# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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. 
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data_AJ0030
_database_code_depnum_ccdc_archive 'CCDC 1843001'
_audit_update_record             
;
2018-07-30 deposited with the CCDC.
2018-09-26 downloaded from the CCDC.
;
#Start Validation Reply Form
_vrf_PLAT417_AJ0030              
;
PROBLEM: Short Inter D-H..H-D H5O ..H6O 1.84 Ang.
RESPONSE: There are various hydrogen bonding interactions
possible in the structure. Water hydrogen atoms were located 
and then refined with constraints (DFIX O-H and H-H, and Uiso
as dependent on the parent oxygen atom).
As one hydrogen atom engages in strong hydrogen bonding the second 
is forced into a less beneficial position including H,H proximity.
;
_vrf_PLAT420_AJ0030              
;
PROBLEM: D-H Without Acceptor O5 --H5P Please Check
RESPONSE: There are various hydrogen bonding interactions
possible in the structure. Water hydrogen atoms were located 
and then refined with constraints (DFIX O-H and H-H, and Uiso
as dependent on the parent oxygen atom).
As one hydrogen atom engages in strong hydrogen bonding the second 
is forced into a less beneficial position including having no hydrogen 
bonding acceptor in suitable position nearby.
;
_vrf_DIFMX02_AJ0030              
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75
RESPONSE: The highest peak resides 0.14 Ang. from water hydrogen 
atom H6O. Due to various potential hydrogen bonding interactions
it may represent a minor occupancy orientation of a water 
hydrogen atom on a slightly shifted oxygen atom. 
A fully missed atom site can be excluded.
;
_vrf_PLAT355_AJ0030              
;
PROBLEM: Long O-H (X0.82,N0.98A) O6 - H6O . 1.15 Ang.
RESPONSE: The water hydrogen atom is pulled by strong hydrogen bonding
interaction towards the adjacent water oxygen atom.
;
_vrf_PLAT094_AJ0030              
;
PROBLEM: Ratio of Maximum / Minimum Residual Density .... 3.11 Report
RESPONSE: See response to DIFMX02.
;
_vrf_PLAT097_AJ0030              
;
PROBLEM: Large Reported Max. (Positive) Residual Density 1.34 eA-3
RESPONSE: See response to DIFMX02.
;
_vrf_PLAT220_AJ0030              
;
PROBLEM: Non-Solvent Resd 1 C Ueq(max)/Ueq(min) Range 3.6 Ratio
RESPONSE: This is not unusual for compounds bearing rigid phenyl 
carbon atoms and flexible/rotatable iso-propyl substituents.
;
_vrf_PLAT601_AJ0030              
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of . 58 Ang**3
RESPONSE: No sufficient electron density was observed within the void
to assign atom positions.
;
_vrf_PLAT906_AJ0030              
;
PROBLEM: Large K Value in the Analysis of Variance ...... 2.573 Check
RESPONSE: The K value is large only for weak reflections with Fc/Fcmax 
lower than 0.008.
;
# end Validation Reply Form
_audit_creation_date             2018-07-24
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C70 H63 O4 P, 2(H2 O)'
_chemical_formula_sum            'C70 H67 O6 P'
_chemical_formula_weight         1035.20
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/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                   10.6501(3)
_cell_length_b                   37.3357(7)
_cell_length_c                   14.6867(3)
_cell_angle_alpha                90
_cell_angle_beta                 97.195(2)
_cell_angle_gamma                90
_cell_volume                     5793.9(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    26641
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.6710
_cell_measurement_theta_min      2.7410
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.372
_exptl_crystal_size_mid          0.323
_exptl_crystal_size_min          0.204
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            61616
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.500
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         2.519
_diffrn_ambient_temperature      120.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9728
_reflns_number_total             11997
_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 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.340
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         11997
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0458
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0506P)²+2.7644P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1177
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O5-H5A = O5-H5B = O6-H6A = O6-H6B
 0.96 with sigma of 0.02
 H5A-H5B = H6A-H6B
 1.52 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C42(H42), C43(H43), C44(H44)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21), C25(H25), C26(H26), C27(H27), C28(H28),
  C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C38(H38),
 C40(H40), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53),
  C54(H54), C55(H55), C56(H56), C60(H60), C61(H61), C62(H62), C63(H63),
 C64(H64), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70)
3.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C57(H57A,H57B,H57C), C58(H58A,H58B,
 H58C)
3.d Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_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
P1 P 0.69533(4) 0.59962(2) 0.68474(3) 0.01649(10) Uani 1 1 d . . . . .
O1 O 0.59619(10) 0.58926(3) 0.75159(7) 0.0161(2) Uani 1 1 d . . . . .
O2 O 0.65267(10) 0.63969(3) 0.66823(7) 0.0177(2) Uani 1 1 d . . . . .
O3 O 0.82694(10) 0.60139(3) 0.74282(8) 0.0237(2) Uani 1 1 d . . . . .
H3 H 0.874407 0.585693 0.724502 0.035 Uiso 1 1 calc GR . . . .
O4 O 0.68856(10) 0.57696(3) 0.60271(7) 0.0217(2) Uani 1 1 d . . . . .
C1 C 0.53148(14) 0.55635(4) 0.75036(10) 0.0144(3) Uani 1 1 d . . . . .
C2 C 0.57526(14) 0.53102(4) 0.81641(10) 0.0147(3) Uani 1 1 d . . . . .
C3 C 0.50276(14) 0.50024(4) 0.82157(10) 0.0158(3) Uani 1 1 d . . . . .
H3A H 0.531085 0.482339 0.865352 0.019 Uiso 1 1 calc R . . . .
C4 C 0.38945(14) 0.49495(4) 0.76413(10) 0.0160(3) Uani 1 1 d . . . . .
C5 C 0.35248(14) 0.52062(4) 0.69754(10) 0.0168(3) Uani 1 1 d . . . . .
H5 H 0.277378 0.516804 0.656508 0.020 Uiso 1 1 calc R . . . .
C6 C 0.42250(14) 0.55188(4) 0.68911(10) 0.0150(3) Uani 1 1 d . . . . .
C7 C 0.69505(14) 0.53938(4) 0.88138(10) 0.0160(3) Uani 1 1 d . . . . .
H7 H 0.756938 0.549627 0.842558 0.019 Uiso 1 1 calc R . . . .
C8 C 0.31284(15) 0.46102(4) 0.77280(11) 0.0202(3) Uani 1 1 d . . . . .
H8 H 0.332000 0.452368 0.837483 0.024 Uiso 1 1 calc R . . . .
C9 C 0.37851(14) 0.58012(4) 0.61763(10) 0.0166(3) Uani 1 1 d . . . . .
H9 H 0.456027 0.593428 0.605158 0.020 Uiso 1 1 calc R . . . .
C10 C 0.67098(15) 0.56855(4) 0.95007(10) 0.0180(3) Uani 1 1 d . . . . .
C11 C 0.55389(15) 0.57313(4) 0.98097(11) 0.0218(3) Uani 1 1 d . . . . .
H11 H 0.485090 0.558122 0.958005 0.026 Uiso 1 1 calc R . . . .
C12 C 0.53647(17) 0.59946(5) 1.04520(12) 0.0277(4) Uani 1 1 d . . . . .
H12 H 0.456155 0.602200 1.066144 0.033 Uiso 1 1 calc R . . . .
C13 C 0.63521(18) 0.62162(4) 1.07864(12) 0.0295(4) Uani 1 1 d . . . . .
H13 H 0.623236 0.639554 1.122615 0.035 Uiso 1 1 calc R . . . .
C14 C 0.75184(18) 0.61754(4) 1.04767(12) 0.0299(4) Uani 1 1 d . . . . .
H14 H 0.820118 0.632779 1.070287 0.036 Uiso 1 1 calc R . . . .
C15 C 0.76933(16) 0.59133(4) 0.98388(11) 0.0239(3) Uani 1 1 d . . . . .
H15 H 0.849673 0.588842 0.962840 0.029 Uiso 1 1 calc R . . . .
C16 C 0.75845(14) 0.50660(4) 0.92858(10) 0.0173(3) Uani 1 1 d . . . . .
C17 C 0.71711(15) 0.49171(4) 1.00636(11) 0.0222(3) Uani 1 1 d . . . . .
H17 H 0.647764 0.502257 1.031315 0.027 Uiso 1 1 calc R . . . .
C18 C 0.77548(16) 0.46178(5) 1.04791(12) 0.0290(4) Uani 1 1 d . . . . .
H18 H 0.745701 0.451847 1.100779 0.035 Uiso 1 1 calc R . . . .
C19 C 0.87700(17) 0.44625(5) 1.01278(13) 0.0340(4) Uani 1 1 d . . . . .
H19 H 0.916393 0.425505 1.040818 0.041 Uiso 1 1 calc R . . . .
C20 C 0.92085(18) 0.46117(5) 0.93640(13) 0.0342(4) Uani 1 1 d . . . . .
H20 H 0.991225 0.450812 0.912342 0.041 Uiso 1 1 calc R . . . .
C21 C 0.86232(15) 0.49117(5) 0.89505(11) 0.0242(4) Uani 1 1 d . . . . .
H21 H 0.893526 0.501350 0.843021 0.029 Uiso 1 1 calc R . . . .
C22 C 0.35545(19) 0.43195(4) 0.71026(13) 0.0315(4) Uani 1 1 d . . . . .
H22A H 0.338710 0.439773 0.646199 0.047 Uiso 1 1 calc GR . . . .
H22B H 0.308685 0.409801 0.718313 0.047 Uiso 1 1 calc GR . . . .
H22C H 0.446306 0.427604 0.726144 0.047 Uiso 1 1 calc GR . . . .
C23 C 0.17020(16) 0.46674(5) 0.75361(14) 0.0320(4) Uani 1 1 d . . . . .
H23A H 0.144941 0.485856 0.793271 0.048 Uiso 1 1 calc GR . . . .
H23B H 0.126419 0.444519 0.766042 0.048 Uiso 1 1 calc GR . . . .
H23C H 0.147583 0.473516 0.689177 0.048 Uiso 1 1 calc GR . . . .
C24 C 0.32446(15) 0.56271(4) 0.52693(10) 0.0187(3) Uani 1 1 d . . . . .
C25 C 0.40648(16) 0.54361(4) 0.47824(11) 0.0236(3) Uani 1 1 d . . . . .
H25 H 0.492828 0.541171 0.503010 0.028 Uiso 1 1 calc R . . . .
C26 C 0.36438(19) 0.52815(5) 0.39464(12) 0.0325(4) Uani 1 1 d . . . . .
H26 H 0.421476 0.515048 0.362582 0.039 Uiso 1 1 calc R . . . .
C27 C 0.2398(2) 0.53170(6) 0.35767(14) 0.0447(5) Uani 1 1 d . . . . .
H27 H 0.211242 0.521596 0.299391 0.054 Uiso 1 1 calc R . . . .
C28 C 0.1566(2) 0.54998(6) 0.40547(15) 0.0503(6) Uani 1 1 d . . . . .
H28 H 0.070174 0.552060 0.380533 0.060 Uiso 1 1 calc R . . . .
C29 C 0.19870(17) 0.56545(5) 0.49039(13) 0.0331(4) Uani 1 1 d . . . . .
H29 H 0.140774 0.577894 0.523159 0.040 Uiso 1 1 calc R . . . .
C30 C 0.29051(15) 0.60774(4) 0.65205(10) 0.0193(3) Uani 1 1 d . . . . .
C31 C 0.2719(2) 0.63996(5) 0.60600(13) 0.0450(6) Uani 1 1 d . . . . .
H31 H 0.319510 0.645199 0.557083 0.054 Uiso 1 1 calc R . . . .
C32 C 0.1850(3) 0.66474(6) 0.62999(15) 0.0522(6) Uani 1 1 d . . . . .
H32 H 0.171837 0.686399 0.596189 0.063 Uiso 1 1 calc R . . . .
C33 C 0.11793(19) 0.65831(5) 0.70203(14) 0.0366(4) Uani 1 1 d . . . . .
H33 H 0.057844 0.675231 0.718140 0.044 Uiso 1 1 calc R . . . .
C34 C 0.1388(2) 0.62726(5) 0.75013(16) 0.0435(5) Uani 1 1 d . . . . .
H34 H 0.093843 0.622688 0.800833 0.052 Uiso 1 1 calc R . . . .
C35 C 0.22541(18) 0.60211(5) 0.72590(14) 0.0346(4) Uani 1 1 d . . . . .
H35 H 0.239655 0.580765 0.760903 0.042 Uiso 1 1 calc R . . . .
C36 C 0.73298(14) 0.66913(4) 0.65783(10) 0.0172(3) Uani 1 1 d . . . . .
C37 C 0.76462(15) 0.67663(4) 0.57086(10) 0.0185(3) Uani 1 1 d . . . . .
C38 C 0.83681(15) 0.70712(4) 0.56159(11) 0.0208(3) Uani 1 1 d . . . . .
H38 H 0.860923 0.712727 0.503113 0.025 Uiso 1 1 calc R . . . .
C39 C 0.87484(15) 0.72968(4) 0.63526(11) 0.0210(3) Uani 1 1 d . . . . .
C40 C 0.83959(15) 0.72100(4) 0.72083(11) 0.0205(3) Uani 1 1 d . . . . .
H40 H 0.865057 0.736255 0.771558 0.025 Uiso 1 1 calc R . . . .
C41 C 0.76809(14) 0.69060(4) 0.73422(10) 0.0180(3) Uani 1 1 d . . . . .
C42 C 0.71693(15) 0.65279(4) 0.48949(10) 0.0190(3) Uani 1 1 d . . . . .
H42 H 0.717686 0.627750 0.513718 0.023 Uiso 1 1 calc R . . . .
C43 C 0.95207(16) 0.76304(4) 0.62066(11) 0.0253(4) Uani 1 1 d . . . . .
H43 H 0.975642 0.761856 0.556923 0.030 Uiso 1 1 calc R . . . .
C44 C 0.72423(15) 0.68115(4) 0.82644(10) 0.0190(3) Uani 1 1 d . . . . .
H44 H 0.720320 0.654402 0.828561 0.023 Uiso 1 1 calc R . . . .
C45 C 0.58003(15) 0.66102(4) 0.45277(10) 0.0200(3) Uani 1 1 d . . . . .
C46 C 0.50340(16) 0.63324(4) 0.41502(11) 0.0246(4) Uani 1 1 d . . . . .
H46 H 0.536024 0.609536 0.416426 0.030 Uiso 1 1 calc R . . . .
C47 C 0.38051(17) 0.63953(5) 0.37545(12) 0.0316(4) Uani 1 1 d . . . . .
H47 H 0.329915 0.620310 0.349103 0.038 Uiso 1 1 calc R . . . .
C48 C 0.33146(18) 0.67390(5) 0.37435(12) 0.0339(4) Uani 1 1 d . . . . .
H48 H 0.247398 0.678448 0.346893 0.041 Uiso 1 1 calc R . . . .
C49 C 0.40579(18) 0.70148(5) 0.41350(13) 0.0340(4) Uani 1 1 d . . . . .
H49 H 0.371985 0.725014 0.413919 0.041 Uiso 1 1 calc R . . . .
C50 C 0.52920(17) 0.69519(4) 0.45221(12) 0.0275(4) Uani 1 1 d . . . . .
H50 H 0.579413 0.714477 0.478592 0.033 Uiso 1 1 calc R . . . .
C51 C 0.80504(15) 0.65296(4) 0.41539(11) 0.0196(3) Uani 1 1 d . . . . .
C52 C 0.77001(16) 0.66626(4) 0.32798(11) 0.0213(3) Uani 1 1 d . . . . .
H52 H 0.688300 0.676432 0.312854 0.026 Uiso 1 1 calc R . . . .
C53 C 0.85282(17) 0.66494(4) 0.26194(11) 0.0260(4) Uani 1 1 d . . . . .
H53 H 0.827194 0.674179 0.202233 0.031 Uiso 1 1 calc R . . . .
C54 C 0.97114(18) 0.65040(5) 0.28247(13) 0.0336(4) Uani 1 1 d . . . . .
H54 H 1.027424 0.649389 0.237205 0.040 Uiso 1 1 calc R . . . .
C55 C 1.0078(2) 0.63719(6) 0.36983(15) 0.0451(5) Uani 1 1 d . . . . .
H55 H 1.089898 0.627261 0.384902 0.054 Uiso 1 1 calc R . . . .
C56 C 0.92502(18) 0.63842(6) 0.43516(13) 0.0364(4) Uani 1 1 d . . . . .
H56 H 0.950942 0.629125 0.494770 0.044 Uiso 1 1 calc R . . . .
C57 C 0.87418(19) 0.79677(5) 0.62715(15) 0.0371(5) Uani 1 1 d . . . . .
H57A H 0.796490 0.795197 0.583864 0.056 Uiso 1 1 calc GR . . . .
H57B H 0.923427 0.817640 0.612073 0.056 Uiso 1 1 calc GR . . . .
H57C H 0.852315 0.799251 0.689702 0.056 Uiso 1 1 calc GR . . . .
C58 C 1.07425(18) 0.76474(5) 0.68615(14) 0.0346(4) Uani 1 1 d . . . . .
H58A H 1.054407 0.767328 0.749196 0.052 Uiso 1 1 calc GR . . . .
H58B H 1.124478 0.785319 0.670473 0.052 Uiso 1 1 calc GR . . . .
H58C H 1.122659 0.742667 0.681018 0.052 Uiso 1 1 calc GR . . . .
C59 C 0.81851(15) 0.69243(4) 0.90835(11) 0.0219(3) Uani 1 1 d . . . . .
C60 C 0.94196(18) 0.67993(6) 0.91388(13) 0.0379(5) Uani 1 1 d . . . . .
H60 H 0.965999 0.665421 0.865824 0.045 Uiso 1 1 calc R . . . .
C61 C 1.0309(2) 0.68819(7) 0.98807(14) 0.0497(6) Uani 1 1 d . . . . .
H61 H 1.114920 0.679374 0.990380 0.060 Uiso 1 1 calc R . . . .
C62 C 0.9976(2) 0.70919(6) 1.05862(13) 0.0416(5) Uani 1 1 d . . . . .
H62 H 1.058645 0.715182 1.109163 0.050 Uiso 1 1 calc R . . . .
C63 C 0.87574(19) 0.72131(5) 1.05494(12) 0.0342(4) Uani 1 1 d . . . . .
H63 H 0.852084 0.735583 1.103559 0.041 Uiso 1 1 calc R . . . .
C64 C 0.78628(17) 0.71291(4) 0.98077(11) 0.0270(4) Uani 1 1 d . . . . .
H64 H 0.701911 0.721322 0.979653 0.032 Uiso 1 1 calc R . . . .
C65 C 0.59062(16) 0.69423(4) 0.83220(11) 0.0217(3) Uani 1 1 d . . . . .
C66 C 0.55415(19) 0.72922(5) 0.81145(13) 0.0347(4) Uani 1 1 d . . . . .
H66 H 0.612478 0.745361 0.789568 0.042 Uiso 1 1 calc R . . . .
C67 C 0.4333(2) 0.74087(6) 0.82234(14) 0.0464(5) Uani 1 1 d . . . . .
H67 H 0.409483 0.764943 0.808068 0.056 Uiso 1 1 calc R . . . .
C68 C 0.3478(2) 0.71776(7) 0.85368(14) 0.0468(6) Uani 1 1 d . . . . .
H68 H 0.265179 0.725821 0.861285 0.056 Uiso 1 1 calc R . . . .
C69 C 0.38248(18) 0.68305(6) 0.87389(14) 0.0415(5) Uani 1 1 d . . . . .
H69 H 0.323512 0.666993 0.895321 0.050 Uiso 1 1 calc R . . . .
C70 C 0.50316(17) 0.67124(5) 0.86321(12) 0.0296(4) Uani 1 1 d . . . . .
H70 H 0.526139 0.647098 0.877328 0.036 Uiso 1 1 calc R . . . .
O5 O 0.8659(2) 0.53562(5) 0.52272(14) 0.0751(6) Uani 1 1 d D . . . .
H5A H 0.792(2) 0.5497(7) 0.542(2) 0.113 Uiso 1 1 d DR . . . .
H5B H 0.830(3) 0.5117(5) 0.525(2) 0.113 Uiso 1 1 d DR . . . .
O6 O 0.97519(16) 0.55213(5) 0.69098(14) 0.0635(5) Uani 1 1 d D . . . .
H6A H 0.938(3) 0.5413(8) 0.6197(14) 0.095 Uiso 1 1 d DR . . . .
H6B H 1.050(2) 0.5616(8) 0.6769(19) 0.095 Uiso 1 1 d DR . . . .


_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 1.5775(11) . ?
P1 O2 1.5734(11) . ?
P1 O3 1.5483(11) . ?
P1 O4 1.4665(11) . ?
O1 C1 1.4077(17) . ?
O2 C36 1.4127(17) . ?
O3 H3 0.8400 . ?
C1 C2 1.393(2) . ?
C1 C6 1.387(2) . ?
C2 C3 1.392(2) . ?
C2 C7 1.527(2) . ?
C3 H3A 0.9500 . ?
C3 C4 1.397(2) . ?
C4 C5 1.390(2) . ?
C4 C8 1.521(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.399(2) . ?
C6 C9 1.520(2) . ?
C7 H7 1.0000 . ?
C7 C10 1.528(2) . ?
C7 C16 1.522(2) . ?
C8 H8 1.0000 . ?
C8 C22 1.527(2) . ?
C8 C23 1.525(2) . ?
C9 H9 1.0000 . ?
C9 C24 1.528(2) . ?
C9 C30 1.522(2) . ?
C10 C11 1.390(2) . ?
C10 C15 1.392(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.391(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.379(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.384(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.383(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.390(2) . ?
C16 C21 1.391(2) . ?
C17 H17 0.9500 . ?
C17 C18 1.383(2) . ?
C18 H18 0.9500 . ?
C18 C19 1.382(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.385(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.384(2) . ?
C21 H21 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.393(2) . ?
C24 C29 1.383(2) . ?
C25 H25 0.9500 . ?
C25 C26 1.380(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.375(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.378(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.396(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.382(2) . ?
C30 C35 1.375(2) . ?
C31 H31 0.9500 . ?
C31 C32 1.385(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.370(3) . ?
C33 H33 0.9500 . ?
C33 C34 1.361(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.393(3) . ?
C35 H35 0.9500 . ?
C36 C37 1.390(2) . ?
C36 C41 1.391(2) . ?
C37 C38 1.390(2) . ?
C37 C42 1.525(2) . ?
C38 H38 0.9500 . ?
C38 C39 1.391(2) . ?
C39 C40 1.394(2) . ?
C39 C43 1.523(2) . ?
C40 H40 0.9500 . ?
C40 C41 1.394(2) . ?
C41 C44 1.528(2) . ?
C42 H42 1.0000 . ?
C42 C45 1.521(2) . ?
C42 C51 1.523(2) . ?
C43 H43 1.0000 . ?
C43 C57 1.517(3) . ?
C43 C58 1.519(2) . ?
C44 H44 1.0000 . ?
C44 C59 1.527(2) . ?
C44 C65 1.517(2) . ?
C45 C46 1.391(2) . ?
C45 C50 1.386(2) . ?
C46 H46 0.9500 . ?
C46 C47 1.384(2) . ?
C47 H47 0.9500 . ?
C47 C48 1.385(3) . ?
C48 H48 0.9500 . ?
C48 C49 1.380(3) . ?
C49 H49 0.9500 . ?
C49 C50 1.385(3) . ?
C50 H50 0.9500 . ?
C51 C52 1.383(2) . ?
C51 C56 1.385(2) . ?
C52 H52 0.9500 . ?
C52 C53 1.391(2) . ?
C53 H53 0.9500 . ?
C53 C54 1.371(3) . ?
C54 H54 0.9500 . ?
C54 C55 1.384(3) . ?
C55 H55 0.9500 . ?
C55 C56 1.383(3) . ?
C56 H56 0.9500 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 C60 1.388(3) . ?
C59 C64 1.388(2) . ?
C60 H60 0.9500 . ?
C60 C61 1.386(3) . ?
C61 H61 0.9500 . ?
C61 C62 1.381(3) . ?
C62 H62 0.9500 . ?
C62 C63 1.369(3) . ?
C63 H63 0.9500 . ?
C63 C64 1.390(2) . ?
C64 H64 0.9500 . ?
C65 C66 1.386(2) . ?
C65 C70 1.385(2) . ?
C66 H66 0.9500 . ?
C66 C67 1.387(3) . ?
C67 H67 0.9500 . ?
C67 C68 1.375(3) . ?
C68 H68 0.9500 . ?
C68 C69 1.370(3) . ?
C69 H69 0.9500 . ?
C69 C70 1.386(3) . ?
C70 H70 0.9500 . ?
O5 H5A 1.013(17) . ?
O5 H5B 0.975(17) . ?
O6 H6A 1.145(17) . ?
O6 H6B 0.922(17) . ?

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
O2 P1 O1 97.25(6) . . ?
O3 P1 O1 107.33(6) . . ?
O3 P1 O2 105.57(6) . . ?
O4 P1 O1 113.70(6) . . ?
O4 P1 O2 116.01(6) . . ?
O4 P1 O3 115.16(7) . . ?
C1 O1 P1 124.81(9) . . ?
C36 O2 P1 126.11(9) . . ?
P1 O3 H3 109.5 . . ?
C2 C1 O1 117.59(12) . . ?
C6 C1 O1 118.82(12) . . ?
C6 C1 C2 123.38(13) . . ?
C1 C2 C7 118.50(13) . . ?
C3 C2 C1 117.33(13) . . ?
C3 C2 C7 124.10(13) . . ?
C2 C3 H3A 119.1 . . ?
C2 C3 C4 121.80(13) . . ?
C4 C3 H3A 119.1 . . ?
C3 C4 C8 119.94(13) . . ?
C5 C4 C3 118.32(13) . . ?
C5 C4 C8 121.69(13) . . ?
C4 C5 H5 119.0 . . ?
C4 C5 C6 122.02(14) . . ?
C6 C5 H5 119.0 . . ?
C1 C6 C5 117.07(13) . . ?
C1 C6 C9 121.69(13) . . ?
C5 C6 C9 121.22(13) . . ?
C2 C7 H7 106.3 . . ?
C2 C7 C10 111.24(12) . . ?
C10 C7 H7 106.3 . . ?
C16 C7 C2 114.11(12) . . ?
C16 C7 H7 106.3 . . ?
C16 C7 C10 111.95(12) . . ?
C4 C8 H8 107.5 . . ?
C4 C8 C22 109.80(13) . . ?
C4 C8 C23 113.61(13) . . ?
C22 C8 H8 107.5 . . ?
C23 C8 H8 107.5 . . ?
C23 C8 C22 110.64(14) . . ?
C6 C9 H9 106.3 . . ?
C6 C9 C24 110.92(12) . . ?
C6 C9 C30 112.95(12) . . ?
C24 C9 H9 106.3 . . ?
C30 C9 H9 106.3 . . ?
C30 C9 C24 113.41(12) . . ?
C11 C10 C7 122.33(14) . . ?
C11 C10 C15 118.32(14) . . ?
C15 C10 C7 119.35(14) . . ?
C10 C11 H11 119.7 . . ?
C10 C11 C12 120.64(15) . . ?
C12 C11 H11 119.7 . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.33(17) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 120.2 . . ?
C12 C13 C14 119.53(16) . . ?
C14 C13 H13 120.2 . . ?
C13 C14 H14 119.9 . . ?
C15 C14 C13 120.21(16) . . ?
C15 C14 H14 119.9 . . ?
C10 C15 H15 119.5 . . ?
C14 C15 C10 120.98(16) . . ?
C14 C15 H15 119.5 . . ?
C17 C16 C7 121.84(14) . . ?
C17 C16 C21 118.23(14) . . ?
C21 C16 C7 119.92(14) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 C16 120.96(15) . . ?
C18 C17 H17 119.5 . . ?
C17 C18 H18 119.9 . . ?
C19 C18 C17 120.22(16) . . ?
C19 C18 H18 119.9 . . ?
C18 C19 H19 120.2 . . ?
C18 C19 C20 119.51(16) . . ?
C20 C19 H19 120.2 . . ?
C19 C20 H20 119.9 . . ?
C21 C20 C19 120.11(17) . . ?
C21 C20 H20 119.9 . . ?
C16 C21 H21 119.5 . . ?
C20 C21 C16 120.94(16) . . ?
C20 C21 H21 119.5 . . ?
C8 C22 H22A 109.5 . . ?
C8 C22 H22B 109.5 . . ?
C8 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C8 C23 H23A 109.5 . . ?
C8 C23 H23B 109.5 . . ?
C8 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C9 118.25(14) . . ?
C29 C24 C9 123.20(14) . . ?
C29 C24 C25 118.55(15) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 C24 121.08(16) . . ?
C26 C25 H25 119.5 . . ?
C25 C26 H26 120.0 . . ?
C27 C26 C25 120.05(17) . . ?
C27 C26 H26 120.0 . . ?
C26 C27 H27 120.1 . . ?
C26 C27 C28 119.78(17) . . ?
C28 C27 H27 120.1 . . ?
C27 C28 H28 119.9 . . ?
C27 C28 C29 120.29(19) . . ?
C29 C28 H28 119.9 . . ?
C24 C29 C28 120.21(18) . . ?
C24 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C31 C30 C9 118.93(15) . . ?
C35 C30 C9 123.43(14) . . ?
C35 C30 C31 117.62(16) . . ?
C30 C31 H31 119.5 . . ?
C30 C31 C32 121.09(18) . . ?
C32 C31 H31 119.5 . . ?
C31 C32 H32 119.7 . . ?
C33 C32 C31 120.61(18) . . ?
C33 C32 H32 119.7 . . ?
C32 C33 H33 120.6 . . ?
C34 C33 C32 118.87(17) . . ?
C34 C33 H33 120.6 . . ?
C33 C34 H34 119.6 . . ?
C33 C34 C35 120.79(19) . . ?
C35 C34 H34 119.6 . . ?
C30 C35 C34 120.92(17) . . ?
C30 C35 H35 119.5 . . ?
C34 C35 H35 119.5 . . ?
C37 C36 O2 118.42(13) . . ?
C37 C36 C41 123.60(13) . . ?
C41 C36 O2 117.79(13) . . ?
C36 C37 C38 117.12(14) . . ?
C36 C37 C42 120.48(13) . . ?
C38 C37 C42 122.36(13) . . ?
C37 C38 H38 119.0 . . ?
C37 C38 C39 122.05(14) . . ?
C39 C38 H38 119.0 . . ?
C38 C39 C40 118.38(14) . . ?
C38 C39 C43 119.72(14) . . ?
C40 C39 C43 121.90(14) . . ?
C39 C40 H40 119.0 . . ?
C39 C40 C41 122.00(14) . . ?
C41 C40 H40 119.0 . . ?
C36 C41 C40 116.84(14) . . ?
C36 C41 C44 120.03(13) . . ?
C40 C41 C44 123.09(13) . . ?
C37 C42 H42 106.2 . . ?
C45 C42 C37 111.73(13) . . ?
C45 C42 H42 106.2 . . ?
C45 C42 C51 113.24(13) . . ?
C51 C42 C37 112.51(13) . . ?
C51 C42 H42 106.2 . . ?
C39 C43 H43 107.4 . . ?
C57 C43 C39 111.15(14) . . ?
C57 C43 H43 107.4 . . ?
C57 C43 C58 110.93(15) . . ?
C58 C43 C39 112.32(14) . . ?
C58 C43 H43 107.4 . . ?
C41 C44 H44 106.1 . . ?
C59 C44 C41 113.00(13) . . ?
C59 C44 H44 106.1 . . ?
C65 C44 C41 111.60(13) . . ?
C65 C44 H44 106.1 . . ?
C65 C44 C59 113.34(13) . . ?
C46 C45 C42 118.61(14) . . ?
C50 C45 C42 123.00(14) . . ?
C50 C45 C46 118.35(15) . . ?
C45 C46 H46 119.4 . . ?
C47 C46 C45 121.17(16) . . ?
C47 C46 H46 119.4 . . ?
C46 C47 H47 120.1 . . ?
C46 C47 C48 119.84(17) . . ?
C48 C47 H47 120.1 . . ?
C47 C48 H48 120.3 . . ?
C49 C48 C47 119.39(17) . . ?
C49 C48 H48 120.3 . . ?
C48 C49 H49 119.7 . . ?
C48 C49 C50 120.68(17) . . ?
C50 C49 H49 119.7 . . ?
C45 C50 H50 119.7 . . ?
C49 C50 C45 120.55(16) . . ?
C49 C50 H50 119.7 . . ?
C52 C51 C42 123.08(14) . . ?
C52 C51 C56 118.01(15) . . ?
C56 C51 C42 118.89(14) . . ?
C51 C52 H52 119.6 . . ?
C51 C52 C53 120.89(16) . . ?
C53 C52 H52 119.6 . . ?
C52 C53 H53 119.8 . . ?
C54 C53 C52 120.42(16) . . ?
C54 C53 H53 119.8 . . ?
C53 C54 H54 120.3 . . ?
C53 C54 C55 119.33(17) . . ?
C55 C54 H54 120.3 . . ?
C54 C55 H55 120.0 . . ?
C56 C55 C54 120.07(18) . . ?
C56 C55 H55 120.0 . . ?
C51 C56 H56 119.4 . . ?
C55 C56 C51 121.27(17) . . ?
C55 C56 H56 119.4 . . ?
C43 C57 H57A 109.5 . . ?
C43 C57 H57B 109.5 . . ?
C43 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C43 C58 H58A 109.5 . . ?
C43 C58 H58B 109.5 . . ?
C43 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C60 C59 C44 118.57(15) . . ?
C64 C59 C44 123.69(15) . . ?
C64 C59 C60 117.64(16) . . ?
C59 C60 H60 119.3 . . ?
C61 C60 C59 121.36(18) . . ?
C61 C60 H60 119.3 . . ?
C60 C61 H61 119.9 . . ?
C62 C61 C60 120.1(2) . . ?
C62 C61 H61 119.9 . . ?
C61 C62 H62 120.4 . . ?
C63 C62 C61 119.29(18) . . ?
C63 C62 H62 120.4 . . ?
C62 C63 H63 119.7 . . ?
C62 C63 C64 120.65(18) . . ?
C64 C63 H63 119.7 . . ?
C59 C64 C63 120.92(17) . . ?
C59 C64 H64 119.5 . . ?
C63 C64 H64 119.5 . . ?
C66 C65 C44 122.03(15) . . ?
C70 C65 C44 119.55(15) . . ?
C70 C65 C66 118.36(16) . . ?
C65 C66 H66 119.7 . . ?
C65 C66 C67 120.61(19) . . ?
C67 C66 H66 119.7 . . ?
C66 C67 H67 119.8 . . ?
C68 C67 C66 120.30(19) . . ?
C68 C67 H67 119.8 . . ?
C67 C68 H68 120.2 . . ?
C69 C68 C67 119.64(19) . . ?
C69 C68 H68 120.2 . . ?
C68 C69 H69 119.8 . . ?
C68 C69 C70 120.3(2) . . ?
C70 C69 H69 119.8 . . ?
C65 C70 C69 120.76(18) . . ?
C65 C70 H70 119.6 . . ?
C69 C70 H70 119.6 . . ?
H5A O5 H5B 98.3(19) . . ?
H6A O6 H6B 97.9(17) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3 O6 0.84 1.76 2.599(2) 177.5 .
O5 H5A O4 1.013(17) 1.816(19) 2.808(2) 165(3) .
O6 H6A O5 1.145(17) 1.547(18) 2.668(3) 165(3) .

_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_AJ0074
_database_code_depnum_ccdc_archive 'CCDC 1843002'
_audit_update_record             
;
2018-07-30 deposited with the CCDC.
2018-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H35 O4 P'
_chemical_formula_sum            'C24 H35 O4 P'
_chemical_oxdiff_formula         'C25 H26 O6 P1'
_chemical_formula_weight         418.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.6709(3)
_cell_length_b                   11.8216(5)
_cell_length_c                   12.5323(3)
_cell_angle_alpha                71.887(3)
_cell_angle_beta                 79.512(3)
_cell_angle_gamma                77.411(3)
_cell_volume                     1182.52(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9717
_cell_measurement_theta_min      3.1390
_cell_measurement_theta_max      29.2480

_exptl_crystal_description       trapezoid
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_F_000             452
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.596
_exptl_crystal_size_mid          0.406
_exptl_crystal_size_min          0.156
_exptl_absorpt_coefficient_mu    0.142
_shelx_estimated_absorpt_T_min   0.920
_shelx_estimated_absorpt_T_max   0.978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.88702
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17388
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.780
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             4872
_reflns_number_gt                4376
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0396P)²+0.4017P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4872
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0880
_refine_ls_wR_factor_gt          0.0856
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.11588(3) 0.55076(2) 0.84040(2) 0.01185(9) Uani 1 1 d . . . . .
O1 O 0.27072(9) 0.52665(7) 0.75818(6) 0.01392(17) Uani 1 1 d . . . . .
O2 O 0.01282(9) 0.65837(7) 0.75866(6) 0.01478(18) Uani 1 1 d . . . . .
O3 O 0.16644(9) 0.59523(7) 0.93001(7) 0.01603(18) Uani 1 1 d . . . . .
H3 H 0.103950 0.578843 0.990163 0.024 Uiso 1 1 calc R U . . .
O4 O 0.02561(9) 0.44986(7) 0.88751(7) 0.01520(18) Uani 1 1 d . . . . .
C1 C 0.42096(13) 0.46006(10) 0.78860(9) 0.0148(2) Uani 1 1 d . . . . .
C2 C 0.44976(14) 0.33585(11) 0.80196(10) 0.0187(3) Uani 1 1 d . . . . .
C3 C 0.60183(16) 0.27391(12) 0.82653(11) 0.0254(3) Uani 1 1 d . . . . .
H3A H 0.625687 0.188815 0.839023 0.030 Uiso 1 1 calc R U . . .
C4 C 0.71816(15) 0.33440(13) 0.83297(11) 0.0274(3) Uani 1 1 d . . . . .
H4 H 0.820898 0.290762 0.849395 0.033 Uiso 1 1 calc R U . . .
C5 C 0.68533(15) 0.45797(13) 0.81558(11) 0.0244(3) Uani 1 1 d . . . . .
H5 H 0.767049 0.498548 0.818544 0.029 Uiso 1 1 calc R U . . .
C6 C 0.53484(14) 0.52456(11) 0.79376(10) 0.0180(2) Uani 1 1 d . . . . .
C7 C 0.32556(16) 0.26907(11) 0.79034(12) 0.0245(3) Uani 1 1 d . . . . .
H7 H 0.230302 0.330393 0.764983 0.029 Uiso 1 1 calc R U . . .
C8 C 0.2733(2) 0.18393(14) 0.90444(14) 0.0415(4) Uani 1 1 d . . . . .
H8A H 0.363569 0.120505 0.929550 0.062 Uiso 1 1 calc R U . . .
H8B H 0.186593 0.147040 0.896801 0.062 Uiso 1 1 calc R U . . .
H8C H 0.236369 0.229590 0.960221 0.062 Uiso 1 1 calc R U . . .
C9 C 0.38605(18) 0.20077(14) 0.70094(13) 0.0334(3) Uani 1 1 d . . . . .
H9A H 0.419782 0.257171 0.628864 0.050 Uiso 1 1 calc R U . . .
H9B H 0.300486 0.164003 0.691242 0.050 Uiso 1 1 calc R U . . .
H9C H 0.476603 0.137423 0.725522 0.050 Uiso 1 1 calc R U . . .
C10 C 0.50378(15) 0.66074(12) 0.77341(11) 0.0219(3) Uani 1 1 d . . . . .
H10 H 0.386709 0.690022 0.772012 0.026 Uiso 1 1 calc R U . . .
C11 C 0.5890(2) 0.72192(14) 0.65833(13) 0.0373(4) Uani 1 1 d . . . . .
H11A H 0.704256 0.694994 0.657933 0.056 Uiso 1 1 calc R U . . .
H11B H 0.564085 0.809799 0.644732 0.056 Uiso 1 1 calc R U . . .
H11C H 0.553239 0.700123 0.598683 0.056 Uiso 1 1 calc R U . . .
C12 C 0.5541(2) 0.69588(15) 0.86804(14) 0.0374(4) Uani 1 1 d . . . . .
H12A H 0.500111 0.654615 0.941068 0.056 Uiso 1 1 calc R U . . .
H12B H 0.524678 0.783503 0.855371 0.056 Uiso 1 1 calc R U . . .
H12C H 0.669588 0.672035 0.868281 0.056 Uiso 1 1 calc R U . . .
C13 C 0.07966(13) 0.75500(10) 0.67770(10) 0.0157(2) Uani 1 1 d . . . . .
C14 C 0.08022(15) 0.85836(11) 0.70885(10) 0.0200(3) Uani 1 1 d . . . . .
C15 C 0.14875(17) 0.95033(11) 0.62761(11) 0.0267(3) Uani 1 1 d . . . . .
H15 H 0.152560 1.021684 0.646079 0.032 Uiso 1 1 calc R U . . .
C16 C 0.21134(17) 0.93985(12) 0.52065(11) 0.0270(3) Uani 1 1 d . . . . .
H16 H 0.259729 1.002749 0.467093 0.032 Uiso 1 1 calc R U . . .
C17 C 0.20322(15) 0.83736(11) 0.49189(10) 0.0222(3) Uani 1 1 d . . . . .
H17 H 0.244747 0.831530 0.417856 0.027 Uiso 1 1 calc R U . . .
C18 C 0.13550(14) 0.74270(11) 0.56918(10) 0.0170(2) Uani 1 1 d . . . . .
C19 C 0.00610(17) 0.87466(11) 0.82430(11) 0.0246(3) Uani 1 1 d . . . . .
H19 H -0.037353 0.799928 0.869567 0.030 Uiso 1 1 calc R U . . .
C20 C 0.1292(2) 0.89131(13) 0.88857(12) 0.0356(4) Uani 1 1 d . . . . .
H20A H 0.213255 0.819838 0.900344 0.053 Uiso 1 1 calc R U . . .
H20B H 0.077492 0.901895 0.962007 0.053 Uiso 1 1 calc R U . . .
H20C H 0.175745 0.962868 0.844641 0.053 Uiso 1 1 calc R U . . .
C21 C -0.1326(2) 0.98141(13) 0.81062(13) 0.0401(4) Uani 1 1 d . . . . .
H21A H -0.093035 1.055653 0.765395 0.060 Uiso 1 1 calc R U . . .
H21B H -0.181138 0.989920 0.885328 0.060 Uiso 1 1 calc R U . . .
H21C H -0.212387 0.966953 0.772389 0.060 Uiso 1 1 calc R U . . .
C22 C 0.11934(15) 0.63496(11) 0.53297(10) 0.0188(3) Uani 1 1 d . . . . .
H22 H 0.071527 0.576249 0.600343 0.023 Uiso 1 1 calc R U . . .
C23 C 0.00547(16) 0.67610(13) 0.44200(11) 0.0258(3) Uani 1 1 d . . . . .
H23A H -0.098580 0.713671 0.472231 0.039 Uiso 1 1 calc R U . . .
H23B H -0.006805 0.606022 0.420309 0.039 Uiso 1 1 calc R U . . .
H23C H 0.049273 0.734800 0.375500 0.039 Uiso 1 1 calc R U . . .
C24 C 0.28063(16) 0.57016(12) 0.48981(11) 0.0253(3) Uani 1 1 d . . . . .
H24A H 0.326987 0.624746 0.421136 0.038 Uiso 1 1 calc R U . . .
H24B H 0.265600 0.498154 0.472644 0.038 Uiso 1 1 calc R U . . .
H24C H 0.352410 0.546181 0.548056 0.038 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 O4 1.4781(8) . ?
P1 O3 1.5417(8) . ?
P1 O1 1.5676(8) . ?
P1 O2 1.5791(8) . ?
O1 C1 1.4175(13) . ?
O2 C13 1.4226(14) . ?
O3 H3 0.8400 . ?
C1 C6 1.3938(17) . ?
C1 C2 1.3961(17) . ?
C2 C3 1.3987(18) . ?
C2 C7 1.5178(18) . ?
C3 C4 1.384(2) . ?
C3 H3A 0.9500 . ?
C4 C5 1.381(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.3948(17) . ?
C5 H5 0.9500 . ?
C6 C10 1.5199(17) . ?
C7 C8 1.527(2) . ?
C7 C9 1.5317(18) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C12 1.5307(19) . ?
C10 C11 1.5315(19) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.3947(17) . ?
C13 C18 1.3992(16) . ?
C14 C15 1.3946(18) . ?
C14 C19 1.5246(17) . ?
C15 C16 1.3841(19) . ?
C15 H15 0.9500 . ?
C16 C17 1.3860(19) . ?
C16 H16 0.9500 . ?
C17 C18 1.3931(17) . ?
C17 H17 0.9500 . ?
C18 C22 1.5193(17) . ?
C19 C20 1.526(2) . ?
C19 C21 1.5321(19) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C24 1.5332(17) . ?
C22 C23 1.5385(17) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 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
O4 P1 O3 114.46(5) . . ?
O4 P1 O1 115.53(5) . . ?
O3 P1 O1 106.04(4) . . ?
O4 P1 O2 108.59(5) . . ?
O3 P1 O2 110.23(5) . . ?
O1 P1 O2 101.15(4) . . ?
C1 O1 P1 126.97(7) . . ?
C13 O2 P1 122.43(7) . . ?
P1 O3 H3 109.5 . . ?
C6 C1 C2 124.19(11) . . ?
C6 C1 O1 117.63(10) . . ?
C2 C1 O1 117.94(10) . . ?
C1 C2 C3 116.45(12) . . ?
C1 C2 C7 122.98(11) . . ?
C3 C2 C7 120.57(11) . . ?
C4 C3 C2 121.17(12) . . ?
C4 C3 H3A 119.4 . . ?
C2 C3 H3A 119.4 . . ?
C5 C4 C3 120.19(12) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 121.47(12) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C1 C6 C5 116.48(11) . . ?
C1 C6 C10 123.52(11) . . ?
C5 C6 C10 119.98(11) . . ?
C2 C7 C8 110.57(12) . . ?
C2 C7 C9 111.51(11) . . ?
C8 C7 C9 111.10(11) . . ?
C2 C7 H7 107.8 . . ?
C8 C7 H7 107.8 . . ?
C9 C7 H7 107.8 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 C12 111.69(11) . . ?
C6 C10 C11 110.29(11) . . ?
C12 C10 C11 110.65(12) . . ?
C6 C10 H10 108.0 . . ?
C12 C10 H10 108.0 . . ?
C11 C10 H10 108.0 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C18 123.55(11) . . ?
C14 C13 O2 118.66(10) . . ?
C18 C13 O2 117.74(10) . . ?
C15 C14 C13 116.90(11) . . ?
C15 C14 C19 120.18(11) . . ?
C13 C14 C19 122.90(11) . . ?
C16 C15 C14 121.40(12) . . ?
C16 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
C15 C16 C17 119.82(12) . . ?
C15 C16 H16 120.1 . . ?
C17 C16 H16 120.1 . . ?
C16 C17 C18 121.43(12) . . ?
C16 C17 H17 119.3 . . ?
C18 C17 H17 119.3 . . ?
C17 C18 C13 116.78(11) . . ?
C17 C18 C22 120.16(11) . . ?
C13 C18 C22 123.01(11) . . ?
C14 C19 C20 111.65(12) . . ?
C14 C19 C21 110.07(11) . . ?
C20 C19 C21 110.93(12) . . ?
C14 C19 H19 108.0 . . ?
C20 C19 H19 108.0 . . ?
C21 C19 H19 108.0 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22 C24 112.22(10) . . ?
C18 C22 C23 109.73(10) . . ?
C24 C22 C23 110.52(10) . . ?
C18 C22 H22 108.1 . . ?
C24 C22 H22 108.1 . . ?
C23 C22 H22 108.1 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3 O4 0.84 1.72 2.5553(11) 178.2 2_567

_refine_diff_density_max         0.253
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.043


####################################################################### 
# 
# 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_aj0386
_database_code_depnum_ccdc_archive 'CCDC 1843004'
_audit_update_record             
;
2018-07-30 deposited with the CCDC.
2018-09-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT234_aj0386              
;
PROBLEM: Large Hirshfeld Difference N1       --C73'             0.16 Ang.  
RESPONSE: These two atoms constitute the link between a disordered ethyl
substituent and the central nitrogen atom of the ammonium cation, which 
was not treated as disodered.
;
_vrf_PLAT244_aj0386              
;
PROBLEM: Low    'Solvent' Ueq as Compared to Neighbors of         N1 Check 
RESPONSE: See response to PLAT234.
;
_vrf_PLAT480_aj0386              
;
PROBLEM: Long H...A H-Bond Reported H71B     ..O2               2.65 Ang.  
RESPONSE: he hydrogen bonds were identified with HTAB in ShelXL. 
Despite being long they are in reasonable arrangement for an interaction.
;
_vrf_PLAT906_aj0386              
;
PROBLEM: Large K Value in the Analysis of Variance ......      4.104 Check 
RESPONSE: The K Value in the Analysis of Variance is only large for the 
weakest fraction of reflexes with Fc/Fc(max) < 0.004.
;
_vrf_PLAT976_aj0386              
;
PROBLEM: Check Calcd Resid. Dens.  0.91A   From O5             -0.55 eA-3  
RESPONSE: The refined water hydrogen atoms' locations might represent oly 
the major orientation of the two water molecules with other orientations 
possibly partially occupied, albeit only as minor contributions as all 
hydrogen atoms of water were only restrained by DFIX for O-H and H H 
distances but not their Uiso values. 
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C70 H62 O4 P, C6 H16 N, 2(C2 H3 N), 2(H2 O)'
_chemical_formula_sum            'C80 H88 N3 O6 P'
_chemical_formula_weight         1218.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.4577(4)
_cell_length_b                   14.9850(4)
_cell_length_c                   27.7532(8)
_cell_angle_alpha                90
_cell_angle_beta                 96.392(2)
_cell_angle_gamma                90
_cell_volume                     6801.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    28166
_cell_measurement_theta_min      2.7230
_cell_measurement_theta_max      28.7350

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_F_000             2608
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.466
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.224
_exptl_absorpt_coefficient_mu    0.096
_shelx_estimated_absorpt_T_min   0.956
_shelx_estimated_absorpt_T_max   0.979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.57859
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            84684
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.447
_diffrn_reflns_theta_max         28.835
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             15942
_reflns_number_gt                12391
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0833P)²+4.2056P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15942
_refine_ls_number_parameters     884
_refine_ls_number_restraints     224
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0580
_refine_ls_wR_factor_ref         0.1640
_refine_ls_wR_factor_gt          0.1527
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.69100(2) 0.30588(3) 0.58590(2) 0.02060(11) Uani 1 1 d . . . . .
O1 O 0.78933(7) 0.30533(8) 0.58653(4) 0.0207(2) Uani 1 1 d . . . . .
O2 O 0.68410(7) 0.29041(7) 0.64232(4) 0.0213(2) Uani 1 1 d . . . . .
O3 O 0.65819(7) 0.39871(8) 0.57736(4) 0.0267(3) Uani 1 1 d . . . . .
O4 O 0.65427(7) 0.23332(8) 0.55460(4) 0.0268(3) Uani 1 1 d . . . . .
C1 C 0.82733(9) 0.29735(11) 0.54381(5) 0.0192(3) Uani 1 1 d . . . . .
C2 C 0.84619(10) 0.21242(11) 0.52726(6) 0.0212(3) Uani 1 1 d . . . . .
C3 C 0.88661(10) 0.20783(11) 0.48571(6) 0.0227(3) Uani 1 1 d . . . . .
H3 H 0.898901 0.150851 0.473377 0.027 Uiso 1 1 calc R U . . .
C4 C 0.90943(10) 0.28337(11) 0.46183(6) 0.0236(3) Uani 1 1 d . . . . .
C5 C 0.89012(10) 0.36649(11) 0.47986(6) 0.0223(3) Uani 1 1 d . . . . .
H5 H 0.905440 0.418652 0.463643 0.027 Uiso 1 1 calc R U . . .
C6 C 0.84905(9) 0.37585(11) 0.52094(6) 0.0204(3) Uani 1 1 d . . . . .
C7 C 0.82715(10) 0.46793(11) 0.53988(6) 0.0234(3) Uani 1 1 d . . . . .
H7 H 0.769683 0.463377 0.548138 0.028 Uiso 1 1 calc R U . . .
C8 C 0.95014(12) 0.27540(13) 0.41568(7) 0.0312(4) Uani 1 1 d . . . . .
H8 H 0.966398 0.336555 0.405971 0.037 Uiso 1 1 calc R U . . .
C9 C 0.82603(10) 0.12669(11) 0.55291(6) 0.0228(3) Uani 1 1 d . . . . .
H9 H 0.780359 0.140805 0.572604 0.027 Uiso 1 1 calc R U . . .
C10 C 0.87944(11) 0.49643(11) 0.58653(6) 0.0252(4) Uani 1 1 d . . . . .
C11 C 0.94796(12) 0.45054(13) 0.60657(7) 0.0329(4) Uani 1 1 d . . . . .
H11 H 0.963820 0.397365 0.591486 0.039 Uiso 1 1 calc R U . . .
C12 C 0.99406(13) 0.48096(15) 0.64845(8) 0.0403(5) Uani 1 1 d . . . . .
H12 H 1.040954 0.448592 0.661665 0.048 Uiso 1 1 calc R U . . .
C13 C 0.97178(14) 0.55799(15) 0.67079(7) 0.0412(5) Uani 1 1 d . . . . .
H13 H 1.003489 0.579137 0.699198 0.049 Uiso 1 1 calc R U . . .
C14 C 0.90319(15) 0.60411(14) 0.65163(7) 0.0407(5) Uani 1 1 d . . . . .
H14 H 0.887347 0.656935 0.667045 0.049 Uiso 1 1 calc R U . . .
C15 C 0.85720(13) 0.57367(13) 0.60990(7) 0.0334(4) Uani 1 1 d . . . . .
H15 H 0.809938 0.605854 0.597087 0.040 Uiso 1 1 calc R U . . .
C16 C 0.82710(11) 0.54080(12) 0.50160(7) 0.0274(4) Uani 1 1 d D U . . .
C17 C 0.7622(4) 0.5495(5) 0.4641(3) 0.0400(12) Uani 0.498(9) 1 d D U P A 1
H17 H 0.716095 0.511243 0.463626 0.048 Uiso 0.498(9) 1 calc R U P A 1
C18 C 0.7645(3) 0.6132(4) 0.4278(2) 0.0461(13) Uani 0.498(9) 1 d D U P A 1
H18 H 0.718414 0.620977 0.404362 0.055 Uiso 0.498(9) 1 calc R U P A 1
C19 C 0.8337(4) 0.6655(5) 0.4255(3) 0.0419(14) Uani 0.498(9) 1 d D U P A 1
H19 H 0.836105 0.707795 0.400175 0.050 Uiso 0.498(9) 1 calc R U P A 1
C17' C 0.7522(4) 0.5731(4) 0.4804(3) 0.0397(12) Uani 0.502(9) 1 d D U P A 2
H17' H 0.702835 0.546752 0.488275 0.048 Uiso 0.502(9) 1 calc R U P A 2
C18' C 0.7494(4) 0.6437(4) 0.4480(3) 0.0490(13) Uani 0.502(9) 1 d D U P A 2
H18' H 0.698037 0.665099 0.433481 0.059 Uiso 0.502(9) 1 calc R U P A 2
C19' C 0.8201(5) 0.6830(5) 0.4366(3) 0.0442(15) Uani 0.502(9) 1 d D U P A 2
H19' H 0.817608 0.729241 0.413077 0.053 Uiso 0.502(9) 1 calc R U P A 2
C20 C 0.89665(13) 0.65493(13) 0.45972(7) 0.0363(4) Uani 1 1 d D U . . .
H20 H 0.942436 0.693628 0.460082 0.044 Uiso 1 1 calc R U . A 1
C21 C 0.89696(12) 0.58904(12) 0.49470(7) 0.0308(4) Uani 1 1 d . . . . .
H21 H 0.946414 0.576431 0.514577 0.037 Uiso 1 1 calc R U . . .
C22 C 0.88888(16) 0.23781(17) 0.37506(7) 0.0480(6) Uani 1 1 d . . . . .
H22A H 0.876383 0.175643 0.382344 0.072 Uiso 1 1 calc R U . . .
H22B H 0.912586 0.240567 0.344225 0.072 Uiso 1 1 calc R U . . .
H22C H 0.838519 0.273210 0.372639 0.072 Uiso 1 1 calc R U . . .
C23 C 1.02668(13) 0.21711(14) 0.42184(8) 0.0392(5) Uani 1 1 d . . . . .
H23A H 1.065101 0.240669 0.448299 0.059 Uiso 1 1 calc R U . . .
H23B H 1.052522 0.217351 0.391687 0.059 Uiso 1 1 calc R U . . .
H23C H 1.011540 0.155892 0.429485 0.059 Uiso 1 1 calc R U . . .
C24 C 0.79481(11) 0.05361(12) 0.51649(6) 0.0251(3) Uani 1 1 d . . . . .
C25 C 0.71954(12) 0.06506(13) 0.48880(7) 0.0328(4) Uani 1 1 d . . . . .
H25 H 0.688891 0.117838 0.492569 0.039 Uiso 1 1 calc R U . . .
C26 C 0.68875(12) 0.00077(15) 0.45591(8) 0.0404(5) Uani 1 1 d . . . . .
H26 H 0.637732 0.010103 0.436966 0.048 Uiso 1 1 calc R U . . .
C27 C 0.73215(14) -0.07721(15) 0.45052(8) 0.0433(5) Uani 1 1 d . . . . .
H27 H 0.710935 -0.121703 0.428186 0.052 Uiso 1 1 calc R U . . .
C28 C 0.80661(14) -0.08951(15) 0.47800(9) 0.0467(5) Uani 1 1 d . . . . .
H28 H 0.836633 -0.142849 0.474573 0.056 Uiso 1 1 calc R U . . .
C29 C 0.83785(13) -0.02456(13) 0.51054(8) 0.0371(4) Uani 1 1 d . . . . .
H29 H 0.889349 -0.033687 0.528981 0.045 Uiso 1 1 calc R U . . .
C30 C 0.89780(11) 0.09321(11) 0.58817(6) 0.0265(4) Uani 1 1 d . . . . .
C31 C 0.97827(12) 0.09210(13) 0.57715(7) 0.0311(4) Uani 1 1 d . . . . .
H31 H 0.991082 0.117432 0.547535 0.037 Uiso 1 1 calc R U . . .
C32 C 1.04015(13) 0.05438(14) 0.60892(8) 0.0391(5) Uani 1 1 d . . . . .
H32 H 1.094598 0.053024 0.600615 0.047 Uiso 1 1 calc R U . . .
C33 C 1.02273(15) 0.01911(15) 0.65224(8) 0.0454(5) Uani 1 1 d . . . . .
H33 H 1.065047 -0.006588 0.673933 0.055 Uiso 1 1 calc R U . . .
C34 C 0.94364(16) 0.02110(15) 0.66417(8) 0.0461(5) Uani 1 1 d . . . . .
H34 H 0.931668 -0.002454 0.694369 0.055 Uiso 1 1 calc R U . . .
C35 C 0.88126(14) 0.05748(13) 0.63215(7) 0.0358(4) Uani 1 1 d . . . . .
H35 H 0.826828 0.057848 0.640495 0.043 Uiso 1 1 calc R U . . .
C36 C 0.71230(10) 0.21618(11) 0.67021(6) 0.0215(3) Uani 1 1 d . . . . .
C37 C 0.66255(10) 0.14113(11) 0.67143(6) 0.0240(3) Uani 1 1 d . . . . .
C38 C 0.68957(10) 0.07261(12) 0.70368(6) 0.0266(4) Uani 1 1 d . . . . .
H38 H 0.657235 0.020243 0.704547 0.032 Uiso 1 1 calc R U . . .
C39 C 0.76206(11) 0.07862(12) 0.73444(6) 0.0260(4) Uani 1 1 d . . . . .
C40 C 0.80942(10) 0.15531(12) 0.73188(6) 0.0248(3) Uani 1 1 d . . . . .
H40 H 0.859679 0.159859 0.752176 0.030 Uiso 1 1 calc R U . . .
C41 C 0.78552(10) 0.22521(11) 0.70063(6) 0.0226(3) Uani 1 1 d . . . . .
C42 C 0.57722(10) 0.13833(12) 0.64359(6) 0.0255(4) Uani 1 1 d . . . . .
H42 H 0.577940 0.180048 0.615519 0.031 Uiso 1 1 calc R U . . .
C43 C 0.78857(11) 0.00824(12) 0.77289(7) 0.0303(4) Uani 1 1 d . . . . .
H43 H 0.845863 -0.009420 0.768462 0.036 Uiso 1 1 calc R U . . .
C44 C 0.83197(10) 0.31345(11) 0.70393(6) 0.0234(3) Uani 1 1 d . . . . .
H44 H 0.822769 0.341742 0.671142 0.028 Uiso 1 1 calc R U . . .
C45 C 0.55554(10) 0.04612(12) 0.62235(7) 0.0278(4) Uani 1 1 d . . . . .
C46 C 0.57251(13) 0.02614(14) 0.57583(8) 0.0375(4) Uani 1 1 d . . . . .
H46 H 0.597631 0.069731 0.557517 0.045 Uiso 1 1 calc R U . . .
C47 C 0.55318(15) -0.05694(16) 0.55568(9) 0.0489(6) Uani 1 1 d . . . . .
H47 H 0.564406 -0.069478 0.523525 0.059 Uiso 1 1 calc R U . . .
C48 C 0.51772(14) -0.12158(15) 0.58202(9) 0.0470(5) Uani 1 1 d . . . . .
H48 H 0.505582 -0.178822 0.568359 0.056 Uiso 1 1 calc R U . . .
C49 C 0.50009(14) -0.10231(15) 0.62829(9) 0.0450(5) Uani 1 1 d . . . . .
H49 H 0.475598 -0.146301 0.646655 0.054 Uiso 1 1 calc R U . . .
C50 C 0.51815(13) -0.01864(14) 0.64803(8) 0.0385(5) Uani 1 1 d . . . . .
H50 H 0.504684 -0.005435 0.679669 0.046 Uiso 1 1 calc R U . . .
C51 C 0.51179(11) 0.17302(12) 0.67400(7) 0.0278(4) Uani 1 1 d . . . . .
C52 C 0.43174(12) 0.18134(16) 0.65192(8) 0.0428(5) Uani 1 1 d . . . . .
H52 H 0.419629 0.166049 0.618675 0.051 Uiso 1 1 calc R U . . .
C53 C 0.36963(13) 0.21147(16) 0.67756(9) 0.0482(6) Uani 1 1 d . . . . .
H53 H 0.315464 0.216342 0.661913 0.058 Uiso 1 1 calc R U . . .
C54 C 0.38626(13) 0.23444(14) 0.72580(9) 0.0422(5) Uani 1 1 d . . . . .
H54 H 0.343682 0.254327 0.743652 0.051 Uiso 1 1 calc R U . . .
C55 C 0.46497(14) 0.22820(15) 0.74765(8) 0.0411(5) Uani 1 1 d . . . . .
H55 H 0.476886 0.244993 0.780689 0.049 Uiso 1 1 calc R U . . .
C56 C 0.52786(12) 0.19757(13) 0.72210(7) 0.0338(4) Uani 1 1 d . . . . .
H56 H 0.582004 0.193573 0.737877 0.041 Uiso 1 1 calc R U . . .
C57 C 0.73735(14) -0.07553(14) 0.76867(9) 0.0463(5) Uani 1 1 d . . . . .
H57A H 0.680999 -0.061006 0.774038 0.069 Uiso 1 1 calc R U . . .
H57B H 0.759827 -0.118898 0.793024 0.069 Uiso 1 1 calc R U . . .
H57C H 0.737965 -0.101073 0.736206 0.069 Uiso 1 1 calc R U . . .
C58 C 0.79022(19) 0.04781(17) 0.82321(8) 0.0559(6) Uani 1 1 d . . . . .
H58A H 0.826533 0.099826 0.826036 0.084 Uiso 1 1 calc R U . . .
H58B H 0.810317 0.003041 0.847388 0.084 Uiso 1 1 calc R U . . .
H58C H 0.734872 0.066176 0.828762 0.084 Uiso 1 1 calc R U . . .
C59 C 0.79657(11) 0.37691(12) 0.73916(6) 0.0268(4) Uani 1 1 d . . . . .
C60 C 0.75671(12) 0.34817(13) 0.77779(7) 0.0335(4) Uani 1 1 d . . . . .
H60 H 0.749502 0.286089 0.782796 0.040 Uiso 1 1 calc R U . . .
C61 C 0.72722(15) 0.40915(16) 0.80924(8) 0.0472(5) Uani 1 1 d . . . . .
H61 H 0.699972 0.388380 0.835511 0.057 Uiso 1 1 calc R U . . .
C62 C 0.73704(17) 0.49922(17) 0.80277(10) 0.0570(7) Uani 1 1 d . . . . .
H62 H 0.716986 0.540589 0.824534 0.068 Uiso 1 1 calc R U . . .
C63 C 0.77629(17) 0.52918(16) 0.76436(11) 0.0575(7) Uani 1 1 d . . . . .
H63 H 0.783205 0.591359 0.759536 0.069 Uiso 1 1 calc R U . . .
C64 C 0.80554(14) 0.46840(14) 0.73292(9) 0.0416(5) Uani 1 1 d . . . . .
H64 H 0.832281 0.489573 0.706529 0.050 Uiso 1 1 calc R U . . .
C65 C 0.92422(11) 0.29944(11) 0.71511(6) 0.0249(3) Uani 1 1 d . . . . .
C66 C 0.96824(11) 0.32548(13) 0.75845(6) 0.0288(4) Uani 1 1 d . . . . .
H66 H 0.940882 0.354705 0.782386 0.035 Uiso 1 1 calc R U . . .
C67 C 1.05196(12) 0.30934(14) 0.76729(7) 0.0363(4) Uani 1 1 d . . . . .
H67 H 1.080926 0.327078 0.797286 0.044 Uiso 1 1 calc R U . . .
C68 C 1.09304(12) 0.26791(14) 0.73295(9) 0.0395(5) Uani 1 1 d . . . . .
H68 H 1.150031 0.256492 0.739130 0.047 Uiso 1 1 calc R U . . .
C69 C 1.05032(13) 0.24324(15) 0.68948(9) 0.0446(5) Uani 1 1 d . . . . .
H69 H 1.078239 0.215241 0.665391 0.054 Uiso 1 1 calc R U . . .
C70 C 0.96684(12) 0.25890(14) 0.68054(7) 0.0366(4) Uani 1 1 d . . . . .
H70 H 0.938412 0.241631 0.650307 0.044 Uiso 1 1 calc R U . . .
N1 N 0.57418(12) 0.48943(14) 0.64174(7) 0.0453(4) Uani 1 1 d D . . . .
C71 C 0.58643(15) 0.44116(17) 0.68881(8) 0.0476(6) Uani 1 1 d . . . . .
H71A H 0.645508 0.441542 0.700488 0.057 Uiso 1 1 calc R U . . .
H71B H 0.569851 0.378179 0.683176 0.057 Uiso 1 1 calc R U . . .
C72 C 0.5403(2) 0.4786(2) 0.72815(10) 0.0684(8) Uani 1 1 d . . . . .
H72A H 0.556138 0.540942 0.734231 0.103 Uiso 1 1 calc R U . . .
H72B H 0.553202 0.443793 0.757923 0.103 Uiso 1 1 calc R U . . .
H72C H 0.481396 0.475326 0.717906 0.103 Uiso 1 1 calc R U . . .
C73 C 0.4885(5) 0.5080(7) 0.6239(3) 0.058(2) Uani 0.602(18) 1 d D U P B 1
H73A H 0.485302 0.537419 0.591747 0.070 Uiso 0.602(18) 1 calc R U P B 1
H73B H 0.464286 0.548649 0.646526 0.070 Uiso 0.602(18) 1 calc R U P B 1
C74 C 0.4416(5) 0.4208(8) 0.6198(2) 0.086(3) Uani 0.602(18) 1 d . U P B 1
H74A H 0.462087 0.383429 0.594755 0.129 Uiso 0.602(18) 1 calc R U P B 1
H74B H 0.383340 0.432957 0.610917 0.129 Uiso 0.602(18) 1 calc R U P B 1
H74C H 0.449071 0.389507 0.650952 0.129 Uiso 0.602(18) 1 calc R U P B 1
C73' C 0.4888(7) 0.4781(11) 0.6145(7) 0.083(4) Uani 0.398(18) 1 d D U P B 2
H73C H 0.486588 0.510040 0.583129 0.100 Uiso 0.398(18) 1 calc R U P B 2
H73D H 0.448364 0.506142 0.633578 0.100 Uiso 0.398(18) 1 calc R U P B 2
C74' C 0.4639(6) 0.3782(8) 0.6044(9) 0.129(6) Uani 0.398(18) 1 d . U P B 2
H74D H 0.478855 0.360386 0.572612 0.193 Uiso 0.398(18) 1 calc R U P B 2
H74E H 0.404683 0.371763 0.604819 0.193 Uiso 0.398(18) 1 calc R U P B 2
H74F H 0.492449 0.340178 0.629561 0.193 Uiso 0.398(18) 1 calc R U P B 2
C75 C 0.6147(2) 0.58058(19) 0.64404(11) 0.0724(8) Uani 1 1 d . . . . .
H75A H 0.585383 0.620394 0.664716 0.087 Uiso 1 1 calc R U . . .
H75B H 0.671699 0.574500 0.659399 0.087 Uiso 1 1 calc R U . . .
C76 C 0.6155(2) 0.6223(2) 0.59550(12) 0.0742(9) Uani 1 1 d . . . . .
H76A H 0.639854 0.580783 0.573894 0.111 Uiso 1 1 calc R U . . .
H76B H 0.647729 0.677347 0.598602 0.111 Uiso 1 1 calc R U . . .
H76C H 0.559331 0.636138 0.581991 0.111 Uiso 1 1 calc R U . . .
H1N H 0.5975(16) 0.4529(18) 0.6174(10) 0.054(7) Uiso 1 1 d . . . . .
N2 N 0.7406(2) 0.7562(2) 0.67440(11) 0.0861(8) Uani 1 1 d . . . . .
C77 C 0.74540(17) 0.8038(2) 0.64316(13) 0.0632(7) Uani 1 1 d . . . . .
C78 C 0.7505(2) 0.8613(3) 0.60261(19) 0.1218(18) Uani 1 1 d . . . . .
H78A H 0.736769 0.827712 0.572513 0.183 Uiso 1 1 calc R U . . .
H78B H 0.806298 0.884732 0.603528 0.183 Uiso 1 1 calc R U . . .
H78C H 0.712120 0.910970 0.603948 0.183 Uiso 1 1 calc R U . . .
N3 N 0.61210(18) 0.2984(2) 0.34890(9) 0.0823(8) Uani 1 1 d . . . . .
C79 C 0.64236(13) 0.30016(14) 0.38707(8) 0.0408(5) Uani 1 1 d . . . . .
C80 C 0.68144(19) 0.3022(3) 0.43543(10) 0.0718(9) Uani 1 1 d . . . . .
H80A H 0.715900 0.249146 0.441363 0.108 Uiso 1 1 calc R U . . .
H80B H 0.639950 0.303010 0.458163 0.108 Uiso 1 1 calc R U . . .
H80C H 0.715399 0.355915 0.440078 0.108 Uiso 1 1 calc R U . . .
O5 O 0.48985(18) 0.2517(2) 0.51863(14) 0.1276(12) Uani 1 1 d D . . . .
H5O H 0.508(3) 0.291(4) 0.4936(16) 0.191 Uiso 1 1 d D U . . .
H5P H 0.5405(18) 0.240(4) 0.5389(17) 0.191 Uiso 1 1 d D U . . .
O6 O 0.54917(19) 0.4263(2) 0.49549(9) 0.1084(10) Uani 1 1 d D . . . .
H6O H 0.585(2) 0.402(3) 0.5223(12) 0.163 Uiso 1 1 d D U . . .
H6P H 0.565(3) 0.4901(10) 0.4982(18) 0.163 Uiso 1 1 d D 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 O4 1.4783(13) . ?
P1 O3 1.5013(13) . ?
P1 O2 1.5996(11) . ?
P1 O1 1.6165(12) . ?
O1 C1 1.4058(18) . ?
O2 C36 1.4042(19) . ?
C1 C2 1.400(2) . ?
C1 C6 1.402(2) . ?
C2 C3 1.396(2) . ?
C2 C9 1.523(2) . ?
C3 C4 1.385(2) . ?
C4 C5 1.392(2) . ?
C4 C8 1.515(2) . ?
C5 C6 1.396(2) . ?
C6 C7 1.534(2) . ?
C7 C16 1.523(2) . ?
C7 C10 1.533(2) . ?
C8 C23 1.527(3) . ?
C8 C22 1.533(3) . ?
C9 C30 1.532(2) . ?
C9 C24 1.539(2) . ?
C10 C11 1.384(3) . ?
C10 C15 1.395(3) . ?
C11 C12 1.392(3) . ?
C12 C13 1.379(3) . ?
C13 C14 1.379(3) . ?
C14 C15 1.388(3) . ?
C16 C21 1.389(3) . ?
C16 C17' 1.392(6) . ?
C16 C17 1.413(6) . ?
C17 C18 1.391(7) . ?
C18 C19 1.389(9) . ?
C19 C20 1.335(8) . ?
C17' C18' 1.387(7) . ?
C18' C19' 1.372(9) . ?
C19' C20 1.412(8) . ?
C20 C21 1.384(3) . ?
C24 C29 1.388(3) . ?
C24 C25 1.394(3) . ?
C25 C26 1.384(3) . ?
C26 C27 1.386(3) . ?
C27 C28 1.382(3) . ?
C28 C29 1.387(3) . ?
C30 C35 1.387(3) . ?
C30 C31 1.392(3) . ?
C31 C32 1.391(3) . ?
C32 C33 1.372(3) . ?
C33 C34 1.379(3) . ?
C34 C35 1.392(3) . ?
C36 C37 1.394(2) . ?
C36 C41 1.399(2) . ?
C37 C38 1.401(2) . ?
C37 C42 1.526(2) . ?
C38 C39 1.390(2) . ?
C39 C40 1.395(2) . ?
C39 C43 1.529(2) . ?
C40 C41 1.389(2) . ?
C41 C44 1.525(2) . ?
C42 C45 1.529(2) . ?
C42 C51 1.531(2) . ?
C43 C57 1.509(3) . ?
C43 C58 1.515(3) . ?
C44 C59 1.525(2) . ?
C44 C65 1.530(2) . ?
C45 C46 1.384(3) . ?
C45 C50 1.388(3) . ?
C46 C47 1.387(3) . ?
C47 C48 1.381(3) . ?
C48 C49 1.378(3) . ?
C49 C50 1.387(3) . ?
C51 C56 1.382(3) . ?
C51 C52 1.395(3) . ?
C52 C53 1.385(3) . ?
C53 C54 1.380(3) . ?
C54 C55 1.371(3) . ?
C55 C56 1.396(3) . ?
C59 C60 1.386(3) . ?
C59 C64 1.392(3) . ?
C60 C61 1.388(3) . ?
C61 C62 1.373(4) . ?
C62 C63 1.382(4) . ?
C63 C64 1.384(3) . ?
C65 C66 1.389(2) . ?
C65 C70 1.390(3) . ?
C66 C67 1.394(3) . ?
C67 C68 1.377(3) . ?
C68 C69 1.377(3) . ?
C69 C70 1.389(3) . ?
N1 C73 1.469(7) . ?
N1 C71 1.487(3) . ?
N1 C75 1.518(4) . ?
N1 C73' 1.530(13) . ?
C71 C72 1.506(3) . ?
C73 C74 1.516(11) . ?
C73' C74' 1.568(17) . ?
C75 C76 1.486(4) . ?
N2 C77 1.132(4) . ?
C77 C78 1.427(5) . ?
N3 C79 1.120(3) . ?
C79 C80 1.423(3) . ?

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
O4 P1 O3 118.20(7) . . ?
O4 P1 O2 113.55(7) . . ?
O3 P1 O2 103.02(7) . . ?
O4 P1 O1 110.25(7) . . ?
O3 P1 O1 110.40(7) . . ?
O2 P1 O1 99.71(6) . . ?
C1 O1 P1 122.00(10) . . ?
C36 O2 P1 126.83(10) . . ?
C2 C1 C6 122.50(14) . . ?
C2 C1 O1 119.34(14) . . ?
C6 C1 O1 118.07(14) . . ?
C3 C2 C1 117.36(15) . . ?
C3 C2 C9 119.55(14) . . ?
C1 C2 C9 123.07(14) . . ?
C4 C3 C2 122.34(15) . . ?
C3 C4 C5 118.31(15) . . ?
C3 C4 C8 120.63(15) . . ?
C5 C4 C8 120.97(15) . . ?
C4 C5 C6 122.29(15) . . ?
C5 C6 C1 117.18(14) . . ?
C5 C6 C7 121.60(14) . . ?
C1 C6 C7 121.21(14) . . ?
C16 C7 C6 112.82(14) . . ?
C16 C7 C10 110.23(14) . . ?
C6 C7 C10 114.13(14) . . ?
C4 C8 C23 112.79(16) . . ?
C4 C8 C22 109.51(16) . . ?
C23 C8 C22 109.81(17) . . ?
C2 C9 C30 112.47(14) . . ?
C2 C9 C24 111.55(13) . . ?
C30 C9 C24 111.33(14) . . ?
C11 C10 C15 118.02(17) . . ?
C11 C10 C7 123.81(16) . . ?
C15 C10 C7 118.16(16) . . ?
C10 C11 C12 121.11(19) . . ?
C13 C12 C11 120.1(2) . . ?
C12 C13 C14 119.55(19) . . ?
C13 C14 C15 120.27(19) . . ?
C14 C15 C10 120.9(2) . . ?
C21 C16 C17' 117.9(3) . . ?
C21 C16 C17 114.8(3) . . ?
C21 C16 C7 122.20(16) . . ?
C17' C16 C7 118.4(3) . . ?
C17 C16 C7 121.5(3) . . ?
C18 C17 C16 121.2(5) . . ?
C19 C18 C17 120.6(5) . . ?
C20 C19 C18 118.4(6) . . ?
C18' C17' C16 120.2(5) . . ?
C19' C18' C17' 120.6(5) . . ?
C18' C19' C20 120.3(6) . . ?
C19 C20 C21 121.7(4) . . ?
C21 C20 C19' 117.7(4) . . ?
C20 C21 C16 121.96(19) . . ?
C29 C24 C25 118.18(17) . . ?
C29 C24 C9 122.76(16) . . ?
C25 C24 C9 119.06(16) . . ?
C26 C25 C24 121.04(18) . . ?
C25 C26 C27 120.17(19) . . ?
C28 C27 C26 119.27(19) . . ?
C27 C28 C29 120.5(2) . . ?
C28 C29 C24 120.84(19) . . ?
C35 C30 C31 118.26(17) . . ?
C35 C30 C9 118.40(17) . . ?
C31 C30 C9 123.23(16) . . ?
C32 C31 C30 120.85(18) . . ?
C33 C32 C31 120.2(2) . . ?
C32 C33 C34 119.8(2) . . ?
C33 C34 C35 120.3(2) . . ?
C30 C35 C34 120.7(2) . . ?
C37 C36 C41 122.16(15) . . ?
C37 C36 O2 119.58(14) . . ?
C41 C36 O2 117.75(14) . . ?
C36 C37 C38 117.47(15) . . ?
C36 C37 C42 121.32(15) . . ?
C38 C37 C42 120.78(15) . . ?
C39 C38 C37 122.29(16) . . ?
C38 C39 C40 117.91(16) . . ?
C38 C39 C43 122.86(16) . . ?
C40 C39 C43 119.09(16) . . ?
C41 C40 C39 122.17(16) . . ?
C40 C41 C36 117.97(15) . . ?
C40 C41 C44 120.76(15) . . ?
C36 C41 C44 120.83(15) . . ?
C37 C42 C45 112.47(14) . . ?
C37 C42 C51 112.06(14) . . ?
C45 C42 C51 111.78(14) . . ?
C57 C43 C58 110.47(18) . . ?
C57 C43 C39 113.95(16) . . ?
C58 C43 C39 110.36(16) . . ?
C41 C44 C59 110.76(14) . . ?
C41 C44 C65 111.88(14) . . ?
C59 C44 C65 113.37(14) . . ?
C46 C45 C50 118.37(18) . . ?
C46 C45 C42 119.51(16) . . ?
C50 C45 C42 122.12(17) . . ?
C45 C46 C47 120.6(2) . . ?
C48 C47 C46 120.5(2) . . ?
C49 C48 C47 119.4(2) . . ?
C48 C49 C50 120.0(2) . . ?
C49 C50 C45 121.1(2) . . ?
C56 C51 C52 118.06(18) . . ?
C56 C51 C42 123.52(16) . . ?
C52 C51 C42 118.41(17) . . ?
C53 C52 C51 121.2(2) . . ?
C54 C53 C52 120.1(2) . . ?
C55 C54 C53 119.19(19) . . ?
C54 C55 C56 121.0(2) . . ?
C51 C56 C55 120.36(19) . . ?
C60 C59 C64 117.91(18) . . ?
C60 C59 C44 123.33(16) . . ?
C64 C59 C44 118.75(17) . . ?
C59 C60 C61 120.69(19) . . ?
C62 C61 C60 120.7(2) . . ?
C61 C62 C63 119.5(2) . . ?
C62 C63 C64 119.9(2) . . ?
C63 C64 C59 121.4(2) . . ?
C66 C65 C70 117.77(17) . . ?
C66 C65 C44 123.17(15) . . ?
C70 C65 C44 119.06(16) . . ?
C65 C66 C67 120.92(18) . . ?
C68 C67 C66 120.57(19) . . ?
C67 C68 C69 119.03(19) . . ?
C68 C69 C70 120.63(19) . . ?
C69 C70 C65 121.05(19) . . ?
C73 N1 C71 114.9(4) . . ?
C73 N1 C75 104.1(5) . . ?
C71 N1 C75 112.6(2) . . ?
C71 N1 C73' 114.1(6) . . ?
C75 N1 C73' 119.8(6) . . ?
N1 C71 C72 115.20(19) . . ?
N1 C73 C74 108.8(6) . . ?
N1 C73' C74' 113.7(11) . . ?
C76 C75 N1 112.8(2) . . ?
N2 C77 C78 178.0(4) . . ?
N3 C79 C80 179.5(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C71 H71B O2 0.99 2.65 3.133(2) 110.1 .
C73 H73A O6 0.99 2.48 3.445(8) 163.3 3_666
C73 H73B N3 0.99 2.62 3.464(10) 142.8 3_666
C73' H73C O6 0.99 2.39 3.366(17) 167.1 3_666
C74' H74D O5 0.98 2.23 3.11(3) 148.3 .
C74' H74D O6 0.98 2.73 3.55(2) 141.2 .
N1 H1N O3 0.98(3) 1.77(3) 2.739(2) 168(2) .
O5 H5O O6 0.979(10) 2.14(5) 2.890(5) 132(5) .
O5 H5P O4 0.969(10) 1.88(2) 2.792(3) 156(5) .
O6 H6O O3 0.970(10) 1.837(19) 2.765(2) 159(4) .

_refine_diff_density_max         0.770
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.055



####################################################################### 
# 
# 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_aj0390
_database_code_depnum_ccdc_archive 'CCDC 1843003'
_audit_update_record             
;
2018-07-30 deposited with the CCDC.
2018-09-26 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT220_aj0390              
;
PROBLEM: Non-Solvent  Resd 1  C   Ueq(max)/Ueq(min) Range        3.5 Ratio 
RESPONSE: The structure contains a large range of different carbon atoms 
(aromatic/rigid; solvent and tBu/flexible).
;
_vrf_PLAT244_aj0390              
;
PROBLEM: Low    'Solvent' Ueq as Compared to Neighbors of        C80 Check 
RESPONSE: This is the central carbon atom of a solvent acetonitrile. 
Its two neighbours appear to move sideways to some extent with the 
central carbon atom serving as pivot.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C70 H62 O4 P, C6 H16 N, 2(C2 H3 N)'
_chemical_formula_sum            'C80 H84 N3 O4 P'
_chemical_formula_weight         1182.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.4315(3)
_cell_length_b                   12.5478(3)
_cell_length_c                   22.9017(5)
_cell_angle_alpha                90.892(2)
_cell_angle_beta                 95.969(2)
_cell_angle_gamma                108.698(2)
_cell_volume                     3360.96(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    18969
_cell_measurement_theta_min      2.8190
_cell_measurement_theta_max      28.8870

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_F_000             1264
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.564
_exptl_crystal_size_mid          0.369
_exptl_crystal_size_min          0.207
_exptl_absorpt_coefficient_mu    0.093
_shelx_estimated_absorpt_T_min   0.949
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.61475
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            49656
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.638
_diffrn_reflns_theta_max         29.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             15378
_reflns_number_gt                12099
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0478P)²+0.6338P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15378
_refine_ls_number_parameters     806
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0432
_refine_ls_wR_factor_ref         0.1095
_refine_ls_wR_factor_gt          0.1029
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.20945(3) 0.18856(3) 0.72853(2) 0.01484(8) Uani 1 1 d . . . . .
O1 O 0.23745(7) 0.31408(7) 0.70559(4) 0.01613(18) Uani 1 1 d . . . . .
O2 O 0.26435(7) 0.22053(7) 0.79649(3) 0.01451(17) Uani 1 1 d . . . . .
O3 O 0.08246(7) 0.14471(7) 0.72554(4) 0.0211(2) Uani 1 1 d . . . . .
O4 O 0.26852(8) 0.12067(7) 0.69983(4) 0.02022(19) Uani 1 1 d . . . . .
C1 C 0.34766(10) 0.38724(10) 0.70022(5) 0.0162(2) Uani 1 1 d . . . . .
C2 C 0.39886(11) 0.37760(10) 0.64993(5) 0.0189(3) Uani 1 1 d . . . . .
C3 C 0.50625(11) 0.45457(11) 0.64447(5) 0.0222(3) Uani 1 1 d . . . . .
H3 H 0.542581 0.448441 0.610661 0.027 Uiso 1 1 calc R U . . .
C4 C 0.56161(11) 0.53993(11) 0.68704(5) 0.0221(3) Uani 1 1 d . . . . .
C5 C 0.50548(11) 0.54937(11) 0.73536(5) 0.0207(3) Uani 1 1 d . . . . .
H5 H 0.541801 0.608820 0.764171 0.025 Uiso 1 1 calc R U . . .
C6 C 0.39804(11) 0.47501(10) 0.74316(5) 0.0173(3) Uani 1 1 d . . . . .
C7 C 0.33742(11) 0.29094(11) 0.59999(5) 0.0196(3) Uani 1 1 d . . . . .
H7 H 0.286166 0.224980 0.618514 0.023 Uiso 1 1 calc R U . . .
C8 C 0.25965(11) 0.33331(11) 0.55701(5) 0.0213(3) Uani 1 1 d . . . . .
C9 C 0.25175(13) 0.44057(12) 0.56108(6) 0.0303(3) Uani 1 1 d . . . . .
H9 H 0.299491 0.493174 0.590820 0.036 Uiso 1 1 calc R U . . .
C10 C 0.17540(15) 0.47284(14) 0.52256(7) 0.0398(4) Uani 1 1 d . . . . .
H10 H 0.170649 0.546632 0.526494 0.048 Uiso 1 1 calc R U . . .
C11 C 0.10621(14) 0.39801(14) 0.47849(7) 0.0382(4) Uani 1 1 d . . . . .
H11 H 0.054039 0.420059 0.452040 0.046 Uiso 1 1 calc R U . . .
C12 C 0.11376(13) 0.29091(14) 0.47331(6) 0.0337(3) Uani 1 1 d . . . . .
H12 H 0.067060 0.239130 0.442962 0.040 Uiso 1 1 calc R U . . .
C13 C 0.18911(12) 0.25884(12) 0.51220(6) 0.0278(3) Uani 1 1 d . . . . .
H13 H 0.193007 0.184708 0.508373 0.033 Uiso 1 1 calc R U . . .
C14 C 0.42103(11) 0.24754(11) 0.57069(6) 0.0237(3) Uani 1 1 d . . . . .
C15 C 0.46282(13) 0.28727(14) 0.51832(6) 0.0349(4) Uani 1 1 d . . . . .
H15 H 0.439108 0.344085 0.499304 0.042 Uiso 1 1 calc R U . . .
C16 C 0.53908(15) 0.24437(17) 0.49363(7) 0.0458(4) Uani 1 1 d . . . . .
H16 H 0.567424 0.272286 0.457990 0.055 Uiso 1 1 calc R U . . .
C17 C 0.57356(15) 0.16162(16) 0.52067(8) 0.0472(5) Uani 1 1 d . . . . .
H17 H 0.623960 0.130983 0.503193 0.057 Uiso 1 1 calc R U . . .
C18 C 0.53462(14) 0.12326(15) 0.57334(8) 0.0425(4) Uani 1 1 d . . . . .
H18 H 0.559418 0.067189 0.592472 0.051 Uiso 1 1 calc R U . . .
C19 C 0.45940(12) 0.16657(12) 0.59825(7) 0.0313(3) Uani 1 1 d . . . . .
H19 H 0.433768 0.140457 0.634701 0.038 Uiso 1 1 calc R U . . .
C20 C 0.67941(11) 0.62175(12) 0.68057(6) 0.0268(3) Uani 1 1 d . . . . .
H20 H 0.712997 0.659256 0.720169 0.032 Uiso 1 1 calc R U . . .
C21 C 0.67241(14) 0.71367(13) 0.63894(7) 0.0369(4) Uani 1 1 d . . . . .
H21A H 0.644763 0.680096 0.599043 0.055 Uiso 1 1 calc R U . . .
H21B H 0.748424 0.769700 0.639148 0.055 Uiso 1 1 calc R U . . .
H21C H 0.619530 0.750239 0.651898 0.055 Uiso 1 1 calc R U . . .
C22 C 0.76004(12) 0.56308(14) 0.66051(7) 0.0358(4) Uani 1 1 d . . . . .
H22A H 0.762467 0.502966 0.686914 0.054 Uiso 1 1 calc R U . . .
H22B H 0.836909 0.617827 0.661322 0.054 Uiso 1 1 calc R U . . .
H22C H 0.732674 0.530660 0.620384 0.054 Uiso 1 1 calc R U . . .
C23 C 0.33528(11) 0.48700(10) 0.79557(5) 0.0179(3) Uani 1 1 d . . . . .
H23 H 0.312030 0.411831 0.813323 0.021 Uiso 1 1 calc R U . . .
C24 C 0.41003(10) 0.57156(10) 0.84400(5) 0.0173(2) Uani 1 1 d . . . . .
C25 C 0.45121(11) 0.53442(11) 0.89572(6) 0.0233(3) Uani 1 1 d . . . . .
H25 H 0.434989 0.455923 0.900344 0.028 Uiso 1 1 calc R U . . .
C26 C 0.51592(12) 0.61070(12) 0.94087(6) 0.0294(3) Uani 1 1 d . . . . .
H26 H 0.542790 0.583951 0.976187 0.035 Uiso 1 1 calc R U . . .
C27 C 0.54129(11) 0.72511(12) 0.93460(6) 0.0276(3) Uani 1 1 d . . . . .
H27 H 0.584811 0.777111 0.965624 0.033 Uiso 1 1 calc R U . . .
C28 C 0.50293(12) 0.76340(11) 0.88291(6) 0.0259(3) Uani 1 1 d . . . . .
H28 H 0.521973 0.842045 0.877901 0.031 Uiso 1 1 calc R U . . .
C29 C 0.43673(11) 0.68742(11) 0.83830(6) 0.0229(3) Uani 1 1 d . . . . .
H29 H 0.409135 0.714658 0.803325 0.028 Uiso 1 1 calc R U . . .
C30 C 0.22540(11) 0.51519(10) 0.77888(6) 0.0202(3) Uani 1 1 d . . . . .
C31 C 0.19883(12) 0.55526(11) 0.72486(6) 0.0250(3) Uani 1 1 d . . . . .
H31 H 0.248682 0.563126 0.695292 0.030 Uiso 1 1 calc R U . . .
C32 C 0.09946(13) 0.58394(12) 0.71387(7) 0.0309(3) Uani 1 1 d . . . . .
H32 H 0.081361 0.610218 0.676648 0.037 Uiso 1 1 calc R U . . .
C33 C 0.02716(12) 0.57436(12) 0.75680(7) 0.0342(3) Uani 1 1 d . . . . .
H33 H -0.039709 0.595406 0.749387 0.041 Uiso 1 1 calc R U . . .
C34 C 0.05236(12) 0.53399(13) 0.81071(7) 0.0349(4) Uani 1 1 d . . . . .
H34 H 0.002675 0.527055 0.840291 0.042 Uiso 1 1 calc R U . . .
C35 C 0.15010(12) 0.50379(12) 0.82135(6) 0.0276(3) Uani 1 1 d . . . . .
H35 H 0.166215 0.474844 0.858122 0.033 Uiso 1 1 calc R U . . .
C36 C 0.27706(10) 0.13802(9) 0.83470(5) 0.0133(2) Uani 1 1 d . . . . .
C37 C 0.37886(10) 0.11246(10) 0.83967(5) 0.0146(2) Uani 1 1 d . . . . .
C38 C 0.38965(10) 0.03291(10) 0.87994(5) 0.0166(2) Uani 1 1 d . . . . .
H38 H 0.457904 0.013669 0.883598 0.020 Uiso 1 1 calc R U . . .
C39 C 0.30467(10) -0.01925(10) 0.91487(5) 0.0166(2) Uani 1 1 d . . . . .
C40 C 0.20558(10) 0.01046(10) 0.90886(5) 0.0164(2) Uani 1 1 d . . . . .
H40 H 0.147015 -0.023399 0.932772 0.020 Uiso 1 1 calc R U . . .
C41 C 0.18924(10) 0.08829(10) 0.86891(5) 0.0144(2) Uani 1 1 d . . . . .
C42 C 0.47522(10) 0.16987(10) 0.80321(5) 0.0157(2) Uani 1 1 d . . . . .
H42 H 0.439341 0.192198 0.766326 0.019 Uiso 1 1 calc R U . . .
C43 C 0.56034(10) 0.27695(10) 0.83362(5) 0.0162(2) Uani 1 1 d . . . . .
C44 C 0.62403(11) 0.35867(11) 0.79915(6) 0.0226(3) Uani 1 1 d . . . . .
H44 H 0.609498 0.348920 0.757532 0.027 Uiso 1 1 calc R U . . .
C45 C 0.70850(12) 0.45422(12) 0.82472(6) 0.0277(3) Uani 1 1 d . . . . .
H45 H 0.751221 0.509176 0.800541 0.033 Uiso 1 1 calc R U . . .
C46 C 0.73078(12) 0.46983(11) 0.88527(6) 0.0258(3) Uani 1 1 d . . . . .
H46 H 0.789504 0.534609 0.902741 0.031 Uiso 1 1 calc R U . . .
C47 C 0.66667(12) 0.39010(11) 0.92023(6) 0.0247(3) Uani 1 1 d . . . . .
H47 H 0.680712 0.400792 0.961832 0.030 Uiso 1 1 calc R U . . .
C48 C 0.58193(11) 0.29461(11) 0.89455(6) 0.0206(3) Uani 1 1 d . . . . .
H48 H 0.538150 0.240657 0.918840 0.025 Uiso 1 1 calc R U . . .
C49 C 0.53393(10) 0.08646(10) 0.78502(5) 0.0167(2) Uani 1 1 d . . . . .
C50 C 0.63478(10) 0.08126(11) 0.81571(5) 0.0191(3) Uani 1 1 d . . . . .
H50 H 0.672812 0.135258 0.846911 0.023 Uiso 1 1 calc R U . . .
C51 C 0.68039(11) -0.00191(11) 0.80123(6) 0.0233(3) Uani 1 1 d . . . . .
H51 H 0.748610 -0.005161 0.822905 0.028 Uiso 1 1 calc R U . . .
C52 C 0.62680(12) -0.08001(12) 0.75535(6) 0.0272(3) Uani 1 1 d . . . . .
H52 H 0.657686 -0.137253 0.745630 0.033 Uiso 1 1 calc R U . . .
C53 C 0.52775(13) -0.07432(12) 0.72361(6) 0.0286(3) Uani 1 1 d . . . . .
H53 H 0.491496 -0.126938 0.691579 0.034 Uiso 1 1 calc R U . . .
C54 C 0.48145(11) 0.00778(11) 0.73842(6) 0.0232(3) Uani 1 1 d . . . . .
H54 H 0.413181 0.010596 0.716607 0.028 Uiso 1 1 calc R U . . .
C55 C 0.31689(11) -0.10904(11) 0.95613(6) 0.0215(3) Uani 1 1 d . . . . .
H55 H 0.395913 -0.112919 0.955743 0.026 Uiso 1 1 calc R U . . .
C56 C 0.30328(14) -0.08021(13) 1.01938(6) 0.0332(3) Uani 1 1 d . . . . .
H56A H 0.358907 -0.006546 1.032432 0.050 Uiso 1 1 calc R U . . .
H56B H 0.316470 -0.137782 1.044933 0.050 Uiso 1 1 calc R U . . .
H56C H 0.225728 -0.077779 1.021377 0.050 Uiso 1 1 calc R U . . .
C57 C 0.23329(14) -0.22421(12) 0.93471(7) 0.0361(4) Uani 1 1 d . . . . .
H57A H 0.154813 -0.223534 0.935382 0.054 Uiso 1 1 calc R U . . .
H57B H 0.246265 -0.281556 0.960495 0.054 Uiso 1 1 calc R U . . .
H57C H 0.244970 -0.241658 0.894468 0.054 Uiso 1 1 calc R U . . .
C58 C 0.07795(10) 0.11624(10) 0.86276(5) 0.0155(2) Uani 1 1 d . . . . .
H58 H 0.067812 0.140640 0.821766 0.019 Uiso 1 1 calc R U . . .
C59 C -0.02115(10) 0.00872(10) 0.86747(5) 0.0177(3) Uani 1 1 d . . . . .
C60 C -0.05661(11) -0.06738(11) 0.81869(6) 0.0250(3) Uani 1 1 d . . . . .
H60 H -0.024771 -0.047218 0.782894 0.030 Uiso 1 1 calc R U . . .
C61 C -0.13765(12) -0.17180(12) 0.82202(8) 0.0357(4) Uani 1 1 d . . . . .
H61 H -0.159478 -0.223684 0.788866 0.043 Uiso 1 1 calc R U . . .
C62 C -0.18722(12) -0.20131(12) 0.87336(8) 0.0392(4) Uani 1 1 d . . . . .
H62 H -0.243439 -0.272856 0.875400 0.047 Uiso 1 1 calc R U . . .
C63 C -0.15421(12) -0.12575(12) 0.92167(7) 0.0334(3) Uani 1 1 d . . . . .
H63 H -0.188413 -0.145140 0.956908 0.040 Uiso 1 1 calc R U . . .
C64 C -0.07115(11) -0.02156(11) 0.91875(6) 0.0225(3) Uani 1 1 d . . . . .
H64 H -0.048355 0.029492 0.952258 0.027 Uiso 1 1 calc R U . . .
C65 C 0.08075(10) 0.21451(10) 0.90380(5) 0.0171(2) Uani 1 1 d . . . . .
C66 C 0.17958(11) 0.27814(11) 0.93872(6) 0.0219(3) Uani 1 1 d . . . . .
H66 H 0.247326 0.258515 0.938865 0.026 Uiso 1 1 calc R U . . .
C67 C 0.18009(13) 0.37030(12) 0.97345(6) 0.0301(3) Uani 1 1 d . . . . .
H67 H 0.248160 0.413139 0.997114 0.036 Uiso 1 1 calc R U . . .
C68 C 0.08236(13) 0.39991(12) 0.97375(7) 0.0313(3) Uani 1 1 d . . . . .
H68 H 0.082952 0.462717 0.997645 0.038 Uiso 1 1 calc R U . . .
C69 C -0.01633(12) 0.33767(12) 0.93911(6) 0.0289(3) Uani 1 1 d . . . . .
H69 H -0.083826 0.357694 0.939138 0.035 Uiso 1 1 calc R U . . .
C70 C -0.01699(11) 0.24596(11) 0.90429(6) 0.0226(3) Uani 1 1 d . . . . .
H70 H -0.085107 0.203960 0.880403 0.027 Uiso 1 1 calc R U . . .
N1 N -0.08493(10) 0.17575(10) 0.65693(5) 0.0261(3) Uani 1 1 d . . . . .
C71 C -0.03338(13) 0.28008(13) 0.62559(7) 0.0346(3) Uani 1 1 d . . . . .
H71A H 0.027035 0.269152 0.603560 0.042 Uiso 1 1 calc R U . . .
H71B H 0.003442 0.343226 0.655080 0.042 Uiso 1 1 calc R U . . .
C72 C -0.11841(19) 0.3122(2) 0.58325(10) 0.0673(6) Uani 1 1 d . . . . .
H72A H -0.152424 0.251897 0.552599 0.101 Uiso 1 1 calc R U . . .
H72B H -0.079172 0.382190 0.565145 0.101 Uiso 1 1 calc R U . . .
H72C H -0.178678 0.323216 0.604609 0.101 Uiso 1 1 calc R U . . .
C73 C -0.13364(15) 0.06964(15) 0.61793(8) 0.0461(4) Uani 1 1 d . . . . .
H73A H -0.164140 0.005155 0.642614 0.055 Uiso 1 1 calc R U . . .
H73B H -0.198196 0.076076 0.590638 0.055 Uiso 1 1 calc R U . . .
C74 C -0.04770(18) 0.04616(16) 0.58284(8) 0.0546(5) Uani 1 1 d . . . . .
H74A H -0.027109 0.102791 0.553362 0.082 Uiso 1 1 calc R U . . .
H74B H -0.080635 -0.028920 0.563099 0.082 Uiso 1 1 calc R U . . .
H74C H 0.020810 0.049253 0.609106 0.082 Uiso 1 1 calc R U . . .
C75 C -0.17244(13) 0.18408(14) 0.69550(7) 0.0375(4) Uani 1 1 d . . . . .
H75A H -0.238152 0.194356 0.670688 0.045 Uiso 1 1 calc R U . . .
H75B H -0.200656 0.112478 0.715326 0.045 Uiso 1 1 calc R U . . .
C76 C -0.12697(15) 0.27916(15) 0.74109(8) 0.0452(4) Uani 1 1 d . . . . .
H76A H -0.054313 0.277023 0.761342 0.068 Uiso 1 1 calc R U . . .
H76B H -0.182124 0.271789 0.769630 0.068 Uiso 1 1 calc R U . . .
H76C H -0.114678 0.350940 0.722151 0.068 Uiso 1 1 calc R U . . .
H1N H -0.0208(15) 0.1660(13) 0.6826(7) 0.037(4) Uiso 1 1 d . . . . .
N2 N 0.00284(12) 0.83148(11) 0.67473(6) 0.0407(3) Uani 1 1 d . . . . .
C77 C 0.07684(13) 0.84442(12) 0.71077(7) 0.0292(3) Uani 1 1 d . . . . .
C79 C 0.17159(13) 0.86146(13) 0.75665(7) 0.0359(4) Uani 1 1 d . . . . .
H79A H 0.216924 0.813668 0.747345 0.054 Uiso 1 1 calc R U . . .
H79B H 0.141840 0.841533 0.794392 0.054 Uiso 1 1 calc R U . . .
H79C H 0.219907 0.940681 0.759150 0.054 Uiso 1 1 calc R U . . .
N3 N 0.7390(2) 0.2394(2) 0.39265(10) 0.0937(7) Uani 1 1 d . . . . .
C80 C 0.76329(18) 0.16116(18) 0.40337(8) 0.0520(5) Uani 1 1 d . . . . .
C81 C 0.79352(15) 0.06160(14) 0.41730(7) 0.0433(4) Uani 1 1 d . . . . .
H81A H 0.745378 0.019895 0.446142 0.065 Uiso 1 1 calc R U . . .
H81B H 0.874024 0.083859 0.433741 0.065 Uiso 1 1 calc R U . . .
H81C H 0.781643 0.013602 0.381472 0.065 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 O4 1.4769(9) . ?
P1 O3 1.4896(9) . ?
P1 O1 1.6095(9) . ?
P1 O2 1.6227(8) . ?
O1 C1 1.4026(14) . ?
O2 C36 1.4023(14) . ?
C1 C2 1.3941(17) . ?
C1 C6 1.4030(17) . ?
C2 C3 1.3938(18) . ?
C2 C7 1.5235(16) . ?
C3 C4 1.3880(18) . ?
C3 H3 0.9500 . ?
C4 C5 1.3911(18) . ?
C4 C20 1.5187(18) . ?
C5 C6 1.3935(18) . ?
C5 H5 0.9500 . ?
C6 C23 1.5286(17) . ?
C7 C14 1.5243(18) . ?
C7 C8 1.5278(18) . ?
C7 H7 1.0000 . ?
C8 C9 1.383(2) . ?
C8 C13 1.3975(18) . ?
C9 C10 1.388(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.383(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.381(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.383(2) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C19 1.388(2) . ?
C14 C15 1.392(2) . ?
C15 C16 1.392(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.377(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.382(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.387(2) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C22 1.522(2) . ?
C20 C21 1.526(2) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.5284(17) . ?
C23 C30 1.5305(18) . ?
C23 H23 1.0000 . ?
C24 C25 1.3879(18) . ?
C24 C29 1.3951(18) . ?
C25 C26 1.3911(19) . ?
C25 H25 0.9500 . ?
C26 C27 1.381(2) . ?
C26 H26 0.9500 . ?
C27 C28 1.381(2) . ?
C27 H27 0.9500 . ?
C28 C29 1.3862(19) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 C31 1.3904(19) . ?
C30 C35 1.3965(19) . ?
C31 C32 1.394(2) . ?
C31 H31 0.9500 . ?
C32 C33 1.381(2) . ?
C32 H32 0.9500 . ?
C33 C34 1.385(2) . ?
C33 H33 0.9500 . ?
C34 C35 1.384(2) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.3959(16) . ?
C36 C41 1.3969(17) . ?
C37 C38 1.3978(17) . ?
C37 C42 1.5248(16) . ?
C38 C39 1.3903(17) . ?
C38 H38 0.9500 . ?
C39 C40 1.3914(17) . ?
C39 C55 1.5161(17) . ?
C40 C41 1.3958(17) . ?
C40 H40 0.9500 . ?
C41 C58 1.5261(16) . ?
C42 C43 1.5218(17) . ?
C42 C49 1.5300(17) . ?
C42 H42 1.0000 . ?
C43 C44 1.3915(18) . ?
C43 C48 1.3937(17) . ?
C44 C45 1.3878(19) . ?
C44 H44 0.9500 . ?
C45 C46 1.384(2) . ?
C45 H45 0.9500 . ?
C46 C47 1.387(2) . ?
C46 H46 0.9500 . ?
C47 C48 1.3897(18) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C49 C50 1.3931(17) . ?
C49 C54 1.3961(17) . ?
C50 C51 1.3886(18) . ?
C50 H50 0.9500 . ?
C51 C52 1.3828(19) . ?
C51 H51 0.9500 . ?
C52 C53 1.386(2) . ?
C52 H52 0.9500 . ?
C53 C54 1.3847(19) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
C55 C57 1.522(2) . ?
C55 C56 1.5270(19) . ?
C55 H55 1.0000 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 C59 1.5219(17) . ?
C58 C65 1.5281(16) . ?
C58 H58 1.0000 . ?
C59 C64 1.3873(18) . ?
C59 C60 1.3959(18) . ?
C60 C61 1.382(2) . ?
C60 H60 0.9500 . ?
C61 C62 1.385(2) . ?
C61 H61 0.9500 . ?
C62 C63 1.384(2) . ?
C62 H62 0.9500 . ?
C63 C64 1.390(2) . ?
C63 H63 0.9500 . ?
C64 H64 0.9500 . ?
C65 C66 1.3904(18) . ?
C65 C70 1.3937(18) . ?
C66 C67 1.3912(19) . ?
C66 H66 0.9500 . ?
C67 C68 1.380(2) . ?
C67 H67 0.9500 . ?
C68 C69 1.381(2) . ?
C68 H68 0.9500 . ?
C69 C70 1.3872(19) . ?
C69 H69 0.9500 . ?
C70 H70 0.9500 . ?
N1 C71 1.4921(19) . ?
N1 C75 1.4984(19) . ?
N1 C73 1.507(2) . ?
N1 H1N 0.981(17) . ?
C71 C72 1.514(2) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 C74 1.499(3) . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 C76 1.496(2) . ?
C75 H75A 0.9900 . ?
C75 H75B 0.9900 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
N2 C77 1.1384(19) . ?
C77 C79 1.453(2) . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
N3 C80 1.139(3) . ?
C80 C81 1.446(3) . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 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
O4 P1 O3 118.70(5) . . ?
O4 P1 O1 113.38(5) . . ?
O3 P1 O1 104.69(5) . . ?
O4 P1 O2 109.98(5) . . ?
O3 P1 O2 109.51(5) . . ?
O1 P1 O2 98.63(4) . . ?
C1 O1 P1 124.63(7) . . ?
C36 O2 P1 121.60(7) . . ?
C2 C1 O1 119.30(10) . . ?
C2 C1 C6 121.99(11) . . ?
O1 C1 C6 118.41(11) . . ?
C3 C2 C1 118.16(11) . . ?
C3 C2 C7 119.98(11) . . ?
C1 C2 C7 121.74(11) . . ?
C4 C3 C2 121.85(12) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C5 118.13(12) . . ?
C3 C4 C20 120.91(12) . . ?
C5 C4 C20 120.96(11) . . ?
C4 C5 C6 122.57(11) . . ?
C4 C5 H5 118.7 . . ?
C6 C5 H5 118.7 . . ?
C5 C6 C1 117.19(11) . . ?
C5 C6 C23 122.53(11) . . ?
C1 C6 C23 120.28(11) . . ?
C2 C7 C14 111.31(10) . . ?
C2 C7 C8 112.19(10) . . ?
C14 C7 C8 113.90(10) . . ?
C2 C7 H7 106.3 . . ?
C14 C7 H7 106.3 . . ?
C8 C7 H7 106.3 . . ?
C9 C8 C13 117.67(13) . . ?
C9 C8 C7 123.68(11) . . ?
C13 C8 C7 118.61(12) . . ?
C8 C9 C10 121.27(13) . . ?
C8 C9 H9 119.4 . . ?
C10 C9 H9 119.4 . . ?
C11 C10 C9 120.27(15) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C12 C11 C10 119.30(14) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C11 C12 C13 120.17(13) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C12 C13 C8 121.31(14) . . ?
C12 C13 H13 119.3 . . ?
C8 C13 H13 119.3 . . ?
C19 C14 C15 118.47(13) . . ?
C19 C14 C7 118.42(12) . . ?
C15 C14 C7 123.09(13) . . ?
C16 C15 C14 120.50(16) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C17 C16 C15 120.22(16) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 119.81(15) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C17 C18 C19 120.03(16) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C18 C19 C14 120.92(15) . . ?
C18 C19 H19 119.5 . . ?
C14 C19 H19 119.5 . . ?
C4 C20 C22 112.56(12) . . ?
C4 C20 C21 111.43(12) . . ?
C22 C20 C21 110.07(12) . . ?
C4 C20 H20 107.5 . . ?
C22 C20 H20 107.5 . . ?
C21 C20 H20 107.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C6 113.67(10) . . ?
C24 C23 C30 109.05(10) . . ?
C6 C23 C30 113.91(10) . . ?
C24 C23 H23 106.6 . . ?
C6 C23 H23 106.6 . . ?
C30 C23 H23 106.6 . . ?
C25 C24 C29 118.12(11) . . ?
C25 C24 C23 120.44(11) . . ?
C29 C24 C23 121.42(11) . . ?
C24 C25 C26 120.84(12) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C27 C26 C25 120.31(13) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C26 C27 C28 119.52(12) . . ?
C26 C27 H27 120.2 . . ?
C28 C27 H27 120.2 . . ?
C27 C28 C29 120.21(13) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C28 C29 C24 120.98(12) . . ?
C28 C29 H29 119.5 . . ?
C24 C29 H29 119.5 . . ?
C31 C30 C35 118.53(13) . . ?
C31 C30 C23 123.69(12) . . ?
C35 C30 C23 117.74(12) . . ?
C30 C31 C32 120.34(13) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C33 C32 C31 120.35(14) . . ?
C33 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C32 C33 C34 119.86(14) . . ?
C32 C33 H33 120.1 . . ?
C34 C33 H33 120.1 . . ?
C35 C34 C33 119.83(14) . . ?
C35 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C34 C35 C30 121.05(14) . . ?
C34 C35 H35 119.5 . . ?
C30 C35 H35 119.5 . . ?
C37 C36 C41 122.10(11) . . ?
C37 C36 O2 119.27(10) . . ?
C41 C36 O2 118.54(10) . . ?
C36 C37 C38 117.38(11) . . ?
C36 C37 C42 121.46(10) . . ?
C38 C37 C42 121.16(10) . . ?
C39 C38 C37 122.75(11) . . ?
C39 C38 H38 118.6 . . ?
C37 C38 H38 118.6 . . ?
C38 C39 C40 117.60(11) . . ?
C38 C39 C55 121.39(11) . . ?
C40 C39 C55 120.96(11) . . ?
C39 C40 C41 122.29(11) . . ?
C39 C40 H40 118.9 . . ?
C41 C40 H40 118.9 . . ?
C40 C41 C36 117.87(10) . . ?
C40 C41 C58 120.49(11) . . ?
C36 C41 C58 121.64(10) . . ?
C43 C42 C37 113.04(10) . . ?
C43 C42 C49 111.95(10) . . ?
C37 C42 C49 110.26(10) . . ?
C43 C42 H42 107.1 . . ?
C37 C42 H42 107.1 . . ?
C49 C42 H42 107.1 . . ?
C44 C43 C48 118.27(11) . . ?
C44 C43 C42 118.54(11) . . ?
C48 C43 C42 123.10(11) . . ?
C45 C44 C43 120.92(12) . . ?
C45 C44 H44 119.5 . . ?
C43 C44 H44 119.5 . . ?
C46 C45 C44 120.32(13) . . ?
C46 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
C45 C46 C47 119.45(12) . . ?
C45 C46 H46 120.3 . . ?
C47 C46 H46 120.3 . . ?
C46 C47 C48 120.14(12) . . ?
C46 C47 H47 119.9 . . ?
C48 C47 H47 119.9 . . ?
C47 C48 C43 120.87(12) . . ?
C47 C48 H48 119.6 . . ?
C43 C48 H48 119.6 . . ?
C50 C49 C54 118.36(11) . . ?
C50 C49 C42 122.29(11) . . ?
C54 C49 C42 119.22(11) . . ?
C51 C50 C49 120.79(12) . . ?
C51 C50 H50 119.6 . . ?
C49 C50 H50 119.6 . . ?
C52 C51 C50 120.18(12) . . ?
C52 C51 H51 119.9 . . ?
C50 C51 H51 119.9 . . ?
C51 C52 C53 119.63(12) . . ?
C51 C52 H52 120.2 . . ?
C53 C52 H52 120.2 . . ?
C54 C53 C52 120.25(13) . . ?
C54 C53 H53 119.9 . . ?
C52 C53 H53 119.9 . . ?
C53 C54 C49 120.76(12) . . ?
C53 C54 H54 119.6 . . ?
C49 C54 H54 119.6 . . ?
C39 C55 C57 110.92(11) . . ?
C39 C55 C56 112.09(11) . . ?
C57 C55 C56 110.98(12) . . ?
C39 C55 H55 107.5 . . ?
C57 C55 H55 107.5 . . ?
C56 C55 H55 107.5 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C55 C57 H57A 109.5 . . ?
C55 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C55 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C59 C58 C41 108.85(10) . . ?
C59 C58 C65 114.52(10) . . ?
C41 C58 C65 113.46(10) . . ?
C59 C58 H58 106.5 . . ?
C41 C58 H58 106.5 . . ?
C65 C58 H58 106.5 . . ?
C64 C59 C60 118.59(12) . . ?
C64 C59 C58 123.62(11) . . ?
C60 C59 C58 117.56(11) . . ?
C61 C60 C59 120.57(14) . . ?
C61 C60 H60 119.7 . . ?
C59 C60 H60 119.7 . . ?
C60 C61 C62 120.44(14) . . ?
C60 C61 H61 119.8 . . ?
C62 C61 H61 119.8 . . ?
C63 C62 C61 119.47(14) . . ?
C63 C62 H62 120.3 . . ?
C61 C62 H62 120.3 . . ?
C62 C63 C64 120.16(15) . . ?
C62 C63 H63 119.9 . . ?
C64 C63 H63 119.9 . . ?
C59 C64 C63 120.74(13) . . ?
C59 C64 H64 119.6 . . ?
C63 C64 H64 119.6 . . ?
C66 C65 C70 118.30(11) . . ?
C66 C65 C58 122.27(11) . . ?
C70 C65 C58 119.34(11) . . ?
C65 C66 C67 120.57(12) . . ?
C65 C66 H66 119.7 . . ?
C67 C66 H66 119.7 . . ?
C68 C67 C66 120.43(13) . . ?
C68 C67 H67 119.8 . . ?
C66 C67 H67 119.8 . . ?
C67 C68 C69 119.61(13) . . ?
C67 C68 H68 120.2 . . ?
C69 C68 H68 120.2 . . ?
C68 C69 C70 120.09(13) . . ?
C68 C69 H69 120.0 . . ?
C70 C69 H69 120.0 . . ?
C69 C70 C65 121.00(12) . . ?
C69 C70 H70 119.5 . . ?
C65 C70 H70 119.5 . . ?
C71 N1 C75 114.19(12) . . ?
C71 N1 C73 114.85(12) . . ?
C75 N1 C73 109.11(12) . . ?
C71 N1 H1N 104.8(10) . . ?
C75 N1 H1N 107.3(10) . . ?
C73 N1 H1N 105.9(9) . . ?
N1 C71 C72 113.94(14) . . ?
N1 C71 H71A 108.8 . . ?
C72 C71 H71A 108.8 . . ?
N1 C71 H71B 108.8 . . ?
C72 C71 H71B 108.8 . . ?
H71A C71 H71B 107.7 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C74 C73 N1 113.20(14) . . ?
C74 C73 H73A 108.9 . . ?
N1 C73 H73A 108.9 . . ?
C74 C73 H73B 108.9 . . ?
N1 C73 H73B 108.9 . . ?
H73A C73 H73B 107.8 . . ?
C73 C74 H74A 109.5 . . ?
C73 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C73 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C76 C75 N1 113.03(13) . . ?
C76 C75 H75A 109.0 . . ?
N1 C75 H75A 109.0 . . ?
C76 C75 H75B 109.0 . . ?
N1 C75 H75B 109.0 . . ?
H75A C75 H75B 107.8 . . ?
C75 C76 H76A 109.5 . . ?
C75 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C75 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
N2 C77 C79 179.7(2) . . ?
C77 C79 H79A 109.5 . . ?
C77 C79 H79B 109.5 . . ?
H79A C79 H79B 109.5 . . ?
C77 C79 H79C 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
N3 C80 C81 179.6(2) . . ?
C80 C81 H81A 109.5 . . ?
C80 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
C80 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1N O3 0.981(17) 1.629(17) 2.6095(14) 177.7(16) .
C79 H79C O4 0.98 2.59 3.4159(19) 142.1 1_565
C81 H81C O4 0.98 2.38 3.3571(18) 172.1 2_656

_refine_diff_density_max         0.368
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.044



