#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:41:06 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224308 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/87/7048789.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_7048789
loop_
_publ_author_name
'Zhang, Congcong'
'Hou, Guohua'
'Zi, Guofu'
'Walter, Marc D.'
_publ_section_title
;
 A base-free terminal thorium phosphinidene metallocene and its reactivity
 toward selected organic molecules.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2377
_journal_page_last               2387
_journal_paper_doi               10.1039/c9dt00012g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C42 H68 N4 Th'
_chemical_formula_sum            'C42 H68 N4 Th'
_chemical_formula_weight         861.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-12-06 deposited with the CCDC.
2019-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.625(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4503(4)
_cell_length_b                   17.0758(5)
_cell_length_c                   17.6755(5)
_cell_measurement_reflns_used    5951
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.1480
_cell_measurement_theta_min      4.0620
_cell_volume                     4023.7(2)
_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      100.01(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_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_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_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_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.421
_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
_refine_diff_density_max         1.152
_refine_diff_density_min         -2.099
_refine_diff_density_rms         0.139
_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_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0336
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4455
_reflns_number_total             4841
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt00012g2.cif
_cod_data_source_block           compound11
_cod_depositor_comments
'Adding full bibliography for 7048788--7048794.cif.'
_cod_database_code               7048789
_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 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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)
;
_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
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'
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
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
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'
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
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_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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_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
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)
