#------------------------------------------------------------------------------
#$Date: 2021-08-05 03:35:14 +0300 (Thu, 05 Aug 2021) $
#$Revision: 267947 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/43/1564322.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_1564322
loop_
_publ_author_name
'Dengler, Sebastian'
'Mandal, Pradeep K.'
'Allmendinger, Lars'
'Douat, Céline'
'Huc, Ivan'
_publ_section_title
;
 Conformational interplay in hybrid peptide--helical aromatic foldamer
 macrocycles
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC03640H
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C55 H57 Ca N14 O22 S3'
_chemical_formula_sum            'C54.26 H54 Ca0.75 N14 O39.41 S3'
_chemical_formula_weight         1659.17
_chemical_name_common            'hybrid Foldamer-peptide macrocycle'
_chemical_properties_physical    Moisture-sensitive,Heat-sensitive
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-05-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-07 deposited with the CCDC.	2021-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   17.90824(9)
_cell_length_b                   17.90824(9)
_cell_length_c                   46.5216(2)
_cell_measurement_reflns_used    160150
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      1.48
_cell_volume                     12920.85(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  KM4CCD
_diffrn_measurement_method       ω-scans
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.800
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            160022
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        28.685
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         1.478
_diffrn_source                   'PXII - X10SA, SLS'
_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_T_max  1.1771
_exptl_absorpt_correction_T_min  0.9070
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'Light yellow'
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       prism
_exptl_crystal_F_000             5135
_exptl_crystal_recrystallization_method 'Vapor Diffusion Method'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 6845 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.061(8)
_refine_ls_extinction_coef       0.0032(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.714
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     842
_refine_ls_number_reflns         17481
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.715
_refine_ls_R_factor_all          0.1260
_refine_ls_R_factor_gt           0.1215
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3408
_refine_ls_wR_factor_ref         0.3576
_reflns_Friedel_coverage         0.966
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                15452
_reflns_number_total             17481
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1sc03640h2.cif
_cod_data_source_block           SD3_121
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Empirical' was
changed to 'empirical' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        12920.85(14)
_cod_database_code               1564322
_shelx_shelxl_version_number     2018/3
_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. 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
2. Restrained distances
 C74-C73
 1.54 with sigma of 0.02
 C22-C29
 1.54 with sigma of 0.02
 C33-C32
 1.54 with sigma of 0.02
 C85-O87
 1.27 with sigma of 0.02
 N83-C84
 1.47 with sigma of 0.02
 C85-O86
 1.27 with sigma of 0.02
 C84-C85
 1.54 with sigma of 0.02
 Ca89-O95 \\sim Ca89-O91 \\sim Ca89-O92 \\sim Ca89-O93 \\sim Ca89-O94
 with sigma of 0.02
 C84-O86 \\sim C84-O87
 with sigma of 0.02
3. Restrained planarity
 O87, C85, O86, C84
 with sigma of 0.1
4. Others
 Fixed Uiso: O86(0.25) C85(0.25)
5.a Ternary CH refined with riding coordinates:
 C65(H65), C71(H71), C63(H63), C79(H79)
5.b Secondary CH2 refined with riding coordinates:
 C59(H59A,H59B), C1(H1A,H1B), C5(H5A,H5B), C32(H32A,H32B), C80(H80A,H80B),
 C72(H72A,H72B), C73(H73A,H73B), C64(H64A,H64B), C74(H74A,H74B), C75(H75A,H75B),
  C84(H84A,H84B)
5.c Aromatic/amide H refined with riding coordinates:
 N41(H41), N4(H4), C50(H50), N31(H31), C34(H34), N70(H70), N62(H62), C45(H45),
 C23(H23), C36(H36), C7(H7), N78(H78), C43(H43), C16(H16), N83(H83), C35(H35),
 C44(H44), C9(H9), C17(H17), N58(H58), N14(H14), C18(H18), C8(H8)
5.d X=CH2 refined with riding coordinates:
 N76(H76A,H76B)
5.e Idealised Me refined as rotating group:
 C67(H67A,H67B,H67C), C66(H66A,H66B,H66C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+5/6'
'-y, x-y, z+2/3'
'-x, -y, z+1/2'
'-x+y, -x, z+1/3'
'y, -x+y, z+1/6'
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
S81 S 0.00860(19) -0.2765(2) -0.53603(4) 0.1133(7) Uani 1 1 d . . . . .
S52 S -0.43676(19) -0.2099(3) -0.67981(6) 0.1380(13) Uani 1 1 d . . . . .
S25 S -0.3745(3) -0.5378(3) -0.62440(8) 0.1525(16) Uani 1 1 d . . . . .
O57 O -0.2471(3) -0.3648(4) -0.68102(12) 0.0963(13) Uani 1 1 d . . . . .
N21 N -0.1747(4) -0.2649(5) -0.59652(12) 0.0887(15) Uani 1 1 d . . . . .
N48 N -0.1625(3) -0.1488(4) -0.65778(10) 0.0766(11) Uani 1 1 d . . . . .
C56 C -0.1957(3) -0.2894(4) -0.67426(12) 0.0809(14) Uani 1 1 d . . . . .
C59 C -0.0704(4) -0.3108(4) -0.68090(14) 0.0801(12) Uani 1 1 d . . . . .
H59A H -0.089114 -0.334916 -0.699965 0.096 Uiso 1 1 calc R . . . .
H59B H -0.086969 -0.357665 -0.667355 0.096 Uiso 1 1 calc R . . . .
N38 N 0.0663(4) -0.0439(5) -0.61292(11) 0.0886(15) Uani 1 1 d . . . . .
C20 C -0.2606(5) -0.2855(6) -0.59843(13) 0.096(2) Uani 1 1 d . . . . .
C49 C -0.2212(4) -0.2252(5) -0.66811(12) 0.0806(14) Uani 1 1 d . . . . .
C47 C -0.1839(5) -0.0866(6) -0.65358(13) 0.0888(17) Uani 1 1 d . . . . .
O61 O 0.0580(3) -0.1740(4) -0.67604(11) 0.0888(11) Uani 1 1 d . . . . .
N41 N -0.0442(4) -0.0032(4) -0.63405(11) 0.0865(13) Uani 1 1 d . . . . .
H41 H -0.045874 -0.052016 -0.634175 0.104 Uiso 1 1 calc R . . . .
C37 C 0.0950(5) 0.0409(5) -0.61474(15) 0.0921(17) Uani 1 1 d . . . . .
O30 O -0.0305(5) -0.3436(5) -0.60865(14) 0.1113(18) Uani 1 1 d . . . . .
C19 C -0.3243(5) -0.3704(8) -0.60756(18) 0.115(3) Uani 1 1 d . . . . .
N4 N 0.0218(5) -0.0764(6) -0.52501(13) 0.105(2) Uani 1 1 d . . . . .
H4 H -0.033636 -0.104691 -0.524886 0.126 Uiso 1 1 calc R . . . .
O40 O 0.0476(5) 0.1427(5) -0.62592(16) 0.1143(18) Uani 1 1 d . . . . .
C15 C -0.2819(5) -0.2244(8) -0.59232(17) 0.108(3) Uani 1 1 d . . . . .
C50 C -0.3077(5) -0.2466(6) -0.67365(15) 0.0957(19) Uani 1 1 d . . . . .
H50 H -0.348795 -0.301899 -0.679424 0.115 Uiso 1 1 calc R . . . .
N31 N -0.0090(4) -0.2110(5) -0.60123(12) 0.0872(14) Uani 1 1 d . . . . .
H31 H -0.033572 -0.180985 -0.598159 0.105 Uiso 1 1 calc R . . . .
C1 C 0.0145(6) -0.2062(8) -0.50632(16) 0.106(2) Uani 1 1 d . . . . .
H1A H -0.043036 -0.218804 -0.500990 0.128 Uiso 1 1 calc R . . . .
H1B H 0.041184 -0.215878 -0.489686 0.128 Uiso 1 1 calc R . . . .
C42 C -0.1200(5) -0.0059(5) -0.64305(15) 0.0880(15) Uani 1 1 d . . . . .
C34 C 0.2045(5) -0.0120(8) -0.59587(18) 0.109(3) Uani 1 1 d . . . . .
H34 H 0.240869 -0.031387 -0.589272 0.130 Uiso 1 1 calc R . . . .
C29 C -0.0590(4) -0.2945(5) -0.60420(12) 0.0869(16) Uani 1 1 d D . . . .
C6 C 0.0063(8) 0.0382(8) -0.54616(18) 0.119(3) Uani 1 1 d . . . . .
C22 C -0.1524(5) -0.3210(5) -0.60324(12) 0.0884(16) Uani 1 1 d D . . . .
O55 O -0.4781(6) -0.2941(11) -0.6880(2) 0.169(5) Uani 1 1 d . . . . .
N70 N 0.1790(5) -0.2885(6) -0.63672(14) 0.0987(17) Uani 1 1 d . . . . .
H70 H 0.140660 -0.338772 -0.642647 0.118 Uiso 1 1 calc R . . . .
C24 C -0.2983(5) -0.4307(7) -0.61446(18) 0.104(2) Uani 1 1 d . . . . .
N62 N 0.0714(4) -0.2903(5) -0.68512(14) 0.0914(14) Uani 1 1 d . . . . .
H62 H 0.044269 -0.345023 -0.688139 0.110 Uiso 1 1 calc R . . . .
C12 C -0.2067(7) -0.0652(8) -0.57632(18) 0.111(3) Uani 1 1 d . . . . .
C46 C -0.2661(5) -0.0989(7) -0.66090(15) 0.100(2) Uani 1 1 d . . . . .
N11 N -0.0699(6) -0.0228(6) -0.55590(12) 0.106(2) Uani 1 1 d . . . . .
C51 C -0.3289(5) -0.1833(8) -0.67024(15) 0.102(2) Uani 1 1 d . . . . .
C33 C 0.1199(4) -0.0697(6) -0.60429(13) 0.0928(19) Uani 1 1 d D . . . .
C10 C -0.1275(7) 0.0006(7) -0.56656(17) 0.106(2) Uani 1 1 d . . . . .
C2 C 0.0666(6) -0.1149(10) -0.5159(2) 0.121(3) Uani 1 1 d . . . . .
C45 C -0.2810(8) -0.0273(10) -0.6589(2) 0.116(3) Uani 1 1 d . . . . .
H45 H -0.334040 -0.033696 -0.664047 0.139 Uiso 1 1 calc R . . . .
C60 C 0.0265(4) -0.2506(5) -0.68034(14) 0.0839(14) Uani 1 1 d . . . . .
C23 C -0.2147(6) -0.4091(7) -0.61175(18) 0.111(3) Uani 1 1 d . . . . .
H23 H -0.197361 -0.449281 -0.615225 0.133 Uiso 1 1 calc R . . . .
C36 C 0.1804(6) 0.1046(7) -0.6073(2) 0.115(3) Uani 1 1 d . . . . .
H36 H 0.200005 0.163342 -0.608900 0.138 Uiso 1 1 calc R . . . .
O90 O 0.1104(6) -0.4207(7) -0.59582(17) 0.124(2) Uani 1 1 d . . . . .
C65 C 0.2984(7) -0.2567(11) -0.7009(3) 0.131(4) Uani 1 1 d . . . . .
H65 H 0.315680 -0.253718 -0.680734 0.157 Uiso 1 1 calc R . . . .
C71 C 0.2169(7) -0.2798(9) -0.6086(2) 0.115(3) Uani 1 1 d . . . . .
H71 H 0.233926 -0.222718 -0.600732 0.138 Uiso 1 1 calc R . . . .
C7 C 0.0332(11) 0.1316(9) -0.5481(2) 0.128(4) Uani 1 1 d . . . . .
H7 H 0.087385 0.174214 -0.541878 0.154 Uiso 1 1 calc R . . . .
N78 N 0.1403(7) -0.3202(10) -0.56343(18) 0.133(3) Uani 1 1 d . . . . .
H78 H 0.170047 -0.266057 -0.559632 0.160 Uiso 1 1 calc R . . . .
O3 O 0.1446(5) -0.0796(8) -0.5152(2) 0.146(3) Uani 1 1 d . . . . .
O54 O -0.4274(8) -0.1543(12) -0.7033(2) 0.177(5) Uani 1 1 d . . . . .
O13 O -0.2707(6) -0.0564(8) -0.58153(19) 0.143(3) Uani 1 1 d . . . . .
C5 C 0.0666(7) 0.0106(9) -0.53473(18) 0.118(3) Uani 1 1 d . . . . .
H5A H 0.106997 0.016601 -0.549692 0.141 Uiso 1 1 calc R . . . .
H5B H 0.099407 0.047976 -0.518908 0.141 Uiso 1 1 calc R . . . .
C43 C -0.1331(8) 0.0641(7) -0.64046(19) 0.108(2) Uani 1 1 d . . . . .
H43 H -0.091048 0.117338 -0.633398 0.130 Uiso 1 1 calc R . . . .
C77 C 0.1485(7) -0.3513(10) -0.58817(17) 0.117(3) Uani 1 1 d . . . . .
C16 C -0.3633(6) -0.2358(11) -0.5962(2) 0.127(4) Uani 1 1 d . . . . .
H16 H -0.376482 -0.192786 -0.592360 0.153 Uiso 1 1 calc R . . . .
C68 C 0.2022(5) -0.2197(7) -0.65383(16) 0.097(2) Uani 1 1 d . . . . .
C39 C 0.0314(5) 0.0643(5) -0.62518(16) 0.0955(19) Uani 1 1 d . . . . .
C63 C 0.1682(5) -0.2420(6) -0.68536(17) 0.0961(18) Uani 1 1 d . . . . .
H63 H 0.188007 -0.187983 -0.695902 0.115 Uiso 1 1 calc R . . . .
C82 C 0.103(2) -0.444(2) -0.5275(8) 0.199(10) Uani 1 1 d . . . . .
C32 C 0.0841(5) -0.1652(6) -0.60269(14) 0.0941(19) Uani 1 1 d D . . . .
H32A H 0.102241 -0.184066 -0.619492 0.113 Uiso 1 1 calc R . . . .
H32B H 0.107015 -0.178626 -0.585814 0.113 Uiso 1 1 calc R . . . .
N83 N 0.171(2) -0.4131(16) -0.5180(6) 0.203(9) Uani 1 1 d D . . . .
H83 H 0.211915 -0.364277 -0.524049 0.244 Uiso 1 1 calc R . . . .
C35 C 0.2316(7) 0.0734(9) -0.5977(2) 0.127(4) Uani 1 1 d . . . . .
H35 H 0.287713 0.112548 -0.592089 0.153 Uiso 1 1 calc R . . . .
C67 C 0.3407(8) -0.1754(12) -0.7116(4) 0.145(5) Uani 1 1 d . . . . .
H67A H 0.302364 -0.166102 -0.723490 0.218 Uiso 1 1 calc GR . . . .
H67B H 0.389107 -0.167636 -0.722778 0.218 Uiso 1 1 calc GR . . . .
H67C H 0.360728 -0.134749 -0.695989 0.218 Uiso 1 1 calc GR . . . .
C80 C 0.0585(17) -0.3316(18) -0.5189(3) 0.173(8) Uani 1 1 d . . . . .
H80A H 0.112781 -0.289674 -0.510291 0.208 Uiso 1 1 calc R . . . .
H80B H 0.021176 -0.368985 -0.503840 0.208 Uiso 1 1 calc R . . . .
C44 C -0.2184(8) 0.0474(10) -0.6498(2) 0.119(3) Uani 1 1 d . . . . .
H44 H -0.228986 0.093217 -0.649119 0.143 Uiso 1 1 calc R . . . .
C9 C -0.1055(12) 0.0892(10) -0.5670(2) 0.135(5) Uani 1 1 d . . . . .
H9 H -0.145521 0.104986 -0.572691 0.162 Uiso 1 1 calc R . . . .
C72 C 0.2965(8) -0.2912(14) -0.6106(3) 0.155(6) Uani 1 1 d . . . . .
H72A H 0.334472 -0.256321 -0.625947 0.186 Uiso 1 1 calc R . . . .
H72B H 0.279443 -0.351120 -0.613952 0.186 Uiso 1 1 calc R . . . .
O92 O 0.0933(10) -0.4809(12) -0.6569(3) 0.185(5) Uani 1 1 d D . . . .
C66 C 0.3187(12) -0.3195(17) -0.7161(4) 0.169(7) Uani 1 1 d . . . . .
H66A H 0.304314 -0.322241 -0.736142 0.253 Uiso 1 1 calc GR . . . .
H66B H 0.285486 -0.375699 -0.707705 0.253 Uiso 1 1 calc GR . . . .
H66C H 0.378988 -0.300316 -0.714220 0.253 Uiso 1 1 calc GR . . . .
C17 C -0.4271(7) -0.3210(13) -0.6068(3) 0.141(5) Uani 1 1 d . . . . .
H17 H -0.482613 -0.331605 -0.610404 0.170 Uiso 1 1 calc R . . . .
N58 N -0.1087(3) -0.2585(4) -0.67288(11) 0.0797(11) Uani 1 1 d . . . . .
H58 H -0.075567 -0.206454 -0.667092 0.096 Uiso 1 1 calc R . . . .
O53 O -0.4744(4) -0.1957(7) -0.65398(19) 0.135(3) Uani 1 1 d . . . . .
O94 O 0.1487(17) -0.5708(19) -0.5952(9) 0.262(12) Uani 1 1 d D . . . .
O28 O -0.4349(7) -0.5769(7) -0.6005(2) 0.172(5) Uani 1 1 d . . . . .
N14 N -0.2102(4) -0.1429(5) -0.58107(13) 0.0953(16) Uani 1 1 d . . . . .
H14 H -0.164011 -0.144029 -0.576880 0.114 Uiso 1 1 calc R . . . .
C18 C -0.4102(6) -0.3843(10) -0.6117(3) 0.130(4) Uani 1 1 d . . . . .
H18 H -0.454064 -0.437896 -0.617900 0.156 Uiso 1 1 calc R . . . .
C73 C 0.3411(10) -0.2608(19) -0.5810(4) 0.182(9) Uani 1 1 d D . . . .
H73A H 0.344182 -0.206682 -0.576034 0.218 Uiso 1 1 calc R . . . .
H73B H 0.306460 -0.302924 -0.566530 0.218 Uiso 1 1 calc R . . . .
C64 C 0.1993(5) -0.2965(7) -0.70152(17) 0.099(2) Uani 1 1 d . . . . .
H64A H 0.180425 -0.302927 -0.721366 0.119 Uiso 1 1 calc R . . . .
H64B H 0.172671 -0.353563 -0.693011 0.119 Uiso 1 1 calc R . . . .
C8 C -0.0224(14) 0.1511(10) -0.5587(3) 0.141(5) Uani 1 1 d . . . . .
H8 H -0.005713 0.208978 -0.560907 0.170 Uiso 1 1 calc R . . . .
Ca89 Ca 0.0302(4) -0.5636(3) -0.61415(11) 0.1734(14) Uani 1 1 d D . . . .
C74 C 0.4292(12) -0.249(2) -0.5808(6) 0.200(11) Uani 1 1 d D . . . .
H74A H 0.459424 -0.217919 -0.597987 0.240 Uiso 1 1 calc R . . . .
H74B H 0.425209 -0.304743 -0.581100 0.240 Uiso 1 1 calc R . . . .
C79 C 0.0745(11) -0.3855(13) -0.5413(3) 0.146(5) Uani 1 1 d . . . . .
H79 H 0.020128 -0.421806 -0.551432 0.175 Uiso 1 1 calc R . . . .
O88 O 0.0440(19) -0.526(3) -0.5239(7) 0.273(13) Uani 1 1 d . . . . .
O91 O -0.0605(11) -0.5057(12) -0.6249(5) 0.203(7) Uani 1 1 d D . . . .
O93 O -0.0429(19) -0.662(2) -0.6526(8) 0.286(15) Uani 1 1 d D . . . .
O87 O 0.1688(18) -0.5540(17) -0.5286(6) 0.245(9) Uiso 1 1 d D . . . .
O27 O -0.4156(8) -0.5299(9) -0.6498(2) 0.183(6) Uani 1 1 d . . . . .
O26 O -0.3266(12) -0.5811(8) -0.6289(3) 0.183(6) Uani 1 1 d . . . . .
N76 N 0.5063(19) -0.119(3) -0.5445(5) 0.31(2) Uani 1 1 d . . . . .
H76A H 0.492469 -0.085684 -0.553816 0.377 Uiso 1 1 calc R . . . .
H76B H 0.536042 -0.100443 -0.528991 0.377 Uiso 1 1 calc R . . . .
C75 C 0.4813(17) -0.199(3) -0.5544(9) 0.28(2) Uani 1 1 d . . . . .
H75A H 0.450587 -0.236225 -0.538376 0.337 Uiso 1 1 calc R . . . .
H75B H 0.534605 -0.200098 -0.556048 0.337 Uiso 1 1 calc R . . . .
O69 O 0.2483(5) -0.1478(6) -0.64700(18) 0.1192(19) Uani 1 1 d . . . . .
C84 C 0.185(2) -0.4625(16) -0.4942(8) 0.27(2) Uani 1 1 d D . . . .
H84A H 0.231323 -0.421730 -0.481861 0.328 Uiso 1 1 calc R . . . .
H84B H 0.133361 -0.491675 -0.482701 0.328 Uiso 1 1 calc R . . . .
O95 O -0.028(3) -0.625(3) -0.5682(7) 0.36(3) Uani 1 1 d D . . . .
O86 O 0.2538(18) -0.5317(19) -0.4842(7) 0.250 Uiso 1 1 d D . . . .
C85 C 0.2083(19) -0.529(2) -0.5047(7) 0.250 Uiso 1 1 d D . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0050 0.0020 '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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1490 0.1570 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C80 S81 C1 99.7(7) . . ?
O55 S52 C51 106.2(5) . . ?
O55 S52 O54 111.5(9) . . ?
O55 S52 O53 112.4(7) . . ?
O54 S52 C51 105.6(6) . . ?
O54 S52 O53 114.2(7) . . ?
O53 S52 C51 106.2(4) . . ?
O28 S25 C24 107.7(7) . . ?
O27 S25 C24 105.3(7) . . ?
O27 S25 O28 112.3(8) . . ?
O26 S25 C24 106.3(7) . . ?
O26 S25 O28 110.6(9) . . ?
O26 S25 O27 114.1(11) . . ?
C22 N21 C20 120.6(8) . . ?
C49 N48 C47 119.5(6) . . ?
O57 C56 C49 123.6(6) . . ?
O57 C56 N58 122.0(7) . . ?
N58 C56 C49 114.4(6) . . ?
N58 C59 C60 106.1(5) . . ?
C33 N38 C37 118.8(7) . . ?
N21 C20 C19 119.0(9) . . ?
C15 C20 N21 119.5(9) . . ?
C15 C20 C19 121.5(8) . . ?
N48 C49 C56 118.9(5) . . ?
N48 C49 C50 122.5(7) . . ?
C50 C49 C56 118.7(7) . . ?
N48 C47 C42 118.3(6) . . ?
N48 C47 C46 122.3(8) . . ?
C42 C47 C46 119.3(8) . . ?
C39 N41 C42 130.0(7) . . ?
N38 C37 C36 123.0(10) . . ?
N38 C37 C39 115.4(7) . . ?
C36 C37 C39 121.6(9) . . ?
C20 C19 C18 115.9(13) . . ?
C24 C19 C20 119.2(8) . . ?
C24 C19 C18 124.6(12) . . ?
C2 N4 C5 120.0(9) . . ?
C20 C15 C16 123.7(12) . . ?
C20 C15 N14 114.6(6) . . ?
C16 C15 N14 121.7(11) . . ?
C51 C50 C49 118.1(8) . . ?
C29 N31 C32 125.3(7) . . ?
C2 C1 S81 108.4(6) . . ?
N41 C42 C47 114.6(6) . . ?
C43 C42 C47 122.6(8) . . ?
C43 C42 N41 122.8(8) . . ?
C35 C34 C33 117.4(10) . . ?
O30 C29 N31 122.7(7) . . ?
O30 C29 C22 125.1(8) . . ?
N31 C29 C22 112.1(7) . . ?
N11 C6 C7 121.6(12) . . ?
N11 C6 C5 117.6(11) . . ?
C5 C6 C7 120.6(12) . . ?
N21 C22 C29 119.6(7) . . ?
N21 C22 C23 122.6(8) . . ?
C23 C22 C29 117.7(8) . . ?
C68 N70 C71 121.5(9) . . ?
C19 C24 S25 121.2(7) . . ?
C23 C24 S25 118.5(10) . . ?
C23 C24 C19 120.1(9) . . ?
C60 N62 C63 121.7(7) . . ?
O13 C12 C10 124.5(12) . . ?
O13 C12 N14 120.8(12) . . ?
N14 C12 C10 114.7(8) . . ?
C47 C46 C51 116.3(8) . . ?
C47 C46 C45 119.2(10) . . ?
C51 C46 C45 124.5(8) . . ?
C6 N11 C10 119.1(10) . . ?
C50 C51 S52 117.2(8) . . ?
C50 C51 C46 120.9(6) . . ?
C46 C51 S52 121.8(7) . . ?
N38 C33 C34 122.5(9) . . ?
N38 C33 C32 116.4(6) . . ?
C34 C33 C32 121.1(8) . . ?
C12 C10 C9 122.1(11) . . ?
N11 C10 C12 117.4(9) . . ?
N11 C10 C9 120.5(12) . . ?
N4 C2 C1 116.4(8) . . ?
O3 C2 N4 124.3(14) . . ?
O3 C2 C1 119.3(12) . . ?
C44 C45 C46 119.0(9) . . ?
O61 C60 C59 121.8(6) . . ?
O61 C60 N62 124.6(6) . . ?
N62 C60 C59 113.5(7) . . ?
C24 C23 C22 118.3(11) . . ?
C35 C36 C37 115.1(11) . . ?
C77 O90 Ca89 177.1(8) . . ?
C67 C65 C66 114.3(15) . . ?
C67 C65 C64 112.6(10) . . ?
C66 C65 C64 107.0(13) . . ?
N70 C71 C77 109.1(8) . . ?
N70 C71 C72 110.3(9) . . ?
C72 C71 C77 108.9(11) . . ?
C8 C7 C6 117.3(14) . . ?
C77 N78 C79 117.5(14) . . ?
N4 C5 C6 111.7(9) . . ?
C42 C43 C44 114.7(11) . . ?
O90 C77 C71 120.0(9) . . ?
O90 C77 N78 127.1(14) . . ?
N78 C77 C71 112.9(13) . . ?
C15 C16 C17 114.6(14) . . ?
N70 C68 C63 114.8(8) . . ?
O69 C68 N70 124.8(8) . . ?
O69 C68 C63 120.3(9) . . ?
N41 C39 C37 114.5(8) . . ?
O40 C39 N41 123.2(9) . . ?
O40 C39 C37 122.3(8) . . ?
N62 C63 C68 109.3(6) . . ?
N62 C63 C64 108.6(7) . . ?
C64 C63 C68 113.7(7) . . ?
N83 C82 C79 118(3) . . ?
N83 C82 O88 124(4) . . ?
O88 C82 C79 118(3) . . ?
N31 C32 C33 111.3(6) . . ?
C82 N83 C84 117(3) . . ?
C34 C35 C36 123.2(9) . . ?
C79 C80 S81 110.0(11) . . ?
C45 C44 C43 125.0(10) . . ?
C8 C9 C10 118.0(13) . . ?
C71 C72 C73 104.4(14) . . ?
C18 C17 C16 123.8(10) . . ?
C56 N58 C59 122.2(6) . . ?
C12 N14 C15 129.3(7) . . ?
C17 C18 C19 120.3(13) . . ?
C74 C73 C72 112.6(18) . . ?
C63 C64 C65 113.2(9) . . ?
C7 C8 C9 123.2(14) . . ?
O90 Ca89 O92 77.8(6) . . ?
O90 Ca89 O93 150.9(11) . . ?
O90 Ca89 O95 93.5(11) . . ?
O94 Ca89 O90 81.4(8) . . ?
O94 Ca89 O92 100.6(11) . . ?
O94 Ca89 O91 158.7(9) . . ?
O94 Ca89 O93 114.6(12) . . ?
O94 Ca89 O95 80.9(14) . . ?
O91 Ca89 O90 77.4(5) . . ?
O91 Ca89 O92 76.7(7) . . ?
O91 Ca89 O93 85.5(10) . . ?
O91 Ca89 O95 98.5(12) . . ?
O93 Ca89 O92 75.5(11) . . ?
O93 Ca89 O95 112.3(15) . . ?
O95 Ca89 O92 170.7(12) . . ?
C73 C74 C75 112.7(18) . . ?
C82 C79 N78 114.2(15) . . ?
C82 C79 C80 112.3(16) . . ?
C80 C79 N78 106.5(16) . . ?
N76 C75 C74 132(4) . . ?
C85 C84 N83 114(3) . . ?
O87 C85 C84 104(2) . . ?
O87 C85 O86 153(4) . . ?
O86 C85 C84 103(2) . . ?
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
S81 C1 1.837(10) . ?
S81 C80 1.813(15) . ?
S52 O55 1.360(16) . ?
S52 C51 1.799(7) . ?
S52 O54 1.431(13) . ?
S52 O53 1.461(9) . ?
S25 C24 1.771(10) . ?
S25 O28 1.463(13) . ?
S25 O27 1.437(11) . ?
S25 O26 1.43(2) . ?
O57 C56 1.236(10) . ?
N21 C20 1.395(10) . ?
N21 C22 1.290(11) . ?
N48 C49 1.331(10) . ?
N48 C47 1.361(10) . ?
C56 C49 1.461(11) . ?
C56 N58 1.368(8) . ?
C59 C60 1.517(9) . ?
C59 N58 1.461(9) . ?
N38 C37 1.341(12) . ?
N38 C33 1.317(11) . ?
C20 C19 1.435(16) . ?
C20 C15 1.355(15) . ?
C49 C50 1.422(9) . ?
C47 C42 1.409(12) . ?
C47 C46 1.418(10) . ?
O61 C60 1.211(10) . ?
N41 C42 1.398(10) . ?
N41 C39 1.351(11) . ?
C37 C36 1.419(12) . ?
C37 C39 1.479(14) . ?
O30 C29 1.235(10) . ?
C19 C24 1.411(18) . ?
C19 C18 1.444(14) . ?
N4 C2 1.359(15) . ?
N4 C5 1.424(17) . ?
O40 C39 1.284(12) . ?
C15 C16 1.379(12) . ?
C15 N14 1.476(15) . ?
C50 C51 1.373(14) . ?
N31 C29 1.311(11) . ?
N31 C32 1.446(9) . ?
C1 C2 1.489(19) . ?
C42 C43 1.391(12) . ?
C34 C33 1.398(11) . ?
C34 C35 1.36(2) . ?
C29 C22 1.494(10) . ?
C6 N11 1.330(15) . ?
C6 C7 1.494(19) . ?
C6 C5 1.493(18) . ?
C22 C23 1.460(13) . ?
N70 C71 1.446(10) . ?
N70 C68 1.345(13) . ?
C24 C23 1.352(15) . ?
N62 C60 1.332(10) . ?
N62 C63 1.502(10) . ?
C12 C10 1.391(18) . ?
C12 O13 1.256(12) . ?
C12 N14 1.380(15) . ?
C46 C51 1.428(16) . ?
C46 C45 1.436(16) . ?
N11 C10 1.384(13) . ?
C33 C32 1.498(13) . ?
C10 C9 1.432(17) . ?
C2 O3 1.212(14) . ?
C45 C44 1.31(2) . ?
C36 C35 1.37(2) . ?
O90 C77 1.135(17) . ?
O90 Ca89 2.380(12) . ?
C65 C67 1.36(2) . ?
C65 C66 1.52(2) . ?
C65 C64 1.547(12) . ?
C71 C77 1.572(19) . ?
C71 C72 1.541(16) . ?
C7 C8 1.31(3) . ?
N78 C77 1.318(13) . ?
N78 C79 1.56(2) . ?
C43 C44 1.468(17) . ?
C16 C17 1.46(3) . ?
C68 C63 1.562(10) . ?
C68 O69 1.174(13) . ?
C63 C64 1.539(12) . ?
C82 N83 1.15(4) . ?
C82 C79 1.52(4) . ?
C82 O88 1.31(5) . ?
N83 C84 1.52(2) . ?
C80 C79 1.54(2) . ?
C9 C8 1.39(3) . ?
C72 C73 1.55(2) . ?
O92 Ca89 2.397(15) . ?
C17 C18 1.33(3) . ?
O94 Ca89 2.359(18) . ?
C73 C74 1.483(19) . ?
Ca89 O91 2.378(15) . ?
Ca89 O93 2.39(2) . ?
Ca89 O95 2.39(2) . ?
C74 C75 1.53(3) . ?
O87 C85 1.27(3) . ?
N76 C75 1.35(5) . ?
C84 C85 1.51(3) . ?
O86 C85 1.27(3) . ?
