#------------------------------------------------------------------------------
#$Date: 2025-04-05 05:36:07 +0300 (Sat, 05 Apr 2025) $
#$Revision: 298844 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/25/00/7250047.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_7250047
loop_
_publ_author_name
'Yang, Tian-Shu'
'Duan, Xiao-Fang'
'Yin, Fan'
'Cai, Li-Xuan'
'Zhou, Li-Peng'
'Hu, Shao-Jun'
'Guo, Xiao-Qing'
'Sun, Qing-Fu'
_publ_section_title
;
 Guest-adaptive hydrogen-bonded dimerization of a C3-symmetric
 tribenzotriquinacene molecular bowl
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              2025
_journal_page_last               2032
_journal_paper_doi               10.1039/D5CE00038F
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety
'2(C59 H57 N15 O3), 3.5(C6 H12), 3(C1 H1 Cl3), 2.1[CHCl3], 2.1[CHCl3]'
_chemical_formula_sum            'C146.2 H163.2 Cl21.6 N30 O6'
_chemical_formula_weight         3202.38
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2mbpvj
_audit_creation_date             2025-02-09
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-02-12 deposited with the CCDC.	2025-02-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   22.8874(11)
_cell_length_b                   22.8874(11)
_cell_length_c                   57.200(5)
_cell_measurement_reflns_used    6314
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      66.3210
_cell_measurement_theta_min      2.4190
_cell_volume                     25949(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -53.00 -27.00   0.50    3.50    --  -97.00  54.00-179.00   52
  2  ω    -53.00 -24.00   0.50    3.50    --  -97.00  45.00 -90.00   58
  3  ω    -69.00 -27.00   0.50    3.50    --  -97.00  61.00 -60.00   84
  4  ω    -54.00 -29.00   0.50    3.50    --  -97.00  45.00 -60.00   50
  5  ω    -54.00 -27.00   0.50    3.50    --  -97.00  45.00 120.00   54
  6  ω    -98.00 -39.00   0.50    3.50    --  -97.00 117.00 154.00  118
  7  ω     66.00 114.00   0.50    0.88    --   46.22 141.00  50.00   96
  8  ω    112.00 163.00   0.50    3.50    --  107.47  54.00-179.00  102
  9  ω    -24.00  21.00   0.50    0.88    --   46.22 -19.00 -30.00   90
 10  ω   -118.00 -93.00   0.50    0.88    --  -46.22-141.00  -7.00   50
 11  ω    -28.00  11.00   0.50    0.88    --   46.22 -19.00  60.00   78
 12  ω     40.00  68.00   0.50    3.50    --  107.47-113.00-114.00   56
 13  ω     76.00 108.00   0.50    3.50    --  107.47-113.00-114.00   64
 14  ω     61.00  92.00   0.50    3.50    --  107.47 -95.00 -90.00   62
 15  ω     50.00  79.00   0.50    3.50    --  107.47 -81.00  48.00   58
 16  ω    106.00 133.00   0.50    3.50    --  107.47 -81.00  48.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0159408000
_diffrn_orient_matrix_UB_12      0.0280516000
_diffrn_orient_matrix_UB_13      0.0251292000
_diffrn_orient_matrix_UB_21      -0.0479422667
_diffrn_orient_matrix_UB_22      -0.0711899333
_diffrn_orient_matrix_UB_23      0.0096397667
_diffrn_orient_matrix_UB_31      0.0589909333
_diffrn_orient_matrix_UB_32      -0.0140533333
_diffrn_orient_matrix_UB_33      0.0010913667
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       67
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            29664
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        66.564
_diffrn_reflns_theta_max         66.564
_diffrn_reflns_theta_min         2.359
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.585
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       block
_exptl_crystal_F_000             9994
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.456
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         9828
_refine_ls_number_restraints     390
_refine_ls_restrained_S_all      1.515
_refine_ls_R_factor_all          0.1723
_refine_ls_R_factor_gt           0.1446
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3752
_refine_ls_wR_factor_ref         0.4041
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5921
_reflns_number_total             9828
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5ce00038f2.cif
_cod_data_source_block           CYH
_cod_depositor_comments
'Adding full bibliography for 7250046--7250051.cif.'
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C146.20 H163.20 Cl21.60 N30 O6'
_cod_database_code               7250047
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C H O N Cl'
_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.
;
_shelx_estimated_absorpt_t_max   0.716
_shelx_estimated_absorpt_t_min   0.653
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C45-C44 \\sim C44-C43 \\sim C48-C43 \\sim C48-C47 \\sim C47-C46 \\sim C46-C45
 with sigma of 0.02
 C43-C45 \\sim C44-C46 \\sim C45-C47 \\sim C46-C48 \\sim C47-C43 \\sim C48-C44
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C43A \\sim C44A
\\sim C45A \\sim C46A \\sim C47A \\sim C48A: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 2A
C40 \\sim C41 \\sim C42 \\sim C41A \\sim C42A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C50 \\sim C50A \\sim Cl1 \\sim Cl2 \\sim Cl3 \\sim Cl1A \\sim Cl2A \\sim Cl3A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C19 \\sim C20 \\sim C21 \\sim C20A \\sim C21A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
4. Same fragment restrains
{C19, C20A, C21A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C19, C20, C21}
{C40, C41A, C42A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C40, C41, C42}
{C43A, C44A, C45A, C46A, C47A, C48A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C43, C44, C45, C46, C47, C48}
{C50A, Cl1A, Cl2A, Cl3A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C50, Cl1, Cl2, Cl3}
5. Others
 Sof(H19A)=Sof(H40A)=Sof(C43A)=Sof(H43C)=Sof(H43D)=Sof(C44A)=Sof(H44C)=
 Sof(H44D)=Sof(C45A)=Sof(H45C)=Sof(H45D)=Sof(C46A)=Sof(H46C)=Sof(H46D)=
 Sof(C47A)=Sof(H47C)=Sof(H47D)=Sof(C48A)=Sof(H48C)=Sof(H48D)=Sof(C49A)=
 Sof(H49C)=Sof(H49D)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21A)=
 Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=
 Sof(C42A)=Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(1)
 Sof(H19)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=Sof(H21B)=
 Sof(H21C)=Sof(H40)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42A)=
 Sof(H42B)=Sof(H42C)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C47)=Sof(H47A)=
 Sof(H47B)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C49)=Sof(H49A)=Sof(H49B)=FVAR(1)
 Sof(C50A)=Sof(H50A)=Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3A)=1-FVAR(2)
 Sof(C50)=Sof(H50)=Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=FVAR(2)
 Fixed Sof: H1A(0.33333) H1B(0.33333) H1C(0.33333) H22A(0.33333) H22B(0.33333)
 H22C(0.33333)
6.a Ternary CH refined with riding coordinates:
 C19(H19), C19(H19A), C40(H40), C40(H40A), C50(H50), C50A(H50A)
6.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,
 H47B), C48(H48A,H48B), C49(H49A,H49B), C43A(H43C,H43D), C44A(H44C,H44D),
 C45A(H45C,H45D), C46A(H46C,H46D), C47A(H47C,H47D), C48A(H48C,H48D), C49A(H49C,
 H49D)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C11(H11), C15(H15), C16(H16), C17(H17), N5(H5),
 C27(H27), C28(H28), C30(H30), C32(H32), C36(H36), C37(H37), C38(H38), N10(H10)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C),
 C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C20A(H20D,H20E,H20F), C21A(H21D,H21E,H21F), C41A(H41D,H41E,H41F),
 C42A(H42D,H42E,H42F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1440 electrons were 
found in a volume of 6405Å³ in 2 voids per unit cell. 
This is consistent with the presence of 
2.1[CHCl3], 2.1[CHCl3] per Asymmetric Unit 
which account for 1462 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 2.338
_oxdiff_exptl_absorpt_empirical_full_min 0.336
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.666667 0.333333 0.20994(13) 0.101(2) Uani 1 3 d S T P . .
H1A H 0.661617 0.370940 0.204228 0.151 Uiso 0.3333 1 calc R U P A -1
H1B H 0.629060 0.290676 0.204228 0.151 Uiso 0.3333 1 calc R U P A -1
H1C H 0.709324 0.338383 0.204228 0.151 Uiso 0.3333 1 calc R U P A -1
C2 C 0.666667 0.333333 0.23677(12) 0.0877(17) Uani 1 3 d S T P . .
C3 C 0.7184(2) 0.4050(2) 0.24728(7) 0.0850(10) Uani 1 1 d . . . . .
C4 C 0.7631(2) 0.4614(2) 0.22969(8) 0.0957(11) Uani 1 1 d . . . . .
H4A H 0.791185 0.447909 0.220912 0.144 Uiso 1 1 calc R U . . .
H4B H 0.792073 0.503291 0.238217 0.144 Uiso 1 1 calc R U . . .
H4C H 0.734231 0.468719 0.218829 0.144 Uiso 1 1 calc R U . . .
C5 C 0.67502(19) 0.42412(18) 0.26184(6) 0.0782(9) Uani 1 1 d . . . . .
C6 C 0.6955(2) 0.48420(19) 0.27383(7) 0.0836(10) Uani 1 1 d . . . . .
H6 H 0.739923 0.521169 0.271780 0.100 Uiso 1 1 calc R U . . .
C7 C 0.65125(19) 0.48992(18) 0.28870(7) 0.0821(9) Uani 1 1 d . . . . .
H7 H 0.664330 0.530860 0.296814 0.099 Uiso 1 1 calc R U . . .
C8 C 0.58617(19) 0.43371(19) 0.29159(6) 0.0802(9) Uani 1 1 d . . . . .
C9 C 0.56329(19) 0.37579(19) 0.27857(6) 0.0810(9) Uani 1 1 d . . . . .
H9 H 0.518217 0.339582 0.279969 0.097 Uiso 1 1 calc R U . . .
C10 C 0.60881(19) 0.37223(19) 0.26323(6) 0.0788(9) Uani 1 1 d . . . . .
C11 C 0.56180(19) 0.47878(18) 0.32795(7) 0.0783(9) Uani 1 1 d . . . . .
H11 H 0.604376 0.517700 0.330837 0.094 Uiso 1 1 calc R U . . .
C12 C 0.5052(2) 0.45372(19) 0.34141(7) 0.0831(10) Uani 1 1 d . . . . .
C13 C 0.4953(2) 0.47785(19) 0.36386(7) 0.0800(9) Uani 1 1 d . . . . .
C14 C 0.5411(2) 0.5500(2) 0.39454(7) 0.0891(11) Uani 1 1 d . . . . .
C15 C 0.4832(3) 0.5231(3) 0.40607(9) 0.1088(14) Uani 1 1 d . . . . .
H15 H 0.480662 0.540470 0.420882 0.131 Uiso 1 1 calc R U . . .
C16 C 0.4260(3) 0.4690(3) 0.39616(10) 0.1174(15) Uani 1 1 d . . . . .
H16 H 0.384034 0.448941 0.404186 0.141 Uiso 1 1 calc R U . . .
C17 C 0.4309(3) 0.4452(2) 0.37486(9) 0.0996(12) Uani 1 1 d . . . . .
H17 H 0.392977 0.408378 0.367652 0.120 Uiso 1 1 calc R U . . .
C18 C 0.6027(3) 0.6110(2) 0.40421(8) 0.0997(13) Uani 1 1 d . . . . .
C19 C 0.7234(3) 0.6918(3) 0.40058(11) 0.1246(17) Uani 1 1 d D U . . .
H19 H 0.723362 0.700082 0.417735 0.149 Uiso 0.576(8) 1 calc R U P B 1
H19A H 0.713561 0.709710 0.415067 0.149 Uiso 0.424(8) 1 calc R U P B 2
C20 C 0.7843(7) 0.6853(8) 0.3942(3) 0.146(5) Uani 0.576(8) 1 d D U P B 1
H20A H 0.786874 0.682576 0.377144 0.219 Uiso 0.576(8) 1 calc R U P B 1
H20B H 0.779864 0.644278 0.401290 0.219 Uiso 0.576(8) 1 calc R U P B 1
H20C H 0.825374 0.724695 0.399970 0.219 Uiso 0.576(8) 1 calc R U P B 1
C21 C 0.7283(8) 0.7502(8) 0.3870(3) 0.121(4) Uani 0.576(8) 1 d D U P B 1
H21A H 0.769196 0.791786 0.391645 0.181 Uiso 0.576(8) 1 calc R U P B 1
H21B H 0.688644 0.754606 0.390199 0.181 Uiso 0.576(8) 1 calc R U P B 1
H21C H 0.730402 0.742472 0.370226 0.181 Uiso 0.576(8) 1 calc R U P B 1
N1 N 0.54411(15) 0.43629(15) 0.30967(5) 0.0785(8) Uani 1 1 d . . . . .
N2 N 0.47889(17) 0.38721(18) 0.31152(6) 0.0926(9) Uani 1 1 d . . . . .
N3 N 0.45522(17) 0.39725(17) 0.33081(6) 0.0909(9) Uani 1 1 d . . . . .
N4 N 0.54880(18) 0.52845(16) 0.37314(6) 0.0847(8) Uani 1 1 d . . . . .
N5 N 0.6609(2) 0.63139(18) 0.39386(7) 0.1028(11) Uani 1 1 d . . . . .
H5 H 0.662314 0.607185 0.382145 0.123 Uiso 1 1 calc R U . . .
O1 O 0.5960(2) 0.63827(19) 0.42211(7) 0.1245(11) Uani 1 1 d . . . . .
C22 C 0.333333 0.666667 0.28995(19) 0.139(4) Uani 1 3 d S T P . .
H22A H 0.311822 0.691725 0.284234 0.209 Uiso 0.3333 1 calc R U P C -1
H22B H 0.308275 0.620097 0.284234 0.209 Uiso 0.3333 1 calc R U P C -1
H22C H 0.379903 0.688178 0.284234 0.209 Uiso 0.3333 1 calc R U P C -1
C23 C 0.333333 0.666667 0.31775(18) 0.117(3) Uani 1 3 d S T P . .
C24 C 0.3491(3) 0.6123(3) 0.32782(10) 0.1124(14) Uani 1 1 d . . . . .
C25 C 0.3602(3) 0.5681(3) 0.31016(12) 0.1346(19) Uani 1 1 d . . . . .
H25A H 0.317136 0.536251 0.302858 0.202 Uiso 1 1 calc R U . . .
H25B H 0.378609 0.543116 0.318277 0.202 Uiso 1 1 calc R U . . .
H25C H 0.392080 0.596854 0.298096 0.202 Uiso 1 1 calc R U . . .
C26 C 0.4117(3) 0.6540(3) 0.34274(10) 0.1091(13) Uani 1 1 d . . . . .
C27 C 0.4480(3) 0.6301(3) 0.35570(11) 0.1175(15) Uani 1 1 d . . . . .
H27 H 0.437512 0.584467 0.354382 0.141 Uiso 1 1 calc R U . . .
C28 C 0.4982(3) 0.6737(3) 0.37011(13) 0.1298(18) Uani 1 1 d . . . . .
H28 H 0.522758 0.658348 0.379127 0.156 Uiso 1 1 calc R U . . .
C29 C 0.5136(3) 0.7401(3) 0.37170(12) 0.1208(16) Uani 1 1 d . . . . .
C30 C 0.4827(3) 0.7650(3) 0.35784(11) 0.1141(15) Uani 1 1 d . . . . .
H30 H 0.496896 0.811771 0.357981 0.137 Uiso 1 1 calc R U . . .
C31 C 0.4306(3) 0.7212(3) 0.34365(10) 0.1086(13) Uani 1 1 d . . . . .
C32 C 0.5837(3) 0.7686(3) 0.40800(12) 0.1216(16) Uani 1 1 d . . . . .
H32 H 0.572806 0.724853 0.413139 0.146 Uiso 1 1 calc R U . . .
C33 C 0.6237(4) 0.8273(3) 0.41837(16) 0.149(3) Uani 1 1 d . . . . .
C34 C 0.6559(4) 0.8392(3) 0.44184(15) 0.144(2) Uani 1 1 d . . . . .
C35 C 0.6756(3) 0.7915(3) 0.47375(12) 0.1242(18) Uani 1 1 d . . . . .
C36 C 0.7063(4) 0.8517(5) 0.48512(16) 0.164(3) Uani 1 1 d . . . . .
H36 H 0.723868 0.855332 0.500424 0.196 Uiso 1 1 calc R U . . .
C37 C 0.7114(6) 0.9090(5) 0.4737(3) 0.204(5) Uani 1 1 d . . . . .
H37 H 0.732664 0.951675 0.481223 0.245 Uiso 1 1 calc R U . . .
C38 C 0.6867(5) 0.9028(4) 0.4525(2) 0.181(4) Uani 1 1 d . . . . .
H38 H 0.689585 0.940673 0.444635 0.217 Uiso 1 1 calc R U . . .
C39 C 0.6698(3) 0.7306(3) 0.48452(11) 0.1196(17) Uani 1 1 d . . . . .
C40 C 0.6423(5) 0.6137(4) 0.47903(14) 0.155(2) Uani 1 1 d D U . . .
H40 H 0.655547 0.619112 0.495893 0.186 Uiso 0.576(8) 1 calc R U P B 1
H40A H 0.642475 0.611214 0.496482 0.186 Uiso 0.424(8) 1 calc R U P B 2
C41 C 0.6878(8) 0.5939(10) 0.4662(4) 0.160(5) Uani 0.576(8) 1 d D U P B 1
H41A H 0.696353 0.564049 0.476062 0.240 Uiso 0.576(8) 1 calc R U P B 1
H41B H 0.730688 0.634562 0.462438 0.240 Uiso 0.576(8) 1 calc R U P B 1
H41C H 0.665801 0.570416 0.451655 0.240 Uiso 0.576(8) 1 calc R U P B 1
C42 C 0.5682(7) 0.5570(12) 0.4776(4) 0.198(8) Uani 0.576(8) 1 d D U P B 1
H42A H 0.556503 0.543021 0.461239 0.297 Uiso 0.576(8) 1 calc R U P B 1
H42B H 0.538990 0.573521 0.483582 0.297 Uiso 0.576(8) 1 calc R U P B 1
H42C H 0.561881 0.518438 0.486933 0.297 Uiso 0.576(8) 1 calc R U P B 1
N6 N 0.5625(3) 0.7847(2) 0.38905(11) 0.1352(17) Uani 1 1 d . . . . .
N7 N 0.5866(4) 0.8499(3) 0.38715(15) 0.179(3) Uani 1 1 d . . . . .
N8 N 0.6232(4) 0.8758(3) 0.40573(18) 0.192(3) Uani 1 1 d . . . . .
N9 N 0.6512(2) 0.7845(2) 0.45209(10) 0.1224(15) Uani 1 1 d . . . . .
N10 N 0.6449(3) 0.6753(2) 0.47173(8) 0.1189(13) Uani 1 1 d . . . . .
H10 H 0.628803 0.676074 0.457835 0.143 Uiso 1 1 calc R U . . .
O2 O 0.6908(2) 0.7336(3) 0.50540(8) 0.1423(14) Uani 1 1 d . . . . .
C43 C 0.6330(7) 0.7354(6) 0.3218(2) 0.205(6) Uani 0.576(8) 1 d D U P B 1
H43A H 0.673863 0.758926 0.311885 0.246 Uiso 0.576(8) 1 calc R U P B 1
H43B H 0.645351 0.754929 0.337652 0.246 Uiso 0.576(8) 1 calc R U P B 1
C44 C 0.6132(4) 0.6631(4) 0.32311(16) 0.115(3) Uani 0.576(8) 1 d D U P B 1
H44A H 0.588634 0.644333 0.337947 0.138 Uiso 0.576(8) 1 calc R U P B 1
H44B H 0.654690 0.659737 0.323585 0.138 Uiso 0.576(8) 1 calc R U P B 1
C45 C 0.5698(9) 0.6206(6) 0.3032(2) 0.130(4) Uani 0.576(8) 1 d D U P B 1
H45A H 0.591838 0.597243 0.295985 0.156 Uiso 0.576(8) 1 calc R U P B 1
H45B H 0.526051 0.585534 0.309680 0.156 Uiso 0.576(8) 1 calc R U P B 1
C46 C 0.5565(8) 0.6578(7) 0.2847(2) 0.174(4) Uani 0.576(8) 1 d D U P B 1
H46A H 0.589692 0.666946 0.272103 0.209 Uiso 0.576(8) 1 calc R U P B 1
H46B H 0.511568 0.626087 0.278150 0.209 Uiso 0.576(8) 1 calc R U P B 1
C47 C 0.5574(8) 0.7200(6) 0.2890(3) 0.147(4) Uani 0.576(8) 1 d D U P B 1
H47A H 0.511219 0.712145 0.286587 0.177 Uiso 0.576(8) 1 calc R U P B 1
H47B H 0.586861 0.753262 0.277160 0.177 Uiso 0.576(8) 1 calc R U P B 1
C48 C 0.5804(7) 0.7500(5) 0.31215(19) 0.125(3) Uani 0.576(8) 1 d D U P B 1
H48A H 0.541395 0.731858 0.322965 0.150 Uiso 0.576(8) 1 calc R U P B 1
H48B H 0.599464 0.799474 0.311095 0.150 Uiso 0.576(8) 1 calc R U P B 1
C49 C 0.6475(6) 0.3961(6) 0.33557(16) 0.061(3) Uani 0.576(8) 1 d . . P B 1
H49A H 0.643704 0.408340 0.351871 0.073 Uiso 0.576(8) 1 calc R U P B 1
H49B H 0.638504 0.425326 0.325201 0.073 Uiso 0.576(8) 1 calc R U P B 1
C50 C 0.5919(7) 0.6984(6) 0.5440(3) 0.160(4) Uani 0.488(6) 1 d D U P D 1
H50 H 0.636139 0.717705 0.535725 0.192 Uiso 0.488(6) 1 calc R U P D 1
Cl1 Cl 0.5653(8) 0.6150(4) 0.5505(2) 0.203(4) Uani 0.488(6) 1 d D U P D 1
Cl2 Cl 0.5326(3) 0.6999(3) 0.52458(11) 0.193(2) Uani 0.488(6) 1 d D U P D 1
Cl3 Cl 0.6013(4) 0.7478(4) 0.56651(11) 0.231(4) Uani 0.488(6) 1 d D U P D 1
C43A C 0.5977(7) 0.6953(7) 0.3064(3) 0.166(4) Uani 0.424(8) 1 d D U P B 2
H43C H 0.633309 0.709658 0.294336 0.199 Uiso 0.424(8) 1 calc R U P B 2
H43D H 0.619694 0.716265 0.321414 0.199 Uiso 0.424(8) 1 calc R U P B 2
C44A C 0.5615(10) 0.6192(7) 0.3088(3) 0.132(5) Uani 0.424(8) 1 d D U P B 2
H44C H 0.595080 0.604654 0.311444 0.158 Uiso 0.424(8) 1 calc R U P B 2
H44D H 0.531332 0.605528 0.322586 0.158 Uiso 0.424(8) 1 calc R U P B 2
C45A C 0.5210(7) 0.5850(6) 0.2875(2) 0.142(4) Uani 0.424(8) 1 d D U P B 2
H45C H 0.473982 0.553266 0.292383 0.171 Uiso 0.424(8) 1 calc R U P B 2
H45D H 0.539251 0.558049 0.280378 0.171 Uiso 0.424(8) 1 calc R U P B 2
C46A C 0.5200(12) 0.6315(9) 0.2694(3) 0.209(7) Uani 0.424(8) 1 d D U P B 2
H46C H 0.554758 0.638391 0.257722 0.250 Uiso 0.424(8) 1 calc R U P B 2
H46D H 0.475882 0.606469 0.261368 0.250 Uiso 0.424(8) 1 calc R U P B 2
C47A C 0.5296(6) 0.6959(7) 0.2746(2) 0.125(4) Uani 0.424(8) 1 d D U P B 2
H47C H 0.487602 0.696059 0.270520 0.150 Uiso 0.424(8) 1 calc R U P B 2
H47D H 0.565702 0.729085 0.264315 0.150 Uiso 0.424(8) 1 calc R U P B 2
C48A C 0.5475(7) 0.7202(7) 0.2994(2) 0.104(3) Uani 0.424(8) 1 d D U P B 2
H48C H 0.507110 0.699923 0.309568 0.125 Uiso 0.424(8) 1 calc R U P B 2
H48D H 0.569526 0.769981 0.300292 0.125 Uiso 0.424(8) 1 calc R U P B 2
C49A C 0.6272(10) 0.3732(8) 0.3392(2) 0.063(4) Uani 0.424(8) 1 d . . P B 2
H49C H 0.603071 0.397513 0.334970 0.076 Uiso 0.424(8) 1 calc R U P B 2
H49D H 0.629228 0.371117 0.356416 0.076 Uiso 0.424(8) 1 calc R U P B 2
C50A C 0.6029(7) 0.6967(6) 0.5508(2) 0.152(3) Uani 0.512(6) 1 d D U P D 2
H50A H 0.637608 0.712867 0.538164 0.183 Uiso 0.512(6) 1 calc R U P D 2
Cl1A Cl 0.5476(6) 0.6111(4) 0.5469(2) 0.182(3) Uani 0.512(6) 1 d D U P D 2
Cl2A Cl 0.5551(2) 0.7375(2) 0.54783(11) 0.170(2) Uani 0.512(6) 1 d D U P D 2
Cl3A Cl 0.64225(19) 0.7185(2) 0.57658(6) 0.1488(15) Uani 0.512(6) 1 d D U P D 2
C20A C 0.7730(9) 0.6713(9) 0.4070(3) 0.123(5) Uani 0.424(8) 1 d D U P B 2
H20D H 0.781278 0.649915 0.393564 0.185 Uiso 0.424(8) 1 calc R U P B 2
H20E H 0.755331 0.639196 0.420043 0.185 Uiso 0.424(8) 1 calc R U P B 2
H20F H 0.815356 0.711133 0.411753 0.185 Uiso 0.424(8) 1 calc R U P B 2
C21A C 0.7454(10) 0.7444(9) 0.3829(3) 0.115(4) Uani 0.424(8) 1 d D U P B 2
H21D H 0.781902 0.786868 0.389212 0.173 Uiso 0.424(8) 1 calc R U P B 2
H21E H 0.707419 0.750459 0.378418 0.173 Uiso 0.424(8) 1 calc R U P B 2
H21F H 0.761738 0.731428 0.369098 0.173 Uiso 0.424(8) 1 calc R U P B 2
C41A C 0.7057(8) 0.6163(12) 0.4691(6) 0.144(5) Uani 0.424(8) 1 d D U P B 2
H41D H 0.704431 0.573690 0.472382 0.216 Uiso 0.424(8) 1 calc R U P B 2
H41E H 0.745797 0.653610 0.476319 0.216 Uiso 0.424(8) 1 calc R U P B 2
H41F H 0.707336 0.623299 0.452122 0.216 Uiso 0.424(8) 1 calc R U P B 2
C42A C 0.5795(8) 0.5504(11) 0.4690(5) 0.156(6) Uani 0.424(8) 1 d D U P B 2
H42D H 0.575245 0.557019 0.452294 0.234 Uiso 0.424(8) 1 calc R U P B 2
H42E H 0.538949 0.543597 0.477214 0.234 Uiso 0.424(8) 1 calc R U P B 2
H42F H 0.584571 0.510725 0.471178 0.234 Uiso 0.424(8) 1 calc R U P B 2
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'
Cl Cl 0.3639 0.7018 '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'
O O 0.0492 0.0322 '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
_geom_angle_publ_flag
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C1 C2 C3 112.3(3) . . ?
C1 C2 C3 112.3(3) . 2_655 ?
C1 C2 C3 112.3(3) . 3_665 ?
C3 C2 C3 106.5(3) 3_665 2_655 ?
C3 C2 C3 106.5(3) 3_665 . ?
C3 C2 C3 106.5(3) . 2_655 ?
C4 C3 C2 117.1(4) . . ?
C5 C3 C2 104.4(3) . . ?
C5 C3 C4 111.7(3) . . ?
C5 C3 C10 109.8(3) . 3_665 ?
C10 C3 C2 104.2(3) 3_665 . ?
C10 C3 C4 109.2(3) 3_665 . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C3 127.5(4) . . ?
C10 C5 C3 112.2(3) . . ?
C10 C5 C6 120.2(4) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 C5 119.8(4) . . ?
C7 C6 H6 120.1 . . ?
C6 C7 H7 120.7 . . ?
C6 C7 C8 118.5(3) . . ?
C8 C7 H7 120.7 . . ?
C7 C8 N1 118.2(3) . . ?
C9 C8 C7 122.4(4) . . ?
C9 C8 N1 119.4(4) . . ?
C8 C9 H9 121.3 . . ?
C8 C9 C10 117.5(4) . . ?
C10 C9 H9 121.3 . . ?
C5 C10 C3 112.3(3) . 2_655 ?
C5 C10 C9 121.0(3) . . ?
C9 C10 C3 126.7(4) . 2_655 ?
C12 C11 H11 127.6 . . ?
N1 C11 H11 127.6 . . ?
N1 C11 C12 104.8(3) . . ?
C11 C12 C13 129.3(4) . . ?
C11 C12 N3 108.5(4) . . ?
N3 C12 C13 122.2(4) . . ?
C17 C13 C12 120.5(4) . . ?
N4 C13 C12 116.0(3) . . ?
N4 C13 C17 123.5(4) . . ?
C15 C14 C18 120.1(4) . . ?
C15 C14 N4 124.0(4) . . ?
N4 C14 C18 115.8(4) . . ?
C14 C15 H15 120.4 . . ?
C14 C15 C16 119.1(5) . . ?
C16 C15 H15 120.4 . . ?
C15 C16 H16 120.4 . . ?
C17 C16 C15 119.3(5) . . ?
C17 C16 H16 120.4 . . ?
C13 C17 H17 121.4 . . ?
C16 C17 C13 117.2(5) . . ?
C16 C17 H17 121.4 . . ?
N5 C18 C14 118.5(4) . . ?
O1 C18 C14 118.3(5) . . ?
O1 C18 N5 123.2(5) . . ?
C20 C19 H19 110.2 . . ?
C21 C19 H19 110.2 . . ?
C21 C19 C20 107.4(9) . . ?
N5 C19 H19 110.2 . . ?
N5 C19 H19A 106.9 . . ?
N5 C19 C20 110.9(7) . . ?
N5 C19 C21 108.0(9) . . ?
N5 C19 C20A 108.1(8) . . ?
C20A C19 H19A 106.9 . . ?
C21A C19 H19A 106.9 . . ?
C21A C19 N5 111.7(11) . . ?
C21A C19 C20A 115.7(11) . . ?
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 . . ?
C11 N1 C8 128.7(3) . . ?
C11 N1 N2 110.4(3) . . ?
N2 N1 C8 120.5(3) . . ?
N3 N2 N1 107.7(3) . . ?
N2 N3 C12 108.5(3) . . ?
C13 N4 C14 116.9(4) . . ?
C18 N5 C19 124.0(4) . . ?
C18 N5 H5 118.0 . . ?
C19 N5 H5 118.0 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
C23 C22 H22C 109.5 . . ?
C24 C23 C22 111.5(4) 3_565 . ?
C24 C23 C22 111.5(4) 2_665 . ?
C24 C23 C22 111.5(4) . . ?
C24 C23 C24 107.3(4) 3_565 . ?
C24 C23 C24 107.3(4) 2_665 . ?
C24 C23 C24 107.3(4) 3_565 2_665 ?
C25 C24 C23 117.4(6) . . ?
C26 C24 C23 103.0(4) . . ?
C26 C24 C25 111.5(5) . . ?
C31 C24 C23 104.8(4) 3_565 . ?
C31 C24 C25 110.6(5) 3_565 . ?
C31 C24 C26 108.8(4) 3_565 . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C24 126.9(5) . . ?
C31 C26 C24 113.2(5) . . ?
C31 C26 C27 119.8(5) . . ?
C26 C27 H27 120.7 . . ?
C28 C27 C26 118.6(5) . . ?
C28 C27 H27 120.7 . . ?
C27 C28 H28 119.8 . . ?
C27 C28 C29 120.3(5) . . ?
C29 C28 H28 119.8 . . ?
C28 C29 N6 119.9(5) . . ?
C30 C29 C28 121.5(6) . . ?
C30 C29 N6 118.6(5) . . ?
C29 C30 H30 120.7 . . ?
C29 C30 C31 118.7(5) . . ?
C31 C30 H30 120.7 . . ?
C26 C31 C24 111.4(5) . 2_665 ?
C26 C31 C30 120.8(5) . . ?
C30 C31 C24 127.8(5) . 2_665 ?
C33 C32 H32 127.7 . . ?
N6 C32 H32 127.7 . . ?
N6 C32 C33 104.5(5) . . ?
C32 C33 C34 128.1(6) . . ?
C32 C33 N8 108.1(6) . . ?
N8 C33 C34 123.1(6) . . ?
C38 C34 C33 122.1(7) . . ?
N9 C34 C33 114.9(5) . . ?
N9 C34 C38 122.9(7) . . ?
C36 C35 C39 121.2(7) . . ?
N9 C35 C36 122.5(7) . . ?
N9 C35 C39 116.2(5) . . ?
C35 C36 H36 120.7 . . ?
C35 C36 C37 118.6(8) . . ?
C37 C36 H36 120.7 . . ?
C36 C37 H37 120.2 . . ?
C38 C37 C36 119.6(7) . . ?
C38 C37 H37 120.2 . . ?
C34 C38 H38 120.6 . . ?
C37 C38 C34 118.8(8) . . ?
C37 C38 H38 120.6 . . ?
N10 C39 C35 117.9(5) . . ?
O2 C39 C35 119.3(5) . . ?
O2 C39 N10 122.8(6) . . ?
C41 C40 H40 107.2 . . ?
C41 C40 C42 110.8(12) . . ?
C42 C40 H40 107.2 . . ?
N10 C40 H40 107.2 . . ?
N10 C40 H40A 110.1 . . ?
N10 C40 C41 116.9(12) . . ?
N10 C40 C42 107.3(13) . . ?
N10 C40 C41A 106.2(13) . . ?
N10 C40 C42A 111.8(12) . . ?
C41A C40 H40A 110.1 . . ?
C41A C40 C42A 108.5(11) . . ?
C42A C40 H40A 110.1 . . ?
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 . . ?
C32 N6 C29 128.7(5) . . ?
N7 N6 C29 118.6(5) . . ?
N7 N6 C32 112.5(6) . . ?
N8 N7 N6 105.1(6) . . ?
N7 N8 C33 109.7(6) . . ?
C35 N9 C34 117.5(5) . . ?
C39 N10 C40 124.3(5) . . ?
C39 N10 H10 117.8 . . ?
C40 N10 H10 117.8 . . ?
H43A C43 H43B 107.4 . . ?
C44 C43 H43A 108.3 . . ?
C44 C43 H43B 108.3 . . ?
C44 C43 C48 115.8(8) . . ?
C48 C43 H43A 108.3 . . ?
C48 C43 H43B 108.3 . . ?
C43 C44 H44A 108.6 . . ?
C43 C44 H44B 108.6 . . ?
C43 C44 C45 114.6(7) . . ?
H44A C44 H44B 107.6 . . ?
C45 C44 H44A 108.6 . . ?
C45 C44 H44B 108.6 . . ?
C44 C45 H45A 108.4 . . ?
C44 C45 H45B 108.4 . . ?
H45A C45 H45B 107.5 . . ?
C46 C45 C44 115.3(8) . . ?
C46 C45 H45A 108.4 . . ?
C46 C45 H45B 108.4 . . ?
C45 C46 H46A 106.6 . . ?
C45 C46 H46B 106.6 . . ?
H46A C46 H46B 106.6 . . ?
C47 C46 C45 122.8(9) . . ?
C47 C46 H46A 106.6 . . ?
C47 C46 H46B 106.6 . . ?
C46 C47 H47A 108.2 . . ?
C46 C47 H47B 108.2 . . ?
C46 C47 C48 116.5(7) . . ?
H47A C47 H47B 107.3 . . ?
C48 C47 H47A 108.2 . . ?
C48 C47 H47B 108.2 . . ?
C43 C48 H48A 109.4 . . ?
C43 C48 H48B 109.4 . . ?
C47 C48 C43 111.4(7) . . ?
C47 C48 H48A 109.4 . . ?
C47 C48 H48B 109.4 . . ?
H48A C48 H48B 108.0 . . ?
C49 C49 C49 117.8(3) 18_545 17 ?
C49 C49 H49A 107.9 18_545 . ?
C49 C49 H49A 107.9 17 . ?
C49 C49 H49B 107.9 17 . ?
C49 C49 H49B 107.9 18_545 . ?
H49A C49 H49B 107.2 . . ?
Cl1 C50 H50 108.0 . . ?
Cl1 C50 Cl2 107.8(8) . . ?
Cl2 C50 H50 108.0 . . ?
Cl3 C50 H50 108.0 . . ?
Cl3 C50 Cl1 116.3(10) . . ?
Cl3 C50 Cl2 108.3(7) . . ?
H43C C43A H43D 108.0 . . ?
C44A C43A H43C 109.4 . . ?
C44A C43A H43D 109.4 . . ?
C44A C43A C48A 111.2(10) . . ?
C48A C43A H43C 109.4 . . ?
C48A C43A H43D 109.4 . . ?
C43A C44A H44C 109.3 . . ?
C43A C44A H44D 109.3 . . ?
H44C C44A H44D 108.0 . . ?
C45A C44A C43A 111.6(9) . . ?
C45A C44A H44C 109.3 . . ?
C45A C44A H44D 109.3 . . ?
C44A C45A H45C 108.6 . . ?
C44A C45A H45D 108.6 . . ?
C44A C45A C46A 114.7(10) . . ?
H45C C45A H45D 107.6 . . ?
C46A C45A H45C 108.6 . . ?
C46A C45A H45D 108.6 . . ?
C45A C46A H46C 106.5 . . ?
C45A C46A H46D 106.5 . . ?
H46C C46A H46D 106.5 . . ?
C47A C46A C45A 123.3(11) . . ?
C47A C46A H46C 106.5 . . ?
C47A C46A H46D 106.5 . . ?
C46A C47A H47C 108.0 . . ?
C46A C47A H47D 108.0 . . ?
C46A C47A C48A 117.2(9) . . ?
H47C C47A H47D 107.2 . . ?
C48A C47A H47C 108.0 . . ?
C48A C47A H47D 108.0 . . ?
C43A C48A H48C 111.2 . . ?
C43A C48A H48D 111.2 . . ?
C47A C48A C43A 102.8(8) . . ?
C47A C48A H48C 111.2 . . ?
C47A C48A H48D 111.2 . . ?
H48C C48A H48D 109.1 . . ?
C49A C49A C49A 105.7(8) 17 18_545 ?
C49A C49A H49C 110.6 17 . ?
C49A C49A H49C 110.6 18_545 . ?
C49A C49A H49D 110.6 18_545 . ?
C49A C49A H49D 110.6 17 . ?
H49C C49A H49D 108.7 . . ?
Cl1A C50A H50A 108.7 . . ?
Cl1A C50A Cl2A 106.8(8) . . ?
Cl2A C50A H50A 108.7 . . ?
Cl3A C50A H50A 108.7 . . ?
Cl3A C50A Cl1A 115.6(9) . . ?
Cl3A C50A Cl2A 108.3(6) . . ?
C19 C20A H20D 109.5 . . ?
C19 C20A H20E 109.5 . . ?
C19 C20A H20F 109.5 . . ?
H20D C20A H20E 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
C19 C21A H21D 109.5 . . ?
C19 C21A H21E 109.5 . . ?
C19 C21A H21F 109.5 . . ?
H21D C21A H21E 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?
C40 C41A H41D 109.5 . . ?
C40 C41A H41E 109.5 . . ?
C40 C41A H41F 109.5 . . ?
H41D C41A H41E 109.5 . . ?
H41D C41A H41F 109.5 . . ?
H41E C41A H41F 109.5 . . ?
C40 C42A H42D 109.5 . . ?
C40 C42A H42E 109.5 . . ?
C40 C42A H42F 109.5 . . ?
H42D C42A H42E 109.5 . . ?
H42D C42A H42F 109.5 . . ?
H42E C42A H42F 109.5 . . ?
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 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.535(11) . ?
C2 C3 1.585(5) 3_665 ?
C2 C3 1.585(5) . ?
C2 C3 1.585(5) 2_655 ?
C3 C4 1.550(6) . ?
C3 C5 1.518(6) . ?
C3 C10 1.523(5) 3_665 ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.391(6) . ?
C5 C10 1.383(6) . ?
C6 H6 0.9500 . ?
C6 C7 1.378(6) . ?
C7 H7 0.9500 . ?
C7 C8 1.409(6) . ?
C8 C9 1.376(5) . ?
C8 N1 1.434(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.395(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.362(6) . ?
C11 N1 1.345(5) . ?
C12 C13 1.460(6) . ?
C12 N3 1.367(5) . ?
C13 C17 1.423(6) . ?
C13 N4 1.306(5) . ?
C14 C15 1.324(7) . ?
C14 C18 1.508(7) . ?
C14 N4 1.363(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.396(8) . ?
C16 H16 0.9500 . ?
C16 C17 1.362(7) . ?
C17 H17 0.9500 . ?
C18 N5 1.313(7) . ?
C18 O1 1.248(6) . ?
C19 H19 1.0000 . ?
C19 H19A 1.0000 . ?
C19 C20 1.517(12) . ?
C19 C21 1.503(11) . ?
C19 N5 1.459(7) . ?
C19 C20A 1.474(12) . ?
C19 C21A 1.458(12) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N1 N2 1.351(5) . ?
N2 N3 1.299(5) . ?
N5 H5 0.8800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C22 C23 1.590(15) . ?
C23 C24 1.568(7) . ?
C23 C24 1.568(7) 2_665 ?
C23 C24 1.568(7) 3_565 ?
C24 C25 1.538(8) . ?
C24 C26 1.525(8) . ?
C24 C31 1.504(7) 3_565 ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.413(8) . ?
C26 C31 1.374(8) . ?
C27 H27 0.9500 . ?
C27 C28 1.359(9) . ?
C28 H28 0.9500 . ?
C28 C29 1.381(8) . ?
C29 C30 1.363(8) . ?
C29 N6 1.462(8) . ?
C30 H30 0.9500 . ?
C30 C31 1.375(8) . ?
C32 H32 0.9500 . ?
C32 C33 1.328(8) . ?
C32 N6 1.313(8) . ?
C33 C34 1.489(11) . ?
C33 N8 1.330(9) . ?
C34 C38 1.400(10) . ?
C34 N9 1.339(8) . ?
C35 C36 1.360(9) . ?
C35 C39 1.467(9) . ?
C35 N9 1.336(8) . ?
C36 H36 0.9500 . ?
C36 C37 1.418(15) . ?
C37 H37 0.9500 . ?
C37 C38 1.311(14) . ?
C38 H38 0.9500 . ?
C39 N10 1.318(7) . ?
C39 O2 1.276(7) . ?
C40 H40 1.0000 . ?
C40 H40A 1.0000 . ?
C40 C41 1.517(15) . ?
C40 C42 1.538(14) . ?
C40 N10 1.444(9) . ?
C40 C41A 1.531(15) . ?
C40 C42A 1.553(15) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
N6 N7 1.311(7) . ?
N7 N8 1.299(10) . ?
N10 H10 0.8800 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.483(11) . ?
C43 C48 1.506(11) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.503(12) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.483(11) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 C47 1.435(11) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.463(11) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C49 1.718(9) 18_545 ?
C49 C49 1.718(9) 17 ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50 1.0000 . ?
C50 Cl1 1.728(11) . ?
C50 Cl2 1.767(14) . ?
C50 Cl3 1.655(14) . ?
C43A H43C 0.9900 . ?
C43A H43D 0.9900 . ?
C43A C44A 1.514(13) . ?
C43A C48A 1.569(13) . ?
C44A H44C 0.9900 . ?
C44A H44D 0.9900 . ?
C44A C45A 1.493(15) . ?
C45A H45C 0.9900 . ?
C45A H45D 0.9900 . ?
C45A C46A 1.495(13) . ?
C46A H46C 0.9900 . ?
C46A H46D 0.9900 . ?
C46A C47A 1.410(13) . ?
C47A H47C 0.9900 . ?
C47A H47D 0.9900 . ?
C47A C48A 1.503(14) . ?
C48A H48C 0.9900 . ?
C48A H48D 0.9900 . ?
C49A C49A 1.708(12) 18_545 ?
C49A C49A 1.708(12) 17 ?
C49A H49C 0.9900 . ?
C49A H49D 0.9900 . ?
C50A H50A 1.0000 . ?
C50A Cl1A 1.736(11) . ?
C50A Cl2A 1.767(14) . ?
C50A Cl3A 1.666(14) . ?
C20A H20D 0.9800 . ?
C20A H20E 0.9800 . ?
C20A H20F 0.9800 . ?
C21A H21D 0.9800 . ?
C21A H21E 0.9800 . ?
C21A H21F 0.9800 . ?
C41A H41D 0.9800 . ?
C41A H41E 0.9800 . ?
C41A H41F 0.9800 . ?
C42A H42D 0.9800 . ?
C42A H42E 0.9800 . ?
C42A H42F 0.9800 . ?
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 -3.6(4) . . . . ?
C1 C2 C3 C5 120.5(2) . . . . ?
C1 C2 C3 C10 -124.3(2) . . . 3_665 ?
C2 C3 C5 C6 -176.4(4) . . . . ?
C2 C3 C5 C10 6.3(4) . . . . ?
C3 C2 C3 C4 119.7(5) 3_665 . . . ?
C3 C2 C3 C4 -126.9(5) 2_655 . . . ?
C3 C2 C3 C5 -116.2(2) 3_665 . . . ?
C3 C2 C3 C5 -2.8(5) 2_655 . . . ?
C3 C2 C3 C10 -1.1(4) 3_665 . . 3_665 ?
C3 C2 C3 C10 112.4(3) 2_655 . . 3_665 ?
C3 C5 C6 C7 -171.6(4) . . . . ?
C3 C5 C10 C3 -7.5(4) . . . 2_655 ?
C3 C5 C10 C9 170.3(3) . . . . ?
C4 C3 C5 C6 -48.9(5) . . . . ?
C4 C3 C5 C10 133.8(3) . . . . ?
C5 C6 C7 C8 1.0(5) . . . . ?
C6 C5 C10 C3 175.0(3) . . . 2_655 ?
C6 C5 C10 C9 -7.2(5) . . . . ?
C6 C7 C8 C9 -6.1(5) . . . . ?
C6 C7 C8 N1 170.5(3) . . . . ?
C7 C8 C9 C10 4.5(5) . . . . ?
C7 C8 N1 C11 -15.8(5) . . . . ?
C7 C8 N1 N2 172.6(3) . . . . ?
C8 C9 C10 C3 179.6(3) . . . 2_655 ?
C8 C9 C10 C5 2.2(5) . . . . ?
C8 N1 N2 N3 172.1(3) . . . . ?
C9 C8 N1 C11 161.0(3) . . . . ?
C9 C8 N1 N2 -10.7(5) . . . . ?
C10 C3 C5 C6 72.4(5) 3_665 . . . ?
C10 C3 C5 C10 -104.8(4) 3_665 . . . ?
C10 C5 C6 C7 5.5(5) . . . . ?
C11 C12 C13 C17 178.2(4) . . . . ?
C11 C12 C13 N4 -4.1(6) . . . . ?
C11 C12 N3 N2 -0.3(4) . . . . ?
C11 N1 N2 N3 -0.9(4) . . . . ?
C12 C11 N1 C8 -171.6(3) . . . . ?
C12 C11 N1 N2 0.7(4) . . . . ?
C12 C13 C17 C16 177.7(4) . . . . ?
C12 C13 N4 C14 -177.5(3) . . . . ?
C13 C12 N3 N2 -178.5(3) . . . . ?
C14 C15 C16 C17 -0.2(8) . . . . ?
C14 C18 N5 C19 176.3(4) . . . . ?
C15 C14 C18 N5 172.0(4) . . . . ?
C15 C14 C18 O1 -5.9(6) . . . . ?
C15 C14 N4 C13 -0.6(6) . . . . ?
C15 C16 C17 C13 -0.2(8) . . . . ?
C17 C13 N4 C14 0.1(5) . . . . ?
C18 C14 C15 C16 176.5(4) . . . . ?
C18 C14 N4 C13 -176.6(3) . . . . ?
C20 C19 N5 C18 153.4(9) . . . . ?
C21 C19 N5 C18 -89.2(8) . . . . ?
N1 C8 C9 C10 -172.1(3) . . . . ?
N1 C11 C12 C13 177.7(3) . . . . ?
N1 C11 C12 N3 -0.3(4) . . . . ?
N1 N2 N3 C12 0.7(4) . . . . ?
N3 C12 C13 C17 -4.0(6) . . . . ?
N3 C12 C13 N4 173.7(3) . . . . ?
N4 C13 C17 C16 0.2(6) . . . . ?
N4 C14 C15 C16 0.6(7) . . . . ?
N4 C14 C18 N5 -11.8(6) . . . . ?
N4 C14 C18 O1 170.3(4) . . . . ?
O1 C18 N5 C19 -6.0(7) . . . . ?
C22 C23 C24 C25 -1.2(5) . . . . ?
C22 C23 C24 C26 121.8(3) . . . . ?
C22 C23 C24 C31 -124.4(3) . . . 3_565 ?
C23 C24 C26 C27 -179.2(6) . . . . ?
C23 C24 C26 C31 3.5(6) . . . . ?
C24 C23 C24 C25 121.3(7) 3_565 . . . ?
C24 C23 C24 C25 -123.7(7) 2_665 . . . ?
C24 C23 C24 C26 -0.7(7) 2_665 . . . ?
C24 C23 C24 C26 -115.8(4) 3_565 . . . ?
C24 C23 C24 C31 113.1(4) 2_665 . . 3_565 ?
C24 C23 C24 C31 -2.0(7) 3_565 . . 3_565 ?
C24 C26 C27 C28 -172.7(6) . . . . ?
C24 C26 C31 C24 -5.1(6) . . . 2_665 ?
C24 C26 C31 C30 174.7(5) . . . . ?
C25 C24 C26 C27 -52.4(7) . . . . ?
C25 C24 C26 C31 130.3(5) . . . . ?
C26 C27 C28 C29 -0.8(10) . . . . ?
C27 C26 C31 C24 177.4(5) . . . 2_665 ?
C27 C26 C31 C30 -2.8(8) . . . . ?
C27 C28 C29 C30 -4.7(11) . . . . ?
C27 C28 C29 N6 173.4(6) . . . . ?
C28 C29 C30 C31 6.4(9) . . . . ?
C28 C29 N6 C32 -19.1(10) . . . . ?
C28 C29 N6 N7 166.2(7) . . . . ?
C29 C30 C31 C24 177.2(6) . . . 2_665 ?
C29 C30 C31 C26 -2.5(8) . . . . ?
C29 N6 N7 N8 174.4(7) . . . . ?
C30 C29 N6 C32 159.1(6) . . . . ?
C30 C29 N6 N7 -15.7(10) . . . . ?
C31 C24 C26 C27 70.0(7) 3_565 . . . ?
C31 C24 C26 C31 -107.4(5) 3_565 . . . ?
C31 C26 C27 C28 4.5(8) . . . . ?
C32 C33 C34 C38 -167.9(9) . . . . ?
C32 C33 C34 N9 10.3(12) . . . . ?
C32 C33 N8 N7 -2.9(12) . . . . ?
C32 N6 N7 N8 -1.2(10) . . . . ?
C33 C32 N6 C29 -175.6(7) . . . . ?
C33 C32 N6 N7 -0.6(9) . . . . ?
C33 C34 C38 C37 177.1(10) . . . . ?
C33 C34 N9 C35 -176.1(6) . . . . ?
C34 C33 N8 N7 -174.2(8) . . . . ?
C35 C36 C37 C38 0.1(16) . . . . ?
C35 C39 N10 C40 173.5(7) . . . . ?
C36 C35 C39 N10 -174.1(6) . . . . ?
C36 C35 C39 O2 3.7(9) . . . . ?
C36 C35 N9 C34 -2.1(10) . . . . ?
C36 C37 C38 C34 -0.2(17) . . . . ?
C38 C34 N9 C35 2.0(11) . . . . ?
C39 C35 C36 C37 178.9(8) . . . . ?
C39 C35 N9 C34 180.0(6) . . . . ?
C41 C40 N10 C39 -111.4(11) . . . . ?
C42 C40 N10 C39 123.6(11) . . . . ?
N6 C29 C30 C31 -171.8(5) . . . . ?
N6 C32 C33 C34 172.7(8) . . . . ?
N6 C32 C33 N8 2.1(9) . . . . ?
N6 N7 N8 C33 2.5(11) . . . . ?
N8 C33 C34 C38 1.6(14) . . . . ?
N8 C33 C34 N9 179.7(8) . . . . ?
N9 C34 C38 C37 -0.9(15) . . . . ?
N9 C35 C36 C37 1.1(12) . . . . ?
N9 C35 C39 N10 3.8(8) . . . . ?
N9 C35 C39 O2 -178.4(5) . . . . ?
O2 C39 N10 C40 -4.2(10) . . . . ?
C43 C44 C45 C46 3.2(18) . . . . ?
C44 C43 C48 C47 -55.6(13) . . . . ?
C44 C45 C46 C47 -26(2) . . . . ?
C45 C46 C47 C48 7(2) . . . . ?
C46 C47 C48 C43 32.3(16) . . . . ?
C48 C43 C44 C45 36.6(16) . . . . ?
C43A C44A C45A C46A -5(2) . . . . ?
C44A C43A C48A C47A -70.0(12) . . . . ?
C44A C45A C46A C47A -26(3) . . . . ?
C45A C46A C47A C48A 5(3) . . . . ?
C46A C47A C48A C43A 39.6(16) . . . . ?
C48A C43A C44A C45A 52.6(17) . . . . ?
C20A C19 N5 C18 121.0(10) . . . . ?
C21A C19 N5 C18 -110.5(9) . . . . ?
C41A C40 N10 C39 -94.7(13) . . . . ?
C42A C40 N10 C39 147.2(13) . . . . ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.209 589.6 120.3 '2.1 CHCl3'
2 0.000 0.000 0.500 955.2 239.7 '4.2 CHCl3'
3 0.000 0.000 0.791 589.6 113.3 '2.1 CHCl3'
4 -0.333 0.333 0.833 955.2 239.7 '4.2 CHCl3'
5 0.333 0.667 0.167 955.2 239.7 '4.2 CHCl3'
6 0.333 0.667 0.458 589.6 113.3 '2.1 CHCl3'
7 0.333 0.667 0.875 589.6 120.3 '2.1 CHCl3'
8 0.667 0.333 0.125 589.6 113.3 '2.1 CHCl3'
9 0.667 0.333 0.542 589.6 120.3 '2.1 CHCl3'
