# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_exp_1018
_database_code_depnum_ccdc_archive 'CCDC 1894664'
loop_
_audit_author_name
_audit_author_address
'Zhongshu Li'
;Lehn Institute of Functional Materials, School of Chemistry, Sun Yat Sen University
China
;
_audit_update_record             
;
2022-05-18 deposited with the CCDC.	2022-06-06 downloaded from the CCDC.
;
_audit_creation_date             2022-05-07
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_chemical_formula_moiety         '1.5(C32 H48 Na2 O12 P2)'
_chemical_formula_sum            'C48 H72 Na3 O18 P3'
_chemical_formula_weight         1098.987
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.01920 0.00962 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.21560 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.00304 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Na 0.13799 0.12245 4.76260 3.17360 1.26740 1.11280 3.28500 8.84220 0.31360
129.42400 0.67600 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.05239 0.03377 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.25080 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
P 0.30360 0.43703 6.43450 4.17910 1.78000 1.49080 1.90670 27.15700 0.52600
68.16450 1.11490 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_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_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z+1/2
3 -x,-y,-z
4 x,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   13.2833(3)
_cell_length_b                   14.4071(3)
_cell_length_c                   30.5777(8)
_cell_angle_alpha                90
_cell_angle_beta                 100.568(2)
_cell_angle_gamma                90
_cell_volume                     5752.5(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12207
_cell_measurement_temperature    150.10(10)
_cell_measurement_theta_max      71.1320
_cell_measurement_theta_min      4.0240
_exptl_absorpt_coefficient_mu    1.731
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       needle
_exptl_crystal_F_000             2340.843
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.9977
_diffrn_reflns_Laue_measured_fraction_max 0.9813
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            33361
_diffrn_reflns_point_group_measured_fraction_full 0.9977
_diffrn_reflns_point_group_measured_fraction_max 0.9813
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         71.14
_diffrn_reflns_theta_min         3.38
_diffrn_ambient_temperature      150.10(10)
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.9813
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -96.00  -2.00   1.00   40.00    --  -41.20 125.00 -30.00   94
  2  ω    -66.00  33.00   1.00   40.00    --  -41.20  38.00 -90.00   99
  3  ω   -110.00 -17.00   1.00   40.00    --  -41.20 -38.00  90.00   93
  4  ω     25.00 130.00   1.00  120.00    --  101.52 -30.00-150.00  105
  5  ω     25.00 130.00   1.00  120.00    --  101.52 -30.00   0.00  105
  6  ω     37.00 109.00   1.00  120.00    --  101.52 -94.00 -90.00   72
  7  ω     79.00 167.00   1.00  120.00    --  101.52  45.00-180.00   88
  8  ω    113.00 166.00   1.00  120.00    --  101.52 125.00 -30.00   53
  9  ω     29.00 122.00   1.00  120.00    --  101.52-125.00-150.00   93
 10  ω     94.00 136.00   1.00  120.00    --  101.52 125.00   0.00   42
 11  ω     25.00 134.00   1.00  120.00    --  101.52 -77.00   0.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -16
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              37
_reflns_limit_l_min              0
_reflns_number_gt                8154
_reflns_number_total             10920
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.3351
_refine_diff_density_min         -0.3675
_refine_diff_density_rms         0.0617
_refine_ls_d_res_high            0.8146
_refine_ls_d_res_low             13.0580
_refine_ls_goodness_of_fit_ref   1.0214
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    132
_refine_ls_number_parameters     761
_refine_ls_number_reflns         10920
_refine_ls_number_restraints     107
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0479
_refine_ls_restrained_S_all      1.0148
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0851P)²+0.3287P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1302
_refine_ls_wR_factor_ref         0.1449
_olex2_refinement_description    
;
1. Restrained distances
 Na1-O8 \\sim Na1-O8A
 with sigma of 0.02
 Na1-O7 \\sim Na1-O7A
 with sigma of 0.02
 O8-C27 \\sim O8A-C27A
 with sigma of 0.02
 O8-C28 \\sim O8A-C28A
 with sigma of 0.02
 O7-C26 \\sim O7A-C26A
 with sigma of 0.02
 C27-C26 \\sim C27A-C26A
 with sigma of 0.02
 O7-C25 \\sim O7A-C25A
 with sigma of 0.02
 C27-C28 \\sim C27A-C28A
 with sigma of 0.04
 Na1-C27 \\sim Na1-C27A
 with sigma of 0.04
 C26-C25 \\sim C26A-C25A
 with sigma of 0.04
 Na1-C28 \\sim Na1-C28A
 with sigma of 0.04
 Na1-C26 \\sim Na1-C26A
 with sigma of 0.04
 Na1-C25 \\sim Na1-C25A
 with sigma of 0.04
 O8-C26 \\sim O8A-C26A
 with sigma of 0.04
 O7-C27 \\sim O7A-C27A
 with sigma of 0.04
 C42-C0AA \\sim C42A-C0AB
 with sigma of 0.04
 C44-C0AA \\sim C44A-C0AB
 with sigma of 0.02
 O16-C44 \\sim O16A-C44A
 with sigma of 0.02
 C44-O0AA \\sim C44A-O0AB
 with sigma of 0.04
 O16-C45 \\sim O16A-C45A
 with sigma of 0.02
 C44-C45 \\sim C44A-C45A
 with sigma of 0.04
 C42-O0AA \\sim C42A-O0AB
 with sigma of 0.02
 C0AA-O0AA \\sim C0AB-O0AB
 with sigma of 0.02
 O16-C0AA \\sim O16A-C0AB
 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
C25A \\sim O8A \\sim C27A \\sim C28A \\sim C26A \\sim O7A: within 2A with sigma
of 0.001 and sigma for terminal atoms of 0.002 within 2A
3. Rigid body (RIGU) restrains
 C44, O16, C45, C0AA, O0AA, C42
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C0AB, O0AB, C42A, C44A, O16A, C45A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(O8A)=Sof(O7A)=Sof(C27A)=Sof(H27c)=Sof(H27d)=Sof(C28A)=Sof(H28d)=Sof(H28e)=
 Sof(H28f)=Sof(C26A)=Sof(H26c)=Sof(H26d)=Sof(C25A)=Sof(H25d)=Sof(H25e)=
 Sof(H25f)=1-FVAR(1)
 Sof(O8)=Sof(O7)=Sof(C27)=Sof(H27a)=Sof(H27b)=Sof(C28)=Sof(H28a)=Sof(H28b)=
 Sof(H28c)=Sof(C26)=Sof(H26a)=Sof(H26b)=Sof(C25)=Sof(H25a)=Sof(H25b)=Sof(H25c)=
 FVAR(1)
 Sof(O0AB)=Sof(O16A)=Sof(C44A)=Sof(H44c)=Sof(H44d)=Sof(C45A)=Sof(H45d)=
 Sof(H45e)=Sof(H45f)=Sof(C0AB)=Sof(H0Ac)=Sof(H0Ad)=Sof(C42A)=Sof(H42d)=
 Sof(H42e)=Sof(H42f)=1-FVAR(2)
 Sof(O16)=Sof(C44)=Sof(H44a)=Sof(H44b)=Sof(C45)=Sof(H45a)=Sof(H45b)=Sof(H45c)=
 Sof(C42)=Sof(H42a)=Sof(H42b)=Sof(H42c)=Sof(C0AA)=Sof(H0Aa)=Sof(H0Ab)=Sof(O0AA)=
 FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C30(H30a,H30b), C36(H36a,H36b), C31(H31a,H31b), C48(H48a,H48b), C47(H47a,
 H47b), C39(H39a,H39b), C27(H27a,H27b), C44(H44a,H44b), C26(H26a,H26b),
 C0AA(H0Aa,H0Ab), C27A(H27c,H27d), C26A(H26c,H26d), C44A(H44c,H44d), C0AB(H0Ac,
 H0Ad)
5.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C8(H8), C19(H19), C5(H5), C21(H21), C20(H20), C11(H11), C14(H14),
 C12(H12), C6(H6), C13(H13), C7(H7)
5.c Idealised Me refined as rotating group:
 C29(H29a,H29b,H29c), C37(H37a,H37b,H37c), C33(H33a,H33b,H33c), C46(H46a,H46b,
 H46c), C49(H49a,H49b,H49c), C32(H32a,H32b,H32c), C28(H28a,H28b,H28c), C38(H38a,
 H38b,H38c), C45(H45a,H45b,H45c), C41(H41a,H41b,H41c), C25(H25a,H25b,H25c),
 C42(H42a,H42b,H42c), C28A(H28d,H28e,H28f), C25A(H25d,H25e,H25f), C45A(H45d,
 H45e,H45f), C42A(H42d,H42e,H42f)
;
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_disorder_group
P2 P 0.07840(4) 0.94937(3) 0.393427(18) 0.03774(14) Uani 1.000000 . . .
P3 P 0.58490(4) 0.45599(3) 0.767342(19) 0.03938(14) Uani 1.000000 . . .
P1 P 0.23496(4) 0.45527(3) 0.430338(19) 0.04045(14) Uani 1.000000 . . .
Na2 Na 0.19987(5) 0.74766(5) 0.51355(2) 0.03162(17) Uani 1.000000 . . .
Na1 Na 0.12903(6) 0.23980(5) 0.31402(2) 0.03286(18) Uani 1.000000 D . .
Na3 Na 0.45066(5) 0.24625(5) 0.64930(2) 0.03316(18) Uani 1.000000 . . .
O12 O 0.02076(11) 0.78098(9) 0.50989(5) 0.0406(3) Uani 1.000000 . . .
O9 O 0.22101(11) 0.11716(9) 0.28285(5) 0.0406(3) Uani 1.000000 . . .
O11 O 0.12614(11) 0.63460(10) 0.55762(5) 0.0414(3) Uani 1.000000 . . .
O6 O 0.57555(11) 0.62778(9) 0.80357(5) 0.0412(3) Uani 1.000000 . . .
O18 O 0.63311(11) 0.27823(9) 0.65142(5) 0.0431(3) Uani 1.000000 . . .
O3 O 0.08285(12) 1.12414(10) 0.35991(5) 0.0430(3) Uani 1.000000 . . .
O10 O 0.31879(11) 0.27169(9) 0.32688(5) 0.0437(3) Uani 1.000000 . . .
O2 O 0.21274(12) 0.62446(10) 0.46734(5) 0.0457(4) Uani 1.000000 . . .
O17 O 0.53099(11) 0.12440(11) 0.60777(5) 0.0473(4) Uani 1.000000 . . .
O4 O 0.19903(13) 0.85999(10) 0.46230(5) 0.0477(4) Uani 1.000000 . . .
O5 O 0.46290(13) 0.36645(10) 0.69855(6) 0.0522(4) Uani 1.000000 . . .
O1 O 0.12555(13) 0.36682(10) 0.35757(6) 0.0529(4) Uani 1.000000 . . .
O13 O 0.37209(11) 0.70372(12) 0.54589(6) 0.0521(4) Uani 1.000000 . . .
O14 O 0.26196(13) 0.84246(12) 0.58142(5) 0.0531(4) Uani 1.000000 . . .
O8 O -0.04589(16) 0.21447(13) 0.27386(7) 0.0483(5) Uani 0.903(4) D . 1
O7 O 0.10129(14) 0.31093(13) 0.23888(6) 0.0489(5) Uani 0.903(4) D . 1
O16 O 0.2719(6) 0.2032(5) 0.6137(3) 0.0363(13) Uani 0.360(6) D U 1
C23 C 0.44145(14) 0.59250(12) 0.74235(6) 0.0301(4) Uani 1.000000 . . .
C10 C 0.21094(14) 1.09127(13) 0.42359(6) 0.0323(4) Uani 1.000000 . . .
C3 C 0.09047(15) 0.58951(13) 0.40234(6) 0.0328(4) Uani 1.000000 . . .
C24 C 0.53737(14) 0.57081(13) 0.77501(6) 0.0328(4) Uani 1.000000 . . .
C18 C 0.40980(15) 0.51971(12) 0.71357(6) 0.0327(4) Uani 1.000000 . . .
C15 C 0.24337(15) 1.01770(13) 0.45177(6) 0.0338(4) Uani 1.000000 . . .
C4 C 0.06490(15) 0.51707(13) 0.37262(7) 0.0342(4) Uani 1.000000 . . .
C2 C 0.18193(15) 0.56837(13) 0.43752(6) 0.0344(4) Uani 1.000000 . . .
C16 C 0.18000(16) 0.93200(13) 0.44068(7) 0.0363(4) Uani 1.000000 . . .
C9 C 0.12042(15) 1.06690(13) 0.38839(6) 0.0335(4) Uani 1.000000 . . .
C22 C 0.38668(16) 0.67489(13) 0.73961(7) 0.0376(4) Uani 1.000000 . . .
H22 H 0.40887(16) 0.72502(13) 0.75920(7) 0.0451(5) Uiso 1.000000 R . .
C17 C 0.47995(16) 0.43701(13) 0.72167(7) 0.0379(5) Uani 1.000000 . . .
C1 C 0.13707(16) 0.43629(13) 0.38179(7) 0.0397(5) Uani 1.000000 . . .
C8 C 0.03334(17) 0.67060(14) 0.39831(7) 0.0420(5) Uani 1.000000 . . .
H8 H 0.05090(17) 0.72019(14) 0.41876(7) 0.0504(6) Uiso 1.000000 R . .
C29 C 0.17670(17) 0.02710(14) 0.27953(7) 0.0436(5) Uani 1.000000 . . .
H29a H 0.1815(11) 0.0007(5) 0.30937(8) 0.0655(7) Uiso 1.000000 GR . .
H29b H 0.1046(4) 0.0313(2) 0.2651(5) 0.0655(7) Uiso 1.000000 GR . .
H29c H 0.2135(8) -0.0128(3) 0.2618(5) 0.0655(7) Uiso 1.000000 GR . .
C19 C 0.32226(16) 0.52678(15) 0.68164(7) 0.0412(5) Uani 1.000000 . . .
H19 H 0.30066(16) 0.47675(15) 0.66191(7) 0.0494(6) Uiso 1.000000 R . .
C5 C -0.01939(17) 0.52370(15) 0.33860(7) 0.0442(5) Uani 1.000000 . . .
H5 H -0.03762(17) 0.47360(15) 0.31851(7) 0.0530(6) Uiso 1.000000 R . .
C21 C 0.29837(18) 0.68208(15) 0.70741(7) 0.0451(5) Uani 1.000000 . . .
H21 H 0.25973(18) 0.73793(15) 0.70492(7) 0.0541(6) Uiso 1.000000 R . .
C35 C 0.02125(16) 0.62788(16) 0.53680(8) 0.0445(5) Uani 1.000000 . . .
C20 C 0.26602(17) 0.60909(16) 0.67896(8) 0.0466(5) Uani 1.000000 . . .
H20 H 0.20501(17) 0.61498(16) 0.65740(8) 0.0559(6) Uiso 1.000000 R . .
C37 C -0.02154(17) 0.87191(15) 0.50652(8) 0.0448(5) Uani 1.000000 . . .
H37a H -0.0071(11) 0.9021(4) 0.53573(14) 0.0672(7) Uiso 1.000000 GR . .
H37b H 0.0091(10) 0.9082(4) 0.4852(4) 0.0672(7) Uiso 1.000000 GR . .
H37c H -0.0958(2) 0.86815(16) 0.4963(5) 0.0672(7) Uiso 1.000000 GR . .
C11 C 0.25729(16) 1.17729(14) 0.42931(7) 0.0407(5) Uani 1.000000 . . .
H11 H 0.23435(16) 1.22736(14) 0.40980(7) 0.0489(6) Uiso 1.000000 R . .
C30 C 0.32434(15) 0.11507(14) 0.30499(7) 0.0414(5) Uani 1.000000 . . .
H30a H 0.36305(15) 0.06897(14) 0.29066(7) 0.0497(6) Uiso 1.000000 R . .
H30b H 0.32787(15) 0.09660(14) 0.33642(7) 0.0497(6) Uiso 1.000000 R . .
C14 C 0.32574(17) 1.02772(16) 0.48637(7) 0.0447(5) Uani 1.000000 . . .
H14 H 0.34923(17) 0.97720(16) 0.50551(7) 0.0536(6) Uiso 1.000000 R . .
C36 C -0.02689(16) 0.72202(15) 0.53733(8) 0.0447(5) Uani 1.000000 . . .
H36a H -0.01631(16) 0.74654(15) 0.56808(8) 0.0537(6) Uiso 1.000000 R . .
H36b H -0.10143(16) 0.71822(15) 0.52576(8) 0.0537(6) Uiso 1.000000 R . .
C31 C 0.37056(16) 0.20944(15) 0.30286(8) 0.0448(5) Uani 1.000000 . . .
H31a H 0.44439(16) 0.20776(15) 0.31606(8) 0.0538(6) Uiso 1.000000 R . .
H31b H 0.36323(16) 0.22985(15) 0.27152(8) 0.0538(6) Uiso 1.000000 R . .
C12 C 0.33851(18) 1.18804(16) 0.46455(8) 0.0502(6) Uani 1.000000 . . .
H12 H 0.37075(18) 1.24689(16) 0.46971(8) 0.0602(7) Uiso 1.000000 R . .
C33 C 0.17357(19) 0.54605(15) 0.56167(8) 0.0495(5) Uani 1.000000 . . .
H33a H 0.1687(12) 0.5183(5) 0.53210(10) 0.0742(8) Uiso 1.000000 GR . .
H33b H 0.2458(4) 0.5527(2) 0.5755(5) 0.0742(8) Uiso 1.000000 GR . .
H33c H 0.1390(9) 0.5059(4) 0.5802(5) 0.0742(8) Uiso 1.000000 GR . .
C46 C 0.48947(19) 0.03331(16) 0.60621(8) 0.0527(6) Uani 1.000000 . . .
H46a H 0.4943(13) 0.0095(5) 0.63656(9) 0.0790(9) Uiso 1.000000 GR . .
H46b H 0.4175(4) 0.0349(3) 0.5915(6) 0.0790(9) Uiso 1.000000 GR . .
H46c H 0.5280(9) -0.0074(3) 0.5895(5) 0.0790(9) Uiso 1.000000 GR . .
C48 C 0.68096(17) 0.21751(16) 0.62500(8) 0.0497(6) Uani 1.000000 . . .
H48a H 0.66873(17) 0.23927(16) 0.59377(8) 0.0596(7) Uiso 1.000000 R . .
H48b H 0.75578(17) 0.21610(16) 0.63616(8) 0.0596(7) Uiso 1.000000 R . .
C6 C -0.07709(18) 0.60522(17) 0.33434(8) 0.0503(5) Uani 1.000000 . . .
H6 H -0.13509(18) 0.61084(17) 0.31115(8) 0.0603(6) Uiso 1.000000 R . .
C49 C 0.68452(17) 0.36478(16) 0.65876(9) 0.0509(6) Uani 1.000000 . . .
H49a H 0.6782(12) 0.3983(6) 0.63051(13) 0.0764(8) Uiso 1.000000 GR . .
H49b H 0.6537(9) 0.4017(5) 0.6798(5) 0.0764(8) Uiso 1.000000 GR . .
H49c H 0.7571(3) 0.35410(16) 0.6710(6) 0.0764(8) Uiso 1.000000 GR . .
C32 C 0.36682(18) 0.35998(15) 0.33241(8) 0.0502(6) Uani 1.000000 . . .
H32a H 0.3636(12) 0.3892(5) 0.30325(10) 0.0753(8) Uiso 1.000000 GR . .
H32b H 0.3315(9) 0.3992(4) 0.3510(5) 0.0753(8) Uiso 1.000000 GR . .
H32c H 0.4386(4) 0.35246(19) 0.3468(5) 0.0753(8) Uiso 1.000000 GR . .
C13 C 0.37337(18) 1.11457(18) 0.49231(8) 0.0544(6) Uani 1.000000 . . .
H13 H 0.43040(18) 1.12318(18) 0.51571(8) 0.0652(7) Uiso 1.000000 R . .
C7 C -0.05024(18) 0.67774(16) 0.36368(8) 0.0504(6) Uani 1.000000 . . .
H7 H -0.08941(18) 0.73330(16) 0.36015(8) 0.0605(7) Uiso 1.000000 R . .
C47 C 0.63664(16) 0.12262(16) 0.62755(9) 0.0498(6) Uani 1.000000 . . .
H47a H 0.67334(16) 0.07759(16) 0.61170(9) 0.0598(7) Uiso 1.000000 R . .
H47b H 0.64459(16) 0.10294(16) 0.65902(9) 0.0598(7) Uiso 1.000000 R . .
C40 C 0.4209(2) 0.77516(19) 0.57328(9) 0.0569(6) Uani 1.000000 . . .
C39 C 0.35345(19) 0.80262(19) 0.60478(8) 0.0576(6) Uani 1.000000 . . .
H39a H 0.33702(19) 0.74742(19) 0.62143(8) 0.0691(8) Uiso 1.000000 R . .
H39b H 0.38950(19) 0.84801(19) 0.62647(8) 0.0691(8) Uiso 1.000000 R . .
C27 C -0.0706(2) 0.2619(2) 0.23261(10) 0.0543(8) Uani 0.903(4) D . 1
H27a H -0.1426(2) 0.2833(2) 0.22796(10) 0.0651(9) Uiso 0.903(4) R . 1
H27b H -0.0632(2) 0.2193(2) 0.20800(10) 0.0651(9) Uiso 0.903(4) R . 1
C28 C -0.0979(3) 0.1287(3) 0.27342(14) 0.0570(11) Uani 0.903(4) D . 1
H28a H -0.0814(18) 0.0896(9) 0.2495(7) 0.0855(16) Uiso 0.903(4) GR . 1
H28b H -0.0765(17) 0.0972(10) 0.3020(4) 0.0855(16) Uiso 0.903(4) GR . 1
H28c H -0.1719(3) 0.1398(4) 0.2684(9) 0.0855(16) Uiso 0.903(4) GR . 1
C44 C 0.2607(7) 0.2724(7) 0.5669(3) 0.0482(19) Uani 0.360(6) D U 1
H44a H 0.2018(7) 0.3143(7) 0.5672(3) 0.058(2) Uiso 0.360(6) R . 1
H44b H 0.2415(7) 0.2312(7) 0.5408(3) 0.058(2) Uiso 0.360(6) R . 1
C26 C -0.0014(2) 0.34286(19) 0.23250(9) 0.0536(8) Uani 0.903(4) D . 1
H26a H -0.0187(2) 0.37623(19) 0.20380(9) 0.0643(9) Uiso 0.903(4) R . 1
H26b H -0.0099(2) 0.38634(19) 0.25664(9) 0.0643(9) Uiso 0.903(4) R . 1
C38 C 0.1922(2) 0.8647(2) 0.60997(9) 0.0631(7) Uani 1.000000 . . .
H38a H 0.1356(8) 0.9016(12) 0.5936(2) 0.0947(10) Uiso 1.000000 GR . .
H38b H 0.1651(12) 0.8074(2) 0.6206(5) 0.0947(10) Uiso 1.000000 GR . .
H38c H 0.2278(4) 0.9006(12) 0.6354(4) 0.0947(10) Uiso 1.000000 GR . .
C45 C 0.2255(8) 0.1293(7) 0.6027(4) 0.0436(19) Uani 0.360(6) D U 1
H45a H 0.243(3) 0.1070(19) 0.5747(9) 0.065(3) Uiso 0.360(6) GR . 1
H45b H 0.246(3) 0.0827(12) 0.6260(8) 0.065(3) Uiso 0.360(6) GR . 1
H45c H 0.1515(8) 0.1401(10) 0.5987(16) 0.065(3) Uiso 0.360(6) GR . 1
C41 C 0.43320(19) 0.6648(2) 0.51687(11) 0.0690(8) Uani 1.000000 . . .
H41a H 0.3952(7) 0.6147(10) 0.4995(5) 0.1036(12) Uiso 1.000000 GR . .
H41b H 0.4499(14) 0.7130(4) 0.4967(5) 0.1036(12) Uiso 1.000000 GR . .
H41c H 0.4966(8) 0.6399(14) 0.53444(11) 0.1036(12) Uiso 1.000000 GR . .
C25 C 0.1704(3) 0.3806(3) 0.23144(12) 0.0696(9) Uani 0.903(4) D . 1
H25a H 0.1744(15) 0.4282(9) 0.2546(5) 0.1044(14) Uiso 0.903(4) GR . 1
H25b H 0.2383(5) 0.3533(4) 0.2323(8) 0.1044(14) Uiso 0.903(4) GR . 1
H25c H 0.1466(11) 0.4089(12) 0.2022(4) 0.1044(14) Uiso 0.903(4) GR . 1
C42 C 0.4622(6) 0.4462(6) 0.5910(3) 0.0546(19) Uani 0.360(6) D U 1
H42a H 0.489(3) 0.476(3) 0.6195(5) 0.082(3) Uiso 0.360(6) GR . 1
H42b H 0.519(2) 0.4159(8) 0.5799(17) 0.082(3) Uiso 0.360(6) GR . 1
H42c H 0.4305(11) 0.493(2) 0.5694(14) 0.082(3) Uiso 0.360(6) GR . 1
H35a H -0.0127(19) 0.5871(18) 0.5540(8) 0.058(7) Uiso 1.000000 . . .
H40a H 0.431(2) 0.8303(19) 0.5541(9) 0.062(8) Uiso 1.000000 . . .
H35b H 0.015(2) 0.6056(19) 0.5048(10) 0.068(8) Uiso 1.000000 . . .
H40b H 0.489(2) 0.7505(18) 0.5889(9) 0.066(8) Uiso 1.000000 . . .
C0AA C 0.3473(6) 0.3313(5) 0.5583(3) 0.0489(17) Uani 0.360(6) D U 1
H0Aa H 0.4007(6) 0.2920(5) 0.5490(3) 0.059(2) Uiso 0.360(6) R . 1
H0Ab H 0.3227(6) 0.3761(5) 0.5341(3) 0.059(2) Uiso 0.360(6) R . 1
O0AA O 0.3877(4) 0.3785(4) 0.59698(16) 0.0490(15) Uani 0.360(6) D U 1
O8A O -0.0128(13) 0.2018(12) 0.2623(6) 0.039(3) Uiso 0.097(4) D . 2
O7A O 0.0941(11) 0.3613(11) 0.2561(5) 0.040(3) Uiso 0.097(4) D . 2
C27A C -0.0400(18) 0.2672(19) 0.2253(9) 0.039(3) Uiso 0.097(4) D . 2
H27c H -0.0736(18) 0.2348(19) 0.1980(9) 0.047(4) Uiso 0.097(4) R . 2
H27d H -0.0865(18) 0.3161(19) 0.2327(9) 0.047(4) Uiso 0.097(4) R . 2
C28A C -0.087(3) 0.132(3) 0.2631(14) 0.039(3) Uiso 0.097(4) D . 2
H28d H -0.079(11) 0.105(11) 0.293(2) 0.058(5) Uiso 0.097(4) GR . 2
H28e H -0.156(3) 0.159(4) 0.255(7) 0.058(5) Uiso 0.097(4) GR . 2
H28f H -0.079(11) 0.083(8) 0.242(5) 0.058(5) Uiso 0.097(4) GR . 2
C26A C 0.0590(17) 0.3072(15) 0.2196(8) 0.040(3) Uiso 0.097(4) D . 2
H26c H 0.0501(17) 0.3452(15) 0.1922(8) 0.048(4) Uiso 0.097(4) R . 2
H26d H 0.1086(17) 0.2570(15) 0.2171(8) 0.048(4) Uiso 0.097(4) R . 2
C25A C 0.1881(17) 0.4115(16) 0.2518(9) 0.040(3) Uiso 0.097(4) D . 2
H25d H 0.213(7) 0.447(9) 0.279(2) 0.060(5) Uiso 0.097(4) GR . 2
H25e H 0.241(4) 0.3670(17) 0.247(5) 0.060(5) Uiso 0.097(4) GR . 2
H25f H 0.174(3) 0.454(8) 0.226(3) 0.060(5) Uiso 0.097(4) GR . 2
O0AB O 0.3998(2) 0.3295(2) 0.57762(10) 0.0500(9) Uani 0.640(6) D U 2
O16A O 0.2919(4) 0.2055(4) 0.60493(18) 0.0601(14) Uani 0.640(6) D U 2
C44A C 0.2429(4) 0.2456(3) 0.56994(16) 0.0473(10) Uani 0.640(6) D U 2
H44c H 0.2502(4) 0.2105(3) 0.54285(16) 0.0568(13) Uiso 0.640(6) R . 2
H44d H 0.1692(4) 0.2509(3) 0.57127(16) 0.0568(13) Uiso 0.640(6) R . 2
C45A C 0.2346(5) 0.1153(4) 0.6154(2) 0.0558(16) Uani 0.640(6) D U 2
H45d H 0.238(2) 0.0685(8) 0.5924(6) 0.084(2) Uiso 0.640(6) GR . 2
H45e H 0.2669(16) 0.0910(13) 0.6445(5) 0.084(2) Uiso 0.640(6) GR . 2
H45f H 0.1627(8) 0.1300(6) 0.6156(10) 0.084(2) Uiso 0.640(6) GR . 2
C0AB C 0.2910(3) 0.3392(3) 0.57006(13) 0.0493(9) Uani 0.640(6) D U 2
H0Ac H 0.2708(3) 0.3779(3) 0.59375(13) 0.0592(11) Uiso 0.640(6) R . 2
H0Ad H 0.2670(3) 0.3702(3) 0.54114(13) 0.0592(11) Uiso 0.640(6) R . 2
C42A C 0.4471(4) 0.4161(4) 0.5732(2) 0.0678(13) Uani 0.640(6) D U 2
H42d H 0.438(3) 0.4566(10) 0.5980(7) 0.102(2) Uiso 0.640(6) GR . 2
H42e H 0.5203(7) 0.4067(4) 0.5736(13) 0.102(2) Uiso 0.640(6) GR . 2
H42f H 0.415(2) 0.4450(13) 0.5450(6) 0.102(2) Uiso 0.640(6) GR . 2


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
P2 C16 1.805(2) . ?
P2 C9 1.7984(19) . ?
P3 C24 1.8012(19) . ?
P3 C17 1.804(2) . ?
P1 C2 1.8046(19) . ?
P1 C1 1.806(2) . ?
Na2 O12 2.4095(15) . y
Na2 O11 2.4317(15) . y
Na2 O2 2.2946(15) . y
Na2 O4 2.2513(15) . y
Na2 O13 2.4047(17) . y
Na2 O14 2.4950(17) . y
Na1 O9 2.4394(15) . y
Na1 O3 2.3318(15) 1_545 y
Na1 O10 2.5210(16) . y
Na1 O1 2.2687(15) . y
Na1 O8 2.448(2) . y
Na1 O7 2.4809(19) . y
Na1 O8A 2.293(16) . y
Na1 O7A 2.472(14) . y
Na3 O6 2.3013(15) 2_646 y
Na3 O18 2.4560(15) . y
Na3 O17 2.5160(16) . y
Na3 O5 2.2811(15) . y
Na3 O16 2.503(9) . y
Na3 O0AA 2.529(5) . y
Na3 O0AB 2.481(3) . y
Na3 O16A 2.363(6) . y
O12 C37 1.422(2) . ?
O12 C36 1.422(2) . ?
O9 C29 1.421(2) . ?
O9 C30 1.415(2) . ?
O11 C35 1.425(3) . ?
O11 C33 1.418(3) . ?
O6 C24 1.237(2) . ?
O18 C48 1.418(2) . ?
O18 C49 1.420(3) . ?
O3 C9 1.236(2) . ?
O10 C31 1.415(2) . ?
O10 C32 1.419(2) . ?
O2 C2 1.231(2) . ?
O17 C46 1.421(3) . ?
O17 C47 1.423(3) . ?
O4 C16 1.231(2) . ?
O5 C17 1.235(2) . ?
O1 C1 1.238(2) . ?
O13 C40 1.408(3) . ?
O13 C41 1.423(3) . ?
O14 C39 1.414(3) . ?
O14 C38 1.421(3) . ?
O8 C27 1.419(3) . ?
O8 C28 1.415(4) . ?
O7 C26 1.419(3) . ?
O7 C25 1.407(4) . ?
O16 C44 1.729(12) . ?
O16 C45 1.244(13) . ?
C23 C24 1.501(3) . ?
C23 C18 1.384(3) . ?
C23 C22 1.387(3) . ?
C10 C15 1.384(3) . ?
C10 C9 1.501(3) . ?
C10 C11 1.381(3) . ?
C3 C4 1.385(3) . ?
C3 C2 1.499(3) . ?
C3 C8 1.386(3) . ?
C18 C17 1.505(3) . ?
C18 C19 1.378(3) . ?
C15 C16 1.498(3) . ?
C15 C14 1.383(3) . ?
C4 C1 1.501(3) . ?
C4 C5 1.385(3) . ?
C22 H22 0.9500 . ?
C22 C21 1.390(3) . ?
C8 H8 0.9500 . ?
C8 C7 1.391(3) . ?
C29 H29a 0.9800 . ?
C29 H29b 0.9800 . ?
C29 H29c 0.9800 . ?
C19 H19 0.9500 . ?
C19 C20 1.396(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.395(3) . ?
C21 H21 0.9500 . ?
C21 C20 1.382(3) . ?
C35 C36 1.501(3) . ?
C35 H35a 0.96(3) . ?
C35 H35b 1.02(3) . ?
C20 H20 0.9500 . ?
C37 H37a 0.9800 . ?
C37 H37b 0.9800 . ?
C37 H37c 0.9800 . ?
C11 H11 0.9500 . ?
C11 C12 1.387(3) . ?
C30 H30a 0.9900 . ?
C30 H30b 0.9900 . ?
C30 C31 1.498(3) . ?
C14 H14 0.9500 . ?
C14 C13 1.399(3) . ?
C36 H36a 0.9900 . ?
C36 H36b 0.9900 . ?
C31 H31a 0.9900 . ?
C31 H31b 0.9900 . ?
C12 H12 0.9500 . ?
C12 C13 1.382(4) . ?
C33 H33a 0.9800 . ?
C33 H33b 0.9800 . ?
C33 H33c 0.9800 . ?
C46 H46a 0.9800 . ?
C46 H46b 0.9800 . ?
C46 H46c 0.9800 . ?
C48 H48a 0.9900 . ?
C48 H48b 0.9900 . ?
C48 C47 1.496(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.381(3) . ?
C49 H49a 0.9800 . ?
C49 H49b 0.9800 . ?
C49 H49c 0.9800 . ?
C32 H32a 0.9800 . ?
C32 H32b 0.9800 . ?
C32 H32c 0.9800 . ?
C13 H13 0.9500 . ?
C7 H7 0.9500 . ?
C47 H47a 0.9900 . ?
C47 H47b 0.9900 . ?
C40 C39 1.484(4) . ?
C40 H40a 1.01(3) . ?
C40 H40b 1.01(3) . ?
C39 H39a 0.9900 . ?
C39 H39b 0.9900 . ?
C27 H27a 0.9900 . ?
C27 H27b 0.9900 . ?
C27 C26 1.485(4) . ?
C28 H28a 0.9800 . ?
C28 H28b 0.9800 . ?
C28 H28c 0.9800 . ?
C44 H44a 0.9900 . ?
C44 H44b 0.9900 . ?
C44 C0AA 1.492(10) . ?
C26 H26a 0.9900 . ?
C26 H26b 0.9900 . ?
C38 H38a 0.9800 . ?
C38 H38b 0.9800 . ?
C38 H38c 0.9800 . ?
C45 H45a 0.9800 . ?
C45 H45b 0.9800 . ?
C45 H45c 0.9800 . ?
C41 H41a 0.9800 . ?
C41 H41b 0.9800 . ?
C41 H41c 0.9800 . ?
C25 H25a 0.9800 . ?
C25 H25b 0.9800 . ?
C25 H25c 0.9800 . ?
C42 H42a 0.9800 . ?
C42 H42b 0.9800 . ?
C42 H42c 0.9800 . ?
C42 O0AA 1.425(8) . ?
C0AA H0Aa 0.9900 . ?
C0AA H0Ab 0.9900 . ?
C0AA O0AA 1.384(9) . ?
O8A C27A 1.47(3) . ?
O8A C28A 1.42(3) . ?
O7A C26A 1.37(2) . ?
O7A C25A 1.47(2) . ?
C27A H27c 0.9900 . ?
C27A H27d 0.9900 . ?
C27A C26A 1.48(3) . ?
C28A H28d 0.9800 . ?
C28A H28e 0.9800 . ?
C28A H28f 0.9800 . ?
C26A H26c 0.9900 . ?
C26A H26d 0.9900 . ?
C25A H25d 0.9800 . ?
C25A H25e 0.9800 . ?
C25A H25f 0.9800 . ?
O0AB C0AB 1.429(5) . ?
O0AB C42A 1.414(5) . ?
O16A C44A 1.283(8) . ?
O16A C45A 1.567(8) . ?
C44A H44c 0.9900 . ?
C44A H44d 0.9900 . ?
C44A C0AB 1.492(6) . ?
C45A H45d 0.9800 . ?
C45A H45e 0.9800 . ?
C45A H45f 0.9800 . ?
C0AB H0Ac 0.9900 . ?
C0AB H0Ad 0.9900 . ?
C42A H42d 0.9800 . ?
C42A H42e 0.9800 . ?
C42A H42f 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
C9 P2 C16 90.05(9) . . ?
C17 P3 C24 90.03(9) . . ?
C1 P1 C2 89.91(9) . . ?
O11 Na2 O12 70.40(5) . . y
O2 Na2 O12 108.06(6) . . y
O2 Na2 O11 84.62(6) . . y
O4 Na2 O12 86.89(6) . . y
O4 Na2 O11 156.38(6) . . y
O4 Na2 O2 96.83(6) . . y
O13 Na2 O12 158.17(6) . . y
O13 Na2 O11 92.59(6) . . y
O13 Na2 O2 82.93(6) . . y
O13 Na2 O4 111.00(6) . . y
O14 Na2 O12 95.88(6) . . y
O14 Na2 O11 90.63(6) . . y
O14 Na2 O2 152.26(6) . . y
O14 Na2 O4 98.29(6) . . y
O14 Na2 O13 69.97(6) . . y
O3 Na1 O9 85.61(5) 1_545 . y
O10 Na1 O9 68.58(5) . . y
O10 Na1 O3 113.72(6) . 1_545 y
O1 Na1 O9 151.55(6) . . y
O1 Na1 O3 100.80(6) . 1_545 y
O1 Na1 O10 83.62(6) . . y
O8 Na1 O9 101.15(7) . . y
O8 Na1 O3 82.25(6) . 1_545 y
O8 Na1 O10 159.26(7) . . y
O8 Na1 O1 107.16(7) . . y
O7 Na1 O9 86.40(6) . . y
O7 Na1 O3 147.32(7) . 1_545 y
O7 Na1 O10 92.50(6) . . y
O7 Na1 O1 101.23(7) . . y
O7 Na1 O8 68.34(7) . . y
O8A Na1 O9 88.0(5) . . y
O8A Na1 O3 88.3(4) . 1_545 y
O8A Na1 O10 145.3(5) . . y
O8A Na1 O1 119.7(5) . . y
O8A Na1 O8 15.0(5) . . y
O8A Na1 O7 59.7(4) . . y
O7A Na1 O9 105.9(4) . . y
O7A Na1 O3 154.3(3) . 1_545 y
O7A Na1 O10 91.9(3) . . y
O7A Na1 O1 80.1(4) . . y
O7A Na1 O8 73.1(3) . . y
O7A Na1 O7 21.2(4) . . y
O7A Na1 O8A 69.7(5) . . y
O18 Na3 O6 112.61(6) . 2_646 y
O17 Na3 O6 85.72(6) . 2_646 y
O17 Na3 O18 68.68(5) . . y
O5 Na3 O6 98.64(6) . 2_646 y
O5 Na3 O18 83.67(6) . . y
O5 Na3 O17 151.34(6) . . y
O16 Na3 O6 81.25(17) . 2_646 y
O16 Na3 O18 155.66(18) . . y
O16 Na3 O17 93.7(2) . . y
O16 Na3 O5 115.0(2) . . y
O0AA Na3 O6 152.16(12) . 2_646 y
O0AA Na3 O18 94.92(11) . . y
O0AA Na3 O17 109.14(14) . . y
O0AA Na3 O5 79.70(14) . . y
O0AA Na3 O16 74.6(2) . . y
O0AB Na3 O6 149.75(8) . 2_646 y
O0AB Na3 O18 92.30(8) . . y
O0AB Na3 O17 87.88(9) . . y
O0AB Na3 O5 101.04(9) . . y
O0AB Na3 O16 69.68(17) . . y
O0AB Na3 O0AA 21.93(11) . . y
O16A Na3 O6 87.33(12) . 2_646 y
O16A Na3 O18 146.54(14) . . y
O16A Na3 O17 87.31(15) . . y
O16A Na3 O5 121.06(15) . . y
O16A Na3 O16 9.1(2) . . y
O16A Na3 O0AA 70.57(16) . . y
O16A Na3 O0AB 62.82(14) . . y
C37 O12 Na2 124.10(12) . . ?
C36 O12 Na2 113.35(12) . . ?
C36 O12 C37 112.37(15) . . ?
C29 O9 Na1 117.30(12) . . ?
C30 O9 Na1 109.86(11) . . ?
C30 O9 C29 111.57(15) . . ?
C35 O11 Na2 104.95(12) . . ?
C33 O11 Na2 115.68(12) . . ?
C33 O11 C35 111.11(16) . . ?
C24 O6 Na3 147.62(13) . 2_656 ?
C48 O18 Na3 114.36(13) . . ?
C49 O18 Na3 127.79(12) . . ?
C49 O18 C48 112.27(16) . . ?
C9 O3 Na1 141.61(14) . 1_565 ?
C31 O10 Na1 111.76(12) . . ?
C32 O10 Na1 126.64(13) . . ?
C32 O10 C31 112.29(16) . . ?
C2 O2 Na2 155.76(14) . . ?
C46 O17 Na3 117.60(13) . . ?
C47 O17 Na3 105.93(12) . . ?
C47 O17 C46 110.13(17) . . ?
C16 O4 Na2 162.52(14) . . ?
C17 O5 Na3 170.40(14) . . ?
C1 O1 Na1 171.84(15) . . ?
C40 O13 Na2 110.58(15) . . ?
C41 O13 Na2 117.11(15) . . ?
C41 O13 C40 113.96(18) . . ?
C39 O14 Na2 108.69(14) . . ?
C38 O14 Na2 118.77(14) . . ?
C38 O14 C39 112.22(19) . . ?
C27 O8 Na1 114.69(16) . . ?
C28 O8 Na1 123.5(2) . . ?
C28 O8 C27 112.3(3) . . ?
C26 O7 Na1 103.71(15) . . ?
C25 O7 Na1 117.01(19) . . ?
C25 O7 C26 112.7(2) . . ?
C44 O16 Na3 98.5(4) . . ?
C45 O16 Na3 135.5(7) . . ?
C45 O16 C44 107.9(8) . . ?
C18 C23 C24 112.78(16) . . ?
C22 C23 C24 126.19(17) . . ?
C22 C23 C18 121.03(18) . . ?
C9 C10 C15 112.60(16) . . ?
C11 C10 C15 121.86(19) . . ?
C11 C10 C9 125.51(18) . . ?
C2 C3 C4 112.77(17) . . ?
C8 C3 C4 120.83(19) . . ?
C8 C3 C2 126.40(18) . . ?
O6 C24 P3 126.37(15) . . ?
C23 C24 P3 112.32(13) . . ?
C23 C24 O6 121.31(17) . . ?
C17 C18 C23 112.87(18) . . ?
C19 C18 C23 120.86(18) . . ?
C19 C18 C17 126.28(18) . . ?
C16 C15 C10 113.11(18) . . ?
C14 C15 C10 120.58(19) . . ?
C14 C15 C16 126.31(18) . . ?
C1 C4 C3 112.97(18) . . ?
C5 C4 C3 120.55(18) . . ?
C5 C4 C1 126.48(18) . . ?
O2 C2 P1 126.79(16) . . ?
C3 C2 P1 112.28(13) . . ?
C3 C2 O2 120.93(17) . . ?
O4 C16 P2 126.62(17) . . ?
C15 C16 P2 111.95(14) . . ?
C15 C16 O4 121.4(2) . . ?
O3 C9 P2 126.66(16) . . ?
C10 C9 P2 112.29(13) . . ?
C10 C9 O3 121.05(17) . . ?
H22 C22 C23 120.93(12) . . ?
C21 C22 C23 118.14(18) . . ?
C21 C22 H22 120.93(12) . . ?
O5 C17 P3 127.03(17) . . ?
C18 C17 P3 112.00(14) . . ?
C18 C17 O5 121.0(2) . . ?
O1 C1 P1 127.28(17) . . ?
C4 C1 P1 112.03(14) . . ?
C4 C1 O1 120.7(2) . . ?
H8 C8 C3 120.74(12) . . ?
C7 C8 C3 118.53(19) . . ?
C7 C8 H8 120.74(12) . . ?
H29a C29 O9 109.5 . . ?
H29b C29 O9 109.5 . . ?
H29b C29 H29a 109.5 . . ?
H29c C29 O9 109.5 . . ?
H29c C29 H29a 109.5 . . ?
H29c C29 H29b 109.5 . . ?
H19 C19 C18 120.74(11) . . ?
C20 C19 C18 118.52(19) . . ?
C20 C19 H19 120.74(13) . . ?
H5 C5 C4 120.57(12) . . ?
C6 C5 C4 118.9(2) . . ?
C6 C5 H5 120.57(13) . . ?
H21 C21 C22 119.54(12) . . ?
C20 C21 C22 120.91(19) . . ?
C20 C21 H21 119.54(13) . . ?
C36 C35 O11 108.50(17) . . ?
H35a C35 O11 108.5(15) . . ?
H35a C35 C36 107.7(15) . . ?
H35b C35 O11 110.9(16) . . ?
H35b C35 C36 109.5(16) . . ?
H35b C35 H35a 112(2) . . ?
C21 C20 C19 120.5(2) . . ?
H20 C20 C19 119.73(13) . . ?
H20 C20 C21 119.73(13) . . ?
H37a C37 O12 109.5 . . ?
H37b C37 O12 109.5 . . ?
H37b C37 H37a 109.5 . . ?
H37c C37 O12 109.5 . . ?
H37c C37 H37a 109.5 . . ?
H37c C37 H37b 109.5 . . ?
H11 C11 C10 121.17(13) . . ?
C12 C11 C10 117.7(2) . . ?
C12 C11 H11 121.17(13) . . ?
H30a C30 O9 109.84(10) . . ?
H30b C30 O9 109.84(11) . . ?
H30b C30 H30a 108.3 . . ?
C31 C30 O9 109.22(17) . . ?
C31 C30 H30a 109.84(11) . . ?
C31 C30 H30b 109.84(13) . . ?
H14 C14 C15 121.05(12) . . ?
C13 C14 C15 117.9(2) . . ?
C13 C14 H14 121.05(14) . . ?
C35 C36 O12 107.26(17) . . ?
H36a C36 O12 110.26(11) . . ?
H36a C36 C35 110.26(13) . . ?
H36b C36 O12 110.26(11) . . ?
H36b C36 C35 110.26(11) . . ?
H36b C36 H36a 108.5 . . ?
C30 C31 O10 108.10(16) . . ?
H31a C31 O10 110.08(11) . . ?
H31a C31 C30 110.08(11) . . ?
H31b C31 O10 110.08(12) . . ?
H31b C31 C30 110.08(13) . . ?
H31b C31 H31a 108.4 . . ?
H12 C12 C11 119.44(13) . . ?
C13 C12 C11 121.1(2) . . ?
C13 C12 H12 119.44(14) . . ?
H33a C33 O11 109.5 . . ?
H33b C33 O11 109.5 . . ?
H33b C33 H33a 109.5 . . ?
H33c C33 O11 109.5 . . ?
H33c C33 H33a 109.5 . . ?
H33c C33 H33b 109.5 . . ?
H46a C46 O17 109.5 . . ?
H46b C46 O17 109.5 . . ?
H46b C46 H46a 109.5 . . ?
H46c C46 O17 109.5 . . ?
H46c C46 H46a 109.5 . . ?
H46c C46 H46b 109.5 . . ?
H48a C48 O18 110.06(12) . . ?
H48b C48 O18 110.06(12) . . ?
H48b C48 H48a 108.4 . . ?
C47 C48 O18 108.20(17) . . ?
C47 C48 H48a 110.06(14) . . ?
C47 C48 H48b 110.06(12) . . ?
H6 C6 C5 119.86(13) . . ?
C7 C6 C5 120.3(2) . . ?
C7 C6 H6 119.86(14) . . ?
H49a C49 O18 109.5 . . ?
H49b C49 O18 109.5 . . ?
H49b C49 H49a 109.5 . . ?
H49c C49 O18 109.5 . . ?
H49c C49 H49a 109.5 . . ?
H49c C49 H49b 109.5 . . ?
H32a C32 O10 109.5 . . ?
H32b C32 O10 109.5 . . ?
H32b C32 H32a 109.5 . . ?
H32c C32 O10 109.5 . . ?
H32c C32 H32a 109.5 . . ?
H32c C32 H32b 109.5 . . ?
C12 C13 C14 120.8(2) . . ?
H13 C13 C14 119.58(14) . . ?
H13 C13 C12 119.58(14) . . ?
C6 C7 C8 120.9(2) . . ?
H7 C7 C8 119.54(12) . . ?
H7 C7 C6 119.54(14) . . ?
C48 C47 O17 109.16(19) . . ?
H47a C47 O17 109.85(11) . . ?
H47a C47 C48 109.85(11) . . ?
H47b C47 O17 109.85(12) . . ?
H47b C47 C48 109.85(14) . . ?
H47b C47 H47a 108.3 . . ?
C39 C40 O13 108.3(2) . . ?
H40a C40 O13 109.0(15) . . ?
H40a C40 C39 109.1(15) . . ?
H40b C40 O13 107.5(16) . . ?
H40b C40 C39 112.6(15) . . ?
H40b C40 H40a 110(2) . . ?
C40 C39 O14 110.2(2) . . ?
H39a C39 O14 109.62(13) . . ?
H39a C39 C40 109.62(15) . . ?
H39b C39 O14 109.62(13) . . ?
H39b C39 C40 109.62(13) . . ?
H39b C39 H39a 108.1 . . ?
H27a C27 O8 109.72(13) . . ?
H27b C27 O8 109.72(16) . . ?
H27b C27 H27a 108.2 . . ?
C26 C27 O8 109.7(2) . . ?
C26 C27 H27a 109.72(15) . . ?
C26 C27 H27b 109.72(16) . . ?
H28a C28 O8 109.5 . . ?
H28b C28 O8 109.5 . . ?
H28b C28 H28a 109.5 . . ?
H28c C28 O8 109.5 . . ?
H28c C28 H28a 109.5 . . ?
H28c C28 H28b 109.5 . . ?
H44a C44 O16 107.0(4) . . ?
H44b C44 O16 107.0(4) . . ?
H44b C44 H44a 106.7 . . ?
C0AA C44 O16 121.5(7) . . ?
C0AA C44 H44a 107.0(5) . . ?
C0AA C44 H44b 107.0(5) . . ?
C27 C26 O7 109.0(2) . . ?
H26a C26 O7 109.89(13) . . ?
H26a C26 C27 109.89(15) . . ?
H26b C26 O7 109.89(15) . . ?
H26b C26 C27 109.89(16) . . ?
H26b C26 H26a 108.3 . . ?
H38a C38 O14 109.5 . . ?
H38b C38 O14 109.5 . . ?
H38b C38 H38a 109.5 . . ?
H38c C38 O14 109.5 . . ?
H38c C38 H38a 109.5 . . ?
H38c C38 H38b 109.5 . . ?
H45a C45 O16 109.5 . . ?
H45b C45 O16 109.5 . . ?
H45b C45 H45a 109.5 . . ?
H45c C45 O16 109.5 . . ?
H45c C45 H45a 109.5 . . ?
H45c C45 H45b 109.5 . . ?
H41a C41 O13 109.5 . . ?
H41b C41 O13 109.5 . . ?
H41b C41 H41a 109.5 . . ?
H41c C41 O13 109.5 . . ?
H41c C41 H41a 109.5 . . ?
H41c C41 H41b 109.5 . . ?
H25a C25 O7 109.5 . . ?
H25b C25 O7 109.5 . . ?
H25b C25 H25a 109.5 . . ?
H25c C25 O7 109.5 . . ?
H25c C25 H25a 109.5 . . ?
H25c C25 H25b 109.5 . . ?
H42b C42 H42a 109.5 . . ?
H42c C42 H42a 109.5 . . ?
H42c C42 H42b 109.5 . . ?
O0AA C42 H42a 109.5 . . ?
O0AA C42 H42b 109.5 . . ?
O0AA C42 H42c 109.5 . . ?
H0Aa C0AA C44 110.0(5) . . ?
H0Ab C0AA C44 110.0(5) . . ?
H0Ab C0AA H0Aa 108.3 . . ?
O0AA C0AA C44 108.6(7) . . ?
O0AA C0AA H0Aa 110.0(4) . . ?
O0AA C0AA H0Ab 110.0(4) . . ?
C42 O0AA Na3 116.1(4) . . ?
C0AA O0AA Na3 101.7(4) . . ?
C0AA O0AA C42 113.3(5) . . ?
C27A O8A Na1 115.7(13) . . ?
C28A O8A Na1 130(2) . . ?
C28A O8A C27A 113(2) . . ?
C26A O7A Na1 99.9(13) . . ?
C25A O7A Na1 111.2(12) . . ?
C25A O7A C26A 111.9(16) . . ?
H27c C27A O8A 110.9(13) . . ?
H27d C27A O8A 110.9(13) . . ?
H27d C27A H27c 109.0 . . ?
C26A C27A O8A 104.1(19) . . ?
C26A C27A H27c 110.9(14) . . ?
C26A C27A H27d 110.9(15) . . ?
H28d C28A O8A 109.5 . . ?
H28e C28A O8A 109.5 . . ?
H28e C28A H28d 109.5 . . ?
H28f C28A O8A 109.5 . . ?
H28f C28A H28d 109.5 . . ?
H28f C28A H28e 109.5 . . ?
C27A C26A O7A 107.6(19) . . ?
H26c C26A O7A 110.2(11) . . ?
H26c C26A C27A 110.2(14) . . ?
H26d C26A O7A 110.2(12) . . ?
H26d C26A C27A 110.2(14) . . ?
H26d C26A H26c 108.5 . . ?
H25d C25A O7A 109.5 . . ?
H25e C25A O7A 109.5 . . ?
H25e C25A H25d 109.5 . . ?
H25f C25A O7A 109.5 . . ?
H25f C25A H25d 109.5 . . ?
H25f C25A H25e 109.5 . . ?
C0AB O0AB Na3 107.1(2) . . ?
C42A O0AB Na3 117.2(3) . . ?
C42A O0AB C0AB 110.6(3) . . ?
C44A O16A Na3 129.0(4) . . ?
C45A O16A Na3 120.3(4) . . ?
C45A O16A C44A 110.6(5) . . ?
H44c C44A O16A 110.8(3) . . ?
H44d C44A O16A 110.8(4) . . ?
H44d C44A H44c 108.9 . . ?
C0AB C44A O16A 104.7(4) . . ?
C0AB C44A H44c 110.8(2) . . ?
C0AB C44A H44d 110.8(2) . . ?
H45d C45A O16A 109.5 . . ?
H45e C45A O16A 109.5 . . ?
H45e C45A H45d 109.5 . . ?
H45f C45A O16A 109.5 . . ?
H45f C45A H45d 109.5 . . ?
H45f C45A H45e 109.5 . . ?
C44A C0AB O0AB 109.4(3) . . ?
H0Ac C0AB O0AB 109.8(2) . . ?
H0Ac C0AB C44A 109.8(3) . . ?
H0Ad C0AB O0AB 109.8(2) . . ?
H0Ad C0AB C44A 109.8(2) . . ?
H0Ad C0AB H0Ac 108.2 . . ?
H42d C42A O0AB 109.5 . . ?
H42e C42A O0AB 109.5 . . ?
H42e C42A H42d 109.5 . . ?
H42f C42A O0AB 109.5 . . ?
H42f C42A H42d 109.5 . . ?
H42f C42A H42e 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
P2 C16 O4 Na2 -88.9(4) . . . . ?
P2 C16 C15 C10 -0.16(14) . . . . ?
P2 C16 C15 C14 178.98(14) . . . . ?
P2 C9 O3 Na1 -139.09(10) . . . 1_565 ?
P2 C9 C10 C15 0.99(14) . . . . ?
P2 C9 C10 C11 -177.17(13) . . . . ?
P3 C24 O6 Na3 -146.32(9) . . . 2_656 ?
P3 C24 C23 C18 0.33(14) . . . . ?
P3 C24 C23 C22 -179.85(13) . . . . ?
P3 C17 C18 C23 0.79(14) . . . . ?
P3 C17 C18 C19 -179.06(13) . . . . ?
P1 C2 O2 Na2 -156.82(10) . . . . ?
P1 C2 C3 C4 1.47(14) . . . . ?
P1 C2 C3 C8 -179.32(14) . . . . ?
P1 C1 C4 C3 1.82(15) . . . . ?
P1 C1 C4 C5 -178.55(14) . . . . ?
Na2 O12 C36 C35 -35.23(13) . . . . ?
Na2 O11 C35 C36 -59.47(12) . . . . ?
Na2 O2 C2 C3 22.3(3) . . . . ?
Na2 O4 C16 C15 91.5(5) . . . . ?
Na2 O13 C40 C39 51.32(15) . . . . ?
Na2 O14 C39 C40 43.03(15) . . . . ?
Na1 O9 C30 C31 -54.67(12) . . . . ?
Na1 O3 C9 C10 40.5(2) 1_565 . . . ?
Na1 O10 C31 C30 -39.64(13) . . . . ?
Na1 O8 C27 C26 -22.90(17) . . . . ?
Na1 O7 C26 C27 -63.04(17) . . . . ?
Na1 O8A C27A C26A 30.3(14) . . . . ?
Na1 O7A C26A C27A 67.5(13) . . . . ?
Na3 O6 C24 C23 32.9(2) 2_656 . . . ?
Na3 O18 C48 C47 -36.61(14) . . . . ?
Na3 O17 C47 C48 -57.05(13) . . . . ?
Na3 O0AA C0AA C44 62.5(5) . . . . ?
Na3 O0AB C0AB C44A -57.5(3) . . . . ?
Na3 O16A C44A C0AB -16.0(5) . . . . ?
O12 C36 C35 O11 65.49(18) . . . . ?
O9 C30 C31 O10 64.35(18) . . . . ?
O6 C24 C23 C18 -179.02(18) . . . . ?
O6 C24 C23 C22 0.8(2) . . . . ?
O18 C48 C47 O17 64.8(2) . . . . ?
O3 C9 C10 C15 -178.65(18) . . . . ?
O3 C9 C10 C11 3.2(2) . . . . ?
O2 C2 C3 C4 -177.76(18) . . . . ?
O2 C2 C3 C8 1.5(2) . . . . ?
O4 C16 C15 C10 179.46(18) . . . . ?
O4 C16 C15 C14 -1.4(2) . . . . ?
O5 C17 C18 C23 -179.43(18) . . . . ?
O5 C17 C18 C19 0.7(2) . . . . ?
O1 C1 C4 C3 -178.59(19) . . . . ?
O1 C1 C4 C5 1.0(2) . . . . ?
O13 C40 C39 O14 -65.4(2) . . . . ?
O8 C27 C26 O7 59.8(2) . . . . ?
O16 C44 C0AA O0AA -46.9(9) . . . . ?
C23 C18 C19 C20 -0.0(2) . . . . ?
C23 C22 C21 C20 0.1(2) . . . . ?
C10 C15 C14 C13 1.2(2) . . . . ?
C10 C11 C12 C13 1.5(2) . . . . ?
C3 C4 C5 C6 1.1(2) . . . . ?
C3 C8 C7 C6 1.1(2) . . . . ?
C18 C19 C20 C21 0.8(2) . . . . ?
C15 C14 C13 C12 0.4(2) . . . . ?
C4 C5 C6 C7 -0.1(2) . . . . ?
C22 C21 C20 C19 -0.8(3) . . . . ?
C8 C7 C6 C5 -1.1(3) . . . . ?
C11 C12 C13 C14 -1.8(3) . . . . ?
C44 C0AA O0AA C42 -172.1(7) . . . . ?
O8A C27A C26A O7A -69(2) . . . . ?
O0AB C0AB C44A O16A 48.3(5) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_id
Na1 O8 1 1
Na1 O7 1 2
Na1 C27 1 9
Na1 C28 1 11
Na1 C26 1 12
Na1 C25 1 13
Na1 O8A 1 1
Na1 O7A 1 2
Na1 C27A 1 9
Na1 C28A 1 11
Na1 C26A 1 12
Na1 C25A 1 13
O8 C27 1 3
O8 C28 1 4
O8 C26 1 14
O7 C27 1 15
O7 C26 1 5
O7 C25 1 7
O16 C44 1 18
O16 C45 1 20
O16 C0AA 1 24
C27 C28 1 8
C27 C26 1 6
C44 C45 1 21
C44 C0AA 1 17
C44 O0AA 1 19
C26 C25 1 10
C42 C0AA 1 16
C42 O0AA 1 22
C0AA O0AA 1 23
O8A C27A 1 3
O8A C28A 1 4
O8A C26A 1 14
O7A C27A 1 15
O7A C26A 1 5
O7A C25A 1 7
C27A C28A 1 8
C27A C26A 1 6
C26A C25A 1 10
O16A C44A 1 18
O16A C45A 1 20
O16A C0AB 1 24
C44A O0AB 1 19
C44A C45A 1 21
C44A C0AB 1 17
C0AB O0AB 1 23
C42A O0AB 1 22
C42A C0AB 1 16

loop_
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
_restr_equal_distance_class_average
_restr_equal_distance_class_esd
_restr_equal_distance_class_diff_max
1 0.0200 2.3704 0.0777 0.0777
2 0.0200 2.4765 0.0043 0.0043
3 0.0200 1.4426 0.0231 0.0231
4 0.0200 1.4171 0.0020 0.0020
5 0.0200 1.3954 0.0238 0.0238
6 0.0200 1.4802 0.0049 0.0049
7 0.0200 1.4389 0.0318 0.0318
8 0.0400 2.3827 0.0287 0.0287
9 0.0400 3.2579 0.0453 0.0453
10 0.0400 2.3542 0.0018 0.0018
11 0.0400 3.4128 0.0254 0.0254
12 0.0400 3.0816 0.0549 0.0549
13 0.0400 3.3323 0.0300 0.0300
14 0.0400 2.3473 0.0285 0.0285
15 0.0400 2.3309 0.0332 0.0332
16 0.0400 2.3418 0.0046 0.0046
17 0.0200 1.4919 0.0001 0.0001
18 0.0200 1.5061 0.2226 0.2226
19 0.0400 2.3603 0.0238 0.0238
20 0.0200 1.4057 0.1617 0.1617
21 0.0400 2.3844 0.0354 0.0354
22 0.0200 1.4198 0.0054 0.0054
23 0.0200 1.4063 0.0222 0.0222
24 0.0400 2.5062 0.3057 0.3057

loop_
_restr_RIGU_atom_site_label_1
_restr_RIGU_atom_site_label_2
_restr_RIGU_target_weight_param
_restr_RIGU_U13_diff
_restr_RIGU_U23_diff
_restr_RIGU_U33_diff
O16 C44 0.001000 -0.000856 -0.002472 -0.000443
O16 C45 0.001000 -0.000594 -0.000512 -0.001533
O16 C0AA 0.001000 -0.006062 -0.001807 -0.001956
C44 C45 0.001000 0.000577 -0.001187 -0.001136
C44 C0AA 0.001000 0.000354 0.001368 0.001359
C44 O0AA 0.001000 -0.007806 0.005656 -0.000350
C42 C0AA 0.001000 -0.000734 -0.003148 -0.000573
C42 O0AA 0.001000 -0.001017 -0.000286 0.000470
C0AA O0AA 0.001000 -0.000341 0.000664 0.000716
O0AB C44A 0.001000 -0.005800 -0.006984 0.002211
O0AB C0AB 0.001000 -0.002120 -0.001669 -0.001625
O0AB C42A 0.001000 0.003141 0.000342 -0.001850
O16A C44A 0.001000 0.002272 -0.001396 0.001035
O16A C45A 0.001000 -0.006299 0.001660 -0.001158
O16A C0AB 0.001000 0.002211 0.005975 0.004285
C44A C45A 0.001000 0.004152 -0.004149 -0.002765
C44A C0AB 0.001000 -0.002880 0.003136 0.001119
C0AB C42A 0.001000 -0.013874 0.004285 -0.004697

loop_
_restr_U_similar_atom_site_label_1
_restr_U_similar_atom_site_label_2
_restr_U_similar_weight_param
O8A C27A 0.0010
O8A C28A 0.0010
O7A C26A 0.0010
O7A C25A 0.0010
C27A C26A 0.0010

####################################################################### 
# 
# 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_exp_694
_database_code_depnum_ccdc_archive 'CCDC 1894665'
loop_
_audit_author_name
_audit_author_address
'Zhongshu Li'
;Lehn Institute of Functional Materials, School of Chemistry, Sun Yat Sen University
China
;
_audit_update_record             
;
2022-05-18 deposited with the CCDC.	2022-06-06 downloaded from the CCDC.
;
_audit_creation_date             2022-05-09
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H7 O2 P'
_chemical_formula_sum            'C9 H7 O2 P'
_chemical_formula_weight         178.12
_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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   7.8469(2)
_cell_length_b                   7.1421(2)
_cell_length_c                   15.2070(4)
_cell_angle_alpha                90
_cell_angle_beta                 100.147(3)
_cell_angle_gamma                90
_cell_volume                     838.92(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2331
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.4190
_cell_measurement_theta_min      5.7190
_shelx_estimated_absorpt_T_max   0.843
_shelx_estimated_absorpt_T_min   0.804
_exptl_absorpt_coefficient_mu    2.528
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4068
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.752
_diffrn_reflns_theta_min         5.728
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -14.00  18.00   0.50    1.00    --    0.00 -57.00  60.00   64
  2  ω     27.00  88.00   0.50    1.00    --    0.00  19.00  30.00  122
  3  ω    -63.00 -11.00   0.50    1.00    --    0.00 -57.00-120.00  104
  4  ω    -18.00  16.00   0.50    1.00    --    0.00  19.00  30.00   68
  5  ω     75.00 112.00   0.50    5.00    --   95.20  77.00  90.00   74
  6  ω     55.00 113.00   0.50    5.00    --   95.20 -45.00 -30.00  116
  7  ω    157.00 184.00   0.50    5.00    --   95.20  30.00 150.00   54
  8  ω     49.00 114.00   0.50    5.00    --   95.20 -61.00 -30.00  130
  9  ω     10.00 111.00   0.50    5.00    --   95.20 -30.00-180.00  202
 10  ω      6.00  44.00   0.50    5.00    --   95.20 -61.00 -30.00   76
 11  ω     85.00 124.00   0.50    5.00    --   95.20  30.00 150.00   78
 12  ω    130.00 156.00   0.50    5.00    --   95.20  77.00  90.00   52
 13  ω     23.00  49.00   0.50    5.00    --   95.20 -45.00 -30.00   52
 14  ω     29.00 124.00   0.50    5.00    --   95.20 -77.00 150.00  190
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual offset/far'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0487025000
_diffrn_orient_matrix_UB_12      0.1529593000
_diffrn_orient_matrix_UB_13      0.0625329000
_diffrn_orient_matrix_UB_21      -0.1102852000
_diffrn_orient_matrix_UB_22      0.0987033000
_diffrn_orient_matrix_UB_23      -0.0805125000
_diffrn_orient_matrix_UB_31      -0.1589669000
_diffrn_orient_matrix_UB_32      -0.1157113000
_diffrn_orient_matrix_UB_33      0.0139047000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1499
_reflns_number_total             1639
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1639
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0588
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1134P)²+0.0827P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1568
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8), C6(H6), C7(H7)
1.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_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 0.24621(6) 0.51402(7) 0.27622(3) 0.0351(3) Uani 1 1 d . . . . .
O1 O 0.5580(2) 0.5314(2) 0.21648(10) 0.0432(4) Uani 1 1 d . . . . .
O2 O 0.13552(18) 0.7568(3) 0.39571(11) 0.0514(5) Uani 1 1 d . . . . .
C4 C 0.5603(2) 0.6321(3) 0.36720(11) 0.0289(4) Uani 1 1 d . . . . .
C3 C 0.4401(2) 0.6925(3) 0.41908(12) 0.0298(4) Uani 1 1 d . . . . .
C9 C 0.4955(2) 0.7694(3) 0.50336(11) 0.0330(5) Uani 1 1 d . . . . .
H9 H 0.416058 0.808481 0.538253 0.040 Uiso 1 1 calc R U . . .
C1 C 0.4795(2) 0.5604(3) 0.27782(12) 0.0324(4) Uani 1 1 d . . . . .
C8 C 0.6712(3) 0.7865(3) 0.53398(12) 0.0356(5) Uani 1 1 d . . . . .
H8 H 0.710167 0.837867 0.590105 0.043 Uiso 1 1 calc R U . . .
C6 C 0.7363(2) 0.6499(3) 0.39836(12) 0.0335(4) Uani 1 1 d . . . . .
H6 H 0.816379 0.610395 0.363874 0.040 Uiso 1 1 calc R U . . .
C2 C 0.2577(2) 0.6774(3) 0.37265(13) 0.0353(5) Uani 1 1 d . . . . .
C7 C 0.7907(3) 0.7280(3) 0.48228(13) 0.0367(5) Uani 1 1 d . . . . .
H7 H 0.908453 0.741317 0.504131 0.044 Uiso 1 1 calc R U . . .
C5 C 0.1371(3) 0.6528(4) 0.18154(15) 0.0477(6) Uani 1 1 d . . . . .
H5A H 0.204466 0.762527 0.175015 0.072 Uiso 1 1 calc R U . . .
H5B H 0.024675 0.689505 0.192009 0.072 Uiso 1 1 calc R U . . .
H5C H 0.124950 0.579227 0.127976 0.072 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 C1 1.856(2) . ?
P1 C2 1.864(2) . ?
P1 C5 1.832(2) . ?
O1 C1 1.222(2) . ?
O2 C2 1.217(2) . ?
C4 C3 1.400(2) . ?
C4 C1 1.486(2) . ?
C4 C6 1.385(3) . ?
C3 C9 1.392(2) . ?
C3 C2 1.484(3) . ?
C9 H9 0.9300 . ?
C9 C8 1.380(3) . ?
C8 H8 0.9300 . ?
C8 C7 1.390(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.389(3) . ?
C7 H7 0.9300 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 C2 88.12(8) . . ?
C5 P1 C1 103.72(10) . . ?
C5 P1 C2 103.33(10) . . ?
C3 C4 C1 113.59(16) . . ?
C6 C4 C3 120.63(16) . . ?
C6 C4 C1 125.71(16) . . ?
C4 C3 C2 113.50(16) . . ?
C9 C3 C4 120.53(16) . . ?
C9 C3 C2 125.84(16) . . ?
C3 C9 H9 120.8 . . ?
C8 C9 C3 118.49(16) . . ?
C8 C9 H9 120.8 . . ?
O1 C1 P1 126.01(15) . . ?
O1 C1 C4 124.41(17) . . ?
C4 C1 P1 109.55(12) . . ?
C9 C8 H8 119.5 . . ?
C9 C8 C7 121.07(17) . . ?
C7 C8 H8 119.5 . . ?
C4 C6 H6 120.7 . . ?
C4 C6 C7 118.51(17) . . ?
C7 C6 H6 120.7 . . ?
O2 C2 P1 125.94(16) . . ?
O2 C2 C3 124.86(19) . . ?
C3 C2 P1 109.18(13) . . ?
C8 C7 H7 119.6 . . ?
C6 C7 C8 120.77(18) . . ?
C6 C7 H7 119.6 . . ?
P1 C5 H5A 109.5 . . ?
P1 C5 H5B 109.5 . . ?
P1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 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
C4 C3 C9 C8 0.7(3) . . . . ?
C4 C3 C2 P1 18.1(2) . . . . ?
C4 C3 C2 O2 -163.3(2) . . . . ?
C4 C6 C7 C8 0.2(3) . . . . ?
C3 C4 C1 P1 -15.5(2) . . . . ?
C3 C4 C1 O1 166.7(2) . . . . ?
C3 C4 C6 C7 0.3(3) . . . . ?
C3 C9 C8 C7 -0.2(3) . . . . ?
C9 C3 C2 P1 -166.08(16) . . . . ?
C9 C3 C2 O2 12.5(3) . . . . ?
C9 C8 C7 C6 -0.3(3) . . . . ?
C1 P1 C2 O2 159.4(2) . . . . ?
C1 P1 C2 C3 -22.10(14) . . . . ?
C1 C4 C3 C9 -177.83(16) . . . . ?
C1 C4 C3 C2 -1.8(2) . . . . ?
C1 C4 C6 C7 176.99(18) . . . . ?
C6 C4 C3 C9 -0.8(3) . . . . ?
C6 C4 C3 C2 175.28(17) . . . . ?
C6 C4 C1 P1 167.63(16) . . . . ?
C6 C4 C1 O1 -10.2(3) . . . . ?
C2 P1 C1 O1 -161.0(2) . . . . ?
C2 P1 C1 C4 21.19(14) . . . . ?
C2 C3 C9 C8 -174.84(18) . . . . ?
C5 P1 C1 O1 -57.8(2) . . . . ?
C5 P1 C1 C4 124.46(15) . . . . ?
C5 P1 C2 O2 55.7(2) . . . . ?
C5 P1 C2 C3 -125.75(14) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.610
_oxdiff_exptl_absorpt_empirical_full_min 0.722
####################################################################### 
# 
# 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_exp_1006
_database_code_depnum_ccdc_archive 'CCDC 1894666'
loop_
_audit_author_name
_audit_author_address
'Zhongshu Li'
;Lehn Institute of Functional Materials, School of Chemistry, Sun Yat Sen University
China
;
_audit_update_record             
;
2022-05-18 deposited with the CCDC.	2022-06-06 downloaded from the CCDC.
;
_audit_creation_date             2022-05-09
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H42 B N2 O2 P'
_chemical_formula_sum            'C34 H42 B N2 O2 P'
_chemical_formula_weight         552.47
_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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 '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                   15.4261(2)
_cell_length_b                   12.4164(2)
_cell_length_c                   16.4259(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.0090(10)
_cell_angle_gamma                90
_cell_volume                     3128.87(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10049
_cell_measurement_temperature    150.10(10)
_cell_measurement_theta_max      74.2510
_cell_measurement_theta_min      3.5370
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.018
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18562
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.240
_diffrn_reflns_theta_min         4.473
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      150.10(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -68.00  28.00   1.00    1.50    --  -41.20  57.00-180.00   96
  2  ω     54.00  82.00   1.00    1.50    --   41.20 -99.00-180.00   28
  3  ω     38.00 136.00   1.00    4.00    --  107.98 -77.00 -60.00   98
  4  ω     96.00 121.00   1.00    4.00    --  107.98-125.00  30.00   25
  5  ω     38.00  78.00   1.00    4.00    --  107.98-125.00  30.00   40
  6  ω     34.00 109.00   1.00    4.00    --  107.98 -94.00 120.00   75
  7  ω     35.00 134.00   1.00    4.00    --  107.98 -30.00 -30.00   99
  8  ω    150.00 177.00   1.00    4.00    --  107.98  30.00 -30.00   27
  9  ω     84.00 124.00   1.00    4.00    --  107.98  30.00 -30.00   40
 10  ω     32.00 126.00   1.00    4.00    --  107.98 -30.00 150.00   94
 11  ω     82.00 171.00   1.00    4.00    --  107.98  45.00 150.00   89
 12  ω     34.00 134.00   1.00    4.00    --  107.98 -77.00 150.00  100
 13  ω   -107.00  -9.00   1.00    1.50    --  -41.20 -77.00  30.00   98
 14  ω   -110.00 -14.00   1.00    1.50    --  -41.20 -57.00 -90.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0671647000
_diffrn_orient_matrix_UB_12      0.0895962000
_diffrn_orient_matrix_UB_13      -0.0098894000
_diffrn_orient_matrix_UB_21      0.0223498000
_diffrn_orient_matrix_UB_22      0.0038353000
_diffrn_orient_matrix_UB_23      0.0936361000
_diffrn_orient_matrix_UB_31      0.0711134000
_diffrn_orient_matrix_UB_32      -0.0857346000
_diffrn_orient_matrix_UB_33      -0.0063754000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5735
_reflns_number_total             6283
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         6283
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0444
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0780P)²+0.7450P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1242
_refine_special_details          ?
_olex2_refinement_description    
;
1. Rigid bond restraints
 P1, C1
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
2.a Ternary CH refined with riding coordinates:
 C33(H33), C21(H21), C18(H18), C30(H30)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C9(H9A,H9B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C5(H5), C25(H25), C15(H15), C8(H8), C14(H14), C26(H26), C7(H7),
 C27(H27), C6(H6)
2.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C22(H22A,H22B,
 H22C), C32(H32A,H32B,H32C), C20(H20A,H20B,H20C), C31(H31A,H31B,H31C), C29(H29A,
 H29B,H29C)
;
_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 0.43204(2) 0.61540(3) 0.31661(2) 0.03171(12) Uani 1 1 d . U . . .
O1 O 0.27361(6) 0.67166(7) 0.36841(5) 0.0255(2) Uani 1 1 d . . . . .
O2 O 0.59501(6) 0.59441(9) 0.39976(7) 0.0391(2) Uani 1 1 d . . . . .
N2 N 0.14595(7) 0.72473(9) 0.27888(6) 0.0239(2) Uani 1 1 d . . . . .
N1 N 0.22317(7) 0.57964(9) 0.23217(6) 0.0244(2) Uani 1 1 d . . . . .
C4 C 0.39316(8) 0.66448(10) 0.46980(8) 0.0236(2) Uani 1 1 d . . . . .
C1 C 0.35889(8) 0.65096(10) 0.38336(8) 0.0235(2) Uani 1 1 d . U . . .
C11 C 0.12577(8) 0.82411(10) 0.31660(7) 0.0238(2) Uani 1 1 d . . . . .
C3 C 0.48273(8) 0.64376(10) 0.48323(8) 0.0256(3) Uani 1 1 d . . . . .
C12 C 0.05843(8) 0.82630(10) 0.36819(8) 0.0262(3) Uani 1 1 d . . . . .
C23 C 0.25921(8) 0.47290(10) 0.23679(8) 0.0250(3) Uani 1 1 d . . . . .
C24 C 0.23817(8) 0.40202(10) 0.29844(8) 0.0275(3) Uani 1 1 d . . . . .
C16 C 0.17102(8) 0.91813(11) 0.30020(8) 0.0277(3) Uani 1 1 d . . . . .
C10 C 0.10452(9) 0.70079(11) 0.19645(8) 0.0306(3) Uani 1 1 d . . . . .
H10A H 0.119594 0.755990 0.156785 0.037 Uiso 1 1 calc R U . . .
H10B H 0.040330 0.697439 0.195767 0.037 Uiso 1 1 calc R U . . .
C13 C 0.03871(9) 0.92381(12) 0.40380(9) 0.0316(3) Uani 1 1 d . . . . .
H13 H -0.005725 0.926308 0.439667 0.038 Uiso 1 1 calc R U . . .
C2 C 0.51924(8) 0.61498(10) 0.40560(9) 0.0284(3) Uani 1 1 d . . . . .
C5 C 0.34738(9) 0.69488(11) 0.53402(8) 0.0307(3) Uani 1 1 d . . . . .
H5 H 0.286669 0.709500 0.525323 0.037 Uiso 1 1 calc R U . . .
C28 C 0.31147(9) 0.43877(12) 0.17618(9) 0.0309(3) Uani 1 1 d . . . . .
C25 C 0.27359(9) 0.29822(11) 0.30004(10) 0.0348(3) Uani 1 1 d . . . . .
H25 H 0.261917 0.250027 0.342472 0.042 Uiso 1 1 calc R U . . .
C9 C 0.14170(9) 0.59109(12) 0.17660(9) 0.0338(3) Uani 1 1 d . . . . .
H9A H 0.100133 0.532914 0.186349 0.041 Uiso 1 1 calc R U . . .
H9B H 0.154042 0.588167 0.118696 0.041 Uiso 1 1 calc R U . . .
C15 C 0.14790(10) 1.01431(11) 0.33625(10) 0.0347(3) Uani 1 1 d . . . . .
H15 H 0.177472 1.078916 0.325102 0.042 Uiso 1 1 calc R U . . .
C33 C 0.17547(9) 0.43101(11) 0.36060(8) 0.0297(3) Uani 1 1 d . . . . .
H33 H 0.157672 0.507778 0.350971 0.036 Uiso 1 1 calc R U . . .
C21 C 0.01034(9) 0.72415(12) 0.38693(9) 0.0330(3) Uani 1 1 d . . . . .
H21 H 0.012054 0.674379 0.339258 0.040 Uiso 1 1 calc R U . . .
C18 C 0.24383(9) 0.91823(12) 0.24476(9) 0.0333(3) Uani 1 1 d . . . . .
H18 H 0.249858 0.843124 0.224109 0.040 Uiso 1 1 calc R U . . .
C8 C 0.52715(9) 0.65216(12) 0.56032(9) 0.0332(3) Uani 1 1 d . . . . .
H8 H 0.587894 0.637732 0.569015 0.040 Uiso 1 1 calc R U . . .
C14 C 0.08288(10) 1.01716(12) 0.38774(9) 0.0353(3) Uani 1 1 d . . . . .
H14 H 0.068399 1.083203 0.412197 0.042 Uiso 1 1 calc R U . . .
C26 C 0.32532(10) 0.26437(12) 0.24099(10) 0.0394(3) Uani 1 1 d . . . . .
H26 H 0.348614 0.193481 0.242951 0.047 Uiso 1 1 calc R U . . .
C7 C 0.48096(10) 0.68226(14) 0.62510(9) 0.0387(3) Uani 1 1 d . . . . .
H7 H 0.510369 0.688209 0.678695 0.046 Uiso 1 1 calc R U . . .
C27 C 0.34294(10) 0.33372(12) 0.17941(10) 0.0373(3) Uani 1 1 d . . . . .
H27 H 0.377266 0.309325 0.138318 0.045 Uiso 1 1 calc R U . . .
C6 C 0.39250(10) 0.70360(13) 0.61202(9) 0.0373(3) Uani 1 1 d . . . . .
H6 H 0.362003 0.724498 0.656815 0.045 Uiso 1 1 calc R U . . .
C34 C 0.21752(11) 0.42194(14) 0.44861(9) 0.0402(3) Uani 1 1 d . . . . .
H34A H 0.234210 0.346933 0.460344 0.060 Uiso 1 1 calc R U . . .
H34B H 0.175880 0.445285 0.486185 0.060 Uiso 1 1 calc R U . . .
H34C H 0.269469 0.467779 0.455857 0.060 Uiso 1 1 calc R U . . .
C30 C 0.33284(10) 0.51135(14) 0.10672(9) 0.0400(3) Uani 1 1 d . . . . .
H30 H 0.314556 0.586231 0.119448 0.048 Uiso 1 1 calc R U . . .
C17 C 0.33109(10) 0.95007(14) 0.29174(10) 0.0408(3) Uani 1 1 d . . . . .
H17A H 0.326030 1.021885 0.315541 0.061 Uiso 1 1 calc R U . . .
H17B H 0.376445 0.950915 0.254188 0.061 Uiso 1 1 calc R U . . .
H17C H 0.346623 0.897791 0.335540 0.061 Uiso 1 1 calc R U . . .
C19 C 0.22136(11) 0.99110(15) 0.17066(10) 0.0447(4) Uani 1 1 d . . . . .
H19A H 0.165723 0.968335 0.141453 0.067 Uiso 1 1 calc R U . . .
H19B H 0.267346 0.985968 0.133949 0.067 Uiso 1 1 calc R U . . .
H19C H 0.216588 1.065765 0.189012 0.067 Uiso 1 1 calc R U . . .
B1 B 0.21929(9) 0.65717(11) 0.29546(8) 0.0219(3) Uani 1 1 d . . . . .
C22 C -0.08578(10) 0.74420(15) 0.39877(12) 0.0487(4) Uani 1 1 d . . . . .
H22A H -0.089419 0.786126 0.448841 0.073 Uiso 1 1 calc R U . . .
H22B H -0.115510 0.675040 0.403297 0.073 Uiso 1 1 calc R U . . .
H22C H -0.113732 0.784218 0.351718 0.073 Uiso 1 1 calc R U . . .
C32 C 0.09294(10) 0.36165(15) 0.34735(11) 0.0447(4) Uani 1 1 d . . . . .
H32A H 0.066519 0.369790 0.290789 0.067 Uiso 1 1 calc R U . . .
H32B H 0.051372 0.384912 0.385014 0.067 Uiso 1 1 calc R U . . .
H32C H 0.108201 0.285924 0.357797 0.067 Uiso 1 1 calc R U . . .
C20 C 0.05745(12) 0.66870(14) 0.46201(11) 0.0476(4) Uani 1 1 d . . . . .
H20A H 0.118492 0.656326 0.453112 0.071 Uiso 1 1 calc R U . . .
H20B H 0.029246 0.599573 0.470870 0.071 Uiso 1 1 calc R U . . .
H20C H 0.054829 0.714639 0.510207 0.071 Uiso 1 1 calc R U . . .
C31 C 0.43054(12) 0.51375(17) 0.09629(12) 0.0519(4) Uani 1 1 d . . . . .
H31A H 0.463363 0.535957 0.147867 0.078 Uiso 1 1 calc R U . . .
H31B H 0.441115 0.565046 0.053068 0.078 Uiso 1 1 calc R U . . .
H31C H 0.449534 0.441782 0.081256 0.078 Uiso 1 1 calc R U . . .
C29 C 0.28117(15) 0.4770(2) 0.02597(11) 0.0633(6) Uani 1 1 d . . . . .
H29A H 0.300908 0.405691 0.010105 0.095 Uiso 1 1 calc R U . . .
H29B H 0.290674 0.529264 -0.016889 0.095 Uiso 1 1 calc R U . . .
H29C H 0.218940 0.473985 0.033132 0.095 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 C1 1.7116(13) . ?
P1 C2 1.8799(14) . ?
O1 C1 1.3377(15) . ?
O1 B1 1.4000(16) . ?
O2 C2 1.2100(17) . ?
N2 C11 1.4296(16) . ?
N2 C10 1.4659(16) . ?
N2 B1 1.4118(17) . ?
N1 C23 1.4360(16) . ?
N1 C9 1.4808(16) . ?
N1 B1 1.4228(17) . ?
C4 C1 1.4719(17) . ?
C4 C3 1.4000(17) . ?
C4 C5 1.3821(18) . ?
C11 C12 1.4080(18) . ?
C11 C16 1.4007(18) . ?
C3 C2 1.4905(18) . ?
C3 C8 1.3792(19) . ?
C12 C13 1.3920(19) . ?
C12 C21 1.5171(18) . ?
C23 C24 1.4051(19) . ?
C23 C28 1.4102(18) . ?
C24 C25 1.3991(19) . ?
C24 C33 1.5212(19) . ?
C16 C15 1.396(2) . ?
C16 C18 1.5182(18) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C9 1.5262(19) . ?
C13 H13 0.9500 . ?
C13 C14 1.384(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.397(2) . ?
C28 C27 1.391(2) . ?
C28 C30 1.517(2) . ?
C25 H25 0.9500 . ?
C25 C26 1.384(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C15 H15 0.9500 . ?
C15 C14 1.378(2) . ?
C33 H33 1.0000 . ?
C33 C34 1.525(2) . ?
C33 C32 1.5335(19) . ?
C21 H21 1.0000 . ?
C21 C22 1.536(2) . ?
C21 C20 1.528(2) . ?
C18 H18 1.0000 . ?
C18 C17 1.532(2) . ?
C18 C19 1.527(2) . ?
C8 H8 0.9500 . ?
C8 C7 1.392(2) . ?
C14 H14 0.9500 . ?
C26 H26 0.9500 . ?
C26 C27 1.377(2) . ?
C7 H7 0.9500 . ?
C7 C6 1.385(2) . ?
C27 H27 0.9500 . ?
C6 H6 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C30 H30 1.0000 . ?
C30 C31 1.535(2) . ?
C30 C29 1.535(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 C2 88.21(6) . . ?
C1 O1 B1 128.42(10) . . ?
C11 N2 C10 118.79(10) . . ?
B1 N2 C11 129.48(11) . . ?
B1 N2 C10 108.71(10) . . ?
C23 N1 C9 114.84(10) . . ?
B1 N1 C23 129.16(11) . . ?
B1 N1 C9 106.71(10) . . ?
C3 C4 C1 112.33(11) . . ?
C5 C4 C1 127.36(12) . . ?
C5 C4 C3 120.30(12) . . ?
O1 C1 P1 129.32(9) . . ?
O1 C1 C4 113.72(11) . . ?
C4 C1 P1 116.94(9) . . ?
C12 C11 N2 119.04(11) . . ?
C16 C11 N2 120.03(11) . . ?
C16 C11 C12 120.90(12) . . ?
C4 C3 C2 111.36(11) . . ?
C8 C3 C4 121.21(12) . . ?
C8 C3 C2 127.42(12) . . ?
C11 C12 C21 120.87(12) . . ?
C13 C12 C11 118.50(12) . . ?
C13 C12 C21 120.60(12) . . ?
C24 C23 N1 119.92(11) . . ?
C24 C23 C28 120.85(12) . . ?
C28 C23 N1 119.13(12) . . ?
C23 C24 C33 123.14(12) . . ?
C25 C24 C23 118.12(12) . . ?
C25 C24 C33 118.67(12) . . ?
C11 C16 C18 122.07(12) . . ?
C15 C16 C11 118.48(12) . . ?
C15 C16 C18 119.45(12) . . ?
N2 C10 H10A 111.0 . . ?
N2 C10 H10B 111.0 . . ?
N2 C10 C9 103.95(10) . . ?
H10A C10 H10B 109.0 . . ?
C9 C10 H10A 111.0 . . ?
C9 C10 H10B 111.0 . . ?
C12 C13 H13 119.5 . . ?
C14 C13 C12 120.98(13) . . ?
C14 C13 H13 119.5 . . ?
O2 C2 P1 123.88(11) . . ?
O2 C2 C3 124.96(13) . . ?
C3 C2 P1 111.15(9) . . ?
C4 C5 H5 120.8 . . ?
C4 C5 C6 118.42(12) . . ?
C6 C5 H5 120.8 . . ?
C23 C28 C30 122.52(13) . . ?
C27 C28 C23 118.55(13) . . ?
C27 C28 C30 118.91(13) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 C24 121.28(14) . . ?
C26 C25 H25 119.4 . . ?
N1 C9 C10 105.53(10) . . ?
N1 C9 H9A 110.6 . . ?
N1 C9 H9B 110.6 . . ?
C10 C9 H9A 110.6 . . ?
C10 C9 H9B 110.6 . . ?
H9A C9 H9B 108.8 . . ?
C16 C15 H15 119.4 . . ?
C14 C15 C16 121.12(13) . . ?
C14 C15 H15 119.4 . . ?
C24 C33 H33 107.6 . . ?
C24 C33 C34 112.43(12) . . ?
C24 C33 C32 110.40(12) . . ?
C34 C33 H33 107.6 . . ?
C34 C33 C32 110.93(12) . . ?
C32 C33 H33 107.6 . . ?
C12 C21 H21 107.7 . . ?
C12 C21 C22 112.90(13) . . ?
C12 C21 C20 109.82(12) . . ?
C22 C21 H21 107.7 . . ?
C20 C21 H21 107.7 . . ?
C20 C21 C22 110.77(13) . . ?
C16 C18 H18 107.7 . . ?
C16 C18 C17 111.37(12) . . ?
C16 C18 C19 110.99(12) . . ?
C17 C18 H18 107.7 . . ?
C19 C18 H18 107.7 . . ?
C19 C18 C17 111.27(12) . . ?
C3 C8 H8 120.7 . . ?
C3 C8 C7 118.50(12) . . ?
C7 C8 H8 120.7 . . ?
C13 C14 H14 120.0 . . ?
C15 C14 C13 119.99(13) . . ?
C15 C14 H14 120.0 . . ?
C25 C26 H26 120.1 . . ?
C27 C26 C25 119.84(13) . . ?
C27 C26 H26 120.1 . . ?
C8 C7 H7 119.7 . . ?
C6 C7 C8 120.51(13) . . ?
C6 C7 H7 119.7 . . ?
C28 C27 H27 119.4 . . ?
C26 C27 C28 121.30(14) . . ?
C26 C27 H27 119.4 . . ?
C5 C6 H6 119.5 . . ?
C7 C6 C5 121.06(13) . . ?
C7 C6 H6 119.5 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C28 C30 H30 107.9 . . ?
C28 C30 C31 112.88(14) . . ?
C28 C30 C29 110.53(15) . . ?
C31 C30 H30 107.9 . . ?
C29 C30 H30 107.9 . . ?
C29 C30 C31 109.63(14) . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O1 B1 N2 118.98(11) . . ?
O1 B1 N1 130.18(11) . . ?
N2 B1 N1 110.81(11) . . ?
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 . . ?
C33 C32 H32A 109.5 . . ?
C33 C32 H32B 109.5 . . ?
C33 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
C21 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 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
N2 C11 C12 C13 -179.27(11) . . . . ?
N2 C11 C12 C21 2.74(18) . . . . ?
N2 C11 C16 C15 178.19(12) . . . . ?
N2 C11 C16 C18 -1.78(19) . . . . ?
N2 C10 C9 N1 -20.79(14) . . . . ?
N1 C23 C24 C25 179.04(11) . . . . ?
N1 C23 C24 C33 2.12(18) . . . . ?
N1 C23 C28 C27 -177.33(12) . . . . ?
N1 C23 C28 C30 1.25(19) . . . . ?
C4 C3 C2 P1 -0.46(13) . . . . ?
C4 C3 C2 O2 179.19(13) . . . . ?
C4 C3 C8 C7 -0.2(2) . . . . ?
C4 C5 C6 C7 -0.1(2) . . . . ?
C1 P1 C2 O2 -179.65(13) . . . . ?
C1 P1 C2 C3 0.00(9) . . . . ?
C1 O1 B1 N2 -151.33(12) . . . . ?
C1 O1 B1 N1 31.1(2) . . . . ?
C1 C4 C3 C2 0.78(15) . . . . ?
C1 C4 C3 C8 179.94(12) . . . . ?
C1 C4 C5 C6 -179.68(13) . . . . ?
C11 N2 C10 C9 179.44(11) . . . . ?
C11 N2 B1 O1 15.16(19) . . . . ?
C11 N2 B1 N1 -166.83(11) . . . . ?
C11 C12 C13 C14 1.3(2) . . . . ?
C11 C12 C21 C22 -146.93(13) . . . . ?
C11 C12 C21 C20 88.91(15) . . . . ?
C11 C16 C15 C14 0.9(2) . . . . ?
C11 C16 C18 C17 -116.67(14) . . . . ?
C11 C16 C18 C19 118.77(14) . . . . ?
C3 C4 C1 P1 -0.84(14) . . . . ?
C3 C4 C1 O1 -179.14(10) . . . . ?
C3 C4 C5 C6 -0.4(2) . . . . ?
C3 C8 C7 C6 -0.2(2) . . . . ?
C12 C11 C16 C15 0.03(19) . . . . ?
C12 C11 C16 C18 -179.93(12) . . . . ?
C12 C13 C14 C15 -0.5(2) . . . . ?
C23 N1 C9 C10 166.96(11) . . . . ?
C23 N1 B1 O1 27.0(2) . . . . ?
C23 N1 B1 N2 -150.71(12) . . . . ?
C23 C24 C25 C26 -2.4(2) . . . . ?
C23 C24 C33 C34 -122.28(14) . . . . ?
C23 C24 C33 C32 113.26(15) . . . . ?
C23 C28 C27 C26 -1.2(2) . . . . ?
C23 C28 C30 C31 130.50(15) . . . . ?
C23 C28 C30 C29 -106.31(17) . . . . ?
C24 C23 C28 C27 -0.97(19) . . . . ?
C24 C23 C28 C30 177.60(13) . . . . ?
C24 C25 C26 C27 0.3(2) . . . . ?
C16 C11 C12 C13 -1.09(18) . . . . ?
C16 C11 C12 C21 -179.09(12) . . . . ?
C16 C15 C14 C13 -0.7(2) . . . . ?
C10 N2 C11 C12 93.62(14) . . . . ?
C10 N2 C11 C16 -84.57(15) . . . . ?
C10 N2 B1 O1 174.81(11) . . . . ?
C10 N2 B1 N1 -7.18(14) . . . . ?
C13 C12 C21 C22 35.12(18) . . . . ?
C13 C12 C21 C20 -89.04(16) . . . . ?
C2 P1 C1 O1 178.44(12) . . . . ?
C2 P1 C1 C4 0.46(10) . . . . ?
C2 C3 C8 C7 178.79(14) . . . . ?
C5 C4 C1 P1 178.50(11) . . . . ?
C5 C4 C1 O1 0.20(18) . . . . ?
C5 C4 C3 C2 -178.61(12) . . . . ?
C5 C4 C3 C8 0.6(2) . . . . ?
C28 C23 C24 C25 2.71(18) . . . . ?
C28 C23 C24 C33 -174.20(12) . . . . ?
C25 C24 C33 C34 60.83(16) . . . . ?
C25 C24 C33 C32 -63.64(17) . . . . ?
C25 C26 C27 C28 1.6(2) . . . . ?
C9 N1 C23 C24 -93.62(14) . . . . ?
C9 N1 C23 C28 82.77(15) . . . . ?
C9 N1 B1 O1 171.14(13) . . . . ?
C9 N1 B1 N2 -6.59(14) . . . . ?
C15 C16 C18 C17 63.36(17) . . . . ?
C15 C16 C18 C19 -61.20(17) . . . . ?
C33 C24 C25 C26 174.69(13) . . . . ?
C21 C12 C13 C14 179.31(13) . . . . ?
C18 C16 C15 C14 -179.18(13) . . . . ?
C8 C3 C2 P1 -179.56(12) . . . . ?
C8 C3 C2 O2 0.1(2) . . . . ?
C8 C7 C6 C5 0.4(3) . . . . ?
C27 C28 C30 C31 -50.93(19) . . . . ?
C27 C28 C30 C29 72.26(18) . . . . ?
C30 C28 C27 C26 -179.85(14) . . . . ?
B1 O1 C1 P1 8.47(19) . . . . ?
B1 O1 C1 C4 -173.49(11) . . . . ?
B1 N2 C11 C12 -108.45(15) . . . . ?
B1 N2 C11 C16 73.35(17) . . . . ?
B1 N2 C10 C9 17.28(14) . . . . ?
B1 N1 C23 C24 48.16(18) . . . . ?
B1 N1 C23 C28 -135.46(13) . . . . ?
B1 N1 C9 C10 17.02(14) . . . . ?

_olex2_date_sample_data_collection 2017-03-02
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.060
_oxdiff_exptl_absorpt_empirical_full_min 0.594
####################################################################### 
# 
# 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_exp_1912
_database_code_depnum_ccdc_archive 'CCDC 1894672'
loop_
_audit_author_name
_audit_author_address
'Zhongshu Li'
;Lehn Institute of Functional Materials, School of Chemistry, Sun Yat Sen University
China
;
_audit_update_record             
;
2022-05-18 deposited with the CCDC.	2022-06-06 downloaded from the CCDC.
;
_audit_creation_date             2022-05-07
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C6 H4 N0.5 O2 P0.5), C7 H8'
_chemical_formula_sum            'C19 H16 N O4 P'
_chemical_formula_weight         353.30
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O P Br'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   10.3706(2)
_cell_length_b                   14.3699(3)
_cell_length_c                   11.4240(3)
_cell_angle_alpha                90
_cell_angle_beta                 95.344(2)
_cell_angle_gamma                90
_cell_volume                     1695.06(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4655
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      65.0080
_cell_measurement_theta_min      3.8780
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.649
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0130
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7327
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        65.033
_diffrn_reflns_theta_max         65.033
_diffrn_reflns_theta_min         3.886
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.6525
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -41.00   30.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.7038   38.0000 -150.0000 71

#__ type_ start__ end____ width___ exp.time_
  2 omega  -43.00   28.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.7038   38.0000   90.0000 71

#__ type_ start__ end____ width___ exp.time_
  3 omega  -44.00   34.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.7038   38.0000  -30.0000 78

#__ type_ start__ end____ width___ exp.time_
  4 omega   15.00  121.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7118  -77.0000  -30.0000 106

#__ type_ start__ end____ width___ exp.time_
  5 omega   60.00  142.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7118   61.0000  120.0000 82

#__ type_ start__ end____ width___ exp.time_
  6 omega   97.00  161.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7118  125.0000    0.0000 64

#__ type_ start__ end____ width___ exp.time_
  7 omega   32.00  108.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7118 -125.0000  -30.0000 76

#__ type_ start__ end____ width___ exp.time_
  8 omega   49.00  117.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7118 -125.0000 -180.0000 68

#__ type_ start__ end____ width___ exp.time_
  9 omega   19.00   82.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7118  -30.0000  120.0000 63
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0090595000
_diffrn_orient_matrix_UB_12      0.0220174000
_diffrn_orient_matrix_UB_13      -0.1309388000
_diffrn_orient_matrix_UB_21      0.0700099000
_diffrn_orient_matrix_UB_22      0.0920200000
_diffrn_orient_matrix_UB_23      0.0340931000
_diffrn_orient_matrix_UB_31      0.1314345000
_diffrn_orient_matrix_UB_32      -0.0504860000
_diffrn_orient_matrix_UB_33      0.0052320000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2733
_reflns_number_total             2907
_reflns_odcompleteness_completeness 98.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         2907
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0290
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0390P)²+0.8166P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0781
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Sof: H16A(0.5) H16B(0.5) H15A(0.5) H15B(0.5) H7A(0.5) H7B(0.5) H8A(0.5)
 H8B(0.5)
2.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C15(H15A,H15B), C7(H7A,H7B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C11(H11), C12(H12), C23(H23), C22(H22), C19(H19), C4(H4), C21(H21),
 C20(H20)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
;
_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 0.12682(5) 0.750000 0.43792(4) 0.01826(13) Uani 1 2 d S T P . .
P2 P 0.86980(5) 0.750000 0.99286(4) 0.02050(14) Uani 1 2 d S T P . .
O3 O 0.13733(13) 0.750000 0.70636(12) 0.0271(3) Uani 1 2 d S T P . .
O1 O 0.20567(10) 0.57921(7) 0.36167(8) 0.0270(2) Uani 1 1 d . . . . .
O2 O 0.42241(14) 0.750000 0.42504(12) 0.0291(3) Uani 1 2 d S T P . .
O5 O 0.87708(14) 0.750000 1.26025(12) 0.0306(4) Uani 1 2 d S T P . .
O6 O 0.57288(14) 0.750000 0.94516(13) 0.0326(4) Uani 1 2 d S T P . .
O4 O 0.78518(11) 0.58002(7) 0.90238(9) 0.0304(3) Uani 1 1 d . . . . .
N009 N 0.74688(15) 0.750000 1.08492(14) 0.0192(3) Uani 1 2 d S T P . .
N00A N 0.25653(15) 0.750000 0.54504(14) 0.0178(3) Uani 1 2 d S T P . .
C2 C 0.19006(12) 0.70136(9) 0.21720(11) 0.0172(3) Uani 1 1 d . . . . .
C3 C 0.20084(12) 0.65185(10) 0.11394(12) 0.0198(3) Uani 1 1 d . . . . .
H3 H 0.200681 0.587132 0.113788 0.024 Uiso 1 1 calc R U . . .
C10 C 0.81382(12) 0.70137(9) 0.76272(12) 0.0185(3) Uani 1 1 d . . . . .
C11 C 0.81333(13) 0.65183(10) 0.65788(12) 0.0206(3) Uani 1 1 d . . . . .
H11 H 0.812455 0.587119 0.657565 0.025 Uiso 1 1 calc R U . . .
C5 C 0.38774(18) 0.750000 0.52276(17) 0.0204(4) Uani 1 2 d S T P . .
C6 C 0.24100(19) 0.750000 0.66644(17) 0.0201(4) Uani 1 2 d S T P . .
C1 C 0.18296(12) 0.65948(9) 0.33528(11) 0.0188(3) Uani 1 1 d . . . . .
C16 C 0.64153(19) 0.750000 1.25898(17) 0.0233(4) Uani 1 2 d S T P . .
H16A H 0.632914 0.804847 1.307128 0.028 Uiso 0.5 1 calc R U P . .
H16B H 0.632914 0.695153 1.307128 0.028 Uiso 0.5 1 calc R U P . .
C15 C 0.53902(19) 0.750000 1.15435(17) 0.0233(4) Uani 1 2 d S T P . .
H15A H 0.484697 0.695121 1.155508 0.028 Uiso 0.5 1 calc R U P . .
H15B H 0.484697 0.804879 1.155508 0.028 Uiso 0.5 1 calc R U P . .
C9 C 0.81256(13) 0.65958(9) 0.88115(12) 0.0205(3) Uani 1 1 d . . . . .
C18 C 0.77031(14) 0.49937(9) 1.23139(13) 0.0244(3) Uani 1 1 d . . . . .
C14 C 0.61333(18) 0.750000 1.04719(17) 0.0216(4) Uani 1 2 d S T P . .
C7 C 0.37365(19) 0.750000 0.73229(17) 0.0230(4) Uani 1 2 d S T P . .
H7A H 0.385519 0.695147 0.781607 0.028 Uiso 0.5 1 calc R U P . .
H7B H 0.385519 0.804853 0.781607 0.028 Uiso 0.5 1 calc R U P . .
C12 C 0.81419(13) 0.70143(10) 0.55439(12) 0.0222(3) Uani 1 1 d . . . . .
H12 H 0.814772 0.669591 0.483566 0.027 Uiso 1 1 calc R U . . .
C23 C 0.66352(15) 0.50636(10) 1.14861(13) 0.0250(3) Uani 1 1 d . . . . .
H23 H 0.676289 0.512302 1.069454 0.030 Uiso 1 1 calc R U . . .
C22 C 0.53807(15) 0.50463(10) 1.18214(14) 0.0282(3) Uani 1 1 d . . . . .
H22 H 0.467833 0.508118 1.125427 0.034 Uiso 1 1 calc R U . . .
C13 C 0.77022(19) 0.750000 1.20826(17) 0.0214(4) Uani 1 2 d S T P . .
C8 C 0.46927(19) 0.750000 0.63904(17) 0.0236(4) Uani 1 2 d S T P . .
H8A H 0.523899 0.804870 0.646464 0.028 Uiso 0.5 1 calc R U P . .
H8B H 0.523899 0.695130 0.646464 0.028 Uiso 0.5 1 calc R U P . .
C19 C 0.74807(15) 0.49048(10) 1.34931(13) 0.0280(3) Uani 1 1 d . . . . .
H19 H 0.817961 0.484590 1.406035 0.034 Uiso 1 1 calc R U . . .
C4 C 0.21185(13) 0.70146(10) 0.01122(12) 0.0222(3) Uani 1 1 d . . . . .
H4 H 0.219328 0.669559 -0.058656 0.027 Uiso 1 1 calc R U . . .
C21 C 0.51763(15) 0.49774(11) 1.29967(14) 0.0314(4) Uani 1 1 d . . . . .
H21 H 0.433917 0.498078 1.322619 0.038 Uiso 1 1 calc R U . . .
C20 C 0.62334(16) 0.49030(11) 1.38311(14) 0.0320(4) Uani 1 1 d . . . . .
H20 H 0.610241 0.485170 1.462285 0.038 Uiso 1 1 calc R U . . .
C17 C 0.90603(16) 0.49993(12) 1.19534(15) 0.0362(4) Uani 1 1 d . . . . .
H17A H 0.945116 0.440137 1.211188 0.054 Uiso 1 1 calc R U . . .
H17B H 0.955796 0.546838 1.238993 0.054 Uiso 1 1 calc R U . . .
H17C H 0.903861 0.513159 1.112812 0.054 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 N00A 1.7321(16) . ?
P1 C1 1.8796(14) . ?
P1 C1 1.8797(14) 4_575 ?
P2 N009 1.7264(16) . ?
P2 C9 1.8784(14) 4_575 ?
P2 C9 1.8783(14) . ?
O3 C6 1.206(2) . ?
O1 C1 1.2098(16) . ?
O2 C5 1.204(2) . ?
O5 C13 1.208(2) . ?
O6 C14 1.202(2) . ?
O4 C9 1.2080(17) . ?
N009 C14 1.412(2) . ?
N009 C13 1.407(2) . ?
N00A C5 1.407(2) . ?
N00A C6 1.411(2) . ?
C2 C2 1.398(3) 4_575 ?
C2 C3 1.3911(18) . ?
C2 C1 1.4851(18) . ?
C3 H3 0.9300 . ?
C3 C4 1.387(2) . ?
C10 C10 1.397(3) 4_575 ?
C10 C11 1.3930(19) . ?
C10 C9 1.4814(19) . ?
C11 H11 0.9300 . ?
C11 C12 1.381(2) . ?
C5 C8 1.507(3) . ?
C6 C7 1.505(3) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C15 1.524(3) . ?
C16 C13 1.504(3) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C14 1.506(3) . ?
C18 C23 1.391(2) . ?
C18 C19 1.394(2) . ?
C18 C17 1.503(2) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.522(3) . ?
C12 C12 1.396(3) 4_575 ?
C12 H12 0.9300 . ?
C23 H23 0.9300 . ?
C23 C22 1.390(2) . ?
C22 H22 0.9300 . ?
C22 C21 1.382(2) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C19 H19 0.9300 . ?
C19 C20 1.384(2) . ?
C4 C4 1.395(3) 4_575 ?
C4 H4 0.9300 . ?
C21 H21 0.9300 . ?
C21 C20 1.388(2) . ?
C20 H20 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N00A P1 C1 100.11(6) . . ?
N00A P1 C1 100.10(6) . 4_575 ?
C1 P1 C1 87.58(8) . 4_575 ?
N009 P2 C9 102.09(6) . . ?
N009 P2 C9 102.09(6) . 4_575 ?
C9 P2 C9 87.54(8) . 4_575 ?
C14 N009 P2 124.96(13) . . ?
C13 N009 P2 122.82(13) . . ?
C13 N009 C14 112.21(16) . . ?
C5 N00A P1 124.93(13) . . ?
C5 N00A C6 112.24(15) . . ?
C6 N00A P1 122.84(13) . . ?
C2 C2 C1 113.91(7) 4_575 . ?
C3 C2 C2 120.76(8) . 4_575 ?
C3 C2 C1 125.29(12) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 C2 118.30(13) . . ?
C4 C3 H3 120.8 . . ?
C10 C10 C9 113.92(7) 4_575 . ?
C11 C10 C10 120.73(8) . 4_575 ?
C11 C10 C9 125.34(12) . . ?
C10 C11 H11 120.9 . . ?
C12 C11 C10 118.20(13) . . ?
C12 C11 H11 120.9 . . ?
O2 C5 N00A 123.01(18) . . ?
O2 C5 C8 128.74(18) . . ?
N00A C5 C8 108.25(16) . . ?
O3 C6 N00A 123.97(17) . . ?
O3 C6 C7 128.05(18) . . ?
N00A C6 C7 107.98(16) . . ?
O1 C1 P1 124.67(10) . . ?
O1 C1 C2 126.00(12) . . ?
C2 C1 P1 109.30(9) . . ?
H16A C16 H16B 108.7 . . ?
C15 C16 H16A 110.5 . . ?
C15 C16 H16B 110.5 . . ?
C13 C16 H16A 110.5 . . ?
C13 C16 H16B 110.5 . . ?
C13 C16 C15 106.09(15) . . ?
C16 C15 H15A 110.7 . . ?
C16 C15 H15B 110.7 . . ?
H15A C15 H15B 108.8 . . ?
C14 C15 C16 105.38(16) . . ?
C14 C15 H15A 110.7 . . ?
C14 C15 H15B 110.7 . . ?
O4 C9 P2 125.70(11) . . ?
O4 C9 C10 126.10(13) . . ?
C10 C9 P2 108.12(9) . . ?
C23 C18 C19 118.08(14) . . ?
C23 C18 C17 121.32(14) . . ?
C19 C18 C17 120.59(14) . . ?
O6 C14 N009 122.70(18) . . ?
O6 C14 C15 129.03(18) . . ?
N009 C14 C15 108.27(16) . . ?
C6 C7 H7A 110.5 . . ?
C6 C7 H7B 110.5 . . ?
C6 C7 C8 105.96(16) . . ?
H7A C7 H7B 108.7 . . ?
C8 C7 H7A 110.5 . . ?
C8 C7 H7B 110.5 . . ?
C11 C12 C12 121.06(8) . 4_575 ?
C11 C12 H12 119.5 . . ?
C12 C12 H12 119.5 4_575 . ?
C18 C23 H23 119.4 . . ?
C22 C23 C18 121.17(14) . . ?
C22 C23 H23 119.4 . . ?
C23 C22 H22 120.0 . . ?
C21 C22 C23 120.06(14) . . ?
C21 C22 H22 120.0 . . ?
O5 C13 N009 123.83(18) . . ?
O5 C13 C16 128.12(18) . . ?
N009 C13 C16 108.04(16) . . ?
C5 C8 C7 105.57(16) . . ?
C5 C8 H8A 110.6 . . ?
C5 C8 H8B 110.6 . . ?
C7 C8 H8A 110.6 . . ?
C7 C8 H8B 110.6 . . ?
H8A C8 H8B 108.8 . . ?
C18 C19 H19 119.6 . . ?
C20 C19 C18 120.86(14) . . ?
C20 C19 H19 119.6 . . ?
C3 C4 C4 120.93(8) . 4_575 ?
C3 C4 H4 119.5 . . ?
C4 C4 H4 119.5 4_575 . ?
C22 C21 H21 120.3 . . ?
C22 C21 C20 119.33(14) . . ?
C20 C21 H21 120.3 . . ?
C19 C20 C21 120.47(14) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 H20 119.8 . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 N00A C5 O2 0.000(0) . . . . ?
P1 N00A C5 C8 180.000(0) . . . . ?
P1 N00A C6 O3 0.000(1) . . . . ?
P1 N00A C6 C7 180.000(0) . . . . ?
P2 N009 C14 O6 0.000(1) . . . . ?
P2 N009 C14 C15 180.000(1) . . . . ?
P2 N009 C13 O5 0.000(1) . . . . ?
P2 N009 C13 C16 180.000(1) . . . . ?
O3 C6 C7 C8 180.000(1) . . . . ?
O2 C5 C8 C7 180.000(0) . . . . ?
N009 P2 C9 O4 -55.90(14) . . . . ?
N009 P2 C9 C10 127.13(9) . . . . ?
N00A P1 C1 O1 60.71(13) . . . . ?
N00A P1 C1 C2 -121.30(9) . . . . ?
N00A C5 C8 C7 0.000(0) . . . . ?
N00A C6 C7 C8 0.000(0) . . . . ?
C2 C2 C3 C4 0.13(15) 4_575 . . . ?
C2 C2 C1 P1 16.80(9) 4_575 . . . ?
C2 C2 C1 O1 -165.25(11) 4_575 . . . ?
C2 C3 C4 C4 -0.13(15) . . . 4_575 ?
C3 C2 C1 P1 -165.57(11) . . . . ?
C3 C2 C1 O1 12.4(2) . . . . ?
C10 C10 C11 C12 0.65(15) 4_575 . . . ?
C10 C10 C9 P2 -19.73(9) 4_575 . . . ?
C10 C10 C9 O4 163.32(12) 4_575 . . . ?
C10 C11 C12 C12 -0.65(15) . . . 4_575 ?
C11 C10 C9 P2 161.10(11) . . . . ?
C11 C10 C9 O4 -15.9(2) . . . . ?
C5 N00A C6 O3 180.000(0) . . . . ?
C5 N00A C6 C7 0.000(0) . . . . ?
C6 N00A C5 O2 180.000(0) . . . . ?
C6 N00A C5 C8 0.000(0) . . . . ?
C6 C7 C8 C5 0.000(0) . . . . ?
C1 P1 N00A C5 44.66(4) . . . . ?
C1 P1 N00A C5 -44.66(4) 4_575 . . . ?
C1 P1 N00A C6 135.34(4) 4_575 . . . ?
C1 P1 N00A C6 -135.34(4) . . . . ?
C1 P1 C1 O1 160.54(9) 4_575 . . . ?
C1 P1 C1 C2 -21.47(11) 4_575 . . . ?
C1 C2 C3 C4 -177.35(12) . . . . ?
C16 C15 C14 O6 180.000(1) . . . . ?
C16 C15 C14 N009 0.000(1) . . . . ?
C15 C16 C13 O5 180.000(1) . . . . ?
C15 C16 C13 N009 0.000(1) . . . . ?
C9 P2 N009 C14 -45.03(4) . . . . ?
C9 P2 N009 C14 45.03(4) 4_575 . . . ?
C9 P2 N009 C13 -134.97(4) 4_575 . . . ?
C9 P2 N009 C13 134.97(4) . . . . ?
C9 P2 C9 O4 -157.74(10) 4_575 . . . ?
C9 P2 C9 C10 25.30(12) 4_575 . . . ?
C9 C10 C11 C12 179.77(12) . . . . ?
C18 C23 C22 C21 1.3(2) . . . . ?
C18 C19 C20 C21 0.9(2) . . . . ?
C14 N009 C13 O5 180.000(1) . . . . ?
C14 N009 C13 C16 0.000(1) . . . . ?
C23 C18 C19 C20 -1.1(2) . . . . ?
C23 C22 C21 C20 -1.6(2) . . . . ?
C22 C21 C20 C19 0.5(2) . . . . ?
C13 N009 C14 O6 180.000(1) . . . . ?
C13 N009 C14 C15 0.000(1) . . . . ?
C13 C16 C15 C14 0.000(1) . . . . ?
C19 C18 C23 C22 0.0(2) . . . . ?
C17 C18 C23 C22 179.17(14) . . . . ?
C17 C18 C19 C20 179.73(14) . . . . ?

_olex2_date_sample_data_collection 2015-05-09
_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_exp_1049
_database_code_depnum_ccdc_archive 'CCDC 1894670'
loop_
_audit_author_name
_audit_author_address
'Zhongshu Li'
;Lehn Institute of Functional Materials, School of Chemistry, Sun Yat Sen University
China
;
_audit_update_record             
;
2022-05-18 deposited with the CCDC.	2022-06-06 downloaded from the CCDC.
;
_audit_creation_date             2022-05-07
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C20 H14 O2 P2'
_chemical_formula_sum            'C20 H14 O2 P2'
_chemical_formula_weight         348.25
_chemical_absolute_configuration ?
_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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
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'

_cell_length_a                   12.7782(2)
_cell_length_b                   10.31430(10)
_cell_length_c                   13.0467(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1719.53(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6842
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      74.1550
_cell_measurement_theta_min      4.2420
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.367
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81004
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9100
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.311
_diffrn_reflns_theta_min         5.467
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -63.00  33.00   1.00    2.00    --  -41.08  38.00-120.00   96
  2  ω    100.00 130.00   1.00    2.00    --   41.08 178.00-150.00   30
  3  ω     83.00 178.00   1.00    5.00    --  107.98  45.00  90.00   95
  4  ω     50.00 121.00   1.00    5.00    --  107.98-125.00   0.00   71
  5  ω     46.00 135.00   1.00    5.00    --  107.98 -30.00  60.00   89
  6  ω     51.00 131.00   1.00    5.00    --  107.98 -45.00 150.00   80
  7  ω     32.00 137.00   1.00    5.00    --  107.98 -77.00   0.00  105
  8  ω     40.00 109.00   1.00    5.00    --  107.98 -94.00-180.00   69
  9  ω     36.00 150.00   1.00    5.00    --  107.98 -15.00 -90.00  114
 10  ω    -74.00  27.00   1.00    2.00    --  -41.08  77.00 -30.00  101
 11  ω   -114.00 -20.00   1.00    2.00    --  -41.08 -38.00  60.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0957181000
_diffrn_orient_matrix_UB_12      0.0896079000
_diffrn_orient_matrix_UB_13      -0.0100195000
_diffrn_orient_matrix_UB_21      -0.0340362000
_diffrn_orient_matrix_UB_22      0.0735961000
_diffrn_orient_matrix_UB_23      0.0973866000
_diffrn_orient_matrix_UB_31      0.0645350000
_diffrn_orient_matrix_UB_32      -0.0942649000
_diffrn_orient_matrix_UB_33      0.0662745000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.847
_reflns_Friedel_fraction_full    0.963
_reflns_Friedel_fraction_max     0.916
_reflns_number_gt                3314
_reflns_number_total             3350
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 
;
 Flack x determined using 1491 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.009(12)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3350
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0356
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0682P)²+0.2805P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0919
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C19(H19), C18(H18), C16(H16), C17(H17), C10(H10), C5(H5), C6(H6),
 C8(H8), C12(H12), C7(H7), C11(H11), C13(H13), C14(H14)
;
_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
P2 P 0.33339(4) 0.48162(6) 0.51350(6) 0.02040(18) Uani 1 1 d . . . . .
P1 P 0.40119(5) 0.56516(6) 0.65517(6) 0.02283(18) Uani 1 1 d . . . . .
O1 O 0.20434(18) 0.6440(2) 0.71247(19) 0.0353(5) Uani 1 1 d . . . . .
O2 O 0.56175(17) 0.6958(2) 0.5599(2) 0.0383(6) Uani 1 1 d . . . . .
C20 C 0.4101(2) 0.2724(3) 0.4074(2) 0.0236(6) Uani 1 1 d . . . . .
H20 H 0.341649 0.268727 0.383236 0.028 Uiso 1 1 calc R U . . .
C15 C 0.4392(2) 0.3716(3) 0.4743(2) 0.0207(5) Uani 1 1 d . . . . .
C2 C 0.4784(2) 0.7053(3) 0.6031(2) 0.0255(6) Uani 1 1 d . . . . .
C1 C 0.2895(2) 0.6779(3) 0.6826(2) 0.0238(5) Uani 1 1 d . . . . .
C3 C 0.4218(2) 0.8284(3) 0.6224(2) 0.0250(6) Uani 1 1 d . . . . .
C4 C 0.3224(2) 0.8143(3) 0.6646(2) 0.0245(6) Uani 1 1 d . . . . .
C19 C 0.4812(3) 0.1798(3) 0.3766(2) 0.0284(6) Uani 1 1 d . . . . .
H19 H 0.461149 0.115113 0.331021 0.034 Uiso 1 1 calc R U . . .
C18 C 0.5827(2) 0.1834(3) 0.4138(2) 0.0301(6) Uani 1 1 d . . . . .
H18 H 0.630577 0.120006 0.394470 0.036 Uiso 1 1 calc R U . . .
C16 C 0.5420(2) 0.3761(3) 0.5094(3) 0.0315(6) Uani 1 1 d . . . . .
H16 H 0.563284 0.442652 0.552640 0.038 Uiso 1 1 calc R U . . .
C9 C 0.3427(2) 0.6157(3) 0.4210(2) 0.0224(5) Uani 1 1 d . . . . .
C17 C 0.6125(2) 0.2812(4) 0.4797(3) 0.0370(8) Uani 1 1 d . . . . .
H17 H 0.680735 0.283540 0.504500 0.044 Uiso 1 1 calc R U . . .
C10 C 0.2607(3) 0.7045(3) 0.4205(3) 0.0331(7) Uani 1 1 d . . . . .
H10 H 0.203408 0.692555 0.463453 0.040 Uiso 1 1 calc R U . . .
C5 C 0.2608(3) 0.9216(3) 0.6860(2) 0.0314(7) Uani 1 1 d . . . . .
H5 H 0.194344 0.912045 0.713942 0.038 Uiso 1 1 calc R U . . .
C6 C 0.3011(3) 1.0436(3) 0.6646(3) 0.0387(7) Uani 1 1 d . . . . .
H6 H 0.261449 1.116973 0.679193 0.046 Uiso 1 1 calc R U . . .
C8 C 0.4617(3) 0.9499(3) 0.5999(3) 0.0338(7) Uani 1 1 d . . . . .
H8 H 0.527777 0.959258 0.571091 0.041 Uiso 1 1 calc R U . . .
C12 C 0.3478(4) 0.8284(3) 0.2898(3) 0.0483(9) Uani 1 1 d . . . . .
H12 H 0.349976 0.899844 0.246347 0.058 Uiso 1 1 calc R U . . .
C7 C 0.4001(3) 1.0572(3) 0.6217(3) 0.0395(9) Uani 1 1 d . . . . .
H7 H 0.425540 1.139755 0.607268 0.047 Uiso 1 1 calc R U . . .
C11 C 0.2647(3) 0.8112(3) 0.3556(3) 0.0432(9) Uani 1 1 d . . . . .
H11 H 0.210645 0.871549 0.356598 0.052 Uiso 1 1 calc R U . . .
C13 C 0.4281(3) 0.7382(4) 0.2892(3) 0.0438(8) Uani 1 1 d . . . . .
H13 H 0.483774 0.748433 0.244006 0.053 Uiso 1 1 calc R U . . .
C14 C 0.4265(3) 0.6334(3) 0.3548(2) 0.0310(6) Uani 1 1 d . . . . .
H14 H 0.481615 0.574463 0.354616 0.037 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
P2 P1 2.2157(10) . ?
P2 C15 1.838(3) . ?
P2 C9 1.839(3) . ?
P1 C2 1.877(3) . ?
P1 C1 1.876(3) . ?
O1 C1 1.207(4) . ?
O2 C2 1.209(4) . ?
C20 H20 0.9300 . ?
C20 C15 1.395(4) . ?
C20 C19 1.379(4) . ?
C15 C16 1.391(4) . ?
C2 C3 1.482(4) . ?
C1 C4 1.488(4) . ?
C3 C4 1.391(4) . ?
C3 C8 1.384(4) . ?
C4 C5 1.386(4) . ?
C19 H19 0.9300 . ?
C19 C18 1.385(4) . ?
C18 H18 0.9300 . ?
C18 C17 1.379(5) . ?
C16 H16 0.9300 . ?
C16 C17 1.385(4) . ?
C9 C10 1.392(4) . ?
C9 C14 1.388(4) . ?
C17 H17 0.9300 . ?
C10 H10 0.9300 . ?
C10 C11 1.389(5) . ?
C5 H5 0.9300 . ?
C5 C6 1.388(5) . ?
C6 H6 0.9300 . ?
C6 C7 1.392(6) . ?
C8 H8 0.9300 . ?
C8 C7 1.387(5) . ?
C12 H12 0.9300 . ?
C12 C11 1.377(6) . ?
C12 C13 1.386(6) . ?
C7 H7 0.9300 . ?
C11 H11 0.9300 . ?
C13 H13 0.9300 . ?
C13 C14 1.379(5) . ?
C14 H14 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C15 P2 P1 100.63(9) . . ?
C15 P2 C9 103.54(12) . . ?
C9 P2 P1 103.28(9) . . ?
C2 P1 P2 101.72(9) . . ?
C1 P1 P2 95.88(9) . . ?
C1 P1 C2 89.50(13) . . ?
C15 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
C19 C20 C15 120.9(3) . . ?
C20 C15 P2 115.5(2) . . ?
C16 C15 P2 125.6(2) . . ?
C16 C15 C20 118.8(2) . . ?
O2 C2 P1 124.7(2) . . ?
O2 C2 C3 125.3(3) . . ?
C3 C2 P1 110.0(2) . . ?
O1 C1 P1 124.6(2) . . ?
O1 C1 C4 125.4(3) . . ?
C4 C1 P1 109.9(2) . . ?
C4 C3 C2 115.0(3) . . ?
C8 C3 C2 124.0(3) . . ?
C8 C3 C4 120.9(3) . . ?
C3 C4 C1 114.8(2) . . ?
C5 C4 C1 124.2(3) . . ?
C5 C4 C3 121.0(3) . . ?
C20 C19 H19 120.1 . . ?
C20 C19 C18 119.8(3) . . ?
C18 C19 H19 120.1 . . ?
C19 C18 H18 120.1 . . ?
C17 C18 C19 119.8(3) . . ?
C17 C18 H18 120.1 . . ?
C15 C16 H16 120.0 . . ?
C17 C16 C15 119.9(3) . . ?
C17 C16 H16 120.0 . . ?
C10 C9 P2 116.7(2) . . ?
C14 C9 P2 123.8(2) . . ?
C14 C9 C10 119.4(3) . . ?
C18 C17 C16 120.7(3) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C9 C10 H10 120.1 . . ?
C11 C10 C9 119.8(3) . . ?
C11 C10 H10 120.1 . . ?
C4 C5 H5 120.9 . . ?
C4 C5 C6 118.2(3) . . ?
C6 C5 H5 120.9 . . ?
C5 C6 H6 119.7 . . ?
C5 C6 C7 120.6(3) . . ?
C7 C6 H6 119.7 . . ?
C3 C8 H8 121.0 . . ?
C3 C8 C7 118.1(3) . . ?
C7 C8 H8 121.0 . . ?
C11 C12 H12 120.4 . . ?
C11 C12 C13 119.2(3) . . ?
C13 C12 H12 120.4 . . ?
C6 C7 H7 119.4 . . ?
C8 C7 C6 121.1(3) . . ?
C8 C7 H7 119.4 . . ?
C10 C11 H11 119.6 . . ?
C12 C11 C10 120.7(3) . . ?
C12 C11 H11 119.6 . . ?
C12 C13 H13 119.6 . . ?
C14 C13 C12 120.8(4) . . ?
C14 C13 H13 119.6 . . ?
C9 C14 H14 120.0 . . ?
C13 C14 C9 120.0(3) . . ?
C13 C14 H14 120.0 . . ?

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
P2 P1 C2 O2 -76.3(3) . . . . ?
P2 P1 C2 C3 103.50(18) . . . . ?
P2 P1 C1 O1 72.0(3) . . . . ?
P2 P1 C1 C4 -109.47(18) . . . . ?
P2 C15 C16 C17 175.1(3) . . . . ?
P2 C9 C10 C11 177.3(3) . . . . ?
P2 C9 C14 C13 -178.7(3) . . . . ?
P1 P2 C15 C20 159.7(2) . . . . ?
P1 P2 C15 C16 -17.1(3) . . . . ?
P1 P2 C9 C10 -86.0(2) . . . . ?
P1 P2 C9 C14 92.7(3) . . . . ?
P1 C2 C3 C4 -5.8(3) . . . . ?
P1 C2 C3 C8 175.1(2) . . . . ?
P1 C1 C4 C3 6.2(3) . . . . ?
P1 C1 C4 C5 -174.4(2) . . . . ?
O1 C1 C4 C3 -175.2(3) . . . . ?
O1 C1 C4 C5 4.1(5) . . . . ?
O2 C2 C3 C4 174.0(3) . . . . ?
O2 C2 C3 C8 -5.1(5) . . . . ?
C20 C15 C16 C17 -1.6(5) . . . . ?
C20 C19 C18 C17 -1.4(5) . . . . ?
C15 P2 C9 C10 169.4(2) . . . . ?
C15 P2 C9 C14 -11.9(3) . . . . ?
C15 C20 C19 C18 1.2(5) . . . . ?
C15 C16 C17 C18 1.4(6) . . . . ?
C2 P1 C1 O1 173.7(3) . . . . ?
C2 P1 C1 C4 -7.7(2) . . . . ?
C2 C3 C4 C1 -0.3(4) . . . . ?
C2 C3 C4 C5 -179.7(3) . . . . ?
C2 C3 C8 C7 179.8(3) . . . . ?
C1 P1 C2 O2 -172.2(3) . . . . ?
C1 P1 C2 C3 7.6(2) . . . . ?
C1 C4 C5 C6 -179.5(3) . . . . ?
C3 C4 C5 C6 -0.2(4) . . . . ?
C3 C8 C7 C6 -0.1(5) . . . . ?
C4 C3 C8 C7 0.7(5) . . . . ?
C4 C5 C6 C7 0.8(5) . . . . ?
C19 C20 C15 P2 -176.7(2) . . . . ?
C19 C20 C15 C16 0.3(4) . . . . ?
C19 C18 C17 C16 0.1(6) . . . . ?
C9 P2 C15 C20 -93.7(2) . . . . ?
C9 P2 C15 C16 89.5(3) . . . . ?
C9 C10 C11 C12 1.6(5) . . . . ?
C10 C9 C14 C13 0.0(5) . . . . ?
C5 C6 C7 C8 -0.6(5) . . . . ?
C8 C3 C4 C1 178.8(3) . . . . ?
C8 C3 C4 C5 -0.6(4) . . . . ?
C12 C13 C14 C9 1.4(6) . . . . ?
C11 C12 C13 C14 -1.2(6) . . . . ?
C13 C12 C11 C10 -0.2(6) . . . . ?
C14 C9 C10 C11 -1.4(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.516
_oxdiff_exptl_absorpt_empirical_full_min 0.470
####################################################################### 
# 
# 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_exp_598
_database_code_depnum_ccdc_archive 'CCDC 1894667'
loop_
_audit_author_name
_audit_author_address
'Zhongshu Li'
;Lehn Institute of Functional Materials (LIFM), School of Chemistry, Sun Yat Sen University
China
;
_audit_update_record             
;
2022-06-02 deposited with the CCDC.	2022-06-06 downloaded from the CCDC.
;
_audit_creation_date             2022-06-02
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C38 H48 Al N2 O2 P'
_chemical_formula_sum            'C38 H48 Al N2 O2 P'
_chemical_formula_weight         622.73
_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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   13.08240(10)
_cell_length_b                   20.5977(2)
_cell_length_c                   13.70050(10)
_cell_angle_alpha                90
_cell_angle_beta                 104.1500(10)
_cell_angle_gamma                90
_cell_volume                     3579.82(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12190
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.8430
_cell_measurement_theta_min      3.9870
_shelx_estimated_absorpt_T_max   0.902
_shelx_estimated_absorpt_T_min   0.882
_exptl_absorpt_coefficient_mu    1.173
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21246
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.182
_diffrn_reflns_theta_min         3.960
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     46.00  89.00   0.50    2.00    --    0.00  38.00  30.00   86
  2  ω     36.00  85.00   0.50    2.00    --    0.00  82.00 150.00   98
  3  ω    -23.00   5.00   0.50    2.00    --    0.00  82.00 150.00   56
  4  ω    -18.00   9.00   0.50    2.00    --    0.00 -38.00 -90.00   54
  5  ω    -17.00  19.00   0.50    2.00    --    0.00  38.00  30.00   72
  6  ω    132.00 183.00   0.50    8.00    --   95.20  61.00  90.00  102
  7  ω     76.00 117.00   0.50    8.00    --   95.20 -61.00-180.00   82
  8  ω     16.00  55.00   0.50    8.00    --   95.20 -30.00-180.00   78
  9  ω     22.00 125.00   0.50    8.00    --   95.20 -77.00-180.00  206
 10  ω     72.00 175.00   0.50    8.00    --   95.20  15.00 -60.00  206
 11  ω      6.00 119.00   0.50    8.00    --   95.20 -61.00  30.00  226
 12  ω     78.00 110.00   0.50    8.00    --   95.20  45.00 -30.00   64
 13  ω     72.00 172.00   0.50    8.00    --   95.20  61.00 -30.00  200
 14  ω     82.00 108.00   0.50    8.00    --   95.20 -30.00-180.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0188899000
_diffrn_orient_matrix_UB_12      0.0209231000
_diffrn_orient_matrix_UB_13      -0.1109099000
_diffrn_orient_matrix_UB_21      -0.0422572000
_diffrn_orient_matrix_UB_22      0.0659333000
_diffrn_orient_matrix_UB_23      0.0258813000
_diffrn_orient_matrix_UB_31      0.1123652000
_diffrn_orient_matrix_UB_32      0.0283306000
_diffrn_orient_matrix_UB_33      0.0216106000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6339
_reflns_number_total             7076
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7076
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0392
_refine_ls_restrained_S_all      1.083
_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)+(0.0508P)²+1.2262P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1087
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(P1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Sof(H9BD)=Sof(H9BE)=Sof(H9BF)=1-FVAR(1)
 Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=FVAR(1)
 Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(2)
 Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C22(H22), C36(H36), C25(H25), C34(H34)
4.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C31(H31), C19(H19), C11(H11), C29(H29), C18(H18), C30(H30), C5(H5),
 C8(H8), C7(H7), C6(H6)
4.c Idealised Me refined as rotating group:
 C9(H9AA,H9AB,H9AC), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C23(H23A,H23B,
 H23C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C33(H33A,
 H33B,H33C), C37(H37A,H37B,H37C), C35(H35A,H35B,H35C), C38(H38A,H38B,H38C)
;
_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
Al2 Al 0.72530(3) 0.34572(2) 0.67607(3) 0.02167(10) Uani 1 1 d . . . . .
P1 P 0.48865(3) 0.44169(2) 0.70502(3) 0.04170(12) Uani 1 1 d . U . . .
O1 O 0.66251(7) 0.36590(5) 0.77560(7) 0.0282(2) Uani 1 1 d . . . . .
N2 N 0.77733(8) 0.42432(5) 0.63438(8) 0.0234(2) Uani 1 1 d . . . . .
N1 N 0.62140(8) 0.32877(5) 0.55715(8) 0.0227(2) Uani 1 1 d . . . . .
C15 C 0.88000(10) 0.44967(6) 0.68632(10) 0.0249(3) Uani 1 1 d . . . . .
C12 C 0.57602(10) 0.37787(7) 0.49728(10) 0.0263(3) Uani 1 1 d . . . . .
C16 C 0.96996(11) 0.42740(7) 0.65757(11) 0.0272(3) Uani 1 1 d . . . . .
C27 C 0.58945(10) 0.26334(6) 0.52346(10) 0.0242(3) Uani 1 1 d . . . . .
C20 C 0.88684(11) 0.49559(7) 0.76372(11) 0.0275(3) Uani 1 1 d . . . . .
C10 C 0.71634(11) 0.46077(7) 0.56214(10) 0.0263(3) Uani 1 1 d . . . . .
O2 O 0.33096(11) 0.48175(9) 0.79059(14) 0.0769(5) Uani 1 1 d . . . . .
C32 C 0.50862(11) 0.23187(7) 0.55551(11) 0.0280(3) Uani 1 1 d . . . . .
C28 C 0.64107(11) 0.23381(7) 0.45635(10) 0.0287(3) Uani 1 1 d . . . . .
C1 C 0.58063(11) 0.39616(7) 0.78983(11) 0.0292(3) Uani 1 1 d . . . . .
C17 C 1.06722(11) 0.45394(8) 0.70689(11) 0.0327(3) Uani 1 1 d . . . . .
H17 H 1.127914 0.440043 0.689227 0.039 Uiso 1 1 calc R U . . .
C9 C 0.82386(12) 0.27576(7) 0.72502(12) 0.0315(3) Uani 1 1 d . . . . .
H9AA H 0.894571 0.292324 0.739719 0.047 Uiso 0.42(5) 1 calc R U P A 1
H9AB H 0.815893 0.242593 0.674493 0.047 Uiso 0.42(5) 1 calc R U P A 1
H9AC H 0.809875 0.257757 0.785080 0.047 Uiso 0.42(5) 1 calc R U P A 1
C31 C 0.47598(12) 0.17094(7) 0.51430(11) 0.0340(3) Uani 1 1 d . . . . .
H31 H 0.421326 0.149528 0.533338 0.041 Uiso 1 1 calc R U . . .
C19 C 0.98627(12) 0.52034(7) 0.80971(12) 0.0327(3) Uani 1 1 d . . . . .
H19 H 0.992654 0.551005 0.860676 0.039 Uiso 1 1 calc R U . . .
C11 C 0.61795(11) 0.44025(7) 0.50464(11) 0.0287(3) Uani 1 1 d . . . . .
H11 H 0.575604 0.472111 0.466889 0.034 Uiso 1 1 calc R U . . .
C22 C 0.79217(12) 0.51707(7) 0.80185(12) 0.0340(3) Uani 1 1 d . . . . .
H22 H 0.728760 0.498523 0.757185 0.041 Uiso 1 1 calc R U . . .
C29 C 0.60616(13) 0.17269(8) 0.41858(11) 0.0351(3) Uani 1 1 d . . . . .
H29 H 0.639223 0.152187 0.374137 0.042 Uiso 1 1 calc R U . . .
C36 C 0.73162(12) 0.26705(8) 0.42477(11) 0.0348(3) Uani 1 1 d . . . . .
H36 H 0.756272 0.302370 0.472656 0.042 Uiso 1 1 calc R U . . .
C25 C 0.96272(11) 0.37696(7) 0.57500(11) 0.0309(3) Uani 1 1 d . . . . .
H25 H 0.903043 0.348569 0.576595 0.037 Uiso 1 1 calc R U . . .
C18 C 1.07531(12) 0.50023(8) 0.78110(12) 0.0345(3) Uani 1 1 d . . . . .
H18 H 1.140687 0.517877 0.811840 0.041 Uiso 1 1 calc R U . . .
C13 C 0.47558(12) 0.36590(8) 0.41772(12) 0.0370(3) Uani 1 1 d . . . . .
H13A H 0.486716 0.331646 0.373926 0.055 Uiso 1 1 calc R U . . .
H13B H 0.455506 0.404810 0.379242 0.055 Uiso 1 1 calc R U . . .
H13C H 0.420601 0.353612 0.449348 0.055 Uiso 1 1 calc R U . . .
C14 C 0.75297(13) 0.52681(8) 0.53726(13) 0.0352(3) Uani 1 1 d . . . . .
H14A H 0.747197 0.557118 0.588864 0.053 Uiso 0.74(3) 1 calc R U P B 1
H14B H 0.709917 0.541121 0.473751 0.053 Uiso 0.74(3) 1 calc R U P B 1
H14C H 0.825122 0.524199 0.533313 0.053 Uiso 0.74(3) 1 calc R U P B 1
C4 C 0.56262(12) 0.39160(7) 0.89219(11) 0.0329(3) Uani 1 1 d . . . . .
C30 C 0.52358(13) 0.14208(7) 0.44584(12) 0.0364(3) Uani 1 1 d . . . . .
H30 H 0.499946 0.101973 0.418102 0.044 Uiso 1 1 calc R U . . .
C34 C 0.45987(12) 0.26123(8) 0.63488(12) 0.0358(3) Uani 1 1 d . . . . .
H34 H 0.481631 0.306850 0.642551 0.043 Uiso 1 1 calc R U . . .
C3 C 0.47190(13) 0.42386(8) 0.90123(14) 0.0418(4) Uani 1 1 d . . . . .
C23 C 0.77878(14) 0.59113(8) 0.80174(15) 0.0472(4) Uani 1 1 d . . . . .
H23A H 0.836188 0.610060 0.850834 0.071 Uiso 1 1 calc R U . . .
H23B H 0.713434 0.601714 0.818050 0.071 Uiso 1 1 calc R U . . .
H23C H 0.778332 0.607912 0.736269 0.071 Uiso 1 1 calc R U . . .
C21 C 0.80106(14) 0.49026(9) 0.90763(13) 0.0421(4) Uani 1 1 d . . . . .
H21A H 0.808903 0.443930 0.906935 0.063 Uiso 1 1 calc R U . . .
H21B H 0.738534 0.501004 0.929045 0.063 Uiso 1 1 calc R U . . .
H21C H 0.861342 0.508991 0.953349 0.063 Uiso 1 1 calc R U . . .
C5 C 0.62614(15) 0.36033(9) 0.97359(12) 0.0440(4) Uani 1 1 d . . . . .
H5 H 0.685878 0.337873 0.967309 0.053 Uiso 1 1 calc R U . . .
C2 C 0.41494(14) 0.45385(9) 0.80321(16) 0.0487(4) Uani 1 1 d . . . . .
C24 C 1.06040(16) 0.33413(10) 0.59093(16) 0.0547(5) Uani 1 1 d . . . . .
H24A H 1.119229 0.359700 0.583116 0.082 Uiso 1 1 calc R U . . .
H24B H 1.047858 0.299693 0.542231 0.082 Uiso 1 1 calc R U . . .
H24C H 1.075639 0.316000 0.657483 0.082 Uiso 1 1 calc R U . . .
C26 C 0.94013(15) 0.40777(9) 0.47031(13) 0.0437(4) Uani 1 1 d . . . . .
H26A H 0.872404 0.428545 0.456012 0.065 Uiso 1 1 calc R U . . .
H26B H 0.940299 0.374724 0.420934 0.065 Uiso 1 1 calc R U . . .
H26C H 0.993498 0.439375 0.468269 0.065 Uiso 1 1 calc R U . . .
C33 C 0.50286(17) 0.22822(10) 0.73601(14) 0.0523(5) Uani 1 1 d . . . . .
H33A H 0.481703 0.183473 0.731470 0.079 Uiso 1 1 calc R U . . .
H33B H 0.475574 0.249521 0.786613 0.079 Uiso 1 1 calc R U . . .
H33C H 0.578419 0.230852 0.753723 0.079 Uiso 1 1 calc R U . . .
C37 C 0.69698(16) 0.29749(10) 0.32058(13) 0.0511(5) Uani 1 1 d . . . . .
H37A H 0.668279 0.264503 0.272113 0.077 Uiso 1 1 calc R U . . .
H37B H 0.756598 0.317279 0.303224 0.077 Uiso 1 1 calc R U . . .
H37C H 0.644244 0.329867 0.320729 0.077 Uiso 1 1 calc R U . . .
C8 C 0.44477(18) 0.42618(11) 0.99237(18) 0.0605(6) Uani 1 1 d . . . . .
H8 H 0.383981 0.447564 0.998351 0.073 Uiso 1 1 calc R U . . .
C35 C 0.33933(15) 0.26001(12) 0.60594(18) 0.0622(6) Uani 1 1 d . . . . .
H35A H 0.314075 0.278173 0.539898 0.093 Uiso 1 1 calc R U . . .
H35B H 0.313011 0.285089 0.653597 0.093 Uiso 1 1 calc R U . . .
H35C H 0.315226 0.216000 0.606157 0.093 Uiso 1 1 calc R U . . .
C7 C 0.5105(2) 0.39577(12) 1.07533(16) 0.0657(6) Uani 1 1 d . . . . .
H7 H 0.494287 0.397641 1.137695 0.079 Uiso 1 1 calc R U . . .
C6 C 0.59880(19) 0.36313(11) 1.06551(15) 0.0600(5) Uani 1 1 d . . . . .
H6 H 0.641186 0.342490 1.121286 0.072 Uiso 1 1 calc R U . . .
C38 C 0.82421(16) 0.22142(12) 0.43075(18) 0.0612(6) Uani 1 1 d . . . . .
H38A H 0.844520 0.202643 0.496800 0.092 Uiso 1 1 calc R U . . .
H38B H 0.882500 0.245230 0.417592 0.092 Uiso 1 1 calc R U . . .
H38C H 0.804119 0.187573 0.381632 0.092 Uiso 1 1 calc R U . . .
H9BD H 0.881(4) 0.291(2) 0.778(4) 0.064(13) Uiso 0.58(5) 1 d . . P A 2
H9BE H 0.785(3) 0.236(2) 0.742(4) 0.050(11) Uiso 0.58(5) 1 d . . P A 2
H9BF H 0.864(4) 0.258(2) 0.672(3) 0.053(11) Uiso 0.58(5) 1 d . . P A 2
H14D H 0.764(6) 0.521(4) 0.464(6) 0.04(2) Uiso 0.26(3) 1 d . . P B 2
H14E H 0.692(5) 0.559(3) 0.521(5) 0.026(18) Uiso 0.26(3) 1 d . . P B 2
H14F H 0.806(5) 0.543(3) 0.579(5) 0.019(16) Uiso 0.26(3) 1 d . . P B 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
Al2 O1 1.8041(10) . ?
Al2 N2 1.8976(12) . ?
Al2 N1 1.8818(12) . ?
Al2 C9 1.9406(15) . ?
P1 C1 1.7303(15) . ?
P1 C2 1.854(2) . ?
O1 C1 1.2947(17) . ?
N2 C15 1.4546(17) . ?
N2 C10 1.3393(17) . ?
N1 C12 1.3453(17) . ?
N1 C27 1.4526(17) . ?
C15 C16 1.4061(19) . ?
C15 C20 1.407(2) . ?
C12 C11 1.391(2) . ?
C12 C13 1.5084(19) . ?
C16 C17 1.398(2) . ?
C16 C25 1.522(2) . ?
C27 C32 1.3993(19) . ?
C27 C28 1.4053(19) . ?
C20 C19 1.396(2) . ?
C20 C22 1.523(2) . ?
C10 C11 1.400(2) . ?
C10 C14 1.509(2) . ?
O2 C2 1.214(2) . ?
C32 C31 1.400(2) . ?
C32 C34 1.515(2) . ?
C28 C29 1.395(2) . ?
C28 C36 1.520(2) . ?
C1 C4 1.481(2) . ?
C17 H17 0.9300 . ?
C17 C18 1.379(2) . ?
C9 H9AA 0.9600 . ?
C9 H9AB 0.9600 . ?
C9 H9AC 0.9600 . ?
C9 H9BD 0.95(4) . ?
C9 H9BE 1.02(4) . ?
C9 H9BF 1.06(4) . ?
C31 H31 0.9300 . ?
C31 C30 1.381(2) . ?
C19 H19 0.9300 . ?
C19 C18 1.380(2) . ?
C11 H11 0.9300 . ?
C22 H22 0.9800 . ?
C22 C23 1.535(2) . ?
C22 C21 1.529(2) . ?
C29 H29 0.9300 . ?
C29 C30 1.379(2) . ?
C36 H36 0.9800 . ?
C36 C37 1.523(2) . ?
C36 C38 1.519(2) . ?
C25 H25 0.9800 . ?
C25 C24 1.524(2) . ?
C25 C26 1.530(2) . ?
C18 H18 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C14 H14D 1.05(7) . ?
C14 H14E 1.03(6) . ?
C14 H14F 0.86(6) . ?
C4 C3 1.392(2) . ?
C4 C5 1.377(2) . ?
C30 H30 0.9300 . ?
C34 H34 0.9800 . ?
C34 C33 1.522(3) . ?
C34 C35 1.529(2) . ?
C3 C2 1.500(3) . ?
C3 C8 1.380(3) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C5 H5 0.9300 . ?
C5 C6 1.392(2) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C8 H8 0.9300 . ?
C8 C7 1.395(4) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C7 H7 0.9300 . ?
C7 C6 1.372(3) . ?
C6 H6 0.9300 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Al2 N2 107.10(5) . . ?
O1 Al2 N1 109.34(5) . . ?
O1 Al2 C9 107.26(6) . . ?
N2 Al2 C9 118.73(6) . . ?
N1 Al2 N2 97.70(5) . . ?
N1 Al2 C9 116.09(6) . . ?
C1 P1 C2 89.18(8) . . ?
C1 O1 Al2 140.46(9) . . ?
C15 N2 Al2 121.02(8) . . ?
C10 N2 Al2 120.53(9) . . ?
C10 N2 C15 118.19(11) . . ?
C12 N1 Al2 120.40(9) . . ?
C12 N1 C27 117.00(11) . . ?
C27 N1 Al2 122.55(8) . . ?
C16 C15 N2 118.81(12) . . ?
C16 C15 C20 121.79(12) . . ?
C20 C15 N2 119.40(12) . . ?
N1 C12 C11 122.87(12) . . ?
N1 C12 C13 119.62(13) . . ?
C11 C12 C13 117.51(12) . . ?
C15 C16 C25 121.78(12) . . ?
C17 C16 C15 117.54(13) . . ?
C17 C16 C25 120.68(13) . . ?
C32 C27 N1 120.72(12) . . ?
C32 C27 C28 121.72(13) . . ?
C28 C27 N1 117.55(12) . . ?
C15 C20 C22 123.13(12) . . ?
C19 C20 C15 117.79(13) . . ?
C19 C20 C22 119.03(13) . . ?
N2 C10 C11 123.11(13) . . ?
N2 C10 C14 120.51(13) . . ?
C11 C10 C14 116.37(12) . . ?
C27 C32 C31 117.92(13) . . ?
C27 C32 C34 121.57(13) . . ?
C31 C32 C34 120.48(13) . . ?
C27 C28 C36 121.60(13) . . ?
C29 C28 C27 117.85(13) . . ?
C29 C28 C36 120.54(13) . . ?
O1 C1 P1 128.68(11) . . ?
O1 C1 C4 116.18(13) . . ?
C4 C1 P1 115.15(11) . . ?
C16 C17 H17 119.2 . . ?
C18 C17 C16 121.57(14) . . ?
C18 C17 H17 119.2 . . ?
Al2 C9 H9AA 109.5 . . ?
Al2 C9 H9AB 109.5 . . ?
Al2 C9 H9AC 109.5 . . ?
Al2 C9 H9BD 111(2) . . ?
Al2 C9 H9BE 110.0(19) . . ?
Al2 C9 H9BF 114(2) . . ?
H9AA C9 H9AB 109.5 . . ?
H9AA C9 H9AC 109.5 . . ?
H9AB C9 H9AC 109.5 . . ?
H9BD C9 H9BE 115(3) . . ?
H9BD C9 H9BF 101(3) . . ?
H9BE C9 H9BF 105(3) . . ?
C32 C31 H31 119.5 . . ?
C30 C31 C32 121.08(14) . . ?
C30 C31 H31 119.5 . . ?
C20 C19 H19 119.3 . . ?
C18 C19 C20 121.34(14) . . ?
C18 C19 H19 119.3 . . ?
C12 C11 C10 127.71(13) . . ?
C12 C11 H11 116.1 . . ?
C10 C11 H11 116.1 . . ?
C20 C22 H22 107.9 . . ?
C20 C22 C23 112.98(13) . . ?
C20 C22 C21 109.91(12) . . ?
C23 C22 H22 107.9 . . ?
C21 C22 H22 107.9 . . ?
C21 C22 C23 110.01(14) . . ?
C28 C29 H29 119.4 . . ?
C30 C29 C28 121.29(14) . . ?
C30 C29 H29 119.4 . . ?
C28 C36 H36 107.2 . . ?
C28 C36 C37 112.22(13) . . ?
C37 C36 H36 107.2 . . ?
C38 C36 C28 111.88(15) . . ?
C38 C36 H36 107.2 . . ?
C38 C36 C37 110.84(15) . . ?
C16 C25 H25 107.2 . . ?
C16 C25 C24 113.03(13) . . ?
C16 C25 C26 112.11(13) . . ?
C24 C25 H25 107.2 . . ?
C24 C25 C26 109.72(14) . . ?
C26 C25 H25 107.2 . . ?
C17 C18 C19 119.92(14) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
C10 C14 H14D 104(4) . . ?
C10 C14 H14E 112(3) . . ?
C10 C14 H14F 117(4) . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
H14D C14 H14E 99(5) . . ?
H14D C14 H14F 114(5) . . ?
H14E C14 H14F 110(5) . . ?
C3 C4 C1 112.99(14) . . ?
C5 C4 C1 126.34(14) . . ?
C5 C4 C3 120.67(15) . . ?
C31 C30 H30 120.0 . . ?
C29 C30 C31 120.03(14) . . ?
C29 C30 H30 120.0 . . ?
C32 C34 H34 107.3 . . ?
C32 C34 C33 110.39(14) . . ?
C32 C34 C35 113.32(14) . . ?
C33 C34 H34 107.3 . . ?
C33 C34 C35 110.90(15) . . ?
C35 C34 H34 107.3 . . ?
C4 C3 C2 111.38(15) . . ?
C8 C3 C4 120.71(19) . . ?
C8 C3 C2 127.90(18) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C4 C5 H5 120.8 . . ?
C4 C5 C6 118.40(18) . . ?
C6 C5 H5 120.8 . . ?
O2 C2 P1 125.01(18) . . ?
O2 C2 C3 123.81(19) . . ?
C3 C2 P1 111.18(11) . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
C25 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C34 C33 H33A 109.5 . . ?
C34 C33 H33B 109.5 . . ?
C34 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C3 C8 H8 120.7 . . ?
C3 C8 C7 118.57(19) . . ?
C7 C8 H8 120.7 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C8 C7 H7 119.8 . . ?
C6 C7 C8 120.43(18) . . ?
C6 C7 H7 119.8 . . ?
C5 C6 H6 119.4 . . ?
C7 C6 C5 121.2(2) . . ?
C7 C6 H6 119.4 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 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
Al2 O1 C1 P1 -6.0(2) . . . . ?
Al2 O1 C1 C4 174.09(11) . . . . ?
Al2 N2 C15 C16 85.73(14) . . . . ?
Al2 N2 C15 C20 -94.23(13) . . . . ?
Al2 N2 C10 C11 -8.41(19) . . . . ?
Al2 N2 C10 C14 172.97(11) . . . . ?
Al2 N1 C12 C11 15.69(18) . . . . ?
Al2 N1 C12 C13 -164.67(11) . . . . ?
Al2 N1 C27 C32 88.47(14) . . . . ?
Al2 N1 C27 C28 -92.83(13) . . . . ?
P1 C1 C4 C3 1.62(17) . . . . ?
P1 C1 C4 C5 -177.60(14) . . . . ?
O1 Al2 N2 C15 85.28(10) . . . . ?
O1 Al2 N2 C10 -88.67(11) . . . . ?
O1 Al2 N1 C12 83.33(11) . . . . ?
O1 Al2 N1 C27 -99.19(10) . . . . ?
O1 C1 C4 C3 -178.46(13) . . . . ?
O1 C1 C4 C5 2.3(2) . . . . ?
N2 Al2 O1 C1 68.67(16) . . . . ?
N2 Al2 N1 C12 -27.89(11) . . . . ?
N2 Al2 N1 C27 149.60(10) . . . . ?
N2 C15 C16 C17 178.27(12) . . . . ?
N2 C15 C16 C25 -0.94(19) . . . . ?
N2 C15 C20 C19 -178.04(12) . . . . ?
N2 C15 C20 C22 4.5(2) . . . . ?
N2 C10 C11 C12 -13.2(2) . . . . ?
N1 Al2 O1 C1 -36.19(16) . . . . ?
N1 Al2 N2 C15 -161.69(10) . . . . ?
N1 Al2 N2 C10 24.36(11) . . . . ?
N1 C12 C11 C10 9.1(2) . . . . ?
N1 C27 C32 C31 175.13(12) . . . . ?
N1 C27 C32 C34 -6.9(2) . . . . ?
N1 C27 C28 C29 -175.91(12) . . . . ?
N1 C27 C28 C36 3.68(19) . . . . ?
C15 N2 C10 C11 177.47(13) . . . . ?
C15 N2 C10 C14 -1.14(19) . . . . ?
C15 C16 C17 C18 0.0(2) . . . . ?
C15 C16 C25 C24 -149.28(15) . . . . ?
C15 C16 C25 C26 86.07(17) . . . . ?
C15 C20 C19 C18 -0.5(2) . . . . ?
C15 C20 C22 C23 -127.31(15) . . . . ?
C15 C20 C22 C21 109.40(16) . . . . ?
C12 N1 C27 C32 -93.96(15) . . . . ?
C12 N1 C27 C28 84.74(15) . . . . ?
C16 C15 C20 C19 2.0(2) . . . . ?
C16 C15 C20 C22 -175.43(13) . . . . ?
C16 C17 C18 C19 1.4(2) . . . . ?
C27 N1 C12 C11 -161.93(13) . . . . ?
C27 N1 C12 C13 17.70(18) . . . . ?
C27 C32 C31 C30 1.4(2) . . . . ?
C27 C32 C34 C33 -102.34(16) . . . . ?
C27 C32 C34 C35 132.59(17) . . . . ?
C27 C28 C29 C30 0.1(2) . . . . ?
C27 C28 C36 C37 -101.44(17) . . . . ?
C27 C28 C36 C38 133.24(16) . . . . ?
C20 C15 C16 C17 -1.8(2) . . . . ?
C20 C15 C16 C25 179.02(13) . . . . ?
C20 C19 C18 C17 -1.2(2) . . . . ?
C10 N2 C15 C16 -100.18(15) . . . . ?
C10 N2 C15 C20 79.86(16) . . . . ?
C32 C27 C28 C29 2.8(2) . . . . ?
C32 C27 C28 C36 -177.63(13) . . . . ?
C32 C31 C30 C29 1.4(2) . . . . ?
C28 C27 C32 C31 -3.5(2) . . . . ?
C28 C27 C32 C34 174.42(13) . . . . ?
C28 C29 C30 C31 -2.1(2) . . . . ?
C1 P1 C2 O2 -175.89(19) . . . . ?
C1 P1 C2 C3 3.39(13) . . . . ?
C1 C4 C3 C2 1.11(19) . . . . ?
C1 C4 C3 C8 -178.07(16) . . . . ?
C1 C4 C5 C6 177.62(17) . . . . ?
C17 C16 C25 C24 31.5(2) . . . . ?
C17 C16 C25 C26 -93.12(17) . . . . ?
C9 Al2 O1 C1 -162.85(15) . . . . ?
C9 Al2 N2 C15 -36.22(12) . . . . ?
C9 Al2 N2 C10 149.83(11) . . . . ?
C9 Al2 N1 C12 -155.21(10) . . . . ?
C9 Al2 N1 C27 22.27(12) . . . . ?
C31 C32 C34 C33 75.54(18) . . . . ?
C31 C32 C34 C35 -49.5(2) . . . . ?
C19 C20 C22 C23 55.29(19) . . . . ?
C19 C20 C22 C21 -68.01(17) . . . . ?
C22 C20 C19 C18 177.03(14) . . . . ?
C29 C28 C36 C37 78.15(19) . . . . ?
C29 C28 C36 C38 -47.2(2) . . . . ?
C36 C28 C29 C30 -179.49(14) . . . . ?
C25 C16 C17 C18 179.26(13) . . . . ?
C13 C12 C11 C10 -170.51(14) . . . . ?
C14 C10 C11 C12 165.48(15) . . . . ?
C4 C3 C2 P1 -3.16(18) . . . . ?
C4 C3 C2 O2 176.13(18) . . . . ?
C4 C3 C8 C7 0.3(3) . . . . ?
C4 C5 C6 C7 0.4(3) . . . . ?
C34 C32 C31 C30 -176.54(14) . . . . ?
C3 C4 C5 C6 -1.5(3) . . . . ?
C3 C8 C7 C6 -1.4(3) . . . . ?
C5 C4 C3 C2 -179.63(16) . . . . ?
C5 C4 C3 C8 1.2(3) . . . . ?
C2 P1 C1 O1 177.22(14) . . . . ?
C2 P1 C1 C4 -2.87(12) . . . . ?
C2 C3 C8 C7 -178.73(18) . . . . ?
C8 C3 C2 P1 175.94(16) . . . . ?
C8 C3 C2 O2 -4.8(3) . . . . ?
C8 C7 C6 C5 1.1(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.338
_oxdiff_exptl_absorpt_empirical_full_min 0.786
####################################################################### 
# 
# 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_exp_684
_database_code_depnum_ccdc_archive 'CCDC 2162217'
loop_
_audit_author_name
_audit_author_address
'Xiaodan Chen'
;Jinan University
China
;
_audit_update_record             
;
2022-05-18 deposited with the CCDC.	2022-06-06 downloaded from the CCDC.
;
_audit_creation_date             2022-05-09
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H19 O2 P'
_chemical_formula_sum            'C27 H19 O2 P'
_chemical_formula_weight         406.39
_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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.9231(2)
_cell_length_b                   15.9165(3)
_cell_length_c                   23.5573(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.171(2)
_cell_angle_gamma                90
_cell_volume                     4092.67(13)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    6989
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.2660
_cell_measurement_theta_min      3.7530
_shelx_estimated_absorpt_T_max   0.935
_shelx_estimated_absorpt_T_min   0.876
_exptl_absorpt_coefficient_mu    1.354
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            20142
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.379
_diffrn_reflns_theta_min         3.352
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00  17.00   0.50   14.54    --    0.00 -19.00 -60.00  134
  2  ω    -17.00  49.00   0.50   14.54    --    0.00  19.00-150.00  132
  3  ω     14.00  41.00   0.50   14.54    --    0.00  57.00   0.00   54
  4  ω     59.00  88.00   0.50   14.54    --    0.00  19.00-150.00   58
  5  ω    -88.00 -59.00   0.50   14.54    --    0.00 -19.00 -60.00   58
  6  ω     13.00 119.00   0.50   50.00    --   95.20 -61.00   0.00  212
  7  ω     81.00 184.00   0.50   50.00    --   95.20  45.00 150.00  206
  8  ω      6.00 117.00   0.50   50.00    --   95.20 -15.00   0.00  222
  9  ω     77.00 103.00   0.50   50.00    --   95.20 -45.00  30.00   52
 10  ω      6.00 107.00   0.50   50.00    --   95.20 -45.00 150.00  202
 11  ω     11.00  36.00   0.50   50.00    --   95.20 -82.00   0.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0605856000
_diffrn_orient_matrix_UB_12      0.0587258000
_diffrn_orient_matrix_UB_13      0.0426990000
_diffrn_orient_matrix_UB_21      -0.0069172000
_diffrn_orient_matrix_UB_22      0.0700781000
_diffrn_orient_matrix_UB_23      -0.0450937000
_diffrn_orient_matrix_UB_31      -0.1272715000
_diffrn_orient_matrix_UB_32      -0.0318260000
_diffrn_orient_matrix_UB_33      -0.0206158000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5852
_reflns_number_total             7820
_reflns_odcompleteness_completeness 97.04
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         7820
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0517
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0772P)²+0.8636P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1440
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Aromatic/amide H refined with riding coordinates:
 C47(H47), C43(H43), C5(H5), C21(H21), C53(H53), C44(H44), C27(H27), C46(H46),
 C23(H23), C45(H45), C6(H6), C52(H52), C49(H49), C24(H24), C7(H7), C8(H8),
 C15(H15), C17(H17), C19(H19), C25(H25), C20(H20), C11(H11), C18(H18), C26(H26),
  C13(H13), C14(H14), C12(H12), C51(H51), C41(H41), C50(H50), C35(H35),
 C37(H37), C34(H34), C32(H32), C40(H40), C38(H38), C33(H33), C39(H39)
;
_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 0.36883(5) 0.40787(4) 0.44842(2) 0.03559(15) Uani 1 1 d . . . . .
P2 P 0.63837(6) 0.95747(4) 0.38012(3) 0.03650(16) Uani 1 1 d . . . . .
O1 O 0.53041(15) 0.52653(11) 0.40905(8) 0.0467(4) Uani 1 1 d . . . . .
O004 O 0.51267(17) 0.85274(11) 0.45222(7) 0.0492(4) Uani 1 1 d . . . . .
O005 O 0.88317(19) 1.00227(12) 0.39640(9) 0.0611(5) Uani 1 1 d . . . . .
O2 O 0.12365(17) 0.42449(12) 0.47044(9) 0.0600(5) Uani 1 1 d . . . . .
C10 C 0.4538(2) 0.29737(14) 0.36633(9) 0.0348(5) Uani 1 1 d . . . . .
C22 C 0.3173(2) 0.41719(14) 0.32946(9) 0.0350(5) Uani 1 1 d . . . . .
C42 C 0.5498(2) 0.82212(13) 0.32162(9) 0.0320(5) Uani 1 1 d . . . . .
C48 C 0.7822(2) 0.82061(14) 0.34026(9) 0.0335(5) Uani 1 1 d . . . . .
C4 C 0.3529(2) 0.58051(15) 0.45320(9) 0.0348(5) Uani 1 1 d . . . . .
C30 C 0.6680(2) 0.87397(14) 0.32467(9) 0.0335(5) Uani 1 1 d . . . . .
C3 C 0.3398(2) 0.35196(14) 0.37690(9) 0.0333(5) Uani 1 1 d . . . . .
C1 C 0.4336(2) 0.51378(15) 0.43132(10) 0.0365(5) Uani 1 1 d . . . . .
C47 C 0.5491(2) 0.73505(14) 0.32411(10) 0.0360(5) Uani 1 1 d . . . . .
H47 H 0.622843 0.706080 0.328146 0.043 Uiso 1 1 calc R U . . .
C16 C 0.2290(2) 0.29385(14) 0.38497(9) 0.0355(5) Uani 1 1 d . . . . .
C9 C 0.2398(2) 0.55190(15) 0.47095(10) 0.0368(5) Uani 1 1 d . . . . .
C43 C 0.4372(2) 0.86351(14) 0.31548(9) 0.0364(5) Uani 1 1 d . . . . .
H43 H 0.435570 0.921801 0.312852 0.044 Uiso 1 1 calc R U . . .
C5 C 0.3821(2) 0.66540(15) 0.45654(10) 0.0393(5) Uani 1 1 d . . . . .
H5 H 0.457550 0.684901 0.445087 0.047 Uiso 1 1 calc R U . . .
C21 C 0.2159(2) 0.25023(14) 0.43565(10) 0.0396(5) Uani 1 1 d . . . . .
H21 H 0.272478 0.258618 0.465607 0.047 Uiso 1 1 calc R U . . .
C53 C 0.7945(2) 0.78042(15) 0.39295(10) 0.0388(5) Uani 1 1 d . . . . .
H53 H 0.734006 0.787445 0.419267 0.047 Uiso 1 1 calc R U . . .
C44 C 0.3281(2) 0.81934(15) 0.31323(10) 0.0401(5) Uani 1 1 d . . . . .
H44 H 0.253970 0.848010 0.309996 0.048 Uiso 1 1 calc R U . . .
C27 C 0.4020(2) 0.43256(15) 0.28845(10) 0.0394(5) Uani 1 1 d . . . . .
H27 H 0.474760 0.402183 0.289063 0.047 Uiso 1 1 calc R U . . .
C46 C 0.4401(2) 0.69075(15) 0.32066(10) 0.0407(5) Uani 1 1 d . . . . .
H46 H 0.441460 0.632344 0.321615 0.049 Uiso 1 1 calc R U . . .
C23 C 0.2092(2) 0.46449(15) 0.32720(10) 0.0409(5) Uani 1 1 d . . . . .
H23 H 0.150630 0.455505 0.354180 0.049 Uiso 1 1 calc R U . . .
C45 C 0.3292(2) 0.73244(15) 0.31580(10) 0.0413(5) Uani 1 1 d . . . . .
H45 H 0.256103 0.702440 0.314264 0.050 Uiso 1 1 calc R U . . .
C36 C 0.6832(2) 0.92332(15) 0.26888(10) 0.0393(5) Uani 1 1 d . . . . .
C6 C 0.2964(2) 0.72013(16) 0.47728(10) 0.0430(6) Uani 1 1 d . . . . .
H6 H 0.314122 0.777228 0.479269 0.052 Uiso 1 1 calc R U . . .
C29 C 0.5908(2) 0.90610(15) 0.44708(10) 0.0396(5) Uani 1 1 d . . . . .
C00U C 0.6600(2) 0.94686(16) 0.49519(11) 0.0444(6) Uani 1 1 d . . . . .
C2 C 0.2207(2) 0.45965(16) 0.46370(10) 0.0410(5) Uani 1 1 d . . . . .
C52 C 0.8947(2) 0.73051(16) 0.40670(11) 0.0450(6) Uani 1 1 d . . . . .
H52 H 0.900171 0.703511 0.441713 0.054 Uiso 1 1 calc R U . . .
C49 C 0.8734(2) 0.80797(17) 0.30228(10) 0.0437(6) Uani 1 1 d . . . . .
H49 H 0.866676 0.832750 0.266550 0.052 Uiso 1 1 calc R U . . .
C24 C 0.1883(3) 0.52428(15) 0.28550(11) 0.0484(6) Uani 1 1 d . . . . .
H24 H 0.115926 0.555102 0.284752 0.058 Uiso 1 1 calc R U . . .
C7 C 0.1843(2) 0.69132(17) 0.49519(11) 0.0455(6) Uani 1 1 d . . . . .
H7 H 0.128412 0.729275 0.509373 0.055 Uiso 1 1 calc R U . . .
C8 C 0.1547(2) 0.60712(16) 0.49224(11) 0.0432(6) Uani 1 1 d . . . . .
H8 H 0.079596 0.587876 0.504229 0.052 Uiso 1 1 calc R U . . .
C15 C 0.4412(2) 0.22182(15) 0.33711(11) 0.0439(6) Uani 1 1 d . . . . .
H15 H 0.363463 0.203573 0.325271 0.053 Uiso 1 1 calc R U . . .
C17 C 0.1450(2) 0.27776(16) 0.34048(11) 0.0427(6) Uani 1 1 d . . . . .
H17 H 0.152138 0.305531 0.306028 0.051 Uiso 1 1 calc R U . . .
C19 C 0.0364(2) 0.18001(16) 0.39786(12) 0.0478(6) Uani 1 1 d . . . . .
H19 H -0.028632 0.143206 0.402427 0.057 Uiso 1 1 calc R U . . .
C25 C 0.2736(3) 0.53876(16) 0.24496(11) 0.0501(7) Uani 1 1 d . . . . .
H25 H 0.259362 0.579205 0.216996 0.060 Uiso 1 1 calc R U . . .
C20 C 0.1205(2) 0.19488(15) 0.44209(11) 0.0454(6) Uani 1 1 d . . . . .
H20 H 0.112522 0.167231 0.476527 0.054 Uiso 1 1 calc R U . . .
C11 C 0.5712(2) 0.32330(17) 0.38225(11) 0.0453(6) Uani 1 1 d . . . . .
H11 H 0.582479 0.374125 0.401221 0.054 Uiso 1 1 calc R U . . .
C18 C 0.0506(3) 0.22058(17) 0.34706(12) 0.0497(6) Uani 1 1 d . . . . .
H18 H -0.003733 0.209579 0.316629 0.060 Uiso 1 1 calc R U . . .
C28 C 0.7858(2) 0.98596(15) 0.41734(12) 0.0449(6) Uani 1 1 d . . . . .
C26 C 0.3804(3) 0.49239(16) 0.24649(11) 0.0480(6) Uani 1 1 d . . . . .
H26 H 0.438229 0.501323 0.219167 0.058 Uiso 1 1 calc R U . . .
C13 C 0.6583(3) 0.19941(17) 0.34215(11) 0.0486(6) Uani 1 1 d . . . . .
H13 H 0.726222 0.166613 0.334568 0.058 Uiso 1 1 calc R U . . .
C31 C 0.7639(3) 0.99051(16) 0.47878(11) 0.0468(6) Uani 1 1 d . . . . .
C14 C 0.5422(3) 0.17324(16) 0.32529(12) 0.0517(7) Uani 1 1 d . . . . .
H14 H 0.531734 0.122707 0.305885 0.062 Uiso 1 1 calc R U . . .
C12 C 0.6723(2) 0.27453(18) 0.37029(11) 0.0499(6) Uani 1 1 d . . . . .
H12 H 0.750332 0.292918 0.381454 0.060 Uiso 1 1 calc R U . . .
C51 C 0.9868(3) 0.72048(19) 0.36881(11) 0.0525(7) Uani 1 1 d . . . . .
H51 H 1.055592 0.688356 0.378406 0.063 Uiso 1 1 calc R U . . .
C41 C 0.6213(3) 0.90263(19) 0.21891(11) 0.0507(7) Uani 1 1 d . . . . .
H41 H 0.567527 0.857308 0.218144 0.061 Uiso 1 1 calc R U . . .
C50 C 0.9750(3) 0.7589(2) 0.31645(12) 0.0550(7) Uani 1 1 d . . . . .
H50 H 1.035829 0.751904 0.290309 0.066 Uiso 1 1 calc R U . . .
C35 C 0.6289(3) 0.94334(19) 0.55133(11) 0.0574(8) Uani 1 1 d . . . . .
H35 H 0.560329 0.913725 0.562364 0.069 Uiso 1 1 calc R U . . .
C37 C 0.7644(3) 0.99103(17) 0.26823(13) 0.0551(7) Uani 1 1 d . . . . .
H37 H 0.807916 1.006030 0.301382 0.066 Uiso 1 1 calc R U . . .
C34 C 0.7041(4) 0.9859(2) 0.59092(13) 0.0737(11) Uani 1 1 d . . . . .
H34 H 0.684430 0.985143 0.628990 0.088 Uiso 1 1 calc R U . . .
C32 C 0.8383(3) 1.03199(19) 0.51921(14) 0.0644(9) Uani 1 1 d . . . . .
H32 H 0.907823 1.060973 0.508650 0.077 Uiso 1 1 calc R U . . .
C40 C 0.6378(3) 0.9484(2) 0.16954(13) 0.0679(9) Uani 1 1 d . . . . .
H40 H 0.594808 0.933648 0.136203 0.081 Uiso 1 1 calc R U . . .
C38 C 0.7809(3) 1.0360(2) 0.21900(16) 0.0737(10) Uani 1 1 d . . . . .
H38 H 0.835657 1.080773 0.219322 0.088 Uiso 1 1 calc R U . . .
C33 C 0.8063(4) 1.0289(2) 0.57516(15) 0.0757(11) Uani 1 1 d . . . . .
H33 H 0.854737 1.056370 0.602691 0.091 Uiso 1 1 calc R U . . .
C39 C 0.7174(3) 1.0154(2) 0.16964(15) 0.0736(10) Uani 1 1 d . . . . .
H39 H 0.727945 1.046309 0.136673 0.088 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 C3 1.921(2) . ?
P1 C1 1.878(2) . ?
P1 C2 1.863(3) . ?
P2 C30 1.900(2) . ?
P2 C29 1.868(3) . ?
P2 C28 1.860(3) . ?
O1 C1 1.215(3) . ?
O004 C29 1.213(3) . ?
O005 C28 1.218(3) . ?
O2 C2 1.215(3) . ?
C10 C3 1.546(3) . ?
C10 C15 1.390(3) . ?
C10 C11 1.386(3) . ?
C22 C3 1.538(3) . ?
C22 C27 1.384(3) . ?
C22 C23 1.399(3) . ?
C42 C30 1.532(3) . ?
C42 C47 1.387(3) . ?
C42 C43 1.398(3) . ?
C48 C30 1.542(3) . ?
C48 C53 1.398(3) . ?
C48 C49 1.379(3) . ?
C4 C1 1.485(3) . ?
C4 C9 1.396(3) . ?
C4 C5 1.390(3) . ?
C30 C36 1.545(3) . ?
C3 C16 1.541(3) . ?
C47 H47 0.9300 . ?
C47 C46 1.383(3) . ?
C16 C21 1.393(3) . ?
C16 C17 1.390(3) . ?
C9 C2 1.492(3) . ?
C9 C8 1.387(3) . ?
C43 H43 0.9300 . ?
C43 C44 1.382(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.381(3) . ?
C21 H21 0.9300 . ?
C21 C20 1.377(3) . ?
C53 H53 0.9300 . ?
C53 C52 1.381(3) . ?
C44 H44 0.9300 . ?
C44 C45 1.384(3) . ?
C27 H27 0.9300 . ?
C27 C26 1.387(3) . ?
C46 H46 0.9300 . ?
C46 C45 1.382(3) . ?
C23 H23 0.9300 . ?
C23 C24 1.380(3) . ?
C45 H45 0.9300 . ?
C36 C41 1.375(4) . ?
C36 C37 1.396(4) . ?
C6 H6 0.9300 . ?
C6 C7 1.388(4) . ?
C29 C00U 1.488(3) . ?
C00U C31 1.397(4) . ?
C00U C35 1.379(4) . ?
C52 H52 0.9300 . ?
C52 C51 1.379(4) . ?
C49 H49 0.9300 . ?
C49 C50 1.387(4) . ?
C24 H24 0.9300 . ?
C24 C25 1.379(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.380(4) . ?
C8 H8 0.9300 . ?
C15 H15 0.9300 . ?
C15 C14 1.384(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.388(3) . ?
C19 H19 0.9300 . ?
C19 C20 1.383(4) . ?
C19 C18 1.374(4) . ?
C25 H25 0.9300 . ?
C25 C26 1.379(4) . ?
C20 H20 0.9300 . ?
C11 H11 0.9300 . ?
C11 C12 1.387(4) . ?
C18 H18 0.9300 . ?
C28 C31 1.478(4) . ?
C26 H26 0.9300 . ?
C13 H13 0.9300 . ?
C13 C14 1.379(4) . ?
C13 C12 1.373(4) . ?
C31 C32 1.395(4) . ?
C14 H14 0.9300 . ?
C12 H12 0.9300 . ?
C51 H51 0.9300 . ?
C51 C50 1.379(4) . ?
C41 H41 0.9300 . ?
C41 C40 1.390(4) . ?
C50 H50 0.9300 . ?
C35 H35 0.9300 . ?
C35 C34 1.395(5) . ?
C37 H37 0.9300 . ?
C37 C38 1.381(4) . ?
C34 H34 0.9300 . ?
C34 C33 1.373(5) . ?
C32 H32 0.9300 . ?
C32 C33 1.377(5) . ?
C40 H40 0.9300 . ?
C40 C39 1.375(5) . ?
C38 H38 0.9300 . ?
C38 C39 1.371(5) . ?
C33 H33 0.9300 . ?
C39 H39 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 C3 106.19(10) . . ?
C2 P1 C3 104.98(10) . . ?
C2 P1 C1 88.95(11) . . ?
C29 P2 C30 109.55(10) . . ?
C28 P2 C30 109.12(11) . . ?
C28 P2 C29 88.42(12) . . ?
C15 C10 C3 120.0(2) . . ?
C11 C10 C3 122.1(2) . . ?
C11 C10 C15 117.7(2) . . ?
C27 C22 C3 122.3(2) . . ?
C27 C22 C23 117.6(2) . . ?
C23 C22 C3 120.1(2) . . ?
C47 C42 C30 122.8(2) . . ?
C47 C42 C43 117.9(2) . . ?
C43 C42 C30 119.20(19) . . ?
C53 C48 C30 120.9(2) . . ?
C49 C48 C30 121.6(2) . . ?
C49 C48 C53 117.5(2) . . ?
C9 C4 C1 114.5(2) . . ?
C5 C4 C1 125.2(2) . . ?
C5 C4 C9 120.3(2) . . ?
C42 C30 P2 104.11(14) . . ?
C42 C30 C48 112.77(17) . . ?
C42 C30 C36 110.59(18) . . ?
C48 C30 P2 112.27(15) . . ?
C48 C30 C36 111.74(18) . . ?
C36 C30 P2 104.82(15) . . ?
C10 C3 P1 107.10(15) . . ?
C22 C3 P1 109.93(14) . . ?
C22 C3 C10 111.68(18) . . ?
C22 C3 C16 112.99(18) . . ?
C16 C3 P1 105.93(14) . . ?
C16 C3 C10 108.89(18) . . ?
O1 C1 P1 125.72(18) . . ?
O1 C1 C4 124.6(2) . . ?
C4 C1 P1 109.50(16) . . ?
C42 C47 H47 119.6 . . ?
C46 C47 C42 120.9(2) . . ?
C46 C47 H47 119.6 . . ?
C21 C16 C3 120.8(2) . . ?
C17 C16 C3 121.1(2) . . ?
C17 C16 C21 117.9(2) . . ?
C4 C9 C2 114.1(2) . . ?
C8 C9 C4 121.0(2) . . ?
C8 C9 C2 124.9(2) . . ?
C42 C43 H43 119.4 . . ?
C44 C43 C42 121.2(2) . . ?
C44 C43 H43 119.4 . . ?
C4 C5 H5 120.8 . . ?
C6 C5 C4 118.4(2) . . ?
C6 C5 H5 120.8 . . ?
C16 C21 H21 119.5 . . ?
C20 C21 C16 121.0(2) . . ?
C20 C21 H21 119.5 . . ?
C48 C53 H53 119.3 . . ?
C52 C53 C48 121.3(2) . . ?
C52 C53 H53 119.3 . . ?
C43 C44 H44 120.0 . . ?
C43 C44 C45 120.0(2) . . ?
C45 C44 H44 120.0 . . ?
C22 C27 H27 119.4 . . ?
C22 C27 C26 121.2(2) . . ?
C26 C27 H27 119.4 . . ?
C47 C46 H46 119.7 . . ?
C45 C46 C47 120.6(2) . . ?
C45 C46 H46 119.7 . . ?
C22 C23 H23 119.5 . . ?
C24 C23 C22 121.0(2) . . ?
C24 C23 H23 119.5 . . ?
C44 C45 H45 120.3 . . ?
C46 C45 C44 119.3(2) . . ?
C46 C45 H45 120.3 . . ?
C41 C36 C30 122.7(2) . . ?
C41 C36 C37 117.9(2) . . ?
C37 C36 C30 119.4(2) . . ?
C5 C6 H6 119.4 . . ?
C5 C6 C7 121.1(2) . . ?
C7 C6 H6 119.4 . . ?
O004 C29 P2 127.60(19) . . ?
O004 C29 C00U 124.6(2) . . ?
C00U C29 P2 107.62(18) . . ?
C31 C00U C29 113.6(2) . . ?
C35 C00U C29 125.2(3) . . ?
C35 C00U C31 121.2(3) . . ?
O2 C2 P1 126.2(2) . . ?
O2 C2 C9 123.9(2) . . ?
C9 C2 P1 109.81(17) . . ?
C53 C52 H52 119.8 . . ?
C51 C52 C53 120.4(2) . . ?
C51 C52 H52 119.8 . . ?
C48 C49 H49 119.4 . . ?
C48 C49 C50 121.1(2) . . ?
C50 C49 H49 119.4 . . ?
C23 C24 H24 119.7 . . ?
C25 C24 C23 120.7(3) . . ?
C25 C24 H24 119.7 . . ?
C6 C7 H7 119.6 . . ?
C8 C7 C6 120.9(2) . . ?
C8 C7 H7 119.6 . . ?
C9 C8 H8 120.8 . . ?
C7 C8 C9 118.4(2) . . ?
C7 C8 H8 120.8 . . ?
C10 C15 H15 119.4 . . ?
C14 C15 C10 121.2(3) . . ?
C14 C15 H15 119.4 . . ?
C16 C17 H17 119.7 . . ?
C18 C17 C16 120.5(2) . . ?
C18 C17 H17 119.7 . . ?
C20 C19 H19 120.6 . . ?
C18 C19 H19 120.6 . . ?
C18 C19 C20 118.8(2) . . ?
C24 C25 H25 120.5 . . ?
C24 C25 C26 119.0(2) . . ?
C26 C25 H25 120.5 . . ?
C21 C20 C19 120.7(2) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C10 C11 H11 119.5 . . ?
C10 C11 C12 120.9(2) . . ?
C12 C11 H11 119.5 . . ?
C17 C18 H18 119.5 . . ?
C19 C18 C17 121.0(2) . . ?
C19 C18 H18 119.5 . . ?
O005 C28 P2 128.0(2) . . ?
O005 C28 C31 124.2(3) . . ?
C31 C28 P2 107.72(19) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 C27 120.5(3) . . ?
C25 C26 H26 119.8 . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C12 C13 C14 119.1(2) . . ?
C00U C31 C28 114.2(2) . . ?
C32 C31 C00U 120.3(3) . . ?
C32 C31 C28 125.5(3) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 C15 120.3(3) . . ?
C13 C14 H14 119.8 . . ?
C11 C12 H12 119.6 . . ?
C13 C12 C11 120.7(3) . . ?
C13 C12 H12 119.6 . . ?
C52 C51 H51 120.6 . . ?
C50 C51 C52 118.8(2) . . ?
C50 C51 H51 120.6 . . ?
C36 C41 H41 119.5 . . ?
C36 C41 C40 121.0(3) . . ?
C40 C41 H41 119.5 . . ?
C49 C50 H50 119.6 . . ?
C51 C50 C49 120.8(2) . . ?
C51 C50 H50 119.6 . . ?
C00U C35 H35 121.3 . . ?
C00U C35 C34 117.4(3) . . ?
C34 C35 H35 121.3 . . ?
C36 C37 H37 119.6 . . ?
C38 C37 C36 120.9(3) . . ?
C38 C37 H37 119.6 . . ?
C35 C34 H34 119.1 . . ?
C33 C34 C35 121.7(3) . . ?
C33 C34 H34 119.1 . . ?
C31 C32 H32 120.9 . . ?
C33 C32 C31 118.3(3) . . ?
C33 C32 H32 120.9 . . ?
C41 C40 H40 119.8 . . ?
C39 C40 C41 120.5(3) . . ?
C39 C40 H40 119.8 . . ?
C37 C38 H38 119.7 . . ?
C39 C38 C37 120.7(3) . . ?
C39 C38 H38 119.7 . . ?
C34 C33 C32 121.0(3) . . ?
C34 C33 H33 119.5 . . ?
C32 C33 H33 119.5 . . ?
C40 C39 H39 120.5 . . ?
C38 C39 C40 119.1(3) . . ?
C38 C39 H39 120.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C3 C16 C21 -39.0(3) . . . . ?
P1 C3 C16 C17 146.6(2) . . . . ?
P2 C30 C36 C41 -130.4(2) . . . . ?
P2 C30 C36 C37 50.7(3) . . . . ?
P2 C29 C00U C31 -18.6(2) . . . . ?
P2 C29 C00U C35 161.7(2) . . . . ?
P2 C28 C31 C00U 20.7(3) . . . . ?
P2 C28 C31 C32 -160.8(2) . . . . ?
O004 C29 C00U C31 165.4(2) . . . . ?
O004 C29 C00U C35 -14.3(4) . . . . ?
O005 C28 C31 C00U -162.4(2) . . . . ?
O005 C28 C31 C32 16.2(4) . . . . ?
C10 C3 C16 C21 75.9(3) . . . . ?
C10 C3 C16 C17 -98.5(2) . . . . ?
C10 C15 C14 C13 -0.4(4) . . . . ?
C10 C11 C12 C13 0.2(4) . . . . ?
C22 C3 C16 C21 -159.4(2) . . . . ?
C22 C3 C16 C17 26.2(3) . . . . ?
C22 C27 C26 C25 0.6(4) . . . . ?
C22 C23 C24 C25 0.1(4) . . . . ?
C42 C30 C36 C41 -18.7(3) . . . . ?
C42 C30 C36 C37 162.4(2) . . . . ?
C42 C47 C46 C45 -1.3(4) . . . . ?
C42 C43 C44 C45 -1.5(3) . . . . ?
C48 C30 C36 C41 107.8(3) . . . . ?
C48 C30 C36 C37 -71.1(3) . . . . ?
C48 C53 C52 C51 1.3(4) . . . . ?
C48 C49 C50 C51 0.8(4) . . . . ?
C4 C9 C2 P1 12.9(3) . . . . ?
C4 C9 C2 O2 -171.2(2) . . . . ?
C4 C9 C8 C7 0.3(4) . . . . ?
C4 C5 C6 C7 0.9(4) . . . . ?
C30 P2 C29 O004 -49.3(2) . . . . ?
C30 P2 C29 C00U 134.79(16) . . . . ?
C30 P2 C28 O005 47.3(3) . . . . ?
C30 P2 C28 C31 -135.89(16) . . . . ?
C30 C42 C47 C46 -179.4(2) . . . . ?
C30 C42 C43 C44 -179.2(2) . . . . ?
C30 C48 C53 C52 178.1(2) . . . . ?
C30 C48 C49 C50 -179.1(2) . . . . ?
C30 C36 C41 C40 -179.8(2) . . . . ?
C30 C36 C37 C38 179.5(3) . . . . ?
C3 P1 C1 O1 -63.6(2) . . . . ?
C3 P1 C1 C4 120.68(15) . . . . ?
C3 P1 C2 O2 61.9(3) . . . . ?
C3 P1 C2 C9 -122.36(17) . . . . ?
C3 C10 C15 C14 177.7(2) . . . . ?
C3 C10 C11 C12 -177.5(2) . . . . ?
C3 C22 C27 C26 -179.2(2) . . . . ?
C3 C22 C23 C24 178.9(2) . . . . ?
C3 C16 C21 C20 -176.6(2) . . . . ?
C3 C16 C17 C18 175.3(2) . . . . ?
C1 P1 C2 O2 168.4(2) . . . . ?
C1 P1 C2 C9 -15.87(17) . . . . ?
C1 C4 C9 C2 -0.9(3) . . . . ?
C1 C4 C9 C8 -179.8(2) . . . . ?
C1 C4 C5 C6 179.2(2) . . . . ?
C47 C42 C30 P2 -131.16(19) . . . . ?
C47 C42 C30 C48 -9.2(3) . . . . ?
C47 C42 C30 C36 116.7(2) . . . . ?
C47 C42 C43 C44 1.4(3) . . . . ?
C47 C46 C45 C44 1.3(4) . . . . ?
C16 C21 C20 C19 1.3(4) . . . . ?
C16 C17 C18 C19 1.4(4) . . . . ?
C9 C4 C1 P1 -11.4(2) . . . . ?
C9 C4 C1 O1 172.8(2) . . . . ?
C9 C4 C5 C6 -0.5(3) . . . . ?
C43 C42 C30 P2 49.5(2) . . . . ?
C43 C42 C30 C48 171.49(19) . . . . ?
C43 C42 C30 C36 -62.6(3) . . . . ?
C43 C42 C47 C46 -0.1(3) . . . . ?
C43 C44 C45 C46 0.1(4) . . . . ?
C5 C4 C1 P1 168.87(19) . . . . ?
C5 C4 C1 O1 -6.9(4) . . . . ?
C5 C4 C9 C2 178.8(2) . . . . ?
C5 C4 C9 C8 -0.1(3) . . . . ?
C5 C6 C7 C8 -0.7(4) . . . . ?
C21 C16 C17 C18 0.7(4) . . . . ?
C53 C48 C30 P2 53.6(2) . . . . ?
C53 C48 C30 C42 -63.7(3) . . . . ?
C53 C48 C30 C36 171.0(2) . . . . ?
C53 C48 C49 C50 -1.6(4) . . . . ?
C53 C52 C51 C50 -2.0(4) . . . . ?
C27 C22 C3 P1 108.7(2) . . . . ?
C27 C22 C3 C10 -10.0(3) . . . . ?
C27 C22 C3 C16 -133.2(2) . . . . ?
C27 C22 C23 C24 0.0(3) . . . . ?
C23 C22 C3 P1 -70.2(2) . . . . ?
C23 C22 C3 C10 171.1(2) . . . . ?
C23 C22 C3 C16 47.9(3) . . . . ?
C23 C22 C27 C26 -0.3(3) . . . . ?
C23 C24 C25 C26 0.2(4) . . . . ?
C36 C41 C40 C39 0.3(5) . . . . ?
C36 C37 C38 C39 0.3(5) . . . . ?
C6 C7 C8 C9 0.0(4) . . . . ?
C29 P2 C30 C42 53.86(17) . . . . ?
C29 P2 C30 C48 -68.43(18) . . . . ?
C29 P2 C30 C36 170.07(15) . . . . ?
C29 P2 C28 O005 157.5(3) . . . . ?
C29 P2 C28 C31 -25.73(17) . . . . ?
C29 C00U C31 C28 -1.3(3) . . . . ?
C29 C00U C31 C32 -179.9(2) . . . . ?
C29 C00U C35 C34 -179.6(2) . . . . ?
C00U C31 C32 C33 -0.3(4) . . . . ?
C00U C35 C34 C33 -0.9(4) . . . . ?
C2 P1 C1 O1 -168.9(2) . . . . ?
C2 P1 C1 C4 15.38(16) . . . . ?
C2 C9 C8 C7 -178.5(2) . . . . ?
C52 C51 C50 C49 1.0(5) . . . . ?
C49 C48 C30 P2 -129.0(2) . . . . ?
C49 C48 C30 C42 113.8(2) . . . . ?
C49 C48 C30 C36 -11.5(3) . . . . ?
C49 C48 C53 C52 0.5(3) . . . . ?
C24 C25 C26 C27 -0.5(4) . . . . ?
C8 C9 C2 P1 -168.2(2) . . . . ?
C8 C9 C2 O2 7.7(4) . . . . ?
C15 C10 C3 P1 147.52(19) . . . . ?
C15 C10 C3 C22 -92.1(2) . . . . ?
C15 C10 C3 C16 33.4(3) . . . . ?
C15 C10 C11 C12 -1.2(4) . . . . ?
C17 C16 C21 C20 -2.0(4) . . . . ?
C20 C19 C18 C17 -2.2(4) . . . . ?
C11 C10 C3 P1 -36.3(3) . . . . ?
C11 C10 C3 C22 84.1(3) . . . . ?
C11 C10 C3 C16 -150.4(2) . . . . ?
C11 C10 C15 C14 1.3(4) . . . . ?
C18 C19 C20 C21 0.9(4) . . . . ?
C28 P2 C30 C42 149.14(15) . . . . ?
C28 P2 C30 C48 26.85(18) . . . . ?
C28 P2 C30 C36 -94.64(17) . . . . ?
C28 P2 C29 O004 -159.1(2) . . . . ?
C28 P2 C29 C00U 25.04(17) . . . . ?
C28 C31 C32 C33 -178.7(3) . . . . ?
C31 C00U C35 C34 0.8(4) . . . . ?
C31 C32 C33 C34 0.2(5) . . . . ?
C14 C13 C12 C11 0.7(4) . . . . ?
C12 C13 C14 C15 -0.6(4) . . . . ?
C41 C36 C37 C38 0.5(4) . . . . ?
C41 C40 C39 C38 0.5(5) . . . . ?
C35 C00U C31 C28 178.4(2) . . . . ?
C35 C00U C31 C32 -0.3(4) . . . . ?
C35 C34 C33 C32 0.3(5) . . . . ?
C37 C36 C41 C40 -0.8(4) . . . . ?
C37 C38 C39 C40 -0.8(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.165
_oxdiff_exptl_absorpt_empirical_full_min 0.845
####################################################################### 
# 
# 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_exp_1755
_database_code_depnum_ccdc_archive 'CCDC 1894671'
loop_
_audit_author_name
_audit_author_address
'Zhongshu Li'
;Lehn Institute of Functional Materials, School of Chemistry, Sun Yat Sen University
China
;
_audit_update_record             
;
2022-05-18 deposited with the CCDC.	2022-06-06 downloaded from the CCDC.
;
_audit_creation_date             2022-05-09
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C34 H42 N2 O2 P2'
_chemical_formula_sum            'C34 H42 N2 O2 P2'
_chemical_formula_weight         572.63
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O P'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   11.1651(4)
_cell_length_b                   16.2523(6)
_cell_length_c                   17.4007(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90.01
_cell_volume                     3157.5(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13458
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.7530
_cell_measurement_theta_min      4.6950
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.495
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20679
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.578
_diffrn_reflns_theta_min         3.721
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 10.6525
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -49.00   35.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.6498   38.0000 -180.0000 84

#__ type_ start__ end____ width___ exp.time_
  2 omega  -79.00   32.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.6498   19.0000  120.0000 111

#__ type_ start__ end____ width___ exp.time_
  3 omega  -67.00   -5.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.6498  125.0000  -90.0000 62

#__ type_ start__ end____ width___ exp.time_
  4 omega   35.00   93.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       39.6498 -125.0000  -90.0000 58

#__ type_ start__ end____ width___ exp.time_
  5 omega   46.00   75.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       39.6498 -123.0000  103.0000 29

#__ type_ start__ end____ width___ exp.time_
  6 omega    3.00   29.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       39.6498  -99.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
  7 omega   98.00  124.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7866  125.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
  8 omega   46.00  135.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7866  -61.0000  -30.0000 89

#__ type_ start__ end____ width___ exp.time_
  9 omega   48.00   91.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7866  -30.0000   60.0000 43

#__ type_ start__ end____ width___ exp.time_
 10 omega   24.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7866  -95.0000  -60.0000 85

#__ type_ start__ end____ width___ exp.time_
 11 omega   78.00  177.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7866   30.0000   60.0000 99

#__ type_ start__ end____ width___ exp.time_
 12 omega   59.00  121.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7866 -125.0000 -180.0000 62

#__ type_ start__ end____ width___ exp.time_
 13 omega   30.00   90.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7866  -30.0000  120.0000 60

#__ type_ start__ end____ width___ exp.time_
 14 omega  136.00  166.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7866  125.0000  -60.0000 30

#__ type_ start__ end____ width___ exp.time_
 15 omega   55.00   90.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7866  -30.0000  -90.0000 35

#__ type_ start__ end____ width___ exp.time_
 16 omega   74.00  100.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7866  -95.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
 17 omega   87.00  159.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7866   45.0000  120.0000 72

#__ type_ start__ end____ width___ exp.time_
 18 omega  101.00  135.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7866 -150.0000  -58.0000 34

#__ type_ start__ end____ width___ exp.time_
 19 omega  103.00  151.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7866  125.0000  -30.0000 48

#__ type_ start__ end____ width___ exp.time_
 20 omega  111.00  172.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7866  125.0000    0.0000 61

#__ type_ start__ end____ width___ exp.time_
 21 omega   38.00   65.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7866  -30.0000 -120.0000 27

#__ type_ start__ end____ width___ exp.time_
 22 omega   69.00   98.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7866  -45.0000 -120.0000 29
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0723490000
_diffrn_orient_matrix_UB_12      -0.0169267000
_diffrn_orient_matrix_UB_13      0.0740350000
_diffrn_orient_matrix_UB_21      0.1148681000
_diffrn_orient_matrix_UB_22      -0.0094870000
_diffrn_orient_matrix_UB_23      -0.0477719000
_diffrn_orient_matrix_UB_31      0.0248634000
_diffrn_orient_matrix_UB_32      0.0927635000
_diffrn_orient_matrix_UB_33      0.0086596000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5955
_reflns_number_total             6313
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         6313
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0372
_refine_ls_restrained_S_all      1.044
_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)+(0.0625P)²+1.1846P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1033
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H9(0.024) H10(0.025) H12(0.024) H16(0.023) H17(0.032) H18(0.025)
 H19(0.024) H20(0.022) H21(0.029) H23A(0.022) H23B(0.022) H24(0.027) H26(0.019)
 H27(0.025) H28A(0.033) H28B(0.033) H28C(0.033) H29A(0.045) H29B(0.045)
 H29C(0.045) H30(0.022) H31(0.031) H32A(0.053) H32B(0.053) H32C(0.053)
 H33A(0.022) H33B(0.022) H34A(0.037) H34B(0.037) H34C(0.037) H35A(0.055)
 H35B(0.055) H35C(0.055) H36A(0.055) H36B(0.055) H36C(0.055) H37A(0.051)
 H37B(0.051) H37C(0.051) H38A(0.076) H38B(0.076) H38C(0.076)
 Fixed X: H9(0.3985) H10(0.6281) H12(0.2351) H16(0.4713) H17(0.9575)
 H18(0.5095) H19(0.3496) H20(0.4932) H21(1.0377) H23A(0.2157) H23B(0.3245)
 H24(0.2154) H26(0.2888) H27(0.5142) H28A(0.4192) H28B(0.2959) H28C(0.3313)
 H29A(0.6609) H29B(0.6897) H29C(0.6858) H30(0.3024) H31(0.7561) H32A(0.3749)
 H32B(0.4957) H32C(0.4693) H33A(0.2937) H33B(0.2137) H34A(0.1312) H34B(0.1069)
 H34C(0.1086) H35A(0.2884) H35B(0.2326) H35C(0.3574) H36A(0.6757) H36B(0.6893)
 H36C(0.6442) H37A(0.4592) H37B(0.5068) H37C(0.379) H38A(0.0512) H38B(0.0455)
 H38C(0.088)
 Fixed Y: H9(0.8596) H10(0.6247) H12(1.0413) H16(0.8837) H17(0.5316)
 H18(0.7024) H19(0.9976) H20(0.7478) H21(0.6642) H23A(0.7912) H23B(0.7294)
 H24(0.9461) H26(0.9548) H27(0.7637) H28A(1.0502) H28B(1.0937) H28C(1.0654)
 H29A(0.6987) H29B(0.6552) H29C(0.7515) H30(0.9549) H31(0.5124) H32A(0.6211)
 H32B(0.574) H32C(0.6148) H33A(0.7169) H33B(0.7967) H34A(0.9874) H34B(1.0123)
 H34C(0.9192) H35A(1.1057) H35B(1.0867) H35C(1.0495) H36A(0.8422) H36B(0.7509)
 H36C(0.8187) H37A(0.7311) H37B(0.6653) H37C(0.7035) H38A(0.9599) H38B(1.0263)
 H38C(1.0511)
 Fixed Z: H9(-0.1856) H10(0.1938) H12(0.4011) H16(0.4919) H17(0.1556)
 H18(0.07) H19(0.504) H20(-0.1305) H21(0.1516) H23A(0.2469) H23B(0.2477)
 H24(0.2176) H26(0.095) H27(0.3231) H28A(0.041) H28B(0.0553) H28C(-0.0278)
 H29A(-0.0603) H29B(0.018) H29C(0.0134) H30(-0.1093) H31(0.1785) H32A(-0.0018)
 H32B(0.0116) H32C(-0.0682) H33A(0.1222) H33B(0.1194) H34A(-0.0288)
 H34B(0.0568) H34C(0.0332) H35A(0.2634) H35B(0.1827) H35C(0.2051) H36A(0.3679)
 H36B(0.3957) H36C(0.4529) H37A(0.4788) H37B(0.4205) H37C(0.4095) H38A(0.3002)
 H38B(0.2349) H38C(0.3175)
;
_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 0.47572(3) 0.86701(2) 0.17416(2) 0.01174(9) Uani 1 1 d . . . . .
P2 P 0.77865(3) 0.87798(2) 0.18359(2) 0.02053(10) Uani 1 1 d . . . . .
O1 O 0.57430(8) 0.78265(5) 0.19168(5) 0.01647(18) Uani 1 1 d . . . . .
N2 N 0.39041(9) 0.82107(6) 0.10832(6) 0.0131(2) Uani 1 1 d . . . . .
N3 N 0.37655(9) 0.84875(6) 0.24316(6) 0.0136(2) Uani 1 1 d . . . . .
C4 C 0.43596(11) 0.85951(7) 0.38014(7) 0.0156(2) Uani 1 1 d . . . . .
C5 C 0.39623(10) 0.83342(7) 0.02636(7) 0.0131(2) Uani 1 1 d . . . . .
O6 O 1.01543(9) 0.83713(7) 0.16712(8) 0.0389(3) Uani 1 1 d . . . . .
C7 C 0.88014(12) 0.72232(8) 0.17039(7) 0.0188(3) Uani 1 1 d . . . . .
C8 C 0.29140(11) 0.95633(7) 0.32438(7) 0.0163(2) Uani 1 1 d . . . . .
C9 C 0.39786(12) 0.85308(8) -0.13249(7) 0.0199(3) Uani 1 1 d . . . . .
H9 H 0.3985 0.8596 -0.1856 0.024 Uiso 1 1 calc R U . . .
C10 C 0.70955(13) 0.63258(8) 0.18534(8) 0.0210(3) Uani 1 1 d . . . . .
H10 H 0.6281 0.6247 0.1938 0.025 Uiso 1 1 calc R U . . .
C11 C 0.36982(10) 0.88900(7) 0.31675(7) 0.0138(2) Uani 1 1 d . . . . .
C12 C 0.28552(12) 0.99616(8) 0.39527(7) 0.0199(3) Uani 1 1 d . . . . .
H12 H 0.2351 1.0413 0.4011 0.024 Uiso 1 1 calc R U . . .
C13 C 0.45415(11) 0.77455(7) -0.01965(7) 0.0154(2) Uani 1 1 d . . . . .
C14 C 0.33883(10) 0.90228(7) -0.00680(7) 0.0146(2) Uani 1 1 d . . . . .
C15 C 0.69206(11) 0.78989(7) 0.18659(7) 0.0151(2) Uani 1 1 d . . . . .
C16 C 0.42704(11) 0.90166(8) 0.44987(7) 0.0190(3) Uani 1 1 d . . . . .
H16 H 0.4713 0.8837 0.4919 0.023 Uiso 1 1 calc R U . . .
C17 C 0.90803(14) 0.57692(9) 0.16274(7) 0.0264(3) Uani 1 1 d . . . . .
H17 H 0.9575 0.5316 0.1556 0.032 Uiso 1 1 calc R U . . .
C18 C 0.51747(13) 0.69999(8) 0.01398(7) 0.0208(3) Uani 1 1 d . . . . .
H18 H 0.5095 0.7024 0.0700 0.025 Uiso 1 1 calc R U . . .
C19 C 0.35350(12) 0.96968(8) 0.45742(7) 0.0198(3) Uani 1 1 d . . . . .
H19 H 0.3496 0.9976 0.5040 0.024 Uiso 1 1 calc R U . . .
C20 C 0.45446(12) 0.78588(8) -0.09925(7) 0.0187(3) Uani 1 1 d . . . . .
H20 H 0.4932 0.7478 -0.1305 0.022 Uiso 1 1 calc R U . . .
C21 C 0.95631(12) 0.65614(9) 0.16009(7) 0.0240(3) Uani 1 1 d . . . . .
H21 H 1.0377 0.6642 0.1516 0.029 Uiso 1 1 calc R U . . .
C22 C 0.91325(12) 0.81150(9) 0.17189(8) 0.0233(3) Uani 1 1 d . . . . .
C23 C 0.29456(12) 0.78033(8) 0.22581(7) 0.0183(3) Uani 1 1 d . . . . .
H23A H 0.2157 0.7912 0.2469 0.022 Uiso 1 1 calc R U . . .
H23B H 0.3245 0.7294 0.2477 0.022 Uiso 1 1 calc R U . . .
C24 C 0.21714(12) 0.98865(8) 0.25745(7) 0.0225(3) Uani 1 1 d . . . . .
H24 H 0.2154 0.9461 0.2176 0.027 Uiso 1 1 calc R U . . .
C25 C 0.75789(11) 0.71091(8) 0.18176(7) 0.0161(2) Uani 1 1 d . . . . .
C26 C 0.27815(11) 0.96845(7) 0.04052(7) 0.0154(2) Uani 1 1 d . . . . .
H26 H 0.2888 0.9548 0.0950 0.019 Uiso 1 1 calc R U . . .
C27 C 0.51323(12) 0.78283(8) 0.37649(7) 0.0206(3) Uani 1 1 d . . . . .
H27 H 0.5142 0.7637 0.3231 0.025 Uiso 1 1 calc R U . . .
C28 C 0.33661(12) 1.05223(8) 0.02588(8) 0.0217(3) Uani 1 1 d . . . . .
H28A H 0.4192 1.0502 0.0410 0.033 Uiso 1 1 calc R U . . .
H28B H 0.2959 1.0937 0.0553 0.033 Uiso 1 1 calc R U . . .
H28C H 0.3313 1.0654 -0.0278 0.033 Uiso 1 1 calc R U . . .
C29 C 0.65088(14) 0.70149(10) -0.00554(9) 0.0297(3) Uani 1 1 d . . . . .
H29A H 0.6609 0.6987 -0.0603 0.045 Uiso 1 1 calc R U . . .
H29B H 0.6897 0.6552 0.0180 0.045 Uiso 1 1 calc R U . . .
H29C H 0.6858 0.7515 0.0134 0.045 Uiso 1 1 calc R U . . .
C30 C 0.34056(11) 0.91026(8) -0.08656(7) 0.0182(2) Uani 1 1 d . . . . .
H30 H 0.3024 0.9549 -0.1093 0.022 Uiso 1 1 calc R U . . .
C31 C 0.78675(14) 0.56552(9) 0.17592(8) 0.0258(3) Uani 1 1 d . . . . .
H31 H 0.7561 0.5124 0.1785 0.031 Uiso 1 1 calc R U . . .
C32 C 0.45888(17) 0.62003(9) -0.01370(10) 0.0351(4) Uani 1 1 d . . . . .
H32A H 0.3749 0.6211 -0.0018 0.053 Uiso 1 1 calc R U . . .
H32B H 0.4957 0.5740 0.0116 0.053 Uiso 1 1 calc R U . . .
H32C H 0.4693 0.6148 -0.0682 0.053 Uiso 1 1 calc R U . . .
C33 C 0.28844(11) 0.77397(8) 0.13823(7) 0.0180(2) Uani 1 1 d . . . . .
H33A H 0.2937 0.7169 0.1222 0.022 Uiso 1 1 calc R U . . .
H33B H 0.2137 0.7967 0.1194 0.022 Uiso 1 1 calc R U . . .
C34 C 0.14370(12) 0.97216(8) 0.02387(9) 0.0249(3) Uani 1 1 d . . . . .
H34A H 0.1312 0.9874 -0.0288 0.037 Uiso 1 1 calc R U . . .
H34B H 0.1069 1.0123 0.0568 0.037 Uiso 1 1 calc R U . . .
H34C H 0.1086 0.9192 0.0332 0.037 Uiso 1 1 calc R U . . .
C35 C 0.27975(18) 1.06474(9) 0.22403(9) 0.0365(4) Uani 1 1 d . . . . .
H35A H 0.2884 1.1057 0.2634 0.055 Uiso 1 1 calc R U . . .
H35B H 0.2326 1.0867 0.1827 0.055 Uiso 1 1 calc R U . . .
H35C H 0.3574 1.0495 0.2051 0.055 Uiso 1 1 calc R U . . .
C36 C 0.64266(14) 0.80027(11) 0.40049(11) 0.0367(4) Uani 1 1 d . . . . .
H36A H 0.6757 0.8422 0.3679 0.055 Uiso 1 1 calc R U . . .
H36B H 0.6893 0.7509 0.3957 0.055 Uiso 1 1 calc R U . . .
H36C H 0.6442 0.8187 0.4529 0.055 Uiso 1 1 calc R U . . .
C37 C 0.45956(16) 0.71430(9) 0.42590(10) 0.0337(3) Uani 1 1 d . . . . .
H37A H 0.4592 0.7311 0.4788 0.051 Uiso 1 1 calc R U . . .
H37B H 0.5068 0.6653 0.4205 0.051 Uiso 1 1 calc R U . . .
H37C H 0.3790 0.7035 0.4095 0.051 Uiso 1 1 calc R U . . .
C38 C 0.08863(16) 1.00831(16) 0.27954(10) 0.0507(5) Uani 1 1 d . . . . .
H38A H 0.0512 0.9599 0.3002 0.076 Uiso 1 1 calc R U . . .
H38B H 0.0455 1.0263 0.2349 0.076 Uiso 1 1 calc R U . . .
H38C H 0.0880 1.0511 0.3175 0.076 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 1.7845(9) . ?
P1 N2 1.6664(10) . ?
P1 N3 1.6600(10) . ?
P2 C15 1.7283(12) . ?
P2 C22 1.8621(14) . ?
O1 C15 1.3230(15) . ?
N2 C5 1.4417(14) . ?
N2 C33 1.4673(15) . ?
N3 C11 1.4398(15) . ?
N3 C23 1.4716(15) . ?
C4 C11 1.4114(17) . ?
C4 C16 1.3969(18) . ?
C4 C27 1.5171(17) . ?
C5 C13 1.4053(16) . ?
C5 C14 1.4130(16) . ?
O6 C22 1.2173(18) . ?
C7 C21 1.3829(18) . ?
C7 C22 1.4961(19) . ?
C7 C25 1.3916(18) . ?
C8 C11 1.4077(17) . ?
C8 C12 1.3947(17) . ?
C8 C24 1.5230(17) . ?
C9 H9 0.9300 . ?
C9 C20 1.3881(19) . ?
C9 C30 1.3826(18) . ?
C10 H10 0.9300 . ?
C10 C25 1.3840(18) . ?
C10 C31 1.3993(19) . ?
C12 H12 0.9300 . ?
C12 C19 1.3897(19) . ?
C13 C18 1.5201(17) . ?
C13 C20 1.3972(17) . ?
C14 C26 1.5145(16) . ?
C14 C30 1.3941(17) . ?
C15 C25 1.4816(16) . ?
C16 H16 0.9300 . ?
C16 C19 1.3834(19) . ?
C17 H17 0.9300 . ?
C17 C21 1.397(2) . ?
C17 C31 1.386(2) . ?
C18 H18 0.9800 . ?
C18 C29 1.5280(19) . ?
C18 C32 1.533(2) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C33 1.5290(17) . ?
C24 H24 0.9800 . ?
C24 C35 1.535(2) . ?
C24 C38 1.519(2) . ?
C26 H26 0.9800 . ?
C26 C28 1.5312(16) . ?
C26 C34 1.5300(17) . ?
C27 H27 0.9800 . ?
C27 C36 1.531(2) . ?
C27 C37 1.5293(19) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 P1 O1 97.22(5) . . ?
N3 P1 O1 98.66(5) . . ?
N3 P1 N2 92.06(5) . . ?
C15 P2 C22 88.51(6) . . ?
C15 O1 P1 122.22(7) . . ?
C5 N2 P1 126.30(8) . . ?
C5 N2 C33 117.28(9) . . ?
C33 N2 P1 115.68(8) . . ?
C11 N3 P1 126.64(8) . . ?
C11 N3 C23 119.56(9) . . ?
C23 N3 P1 113.68(8) . . ?
C11 C4 C27 122.94(11) . . ?
C16 C4 C11 118.36(11) . . ?
C16 C4 C27 118.67(11) . . ?
C13 C5 N2 119.32(10) . . ?
C13 C5 C14 121.03(11) . . ?
C14 C5 N2 119.58(10) . . ?
C21 C7 C22 127.14(12) . . ?
C21 C7 C25 121.21(13) . . ?
C25 C7 C22 111.65(11) . . ?
C11 C8 C24 122.32(11) . . ?
C12 C8 C11 118.26(11) . . ?
C12 C8 C24 119.38(11) . . ?
C20 C9 H9 120.0 . . ?
C30 C9 H9 120.0 . . ?
C30 C9 C20 119.91(12) . . ?
C25 C10 H10 121.0 . . ?
C25 C10 C31 118.09(13) . . ?
C31 C10 H10 121.0 . . ?
C4 C11 N3 120.89(11) . . ?
C8 C11 N3 118.00(10) . . ?
C8 C11 C4 121.05(11) . . ?
C8 C12 H12 119.4 . . ?
C19 C12 C8 121.25(12) . . ?
C19 C12 H12 119.4 . . ?
C5 C13 C18 122.51(11) . . ?
C20 C13 C5 118.43(11) . . ?
C20 C13 C18 119.05(11) . . ?
C5 C14 C26 122.92(11) . . ?
C30 C14 C5 118.28(11) . . ?
C30 C14 C26 118.78(11) . . ?
O1 C15 P2 129.17(9) . . ?
O1 C15 C25 114.82(10) . . ?
C25 C15 P2 116.01(9) . . ?
C4 C16 H16 119.4 . . ?
C19 C16 C4 121.11(12) . . ?
C19 C16 H16 119.4 . . ?
C21 C17 H17 119.8 . . ?
C31 C17 H17 119.8 . . ?
C31 C17 C21 120.39(12) . . ?
C13 C18 H18 108.0 . . ?
C13 C18 C29 110.80(11) . . ?
C13 C18 C32 110.89(12) . . ?
C29 C18 H18 108.0 . . ?
C29 C18 C32 111.08(12) . . ?
C32 C18 H18 108.0 . . ?
C12 C19 H19 120.1 . . ?
C16 C19 C12 119.86(11) . . ?
C16 C19 H19 120.1 . . ?
C9 C20 C13 121.04(12) . . ?
C9 C20 H20 119.5 . . ?
C13 C20 H20 119.5 . . ?
C7 C21 C17 118.38(13) . . ?
C7 C21 H21 120.8 . . ?
C17 C21 H21 120.8 . . ?
O6 C22 P2 124.42(12) . . ?
O6 C22 C7 124.18(13) . . ?
C7 C22 P2 111.39(9) . . ?
N3 C23 H23A 110.4 . . ?
N3 C23 H23B 110.4 . . ?
N3 C23 C33 106.46(9) . . ?
H23A C23 H23B 108.6 . . ?
C33 C23 H23A 110.4 . . ?
C33 C23 H23B 110.4 . . ?
C8 C24 H24 108.0 . . ?
C8 C24 C35 108.64(12) . . ?
C35 C24 H24 108.0 . . ?
C38 C24 C8 113.16(12) . . ?
C38 C24 H24 108.0 . . ?
C38 C24 C35 110.88(14) . . ?
C7 C25 C15 112.29(11) . . ?
C10 C25 C7 120.75(12) . . ?
C10 C25 C15 126.94(12) . . ?
C14 C26 H26 108.1 . . ?
C14 C26 C28 110.51(10) . . ?
C14 C26 C34 111.35(10) . . ?
C28 C26 H26 108.1 . . ?
C34 C26 H26 108.1 . . ?
C34 C26 C28 110.59(10) . . ?
C4 C27 H27 107.9 . . ?
C4 C27 C36 111.93(12) . . ?
C4 C27 C37 110.60(11) . . ?
C36 C27 H27 107.9 . . ?
C37 C27 H27 107.9 . . ?
C37 C27 C36 110.57(12) . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C18 C29 H29A 109.5 . . ?
C18 C29 H29B 109.5 . . ?
C18 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C9 C30 C14 121.30(12) . . ?
C9 C30 H30 119.4 . . ?
C14 C30 H30 119.4 . . ?
C10 C31 H31 119.4 . . ?
C17 C31 C10 121.15(13) . . ?
C17 C31 H31 119.4 . . ?
C18 C32 H32A 109.5 . . ?
C18 C32 H32B 109.5 . . ?
C18 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N2 C33 C23 106.48(10) . . ?
N2 C33 H33A 110.4 . . ?
N2 C33 H33B 110.4 . . ?
C23 C33 H33A 110.4 . . ?
C23 C33 H33B 110.4 . . ?
H33A C33 H33B 108.6 . . ?
C26 C34 H34A 109.5 . . ?
C26 C34 H34B 109.5 . . ?
C26 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C24 C35 H35A 109.5 . . ?
C24 C35 H35B 109.5 . . ?
C24 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C27 C36 H36A 109.5 . . ?
C27 C36 H36B 109.5 . . ?
C27 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C27 C37 H37A 109.5 . . ?
C27 C37 H37B 109.5 . . ?
C27 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C24 C38 H38A 109.5 . . ?
C24 C38 H38B 109.5 . . ?
C24 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 O1 C15 P2 15.05(15) . . . . ?
P1 O1 C15 C25 -164.03(8) . . . . ?
P1 N2 C5 C13 101.81(12) . . . . ?
P1 N2 C5 C14 -81.20(13) . . . . ?
P1 N2 C33 C23 -1.49(13) . . . . ?
P1 N3 C11 C4 -87.56(13) . . . . ?
P1 N3 C11 C8 95.18(12) . . . . ?
P1 N3 C23 C33 -25.48(12) . . . . ?
P2 C15 C25 C7 -3.98(14) . . . . ?
P2 C15 C25 C10 177.83(11) . . . . ?
O1 P1 N2 C5 -102.54(10) . . . . ?
O1 P1 N2 C33 87.60(9) . . . . ?
O1 P1 N3 C11 100.14(10) . . . . ?
O1 P1 N3 C23 -75.79(9) . . . . ?
O1 C15 C25 C7 175.22(10) . . . . ?
O1 C15 C25 C10 -2.97(18) . . . . ?
N2 P1 O1 C15 126.13(9) . . . . ?
N2 P1 N3 C11 -162.23(10) . . . . ?
N2 P1 N3 C23 21.84(9) . . . . ?
N2 C5 C13 C18 -3.43(17) . . . . ?
N2 C5 C13 C20 177.35(11) . . . . ?
N2 C5 C14 C26 4.74(17) . . . . ?
N2 C5 C14 C30 -176.65(10) . . . . ?
N3 P1 O1 C15 -140.67(9) . . . . ?
N3 P1 N2 C5 158.46(10) . . . . ?
N3 P1 N2 C33 -11.39(9) . . . . ?
N3 C23 C33 N2 15.90(13) . . . . ?
C4 C16 C19 C12 1.07(19) . . . . ?
C5 N2 C33 C23 -172.30(10) . . . . ?
C5 C13 C18 C29 -118.29(13) . . . . ?
C5 C13 C18 C32 117.88(13) . . . . ?
C5 C13 C20 C9 -0.72(18) . . . . ?
C5 C14 C26 C28 119.62(12) . . . . ?
C5 C14 C26 C34 -117.07(13) . . . . ?
C5 C14 C30 C9 -0.71(18) . . . . ?
C8 C12 C19 C16 -1.21(19) . . . . ?
C11 N3 C23 C33 158.28(10) . . . . ?
C11 C4 C16 C19 1.30(18) . . . . ?
C11 C4 C27 C36 124.53(14) . . . . ?
C11 C4 C27 C37 -111.70(14) . . . . ?
C11 C8 C12 C19 -1.04(19) . . . . ?
C11 C8 C24 C35 -99.81(14) . . . . ?
C11 C8 C24 C38 136.60(15) . . . . ?
C12 C8 C11 N3 -179.28(11) . . . . ?
C12 C8 C11 C4 3.46(18) . . . . ?
C12 C8 C24 C35 77.82(15) . . . . ?
C12 C8 C24 C38 -45.77(19) . . . . ?
C13 C5 C14 C26 -178.33(11) . . . . ?
C13 C5 C14 C30 0.29(17) . . . . ?
C14 C5 C13 C18 179.62(11) . . . . ?
C14 C5 C13 C20 0.41(17) . . . . ?
C15 P2 C22 O6 -178.54(14) . . . . ?
C15 P2 C22 C7 0.51(10) . . . . ?
C16 C4 C11 N3 179.22(10) . . . . ?
C16 C4 C11 C8 -3.60(17) . . . . ?
C16 C4 C27 C36 -57.31(16) . . . . ?
C16 C4 C27 C37 66.47(16) . . . . ?
C18 C13 C20 C9 -179.96(12) . . . . ?
C20 C9 C30 C14 0.41(19) . . . . ?
C20 C13 C18 C29 60.92(16) . . . . ?
C20 C13 C18 C32 -62.92(15) . . . . ?
C21 C7 C22 P2 177.76(11) . . . . ?
C21 C7 C22 O6 -3.2(2) . . . . ?
C21 C7 C25 C10 1.93(19) . . . . ?
C21 C7 C25 C15 -176.39(11) . . . . ?
C21 C17 C31 C10 1.3(2) . . . . ?
C22 P2 C15 O1 -177.21(12) . . . . ?
C22 P2 C15 C25 1.86(10) . . . . ?
C22 C7 C21 C17 178.19(12) . . . . ?
C22 C7 C25 C10 -177.51(12) . . . . ?
C22 C7 C25 C15 4.17(15) . . . . ?
C23 N3 C11 C4 88.15(14) . . . . ?
C23 N3 C11 C8 -89.11(14) . . . . ?
C24 C8 C11 N3 -1.62(17) . . . . ?
C24 C8 C11 C4 -178.88(11) . . . . ?
C24 C8 C12 C19 -178.76(12) . . . . ?
C25 C7 C21 C17 -1.15(19) . . . . ?
C25 C7 C22 P2 -2.85(14) . . . . ?
C25 C7 C22 O6 176.21(14) . . . . ?
C25 C10 C31 C17 -0.5(2) . . . . ?
C26 C14 C30 C9 177.97(11) . . . . ?
C27 C4 C11 N3 -2.61(17) . . . . ?
C27 C4 C11 C8 174.58(11) . . . . ?
C27 C4 C16 C19 -176.95(11) . . . . ?
C30 C9 C20 C13 0.32(19) . . . . ?
C30 C14 C26 C28 -59.00(14) . . . . ?
C30 C14 C26 C34 64.32(14) . . . . ?
C31 C10 C25 C7 -1.07(19) . . . . ?
C31 C10 C25 C15 176.99(12) . . . . ?
C31 C17 C21 C7 -0.43(19) . . . . ?
C33 N2 C5 C13 -88.49(13) . . . . ?
C33 N2 C5 C14 88.50(13) . . . . ?

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

data_exp_2033
_database_code_depnum_ccdc_archive 'CCDC 1894669'
loop_
_audit_author_name
_audit_author_address
'Zhongshu Li'
;Lehn Institute of Functional Materials, School of Chemistry, Sun Yat Sen University
China
;
_audit_update_record             
;
2022-05-18 deposited with the CCDC.	2022-06-06 downloaded from the CCDC.
;
_audit_creation_date             2022-05-09
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_chemical_formula_moiety         'C16 H8 O4 P2'
_chemical_formula_sum            'C16 H8 O4 P2'
_chemical_formula_weight         326.187
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00330 0.00160 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C' custom
H 0.00000 0.00000 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C' custom
O 0.01060 0.00600 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C' custom
P 0.10230 0.09420 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C' custom

_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_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z+1/2
3 -x,-y,-z
4 x,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   10.5737(4)
_cell_length_b                   11.8608(3)
_cell_length_c                   11.4453(4)
_cell_angle_alpha                90
_cell_angle_beta                 100.127(3)
_cell_angle_gamma                90
_cell_volume                     1413.02(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10803
_cell_measurement_temperature    100
_cell_measurement_theta_max      150.10
_cell_measurement_theta_min      71.132
_exptl_absorpt_coefficient_mu    0.322
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       block
_exptl_crystal_F_000             665.202
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.9988
_diffrn_reflns_Laue_measured_fraction_max 0.9392
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23212
_diffrn_reflns_point_group_measured_fraction_full 0.9988
_diffrn_reflns_point_group_measured_fraction_max 0.9392
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         32.69
_diffrn_reflns_theta_min         2.97
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.9988
_diffrn_measured_fraction_theta_max 0.9392
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at Zero, Atlas'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                4201
_reflns_number_total             4867
_reflns_threshold_expression     I>=2u(I)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.4846
_refine_diff_density_min         -0.4216
_refine_diff_density_rms         0.1114
_refine_ls_d_res_high            0.6579
_refine_ls_d_res_low             6.8653
_refine_ls_goodness_of_fit_ref   1.1098
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4867
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0452
_refine_ls_restrained_S_all      1.1098
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0193P)²+0.3871P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0755
_refine_special_details          
;
Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       ORCA 5.0
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         PBE
   BASIS SET:      def2-TZVP
   CHARGE:         0
   MULTIPLICITY:   1
   DATE:           2022-04-29_09-47-23
;
_olex2_refinement_description    
;
;
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_refinement_flags_posn
P1 P 0.22239(4) 0.07976(3) 0.96139(3) 0.01918(8) Uani 1.000000 .
P2 P 0.40286(3) 0.06972(3) 0.89167(3) 0.01679(8) Uani 1.000000 .
O1 O 0.07582(11) 0.00630(8) 0.75385(8) 0.0288(2) Uani 1.000000 .
O2 O 0.32578(10) -0.03753(9) 1.16466(8) 0.0284(2) Uani 1.000000 .
C5 C 0.08323(13) -0.11676(10) 0.92109(11) 0.0173(2) Uani 1.000000 .
O3 O 0.31171(11) 0.24691(7) 0.74370(9) 0.0262(2) Uani 1.000000 .
C11 C 0.34810(12) 0.07337(9) 0.64724(11) 0.0163(2) Uani 1.000000 .
O4 O 0.38516(10) -0.15904(7) 0.84745(9) 0.0262(2) Uani 1.000000 .
C12 C 0.37314(12) -0.04008(10) 0.67635(11) 0.0157(2) Uani 1.000000 .
C1 C 0.11473(13) -0.01441(10) 0.85763(11) 0.0191(2) Uani 1.000000 .
C4 C 0.38635(13) -0.06574(10) 0.80472(11) 0.0175(2) Uani 1.000000 .
C3 C 0.34439(13) 0.14915(10) 0.74993(11) 0.0173(2) Uani 1.000000 .
C10 C -0.00221(14) -0.20042(11) 0.87134(13) 0.0227(3) Uani 1.000000 .
C13 C 0.37680(13) -0.11993(10) 0.58755(12) 0.0190(3) Uani 1.000000 .
C8 C 0.04744(15) -0.30328(11) 1.05659(14) 0.0256(3) Uani 1.000000 .
C6 C 0.15054(13) -0.12667(10) 1.03718(11) 0.0173(2) Uani 1.000000 .
C14 C 0.35229(14) -0.08534(11) 0.46962(12) 0.0217(3) Uani 1.000000 .
C15 C 0.32563(14) 0.02798(11) 0.44061(12) 0.0221(3) Uani 1.000000 .
C16 C 0.32478(14) 0.10794(11) 0.52914(12) 0.0202(3) Uani 1.000000 .
C9 C -0.01764(15) -0.29450(11) 0.93976(13) 0.0252(3) Uani 1.000000 .
C2 C 0.24675(13) -0.03635(11) 1.07454(11) 0.0195(3) Uani 1.000000 .
C7 C 0.13169(14) -0.21944(11) 1.10719(13) 0.0228(3) Uani 1.000000 .
H10 H -0.0532(17) -0.1891(13) 0.7817(14) 0.037(4) Uani 1.000000 .
H16 H 0.3059(18) 0.1924(12) 0.5068(14) 0.042(5) Uani 1.000000 .
H15 H 0.3108(17) 0.0516(13) 0.3518(13) 0.039(5) Uani 1.000000 .
H13 H 0.3968(17) -0.2060(12) 0.6123(14) 0.036(4) Uani 1.000000 .
H8 H 0.0335(16) -0.3748(13) 1.1072(15) 0.039(4) Uani 1.000000 .
H9 H -0.0831(18) -0.3606(14) 0.9031(16) 0.049(5) Uani 1.000000 .
H14 H 0.3514(17) -0.1450(13) 0.3992(13) 0.038(5) Uani 1.000000 .
H7 H 0.1830(18) -0.2268(15) 1.1971(15) 0.045(5) Uani 1.000000 .


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 P2 2.1972(5) . ?
P1 C1 1.8650(13) . ?
P1 C2 1.8770(13) . ?
P2 C4 1.8818(12) . ?
P2 C3 1.8838(13) . ?
O1 C1 1.2119(15) . ?
O2 C2 1.2080(16) . ?
C5 C1 1.4823(17) . ?
C5 C10 1.3943(18) . ?
C5 C6 1.3976(17) . ?
O3 C3 1.2084(14) . ?
C11 C12 1.4003(16) . ?
C11 C3 1.4855(17) . ?
C11 C16 1.3924(17) . ?
O4 C4 1.2109(14) . ?
C12 C4 1.4828(17) . ?
C12 C13 1.3947(17) . ?
C10 C9 1.389(2) . ?
C10 H10 1.080(16) . ?
C13 C14 1.3908(19) . ?
C13 H13 1.071(15) . ?
C8 C9 1.396(2) . ?
C8 C7 1.392(2) . ?
C8 H8 1.052(15) . ?
C6 C2 1.4873(18) . ?
C6 C7 1.3960(17) . ?
C14 C15 1.4012(18) . ?
C14 H14 1.071(14) . ?
C15 C16 1.3891(18) . ?
C15 H15 1.039(14) . ?
C16 H16 1.045(14) . ?
C9 H9 1.081(15) . ?
C7 H7 1.080(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 P2 102.01(4) . . ?
C2 P1 P2 100.85(4) . . ?
C2 P1 C1 89.67(6) . . ?
C4 P2 P1 103.45(4) . . ?
C3 P2 P1 96.38(4) . . ?
C3 P2 C4 89.18(5) . . ?
C10 C5 C1 124.62(12) . . ?
C6 C5 C1 114.45(11) . . ?
C6 C5 C10 120.89(12) . . ?
C3 C11 C12 115.05(11) . . ?
C16 C11 C12 120.51(11) . . ?
C16 C11 C3 124.41(11) . . ?
C4 C12 C11 114.45(10) . . ?
C13 C12 C11 120.50(11) . . ?
C13 C12 C4 124.95(11) . . ?
O1 C1 P1 124.53(10) . . ?
C5 C1 P1 110.07(9) . . ?
C5 C1 O1 125.41(12) . . ?
O4 C4 P2 124.98(10) . . ?
C12 C4 P2 109.43(8) . . ?
C12 C4 O4 125.59(11) . . ?
O3 C3 P2 125.30(10) . . ?
C11 C3 P2 109.17(8) . . ?
C11 C3 O3 125.51(12) . . ?
C9 C10 C5 118.25(13) . . ?
H10 C10 C5 118.6(8) . . ?
H10 C10 C9 123.1(8) . . ?
C14 C13 C12 118.85(12) . . ?
H13 C13 C12 119.0(8) . . ?
H13 C13 C14 122.2(8) . . ?
C7 C8 C9 121.13(13) . . ?
H8 C8 C9 119.6(10) . . ?
H8 C8 C7 119.2(10) . . ?
C2 C6 C5 114.90(11) . . ?
C7 C6 C5 120.78(12) . . ?
C7 C6 C2 124.20(12) . . ?
C15 C14 C13 120.56(12) . . ?
H14 C14 C13 120.7(9) . . ?
H14 C14 C15 118.7(9) . . ?
C16 C15 C14 120.59(13) . . ?
H15 C15 C14 118.7(8) . . ?
H15 C15 C16 120.7(8) . . ?
C15 C16 C11 118.97(12) . . ?
H16 C16 C11 120.9(9) . . ?
H16 C16 C15 120.1(9) . . ?
C8 C9 C10 120.86(13) . . ?
H9 C9 C10 119.6(10) . . ?
H9 C9 C8 119.5(10) . . ?
O2 C2 P1 126.01(10) . . ?
C6 C2 P1 109.04(9) . . ?
C6 C2 O2 124.94(12) . . ?
C6 C7 C8 118.03(13) . . ?
H7 C7 C8 121.1(9) . . ?
H7 C7 C6 120.8(9) . . ?

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 C5 C10 175.31(9) . . . . ?
P1 C1 C5 C6 -6.93(10) . . . . ?
P1 C2 C6 C5 11.53(10) . . . . ?
P1 C2 C6 C7 -172.40(9) . . . . ?
P2 C4 C12 C11 -13.07(10) . . . . ?
P2 C4 C12 C13 170.65(9) . . . . ?
P2 C3 C11 C12 9.41(10) . . . . ?
P2 C3 C11 C16 -172.69(9) . . . . ?
O1 C1 C5 C10 -4.09(17) . . . . ?
O1 C1 C5 C6 173.67(14) . . . . ?
O2 C2 C6 C5 -169.78(14) . . . . ?
O2 C2 C6 C7 6.28(17) . . . . ?
C5 C10 C9 C8 2.10(16) . . . . ?
C5 C6 C7 C8 2.17(15) . . . . ?
O3 C3 C11 C12 -172.04(14) . . . . ?
O3 C3 C11 C16 5.87(17) . . . . ?
C11 C12 C4 O4 166.07(12) . . . . ?
C11 C12 C13 C14 -1.44(15) . . . . ?
C11 C16 C15 C14 -1.38(16) . . . . ?
O4 C4 C12 C13 -10.21(17) . . . . ?
C12 C13 C14 C15 0.62(15) . . . . ?
C10 C9 C8 C7 -1.40(17) . . . . ?
C13 C14 C15 C16 0.80(16) . . . . ?
C8 C7 C6 C2 -173.68(12) . . . . ?


_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_exp_1048
_database_code_depnum_ccdc_archive 'CCDC 1894668'
loop_
_audit_author_name
_audit_author_address
'Zhongshu Li'
;Lehn Institute of Functional Materials (LIFM), School of Chemistry, Sun Yat Sen University
China
;
_audit_update_record             
;
2022-06-02 deposited with the CCDC.	2022-06-06 downloaded from the CCDC.
;
_audit_creation_date             2022-06-02
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_chemical_formula_moiety         '4(C26 H19 Ge O2 P), 1[C6H5F]'
_chemical_formula_sum            'C110 H81 F1 Ge4 O8 P4'
_chemical_formula_weight         1964.208
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.01920 0.00962 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.21560 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Ge -1.09680 0.92099 16.08160 6.37470 3.70680 3.68300 2.85090 0.25160 11.44680
54.76250 2.13130 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.00304 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.05239 0.03377 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.25080 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
P 0.30360 0.43703 6.43450 4.17910 1.78000 1.49080 1.90670 27.15700 0.52600
68.16450 1.11490 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_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_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z+1/2
3 -x,-y,-z
4 x,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   17.5402(3)
_cell_length_b                   8.8075(2)
_cell_length_c                   30.5468(6)
_cell_angle_alpha                90
_cell_angle_beta                 100.328(2)
_cell_angle_gamma                90
_cell_volume                     4642.57(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12970
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.9790
_cell_measurement_theta_min      4.2260
_exptl_absorpt_coefficient_mu    2.635
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       block
_exptl_crystal_F_000             2003.029
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.9956
_diffrn_reflns_Laue_measured_fraction_max 0.9734
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            26413
_diffrn_reflns_point_group_measured_fraction_full 0.9956
_diffrn_reflns_point_group_measured_fraction_max 0.9734
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         74.31
_diffrn_reflns_theta_min         3.54
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9956
_diffrn_measured_fraction_theta_max 0.9734
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -65.00  33.00   1.00    2.50    --  -41.20  38.00-120.00   98
  2  ω    -69.00  32.00   1.00    2.50    --  -41.20  57.00 -30.00  101
  3  ω    -74.00  26.00   1.00    2.50    --  -41.20  77.00  90.00  100
  4  ω     56.00 125.00   1.00    6.00    --  107.98 -30.00  60.00   69
  5  ω    144.00 178.00   1.00    6.00    --  107.98  30.00 -90.00   34
  6  ω    147.00 176.00   1.00    6.00    --  107.98  30.00-120.00   29
  7  ω     99.00 173.00   1.00    6.00    --  107.98 125.00-180.00   74
  8  ω     88.00 143.00   1.00    6.00    --  107.98  30.00 -90.00   55
  9  ω     84.00 120.00   1.00    6.00    --  107.98  30.00-120.00   36
 10  ω     32.00 136.00   1.00    6.00    --  107.98 -30.00-120.00  104
 11  ω     35.00 117.00   1.00    6.00    --  107.98-125.00  60.00   82
 12  ω     31.00 110.00   1.00    6.00    --  107.98 -98.00 127.00   79
 13  ω     32.00 140.00   1.00    6.00    --  107.98 -77.00-150.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              21
_reflns_limit_h_min              -21
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              37
_reflns_limit_l_min              0
_reflns_number_gt                8218
_reflns_number_total             9196
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         0.5330
_refine_diff_density_min         -0.5466
_refine_diff_density_rms         0.0707
_refine_ls_d_res_high            0.8007
_refine_ls_d_res_low             12.4956
_refine_ls_goodness_of_fit_ref   1.0431
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    81
_refine_ls_number_parameters     590
_refine_ls_number_reflns         9196
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0419
_refine_ls_restrained_S_all      1.0431
_refine_ls_shift/su_max          0.0013
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0681P)²+2.5336P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1179
_olex2_refinement_description    
;
1. Others
 Sof(C34A)=Sof(H34A)=Sof(C33A)=Sof(H33A)=Sof(C32A)=Sof(H32A)=Sof(C31A)=
 Sof(H31A)=1-FVAR(1)
 Sof(C31)=Sof(H31)=Sof(C34)=Sof(H34)=Sof(C33)=Sof(H33)=Sof(C32)=Sof(H32)=FVAR(1)
2.a Aromatic/amide H refined with riding coordinates:
 C46(H46), C10(H10), C42(H42), C26(H26), C44(H44), C40(H40), C45(H45),
 C18(H18), C24(H24), C22(H22), C43(H43), C16(H16), C25(H25), C20(H20), C17(H17),
  C23(H23), C52(H52), C11(H11), C19(H19), C14(H14), C36(H36), C48(H48),
 C39(H39), C50(H50), C13(H13), C8(H8), C12(H12), C38(H38), C49(H49), C51(H51),
 C7(H7), C6(H6), C37(H37), C31(H31), C5(H5), C34(H34), C33(H33), C32(H32)
;
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_refinement_flags_posn
_atom_site_disorder_group
Ge2 Ge 0.730392(15) 0.29761(3) 0.684046(9) 0.03158(9) Uani 1.000000 . .
Ge1 Ge 0.210564(16) 0.89085(3) 0.592186(9) 0.03350(9) Uani 1.000000 . .
P2 P 0.72578(4) 0.28635(7) 0.76042(2) 0.03563(14) Uani 1.000000 . .
P1 P 0.22391(5) 0.63404(8) 0.61134(2) 0.0540(2) Uani 1.000000 . .
O3 O 0.86089(13) 0.1224(3) 0.77383(8) 0.0649(6) Uani 1.000000 . .
O4 O 0.57264(13) 0.1980(4) 0.74853(9) 0.0753(8) Uani 1.000000 . .
O2 O 0.06749(16) 0.5782(3) 0.58612(10) 0.0774(8) Uani 1.000000 . .
C41 C 0.82655(14) 0.4008(3) 0.67891(9) 0.0354(5) Uani 1.000000 . .
C47 C 0.63909(14) 0.4073(3) 0.65453(10) 0.0418(6) Uani 1.000000 . .
C15 C 0.13216(14) 0.9819(3) 0.62154(7) 0.0348(5) Uani 1.000000 . .
C35 C 0.73030(16) 0.0913(3) 0.66108(9) 0.0388(5) Uani 1.000000 . .
C9 C 0.31105(14) 0.9871(3) 0.61168(8) 0.0393(5) Uani 1.000000 . .
C21 C 0.17913(15) 0.9029(3) 0.52782(8) 0.0353(5) Uani 1.000000 . .
C46 C 0.84594(15) 0.4159(3) 0.63706(9) 0.0402(5) Uani 1.000000 . .
H46 H 0.81290(15) 0.3773(3) 0.61233(9) 0.0482(6) Uiso 1.000000 R .
C10 C 0.37140(15) 0.9179(4) 0.64034(9) 0.0448(6) Uani 1.000000 . .
H10 H 0.36613(15) 0.8187(4) 0.64978(9) 0.0537(7) Uiso 1.000000 R .
C42 C 0.87670(16) 0.4588(4) 0.71527(9) 0.0473(6) Uani 1.000000 . .
H42 H 0.86448(16) 0.4502(4) 0.74356(9) 0.0568(8) Uiso 1.000000 R .
C28 C 0.63955(18) 0.1569(4) 0.75619(9) 0.0491(7) Uani 1.000000 . .
C27 C 0.79090(18) 0.1171(3) 0.76984(8) 0.0441(6) Uani 1.000000 . .
C26 C 0.10092(16) 0.8925(3) 0.50881(9) 0.0415(6) Uani 1.000000 . .
H26 H 0.06385(16) 0.8857(3) 0.52701(9) 0.0497(7) Uiso 1.000000 R .
C44 C 0.96362(15) 0.5436(3) 0.66821(10) 0.0449(6) Uani 1.000000 . .
H44 H 1.00963(15) 0.5904(3) 0.66462(10) 0.0539(7) Uiso 1.000000 R .
C40 C 0.79796(18) 0.0057(3) 0.66699(9) 0.0472(6) Uani 1.000000 . .
H40 H 0.84482(18) 0.0496(3) 0.67992(9) 0.0567(8) Uiso 1.000000 R .
C3 C 0.14819(19) 0.4721(3) 0.53916(9) 0.0481(6) Uani 1.000000 . .
C45 C 0.91385(15) 0.4879(3) 0.63158(9) 0.0440(6) Uani 1.000000 . .
H45 H 0.92586(15) 0.4986(3) 0.60330(9) 0.0527(7) Uiso 1.000000 R .
C18 C 0.02252(16) 1.1272(4) 0.66294(9) 0.0470(6) Uani 1.000000 . .
H18 H -0.01379(16) 1.1755(4) 0.67689(9) 0.0564(8) Uiso 1.000000 R .
C24 C 0.13287(19) 0.9032(4) 0.43598(9) 0.0505(7) Uani 1.000000 . .
H24 H 0.11750(19) 0.9031(4) 0.40522(9) 0.0606(8) Uiso 1.000000 R .
C22 C 0.23363(16) 0.9132(3) 0.50036(9) 0.0439(6) Uani 1.000000 . .
H22 H 0.28602(16) 0.9195(3) 0.51268(9) 0.0527(7) Uiso 1.000000 R .
C43 C 0.94549(17) 0.5301(4) 0.70979(10) 0.0528(7) Uani 1.000000 . .
H43 H 0.97895(17) 0.5685(4) 0.73439(10) 0.0633(9) Uiso 1.000000 R .
C16 C 0.08815(17) 0.9007(3) 0.64693(10) 0.0472(6) Uani 1.000000 . .
H16 H 0.09494(17) 0.7963(3) 0.65025(10) 0.0566(8) Uiso 1.000000 R .
C25 C 0.07807(17) 0.8921(3) 0.46307(9) 0.0483(7) Uani 1.000000 . .
H25 H 0.02581(17) 0.8845(3) 0.45058(9) 0.0580(8) Uiso 1.000000 R .
C20 C 0.11981(17) 1.1369(3) 0.61703(11) 0.0494(7) Uani 1.000000 . .
H20 H 0.14852(17) 1.1933(3) 0.59999(11) 0.0593(8) Uiso 1.000000 R .
C30 C 0.7444(2) -0.0221(3) 0.77198(8) 0.0541(8) Uani 1.000000 . .
C29 C 0.6649(2) -0.0010(4) 0.76519(9) 0.0552(8) Uani 1.000000 . .
C34A C 0.6290(12) -0.1374(16) 0.7685(3) 0.057(3) Uani 0.60(3) . 2
H34A H 0.572(4) -0.122(10) 0.764(3) 0.069(4) Uiso 0.60(3) R 2
C33A C 0.6653(15) -0.2729(13) 0.7773(4) 0.061(5) Uani 0.60(3) . 2
H33A H 0.640(4) -0.378(8) 0.783(2) 0.074(6) Uiso 0.60(3) R 2
C32A C 0.7447(15) -0.2890(10) 0.7837(3) 0.069(5) Uani 0.60(3) . 2
H32A H 0.763(4) -0.384(9) 0.788(2) 0.083(6) Uiso 0.60(3) R 2
C31A C 0.7904(12) -0.1615(11) 0.7808(3) 0.053(3) Uani 0.60(3) . 2
H31A H 0.844(4) -0.152(8) 0.785(2) 0.064(4) Uiso 0.60(3) R 2
O1 O 0.34034(15) 0.6141(4) 0.56101(14) 0.1024(12) Uani 1.000000 . .
C17 C 0.03401(18) 0.9745(4) 0.66741(10) 0.0534(7) Uani 1.000000 . .
H17 H 0.00508(18) 0.9187(4) 0.68447(10) 0.0641(8) Uiso 1.000000 R .
C2 C 0.1314(2) 0.5613(3) 0.57762(9) 0.0501(7) Uani 1.000000 . .
C23 C 0.21028(18) 0.9142(4) 0.45439(9) 0.0510(7) Uani 1.000000 . .
H23 H 0.24705(18) 0.9224(4) 0.43604(9) 0.0612(8) Uiso 1.000000 R .
C4 C 0.2234(2) 0.4820(3) 0.53233(11) 0.0531(7) Uani 1.000000 . .
C52 C 0.59109(17) 0.4851(4) 0.67881(13) 0.0562(8) Uani 1.000000 . .
H52 H 0.60174(17) 0.4820(4) 0.70974(13) 0.0674(9) Uiso 1.000000 R .
C11 C 0.44028(17) 0.9979(5) 0.65501(11) 0.0589(8) Uani 1.000000 . .
H11 H 0.48114(17) 0.9506(5) 0.67362(11) 0.0707(10) Uiso 1.000000 R .
C19 C 0.06554(19) 1.2095(4) 0.63742(12) 0.0553(7) Uani 1.000000 . .
H19 H 0.05799(19) 1.3137(4) 0.63396(12) 0.0663(9) Uiso 1.000000 R .
C14 C 0.32053(17) 1.1361(4) 0.59823(11) 0.0517(7) Uani 1.000000 . .
H14 H 0.28081(17) 1.1833(4) 0.57869(11) 0.0620(8) Uiso 1.000000 R .
C36 C 0.66129(19) 0.0231(4) 0.64101(13) 0.0596(9) Uani 1.000000 . .
H36 H 0.61551(19) 0.0788(4) 0.63651(13) 0.0716(10) Uiso 1.000000 R .
C48 C 0.6220(2) 0.4120(4) 0.60866(11) 0.0606(9) Uani 1.000000 . .
H48 H 0.6528(2) 0.3602(4) 0.59178(11) 0.0727(10) Uiso 1.000000 R .
C39 C 0.7959(2) -0.1452(4) 0.65365(12) 0.0629(9) Uani 1.000000 . .
H39 H 0.8412(2) -0.2023(4) 0.65781(12) 0.0754(11) Uiso 1.000000 R .
C50 C 0.5117(2) 0.5728(5) 0.6128(2) 0.0846(15) Uani 1.000000 . .
H50 H 0.4692(2) 0.6288(5) 0.5989(2) 0.1015(18) Uiso 1.000000 R .
C13 C 0.38852(19) 1.2149(4) 0.61364(13) 0.0625(9) Uani 1.000000 . .
H13 H 0.39396(19) 1.3147(4) 0.60472(13) 0.0750(10) Uiso 1.000000 R .
C8 C 0.0933(2) 0.3845(4) 0.51112(12) 0.0638(9) Uani 1.000000 . .
H8 H 0.0424(2) 0.3786(4) 0.51578(12) 0.0766(11) Uiso 1.000000 R .
C1 C 0.2752(2) 0.5780(4) 0.56473(13) 0.0628(9) Uani 1.000000 . .
C12 C 0.44793(18) 1.1453(5) 0.64216(13) 0.0644(9) Uani 1.000000 . .
H12 H 0.49332(18) 1.1984(5) 0.65272(13) 0.0773(11) Uiso 1.000000 R .
C38 C 0.7268(3) -0.2103(4) 0.63431(15) 0.0763(12) Uani 1.000000 . .
H38 H 0.7255(3) -0.3117(4) 0.62569(15) 0.0915(15) Uiso 1.000000 R .
C49 C 0.5571(3) 0.4969(5) 0.58762(15) 0.0846(15) Uani 1.000000 . .
H49 H 0.5451(3) 0.5013(5) 0.55673(15) 0.1016(17) Uiso 1.000000 R .
C51 C 0.5283(2) 0.5665(4) 0.65749(18) 0.0773(12) Uani 1.000000 . .
H51 H 0.4969(2) 0.6176(4) 0.67418(18) 0.0928(15) Uiso 1.000000 R .
C7 C 0.1161(3) 0.3080(4) 0.47675(12) 0.0736(11) Uani 1.000000 . .
H7 H 0.0803(3) 0.2487(4) 0.45800(12) 0.0883(13) Uiso 1.000000 R .
C6 C 0.1907(3) 0.3172(4) 0.46946(13) 0.0786(12) Uani 1.000000 . .
H6 H 0.2048(3) 0.2637(4) 0.44587(13) 0.0943(14) Uiso 1.000000 R .
C37 C 0.6604(2) -0.1272(4) 0.62770(17) 0.0817(14) Uani 1.000000 . .
H37 H 0.6141(2) -0.1716(4) 0.61415(17) 0.0981(16) Uiso 1.000000 R .
C31 C 0.7562(12) -0.1718(19) 0.7790(5) 0.051(3) Uani 0.40(3) . 1
H31 H 0.8076(12) -0.2038(19) 0.7843(5) 0.061(4) Uiso 0.40(3) R 1
C5 C 0.2456(3) 0.4043(4) 0.49648(14) 0.0738(10) Uani 1.000000 . .
H5 H 0.2960(3) 0.4113(4) 0.49104(14) 0.0886(13) Uiso 1.000000 R .
C34 C 0.5974(11) -0.1034(19) 0.7642(5) 0.043(3) Uani 0.40(3) . 1
H34 H 0.5459(11) -0.0725(19) 0.7600(5) 0.052(4) Uiso 0.40(3) R 1
C33 C 0.6224(15) -0.250(2) 0.7704(6) 0.051(4) Uani 0.40(3) . 1
H33 H 0.5866(15) -0.329(2) 0.7688(6) 0.061(5) Uiso 0.40(3) R 1
C32 C 0.7017(14) -0.282(3) 0.7792(8) 0.057(5) Uani 0.40(3) . 1
H32 H 0.7179(14) -0.382(3) 0.7854(8) 0.068(6) Uiso 0.40(3) R 1


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
Ge2 P2 2.3509(7) . ?
Ge2 C41 1.947(2) . ?
Ge2 C47 1.947(3) . ?
Ge2 C35 1.947(2) . ?
Ge1 P1 2.3376(8) . ?
Ge1 C15 1.944(3) . ?
Ge1 C9 1.950(2) . ?
Ge1 C21 1.947(2) . ?
P2 C28 1.880(3) . ?
P2 C27 1.869(3) . ?
P1 C2 1.872(3) . ?
P1 C1 1.882(4) . ?
O3 C27 1.213(4) . ?
O4 C28 1.210(4) . ?
O2 C2 1.205(4) . ?
C41 C46 1.387(4) . ?
C41 C42 1.385(4) . ?
C47 C52 1.398(4) . ?
C47 C48 1.380(4) . ?
C15 C16 1.387(4) . ?
C15 C20 1.385(4) . ?
C35 C40 1.391(4) . ?
C35 C36 1.391(4) . ?
C9 C10 1.388(4) . ?
C9 C14 1.395(4) . ?
C21 C26 1.393(4) . ?
C21 C22 1.383(4) . ?
C46 H46 0.9300 . ?
C46 C45 1.386(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.401(4) . ?
C42 H42 0.9300 . ?
C42 C43 1.397(4) . ?
C28 C29 1.471(5) . ?
C27 C30 1.480(4) . ?
C26 H26 0.9300 . ?
C26 C25 1.383(4) . ?
C44 H44 0.9300 . ?
C44 C45 1.380(4) . ?
C44 C43 1.369(4) . ?
C40 H40 0.9300 . ?
C40 C39 1.389(4) . ?
C3 C2 1.486(4) . ?
C3 C4 1.375(5) . ?
C3 C8 1.400(4) . ?
C45 H45 0.9300 . ?
C18 H18 0.9300 . ?
C18 C17 1.364(4) . ?
C18 C19 1.383(4) . ?
C24 H24 0.9300 . ?
C24 C25 1.380(4) . ?
C24 C23 1.377(4) . ?
C22 H22 0.9300 . ?
C22 C23 1.391(4) . ?
C43 H43 0.9300 . ?
C16 H16 0.9300 . ?
C16 C17 1.389(4) . ?
C25 H25 0.9300 . ?
C20 H20 0.9300 . ?
C20 C19 1.384(4) . ?
C30 C29 1.384(5) . ?
C30 C31A 1.467(12) . ?
C30 C31 1.346(17) . ?
C29 C34A 1.369(10) . ?
C29 C34 1.486(15) . ?
C34A H34A 0.99(8) . ?
C34A C33A 1.357(15) . ?
C33A H33A 1.06(7) . ?
C33A C32A 1.380(15) . ?
C32A H32A 0.90(8) . ?
C32A C31A 1.391(15) . ?
C31A H31A 0.92(7) . ?
O1 C1 1.210(5) . ?
C17 H17 0.9300 . ?
C23 H23 0.9300 . ?
C4 C1 1.483(5) . ?
C4 C5 1.404(5) . ?
C52 H52 0.9300 . ?
C52 C51 1.376(5) . ?
C11 H11 0.9300 . ?
C11 C12 1.369(6) . ?
C19 H19 0.9300 . ?
C14 H14 0.9300 . ?
C14 C13 1.387(4) . ?
C36 H36 0.9300 . ?
C36 C37 1.384(5) . ?
C48 H48 0.9300 . ?
C48 C49 1.417(5) . ?
C39 H39 0.9300 . ?
C39 C38 1.374(6) . ?
C50 H50 0.9300 . ?
C50 C49 1.376(7) . ?
C50 C51 1.345(7) . ?
C13 H13 0.9300 . ?
C13 C12 1.377(5) . ?
C8 H8 0.9300 . ?
C8 C7 1.366(5) . ?
C12 H12 0.9300 . ?
C38 H38 0.9300 . ?
C38 C37 1.360(6) . ?
C49 H49 0.9300 . ?
C51 H51 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.370(6) . ?
C6 H6 0.9300 . ?
C6 C5 1.383(6) . ?
C37 H37 0.9300 . ?
C31 H31 0.9300 . ?
C31 C32 1.36(2) . ?
C5 H5 0.9300 . ?
C34 H34 0.9300 . ?
C34 C33 1.37(2) . ?
C33 H33 0.9300 . ?
C33 C32 1.397(17) . ?
C32 H32 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C41 Ge2 P2 106.50(8) . . ?
C47 Ge2 P2 107.98(9) . . ?
C47 Ge2 C41 112.56(10) . . ?
C35 Ge2 P2 108.67(8) . . ?
C35 Ge2 C41 110.56(10) . . ?
C35 Ge2 C47 110.39(12) . . ?
C15 Ge1 P1 109.34(8) . . ?
C9 Ge1 P1 107.43(9) . . ?
C9 Ge1 C15 110.80(10) . . ?
C21 Ge1 P1 107.64(8) . . ?
C21 Ge1 C15 110.33(10) . . ?
C21 Ge1 C9 111.19(11) . . ?
C28 P2 Ge2 97.34(9) . . ?
C27 P2 Ge2 93.31(9) . . ?
C27 P2 C28 89.35(15) . . ?
C2 P1 Ge1 98.93(10) . . ?
C1 P1 Ge1 96.00(11) . . ?
C1 P1 C2 88.79(15) . . ?
C46 C41 Ge2 118.57(19) . . ?
C42 C41 Ge2 122.86(19) . . ?
C42 C41 C46 118.6(2) . . ?
C52 C47 Ge2 121.4(2) . . ?
C48 C47 Ge2 119.7(3) . . ?
C48 C47 C52 118.8(3) . . ?
C16 C15 Ge1 123.7(2) . . ?
C20 C15 Ge1 118.14(19) . . ?
C20 C15 C16 118.1(3) . . ?
C40 C35 Ge2 120.9(2) . . ?
C36 C35 Ge2 120.4(2) . . ?
C36 C35 C40 118.5(3) . . ?
C10 C9 Ge1 123.2(2) . . ?
C14 C9 Ge1 117.9(2) . . ?
C14 C9 C10 118.8(3) . . ?
C26 C21 Ge1 119.77(19) . . ?
C22 C21 Ge1 120.96(19) . . ?
C22 C21 C26 119.2(2) . . ?
H46 C46 C41 119.56(15) . . ?
C45 C46 C41 120.9(2) . . ?
C45 C46 H46 119.56(16) . . ?
H10 C10 C9 120.09(17) . . ?
C11 C10 C9 119.8(3) . . ?
C11 C10 H10 120.1(2) . . ?
H42 C42 C41 119.73(15) . . ?
C43 C42 C41 120.5(3) . . ?
C43 C42 H42 119.73(17) . . ?
O4 C28 P2 124.9(3) . . ?
C29 C28 P2 110.3(2) . . ?
C29 C28 O4 124.7(3) . . ?
O3 C27 P2 124.3(2) . . ?
C30 C27 P2 109.9(2) . . ?
C30 C27 O3 125.7(3) . . ?
H26 C26 C21 119.78(15) . . ?
C25 C26 C21 120.4(3) . . ?
C25 C26 H26 119.78(17) . . ?
C45 C44 H44 119.90(15) . . ?
C43 C44 H44 119.90(16) . . ?
C43 C44 C45 120.2(2) . . ?
H40 C40 C35 119.87(16) . . ?
C39 C40 C35 120.3(3) . . ?
C39 C40 H40 119.9(2) . . ?
C4 C3 C2 114.7(3) . . ?
C8 C3 C2 124.2(3) . . ?
C8 C3 C4 121.1(3) . . ?
C44 C45 C46 119.8(2) . . ?
H45 C45 C46 120.08(16) . . ?
H45 C45 C44 120.08(15) . . ?
C17 C18 H18 120.41(17) . . ?
C19 C18 H18 120.41(18) . . ?
C19 C18 C17 119.2(3) . . ?
C25 C24 H24 119.93(16) . . ?
C23 C24 H24 119.93(17) . . ?
C23 C24 C25 120.1(3) . . ?
H22 C22 C21 119.92(15) . . ?
C23 C22 C21 120.2(3) . . ?
C23 C22 H22 119.92(17) . . ?
C44 C43 C42 120.0(3) . . ?
H43 C43 C42 120.01(17) . . ?
H43 C43 C44 120.01(16) . . ?
H16 C16 C15 119.85(17) . . ?
C17 C16 C15 120.3(3) . . ?
C17 C16 H16 119.85(17) . . ?
C24 C25 C26 119.9(3) . . ?
H25 C25 C26 120.03(17) . . ?
H25 C25 C24 120.03(16) . . ?
H20 C20 C15 119.39(16) . . ?
C19 C20 C15 121.2(3) . . ?
C19 C20 H20 119.39(18) . . ?
C29 C30 C27 115.5(3) . . ?
C31A C30 C27 114.3(8) . . ?
C31A C30 C29 130.2(8) . . ?
C31 C30 C27 138.4(9) . . ?
C31 C30 C29 106.1(9) . . ?
C31 C30 C31A 24.1(5) . . ?
C30 C29 C28 114.7(3) . . ?
C34A C29 C28 135.7(10) . . ?
C34A C29 C30 109.6(10) . . ?
C34 C29 C28 110.9(8) . . ?
C34 C29 C30 134.4(8) . . ?
C34 C29 C34A 24.8(5) . . ?
H34A C34A C29 110(5) . . ?
C33A C34A C29 125.6(11) . . ?
C33A C34A H34A 125(5) . . ?
H33A C33A C34A 127(4) . . ?
C32A C33A C34A 123.0(11) . . ?
C32A C33A H33A 109(4) . . ?
H32A C32A C33A 116(5) . . ?
C31A C32A C33A 119.1(10) . . ?
C31A C32A H32A 124(5) . . ?
C32A C31A C30 112.5(9) . . ?
H31A C31A C30 117(4) . . ?
H31A C31A C32A 130(4) . . ?
C16 C17 C18 121.2(3) . . ?
H17 C17 C18 119.42(17) . . ?
H17 C17 C16 119.42(17) . . ?
O2 C2 P1 126.0(2) . . ?
C3 C2 P1 109.9(2) . . ?
C3 C2 O2 124.0(3) . . ?
C22 C23 C24 120.2(3) . . ?
H23 C23 C24 119.92(17) . . ?
H23 C23 C22 119.92(17) . . ?
C1 C4 C3 115.2(3) . . ?
C5 C4 C3 119.7(3) . . ?
C5 C4 C1 125.1(4) . . ?
H52 C52 C47 119.61(18) . . ?
C51 C52 C47 120.8(4) . . ?
C51 C52 H52 119.6(3) . . ?
H11 C11 C10 119.7(2) . . ?
C12 C11 C10 120.6(3) . . ?
C12 C11 H11 119.72(19) . . ?
C20 C19 C18 120.0(3) . . ?
H19 C19 C18 119.99(18) . . ?
H19 C19 C20 119.99(18) . . ?
H14 C14 C9 119.62(16) . . ?
C13 C14 C9 120.8(3) . . ?
C13 C14 H14 119.6(2) . . ?
H36 C36 C35 119.82(17) . . ?
C37 C36 C35 120.4(3) . . ?
C37 C36 H36 119.8(2) . . ?
H48 C48 C47 120.4(2) . . ?
C49 C48 C47 119.2(4) . . ?
C49 C48 H48 120.4(3) . . ?
H39 C39 C40 120.0(2) . . ?
C38 C39 C40 120.0(3) . . ?
C38 C39 H39 120.0(2) . . ?
C49 C50 H50 119.8(2) . . ?
C51 C50 H50 119.8(3) . . ?
C51 C50 C49 120.4(4) . . ?
H13 C13 C14 120.0(2) . . ?
C12 C13 C14 119.9(3) . . ?
C12 C13 H13 120.0(2) . . ?
H8 C8 C3 120.7(2) . . ?
C7 C8 C3 118.5(4) . . ?
C7 C8 H8 120.7(3) . . ?
O1 C1 P1 126.1(3) . . ?
C4 C1 P1 109.6(3) . . ?
C4 C1 O1 124.3(4) . . ?
C13 C12 C11 120.1(3) . . ?
H12 C12 C11 119.95(19) . . ?
H12 C12 C13 120.0(2) . . ?
H38 C38 C39 119.8(2) . . ?
C37 C38 C39 120.3(3) . . ?
C37 C38 H38 119.8(2) . . ?
C50 C49 C48 120.1(4) . . ?
H49 C49 C48 119.9(3) . . ?
H49 C49 C50 119.9(2) . . ?
C50 C51 C52 120.7(4) . . ?
H51 C51 C52 119.6(3) . . ?
H51 C51 C50 119.6(3) . . ?
H7 C7 C8 119.5(3) . . ?
C6 C7 C8 121.1(4) . . ?
C6 C7 H7 119.5(2) . . ?
H6 C6 C7 119.4(2) . . ?
C5 C6 C7 121.3(4) . . ?
C5 C6 H6 119.4(3) . . ?
C38 C37 C36 120.5(4) . . ?
H37 C37 C36 119.8(2) . . ?
H37 C37 C38 119.8(2) . . ?
H31 C31 C30 116.2(9) . . ?
C32 C31 C30 127.6(12) . . ?
C32 C31 H31 116.2(9) . . ?
C6 C5 C4 118.4(4) . . ?
H5 C5 C4 120.8(2) . . ?
H5 C5 C6 120.8(3) . . ?
H34 C34 C29 125.1(8) . . ?
C33 C34 C29 109.7(9) . . ?
C33 C34 H34 125.1(8) . . ?
H33 C33 C34 120.0(8) . . ?
C32 C33 C34 119.9(19) . . ?
C32 C33 H33 120.0(15) . . ?
C33 C32 C31 122(2) . . ?
H32 C32 C31 119.0(9) . . ?
H32 C32 C33 119.0(15) . . ?

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
Ge2 C41 C46 C45 -179.7(2) . . . . ?
Ge2 C41 C42 C43 179.2(3) . . . . ?
Ge2 C47 C52 C51 177.8(3) . . . . ?
Ge2 C47 C48 C49 -177.7(2) . . . . ?
Ge2 C35 C40 C39 174.8(2) . . . . ?
Ge2 C35 C36 C37 -175.1(3) . . . . ?
Ge1 C15 C16 C17 179.0(2) . . . . ?
Ge1 C15 C20 C19 -179.3(2) . . . . ?
Ge1 C9 C10 C11 -176.1(2) . . . . ?
Ge1 C9 C14 C13 175.1(3) . . . . ?
Ge1 C21 C26 C25 -176.3(2) . . . . ?
Ge1 C21 C22 C23 176.8(2) . . . . ?
P2 C28 C29 C30 -3.6(2) . . . . ?
P2 C28 C29 C34A 176.8(5) . . . . ?
P2 C28 C29 C34 177.1(6) . . . . ?
P2 C27 C30 C29 2.3(2) . . . . ?
P2 C27 C30 C31A -178.1(4) . . . . ?
P2 C27 C30 C31 -177.6(11) . . . . ?
P1 C2 C3 C4 -10.0(2) . . . . ?
P1 C2 C3 C8 170.5(2) . . . . ?
P1 C1 C4 C3 8.6(3) . . . . ?
P1 C1 C4 C5 -171.6(2) . . . . ?
O3 C27 C30 C29 -178.2(3) . . . . ?
O3 C27 C30 C31A 1.4(5) . . . . ?
O3 C27 C30 C31 2.0(11) . . . . ?
O4 C28 C29 C30 178.5(3) . . . . ?
O4 C28 C29 C34A -1.1(6) . . . . ?
O4 C28 C29 C34 -0.8(6) . . . . ?
O2 C2 C3 C4 172.6(3) . . . . ?
O2 C2 C3 C8 -6.9(4) . . . . ?
C41 C46 C45 C44 0.9(3) . . . . ?
C41 C42 C43 C44 0.2(4) . . . . ?
C47 C52 C51 C50 -0.0(4) . . . . ?
C47 C48 C49 C50 -0.2(4) . . . . ?
C15 C16 C17 C18 0.3(3) . . . . ?
C15 C20 C19 C18 0.1(4) . . . . ?
C35 C40 C39 C38 0.4(4) . . . . ?
C35 C36 C37 C38 0.4(4) . . . . ?
C9 C10 C11 C12 1.6(3) . . . . ?
C9 C14 C13 C12 0.7(4) . . . . ?
C21 C26 C25 C24 -0.4(3) . . . . ?
C21 C22 C23 C24 -0.8(3) . . . . ?
C46 C45 C44 C43 -1.0(3) . . . . ?
C10 C11 C12 C13 -1.8(4) . . . . ?
C42 C43 C44 C45 0.5(4) . . . . ?
C28 C29 C30 C27 0.9(3) . . . . ?
C28 C29 C30 C31A -178.6(5) . . . . ?
C28 C29 C30 C31 -179.2(8) . . . . ?
C28 C29 C34A C33A 180.0(8) . . . . ?
C28 C29 C34 C33 176.9(9) . . . . ?
C27 C30 C29 C34A -179.4(4) . . . . ?
C27 C30 C29 C34 179.9(7) . . . . ?
C27 C30 C31A C32A 178.4(5) . . . . ?
C27 C30 C31 C32 -179.8(17) . . . . ?
C26 C25 C24 C23 0.1(4) . . . . ?
C40 C39 C38 C37 0.7(4) . . . . ?
C3 C4 C1 O1 -171.0(3) . . . . ?
C3 C4 C5 C6 -1.2(4) . . . . ?
C3 C8 C7 C6 -0.5(4) . . . . ?
C30 C29 C34A C33A 0.4(6) . . . . ?
C30 C29 C34 C33 -2.1(8) . . . . ?
C30 C31A C32A C33A 1.7(9) . . . . ?
C30 C31 C32 C33 2(2) . . . . ?
C29 C34A C33A C32A -0.6(10) . . . . ?
C29 C34 C33 C32 4.1(16) . . . . ?
C34A C33A C32A C31A -0.6(12) . . . . ?
O1 C1 C4 C5 8.8(5) . . . . ?
C4 C5 C6 C7 1.0(4) . . . . ?
C52 C51 C50 C49 0.5(4) . . . . ?
C11 C12 C13 C14 0.6(4) . . . . ?
C36 C37 C38 C39 -1.0(5) . . . . ?
C48 C49 C50 C51 -0.3(4) . . . . ?
C8 C7 C6 C5 -0.2(5) . . . . ?
C31 C32 C33 C34 -4(3) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 104 electrons were 
found in a volume of 426Å³ in 1 void per unit cell. 
This is consistent with the presence of 1[C6H5F] per Formula Unit 
which account for 100 electrons per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 -0.147 0.500 213.2 51.8 '1 C6H5F'
2 0.500 0.213 0.000 213.2 51.8 '1 C6H5F'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
