#------------------------------------------------------------------------------
#$Date: 2019-11-07 23:19:42 +0100 (jue 07 de nov de 2019) $
#$Revision: 224228 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/99/7049929.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7049929
loop_
_publ_author_name
'Zhang, Congcong'
'Wang, Yongsong'
'Hou, Guohua'
'Ding, Wanjian'
'Zi, Guofu'
'Walter, Marc D.'
_publ_section_title
;
 Experimental and computational studies on a three-membered diphosphido
 thorium metallaheterocycle
 [η⁵-1,3-(Me₃C)₂C₅H₃]₂Th[η²-P₂(2,4,6-ⁱPr₃C₆H₂)₂].
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6921
_journal_page_last               6930
_journal_paper_doi               10.1039/c9dt01160a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C63 H93 N P2 Th, C6 H6, 0.5(C6 H14)'
_chemical_formula_sum            'C72 H106 N P2 Th'
_chemical_formula_weight         1279.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-08-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2019-02-25 deposited with the CCDC.    2019-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.5700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9693(3)
_cell_length_b                   18.0772(2)
_cell_length_c                   18.9897(3)
_cell_measurement_reflns_used    15394
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.1220
_cell_measurement_theta_min      4.5260
_cell_volume                     6690.76(17)
_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)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -47.00  33.00   1.00    1.00    --  -41.49  37.00  90.00   80
  2  ω     25.00  93.00   1.00    1.00    --   41.49-125.00-150.00   68
  3  ω     73.00 108.00   1.00    1.00    --   41.49  37.00-180.00   35
  4  ω     24.00  91.00   1.00    1.00    --   41.49-125.00  60.00   67
  5  ω     81.00 150.00   1.00    1.00    --  107.19  45.00-150.00   69
  6  ω     34.00 140.00   1.00    1.00    --  107.19 -77.00-150.00  106
  7  ω     97.00 135.00   1.00    1.00    --  107.19 -61.00 -30.00   38
  8  ω     35.00 107.00   1.00    1.00    --  107.19 -94.00 120.00   72
  9  ω     34.00 115.00   1.00    1.00    --  107.19-125.00  90.00   81
 10  ω     89.00 169.00   1.00    1.00    --  107.19  45.00 -30.00   80
 11  ω     93.00 118.00   1.00    1.00    --  107.19  45.00   0.00   25
;
_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      0.0735065000
_diffrn_orient_matrix_UB_12      0.0031887000
_diffrn_orient_matrix_UB_13      -0.0128445000
_diffrn_orient_matrix_UB_21      -0.0141855000
_diffrn_orient_matrix_UB_22      0.0779958000
_diffrn_orient_matrix_UB_23      -0.0324830000
_diffrn_orient_matrix_UB_31      0.0253750000
_diffrn_orient_matrix_UB_32      0.0342857000
_diffrn_orient_matrix_UB_33      0.0753765000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27849
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.227
_diffrn_reflns_theta_min         3.802
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.920
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66071
_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_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       block
_exptl_crystal_F_000             2660
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.453
_refine_diff_density_min         -1.804
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         13109
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0452P)²+11.6778P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11539
_reflns_number_total             13109
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt01160a2.cif
_cod_data_source_block           compound6
_cod_depositor_comments
'Adding full bibliography for 7049925--7049929.cif.'
_cod_database_code               7049929
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1P1Th1
_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.
;
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 C64-C69
 1.39 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 C40(H40), C43(H43), C46(H46), C55(H55), C58(H58), C61(H61)
3.b Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C72(H72A,H72B)
3.c Aromatic/amide H refined with riding coordinates:
 C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69), C2(H2), C4(H4),
 C5(H5), C15(H15), C17(H17), C18(H18), C29(H29), C30(H30), C31(H31), C32(H32),
 C33(H33), C36(H36), C38(H38), C51(H51), C53(H53)
3.d Fitted hexagon refined as free rotating group:
 C64(C65,C66,C67,C68,C69)
3.e 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), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C),
 C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C56(H56A,H56B,
 H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,
 H62B,H62C), C63(H63A,H63B,H63C), C70(H70A,H70B,H70C)
;
_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 1.422
_oxdiff_exptl_absorpt_empirical_full_min 0.763
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'
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
C64 C 0.6384(3) 0.3230(4) 0.8063(3) 0.097(3) Uani 1 1 d D
H64 H 0.6641 0.3436 0.7758 0.117 Uiso 1 1 calc R
C65 C 0.5981(4) 0.3680(3) 0.8395(4) 0.102(4) Uani 1 1 d G
H65 H 0.5967 0.4187 0.8313 0.123 Uiso 1 1 calc R
C66 C 0.5597(3) 0.3371(4) 0.8850(3) 0.088(3) Uani 1 1 d G
H66 H 0.5327 0.3673 0.9073 0.105 Uiso 1 1 calc R
C67 C 0.5617(3) 0.2613(4) 0.8972(3) 0.082(3) Uani 1 1 d G
H67 H 0.5361 0.2406 0.9277 0.098 Uiso 1 1 calc R
C68 C 0.6021(4) 0.2163(3) 0.8640(3) 0.093(3) Uani 1 1 d G
H68 H 0.6034 0.1655 0.8722 0.112 Uiso 1 1 calc R
C69 C 0.6404(3) 0.2471(4) 0.8185(3) 0.087(3) Uani 1 1 d DG
H69 H 0.6674 0.2170 0.7962 0.105 Uiso 1 1 calc R
C1 C 0.0327(2) 0.4288(3) 0.1812(2) 0.0202(9) Uani 1 1 d .
C2 C 0.0689(2) 0.4885(3) 0.1588(2) 0.0219(9) Uani 1 1 d .
H2 H 0.0717 0.5360 0.1782 0.026 Uiso 1 1 calc R
C3 C 0.1003(2) 0.4652(3) 0.1023(2) 0.0229(9) Uani 1 1 d .
C4 C 0.0855(2) 0.3893(3) 0.0912(2) 0.0222(10) Uani 1 1 d .
H4 H 0.0999 0.3591 0.0577 0.027 Uiso 1 1 calc R
C5 C 0.0445(2) 0.3666(3) 0.1404(2) 0.0209(9) Uani 1 1 d .
H5 H 0.0284 0.3190 0.1449 0.025 Uiso 1 1 calc R
C6 C -0.0180(2) 0.4328(3) 0.2299(2) 0.0201(9) Uani 1 1 d .
C7 C -0.0889(2) 0.4514(3) 0.1825(3) 0.0316(11) Uani 1 1 d .
H7A H -0.0873 0.4993 0.1611 0.047 Uiso 1 1 calc GR
H7B H -0.1226 0.4516 0.2117 0.047 Uiso 1 1 calc GR
H7C H -0.1010 0.4149 0.1451 0.047 Uiso 1 1 calc GR
C8 C -0.0231(3) 0.3585(3) 0.2666(3) 0.0265(10) Uani 1 1 d .
H8A H -0.0382 0.3213 0.2306 0.040 Uiso 1 1 calc GR
H8B H -0.0555 0.3624 0.2971 0.040 Uiso 1 1 calc GR
H8C H 0.0210 0.3452 0.2952 0.040 Uiso 1 1 calc GR
C9 C 0.0014(2) 0.4931(3) 0.2873(2) 0.0220(9) Uani 1 1 d .
H9A H 0.0455 0.4822 0.3173 0.033 Uiso 1 1 calc GR
H9B H -0.0324 0.4950 0.3163 0.033 Uiso 1 1 calc GR
H9C H 0.0032 0.5401 0.2641 0.033 Uiso 1 1 calc GR
C10 C 0.1416(2) 0.5133(3) 0.0615(2) 0.0263(10) Uani 1 1 d .
C11 C 0.2078(2) 0.5376(3) 0.1145(3) 0.0320(11) Uani 1 1 d .
H11A H 0.1961 0.5625 0.1548 0.048 Uiso 1 1 calc GR
H11B H 0.2332 0.5706 0.0904 0.048 Uiso 1 1 calc GR
H11C H 0.2352 0.4949 0.1311 0.048 Uiso 1 1 calc GR
C12 C 0.0993(3) 0.5810(3) 0.0307(3) 0.0334(12) Uani 1 1 d .
H12A H 0.0585 0.5652 -0.0026 0.050 Uiso 1 1 calc GR
H12B H 0.1259 0.6119 0.0060 0.050 Uiso 1 1 calc GR
H12C H 0.0870 0.6084 0.0692 0.050 Uiso 1 1 calc GR
C13 C 0.1616(3) 0.4699(3) -0.0001(3) 0.0362(12) Uani 1 1 d .
H13A H 0.1898 0.4286 0.0193 0.054 Uiso 1 1 calc GR
H13B H 0.1865 0.5016 -0.0259 0.054 Uiso 1 1 calc GR
H13C H 0.1209 0.4523 -0.0325 0.054 Uiso 1 1 calc GR
C14 C 0.2994(2) 0.3230(3) 0.2168(3) 0.0218(9) Uani 1 1 d .
C15 C 0.2738(2) 0.2782(3) 0.2655(2) 0.0211(9) Uani 1 1 d .
H15 H 0.2931 0.2741 0.3145 0.025 Uiso 1 1 calc R
C16 C 0.2141(2) 0.2403(2) 0.2290(3) 0.0216(9) Uani 1 1 d .
C17 C 0.2010(2) 0.2659(3) 0.1562(3) 0.0229(9) Uani 1 1 d .
H17 H 0.1641 0.2519 0.1197 0.027 Uiso 1 1 calc R
C18 C 0.2533(2) 0.3160(3) 0.1488(3) 0.0233(9) Uani 1 1 d .
H18 H 0.2569 0.3403 0.1066 0.028 Uiso 1 1 calc R
C19 C 0.3696(2) 0.3594(3) 0.2291(3) 0.0239(10) Uani 1 1 d .
C20 C 0.4152(2) 0.3121(3) 0.1918(3) 0.0326(12) Uani 1 1 d .
H20A H 0.4178 0.2628 0.2109 0.049 Uiso 1 1 calc GR
H20B H 0.4604 0.3332 0.2002 0.049 Uiso 1 1 calc GR
H20C H 0.3960 0.3107 0.1409 0.049 Uiso 1 1 calc GR
C21 C 0.3657(3) 0.4380(3) 0.1984(3) 0.0310(11) Uani 1 1 d .
H21A H 0.3438 0.4369 0.1481 0.047 Uiso 1 1 calc GR
H21B H 0.4112 0.4577 0.2039 0.047 Uiso 1 1 calc GR
H21C H 0.3397 0.4688 0.2238 0.047 Uiso 1 1 calc GR
C22 C 0.4026(2) 0.3635(3) 0.3099(3) 0.0307(11) Uani 1 1 d .
H22A H 0.3746 0.3934 0.3338 0.046 Uiso 1 1 calc GR
H22B H 0.4474 0.3850 0.3165 0.046 Uiso 1 1 calc GR
H22C H 0.4062 0.3145 0.3300 0.046 Uiso 1 1 calc GR
C23 C 0.1757(2) 0.1787(3) 0.2572(3) 0.0241(10) Uani 1 1 d .
C24 C 0.2012(2) 0.1696(3) 0.3384(3) 0.0303(11) Uani 1 1 d .
H24A H 0.2493 0.1580 0.3489 0.045 Uiso 1 1 calc GR
H24B H 0.1764 0.1303 0.3552 0.045 Uiso 1 1 calc GR
H24C H 0.1940 0.2148 0.3622 0.045 Uiso 1 1 calc GR
C25 C 0.0983(2) 0.1916(3) 0.2407(3) 0.0258(10) Uani 1 1 d .
H25A H 0.0884 0.2357 0.2646 0.039 Uiso 1 1 calc GR
H25B H 0.0761 0.1501 0.2575 0.039 Uiso 1 1 calc GR
H25C H 0.0818 0.1969 0.1895 0.039 Uiso 1 1 calc GR
C26 C 0.1900(3) 0.1066(3) 0.2191(3) 0.0356(13) Uani 1 1 d .
H26A H 0.1732 0.1117 0.1679 0.053 Uiso 1 1 calc GR
H26B H 0.1671 0.0659 0.2364 0.053 Uiso 1 1 calc GR
H26C H 0.2385 0.0973 0.2292 0.053 Uiso 1 1 calc GR
C27 C 0.1488(2) 0.3971(2) 0.3993(3) 0.0195(9) Uani 1 1 d .
C28 C 0.1023(2) 0.3652(3) 0.4433(2) 0.0199(9) Uani 1 1 d .
C29 C 0.0796(2) 0.2920(3) 0.4309(2) 0.0228(9) Uani 1 1 d .
H29 H 0.0956 0.2632 0.3974 0.027 Uiso 1 1 calc R
C30 C 0.0332(2) 0.2622(3) 0.4685(3) 0.0270(10) Uani 1 1 d .
H30 H 0.0180 0.2137 0.4598 0.032 Uiso 1 1 calc R
C31 C 0.0099(2) 0.3043(3) 0.5182(3) 0.0309(11) Uani 1 1 d .
H31 H -0.0214 0.2844 0.5427 0.037 Uiso 1 1 calc R
C32 C 0.0327(3) 0.3768(3) 0.5325(3) 0.0303(11) Uani 1 1 d .
H32 H 0.0174 0.4049 0.5669 0.036 Uiso 1 1 calc R
C33 C 0.0788(2) 0.4066(3) 0.4947(3) 0.0263(10) Uani 1 1 d .
H33 H 0.0941 0.4549 0.5041 0.032 Uiso 1 1 calc R
C34 C 0.2450(2) 0.4824(3) 0.5133(2) 0.0198(9) Uani 1 1 d .
C35 C 0.2366(2) 0.5367(3) 0.5648(2) 0.0212(9) Uani 1 1 d .
C36 C 0.2788(2) 0.5337(3) 0.6336(2) 0.0225(9) Uani 1 1 d .
H36 H 0.2740 0.5700 0.6669 0.027 Uiso 1 1 calc R
C37 C 0.3279(2) 0.4787(3) 0.6546(2) 0.0211(9) Uani 1 1 d .
C38 C 0.3356(2) 0.4264(3) 0.6038(2) 0.0223(9) Uani 1 1 d .
H38 H 0.3682 0.3894 0.6170 0.027 Uiso 1 1 calc R
C39 C 0.2960(2) 0.4273(3) 0.5334(2) 0.0198(9) Uani 1 1 d .
C40 C 0.1834(2) 0.5987(3) 0.5495(2) 0.0242(10) Uani 1 1 d .
H40 H 0.1486 0.5833 0.5073 0.029 Uiso 1 1 calc R
C41 C 0.2157(3) 0.6697(3) 0.5280(3) 0.0403(13) Uani 1 1 d .
H41A H 0.2506 0.6866 0.5678 0.060 Uiso 1 1 calc GR
H41B H 0.1810 0.7070 0.5155 0.060 Uiso 1 1 calc GR
H41C H 0.2356 0.6599 0.4873 0.060 Uiso 1 1 calc GR
C42 C 0.1465(3) 0.6113(4) 0.6099(3) 0.0431(15) Uani 1 1 d .
H42A H 0.1305 0.5648 0.6244 0.065 Uiso 1 1 calc GR
H42B H 0.1081 0.6436 0.5935 0.065 Uiso 1 1 calc GR
H42C H 0.1773 0.6335 0.6502 0.065 Uiso 1 1 calc GR
C43 C 0.3706(2) 0.4769(3) 0.7318(2) 0.0253(10) Uani 1 1 d .
H43 H 0.3410 0.4936 0.7636 0.030 Uiso 1 1 calc R
C44 C 0.4305(3) 0.5310(3) 0.7405(3) 0.0356(12) Uani 1 1 d .
H44A H 0.4604 0.5164 0.7096 0.053 Uiso 1 1 calc GR
H44B H 0.4556 0.5308 0.7898 0.053 Uiso 1 1 calc GR
H44C H 0.4133 0.5799 0.7277 0.053 Uiso 1 1 calc GR
C45 C 0.3965(3) 0.3995(3) 0.7569(3) 0.0371(13) Uani 1 1 d .
H45A H 0.3585 0.3657 0.7494 0.056 Uiso 1 1 calc GR
H45B H 0.4180 0.4009 0.8073 0.056 Uiso 1 1 calc GR
H45C H 0.4292 0.3833 0.7298 0.056 Uiso 1 1 calc GR
C46 C 0.3080(2) 0.3655(3) 0.4834(2) 0.0211(9) Uani 1 1 d .
H46 H 0.2857 0.3787 0.4338 0.025 Uiso 1 1 calc R
C47 C 0.3849(2) 0.3521(3) 0.4869(3) 0.0282(10) Uani 1 1 d .
H47A H 0.4056 0.3971 0.4753 0.042 Uiso 1 1 calc GR
H47B H 0.3900 0.3144 0.4529 0.042 Uiso 1 1 calc GR
H47C H 0.4069 0.3365 0.5346 0.042 Uiso 1 1 calc GR
C48 C 0.2760(2) 0.2937(3) 0.5035(3) 0.0284(10) Uani 1 1 d .
H48A H 0.2978 0.2799 0.5519 0.043 Uiso 1 1 calc GR
H48B H 0.2824 0.2551 0.4709 0.043 Uiso 1 1 calc GR
H48C H 0.2279 0.3011 0.5005 0.043 Uiso 1 1 calc GR
C49 C 0.2640(2) 0.5996(2) 0.3486(2) 0.0191(9) Uani 1 1 d .
C50 C 0.2167(2) 0.6578(3) 0.3265(3) 0.0238(10) Uani 1 1 d .
C51 C 0.2381(3) 0.7308(3) 0.3422(3) 0.0315(11) Uani 1 1 d .
H51 H 0.2070 0.7688 0.3267 0.038 Uiso 1 1 calc R
C52 C 0.3033(3) 0.7487(3) 0.3797(4) 0.0380(13) Uani 1 1 d .
C53 C 0.3494(2) 0.6920(3) 0.3993(3) 0.0327(12) Uani 1 1 d .
H53 H 0.3941 0.7033 0.4228 0.039 Uiso 1 1 calc R
C54 C 0.3316(2) 0.6179(3) 0.3852(3) 0.0233(10) Uani 1 1 d .
C55 C 0.1417(2) 0.6461(3) 0.2902(3) 0.0261(10) Uani 1 1 d .
H55 H 0.1348 0.5932 0.2797 0.031 Uiso 1 1 calc R
C56 C 0.1218(3) 0.6883(3) 0.2187(3) 0.0335(12) Uani 1 1 d .
H56A H 0.1290 0.7403 0.2275 0.050 Uiso 1 1 calc GR
H56B H 0.0743 0.6795 0.1974 0.050 Uiso 1 1 calc GR
H56C H 0.1495 0.6716 0.1865 0.050 Uiso 1 1 calc GR
C57 C 0.0953(2) 0.6682(3) 0.3405(3) 0.0263(10) Uani 1 1 d .
H57A H 0.1050 0.6375 0.3828 0.039 Uiso 1 1 calc GR
H57B H 0.0482 0.6621 0.3162 0.039 Uiso 1 1 calc GR
H57C H 0.1036 0.7190 0.3545 0.039 Uiso 1 1 calc GR
C58 C 0.3226(3) 0.8287(3) 0.4042(4) 0.0525(18) Uani 1 1 d .
H58 H 0.3718 0.8295 0.4262 0.063 Uiso 1 1 calc R
C59 C 0.3107(6) 0.8800(4) 0.3460(5) 0.083(3) Uani 1 1 d .
H59A H 0.3397 0.8681 0.3134 0.124 Uiso 1 1 calc GR
H59B H 0.3209 0.9292 0.3645 0.124 Uiso 1 1 calc GR
H59C H 0.2635 0.8774 0.3209 0.124 Uiso 1 1 calc GR
C60 C 0.2847(4) 0.8540(4) 0.4608(5) 0.072(2) Uani 1 1 d .
H60A H 0.2362 0.8477 0.4428 0.108 Uiso 1 1 calc GR
H60B H 0.2944 0.9053 0.4716 0.108 Uiso 1 1 calc GR
H60C H 0.2993 0.8251 0.5038 0.108 Uiso 1 1 calc GR
C61 C 0.3865(2) 0.5606(3) 0.4127(3) 0.0269(10) Uani 1 1 d .
H61 H 0.3652 0.5116 0.4038 0.032 Uiso 1 1 calc R
C62 C 0.4442(3) 0.5649(3) 0.3717(3) 0.0346(12) Uani 1 1 d .
H62A H 0.4260 0.5559 0.3214 0.052 Uiso 1 1 calc GR
H62B H 0.4784 0.5284 0.3903 0.052 Uiso 1 1 calc GR
H62C H 0.4646 0.6132 0.3778 0.052 Uiso 1 1 calc GR
C63 C 0.4152(3) 0.5678(3) 0.4939(3) 0.0321(11) Uani 1 1 d .
H63A H 0.4386 0.6142 0.5039 0.048 Uiso 1 1 calc GR
H63B H 0.4468 0.5281 0.5100 0.048 Uiso 1 1 calc GR
H63C H 0.3783 0.5655 0.5188 0.048 Uiso 1 1 calc GR
N1 N 0.15415(18) 0.3706(2) 0.33815(18) 0.0181(7) Uani 1 1 d .
P1 P 0.18632(5) 0.48932(6) 0.42331(6) 0.0171(2) Uani 1 1 d .
P2 P 0.23926(5) 0.50020(6) 0.33556(6) 0.0173(2) Uani 1 1 d .
Th1 Th 0.17392(2) 0.39237(2) 0.22905(2) 0.01651(6) Uani 1 1 d .
C70 C 0.3623(5) 0.4078(6) 0.9813(5) 0.100(4) Uani 1 1 d .
H70A H 0.3615 0.3871 0.9345 0.150 Uiso 1 1 calc GR
H70B H 0.3350 0.4519 0.9760 0.150 Uiso 1 1 calc GR
H70C H 0.3440 0.3725 1.0099 0.150 Uiso 1 1 calc GR
C71 C 0.4346(5) 0.4261(7) 1.0177(5) 0.105(4) Uani 1 1 d .
H71A H 0.4361 0.4385 1.0678 0.126 Uiso 1 1 calc R
H71B H 0.4631 0.3827 1.0171 0.126 Uiso 1 1 calc R
C72 C 0.4634(4) 0.4891(5) 0.9827(4) 0.076(3) Uani 1 1 d .
H72A H 0.4341 0.5318 0.9830 0.091 Uiso 1 1 calc R
H72B H 0.4614 0.4762 0.9327 0.091 Uiso 1 1 calc R
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'
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
C65 C64 H64 120.0 . .
C65 C64 C69 120.0 . .
C69 C64 H64 120.0 . .
C64 C65 H65 120.0 . .
C66 C65 C64 120.0 . .
C66 C65 H65 120.0 . .
C65 C66 H66 120.0 . .
C65 C66 C67 120.0 . .
C67 C66 H66 120.0 . .
C66 C67 H67 120.0 . .
C68 C67 C66 120.0 . .
C68 C67 H67 120.0 . .
C67 C68 H68 120.0 . .
C67 C68 C69 120.0 . .
C69 C68 H68 120.0 . .
C64 C69 H69 120.0 . .
C68 C69 C64 120.0 . .
C68 C69 H69 120.0 . .
C2 C1 C6 126.9(4) . .
C2 C1 Th1 74.8(2) . .
C5 C1 C2 106.6(4) . .
C5 C1 C6 125.8(4) . .
C5 C1 Th1 73.7(2) . .
C6 C1 Th1 124.3(3) . .
C1 C2 H2 125.1 . .
C1 C2 C3 109.8(4) . .
C1 C2 Th1 76.3(3) . .
C3 C2 H2 125.1 . .
C3 C2 Th1 76.7(3) . .
Th1 C2 H2 113.9 . .
C2 C3 C10 126.4(4) . .
C2 C3 Th1 74.4(2) . .
C4 C3 C2 106.8(4) . .
C4 C3 C10 126.8(4) . .
C4 C3 Th1 74.3(3) . .
C10 C3 Th1 117.1(3) . .
C3 C4 H4 125.9 . .
C3 C4 C5 108.2(4) . .
C3 C4 Th1 76.9(3) . .
C5 C4 H4 125.9 . .
C5 C4 Th1 74.4(2) . .
Th1 C4 H4 115.0 . .
C1 C5 C4 108.5(4) . .
C1 C5 H5 125.8 . .
C1 C5 Th1 77.3(2) . .
C4 C5 H5 125.8 . .
C4 C5 Th1 76.1(2) . .
Th1 C5 H5 113.1 . .
C1 C6 C7 107.7(4) . .
C1 C6 C8 111.0(4) . .
C1 C6 C9 111.7(4) . .
C8 C6 C7 108.3(4) . .
C8 C6 C9 109.5(4) . .
C9 C6 C7 108.5(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 . .
C3 C10 C11 108.3(4) . .
C3 C10 C12 109.7(4) . .
C3 C10 C13 110.9(4) . .
C12 C10 C11 110.2(4) . .
C12 C10 C13 109.4(4) . .
C13 C10 C11 108.4(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 . .
C15 C14 C18 106.9(4) . .
C15 C14 C19 127.2(4) . .
C15 C14 Th1 75.4(2) . .
C18 C14 C19 124.8(4) . .
C18 C14 Th1 72.9(2) . .
C19 C14 Th1 126.4(3) . .
C14 C15 H15 124.9 . .
C14 C15 C16 110.1(4) . .
C14 C15 Th1 76.0(3) . .
C16 C15 H15 124.9 . .
C16 C15 Th1 76.2(3) . .
Th1 C15 H15 114.7 . .
C15 C16 C17 105.9(4) . .
C15 C16 C23 128.2(4) . .
C15 C16 Th1 75.0(3) . .
C17 C16 C23 125.6(4) . .
C17 C16 Th1 72.3(3) . .
C23 C16 Th1 122.8(3) . .
C16 C17 H17 125.6 . .
C16 C17 Th1 78.4(3) . .
C18 C17 C16 108.7(4) . .
C18 C17 H17 125.6 . .
C18 C17 Th1 75.5(3) . .
Th1 C17 H17 112.7 . .
C14 C18 H18 125.9 . .
C14 C18 Th1 78.0(3) . .
C17 C18 C14 108.3(4) . .
C17 C18 H18 125.9 . .
C17 C18 Th1 75.1(3) . .
Th1 C18 H18 113.4 . .
C14 C19 C20 108.0(4) . .
C14 C19 C21 112.0(4) . .
C14 C19 C22 110.7(4) . .
C20 C19 C21 109.2(4) . .
C20 C19 C22 108.7(4) . .
C21 C19 C22 108.2(4) . .
C19 C20 H20A 109.5 . .
C19 C20 H20B 109.5 . .
C19 C20 H20C 109.5 . .
H20A C20 H20B 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C19 C21 H21A 109.5 . .
C19 C21 H21B 109.5 . .
C19 C21 H21C 109.5 . .
H21A C21 H21B 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C19 C22 H22A 109.5 . .
C19 C22 H22B 109.5 . .
C19 C22 H22C 109.5 . .
H22A C22 H22B 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C16 C23 C24 110.8(4) . .
C16 C23 C25 112.5(4) . .
C16 C23 C26 107.1(4) . .
C24 C23 C25 109.0(4) . .
C24 C23 C26 109.1(4) . .
C25 C23 C26 108.2(4) . .
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 P1 118.6(3) . .
N1 C27 C28 123.2(4) . .
N1 C27 P1 116.9(3) . .
C29 C28 C27 119.1(4) . .
C33 C28 C27 122.1(4) . .
C33 C28 C29 118.7(4) . .
C28 C29 H29 119.9 . .
C30 C29 C28 120.2(5) . .
C30 C29 H29 119.9 . .
C29 C30 H30 120.0 . .
C31 C30 C29 120.0(5) . .
C31 C30 H30 120.0 . .
C30 C31 H31 119.6 . .
C30 C31 C32 120.7(5) . .
C32 C31 H31 119.6 . .
C31 C32 H32 120.4 . .
C33 C32 C31 119.2(5) . .
C33 C32 H32 120.4 . .
C28 C33 C32 121.0(5) . .
C28 C33 H33 119.5 . .
C32 C33 H33 119.5 . .
C35 C34 P1 116.2(3) . .
C39 C34 C35 119.1(4) . .
C39 C34 P1 124.7(3) . .
C34 C35 C40 123.9(4) . .
C36 C35 C34 118.7(4) . .
C36 C35 C40 117.4(4) . .
C35 C36 H36 118.6 . .
C37 C36 C35 122.7(4) . .
C37 C36 H36 118.6 . .
C36 C37 C43 120.1(4) . .
C38 C37 C36 117.8(4) . .
C38 C37 C43 122.1(4) . .
C37 C38 H38 118.9 . .
C37 C38 C39 122.3(4) . .
C39 C38 H38 118.9 . .
C34 C39 C46 123.5(4) . .
C38 C39 C34 119.3(4) . .
C38 C39 C46 117.1(4) . .
C35 C40 H40 106.6 . .
C35 C40 C41 110.5(4) . .
C41 C40 H40 106.6 . .
C42 C40 C35 113.6(4) . .
C42 C40 H40 106.6 . .
C42 C40 C41 112.3(4) . .
C40 C41 H41A 109.5 . .
C40 C41 H41B 109.5 . .
C40 C41 H41C 109.5 . .
H41A C41 H41B 109.5 . .
H41A C41 H41C 109.5 . .
H41B C41 H41C 109.5 . .
C40 C42 H42A 109.5 . .
C40 C42 H42B 109.5 . .
C40 C42 H42C 109.5 . .
H42A C42 H42B 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
C37 C43 H43 107.4 . .
C37 C43 C45 113.5(4) . .
C44 C43 C37 110.6(4) . .
C44 C43 H43 107.4 . .
C44 C43 C45 110.4(4) . .
C45 C43 H43 107.4 . .
C43 C44 H44A 109.5 . .
C43 C44 H44B 109.5 . .
C43 C44 H44C 109.5 . .
H44A C44 H44B 109.5 . .
H44A C44 H44C 109.5 . .
H44B C44 H44C 109.5 . .
C43 C45 H45A 109.5 . .
C43 C45 H45B 109.5 . .
C43 C45 H45C 109.5 . .
H45A C45 H45B 109.5 . .
H45A C45 H45C 109.5 . .
H45B C45 H45C 109.5 . .
C39 C46 H46 108.7 . .
C39 C46 C47 112.3(4) . .
C39 C46 C48 109.7(4) . .
C47 C46 H46 108.7 . .
C48 C46 H46 108.7 . .
C48 C46 C47 108.8(4) . .
C46 C47 H47A 109.5 . .
C46 C47 H47B 109.5 . .
C46 C47 H47C 109.5 . .
H47A C47 H47B 109.5 . .
H47A C47 H47C 109.5 . .
H47B C47 H47C 109.5 . .
C46 C48 H48A 109.5 . .
C46 C48 H48B 109.5 . .
C46 C48 H48C 109.5 . .
H48A C48 H48B 109.5 . .
H48A C48 H48C 109.5 . .
H48B C48 H48C 109.5 . .
C50 C49 C54 118.4(4) . .
C50 C49 P2 122.5(3) . .
C54 C49 P2 119.1(3) . .
C49 C50 C55 124.0(4) . .
C51 C50 C49 119.0(4) . .
C51 C50 C55 116.8(4) . .
C50 C51 H51 118.6 . .
C52 C51 C50 122.8(5) . .
C52 C51 H51 118.6 . .
C51 C52 C58 121.5(5) . .
C53 C52 C51 117.7(5) . .
C53 C52 C58 120.6(5) . .
C52 C53 H53 118.7 . .
C52 C53 C54 122.5(5) . .
C54 C53 H53 118.7 . .
C49 C54 C61 123.4(4) . .
C53 C54 C49 119.5(4) . .
C53 C54 C61 117.1(4) . .
C50 C55 H55 107.9 . .
C50 C55 C56 111.9(4) . .
C56 C55 H55 107.9 . .
C57 C55 C50 110.6(4) . .
C57 C55 H55 107.9 . .
C57 C55 C56 110.5(4) . .
C55 C56 H56A 109.5 . .
C55 C56 H56B 109.5 . .
C55 C56 H56C 109.5 . .
H56A C56 H56B 109.5 . .
H56A C56 H56C 109.5 . .
H56B C56 H56C 109.5 . .
C55 C57 H57A 109.5 . .
C55 C57 H57B 109.5 . .
C55 C57 H57C 109.5 . .
H57A C57 H57B 109.5 . .
H57A C57 H57C 109.5 . .
H57B C57 H57C 109.5 . .
C52 C58 H58 107.7 . .
C59 C58 C52 112.9(6) . .
C59 C58 H58 107.7 . .
C59 C58 C60 109.2(7) . .
C60 C58 C52 111.5(5) . .
C60 C58 H58 107.7 . .
C58 C59 H59A 109.5 . .
C58 C59 H59B 109.5 . .
C58 C59 H59C 109.5 . .
H59A C59 H59B 109.5 . .
H59A C59 H59C 109.5 . .
H59B C59 H59C 109.5 . .
C58 C60 H60A 109.5 . .
C58 C60 H60B 109.5 . .
C58 C60 H60C 109.5 . .
H60A C60 H60B 109.5 . .
H60A C60 H60C 109.5 . .
H60B C60 H60C 109.5 . .
C54 C61 H61 107.7 . .
C54 C61 C62 111.0(4) . .
C54 C61 C63 111.9(4) . .
C62 C61 H61 107.7 . .
C62 C61 C63 110.5(4) . .
C63 C61 H61 107.7 . .
C61 C62 H62A 109.5 . .
C61 C62 H62B 109.5 . .
C61 C62 H62C 109.5 . .
H62A C62 H62B 109.5 . .
H62A C62 H62C 109.5 . .
H62B C62 H62C 109.5 . .
C61 C63 H63A 109.5 . .
C61 C63 H63B 109.5 . .
C61 C63 H63C 109.5 . .
H63A C63 H63B 109.5 . .
H63A C63 H63C 109.5 . .
H63B C63 H63C 109.5 . .
C27 N1 Th1 147.5(3) . .
C27 P1 C34 108.0(2) . .
C27 P1 P2 97.58(16) . .
C34 P1 P2 113.49(14) . .
C49 P2 P1 98.30(15) . .
C49 P2 Th1 143.53(15) . .
P1 P2 Th1 104.71(5) . .
C1 Th1 C3 48.00(13) . .
C1 Th1 C14 154.37(13) . .
C1 Th1 C15 146.96(13) . .
C1 Th1 C16 118.70(13) . .
C1 Th1 P2 109.31(9) . .
C2 Th1 C1 28.88(13) . .
C2 Th1 C3 28.94(12) . .
C2 Th1 C14 143.71(13) . .
C2 Th1 C15 165.71(13) . .
C2 Th1 C16 140.32(13) . .
C2 Th1 P2 95.19(10) . .
C3 Th1 C14 115.73(13) . .
C3 Th1 C16 122.36(13) . .
C3 Th1 P2 110.39(10) . .
C4 Th1 C1 48.04(13) . .
C4 Th1 C2 47.45(13) . .
C4 Th1 C3 28.76(13) . .
C4 Th1 C14 107.40(13) . .
C4 Th1 C15 118.36(13) . .
C4 Th1 C16 95.70(13) . .
C4 Th1 P2 138.99(10) . .
C5 Th1 C1 29.00(13) . .
C5 Th1 C2 47.56(13) . .
C5 Th1 C3 48.00(13) . .
C5 Th1 C4 29.45(13) . .
C5 Th1 C14 126.12(13) . .
C5 Th1 C15 122.12(13) . .
C5 Th1 C16 93.54(13) . .
C5 Th1 P2 138.25(10) . .
C14 Th1 C16 47.76(12) . .
C14 Th1 P2 94.72(9) . .
C15 Th1 C3 138.08(13) . .
C15 Th1 C14 28.53(13) . .
C15 Th1 C16 28.78(12) . .
C15 Th1 P2 97.59(9) . .
C16 Th1 P2 124.13(9) . .
C17 Th1 C1 108.50(13) . .
C17 Th1 C2 118.36(13) . .
C17 Th1 C3 94.58(14) . .
C17 Th1 C4 70.91(13) . .
C17 Th1 C5 79.53(13) . .
C17 Th1 C14 47.99(13) . .
C17 Th1 C15 47.53(13) . .
C17 Th1 C16 29.21(13) . .
C17 Th1 C18 29.36(13) . .
C17 Th1 P2 142.18(9) . .
C18 Th1 C1 125.54(13) . .
C18 Th1 C2 119.87(13) . .
C18 Th1 C3 91.00(14) . .
C18 Th1 C4 78.42(13) . .
C18 Th1 C5 98.59(13) . .
C18 Th1 C14 29.07(13) . .
C18 Th1 C15 47.44(14) . .
C18 Th1 C16 48.15(13) . .
C18 Th1 P2 119.29(9) . .
N1 Th1 C1 88.53(13) . .
N1 Th1 C2 106.52(13) . .
N1 Th1 C3 134.66(13) . .
N1 Th1 C4 131.11(13) . .
N1 Th1 C5 101.69(13) . .
N1 Th1 C14 109.52(13) . .
N1 Th1 C15 84.38(13) . .
N1 Th1 C16 86.38(13) . .
N1 Th1 C17 114.18(14) . .
N1 Th1 C18 131.07(14) . .
N1 Th1 P2 67.35(10) . .
H70A C70 H70B 109.5 . .
H70A C70 H70C 109.5 . .
H70B C70 H70C 109.5 . .
C71 C70 H70A 109.5 . .
C71 C70 H70B 109.5 . .
C71 C70 H70C 109.5 . .
C70 C71 H71A 109.0 . .
C70 C71 H71B 109.0 . .
H71A C71 H71B 107.8 . .
C72 C71 C70 112.8(9) . .
C72 C71 H71A 109.0 . .
C72 C71 H71B 109.0 . .
C71 C72 C72 115.7(10) . 3_667
C71 C72 H72A 108.4 . .
C71 C72 H72B 108.4 . .
C72 C72 H72A 108.4 3_667 .
C72 C72 H72B 108.4 3_667 .
H72A C72 H72B 107.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C64 H64 0.9300 .
C64 C65 1.3900 .
C64 C69 1.3900 .
C65 H65 0.9300 .
C65 C66 1.3900 .
C66 H66 0.9300 .
C66 C67 1.3900 .
C67 H67 0.9300 .
C67 C68 1.3900 .
C68 H68 0.9300 .
C68 C69 1.3900 .
C69 H69 0.9300 .
C1 C2 1.414(6) .
C1 C5 1.414(6) .
C1 C6 1.515(6) .
C1 Th1 2.845(4) .
C2 H2 0.9300 .
C2 C3 1.420(6) .
C2 Th1 2.825(4) .
C3 C4 1.410(6) .
C3 C10 1.522(6) .
C3 Th1 2.855(4) .
C4 H4 0.9300 .
C4 C5 1.429(6) .
C4 Th1 2.821(4) .
C5 H5 0.9300 .
C5 Th1 2.799(4) .
C6 C7 1.541(6) .
C6 C8 1.526(6) .
C6 C9 1.531(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 1.540(7) .
C10 C12 1.529(7) .
C10 C13 1.532(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 1.405(6) .
C14 C18 1.418(6) .
C14 C19 1.522(6) .
C14 Th1 2.856(4) .
C15 H15 0.9300 .
C15 C16 1.419(6) .
C15 Th1 2.848(4) .
C16 C17 1.427(6) .
C16 C23 1.514(6) .
C16 Th1 2.864(4) .
C17 H17 0.9300 .
C17 C18 1.413(6) .
C17 Th1 2.786(4) .
C18 H18 0.9300 .
C18 Th1 2.791(4) .
C19 C20 1.530(6) .
C19 C21 1.531(7) .
C19 C22 1.534(7) .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
C21 H21A 0.9600 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
C22 H22A 0.9600 .
C22 H22B 0.9600 .
C22 H22C 0.9600 .
C23 C24 1.522(7) .
C23 C25 1.527(6) .
C23 C26 1.549(6) .
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 1.494(6) .
C27 N1 1.282(6) .
C27 P1 1.844(4) .
C28 C29 1.403(6) .
C28 C33 1.389(7) .
C29 H29 0.9300 .
C29 C30 1.396(6) .
C30 H30 0.9300 .
C30 C31 1.371(7) .
C31 H31 0.9300 .
C31 C32 1.394(7) .
C32 H32 0.9300 .
C32 C33 1.392(7) .
C33 H33 0.9300 .
C34 C35 1.421(6) .
C34 C39 1.415(6) .
C34 P1 1.855(4) .
C35 C36 1.394(6) .
C35 C40 1.528(6) .
C36 H36 0.9300 .
C36 C37 1.392(6) .
C37 C38 1.382(6) .
C37 C43 1.527(6) .
C38 H38 0.9300 .
C38 C39 1.398(6) .
C39 C46 1.520(6) .
C40 H40 0.9800 .
C40 C41 1.530(7) .
C40 C42 1.510(7) .
C41 H41A 0.9600 .
C41 H41B 0.9600 .
C41 H41C 0.9600 .
C42 H42A 0.9600 .
C42 H42B 0.9600 .
C42 H42C 0.9600 .
C43 H43 0.9800 .
C43 C44 1.526(7) .
C43 C45 1.531(7) .
C44 H44A 0.9600 .
C44 H44B 0.9600 .
C44 H44C 0.9600 .
C45 H45A 0.9600 .
C45 H45B 0.9600 .
C45 H45C 0.9600 .
C46 H46 0.9800 .
C46 C47 1.541(6) .
C46 C48 1.530(6) .
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 1.414(6) .
C49 C54 1.418(6) .
C49 P2 1.866(4) .
C50 C51 1.399(7) .
C50 C55 1.522(6) .
C51 H51 0.9300 .
C51 C52 1.379(7) .
C52 C53 1.375(7) .
C52 C58 1.542(7) .
C53 H53 0.9300 .
C53 C54 1.396(6) .
C54 C61 1.515(6) .
C55 H55 0.9800 .
C55 C56 1.532(7) .
C55 C57 1.521(7) .
C56 H56A 0.9600 .
C56 H56B 0.9600 .
C56 H56C 0.9600 .
C57 H57A 0.9600 .
C57 H57B 0.9600 .
C57 H57C 0.9600 .
C58 H58 0.9800 .
C58 C59 1.423(10) .
C58 C60 1.514(10) .
C59 H59A 0.9600 .
C59 H59B 0.9600 .
C59 H59C 0.9600 .
C60 H60A 0.9600 .
C60 H60B 0.9600 .
C60 H60C 0.9600 .
C61 H61 0.9800 .
C61 C62 1.527(7) .
C61 C63 1.529(7) .
C62 H62A 0.9600 .
C62 H62B 0.9600 .
C62 H62C 0.9600 .
C63 H63A 0.9600 .
C63 H63B 0.9600 .
C63 H63C 0.9600 .
N1 Th1 2.227(3) .
P1 P2 2.1677(15) .
P2 Th1 2.9059(11) .
C70 H70A 0.9600 .
C70 H70B 0.9600 .
C70 H70C 0.9600 .
C70 C71 1.496(12) .
C71 H71A 0.9700 .
C71 H71B 0.9700 .
C71 C72 1.495(12) .
C72 C72 1.520(14) 3_667
C72 H72A 0.9700 .
C72 H72B 0.9700 .
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_4
C64 C65 C66 C67 0.0 .
C65 C64 C69 C68 0.0 .
C65 C66 C67 C68 0.0 .
C66 C67 C68 C69 0.0 .
C67 C68 C69 C64 0.0 .
C69 C64 C65 C66 0.0 .
C1 C2 C3 C4 -2.2(5) .
C1 C2 C3 C10 177.6(4) .
C1 C2 C3 Th1 -69.9(3) .
C2 C1 C5 C4 -2.4(5) .
C2 C1 C5 Th1 68.1(3) .
C2 C1 C6 C7 85.4(5) .
C2 C1 C6 C8 -156.2(4) .
C2 C1 C6 C9 -33.7(6) .
C2 C3 C4 C5 0.6(5) .
C2 C3 C4 Th1 -67.8(3) .
C2 C3 C10 C11 66.3(6) .
C2 C3 C10 C12 -54.0(6) .
C2 C3 C10 C13 -174.9(4) .
C3 C4 C5 C1 1.1(5) .
C3 C4 C5 Th1 -70.2(3) .
C4 C3 C10 C11 -114.0(5) .
C4 C3 C10 C12 125.7(5) .
C4 C3 C10 C13 4.8(6) .
C5 C1 C2 C3 2.8(5) .
C5 C1 C2 Th1 -67.3(3) .
C5 C1 C6 C7 -83.8(5) .
C5 C1 C6 C8 34.6(6) .
C5 C1 C6 C9 157.1(4) .
C6 C1 C2 C3 -168.1(4) .
C6 C1 C2 Th1 121.7(4) .
C6 C1 C5 C4 168.7(4) .
C6 C1 C5 Th1 -120.8(4) .
C10 C3 C4 C5 -179.1(4) .
C10 C3 C4 Th1 112.4(4) .
C14 C15 C16 C17 -3.0(5) .
C14 C15 C16 C23 170.5(4) .
C14 C15 C16 Th1 -69.3(3) .
C15 C14 C18 C17 -1.3(5) .
C15 C14 C18 Th1 68.4(3) .
C15 C14 C19 C20 100.2(5) .
C15 C14 C19 C21 -139.6(5) .
C15 C14 C19 C22 -18.7(7) .
C15 C16 C17 C18 2.1(5) .
C15 C16 C17 Th1 -68.1(3) .
C15 C16 C23 C24 10.8(6) .
C15 C16 C23 C25 133.1(5) .
C15 C16 C23 C26 -108.1(5) .
C16 C17 C18 C14 -0.5(5) .
C16 C17 C18 Th1 -72.2(3) .
C17 C16 C23 C24 -176.9(4) .
C17 C16 C23 C25 -54.6(6) .
C17 C16 C23 C26 64.2(6) .
C18 C14 C15 C16 2.7(5) .
C18 C14 C15 Th1 -66.7(3) .
C18 C14 C19 C20 -66.3(6) .
C18 C14 C19 C21 54.0(6) .
C18 C14 C19 C22 174.8(4) .
C19 C14 C15 C16 -165.7(4) .
C19 C14 C15 Th1 124.9(5) .
C19 C14 C18 C17 167.4(4) .
C19 C14 C18 Th1 -122.9(4) .
C23 C16 C17 C18 -171.6(4) .
C23 C16 C17 Th1 118.2(4) .
C27 C28 C29 C30 -176.5(4) .
C27 C28 C33 C32 176.7(4) .
C28 C27 N1 Th1 148.8(4) .
C28 C27 P1 C34 65.7(4) .
C28 C27 P1 P2 -176.6(3) .
C28 C29 C30 C31 -0.5(7) .
C29 C28 C33 C32 -1.1(7) .
C29 C30 C31 C32 -0.7(7) .
C30 C31 C32 C33 1.0(8) .
C31 C32 C33 C28 -0.1(8) .
C33 C28 C29 C30 1.4(6) .
C34 C35 C36 C37 -1.6(7) .
C34 C35 C40 C41 -95.9(5) .
C34 C35 C40 C42 136.8(5) .
C34 C39 C46 C47 136.9(4) .
C34 C39 C46 C48 -102.0(5) .
C35 C34 C39 C38 1.7(6) .
C35 C34 C39 C46 178.2(4) .
C35 C34 P1 C27 -130.6(3) .
C35 C34 P1 P2 122.4(3) .
C35 C36 C37 C38 1.7(7) .
C35 C36 C37 C43 -177.5(4) .
C36 C35 C40 C41 84.2(5) .
C36 C35 C40 C42 -43.1(6) .
C36 C37 C38 C39 -0.1(7) .
C36 C37 C43 C44 -81.7(5) .
C36 C37 C43 C45 153.6(5) .
C37 C38 C39 C34 -1.6(7) .
C37 C38 C39 C46 -178.3(4) .
C38 C37 C43 C44 99.1(5) .
C38 C37 C43 C45 -25.6(6) .
C38 C39 C46 C47 -46.5(5) .
C38 C39 C46 C48 74.6(5) .
C39 C34 C35 C36 -0.1(6) .
C39 C34 C35 C40 180.0(4) .
C39 C34 P1 C27 48.9(4) .
C39 C34 P1 P2 -58.1(4) .
C40 C35 C36 C37 178.3(4) .
C43 C37 C38 C39 179.1(4) .
C49 C50 C51 C52 -1.2(8) .
C49 C50 C55 C56 -126.1(5) .
C49 C50 C55 C57 110.3(5) .
C49 C54 C61 C62 113.4(5) .
C49 C54 C61 C63 -122.6(5) .
C50 C49 C54 C53 0.9(7) .
C50 C49 C54 C61 179.0(4) .
C50 C49 P2 P1 -77.1(4) .
C50 C49 P2 Th1 51.9(5) .
C50 C51 C52 C53 2.9(9) .
C50 C51 C52 C58 -172.5(6) .
C51 C50 C55 C56 57.8(6) .
C51 C50 C55 C57 -65.8(6) .
C51 C52 C53 C54 -2.7(9) .
C51 C52 C58 C59 -56.8(9) .
C51 C52 C58 C60 66.5(9) .
C52 C53 C54 C49 0.9(8) .
C52 C53 C54 C61 -177.3(5) .
C53 C52 C58 C59 128.0(8) .
C53 C52 C58 C60 -108.7(7) .
C53 C54 C61 C62 -68.5(6) .
C53 C54 C61 C63 55.5(6) .
C54 C49 C50 C51 -0.8(7) .
C54 C49 C50 C55 -176.8(4) .
C54 C49 P2 P1 99.7(4) .
C54 C49 P2 Th1 -131.3(3) .
C55 C50 C51 C52 175.1(5) .
C58 C52 C53 C54 172.7(6) .
N1 C27 C28 C29 20.6(6) .
N1 C27 C28 C33 -157.3(4) .
N1 C27 P1 C34 -126.9(3) .
N1 C27 P1 P2 -9.2(3) .
P1 C27 C28 C29 -172.9(3) .
P1 C27 C28 C33 9.3(6) .
P1 C27 N1 Th1 -18.0(7) .
P1 C34 C35 C36 179.4(3) .
P1 C34 C35 C40 -0.5(6) .
P1 C34 C39 C38 -177.8(3) .
P1 C34 C39 C46 -1.3(6) .
P2 C49 C50 C51 176.0(4) .
P2 C49 C50 C55 0.1(7) .
P2 C49 C54 C53 -176.0(4) .
P2 C49 C54 C61 2.0(6) .
Th1 C1 C2 C3 70.2(3) .
Th1 C1 C5 C4 -70.5(3) .
Th1 C1 C6 C7 -178.0(3) .
Th1 C1 C6 C8 -59.6(5) .
Th1 C1 C6 C9 62.9(5) .
Th1 C2 C3 C4 67.8(3) .
Th1 C2 C3 C10 -112.5(4) .
Th1 C3 C4 C5 68.5(3) .
Th1 C3 C10 C11 -23.8(5) .
Th1 C3 C10 C12 -144.1(3) .
Th1 C3 C10 C13 95.0(4) .
Th1 C4 C5 C1 71.3(3) .
Th1 C14 C15 C16 69.4(3) .
Th1 C14 C18 C17 -69.7(3) .
Th1 C14 C19 C20 -160.2(3) .
Th1 C14 C19 C21 -40.0(5) .
Th1 C14 C19 C22 80.9(5) .
Th1 C15 C16 C17 66.2(3) .
Th1 C15 C16 C23 -120.2(5) .
Th1 C16 C17 C18 70.2(3) .
Th1 C16 C23 C24 -85.8(4) .
Th1 C16 C23 C25 36.5(5) .
Th1 C16 C23 C26 155.3(3) .
Th1 C17 C18 C14 71.7(3) .
C70 C71 C72 C72 179.7(11) 3_667
