uiso 1 1 calc R U . . .
H8B H 0.384778 0.600525 0.871047 0.062 Uiso 1 1 calc R U . . .
H8C H 0.430274 0.549397 0.939963 0.062 Uiso 1 1 calc R U . . .
C9 C 0.60317(14) 0.64441(5) 0.73205(16) 0.0209(3) Uani 1 1 d . . . . .
C10 C 0.70513(15) 0.67122(6) 0.82019(19) 0.0282(3) Uani 1 1 d . . . . .
H10 H 0.780006 0.656158 0.880389 0.034 Uiso 1 1 calc R U . . .
C11 C 0.69450(16) 0.71953(6) 0.8177(2) 0.0310(3) Uani 1 1 d . . . . .
H11 H 0.762650 0.738477 0.875340 0.037 Uiso 1 1 calc R U . . .
C12 C 0.58201(15) 0.74078(5) 0.72910(18) 0.0250(3) Uani 1 1 d . . . . .
C13 C 0.48194(14) 0.71092(5) 0.64888(16) 0.0202(3) Uani 1 1 d . . . . .
C14 C 0.36157(14) 0.73197(5) 0.56267(16) 0.0211(3) Uani 1 1 d . . . . .
C15 C 0.35004(15) 0.78186(5) 0.55566(18) 0.0245(3) Uani 1 1 d . . . . .
C16 C 0.45614(17) 0.81067(5) 0.6361(2) 0.0309(3) Uani 1 1 d . . . . .
H16 H 0.448307 0.844148 0.630713 0.037 Uiso 1 1 calc R U . . .
C17 C 0.56617(16) 0.79121(6) 0.7189(2) 0.0315(3) Uani 1 1 d . . . . .
H17 H 0.634477 0.811114 0.771461 0.038 Uiso 1 1 calc R U . . .
C18 C 0.23291(16) 0.80102(5) 0.47027(19) 0.0293(3) Uani 1 1 d . . . . .
H18 H 0.221930 0.834355 0.462140 0.035 Uiso 1 1 calc R U . . .
C19 C 0.13456(16) 0.77159(6) 0.39875(19) 0.0290(3) Uani 1 1 d . . . . .
H19 H 0.055019 0.784054 0.340037 0.035 Uiso 1 1 calc R U . . .
C20 C 0.15408(14) 0.72242(5) 0.41427(17) 0.0236(3) Uani 1 1 d . . . . .
C21 C -0.05117(16) 0.66234(6) 0.5069(2) 0.0328(4) Uani 1 1 d . . . . .
H21A H -0.075932 0.690323 0.566884 0.039 Uiso 1 1 calc R U . . .
H21B H -0.134584 0.644915 0.468739 0.039 Uiso 1 1 calc R U . . .
C22 C 0.03741(19) 0.63049(7) 0.6236(2) 0.0372(4) Uani 1 1 d . . . . .
H22A H 0.053629 0.600665 0.570207 0.056 Uiso 1 1 calc R U . . .
H22B H -0.007244 0.623961 0.717076 0.056 Uiso 1 1 calc R U . . .
H22C H 0.122754 0.646377 0.658312 0.056 Uiso 1 1 calc R U . . .
C23 C 0.08815(14) 0.63162(5) 0.24807(17) 0.0227(3) Uani 1 1 d . . . . .
C24 C 0.20854(15) 0.60961(6) 0.30931(19) 0.0274(3) Uani 1 1 d . . . . .
H24 H 0.264862 0.623227 0.397364 0.033 Uiso 1 1 calc R U . . .
C25 C 0.24542(16) 0.56789(6) 0.2412(2) 0.0307(3) Uani 1 1 d . . . . .
H25 H 0.327262 0.553032 0.282999 0.037 Uiso 1 1 calc R U . . .
C26 C 0.16409(16) 0.54757(6) 0.11250(18) 0.0295(3) Uani 1 1 d . . . . .
H26 H 0.189516 0.518686 0.067744 0.035 Uiso 1 1 calc R U . . .
C27 C 0.04587(17) 0.56953(6) 0.04967(18) 0.0310(3) Uani 1 1 d . . . . .
H27 H -0.009273 0.556020 -0.039568 0.037 Uiso 1 1 calc R U . . .
C28 C 0.00796(16) 0.61124(6) 0.11699(18) 0.0278(3) Uani 1 1 d . . . . .
H28 H -0.073410 0.626134 0.073583 0.033 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
P1 O1 1.4875(10) . ?
P1 C1 1.8035(14) . ?
P1 C7 1.8002(16) . ?
P1 C9 1.8200(15) . ?
N1 C9 1.3330(18) . ?
N1 C13 1.3578(19) . ?
C1 C2 1.391(2) . ?
C1 C6 1.3981(19) . ?
P2 O2 1.4882(11) . ?
P2 C20 1.8210(15) . ?
P2 C21 1.8118(17) . ?
P2 C23 1.8070(15) . ?
N2 C14 1.3510(18) . ?
N2 C20 1.3295(18) . ?
C2 H2 0.9500 . ?
C2 C3 1.391(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.383(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.382(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.389(2) . ?
C6 H6 0.9500 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.521(2) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.404(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.370(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.404(2) . ?
C12 C13 1.4136(19) . ?
C12 C17 1.436(2) . ?
C13 C14 1.4530(19) . ?
C14 C15 1.416(2) . ?
C15 C16 1.438(2) . ?
C15 C18 1.404(2) . ?
C16 H16 0.9500 . ?
C16 C17 1.344(2) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C18 C19 1.369(2) . ?
C19 H19 0.9500 . ?
C19 C20 1.407(2) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.526(2) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.399(2) . ?
C23 C28 1.398(2) . ?
C24 H24 0.9500 . ?
C24 C25 1.386(2) . ?
C25 H25 0.9500 . ?
C25 C26 1.388(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.384(2) . ?
C27 H27 0.9500 . ?
C27 C28 1.386(2) . ?
C28 H28 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 P1 C1 112.60(6) . . ?
O1 P1 C7 115.73(7) . . ?
O1 P1 C9 111.83(6) . . ?
C1 P1 C9 105.32(6) . . ?
C7 P1 C1 104.98(7) . . ?
C7 P1 C9 105.54(7) . . ?
C9 N1 C13 117.36(12) . . ?
C2 C1 P1 118.86(10) . . ?
C2 C1 C6 119.62(13) . . ?
C6 C1 P1 121.52(11) . . ?
O2 P2 C20 111.60(7) . . ?
O2 P2 C21 112.19(8) . . ?
O2 P2 C23 112.79(7) . . ?
C21 P2 C20 104.62(7) . . ?
C23 P2 C20 109.01(7) . . ?
C23 P2 C21 106.16(8) . . ?
C20 N2 C14 118.22(12) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 C1 120.01(14) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 120.05(15) . . ?
C4 C3 H3 120.0 . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120.29(14) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 119.9 . . ?
C4 C5 C6 120.18(14) . . ?
C6 C5 H5 119.9 . . ?
C1 C6 H6 120.1 . . ?
C5 C6 C1 119.84(14) . . ?
C5 C6 H6 120.1 . . ?
P1 C7 H7A 109.0 . . ?
P1 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C8 C7 P1 113.12(11) . . ?
C8 C7 H7A 109.0 . . ?
C8 C7 H7B 109.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 P1 116.65(10) . . ?
N1 C9 C10 123.89(13) . . ?
C10 C9 P1 119.43(11) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 C9 118.68(14) . . ?
C11 C10 H10 120.7 . . ?
C10 C11 H11 120.3 . . ?
C10 C11 C12 119.39(14) . . ?
C12 C11 H11 120.3 . . ?
C11 C12 C13 118.00(13) . . ?
C11 C12 C17 122.13(14) . . ?
C13 C12 C17 119.87(14) . . ?
N1 C13 C12 122.60(13) . . ?
N1 C13 C14 118.30(12) . . ?
C12 C13 C14 119.10(13) . . ?
N2 C14 C13 118.48(12) . . ?
N2 C14 C15 122.38(13) . . ?
C15 C14 C13 119.14(13) . . ?
C14 C15 C16 119.54(14) . . ?
C18 C15 C14 117.65(14) . . ?
C18 C15 C16 122.80(14) . . ?
C15 C16 H16 119.3 . . ?
C17 C16 C15 121.33(14) . . ?
C17 C16 H16 119.3 . . ?
C12 C17 H17 119.5 . . ?
C16 C17 C12 120.97(14) . . ?
C16 C17 H17 119.5 . . ?
C15 C18 H18 120.1 . . ?
C19 C18 C15 119.88(14) . . ?
C19 C18 H18 120.1 . . ?
C18 C19 H19 120.8 . . ?
C18 C19 C20 118.41(14) . . ?
C20 C19 H19 120.8 . . ?
N2 C20 P2 117.75(11) . . ?
N2 C20 C19 123.44(14) . . ?
C19 C20 P2 118.69(11) . . ?
P2 C21 H21A 108.1 . . ?
P2 C21 H21B 108.1 . . ?
H21A C21 H21B 107.3 . . ?
C22 C21 P2 116.81(12) . . ?
C22 C21 H21A 108.1 . . ?
C22 C21 H21B 108.1 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 P2 125.42(11) . . ?
C28 C23 P2 115.45(11) . . ?
C28 C23 C24 118.99(14) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 C23 119.82(14) . . ?
C25 C24 H24 120.1 . . ?
C24 C25 H25 119.6 . . ?
C24 C25 C26 120.73(15) . . ?
C26 C25 H25 119.6 . . ?
C25 C26 H26 120.1 . . ?
C27 C26 C25 119.77(15) . . ?
C27 C26 H26 120.1 . . ?
C26 C27 H27 120.0 . . ?
C26 C27 C28 119.97(14) . . ?
C28 C27 H27 120.0 . . ?
C23 C28 H28 119.6 . . ?
C27 C28 C23 120.71(14) . . ?
C27 C28 H28 119.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C1 C2 C3 178.20(12) . . . . ?
P1 C1 C6 C5 -178.50(12) . . . . ?
P1 C9 C10 C11 176.11(12) . . . . ?
O1 P1 C1 C2 8.39(14) . . . . ?
O1 P1 C1 C6 -172.53(11) . . . . ?
O1 P1 C7 C8 58.37(14) . . . . ?
O1 P1 C9 N1 -158.29(10) . . . . ?
O1 P1 C9 C10 23.34(14) . . . . ?
N1 C9 C10 C11 -2.1(2) . . . . ?
N1 C13 C14 N2 3.37(19) . . . . ?
N1 C13 C14 C15 -177.46(13) . . . . ?
C1 P1 C7 C8 -176.85(12) . . . . ?
C1 P1 C9 N1 79.10(12) . . . . ?
C1 P1 C9 C10 -99.27(12) . . . . ?
C1 C2 C3 C4 0.6(2) . . . . ?
P2 C23 C24 C25 174.40(13) . . . . ?
P2 C23 C28 C27 -174.92(12) . . . . ?
O2 P2 C20 N2 -166.47(11) . . . . ?
O2 P2 C20 C19 17.37(14) . . . . ?
O2 P2 C21 C22 171.83(12) . . . . ?
O2 P2 C23 C24 160.38(13) . . . . ?
O2 P2 C23 C28 -24.17(14) . . . . ?
N2 C14 C15 C16 178.00(14) . . . . ?
N2 C14 C15 C18 -1.4(2) . . . . ?
C2 C1 C6 C5 0.6(2) . . . . ?
C2 C3 C4 C5 0.1(2) . . . . ?
C3 C4 C5 C6 -0.4(2) . . . . ?
C4 C5 C6 C1 0.1(2) . . . . ?
C6 C1 C2 C3 -0.9(2) . . . . ?
C7 P1 C1 C2 -118.34(12) . . . . ?
C7 P1 C1 C6 60.74(13) . . . . ?
C7 P1 C9 N1 -31.65(12) . . . . ?
C7 P1 C9 C10 149.98(12) . . . . ?
C9 P1 C1 C2 130.51(12) . . . . ?
C9 P1 C1 C6 -50.41(13) . . . . ?
C9 P1 C7 C8 -65.85(14) . . . . ?
C9 N1 C13 C12 1.6(2) . . . . ?
C9 N1 C13 C14 -178.39(12) . . . . ?
C9 C10 C11 C12 0.7(2) . . . . ?
C10 C11 C12 C13 1.6(2) . . . . ?
C10 C11 C12 C17 -178.71(16) . . . . ?
C11 C12 C13 N1 -2.8(2) . . . . ?
C11 C12 C13 C14 177.10(13) . . . . ?
C11 C12 C17 C16 -178.54(16) . . . . ?
C12 C13 C14 N2 -176.58(13) . . . . ?
C12 C13 C14 C15 2.6(2) . . . . ?
C13 N1 C9 P1 -177.30(10) . . . . ?
C13 N1 C9 C10 1.0(2) . . . . ?
C13 C12 C17 C16 1.1(2) . . . . ?
C13 C14 C15 C16 -1.1(2) . . . . ?
C13 C14 C15 C18 179.48(13) . . . . ?
C14 N2 C20 P2 -176.09(10) . . . . ?
C14 N2 C20 C19 -0.1(2) . . . . ?
C14 C15 C16 C17 -0.3(2) . . . . ?
C14 C15 C18 C19 0.6(2) . . . . ?
C15 C16 C17 C12 0.4(3) . . . . ?
C15 C18 C19 C20 0.4(2) . . . . ?
C16 C15 C18 C19 -178.80(15) . . . . ?
C17 C12 C13 N1 177.46(14) . . . . ?
C17 C12 C13 C14 -2.6(2) . . . . ?
C18 C15 C16 C17 178.99(16) . . . . ?
C18 C19 C20 P2 175.28(12) . . . . ?
C18 C19 C20 N2 -0.6(2) . . . . ?
C20 P2 C21 C22 -67.03(14) . . . . ?
C20 P2 C23 C24 35.83(15) . . . . ?
C20 P2 C23 C28 -148.72(11) . . . . ?
C20 N2 C14 C13 -179.70(12) . . . . ?
C20 N2 C14 C15 1.2(2) . . . . ?
C21 P2 C20 N2 71.99(13) . . . . ?
C21 P2 C20 C19 -104.17(13) . . . . ?
C21 P2 C23 C24 -76.37(15) . . . . ?
C21 P2 C23 C28 99.08(12) . . . . ?
C23 P2 C20 N2 -41.22(13) . . . . ?
C23 P2 C20 C19 142.62(12) . . . . ?
C23 P2 C21 C22 48.20(14) . . . . ?
C23 C24 C25 C26 0.0(2) . . . . ?
C24 C23 C28 C27 0.8(2) . . . . ?
C24 C25 C26 C27 1.0(2) . . . . ?
C25 C26 C27 C28 -1.1(2) . . . . ?
C26 C27 C28 C23 0.2(2) . . . . ?
C28 C23 C24 C25 -0.9(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_230721_u_et_ph
_database_code_depnum_ccdc_archive 'CCDC 2293649'
loop_
_audit_author_name
_audit_author_address
'Xiaofan Yang'
;Zhejiang University
China
;
_audit_update_record             
;
2023-09-07 deposited with the CCDC.	2024-04-04 downloaded from the CCDC.
;
_audit_creation_date             2023-07-22
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C28 H26 N3 O7 P2 U), N4 O14 U'
_chemical_formula_sum            'C56 H52 N10 O28 P4 U3'
_chemical_formula_weight         2151.04
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0137 0.0067 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2543 0.3332 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -3.9641 10.8496 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   19.1125(8)
_cell_length_b                   10.6852(4)
_cell_length_c                   17.9947(7)
_cell_angle_alpha                90
_cell_angle_beta                 107.7160(10)
_cell_angle_gamma                90
_cell_volume                     3500.6(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      60.577
_cell_measurement_theta_min      4.173
_shelx_estimated_absorpt_T_max   0.652
_shelx_estimated_absorpt_T_min   0.408
_exptl_absorpt_coefficient_mu    15.608
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.3798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1640 before and 0.0939 after correction.
The Ratio of minimum to maximum transmission is 0.5051.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.041
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2036
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43861
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.835
_diffrn_reflns_theta_min         2.111
_diffrn_ambient_temperature      170.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'zju Bruker D8 Venture'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   ?
_diffrn_source_current           3.57
_diffrn_source_power             0.24954300000000001
_diffrn_source_voltage           69.9
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6499
_reflns_number_total             7954
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.14'
_computing_data_reduction        'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.231
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         7954
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0375
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0343P)²+3.3093P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0827
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C27(H27A,H27B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C16(H16),
 C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C28(H28A,H28B,H28C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.17767(2) 0.36230(2) 0.44148(2) 0.03733(7) Uani 1 1 d . . . . .
P1 P 0.12147(12) 0.1618(2) 0.27547(11) 0.0706(6) Uani 1 1 d . . . . .
P2 P 0.28999(8) 0.58347(13) 0.56971(8) 0.0364(3) Uani 1 1 d . . . . .
O1 O 0.1156(3) 0.2078(6) 0.3523(3) 0.0814(19) Uani 1 1 d . . . . .
O2 O 0.2334(2) 0.4805(3) 0.5552(2) 0.0387(9) Uani 1 1 d . . . . .
O3 O 0.1067(2) 0.3996(5) 0.5376(2) 0.0532(11) Uani 1 1 d . . . . .
O4 O 0.0460(3) 0.3012(7) 0.4358(3) 0.099(2) Uani 1 1 d . . . . .
O5 O -0.0098(3) 0.3617(6) 0.5177(3) 0.0731(16) Uani 1 1 d . . . . .
O6 O 0.1344(2) 0.4917(4) 0.3859(2) 0.0528(11) Uani 1 1 d . . . . .
O7 O 0.2245(3) 0.2351(4) 0.4951(2) 0.0535(11) Uani 1 1 d . . . . .
N1 N 0.2345(3) 0.3142(4) 0.3242(3) 0.0377(11) Uani 1 1 d . . . . .
N2 N 0.3017(2) 0.4794(4) 0.4400(3) 0.0327(10) Uani 1 1 d . . . . .
N3 N 0.0457(3) 0.3540(6) 0.4972(3) 0.0609(16) Uani 1 1 d . . . . .
C1 C 0.1340(5) -0.0021(8) 0.2744(4) 0.079(3) Uani 1 1 d . . . . .
C2 C 0.0992(6) -0.0776(10) 0.2113(5) 0.096(3) Uani 1 1 d . . . . .
H2 H 0.066825 -0.040928 0.165606 0.116 Uiso 1 1 calc R U . . .
C3 C 0.1108(7) -0.2033(11) 0.2138(7) 0.119(5) Uani 1 1 d . . . . .
H3 H 0.086031 -0.254128 0.170407 0.143 Uiso 1 1 calc R U . . .
C4 C 0.1580(9) -0.2560(10) 0.2784(7) 0.135(6) Uani 1 1 d . . . . .
H4 H 0.165225 -0.344042 0.280271 0.162 Uiso 1 1 calc R U . . .
C5 C 0.1961(9) -0.1823(11) 0.3426(6) 0.154(7) Uani 1 1 d . . . . .
H5 H 0.230354 -0.219276 0.386938 0.185 Uiso 1 1 calc R U . . .
C6 C 0.1830(8) -0.0562(10) 0.3400(6) 0.121(5) Uani 1 1 d . . . . .
H6 H 0.207529 -0.005264 0.383378 0.145 Uiso 1 1 calc R U . . .
C7 C 0.0446(5) 0.2074(13) 0.1954(5) 0.107(4) Uani 1 1 d . . . . .
H7A H 0.048902 0.169144 0.146849 0.129 Uiso 1 1 calc R U . . .
H7B H -0.001087 0.175701 0.203814 0.129 Uiso 1 1 calc R U . . .
C8 C 0.0396(5) 0.3522(13) 0.1857(6) 0.114(4) Uani 1 1 d . . . . .
H8A H -0.008773 0.375101 0.150563 0.170 Uiso 1 1 calc R U . . .
H8B H 0.077838 0.381356 0.163839 0.170 Uiso 1 1 calc R U . . .
H8C H 0.046758 0.391335 0.236772 0.170 Uiso 1 1 calc R U . . .
C9 C 0.2024(3) 0.2375(6) 0.2658(3) 0.0432(14) Uani 1 1 d . . . . .
C10 C 0.2297(4) 0.2101(6) 0.2033(3) 0.0449(14) Uani 1 1 d . . . . .
H10 H 0.204882 0.152419 0.163940 0.054 Uiso 1 1 calc R U . . .
C11 C 0.2916(3) 0.2672(6) 0.2005(3) 0.0418(13) Uani 1 1 d . . . . .
H11 H 0.310767 0.250641 0.158628 0.050 Uiso 1 1 calc R U . . .
C12 C 0.3278(3) 0.3517(5) 0.2599(3) 0.0401(13) Uani 1 1 d . . . . .
C13 C 0.2975(3) 0.3721(5) 0.3208(3) 0.0330(11) Uani 1 1 d . . . . .
C14 C 0.3319(3) 0.4575(5) 0.3821(3) 0.0347(12) Uani 1 1 d . . . . .
C15 C 0.3974(3) 0.5175(6) 0.3798(4) 0.0452(14) Uani 1 1 d . . . . .
C16 C 0.4266(4) 0.4951(7) 0.3172(5) 0.064(2) Uani 1 1 d . . . . .
H16 H 0.470044 0.536827 0.315826 0.077 Uiso 1 1 calc R U . . .
C17 C 0.3928(4) 0.4149(7) 0.2598(4) 0.0566(18) Uani 1 1 d . . . . .
H17 H 0.413017 0.400469 0.218368 0.068 Uiso 1 1 calc R U . . .
C18 C 0.4310(4) 0.5999(6) 0.4414(4) 0.0571(18) Uani 1 1 d . . . . .
H18 H 0.475475 0.640695 0.442460 0.069 Uiso 1 1 calc R U . . .
C19 C 0.4011(4) 0.6213(6) 0.4984(4) 0.0496(16) Uani 1 1 d . . . . .
H19 H 0.423952 0.677180 0.539718 0.060 Uiso 1 1 calc R U . . .
C20 C 0.3364(3) 0.5609(5) 0.4963(3) 0.0380(12) Uani 1 1 d . . . . .
C21 C 0.2476(3) 0.7353(5) 0.5576(3) 0.0343(12) Uani 1 1 d . . . . .
C22 C 0.1719(3) 0.7406(6) 0.5393(4) 0.0464(14) Uani 1 1 d . . . . .
H22 H 0.143659 0.665817 0.531015 0.056 Uiso 1 1 calc R U . . .
C23 C 0.1376(4) 0.8569(6) 0.5331(4) 0.0564(18) Uani 1 1 d . . . . .
H23 H 0.085763 0.861644 0.521840 0.068 Uiso 1 1 calc R U . . .
C24 C 0.1786(4) 0.9650(6) 0.5432(4) 0.0523(16) Uani 1 1 d . . . . .
H24 H 0.155069 1.044222 0.537998 0.063 Uiso 1 1 calc R U . . .
C25 C 0.2539(4) 0.9579(6) 0.5609(4) 0.0499(15) Uani 1 1 d . . . . .
H25 H 0.281851 1.032858 0.568193 0.060 Uiso 1 1 calc R U . . .
C26 C 0.2895(3) 0.8438(5) 0.5683(4) 0.0448(14) Uani 1 1 d . . . . .
H26 H 0.341448 0.839761 0.580266 0.054 Uiso 1 1 calc R U . . .
C27 C 0.3559(4) 0.5784(6) 0.6641(3) 0.0481(15) Uani 1 1 d . . . . .
H27A H 0.375530 0.492277 0.674626 0.058 Uiso 1 1 calc R U . . .
H27B H 0.397354 0.634621 0.665000 0.058 Uiso 1 1 calc R U . . .
C28 C 0.3233(4) 0.6178(6) 0.7285(4) 0.0609(19) Uani 1 1 d . . . . .
H28A H 0.302788 0.702287 0.717682 0.091 Uiso 1 1 calc R U . . .
H28B H 0.361984 0.617248 0.778915 0.091 Uiso 1 1 calc R U . . .
H28C H 0.284440 0.559123 0.730131 0.091 Uiso 1 1 calc R U . . .
U2 U 0.500000 0.000000 0.500000 0.04172(9) Uani 1 2 d S . P . .
O8 O 0.5243(2) 0.1361(4) 0.4036(2) 0.0479(10) Uani 1 1 d . . . . .
O9 O 0.4290(5) 0.0934(8) 0.3096(4) 0.153(4) Uani 1 1 d . . . . .
O10 O 0.5156(4) 0.1979(5) 0.2872(3) 0.0785(16) Uani 1 1 d . . . . .
O11 O 0.4330(2) 0.2080(4) 0.4844(3) 0.0518(11) Uani 1 1 d . . . . .
O12 O 0.4274(3) 0.0976(4) 0.5817(3) 0.0557(11) Uani 1 1 d . . . . .
O13 O 0.3905(3) 0.2926(5) 0.5728(3) 0.0657(13) Uani 1 1 d . . . . .
O14 O 0.4209(2) -0.0758(4) 0.4400(2) 0.0520(11) Uani 1 1 d . . . . .
N4 N 0.4874(4) 0.1421(5) 0.3302(3) 0.0613(17) Uani 1 1 d . . . . .
N5 N 0.4148(3) 0.2040(5) 0.5462(3) 0.0513(13) 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
U1 O1 2.356(4) . ?
U1 O2 2.365(4) . ?
U1 O3 2.533(4) . ?
U1 O4 2.571(5) . ?
U1 O6 1.758(4) . ?
U1 O7 1.747(4) . ?
U1 N1 2.701(4) . ?
U1 N2 2.687(4) . ?
U1 N3 2.986(6) . ?
P1 O1 1.503(4) . ?
P1 C1 1.768(9) . ?
P1 C7 1.785(11) . ?
P1 C9 1.800(6) . ?
P2 O2 1.509(4) . ?
P2 C20 1.818(6) . ?
P2 C21 1.797(6) . ?
P2 C27 1.781(6) . ?
O3 N3 1.268(7) . ?
O4 N3 1.243(7) . ?
O5 N3 1.226(7) . ?
N1 C9 1.327(7) . ?
N1 C13 1.371(7) . ?
N2 C14 1.356(7) . ?
N2 C20 1.349(7) . ?
C1 C2 1.386(10) . ?
C1 C6 1.391(15) . ?
C2 H2 0.9500 . ?
C2 C3 1.360(16) . ?
C3 H3 0.9500 . ?
C3 C4 1.358(17) . ?
C4 H4 0.9500 . ?
C4 C5 1.405(15) . ?
C5 H5 0.9500 . ?
C5 C6 1.369(16) . ?
C6 H6 0.9500 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.557(14) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.405(8) . ?
C10 H10 0.9500 . ?
C10 C11 1.346(8) . ?
C11 H11 0.9500 . ?
C11 C12 1.409(8) . ?
C12 C13 1.403(7) . ?
C12 C17 1.416(8) . ?
C13 C14 1.427(7) . ?
C14 C15 1.418(7) . ?
C15 C16 1.422(9) . ?
C15 C18 1.408(9) . ?
C16 H16 0.9500 . ?
C16 C17 1.346(10) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C18 C19 1.337(9) . ?
C19 H19 0.9500 . ?
C19 C20 1.385(8) . ?
C21 C22 1.384(8) . ?
C21 C26 1.389(7) . ?
C22 H22 0.9500 . ?
C22 C23 1.394(9) . ?
C23 H23 0.9500 . ?
C23 C24 1.376(9) . ?
C24 H24 0.9500 . ?
C24 C25 1.378(9) . ?
C25 H25 0.9500 . ?
C25 C26 1.383(8) . ?
C26 H26 0.9500 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.532(9) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
U2 O8 2.414(4) 3_656 ?
U2 O8 2.414(4) . ?
U2 O11 2.538(4) . ?
U2 O11 2.538(4) 3_656 ?
U2 O12 2.532(4) 3_656 ?
U2 O12 2.532(4) . ?
U2 O14 1.764(4) 3_656 ?
U2 O14 1.764(4) . ?
U2 N5 2.987(6) . ?
U2 N5 2.987(6) 3_656 ?
O8 N4 1.296(7) . ?
O9 N4 1.184(8) . ?
O10 N4 1.225(7) . ?
O11 N5 1.264(6) . ?
O12 N5 1.290(7) . ?
O13 N5 1.214(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2 164.73(15) . . ?
O1 U1 O3 108.16(14) . . ?
O1 U1 O4 60.72(16) . . ?
O1 U1 N1 64.75(14) . . ?
O1 U1 N2 125.61(13) . . ?
O1 U1 N3 84.61(15) . . ?
O2 U1 O3 61.25(13) . . ?
O2 U1 O4 110.34(14) . . ?
O2 U1 N1 126.56(13) . . ?
O2 U1 N2 66.05(13) . . ?
O2 U1 N3 85.93(14) . . ?
O3 U1 O4 49.16(14) . . ?
O3 U1 N1 171.77(13) . . ?
O3 U1 N2 126.23(13) . . ?
O3 U1 N3 24.86(14) . . ?
O4 U1 N1 122.83(14) . . ?
O4 U1 N2 166.7(2) . . ?
O4 U1 N3 24.41(14) . . ?
O6 U1 O1 96.4(2) . . ?
O6 U1 O2 94.72(17) . . ?
O6 U1 O3 90.41(17) . . ?
O6 U1 O4 83.8(2) . . ?
O6 U1 N1 86.39(17) . . ?
O6 U1 N2 83.81(17) . . ?
O6 U1 N3 85.12(18) . . ?
O7 U1 O1 84.2(2) . . ?
O7 U1 O2 85.27(16) . . ?
O7 U1 O3 92.12(18) . . ?
O7 U1 O4 99.0(2) . . ?
O7 U1 O6 177.11(19) . . ?
O7 U1 N1 91.29(17) . . ?
O7 U1 N2 93.56(17) . . ?
O7 U1 N3 97.76(19) . . ?
N1 U1 N3 147.01(15) . . ?
N2 U1 N1 60.97(13) . . ?
N2 U1 N3 148.76(15) . . ?
O1 P1 C1 112.5(4) . . ?
O1 P1 C7 112.3(4) . . ?
O1 P1 C9 104.4(3) . . ?
C1 P1 C7 110.0(5) . . ?
C1 P1 C9 108.7(3) . . ?
C7 P1 C9 108.7(4) . . ?
O2 P2 C20 105.1(2) . . ?
O2 P2 C21 111.4(2) . . ?
O2 P2 C27 113.9(3) . . ?
C21 P2 C20 109.5(2) . . ?
C27 P2 C20 109.2(3) . . ?
C27 P2 C21 107.7(3) . . ?
P1 O1 U1 133.8(3) . . ?
P2 O2 U1 130.5(2) . . ?
N3 O3 U1 98.0(3) . . ?
N3 O4 U1 96.8(4) . . ?
C9 N1 U1 122.5(3) . . ?
C9 N1 C13 116.4(4) . . ?
C13 N1 U1 121.1(3) . . ?
C14 N2 U1 120.7(3) . . ?
C20 N2 U1 121.8(3) . . ?
C20 N2 C14 117.5(4) . . ?
O3 N3 U1 57.1(3) . . ?
O4 N3 U1 58.7(3) . . ?
O4 N3 O3 115.5(5) . . ?
O5 N3 U1 174.1(5) . . ?
O5 N3 O3 122.1(5) . . ?
O5 N3 O4 122.4(6) . . ?
C2 C1 P1 123.6(8) . . ?
C2 C1 C6 119.0(9) . . ?
C6 C1 P1 117.4(6) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 C1 121.0(11) . . ?
C3 C2 H2 119.5 . . ?
C2 C3 H3 120.1 . . ?
C4 C3 C2 119.8(10) . . ?
C4 C3 H3 120.1 . . ?
C3 C4 H4 119.5 . . ?
C3 C4 C5 121.0(12) . . ?
C5 C4 H4 119.5 . . ?
C4 C5 H5 120.7 . . ?
C6 C5 C4 118.7(13) . . ?
C6 C5 H5 120.7 . . ?
C1 C6 H6 119.7 . . ?
C5 C6 C1 120.5(10) . . ?
C5 C6 H6 119.7 . . ?
P1 C7 H7A 109.3 . . ?
P1 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
C8 C7 P1 111.6(6) . . ?
C8 C7 H7A 109.3 . . ?
C8 C7 H7B 109.3 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 P1 113.9(4) . . ?
N1 C9 C10 124.5(5) . . ?
C10 C9 P1 121.5(5) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 C9 118.7(5) . . ?
C11 C10 H10 120.7 . . ?
C10 C11 H11 120.1 . . ?
C10 C11 C12 119.7(5) . . ?
C12 C11 H11 120.1 . . ?
C11 C12 C17 122.2(5) . . ?
C13 C12 C11 117.9(5) . . ?
C13 C12 C17 119.9(6) . . ?
N1 C13 C12 122.7(5) . . ?
N1 C13 C14 117.2(5) . . ?
C12 C13 C14 120.0(5) . . ?
N2 C14 C13 120.0(5) . . ?
N2 C14 C15 122.0(5) . . ?
C15 C14 C13 118.0(5) . . ?
C14 C15 C16 120.6(6) . . ?
C18 C15 C14 117.1(5) . . ?
C18 C15 C16 122.3(6) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 C15 120.3(6) . . ?
C17 C16 H16 119.9 . . ?
C12 C17 H17 119.4 . . ?
C16 C17 C12 121.2(6) . . ?
C16 C17 H17 119.4 . . ?
C15 C18 H18 119.6 . . ?
C19 C18 C15 120.8(6) . . ?
C19 C18 H18 119.6 . . ?
C18 C19 H19 120.5 . . ?
C18 C19 C20 119.1(6) . . ?
C20 C19 H19 120.5 . . ?
N2 C20 P2 113.2(4) . . ?
N2 C20 C19 123.6(5) . . ?
C19 C20 P2 123.2(4) . . ?
C22 C21 P2 117.7(4) . . ?
C22 C21 C26 121.1(5) . . ?
C26 C21 P2 121.1(4) . . ?
C21 C22 H22 120.4 . . ?
C21 C22 C23 119.2(6) . . ?
C23 C22 H22 120.4 . . ?
C22 C23 H23 119.9 . . ?
C24 C23 C22 120.2(6) . . ?
C24 C23 H23 119.9 . . ?
C23 C24 H24 120.1 . . ?
C23 C24 C25 119.8(6) . . ?
C25 C24 H24 120.1 . . ?
C24 C25 H25 119.3 . . ?
C24 C25 C26 121.3(6) . . ?
C26 C25 H25 119.3 . . ?
C21 C26 H26 120.8 . . ?
C25 C26 C21 118.4(6) . . ?
C25 C26 H26 120.8 . . ?
P2 C27 H27A 109.1 . . ?
P2 C27 H27B 109.1 . . ?
H27A C27 H27B 107.9 . . ?
C28 C27 P2 112.4(5) . . ?
C28 C27 H27A 109.1 . . ?
C28 C27 H27B 109.1 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O8 U2 O8 180.0(2) 3_656 . ?
O8 U2 O11 66.04(14) . . ?
O8 U2 O11 113.96(14) 3_656 . ?
O8 U2 O11 66.04(14) 3_656 3_656 ?
O8 U2 O11 113.96(14) . 3_656 ?
O8 U2 O12 64.64(14) 3_656 . ?
O8 U2 O12 115.36(15) 3_656 3_656 ?
O8 U2 O12 115.36(15) . . ?
O8 U2 O12 64.64(14) . 3_656 ?
O8 U2 N5 90.07(14) . . ?
O8 U2 N5 89.93(14) 3_656 . ?
O8 U2 N5 89.93(14) . 3_656 ?
O8 U2 N5 90.07(14) 3_656 3_656 ?
O11 U2 O11 180.0 3_656 . ?
O11 U2 N5 24.78(13) . . ?
O11 U2 N5 155.22(13) 3_656 . ?
O11 U2 N5 155.22(13) . 3_656 ?
O11 U2 N5 24.78(13) 3_656 3_656 ?
O12 U2 O11 49.96(14) . . ?
O12 U2 O11 49.96(14) 3_656 3_656 ?
O12 U2 O11 130.04(14) 3_656 . ?
O12 U2 O11 130.04(14) . 3_656 ?
O12 U2 O12 180.0 . 3_656 ?
O12 U2 N5 154.63(13) 3_656 . ?
O12 U2 N5 25.37(13) . . ?
O12 U2 N5 25.37(13) 3_656 3_656 ?
O12 U2 N5 154.63(13) . 3_656 ?
O14 U2 O8 81.21(16) 3_656 . ?
O14 U2 O8 81.21(16) . 3_656 ?
O14 U2 O8 98.79(16) . . ?
O14 U2 O8 98.79(16) 3_656 3_656 ?
O14 U2 O11 91.46(18) . . ?
O14 U2 O11 91.46(18) 3_656 3_656 ?
O14 U2 O11 88.54(18) 3_656 . ?
O14 U2 O11 88.54(18) . 3_656 ?
O14 U2 O12 88.51(19) 3_656 . ?
O14 U2 O12 91.49(19) 3_656 3_656 ?
O14 U2 O12 88.51(19) . 3_656 ?
O14 U2 O12 91.49(19) . . ?
O14 U2 O14 180.0(2) . 3_656 ?
O14 U2 N5 93.86(18) . . ?
O14 U2 N5 86.14(18) 3_656 . ?
O14 U2 N5 86.13(18) . 3_656 ?
O14 U2 N5 93.87(18) 3_656 3_656 ?
N5 U2 N5 180.00(16) 3_656 . ?
N4 O8 U2 126.7(4) . . ?
N5 O11 U2 97.9(4) . . ?
N5 O12 U2 97.4(3) . . ?
O9 N4 O8 117.8(6) . . ?
O9 N4 O10 124.8(6) . . ?
O10 N4 O8 117.4(6) . . ?
O11 N5 U2 57.3(3) . . ?
O11 N5 O12 113.9(6) . . ?
O12 N5 U2 57.2(3) . . ?
O13 N5 U2 169.9(4) . . ?
O13 N5 O11 124.1(6) . . ?
O13 N5 O12 121.9(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 O3 N3 O4 6.9(7) . . . . ?
U1 O3 N3 O5 -173.1(6) . . . . ?
U1 O4 N3 O3 -6.8(7) . . . . ?
U1 O4 N3 O5 173.2(6) . . . . ?
U1 N1 C9 P1 -3.7(6) . . . . ?
U1 N1 C9 C10 179.7(5) . . . . ?
U1 N1 C13 C12 -178.5(4) . . . . ?
U1 N1 C13 C14 0.6(6) . . . . ?
U1 N2 C14 C13 0.4(7) . . . . ?
U1 N2 C14 C15 -179.8(4) . . . . ?
U1 N2 C20 P2 -1.1(5) . . . . ?
U1 N2 C20 C19 178.7(5) . . . . ?
P1 C1 C2 C3 -179.9(7) . . . . ?
P1 C1 C6 C5 -179.0(9) . . . . ?
P1 C9 C10 C11 -178.2(5) . . . . ?
P2 C21 C22 C23 177.1(5) . . . . ?
P2 C21 C26 C25 -177.7(5) . . . . ?
O1 P1 C1 C2 139.0(6) . . . . ?
O1 P1 C1 C6 -42.8(8) . . . . ?
O1 P1 C7 C8 63.7(7) . . . . ?
O1 P1 C9 N1 -1.8(6) . . . . ?
O1 P1 C9 C10 175.0(5) . . . . ?
O2 P2 C20 N2 12.3(5) . . . . ?
O2 P2 C20 C19 -167.5(5) . . . . ?
O2 P2 C21 C22 1.5(5) . . . . ?
O2 P2 C21 C26 180.0(4) . . . . ?
O2 P2 C27 C28 -72.3(5) . . . . ?
N1 C9 C10 C11 -1.8(10) . . . . ?
N1 C13 C14 N2 -0.6(7) . . . . ?
N1 C13 C14 C15 179.5(5) . . . . ?
N2 C14 C15 C16 -178.3(6) . . . . ?
N2 C14 C15 C18 1.1(9) . . . . ?
C1 P1 O1 U1 126.3(5) . . . . ?
C1 P1 C7 C8 -170.2(6) . . . . ?
C1 P1 C9 N1 -122.0(5) . . . . ?
C1 P1 C9 C10 54.7(6) . . . . ?
C1 C2 C3 C4 -1.0(15) . . . . ?
C2 C1 C6 C5 -0.7(15) . . . . ?
C2 C3 C4 C5 -1.1(18) . . . . ?
C3 C4 C5 C6 2.3(19) . . . . ?
C4 C5 C6 C1 -1.3(18) . . . . ?
C6 C1 C2 C3 1.9(13) . . . . ?
C7 P1 O1 U1 -108.9(6) . . . . ?
C7 P1 C1 C2 13.0(8) . . . . ?
C7 P1 C1 C6 -168.8(7) . . . . ?
C7 P1 C9 N1 118.3(6) . . . . ?
C7 P1 C9 C10 -65.0(7) . . . . ?
C9 P1 O1 U1 8.6(6) . . . . ?
C9 P1 C1 C2 -105.9(7) . . . . ?
C9 P1 C1 C6 72.3(7) . . . . ?
C9 P1 C7 C8 -51.4(7) . . . . ?
C9 N1 C13 C12 -0.6(8) . . . . ?
C9 N1 C13 C14 178.4(5) . . . . ?
C9 C10 C11 C12 0.5(9) . . . . ?
C10 C11 C12 C13 0.5(8) . . . . ?
C10 C11 C12 C17 -179.7(6) . . . . ?
C11 C12 C13 N1 -0.5(8) . . . . ?
C11 C12 C13 C14 -179.5(5) . . . . ?
C11 C12 C17 C16 -179.9(7) . . . . ?
C12 C13 C14 N2 178.4(5) . . . . ?
C12 C13 C14 C15 -1.4(8) . . . . ?
C13 N1 C9 P1 178.4(4) . . . . ?
C13 N1 C9 C10 1.8(9) . . . . ?
C13 C12 C17 C16 -0.1(10) . . . . ?
C13 C14 C15 C16 1.6(9) . . . . ?
C13 C14 C15 C18 -179.1(6) . . . . ?
C14 N2 C20 P2 179.4(4) . . . . ?
C14 N2 C20 C19 -0.9(8) . . . . ?
C14 C15 C16 C17 -1.0(11) . . . . ?
C14 C15 C18 C19 -1.1(10) . . . . ?
C15 C16 C17 C12 0.3(12) . . . . ?
C15 C18 C19 C20 0.2(11) . . . . ?
C16 C15 C18 C19 178.3(7) . . . . ?
C17 C12 C13 N1 179.7(6) . . . . ?
C17 C12 C13 C14 0.7(8) . . . . ?
C18 C15 C16 C17 179.6(7) . . . . ?
C18 C19 C20 P2 -179.4(5) . . . . ?
C18 C19 C20 N2 0.9(10) . . . . ?
C20 P2 O2 U1 -22.5(4) . . . . ?
C20 P2 C21 C22 117.3(5) . . . . ?
C20 P2 C21 C26 -64.2(5) . . . . ?
C20 P2 C27 C28 170.6(4) . . . . ?
C20 N2 C14 C13 -180.0(5) . . . . ?
C20 N2 C14 C15 -0.2(8) . . . . ?
C21 P2 O2 U1 95.9(3) . . . . ?
C21 P2 C20 N2 -107.5(4) . . . . ?
C21 P2 C20 C19 72.7(6) . . . . ?
C21 P2 C27 C28 51.8(5) . . . . ?
C21 C22 C23 C24 1.6(10) . . . . ?
C22 C21 C26 C25 0.7(9) . . . . ?
C22 C23 C24 C25 -1.2(11) . . . . ?
C23 C24 C25 C26 0.5(10) . . . . ?
C24 C25 C26 C21 -0.2(10) . . . . ?
C26 C21 C22 C23 -1.4(9) . . . . ?
C27 P2 O2 U1 -142.0(3) . . . . ?
C27 P2 C20 N2 134.8(4) . . . . ?
C27 P2 C20 C19 -45.0(6) . . . . ?
C27 P2 C21 C22 -124.1(5) . . . . ?
C27 P2 C21 C26 54.4(5) . . . . ?
U2 O8 N4 O9 14.1(10) . . . . ?
U2 O8 N4 O10 -165.9(4) . . . . ?
U2 O11 N5 O12 -8.8(5) . . . . ?
U2 O11 N5 O13 168.0(5) . . . . ?
U2 O12 N5 O11 8.8(5) . . . . ?
U2 O12 N5 O13 -168.1(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_230905_et_ph_rr
_database_code_depnum_ccdc_archive 'CCDC 2293651'
loop_
_audit_author_name
_audit_author_address
'Xiaofan Yang'
;Zhejiang University
China
;
_audit_update_record             
;
2023-09-07 deposited with the CCDC.	2024-04-04 downloaded from the CCDC.
;
_audit_creation_date             2023-09-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H26 N2 O2 P2'
_chemical_formula_sum            'C28 H26 N2 O2 P2'
_chemical_formula_weight         484.45
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   8.2310(3)
_cell_length_b                   11.7984(5)
_cell_length_c                   13.6524(5)
_cell_angle_alpha                73.8290(10)
_cell_angle_beta                 85.3630(10)
_cell_angle_gamma                76.8650(10)
_cell_volume                     1239.83(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9782
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      27.552
_cell_measurement_theta_min      2.540
_shelx_estimated_absorpt_T_max   0.945
_shelx_estimated_absorpt_T_min   0.919
_exptl_absorpt_coefficient_mu    0.204
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0802 before and 0.0513 after correction.
The Ratio of minimum to maximum transmission is 0.9678.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.28
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            62474
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.561
_diffrn_reflns_theta_min         2.065
_diffrn_ambient_temperature      170.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'zju Bruker D8 Venture'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5400
_reflns_number_total             5697
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.14'
_computing_data_reduction        'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5697
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0332
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0409P)²+0.5469P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0903
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C21(H21A,H21B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C16(H16),
 C17(H17), C18(H18), C19(H19), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C22(H22A,H22B,H22C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.67714(4) 0.51844(3) 0.62710(2) 0.02259(9) Uani 1 1 d . . . . .
O1 O 0.73761(13) 0.42646(8) 0.56922(8) 0.0314(2) Uani 1 1 d . . . . .
N1 N 0.66204(13) 0.75001(9) 0.61037(8) 0.0208(2) Uani 1 1 d . . . . .
C1 C 0.89732(18) 0.37065(13) 0.77441(11) 0.0327(3) Uani 1 1 d . . . . .
H1 H 0.933434 0.326874 0.724977 0.039 Uiso 1 1 calc R U . . .
P2 P 0.34402(4) 0.96745(3) 0.86858(2) 0.02020(8) Uani 1 1 d . . . . .
O2 O 0.27283(12) 1.07118(9) 0.91191(8) 0.0311(2) Uani 1 1 d . . . . .
N2 N 0.52713(12) 0.92599(9) 0.70529(7) 0.01864(19) Uani 1 1 d . . . . .
C2 C 0.97567(19) 0.33329(15) 0.86810(13) 0.0407(4) Uani 1 1 d . . . . .
H2 H 1.065348 0.264639 0.882460 0.049 Uiso 1 1 calc R U . . .
C3 C 0.9224(2) 0.39642(15) 0.93981(12) 0.0429(4) Uani 1 1 d . . . . .
H3 H 0.975582 0.371076 1.003872 0.052 Uiso 1 1 calc R U . . .
C4 C 0.7920(2) 0.49656(15) 0.91928(12) 0.0432(4) Uani 1 1 d . . . . .
H4 H 0.755539 0.539259 0.969417 0.052 Uiso 1 1 calc R U . . .
C5 C 0.7143(2) 0.53480(13) 0.82579(11) 0.0343(3) Uani 1 1 d . . . . .
H5 H 0.625438 0.604033 0.811697 0.041 Uiso 1 1 calc R U . . .
C6 C 0.76652(16) 0.47157(11) 0.75245(10) 0.0248(2) Uani 1 1 d . . . . .
C7 C 0.45363(16) 0.56172(11) 0.64052(10) 0.0258(3) Uani 1 1 d . . . . .
H7A H 0.427008 0.625299 0.677289 0.031 Uiso 1 1 calc R U . . .
H7B H 0.405534 0.597201 0.571712 0.031 Uiso 1 1 calc R U . . .
C8 C 0.3703(2) 0.45879(14) 0.69690(14) 0.0427(4) Uani 1 1 d . . . . .
H8A H 0.397084 0.394641 0.661783 0.064 Uiso 1 1 calc R U . . .
H8B H 0.249178 0.488723 0.698420 0.064 Uiso 1 1 calc R U . . .
H8C H 0.411047 0.426625 0.766850 0.064 Uiso 1 1 calc R U . . .
C9 C 0.73495(16) 0.66278(11) 0.56714(9) 0.0224(2) Uani 1 1 d . . . . .
C10 C 0.84732(17) 0.67844(12) 0.48376(10) 0.0284(3) Uani 1 1 d . . . . .
H10 H 0.899578 0.612754 0.456821 0.034 Uiso 1 1 calc R U . . .
C11 C 0.87930(17) 0.79174(13) 0.44237(10) 0.0287(3) Uani 1 1 d . . . . .
H11 H 0.953995 0.805446 0.385638 0.034 Uiso 1 1 calc R U . . .
C12 C 0.80141(15) 0.88723(11) 0.48406(9) 0.0220(2) Uani 1 1 d . . . . .
C13 C 0.69493(14) 0.86084(10) 0.57033(9) 0.0189(2) Uani 1 1 d . . . . .
C14 C 0.62001(14) 0.95536(10) 0.61945(9) 0.0184(2) Uani 1 1 d . . . . .
C15 C 0.65213(15) 1.07243(10) 0.57818(9) 0.0209(2) Uani 1 1 d . . . . .
C16 C 0.75596(15) 1.09612(11) 0.48826(10) 0.0243(2) Uani 1 1 d . . . . .
H16 H 0.774410 1.175424 0.459658 0.029 Uiso 1 1 calc R U . . .
C17 C 0.82771(16) 1.00789(12) 0.44370(10) 0.0249(3) Uani 1 1 d . . . . .
H17 H 0.896749 1.025847 0.384691 0.030 Uiso 1 1 calc R U . . .
C18 C 0.58190(16) 1.16146(11) 0.62894(10) 0.0255(3) Uani 1 1 d . . . . .
H18 H 0.601597 1.240876 0.604069 0.031 Uiso 1 1 calc R U . . .
C19 C 0.48441(16) 1.13199(11) 0.71498(10) 0.0247(2) Uani 1 1 d . . . . .
H19 H 0.433592 1.190988 0.749633 0.030 Uiso 1 1 calc R U . . .
C20 C 0.46153(14) 1.01267(10) 0.75057(9) 0.0197(2) Uani 1 1 d . . . . .
C21 C 0.48854(16) 0.84633(12) 0.94920(10) 0.0275(3) Uani 1 1 d . . . . .
H21A H 0.534777 0.784268 0.912435 0.033 Uiso 1 1 calc R U . . .
H21B H 0.582284 0.877970 0.964624 0.033 Uiso 1 1 calc R U . . .
C22 C 0.4062(2) 0.78817(18) 1.04879(12) 0.0509(5) Uani 1 1 d . . . . .
H22A H 0.321602 0.748765 1.034271 0.076 Uiso 1 1 calc R U . . .
H22B H 0.353078 0.850390 1.083014 0.076 Uiso 1 1 calc R U . . .
H22C H 0.490794 0.727939 1.093137 0.076 Uiso 1 1 calc R U . . .
C23 C 0.18557(15) 0.90058(11) 0.83730(9) 0.0216(2) Uani 1 1 d . . . . .
C24 C 0.22244(16) 0.79773(12) 0.80119(10) 0.0269(3) Uani 1 1 d . . . . .
H24 H 0.335305 0.760020 0.791713 0.032 Uiso 1 1 calc R U . . .
C25 C 0.09417(18) 0.75062(13) 0.77915(10) 0.0300(3) Uani 1 1 d . . . . .
H25 H 0.119417 0.680343 0.754983 0.036 Uiso 1 1 calc R U . . .
C26 C -0.07057(18) 0.80575(14) 0.79228(11) 0.0328(3) Uani 1 1 d . . . . .
H26 H -0.158155 0.773368 0.777054 0.039 Uiso 1 1 calc R U . . .
C27 C -0.10728(18) 0.90750(15) 0.82739(13) 0.0395(3) Uani 1 1 d . . . . .
H27 H -0.220402 0.945439 0.835813 0.047 Uiso 1 1 calc R U . . .
C28 C 0.01987(17) 0.95525(14) 0.85066(12) 0.0323(3) Uani 1 1 d . . . . .
H28 H -0.006376 1.024967 0.875593 0.039 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
P1 O1 1.4896(9) . ?
P1 C6 1.8075(13) . ?
P1 C7 1.8026(14) . ?
P1 C9 1.8235(13) . ?
N1 C9 1.3296(15) . ?
N1 C13 1.3494(15) . ?
C1 H1 0.9500 . ?
C1 C2 1.392(2) . ?
C1 C6 1.3919(18) . ?
P2 O2 1.4874(9) . ?
P2 C20 1.8219(12) . ?
P2 C21 1.7977(13) . ?
P2 C23 1.8031(12) . ?
N2 C14 1.3518(15) . ?
N2 C20 1.3292(15) . ?
C2 H2 0.9500 . ?
C2 C3 1.376(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.384(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.386(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.3945(18) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.5198(19) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.4057(18) . ?
C10 H10 0.9500 . ?
C10 C11 1.3750(19) . ?
C11 H11 0.9500 . ?
C11 C12 1.4050(17) . ?
C12 C13 1.4161(16) . ?
C12 C17 1.4356(17) . ?
C13 C14 1.4529(16) . ?
C14 C15 1.4155(16) . ?
C15 C16 1.4364(17) . ?
C15 C18 1.4080(17) . ?
C16 H16 0.9500 . ?
C16 C17 1.3482(18) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C18 C19 1.3753(18) . ?
C19 H19 0.9500 . ?
C19 C20 1.4064(16) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.524(2) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.3961(17) . ?
C23 C28 1.3910(18) . ?
C24 H24 0.9500 . ?
C24 C25 1.3876(18) . ?
C25 H25 0.9500 . ?
C25 C26 1.385(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.376(2) . ?
C27 H27 0.9500 . ?
C27 C28 1.391(2) . ?
C28 H28 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 P1 C6 111.89(6) . . ?
O1 P1 C7 115.26(6) . . ?
O1 P1 C9 113.42(6) . . ?
C6 P1 C9 104.28(6) . . ?
C7 P1 C6 108.51(6) . . ?
C7 P1 C9 102.53(6) . . ?
C9 N1 C13 118.04(10) . . ?
C2 C1 H1 119.7 . . ?
C6 C1 H1 119.7 . . ?
C6 C1 C2 120.61(14) . . ?
O2 P2 C20 111.83(6) . . ?
O2 P2 C21 114.98(6) . . ?
O2 P2 C23 112.57(6) . . ?
C21 P2 C20 104.48(6) . . ?
C21 P2 C23 106.35(6) . . ?
C23 P2 C20 105.88(5) . . ?
C20 N2 C14 117.60(10) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 C1 119.57(14) . . ?
C3 C2 H2 120.2 . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.47(14) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 119.9 . . ?
C3 C4 C5 120.23(15) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 119.96(14) . . ?
C6 C5 H5 120.0 . . ?
C1 C6 P1 118.03(10) . . ?
C1 C6 C5 119.15(13) . . ?
C5 C6 P1 122.77(10) . . ?
P1 C7 H7A 108.7 . . ?
P1 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
C8 C7 P1 114.44(10) . . ?
C8 C7 H7A 108.7 . . ?
C8 C7 H7B 108.7 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 P1 113.60(9) . . ?
N1 C9 C10 123.89(11) . . ?
C10 C9 P1 122.51(9) . . ?
C9 C10 H10 121.0 . . ?
C11 C10 C9 117.96(12) . . ?
C11 C10 H10 121.0 . . ?
C10 C11 H11 120.0 . . ?
C10 C11 C12 119.95(12) . . ?
C12 C11 H11 120.0 . . ?
C11 C12 C13 117.58(11) . . ?
C11 C12 C17 122.74(11) . . ?
C13 C12 C17 119.67(11) . . ?
N1 C13 C12 122.51(11) . . ?
N1 C13 C14 118.20(10) . . ?
C12 C13 C14 119.28(10) . . ?
N2 C14 C13 118.11(10) . . ?
N2 C14 C15 122.81(11) . . ?
C15 C14 C13 119.04(10) . . ?
C14 C15 C16 119.70(11) . . ?
C18 C15 C14 117.88(11) . . ?
C18 C15 C16 122.41(11) . . ?
C15 C16 H16 119.4 . . ?
C17 C16 C15 121.22(11) . . ?
C17 C16 H16 119.4 . . ?
C12 C17 H17 119.5 . . ?
C16 C17 C12 121.02(11) . . ?
C16 C17 H17 119.5 . . ?
C15 C18 H18 120.4 . . ?
C19 C18 C15 119.16(11) . . ?
C19 C18 H18 120.4 . . ?
C18 C19 H19 120.7 . . ?
C18 C19 C20 118.60(11) . . ?
C20 C19 H19 120.7 . . ?
N2 C20 P2 116.00(8) . . ?
N2 C20 C19 123.92(11) . . ?
C19 C20 P2 120.02(9) . . ?
P2 C21 H21A 109.2 . . ?
P2 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
C22 C21 P2 111.96(11) . . ?
C22 C21 H21A 109.2 . . ?
C22 C21 H21B 109.2 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 P2 123.01(9) . . ?
C28 C23 P2 117.46(10) . . ?
C28 C23 C24 119.53(12) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 C23 119.97(12) . . ?
C25 C24 H24 120.0 . . ?
C24 C25 H25 119.9 . . ?
C26 C25 C24 120.20(13) . . ?
C26 C25 H25 119.9 . . ?
C25 C26 H26 120.0 . . ?
C27 C26 C25 119.94(12) . . ?
C27 C26 H26 120.0 . . ?
C26 C27 H27 119.7 . . ?
C26 C27 C28 120.56(13) . . ?
C28 C27 H27 119.7 . . ?
C23 C28 C27 119.79(13) . . ?
C23 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C9 C10 C11 178.33(10) . . . . ?
O1 P1 C6 C1 10.65(13) . . . . ?
O1 P1 C6 C5 -171.89(12) . . . . ?
O1 P1 C7 C8 60.81(13) . . . . ?
O1 P1 C9 N1 171.08(9) . . . . ?
O1 P1 C9 C10 -9.46(13) . . . . ?
N1 C9 C10 C11 -2.3(2) . . . . ?
N1 C13 C14 N2 2.83(16) . . . . ?
N1 C13 C14 C15 -179.59(10) . . . . ?
C1 C2 C3 C4 -0.1(2) . . . . ?
P2 C23 C24 C25 179.63(10) . . . . ?
P2 C23 C28 C27 179.81(12) . . . . ?
O2 P2 C20 N2 -178.75(8) . . . . ?
O2 P2 C20 C19 3.97(12) . . . . ?
O2 P2 C21 C22 62.63(12) . . . . ?
O2 P2 C23 C24 -176.15(10) . . . . ?
O2 P2 C23 C28 3.64(13) . . . . ?
N2 C14 C15 C16 178.22(11) . . . . ?
N2 C14 C15 C18 -0.74(17) . . . . ?
C2 C1 C6 P1 177.31(11) . . . . ?
C2 C1 C6 C5 -0.2(2) . . . . ?
C2 C3 C4 C5 -0.4(3) . . . . ?
C3 C4 C5 C6 0.6(3) . . . . ?
C4 C5 C6 P1 -177.69(12) . . . . ?
C4 C5 C6 C1 -0.3(2) . . . . ?
C6 P1 C7 C8 -65.54(12) . . . . ?
C6 P1 C9 N1 -66.95(10) . . . . ?
C6 P1 C9 C10 112.50(11) . . . . ?
C6 C1 C2 C3 0.4(2) . . . . ?
C7 P1 C6 C1 138.93(11) . . . . ?
C7 P1 C6 C5 -43.62(13) . . . . ?
C7 P1 C9 N1 46.14(10) . . . . ?
C7 P1 C9 C10 -134.41(11) . . . . ?
C9 P1 C6 C1 -112.32(11) . . . . ?
C9 P1 C6 C5 65.13(13) . . . . ?
C9 P1 C7 C8 -175.47(11) . . . . ?
C9 N1 C13 C12 0.87(17) . . . . ?
C9 N1 C13 C14 -177.94(10) . . . . ?
C9 C10 C11 C12 0.5(2) . . . . ?
C10 C11 C12 C13 1.73(19) . . . . ?
C10 C11 C12 C17 -179.19(12) . . . . ?
C11 C12 C13 N1 -2.50(18) . . . . ?
C11 C12 C13 C14 176.30(11) . . . . ?
C11 C12 C17 C16 -177.32(12) . . . . ?
C12 C13 C14 N2 -176.02(10) . . . . ?
C12 C13 C14 C15 1.57(16) . . . . ?
C13 N1 C9 P1 -178.97(8) . . . . ?
C13 N1 C9 C10 1.58(18) . . . . ?
C13 C12 C17 C16 1.74(18) . . . . ?
C13 C14 C15 C16 0.75(17) . . . . ?
C13 C14 C15 C18 -178.21(10) . . . . ?
C14 N2 C20 P2 -177.76(8) . . . . ?
C14 N2 C20 C19 -0.60(17) . . . . ?
C14 C15 C16 C17 -1.89(18) . . . . ?
C14 C15 C18 C19 -0.72(18) . . . . ?
C15 C16 C17 C12 0.64(19) . . . . ?
C15 C18 C19 C20 1.45(19) . . . . ?
C16 C15 C18 C19 -179.65(12) . . . . ?
C17 C12 C13 N1 178.39(11) . . . . ?
C17 C12 C13 C14 -2.81(17) . . . . ?
C18 C15 C16 C17 177.02(12) . . . . ?
C18 C19 C20 P2 176.23(9) . . . . ?
C18 C19 C20 N2 -0.82(19) . . . . ?
C20 P2 C21 C22 -174.42(11) . . . . ?
C20 P2 C23 C24 61.38(12) . . . . ?
C20 P2 C23 C28 -118.83(11) . . . . ?
C20 N2 C14 C13 178.88(10) . . . . ?
C20 N2 C14 C15 1.38(16) . . . . ?
C21 P2 C20 N2 56.27(10) . . . . ?
C21 P2 C20 C19 -121.01(10) . . . . ?
C21 P2 C23 C24 -49.38(12) . . . . ?
C21 P2 C23 C28 130.41(11) . . . . ?
C23 P2 C20 N2 -55.80(10) . . . . ?
C23 P2 C20 C19 126.92(10) . . . . ?
C23 P2 C21 C22 -62.68(12) . . . . ?
C23 C24 C25 C26 0.4(2) . . . . ?
C24 C23 C28 C27 -0.4(2) . . . . ?
C24 C25 C26 C27 -0.1(2) . . . . ?
C25 C26 C27 C28 -0.5(2) . . . . ?
C26 C27 C28 C23 0.7(2) . . . . ?
C28 C23 C24 C25 -0.2(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
