#------------------------------------------------------------------------------
#$Date: 2023-07-27 00:59:25 +0300 (Thu, 27 Jul 2023) $
#$Revision: 285353 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/19/7131931.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_7131931
loop_
_publ_author_name
'Kim, Sung Kuk'
'Yang, Ju Ho'
_publ_section_title
;
 A Squaramide Cage Capable of Binding and Extracting H2PO4- and HP2O73- in
 Highly Polar Protic Media
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC02611F
_journal_year                    2023
_chemical_formula_moiety
'C60 H59.962 Cl0.038 N6 O9, C16 H36 N, 3(C H4 O), C H Cl2.864, 1.045(C H Cl3), H2 O4 P'
_chemical_formula_sum            'C81.04 H112.01 Cl6.04 N7 O16 P'
_chemical_formula_weight         1685.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-07
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-05-30 deposited with the CCDC.	2023-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.6710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.13170(10)
_cell_length_b                   19.00400(10)
_cell_length_c                   34.9608(2)
_cell_measurement_reflns_used    40929
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      76.8940
_cell_measurement_theta_min      2.5390
_cell_volume                     8665.57(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -120.00 -30.00   0.50   27.00    --  -48.70 -67.00-104.00  180
  2  ω    -67.00  24.00   0.50   27.00    --  -48.70  67.00  29.00  182
  3  ω    -23.00  67.00   0.50   27.00    --   48.70 -67.00-104.00  180
  4  ω     35.00 127.00   0.50  103.00    --  107.75 -67.00-104.00  184
  5  ω     89.00 178.00   0.50  103.00    --  107.75  67.00  29.00  178
  6  ω   -120.00 -73.00   0.50   27.00    --  -48.70-125.00  30.00   94
  7  ω     30.00 120.00   0.50   27.00    --   48.70  67.00  29.00  180
  8  ω     35.00 120.00   0.50  103.00    --  107.75 -38.00-120.00  170
  9  ω     35.00 106.00   0.50  103.00    --  107.75 -99.00-180.00  142
 10  ω     95.00 178.00   0.50  103.00    --  107.75  38.00 -60.00  166
 11  ω     85.00 178.00   0.50  103.00    --  107.75  77.00   0.00  186
 12  ω     35.00 106.00   0.50  103.00    --  107.75 -99.00 120.00  142
 13  ω   -120.00 -45.00   0.50   27.00    --  -48.70 -77.00 -30.00  150
 14  ω   -120.00 -73.50   0.50   27.00    --  -48.70 -77.00 150.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0655290000
_diffrn_orient_matrix_UB_12      0.0507183000
_diffrn_orient_matrix_UB_13      0.0213322000
_diffrn_orient_matrix_UB_21      -0.0980693000
_diffrn_orient_matrix_UB_22      -0.0371224000
_diffrn_orient_matrix_UB_23      -0.0182669000
_diffrn_orient_matrix_UB_31      0.0063044000
_diffrn_orient_matrix_UB_32      -0.0512052000
_diffrn_orient_matrix_UB_33      0.0343418000
_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  0.0320
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            65351
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.117
_diffrn_reflns_theta_min         2.545
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.538
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       plate
_exptl_crystal_F_000             3572
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.963
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1097
_refine_ls_number_reflns         17522
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0642P)²+6.9455P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1229
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15869
_reflns_number_total             17522
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3cc02611f2.cif
_cod_data_source_block           yjh-4
_cod_database_code               7131931
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C81H106N7O16Cl6P
_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   0.867
_shelx_estimated_absorpt_t_min   0.655
_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, All O(H) groups
2. Restrained distances
 H34-O10
 1.85 with sigma of 0.05
 C77A-Cl6A
 1.77 with sigma of 0.02
 C77A-Cl4A
 1.77 with sigma of 0.02
 C77A-Cl5A
 1.77 with sigma of 0.02
 C81-O16 = C81A-O16A
 1.45 with sigma of 0.01
 Cl6-C77
 1.77 with sigma of 0.02
 Cl4-C77
 1.77 with sigma of 0.02
 Cl5-C77
 1.77 with sigma of 0.02
 Cl6-C77 \\sim Cl6A-C77
 with sigma of 0.02
 Cl4-C77 \\sim Cl4A-C77
 with sigma of 0.02
 Cl5-C77 \\sim Cl5A-C77
 with sigma of 0.02
 Cl4-Cl5 \\sim Cl4-Cl6 \\sim Cl5-Cl6 \\sim Cl4A-Cl5A \\sim Cl4A-Cl6A \\sim
Cl5A-Cl6A
 with sigma of 0.03
 O16-C81 \\sim O16A-C81A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl4 \\sim Cl4A \\sim Cl5 \\sim Cl5A \\sim Cl6 \\sim Cl6A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
C81 \\sim C81A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O16 \\sim O16A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C81) \\sim Ueq, Uanis(C81A) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O16A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O16) \\sim Ueq, Uanis(O16A) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C81A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl4) = Uanis(Cl4A)
Uanis(Cl6) = Uanis(Cl6A)
Uanis(Cl5) = Uanis(Cl5A)
4. Others
 Sof(O16A)=Sof(H19)=Sof(C81A)=Sof(H27)=Sof(H28)=Sof(H29)=1-FVAR(1)
 Sof(O16)=Sof(H18)=Sof(C81)=Sof(H24)=Sof(H25)=Sof(H26)=FVAR(1)
 Sof(Cl4A)=Sof(Cl5A)=Sof(Cl6A)=Sof(C77A)=Sof(H31)=1-FVAR(2)
 Sof(Cl4)=Sof(Cl5)=Sof(Cl6)=FVAR(2)
 Fixed Sof: Cl7(0.038) H7(0.962)
 Fixed Uiso: C77A(0.03797)
5.a Ternary CH refined with riding coordinates:
 C77A(H31), C78(H42)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C18(H18A,H18B), C29(H29A,H29B), C36(H36A,H36B), C37(H37A,
 H37B), C48(H48A,H48B), C49(H49A,H49B), C51(H51A,H51B), C53(H53A,H53B),
 C55(H55A,H55B), C57(H57A,H57B), C59(H59A,H59B), C61(H,HA), C62(HB,HC), C63(HD,
 HE), C65(HI,HJ), C66(HK,HL), C67(HM,HN), C69(HR,HS), C70(HT,HU), C71(HV,HW),
 C73(H8,H10), C74(H11,H12), C75(H13,H14)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6A), C7(H7A), C9(H9), C20(H20), C21(H21), C22(H22), C23(H23), C43(H43),
 C44(H44), C45(H45), C46(H46)
5.d Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C56(H56A,H56B,
 H56C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C64(HF,HG,HH), C68(HO,HP,HQ),
 C72(HX,HY,HZ), C76(H15,H16,H17), C81(H24,H25,H26), C81A(H27,H28,H29), C80(H35,
 H36,H37), C79(H39,H40,H41)
5.e Idealised tetrahedral OH refined as rotating group:
 O16(H18), O16A(H19), O15(H34)
;
_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 1.901
_oxdiff_exptl_absorpt_empirical_full_min 0.585
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Cl7 Cl 0.8147(10) 0.1631(7) 0.2329(3) 0.030(2) Uiso 0.038 1 d . . P A 2
H7 H 0.757(2) 0.1751(14) 0.2349(7) 0.037(7) Uiso 0.962 1 d . . P B 2
O1 O 0.11965(10) 0.07408(7) 0.25781(4) 0.0286(3) Uani 1 1 d . . . . .
O2 O 0.37009(9) 0.05189(7) 0.26235(4) 0.0236(3) Uani 1 1 d . . . . .
O3 O 0.56125(9) 0.28993(6) 0.30948(3) 0.0201(2) Uani 1 1 d . . . . .
O4 O 0.50602(9) 0.33915(7) 0.47455(3) 0.0226(3) Uani 1 1 d . . . . .
O5 O 0.46934(9) 0.58469(6) 0.35646(4) 0.0219(3) Uani 1 1 d . . . . .
O6 O 0.06290(10) 0.11026(7) 0.45391(4) 0.0270(3) Uani 1 1 d . . . . .
O7 O 0.28791(11) 0.08859(7) 0.50085(4) 0.0300(3) Uani 1 1 d . . . . .
O8 O -0.04319(11) 0.61540(8) 0.38343(4) 0.0335(3) Uani 1 1 d . . . . .
O9 O 0.15584(11) 0.72126(7) 0.38951(4) 0.0303(3) Uani 1 1 d . . . . .
N1 N 0.15489(11) 0.24008(8) 0.27473(4) 0.0185(3) Uani 1 1 d . . . . .
H1 H 0.1826(19) 0.2776(14) 0.2788(7) 0.031(6) Uiso 1 1 d . . . . .
N2 N 0.39881(11) 0.22451(8) 0.27118(4) 0.0178(3) Uani 1 1 d . . . . .
H2 H 0.3864(17) 0.2635(13) 0.2776(7) 0.025(6) Uiso 1 1 d . . . . .
N3 N 0.12026(12) 0.27403(8) 0.43529(4) 0.0213(3) Uani 1 1 d . . . . .
H3 H 0.1523(19) 0.3087(14) 0.4321(7) 0.029(6) Uiso 1 1 d . . . . .
N4 N 0.34362(12) 0.25819(9) 0.48079(4) 0.0213(3) Uani 1 1 d . . . . .
H4 H 0.3366(18) 0.2928(14) 0.4694(7) 0.026(6) Uiso 1 1 d . . . . .
N5 N 0.07508(11) 0.50876(8) 0.32960(4) 0.0185(3) Uani 1 1 d . . . . .
H5 H 0.1211(19) 0.4905(13) 0.3204(7) 0.030(6) Uiso 1 1 d . . . . .
N6 N 0.27202(11) 0.60843(8) 0.33685(4) 0.0188(3) Uani 1 1 d . . . . .
H6 H 0.2869(17) 0.5685(13) 0.3279(6) 0.024(5) Uiso 1 1 d . . . . .
C1 C 0.21402(13) 0.18665(9) 0.26882(4) 0.0170(3) Uani 1 1 d . . . . .
C2 C 0.19650(13) 0.11129(9) 0.26187(5) 0.0201(3) Uani 1 1 d . . . . .
C3 C 0.31037(13) 0.10229(9) 0.26298(5) 0.0193(3) Uani 1 1 d . . . . .
C4 C 0.32163(12) 0.17854(9) 0.26754(4) 0.0169(3) Uani 1 1 d . . . . .
C5 C 0.49826(13) 0.20957(9) 0.26139(4) 0.0172(3) Uani 1 1 d . . . . .
C6 C 0.51251(14) 0.16328(9) 0.23161(5) 0.0219(3) Uani 1 1 d . . . . .
H6A H 0.454966 0.140447 0.217991 0.026 Uiso 1 1 calc R U . . .
C7 C 0.60988(15) 0.15021(10) 0.22165(5) 0.0251(4) Uani 1 1 d . . . . .
H7A H 0.619126 0.118779 0.201208 0.030 Uiso 1 1 calc R U . . .
C8 C 0.69355(15) 0.18331(10) 0.24173(6) 0.0258(4) Uani 1 1 d . . . . .
C9 C 0.68089(14) 0.22975(10) 0.27154(5) 0.0231(4) Uani 1 1 d . . . . .
H9 H 0.738930 0.251836 0.285271 0.028 Uiso 1 1 calc R U . . .
C10 C 0.58287(13) 0.24387(9) 0.28126(5) 0.0186(3) Uani 1 1 d . . . . .
C11 C 0.64898(13) 0.32564(10) 0.32931(5) 0.0221(3) Uani 1 1 d . . . . .
H11A H 0.684517 0.352284 0.310457 0.026 Uiso 1 1 calc R U . . .
H11B H 0.697593 0.290474 0.341807 0.026 Uiso 1 1 calc R U . . .
C12 C 0.61723(12) 0.37543(9) 0.35935(5) 0.0191(3) Uani 1 1 d . . . . .
C13 C 0.61115(12) 0.35065(9) 0.39691(5) 0.0190(3) Uani 1 1 d . . . . .
C14 C 0.59422(13) 0.39861(9) 0.42611(5) 0.0195(3) Uani 1 1 d . . . . .
C15 C 0.58021(13) 0.47043(9) 0.41771(5) 0.0194(3) Uani 1 1 d . . . . .
C16 C 0.58544(12) 0.49426(9) 0.37997(5) 0.0187(3) Uani 1 1 d . . . . .
C17 C 0.60271(12) 0.44682(9) 0.35057(5) 0.0180(3) Uani 1 1 d . . . . .
C18 C 0.60070(14) 0.37247(10) 0.46716(5) 0.0232(4) Uani 1 1 d . . . . .
H18A H 0.657728 0.338344 0.471904 0.028 Uiso 1 1 calc R U . . .
H18B H 0.615413 0.412528 0.485052 0.028 Uiso 1 1 calc R U . . .
C19 C 0.51196(13) 0.29741(9) 0.50694(5) 0.0203(3) Uani 1 1 d . . . . .
C20 C 0.59361(14) 0.29756(10) 0.53623(5) 0.0245(4) Uani 1 1 d . . . . .
H20 H 0.649382 0.329000 0.535021 0.029 Uiso 1 1 calc R U . . .
C21 C 0.59345(15) 0.25150(11) 0.56734(5) 0.0273(4) Uani 1 1 d . . . . .
H21 H 0.649241 0.251504 0.587238 0.033 Uiso 1 1 calc R U . . .
C22 C 0.51233(16) 0.20599(11) 0.56919(5) 0.0297(4) Uani 1 1 d . . . . .
H22 H 0.513411 0.173684 0.589972 0.036 Uiso 1 1 calc R U . . .
C23 C 0.42858(15) 0.20723(11) 0.54063(5) 0.0271(4) Uani 1 1 d . . . . .
H23 H 0.371950 0.176790 0.542433 0.033 Uiso 1 1 calc R U . . .
C24 C 0.42803(13) 0.25288(9) 0.50961(5) 0.0209(3) Uani 1 1 d . . . . .
C25 C 0.26550(13) 0.21227(9) 0.47477(5) 0.0201(3) Uani 1 1 d . . . . .
C26 C 0.24354(14) 0.13795(10) 0.48387(5) 0.0233(4) Uani 1 1 d . . . . .
C27 C 0.13861(14) 0.14734(9) 0.46189(5) 0.0215(3) Uani 1 1 d . . . . .
C28 C 0.16715(13) 0.22064(9) 0.45402(5) 0.0199(3) Uani 1 1 d . . . . .
C29 C 0.01372(13) 0.27043(9) 0.41720(5) 0.0205(3) Uani 1 1 d . . . . .
H29A H -0.030798 0.298339 0.432458 0.025 Uiso 1 1 calc R U . . .
H29B H -0.010182 0.220995 0.416734 0.025 Uiso 1 1 calc R U . . .
C30 C 0.00592(12) 0.29883(9) 0.37647(5) 0.0183(3) Uani 1 1 d . . . . .
C31 C -0.00798(12) 0.37132(9) 0.37032(5) 0.0174(3) Uani 1 1 d . . . . .
C32 C -0.01595(12) 0.39750(9) 0.33239(5) 0.0166(3) Uani 1 1 d . . . . .
C33 C -0.00531(12) 0.35233(9) 0.30131(5) 0.0173(3) Uani 1 1 d . . . . .
C34 C 0.01507(12) 0.28053(9) 0.30835(5) 0.0177(3) Uani 1 1 d . . . . .
C35 C 0.01982(12) 0.25330(9) 0.34582(5) 0.0185(3) Uani 1 1 d . . . . .
C36 C 0.04335(12) 0.23432(9) 0.27573(5) 0.0191(3) Uani 1 1 d . . . . .
H36A H 0.024263 0.184821 0.280121 0.023 Uiso 1 1 calc R U . . .
H36B H 0.006366 0.250115 0.250927 0.023 Uiso 1 1 calc R U . . .
C37 C -0.02652(12) 0.47608(9) 0.32605(5) 0.0178(3) Uani 1 1 d . . . . .
H37A H -0.062693 0.485415 0.300100 0.021 Uiso 1 1 calc R U . . .
H37B H -0.067493 0.496617 0.345323 0.021 Uiso 1 1 calc R U . . .
C38 C 0.09563(13) 0.56900(9) 0.34753(5) 0.0180(3) Uani 1 1 d . . . . .
C39 C 0.04029(14) 0.61686(10) 0.37101(5) 0.0231(4) Uani 1 1 d . . . . .
C40 C 0.13213(14) 0.66482(10) 0.37401(5) 0.0232(4) Uani 1 1 d . . . . .
C41 C 0.18175(13) 0.61398(9) 0.35050(4) 0.0177(3) Uani 1 1 d . . . . .
C42 C 0.34106(13) 0.66542(9) 0.33550(5) 0.0182(3) Uani 1 1 d . . . . .
C43 C 0.30781(14) 0.73235(9) 0.32439(5) 0.0214(3) Uani 1 1 d . . . . .
H43 H 0.236634 0.741246 0.318124 0.026 Uiso 1 1 calc R U . . .
C44 C 0.37824(15) 0.78668(9) 0.32237(5) 0.0240(4) Uani 1 1 d . . . . .
H44 H 0.355382 0.832695 0.315050 0.029 Uiso 1 1 calc R U . . .
C45 C 0.48153(15) 0.77299(9) 0.33112(5) 0.0242(4) Uani 1 1 d . . . . .
H45 H 0.529662 0.809850 0.329424 0.029 Uiso 1 1 calc R U . . .
C46 C 0.51660(14) 0.70585(9) 0.34242(5) 0.0224(3) Uani 1 1 d . . . . .
H46 H 0.587920 0.697081 0.348329 0.027 Uiso 1 1 calc R U . . .
C47 C 0.44610(13) 0.65218(9) 0.34492(5) 0.0185(3) Uani 1 1 d . . . . .
C48 C 0.57515(13) 0.57143(9) 0.37055(5) 0.0209(3) Uani 1 1 d . . . . .
H48A H 0.595681 0.599992 0.393852 0.025 Uiso 1 1 calc R U . . .
H48B H 0.619891 0.584101 0.350685 0.025 Uiso 1 1 calc R U . . .
C49 C 0.56116(15) 0.52236(10) 0.44915(5) 0.0270(4) Uani 1 1 d . . . . .
H49A H 0.524854 0.498026 0.468623 0.032 Uiso 1 1 calc R U . . .
H49B H 0.516182 0.560586 0.437781 0.032 Uiso 1 1 calc R U . . .
C50 C 0.66068(18) 0.55449(11) 0.46904(6) 0.0353(5) Uani 1 1 d . . . . .
H50A H 0.695144 0.580798 0.450155 0.053 Uiso 1 1 calc R U . . .
H50B H 0.705844 0.516843 0.480132 0.053 Uiso 1 1 calc R U . . .
H50C H 0.644621 0.586346 0.489556 0.053 Uiso 1 1 calc R U . . .
C51 C 0.60749(14) 0.47351(10) 0.30993(5) 0.0234(4) Uani 1 1 d . . . . .
H51A H 0.559830 0.513705 0.304957 0.028 Uiso 1 1 calc R U . . .
H51B H 0.584632 0.435744 0.291390 0.028 Uiso 1 1 calc R U . . .
C52 C 0.71597(15) 0.49697(11) 0.30333(6) 0.0290(4) Uani 1 1 d . . . . .
H52A H 0.715857 0.512817 0.276653 0.044 Uiso 1 1 calc R U . . .
H52B H 0.763464 0.457356 0.308243 0.044 Uiso 1 1 calc R U . . .
H52C H 0.737819 0.535714 0.320893 0.044 Uiso 1 1 calc R U . . .
C53 C 0.62348(14) 0.27267(9) 0.40559(5) 0.0248(4) Uani 1 1 d . . . . .
H53A H 0.594949 0.245689 0.382583 0.030 Uiso 1 1 calc R U . . .
H53B H 0.582873 0.260608 0.426824 0.030 Uiso 1 1 calc R U . . .
C54 C 0.73483(16) 0.24973(11) 0.41688(6) 0.0321(4) Uani 1 1 d . . . . .
H54A H 0.776168 0.262578 0.396345 0.048 Uiso 1 1 calc R U . . .
H54B H 0.737393 0.198649 0.420701 0.048 Uiso 1 1 calc R U . . .
H54C H 0.762127 0.273314 0.440831 0.048 Uiso 1 1 calc R U . . .
C55 C 0.03624(15) 0.17521(10) 0.35333(5) 0.0252(4) Uani 1 1 d . . . . .
H55A H 0.074084 0.168415 0.379248 0.030 Uiso 1 1 calc R U . . .
H55B H 0.078359 0.155511 0.334182 0.030 Uiso 1 1 calc R U . . .
C56 C -0.06628(18) 0.13573(11) 0.35083(7) 0.0375(5) Uani 1 1 d . . . . .
H56A H -0.101657 0.139671 0.324654 0.056 Uiso 1 1 calc R U . . .
H56B H -0.109045 0.156306 0.369120 0.056 Uiso 1 1 calc R U . . .
H56C H -0.053585 0.086019 0.357136 0.056 Uiso 1 1 calc R U . . .
C57 C -0.01954(13) 0.37890(9) 0.26001(5) 0.0201(3) Uani 1 1 d . . . . .
H57A H 0.030907 0.355881 0.245148 0.024 Uiso 1 1 calc R U . . .
H57B H -0.007345 0.430296 0.259701 0.024 Uiso 1 1 calc R U . . .
C58 C -0.12854(14) 0.36284(11) 0.24125(5) 0.0249(4) Uani 1 1 d . . . . .
H58A H -0.137185 0.380929 0.214825 0.037 Uiso 1 1 calc R U . . .
H58B H -0.178338 0.385482 0.256082 0.037 Uiso 1 1 calc R U . . .
H58C H -0.139709 0.311845 0.240873 0.037 Uiso 1 1 calc R U . . .
C59 C -0.01418(13) 0.42168(9) 0.40389(5) 0.0203(3) Uani 1 1 d . . . . .
H59A H 0.018773 0.466710 0.398140 0.024 Uiso 1 1 calc R U . . .
H59B H 0.025013 0.401532 0.427231 0.024 Uiso 1 1 calc R U . . .
C60 C -0.12408(14) 0.43660(11) 0.41237(5) 0.0267(4) Uani 1 1 d . . . . .
H60A H -0.163925 0.455718 0.389262 0.040 Uiso 1 1 calc R U . . .
H60B H -0.122797 0.470825 0.433395 0.040 Uiso 1 1 calc R U . . .
H60C H -0.155766 0.392806 0.419894 0.040 Uiso 1 1 calc R U . . .
N7 N 0.14755(12) -0.11187(8) 0.46023(4) 0.0247(3) Uani 1 1 d . . . . .
C61 C 0.04857(15) -0.07005(10) 0.45948(5) 0.0271(4) Uani 1 1 d . . . . .
H H 0.020882 -0.077224 0.484353 0.033 Uiso 1 1 calc R U . . .
HA H 0.065268 -0.019453 0.457613 0.033 Uiso 1 1 calc R U . . .
C62 C -0.03478(17) -0.08767(12) 0.42740(6) 0.0333(4) Uani 1 1 d . . . . .
HB H -0.057617 -0.136880 0.430126 0.040 Uiso 1 1 calc R U . . .
HC H -0.008002 -0.082993 0.402193 0.040 Uiso 1 1 calc R U . . .
C63 C -0.12514(17) -0.03752(12) 0.42926(6) 0.0371(5) Uani 1 1 d . . . . .
HD H -0.147264 -0.039707 0.455355 0.045 Uiso 1 1 calc R U . . .
HE H -0.102204 0.011187 0.424991 0.045 Uiso 1 1 calc R U . . .
C64 C -0.2155(2) -0.05436(18) 0.39996(8) 0.0565(7) Uani 1 1 d . . . . .
HF H -0.194023 -0.052715 0.374044 0.085 Uiso 1 1 calc R U . . .
HG H -0.269963 -0.019773 0.401909 0.085 Uiso 1 1 calc R U . . .
HH H -0.241057 -0.101552 0.404897 0.085 Uiso 1 1 calc R U . . .
C65 C 0.21390(16) -0.08819(11) 0.49644(5) 0.0286(4) Uani 1 1 d . . . . .
HI H 0.214358 -0.036104 0.496782 0.034 Uiso 1 1 calc R U . . .
HJ H 0.180566 -0.103988 0.518931 0.034 Uiso 1 1 calc R U . . .
C66 C 0.32406(17) -0.11322(13) 0.50193(6) 0.0351(5) Uani 1 1 d . . . . .
HK H 0.358637 -0.100628 0.479174 0.042 Uiso 1 1 calc R U . . .
HL H 0.326376 -0.165006 0.504979 0.042 Uiso 1 1 calc R U . . .
C67 C 0.37830(17) -0.07779(13) 0.53801(6) 0.0364(5) Uani 1 1 d . . . . .
HM H 0.371841 -0.026098 0.535150 0.044 Uiso 1 1 calc R U . . .
HN H 0.343940 -0.091816 0.560585 0.044 Uiso 1 1 calc R U . . .
C68 C 0.49063(19) -0.09699(15) 0.54529(7) 0.0471(6) Uani 1 1 d . . . . .
HO H 0.525457 -0.082067 0.523334 0.071 Uiso 1 1 calc R U . . .
HP H 0.497491 -0.148045 0.548576 0.071 Uiso 1 1 calc R U . . .
HQ H 0.521727 -0.073295 0.568676 0.071 Uiso 1 1 calc R U . . .
C69 C 0.19985(15) -0.09758(10) 0.42430(5) 0.0266(4) Uani 1 1 d . . . . .
HR H 0.265640 -0.123549 0.426735 0.032 Uiso 1 1 calc R U . . .
HS H 0.156266 -0.117227 0.401825 0.032 Uiso 1 1 calc R U . . .
C70 C 0.22150(16) -0.02131(11) 0.41595(6) 0.0296(4) Uani 1 1 d . . . . .
HT H 0.258938 0.000999 0.439032 0.035 Uiso 1 1 calc R U . . .
HU H 0.156211 0.004346 0.409352 0.035 Uiso 1 1 calc R U . . .
C71 C 0.28627(16) -0.01752(12) 0.38218(6) 0.0331(4) Uani 1 1 d . . . . .
HV H 0.356562 -0.034207 0.390894 0.040 Uiso 1 1 calc R U . . .
HW H 0.256356 -0.049246 0.361383 0.040 Uiso 1 1 calc R U . . .
C72 C 0.29156(18) 0.05613(13) 0.36645(7) 0.0405(5) Uani 1 1 d . . . . .
HX H 0.336307 0.056630 0.345888 0.061 Uiso 1 1 calc R U . . .
HY H 0.319186 0.088006 0.387138 0.061 Uiso 1 1 calc R U . . .
HZ H 0.222638 0.071619 0.356117 0.061 Uiso 1 1 calc R U . . .
C73 C 0.12795(16) -0.19101(10) 0.45987(5) 0.0271(4) Uani 1 1 d . . . . .
H8 H 0.094139 -0.203948 0.434036 0.032 Uiso 1 1 calc R U . . .
H10 H 0.195149 -0.215206 0.463391 0.032 Uiso 1 1 calc R U . . .
C74 C 0.06315(17) -0.21965(11) 0.48974(6) 0.0326(4) Uani 1 1 d . . . . .
H11 H 0.003169 -0.188624 0.491205 0.039 Uiso 1 1 calc R U . . .
H12 H 0.104195 -0.220026 0.515350 0.039 Uiso 1 1 calc R U . . .
C75 C 0.02633(18) -0.29441(12) 0.47922(6) 0.0351(5) Uani 1 1 d . . . . .
H13 H -0.022683 -0.308918 0.497215 0.042 Uiso 1 1 calc R U . . .
H14 H -0.011429 -0.293496 0.453013 0.042 Uiso 1 1 calc R U . . .
C76 C 0.10993(19) -0.34954(13) 0.48018(7) 0.0415(5) Uani 1 1 d . . . . .
H15 H 0.158081 -0.336650 0.461932 0.062 Uiso 1 1 calc R U . . .
H16 H 0.079220 -0.395372 0.473012 0.062 Uiso 1 1 calc R U . . .
H17 H 0.146564 -0.352273 0.506204 0.062 Uiso 1 1 calc R U . . .
O16 O 0.7696(15) 0.6816(9) 0.3864(6) 0.095(5) Uani 0.42(2) 1 d D U P C 1
H18 H 0.819982 0.654330 0.386819 0.143 Uiso 0.42(2) 1 calc R U P C 1
O16A O 0.7662(10) 0.6774(4) 0.3722(4) 0.068(2) Uani 0.58(2) 1 d D U P C 2
H19 H 0.818335 0.652192 0.377815 0.102 Uiso 0.58(2) 1 calc R U P C 2
C81 C 0.7930(9) 0.7486(6) 0.3673(6) 0.076(4) Uani 0.42(2) 1 d D U P C 1
H24 H 0.805800 0.739054 0.340768 0.114 Uiso 0.42(2) 1 calc R U P C 1
H25 H 0.853964 0.770225 0.381410 0.114 Uiso 0.42(2) 1 calc R U P C 1
H26 H 0.734625 0.780795 0.367250 0.114 Uiso 0.42(2) 1 calc R U P C 1
C81A C 0.7845(8) 0.7486(6) 0.3898(6) 0.088(4) Uani 0.58(2) 1 d D U P C 2
H27 H 0.723372 0.777887 0.383491 0.133 Uiso 0.58(2) 1 calc R U P C 2
H28 H 0.843182 0.770704 0.379650 0.133 Uiso 0.58(2) 1 calc R U P C 2
H29 H 0.798768 0.743954 0.417829 0.133 Uiso 0.58(2) 1 calc R U P C 2
Cl4 Cl 0.44686(4) 0.31985(3) 0.16606(2) 0.03696(13) Uani 0.9546(8) 1 d D U P D 1
Cl4A Cl 0.4061(8) 0.3473(6) 0.1827(3) 0.03696(13) Uani 0.0454(8) 1 d D U P D 2
Cl5 Cl 0.63060(5) 0.37754(4) 0.20769(2) 0.05221(18) Uani 0.9546(8) 1 d D U P D 1
Cl5A Cl 0.6283(9) 0.3291(8) 0.1881(4) 0.05221(18) Uani 0.0454(8) 1 d D U P D 2
Cl6 Cl 0.46823(6) 0.46975(3) 0.17650(2) 0.05006(17) Uani 0.9546(8) 1 d D U P D 1
Cl6A Cl 0.5440(12) 0.4638(6) 0.1936(4) 0.05006(17) Uani 0.0454(8) 1 d D U P D 2
C77 C 0.49791(17) 0.38629(12) 0.19718(6) 0.0343(5) Uani 1 1 d D . . D 1
H30 H 0.4674(18) 0.3830(13) 0.2216(7) 0.032(6) Uiso 1 1 d . . . E 1
C77A C 0.5277(15) 0.3749(11) 0.2061(10) 0.038 Uiso 0.0454(8) 1 d D U P D 2
H31 H 0.530896 0.369298 0.234630 0.046 Uiso 0.0454(8) 1 calc R U P D 2
P1 P 0.29024(3) 0.41899(2) 0.28151(2) 0.01886(10) Uani 1 1 d . . . . .
O10 O 0.30160(10) 0.34340(6) 0.29378(4) 0.0231(3) Uani 1 1 d D . . . .
O11 O 0.26402(10) 0.47064(7) 0.31108(4) 0.0253(3) Uani 1 1 d . . . . .
O12 O 0.39305(10) 0.44019(7) 0.26533(4) 0.0238(3) Uani 1 1 d . . . . .
H32 H 0.391(2) 0.4778(17) 0.2577(9) 0.050(9) Uiso 1 1 d . . . . .
O13 O 0.20504(10) 0.42080(7) 0.24544(4) 0.0280(3) Uani 1 1 d . . . . .
H33 H 0.181(3) 0.4578(19) 0.2424(10) 0.069(11) Uiso 1 1 d . . . . .
O15 O 0.35616(16) 0.31078(9) 0.36963(5) 0.0480(4) Uani 1 1 d . . . . .
H34 H 0.335969 0.326715 0.347638 0.072 Uiso 1 1 calc DR U . . .
C80 C 0.3414(2) 0.23835(13) 0.36988(6) 0.0401(5) Uani 1 1 d . . . . .
H35 H 0.387017 0.215822 0.353274 0.060 Uiso 1 1 calc R U . . .
H36 H 0.269959 0.227588 0.360304 0.060 Uiso 1 1 calc R U . . .
H37 H 0.356720 0.220592 0.396234 0.060 Uiso 1 1 calc R U . . .
O14 O 0.27377(11) 0.37368(8) 0.42597(4) 0.0304(3) Uani 1 1 d . . . . .
H38 H 0.301(2) 0.3526(17) 0.4065(9) 0.055(8) Uiso 1 1 d . . . . .
C79 C 0.2804(2) 0.44816(12) 0.42133(7) 0.0416(5) Uani 1 1 d . . . . .
H39 H 0.256509 0.460755 0.394605 0.062 Uiso 1 1 calc R U . . .
H40 H 0.351795 0.463209 0.427571 0.062 Uiso 1 1 calc R U . . .
H41 H 0.237518 0.471610 0.438613 0.062 Uiso 1 1 calc R U . . .
Cl1 Cl 0.57618(5) 0.11286(3) 0.35133(2) 0.04203(13) Uani 1 1 d . . . . .
Cl2 Cl 0.52763(4) -0.03356(3) 0.33708(2) 0.03622(12) Uani 1 1 d . . . . .
Cl3 Cl 0.69825(4) 0.03039(3) 0.30421(2) 0.03897(12) Uani 1 1 d . . . . .
C78 C 0.57476(15) 0.04378(10) 0.31762(5) 0.0269(4) Uani 1 1 d . . . . .
H42 H 0.527819 0.057116 0.294151 0.032 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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 2 -22 0.0290
0 -2 22 0.0290
-8 0 6 0.0697
8 0 -6 0.0697
-2 8 -16 0.0705
2 -8 16 0.0705
0 -12 -3 0.0821
0 12 3 0.0991
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
C8 Cl7 H7 6(2) . . ?
C10 O3 C11 115.13(13) . . ?
C19 O4 C18 115.57(13) . . ?
C47 O5 C48 115.96(13) . . ?
C1 N1 H1 116.8(17) . . ?
C1 N1 C36 123.76(15) . . ?
C36 N1 H1 119.4(17) . . ?
C4 N2 H2 117.2(17) . . ?
C4 N2 C5 123.90(15) . . ?
C5 N2 H2 118.7(17) . . ?
C28 N3 H3 118.8(18) . . ?
C28 N3 C29 122.94(16) . . ?
C29 N3 H3 118.1(17) . . ?
C24 N4 H4 117.8(18) . . ?
C25 N4 H4 115.6(18) . . ?
C25 N4 C24 125.91(16) . . ?
C37 N5 H5 120.5(18) . . ?
C38 N5 H5 116.6(18) . . ?
C38 N5 C37 122.90(15) . . ?
C41 N6 H6 117.0(15) . . ?
C41 N6 C42 123.42(15) . . ?
C42 N6 H6 119.6(15) . . ?
N1 C1 C2 134.36(16) . . ?
N1 C1 C4 134.12(16) . . ?
C4 C1 C2 91.50(13) . . ?
O1 C2 C1 133.88(16) . . ?
O1 C2 C3 137.81(16) . . ?
C1 C2 C3 88.30(13) . . ?
O2 C3 C2 135.87(16) . . ?
O2 C3 C4 135.31(16) . . ?
C4 C3 C2 88.72(13) . . ?
N2 C4 C1 132.13(16) . . ?
N2 C4 C3 136.50(16) . . ?
C1 C4 C3 91.29(13) . . ?
C6 C5 N2 121.00(15) . . ?
C6 C5 C10 119.81(15) . . ?
C10 C5 N2 119.16(14) . . ?
C5 C6 H6A 119.7 . . ?
C7 C6 C5 120.61(16) . . ?
C7 C6 H6A 119.7 . . ?
C6 C7 H7A 120.3 . . ?
C8 C7 C6 119.48(16) . . ?
C8 C7 H7A 120.3 . . ?
Cl7 C8 H7 5.6(18) . . ?
C7 C8 Cl7 120.6(4) . . ?
C7 C8 H7 119.1(17) . . ?
C7 C8 C9 120.77(17) . . ?
C9 C8 Cl7 118.4(4) . . ?
C9 C8 H7 120.1(17) . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 119.92(17) . . ?
C10 C9 H9 120.0 . . ?
O3 C10 C5 115.76(14) . . ?
O3 C10 C9 124.85(15) . . ?
C9 C10 C5 119.39(15) . . ?
O3 C11 H11A 109.4 . . ?
O3 C11 H11B 109.4 . . ?
O3 C11 C12 111.08(13) . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 H11A 109.4 . . ?
C12 C11 H11B 109.4 . . ?
C13 C12 C11 119.38(16) . . ?
C17 C12 C11 119.82(15) . . ?
C17 C12 C13 120.57(15) . . ?
C12 C13 C53 119.83(15) . . ?
C14 C13 C12 119.49(16) . . ?
C14 C13 C53 120.68(16) . . ?
C13 C14 C18 118.71(16) . . ?
C15 C14 C13 120.43(16) . . ?
C15 C14 C18 120.65(15) . . ?
C14 C15 C16 119.39(15) . . ?
C14 C15 C49 120.59(16) . . ?
C16 C15 C49 120.02(16) . . ?
C15 C16 C17 120.67(16) . . ?
C15 C16 C48 120.45(15) . . ?
C17 C16 C48 118.86(15) . . ?
C12 C17 C16 119.41(15) . . ?
C12 C17 C51 120.69(15) . . ?
C16 C17 C51 119.89(16) . . ?
O4 C18 C14 111.04(14) . . ?
O4 C18 H18A 109.4 . . ?
O4 C18 H18B 109.4 . . ?
C14 C18 H18A 109.4 . . ?
C14 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
O4 C19 C20 124.62(16) . . ?
O4 C19 C24 115.63(15) . . ?
C20 C19 C24 119.75(16) . . ?
C19 C20 H20 120.0 . . ?
C19 C20 C21 120.02(18) . . ?
C21 C20 H20 120.0 . . ?
C20 C21 H21 120.0 . . ?
C22 C21 C20 120.05(17) . . ?
C22 C21 H21 120.0 . . ?
C21 C22 H22 119.9 . . ?
C21 C22 C23 120.25(17) . . ?
C23 C22 H22 119.9 . . ?
C22 C23 H23 120.0 . . ?
C24 C23 C22 120.08(18) . . ?
C24 C23 H23 120.0 . . ?
C19 C24 N4 117.89(15) . . ?
C23 C24 N4 122.30(17) . . ?
C23 C24 C19 119.77(16) . . ?
N4 C25 C26 138.43(16) . . ?
N4 C25 C28 129.91(16) . . ?
C28 C25 C26 91.63(14) . . ?
O7 C26 C25 137.90(18) . . ?
O7 C26 C27 133.99(18) . . ?
C25 C26 C27 88.11(14) . . ?
O6 C27 C26 135.87(17) . . ?
O6 C27 C28 135.85(17) . . ?
C28 C27 C26 88.28(14) . . ?
N3 C28 C25 133.31(17) . . ?
N3 C28 C27 134.70(17) . . ?
C25 C28 C27 91.98(14) . . ?
N3 C29 H29A 109.6 . . ?
N3 C29 H29B 109.6 . . ?
N3 C29 C30 110.19(14) . . ?
H29A C29 H29B 108.1 . . ?
C30 C29 H29A 109.6 . . ?
C30 C29 H29B 109.6 . . ?
C31 C30 C29 119.16(15) . . ?
C31 C30 C35 120.90(15) . . ?
C35 C30 C29 119.78(15) . . ?
C30 C31 C32 119.03(15) . . ?
C30 C31 C59 121.08(15) . . ?
C32 C31 C59 119.89(15) . . ?
C31 C32 C37 118.80(15) . . ?
C33 C32 C31 120.61(15) . . ?
C33 C32 C37 120.36(14) . . ?
C32 C33 C34 119.45(15) . . ?
C32 C33 C57 121.29(15) . . ?
C34 C33 C57 119.22(15) . . ?
C33 C34 C36 119.18(14) . . ?
C35 C34 C33 120.53(15) . . ?
C35 C34 C36 119.96(15) . . ?
C30 C35 C55 119.88(15) . . ?
C34 C35 C30 119.28(16) . . ?
C34 C35 C55 120.80(15) . . ?
N1 C36 C34 107.77(13) . . ?
N1 C36 H36A 110.2 . . ?
N1 C36 H36B 110.2 . . ?
C34 C36 H36A 110.2 . . ?
C34 C36 H36B 110.2 . . ?
H36A C36 H36B 108.5 . . ?
N5 C37 C32 109.82(13) . . ?
N5 C37 H37A 109.7 . . ?
N5 C37 H37B 109.7 . . ?
C32 C37 H37A 109.7 . . ?
C32 C37 H37B 109.7 . . ?
H37A C37 H37B 108.2 . . ?
N5 C38 C39 135.62(16) . . ?
N5 C38 C41 132.75(16) . . ?
C41 C38 C39 91.61(14) . . ?
O8 C39 C38 134.70(18) . . ?
O8 C39 C40 137.00(17) . . ?
C38 C39 C40 88.25(14) . . ?
O9 C40 C39 136.14(17) . . ?
O9 C40 C41 135.78(18) . . ?
C41 C40 C39 88.08(14) . . ?
N6 C41 C38 131.62(15) . . ?
N6 C41 C40 136.32(16) . . ?
C38 C41 C40 92.05(14) . . ?
C43 C42 N6 121.94(16) . . ?
C43 C42 C47 119.97(16) . . ?
C47 C42 N6 118.07(15) . . ?
C42 C43 H43 119.8 . . ?
C42 C43 C44 120.33(17) . . ?
C44 C43 H43 119.8 . . ?
C43 C44 H44 120.3 . . ?
C45 C44 C43 119.35(17) . . ?
C45 C44 H44 120.3 . . ?
C44 C45 H45 119.4 . . ?
C44 C45 C46 121.19(17) . . ?
C46 C45 H45 119.4 . . ?
C45 C46 H46 120.4 . . ?
C47 C46 C45 119.25(17) . . ?
C47 C46 H46 120.4 . . ?
O5 C47 C42 114.63(14) . . ?
O5 C47 C46 125.46(16) . . ?
C46 C47 C42 119.90(16) . . ?
O5 C48 C16 107.67(13) . . ?
O5 C48 H48A 110.2 . . ?
O5 C48 H48B 110.2 . . ?
C16 C48 H48A 110.2 . . ?
C16 C48 H48B 110.2 . . ?
H48A C48 H48B 108.5 . . ?
C15 C49 H49A 109.1 . . ?
C15 C49 H49B 109.1 . . ?
C15 C49 C50 112.54(16) . . ?
H49A C49 H49B 107.8 . . ?
C50 C49 H49A 109.1 . . ?
C50 C49 H49B 109.1 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C17 C51 H51A 109.2 . . ?
C17 C51 H51B 109.2 . . ?
C17 C51 C52 112.20(14) . . ?
H51A C51 H51B 107.9 . . ?
C52 C51 H51A 109.2 . . ?
C52 C51 H51B 109.2 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C13 C53 H53A 108.8 . . ?
C13 C53 H53B 108.8 . . ?
C13 C53 C54 113.93(15) . . ?
H53A C53 H53B 107.7 . . ?
C54 C53 H53A 108.8 . . ?
C54 C53 H53B 108.8 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C35 C55 H55A 109.4 . . ?
C35 C55 H55B 109.4 . . ?
C35 C55 C56 111.22(16) . . ?
H55A C55 H55B 108.0 . . ?
C56 C55 H55A 109.4 . . ?
C56 C55 H55B 109.4 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C33 C57 H57A 109.6 . . ?
C33 C57 H57B 109.6 . . ?
C33 C57 C58 110.20(14) . . ?
H57A C57 H57B 108.1 . . ?
C58 C57 H57A 109.6 . . ?
C58 C57 H57B 109.6 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C31 C59 H59A 108.8 . . ?
C31 C59 H59B 108.8 . . ?
C31 C59 C60 113.64(14) . . ?
H59A C59 H59B 107.7 . . ?
C60 C59 H59A 108.8 . . ?
C60 C59 H59B 108.8 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C61 N7 C69 111.02(14) . . ?
C61 N7 C73 111.83(15) . . ?
C65 N7 C61 105.41(14) . . ?
C65 N7 C69 111.36(15) . . ?
C65 N7 C73 112.26(14) . . ?
C69 N7 C73 105.10(13) . . ?
N7 C61 H 108.3 . . ?
N7 C61 HA 108.3 . . ?
H C61 HA 107.4 . . ?
C62 C61 N7 116.15(15) . . ?
C62 C61 H 108.3 . . ?
C62 C61 HA 108.3 . . ?
C61 C62 HB 109.8 . . ?
C61 C62 HC 109.8 . . ?
C61 C62 C63 109.20(17) . . ?
HB C62 HC 108.3 . . ?
C63 C62 HB 109.8 . . ?
C63 C62 HC 109.8 . . ?
C62 C63 HD 109.0 . . ?
C62 C63 HE 109.0 . . ?
HD C63 HE 107.8 . . ?
C64 C63 C62 113.0(2) . . ?
C64 C63 HD 109.0 . . ?
C64 C63 HE 109.0 . . ?
C63 C64 HF 109.5 . . ?
C63 C64 HG 109.5 . . ?
C63 C64 HH 109.5 . . ?
HF C64 HG 109.5 . . ?
HF C64 HH 109.5 . . ?
HG C64 HH 109.5 . . ?
N7 C65 HI 108.0 . . ?
N7 C65 HJ 108.0 . . ?
HI C65 HJ 107.2 . . ?
C66 C65 N7 117.37(15) . . ?
C66 C65 HI 108.0 . . ?
C66 C65 HJ 108.0 . . ?
C65 C66 HK 110.1 . . ?
C65 C66 HL 110.1 . . ?
C65 C66 C67 108.21(17) . . ?
HK C66 HL 108.4 . . ?
C67 C66 HK 110.1 . . ?
C67 C66 HL 110.1 . . ?
C66 C67 HM 109.1 . . ?
C66 C67 HN 109.1 . . ?
HM C67 HN 107.8 . . ?
C68 C67 C66 112.57(19) . . ?
C68 C67 HM 109.1 . . ?
C68 C67 HN 109.1 . . ?
C67 C68 HO 109.5 . . ?
C67 C68 HP 109.5 . . ?
C67 C68 HQ 109.5 . . ?
HO C68 HP 109.5 . . ?
HO C68 HQ 109.5 . . ?
HP C68 HQ 109.5 . . ?
N7 C69 HR 108.2 . . ?
N7 C69 HS 108.2 . . ?
HR C69 HS 107.4 . . ?
C70 C69 N7 116.28(15) . . ?
C70 C69 HR 108.2 . . ?
C70 C69 HS 108.2 . . ?
C69 C70 HT 109.9 . . ?
C69 C70 HU 109.9 . . ?
C69 C70 C71 109.08(16) . . ?
HT C70 HU 108.3 . . ?
C71 C70 HT 109.9 . . ?
C71 C70 HU 109.9 . . ?
C70 C71 HV 109.2 . . ?
C70 C71 HW 109.2 . . ?
HV C71 HW 107.9 . . ?
C72 C71 C70 112.15(18) . . ?
C72 C71 HV 109.2 . . ?
C72 C71 HW 109.2 . . ?
C71 C72 HX 109.5 . . ?
C71 C72 HY 109.5 . . ?
C71 C72 HZ 109.5 . . ?
HX C72 HY 109.5 . . ?
HX C72 HZ 109.5 . . ?
HY C72 HZ 109.5 . . ?
N7 C73 H8 108.0 . . ?
N7 C73 H10 108.0 . . ?
H8 C73 H10 107.3 . . ?
C74 C73 N7 117.00(15) . . ?
C74 C73 H8 108.0 . . ?
C74 C73 H10 108.0 . . ?
C73 C74 H11 109.5 . . ?
C73 C74 H12 109.5 . . ?
C73 C74 C75 110.67(16) . . ?
H11 C74 H12 108.1 . . ?
C75 C74 H11 109.5 . . ?
C75 C74 H12 109.5 . . ?
C74 C75 H13 108.4 . . ?
C74 C75 H14 108.4 . . ?
H13 C75 H14 107.5 . . ?
C76 C75 C74 115.4(2) . . ?
C76 C75 H13 108.4 . . ?
C76 C75 H14 108.4 . . ?
C75 C76 H15 109.5 . . ?
C75 C76 H16 109.5 . . ?
C75 C76 H17 109.5 . . ?
H15 C76 H16 109.5 . . ?
H15 C76 H17 109.5 . . ?
H16 C76 H17 109.5 . . ?
C81 O16 H18 109.5 . . ?
C81A O16A H19 109.5 . . ?
O16 C81 H24 109.5 . . ?
O16 C81 H25 109.5 . . ?
O16 C81 H26 109.5 . . ?
H24 C81 H25 109.5 . . ?
H24 C81 H26 109.5 . . ?
H25 C81 H26 109.5 . . ?
O16A C81A H27 109.5 . . ?
O16A C81A H28 109.5 . . ?
O16A C81A H29 109.5 . . ?
H27 C81A H28 109.5 . . ?
H27 C81A H29 109.5 . . ?
H28 C81A H29 109.5 . . ?
Cl4 C77 Cl6 110.05(12) . . ?
Cl4 C77 H30 109.2(14) . . ?
Cl5 C77 Cl4 111.30(13) . . ?
Cl5 C77 Cl6 109.79(12) . . ?
Cl5 C77 H30 107.9(14) . . ?
Cl6 C77 H30 108.5(14) . . ?
Cl4A C77A H31 110.9 . . ?
Cl5A C77A Cl4A 111.1(15) . . ?
Cl5A C77A Cl6A 105.6(14) . . ?
Cl5A C77A H31 110.9 . . ?
Cl6A C77A Cl4A 107.3(14) . . ?
Cl6A C77A H31 110.9 . . ?
O10 P1 O12 106.64(7) . . ?
O10 P1 O13 106.58(8) . . ?
O11 P1 O10 116.99(8) . . ?
O11 P1 O12 110.88(7) . . ?
O11 P1 O13 109.75(8) . . ?
O12 P1 O13 105.29(8) . . ?
P1 O12 H32 111(2) . . ?
P1 O13 H33 112(3) . . ?
C80 O15 H34 109.5 . . ?
O15 C80 H35 109.5 . . ?
O15 C80 H36 109.5 . . ?
O15 C80 H37 109.5 . . ?
H35 C80 H36 109.5 . . ?
H35 C80 H37 109.5 . . ?
H36 C80 H37 109.5 . . ?
C79 O14 H38 109(2) . . ?
O14 C79 H39 109.5 . . ?
O14 C79 H40 109.5 . . ?
O14 C79 H41 109.5 . . ?
H39 C79 H40 109.5 . . ?
H39 C79 H41 109.5 . . ?
H40 C79 H41 109.5 . . ?
Cl1 C78 H42 108.5 . . ?
Cl2 C78 Cl1 109.88(10) . . ?
Cl2 C78 H42 108.5 . . ?
Cl3 C78 Cl1 110.35(11) . . ?
Cl3 C78 Cl2 111.01(11) . . ?
Cl3 C78 H42 108.5 . . ?
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
Cl7 H7 0.80(3) . ?
Cl7 C8 1.699(14) . ?
O1 C2 1.227(2) . ?
O2 C3 1.240(2) . ?
O3 C10 1.373(2) . ?
O3 C11 1.443(2) . ?
O4 C18 1.445(2) . ?
O4 C19 1.377(2) . ?
O5 C47 1.368(2) . ?
O5 C48 1.441(2) . ?
O6 C27 1.224(2) . ?
O7 C26 1.221(2) . ?
O8 C39 1.225(2) . ?
O9 C40 1.225(2) . ?
N1 H1 0.81(3) . ?
N1 C1 1.309(2) . ?
N1 C36 1.473(2) . ?
N2 H2 0.80(3) . ?
N2 C4 1.333(2) . ?
N2 C5 1.417(2) . ?
N3 H3 0.80(3) . ?
N3 C28 1.320(2) . ?
N3 C29 1.468(2) . ?
N4 H4 0.77(3) . ?
N4 C24 1.412(2) . ?
N4 C25 1.345(2) . ?
N5 H5 0.80(3) . ?
N5 C37 1.464(2) . ?
N5 C38 1.318(2) . ?
N6 H6 0.85(2) . ?
N6 C41 1.332(2) . ?
N6 C42 1.417(2) . ?
C1 C2 1.466(2) . ?
C1 C4 1.427(2) . ?
C2 C3 1.501(2) . ?
C3 C4 1.463(2) . ?
C5 C6 1.392(2) . ?
C5 C10 1.401(2) . ?
C6 H6A 0.9500 . ?
C6 C7 1.386(3) . ?
C7 H7A 0.9500 . ?
C7 C8 1.384(3) . ?
C8 H7 0.91(3) . ?
C8 C9 1.390(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.395(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.508(2) . ?
C12 C13 1.406(2) . ?
C12 C17 1.399(2) . ?
C13 C14 1.406(2) . ?
C13 C53 1.518(2) . ?
C14 C15 1.404(2) . ?
C14 C18 1.511(2) . ?
C15 C16 1.404(2) . ?
C15 C49 1.519(2) . ?
C16 C17 1.406(2) . ?
C16 C48 1.506(2) . ?
C17 C51 1.517(2) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.394(2) . ?
C19 C24 1.401(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.396(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.379(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.397(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.388(3) . ?
C25 C26 1.483(2) . ?
C25 C28 1.415(2) . ?
C26 C27 1.508(3) . ?
C27 C28 1.477(2) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.515(2) . ?
C30 C31 1.403(2) . ?
C30 C35 1.406(2) . ?
C31 C32 1.409(2) . ?
C31 C59 1.524(2) . ?
C32 C33 1.404(2) . ?
C32 C37 1.514(2) . ?
C33 C34 1.407(2) . ?
C33 C57 1.521(2) . ?
C34 C35 1.403(2) . ?
C34 C36 1.519(2) . ?
C35 C55 1.518(2) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.472(2) . ?
C38 C41 1.412(2) . ?
C39 C40 1.506(3) . ?
C40 C41 1.469(2) . ?
C42 C43 1.386(2) . ?
C42 C47 1.403(2) . ?
C43 H43 0.9500 . ?
C43 C44 1.393(3) . ?
C44 H44 0.9500 . ?
C44 C45 1.380(3) . ?
C45 H45 0.9500 . ?
C45 C46 1.398(3) . ?
C46 H46 0.9500 . ?
C46 C47 1.387(2) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C50 1.534(3) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C51 C52 1.535(2) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C54 1.533(3) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C55 C56 1.535(3) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C57 C58 1.534(2) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C59 C60 1.533(2) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
N7 C61 1.521(2) . ?
N7 C65 1.519(2) . ?
N7 C69 1.524(2) . ?
N7 C73 1.526(2) . ?
C61 H 0.9900 . ?
C61 HA 0.9900 . ?
C61 C62 1.511(3) . ?
C62 HB 0.9900 . ?
C62 HC 0.9900 . ?
C62 C63 1.529(3) . ?
C63 HD 0.9900 . ?
C63 HE 0.9900 . ?
C63 C64 1.509(4) . ?
C64 HF 0.9800 . ?
C64 HG 0.9800 . ?
C64 HH 0.9800 . ?
C65 HI 0.9900 . ?
C65 HJ 0.9900 . ?
C65 C66 1.514(3) . ?
C66 HK 0.9900 . ?
C66 HL 0.9900 . ?
C66 C67 1.531(3) . ?
C67 HM 0.9900 . ?
C67 HN 0.9900 . ?
C67 C68 1.512(3) . ?
C68 HO 0.9800 . ?
C68 HP 0.9800 . ?
C68 HQ 0.9800 . ?
C69 HR 0.9900 . ?
C69 HS 0.9900 . ?
C69 C70 1.512(3) . ?
C70 HT 0.9900 . ?
C70 HU 0.9900 . ?
C70 C71 1.535(3) . ?
C71 HV 0.9900 . ?
C71 HW 0.9900 . ?
C71 C72 1.508(3) . ?
C72 HX 0.9800 . ?
C72 HY 0.9800 . ?
C72 HZ 0.9800 . ?
C73 H8 0.9900 . ?
C73 H10 0.9900 . ?
C73 C74 1.522(3) . ?
C74 H11 0.9900 . ?
C74 H12 0.9900 . ?
C74 C75 1.532(3) . ?
C75 H13 0.9900 . ?
C75 H14 0.9900 . ?
C75 C76 1.515(3) . ?
C76 H15 0.9800 . ?
C76 H16 0.9800 . ?
C76 H17 0.9800 . ?
O16 H18 0.8400 . ?
O16 C81 1.486(8) . ?
O16A H19 0.8400 . ?
O16A C81A 1.494(7) . ?
C81 H24 0.9800 . ?
C81 H25 0.9800 . ?
C81 H26 0.9800 . ?
C81A H27 0.9800 . ?
C81A H28 0.9800 . ?
C81A H29 0.9800 . ?
Cl4 C77 1.749(2) . ?
Cl4A C77A 1.79(2) . ?
Cl5 C77 1.746(2) . ?
Cl5A C77A 1.76(2) . ?
Cl6 C77 1.768(2) . ?
Cl6A C77A 1.76(2) . ?
C77 H30 0.99(2) . ?
C77A H31 1.0000 . ?
P1 O10 1.5016(13) . ?
P1 O11 1.4946(13) . ?
P1 O12 1.5755(13) . ?
P1 O13 1.5860(14) . ?
O12 H32 0.76(3) . ?
O13 H33 0.77(4) . ?
O15 H34 0.8400 . ?
O15 C80 1.390(3) . ?
C80 H35 0.9800 . ?
C80 H36 0.9800 . ?
C80 H37 0.9800 . ?
O14 H38 0.90(3) . ?
O14 C79 1.429(3) . ?
C79 H39 0.9800 . ?
C79 H40 0.9800 . ?
C79 H41 0.9800 . ?
Cl1 C78 1.7628(19) . ?
Cl2 C78 1.762(2) . ?
Cl3 C78 1.758(2) . ?
C78 H42 1.0000 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 O10 0.81(3) 2.02(3) 2.777(2) 156(2) . yes
N2 H2 O10 0.80(3) 2.00(3) 2.7557(19) 158(2) . yes
N3 H3 O14 0.80(3) 2.05(3) 2.812(2) 161(2) . yes
N4 H4 O14 0.77(3) 2.25(3) 2.987(2) 161(2) . yes
N5 H5 O11 0.80(3) 1.98(3) 2.734(2) 158(2) . yes
N6 H6 O11 0.85(2) 1.96(3) 2.7672(19) 157(2) . yes
O16 H18 O8 0.84 1.96 2.78(2) 163.5 1_655 yes
O16A H19 O8 0.84 1.94 2.753(13) 163.6 1_655 yes
O12 H32 O1 0.76(3) 1.91(3) 2.6694(19) 175(3) 2 yes
O13 H33 O2 0.77(4) 1.91(4) 2.6817(19) 176(4) 2 yes
O15 H34 O10 0.84 1.91 2.736(2) 167.1 . yes
O14 H38 O15 0.90(3) 1.74(3) 2.641(2) 178(3) . yes
C78 H42 O2 1.00 2.24 3.126(2) 147.5 . yes
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
Cl7 C8 C9 C10 -175.8(5) . . . . ?
O1 C2 C3 O2 -5.3(4) . . . . ?
O1 C2 C3 C4 178.0(2) . . . . ?
O2 C3 C4 N2 3.5(3) . . . . ?
O2 C3 C4 C1 -173.5(2) . . . . ?
O3 C11 C12 C13 89.01(19) . . . . ?
O3 C11 C12 C17 -96.44(18) . . . . ?
O4 C19 C20 C21 -178.03(16) . . . . ?
O4 C19 C24 N4 -4.2(2) . . . . ?
O4 C19 C24 C23 177.94(16) . . . . ?
O6 C27 C28 N3 0.4(4) . . . . ?
O6 C27 C28 C25 180.0(2) . . . . ?
O7 C26 C27 O6 0.9(4) . . . . ?
O7 C26 C27 C28 -178.8(2) . . . . ?
O8 C39 C40 O9 -2.0(4) . . . . ?
O8 C39 C40 C41 177.5(2) . . . . ?
O9 C40 C41 N6 0.6(4) . . . . ?
O9 C40 C41 C38 179.6(2) . . . . ?
N1 C1 C2 O1 3.4(3) . . . . ?
N1 C1 C2 C3 -175.42(19) . . . . ?
N1 C1 C4 N2 -1.9(3) . . . . ?
N1 C1 C4 C3 175.34(19) . . . . ?
N2 C5 C6 C7 178.51(16) . . . . ?
N2 C5 C10 O3 0.4(2) . . . . ?
N2 C5 C10 C9 -179.52(15) . . . . ?
N3 C29 C30 C31 -86.68(18) . . . . ?
N3 C29 C30 C35 88.87(19) . . . . ?
N4 C25 C26 O7 0.7(4) . . . . ?
N4 C25 C26 C27 -178.3(2) . . . . ?
N4 C25 C28 N3 -1.8(3) . . . . ?
N4 C25 C28 C27 178.60(18) . . . . ?
N5 C38 C39 O8 3.9(4) . . . . ?
N5 C38 C39 C40 -178.4(2) . . . . ?
N5 C38 C41 N6 -2.5(3) . . . . ?
N5 C38 C41 C40 178.42(19) . . . . ?
N6 C42 C43 C44 -178.18(15) . . . . ?
N6 C42 C47 O5 -3.2(2) . . . . ?
N6 C42 C47 C46 177.32(15) . . . . ?
C1 N1 C36 C34 139.09(16) . . . . ?
C1 C2 C3 O2 173.5(2) . . . . ?
C1 C2 C3 C4 -3.19(12) . . . . ?
C2 C1 C4 N2 179.44(18) . . . . ?
C2 C1 C4 C3 -3.35(13) . . . . ?
C2 C3 C4 N2 -179.74(19) . . . . ?
C2 C3 C4 C1 3.27(13) . . . . ?
C4 N2 C5 C6 31.6(2) . . . . ?
C4 N2 C5 C10 -150.52(16) . . . . ?
C4 C1 C2 O1 -177.9(2) . . . . ?
C4 C1 C2 C3 3.27(13) . . . . ?
C5 N2 C4 C1 -166.62(16) . . . . ?
C5 N2 C4 C3 17.4(3) . . . . ?
C5 C6 C7 C8 0.4(3) . . . . ?
C6 C5 C10 O3 178.34(15) . . . . ?
C6 C5 C10 C9 -1.6(3) . . . . ?
C6 C7 C8 Cl7 174.7(5) . . . . ?
C6 C7 C8 C9 -0.4(3) . . . . ?
C7 C8 C9 C10 -0.6(3) . . . . ?
C8 C9 C10 O3 -178.38(17) . . . . ?
C8 C9 C10 C5 1.6(3) . . . . ?
C10 O3 C11 C12 179.40(14) . . . . ?
C10 C5 C6 C7 0.7(3) . . . . ?
C11 O3 C10 C5 -179.13(15) . . . . ?
C11 O3 C10 C9 0.8(2) . . . . ?
C11 C12 C13 C14 172.07(15) . . . . ?
C11 C12 C13 C53 -7.6(2) . . . . ?
C11 C12 C17 C16 -172.28(15) . . . . ?
C11 C12 C17 C51 6.5(2) . . . . ?
C12 C13 C14 C15 2.0(2) . . . . ?
C12 C13 C14 C18 -172.67(15) . . . . ?
C12 C13 C53 C54 88.4(2) . . . . ?
C12 C17 C51 C52 -91.2(2) . . . . ?
C13 C12 C17 C16 2.2(2) . . . . ?
C13 C12 C17 C51 -178.99(15) . . . . ?
C13 C14 C15 C16 -1.3(2) . . . . ?
C13 C14 C15 C49 179.57(16) . . . . ?
C13 C14 C18 O4 -81.95(19) . . . . ?
C14 C13 C53 C54 -91.2(2) . . . . ?
C14 C15 C16 C17 1.1(2) . . . . ?
C14 C15 C16 C48 -177.40(15) . . . . ?
C14 C15 C49 C50 90.9(2) . . . . ?
C15 C14 C18 O4 103.39(18) . . . . ?
C15 C16 C17 C12 -1.5(2) . . . . ?
C15 C16 C17 C51 179.65(15) . . . . ?
C15 C16 C48 O5 -95.12(18) . . . . ?
C16 C15 C49 C50 -88.1(2) . . . . ?
C16 C17 C51 C52 87.6(2) . . . . ?
C17 C12 C13 C14 -2.4(2) . . . . ?
C17 C12 C13 C53 177.90(15) . . . . ?
C17 C16 C48 O5 86.35(18) . . . . ?
C18 O4 C19 C20 14.4(2) . . . . ?
C18 O4 C19 C24 -166.12(15) . . . . ?
C18 C14 C15 C16 173.22(15) . . . . ?
C18 C14 C15 C49 -5.9(2) . . . . ?
C19 O4 C18 C14 163.30(14) . . . . ?
C19 C20 C21 C22 -0.2(3) . . . . ?
C20 C19 C24 N4 175.32(16) . . . . ?
C20 C19 C24 C23 -2.5(3) . . . . ?
C20 C21 C22 C23 -2.0(3) . . . . ?
C21 C22 C23 C24 1.9(3) . . . . ?
C22 C23 C24 N4 -177.42(17) . . . . ?
C22 C23 C24 C19 0.3(3) . . . . ?
C24 N4 C25 C26 -20.3(3) . . . . ?
C24 N4 C25 C28 162.22(17) . . . . ?
C24 C19 C20 C21 2.5(3) . . . . ?
C25 N4 C24 C19 167.50(16) . . . . ?
C25 N4 C24 C23 -14.7(3) . . . . ?
C25 C26 C27 O6 180.0(2) . . . . ?
C25 C26 C27 C28 0.28(12) . . . . ?
C26 C25 C28 N3 179.89(19) . . . . ?
C26 C25 C28 C27 0.30(13) . . . . ?
C26 C27 C28 N3 -179.9(2) . . . . ?
C26 C27 C28 C25 -0.29(13) . . . . ?
C28 N3 C29 C30 -132.18(17) . . . . ?
C28 C25 C26 O7 178.7(2) . . . . ?
C28 C25 C26 C27 -0.29(13) . . . . ?
C29 N3 C28 C25 -176.94(17) . . . . ?
C29 N3 C28 C27 2.5(3) . . . . ?
C29 C30 C31 C32 -179.54(14) . . . . ?
C29 C30 C31 C59 0.6(2) . . . . ?
C29 C30 C35 C34 -178.35(15) . . . . ?
C29 C30 C35 C55 3.6(2) . . . . ?
C30 C31 C32 C33 -3.0(2) . . . . ?
C30 C31 C32 C37 -177.49(14) . . . . ?
C30 C31 C59 C60 -93.91(19) . . . . ?
C30 C35 C55 C56 88.1(2) . . . . ?
C31 C30 C35 C34 -2.9(2) . . . . ?
C31 C30 C35 C55 179.11(15) . . . . ?
C31 C32 C33 C34 -1.0(2) . . . . ?
C31 C32 C33 C57 176.58(15) . . . . ?
C31 C32 C37 N5 85.78(17) . . . . ?
C32 C31 C59 C60 86.27(19) . . . . ?
C32 C33 C34 C35 3.1(2) . . . . ?
C32 C33 C34 C36 -170.28(14) . . . . ?
C32 C33 C57 C58 -97.25(18) . . . . ?
C33 C32 C37 N5 -88.72(18) . . . . ?
C33 C34 C35 C30 -1.2(2) . . . . ?
C33 C34 C35 C55 176.78(15) . . . . ?
C33 C34 C36 N1 86.17(18) . . . . ?
C34 C33 C57 C58 80.32(19) . . . . ?
C34 C35 C55 C56 -89.9(2) . . . . ?
C35 C30 C31 C32 5.0(2) . . . . ?
C35 C30 C31 C59 -174.86(15) . . . . ?
C35 C34 C36 N1 -87.27(18) . . . . ?
C36 N1 C1 C2 0.0(3) . . . . ?
C36 N1 C1 C4 -178.12(16) . . . . ?
C36 C34 C35 C30 172.14(15) . . . . ?
C36 C34 C35 C55 -9.9(2) . . . . ?
C37 N5 C38 C39 7.0(3) . . . . ?
C37 N5 C38 C41 -170.96(17) . . . . ?
C37 C32 C33 C34 173.42(14) . . . . ?
C37 C32 C33 C57 -9.0(2) . . . . ?
C38 N5 C37 C32 -138.62(16) . . . . ?
C38 C39 C40 O9 -179.6(2) . . . . ?
C38 C39 C40 C41 -0.16(13) . . . . ?
C39 C38 C41 N6 178.94(18) . . . . ?
C39 C38 C41 C40 -0.17(13) . . . . ?
C39 C40 C41 N6 -178.9(2) . . . . ?
C39 C40 C41 C38 0.17(13) . . . . ?
C41 N6 C42 C43 -41.8(2) . . . . ?
C41 N6 C42 C47 139.75(17) . . . . ?
C41 C38 C39 O8 -177.5(2) . . . . ?
C41 C38 C39 C40 0.17(13) . . . . ?
C42 N6 C41 C38 165.80(17) . . . . ?
C42 N6 C41 C40 -15.5(3) . . . . ?
C42 C43 C44 C45 0.7(3) . . . . ?
C43 C42 C47 O5 178.29(14) . . . . ?
C43 C42 C47 C46 -1.2(2) . . . . ?
C43 C44 C45 C46 -0.8(3) . . . . ?
C44 C45 C46 C47 -0.1(3) . . . . ?
C45 C46 C47 O5 -178.31(16) . . . . ?
C45 C46 C47 C42 1.1(3) . . . . ?
C47 O5 C48 C16 -177.51(13) . . . . ?
C47 C42 C43 C44 0.2(2) . . . . ?
C48 O5 C47 C42 -173.12(14) . . . . ?
C48 O5 C47 C46 6.3(2) . . . . ?
C48 C16 C17 C12 177.00(14) . . . . ?
C48 C16 C17 C51 -1.8(2) . . . . ?
C49 C15 C16 C17 -179.81(15) . . . . ?
C49 C15 C16 C48 1.7(2) . . . . ?
C53 C13 C14 C15 -178.34(16) . . . . ?
C53 C13 C14 C18 7.0(2) . . . . ?
C57 C33 C34 C35 -174.49(15) . . . . ?
C57 C33 C34 C36 12.1(2) . . . . ?
C59 C31 C32 C33 176.82(15) . . . . ?
C59 C31 C32 C37 2.3(2) . . . . ?
N7 C61 C62 C63 -176.00(16) . . . . ?
N7 C65 C66 C67 174.88(17) . . . . ?
N7 C69 C70 C71 172.66(16) . . . . ?
N7 C73 C74 C75 164.76(17) . . . . ?
C61 N7 C65 C66 -171.31(17) . . . . ?
C61 N7 C69 C70 54.7(2) . . . . ?
C61 N7 C73 C74 -51.5(2) . . . . ?
C61 C62 C63 C64 -175.9(2) . . . . ?
C65 N7 C61 C62 -175.76(16) . . . . ?
C65 N7 C69 C70 -62.4(2) . . . . ?
C65 N7 C73 C74 66.8(2) . . . . ?
C65 C66 C67 C68 -177.7(2) . . . . ?
C69 N7 C61 C62 63.5(2) . . . . ?
C69 N7 C65 C66 -50.8(2) . . . . ?
C69 N7 C73 C74 -172.05(17) . . . . ?
C69 C70 C71 C72 167.43(18) . . . . ?
C73 N7 C61 C62 -53.5(2) . . . . ?
C73 N7 C65 C66 66.7(2) . . . . ?
C73 N7 C69 C70 175.81(16) . . . . ?
C73 C74 C75 C76 65.5(2) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.1570 1.5569 -22.3096 -0.3867 0.3651 -0.8469
0.1570 -1.5569 22.3096 0.3867 -0.3651 0.8469
-8.3955 -0.2394 6.4823 0.6763 0.7138 0.1819
8.3955 0.2394 -6.4823 -0.6763 -0.7138 -0.1819
-1.6706 7.8705 -16.2707 0.1616 0.1689 -0.9723
1.6706 -7.8705 16.2707 -0.1616 -0.1689 0.9723
-0.1026 -12.2348 -2.8132 -0.6738 0.5156 0.5292
0.1026 12.2348 2.8132 0.6738 -0.5156 -0.5292
