# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_ax1822_MesStarPIMe4_cmp6
_database_code_depnum_ccdc_archive 'CCDC 2046859'
loop_
_audit_author_name
_audit_author_address
'Hering-Junghans C.'
;LIKAT Rostock
Germany
;
_audit_update_record             
;
2020-11-27 deposited with the CCDC.	2021-01-13 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H41 N2 P, C4 H8 O'
_chemical_formula_sum            'C29 H49 N2 O P'
_chemical_formula_weight         472.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

#==============================================================================

# CRYSTAL DATA

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

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

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

_cell_length_a                   15.0307(9)
_cell_length_b                   9.7034(6)
_cell_length_c                   20.4134(12)
_cell_angle_alpha                90
_cell_angle_beta                 104.0204(24)
_cell_angle_gamma                90
_cell_volume                     2888.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9879
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      30.16

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_F_000             1040
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.117
_shelx_estimated_absorpt_T_min   0.958
_shelx_estimated_absorpt_T_max   0.995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.958
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014)'

#==============================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            59656
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.396
_diffrn_reflns_theta_max         30.000
_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             8430
_reflns_number_gt                6370
_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.
 
 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.
;

_computing_data_collection       'Bruker Apex V7.51A'
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms 
 were positioned geometrically and refined using a riding model, with C---H = 
 0.98 (methyl groups), 0.99Å (methylene groups), 1.00Å (methine groups) or 
 0.95 Å (aryl CH) and with Uiso(H) = 1.5 times Ueq(C) 
 (methyl groups) or with Uiso(H) = 1.2 times Ueq(C) 
 (methylene  groups, aryl CH, methine groups). Torsion angles of all methyl 
 groups were allowed to refine. One of the o-mesityl groups in the terphenyl
 moiety was found to be disordered and was split in two parts.
 The occupancy of each part was allowed to refine freely. 

 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 > 2σ(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.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 -0.001 0.250 317 78 ' '
2 0.000 -0.018 0.750 317 78 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The unit cell contains four disordered THF molecules. These 
have been treated as a diffuse contribution to the overall scattering 
without specific atom positions by SQUEEZE/PLATON.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0548P)²+0.7221P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8430
_refine_ls_number_parameters     266
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0405
_refine_ls_wR_factor_ref         0.1136
_refine_ls_wR_factor_gt          0.1018
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.17049(2) 0.61619(3) 0.51347(2) 0.02325(8) Uani 1 1 d . . . . .
N1 N 0.14369(6) 0.34643(10) 0.47576(5) 0.0243(2) Uani 1 1 d . . . . .
N2 N 0.27075(6) 0.36100(10) 0.55322(5) 0.02243(19) Uani 1 1 d . . . . .
C1 C 0.28157(7) 0.70024(11) 0.55462(5) 0.0193(2) Uani 1 1 d . . . . .
C2 C 0.35408(7) 0.71085(11) 0.52088(5) 0.0211(2) Uani 1 1 d . . . . .
C3 C 0.44137(7) 0.75015(12) 0.55850(6) 0.0228(2) Uani 1 1 d . . . . .
H3 H 0.4904 0.7516 0.5366 0.027 Uiso 1 1 calc R U . . .
C4 C 0.45960(7) 0.78691(11) 0.62586(5) 0.0209(2) Uani 1 1 d . . . . .
C5 C 0.38536(7) 0.79233(12) 0.65545(5) 0.0219(2) Uani 1 1 d . . . . .
H5 H 0.3956 0.8231 0.7008 0.026 Uiso 1 1 calc R U . . .
C6 C 0.29664(7) 0.75461(11) 0.62150(5) 0.0199(2) Uani 1 1 d . . . . .
C7 C 0.34247(8) 0.69081(12) 0.44357(6) 0.0250(2) Uani 1 1 d . . . . .
C8 C 0.26716(9) 0.78857(14) 0.40543(6) 0.0313(3) Uani 1 1 d . . . . .
H8A H 0.2613 0.7796 0.3567 0.047 Uiso 1 1 calc R U . . .
H8B H 0.2834 0.8838 0.4194 0.047 Uiso 1 1 calc R U . . .
H8C H 0.2087 0.7647 0.4158 0.047 Uiso 1 1 calc R U . . .
C9 C 0.32230(10) 0.54143(14) 0.41939(6) 0.0351(3) Uani 1 1 d . . . . .
H9A H 0.3282 0.5330 0.3728 0.053 Uiso 1 1 calc R U . . .
H9B H 0.2598 0.5167 0.4214 0.053 Uiso 1 1 calc R U . . .
H9C H 0.3661 0.4793 0.4486 0.053 Uiso 1 1 calc R U . . .
C10 C 0.43020(9) 0.73177(16) 0.42183(6) 0.0366(3) Uani 1 1 d . . . . .
H10A H 0.4798 0.6680 0.4420 0.055 Uiso 1 1 calc R U . . .
H10B H 0.4479 0.8258 0.4372 0.055 Uiso 1 1 calc R U . . .
H10C H 0.4186 0.7276 0.3725 0.055 Uiso 1 1 calc R U . . .
C11 C 0.55627(7) 0.82428(12) 0.66703(6) 0.0240(2) Uani 1 1 d . . . . .
C12 C 0.59008(9) 0.71011(14) 0.71916(7) 0.0330(3) Uani 1 1 d . . . . .
H12A H 0.5916 0.6222 0.6958 0.049 Uiso 1 1 calc R U . . .
H12B H 0.5484 0.7026 0.7492 0.049 Uiso 1 1 calc R U . . .
H12C H 0.6518 0.7326 0.7458 0.049 Uiso 1 1 calc R U . . .
C13 C 0.55403(8) 0.96186(13) 0.70428(6) 0.0310(3) Uani 1 1 d . . . . .
H13A H 0.6165 0.9873 0.7284 0.047 Uiso 1 1 calc R U . . .
H13B H 0.5158 0.9518 0.7366 0.047 Uiso 1 1 calc R U . . .
H13C H 0.5284 1.0339 0.6715 0.047 Uiso 1 1 calc R U . . .
C14 C 0.62480(8) 0.83929(15) 0.62278(7) 0.0326(3) Uani 1 1 d . . . . .
H14A H 0.6325 0.7501 0.6023 0.049 Uiso 1 1 calc R U . . .
H14B H 0.6840 0.8702 0.6506 0.049 Uiso 1 1 calc R U . . .
H14C H 0.6017 0.9072 0.5872 0.049 Uiso 1 1 calc R U . . .
C15 C 0.21910(7) 0.77897(12) 0.65871(6) 0.0239(2) Uani 1 1 d . . . . .
C16 C 0.18244(9) 0.64316(14) 0.68103(7) 0.0319(3) Uani 1 1 d . . . . .
H16A H 0.1329 0.6632 0.7032 0.048 Uiso 1 1 calc R U . . .
H16B H 0.2321 0.5950 0.7127 0.048 Uiso 1 1 calc R U . . .
H16C H 0.1589 0.5849 0.6414 0.048 Uiso 1 1 calc R U . . .
C17 C 0.14055(8) 0.86275(13) 0.61398(6) 0.0281(2) Uani 1 1 d . . . . .
H17A H 0.1141 0.8109 0.5726 0.042 Uiso 1 1 calc R U . . .
H17B H 0.1644 0.9509 0.6022 0.042 Uiso 1 1 calc R U . . .
H17C H 0.0932 0.8797 0.6386 0.042 Uiso 1 1 calc R U . . .
C18 C 0.25272(9) 0.86597(15) 0.72305(6) 0.0337(3) Uani 1 1 d . . . . .
H18A H 0.2012 0.8850 0.7433 0.051 Uiso 1 1 calc R U . . .
H18B H 0.2781 0.9531 0.7114 0.051 Uiso 1 1 calc R U . . .
H18C H 0.3003 0.8152 0.7554 0.051 Uiso 1 1 calc R U . . .
C19 C 0.20011(7) 0.43926(12) 0.51661(5) 0.0212(2) Uani 1 1 d . . . . .
C20 C 0.17794(8) 0.21255(12) 0.48741(6) 0.0268(2) Uani 1 1 d . . . . .
C21 C 0.25744(8) 0.22126(12) 0.53512(6) 0.0252(2) Uani 1 1 d . . . . .
C22 C 0.06160(8) 0.38649(13) 0.42547(6) 0.0314(3) Uani 1 1 d . . . . .
H22A H 0.0110 0.3998 0.4474 0.047 Uiso 1 1 calc R U . . .
H22B H 0.0454 0.3140 0.3913 0.047 Uiso 1 1 calc R U . . .
H22C H 0.0731 0.4727 0.4039 0.047 Uiso 1 1 calc R U . . .
C23 C 0.12874(10) 0.09108(14) 0.45105(8) 0.0389(3) Uani 1 1 d . . . . .
H23A H 0.1624 0.0067 0.4680 0.058 Uiso 1 1 calc R U . . .
H23B H 0.1246 0.1003 0.4026 0.058 Uiso 1 1 calc R U . . .
H23C H 0.0669 0.0864 0.4587 0.058 Uiso 1 1 calc R U . . .
C24 C 0.32382(9) 0.11213(13) 0.56608(7) 0.0339(3) Uani 1 1 d . . . . .
H24A H 0.3022 0.0227 0.5461 0.051 Uiso 1 1 calc R U . . .
H24B H 0.3291 0.1091 0.6149 0.051 Uiso 1 1 calc R U . . .
H24C H 0.3839 0.1326 0.5577 0.051 Uiso 1 1 calc R U . . .
C25 C 0.34317(8) 0.41064(13) 0.60892(6) 0.0288(3) Uani 1 1 d . . . . .
H25A H 0.3847 0.4703 0.5914 0.043 Uiso 1 1 calc R U . . .
H25B H 0.3775 0.3321 0.6326 0.043 Uiso 1 1 calc R U . . .
H25C H 0.3161 0.4631 0.6403 0.043 Uiso 1 1 calc R U . . .


#==============================================================================

# MOLECULAR GEOMETRY

_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 C19 1.7709(12) . ?
P1 C1 1.8653(11) . ?
N1 C19 1.3723(14) . ?
N1 C20 1.3964(15) . ?
N1 C22 1.4539(15) . ?
N2 C19 1.3704(14) . ?
N2 C21 1.4069(15) . ?
N2 C25 1.4527(14) . ?
C1 C2 1.4270(15) . ?
C1 C6 1.4296(15) . ?
C2 C3 1.4030(15) . ?
C2 C7 1.5575(15) . ?
C3 C4 1.3822(15) . ?
C3 H3 0.9500 . ?
C4 C5 1.3926(15) . ?
C4 C11 1.5354(15) . ?
C5 C6 1.3946(15) . ?
C5 H5 0.9500 . ?
C6 C15 1.5556(15) . ?
C7 C8 1.5364(17) . ?
C7 C9 1.5376(18) . ?
C7 C10 1.5417(17) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C14 1.5326(17) . ?
C11 C12 1.5350(17) . ?
C11 C13 1.5407(17) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C17 1.5383(16) . ?
C15 C16 1.5393(17) . ?
C15 C18 1.5400(16) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C20 C21 1.3490(17) . ?
C20 C23 1.4903(17) . ?
C21 C24 1.4869(17) . ?
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 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 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
C19 P1 C1 102.58(5) . . ?
C19 N1 C20 111.05(9) . . ?
C19 N1 C22 123.19(10) . . ?
C20 N1 C22 125.72(10) . . ?
C19 N2 C21 110.42(9) . . ?
C19 N2 C25 125.29(10) . . ?
C21 N2 C25 123.85(9) . . ?
C2 C1 C6 118.13(9) . . ?
C2 C1 P1 121.27(8) . . ?
C6 C1 P1 120.59(8) . . ?
C3 C2 C1 118.54(9) . . ?
C3 C2 C7 116.67(10) . . ?
C1 C2 C7 124.68(10) . . ?
C4 C3 C2 123.25(10) . . ?
C4 C3 H3 118.4 . . ?
C2 C3 H3 118.4 . . ?
C3 C4 C5 117.05(10) . . ?
C3 C4 C11 122.59(10) . . ?
C5 C4 C11 120.34(10) . . ?
C4 C5 C6 123.01(10) . . ?
C4 C5 H5 118.5 . . ?
C6 C5 H5 118.5 . . ?
C5 C6 C1 118.85(9) . . ?
C5 C6 C15 117.19(9) . . ?
C1 C6 C15 123.94(9) . . ?
C8 C7 C9 110.83(10) . . ?
C8 C7 C10 105.76(10) . . ?
C9 C7 C10 105.45(10) . . ?
C8 C7 C2 108.93(9) . . ?
C9 C7 C2 114.08(9) . . ?
C10 C7 C2 111.46(10) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C14 C11 C12 108.68(10) . . ?
C14 C11 C4 112.46(9) . . ?
C12 C11 C4 108.62(9) . . ?
C14 C11 C13 107.86(10) . . ?
C12 C11 C13 109.04(10) . . ?
C4 C11 C13 110.11(9) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C17 C15 C16 110.48(10) . . ?
C17 C15 C18 105.23(10) . . ?
C16 C15 C18 106.49(10) . . ?
C17 C15 C6 110.39(9) . . ?
C16 C15 C6 112.25(10) . . ?
C18 C15 C6 111.70(9) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C19 N1 104.52(9) . . ?
N2 C19 P1 135.38(8) . . ?
N1 C19 P1 120.09(8) . . ?
C21 C20 N1 106.87(10) . . ?
C21 C20 C23 130.92(12) . . ?
N1 C20 C23 122.21(11) . . ?
C20 C21 N2 107.14(10) . . ?
C20 C21 C24 130.40(11) . . ?
N2 C21 C24 122.46(10) . . ?
N1 C22 H22A 109.5 . . ?
N1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N1 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 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N2 C25 H25A 109.5 . . ?
N2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 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
C19 P1 C1 C2 73.25(10) . . . . ?
C19 P1 C1 C6 -106.03(9) . . . . ?
C6 C1 C2 C3 11.55(15) . . . . ?
P1 C1 C2 C3 -167.75(8) . . . . ?
C6 C1 C2 C7 -164.39(10) . . . . ?
P1 C1 C2 C7 16.31(15) . . . . ?
C1 C2 C3 C4 -3.87(17) . . . . ?
C7 C2 C3 C4 172.40(10) . . . . ?
C2 C3 C4 C5 -3.98(17) . . . . ?
C2 C3 C4 C11 177.58(10) . . . . ?
C3 C4 C5 C6 4.04(17) . . . . ?
C11 C4 C5 C6 -177.48(10) . . . . ?
C4 C5 C6 C1 3.75(17) . . . . ?
C4 C5 C6 C15 -174.45(10) . . . . ?
C2 C1 C6 C5 -11.52(15) . . . . ?
P1 C1 C6 C5 167.78(8) . . . . ?
C2 C1 C6 C15 166.55(10) . . . . ?
P1 C1 C6 C15 -14.15(15) . . . . ?
C3 C2 C7 C8 -121.41(11) . . . . ?
C1 C2 C7 C8 54.61(14) . . . . ?
C3 C2 C7 C9 114.19(12) . . . . ?
C1 C2 C7 C9 -69.79(14) . . . . ?
C3 C2 C7 C10 -5.10(15) . . . . ?
C1 C2 C7 C10 170.92(11) . . . . ?
C3 C4 C11 C14 9.50(16) . . . . ?
C5 C4 C11 C14 -168.89(11) . . . . ?
C3 C4 C11 C12 -110.84(12) . . . . ?
C5 C4 C11 C12 70.77(13) . . . . ?
C3 C4 C11 C13 129.82(12) . . . . ?
C5 C4 C11 C13 -48.58(14) . . . . ?
C5 C6 C15 C17 126.94(11) . . . . ?
C1 C6 C15 C17 -51.16(14) . . . . ?
C5 C6 C15 C16 -109.32(12) . . . . ?
C1 C6 C15 C16 72.58(13) . . . . ?
C5 C6 C15 C18 10.22(14) . . . . ?
C1 C6 C15 C18 -167.88(11) . . . . ?
C21 N2 C19 N1 -0.27(12) . . . . ?
C25 N2 C19 N1 -172.85(10) . . . . ?
C21 N2 C19 P1 178.58(9) . . . . ?
C25 N2 C19 P1 6.00(18) . . . . ?
C20 N1 C19 N2 0.82(12) . . . . ?
C22 N1 C19 N2 -176.76(10) . . . . ?
C20 N1 C19 P1 -178.25(8) . . . . ?
C22 N1 C19 P1 4.17(15) . . . . ?
C1 P1 C19 N2 18.77(13) . . . . ?
C1 P1 C19 N1 -162.52(9) . . . . ?
C19 N1 C20 C21 -1.07(13) . . . . ?
C22 N1 C20 C21 176.43(11) . . . . ?
C19 N1 C20 C23 178.37(11) . . . . ?
C22 N1 C20 C23 -4.12(19) . . . . ?
N1 C20 C21 N2 0.85(13) . . . . ?
C23 C20 C21 N2 -178.53(13) . . . . ?
N1 C20 C21 C24 -178.80(12) . . . . ?
C23 C20 C21 C24 1.8(2) . . . . ?
C19 N2 C21 C20 -0.38(13) . . . . ?
C25 N2 C21 C20 172.33(11) . . . . ?
C19 N2 C21 C24 179.31(11) . . . . ?
C25 N2 C21 C24 -7.98(18) . . . . ?

_refine_diff_density_max         0.389
_refine_diff_density_min         -0.165
_refine_diff_density_rms         0.042


####################################################################### 
# 
# 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_ax1867_DippTerPIMe4_cmp12
_database_code_depnum_ccdc_archive 'CCDC 2046862'
loop_
_audit_author_name
_audit_author_address
'Hering-Junghans C.'
;LIKAT Rostock
Germany
;
_audit_update_record             
;
2020-11-27 deposited with the CCDC.	2021-01-13 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT230_ax1867_DippTerPIMe4_cmp12 
;
PROBLEM: Hirshfeld Test Diff for    P1       --C31      .        7.4 s.u.
RESPONSE: This was carefully checked for an underlying disorder. No indication of such were found.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H49 N2 P, C5 H12'
_chemical_formula_sum            'C42 H61 N2 P'
_chemical_formula_weight         624.89

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

#==============================================================================

# CRYSTAL DATA

_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                   11.1141(8)
_cell_length_b                   13.0309(9)
_cell_length_c                   14.5537(10)
_cell_angle_alpha                107.3420(10)
_cell_angle_beta                 102.5540(10)
_cell_angle_gamma                96.1670(10)
_cell_volume                     1930.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9842
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      30.17

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_F_000             684
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.101
_shelx_estimated_absorpt_T_min   0.973
_shelx_estimated_absorpt_T_max   0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014)'

#==============================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            66599
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.519
_diffrn_reflns_theta_max         29.999
_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             11264
_reflns_number_gt                8675
_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.
 
 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.
;

_computing_data_collection       'Bruker Apex V7.51A'
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms 
 were positioned geometrically and refined using a riding model, with C---H = 
 0.98 (methyl groups), 0.99Å (methylene groups), 1.00Å (methine groups) or 
 0.95 Å (aryl CH) and with Uiso(H) = 1.5 times Ueq(C) 
 (methyl groups) or with Uiso(H) = 1.2 times Ueq(C) 
 (methylene  groups, aryl CH, methine groups). Torsion angles of all methyl 
 groups were allowed to refine. 

 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 > 2σ(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.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.500 400 82 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The unit cell contains two heavily disordered pentane molecules. These 
have been treated as a diffuse contribution to the overall scattering 
without specific atom positions by SQUEEZE/PLATON.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0622P)²+0.3078P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11264
_refine_ls_number_parameters     373
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0425
_refine_ls_wR_factor_ref         0.1213
_refine_ls_wR_factor_gt          0.1108
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.35461(3) 0.47688(2) 0.31889(2) 0.02934(8) Uani 1 1 d . . . . .
N1 N 0.56983(9) 0.64770(8) 0.39092(7) 0.0311(2) Uani 1 1 d . . . . .
N2 N 0.46492(9) 0.64994(7) 0.49926(7) 0.02875(19) Uani 1 1 d . . . . .
C1 C 0.28615(9) 0.51247(7) 0.20898(7) 0.02034(18) Uani 1 1 d . . . . .
C2 C 0.25541(9) 0.42645(8) 0.11570(7) 0.02166(19) Uani 1 1 d . . . . .
C3 C 0.19480(9) 0.44225(8) 0.02807(7) 0.0246(2) Uani 1 1 d . . . . .
H3 H 0.1768 0.3839 -0.0334 0.030 Uiso 1 1 calc R U . . .
C4 C 0.16019(10) 0.54159(8) 0.02871(8) 0.0258(2) Uani 1 1 d . . . . .
H4 H 0.1215 0.5526 -0.0317 0.031 Uiso 1 1 calc R U . . .
C5 C 0.18350(9) 0.62421(8) 0.11947(8) 0.0242(2) Uani 1 1 d . . . . .
H5 H 0.1577 0.6917 0.1208 0.029 Uiso 1 1 calc R U . . .
C6 C 0.24367(9) 0.61171(8) 0.20917(7) 0.02091(18) Uani 1 1 d . . . . .
C7 C 0.27711(9) 0.31243(8) 0.10709(7) 0.02310(19) Uani 1 1 d . . . . .
C8 C 0.18335(10) 0.23819(8) 0.11742(8) 0.0270(2) Uani 1 1 d . . . . .
C9 C 0.19818(11) 0.12942(9) 0.10017(8) 0.0329(2) Uani 1 1 d . . . . .
H9 H 0.1355 0.0786 0.1070 0.040 Uiso 1 1 calc R U . . .
C10 C 0.30234(12) 0.09489(9) 0.07349(9) 0.0361(3) Uani 1 1 d . . . . .
H10 H 0.3108 0.0206 0.0615 0.043 Uiso 1 1 calc R U . . .
C11 C 0.39466(12) 0.16818(9) 0.06411(9) 0.0341(2) Uani 1 1 d . . . . .
H11 H 0.4664 0.1437 0.0461 0.041 Uiso 1 1 calc R U . . .
C12 C 0.38413(10) 0.27773(8) 0.08063(8) 0.0265(2) Uani 1 1 d . . . . .
C13 C 0.06620(11) 0.27247(9) 0.14537(10) 0.0352(3) Uani 1 1 d . . . . .
H13 H 0.0727 0.3523 0.1550 0.042 Uiso 1 1 calc R U . . .
C14 C 0.05653(14) 0.25679(13) 0.24344(11) 0.0498(3) Uani 1 1 d . . . . .
H14A H 0.0493 0.1790 0.2362 0.075 Uiso 1 1 calc R U . . .
H14B H -0.0177 0.2829 0.2608 0.075 Uiso 1 1 calc R U . . .
H14C H 0.1318 0.2984 0.2964 0.075 Uiso 1 1 calc R U . . .
C15 C -0.05198(13) 0.21210(13) 0.06140(12) 0.0505(3) Uani 1 1 d . . . . .
H15A H -0.0435 0.2237 -0.0006 0.076 Uiso 1 1 calc R U . . .
H15B H -0.1251 0.2403 0.0790 0.076 Uiso 1 1 calc R U . . .
H15C H -0.0629 0.1337 0.0520 0.076 Uiso 1 1 calc R U . . .
C16 C 0.48436(11) 0.35603(9) 0.06650(9) 0.0313(2) Uani 1 1 d . . . . .
H16 H 0.4729 0.4320 0.0998 0.038 Uiso 1 1 calc R U . . .
C17 C 0.46830(14) 0.34084(12) -0.04398(10) 0.0454(3) Uani 1 1 d . . . . .
H17A H 0.4742 0.2656 -0.0795 0.068 Uiso 1 1 calc R U . . .
H17B H 0.5343 0.3918 -0.0512 0.068 Uiso 1 1 calc R U . . .
H17C H 0.3861 0.3554 -0.0721 0.068 Uiso 1 1 calc R U . . .
C18 C 0.61743(12) 0.34630(12) 0.11485(12) 0.0479(3) Uani 1 1 d . . . . .
H18A H 0.6254 0.3537 0.1850 0.072 Uiso 1 1 calc R U . . .
H18B H 0.6778 0.4042 0.1106 0.072 Uiso 1 1 calc R U . . .
H18C H 0.6343 0.2747 0.0798 0.072 Uiso 1 1 calc R U . . .
C19 C 0.24801(9) 0.70341(8) 0.30223(7) 0.02317(19) Uani 1 1 d . . . . .
C20 C 0.16029(10) 0.69120(9) 0.35733(8) 0.0269(2) Uani 1 1 d . . . . .
C21 C 0.15863(12) 0.77967(10) 0.43876(9) 0.0355(3) Uani 1 1 d . . . . .
H21 H 0.1012 0.7721 0.4771 0.043 Uiso 1 1 calc R U . . .
C22 C 0.23916(13) 0.87872(11) 0.46505(10) 0.0423(3) Uani 1 1 d . . . . .
H22 H 0.2371 0.9380 0.5213 0.051 Uiso 1 1 calc R U . . .
C23 C 0.32206(12) 0.89118(10) 0.40974(9) 0.0391(3) Uani 1 1 d . . . . .
H23 H 0.3762 0.9596 0.4278 0.047 Uiso 1 1 calc R U . . .
C24 C 0.32787(10) 0.80488(8) 0.32745(8) 0.0280(2) Uani 1 1 d . . . . .
C25 C 0.06142(11) 0.58801(10) 0.32281(9) 0.0356(3) Uani 1 1 d . . . . .
H25 H 0.0970 0.5260 0.2860 0.043 Uiso 1 1 calc R U . . .
C26 C 0.02058(14) 0.55794(13) 0.40657(12) 0.0490(3) Uani 1 1 d . . . . .
H26A H 0.0946 0.5541 0.4554 0.074 Uiso 1 1 calc R U . . .
H26B H -0.0360 0.4867 0.3787 0.074 Uiso 1 1 calc R U . . .
H26C H -0.0230 0.6137 0.4394 0.074 Uiso 1 1 calc R U . . .
C27 C -0.05372(13) 0.59965(15) 0.24967(11) 0.0570(4) Uani 1 1 d . . . . .
H27A H -0.0911 0.6596 0.2841 0.085 Uiso 1 1 calc R U . . .
H27B H -0.1153 0.5313 0.2240 0.085 Uiso 1 1 calc R U . . .
H27C H -0.0285 0.6155 0.1941 0.085 Uiso 1 1 calc R U . . .
C28 C 0.41656(11) 0.82400(9) 0.26582(9) 0.0315(2) Uani 1 1 d . . . . .
H28 H 0.4288 0.7510 0.2252 0.038 Uiso 1 1 calc R U . . .
C29 C 0.36287(13) 0.88344(10) 0.19361(10) 0.0413(3) Uani 1 1 d . . . . .
H29A H 0.2864 0.8371 0.1450 0.062 Uiso 1 1 calc R U . . .
H29B H 0.4250 0.8985 0.1585 0.062 Uiso 1 1 calc R U . . .
H29C H 0.3430 0.9525 0.2314 0.062 Uiso 1 1 calc R U . . .
C30 C 0.54537(12) 0.89017(11) 0.33018(11) 0.0430(3) Uani 1 1 d . . . . .
H30A H 0.5390 0.9671 0.3582 0.065 Uiso 1 1 calc R U . . .
H30B H 0.6051 0.8843 0.2891 0.065 Uiso 1 1 calc R U . . .
H30C H 0.5746 0.8615 0.3845 0.065 Uiso 1 1 calc R U . . .
C31 C 0.46143(10) 0.60030(8) 0.40215(8) 0.0267(2) Uani 1 1 d . . . . .
C32 C 0.64026(11) 0.72622(9) 0.48049(9) 0.0344(3) Uani 1 1 d . . . . .
C33 C 0.57383(11) 0.72770(9) 0.54805(8) 0.0322(2) Uani 1 1 d . . . . .
C34 C 0.61205(13) 0.61284(12) 0.30071(10) 0.0428(3) Uani 1 1 d . . . . .
H34A H 0.5560 0.5458 0.2537 0.064 Uiso 1 1 calc R U . . .
H34B H 0.6976 0.5987 0.3174 0.064 Uiso 1 1 calc R U . . .
H34C H 0.6110 0.6705 0.2702 0.064 Uiso 1 1 calc R U . . .
C35 C 0.36990(12) 0.62453(11) 0.54768(9) 0.0376(3) Uani 1 1 d . . . . .
H35A H 0.3038 0.5650 0.4998 0.056 Uiso 1 1 calc R U . . .
H35B H 0.3336 0.6895 0.5718 0.056 Uiso 1 1 calc R U . . .
H35C H 0.4082 0.6020 0.6041 0.056 Uiso 1 1 calc R U . . .
C36 C 0.76714(13) 0.78768(12) 0.49248(12) 0.0499(3) Uani 1 1 d . . . . .
H36A H 0.7923 0.8481 0.5561 0.075 Uiso 1 1 calc R U . . .
H36B H 0.7646 0.8169 0.4375 0.075 Uiso 1 1 calc R U . . .
H36C H 0.8278 0.7383 0.4917 0.075 Uiso 1 1 calc R U . . .
C37 C 0.60043(14) 0.79571(10) 0.65493(9) 0.0425(3) Uani 1 1 d . . . . .
H37A H 0.6816 0.8450 0.6750 0.064 Uiso 1 1 calc R U . . .
H37B H 0.6029 0.7480 0.6960 0.064 Uiso 1 1 calc R U . . .
H37C H 0.5343 0.8388 0.6642 0.064 Uiso 1 1 calc R U . . .


#==============================================================================

# MOLECULAR GEOMETRY

_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 C31 1.8074(11) . ?
P1 C1 1.8280(10) . ?
N1 C31 1.3585(15) . ?
N1 C32 1.3958(14) . ?
N1 C34 1.4520(16) . ?
N2 C31 1.3576(14) . ?
N2 C33 1.3891(14) . ?
N2 C35 1.4523(16) . ?
C1 C6 1.4229(13) . ?
C1 C2 1.4231(13) . ?
C2 C3 1.3913(14) . ?
C2 C7 1.5035(13) . ?
C3 C4 1.3875(14) . ?
C3 H3 0.9500 . ?
C4 C5 1.3837(14) . ?
C4 H4 0.9500 . ?
C5 C6 1.3960(14) . ?
C5 H5 0.9500 . ?
C6 C19 1.5030(13) . ?
C7 C12 1.4066(15) . ?
C7 C8 1.4080(14) . ?
C8 C9 1.3983(15) . ?
C8 C13 1.5189(16) . ?
C9 C10 1.3772(18) . ?
C9 H9 0.9500 . ?
C10 C11 1.3826(17) . ?
C10 H10 0.9500 . ?
C11 C12 1.3974(15) . ?
C11 H11 0.9500 . ?
C12 C16 1.5182(15) . ?
C13 C14 1.5253(19) . ?
C13 C15 1.5312(18) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.5278(18) . ?
C16 C18 1.5295(18) . ?
C16 H16 1.0000 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C24 1.4098(14) . ?
C19 C20 1.4148(15) . ?
C20 C21 1.3905(15) . ?
C20 C25 1.5191(15) . ?
C21 C22 1.3863(18) . ?
C21 H21 0.9500 . ?
C22 C23 1.3754(19) . ?
C22 H22 0.9500 . ?
C23 C24 1.3963(15) . ?
C23 H23 0.9500 . ?
C24 C28 1.5176(16) . ?
C25 C26 1.5273(18) . ?
C25 C27 1.530(2) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C30 1.5299(17) . ?
C28 C29 1.5402(17) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C32 C33 1.3490(18) . ?
C32 C36 1.4924(18) . ?
C33 C37 1.4881(16) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 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
C31 P1 C1 104.21(5) . . ?
C31 N1 C32 110.82(10) . . ?
C31 N1 C34 124.14(10) . . ?
C32 N1 C34 124.74(10) . . ?
C31 N2 C33 111.01(10) . . ?
C31 N2 C35 125.24(10) . . ?
C33 N2 C35 123.74(10) . . ?
C6 C1 C2 116.90(8) . . ?
C6 C1 P1 126.20(7) . . ?
C2 C1 P1 116.16(7) . . ?
C3 C2 C1 121.04(9) . . ?
C3 C2 C7 116.40(8) . . ?
C1 C2 C7 122.40(9) . . ?
C4 C3 C2 121.28(9) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C5 C4 C3 118.36(9) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
C4 C5 C6 122.19(9) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C5 C6 C1 120.01(9) . . ?
C5 C6 C19 115.73(9) . . ?
C1 C6 C19 124.00(9) . . ?
C12 C7 C8 120.45(9) . . ?
C12 C7 C2 120.52(9) . . ?
C8 C7 C2 118.81(9) . . ?
C9 C8 C7 118.82(10) . . ?
C9 C8 C13 119.21(10) . . ?
C7 C8 C13 121.97(9) . . ?
C10 C9 C8 120.93(10) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C9 C10 C11 120.11(10) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C10 C11 C12 121.09(11) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C11 C12 C7 118.61(10) . . ?
C11 C12 C16 120.28(10) . . ?
C7 C12 C16 121.08(9) . . ?
C8 C13 C14 111.63(11) . . ?
C8 C13 C15 111.26(11) . . ?
C14 C13 C15 111.10(11) . . ?
C8 C13 H13 107.5 . . ?
C14 C13 H13 107.5 . . ?
C15 C13 H13 107.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C12 C16 C17 111.01(10) . . ?
C12 C16 C18 112.81(10) . . ?
C17 C16 C18 110.44(11) . . ?
C12 C16 H16 107.4 . . ?
C17 C16 H16 107.4 . . ?
C18 C16 H16 107.4 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C24 C19 C20 120.20(9) . . ?
C24 C19 C6 120.31(9) . . ?
C20 C19 C6 119.04(9) . . ?
C21 C20 C19 118.55(10) . . ?
C21 C20 C25 120.22(10) . . ?
C19 C20 C25 120.95(9) . . ?
C22 C21 C20 121.26(11) . . ?
C22 C21 H21 119.4 . . ?
C20 C21 H21 119.4 . . ?
C23 C22 C21 120.02(11) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C24 121.05(11) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C23 C24 C19 118.87(10) . . ?
C23 C24 C28 119.16(10) . . ?
C19 C24 C28 121.95(9) . . ?
C20 C25 C26 114.79(11) . . ?
C20 C25 C27 109.41(11) . . ?
C26 C25 C27 109.20(11) . . ?
C20 C25 H25 107.7 . . ?
C26 C25 H25 107.7 . . ?
C27 C25 H25 107.7 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 C28 C30 112.69(10) . . ?
C24 C28 C29 111.99(10) . . ?
C30 C28 C29 108.11(10) . . ?
C24 C28 H28 108.0 . . ?
C30 C28 H28 108.0 . . ?
C29 C28 H28 108.0 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N2 C31 N1 104.71(9) . . ?
N2 C31 P1 125.47(9) . . ?
N1 C31 P1 128.21(8) . . ?
C33 C32 N1 106.58(10) . . ?
C33 C32 C36 130.32(11) . . ?
N1 C32 C36 123.01(12) . . ?
C32 C33 N2 106.87(10) . . ?
C32 C33 C37 130.95(11) . . ?
N2 C33 C37 122.17(12) . . ?
N1 C34 H34A 109.5 . . ?
N1 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N1 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N2 C35 H35A 109.5 . . ?
N2 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
N2 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C32 C36 H36A 109.5 . . ?
C32 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C32 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C33 C37 H37A 109.5 . . ?
C33 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C33 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 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
C31 P1 C1 C6 -43.18(9) . . . . ?
C31 P1 C1 C2 147.01(7) . . . . ?
C6 C1 C2 C3 4.64(14) . . . . ?
P1 C1 C2 C3 175.44(8) . . . . ?
C6 C1 C2 C7 -170.59(9) . . . . ?
P1 C1 C2 C7 0.20(12) . . . . ?
C1 C2 C3 C4 -1.19(15) . . . . ?
C7 C2 C3 C4 174.32(9) . . . . ?
C2 C3 C4 C5 -2.20(15) . . . . ?
C3 C4 C5 C6 1.98(15) . . . . ?
C4 C5 C6 C1 1.62(15) . . . . ?
C4 C5 C6 C19 -172.81(9) . . . . ?
C2 C1 C6 C5 -4.82(13) . . . . ?
P1 C1 C6 C5 -174.57(7) . . . . ?
C2 C1 C6 C19 169.12(9) . . . . ?
P1 C1 C6 C19 -0.62(14) . . . . ?
C3 C2 C7 C12 86.03(12) . . . . ?
C1 C2 C7 C12 -98.53(12) . . . . ?
C3 C2 C7 C8 -88.52(12) . . . . ?
C1 C2 C7 C8 86.93(12) . . . . ?
C12 C7 C8 C9 -0.48(15) . . . . ?
C2 C7 C8 C9 174.06(9) . . . . ?
C12 C7 C8 C13 -179.68(10) . . . . ?
C2 C7 C8 C13 -5.14(15) . . . . ?
C7 C8 C9 C10 -0.03(17) . . . . ?
C13 C8 C9 C10 179.20(11) . . . . ?
C8 C9 C10 C11 0.49(18) . . . . ?
C9 C10 C11 C12 -0.44(18) . . . . ?
C10 C11 C12 C7 -0.07(17) . . . . ?
C10 C11 C12 C16 -177.90(11) . . . . ?
C8 C7 C12 C11 0.53(15) . . . . ?
C2 C7 C12 C11 -173.92(10) . . . . ?
C8 C7 C12 C16 178.35(10) . . . . ?
C2 C7 C12 C16 3.89(15) . . . . ?
C9 C8 C13 C14 61.90(14) . . . . ?
C7 C8 C13 C14 -118.91(12) . . . . ?
C9 C8 C13 C15 -62.84(14) . . . . ?
C7 C8 C13 C15 116.35(12) . . . . ?
C11 C12 C16 C17 78.52(14) . . . . ?
C7 C12 C16 C17 -99.27(12) . . . . ?
C11 C12 C16 C18 -46.05(15) . . . . ?
C7 C12 C16 C18 136.16(11) . . . . ?
C5 C6 C19 C24 -72.69(12) . . . . ?
C1 C6 C19 C24 113.13(11) . . . . ?
C5 C6 C19 C20 99.62(11) . . . . ?
C1 C6 C19 C20 -74.56(13) . . . . ?
C24 C19 C20 C21 -2.65(15) . . . . ?
C6 C19 C20 C21 -174.98(10) . . . . ?
C24 C19 C20 C25 171.37(10) . . . . ?
C6 C19 C20 C25 -0.95(15) . . . . ?
C19 C20 C21 C22 1.14(18) . . . . ?
C25 C20 C21 C22 -172.93(12) . . . . ?
C20 C21 C22 C23 0.5(2) . . . . ?
C21 C22 C23 C24 -0.7(2) . . . . ?
C22 C23 C24 C19 -0.78(19) . . . . ?
C22 C23 C24 C28 177.19(12) . . . . ?
C20 C19 C24 C23 2.48(16) . . . . ?
C6 C19 C24 C23 174.71(10) . . . . ?
C20 C19 C24 C28 -175.43(10) . . . . ?
C6 C19 C24 C28 -3.20(15) . . . . ?
C21 C20 C25 C26 -36.09(16) . . . . ?
C19 C20 C25 C26 149.98(11) . . . . ?
C21 C20 C25 C27 87.05(14) . . . . ?
C19 C20 C25 C27 -86.88(13) . . . . ?
C23 C24 C28 C30 43.31(15) . . . . ?
C19 C24 C28 C30 -138.79(11) . . . . ?
C23 C24 C28 C29 -78.83(13) . . . . ?
C19 C24 C28 C29 99.07(12) . . . . ?
C33 N2 C31 N1 0.24(12) . . . . ?
C35 N2 C31 N1 -178.39(10) . . . . ?
C33 N2 C31 P1 166.70(8) . . . . ?
C35 N2 C31 P1 -11.93(15) . . . . ?
C32 N1 C31 N2 0.05(12) . . . . ?
C34 N1 C31 N2 174.02(11) . . . . ?
C32 N1 C31 P1 -165.91(8) . . . . ?
C34 N1 C31 P1 8.07(16) . . . . ?
C1 P1 C31 N2 128.71(9) . . . . ?
C1 P1 C31 N1 -68.03(10) . . . . ?
C31 N1 C32 C33 -0.32(13) . . . . ?
C34 N1 C32 C33 -174.25(11) . . . . ?
C31 N1 C32 C36 176.64(11) . . . . ?
C34 N1 C32 C36 2.71(19) . . . . ?
N1 C32 C33 N2 0.44(12) . . . . ?
C36 C32 C33 N2 -176.21(12) . . . . ?
N1 C32 C33 C37 -178.80(11) . . . . ?
C36 C32 C33 C37 4.5(2) . . . . ?
C31 N2 C33 C32 -0.44(12) . . . . ?
C35 N2 C33 C32 178.21(10) . . . . ?
C31 N2 C33 C37 178.89(10) . . . . ?
C35 N2 C33 C37 -2.46(16) . . . . ?

_refine_diff_density_max         0.335
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.039


####################################################################### 
# 
# 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_ax1782_DipTerPPMe3_cmp4
_database_code_depnum_ccdc_archive 'CCDC 2046869'
loop_
_audit_author_name
_audit_author_address
'Hering-Junghans C.'
;LIKAT Rostock
Germany
;
_audit_update_record             
;
2020-11-27 deposited with the CCDC.	2021-01-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H46 P2'
_chemical_formula_sum            'C33 H46 P2'
_chemical_formula_weight         504.64

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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

#==============================================================================

# CRYSTAL DATA

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

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

_cell_length_a                   9.921(2)
_cell_length_b                   18.279(4)
_cell_length_c                   17.314(4)
_cell_angle_alpha                90
_cell_angle_beta                 101.82(3)
_cell_angle_gamma                90
_cell_volume                     3073.4(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2368
_cell_measurement_theta_min      12.78
_cell_measurement_theta_max      69.55

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_F_000             1096
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.116
_exptl_absorpt_coefficient_mu    1.400
_shelx_estimated_absorpt_T_min   0.735
_shelx_estimated_absorpt_T_max   0.854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.735
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?

#==============================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         microfocus
_diffrn_radiation_monochromator  multilayer
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            58227
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_av_R_equivalents  0.1055
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.556
_diffrn_reflns_theta_max         70.080
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5799
_reflns_number_gt                4923
_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       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms 
 were positioned geometrically and refined using a riding model, with C---H = 
 0.98 (methyl groups), 0.99Å (methylene groups), 1.00Å (methine groups) or 
 0.95 Å (aryl CH) and with Uiso(H) = 1.5 times Ueq(C) 
 (methyl groups) or with Uiso(H) = 1.2 times Ueq(C) 
 (methylene  groups, aryl CH, methine groups). Torsion angles of all methyl 
 groups were allowed to refine. 
 
 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 > 2σ(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     
'w=1/[σ²(Fo²)+(0.0837P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5799
_refine_ls_number_parameters     327
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.1157
_refine_ls_wR_factor_gt          0.1114
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.66314(3) 0.21924(2) 0.19824(2) 0.02447(12) Uani 1 1 d . . . . .
P2 P 0.49567(3) 0.18845(2) 0.24765(2) 0.02315(12) Uani 1 1 d . . . . .
C1 C 0.76519(13) 0.28830(7) 0.26314(8) 0.0211(3) Uani 1 1 d . . . . .
C2 C 0.72254(14) 0.35210(8) 0.29810(8) 0.0236(3) Uani 1 1 d . . . . .
C3 C 0.82202(15) 0.39987(9) 0.33958(9) 0.0296(3) Uani 1 1 d . . . . .
H3 H 0.7925 0.4420 0.3636 0.035 Uiso 1 1 calc R U . . .
C4 C 0.96221(15) 0.38782(9) 0.34679(10) 0.0325(3) Uani 1 1 d . . . . .
H4 H 1.0276 0.4202 0.3768 0.039 Uiso 1 1 calc R U . . .
C5 C 1.00476(14) 0.32763(9) 0.30930(9) 0.0280(3) Uani 1 1 d . . . . .
H5 H 1.1002 0.3195 0.3122 0.034 Uiso 1 1 calc R U . . .
C6 C 0.90925(13) 0.27908(8) 0.26762(8) 0.0226(3) Uani 1 1 d . . . . .
C7 C 0.57625(14) 0.37852(7) 0.28940(8) 0.0237(3) Uani 1 1 d . . . . .
C8 C 0.51689(14) 0.38547(8) 0.35669(9) 0.0262(3) Uani 1 1 d . . . . .
C9 C 0.38859(15) 0.41986(9) 0.34853(9) 0.0296(3) Uani 1 1 d . . . . .
H9 H 0.3488 0.4255 0.3936 0.036 Uiso 1 1 calc R U . . .
C10 C 0.31871(15) 0.44569(9) 0.27652(10) 0.0316(3) Uani 1 1 d . . . . .
H10 H 0.2315 0.4686 0.2722 0.038 Uiso 1 1 calc R U . . .
C11 C 0.37650(15) 0.43804(8) 0.21049(9) 0.0285(3) Uani 1 1 d . . . . .
H11 H 0.3276 0.4554 0.1609 0.034 Uiso 1 1 calc R U . . .
C12 C 0.50477(14) 0.40536(8) 0.21551(9) 0.0250(3) Uani 1 1 d . . . . .
C13 C 0.58370(16) 0.35553(9) 0.43780(9) 0.0322(3) Uani 1 1 d . . . . .
H13 H 0.6603 0.3222 0.4310 0.039 Uiso 1 1 calc R U . . .
C14 C 0.48072(19) 0.31067(11) 0.47393(10) 0.0418(4) Uani 1 1 d . . . . .
H14A H 0.4108 0.3434 0.4874 0.063 Uiso 1 1 calc R U . . .
H14B H 0.5297 0.2859 0.5217 0.063 Uiso 1 1 calc R U . . .
H14C H 0.4361 0.2742 0.4357 0.063 Uiso 1 1 calc R U . . .
C15 C 0.6448(2) 0.41569(12) 0.49623(11) 0.0465(4) Uani 1 1 d . . . . .
H15A H 0.7137 0.4433 0.4750 0.070 Uiso 1 1 calc R U . . .
H15B H 0.6884 0.3935 0.5467 0.070 Uiso 1 1 calc R U . . .
H15C H 0.5713 0.4488 0.5044 0.070 Uiso 1 1 calc R U . . .
C16 C 0.56890(15) 0.40292(8) 0.14272(9) 0.0281(3) Uani 1 1 d . . . . .
H16 H 0.6337 0.3604 0.1493 0.034 Uiso 1 1 calc R U . . .
C17 C 0.6537(2) 0.47149(11) 0.13740(12) 0.0482(4) Uani 1 1 d . . . . .
H17A H 0.7029 0.4662 0.0941 0.072 Uiso 1 1 calc R U . . .
H17B H 0.7203 0.4783 0.1871 0.072 Uiso 1 1 calc R U . . .
H17C H 0.5925 0.5140 0.1276 0.072 Uiso 1 1 calc R U . . .
C18 C 0.46386(19) 0.39095(13) 0.06598(10) 0.0474(5) Uani 1 1 d . . . . .
H18A H 0.4060 0.4346 0.0540 0.071 Uiso 1 1 calc R U . . .
H18B H 0.4060 0.3487 0.0718 0.071 Uiso 1 1 calc R U . . .
H18C H 0.5122 0.3819 0.0229 0.071 Uiso 1 1 calc R U . . .
C19 C 0.95950(13) 0.21873(8) 0.22131(8) 0.0238(3) Uani 1 1 d . . . . .
C20 C 0.99886(13) 0.15079(8) 0.25654(8) 0.0251(3) Uani 1 1 d . . . . .
C21 C 1.04163(15) 0.09581(9) 0.21070(9) 0.0306(3) Uani 1 1 d . . . . .
H21 H 1.0684 0.0495 0.2336 0.037 Uiso 1 1 calc R U . . .
C22 C 1.04533(16) 0.10820(9) 0.13235(10) 0.0351(4) Uani 1 1 d . . . . .
H22 H 1.0737 0.0702 0.1018 0.042 Uiso 1 1 calc R U . . .
C23 C 1.00800(15) 0.17562(10) 0.09825(9) 0.0330(3) Uani 1 1 d . . . . .
H23 H 1.0118 0.1837 0.0445 0.040 Uiso 1 1 calc R U . . .
C24 C 0.96471(13) 0.23192(8) 0.14210(9) 0.0263(3) Uani 1 1 d . . . . .
C25 C 0.99902(14) 0.13753(8) 0.34303(9) 0.0279(3) Uani 1 1 d . . . . .
H25 H 0.9411 0.1764 0.3607 0.033 Uiso 1 1 calc R U . . .
C26 C 0.9381(2) 0.06343(10) 0.35841(11) 0.0427(4) Uani 1 1 d . . . . .
H26A H 0.9962 0.0242 0.3446 0.064 Uiso 1 1 calc R U . . .
H26B H 0.8450 0.0590 0.3262 0.064 Uiso 1 1 calc R U . . .
H26C H 0.9342 0.0596 0.4144 0.064 Uiso 1 1 calc R U . . .
C27 C 1.14559(17) 0.14530(12) 0.39229(10) 0.0427(4) Uani 1 1 d . . . . .
H27A H 1.1452 0.1348 0.4478 0.064 Uiso 1 1 calc R U . . .
H27B H 1.1785 0.1953 0.3875 0.064 Uiso 1 1 calc R U . . .
H27C H 1.2067 0.1107 0.3731 0.064 Uiso 1 1 calc R U . . .
C28 C 0.92688(15) 0.30633(9) 0.10429(9) 0.0295(3) Uani 1 1 d . . . . .
H28 H 0.8752 0.3336 0.1391 0.035 Uiso 1 1 calc R U . . .
C29 C 1.05760(17) 0.35001(10) 0.10189(11) 0.0418(4) Uani 1 1 d . . . . .
H29A H 1.1099 0.3575 0.1558 0.063 Uiso 1 1 calc R U . . .
H29B H 1.0324 0.3976 0.0769 0.063 Uiso 1 1 calc R U . . .
H29C H 1.1142 0.3229 0.0714 0.063 Uiso 1 1 calc R U . . .
C30 C 0.83324(18) 0.30139(11) 0.02253(10) 0.0414(4) Uani 1 1 d . . . . .
H30A H 0.8832 0.2780 -0.0141 0.062 Uiso 1 1 calc R U . . .
H30B H 0.8050 0.3507 0.0036 0.062 Uiso 1 1 calc R U . . .
H30C H 0.7515 0.2723 0.0257 0.062 Uiso 1 1 calc R U . . .
C31 C 0.54331(17) 0.16106(10) 0.35007(9) 0.0373(4) Uani 1 1 d . . . . .
H31A H 0.4601 0.1495 0.3699 0.056 Uiso 1 1 calc R U . . .
H31B H 0.5931 0.2011 0.3812 0.056 Uiso 1 1 calc R U . . .
H31C H 0.6026 0.1177 0.3546 0.056 Uiso 1 1 calc R U . . .
C32 C 0.33910(14) 0.24189(9) 0.23956(10) 0.0331(3) Uani 1 1 d . . . . .
H32A H 0.2674 0.2117 0.2551 0.050 Uiso 1 1 calc R U . . .
H32B H 0.3080 0.2582 0.1849 0.050 Uiso 1 1 calc R U . . .
H32C H 0.3574 0.2846 0.2743 0.050 Uiso 1 1 calc R U . . .
C33 C 0.43487(15) 0.10666(9) 0.19238(10) 0.0316(3) Uani 1 1 d . . . . .
H33A H 0.5094 0.0706 0.1988 0.047 Uiso 1 1 calc R U . . .
H33B H 0.4052 0.1190 0.1364 0.047 Uiso 1 1 calc R U . . .
H33C H 0.3570 0.0862 0.2120 0.047 Uiso 1 1 calc R U . . .


#==============================================================================

# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C1 1.8481(14) . ?
P1 P2 2.0955(7) . ?
P2 C31 1.8098(17) . ?
P2 C33 1.8105(16) . ?
P2 C32 1.8161(15) . ?
C1 C2 1.418(2) . ?
C1 C6 1.4254(18) . ?
C2 C3 1.401(2) . ?
C2 C7 1.5076(18) . ?
C3 C4 1.388(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.388(2) . ?
C5 H5 0.9500 . ?
C6 C19 1.5073(19) . ?
C7 C8 1.415(2) . ?
C7 C12 1.417(2) . ?
C8 C9 1.401(2) . ?
C8 C13 1.526(2) . ?
C9 C10 1.380(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.387(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.392(2) . ?
C11 H11 0.9500 . ?
C12 C16 1.524(2) . ?
C13 C15 1.533(2) . ?
C13 C14 1.539(2) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.523(2) . ?
C16 C18 1.527(2) . ?
C16 H16 1.0000 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.403(2) . ?
C19 C24 1.404(2) . ?
C20 C21 1.399(2) . ?
C20 C25 1.517(2) . ?
C21 C22 1.383(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.384(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.398(2) . ?
C23 H23 0.9500 . ?
C24 C28 1.523(2) . ?
C25 C26 1.528(2) . ?
C25 C27 1.534(2) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C30 1.529(2) . ?
C28 C29 1.531(2) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
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 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 P2 108.47(5) . . ?
C31 P2 C33 106.34(8) . . ?
C31 P2 C32 105.78(8) . . ?
C33 P2 C32 102.49(8) . . ?
C31 P2 P1 113.86(6) . . ?
C33 P2 P1 102.25(5) . . ?
C32 P2 P1 124.14(6) . . ?
C2 C1 C6 117.24(12) . . ?
C2 C1 P1 130.33(10) . . ?
C6 C1 P1 111.76(10) . . ?
C3 C2 C1 119.41(13) . . ?
C3 C2 C7 114.48(13) . . ?
C1 C2 C7 125.89(12) . . ?
C4 C3 C2 122.35(14) . . ?
C4 C3 H3 118.8 . . ?
C2 C3 H3 118.8 . . ?
C5 C4 C3 118.64(14) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
C4 C5 C6 120.66(13) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C1 121.52(13) . . ?
C5 C6 C19 118.66(12) . . ?
C1 C6 C19 119.66(12) . . ?
C8 C7 C12 119.77(13) . . ?
C8 C7 C2 120.08(13) . . ?
C12 C7 C2 119.64(12) . . ?
C9 C8 C7 118.70(13) . . ?
C9 C8 C13 117.92(13) . . ?
C7 C8 C13 123.36(13) . . ?
C10 C9 C8 121.52(14) . . ?
C10 C9 H9 119.2 . . ?
C8 C9 H9 119.2 . . ?
C9 C10 C11 119.62(14) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C10 C11 C12 121.23(14) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
C11 C12 C7 119.14(14) . . ?
C11 C12 C16 119.46(13) . . ?
C7 C12 C16 121.32(12) . . ?
C8 C13 C15 112.86(14) . . ?
C8 C13 C14 111.45(13) . . ?
C15 C13 C14 108.63(14) . . ?
C8 C13 H13 107.9 . . ?
C15 C13 H13 107.9 . . ?
C14 C13 H13 107.9 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C12 110.81(13) . . ?
C17 C16 C18 110.63(15) . . ?
C12 C16 C18 113.42(13) . . ?
C17 C16 H16 107.2 . . ?
C12 C16 H16 107.2 . . ?
C18 C16 H16 107.2 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C24 120.93(13) . . ?
C20 C19 C6 120.62(13) . . ?
C24 C19 C6 118.45(13) . . ?
C21 C20 C19 118.61(14) . . ?
C21 C20 C25 120.41(14) . . ?
C19 C20 C25 120.96(13) . . ?
C22 C21 C20 120.72(15) . . ?
C22 C21 H21 119.6 . . ?
C20 C21 H21 119.6 . . ?
C21 C22 C23 120.37(15) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
C22 C23 C24 120.61(15) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
C23 C24 C19 118.76(14) . . ?
C23 C24 C28 120.02(14) . . ?
C19 C24 C28 121.21(13) . . ?
C20 C25 C26 113.15(13) . . ?
C20 C25 C27 110.08(12) . . ?
C26 C25 C27 110.40(15) . . ?
C20 C25 H25 107.7 . . ?
C26 C25 H25 107.7 . . ?
C27 C25 H25 107.7 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 C28 C30 113.26(14) . . ?
C24 C28 C29 110.00(13) . . ?
C30 C28 C29 111.31(14) . . ?
C24 C28 H28 107.3 . . ?
C30 C28 H28 107.3 . . ?
C29 C28 H28 107.3 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
P2 C31 H31A 109.5 . . ?
P2 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
P2 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
P2 C32 H32A 109.5 . . ?
P2 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
P2 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
P2 C33 H33A 109.5 . . ?
P2 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
P2 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

_refine_diff_density_max         0.465
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.054

####################################################################### 
# 
# 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_ax1935_MesStarP_MeIMes_cmp8
_database_code_depnum_ccdc_archive 'CCDC 2046860'
loop_
_audit_author_name
_audit_author_address
'Hering-Junghans C.'
;LIKAT Rostock
Germany
;
_audit_update_record             
;
2020-11-27 deposited with the CCDC.	2021-01-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2 (C41 H57 N2 P), C6 H14'
_chemical_formula_sum            'C88 H128 N4 P2'
_chemical_formula_weight         1303.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#==============================================================================

# CRYSTAL DATA

_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                   9.8045(4)
_cell_length_b                   17.1656(8)
_cell_length_c                   24.3050(11)
_cell_angle_alpha                86.6392(22)
_cell_angle_beta                 87.4849(22)
_cell_angle_gamma                84.6245(21)
_cell_volume                     4062.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9823
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      66.68

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.066
_exptl_crystal_F_000             1428
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.810
_shelx_estimated_absorpt_T_min   0.829
_shelx_estimated_absorpt_T_max   0.976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?

#==============================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         microfocus
_diffrn_radiation_monochromator  multilayer
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            71311
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.822
_diffrn_reflns_theta_max         66.761
_diffrn_reflns_theta_full        66.761
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             14362
_reflns_number_gt                11989
_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       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms 
 were positioned geometrically and refined using a riding model, with C---H = 
 0.98 (methyl groups), 0.99Å (methylene groups), 1.00Å (methine groups) or 
 0.95 Å (aryl CH) and with Uiso(H) = 1.5 times Ueq(C) 
 (methyl groups) or with Uiso(H) = 1.2 times Ueq(C) 
 (methylene  groups, aryl CH, methine groups). Torsion angles of all methyl 
 groups were allowed to refine. One of the tBu groups (C52-C55) was found to be
 disordered and was split in two parts and the occupancy of each part was 
 allowed to refine freely. One solvent molecule of n-hexane was found to be
 disordered and was split in two parts and the occupancy of each part
 was allowed to refine freely.
 
 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 > 2σ(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     
'w=1/[σ²(Fo²)+(0.0821P)²+1.0853P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14362
_refine_ls_number_parameters     924
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.1454
_refine_ls_wR_factor_gt          0.1363
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.59092(5) 0.64722(3) 0.72256(2) 0.04221(12) Uani 1 1 d . . . . .
N1 N 0.58727(16) 0.76233(9) 0.80676(6) 0.0441(3) Uani 1 1 d . . . . .
N2 N 0.52989(15) 0.80580(9) 0.72387(6) 0.0417(3) Uani 1 1 d . . . . .
C1 C 0.70003(17) 0.57773(10) 0.76787(7) 0.0386(4) Uani 1 1 d . . . . .
C2 C 0.64357(17) 0.51806(11) 0.80250(7) 0.0385(4) Uani 1 1 d . . . . .
C3 C 0.72299(17) 0.47973(11) 0.84387(7) 0.0397(4) Uani 1 1 d . . . . .
H3 H 0.6822 0.4433 0.8689 0.048 Uiso 1 1 calc R U . . .
C4 C 0.85922(17) 0.49250(11) 0.85011(7) 0.0394(4) Uani 1 1 d . . . . .
C5 C 0.91951(17) 0.53865(11) 0.80864(7) 0.0410(4) Uani 1 1 d . . . . .
H5 H 1.0154 0.5427 0.8091 0.049 Uiso 1 1 calc R U . . .
C6 C 0.84599(17) 0.57929(11) 0.76643(7) 0.0396(4) Uani 1 1 d . . . . .
C7 C 0.50230(18) 0.48687(12) 0.79310(8) 0.0434(4) Uani 1 1 d . . . . .
C8 C 0.4946(2) 0.46870(13) 0.73225(8) 0.0535(5) Uani 1 1 d . . . . .
H8A H 0.4094 0.4449 0.7269 0.080 Uiso 1 1 calc R U . . .
H8B H 0.5732 0.4322 0.7219 0.080 Uiso 1 1 calc R U . . .
H8C H 0.4963 0.5174 0.7091 0.080 Uiso 1 1 calc R U . . .
C9 C 0.3804(2) 0.54270(14) 0.81036(10) 0.0583(5) Uani 1 1 d . . . . .
H9A H 0.2952 0.5191 0.8047 0.087 Uiso 1 1 calc R U . . .
H9B H 0.3816 0.5921 0.7881 0.087 Uiso 1 1 calc R U . . .
H9C H 0.3857 0.5529 0.8494 0.087 Uiso 1 1 calc R U . . .
C10 C 0.4861(2) 0.40856(13) 0.82614(9) 0.0534(5) Uani 1 1 d . . . . .
H10A H 0.4826 0.4172 0.8657 0.080 Uiso 1 1 calc R U . . .
H10B H 0.5643 0.3709 0.8174 0.080 Uiso 1 1 calc R U . . .
H10C H 0.4011 0.3878 0.8164 0.080 Uiso 1 1 calc R U . . .
C11 C 0.94589(18) 0.45180(12) 0.89652(7) 0.0446(4) Uani 1 1 d . . . . .
C12 C 1.0319(2) 0.51053(13) 0.92110(8) 0.0521(5) Uani 1 1 d . . . . .
H12A H 1.0937 0.5315 0.8923 0.078 Uiso 1 1 calc R U . . .
H12B H 1.0860 0.4840 0.9508 0.078 Uiso 1 1 calc R U . . .
H12C H 0.9710 0.5536 0.9358 0.078 Uiso 1 1 calc R U . . .
C13 C 1.0444(2) 0.38626(14) 0.87290(9) 0.0592(5) Uani 1 1 d . . . . .
H13A H 0.9915 0.3470 0.8582 0.089 Uiso 1 1 calc R U . . .
H13B H 1.1020 0.3615 0.9022 0.089 Uiso 1 1 calc R U . . .
H13C H 1.1026 0.4084 0.8433 0.089 Uiso 1 1 calc R U . . .
C14 C 0.8561(2) 0.41683(14) 0.94312(8) 0.0568(5) Uani 1 1 d . . . . .
H14A H 0.7900 0.4580 0.9572 0.085 Uiso 1 1 calc R U . . .
H14B H 0.9141 0.3945 0.9730 0.085 Uiso 1 1 calc R U . . .
H14C H 0.8069 0.3756 0.9290 0.085 Uiso 1 1 calc R U . . .
C15 C 0.93038(18) 0.61421(11) 0.71655(8) 0.0438(4) Uani 1 1 d . . . . .
C16 C 0.9153(2) 0.70379(12) 0.71050(9) 0.0551(5) Uani 1 1 d . . . . .
H16A H 0.9672 0.7212 0.6774 0.083 Uiso 1 1 calc R U . . .
H16B H 0.9508 0.7251 0.7430 0.083 Uiso 1 1 calc R U . . .
H16C H 0.8183 0.7224 0.7072 0.083 Uiso 1 1 calc R U . . .
C17 C 0.8881(2) 0.58020(12) 0.66339(8) 0.0495(4) Uani 1 1 d . . . . .
H17A H 0.7903 0.5947 0.6581 0.074 Uiso 1 1 calc R U . . .
H17B H 0.9054 0.5230 0.6663 0.074 Uiso 1 1 calc R U . . .
H17C H 0.9416 0.6012 0.6319 0.074 Uiso 1 1 calc R U . . .
C18 C 1.0848(2) 0.58901(14) 0.72031(9) 0.0561(5) Uani 1 1 d . . . . .
H18A H 1.1329 0.6060 0.6861 0.084 Uiso 1 1 calc R U . . .
H18B H 1.0990 0.5318 0.7257 0.084 Uiso 1 1 calc R U . . .
H18C H 1.1208 0.6132 0.7515 0.084 Uiso 1 1 calc R U . . .
C19 C 0.57394(17) 0.73754(11) 0.75432(7) 0.0406(4) Uani 1 1 d . . . . .
C20 C 0.5480(2) 0.84371(12) 0.80810(8) 0.0485(4) Uani 1 1 d . . . . .
C21 C 0.51225(19) 0.86997(11) 0.75750(8) 0.0462(4) Uani 1 1 d . . . . .
C22 C 0.5493(3) 0.88529(14) 0.86039(9) 0.0605(5) Uani 1 1 d . . . . .
H22A H 0.5239 0.9414 0.8529 0.091 Uiso 1 1 calc R U . . .
H22B H 0.6414 0.8777 0.8751 0.091 Uiso 1 1 calc R U . . .
H22C H 0.4834 0.8641 0.8874 0.091 Uiso 1 1 calc R U . . .
C23 C 0.4583(2) 0.94963(12) 0.73576(9) 0.0541(5) Uani 1 1 d . . . . .
H23A H 0.4457 0.9851 0.7661 0.081 Uiso 1 1 calc R U . . .
H23B H 0.3702 0.9464 0.7189 0.081 Uiso 1 1 calc R U . . .
H23C H 0.5237 0.9696 0.7080 0.081 Uiso 1 1 calc R U . . .
C24 C 0.58737(19) 0.71419(11) 0.85762(7) 0.0439(4) Uani 1 1 d . . . . .
C25 C 0.70882(19) 0.69651(11) 0.88542(8) 0.0447(4) Uani 1 1 d . . . . .
C26 C 0.7014(2) 0.65688(12) 0.93702(8) 0.0501(4) Uani 1 1 d . . . . .
H26 H 0.7835 0.6438 0.9562 0.060 Uiso 1 1 calc R U . . .
C27 C 0.5788(2) 0.63583(13) 0.96130(8) 0.0536(5) Uani 1 1 d . . . . .
C28 C 0.4598(2) 0.65584(13) 0.93281(8) 0.0532(5) Uani 1 1 d . . . . .
H28 H 0.3749 0.6418 0.9489 0.064 Uiso 1 1 calc R U . . .
C29 C 0.4612(2) 0.69595(12) 0.88133(8) 0.0483(4) Uani 1 1 d . . . . .
C30 C 0.8433(2) 0.72274(13) 0.86294(8) 0.0508(5) Uani 1 1 d . . . . .
H30A H 0.8396 0.7323 0.8229 0.076 Uiso 1 1 calc R U . . .
H30B H 0.9171 0.6819 0.8715 0.076 Uiso 1 1 calc R U . . .
H30C H 0.8609 0.7711 0.8798 0.076 Uiso 1 1 calc R U . . .
C31 C 0.5741(3) 0.59637(18) 1.01839(10) 0.0726(7) Uani 1 1 d . . . . .
H31A H 0.6168 0.5425 1.0171 0.109 Uiso 1 1 calc R U . . .
H31B H 0.4785 0.5956 1.0318 0.109 Uiso 1 1 calc R U . . .
H31C H 0.6239 0.6254 1.0433 0.109 Uiso 1 1 calc R U . . .
C32 C 0.3284(2) 0.72388(14) 0.85456(9) 0.0571(5) Uani 1 1 d . . . . .
H32A H 0.3033 0.7789 0.8622 0.086 Uiso 1 1 calc R U . . .
H32B H 0.2560 0.6920 0.8694 0.086 Uiso 1 1 calc R U . . .
H32C H 0.3396 0.7189 0.8146 0.086 Uiso 1 1 calc R U . . .
C33 C 0.51004(18) 0.81245(10) 0.66545(7) 0.0407(4) Uani 1 1 d . . . . .
C34 C 0.39220(19) 0.78655(11) 0.64509(8) 0.0464(4) Uani 1 1 d . . . . .
C35 C 0.3754(2) 0.79375(12) 0.58876(9) 0.0524(5) Uani 1 1 d . . . . .
H35 H 0.2970 0.7747 0.5745 0.063 Uiso 1 1 calc R U . . .
C36 C 0.4684(2) 0.82762(13) 0.55230(9) 0.0545(5) Uani 1 1 d . . . . .
C37 C 0.5814(2) 0.85513(12) 0.57401(8) 0.0513(5) Uani 1 1 d . . . . .
H37 H 0.6451 0.8797 0.5498 0.062 Uiso 1 1 calc R U . . .
C38 C 0.60509(18) 0.84817(11) 0.62992(8) 0.0436(4) Uani 1 1 d . . . . .
C39 C 0.2848(2) 0.75293(15) 0.68290(10) 0.0624(6) Uani 1 1 d . . . . .
H39A H 0.3177 0.6997 0.6960 0.094 Uiso 1 1 calc R U . . .
H39B H 0.2005 0.7514 0.6629 0.094 Uiso 1 1 calc R U . . .
H39C H 0.2660 0.7858 0.7145 0.094 Uiso 1 1 calc R U . . .
C40 C 0.4483(3) 0.83327(18) 0.49087(10) 0.0773(7) Uani 1 1 d . . . . .
H40A H 0.4491 0.8880 0.4770 0.116 Uiso 1 1 calc R U . . .
H40B H 0.3601 0.8142 0.4834 0.116 Uiso 1 1 calc R U . . .
H40C H 0.5226 0.8013 0.4724 0.116 Uiso 1 1 calc R U . . .
C41 C 0.7318(2) 0.87862(12) 0.65054(9) 0.0514(5) Uani 1 1 d . . . . .
H41A H 0.8135 0.8485 0.6355 0.077 Uiso 1 1 calc R U . . .
H41B H 0.7303 0.8731 0.6909 0.077 Uiso 1 1 calc R U . . .
H41C H 0.7340 0.9340 0.6386 0.077 Uiso 1 1 calc R U . . .
P2 P 0.80875(5) 0.78660(3) 0.37504(2) 0.04414(13) Uani 1 1 d . . . . .
N3 N 1.10548(15) 0.74078(9) 0.37014(6) 0.0419(3) Uani 1 1 d . . . . .
N4 N 0.97678(16) 0.68031(9) 0.43170(7) 0.0461(4) Uani 1 1 d . . . . .
C42 C 0.84441(17) 0.86758(11) 0.32347(8) 0.0406(4) Uani 1 1 d . . . . .
C43 C 0.88441(17) 0.94031(11) 0.33997(8) 0.0413(4) Uani 1 1 d . . . . .
C44 C 0.93181(18) 0.99333(11) 0.29906(8) 0.0435(4) Uani 1 1 d . . . . .
H44 H 0.9644 1.0402 0.3101 0.052 Uiso 1 1 calc R U . . .
C45 C 0.93324(18) 0.98056(11) 0.24336(8) 0.0439(4) Uani 1 1 d . . . . .
C46 C 0.87185(18) 0.91588(12) 0.22819(8) 0.0452(4) Uani 1 1 d . . . . .
H46 H 0.8630 0.9090 0.1901 0.054 Uiso 1 1 calc R U . . .
C47 C 0.82255(18) 0.86058(11) 0.26644(8) 0.0423(4) Uani 1 1 d . . . . .
C48 C 0.8621(2) 0.96941(11) 0.39942(8) 0.0457(4) Uani 1 1 d . . . . .
C49 C 0.9452(3) 0.92198(14) 0.44412(9) 0.0645(6) Uani 1 1 d . . . . .
H49A H 0.9169 0.9415 0.4803 0.097 Uiso 1 1 calc R U . . .
H49B H 1.0430 0.9275 0.4369 0.097 Uiso 1 1 calc R U . . .
H49C H 0.9286 0.8666 0.4437 0.097 Uiso 1 1 calc R U . . .
C50 C 0.7080(2) 0.97017(13) 0.41494(9) 0.0572(5) Uani 1 1 d . . . . .
H50A H 0.6801 0.9169 0.4146 0.086 Uiso 1 1 calc R U . . .
H50B H 0.6555 1.0044 0.3882 0.086 Uiso 1 1 calc R U . . .
H50C H 0.6903 0.9898 0.4519 0.086 Uiso 1 1 calc R U . . .
C51 C 0.8976(2) 1.05411(13) 0.40294(9) 0.0560(5) Uani 1 1 d . . . . .
H51A H 0.8731 1.0717 0.4400 0.084 Uiso 1 1 calc R U . . .
H51B H 0.8462 1.0881 0.3757 0.084 Uiso 1 1 calc R U . . .
H51C H 0.9961 1.0566 0.3953 0.084 Uiso 1 1 calc R U . . .
C52A C 0.9896(10) 1.0368(6) 0.2003(4) 0.0466(17) Uani 0.798(4) 1 d . . P A 1
C53A C 0.8753(5) 1.0988(3) 0.1826(2) 0.121(3) Uani 0.798(4) 1 d . . P A 1
H53A H 0.9119 1.1355 0.1546 0.181 Uiso 0.798(4) 1 calc R U P A 1
H53B H 0.8013 1.0733 0.1672 0.181 Uiso 0.798(4) 1 calc R U P A 1
H53C H 0.8394 1.1275 0.2147 0.181 Uiso 0.798(4) 1 calc R U P A 1
C54A C 1.1073(5) 1.0790(3) 0.22247(16) 0.0843(12) Uani 0.798(4) 1 d . . P A 1
H54A H 1.1414 1.1150 0.1934 0.126 Uiso 0.798(4) 1 calc R U P A 1
H54B H 1.0729 1.1085 0.2543 0.126 Uiso 0.798(4) 1 calc R U P A 1
H54C H 1.1819 1.0400 0.2336 0.126 Uiso 0.798(4) 1 calc R U P A 1
C55A C 1.0524(4) 0.9982(2) 0.14948(14) 0.0756(10) Uani 0.798(4) 1 d . . P A 1
H55A H 1.0868 1.0382 0.1234 0.113 Uiso 0.798(4) 1 calc R U P A 1
H55B H 1.1284 0.9598 0.1601 0.113 Uiso 0.798(4) 1 calc R U P A 1
H55C H 0.9827 0.9717 0.1321 0.113 Uiso 0.798(4) 1 calc R U P A 1
C52B C 0.971(4) 1.056(2) 0.1987(15) 0.053(10) Uani 0.202(4) 1 d . . P A 2
C53B C 0.915(2) 1.1266(13) 0.2204(10) 0.121(3) Uani 0.202(4) 1 d . . P A 2
H53D H 0.9471 1.1298 0.2578 0.181 Uiso 0.202(4) 1 calc R U P A 2
H53E H 0.9446 1.1708 0.1970 0.181 Uiso 0.202(4) 1 calc R U P A 2
H53F H 0.8149 1.1284 0.2216 0.181 Uiso 0.202(4) 1 calc R U P A 2
C54B C 0.9452(19) 1.0312(10) 0.1433(6) 0.0843(12) Uani 0.202(4) 1 d . . P A 2
H54D H 0.9951 0.9800 0.1376 0.126 Uiso 0.202(4) 1 calc R U P A 2
H54E H 0.8467 1.0275 0.1401 0.126 Uiso 0.202(4) 1 calc R U P A 2
H54F H 0.9765 1.0698 0.1154 0.126 Uiso 0.202(4) 1 calc R U P A 2
C55B C 1.1301(17) 1.0483(10) 0.2015(7) 0.0756(10) Uani 0.202(4) 1 d . . P A 2
H55D H 1.1679 0.9989 0.1863 0.113 Uiso 0.202(4) 1 calc R U P A 2
H55E H 1.1669 1.0923 0.1800 0.113 Uiso 0.202(4) 1 calc R U P A 2
H55F H 1.1557 1.0492 0.2400 0.113 Uiso 0.202(4) 1 calc R U P A 2
C56 C 0.7352(2) 0.79879(12) 0.24439(8) 0.0500(5) Uani 1 1 d . . . . .
C57 C 0.5943(2) 0.80344(14) 0.27526(10) 0.0603(5) Uani 1 1 d . . . . .
H57A H 0.5362 0.7676 0.2596 0.090 Uiso 1 1 calc R U . . .
H57B H 0.5507 0.8571 0.2714 0.090 Uiso 1 1 calc R U . . .
H57C H 0.6064 0.7885 0.3144 0.090 Uiso 1 1 calc R U . . .
C58 C 0.7061(3) 0.81606(17) 0.18277(10) 0.0715(7) Uani 1 1 d . . . . .
H58A H 0.7922 0.8093 0.1608 0.107 Uiso 1 1 calc R U . . .
H58B H 0.6650 0.8700 0.1771 0.107 Uiso 1 1 calc R U . . .
H58C H 0.6428 0.7798 0.1713 0.107 Uiso 1 1 calc R U . . .
C59 C 0.8048(2) 0.71523(13) 0.24944(10) 0.0564(5) Uani 1 1 d . . . . .
H59A H 0.8210 0.7004 0.2883 0.085 Uiso 1 1 calc R U . . .
H59B H 0.8924 0.7127 0.2283 0.085 Uiso 1 1 calc R U . . .
H59C H 0.7454 0.6791 0.2349 0.085 Uiso 1 1 calc R U . . .
C60 C 0.97016(18) 0.73757(10) 0.38919(7) 0.0408(4) Uani 1 1 d . . . . .
C61 C 1.1916(2) 0.68559(12) 0.40170(8) 0.0491(4) Uani 1 1 d . . . . .
C62 C 1.1129(2) 0.64939(12) 0.43906(8) 0.0505(5) Uani 1 1 d . . . . .
C63 C 1.3434(2) 0.67612(14) 0.38967(10) 0.0588(5) Uani 1 1 d . . . . .
H63A H 1.3872 0.6401 0.4178 0.088 Uiso 1 1 calc R U . . .
H63B H 1.3802 0.7272 0.3900 0.088 Uiso 1 1 calc R U . . .
H63C H 1.3619 0.6548 0.3533 0.088 Uiso 1 1 calc R U . . .
C64 C 1.1466(3) 0.58448(15) 0.48151(11) 0.0698(6) Uani 1 1 d . . . . .
H64A H 1.2461 0.5714 0.4813 0.105 Uiso 1 1 calc R U . . .
H64B H 1.1016 0.5382 0.4730 0.105 Uiso 1 1 calc R U . . .
H64C H 1.1142 0.6013 0.5180 0.105 Uiso 1 1 calc R U . . .
C65 C 1.15014(17) 0.76390(11) 0.31465(8) 0.0422(4) Uani 1 1 d . . . . .
C66 C 1.14820(18) 0.70931(12) 0.27435(8) 0.0462(4) Uani 1 1 d . . . . .
C67 C 1.19595(19) 0.72929(14) 0.22126(9) 0.0529(5) Uani 1 1 d . . . . .
H67 H 1.1928 0.6930 0.1934 0.063 Uiso 1 1 calc R U . . .
C68 C 1.2481(2) 0.80050(14) 0.20767(9) 0.0562(5) Uani 1 1 d . . . . .
C69 C 1.25467(19) 0.85142(13) 0.24939(9) 0.0533(5) Uani 1 1 d . . . . .
H69 H 1.2919 0.9000 0.2409 0.064 Uiso 1 1 calc R U . . .
C70 C 1.20890(18) 0.83422(11) 0.30330(8) 0.0460(4) Uani 1 1 d . . . . .
C71 C 1.1068(2) 0.62795(12) 0.28825(9) 0.0537(5) Uani 1 1 d . . . . .
H71A H 1.1818 0.5963 0.3066 0.081 Uiso 1 1 calc R U . . .
H71B H 1.0869 0.6038 0.2543 0.081 Uiso 1 1 calc R U . . .
H71C H 1.0248 0.6308 0.3129 0.081 Uiso 1 1 calc R U . . .
C72 C 1.3014(3) 0.81926(19) 0.14963(11) 0.0778(7) Uani 1 1 d . . . . .
H72A H 1.3660 0.7759 0.1377 0.117 Uiso 1 1 calc R U . . .
H72B H 1.3482 0.8674 0.1487 0.117 Uiso 1 1 calc R U . . .
H72C H 1.2246 0.8267 0.1248 0.117 Uiso 1 1 calc R U . . .
C73 C 1.2335(2) 0.88762(12) 0.34779(10) 0.0548(5) Uani 1 1 d . . . . .
H73A H 1.3310 0.8962 0.3472 0.082 Uiso 1 1 calc R U . . .
H73B H 1.2066 0.8636 0.3837 0.082 Uiso 1 1 calc R U . . .
H73C H 1.1789 0.9379 0.3415 0.082 Uiso 1 1 calc R U . . .
C74 C 0.8608(2) 0.66031(11) 0.46619(8) 0.0453(4) Uani 1 1 d . . . . .
C75 C 0.8391(2) 0.69187(11) 0.51744(8) 0.0472(4) Uani 1 1 d . . . . .
C76 C 0.7264(2) 0.67159(12) 0.55033(8) 0.0497(4) Uani 1 1 d . . . . .
H76 H 0.7108 0.6928 0.5855 0.060 Uiso 1 1 calc R U . . .
C77 C 0.6362(2) 0.62117(11) 0.53288(8) 0.0480(4) Uani 1 1 d . . . . .
C78 C 0.6610(2) 0.59080(11) 0.48147(8) 0.0478(4) Uani 1 1 d . . . . .
H78 H 0.5996 0.5566 0.4691 0.057 Uiso 1 1 calc R U . . .
C79 C 0.7726(2) 0.60861(11) 0.44736(8) 0.0465(4) Uani 1 1 d . . . . .
C80 C 0.9344(2) 0.74662(14) 0.53846(9) 0.0586(5) Uani 1 1 d . . . . .
H80A H 0.8855 0.7987 0.5418 0.088 Uiso 1 1 calc R U . . .
H80B H 1.0133 0.7503 0.5126 0.088 Uiso 1 1 calc R U . . .
H80C H 0.9662 0.7264 0.5747 0.088 Uiso 1 1 calc R U . . .
C81 C 0.5171(2) 0.59761(14) 0.56982(9) 0.0603(5) Uani 1 1 d . . . . .
H81A H 0.5106 0.6280 0.6029 0.090 Uiso 1 1 calc R U . . .
H81B H 0.5315 0.5416 0.5806 0.090 Uiso 1 1 calc R U . . .
H81C H 0.4319 0.6079 0.5499 0.090 Uiso 1 1 calc R U . . .
C82 C 0.7979(3) 0.57214(13) 0.39271(9) 0.0594(5) Uani 1 1 d . . . . .
H82A H 0.7404 0.5287 0.3910 0.089 Uiso 1 1 calc R U . . .
H82B H 0.8947 0.5524 0.3886 0.089 Uiso 1 1 calc R U . . .
H82C H 0.7752 0.6115 0.3629 0.089 Uiso 1 1 calc R U . . .
C90A C 0.5840(11) 0.8563(7) 0.0265(3) 0.198(4) Uani 0.798(4) 1 d D . P A 1
H90A H 0.5841 0.8178 -0.0017 0.298 Uiso 0.798(4) 1 calc R U P A 1
H90B H 0.5065 0.8962 0.0214 0.298 Uiso 0.798(4) 1 calc R U P A 1
H90C H 0.5754 0.8299 0.0632 0.298 Uiso 0.798(4) 1 calc R U P A 1
C91A C 0.7197(12) 0.8960(8) 0.0213(5) 0.191(4) Uani 0.798(4) 1 d D . P A 1
H91A H 0.7165 0.9352 -0.0103 0.229 Uiso 0.798(4) 1 calc R U P A 1
H91B H 0.7318 0.9235 0.0552 0.229 Uiso 0.798(4) 1 calc R U P A 1
C92A C 0.8358(9) 0.8365(4) 0.0128(2) 0.144(3) Uani 0.798(4) 1 d D . P A 1
H92A H 0.8217 0.8086 -0.0207 0.173 Uiso 0.798(4) 1 calc R U P A 1
H92B H 0.8381 0.7977 0.0446 0.173 Uiso 0.798(4) 1 calc R U P A 1
C93A C 0.9743(8) 0.8721(4) 0.0066(2) 0.132(2) Uani 0.798(4) 1 d D . P A 1
H93A H 0.9688 0.9128 -0.0241 0.159 Uiso 0.798(4) 1 calc R U P A 1
H93B H 0.9880 0.8987 0.0407 0.159 Uiso 0.798(4) 1 calc R U P A 1
C94A C 1.1003(10) 0.8153(4) -0.0044(3) 0.156(3) Uani 0.798(4) 1 d D . P A 1
H94A H 1.0899 0.7904 -0.0395 0.188 Uiso 0.798(4) 1 calc R U P A 1
H94B H 1.1054 0.7734 0.0254 0.188 Uiso 0.798(4) 1 calc R U P A 1
C95A C 1.2361(15) 0.8552(9) -0.0079(6) 0.259(8) Uani 0.798(4) 1 d D . P A 1
H95A H 1.2481 0.8810 -0.0446 0.389 Uiso 0.798(4) 1 calc R U P A 1
H95B H 1.3132 0.8156 -0.0013 0.389 Uiso 0.798(4) 1 calc R U P A 1
H95C H 1.2329 0.8943 0.0201 0.389 Uiso 0.798(4) 1 calc R U P A 1
C90B C 1.2273(15) 0.8418(10) -0.0125(8) 0.065(4) Uiso 0.202(4) 1 d D U P A 2
H90D H 1.2911 0.8827 -0.0165 0.097 Uiso 0.202(4) 1 calc R U P A 2
H90E H 1.2632 0.7998 0.0134 0.097 Uiso 0.202(4) 1 calc R U P A 2
H90F H 1.2171 0.8205 -0.0485 0.097 Uiso 0.202(4) 1 calc R U P A 2
C91B C 1.091(2) 0.8763(17) 0.0090(12) 0.143(9) Uiso 0.202(4) 1 d D U P A 2
H91C H 1.1060 0.8996 0.0442 0.171 Uiso 0.202(4) 1 calc R U P A 2
H91D H 1.0601 0.9202 -0.0172 0.171 Uiso 0.202(4) 1 calc R U P A 2
C92B C 0.975(2) 0.8283(18) 0.0189(17) 0.172(13) Uiso 0.202(4) 1 d D U P A 2
H92C H 0.9837 0.7983 0.0548 0.206 Uiso 0.202(4) 1 calc R U P A 2
H92D H 0.9743 0.7907 -0.0104 0.206 Uiso 0.202(4) 1 calc R U P A 2
C93B C 0.839(2) 0.8840(15) 0.0192(11) 0.106(6) Uiso 0.202(4) 1 d D U P A 2
H93C H 0.8431 0.9168 0.0511 0.127 Uiso 0.202(4) 1 calc R U P A 2
H93D H 0.8459 0.9196 -0.0142 0.127 Uiso 0.202(4) 1 calc R U P A 2
C94B C 0.695(3) 0.858(2) 0.021(3) 0.18(2) Uiso 0.202(4) 1 d D U P A 2
H94C H 0.6908 0.8137 0.0488 0.221 Uiso 0.202(4) 1 calc R U P A 2
H94D H 0.6783 0.8384 -0.0153 0.221 Uiso 0.202(4) 1 calc R U P A 2
C95B C 0.575(3) 0.9230(18) 0.0354(13) 0.145(10) Uiso 0.202(4) 1 d D U P A 2
H95D H 0.4868 0.9004 0.0356 0.217 Uiso 0.202(4) 1 calc R U P A 2
H95E H 0.5882 0.9420 0.0719 0.217 Uiso 0.202(4) 1 calc R U P A 2
H95F H 0.5756 0.9668 0.0077 0.217 Uiso 0.202(4) 1 calc R U P A 2


#==============================================================================

# MOLECULAR GEOMETRY

_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 C19 1.7630(19) . ?
P1 C1 1.8683(18) . ?
N1 C19 1.383(2) . ?
N1 C20 1.416(3) . ?
N1 C24 1.446(2) . ?
N2 C19 1.392(2) . ?
N2 C21 1.403(3) . ?
N2 C33 1.438(2) . ?
C1 C2 1.424(2) . ?
C1 C6 1.433(2) . ?
C2 C3 1.395(2) . ?
C2 C7 1.562(2) . ?
C3 C4 1.390(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.391(3) . ?
C4 C11 1.537(2) . ?
C5 C6 1.395(3) . ?
C5 H5 0.9500 . ?
C6 C15 1.560(2) . ?
C7 C9 1.520(3) . ?
C7 C8 1.536(3) . ?
C7 C10 1.542(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C14 1.533(3) . ?
C11 C13 1.533(3) . ?
C11 C12 1.536(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.530(3) . ?
C15 C17 1.537(3) . ?
C15 C18 1.540(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C20 C21 1.335(3) . ?
C20 C22 1.495(3) . ?
C21 C23 1.494(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.395(3) . ?
C24 C29 1.396(3) . ?
C25 C26 1.394(3) . ?
C25 C30 1.503(3) . ?
C26 C27 1.385(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.388(3) . ?
C27 C31 1.509(3) . ?
C28 C29 1.392(3) . ?
C28 H28 0.9500 . ?
C29 C32 1.506(3) . ?
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 C34 1.396(3) . ?
C33 C38 1.402(2) . ?
C34 C35 1.383(3) . ?
C34 C39 1.501(3) . ?
C35 C36 1.387(3) . ?
C35 H35 0.9500 . ?
C36 C37 1.381(3) . ?
C36 C40 1.511(3) . ?
C37 C38 1.385(3) . ?
C37 H37 0.9500 . ?
C38 C41 1.509(3) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
P2 C60 1.7594(19) . ?
P2 C42 1.8639(18) . ?
N3 C60 1.391(2) . ?
N3 C61 1.422(2) . ?
N3 C65 1.444(2) . ?
N4 C60 1.383(2) . ?
N4 C62 1.405(3) . ?
N4 C74 1.438(2) . ?
C42 C47 1.426(3) . ?
C42 C43 1.427(3) . ?
C43 C44 1.402(3) . ?
C43 C48 1.556(3) . ?
C44 C45 1.383(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.387(3) . ?
C45 C52A 1.504(10) . ?
C45 C52B 1.69(3) . ?
C46 C47 1.394(3) . ?
C46 H46 0.9500 . ?
C47 C56 1.556(3) . ?
C48 C51 1.534(3) . ?
C48 C49 1.535(3) . ?
C48 C50 1.540(3) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52A C55A 1.516(11) . ?
C52A C53A 1.530(9) . ?
C52A C54A 1.549(9) . ?
C53A H53A 0.9800 . ?
C53A H53B 0.9800 . ?
C53A H53C 0.9800 . ?
C54A H54A 0.9800 . ?
C54A H54B 0.9800 . ?
C54A H54C 0.9800 . ?
C55A H55A 0.9800 . ?
C55A H55B 0.9800 . ?
C55A H55C 0.9800 . ?
C52B C53B 1.41(5) . ?
C52B C54B 1.47(4) . ?
C52B C55B 1.56(4) . ?
C53B H53D 0.9800 . ?
C53B H53E 0.9800 . ?
C53B H53F 0.9800 . ?
C54B H54D 0.9800 . ?
C54B H54E 0.9800 . ?
C54B H54F 0.9800 . ?
C55B H55D 0.9800 . ?
C55B H55E 0.9800 . ?
C55B H55F 0.9800 . ?
C56 C59 1.530(3) . ?
C56 C57 1.541(3) . ?
C56 C58 1.543(3) . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C61 C62 1.330(3) . ?
C61 C63 1.499(3) . ?
C62 C64 1.497(3) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 C70 1.394(3) . ?
C65 C66 1.397(3) . ?
C66 C67 1.388(3) . ?
C66 C71 1.506(3) . ?
C67 C68 1.385(3) . ?
C67 H67 0.9500 . ?
C68 C69 1.384(3) . ?
C68 C72 1.510(3) . ?
C69 C70 1.390(3) . ?
C69 H69 0.9500 . ?
C70 C73 1.500(3) . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 C75 1.388(3) . ?
C74 C79 1.404(3) . ?
C75 C76 1.394(3) . ?
C75 C80 1.510(3) . ?
C76 C77 1.389(3) . ?
C76 H76 0.9500 . ?
C77 C78 1.385(3) . ?
C77 C81 1.513(3) . ?
C78 C79 1.390(3) . ?
C78 H78 0.9500 . ?
C79 C82 1.502(3) . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C90A C91A 1.548(15) . ?
C90A H90A 0.9800 . ?
C90A H90B 0.9800 . ?
C90A H90C 0.9800 . ?
C91A C92A 1.471(11) . ?
C91A H91A 0.9900 . ?
C91A H91B 0.9900 . ?
C92A C93A 1.539(9) . ?
C92A H92A 0.9900 . ?
C92A H92B 0.9900 . ?
C93A C94A 1.525(11) . ?
C93A H93A 0.9900 . ?
C93A H93B 0.9900 . ?
C94A C95A 1.551(14) . ?
C94A H94A 0.9900 . ?
C94A H94B 0.9900 . ?
C95A H95A 0.9800 . ?
C95A H95B 0.9800 . ?
C95A H95C 0.9800 . ?
C90B C91B 1.50(2) . ?
C90B H90D 0.9800 . ?
C90B H90E 0.9800 . ?
C90B H90F 0.9800 . ?
C91B C92B 1.46(2) . ?
C91B H91C 0.9900 . ?
C91B H91D 0.9900 . ?
C92B C93B 1.565(18) . ?
C92B H92C 0.9900 . ?
C92B H92D 0.9900 . ?
C93B C94B 1.52(2) . ?
C93B H93C 0.9900 . ?
C93B H93D 0.9900 . ?
C94B C95B 1.59(2) . ?
C94B H94C 0.9900 . ?
C94B H94D 0.9900 . ?
C95B H95D 0.9800 . ?
C95B H95E 0.9800 . ?
C95B H95F 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
C19 P1 C1 106.38(8) . . ?
C19 N1 C20 110.06(15) . . ?
C19 N1 C24 126.53(16) . . ?
C20 N1 C24 119.44(15) . . ?
C19 N2 C21 110.86(15) . . ?
C19 N2 C33 125.87(16) . . ?
C21 N2 C33 123.23(15) . . ?
C2 C1 C6 117.14(16) . . ?
C2 C1 P1 121.84(12) . . ?
C6 C1 P1 120.91(13) . . ?
C3 C2 C1 118.90(15) . . ?
C3 C2 C7 117.38(15) . . ?
C1 C2 C7 123.43(15) . . ?
C4 C3 C2 122.91(16) . . ?
C4 C3 H3 118.5 . . ?
C2 C3 H3 118.5 . . ?
C3 C4 C5 116.44(16) . . ?
C3 C4 C11 122.99(16) . . ?
C5 C4 C11 120.28(15) . . ?
C4 C5 C6 123.19(16) . . ?
C4 C5 H5 118.4 . . ?
C6 C5 H5 118.4 . . ?
C5 C6 C1 118.44(15) . . ?
C5 C6 C15 117.20(15) . . ?
C1 C6 C15 123.84(15) . . ?
C9 C7 C8 110.44(17) . . ?
C9 C7 C10 106.30(16) . . ?
C8 C7 C10 105.49(16) . . ?
C9 C7 C2 113.39(16) . . ?
C8 C7 C2 109.36(14) . . ?
C10 C7 C2 111.54(15) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C14 C11 C13 109.13(18) . . ?
C14 C11 C12 108.23(16) . . ?
C13 C11 C12 108.05(16) . . ?
C14 C11 C4 111.71(15) . . ?
C13 C11 C4 109.37(15) . . ?
C12 C11 C4 110.26(16) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C17 109.84(17) . . ?
C16 C15 C18 106.69(16) . . ?
C17 C15 C18 105.11(16) . . ?
C16 C15 C6 114.16(16) . . ?
C17 C15 C6 108.88(14) . . ?
C18 C15 C6 111.77(15) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 N2 103.92(16) . . ?
N1 C19 P1 136.38(14) . . ?
N2 C19 P1 119.61(13) . . ?
C21 C20 N1 107.97(17) . . ?
C21 C20 C22 130.90(19) . . ?
N1 C20 C22 121.12(18) . . ?
C20 C21 N2 107.15(17) . . ?
C20 C21 C23 131.00(19) . . ?
N2 C21 C23 121.83(17) . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C29 121.50(17) . . ?
C25 C24 N1 119.88(17) . . ?
C29 C24 N1 118.01(17) . . ?
C26 C25 C24 117.85(17) . . ?
C26 C25 C30 119.92(17) . . ?
C24 C25 C30 122.13(17) . . ?
C27 C26 C25 122.39(19) . . ?
C27 C26 H26 118.8 . . ?
C25 C26 H26 118.8 . . ?
C26 C27 C28 118.03(18) . . ?
C26 C27 C31 120.8(2) . . ?
C28 C27 C31 121.1(2) . . ?
C27 C28 C29 121.94(19) . . ?
C27 C28 H28 119.0 . . ?
C29 C28 H28 119.0 . . ?
C28 C29 C24 118.23(18) . . ?
C28 C29 C32 120.12(18) . . ?
C24 C29 C32 121.49(18) . . ?
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 . . ?
C34 C33 C38 120.69(17) . . ?
C34 C33 N2 119.29(16) . . ?
C38 C33 N2 119.94(16) . . ?
C35 C34 C33 118.15(17) . . ?
C35 C34 C39 120.38(18) . . ?
C33 C34 C39 121.46(18) . . ?
C34 C35 C36 122.68(19) . . ?
C34 C35 H35 118.7 . . ?
C36 C35 H35 118.7 . . ?
C37 C36 C35 117.67(19) . . ?
C37 C36 C40 121.0(2) . . ?
C35 C36 C40 121.3(2) . . ?
C36 C37 C38 122.25(18) . . ?
C36 C37 H37 118.9 . . ?
C38 C37 H37 118.9 . . ?
C37 C38 C33 118.49(17) . . ?
C37 C38 C41 119.28(17) . . ?
C33 C38 C41 122.23(17) . . ?
C34 C39 H39A 109.5 . . ?
C34 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C34 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C36 C40 H40A 109.5 . . ?
C36 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C36 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C60 P2 C42 105.22(8) . . ?
C60 N3 C61 109.36(15) . . ?
C60 N3 C65 125.84(14) . . ?
C61 N3 C65 118.84(15) . . ?
C60 N4 C62 110.66(16) . . ?
C60 N4 C74 124.06(15) . . ?
C62 N4 C74 125.09(16) . . ?
C47 C42 C43 117.87(16) . . ?
C47 C42 P2 120.54(14) . . ?
C43 C42 P2 121.43(14) . . ?
C44 C43 C42 118.25(17) . . ?
C44 C43 C48 117.10(16) . . ?
C42 C43 C48 124.20(16) . . ?
C45 C44 C43 123.03(18) . . ?
C45 C44 H44 118.5 . . ?
C43 C44 H44 118.5 . . ?
C44 C45 C46 117.08(17) . . ?
C44 C45 C52A 122.1(4) . . ?
C46 C45 C52A 120.7(4) . . ?
C44 C45 C52B 117.2(14) . . ?
C46 C45 C52B 123.7(14) . . ?
C45 C46 C47 122.88(18) . . ?
C45 C46 H46 118.6 . . ?
C47 C46 H46 118.6 . . ?
C46 C47 C42 118.74(17) . . ?
C46 C47 C56 117.32(16) . . ?
C42 C47 C56 123.72(16) . . ?
C51 C48 C49 105.13(17) . . ?
C51 C48 C50 105.91(17) . . ?
C49 C48 C50 109.55(18) . . ?
C51 C48 C43 112.33(16) . . ?
C49 C48 C43 115.90(16) . . ?
C50 C48 C43 107.59(15) . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C48 C51 H51A 109.5 . . ?
C48 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C48 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C45 C52A C55A 114.0(6) . . ?
C45 C52A C53A 109.4(7) . . ?
C55A C52A C53A 108.7(6) . . ?
C45 C52A C54A 111.7(6) . . ?
C55A C52A C54A 104.4(6) . . ?
C53A C52A C54A 108.4(6) . . ?
C52A C53A H53A 109.5 . . ?
C52A C53A H53B 109.5 . . ?
H53A C53A H53B 109.5 . . ?
C52A C53A H53C 109.5 . . ?
H53A C53A H53C 109.5 . . ?
H53B C53A H53C 109.5 . . ?
C52A C54A H54A 109.5 . . ?
C52A C54A H54B 109.5 . . ?
H54A C54A H54B 109.5 . . ?
C52A C54A H54C 109.5 . . ?
H54A C54A H54C 109.5 . . ?
H54B C54A H54C 109.5 . . ?
C52A C55A H55A 109.5 . . ?
C52A C55A H55B 109.5 . . ?
H55A C55A H55B 109.5 . . ?
C52A C55A H55C 109.5 . . ?
H55A C55A H55C 109.5 . . ?
H55B C55A H55C 109.5 . . ?
C53B C52B C54B 124(3) . . ?
C53B C52B C55B 110(3) . . ?
C54B C52B C55B 105(2) . . ?
C53B C52B C45 109(2) . . ?
C54B C52B C45 106(2) . . ?
C55B C52B C45 100(2) . . ?
C52B C53B H53D 109.5 . . ?
C52B C53B H53E 109.5 . . ?
H53D C53B H53E 109.5 . . ?
C52B C53B H53F 109.5 . . ?
H53D C53B H53F 109.5 . . ?
H53E C53B H53F 109.5 . . ?
C52B C54B H54D 109.5 . . ?
C52B C54B H54E 109.5 . . ?
H54D C54B H54E 109.5 . . ?
C52B C54B H54F 109.5 . . ?
H54D C54B H54F 109.5 . . ?
H54E C54B H54F 109.5 . . ?
C52B C55B H55D 109.5 . . ?
C52B C55B H55E 109.5 . . ?
H55D C55B H55E 109.5 . . ?
C52B C55B H55F 109.5 . . ?
H55D C55B H55F 109.5 . . ?
H55E C55B H55F 109.5 . . ?
C59 C56 C57 110.40(17) . . ?
C59 C56 C58 106.34(19) . . ?
C57 C56 C58 106.10(18) . . ?
C59 C56 C47 113.13(15) . . ?
C57 C56 C47 109.04(17) . . ?
C58 C56 C47 111.58(17) . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C56 C58 H58A 109.5 . . ?
C56 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C56 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C56 C59 H59A 109.5 . . ?
C56 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C56 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
N4 C60 N3 104.43(15) . . ?
N4 C60 P2 117.84(13) . . ?
N3 C60 P2 137.68(14) . . ?
C62 C61 N3 107.93(17) . . ?
C62 C61 C63 131.32(19) . . ?
N3 C61 C63 120.75(18) . . ?
C61 C62 N4 107.61(17) . . ?
C61 C62 C64 131.4(2) . . ?
N4 C62 C64 120.90(19) . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C62 C64 H64A 109.5 . . ?
C62 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C62 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C70 C65 C66 121.03(18) . . ?
C70 C65 N3 120.87(17) . . ?
C66 C65 N3 117.62(16) . . ?
C67 C66 C65 118.46(19) . . ?
C67 C66 C71 119.74(19) . . ?
C65 C66 C71 121.61(18) . . ?
C68 C67 C66 122.0(2) . . ?
C68 C67 H67 119.0 . . ?
C66 C67 H67 119.0 . . ?
C69 C68 C67 117.76(19) . . ?
C69 C68 C72 121.9(2) . . ?
C67 C68 C72 120.3(2) . . ?
C68 C69 C70 122.57(19) . . ?
C68 C69 H69 118.7 . . ?
C70 C69 H69 118.7 . . ?
C69 C70 C65 117.91(19) . . ?
C69 C70 C73 119.82(18) . . ?
C65 C70 C73 122.09(18) . . ?
C66 C71 H71A 109.5 . . ?
C66 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
C66 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C68 C72 H72A 109.5 . . ?
C68 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C68 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C70 C73 H73A 109.5 . . ?
C70 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C70 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C75 C74 C79 121.39(18) . . ?
C75 C74 N4 119.47(17) . . ?
C79 C74 N4 119.14(18) . . ?
C74 C75 C76 118.61(18) . . ?
C74 C75 C80 121.85(19) . . ?
C76 C75 C80 119.54(18) . . ?
C77 C76 C75 121.61(19) . . ?
C77 C76 H76 119.2 . . ?
C75 C76 H76 119.2 . . ?
C78 C77 C76 118.23(19) . . ?
C78 C77 C81 120.76(18) . . ?
C76 C77 C81 120.97(19) . . ?
C77 C78 C79 122.37(18) . . ?
C77 C78 H78 118.8 . . ?
C79 C78 H78 118.8 . . ?
C78 C79 C74 117.79(18) . . ?
C78 C79 C82 120.44(18) . . ?
C74 C79 C82 121.76(18) . . ?
C75 C80 H80A 109.5 . . ?
C75 C80 H80B 109.5 . . ?
H80A C80 H80B 109.5 . . ?
C75 C80 H80C 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
C77 C81 H81A 109.5 . . ?
C77 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
C77 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C79 C82 H82A 109.5 . . ?
C79 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C79 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C91A C90A H90A 109.5 . . ?
C91A C90A H90B 109.5 . . ?
H90A C90A H90B 109.5 . . ?
C91A C90A H90C 109.5 . . ?
H90A C90A H90C 109.5 . . ?
H90B C90A H90C 109.5 . . ?
C92A C91A C90A 109.8(12) . . ?
C92A C91A H91A 109.7 . . ?
C90A C91A H91A 109.7 . . ?
C92A C91A H91B 109.7 . . ?
C90A C91A H91B 109.7 . . ?
H91A C91A H91B 108.2 . . ?
C91A C92A C93A 112.6(9) . . ?
C91A C92A H92A 109.1 . . ?
C93A C92A H92A 109.1 . . ?
C91A C92A H92B 109.1 . . ?
C93A C92A H92B 109.1 . . ?
H92A C92A H92B 107.8 . . ?
C94A C93A C92A 116.4(6) . . ?
C94A C93A H93A 108.2 . . ?
C92A C93A H93A 108.2 . . ?
C94A C93A H93B 108.2 . . ?
C92A C93A H93B 108.2 . . ?
H93A C93A H93B 107.3 . . ?
C93A C94A C95A 113.2(8) . . ?
C93A C94A H94A 108.9 . . ?
C95A C94A H94A 108.9 . . ?
C93A C94A H94B 108.9 . . ?
C95A C94A H94B 108.9 . . ?
H94A C94A H94B 107.8 . . ?
C94A C95A H95A 109.5 . . ?
C94A C95A H95B 109.5 . . ?
H95A C95A H95B 109.5 . . ?
C94A C95A H95C 109.5 . . ?
H95A C95A H95C 109.5 . . ?
H95B C95A H95C 109.5 . . ?
C91B C90B H90D 109.5 . . ?
C91B C90B H90E 109.5 . . ?
H90D C90B H90E 109.5 . . ?
C91B C90B H90F 109.5 . . ?
H90D C90B H90F 109.5 . . ?
H90E C90B H90F 109.5 . . ?
C92B C91B C90B 121(2) . . ?
C92B C91B H91C 107.0 . . ?
C90B C91B H91C 107.0 . . ?
C92B C91B H91D 107.0 . . ?
C90B C91B H91D 107.0 . . ?
H91C C91B H91D 106.7 . . ?
C91B C92B C93B 108(2) . . ?
C91B C92B H92C 110.0 . . ?
C93B C92B H92C 110.0 . . ?
C91B C92B H92D 110.0 . . ?
C93B C92B H92D 110.0 . . ?
H92C C92B H92D 108.4 . . ?
C94B C93B C92B 126(2) . . ?
C94B C93B H93C 105.9 . . ?
C92B C93B H93C 105.9 . . ?
C94B C93B H93D 105.9 . . ?
C92B C93B H93D 105.9 . . ?
H93C C93B H93D 106.2 . . ?
C93B C94B C95B 116(2) . . ?
C93B C94B H94C 108.3 . . ?
C95B C94B H94C 108.3 . . ?
C93B C94B H94D 108.3 . . ?
C95B C94B H94D 108.3 . . ?
H94C C94B H94D 107.4 . . ?
C94B C95B H95D 109.5 . . ?
C94B C95B H95E 109.5 . . ?
H95D C95B H95E 109.5 . . ?
C94B C95B H95F 109.5 . . ?
H95D C95B H95F 109.5 . . ?
H95E C95B H95F 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
C19 P1 C1 C2 105.06(15) . . . . ?
C19 P1 C1 C6 -79.01(16) . . . . ?
C6 C1 C2 C3 18.0(2) . . . . ?
P1 C1 C2 C3 -165.93(14) . . . . ?
C6 C1 C2 C7 -155.59(17) . . . . ?
P1 C1 C2 C7 20.5(2) . . . . ?
C1 C2 C3 C4 -5.5(3) . . . . ?
C7 C2 C3 C4 168.52(17) . . . . ?
C2 C3 C4 C5 -7.8(3) . . . . ?
C2 C3 C4 C11 178.48(17) . . . . ?
C3 C4 C5 C6 8.3(3) . . . . ?
C11 C4 C5 C6 -177.76(17) . . . . ?
C4 C5 C6 C1 4.3(3) . . . . ?
C4 C5 C6 C15 -167.68(17) . . . . ?
C2 C1 C6 C5 -17.4(2) . . . . ?
P1 C1 C6 C5 166.46(14) . . . . ?
C2 C1 C6 C15 154.03(17) . . . . ?
P1 C1 C6 C15 -22.1(2) . . . . ?
C3 C2 C7 C9 110.6(2) . . . . ?
C1 C2 C7 C9 -75.8(2) . . . . ?
C3 C2 C7 C8 -125.71(18) . . . . ?
C1 C2 C7 C8 48.0(2) . . . . ?
C3 C2 C7 C10 -9.4(2) . . . . ?
C1 C2 C7 C10 164.26(18) . . . . ?
C3 C4 C11 C14 -17.0(3) . . . . ?
C5 C4 C11 C14 169.50(18) . . . . ?
C3 C4 C11 C13 103.9(2) . . . . ?
C5 C4 C11 C13 -69.6(2) . . . . ?
C3 C4 C11 C12 -137.40(19) . . . . ?
C5 C4 C11 C12 49.1(2) . . . . ?
C5 C6 C15 C16 -114.94(19) . . . . ?
C1 C6 C15 C16 73.5(2) . . . . ?
C5 C6 C15 C17 121.93(18) . . . . ?
C1 C6 C15 C17 -49.6(2) . . . . ?
C5 C6 C15 C18 6.3(2) . . . . ?
C1 C6 C15 C18 -165.29(18) . . . . ?
C20 N1 C19 N2 1.67(19) . . . . ?
C24 N1 C19 N2 158.82(17) . . . . ?
C20 N1 C19 P1 -174.77(15) . . . . ?
C24 N1 C19 P1 -17.6(3) . . . . ?
C21 N2 C19 N1 -2.05(18) . . . . ?
C33 N2 C19 N1 175.34(15) . . . . ?
C21 N2 C19 P1 175.12(12) . . . . ?
C33 N2 C19 P1 -7.5(2) . . . . ?
C1 P1 C19 N1 -21.0(2) . . . . ?
C1 P1 C19 N2 162.97(13) . . . . ?
C19 N1 C20 C21 -0.7(2) . . . . ?
C24 N1 C20 C21 -159.72(17) . . . . ?
C19 N1 C20 C22 178.42(18) . . . . ?
C24 N1 C20 C22 19.4(3) . . . . ?
N1 C20 C21 N2 -0.6(2) . . . . ?
C22 C20 C21 N2 -179.6(2) . . . . ?
N1 C20 C21 C23 177.57(19) . . . . ?
C22 C20 C21 C23 -1.4(4) . . . . ?
C19 N2 C21 C20 1.7(2) . . . . ?
C33 N2 C21 C20 -175.78(16) . . . . ?
C19 N2 C21 C23 -176.67(17) . . . . ?
C33 N2 C21 C23 5.9(3) . . . . ?
C19 N1 C24 C25 108.4(2) . . . . ?
C20 N1 C24 C25 -96.3(2) . . . . ?
C19 N1 C24 C29 -80.4(2) . . . . ?
C20 N1 C24 C29 74.8(2) . . . . ?
C29 C24 C25 C26 2.6(3) . . . . ?
N1 C24 C25 C26 173.49(17) . . . . ?
C29 C24 C25 C30 -173.86(19) . . . . ?
N1 C24 C25 C30 -3.0(3) . . . . ?
C24 C25 C26 C27 -0.8(3) . . . . ?
C30 C25 C26 C27 175.7(2) . . . . ?
C25 C26 C27 C28 -0.4(3) . . . . ?
C25 C26 C27 C31 -177.1(2) . . . . ?
C26 C27 C28 C29 -0.1(3) . . . . ?
C31 C27 C28 C29 176.6(2) . . . . ?
C27 C28 C29 C24 1.8(3) . . . . ?
C27 C28 C29 C32 -173.6(2) . . . . ?
C25 C24 C29 C28 -3.1(3) . . . . ?
N1 C24 C29 C28 -174.13(18) . . . . ?
C25 C24 C29 C32 172.21(19) . . . . ?
N1 C24 C29 C32 1.2(3) . . . . ?
C19 N2 C33 C34 77.8(2) . . . . ?
C21 N2 C33 C34 -105.1(2) . . . . ?
C19 N2 C33 C38 -105.3(2) . . . . ?
C21 N2 C33 C38 71.8(2) . . . . ?
C38 C33 C34 C35 3.0(3) . . . . ?
N2 C33 C34 C35 179.86(17) . . . . ?
C38 C33 C34 C39 -175.97(19) . . . . ?
N2 C33 C34 C39 0.9(3) . . . . ?
C33 C34 C35 C36 -2.0(3) . . . . ?
C39 C34 C35 C36 177.0(2) . . . . ?
C34 C35 C36 C37 -0.2(3) . . . . ?
C34 C35 C36 C40 178.9(2) . . . . ?
C35 C36 C37 C38 1.5(3) . . . . ?
C40 C36 C37 C38 -177.6(2) . . . . ?
C36 C37 C38 C33 -0.5(3) . . . . ?
C36 C37 C38 C41 179.2(2) . . . . ?
C34 C33 C38 C37 -1.8(3) . . . . ?
N2 C33 C38 C37 -178.64(17) . . . . ?
C34 C33 C38 C41 178.52(18) . . . . ?
N2 C33 C38 C41 1.7(3) . . . . ?
C60 P2 C42 C47 101.47(15) . . . . ?
C60 P2 C42 C43 -83.20(16) . . . . ?
C47 C42 C43 C44 -15.1(2) . . . . ?
P2 C42 C43 C44 169.40(13) . . . . ?
C47 C42 C43 C48 156.87(17) . . . . ?
P2 C42 C43 C48 -18.6(2) . . . . ?
C42 C43 C44 C45 4.3(3) . . . . ?
C48 C43 C44 C45 -168.32(17) . . . . ?
C43 C44 C45 C46 6.6(3) . . . . ?
C43 C44 C45 C52A -177.6(5) . . . . ?
C43 C44 C45 C52B 171.1(15) . . . . ?
C44 C45 C46 C47 -6.5(3) . . . . ?
C52A C45 C46 C47 177.6(5) . . . . ?
C52B C45 C46 C47 -169.9(16) . . . . ?
C45 C46 C47 C42 -4.5(3) . . . . ?
C45 C46 C47 C56 170.26(18) . . . . ?
C43 C42 C47 C46 15.3(3) . . . . ?
P2 C42 C47 C46 -169.21(14) . . . . ?
C43 C42 C47 C56 -159.08(17) . . . . ?
P2 C42 C47 C56 16.4(2) . . . . ?
C44 C43 C48 C51 -0.2(2) . . . . ?
C42 C43 C48 C51 -172.27(17) . . . . ?
C44 C43 C48 C49 -121.0(2) . . . . ?
C42 C43 C48 C49 66.9(2) . . . . ?
C44 C43 C48 C50 116.01(18) . . . . ?
C42 C43 C48 C50 -56.1(2) . . . . ?
C44 C45 C52A C55A 149.0(4) . . . . ?
C46 C45 C52A C55A -35.3(8) . . . . ?
C44 C45 C52A C53A -89.1(6) . . . . ?
C46 C45 C52A C53A 86.6(7) . . . . ?
C44 C45 C52A C54A 31.0(9) . . . . ?
C46 C45 C52A C54A -153.4(5) . . . . ?
C44 C45 C52B C53B -36(3) . . . . ?
C46 C45 C52B C53B 128(2) . . . . ?
C44 C45 C52B C54B -171.6(15) . . . . ?
C46 C45 C52B C54B -8(3) . . . . ?
C44 C45 C52B C55B 80(2) . . . . ?
C46 C45 C52B C55B -116.7(18) . . . . ?
C46 C47 C56 C59 113.9(2) . . . . ?
C42 C47 C56 C59 -71.6(2) . . . . ?
C46 C47 C56 C57 -122.83(19) . . . . ?
C42 C47 C56 C57 51.6(2) . . . . ?
C46 C47 C56 C58 -6.0(3) . . . . ?
C42 C47 C56 C58 168.5(2) . . . . ?
C62 N4 C60 N3 0.5(2) . . . . ?
C74 N4 C60 N3 175.83(16) . . . . ?
C62 N4 C60 P2 -177.54(13) . . . . ?
C74 N4 C60 P2 -2.2(2) . . . . ?
C61 N3 C60 N4 -0.28(19) . . . . ?
C65 N3 C60 N4 151.93(17) . . . . ?
C61 N3 C60 P2 177.15(17) . . . . ?
C65 N3 C60 P2 -30.6(3) . . . . ?
C42 P2 C60 N4 171.93(14) . . . . ?
C42 P2 C60 N3 -5.3(2) . . . . ?
C60 N3 C61 C62 0.0(2) . . . . ?
C65 N3 C61 C62 -154.49(17) . . . . ?
C60 N3 C61 C63 179.51(18) . . . . ?
C65 N3 C61 C63 25.1(3) . . . . ?
N3 C61 C62 N4 0.4(2) . . . . ?
C63 C61 C62 N4 -179.1(2) . . . . ?
N3 C61 C62 C64 177.4(2) . . . . ?
C63 C61 C62 C64 -2.1(4) . . . . ?
C60 N4 C62 C61 -0.6(2) . . . . ?
C74 N4 C62 C61 -175.82(18) . . . . ?
C60 N4 C62 C64 -178.0(2) . . . . ?
C74 N4 C62 C64 6.7(3) . . . . ?
C60 N3 C65 C70 110.3(2) . . . . ?
C61 N3 C65 C70 -99.8(2) . . . . ?
C60 N3 C65 C66 -77.5(2) . . . . ?
C61 N3 C65 C66 72.4(2) . . . . ?
C70 C65 C66 C67 -5.3(3) . . . . ?
N3 C65 C66 C67 -177.44(16) . . . . ?
C70 C65 C66 C71 169.69(18) . . . . ?
N3 C65 C66 C71 -2.5(3) . . . . ?
C65 C66 C67 C68 1.6(3) . . . . ?
C71 C66 C67 C68 -173.43(18) . . . . ?
C66 C67 C68 C69 1.6(3) . . . . ?
C66 C67 C68 C72 178.86(19) . . . . ?
C67 C68 C69 C70 -1.3(3) . . . . ?
C72 C68 C69 C70 -178.5(2) . . . . ?
C68 C69 C70 C65 -2.2(3) . . . . ?
C68 C69 C70 C73 173.04(18) . . . . ?
C66 C65 C70 C69 5.5(3) . . . . ?
N3 C65 C70 C69 177.46(16) . . . . ?
C66 C65 C70 C73 -169.62(17) . . . . ?
N3 C65 C70 C73 2.3(3) . . . . ?
C60 N4 C74 C75 -97.9(2) . . . . ?
C62 N4 C74 C75 76.8(2) . . . . ?
C60 N4 C74 C79 82.6(2) . . . . ?
C62 N4 C74 C79 -102.7(2) . . . . ?
C79 C74 C75 C76 -0.3(3) . . . . ?
N4 C74 C75 C76 -179.81(17) . . . . ?
C79 C74 C75 C80 179.12(18) . . . . ?
N4 C74 C75 C80 -0.3(3) . . . . ?
C74 C75 C76 C77 -0.2(3) . . . . ?
C80 C75 C76 C77 -179.70(19) . . . . ?
C75 C76 C77 C78 0.2(3) . . . . ?
C75 C76 C77 C81 177.96(19) . . . . ?
C76 C77 C78 C79 0.4(3) . . . . ?
C81 C77 C78 C79 -177.33(19) . . . . ?
C77 C78 C79 C74 -1.0(3) . . . . ?
C77 C78 C79 C82 177.96(19) . . . . ?
C75 C74 C79 C78 0.9(3) . . . . ?
N4 C74 C79 C78 -179.61(16) . . . . ?
C75 C74 C79 C82 -178.01(19) . . . . ?
N4 C74 C79 C82 1.5(3) . . . . ?
C90A C91A C92A C93A 179.4(6) . . . . ?
C91A C92A C93A C94A -177.9(7) . . . . ?
C92A C93A C94A C95A -177.7(7) . . . . ?
C90B C91B C92B C93B -159(2) . . . . ?
C91B C92B C93B C94B 172(4) . . . . ?
C92B C93B C94B C95B 166(3) . . . . ?

_refine_diff_density_max         0.374
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.040

####################################################################### 
# 
# 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_ax1921_MesStarPHCHMeIDip_cmp19
_database_code_depnum_ccdc_archive 'CCDC 2046868'
loop_
_audit_author_name
_audit_author_address
'Hering-Junghans C.'
;LIKAT Rostock
Germany
;
_audit_update_record             
;
2020-11-27 deposited with the CCDC.	2021-01-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H71 N2 P'
_chemical_formula_sum            'C48 H71 N2 P'
_chemical_formula_weight         707.03

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

#==============================================================================

# CRYSTAL DATA

_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                   10.4250(10)
_cell_length_b                   13.7255(13)
_cell_length_c                   16.5992(16)
_cell_angle_alpha                77.9987(25)
_cell_angle_beta                 74.6150(25)
_cell_angle_gamma                71.7355(25)
_cell_volume                     2154.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9272
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      29.45

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_F_000             776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.306
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.072
_exptl_absorpt_coefficient_mu    0.097
_shelx_estimated_absorpt_T_min   0.971
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?

#==============================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            87182
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.577
_diffrn_reflns_theta_max         29.000
_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             11466
_reflns_number_gt                8784
_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       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms 
 were positioned geometrically and refined using a riding model, with C---H = 
 0.98 (methyl groups), 0.99Å (methylene groups), 1.00Å (methine groups) or 
 0.95 Å (aryl CH) and with Uiso(H) = 1.5 times Ueq(C) 
 (methyl groups) or with Uiso(H) = 1.2 times Ueq(C) 
 (methylene  groups, aryl CH, methine groups). Torsion angles of all methyl 
 groups were allowed to refine.
 
 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 > 2σ(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     
'w=1/[σ²(Fo²)+(0.0679P)²+1.1525P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11466
_refine_ls_number_parameters     518
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0530
_refine_ls_wR_factor_ref         0.1482
_refine_ls_wR_factor_gt          0.1334
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.46280(4) 0.57147(3) 0.16759(2) 0.02603(10) Uani 1 1 d . . . . .
N1 N 0.36148(13) 0.82081(9) 0.20092(7) 0.0235(3) Uani 1 1 d . . . . .
N2 N 0.37656(13) 0.78457(9) 0.33367(7) 0.0224(2) Uani 1 1 d . . . . .
C1 C 0.39716(14) 0.73761(11) 0.26244(8) 0.0203(3) Uani 1 1 d . . . . .
C2 C 0.31565(17) 0.91525(12) 0.23482(9) 0.0271(3) Uani 1 1 d . . . . .
C3 C 0.32580(16) 0.89287(12) 0.31574(9) 0.0250(3) Uani 1 1 d . . . . .
C4 C 0.44368(16) 0.63372(12) 0.25786(9) 0.0255(3) Uani 1 1 d . . . . .
H4 H 0.4685 0.5898 0.3069 0.031 Uiso 1 1 calc R U . . .
C5 C 0.2675(2) 1.01673(13) 0.18349(11) 0.0390(4) Uani 1 1 d . . . . .
H5A H 0.2534 1.0729 0.2158 0.059 Uiso 1 1 calc R U . . .
H5B H 0.1802 1.0208 0.1695 0.059 Uiso 1 1 calc R U . . .
H5C H 0.3373 1.0234 0.1314 0.059 Uiso 1 1 calc R U . . .
C6 C 0.29812(19) 0.96286(13) 0.37984(10) 0.0321(3) Uani 1 1 d . . . . .
H6A H 0.2616 1.0347 0.3556 0.048 Uiso 1 1 calc R U . . .
H6B H 0.3843 0.9557 0.3966 0.048 Uiso 1 1 calc R U . . .
H6C H 0.2303 0.9441 0.4294 0.048 Uiso 1 1 calc R U . . .
C7 C 0.37204(15) 0.81358(11) 0.11425(8) 0.0221(3) Uani 1 1 d . . . . .
C8 C 0.25234(17) 0.81856(12) 0.08822(10) 0.0282(3) Uani 1 1 d . . . . .
C9 C 0.2663(2) 0.80785(14) 0.00427(11) 0.0367(4) Uani 1 1 d . . . . .
H9 H 0.1870 0.8106 -0.0150 0.044 Uiso 1 1 calc R U . . .
C10 C 0.3930(2) 0.79335(14) -0.05104(10) 0.0378(4) Uani 1 1 d . . . . .
H10 H 0.4011 0.7838 -0.1074 0.045 Uiso 1 1 calc R U . . .
C11 C 0.50823(19) 0.79263(13) -0.02484(10) 0.0322(3) Uani 1 1 d . . . . .
H11 H 0.5944 0.7848 -0.0642 0.039 Uiso 1 1 calc R U . . .
C12 C 0.50108(16) 0.80309(11) 0.05819(9) 0.0243(3) Uani 1 1 d . . . . .
C13 C 0.11173(18) 0.83356(16) 0.14746(12) 0.0402(4) Uani 1 1 d . . . . .
H13 H 0.1193 0.8496 0.2018 0.048 Uiso 1 1 calc R U . . .
C14 C 0.0642(2) 0.73474(19) 0.16593(17) 0.0590(6) Uani 1 1 d . . . . .
H14A H 0.0562 0.7178 0.1133 0.089 Uiso 1 1 calc R U . . .
H14B H -0.0259 0.7457 0.2054 0.089 Uiso 1 1 calc R U . . .
H14C H 0.1320 0.6775 0.1909 0.089 Uiso 1 1 calc R U . . .
C15 C 0.0028(2) 0.92402(19) 0.11150(17) 0.0604(6) Uani 1 1 d . . . . .
H15A H 0.0340 0.9870 0.0986 0.091 Uiso 1 1 calc R U . . .
H15B H -0.0851 0.9349 0.1531 0.091 Uiso 1 1 calc R U . . .
H15C H -0.0100 0.9079 0.0598 0.091 Uiso 1 1 calc R U . . .
C16 C 0.62856(17) 0.80167(13) 0.08669(10) 0.0306(3) Uani 1 1 d . . . . .
H16 H 0.6276 0.7588 0.1434 0.037 Uiso 1 1 calc R U . . .
C17 C 0.6276(2) 0.91069(17) 0.09558(16) 0.0505(5) Uani 1 1 d . . . . .
H17A H 0.6210 0.9557 0.0418 0.076 Uiso 1 1 calc R U . . .
H17B H 0.7133 0.9077 0.1112 0.076 Uiso 1 1 calc R U . . .
H17C H 0.5481 0.9385 0.1395 0.076 Uiso 1 1 calc R U . . .
C18 C 0.76355(19) 0.75402(15) 0.02697(13) 0.0406(4) Uani 1 1 d . . . . .
H18A H 0.7614 0.6871 0.0161 0.061 Uiso 1 1 calc R U . . .
H18B H 0.8418 0.7439 0.0529 0.061 Uiso 1 1 calc R U . . .
H18C H 0.7738 0.8006 -0.0263 0.061 Uiso 1 1 calc R U . . .
C19 C 0.38258(15) 0.72901(11) 0.41641(8) 0.0223(3) Uani 1 1 d . . . . .
C20 C 0.25882(17) 0.72111(14) 0.47362(9) 0.0307(3) Uani 1 1 d . . . . .
C21 C 0.26820(19) 0.66867(15) 0.55439(10) 0.0354(4) Uani 1 1 d . . . . .
H21 H 0.1859 0.6632 0.5946 0.042 Uiso 1 1 calc R U . . .
C22 C 0.39417(19) 0.62461(13) 0.57711(9) 0.0321(3) Uani 1 1 d . . . . .
H22 H 0.3982 0.5884 0.6322 0.039 Uiso 1 1 calc R U . . .
C23 C 0.51403(18) 0.63329(13) 0.51978(10) 0.0305(3) Uani 1 1 d . . . . .
H23 H 0.6005 0.6023 0.5357 0.037 Uiso 1 1 calc R U . . .
C24 C 0.51092(16) 0.68666(12) 0.43892(9) 0.0260(3) Uani 1 1 d . . . . .
C25A C 0.1204(8) 0.7710(7) 0.4492(5) 0.0353(13) Uani 0.70(3) 1 d . . P A 1
H25A H 0.1344 0.8128 0.3921 0.042 Uiso 0.70(3) 1 calc R U P A 1
C26A C 0.0648(15) 0.6807(14) 0.4451(11) 0.086(4) Uani 0.70(3) 1 d . . P A 1
H26A H 0.0508 0.6398 0.5010 0.129 Uiso 0.70(3) 1 calc R U P A 1
H26B H 0.1317 0.6365 0.4047 0.129 Uiso 0.70(3) 1 calc R U P A 1
H26C H -0.0234 0.7084 0.4270 0.129 Uiso 0.70(3) 1 calc R U P A 1
C27A C 0.0108(11) 0.8397(8) 0.5122(4) 0.0430(13) Uani 0.70(3) 1 d . . P A 1
H27A H -0.0088 0.7974 0.5670 0.064 Uiso 0.70(3) 1 calc R U P A 1
H27B H -0.0743 0.8699 0.4909 0.064 Uiso 0.70(3) 1 calc R U P A 1
H27C H 0.0460 0.8952 0.5189 0.064 Uiso 0.70(3) 1 calc R U P A 1
C25B C 0.1158(19) 0.739(2) 0.4498(12) 0.043(5) Uani 0.30(3) 1 d . . P A 2
H25B H 0.1303 0.7639 0.3878 0.051 Uiso 0.30(3) 1 calc R U P A 2
C26B C 0.059(3) 0.652(3) 0.4633(16) 0.058(5) Uani 0.30(3) 1 d . . P A 2
H26D H 0.1281 0.5949 0.4360 0.087 Uiso 0.30(3) 1 calc R U P A 2
H26E H -0.0234 0.6728 0.4390 0.087 Uiso 0.30(3) 1 calc R U P A 2
H26F H 0.0331 0.6295 0.5239 0.087 Uiso 0.30(3) 1 calc R U P A 2
C27B C 0.024(3) 0.828(2) 0.490(3) 0.072(7) Uani 0.30(3) 1 d . . P A 2
H27D H 0.0174 0.8113 0.5514 0.109 Uiso 0.30(3) 1 calc R U P A 2
H27E H -0.0679 0.8432 0.4783 0.109 Uiso 0.30(3) 1 calc R U P A 2
H27F H 0.0608 0.8877 0.4687 0.109 Uiso 0.30(3) 1 calc R U P A 2
C28 C 0.64336(18) 0.70238(17) 0.37957(11) 0.0418(4) Uani 1 1 d . . . . .
H28 H 0.6261 0.7281 0.3214 0.050 Uiso 1 1 calc R U . . .
C29 C 0.6870(3) 0.78477(18) 0.4097(2) 0.0757(9) Uani 1 1 d . . . . .
H29A H 0.6110 0.8486 0.4129 0.114 Uiso 1 1 calc R U . . .
H29B H 0.7689 0.7992 0.3696 0.114 Uiso 1 1 calc R U . . .
H29C H 0.7085 0.7585 0.4655 0.114 Uiso 1 1 calc R U . . .
C30 C 0.7633(2) 0.60502(17) 0.37715(16) 0.0544(6) Uani 1 1 d . . . . .
H30A H 0.7883 0.5845 0.4323 0.082 Uiso 1 1 calc R U . . .
H30B H 0.8429 0.6185 0.3340 0.082 Uiso 1 1 calc R U . . .
H30C H 0.7362 0.5492 0.3635 0.082 Uiso 1 1 calc R U . . .
C31 C 0.53068(15) 0.43024(11) 0.20458(8) 0.0225(3) Uani 1 1 d . . . . .
C32 C 0.43755(16) 0.36805(12) 0.24670(9) 0.0257(3) Uani 1 1 d . . . . .
C33 C 0.49222(18) 0.26665(12) 0.28156(9) 0.0292(3) Uani 1 1 d . . . . .
H33 H 0.4298 0.2270 0.3112 0.035 Uiso 1 1 calc R U . . .
C34 C 0.63262(18) 0.22026(12) 0.27542(9) 0.0286(3) Uani 1 1 d . . . . .
C35 C 0.72111(17) 0.27758(12) 0.22811(9) 0.0272(3) Uani 1 1 d . . . . .
H35 H 0.8179 0.2459 0.2204 0.033 Uiso 1 1 calc R U . . .
C36 C 0.67587(16) 0.38011(12) 0.19083(9) 0.0240(3) Uani 1 1 d . . . . .
C37 C 0.27891(17) 0.40298(14) 0.25363(11) 0.0324(3) Uani 1 1 d . . . . .
C38 C 0.2097(2) 0.31553(18) 0.29627(15) 0.0509(5) Uani 1 1 d . . . . .
H38A H 0.2265 0.2921 0.3534 0.076 Uiso 1 1 calc R U . . .
H38B H 0.2486 0.2575 0.2633 0.076 Uiso 1 1 calc R U . . .
H38C H 0.1098 0.3415 0.2992 0.076 Uiso 1 1 calc R U . . .
C39 C 0.2457(2) 0.43384(17) 0.16517(12) 0.0421(4) Uani 1 1 d . . . . .
H39A H 0.1453 0.4605 0.1705 0.063 Uiso 1 1 calc R U . . .
H39B H 0.2804 0.3731 0.1353 0.063 Uiso 1 1 calc R U . . .
H39C H 0.2902 0.4876 0.1334 0.063 Uiso 1 1 calc R U . . .
C40 C 0.20796(18) 0.48987(15) 0.30869(11) 0.0373(4) Uani 1 1 d . . . . .
H40A H 0.2468 0.5488 0.2850 0.056 Uiso 1 1 calc R U . . .
H40B H 0.2232 0.4646 0.3660 0.056 Uiso 1 1 calc R U . . .
H40C H 0.1085 0.5119 0.3103 0.056 Uiso 1 1 calc R U . . .
C41 C 0.6834(2) 0.10765(13) 0.31447(11) 0.0380(4) Uani 1 1 d . . . . .
C42 C 0.6087(3) 0.09308(15) 0.40725(12) 0.0523(6) Uani 1 1 d . . . . .
H42A H 0.6427 0.0211 0.4321 0.078 Uiso 1 1 calc R U . . .
H42B H 0.5090 0.1094 0.4109 0.078 Uiso 1 1 calc R U . . .
H42C H 0.6266 0.1394 0.4381 0.078 Uiso 1 1 calc R U . . .
C43 C 0.6486(2) 0.03869(14) 0.26540(12) 0.0449(5) Uani 1 1 d . . . . .
H43A H 0.6926 0.0502 0.2056 0.067 Uiso 1 1 calc R U . . .
H43B H 0.5481 0.0563 0.2717 0.067 Uiso 1 1 calc R U . . .
H43C H 0.6830 -0.0342 0.2878 0.067 Uiso 1 1 calc R U . . .
C44 C 0.8376(3) 0.07418(17) 0.31020(16) 0.0581(6) Uani 1 1 d . . . . .
H44A H 0.8872 0.0804 0.2511 0.087 Uiso 1 1 calc R U . . .
H44B H 0.8649 0.0020 0.3363 0.087 Uiso 1 1 calc R U . . .
H44C H 0.8606 0.1185 0.3404 0.087 Uiso 1 1 calc R U . . .
C45 C 0.79149(17) 0.42840(13) 0.13421(10) 0.0299(3) Uani 1 1 d . . . . .
C46 C 0.93607(19) 0.35076(16) 0.12641(14) 0.0457(5) Uani 1 1 d . . . . .
H46A H 1.0051 0.3844 0.0898 0.069 Uiso 1 1 calc R U . . .
H46B H 0.9374 0.2911 0.1021 0.069 Uiso 1 1 calc R U . . .
H46C H 0.9578 0.3273 0.1824 0.069 Uiso 1 1 calc R U . . .
C47 C 0.80247(19) 0.51827(14) 0.17173(12) 0.0358(4) Uani 1 1 d . . . . .
H47A H 0.8302 0.4918 0.2259 0.054 Uiso 1 1 calc R U . . .
H47B H 0.7125 0.5702 0.1804 0.054 Uiso 1 1 calc R U . . .
H47C H 0.8717 0.5500 0.1328 0.054 Uiso 1 1 calc R U . . .
C48 C 0.7700(2) 0.45905(15) 0.04289(10) 0.0370(4) Uani 1 1 d . . . . .
H48A H 0.6816 0.5120 0.0420 0.056 Uiso 1 1 calc R U . . .
H48B H 0.7692 0.3979 0.0214 0.056 Uiso 1 1 calc R U . . .
H48C H 0.8455 0.4867 0.0073 0.056 Uiso 1 1 calc R U . . .
H1A H 0.571(3) 0.586(2) 0.1146(17) 0.010(8) Uiso 0.53(4) 1 d . . P B 1
H1B H 0.341(4) 0.583(3) 0.159(2) 0.021(11) Uiso 0.47(4) 1 d . . P B 2


#==============================================================================

# MOLECULAR GEOMETRY

_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 C4 1.8117(15) . ?
P1 C31 1.8738(15) . ?
P1 H1A 1.28(3) . ?
P1 H1B 1.28(4) . ?
N1 C1 1.3913(17) . ?
N1 C2 1.4134(19) . ?
N1 C7 1.4354(17) . ?
N2 C1 1.3981(17) . ?
N2 C3 1.4088(19) . ?
N2 C19 1.4324(17) . ?
C1 C4 1.366(2) . ?
C2 C3 1.339(2) . ?
C2 C5 1.488(2) . ?
C3 C6 1.492(2) . ?
C4 H4 0.9500 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C12 1.402(2) . ?
C7 C8 1.403(2) . ?
C8 C9 1.396(2) . ?
C8 C13 1.513(2) . ?
C9 C10 1.377(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.378(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.395(2) . ?
C11 H11 0.9500 . ?
C12 C16 1.518(2) . ?
C13 C14 1.532(3) . ?
C13 C15 1.535(3) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.531(3) . ?
C16 C18 1.531(2) . ?
C16 H16 1.0000 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C24 1.398(2) . ?
C19 C20 1.405(2) . ?
C20 C21 1.396(2) . ?
C20 C25A 1.514(8) . ?
C20 C25B 1.574(17) . ?
C21 C22 1.379(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.377(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.392(2) . ?
C23 H23 0.9500 . ?
C24 C28 1.517(2) . ?
C25A C26A 1.544(13) . ?
C25A C27A 1.546(9) . ?
C25A H25A 1.0000 . ?
C26A H26A 0.9800 . ?
C26A H26B 0.9800 . ?
C26A H26C 0.9800 . ?
C27A H27A 0.9800 . ?
C27A H27B 0.9800 . ?
C27A H27C 0.9800 . ?
C25B C27B 1.45(3) . ?
C25B C26B 1.45(3) . ?
C25B H25B 1.0000 . ?
C26B H26D 0.9800 . ?
C26B H26E 0.9800 . ?
C26B H26F 0.9800 . ?
C27B H27D 0.9800 . ?
C27B H27E 0.9800 . ?
C27B H27F 0.9800 . ?
C28 C30 1.516(3) . ?
C28 C29 1.554(3) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C36 1.430(2) . ?
C31 C32 1.439(2) . ?
C32 C33 1.393(2) . ?
C32 C37 1.550(2) . ?
C33 C34 1.386(2) . ?
C33 H33 0.9500 . ?
C34 C35 1.379(2) . ?
C34 C41 1.530(2) . ?
C35 C36 1.401(2) . ?
C35 H35 0.9500 . ?
C36 C45 1.554(2) . ?
C37 C40 1.532(2) . ?
C37 C39 1.541(2) . ?
C37 C38 1.543(3) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C44 1.513(3) . ?
C41 C42 1.534(3) . ?
C41 C43 1.544(3) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C47 1.539(2) . ?
C45 C46 1.540(2) . ?
C45 C48 1.543(2) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 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
C4 P1 C31 103.86(6) . . ?
C4 P1 H1A 107.1(12) . . ?
C31 P1 H1A 99.1(12) . . ?
C4 P1 H1B 106.4(16) . . ?
C31 P1 H1B 105.5(16) . . ?
C1 N1 C2 110.65(11) . . ?
C1 N1 C7 125.43(12) . . ?
C2 N1 C7 123.91(12) . . ?
C1 N2 C3 110.49(11) . . ?
C1 N2 C19 124.03(12) . . ?
C3 N2 C19 124.60(11) . . ?
C4 C1 N1 130.34(12) . . ?
C4 C1 N2 126.03(12) . . ?
N1 C1 N2 103.62(12) . . ?
C3 C2 N1 107.46(13) . . ?
C3 C2 C5 130.37(14) . . ?
N1 C2 C5 122.18(13) . . ?
C2 C3 N2 107.74(12) . . ?
C2 C3 C6 130.23(14) . . ?
N2 C3 C6 121.97(13) . . ?
C1 C4 P1 126.47(11) . . ?
C1 C4 H4 116.8 . . ?
P1 C4 H4 116.8 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C12 C7 C8 122.18(13) . . ?
C12 C7 N1 119.00(13) . . ?
C8 C7 N1 118.82(13) . . ?
C9 C8 C7 117.66(15) . . ?
C9 C8 C13 119.71(15) . . ?
C7 C8 C13 122.63(14) . . ?
C10 C9 C8 121.09(16) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C9 C10 C11 120.19(15) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C10 C11 C12 121.46(16) . . ?
C10 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C11 C12 C7 117.33(14) . . ?
C11 C12 C16 121.15(14) . . ?
C7 C12 C16 121.52(13) . . ?
C8 C13 C14 110.90(17) . . ?
C8 C13 C15 111.57(17) . . ?
C14 C13 C15 109.42(18) . . ?
C8 C13 H13 108.3 . . ?
C14 C13 H13 108.3 . . ?
C15 C13 H13 108.3 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C12 C16 C17 111.42(14) . . ?
C12 C16 C18 112.79(14) . . ?
C17 C16 C18 108.60(15) . . ?
C12 C16 H16 108.0 . . ?
C17 C16 H16 108.0 . . ?
C18 C16 H16 108.0 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C24 C19 C20 121.73(13) . . ?
C24 C19 N2 119.21(13) . . ?
C20 C19 N2 119.03(13) . . ?
C21 C20 C19 117.52(15) . . ?
C21 C20 C25A 121.5(4) . . ?
C19 C20 C25A 121.0(4) . . ?
C21 C20 C25B 114.9(6) . . ?
C19 C20 C25B 125.6(6) . . ?
C22 C21 C20 121.50(15) . . ?
C22 C21 H21 119.2 . . ?
C20 C21 H21 119.2 . . ?
C23 C22 C21 119.83(14) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C24 121.25(15) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 H23 119.4 . . ?
C23 C24 C19 118.14(14) . . ?
C23 C24 C28 120.03(14) . . ?
C19 C24 C28 121.75(13) . . ?
C20 C25A C26A 105.7(8) . . ?
C20 C25A C27A 115.0(6) . . ?
C26A C25A C27A 107.7(8) . . ?
C20 C25A H25A 109.4 . . ?
C26A C25A H25A 109.4 . . ?
C27A C25A H25A 109.4 . . ?
C25A C26A H26A 109.5 . . ?
C25A C26A H26B 109.5 . . ?
H26A C26A H26B 109.5 . . ?
C25A C26A H26C 109.5 . . ?
H26A C26A H26C 109.5 . . ?
H26B C26A H26C 109.5 . . ?
C25A C27A H27A 109.5 . . ?
C25A C27A H27B 109.5 . . ?
H27A C27A H27B 109.5 . . ?
C25A C27A H27C 109.5 . . ?
H27A C27A H27C 109.5 . . ?
H27B C27A H27C 109.5 . . ?
C27B C25B C26B 114(2) . . ?
C27B C25B C20 105.0(15) . . ?
C26B C25B C20 118.6(19) . . ?
C27B C25B H25B 105.9 . . ?
C26B C25B H25B 105.9 . . ?
C20 C25B H25B 105.9 . . ?
C25B C26B H26D 109.5 . . ?
C25B C26B H26E 109.5 . . ?
H26D C26B H26E 109.5 . . ?
C25B C26B H26F 109.5 . . ?
H26D C26B H26F 109.5 . . ?
H26E C26B H26F 109.5 . . ?
C25B C27B H27D 109.5 . . ?
C25B C27B H27E 109.5 . . ?
H27D C27B H27E 109.5 . . ?
C25B C27B H27F 109.5 . . ?
H27D C27B H27F 109.5 . . ?
H27E C27B H27F 109.5 . . ?
C30 C28 C24 113.43(16) . . ?
C30 C28 C29 107.22(17) . . ?
C24 C28 C29 108.67(17) . . ?
C30 C28 H28 109.1 . . ?
C24 C28 H28 109.1 . . ?
C29 C28 H28 109.1 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C36 C31 C32 117.72(13) . . ?
C36 C31 P1 121.50(11) . . ?
C32 C31 P1 120.77(11) . . ?
C33 C32 C31 118.68(14) . . ?
C33 C32 C37 116.06(14) . . ?
C31 C32 C37 125.21(14) . . ?
C34 C33 C32 123.71(15) . . ?
C34 C33 H33 118.1 . . ?
C32 C33 H33 118.1 . . ?
C35 C34 C33 116.87(14) . . ?
C35 C34 C41 122.90(16) . . ?
C33 C34 C41 120.07(15) . . ?
C34 C35 C36 123.45(15) . . ?
C34 C35 H35 118.3 . . ?
C36 C35 H35 118.3 . . ?
C35 C36 C31 118.94(14) . . ?
C35 C36 C45 115.55(14) . . ?
C31 C36 C45 125.47(13) . . ?
C40 C37 C39 112.09(15) . . ?
C40 C37 C38 104.92(15) . . ?
C39 C37 C38 105.07(15) . . ?
C40 C37 C32 111.41(13) . . ?
C39 C37 C32 110.40(13) . . ?
C38 C37 C32 112.69(15) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C44 C41 C34 112.55(16) . . ?
C44 C41 C42 108.37(17) . . ?
C34 C41 C42 109.92(15) . . ?
C44 C41 C43 109.10(17) . . ?
C34 C41 C43 107.70(14) . . ?
C42 C41 C43 109.16(17) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C47 C45 C46 104.77(14) . . ?
C47 C45 C48 113.31(14) . . ?
C46 C45 C48 104.38(15) . . ?
C47 C45 C36 111.46(13) . . ?
C46 C45 C36 112.49(14) . . ?
C48 C45 C36 110.14(13) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 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
C2 N1 C1 C4 178.78(16) . . . . ?
C7 N1 C1 C4 -2.6(2) . . . . ?
C2 N1 C1 N2 -2.13(16) . . . . ?
C7 N1 C1 N2 176.52(13) . . . . ?
C3 N2 C1 C4 -179.08(15) . . . . ?
C19 N2 C1 C4 -9.4(2) . . . . ?
C3 N2 C1 N1 1.77(15) . . . . ?
C19 N2 C1 N1 171.42(13) . . . . ?
C1 N1 C2 C3 1.75(18) . . . . ?
C7 N1 C2 C3 -176.93(14) . . . . ?
C1 N1 C2 C5 -178.43(15) . . . . ?
C7 N1 C2 C5 2.9(2) . . . . ?
N1 C2 C3 N2 -0.57(18) . . . . ?
C5 C2 C3 N2 179.63(18) . . . . ?
N1 C2 C3 C6 176.67(16) . . . . ?
C5 C2 C3 C6 -3.1(3) . . . . ?
C1 N2 C3 C2 -0.78(17) . . . . ?
C19 N2 C3 C2 -170.36(14) . . . . ?
C1 N2 C3 C6 -178.30(14) . . . . ?
C19 N2 C3 C6 12.1(2) . . . . ?
N1 C1 C4 P1 -4.3(2) . . . . ?
N2 C1 C4 P1 176.76(11) . . . . ?
C31 P1 C4 C1 179.91(14) . . . . ?
C1 N1 C7 C12 -80.58(19) . . . . ?
C2 N1 C7 C12 97.89(17) . . . . ?
C1 N1 C7 C8 100.21(17) . . . . ?
C2 N1 C7 C8 -81.31(19) . . . . ?
C12 C7 C8 C9 2.9(2) . . . . ?
N1 C7 C8 C9 -177.90(14) . . . . ?
C12 C7 C8 C13 -177.84(15) . . . . ?
N1 C7 C8 C13 1.3(2) . . . . ?
C7 C8 C9 C10 -0.3(3) . . . . ?
C13 C8 C9 C10 -179.52(17) . . . . ?
C8 C9 C10 C11 -2.2(3) . . . . ?
C9 C10 C11 C12 2.1(3) . . . . ?
C10 C11 C12 C7 0.5(2) . . . . ?
C10 C11 C12 C16 179.68(15) . . . . ?
C8 C7 C12 C11 -3.0(2) . . . . ?
N1 C7 C12 C11 177.80(13) . . . . ?
C8 C7 C12 C16 177.78(14) . . . . ?
N1 C7 C12 C16 -1.4(2) . . . . ?
C9 C8 C13 C14 69.1(2) . . . . ?
C7 C8 C13 C14 -110.07(19) . . . . ?
C9 C8 C13 C15 -53.1(2) . . . . ?
C7 C8 C13 C15 127.67(18) . . . . ?
C11 C12 C16 C17 103.83(18) . . . . ?
C7 C12 C16 C17 -77.01(19) . . . . ?
C11 C12 C16 C18 -18.6(2) . . . . ?
C7 C12 C16 C18 160.55(15) . . . . ?
C1 N2 C19 C24 84.35(18) . . . . ?
C3 N2 C19 C24 -107.44(17) . . . . ?
C1 N2 C19 C20 -97.47(17) . . . . ?
C3 N2 C19 C20 70.7(2) . . . . ?
C24 C19 C20 C21 -0.3(2) . . . . ?
N2 C19 C20 C21 -178.42(14) . . . . ?
C24 C19 C20 C25A 177.6(4) . . . . ?
N2 C19 C20 C25A -0.5(4) . . . . ?
C24 C19 C20 C25B -163.3(14) . . . . ?
N2 C19 C20 C25B 18.6(14) . . . . ?
C19 C20 C21 C22 -1.0(3) . . . . ?
C25A C20 C21 C22 -178.9(4) . . . . ?
C25B C20 C21 C22 163.8(13) . . . . ?
C20 C21 C22 C23 1.0(3) . . . . ?
C21 C22 C23 C24 0.5(3) . . . . ?
C22 C23 C24 C19 -1.8(2) . . . . ?
C22 C23 C24 C28 175.06(16) . . . . ?
C20 C19 C24 C23 1.7(2) . . . . ?
N2 C19 C24 C23 179.79(13) . . . . ?
C20 C19 C24 C28 -175.10(16) . . . . ?
N2 C19 C24 C28 3.0(2) . . . . ?
C21 C20 C25A C26A -70.2(8) . . . . ?
C19 C20 C25A C26A 112.0(6) . . . . ?
C21 C20 C25A C27A 48.5(9) . . . . ?
C19 C20 C25A C27A -129.3(6) . . . . ?
C21 C20 C25B C27B 79(2) . . . . ?
C19 C20 C25B C27B -117.2(14) . . . . ?
C21 C20 C25B C26B -50(2) . . . . ?
C19 C20 C25B C26B 113.4(16) . . . . ?
C23 C24 C28 C30 46.1(2) . . . . ?
C19 C24 C28 C30 -137.20(17) . . . . ?
C23 C24 C28 C29 -73.1(2) . . . . ?
C19 C24 C28 C29 103.66(19) . . . . ?
C4 P1 C31 C36 -92.68(12) . . . . ?
C4 P1 C31 C32 88.42(12) . . . . ?
C36 C31 C32 C33 8.3(2) . . . . ?
P1 C31 C32 C33 -172.74(11) . . . . ?
C36 C31 C32 C37 -168.87(13) . . . . ?
P1 C31 C32 C37 10.1(2) . . . . ?
C31 C32 C33 C34 -2.5(2) . . . . ?
C37 C32 C33 C34 174.94(14) . . . . ?
C32 C33 C34 C35 -3.5(2) . . . . ?
C32 C33 C34 C41 -178.94(14) . . . . ?
C33 C34 C35 C36 3.5(2) . . . . ?
C41 C34 C35 C36 178.87(14) . . . . ?
C34 C35 C36 C31 2.4(2) . . . . ?
C34 C35 C36 C45 -175.40(13) . . . . ?
C32 C31 C36 C35 -8.27(19) . . . . ?
P1 C31 C36 C35 172.80(10) . . . . ?
C32 C31 C36 C45 169.28(13) . . . . ?
P1 C31 C36 C45 -9.65(19) . . . . ?
C33 C32 C37 C40 115.61(16) . . . . ?
C31 C32 C37 C40 -67.14(19) . . . . ?
C33 C32 C37 C39 -119.17(16) . . . . ?
C31 C32 C37 C39 58.1(2) . . . . ?
C33 C32 C37 C38 -2.0(2) . . . . ?
C31 C32 C37 C38 175.22(15) . . . . ?
C35 C34 C41 C44 11.3(2) . . . . ?
C33 C34 C41 C44 -173.51(16) . . . . ?
C35 C34 C41 C42 132.19(18) . . . . ?
C33 C34 C41 C42 -52.6(2) . . . . ?
C35 C34 C41 C43 -108.99(19) . . . . ?
C33 C34 C41 C43 66.2(2) . . . . ?
C35 C36 C45 C47 -114.52(15) . . . . ?
C31 C36 C45 C47 67.85(19) . . . . ?
C35 C36 C45 C46 2.83(19) . . . . ?
C31 C36 C45 C46 -174.80(15) . . . . ?
C35 C36 C45 C48 118.82(15) . . . . ?
C31 C36 C45 C48 -58.81(19) . . . . ?

_refine_diff_density_max         1.038
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.049

####################################################################### 
# 
# 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_ax1821_MesStarPHCHIDip_cmp13
_database_code_depnum_ccdc_archive 'CCDC 2046863'
loop_
_audit_author_name
_audit_author_address
'Hering-Junghans C.'
;LIKAT Rostock
Germany
;
_audit_update_record             
;
2020-11-27 deposited with the CCDC.	2021-01-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H67 N2 P, C6 H14'
_chemical_formula_sum            'C52 H81 N2 P'
_chemical_formula_weight         751.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.9777(3)
_cell_length_b                   17.4497(3)
_cell_length_c                   19.3800(4)
_cell_angle_alpha                90
_cell_angle_beta                 106.6127(10)
_cell_angle_gamma                90
_cell_volume                     4853.66(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7734
_cell_measurement_theta_min      3.31
_cell_measurement_theta_max      66.57

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.047
_exptl_crystal_F_000             1688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.738
_shelx_estimated_absorpt_T_min   0.891
_shelx_estimated_absorpt_T_max   0.964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.891
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?

#==============================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         microfocus
_diffrn_radiation_monochromator  multilayer
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33300
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.310
_diffrn_reflns_theta_max         66.670
_diffrn_reflns_theta_full        66.670
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8557
_reflns_number_gt                7106
_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.
 
 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.
;

_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms 
 were positioned geometrically and refined using a riding model, with C---H = 
 0.98 (methyl groups), 0.99Å (methylene groups), 1.00Å (methine groups) or 
 0.95 Å (aryl CH) and with Uiso(H) = 1.5 times Ueq(C) 
 (methyl groups) or with Uiso(H) = 1.2 times Ueq(C) 
 (methylene  groups, aryl CH, methine groups). Torsion angles of all methyl 
 groups were allowed to refine.
 
 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 > 2σ(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.
 
 loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.075  0.250  0.444       498        96 ' '
   2 -0.045  0.750  0.437       499        96 ' '
   3  0.056  0.530  0.015        11         0 ' '
   4  0.443  0.030  0.485        10         0 ' '
   5  0.569  0.964  0.518         9         0 ' '
   6  0.931  0.464  0.982         8         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           
The unit cell contains four disordered n-hexane molecules. These 
have been treated as a diffuse contribution to the overall scattering 
without specific atom positions by SQUEEZE/PLATON.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0730P)²+2.1990P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8557
_refine_ls_number_parameters     467
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0514
_refine_ls_wR_factor_ref         0.1458
_refine_ls_wR_factor_gt          0.1363
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.68808(3) 0.23826(3) 0.76133(2) 0.02868(13) Uani 1 1 d . . . . .
N1 N 0.77306(10) 0.41093(8) 0.73862(7) 0.0247(3) Uani 1 1 d . . . . .
N2 N 0.66781(10) 0.47441(8) 0.77434(7) 0.0249(3) Uani 1 1 d . . . . .
C1 C 0.69430(11) 0.40034(10) 0.76207(8) 0.0229(3) Uani 1 1 d . . . . .
C2 C 0.79145(12) 0.48946(10) 0.73568(9) 0.0293(4) Uani 1 1 d . . . . .
H2 H 0.8413 0.5114 0.7212 0.035 Uiso 1 1 calc R U . . .
C3 C 0.72737(12) 0.52791(10) 0.75663(9) 0.0277(4) Uani 1 1 d . . . . .
H3 H 0.7227 0.5821 0.7592 0.033 Uiso 1 1 calc R U . . .
C4 C 0.65066(12) 0.33459(10) 0.77172(10) 0.0307(4) Uani 1 1 d . . . . .
H4 H 0.5948 0.3400 0.7853 0.037 Uiso 1 1 calc R U . . .
C5 C 0.82810(11) 0.35101(9) 0.72068(9) 0.0248(3) Uani 1 1 d . . . . .
C6 C 0.90713(13) 0.32493(11) 0.77319(10) 0.0333(4) Uani 1 1 d . . . . .
C7 C 0.95751(15) 0.26488(12) 0.75510(11) 0.0428(5) Uani 1 1 d . . . . .
H7 H 1.0116 0.2462 0.7898 0.051 Uiso 1 1 calc R U . . .
C8 C 0.93023(16) 0.23225(12) 0.68791(12) 0.0451(5) Uani 1 1 d . . . . .
H8 H 0.9642 0.1902 0.6771 0.054 Uiso 1 1 calc R U . . .
C9 C 0.85397(15) 0.26005(12) 0.63599(11) 0.0423(5) Uani 1 1 d . . . . .
H9 H 0.8368 0.2377 0.5894 0.051 Uiso 1 1 calc R U . . .
C10 C 0.80163(12) 0.32055(11) 0.65084(9) 0.0309(4) Uani 1 1 d . . . . .
C11 C 0.93728(16) 0.36046(15) 0.84763(11) 0.0508(6) Uani 1 1 d . . . . .
H11 H 0.8853 0.3937 0.8532 0.061 Uiso 1 1 calc R U . . .
C12 C 0.9558(3) 0.2981(2) 0.90652(14) 0.0922(12) Uani 1 1 d . . . . .
H12A H 1.0120 0.2694 0.9066 0.138 Uiso 1 1 calc R U . . .
H12B H 0.9025 0.2631 0.8968 0.138 Uiso 1 1 calc R U . . .
H12C H 0.9645 0.3223 0.9536 0.138 Uiso 1 1 calc R U . . .
C13 C 1.0204(3) 0.4083(2) 0.85843(18) 0.1020(14) Uani 1 1 d . . . . .
H13A H 1.0745 0.3757 0.8610 0.153 Uiso 1 1 calc R U . . .
H13B H 1.0308 0.4372 0.9034 0.153 Uiso 1 1 calc R U . . .
H13C H 1.0114 0.4441 0.8181 0.153 Uiso 1 1 calc R U . . .
C14 C 0.71986(14) 0.35311(13) 0.59293(10) 0.0400(5) Uani 1 1 d . . . . .
H14 H 0.6748 0.3753 0.6169 0.048 Uiso 1 1 calc R U . . .
C15 C 0.7536(2) 0.41772(14) 0.55332(14) 0.0633(7) Uani 1 1 d . . . . .
H15A H 0.7865 0.4563 0.5882 0.095 Uiso 1 1 calc R U . . .
H15B H 0.7000 0.4415 0.5187 0.095 Uiso 1 1 calc R U . . .
H15C H 0.7959 0.3968 0.5278 0.095 Uiso 1 1 calc R U . . .
C16 C 0.66821(18) 0.29372(15) 0.53806(11) 0.0549(6) Uani 1 1 d . . . . .
H16A H 0.7078 0.2776 0.5083 0.082 Uiso 1 1 calc R U . . .
H16B H 0.6106 0.3163 0.5073 0.082 Uiso 1 1 calc R U . . .
H16C H 0.6531 0.2492 0.5634 0.082 Uiso 1 1 calc R U . . .
C17 C 0.58524(12) 0.49347(10) 0.79419(9) 0.0268(4) Uani 1 1 d . . . . .
C18 C 0.59000(13) 0.49907(11) 0.86719(10) 0.0324(4) Uani 1 1 d . . . . .
C19 C 0.50946(15) 0.52084(13) 0.88453(12) 0.0437(5) Uani 1 1 d . . . . .
H19 H 0.5108 0.5254 0.9337 0.052 Uiso 1 1 calc R U . . .
C20 C 0.42792(15) 0.53590(14) 0.83141(13) 0.0487(5) Uani 1 1 d . . . . .
H20 H 0.3739 0.5513 0.8442 0.058 Uiso 1 1 calc R U . . .
C21 C 0.42438(14) 0.52870(14) 0.75991(12) 0.0457(5) Uani 1 1 d . . . . .
H21 H 0.3675 0.5386 0.7239 0.055 Uiso 1 1 calc R U . . .
C22 C 0.50278(13) 0.50706(11) 0.73954(10) 0.0340(4) Uani 1 1 d . . . . .
C23 C 0.68030(14) 0.48435(13) 0.92566(10) 0.0396(5) Uani 1 1 d . . . . .
H23 H 0.7165 0.4454 0.9070 0.047 Uiso 1 1 calc R U . . .
C24 C 0.66502(17) 0.45254(14) 0.99508(11) 0.0496(5) Uani 1 1 d . . . . .
H24A H 0.6393 0.4929 1.0190 0.074 Uiso 1 1 calc R U . . .
H24B H 0.7246 0.4350 1.0272 0.074 Uiso 1 1 calc R U . . .
H24C H 0.6213 0.4094 0.9834 0.074 Uiso 1 1 calc R U . . .
C25 C 0.73866(17) 0.55651(18) 0.94235(12) 0.0621(7) Uani 1 1 d . . . . .
H25A H 0.7476 0.5772 0.8978 0.093 Uiso 1 1 calc R U . . .
H25B H 0.7994 0.5445 0.9761 0.093 Uiso 1 1 calc R U . . .
H25C H 0.7068 0.5946 0.9640 0.093 Uiso 1 1 calc R U . . .
C26 C 0.49793(14) 0.50077(13) 0.66051(11) 0.0444(5) Uani 1 1 d . . . . .
H26 H 0.5559 0.4747 0.6571 0.053 Uiso 1 1 calc R U . . .
C27 C 0.4146(2) 0.45332(15) 0.61800(14) 0.0664(8) Uani 1 1 d . . . . .
H27A H 0.4136 0.4044 0.6427 0.100 Uiso 1 1 calc R U . . .
H27B H 0.4199 0.4436 0.5695 0.100 Uiso 1 1 calc R U . . .
H27C H 0.3569 0.4815 0.6146 0.100 Uiso 1 1 calc R U . . .
C28 C 0.49472(18) 0.58015(16) 0.62711(12) 0.0579(6) Uani 1 1 d . . . . .
H28A H 0.4374 0.6063 0.6286 0.087 Uiso 1 1 calc R U . . .
H28B H 0.4959 0.5752 0.5770 0.087 Uiso 1 1 calc R U . . .
H28C H 0.5488 0.6100 0.6543 0.087 Uiso 1 1 calc R U . . .
C29 C 0.60239(12) 0.17506(9) 0.78738(9) 0.0263(4) Uani 1 1 d . . . . .
C30 C 0.52341(12) 0.14522(10) 0.73361(9) 0.0274(4) Uani 1 1 d . . . . .
C31 C 0.46538(12) 0.09250(10) 0.75425(9) 0.0297(4) Uani 1 1 d . . . . .
H31 H 0.4126 0.0737 0.7184 0.036 Uiso 1 1 calc R U . . .
C32 C 0.48069(12) 0.06646(10) 0.82377(10) 0.0300(4) Uani 1 1 d . . . . .
C33 C 0.55804(13) 0.09525(10) 0.87514(9) 0.0310(4) Uani 1 1 d . . . . .
H33 H 0.5699 0.0777 0.9233 0.037 Uiso 1 1 calc R U . . .
C34 C 0.61918(12) 0.14845(10) 0.86007(9) 0.0285(4) Uani 1 1 d . . . . .
C35 C 0.49687(13) 0.16322(11) 0.65139(10) 0.0320(4) Uani 1 1 d . . . . .
C36 C 0.40165(14) 0.12913(13) 0.60981(11) 0.0423(5) Uani 1 1 d . . . . .
H36A H 0.3538 0.1472 0.6314 0.063 Uiso 1 1 calc R U . . .
H36B H 0.4050 0.0731 0.6122 0.063 Uiso 1 1 calc R U . . .
H36C H 0.3857 0.1455 0.5594 0.063 Uiso 1 1 calc R U . . .
C37 C 0.48601(15) 0.24986(11) 0.63570(11) 0.0394(5) Uani 1 1 d . . . . .
H37A H 0.4672 0.2583 0.5835 0.059 Uiso 1 1 calc R U . . .
H37B H 0.5456 0.2756 0.6575 0.059 Uiso 1 1 calc R U . . .
H37C H 0.4384 0.2708 0.6561 0.059 Uiso 1 1 calc R U . . .
C38 C 0.56745(15) 0.12514(12) 0.61776(10) 0.0396(5) Uani 1 1 d . . . . .
H38A H 0.5679 0.0697 0.6257 0.059 Uiso 1 1 calc R U . . .
H38B H 0.6298 0.1459 0.6403 0.059 Uiso 1 1 calc R U . . .
H38C H 0.5496 0.1356 0.5659 0.059 Uiso 1 1 calc R U . . .
C39 C 0.41654(13) 0.00840(12) 0.84514(11) 0.0362(4) Uani 1 1 d . . . . .
C40 C 0.33443(15) -0.01513(15) 0.78138(13) 0.0518(6) Uani 1 1 d . . . . .
H40A H 0.2993 0.0306 0.7600 0.078 Uiso 1 1 calc R U . . .
H40B H 0.2936 -0.0499 0.7981 0.078 Uiso 1 1 calc R U . . .
H40C H 0.3578 -0.0411 0.7452 0.078 Uiso 1 1 calc R U . . .
C41 C 0.37656(18) 0.04498(15) 0.90207(14) 0.0557(6) Uani 1 1 d . . . . .
H41A H 0.4277 0.0587 0.9445 0.084 Uiso 1 1 calc R U . . .
H41B H 0.3351 0.0084 0.9159 0.084 Uiso 1 1 calc R U . . .
H41C H 0.3414 0.0912 0.8821 0.084 Uiso 1 1 calc R U . . .
C42 C 0.47211(16) -0.06363(13) 0.87558(13) 0.0499(5) Uani 1 1 d . . . . .
H42A H 0.4964 -0.0869 0.8386 0.075 Uiso 1 1 calc R U . . .
H42B H 0.4314 -0.1003 0.8902 0.075 Uiso 1 1 calc R U . . .
H42C H 0.5241 -0.0498 0.9174 0.075 Uiso 1 1 calc R U . . .
C43 C 0.70250(13) 0.17264(11) 0.92544(10) 0.0332(4) Uani 1 1 d . . . . .
C44 C 0.70943(15) 0.26010(11) 0.93525(11) 0.0397(5) Uani 1 1 d . . . . .
H44A H 0.7589 0.2724 0.9792 0.060 Uiso 1 1 calc R U . . .
H44B H 0.6499 0.2802 0.9391 0.060 Uiso 1 1 calc R U . . .
H44C H 0.7239 0.2834 0.8937 0.060 Uiso 1 1 calc R U . . .
C45 C 0.79440(14) 0.13767(13) 0.91903(12) 0.0451(5) Uani 1 1 d . . . . .
H45A H 0.8067 0.1563 0.8749 0.068 Uiso 1 1 calc R U . . .
H45B H 0.7892 0.0817 0.9173 0.068 Uiso 1 1 calc R U . . .
H45C H 0.8457 0.1528 0.9608 0.068 Uiso 1 1 calc R U . . .
C46 C 0.69257(17) 0.14194(13) 0.99749(11) 0.0482(5) Uani 1 1 d . . . . .
H46A H 0.7455 0.1594 1.0370 0.072 Uiso 1 1 calc R U . . .
H46B H 0.6914 0.0858 0.9964 0.072 Uiso 1 1 calc R U . . .
H46C H 0.6345 0.1611 1.0049 0.072 Uiso 1 1 calc R U . . .
H1A H 0.762(2) 0.2266(18) 0.8135(17) 0.012(8) Uiso 0.5 1 d . . P . .
H1B H 0.670(2) 0.2265(18) 0.6954(16) 0.010(7) Uiso 0.5 1 d . . P . .


#==============================================================================

# MOLECULAR GEOMETRY

_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 C4 1.8013(18) . ?
P1 C29 1.8679(17) . ?
P1 H1A 1.28(3) . ?
P1 H1B 1.24(3) . ?
N1 C1 1.392(2) . ?
N1 C2 1.402(2) . ?
N1 C5 1.434(2) . ?
N2 C1 1.392(2) . ?
N2 C3 1.400(2) . ?
N2 C17 1.435(2) . ?
C1 C4 1.360(2) . ?
C2 C3 1.326(3) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 C6 1.398(2) . ?
C5 C10 1.402(2) . ?
C6 C7 1.393(3) . ?
C6 C11 1.516(3) . ?
C7 C8 1.372(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.377(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.393(3) . ?
C9 H9 0.9500 . ?
C10 C14 1.515(3) . ?
C11 C13 1.463(4) . ?
C11 C12 1.543(4) . ?
C11 H11 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C16 1.527(3) . ?
C14 C15 1.529(3) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C22 1.398(2) . ?
C17 C18 1.399(3) . ?
C18 C19 1.394(3) . ?
C18 C23 1.518(3) . ?
C19 C20 1.379(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.377(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.394(3) . ?
C21 H21 0.9500 . ?
C22 C26 1.517(3) . ?
C23 C25 1.514(3) . ?
C23 C24 1.532(3) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C28 1.524(3) . ?
C26 C27 1.527(3) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.432(2) . ?
C29 C34 1.435(2) . ?
C30 C31 1.400(2) . ?
C30 C35 1.560(2) . ?
C31 C32 1.377(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.388(3) . ?
C32 C39 1.533(2) . ?
C33 C34 1.392(3) . ?
C33 H33 0.9500 . ?
C34 C43 1.561(2) . ?
C35 C37 1.541(3) . ?
C35 C38 1.542(3) . ?
C35 C36 1.543(3) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.529(3) . ?
C39 C42 1.530(3) . ?
C39 C41 1.537(3) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.538(3) . ?
C43 C46 1.542(3) . ?
C43 C45 1.543(3) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 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
C4 P1 C29 105.12(8) . . ?
C4 P1 H1A 106.6(14) . . ?
C29 P1 H1A 101.2(14) . . ?
C4 P1 H1B 106.5(15) . . ?
C29 P1 H1B 102.4(15) . . ?
H1A P1 H1B 132(2) . . ?
C1 N1 C2 109.73(14) . . ?
C1 N1 C5 125.56(14) . . ?
C2 N1 C5 124.71(14) . . ?
C1 N2 C3 110.14(14) . . ?
C1 N2 C17 124.78(14) . . ?
C3 N2 C17 124.71(14) . . ?
C4 C1 N2 126.03(15) . . ?
C4 C1 N1 129.97(16) . . ?
N2 C1 N1 104.01(14) . . ?
C3 C2 N1 108.31(15) . . ?
C3 C2 H2 125.8 . . ?
N1 C2 H2 125.8 . . ?
C2 C3 N2 107.78(15) . . ?
C2 C3 H3 126.1 . . ?
N2 C3 H3 126.1 . . ?
C1 C4 P1 126.51(14) . . ?
C1 C4 H4 116.7 . . ?
P1 C4 H4 116.7 . . ?
C6 C5 C10 121.75(16) . . ?
C6 C5 N1 119.11(15) . . ?
C10 C5 N1 119.14(15) . . ?
C7 C6 C5 117.93(17) . . ?
C7 C6 C11 120.78(18) . . ?
C5 C6 C11 121.30(17) . . ?
C8 C7 C6 121.00(19) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C7 C8 C9 120.48(19) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C8 C9 C10 120.95(18) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
C9 C10 C5 117.79(17) . . ?
C9 C10 C14 120.97(17) . . ?
C5 C10 C14 121.24(16) . . ?
C13 C11 C6 112.3(2) . . ?
C13 C11 C12 109.3(2) . . ?
C6 C11 C12 110.9(2) . . ?
C13 C11 H11 108.0 . . ?
C6 C11 H11 108.0 . . ?
C12 C11 H11 108.0 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 C16 113.73(19) . . ?
C10 C14 C15 109.59(17) . . ?
C16 C14 C15 108.97(18) . . ?
C10 C14 H14 108.1 . . ?
C16 C14 H14 108.1 . . ?
C15 C14 H14 108.1 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C22 C17 C18 122.17(16) . . ?
C22 C17 N2 118.58(16) . . ?
C18 C17 N2 119.23(15) . . ?
C19 C18 C17 117.72(17) . . ?
C19 C18 C23 120.92(17) . . ?
C17 C18 C23 121.33(16) . . ?
C20 C19 C18 120.96(19) . . ?
C20 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
C21 C20 C19 120.33(19) . . ?
C21 C20 H20 119.8 . . ?
C19 C20 H20 119.8 . . ?
C20 C21 C22 121.09(19) . . ?
C20 C21 H21 119.5 . . ?
C22 C21 H21 119.5 . . ?
C21 C22 C17 117.69(18) . . ?
C21 C22 C26 120.31(17) . . ?
C17 C22 C26 121.98(17) . . ?
C25 C23 C18 110.83(18) . . ?
C25 C23 C24 109.62(18) . . ?
C18 C23 C24 113.09(17) . . ?
C25 C23 H23 107.7 . . ?
C18 C23 H23 107.7 . . ?
C24 C23 H23 107.7 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C26 C28 110.48(18) . . ?
C22 C26 C27 112.3(2) . . ?
C28 C26 C27 110.00(18) . . ?
C22 C26 H26 108.0 . . ?
C28 C26 H26 108.0 . . ?
C27 C26 H26 108.0 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C34 118.23(15) . . ?
C30 C29 P1 120.42(13) . . ?
C34 C29 P1 121.00(13) . . ?
C31 C30 C29 118.81(15) . . ?
C31 C30 C35 115.24(15) . . ?
C29 C30 C35 125.89(15) . . ?
C32 C31 C30 123.55(16) . . ?
C32 C31 H31 118.2 . . ?
C30 C31 H31 118.2 . . ?
C31 C32 C33 116.98(16) . . ?
C31 C32 C39 122.71(16) . . ?
C33 C32 C39 120.30(16) . . ?
C32 C33 C34 123.71(16) . . ?
C32 C33 H33 118.1 . . ?
C34 C33 H33 118.1 . . ?
C33 C34 C29 118.70(16) . . ?
C33 C34 C43 115.54(15) . . ?
C29 C34 C43 125.74(15) . . ?
C37 C35 C38 112.68(16) . . ?
C37 C35 C36 104.21(15) . . ?
C38 C35 C36 104.84(16) . . ?
C37 C35 C30 112.38(15) . . ?
C38 C35 C30 109.85(14) . . ?
C36 C35 C30 112.55(15) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 C42 108.30(19) . . ?
C40 C39 C32 112.37(16) . . ?
C42 C39 C32 109.48(16) . . ?
C40 C39 C41 107.65(18) . . ?
C42 C39 C41 110.20(18) . . ?
C32 C39 C41 108.82(17) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 C46 104.68(16) . . ?
C44 C43 C45 111.85(17) . . ?
C46 C43 C45 104.76(17) . . ?
C44 C43 C34 112.26(15) . . ?
C46 C43 C34 112.29(16) . . ?
C45 C43 C34 110.63(15) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 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
C3 N2 C1 C4 -178.28(16) . . . . ?
C17 N2 C1 C4 -5.0(3) . . . . ?
C3 N2 C1 N1 1.76(17) . . . . ?
C17 N2 C1 N1 175.06(14) . . . . ?
C2 N1 C1 C4 178.83(17) . . . . ?
C5 N1 C1 C4 -1.7(3) . . . . ?
C2 N1 C1 N2 -1.21(17) . . . . ?
C5 N1 C1 N2 178.26(14) . . . . ?
C1 N1 C2 C3 0.2(2) . . . . ?
C5 N1 C2 C3 -179.26(15) . . . . ?
N1 C2 C3 N2 0.89(19) . . . . ?
C1 N2 C3 C2 -1.71(19) . . . . ?
C17 N2 C3 C2 -175.01(15) . . . . ?
N2 C1 C4 P1 -175.95(13) . . . . ?
N1 C1 C4 P1 4.0(3) . . . . ?
C29 P1 C4 C1 176.76(16) . . . . ?
C1 N1 C5 C6 -94.6(2) . . . . ?
C2 N1 C5 C6 84.8(2) . . . . ?
C1 N1 C5 C10 85.9(2) . . . . ?
C2 N1 C5 C10 -94.7(2) . . . . ?
C10 C5 C6 C7 -2.7(3) . . . . ?
N1 C5 C6 C7 177.82(17) . . . . ?
C10 C5 C6 C11 177.51(19) . . . . ?
N1 C5 C6 C11 -2.0(3) . . . . ?
C5 C6 C7 C8 -0.2(3) . . . . ?
C11 C6 C7 C8 179.7(2) . . . . ?
C6 C7 C8 C9 2.2(3) . . . . ?
C7 C8 C9 C10 -1.5(3) . . . . ?
C8 C9 C10 C5 -1.3(3) . . . . ?
C8 C9 C10 C14 177.7(2) . . . . ?
C6 C5 C10 C9 3.4(3) . . . . ?
N1 C5 C10 C9 -177.13(16) . . . . ?
C6 C5 C10 C14 -175.60(17) . . . . ?
N1 C5 C10 C14 3.9(3) . . . . ?
C7 C6 C11 C13 73.3(3) . . . . ?
C5 C6 C11 C13 -106.9(3) . . . . ?
C7 C6 C11 C12 -49.4(3) . . . . ?
C5 C6 C11 C12 130.4(2) . . . . ?
C9 C10 C14 C16 32.5(3) . . . . ?
C5 C10 C14 C16 -148.58(18) . . . . ?
C9 C10 C14 C15 -89.7(2) . . . . ?
C5 C10 C14 C15 89.2(2) . . . . ?
C1 N2 C17 C22 -89.1(2) . . . . ?
C3 N2 C17 C22 83.3(2) . . . . ?
C1 N2 C17 C18 92.0(2) . . . . ?
C3 N2 C17 C18 -95.7(2) . . . . ?
C22 C17 C18 C19 -1.6(3) . . . . ?
N2 C17 C18 C19 177.36(17) . . . . ?
C22 C17 C18 C23 -179.78(18) . . . . ?
N2 C17 C18 C23 -0.8(3) . . . . ?
C17 C18 C19 C20 0.3(3) . . . . ?
C23 C18 C19 C20 178.5(2) . . . . ?
C18 C19 C20 C21 0.8(4) . . . . ?
C19 C20 C21 C22 -0.8(4) . . . . ?
C20 C21 C22 C17 -0.4(3) . . . . ?
C20 C21 C22 C26 -178.9(2) . . . . ?
C18 C17 C22 C21 1.6(3) . . . . ?
N2 C17 C22 C21 -177.30(17) . . . . ?
C18 C17 C22 C26 -179.89(18) . . . . ?
N2 C17 C22 C26 1.2(3) . . . . ?
C19 C18 C23 C25 -91.8(2) . . . . ?
C17 C18 C23 C25 86.3(2) . . . . ?
C19 C18 C23 C24 31.7(3) . . . . ?
C17 C18 C23 C24 -150.14(19) . . . . ?
C21 C22 C26 C28 73.5(3) . . . . ?
C17 C22 C26 C28 -104.9(2) . . . . ?
C21 C22 C26 C27 -49.7(3) . . . . ?
C17 C22 C26 C27 131.9(2) . . . . ?
C4 P1 C29 C30 94.81(15) . . . . ?
C4 P1 C29 C34 -92.12(15) . . . . ?
C34 C29 C30 C31 0.9(2) . . . . ?
P1 C29 C30 C31 174.21(13) . . . . ?
C34 C29 C30 C35 -176.19(16) . . . . ?
P1 C29 C30 C35 -2.9(2) . . . . ?
C29 C30 C31 C32 -1.0(3) . . . . ?
C35 C30 C31 C32 176.41(17) . . . . ?
C30 C31 C32 C33 0.3(3) . . . . ?
C30 C31 C32 C39 -179.68(17) . . . . ?
C31 C32 C33 C34 0.4(3) . . . . ?
C39 C32 C33 C34 -179.55(17) . . . . ?
C32 C33 C34 C29 -0.5(3) . . . . ?
C32 C33 C34 C43 -179.30(17) . . . . ?
C30 C29 C34 C33 -0.2(2) . . . . ?
P1 C29 C34 C33 -173.46(13) . . . . ?
C30 C29 C34 C43 178.45(16) . . . . ?
P1 C29 C34 C43 5.2(2) . . . . ?
C31 C30 C35 C37 126.65(18) . . . . ?
C29 C30 C35 C37 -56.1(2) . . . . ?
C31 C30 C35 C38 -107.05(18) . . . . ?
C29 C30 C35 C38 70.2(2) . . . . ?
C31 C30 C35 C36 9.4(2) . . . . ?
C29 C30 C35 C36 -173.40(17) . . . . ?
C31 C32 C39 C40 -1.1(3) . . . . ?
C33 C32 C39 C40 178.89(18) . . . . ?
C31 C32 C39 C42 119.3(2) . . . . ?
C33 C32 C39 C42 -60.7(2) . . . . ?
C31 C32 C39 C41 -120.2(2) . . . . ?
C33 C32 C39 C41 59.8(2) . . . . ?
C33 C34 C43 C44 -126.59(18) . . . . ?
C29 C34 C43 C44 54.7(2) . . . . ?
C33 C34 C43 C46 -9.0(2) . . . . ?
C29 C34 C43 C46 172.31(18) . . . . ?
C33 C34 C43 C45 107.69(19) . . . . ?
C29 C34 C43 C45 -71.0(2) . . . . ?

_refine_diff_density_max         1.073
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.044


####################################################################### 
# 
# 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_ax1864_TerPHCHIDip_cmp14
_database_code_depnum_ccdc_archive 'CCDC 2046864'
loop_
_audit_author_name
_audit_author_address
'Hering-Junghans C.'
;LIKAT Rostock
Germany
;
_audit_update_record             
;
2020-11-27 deposited with the CCDC.	2021-01-13 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H63 N2 P, C5 H12'
_chemical_formula_sum            'C57 H75 N2 P'
_chemical_formula_weight         819.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#==============================================================================

# CRYSTAL DATA

_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                   10.6116(3)
_cell_length_b                   10.7511(3)
_cell_length_c                   22.9820(6)
_cell_angle_alpha                83.9073(11)
_cell_angle_beta                 80.6522(11)
_cell_angle_gamma                67.6900(10)
_cell_volume                     2390.61(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9995
_cell_measurement_theta_min      3.90
_cell_measurement_theta_max      66.72

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_F_000             892
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.031
_exptl_absorpt_coefficient_mu    0.786
_shelx_estimated_absorpt_T_min   0.814
_shelx_estimated_absorpt_T_max   0.976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.814
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014)'

#==============================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         microfocus
_diffrn_radiation_monochromator  multilayer
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26537
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.950
_diffrn_reflns_theta_max         66.717
_diffrn_reflns_theta_full        66.717
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             8411
_reflns_number_gt                7420
_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.
 
 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.
;

_computing_data_collection       'Bruker Apex V7.51A'
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms 
 were positioned geometrically and refined using a riding model, with C---H = 
 0.98 (methyl groups), 0.99Å (methylene groups), 1.00Å (methine groups) or 
 0.95 Å (aryl CH) and with Uiso(H) = 1.5 times Ueq(C) 
 (methyl groups) or with Uiso(H) = 1.2 times Ueq(C) 
 (methylene  groups, aryl CH, methine groups). Torsion angles of all methyl 
 groups were allowed to refine.

 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 > 2σ(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.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 248 42 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The unit cell contains one disordered n-pentane molecule. This 
has been treated as a diffuse contribution to the overall scattering 
without specific atom positions by SQUEEZE/PLATON.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0655P)²+0.5068P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8411
_refine_ls_number_parameters     518
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0407
_refine_ls_wR_factor_ref         0.1168
_refine_ls_wR_factor_gt          0.1116
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.88884(3) 0.65903(3) 0.67856(2) 0.03033(10) Uani 1 1 d . . . . .
N1 N 0.53456(11) 0.79818(11) 0.79842(5) 0.0304(2) Uani 1 1 d . . . . .
N2 N 0.59240(11) 0.62729(11) 0.74172(5) 0.0305(2) Uani 1 1 d . . . . .
C1 C 0.63894(13) 0.72341(12) 0.75616(6) 0.0268(3) Uani 1 1 d . . . . .
C2 C 0.42951(14) 0.74682(15) 0.80893(6) 0.0349(3) Uani 1 1 d . . . . .
H2 H 0.3479 0.7794 0.8361 0.042 Uiso 1 1 calc R U . . .
C3 C 0.46379(14) 0.64471(15) 0.77436(6) 0.0358(3) Uani 1 1 d . . . . .
H3 H 0.4103 0.5923 0.7721 0.043 Uiso 1 1 calc R U . . .
C4 C 0.75533(13) 0.74723(13) 0.73516(6) 0.0283(3) Uani 1 1 d . . . . .
H4 H 0.7676 0.8180 0.7521 0.034 Uiso 1 1 calc R U . . .
C5 C 0.55225(13) 0.88462(14) 0.83682(6) 0.0319(3) Uani 1 1 d . . . . .
C6 C 0.59455(15) 0.83169(16) 0.89176(6) 0.0382(3) Uani 1 1 d . . . . .
C7 C 0.60578(19) 0.91966(18) 0.92918(7) 0.0486(4) Uani 1 1 d . . . . .
H7 H 0.6332 0.8870 0.9670 0.058 Uiso 1 1 calc R U . . .
C8 C 0.57766(19) 1.05356(18) 0.91224(7) 0.0510(4) Uani 1 1 d . . . . .
H8 H 0.5854 1.1121 0.9385 0.061 Uiso 1 1 calc R U . . .
C9 C 0.53829(17) 1.10293(16) 0.85734(7) 0.0445(4) Uani 1 1 d . . . . .
H9 H 0.5195 1.1952 0.8462 0.053 Uiso 1 1 calc R U . . .
C10 C 0.52581(14) 1.01928(14) 0.81819(6) 0.0361(3) Uani 1 1 d . . . . .
C11 C 0.62990(17) 0.68357(17) 0.91004(7) 0.0437(4) Uani 1 1 d . . . . .
H11 H 0.6129 0.6393 0.8776 0.052 Uiso 1 1 calc R U . . .
C12 C 0.7812(2) 0.61526(19) 0.91795(9) 0.0564(4) Uani 1 1 d . . . . .
H12A H 0.8381 0.6236 0.8808 0.085 Uiso 1 1 calc R U . . .
H12B H 0.8017 0.5198 0.9293 0.085 Uiso 1 1 calc R U . . .
H12C H 0.8012 0.6584 0.9489 0.085 Uiso 1 1 calc R U . . .
C13 C 0.5393(2) 0.6633(2) 0.96635(10) 0.0739(6) Uani 1 1 d . . . . .
H13A H 0.5552 0.7047 0.9991 0.111 Uiso 1 1 calc R U . . .
H13B H 0.5623 0.5668 0.9757 0.111 Uiso 1 1 calc R U . . .
H13C H 0.4425 0.7055 0.9603 0.111 Uiso 1 1 calc R U . . .
C14 C 0.48153(16) 1.07102(15) 0.75782(7) 0.0407(3) Uani 1 1 d . . . . .
H14 H 0.5217 0.9935 0.7314 0.049 Uiso 1 1 calc R U . . .
C15 C 0.32497(18) 1.11937(19) 0.76185(9) 0.0544(4) Uani 1 1 d . . . . .
H15A H 0.2950 1.0448 0.7767 0.082 Uiso 1 1 calc R U . . .
H15B H 0.2974 1.1510 0.7226 0.082 Uiso 1 1 calc R U . . .
H15C H 0.2823 1.1933 0.7888 0.082 Uiso 1 1 calc R U . . .
C16 C 0.53445(19) 1.18031(17) 0.72994(8) 0.0527(4) Uani 1 1 d . . . . .
H16A H 0.4941 1.2594 0.7541 0.079 Uiso 1 1 calc R U . . .
H16B H 0.5085 1.2056 0.6901 0.079 Uiso 1 1 calc R U . . .
H16C H 0.6348 1.1462 0.7277 0.079 Uiso 1 1 calc R U . . .
C17 C 0.66823(15) 0.51584(14) 0.70524(6) 0.0354(3) Uani 1 1 d . . . . .
C18 C 0.62601(17) 0.51599(18) 0.65040(7) 0.0457(4) Uani 1 1 d . . . . .
C19 C 0.6993(2) 0.4040(2) 0.61693(9) 0.0626(6) Uani 1 1 d . . . . .
H19 H 0.6726 0.3995 0.5799 0.075 Uiso 1 1 calc R U . . .
C20 C 0.8096(2) 0.2998(2) 0.63627(11) 0.0711(7) Uani 1 1 d . . . . .
H20 H 0.8597 0.2260 0.6119 0.085 Uiso 1 1 calc R U . . .
C21 C 0.8484(2) 0.30100(18) 0.69037(10) 0.0615(5) Uani 1 1 d . . . . .
H21 H 0.9245 0.2276 0.7030 0.074 Uiso 1 1 calc R U . . .
C22 C 0.77768(16) 0.40846(15) 0.72709(8) 0.0438(4) Uani 1 1 d . . . . .
C23 C 0.50799(18) 0.6350(2) 0.62862(7) 0.0517(4) Uani 1 1 d . . . . .
H23 H 0.4317 0.6608 0.6622 0.062 Uiso 1 1 calc R U . . .
C24 C 0.4506(3) 0.6047(3) 0.57698(9) 0.0832(8) Uani 1 1 d . . . . .
H24A H 0.5198 0.5891 0.5419 0.125 Uiso 1 1 calc R U . . .
H24B H 0.3677 0.6814 0.5687 0.125 Uiso 1 1 calc R U . . .
H24C H 0.4277 0.5243 0.5873 0.125 Uiso 1 1 calc R U . . .
C25 C 0.5493(2) 0.7569(2) 0.61080(9) 0.0694(6) Uani 1 1 d . . . . .
H25A H 0.5781 0.7822 0.6447 0.104 Uiso 1 1 calc R U . . .
H25B H 0.4707 0.8325 0.5978 0.104 Uiso 1 1 calc R U . . .
H25C H 0.6256 0.7341 0.5785 0.104 Uiso 1 1 calc R U . . .
C26 C 0.81208(17) 0.40627(16) 0.78864(8) 0.0467(4) Uani 1 1 d . . . . .
H26 H 0.7882 0.5016 0.7985 0.056 Uiso 1 1 calc R U . . .
C27 C 0.7232(2) 0.34723(19) 0.83348(9) 0.0581(5) Uani 1 1 d . . . . .
H27A H 0.6259 0.4007 0.8313 0.087 Uiso 1 1 calc R U . . .
H27B H 0.7438 0.3493 0.8734 0.087 Uiso 1 1 calc R U . . .
H27C H 0.7433 0.2540 0.8245 0.087 Uiso 1 1 calc R U . . .
C28 C 0.9638(2) 0.3299(2) 0.79477(12) 0.0686(6) Uani 1 1 d . . . . .
H28A H 0.9873 0.2337 0.7904 0.103 Uiso 1 1 calc R U . . .
H28B H 0.9812 0.3434 0.8338 0.103 Uiso 1 1 calc R U . . .
H28C H 1.0202 0.3636 0.7641 0.103 Uiso 1 1 calc R U . . .
C29 C 0.98027(12) 0.77764(12) 0.66027(5) 0.0256(3) Uani 1 1 d . . . . .
C30 C 0.97699(13) 0.84736(13) 0.60444(6) 0.0287(3) Uani 1 1 d . . . . .
C31 C 1.04729(16) 0.93513(14) 0.59069(6) 0.0362(3) Uani 1 1 d . . . . .
H31 H 1.0437 0.9827 0.5533 0.043 Uiso 1 1 calc R U . . .
C32 C 1.12243(16) 0.95409(15) 0.63068(7) 0.0387(3) Uani 1 1 d . . . . .
H32 H 1.1686 1.0154 0.6211 0.046 Uiso 1 1 calc R U . . .
C33 C 1.12956(15) 0.88323(14) 0.68441(6) 0.0333(3) Uani 1 1 d . . . . .
H33 H 1.1826 0.8947 0.7115 0.040 Uiso 1 1 calc R U . . .
C34 C 1.05991(13) 0.79467(13) 0.69972(6) 0.0271(3) Uani 1 1 d . . . . .
C35 C 0.90807(14) 0.82517(14) 0.55669(6) 0.0306(3) Uani 1 1 d . . . . .
C36 C 0.97917(15) 0.71538(15) 0.52093(6) 0.0349(3) Uani 1 1 d . . . . .
C37 C 0.91988(17) 0.69770(17) 0.47427(6) 0.0406(3) Uani 1 1 d . . . . .
H37 H 0.9684 0.6231 0.4502 0.049 Uiso 1 1 calc R U . . .
C38 C 0.79149(17) 0.78651(17) 0.46210(6) 0.0403(3) Uani 1 1 d . . . . .
C39 C 0.72361(15) 0.89538(16) 0.49728(7) 0.0398(3) Uani 1 1 d . . . . .
H39 H 0.6363 0.9577 0.4889 0.048 Uiso 1 1 calc R U . . .
C40 C 0.77917(15) 0.91656(15) 0.54459(6) 0.0356(3) Uani 1 1 d . . . . .
C41 C 1.11916(17) 0.61733(17) 0.53241(7) 0.0470(4) Uani 1 1 d . . . . .
H41A H 1.1532 0.5475 0.5034 0.071 Uiso 1 1 calc R U . . .
H41B H 1.1128 0.5755 0.5722 0.071 Uiso 1 1 calc R U . . .
H41C H 1.1826 0.6651 0.5291 0.071 Uiso 1 1 calc R U . . .
C42 C 0.7284(2) 0.7634(2) 0.41182(8) 0.0563(5) Uani 1 1 d . . . . .
H42A H 0.6777 0.7041 0.4259 0.084 Uiso 1 1 calc R U . . .
H42B H 0.8013 0.7213 0.3799 0.084 Uiso 1 1 calc R U . . .
H42C H 0.6654 0.8498 0.3970 0.084 Uiso 1 1 calc R U . . .
C43 C 0.69910(18) 1.03412(18) 0.58243(9) 0.0556(4) Uani 1 1 d . . . . .
H43A H 0.7418 1.1016 0.5746 0.083 Uiso 1 1 calc R U . . .
H43B H 0.6988 1.0035 0.6241 0.083 Uiso 1 1 calc R U . . .
H43C H 0.6044 1.0740 0.5733 0.083 Uiso 1 1 calc R U . . .
C44 C 1.08007(13) 0.71979(13) 0.75844(6) 0.0282(3) Uani 1 1 d . . . . .
C45 C 1.16644(13) 0.58357(14) 0.76135(6) 0.0318(3) Uani 1 1 d . . . . .
C46 C 1.19266(16) 0.51983(16) 0.81664(7) 0.0407(3) Uani 1 1 d . . . . .
H46 H 1.2494 0.4271 0.8188 0.049 Uiso 1 1 calc R U . . .
C47 C 1.13908(18) 0.58681(19) 0.86829(7) 0.0477(4) Uani 1 1 d . . . . .
C48 C 1.05507(17) 0.72167(18) 0.86450(7) 0.0443(4) Uani 1 1 d . . . . .
H48 H 1.0179 0.7691 0.8997 0.053 Uiso 1 1 calc R U . . .
C49 C 1.02360(15) 0.78950(15) 0.81065(6) 0.0348(3) Uani 1 1 d . . . . .
C51 C 1.23678(15) 0.50578(15) 0.70696(7) 0.0391(3) Uani 1 1 d . . . . .
H51A H 1.2155 0.5658 0.6717 0.059 Uiso 1 1 calc R U . . .
H51B H 1.2043 0.4321 0.7060 0.059 Uiso 1 1 calc R U . . .
H51C H 1.3364 0.4688 0.7077 0.059 Uiso 1 1 calc R U . . .
C52 C 1.1704(3) 0.5151(3) 0.92744(9) 0.0772(7) Uani 1 1 d . . . . .
H52A H 1.1006 0.4770 0.9432 0.116 Uiso 1 1 calc R U . . .
H52B H 1.1699 0.5792 0.9549 0.116 Uiso 1 1 calc R U . . .
H52C H 1.2612 0.4427 0.9226 0.116 Uiso 1 1 calc R U . . .
C53 C 0.93046(18) 0.93571(16) 0.81001(7) 0.0456(4) Uani 1 1 d . . . . .
H53A H 0.8643 0.9530 0.8461 0.068 Uiso 1 1 calc R U . . .
H53B H 0.8810 0.9574 0.7755 0.068 Uiso 1 1 calc R U . . .
H53C H 0.9855 0.9919 0.8080 0.068 Uiso 1 1 calc R U . . .
H1A H 0.838(3) 0.676(3) 0.6316(13) 0.027(7) Uiso 0.5 1 d . . P . .
H1B H 0.982(3) 0.550(3) 0.6986(12) 0.020(6) Uiso 0.5 1 d . . P . .


#==============================================================================

# MOLECULAR GEOMETRY

_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 C4 1.8005(13) . ?
P1 C29 1.8540(13) . ?
P1 H1A 1.25(3) . ?
P1 H1B 1.31(3) . ?
N1 C1 1.3987(17) . ?
N1 C2 1.3991(18) . ?
N1 C5 1.4277(18) . ?
N2 C1 1.3912(17) . ?
N2 C3 1.4011(17) . ?
N2 C17 1.4312(18) . ?
C1 C4 1.3580(18) . ?
C2 C3 1.325(2) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 C10 1.399(2) . ?
C5 C6 1.399(2) . ?
C6 C7 1.393(2) . ?
C6 C11 1.519(2) . ?
C7 C8 1.380(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.382(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.392(2) . ?
C9 H9 0.9500 . ?
C10 C14 1.518(2) . ?
C11 C12 1.523(2) . ?
C11 C13 1.530(2) . ?
C11 H11 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C16 1.527(2) . ?
C14 C15 1.531(2) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.404(2) . ?
C17 C22 1.408(2) . ?
C18 C19 1.392(3) . ?
C18 C23 1.519(3) . ?
C19 C20 1.375(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.375(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.397(2) . ?
C21 H21 0.9500 . ?
C22 C26 1.513(3) . ?
C23 C25 1.531(3) . ?
C23 C24 1.534(2) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C28 1.527(2) . ?
C26 C27 1.534(2) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C34 1.4041(18) . ?
C29 C30 1.4142(18) . ?
C30 C31 1.3933(19) . ?
C30 C35 1.4983(18) . ?
C31 C32 1.387(2) . ?
C31 H31 0.9500 . ?
C32 C33 1.378(2) . ?
C32 H32 0.9500 . ?
C33 C34 1.3983(18) . ?
C33 H33 0.9500 . ?
C34 C44 1.4990(17) . ?
C35 C40 1.400(2) . ?
C35 C36 1.402(2) . ?
C36 C37 1.391(2) . ?
C36 C41 1.506(2) . ?
C37 C38 1.388(2) . ?
C37 H37 0.9500 . ?
C38 C39 1.384(2) . ?
C38 C42 1.511(2) . ?
C39 C40 1.394(2) . ?
C39 H39 0.9500 . ?
C40 C43 1.501(2) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C45 1.4034(19) . ?
C44 C49 1.406(2) . ?
C45 C46 1.395(2) . ?
C45 C51 1.505(2) . ?
C46 C47 1.379(3) . ?
C46 H46 0.9500 . ?
C47 C48 1.386(3) . ?
C47 C52 1.511(2) . ?
C48 C49 1.390(2) . ?
C48 H48 0.9500 . ?
C49 C53 1.506(2) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 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
C4 P1 C29 100.59(6) . . ?
C4 P1 H1A 108.3(13) . . ?
C29 P1 H1A 98.2(13) . . ?
C4 P1 H1B 113.5(12) . . ?
C29 P1 H1B 103.4(12) . . ?
H1A P1 H1B 127.7(18) . . ?
C1 N1 C2 109.77(11) . . ?
C1 N1 C5 123.59(11) . . ?
C2 N1 C5 124.18(11) . . ?
C1 N2 C3 109.68(11) . . ?
C1 N2 C17 126.56(11) . . ?
C3 N2 C17 123.32(11) . . ?
C4 C1 N2 130.66(12) . . ?
C4 C1 N1 125.19(12) . . ?
N2 C1 N1 104.13(11) . . ?
C3 C2 N1 108.02(12) . . ?
C3 C2 H2 126.0 . . ?
N1 C2 H2 126.0 . . ?
C2 C3 N2 108.40(12) . . ?
C2 C3 H3 125.8 . . ?
N2 C3 H3 125.8 . . ?
C1 C4 P1 126.93(10) . . ?
C1 C4 H4 116.5 . . ?
P1 C4 H4 116.5 . . ?
C10 C5 C6 122.52(13) . . ?
C10 C5 N1 118.70(12) . . ?
C6 C5 N1 118.78(13) . . ?
C7 C6 C5 117.45(14) . . ?
C7 C6 C11 120.69(14) . . ?
C5 C6 C11 121.85(13) . . ?
C8 C7 C6 121.08(15) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C7 C8 C9 120.37(15) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C8 C9 C10 120.88(15) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 H9 119.6 . . ?
C9 C10 C5 117.66(14) . . ?
C9 C10 C14 122.03(14) . . ?
C5 C10 C14 120.29(13) . . ?
C6 C11 C12 111.02(14) . . ?
C6 C11 C13 111.84(15) . . ?
C12 C11 C13 110.30(15) . . ?
C6 C11 H11 107.8 . . ?
C12 C11 H11 107.8 . . ?
C13 C11 H11 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 C16 112.83(14) . . ?
C10 C14 C15 109.98(13) . . ?
C16 C14 C15 111.44(13) . . ?
C10 C14 H14 107.4 . . ?
C16 C14 H14 107.4 . . ?
C15 C14 H14 107.4 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C22 123.03(14) . . ?
C18 C17 N2 118.37(14) . . ?
C22 C17 N2 118.53(13) . . ?
C19 C18 C17 116.82(18) . . ?
C19 C18 C23 122.18(17) . . ?
C17 C18 C23 120.98(14) . . ?
C20 C19 C18 121.38(19) . . ?
C20 C19 H19 119.3 . . ?
C18 C19 H19 119.3 . . ?
C21 C20 C19 120.84(17) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C20 C21 C22 121.1(2) . . ?
C20 C21 H21 119.5 . . ?
C22 C21 H21 119.5 . . ?
C21 C22 C17 116.80(17) . . ?
C21 C22 C26 121.62(17) . . ?
C17 C22 C26 121.50(14) . . ?
C18 C23 C25 111.31(14) . . ?
C18 C23 C24 113.99(18) . . ?
C25 C23 C24 108.88(17) . . ?
C18 C23 H23 107.5 . . ?
C25 C23 H23 107.5 . . ?
C24 C23 H23 107.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C26 C28 113.81(17) . . ?
C22 C26 C27 110.05(14) . . ?
C28 C26 C27 109.89(15) . . ?
C22 C26 H26 107.6 . . ?
C28 C26 H26 107.6 . . ?
C27 C26 H26 107.6 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C34 C29 C30 118.64(11) . . ?
C34 C29 P1 121.20(9) . . ?
C30 C29 P1 120.07(9) . . ?
C31 C30 C29 119.80(12) . . ?
C31 C30 C35 117.10(12) . . ?
C29 C30 C35 122.98(12) . . ?
C32 C31 C30 121.02(13) . . ?
C32 C31 H31 119.5 . . ?
C30 C31 H31 119.5 . . ?
C33 C32 C31 119.44(13) . . ?
C33 C32 H32 120.3 . . ?
C31 C32 H32 120.3 . . ?
C32 C33 C34 121.03(13) . . ?
C32 C33 H33 119.5 . . ?
C34 C33 H33 119.5 . . ?
C33 C34 C29 120.01(12) . . ?
C33 C34 C44 115.90(11) . . ?
C29 C34 C44 124.07(11) . . ?
C40 C35 C36 119.67(13) . . ?
C40 C35 C30 121.37(12) . . ?
C36 C35 C30 118.81(12) . . ?
C37 C36 C35 119.54(14) . . ?
C37 C36 C41 119.88(14) . . ?
C35 C36 C41 120.57(13) . . ?
C38 C37 C36 121.51(15) . . ?
C38 C37 H37 119.2 . . ?
C36 C37 H37 119.2 . . ?
C39 C38 C37 118.20(13) . . ?
C39 C38 C42 121.43(15) . . ?
C37 C38 C42 120.37(15) . . ?
C38 C39 C40 122.11(14) . . ?
C38 C39 H39 118.9 . . ?
C40 C39 H39 118.9 . . ?
C39 C40 C35 118.95(14) . . ?
C39 C40 C43 119.85(14) . . ?
C35 C40 C43 121.18(13) . . ?
C36 C41 H41A 109.5 . . ?
C36 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C36 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C38 C42 H42A 109.5 . . ?
C38 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C38 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C45 C44 C49 119.83(12) . . ?
C45 C44 C34 120.07(12) . . ?
C49 C44 C34 119.78(12) . . ?
C46 C45 C44 118.70(13) . . ?
C46 C45 C51 118.90(13) . . ?
C44 C45 C51 122.35(12) . . ?
C47 C46 C45 122.28(14) . . ?
C47 C46 H46 118.9 . . ?
C45 C46 H46 118.9 . . ?
C46 C47 C48 118.18(14) . . ?
C46 C47 C52 120.97(17) . . ?
C48 C47 C52 120.85(18) . . ?
C47 C48 C49 121.92(15) . . ?
C47 C48 H48 119.0 . . ?
C49 C48 H48 119.0 . . ?
C48 C49 C44 119.06(14) . . ?
C48 C49 C53 118.96(14) . . ?
C44 C49 C53 121.98(13) . . ?
C45 C51 H51A 109.5 . . ?
C45 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C45 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C47 C52 H52A 109.5 . . ?
C47 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C47 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C49 C53 H53A 109.5 . . ?
C49 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C49 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 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
C3 N2 C1 C4 -178.46(13) . . . . ?
C17 N2 C1 C4 9.0(2) . . . . ?
C3 N2 C1 N1 0.17(14) . . . . ?
C17 N2 C1 N1 -172.38(12) . . . . ?
C2 N1 C1 C4 179.13(13) . . . . ?
C5 N1 C1 C4 -18.1(2) . . . . ?
C2 N1 C1 N2 0.40(14) . . . . ?
C5 N1 C1 N2 163.19(12) . . . . ?
C1 N1 C2 C3 -0.85(16) . . . . ?
C5 N1 C2 C3 -163.52(13) . . . . ?
N1 C2 C3 N2 0.93(16) . . . . ?
C1 N2 C3 C2 -0.70(16) . . . . ?
C17 N2 C3 C2 172.14(13) . . . . ?
N2 C1 C4 P1 1.4(2) . . . . ?
N1 C1 C4 P1 -177.00(10) . . . . ?
C29 P1 C4 C1 164.34(12) . . . . ?
C1 N1 C5 C10 89.60(16) . . . . ?
C2 N1 C5 C10 -110.06(15) . . . . ?
C1 N1 C5 C6 -90.78(16) . . . . ?
C2 N1 C5 C6 69.56(18) . . . . ?
C10 C5 C6 C7 2.0(2) . . . . ?
N1 C5 C6 C7 -177.58(13) . . . . ?
C10 C5 C6 C11 -176.80(13) . . . . ?
N1 C5 C6 C11 3.6(2) . . . . ?
C5 C6 C7 C8 -0.7(2) . . . . ?
C11 C6 C7 C8 178.13(16) . . . . ?
C6 C7 C8 C9 -0.4(3) . . . . ?
C7 C8 C9 C10 0.2(3) . . . . ?
C8 C9 C10 C5 1.0(2) . . . . ?
C8 C9 C10 C14 179.44(15) . . . . ?
C6 C5 C10 C9 -2.2(2) . . . . ?
N1 C5 C10 C9 177.42(12) . . . . ?
C6 C5 C10 C14 179.38(13) . . . . ?
N1 C5 C10 C14 -1.01(19) . . . . ?
C7 C6 C11 C12 -63.4(2) . . . . ?
C5 C6 C11 C12 115.42(16) . . . . ?
C7 C6 C11 C13 60.3(2) . . . . ?
C5 C6 C11 C13 -120.91(18) . . . . ?
C9 C10 C14 C16 34.9(2) . . . . ?
C5 C10 C14 C16 -146.77(14) . . . . ?
C9 C10 C14 C15 -90.22(18) . . . . ?
C5 C10 C14 C15 88.14(16) . . . . ?
C1 N2 C17 C18 -112.30(15) . . . . ?
C3 N2 C17 C18 76.10(17) . . . . ?
C1 N2 C17 C22 70.53(18) . . . . ?
C3 N2 C17 C22 -101.07(16) . . . . ?
C22 C17 C18 C19 -0.9(2) . . . . ?
N2 C17 C18 C19 -177.97(13) . . . . ?
C22 C17 C18 C23 -179.49(13) . . . . ?
N2 C17 C18 C23 3.5(2) . . . . ?
C17 C18 C19 C20 -1.3(2) . . . . ?
C23 C18 C19 C20 177.19(16) . . . . ?
C18 C19 C20 C21 2.1(3) . . . . ?
C19 C20 C21 C22 -0.5(3) . . . . ?
C20 C21 C22 C17 -1.7(2) . . . . ?
C20 C21 C22 C26 175.16(16) . . . . ?
C18 C17 C22 C21 2.4(2) . . . . ?
N2 C17 C22 C21 179.43(13) . . . . ?
C18 C17 C22 C26 -174.43(13) . . . . ?
N2 C17 C22 C26 2.6(2) . . . . ?
C19 C18 C23 C25 -106.76(19) . . . . ?
C17 C18 C23 C25 71.7(2) . . . . ?
C19 C18 C23 C24 16.9(2) . . . . ?
C17 C18 C23 C24 -164.65(15) . . . . ?
C21 C22 C26 C28 32.5(2) . . . . ?
C17 C22 C26 C28 -150.82(14) . . . . ?
C21 C22 C26 C27 -91.34(18) . . . . ?
C17 C22 C26 C27 85.33(17) . . . . ?
C4 P1 C29 C34 71.10(11) . . . . ?
C4 P1 C29 C30 -112.48(11) . . . . ?
C34 C29 C30 C31 -2.71(19) . . . . ?
P1 C29 C30 C31 -179.22(10) . . . . ?
C34 C29 C30 C35 173.20(12) . . . . ?
P1 C29 C30 C35 -3.32(17) . . . . ?
C29 C30 C31 C32 0.9(2) . . . . ?
C35 C30 C31 C32 -175.24(14) . . . . ?
C30 C31 C32 C33 1.1(2) . . . . ?
C31 C32 C33 C34 -1.3(2) . . . . ?
C32 C33 C34 C29 -0.5(2) . . . . ?
C32 C33 C34 C44 177.81(13) . . . . ?
C30 C29 C34 C33 2.51(19) . . . . ?
P1 C29 C34 C33 178.99(10) . . . . ?
C30 C29 C34 C44 -175.65(12) . . . . ?
P1 C29 C34 C44 0.82(18) . . . . ?
C31 C30 C35 C40 -81.42(17) . . . . ?
C29 C30 C35 C40 102.57(16) . . . . ?
C31 C30 C35 C36 94.05(16) . . . . ?
C29 C30 C35 C36 -81.96(17) . . . . ?
C40 C35 C36 C37 -0.8(2) . . . . ?
C30 C35 C36 C37 -176.35(13) . . . . ?
C40 C35 C36 C41 178.80(14) . . . . ?
C30 C35 C36 C41 3.3(2) . . . . ?
C35 C36 C37 C38 0.1(2) . . . . ?
C41 C36 C37 C38 -179.55(14) . . . . ?
C36 C37 C38 C39 0.9(2) . . . . ?
C36 C37 C38 C42 -178.87(15) . . . . ?
C37 C38 C39 C40 -1.1(2) . . . . ?
C42 C38 C39 C40 178.66(14) . . . . ?
C38 C39 C40 C35 0.3(2) . . . . ?
C38 C39 C40 C43 -178.15(15) . . . . ?
C36 C35 C40 C39 0.6(2) . . . . ?
C30 C35 C40 C39 176.03(12) . . . . ?
C36 C35 C40 C43 179.08(14) . . . . ?
C30 C35 C40 C43 -5.5(2) . . . . ?
C33 C34 C44 C45 -104.16(15) . . . . ?
C29 C34 C44 C45 74.07(17) . . . . ?
C33 C34 C44 C49 69.39(16) . . . . ?
C29 C34 C44 C49 -112.37(15) . . . . ?
C49 C44 C45 C46 0.89(19) . . . . ?
C34 C44 C45 C46 174.45(12) . . . . ?
C49 C44 C45 C51 -176.22(12) . . . . ?
C34 C44 C45 C51 -2.66(19) . . . . ?
C44 C45 C46 C47 -1.4(2) . . . . ?
C51 C45 C46 C47 175.77(14) . . . . ?
C45 C46 C47 C48 0.8(2) . . . . ?
C45 C46 C47 C52 -179.47(17) . . . . ?
C46 C47 C48 C49 0.4(2) . . . . ?
C52 C47 C48 C49 -179.36(17) . . . . ?
C47 C48 C49 C44 -0.9(2) . . . . ?
C47 C48 C49 C53 179.40(15) . . . . ?
C45 C44 C49 C48 0.2(2) . . . . ?
C34 C44 C49 C48 -173.36(13) . . . . ?
C45 C44 C49 C53 179.94(13) . . . . ?
C34 C44 C49 C53 6.4(2) . . . . ?

_refine_diff_density_max         0.288
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.036


####################################################################### 
# 
# 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_ax1685_DipTerPHCHIDip_cmp16
_database_code_depnum_ccdc_archive 'CCDC 2046865'
loop_
_audit_author_name
_audit_author_address
'Hering-Junghans C.'
;LIKAT Rostock
Germany
;
_audit_update_record             
;
2020-11-27 deposited with the CCDC.	2021-01-13 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C58 H75 N2 P, C5 H12'
_chemical_formula_sum            'C63 H87 N2 P'
_chemical_formula_weight         903.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#==============================================================================

# CRYSTAL DATA

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

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

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

_cell_length_a                   13.3114(4)
_cell_length_b                   18.0342(5)
_cell_length_c                   24.3084(7)
_cell_angle_alpha                90
_cell_angle_beta                 104.2346(19)
_cell_angle_gamma                90
_cell_volume                     5656.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6511
_cell_measurement_theta_min      3.09
_cell_measurement_theta_max      66.45

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_F_000             1976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.044
_exptl_absorpt_coefficient_mu    0.703
_shelx_estimated_absorpt_T_min   0.825
_shelx_estimated_absorpt_T_max   0.970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014)'

#==============================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         microfocus
_diffrn_radiation_monochromator  multilayer
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48976
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.086
_diffrn_reflns_theta_max         65.000
_diffrn_reflns_theta_full        65.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9620
_reflns_number_gt                7565
_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.
 
 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.
;

_computing_data_collection       'Bruker Apex V7.51A'
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms 
 were positioned geometrically and refined using a riding model, with C---H = 
 0.98 (methyl groups), 0.99Å (methylene groups), 1.00Å (methine groups) or 
 0.95 Å (aryl CH) and with Uiso(H) = 1.5 times Ueq(C) 
 (methyl groups) or with Uiso(H) = 1.2 times Ueq(C) 
 (methylene  groups, aryl CH, methine groups). Torsion angles of all methyl 
 groups were allowed to refine. One of isopropyl groups of the Dip moiety was
 found to be disordered and was split in two parts. The occupancy of each part
 was allowed to refine freely. 

 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 > 2σ(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.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.500 470 85 ' '
2 0.000 0.500 1.000 470 85 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The unit cell contains four disordered n-pentane molecules. These 
have been treated as a diffuse contribution to the overall scattering 
without specific atom positions by SQUEEZE/PLATON.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0895P)²+0.8111P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9620
_refine_ls_number_parameters     595
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0521
_refine_ls_wR_factor_ref         0.1579
_refine_ls_wR_factor_gt          0.1434
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.29838(4) 0.41305(2) 0.65811(2) 0.04738(14) Uani 1 1 d . . . . .
N1 N 0.25291(15) 0.57735(8) 0.70349(7) 0.0556(4) Uani 1 1 d . . . . .
N2 N 0.26654(15) 0.54467(9) 0.79188(7) 0.0582(4) Uani 1 1 d . . . . .
C1 C 0.26778(15) 0.51572(10) 0.73865(8) 0.0484(4) Uani 1 1 d . . . . .
C2 C 0.2453(2) 0.64091(12) 0.73481(10) 0.0747(7) Uani 1 1 d . . . . .
H2 H 0.2363 0.6901 0.7205 0.090 Uiso 1 1 calc R U . . .
C3 C 0.2528(2) 0.62083(12) 0.78786(10) 0.0707(6) Uani 1 1 d . . . . .
H3 H 0.2494 0.6532 0.8182 0.085 Uiso 1 1 calc R U . . .
C4 C 0.28267(16) 0.44372(10) 0.72586(8) 0.0509(4) Uani 1 1 d . . . . .
H4 H 0.2849 0.4075 0.7545 0.061 Uiso 1 1 calc R U . . .
C5 C 0.23122(16) 0.57962(9) 0.64256(8) 0.0506(4) Uani 1 1 d . . . . .
C6 C 0.30849(17) 0.60565(11) 0.61772(8) 0.0554(5) Uani 1 1 d . . . . .
C7 C 0.28458(18) 0.61183(14) 0.55900(9) 0.0656(5) Uani 1 1 d . . . . .
H7 H 0.3353 0.6304 0.5411 0.079 Uiso 1 1 calc R U . . .
C8 C 0.18910(19) 0.59162(14) 0.52629(9) 0.0674(6) Uani 1 1 d . . . . .
H8 H 0.1748 0.5953 0.4861 0.081 Uiso 1 1 calc R U . . .
C9 C 0.11410(18) 0.56596(13) 0.55160(9) 0.0631(5) Uani 1 1 d . . . . .
H9 H 0.0485 0.5518 0.5285 0.076 Uiso 1 1 calc R U . . .
C10 C 0.13229(17) 0.56026(11) 0.61029(9) 0.0582(5) Uani 1 1 d . . . . .
C11 C 0.41588(18) 0.62588(13) 0.65272(10) 0.0656(5) Uani 1 1 d . . . . .
H11 H 0.4210 0.6104 0.6928 0.079 Uiso 1 1 calc R U . . .
C12 C 0.4990(2) 0.58375(15) 0.63151(13) 0.0786(7) Uani 1 1 d . . . . .
H12A H 0.5030 0.6036 0.5946 0.118 Uiso 1 1 calc R U . . .
H12B H 0.4809 0.5310 0.6276 0.118 Uiso 1 1 calc R U . . .
H12C H 0.5663 0.5897 0.6588 0.118 Uiso 1 1 calc R U . . .
C13 C 0.4366(2) 0.70880(15) 0.65259(13) 0.0867(8) Uani 1 1 d . . . . .
H13A H 0.4315 0.7254 0.6136 0.130 Uiso 1 1 calc R U . . .
H13B H 0.5064 0.7192 0.6760 0.130 Uiso 1 1 calc R U . . .
H13C H 0.3854 0.7352 0.6681 0.130 Uiso 1 1 calc R U . . .
C14A C 0.0537(4) 0.5320(3) 0.6409(3) 0.0650(13) Uani 0.692(7) 1 d . . P A 1
H14 H 0.0912 0.5058 0.6762 0.078 Uiso 0.692(7) 1 calc R U P A 1
C15A C -0.0005(4) 0.6008(3) 0.6577(2) 0.1038(18) Uani 0.692(7) 1 d . . P A 1
H15A H 0.0515 0.6341 0.6806 0.156 Uiso 0.692(7) 1 calc R U P A 1
H15B H -0.0381 0.6267 0.6233 0.156 Uiso 0.692(7) 1 calc R U P A 1
H15C H -0.0493 0.5854 0.6798 0.156 Uiso 0.692(7) 1 calc R U P A 1
C16A C -0.0228(4) 0.4804(4) 0.6061(3) 0.0849(15) Uani 0.692(7) 1 d . . P A 1
H16A H -0.0714 0.4640 0.6280 0.127 Uiso 0.692(7) 1 calc R U P A 1
H16B H -0.0609 0.5058 0.5716 0.127 Uiso 0.692(7) 1 calc R U P A 1
H16C H 0.0134 0.4373 0.5957 0.127 Uiso 0.692(7) 1 calc R U P A 1
C14B C 0.0327(10) 0.5471(7) 0.6329(6) 0.059(4) Uiso 0.308(7) 1 d . . P A 2
H14B H 0.0492 0.5625 0.6737 0.071 Uiso 0.308(7) 1 calc R U P A 2
C15B C 0.0068(9) 0.4598(6) 0.6301(6) 0.072(3) Uani 0.308(7) 1 d . . P A 2
H15D H 0.0692 0.4320 0.6487 0.107 Uiso 0.308(7) 1 calc R U P A 2
H15E H -0.0481 0.4500 0.6496 0.107 Uiso 0.308(7) 1 calc R U P A 2
H15F H -0.0163 0.4443 0.5903 0.107 Uiso 0.308(7) 1 calc R U P A 2
C16B C -0.0704(7) 0.5840(6) 0.6027(5) 0.087(3) Uani 0.308(7) 1 d . . P A 2
H16D H -0.1242 0.5703 0.6220 0.131 Uiso 0.308(7) 1 calc R U P A 2
H16E H -0.0619 0.6380 0.6037 0.131 Uiso 0.308(7) 1 calc R U P A 2
H16F H -0.0907 0.5672 0.5632 0.131 Uiso 0.308(7) 1 calc R U P A 2
C17 C 0.2555(2) 0.50464(11) 0.84136(9) 0.0619(5) Uani 1 1 d . . . . .
C18 C 0.3444(2) 0.47653(13) 0.87888(9) 0.0697(6) Uani 1 1 d . . . . .
C19 C 0.3340(3) 0.44534(16) 0.93012(11) 0.0852(8) Uani 1 1 d . . . . .
H19 H 0.3932 0.4260 0.9564 0.102 Uiso 1 1 calc R U . . .
C20 C 0.2393(3) 0.44261(19) 0.94234(12) 0.0981(10) Uani 1 1 d . . . . .
H20 H 0.2335 0.4224 0.9775 0.118 Uiso 1 1 calc R U . . .
C21 C 0.1515(3) 0.46890(18) 0.90404(13) 0.0912(9) Uani 1 1 d . . . . .
H21 H 0.0863 0.4656 0.9132 0.109 Uiso 1 1 calc R U . . .
C22 C 0.1570(2) 0.50025(13) 0.85224(11) 0.0737(7) Uani 1 1 d . . . . .
C23 C 0.4503(2) 0.47841(13) 0.86667(10) 0.0705(6) Uani 1 1 d . . . . .
H23 H 0.4423 0.5000 0.8279 0.085 Uiso 1 1 calc R U . . .
C24 C 0.4938(3) 0.39957(16) 0.86617(14) 0.0912(8) Uani 1 1 d . . . . .
H24A H 0.5606 0.4016 0.8560 0.137 Uiso 1 1 calc R U . . .
H24B H 0.4451 0.3694 0.8383 0.137 Uiso 1 1 calc R U . . .
H24C H 0.5035 0.3774 0.9039 0.137 Uiso 1 1 calc R U . . .
C25 C 0.5249(3) 0.52799(19) 0.90885(12) 0.0946(9) Uani 1 1 d . . . . .
H25A H 0.5366 0.5069 0.9470 0.142 Uiso 1 1 calc R U . . .
H25B H 0.4950 0.5777 0.9085 0.142 Uiso 1 1 calc R U . . .
H25C H 0.5910 0.5312 0.8981 0.142 Uiso 1 1 calc R U . . .
C26 C 0.0600(2) 0.52471(15) 0.80952(12) 0.0788(7) Uani 1 1 d . . . . .
H26 H 0.0817 0.5582 0.7818 0.095 Uiso 1 1 calc R U . . .
C27 C -0.0136(3) 0.5679(2) 0.83600(19) 0.1169(12) Uani 1 1 d . . . . .
H27A H -0.0403 0.5354 0.8614 0.175 Uiso 1 1 calc R U . . .
H27B H -0.0715 0.5865 0.8060 0.175 Uiso 1 1 calc R U . . .
H27C H 0.0233 0.6098 0.8576 0.175 Uiso 1 1 calc R U . . .
C28 C 0.0059(3) 0.45811(18) 0.77659(16) 0.0997(9) Uani 1 1 d . . . . .
H28A H 0.0537 0.4328 0.7579 0.150 Uiso 1 1 calc R U . . .
H28B H -0.0552 0.4749 0.7479 0.150 Uiso 1 1 calc R U . . .
H28C H -0.0156 0.4238 0.8028 0.150 Uiso 1 1 calc R U . . .
C29 C 0.35648(14) 0.31984(9) 0.67332(7) 0.0443(4) Uani 1 1 d . . . . .
C30 C 0.45645(14) 0.30752(10) 0.66592(7) 0.0451(4) Uani 1 1 d . . . . .
C31 C 0.50094(16) 0.23729(11) 0.67608(8) 0.0523(4) Uani 1 1 d . . . . .
H31 H 0.5697 0.2298 0.6724 0.063 Uiso 1 1 calc R U . . .
C32 C 0.44741(17) 0.17841(11) 0.69128(9) 0.0563(5) Uani 1 1 d . . . . .
H32 H 0.4797 0.1313 0.6994 0.068 Uiso 1 1 calc R U . . .
C33 C 0.34656(17) 0.18881(10) 0.69449(9) 0.0549(5) Uani 1 1 d . . . . .
H33 H 0.3081 0.1477 0.7026 0.066 Uiso 1 1 calc R U . . .
C34 C 0.29958(15) 0.25847(10) 0.68605(8) 0.0477(4) Uani 1 1 d . . . . .
C35 C 0.51848(15) 0.36279(10) 0.64116(9) 0.0498(4) Uani 1 1 d . . . . .
C36 C 0.60619(15) 0.39715(11) 0.67571(9) 0.0526(4) Uani 1 1 d . . . . .
C37 C 0.67272(17) 0.43670(12) 0.64986(11) 0.0641(5) Uani 1 1 d . . . . .
H37 H 0.7331 0.4594 0.6728 0.077 Uiso 1 1 calc R U . . .
C38 C 0.6518(2) 0.44317(15) 0.59151(12) 0.0757(7) Uani 1 1 d . . . . .
H38 H 0.6988 0.4688 0.5745 0.091 Uiso 1 1 calc R U . . .
C39 C 0.5627(2) 0.41243(16) 0.55798(11) 0.0771(7) Uani 1 1 d . . . . .
H39 H 0.5470 0.4194 0.5180 0.092 Uiso 1 1 calc R U . . .
C40 C 0.49500(18) 0.37121(13) 0.58184(10) 0.0632(5) Uani 1 1 d . . . . .
C41 C 0.63163(17) 0.39356(12) 0.73949(10) 0.0618(5) Uani 1 1 d . . . . .
H41 H 0.5745 0.3660 0.7506 0.074 Uiso 1 1 calc R U . . .
C42 C 0.7323(2) 0.35126(17) 0.76291(14) 0.0929(9) Uani 1 1 d . . . . .
H42A H 0.7273 0.3019 0.7456 0.139 Uiso 1 1 calc R U . . .
H42B H 0.7442 0.3463 0.8042 0.139 Uiso 1 1 calc R U . . .
H42C H 0.7901 0.3784 0.7540 0.139 Uiso 1 1 calc R U . . .
C43 C 0.6368(3) 0.47090(16) 0.76505(13) 0.0931(9) Uani 1 1 d . . . . .
H43A H 0.6879 0.5006 0.7519 0.140 Uiso 1 1 calc R U . . .
H43B H 0.6571 0.4673 0.8065 0.140 Uiso 1 1 calc R U . . .
H43C H 0.5686 0.4945 0.7532 0.140 Uiso 1 1 calc R U . . .
C44 C 0.4005(2) 0.33609(16) 0.54297(10) 0.0750(7) Uani 1 1 d . . . . .
H44 H 0.3547 0.3184 0.5673 0.090 Uiso 1 1 calc R U . . .
C45 C 0.3380(2) 0.3917(2) 0.50049(12) 0.0925(9) Uani 1 1 d . . . . .
H45A H 0.3221 0.4353 0.5209 0.139 Uiso 1 1 calc R U . . .
H45B H 0.2733 0.3685 0.4796 0.139 Uiso 1 1 calc R U . . .
H45C H 0.3786 0.4069 0.4738 0.139 Uiso 1 1 calc R U . . .
C46 C 0.4298(3) 0.2686(2) 0.51263(14) 0.1026(10) Uani 1 1 d . . . . .
H46A H 0.4770 0.2837 0.4894 0.154 Uiso 1 1 calc R U . . .
H46B H 0.3672 0.2468 0.4882 0.154 Uiso 1 1 calc R U . . .
H46C H 0.4642 0.2319 0.5407 0.154 Uiso 1 1 calc R U . . .
C47 C 0.18706(15) 0.26364(10) 0.68586(9) 0.0528(4) Uani 1 1 d . . . . .
C48 C 0.11285(16) 0.26504(11) 0.63326(10) 0.0590(5) Uani 1 1 d . . . . .
C49 C 0.00823(18) 0.26979(13) 0.63309(12) 0.0704(6) Uani 1 1 d . . . . .
H49 H -0.0427 0.2717 0.5980 0.085 Uiso 1 1 calc R U . . .
C50 C -0.02187(19) 0.27180(14) 0.68338(13) 0.0757(7) Uani 1 1 d . . . . .
H50 H -0.0932 0.2766 0.6827 0.091 Uiso 1 1 calc R U . . .
C51 C 0.05079(19) 0.26687(13) 0.73485(12) 0.0689(6) Uani 1 1 d . . . . .
H51 H 0.0285 0.2666 0.7691 0.083 Uiso 1 1 calc R U . . .
C52 C 0.15605(17) 0.26229(11) 0.73718(10) 0.0585(5) Uani 1 1 d . . . . .
C53 C 0.14348(19) 0.25466(14) 0.57730(11) 0.0692(6) Uani 1 1 d . . . . .
H53 H 0.2189 0.2666 0.5845 0.083 Uiso 1 1 calc R U . . .
C54 C 0.0861(2) 0.30532(19) 0.52942(12) 0.0881(8) Uani 1 1 d . . . . .
H54A H 0.0117 0.2948 0.5210 0.132 Uiso 1 1 calc R U . . .
H54B H 0.1115 0.2964 0.4954 0.132 Uiso 1 1 calc R U . . .
H54C H 0.0984 0.3572 0.5411 0.132 Uiso 1 1 calc R U . . .
C55 C 0.1304(3) 0.17345(18) 0.55928(14) 0.0960(9) Uani 1 1 d . . . . .
H55A H 0.1726 0.1423 0.5892 0.144 Uiso 1 1 calc R U . . .
H55B H 0.1530 0.1666 0.5242 0.144 Uiso 1 1 calc R U . . .
H55C H 0.0574 0.1593 0.5529 0.144 Uiso 1 1 calc R U . . .
C56 C 0.2335(2) 0.25222(14) 0.79427(11) 0.0694(6) Uani 1 1 d . . . . .
H56 H 0.3034 0.2668 0.7896 0.083 Uiso 1 1 calc R U . . .
C57 C 0.2392(3) 0.17061(17) 0.81303(15) 0.0927(9) Uani 1 1 d . . . . .
H57A H 0.1701 0.1537 0.8148 0.139 Uiso 1 1 calc R U . . .
H57B H 0.2870 0.1659 0.8506 0.139 Uiso 1 1 calc R U . . .
H57C H 0.2641 0.1403 0.7857 0.139 Uiso 1 1 calc R U . . .
C58 C 0.2106(2) 0.29884(16) 0.84151(12) 0.0835(7) Uani 1 1 d . . . . .
H58A H 0.1454 0.2824 0.8494 0.125 Uiso 1 1 calc R U . . .
H58B H 0.2046 0.3510 0.8299 0.125 Uiso 1 1 calc R U . . .
H58C H 0.2670 0.2933 0.8758 0.125 Uiso 1 1 calc R U . . .
H1A H 0.208(2) 0.3995(14) 0.6273(11) 0.011(6) Uiso 0.5 1 d . . P . .
H1B H 0.377(4) 0.450(3) 0.651(2) 0.078(15) Uiso 0.5 1 d . . P . .


#==============================================================================

# MOLECULAR GEOMETRY

_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 C4 1.7976(18) . ?
P1 C29 1.8493(17) . ?
P1 H1A 1.27(3) . ?
P1 H1B 1.29(5) . ?
N1 C1 1.386(3) . ?
N1 C2 1.393(3) . ?
N1 C5 1.438(3) . ?
N2 C3 1.386(3) . ?
N2 C1 1.399(3) . ?
N2 C17 1.441(3) . ?
C1 C4 1.361(3) . ?
C2 C3 1.319(3) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 C6 1.396(3) . ?
C5 C10 1.401(3) . ?
C6 C7 1.389(3) . ?
C6 C11 1.517(3) . ?
C7 C8 1.372(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.375(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.391(3) . ?
C9 H9 0.9500 . ?
C10 C14A 1.513(6) . ?
C10 C14B 1.574(15) . ?
C11 C13 1.521(4) . ?
C11 C12 1.532(4) . ?
C11 H11 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14A C16A 1.480(8) . ?
C14A C15A 1.540(7) . ?
C14A H14 1.0000 . ?
C15A H15A 0.9800 . ?
C15A H15B 0.9800 . ?
C15A H15C 0.9800 . ?
C16A H16A 0.9800 . ?
C16A H16B 0.9800 . ?
C16A H16C 0.9800 . ?
C14B C16B 1.538(15) . ?
C14B C15B 1.610(17) . ?
C14B H14B 1.0000 . ?
C15B H15D 0.9800 . ?
C15B H15E 0.9800 . ?
C15B H15F 0.9800 . ?
C16B H16D 0.9800 . ?
C16B H16E 0.9800 . ?
C16B H16F 0.9800 . ?
C17 C18 1.399(4) . ?
C17 C22 1.402(4) . ?
C18 C19 1.404(3) . ?
C18 C23 1.511(4) . ?
C19 C20 1.365(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.387(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.398(4) . ?
C21 H21 0.9500 . ?
C22 C26 1.510(4) . ?
C23 C25 1.528(4) . ?
C23 C24 1.536(4) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.514(4) . ?
C26 C28 1.523(4) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.404(3) . ?
C29 C34 1.418(3) . ?
C30 C31 1.394(3) . ?
C30 C35 1.511(2) . ?
C31 C32 1.379(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.377(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.396(3) . ?
C33 H33 0.9500 . ?
C34 C47 1.500(3) . ?
C35 C36 1.404(3) . ?
C35 C40 1.406(3) . ?
C36 C37 1.401(3) . ?
C36 C41 1.505(3) . ?
C37 C38 1.382(4) . ?
C37 H37 0.9500 . ?
C38 C39 1.380(4) . ?
C38 H38 0.9500 . ?
C39 C40 1.399(3) . ?
C39 H39 0.9500 . ?
C40 C44 1.514(3) . ?
C41 C43 1.522(4) . ?
C41 C42 1.525(4) . ?
C41 H41 1.0000 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C46 1.523(4) . ?
C44 C45 1.530(4) . ?
C44 H44 1.0000 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C52 1.407(3) . ?
C47 C48 1.411(3) . ?
C48 C49 1.394(3) . ?
C48 C53 1.525(3) . ?
C49 C50 1.377(4) . ?
C49 H49 0.9500 . ?
C50 C51 1.383(4) . ?
C50 H50 0.9500 . ?
C51 C52 1.391(3) . ?
C51 H51 0.9500 . ?
C52 C56 1.522(4) . ?
C53 C55 1.526(4) . ?
C53 C54 1.528(4) . ?
C53 H53 1.0000 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 C58 1.514(4) . ?
C56 C57 1.537(4) . ?
C56 H56 1.0000 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 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
C4 P1 C29 103.52(8) . . ?
C4 P1 H1A 107.0(12) . . ?
C29 P1 H1A 103.3(12) . . ?
C4 P1 H1B 104(2) . . ?
C29 P1 H1B 101(2) . . ?
H1A P1 H1B 134(3) . . ?
C1 N1 C2 109.95(17) . . ?
C1 N1 C5 128.31(15) . . ?
C2 N1 C5 121.07(17) . . ?
C3 N2 C1 109.63(17) . . ?
C3 N2 C17 121.12(17) . . ?
C1 N2 C17 127.72(16) . . ?
C4 C1 N1 129.10(17) . . ?
C4 C1 N2 127.07(17) . . ?
N1 C1 N2 103.81(16) . . ?
C3 C2 N1 108.06(19) . . ?
C3 C2 H2 126.0 . . ?
N1 C2 H2 126.0 . . ?
C2 C3 N2 108.54(19) . . ?
C2 C3 H3 125.7 . . ?
N2 C3 H3 125.7 . . ?
C1 C4 P1 124.00(14) . . ?
C1 C4 H4 118.0 . . ?
P1 C4 H4 118.0 . . ?
C6 C5 C10 122.19(19) . . ?
C6 C5 N1 118.19(19) . . ?
C10 C5 N1 119.50(19) . . ?
C7 C6 C5 117.7(2) . . ?
C7 C6 C11 120.2(2) . . ?
C5 C6 C11 122.09(18) . . ?
C8 C7 C6 121.3(2) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
C7 C8 C9 120.1(2) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C8 C9 C10 121.4(2) . . ?
C8 C9 H9 119.3 . . ?
C10 C9 H9 119.3 . . ?
C9 C10 C5 117.3(2) . . ?
C9 C10 C14A 124.2(3) . . ?
C5 C10 C14A 118.5(3) . . ?
C9 C10 C14B 114.9(5) . . ?
C5 C10 C14B 126.8(5) . . ?
C6 C11 C13 112.4(2) . . ?
C6 C11 C12 110.5(2) . . ?
C13 C11 C12 109.9(2) . . ?
C6 C11 H11 107.9 . . ?
C13 C11 H11 107.9 . . ?
C12 C11 H11 107.9 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C16A C14A C10 113.1(4) . . ?
C16A C14A C15A 110.9(5) . . ?
C10 C14A C15A 106.5(4) . . ?
C16A C14A H14 108.7 . . ?
C10 C14A H14 108.7 . . ?
C15A C14A H14 108.7 . . ?
C14A C15A H15A 109.5 . . ?
C14A C15A H15B 109.5 . . ?
H15A C15A H15B 109.5 . . ?
C14A C15A H15C 109.5 . . ?
H15A C15A H15C 109.5 . . ?
H15B C15A H15C 109.5 . . ?
C14A C16A H16A 109.5 . . ?
C14A C16A H16B 109.5 . . ?
H16A C16A H16B 109.5 . . ?
C14A C16A H16C 109.5 . . ?
H16A C16A H16C 109.5 . . ?
H16B C16A H16C 109.5 . . ?
C16B C14B C10 119.8(9) . . ?
C16B C14B C15B 104.2(10) . . ?
C10 C14B C15B 108.8(9) . . ?
C16B C14B H14B 107.8 . . ?
C10 C14B H14B 107.8 . . ?
C15B C14B H14B 107.8 . . ?
C14B C15B H15D 109.5 . . ?
C14B C15B H15E 109.5 . . ?
H15D C15B H15E 109.5 . . ?
C14B C15B H15F 109.5 . . ?
H15D C15B H15F 109.5 . . ?
H15E C15B H15F 109.5 . . ?
C14B C16B H16D 109.5 . . ?
C14B C16B H16E 109.5 . . ?
H16D C16B H16E 109.5 . . ?
C14B C16B H16F 109.5 . . ?
H16D C16B H16F 109.5 . . ?
H16E C16B H16F 109.5 . . ?
C18 C17 C22 122.5(2) . . ?
C18 C17 N2 118.8(2) . . ?
C22 C17 N2 118.5(2) . . ?
C17 C18 C19 118.1(3) . . ?
C17 C18 C23 123.0(2) . . ?
C19 C18 C23 118.9(3) . . ?
C20 C19 C18 120.3(3) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C19 C20 C21 120.8(3) . . ?
C19 C20 H20 119.6 . . ?
C21 C20 H20 119.6 . . ?
C20 C21 C22 121.4(3) . . ?
C20 C21 H21 119.3 . . ?
C22 C21 H21 119.3 . . ?
C21 C22 C17 116.8(3) . . ?
C21 C22 C26 120.8(3) . . ?
C17 C22 C26 122.3(2) . . ?
C18 C23 C25 111.4(2) . . ?
C18 C23 C24 110.6(2) . . ?
C25 C23 C24 111.3(3) . . ?
C18 C23 H23 107.8 . . ?
C25 C23 H23 107.8 . . ?
C24 C23 H23 107.8 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C26 C27 113.0(3) . . ?
C22 C26 C28 110.2(2) . . ?
C27 C26 C28 110.9(3) . . ?
C22 C26 H26 107.5 . . ?
C27 C26 H26 107.5 . . ?
C28 C26 H26 107.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C34 118.60(16) . . ?
C30 C29 P1 118.78(13) . . ?
C34 C29 P1 122.25(14) . . ?
C31 C30 C29 119.73(16) . . ?
C31 C30 C35 114.83(16) . . ?
C29 C30 C35 125.09(16) . . ?
C32 C31 C30 121.46(18) . . ?
C32 C31 H31 119.3 . . ?
C30 C31 H31 119.3 . . ?
C33 C32 C31 119.06(18) . . ?
C33 C32 H32 120.5 . . ?
C31 C32 H32 120.5 . . ?
C32 C33 C34 121.48(17) . . ?
C32 C33 H33 119.3 . . ?
C34 C33 H33 119.3 . . ?
C33 C34 C29 119.38(17) . . ?
C33 C34 C47 117.86(16) . . ?
C29 C34 C47 122.53(16) . . ?
C36 C35 C40 120.55(17) . . ?
C36 C35 C30 120.57(17) . . ?
C40 C35 C30 118.31(18) . . ?
C37 C36 C35 118.7(2) . . ?
C37 C36 C41 118.5(2) . . ?
C35 C36 C41 122.74(17) . . ?
C38 C37 C36 120.9(2) . . ?
C38 C37 H37 119.5 . . ?
C36 C37 H37 119.5 . . ?
C39 C38 C37 119.9(2) . . ?
C39 C38 H38 120.0 . . ?
C37 C38 H38 120.0 . . ?
C38 C39 C40 121.1(2) . . ?
C38 C39 H39 119.4 . . ?
C40 C39 H39 119.4 . . ?
C39 C40 C35 118.6(2) . . ?
C39 C40 C44 119.0(2) . . ?
C35 C40 C44 122.40(18) . . ?
C36 C41 C43 110.95(19) . . ?
C36 C41 C42 111.1(2) . . ?
C43 C41 C42 111.0(2) . . ?
C36 C41 H41 107.9 . . ?
C43 C41 H41 107.9 . . ?
C42 C41 H41 107.9 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C40 C44 C46 111.4(2) . . ?
C40 C44 C45 112.2(2) . . ?
C46 C44 C45 111.0(2) . . ?
C40 C44 H44 107.3 . . ?
C46 C44 H44 107.3 . . ?
C45 C44 H44 107.3 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C52 C47 C48 120.74(19) . . ?
C52 C47 C34 120.45(19) . . ?
C48 C47 C34 118.69(18) . . ?
C49 C48 C47 118.7(2) . . ?
C49 C48 C53 119.4(2) . . ?
C47 C48 C53 121.69(19) . . ?
C50 C49 C48 120.5(2) . . ?
C50 C49 H49 119.8 . . ?
C48 C49 H49 119.8 . . ?
C49 C50 C51 120.6(2) . . ?
C49 C50 H50 119.7 . . ?
C51 C50 H50 119.7 . . ?
C50 C51 C52 120.9(2) . . ?
C50 C51 H51 119.5 . . ?
C52 C51 H51 119.5 . . ?
C51 C52 C47 118.4(2) . . ?
C51 C52 C56 119.6(2) . . ?
C47 C52 C56 121.98(19) . . ?
C48 C53 C55 109.7(2) . . ?
C48 C53 C54 114.4(2) . . ?
C55 C53 C54 110.8(2) . . ?
C48 C53 H53 107.2 . . ?
C55 C53 H53 107.2 . . ?
C54 C53 H53 107.2 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C58 C56 C52 114.1(2) . . ?
C58 C56 C57 108.1(2) . . ?
C52 C56 C57 110.9(2) . . ?
C58 C56 H56 107.8 . . ?
C52 C56 H56 107.8 . . ?
C57 C56 H56 107.8 . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C56 C58 H58A 109.5 . . ?
C56 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C56 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 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
C2 N1 C1 C4 -177.4(2) . . . . ?
C5 N1 C1 C4 12.1(4) . . . . ?
C2 N1 C1 N2 1.2(2) . . . . ?
C5 N1 C1 N2 -169.3(2) . . . . ?
C3 N2 C1 C4 177.9(2) . . . . ?
C17 N2 C1 C4 -16.4(4) . . . . ?
C3 N2 C1 N1 -0.8(2) . . . . ?
C17 N2 C1 N1 165.0(2) . . . . ?
C1 N1 C2 C3 -1.2(3) . . . . ?
C5 N1 C2 C3 170.1(2) . . . . ?
N1 C2 C3 N2 0.7(3) . . . . ?
C1 N2 C3 C2 0.1(3) . . . . ?
C17 N2 C3 C2 -166.8(2) . . . . ?
N1 C1 C4 P1 6.0(3) . . . . ?
N2 C1 C4 P1 -172.28(16) . . . . ?
C29 P1 C4 C1 162.34(18) . . . . ?
C1 N1 C5 C6 -109.8(2) . . . . ?
C2 N1 C5 C6 80.6(3) . . . . ?
C1 N1 C5 C10 74.0(3) . . . . ?
C2 N1 C5 C10 -95.6(3) . . . . ?
C10 C5 C6 C7 -0.2(3) . . . . ?
N1 C5 C6 C7 -176.19(18) . . . . ?
C10 C5 C6 C11 -179.40(19) . . . . ?
N1 C5 C6 C11 4.6(3) . . . . ?
C5 C6 C7 C8 -1.4(3) . . . . ?
C11 C6 C7 C8 177.9(2) . . . . ?
C6 C7 C8 C9 1.3(4) . . . . ?
C7 C8 C9 C10 0.4(4) . . . . ?
C8 C9 C10 C5 -1.9(3) . . . . ?
C8 C9 C10 C14A -179.5(3) . . . . ?
C8 C9 C10 C14B 167.1(6) . . . . ?
C6 C5 C10 C9 1.7(3) . . . . ?
N1 C5 C10 C9 177.71(18) . . . . ?
C6 C5 C10 C14A 179.5(3) . . . . ?
N1 C5 C10 C14A -4.5(4) . . . . ?
C6 C5 C10 C14B -165.7(6) . . . . ?
N1 C5 C10 C14B 10.3(6) . . . . ?
C7 C6 C11 C13 69.7(3) . . . . ?
C5 C6 C11 C13 -111.1(2) . . . . ?
C7 C6 C11 C12 -53.6(3) . . . . ?
C5 C6 C11 C12 125.6(2) . . . . ?
C9 C10 C14A C16A 26.4(7) . . . . ?
C5 C10 C14A C16A -151.2(5) . . . . ?
C9 C10 C14A C15A -95.6(4) . . . . ?
C5 C10 C14A C15A 86.7(5) . . . . ?
C9 C10 C14B C16B -35.5(12) . . . . ?
C5 C10 C14B C16B 132.2(9) . . . . ?
C9 C10 C14B C15B 84.1(9) . . . . ?
C5 C10 C14B C15B -108.2(9) . . . . ?
C3 N2 C17 C18 -108.0(3) . . . . ?
C1 N2 C17 C18 87.7(3) . . . . ?
C3 N2 C17 C22 67.3(3) . . . . ?
C1 N2 C17 C22 -97.1(3) . . . . ?
C22 C17 C18 C19 -2.4(3) . . . . ?
N2 C17 C18 C19 172.7(2) . . . . ?
C22 C17 C18 C23 177.7(2) . . . . ?
N2 C17 C18 C23 -7.2(3) . . . . ?
C17 C18 C19 C20 0.3(4) . . . . ?
C23 C18 C19 C20 -179.8(3) . . . . ?
C18 C19 C20 C21 1.5(5) . . . . ?
C19 C20 C21 C22 -1.2(5) . . . . ?
C20 C21 C22 C17 -0.8(4) . . . . ?
C20 C21 C22 C26 176.5(3) . . . . ?
C18 C17 C22 C21 2.6(3) . . . . ?
N2 C17 C22 C21 -172.4(2) . . . . ?
C18 C17 C22 C26 -174.7(2) . . . . ?
N2 C17 C22 C26 10.3(3) . . . . ?
C17 C18 C23 C25 115.2(3) . . . . ?
C19 C18 C23 C25 -64.7(3) . . . . ?
C17 C18 C23 C24 -120.5(2) . . . . ?
C19 C18 C23 C24 59.6(3) . . . . ?
C21 C22 C26 C27 45.1(4) . . . . ?
C17 C22 C26 C27 -137.7(3) . . . . ?
C21 C22 C26 C28 -79.7(3) . . . . ?
C17 C22 C26 C28 97.5(3) . . . . ?
C4 P1 C29 C30 -116.57(15) . . . . ?
C4 P1 C29 C34 70.59(17) . . . . ?
C34 C29 C30 C31 -5.7(3) . . . . ?
P1 C29 C30 C31 -178.76(14) . . . . ?
C34 C29 C30 C35 167.24(18) . . . . ?
P1 C29 C30 C35 -5.9(3) . . . . ?
C29 C30 C31 C32 2.5(3) . . . . ?
C35 C30 C31 C32 -171.12(19) . . . . ?
C30 C31 C32 C33 2.3(3) . . . . ?
C31 C32 C33 C34 -3.9(3) . . . . ?
C32 C33 C34 C29 0.6(3) . . . . ?
C32 C33 C34 C47 175.37(19) . . . . ?
C30 C29 C34 C33 4.1(3) . . . . ?
P1 C29 C34 C33 177.00(15) . . . . ?
C30 C29 C34 C47 -170.33(18) . . . . ?
P1 C29 C34 C47 2.5(3) . . . . ?
C31 C30 C35 C36 -77.2(2) . . . . ?
C29 C30 C35 C36 109.6(2) . . . . ?
C31 C30 C35 C40 94.2(2) . . . . ?
C29 C30 C35 C40 -79.0(2) . . . . ?
C40 C35 C36 C37 -3.3(3) . . . . ?
C30 C35 C36 C37 167.88(18) . . . . ?
C40 C35 C36 C41 176.4(2) . . . . ?
C30 C35 C36 C41 -12.4(3) . . . . ?
C35 C36 C37 C38 1.2(3) . . . . ?
C41 C36 C37 C38 -178.5(2) . . . . ?
C36 C37 C38 C39 2.1(4) . . . . ?
C37 C38 C39 C40 -3.3(4) . . . . ?
C38 C39 C40 C35 1.3(4) . . . . ?
C38 C39 C40 C44 -177.6(3) . . . . ?
C36 C35 C40 C39 2.1(3) . . . . ?
C30 C35 C40 C39 -169.3(2) . . . . ?
C36 C35 C40 C44 -179.1(2) . . . . ?
C30 C35 C40 C44 9.5(3) . . . . ?
C37 C36 C41 C43 58.9(3) . . . . ?
C35 C36 C41 C43 -120.9(2) . . . . ?
C37 C36 C41 C42 -65.2(3) . . . . ?
C35 C36 C41 C42 115.1(2) . . . . ?
C39 C40 C44 C46 74.3(3) . . . . ?
C35 C40 C44 C46 -104.4(3) . . . . ?
C39 C40 C44 C45 -50.8(3) . . . . ?
C35 C40 C44 C45 130.4(2) . . . . ?
C33 C34 C47 C52 77.5(2) . . . . ?
C29 C34 C47 C52 -107.9(2) . . . . ?
C33 C34 C47 C48 -98.4(2) . . . . ?
C29 C34 C47 C48 76.1(2) . . . . ?
C52 C47 C48 C49 4.0(3) . . . . ?
C34 C47 C48 C49 179.96(18) . . . . ?
C52 C47 C48 C53 -170.52(19) . . . . ?
C34 C47 C48 C53 5.4(3) . . . . ?
C47 C48 C49 C50 -1.1(3) . . . . ?
C53 C48 C49 C50 173.6(2) . . . . ?
C48 C49 C50 C51 -2.0(4) . . . . ?
C49 C50 C51 C52 2.2(4) . . . . ?
C50 C51 C52 C47 0.7(3) . . . . ?
C50 C51 C52 C56 -176.3(2) . . . . ?
C48 C47 C52 C51 -3.8(3) . . . . ?
C34 C47 C52 C51 -179.70(18) . . . . ?
C48 C47 C52 C56 173.15(19) . . . . ?
C34 C47 C52 C56 -2.7(3) . . . . ?
C49 C48 C53 C55 -79.4(3) . . . . ?
C47 C48 C53 C55 95.1(3) . . . . ?
C49 C48 C53 C54 45.8(3) . . . . ?
C47 C48 C53 C54 -139.7(2) . . . . ?
C51 C52 C56 C58 -41.7(3) . . . . ?
C47 C52 C56 C58 141.3(2) . . . . ?
C51 C52 C56 C57 80.7(3) . . . . ?
C47 C52 C56 C57 -96.3(2) . . . . ?

_refine_diff_density_max         0.370
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.035


####################################################################### 
# 
# 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_ax1912_TerPIiPr2_cmp10
_database_code_depnum_ccdc_archive 'CCDC 2046861'
loop_
_audit_author_name
_audit_author_address
'Hering-Junghans C.'
;LIKAT Rostock
Germany
;
_audit_update_record             
;
2020-11-27 deposited with the CCDC.	2021-01-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

#==============================================================================

# CHEMICAL DATA
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H41 N2 P'
_chemical_formula_sum            'C33 H41 N2 P'
_chemical_formula_weight         496.65

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

#==============================================================================

# CRYSTAL DATA

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

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

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

_cell_length_a                   8.324(2)
_cell_length_b                   10.832(3)
_cell_length_c                   16.967(4)
_cell_angle_alpha                80.3487(38)
_cell_angle_beta                 76.2360(36)
_cell_angle_gamma                73.6442(37)
_cell_volume                     1417.3(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2484
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      24.23

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_F_000             536
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.121
_shelx_estimated_absorpt_T_min   0.982
_shelx_estimated_absorpt_T_max   0.992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.967
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?

#==============================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19377
_diffrn_reflns_av_unetI/netI     0.0797
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.971
_diffrn_reflns_theta_max         27.500
_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             6496
_reflns_number_gt                4010
_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       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms 
 were positioned geometrically and refined using a riding model, with C---H = 
 0.98 (methyl groups), 0.99Å (methylene groups), 1.00Å (methine groups) or 
 0.95 Å (aryl CH) and with Uiso(H) = 1.5 times Ueq(C) 
 (methyl groups) or with Uiso(H) = 1.2 times Ueq(C) 
 (methylene  groups, aryl CH, methine groups). Torsion angles of all methyl 
 groups were allowed to refine.
 
 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 > 2σ(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     
'w=1/[σ²(Fo²)+(0.0705P)²+0.0020P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6496
_refine_ls_number_parameters     335
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0559
_refine_ls_wR_factor_ref         0.1467
_refine_ls_wR_factor_gt          0.1242
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.49065(8) 0.45736(6) 0.72510(4) 0.02905(17) Uani 1 1 d . . . . .
N1 N 0.4870(2) 0.20389(17) 0.72154(11) 0.0308(4) Uani 1 1 d . . . . .
N2 N 0.2699(2) 0.33426(17) 0.67681(11) 0.0302(4) Uani 1 1 d . . . . .
C6 C 0.2967(3) 0.6997(2) 0.76577(12) 0.0269(5) Uani 1 1 d . . . . .
C16 C 0.4331(3) 0.74710(19) 0.70362(13) 0.0278(5) Uani 1 1 d . . . . .
C1 C 0.3051(3) 0.5658(2) 0.78257(12) 0.0258(5) Uani 1 1 d . . . . .
C7 C 0.1952(3) 0.3857(2) 0.88059(12) 0.0268(5) Uani 1 1 d . . . . .
C8 C 0.3196(3) 0.3175(2) 0.92647(12) 0.0283(5) Uani 1 1 d . . . . .
C25 C 0.4050(3) 0.3307(2) 0.71101(12) 0.0275(5) Uani 1 1 d . . . . .
C2 C 0.1836(3) 0.5255(2) 0.84904(12) 0.0272(5) Uani 1 1 d . . . . .
C12 C 0.0759(3) 0.3234(2) 0.87026(13) 0.0294(5) Uani 1 1 d . . . . .
C17 C 0.4089(3) 0.7957(2) 0.62427(13) 0.0312(5) Uani 1 1 d . . . . .
C9 C 0.3290(3) 0.1884(2) 0.95476(13) 0.0318(5) Uani 1 1 d . . . . .
H9 H 0.4124 0.1433 0.9862 0.038 Uiso 1 1 calc R U . . .
C11 C 0.0943(3) 0.1927(2) 0.89761(13) 0.0321(5) Uani 1 1 d . . . . .
H11 H 0.0167 0.1503 0.8875 0.039 Uiso 1 1 calc R U . . .
C19 C 0.6965(3) 0.8269(2) 0.58701(14) 0.0337(5) Uani 1 1 d . . . . .
C10 C 0.2209(3) 0.1226(2) 0.93883(13) 0.0316(5) Uani 1 1 d . . . . .
C21 C 0.5873(3) 0.74216(19) 0.72515(13) 0.0285(5) Uani 1 1 d . . . . .
C20 C 0.7167(3) 0.7807(2) 0.66660(14) 0.0318(5) Uani 1 1 d . . . . .
H20 H 0.8219 0.7754 0.6813 0.038 Uiso 1 1 calc R U . . .
C3 C 0.0532(3) 0.6184(2) 0.89066(13) 0.0343(5) Uani 1 1 d . . . . .
H3 H -0.0304 0.5911 0.9334 0.041 Uiso 1 1 calc R U . . .
C4 C 0.0428(3) 0.7488(2) 0.87123(14) 0.0381(6) Uani 1 1 d . . . . .
H4 H -0.0478 0.8106 0.8998 0.046 Uiso 1 1 calc R U . . .
C5 C 0.1652(3) 0.7888(2) 0.80989(14) 0.0335(5) Uani 1 1 d . . . . .
H5 H 0.1599 0.8785 0.7975 0.040 Uiso 1 1 calc R U . . .
C31 C 0.1742(3) 0.4530(2) 0.63354(14) 0.0360(6) Uani 1 1 d . . . . .
H31 H 0.1478 0.5261 0.6674 0.043 Uiso 1 1 calc R U . . .
C24 C 0.6128(3) 0.6959(2) 0.81129(14) 0.0361(6) Uani 1 1 d . . . . .
H24A H 0.7258 0.7013 0.8158 0.054 Uiso 1 1 calc R U . . .
H24B H 0.6049 0.6060 0.8249 0.054 Uiso 1 1 calc R U . . .
H24C H 0.5243 0.7504 0.8491 0.054 Uiso 1 1 calc R U . . .
C26 C 0.4047(3) 0.1287(2) 0.69440(14) 0.0374(6) Uani 1 1 d . . . . .
H26 H 0.4374 0.0372 0.6950 0.045 Uiso 1 1 calc R U . . .
C18 C 0.5408(3) 0.8347(2) 0.56796(14) 0.0351(6) Uani 1 1 d . . . . .
H18 H 0.5237 0.8680 0.5143 0.042 Uiso 1 1 calc R U . . .
C28 C 0.6469(3) 0.1547(2) 0.75193(15) 0.0368(6) Uani 1 1 d . . . . .
H28 H 0.6514 0.2184 0.7872 0.044 Uiso 1 1 calc R U . . .
C27 C 0.2709(3) 0.2098(2) 0.66741(14) 0.0376(6) Uani 1 1 d . . . . .
H27 H 0.1903 0.1862 0.6455 0.045 Uiso 1 1 calc R U . . .
C13 C 0.4386(3) 0.3844(2) 0.94679(14) 0.0383(6) Uani 1 1 d . . . . .
H13A H 0.5073 0.3254 0.9838 0.057 Uiso 1 1 calc R U . . .
H13B H 0.3716 0.4618 0.9732 0.057 Uiso 1 1 calc R U . . .
H13C H 0.5143 0.4093 0.8965 0.057 Uiso 1 1 calc R U . . .
C15 C -0.0779(3) 0.3964(2) 0.83508(16) 0.0423(6) Uani 1 1 d . . . . .
H15A H -0.1146 0.3372 0.8094 0.063 Uiso 1 1 calc R U . . .
H15B H -0.0486 0.4661 0.7941 0.063 Uiso 1 1 calc R U . . .
H15C H -0.1709 0.4334 0.8788 0.063 Uiso 1 1 calc R U . . .
C14 C 0.2409(3) -0.0196(2) 0.96644(16) 0.0422(6) Uani 1 1 d . . . . .
H14A H 0.1394 -0.0445 0.9616 0.063 Uiso 1 1 calc R U . . .
H14B H 0.2537 -0.0370 1.0235 0.063 Uiso 1 1 calc R U . . .
H14C H 0.3424 -0.0698 0.9322 0.063 Uiso 1 1 calc R U . . .
C22 C 0.2417(3) 0.8061(3) 0.60098(16) 0.0439(6) Uani 1 1 d . . . . .
H22A H 0.1544 0.8784 0.6256 0.066 Uiso 1 1 calc R U . . .
H22B H 0.2064 0.7255 0.6207 0.066 Uiso 1 1 calc R U . . .
H22C H 0.2555 0.8213 0.5414 0.066 Uiso 1 1 calc R U . . .
C30 C 0.6568(4) 0.0262(2) 0.80315(16) 0.0447(7) Uani 1 1 d . . . . .
H30A H 0.5563 0.0330 0.8477 0.067 Uiso 1 1 calc R U . . .
H30B H 0.7606 0.0015 0.8259 0.067 Uiso 1 1 calc R U . . .
H30C H 0.6601 -0.0396 0.7692 0.067 Uiso 1 1 calc R U . . .
C32 C 0.0071(3) 0.4379(3) 0.61997(16) 0.0466(7) Uani 1 1 d . . . . .
H32A H 0.0313 0.3780 0.5788 0.070 Uiso 1 1 calc R U . . .
H32B H -0.0614 0.5224 0.6010 0.070 Uiso 1 1 calc R U . . .
H32C H -0.0564 0.4036 0.6714 0.070 Uiso 1 1 calc R U . . .
C23 C 0.8395(4) 0.8675(3) 0.52467(16) 0.0470(7) Uani 1 1 d . . . . .
H23A H 0.7962 0.9133 0.4760 0.071 Uiso 1 1 calc R U . . .
H23B H 0.9311 0.7907 0.5096 0.071 Uiso 1 1 calc R U . . .
H23C H 0.8842 0.9249 0.5478 0.071 Uiso 1 1 calc R U . . .
C33 C 0.2892(4) 0.4847(3) 0.55268(15) 0.0486(7) Uani 1 1 d . . . . .
H33A H 0.3944 0.4969 0.5630 0.073 Uiso 1 1 calc R U . . .
H33B H 0.2295 0.5643 0.5240 0.073 Uiso 1 1 calc R U . . .
H33C H 0.3177 0.4134 0.5190 0.073 Uiso 1 1 calc R U . . .
C29 C 0.7973(3) 0.1496(3) 0.67980(18) 0.0561(8) Uani 1 1 d . . . . .
H29A H 0.7956 0.0883 0.6437 0.084 Uiso 1 1 calc R U . . .
H29B H 0.9045 0.1215 0.6998 0.084 Uiso 1 1 calc R U . . .
H29C H 0.7884 0.2359 0.6495 0.084 Uiso 1 1 calc R U . . .


#==============================================================================

# MOLECULAR GEOMETRY

_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 C25 1.786(2) . ?
P1 C1 1.833(2) . ?
N1 C25 1.354(3) . ?
N1 C26 1.391(3) . ?
N1 C28 1.468(3) . ?
N2 C25 1.372(3) . ?
N2 C27 1.381(3) . ?
N2 C31 1.488(3) . ?
C6 C5 1.395(3) . ?
C6 C1 1.415(3) . ?
C6 C16 1.497(3) . ?
C16 C17 1.401(3) . ?
C16 C21 1.401(3) . ?
C1 C2 1.423(3) . ?
C7 C12 1.404(3) . ?
C7 C8 1.409(3) . ?
C7 C2 1.502(3) . ?
C8 C9 1.387(3) . ?
C8 C13 1.508(3) . ?
C2 C3 1.396(3) . ?
C12 C11 1.391(3) . ?
C12 C15 1.502(3) . ?
C17 C18 1.387(3) . ?
C17 C22 1.504(3) . ?
C9 C10 1.390(3) . ?
C9 H9 0.9500 . ?
C11 C10 1.378(3) . ?
C11 H11 0.9500 . ?
C19 C18 1.385(3) . ?
C19 C20 1.392(3) . ?
C19 C23 1.506(3) . ?
C10 C14 1.507(3) . ?
C21 C20 1.388(3) . ?
C21 C24 1.508(3) . ?
C20 H20 0.9500 . ?
C3 C4 1.378(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.379(3) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C31 C32 1.519(4) . ?
C31 C33 1.522(3) . ?
C31 H31 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C26 C27 1.334(3) . ?
C26 H26 0.9500 . ?
C18 H18 0.9500 . ?
C28 C30 1.504(3) . ?
C28 C29 1.524(4) . ?
C28 H28 1.0000 . ?
C27 H27 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C25 P1 C1 102.90(10) . . ?
C25 N1 C26 110.36(19) . . ?
C25 N1 C28 124.35(19) . . ?
C26 N1 C28 125.16(18) . . ?
C25 N2 C27 109.42(19) . . ?
C25 N2 C31 123.66(19) . . ?
C27 N2 C31 124.32(19) . . ?
C5 C6 C1 120.2(2) . . ?
C5 C6 C16 119.09(19) . . ?
C1 C6 C16 120.62(18) . . ?
C17 C16 C21 119.6(2) . . ?
C17 C16 C6 121.0(2) . . ?
C21 C16 C6 119.43(19) . . ?
C6 C1 C2 117.94(19) . . ?
C6 C1 P1 116.28(16) . . ?
C2 C1 P1 125.23(16) . . ?
C12 C7 C8 118.7(2) . . ?
C12 C7 C2 121.14(19) . . ?
C8 C7 C2 120.0(2) . . ?
C9 C8 C7 119.2(2) . . ?
C9 C8 C13 120.0(2) . . ?
C7 C8 C13 120.7(2) . . ?
N1 C25 N2 105.26(18) . . ?
N1 C25 P1 122.85(17) . . ?
N2 C25 P1 131.07(17) . . ?
C3 C2 C1 119.5(2) . . ?
C3 C2 C7 117.6(2) . . ?
C1 C2 C7 122.80(18) . . ?
C11 C12 C7 119.5(2) . . ?
C11 C12 C15 118.8(2) . . ?
C7 C12 C15 121.5(2) . . ?
C18 C17 C16 119.0(2) . . ?
C18 C17 C22 120.7(2) . . ?
C16 C17 C22 120.3(2) . . ?
C8 C9 C10 122.4(2) . . ?
C8 C9 H9 118.8 . . ?
C10 C9 H9 118.8 . . ?
C10 C11 C12 122.3(2) . . ?
C10 C11 H11 118.8 . . ?
C12 C11 H11 118.8 . . ?
C18 C19 C20 117.6(2) . . ?
C18 C19 C23 121.8(2) . . ?
C20 C19 C23 120.6(2) . . ?
C11 C10 C9 117.4(2) . . ?
C11 C10 C14 121.5(2) . . ?
C9 C10 C14 121.1(2) . . ?
C20 C21 C16 119.5(2) . . ?
C20 C21 C24 120.1(2) . . ?
C16 C21 C24 120.4(2) . . ?
C21 C20 C19 121.8(2) . . ?
C21 C20 H20 119.1 . . ?
C19 C20 H20 119.1 . . ?
C4 C3 C2 121.6(2) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C3 C4 C5 119.4(2) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C4 C5 C6 121.1(2) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
N2 C31 C32 112.3(2) . . ?
N2 C31 C33 108.31(19) . . ?
C32 C31 C33 110.9(2) . . ?
N2 C31 H31 108.4 . . ?
C32 C31 H31 108.4 . . ?
C33 C31 H31 108.4 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C27 C26 N1 106.7(2) . . ?
C27 C26 H26 126.6 . . ?
N1 C26 H26 126.6 . . ?
C19 C18 C17 122.5(2) . . ?
C19 C18 H18 118.7 . . ?
C17 C18 H18 118.7 . . ?
N1 C28 C30 112.7(2) . . ?
N1 C28 C29 108.9(2) . . ?
C30 C28 C29 112.1(2) . . ?
N1 C28 H28 107.6 . . ?
C30 C28 H28 107.6 . . ?
C29 C28 H28 107.6 . . ?
C26 C27 N2 108.2(2) . . ?
C26 C27 H27 125.9 . . ?
N2 C27 H27 125.9 . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C19 C23 H23A 109.5 . . ?
C19 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C19 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 C6 C16 C17 -83.9(3) . . . . ?
C1 C6 C16 C17 99.1(2) . . . . ?
C5 C6 C16 C21 96.4(2) . . . . ?
C1 C6 C16 C21 -80.6(3) . . . . ?
C5 C6 C1 C2 -4.4(3) . . . . ?
C16 C6 C1 C2 172.46(18) . . . . ?
C5 C6 C1 P1 -176.37(16) . . . . ?
C16 C6 C1 P1 0.5(3) . . . . ?
C25 P1 C1 C6 -145.75(16) . . . . ?
C25 P1 C1 C2 43.0(2) . . . . ?
C12 C7 C8 C9 4.8(3) . . . . ?
C2 C7 C8 C9 -179.68(19) . . . . ?
C12 C7 C8 C13 -173.55(19) . . . . ?
C2 C7 C8 C13 2.0(3) . . . . ?
C26 N1 C25 N2 0.0(2) . . . . ?
C28 N1 C25 N2 175.97(19) . . . . ?
C26 N1 C25 P1 -170.74(16) . . . . ?
C28 N1 C25 P1 5.3(3) . . . . ?
C27 N2 C25 N1 0.3(2) . . . . ?
C31 N2 C25 N1 -162.06(19) . . . . ?
C27 N2 C25 P1 169.96(17) . . . . ?
C31 N2 C25 P1 7.6(3) . . . . ?
C1 P1 C25 N1 -136.19(18) . . . . ?
C1 P1 C25 N2 55.7(2) . . . . ?
C6 C1 C2 C3 5.3(3) . . . . ?
P1 C1 C2 C3 176.39(16) . . . . ?
C6 C1 C2 C7 -170.71(19) . . . . ?
P1 C1 C2 C7 0.4(3) . . . . ?
C12 C7 C2 C3 72.9(3) . . . . ?
C8 C7 C2 C3 -102.5(2) . . . . ?
C12 C7 C2 C1 -111.0(2) . . . . ?
C8 C7 C2 C1 73.5(3) . . . . ?
C8 C7 C12 C11 -6.9(3) . . . . ?
C2 C7 C12 C11 177.65(19) . . . . ?
C8 C7 C12 C15 169.2(2) . . . . ?
C2 C7 C12 C15 -6.3(3) . . . . ?
C21 C16 C17 C18 1.7(3) . . . . ?
C6 C16 C17 C18 -177.95(19) . . . . ?
C21 C16 C17 C22 -177.8(2) . . . . ?
C6 C16 C17 C22 2.5(3) . . . . ?
C7 C8 C9 C10 0.7(3) . . . . ?
C13 C8 C9 C10 179.1(2) . . . . ?
C7 C12 C11 C10 3.6(3) . . . . ?
C15 C12 C11 C10 -172.6(2) . . . . ?
C12 C11 C10 C9 1.9(3) . . . . ?
C12 C11 C10 C14 -178.7(2) . . . . ?
C8 C9 C10 C11 -4.1(3) . . . . ?
C8 C9 C10 C14 176.5(2) . . . . ?
C17 C16 C21 C20 -2.6(3) . . . . ?
C6 C16 C21 C20 177.15(18) . . . . ?
C17 C16 C21 C24 177.19(19) . . . . ?
C6 C16 C21 C24 -3.1(3) . . . . ?
C16 C21 C20 C19 1.3(3) . . . . ?
C24 C21 C20 C19 -178.4(2) . . . . ?
C18 C19 C20 C21 0.7(3) . . . . ?
C23 C19 C20 C21 -179.7(2) . . . . ?
C1 C2 C3 C4 -2.7(3) . . . . ?
C7 C2 C3 C4 173.5(2) . . . . ?
C2 C3 C4 C5 -0.8(4) . . . . ?
C3 C4 C5 C6 1.7(4) . . . . ?
C1 C6 C5 C4 1.0(3) . . . . ?
C16 C6 C5 C4 -175.9(2) . . . . ?
C25 N2 C31 C32 -166.2(2) . . . . ?
C27 N2 C31 C32 34.0(3) . . . . ?
C25 N2 C31 C33 71.0(3) . . . . ?
C27 N2 C31 C33 -88.8(3) . . . . ?
C25 N1 C26 C27 -0.3(3) . . . . ?
C28 N1 C26 C27 -176.2(2) . . . . ?
C20 C19 C18 C17 -1.5(3) . . . . ?
C23 C19 C18 C17 178.9(2) . . . . ?
C16 C17 C18 C19 0.3(3) . . . . ?
C22 C17 C18 C19 179.9(2) . . . . ?
C25 N1 C28 C30 145.8(2) . . . . ?
C26 N1 C28 C30 -38.8(3) . . . . ?
C25 N1 C28 C29 -89.0(3) . . . . ?
C26 N1 C28 C29 86.4(3) . . . . ?
N1 C26 C27 N2 0.5(3) . . . . ?
C25 N2 C27 C26 -0.5(3) . . . . ?
C31 N2 C27 C26 161.7(2) . . . . ?

_refine_diff_density_max         0.405
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.054

####################################################################### 
# 
# 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_ax1871_MesStarPHC3H3IDip_cmp17
_database_code_depnum_ccdc_archive 'CCDC 2046866'
loop_
_audit_author_name
_audit_author_address
'Hering-Junghans C.'
;LIKAT Rostock
Germany
;
_audit_update_record             
;
2020-11-27 deposited with the CCDC.	2021-01-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H69 N2 P'
_chemical_formula_sum            'C48 H69 N2 P'
_chemical_formula_weight         705.02

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#==============================================================================

# CRYSTAL DATA

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

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

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

_cell_length_a                   10.4692(4)
_cell_length_b                   18.3677(7)
_cell_length_c                   23.4081(9)
_cell_angle_alpha                90
_cell_angle_beta                 100.562(2)
_cell_angle_gamma                90
_cell_volume                     4425.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9855
_cell_measurement_theta_min      3.84
_cell_measurement_theta_max      66.63

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.058
_exptl_crystal_F_000             1544
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.776
_shelx_estimated_absorpt_T_min   0.873
_shelx_estimated_absorpt_T_max   0.948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?

#==============================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         microfocus
_diffrn_radiation_monochromator  multilayer
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36806
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.078
_diffrn_reflns_theta_max         66.667
_diffrn_reflns_theta_full        66.667
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             7781
_reflns_number_gt                7065
_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       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms 
 were positioned geometrically and refined using a riding model, with C---H = 
 0.98 (methyl groups), 0.99Å (methylene groups), 1.00Å (methine groups) or 
 0.95 Å (aryl CH) and with Uiso(H) = 1.5 times Ueq(C) 
 (methyl groups) or with Uiso(H) = 1.2 times Ueq(C) 
 (methylene  groups, aryl CH, methine groups). Torsion angles of all methyl 
 groups were allowed to refine. One of the iPr groups (C28-C30) was found to be
 disordered and was split in two parts and the occupancy of each part was 
 allowed to refine freely. The proton on P1 is disordered about two positions
 which could be located and the occupancies were set to 0.5/0.5. A minor
 orientation of the PHC3H3 in its trans-configuration could not be sufficiently
 modelled, however, its occupancy is estimated to be ca. 8%.
 
 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 > 2σ(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     
'w=1/[σ²(Fo²)+(0.0674P)²+2.3717P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7781
_refine_ls_number_parameters     509
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0496
_refine_ls_wR_factor_ref         0.1369
_refine_ls_wR_factor_gt          0.1326
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.58490(5) 0.27133(2) 0.47903(2) 0.03501(14) Uani 1 1 d . . . . .
N1 N 0.60762(13) 0.09617(7) 0.67034(6) 0.0278(3) Uani 1 1 d . . . . .
N2 N 0.66795(13) 0.19490(7) 0.72027(6) 0.0275(3) Uani 1 1 d . . . . .
C1 C 0.63256(15) 0.16948(8) 0.66373(7) 0.0256(3) Uani 1 1 d . . . . .
C2 C 0.66387(17) 0.13812(9) 0.75977(7) 0.0317(4) Uani 1 1 d . . . . .
H2 H 0.6846 0.1416 0.8009 0.038 Uiso 1 1 calc R U . . .
C3 C 0.62580(17) 0.07844(9) 0.72926(7) 0.0320(4) Uani 1 1 d . . . . .
H3 H 0.6132 0.0318 0.7448 0.038 Uiso 1 1 calc R U . . .
C4 C 0.62123(16) 0.20485(9) 0.61122(7) 0.0298(3) Uani 1 1 d . . . . .
H4 H 0.5992 0.1754 0.5775 0.036 Uiso 1 1 calc R U . . .
C5 C 0.63862(17) 0.28032(9) 0.60140(7) 0.0323(4) Uani 1 1 d . . . . .
H5 H 0.6623 0.3097 0.6351 0.039 Uiso 1 1 calc R U . . .
C6 C 0.62524(18) 0.31509(9) 0.54959(7) 0.0344(4) Uani 1 1 d . . . . .
H6 H 0.6380 0.3663 0.5502 0.041 Uiso 1 1 calc R U . . .
C7 C 0.71804(16) 0.26580(8) 0.73728(7) 0.0274(3) Uani 1 1 d . . . . .
C8 C 0.84902(17) 0.27988(9) 0.73692(7) 0.0322(4) Uani 1 1 d . . . . .
C9 C 0.89454(19) 0.34959(11) 0.75222(8) 0.0409(4) Uani 1 1 d . . . . .
H9 H 0.9832 0.3610 0.7526 0.049 Uiso 1 1 calc R U . . .
C10 C 0.8125(2) 0.40238(10) 0.76685(9) 0.0436(4) Uani 1 1 d . . . . .
H10 H 0.8448 0.4501 0.7762 0.052 Uiso 1 1 calc R U . . .
C11 C 0.68451(19) 0.38678(10) 0.76810(8) 0.0387(4) Uani 1 1 d . . . . .
H11 H 0.6300 0.4236 0.7790 0.046 Uiso 1 1 calc R U . . .
C12 C 0.63371(17) 0.31775(9) 0.75355(7) 0.0306(4) Uani 1 1 d . . . . .
C13 C 0.93846(18) 0.22200(10) 0.71952(8) 0.0379(4) Uani 1 1 d . . . . .
H13 H 0.8818 0.1812 0.7015 0.045 Uiso 1 1 calc R U . . .
C14 C 1.0285(3) 0.19083(19) 0.77153(11) 0.0883(11) Uani 1 1 d . . . . .
H14A H 1.0785 0.1507 0.7590 0.132 Uiso 1 1 calc R U . . .
H14B H 0.9774 0.1727 0.7997 0.132 Uiso 1 1 calc R U . . .
H14C H 1.0881 0.2289 0.7897 0.132 Uiso 1 1 calc R U . . .
C15 C 1.0101(3) 0.24988(16) 0.67402(12) 0.0720(8) Uani 1 1 d . . . . .
H15A H 1.0748 0.2859 0.6914 0.108 Uiso 1 1 calc R U . . .
H15B H 0.9484 0.2727 0.6426 0.108 Uiso 1 1 calc R U . . .
H15C H 1.0538 0.2093 0.6584 0.108 Uiso 1 1 calc R U . . .
C16 C 0.49194(17) 0.30016(10) 0.75298(8) 0.0371(4) Uani 1 1 d . . . . .
H16 H 0.4856 0.2464 0.7588 0.045 Uiso 1 1 calc R U . . .
C17 C 0.4099(2) 0.31819(15) 0.69391(10) 0.0590(6) Uani 1 1 d . . . . .
H17A H 0.4167 0.3703 0.6861 0.088 Uiso 1 1 calc R U . . .
H17B H 0.3189 0.3057 0.6940 0.088 Uiso 1 1 calc R U . . .
H17C H 0.4413 0.2901 0.6637 0.088 Uiso 1 1 calc R U . . .
C18 C 0.4388(2) 0.33744(13) 0.80200(10) 0.0553(6) Uani 1 1 d . . . . .
H18A H 0.4960 0.3272 0.8392 0.083 Uiso 1 1 calc R U . . .
H18B H 0.3514 0.3189 0.8030 0.083 Uiso 1 1 calc R U . . .
H18C H 0.4347 0.3901 0.7953 0.083 Uiso 1 1 calc R U . . .
C19 C 0.55344(15) 0.04638(8) 0.62530(7) 0.0260(3) Uani 1 1 d . . . . .
C20 C 0.41951(16) 0.04898(9) 0.60386(7) 0.0316(4) Uani 1 1 d . . . . .
C21 C 0.36677(19) -0.00482(11) 0.56487(8) 0.0426(4) Uani 1 1 d . . . . .
H21 H 0.2761 -0.0047 0.5498 0.051 Uiso 1 1 calc R U . . .
C22 C 0.4432(2) -0.05800(10) 0.54786(8) 0.0464(5) Uani 1 1 d . . . . .
H22 H 0.4047 -0.0948 0.5218 0.056 Uiso 1 1 calc R U . . .
C23 C 0.5752(2) -0.05878(10) 0.56813(8) 0.0426(5) Uani 1 1 d . . . . .
H23 H 0.6270 -0.0956 0.5552 0.051 Uiso 1 1 calc R U . . .
C24 C 0.63412(17) -0.00629(9) 0.60729(7) 0.0331(4) Uani 1 1 d . . . . .
C25 C 0.33362(18) 0.10731(11) 0.62323(9) 0.0405(4) Uani 1 1 d . . . . .
H25 H 0.3921 0.1444 0.6458 0.049 Uiso 1 1 calc R U . . .
C26 C 0.2508(3) 0.14631(16) 0.57227(11) 0.0703(7) Uani 1 1 d . . . . .
H26A H 0.3068 0.1658 0.5467 0.106 Uiso 1 1 calc R U . . .
H26B H 0.2036 0.1863 0.5868 0.106 Uiso 1 1 calc R U . . .
H26C H 0.1885 0.1119 0.5505 0.106 Uiso 1 1 calc R U . . .
C27 C 0.2509(2) 0.07468(15) 0.66418(12) 0.0670(7) Uani 1 1 d . . . . .
H27A H 0.1940 0.0370 0.6437 0.101 Uiso 1 1 calc R U . . .
H27B H 0.1979 0.1130 0.6773 0.101 Uiso 1 1 calc R U . . .
H27C H 0.3077 0.0531 0.6979 0.101 Uiso 1 1 calc R U . . .
C28A C 0.7777(6) -0.0081(3) 0.6300(3) 0.0399(11) Uani 0.783(12) 1 d . . P A 1
H28A H 0.7935 0.0027 0.6726 0.048 Uiso 0.783(12) 1 calc R U P A 1
C29A C 0.8408(4) -0.0820(2) 0.6205(3) 0.0593(13) Uani 0.783(12) 1 d . . P A 1
H29A H 0.7962 -0.1209 0.6378 0.089 Uiso 0.783(12) 1 calc R U P A 1
H29B H 0.9327 -0.0812 0.6390 0.089 Uiso 0.783(12) 1 calc R U P A 1
H29C H 0.8336 -0.0910 0.5788 0.089 Uiso 0.783(12) 1 calc R U P A 1
C30A C 0.8439(5) 0.0508(2) 0.5993(2) 0.0443(10) Uani 0.783(12) 1 d . . P A 1
H30A H 0.8310 0.0401 0.5577 0.066 Uiso 0.783(12) 1 calc R U P A 1
H30B H 0.9372 0.0516 0.6155 0.066 Uiso 0.783(12) 1 calc R U P A 1
H30C H 0.8060 0.0984 0.6053 0.066 Uiso 0.783(12) 1 calc R U P A 1
C28B C 0.792(3) 0.0081(15) 0.6241(13) 0.0399(11) Uani 0.217(12) 1 d . . P A 2
H28B H 0.8026 0.0484 0.6533 0.048 Uiso 0.217(12) 1 calc R U P A 2
C29B C 0.8562(19) 0.0334(18) 0.5772(10) 0.079(7) Uani 0.217(12) 1 d . . P A 2
H29D H 0.9482 0.0428 0.5927 0.118 Uiso 0.217(12) 1 calc R U P A 2
H29E H 0.8147 0.0783 0.5604 0.118 Uiso 0.217(12) 1 calc R U P A 2
H29F H 0.8491 -0.0041 0.5469 0.118 Uiso 0.217(12) 1 calc R U P A 2
C30B C 0.8538(10) -0.0593(9) 0.6571(9) 0.057(5) Uani 0.217(12) 1 d . . P A 2
H30D H 0.8307 -0.1028 0.6333 0.086 Uiso 0.217(12) 1 calc R U P A 2
H30E H 0.8218 -0.0642 0.6937 0.086 Uiso 0.217(12) 1 calc R U P A 2
H30F H 0.9485 -0.0536 0.6653 0.086 Uiso 0.217(12) 1 calc R U P A 2
C31 C 0.66733(16) 0.33728(9) 0.43744(7) 0.0280(3) Uani 1 1 d . . . . .
C32 C 0.60320(16) 0.40234(9) 0.41393(7) 0.0281(3) Uani 1 1 d . . . . .
C33 C 0.67979(16) 0.45920(9) 0.39974(7) 0.0300(3) Uani 1 1 d . . . . .
H33 H 0.6379 0.5030 0.3851 0.036 Uiso 1 1 calc R U . . .
C34 C 0.81380(16) 0.45524(9) 0.40578(7) 0.0307(4) Uani 1 1 d . . . . .
C35 C 0.87152(16) 0.38880(9) 0.42224(7) 0.0310(4) Uani 1 1 d . . . . .
H35 H 0.9623 0.3838 0.4234 0.037 Uiso 1 1 calc R U . . .
C36 C 0.80247(16) 0.32881(9) 0.43720(7) 0.0288(3) Uani 1 1 d . . . . .
C37 C 0.45289(16) 0.41311(10) 0.40045(7) 0.0330(4) Uani 1 1 d . . . . .
C38 C 0.39243(19) 0.42057(12) 0.45562(9) 0.0447(5) Uani 1 1 d . . . . .
H38A H 0.4244 0.4652 0.4764 0.067 Uiso 1 1 calc R U . . .
H38B H 0.4170 0.3784 0.4809 0.067 Uiso 1 1 calc R U . . .
H38C H 0.2976 0.4228 0.4446 0.067 Uiso 1 1 calc R U . . .
C39 C 0.38897(18) 0.35068(12) 0.36152(9) 0.0442(5) Uani 1 1 d . . . . .
H39A H 0.2943 0.3566 0.3545 0.066 Uiso 1 1 calc R U . . .
H39B H 0.4124 0.3040 0.3809 0.066 Uiso 1 1 calc R U . . .
H39C H 0.4195 0.3518 0.3244 0.066 Uiso 1 1 calc R U . . .
C40 C 0.41364(19) 0.48297(12) 0.36504(10) 0.0476(5) Uani 1 1 d . . . . .
H40A H 0.4498 0.4817 0.3293 0.071 Uiso 1 1 calc R U . . .
H40B H 0.4475 0.5256 0.3882 0.071 Uiso 1 1 calc R U . . .
H40C H 0.3187 0.4860 0.3552 0.071 Uiso 1 1 calc R U . . .
C41 C 0.89153(18) 0.52156(10) 0.39098(8) 0.0379(4) Uani 1 1 d . . . . .
C42 C 0.8592(2) 0.53459(11) 0.32550(9) 0.0465(5) Uani 1 1 d . . . . .
H42A H 0.8832 0.4916 0.3051 0.070 Uiso 1 1 calc R U . . .
H42B H 0.9077 0.5769 0.3156 0.070 Uiso 1 1 calc R U . . .
H42C H 0.7658 0.5436 0.3138 0.070 Uiso 1 1 calc R U . . .
C43 C 1.0382(2) 0.51114(13) 0.40904(12) 0.0614(6) Uani 1 1 d . . . . .
H43A H 1.0594 0.5006 0.4508 0.092 Uiso 1 1 calc R U . . .
H43B H 1.0829 0.5557 0.4007 0.092 Uiso 1 1 calc R U . . .
H43C H 1.0662 0.4704 0.3873 0.092 Uiso 1 1 calc R U . . .
C44 C 0.8532(2) 0.58937(11) 0.42265(9) 0.0478(5) Uani 1 1 d . . . . .
H44A H 0.7597 0.5980 0.4111 0.072 Uiso 1 1 calc R U . . .
H44B H 0.9011 0.6317 0.4123 0.072 Uiso 1 1 calc R U . . .
H44C H 0.8745 0.5815 0.4647 0.072 Uiso 1 1 calc R U . . .
C45 C 0.87934(17) 0.25620(9) 0.45072(7) 0.0336(4) Uani 1 1 d . . . . .
C46 C 0.8129(2) 0.19585(10) 0.41041(9) 0.0449(5) Uani 1 1 d . . . . .
H46A H 0.8590 0.1498 0.4201 0.067 Uiso 1 1 calc R U . . .
H46B H 0.8149 0.2086 0.3699 0.067 Uiso 1 1 calc R U . . .
H46C H 0.7225 0.1907 0.4155 0.067 Uiso 1 1 calc R U . . .
C47 C 0.8959(2) 0.23394(11) 0.51500(8) 0.0432(5) Uani 1 1 d . . . . .
H47A H 0.8108 0.2221 0.5244 0.065 Uiso 1 1 calc R U . . .
H47B H 0.9348 0.2743 0.5396 0.065 Uiso 1 1 calc R U . . .
H47C H 0.9527 0.1912 0.5220 0.065 Uiso 1 1 calc R U . . .
C48 C 1.01889(19) 0.26191(11) 0.43873(9) 0.0451(5) Uani 1 1 d . . . . .
H48A H 1.0611 0.2142 0.4445 0.068 Uiso 1 1 calc R U . . .
H48B H 1.0681 0.2972 0.4655 0.068 Uiso 1 1 calc R U . . .
H48C H 1.0162 0.2780 0.3986 0.068 Uiso 1 1 calc R U . . .
H1A H 0.462(3) 0.2830(16) 0.4624(13) 0.010(7) Uiso 0.5 1 d . . P . .
H1B H 0.655(5) 0.211(3) 0.485(2) 0.061(14) Uiso 0.5 1 d . . P . .


#==============================================================================

# MOLECULAR GEOMETRY

_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 C6 1.8157(18) . ?
P1 C31 1.8623(16) . ?
P1 H1A 1.30(3) . ?
P1 H1B 1.31(5) . ?
N1 C1 1.386(2) . ?
N1 C3 1.396(2) . ?
N1 C19 1.432(2) . ?
N2 C1 1.388(2) . ?
N2 C2 1.400(2) . ?
N2 C7 1.433(2) . ?
C1 C4 1.376(2) . ?
C2 C3 1.329(2) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 C5 1.422(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.355(2) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.397(2) . ?
C7 C12 1.399(2) . ?
C8 C9 1.390(3) . ?
C8 C13 1.521(2) . ?
C9 C10 1.379(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.376(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.393(2) . ?
C11 H11 0.9500 . ?
C12 C16 1.517(2) . ?
C13 C15 1.501(3) . ?
C13 C14 1.509(3) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.524(3) . ?
C16 C18 1.526(3) . ?
C16 H16 1.0000 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C24 1.399(2) . ?
C19 C20 1.401(2) . ?
C20 C21 1.389(3) . ?
C20 C25 1.520(2) . ?
C21 C22 1.367(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.377(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.394(3) . ?
C23 H23 0.9500 . ?
C24 C28A 1.501(7) . ?
C24 C28B 1.65(3) . ?
C25 C26 1.520(3) . ?
C25 C27 1.527(3) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28A C30A 1.531(6) . ?
C28A C29A 1.544(7) . ?
C28A H28A 1.0000 . ?
C29A H29A 0.9800 . ?
C29A H29B 0.9800 . ?
C29A H29C 0.9800 . ?
C30A H30A 0.9800 . ?
C30A H30B 0.9800 . ?
C30A H30C 0.9800 . ?
C28B C29B 1.47(3) . ?
C28B C30B 1.54(3) . ?
C28B H28B 1.0000 . ?
C29B H29D 0.9800 . ?
C29B H29E 0.9800 . ?
C29B H29F 0.9800 . ?
C30B H30D 0.9800 . ?
C30B H30E 0.9800 . ?
C30B H30F 0.9800 . ?
C31 C36 1.424(2) . ?
C31 C32 1.431(2) . ?
C32 C33 1.393(2) . ?
C32 C37 1.560(2) . ?
C33 C34 1.386(2) . ?
C33 H33 0.9500 . ?
C34 C35 1.385(2) . ?
C34 C41 1.539(2) . ?
C35 C36 1.397(2) . ?
C35 H35 0.9500 . ?
C36 C45 1.560(2) . ?
C37 C39 1.539(3) . ?
C37 C40 1.542(3) . ?
C37 C38 1.545(2) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.527(3) . ?
C41 C43 1.528(3) . ?
C41 C44 1.540(3) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.537(3) . ?
C45 C47 1.538(2) . ?
C45 C48 1.541(3) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 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
C6 P1 C31 97.74(8) . . ?
C6 P1 H1A 104.6(13) . . ?
C31 P1 H1A 105.5(13) . . ?
C6 P1 H1B 104(2) . . ?
C31 P1 H1B 108(2) . . ?
H1A P1 H1B 132(3) . . ?
C1 N1 C3 110.04(13) . . ?
C1 N1 C19 126.56(13) . . ?
C3 N1 C19 122.85(13) . . ?
C1 N2 C2 110.12(13) . . ?
C1 N2 C7 126.22(13) . . ?
C2 N2 C7 123.20(13) . . ?
C4 C1 N1 124.84(15) . . ?
C4 C1 N2 131.08(15) . . ?
N1 C1 N2 104.08(13) . . ?
C3 C2 N2 107.58(14) . . ?
C3 C2 H2 126.2 . . ?
N2 C2 H2 126.2 . . ?
C2 C3 N1 108.16(14) . . ?
C2 C3 H3 125.9 . . ?
N1 C3 H3 125.9 . . ?
C1 C4 C5 127.72(16) . . ?
C1 C4 H4 116.1 . . ?
C5 C4 H4 116.1 . . ?
C6 C5 C4 127.50(16) . . ?
C6 C5 H5 116.3 . . ?
C4 C5 H5 116.3 . . ?
C5 C6 P1 125.03(13) . . ?
C5 C6 H6 117.5 . . ?
P1 C6 H6 117.5 . . ?
C8 C7 C12 122.98(15) . . ?
C8 C7 N2 118.44(14) . . ?
C12 C7 N2 118.58(15) . . ?
C9 C8 C7 117.36(16) . . ?
C9 C8 C13 120.94(16) . . ?
C7 C8 C13 121.69(15) . . ?
C10 C9 C8 120.79(17) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C11 C10 C9 120.79(17) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C10 C11 C12 120.93(17) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C11 C12 C7 117.11(16) . . ?
C11 C12 C16 121.68(15) . . ?
C7 C12 C16 121.17(15) . . ?
C15 C13 C14 112.5(2) . . ?
C15 C13 C8 111.33(17) . . ?
C14 C13 C8 111.92(16) . . ?
C15 C13 H13 106.9 . . ?
C14 C13 H13 106.9 . . ?
C8 C13 H13 106.9 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C12 C16 C17 110.46(16) . . ?
C12 C16 C18 112.89(16) . . ?
C17 C16 C18 111.21(17) . . ?
C12 C16 H16 107.3 . . ?
C17 C16 H16 107.3 . . ?
C18 C16 H16 107.3 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C24 C19 C20 122.38(15) . . ?
C24 C19 N1 118.94(14) . . ?
C20 C19 N1 118.52(14) . . ?
C21 C20 C19 117.54(16) . . ?
C21 C20 C25 120.77(16) . . ?
C19 C20 C25 121.68(16) . . ?
C22 C21 C20 121.08(18) . . ?
C22 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C21 C22 C23 120.73(17) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 H22 119.6 . . ?
C22 C23 C24 120.97(17) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C23 C24 C19 117.24(16) . . ?
C23 C24 C28A 120.8(3) . . ?
C19 C24 C28A 122.0(3) . . ?
C23 C24 C28B 124.8(11) . . ?
C19 C24 C28B 116.8(11) . . ?
C26 C25 C20 112.45(17) . . ?
C26 C25 C27 111.72(19) . . ?
C20 C25 C27 110.18(16) . . ?
C26 C25 H25 107.4 . . ?
C20 C25 H25 107.4 . . ?
C27 C25 H25 107.4 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 C28A C30A 109.2(4) . . ?
C24 C28A C29A 113.3(4) . . ?
C30A C28A C29A 108.2(4) . . ?
C24 C28A H28A 108.7 . . ?
C30A C28A H28A 108.7 . . ?
C29A C28A H28A 108.7 . . ?
C28A C29A H29A 109.5 . . ?
C28A C29A H29B 109.5 . . ?
H29A C29A H29B 109.5 . . ?
C28A C29A H29C 109.5 . . ?
H29A C29A H29C 109.5 . . ?
H29B C29A H29C 109.5 . . ?
C28A C30A H30A 109.5 . . ?
C28A C30A H30B 109.5 . . ?
H30A C30A H30B 109.5 . . ?
C28A C30A H30C 109.5 . . ?
H30A C30A H30C 109.5 . . ?
H30B C30A H30C 109.5 . . ?
C29B C28B C30B 115(2) . . ?
C29B C28B C24 116.9(19) . . ?
C30B C28B C24 107.7(15) . . ?
C29B C28B H28B 105.5 . . ?
C30B C28B H28B 105.5 . . ?
C24 C28B H28B 105.5 . . ?
C28B C29B H29D 109.5 . . ?
C28B C29B H29E 109.5 . . ?
H29D C29B H29E 109.5 . . ?
C28B C29B H29F 109.5 . . ?
H29D C29B H29F 109.5 . . ?
H29E C29B H29F 109.5 . . ?
C28B C30B H30D 109.5 . . ?
C28B C30B H30E 109.5 . . ?
H30D C30B H30E 109.5 . . ?
C28B C30B H30F 109.5 . . ?
H30D C30B H30F 109.5 . . ?
H30E C30B H30F 109.5 . . ?
C36 C31 C32 119.09(14) . . ?
C36 C31 P1 119.13(12) . . ?
C32 C31 P1 120.98(12) . . ?
C33 C32 C31 117.89(15) . . ?
C33 C32 C37 117.39(14) . . ?
C31 C32 C37 124.66(14) . . ?
C34 C33 C32 123.53(15) . . ?
C34 C33 H33 118.2 . . ?
C32 C33 H33 118.2 . . ?
C35 C34 C33 117.17(15) . . ?
C35 C34 C41 122.57(15) . . ?
C33 C34 C41 120.17(15) . . ?
C34 C35 C36 123.04(15) . . ?
C34 C35 H35 118.5 . . ?
C36 C35 H35 118.5 . . ?
C35 C36 C31 118.35(15) . . ?
C35 C36 C45 116.98(15) . . ?
C31 C36 C45 124.64(14) . . ?
C39 C37 C40 104.92(15) . . ?
C39 C37 C38 111.14(15) . . ?
C40 C37 C38 105.42(15) . . ?
C39 C37 C32 109.77(14) . . ?
C40 C37 C32 111.96(14) . . ?
C38 C37 C32 113.26(14) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 C43 108.92(18) . . ?
C42 C41 C34 108.71(15) . . ?
C43 C41 C34 112.61(15) . . ?
C42 C41 C44 109.09(16) . . ?
C43 C41 C44 107.77(18) . . ?
C34 C41 C44 109.68(15) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 C47 111.47(16) . . ?
C46 C45 C48 105.95(15) . . ?
C47 C45 C48 104.80(15) . . ?
C46 C45 C36 109.48(14) . . ?
C47 C45 C36 112.78(14) . . ?
C48 C45 C36 112.08(14) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 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
C3 N1 C1 C4 -178.69(15) . . . . ?
C19 N1 C1 C4 -7.0(3) . . . . ?
C3 N1 C1 N2 0.82(17) . . . . ?
C19 N1 C1 N2 172.47(14) . . . . ?
C2 N2 C1 C4 179.29(17) . . . . ?
C7 N2 C1 C4 -8.3(3) . . . . ?
C2 N2 C1 N1 -0.17(17) . . . . ?
C7 N2 C1 N1 172.20(14) . . . . ?
C1 N2 C2 C3 -0.56(19) . . . . ?
C7 N2 C2 C3 -173.21(15) . . . . ?
N2 C2 C3 N1 1.05(19) . . . . ?
C1 N1 C3 C2 -1.21(19) . . . . ?
C19 N1 C3 C2 -173.23(15) . . . . ?
N1 C1 C4 C5 176.42(16) . . . . ?
N2 C1 C4 C5 -2.9(3) . . . . ?
C1 C4 C5 C6 -178.81(17) . . . . ?
C4 C5 C6 P1 -1.7(3) . . . . ?
C31 P1 C6 C5 -151.86(16) . . . . ?
C1 N2 C7 C8 -79.1(2) . . . . ?
C2 N2 C7 C8 92.34(19) . . . . ?
C1 N2 C7 C12 100.95(18) . . . . ?
C2 N2 C7 C12 -87.6(2) . . . . ?
C12 C7 C8 C9 -1.6(2) . . . . ?
N2 C7 C8 C9 178.46(15) . . . . ?
C12 C7 C8 C13 179.44(16) . . . . ?
N2 C7 C8 C13 -0.5(2) . . . . ?
C7 C8 C9 C10 -0.3(3) . . . . ?
C13 C8 C9 C10 178.69(17) . . . . ?
C8 C9 C10 C11 1.7(3) . . . . ?
C9 C10 C11 C12 -1.3(3) . . . . ?
C10 C11 C12 C7 -0.5(3) . . . . ?
C10 C11 C12 C16 -178.20(17) . . . . ?
C8 C7 C12 C11 2.0(2) . . . . ?
N2 C7 C12 C11 -178.06(15) . . . . ?
C8 C7 C12 C16 179.67(15) . . . . ?
N2 C7 C12 C16 -0.4(2) . . . . ?
C9 C8 C13 C15 -50.3(3) . . . . ?
C7 C8 C13 C15 128.7(2) . . . . ?
C9 C8 C13 C14 76.6(3) . . . . ?
C7 C8 C13 C14 -104.5(2) . . . . ?
C11 C12 C16 C17 87.6(2) . . . . ?
C7 C12 C16 C17 -89.9(2) . . . . ?
C11 C12 C16 C18 -37.6(2) . . . . ?
C7 C12 C16 C18 144.83(17) . . . . ?
C1 N1 C19 C24 107.69(18) . . . . ?
C3 N1 C19 C24 -81.7(2) . . . . ?
C1 N1 C19 C20 -76.8(2) . . . . ?
C3 N1 C19 C20 93.82(19) . . . . ?
C24 C19 C20 C21 2.2(2) . . . . ?
N1 C19 C20 C21 -173.08(15) . . . . ?
C24 C19 C20 C25 -179.06(15) . . . . ?
N1 C19 C20 C25 5.6(2) . . . . ?
C19 C20 C21 C22 -0.4(3) . . . . ?
C25 C20 C21 C22 -179.13(17) . . . . ?
C20 C21 C22 C23 -1.3(3) . . . . ?
C21 C22 C23 C24 1.2(3) . . . . ?
C22 C23 C24 C19 0.5(3) . . . . ?
C22 C23 C24 C28A 179.0(3) . . . . ?
C22 C23 C24 C28B -167.1(10) . . . . ?
C20 C19 C24 C23 -2.3(2) . . . . ?
N1 C19 C24 C23 173.00(14) . . . . ?
C20 C19 C24 C28A 179.3(3) . . . . ?
N1 C19 C24 C28A -5.5(3) . . . . ?
C20 C19 C24 C28B 166.3(10) . . . . ?
N1 C19 C24 C28B -18.4(10) . . . . ?
C21 C20 C25 C26 -53.1(2) . . . . ?
C19 C20 C25 C26 128.2(2) . . . . ?
C21 C20 C25 C27 72.2(2) . . . . ?
C19 C20 C25 C27 -106.4(2) . . . . ?
C23 C24 C28A C30A 103.9(4) . . . . ?
C19 C24 C28A C30A -77.7(5) . . . . ?
C23 C24 C28A C29A -16.7(6) . . . . ?
C19 C24 C28A C29A 161.7(4) . . . . ?
C23 C24 C28B C29B 64(3) . . . . ?
C19 C24 C28B C29B -104(3) . . . . ?
C23 C24 C28B C30B -67(2) . . . . ?
C19 C24 C28B C30B 125.3(16) . . . . ?
C6 P1 C31 C36 84.75(14) . . . . ?
C6 P1 C31 C32 -84.95(14) . . . . ?
C36 C31 C32 C33 -9.4(2) . . . . ?
P1 C31 C32 C33 160.31(12) . . . . ?
C36 C31 C32 C37 167.80(15) . . . . ?
P1 C31 C32 C37 -22.5(2) . . . . ?
C31 C32 C33 C34 1.7(2) . . . . ?
C37 C32 C33 C34 -175.65(15) . . . . ?
C32 C33 C34 C35 5.5(2) . . . . ?
C32 C33 C34 C41 -177.96(16) . . . . ?
C33 C34 C35 C36 -5.3(2) . . . . ?
C41 C34 C35 C36 178.31(16) . . . . ?
C34 C35 C36 C31 -2.2(2) . . . . ?
C34 C35 C36 C45 175.96(15) . . . . ?
C32 C31 C36 C35 9.6(2) . . . . ?
P1 C31 C36 C35 -160.24(12) . . . . ?
C32 C31 C36 C45 -168.41(15) . . . . ?
P1 C31 C36 C45 21.7(2) . . . . ?
C33 C32 C37 C39 124.08(17) . . . . ?
C31 C32 C37 C39 -53.1(2) . . . . ?
C33 C32 C37 C40 8.0(2) . . . . ?
C31 C32 C37 C40 -169.22(16) . . . . ?
C33 C32 C37 C38 -111.05(18) . . . . ?
C31 C32 C37 C38 71.7(2) . . . . ?
C35 C34 C41 C42 108.26(19) . . . . ?
C33 C34 C41 C42 -68.1(2) . . . . ?
C35 C34 C41 C43 -12.5(3) . . . . ?
C33 C34 C41 C43 171.15(18) . . . . ?
C35 C34 C41 C44 -132.54(18) . . . . ?
C33 C34 C41 C44 51.1(2) . . . . ?
C35 C36 C45 C46 -123.22(17) . . . . ?
C31 C36 C45 C46 54.9(2) . . . . ?
C35 C36 C45 C47 112.04(18) . . . . ?
C31 C36 C45 C47 -69.9(2) . . . . ?
C35 C36 C45 C48 -6.0(2) . . . . ?
C31 C36 C45 C48 172.12(16) . . . . ?

_refine_diff_density_max         1.065
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.044

####################################################################### 
# 
# 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_ax1913_TerPHC3H3IDip_cmp18
_database_code_depnum_ccdc_archive 'CCDC 2046867'
loop_
_audit_author_name
_audit_author_address
'Hering-Junghans C.'
;LIKAT Rostock
Germany
;
_audit_update_record             
;
2020-11-27 deposited with the CCDC.	2021-01-13 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H65 N2 P, 0.5 (C6 H14)'
_chemical_formula_sum            'C57 H72 N2 P'
_chemical_formula_weight         816.13

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

#==============================================================================

# CRYSTAL DATA

_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                   9.0953(9)
_cell_length_b                   12.8174(12)
_cell_length_c                   22.854(2)
_cell_angle_alpha                86.172(3)
_cell_angle_beta                 87.117(3)
_cell_angle_gamma                69.713(3)
_cell_volume                     2492.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9932
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      29.79

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_F_000             886
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.092
_shelx_estimated_absorpt_T_min   0.973
_shelx_estimated_absorpt_T_max   0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014)'

#==============================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            102569
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.696
_diffrn_reflns_theta_max         30.000
_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             14514
_reflns_number_gt                10677
_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.
 
 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.
;

_computing_data_collection       'Bruker Apex V7.51A'
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms 
 were positioned geometrically and refined using a riding model, with C---H = 
 0.98 (methyl groups), 0.99Å (methylene groups), 1.00Å (methine groups) or 
 0.95 Å (aryl CH) and with Uiso(H) = 1.5 times Ueq(C) 
 (methyl groups) or with Uiso(H) = 1.2 times Ueq(C) 
 (methylene  groups, aryl CH, methine groups). Torsion angles of all methyl 
 groups were allowed to refine. One of the o-mesityl groups in the terphenyl
 moiety was found to be disordered and was split in two parts.
 The occupancy of each part was allowed to refine freely. 

 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 > 2σ(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.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.023 0.000 0.500 235 48 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The unit cell contains one disordered n-hexane molecule. This 
has been treated as a diffuse contribution to the overall scattering 
without specific atom positions by SQUEEZE/PLATON.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0622P)²+0.6091P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14514
_refine_ls_number_parameters     605
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0473
_refine_ls_wR_factor_ref         0.1346
_refine_ls_wR_factor_gt          0.1201
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.58450(5) 0.45557(3) 0.29700(2) 0.03493(9) Uani 1 1 d . . . . .
N1 N 0.14273(11) 0.88343(8) 0.13866(4) 0.02300(18) Uani 1 1 d . . . . .
N2 N 0.07010(11) 0.85152(8) 0.22881(4) 0.0264(2) Uani 1 1 d . . . . .
C1 C 0.18567(13) 0.80801(9) 0.18666(5) 0.0225(2) Uani 1 1 d . . . . .
C2 C 0.00226(13) 0.96886(10) 0.15130(5) 0.0273(2) Uani 1 1 d . . . . .
H2 H -0.0521 1.0297 0.1254 0.033 Uiso 1 1 calc R U . . .
C3 C -0.04176(14) 0.94936(10) 0.20651(5) 0.0294(2) Uani 1 1 d . . . . .
H3 H -0.1330 0.9942 0.2269 0.035 Uiso 1 1 calc R U . . .
C4 C 0.31857(13) 0.71484(9) 0.18833(5) 0.0246(2) Uani 1 1 d . . . . .
H4 H 0.3837 0.7034 0.1538 0.030 Uiso 1 1 calc R U . . .
C5 C 0.37131(13) 0.63283(9) 0.23549(5) 0.0248(2) Uani 1 1 d . . . . .
H5 H 0.3020 0.6354 0.2683 0.030 Uiso 1 1 calc R U . . .
C6 C 0.51369(14) 0.55216(9) 0.23604(5) 0.0256(2) Uani 1 1 d . . . . .
H6 H 0.5802 0.5463 0.2021 0.031 Uiso 1 1 calc R U . . .
C7 C 0.22316(13) 0.86779(9) 0.08258(5) 0.0225(2) Uani 1 1 d . . . . .
C8 C 0.16254(13) 0.82560(9) 0.03813(5) 0.0251(2) Uani 1 1 d . . . . .
C9 C 0.24602(15) 0.80765(11) -0.01547(5) 0.0304(2) Uani 1 1 d . . . . .
H9 H 0.2084 0.7787 -0.0464 0.036 Uiso 1 1 calc R U . . .
C10 C 0.38273(15) 0.83157(11) -0.02400(5) 0.0319(3) Uani 1 1 d . . . . .
H10 H 0.4380 0.8190 -0.0607 0.038 Uiso 1 1 calc R U . . .
C11 C 0.43990(14) 0.87373(10) 0.02064(5) 0.0293(2) Uani 1 1 d . . . . .
H11 H 0.5338 0.8900 0.0140 0.035 Uiso 1 1 calc R U . . .
C12 C 0.36196(13) 0.89256(9) 0.07504(5) 0.0242(2) Uani 1 1 d . . . . .
C13 C 0.01786(14) 0.79283(10) 0.04926(5) 0.0292(2) Uani 1 1 d . . . . .
H13 H -0.0468 0.8389 0.0812 0.035 Uiso 1 1 calc R U . . .
C14 C -0.08388(16) 0.81464(13) -0.00438(6) 0.0398(3) Uani 1 1 d . . . . .
H14A H -0.1125 0.8931 -0.0180 0.060 Uiso 1 1 calc R U . . .
H14B H -0.1792 0.7976 0.0061 0.060 Uiso 1 1 calc R U . . .
H14C H -0.0253 0.7673 -0.0357 0.060 Uiso 1 1 calc R U . . .
C15 C 0.06688(19) 0.67080(13) 0.07121(8) 0.0475(4) Uani 1 1 d . . . . .
H15A H 0.1259 0.6234 0.0400 0.071 Uiso 1 1 calc R U . . .
H15B H -0.0268 0.6520 0.0824 0.071 Uiso 1 1 calc R U . . .
H15C H 0.1329 0.6587 0.1054 0.071 Uiso 1 1 calc R U . . .
C16 C 0.42236(14) 0.93834(10) 0.12485(5) 0.0271(2) Uani 1 1 d . . . . .
H16 H 0.4008 0.9004 0.1623 0.032 Uiso 1 1 calc R U . . .
C17 C 0.59883(14) 0.91489(12) 0.12006(6) 0.0341(3) Uani 1 1 d . . . . .
H17A H 0.6539 0.8350 0.1159 0.051 Uiso 1 1 calc R U . . .
H17B H 0.6331 0.9378 0.1555 0.051 Uiso 1 1 calc R U . . .
H17C H 0.6229 0.9568 0.0857 0.051 Uiso 1 1 calc R U . . .
C18 C 0.33270(15) 1.06337(11) 0.12898(6) 0.0330(3) Uani 1 1 d . . . . .
H18A H 0.3507 1.1031 0.0927 0.049 Uiso 1 1 calc R U . . .
H18B H 0.3697 1.0907 0.1623 0.049 Uiso 1 1 calc R U . . .
H18C H 0.2203 1.0763 0.1345 0.049 Uiso 1 1 calc R U . . .
C19 C 0.06048(14) 0.80118(10) 0.28617(5) 0.0292(2) Uani 1 1 d . . . . .
C20 C -0.02355(16) 0.72813(11) 0.29376(6) 0.0353(3) Uani 1 1 d . . . . .
C21 C -0.0244(2) 0.67675(14) 0.34960(7) 0.0502(4) Uani 1 1 d . . . . .
H21 H -0.0794 0.6260 0.3564 0.060 Uiso 1 1 calc R U . . .
C22 C 0.0531(2) 0.69852(16) 0.39490(7) 0.0596(5) Uani 1 1 d . . . . .
H22 H 0.0512 0.6626 0.4325 0.072 Uiso 1 1 calc R U . . .
C23 C 0.1335(2) 0.77208(15) 0.38613(7) 0.0547(4) Uani 1 1 d . . . . .
H23 H 0.1854 0.7868 0.4180 0.066 Uiso 1 1 calc R U . . .
C24 C 0.13988(18) 0.82502(12) 0.33139(6) 0.0384(3) Uani 1 1 d . . . . .
C25 C -0.10913(17) 0.70326(13) 0.24443(7) 0.0424(3) Uani 1 1 d . . . . .
H25 H -0.0900 0.7452 0.2081 0.051 Uiso 1 1 calc R U . . .
C26 C -0.0487(2) 0.57973(15) 0.23242(9) 0.0608(5) Uani 1 1 d . . . . .
H26A H 0.0642 0.5555 0.2234 0.091 Uiso 1 1 calc R U . . .
H26B H -0.1031 0.5674 0.1990 0.091 Uiso 1 1 calc R U . . .
H26C H -0.0685 0.5369 0.2672 0.091 Uiso 1 1 calc R U . . .
C27 C -0.28557(19) 0.74362(15) 0.25768(9) 0.0566(4) Uani 1 1 d . . . . .
H27A H -0.3079 0.7014 0.2922 0.085 Uiso 1 1 calc R U . . .
H27B H -0.3397 0.7324 0.2239 0.085 Uiso 1 1 calc R U . . .
H27C H -0.3224 0.8230 0.2654 0.085 Uiso 1 1 calc R U . . .
C28 C 0.2305(2) 0.90478(15) 0.32084(7) 0.0531(4) Uani 1 1 d . . . . .
H28 H 0.2643 0.9033 0.2785 0.064 Uiso 1 1 calc R U . . .
C29 C 0.1255(3) 1.02296(17) 0.33255(11) 0.0832(7) Uani 1 1 d . . . . .
H29A H 0.0927 1.0273 0.3741 0.125 Uiso 1 1 calc R U . . .
H29B H 0.0328 1.0439 0.3083 0.125 Uiso 1 1 calc R U . . .
H29C H 0.1833 1.0740 0.3228 0.125 Uiso 1 1 calc R U . . .
C30 C 0.3773(2) 0.87132(19) 0.35706(9) 0.0688(5) Uani 1 1 d . . . . .
H30A H 0.3471 0.8824 0.3986 0.103 Uiso 1 1 calc R U . . .
H30B H 0.4403 0.9173 0.3440 0.103 Uiso 1 1 calc R U . . .
H30C H 0.4389 0.7927 0.3520 0.103 Uiso 1 1 calc R U . . .
C31 C 0.56949(14) 0.32036(10) 0.28004(5) 0.0269(2) Uani 1 1 d . . . . .
C32 C 0.60673(13) 0.27579(9) 0.22410(5) 0.0262(2) Uani 1 1 d . . . . .
C33 C 0.60204(15) 0.17005(10) 0.21583(5) 0.0303(2) Uani 1 1 d . . . . .
H33 H 0.6263 0.1405 0.1781 0.036 Uiso 1 1 calc R U . . .
C34 C 0.56266(16) 0.10758(10) 0.26168(6) 0.0357(3) Uani 1 1 d . . . . .
H34 H 0.5603 0.0356 0.2555 0.043 Uiso 1 1 calc R U . . .
C35 C 0.52679(17) 0.15057(11) 0.31649(6) 0.0363(3) Uani 1 1 d . . . . .
H35 H 0.4999 0.1076 0.3479 0.044 Uiso 1 1 calc R U . . .
C36 C 0.52940(15) 0.25622(10) 0.32648(5) 0.0311(3) Uani 1 1 d . . . . .
C37 C 0.64382(14) 0.34110(9) 0.17240(5) 0.0264(2) Uani 1 1 d . . . . .
C38 C 0.79392(14) 0.34758(10) 0.16306(5) 0.0293(2) Uani 1 1 d . . . . .
C39 C 0.81892(15) 0.41807(11) 0.11738(6) 0.0326(3) Uani 1 1 d . . . . .
H39 H 0.9207 0.4224 0.1109 0.039 Uiso 1 1 calc R U . . .
C40 C 0.69867(16) 0.48214(11) 0.08102(5) 0.0331(3) Uani 1 1 d . . . . .
C41 C 0.55296(16) 0.47046(11) 0.08926(5) 0.0319(3) Uani 1 1 d . . . . .
H41 H 0.4712 0.5112 0.0637 0.038 Uiso 1 1 calc R U . . .
C42 C 0.52325(14) 0.40063(10) 0.13400(5) 0.0279(2) Uani 1 1 d . . . . .
C43 C 0.92665(16) 0.28306(12) 0.20279(7) 0.0389(3) Uani 1 1 d . . . . .
H43A H 1.0230 0.2955 0.1885 0.058 Uiso 1 1 calc R U . . .
H43B H 0.9423 0.2035 0.2029 0.058 Uiso 1 1 calc R U . . .
H43C H 0.9007 0.3084 0.2428 0.058 Uiso 1 1 calc R U . . .
C44 C 0.7231(2) 0.56617(13) 0.03557(6) 0.0451(3) Uani 1 1 d . . . . .
H44A H 0.6570 0.5724 0.0020 0.068 Uiso 1 1 calc R U . . .
H44B H 0.8335 0.5418 0.0224 0.068 Uiso 1 1 calc R U . . .
H44C H 0.6946 0.6388 0.0528 0.068 Uiso 1 1 calc R U . . .
C45 C 0.36064(15) 0.39609(12) 0.14357(6) 0.0353(3) Uani 1 1 d . . . . .
H45A H 0.2921 0.4437 0.1134 0.053 Uiso 1 1 calc R U . . .
H45B H 0.3196 0.4225 0.1824 0.053 Uiso 1 1 calc R U . . .
H45C H 0.3643 0.3192 0.1412 0.053 Uiso 1 1 calc R U . . .
C46A C 0.4811(19) 0.2996(10) 0.3878(4) 0.032(3) Uani 0.432(14) 1 d . . P A 1
C47A C 0.3102(18) 0.3458(13) 0.3982(7) 0.0293(18) Uani 0.432(14) 1 d . . P A 1
C48A C 0.267(2) 0.388(2) 0.4540(10) 0.047(3) Uani 0.432(14) 1 d . . P A 1
H48A H 0.1582 0.4233 0.4617 0.056 Uiso 0.432(14) 1 calc R U P A 1
C49A C 0.370(2) 0.3828(15) 0.5012(9) 0.048(2) Uani 0.432(14) 1 d . . P A 1
C50A C 0.532(3) 0.338(2) 0.4855(9) 0.048(3) Uani 0.432(14) 1 d . . P A 1
H50A H 0.6090 0.3344 0.5128 0.057 Uiso 0.432(14) 1 calc R U P A 1
C51A C 0.5762(19) 0.2987(15) 0.4292(7) 0.041(3) Uani 0.432(14) 1 d . . P A 1
C52A C 0.1878(15) 0.3512(10) 0.3594(4) 0.050(2) Uani 0.432(14) 1 d . . P A 1
H52A H 0.2346 0.3192 0.3222 0.075 Uiso 0.432(14) 1 calc R U P A 1
H52B H 0.1244 0.3089 0.3775 0.075 Uiso 0.432(14) 1 calc R U P A 1
H52C H 0.1211 0.4290 0.3520 0.075 Uiso 0.432(14) 1 calc R U P A 1
C53A C 0.321(4) 0.428(3) 0.5590(19) 0.093(3) Uani 0.432(14) 1 d . . P A 1
H53A H 0.2063 0.4554 0.5627 0.140 Uiso 0.432(14) 1 calc R U P A 1
H53B H 0.3646 0.3694 0.5895 0.140 Uiso 0.432(14) 1 calc R U P A 1
H53C H 0.3597 0.4895 0.5633 0.140 Uiso 0.432(14) 1 calc R U P A 1
C54A C 0.7626(17) 0.2481(9) 0.4141(6) 0.052(3) Uani 0.432(14) 1 d . . P A 1
H54A H 0.8209 0.2520 0.4483 0.078 Uiso 0.432(14) 1 calc R U P A 1
H54B H 0.7911 0.1703 0.4040 0.078 Uiso 0.432(14) 1 calc R U P A 1
H54C H 0.7887 0.2914 0.3808 0.078 Uiso 0.432(14) 1 calc R U P A 1
C46B C 0.4850(14) 0.2990(8) 0.3849(4) 0.042(3) Uani 0.568(14) 1 d . . P A 2
C47B C 0.3361(17) 0.3447(12) 0.4053(7) 0.046(3) Uani 0.568(14) 1 d . . P A 2
C48B C 0.2933(17) 0.3820(16) 0.4610(7) 0.058(3) Uani 0.568(14) 1 d . . P A 2
H48B H 0.1862 0.4094 0.4736 0.069 Uiso 0.568(14) 1 calc R U P A 2
C49B C 0.4067(19) 0.3786(12) 0.4967(6) 0.060(3) Uani 0.568(14) 1 d . . P A 2
C50B C 0.558(3) 0.3342(16) 0.4793(7) 0.061(4) Uani 0.568(14) 1 d . . P A 2
H50B H 0.6345 0.3327 0.5063 0.073 Uiso 0.568(14) 1 calc R U P A 2
C51B C 0.6115(14) 0.2905(10) 0.4252(4) 0.0359(19) Uani 0.568(14) 1 d . . P A 2
C52B C 0.2079(13) 0.3570(8) 0.3587(4) 0.067(3) Uani 0.568(14) 1 d . . P A 2
H52D H 0.1033 0.3906 0.3767 0.101 Uiso 0.568(14) 1 calc R U P A 2
H52E H 0.2216 0.4047 0.3251 0.101 Uiso 0.568(14) 1 calc R U P A 2
H52F H 0.2193 0.2834 0.3455 0.101 Uiso 0.568(14) 1 calc R U P A 2
C53B C 0.354(3) 0.419(3) 0.5593(15) 0.093(3) Uani 0.568(14) 1 d . . P A 2
H53D H 0.4460 0.4131 0.5816 0.140 Uiso 0.568(14) 1 calc R U P A 2
H53E H 0.2838 0.4971 0.5566 0.140 Uiso 0.568(14) 1 calc R U P A 2
H53F H 0.2981 0.3732 0.5792 0.140 Uiso 0.568(14) 1 calc R U P A 2
C54B C 0.7735(13) 0.2424(9) 0.4084(5) 0.072(3) Uani 0.568(14) 1 d . . P A 2
H54D H 0.7828 0.2173 0.3684 0.108 Uiso 0.568(14) 1 calc R U P A 2
H54E H 0.8244 0.2981 0.4100 0.108 Uiso 0.568(14) 1 calc R U P A 2
H54F H 0.8245 0.1787 0.4354 0.108 Uiso 0.568(14) 1 calc R U P A 2
H1 H 0.466(2) 0.4889(16) 0.3277(8) 0.066(6) Uiso 1 1 d . . . . .


#==============================================================================

# MOLECULAR GEOMETRY

_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 C6 1.7876(12) . ?
P1 C31 1.8523(12) . ?
P1 H1 1.215(19) . ?
N1 C1 1.3893(14) . ?
N1 C2 1.3964(14) . ?
N1 C7 1.4340(14) . ?
N2 C1 1.3812(14) . ?
N2 C3 1.3963(15) . ?
N2 C19 1.4342(15) . ?
C1 C4 1.3734(16) . ?
C2 C3 1.3386(17) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 C5 1.4309(15) . ?
C4 H4 0.9500 . ?
C5 C6 1.3483(16) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.4016(15) . ?
C7 C12 1.4046(15) . ?
C8 C9 1.3975(16) . ?
C8 C13 1.5193(16) . ?
C9 C10 1.3821(17) . ?
C9 H9 0.9500 . ?
C10 C11 1.3874(17) . ?
C10 H10 0.9500 . ?
C11 C12 1.3925(16) . ?
C11 H11 0.9500 . ?
C12 C16 1.5225(15) . ?
C13 C14 1.5252(17) . ?
C13 C15 1.5268(19) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.5267(16) . ?
C16 C18 1.5324(18) . ?
C16 H16 1.0000 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.3972(18) . ?
C19 C24 1.3977(19) . ?
C20 C21 1.397(2) . ?
C20 C25 1.512(2) . ?
C21 C22 1.377(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.380(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.391(2) . ?
C23 H23 0.9500 . ?
C24 C28 1.521(2) . ?
C25 C26 1.524(2) . ?
C25 C27 1.527(2) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.518(3) . ?
C28 C30 1.523(3) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C36 1.4098(17) . ?
C31 C32 1.4127(16) . ?
C32 C33 1.3962(16) . ?
C32 C37 1.4948(16) . ?
C33 C34 1.3845(18) . ?
C33 H33 0.9500 . ?
C34 C35 1.3805(19) . ?
C34 H34 0.9500 . ?
C35 C36 1.3966(18) . ?
C35 H35 0.9500 . ?
C36 C46B 1.461(8) . ?
C36 C46A 1.529(8) . ?
C37 C38 1.4012(17) . ?
C37 C42 1.4079(16) . ?
C38 C39 1.3966(18) . ?
C38 C43 1.5111(18) . ?
C39 C40 1.3923(19) . ?
C39 H39 0.9500 . ?
C40 C41 1.3867(19) . ?
C40 C44 1.5105(18) . ?
C41 C42 1.3919(17) . ?
C41 H41 0.9500 . ?
C42 C45 1.5047(18) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46A C51A 1.31(2) . ?
C46A C47A 1.47(2) . ?
C47A C48A 1.40(3) . ?
C47A C52A 1.44(2) . ?
C48A C49A 1.44(3) . ?
C48A H48A 0.9500 . ?
C49A C50A 1.42(3) . ?
C49A C53A 1.46(5) . ?
C50A C51A 1.40(3) . ?
C50A H50A 0.9500 . ?
C51A C54A 1.619(19) . ?
C52A H52A 0.9800 . ?
C52A H52B 0.9800 . ?
C52A H52C 0.9800 . ?
C53A H53A 0.9800 . ?
C53A H53B 0.9800 . ?
C53A H53C 0.9800 . ?
C54A H54A 0.9800 . ?
C54A H54B 0.9800 . ?
C54A H54C 0.9800 . ?
C46B C47B 1.35(2) . ?
C46B C51B 1.480(15) . ?
C47B C48B 1.38(2) . ?
C47B C52B 1.578(16) . ?
C48B C49B 1.33(2) . ?
C48B H48B 0.9500 . ?
C49B C50B 1.34(2) . ?
C49B C53B 1.55(4) . ?
C50B C51B 1.39(2) . ?
C50B H50B 0.9500 . ?
C51B C54B 1.430(16) . ?
C52B H52D 0.9800 . ?
C52B H52E 0.9800 . ?
C52B H52F 0.9800 . ?
C53B H53D 0.9800 . ?
C53B H53E 0.9800 . ?
C53B H53F 0.9800 . ?
C54B H54D 0.9800 . ?
C54B H54E 0.9800 . ?
C54B H54F 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
C6 P1 C31 108.27(5) . . ?
C6 P1 H1 96.4(9) . . ?
C31 P1 H1 98.1(9) . . ?
C1 N1 C2 110.13(9) . . ?
C1 N1 C7 124.05(9) . . ?
C2 N1 C7 125.49(9) . . ?
C1 N2 C3 110.12(9) . . ?
C1 N2 C19 125.39(10) . . ?
C3 N2 C19 124.41(10) . . ?
C4 C1 N2 131.20(10) . . ?
C4 C1 N1 124.45(10) . . ?
N2 C1 N1 104.32(9) . . ?
C3 C2 N1 107.48(10) . . ?
C3 C2 H2 126.3 . . ?
N1 C2 H2 126.3 . . ?
C2 C3 N2 107.93(10) . . ?
C2 C3 H3 126.0 . . ?
N2 C3 H3 126.0 . . ?
C1 C4 C5 128.19(10) . . ?
C1 C4 H4 115.9 . . ?
C5 C4 H4 115.9 . . ?
C6 C5 C4 123.78(11) . . ?
C6 C5 H5 118.1 . . ?
C4 C5 H5 118.1 . . ?
C5 C6 P1 123.74(9) . . ?
C5 C6 H6 118.1 . . ?
P1 C6 H6 118.1 . . ?
C8 C7 C12 122.75(10) . . ?
C8 C7 N1 118.73(10) . . ?
C12 C7 N1 118.50(9) . . ?
C9 C8 C7 117.57(10) . . ?
C9 C8 C13 121.15(10) . . ?
C7 C8 C13 121.13(10) . . ?
C10 C9 C8 120.75(11) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C9 C10 C11 120.54(11) . . ?
C9 C10 H10 119.7 . . ?
C11 C10 H10 119.7 . . ?
C10 C11 C12 121.11(11) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
C11 C12 C7 117.27(10) . . ?
C11 C12 C16 122.21(10) . . ?
C7 C12 C16 120.51(10) . . ?
C8 C13 C14 112.97(10) . . ?
C8 C13 C15 109.61(10) . . ?
C14 C13 C15 110.96(11) . . ?
C8 C13 H13 107.7 . . ?
C14 C13 H13 107.7 . . ?
C15 C13 H13 107.7 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C12 C16 C17 113.09(10) . . ?
C12 C16 C18 110.59(10) . . ?
C17 C16 C18 110.67(10) . . ?
C12 C16 H16 107.4 . . ?
C17 C16 H16 107.4 . . ?
C18 C16 H16 107.4 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C24 123.18(12) . . ?
C20 C19 N2 118.54(11) . . ?
C24 C19 N2 118.25(11) . . ?
C19 C20 C21 116.95(13) . . ?
C19 C20 C25 122.60(12) . . ?
C21 C20 C25 120.46(13) . . ?
C22 C21 C20 121.08(15) . . ?
C22 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C21 C22 C23 120.55(14) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C22 C23 C24 121.03(15) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C23 C24 C19 117.21(14) . . ?
C23 C24 C28 121.59(14) . . ?
C19 C24 C28 121.20(12) . . ?
C20 C25 C26 111.84(13) . . ?
C20 C25 C27 110.66(13) . . ?
C26 C25 C27 110.50(13) . . ?
C20 C25 H25 107.9 . . ?
C26 C25 H25 107.9 . . ?
C27 C25 H25 107.9 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C24 110.50(16) . . ?
C29 C28 C30 110.39(15) . . ?
C24 C28 C30 112.71(15) . . ?
C29 C28 H28 107.7 . . ?
C24 C28 H28 107.7 . . ?
C30 C28 H28 107.7 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C36 C31 C32 118.94(11) . . ?
C36 C31 P1 117.84(9) . . ?
C32 C31 P1 123.07(9) . . ?
C33 C32 C31 119.57(11) . . ?
C33 C32 C37 118.65(10) . . ?
C31 C32 C37 121.71(10) . . ?
C34 C33 C32 121.12(11) . . ?
C34 C33 H33 119.4 . . ?
C32 C33 H33 119.4 . . ?
C35 C34 C33 119.54(12) . . ?
C35 C34 H34 120.2 . . ?
C33 C34 H34 120.2 . . ?
C34 C35 C36 121.07(12) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 H35 119.5 . . ?
C35 C36 C31 119.76(11) . . ?
C35 C36 C46B 118.7(4) . . ?
C31 C36 C46B 121.5(4) . . ?
C35 C36 C46A 117.7(5) . . ?
C31 C36 C46A 122.5(5) . . ?
C38 C37 C42 119.83(11) . . ?
C38 C37 C32 121.20(11) . . ?
C42 C37 C32 118.92(11) . . ?
C39 C38 C37 119.03(11) . . ?
C39 C38 C43 119.79(12) . . ?
C37 C38 C43 121.15(12) . . ?
C40 C39 C38 121.76(12) . . ?
C40 C39 H39 119.1 . . ?
C38 C39 H39 119.1 . . ?
C41 C40 C39 118.23(12) . . ?
C41 C40 C44 120.47(12) . . ?
C39 C40 C44 121.24(12) . . ?
C40 C41 C42 121.82(12) . . ?
C40 C41 H41 119.1 . . ?
C42 C41 H41 119.1 . . ?
C41 C42 C37 119.17(11) . . ?
C41 C42 C45 119.89(11) . . ?
C37 C42 C45 120.78(11) . . ?
C38 C43 H43A 109.5 . . ?
C38 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C38 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C40 C44 H44A 109.5 . . ?
C40 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C40 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C51A C46A C47A 120.2(11) . . ?
C51A C46A C36 126.1(14) . . ?
C47A C46A C36 113.7(10) . . ?
C48A C47A C52A 118.3(14) . . ?
C48A C47A C46A 113.2(15) . . ?
C52A C47A C46A 128.4(12) . . ?
C47A C48A C49A 127.5(17) . . ?
C47A C48A H48A 116.2 . . ?
C49A C48A H48A 116.2 . . ?
C50A C49A C48A 113.7(17) . . ?
C50A C49A C53A 120(2) . . ?
C48A C49A C53A 126(2) . . ?
C51A C50A C49A 119.1(19) . . ?
C51A C50A H50A 120.5 . . ?
C49A C50A H50A 120.5 . . ?
C46A C51A C50A 126.1(18) . . ?
C46A C51A C54A 117.2(13) . . ?
C50A C51A C54A 116.7(16) . . ?
C47A C52A H52A 109.5 . . ?
C47A C52A H52B 109.5 . . ?
H52A C52A H52B 109.5 . . ?
C47A C52A H52C 109.5 . . ?
H52A C52A H52C 109.5 . . ?
H52B C52A H52C 109.5 . . ?
C49A C53A H53A 109.5 . . ?
C49A C53A H53B 109.5 . . ?
H53A C53A H53B 109.5 . . ?
C49A C53A H53C 109.5 . . ?
H53A C53A H53C 109.5 . . ?
H53B C53A H53C 109.5 . . ?
C51A C54A H54A 109.5 . . ?
C51A C54A H54B 109.5 . . ?
H54A C54A H54B 109.5 . . ?
C51A C54A H54C 109.5 . . ?
H54A C54A H54C 109.5 . . ?
H54B C54A H54C 109.5 . . ?
C47B C46B C36 124.6(10) . . ?
C47B C46B C51B 117.1(9) . . ?
C36 C46B C51B 118.2(9) . . ?
C46B C47B C48B 125.0(13) . . ?
C46B C47B C52B 114.2(11) . . ?
C48B C47B C52B 120.8(12) . . ?
C49B C48B C47B 118.0(13) . . ?
C49B C48B H48B 121.0 . . ?
C47B C48B H48B 121.0 . . ?
C48B C49B C50B 120.1(14) . . ?
C48B C49B C53B 116.4(14) . . ?
C50B C49B C53B 123.4(16) . . ?
C49B C50B C51B 125.7(16) . . ?
C49B C50B H50B 117.1 . . ?
C51B C50B H50B 117.1 . . ?
C50B C51B C54B 124.1(12) . . ?
C50B C51B C46B 113.9(13) . . ?
C54B C51B C46B 121.9(8) . . ?
C47B C52B H52D 109.5 . . ?
C47B C52B H52E 109.5 . . ?
H52D C52B H52E 109.5 . . ?
C47B C52B H52F 109.5 . . ?
H52D C52B H52F 109.5 . . ?
H52E C52B H52F 109.5 . . ?
C49B C53B H53D 109.5 . . ?
C49B C53B H53E 109.5 . . ?
H53D C53B H53E 109.5 . . ?
C49B C53B H53F 109.5 . . ?
H53D C53B H53F 109.5 . . ?
H53E C53B H53F 109.5 . . ?
C51B C54B H54D 109.5 . . ?
C51B C54B H54E 109.5 . . ?
H54D C54B H54E 109.5 . . ?
C51B C54B H54F 109.5 . . ?
H54D C54B H54F 109.5 . . ?
H54E C54B H54F 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
C3 N2 C1 C4 179.35(12) . . . . ?
C19 N2 C1 C4 -3.80(19) . . . . ?
C3 N2 C1 N1 1.30(12) . . . . ?
C19 N2 C1 N1 178.14(10) . . . . ?
C2 N1 C1 C4 -179.69(11) . . . . ?
C7 N1 C1 C4 6.65(17) . . . . ?
C2 N1 C1 N2 -1.46(12) . . . . ?
C7 N1 C1 N2 -175.12(10) . . . . ?
C1 N1 C2 C3 1.10(13) . . . . ?
C7 N1 C2 C3 174.65(10) . . . . ?
N1 C2 C3 N2 -0.26(13) . . . . ?
C1 N2 C3 C2 -0.68(14) . . . . ?
C19 N2 C3 C2 -177.56(11) . . . . ?
N2 C1 C4 C5 2.6(2) . . . . ?
N1 C1 C4 C5 -179.68(11) . . . . ?
C1 C4 C5 C6 -170.82(11) . . . . ?
C4 C5 C6 P1 175.64(9) . . . . ?
C31 P1 C6 C5 103.08(11) . . . . ?
C1 N1 C7 C8 97.95(13) . . . . ?
C2 N1 C7 C8 -74.74(14) . . . . ?
C1 N1 C7 C12 -80.32(14) . . . . ?
C2 N1 C7 C12 107.00(13) . . . . ?
C12 C7 C8 C9 0.28(17) . . . . ?
N1 C7 C8 C9 -177.91(10) . . . . ?
C12 C7 C8 C13 175.99(10) . . . . ?
N1 C7 C8 C13 -2.19(16) . . . . ?
C7 C8 C9 C10 -0.39(18) . . . . ?
C13 C8 C9 C10 -176.11(12) . . . . ?
C8 C9 C10 C11 0.1(2) . . . . ?
C9 C10 C11 C12 0.3(2) . . . . ?
C10 C11 C12 C7 -0.39(18) . . . . ?
C10 C11 C12 C16 179.77(11) . . . . ?
C8 C7 C12 C11 0.11(17) . . . . ?
N1 C7 C12 C11 178.30(10) . . . . ?
C8 C7 C12 C16 179.95(10) . . . . ?
N1 C7 C12 C16 -1.86(16) . . . . ?
C9 C8 C13 C14 -38.26(16) . . . . ?
C7 C8 C13 C14 146.17(12) . . . . ?
C9 C8 C13 C15 86.03(15) . . . . ?
C7 C8 C13 C15 -89.53(14) . . . . ?
C11 C12 C16 C17 -24.52(16) . . . . ?
C7 C12 C16 C17 155.64(11) . . . . ?
C11 C12 C16 C18 100.23(13) . . . . ?
C7 C12 C16 C18 -79.61(13) . . . . ?
C1 N2 C19 C20 -90.33(15) . . . . ?
C3 N2 C19 C20 86.08(15) . . . . ?
C1 N2 C19 C24 87.72(15) . . . . ?
C3 N2 C19 C24 -95.87(15) . . . . ?
C24 C19 C20 C21 -0.8(2) . . . . ?
N2 C19 C20 C21 177.16(12) . . . . ?
C24 C19 C20 C25 179.90(13) . . . . ?
N2 C19 C20 C25 -2.16(19) . . . . ?
C19 C20 C21 C22 0.6(2) . . . . ?
C25 C20 C21 C22 179.94(16) . . . . ?
C20 C21 C22 C23 0.1(3) . . . . ?
C21 C22 C23 C24 -0.7(3) . . . . ?
C22 C23 C24 C19 0.5(3) . . . . ?
C22 C23 C24 C28 -178.93(18) . . . . ?
C20 C19 C24 C23 0.2(2) . . . . ?
N2 C19 C24 C23 -177.72(13) . . . . ?
C20 C19 C24 C28 179.69(14) . . . . ?
N2 C19 C24 C28 1.7(2) . . . . ?
C19 C20 C25 C26 120.43(15) . . . . ?
C21 C20 C25 C26 -58.86(19) . . . . ?
C19 C20 C25 C27 -115.90(15) . . . . ?
C21 C20 C25 C27 64.80(18) . . . . ?
C23 C24 C28 C29 -90.1(2) . . . . ?
C19 C24 C28 C29 90.46(18) . . . . ?
C23 C24 C28 C30 33.9(2) . . . . ?
C19 C24 C28 C30 -145.50(15) . . . . ?
C6 P1 C31 C36 -143.92(10) . . . . ?
C6 P1 C31 C32 40.60(12) . . . . ?
C36 C31 C32 C33 0.46(17) . . . . ?
P1 C31 C32 C33 175.90(9) . . . . ?
C36 C31 C32 C37 177.45(11) . . . . ?
P1 C31 C32 C37 -7.11(16) . . . . ?
C31 C32 C33 C34 -0.51(18) . . . . ?
C37 C32 C33 C34 -177.60(11) . . . . ?
C32 C33 C34 C35 0.3(2) . . . . ?
C33 C34 C35 C36 0.1(2) . . . . ?
C34 C35 C36 C31 -0.1(2) . . . . ?
C34 C35 C36 C46B 177.9(5) . . . . ?
C34 C35 C36 C46A 177.3(7) . . . . ?
C32 C31 C36 C35 -0.15(18) . . . . ?
P1 C31 C36 C35 -175.83(10) . . . . ?
C32 C31 C36 C46B -178.1(6) . . . . ?
P1 C31 C36 C46B 6.2(6) . . . . ?
C32 C31 C36 C46A -177.5(7) . . . . ?
P1 C31 C36 C46A 6.8(7) . . . . ?
C33 C32 C37 C38 -101.06(13) . . . . ?
C31 C32 C37 C38 81.93(15) . . . . ?
C33 C32 C37 C42 81.60(14) . . . . ?
C31 C32 C37 C42 -95.42(14) . . . . ?
C42 C37 C38 C39 3.38(17) . . . . ?
C32 C37 C38 C39 -173.94(11) . . . . ?
C42 C37 C38 C43 -178.86(11) . . . . ?
C32 C37 C38 C43 3.82(17) . . . . ?
C37 C38 C39 C40 0.15(18) . . . . ?
C43 C38 C39 C40 -177.65(12) . . . . ?
C38 C39 C40 C41 -3.17(18) . . . . ?
C38 C39 C40 C44 174.05(12) . . . . ?
C39 C40 C41 C42 2.72(18) . . . . ?
C44 C40 C41 C42 -174.52(12) . . . . ?
C40 C41 C42 C37 0.72(18) . . . . ?
C40 C41 C42 C45 176.19(12) . . . . ?
C38 C37 C42 C41 -3.81(17) . . . . ?
C32 C37 C42 C41 173.57(11) . . . . ?
C38 C37 C42 C45 -179.24(11) . . . . ?
C32 C37 C42 C45 -1.86(17) . . . . ?
C35 C36 C46A C51A 99.7(14) . . . . ?
C31 C36 C46A C51A -82.9(15) . . . . ?
C35 C36 C46A C47A -80.4(11) . . . . ?
C31 C36 C46A C47A 97.0(11) . . . . ?
C51A C46A C47A C48A 1(2) . . . . ?
C36 C46A C47A C48A -178.7(15) . . . . ?
C51A C46A C47A C52A -177.9(16) . . . . ?
C36 C46A C47A C52A 2(2) . . . . ?
C52A C47A C48A C49A 175(2) . . . . ?
C46A C47A C48A C49A -4(3) . . . . ?
C47A C48A C49A C50A 5(4) . . . . ?
C47A C48A C49A C53A 180(3) . . . . ?
C48A C49A C50A C51A -3(3) . . . . ?
C53A C49A C50A C51A -178(2) . . . . ?
C47A C46A C51A C50A 1(3) . . . . ?
C36 C46A C51A C50A -179.6(16) . . . . ?
C47A C46A C51A C54A -179.2(12) . . . . ?
C36 C46A C51A C54A 1(2) . . . . ?
C49A C50A C51A C46A 0(3) . . . . ?
C49A C50A C51A C54A -179.8(16) . . . . ?
C35 C36 C46B C47B -79.8(12) . . . . ?
C31 C36 C46B C47B 98.2(12) . . . . ?
C35 C36 C46B C51B 99.2(9) . . . . ?
C31 C36 C46B C51B -82.8(9) . . . . ?
C36 C46B C47B C48B 177.8(14) . . . . ?
C51B C46B C47B C48B -1(2) . . . . ?
C36 C46B C47B C52B -4.2(17) . . . . ?
C51B C46B C47B C52B 176.8(10) . . . . ?
C46B C47B C48B C49B 4(3) . . . . ?
C52B C47B C48B C49B -174.1(14) . . . . ?
C47B C48B C49B C50B -4(3) . . . . ?
C47B C48B C49B C53B -178.9(18) . . . . ?
C48B C49B C50B C51B 1(3) . . . . ?
C53B C49B C50B C51B 175.9(19) . . . . ?
C49B C50B C51B C54B -179.0(14) . . . . ?
C49B C50B C51B C46B 2(2) . . . . ?
C47B C46B C51B C50B -1.5(17) . . . . ?
C36 C46B C51B C50B 179.5(11) . . . . ?
C47B C46B C51B C54B 179.3(12) . . . . ?
C36 C46B C51B C54B 0.2(15) . . . . ?

_refine_diff_density_max         0.545
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.040


