#------------------------------------------------------------------------------
#$Date: 2023-09-05 22:07:30 +0300 (Tue, 05 Sep 2023) $
#$Revision: 286035 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/93/1569301.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_1569301
loop_
_publ_author_name
'Murillo, Jesse'
'Goodwin, Conrad A. P.'
'Stevens, Lauren'
'Fortier, Skye'
'Gaunt, Andrew J.'
'Scott, Brian L.'
_publ_section_title
;
 Synthesis and comparison of iso-structural f-block metal complexes (Ce,
 U, Np, Pu) featuring η⁶-arene interactions.
;
_journal_issue                   27
_journal_name_full               'Chemical science'
_journal_page_first              7438
_journal_page_last               7446
_journal_paper_doi               10.1039/d3sc02194g
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C50 H66 Cl2 K N2 Np O4, C4 H9 O2'
_chemical_formula_sum            'C54 H75 Cl2 K N2 Np O6'
_chemical_formula_weight         1195.16
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2023-01-27 deposited with the CCDC.	2023-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.882(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9304(14)
_cell_length_b                   12.0060(7)
_cell_length_c                   26.7063(18)
_cell_measurement_reflns_used    11223
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      30.6520
_cell_measurement_theta_min      2.0830
_cell_volume                     5471.4(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      2.26 122.26   0.50   60.00    --   28.00  73.75 -25.74  240
  2  ω      2.26 122.26   0.50   60.00    --   28.00  73.75  64.26  240
  3  ω    -53.74  65.76   0.50   60.00    --  -28.00  73.75 154.26  239
  4  ω    -53.74  65.76   0.50   60.00    --  -28.00  73.75-115.74  239
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0012990000
_diffrn_orient_matrix_UB_12      -0.0116774000
_diffrn_orient_matrix_UB_13      0.0262452000
_diffrn_orient_matrix_UB_21      -0.0344181000
_diffrn_orient_matrix_UB_22      -0.0328375000
_diffrn_orient_matrix_UB_23      -0.0093742000
_diffrn_orient_matrix_UB_31      0.0233492000
_diffrn_orient_matrix_UB_32      -0.0477512000
_diffrn_orient_matrix_UB_33      0.0000230000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0902
_diffrn_reflns_av_unetI/netI     0.0893
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            35831
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         1.876
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.121
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       block
_exptl_crystal_F_000             2428
_exptl_crystal_preparation       'By AJG, JM, CAPG'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.447
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         11123
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0448
_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)+(0.0236P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0883
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8172
_reflns_number_total             11123
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc02194g2.cif
_cod_data_source_block           2_Np
_cod_depositor_comments
'Adding full bibliography for 1569298--1569306.cif.'
_cod_database_code               1569301
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         NpCl2KN2C50O6
_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   0.816
_shelx_estimated_absorpt_t_min   0.676
_reflns_odcompleteness_completeness 99.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C25(H25), C28(H28), C37(H37), C40(H40)
2.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C45(H45A,H45B), C48(H48A,H48B), C49(H49A,H49B), C52(H52A,H52B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17), C21(H21), C22(H22), C23(H23), C33(H33), C34(H34),
  C35(H35), C53(H53)
2.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C43(H43A,H43B,H43C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C54(H54A,H54B,H54C)
;
_lanl_internal_coll_client       CAPG/JM/AJG
_lanl_internal_coll_date         2/4/21
_lanl_internal_coll_frame_method '\w scans'
_lanl_internal_coll_frame_time   60s
_lanl_internal_coll_frame_width  0.5
_lanl_internal_coll_name         ms0486
_lanl_internal_coll_type         custom
_lanl_internal_coll_user         CAPG
_lanl_internal_process_date      2/5/21
_lanl_internal_process_user      CAPG
_lanl_internal_refinement_date   2/6/21
_lanl_internal_refinement_user   CAPG
_lanl_internal_solution_date     2/5/21
_lanl_internal_solution_user     CAPG
_olex2_exptl_crystal_mounting_method
'Coated in NVH oil, mounted insisde a quartz capillary that was sealed at both ends with capillary wax. The outside of the capillary was then coated in Tough As Nails clear nail varnish to provide shatter resistance.'
_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 2.469
_oxdiff_exptl_absorpt_empirical_full_min 0.233
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
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C14 C 0.8892(3) 0.2373(4) 0.28082(17) 0.0251(11) Uani 1 1 d . . . . .
Cl1 Cl 0.68862(8) 0.48087(12) 0.28236(5) 0.0392(3) Uani 1 1 d . . . . .
K1 K 0.58488(7) 0.17413(11) 0.44051(5) 0.0400(3) Uani 1 1 d . . . . .
N2 N 0.8381(2) 0.2275(3) 0.31033(15) 0.0250(9) Uani 1 1 d . . . . .
Np1 Np 0.79116(2) 0.37410(2) 0.35898(2) 0.02311(6) Uani 1 1 d . . . . .
O1 O 0.4403(2) 0.2648(3) 0.39778(15) 0.0477(10) Uani 1 1 d . . . . .
C15 C 0.9013(3) 0.1551(4) 0.24652(19) 0.0336(13) Uani 1 1 d . . . . .
H2 H 0.876268 0.084809 0.244783 0.040 Uiso 1 1 calc R U . . .
Cl2 Cl 0.69840(8) 0.21933(11) 0.38074(5) 0.0380(3) Uani 1 1 d . . . . .
N1 N 0.7790(2) 0.4742(3) 0.43792(14) 0.0247(9) Uani 1 1 d . . . . .
O2 O 0.4805(3) 0.0801(4) 0.34925(15) 0.0502(11) Uani 1 1 d . . . . .
C16 C 0.9489(3) 0.1743(4) 0.21533(18) 0.0320(13) Uani 1 1 d . . . . .
H3 H 0.955837 0.117026 0.192606 0.038 Uiso 1 1 calc R U . . .
O3 O 0.6024(2) 0.0766(3) 0.53770(15) 0.0479(11) Uani 1 1 d . . . . .
C17 C 0.9864(3) 0.2749(5) 0.2166(2) 0.0344(13) Uani 1 1 d . . . . .
H4 H 1.017074 0.288528 0.193844 0.041 Uiso 1 1 calc R U . . .
O4 O 0.6498(2) -0.0375(3) 0.46112(15) 0.0468(10) Uani 1 1 d . . . . .
C18 C 0.9787(3) 0.3549(4) 0.25119(19) 0.0315(12) Uani 1 1 d . . . . .
H5 H 1.005456 0.423816 0.252880 0.038 Uiso 1 1 calc R U . . .
C13 C 0.9326(3) 0.3375(4) 0.28398(18) 0.0266(12) Uani 1 1 d . . . . .
C4 C 0.9271(3) 0.4203(4) 0.32388(18) 0.0262(11) Uani 1 1 d . . . . .
C5 C 0.8849(3) 0.5194(4) 0.31167(19) 0.0294(12) Uani 1 1 d . . . . .
H8 H 0.864442 0.541902 0.275960 0.035 Uiso 1 1 calc R U . . .
C6 C 0.8722(3) 0.5855(4) 0.35083(18) 0.0272(12) Uani 1 1 d . . . . .
H9 H 0.843510 0.652928 0.341688 0.033 Uiso 1 1 calc R U . . .
C1 C 0.9013(3) 0.5539(4) 0.40366(18) 0.0256(11) Uani 1 1 d . . . . .
C2 C 0.9467(3) 0.4566(4) 0.41606(18) 0.0260(11) Uani 1 1 d . . . . .
H11 H 0.969005 0.435745 0.451883 0.031 Uiso 1 1 calc R U . . .
C3 C 0.9595(3) 0.3909(4) 0.37734(17) 0.0247(11) Uani 1 1 d . . . . .
H12 H 0.990331 0.325276 0.386629 0.030 Uiso 1 1 calc R U . . .
C7 C 0.8796(3) 0.6157(4) 0.44551(17) 0.0253(11) Uani 1 1 d . . . . .
C12 C 0.9206(3) 0.7113(4) 0.46862(19) 0.0330(13) Uani 1 1 d . . . . .
H14 H 0.961580 0.739349 0.456516 0.040 Uiso 1 1 calc R U . . .
C11 C 0.9019(3) 0.7651(4) 0.5091(2) 0.0365(13) Uani 1 1 d . . . . .
H15 H 0.929254 0.830348 0.524698 0.044 Uiso 1 1 calc R U . . .
C10 C 0.8429(3) 0.7224(4) 0.52629(19) 0.0336(13) Uani 1 1 d . . . . .
H16 H 0.830190 0.758370 0.554289 0.040 Uiso 1 1 calc R U . . .
C9 C 0.8013(3) 0.6275(4) 0.50364(18) 0.0318(12) Uani 1 1 d . . . . .
H17 H 0.760649 0.600962 0.516421 0.038 Uiso 1 1 calc R U . . .
C8 C 0.8178(3) 0.5700(4) 0.46232(18) 0.0247(11) Uani 1 1 d . . . . .
C31 C 0.8034(3) 0.1172(4) 0.30730(18) 0.0271(11) Uani 1 1 d . . . . .
C32 C 0.8420(3) 0.0359(4) 0.34355(19) 0.0298(12) Uani 1 1 d . . . . .
C33 C 0.8075(4) -0.0699(5) 0.3404(2) 0.0404(14) Uani 1 1 d . . . . .
H21 H 0.833209 -0.126018 0.364712 0.048 Uiso 1 1 calc R U . . .
C34 C 0.7369(4) -0.0945(5) 0.3027(2) 0.0485(16) Uani 1 1 d . . . . .
H22 H 0.714112 -0.166229 0.301527 0.058 Uiso 1 1 calc R U . . .
C35 C 0.7002(4) -0.0146(5) 0.2671(2) 0.0409(14) Uani 1 1 d . . . . .
H23 H 0.652054 -0.031985 0.241164 0.049 Uiso 1 1 calc R U . . .
C36 C 0.7322(3) 0.0931(4) 0.26809(19) 0.0327(13) Uani 1 1 d . . . . .
C40 C 0.6902(3) 0.1794(5) 0.22750(19) 0.0357(13) Uani 1 1 d . . . . .
H25 H 0.721825 0.249485 0.234980 0.043 Uiso 1 1 calc R U . . .
C41 C 0.6081(3) 0.2066(5) 0.2301(2) 0.0452(15) Uani 1 1 d . . . . .
H26A H 0.576504 0.138469 0.224452 0.068 Uiso 1 1 calc R U . . .
H26B H 0.583208 0.261133 0.202778 0.068 Uiso 1 1 calc R U . . .
H26C H 0.612010 0.237650 0.264757 0.068 Uiso 1 1 calc R U . . .
C42 C 0.6852(4) 0.1413(5) 0.1715(2) 0.0516(17) Uani 1 1 d . . . . .
H27A H 0.738180 0.128530 0.169432 0.077 Uiso 1 1 calc R U . . .
H27B H 0.659331 0.199023 0.146230 0.077 Uiso 1 1 calc R U . . .
H27C H 0.655014 0.072005 0.163300 0.077 Uiso 1 1 calc R U . . .
C37 C 0.9183(3) 0.0613(4) 0.3864(2) 0.0325(13) Uani 1 1 d . . . . .
H28 H 0.936614 0.136469 0.379050 0.039 Uiso 1 1 calc R U . . .
C39 C 0.9049(4) 0.0662(7) 0.4400(2) 0.065(2) Uani 1 1 d . . . . .
H29A H 0.865266 0.122831 0.439349 0.098 Uiso 1 1 calc R U . . .
H29B H 0.954089 0.085376 0.466947 0.098 Uiso 1 1 calc R U . . .
H29C H 0.886652 -0.006595 0.448080 0.098 Uiso 1 1 calc R U . . .
C38 C 0.9823(4) -0.0218(5) 0.3877(3) 0.0564(18) Uani 1 1 d . . . . .
H30A H 0.967855 -0.095059 0.398045 0.085 Uiso 1 1 calc R U . . .
H30B H 1.031585 0.002629 0.413180 0.085 Uiso 1 1 calc R U . . .
H30C H 0.988986 -0.026943 0.352695 0.085 Uiso 1 1 calc R U . . .
C19 C 0.7227(3) 0.4377(4) 0.46255(18) 0.0247(11) Uani 1 1 d . . . . .
C20 C 0.6446(3) 0.4773(4) 0.44422(19) 0.0291(12) Uani 1 1 d . . . . .
C21 C 0.5934(3) 0.4488(4) 0.4731(2) 0.0341(13) Uani 1 1 d . . . . .
H33 H 0.541052 0.475581 0.461544 0.041 Uiso 1 1 calc R U . . .
C22 C 0.6166(3) 0.3840(5) 0.5172(2) 0.0378(14) Uani 1 1 d . . . . .
H34 H 0.581672 0.368747 0.536798 0.045 Uiso 1 1 calc R U . . .
C23 C 0.6925(3) 0.3403(4) 0.5330(2) 0.0333(13) Uani 1 1 d . . . . .
H35 H 0.707998 0.292131 0.562585 0.040 Uiso 1 1 calc R U . . .
C24 C 0.7459(3) 0.3658(4) 0.50623(18) 0.0287(12) Uani 1 1 d . . . . .
C28 C 0.8277(3) 0.3166(4) 0.52491(18) 0.0312(12) Uani 1 1 d . . . . .
H37 H 0.852712 0.328881 0.496669 0.037 Uiso 1 1 calc R U . . .
C30 C 0.8279(4) 0.1912(5) 0.5355(2) 0.0506(16) Uani 1 1 d . . . . .
H38A H 0.880144 0.160869 0.539360 0.076 Uiso 1 1 calc R U . . .
H38B H 0.789321 0.154406 0.505986 0.076 Uiso 1 1 calc R U . . .
H38C H 0.814490 0.178085 0.567910 0.076 Uiso 1 1 calc R U . . .
C29 C 0.8780(3) 0.3745(5) 0.5746(2) 0.0495(15) Uani 1 1 d . . . . .
H39A H 0.854021 0.364989 0.602778 0.074 Uiso 1 1 calc R U . . .
H39B H 0.881656 0.454100 0.567559 0.074 Uiso 1 1 calc R U . . .
H39C H 0.930559 0.341729 0.585544 0.074 Uiso 1 1 calc R U . . .
C25 C 0.6139(3) 0.5491(5) 0.3958(2) 0.0370(14) Uani 1 1 d . . . . .
H40 H 0.658804 0.564838 0.382079 0.044 Uiso 1 1 calc R U . . .
C26 C 0.5520(3) 0.4869(5) 0.3528(2) 0.0463(16) Uani 1 1 d . . . . .
H41A H 0.505491 0.474790 0.364060 0.069 Uiso 1 1 calc R U . . .
H41B H 0.573103 0.414854 0.346400 0.069 Uiso 1 1 calc R U . . .
H41C H 0.537655 0.531047 0.320403 0.069 Uiso 1 1 calc R U . . .
C27 C 0.5829(4) 0.6607(5) 0.4079(3) 0.0544(17) Uani 1 1 d . . . . .
H42A H 0.571778 0.708977 0.376884 0.082 Uiso 1 1 calc R U . . .
H42B H 0.622286 0.696185 0.437458 0.082 Uiso 1 1 calc R U . . .
H42C H 0.534679 0.648872 0.417181 0.082 Uiso 1 1 calc R U . . .
C43 C 0.3948(4) 0.3274(5) 0.4238(3) 0.0536(17) Uani 1 1 d . . . . .
H43A H 0.382916 0.400940 0.407333 0.080 Uiso 1 1 calc R U . . .
H43B H 0.424675 0.336209 0.461020 0.080 Uiso 1 1 calc R U . . .
H43C H 0.345851 0.287758 0.420692 0.080 Uiso 1 1 calc R U . . .
C44 C 0.3955(4) 0.2347(6) 0.3455(2) 0.0566(18) Uani 1 1 d . . . . .
H44A H 0.372091 0.302059 0.325425 0.068 Uiso 1 1 calc R U . . .
H44B H 0.352472 0.183848 0.346473 0.068 Uiso 1 1 calc R U . . .
C45 C 0.4479(4) 0.1782(5) 0.3193(2) 0.0542(18) Uani 1 1 d . . . . .
H45A H 0.417694 0.157094 0.282868 0.065 Uiso 1 1 calc R U . . .
H45B H 0.490548 0.229248 0.317779 0.065 Uiso 1 1 calc R U . . .
C46 C 0.5186(4) 0.0075(5) 0.3219(2) 0.0560(18) Uani 1 1 d . . . . .
H46A H 0.480854 -0.016026 0.288584 0.084 Uiso 1 1 calc R U . . .
H46B H 0.538763 -0.058132 0.343690 0.084 Uiso 1 1 calc R U . . .
H46C H 0.562070 0.047142 0.314890 0.084 Uiso 1 1 calc R U . . .
C47 C 0.5564(4) 0.1083(5) 0.5708(2) 0.0519(17) Uani 1 1 d . . . . .
H47A H 0.505311 0.071018 0.558844 0.078 Uiso 1 1 calc R U . . .
H47B H 0.548669 0.189174 0.569127 0.078 Uiso 1 1 calc R U . . .
H47C H 0.583642 0.086324 0.607217 0.078 Uiso 1 1 calc R U . . .
C48 C 0.6220(4) -0.0389(5) 0.5433(2) 0.0504(17) Uani 1 1 d . . . . .
H48A H 0.574229 -0.084306 0.528430 0.060 Uiso 1 1 calc R U . . .
H48B H 0.644402 -0.057703 0.581029 0.060 Uiso 1 1 calc R U . . .
C49 C 0.6799(4) -0.0644(5) 0.5153(2) 0.0514(17) Uani 1 1 d . . . . .
H49A H 0.728477 -0.021331 0.531381 0.062 Uiso 1 1 calc R U . . .
H49B H 0.693300 -0.144556 0.519194 0.062 Uiso 1 1 calc R U . . .
C50 C 0.7037(4) -0.0670(5) 0.4332(2) 0.0533(17) Uani 1 1 d . . . . .
H50A H 0.681607 -0.045719 0.396116 0.080 Uiso 1 1 calc R U . . .
H50B H 0.712788 -0.147598 0.435653 0.080 Uiso 1 1 calc R U . . .
H50C H 0.753417 -0.027896 0.448621 0.080 Uiso 1 1 calc R U . . .
O5 O 0.7770(2) 0.9589(3) 0.67483(15) 0.0490(11) Uani 1 1 d . . . . .
O6 O 0.7988(2) 0.7388(3) 0.63953(15) 0.0471(10) Uani 1 1 d . . . . .
C51 C 0.7597(4) 1.0741(5) 0.6677(2) 0.0516(17) Uani 1 1 d . . . . .
H51A H 0.741028 1.091048 0.629960 0.077 Uiso 1 1 calc R U . . .
H51B H 0.807070 1.117403 0.684438 0.077 Uiso 1 1 calc R U . . .
H51C H 0.718921 1.093345 0.683628 0.077 Uiso 1 1 calc R U . . .
C52 C 0.8402(3) 0.9263(5) 0.6568(2) 0.0445(15) Uani 1 1 d . . . . .
H52A H 0.886651 0.973021 0.673560 0.053 Uiso 1 1 calc R U . . .
H52B H 0.825834 0.936710 0.618204 0.053 Uiso 1 1 calc R U . . .
C53 C 0.8589(4) 0.8075(6) 0.6701(2) 0.0553(18) Uani 1 1 d . . . . .
H53 H 0.905050 0.781589 0.695800 0.066 Uiso 1 1 calc R U . . .
C54 C 0.8136(4) 0.6256(6) 0.6532(3) 0.0642(19) Uani 1 1 d . . . . .
H54A H 0.771890 0.579603 0.630068 0.096 Uiso 1 1 calc R U . . .
H54B H 0.815017 0.614502 0.689805 0.096 Uiso 1 1 calc R U . . .
H54C H 0.864096 0.603946 0.649081 0.096 Uiso 1 1 calc R U . . .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'
Np Np -11.4937 4.1493 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N2 C14 C15 124.9(5) . . ?
N2 C14 C13 119.0(4) . . ?
C15 C14 C13 116.1(4) . . ?
O1 K1 Cl2 114.82(10) . . ?
O1 K1 O2 60.14(12) . . ?
O1 K1 O3 112.40(12) . . ?
O1 K1 O4 137.47(13) . . ?
O1 K1 C21 71.42(13) . . ?
O1 K1 C22 84.96(14) . . ?
O1 K1 C23 109.59(14) . . ?
O1 K1 C45 43.94(14) . . ?
Cl2 K1 C21 88.65(9) . . ?
Cl2 K1 C22 100.52(10) . . ?
Cl2 K1 C23 87.26(10) . . ?
Cl2 K1 C45 84.29(11) . . ?
O2 K1 Cl2 89.50(9) . . ?
O2 K1 C21 125.20(13) . . ?
O2 K1 C22 144.50(14) . . ?
O2 K1 C23 166.42(14) . . ?
O2 K1 C45 24.48(13) . . ?
O3 K1 Cl2 132.39(10) . . ?
O3 K1 O2 119.65(12) . . ?
O3 K1 O4 60.58(12) . . ?
O3 K1 C21 100.74(12) . . ?
O3 K1 C22 77.66(13) . . ?
O3 K1 C23 71.52(13) . . ?
O3 K1 C45 137.33(14) . . ?
O4 K1 Cl2 87.67(9) . . ?
O4 K1 O2 86.07(13) . . ?
O4 K1 C21 148.48(13) . . ?
O4 K1 C22 127.93(14) . . ?
O4 K1 C23 106.96(13) . . ?
O4 K1 C45 109.69(14) . . ?
C21 K1 C45 101.06(15) . . ?
C22 K1 C21 23.61(12) . . ?
C22 K1 C23 24.81(13) . . ?
C22 K1 C45 122.22(16) . . ?
C23 K1 C21 41.57(13) . . ?
C23 K1 C45 141.94(15) . . ?
C14 N2 Np1 128.8(3) . . ?
C14 N2 C31 113.1(4) . . ?
C31 N2 Np1 117.8(3) . . ?
Cl1 Np1 Cl2 100.09(5) . . ?
Cl1 Np1 C4 96.37(10) . . ?
Cl1 Np1 C5 74.53(11) . . ?
Cl1 Np1 C6 76.51(10) . . ?
Cl1 Np1 C1 100.44(11) . . ?
Cl1 Np1 C2 124.81(10) . . ?
Cl1 Np1 C3 122.60(10) . . ?
N2 Np1 Cl1 101.95(9) . . ?
N2 Np1 Cl2 87.39(9) . . ?
N2 Np1 N1 156.29(13) . . ?
N2 Np1 C4 61.07(13) . . ?
N2 Np1 C5 82.32(13) . . ?
N2 Np1 C6 108.41(13) . . ?
N2 Np1 C1 116.24(13) . . ?
N2 Np1 C2 95.22(13) . . ?
N2 Np1 C3 68.70(13) . . ?
Cl2 Np1 C4 146.90(11) . . ?
Cl2 Np1 C5 167.03(10) . . ?
Cl2 Np1 C6 164.18(10) . . ?
Cl2 Np1 C1 144.31(9) . . ?
Cl2 Np1 C2 133.04(10) . . ?
Cl2 Np1 C3 133.87(10) . . ?
N1 Np1 Cl1 101.61(9) . . ?
N1 Np1 Cl2 85.94(9) . . ?
N1 Np1 C4 118.58(13) . . ?
N1 Np1 C5 106.59(13) . . ?
N1 Np1 C6 79.74(13) . . ?
N1 Np1 C1 61.49(13) . . ?
N1 Np1 C2 73.26(13) . . ?
N1 Np1 C3 100.36(13) . . ?
C4 Np1 C5 27.41(13) . . ?
C4 Np1 C6 48.55(14) . . ?
C4 Np1 C1 57.64(13) . . ?
C5 Np1 C6 27.05(13) . . ?
C1 Np1 C5 48.55(13) . . ?
C1 Np1 C6 27.46(12) . . ?
C2 Np1 C4 48.97(13) . . ?
C2 Np1 C5 56.29(14) . . ?
C2 Np1 C6 48.31(14) . . ?
C2 Np1 C1 27.86(13) . . ?
C2 Np1 C3 27.31(12) . . ?
C3 Np1 C4 28.00(12) . . ?
C3 Np1 C5 48.43(13) . . ?
C3 Np1 C6 56.45(14) . . ?
C3 Np1 C1 49.05(13) . . ?
C43 O1 K1 128.1(4) . . ?
C44 O1 K1 119.2(4) . . ?
C44 O1 C43 111.9(5) . . ?
C14 C15 H2 119.3 . . ?
C16 C15 C14 121.5(5) . . ?
C16 C15 H2 119.3 . . ?
Np1 Cl2 K1 144.21(6) . . ?
C8 N1 Np1 129.0(3) . . ?
C8 N1 C19 111.0(4) . . ?
C19 N1 Np1 119.9(3) . . ?
C45 O2 K1 101.6(3) . . ?
C46 O2 K1 112.9(3) . . ?
C46 O2 C45 112.8(4) . . ?
C15 C16 H3 119.4 . . ?
C17 C16 C15 121.2(5) . . ?
C17 C16 H3 119.4 . . ?
C47 O3 K1 122.9(3) . . ?
C48 O3 K1 117.4(3) . . ?
C48 O3 C47 111.3(4) . . ?
C16 C17 H4 120.6 . . ?
C18 C17 C16 118.8(4) . . ?
C18 C17 H4 120.6 . . ?
C49 O4 K1 114.5(3) . . ?
C49 O4 C50 111.7(5) . . ?
C50 O4 K1 115.5(3) . . ?
C17 C18 H5 119.3 . . ?
C17 C18 C13 121.4(5) . . ?
C13 C18 H5 119.3 . . ?
C14 C13 C4 117.0(4) . . ?
C18 C13 C14 120.7(4) . . ?
C18 C13 C4 122.3(5) . . ?
C13 C4 Np1 110.5(3) . . ?
C5 C4 Np1 77.9(3) . . ?
C5 C4 C13 123.7(4) . . ?
C5 C4 C3 118.4(4) . . ?
C3 C4 Np1 75.7(3) . . ?
C3 C4 C13 117.5(4) . . ?
Np1 C5 H8 120.1 . . ?
C4 C5 Np1 74.7(3) . . ?
C4 C5 H8 119.5 . . ?
C6 C5 Np1 76.7(3) . . ?
C6 C5 C4 121.0(5) . . ?
C6 C5 H8 119.5 . . ?
Np1 C6 H9 120.6 . . ?
C5 C6 Np1 76.3(3) . . ?
C5 C6 H9 119.7 . . ?
C5 C6 C1 120.6(5) . . ?
C1 C6 Np1 74.5(3) . . ?
C1 C6 H9 119.7 . . ?
C6 C1 Np1 78.0(3) . . ?
C6 C1 C2 118.3(4) . . ?
C6 C1 C7 121.3(5) . . ?
C2 C1 Np1 75.6(3) . . ?
C2 C1 C7 120.3(4) . . ?
C7 C1 Np1 112.0(3) . . ?
Np1 C2 H11 118.5 . . ?
C1 C2 Np1 76.5(3) . . ?
C1 C2 H11 119.4 . . ?
C3 C2 Np1 76.4(3) . . ?
C3 C2 C1 121.2(4) . . ?
C3 C2 H11 119.4 . . ?
Np1 C3 H12 118.4 . . ?
C4 C3 Np1 76.3(3) . . ?
C4 C3 H12 119.8 . . ?
C2 C3 Np1 76.3(3) . . ?
C2 C3 C4 120.4(5) . . ?
C2 C3 H12 119.8 . . ?
C12 C7 C1 121.0(4) . . ?
C12 C7 C8 122.1(4) . . ?
C8 C7 C1 116.9(4) . . ?
C7 C12 H14 119.9 . . ?
C11 C12 C7 120.3(5) . . ?
C11 C12 H14 119.9 . . ?
C12 C11 H15 120.6 . . ?
C10 C11 C12 118.8(5) . . ?
C10 C11 H15 120.6 . . ?
C11 C10 H16 119.2 . . ?
C11 C10 C9 121.6(5) . . ?
C9 C10 H16 119.2 . . ?
C10 C9 H17 119.1 . . ?
C10 C9 C8 121.9(5) . . ?
C8 C9 H17 119.1 . . ?
N1 C8 C7 119.6(4) . . ?
N1 C8 C9 125.0(4) . . ?
C9 C8 C7 115.3(4) . . ?
C32 C31 N2 118.9(4) . . ?
C32 C31 C36 120.9(5) . . ?
C36 C31 N2 120.2(4) . . ?
C31 C32 C33 118.4(5) . . ?
C31 C32 C37 121.4(5) . . ?
C33 C32 C37 120.3(5) . . ?
C32 C33 H21 119.3 . . ?
C34 C33 C32 121.5(5) . . ?
C34 C33 H21 119.3 . . ?
C33 C34 H22 120.2 . . ?
C35 C34 C33 119.5(5) . . ?
C35 C34 H22 120.2 . . ?
C34 C35 H23 119.2 . . ?
C34 C35 C36 121.6(5) . . ?
C36 C35 H23 119.2 . . ?
C31 C36 C35 118.1(5) . . ?
C31 C36 C40 121.8(5) . . ?
C35 C36 C40 120.1(5) . . ?
C36 C40 H25 107.7 . . ?
C36 C40 C41 112.7(4) . . ?
C36 C40 C42 111.0(5) . . ?
C41 C40 H25 107.7 . . ?
C41 C40 C42 109.7(4) . . ?
C42 C40 H25 107.7 . . ?
C40 C41 H26A 109.5 . . ?
C40 C41 H26B 109.5 . . ?
C40 C41 H26C 109.5 . . ?
H26A C41 H26B 109.5 . . ?
H26A C41 H26C 109.5 . . ?
H26B C41 H26C 109.5 . . ?
C40 C42 H27A 109.5 . . ?
C40 C42 H27B 109.5 . . ?
C40 C42 H27C 109.5 . . ?
H27A C42 H27B 109.5 . . ?
H27A C42 H27C 109.5 . . ?
H27B C42 H27C 109.5 . . ?
C32 C37 H28 107.9 . . ?
C32 C37 C39 110.5(4) . . ?
C39 C37 H28 107.9 . . ?
C38 C37 C32 112.6(4) . . ?
C38 C37 H28 107.9 . . ?
C38 C37 C39 110.0(5) . . ?
C37 C39 H29A 109.5 . . ?
C37 C39 H29B 109.5 . . ?
C37 C39 H29C 109.5 . . ?
H29A C39 H29B 109.5 . . ?
H29A C39 H29C 109.5 . . ?
H29B C39 H29C 109.5 . . ?
C37 C38 H30A 109.5 . . ?
C37 C38 H30B 109.5 . . ?
C37 C38 H30C 109.5 . . ?
H30A C38 H30B 109.5 . . ?
H30A C38 H30C 109.5 . . ?
H30B C38 H30C 109.5 . . ?
C20 C19 N1 120.0(4) . . ?
C24 C19 N1 119.8(4) . . ?
C24 C19 C20 120.2(4) . . ?
C19 C20 C25 123.4(4) . . ?
C21 C20 C19 118.0(5) . . ?
C21 C20 C25 118.6(5) . . ?
K1 C21 H33 106.4 . . ?
C20 C21 K1 94.6(3) . . ?
C20 C21 H33 118.9 . . ?
C22 C21 K1 69.2(3) . . ?
C22 C21 C20 122.2(5) . . ?
C22 C21 H33 118.9 . . ?
K1 C22 H34 100.6 . . ?
C21 C22 K1 87.1(3) . . ?
C21 C22 H34 120.5 . . ?
C21 C22 C23 119.0(5) . . ?
C23 C22 K1 82.1(3) . . ?
C23 C22 H34 120.5 . . ?
K1 C23 H35 102.1 . . ?
C22 C23 K1 73.1(3) . . ?
C22 C23 H35 119.3 . . ?
C24 C23 K1 94.9(3) . . ?
C24 C23 C22 121.5(5) . . ?
C24 C23 H35 119.3 . . ?
C19 C24 C28 121.5(4) . . ?
C23 C24 C19 119.0(5) . . ?
C23 C24 C28 119.6(5) . . ?
C24 C28 H37 107.9 . . ?
C24 C28 C30 113.0(5) . . ?
C24 C28 C29 111.3(4) . . ?
C30 C28 H37 107.9 . . ?
C29 C28 H37 107.9 . . ?
C29 C28 C30 108.7(5) . . ?
C28 C30 H38A 109.5 . . ?
C28 C30 H38B 109.5 . . ?
C28 C30 H38C 109.5 . . ?
H38A C30 H38B 109.5 . . ?
H38A C30 H38C 109.5 . . ?
H38B C30 H38C 109.5 . . ?
C28 C29 H39A 109.5 . . ?
C28 C29 H39B 109.5 . . ?
C28 C29 H39C 109.5 . . ?
H39A C29 H39B 109.5 . . ?
H39A C29 H39C 109.5 . . ?
H39B C29 H39C 109.5 . . ?
C20 C25 H40 107.4 . . ?
C20 C25 C26 110.8(5) . . ?
C20 C25 C27 112.4(5) . . ?
C26 C25 H40 107.4 . . ?
C27 C25 H40 107.4 . . ?
C27 C25 C26 111.2(5) . . ?
C25 C26 H41A 109.5 . . ?
C25 C26 H41B 109.5 . . ?
C25 C26 H41C 109.5 . . ?
H41A C26 H41B 109.5 . . ?
H41A C26 H41C 109.5 . . ?
H41B C26 H41C 109.5 . . ?
C25 C27 H42A 109.5 . . ?
C25 C27 H42B 109.5 . . ?
C25 C27 H42C 109.5 . . ?
H42A C27 H42B 109.5 . . ?
H42A C27 H42C 109.5 . . ?
H42B C27 H42C 109.5 . . ?
O1 C43 H43A 109.5 . . ?
O1 C43 H43B 109.5 . . ?
O1 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O1 C44 H44A 109.9 . . ?
O1 C44 H44B 109.9 . . ?
O1 C44 C45 109.1(5) . . ?
H44A C44 H44B 108.3 . . ?
C45 C44 H44A 109.9 . . ?
C45 C44 H44B 109.9 . . ?
K1 C45 H45A 161.2 . . ?
K1 C45 H45B 73.0 . . ?
O2 C45 K1 53.9(3) . . ?
O2 C45 C44 108.4(5) . . ?
O2 C45 H45A 110.0 . . ?
O2 C45 H45B 110.0 . . ?
C44 C45 K1 86.3(3) . . ?
C44 C45 H45A 110.0 . . ?
C44 C45 H45B 110.0 . . ?
H45A C45 H45B 108.4 . . ?
O2 C46 H46A 109.5 . . ?
O2 C46 H46B 109.5 . . ?
O2 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
O3 C47 H47A 109.5 . . ?
O3 C47 H47B 109.5 . . ?
O3 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
O3 C48 H48A 109.7 . . ?
O3 C48 H48B 109.7 . . ?
O3 C48 C49 109.6(5) . . ?
H48A C48 H48B 108.2 . . ?
C49 C48 H48A 109.7 . . ?
C49 C48 H48B 109.7 . . ?
O4 C49 C48 111.2(5) . . ?
O4 C49 H49A 109.4 . . ?
O4 C49 H49B 109.4 . . ?
C48 C49 H49A 109.4 . . ?
C48 C49 H49B 109.4 . . ?
H49A C49 H49B 108.0 . . ?
O4 C50 H50A 109.5 . . ?
O4 C50 H50B 109.5 . . ?
O4 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C52 O5 C51 112.8(5) . . ?
C53 O6 C54 111.5(5) . . ?
O5 C51 H51A 109.5 . . ?
O5 C51 H51B 109.5 . . ?
O5 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
O5 C52 H52A 109.8 . . ?
O5 C52 H52B 109.8 . . ?
O5 C52 C53 109.2(5) . . ?
H52A C52 H52B 108.3 . . ?
C53 C52 H52A 109.8 . . ?
C53 C52 H52B 109.8 . . ?
O6 C53 C52 110.4(5) . . ?
O6 C53 H53 124.8 . . ?
C52 C53 H53 124.8 . . ?
O6 C54 H54A 109.5 . . ?
O6 C54 H54B 109.5 . . ?
O6 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 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
C14 N2 1.384(6) . ?
C14 C15 1.408(6) . ?
C14 C13 1.422(7) . ?
Cl1 Np1 2.6268(13) . ?
K1 O1 2.718(4) . ?
K1 Cl2 2.9968(17) . ?
K1 O2 2.814(4) . ?
K1 O3 2.776(4) . ?
K1 O4 2.779(4) . ?
K1 C21 3.402(5) . ?
K1 C22 3.185(5) . ?
K1 C23 3.297(5) . ?
K1 C45 3.411(6) . ?
N2 Np1 2.483(4) . ?
N2 C31 1.454(6) . ?
Np1 Cl2 2.6740(13) . ?
Np1 N1 2.494(4) . ?
Np1 C4 2.921(5) . ?
Np1 C5 2.961(5) . ?
Np1 C6 2.966(5) . ?
Np1 C1 2.922(5) . ?
Np1 C2 2.911(5) . ?
Np1 C3 2.913(5) . ?
O1 C43 1.435(7) . ?
O1 C44 1.428(7) . ?
C15 H2 0.9500 . ?
C15 C16 1.382(7) . ?
N1 C8 1.398(6) . ?
N1 C19 1.432(6) . ?
O2 C45 1.443(7) . ?
O2 C46 1.437(7) . ?
C16 H3 0.9500 . ?
C16 C17 1.379(7) . ?
O3 C47 1.435(6) . ?
O3 C48 1.427(7) . ?
C17 H4 0.9500 . ?
C17 C18 1.369(7) . ?
O4 C49 1.418(6) . ?
O4 C50 1.435(6) . ?
C18 H5 0.9500 . ?
C18 C13 1.393(7) . ?
C13 C4 1.482(7) . ?
C4 C5 1.394(7) . ?
C4 C3 1.411(6) . ?
C5 H8 0.9500 . ?
C5 C6 1.386(6) . ?
C6 H9 0.9500 . ?
C6 C1 1.398(6) . ?
C1 C2 1.405(7) . ?
C1 C7 1.490(6) . ?
C2 H11 0.9500 . ?
C2 C3 1.375(6) . ?
C3 H12 0.9500 . ?
C7 C12 1.400(7) . ?
C7 C8 1.426(6) . ?
C12 H14 0.9500 . ?
C12 C11 1.387(7) . ?
C11 H15 0.9500 . ?
C11 C10 1.374(7) . ?
C10 H16 0.9500 . ?
C10 C9 1.393(7) . ?
C9 H17 0.9500 . ?
C9 C8 1.408(6) . ?
C31 C32 1.400(7) . ?
C31 C36 1.410(7) . ?
C32 C33 1.404(7) . ?
C32 C37 1.521(7) . ?
C33 H21 0.9500 . ?
C33 C34 1.387(8) . ?
C34 H22 0.9500 . ?
C34 C35 1.367(8) . ?
C35 H23 0.9500 . ?
C35 C36 1.412(7) . ?
C36 C40 1.521(7) . ?
C40 H25 1.0000 . ?
C40 C41 1.531(8) . ?
C40 C42 1.539(7) . ?
C41 H26A 0.9800 . ?
C41 H26B 0.9800 . ?
C41 H26C 0.9800 . ?
C42 H27A 0.9800 . ?
C42 H27B 0.9800 . ?
C42 H27C 0.9800 . ?
C37 H28 1.0000 . ?
C37 C39 1.522(7) . ?
C37 C38 1.514(7) . ?
C39 H29A 0.9800 . ?
C39 H29B 0.9800 . ?
C39 H29C 0.9800 . ?
C38 H30A 0.9800 . ?
C38 H30B 0.9800 . ?
C38 H30C 0.9800 . ?
C19 C20 1.416(7) . ?
C19 C24 1.408(7) . ?
C20 C21 1.411(7) . ?
C20 C25 1.510(7) . ?
C21 H33 0.9500 . ?
C21 C22 1.364(7) . ?
C22 H34 0.9500 . ?
C22 C23 1.397(7) . ?
C23 H35 0.9500 . ?
C23 C24 1.393(7) . ?
C24 C28 1.515(7) . ?
C28 H37 1.0000 . ?
C28 C30 1.532(7) . ?
C28 C29 1.525(7) . ?
C30 H38A 0.9800 . ?
C30 H38B 0.9800 . ?
C30 H38C 0.9800 . ?
C29 H39A 0.9800 . ?
C29 H39B 0.9800 . ?
C29 H39C 0.9800 . ?
C25 H40 1.0000 . ?
C25 C26 1.524(8) . ?
C25 C27 1.523(7) . ?
C26 H41A 0.9800 . ?
C26 H41B 0.9800 . ?
C26 H41C 0.9800 . ?
C27 H42A 0.9800 . ?
C27 H42B 0.9800 . ?
C27 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.496(9) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C49 1.485(8) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
O5 C51 1.417(7) . ?
O5 C52 1.417(6) . ?
O6 C53 1.404(7) . ?
O6 C54 1.411(7) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C52 C53 1.484(8) . ?
C53 H53 0.9500 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 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
C14 N2 C31 C32 89.3(5) . . . . ?
C14 N2 C31 C36 -90.2(5) . . . . ?
C14 C15 C16 C17 0.0(8) . . . . ?
C14 C13 C4 Np1 -17.5(5) . . . . ?
C14 C13 C4 C5 -106.3(5) . . . . ?
C14 C13 C4 C3 66.6(6) . . . . ?
K1 O1 C44 C45 -14.5(6) . . . . ?
K1 O2 C45 C44 -70.9(5) . . . . ?
K1 O3 C48 C49 39.8(6) . . . . ?
K1 O4 C49 C48 49.3(6) . . . . ?
K1 C21 C22 C23 79.3(5) . . . . ?
K1 C22 C23 C24 85.3(5) . . . . ?
K1 C23 C24 C19 73.5(5) . . . . ?
K1 C23 C24 C28 -107.0(4) . . . . ?
N2 C14 C15 C16 175.0(5) . . . . ?
N2 C14 C13 C18 -173.7(5) . . . . ?
N2 C14 C13 C4 7.1(7) . . . . ?
N2 C31 C32 C33 179.5(4) . . . . ?
N2 C31 C32 C37 1.3(7) . . . . ?
N2 C31 C36 C35 -179.2(4) . . . . ?
N2 C31 C36 C40 1.0(7) . . . . ?
Np1 N2 C31 C32 -96.1(4) . . . . ?
Np1 N2 C31 C36 84.4(5) . . . . ?
Np1 N1 C8 C7 -7.2(6) . . . . ?
Np1 N1 C8 C9 173.0(4) . . . . ?
Np1 N1 C19 C20 -86.5(5) . . . . ?
Np1 N1 C19 C24 95.9(5) . . . . ?
Np1 C4 C5 C6 63.7(4) . . . . ?
Np1 C4 C3 C2 -64.8(4) . . . . ?
Np1 C5 C6 C1 62.4(4) . . . . ?
Np1 C6 C1 C2 66.3(4) . . . . ?
Np1 C6 C1 C7 -108.6(4) . . . . ?
Np1 C1 C2 C3 64.7(4) . . . . ?
Np1 C1 C7 C12 -174.2(4) . . . . ?
Np1 C1 C7 C8 8.7(5) . . . . ?
Np1 C2 C3 C4 64.8(4) . . . . ?
O1 C44 C45 K1 10.0(4) . . . . ?
O1 C44 C45 O2 60.0(7) . . . . ?
C15 C14 N2 Np1 -167.3(4) . . . . ?
C15 C14 N2 C31 6.5(7) . . . . ?
C15 C14 C13 C18 5.4(7) . . . . ?
C15 C14 C13 C4 -173.8(4) . . . . ?
C15 C16 C17 C18 2.9(8) . . . . ?
N1 C19 C20 C21 -173.3(4) . . . . ?
N1 C19 C20 C25 6.1(7) . . . . ?
N1 C19 C24 C23 173.5(4) . . . . ?
N1 C19 C24 C28 -6.0(7) . . . . ?
C16 C17 C18 C13 -1.5(8) . . . . ?
O3 C48 C49 O4 -58.9(7) . . . . ?
C17 C18 C13 C14 -2.8(8) . . . . ?
C17 C18 C13 C4 176.4(5) . . . . ?
C18 C13 C4 Np1 163.4(4) . . . . ?
C18 C13 C4 C5 74.6(7) . . . . ?
C18 C13 C4 C3 -112.5(5) . . . . ?
C13 C14 N2 Np1 11.7(6) . . . . ?
C13 C14 N2 C31 -174.4(4) . . . . ?
C13 C14 C15 C16 -4.1(7) . . . . ?
C13 C4 C5 Np1 106.7(4) . . . . ?
C13 C4 C5 C6 170.4(5) . . . . ?
C13 C4 C3 Np1 -105.9(4) . . . . ?
C13 C4 C3 C2 -170.7(4) . . . . ?
C4 C5 C6 Np1 -62.7(4) . . . . ?
C4 C5 C6 C1 -0.3(7) . . . . ?
C5 C4 C3 Np1 67.4(4) . . . . ?
C5 C4 C3 C2 2.6(7) . . . . ?
C5 C6 C1 Np1 -63.3(4) . . . . ?
C5 C6 C1 C2 3.0(7) . . . . ?
C5 C6 C1 C7 -171.8(5) . . . . ?
C6 C1 C2 Np1 -67.6(4) . . . . ?
C6 C1 C2 C3 -2.9(7) . . . . ?
C6 C1 C7 C12 -85.1(6) . . . . ?
C6 C1 C7 C8 97.7(6) . . . . ?
C1 C2 C3 Np1 -64.7(4) . . . . ?
C1 C2 C3 C4 0.1(7) . . . . ?
C1 C7 C12 C11 -177.2(5) . . . . ?
C1 C7 C8 N1 -2.7(7) . . . . ?
C1 C7 C8 C9 177.1(4) . . . . ?
C2 C1 C7 C12 100.1(6) . . . . ?
C2 C1 C7 C8 -77.0(6) . . . . ?
C3 C4 C5 Np1 -66.2(4) . . . . ?
C3 C4 C5 C6 -2.5(7) . . . . ?
C7 C1 C2 Np1 107.3(4) . . . . ?
C7 C1 C2 C3 172.0(4) . . . . ?
C7 C12 C11 C10 0.6(8) . . . . ?
C12 C7 C8 N1 -179.8(4) . . . . ?
C12 C7 C8 C9 0.0(7) . . . . ?
C12 C11 C10 C9 -0.7(8) . . . . ?
C11 C10 C9 C8 0.5(8) . . . . ?
C10 C9 C8 N1 179.6(5) . . . . ?
C10 C9 C8 C7 -0.1(7) . . . . ?
C8 N1 C19 C20 90.3(5) . . . . ?
C8 N1 C19 C24 -87.3(5) . . . . ?
C8 C7 C12 C11 -0.2(8) . . . . ?
C31 C32 C33 C34 -0.2(8) . . . . ?
C31 C32 C37 C39 108.5(6) . . . . ?
C31 C32 C37 C38 -128.1(5) . . . . ?
C31 C36 C40 C41 -119.3(5) . . . . ?
C31 C36 C40 C42 117.2(5) . . . . ?
C32 C31 C36 C35 1.3(7) . . . . ?
C32 C31 C36 C40 -178.5(4) . . . . ?
C32 C33 C34 C35 0.9(9) . . . . ?
C33 C32 C37 C39 -69.8(6) . . . . ?
C33 C32 C37 C38 53.6(6) . . . . ?
C33 C34 C35 C36 -0.5(9) . . . . ?
C34 C35 C36 C31 -0.6(8) . . . . ?
C34 C35 C36 C40 179.3(5) . . . . ?
C35 C36 C40 C41 60.9(6) . . . . ?
C35 C36 C40 C42 -62.6(7) . . . . ?
C36 C31 C32 C33 -1.0(7) . . . . ?
C36 C31 C32 C37 -179.2(4) . . . . ?
C37 C32 C33 C34 178.1(5) . . . . ?
C19 N1 C8 C7 176.3(4) . . . . ?
C19 N1 C8 C9 -3.4(7) . . . . ?
C19 C20 C21 K1 -69.2(4) . . . . ?
C19 C20 C21 C22 -0.8(8) . . . . ?
C19 C20 C25 C26 113.7(5) . . . . ?
C19 C20 C25 C27 -121.1(5) . . . . ?
C19 C24 C28 C30 -133.0(5) . . . . ?
C19 C24 C28 C29 104.4(5) . . . . ?
C20 C19 C24 C23 -4.1(7) . . . . ?
C20 C19 C24 C28 176.4(4) . . . . ?
C20 C21 C22 K1 -82.2(5) . . . . ?
C20 C21 C22 C23 -2.8(8) . . . . ?
C21 C20 C25 C26 -66.8(6) . . . . ?
C21 C20 C25 C27 58.3(7) . . . . ?
C21 C22 C23 K1 -82.3(5) . . . . ?
C21 C22 C23 C24 3.1(8) . . . . ?
C22 C23 C24 C19 0.4(8) . . . . ?
C22 C23 C24 C28 179.8(5) . . . . ?
C23 C24 C28 C30 47.6(6) . . . . ?
C23 C24 C28 C29 -75.0(6) . . . . ?
C24 C19 C20 C21 4.3(7) . . . . ?
C24 C19 C20 C25 -176.3(5) . . . . ?
C25 C20 C21 K1 111.4(4) . . . . ?
C25 C20 C21 C22 179.7(5) . . . . ?
C43 O1 C44 C45 175.3(5) . . . . ?
C46 O2 C45 K1 -121.2(5) . . . . ?
C46 O2 C45 C44 167.9(5) . . . . ?
C47 O3 C48 C49 -170.9(5) . . . . ?
C50 O4 C49 C48 -177.0(5) . . . . ?
O5 C52 C53 O6 69.8(6) . . . . ?
C51 O5 C52 C53 174.9(5) . . . . ?
C54 O6 C53 C52 -177.4(5) . . . . ?
