# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lcycage3poh
_audit_block_doi                 10.5517/ccdc.csd.cc28gn7n
_database_code_depnum_ccdc_archive 'CCDC 2099451'
loop_
_audit_author_name
_audit_author_address
lcycagepoh
;ecole centrale de marseille
France
;
_audit_update_record             
;
2021-07-26 deposited with the CCDC.	2022-02-03 downloaded from the CCDC.
;
_audit_creation_date             2021-07-26
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.6(Br), C60 H65.6 N4 O10 P, C H Cl3'
_chemical_formula_sum            'C61 H66.60 Br0.60 Cl3 N4 O10 P'
_chemical_formula_weight         1201.04
_chemical_melting_point          ?
_chemical_oxdiff_formula         'c60 h71 n4 o10 p1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   12.4213(8)
_cell_length_b                   29.5258(19)
_cell_length_c                   17.9736(8)
_cell_angle_alpha                90
_cell_angle_beta                 102.414(6)
_cell_angle_gamma                90
_cell_volume                     6437.7(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5317
_cell_measurement_temperature    153.01(10)
_cell_measurement_theta_max      70.2570
_cell_measurement_theta_min      2.9310
_shelx_estimated_absorpt_T_max   0.909
_shelx_estimated_absorpt_T_min   0.698
_exptl_absorpt_coefficient_mu    2.419
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
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    1.239
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2510
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0899
_diffrn_reflns_av_unetI/netI     0.1362
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29490
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.821
_diffrn_reflns_theta_min         2.929
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      153.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -52.00 -27.00   1.00    5.00    --    0.00 115.00  56.00   25
  2  ω    -99.00 -74.00   1.00    5.00    --    0.00-168.00-177.00   25
  3  ω   -130.00-103.00   1.00   15.00    --  -54.96-168.00-177.00   27
  4  ω   -111.00 -84.00   1.00   15.00    --  -54.96-115.00 -33.00   27
  5  ω     85.00 142.00   1.00   15.00    --   54.96 168.00-159.00   57
  6  ω     66.00 113.00   1.00   45.00    --  109.93-115.00 -33.00   47
  7  ω    114.00 139.00   1.00   45.00    --  109.93 115.00  56.00   25
  8  ω     87.00 112.00   1.00   45.00    --  109.93 168.00-159.00   25
  9  ω     60.00 148.00   1.00   45.00    --  109.93-168.00-177.00   88
 10  ω      3.00  32.00   1.00    5.00    --    0.00 -99.00-150.00   29
 11  ω     57.00  83.00   1.00    5.00    --    0.00 178.00 -30.00   26
 12  ω     25.00  52.00   1.00    5.00    --    0.00 -99.00  90.00   27
 13  ω     70.00  99.00   1.00    5.00    --    0.00 178.00 -90.00   29
 14  ω     18.00  45.00   1.00    5.00    --    0.00 -99.00 150.00   27
 15  ω     57.00  83.00   1.00    5.00    --    0.00 178.00  90.00   26
 16  ω   -146.00 -79.00   1.00   15.00    --  -54.96 -99.00 150.00   67
 17  ω   -150.00 -86.00   1.00   15.00    --  -54.96 -99.00   0.00   64
 18  ω   -149.00 -82.00   1.00   15.00    --  -54.96 -99.00  90.00   67
 19  ω   -121.00 -84.00   1.00   15.00    --  -54.96 -99.00  30.00   37
 20  ω    116.00 147.00   1.00   15.00    --   54.96 125.00 120.00   31
 21  ω    107.00 146.00   1.00   15.00    --   54.96 125.00 -60.00   39
 22  ω    108.00 178.00   1.00   45.00    --  109.93 111.00 120.00   70
 23  ω     66.00 178.00   1.00   45.00    --  109.93  77.00  60.00  112
 24  ω     34.00 109.00   1.00   45.00    --  109.93-111.00-180.00   75
 25  ω     85.00 168.00   1.00   45.00    --  109.93  38.00  30.00   83
 26  ω    103.00 128.00   1.00   45.00    --  109.93 178.00 -60.00   25
 27  ω     59.00  92.00   1.00   45.00    --  109.93 178.00 -60.00   33
 28  ω    104.00 173.00   1.00   45.00    --  109.93 111.00  90.00   69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0289046000
_diffrn_orient_matrix_UB_12      -0.0504633000
_diffrn_orient_matrix_UB_13      -0.0056313000
_diffrn_orient_matrix_UB_21      -0.1209464000
_diffrn_orient_matrix_UB_22      -0.0101803000
_diffrn_orient_matrix_UB_23      -0.0383217000
_diffrn_orient_matrix_UB_31      0.0262694000
_diffrn_orient_matrix_UB_32      0.0085391000
_diffrn_orient_matrix_UB_33      -0.0786800000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4979
_reflns_number_total             11984
_reflns_odcompleteness_completeness 99.07
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         11984
_refine_ls_number_restraints     56
_refine_ls_R_factor_all          0.2146
_refine_ls_R_factor_gt           0.1294
_refine_ls_restrained_S_all      1.140
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0500P)²+15.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2712
_refine_ls_wR_factor_ref         0.3175
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All P(H) groups
2. Restrained distances
 C62-Cl7
 1.75 with sigma of 0.005
 O6-C39 = O6-C40
 1.45 with sigma of 0.005
 C62-Cl3
 1.75 with sigma of 0.005
 C62-Cl5
 1.75 with sigma of 0.005
 C62-Cl4
 1.75 with sigma of 0.005
 C62-Cl6
 1.75 with sigma of 0.005
 C62-Cl2
 1.75 with sigma of 0.005
3. Rigid bond restraints
 C62, Cl4, C62, Cl5, C62, Cl6
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
O6 \\sim C39: within 1.7A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 1.7A
O6 \\sim C40: within 1.7A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 1.7A
5. Rigid body (RIGU) restrains
 C62, Cl7, Cl2, Cl3, Cl4, Cl5, Cl6
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
6. Others
 Fixed Sof: Br1(0.6) H4A(0.6) C40(0.75) H40A(0.75) H40B(0.75) H40C(0.75)
 C39(0.25) H39A(0.25) H39B(0.25) H39C(0.25) H62(0.85) H62A(0.15) Cl7(0.85)
 Cl2(0.85) Cl3(0.85) Cl4(0.15) Cl5(0.15) Cl6(0.15)
7.a Riding coordinates:
 P1(H1)
7.b Ternary CH refined with riding coordinates:
 C62(H62), C62(H62A)
7.c Secondary CH2 refined with riding coordinates:
 N4(H4A,H4B), C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C10(H10A,H10B), C11(H11A,
 H11B), C12(H12A,H12B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B),
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C42(H42A,H42B), C43(H43A,H43B),
  C44(H44A,H44B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B)
7.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9), C14(H14), C17(H17), C25(H25), C26(H26),
 C28(H28), C29(H29), C34(H34), C37(H37), C46(H46), C47(H47), C49(H49), C50(H50),
  C55(H55), C58(H58)
7.e Idealised Me refined with riding coordinates:
 C19(H19A,H19B,H19C), C60(H60A,H60B,H60C), C40(H40A,H40B,H40C), C39(H39A,H39B,
 H39C)
;
_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
Br1 Br 0.71332(16) 0.55235(6) 0.91261(9) 0.0865(5) Uani 0.6 1 d . . P . .
P1 P 0.2787(2) 0.61086(9) 0.74856(13) 0.0724(6) Uani 1 1 d . . . . .
H1 H 0.244582 0.639955 0.702939 0.109 Uiso 1 1 d R U . . .
O1 O 0.6243(7) 0.8112(2) 0.9770(4) 0.111(3) Uani 1 1 d . . . . .
O2 O 0.8362(6) 0.8727(3) 0.9325(4) 0.102(2) Uani 1 1 d . . . . .
O3 O 0.9497(7) 0.8281(3) 0.8414(5) 0.120(3) Uani 1 1 d . . . . .
O4 O 0.0231(6) 0.7822(3) 0.6351(4) 0.109(2) Uani 1 1 d . . . . .
O005 O 0.3363(5) 0.5771(2) 0.7082(3) 0.0767(17) Uani 1 1 d . . . . .
O5 O 0.2216(6) 0.8990(2) 0.6611(4) 0.091(2) Uani 1 1 d . . . . .
O6 O 0.3183(7) 0.9181(4) 0.8008(4) 0.137(3) Uani 1 1 d D U . . .
O7 O 0.7099(5) 0.6605(2) 0.5685(3) 0.0837(19) Uani 1 1 d . . . . .
O8 O 0.6517(6) 0.7741(2) 0.4767(3) 0.089(2) Uani 1 1 d . . . . .
O9 O 0.4623(6) 0.8079(3) 0.4176(3) 0.097(2) Uani 1 1 d . . . . .
N1 N 0.3612(7) 0.5442(3) 0.8812(4) 0.079(2) Uani 1 1 d . . . . .
N2 N 0.3577(6) 0.6367(2) 0.8220(4) 0.0693(19) Uani 1 1 d . . . . .
N3 N 0.1686(6) 0.5893(3) 0.7730(5) 0.087(2) Uani 1 1 d . . . . .
N4 N 0.5044(7) 0.5251(2) 0.7790(4) 0.078(2) Uani 1 1 d . . . . .
H4A H 0.563491 0.535680 0.813745 0.094 Uiso 0.6 1 calc R U P . .
H4B H 0.455269 0.548254 0.767438 0.094 Uiso 1 1 calc R U . . .
C1 C 0.4057(9) 0.5819(3) 0.9301(5) 0.087(3) Uani 1 1 d . . . . .
H1A H 0.485833 0.584432 0.932513 0.104 Uiso 1 1 calc R U . . .
H1B H 0.394924 0.576288 0.982277 0.104 Uiso 1 1 calc R U . . .
C2 C 0.3496(8) 0.6259(3) 0.9003(4) 0.081(3) Uani 1 1 d . . . . .
H2A H 0.270731 0.624107 0.902494 0.097 Uiso 1 1 calc R U . . .
H2B H 0.382977 0.650959 0.934186 0.097 Uiso 1 1 calc R U . . .
C3 C 0.4651(7) 0.6525(3) 0.8093(5) 0.071(2) Uani 1 1 d . . . . .
H3A H 0.458351 0.659500 0.754604 0.085 Uiso 1 1 calc R U . . .
H3B H 0.520400 0.628039 0.823154 0.085 Uiso 1 1 calc R U . . .
C4 C 0.5037(8) 0.6940(3) 0.8561(5) 0.068(2) Uani 1 1 d . . . . .
C5 C 0.4472(9) 0.7342(4) 0.8474(6) 0.089(3) Uani 1 1 d . . . . .
H5 H 0.378043 0.735981 0.812530 0.107 Uiso 1 1 calc R U . . .
C6 C 0.4898(10) 0.7728(3) 0.8893(6) 0.092(3) Uani 1 1 d . . . . .
H6 H 0.450161 0.800560 0.882161 0.110 Uiso 1 1 calc R U . . .
C7 C 0.5894(10) 0.7702(4) 0.9408(6) 0.087(3) Uani 1 1 d . . . . .
C8 C 0.6441(9) 0.7307(4) 0.9503(6) 0.093(3) Uani 1 1 d . . . . .
H8 H 0.712354 0.728607 0.986091 0.111 Uiso 1 1 calc R U . . .
C9 C 0.6015(8) 0.6930(3) 0.9083(5) 0.081(3) Uani 1 1 d . . . . .
H9 H 0.641692 0.665367 0.916061 0.097 Uiso 1 1 calc R U . . .
C10 C 0.7368(11) 0.8109(4) 1.0234(6) 0.119(5) Uani 1 1 d . . . . .
H10A H 0.789092 0.798418 0.994105 0.143 Uiso 1 1 calc R U . . .
H10B H 0.740994 0.792367 1.069864 0.143 Uiso 1 1 calc R U . . .
C11 C 0.7633(13) 0.8606(4) 1.0441(6) 0.136(5) Uani 1 1 d . . . . .
H11A H 0.709422 0.872399 1.072713 0.164 Uiso 1 1 calc R U . . .
H11B H 0.837560 0.862674 1.077698 0.164 Uiso 1 1 calc R U . . .
C12 C 0.7597(12) 0.8898(4) 0.9743(5) 0.111(4) Uani 1 1 d . . . . .
H12A H 0.684398 0.889428 0.941846 0.133 Uiso 1 1 calc R U . . .
H12B H 0.778646 0.921421 0.989896 0.133 Uiso 1 1 calc R U . . .
C13 C 0.8211(8) 0.8858(4) 0.8569(5) 0.083(3) Uani 1 1 d . . . . .
C14 C 0.7555(8) 0.9214(3) 0.8289(5) 0.074(2) Uani 1 1 d . . . . .
H14 H 0.722359 0.938996 0.862195 0.089 Uiso 1 1 calc R U . . .
C15 C 0.7362(7) 0.9325(3) 0.7509(5) 0.069(2) Uani 1 1 d . . . . .
C16 C 0.7884(7) 0.9073(3) 0.7026(5) 0.071(2) Uani 1 1 d . . . . .
C17 C 0.8576(7) 0.8731(3) 0.7364(5) 0.073(2) Uani 1 1 d . . . . .
H17 H 0.895199 0.856174 0.704854 0.088 Uiso 1 1 calc R U . . .
C18 C 0.8758(8) 0.8618(3) 0.8111(6) 0.081(3) Uani 1 1 d . . . . .
C19 C 0.9144(14) 0.7883(5) 0.8416(8) 0.164(7) Uani 1 1 d . . . . .
H19A H 0.870768 0.780850 0.790884 0.246 Uiso 1 1 calc R U . . .
H19B H 0.868032 0.785728 0.879135 0.246 Uiso 1 1 calc R U . . .
H19C H 0.976735 0.767382 0.854827 0.246 Uiso 1 1 calc R U . . .
C20 C 0.6569(8) 0.9720(3) 0.7246(5) 0.077(3) Uani 1 1 d . . . . .
C21 C 0.2433(10) 0.5347(3) 0.8783(5) 0.096(4) Uani 1 1 d . . . . .
H21A H 0.216885 0.554677 0.914959 0.116 Uiso 1 1 calc R U . . .
H21B H 0.234902 0.502950 0.893710 0.116 Uiso 1 1 calc R U . . .
C22 C 0.1748(10) 0.5423(4) 0.8005(7) 0.109(4) Uani 1 1 d . . . . .
H22A H 0.204529 0.523282 0.764236 0.130 Uiso 1 1 calc R U . . .
H22B H 0.098982 0.531654 0.799742 0.130 Uiso 1 1 calc R U . . .
C23 C 0.0798(9) 0.6173(4) 0.7912(7) 0.104(4) Uani 1 1 d . . . . .
H23A H 0.095085 0.622298 0.846979 0.125 Uiso 1 1 calc R U . . .
H23B H 0.009585 0.600315 0.777118 0.125 Uiso 1 1 calc R U . . .
C24 C 0.0654(9) 0.6623(4) 0.7522(7) 0.088(3) Uani 1 1 d . . . . .
C25 C 0.0054(9) 0.6654(5) 0.6787(8) 0.121(5) Uani 1 1 d . . . . .
H25 H -0.028219 0.639116 0.653461 0.145 Uiso 1 1 calc R U . . .
C26 C -0.0064(11) 0.7062(5) 0.6415(7) 0.119(4) Uani 1 1 d . . . . .
H26 H -0.050632 0.708349 0.591426 0.143 Uiso 1 1 calc R U . . .
C27 C 0.0445(9) 0.7432(4) 0.6758(6) 0.092(3) Uani 1 1 d . . . . .
C28 C 0.1066(10) 0.7408(4) 0.7483(5) 0.098(3) Uani 1 1 d . . . . .
H28 H 0.143325 0.766917 0.772108 0.118 Uiso 1 1 calc R U . . .
C29 C 0.1155(9) 0.7006(4) 0.7861(6) 0.094(3) Uani 1 1 d . . . . .
H29 H 0.157113 0.699109 0.836962 0.113 Uiso 1 1 calc R U . . .
C30 C 0.1028(9) 0.8159(4) 0.6509(6) 0.103(4) Uani 1 1 d . . . . .
H30A H 0.175872 0.803115 0.649191 0.124 Uiso 1 1 calc R U . . .
H30B H 0.106349 0.828063 0.702726 0.124 Uiso 1 1 calc R U . . .
C31 C 0.0751(8) 0.8535(4) 0.5935(6) 0.100(4) Uani 1 1 d . . . . .
H31A H 0.019677 0.873771 0.608151 0.121 Uiso 1 1 calc R U . . .
H31B H 0.042535 0.840488 0.542871 0.121 Uiso 1 1 calc R U . . .
C32 C 0.1762(8) 0.8806(3) 0.5884(6) 0.085(3) Uani 1 1 d . . . . .
H32A H 0.231002 0.860821 0.571781 0.102 Uiso 1 1 calc R U . . .
H32B H 0.156180 0.905255 0.550685 0.102 Uiso 1 1 calc R U . . .
C33 C 0.3266(8) 0.9164(3) 0.6724(5) 0.078(3) Uani 1 1 d . . . . .
C34 C 0.3785(8) 0.9261(3) 0.6123(5) 0.073(2) Uani 1 1 d . . . . .
H34 H 0.341335 0.920331 0.561250 0.088 Uiso 1 1 calc R U . . .
C35 C 0.4850(8) 0.9443(3) 0.6276(5) 0.067(2) Uani 1 1 d . . . . .
C36 C 0.5394(9) 0.9535(3) 0.7009(5) 0.077(3) Uani 1 1 d . . . . .
C37 C 0.4827(9) 0.9445(3) 0.7594(6) 0.083(3) Uani 1 1 d . . . . .
H37 H 0.517443 0.951384 0.810546 0.100 Uiso 1 1 calc R U . . .
C38 C 0.3796(10) 0.9264(4) 0.7446(5) 0.094(4) Uani 1 1 d . . . . .
C41 C 0.5393(8) 0.9510(3) 0.5579(5) 0.077(3) Uani 1 1 d . . . . .
C42 C 0.4315(10) 0.5040(3) 0.8909(5) 0.094(3) Uani 1 1 d . . . . .
H42A H 0.395687 0.479492 0.914288 0.113 Uiso 1 1 calc R U . . .
H42B H 0.502701 0.511185 0.925718 0.113 Uiso 1 1 calc R U . . .
C43 C 0.4524(9) 0.4880(3) 0.8145(5) 0.083(3) Uani 1 1 d . . . . .
H43A H 0.501491 0.461199 0.822283 0.099 Uiso 1 1 calc R U . . .
H43B H 0.381839 0.479126 0.780424 0.099 Uiso 1 1 calc R U . . .
C44 C 0.5421(9) 0.5118(3) 0.7083(5) 0.088(3) Uani 1 1 d . . . . .
H44A H 0.479580 0.498234 0.671521 0.106 Uiso 1 1 calc R U . . .
H44B H 0.600694 0.488643 0.721238 0.106 Uiso 1 1 calc R U . . .
C45 C 0.5858(8) 0.5520(3) 0.6716(5) 0.079(3) Uani 1 1 d . . . . .
C46 C 0.6726(8) 0.5773(3) 0.7077(5) 0.084(3) Uani 1 1 d . . . . .
H46 H 0.707256 0.569732 0.758570 0.100 Uiso 1 1 calc R U . . .
C47 C 0.7126(8) 0.6135(3) 0.6735(5) 0.084(3) Uani 1 1 d . . . . .
H47 H 0.773622 0.630452 0.700435 0.101 Uiso 1 1 calc R U . . .
C48 C 0.6626(7) 0.6248(3) 0.5993(5) 0.072(2) Uani 1 1 d . . . . .
C49 C 0.5743(8) 0.6010(4) 0.5630(5) 0.089(3) Uani 1 1 d . . . . .
H49 H 0.538042 0.608989 0.512643 0.107 Uiso 1 1 calc R U . . .
C50 C 0.5361(8) 0.5645(4) 0.5996(6) 0.093(3) Uani 1 1 d . . . . .
H50 H 0.473635 0.548009 0.573528 0.112 Uiso 1 1 calc R U . . .
C51 C 0.6649(8) 0.6726(3) 0.4918(4) 0.083(3) Uani 1 1 d . . . . .
H51A H 0.591201 0.686403 0.487476 0.100 Uiso 1 1 calc R U . . .
H51B H 0.657121 0.645424 0.458809 0.100 Uiso 1 1 calc R U . . .
C52 C 0.7416(9) 0.7057(3) 0.4679(5) 0.083(3) Uani 1 1 d . . . . .
H52A H 0.718412 0.709901 0.412046 0.100 Uiso 1 1 calc R U . . .
H52B H 0.816160 0.692101 0.478167 0.100 Uiso 1 1 calc R U . . .
C53 C 0.7502(8) 0.7527(3) 0.5055(5) 0.081(3) Uani 1 1 d . . . . .
H53A H 0.762299 0.749827 0.561524 0.097 Uiso 1 1 calc R U . . .
H53B H 0.812217 0.770041 0.492951 0.097 Uiso 1 1 calc R U . . .
C54 C 0.6354(8) 0.8174(3) 0.4988(5) 0.069(2) Uani 1 1 d . . . . .
C55 C 0.7093(7) 0.8438(3) 0.5467(4) 0.067(2) Uani 1 1 d . . . . .
H55 H 0.780253 0.831684 0.567172 0.080 Uiso 1 1 calc R U . . .
C56 C 0.6863(7) 0.8883(3) 0.5679(4) 0.063(2) Uani 1 1 d . . . . .
C57 C 0.5794(7) 0.9050(3) 0.5366(5) 0.067(2) Uani 1 1 d . . . . .
C58 C 0.5055(8) 0.8787(3) 0.4864(5) 0.071(2) Uani 1 1 d . . . . .
H58 H 0.434936 0.890773 0.464247 0.085 Uiso 1 1 calc R U . . .
C59 C 0.5309(7) 0.8362(3) 0.4679(5) 0.071(2) Uani 1 1 d . . . . .
C60 C 0.3615(8) 0.8272(4) 0.3766(6) 0.120(4) Uani 1 1 d . . . . .
H60A H 0.318357 0.803980 0.344390 0.180 Uiso 1 1 calc R U . . .
H60B H 0.377796 0.852083 0.344608 0.180 Uiso 1 1 calc R U . . .
H60C H 0.319294 0.838844 0.412700 0.180 Uiso 1 1 calc R U . . .
C61 C 0.7752(7) 0.9162(3) 0.6170(4) 0.068(2) Uani 1 1 d . . . . .
C40 C 0.3803(12) 0.9106(7) 0.8772(6) 0.151(5) Uani 0.75 1 d D U P A 1
H40A H 0.449847 0.895425 0.875436 0.226 Uiso 0.75 1 calc R U P A 1
H40B H 0.337332 0.891511 0.904758 0.226 Uiso 0.75 1 calc R U P A 1
H40C H 0.395797 0.939719 0.903495 0.226 Uiso 0.75 1 calc R U P A 1
C39 C 0.293(4) 0.8735(7) 0.825(3) 0.134(6) Uani 0.25 1 d D U P A 2
H39A H 0.303942 0.851014 0.787558 0.201 Uiso 0.25 1 calc R U P A 2
H39B H 0.215492 0.872688 0.830061 0.201 Uiso 0.25 1 calc R U P A 2
H39C H 0.340803 0.866556 0.874625 0.201 Uiso 0.25 1 calc R U P A 2
C62 C 0.5389(5) 0.7941(2) 0.6590(5) 0.156(3) Uani 1 1 d D U . . .
H62 H 0.553716 0.809244 0.612462 0.187 Uiso 0.85 1 calc R U P B 1
H62A H 0.567283 0.809895 0.617895 0.187 Uiso 0.15 1 calc R U P C 2
Cl7 Cl 0.5816(4) 0.82827(16) 0.7386(3) 0.1529(16) Uani 0.85 1 d D . P D 1
Cl2 Cl 0.3982(4) 0.7864(2) 0.6508(3) 0.188(2) Uani 0.85 1 d D . P D 1
Cl3 Cl 0.6069(7) 0.7423(2) 0.6738(5) 0.223(3) Uani 0.85 1 d D . P D 1
Cl4 Cl 0.470(3) 0.8305(11) 0.709(2) 0.203(4) Uani 0.15 1 d D U P D 2
Cl5 Cl 0.468(3) 0.7441(7) 0.6273(16) 0.164(6) Uani 0.15 1 d D U P D 2
Cl6 Cl 0.6445(19) 0.7711(13) 0.7292(14) 0.175(5) Uani 0.15 1 d D U P D 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 H1 1.2003 . ?
P1 O005 1.503(6) . ?
P1 N2 1.652(7) . ?
P1 N3 1.652(7) . ?
O1 C7 1.398(11) . ?
O1 C10 1.466(13) . ?
O2 C12 1.425(13) . ?
O2 C13 1.386(10) . ?
O3 C18 1.385(11) . ?
O3 C19 1.252(15) . ?
O4 C27 1.358(12) . ?
O4 C30 1.390(12) . ?
O5 C32 1.415(11) . ?
O5 C33 1.377(11) . ?
O6 C38 1.410(10) . ?
O6 C40 1.440(5) . ?
O6 C39 1.446(5) . ?
O7 C48 1.378(10) . ?
O7 C51 1.418(9) . ?
O8 C53 1.374(10) . ?
O8 C54 1.368(10) . ?
O9 C59 1.381(11) . ?
O9 C60 1.427(11) . ?
N1 C1 1.453(11) . ?
N1 C21 1.480(12) . ?
N1 C42 1.460(12) . ?
N2 C2 1.468(9) . ?
N2 C3 1.477(9) . ?
N3 C22 1.468(12) . ?
N3 C23 1.471(11) . ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N4 C43 1.485(10) . ?
N4 C44 1.498(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.517(12) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.506(11) . ?
C4 C5 1.370(12) . ?
C4 C9 1.366(12) . ?
C5 H5 0.9500 . ?
C5 C6 1.405(13) . ?
C6 H6 0.9500 . ?
C6 C7 1.379(14) . ?
C7 C8 1.342(14) . ?
C8 H8 0.9500 . ?
C8 C9 1.386(12) . ?
C9 H9 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.534(14) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.514(12) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.358(13) . ?
C13 C18 1.372(14) . ?
C14 H14 0.9500 . ?
C14 C15 1.410(11) . ?
C15 C16 1.403(12) . ?
C15 C20 1.534(12) . ?
C16 C17 1.380(11) . ?
C16 C61 1.535(11) . ?
C17 H17 0.9500 . ?
C17 C18 1.355(12) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C36 1.531(13) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.490(14) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.496(14) . ?
C24 C25 1.373(14) . ?
C24 C29 1.370(13) . ?
C25 H25 0.9500 . ?
C25 C26 1.370(16) . ?
C26 H26 0.9500 . ?
C26 C27 1.344(15) . ?
C27 C28 1.366(13) . ?
C28 H28 0.9500 . ?
C28 C29 1.359(13) . ?
C29 H29 0.9500 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.504(13) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.507(13) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.400(11) . ?
C33 C38 1.356(13) . ?
C34 H34 0.9500 . ?
C34 C35 1.400(12) . ?
C35 C36 1.373(12) . ?
C35 C41 1.557(10) . ?
C36 C37 1.410(12) . ?
C37 H37 0.9500 . ?
C37 C38 1.361(14) . ?
C41 C57 1.524(12) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 C43 1.528(11) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.514(12) . ?
C45 C46 1.357(13) . ?
C45 C50 1.359(12) . ?
C46 H46 0.9500 . ?
C46 C47 1.377(12) . ?
C47 H47 0.9500 . ?
C47 C48 1.386(11) . ?
C48 C49 1.348(12) . ?
C49 H49 0.9500 . ?
C49 C50 1.398(13) . ?
C50 H50 0.9500 . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C51 C52 1.491(12) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C52 C53 1.538(12) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.361(12) . ?
C54 C59 1.410(12) . ?
C55 H55 0.9500 . ?
C55 C56 1.413(11) . ?
C56 C57 1.414(11) . ?
C56 C61 1.503(11) . ?
C57 C58 1.380(12) . ?
C58 H58 0.9500 . ?
C58 C59 1.354(12) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C62 H62 1.0000 . ?
C62 H62A 1.0000 . ?
C62 Cl7 1.738(5) . ?
C62 Cl2 1.736(5) . ?
C62 Cl3 1.739(5) . ?
C62 Cl4 1.744(5) . ?
C62 Cl5 1.751(5) . ?
C62 Cl6 1.751(5) . ?

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
O005 P1 H1 106.3 . . ?
O005 P1 N2 115.4(4) . . ?
O005 P1 N3 112.3(4) . . ?
N2 P1 H1 106.1 . . ?
N2 P1 N3 110.5(4) . . ?
N3 P1 H1 105.5 . . ?
C7 O1 C10 114.9(10) . . ?
C13 O2 C12 116.9(9) . . ?
C19 O3 C18 118.1(11) . . ?
C27 O4 C30 116.7(9) . . ?
C33 O5 C32 117.1(7) . . ?
C38 O6 C40 116.7(11) . . ?
C38 O6 C39 124(2) . . ?
C48 O7 C51 118.1(7) . . ?
C54 O8 C53 119.7(8) . . ?
C59 O9 C60 116.5(8) . . ?
C1 N1 C21 114.2(8) . . ?
C1 N1 C42 114.2(9) . . ?
C42 N1 C21 114.4(8) . . ?
C2 N2 P1 121.0(6) . . ?
C2 N2 C3 117.8(7) . . ?
C3 N2 P1 115.1(5) . . ?
C22 N3 P1 117.9(7) . . ?
C22 N3 C23 116.4(8) . . ?
C23 N3 P1 123.1(7) . . ?
H4A N4 H4B 107.6 . . ?
C43 N4 H4A 108.6 . . ?
C43 N4 H4B 108.6 . . ?
C43 N4 C44 114.5(7) . . ?
C44 N4 H4A 108.6 . . ?
C44 N4 H4B 108.6 . . ?
N1 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
N1 C1 C2 111.0(8) . . ?
H1A C1 H1B 108.0 . . ?
C2 C1 H1A 109.4 . . ?
C2 C1 H1B 109.4 . . ?
N2 C2 C1 113.8(7) . . ?
N2 C2 H2A 108.8 . . ?
N2 C2 H2B 108.8 . . ?
C1 C2 H2A 108.8 . . ?
C1 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
N2 C3 H3A 109.4 . . ?
N2 C3 H3B 109.4 . . ?
N2 C3 C4 111.1(7) . . ?
H3A C3 H3B 108.0 . . ?
C4 C3 H3A 109.4 . . ?
C4 C3 H3B 109.4 . . ?
C5 C4 C3 123.2(9) . . ?
C9 C4 C3 119.6(9) . . ?
C9 C4 C5 117.1(9) . . ?
C4 C5 H5 119.4 . . ?
C4 C5 C6 121.1(11) . . ?
C6 C5 H5 119.4 . . ?
C5 C6 H6 120.2 . . ?
C7 C6 C5 119.6(10) . . ?
C7 C6 H6 120.2 . . ?
C6 C7 O1 114.1(11) . . ?
C8 C7 O1 126.5(12) . . ?
C8 C7 C6 119.4(10) . . ?
C7 C8 H8 119.8 . . ?
C7 C8 C9 120.4(11) . . ?
C9 C8 H8 119.8 . . ?
C4 C9 C8 122.3(10) . . ?
C4 C9 H9 118.8 . . ?
C8 C9 H9 118.8 . . ?
O1 C10 H10A 110.7 . . ?
O1 C10 H10B 110.7 . . ?
O1 C10 C11 105.0(11) . . ?
H10A C10 H10B 108.8 . . ?
C11 C10 H10A 110.7 . . ?
C11 C10 H10B 110.7 . . ?
C10 C11 H11A 109.2 . . ?
C10 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C12 C11 C10 112.1(8) . . ?
C12 C11 H11A 109.2 . . ?
C12 C11 H11B 109.2 . . ?
O2 C12 C11 109.4(10) . . ?
O2 C12 H12A 109.8 . . ?
O2 C12 H12B 109.8 . . ?
C11 C12 H12A 109.8 . . ?
C11 C12 H12B 109.8 . . ?
H12A C12 H12B 108.2 . . ?
C14 C13 O2 121.6(11) . . ?
C14 C13 C18 120.8(9) . . ?
C18 C13 O2 117.5(10) . . ?
C13 C14 H14 119.7 . . ?
C13 C14 C15 120.6(10) . . ?
C15 C14 H14 119.7 . . ?
C14 C15 C20 116.3(9) . . ?
C16 C15 C14 119.3(9) . . ?
C16 C15 C20 124.4(8) . . ?
C15 C16 C61 124.4(8) . . ?
C17 C16 C15 116.3(9) . . ?
C17 C16 C61 119.2(9) . . ?
C16 C17 H17 117.6 . . ?
C18 C17 C16 124.8(10) . . ?
C18 C17 H17 117.6 . . ?
C13 C18 O3 120.5(9) . . ?
C17 C18 O3 121.5(10) . . ?
C17 C18 C13 118.0(9) . . ?
O3 C19 H19A 109.5 . . ?
O3 C19 H19B 109.5 . . ?
O3 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C36 C20 C15 109.0(7) . . ?
N1 C21 H21A 109.3 . . ?
N1 C21 H21B 109.3 . . ?
N1 C21 C22 111.4(7) . . ?
H21A C21 H21B 108.0 . . ?
C22 C21 H21A 109.3 . . ?
C22 C21 H21B 109.3 . . ?
N3 C22 C21 115.8(9) . . ?
N3 C22 H22A 108.3 . . ?
N3 C22 H22B 108.3 . . ?
C21 C22 H22A 108.3 . . ?
C21 C22 H22B 108.3 . . ?
H22A C22 H22B 107.4 . . ?
N3 C23 H23A 108.6 . . ?
N3 C23 H23B 108.6 . . ?
N3 C23 C24 114.5(9) . . ?
H23A C23 H23B 107.6 . . ?
C24 C23 H23A 108.6 . . ?
C24 C23 H23B 108.6 . . ?
C25 C24 C23 119.8(11) . . ?
C29 C24 C23 121.9(11) . . ?
C29 C24 C25 118.2(12) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 C24 120.5(12) . . ?
C26 C25 H25 119.7 . . ?
C25 C26 H26 120.0 . . ?
C27 C26 C25 120.0(12) . . ?
C27 C26 H26 120.0 . . ?
O4 C27 C28 124.3(11) . . ?
C26 C27 O4 115.0(11) . . ?
C26 C27 C28 120.6(12) . . ?
C27 C28 H28 120.3 . . ?
C29 C28 C27 119.4(11) . . ?
C29 C28 H28 120.3 . . ?
C24 C29 H29 119.4 . . ?
C28 C29 C24 121.2(11) . . ?
C28 C29 H29 119.4 . . ?
O4 C30 H30A 109.7 . . ?
O4 C30 H30B 109.7 . . ?
O4 C30 C31 110.0(9) . . ?
H30A C30 H30B 108.2 . . ?
C31 C30 H30A 109.7 . . ?
C31 C30 H30B 109.7 . . ?
C30 C31 H31A 109.4 . . ?
C30 C31 H31B 109.4 . . ?
C30 C31 C32 111.2(9) . . ?
H31A C31 H31B 108.0 . . ?
C32 C31 H31A 109.4 . . ?
C32 C31 H31B 109.4 . . ?
O5 C32 C31 108.6(8) . . ?
O5 C32 H32A 110.0 . . ?
O5 C32 H32B 110.0 . . ?
C31 C32 H32A 110.0 . . ?
C31 C32 H32B 110.0 . . ?
H32A C32 H32B 108.3 . . ?
O5 C33 C34 122.8(9) . . ?
C38 C33 O5 118.1(8) . . ?
C38 C33 C34 119.0(10) . . ?
C33 C34 H34 120.0 . . ?
C33 C34 C35 120.0(9) . . ?
C35 C34 H34 120.0 . . ?
C34 C35 C41 116.5(9) . . ?
C36 C35 C34 120.9(8) . . ?
C36 C35 C41 122.6(9) . . ?
C35 C36 C20 125.5(8) . . ?
C35 C36 C37 117.2(10) . . ?
C37 C36 C20 117.3(9) . . ?
C36 C37 H37 119.1 . . ?
C38 C37 C36 121.9(9) . . ?
C38 C37 H37 119.1 . . ?
C33 C38 O6 115.0(11) . . ?
C33 C38 C37 121.0(8) . . ?
C37 C38 O6 123.9(10) . . ?
C57 C41 C35 108.1(6) . . ?
N1 C42 H42A 109.5 . . ?
N1 C42 H42B 109.5 . . ?
N1 C42 C43 110.9(7) . . ?
H42A C42 H42B 108.0 . . ?
C43 C42 H42A 109.5 . . ?
C43 C42 H42B 109.5 . . ?
N4 C43 C42 109.3(7) . . ?
N4 C43 H43A 109.8 . . ?
N4 C43 H43B 109.8 . . ?
C42 C43 H43A 109.8 . . ?
C42 C43 H43B 109.8 . . ?
H43A C43 H43B 108.3 . . ?
N4 C44 H44A 109.3 . . ?
N4 C44 H44B 109.3 . . ?
N4 C44 C45 111.8(8) . . ?
H44A C44 H44B 107.9 . . ?
C45 C44 H44A 109.3 . . ?
C45 C44 H44B 109.3 . . ?
C46 C45 C44 123.1(9) . . ?
C46 C45 C50 117.2(9) . . ?
C50 C45 C44 119.7(10) . . ?
C45 C46 H46 118.7 . . ?
C45 C46 C47 122.6(9) . . ?
C47 C46 H46 118.7 . . ?
C46 C47 H47 120.4 . . ?
C46 C47 C48 119.2(10) . . ?
C48 C47 H47 120.4 . . ?
O7 C48 C47 115.5(9) . . ?
C49 C48 O7 125.3(8) . . ?
C49 C48 C47 119.3(9) . . ?
C48 C49 H49 120.1 . . ?
C48 C49 C50 119.9(9) . . ?
C50 C49 H49 120.1 . . ?
C45 C50 C49 121.8(10) . . ?
C45 C50 H50 119.1 . . ?
C49 C50 H50 119.1 . . ?
O7 C51 H51A 110.2 . . ?
O7 C51 H51B 110.2 . . ?
O7 C51 C52 107.7(8) . . ?
H51A C51 H51B 108.5 . . ?
C52 C51 H51A 110.2 . . ?
C52 C51 H51B 110.2 . . ?
C51 C52 H52A 108.1 . . ?
C51 C52 H52B 108.1 . . ?
C51 C52 C53 117.0(8) . . ?
H52A C52 H52B 107.3 . . ?
C53 C52 H52A 108.1 . . ?
C53 C52 H52B 108.1 . . ?
O8 C53 C52 106.1(8) . . ?
O8 C53 H53A 110.5 . . ?
O8 C53 H53B 110.5 . . ?
C52 C53 H53A 110.5 . . ?
C52 C53 H53B 110.5 . . ?
H53A C53 H53B 108.7 . . ?
O8 C54 C59 115.7(9) . . ?
C55 C54 O8 126.7(9) . . ?
C55 C54 C59 117.5(9) . . ?
C54 C55 H55 118.1 . . ?
C54 C55 C56 123.7(9) . . ?
C56 C55 H55 118.1 . . ?
C55 C56 C57 116.3(9) . . ?
C55 C56 C61 120.1(8) . . ?
C57 C56 C61 123.5(8) . . ?
C56 C57 C41 122.7(9) . . ?
C58 C57 C41 117.3(8) . . ?
C58 C57 C56 120.1(9) . . ?
C57 C58 H58 119.2 . . ?
C59 C58 C57 121.6(9) . . ?
C59 C58 H58 119.2 . . ?
O9 C59 C54 114.0(9) . . ?
C58 C59 O9 125.2(9) . . ?
C58 C59 C54 120.7(9) . . ?
O9 C60 H60A 109.5 . . ?
O9 C60 H60B 109.5 . . ?
O9 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C56 C61 C16 113.7(6) . . ?
O6 C40 H40A 109.5 . . ?
O6 C40 H40B 109.5 . . ?
O6 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O6 C39 H39A 109.5 . . ?
O6 C39 H39B 109.5 . . ?
O6 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
Cl7 C62 H62 110.5 . . ?
Cl7 C62 Cl3 109.4(5) . . ?
Cl2 C62 H62 110.5 . . ?
Cl2 C62 Cl7 105.6(5) . . ?
Cl2 C62 Cl3 110.2(5) . . ?
Cl3 C62 H62 110.5 . . ?
Cl4 C62 H62A 112.7 . . ?
Cl4 C62 Cl5 114.8(18) . . ?
Cl4 C62 Cl6 104.0(18) . . ?
Cl5 C62 H62A 112.7 . . ?
Cl5 C62 Cl6 98.8(17) . . ?
Cl6 C62 H62A 112.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 N2 C2 C1 77.3(10) . . . . ?
P1 N2 C3 C4 150.1(6) . . . . ?
P1 N3 C22 C21 72.9(10) . . . . ?
P1 N3 C23 C24 28.2(14) . . . . ?
O1 C7 C8 C9 -177.5(9) . . . . ?
O1 C10 C11 C12 -61.4(14) . . . . ?
O2 C13 C14 C15 -176.2(8) . . . . ?
O2 C13 C18 O3 -4.9(14) . . . . ?
O2 C13 C18 C17 177.0(8) . . . . ?
O4 C27 C28 C29 174.7(10) . . . . ?
O4 C30 C31 C32 -157.6(9) . . . . ?
O005 P1 N2 C2 -107.8(7) . . . . ?
O005 P1 N2 C3 44.1(7) . . . . ?
O005 P1 N3 C22 38.7(9) . . . . ?
O005 P1 N3 C23 -160.7(8) . . . . ?
O5 C33 C34 C35 179.3(8) . . . . ?
O5 C33 C38 O6 -1.0(14) . . . . ?
O5 C33 C38 C37 -178.7(9) . . . . ?
O7 C48 C49 C50 177.9(9) . . . . ?
O7 C51 C52 C53 -68.4(11) . . . . ?
O8 C54 C55 C56 -179.2(7) . . . . ?
O8 C54 C59 O9 -2.2(11) . . . . ?
O8 C54 C59 C58 179.4(7) . . . . ?
N1 C1 C2 N2 -57.3(11) . . . . ?
N1 C21 C22 N3 -65.7(12) . . . . ?
N1 C42 C43 N4 58.2(11) . . . . ?
N2 P1 N3 C22 -91.7(8) . . . . ?
N2 P1 N3 C23 68.8(10) . . . . ?
N2 C3 C4 C5 -62.1(11) . . . . ?
N2 C3 C4 C9 120.2(9) . . . . ?
N3 P1 N2 C2 21.0(8) . . . . ?
N3 P1 N2 C3 172.9(6) . . . . ?
N3 C23 C24 C25 82.4(14) . . . . ?
N3 C23 C24 C29 -94.1(12) . . . . ?
N4 C44 C45 C46 59.8(13) . . . . ?
N4 C44 C45 C50 -119.1(10) . . . . ?
C1 N1 C21 C22 115.8(9) . . . . ?
C1 N1 C42 C43 -127.6(9) . . . . ?
C2 N2 C3 C4 -57.1(10) . . . . ?
C3 N2 C2 C1 -73.8(10) . . . . ?
C3 C4 C5 C6 -176.2(8) . . . . ?
C3 C4 C9 C8 176.7(8) . . . . ?
C4 C5 C6 C7 -0.9(15) . . . . ?
C5 C4 C9 C8 -1.1(14) . . . . ?
C5 C6 C7 O1 178.1(8) . . . . ?
C5 C6 C7 C8 -0.2(16) . . . . ?
C6 C7 C8 C9 0.7(16) . . . . ?
C7 O1 C10 C11 169.6(8) . . . . ?
C7 C8 C9 C4 0.0(15) . . . . ?
C9 C4 C5 C6 1.5(13) . . . . ?
C10 O1 C7 C6 -171.5(9) . . . . ?
C10 O1 C7 C8 6.7(14) . . . . ?
C10 C11 C12 O2 -58.3(15) . . . . ?
C12 O2 C13 C14 15.9(13) . . . . ?
C12 O2 C13 C18 -164.7(9) . . . . ?
C13 O2 C12 C11 160.9(8) . . . . ?
C13 C14 C15 C16 -2.1(13) . . . . ?
C13 C14 C15 C20 177.4(8) . . . . ?
C14 C13 C18 O3 174.5(8) . . . . ?
C14 C13 C18 C17 -3.5(14) . . . . ?
C14 C15 C16 C17 -0.8(12) . . . . ?
C14 C15 C16 C61 -179.4(7) . . . . ?
C14 C15 C20 C36 -89.9(9) . . . . ?
C15 C16 C17 C18 1.6(13) . . . . ?
C15 C16 C61 C56 -93.6(10) . . . . ?
C15 C20 C36 C35 -98.0(10) . . . . ?
C15 C20 C36 C37 81.1(10) . . . . ?
C16 C15 C20 C36 89.6(10) . . . . ?
C16 C17 C18 O3 -177.5(9) . . . . ?
C16 C17 C18 C13 0.5(15) . . . . ?
C17 C16 C61 C56 87.9(10) . . . . ?
C18 C13 C14 C15 4.4(14) . . . . ?
C19 O3 C18 C13 91.9(15) . . . . ?
C19 O3 C18 C17 -90.2(15) . . . . ?
C20 C15 C16 C17 179.7(8) . . . . ?
C20 C15 C16 C61 1.1(13) . . . . ?
C20 C36 C37 C38 -177.4(9) . . . . ?
C21 N1 C1 C2 -64.0(10) . . . . ?
C21 N1 C42 C43 98.2(9) . . . . ?
C22 N3 C23 C24 -170.9(10) . . . . ?
C23 N3 C22 C21 -89.0(12) . . . . ?
C23 C24 C25 C26 -178.5(11) . . . . ?
C23 C24 C29 C28 176.3(10) . . . . ?
C24 C25 C26 C27 3(2) . . . . ?
C25 C24 C29 C28 -0.2(17) . . . . ?
C25 C26 C27 O4 -177.1(11) . . . . ?
C25 C26 C27 C28 -1(2) . . . . ?
C26 C27 C28 C29 -0.9(19) . . . . ?
C27 O4 C30 C31 171.3(9) . . . . ?
C27 C28 C29 C24 1.6(18) . . . . ?
C29 C24 C25 C26 -1.9(18) . . . . ?
C30 O4 C27 C26 -154.5(11) . . . . ?
C30 O4 C27 C28 29.8(16) . . . . ?
C30 C31 C32 O5 -59.1(12) . . . . ?
C32 O5 C33 C34 15.1(13) . . . . ?
C32 O5 C33 C38 -167.9(9) . . . . ?
C33 O5 C32 C31 166.3(8) . . . . ?
C33 C34 C35 C36 -0.9(13) . . . . ?
C33 C34 C35 C41 176.0(7) . . . . ?
C34 C33 C38 O6 176.1(8) . . . . ?
C34 C33 C38 C37 -1.5(15) . . . . ?
C34 C35 C36 C20 178.1(8) . . . . ?
C34 C35 C36 C37 -1.1(13) . . . . ?
C34 C35 C41 C57 -77.5(9) . . . . ?
C35 C36 C37 C38 1.8(14) . . . . ?
C35 C41 C57 C56 -90.1(10) . . . . ?
C35 C41 C57 C58 88.0(9) . . . . ?
C36 C35 C41 C57 99.4(10) . . . . ?
C36 C37 C38 O6 -178.0(9) . . . . ?
C36 C37 C38 C33 -0.5(16) . . . . ?
C38 C33 C34 C35 2.3(13) . . . . ?
C41 C35 C36 C20 1.3(13) . . . . ?
C41 C35 C36 C37 -177.8(8) . . . . ?
C41 C57 C58 C59 -175.6(7) . . . . ?
C42 N1 C1 C2 161.7(7) . . . . ?
C42 N1 C21 C22 -110.0(9) . . . . ?
C43 N4 C44 C45 175.4(8) . . . . ?
C44 N4 C43 C42 172.7(8) . . . . ?
C44 C45 C46 C47 179.2(9) . . . . ?
C44 C45 C50 C49 -179.1(9) . . . . ?
C45 C46 C47 C48 0.0(16) . . . . ?
C46 C45 C50 C49 1.9(16) . . . . ?
C46 C47 C48 O7 -177.9(9) . . . . ?
C46 C47 C48 C49 1.8(15) . . . . ?
C47 C48 C49 C50 -1.8(16) . . . . ?
C48 O7 C51 C52 -169.9(8) . . . . ?
C48 C49 C50 C45 -0.1(17) . . . . ?
C50 C45 C46 C47 -1.8(16) . . . . ?
C51 O7 C48 C47 177.7(8) . . . . ?
C51 O7 C48 C49 -1.9(14) . . . . ?
C51 C52 C53 O8 -70.4(10) . . . . ?
C53 O8 C54 C55 1.8(13) . . . . ?
C53 O8 C54 C59 -178.4(7) . . . . ?
C54 O8 C53 C52 -178.7(7) . . . . ?
C54 C55 C56 C57 0.5(11) . . . . ?
C54 C55 C56 C61 -175.9(7) . . . . ?
C55 C54 C59 O9 177.7(7) . . . . ?
C55 C54 C59 C58 -0.7(12) . . . . ?
C55 C56 C57 C41 175.8(7) . . . . ?
C55 C56 C57 C58 -2.2(11) . . . . ?
C55 C56 C61 C16 -84.5(9) . . . . ?
C56 C57 C58 C59 2.5(12) . . . . ?
C57 C56 C61 C16 99.4(9) . . . . ?
C57 C58 C59 O9 -179.2(8) . . . . ?
C57 C58 C59 C54 -1.0(13) . . . . ?
C59 C54 C55 C56 1.0(12) . . . . ?
C60 O9 C59 C54 -171.6(8) . . . . ?
C60 O9 C59 C58 6.7(13) . . . . ?
C61 C16 C17 C18 -179.7(8) . . . . ?
C61 C56 C57 C41 -8.0(11) . . . . ?
C61 C56 C57 C58 174.0(7) . . . . ?
C40 O6 C38 C33 156.0(13) . . . . ?
C40 O6 C38 C37 -26.4(18) . . . . ?
C39 O6 C38 C33 71(3) . . . . ?
C39 O6 C38 C37 -111(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.306 0.000 0.000 342.1 71.4 ?
2 -0.481 0.500 0.500 342.1 71.4 ?
3 0.047 0.450 0.129 9.9 0.0 ?
4 -0.047 0.550 0.871 9.9 0.0 ?
5 0.453 0.950 0.371 9.9 0.0 ?
6 0.547 0.050 0.629 9.9 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.192
_oxdiff_exptl_absorpt_empirical_full_min 0.581
####################################################################### 
# 
# 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_lcycage4php
_database_code_depnum_ccdc_archive 'CCDC 2093016'
loop_
_audit_author_name
_audit_author_address
lcycage
;ecolecentrale de marseille
France
;
_audit_update_record             
;
2021-06-29 deposited with the CCDC.	2022-02-03 downloaded from the CCDC.
;
_audit_creation_date             2021-06-10
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '1(Cl), C54 H58 N4 O9 P, C4 H10 O'
_chemical_formula_sum            'C58 H68 Cl N4 O10 P'
_chemical_formula_weight         1047.58
_chemical_melting_point          ?
_chemical_oxdiff_formula         'c54 h58 Cl1 n4 o9 p1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.2610(2)
_cell_length_b                   10.87103(19)
_cell_length_c                   26.4434(4)
_cell_angle_alpha                82.7150(14)
_cell_angle_beta                 86.3036(16)
_cell_angle_gamma                77.2137(17)
_cell_volume                     2851.32(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    26744
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      70.8770
_cell_measurement_theta_min      3.3770
_shelx_estimated_absorpt_T_max   0.924
_shelx_estimated_absorpt_T_min   0.739
_exptl_absorpt_coefficient_mu    1.340
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.106a (Rigaku Oxford Diffraction, 2021)
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    1.220
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            49135
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.883
_diffrn_reflns_theta_min         3.372
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      7.00  48.00   1.00    2.00    --    0.00-104.00  54.00   41
  2  ω    -31.00  11.00   1.00    2.00    --    0.00 104.00 155.00   42
  3  ω   -143.00 -96.00   1.00    5.00    --  -54.36-104.00  54.00   47
  4  ω     38.00 105.00   1.00    5.00    --   54.36-104.00  54.00   67
  5  ω     58.00 111.00   1.00   15.00    --  108.73-104.00  54.00   53
  6  ω    115.00 140.00   1.00   15.00    --  108.73 104.00 155.00   25
  7  ω     25.00  57.00   1.00   15.00    --  108.73-104.00  54.00   32
  8  ω    -86.00 -38.00   1.00    2.00    --    0.00 -38.00  90.00   48
  9  ω    -88.00  35.00   1.00    2.00    --    0.00 -57.00   0.00  123
 10  ω    -34.00  42.00   1.00    2.00    --    0.00 -38.00  90.00   76
 11  ω    -39.00 -11.00   1.00    2.00    --   14.00 127.00 -69.93   28
 12  ω    -37.00  -4.00   1.00    2.00    --   26.00 128.00 101.96   33
 13  ω      0.00  27.00   1.00    5.00    --   46.00  93.00-138.29   27
 14  ω     -2.00  23.00   1.00    5.00    --   46.00  95.00   2.70   25
 15  ω      7.00  33.00   1.00    5.00    --   50.00  88.00 154.33   26
 16  ω      6.00  31.00   1.00    5.00    --   50.00  87.00  76.74   25
 17  ω     12.00  37.00   1.00    5.00    --   54.00  83.00-173.33   25
 18  ω    -91.00  -3.00   1.00    5.00    --  -54.36 125.00-120.00   88
 19  ω    -55.00 -29.00   1.00    5.00    --  -54.36 104.00 155.00   26
 20  ω     12.00  37.00   1.00    5.00    --   54.36  84.00 -95.06   25
 21  ω     13.00  40.00   1.00    5.00    --   54.36  83.00  31.57   27
 22  ω     15.00  42.00   1.00    5.00    --   54.36  57.00 -90.00   27
 23  ω     48.00 141.00   1.00    5.00    --   54.36  57.00 -90.00   93
 24  ω     17.00  44.00   1.00    5.00    --   58.00  82.00-165.92   27
 25  ω     16.00  42.00   1.00    5.00    --   58.00  82.00 112.19   26
 26  ω     16.00  43.00   1.00    5.00    --   58.00  82.00 -54.22   27
 27  ω     17.00  44.00   1.00    5.00    --   58.00  82.00 -91.57   27
 28  ω     25.00 162.00   1.00    5.00    --   66.00  76.00  -2.28  137
 29  ω     29.00 165.00   1.00    5.00    --   70.00  75.00 119.65  136
 30  ω     29.00  55.00   1.00    5.00    --   70.00  75.00 175.39   26
 31  ω     66.00 165.00   1.00    5.00    --   70.00  75.00 175.39   99
 32  ω     35.00  62.00   1.00    5.00    --   74.00  75.00  12.50   27
 33  ω     33.00 117.00   1.00    5.00    --   74.00  77.00  64.85   84
 34  ω     34.00  60.00   1.00    5.00    --   74.00  73.00-106.56   26
 35  ω    129.00 156.00   1.00    5.00    --   74.00  73.00-106.56   27
 36  ω     34.00  59.00   1.00    5.00    --   74.00  74.00 -74.98   25
 37  ω     33.00  59.00   1.00    5.00    --   74.00  74.00-126.98   26
 38  ω     37.00  66.00   1.00    5.00    --   78.00  75.00  47.27   29
 39  ω     39.00  65.00   1.00    5.00    --   78.00  69.00-147.17   26
 40  ω     41.00  68.00   1.00   15.00    --   82.00  73.00 -65.90   27
 41  ω     41.00  68.00   1.00   15.00    --   82.00  73.00 144.33   27
 42  ω     45.00  72.00   1.00   15.00    --   82.00  70.00 124.63   27
 43  ω     42.00  68.00   1.00   15.00    --   82.00  70.00-167.37   26
 44  ω     81.00 173.00   1.00   15.00    --   90.00  72.00 -39.62   92
 45  ω     49.00  76.00   1.00   15.00    --   90.00  67.00 -94.23   27
 46  ω     49.00  79.00   1.00   15.00    --   90.00  72.00 -39.62   30
 47  ω     49.00  76.00   1.00   15.00    --   90.00  73.00  32.15   27
 48  ω     49.00  81.00   1.00   15.00    --   90.00  76.00  84.44   32
 49  ω     49.00  80.00   1.00   15.00    --   90.00  73.00  -6.10   31
 50  ω     98.00 177.00   1.00   15.00    --   94.00  77.00-139.26   79
 51  ω     60.00  87.00   1.00   15.00    --   94.00  67.00-175.23   27
 52  ω     53.00  95.00   1.00   15.00    --   94.00  77.00-139.26   42
 53  ω     62.00  92.00   1.00   15.00    --  102.00  74.00  -7.27   30
 54  ω     61.00  87.00   1.00   15.00    --  102.00  76.00 -76.15   26
 55  ω    106.00 163.00   1.00   15.00    --  108.73  75.00-128.20   57
 56  ω     69.00  96.00   1.00   15.00    --  108.73  75.00-128.20   27
 57  ω     71.00 113.00   1.00   15.00    --  108.73  63.00 150.00   42
 58  ω     73.00 100.00   1.00   15.00    --  108.73  63.00 120.00   27
 59  ω     67.00 178.00   1.00   15.00    --  108.73  77.00  90.00  111
 60  ω     69.00 171.00   1.00   15.00    --  108.73  77.00   0.00  102
 61  ω     68.00 172.00   1.00   15.00    --  108.73  77.00 -60.00  104
 62  ω     21.00 112.00   1.00   15.00    --  108.73-111.00 -30.00   91
 63  ω    129.00 163.00   1.00   15.00    --  108.73 111.00-120.00   34
 64  ω     68.00 173.00   1.00   15.00    --  108.73  77.00-180.00  105
 65  ω     67.00 177.00   1.00   15.00    --  108.73  77.00  30.00  110
 66  ω     68.00 148.00   1.00   15.00    --  108.73  77.00-150.00   80
 67  ω     51.00 106.00   1.00   15.00    --  108.73-111.00 -90.00   55
 68  ω    101.00 178.00   1.00   15.00    --  108.73 111.00 120.00   77
 69  ω    151.00 176.00   1.00   15.00    --  108.73 111.00  30.00   25
 70  ω    141.00 168.00   1.00   15.00    --  108.73 111.00 -90.00   27
 71  ω     86.00 151.00   1.00   15.00    --  108.73 -91.00  90.00   65
 72  ω     26.00  85.00   1.00   15.00    --  108.73 -91.00  90.00   59
 73  ω    103.00 144.00   1.00   15.00    --  108.73  77.00 120.00   41
 74  ω     68.00 135.00   1.00   15.00    --  108.73  77.00 150.00   67
 75  ω     68.00 149.00   1.00   15.00    --  108.73  77.00  60.00   81
 76  ω     70.00 172.00   1.00   15.00    --  108.73  63.00 -90.00  102
 77  ω     68.00  94.00   1.00   15.00    --  108.73  63.00  60.00   26
 78  ω     68.00 176.00   1.00   15.00    --  108.73  63.00 -30.00  108
 79  ω     67.00  94.00   1.00   15.00    --  108.73  77.00 120.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1094013000
_diffrn_orient_matrix_UB_12      0.0761521000
_diffrn_orient_matrix_UB_13      -0.0149860000
_diffrn_orient_matrix_UB_21      0.0519114000
_diffrn_orient_matrix_UB_22      -0.0328449000
_diffrn_orient_matrix_UB_23      0.0545114000
_diffrn_orient_matrix_UB_31      0.0952482000
_diffrn_orient_matrix_UB_32      -0.1205199000
_diffrn_orient_matrix_UB_33      -0.0160745000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9371
_reflns_number_total             10867
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.41.106a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.258
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         10867
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0641
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0978P)²+2.5631P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1779
_refine_ls_wR_factor_ref         0.1845
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All P(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C29-O5
 1.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O4: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
1.7A
4. Rigid body (RIGU) restrains
 O4, C28, O5, C29
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: Cl1(0.7) Cl2(0.2) Cl3(0.1)
6.a Riding coordinates:
 P1(H1)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C10(H10A,H10B), C18(H18A,H18B),
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C28(H28A,H28B), C36(H36A,H36B),
  C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C46(H46A,H46B), C54(H54A,
 H54B), C71(H71A,H71B), C73(H73A,H73B)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9), C12(H12), C15(H15), C23(H23), C24(H24),
 C26(H26), C27(H27), C30(H30), C33(H33), C41(H41), C42(H42), C44(H44), C45(H45),
  C48(H48), C51(H51)
6.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C35(H35A,H35B,H35C), C53(H53A,H53B,H53C), C72(H72A,H72B,
 H72C), C74(H74A,H74B,H74C)
;
_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
Cl1 Cl 0.2130(3) 0.2456(3) 0.01365(11) 0.1095(10) Uani 0.7 1 d . . P A 1
Cl2 Cl 0.1548(10) 0.1995(7) 0.0295(3) 0.092(3) Uani 0.2 1 d . . P B 2
P1 P 0.20201(6) 0.54488(6) 0.13279(2) 0.03170(16) Uani 1 1 d . . . . .
H1 H 0.285388 0.496122 0.169116 0.038 Uiso 1 1 d R U . . .
O1 O 0.18276(16) 0.41454(15) 0.38667(6) 0.0322(4) Uani 1 1 d . . . . .
O2 O 0.12885(16) 0.22274(15) 0.37101(6) 0.0315(4) Uani 1 1 d . . . . .
O3 O 0.17217(16) 0.00122(15) 0.33617(7) 0.0356(4) Uani 1 1 d . . . . .
O4 O 0.7625(2) 0.4227(2) 0.25799(9) 0.0543(5) Uani 1 1 d . . . . .
O5 O 0.7754(2) 0.49863(19) 0.33563(9) 0.0532(5) Uani 1 1 d D . . C 1
O6 O 0.54007(17) 0.56701(15) 0.39047(7) 0.0376(4) Uani 1 1 d . . . . .
O7 O 0.5196(2) -0.11075(19) 0.20232(10) 0.0600(6) Uani 1 1 d . . . . .
O8 O 0.74054(18) -0.18234(16) 0.22140(7) 0.0387(4) Uani 1 1 d . . . . .
O9 O 0.8941(2) -0.00957(19) 0.21210(9) 0.0533(5) Uani 1 1 d . . . . .
N1 N 0.0674(2) 0.6165(2) 0.08075(9) 0.0422(5) Uani 1 1 d . . . . .
N2 N 0.1533(2) 0.6829(2) 0.15641(8) 0.0381(5) Uani 1 1 d . . . . .
N3 N 0.3171(2) 0.5333(2) 0.08477(8) 0.0412(5) Uani 1 1 d . . . . .
N4 N 0.1153(2) 0.4322(2) 0.14857(9) 0.0410(5) Uani 1 1 d . . . . .
C1 C -0.0309(3) 0.7213(3) 0.10277(12) 0.0532(8) Uani 1 1 d . . . . .
H1A H -0.097358 0.686892 0.125879 0.064 Uiso 1 1 calc R U . . .
H1B H -0.078618 0.781848 0.075359 0.064 Uiso 1 1 calc R U . . .
C2 C 0.0519(3) 0.7858(3) 0.13189(11) 0.0506(7) Uani 1 1 d . . . . .
H2A H 0.094431 0.845106 0.108416 0.061 Uiso 1 1 calc R U . . .
H2B H -0.004520 0.833759 0.157744 0.061 Uiso 1 1 calc R U . . .
C3 C 0.2307(3) 0.7132(3) 0.19625(10) 0.0412(6) Uani 1 1 d . . . . .
H3A H 0.200003 0.804195 0.200845 0.049 Uiso 1 1 calc R U . . .
H3B H 0.326255 0.698668 0.185087 0.049 Uiso 1 1 calc R U . . .
C4 C 0.2163(2) 0.6337(2) 0.24686(9) 0.0324(5) Uani 1 1 d . . . . .
C5 C 0.0917(2) 0.6382(2) 0.27143(9) 0.0321(5) Uani 1 1 d . . . . .
H5 H 0.015054 0.692793 0.256365 0.039 Uiso 1 1 calc R U . . .
C6 C 0.0768(2) 0.5651(2) 0.31728(9) 0.0308(5) Uani 1 1 d . . . . .
H6 H -0.008878 0.570742 0.333920 0.037 Uiso 1 1 calc R U . . .
C7 C 0.1882(2) 0.4835(2) 0.33874(9) 0.0285(5) Uani 1 1 d . . . . .
C8 C 0.3124(2) 0.4764(3) 0.31478(10) 0.0392(6) Uani 1 1 d . . . . .
H8 H 0.388560 0.419889 0.329363 0.047 Uiso 1 1 calc R U . . .
C9 C 0.3258(3) 0.5520(3) 0.26930(10) 0.0421(6) Uani 1 1 d . . . . .
H9 H 0.411936 0.547658 0.253193 0.051 Uiso 1 1 calc R U . . .
C10 C 0.0919(2) 0.3332(2) 0.39633(9) 0.0301(5) Uani 1 1 d . . . . .
H10A H 0.002299 0.380579 0.385416 0.036 Uiso 1 1 calc R U . . .
H10B H 0.085215 0.307533 0.433524 0.036 Uiso 1 1 calc R U . . .
C11 C 0.2458(2) 0.1379(2) 0.38517(9) 0.0278(5) Uani 1 1 d . . . . .
C12 C 0.3376(2) 0.1602(2) 0.41651(9) 0.0288(5) Uani 1 1 d . . . . .
H12 H 0.316633 0.235283 0.433002 0.035 Uiso 1 1 calc R U . . .
C13 C 0.4614(2) 0.0760(2) 0.42504(9) 0.0281(5) Uani 1 1 d . . . . .
C14 C 0.4905(2) -0.0351(2) 0.40129(9) 0.0289(5) Uani 1 1 d . . . . .
C15 C 0.3930(2) -0.0610(2) 0.37215(9) 0.0301(5) Uani 1 1 d . . . . .
H15 H 0.411145 -0.138645 0.357471 0.036 Uiso 1 1 calc R U . . .
C16 C 0.2710(2) 0.0223(2) 0.36384(9) 0.0283(5) Uani 1 1 d . . . . .
C17 C 0.1966(3) -0.1175(2) 0.31561(11) 0.0398(6) Uani 1 1 d . . . . .
H17A H 0.273481 -0.123083 0.291385 0.060 Uiso 1 1 calc R U . . .
H17B H 0.117489 -0.123696 0.298014 0.060 Uiso 1 1 calc R U . . .
H17C H 0.215470 -0.187105 0.343331 0.060 Uiso 1 1 calc R U . . .
C18 C 0.5588(2) 0.1182(2) 0.45648(9) 0.0320(5) Uani 1 1 d . . . . .
H18A H 0.510731 0.154089 0.486773 0.038 Uiso 1 1 calc R U . . .
H18B H 0.629043 0.043934 0.468535 0.038 Uiso 1 1 calc R U . . .
C19 C 0.1409(4) 0.6624(3) 0.03508(11) 0.0572(8) Uani 1 1 d . . . . .
H19A H 0.155648 0.748101 0.038021 0.069 Uiso 1 1 calc R U . . .
H19B H 0.090127 0.666477 0.004095 0.069 Uiso 1 1 calc R U . . .
C20 C 0.2734(4) 0.5677(3) 0.03233(11) 0.0564(8) Uani 1 1 d . . . . .
H20A H 0.262153 0.491673 0.017528 0.068 Uiso 1 1 calc R U . . .
H20B H 0.339872 0.606346 0.010883 0.068 Uiso 1 1 calc R U . . .
C21 C 0.4410(3) 0.4338(3) 0.08947(12) 0.0520(7) Uani 1 1 d . . . . .
H21A H 0.496953 0.443040 0.057874 0.062 Uiso 1 1 calc R U . . .
H21B H 0.416682 0.349994 0.091732 0.062 Uiso 1 1 calc R U . . .
C22 C 0.5245(3) 0.4340(3) 0.13452(11) 0.0408(6) Uani 1 1 d . . . . .
C23 C 0.5698(3) 0.5409(3) 0.14249(11) 0.0427(6) Uani 1 1 d . . . . .
H23 H 0.546564 0.616253 0.119550 0.051 Uiso 1 1 calc R U . . .
C24 C 0.6481(3) 0.5396(3) 0.18325(11) 0.0408(6) Uani 1 1 d . . . . .
H24 H 0.678241 0.613562 0.188232 0.049 Uiso 1 1 calc R U . . .
C25 C 0.6825(2) 0.4299(2) 0.21683(11) 0.0395(6) Uani 1 1 d . . . . .
C26 C 0.6387(3) 0.3225(3) 0.20945(12) 0.0460(7) Uani 1 1 d . . . . .
H26 H 0.662551 0.247041 0.232327 0.055 Uiso 1 1 calc R U . . .
C27 C 0.5598(3) 0.3250(3) 0.16848(13) 0.0474(7) Uani 1 1 d . . . . .
H27 H 0.529515 0.251029 0.163622 0.057 Uiso 1 1 calc R U . . .
C28 C 0.7265(3) 0.5314(3) 0.28941(14) 0.0570(7) Uani 1 1 d . . . C 1
H28A H 0.762497 0.603832 0.272172 0.068 Uiso 1 1 calc R U . C 1
H28B H 0.627980 0.558961 0.292454 0.068 Uiso 1 1 calc R U . C 1
C29 C 0.7168(3) 0.4070(2) 0.36284(12) 0.0440(6) Uani 1 1 d D . . . .
C30 C 0.7843(3) 0.2826(2) 0.36465(12) 0.0412(6) Uani 1 1 d . . . . .
H30 H 0.863759 0.262019 0.344134 0.049 Uiso 1 1 calc R U . . .
C31 C 0.7401(2) 0.1865(2) 0.39539(10) 0.0331(5) Uani 1 1 d . . . . .
C32 C 0.6229(2) 0.2169(2) 0.42529(9) 0.0298(5) Uani 1 1 d . . . . .
C33 C 0.5564(2) 0.3449(2) 0.42418(9) 0.0295(5) Uani 1 1 d . . . . .
H33 H 0.478513 0.366241 0.445470 0.035 Uiso 1 1 calc R U . . .
C34 C 0.6005(2) 0.4406(2) 0.39323(10) 0.0327(5) Uani 1 1 d . . . . .
C35 C 0.4258(3) 0.5996(2) 0.42387(11) 0.0394(6) Uani 1 1 d . . . . .
H35A H 0.355078 0.559231 0.415219 0.059 Uiso 1 1 calc R U . . .
H35B H 0.393497 0.692010 0.420088 0.059 Uiso 1 1 calc R U . . .
H35C H 0.450635 0.569949 0.459223 0.059 Uiso 1 1 calc R U . . .
C36 C 0.8228(2) 0.0516(2) 0.39454(11) 0.0381(6) Uani 1 1 d . . . . .
H36A H 0.918918 0.053744 0.393044 0.046 Uiso 1 1 calc R U . . .
H36B H 0.804143 -0.000231 0.426635 0.046 Uiso 1 1 calc R U . . .
C37 C 0.0040(3) 0.5101(3) 0.07185(13) 0.0555(8) Uani 1 1 d . . . . .
H37A H 0.059132 0.457672 0.047029 0.067 Uiso 1 1 calc R U . . .
H37B H -0.086171 0.543979 0.058260 0.067 Uiso 1 1 calc R U . . .
C38 C -0.0050(3) 0.4325(3) 0.12245(14) 0.0561(8) Uani 1 1 d . . . . .
H38A H -0.085547 0.470527 0.142391 0.067 Uiso 1 1 calc R U . . .
H38B H -0.009981 0.344810 0.117699 0.067 Uiso 1 1 calc R U . . .
C39 C 0.1353(3) 0.3552(3) 0.19816(12) 0.0474(7) Uani 1 1 d . . . . .
H39A H 0.049390 0.333325 0.210788 0.057 Uiso 1 1 calc R U . . .
H39B H 0.160491 0.407008 0.222620 0.057 Uiso 1 1 calc R U . . .
C40 C 0.2412(3) 0.2337(2) 0.19743(10) 0.0391(6) Uani 1 1 d . . . . .
C41 C 0.3119(3) 0.1837(3) 0.24076(11) 0.0505(7) Uani 1 1 d . . . . .
H41 H 0.294606 0.227391 0.270225 0.061 Uiso 1 1 calc R U . . .
C42 C 0.4073(3) 0.0714(3) 0.24217(12) 0.0522(7) Uani 1 1 d . . . . .
H42 H 0.456573 0.039190 0.271981 0.063 Uiso 1 1 calc R U . . .
C43 C 0.4300(3) 0.0070(2) 0.19962(12) 0.0453(7) Uani 1 1 d . . . . .
C44 C 0.3621(3) 0.0549(3) 0.15599(12) 0.0437(6) Uani 1 1 d . . . . .
H44 H 0.378939 0.010221 0.126801 0.052 Uiso 1 1 calc R U . . .
C45 C 0.2683(3) 0.1694(3) 0.15463(11) 0.0407(6) Uani 1 1 d . . . . .
H45 H 0.222583 0.203714 0.124171 0.049 Uiso 1 1 calc R U . . .
C46 C 0.6519(3) -0.1094(3) 0.18477(12) 0.0469(7) Uani 1 1 d . . . . .
H46A H 0.664819 -0.021048 0.179430 0.056 Uiso 1 1 calc R U . . .
H46B H 0.670121 -0.145392 0.151816 0.056 Uiso 1 1 calc R U . . .
C47 C 0.7536(2) -0.1209(2) 0.26357(10) 0.0340(5) Uani 1 1 d . . . . .
C48 C 0.6921(2) -0.1515(2) 0.30973(10) 0.0325(5) Uani 1 1 d . . . . .
H48 H 0.636941 -0.211821 0.312146 0.039 Uiso 1 1 calc R U . . .
C49 C 0.7086(2) -0.0962(2) 0.35340(10) 0.0313(5) Uani 1 1 d . . . . .
C50 C 0.7935(2) -0.0115(2) 0.34947(10) 0.0336(5) Uani 1 1 d . . . . .
C51 C 0.8559(2) 0.0191(2) 0.30235(11) 0.0383(6) Uani 1 1 d . . . . .
H51 H 0.913166 0.077552 0.299913 0.046 Uiso 1 1 calc R U . . .
C52 C 0.8363(2) -0.0337(2) 0.25912(11) 0.0379(6) Uani 1 1 d . . . . .
C53 C 0.9747(3) 0.0834(3) 0.20530(14) 0.0570(8) Uani 1 1 d . . . . .
H53A H 1.007282 0.092932 0.169671 0.085 Uiso 1 1 calc R U . . .
H53B H 1.050915 0.056187 0.227605 0.085 Uiso 1 1 calc R U . . .
H53C H 0.921034 0.164982 0.213969 0.085 Uiso 1 1 calc R U . . .
C54 C 0.6265(2) -0.1261(2) 0.40134(10) 0.0328(5) Uani 1 1 d . . . . .
H54A H 0.674730 -0.119116 0.431718 0.039 Uiso 1 1 calc R U . . .
H54B H 0.614184 -0.214435 0.403265 0.039 Uiso 1 1 calc R U . . .
O70 O 0.0642(2) 0.29623(18) 0.52758(7) 0.0432(4) Uani 1 1 d . . . . .
C71 C 0.1126(3) 0.3846(3) 0.55212(10) 0.0424(6) Uani 1 1 d . . . . .
H71A H 0.147440 0.344274 0.585683 0.051 Uiso 1 1 calc R U . . .
H71B H 0.039180 0.458159 0.557807 0.051 Uiso 1 1 calc R U . . .
C72 C 0.2220(3) 0.4281(3) 0.51921(11) 0.0488(7) Uani 1 1 d . . . . .
H72A H 0.297247 0.355894 0.515872 0.073 Uiso 1 1 calc R U . . .
H72B H 0.251937 0.493571 0.534867 0.073 Uiso 1 1 calc R U . . .
H72C H 0.188351 0.463260 0.485383 0.073 Uiso 1 1 calc R U . . .
C73 C -0.0399(3) 0.2499(3) 0.55635(12) 0.0468(7) Uani 1 1 d . . . . .
H73A H -0.109759 0.321938 0.566619 0.056 Uiso 1 1 calc R U . . .
H73B H -0.004065 0.196493 0.587633 0.056 Uiso 1 1 calc R U . . .
C74 C -0.0985(4) 0.1738(4) 0.52468(15) 0.0673(9) Uani 1 1 d . . . . .
H74A H -0.141294 0.229115 0.495446 0.101 Uiso 1 1 calc R U . . .
H74B H -0.165339 0.135499 0.545261 0.101 Uiso 1 1 calc R U . . .
H74C H -0.027665 0.106733 0.512459 0.101 Uiso 1 1 calc R U . . .
Cl3 Cl 0.1055(16) 0.0364(15) 0.0410(7) 0.134(7) Uani 0.1 1 d . . P D 3


_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 H1 1.3084 . ?
P1 N1 1.976(2) . ?
P1 N2 1.660(2) . ?
P1 N3 1.675(2) . ?
P1 N4 1.665(2) . ?
O1 C7 1.393(3) . ?
O1 C10 1.412(3) . ?
O2 C10 1.415(3) . ?
O2 C11 1.382(3) . ?
O3 C16 1.363(3) . ?
O3 C17 1.429(3) . ?
O4 C25 1.390(3) . ?
O4 C28 1.497(4) . ?
O5 C28 1.327(4) . ?
O5 C29 1.378(3) . ?
O6 C34 1.372(3) . ?
O6 C35 1.429(3) . ?
O7 C43 1.397(3) . ?
O7 C46 1.409(4) . ?
O8 C46 1.412(3) . ?
O8 C47 1.399(3) . ?
O9 C52 1.363(3) . ?
O9 C53 1.429(3) . ?
N1 C1 1.496(3) . ?
N1 C19 1.474(4) . ?
N1 C37 1.496(4) . ?
N2 C2 1.464(4) . ?
N2 C3 1.470(3) . ?
N3 C20 1.462(4) . ?
N3 C21 1.476(4) . ?
N4 C38 1.452(4) . ?
N4 C39 1.464(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.513(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.516(4) . ?
C4 C5 1.391(3) . ?
C4 C9 1.383(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.382(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.387(3) . ?
C7 C8 1.377(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.385(4) . ?
C9 H9 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.374(3) . ?
C11 C16 1.408(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.405(3) . ?
C13 C14 1.397(3) . ?
C13 C18 1.519(3) . ?
C14 C15 1.397(3) . ?
C14 C54 1.521(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.385(3) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C32 1.510(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.516(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.512(4) . ?
C22 C23 1.387(4) . ?
C22 C27 1.387(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.382(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.386(4) . ?
C25 C26 1.380(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.388(4) . ?
C27 H27 0.9500 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.373(4) . ?
C29 C34 1.401(4) . ?
C30 H30 0.9500 . ?
C30 C31 1.380(4) . ?
C31 C32 1.396(3) . ?
C31 C36 1.525(3) . ?
C32 C33 1.405(3) . ?
C33 H33 0.9500 . ?
C33 C34 1.378(3) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C50 1.525(4) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.498(5) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.515(4) . ?
C40 C41 1.382(4) . ?
C40 C45 1.386(4) . ?
C41 H41 0.9500 . ?
C41 C42 1.384(5) . ?
C42 H42 0.9500 . ?
C42 C43 1.380(5) . ?
C43 C44 1.371(4) . ?
C44 H44 0.9500 . ?
C44 C45 1.393(4) . ?
C45 H45 0.9500 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.375(4) . ?
C47 C52 1.395(3) . ?
C48 H48 0.9500 . ?
C48 C49 1.404(4) . ?
C49 C50 1.392(3) . ?
C49 C54 1.517(4) . ?
C50 C51 1.400(4) . ?
C51 H51 0.9500 . ?
C51 C52 1.387(4) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
O70 C71 1.415(3) . ?
O70 C73 1.417(4) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C71 C72 1.498(4) . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C73 C74 1.486(5) . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 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
N1 P1 H1 176.6 . . ?
N2 P1 H1 93.6 . . ?
N2 P1 N1 85.76(10) . . ?
N2 P1 N3 118.56(12) . . ?
N2 P1 N4 119.46(12) . . ?
N3 P1 H1 96.1 . . ?
N3 P1 N1 87.15(11) . . ?
N4 P1 H1 91.3 . . ?
N4 P1 N1 86.19(11) . . ?
N4 P1 N3 120.79(12) . . ?
C7 O1 C10 119.26(17) . . ?
C11 O2 C10 117.20(17) . . ?
C16 O3 C17 116.72(18) . . ?
C25 O4 C28 115.7(2) . . ?
C28 O5 C29 111.1(2) . . ?
C34 O6 C35 116.17(19) . . ?
C43 O7 C46 116.2(2) . . ?
C47 O8 C46 114.78(19) . . ?
C52 O9 C53 118.2(2) . . ?
C1 N1 P1 106.78(17) . . ?
C19 N1 P1 106.37(19) . . ?
C19 N1 C1 112.6(2) . . ?
C19 N1 C37 112.6(2) . . ?
C37 N1 P1 106.11(17) . . ?
C37 N1 C1 111.9(2) . . ?
C2 N2 P1 121.47(18) . . ?
C2 N2 C3 117.7(2) . . ?
C3 N2 P1 119.67(18) . . ?
C20 N3 P1 119.0(2) . . ?
C20 N3 C21 113.4(2) . . ?
C21 N3 P1 120.1(2) . . ?
C38 N4 P1 121.2(2) . . ?
C38 N4 C39 117.2(2) . . ?
C39 N4 P1 119.0(2) . . ?
N1 C1 H1A 110.7 . . ?
N1 C1 H1B 110.7 . . ?
N1 C1 C2 105.2(2) . . ?
H1A C1 H1B 108.8 . . ?
C2 C1 H1A 110.7 . . ?
C2 C1 H1B 110.7 . . ?
N2 C2 C1 105.3(2) . . ?
N2 C2 H2A 110.7 . . ?
N2 C2 H2B 110.7 . . ?
C1 C2 H2A 110.7 . . ?
C1 C2 H2B 110.7 . . ?
H2A C2 H2B 108.8 . . ?
N2 C3 H3A 109.2 . . ?
N2 C3 H3B 109.2 . . ?
N2 C3 C4 112.3(2) . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
C5 C4 C3 120.8(2) . . ?
C9 C4 C3 121.2(2) . . ?
C9 C4 C5 118.0(2) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 C4 121.5(2) . . ?
C6 C5 H5 119.3 . . ?
C5 C6 H6 120.4 . . ?
C5 C6 C7 119.3(2) . . ?
C7 C6 H6 120.4 . . ?
C6 C7 O1 122.4(2) . . ?
C8 C7 O1 117.1(2) . . ?
C8 C7 C6 120.3(2) . . ?
C7 C8 H8 120.2 . . ?
C7 C8 C9 119.7(2) . . ?
C9 C8 H8 120.2 . . ?
C4 C9 C8 121.3(2) . . ?
C4 C9 H9 119.3 . . ?
C8 C9 H9 119.3 . . ?
O1 C10 O2 113.38(18) . . ?
O1 C10 H10A 108.9 . . ?
O1 C10 H10B 108.9 . . ?
O2 C10 H10A 108.9 . . ?
O2 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
O2 C11 C16 115.6(2) . . ?
C12 C11 O2 125.1(2) . . ?
C12 C11 C16 119.3(2) . . ?
C11 C12 H12 118.8 . . ?
C11 C12 C13 122.3(2) . . ?
C13 C12 H12 118.8 . . ?
C12 C13 C18 116.8(2) . . ?
C14 C13 C12 118.5(2) . . ?
C14 C13 C18 124.6(2) . . ?
C13 C14 C15 118.8(2) . . ?
C13 C14 C54 124.2(2) . . ?
C15 C14 C54 116.8(2) . . ?
C14 C15 H15 118.7 . . ?
C16 C15 C14 122.5(2) . . ?
C16 C15 H15 118.7 . . ?
O3 C16 C11 116.77(19) . . ?
O3 C16 C15 124.9(2) . . ?
C15 C16 C11 118.3(2) . . ?
O3 C17 H17A 109.5 . . ?
O3 C17 H17B 109.5 . . ?
O3 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C32 C18 C13 110.81(19) . . ?
C32 C18 H18A 109.5 . . ?
C32 C18 H18B 109.5 . . ?
N1 C19 H19A 110.5 . . ?
N1 C19 H19B 110.5 . . ?
N1 C19 C20 106.2(2) . . ?
H19A C19 H19B 108.7 . . ?
C20 C19 H19A 110.5 . . ?
C20 C19 H19B 110.5 . . ?
N3 C20 C19 106.3(2) . . ?
N3 C20 H20A 110.5 . . ?
N3 C20 H20B 110.5 . . ?
C19 C20 H20A 110.5 . . ?
C19 C20 H20B 110.5 . . ?
H20A C20 H20B 108.7 . . ?
N3 C21 H21A 108.3 . . ?
N3 C21 H21B 108.3 . . ?
N3 C21 C22 115.8(2) . . ?
H21A C21 H21B 107.4 . . ?
C22 C21 H21A 108.3 . . ?
C22 C21 H21B 108.3 . . ?
C23 C22 C21 121.5(3) . . ?
C27 C22 C21 120.1(3) . . ?
C27 C22 C23 118.4(3) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 C22 121.1(3) . . ?
C24 C23 H23 119.4 . . ?
C23 C24 H24 120.1 . . ?
C23 C24 C25 119.7(3) . . ?
C25 C24 H24 120.1 . . ?
C24 C25 O4 122.2(2) . . ?
C26 C25 O4 117.8(2) . . ?
C26 C25 C24 120.0(3) . . ?
C25 C26 H26 120.1 . . ?
C25 C26 C27 119.7(3) . . ?
C27 C26 H26 120.1 . . ?
C22 C27 C26 121.0(3) . . ?
C22 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
O4 C28 H28A 109.4 . . ?
O4 C28 H28B 109.4 . . ?
O5 C28 O4 111.0(2) . . ?
O5 C28 H28A 109.4 . . ?
O5 C28 H28B 109.4 . . ?
H28A C28 H28B 108.0 . . ?
O5 C29 C34 121.0(2) . . ?
C30 C29 O5 118.2(2) . . ?
C30 C29 C34 120.3(2) . . ?
C29 C30 H30 119.0 . . ?
C29 C30 C31 122.0(2) . . ?
C31 C30 H30 119.0 . . ?
C30 C31 C32 118.9(2) . . ?
C30 C31 C36 117.7(2) . . ?
C32 C31 C36 123.4(2) . . ?
C31 C32 C18 123.2(2) . . ?
C31 C32 C33 118.7(2) . . ?
C33 C32 C18 118.0(2) . . ?
C32 C33 H33 118.9 . . ?
C34 C33 C32 122.2(2) . . ?
C34 C33 H33 118.9 . . ?
O6 C34 C29 117.2(2) . . ?
O6 C34 C33 124.9(2) . . ?
C33 C34 C29 117.9(2) . . ?
O6 C35 H35A 109.5 . . ?
O6 C35 H35B 109.5 . . ?
O6 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C31 C36 H36A 109.0 . . ?
C31 C36 H36B 109.0 . . ?
H36A C36 H36B 107.8 . . ?
C50 C36 C31 112.9(2) . . ?
C50 C36 H36A 109.0 . . ?
C50 C36 H36B 109.0 . . ?
N1 C37 H37A 110.4 . . ?
N1 C37 H37B 110.4 . . ?
N1 C37 C38 106.6(2) . . ?
H37A C37 H37B 108.6 . . ?
C38 C37 H37A 110.4 . . ?
C38 C37 H37B 110.4 . . ?
N4 C38 C37 106.3(2) . . ?
N4 C38 H38A 110.5 . . ?
N4 C38 H38B 110.5 . . ?
C37 C38 H38A 110.5 . . ?
C37 C38 H38B 110.5 . . ?
H38A C38 H38B 108.7 . . ?
N4 C39 H39A 108.7 . . ?
N4 C39 H39B 108.7 . . ?
N4 C39 C40 114.4(2) . . ?
H39A C39 H39B 107.6 . . ?
C40 C39 H39A 108.7 . . ?
C40 C39 H39B 108.7 . . ?
C41 C40 C39 119.5(3) . . ?
C41 C40 C45 118.6(3) . . ?
C45 C40 C39 121.9(3) . . ?
C40 C41 H41 119.3 . . ?
C40 C41 C42 121.4(3) . . ?
C42 C41 H41 119.3 . . ?
C41 C42 H42 120.5 . . ?
C43 C42 C41 119.0(3) . . ?
C43 C42 H42 120.5 . . ?
C42 C43 O7 118.9(3) . . ?
C44 C43 O7 120.3(3) . . ?
C44 C43 C42 120.7(3) . . ?
C43 C44 H44 120.1 . . ?
C43 C44 C45 119.7(3) . . ?
C45 C44 H44 120.1 . . ?
C40 C45 C44 120.4(3) . . ?
C40 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
O7 C46 O8 108.9(2) . . ?
O7 C46 H46A 109.9 . . ?
O7 C46 H46B 109.9 . . ?
O8 C46 H46A 109.9 . . ?
O8 C46 H46B 109.9 . . ?
H46A C46 H46B 108.3 . . ?
C48 C47 O8 120.4(2) . . ?
C48 C47 C52 120.3(2) . . ?
C52 C47 O8 119.2(2) . . ?
C47 C48 H48 119.1 . . ?
C47 C48 C49 121.8(2) . . ?
C49 C48 H48 119.1 . . ?
C48 C49 C54 118.0(2) . . ?
C50 C49 C48 118.2(2) . . ?
C50 C49 C54 123.7(2) . . ?
C49 C50 C36 123.1(2) . . ?
C49 C50 C51 119.7(2) . . ?
C51 C50 C36 117.3(2) . . ?
C50 C51 H51 119.2 . . ?
C52 C51 C50 121.7(2) . . ?
C52 C51 H51 119.2 . . ?
O9 C52 C47 116.4(2) . . ?
O9 C52 C51 125.2(2) . . ?
C51 C52 C47 118.4(2) . . ?
O9 C53 H53A 109.5 . . ?
O9 C53 H53B 109.5 . . ?
O9 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C14 C54 H54A 109.5 . . ?
C14 C54 H54B 109.5 . . ?
C49 C54 C14 110.61(18) . . ?
C49 C54 H54A 109.5 . . ?
C49 C54 H54B 109.5 . . ?
H54A C54 H54B 108.1 . . ?
C71 O70 C73 112.6(2) . . ?
O70 C71 H71A 109.9 . . ?
O70 C71 H71B 109.9 . . ?
O70 C71 C72 109.0(2) . . ?
H71A C71 H71B 108.3 . . ?
C72 C71 H71A 109.9 . . ?
C72 C71 H71B 109.9 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72B 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
O70 C73 H73A 109.9 . . ?
O70 C73 H73B 109.9 . . ?
O70 C73 C74 109.0(3) . . ?
H73A C73 H73B 108.3 . . ?
C74 C73 H73A 109.9 . . ?
C74 C73 H73B 109.9 . . ?
C73 C74 H74A 109.5 . . ?
C73 C74 H74B 109.5 . . ?
C73 C74 H74C 109.5 . . ?
H74A C74 H74B 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 N1 C1 C2 38.2(3) . . . . ?
P1 N1 C19 C20 36.9(3) . . . . ?
P1 N1 C37 C38 36.3(3) . . . . ?
P1 N2 C2 C1 25.2(3) . . . . ?
P1 N2 C3 C4 -70.5(3) . . . . ?
P1 N3 C20 C19 26.1(4) . . . . ?
P1 N3 C21 C22 -57.0(3) . . . . ?
P1 N4 C38 C37 22.0(3) . . . . ?
P1 N4 C39 C40 -91.9(3) . . . . ?
O1 C7 C8 C9 -174.0(2) . . . . ?
O2 C11 C12 C13 -172.9(2) . . . . ?
O2 C11 C16 O3 -6.6(3) . . . . ?
O2 C11 C16 C15 173.2(2) . . . . ?
O4 C25 C26 C27 -179.3(3) . . . . ?
O5 C29 C30 C31 172.9(3) . . . . ?
O5 C29 C34 O6 6.7(4) . . . . ?
O5 C29 C34 C33 -172.3(3) . . . . ?
O7 C43 C44 C45 176.9(2) . . . . ?
O8 C47 C48 C49 176.8(2) . . . . ?
O8 C47 C52 O9 3.4(3) . . . . ?
O8 C47 C52 C51 -175.2(2) . . . . ?
N1 P1 N2 C2 -2.3(2) . . . . ?
N1 P1 N2 C3 -169.8(2) . . . . ?
N1 P1 N3 C20 -3.8(2) . . . . ?
N1 P1 N3 C21 -151.4(2) . . . . ?
N1 P1 N4 C38 -0.5(2) . . . . ?
N1 P1 N4 C39 -162.0(2) . . . . ?
N1 C1 C2 N2 -39.3(3) . . . . ?
N1 C19 C20 N3 -39.8(4) . . . . ?
N1 C37 C38 N4 -36.8(3) . . . . ?
N2 P1 N3 C20 -87.4(3) . . . . ?
N2 P1 N3 C21 125.0(2) . . . . ?
N2 P1 N4 C38 82.4(3) . . . . ?
N2 P1 N4 C39 -79.1(2) . . . . ?
N2 C3 C4 C5 -59.9(3) . . . . ?
N2 C3 C4 C9 118.3(3) . . . . ?
N3 P1 N2 C2 82.1(3) . . . . ?
N3 P1 N2 C3 -85.4(2) . . . . ?
N3 P1 N4 C38 -84.9(2) . . . . ?
N3 P1 N4 C39 113.6(2) . . . . ?
N3 C21 C22 C23 -56.0(4) . . . . ?
N3 C21 C22 C27 125.3(3) . . . . ?
N4 P1 N2 C2 -85.5(3) . . . . ?
N4 P1 N2 C3 107.0(2) . . . . ?
N4 P1 N3 C20 80.0(3) . . . . ?
N4 P1 N3 C21 -67.6(2) . . . . ?
N4 C39 C40 C41 150.9(3) . . . . ?
N4 C39 C40 C45 -30.2(4) . . . . ?
C1 N1 C19 C20 153.6(3) . . . . ?
C1 N1 C37 C38 -79.7(3) . . . . ?
C2 N2 C3 C4 121.5(3) . . . . ?
C3 N2 C2 C1 -167.1(2) . . . . ?
C3 C4 C5 C6 179.2(2) . . . . ?
C3 C4 C9 C8 -178.0(2) . . . . ?
C4 C5 C6 C7 -1.3(4) . . . . ?
C5 C4 C9 C8 0.2(4) . . . . ?
C5 C6 C7 O1 174.8(2) . . . . ?
C5 C6 C7 C8 0.6(3) . . . . ?
C6 C7 C8 C9 0.6(4) . . . . ?
C7 O1 C10 O2 71.7(2) . . . . ?
C7 C8 C9 C4 -1.0(4) . . . . ?
C9 C4 C5 C6 0.9(4) . . . . ?
C10 O1 C7 C6 56.4(3) . . . . ?
C10 O1 C7 C8 -129.2(2) . . . . ?
C10 O2 C11 C12 -9.4(3) . . . . ?
C10 O2 C11 C16 172.5(2) . . . . ?
C11 O2 C10 O1 64.7(3) . . . . ?
C11 C12 C13 C14 -1.0(3) . . . . ?
C11 C12 C13 C18 174.3(2) . . . . ?
C12 C11 C16 O3 175.2(2) . . . . ?
C12 C11 C16 C15 -5.0(3) . . . . ?
C12 C13 C14 C15 -3.1(3) . . . . ?
C12 C13 C14 C54 171.7(2) . . . . ?
C12 C13 C18 C32 -75.7(3) . . . . ?
C13 C14 C15 C16 3.2(3) . . . . ?
C13 C14 C54 C49 -94.9(3) . . . . ?
C13 C18 C32 C31 -88.7(3) . . . . ?
C13 C18 C32 C33 87.5(3) . . . . ?
C14 C13 C18 C32 99.3(3) . . . . ?
C14 C15 C16 O3 -179.4(2) . . . . ?
C14 C15 C16 C11 0.8(4) . . . . ?
C15 C14 C54 C49 80.0(3) . . . . ?
C16 C11 C12 C13 5.1(3) . . . . ?
C17 O3 C16 C11 -178.5(2) . . . . ?
C17 O3 C16 C15 1.7(3) . . . . ?
C18 C13 C14 C15 -178.1(2) . . . . ?
C18 C13 C14 C54 -3.3(4) . . . . ?
C18 C32 C33 C34 -174.0(2) . . . . ?
C19 N1 C1 C2 -78.2(3) . . . . ?
C19 N1 C37 C38 152.3(2) . . . . ?
C20 N3 C21 C22 153.7(3) . . . . ?
C21 N3 C20 C19 175.7(3) . . . . ?
C21 C22 C23 C24 -178.8(2) . . . . ?
C21 C22 C27 C26 178.6(3) . . . . ?
C22 C23 C24 C25 0.1(4) . . . . ?
C23 C22 C27 C26 -0.1(4) . . . . ?
C23 C24 C25 O4 179.0(2) . . . . ?
C23 C24 C25 C26 0.1(4) . . . . ?
C24 C25 C26 C27 -0.3(4) . . . . ?
C25 O4 C28 O5 159.0(2) . . . . ?
C25 C26 C27 C22 0.3(4) . . . . ?
C27 C22 C23 C24 -0.1(4) . . . . ?
C28 O4 C25 C24 46.6(4) . . . . ?
C28 O4 C25 C26 -134.4(3) . . . . ?
C28 O5 C29 C30 98.3(3) . . . . ?
C28 O5 C29 C34 -89.8(3) . . . . ?
C29 O5 C28 O4 -65.5(3) . . . . ?
C29 C30 C31 C32 0.4(4) . . . . ?
C29 C30 C31 C36 -179.9(3) . . . . ?
C30 C29 C34 O6 178.4(2) . . . . ?
C30 C29 C34 C33 -0.6(4) . . . . ?
C30 C31 C32 C18 174.2(2) . . . . ?
C30 C31 C32 C33 -2.0(3) . . . . ?
C30 C31 C36 C50 -81.6(3) . . . . ?
C31 C32 C33 C34 2.4(3) . . . . ?
C31 C36 C50 C49 -99.1(3) . . . . ?
C31 C36 C50 C51 80.8(3) . . . . ?
C32 C31 C36 C50 98.1(3) . . . . ?
C32 C33 C34 O6 -180.0(2) . . . . ?
C32 C33 C34 C29 -1.1(4) . . . . ?
C34 C29 C30 C31 1.0(4) . . . . ?
C35 O6 C34 C29 -176.7(2) . . . . ?
C35 O6 C34 C33 2.2(3) . . . . ?
C36 C31 C32 C18 -5.5(4) . . . . ?
C36 C31 C32 C33 178.3(2) . . . . ?
C36 C50 C51 C52 179.7(2) . . . . ?
C37 N1 C1 C2 153.9(3) . . . . ?
C37 N1 C19 C20 -78.9(3) . . . . ?
C38 N4 C39 C40 105.8(3) . . . . ?
C39 N4 C38 C37 -176.2(2) . . . . ?
C39 C40 C41 C42 178.5(3) . . . . ?
C39 C40 C45 C44 -177.1(3) . . . . ?
C40 C41 C42 C43 -1.4(5) . . . . ?
C41 C40 C45 C44 1.9(4) . . . . ?
C41 C42 C43 O7 -175.6(3) . . . . ?
C41 C42 C43 C44 1.9(4) . . . . ?
C42 C43 C44 C45 -0.6(4) . . . . ?
C43 O7 C46 O8 131.8(3) . . . . ?
C43 C44 C45 C40 -1.4(4) . . . . ?
C45 C40 C41 C42 -0.5(4) . . . . ?
C46 O7 C43 C42 -95.1(3) . . . . ?
C46 O7 C43 C44 87.4(3) . . . . ?
C46 O8 C47 C48 104.2(3) . . . . ?
C46 O8 C47 C52 -79.6(3) . . . . ?
C47 O8 C46 O7 -78.6(3) . . . . ?
C47 C48 C49 C50 -2.2(3) . . . . ?
C47 C48 C49 C54 174.2(2) . . . . ?
C48 C47 C52 O9 179.5(2) . . . . ?
C48 C47 C52 C51 0.9(4) . . . . ?
C48 C49 C50 C36 -178.1(2) . . . . ?
C48 C49 C50 C51 2.1(3) . . . . ?
C48 C49 C54 C14 -86.7(2) . . . . ?
C49 C50 C51 C52 -0.5(4) . . . . ?
C50 C49 C54 C14 89.6(3) . . . . ?
C50 C51 C52 O9 -179.5(2) . . . . ?
C50 C51 C52 C47 -1.0(4) . . . . ?
C52 C47 C48 C49 0.7(4) . . . . ?
C53 O9 C52 C47 177.2(2) . . . . ?
C53 O9 C52 C51 -4.3(4) . . . . ?
C54 C14 C15 C16 -172.0(2) . . . . ?
C54 C49 C50 C36 5.6(3) . . . . ?
C54 C49 C50 C51 -174.2(2) . . . . ?
C71 O70 C73 C74 171.5(2) . . . . ?
C73 O70 C71 C72 179.9(2) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 1.000 1.000 277.4 58.4 ?
2 0.468 0.795 0.685 12.1 0.0 ?
3 0.532 0.205 0.315 12.1 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.796
_oxdiff_exptl_absorpt_empirical_full_min 0.685
