# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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. 
# 
#######################################################################

data_x0376fin_3S
_database_code_depnum_ccdc_archive 'CCDC 1854866'
_audit_update_record             
;
2018-07-10 deposited with the CCDC.
2018-11-14 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         ?
_chemical_formula_sum            'C69 H93 N3 O P4'
_chemical_formula_weight         1104.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
P P 0.1023 0.0942 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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'

_cell_length_a                   11.6268(4)
_cell_length_b                   12.1381(5)
_cell_length_c                   13.2236(4)
_cell_angle_alpha                88.667(3)
_cell_angle_beta                 70.775(3)
_cell_angle_gamma                64.619(4)
_cell_volume                     1576.78(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    9054
_cell_measurement_theta_min      2.6500
_cell_measurement_theta_max      32.2423

_exptl_crystal_description       plates
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_F_000             596
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    0.164
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.99026
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET)
(compiled Nov 29 2007,17:23:28)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'ccd Xcalibur S'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 16.3560
_diffrn_reflns_number            31375
_diffrn_reflns_av_unetI/netI     0.0931
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_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         2.661
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_full        24.713
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             10714
_reflns_number_gt                6768
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.996
_reflns_Friedel_fraction_max     0.994
_reflns_Friedel_fraction_full    0.994

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

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET)
(compiled Nov 29 2007,17:23:28)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET)
(compiled Nov 29 2007,17:23:28)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET)
(compiled Nov 29 2007,17:23:28)
;
_computing_structure_solution    'SIR92 (Giacovazzo 1993)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'ORTEP3 for Windows (L. J. Farrugia, 1997)'
_computing_publication_material  'WINGX  (L.J. Farrugia,1999)'
_refine_special_details          
;
Disordered substituent C46 to C48.
The anisotropic displacement parameters of other substituents indicate a
relatively strong libration or may be a result of a marginal disorder
ar well.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0701P)²] 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_abs_structure_details 
;
 Flack x determined using 2534 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(6)
_chemical_absolute_configuration rmad
_refine_ls_number_reflns         10714
_refine_ls_number_parameters     719
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0519
_refine_ls_wR_factor_ref         0.1282
_refine_ls_wR_factor_gt          0.1195
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_restrained_S_all      0.913
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.36025(17) 0.65823(16) 0.99607(15) 0.0274(5) Uani 1 1 d . . . . .
P2 P 0.90661(18) 0.55464(17) 0.81940(16) 0.0304(6) Uani 1 1 d . . . . .
P3 P 0.68917(17) 0.71203(16) 1.15840(15) 0.0278(5) Uani 1 1 d . . . . .
P4 P 0.13728(18) 0.81684(17) 1.33426(15) 0.0288(5) Uani 1 1 d . . . . .
N1 N 0.2156(6) 0.6228(5) 1.1895(5) 0.0293(16) Uani 1 1 d . . . . .
N2 N 0.8086(6) 0.7571(5) 0.9639(5) 0.0254(15) Uani 1 1 d . . . . .
C1 C 0.2549(7) 0.5842(7) 1.0749(6) 0.0255(19) Uani 1 1 d . . . . .
H1A H 0.172775 0.609042 1.055466 0.031 Uiso 1 1 calc R U . . .
H1B H 0.307619 0.493485 1.058272 0.031 Uiso 1 1 calc R U . . .
C2 C 0.5364(8) 0.5414(7) 0.9719(7) 0.030(2) Uani 1 1 d . . . . .
H2A H 0.547658 0.521465 1.042104 0.036 Uiso 1 1 calc R U . . .
H2B H 0.553924 0.465076 0.931008 0.036 Uiso 1 1 calc R U . . .
C3 C 0.6386(8) 0.5866(7) 0.9090(8) 0.035(2) Uani 1 1 d . . . . .
H3A H 0.613095 0.668628 0.944833 0.043 Uiso 1 1 calc R U . . .
H3B H 0.635478 0.595837 0.835277 0.043 Uiso 1 1 calc R U . . .
C4 C 0.7869(7) 0.4970(7) 0.9008(6) 0.0269(19) Uani 1 1 d . . . . .
H4A H 0.812328 0.414120 0.866851 0.032 Uiso 1 1 calc R U . . .
H4B H 0.791820 0.490136 0.974150 0.032 Uiso 1 1 calc R U . . .
C5 C 0.9253(8) 0.6398(7) 0.9247(6) 0.033(2) Uani 1 1 d . . . . .
H5A H 0.934277 0.591272 0.985289 0.039 Uiso 1 1 calc R U . . .
H5B H 1.008545 0.651516 0.893106 0.039 Uiso 1 1 calc R U . . .
C6 C 0.7762(8) 0.7994(7) 1.0785(6) 0.028(2) Uani 1 1 d . . . . .
H6A H 0.715918 0.889027 1.096701 0.034 Uiso 1 1 calc R U . . .
H6B H 0.860380 0.781714 1.092839 0.034 Uiso 1 1 calc R U . . .
C7 C 0.5117(7) 0.8253(7) 1.1840(7) 0.028(2) Uani 1 1 d . . . . .
H7A H 0.492241 0.901293 1.226472 0.034 Uiso 1 1 calc R U . . .
H7B H 0.500450 0.846680 1.114002 0.034 Uiso 1 1 calc R U . . .
C8 C 0.4085(7) 0.7783(7) 1.2451(6) 0.0268(19) Uani 1 1 d . . . . .
H8A H 0.432154 0.698742 1.205741 0.032 Uiso 1 1 calc R U . . .
H8B H 0.413971 0.763693 1.317658 0.032 Uiso 1 1 calc R U . . .
C9 C 0.2662(7) 0.8670(8) 1.2571(8) 0.038(2) Uani 1 1 d . . . . .
H9A H 0.260768 0.879395 1.184216 0.046 Uiso 1 1 calc R U . . .
H9B H 0.244466 0.947353 1.293747 0.046 Uiso 1 1 calc R U . . .
C10 C 0.1093(7) 0.7524(6) 1.2254(6) 0.028(2) Uani 1 1 d . . . . .
H10A H 0.017732 0.755334 1.251938 0.034 Uiso 1 1 calc R U . . .
H10B H 0.115469 0.800728 1.164197 0.034 Uiso 1 1 calc R U . . .
C11 C 0.1794(7) 0.5389(6) 1.2606(6) 0.0348(17) Uani 1 1 d D . . . .
C12 C 0.3072(7) 0.4219(6) 1.2506(5) 0.0376(16) Uani 1 1 d . . . . .
C13 C 0.4178(10) 0.4363(8) 1.2528(10) 0.077(4) Uani 1 1 d . . . . .
H13 H 0.411531 0.516386 1.261834 0.092 Uiso 1 1 calc R U . . .
C14 C 0.5394(10) 0.3319(8) 1.2415(12) 0.128(6) Uani 1 1 d . . . . .
H14 H 0.616852 0.342059 1.239219 0.154 Uiso 1 1 calc R U . . .
C15 C 0.5491(11) 0.2191(9) 1.2340(13) 0.156(7) Uani 1 1 d . . . . .
H15 H 0.632423 0.149299 1.226438 0.188 Uiso 1 1 calc R U . . .
C16 C 0.4337(10) 0.2042(9) 1.2373(12) 0.126(6) Uani 1 1 d . . . . .
H16 H 0.437649 0.124475 1.234699 0.151 Uiso 1 1 calc R U . . .
C17 C 0.3148(8) 0.3075(8) 1.2444(8) 0.048(2) Uani 1 1 d . . . . .
C18 C 0.1982(8) 0.2856(7) 1.2402(7) 0.060(2) Uani 1 1 d . . . . .
H18A H 0.196874 0.214612 1.278069 0.072 Uiso 1 1 calc R U . . .
H18B H 0.210706 0.265812 1.164000 0.072 Uiso 1 1 calc R U . . .
C19 C 0.0647(7) 0.3985(7) 1.2930(7) 0.057(2) Uani 1 1 d . . . . .
H19A H 0.046928 0.413414 1.371198 0.068 Uiso 1 1 calc R U . . .
H19B H -0.010560 0.385855 1.284819 0.068 Uiso 1 1 calc R U . . .
C20 C 0.0720(7) 0.5085(7) 1.2397(7) 0.042(2) Uani 1 1 d . . . . .
H20A H -0.018246 0.580854 1.268433 0.051 Uiso 1 1 calc R U . . .
H20B H 0.095819 0.490709 1.160848 0.051 Uiso 1 1 calc R U . . .
C21 C 0.3540(8) 0.6556(7) 0.8588(7) 0.031(2) Uani 1 1 d . . . . .
C22 C 0.3456(8) 0.5605(7) 0.8051(7) 0.032(2) Uani 1 1 d . . . . .
C23 C 0.3395(8) 0.5696(8) 0.7013(8) 0.043(2) Uani 1 1 d . . . . .
H23 H 0.330706 0.507007 0.667250 0.052 Uiso 1 1 calc R U . . .
C24 C 0.3456(9) 0.6629(9) 0.6481(7) 0.043(2) Uani 1 1 d . . . . .
C25 C 0.3471(9) 0.7604(9) 0.7002(9) 0.058(3) Uani 1 1 d . . . . .
H25 H 0.346652 0.829274 0.664445 0.069 Uiso 1 1 calc R U . . .
C26 C 0.3492(8) 0.7561(7) 0.8078(7) 0.036(2) Uani 1 1 d . . . . .
C27 C 0.3516(9) 0.4470(8) 0.8467(7) 0.043(2) Uani 1 1 d . . . . .
H27A H 0.432391 0.407044 0.867084 0.064 Uiso 1 1 calc R U . . .
H27B H 0.356793 0.391786 0.790670 0.064 Uiso 1 1 calc R U . . .
H27C H 0.269797 0.465668 0.910198 0.064 Uiso 1 1 calc R U . . .
C28 C 0.3432(10) 0.6712(10) 0.5337(8) 0.067(3) Uani 1 1 d . . . . .
H28A H 0.424428 0.602509 0.484010 0.100 Uiso 1 1 calc R U . . .
H28B H 0.342015 0.749248 0.511787 0.100 Uiso 1 1 calc R U . . .
H28C H 0.261589 0.667160 0.531611 0.100 Uiso 1 1 calc R U . . .
C29 C 0.3609(10) 0.8618(8) 0.8540(8) 0.055(3) Uani 1 1 d . . . . .
H29A H 0.361658 0.920146 0.801578 0.083 Uiso 1 1 calc R U . . .
H29B H 0.445545 0.830252 0.869293 0.083 Uiso 1 1 calc R U . . .
H29C H 0.283187 0.903557 0.921012 0.083 Uiso 1 1 calc R U . . .
C30 C 1.0694(8) 0.4160(7) 0.7720(7) 0.034(2) Uani 1 1 d . . . . .
C31 C 1.1253(9) 0.3229(8) 0.8302(9) 0.045(2) Uani 1 1 d . . . . .
C32 C 1.2453(10) 0.2173(8) 0.7777(11) 0.062(3) Uani 1 1 d . . . . .
H32 H 1.279935 0.155671 0.819797 0.074 Uiso 1 1 calc R U . . .
C33 C 1.3129(11) 0.1984(10) 0.6736(12) 0.068(3) Uani 1 1 d . . . . .
C34 C 1.2649(9) 0.2884(10) 0.6139(9) 0.060(3) Uani 1 1 d . . . . .
H34 H 1.313575 0.274088 0.538283 0.072 Uiso 1 1 calc R U . . .
C35 C 1.1480(9) 0.4011(9) 0.6570(8) 0.053(3) Uani 1 1 d . . . . .
C36 C 1.0639(9) 0.3358(8) 0.9528(8) 0.054(3) Uani 1 1 d . . . . .
H36A H 0.964758 0.369579 0.975239 0.081 Uiso 1 1 calc R U . . .
H36B H 1.086993 0.391397 0.985586 0.081 Uiso 1 1 calc R U . . .
H36C H 1.100433 0.254843 0.976495 0.081 Uiso 1 1 calc R U . . .
C37 C 1.4417(11) 0.0824(9) 0.6144(12) 0.098(5) Uani 1 1 d . . . . .
H37A H 1.496457 0.052096 0.660725 0.147 Uiso 1 1 calc R U . . .
H37B H 1.494413 0.101122 0.547632 0.147 Uiso 1 1 calc R U . . .
H37C H 1.417430 0.019225 0.596748 0.147 Uiso 1 1 calc R U . . .
C38 C 1.1022(9) 0.4972(11) 0.5872(8) 0.066(3) Uani 1 1 d . . . . .
H38A H 1.175771 0.477853 0.517215 0.099 Uiso 1 1 calc R U . . .
H38B H 1.078492 0.577909 0.622659 0.099 Uiso 1 1 calc R U . . .
H38C H 1.022284 0.498754 0.576054 0.099 Uiso 1 1 calc R U . . .
C39 C 0.7993(8) 0.8513(7) 0.8880(6) 0.0408(19) Uani 1 1 d D . . . .
C40 C 0.8319(8) 0.9522(7) 0.9159(6) 0.0520(19) Uani 1 1 d . . . . .
C41 C 0.9575(9) 0.9226(10) 0.9209(8) 0.067(3) Uani 1 1 d . . . . .
H41 H 1.024854 0.839286 0.902201 0.081 Uiso 1 1 calc R U . . .
C42 C 0.9880(12) 1.0102(15) 0.9521(9) 0.104(4) Uani 1 1 d . . . . .
H42 H 1.074399 0.987854 0.957622 0.124 Uiso 1 1 calc R U . . .
C43 C 0.890(2) 1.1326(16) 0.9756(14) 0.150(7) Uani 1 1 d . . . . .
H43 H 0.908440 1.195296 0.998362 0.180 Uiso 1 1 calc R U . . .
C44 C 0.7701(16) 1.1604(10) 0.9655(14) 0.148(7) Uani 1 1 d . . . . .
H44 H 0.706313 1.244664 0.976921 0.178 Uiso 1 1 calc R U . . .
C45 C 0.7345(13) 1.0753(9) 0.9399(10) 0.078(4) Uani 1 1 d . . . . .
C46 C 0.5970(11) 1.1150(9) 0.9276(10) 0.094(4) Uani 0.609(19) 1 d . . P A 1
H46A H 0.600433 1.143750 0.856425 0.113 Uiso 0.609(19) 1 calc R U P A 1
H46B H 0.526002 1.184142 0.984631 0.113 Uiso 0.609(19) 1 calc R U P A 1
C47 C 0.5600(13) 1.0026(11) 0.9369(10) 0.037(4) Uani 0.609(19) 1 d . . P A 1
H47A H 0.541142 0.983144 1.011976 0.044 Uiso 0.609(19) 1 calc R U P A 1
H47B H 0.477042 1.025145 0.919119 0.044 Uiso 0.609(19) 1 calc R U P A 1
C48 C 0.6636(12) 0.9034(10) 0.8688(12) 0.088(4) Uani 0.609(19) 1 d . . P A 1
H48A H 0.679815 0.924880 0.794347 0.106 Uiso 0.609(19) 1 calc R U P A 1
H48B H 0.634690 0.837198 0.872335 0.106 Uiso 0.609(19) 1 calc R U P A 1
C46F C 0.5970(11) 1.1150(9) 0.9276(10) 0.094(4) Uani 0.391(19) 1 d . . P A 2
H46C H 0.569858 1.195942 0.900881 0.113 Uiso 0.391(19) 1 calc R U P A 2
H46D H 0.527859 1.125131 0.999313 0.113 Uiso 0.391(19) 1 calc R U P A 2
C47F C 0.5994(19) 1.0153(15) 0.8436(18) 0.058(8) Uani 0.391(19) 1 d . . P A 2
H47C H 0.505477 1.032516 0.851180 0.070 Uiso 0.391(19) 1 calc R U P A 2
H47D H 0.648159 1.020599 0.767937 0.070 Uiso 0.391(19) 1 calc R U P A 2
C48F C 0.6636(12) 0.9034(10) 0.8688(12) 0.088(4) Uani 0.391(19) 1 d . . P A 2
H48C H 0.676454 0.844528 0.810747 0.106 Uiso 0.391(19) 1 calc R U P A 2
H48D H 0.597219 0.896398 0.935172 0.106 Uiso 0.391(19) 1 calc R U P A 2
C49 C 0.7030(8) 0.7134(7) 1.2939(7) 0.030(2) Uani 1 1 d . . . . .
C50 C 0.7005(8) 0.8090(9) 1.3536(7) 0.041(2) Uani 1 1 d . . . . .
C51 C 0.7084(8) 0.7951(10) 1.4560(6) 0.062(3) Uani 1 1 d . . . . .
H51 H 0.709167 0.859189 1.495286 0.074 Uiso 1 1 calc R U . . .
C52 C 0.7151(9) 0.6893(13) 1.5025(9) 0.071(4) Uani 1 1 d . . . . .
C53 C 0.7115(9) 0.6010(12) 1.4475(9) 0.065(3) Uani 1 1 d . . . . .
H53 H 0.713451 0.529961 1.480236 0.078 Uiso 1 1 calc R U . . .
C54 C 0.7049(9) 0.6083(10) 1.3438(9) 0.062(3) Uani 1 1 d . . . . .
C55 C 0.6932(10) 0.9292(7) 1.3094(8) 0.056(3) Uani 1 1 d . . . . .
H55A H 0.674739 0.989172 1.368122 0.084 Uiso 1 1 calc R U . . .
H55B H 0.620064 0.962553 1.279639 0.084 Uiso 1 1 calc R U . . .
H55C H 0.780095 0.912555 1.252439 0.084 Uiso 1 1 calc R U . . .
C56 C 0.7139(12) 0.6793(16) 1.6177(9) 0.136(7) Uani 1 1 d . . . . .
H56A H 0.620016 0.708049 1.667847 0.203 Uiso 1 1 calc R U . . .
H56B H 0.753052 0.730108 1.635439 0.203 Uiso 1 1 calc R U . . .
H56C H 0.767886 0.593245 1.624065 0.203 Uiso 1 1 calc R U . . .
C57 C 0.7076(12) 0.5030(9) 1.2844(11) 0.089(5) Uani 1 1 d . . . . .
H57A H 0.615226 0.522422 1.288168 0.133 Uiso 1 1 calc R U . . .
H57B H 0.742831 0.428508 1.317563 0.133 Uiso 1 1 calc R U . . .
H57C H 0.766632 0.489278 1.208564 0.133 Uiso 1 1 calc R U . . .
C58 C -0.0237(8) 0.9615(7) 1.3954(7) 0.034(2) Uani 1 1 d . . . . .
C59 C -0.0732(9) 1.0608(8) 1.3378(8) 0.045(2) Uani 1 1 d . . . . .
C60 C -0.1907(9) 1.1645(8) 1.3925(10) 0.056(3) Uani 1 1 d . . . . .
H60 H -0.222733 1.231533 1.354154 0.067 Uiso 1 1 calc R U . . .
C61 C -0.2635(9) 1.1752(8) 1.5002(10) 0.057(3) Uani 1 1 d . . . . .
C62 C -0.2124(10) 1.0763(10) 1.5541(9) 0.069(3) Uani 1 1 d . . . . .
H62 H -0.260079 1.080008 1.628694 0.083 Uiso 1 1 calc R U . . .
C63 C -0.0916(9) 0.9715(8) 1.4998(8) 0.042(2) Uani 1 1 d . . . . .
C64 C -0.0037(11) 1.0639(9) 1.2209(8) 0.074(3) Uani 1 1 d . . . . .
H64A H -0.069502 1.125039 1.192945 0.112 Uiso 1 1 calc R U . . .
H64B H 0.033949 0.982554 1.179799 0.112 Uiso 1 1 calc R U . . .
H64C H 0.070095 1.086165 1.213604 0.112 Uiso 1 1 calc R U . . .
C65 C -0.3878(11) 1.2949(10) 1.5627(11) 0.108(5) Uani 1 1 d . . . . .
H65A H -0.364418 1.333612 1.611991 0.162 Uiso 1 1 calc R U . . .
H65B H -0.462851 1.276445 1.604400 0.162 Uiso 1 1 calc R U . . .
H65C H -0.415619 1.351142 1.511591 0.162 Uiso 1 1 calc R U . . .
C66 C -0.0488(12) 0.8700(11) 1.5664(8) 0.096(5) Uani 1 1 d . . . . .
H66A H -0.045230 0.795722 1.535172 0.144 Uiso 1 1 calc R U . . .
H66B H -0.114568 0.895464 1.640605 0.144 Uiso 1 1 calc R U . . .
H66C H 0.041438 0.852725 1.566963 0.144 Uiso 1 1 calc R U . . .
H39 H 0.877(6) 0.798(5) 0.818(4) 0.03(2) Uiso 1 1 d D . . . .
H11 H 0.139(6) 0.584(5) 1.336(3) 0.029(19) Uiso 1 1 d D . . . .
O1 O -0.2859(18) 0.297(2) 0.7627(16) 0.106(9) Uiso 0.308(12) 1 d D . P B 1
N3 N -0.0657(15) 0.2177(14) 0.6562(12) 0.036(5) Uiso 0.308(12) 1 d D . P B 1
C67 C 0.071(2) 0.110(2) 0.619(3) 0.111(5) Uiso 0.308(12) 1 d D . P B 1
H67A H 0.134844 0.129628 0.561981 0.166 Uiso 0.308(12) 1 calc R U P B 1
H67B H 0.103108 0.089675 0.680401 0.166 Uiso 0.308(12) 1 calc R U P B 1
H67C H 0.064849 0.039075 0.591733 0.166 Uiso 0.308(12) 1 calc R U P B 1
C68 C -0.080(3) 0.313(3) 0.588(3) 0.20(3) Uiso 0.308(12) 1 d D . P B 1
H68A H 0.009917 0.297819 0.536177 0.294 Uiso 0.308(12) 1 calc R U P B 1
H68B H -0.137783 0.313123 0.547812 0.294 Uiso 0.308(12) 1 calc R U P B 1
H68C H -0.121759 0.393207 0.631996 0.294 Uiso 0.308(12) 1 calc R U P B 1
C69 C -0.175(2) 0.214(2) 0.7376(17) 0.082(10) Uiso 0.308(12) 1 d D . P B 1
H69 H -0.161034 0.142932 0.773680 0.099 Uiso 0.308(12) 1 calc R U P B 1
O1F O 0.2565(19) 0.0549(19) 0.4367(18) 0.280(12) Uiso 0.692(12) 1 d D . P B 2
N3F N 0.0640(14) 0.1471(12) 0.5766(12) 0.111(5) Uiso 0.692(12) 1 d D . P B 2
C67F C -0.022(3) 0.153(3) 0.6884(16) 0.286(19) Uiso 0.692(12) 1 d D . P B 2
H67D H -0.107137 0.228976 0.708020 0.429 Uiso 0.692(12) 1 calc R U P B 2
H67E H -0.041201 0.081817 0.694609 0.429 Uiso 0.692(12) 1 calc R U P B 2
H67F H 0.026302 0.152514 0.737224 0.429 Uiso 0.692(12) 1 calc R U P B 2
C68F C 0.000(3) 0.255(2) 0.526(2) 0.31(2) Uiso 0.692(12) 1 d D . P B 2
H68D H -0.089968 0.310476 0.577923 0.467 Uiso 0.692(12) 1 calc R U P B 2
H68E H 0.056915 0.297674 0.505417 0.467 Uiso 0.692(12) 1 calc R U P B 2
H68F H -0.010490 0.227545 0.461924 0.467 Uiso 0.692(12) 1 calc R U P B 2
C69F C 0.191(2) 0.0528(17) 0.524(2) 0.190(11) Uiso 0.692(12) 1 d D . P B 2
H69F H 0.225487 -0.016136 0.559397 0.228 Uiso 0.692(12) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C21 1.842(9) . ?
P1 C2 1.846(8) . ?
P1 C1 1.858(8) . ?
P2 C30 1.829(8) . ?
P2 C4 1.843(8) . ?
P2 C5 1.874(8) . ?
P3 C7 1.842(7) . ?
P3 C6 1.851(8) . ?
P3 C49 1.852(9) . ?
P4 C10 1.836(7) . ?
P4 C9 1.846(9) . ?
P4 C58 1.869(8) . ?
N1 C1 1.455(9) . ?
N1 C11 1.470(9) . ?
N1 C10 1.486(8) . ?
N2 C5 1.433(9) . ?
N2 C6 1.483(9) . ?
N2 C39 1.496(9) . ?
C2 C3 1.514(10) . ?
C3 C4 1.562(10) . ?
C7 C8 1.531(10) . ?
C8 C9 1.493(10) . ?
C11 C12 1.521(9) . ?
C11 C20 1.548(10) . ?
C12 C17 1.356(10) . ?
C12 C13 1.380(10) . ?
C13 C14 1.401(12) . ?
C14 C15 1.329(13) . ?
C15 C16 1.415(13) . ?
C16 C17 1.388(11) . ?
C17 C18 1.506(11) . ?
C18 C19 1.510(10) . ?
C19 C20 1.517(10) . ?
C21 C26 1.370(11) . ?
C21 C22 1.423(11) . ?
C22 C23 1.398(11) . ?
C22 C27 1.453(11) . ?
C23 C24 1.334(12) . ?
C24 C25 1.391(13) . ?
C24 C28 1.523(12) . ?
C25 C26 1.431(12) . ?
C26 C29 1.509(12) . ?
C30 C31 1.397(12) . ?
C30 C35 1.461(13) . ?
C31 C32 1.393(12) . ?
C31 C36 1.522(13) . ?
C32 C33 1.309(16) . ?
C33 C34 1.362(14) . ?
C33 C37 1.520(14) . ?
C34 C35 1.405(13) . ?
C35 C38 1.496(14) . ?
C39 C40 1.513(11) . ?
C39 C48F 1.535(12) . ?
C39 C48 1.535(12) . ?
C40 C41 1.370(11) . ?
C40 C45 1.396(12) . ?
C41 C42 1.366(15) . ?
C42 C43 1.392(17) . ?
C43 C44 1.344(18) . ?
C44 C45 1.352(14) . ?
C45 C46F 1.523(14) . ?
C45 C46 1.523(14) . ?
C46 C47 1.589(15) . ?
C47 C48 1.343(16) . ?
C46F C47F 1.65(2) . ?
C47F C48F 1.34(2) . ?
C49 C50 1.403(12) . ?
C49 C54 1.418(11) . ?
C50 C51 1.388(11) . ?
C50 C55 1.538(13) . ?
C51 C52 1.394(15) . ?
C52 C53 1.332(16) . ?
C52 C56 1.522(14) . ?
C53 C54 1.397(14) . ?
C54 C57 1.499(15) . ?
C58 C63 1.323(12) . ?
C58 C59 1.420(11) . ?
C59 C60 1.375(12) . ?
C59 C64 1.498(13) . ?
C60 C61 1.373(15) . ?
C61 C62 1.388(15) . ?
C61 C65 1.534(13) . ?
C62 C63 1.398(12) . ?
C63 C66 1.501(13) . ?
O1 C69 1.19(2) . ?
N3 C69 1.389(19) . ?
N3 C68 1.442(13) . ?
N3 C67 1.487(13) . ?
O1F C69F 1.16(2) . ?
N3F C69F 1.372(18) . ?
N3F C67F 1.468(13) . ?
N3F C68F 1.469(13) . ?

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
C21 P1 C2 101.2(4) . . ?
C21 P1 C1 106.7(4) . . ?
C2 P1 C1 103.6(3) . . ?
C30 P2 C4 103.2(4) . . ?
C30 P2 C5 102.9(3) . . ?
C4 P2 C5 102.8(4) . . ?
C7 P3 C6 98.8(4) . . ?
C7 P3 C49 103.0(4) . . ?
C6 P3 C49 107.8(4) . . ?
C10 P4 C9 101.7(4) . . ?
C10 P4 C58 103.8(3) . . ?
C9 P4 C58 105.5(4) . . ?
C1 N1 C11 114.2(6) . . ?
C1 N1 C10 112.8(6) . . ?
C11 N1 C10 111.6(6) . . ?
C5 N2 C6 112.5(6) . . ?
C5 N2 C39 115.9(6) . . ?
C6 N2 C39 116.9(6) . . ?
N1 C1 P1 108.6(5) . . ?
C3 C2 P1 111.4(5) . . ?
C2 C3 C4 112.4(6) . . ?
C3 C4 P2 110.1(5) . . ?
N2 C5 P2 109.6(5) . . ?
N2 C6 P3 105.3(5) . . ?
C8 C7 P3 113.0(5) . . ?
C9 C8 C7 112.2(6) . . ?
C8 C9 P4 113.9(6) . . ?
N1 C10 P4 108.0(5) . . ?
N1 C11 C12 109.7(6) . . ?
N1 C11 C20 113.4(6) . . ?
C12 C11 C20 110.9(6) . . ?
C17 C12 C13 119.7(7) . . ?
C17 C12 C11 123.5(6) . . ?
C13 C12 C11 116.8(6) . . ?
C12 C13 C14 119.4(8) . . ?
C15 C14 C13 121.6(9) . . ?
C14 C15 C16 119.1(9) . . ?
C17 C16 C15 119.2(9) . . ?
C12 C17 C16 120.9(7) . . ?
C12 C17 C18 122.2(7) . . ?
C16 C17 C18 116.9(8) . . ?
C17 C18 C19 110.4(7) . . ?
C18 C19 C20 109.0(7) . . ?
C19 C20 C11 111.3(6) . . ?
C26 C21 C22 118.0(8) . . ?
C26 C21 P1 117.1(7) . . ?
C22 C21 P1 124.8(6) . . ?
C23 C22 C21 119.5(8) . . ?
C23 C22 C27 115.2(8) . . ?
C21 C22 C27 125.1(7) . . ?
C24 C23 C22 122.4(8) . . ?
C23 C24 C25 119.5(9) . . ?
C23 C24 C28 122.6(9) . . ?
C25 C24 C28 117.9(9) . . ?
C24 C25 C26 119.6(9) . . ?
C21 C26 C25 120.7(8) . . ?
C21 C26 C29 123.6(8) . . ?
C25 C26 C29 115.5(8) . . ?
C31 C30 C35 116.8(8) . . ?
C31 C30 P2 128.7(7) . . ?
C35 C30 P2 114.5(7) . . ?
C32 C31 C30 120.5(10) . . ?
C32 C31 C36 117.5(9) . . ?
C30 C31 C36 121.8(8) . . ?
C33 C32 C31 123.6(11) . . ?
C32 C33 C34 118.0(10) . . ?
C32 C33 C37 124.4(13) . . ?
C34 C33 C37 117.6(13) . . ?
C33 C34 C35 124.2(11) . . ?
C34 C35 C30 116.4(10) . . ?
C34 C35 C38 121.6(10) . . ?
C30 C35 C38 121.9(8) . . ?
N2 C39 C40 115.2(6) . . ?
N2 C39 C48F 111.8(7) . . ?
C40 C39 C48F 112.0(7) . . ?
N2 C39 C48 111.8(7) . . ?
C40 C39 C48 112.0(7) . . ?
C41 C40 C45 119.2(9) . . ?
C41 C40 C39 119.8(8) . . ?
C45 C40 C39 121.0(7) . . ?
C42 C41 C40 121.5(10) . . ?
C41 C42 C43 118.9(11) . . ?
C44 C43 C42 118.6(11) . . ?
C43 C44 C45 123.8(13) . . ?
C44 C45 C40 117.8(11) . . ?
C44 C45 C46F 120.3(10) . . ?
C40 C45 C46F 121.6(9) . . ?
C44 C45 C46 120.3(10) . . ?
C40 C45 C46 121.6(9) . . ?
C45 C46 C47 109.8(8) . . ?
C48 C47 C46 110.1(11) . . ?
C47 C48 C39 116.8(11) . . ?
C45 C46F C47F 112.5(10) . . ?
C48F C47F C46F 107.1(16) . . ?
C47F C48F C39 126.6(13) . . ?
C50 C49 C54 118.2(9) . . ?
C50 C49 P3 127.5(6) . . ?
C54 C49 P3 114.1(8) . . ?
C51 C50 C49 119.6(9) . . ?
C51 C50 C55 117.6(9) . . ?
C49 C50 C55 122.8(8) . . ?
C50 C51 C52 121.4(11) . . ?
C53 C52 C51 118.8(10) . . ?
C53 C52 C56 120.3(12) . . ?
C51 C52 C56 120.7(13) . . ?
C52 C53 C54 122.8(10) . . ?
C53 C54 C49 119.0(11) . . ?
C53 C54 C57 120.1(9) . . ?
C49 C54 C57 120.8(10) . . ?
C63 C58 C59 119.2(8) . . ?
C63 C58 P4 116.7(7) . . ?
C59 C58 P4 124.1(7) . . ?
C60 C59 C58 118.8(9) . . ?
C60 C59 C64 116.5(9) . . ?
C58 C59 C64 124.7(8) . . ?
C61 C60 C59 122.7(10) . . ?
C60 C61 C62 117.1(8) . . ?
C60 C61 C65 122.2(11) . . ?
C62 C61 C65 120.4(11) . . ?
C61 C62 C63 120.7(10) . . ?
C58 C63 C62 121.6(9) . . ?
C58 C63 C66 122.8(8) . . ?
C62 C63 C66 115.5(9) . . ?
C69 N3 C68 123.3(12) . . ?
C69 N3 C67 121.0(12) . . ?
C68 N3 C67 114.5(13) . . ?
O1 C69 N3 121.2(16) . . ?
C69F N3F C67F 124.6(12) . . ?
C69F N3F C68F 122.8(12) . . ?
C67F N3F C68F 112.6(12) . . ?
O1F C69F N3F 121.8(16) . . ?

_refine_diff_density_max         0.622
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.051

####################################################################### 
# 
# 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_s14
_database_code_depnum_ccdc_archive 'CCDC 1856396'
_audit_update_record             
;
2018-10-24 deposited with the CCDC.
2018-11-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
1,9-bis((R,S)-α-methylbenzyl)-3,7,11,15-tetramesityl-1,9-diaza-3,7,11,15-(RSSR)-tetraphosphacyclohexadecane
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C62 H82 N2 P4, 4(C6 H6)'
_chemical_formula_sum            'C86 H106 N2 P4'
_chemical_formula_weight         1291.61

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'
N N 0.0311 0.0180 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 21/a'
_symmetry_Int_Tables_number      14

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2-x,1/2+y,-z
3 -x,-y,-z
4 1/2+x,1/2-y,z


_cell_length_a                   9.601(7)
_cell_length_b                   33.967(15)
_cell_length_c                   13.081(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.79(4)
_cell_angle_gamma                90.00
_cell_volume                     4014(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2383
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      18.94

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1392
_exptl_absorpt_coefficient_mu    1.179
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       ω/2τ
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8490
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.60
_diffrn_reflns_theta_max         74.43
_reflns_number_total             7990
_reflns_number_gt                5034
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'MolEN, 1994'
_computing_cell_refinement       'MolEN, 1994'
_computing_data_reduction        'MolEN, 1994'
_computing_structure_solution    'SIR, 19921'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXS-97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXS-97 (Sheldrick, 2008)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1183P)²+0.5708P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7990
_refine_ls_number_parameters     391
_refine_ls_number_restraints     252
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.0642
_refine_ls_wR_factor_ref         0.2146
_refine_ls_wR_factor_gt          0.1796
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C60 C 0.1911(6) 0.1840(2) 0.7743(6) 0.186(3) Uani 1 1 d GU . .
H60 H 0.2937 0.1824 0.7963 0.224 Uiso 1 1 calc R . .
C61 C 0.1245(9) 0.21135(17) 0.8219(4) 0.187(3) Uani 1 1 d GU . .
H61 H 0.1826 0.2281 0.8758 0.224 Uiso 1 1 calc R . .
C62 C -0.0289(10) 0.21369(16) 0.7891(6) 0.202(3) Uani 1 1 d GU . .
H62 H -0.0735 0.2320 0.8210 0.243 Uiso 1 1 calc R . .
C63 C -0.1158(6) 0.1887(2) 0.7086(6) 0.195(3) Uani 1 1 d GU . .
H63 H -0.2184 0.1902 0.6867 0.234 Uiso 1 1 calc R . .
C64 C -0.0492(9) 0.16126(16) 0.6610(4) 0.183(3) Uani 1 1 d GU . .
H64 H -0.1073 0.1445 0.6072 0.219 Uiso 1 1 calc R . .
C65 C 0.1042(10) 0.15892(14) 0.6938(5) 0.174(3) Uani 1 1 d GU . .
H65 H 0.1488 0.1406 0.6620 0.209 Uiso 1 1 calc R . .
C50 C 0.5589(8) 0.1772(3) 0.4350(5) 0.220(4) Uani 1 1 d GU . .
H50 H 0.6157 0.1689 0.3939 0.264 Uiso 1 1 calc R . .
C51 C 0.5480(8) 0.2171(3) 0.4550(5) 0.216(4) Uani 1 1 d GU . .
H51 H 0.5975 0.2355 0.4272 0.259 Uiso 1 1 calc R . .
C52 C 0.4630(10) 0.22944(17) 0.5164(7) 0.237(4) Uani 1 1 d GU . .
H52 H 0.4557 0.2561 0.5298 0.284 Uiso 1 1 calc R . .
C53 C 0.3890(8) 0.2019(3) 0.5579(6) 0.268(5) Uani 1 1 d GU . .
H53 H 0.3322 0.2102 0.5990 0.321 Uiso 1 1 calc R . .
C54 C 0.4000(9) 0.1621(3) 0.5379(7) 0.271(5) Uani 1 1 d GU . .
H54 H 0.3505 0.1437 0.5657 0.325 Uiso 1 1 calc R . .
C55 C 0.4849(10) 0.14969(19) 0.4765(6) 0.248(5) Uani 1 1 d GU . .
H55 H 0.4922 0.1230 0.4631 0.298 Uiso 1 1 calc R . .
C2 C 1.0261(3) 0.12137(8) 0.0282(2) 0.0593(6) Uani 1 1 d U . .
H211 H 0.9670 0.1123 -0.0438 0.071 Uiso 1 1 calc R . .
H212 H 1.0432 0.1494 0.0243 0.071 Uiso 1 1 calc R . .
C4 C 0.8059(3) 0.07051(8) 0.0567(2) 0.0634(7) Uani 1 1 d U . .
H41 H 0.7117 0.0724 0.0687 0.076 Uiso 1 1 calc R . .
H42 H 0.7871 0.0718 -0.0208 0.076 Uiso 1 1 calc R . .
C5 C 0.8799(3) 0.03146(8) 0.1012(2) 0.0604(7) Uani 1 1 d U . .
H5A H 0.9780 0.0311 0.0954 0.072 Uiso 1 1 calc R . .
H5B H 0.8918 0.0298 0.1778 0.072 Uiso 1 1 calc R . .
C6 C 0.7960(3) -0.00454(8) 0.0441(2) 0.0635(7) Uani 1 1 d U . .
H6A H 0.7836 -0.0034 -0.0325 0.076 Uiso 1 1 calc R . .
H6B H 0.6985 -0.0050 0.0510 0.076 Uiso 1 1 calc R . .
C11 C 0.7801(3) -0.08985(8) 0.0236(2) 0.0564(6) Uani 1 1 d . . .
H11 H 0.7853 -0.1126 0.0696 0.068 Uiso 1 1 calc R . .
H12 H 0.6778 -0.0812 -0.0052 0.068 Uiso 1 1 calc R . .
C17 C 1.2815(3) 0.12132(8) 0.1545(2) 0.0600(7) Uani 1 1 d U . .
H17 H 1.2332 0.1291 0.2065 0.072 Uiso 1 1 calc R . .
C18 C 1.4016(3) 0.09268(8) 0.2136(2) 0.0591(6) Uani 1 1 d U . .
C19 C 1.3652(4) 0.05800(10) 0.2529(3) 0.0765(9) Uani 1 1 d U . .
H19 H 1.2661 0.0522 0.2401 0.092 Uiso 1 1 calc R . .
C20 C 1.4718(5) 0.03176(12) 0.3106(3) 0.0998(12) Uani 1 1 d U . .
H20 H 1.4449 0.0089 0.3384 0.120 Uiso 1 1 calc R . .
C21 C 1.6191(5) 0.03949(13) 0.3273(4) 0.1027(13) Uani 1 1 d U . .
H21 H 1.6919 0.0217 0.3655 0.123 Uiso 1 1 calc R . .
C22 C 1.6563(4) 0.07268(13) 0.2881(4) 0.0975(12) Uani 1 1 d U . .
H22 H 1.7555 0.0778 0.2992 0.117 Uiso 1 1 calc R . .
C23 C 1.5508(3) 0.09954(11) 0.2314(3) 0.0789(9) Uani 1 1 d U . .
H23 H 1.5796 0.1224 0.2050 0.095 Uiso 1 1 calc R . .
C24 C 1.3367(4) 0.15936(10) 0.1188(3) 0.0900(11) Uani 1 1 d U . .
H241 H 1.3903 0.1532 0.0708 0.135 Uiso 1 1 calc R . .
H242 H 1.4008 0.1729 0.1815 0.135 Uiso 1 1 calc R . .
H243 H 1.2538 0.1758 0.0817 0.135 Uiso 1 1 calc R . .
C25 C 0.8060(3) 0.15528(8) 0.1105(3) 0.0684(8) Uani 1 1 d U . .
C26 C 0.7028(4) 0.16883(9) 0.0128(3) 0.0796(9) Uani 1 1 d U . .
C27 C 0.6160(4) 0.20157(11) 0.0153(5) 0.1045(14) Uani 1 1 d U . .
H27 H 0.5462 0.2101 -0.0494 0.125 Uiso 1 1 calc R . .
C28 C 0.6294(5) 0.22165(11) 0.1088(6) 0.1162(17) Uani 1 1 d U . .
C29 C 0.7318(6) 0.20857(11) 0.2029(5) 0.1086(15) Uani 1 1 d U . .
H29 H 0.7423 0.2221 0.2669 0.130 Uiso 1 1 calc R . .
C30 C 0.8217(4) 0.17589(9) 0.2075(4) 0.0846(10) Uani 1 1 d U . .
C31 C 0.6812(5) 0.15070(12) -0.0948(3) 0.1039(13) Uani 1 1 d U . .
H311 H 0.7718 0.1522 -0.1104 0.156 Uiso 1 1 calc R . .
H312 H 0.6046 0.1645 -0.1498 0.156 Uiso 1 1 calc R . .
H313 H 0.6533 0.1236 -0.0937 0.156 Uiso 1 1 calc R . .
C32 C 0.5308(7) 0.25638(13) 0.1111(7) 0.186(3) Uani 1 1 d U . .
H321 H 0.4654 0.2618 0.0387 0.280 Uiso 1 1 calc R . .
H322 H 0.5911 0.2791 0.1394 0.280 Uiso 1 1 calc R . .
H323 H 0.4737 0.2502 0.1567 0.280 Uiso 1 1 calc R . .
C33 C 0.9322(6) 0.16467(13) 0.3157(4) 0.1128(14) Uani 1 1 d U . .
H331 H 0.8813 0.1591 0.3658 0.169 Uiso 1 1 calc R . .
H332 H 1.0000 0.1860 0.3431 0.169 Uiso 1 1 calc R . .
H333 H 0.9858 0.1417 0.3074 0.169 Uiso 1 1 calc R . .
C34 C 0.8731(3) -0.05299(8) 0.2376(2) 0.0576(6) Uani 1 1 d U . .
C35 C 0.7378(4) -0.05685(9) 0.2564(2) 0.0678(7) Uani 1 1 d U . .
C36 C 0.7403(5) -0.05934(10) 0.3629(3) 0.0825(9) Uani 1 1 d U . .
H36 H 0.6506 -0.0622 0.3747 0.099 Uiso 1 1 calc R . .
C37 C 0.8679(6) -0.05778(11) 0.4522(3) 0.0893(11) Uani 1 1 d U . .
C38 C 0.9968(5) -0.05415(12) 0.4318(3) 0.0969(12) Uani 1 1 d U . .
H38 H 1.0845 -0.0529 0.4907 0.116 Uiso 1 1 calc R . .
C39 C 1.0053(4) -0.05212(10) 0.3275(3) 0.0761(9) Uani 1 1 d U . .
C40 C 0.5909(4) -0.05801(14) 0.1686(3) 0.0959(12) Uani 1 1 d U . .
H401 H 0.5867 -0.0803 0.1224 0.144 Uiso 1 1 calc R . .
H402 H 0.5769 -0.0343 0.1264 0.144 Uiso 1 1 calc R . .
H403 H 0.5144 -0.0602 0.2001 0.144 Uiso 1 1 calc R . .
C41 C 0.8609(7) -0.05896(16) 0.5666(3) 0.142(2) Uani 1 1 d U . .
H411 H 0.9167 -0.0811 0.6050 0.213 Uiso 1 1 calc R . .
H412 H 0.7597 -0.0614 0.5629 0.213 Uiso 1 1 calc R . .
H413 H 0.9020 -0.0351 0.6041 0.213 Uiso 1 1 calc R . .
C42 C 1.1559(4) -0.04905(16) 0.3154(4) 0.1162(15) Uani 1 1 d U . .
H421 H 1.2131 -0.0720 0.3459 0.174 Uiso 1 1 calc R . .
H422 H 1.2059 -0.0260 0.3529 0.174 Uiso 1 1 calc R . .
H423 H 1.1446 -0.0471 0.2398 0.174 Uiso 1 1 calc R . .
N1 N 1.1675(2) 0.10041(6) 0.06550(17) 0.0530(5) Uani 1 1 d U . .
P3 P 0.92694(8) 0.111834(19) 0.12549(6) 0.0569(2) Uani 1 1 d . . .
P7 P 0.89744(8) -0.04970(2) 0.10403(6) 0.0555(2) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C60 C61 1.3900 . ?
C60 C65 1.3900 . ?
C61 C62 1.3900 . ?
C62 C63 1.3900 . ?
C63 C64 1.3900 . ?
C64 C65 1.3900 . ?
C50 C51 1.3900 . ?
C50 C55 1.3900 . ?
C51 C52 1.3900 . ?
C52 C53 1.3900 . ?
C53 C54 1.3900 . ?
C54 C55 1.3900 . ?
C2 N1 1.462(3) . ?
C2 P3 1.859(3) . ?
C4 C5 1.524(4) . ?
C4 P3 1.850(3) . ?
C5 C6 1.515(4) . ?
C6 P7 1.843(3) . ?
C11 N1 1.462(3) 3_755 ?
C11 P7 1.853(3) . ?
C17 N1 1.481(3) . ?
C17 C18 1.507(4) . ?
C17 C24 1.529(4) . ?
C18 C19 1.377(4) . ?
C18 C23 1.392(4) . ?
C19 C20 1.374(5) . ?
C20 C21 1.381(6) . ?
C21 C22 1.336(6) . ?
C22 C23 1.378(5) . ?
C25 C26 1.403(5) . ?
C25 C30 1.412(5) . ?
C25 P3 1.847(3) . ?
C26 C27 1.396(5) . ?
C26 C31 1.485(5) . ?
C27 C28 1.368(7) . ?
C28 C29 1.364(7) . ?
C28 C32 1.519(5) . ?
C29 C30 1.395(5) . ?
C30 C33 1.503(6) . ?
C34 C35 1.408(4) . ?
C34 C39 1.408(4) . ?
C34 P7 1.843(3) . ?
C35 C36 1.388(4) . ?
C35 C40 1.488(5) . ?
C36 C37 1.378(5) . ?
C37 C38 1.357(6) . ?
C37 C41 1.521(5) . ?
C38 C39 1.396(5) . ?
C39 C42 1.511(6) . ?
N1 C11 1.462(3) 3_755 ?

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
C61 C60 C65 120.0 . . ?
C60 C61 C62 120.0 . . ?
C61 C62 C63 120.0 . . ?
C64 C63 C62 120.0 . . ?
C63 C64 C65 120.0 . . ?
C64 C65 C60 120.0 . . ?
C51 C50 C55 120.0 . . ?
C50 C51 C52 120.0 . . ?
C53 C52 C51 120.0 . . ?
C52 C53 C54 120.0 . . ?
C55 C54 C53 120.0 . . ?
C54 C55 C50 120.0 . . ?
N1 C2 P3 108.61(18) . . ?
C5 C4 P3 109.8(2) . . ?
C6 C5 C4 114.4(2) . . ?
C5 C6 P7 110.2(2) . . ?
N1 C11 P7 109.02(18) 3_755 . ?
N1 C17 C18 109.1(2) . . ?
N1 C17 C24 113.9(2) . . ?
C18 C17 C24 114.7(3) . . ?
C19 C18 C23 117.2(3) . . ?
C19 C18 C17 119.8(3) . . ?
C23 C18 C17 122.9(3) . . ?
C20 C19 C18 121.6(3) . . ?
C19 C20 C21 119.7(4) . . ?
C22 C21 C20 119.5(4) . . ?
C21 C22 C23 121.5(4) . . ?
C22 C23 C18 120.4(3) . . ?
C26 C25 C30 118.9(3) . . ?
C26 C25 P3 125.7(3) . . ?
C30 C25 P3 115.4(3) . . ?
C27 C26 C25 118.9(4) . . ?
C27 C26 C31 117.4(4) . . ?
C25 C26 C31 123.7(3) . . ?
C28 C27 C26 122.8(4) . . ?
C29 C28 C27 117.7(4) . . ?
C29 C28 C32 119.9(6) . . ?
C27 C28 C32 122.3(6) . . ?
C28 C29 C30 123.0(5) . . ?
C29 C30 C25 118.7(4) . . ?
C29 C30 C33 118.1(4) . . ?
C25 C30 C33 123.2(3) . . ?
C35 C34 C39 118.7(3) . . ?
C35 C34 P7 126.3(2) . . ?
C39 C34 P7 115.0(2) . . ?
C36 C35 C34 118.6(3) . . ?
C36 C35 C40 117.6(3) . . ?
C34 C35 C40 123.9(3) . . ?
C37 C36 C35 123.8(4) . . ?
C38 C37 C36 116.4(3) . . ?
C38 C37 C41 122.8(4) . . ?
C36 C37 C41 120.7(5) . . ?
C37 C38 C39 123.7(4) . . ?
C38 C39 C34 118.8(3) . . ?
C38 C39 C42 118.7(3) . . ?
C34 C39 C42 122.5(3) . . ?
C11 N1 C2 112.6(2) 3_755 . ?
C11 N1 C17 112.5(2) 3_755 . ?
C2 N1 C17 112.6(2) . . ?
C25 P3 C4 106.60(14) . . ?
C25 P3 C2 103.74(13) . . ?
C4 P3 C2 100.52(14) . . ?
C34 P7 C6 103.61(13) . . ?
C34 P7 C11 104.22(12) . . ?
C6 P7 C11 103.82(13) . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        74.43
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.054

# start Validation Reply Form
_vrf_PLAT260_s14                 
;
PROBLEM: Large Average Ueq of Residue Including       C50      0.243 Check 
RESPONSE: Bad resolvable solvent
;
# end Validation Reply Form


####################################################################### 
# 
# 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_x0113fin_5RS
_database_code_depnum_ccdc_archive 'CCDC 1854867'
_audit_update_record             
;
2018-10-23 deposited with the CCDC.
2018-11-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C78 H102 N2 O2 P4'
_chemical_formula_weight         1223.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
P P 0.1023 0.0942 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_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                   11.3719(3)
_cell_length_b                   12.9401(5)
_cell_length_c                   13.1119(5)
_cell_angle_alpha                105.891(3)
_cell_angle_beta                 109.761(3)
_cell_angle_gamma                90.192(3)
_cell_volume                     1736.61(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    6683
_cell_measurement_theta_min      2.3820
_cell_measurement_theta_max      26.2730

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_F_000             660
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    0.156
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.95324
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean 16.3560
_diffrn_reflns_number            29902
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.007
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6357
_reflns_number_gt                4873
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    SHELXT-2014-5
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
 ORTEP3 for Windows
 L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.
 or
 DIAMOND Version 3.2k
 K. Brandenburg, Crystal Impact GbR, Bonn, Germany
;
_computing_publication_material  
;
 WINGX
 L.J. Farrugia,
 J. Appl. Cryst., 2012, 45, 849-854.
;
_refine_special_details          
;
Disordered structure: Methyl substituent C13 with ratio 0.783(9):0.217(9).
Solvent toluene molecule C33 to C39 treated as threefold disordered with a
ratio of 0.43(1):0.30(1):0.27(1).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0860P)²+2.6165P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6357
_refine_ls_number_parameters     455
_refine_ls_number_restraints     110
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0742
_refine_ls_wR_factor_ref         0.2045
_refine_ls_wR_factor_gt          0.1910
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.114
_refine_ls_shift/su_max          0.003
_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 0.33305(8) 0.53582(7) 0.58756(7) 0.0322(2) Uani 1 1 d . . . . .
P2 P 0.85286(8) 0.61404(7) 0.77260(7) 0.0345(2) Uani 1 1 d . . . . .
O1 O 0.4105(4) 0.9865(3) 0.3704(4) 0.1085(15) Uani 1 1 d . . . . .
N1 N 0.1595(2) 0.5630(2) 0.3979(2) 0.0319(6) Uani 1 1 d . . . . .
C1 C 0.1008(3) 0.4527(3) 0.3526(3) 0.0359(8) Uani 1 1 d . . . . .
C2 C 0.1969(3) 0.6037(3) 0.5205(3) 0.0354(8) Uani 1 1 d . . . . .
C3 C 0.4679(3) 0.6319(3) 0.6169(3) 0.0359(8) Uani 1 1 d . . . . .
C4 C 0.5908(3) 0.5929(3) 0.6792(3) 0.0343(7) Uani 1 1 d . . . . .
C5 C 0.7055(3) 0.6700(3) 0.7054(3) 0.0379(8) Uani 1 1 d . . . . .
C6 C 0.0835(3) 0.6371(3) 0.3402(3) 0.0452(9) Uani 0.784(9) 1 d D . P A 1
H6 H 0.052839 0.596671 0.257685 0.054 Uiso 0.784(9) 1 calc R U P A 1
C6F C 0.0835(3) 0.6371(3) 0.3402(3) 0.0452(9) Uani 0.216(9) 1 d D . P A 2
H6F H 0.038809 0.669662 0.393246 0.054 Uiso 0.216(9) 1 calc R U P A 2
C7 C 0.1685(4) 0.7337(3) 0.3527(3) 0.0492(10) Uani 1 1 d . . . . .
C8 C 0.1463(5) 0.8397(4) 0.3907(5) 0.0738(14) Uani 1 1 d . . . . .
H8 H 0.075238 0.854340 0.412784 0.089 Uiso 1 1 calc R U . . .
C9 C 0.2263(5) 0.9268(4) 0.3977(5) 0.0775(16) Uani 1 1 d . . . . .
H9 H 0.209237 0.998957 0.424710 0.093 Uiso 1 1 calc R U . . .
C10 C 0.3262(5) 0.9076(4) 0.3664(5) 0.0739(15) Uani 1 1 d . . . . .
C11 C 0.3480(5) 0.8030(4) 0.3247(4) 0.0724(14) Uani 1 1 d . . . . .
H11 H 0.416889 0.789031 0.299215 0.087 Uiso 1 1 calc R U . . .
C12 C 0.2708(4) 0.7182(3) 0.3197(4) 0.0523(10) Uani 1 1 d . . . . .
H12 H 0.289080 0.646490 0.292360 0.063 Uiso 1 1 calc R U . . .
C13 C -0.0311(4) 0.6659(5) 0.3663(5) 0.0527(16) Uani 0.784(9) 1 d D . P A 1
H13A H -0.082477 0.599868 0.354612 0.079 Uiso 0.784(9) 1 calc R U P A 1
H13B H -0.079397 0.706694 0.316096 0.079 Uiso 0.784(9) 1 calc R U P A 1
H13C H -0.007281 0.710311 0.445285 0.079 Uiso 0.784(9) 1 calc R U P A 1
C13F C -0.0198(13) 0.5899(12) 0.2364(11) 0.040(5) Uiso 0.216(9) 1 d D . P A 2
H13D H 0.010350 0.538240 0.183079 0.060 Uiso 0.216(9) 1 calc R U P A 2
H13E H -0.056343 0.646883 0.203331 0.060 Uiso 0.216(9) 1 calc R U P A 2
H13F H -0.083782 0.552338 0.252003 0.060 Uiso 0.216(9) 1 calc R U P A 2
C14 C 0.3950(7) 1.0954(4) 0.4206(8) 0.131(3) Uani 1 1 d . . . . .
H14A H 0.314512 1.113809 0.375094 0.197 Uiso 1 1 calc R U . . .
H14B H 0.463653 1.143546 0.423798 0.197 Uiso 1 1 calc R U . . .
H14C H 0.396064 1.103811 0.497509 0.197 Uiso 1 1 calc R U . . .
C15 C 0.3279(3) 0.5489(3) 0.7291(3) 0.0403(8) Uani 1 1 d . . . . .
C16 C 0.3073(4) 0.6439(4) 0.8034(3) 0.0568(11) Uani 1 1 d . . . . .
C17 C 0.3020(4) 0.6406(5) 0.9065(4) 0.0690(14) Uani 1 1 d . . . . .
H17 H 0.285881 0.704156 0.954627 0.083 Uiso 1 1 calc R U . . .
C18 C 0.3185(4) 0.5516(6) 0.9412(4) 0.0737(16) Uani 1 1 d . . . . .
C19 C 0.3407(4) 0.4580(5) 0.8708(4) 0.0701(15) Uani 1 1 d . . . . .
H19 H 0.353736 0.394883 0.895150 0.084 Uiso 1 1 calc R U . . .
C20 C 0.3442(3) 0.4556(4) 0.7635(3) 0.0507(10) Uani 1 1 d . . . . .
C21 C 0.2939(6) 0.7506(4) 0.7793(4) 0.0881(18) Uani 1 1 d . . . . .
H21A H 0.214543 0.746368 0.717058 0.132 Uiso 1 1 calc R U . . .
H21B H 0.364129 0.768932 0.757794 0.132 Uiso 1 1 calc R U . . .
H21C H 0.294291 0.806467 0.847195 0.132 Uiso 1 1 calc R U . . .
C22 C 0.3153(6) 0.5493(7) 1.0563(4) 0.119(3) Uani 1 1 d . . . . .
H22A H 0.350759 0.619635 1.112264 0.178 Uiso 1 1 calc R U . . .
H22B H 0.364891 0.492918 1.080497 0.178 Uiso 1 1 calc R U . . .
H22C H 0.228201 0.534037 1.049846 0.178 Uiso 1 1 calc R U . . .
C23 C 0.3662(5) 0.3505(4) 0.6909(4) 0.0691(13) Uani 1 1 d . . . . .
H23A H 0.293842 0.325861 0.620141 0.104 Uiso 1 1 calc R U . . .
H23B H 0.377127 0.296040 0.731723 0.104 Uiso 1 1 calc R U . . .
H23C H 0.442017 0.361293 0.673776 0.104 Uiso 1 1 calc R U . . .
C24 C 0.9657(3) 0.7350(3) 0.8548(3) 0.0416(9) Uani 1 1 d . . . . .
C25 C 1.0197(4) 0.7472(3) 0.9726(4) 0.0538(11) Uani 1 1 d . . . . .
C26 C 1.1015(4) 0.8388(4) 1.0428(4) 0.0667(13) Uani 1 1 d . . . . .
H26 H 1.136910 0.846987 1.121713 0.080 Uiso 1 1 calc R U . . .
C27 C 1.1323(4) 0.9165(4) 1.0025(5) 0.0656(14) Uani 1 1 d . . . . .
C28 C 1.0805(4) 0.9051(3) 0.8883(5) 0.0664(13) Uani 1 1 d . . . . .
H28 H 1.101068 0.960416 0.860315 0.080 Uiso 1 1 calc R U . . .
C29 C 0.9980(4) 0.8145(3) 0.8119(4) 0.0527(10) Uani 1 1 d . . . . .
C30 C 0.9945(6) 0.6649(4) 1.0253(4) 0.0895(18) Uani 1 1 d . . . . .
H30A H 1.038381 0.690662 1.107487 0.134 Uiso 1 1 calc R U . . .
H30B H 1.024691 0.596747 0.994211 0.134 Uiso 1 1 calc R U . . .
H30C H 0.903971 0.653156 1.008733 0.134 Uiso 1 1 calc R U . . .
C31 C 1.2226(5) 1.0165(4) 1.0813(6) 0.098(2) Uani 1 1 d . . . . .
H31A H 1.297451 1.017852 1.060326 0.147 Uiso 1 1 calc R U . . .
H31B H 1.247398 1.014068 1.159717 0.147 Uiso 1 1 calc R U . . .
H31C H 1.180852 1.081636 1.074232 0.147 Uiso 1 1 calc R U . . .
C32 C 0.9493(5) 0.8075(4) 0.6870(5) 0.0746(14) Uani 1 1 d . . . . .
H32A H 0.986407 0.749708 0.646121 0.112 Uiso 1 1 calc R U . . .
H32B H 0.972339 0.876440 0.677652 0.112 Uiso 1 1 calc R U . . .
H32C H 0.857597 0.791749 0.656604 0.112 Uiso 1 1 calc R U . . .
H1A H 0.007(4) 0.441(3) 0.330(3) 0.048(11) Uiso 1 1 d . . . . .
H1B H 0.140(3) 0.415(3) 0.410(3) 0.039(9) Uiso 1 1 d . . . . .
H2A H 0.222(3) 0.680(3) 0.542(3) 0.034(9) Uiso 1 1 d . . . . .
H2B H 0.129(3) 0.596(3) 0.547(3) 0.033(9) Uiso 1 1 d . . . . .
H3A H 0.468(3) 0.637(3) 0.546(3) 0.043(10) Uiso 1 1 d . . . . .
H3B H 0.462(3) 0.705(3) 0.650(3) 0.052(11) Uiso 1 1 d . . . . .
H4A H 0.603(4) 0.522(3) 0.637(4) 0.055(12) Uiso 1 1 d . . . . .
H4B H 0.588(4) 0.580(3) 0.750(4) 0.052(11) Uiso 1 1 d . . . . .
H5A H 0.704(3) 0.684(3) 0.642(3) 0.040(10) Uiso 1 1 d . . . . .
H5B H 0.703(4) 0.744(3) 0.762(4) 0.054(11) Uiso 1 1 d . . . . .
C33 C 0.6532(8) 0.8352(7) 0.0862(7) 0.062(3) Uiso 0.432(10) 1 d D . P B 1
C34 C 0.5539(10) 0.8820(12) 0.1104(10) 0.100(5) Uiso 0.432(10) 1 d D . P B 1
H34 H 0.471775 0.865286 0.054819 0.120 Uiso 0.432(10) 1 calc R U P B 1
C35 C 0.5739(12) 0.9533(12) 0.2160(10) 0.124(6) Uiso 0.432(10) 1 d D . P B 1
H35 H 0.506444 0.987918 0.233102 0.149 Uiso 0.432(10) 1 calc R U P B 1
C36 C 0.6932(11) 0.9733(10) 0.2962(10) 0.090(4) Uiso 0.432(10) 1 d D . P B 1
H36 H 0.707138 1.022898 0.368594 0.108 Uiso 0.432(10) 1 calc R U P B 1
C37 C 0.7924(10) 0.9242(10) 0.2749(9) 0.089(4) Uiso 0.432(10) 1 d D . P B 1
H37 H 0.873579 0.936923 0.331883 0.106 Uiso 0.432(10) 1 calc R U P B 1
C38 C 0.7701(8) 0.8548(8) 0.1667(8) 0.062(3) Uiso 0.432(10) 1 d D . P B 1
H38 H 0.837465 0.820740 0.148955 0.075 Uiso 0.432(10) 1 calc R U P B 1
C39 C 0.6300(11) 0.7567(9) -0.0308(9) 0.081(4) Uiso 0.432(10) 1 d D . P B 1
H39A H 0.567906 0.696885 -0.045117 0.122 Uiso 0.432(10) 1 calc R U P B 1
H39B H 0.708886 0.728322 -0.033917 0.122 Uiso 0.432(10) 1 calc R U P B 1
H39C H 0.598290 0.794500 -0.088467 0.122 Uiso 0.432(10) 1 calc R U P B 1
C33F C 0.7558(13) 0.9016(12) 0.2247(12) 0.103(4) Uiso 0.296(9) 1 d D . P C 2
C34F C 0.6323(13) 0.9158(15) 0.1927(13) 0.103(4) Uiso 0.296(9) 1 d D . P C 2
H34F H 0.601497 0.963187 0.245051 0.124 Uiso 0.296(9) 1 calc R U P C 2
C35F C 0.5503(13) 0.8627(17) 0.0855(14) 0.103(4) Uiso 0.296(9) 1 d D . P C 2
H35F H 0.463065 0.870126 0.066477 0.124 Uiso 0.296(9) 1 calc R U P C 2
C36F C 0.5936(14) 0.7987(14) 0.0055(13) 0.103(4) Uiso 0.296(9) 1 d D . P C 2
H36F H 0.537283 0.762911 -0.068819 0.124 Uiso 0.296(9) 1 calc R U P C 2
C37F C 0.7213(14) 0.7879(13) 0.0361(13) 0.103(4) Uiso 0.296(9) 1 d D . P C 2
H37F H 0.753626 0.744671 -0.017548 0.124 Uiso 0.296(9) 1 calc R U P C 2
C38F C 0.8006(14) 0.8399(15) 0.1442(13) 0.103(4) Uiso 0.296(9) 1 d D . P C 2
H38F H 0.888150 0.833410 0.164153 0.124 Uiso 0.296(9) 1 calc R U P C 2
C39F C 0.8447(16) 0.9543(15) 0.3414(13) 0.103(4) Uiso 0.296(9) 1 d D . P C 2
H39D H 0.929251 0.934053 0.347540 0.155 Uiso 0.296(9) 1 calc R U P C 2
H39E H 0.845638 1.032970 0.357852 0.155 Uiso 0.296(9) 1 calc R U P C 2
H39F H 0.817932 0.930726 0.395802 0.155 Uiso 0.296(9) 1 calc R U P C 2
C33G C 0.764(2) 0.871(2) 0.2151(18) 0.286(16) Uiso 0.272(9) 1 d D . P D 3
C34G C 0.650(3) 0.867(2) 0.132(3) 0.286(16) Uiso 0.272(9) 1 d D . P D 3
H34G H 0.626186 0.811208 0.062346 0.343 Uiso 0.272(9) 1 calc R U P D 3
C35G C 0.569(3) 0.944(2) 0.149(3) 0.286(16) Uiso 0.272(9) 1 d D . P D 3
H35G H 0.489649 0.940912 0.091650 0.343 Uiso 0.272(9) 1 calc R U P D 3
C36G C 0.605(3) 1.0251(19) 0.251(3) 0.286(16) Uiso 0.272(9) 1 d D . P D 3
H36G H 0.549721 1.077837 0.264364 0.343 Uiso 0.272(9) 1 calc R U P D 3
C37G C 0.720(4) 1.030(2) 0.3326(18) 0.286(16) Uiso 0.272(9) 1 d D . P D 3
H37G H 0.745064 1.087056 0.401441 0.343 Uiso 0.272(9) 1 calc R U P D 3
C38G C 0.801(3) 0.953(3) 0.3163(18) 0.286(16) Uiso 0.272(9) 1 d D . P D 3
H38G H 0.880580 0.955479 0.373519 0.343 Uiso 0.272(9) 1 calc R U P D 3
C39G C 0.8493(16) 0.786(2) 0.1951(18) 0.286(16) Uiso 0.272(9) 1 d D . P D 3
H39G H 0.926476 0.800275 0.261743 0.428 Uiso 0.272(9) 1 calc R U P D 3
H39H H 0.806854 0.715030 0.181470 0.428 Uiso 0.272(9) 1 calc R U P D 3
H39I H 0.870373 0.787349 0.128802 0.428 Uiso 0.272(9) 1 calc R U 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 C3 1.837(3) . ?
P1 C15 1.839(4) . ?
P1 C2 1.858(3) . ?
P2 C24 1.840(3) . ?
P2 C5 1.862(4) . ?
P2 C1 1.879(4) 2_666 ?
O1 C10 1.377(6) . ?
O1 C14 1.422(7) . ?
N1 C1 1.448(4) . ?
N1 C2 1.454(4) . ?
N1 C6F 1.482(4) . ?
N1 C6 1.482(4) . ?
C1 H1A 1.01(4) . ?
C1 H1B 1.00(4) . ?
C2 H2A 0.97(4) . ?
C2 H2B 0.96(4) . ?
C3 C4 1.528(5) . ?
C3 H3A 0.95(4) . ?
C3 H3B 0.94(4) . ?
C4 C5 1.522(5) . ?
C4 H4A 0.97(4) . ?
C4 H4B 1.00(4) . ?
C5 H5A 0.89(4) . ?
C5 H5B 1.04(4) . ?
C6 C13 1.480(6) . ?
C6 C7 1.516(5) . ?
C6 H6 1.0000 . ?
C6F C13F 1.437(13) . ?
C6F C7 1.516(5) . ?
C6F H6F 1.0000 . ?
C7 C12 1.369(6) . ?
C7 C8 1.381(6) . ?
C8 C9 1.409(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.334(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.372(7) . ?
C11 C12 1.377(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C13F H13D 0.9800 . ?
C13F H13E 0.9800 . ?
C13F H13F 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C20 1.391(6) . ?
C15 C16 1.419(6) . ?
C16 C17 1.386(6) . ?
C16 C21 1.496(7) . ?
C17 C18 1.342(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.389(8) . ?
C18 C22 1.530(6) . ?
C19 C20 1.414(6) . ?
C19 H19 0.9500 . ?
C20 C23 1.507(7) . ?
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 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C29 1.401(6) . ?
C24 C25 1.418(6) . ?
C25 C26 1.390(6) . ?
C25 C30 1.493(7) . ?
C26 C27 1.352(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.375(7) . ?
C27 C31 1.529(6) . ?
C28 C29 1.405(6) . ?
C28 H28 0.9500 . ?
C29 C32 1.517(7) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C38 1.359(8) . ?
C33 C34 1.373(8) . ?
C33 C39 1.525(11) . ?
C34 C35 1.381(9) . ?
C34 H34 0.9500 . ?
C35 C36 1.377(9) . ?
C35 H35 0.9500 . ?
C36 C37 1.370(9) . ?
C36 H36 0.9500 . ?
C37 C38 1.393(8) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C33F C34F 1.352(9) . ?
C33F C38F 1.385(9) . ?
C33F C39F 1.485(13) . ?
C34F C35F 1.378(9) . ?
C34F H34F 0.9500 . ?
C35F C36F 1.380(9) . ?
C35F H35F 0.9500 . ?
C36F C37F 1.389(9) . ?
C36F H36F 0.9500 . ?
C37F C38F 1.373(9) . ?
C37F H37F 0.9500 . ?
C38F H38F 0.9500 . ?
C39F H39D 0.9800 . ?
C39F H39E 0.9800 . ?
C39F H39F 0.9800 . ?
C33G C34G 1.377(10) . ?
C33G C38G 1.379(10) . ?
C33G C39G 1.496(14) . ?
C34G C35G 1.379(10) . ?
C34G H34G 0.9500 . ?
C35G C36G 1.385(10) . ?
C35G H35G 0.9500 . ?
C36G C37G 1.375(10) . ?
C36G H36G 0.9500 . ?
C37G C38G 1.384(10) . ?
C37G H37G 0.9500 . ?
C38G H38G 0.9500 . ?
C39G H39G 0.9800 . ?
C39G H39H 0.9800 . ?
C39G H39I 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
C3 P1 C15 103.20(16) . . ?
C3 P1 C2 102.77(17) . . ?
C15 P1 C2 104.29(16) . . ?
C24 P2 C5 103.56(16) . . ?
C24 P2 C1 106.21(16) . 2_666 ?
C5 P2 C1 101.94(17) . 2_666 ?
C10 O1 C14 116.8(6) . . ?
C1 N1 C2 113.0(3) . . ?
C1 N1 C6F 112.7(3) . . ?
C2 N1 C6F 112.2(3) . . ?
C1 N1 C6 112.7(3) . . ?
C2 N1 C6 112.2(3) . . ?
N1 C1 P2 107.3(2) . 2_666 ?
N1 C1 H1A 118.0(19) . . ?
P2 C1 H1A 110(2) 2_666 . ?
N1 C1 H1B 107(2) . . ?
P2 C1 H1B 106(2) 2_666 . ?
H1A C1 H1B 108(3) . . ?
N1 C2 P1 109.5(2) . . ?
N1 C2 H2A 108(2) . . ?
P1 C2 H2A 109(2) . . ?
N1 C2 H2B 113(2) . . ?
P1 C2 H2B 111(2) . . ?
H2A C2 H2B 107(3) . . ?
C4 C3 P1 110.8(2) . . ?
C4 C3 H3A 110(2) . . ?
P1 C3 H3A 107(2) . . ?
C4 C3 H3B 113(2) . . ?
P1 C3 H3B 117(2) . . ?
H3A C3 H3B 99(3) . . ?
C5 C4 C3 112.8(3) . . ?
C5 C4 H4A 108(2) . . ?
C3 C4 H4A 112(2) . . ?
C5 C4 H4B 111(2) . . ?
C3 C4 H4B 110(2) . . ?
H4A C4 H4B 103(3) . . ?
C4 C5 P2 110.9(2) . . ?
C4 C5 H5A 109(2) . . ?
P2 C5 H5A 113(2) . . ?
C4 C5 H5B 110(2) . . ?
P2 C5 H5B 107(2) . . ?
H5A C5 H5B 106(3) . . ?
C13 C6 N1 116.7(4) . . ?
C13 C6 C7 113.8(4) . . ?
N1 C6 C7 109.5(3) . . ?
C13 C6 H6 105.2 . . ?
N1 C6 H6 105.2 . . ?
C7 C6 H6 105.2 . . ?
C13F C6F N1 117.8(7) . . ?
C13F C6F C7 120.7(6) . . ?
N1 C6F C7 109.5(3) . . ?
C13F C6F H6F 101.6 . . ?
N1 C6F H6F 101.6 . . ?
C7 C6F H6F 101.6 . . ?
C12 C7 C8 116.1(4) . . ?
C12 C7 C6 119.8(3) . . ?
C8 C7 C6 123.9(4) . . ?
C12 C7 C6F 119.8(3) . . ?
C8 C7 C6F 123.9(4) . . ?
C7 C8 C9 121.8(5) . . ?
C7 C8 H8 119.1 . . ?
C9 C8 H8 119.1 . . ?
C10 C9 C8 119.9(4) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C9 C10 C11 119.5(5) . . ?
C9 C10 O1 124.6(5) . . ?
C11 C10 O1 115.8(5) . . ?
C10 C11 C12 120.4(5) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C7 C12 C11 122.3(4) . . ?
C7 C12 H12 118.9 . . ?
C11 C12 H12 118.9 . . ?
C6 C13 H13A 109.5 . . ?
C6 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C6 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C6F C13F H13D 109.5 . . ?
C6F C13F H13E 109.5 . . ?
H13D C13F H13E 109.5 . . ?
C6F C13F H13F 109.5 . . ?
H13D C13F H13F 109.5 . . ?
H13E C13F H13F 109.5 . . ?
O1 C14 H14A 109.5 . . ?
O1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C20 C15 C16 118.6(4) . . ?
C20 C15 P1 115.6(3) . . ?
C16 C15 P1 125.7(3) . . ?
C17 C16 C15 119.3(5) . . ?
C17 C16 C21 116.6(4) . . ?
C15 C16 C21 124.1(4) . . ?
C18 C17 C16 122.8(5) . . ?
C18 C17 H17 118.6 . . ?
C16 C17 H17 118.6 . . ?
C17 C18 C19 119.0(4) . . ?
C17 C18 C22 122.5(6) . . ?
C19 C18 C22 118.5(6) . . ?
C18 C19 C20 120.8(5) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 H19 119.6 . . ?
C15 C20 C19 119.5(4) . . ?
C15 C20 C23 122.8(4) . . ?
C19 C20 C23 117.7(4) . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22 H22A 109.5 . . ?
C18 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C18 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C29 C24 C25 119.2(3) . . ?
C29 C24 P2 126.0(3) . . ?
C25 C24 P2 114.7(3) . . ?
C26 C25 C24 119.1(4) . . ?
C26 C25 C30 117.9(4) . . ?
C24 C25 C30 123.0(3) . . ?
C27 C26 C25 122.2(5) . . ?
C27 C26 H26 118.9 . . ?
C25 C26 H26 118.9 . . ?
C26 C27 C28 119.0(4) . . ?
C26 C27 C31 121.3(5) . . ?
C28 C27 C31 119.7(5) . . ?
C27 C28 C29 122.1(5) . . ?
C27 C28 H28 118.9 . . ?
C29 C28 H28 118.9 . . ?
C24 C29 C28 118.3(4) . . ?
C24 C29 C32 123.4(3) . . ?
C28 C29 C32 118.2(4) . . ?
C25 C30 H30A 109.5 . . ?
C25 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C25 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C27 C31 H31A 109.5 . . ?
C27 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C27 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C38 C33 C34 120.6(7) . . ?
C38 C33 C39 120.1(7) . . ?
C34 C33 C39 119.2(8) . . ?
C33 C34 C35 119.7(8) . . ?
C33 C34 H34 120.1 . . ?
C35 C34 H34 120.1 . . ?
C36 C35 C34 118.9(8) . . ?
C36 C35 H35 120.6 . . ?
C34 C35 H35 120.6 . . ?
C37 C36 C35 122.2(8) . . ?
C37 C36 H36 118.9 . . ?
C35 C36 H36 118.9 . . ?
C36 C37 C38 117.6(8) . . ?
C36 C37 H37 121.2 . . ?
C38 C37 H37 121.2 . . ?
C33 C38 C37 120.9(8) . . ?
C33 C38 H38 119.5 . . ?
C37 C38 H38 119.5 . . ?
C33 C39 H39A 109.5 . . ?
C33 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C33 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C34F C33F C38F 118.4(9) . . ?
C34F C33F C39F 122.0(10) . . ?
C38F C33F C39F 119.5(9) . . ?
C33F C34F C35F 121.1(9) . . ?
C33F C34F H34F 119.5 . . ?
C35F C34F H34F 119.5 . . ?
C34F C35F C36F 120.7(9) . . ?
C34F C35F H35F 119.6 . . ?
C36F C35F H35F 119.6 . . ?
C35F C36F C37F 118.5(9) . . ?
C35F C36F H36F 120.8 . . ?
C37F C36F H36F 120.8 . . ?
C38F C37F C36F 119.7(9) . . ?
C38F C37F H37F 120.2 . . ?
C36F C37F H37F 120.2 . . ?
C37F C38F C33F 121.4(9) . . ?
C37F C38F H38F 119.3 . . ?
C33F C38F H38F 119.3 . . ?
C33F C39F H39D 109.5 . . ?
C33F C39F H39E 109.5 . . ?
H39D C39F H39E 109.5 . . ?
C33F C39F H39F 109.5 . . ?
H39D C39F H39F 109.5 . . ?
H39E C39F H39F 109.5 . . ?
C34G C33G C38G 120.8(9) . . ?
C34G C33G C39G 119.5(11) . . ?
C38G C33G C39G 119.7(11) . . ?
C33G C34G C35G 120.6(10) . . ?
C33G C34G H34G 119.7 . . ?
C35G C34G H34G 119.7 . . ?
C34G C35G C36G 118.8(10) . . ?
C34G C35G H35G 120.6 . . ?
C36G C35G H35G 120.6 . . ?
C37G C36G C35G 120.2(10) . . ?
C37G C36G H36G 119.9 . . ?
C35G C36G H36G 119.9 . . ?
C36G C37G C38G 121.1(10) . . ?
C36G C37G H37G 119.5 . . ?
C38G C37G H37G 119.5 . . ?
C33G C38G C37G 118.4(10) . . ?
C33G C38G H38G 120.8 . . ?
C37G C38G H38G 120.8 . . ?
C33G C39G H39G 109.5 . . ?
C33G C39G H39H 109.5 . . ?
H39G C39G H39H 109.5 . . ?
C33G C39G H39I 109.5 . . ?
H39G C39G H39I 109.5 . . ?
H39H C39G H39I 109.5 . . ?

_refine_diff_density_max         0.859
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.062

