#------------------------------------------------------------------------------
#$Date: 2023-05-05 04:11:39 +0300 (Fri, 05 May 2023) $
#$Revision: 283185 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/86/1568686.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_1568686
loop_
_publ_author_name
'Wang, Hu'
'Jones, Leighton O.'
'Zhao, Tian'
'Hwang, Inhong'
'Lynch, Vincent M.'
'Khashab, Niveen M.'
'Schatz, George C.'
'Page, Zachariah A.'
'Sessler, Jonathan L.'
_publ_section_title
;
 Fluorescent copolymer aggregate sensor for lithium chloride.
;
_journal_issue                   15
_journal_name_full               'Chemical science'
_journal_page_first              4120
_journal_page_last               4125
_journal_paper_doi               10.1039/d2sc05342j
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety
'C58 H68 N4 O10, C14 H16 N, 2.229(C2 H3 N), H2 O, Cl'
_chemical_formula_sum            'C76.46 H92.69 Cl N7.23 O11'
_chemical_formula_weight         1324.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-07-01 deposited with the CCDC.	2023-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                104.805(6)
_cell_angle_beta                 97.924(5)
_cell_angle_gamma                96.664(5)
_cell_formula_units_Z            2
_cell_length_a                   12.7225(8)
_cell_length_b                   15.8452(10)
_cell_length_c                   18.7186(13)
_cell_measurement_reflns_used    4089
_cell_measurement_temperature    100.03(16)
_cell_measurement_theta_max      73.1180
_cell_measurement_theta_min      3.5280
_cell_volume                     3568.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.03(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2940
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -115.00 -16.00   1.00   13.50    --  -41.59 -57.00  60.00   99
  2  ω    -55.00  33.00   1.00   13.50    --  -41.59  38.00-150.00   88
  3  ω      6.00  76.00   1.00   13.50    --   41.59 -99.00 -90.00   70
  4  ω    -21.00  74.00   1.00   13.50    --   41.59 -77.00 -60.00   95
  5  ω     24.00 107.00   1.00   40.50    --  107.09 -94.00-180.00   83
  6  ω     57.00 133.00   1.00   40.50    --  107.09 -45.00   0.00   76
  7  ω     78.00 175.00   1.00   40.50    --  107.09  59.00 -18.00   97
  8  ω     59.00 130.00   1.00   40.50    --  107.09 -61.00 -90.00   71
  9  ω     36.00 128.00   1.00   40.50    --  107.09 -45.00-180.00   92
 10  ω     27.00 107.00   1.00   40.50    --  107.09 -94.00  60.00   80
 11  ω     64.00 107.00   1.00   40.50    --  107.09 -94.00 -90.00   43
 12  ω     21.00 169.00   1.00   40.50    --  107.09   0.00 150.00  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1095505000
_diffrn_orient_matrix_UB_12      -0.0325520000
_diffrn_orient_matrix_UB_13      0.0011470000
_diffrn_orient_matrix_UB_21      -0.0528795000
_diffrn_orient_matrix_UB_22      -0.0861411000
_diffrn_orient_matrix_UB_23      -0.0600471000
_diffrn_orient_matrix_UB_31      0.0230563000
_diffrn_orient_matrix_UB_32      0.0434984000
_diffrn_orient_matrix_UB_33      -0.0621861000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0702
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18197
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.407
_diffrn_reflns_theta_min         2.921
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.996
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.233
_exptl_crystal_description       prism
_exptl_crystal_F_000             1414
_exptl_crystal_size_max          0.244
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.032
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     950
_refine_ls_number_reflns         18197
_refine_ls_number_restraints     634
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1123P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1769
_refine_ls_wR_factor_ref         0.1919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12649
_reflns_number_total             18197
_reflns_threshold_expression     'I > 2σ(I)'
_twin_special_details
;
Component 2 rotated by -179.9912° 
around [0.00 0.00 1.00] (reciprocal) or [0.23 0.30 0.93] (direct)
;
_cod_data_source_file            d2sc05342j4.cif
_cod_data_source_block           1-3calix-dibnzylhcl
_cod_depositor_comments          'Adding full bibliography for 1568686.cif.'
_cod_database_code               1568686
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C76H92N7O11Cl
_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.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4875(11)
 0.5125(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H,H) groups
3. Restrained distances
 C76A-N7
 1.15 with sigma of 0.03
 C80-N78
 2.6 with sigma of 0.02
 N78-C79
 1.15 with sigma of 0.02
 C76-N7
 1.15 with sigma of 0.03
 C76-C75
 1.45 with sigma of 0.03
 C79-C80
 1.45 with sigma of 0.02
 C75A-C76A
 1.45 with sigma of 0.03
 N6-C73 \\sim N6A-C73
 with sigma of 0.04
 N6-C74 \\sim N6A-C74A
 with sigma of 0.02
 C73-C74 \\sim C73-C74A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(N6A) = Uanis(N6)
Uanis(C74A) = Uanis(C74)
5. Others
 Sof(H41)=Sof(O10A)=Sof(O9A)=Sof(C57A)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=
 Sof(C79)=Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(H80C)=Sof(N78)=1-FVAR(1)
 Sof(O9)=Sof(O10)=Sof(H42)=Sof(C57)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=
 FVAR(1)
 Sof(C75A)=Sof(H75D)=Sof(H75E)=Sof(H75F)=Sof(C76A)=1-FVAR(2)
 Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H75C)=Sof(C76)=FVAR(2)
 Sof(H73D)=Sof(H73E)=Sof(H73F)=Sof(C74A)=Sof(N6A)=1-FVAR(3)
 Sof(N6)=Sof(H73A)=Sof(H73B)=Sof(H73C)=Sof(C74)=FVAR(3)
6.a Free rotating group:
 O11(H11A,H11B)
6.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,
 H37B), C38(H38A,H38B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B),
 C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), N5(H5A,H5B), C59(H59A,H59B),
 C66(H66A,H66B)
6.c Me refined with riding coordinates:
 C58(H58A,H58B,H58C), C77(H77A,H77B,H77C)
6.d Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), C2(H2A), C3(H3A), C7(H7), C8(H8), C12(H12),
 C13(H13), C17(H17), C18(H18), C28(H28), C29(H29), C31(H31), C32(H32), C40(H40),
  C41(H41), C42(H42), C43(H43), C52(H52), C53(H53), C55(H55), C56(H56),
 C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C68(H68), C69(H69), C70(H70),
  C71(H71), C72(H72)
6.e Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C73(H73A,H73B,H73C), C73(H73D,
 H73E,H73F), C75(H75A,H75B,H75C), C80(H80A,H80B,H80C), C75A(H75D,H75E,H75F)
;
_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 1.454
_oxdiff_exptl_absorpt_empirical_full_min 0.850
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
O1 O 0.8391(3) 1.0267(2) 0.54784(16) 0.0351(7) Uani 1 1 d . U . . .
O2 O 0.9097(3) 1.0573(2) 0.70381(17) 0.0349(7) Uani 1 1 d . U . . .
O3 O 0.8521(2) 1.0850(2) 0.84518(17) 0.0319(7) Uani 1 1 d . U . . .
O4 O 0.7100(2) 0.98334(19) 0.90420(18) 0.0317(6) Uani 1 1 d . U . . .
O5 O 0.7491(3) 0.8337(2) 0.92392(18) 0.0338(7) Uani 1 1 d . U . . .
O6 O 0.9183(3) 0.7565(2) 0.86624(18) 0.0381(8) Uani 1 1 d . U . . .
O7 O 0.9901(2) 0.7035(2) 0.72480(16) 0.0307(6) Uani 1 1 d . U . . .
O8 O 0.8417(2) 0.5660(2) 0.61629(16) 0.0294(6) Uani 1 1 d . U . . .
O9 O 0.2522(3) 0.8552(3) 0.9264(2) 0.0376(10) Uani 0.771(4) 1 d . U P A 1
O10 O 0.3126(3) 0.9837(3) 0.9048(2) 0.0331(9) Uani 0.771(4) 1 d . U P A 1
N1 N 0.7526(3) 0.7147(2) 0.24518(19) 0.0250(7) Uani 1 1 d . U . . .
H1 H 0.744612 0.708766 0.289689 0.030 Uiso 1 1 calc R U . . .
N2 N 0.5068(3) 0.7272(2) 0.29205(19) 0.0255(7) Uani 1 1 d . U . . .
H2 H 0.556503 0.718764 0.326014 0.031 Uiso 1 1 calc R U . . .
N3 N 0.4985(3) 0.5295(2) 0.32396(19) 0.0245(7) Uani 1 1 d . U . . .
H3 H 0.551260 0.572727 0.347900 0.029 Uiso 1 1 calc R U . . .
N4 N 0.7440(3) 0.5151(2) 0.27716(18) 0.0226(6) Uani 1 1 d . U . . .
H4 H 0.742626 0.560019 0.315829 0.027 Uiso 1 1 calc R U . . .
C1 C 0.8139(3) 0.6675(3) 0.1986(2) 0.0244(8) Uani 1 1 d . U . . .
C2 C 0.8047(4) 0.6946(3) 0.1344(2) 0.0340(10) Uani 1 1 d . U . . .
H2A H 0.838113 0.673826 0.092328 0.041 Uiso 1 1 calc R U . . .
C3 C 0.7356(4) 0.7600(3) 0.1428(2) 0.0353(10) Uani 1 1 d . U . . .
H3A H 0.713900 0.789875 0.106577 0.042 Uiso 1 1 calc R U . . .
C4 C 0.7062(3) 0.7722(3) 0.2115(2) 0.0265(8) Uani 1 1 d . U . . .
C5 C 0.6338(3) 0.8326(3) 0.2496(2) 0.0254(8) Uani 1 1 d . U . . .
C6 C 0.5243(3) 0.7807(3) 0.2459(2) 0.0268(8) Uani 1 1 d . U . . .
C7 C 0.4279(4) 0.7755(3) 0.2007(3) 0.0346(10) Uani 1 1 d . U . . .
H7 H 0.415406 0.805134 0.162907 0.041 Uiso 1 1 calc R U . . .
C8 C 0.3505(4) 0.7181(3) 0.2206(3) 0.0348(10) Uani 1 1 d . U . . .
H8 H 0.276664 0.702393 0.198358 0.042 Uiso 1 1 calc R U . . .
C9 C 0.4005(3) 0.6888(3) 0.2776(2) 0.0262(8) Uani 1 1 d . U . . .
C10 C 0.3577(3) 0.6305(3) 0.3228(2) 0.0270(8) Uani 1 1 d . U . . .
C11 C 0.3936(3) 0.5403(3) 0.3024(2) 0.0240(8) Uani 1 1 d . U . . .
C12 C 0.3376(3) 0.4580(3) 0.2653(2) 0.0262(8) Uani 1 1 d . U . . .
H12 H 0.263543 0.444817 0.243484 0.031 Uiso 1 1 calc R U . . .
C13 C 0.4097(3) 0.3958(3) 0.2653(2) 0.0247(8) Uani 1 1 d . U . . .
H13 H 0.392428 0.333791 0.243266 0.030 Uiso 1 1 calc R U . . .
C14 C 0.5087(3) 0.4415(3) 0.3027(2) 0.0229(8) Uani 1 1 d . U . . .
C15 C 0.6153(3) 0.4089(2) 0.3169(2) 0.0228(8) Uani 1 1 d . U . . .
C16 C 0.6871(3) 0.4317(2) 0.2636(2) 0.0230(8) Uani 1 1 d . U . . .
C17 C 0.7098(3) 0.3810(3) 0.1987(2) 0.0285(9) Uani 1 1 d . U . . .
H17 H 0.682104 0.320326 0.175711 0.034 Uiso 1 1 calc R U . . .
C18 C 0.7833(3) 0.4359(3) 0.1714(2) 0.0258(8) Uani 1 1 d . U . . .
H18 H 0.812413 0.418218 0.126764 0.031 Uiso 1 1 calc R U . . .
C19 C 0.8037(3) 0.5180(3) 0.2212(2) 0.0241(8) Uani 1 1 d . U . . .
C20 C 0.8774(3) 0.6007(3) 0.2227(2) 0.0267(8) Uani 1 1 d . U . . .
C21 C 0.6196(4) 0.9039(3) 0.2083(2) 0.0316(9) Uani 1 1 d . U . . .
H21A H 0.566847 0.939432 0.228648 0.047 Uiso 1 1 calc R U . . .
H21B H 0.594247 0.875591 0.154678 0.047 Uiso 1 1 calc R U . . .
H21C H 0.688616 0.942198 0.215294 0.047 Uiso 1 1 calc R U . . .
C22 C 0.2334(3) 0.6161(3) 0.3056(3) 0.0367(10) Uani 1 1 d . U . . .
H22A H 0.208393 0.673465 0.317650 0.055 Uiso 1 1 calc R U . . .
H22B H 0.204592 0.579978 0.335943 0.055 Uiso 1 1 calc R U . . .
H22C H 0.208560 0.585802 0.252232 0.055 Uiso 1 1 calc R U . . .
C23 C 0.3941(4) 0.6758(3) 0.4069(3) 0.0326(9) Uani 1 1 d . U . . .
H23A H 0.472591 0.683284 0.419333 0.049 Uiso 1 1 calc R U . . .
H23B H 0.362126 0.639204 0.435856 0.049 Uiso 1 1 calc R U . . .
H23C H 0.370705 0.733777 0.419345 0.049 Uiso 1 1 calc R U . . .
C24 C 0.5939(3) 0.3078(3) 0.3015(2) 0.0278(8) Uani 1 1 d . U . . .
H24A H 0.546989 0.291907 0.334934 0.042 Uiso 1 1 calc R U . . .
H24B H 0.662166 0.286010 0.310450 0.042 Uiso 1 1 calc R U . . .
H24C H 0.558908 0.280956 0.249173 0.042 Uiso 1 1 calc R U . . .
C25 C 0.9553(4) 0.5759(3) 0.1676(3) 0.0341(10) Uani 1 1 d . U . . .
H25A H 0.995740 0.531733 0.181285 0.051 Uiso 1 1 calc R U . . .
H25B H 1.005336 0.628824 0.169779 0.051 Uiso 1 1 calc R U . . .
H25C H 0.914436 0.551509 0.116530 0.051 Uiso 1 1 calc R U . . .
C26 C 0.9436(3) 0.6425(3) 0.3015(2) 0.0286(8) Uani 1 1 d . U . . .
H26A H 0.988003 0.600611 0.315334 0.043 Uiso 1 1 calc R U . . .
H26B H 0.895103 0.657039 0.337626 0.043 Uiso 1 1 calc R U . . .
H26C H 0.990077 0.696492 0.301849 0.043 Uiso 1 1 calc R U . . .
C27 C 0.6866(3) 0.8813(3) 0.3316(2) 0.0255(8) Uani 1 1 d . U . . .
C28 C 0.7986(4) 0.9024(3) 0.3525(3) 0.0329(9) Uani 1 1 d . U . . .
H28 H 0.842539 0.883982 0.316142 0.039 Uiso 1 1 calc R U . . .
C29 C 0.8468(4) 0.9495(3) 0.4250(2) 0.0316(9) Uani 1 1 d . U . . .
H29 H 0.922977 0.961413 0.438154 0.038 Uiso 1 1 calc R U . . .
C30 C 0.7841(4) 0.9790(3) 0.4781(2) 0.0289(9) Uani 1 1 d . U . . .
C31 C 0.6729(4) 0.9598(3) 0.4592(2) 0.0309(9) Uani 1 1 d . U . . .
H31 H 0.629428 0.979558 0.495553 0.037 Uiso 1 1 calc R U . . .
C32 C 0.6254(3) 0.9111(3) 0.3860(2) 0.0268(8) Uani 1 1 d . U . . .
H32 H 0.549240 0.898069 0.373283 0.032 Uiso 1 1 calc R U . . .
C33 C 0.7778(4) 1.0632(3) 0.6032(3) 0.0412(11) Uani 1 1 d . U . . .
H33A H 0.731875 1.015291 0.614720 0.049 Uiso 1 1 calc R U . . .
H33B H 0.730783 1.101357 0.584403 0.049 Uiso 1 1 calc R U . . .
C34 C 0.8540(5) 1.1161(3) 0.6718(3) 0.0482(13) Uani 1 1 d . U . . .
H34A H 0.906099 1.158835 0.658868 0.058 Uiso 1 1 calc R U . . .
H34B H 0.814312 1.149652 0.708502 0.058 Uiso 1 1 calc R U . . .
C35 C 0.9857(4) 1.1006(3) 0.7699(2) 0.0360(10) Uani 1 1 d . U . . .
H35A H 1.037469 1.144876 0.758538 0.043 Uiso 1 1 calc R U . . .
H35B H 1.026446 1.056454 0.784984 0.043 Uiso 1 1 calc R U . . .
C36 C 0.9356(4) 1.1464(3) 0.8354(2) 0.0338(10) Uani 1 1 d . U . . .
H36A H 0.990631 1.167466 0.881580 0.041 Uiso 1 1 calc R U . . .
H36B H 0.906210 1.198069 0.825046 0.041 Uiso 1 1 calc R U . . .
C37 C 0.7971(4) 1.1241(3) 0.9036(2) 0.0326(9) Uani 1 1 d . U . . .
H37A H 0.786284 1.184254 0.901149 0.039 Uiso 1 1 calc R U . . .
H37B H 0.840164 1.128875 0.953111 0.039 Uiso 1 1 calc R U . . .
C38 C 0.6909(3) 1.0673(3) 0.8937(3) 0.0294(9) Uani 1 1 d . U . . .
H38A H 0.648417 1.095776 0.930892 0.035 Uiso 1 1 calc R U . . .
H38B H 0.649941 1.058972 0.842819 0.035 Uiso 1 1 calc R U . . .
C39 C 0.6230(3) 0.9284(3) 0.9118(2) 0.0273(8) Uani 1 1 d . U . . .
C40 C 0.5188(3) 0.9477(3) 0.9080(2) 0.0269(8) Uani 1 1 d . U . . .
H40 H 0.502687 1.000565 0.897016 0.032 Uiso 1 1 calc R U . . .
C41 C 0.4376(4) 0.8878(3) 0.9206(2) 0.0281(9) Uani 1 1 d . U . . .
H41 H 0.366221 0.900297 0.918382 0.034 Uiso 0.229(4) 1 calc R U P A 2
C42 C 0.4614(4) 0.8108(3) 0.9362(2) 0.0302(9) Uani 1 1 d . U . . .
H42 H 0.406472 0.771729 0.946288 0.036 Uiso 0.771(4) 1 calc R U P A 1
C43 C 0.5646(4) 0.7897(3) 0.9374(2) 0.0318(9) Uani 1 1 d . U . . .
H43 H 0.579548 0.735979 0.947130 0.038 Uiso 1 1 calc R U . . .
C44 C 0.6456(4) 0.8475(3) 0.9243(2) 0.0283(9) Uani 1 1 d . U . . .
C45 C 0.7710(4) 0.7486(3) 0.9318(3) 0.0362(10) Uani 1 1 d . U . . .
H45A H 0.730525 0.700644 0.888460 0.043 Uiso 1 1 calc R U . . .
H45B H 0.749440 0.738972 0.978238 0.043 Uiso 1 1 calc R U . . .
C46 C 0.8902(4) 0.7494(4) 0.9350(3) 0.0407(11) Uani 1 1 d . U . . .
H46A H 0.930113 0.799999 0.976409 0.049 Uiso 1 1 calc R U . . .
H46B H 0.909785 0.694279 0.944934 0.049 Uiso 1 1 calc R U . . .
C47 C 1.0265(4) 0.7407(4) 0.8630(3) 0.0398(11) Uani 1 1 d . U . . .
H47A H 1.031793 0.678775 0.862806 0.048 Uiso 1 1 calc R U . . .
H47B H 1.075772 0.780304 0.907587 0.048 Uiso 1 1 calc R U . . .
C48 C 1.0576(4) 0.7578(3) 0.7925(2) 0.0356(10) Uani 1 1 d . U . . .
H48A H 1.055097 0.820632 0.794771 0.043 Uiso 1 1 calc R U . . .
H48B H 1.132630 0.747692 0.790650 0.043 Uiso 1 1 calc R U . . .
C49 C 0.9961(3) 0.6120(3) 0.7121(2) 0.0306(9) Uani 1 1 d . U . . .
H49A H 0.951791 0.586292 0.743200 0.037 Uiso 1 1 calc R U . . .
H49B H 1.071351 0.603507 0.725772 0.037 Uiso 1 1 calc R U . . .
C50 C 0.9552(3) 0.5675(3) 0.6305(2) 0.0292(9) Uani 1 1 d . U . . .
H50A H 0.990348 0.600318 0.599421 0.035 Uiso 1 1 calc R U . . .
H50B H 0.971620 0.506474 0.617456 0.035 Uiso 1 1 calc R U . . .
C51 C 0.7894(3) 0.5236(3) 0.5449(2) 0.0247(8) Uani 1 1 d . U . . .
C52 C 0.6790(3) 0.5220(3) 0.5300(2) 0.0257(8) Uani 1 1 d . U . . .
H52 H 0.642335 0.546425 0.569409 0.031 Uiso 1 1 calc R U . . .
C53 C 0.6223(3) 0.4851(3) 0.4580(2) 0.0247(8) Uani 1 1 d . U . . .
H53 H 0.546887 0.484748 0.448766 0.030 Uiso 1 1 calc R U . . .
C54 C 0.6732(3) 0.4483(3) 0.3983(2) 0.0248(8) Uani 1 1 d . U . . .
C55 C 0.7825(3) 0.4452(3) 0.4158(2) 0.0313(9) Uani 1 1 d . U . . .
H55 H 0.818273 0.417002 0.377226 0.038 Uiso 1 1 calc R U . . .
C56 C 0.8403(3) 0.4815(3) 0.4872(2) 0.0316(9) Uani 1 1 d . U . . .
H56 H 0.914713 0.477986 0.497270 0.038 Uiso 1 1 calc R U . . .
C57 C 0.3246(5) 0.9059(4) 0.9176(3) 0.0304(12) Uani 0.771(4) 1 d . U P A 1
C58 C 0.2058(11) 1.0054(14) 0.9056(9) 0.041(3) Uani 0.771(4) 1 d . U P A 1
H58A H 0.203854 1.063155 0.895813 0.061 Uiso 0.771(4) 1 calc R U P A 1
H58B H 0.154749 0.960262 0.866662 0.061 Uiso 0.771(4) 1 calc R U P A 1
H58C H 0.186291 1.007653 0.954798 0.061 Uiso 0.771(4) 1 calc R U P A 1
N5 N 0.8538(3) 0.7983(2) 0.6555(2) 0.0298(8) Uani 1 1 d . U . . .
H5A H 0.900812 0.761068 0.663167 0.036 Uiso 1 1 calc R U . . .
H5B H 0.859078 0.840853 0.699525 0.036 Uiso 1 1 calc R U . . .
C59 C 0.7415(3) 0.7471(3) 0.6348(3) 0.0332(9) Uani 1 1 d . U . . .
H59A H 0.731839 0.710449 0.669811 0.040 Uiso 1 1 calc R U . . .
H59B H 0.732118 0.706723 0.583608 0.040 Uiso 1 1 calc R U . . .
C60 C 0.6564(3) 0.8062(3) 0.6375(3) 0.0293(9) Uani 1 1 d . U . . .
C61 C 0.5984(4) 0.8122(3) 0.5709(2) 0.0336(9) Uani 1 1 d . U . . .
H61 H 0.615199 0.782075 0.524056 0.040 Uiso 1 1 calc R U . . .
C62 C 0.5159(4) 0.8622(3) 0.5729(3) 0.0357(10) Uani 1 1 d . U . . .
H62 H 0.475890 0.865945 0.527402 0.043 Uiso 1 1 calc R U . . .
C63 C 0.4913(3) 0.9067(3) 0.6410(3) 0.0317(9) Uani 1 1 d . U . . .
H63 H 0.434862 0.941172 0.642006 0.038 Uiso 1 1 calc R U . . .
C64 C 0.5493(4) 0.9010(3) 0.7077(2) 0.0305(9) Uani 1 1 d . U . . .
H64 H 0.532912 0.931720 0.754484 0.037 Uiso 1 1 calc R U . . .
C65 C 0.6311(3) 0.8503(3) 0.7058(2) 0.0292(9) Uani 1 1 d . U . . .
H65 H 0.670038 0.845570 0.751320 0.035 Uiso 1 1 calc R U . . .
C66 C 0.8859(4) 0.8414(3) 0.5970(3) 0.0333(9) Uani 1 1 d . U . . .
H66A H 0.833244 0.817604 0.549765 0.040 Uiso 1 1 calc R U . . .
H66B H 0.886319 0.905975 0.614492 0.040 Uiso 1 1 calc R U . . .
C67 C 0.9962(4) 0.8237(3) 0.5829(3) 0.0328(9) Uani 1 1 d . U . . .
C68 C 1.0078(4) 0.7621(4) 0.5175(3) 0.0419(11) Uani 1 1 d . U . . .
H68 H 0.946360 0.733131 0.480821 0.050 Uiso 1 1 calc R U . . .
C69 C 1.1091(5) 0.7430(4) 0.5059(3) 0.0506(13) Uani 1 1 d . U . . .
H69 H 1.116974 0.701777 0.460972 0.061 Uiso 1 1 calc R U . . .
C70 C 1.1986(4) 0.7844(4) 0.5602(3) 0.0504(14) Uani 1 1 d . U . . .
H70 H 1.267665 0.770897 0.552362 0.060 Uiso 1 1 calc R U . . .
C71 C 1.1883(4) 0.8443(4) 0.6248(3) 0.0493(13) Uani 1 1 d . U . . .
H71 H 1.249862 0.871758 0.662033 0.059 Uiso 1 1 calc R U . . .
C72 C 1.0869(4) 0.8649(3) 0.6360(3) 0.0392(10) Uani 1 1 d . U . . .
H72 H 1.080017 0.907687 0.680332 0.047 Uiso 1 1 calc R U . . .
N6 N 0.441(2) 0.4100(13) 0.0386(14) 0.064(4) Uani 0.41(3) 1 d D U P B 1
C73 C 0.5418(4) 0.5485(3) 0.1399(3) 0.0411(11) Uani 1 1 d D U . . .
H73A H 0.540897 0.601089 0.121485 0.062 Uiso 0.41(3) 1 calc R U P B 1
H73B H 0.616376 0.540662 0.154061 0.062 Uiso 0.41(3) 1 calc R U P B 1
H73C H 0.506101 0.555951 0.183756 0.062 Uiso 0.41(3) 1 calc R U P B 1
H73D H 0.591105 0.572006 0.111216 0.062 Uiso 0.59(3) 1 calc R U P B 2
H73E H 0.582325 0.524924 0.176771 0.062 Uiso 0.59(3) 1 calc R U P B 2
H73F H 0.506217 0.595959 0.165937 0.062 Uiso 0.59(3) 1 calc R U P B 2
C74 C 0.486(2) 0.4717(18) 0.0815(18) 0.037(3) Uani 0.41(3) 1 d D U P B 1
N7 N 0.0850(6) 0.6360(4) 0.0216(3) 0.0738(17) Uani 1 1 d D U . . .
C75 C 0.2477(18) 0.5471(13) 0.0357(10) 0.104(8) Uani 0.56(2) 1 d D U P C 1
H75A H 0.295928 0.555850 0.000789 0.156 Uiso 0.56(2) 1 calc R U P C 1
H75B H 0.217852 0.484228 0.023636 0.156 Uiso 0.56(2) 1 calc R U P C 1
H75C H 0.287849 0.566793 0.087158 0.156 Uiso 0.56(2) 1 calc R U P C 1
C76 C 0.1606(15) 0.5981(11) 0.0290(8) 0.064(4) Uani 0.56(2) 1 d D U P C 1
O11 O 0.8919(3) 0.9064(2) 0.80316(19) 0.0389(7) Uani 1 1 d G U . . .
H11A H 0.890181 0.882287 0.839858 0.058 Uiso 1 1 d G U . . .
H11B H 0.872905 0.957863 0.819802 0.058 Uiso 1 1 d G U . . .
Cl1 Cl 0.70556(8) 0.68676(6) 0.40594(5) 0.02432(19) Uani 1 1 d . U . . .
O10A O 0.4240(12) 0.6930(11) 0.9876(8) 0.041(4) Uani 0.229(4) 1 d . U P A 2
O9A O 0.2907(11) 0.7671(9) 0.9612(8) 0.037(3) Uani 0.229(4) 1 d . U P A 2
C57A C 0.3826(16) 0.7548(13) 0.9620(10) 0.030(4) Uani 0.229(4) 1 d . U P A 2
C77 C 0.353(2) 0.6328(15) 1.0119(12) 0.045(5) Uani 0.229(4) 1 d . U P A 2
H77A H 0.394201 0.590880 1.029356 0.068 Uiso 0.229(4) 1 calc R U P A 2
H77B H 0.321659 0.665949 1.053018 0.068 Uiso 0.229(4) 1 calc R U P A 2
H77C H 0.296231 0.600384 0.969916 0.068 Uiso 0.229(4) 1 calc R U P A 2
C79 C 0.122(2) 1.0017(19) 0.9315(15) 0.059(7) Uiso 0.229(4) 1 d D . P A -2
C80 C 0.036(2) 1.013(2) 0.9747(16) 0.065(7) Uiso 0.229(4) 1 d D . P A -2
H80A H -0.021527 0.961634 0.954823 0.098 Uiso 0.229(4) 1 calc R U P A -2
H80B H 0.006519 1.066590 0.970813 0.098 Uiso 0.229(4) 1 calc R U P A -2
H80C H 0.063219 1.018238 1.027387 0.098 Uiso 0.229(4) 1 calc R U P A -2
N78 N 0.186(3) 0.994(4) 0.894(3) 0.060(14) Uani 0.229(4) 1 d D U P A -2
C75A C 0.1657(17) 0.5104(11) 0.0605(10) 0.074(6) Uani 0.44(2) 1 d D U P C 2
H75D H 0.231259 0.504071 0.038988 0.112 Uiso 0.44(2) 1 calc R U P C 2
H75E H 0.116693 0.453892 0.043387 0.112 Uiso 0.44(2) 1 calc R U P C 2
H75F H 0.184109 0.527594 0.115408 0.112 Uiso 0.44(2) 1 calc R U P C 2
C76A C 0.1133(18) 0.5783(12) 0.0363(10) 0.059(5) Uani 0.44(2) 1 d D U P C 2
C74A C 0.4606(14) 0.4776(12) 0.0886(12) 0.037(3) Uani 0.59(3) 1 d D U P B 2
N6A N 0.3985(16) 0.4238(10) 0.0473(9) 0.064(4) Uani 0.59(3) 1 d D 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'
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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 6 -11 0.0361
0 -7 11 0.0452
8 -2 2 0.0971
1 -1 -11 0.0161
-1 1 11 0.0161
-1 -10 4 0.0645
1 10 -4 0.0645
0 -6 11 0.0433
-1 6 -11 0.0315
-7 -4 6 0.1196
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
C30 O1 C33 117.7(4) . . ?
C35 O2 C34 113.9(4) . . ?
C36 O3 C37 112.0(3) . . ?
C39 O4 C38 116.7(3) . . ?
C44 O5 C45 115.7(4) . . ?
C46 O6 C47 110.3(3) . . ?
C49 O7 C48 113.4(3) . . ?
C51 O8 C50 116.6(3) . . ?
C57 O10 C58 114.6(9) . . ?
C1 N1 H1 125.1 . . ?
C4 N1 H1 125.1 . . ?
C4 N1 C1 109.8(3) . . ?
C6 N2 H2 124.8 . . ?
C9 N2 H2 124.8 . . ?
C9 N2 C6 110.4(3) . . ?
C11 N3 H3 124.8 . . ?
C14 N3 H3 124.8 . . ?
C14 N3 C11 110.4(3) . . ?
C16 N4 H4 125.0 . . ?
C16 N4 C19 110.1(3) . . ?
C19 N4 H4 125.0 . . ?
N1 C1 C20 121.2(3) . . ?
C2 C1 N1 107.4(4) . . ?
C2 C1 C20 131.4(4) . . ?
C1 C2 H2A 126.4 . . ?
C1 C2 C3 107.1(4) . . ?
C3 C2 H2A 126.4 . . ?
C2 C3 H3A 125.8 . . ?
C4 C3 C2 108.3(4) . . ?
C4 C3 H3A 125.8 . . ?
N1 C4 C5 121.5(4) . . ?
C3 C4 N1 107.3(4) . . ?
C3 C4 C5 131.1(4) . . ?
C4 C5 C21 108.4(3) . . ?
C4 C5 C27 110.9(3) . . ?
C6 C5 C4 110.5(3) . . ?
C6 C5 C21 108.7(3) . . ?
C6 C5 C27 111.3(3) . . ?
C21 C5 C27 106.8(3) . . ?
N2 C6 C5 122.3(4) . . ?
C7 C6 N2 107.1(4) . . ?
C7 C6 C5 130.6(4) . . ?
C6 C7 H7 126.2 . . ?
C6 C7 C8 107.6(4) . . ?
C8 C7 H7 126.2 . . ?
C7 C8 H8 125.9 . . ?
C9 C8 C7 108.3(4) . . ?
C9 C8 H8 125.9 . . ?
N2 C9 C10 121.6(4) . . ?
C8 C9 N2 106.5(4) . . ?
C8 C9 C10 131.8(4) . . ?
C9 C10 C11 111.5(3) . . ?
C9 C10 C22 108.7(3) . . ?
C9 C10 C23 110.0(3) . . ?
C11 C10 C22 108.0(3) . . ?
C11 C10 C23 110.3(3) . . ?
C23 C10 C22 108.3(4) . . ?
N3 C11 C10 121.7(3) . . ?
C12 C11 N3 106.9(3) . . ?
C12 C11 C10 131.4(4) . . ?
C11 C12 H12 126.0 . . ?
C11 C12 C13 108.0(3) . . ?
C13 C12 H12 126.0 . . ?
C12 C13 H13 126.1 . . ?
C14 C13 C12 107.8(4) . . ?
C14 C13 H13 126.1 . . ?
N3 C14 C15 122.6(3) . . ?
C13 C14 N3 107.0(3) . . ?
C13 C14 C15 130.3(4) . . ?
C14 C15 C16 109.7(3) . . ?
C14 C15 C24 108.7(3) . . ?
C14 C15 C54 112.1(3) . . ?
C16 C15 C24 108.4(3) . . ?
C16 C15 C54 109.8(3) . . ?
C54 C15 C24 108.0(3) . . ?
N4 C16 C15 121.5(3) . . ?
C17 C16 N4 107.5(4) . . ?
C17 C16 C15 130.9(4) . . ?
C16 C17 H17 126.2 . . ?
C16 C17 C18 107.7(4) . . ?
C18 C17 H17 126.2 . . ?
C17 C18 H18 126.2 . . ?
C19 C18 C17 107.5(4) . . ?
C19 C18 H18 126.2 . . ?
N4 C19 C20 121.9(3) . . ?
C18 C19 N4 107.2(4) . . ?
C18 C19 C20 130.9(4) . . ?
C1 C20 C25 108.1(3) . . ?
C1 C20 C26 109.8(3) . . ?
C19 C20 C1 111.1(3) . . ?
C19 C20 C25 109.0(3) . . ?
C19 C20 C26 110.4(3) . . ?
C26 C20 C25 108.4(4) . . ?
C5 C21 H21A 109.5 . . ?
C5 C21 H21B 109.5 . . ?
C5 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C10 C22 H22A 109.5 . . ?
C10 C22 H22B 109.5 . . ?
C10 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C10 C23 H23A 109.5 . . ?
C10 C23 H23B 109.5 . . ?
C10 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C15 C24 H24A 109.5 . . ?
C15 C24 H24B 109.5 . . ?
C15 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C20 C25 H25A 109.5 . . ?
C20 C25 H25B 109.5 . . ?
C20 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C20 C26 H26A 109.5 . . ?
C20 C26 H26B 109.5 . . ?
C20 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C5 121.0(4) . . ?
C32 C27 C5 121.5(4) . . ?
C32 C27 C28 117.3(4) . . ?
C27 C28 H28 119.2 . . ?
C29 C28 C27 121.6(4) . . ?
C29 C28 H28 119.2 . . ?
C28 C29 H29 120.0 . . ?
C30 C29 C28 119.9(4) . . ?
C30 C29 H29 120.0 . . ?
O1 C30 C29 115.7(4) . . ?
O1 C30 C31 124.3(4) . . ?
C29 C30 C31 120.0(4) . . ?
C30 C31 H31 120.3 . . ?
C30 C31 C32 119.4(4) . . ?
C32 C31 H31 120.3 . . ?
C27 C32 C31 121.7(4) . . ?
C27 C32 H32 119.1 . . ?
C31 C32 H32 119.1 . . ?
O1 C33 H33A 110.1 . . ?
O1 C33 H33B 110.1 . . ?
O1 C33 C34 108.0(4) . . ?
H33A C33 H33B 108.4 . . ?
C34 C33 H33A 110.1 . . ?
C34 C33 H33B 110.1 . . ?
O2 C34 C33 108.7(4) . . ?
O2 C34 H34A 109.9 . . ?
O2 C34 H34B 109.9 . . ?
C33 C34 H34A 109.9 . . ?
C33 C34 H34B 109.9 . . ?
H34A C34 H34B 108.3 . . ?
O2 C35 H35A 108.8 . . ?
O2 C35 H35B 108.8 . . ?
O2 C35 C36 113.7(4) . . ?
H35A C35 H35B 107.7 . . ?
C36 C35 H35A 108.8 . . ?
C36 C35 H35B 108.8 . . ?
O3 C36 C35 108.4(4) . . ?
O3 C36 H36A 110.0 . . ?
O3 C36 H36B 110.0 . . ?
C35 C36 H36A 110.0 . . ?
C35 C36 H36B 110.0 . . ?
H36A C36 H36B 108.4 . . ?
O3 C37 H37A 110.0 . . ?
O3 C37 H37B 110.0 . . ?
O3 C37 C38 108.5(3) . . ?
H37A C37 H37B 108.4 . . ?
C38 C37 H37A 110.0 . . ?
C38 C37 H37B 110.0 . . ?
O4 C38 C37 108.3(4) . . ?
O4 C38 H38A 110.0 . . ?
O4 C38 H38B 110.0 . . ?
C37 C38 H38A 110.0 . . ?
C37 C38 H38B 110.0 . . ?
H38A C38 H38B 108.4 . . ?
O4 C39 C40 124.7(4) . . ?
O4 C39 C44 115.0(4) . . ?
C40 C39 C44 120.3(4) . . ?
C39 C40 H40 120.5 . . ?
C39 C40 C41 119.1(4) . . ?
C41 C40 H40 120.5 . . ?
C40 C41 H41 119.9 . . ?
C40 C41 C57 121.0(4) . . ?
C42 C41 C40 120.2(4) . . ?
C42 C41 H41 119.9 . . ?
C42 C41 C57 118.8(4) . . ?
C41 C42 H42 119.6 . . ?
C41 C42 C43 120.9(4) . . ?
C41 C42 C57A 121.0(9) . . ?
C43 C42 H42 119.6 . . ?
C43 C42 C57A 117.7(9) . . ?
C42 C43 H43 120.1 . . ?
C44 C43 C42 119.8(4) . . ?
C44 C43 H43 120.1 . . ?
O5 C44 C39 115.6(4) . . ?
O5 C44 C43 124.8(4) . . ?
C43 C44 C39 119.6(4) . . ?
O5 C45 H45A 110.3 . . ?
O5 C45 H45B 110.3 . . ?
O5 C45 C46 107.1(4) . . ?
H45A C45 H45B 108.6 . . ?
C46 C45 H45A 110.3 . . ?
C46 C45 H45B 110.3 . . ?
O6 C46 C45 109.6(4) . . ?
O6 C46 H46A 109.8 . . ?
O6 C46 H46B 109.8 . . ?
C45 C46 H46A 109.8 . . ?
C45 C46 H46B 109.8 . . ?
H46A C46 H46B 108.2 . . ?
O6 C47 H47A 109.9 . . ?
O6 C47 H47B 109.9 . . ?
O6 C47 C48 108.8(4) . . ?
H47A C47 H47B 108.3 . . ?
C48 C47 H47A 109.9 . . ?
C48 C47 H47B 109.9 . . ?
O7 C48 C47 113.9(4) . . ?
O7 C48 H48A 108.8 . . ?
O7 C48 H48B 108.8 . . ?
C47 C48 H48A 108.8 . . ?
C47 C48 H48B 108.8 . . ?
H48A C48 H48B 107.7 . . ?
O7 C49 H49A 110.1 . . ?
O7 C49 H49B 110.1 . . ?
O7 C49 C50 107.8(3) . . ?
H49A C49 H49B 108.5 . . ?
C50 C49 H49A 110.1 . . ?
C50 C49 H49B 110.1 . . ?
O8 C50 C49 108.4(3) . . ?
O8 C50 H50A 110.0 . . ?
O8 C50 H50B 110.0 . . ?
C49 C50 H50A 110.0 . . ?
C49 C50 H50B 110.0 . . ?
H50A C50 H50B 108.4 . . ?
O8 C51 C52 117.3(4) . . ?
O8 C51 C56 123.8(4) . . ?
C52 C51 C56 118.8(4) . . ?
C51 C52 H52 119.9 . . ?
C53 C52 C51 120.3(4) . . ?
C53 C52 H52 119.9 . . ?
C52 C53 H53 119.2 . . ?
C52 C53 C54 121.7(4) . . ?
C54 C53 H53 119.2 . . ?
C53 C54 C15 124.1(4) . . ?
C55 C54 C15 119.1(4) . . ?
C55 C54 C53 116.8(4) . . ?
C54 C55 H55 118.9 . . ?
C56 C55 C54 122.3(4) . . ?
C56 C55 H55 118.9 . . ?
C51 C56 H56 120.1 . . ?
C55 C56 C51 119.9(4) . . ?
C55 C56 H56 120.1 . . ?
O9 C57 O10 123.9(6) . . ?
O9 C57 C41 122.9(5) . . ?
O10 C57 C41 113.2(5) . . ?
O10 C58 H58A 109.5 . . ?
O10 C58 H58B 109.5 . . ?
O10 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
H5A N5 H5B 107.7 . . ?
C59 N5 H5A 108.8 . . ?
C59 N5 H5B 108.8 . . ?
C59 N5 C66 113.8(4) . . ?
C66 N5 H5A 108.8 . . ?
C66 N5 H5B 108.8 . . ?
N5 C59 H59A 109.1 . . ?
N5 C59 H59B 109.1 . . ?
N5 C59 C60 112.7(3) . . ?
H59A C59 H59B 107.8 . . ?
C60 C59 H59A 109.1 . . ?
C60 C59 H59B 109.1 . . ?
C61 C60 C59 119.6(4) . . ?
C61 C60 C65 119.8(4) . . ?
C65 C60 C59 120.5(4) . . ?
C60 C61 H61 120.1 . . ?
C62 C61 C60 119.8(4) . . ?
C62 C61 H61 120.1 . . ?
C61 C62 H62 119.8 . . ?
C61 C62 C63 120.5(4) . . ?
C63 C62 H62 119.8 . . ?
C62 C63 H63 120.0 . . ?
C62 C63 C64 119.9(4) . . ?
C64 C63 H63 120.0 . . ?
C63 C64 H64 120.1 . . ?
C65 C64 C63 119.7(4) . . ?
C65 C64 H64 120.1 . . ?
C60 C65 H65 119.8 . . ?
C64 C65 C60 120.3(4) . . ?
C64 C65 H65 119.8 . . ?
N5 C66 H66A 109.7 . . ?
N5 C66 H66B 109.7 . . ?
H66A C66 H66B 108.2 . . ?
C67 C66 N5 109.7(3) . . ?
C67 C66 H66A 109.7 . . ?
C67 C66 H66B 109.7 . . ?
C68 C67 C66 120.2(4) . . ?
C72 C67 C66 120.8(4) . . ?
C72 C67 C68 119.0(4) . . ?
C67 C68 H68 119.9 . . ?
C69 C68 C67 120.3(5) . . ?
C69 C68 H68 119.9 . . ?
C68 C69 H69 120.1 . . ?
C70 C69 C68 119.8(5) . . ?
C70 C69 H69 120.1 . . ?
C69 C70 H70 119.7 . . ?
C71 C70 C69 120.6(5) . . ?
C71 C70 H70 119.7 . . ?
C70 C71 H71 120.2 . . ?
C70 C71 C72 119.7(5) . . ?
C72 C71 H71 120.2 . . ?
C67 C72 C71 120.7(5) . . ?
C67 C72 H72 119.7 . . ?
C71 C72 H72 119.7 . . ?
H73A C73 H73B 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
H73D C73 H73E 109.5 . . ?
H73D C73 H73F 109.5 . . ?
H73E C73 H73F 109.5 . . ?
C74 C73 H73A 109.5 . . ?
C74 C73 H73B 109.5 . . ?
C74 C73 H73C 109.5 . . ?
C74A C73 H73D 109.5 . . ?
C74A C73 H73E 109.5 . . ?
C74A C73 H73F 109.5 . . ?
N6 C74 C73 177(4) . . ?
H75A C75 H75B 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
C76 C75 H75A 109.5 . . ?
C76 C75 H75B 109.5 . . ?
C76 C75 H75C 109.5 . . ?
N7 C76 C75 176.5(17) . . ?
H11A O11 H11B 104.5 . . ?
C57A O10A C77 117.9(17) . . ?
O10A C57A C42 113.3(16) . . ?
O9A C57A C42 122.0(17) . . ?
O9A C57A O10A 124.6(18) . . ?
O10A C77 H77A 109.5 . . ?
O10A C77 H77B 109.5 . . ?
O10A C77 H77C 109.5 . . ?
H77A C77 H77B 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
N78 C79 C80 175(5) . . ?
C79 C80 H80A 109.5 . . ?
C79 C80 H80B 109.5 . . ?
C79 C80 H80C 109.5 . . ?
H80A C80 H80B 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
H75D C75A H75E 109.5 . . ?
H75D C75A H75F 109.5 . . ?
H75E C75A H75F 109.5 . . ?
C76A C75A H75D 109.5 . . ?
C76A C75A H75E 109.5 . . ?
C76A C75A H75F 109.5 . . ?
N7 C76A C75A 172(2) . . ?
N6A C74A C73 178(3) . . ?
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
O1 C30 1.374(5) . ?
O1 C33 1.428(6) . ?
O2 C34 1.431(6) . ?
O2 C35 1.422(6) . ?
O3 C36 1.420(5) . ?
O3 C37 1.426(5) . ?
O4 C38 1.436(5) . ?
O4 C39 1.374(5) . ?
O5 C44 1.360(5) . ?
O5 C45 1.447(5) . ?
O6 C46 1.411(6) . ?
O6 C47 1.434(5) . ?
O7 C48 1.433(5) . ?
O7 C49 1.422(5) . ?
O8 C50 1.428(5) . ?
O8 C51 1.368(5) . ?
O9 C57 1.209(7) . ?
O10 C57 1.335(7) . ?
O10 C58 1.441(14) . ?
N1 H1 0.8800 . ?
N1 C1 1.384(5) . ?
N1 C4 1.376(5) . ?
N2 H2 0.8800 . ?
N2 C6 1.378(5) . ?
N2 C9 1.377(5) . ?
N3 H3 0.8800 . ?
N3 C11 1.383(5) . ?
N3 C14 1.375(5) . ?
N4 H4 0.8800 . ?
N4 C16 1.374(5) . ?
N4 C19 1.384(5) . ?
C1 C2 1.369(6) . ?
C1 C20 1.524(5) . ?
C2 H2A 0.9500 . ?
C2 C3 1.427(6) . ?
C3 H3A 0.9500 . ?
C3 C4 1.361(6) . ?
C4 C5 1.520(6) . ?
C5 C6 1.517(6) . ?
C5 C21 1.538(5) . ?
C5 C27 1.546(6) . ?
C6 C7 1.371(6) . ?
C7 H7 0.9500 . ?
C7 C8 1.415(7) . ?
C8 H8 0.9500 . ?
C8 C9 1.375(6) . ?
C9 C10 1.509(6) . ?
C10 C11 1.522(5) . ?
C10 C22 1.548(5) . ?
C10 C23 1.534(6) . ?
C11 C12 1.369(6) . ?
C12 H12 0.9500 . ?
C12 C13 1.422(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.373(5) . ?
C14 C15 1.520(5) . ?
C15 C16 1.524(5) . ?
C15 C24 1.538(5) . ?
C15 C54 1.533(5) . ?
C16 C17 1.362(6) . ?
C17 H17 0.9500 . ?
C17 C18 1.436(6) . ?
C18 H18 0.9500 . ?
C18 C19 1.366(6) . ?
C19 C20 1.511(6) . ?
C20 C25 1.538(6) . ?
C20 C26 1.533(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.402(6) . ?
C27 C32 1.387(6) . ?
C28 H28 0.9500 . ?
C28 C29 1.385(6) . ?
C29 H29 0.9500 . ?
C29 C30 1.383(6) . ?
C30 C31 1.388(6) . ?
C31 H31 0.9500 . ?
C31 C32 1.400(6) . ?
C32 H32 0.9500 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.487(7) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.517(6) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.495(6) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.390(6) . ?
C39 C44 1.415(6) . ?
C40 H40 0.9500 . ?
C40 C41 1.406(6) . ?
C41 H41 0.9500 . ?
C41 C42 1.381(6) . ?
C41 C57 1.495(7) . ?
C42 H42 0.9500 . ?
C42 C43 1.390(7) . ?
C42 C57A 1.474(19) . ?
C43 H43 0.9500 . ?
C43 C44 1.389(6) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.507(7) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.509(7) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C50 1.499(6) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.390(6) . ?
C51 C56 1.399(6) . ?
C52 H52 0.9500 . ?
C52 C53 1.381(6) . ?
C53 H53 0.9500 . ?
C53 C54 1.402(6) . ?
C54 C55 1.393(6) . ?
C55 H55 0.9500 . ?
C55 C56 1.377(6) . ?
C56 H56 0.9500 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
N5 H5A 0.9100 . ?
N5 H5B 0.9100 . ?
N5 C59 1.505(5) . ?
N5 C66 1.509(5) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C59 C60 1.510(6) . ?
C60 C61 1.390(6) . ?
C60 C65 1.392(6) . ?
C61 H61 0.9500 . ?
C61 C62 1.385(7) . ?
C62 H62 0.9500 . ?
C62 C63 1.385(7) . ?
C63 H63 0.9500 . ?
C63 C64 1.391(6) . ?
C64 H64 0.9500 . ?
C64 C65 1.385(6) . ?
C65 H65 0.9500 . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C66 C67 1.508(6) . ?
C67 C68 1.394(7) . ?
C67 C72 1.387(7) . ?
C68 H68 0.9500 . ?
C68 C69 1.390(7) . ?
C69 H69 0.9500 . ?
C69 C70 1.388(8) . ?
C70 H70 0.9500 . ?
C70 C71 1.366(8) . ?
C71 H71 0.9500 . ?
C71 C72 1.398(7) . ?
C72 H72 0.9500 . ?
N6 C74 1.128(15) . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C73 H73D 0.9800 . ?
C73 H73E 0.9800 . ?
C73 H73F 0.9800 . ?
C73 C74 1.444(14) . ?
C73 C74A 1.469(11) . ?
N7 C76 1.203(16) . ?
N7 C76A 1.105(17) . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C75 C76 1.455(18) . ?
O11 H11A 0.8689 . ?
O11 H11B 0.8700 . ?
O10A C57A 1.33(2) . ?
O10A C77 1.43(2) . ?
O9A C57A 1.21(3) . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
C79 C80 1.456(18) . ?
C79 N78 1.140(19) . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C75A H75D 0.9800 . ?
C75A H75E 0.9800 . ?
C75A H75F 0.9800 . ?
C75A C76A 1.463(19) . ?
C74A N6A 1.135(11) . ?
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 Cl1 0.88 2.40 3.275(3) 174.6 . yes
N2 H2 Cl1 0.88 2.43 3.307(3) 172.3 . yes
N3 H3 Cl1 0.88 2.43 3.303(3) 175.1 . yes
N4 H4 Cl1 0.88 2.41 3.276(3) 168.1 . yes
N5 H5A O7 0.91 1.97 2.815(5) 154.3 . yes
N5 H5B O11 0.91 1.91 2.797(5) 163.2 . yes
O11 H11A O6 0.87 2.23 2.943(5) 139.4 . yes
O11 H11B O3 0.87 2.01 2.861(5) 167.5 . 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
O1 C30 C31 C32 179.5(4) . . . . ?
O1 C33 C34 O2 -68.2(5) . . . . ?
O2 C35 C36 O3 51.3(5) . . . . ?
O3 C37 C38 O4 64.7(4) . . . . ?
O4 C39 C40 C41 -176.7(4) . . . . ?
O4 C39 C44 O5 -2.6(5) . . . . ?
O4 C39 C44 C43 176.0(4) . . . . ?
O5 C45 C46 O6 -64.4(5) . . . . ?
O6 C47 C48 O7 -59.3(5) . . . . ?
O7 C49 C50 O8 -71.1(4) . . . . ?
O8 C51 C52 C53 176.0(4) . . . . ?
O8 C51 C56 C55 -176.0(4) . . . . ?
N1 C1 C2 C3 -0.1(5) . . . . ?
N1 C1 C20 C19 73.1(5) . . . . ?
N1 C1 C20 C25 -167.4(4) . . . . ?
N1 C1 C20 C26 -49.3(5) . . . . ?
N1 C4 C5 C6 -75.5(5) . . . . ?
N1 C4 C5 C21 165.4(4) . . . . ?
N1 C4 C5 C27 48.4(5) . . . . ?
N2 C6 C7 C8 0.4(5) . . . . ?
N2 C9 C10 C11 -74.2(5) . . . . ?
N2 C9 C10 C22 166.9(4) . . . . ?
N2 C9 C10 C23 48.6(5) . . . . ?
N3 C11 C12 C13 0.7(5) . . . . ?
N3 C14 C15 C16 -73.3(5) . . . . ?
N3 C14 C15 C24 168.3(4) . . . . ?
N3 C14 C15 C54 49.0(5) . . . . ?
N4 C16 C17 C18 -0.3(4) . . . . ?
N4 C19 C20 C1 -77.5(5) . . . . ?
N4 C19 C20 C25 163.6(4) . . . . ?
N4 C19 C20 C26 44.6(5) . . . . ?
C1 N1 C4 C3 1.5(5) . . . . ?
C1 N1 C4 C5 179.7(4) . . . . ?
C1 C2 C3 C4 1.1(6) . . . . ?
C2 C1 C20 C19 -108.2(5) . . . . ?
C2 C1 C20 C25 11.3(6) . . . . ?
C2 C1 C20 C26 129.4(5) . . . . ?
C2 C3 C4 N1 -1.6(5) . . . . ?
C2 C3 C4 C5 -179.5(4) . . . . ?
C3 C4 C5 C6 102.2(5) . . . . ?
C3 C4 C5 C21 -16.9(7) . . . . ?
C3 C4 C5 C27 -133.9(5) . . . . ?
C4 N1 C1 C2 -0.8(5) . . . . ?
C4 N1 C1 C20 178.2(3) . . . . ?
C4 C5 C6 N2 77.0(5) . . . . ?
C4 C5 C6 C7 -103.0(5) . . . . ?
C4 C5 C27 C28 30.3(5) . . . . ?
C4 C5 C27 C32 -154.1(4) . . . . ?
C5 C6 C7 C8 -179.5(4) . . . . ?
C5 C27 C28 C29 177.1(4) . . . . ?
C5 C27 C32 C31 -176.1(4) . . . . ?
C6 N2 C9 C8 0.6(5) . . . . ?
C6 N2 C9 C10 -176.9(4) . . . . ?
C6 C5 C27 C28 153.8(4) . . . . ?
C6 C5 C27 C32 -30.7(5) . . . . ?
C6 C7 C8 C9 0.0(5) . . . . ?
C7 C8 C9 N2 -0.4(5) . . . . ?
C7 C8 C9 C10 176.8(4) . . . . ?
C8 C9 C10 C11 109.0(5) . . . . ?
C8 C9 C10 C22 -9.9(6) . . . . ?
C8 C9 C10 C23 -128.3(5) . . . . ?
C9 N2 C6 C5 179.3(3) . . . . ?
C9 N2 C6 C7 -0.7(5) . . . . ?
C9 C10 C11 N3 72.8(5) . . . . ?
C9 C10 C11 C12 -110.1(5) . . . . ?
C10 C11 C12 C13 -176.7(4) . . . . ?
C11 N3 C14 C13 1.6(5) . . . . ?
C11 N3 C14 C15 178.4(4) . . . . ?
C11 C12 C13 C14 0.2(5) . . . . ?
C12 C13 C14 N3 -1.1(5) . . . . ?
C12 C13 C14 C15 -177.6(4) . . . . ?
C13 C14 C15 C16 102.7(5) . . . . ?
C13 C14 C15 C24 -15.7(6) . . . . ?
C13 C14 C15 C54 -135.0(4) . . . . ?
C14 N3 C11 C10 176.3(4) . . . . ?
C14 N3 C11 C12 -1.5(5) . . . . ?
C14 C15 C16 N4 79.9(4) . . . . ?
C14 C15 C16 C17 -101.0(5) . . . . ?
C14 C15 C54 C53 19.7(5) . . . . ?
C14 C15 C54 C55 -162.7(4) . . . . ?
C15 C16 C17 C18 -179.5(4) . . . . ?
C15 C54 C55 C56 178.0(4) . . . . ?
C16 N4 C19 C18 0.7(4) . . . . ?
C16 N4 C19 C20 -177.9(3) . . . . ?
C16 C15 C54 C53 142.0(4) . . . . ?
C16 C15 C54 C55 -40.4(5) . . . . ?
C16 C17 C18 C19 0.7(5) . . . . ?
C17 C18 C19 N4 -0.8(4) . . . . ?
C17 C18 C19 C20 177.5(4) . . . . ?
C18 C19 C20 C1 104.4(5) . . . . ?
C18 C19 C20 C25 -14.6(6) . . . . ?
C18 C19 C20 C26 -133.5(4) . . . . ?
C19 N4 C16 C15 179.1(3) . . . . ?
C19 N4 C16 C17 -0.2(4) . . . . ?
C20 C1 C2 C3 -179.0(4) . . . . ?
C21 C5 C6 N2 -164.0(4) . . . . ?
C21 C5 C6 C7 15.9(6) . . . . ?
C21 C5 C27 C28 -87.6(5) . . . . ?
C21 C5 C27 C32 87.9(5) . . . . ?
C22 C10 C11 N3 -167.9(4) . . . . ?
C22 C10 C11 C12 9.2(6) . . . . ?
C23 C10 C11 N3 -49.8(5) . . . . ?
C23 C10 C11 C12 127.3(5) . . . . ?
C24 C15 C16 N4 -161.5(3) . . . . ?
C24 C15 C16 C17 17.7(6) . . . . ?
C24 C15 C54 C53 -100.0(4) . . . . ?
C24 C15 C54 C55 77.6(5) . . . . ?
C27 C5 C6 N2 -46.6(5) . . . . ?
C27 C5 C6 C7 133.3(5) . . . . ?
C27 C28 C29 C30 -1.9(7) . . . . ?
C28 C27 C32 C31 -0.4(6) . . . . ?
C28 C29 C30 O1 -178.6(4) . . . . ?
C28 C29 C30 C31 1.4(6) . . . . ?
C29 C30 C31 C32 -0.5(6) . . . . ?
C30 O1 C33 C34 -176.6(4) . . . . ?
C30 C31 C32 C27 0.0(6) . . . . ?
C32 C27 C28 C29 1.4(6) . . . . ?
C33 O1 C30 C29 176.2(4) . . . . ?
C33 O1 C30 C31 -3.8(6) . . . . ?
C34 O2 C35 C36 65.1(5) . . . . ?
C35 O2 C34 C33 179.7(4) . . . . ?
C36 O3 C37 C38 161.2(4) . . . . ?
C37 O3 C36 C35 -177.2(4) . . . . ?
C38 O4 C39 C40 1.8(6) . . . . ?
C38 O4 C39 C44 -178.2(4) . . . . ?
C39 O4 C38 C37 167.7(3) . . . . ?
C39 C40 C41 C42 -0.3(6) . . . . ?
C39 C40 C41 C57 179.6(4) . . . . ?
C40 C39 C44 O5 177.4(4) . . . . ?
C40 C39 C44 C43 -4.0(6) . . . . ?
C40 C41 C42 C43 -2.1(6) . . . . ?
C40 C41 C42 C57A 169.6(9) . . . . ?
C40 C41 C57 O9 178.3(5) . . . . ?
C40 C41 C57 O10 -2.2(6) . . . . ?
C41 C42 C43 C44 1.4(6) . . . . ?
C41 C42 C57A O10A -168.2(11) . . . . ?
C41 C42 C57A O9A 10(2) . . . . ?
C42 C41 C57 O9 -1.8(7) . . . . ?
C42 C41 C57 O10 177.7(4) . . . . ?
C42 C43 C44 O5 -179.9(4) . . . . ?
C42 C43 C44 C39 1.7(6) . . . . ?
C43 C42 C57A O10A 3.7(18) . . . . ?
C43 C42 C57A O9A -178.2(14) . . . . ?
C44 O5 C45 C46 -176.4(4) . . . . ?
C44 C39 C40 C41 3.3(6) . . . . ?
C45 O5 C44 C39 -176.1(4) . . . . ?
C45 O5 C44 C43 5.3(6) . . . . ?
C46 O6 C47 C48 -174.3(4) . . . . ?
C47 O6 C46 C45 -169.2(4) . . . . ?
C48 O7 C49 C50 -160.5(3) . . . . ?
C49 O7 C48 C47 -64.4(5) . . . . ?
C50 O8 C51 C52 -179.5(4) . . . . ?
C50 O8 C51 C56 1.1(6) . . . . ?
C51 O8 C50 C49 -176.8(3) . . . . ?
C51 C52 C53 C54 0.1(6) . . . . ?
C52 C51 C56 C55 4.7(7) . . . . ?
C52 C53 C54 C15 -178.1(4) . . . . ?
C52 C53 C54 C55 4.2(6) . . . . ?
C53 C54 C55 C56 -4.2(6) . . . . ?
C54 C15 C16 N4 -43.8(5) . . . . ?
C54 C15 C16 C17 135.4(4) . . . . ?
C54 C55 C56 C51 -0.2(7) . . . . ?
C56 C51 C52 C53 -4.7(6) . . . . ?
C57 C41 C42 C43 178.0(4) . . . . ?
C58 O10 C57 O9 2.7(10) . . . . ?
C58 O10 C57 C41 -176.8(8) . . . . ?
N5 C59 C60 C61 106.4(5) . . . . ?
N5 C59 C60 C65 -77.6(5) . . . . ?
N5 C66 C67 C68 105.0(5) . . . . ?
N5 C66 C67 C72 -71.9(5) . . . . ?
C59 N5 C66 C67 -133.2(4) . . . . ?
C59 C60 C61 C62 176.2(4) . . . . ?
C59 C60 C65 C64 -176.8(4) . . . . ?
C60 C61 C62 C63 0.4(7) . . . . ?
C61 C60 C65 C64 -0.9(6) . . . . ?
C61 C62 C63 C64 -0.3(7) . . . . ?
C62 C63 C64 C65 -0.4(7) . . . . ?
C63 C64 C65 C60 0.9(6) . . . . ?
C65 C60 C61 C62 0.2(7) . . . . ?
C66 N5 C59 C60 -71.0(5) . . . . ?
C66 C67 C68 C69 -177.3(5) . . . . ?
C66 C67 C72 C71 176.0(5) . . . . ?
C67 C68 C69 C70 1.1(8) . . . . ?
C68 C67 C72 C71 -1.0(7) . . . . ?
C68 C69 C70 C71 -0.5(9) . . . . ?
C69 C70 C71 C72 -0.8(8) . . . . ?
C70 C71 C72 C67 1.6(8) . . . . ?
C72 C67 C68 C69 -0.3(7) . . . . ?
C57A C42 C43 C44 -170.6(9) . . . . ?
C77 O10A C57A C42 -178.0(14) . . . . ?
C77 O10A C57A O9A 4(3) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.4875(11) 5631 16398 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.5125(11) 5641 16398 nmt -0.9997 -0.0006 -0.0009 -0.0000 -1.0003 0.0005
0.4992 0.6513 0.9998
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
1.9307 6.3861 -10.8973 -0.0089 0.0021 1.0000
0.1491 -6.6884 10.8994 0.2466 -0.0862 -0.9653
7.8646 -2.3884 2.0438 0.9417 -0.3329 -0.0497
1.3543 -0.9299 -11.4161 0.1655 0.6940 0.7007
-1.3543 0.9299 11.4161 -0.1655 -0.6940 -0.7007
-1.4102 -9.8620 3.5727 0.1706 0.7096 -0.6837
1.4102 9.8620 -3.5727 -0.1706 -0.7096 0.6837
0.0577 -6.4612 11.0534 0.2293 -0.1102 -0.9671
-1.4304 6.2980 -10.7576 -0.3741 0.1791 0.9100
-6.8807 -3.7297 6.4394 -0.6250 0.2985 -0.7213
