# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_compound4
_database_code_depnum_ccdc_archive 'CCDC 1883596'
_audit_update_record             
;
2018-12-06 deposited with the CCDC.
2019-01-23 downloaded from the CCDC.
;
_audit_creation_date             2017-10-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C49 H81 P Th'
_chemical_formula_sum            'C49 H81 P Th'
_chemical_formula_weight         933.14
_chemical_melting_point          ?
_chemical_oxdiff_formula         C1H1P1Th1
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'
Th Th -4.1491 12.3296 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   13.8090(3)
_cell_length_b                   21.5866(8)
_cell_length_c                   15.4832(6)
_cell_angle_alpha                90
_cell_angle_beta                 92.980(3)
_cell_angle_gamma                90
_cell_volume                     4609.1(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7058
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.1160
_cell_measurement_theta_min      3.7870
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    10.964
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77309
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0732
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19005
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.566
_diffrn_reflns_theta_min         3.516
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -115.00  37.00   1.00    1.00    --  -39.74   0.00 -90.00  152
  2  ω     81.00 127.00   1.00    1.00    --   39.74-178.00 120.00   46
  3  ω      1.00  39.00   1.00    1.00    --   39.74 -99.00 150.00   38
  4  ω     51.00 140.00   1.00    1.00    --  107.19 -77.00  90.00   89
  5  ω    111.00 176.00   1.00    1.00    --  107.19 125.00 150.00   65
  6  ω     88.00 169.00   1.00    1.00    --  107.19  30.00 -90.00   81
  7  ω    110.00 170.00   1.00    1.00    --  107.19 125.00-150.00   60
  8  ω     34.00 129.00   1.00    1.00    --  107.19 -45.00-180.00   95
  9  ω     49.00 105.00   1.00    1.00    --  107.19-125.00   0.00   56
 10  ω    143.00 170.00   1.00    1.00    --  107.19 125.00  30.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0546458000
_diffrn_orient_matrix_UB_12      -0.0589432000
_diffrn_orient_matrix_UB_13      -0.0254961000
_diffrn_orient_matrix_UB_21      -0.0951810000
_diffrn_orient_matrix_UB_22      -0.0276164000
_diffrn_orient_matrix_UB_23      -0.0396830000
_diffrn_orient_matrix_UB_31      0.0206774000
_diffrn_orient_matrix_UB_32      0.0293268000
_diffrn_orient_matrix_UB_33      -0.0877455000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7613
_reflns_number_total             8988
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         5.980
_refine_diff_density_min         -3.938
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         8988
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0772
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0393P)²+74.7004P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1694
_refine_ls_wR_factor_ref         0.1768
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All P(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C41(H41), C44(H44), C47(H47)
2.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C20(H20), C22(H22), C37(H37), C39(H39)
2.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C17(H17A,H17B,
 H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,
 H49B,H49C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9555(8) 0.4205(6) 0.2668(8) 0.046(3) Uani 1 1 d . . . . .
C2 C 0.9451(8) 0.4870(6) 0.2535(9) 0.048(3) Uani 1 1 d . . . . .
C3 C 0.9007(8) 0.5092(6) 0.3284(8) 0.045(3) Uani 1 1 d . . . . .
H3 H 0.8843 0.5505 0.3373 0.054 Uiso 1 1 calc R . . . .
C4 C 0.8842(8) 0.4601(6) 0.3889(8) 0.046(3) Uani 1 1 d . . . . .
C5 C 0.9150(7) 0.4069(6) 0.3503(9) 0.052(3) Uani 1 1 d . . . . .
H5 H 0.9108 0.3675 0.3740 0.062 Uiso 1 1 calc R . . . .
C6 C 1.0131(8) 0.3690(7) 0.2243(12) 0.064(4) Uani 1 1 d . . . . .
C7 C 1.0124(9) 0.3111(7) 0.2722(11) 0.068(4) Uani 1 1 d . . . . .
H7A H 1.0444 0.3169 0.3281 0.102 Uiso 1 1 calc GR . . . .
H7B H 1.0457 0.2798 0.2411 0.102 Uiso 1 1 calc GR . . . .
H7C H 0.9466 0.2984 0.2789 0.102 Uiso 1 1 calc GR . . . .
C8 C 1.1204(9) 0.3893(7) 0.2236(12) 0.071(5) Uani 1 1 d . . . . .
H8A H 1.1245 0.4286 0.1952 0.106 Uiso 1 1 calc GR . . . .
H8B H 1.1565 0.3590 0.1932 0.106 Uiso 1 1 calc GR . . . .
H8C H 1.1468 0.3928 0.2820 0.106 Uiso 1 1 calc GR . . . .
C9 C 0.9757(10) 0.3558(7) 0.1365(12) 0.076(5) Uani 1 1 d . . . . .
H9A H 0.9496 0.3146 0.1339 0.114 Uiso 1 1 calc GR . . . .
H9B H 1.0273 0.3592 0.0975 0.114 Uiso 1 1 calc GR . . . .
H9C H 0.9256 0.3850 0.1202 0.114 Uiso 1 1 calc GR . . . .
C10 C 0.9910(8) 0.5321(6) 0.1951(8) 0.043(3) Uani 1 1 d . . . . .
C11 C 1.0857(10) 0.5540(8) 0.2335(10) 0.070(4) Uani 1 1 d . . . . .
H11A H 1.0748 0.5824 0.2797 0.105 Uiso 1 1 calc GR . . . .
H11B H 1.1209 0.5746 0.1900 0.105 Uiso 1 1 calc GR . . . .
H11C H 1.1225 0.5193 0.2557 0.105 Uiso 1 1 calc GR . . . .
C12 C 1.0040(10) 0.5103(8) 0.1016(9) 0.069(4) Uani 1 1 d . . . . .
H12A H 1.0400 0.4723 0.1025 0.103 Uiso 1 1 calc GR . . . .
H12B H 1.0384 0.5414 0.0712 0.103 Uiso 1 1 calc GR . . . .
H12C H 0.9415 0.5038 0.0730 0.103 Uiso 1 1 calc GR . . . .
C13 C 0.9243(10) 0.5892(7) 0.1841(12) 0.077(5) Uani 1 1 d . . . . .
H13A H 0.8618 0.5765 0.1606 0.116 Uiso 1 1 calc GR . . . .
H13B H 0.9522 0.6182 0.1454 0.116 Uiso 1 1 calc GR . . . .
H13C H 0.9176 0.6085 0.2393 0.116 Uiso 1 1 calc GR . . . .
C14 C 0.8200(7) 0.4640(5) 0.4660(7) 0.037(2) Uani 1 1 d . . . . .
C15 C 0.8344(12) 0.5267(7) 0.5104(9) 0.070(4) Uani 1 1 d . . . . .
H15A H 0.9018 0.5324 0.5268 0.105 Uiso 1 1 calc GR . . . .
H15B H 0.7971 0.5281 0.5611 0.105 Uiso 1 1 calc GR . . . .
H15C H 0.8132 0.5591 0.4713 0.105 Uiso 1 1 calc GR . . . .
C16 C 0.7183(8) 0.4591(7) 0.4227(8) 0.053(4) Uani 1 1 d . . . . .
H16A H 0.6813 0.4965 0.4326 0.064 Uiso 1 1 calc R . . . .
H16B H 0.6839 0.4240 0.4452 0.064 Uiso 1 1 calc R . . . .
C17 C 0.8454(11) 0.4138(7) 0.5304(10) 0.067(4) Uani 1 1 d . . . . .
H17A H 0.8465 0.3746 0.5011 0.100 Uiso 1 1 calc GR . . . .
H17B H 0.7977 0.4126 0.5733 0.100 Uiso 1 1 calc GR . . . .
H17C H 0.9080 0.4219 0.5577 0.100 Uiso 1 1 calc GR . . . .
C18 C 0.5956(8) 0.5371(5) 0.2394(8) 0.044(3) Uani 1 1 d . . . . .
C19 C 0.5390(8) 0.4806(6) 0.2380(8) 0.043(3) Uani 1 1 d . . . . .
C20 C 0.5677(8) 0.4459(5) 0.1646(7) 0.040(2) Uani 1 1 d . . . . .
H20 H 0.5447 0.4064 0.1511 0.048 Uiso 1 1 calc R . . . .
C21 C 0.6324(7) 0.4771(5) 0.1165(6) 0.030(2) Uani 1 1 d . . . . .
C22 C 0.6525(8) 0.5341(6) 0.1630(8) 0.045(3) Uani 1 1 d . . . . .
H22 H 0.6955 0.5644 0.1465 0.054 Uiso 1 1 calc R . . . .
C23 C 0.5943(8) 0.6010(5) 0.2851(8) 0.039(3) Uani 1 1 d . . . . .
C24 C 0.6903(10) 0.6304(6) 0.2892(12) 0.071(5) Uani 1 1 d . . . . .
H24A H 0.7372 0.6023 0.3153 0.107 Uiso 1 1 calc GR . . . .
H24B H 0.6884 0.6675 0.3231 0.107 Uiso 1 1 calc GR . . . .
H24C H 0.7082 0.6405 0.2317 0.107 Uiso 1 1 calc GR . . . .
C25 C 0.5220(11) 0.6394(8) 0.2317(12) 0.080(5) Uani 1 1 d . . . . .
H25A H 0.5468 0.6474 0.1761 0.120 Uiso 1 1 calc GR . . . .
H25B H 0.5114 0.6780 0.2607 0.120 Uiso 1 1 calc GR . . . .
H25C H 0.4618 0.6173 0.2246 0.120 Uiso 1 1 calc GR . . . .
C26 C 0.5587(11) 0.5984(9) 0.3782(11) 0.081(5) Uani 1 1 d . . . . .
H26A H 0.4937 0.5825 0.3768 0.122 Uiso 1 1 calc GR . . . .
H26B H 0.5597 0.6394 0.4024 0.122 Uiso 1 1 calc GR . . . .
H26C H 0.6006 0.5719 0.4130 0.122 Uiso 1 1 calc GR . . . .
C27 C 0.4527(8) 0.4618(6) 0.2891(10) 0.056(4) Uani 1 1 d . . . . .
C28 C 0.4723(10) 0.4464(10) 0.3821(9) 0.086(6) Uani 1 1 d . . . . .
H28A H 0.5358 0.4285 0.3900 0.128 Uiso 1 1 calc GR . . . .
H28B H 0.4247 0.4174 0.4001 0.128 Uiso 1 1 calc GR . . . .
H28C H 0.4691 0.4835 0.4161 0.128 Uiso 1 1 calc GR . . . .
C29 C 0.3689(9) 0.5078(7) 0.2749(10) 0.063(4) Uani 1 1 d . . . . .
H29A H 0.3826 0.5446 0.3081 0.094 Uiso 1 1 calc GR . . . .
H29B H 0.3100 0.4894 0.2929 0.094 Uiso 1 1 calc GR . . . .
H29C H 0.3616 0.5184 0.2146 0.094 Uiso 1 1 calc GR . . . .
C30 C 0.4086(10) 0.3997(6) 0.2508(9) 0.058(4) Uani 1 1 d . . . . .
H30A H 0.3920 0.4050 0.1902 0.088 Uiso 1 1 calc GR . . . .
H30B H 0.3514 0.3891 0.2803 0.088 Uiso 1 1 calc GR . . . .
H30C H 0.4554 0.3670 0.2584 0.088 Uiso 1 1 calc GR . . . .
C31 C 0.6778(7) 0.4630(5) 0.0298(7) 0.034(2) Uani 1 1 d . . . . .
C32 C 0.6010(10) 0.4272(7) -0.0267(9) 0.060(4) Uani 1 1 d . . . . .
H32A H 0.5787 0.3922 0.0050 0.090 Uiso 1 1 calc GR . . . .
H32B H 0.6293 0.4131 -0.0785 0.090 Uiso 1 1 calc GR . . . .
H32C H 0.5472 0.4540 -0.0417 0.090 Uiso 1 1 calc GR . . . .
C33 C 0.7643(9) 0.4188(8) 0.0482(9) 0.067(4) Uani 1 1 d . . . . .
H33A H 0.8137 0.4397 0.0829 0.100 Uiso 1 1 calc GR . . . .
H33B H 0.7900 0.4062 -0.0055 0.100 Uiso 1 1 calc GR . . . .
H33C H 0.7428 0.3830 0.0786 0.100 Uiso 1 1 calc GR . . . .
C34 C 0.7050(9) 0.5214(6) -0.0169(8) 0.052(3) Uani 1 1 d . . . . .
H34A H 0.6501 0.5487 -0.0216 0.077 Uiso 1 1 calc GR . . . .
H34B H 0.7248 0.5110 -0.0736 0.077 Uiso 1 1 calc GR . . . .
H34C H 0.7576 0.5416 0.0149 0.077 Uiso 1 1 calc GR . . . .
C35 C 0.6047(7) 0.2782(4) 0.2770(7) 0.032(2) Uani 1 1 d . . . . .
C36 C 0.5852(7) 0.2674(5) 0.3634(7) 0.033(2) Uani 1 1 d . . . . .
C37 C 0.4932(7) 0.2455(5) 0.3829(7) 0.036(2) Uani 1 1 d . . . . .
H37 H 0.4801 0.2386 0.4404 0.043 Uiso 1 1 calc R . . . .
C38 C 0.4211(7) 0.2339(5) 0.3195(9) 0.044(3) Uani 1 1 d . . . . .
C39 C 0.4435(7) 0.2404(5) 0.2342(8) 0.042(3) Uani 1 1 d . . . . .
H39 H 0.3973 0.2298 0.1908 0.050 Uiso 1 1 calc R . . . .
C40 C 0.5340(7) 0.2624(5) 0.2112(8) 0.039(3) Uani 1 1 d . . . . .
C41 C 0.6621(9) 0.2741(6) 0.4373(8) 0.045(3) Uani 1 1 d . . . . .
H41 H 0.7103 0.3039 0.4186 0.055 Uiso 1 1 calc R . . . .
C42 C 0.6225(11) 0.2989(7) 0.5206(9) 0.066(4) Uani 1 1 d . . . . .
H42A H 0.5877 0.3367 0.5085 0.099 Uiso 1 1 calc GR . . . .
H42B H 0.6754 0.3069 0.5619 0.099 Uiso 1 1 calc GR . . . .
H42C H 0.5797 0.2689 0.5437 0.099 Uiso 1 1 calc GR . . . .
C43 C 0.7140(11) 0.2124(7) 0.4524(11) 0.076(5) Uani 1 1 d . . . . .
H43A H 0.6686 0.1820 0.4703 0.114 Uiso 1 1 calc GR . . . .
H43B H 0.7648 0.2173 0.4966 0.114 Uiso 1 1 calc GR . . . .
H43C H 0.7413 0.1992 0.3997 0.114 Uiso 1 1 calc GR . . . .
C44 C 0.3217(8) 0.2124(6) 0.3474(9) 0.050(3) Uani 1 1 d . . . . .
H44 H 0.3327 0.1756 0.3837 0.060 Uiso 1 1 calc R . . . .
C45 C 0.2756(11) 0.2613(8) 0.4035(13) 0.089(6) Uani 1 1 d . . . . .
H45A H 0.3136 0.2658 0.4569 0.134 Uiso 1 1 calc GR . . . .
H45B H 0.2110 0.2487 0.4155 0.134 Uiso 1 1 calc GR . . . .
H45C H 0.2732 0.3002 0.3734 0.134 Uiso 1 1 calc GR . . . .
C46 C 0.2528(7) 0.1935(7) 0.2726(10) 0.065(4) Uani 1 1 d . . . . .
H46A H 0.2427 0.2279 0.2339 0.097 Uiso 1 1 calc GR . . . .
H46B H 0.1919 0.1811 0.2944 0.097 Uiso 1 1 calc GR . . . .
H46C H 0.2802 0.1595 0.2422 0.097 Uiso 1 1 calc GR . . . .
C47 C 0.5548(8) 0.2632(6) 0.1132(8) 0.050(3) Uani 1 1 d . . . . .
H47 H 0.6045 0.2948 0.1055 0.060 Uiso 1 1 calc R . . . .
C48 C 0.4683(9) 0.2805(7) 0.0549(9) 0.062(4) Uani 1 1 d . . . . .
H48A H 0.4239 0.2463 0.0507 0.093 Uiso 1 1 calc GR . . . .
H48B H 0.4894 0.2905 -0.0016 0.093 Uiso 1 1 calc GR . . . .
H48C H 0.4366 0.3158 0.0783 0.093 Uiso 1 1 calc GR . . . .
C49 C 0.5972(11) 0.2013(7) 0.0853(9) 0.063(4) Uani 1 1 d . . . . .
H49A H 0.6543 0.1921 0.1209 0.094 Uiso 1 1 calc GR . . . .
H49B H 0.6138 0.2039 0.0259 0.094 Uiso 1 1 calc GR . . . .
H49C H 0.5502 0.1691 0.0913 0.094 Uiso 1 1 calc GR . . . .
P1 P 0.72239(18) 0.31004(12) 0.2437(2) 0.0358(6) Uani 1 1 d . . . . .
H1 H 0.769(9) 0.304(5) 0.289(7) 0.043 Uiso 1 1 d R . . . .
Th1 Th 0.74366(2) 0.44496(2) 0.26028(3) 0.03678(14) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.455(17) . ?
C1 C5 1.464(18) . ?
C1 C6 1.535(17) . ?
C1 Th1 2.969(11) . ?
C2 C3 1.424(17) . ?
C2 C10 1.493(16) . ?
C2 Th1 2.932(12) . ?
C3 H3 0.9300 . ?
C3 C4 1.441(17) . ?
C3 Th1 2.739(12) . ?
C4 C5 1.373(17) . ?
C4 C14 1.526(15) . ?
C4 Th1 2.726(12) . ?
C5 H5 0.9300 . ?
C5 Th1 2.806(11) . ?
C6 C7 1.45(2) . ?
C6 C8 1.544(16) . ?
C6 C9 1.46(2) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.485(17) . ?
C10 C12 1.540(18) . ?
C10 C13 1.543(19) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.526(18) . ?
C14 C16 1.529(15) . ?
C14 C17 1.502(18) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 Th1 2.575(11) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.447(16) . ?
C18 C22 1.454(16) . ?
C18 C23 1.551(15) . ?
C18 Th1 2.858(11) . ?
C19 C20 1.434(16) . ?
C19 C27 1.520(15) . ?
C19 Th1 2.932(11) . ?
C20 H20 0.9300 . ?
C20 C21 1.370(14) . ?
C20 Th1 2.780(11) . ?
C21 C22 1.445(16) . ?
C21 C31 1.540(13) . ?
C21 Th1 2.728(10) . ?
C22 H22 0.9300 . ?
C22 Th1 2.712(12) . ?
C23 C24 1.469(17) . ?
C23 C25 1.511(17) . ?
C23 C26 1.547(19) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.49(2) . ?
C27 C29 1.533(16) . ?
C27 C30 1.576(19) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32 1.548(17) . ?
C31 C33 1.543(15) . ?
C31 C34 1.509(15) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 C36 1.398(15) . ?
C35 C40 1.416(15) . ?
C35 P1 1.861(10) . ?
C36 C37 1.404(14) . ?
C36 C41 1.527(15) . ?
C37 H37 0.9300 . ?
C37 C38 1.384(16) . ?
C38 C39 1.379(17) . ?
C38 C44 1.532(14) . ?
C39 H39 0.9300 . ?
C39 C40 1.401(14) . ?
C40 C47 1.559(17) . ?
C41 H41 0.9800 . ?
C41 C42 1.523(18) . ?
C41 C43 1.524(18) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44 0.9800 . ?
C44 C45 1.527(19) . ?
C44 C46 1.516(18) . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47 0.9800 . ?
C47 C48 1.507(16) . ?
C47 C49 1.530(19) . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
P1 H1 0.94(12) . ?
P1 Th1 2.937(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C5 106.5(11) . . ?
C2 C1 C6 134.6(12) . . ?
C2 C1 Th1 74.3(6) . . ?
C5 C1 C6 117.6(12) . . ?
C5 C1 Th1 69.2(6) . . ?
C6 C1 Th1 130.2(8) . . ?
C1 C2 C10 133.4(11) . . ?
C1 C2 Th1 77.1(6) . . ?
C3 C2 C1 105.1(11) . . ?
C3 C2 C10 119.2(11) . . ?
C3 C2 Th1 68.0(6) . . ?
C10 C2 Th1 131.1(8) . . ?
C2 C3 H3 124.1 . . ?
C2 C3 C4 111.7(11) . . ?
C2 C3 Th1 83.2(7) . . ?
C4 C3 H3 124.1 . . ?
C4 C3 Th1 74.2(7) . . ?
Th1 C3 H3 110.4 . . ?
C3 C4 C14 125.8(10) . . ?
C3 C4 Th1 75.2(7) . . ?
C5 C4 C3 105.7(11) . . ?
C5 C4 C14 126.4(11) . . ?
C5 C4 Th1 78.9(8) . . ?
C14 C4 Th1 99.1(7) . . ?
C1 C5 H5 124.5 . . ?
C1 C5 Th1 81.6(7) . . ?
C4 C5 C1 110.9(11) . . ?
C4 C5 H5 124.5 . . ?
C4 C5 Th1 72.4(7) . . ?
Th1 C5 H5 113.3 . . ?
C1 C6 C8 108.4(11) . . ?
C7 C6 C1 112.7(13) . . ?
C7 C6 C8 106.2(12) . . ?
C7 C6 C9 107.3(13) . . ?
C9 C6 C1 112.0(11) . . ?
C9 C6 C8 110.0(14) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C2 C10 C12 116.3(11) . . ?
C2 C10 C13 108.6(10) . . ?
C11 C10 C2 111.0(11) . . ?
C11 C10 C12 109.3(11) . . ?
C11 C10 C13 107.3(11) . . ?
C12 C10 C13 103.8(12) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C4 C14 C16 102.1(9) . . ?
C15 C14 C4 109.6(10) . . ?
C15 C14 C16 110.7(11) . . ?
C17 C14 C4 110.7(10) . . ?
C17 C14 C15 108.8(11) . . ?
C17 C14 C16 114.7(11) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 110.6 . . ?
C14 C16 H16B 110.6 . . ?
C14 C16 Th1 105.6(7) . . ?
H16A C16 H16B 108.8 . . ?
Th1 C16 H16A 110.6 . . ?
Th1 C16 H16B 110.6 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C22 105.4(10) . . ?
C19 C18 C23 137.4(10) . . ?
C19 C18 Th1 78.4(6) . . ?
C22 C18 C23 115.5(10) . . ?
C22 C18 Th1 69.4(6) . . ?
C23 C18 Th1 126.3(8) . . ?
C18 C19 C27 131.0(11) . . ?
C18 C19 Th1 72.7(6) . . ?
C20 C19 C18 106.3(10) . . ?
C20 C19 C27 121.9(11) . . ?
C20 C19 Th1 69.6(6) . . ?
C27 C19 Th1 130.2(8) . . ?
C19 C20 H20 123.5 . . ?
C19 C20 Th1 81.5(7) . . ?
C21 C20 C19 112.9(10) . . ?
C21 C20 H20 123.5 . . ?
C21 C20 Th1 73.5(6) . . ?
Th1 C20 H20 113.0 . . ?
C20 C21 C22 105.1(9) . . ?
C20 C21 C31 133.2(10) . . ?
C20 C21 Th1 77.7(6) . . ?
C22 C21 C31 121.7(9) . . ?
C22 C21 Th1 74.0(6) . . ?
C31 C21 Th1 115.0(6) . . ?
C18 C22 H22 124.9 . . ?
C18 C22 Th1 80.5(7) . . ?
C21 C22 C18 110.2(10) . . ?
C21 C22 H22 124.9 . . ?
C21 C22 Th1 75.2(6) . . ?
Th1 C22 H22 111.6 . . ?
C24 C23 C18 111.8(9) . . ?
C24 C23 C25 110.8(12) . . ?
C24 C23 C26 107.8(12) . . ?
C25 C23 C18 105.2(11) . . ?
C25 C23 C26 107.2(11) . . ?
C26 C23 C18 114.0(11) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C19 C27 C29 111.0(10) . . ?
C19 C27 C30 109.3(11) . . ?
C28 C27 C19 117.0(12) . . ?
C28 C27 C29 112.4(12) . . ?
C28 C27 C30 102.8(12) . . ?
C29 C27 C30 103.0(11) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C21 C31 C32 107.0(9) . . ?
C21 C31 C33 107.9(9) . . ?
C33 C31 C32 107.2(11) . . ?
C34 C31 C21 112.1(9) . . ?
C34 C31 C32 109.1(10) . . ?
C34 C31 C33 113.3(10) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 C40 119.2(9) . . ?
C36 C35 P1 122.7(8) . . ?
C40 C35 P1 118.0(8) . . ?
C35 C36 C37 118.9(10) . . ?
C35 C36 C41 122.7(9) . . ?
C37 C36 C41 118.2(10) . . ?
C36 C37 H37 118.8 . . ?
C38 C37 C36 122.3(10) . . ?
C38 C37 H37 118.8 . . ?
C37 C38 C44 118.5(11) . . ?
C39 C38 C37 118.2(10) . . ?
C39 C38 C44 123.3(11) . . ?
C38 C39 H39 119.2 . . ?
C38 C39 C40 121.7(11) . . ?
C40 C39 H39 119.2 . . ?
C35 C40 C47 122.9(9) . . ?
C39 C40 C35 119.4(11) . . ?
C39 C40 C47 117.6(10) . . ?
C36 C41 H41 107.3 . . ?
C42 C41 C36 113.7(10) . . ?
C42 C41 H41 107.3 . . ?
C42 C41 C43 111.4(12) . . ?
C43 C41 C36 109.6(10) . . ?
C43 C41 H41 107.3 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C38 C44 H44 106.9 . . ?
C45 C44 C38 111.0(11) . . ?
C45 C44 H44 106.9 . . ?
C46 C44 C38 113.7(11) . . ?
C46 C44 H44 106.9 . . ?
C46 C44 C45 110.9(12) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C40 C47 H47 107.0 . . ?
C48 C47 C40 114.0(10) . . ?
C48 C47 H47 107.0 . . ?
C48 C47 C49 110.5(12) . . ?
C49 C47 C40 111.0(10) . . ?
C49 C47 H47 107.0 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C35 P1 H1 108(7) . . ?
C35 P1 Th1 115.3(3) . . ?
Th1 P1 H1 91(7) . . ?
C2 Th1 C1 28.5(3) . . ?
C2 Th1 P1 113.2(2) . . ?
C3 Th1 C1 47.0(3) . . ?
C3 Th1 C2 28.8(3) . . ?
C3 Th1 C5 47.7(4) . . ?
C3 Th1 C18 103.8(4) . . ?
C3 Th1 C19 130.6(4) . . ?
C3 Th1 C20 148.7(3) . . ?
C3 Th1 P1 127.6(3) . . ?
C4 Th1 C1 48.2(4) . . ?
C4 Th1 C2 49.4(4) . . ?
C4 Th1 C3 30.6(4) . . ?
C4 Th1 C5 28.7(4) . . ?
C4 Th1 C18 118.5(4) . . ?
C4 Th1 C19 134.4(3) . . ?
C4 Th1 C20 163.2(3) . . ?
C4 Th1 C21 156.2(3) . . ?
C4 Th1 P1 104.3(3) . . ?
C5 Th1 C1 29.2(4) . . ?
C5 Th1 C2 48.0(4) . . ?
C5 Th1 C18 147.1(4) . . ?
C5 Th1 C19 156.6(4) . . ?
C5 Th1 P1 80.3(3) . . ?
C16 Th1 C1 99.9(4) . . ?
C16 Th1 C2 100.1(4) . . ?
C16 Th1 C3 73.1(4) . . ?
C16 Th1 C4 53.2(3) . . ?
C16 Th1 C5 72.8(4) . . ?
C16 Th1 C18 84.0(4) . . ?
C16 Th1 C19 84.5(3) . . ?
C16 Th1 C20 111.1(3) . . ?
C16 Th1 C21 131.9(3) . . ?
C16 Th1 C22 112.0(4) . . ?
C16 Th1 P1 100.7(3) . . ?
C18 Th1 C1 145.6(3) . . ?
C18 Th1 C2 117.1(3) . . ?
C18 Th1 C19 28.9(3) . . ?
C18 Th1 P1 127.7(3) . . ?
C19 Th1 C1 173.0(3) . . ?
C19 Th1 C2 145.6(3) . . ?
C19 Th1 P1 99.1(2) . . ?
C20 Th1 C1 148.4(3) . . ?
C20 Th1 C2 141.6(4) . . ?
C20 Th1 C5 163.4(3) . . ?
C20 Th1 C18 48.2(3) . . ?
C20 Th1 C19 28.9(3) . . ?
C20 Th1 P1 83.1(2) . . ?
C21 Th1 C1 125.8(3) . . ?
C21 Th1 C2 112.8(3) . . ?
C21 Th1 C3 125.9(3) . . ?
C21 Th1 C5 154.7(3) . . ?
C21 Th1 C18 50.3(3) . . ?
C21 Th1 C19 48.6(3) . . ?
C21 Th1 C20 28.8(3) . . ?
C21 Th1 P1 97.5(2) . . ?
C22 Th1 C1 125.0(3) . . ?
C22 Th1 C2 100.1(3) . . ?
C22 Th1 C3 101.0(4) . . ?
C22 Th1 C4 127.8(4) . . ?
C22 Th1 C5 147.0(4) . . ?
C22 Th1 C18 30.1(3) . . ?
C22 Th1 C19 48.1(3) . . ?
C22 Th1 C20 48.0(3) . . ?
C22 Th1 C21 30.8(3) . . ?
C22 Th1 P1 127.8(3) . . ?
P1 Th1 C1 85.4(2) . . ?

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
C1 C2 C3 C4 0.9(14) . . . . ?
C1 C2 C3 Th1 -69.0(8) . . . . ?
C1 C2 C10 C11 -84.3(18) . . . . ?
C1 C2 C10 C12 42(2) . . . . ?
C1 C2 C10 C13 158.0(15) . . . . ?
C2 C1 C5 C4 -1.9(14) . . . . ?
C2 C1 C5 Th1 65.6(8) . . . . ?
C2 C1 C6 C7 169.4(14) . . . . ?
C2 C1 C6 C8 52(2) . . . . ?
C2 C1 C6 C9 -69.5(18) . . . . ?
C2 C3 C4 C5 -2.1(14) . . . . ?
C2 C3 C4 C14 -166.4(11) . . . . ?
C2 C3 C4 Th1 -75.8(9) . . . . ?
C3 C2 C10 C11 75.7(15) . . . . ?
C3 C2 C10 C12 -158.5(12) . . . . ?
C3 C2 C10 C13 -42.0(16) . . . . ?
C3 C4 C5 C1 2.4(13) . . . . ?
C3 C4 C5 Th1 -71.0(8) . . . . ?
C3 C4 C14 C15 -40.9(16) . . . . ?
C3 C4 C14 C16 76.6(14) . . . . ?
C3 C4 C14 C17 -160.9(12) . . . . ?
C4 C14 C16 Th1 1.8(10) . . . . ?
C5 C1 C2 C3 0.5(13) . . . . ?
C5 C1 C2 C10 162.5(13) . . . . ?
C5 C1 C2 Th1 -62.1(8) . . . . ?
C5 C1 C6 C7 4.5(16) . . . . ?
C5 C1 C6 C8 -112.9(14) . . . . ?
C5 C1 C6 C9 125.6(14) . . . . ?
C5 C4 C14 C15 158.0(13) . . . . ?
C5 C4 C14 C16 -84.6(15) . . . . ?
C5 C4 C14 C17 38.0(17) . . . . ?
C6 C1 C2 C3 -165.6(14) . . . . ?
C6 C1 C2 C10 -4(3) . . . . ?
C6 C1 C2 Th1 131.7(15) . . . . ?
C6 C1 C5 C4 167.0(10) . . . . ?
C6 C1 C5 Th1 -125.5(10) . . . . ?
C10 C2 C3 C4 -164.1(11) . . . . ?
C10 C2 C3 Th1 125.9(10) . . . . ?
C14 C4 C5 C1 166.6(11) . . . . ?
C14 C4 C5 Th1 93.2(11) . . . . ?
C15 C14 C16 Th1 118.4(9) . . . . ?
C17 C14 C16 Th1 -118.0(10) . . . . ?
C18 C19 C20 C21 -4.0(13) . . . . ?
C18 C19 C20 Th1 64.0(8) . . . . ?
C18 C19 C27 C28 -73.1(18) . . . . ?
C18 C19 C27 C29 58(2) . . . . ?
C18 C19 C27 C30 170.6(12) . . . . ?
C19 C18 C22 C21 -0.7(13) . . . . ?
C19 C18 C22 Th1 -71.0(8) . . . . ?
C19 C18 C23 C24 156.6(15) . . . . ?
C19 C18 C23 C25 -83.0(18) . . . . ?
C19 C18 C23 C26 34(2) . . . . ?
C19 C20 C21 C22 3.5(13) . . . . ?
C19 C20 C21 C31 -174.1(10) . . . . ?
C19 C20 C21 Th1 72.9(9) . . . . ?
C20 C19 C27 C28 118.9(15) . . . . ?
C20 C19 C27 C29 -110.2(14) . . . . ?
C20 C19 C27 C30 2.7(16) . . . . ?
C20 C21 C22 C18 -1.7(13) . . . . ?
C20 C21 C22 Th1 72.1(7) . . . . ?
C20 C21 C31 C32 32.8(16) . . . . ?
C20 C21 C31 C33 -82.2(15) . . . . ?
C20 C21 C31 C34 152.4(12) . . . . ?
C22 C18 C19 C20 2.7(13) . . . . ?
C22 C18 C19 C27 -166.7(13) . . . . ?
C22 C18 C19 Th1 64.6(8) . . . . ?
C22 C18 C23 C24 -41.2(15) . . . . ?
C22 C18 C23 C25 79.2(14) . . . . ?
C22 C18 C23 C26 -163.7(11) . . . . ?
C22 C21 C31 C32 -144.5(11) . . . . ?
C22 C21 C31 C33 100.4(13) . . . . ?
C22 C21 C31 C34 -24.9(14) . . . . ?
C23 C18 C19 C20 166.0(13) . . . . ?
C23 C18 C19 C27 -3(2) . . . . ?
C23 C18 C19 Th1 -132.0(16) . . . . ?
C23 C18 C22 C21 -168.3(10) . . . . ?
C23 C18 C22 Th1 121.4(9) . . . . ?
C27 C19 C20 C21 166.5(11) . . . . ?
C27 C19 C20 Th1 -125.5(11) . . . . ?
C31 C21 C22 C18 176.3(9) . . . . ?
C31 C21 C22 Th1 -109.9(9) . . . . ?
C35 C36 C37 C38 0.4(16) . . . . ?
C35 C36 C41 C42 144.7(11) . . . . ?
C35 C36 C41 C43 -89.9(14) . . . . ?
C35 C40 C47 C48 -147.4(11) . . . . ?
C35 C40 C47 C49 87.0(14) . . . . ?
C36 C35 C40 C39 4.5(16) . . . . ?
C36 C35 C40 C47 -170.4(10) . . . . ?
C36 C35 P1 Th1 -80.5(9) . . . . ?
C36 C37 C38 C39 4.3(16) . . . . ?
C36 C37 C38 C44 -177.7(10) . . . . ?
C37 C36 C41 C42 -39.6(15) . . . . ?
C37 C36 C41 C43 85.8(14) . . . . ?
C37 C38 C39 C40 -4.6(17) . . . . ?
C37 C38 C44 C45 61.3(15) . . . . ?
C37 C38 C44 C46 -172.8(11) . . . . ?
C38 C39 C40 C35 0.3(17) . . . . ?
C38 C39 C40 C47 175.4(11) . . . . ?
C39 C38 C44 C45 -120.7(14) . . . . ?
C39 C38 C44 C46 5.2(17) . . . . ?
C39 C40 C47 C48 37.7(16) . . . . ?
C39 C40 C47 C49 -87.9(13) . . . . ?
C40 C35 C36 C37 -4.8(15) . . . . ?
C40 C35 C36 C41 170.9(10) . . . . ?
C40 C35 P1 Th1 101.8(8) . . . . ?
C41 C36 C37 C38 -175.4(10) . . . . ?
C44 C38 C39 C40 177.5(11) . . . . ?
P1 C35 C36 C37 177.6(8) . . . . ?
P1 C35 C36 C41 -6.8(14) . . . . ?
P1 C35 C40 C39 -177.8(8) . . . . ?
P1 C35 C40 C47 7.4(14) . . . . ?
Th1 C1 C2 C3 62.7(8) . . . . ?
Th1 C1 C2 C10 -135.4(15) . . . . ?
Th1 C1 C5 C4 -67.4(8) . . . . ?
Th1 C1 C6 C7 -80.8(16) . . . . ?
Th1 C1 C6 C8 161.8(10) . . . . ?
Th1 C1 C6 C9 40.3(18) . . . . ?
Th1 C2 C3 C4 70.0(9) . . . . ?
Th1 C2 C10 C11 161.0(10) . . . . ?
Th1 C2 C10 C12 -73.2(14) . . . . ?
Th1 C2 C10 C13 43.3(15) . . . . ?
Th1 C3 C4 C5 73.7(8) . . . . ?
Th1 C3 C4 C14 -90.6(11) . . . . ?
Th1 C4 C5 C1 73.4(9) . . . . ?
Th1 C4 C14 C15 -119.1(9) . . . . ?
Th1 C4 C14 C16 -1.7(9) . . . . ?
Th1 C4 C14 C17 120.9(9) . . . . ?
Th1 C18 C19 C20 -61.9(8) . . . . ?
Th1 C18 C19 C27 128.7(13) . . . . ?
Th1 C18 C22 C21 70.3(8) . . . . ?
Th1 C18 C23 C24 41.1(15) . . . . ?
Th1 C18 C23 C25 161.5(10) . . . . ?
Th1 C18 C23 C26 -81.4(12) . . . . ?
Th1 C19 C20 C21 -68.0(8) . . . . ?
Th1 C19 C27 C28 29.5(18) . . . . ?
Th1 C19 C27 C29 160.4(10) . . . . ?
Th1 C19 C27 C30 -86.7(14) . . . . ?
Th1 C20 C21 C22 -69.4(7) . . . . ?
Th1 C20 C21 C31 112.9(11) . . . . ?
Th1 C21 C22 C18 -73.8(9) . . . . ?
Th1 C21 C31 C32 129.5(8) . . . . ?
Th1 C21 C31 C33 14.4(12) . . . . ?
Th1 C21 C31 C34 -110.9(8) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.630
_oxdiff_exptl_absorpt_empirical_full_min 0.732
####################################################################### 
# 
# 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_compound11
_database_code_depnum_ccdc_archive 'CCDC 1883597'
_audit_update_record             
;
2018-12-06 deposited with the CCDC.
2019-01-23 downloaded from the CCDC.
;
_audit_creation_date             2017-12-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H68 N4 Th'
_chemical_formula_sum            'C42 H68 N4 Th'
_chemical_formula_weight         861.04
_chemical_melting_point          ?
_chemical_oxdiff_formula         C1H1N1P1Th1
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'
Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   13.4503(4)
_cell_length_b                   17.0758(5)
_cell_length_c                   17.6755(5)
_cell_angle_alpha                90
_cell_angle_beta                 97.625(3)
_cell_angle_gamma                90
_cell_volume                     4023.7(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5951
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.1480
_cell_measurement_theta_min      4.0620
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.738
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.848
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11095
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.848
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.688
_diffrn_reflns_theta_min         3.587
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.848
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -14.00  13.00   1.00    5.00    --  -11.20 -99.00   0.00   27
  2  ω     -5.00  28.00   1.00    5.00    --  -11.20 -99.00-180.00   33
  3  ω     65.00  99.00   1.00    5.00    --   12.45 178.00  60.00   34
  4  ω    -67.00  56.00   1.00    5.00    --   12.45   0.00 -60.00  123
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0321786000
_diffrn_orient_matrix_UB_12      0.0321638000
_diffrn_orient_matrix_UB_13      -0.0106867000
_diffrn_orient_matrix_UB_21      -0.0325722000
_diffrn_orient_matrix_UB_22      -0.0249278000
_diffrn_orient_matrix_UB_23      -0.0239463000
_diffrn_orient_matrix_UB_31      -0.0271510000
_diffrn_orient_matrix_UB_32      -0.0082910000
_diffrn_orient_matrix_UB_33      0.0308359000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4455
_reflns_number_total             4841
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.152
_refine_diff_density_min         -2.099
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4841
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0336
_refine_ls_restrained_S_all      1.131
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+13.7900P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0634
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C19(H19), C20(H20)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2831(2) 0.2719(2) 0.20396(19) 0.0128(8) Uani 1 1 d . . . . .
C2 C 0.2905(2) 0.3228(2) 0.26991(19) 0.0131(8) Uani 1 1 d . . . . .
C3 C 0.3358(2) 0.3931(2) 0.24938(19) 0.0120(7) Uani 1 1 d . . . . .
H3 H 0.3519 0.4352 0.2821 0.014 Uiso 1 1 calc R . . . .
C4 C 0.3530(2) 0.3905(2) 0.17175(19) 0.0130(8) Uani 1 1 d . . . . .
C5 C 0.3221(2) 0.3162(2) 0.14635(19) 0.0134(8) Uani 1 1 d . . . . .
H5 H 0.3265 0.2976 0.0974 0.016 Uiso 1 1 calc R . . . .
C6 C 0.2341(3) 0.1914(2) 0.1841(2) 0.0175(8) Uani 1 1 d . . . . .
C7 C 0.2455(3) 0.1689(3) 0.1012(2) 0.0236(9) Uani 1 1 d . . . . .
H7A H 0.2113 0.2067 0.0669 0.035 Uiso 1 1 calc GR . . . .
H7B H 0.2169 0.1180 0.0900 0.035 Uiso 1 1 calc GR . . . .
H7C H 0.3153 0.1680 0.0951 0.035 Uiso 1 1 calc GR . . . .
C8 C 0.1193(3) 0.1960(3) 0.1864(2) 0.0260(10) Uani 1 1 d . . . . .
H8A H 0.1068 0.2045 0.2380 0.039 Uiso 1 1 calc GR . . . .
H8B H 0.0885 0.1478 0.1677 0.039 Uiso 1 1 calc GR . . . .
H8C H 0.0916 0.2386 0.1549 0.039 Uiso 1 1 calc GR . . . .
C9 C 0.2815(3) 0.1241(3) 0.2340(2) 0.0240(9) Uani 1 1 d . . . . .
H9A H 0.3514 0.1201 0.2286 0.036 Uiso 1 1 calc GR . . . .
H9B H 0.2484 0.0759 0.2182 0.036 Uiso 1 1 calc GR . . . .
H9C H 0.2745 0.1342 0.2865 0.036 Uiso 1 1 calc GR . . . .
C10 C 0.2359(3) 0.3213(3) 0.3418(2) 0.0186(9) Uani 1 1 d . . . . .
C11 C 0.1306(3) 0.3556(3) 0.3173(2) 0.0231(9) Uani 1 1 d . . . . .
H11A H 0.1367 0.4084 0.2997 0.035 Uiso 1 1 calc GR . . . .
H11B H 0.0934 0.3554 0.3600 0.035 Uiso 1 1 calc GR . . . .
H11C H 0.0961 0.3244 0.2768 0.035 Uiso 1 1 calc GR . . . .
C12 C 0.2254(3) 0.2408(3) 0.3790(2) 0.0223(9) Uani 1 1 d . . . . .
H12A H 0.1830 0.2079 0.3445 0.033 Uiso 1 1 calc GR . . . .
H12B H 0.1963 0.2473 0.4253 0.033 Uiso 1 1 calc GR . . . .
H12C H 0.2904 0.2171 0.3903 0.033 Uiso 1 1 calc GR . . . .
C13 C 0.2883(3) 0.3756(3) 0.4046(2) 0.0222(9) Uani 1 1 d . . . . .
H13A H 0.3567 0.3591 0.4181 0.033 Uiso 1 1 calc GR . . . .
H13B H 0.2540 0.3729 0.4488 0.033 Uiso 1 1 calc GR . . . .
H13C H 0.2870 0.4285 0.3861 0.033 Uiso 1 1 calc GR . . . .
C14 C 0.3677(3) 0.4591(2) 0.1194(2) 0.0165(8) Uani 1 1 d . . . . .
C15 C 0.4249(3) 0.5271(3) 0.1598(2) 0.0224(9) Uani 1 1 d . . . . .
H15A H 0.3905 0.5449 0.2009 0.034 Uiso 1 1 calc GR . . . .
H15B H 0.4291 0.5691 0.1243 0.034 Uiso 1 1 calc GR . . . .
H15C H 0.4912 0.5102 0.1799 0.034 Uiso 1 1 calc GR . . . .
C16 C 0.4221(3) 0.4328(3) 0.0527(2) 0.0227(9) Uani 1 1 d . . . . .
H16A H 0.4910 0.4217 0.0711 0.034 Uiso 1 1 calc GR . . . .
H16B H 0.4188 0.4738 0.0152 0.034 Uiso 1 1 calc GR . . . .
H16C H 0.3905 0.3866 0.0299 0.034 Uiso 1 1 calc GR . . . .
C17 C 0.2618(3) 0.4878(3) 0.0877(2) 0.0262(10) Uani 1 1 d . . . . .
H17A H 0.2251 0.4459 0.0607 0.039 Uiso 1 1 calc GR . . . .
H17B H 0.2668 0.5309 0.0536 0.039 Uiso 1 1 calc GR . . . .
H17C H 0.2274 0.5044 0.1292 0.039 Uiso 1 1 calc GR . . . .
C18 C 0.4875(3) 0.1837(3) 0.3463(2) 0.0197(9) Uani 1 1 d . . . . .
C19 C 0.4914(3) 0.1551(3) 0.4696(2) 0.0308(12) Uani 1 1 d . . . . .
H19 H 0.4949 0.1276 0.5153 0.037 Uiso 1 1 calc R . . . .
C20 C 0.4845(3) 0.2333(3) 0.4613(2) 0.0261(10) Uani 1 1 d . . . . .
H20 H 0.4821 0.2694 0.5005 0.031 Uiso 1 1 calc R . . . .
C21 C 0.5059(3) 0.0418(3) 0.3805(3) 0.0352(12) Uani 1 1 d . . . . .
H21A H 0.4888 0.0336 0.3266 0.053 Uiso 1 1 calc GR . . . .
H21B H 0.4635 0.0102 0.4077 0.053 Uiso 1 1 calc GR . . . .
H21C H 0.5747 0.0275 0.3955 0.053 Uiso 1 1 calc GR . . . .
N1 N 0.4816(2) 0.2510(2) 0.38479(16) 0.0175(7) Uani 1 1 d . . . . .
N2 N 0.4921(2) 0.1233(2) 0.39791(19) 0.0256(8) Uani 1 1 d . . . . .
Th1 Th 0.5000 0.28753(2) 0.2500 0.00986(6) Uani 1 2 d S T P . .


_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
C1 C2 1.446(5) . ?
C1 C5 1.424(5) . ?
C1 C6 1.544(5) . ?
C1 Th1 2.936(3) . ?
C2 C3 1.415(5) . ?
C2 C10 1.550(5) . ?
C2 Th1 2.947(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.422(4) . ?
C3 Th1 2.850(3) . ?
C4 C5 1.391(5) . ?
C4 C14 1.523(5) . ?
C4 Th1 2.861(4) . ?
C5 H5 0.9300 . ?
C5 Th1 2.856(3) . ?
C6 C7 1.542(5) . ?
C6 C8 1.552(5) . ?
C6 C9 1.536(6) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.542(5) . ?
C10 C12 1.538(6) . ?
C10 C13 1.543(6) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.518(6) . ?
C14 C16 1.535(5) . ?
C14 C17 1.539(5) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 N1 1.344(5) . ?
C18 N2 1.372(5) . ?
C18 Th1 2.479(4) . ?
C19 H19 0.9300 . ?
C19 C20 1.345(7) . ?
C19 N2 1.381(5) . ?
C20 H20 0.9300 . ?
C20 N1 1.382(5) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C21 N2 1.442(6) . ?
N1 Th1 2.507(3) . ?
Th1 C1 2.936(3) 2_655 ?
Th1 C3 2.850(3) 2_655 ?
Th1 C4 2.861(4) 2_655 ?
Th1 C5 2.856(3) 2_655 ?
Th1 C18 2.479(4) 2_655 ?
Th1 N1 2.507(3) 2_655 ?

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
C2 C1 C6 134.4(3) . . ?
C2 C1 Th1 76.21(19) . . ?
C5 C1 C2 105.4(3) . . ?
C5 C1 C6 119.8(3) . . ?
C5 C1 Th1 72.69(18) . . ?
C6 C1 Th1 121.5(2) . . ?
C1 C2 C10 131.4(3) . . ?
C1 C2 Th1 75.33(18) . . ?
C3 C2 C1 106.8(3) . . ?
C3 C2 C10 119.4(3) . . ?
C3 C2 Th1 72.09(19) . . ?
C10 C2 Th1 131.2(2) . . ?
C2 C3 H3 124.7 . . ?
C2 C3 C4 110.6(3) . . ?
C2 C3 Th1 79.7(2) . . ?
C4 C3 H3 124.7 . . ?
C4 C3 Th1 76.0(2) . . ?
Th1 C3 H3 111.7 . . ?
C3 C4 C14 127.8(4) . . ?
C3 C4 Th1 75.1(2) . . ?
C5 C4 C3 105.1(3) . . ?
C5 C4 C14 124.3(3) . . ?
C5 C4 Th1 75.7(2) . . ?
C14 C4 Th1 129.0(2) . . ?
C1 C5 H5 123.9 . . ?
C1 C5 Th1 78.9(2) . . ?
C4 C5 C1 112.1(3) . . ?
C4 C5 H5 123.9 . . ?
C4 C5 Th1 76.1(2) . . ?
Th1 C5 H5 112.8 . . ?
C1 C6 C8 110.2(3) . . ?
C7 C6 C1 110.2(3) . . ?
C7 C6 C8 105.2(3) . . ?
C9 C6 C1 113.8(3) . . ?
C9 C6 C7 105.9(3) . . ?
C9 C6 C8 111.2(3) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 C2 106.3(3) . . ?
C11 C10 C13 106.8(3) . . ?
C12 C10 C2 116.4(3) . . ?
C12 C10 C11 109.1(3) . . ?
C12 C10 C13 106.8(3) . . ?
C13 C10 C2 111.1(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C4 C14 C16 110.8(3) . . ?
C4 C14 C17 106.1(3) . . ?
C15 C14 C4 113.6(3) . . ?
C15 C14 C16 108.8(3) . . ?
C15 C14 C17 108.4(4) . . ?
C16 C14 C17 109.0(3) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N1 C18 N2 107.9(3) . . ?
N1 C18 Th1 75.5(2) . . ?
N2 C18 Th1 172.9(3) . . ?
C20 C19 H19 126.3 . . ?
C20 C19 N2 107.4(4) . . ?
N2 C19 H19 126.3 . . ?
C19 C20 H20 125.8 . . ?
C19 C20 N1 108.5(4) . . ?
N1 C20 H20 125.8 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C21 H21A 109.5 . . ?
N2 C21 H21B 109.5 . . ?
N2 C21 H21C 109.5 . . ?
C18 N1 C20 108.2(4) . . ?
C18 N1 Th1 73.2(2) . . ?
C20 N1 Th1 172.5(3) . . ?
C18 N2 C19 108.0(4) . . ?
C18 N2 C21 125.3(4) . . ?
C19 N2 C21 126.3(4) . . ?
C1 Th1 C1 169.59(15) . 2_655 ?
C3 Th1 C1 143.11(11) . 2_655 ?
C3 Th1 C1 143.11(11) 2_655 . ?
C3 Th1 C1 46.76(11) 2_655 2_655 ?
C3 Th1 C1 46.76(11) . . ?
C3 Th1 C3 101.53(15) . 2_655 ?
C3 Th1 C4 28.84(9) . . ?
C3 Th1 C4 95.66(11) . 2_655 ?
C3 Th1 C4 28.84(9) 2_655 2_655 ?
C3 Th1 C4 95.66(11) 2_655 . ?
C3 Th1 C5 46.07(10) 2_655 2_655 ?
C3 Th1 C5 46.07(10) . . ?
C3 Th1 C5 118.48(11) . 2_655 ?
C3 Th1 C5 118.48(11) 2_655 . ?
C4 Th1 C1 47.48(10) 2_655 2_655 ?
C4 Th1 C1 141.94(10) 2_655 . ?
C4 Th1 C1 141.94(10) . 2_655 ?
C4 Th1 C1 47.48(10) . . ?
C4 Th1 C4 104.17(16) . 2_655 ?
C5 Th1 C1 155.59(9) 2_655 . ?
C5 Th1 C1 155.59(9) . 2_655 ?
C5 Th1 C1 28.41(9) 2_655 2_655 ?
C5 Th1 C1 28.42(9) . . ?
C5 Th1 C4 28.15(11) . . ?
C5 Th1 C4 28.16(11) 2_655 2_655 ?
C5 Th1 C4 132.14(12) 2_655 . ?
C5 Th1 C4 132.14(12) . 2_655 ?
C5 Th1 C5 160.26(16) . 2_655 ?
C18 Th1 C1 88.29(11) . . ?
C18 Th1 C1 84.27(11) 2_655 . ?
C18 Th1 C1 84.27(11) . 2_655 ?
C18 Th1 C1 88.29(11) 2_655 2_655 ?
C18 Th1 C3 124.95(11) . 2_655 ?
C18 Th1 C3 124.94(11) 2_655 . ?
C18 Th1 C3 109.39(11) 2_655 2_655 ?
C18 Th1 C3 109.39(11) . . ?
C18 Th1 C4 102.30(12) . 2_655 ?
C18 Th1 C4 131.77(11) 2_655 2_655 ?
C18 Th1 C4 131.76(11) . . ?
C18 Th1 C4 102.29(12) 2_655 . ?
C18 Th1 C5 115.84(11) 2_655 2_655 ?
C18 Th1 C5 79.01(12) . 2_655 ?
C18 Th1 C5 79.01(12) 2_655 . ?
C18 Th1 C5 115.84(11) . . ?
C18 Th1 C18 88.7(2) 2_655 . ?
C18 Th1 N1 119.93(14) . 2_655 ?
C18 Th1 N1 31.26(13) 2_655 2_655 ?
C18 Th1 N1 119.93(14) 2_655 . ?
C18 Th1 N1 31.26(13) . . ?
N1 Th1 C1 91.20(9) 2_655 2_655 ?
N1 Th1 C1 91.19(9) . . ?
N1 Th1 C1 86.22(9) 2_655 . ?
N1 Th1 C1 86.22(9) . 2_655 ?
N1 Th1 C3 109.15(10) . 2_655 ?
N1 Th1 C3 89.23(10) 2_655 2_655 ?
N1 Th1 C3 109.15(10) 2_655 . ?
N1 Th1 C3 89.23(10) . . ?
N1 Th1 C4 117.59(10) . . ?
N1 Th1 C4 117.59(10) 2_655 2_655 ?
N1 Th1 C4 80.94(10) 2_655 . ?
N1 Th1 C4 80.94(10) . 2_655 ?
N1 Th1 C5 67.24(10) . 2_655 ?
N1 Th1 C5 118.18(9) . . ?
N1 Th1 C5 118.18(9) 2_655 2_655 ?
N1 Th1 C5 67.24(10) 2_655 . ?
N1 Th1 N1 151.19(17) 2_655 . ?

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
C1 C2 C3 C4 2.8(4) . . . . ?
C1 C2 C3 Th1 -67.9(2) . . . . ?
C1 C2 C10 C11 -78.2(5) . . . . ?
C1 C2 C10 C12 43.6(6) . . . . ?
C1 C2 C10 C13 166.0(4) . . . . ?
C2 C1 C5 C4 -0.1(4) . . . . ?
C2 C1 C5 Th1 69.8(2) . . . . ?
C2 C1 C6 C7 176.2(4) . . . . ?
C2 C1 C6 C8 60.6(5) . . . . ?
C2 C1 C6 C9 -65.1(5) . . . . ?
C2 C3 C4 C5 -2.8(4) . . . . ?
C2 C3 C4 C14 158.6(3) . . . . ?
C2 C3 C4 Th1 -73.1(3) . . . . ?
C3 C2 C10 C11 81.6(4) . . . . ?
C3 C2 C10 C12 -156.7(3) . . . . ?
C3 C2 C10 C13 -34.2(5) . . . . ?
C3 C4 C5 C1 1.7(4) . . . . ?
C3 C4 C5 Th1 -70.0(2) . . . . ?
C3 C4 C14 C15 35.8(5) . . . . ?
C3 C4 C14 C16 158.7(3) . . . . ?
C3 C4 C14 C17 -83.1(4) . . . . ?
C5 C1 C2 C3 -1.6(4) . . . . ?
C5 C1 C2 C10 160.0(4) . . . . ?
C5 C1 C2 Th1 -67.3(2) . . . . ?
C5 C1 C6 C7 5.3(5) . . . . ?
C5 C1 C6 C8 -110.4(4) . . . . ?
C5 C1 C6 C9 124.0(3) . . . . ?
C5 C4 C14 C15 -166.1(3) . . . . ?
C5 C4 C14 C16 -43.3(5) . . . . ?
C5 C4 C14 C17 75.0(4) . . . . ?
C6 C1 C2 C3 -173.5(4) . . . . ?
C6 C1 C2 C10 -11.9(7) . . . . ?
C6 C1 C2 Th1 120.8(4) . . . . ?
C6 C1 C5 C4 173.2(3) . . . . ?
C6 C1 C5 Th1 -116.8(3) . . . . ?
C10 C2 C3 C4 -161.5(3) . . . . ?
C10 C2 C3 Th1 127.8(3) . . . . ?
C14 C4 C5 C1 -160.5(3) . . . . ?
C14 C4 C5 Th1 127.8(3) . . . . ?
C19 C20 N1 C18 -0.5(4) . . . . ?
C20 C19 N2 C18 1.1(5) . . . . ?
C20 C19 N2 C21 175.2(4) . . . . ?
N1 C18 N2 C19 -1.4(4) . . . . ?
N1 C18 N2 C21 -175.6(4) . . . . ?
N2 C18 N1 C20 1.2(4) . . . . ?
N2 C18 N1 Th1 173.5(3) . . . . ?
N2 C19 C20 N1 -0.4(5) . . . . ?
Th1 C1 C2 C3 65.7(2) . . . . ?
Th1 C1 C2 C10 -132.6(4) . . . . ?
Th1 C1 C5 C4 -69.9(3) . . . . ?
Th1 C1 C6 C7 -81.8(3) . . . . ?
Th1 C1 C6 C8 162.6(2) . . . . ?
Th1 C1 C6 C9 36.9(4) . . . . ?
Th1 C2 C3 C4 70.7(2) . . . . ?
Th1 C2 C10 C11 172.9(3) . . . . ?
Th1 C2 C10 C12 -65.3(4) . . . . ?
Th1 C2 C10 C13 57.1(5) . . . . ?
Th1 C3 C4 C5 70.4(2) . . . . ?
Th1 C3 C4 C14 -128.3(3) . . . . ?
Th1 C4 C5 C1 71.7(3) . . . . ?
Th1 C4 C14 C15 -66.4(4) . . . . ?
Th1 C4 C14 C16 56.4(4) . . . . ?
Th1 C4 C14 C17 174.7(3) . . . . ?
Th1 C18 N1 C20 -172.3(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.100
_oxdiff_exptl_absorpt_empirical_full_min 0.861
####################################################################### 
# 
# 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_compound8
_database_code_depnum_ccdc_archive 'CCDC 1883599'
_audit_update_record             
;
2018-12-06 deposited with the CCDC.
2019-01-23 downloaded from the CCDC.
;
_audit_creation_date             2018-09-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H66 O Th'
_chemical_formula_sum            'C40 H66 O Th'
_chemical_formula_weight         794.96
_chemical_melting_point          ?
_chemical_oxdiff_formula         C1H1O1P1Th1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Th Th -4.1491 12.3296 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.22930(10)
_cell_length_b                   20.8251(2)
_cell_length_c                   17.4204(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.5370(10)
_cell_angle_gamma                90
_cell_volume                     3693.69(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8934
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      71.9100
_cell_measurement_theta_min      4.8200
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.206
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15173
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.975
_diffrn_reflns_theta_min         4.246
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -83.00  -3.00   1.00    1.00    --  -41.49 125.00 150.00   80
  2  ω   -110.00 -18.00   1.00    1.00    --  -41.49 -37.00  60.00   92
  3  ω     35.00  83.00   1.00    1.00    --   41.49-125.00   0.00   48
  4  ω    -23.00   2.00   1.00    1.00    --   41.49 -19.00  90.00   25
  5  ω     74.00 104.00   1.00    1.00    --  104.69 -94.00 -30.00   30
  6  ω     50.00 117.00   1.00    1.00    --  104.69-125.00 -90.00   67
  7  ω    112.00 140.00   1.00    1.00    --  104.69 104.00   8.00   28
  8  ω     47.00 134.00   1.00    1.00    --  104.69 -61.00   0.00   87
  9  ω    105.00 177.00   1.00    1.00    --  104.69  45.00-180.00   72
 10  ω     32.00  74.00   1.00    1.00    --  104.69 -61.00 -60.00   42
 11  ω    145.00 172.00   1.00    1.00    --  104.69 125.00 -60.00   27
 12  ω     32.00 131.00   1.00    1.00    --  104.69 -45.00  90.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1039727000
_diffrn_orient_matrix_UB_12      0.0530819000
_diffrn_orient_matrix_UB_13      -0.0043030000
_diffrn_orient_matrix_UB_21      0.1084747000
_diffrn_orient_matrix_UB_22      -0.0475303000
_diffrn_orient_matrix_UB_23      0.0304499000
_diffrn_orient_matrix_UB_31      0.0184490000
_diffrn_orient_matrix_UB_32      -0.0200262000
_diffrn_orient_matrix_UB_33      -0.0832782000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6440
_reflns_number_total             7093
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         2.052
_refine_diff_density_min         -2.768
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         7093
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0291
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0373P)²+4.2791P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0731
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C20(H20), C22(H22), C40(H40)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5773(4) 0.78591(19) 0.6287(2) 0.0133(8) Uani 1 1 d . . . . .
C2 C 0.5618(4) 0.72603(19) 0.5871(2) 0.0131(8) Uani 1 1 d . . . . .
C3 C 0.4334(4) 0.70229(19) 0.5991(2) 0.0125(7) Uani 1 1 d . . . . .
H3 H 0.3980 0.6638 0.5796 0.015 Uiso 1 1 calc R . . . .
C4 C 0.3691(4) 0.7457(2) 0.6447(2) 0.0153(8) Uani 1 1 d . . . . .
C5 C 0.4585(4) 0.79585(19) 0.6639(2) 0.0131(7) Uani 1 1 d . . . . .
H5 H 0.4424 0.8306 0.6952 0.016 Uiso 1 1 calc R . . . .
C6 C 0.6821(4) 0.8396(2) 0.6323(2) 0.0159(8) Uani 1 1 d . . . . .
C7 C 0.6405(4) 0.8966(2) 0.6792(3) 0.0229(9) Uani 1 1 d . . . . .
H7A H 0.5584 0.9132 0.6561 0.034 Uiso 1 1 calc GR . . . .
H7B H 0.7063 0.9295 0.6800 0.034 Uiso 1 1 calc GR . . . .
H7C H 0.6307 0.8830 0.7310 0.034 Uiso 1 1 calc GR . . . .
C8 C 0.6965(4) 0.8658(2) 0.5507(2) 0.0233(9) Uani 1 1 d . . . . .
H8A H 0.7334 0.8331 0.5204 0.035 Uiso 1 1 calc GR . . . .
H8B H 0.7535 0.9026 0.5543 0.035 Uiso 1 1 calc GR . . . .
H8C H 0.6118 0.8780 0.5266 0.035 Uiso 1 1 calc GR . . . .
C9 C 0.8165(4) 0.8179(2) 0.6710(3) 0.0205(9) Uani 1 1 d . . . . .
H9A H 0.8091 0.8083 0.7243 0.031 Uiso 1 1 calc GR . . . .
H9B H 0.8796 0.8516 0.6673 0.031 Uiso 1 1 calc GR . . . .
H9C H 0.8448 0.7802 0.6455 0.031 Uiso 1 1 calc GR . . . .
C10 C 0.6402(4) 0.6944(2) 0.5258(2) 0.0164(8) Uani 1 1 d . . . . .
C11 C 0.5920(4) 0.7229(2) 0.4466(2) 0.0241(10) Uani 1 1 d . . . . .
H11A H 0.4997 0.7147 0.4357 0.036 Uiso 1 1 calc GR . . . .
H11B H 0.6388 0.7033 0.4075 0.036 Uiso 1 1 calc GR . . . .
H11C H 0.6073 0.7684 0.4472 0.036 Uiso 1 1 calc GR . . . .
C12 C 0.7897(4) 0.7009(2) 0.5391(2) 0.0229(9) Uani 1 1 d . . . . .
H12A H 0.8135 0.7454 0.5362 0.034 Uiso 1 1 calc GR . . . .
H12B H 0.8296 0.6771 0.5004 0.034 Uiso 1 1 calc GR . . . .
H12C H 0.8197 0.6844 0.5892 0.034 Uiso 1 1 calc GR . . . .
C13 C 0.6116(4) 0.6213(2) 0.5220(2) 0.0222(9) Uani 1 1 d . . . . .
H13A H 0.6365 0.6024 0.5715 0.033 Uiso 1 1 calc GR . . . .
H13B H 0.6610 0.6019 0.4840 0.033 Uiso 1 1 calc GR . . . .
H13C H 0.5195 0.6145 0.5082 0.033 Uiso 1 1 calc GR . . . .
C14 C 0.2470(4) 0.7321(2) 0.6854(2) 0.0150(8) Uani 1 1 d . . . . .
C15 C 0.3001(5) 0.6926(2) 0.7571(3) 0.0244(10) Uani 1 1 d . . . . .
H15A H 0.2629 0.6497 0.7554 0.029 Uiso 1 1 calc R . . . .
H15B H 0.2803 0.7135 0.8043 0.029 Uiso 1 1 calc R . . . .
C16 C 0.1829(4) 0.7948(2) 0.7089(2) 0.0187(8) Uani 1 1 d . . . . .
H16A H 0.2442 0.8185 0.7432 0.028 Uiso 1 1 calc GR . . . .
H16B H 0.1062 0.7851 0.7344 0.028 Uiso 1 1 calc GR . . . .
H16C H 0.1582 0.8201 0.6637 0.028 Uiso 1 1 calc GR . . . .
C17 C 0.1457(4) 0.6952(2) 0.6320(2) 0.0215(9) Uani 1 1 d . . . . .
H17A H 0.1236 0.7196 0.5858 0.032 Uiso 1 1 calc GR . . . .
H17B H 0.0680 0.6883 0.6578 0.032 Uiso 1 1 calc GR . . . .
H17C H 0.1818 0.6545 0.6190 0.032 Uiso 1 1 calc GR . . . .
C18 C 0.7197(4) 0.58989(19) 0.8037(2) 0.0133(8) Uani 1 1 d . . . . .
C19 C 0.6340(4) 0.60049(19) 0.8635(2) 0.0146(8) Uani 1 1 d . . . . .
C20 C 0.5082(4) 0.57619(19) 0.8348(2) 0.0137(8) Uani 1 1 d . . . . .
H20 H 0.4338 0.5774 0.8616 0.016 Uiso 1 1 calc R . . . .
C21 C 0.5121(4) 0.5502(2) 0.7608(2) 0.0145(8) Uani 1 1 d . . . . .
C22 C 0.6411(4) 0.56033(18) 0.7411(2) 0.0126(7) Uani 1 1 d . . . . .
H22 H 0.6708 0.5493 0.6940 0.015 Uiso 1 1 calc R . . . .
C23 C 0.8662(4) 0.6034(2) 0.7988(2) 0.0164(8) Uani 1 1 d . . . . .
C24 C 0.9531(4) 0.5731(2) 0.8668(2) 0.0247(9) Uani 1 1 d . . . . .
H24A H 0.9320 0.5920 0.9143 0.037 Uiso 1 1 calc GR . . . .
H24B H 1.0439 0.5809 0.8603 0.037 Uiso 1 1 calc GR . . . .
H24C H 0.9375 0.5277 0.8679 0.037 Uiso 1 1 calc GR . . . .
C25 C 0.8928(4) 0.6757(2) 0.7945(3) 0.0222(9) Uani 1 1 d . . . . .
H25A H 0.8536 0.6922 0.7462 0.033 Uiso 1 1 calc GR . . . .
H25B H 0.9858 0.6831 0.7985 0.033 Uiso 1 1 calc GR . . . .
H25C H 0.8556 0.6971 0.8361 0.033 Uiso 1 1 calc GR . . . .
C26 C 0.9126(4) 0.5722(2) 0.7255(2) 0.0209(9) Uani 1 1 d . . . . .
H26A H 0.9009 0.5265 0.7277 0.031 Uiso 1 1 calc GR . . . .
H26B H 1.0037 0.5818 0.7226 0.031 Uiso 1 1 calc GR . . . .
H26C H 0.8618 0.5890 0.6807 0.031 Uiso 1 1 calc GR . . . .
C27 C 0.6565(4) 0.6204(2) 0.9493(2) 0.0198(9) Uani 1 1 d . . . . .
C28 C 0.6992(5) 0.5597(2) 0.9967(2) 0.0301(11) Uani 1 1 d . . . . .
H28A H 0.6320 0.5276 0.9890 0.045 Uiso 1 1 calc GR . . . .
H28B H 0.7125 0.5706 1.0505 0.045 Uiso 1 1 calc GR . . . .
H28C H 0.7796 0.5434 0.9801 0.045 Uiso 1 1 calc GR . . . .
C29 C 0.7564(5) 0.6742(2) 0.9679(2) 0.0225(9) Uani 1 1 d . . . . .
H29A H 0.8402 0.6613 0.9527 0.034 Uiso 1 1 calc GR . . . .
H29B H 0.7641 0.6827 1.0223 0.034 Uiso 1 1 calc GR . . . .
H29C H 0.7275 0.7124 0.9404 0.034 Uiso 1 1 calc GR . . . .
C30 C 0.5273(5) 0.6448(3) 0.9773(3) 0.0311(11) Uani 1 1 d . . . . .
H30A H 0.4916 0.6782 0.9436 0.047 Uiso 1 1 calc GR . . . .
H30B H 0.5441 0.6613 1.0287 0.047 Uiso 1 1 calc GR . . . .
H30C H 0.4657 0.6100 0.9771 0.047 Uiso 1 1 calc GR . . . .
C31 C 0.4081(4) 0.50683(19) 0.7177(2) 0.0169(8) Uani 1 1 d . . . . .
C32 C 0.2848(5) 0.5023(3) 0.7606(3) 0.0331(11) Uani 1 1 d . . . . .
H32A H 0.3081 0.4863 0.8118 0.050 Uiso 1 1 calc GR . . . .
H32B H 0.2230 0.4736 0.7336 0.050 Uiso 1 1 calc GR . . . .
H32C H 0.2460 0.5441 0.7634 0.050 Uiso 1 1 calc GR . . . .
C33 C 0.3699(5) 0.5295(2) 0.6352(3) 0.0322(12) Uani 1 1 d . . . . .
H33A H 0.3333 0.5719 0.6362 0.048 Uiso 1 1 calc GR . . . .
H33B H 0.3060 0.5007 0.6103 0.048 Uiso 1 1 calc GR . . . .
H33C H 0.4464 0.5302 0.6073 0.048 Uiso 1 1 calc GR . . . .
C34 C 0.4660(4) 0.4395(2) 0.7142(3) 0.0297(10) Uani 1 1 d . . . . .
H34A H 0.5456 0.4412 0.6893 0.045 Uiso 1 1 calc GR . . . .
H34B H 0.4040 0.4118 0.6856 0.045 Uiso 1 1 calc GR . . . .
H34C H 0.4848 0.4232 0.7656 0.045 Uiso 1 1 calc GR . . . .
C35 C 0.5946(4) 0.8234(2) 0.8662(2) 0.0184(8) Uani 1 1 d . . . . .
C36 C 0.7240(4) 0.8478(2) 0.8949(2) 0.0222(9) Uani 1 1 d . . . . .
H36A H 0.7836 0.8414 0.8555 0.027 Uiso 1 1 calc R . . . .
H36B H 0.7569 0.8228 0.9396 0.027 Uiso 1 1 calc R . . . .
C37 C 0.7255(4) 0.9181(2) 0.9169(3) 0.0275(10) Uani 1 1 d . . . . .
H37A H 0.8043 0.9270 0.9509 0.033 Uiso 1 1 calc R . . . .
H37B H 0.7286 0.9440 0.8709 0.033 Uiso 1 1 calc R . . . .
C38 C 0.6077(5) 0.9369(2) 0.9565(3) 0.0320(11) Uani 1 1 d . . . . .
H38A H 0.6110 0.9827 0.9667 0.038 Uiso 1 1 calc R . . . .
H38B H 0.6105 0.9149 1.0057 0.038 Uiso 1 1 calc R . . . .
C39 C 0.4806(5) 0.9213(2) 0.9099(3) 0.0287(10) Uani 1 1 d . . . . .
H39A H 0.4640 0.9533 0.8696 0.034 Uiso 1 1 calc R . . . .
H39B H 0.4098 0.9238 0.9430 0.034 Uiso 1 1 calc R . . . .
C40 C 0.4803(4) 0.8553(2) 0.8733(2) 0.0186(8) Uani 1 1 d . . . . .
H40 H 0.4009 0.8363 0.8555 0.022 Uiso 1 1 calc R . . . .
O1 O 0.5916(3) 0.76460(14) 0.82972(15) 0.0195(6) Uani 1 1 d . . . . .
Th1 Th 0.54364(2) 0.68914(2) 0.74734(2) 0.01162(6) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.444(5) . ?
C1 C5 1.428(5) . ?
C1 C6 1.546(5) . ?
C1 Th1 2.930(4) . ?
C2 C3 1.438(5) . ?
C2 C10 1.544(5) . ?
C2 Th1 2.918(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.407(5) . ?
C3 Th1 2.729(4) . ?
C4 C5 1.408(6) . ?
C4 C14 1.521(5) . ?
C4 Th1 2.675(4) . ?
C5 H5 0.9300 . ?
C5 Th1 2.750(4) . ?
C6 C7 1.524(6) . ?
C6 C8 1.544(5) . ?
C6 C9 1.540(6) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.538(6) . ?
C10 C12 1.531(6) . ?
C10 C13 1.549(6) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.550(6) . ?
C14 C16 1.535(6) . ?
C14 C17 1.531(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 Th1 2.515(5) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.442(5) . ?
C18 C22 1.430(5) . ?
C18 C23 1.535(5) . ?
C18 Th1 2.853(4) . ?
C19 C20 1.427(5) . ?
C19 C27 1.547(5) . ?
C19 Th1 2.828(4) . ?
C20 H20 0.9300 . ?
C20 C21 1.402(5) . ?
C20 Th1 2.845(4) . ?
C21 C22 1.411(5) . ?
C21 C31 1.535(5) . ?
C21 Th1 2.923(4) . ?
C22 H22 0.9300 . ?
C22 Th1 2.867(4) . ?
C23 C24 1.544(5) . ?
C23 C25 1.534(6) . ?
C23 C26 1.548(5) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.549(6) . ?
C27 C29 1.530(6) . ?
C27 C30 1.538(6) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32 1.531(6) . ?
C31 C33 1.526(6) . ?
C31 C34 1.525(6) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 C36 1.461(6) . ?
C35 C40 1.360(6) . ?
C35 O1 1.379(5) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 C37 1.514(6) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 C38 1.497(7) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 C39 1.500(6) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 C40 1.516(6) . ?
C40 H40 0.9300 . ?
O1 Th1 2.153(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 133.4(3) . . ?
C2 C1 Th1 75.3(2) . . ?
C5 C1 C2 106.5(3) . . ?
C5 C1 C6 119.5(4) . . ?
C5 C1 Th1 68.6(2) . . ?
C6 C1 Th1 126.6(2) . . ?
C1 C2 C10 132.6(3) . . ?
C1 C2 Th1 76.2(2) . . ?
C3 C2 C1 106.3(3) . . ?
C3 C2 C10 119.8(3) . . ?
C3 C2 Th1 68.1(2) . . ?
C10 C2 Th1 129.4(3) . . ?
C2 C3 H3 124.9 . . ?
C2 C3 Th1 82.7(2) . . ?
C4 C3 C2 110.2(3) . . ?
C4 C3 H3 124.9 . . ?
C4 C3 Th1 72.8(2) . . ?
Th1 C3 H3 111.7 . . ?
C3 C4 C5 106.4(3) . . ?
C3 C4 C14 126.4(4) . . ?
C3 C4 Th1 77.1(2) . . ?
C5 C4 C14 124.8(3) . . ?
C5 C4 Th1 77.9(2) . . ?
C14 C4 Th1 97.6(2) . . ?
C1 C5 H5 124.7 . . ?
C1 C5 Th1 82.6(2) . . ?
C4 C5 C1 110.5(3) . . ?
C4 C5 H5 124.7 . . ?
C4 C5 Th1 72.0(2) . . ?
Th1 C5 H5 112.6 . . ?
C7 C6 C1 110.9(3) . . ?
C7 C6 C8 105.9(3) . . ?
C7 C6 C9 106.1(3) . . ?
C8 C6 C1 110.3(3) . . ?
C9 C6 C1 113.1(3) . . ?
C9 C6 C8 110.2(3) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C2 C10 C13 109.9(3) . . ?
C11 C10 C2 108.2(3) . . ?
C11 C10 C13 107.3(3) . . ?
C12 C10 C2 115.8(3) . . ?
C12 C10 C11 109.3(3) . . ?
C12 C10 C13 106.0(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C4 C14 C15 103.6(3) . . ?
C4 C14 C16 110.9(3) . . ?
C4 C14 C17 110.4(3) . . ?
C16 C14 C15 111.2(3) . . ?
C17 C14 C15 112.8(4) . . ?
C17 C14 C16 107.9(3) . . ?
C14 C15 H15A 111.1 . . ?
C14 C15 H15B 111.1 . . ?
C14 C15 Th1 103.5(3) . . ?
H15A C15 H15B 109.0 . . ?
Th1 C15 H15A 111.1 . . ?
Th1 C15 H15B 111.1 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C23 132.6(3) . . ?
C19 C18 Th1 74.4(2) . . ?
C22 C18 C19 106.3(3) . . ?
C22 C18 C23 121.1(3) . . ?
C22 C18 Th1 76.1(2) . . ?
C23 C18 Th1 115.8(2) . . ?
C18 C19 C27 134.0(3) . . ?
C18 C19 Th1 76.2(2) . . ?
C20 C19 C18 106.4(3) . . ?
C20 C19 C27 118.6(3) . . ?
C20 C19 Th1 76.1(2) . . ?
C27 C19 Th1 121.6(3) . . ?
C19 C20 H20 124.6 . . ?
C19 C20 Th1 74.8(2) . . ?
C21 C20 C19 110.7(3) . . ?
C21 C20 H20 124.6 . . ?
C21 C20 Th1 79.1(2) . . ?
Th1 C20 H20 113.5 . . ?
C20 C21 C22 106.0(3) . . ?
C20 C21 C31 126.7(4) . . ?
C20 C21 Th1 72.8(2) . . ?
C22 C21 C31 126.0(4) . . ?
C22 C21 Th1 73.7(2) . . ?
C31 C21 Th1 128.3(2) . . ?
C18 C22 H22 124.8 . . ?
C18 C22 Th1 74.9(2) . . ?
C21 C22 C18 110.4(3) . . ?
C21 C22 H22 124.8 . . ?
C21 C22 Th1 78.1(2) . . ?
Th1 C22 H22 114.1 . . ?
C18 C23 C24 112.1(3) . . ?
C18 C23 C26 110.3(3) . . ?
C24 C23 C26 105.2(3) . . ?
C25 C23 C18 111.2(3) . . ?
C25 C23 C24 110.3(3) . . ?
C25 C23 C26 107.5(3) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C19 C27 C28 107.7(3) . . ?
C29 C27 C19 115.8(3) . . ?
C29 C27 C28 109.6(3) . . ?
C29 C27 C30 105.5(4) . . ?
C30 C27 C19 110.0(3) . . ?
C30 C27 C28 107.9(4) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C21 111.2(3) . . ?
C33 C31 C21 112.4(3) . . ?
C33 C31 C32 109.3(4) . . ?
C34 C31 C21 107.9(3) . . ?
C34 C31 C32 107.7(4) . . ?
C34 C31 C33 108.2(4) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C40 C35 C36 123.9(4) . . ?
C40 C35 O1 119.7(4) . . ?
O1 C35 C36 116.4(4) . . ?
C35 C36 H36A 108.7 . . ?
C35 C36 H36B 108.7 . . ?
C35 C36 C37 114.2(4) . . ?
H36A C36 H36B 107.6 . . ?
C37 C36 H36A 108.7 . . ?
C37 C36 H36B 108.7 . . ?
C36 C37 H37A 109.1 . . ?
C36 C37 H37B 109.1 . . ?
H37A C37 H37B 107.9 . . ?
C38 C37 C36 112.4(4) . . ?
C38 C37 H37A 109.1 . . ?
C38 C37 H37B 109.1 . . ?
C37 C38 H38A 109.0 . . ?
C37 C38 H38B 109.0 . . ?
C37 C38 C39 112.9(4) . . ?
H38A C38 H38B 107.8 . . ?
C39 C38 H38A 109.0 . . ?
C39 C38 H38B 109.0 . . ?
C38 C39 H39A 109.0 . . ?
C38 C39 H39B 109.0 . . ?
C38 C39 C40 113.0(4) . . ?
H39A C39 H39B 107.8 . . ?
C40 C39 H39A 109.0 . . ?
C40 C39 H39B 109.0 . . ?
C35 C40 C39 121.0(4) . . ?
C35 C40 H40 119.5 . . ?
C39 C40 H40 119.5 . . ?
C35 O1 Th1 161.7(3) . . ?
C2 Th1 C1 28.58(11) . . ?
C2 Th1 C21 110.79(11) . . ?
C3 Th1 C1 47.93(11) . . ?
C3 Th1 C2 29.25(11) . . ?
C3 Th1 C5 48.57(12) . . ?
C3 Th1 C18 125.99(11) . . ?
C3 Th1 C19 144.99(12) . . ?
C3 Th1 C20 121.82(11) . . ?
C3 Th1 C21 97.85(11) . . ?
C3 Th1 C22 99.86(11) . . ?
C4 Th1 C1 48.86(11) . . ?
C4 Th1 C2 49.06(11) . . ?
C4 Th1 C3 30.15(11) . . ?
C4 Th1 C5 30.04(12) . . ?
C4 Th1 C18 155.15(11) . . ?
C4 Th1 C19 156.45(12) . . ?
C4 Th1 C20 127.64(12) . . ?
C4 Th1 C21 114.67(11) . . ?
C4 Th1 C22 126.75(11) . . ?
C5 Th1 C1 28.89(11) . . ?
C5 Th1 C2 47.78(11) . . ?
C5 Th1 C18 157.59(11) . . ?
C5 Th1 C19 166.07(12) . . ?
C5 Th1 C20 154.28(11) . . ?
C5 Th1 C21 144.13(11) . . ?
C5 Th1 C22 146.03(11) . . ?
C15 Th1 C1 102.27(12) . . ?
C15 Th1 C2 102.24(12) . . ?
C15 Th1 C3 74.89(13) . . ?
C15 Th1 C4 55.31(13) . . ?
C15 Th1 C5 75.37(13) . . ?
C15 Th1 C18 126.44(13) . . ?
C15 Th1 C19 103.17(13) . . ?
C15 Th1 C20 78.99(13) . . ?
C15 Th1 C21 84.54(13) . . ?
C15 Th1 C22 112.29(13) . . ?
C18 Th1 C1 128.89(11) . . ?
C18 Th1 C2 115.06(11) . . ?
C18 Th1 C21 47.64(10) . . ?
C18 Th1 C22 28.96(10) . . ?
C19 Th1 C1 154.30(11) . . ?
C19 Th1 C2 144.07(11) . . ?
C19 Th1 C18 29.40(11) . . ?
C19 Th1 C20 29.14(11) . . ?
C19 Th1 C21 47.73(10) . . ?
C19 Th1 C22 47.59(11) . . ?
C20 Th1 C1 167.44(11) . . ?
C20 Th1 C2 138.86(11) . . ?
C20 Th1 C18 47.57(11) . . ?
C20 Th1 C21 28.10(11) . . ?
C20 Th1 C22 46.33(11) . . ?
C21 Th1 C1 139.35(11) . . ?
C22 Th1 C1 123.49(11) . . ?
C22 Th1 C2 98.94(11) . . ?
C22 Th1 C21 28.18(11) . . ?
O1 Th1 C1 86.17(11) . . ?
O1 Th1 C2 114.46(11) . . ?
O1 Th1 C3 127.17(11) . . ?
O1 Th1 C4 102.66(11) . . ?
O1 Th1 C5 78.62(11) . . ?
O1 Th1 C15 95.63(13) . . ?
O1 Th1 C18 101.75(11) . . ?
O1 Th1 C19 87.81(11) . . ?
O1 Th1 C20 106.21(11) . . ?
O1 Th1 C21 133.54(10) . . ?
O1 Th1 C22 130.58(10) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.914
_oxdiff_exptl_absorpt_empirical_full_min 0.612
####################################################################### 
# 
# 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_compound3
_database_code_depnum_ccdc_archive 'CCDC 1883600'
_audit_update_record             
;
2018-12-06 deposited with the CCDC.
2019-01-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H68 Se2 Th'
_chemical_formula_sum            'C46 H68 Se2 Th'
_chemical_formula_weight         1010.96

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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   22.726(6)
_cell_length_b                   20.038(5)
_cell_length_c                   19.906(5)
_cell_angle_alpha                90
_cell_angle_beta                 104.794(3)
_cell_angle_gamma                90
_cell_volume                     8764(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9667
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      27.50

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_F_000             4016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    5.093
_shelx_estimated_absorpt_T_min   0.310
_shelx_estimated_absorpt_T_max   0.429
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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            29514
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.584
_diffrn_reflns_theta_max         27.566
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10086
_reflns_number_gt                8665
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0143P)²+2.1978P] 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         10086
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0272
_refine_ls_wR_factor_ref         0.0577
_refine_ls_wR_factor_gt          0.0554
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.38617(13) 0.08564(16) 0.38759(15) 0.0098(6) Uani 1 1 d . . . . .
C2 C 0.35387(13) 0.14811(16) 0.38796(14) 0.0101(6) Uani 1 1 d . . . . .
C3 C 0.32604(13) 0.14353(15) 0.44476(14) 0.0090(6) Uani 1 1 d . . . . .
H3 H 0.3008 0.1770 0.4565 0.011 Uiso 1 1 calc R U . . .
C4 C 0.34100(13) 0.08299(16) 0.48092(15) 0.0105(6) Uani 1 1 d . . . . .
C5 C 0.37502(13) 0.04621(15) 0.44313(15) 0.0098(6) Uani 1 1 d . . . . .
H5 H 0.3886 0.0016 0.4532 0.012 Uiso 1 1 calc R U . . .
C6 C 0.43482(13) 0.06289(16) 0.35022(15) 0.0111(6) Uani 1 1 d . . . . .
C7 C 0.48933(13) 0.11130(17) 0.36732(16) 0.0161(7) Uani 1 1 d . . . . .
H7A H 0.5034 0.1171 0.4178 0.024 Uiso 1 1 calc R U . . .
H7B H 0.4768 0.1546 0.3454 0.024 Uiso 1 1 calc R U . . .
H7C H 0.5225 0.0930 0.3496 0.024 Uiso 1 1 calc R U . . .
C8 C 0.46155(14) -0.00507(16) 0.37854(16) 0.0133(6) Uani 1 1 d . . . . .
H8A H 0.4909 -0.0197 0.3531 0.020 Uiso 1 1 calc R U . . .
H8B H 0.4287 -0.0380 0.3725 0.020 Uiso 1 1 calc R U . . .
H8C H 0.4820 -0.0008 0.4280 0.020 Uiso 1 1 calc R U . . .
C9 C 0.41071(14) 0.05507(18) 0.27158(15) 0.0170(7) Uani 1 1 d . . . . .
H9A H 0.4440 0.0416 0.2515 0.026 Uiso 1 1 calc R U . . .
H9B H 0.3938 0.0977 0.2513 0.026 Uiso 1 1 calc R U . . .
H9C H 0.3788 0.0209 0.2615 0.026 Uiso 1 1 calc R U . . .
C10 C 0.36133(13) 0.21771(16) 0.35844(15) 0.0115(6) Uani 1 1 d . . . . .
C11 C 0.37140(14) 0.21963(17) 0.28486(15) 0.0161(7) Uani 1 1 d . . . . .
H11A H 0.3396 0.1934 0.2533 0.024 Uiso 1 1 calc R U . . .
H11B H 0.4114 0.2007 0.2859 0.024 Uiso 1 1 calc R U . . .
H11C H 0.3696 0.2659 0.2686 0.024 Uiso 1 1 calc R U . . .
C12 C 0.30505(14) 0.26206(16) 0.35700(16) 0.0163(7) Uani 1 1 d . . . . .
H12A H 0.3104 0.3058 0.3372 0.024 Uiso 1 1 calc R U . . .
H12B H 0.3008 0.2679 0.4044 0.024 Uiso 1 1 calc R U . . .
H12C H 0.2684 0.2406 0.3284 0.024 Uiso 1 1 calc R U . . .
C13 C 0.41553(14) 0.25208(17) 0.40956(16) 0.0162(7) Uani 1 1 d . . . . .
H13A H 0.4528 0.2267 0.4118 0.024 Uiso 1 1 calc R U . . .
H13B H 0.4080 0.2538 0.4559 0.024 Uiso 1 1 calc R U . . .
H13C H 0.4201 0.2975 0.3935 0.024 Uiso 1 1 calc R U . . .
C14 C 0.34436(14) 0.07319(16) 0.55860(15) 0.0118(6) Uani 1 1 d . . . . .
C15 C 0.28708(14) 0.09783(18) 0.57848(15) 0.0157(7) Uani 1 1 d . . . . .
H15A H 0.2523 0.0701 0.5555 0.024 Uiso 1 1 calc R U . . .
H15B H 0.2790 0.1443 0.5637 0.024 Uiso 1 1 calc R U . . .
H15C H 0.2934 0.0949 0.6290 0.024 Uiso 1 1 calc R U . . .
C16 C 0.39863(14) 0.11766(18) 0.59607(15) 0.0174(7) Uani 1 1 d . . . . .
H16A H 0.4066 0.1112 0.6464 0.026 Uiso 1 1 calc R U . . .
H16B H 0.3887 0.1646 0.5848 0.026 Uiso 1 1 calc R U . . .
H16C H 0.4349 0.1053 0.5807 0.026 Uiso 1 1 calc R U . . .
C17 C 0.35960(14) 0.00145(17) 0.58206(15) 0.0157(7) Uani 1 1 d . . . . .
H17A H 0.3274 -0.0283 0.5565 0.024 Uiso 1 1 calc R U . . .
H17B H 0.3628 -0.0022 0.6320 0.024 Uiso 1 1 calc R U . . .
H17C H 0.3984 -0.0113 0.5728 0.024 Uiso 1 1 calc R U . . .
C18 C 0.14482(13) 0.03870(15) 0.24059(15) 0.0109(6) Uani 1 1 d . . . . .
C19 C 0.17265(13) 0.10077(15) 0.22743(15) 0.0104(6) Uani 1 1 d . . . . .
C20 C 0.17198(13) 0.14392(16) 0.28446(14) 0.0103(6) Uani 1 1 d . . . . .
H20 H 0.1885 0.1877 0.2902 0.012 Uiso 1 1 calc R U . . .
C21 C 0.14339(13) 0.11251(16) 0.33097(15) 0.0107(6) Uani 1 1 d . . . . .
C22 C 0.12871(13) 0.04789(16) 0.30531(15) 0.0108(6) Uani 1 1 d . . . . .
H22 H 0.1106 0.0147 0.3276 0.013 Uiso 1 1 calc R U . . .
C23 C 0.11444(13) -0.01895(16) 0.19252(15) 0.0122(7) Uani 1 1 d . . . . .
C24 C 0.14745(15) -0.04417(16) 0.13923(16) 0.0170(7) Uani 1 1 d . . . . .
H24A H 0.1223 -0.0779 0.1095 0.025 Uiso 1 1 calc R U . . .
H24B H 0.1865 -0.0640 0.1636 0.025 Uiso 1 1 calc R U . . .
H24C H 0.1546 -0.0068 0.1106 0.025 Uiso 1 1 calc R U . . .
C25 C 0.05056(14) 0.00673(18) 0.15453(16) 0.0186(7) Uani 1 1 d . . . . .
H25A H 0.0546 0.0463 0.1271 0.028 Uiso 1 1 calc R U . . .
H25B H 0.0279 0.0184 0.1887 0.028 Uiso 1 1 calc R U . . .
H25C H 0.0286 -0.0282 0.1236 0.028 Uiso 1 1 calc R U . . .
C26 C 0.10498(15) -0.08046(17) 0.23553(16) 0.0179(7) Uani 1 1 d . . . . .
H26A H 0.0854 -0.1162 0.2041 0.027 Uiso 1 1 calc R U . . .
H26B H 0.0791 -0.0681 0.2661 0.027 Uiso 1 1 calc R U . . .
H26C H 0.1445 -0.0960 0.2637 0.027 Uiso 1 1 calc R U . . .
C27 C 0.19327(14) 0.12683(16) 0.16416(15) 0.0127(7) Uani 1 1 d . . . . .
C28 C 0.24856(14) 0.08748(18) 0.15361(16) 0.0193(7) Uani 1 1 d . . . . .
H28A H 0.2379 0.0401 0.1468 0.029 Uiso 1 1 calc R U . . .
H28B H 0.2828 0.0926 0.1947 0.029 Uiso 1 1 calc R U . . .
H28C H 0.2601 0.1047 0.1127 0.029 Uiso 1 1 calc R U . . .
C29 C 0.14063(14) 0.12652(17) 0.09758(15) 0.0177(7) Uani 1 1 d . . . . .
H29A H 0.1538 0.1487 0.0600 0.027 Uiso 1 1 calc R U . . .
H29B H 0.1056 0.1503 0.1062 0.027 Uiso 1 1 calc R U . . .
H29C H 0.1290 0.0804 0.0842 0.027 Uiso 1 1 calc R U . . .
C30 C 0.21232(14) 0.20074(17) 0.17417(16) 0.0167(7) Uani 1 1 d . . . . .
H30A H 0.2259 0.2161 0.1339 0.025 Uiso 1 1 calc R U . . .
H30B H 0.2456 0.2055 0.2163 0.025 Uiso 1 1 calc R U . . .
H30C H 0.1775 0.2276 0.1787 0.025 Uiso 1 1 calc R U . . .
C31 C 0.11942(13) 0.14925(16) 0.38616(15) 0.0113(6) Uani 1 1 d . . . . .
C32 C 0.06586(15) 0.19262(19) 0.34684(16) 0.0222(8) Uani 1 1 d . . . . .
H32A H 0.0486 0.2166 0.3803 0.033 Uiso 1 1 calc R U . . .
H32B H 0.0345 0.1641 0.3176 0.033 Uiso 1 1 calc R U . . .
H32C H 0.0803 0.2248 0.3176 0.033 Uiso 1 1 calc R U . . .
C33 C 0.16830(14) 0.19455(18) 0.43101(16) 0.0183(7) Uani 1 1 d . . . . .
H33A H 0.2018 0.1672 0.4580 0.028 Uiso 1 1 calc R U . . .
H33B H 0.1506 0.2205 0.4627 0.028 Uiso 1 1 calc R U . . .
H33C H 0.1838 0.2250 0.4010 0.028 Uiso 1 1 calc R U . . .
C34 C 0.09608(15) 0.10123(17) 0.43325(16) 0.0182(7) Uani 1 1 d . . . . .
H34A H 0.1297 0.0732 0.4588 0.027 Uiso 1 1 calc R U . . .
H34B H 0.0640 0.0729 0.4049 0.027 Uiso 1 1 calc R U . . .
H34C H 0.0796 0.1268 0.4662 0.027 Uiso 1 1 calc R U . . .
C35 C 0.34336(13) -0.12176(16) 0.33636(16) 0.0139(7) Uani 1 1 d . . . . .
C36 C 0.35170(14) -0.13315(16) 0.40724(16) 0.0142(7) Uani 1 1 d . . . . .
H36 H 0.3244 -0.1138 0.4308 0.017 Uiso 1 1 calc R U . . .
C37 C 0.39956(14) -0.17253(18) 0.44381(17) 0.0196(7) Uani 1 1 d . . . . .
H37 H 0.4048 -0.1801 0.4921 0.023 Uiso 1 1 calc R U . . .
C38 C 0.43970(15) -0.20086(19) 0.40975(19) 0.0244(8) Uani 1 1 d . . . . .
H38 H 0.4730 -0.2269 0.4349 0.029 Uiso 1 1 calc R U . . .
C39 C 0.43114(15) -0.19102(18) 0.33926(18) 0.0222(8) Uani 1 1 d . . . . .
H39 H 0.4582 -0.2110 0.3159 0.027 Uiso 1 1 calc R U . . .
C40 C 0.38320(14) -0.15217(16) 0.30244(16) 0.0156(7) Uani 1 1 d . . . . .
H40 H 0.3773 -0.1462 0.2538 0.019 Uiso 1 1 calc R U . . .
C41 C 0.16410(13) -0.09966(16) 0.41994(15) 0.0123(6) Uani 1 1 d . . . . .
C42 C 0.18389(15) -0.16162(18) 0.40221(16) 0.0193(7) Uani 1 1 d . . . . .
H42 H 0.2254 -0.1680 0.4027 0.023 Uiso 1 1 calc R U . . .
C43 C 0.14311(16) -0.21357(19) 0.38397(17) 0.0232(8) Uani 1 1 d . . . . .
H43 H 0.1568 -0.2554 0.3715 0.028 Uiso 1 1 calc R U . . .
C44 C 0.08231(16) -0.20570(19) 0.38358(17) 0.0235(8) Uani 1 1 d . . . . .
H44 H 0.0545 -0.2418 0.3713 0.028 Uiso 1 1 calc R U . . .
C45 C 0.06300(15) -0.14455(19) 0.40139(17) 0.0231(8) Uani 1 1 d . . . . .
H45 H 0.0214 -0.1387 0.4008 0.028 Uiso 1 1 calc R U . . .
C46 C 0.10298(14) -0.09134(18) 0.42018(16) 0.0170(7) Uani 1 1 d . . . . .
H46 H 0.0890 -0.0498 0.4331 0.020 Uiso 1 1 calc R U . . .
Se1 Se 0.27799(2) -0.06903(2) 0.28137(2) 0.01385(7) Uani 1 1 d . . . . .
Se2 Se 0.22322(2) -0.03131(2) 0.45768(2) 0.01281(7) Uani 1 1 d . . . . .
Th1 Th 0.25584(2) 0.04921(2) 0.35344(2) 0.00792(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C5 1.433(4) . ?
C1 C2 1.452(4) . ?
C1 C6 1.550(4) . ?
C1 Th1 2.956(3) . ?
C2 C3 1.433(4) . ?
C2 C10 1.539(4) . ?
C2 Th1 2.929(3) . ?
C3 C4 1.407(4) . ?
C3 Th1 2.818(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.415(4) . ?
C4 C14 1.541(4) . ?
C4 Th1 2.852(3) . ?
C5 Th1 2.838(3) . ?
C5 H5 0.9500 . ?
C6 C9 1.529(4) . ?
C6 C8 1.538(4) . ?
C6 C7 1.541(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
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 C11 1.540(4) . ?
C10 C13 1.545(4) . ?
C10 C12 1.552(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C17 1.524(4) . ?
C14 C15 1.536(4) . ?
C14 C16 1.550(4) . ?
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 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C22 1.438(4) . ?
C18 C19 1.449(4) . ?
C18 C23 1.546(4) . ?
C18 Th1 2.926(3) . ?
C19 C20 1.430(4) . ?
C19 C27 1.543(4) . ?
C19 Th1 2.918(3) . ?
C20 C21 1.408(4) . ?
C20 Th1 2.790(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.401(4) . ?
C21 C31 1.533(4) . ?
C21 Th1 2.785(3) . ?
C22 Th1 2.802(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.533(4) . ?
C23 C25 1.544(4) . ?
C23 C26 1.547(4) . ?
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 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C30 1.542(4) . ?
C27 C29 1.542(4) . ?
C27 C28 1.543(4) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
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 C34 1.529(4) . ?
C31 C33 1.532(4) . ?
C31 C32 1.537(4) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.394(4) . ?
C35 C40 1.400(4) . ?
C35 Se1 1.921(3) . ?
C36 C37 1.390(4) . ?
C36 H36 0.9500 . ?
C37 C38 1.389(5) . ?
C37 H37 0.9500 . ?
C38 C39 1.381(5) . ?
C38 H38 0.9500 . ?
C39 C40 1.386(5) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C41 C42 1.396(5) . ?
C41 C46 1.400(4) . ?
C41 Se2 1.931(3) . ?
C42 C43 1.379(5) . ?
C42 H42 0.9500 . ?
C43 C44 1.389(5) . ?
C43 H43 0.9500 . ?
C44 C45 1.378(5) . ?
C44 H44 0.9500 . ?
C45 C46 1.389(5) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
Se1 Th1 2.8799(6) . ?
Se2 Th1 2.8714(6) . ?

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
C5 C1 C2 106.4(2) . . ?
C5 C1 C6 119.7(3) . . ?
C2 C1 C6 132.8(3) . . ?
C5 C1 Th1 71.16(16) . . ?
C2 C1 Th1 74.69(16) . . ?
C6 C1 Th1 127.76(19) . . ?
C3 C2 C1 105.9(3) . . ?
C3 C2 C10 118.2(3) . . ?
C1 C2 C10 132.4(3) . . ?
C3 C2 Th1 71.29(16) . . ?
C1 C2 Th1 76.75(17) . . ?
C10 C2 Th1 132.43(19) . . ?
C4 C3 C2 111.2(3) . . ?
C4 C3 Th1 76.99(18) . . ?
C2 C3 Th1 79.93(17) . . ?
C4 C3 H3 124.4 . . ?
C2 C3 H3 124.4 . . ?
Th1 C3 H3 110.7 . . ?
C3 C4 C5 105.7(2) . . ?
C3 C4 C14 124.5(3) . . ?
C5 C4 C14 125.0(3) . . ?
C3 C4 Th1 74.28(16) . . ?
C5 C4 Th1 75.06(17) . . ?
C14 C4 Th1 135.31(19) . . ?
C4 C5 C1 110.6(3) . . ?
C4 C5 Th1 76.13(17) . . ?
C1 C5 Th1 80.29(17) . . ?
C4 C5 H5 124.7 . . ?
C1 C5 H5 124.7 . . ?
Th1 C5 H5 111.0 . . ?
C9 C6 C8 106.8(3) . . ?
C9 C6 C7 110.4(2) . . ?
C8 C6 C7 104.9(2) . . ?
C9 C6 C1 114.1(2) . . ?
C8 C6 C1 110.3(2) . . ?
C7 C6 C1 109.9(2) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C2 C10 C11 116.3(3) . . ?
C2 C10 C13 107.4(2) . . ?
C11 C10 C13 109.2(2) . . ?
C2 C10 C12 110.8(2) . . ?
C11 C10 C12 106.9(2) . . ?
C13 C10 C12 105.8(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C17 C14 C15 111.5(3) . . ?
C17 C14 C4 112.1(3) . . ?
C15 C14 C4 112.9(2) . . ?
C17 C14 C16 107.7(3) . . ?
C15 C14 C16 108.3(3) . . ?
C4 C14 C16 103.8(2) . . ?
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 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C22 C18 C19 105.9(3) . . ?
C22 C18 C23 118.3(3) . . ?
C19 C18 C23 132.5(3) . . ?
C22 C18 Th1 70.72(16) . . ?
C19 C18 Th1 75.31(16) . . ?
C23 C18 Th1 133.66(19) . . ?
C20 C19 C18 106.4(3) . . ?
C20 C19 C27 120.7(3) . . ?
C18 C19 C27 132.5(3) . . ?
C20 C19 Th1 70.58(16) . . ?
C18 C19 Th1 75.97(16) . . ?
C27 C19 Th1 123.82(18) . . ?
C21 C20 C19 110.6(3) . . ?
C21 C20 Th1 75.18(17) . . ?
C19 C20 Th1 80.50(17) . . ?
C21 C20 H20 124.7 . . ?
C19 C20 H20 124.7 . . ?
Th1 C20 H20 111.7 . . ?
C22 C21 C20 106.3(3) . . ?
C22 C21 C31 127.6(3) . . ?
C20 C21 C31 124.4(3) . . ?
C22 C21 Th1 76.16(17) . . ?
C20 C21 Th1 75.56(17) . . ?
C31 C21 Th1 125.65(19) . . ?
C21 C22 C18 110.7(3) . . ?
C21 C22 Th1 74.81(17) . . ?
C18 C22 Th1 80.30(16) . . ?
C21 C22 H22 124.6 . . ?
C18 C22 H22 124.6 . . ?
Th1 C22 H22 112.3 . . ?
C24 C23 C25 109.6(2) . . ?
C24 C23 C18 117.0(3) . . ?
C25 C23 C18 105.6(3) . . ?
C24 C23 C26 106.4(3) . . ?
C25 C23 C26 106.9(3) . . ?
C18 C23 C26 110.9(2) . . ?
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 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C30 C27 C29 104.2(3) . . ?
C30 C27 C28 107.3(3) . . ?
C29 C27 C28 111.2(2) . . ?
C30 C27 C19 110.7(2) . . ?
C29 C27 C19 111.7(2) . . ?
C28 C27 C19 111.5(3) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C34 C31 C33 109.2(3) . . ?
C34 C31 C21 112.3(3) . . ?
C33 C31 C21 111.4(2) . . ?
C34 C31 C32 108.3(3) . . ?
C33 C31 C32 108.9(3) . . ?
C21 C31 C32 106.6(2) . . ?
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 . . ?
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 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 C40 118.7(3) . . ?
C36 C35 Se1 123.5(2) . . ?
C40 C35 Se1 117.8(2) . . ?
C37 C36 C35 120.6(3) . . ?
C37 C36 H36 119.7 . . ?
C35 C36 H36 119.7 . . ?
C38 C37 C36 120.0(3) . . ?
C38 C37 H37 120.0 . . ?
C36 C37 H37 120.0 . . ?
C39 C38 C37 119.9(3) . . ?
C39 C38 H38 120.1 . . ?
C37 C38 H38 120.1 . . ?
C38 C39 C40 120.3(3) . . ?
C38 C39 H39 119.8 . . ?
C40 C39 H39 119.8 . . ?
C39 C40 C35 120.5(3) . . ?
C39 C40 H40 119.8 . . ?
C35 C40 H40 119.8 . . ?
C42 C41 C46 119.4(3) . . ?
C42 C41 Se2 119.5(2) . . ?
C46 C41 Se2 120.4(3) . . ?
C43 C42 C41 120.0(3) . . ?
C43 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C42 C43 C44 121.1(3) . . ?
C42 C43 H43 119.5 . . ?
C44 C43 H43 119.5 . . ?
C45 C44 C43 118.8(3) . . ?
C45 C44 H44 120.6 . . ?
C43 C44 H44 120.6 . . ?
C44 C45 C46 121.5(3) . . ?
C44 C45 H45 119.3 . . ?
C46 C45 H45 119.3 . . ?
C45 C46 C41 119.3(3) . . ?
C45 C46 H46 120.4 . . ?
C41 C46 H46 120.4 . . ?
C35 Se1 Th1 112.12(9) . . ?
C41 Se2 Th1 113.56(9) . . ?
C21 Th1 C20 29.26(8) . . ?
C21 Th1 C22 29.03(9) . . ?
C20 Th1 C22 47.39(9) . . ?
C21 Th1 C3 98.24(9) . . ?
C20 Th1 C3 93.69(9) . . ?
C22 Th1 C3 126.25(9) . . ?
C21 Th1 C5 143.10(8) . . ?
C20 Th1 C5 138.26(9) . . ?
C22 Th1 C5 161.76(8) . . ?
C3 Th1 C5 46.87(9) . . ?
C21 Th1 C4 114.91(9) . . ?
C20 Th1 C4 119.97(9) . . ?
C22 Th1 C4 135.44(8) . . ?
C3 Th1 C4 28.73(8) . . ?
C5 Th1 C4 28.80(8) . . ?
C21 Th1 Se2 88.64(6) . . ?
C20 Th1 Se2 117.90(6) . . ?
C22 Th1 Se2 78.92(6) . . ?
C3 Th1 Se2 96.82(6) . . ?
C5 Th1 Se2 85.10(6) . . ?
C4 Th1 Se2 74.46(6) . . ?
C21 Th1 Se1 124.37(6) . . ?
C20 Th1 Se1 119.92(6) . . ?
C22 Th1 Se1 96.78(6) . . ?
C3 Th1 Se1 136.97(6) . . ?
C5 Th1 Se1 92.06(6) . . ?
C4 Th1 Se1 118.25(6) . . ?
Se2 Th1 Se1 90.458(19) . . ?
C21 Th1 C19 48.24(8) . . ?
C20 Th1 C19 28.92(8) . . ?
C22 Th1 C19 47.48(8) . . ?
C3 Th1 C19 116.93(9) . . ?
C5 Th1 C19 148.54(8) . . ?
C4 Th1 C19 145.53(9) . . ?
Se2 Th1 C19 126.16(6) . . ?
Se1 Th1 C19 91.16(6) . . ?
C21 Th1 C18 48.20(8) . . ?
C20 Th1 C18 47.49(9) . . ?
C22 Th1 C18 28.98(8) . . ?
C3 Th1 C18 141.14(9) . . ?
C5 Th1 C18 168.11(8) . . ?
C4 Th1 C18 163.00(8) . . ?
Se2 Th1 C18 100.56(6) . . ?
Se1 Th1 C18 77.55(6) . . ?
C19 Th1 C18 28.72(8) . . ?
C21 Th1 C2 109.95(9) . . ?
C20 Th1 C2 92.19(9) . . ?
C22 Th1 C2 137.95(9) . . ?
C3 Th1 C2 28.78(8) . . ?
C5 Th1 C2 47.19(8) . . ?
C4 Th1 C2 47.79(8) . . ?
Se2 Th1 C2 122.13(6) . . ?
Se1 Th1 C2 117.02(6) . . ?
C19 Th1 C2 104.43(8) . . ?
C18 Th1 C2 133.14(9) . . ?
C21 Th1 C1 138.49(9) . . ?
C20 Th1 C1 117.62(9) . . ?
C22 Th1 C1 165.00(9) . . ?
C3 Th1 C1 46.93(8) . . ?
C5 Th1 C1 28.54(8) . . ?
C4 Th1 C1 47.50(8) . . ?
Se2 Th1 C1 113.64(6) . . ?
Se1 Th1 C1 91.46(6) . . ?
C19 Th1 C1 120.10(8) . . ?
C18 Th1 C1 144.21(8) . . ?
C2 Th1 C1 28.56(8) . . ?

_refine_diff_density_max         0.797
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.122

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_compound5
_database_code_depnum_ccdc_archive 'CCDC 1883601'
_audit_update_record             
;
2018-12-06 deposited with the CCDC.
2019-01-23 downloaded from the CCDC.
;
_audit_creation_date             2016-04-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C23 H34 P Th0.5)'
_chemical_formula_sum            'C46 H68 P2 Th'
_chemical_formula_weight         914.98
_chemical_melting_point          ?
_chemical_oxdiff_formula         C1H1P1Th1
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'
Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/n 1'
_space_group_name_Hall           '-P 2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   10.3422(4)
_cell_length_b                   19.3149(5)
_cell_length_c                   21.2672(6)
_cell_angle_alpha                90
_cell_angle_beta                 102.863(3)
_cell_angle_gamma                90
_cell_volume                     4141.7(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9193
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.2080
_cell_measurement_theta_min      3.7670
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.708
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41k (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.870
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38778
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.870
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.827
_diffrn_reflns_theta_min         3.290
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -18.00  10.00   1.00   15.00    --   12.45 -37.00 -30.00   28
  2  ω    -20.00  11.00   1.00   15.00    --  -11.20 -99.00   0.00   31
  3  ω     39.00  92.00   1.00   15.00    --   12.45-178.00  30.00   53
  4  ω    -10.00  27.00   1.00   15.00    --  -11.20 -99.00-180.00   37
  5  ω     13.00  75.00   1.00   15.00    --   12.45  37.00-150.00   62
  6  ω     73.00  99.00   1.00   15.00    --   12.45 178.00-180.00   26
  7  ω    -68.00  52.00   1.00   15.00    --   12.45 -19.00  30.00  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0462126000
_diffrn_orient_matrix_UB_12      0.0057687000
_diffrn_orient_matrix_UB_13      -0.0295833000
_diffrn_orient_matrix_UB_21      0.0442135000
_diffrn_orient_matrix_UB_22      0.0240857000
_diffrn_orient_matrix_UB_23      -0.0092371000
_diffrn_orient_matrix_UB_31      0.0292791000
_diffrn_orient_matrix_UB_32      -0.0271275000
_diffrn_orient_matrix_UB_33      -0.0144703000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7162
_reflns_number_total             10352
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.599
_refine_diff_density_min         -2.806
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         10352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0455
_refine_ls_restrained_S_all      1.129
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0056P)²+12.0397P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0779
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26),
 C28(H28), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0579(5) 0.2181(2) 0.6567(2) 0.0109(10) Uani 1 1 d . . . . .
C2 C 0.0291(5) 0.2894(2) 0.6366(2) 0.0101(10) Uani 1 1 d . . . . .
C3 C 0.1452(5) 0.3156(2) 0.6180(2) 0.0105(10) Uani 1 1 d . . . . .
H3 H 0.1553 0.3616 0.6040 0.013 Uiso 1 1 calc R . . . .
C4 C 0.2417(5) 0.2632(2) 0.6235(2) 0.0091(10) Uani 1 1 d . . . . .
C5 C 0.1890(5) 0.2053(2) 0.6493(2) 0.0116(11) Uani 1 1 d . . . . .
H5 H 0.2353 0.1630 0.6603 0.014 Uiso 1 1 calc R . . . .
C6 C -0.0246(5) 0.1551(3) 0.6676(2) 0.0133(11) Uani 1 1 d . . . . .
C7 C 0.0580(6) 0.1047(3) 0.7169(3) 0.0215(13) Uani 1 1 d . . . . .
H7A H 0.1356 0.0893 0.7014 0.032 Uiso 1 1 calc GR . . . .
H7B H 0.0036 0.0645 0.7223 0.032 Uiso 1 1 calc GR . . . .
H7C H 0.0872 0.1283 0.7584 0.032 Uiso 1 1 calc GR . . . .
C8 C -0.1528(6) 0.1671(3) 0.6913(2) 0.0197(13) Uani 1 1 d . . . . .
H8A H -0.1317 0.1915 0.7328 0.030 Uiso 1 1 calc GR . . . .
H8B H -0.1939 0.1225 0.6967 0.030 Uiso 1 1 calc GR . . . .
H8C H -0.2143 0.1951 0.6596 0.030 Uiso 1 1 calc GR . . . .
C9 C -0.0631(6) 0.1158(3) 0.6023(2) 0.0182(12) Uani 1 1 d . . . . .
H9A H -0.1198 0.1454 0.5701 0.027 Uiso 1 1 calc GR . . . .
H9B H -0.1113 0.0734 0.6081 0.027 Uiso 1 1 calc GR . . . .
H9C H 0.0174 0.1038 0.5877 0.027 Uiso 1 1 calc GR . . . .
C10 C -0.1022(5) 0.3299(3) 0.6207(2) 0.0134(11) Uani 1 1 d . . . . .
C11 C -0.2015(6) 0.2922(3) 0.5660(2) 0.0200(12) Uani 1 1 d . . . . .
H11A H -0.1622 0.2870 0.5284 0.030 Uiso 1 1 calc GR . . . .
H11B H -0.2834 0.3193 0.5540 0.030 Uiso 1 1 calc GR . . . .
H11C H -0.2217 0.2463 0.5811 0.030 Uiso 1 1 calc GR . . . .
C12 C -0.0815(5) 0.4021(3) 0.5930(2) 0.0162(11) Uani 1 1 d . . . . .
H12A H -0.0181 0.4286 0.6252 0.024 Uiso 1 1 calc GR . . . .
H12B H -0.1664 0.4268 0.5824 0.024 Uiso 1 1 calc GR . . . .
H12C H -0.0470 0.3967 0.5540 0.024 Uiso 1 1 calc GR . . . .
C13 C -0.1656(5) 0.3432(3) 0.6783(2) 0.0152(11) Uani 1 1 d . . . . .
H13A H -0.1810 0.2990 0.6979 0.023 Uiso 1 1 calc GR . . . .
H13B H -0.2503 0.3674 0.6635 0.023 Uiso 1 1 calc GR . . . .
H13C H -0.1061 0.3719 0.7102 0.023 Uiso 1 1 calc GR . . . .
C14 C 0.3792(5) 0.2684(2) 0.6092(2) 0.0114(11) Uani 1 1 d . . . . .
C15 C 0.3830(6) 0.3240(2) 0.5586(2) 0.0150(11) Uani 1 1 d . . . . .
H15A H 0.3240 0.3107 0.5176 0.022 Uiso 1 1 calc GR . . . .
H15B H 0.4738 0.3287 0.5525 0.022 Uiso 1 1 calc GR . . . .
H15C H 0.3536 0.3683 0.5730 0.022 Uiso 1 1 calc GR . . . .
C16 C 0.4197(5) 0.1992(2) 0.5851(2) 0.0167(12) Uani 1 1 d . . . . .
H16A H 0.4156 0.1632 0.6170 0.025 Uiso 1 1 calc GR . . . .
H16B H 0.5104 0.2025 0.5786 0.025 Uiso 1 1 calc GR . . . .
H16C H 0.3591 0.1875 0.5441 0.025 Uiso 1 1 calc GR . . . .
C17 C 0.4772(5) 0.2864(2) 0.6726(2) 0.0142(11) Uani 1 1 d . . . . .
H17A H 0.4543 0.3317 0.6880 0.021 Uiso 1 1 calc GR . . . .
H17B H 0.5674 0.2880 0.6653 0.021 Uiso 1 1 calc GR . . . .
H17C H 0.4723 0.2510 0.7050 0.021 Uiso 1 1 calc GR . . . .
C18 C 0.1287(5) 0.4738(2) 0.8266(2) 0.0106(11) Uani 1 1 d . . . . .
C19 C 0.0014(6) 0.4780(2) 0.8379(2) 0.0145(11) Uani 1 1 d . . . . .
H19 H -0.0716 0.4624 0.8056 0.017 Uiso 1 1 calc R . . . .
C20 C -0.0216(6) 0.5046(3) 0.8953(3) 0.0203(13) Uani 1 1 d . . . . .
H20 H -0.1093 0.5073 0.9020 0.024 Uiso 1 1 calc R . . . .
C21 C 0.0852(6) 0.5272(3) 0.9427(2) 0.0219(14) Uani 1 1 d . . . . .
H21 H 0.0708 0.5446 0.9823 0.026 Uiso 1 1 calc R . . . .
C22 C 0.2122(6) 0.5244(2) 0.9323(2) 0.0193(13) Uani 1 1 d . . . . .
H22 H 0.2849 0.5404 0.9647 0.023 Uiso 1 1 calc R . . . .
C23 C 0.2337(6) 0.4984(2) 0.8747(2) 0.0165(12) Uani 1 1 d . . . . .
H23 H 0.3213 0.4972 0.8677 0.020 Uiso 1 1 calc R . . . .
C24 C 0.1588(5) 0.2167(2) 0.3719(2) 0.0107(11) Uani 1 1 d . . . . .
C25 C 0.1636(5) 0.2872(2) 0.3492(2) 0.0103(10) Uani 1 1 d . . . . .
C26 C 0.2988(6) 0.3000(2) 0.3488(2) 0.0115(11) Uani 1 1 d . . . . .
H26 H 0.3310 0.3420 0.3347 0.014 Uiso 1 1 calc R . . . .
C27 C 0.3793(5) 0.2422(2) 0.3721(2) 0.0097(10) Uani 1 1 d . . . . .
C28 C 0.2894(5) 0.1906(2) 0.3832(2) 0.0117(11) Uani 1 1 d . . . . .
H28 H 0.3138 0.1446 0.3965 0.014 Uiso 1 1 calc R . . . .
C29 C 0.0484(6) 0.1769(3) 0.3952(2) 0.0156(11) Uani 1 1 d . . . . .
C30 C 0.0111(6) 0.2164(3) 0.4522(2) 0.0191(12) Uani 1 1 d . . . . .
H30A H 0.0912 0.2247 0.4859 0.029 Uiso 1 1 calc GR . . . .
H30B H -0.0518 0.1887 0.4700 0.029 Uiso 1 1 calc GR . . . .
H30C H -0.0298 0.2608 0.4368 0.029 Uiso 1 1 calc GR . . . .
C31 C -0.0759(5) 0.1631(3) 0.3421(2) 0.0160(11) Uani 1 1 d . . . . .
H31A H -0.1104 0.2070 0.3221 0.024 Uiso 1 1 calc GR . . . .
H31B H -0.1436 0.1408 0.3609 0.024 Uiso 1 1 calc GR . . . .
H31C H -0.0531 0.1326 0.3093 0.024 Uiso 1 1 calc GR . . . .
C32 C 0.0993(6) 0.1056(3) 0.4227(2) 0.0174(12) Uani 1 1 d . . . . .
H32A H 0.1292 0.0788 0.3895 0.026 Uiso 1 1 calc GR . . . .
H32B H 0.0275 0.0806 0.4362 0.026 Uiso 1 1 calc GR . . . .
H32C H 0.1734 0.1120 0.4599 0.026 Uiso 1 1 calc GR . . . .
C33 C 0.0699(6) 0.3505(2) 0.3425(2) 0.0151(11) Uani 1 1 d . . . . .
C34 C -0.0796(5) 0.3385(3) 0.3244(2) 0.0169(12) Uani 1 1 d . . . . .
H34A H -0.1258 0.3830 0.3221 0.025 Uiso 1 1 calc GR . . . .
H34B H -0.1058 0.3092 0.3571 0.025 Uiso 1 1 calc GR . . . .
H34C H -0.1034 0.3154 0.2823 0.025 Uiso 1 1 calc GR . . . .
C35 C 0.0981(6) 0.4014(3) 0.2914(2) 0.0200(13) Uani 1 1 d . . . . .
H35A H 0.0828 0.3781 0.2494 0.030 Uiso 1 1 calc GR . . . .
H35B H 0.1905 0.4169 0.3038 0.030 Uiso 1 1 calc GR . . . .
H35C H 0.0389 0.4414 0.2886 0.030 Uiso 1 1 calc GR . . . .
C36 C 0.1027(6) 0.3891(3) 0.4081(2) 0.0188(12) Uani 1 1 d . . . . .
H36A H 0.0490 0.4313 0.4051 0.028 Uiso 1 1 calc GR . . . .
H36B H 0.1969 0.4014 0.4189 0.028 Uiso 1 1 calc GR . . . .
H36C H 0.0827 0.3590 0.4418 0.028 Uiso 1 1 calc GR . . . .
C37 C 0.5268(5) 0.2361(2) 0.3785(2) 0.0119(11) Uani 1 1 d . . . . .
C38 C 0.5517(5) 0.2178(2) 0.3120(2) 0.0141(11) Uani 1 1 d . . . . .
H38A H 0.5114 0.1728 0.2983 0.021 Uiso 1 1 calc GR . . . .
H38B H 0.6474 0.2155 0.3146 0.021 Uiso 1 1 calc GR . . . .
H38C H 0.5122 0.2533 0.2808 0.021 Uiso 1 1 calc GR . . . .
C39 C 0.5861(5) 0.1799(3) 0.4277(2) 0.0163(12) Uani 1 1 d . . . . .
H39A H 0.5708 0.1922 0.4702 0.025 Uiso 1 1 calc GR . . . .
H39B H 0.6817 0.1763 0.4303 0.025 Uiso 1 1 calc GR . . . .
H39C H 0.5437 0.1354 0.4140 0.025 Uiso 1 1 calc GR . . . .
C40 C 0.5928(5) 0.3058(2) 0.3997(2) 0.0164(11) Uani 1 1 d . . . . .
H40A H 0.5616 0.3405 0.3661 0.025 Uiso 1 1 calc GR . . . .
H40B H 0.6893 0.3010 0.4067 0.025 Uiso 1 1 calc GR . . . .
H40C H 0.5697 0.3206 0.4400 0.025 Uiso 1 1 calc GR . . . .
C41 C 0.0431(6) 0.0313(2) 0.1833(2) 0.0169(12) Uani 1 1 d . . . . .
C42 C -0.0936(6) 0.0338(2) 0.1780(3) 0.0197(12) Uani 1 1 d . . . . .
H42 H -0.1268 0.0530 0.2124 0.024 Uiso 1 1 calc R . . . .
C43 C -0.1824(7) 0.0091(3) 0.1241(3) 0.0300(15) Uani 1 1 d . . . . .
H43 H -0.2752 0.0117 0.1214 0.036 Uiso 1 1 calc R . . . .
C44 C -0.1344(7) -0.0194(3) 0.0742(3) 0.0326(17) Uani 1 1 d . . . . .
H44 H -0.1944 -0.0358 0.0366 0.039 Uiso 1 1 calc R . . . .
C45 C 0.0011(7) -0.0240(3) 0.0789(3) 0.0280(15) Uani 1 1 d . . . . .
H45 H 0.0338 -0.0443 0.0447 0.034 Uiso 1 1 calc R . . . .
C46 C 0.0892(6) 0.0007(2) 0.1331(3) 0.0215(13) Uani 1 1 d . . . . .
H46 H 0.1819 -0.0032 0.1361 0.026 Uiso 1 1 calc R . . . .
P1 P 0.14529(15) 0.43809(6) 0.74868(6) 0.0116(3) Uani 1 1 d . . . . .
P2 P 0.15047(15) 0.06491(7) 0.25810(6) 0.0131(3) Uani 1 1 d . . . . .
Th1 Th 0.2500 0.29998(2) 0.7500 0.00816(7) Uani 1 2 d S T P . .
Th2 Th 0.2500 0.20318(2) 0.2500 0.00905(7) Uani 1 2 d S T P . .


_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
C1 C2 1.452(6) . ?
C1 C5 1.422(7) . ?
C1 C6 1.534(7) . ?
C1 Th1 2.937(5) . ?
C2 C3 1.437(7) . ?
C2 C10 1.539(7) . ?
C2 Th1 2.936(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.408(7) . ?
C3 Th1 2.791(5) . ?
C4 C5 1.406(7) . ?
C4 C14 1.523(7) . ?
C4 Th1 2.765(4) . ?
C5 H5 0.9500 . ?
C5 Th1 2.780(5) . ?
C6 C7 1.542(7) . ?
C6 C8 1.537(7) . ?
C6 C9 1.553(7) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
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 C11 1.552(7) . ?
C10 C12 1.546(7) . ?
C10 C13 1.534(7) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.527(6) . ?
C14 C16 1.523(6) . ?
C14 C17 1.536(7) . ?
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 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.392(7) . ?
C18 C23 1.399(7) . ?
C18 P1 1.837(5) . ?
C19 H19 0.9500 . ?
C19 C20 1.394(7) . ?
C20 H20 0.9500 . ?
C20 C21 1.389(8) . ?
C21 H21 0.9500 . ?
C21 C22 1.380(8) . ?
C22 H22 0.9500 . ?
C22 C23 1.389(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.449(6) . ?
C24 C28 1.411(7) . ?
C24 C29 1.547(7) . ?
C24 Th2 2.961(5) . ?
C25 C26 1.422(7) . ?
C25 C33 1.547(7) . ?
C25 Th2 2.954(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.415(7) . ?
C26 Th2 2.773(5) . ?
C27 C28 1.417(7) . ?
C27 C37 1.506(7) . ?
C27 Th2 2.747(5) . ?
C28 H28 0.9500 . ?
C28 Th2 2.781(5) . ?
C29 C30 1.554(7) . ?
C29 C31 1.533(7) . ?
C29 C32 1.542(7) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.526(8) . ?
C33 C35 1.539(7) . ?
C33 C36 1.552(7) . ?
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 C38 1.534(6) . ?
C37 C39 1.538(7) . ?
C37 C40 1.531(7) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C38 Th2 3.118(5) . ?
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 1.394(8) . ?
C41 C46 1.393(7) . ?
C41 P2 1.844(5) . ?
C42 H42 0.9500 . ?
C42 C43 1.385(8) . ?
C43 H43 0.9500 . ?
C43 C44 1.382(9) . ?
C44 H44 0.9500 . ?
C44 C45 1.385(9) . ?
C45 H45 0.9500 . ?
C45 C46 1.386(8) . ?
C46 H46 0.9500 . ?
P1 P1 2.154(3) 2_556 ?
P1 Th1 2.8769(13) . ?
P2 P2 2.162(3) 2 ?
P2 Th2 2.8812(13) . ?
Th1 C1 2.937(5) 2_556 ?
Th1 C2 2.936(5) 2_556 ?
Th1 C3 2.791(5) 2_556 ?
Th1 C4 2.765(4) 2_556 ?
Th1 C5 2.780(5) 2_556 ?
Th1 P1 2.8769(13) 2_556 ?
Th2 C24 2.961(5) 2 ?
Th2 C25 2.954(4) 2 ?
Th2 C26 2.774(5) 2 ?
Th2 C27 2.747(5) 2 ?
Th2 C28 2.781(5) 2 ?
Th2 P2 2.8812(13) 2 ?

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
C2 C1 C6 135.4(5) . . ?
C2 C1 Th1 75.7(3) . . ?
C5 C1 C2 105.7(4) . . ?
C5 C1 C6 117.1(4) . . ?
C5 C1 Th1 69.5(3) . . ?
C6 C1 Th1 129.9(3) . . ?
C1 C2 C10 131.4(5) . . ?
C1 C2 Th1 75.7(3) . . ?
C3 C2 C1 106.6(4) . . ?
C3 C2 C10 120.7(4) . . ?
C3 C2 Th1 69.9(3) . . ?
C10 C2 Th1 129.2(3) . . ?
C2 C3 H3 124.9 . . ?
C2 C3 Th1 81.2(3) . . ?
C4 C3 C2 110.1(4) . . ?
C4 C3 H3 124.9 . . ?
C4 C3 Th1 74.3(3) . . ?
Th1 C3 H3 111.7 . . ?
C3 C4 C14 127.7(4) . . ?
C3 C4 Th1 76.3(3) . . ?
C5 C4 C3 105.9(4) . . ?
C5 C4 C14 126.2(4) . . ?
C5 C4 Th1 75.9(3) . . ?
C14 C4 Th1 110.4(3) . . ?
C1 C5 H5 124.2 . . ?
C1 C5 Th1 81.8(3) . . ?
C4 C5 C1 111.5(4) . . ?
C4 C5 H5 124.2 . . ?
C4 C5 Th1 74.7(3) . . ?
Th1 C5 H5 111.1 . . ?
C1 C6 C7 111.1(4) . . ?
C1 C6 C8 118.6(4) . . ?
C1 C6 C9 107.1(4) . . ?
C7 C6 C9 107.0(4) . . ?
C8 C6 C7 105.0(4) . . ?
C8 C6 C9 107.4(4) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C2 C10 C11 109.3(4) . . ?
C2 C10 C12 110.7(4) . . ?
C12 C10 C11 105.3(4) . . ?
C13 C10 C2 115.0(4) . . ?
C13 C10 C11 110.3(4) . . ?
C13 C10 C12 105.8(4) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C4 C14 C15 111.1(4) . . ?
C4 C14 C17 107.6(4) . . ?
C15 C14 C17 110.2(4) . . ?
C16 C14 C4 110.3(4) . . ?
C16 C14 C15 109.1(4) . . ?
C16 C14 C17 108.5(4) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C23 117.6(4) . . ?
C19 C18 P1 117.4(4) . . ?
C23 C18 P1 125.0(4) . . ?
C18 C19 H19 119.1 . . ?
C18 C19 C20 121.7(5) . . ?
C20 C19 H19 119.1 . . ?
C19 C20 H20 120.4 . . ?
C21 C20 C19 119.2(5) . . ?
C21 C20 H20 120.4 . . ?
C20 C21 H21 119.9 . . ?
C22 C21 C20 120.3(5) . . ?
C22 C21 H21 119.9 . . ?
C21 C22 H22 120.0 . . ?
C21 C22 C23 120.0(5) . . ?
C23 C22 H22 120.0 . . ?
C18 C23 H23 119.4 . . ?
C22 C23 C18 121.2(5) . . ?
C22 C23 H23 119.4 . . ?
C25 C24 C29 131.0(5) . . ?
C25 C24 Th2 75.6(3) . . ?
C28 C24 C25 106.9(4) . . ?
C28 C24 C29 121.0(4) . . ?
C28 C24 Th2 68.8(3) . . ?
C29 C24 Th2 129.6(3) . . ?
C24 C25 C33 135.0(5) . . ?
C24 C25 Th2 76.1(3) . . ?
C26 C25 C24 105.8(4) . . ?
C26 C25 C33 117.3(4) . . ?
C26 C25 Th2 68.7(3) . . ?
C33 C25 Th2 130.6(3) . . ?
C25 C26 H26 124.3 . . ?
C25 C26 Th2 82.8(3) . . ?
C27 C26 C25 111.3(4) . . ?
C27 C26 H26 124.3 . . ?
C27 C26 Th2 74.1(3) . . ?
Th2 C26 H26 110.7 . . ?
C26 C27 C28 104.8(5) . . ?
C26 C27 C37 126.7(4) . . ?
C26 C27 Th2 76.2(3) . . ?
C28 C27 C37 128.3(4) . . ?
C28 C27 Th2 76.5(3) . . ?
C37 C27 Th2 109.6(3) . . ?
C24 C28 C27 111.1(4) . . ?
C24 C28 H28 124.5 . . ?
C24 C28 Th2 83.0(3) . . ?
C27 C28 H28 124.5 . . ?
C27 C28 Th2 73.9(3) . . ?
Th2 C28 H28 110.7 . . ?
C24 C29 C30 109.5(4) . . ?
C31 C29 C24 114.1(4) . . ?
C31 C29 C30 110.3(4) . . ?
C31 C29 C32 106.5(4) . . ?
C32 C29 C24 110.6(4) . . ?
C32 C29 C30 105.4(4) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C25 C33 C36 106.8(4) . . ?
C34 C33 C25 118.8(4) . . ?
C34 C33 C35 105.1(4) . . ?
C34 C33 C36 107.8(4) . . ?
C35 C33 C25 110.9(4) . . ?
C35 C33 C36 106.9(4) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C27 C37 C38 108.0(4) . . ?
C27 C37 C39 111.1(4) . . ?
C27 C37 C40 109.6(4) . . ?
C38 C37 C39 109.9(4) . . ?
C40 C37 C38 108.6(4) . . ?
C40 C37 C39 109.7(4) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
C37 C38 Th2 93.1(3) . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
Th2 C38 H38A 58.3 . . ?
Th2 C38 H38B 157.3 . . ?
Th2 C38 H38C 63.2 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 P2 117.5(4) . . ?
C46 C41 C42 117.8(5) . . ?
C46 C41 P2 124.6(5) . . ?
C41 C42 H42 119.0 . . ?
C43 C42 C41 121.9(6) . . ?
C43 C42 H42 119.0 . . ?
C42 C43 H43 120.4 . . ?
C44 C43 C42 119.2(6) . . ?
C44 C43 H43 120.4 . . ?
C43 C44 H44 119.9 . . ?
C43 C44 C45 120.1(5) . . ?
C45 C44 H44 119.9 . . ?
C44 C45 H45 119.9 . . ?
C44 C45 C46 120.3(6) . . ?
C46 C45 H45 119.9 . . ?
C41 C46 H46 119.7 . . ?
C45 C46 C41 120.7(6) . . ?
C45 C46 H46 119.7 . . ?
C18 P1 P1 105.77(19) . 2_556 ?
C18 P1 Th1 116.70(15) . . ?
P1 P1 Th1 68.01(3) 2_556 . ?
C41 P2 P2 105.9(2) . 2 ?
C41 P2 Th2 115.43(16) . . ?
P2 P2 Th2 67.97(3) 2 . ?
C1 Th1 C1 114.86(19) . 2_556 ?
C2 Th1 C1 28.62(13) 2_556 2_556 ?
C2 Th1 C1 28.62(13) . . ?
C2 Th1 C1 143.38(14) . 2_556 ?
C2 Th1 C1 143.38(14) 2_556 . ?
C2 Th1 C2 171.99(18) . 2_556 ?
C3 Th1 C1 47.62(13) . . ?
C3 Th1 C1 47.62(13) 2_556 2_556 ?
C3 Th1 C1 142.20(13) . 2_556 ?
C3 Th1 C1 142.20(14) 2_556 . ?
C3 Th1 C2 152.92(14) 2_556 . ?
C3 Th1 C2 152.92(14) . 2_556 ?
C3 Th1 C2 28.92(14) . . ?
C3 Th1 C2 28.92(14) 2_556 2_556 ?
C3 Th1 C3 167.61(19) 2_556 . ?
C3 Th1 P1 88.33(10) 2_556 . ?
C3 Th1 P1 80.16(10) 2_556 2_556 ?
C3 Th1 P1 88.33(10) . 2_556 ?
C3 Th1 P1 80.16(10) . . ?
C4 Th1 C1 112.87(13) . 2_556 ?
C4 Th1 C1 48.30(14) . . ?
C4 Th1 C1 48.30(14) 2_556 2_556 ?
C4 Th1 C1 112.87(14) 2_556 . ?
C4 Th1 C2 129.12(14) 2_556 . ?
C4 Th1 C2 48.18(14) 2_556 2_556 ?
C4 Th1 C2 48.18(14) . . ?
C4 Th1 C2 129.12(14) . 2_556 ?
C4 Th1 C3 157.99(15) . 2_556 ?
C4 Th1 C3 29.34(14) . . ?
C4 Th1 C3 29.34(14) 2_556 2_556 ?
C4 Th1 C3 157.99(15) 2_556 . ?
C4 Th1 C4 150.22(19) . 2_556 ?
C4 Th1 C5 29.38(13) 2_556 2_556 ?
C4 Th1 C5 122.24(14) . 2_556 ?
C4 Th1 C5 29.38(13) . . ?
C4 Th1 C5 122.24(14) 2_556 . ?
C4 Th1 P1 107.37(10) 2_556 2_556 ?
C4 Th1 P1 100.25(10) . 2_556 ?
C4 Th1 P1 100.25(10) 2_556 . ?
C4 Th1 P1 107.38(10) . . ?
C5 Th1 C1 99.78(14) . 2_556 ?
C5 Th1 C1 99.78(14) 2_556 . ?
C5 Th1 C1 28.63(14) . . ?
C5 Th1 C1 28.63(14) 2_556 2_556 ?
C5 Th1 C2 126.05(14) . 2_556 ?
C5 Th1 C2 126.04(15) 2_556 . ?
C5 Th1 C2 47.13(14) 2_556 2_556 ?
C5 Th1 C2 47.13(14) . . ?
C5 Th1 C3 47.56(14) 2_556 2_556 ?
C5 Th1 C3 144.76(14) 2_556 . ?
C5 Th1 C3 144.76(14) . 2_556 ?
C5 Th1 C3 47.56(14) . . ?
C5 Th1 C5 97.8(2) . 2_556 ?
C5 Th1 P1 125.58(11) 2_556 2_556 ?
C5 Th1 P1 125.58(11) . . ?
C5 Th1 P1 129.61(10) . 2_556 ?
C5 Th1 P1 129.61(10) 2_556 . ?
P1 Th1 C1 134.61(9) 2_556 . ?
P1 Th1 C1 134.61(9) . 2_556 ?
P1 Th1 C1 107.22(10) . . ?
P1 Th1 C1 107.22(10) 2_556 2_556 ?
P1 Th1 C2 80.47(10) . . ?
P1 Th1 C2 107.17(10) . 2_556 ?
P1 Th1 C2 107.17(10) 2_556 . ?
P1 Th1 C2 80.47(10) 2_556 2_556 ?
P1 Th1 P1 43.97(6) 2_556 . ?
C24 Th2 C24 169.87(17) 2 . ?
C25 Th2 C24 28.36(12) . . ?
C25 Th2 C24 28.36(12) 2 2 ?
C25 Th2 C24 141.53(13) 2 . ?
C25 Th2 C24 141.53(13) . 2 ?
C25 Th2 C25 113.34(18) 2 . ?
C26 Th2 C24 124.33(14) . 2 ?
C26 Th2 C24 46.92(14) . . ?
C26 Th2 C24 46.92(14) 2 2 ?
C26 Th2 C24 124.33(14) 2 . ?
C26 Th2 C25 97.92(13) 2 . ?
C26 Th2 C25 28.53(15) 2 2 ?
C26 Th2 C25 97.92(13) . 2 ?
C26 Th2 C25 28.53(15) . . ?
C26 Th2 C26 95.2(2) . 2 ?
C26 Th2 C28 47.67(14) 2 2 ?
C26 Th2 C28 142.28(14) . 2 ?
C26 Th2 C28 47.67(14) . . ?
C26 Th2 C28 142.28(14) 2 . ?
C26 Th2 P2 125.93(11) . . ?
C26 Th2 P2 131.53(11) . 2 ?
C26 Th2 P2 125.93(11) 2 2 ?
C26 Th2 P2 131.53(11) 2 . ?
C27 Th2 C24 128.33(14) . 2 ?
C27 Th2 C24 48.04(14) 2 2 ?
C27 Th2 C24 48.04(14) . . ?
C27 Th2 C24 128.33(14) 2 . ?
C27 Th2 C25 111.31(13) . 2 ?
C27 Th2 C25 48.35(14) 2 2 ?
C27 Th2 C25 48.35(14) . . ?
C27 Th2 C25 111.31(13) 2 . ?
C27 Th2 C26 119.95(14) . 2 ?
C27 Th2 C26 119.95(14) 2 . ?
C27 Th2 C26 29.70(14) 2 2 ?
C27 Th2 C26 29.70(14) . . ?
C27 Th2 C27 148.20(19) . 2 ?
C27 Th2 C28 29.70(14) . . ?
C27 Th2 C28 156.41(15) . 2 ?
C27 Th2 C28 156.41(15) 2 . ?
C27 Th2 C28 29.70(14) 2 2 ?
C27 Th2 P2 101.85(10) 2 . ?
C27 Th2 P2 107.62(10) . . ?
C27 Th2 P2 101.85(10) . 2 ?
C27 Th2 P2 107.61(10) 2 2 ?
C28 Th2 C24 153.69(15) 2 . ?
C28 Th2 C24 28.23(14) 2 2 ?
C28 Th2 C24 28.23(14) . . ?
C28 Th2 C24 153.69(15) . 2 ?
C28 Th2 C25 47.11(14) 2 2 ?
C28 Th2 C25 140.94(14) . 2 ?
C28 Th2 C25 140.94(14) 2 . ?
C28 Th2 C25 47.11(14) . . ?
C28 Th2 C28 170.0(2) . 2 ?
C28 Th2 P2 80.30(10) 2 2 ?
C28 Th2 P2 80.30(10) . . ?
C28 Th2 P2 90.39(10) 2 . ?
C28 Th2 P2 90.39(10) . 2 ?
P2 Th2 C24 80.90(9) . . ?
P2 Th2 C24 108.78(9) . 2 ?
P2 Th2 C24 108.78(9) 2 . ?
P2 Th2 C24 80.90(9) 2 2 ?
P2 Th2 C25 107.32(10) . . ?
P2 Th2 C25 136.14(9) . 2 ?
P2 Th2 C25 107.31(10) 2 2 ?
P2 Th2 C25 136.14(9) 2 . ?
P2 Th2 P2 44.06(6) . 2 ?

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
C1 C2 C3 C4 2.1(5) . . . . ?
C1 C2 C3 Th1 -67.5(3) . . . . ?
C1 C2 C10 C11 -57.1(6) . . . . ?
C1 C2 C10 C12 -172.6(4) . . . . ?
C1 C2 C10 C13 67.6(7) . . . . ?
C2 C1 C5 C4 -2.2(5) . . . . ?
C2 C1 C5 Th1 67.7(3) . . . . ?
C2 C1 C6 C7 -153.8(5) . . . . ?
C2 C1 C6 C8 -32.0(8) . . . . ?
C2 C1 C6 C9 89.6(6) . . . . ?
C2 C3 C4 C5 -3.4(5) . . . . ?
C2 C3 C4 C14 -179.6(4) . . . . ?
C2 C3 C4 Th1 -74.2(3) . . . . ?
C3 C2 C10 C11 107.6(5) . . . . ?
C3 C2 C10 C12 -7.9(6) . . . . ?
C3 C2 C10 C13 -127.7(5) . . . . ?
C3 C4 C5 C1 3.5(6) . . . . ?
C3 C4 C5 Th1 -71.0(3) . . . . ?
C3 C4 C14 C15 -27.4(7) . . . . ?
C3 C4 C14 C16 -148.6(5) . . . . ?
C3 C4 C14 C17 93.2(6) . . . . ?
C5 C1 C2 C3 0.1(5) . . . . ?
C5 C1 C2 C10 166.3(5) . . . . ?
C5 C1 C2 Th1 -63.5(3) . . . . ?
C5 C1 C6 C7 44.2(6) . . . . ?
C5 C1 C6 C8 166.0(4) . . . . ?
C5 C1 C6 C9 -72.4(5) . . . . ?
C5 C4 C14 C15 157.1(5) . . . . ?
C5 C4 C14 C16 35.9(6) . . . . ?
C5 C4 C14 C17 -82.2(6) . . . . ?
C6 C1 C2 C3 -163.3(5) . . . . ?
C6 C1 C2 C10 2.9(9) . . . . ?
C6 C1 C2 Th1 133.1(5) . . . . ?
C6 C1 C5 C4 164.7(4) . . . . ?
C6 C1 C5 Th1 -125.3(4) . . . . ?
C10 C2 C3 C4 -165.9(4) . . . . ?
C10 C2 C3 Th1 124.5(4) . . . . ?
C14 C4 C5 C1 179.8(4) . . . . ?
C14 C4 C5 Th1 105.2(5) . . . . ?
C18 C19 C20 C21 -0.3(7) . . . . ?
C19 C18 C23 C22 1.7(7) . . . . ?
C19 C18 P1 P1 -178.7(3) . . . 2_556 ?
C19 C18 P1 Th1 -105.7(4) . . . . ?
C19 C20 C21 C22 1.2(7) . . . . ?
C20 C21 C22 C23 -0.7(7) . . . . ?
C21 C22 C23 C18 -0.8(7) . . . . ?
C23 C18 C19 C20 -1.1(7) . . . . ?
C23 C18 P1 P1 2.9(4) . . . 2_556 ?
C23 C18 P1 Th1 75.8(4) . . . . ?
C24 C25 C26 C27 -2.1(5) . . . . ?
C24 C25 C26 Th2 67.8(3) . . . . ?
C24 C25 C33 C34 -35.1(8) . . . . ?
C24 C25 C33 C35 -156.9(5) . . . . ?
C24 C25 C33 C36 87.0(7) . . . . ?
C25 C24 C28 C27 3.1(5) . . . . ?
C25 C24 C28 Th2 -66.6(3) . . . . ?
C25 C24 C29 C30 -56.8(7) . . . . ?
C25 C24 C29 C31 67.4(7) . . . . ?
C25 C24 C29 C32 -172.6(5) . . . . ?
C25 C26 C27 C28 3.8(5) . . . . ?
C25 C26 C27 C37 179.8(4) . . . . ?
C25 C26 C27 Th2 75.5(3) . . . . ?
C26 C25 C33 C34 163.5(4) . . . . ?
C26 C25 C33 C35 41.7(6) . . . . ?
C26 C25 C33 C36 -74.4(5) . . . . ?
C26 C27 C28 C24 -4.2(5) . . . . ?
C26 C27 C28 Th2 71.4(3) . . . . ?
C26 C27 C37 C38 -81.1(6) . . . . ?
C26 C27 C37 C39 158.4(4) . . . . ?
C26 C27 C37 C40 37.1(6) . . . . ?
C27 C37 C38 Th2 -5.0(4) . . . . ?
C28 C24 C25 C26 -0.6(5) . . . . ?
C28 C24 C25 C33 -163.5(5) . . . . ?
C28 C24 C25 Th2 62.1(3) . . . . ?
C28 C24 C29 C30 109.2(5) . . . . ?
C28 C24 C29 C31 -126.6(5) . . . . ?
C28 C24 C29 C32 -6.6(6) . . . . ?
C28 C27 C37 C38 93.9(6) . . . . ?
C28 C27 C37 C39 -26.6(7) . . . . ?
C28 C27 C37 C40 -147.9(5) . . . . ?
C29 C24 C25 C26 166.9(5) . . . . ?
C29 C24 C25 C33 4.0(9) . . . . ?
C29 C24 C25 Th2 -130.5(5) . . . . ?
C29 C24 C28 C27 -165.9(4) . . . . ?
C29 C24 C28 Th2 124.4(4) . . . . ?
C33 C25 C26 C27 164.4(4) . . . . ?
C33 C25 C26 Th2 -125.8(4) . . . . ?
C37 C27 C28 C24 179.9(4) . . . . ?
C37 C27 C28 Th2 -104.4(5) . . . . ?
C39 C37 C38 Th2 116.3(4) . . . . ?
C40 C37 C38 Th2 -123.7(4) . . . . ?
C41 C42 C43 C44 0.5(8) . . . . ?
C42 C41 C46 C45 2.3(7) . . . . ?
C42 C41 P2 P2 -172.4(3) . . . 2 ?
C42 C41 P2 Th2 -99.6(4) . . . . ?
C42 C43 C44 C45 1.0(8) . . . . ?
C43 C44 C45 C46 -0.9(8) . . . . ?
C44 C45 C46 C41 -0.8(8) . . . . ?
C46 C41 C42 C43 -2.2(7) . . . . ?
C46 C41 P2 P2 10.7(4) . . . 2 ?
C46 C41 P2 Th2 83.5(4) . . . . ?
P1 C18 C19 C20 -179.7(4) . . . . ?
P1 C18 C23 C22 -179.9(4) . . . . ?
P2 C41 C42 C43 -179.2(4) . . . . ?
P2 C41 C46 C45 179.1(4) . . . . ?
Th1 C1 C2 C3 63.5(3) . . . . ?
Th1 C1 C2 C10 -130.2(5) . . . . ?
Th1 C1 C5 C4 -70.0(3) . . . . ?
Th1 C1 C6 C7 -41.0(6) . . . . ?
Th1 C1 C6 C8 80.8(6) . . . . ?
Th1 C1 C6 C9 -157.5(3) . . . . ?
Th1 C2 C3 C4 69.6(3) . . . . ?
Th1 C2 C10 C11 -164.2(3) . . . . ?
Th1 C2 C10 C12 80.3(5) . . . . ?
Th1 C2 C10 C13 -39.5(6) . . . . ?
Th1 C3 C4 C5 70.7(3) . . . . ?
Th1 C3 C4 C14 -105.5(5) . . . . ?
Th1 C4 C5 C1 74.6(4) . . . . ?
Th1 C4 C14 C15 -115.7(4) . . . . ?
Th1 C4 C14 C16 123.1(3) . . . . ?
Th1 C4 C14 C17 5.0(4) . . . . ?
Th2 C24 C25 C26 -62.7(3) . . . . ?
Th2 C24 C25 C33 134.5(6) . . . . ?
Th2 C24 C28 C27 69.7(3) . . . . ?
Th2 C24 C29 C30 -163.8(3) . . . . ?
Th2 C24 C29 C31 -39.6(6) . . . . ?
Th2 C24 C29 C32 80.5(5) . . . . ?
Th2 C25 C26 C27 -69.8(3) . . . . ?
Th2 C25 C33 C34 79.1(5) . . . . ?
Th2 C25 C33 C35 -42.8(6) . . . . ?
Th2 C25 C33 C36 -158.9(3) . . . . ?
Th2 C26 C27 C28 -71.7(3) . . . . ?
Th2 C26 C27 C37 104.3(4) . . . . ?
Th2 C27 C28 C24 -75.7(4) . . . . ?
Th2 C27 C37 C38 6.0(4) . . . . ?
Th2 C27 C37 C39 -114.6(3) . . . . ?
Th2 C27 C37 C40 124.1(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.674
_oxdiff_exptl_absorpt_empirical_full_min 0.657
####################################################################### 
# 
# 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_compound6
_database_code_depnum_ccdc_archive 'CCDC 1883598'
_audit_update_record             
;
2018-12-06 deposited with the CCDC.
2019-01-23 downloaded from the CCDC.
;
_audit_creation_date             2018-02-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C67 H102 N P Th, C3 H7'
_chemical_formula_sum            'C70 H109 N P Th'
_chemical_formula_weight         1227.59
_chemical_melting_point          ?
_chemical_oxdiff_formula         C1H1N1P1Th1
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'
Th Th -4.1491 12.3296 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   12.0224(5)
_cell_length_b                   14.9397(6)
_cell_length_c                   19.8170(8)
_cell_angle_alpha                68.243(4)
_cell_angle_beta                 82.483(4)
_cell_angle_gamma                80.226(4)
_cell_volume                     3248.8(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11403
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.0700
_cell_measurement_theta_min      4.4620
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.905
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1282
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0811
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23582
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.328
_diffrn_reflns_theta_min         3.741
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -109.00 -15.00   1.00    1.00    --  -41.49 -57.00 -30.00   94
  2  ω    -70.00  32.00   1.00    1.00    --  -41.49  57.00-150.00  102
  3  ω   -115.00 -27.00   1.00    1.00    --  -41.49 -37.00  60.00   88
  4  ω     13.00  63.00   1.00    1.00    --   41.49 -99.00 -90.00   50
  5  ω     35.00  93.00   1.00    1.00    --   41.49-125.00  60.00   58
  6  ω     81.00 178.00   1.00    1.00    --  107.19  45.00   0.00   97
  7  ω     35.00 135.00   1.00    1.00    --  107.19 -61.00  30.00  100
  8  ω     31.00 133.00   1.00    1.00    --  107.19 -77.00-180.00  102
  9  ω    146.00 178.00   1.00    1.00    --  107.19  45.00-180.00   32
 10  ω     82.00 121.00   1.00    1.00    --  107.19  45.00-180.00   39
 11  ω     40.00 134.00   1.00    1.00    --  107.19 -30.00-180.00   94
 12  ω     84.00 109.00   1.00    1.00    --  107.19 -94.00-180.00   25
 13  ω     35.00  88.00   1.00    1.00    --  107.19 -61.00 -30.00   53
 14  ω     78.00 117.00   1.00    1.00    --  107.19-125.00-180.00   39
 15  ω     81.00 178.00   1.00    1.00    --  107.19  30.00 120.00   97
 16  ω     50.00 119.00   1.00    1.00    --  107.19-125.00   0.00   69
 17  ω     73.00 109.00   1.00    1.00    --  107.19 -94.00  30.00   36
 18  ω     53.00  90.00   1.00    1.00    --  107.19   0.00 150.00   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0209367000
_diffrn_orient_matrix_UB_12      0.0581657000
_diffrn_orient_matrix_UB_13      0.0460446000
_diffrn_orient_matrix_UB_21      -0.1194265000
_diffrn_orient_matrix_UB_22      -0.0118268000
_diffrn_orient_matrix_UB_23      0.0384357000
_diffrn_orient_matrix_UB_31      0.0479459000
_diffrn_orient_matrix_UB_32      -0.0949847000
_diffrn_orient_matrix_UB_33      0.0587145000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11432
_reflns_number_total             12661
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         3.224
_refine_diff_density_min         -2.256
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         12661
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0422
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0406P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1029
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P1-H1
 1.1 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C68(H68A,H68B), C69(H69A,H69B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C20(H20), C22(H22), C37(H37), C39(H39), C55(H55), C56(H56),
 C58(H58), C59(H59), C62(H62), C63(H63), C65(H65), C66(H66)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C42(H42A,H42B,
 H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C), C60(H60A,H60B,H60C), C67(H67A,H67B,H67C), C70(H70A,H70B,
 H70C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.0707(4) 0.6219(3) 0.6487(3) 0.0146(9) Uani 1 1 d . . . . .
C2 C 1.0721(4) 0.7031(3) 0.6712(3) 0.0156(9) Uani 1 1 d . . . . .
C3 C 1.0724(4) 0.6639(3) 0.7491(3) 0.0199(10) Uani 1 1 d . . . . .
H3 H 1.0683 0.7010 0.7783 0.024 Uiso 1 1 calc R . . . .
C4 C 1.0796(4) 0.5618(4) 0.7756(3) 0.0199(10) Uani 1 1 d . . . . .
C5 C 1.0737(4) 0.5377(3) 0.7139(3) 0.0170(10) Uani 1 1 d . . . . .
H5 H 1.0720 0.4750 0.7154 0.020 Uiso 1 1 calc R . . . .
C6 C 1.0827(4) 0.6116(3) 0.5730(3) 0.0163(9) Uani 1 1 d . . . . .
C7 C 0.9763(4) 0.6585(4) 0.5317(3) 0.0190(10) Uani 1 1 d . . . . .
H7A H 0.9132 0.6261 0.5585 0.029 Uiso 1 1 calc GR . . . .
H7B H 0.9878 0.6529 0.4845 0.029 Uiso 1 1 calc GR . . . .
H7C H 0.9613 0.7259 0.5262 0.029 Uiso 1 1 calc GR . . . .
C8 C 1.1040(4) 0.5041(4) 0.5807(3) 0.0205(10) Uani 1 1 d . . . . .
H8A H 1.1725 0.4738 0.6045 0.031 Uiso 1 1 calc GR . . . .
H8B H 1.1110 0.4993 0.5333 0.031 Uiso 1 1 calc GR . . . .
H8C H 1.0417 0.4719 0.6093 0.031 Uiso 1 1 calc GR . . . .
C9 C 1.1862(4) 0.6546(4) 0.5252(3) 0.0208(10) Uani 1 1 d . . . . .
H9A H 1.1756 0.7238 0.5132 0.031 Uiso 1 1 calc GR . . . .
H9B H 1.1944 0.6404 0.4812 0.031 Uiso 1 1 calc GR . . . .
H9C H 1.2530 0.6265 0.5512 0.031 Uiso 1 1 calc GR . . . .
C10 C 1.1048(4) 0.8069(4) 0.6290(3) 0.0197(10) Uani 1 1 d . . . . .
C11 C 1.0488(4) 0.8639(4) 0.5572(3) 0.0206(10) Uani 1 1 d . . . . .
H11A H 1.0721 0.8304 0.5236 0.031 Uiso 1 1 calc GR . . . .
H11B H 1.0714 0.9278 0.5367 0.031 Uiso 1 1 calc GR . . . .
H11C H 0.9680 0.8690 0.5664 0.031 Uiso 1 1 calc GR . . . .
C12 C 1.2350(4) 0.7972(4) 0.6162(3) 0.0254(12) Uani 1 1 d . . . . .
H12A H 1.2681 0.7600 0.6615 0.038 Uiso 1 1 calc GR . . . .
H12B H 1.2588 0.8606 0.5971 0.038 Uiso 1 1 calc GR . . . .
H12C H 1.2592 0.7647 0.5820 0.038 Uiso 1 1 calc GR . . . .
C13 C 1.0732(5) 0.8692(4) 0.6781(3) 0.0248(11) Uani 1 1 d . . . . .
H13A H 0.9960 0.8649 0.6975 0.037 Uiso 1 1 calc GR . . . .
H13B H 1.0820 0.9357 0.6497 0.037 Uiso 1 1 calc GR . . . .
H13C H 1.1221 0.8454 0.7174 0.037 Uiso 1 1 calc GR . . . .
C14 C 1.1338(4) 0.4934(4) 0.8455(3) 0.0198(10) Uani 1 1 d . . . . .
C15 C 1.1314(5) 0.3863(4) 0.8581(3) 0.0246(11) Uani 1 1 d . . . . .
H15A H 1.0543 0.3743 0.8624 0.037 Uiso 1 1 calc GR . . . .
H15B H 1.1667 0.3462 0.9020 0.037 Uiso 1 1 calc GR . . . .
H15C H 1.1716 0.3712 0.8176 0.037 Uiso 1 1 calc GR . . . .
C16 C 1.2587(5) 0.5112(4) 0.8343(3) 0.0293(12) Uani 1 1 d . . . . .
H16A H 1.2931 0.5005 0.7909 0.044 Uiso 1 1 calc GR . . . .
H16B H 1.2983 0.4672 0.8755 0.044 Uiso 1 1 calc GR . . . .
H16C H 1.2625 0.5769 0.8296 0.044 Uiso 1 1 calc GR . . . .
C17 C 1.0809(5) 0.5138(4) 0.9139(3) 0.0266(12) Uani 1 1 d . . . . .
H17A H 1.0753 0.5821 0.9047 0.040 Uiso 1 1 calc GR . . . .
H17B H 1.1275 0.4781 0.9536 0.040 Uiso 1 1 calc GR . . . .
H17C H 1.0067 0.4939 0.9261 0.040 Uiso 1 1 calc GR . . . .
C18 C 0.7425(4) 0.7118(4) 0.8460(3) 0.0219(11) Uani 1 1 d . . . . .
C19 C 0.6484(4) 0.7145(4) 0.8073(3) 0.0186(10) Uani 1 1 d . . . . .
C20 C 0.6386(4) 0.6171(4) 0.8175(3) 0.0222(11) Uani 1 1 d . . . . .
H20 H 0.5886 0.5989 0.7944 0.027 Uiso 1 1 calc R . . . .
C21 C 0.7142(4) 0.5518(4) 0.8669(3) 0.0219(11) Uani 1 1 d . . . . .
C22 C 0.7827(5) 0.6103(4) 0.8811(3) 0.0217(11) Uani 1 1 d . . . . .
H22 H 0.8448 0.5864 0.9091 0.026 Uiso 1 1 calc R . . . .
C23 C 0.7816(5) 0.7876(4) 0.8704(3) 0.0246(11) Uani 1 1 d . . . . .
C24 C 0.8916(5) 0.7472(4) 0.9085(3) 0.0334(13) Uani 1 1 d . . . . .
H24A H 0.8798 0.6909 0.9510 0.050 Uiso 1 1 calc GR . . . .
H24B H 0.9145 0.7959 0.9226 0.050 Uiso 1 1 calc GR . . . .
H24C H 0.9495 0.7295 0.8758 0.050 Uiso 1 1 calc GR . . . .
C25 C 0.6915(6) 0.8094(4) 0.9271(3) 0.0358(14) Uani 1 1 d . . . . .
H25A H 0.6220 0.8394 0.9046 0.054 Uiso 1 1 calc GR . . . .
H25B H 0.7174 0.8525 0.9457 0.054 Uiso 1 1 calc GR . . . .
H25C H 0.6791 0.7498 0.9664 0.054 Uiso 1 1 calc GR . . . .
C26 C 0.8062(5) 0.8821(4) 0.8081(3) 0.0284(12) Uani 1 1 d . . . . .
H26A H 0.8531 0.8667 0.7697 0.043 Uiso 1 1 calc GR . . . .
H26B H 0.8446 0.9193 0.8259 0.043 Uiso 1 1 calc GR . . . .
H26C H 0.7362 0.9193 0.7896 0.043 Uiso 1 1 calc GR . . . .
C27 C 0.5436(4) 0.7907(4) 0.7775(3) 0.0235(11) Uani 1 1 d . . . . .
C28 C 0.4484(5) 0.7662(4) 0.8397(3) 0.0313(13) Uani 1 1 d . . . . .
H28A H 0.4325 0.7014 0.8502 0.047 Uiso 1 1 calc GR . . . .
H28B H 0.3814 0.8114 0.8250 0.047 Uiso 1 1 calc GR . . . .
H28C H 0.4725 0.7707 0.8826 0.047 Uiso 1 1 calc GR . . . .
C29 C 0.5548(5) 0.8986(4) 0.7555(3) 0.0277(12) Uani 1 1 d . . . . .
H29A H 0.5730 0.9107 0.7968 0.041 Uiso 1 1 calc GR . . . .
H29B H 0.4846 0.9371 0.7386 0.041 Uiso 1 1 calc GR . . . .
H29C H 0.6139 0.9157 0.7173 0.041 Uiso 1 1 calc GR . . . .
C30 C 0.5035(4) 0.7787(4) 0.7113(3) 0.0263(12) Uani 1 1 d . . . . .
H30A H 0.5647 0.7843 0.6743 0.039 Uiso 1 1 calc GR . . . .
H30B H 0.4417 0.8284 0.6925 0.039 Uiso 1 1 calc GR . . . .
H30C H 0.4789 0.7159 0.7258 0.039 Uiso 1 1 calc GR . . . .
C31 C 0.7074(5) 0.4446(4) 0.9100(3) 0.0252(11) Uani 1 1 d . . . . .
C32 C 0.6099(5) 0.4121(4) 0.8860(3) 0.0294(12) Uani 1 1 d . . . . .
H32A H 0.5405 0.4517 0.8923 0.044 Uiso 1 1 calc GR . . . .
H32B H 0.6038 0.3453 0.9151 0.044 Uiso 1 1 calc GR . . . .
H32C H 0.6243 0.4190 0.8357 0.044 Uiso 1 1 calc GR . . . .
C33 C 0.8158(5) 0.3801(5) 0.9033(4) 0.0418(16) Uani 1 1 d . . . . .
H33A H 0.8366 0.3902 0.8528 0.063 Uiso 1 1 calc GR . . . .
H33B H 0.8050 0.3133 0.9290 0.063 Uiso 1 1 calc GR . . . .
H33C H 0.8748 0.3956 0.9237 0.063 Uiso 1 1 calc GR . . . .
C34 C 0.6792(6) 0.4337(4) 0.9901(3) 0.0350(14) Uani 1 1 d . . . . .
H34A H 0.7418 0.4479 1.0082 0.052 Uiso 1 1 calc GR . . . .
H34B H 0.6649 0.3684 1.0181 0.052 Uiso 1 1 calc GR . . . .
H34C H 0.6131 0.4782 0.9941 0.052 Uiso 1 1 calc GR . . . .
C35 C 0.7204(4) 0.3793(3) 0.7170(3) 0.0172(10) Uani 1 1 d . . . . .
C36 C 0.6024(4) 0.3924(3) 0.7097(3) 0.0173(10) Uani 1 1 d . . . . .
C37 C 0.5376(4) 0.3221(3) 0.7584(3) 0.0178(10) Uani 1 1 d . . . . .
H37 H 0.4594 0.3336 0.7562 0.021 Uiso 1 1 calc R . . . .
C38 C 0.5837(4) 0.2369(4) 0.8093(3) 0.0194(10) Uani 1 1 d . . . . .
C39 C 0.7013(4) 0.2160(3) 0.8027(3) 0.0197(10) Uani 1 1 d . . . . .
H39 H 0.7343 0.1548 0.8311 0.024 Uiso 1 1 calc R . . . .
C40 C 0.7719(4) 0.2812(3) 0.7560(3) 0.0171(10) Uani 1 1 d . . . . .
C41 C 0.5400(4) 0.4786(3) 0.6489(3) 0.0171(10) Uani 1 1 d . . . . .
C42 C 0.5204(5) 0.5719(4) 0.6669(3) 0.0248(11) Uani 1 1 d . . . . .
H42A H 0.4775 0.5605 0.7130 0.037 Uiso 1 1 calc GR . . . .
H42B H 0.4794 0.6231 0.6296 0.037 Uiso 1 1 calc GR . . . .
H42C H 0.5920 0.5904 0.6692 0.037 Uiso 1 1 calc GR . . . .
C43 C 0.6045(4) 0.4952(4) 0.5743(3) 0.0200(10) Uani 1 1 d . . . . .
H43A H 0.6783 0.5112 0.5752 0.030 Uiso 1 1 calc GR . . . .
H43B H 0.5636 0.5477 0.5378 0.030 Uiso 1 1 calc GR . . . .
H43C H 0.6122 0.4371 0.5631 0.030 Uiso 1 1 calc GR . . . .
C44 C 0.4231(4) 0.4563(4) 0.6405(3) 0.0255(11) Uani 1 1 d . . . . .
H44A H 0.4317 0.3956 0.6328 0.038 Uiso 1 1 calc GR . . . .
H44B H 0.3900 0.5073 0.5995 0.038 Uiso 1 1 calc GR . . . .
H44C H 0.3748 0.4521 0.6838 0.038 Uiso 1 1 calc GR . . . .
C45 C 0.5137(5) 0.1630(4) 0.8670(3) 0.0244(11) Uani 1 1 d . . . . .
C46 C 0.3885(5) 0.2057(4) 0.8716(3) 0.0281(12) Uani 1 1 d . . . . .
H46A H 0.3823 0.2632 0.8833 0.042 Uiso 1 1 calc GR . . . .
H46B H 0.3472 0.1587 0.9088 0.042 Uiso 1 1 calc GR . . . .
H46C H 0.3578 0.2218 0.8255 0.042 Uiso 1 1 calc GR . . . .
C47 C 0.5218(5) 0.0729(4) 0.8452(3) 0.0302(13) Uani 1 1 d . . . . .
H47A H 0.4831 0.0900 0.8019 0.045 Uiso 1 1 calc GR . . . .
H47B H 0.4875 0.0225 0.8840 0.045 Uiso 1 1 calc GR . . . .
H47C H 0.5999 0.0501 0.8363 0.045 Uiso 1 1 calc GR . . . .
C48 C 0.5591(5) 0.1322(4) 0.9421(3) 0.0345(14) Uani 1 1 d . . . . .
H48A H 0.6355 0.1008 0.9410 0.052 Uiso 1 1 calc GR . . . .
H48B H 0.5128 0.0880 0.9778 0.052 Uiso 1 1 calc GR . . . .
H48C H 0.5575 0.1886 0.9547 0.052 Uiso 1 1 calc GR . . . .
C49 C 0.8978(4) 0.2408(4) 0.7458(3) 0.0212(10) Uani 1 1 d . . . . .
C50 C 0.9170(5) 0.1281(4) 0.7758(3) 0.0320(13) Uani 1 1 d . . . . .
H50A H 0.9030 0.1046 0.8278 0.048 Uiso 1 1 calc GR . . . .
H50B H 0.9937 0.1058 0.7632 0.048 Uiso 1 1 calc GR . . . .
H50C H 0.8663 0.1041 0.7549 0.048 Uiso 1 1 calc GR . . . .
C51 C 0.9776(4) 0.2716(4) 0.7851(3) 0.0287(12) Uani 1 1 d . . . . .
H51A H 0.9709 0.3413 0.7679 0.043 Uiso 1 1 calc GR . . . .
H51B H 1.0542 0.2458 0.7754 0.043 Uiso 1 1 calc GR . . . .
H51C H 0.9578 0.2471 0.8366 0.043 Uiso 1 1 calc GR . . . .
C52 C 0.9338(4) 0.2703(4) 0.6636(3) 0.0240(11) Uani 1 1 d . . . . .
H52A H 0.8873 0.2446 0.6412 0.036 Uiso 1 1 calc GR . . . .
H52B H 1.0116 0.2449 0.6570 0.036 Uiso 1 1 calc GR . . . .
H52C H 0.9249 0.3399 0.6414 0.036 Uiso 1 1 calc GR . . . .
C53 C 0.7516(4) 0.8372(3) 0.5860(3) 0.0158(9) Uani 1 1 d . . . . .
C54 C 0.7177(4) 0.9386(3) 0.5869(3) 0.0171(10) Uani 1 1 d . . . . .
C55 C 0.7817(4) 0.9812(4) 0.6166(3) 0.0198(10) Uani 1 1 d . . . . .
H55 H 0.8509 0.9482 0.6342 0.024 Uiso 1 1 calc R . . . .
C56 C 0.7447(4) 1.0724(4) 0.6208(3) 0.0232(11) Uani 1 1 d . . . . .
H56 H 0.7902 1.1001 0.6400 0.028 Uiso 1 1 calc R . . . .
C57 C 0.6401(4) 1.1231(4) 0.5965(3) 0.0212(10) Uani 1 1 d . . . . .
C58 C 0.5759(4) 1.0803(4) 0.5666(3) 0.0243(11) Uani 1 1 d . . . . .
H58 H 0.5058 1.1126 0.5502 0.029 Uiso 1 1 calc R . . . .
C59 C 0.6139(4) 0.9904(4) 0.5607(3) 0.0208(10) Uani 1 1 d . . . . .
H59 H 0.5702 0.9641 0.5392 0.025 Uiso 1 1 calc R . . . .
C60 C 0.5993(5) 1.2207(4) 0.6034(3) 0.0280(12) Uani 1 1 d . . . . .
H60A H 0.5328 1.2161 0.6364 0.042 Uiso 1 1 calc GR . . . .
H60B H 0.5817 1.2679 0.5565 0.042 Uiso 1 1 calc GR . . . .
H60C H 0.6575 1.2403 0.6217 0.042 Uiso 1 1 calc GR . . . .
C61 C 0.7358(4) 0.8265(3) 0.5154(3) 0.0168(10) Uani 1 1 d . . . . .
C62 C 0.7545(4) 0.9018(4) 0.4495(3) 0.0213(10) Uani 1 1 d . . . . .
H62 H 0.7695 0.9609 0.4495 0.026 Uiso 1 1 calc R . . . .
C63 C 0.7508(4) 0.8890(4) 0.3835(3) 0.0233(11) Uani 1 1 d . . . . .
H63 H 0.7657 0.9394 0.3400 0.028 Uiso 1 1 calc R . . . .
C64 C 0.7254(4) 0.8025(4) 0.3814(3) 0.0204(10) Uani 1 1 d . . . . .
C65 C 0.7050(4) 0.7280(4) 0.4487(3) 0.0194(10) Uani 1 1 d . . . . .
H65 H 0.6872 0.6696 0.4490 0.023 Uiso 1 1 calc R . . . .
C66 C 0.7107(4) 0.7393(3) 0.5142(3) 0.0169(9) Uani 1 1 d . . . . .
H66 H 0.6976 0.6886 0.5578 0.020 Uiso 1 1 calc R . . . .
C67 C 0.7196(5) 0.7896(4) 0.3101(3) 0.0290(12) Uani 1 1 d . . . . .
H67A H 0.6422 0.7901 0.3026 0.043 Uiso 1 1 calc GR . . . .
H67B H 0.7623 0.7286 0.3113 0.043 Uiso 1 1 calc GR . . . .
H67C H 0.7507 0.8417 0.2710 0.043 Uiso 1 1 calc GR . . . .
N1 N 0.7929(3) 0.7663(3) 0.6391(2) 0.0158(8) Uani 1 1 d . . . . .
P1 P 0.79763(11) 0.48664(9) 0.68062(7) 0.0197(3) Uani 1 1 d D . . . .
Th1 Th 0.85107(2) 0.63641(2) 0.73487(2) 0.01462(6) Uani 1 1 d . . . . .
C68 C 0.0377(8) 0.9686(7) 0.9802(6) 0.080(3) Uani 1 1 d . . . . .
H68A H 0.0594 0.9051 1.0163 0.096 Uiso 1 1 calc R . . . .
H68B H -0.0076 0.9595 0.9468 0.096 Uiso 1 1 calc R . . . .
C69 C 0.1444(9) 1.0074(8) 0.9379(6) 0.093(4) Uani 1 1 d . . . . .
H69A H 0.1941 1.0113 0.9713 0.111 Uiso 1 1 calc R . . . .
H69B H 0.1248 1.0726 0.9035 0.111 Uiso 1 1 calc R . . . .
C70 C 0.2070(10) 0.9430(9) 0.8968(8) 0.131(5) Uani 1 1 d . . . . .
H70A H 0.1618 0.9454 0.8596 0.196 Uiso 1 1 calc GR . . . .
H70B H 0.2209 0.8773 0.9301 0.196 Uiso 1 1 calc GR . . . .
H70C H 0.2778 0.9659 0.8749 0.196 Uiso 1 1 calc GR . . . .
H1 H 0.888(3) 0.456(6) 0.672(4) 0.08(3) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.442(6) . ?
C1 C5 1.429(6) . ?
C1 C6 1.550(7) . ?
C1 Th1 2.972(5) . ?
C2 C3 1.433(7) . ?
C2 C10 1.554(7) . ?
C2 Th1 2.956(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.408(7) . ?
C3 Th1 2.825(5) . ?
C4 C5 1.410(7) . ?
C4 C14 1.533(6) . ?
C4 Th1 2.884(5) . ?
C5 H5 0.9300 . ?
C5 Th1 2.887(5) . ?
C6 C7 1.530(6) . ?
C6 C8 1.536(7) . ?
C6 C9 1.539(6) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.536(7) . ?
C10 C12 1.544(7) . ?
C10 C13 1.552(7) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.530(7) . ?
C14 C16 1.543(7) . ?
C14 C17 1.532(7) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.435(7) . ?
C18 C22 1.441(7) . ?
C18 C23 1.544(7) . ?
C18 Th1 2.900(5) . ?
C19 C20 1.415(7) . ?
C19 C27 1.563(7) . ?
C19 Th1 2.952(5) . ?
C20 H20 0.9300 . ?
C20 C21 1.401(7) . ?
C20 Th1 2.845(5) . ?
C21 C22 1.416(7) . ?
C21 C31 1.521(7) . ?
C21 Th1 2.878(5) . ?
C22 H22 0.9300 . ?
C22 Th1 2.805(5) . ?
C23 C24 1.528(8) . ?
C23 C25 1.541(8) . ?
C23 C26 1.537(7) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.551(7) . ?
C27 C29 1.531(7) . ?
C27 C30 1.534(7) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32 1.531(7) . ?
C31 C33 1.506(8) . ?
C31 C34 1.532(8) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 C36 1.418(7) . ?
C35 C40 1.452(6) . ?
C35 P1 1.851(5) . ?
C36 C37 1.404(7) . ?
C36 C41 1.559(6) . ?
C37 H37 0.9300 . ?
C37 C38 1.378(7) . ?
C38 C39 1.394(7) . ?
C38 C45 1.538(7) . ?
C39 H39 0.9300 . ?
C39 C40 1.391(7) . ?
C40 C49 1.548(7) . ?
C41 C42 1.535(6) . ?
C41 C43 1.532(7) . ?
C41 C44 1.542(7) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 C46 1.537(7) . ?
C45 C47 1.543(7) . ?
C45 C48 1.533(7) . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 C50 1.550(7) . ?
C49 C51 1.533(7) . ?
C49 C52 1.544(7) . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C53 C54 1.506(6) . ?
C53 C61 1.506(7) . ?
C53 N1 1.268(6) . ?
C54 C55 1.381(7) . ?
C54 C59 1.403(7) . ?
C55 H55 0.9300 . ?
C55 C56 1.389(7) . ?
C56 H56 0.9300 . ?
C56 C57 1.397(7) . ?
C57 C58 1.388(7) . ?
C57 C60 1.508(7) . ?
C58 H58 0.9300 . ?
C58 C59 1.386(7) . ?
C59 H59 0.9300 . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
C61 C62 1.393(7) . ?
C61 C66 1.395(6) . ?
C62 H62 0.9300 . ?
C62 C63 1.398(7) . ?
C63 H63 0.9300 . ?
C63 C64 1.394(7) . ?
C64 C65 1.409(7) . ?
C64 C67 1.507(7) . ?
C65 H65 0.9300 . ?
C65 C66 1.382(7) . ?
C66 H66 0.9300 . ?
C67 H67A 0.9600 . ?
C67 H67B 0.9600 . ?
C67 H67C 0.9600 . ?
N1 Th1 2.239(4) . ?
P1 Th1 3.0047(13) . ?
P1 H1 1.12(2) . ?
C68 C68 1.544(19) 2_577 ?
C68 H68A 0.9700 . ?
C68 H68B 0.9700 . ?
C68 C69 1.515(14) . ?
C69 H69A 0.9700 . ?
C69 H69B 0.9700 . ?
C69 C70 1.526(16) . ?
C70 H70A 0.9600 . ?
C70 H70B 0.9600 . ?
C70 H70C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 132.8(4) . . ?
C2 C1 Th1 75.3(3) . . ?
C5 C1 C2 106.0(4) . . ?
C5 C1 C6 120.6(4) . . ?
C5 C1 Th1 72.6(3) . . ?
C6 C1 Th1 123.9(3) . . ?
C1 C2 C10 132.0(4) . . ?
C1 C2 Th1 76.5(3) . . ?
C3 C2 C1 106.2(4) . . ?
C3 C2 C10 119.3(4) . . ?
C3 C2 Th1 70.6(3) . . ?
C10 C2 Th1 131.1(3) . . ?
C2 C3 H3 124.5 . . ?
C2 C3 Th1 80.8(3) . . ?
C4 C3 C2 111.1(4) . . ?
C4 C3 H3 124.5 . . ?
C4 C3 Th1 78.1(3) . . ?
Th1 C3 H3 108.9 . . ?
C3 C4 C5 105.1(4) . . ?
C3 C4 C14 125.0(4) . . ?
C3 C4 Th1 73.4(3) . . ?
C5 C4 C14 125.0(4) . . ?
C5 C4 Th1 76.0(3) . . ?
C14 C4 Th1 135.2(3) . . ?
C1 C5 H5 124.3 . . ?
C1 C5 Th1 79.2(3) . . ?
C4 C5 C1 111.4(4) . . ?
C4 C5 H5 124.3 . . ?
C4 C5 Th1 75.7(3) . . ?
Th1 C5 H5 112.6 . . ?
C7 C6 C1 111.7(4) . . ?
C7 C6 C8 107.9(4) . . ?
C7 C6 C9 109.1(4) . . ?
C8 C6 C1 110.8(4) . . ?
C8 C6 C9 104.1(4) . . ?
C9 C6 C1 112.7(4) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 C2 116.0(4) . . ?
C11 C10 C12 110.9(4) . . ?
C11 C10 C13 107.0(4) . . ?
C12 C10 C2 107.4(4) . . ?
C12 C10 C13 105.7(4) . . ?
C13 C10 C2 109.4(4) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C4 C14 C16 105.7(4) . . ?
C15 C14 C4 112.3(4) . . ?
C15 C14 C16 108.0(4) . . ?
C15 C14 C17 109.0(4) . . ?
C17 C14 C4 113.6(4) . . ?
C17 C14 C16 108.0(4) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C22 105.6(4) . . ?
C19 C18 C23 132.9(5) . . ?
C19 C18 Th1 77.8(3) . . ?
C22 C18 C23 119.3(5) . . ?
C22 C18 Th1 71.7(3) . . ?
C23 C18 Th1 127.8(3) . . ?
C18 C19 C27 134.7(5) . . ?
C18 C19 Th1 73.8(3) . . ?
C20 C19 C18 107.1(4) . . ?
C20 C19 C27 115.7(4) . . ?
C20 C19 Th1 71.7(3) . . ?
C27 C19 Th1 132.8(3) . . ?
C19 C20 H20 124.4 . . ?
C19 C20 Th1 80.1(3) . . ?
C21 C20 C19 111.1(5) . . ?
C21 C20 H20 124.4 . . ?
C21 C20 Th1 77.1(3) . . ?
Th1 C20 H20 110.4 . . ?
C20 C21 C22 105.3(5) . . ?
C20 C21 C31 127.4(5) . . ?
C20 C21 Th1 74.5(3) . . ?
C22 C21 C31 125.9(5) . . ?
C22 C21 Th1 72.8(3) . . ?
C31 C21 Th1 128.0(3) . . ?
C18 C22 H22 124.8 . . ?
C18 C22 Th1 79.1(3) . . ?
C21 C22 C18 110.5(5) . . ?
C21 C22 H22 124.8 . . ?
C21 C22 Th1 78.4(3) . . ?
Th1 C22 H22 110.0 . . ?
C24 C23 C18 111.1(4) . . ?
C24 C23 C25 106.5(5) . . ?
C24 C23 C26 105.3(5) . . ?
C25 C23 C18 108.4(5) . . ?
C26 C23 C18 114.5(4) . . ?
C26 C23 C25 110.6(5) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C19 105.3(4) . . ?
C29 C27 C19 118.2(4) . . ?
C29 C27 C28 107.7(4) . . ?
C29 C27 C30 106.6(4) . . ?
C30 C27 C19 111.0(4) . . ?
C30 C27 C28 107.6(5) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C21 C31 C32 110.0(4) . . ?
C21 C31 C34 107.2(4) . . ?
C32 C31 C34 107.2(5) . . ?
C33 C31 C21 113.3(5) . . ?
C33 C31 C32 109.7(5) . . ?
C33 C31 C34 109.3(5) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 C40 116.7(4) . . ?
C36 C35 P1 119.1(4) . . ?
C40 C35 P1 124.2(4) . . ?
C35 C36 C41 124.0(4) . . ?
C37 C36 C35 118.5(4) . . ?
C37 C36 C41 117.5(4) . . ?
C36 C37 H37 118.3 . . ?
C38 C37 C36 123.5(5) . . ?
C38 C37 H37 118.3 . . ?
C37 C38 C39 115.8(5) . . ?
C37 C38 C45 124.1(5) . . ?
C39 C38 C45 119.8(4) . . ?
C38 C39 H39 118.1 . . ?
C40 C39 C38 123.8(5) . . ?
C40 C39 H39 118.1 . . ?
C35 C40 C49 125.3(4) . . ?
C39 C40 C35 117.6(4) . . ?
C39 C40 C49 117.0(4) . . ?
C42 C41 C36 111.2(4) . . ?
C42 C41 C44 107.3(4) . . ?
C43 C41 C36 111.2(4) . . ?
C43 C41 C42 110.9(4) . . ?
C43 C41 C44 104.8(4) . . ?
C44 C41 C36 111.2(4) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C38 C45 C47 108.5(4) . . ?
C46 C45 C38 111.2(4) . . ?
C46 C45 C47 108.5(5) . . ?
C48 C45 C38 110.5(4) . . ?
C48 C45 C46 108.6(5) . . ?
C48 C45 C47 109.4(4) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C40 C49 C50 111.9(4) . . ?
C51 C49 C40 113.8(4) . . ?
C51 C49 C50 105.5(4) . . ?
C51 C49 C52 111.2(4) . . ?
C52 C49 C40 109.2(4) . . ?
C52 C49 C50 105.0(4) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C49 C51 H51A 109.5 . . ?
C49 C51 H51B 109.5 . . ?
C49 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C49 C52 H52A 109.5 . . ?
C49 C52 H52B 109.5 . . ?
C49 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C61 C53 C54 114.5(4) . . ?
N1 C53 C54 123.7(4) . . ?
N1 C53 C61 121.8(4) . . ?
C55 C54 C53 122.5(4) . . ?
C55 C54 C59 118.0(4) . . ?
C59 C54 C53 119.3(4) . . ?
C54 C55 H55 119.4 . . ?
C54 C55 C56 121.2(5) . . ?
C56 C55 H55 119.4 . . ?
C55 C56 H56 119.5 . . ?
C55 C56 C57 121.0(5) . . ?
C57 C56 H56 119.5 . . ?
C56 C57 C60 120.5(5) . . ?
C58 C57 C56 117.8(5) . . ?
C58 C57 C60 121.8(5) . . ?
C57 C58 H58 119.3 . . ?
C59 C58 C57 121.3(5) . . ?
C59 C58 H58 119.3 . . ?
C54 C59 H59 119.7 . . ?
C58 C59 C54 120.7(5) . . ?
C58 C59 H59 119.7 . . ?
C57 C60 H60A 109.5 . . ?
C57 C60 H60B 109.5 . . ?
C57 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C62 C61 C53 119.9(4) . . ?
C62 C61 C66 118.9(5) . . ?
C66 C61 C53 121.0(4) . . ?
C61 C62 H62 119.8 . . ?
C61 C62 C63 120.4(5) . . ?
C63 C62 H62 119.8 . . ?
C62 C63 H63 119.3 . . ?
C64 C63 C62 121.4(5) . . ?
C64 C63 H63 119.3 . . ?
C63 C64 C65 117.2(5) . . ?
C63 C64 C67 121.3(5) . . ?
C65 C64 C67 121.5(5) . . ?
C64 C65 H65 119.1 . . ?
C66 C65 C64 121.7(5) . . ?
C66 C65 H65 119.1 . . ?
C61 C66 H66 119.8 . . ?
C65 C66 C61 120.4(4) . . ?
C65 C66 H66 119.8 . . ?
C64 C67 H67A 109.5 . . ?
C64 C67 H67B 109.5 . . ?
C64 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C53 N1 Th1 175.0(4) . . ?
C35 P1 Th1 136.72(16) . . ?
C35 P1 H1 104(4) . . ?
Th1 P1 H1 96(4) . . ?
C1 Th1 P1 84.10(9) . . ?
C2 Th1 C1 28.16(12) . . ?
C2 Th1 P1 111.94(9) . . ?
C3 Th1 C1 46.65(13) . . ?
C3 Th1 C2 28.59(13) . . ?
C3 Th1 C4 28.53(13) . . ?
C3 Th1 C5 46.09(14) . . ?
C3 Th1 C18 95.62(15) . . ?
C3 Th1 C19 122.60(14) . . ?
C3 Th1 C20 139.01(15) . . ?
C3 Th1 C21 117.31(14) . . ?
C3 Th1 P1 124.29(10) . . ?
C4 Th1 C1 47.19(13) . . ?
C4 Th1 C2 47.28(13) . . ?
C4 Th1 C5 28.28(14) . . ?
C4 Th1 C18 105.34(15) . . ?
C4 Th1 C19 133.11(14) . . ?
C4 Th1 P1 101.59(10) . . ?
C5 Th1 C1 28.19(13) . . ?
C5 Th1 C2 46.21(13) . . ?
C5 Th1 C18 133.55(14) . . ?
C5 Th1 C19 160.36(13) . . ?
C5 Th1 P1 78.28(10) . . ?
C18 Th1 C1 141.38(14) . . ?
C18 Th1 C2 114.61(14) . . ?
C18 Th1 C19 28.37(14) . . ?
C18 Th1 P1 133.09(11) . . ?
C19 Th1 C1 161.81(13) . . ?
C19 Th1 C2 134.56(13) . . ?
C19 Th1 P1 111.29(10) . . ?
C20 Th1 C1 169.93(14) . . ?
C20 Th1 C2 161.44(14) . . ?
C20 Th1 C4 131.83(15) . . ?
C20 Th1 C5 144.94(14) . . ?
C20 Th1 C18 47.02(14) . . ?
C20 Th1 C19 28.18(14) . . ?
C20 Th1 C21 28.33(14) . . ?
C20 Th1 P1 86.61(11) . . ?
C21 Th1 C1 147.12(14) . . ?
C21 Th1 C2 145.89(14) . . ?
C21 Th1 C4 103.75(15) . . ?
C21 Th1 C5 118.95(14) . . ?
C21 Th1 C18 47.92(14) . . ?
C21 Th1 C19 46.93(14) . . ?
C21 Th1 P1 88.81(11) . . ?
C22 Th1 C1 135.81(14) . . ?
C22 Th1 C2 120.02(14) . . ?
C22 Th1 C3 92.81(15) . . ?
C22 Th1 C4 89.10(15) . . ?
C22 Th1 C5 113.78(14) . . ?
C22 Th1 C18 29.19(14) . . ?
C22 Th1 C19 46.80(14) . . ?
C22 Th1 C20 46.68(15) . . ?
C22 Th1 C21 28.82(14) . . ?
C22 Th1 P1 116.28(11) . . ?
N1 Th1 C1 87.47(14) . . ?
N1 Th1 C2 80.67(14) . . ?
N1 Th1 C3 104.13(14) . . ?
N1 Th1 C4 127.94(15) . . ?
N1 Th1 C5 115.42(14) . . ?
N1 Th1 C18 96.47(15) . . ?
N1 Th1 C19 81.40(14) . . ?
N1 Th1 C20 97.42(15) . . ?
N1 Th1 C21 125.27(15) . . ?
N1 Th1 C22 125.07(15) . . ?
N1 Th1 P1 96.30(11) . . ?
C68 C68 H68A 108.1 2_577 . ?
C68 C68 H68B 108.1 2_577 . ?
H68A C68 H68B 107.3 . . ?
C69 C68 C68 116.8(12) . 2_577 ?
C69 C68 H68A 108.1 . . ?
C69 C68 H68B 108.1 . . ?
C68 C69 H69A 109.2 . . ?
C68 C69 H69B 109.2 . . ?
C68 C69 C70 111.9(10) . . ?
H69A C69 H69B 107.9 . . ?
C70 C69 H69A 109.2 . . ?
C70 C69 H69B 109.2 . . ?
C69 C70 H70A 109.5 . . ?
C69 C70 H70B 109.5 . . ?
C69 C70 H70C 109.5 . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 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
C1 C2 C3 C4 4.4(6) . . . . ?
C1 C2 C3 Th1 -69.0(3) . . . . ?
C1 C2 C10 C11 50.6(7) . . . . ?
C1 C2 C10 C12 -74.1(6) . . . . ?
C1 C2 C10 C13 171.7(5) . . . . ?
C2 C1 C5 C4 -1.4(5) . . . . ?
C2 C1 C5 Th1 68.5(3) . . . . ?
C2 C1 C6 C7 -73.5(6) . . . . ?
C2 C1 C6 C8 166.1(5) . . . . ?
C2 C1 C6 C9 49.9(7) . . . . ?
C2 C3 C4 C5 -5.1(6) . . . . ?
C2 C3 C4 C14 150.9(5) . . . . ?
C2 C3 C4 Th1 -75.1(4) . . . . ?
C3 C2 C10 C11 -150.2(5) . . . . ?
C3 C2 C10 C12 85.2(5) . . . . ?
C3 C2 C10 C13 -29.1(6) . . . . ?
C3 C4 C5 C1 4.0(6) . . . . ?
C3 C4 C5 Th1 -68.2(3) . . . . ?
C3 C4 C14 C15 -178.3(5) . . . . ?
C3 C4 C14 C16 -60.7(6) . . . . ?
C3 C4 C14 C17 57.5(7) . . . . ?
C5 C1 C2 C3 -1.7(5) . . . . ?
C5 C1 C2 C10 159.5(5) . . . . ?
C5 C1 C2 Th1 -66.6(3) . . . . ?
C5 C1 C6 C7 117.1(5) . . . . ?
C5 C1 C6 C8 -3.3(6) . . . . ?
C5 C1 C6 C9 -119.5(5) . . . . ?
C5 C4 C14 C15 -26.9(7) . . . . ?
C5 C4 C14 C16 90.6(6) . . . . ?
C5 C4 C14 C17 -151.1(5) . . . . ?
C6 C1 C2 C3 -172.3(5) . . . . ?
C6 C1 C2 C10 -11.1(9) . . . . ?
C6 C1 C2 Th1 122.9(5) . . . . ?
C6 C1 C5 C4 170.5(4) . . . . ?
C6 C1 C5 Th1 -119.6(4) . . . . ?
C10 C2 C3 C4 -159.7(4) . . . . ?
C10 C2 C3 Th1 127.0(4) . . . . ?
C14 C4 C5 C1 -152.0(5) . . . . ?
C14 C4 C5 Th1 135.8(5) . . . . ?
C18 C19 C20 C21 6.1(6) . . . . ?
C18 C19 C20 Th1 -65.9(3) . . . . ?
C18 C19 C27 C28 -91.4(7) . . . . ?
C18 C19 C27 C29 28.9(8) . . . . ?
C18 C19 C27 C30 152.4(6) . . . . ?
C19 C18 C22 C21 -2.0(6) . . . . ?
C19 C18 C22 Th1 71.2(3) . . . . ?
C19 C18 C23 C24 -178.1(5) . . . . ?
C19 C18 C23 C25 65.1(7) . . . . ?
C19 C18 C23 C26 -58.9(8) . . . . ?
C19 C20 C21 C22 -7.2(6) . . . . ?
C19 C20 C21 C31 159.8(5) . . . . ?
C19 C20 C21 Th1 -73.9(4) . . . . ?
C20 C19 C27 C28 67.9(6) . . . . ?
C20 C19 C27 C29 -171.9(5) . . . . ?
C20 C19 C27 C30 -48.3(6) . . . . ?
C20 C21 C22 C18 5.5(6) . . . . ?
C20 C21 C22 Th1 -68.0(3) . . . . ?
C20 C21 C31 C32 6.0(8) . . . . ?
C20 C21 C31 C33 129.2(6) . . . . ?
C20 C21 C31 C34 -110.2(6) . . . . ?
C22 C18 C19 C20 -2.4(5) . . . . ?
C22 C18 C19 C27 158.1(5) . . . . ?
C22 C18 C19 Th1 -66.9(3) . . . . ?
C22 C18 C23 C24 21.6(7) . . . . ?
C22 C18 C23 C25 -95.1(6) . . . . ?
C22 C18 C23 C26 140.8(5) . . . . ?
C22 C21 C31 C32 170.4(5) . . . . ?
C22 C21 C31 C33 -66.4(7) . . . . ?
C22 C21 C31 C34 54.2(7) . . . . ?
C23 C18 C19 C20 -164.6(5) . . . . ?
C23 C18 C19 C27 -4.1(10) . . . . ?
C23 C18 C19 Th1 130.9(6) . . . . ?
C23 C18 C22 C21 163.1(5) . . . . ?
C23 C18 C22 Th1 -123.7(4) . . . . ?
C27 C19 C20 C21 -158.6(4) . . . . ?
C27 C19 C20 Th1 129.4(4) . . . . ?
C31 C21 C22 C18 -161.7(5) . . . . ?
C31 C21 C22 Th1 124.8(5) . . . . ?
C35 C36 C37 C38 -5.5(7) . . . . ?
C35 C36 C41 C42 -78.4(6) . . . . ?
C35 C36 C41 C43 45.8(6) . . . . ?
C35 C36 C41 C44 162.2(5) . . . . ?
C35 C40 C49 C50 -161.7(5) . . . . ?
C35 C40 C49 C51 78.9(6) . . . . ?
C35 C40 C49 C52 -45.9(6) . . . . ?
C36 C35 C40 C39 -20.8(7) . . . . ?
C36 C35 C40 C49 154.5(5) . . . . ?
C36 C35 P1 Th1 87.6(4) . . . . ?
C36 C37 C38 C39 -9.9(7) . . . . ?
C36 C37 C38 C45 175.0(5) . . . . ?
C37 C36 C41 C42 103.8(5) . . . . ?
C37 C36 C41 C43 -132.1(5) . . . . ?
C37 C36 C41 C44 -15.7(6) . . . . ?
C37 C38 C39 C40 9.7(7) . . . . ?
C37 C38 C45 C46 -12.3(7) . . . . ?
C37 C38 C45 C47 107.0(6) . . . . ?
C37 C38 C45 C48 -133.1(5) . . . . ?
C38 C39 C40 C35 5.6(7) . . . . ?
C38 C39 C40 C49 -170.0(5) . . . . ?
C39 C38 C45 C46 172.7(5) . . . . ?
C39 C38 C45 C47 -68.0(6) . . . . ?
C39 C38 C45 C48 52.0(7) . . . . ?
C39 C40 C49 C50 13.6(6) . . . . ?
C39 C40 C49 C51 -105.8(5) . . . . ?
C39 C40 C49 C52 129.4(5) . . . . ?
C40 C35 C36 C37 20.7(7) . . . . ?
C40 C35 C36 C41 -157.1(4) . . . . ?
C40 C35 P1 Th1 -89.6(4) . . . . ?
C41 C36 C37 C38 172.5(4) . . . . ?
C45 C38 C39 C40 -175.0(5) . . . . ?
C53 C54 C55 C56 -175.9(5) . . . . ?
C53 C54 C59 C58 174.4(5) . . . . ?
C53 C61 C62 C63 173.8(5) . . . . ?
C53 C61 C66 C65 -175.0(4) . . . . ?
C54 C53 C61 C62 35.4(6) . . . . ?
C54 C53 C61 C66 -149.3(4) . . . . ?
C54 C55 C56 C57 1.5(8) . . . . ?
C55 C54 C59 C58 -1.8(8) . . . . ?
C55 C56 C57 C58 -1.5(8) . . . . ?
C55 C56 C57 C60 178.1(5) . . . . ?
C56 C57 C58 C59 -0.2(8) . . . . ?
C57 C58 C59 C54 1.9(8) . . . . ?
C59 C54 C55 C56 0.2(8) . . . . ?
C60 C57 C58 C59 -179.8(5) . . . . ?
C61 C53 C54 C55 -137.2(5) . . . . ?
C61 C53 C54 C59 46.8(6) . . . . ?
C61 C62 C63 C64 1.9(8) . . . . ?
C62 C61 C66 C65 0.3(7) . . . . ?
C62 C63 C64 C65 -0.8(7) . . . . ?
C62 C63 C64 C67 179.0(5) . . . . ?
C63 C64 C65 C66 -0.5(7) . . . . ?
C64 C65 C66 C61 0.7(7) . . . . ?
C66 C61 C62 C63 -1.6(7) . . . . ?
C67 C64 C65 C66 179.7(5) . . . . ?
N1 C53 C54 C55 41.0(7) . . . . ?
N1 C53 C54 C59 -135.0(5) . . . . ?
N1 C53 C61 C62 -142.9(5) . . . . ?
N1 C53 C61 C66 32.4(7) . . . . ?
P1 C35 C36 C37 -156.7(4) . . . . ?
P1 C35 C36 C41 25.5(6) . . . . ?
P1 C35 C40 C39 156.5(4) . . . . ?
P1 C35 C40 C49 -28.3(7) . . . . ?
Th1 C1 C2 C3 64.9(3) . . . . ?
Th1 C1 C2 C10 -133.9(5) . . . . ?
Th1 C1 C5 C4 -69.9(4) . . . . ?
Th1 C1 C6 C7 28.4(5) . . . . ?
Th1 C1 C6 C8 -92.0(4) . . . . ?
Th1 C1 C6 C9 151.7(3) . . . . ?
Th1 C2 C3 C4 73.3(4) . . . . ?
Th1 C2 C10 C11 -61.1(6) . . . . ?
Th1 C2 C10 C12 174.3(3) . . . . ?
Th1 C2 C10 C13 60.0(5) . . . . ?
Th1 C3 C4 C5 70.0(3) . . . . ?
Th1 C3 C4 C14 -134.0(5) . . . . ?
Th1 C4 C5 C1 72.1(3) . . . . ?
Th1 C4 C14 C15 79.6(6) . . . . ?
Th1 C4 C14 C16 -162.9(4) . . . . ?
Th1 C4 C14 C17 -44.6(7) . . . . ?
Th1 C18 C19 C20 64.5(3) . . . . ?
Th1 C18 C19 C27 -135.0(6) . . . . ?
Th1 C18 C22 C21 -73.1(4) . . . . ?
Th1 C18 C23 C24 -67.3(6) . . . . ?
Th1 C18 C23 C25 176.0(4) . . . . ?
Th1 C18 C23 C26 51.9(6) . . . . ?
Th1 C19 C20 C21 72.0(4) . . . . ?
Th1 C19 C27 C28 156.3(4) . . . . ?
Th1 C19 C27 C29 -83.5(6) . . . . ?
Th1 C19 C27 C30 40.0(6) . . . . ?
Th1 C20 C21 C22 66.8(3) . . . . ?
Th1 C20 C21 C31 -126.3(5) . . . . ?
Th1 C21 C22 C18 73.6(4) . . . . ?
Th1 C21 C31 C32 -93.8(5) . . . . ?
Th1 C21 C31 C33 29.4(7) . . . . ?
Th1 C21 C31 C34 150.0(4) . . . . ?
C68 C68 C69 C70 -175.7(11) 2_577 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.469
_oxdiff_exptl_absorpt_empirical_full_min 0.678
####################################################################### 
# 
# 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_compound9
_database_code_depnum_ccdc_archive 'CCDC 1883602'
_audit_update_record             
;
2018-12-06 deposited with the CCDC.
2019-01-23 downloaded from the CCDC.
;
_audit_creation_date             2018-05-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C37 H65 O P Th'
_chemical_formula_sum            'C37 H65 O P Th'
_chemical_formula_weight         788.90
_chemical_melting_point          ?
_chemical_oxdiff_formula         C1H1O1P1Th1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Th Th -4.1491 12.3296 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   12.2839(3)
_cell_length_b                   18.1136(5)
_cell_length_c                   16.7491(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.286(2)
_cell_angle_gamma                90
_cell_volume                     3723.81(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10469
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.2310
_cell_measurement_theta_min      3.6270
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.487
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0718
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24887
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.988
_diffrn_reflns_theta_min         3.596
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00 -13.00   1.00    1.00    --  -39.24 -57.00 -60.00   97
  2  ω    -65.00  34.00   1.00    1.00    --  -39.24  57.00  90.00   99
  3  ω    -62.00 -34.00   1.00    1.00    --  -39.24 178.00  90.00   28
  4  ω     17.00 113.00   1.00    1.00    --   39.24  37.00-120.00   96
  5  ω     60.00  97.00   1.00    1.00    --   39.24 178.00 -90.00   37
  6  ω     47.00  74.00   1.00    1.00    --   39.24 -99.00  90.00   27
  7  ω     71.00 128.00   1.00    1.00    --   39.24 178.00 -30.00   57
  8  ω     40.00 137.00   1.00    1.00    --  108.44 -30.00-150.00   97
  9  ω     75.00 119.00   1.00    1.00    --  108.44-125.00 -90.00   44
 10  ω     37.00  79.00   1.00    1.00    --  108.44 -30.00   0.00   42
 11  ω     36.00  64.00   1.00    1.00    --  108.44-125.00 -90.00   28
 12  ω     85.00 177.00   1.00    1.00    --  108.44  45.00  30.00   92
 13  ω     30.00 160.00   1.00    1.00    --  108.44 -15.00  30.00  130
 14  ω     80.00 121.00   1.00    1.00    --  108.44-125.00 120.00   41
 15  ω     82.00 109.00   1.00    1.00    --  108.44 -94.00 -30.00   27
 16  ω     37.00 138.00   1.00    1.00    --  108.44 -61.00  90.00  101
 17  ω    127.00 178.00   1.00    1.00    --  108.44 125.00 -60.00   51
 18  ω     43.00 115.00   1.00    1.00    --  108.44 -61.00   0.00   72
 19  ω     38.00 141.00   1.00    1.00    --  108.44 -77.00-120.00  103
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1031052000
_diffrn_orient_matrix_UB_12      0.0294571000
_diffrn_orient_matrix_UB_13      0.0384110000
_diffrn_orient_matrix_UB_21      -0.0173638000
_diffrn_orient_matrix_UB_22      -0.0757725000
_diffrn_orient_matrix_UB_23      0.0394659000
_diffrn_orient_matrix_UB_31      0.0692429000
_diffrn_orient_matrix_UB_32      0.0249727000
_diffrn_orient_matrix_UB_33      0.0738670000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6176
_reflns_number_total             7437
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         6.457
_refine_diff_density_min         -3.423
_refine_diff_density_rms         0.261
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         7437
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0612
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0801P)²+60.5077P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1534
_refine_ls_wR_factor_ref         0.1686
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C37(H37A,H37B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C20(H20), C22(H22)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Th1 Th 0.73240(2) 0.46558(2) 0.26571(2) 0.01751(13) Uani 1 1 d . . . . .
P1 P 0.84113(19) 0.42673(14) 0.43703(15) 0.0236(5) Uani 1 1 d . . . . .
O1 O 0.8695(5) 0.4847(4) 0.3733(4) 0.0241(14) Uani 1 1 d . . . . .
C1 C 0.7807(8) 0.3219(5) 0.1883(6) 0.0222(19) Uani 1 1 d . . . . .
C2 C 0.7430(7) 0.3681(5) 0.1238(5) 0.0198(18) Uani 1 1 d . . . . .
C3 C 0.8204(7) 0.4263(5) 0.1193(5) 0.0175(17) Uani 1 1 d . . . . .
H3 H 0.8148 0.4656 0.0836 0.021 Uiso 1 1 calc R . . . .
C4 C 0.9076(7) 0.4163(5) 0.1769(6) 0.0224(19) Uani 1 1 d . . . . .
C5 C 0.8798(7) 0.3535(5) 0.2215(6) 0.0193(18) Uani 1 1 d . . . . .
H5 H 0.9196 0.3353 0.2656 0.023 Uiso 1 1 calc R . . . .
C6 C 0.7460(8) 0.2449(5) 0.2163(6) 0.0219(19) Uani 1 1 d . . . . .
C7 C 0.8190(8) 0.2172(6) 0.2874(7) 0.033(2) Uani 1 1 d . . . . .
H7A H 0.8913 0.2086 0.2699 0.050 Uiso 1 1 calc GR . . . .
H7B H 0.7896 0.1721 0.3075 0.050 Uiso 1 1 calc GR . . . .
H7C H 0.8212 0.2537 0.3289 0.050 Uiso 1 1 calc GR . . . .
C8 C 0.6283(8) 0.2388(6) 0.2462(6) 0.029(2) Uani 1 1 d . . . . .
H8A H 0.6244 0.2629 0.2971 0.043 Uiso 1 1 calc GR . . . .
H8B H 0.6092 0.1877 0.2516 0.043 Uiso 1 1 calc GR . . . .
H8C H 0.5785 0.2621 0.2084 0.043 Uiso 1 1 calc GR . . . .
C9 C 0.7646(9) 0.1881(5) 0.1499(7) 0.035(3) Uani 1 1 d . . . . .
H9A H 0.7178 0.1993 0.1042 0.052 Uiso 1 1 calc GR . . . .
H9B H 0.7482 0.1395 0.1690 0.052 Uiso 1 1 calc GR . . . .
H9C H 0.8392 0.1900 0.1351 0.052 Uiso 1 1 calc GR . . . .
C10 C 0.6602(8) 0.3593(6) 0.0527(6) 0.026(2) Uani 1 1 d . . . . .
C11 C 0.5615(9) 0.3079(6) 0.0652(7) 0.035(2) Uani 1 1 d . . . . .
H11A H 0.5871 0.2601 0.0820 0.052 Uiso 1 1 calc GR . . . .
H11B H 0.5194 0.3034 0.0160 0.052 Uiso 1 1 calc GR . . . .
H11C H 0.5170 0.3284 0.1054 0.052 Uiso 1 1 calc GR . . . .
C12 C 0.7234(10) 0.3276(6) -0.0167(7) 0.036(2) Uani 1 1 d . . . . .
H12A H 0.7822 0.3603 -0.0284 0.054 Uiso 1 1 calc GR . . . .
H12B H 0.6754 0.3228 -0.0630 0.054 Uiso 1 1 calc GR . . . .
H12C H 0.7522 0.2800 -0.0019 0.054 Uiso 1 1 calc GR . . . .
C13 C 0.6116(9) 0.4342(6) 0.0261(7) 0.035(3) Uani 1 1 d . . . . .
H13A H 0.5694 0.4542 0.0681 0.053 Uiso 1 1 calc GR . . . .
H13B H 0.5656 0.4275 -0.0210 0.053 Uiso 1 1 calc GR . . . .
H13C H 0.6694 0.4678 0.0147 0.053 Uiso 1 1 calc GR . . . .
C14 C 1.0152(8) 0.4585(6) 0.1820(6) 0.025(2) Uani 1 1 d . . . . .
C15 C 1.0770(9) 0.4342(8) 0.1077(7) 0.043(3) Uani 1 1 d . . . . .
H15A H 1.0830 0.3814 0.1070 0.064 Uiso 1 1 calc GR . . . .
H15B H 1.1485 0.4556 0.1098 0.064 Uiso 1 1 calc GR . . . .
H15C H 1.0379 0.4505 0.0602 0.064 Uiso 1 1 calc GR . . . .
C16 C 0.9964(10) 0.5412(6) 0.1791(10) 0.048(4) Uani 1 1 d . . . . .
H16A H 0.9522 0.5534 0.1324 0.072 Uiso 1 1 calc GR . . . .
H16B H 1.0651 0.5662 0.1772 0.072 Uiso 1 1 calc GR . . . .
H16C H 0.9598 0.5564 0.2260 0.072 Uiso 1 1 calc GR . . . .
C17 C 1.0829(8) 0.4372(7) 0.2564(7) 0.037(3) Uani 1 1 d . . . . .
H17A H 1.0440 0.4498 0.3031 0.056 Uiso 1 1 calc GR . . . .
H17B H 1.1509 0.4633 0.2572 0.056 Uiso 1 1 calc GR . . . .
H17C H 1.0965 0.3850 0.2559 0.056 Uiso 1 1 calc GR . . . .
C18 C 0.6858(7) 0.6245(5) 0.2154(5) 0.0178(17) Uani 1 1 d . U . . .
C19 C 0.6988(7) 0.6277(5) 0.3023(5) 0.0186(17) Uani 1 1 d . U . . .
C20 C 0.6173(7) 0.5794(5) 0.3336(6) 0.0227(19) Uani 1 1 d . . . . .
H20 H 0.6097 0.5691 0.3875 0.027 Uiso 1 1 calc R . . . .
C21 C 0.5513(7) 0.5503(5) 0.2711(6) 0.0222(19) Uani 1 1 d . . . . .
C22 C 0.5956(7) 0.5750(5) 0.1991(6) 0.0210(18) Uani 1 1 d . . . . .
H22 H 0.5700 0.5612 0.1482 0.025 Uiso 1 1 calc R . . . .
C23 C 0.7217(8) 0.6750(6) 0.1497(6) 0.027(2) Uani 1 1 d . . . . .
C24 C 0.7223(8) 0.6323(6) 0.0691(6) 0.028(2) Uani 1 1 d . . . . .
H24A H 0.7739 0.5926 0.0735 0.043 Uiso 1 1 calc GR . . . .
H24B H 0.7423 0.6652 0.0273 0.043 Uiso 1 1 calc GR . . . .
H24C H 0.6510 0.6126 0.0569 0.043 Uiso 1 1 calc GR . . . .
C25 C 0.8324(8) 0.7113(6) 0.1575(6) 0.027(2) Uani 1 1 d . . . . .
H25A H 0.8344 0.7444 0.2022 0.041 Uiso 1 1 calc GR . . . .
H25B H 0.8458 0.7383 0.1096 0.041 Uiso 1 1 calc GR . . . .
H25C H 0.8874 0.6741 0.1656 0.041 Uiso 1 1 calc GR . . . .
C26 C 0.6330(9) 0.7353(6) 0.1390(7) 0.033(2) Uani 1 1 d . . . . .
H26A H 0.5635 0.7124 0.1281 0.050 Uiso 1 1 calc GR . . . .
H26B H 0.6502 0.7669 0.0953 0.050 Uiso 1 1 calc GR . . . .
H26C H 0.6303 0.7640 0.1871 0.050 Uiso 1 1 calc GR . . . .
C27 C 0.7670(8) 0.6760(5) 0.3581(6) 0.0234(19) Uani 1 1 d . . . . .
C28 C 0.8910(8) 0.6709(6) 0.3487(7) 0.032(2) Uani 1 1 d . . . . .
H28A H 0.9155 0.6220 0.3623 0.049 Uiso 1 1 calc GR . . . .
H28B H 0.9271 0.7059 0.3837 0.049 Uiso 1 1 calc GR . . . .
H28C H 0.9077 0.6815 0.2944 0.049 Uiso 1 1 calc GR . . . .
C29 C 0.7288(9) 0.7575(6) 0.3477(7) 0.033(2) Uani 1 1 d . . . . .
H29A H 0.7474 0.7750 0.2959 0.049 Uiso 1 1 calc GR . . . .
H29B H 0.7641 0.7876 0.3881 0.049 Uiso 1 1 calc GR . . . .
H29C H 0.6513 0.7602 0.3525 0.049 Uiso 1 1 calc GR . . . .
C30 C 0.7486(10) 0.6574(6) 0.4461(7) 0.037(3) Uani 1 1 d . . . . .
H30A H 0.6735 0.6658 0.4574 0.055 Uiso 1 1 calc GR . . . .
H30B H 0.7941 0.6884 0.4799 0.055 Uiso 1 1 calc GR . . . .
H30C H 0.7666 0.6066 0.4560 0.055 Uiso 1 1 calc GR . . . .
C31 C 0.4706(7) 0.4866(6) 0.2741(7) 0.029(2) Uani 1 1 d . . . . .
C32 C 0.4217(9) 0.4824(7) 0.3580(8) 0.039(3) Uani 1 1 d . . . . .
H32A H 0.4784 0.4711 0.3972 0.058 Uiso 1 1 calc GR . . . .
H32B H 0.3671 0.4445 0.3581 0.058 Uiso 1 1 calc GR . . . .
H32C H 0.3893 0.5290 0.3705 0.058 Uiso 1 1 calc GR . . . .
C33 C 0.3764(8) 0.4949(7) 0.2119(8) 0.041(3) Uani 1 1 d . . . . .
H33A H 0.3384 0.5403 0.2212 0.061 Uiso 1 1 calc GR . . . .
H33B H 0.3271 0.4542 0.2163 0.061 Uiso 1 1 calc GR . . . .
H33C H 0.4047 0.4957 0.1593 0.061 Uiso 1 1 calc GR . . . .
C34 C 0.5402(8) 0.4177(6) 0.2576(7) 0.029(2) Uani 1 1 d . . . . .
H34A H 0.5222 0.3976 0.2051 0.035 Uiso 1 1 calc R . . . .
H34B H 0.5296 0.3798 0.2975 0.035 Uiso 1 1 calc R . . . .
C35 C 0.8450(10) 0.4698(6) 0.5340(6) 0.032(2) Uani 1 1 d . . . . .
H35A H 0.9162 0.4900 0.5452 0.048 Uiso 1 1 calc GR . . . .
H35B H 0.8291 0.4336 0.5739 0.048 Uiso 1 1 calc GR . . . .
H35C H 0.7918 0.5085 0.5347 0.048 Uiso 1 1 calc GR . . . .
C36 C 0.9454(8) 0.3558(6) 0.4462(7) 0.031(2) Uani 1 1 d . . . . .
H36A H 0.9469 0.3282 0.3973 0.047 Uiso 1 1 calc GR . . . .
H36B H 0.9294 0.3232 0.4893 0.047 Uiso 1 1 calc GR . . . .
H36C H 1.0151 0.3785 0.4568 0.047 Uiso 1 1 calc GR . . . .
C37 C 0.7175(8) 0.3916(6) 0.4043(6) 0.028(2) Uani 1 1 d . . . . .
H37A H 0.6572 0.4075 0.4358 0.034 Uiso 1 1 calc R . . . .
H37B H 0.7173 0.3384 0.3979 0.034 Uiso 1 1 calc R . . . .


_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
Th1 O1 2.442(6) . ?
Th1 C1 2.978(9) . ?
Th1 C2 2.967(9) . ?
Th1 C3 2.811(9) . ?
Th1 C4 2.811(9) . ?
Th1 C5 2.839(9) . ?
Th1 C19 3.031(9) . ?
Th1 C20 2.770(9) . ?
Th1 C21 2.707(9) . ?
Th1 C22 2.801(9) . ?
Th1 C34 2.514(10) . ?
Th1 C37 2.692(10) . ?
P1 O1 1.548(7) . ?
P1 C35 1.801(11) . ?
P1 C36 1.816(10) . ?
P1 C37 1.717(10) . ?
C1 C2 1.430(13) . ?
C1 C5 1.437(12) . ?
C1 C6 1.535(13) . ?
C2 C3 1.424(13) . ?
C2 C10 1.543(12) . ?
C3 H3 0.9300 . ?
C3 C4 1.424(13) . ?
C4 C5 1.411(13) . ?
C4 C14 1.526(13) . ?
C5 H5 0.9300 . ?
C6 C7 1.545(14) . ?
C6 C8 1.553(12) . ?
C6 C9 1.539(13) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.549(14) . ?
C10 C12 1.534(15) . ?
C10 C13 1.542(14) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.547(15) . ?
C14 C16 1.516(14) . ?
C14 C17 1.520(15) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.458(12) . ?
C18 C22 1.443(12) . ?
C18 C23 1.511(14) . ?
C19 C20 1.443(12) . ?
C19 C27 1.510(13) . ?
C20 H20 0.9300 . ?
C20 C21 1.401(14) . ?
C21 C22 1.416(13) . ?
C21 C31 1.523(13) . ?
C22 H22 0.9300 . ?
C23 C24 1.556(14) . ?
C23 C25 1.512(13) . ?
C23 C26 1.547(14) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.540(13) . ?
C27 C29 1.557(14) . ?
C27 C30 1.539(15) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32 1.551(16) . ?
C31 C33 1.533(14) . ?
C31 C34 1.543(14) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Th1 C1 107.6(2) . . ?
O1 Th1 C2 128.6(2) . . ?
O1 Th1 C3 113.7(2) . . ?
O1 Th1 C4 85.1(3) . . ?
O1 Th1 C5 82.3(2) . . ?
O1 Th1 C19 79.0(2) . . ?
O1 Th1 C20 86.6(3) . . ?
O1 Th1 C21 116.0(3) . . ?
O1 Th1 C22 125.4(2) . . ?
O1 Th1 C34 135.0(3) . . ?
O1 Th1 C37 60.2(3) . . ?
C1 Th1 C19 165.0(3) . . ?
C2 Th1 C1 27.8(3) . . ?
C2 Th1 C19 138.5(2) . . ?
C3 Th1 C1 46.3(3) . . ?
C3 Th1 C2 28.4(2) . . ?
C3 Th1 C4 29.4(3) . . ?
C3 Th1 C5 47.1(3) . . ?
C3 Th1 C19 118.8(2) . . ?
C4 Th1 C1 47.3(3) . . ?
C4 Th1 C2 47.8(3) . . ?
C4 Th1 C5 28.9(3) . . ?
C4 Th1 C19 121.9(3) . . ?
C5 Th1 C1 28.5(2) . . ?
C5 Th1 C2 46.9(2) . . ?
C5 Th1 C19 147.1(2) . . ?
C20 Th1 C1 160.6(3) . . ?
C20 Th1 C2 144.2(3) . . ?
C20 Th1 C3 140.1(3) . . ?
C20 Th1 C4 150.2(3) . . ?
C20 Th1 C5 168.8(3) . . ?
C20 Th1 C19 28.4(2) . . ?
C20 Th1 C22 47.8(3) . . ?
C21 Th1 C1 133.5(3) . . ?
C21 Th1 C2 115.2(3) . . ?
C21 Th1 C3 121.2(3) . . ?
C21 Th1 C4 147.7(3) . . ?
C21 Th1 C5 161.4(3) . . ?
C21 Th1 C19 47.6(3) . . ?
C21 Th1 C20 29.6(3) . . ?
C21 Th1 C22 29.7(3) . . ?
C22 Th1 C1 124.9(3) . . ?
C22 Th1 C2 98.4(3) . . ?
C22 Th1 C3 94.4(3) . . ?
C22 Th1 C4 118.3(3) . . ?
C22 Th1 C5 141.3(3) . . ?
C22 Th1 C19 46.4(2) . . ?
C34 Th1 C1 83.0(3) . . ?
C34 Th1 C2 79.8(3) . . ?
C34 Th1 C3 105.0(3) . . ?
C34 Th1 C4 126.8(3) . . ?
C34 Th1 C5 110.3(3) . . ?
C34 Th1 C19 102.1(3) . . ?
C34 Th1 C20 77.6(3) . . ?
C34 Th1 C21 55.0(3) . . ?
C34 Th1 C22 71.0(3) . . ?
C34 Th1 C37 77.2(3) . . ?
C37 Th1 C1 87.8(3) . . ?
C37 Th1 C2 113.6(3) . . ?
C37 Th1 C3 131.9(3) . . ?
C37 Th1 C4 112.2(3) . . ?
C37 Th1 C5 86.3(3) . . ?
C37 Th1 C19 107.1(3) . . ?
C37 Th1 C20 87.9(3) . . ?
C37 Th1 C21 99.7(3) . . ?
C37 Th1 C22 129.4(3) . . ?
O1 P1 Th1 47.8(2) . . ?
O1 P1 C35 109.3(4) . . ?
O1 P1 C36 111.1(5) . . ?
O1 P1 C37 104.6(4) . . ?
C35 P1 Th1 135.2(4) . . ?
C35 P1 C36 103.7(5) . . ?
C36 P1 Th1 120.0(4) . . ?
C37 P1 Th1 57.4(4) . . ?
C37 P1 C35 116.1(5) . . ?
C37 P1 C36 112.1(5) . . ?
P1 O1 Th1 104.2(3) . . ?
C2 C1 Th1 75.7(5) . . ?
C2 C1 C5 107.6(8) . . ?
C2 C1 C6 132.6(9) . . ?
C5 C1 Th1 70.4(5) . . ?
C5 C1 C6 119.0(8) . . ?
C6 C1 Th1 126.7(6) . . ?
C1 C2 Th1 76.5(5) . . ?
C1 C2 C10 134.9(9) . . ?
C3 C2 Th1 69.7(5) . . ?
C3 C2 C1 106.1(7) . . ?
C3 C2 C10 117.2(8) . . ?
C10 C2 Th1 129.2(6) . . ?
Th1 C3 H3 110.3 . . ?
C2 C3 Th1 81.9(5) . . ?
C2 C3 H3 124.6 . . ?
C2 C3 C4 110.8(8) . . ?
C4 C3 Th1 75.3(5) . . ?
C4 C3 H3 124.6 . . ?
C3 C4 Th1 75.3(5) . . ?
C3 C4 C14 126.9(9) . . ?
C5 C4 Th1 76.7(5) . . ?
C5 C4 C3 105.7(8) . . ?
C5 C4 C14 127.0(8) . . ?
C14 C4 Th1 119.4(6) . . ?
Th1 C5 H5 111.5 . . ?
C1 C5 Th1 81.1(5) . . ?
C1 C5 H5 125.2 . . ?
C4 C5 Th1 74.4(5) . . ?
C4 C5 C1 109.6(8) . . ?
C4 C5 H5 125.2 . . ?
C1 C6 C7 111.8(8) . . ?
C1 C6 C8 115.8(8) . . ?
C1 C6 C9 109.6(8) . . ?
C7 C6 C8 104.3(8) . . ?
C9 C6 C7 104.0(8) . . ?
C9 C6 C8 110.6(8) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C2 C10 C11 116.9(9) . . ?
C12 C10 C2 106.6(8) . . ?
C12 C10 C11 107.5(9) . . ?
C12 C10 C13 108.2(9) . . ?
C13 C10 C2 111.6(8) . . ?
C13 C10 C11 105.8(8) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C4 C14 C15 105.3(9) . . ?
C16 C14 C4 111.3(8) . . ?
C16 C14 C15 109.6(10) . . ?
C16 C14 C17 110.8(10) . . ?
C17 C14 C4 111.3(9) . . ?
C17 C14 C15 108.5(9) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 Th1 75.5(5) . . ?
C19 C18 C23 132.8(8) . . ?
C22 C18 Th1 66.4(5) . . ?
C22 C18 C19 105.4(7) . . ?
C22 C18 C23 118.8(8) . . ?
C23 C18 Th1 135.8(6) . . ?
C18 C19 Th1 76.7(5) . . ?
C18 C19 C27 132.6(8) . . ?
C20 C19 Th1 65.7(5) . . ?
C20 C19 C18 106.8(8) . . ?
C20 C19 C27 120.1(8) . . ?
C27 C19 Th1 127.6(6) . . ?
Th1 C20 H20 108.8 . . ?
C19 C20 Th1 85.9(5) . . ?
C19 C20 H20 124.9 . . ?
C21 C20 Th1 72.7(5) . . ?
C21 C20 C19 110.2(9) . . ?
C21 C20 H20 124.9 . . ?
C20 C21 Th1 77.7(5) . . ?
C20 C21 C22 106.7(8) . . ?
C20 C21 C31 128.2(9) . . ?
C22 C21 Th1 78.8(5) . . ?
C22 C21 C31 122.7(9) . . ?
C31 C21 Th1 96.2(6) . . ?
Th1 C22 H22 110.5 . . ?
C18 C22 Th1 85.4(5) . . ?
C18 C22 H22 124.7 . . ?
C21 C22 Th1 71.4(5) . . ?
C21 C22 C18 110.7(8) . . ?
C21 C22 H22 124.7 . . ?
C18 C23 C24 110.0(8) . . ?
C18 C23 C25 119.2(8) . . ?
C18 C23 C26 106.7(8) . . ?
C25 C23 C24 104.8(8) . . ?
C25 C23 C26 109.3(9) . . ?
C26 C23 C24 106.2(8) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C19 C27 C28 115.4(8) . . ?
C19 C27 C29 108.9(8) . . ?
C19 C27 C30 111.6(8) . . ?
C28 C27 C29 109.9(8) . . ?
C30 C27 C28 105.5(8) . . ?
C30 C27 C29 105.0(8) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C21 C31 C32 110.1(9) . . ?
C21 C31 C33 112.2(9) . . ?
C21 C31 C34 103.9(8) . . ?
C33 C31 C32 108.1(9) . . ?
C33 C31 C34 111.5(9) . . ?
C34 C31 C32 111.1(9) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
Th1 C34 H34A 111.0 . . ?
Th1 C34 H34B 111.0 . . ?
C31 C34 Th1 103.7(6) . . ?
C31 C34 H34A 111.0 . . ?
C31 C34 H34B 111.0 . . ?
H34A C34 H34B 109.0 . . ?
P1 C35 H35A 109.5 . . ?
P1 C35 H35B 109.5 . . ?
P1 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
P1 C36 H36A 109.5 . . ?
P1 C36 H36B 109.5 . . ?
P1 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
Th1 C37 H37A 113.6 . . ?
Th1 C37 H37B 113.6 . . ?
P1 C37 Th1 90.1(4) . . ?
P1 C37 H37A 113.6 . . ?
P1 C37 H37B 113.6 . . ?
H37A C37 H37B 110.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Th1 C1 C2 C3 63.9(6) . . . . ?
Th1 C1 C2 C10 -132.6(11) . . . . ?
Th1 C1 C5 C4 -69.9(6) . . . . ?
Th1 C1 C6 C7 -78.1(9) . . . . ?
Th1 C1 C6 C8 41.2(11) . . . . ?
Th1 C1 C6 C9 167.2(7) . . . . ?
Th1 C2 C3 C4 70.9(7) . . . . ?
Th1 C2 C10 C11 -82.0(11) . . . . ?
Th1 C2 C10 C12 157.8(7) . . . . ?
Th1 C2 C10 C13 39.9(12) . . . . ?
Th1 C3 C4 C5 71.3(6) . . . . ?
Th1 C3 C4 C14 -115.9(9) . . . . ?
Th1 C4 C5 C1 74.4(6) . . . . ?
Th1 C4 C14 C15 -161.6(7) . . . . ?
Th1 C4 C14 C16 -43.0(12) . . . . ?
Th1 C4 C14 C17 81.1(9) . . . . ?
Th1 C18 C19 C20 -59.2(6) . . . . ?
Th1 C18 C19 C27 129.4(10) . . . . ?
Th1 C18 C22 C21 68.2(7) . . . . ?
Th1 C18 C23 C24 42.5(11) . . . . ?
Th1 C18 C23 C25 -78.4(12) . . . . ?
Th1 C18 C23 C26 157.3(7) . . . . ?
Th1 C19 C20 C21 -69.9(7) . . . . ?
Th1 C19 C27 C28 47.5(11) . . . . ?
Th1 C19 C27 C29 171.6(6) . . . . ?
Th1 C19 C27 C30 -73.0(10) . . . . ?
Th1 C20 C21 C22 -74.2(6) . . . . ?
Th1 C20 C21 C31 88.2(9) . . . . ?
Th1 C21 C22 C18 -77.5(7) . . . . ?
Th1 C21 C31 C32 109.6(8) . . . . ?
Th1 C21 C31 C33 -130.0(8) . . . . ?
Th1 C21 C31 C34 -9.4(8) . . . . ?
O1 P1 C37 Th1 8.2(4) . . . . ?
C1 C2 C3 Th1 -68.5(6) . . . . ?
C1 C2 C3 C4 2.3(10) . . . . ?
C1 C2 C10 C11 30.7(16) . . . . ?
C1 C2 C10 C12 -89.4(13) . . . . ?
C1 C2 C10 C13 152.7(11) . . . . ?
C2 C1 C5 Th1 67.1(6) . . . . ?
C2 C1 C5 C4 -2.8(10) . . . . ?
C2 C1 C6 C7 176.4(9) . . . . ?
C2 C1 C6 C8 -64.2(13) . . . . ?
C2 C1 C6 C9 61.7(13) . . . . ?
C2 C3 C4 Th1 -75.2(7) . . . . ?
C2 C3 C4 C5 -4.0(10) . . . . ?
C2 C3 C4 C14 168.8(9) . . . . ?
C3 C2 C10 C11 -167.1(9) . . . . ?
C3 C2 C10 C12 72.7(11) . . . . ?
C3 C2 C10 C13 -45.2(12) . . . . ?
C3 C4 C5 Th1 -70.3(6) . . . . ?
C3 C4 C5 C1 4.1(10) . . . . ?
C3 C4 C14 C15 -68.2(12) . . . . ?
C3 C4 C14 C16 50.4(14) . . . . ?
C3 C4 C14 C17 174.5(9) . . . . ?
C5 C1 C2 Th1 -63.6(6) . . . . ?
C5 C1 C2 C3 0.2(10) . . . . ?
C5 C1 C2 C10 163.8(10) . . . . ?
C5 C1 C6 C7 8.1(12) . . . . ?
C5 C1 C6 C8 127.5(9) . . . . ?
C5 C1 C6 C9 -106.6(10) . . . . ?
C5 C4 C14 C15 103.1(11) . . . . ?
C5 C4 C14 C16 -138.3(11) . . . . ?
C5 C4 C14 C17 -14.2(14) . . . . ?
C6 C1 C2 Th1 127.1(10) . . . . ?
C6 C1 C2 C3 -169.0(9) . . . . ?
C6 C1 C2 C10 -5.5(18) . . . . ?
C6 C1 C5 Th1 -121.9(7) . . . . ?
C6 C1 C5 C4 168.2(8) . . . . ?
C10 C2 C3 Th1 124.5(8) . . . . ?
C10 C2 C3 C4 -164.6(8) . . . . ?
C14 C4 C5 Th1 116.9(10) . . . . ?
C14 C4 C5 C1 -168.7(9) . . . . ?
C18 C19 C20 Th1 66.5(6) . . . . ?
C18 C19 C20 C21 -3.4(10) . . . . ?
C18 C19 C27 C28 -60.8(13) . . . . ?
C18 C19 C27 C29 63.3(12) . . . . ?
C18 C19 C27 C30 178.8(9) . . . . ?
C19 C18 C22 Th1 -66.2(6) . . . . ?
C19 C18 C22 C21 2.0(10) . . . . ?
C19 C18 C23 C24 160.1(9) . . . . ?
C19 C18 C23 C25 39.2(15) . . . . ?
C19 C18 C23 C26 -85.1(11) . . . . ?
C19 C20 C21 Th1 78.8(6) . . . . ?
C19 C20 C21 C22 4.6(11) . . . . ?
C19 C20 C21 C31 167.1(9) . . . . ?
C20 C19 C27 C28 128.6(9) . . . . ?
C20 C19 C27 C29 -107.2(10) . . . . ?
C20 C19 C27 C30 8.2(12) . . . . ?
C20 C21 C22 Th1 73.4(6) . . . . ?
C20 C21 C22 C18 -4.1(11) . . . . ?
C20 C21 C31 C32 30.4(13) . . . . ?
C20 C21 C31 C33 150.8(10) . . . . ?
C20 C21 C31 C34 -88.6(12) . . . . ?
C21 C31 C34 Th1 10.3(9) . . . . ?
C22 C18 C19 Th1 60.0(6) . . . . ?
C22 C18 C19 C20 0.9(9) . . . . ?
C22 C18 C19 C27 -170.6(9) . . . . ?
C22 C18 C23 C24 -42.4(11) . . . . ?
C22 C18 C23 C25 -163.3(9) . . . . ?
C22 C18 C23 C26 72.4(11) . . . . ?
C22 C21 C31 C32 -169.7(9) . . . . ?
C22 C21 C31 C33 -49.2(13) . . . . ?
C22 C21 C31 C34 71.3(11) . . . . ?
C23 C18 C19 Th1 -140.4(10) . . . . ?
C23 C18 C19 C20 160.4(9) . . . . ?
C23 C18 C19 C27 -11.0(16) . . . . ?
C23 C18 C22 Th1 130.8(7) . . . . ?
C23 C18 C22 C21 -161.0(8) . . . . ?
C27 C19 C20 Th1 -120.8(8) . . . . ?
C27 C19 C20 C21 169.3(8) . . . . ?
C31 C21 C22 Th1 -90.3(8) . . . . ?
C31 C21 C22 C18 -167.7(8) . . . . ?
C32 C31 C34 Th1 -108.0(8) . . . . ?
C33 C31 C34 Th1 131.4(8) . . . . ?
C35 P1 O1 Th1 -134.3(5) . . . . ?
C35 P1 C37 Th1 128.7(4) . . . . ?
C36 P1 O1 Th1 111.9(4) . . . . ?
C36 P1 C37 Th1 -112.4(5) . . . . ?
C37 P1 O1 Th1 -9.3(5) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.050
_oxdiff_exptl_absorpt_empirical_full_min 0.484
