# Supplementary Information (SI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_naqian
_database_code_depnum_ccdc_archive 'CCDC 2395054'
loop_
_audit_author_name
_audit_author_address
'Anton Cherkasov'
;IOMC RAS
Russia
;
_audit_update_record             
;
2024-10-30 deposited with the CCDC.	2025-02-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C122.50 H140 N4 Na4 O8'
_chemical_formula_sum            'C122.50 H140 N4 Na4 O8'
_chemical_formula_weight         1888.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   25.1779(12)
_cell_length_b                   17.1245(9)
_cell_length_c                   24.3955(12)
_cell_angle_alpha                90
_cell_angle_beta                 100.4410(10)
_cell_angle_gamma                90
_cell_volume                     10344.2(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9925
_cell_measurement_theta_min      2.70
_cell_measurement_theta_max      30.42

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_F_000             4044
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.570
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.390
_exptl_absorpt_coefficient_mu    0.089
_shelx_estimated_absorpt_T_min   0.951
_shelx_estimated_absorpt_T_max   0.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus source'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            117093
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.312
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             22781
_reflns_number_gt                18257
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       APEX2
_computing_cell_refinement       'Saint 8.34a'
_computing_data_reduction        'Saint 8.34a'
_computing_structure_solution    'SHELXT 2018/2'
_computing_structure_refinement  'SHELXL 2018/3'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0708P)²+6.8186P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         22781
_refine_ls_number_parameters     1389
_refine_ls_number_restraints     1876
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0523
_refine_ls_wR_factor_ref         0.1444
_refine_ls_wR_factor_gt          0.1337
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

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
Na1 Na 0.77414(3) 0.37406(4) 0.25100(3) 0.02249(14) Uani 1 1 d . . . . .
Na2 Na 0.76962(3) 0.55870(4) 0.21703(3) 0.02229(14) Uani 1 1 d . . . . .
Na3 Na 0.75817(3) 0.49247(4) 0.35002(3) 0.02128(14) Uani 1 1 d . . . . .
Na4 Na 0.65884(3) 0.48941(4) 0.24196(3) 0.02092(14) Uani 1 1 d . . . . .
O1 O 0.81966(4) 0.48184(7) 0.28817(5) 0.0215(2) Uani 1 1 d . . . . .
O2 O 0.71631(5) 0.58317(6) 0.28347(5) 0.0218(2) Uani 1 1 d . . . . .
O3 O 0.70516(5) 0.39761(6) 0.30382(5) 0.0217(2) Uani 1 1 d . . . . .
O4 O 0.71989(5) 0.45204(6) 0.18388(5) 0.0214(2) Uani 1 1 d . . . . .
N1 N 0.83979(6) 0.58156(9) 0.39054(6) 0.0228(3) Uani 1 1 d . . . . .
H1A H 0.8247(8) 0.6213(11) 0.3807(8) 0.027 Uiso 1 1 d . U . . .
N2 N 0.79323(7) 0.70276(8) 0.25631(7) 0.0257(3) Uani 1 1 d . . . . .
H2A H 0.8185(7) 0.6812(13) 0.2758(9) 0.031 Uiso 1 1 d . U . . .
N3 N 0.60188(5) 0.36449(8) 0.22574(6) 0.0194(3) Uani 1 1 d . . . . .
H3A H 0.6139(8) 0.3555(11) 0.1972(7) 0.023 Uiso 1 1 d . U . . .
N4 N 0.72525(6) 0.27766(8) 0.17479(6) 0.0189(3) Uani 1 1 d . . . . .
H4A H 0.7054(8) 0.2652(9) 0.1945(8) 0.023 Uiso 1 1 d . U . . .
C1 C 0.86371(7) 0.52016(9) 0.30624(7) 0.0209(3) Uani 1 1 d . . . . .
C2 C 0.87597(7) 0.56829(10) 0.35232(7) 0.0230(3) Uani 1 1 d . . . . .
C3 C 0.93185(7) 0.59516(10) 0.35849(7) 0.0248(3) Uani 1 1 d . . . . .
C4 C 0.95230(7) 0.56186(10) 0.31324(7) 0.0247(3) Uani 1 1 d . . . . .
C5 C 0.91249(7) 0.51706(10) 0.27969(7) 0.0230(3) Uani 1 1 d . . . . .
C6 C 0.92474(8) 0.47962(11) 0.23432(8) 0.0305(4) Uani 1 1 d . . . . .
H6A H 0.898389 0.449365 0.210678 0.037 Uiso 1 1 calc R U . . .
C7 C 0.97788(8) 0.48706(13) 0.22335(9) 0.0378(5) Uani 1 1 d . . . . .
H7A H 0.986877 0.461229 0.191799 0.045 Uiso 1 1 calc R U . . .
C8 C 1.01667(8) 0.53019(12) 0.25667(9) 0.0365(4) Uani 1 1 d . . . . .
H8A H 1.051954 0.533343 0.248125 0.044 Uiso 1 1 calc R U . . .
C9 C 1.00470(7) 0.57023(11) 0.30384(8) 0.0295(4) Uani 1 1 d . . . . .
C10 C 1.03956(8) 0.61748(12) 0.34258(8) 0.0355(4) Uani 1 1 d . . . . .
H10A H 1.075890 0.625907 0.338341 0.043 Uiso 1 1 calc R U . . .
C11 C 1.02032(8) 0.65061(12) 0.38592(8) 0.0359(4) Uani 1 1 d . . . . .
H11A H 1.044021 0.682590 0.411178 0.043 Uiso 1 1 calc R U . . .
C12 C 0.96661(8) 0.63986(11) 0.39534(8) 0.0309(4) Uani 1 1 d . . . . .
H12A H 0.955143 0.663219 0.426542 0.037 Uiso 1 1 calc R U . . .
C13 C 0.86274(7) 0.57797(10) 0.44861(7) 0.0235(3) Uani 1 1 d . . . . .
C14 C 0.88917(7) 0.50961(11) 0.47022(7) 0.0258(4) Uani 1 1 d . . . . .
C15 C 0.91407(7) 0.50888(12) 0.52597(8) 0.0307(4) Uani 1 1 d . . . . .
H15A H 0.933069 0.463448 0.540820 0.037 Uiso 1 1 calc R U . . .
C16 C 0.91192(8) 0.57209(13) 0.56010(8) 0.0339(4) Uani 1 1 d . . . . .
H16A H 0.930316 0.571018 0.597709 0.041 Uiso 1 1 calc R U . . .
C17 C 0.88287(8) 0.63699(12) 0.53934(8) 0.0325(4) Uani 1 1 d . . . . .
H17A H 0.880202 0.679808 0.563460 0.039 Uiso 1 1 calc R U . . .
C18 C 0.85726(7) 0.64143(11) 0.48380(7) 0.0284(4) Uani 1 1 d . . . . .
C19 C 0.89095(7) 0.43525(10) 0.43669(8) 0.0274(4) Uani 1 1 d . . . . .
H19A H 0.869664 0.444183 0.398444 0.033 Uiso 1 1 calc R U . . .
C20 C 0.86507(8) 0.36735(12) 0.46305(8) 0.0337(4) Uani 1 1 d . . . . .
H20A H 0.828379 0.381839 0.467291 0.051 Uiso 1 1 calc R U . . .
H20B H 0.886647 0.355479 0.499711 0.051 Uiso 1 1 calc R U . . .
H20C H 0.863616 0.321257 0.439014 0.051 Uiso 1 1 calc R U . . .
C21 C 0.94885(8) 0.41575(12) 0.43125(9) 0.0337(4) Uani 1 1 d . . . . .
H21A H 0.963560 0.458098 0.411477 0.051 Uiso 1 1 calc R U . . .
H21B H 0.949292 0.366976 0.410320 0.051 Uiso 1 1 calc R U . . .
H21C H 0.970921 0.409638 0.468444 0.051 Uiso 1 1 calc R U . . .
C22 C 0.82441(9) 0.71407(11) 0.46376(8) 0.0351(4) Uani 1 1 d . . . . .
H22A H 0.798039 0.699483 0.429518 0.042 Uiso 1 1 calc R U . . .
C23 C 0.79248(9) 0.74505(13) 0.50617(9) 0.0403(5) Uani 1 1 d . . . . .
H23A H 0.770852 0.790002 0.490451 0.060 Uiso 1 1 calc R U . . .
H23B H 0.817412 0.761173 0.539908 0.060 Uiso 1 1 calc R U . . .
H23C H 0.768530 0.703997 0.515570 0.060 Uiso 1 1 calc R U . . .
C24 C 0.86037(12) 0.77732(15) 0.44787(13) 0.0621(7) Uani 1 1 d . . . . .
H24A H 0.877540 0.758909 0.417273 0.093 Uiso 1 1 calc R U . . .
H24B H 0.888244 0.790327 0.480093 0.093 Uiso 1 1 calc R U . . .
H24C H 0.838699 0.823864 0.435895 0.093 Uiso 1 1 calc R U . . .
C25 C 0.72162(7) 0.65269(9) 0.30405(7) 0.0206(3) Uani 1 1 d . . . . .
C26 C 0.75486(7) 0.71285(9) 0.29258(7) 0.0241(3) Uani 1 1 d . . . . .
C27 C 0.74557(7) 0.78239(10) 0.32380(7) 0.0252(3) Uani 1 1 d . . . . .
C28 C 0.70743(7) 0.76040(9) 0.35728(7) 0.0223(3) Uani 1 1 d . . . . .
C29 C 0.69201(6) 0.68230(9) 0.34741(7) 0.0208(3) Uani 1 1 d . . . . .
C30 C 0.65682(7) 0.64971(10) 0.37723(7) 0.0258(4) Uani 1 1 d . . . . .
H30A H 0.645212 0.597152 0.370960 0.031 Uiso 1 1 calc R U . . .
C31 C 0.63804(7) 0.69610(11) 0.41770(8) 0.0299(4) Uani 1 1 d . . . . .
H31A H 0.613915 0.673686 0.439058 0.036 Uiso 1 1 calc R U . . .
C32 C 0.65355(7) 0.77248(11) 0.42712(7) 0.0283(4) Uani 1 1 d . . . . .
H32A H 0.640486 0.801642 0.455040 0.034 Uiso 1 1 calc R U . . .
C33 C 0.68887(7) 0.80816(10) 0.39556(7) 0.0251(3) Uani 1 1 d . . . . .
C34 C 0.70803(8) 0.88653(11) 0.39880(8) 0.0315(4) Uani 1 1 d . . . . .
H34A H 0.696572 0.922365 0.424015 0.038 Uiso 1 1 calc R U . . .
C35 C 0.74304(9) 0.90963(11) 0.36529(9) 0.0358(4) Uani 1 1 d . . . . .
H35A H 0.754710 0.962474 0.367233 0.043 Uiso 1 1 calc R U . . .
C36 C 0.76295(8) 0.85875(10) 0.32764(9) 0.0325(4) Uani 1 1 d . . . . .
H36A H 0.787787 0.877101 0.305548 0.039 Uiso 1 1 calc R U . . .
C37 C 0.80346(8) 0.76648(9) 0.22188(8) 0.0272(4) Uani 1 1 d . . . . .
C38 C 0.85617(8) 0.79609(10) 0.22619(9) 0.0332(4) Uani 1 1 d . . . . .
C39 C 0.86456(9) 0.85705(11) 0.19097(10) 0.0402(5) Uani 1 1 d . . . . .
H39A H 0.899894 0.877870 0.193534 0.048 Uiso 1 1 calc R U . . .
C40 C 0.82340(9) 0.88778(11) 0.15283(10) 0.0425(5) Uani 1 1 d . . . . .
H40A H 0.830079 0.929823 0.129597 0.051 Uiso 1 1 calc R U . . .
C41 C 0.77232(9) 0.85745(11) 0.14833(9) 0.0364(5) Uani 1 1 d . . . . .
H41A H 0.743830 0.878780 0.121644 0.044 Uiso 1 1 calc R U . . .
C42 C 0.76139(8) 0.79601(10) 0.18209(8) 0.0293(4) Uani 1 1 d . . . . .
C43 C 0.90428(8) 0.76719(12) 0.26800(10) 0.0397(5) Uani 1 1 d . . . . .
H43A H 0.895072 0.714511 0.281302 0.048 Uiso 1 1 calc R U . . .
C44 C 0.95580(9) 0.75936(15) 0.24422(12) 0.0510(6) Uani 1 1 d . . . . .
H44A H 0.948742 0.727208 0.210443 0.076 Uiso 1 1 calc R U . . .
H44B H 0.983820 0.734565 0.271858 0.076 Uiso 1 1 calc R U . . .
H44C H 0.968046 0.811251 0.235007 0.076 Uiso 1 1 calc R U . . .
C45 C 0.91438(11) 0.82159(17) 0.31791(11) 0.0580(7) Uani 1 1 d . . . . .
H45A H 0.881947 0.824155 0.334789 0.087 Uiso 1 1 calc R U . . .
H45B H 0.923033 0.873898 0.305799 0.087 Uiso 1 1 calc R U . . .
H45C H 0.944700 0.801850 0.345375 0.087 Uiso 1 1 calc R U . . .
C46 C 0.70423(8) 0.76414(11) 0.17274(8) 0.0311(4) Uani 1 1 d . . . . .
H46A H 0.703705 0.718372 0.198094 0.037 Uiso 1 1 calc R U . . .
C47 C 0.68645(10) 0.73593(12) 0.11318(9) 0.0428(5) Uani 1 1 d . . . . .
H47A H 0.711934 0.696522 0.104557 0.064 Uiso 1 1 calc R U . . .
H47B H 0.685641 0.780131 0.087534 0.064 Uiso 1 1 calc R U . . .
H47C H 0.650297 0.712931 0.109053 0.064 Uiso 1 1 calc R U . . .
C48 C 0.66531(8) 0.82528(12) 0.18787(10) 0.0386(5) Uani 1 1 d . . . . .
H48A H 0.677558 0.842378 0.226422 0.058 Uiso 1 1 calc R U . . .
H48B H 0.629099 0.802598 0.184125 0.058 Uiso 1 1 calc R U . . .
H48C H 0.664261 0.870167 0.162774 0.058 Uiso 1 1 calc R U . . .
C49 C 0.67830(6) 0.33296(9) 0.30179(6) 0.0187(3) Uani 1 1 d . . . . .
C50 C 0.63044(6) 0.31278(9) 0.26737(7) 0.0187(3) Uani 1 1 d . . . . .
C51 C 0.61493(6) 0.23350(9) 0.28016(7) 0.0199(3) Uani 1 1 d . . . . .
C52 C 0.65608(6) 0.20659(9) 0.32346(7) 0.0195(3) Uani 1 1 d . . . . .
C53 C 0.69554(7) 0.26434(9) 0.33821(7) 0.0201(3) Uani 1 1 d . . . . .
C54 C 0.73844(7) 0.24905(10) 0.37967(7) 0.0270(4) Uani 1 1 d . . . . .
H54A H 0.765723 0.287113 0.390748 0.032 Uiso 1 1 calc R U . . .
C55 C 0.74118(8) 0.17506(11) 0.40566(8) 0.0314(4) Uani 1 1 d . . . . .
H55A H 0.770938 0.163894 0.434522 0.038 Uiso 1 1 calc R U . . .
C56 C 0.70251(8) 0.11872(10) 0.39081(7) 0.0278(4) Uani 1 1 d . . . . .
H56A H 0.705869 0.069715 0.409365 0.033 Uiso 1 1 calc R U . . .
C57 C 0.65770(7) 0.13327(9) 0.34805(7) 0.0226(3) Uani 1 1 d . . . . .
C58 C 0.61437(8) 0.08194(10) 0.32688(7) 0.0269(4) Uani 1 1 d . . . . .
H58A H 0.613337 0.030727 0.341628 0.032 Uiso 1 1 calc R U . . .
C59 C 0.57446(7) 0.10687(10) 0.28536(8) 0.0284(4) Uani 1 1 d . . . . .
H59A H 0.545914 0.071825 0.271560 0.034 Uiso 1 1 calc R U . . .
C60 C 0.57333(7) 0.18279(10) 0.26156(7) 0.0244(3) Uani 1 1 d . . . . .
H60A H 0.544206 0.198198 0.233185 0.029 Uiso 1 1 calc R U . . .
C61 C 0.54458(6) 0.36888(9) 0.22029(7) 0.0206(3) Uani 1 1 d . . . . .
C62 C 0.52207(6) 0.39264(9) 0.26602(7) 0.0212(3) Uani 1 1 d . . . . .
C63 C 0.46593(7) 0.39285(10) 0.26075(7) 0.0251(3) Uani 1 1 d . . . . .
H63A H 0.450230 0.406344 0.292058 0.030 Uiso 1 1 calc R U . . .
C64 C 0.43280(7) 0.37395(11) 0.21124(8) 0.0296(4) Uani 1 1 d . . . . .
H64A H 0.394685 0.373201 0.208575 0.036 Uiso 1 1 calc R U . . .
C65 C 0.45562(7) 0.35621(11) 0.16577(8) 0.0295(4) Uani 1 1 d . . . . .
H65A H 0.432659 0.345696 0.131168 0.035 Uiso 1 1 calc R U . . .
C66 C 0.51107(7) 0.35314(10) 0.16869(7) 0.0248(3) Uani 1 1 d . . . . .
C67 C 0.55544(7) 0.42088(10) 0.32054(7) 0.0224(3) Uani 1 1 d . . . . .
H67A H 0.594061 0.423032 0.315873 0.027 Uiso 1 1 calc R U . . .
C68 C 0.53844(7) 0.50332(10) 0.33432(8) 0.0288(4) Uani 1 1 d . . . . .
H68A H 0.542534 0.538798 0.303838 0.043 Uiso 1 1 calc R U . . .
H68B H 0.561291 0.521191 0.368894 0.043 Uiso 1 1 calc R U . . .
H68C H 0.500610 0.502757 0.339038 0.043 Uiso 1 1 calc R U . . .
C69 C 0.55158(8) 0.36464(10) 0.36806(7) 0.0279(4) Uani 1 1 d . . . . .
H69A H 0.566326 0.313755 0.360144 0.042 Uiso 1 1 calc R U . . .
H69B H 0.513664 0.358554 0.371682 0.042 Uiso 1 1 calc R U . . .
H69C H 0.572253 0.385433 0.402913 0.042 Uiso 1 1 calc R U . . .
C70 C 0.53361(7) 0.33129(12) 0.11709(7) 0.0294(4) Uani 1 1 d . . . . .
H70A H 0.570251 0.355474 0.120901 0.035 Uiso 1 1 calc R U . . .
C71 C 0.50007(8) 0.36165(14) 0.06333(8) 0.0404(5) Uani 1 1 d . . . . .
H71A H 0.519429 0.352670 0.032492 0.061 Uiso 1 1 calc R U . . .
H71B H 0.493735 0.417738 0.066890 0.061 Uiso 1 1 calc R U . . .
H71C H 0.465366 0.334160 0.055897 0.061 Uiso 1 1 calc R U . . .
C72 C 0.54078(11) 0.24399(14) 0.11381(10) 0.0504(6) Uani 1 1 d . . . . .
H72A H 0.554541 0.231015 0.079841 0.076 Uiso 1 1 calc R U . . .
H72B H 0.505924 0.218134 0.113016 0.076 Uiso 1 1 calc R U . . .
H72C H 0.566522 0.226158 0.146455 0.076 Uiso 1 1 calc R U . . .
C73 C 0.69704(6) 0.41091(9) 0.14141(6) 0.0191(3) Uani 1 1 d . . . . .
C74 C 0.69718(6) 0.33087(9) 0.13406(6) 0.0191(3) Uani 1 1 d . . . . .
C75 C 0.66814(6) 0.31089(10) 0.07851(7) 0.0202(3) Uani 1 1 d . . . . .
C76 C 0.64955(6) 0.38239(9) 0.05288(7) 0.0199(3) Uani 1 1 d . . . . .
C77 C 0.66550(6) 0.44495(9) 0.08935(7) 0.0200(3) Uani 1 1 d . . . . .
C78 C 0.65178(7) 0.51913(10) 0.07159(7) 0.0256(3) Uani 1 1 d . . . . .
H78A H 0.662105 0.562768 0.095158 0.031 Uiso 1 1 calc R U . . .
C79 C 0.62177(8) 0.52918(11) 0.01713(8) 0.0302(4) Uani 1 1 d . . . . .
H79A H 0.611712 0.580525 0.004606 0.036 Uiso 1 1 calc R U . . .
C80 C 0.60662(7) 0.46769(11) -0.01829(7) 0.0272(4) Uani 1 1 d . . . . .
H80A H 0.586573 0.477031 -0.054588 0.033 Uiso 1 1 calc R U . . .
C81 C 0.62079(6) 0.39023(10) -0.00093(7) 0.0227(3) Uani 1 1 d . . . . .
C82 C 0.60927(7) 0.32002(11) -0.03188(7) 0.0259(4) Uani 1 1 d . . . . .
H82A H 0.589254 0.321416 -0.068833 0.031 Uiso 1 1 calc R U . . .
C83 C 0.62721(7) 0.25074(11) -0.00804(7) 0.0280(4) Uani 1 1 d . . . . .
H83A H 0.619412 0.204352 -0.029343 0.034 Uiso 1 1 calc R U . . .
C84 C 0.65707(7) 0.24438(10) 0.04718(7) 0.0243(3) Uani 1 1 d . . . . .
H84A H 0.669132 0.194899 0.062103 0.029 Uiso 1 1 calc R U . . .
C85 C 0.75409(6) 0.21536(9) 0.15445(6) 0.0193(3) Uani 1 1 d . . . . .
C86 C 0.74334(7) 0.13714(10) 0.16628(7) 0.0236(3) Uani 1 1 d . . . . .
C87 C 0.77141(8) 0.07878(10) 0.14403(8) 0.0297(4) Uani 1 1 d . . . . .
H87A H 0.764823 0.025783 0.152167 0.036 Uiso 1 1 calc R U . . .
C88 C 0.80839(8) 0.09544(10) 0.11063(8) 0.0299(4) Uani 1 1 d . . . . .
H88A H 0.825926 0.054560 0.094508 0.036 Uiso 1 1 calc R U . . .
C89 C 0.81959(7) 0.17210(10) 0.10095(7) 0.0249(3) Uani 1 1 d . . . . .
H89A H 0.845536 0.183713 0.078300 0.030 Uiso 1 1 calc R U . . .
C90 C 0.79414(6) 0.23322(9) 0.12324(7) 0.0205(3) Uani 1 1 d . . . . .
C91 C 0.70135(8) 0.11206(10) 0.20045(8) 0.0305(4) Uani 1 1 d . . . . .
H91A H 0.692208 0.158384 0.221916 0.037 Uiso 1 1 calc R U . . .
C92 C 0.65003(9) 0.08524(15) 0.16199(10) 0.0463(5) Uani 1 1 d . . . . .
H92A H 0.635150 0.128498 0.137680 0.069 Uiso 1 1 calc R U . . .
H92B H 0.623455 0.068525 0.184381 0.069 Uiso 1 1 calc R U . . .
H92C H 0.658478 0.041441 0.139180 0.069 Uiso 1 1 calc R U . . .
C93 C 0.72157(9) 0.04710(12) 0.24191(9) 0.0401(5) Uani 1 1 d . . . . .
H93A H 0.756003 0.062722 0.264838 0.060 Uiso 1 1 calc R U . . .
H93B H 0.726705 -0.000834 0.221560 0.060 Uiso 1 1 calc R U . . .
H93C H 0.694958 0.037740 0.265940 0.060 Uiso 1 1 calc R U . . .
C94 C 0.81244(7) 0.31530(10) 0.11260(7) 0.0237(3) Uani 1 1 d . . . . .
H94A H 0.793867 0.352554 0.134450 0.028 Uiso 1 1 calc R U . . .
C95 C 0.79664(8) 0.33587(11) 0.05101(8) 0.0312(4) Uani 1 1 d . . . . .
H95A H 0.757214 0.334980 0.040159 0.047 Uiso 1 1 calc R U . . .
H95B H 0.812456 0.297689 0.028714 0.047 Uiso 1 1 calc R U . . .
H95C H 0.810089 0.388150 0.044562 0.047 Uiso 1 1 calc R U . . .
C96 C 0.87327(8) 0.32426(12) 0.13162(9) 0.0343(4) Uani 1 1 d . . . . .
H96A H 0.883615 0.378671 0.126878 0.051 Uiso 1 1 calc R U . . .
H96B H 0.892195 0.290212 0.109202 0.051 Uiso 1 1 calc R U . . .
H96C H 0.883086 0.309641 0.170995 0.051 Uiso 1 1 calc R U . . .
O1S O 0.83400(16) 0.2802(2) 0.29108(18) 0.0326(9) Uani 0.562(6) 1 d D U P A 1
C1S C 0.82252(17) 0.1995(2) 0.29626(19) 0.0348(10) Uani 0.562(6) 1 d D U P A 1
H1SA H 0.786461 0.186479 0.274529 0.042 Uiso 0.562(6) 1 calc R U P A 1
H1SB H 0.823260 0.185553 0.335784 0.042 Uiso 0.562(6) 1 calc R U P A 1
C2S C 0.86567(15) 0.1568(3) 0.27389(19) 0.0453(12) Uani 0.562(6) 1 d D U P A 1
H2SA H 0.856066 0.150266 0.232963 0.054 Uiso 0.562(6) 1 calc R U P A 1
H2SB H 0.872542 0.104794 0.291518 0.054 Uiso 0.562(6) 1 calc R U P A 1
C3S C 0.91373(17) 0.2099(3) 0.2896(3) 0.0632(15) Uani 0.562(6) 1 d D U P A 1
H3SA H 0.940021 0.187353 0.320709 0.076 Uiso 0.562(6) 1 calc R U P A 1
H3SB H 0.932000 0.218458 0.257456 0.076 Uiso 0.562(6) 1 calc R U P A 1
C4S C 0.8911(2) 0.2848(3) 0.3070(4) 0.0546(18) Uani 0.562(6) 1 d D U P A 1
H4SA H 0.901264 0.291835 0.347847 0.066 Uiso 0.562(6) 1 calc R U P A 1
H4SB H 0.905194 0.329591 0.288388 0.066 Uiso 0.562(6) 1 calc R U P A 1
O1* O 0.8466(2) 0.2837(3) 0.2750(2) 0.0316(11) Uani 0.438(6) 1 d D U P A 2
C1* C 0.8421(3) 0.2009(3) 0.2779(3) 0.0434(14) Uani 0.438(6) 1 d D U P A 2
H1*A H 0.832845 0.178441 0.239950 0.052 Uiso 0.438(6) 1 calc R U P A 2
H1*B H 0.813605 0.186273 0.299071 0.052 Uiso 0.438(6) 1 calc R U P A 2
C2* C 0.8953(3) 0.1718(4) 0.3064(4) 0.096(3) Uani 0.438(6) 1 d D U P A 2
H2*A H 0.890562 0.130703 0.333688 0.115 Uiso 0.438(6) 1 calc R U P A 2
H2*B H 0.915572 0.149253 0.278995 0.115 Uiso 0.438(6) 1 calc R U P A 2
C3* C 0.9250(2) 0.2385(3) 0.3351(3) 0.0562(17) Uani 0.438(6) 1 d D U P A 2
H3*A H 0.963984 0.235521 0.333642 0.067 Uiso 0.438(6) 1 calc R U P A 2
H3*B H 0.920450 0.241439 0.374552 0.067 Uiso 0.438(6) 1 calc R U P A 2
C4* C 0.8989(2) 0.3066(4) 0.3024(4) 0.0441(18) Uani 0.438(6) 1 d D U P A 2
H4*A H 0.896234 0.351170 0.327547 0.053 Uiso 0.438(6) 1 calc R U P A 2
H4*B H 0.920867 0.323008 0.274571 0.053 Uiso 0.438(6) 1 calc R U P A 2
O2S O 0.81283(7) 0.57915(9) 0.14271(6) 0.0451(4) Uani 1 1 d . . . . .
C5S C 0.79930(11) 0.55275(15) 0.08726(10) 0.0518(6) Uani 1 1 d . . . . .
H5SA H 0.771680 0.587243 0.065517 0.062 Uiso 1 1 calc R U . . .
H5SB H 0.784645 0.499019 0.086212 0.062 Uiso 1 1 calc R U . . .
C6S C 0.85022(13) 0.55435(14) 0.06334(12) 0.0650(8) Uani 1 1 d . . . . .
H6SA H 0.843587 0.578491 0.025849 0.078 Uiso 1 1 calc R U . . .
H6SB H 0.864297 0.500820 0.060391 0.078 Uiso 1 1 calc R U . . .
C7S C 0.88986(11) 0.60300(17) 0.10390(11) 0.0562(7) Uani 1 1 d . . . . .
H7SA H 0.920278 0.570635 0.122915 0.067 Uiso 1 1 calc R U . . .
H7SB H 0.904381 0.646699 0.084505 0.067 Uiso 1 1 calc R U . . .
C8S C 0.85642(10) 0.63278(14) 0.14460(10) 0.0461(5) Uani 1 1 d . . . . .
H8SA H 0.878280 0.635076 0.182629 0.055 Uiso 1 1 calc R U . . .
H8SB H 0.842576 0.685778 0.133909 0.055 Uiso 1 1 calc R U . . .
O3S O 0.73194(5) 0.47859(8) 0.43613(5) 0.0318(3) Uani 1 1 d . . . . .
C9S C 0.74220(8) 0.53332(12) 0.48154(8) 0.0352(4) Uani 1 1 d . . . . .
H9SA H 0.743671 0.587194 0.467162 0.042 Uiso 1 1 calc R U . . .
H9SB H 0.777106 0.521495 0.506034 0.042 Uiso 1 1 calc R U . . .
C10S C 0.69607(8) 0.52536(12) 0.51372(8) 0.0351(4) Uani 1 1 d . . . . .
H10B H 0.709443 0.506289 0.552049 0.042 Uiso 1 1 calc R U . . .
H10C H 0.677632 0.576058 0.515764 0.042 Uiso 1 1 calc R U . . .
C11S C 0.65837(8) 0.46649(12) 0.48069(8) 0.0344(4) Uani 1 1 d . . . . .
H11B H 0.642041 0.431902 0.505611 0.041 Uiso 1 1 calc R U . . .
H11C H 0.629241 0.492743 0.454425 0.041 Uiso 1 1 calc R U . . .
C12S C 0.69543(8) 0.42140(12) 0.44990(9) 0.0352(4) Uani 1 1 d . . . . .
H12B H 0.715011 0.380175 0.473916 0.042 Uiso 1 1 calc R U . . .
H12C H 0.674790 0.396909 0.415830 0.042 Uiso 1 1 calc R U . . .
O4S O 0.58926(6) 0.56971(8) 0.19885(6) 0.0391(3) Uani 1 1 d . . . . .
C13S C 0.57945(9) 0.64950(11) 0.21178(9) 0.0376(4) Uani 1 1 d . . . . .
H13A H 0.613721 0.679251 0.218707 0.045 Uiso 1 1 calc R U . . .
H13B H 0.562778 0.652508 0.245490 0.045 Uiso 1 1 calc R U . . .
C14S C 0.54126(8) 0.68271(12) 0.16151(10) 0.0380(5) Uani 1 1 d . . . . .
H14A H 0.505478 0.694391 0.170956 0.046 Uiso 1 1 calc R U . . .
H14B H 0.556202 0.731137 0.148129 0.046 Uiso 1 1 calc R U . . .
C15S C 0.53689(9) 0.61908(13) 0.11797(10) 0.0443(5) Uani 1 1 d . . . . .
H15B H 0.500144 0.616971 0.095181 0.053 Uiso 1 1 calc R U . . .
H15C H 0.563490 0.626810 0.093135 0.053 Uiso 1 1 calc R U . . .
C16S C 0.54925(8) 0.54619(12) 0.15290(9) 0.0357(4) Uani 1 1 d . . . . .
H16B H 0.516518 0.526992 0.165786 0.043 Uiso 1 1 calc R U . . .
H16C H 0.563174 0.504329 0.131348 0.043 Uiso 1 1 calc R U . . .
C17S C 0.95405(8) 1.11406(14) 0.46259(13) 0.1036(13) Uani 1 1 d DG U . . .
C18S C 0.89805(8) 1.11544(11) 0.45593(11) 0.0706(8) Uani 1 1 d DG U . . .
H18A H 0.880477 1.157974 0.470162 0.085 Uiso 1 1 calc R U . . .
C19S C 0.86775(7) 1.05458(13) 0.42845(11) 0.0848(10) Uani 1 1 d G U . . .
H19B H 0.829474 1.055526 0.423894 0.102 Uiso 1 1 calc R U . . .
C20S C 0.89345(10) 0.99234(12) 0.40762(11) 0.0811(9) Uani 1 1 d G U . . .
H20D H 0.872748 0.950751 0.388836 0.097 Uiso 1 1 calc R U . . .
C21S C 0.94946(10) 0.99096(14) 0.41428(13) 0.1189(15) Uani 1 1 d G U . . .
H21D H 0.967025 0.948422 0.400046 0.143 Uiso 1 1 calc R U . . .
C22S C 0.97975(7) 1.05182(17) 0.44176(15) 0.1373(18) Uani 1 1 d DG U . . .
H22B H 1.018029 1.050870 0.446314 0.165 Uiso 1 1 calc R U . . .
C23S C 0.9843(2) 1.1852(3) 0.4896(2) 0.1310(16) Uani 1 1 d D U . . .
H23D H 0.959365 1.218843 0.505311 0.197 Uiso 1 1 calc R U . . .
H23E H 0.999532 1.214366 0.461527 0.197 Uiso 1 1 calc R U . . .
H23F H 1.013558 1.168232 0.519394 0.197 Uiso 1 1 calc R U . . .
C24S C 0.5057(3) -0.0710(4) -0.0037(3) 0.056(3) Uani 0.288(2) 1 d DG U P B -1
C25S C 0.5323(3) -0.0155(4) 0.0329(3) 0.058(2) Uani 0.288(2) 1 d DG U P B -1
H25A H 0.560187 -0.031177 0.062537 0.070 Uiso 0.288(2) 1 calc R U P B -1
C26S C 0.5182(3) 0.0628(4) 0.0262(3) 0.054(3) Uani 0.288(2) 1 d G U P B -1
H26A H 0.536407 0.100707 0.051197 0.065 Uiso 0.288(2) 1 calc R U P B -1
C27S C 0.4774(3) 0.0857(4) -0.0172(3) 0.052(2) Uani 0.288(2) 1 d G U P B -1
H27A H 0.467773 0.139246 -0.021771 0.063 Uiso 0.288(2) 1 calc R U P B -1
C28S C 0.4508(3) 0.0303(5) -0.0538(3) 0.054(2) Uani 0.288(2) 1 d G U P B -1
H28A H 0.422920 0.045901 -0.083401 0.064 Uiso 0.288(2) 1 calc R U P B -1
C29S C 0.4649(3) -0.0481(4) -0.0470(3) 0.064(3) Uani 0.288(2) 1 d DG U P B -1
H29A H 0.446699 -0.085984 -0.072062 0.076 Uiso 0.288(2) 1 calc R U P B -1
C30S C 0.5215(7) -0.1562(6) 0.0120(7) 0.124(5) Uani 0.288(2) 1 d D U P B -1
H30B H 0.551558 -0.156822 0.043686 0.186 Uiso 0.288(2) 1 calc R U P B -1
H30C H 0.532469 -0.182370 -0.019937 0.186 Uiso 0.288(2) 1 calc R U P B -1
H30D H 0.490458 -0.183592 0.022048 0.186 Uiso 0.288(2) 1 calc R U P B -1
C24* C 0.4984(4) 0.0024(5) 0.0036(4) 0.049(2) Uani 0.212(2) 1 d DG U P C -2
C25* C 0.4886(4) -0.0711(5) -0.0203(4) 0.044(4) Uani 0.212(2) 1 d DG U P C -2
H25B H 0.460799 -0.077914 -0.051831 0.053 Uiso 0.212(2) 1 calc R U P C -2
C26* C 0.5196(4) -0.1346(4) 0.0021(4) 0.062(3) Uani 0.212(2) 1 d G U P C -2
H26B H 0.512860 -0.184810 -0.014202 0.074 Uiso 0.212(2) 1 calc R U P C -2
C27* C 0.5603(3) -0.1246(4) 0.0483(4) 0.051(2) Uani 0.212(2) 1 d G U P C -2
H27B H 0.581411 -0.167951 0.063576 0.061 Uiso 0.212(2) 1 calc R U P C -2
C28* C 0.5701(3) -0.0510(5) 0.0721(3) 0.047(2) Uani 0.212(2) 1 d G U P C -2
H28B H 0.597901 -0.044196 0.103726 0.057 Uiso 0.212(2) 1 calc R U P C -2
C29* C 0.5391(4) 0.0125(4) 0.0498(4) 0.050(3) Uani 0.212(2) 1 d DG U P C -2
H29B H 0.545842 0.062702 0.066097 0.060 Uiso 0.212(2) 1 calc R U P C -2
C30* C 0.4622(7) 0.0700(7) -0.0217(7) 0.074(4) Uani 0.212(2) 1 d D U P C -2
H30E H 0.437368 0.051531 -0.054839 0.111 Uiso 0.212(2) 1 calc R U P C -2
H30F H 0.484587 0.112229 -0.032188 0.111 Uiso 0.212(2) 1 calc R U P C -2
H30G H 0.441363 0.089316 0.005769 0.111 Uiso 0.212(2) 1 calc R U P C -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Na1 O1 2.2729(12) . ?
Na1 O1S 2.297(4) . ?
Na1 O4 2.3492(13) . ?
Na1 O3 2.3770(13) . ?
Na1 O1* 2.383(5) . ?
Na1 N4 2.6205(15) . ?
Na1 C49 2.9895(17) . ?
Na1 C73 3.0713(17) . ?
Na1 Na3 3.2343(9) . ?
Na1 Na2 3.2654(9) . ?
Na1 Na4 3.4851(9) . ?
Na2 O4 2.2783(13) . ?
Na2 O2S 2.3041(15) . ?
Na2 O2 2.3222(13) . ?
Na2 O1 2.3533(13) . ?
Na2 N2 2.6742(16) . ?
Na2 C1 2.9858(18) . ?
Na2 C25 3.0803(17) . ?
Na2 Na4 3.1893(9) . ?
Na2 Na3 3.4976(9) . ?
Na3 O3 2.2684(12) . ?
Na3 O3S 2.3256(14) . ?
Na3 O2 2.3535(13) . ?
Na3 O1 2.3566(13) . ?
Na3 N1 2.6058(15) . ?
Na3 C25 3.0428(17) . ?
Na3 C1 3.0749(17) . ?
Na3 Na4 3.2890(9) . ?
Na4 O2 2.2729(13) . ?
Na4 O4S 2.3233(14) . ?
Na4 O3 2.3390(13) . ?
Na4 O4 2.3599(13) . ?
Na4 N3 2.5659(15) . ?
Na4 C49 3.0479(17) . ?
Na4 C73 3.0990(17) . ?
O1 C1 1.2953(19) . ?
O2 C25 1.2895(19) . ?
O3 C49 1.2938(19) . ?
O4 C73 1.2979(19) . ?
N1 C13 1.431(2) . ?
N1 C2 1.435(2) . ?
N1 H1A 0.79(2) . ?
N2 C37 1.429(2) . ?
N2 C26 1.434(2) . ?
N2 H2A 0.81(2) . ?
N3 C61 1.427(2) . ?
N3 C50 1.438(2) . ?
N3 H3A 0.822(19) . ?
N4 C85 1.4291(19) . ?
N4 C74 1.436(2) . ?
N4 H4A 0.784(19) . ?
C1 C2 1.383(2) . ?
C1 C5 1.490(2) . ?
C2 C3 1.462(2) . ?
C3 C12 1.369(2) . ?
C3 C4 1.420(2) . ?
C4 C9 1.387(2) . ?
C4 C5 1.402(2) . ?
C5 C6 1.362(3) . ?
C6 C7 1.417(3) . ?
C6 H6A 0.9500 . ?
C7 C8 1.369(3) . ?
C7 H7A 0.9500 . ?
C8 C9 1.418(3) . ?
C8 H8A 0.9500 . ?
C9 C10 1.420(3) . ?
C10 C11 1.364(3) . ?
C10 H10A 0.9500 . ?
C11 C12 1.424(3) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9500 . ?
C13 C14 1.401(3) . ?
C13 C18 1.407(2) . ?
C14 C15 1.391(3) . ?
C14 C19 1.518(3) . ?
C15 C16 1.373(3) . ?
C15 H15A 0.9500 . ?
C16 C17 1.376(3) . ?
C16 H16A 0.9500 . ?
C17 C18 1.393(3) . ?
C17 H17A 0.9500 . ?
C18 C22 1.525(3) . ?
C19 C21 1.525(3) . ?
C19 C20 1.530(2) . ?
C19 H19A 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C24 1.507(3) . ?
C22 C23 1.517(3) . ?
C22 H22A 1.0000 . ?
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 C26 1.387(2) . ?
C25 C29 1.489(2) . ?
C26 C27 1.455(2) . ?
C27 C36 1.377(2) . ?
C27 C28 1.420(2) . ?
C28 C33 1.385(2) . ?
C28 C29 1.401(2) . ?
C29 C30 1.363(2) . ?
C30 C31 1.414(2) . ?
C30 H30A 0.9500 . ?
C31 C32 1.372(3) . ?
C31 H31A 0.9500 . ?
C32 C33 1.416(3) . ?
C32 H32A 0.9500 . ?
C33 C34 1.423(3) . ?
C34 C35 1.365(3) . ?
C34 H34A 0.9500 . ?
C35 C36 1.422(3) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?
C37 C42 1.395(3) . ?
C37 C38 1.407(3) . ?
C38 C39 1.392(3) . ?
C38 C43 1.518(3) . ?
C39 C40 1.367(3) . ?
C39 H39A 0.9500 . ?
C40 C41 1.373(3) . ?
C40 H40A 0.9500 . ?
C41 C42 1.394(2) . ?
C41 H41A 0.9500 . ?
C42 C46 1.517(3) . ?
C43 C45 1.518(4) . ?
C43 C44 1.520(3) . ?
C43 H43A 1.0000 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C47 1.520(3) . ?
C46 C48 1.524(3) . ?
C46 H46A 1.0000 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C50 1.382(2) . ?
C49 C53 1.489(2) . ?
C50 C51 1.462(2) . ?
C51 C60 1.373(2) . ?
C51 C52 1.416(2) . ?
C52 C57 1.389(2) . ?
C52 C53 1.402(2) . ?
C53 C54 1.365(2) . ?
C54 C55 1.413(2) . ?
C54 H54A 0.9500 . ?
C55 C56 1.372(3) . ?
C55 H55A 0.9500 . ?
C56 C57 1.413(3) . ?
C56 H56A 0.9500 . ?
C57 C58 1.423(2) . ?
C58 C59 1.360(3) . ?
C58 H58A 0.9500 . ?
C59 C60 1.422(2) . ?
C59 H59A 0.9500 . ?
C60 H60A 0.9500 . ?
C61 C62 1.400(2) . ?
C61 C66 1.409(2) . ?
C62 C63 1.396(2) . ?
C62 C67 1.518(2) . ?
C63 C64 1.376(3) . ?
C63 H63A 0.9500 . ?
C64 C65 1.373(3) . ?
C64 H64A 0.9500 . ?
C65 C66 1.386(2) . ?
C65 H65A 0.9500 . ?
C66 C70 1.518(2) . ?
C67 C69 1.524(2) . ?
C67 C68 1.530(2) . ?
C67 H67A 1.0000 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C70 C72 1.510(3) . ?
C70 C71 1.517(3) . ?
C70 H70A 1.0000 . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 C74 1.382(2) . ?
C73 C77 1.489(2) . ?
C74 C75 1.459(2) . ?
C75 C84 1.372(2) . ?
C75 C76 1.415(2) . ?
C76 C81 1.386(2) . ?
C76 C77 1.404(2) . ?
C77 C78 1.366(2) . ?
C78 C79 1.415(3) . ?
C78 H78A 0.9500 . ?
C79 C80 1.372(3) . ?
C79 H79A 0.9500 . ?
C80 C81 1.418(2) . ?
C80 H80A 0.9500 . ?
C81 C82 1.421(2) . ?
C82 C83 1.362(3) . ?
C82 H82A 0.9500 . ?
C83 C84 1.423(2) . ?
C83 H83A 0.9500 . ?
C84 H84A 0.9500 . ?
C85 C90 1.403(2) . ?
C85 C86 1.407(2) . ?
C86 C87 1.390(2) . ?
C86 C91 1.522(2) . ?
C87 C88 1.374(3) . ?
C87 H87A 0.9500 . ?
C88 C89 1.372(3) . ?
C88 H88A 0.9500 . ?
C89 C90 1.388(2) . ?
C89 H89A 0.9500 . ?
C90 C94 1.516(2) . ?
C91 C92 1.524(3) . ?
C91 C93 1.527(3) . ?
C91 H91A 1.0000 . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 0.9800 . ?
C93 H93A 0.9800 . ?
C93 H93B 0.9800 . ?
C93 H93C 0.9800 . ?
C94 C95 1.524(2) . ?
C94 C96 1.526(2) . ?
C94 H94A 1.0000 . ?
C95 H95A 0.9800 . ?
C95 H95B 0.9800 . ?
C95 H95C 0.9800 . ?
C96 H96A 0.9800 . ?
C96 H96B 0.9800 . ?
C96 H96C 0.9800 . ?
O1S C4S 1.421(4) . ?
O1S C1S 1.423(4) . ?
C1S C2S 1.492(4) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
C2S C3S 1.507(5) . ?
C2S H2SA 0.9900 . ?
C2S H2SB 0.9900 . ?
C3S C4S 1.496(5) . ?
C3S H3SA 0.9900 . ?
C3S H3SB 0.9900 . ?
C4S H4SA 0.9900 . ?
C4S H4SB 0.9900 . ?
O1* C4* 1.420(5) . ?
O1* C1* 1.425(5) . ?
C1* C2* 1.481(5) . ?
C1* H1*A 0.9900 . ?
C1* H1*B 0.9900 . ?
C2* C3* 1.471(5) . ?
C2* H2*A 0.9900 . ?
C2* H2*B 0.9900 . ?
C3* C4* 1.496(5) . ?
C3* H3*A 0.9900 . ?
C3* H3*B 0.9900 . ?
C4* H4*A 0.9900 . ?
C4* H4*B 0.9900 . ?
O2S C5S 1.408(3) . ?
O2S C8S 1.425(3) . ?
C5S C6S 1.502(3) . ?
C5S H5SA 0.9900 . ?
C5S H5SB 0.9900 . ?
C6S C7S 1.520(4) . ?
C6S H6SA 0.9900 . ?
C6S H6SB 0.9900 . ?
C7S C8S 1.503(3) . ?
C7S H7SA 0.9900 . ?
C7S H7SB 0.9900 . ?
C8S H8SA 0.9900 . ?
C8S H8SB 0.9900 . ?
O3S C12S 1.424(2) . ?
O3S C9S 1.438(2) . ?
C9S C10S 1.521(3) . ?
C9S H9SA 0.9900 . ?
C9S H9SB 0.9900 . ?
C10S C11S 1.513(3) . ?
C10S H10B 0.9900 . ?
C10S H10C 0.9900 . ?
C11S C12S 1.512(3) . ?
C11S H11B 0.9900 . ?
C11S H11C 0.9900 . ?
C12S H12B 0.9900 . ?
C12S H12C 0.9900 . ?
O4S C16S 1.423(2) . ?
O4S C13S 1.434(2) . ?
C13S C14S 1.525(3) . ?
C13S H13A 0.9900 . ?
C13S H13B 0.9900 . ?
C14S C15S 1.512(3) . ?
C14S H14A 0.9900 . ?
C14S H14B 0.9900 . ?
C15S C16S 1.512(3) . ?
C15S H15B 0.9900 . ?
C15S H15C 0.9900 . ?
C16S H16B 0.9900 . ?
C16S H16C 0.9900 . ?
C17S C18S 1.3900 . ?
C17S C22S 1.3900 . ?
C17S C23S 1.523(5) . ?
C18S C19S 1.3900 . ?
C18S H18A 0.9500 . ?
C19S C20S 1.3900 . ?
C19S H19B 0.9500 . ?
C20S C21S 1.3900 . ?
C20S H20D 0.9500 . ?
C21S C22S 1.3900 . ?
C21S H21D 0.9500 . ?
C22S H22B 0.9500 . ?
C23S H23D 0.9800 . ?
C23S H23E 0.9800 . ?
C23S H23F 0.9800 . ?
C24S C25S 1.3900 . ?
C24S C29S 1.3900 . ?
C24S C30S 1.542(7) . ?
C25S C26S 1.3900 . ?
C25S H25A 0.9500 . ?
C26S C27S 1.3900 . ?
C26S H26A 0.9500 . ?
C27S C28S 1.3900 . ?
C27S H27A 0.9500 . ?
C28S C29S 1.3900 . ?
C28S H28A 0.9500 . ?
C29S H29A 0.9500 . ?
C30S H30B 0.9800 . ?
C30S H30C 0.9800 . ?
C30S H30D 0.9800 . ?
C24* C25* 1.3900 . ?
C24* C29* 1.3900 . ?
C24* C30* 1.532(7) . ?
C25* C26* 1.3900 . ?
C25* H25B 0.9500 . ?
C26* C27* 1.3900 . ?
C26* H26B 0.9500 . ?
C27* C28* 1.3900 . ?
C27* H27B 0.9500 . ?
C28* C29* 1.3900 . ?
C28* H28B 0.9500 . ?
C29* H29B 0.9500 . ?
C30* H30E 0.9800 . ?
C30* H30F 0.9800 . ?
C30* H30G 0.9800 . ?

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
O1 Na1 O1S 98.85(10) . . ?
O1 Na1 O4 90.22(5) . . ?
O1S Na1 O4 161.46(12) . . ?
O1 Na1 O3 90.64(4) . . ?
O1S Na1 O3 112.05(11) . . ?
O4 Na1 O3 83.79(4) . . ?
O1 Na1 O1* 96.94(12) . . ?
O4 Na1 O1* 149.66(14) . . ?
O3 Na1 O1* 125.37(14) . . ?
O1 Na1 N4 158.85(5) . . ?
O1S Na1 N4 92.80(10) . . ?
O4 Na1 N4 74.01(4) . . ?
O3 Na1 N4 101.31(5) . . ?
O1* Na1 N4 90.33(12) . . ?
O1 Na1 C49 114.36(5) . . ?
O1S Na1 C49 100.11(11) . . ?
O4 Na1 C49 90.67(5) . . ?
O3 Na1 C49 24.68(4) . . ?
O1* Na1 C49 112.63(13) . . ?
N4 Na1 C49 80.51(5) . . ?
O1 Na1 C73 111.95(5) . . ?
O1S Na1 C73 140.96(11) . . ?
O4 Na1 C73 23.16(4) . . ?
O3 Na1 C73 91.63(4) . . ?
O1* Na1 C73 133.04(13) . . ?
N4 Na1 C73 50.98(4) . . ?
C49 Na1 C73 88.79(5) . . ?
O1 Na1 Na3 46.75(3) . . ?
O1S Na1 Na3 106.35(11) . . ?
O4 Na1 Na3 91.66(3) . . ?
O3 Na1 Na3 44.51(3) . . ?
O1* Na1 Na3 114.62(13) . . ?
N4 Na1 Na3 144.97(4) . . ?
C49 Na1 Na3 67.61(3) . . ?
C73 Na1 Na3 112.14(4) . . ?
O1 Na1 Na2 46.11(3) . . ?
O1S Na1 Na2 140.85(10) . . ?
O4 Na1 Na2 44.24(3) . . ?
O3 Na1 Na2 88.74(3) . . ?
O1* Na1 Na2 132.92(12) . . ?
N4 Na1 Na2 116.08(4) . . ?
C49 Na1 Na2 109.85(4) . . ?
C73 Na1 Na2 65.96(3) . . ?
Na3 Na1 Na2 65.11(2) . . ?
O1 Na1 Na4 85.35(4) . . ?
O1S Na1 Na4 153.93(11) . . ?
O4 Na1 Na4 42.38(3) . . ?
O3 Na1 Na4 41.93(3) . . ?
O1* Na1 Na4 167.27(13) . . ?
N4 Na1 Na4 91.92(4) . . ?
C49 Na1 Na4 55.53(3) . . ?
C73 Na1 Na4 55.99(3) . . ?
Na3 Na1 Na4 58.471(19) . . ?
Na2 Na1 Na4 56.275(18) . . ?
O4 Na2 O2S 98.63(5) . . ?
O4 Na2 O2 92.43(5) . . ?
O2S Na2 O2 159.53(6) . . ?
O4 Na2 O1 89.99(4) . . ?
O2S Na2 O1 113.53(6) . . ?
O2 Na2 O1 83.47(4) . . ?
O4 Na2 N2 159.87(5) . . ?
O2S Na2 N2 92.05(5) . . ?
O2 Na2 N2 72.69(4) . . ?
O1 Na2 N2 101.37(5) . . ?
O4 Na2 C1 113.20(5) . . ?
O2S Na2 C1 100.47(6) . . ?
O2 Na2 C1 90.79(5) . . ?
O1 Na2 C1 24.62(4) . . ?
N2 Na2 C1 81.22(5) . . ?
O4 Na2 C25 113.86(5) . . ?
O2S Na2 C25 139.74(5) . . ?
O2 Na2 C25 22.49(4) . . ?
O1 Na2 C25 90.49(4) . . ?
N2 Na2 C25 50.24(4) . . ?
C1 Na2 C25 88.38(5) . . ?
O4 Na2 Na4 47.63(3) . . ?
O2S Na2 Na4 139.51(5) . . ?
O2 Na2 Na4 45.41(3) . . ?
O1 Na2 Na4 91.22(3) . . ?
N2 Na2 Na4 114.84(4) . . ?
C1 Na2 Na4 112.62(4) . . ?
C25 Na2 Na4 66.24(3) . . ?
O4 Na2 Na1 46.01(3) . . ?
O2S Na2 Na1 110.32(5) . . ?
O2 Na2 Na1 89.75(3) . . ?
O1 Na2 Na1 44.11(3) . . ?
N2 Na2 Na1 143.81(4) . . ?
C1 Na2 Na1 67.32(3) . . ?
C25 Na2 Na1 109.33(4) . . ?
Na4 Na2 Na1 65.34(2) . . ?
O4 Na2 Na3 86.39(4) . . ?
O2S Na2 Na3 155.40(5) . . ?
O2 Na2 Na3 41.92(3) . . ?
O1 Na2 Na3 42.08(3) . . ?
N2 Na2 Na3 90.98(4) . . ?
C1 Na2 Na3 55.95(3) . . ?
C25 Na2 Na3 54.66(3) . . ?
Na4 Na2 Na3 58.709(19) . . ?
Na1 Na2 Na3 57.016(18) . . ?
O3 Na3 O3S 97.92(5) . . ?
O3 Na3 O2 88.86(4) . . ?
O3S Na3 O2 121.71(5) . . ?
O3 Na3 O1 91.27(5) . . ?
O3S Na3 O1 153.84(5) . . ?
O2 Na3 O1 82.72(4) . . ?
O3 Na3 N1 163.79(5) . . ?
O3S Na3 N1 92.91(5) . . ?
O2 Na3 N1 95.69(5) . . ?
O1 Na3 N1 73.96(4) . . ?
O3 Na3 C25 110.56(5) . . ?
O3S Na3 C25 107.98(5) . . ?
O2 Na3 C25 23.50(4) . . ?
O1 Na3 C25 91.35(5) . . ?
N1 Na3 C25 77.11(5) . . ?
O3 Na3 C1 113.92(5) . . ?
O3S Na3 C1 137.25(5) . . ?
O2 Na3 C1 88.04(4) . . ?
O1 Na3 C1 23.10(4) . . ?
N1 Na3 C1 50.94(4) . . ?
C25 Na3 C1 87.46(5) . . ?
O3 Na3 Na1 47.27(3) . . ?
O3S Na3 Na1 134.80(4) . . ?
O2 Na3 Na1 89.96(3) . . ?
O1 Na3 Na1 44.63(3) . . ?
N1 Na3 Na1 117.01(4) . . ?
C25 Na3 Na1 111.12(4) . . ?
C1 Na3 Na1 66.74(4) . . ?
O3 Na3 Na4 45.32(3) . . ?
O3S Na3 Na4 115.04(4) . . ?
O2 Na3 Na4 43.71(3) . . ?
O1 Na3 Na4 88.73(3) . . ?
N1 Na3 Na4 138.26(4) . . ?
C25 Na3 Na4 65.40(4) . . ?
C1 Na3 Na4 107.67(4) . . ?
Na1 Na3 Na4 64.58(2) . . ?
O3 Na3 Na2 84.91(4) . . ?
O3S Na3 Na2 162.87(5) . . ?
O2 Na3 Na2 41.24(3) . . ?
O1 Na3 Na2 42.01(3) . . ?
N1 Na3 Na2 88.29(4) . . ?
C25 Na3 Na2 55.67(3) . . ?
C1 Na3 Na2 53.57(3) . . ?
Na1 Na3 Na2 57.874(19) . . ?
Na4 Na3 Na2 55.959(19) . . ?
O2 Na4 O4S 98.66(5) . . ?
O2 Na4 O3 89.12(4) . . ?
O4S Na4 O3 159.51(6) . . ?
O2 Na4 O4 91.59(4) . . ?
O4S Na4 O4 114.11(5) . . ?
O3 Na4 O4 84.39(4) . . ?
O2 Na4 N3 161.90(5) . . ?
O4S Na4 N3 93.96(5) . . ?
O3 Na4 N3 74.84(4) . . ?
O4 Na4 N3 95.04(5) . . ?
O2 Na4 C49 111.93(5) . . ?
O4S Na4 C49 141.22(5) . . ?
O3 Na4 C49 23.39(4) . . ?
O4 Na4 C49 89.05(4) . . ?
N3 Na4 C49 51.52(4) . . ?
O2 Na4 C73 113.28(5) . . ?
O4S Na4 C73 102.43(5) . . ?
O3 Na4 C73 91.67(4) . . ?
O4 Na4 C73 22.75(4) . . ?
N3 Na4 C73 76.18(5) . . ?
C49 Na4 C73 87.23(4) . . ?
O2 Na4 Na2 46.69(3) . . ?
O4S Na4 Na2 107.90(5) . . ?
O3 Na4 Na2 91.26(4) . . ?
O4 Na4 Na2 45.50(3) . . ?
N3 Na4 Na2 139.85(4) . . ?
C49 Na4 Na2 110.37(4) . . ?
C73 Na4 Na2 66.60(3) . . ?
O2 Na4 Na3 45.69(3) . . ?
O4S Na4 Na3 139.01(4) . . ?
O3 Na4 Na3 43.59(3) . . ?
O4 Na4 Na3 90.12(3) . . ?
N3 Na4 Na3 117.35(4) . . ?
C49 Na4 Na3 66.25(3) . . ?
C73 Na4 Na3 109.96(4) . . ?
Na2 Na4 Na3 65.33(2) . . ?
O2 Na4 Na1 85.21(4) . . ?
O4S Na4 Na1 156.24(5) . . ?
O3 Na4 Na1 42.78(3) . . ?
O4 Na4 Na1 42.15(3) . . ?
N3 Na4 Na1 88.46(4) . . ?
C49 Na4 Na1 53.96(3) . . ?
C73 Na4 Na1 55.23(3) . . ?
Na2 Na4 Na1 58.380(19) . . ?
Na3 Na4 Na1 56.950(19) . . ?
C1 O1 Na1 152.37(11) . . ?
C1 O1 Na2 106.18(10) . . ?
Na1 O1 Na2 89.78(4) . . ?
C1 O1 Na3 111.36(10) . . ?
Na1 O1 Na3 88.62(4) . . ?
Na2 O1 Na3 95.91(5) . . ?
C25 O2 Na4 146.96(11) . . ?
C25 O2 Na2 113.97(10) . . ?
Na4 O2 Na2 87.90(4) . . ?
C25 O2 Na3 109.81(10) . . ?
Na4 O2 Na3 90.60(4) . . ?
Na2 O2 Na3 96.84(5) . . ?
C49 O3 Na3 152.67(10) . . ?
C49 O3 Na4 110.76(10) . . ?
Na3 O3 Na4 91.09(4) . . ?
C49 O3 Na1 105.21(10) . . ?
Na3 O3 Na1 88.22(4) . . ?
Na4 O3 Na1 95.29(5) . . ?
C73 O4 Na2 148.65(10) . . ?
C73 O4 Na1 111.44(10) . . ?
Na2 O4 Na1 89.75(4) . . ?
C73 O4 Na4 112.56(10) . . ?
Na2 O4 Na4 86.86(4) . . ?
Na1 O4 Na4 95.47(5) . . ?
C13 N1 C2 116.51(14) . . ?
C13 N1 Na3 119.97(10) . . ?
C2 N1 Na3 102.16(10) . . ?
C13 N1 H1A 114.8(13) . . ?
C2 N1 H1A 105.4(14) . . ?
Na3 N1 H1A 94.9(15) . . ?
C37 N2 C26 118.97(14) . . ?
C37 N2 Na2 123.09(11) . . ?
C26 N2 Na2 101.62(10) . . ?
C37 N2 H2A 119.1(13) . . ?
C26 N2 H2A 103.8(14) . . ?
Na2 N2 H2A 83.7(15) . . ?
C61 N3 C50 117.77(13) . . ?
C61 N3 Na4 119.87(10) . . ?
C50 N3 Na4 102.16(9) . . ?
C61 N3 H3A 116.8(12) . . ?
C50 N3 H3A 105.6(12) . . ?
Na4 N3 H3A 90.4(14) . . ?
C85 N4 C74 116.79(13) . . ?
C85 N4 Na1 120.91(10) . . ?
C74 N4 Na1 101.55(9) . . ?
C85 N4 H4A 115.5(13) . . ?
C74 N4 H4A 108.0(14) . . ?
Na1 N4 H4A 90.4(14) . . ?
O1 C1 C2 129.03(15) . . ?
O1 C1 C5 123.82(15) . . ?
C2 C1 C5 107.13(14) . . ?
O1 C1 Na2 49.20(8) . . ?
C2 C1 Na2 119.44(11) . . ?
C5 C1 Na2 107.39(10) . . ?
O1 C1 Na3 45.54(8) . . ?
C2 C1 Na3 83.63(10) . . ?
C5 C1 Na3 167.96(11) . . ?
Na2 C1 Na3 70.48(4) . . ?
C1 C2 N1 123.24(15) . . ?
C1 C2 C3 109.88(15) . . ?
N1 C2 C3 126.57(15) . . ?
C12 C3 C4 117.15(16) . . ?
C12 C3 C2 137.08(17) . . ?
C4 C3 C2 105.75(15) . . ?
C9 C4 C5 124.12(17) . . ?
C9 C4 C3 125.24(17) . . ?
C5 C4 C3 110.61(15) . . ?
C6 C5 C4 119.25(16) . . ?
C6 C5 C1 134.11(16) . . ?
C4 C5 C1 106.58(15) . . ?
C5 C6 C7 118.15(18) . . ?
C5 C6 H6A 120.9 . . ?
C7 C6 H6A 120.9 . . ?
C8 C7 C6 122.22(19) . . ?
C8 C7 H7A 118.9 . . ?
C6 C7 H7A 118.9 . . ?
C7 C8 C9 120.60(17) . . ?
C7 C8 H8A 119.7 . . ?
C9 C8 H8A 119.7 . . ?
C4 C9 C8 115.64(17) . . ?
C4 C9 C10 116.15(18) . . ?
C8 C9 C10 128.21(17) . . ?
C11 C10 C9 119.29(17) . . ?
C11 C10 H10A 120.4 . . ?
C9 C10 H10A 120.4 . . ?
C10 C11 C12 123.53(18) . . ?
C10 C11 H11A 118.2 . . ?
C12 C11 H11A 118.2 . . ?
C3 C12 C11 118.62(18) . . ?
C3 C12 H12A 120.7 . . ?
C11 C12 H12A 120.7 . . ?
C14 C13 C18 120.53(16) . . ?
C14 C13 N1 119.17(15) . . ?
C18 C13 N1 120.27(16) . . ?
C15 C14 C13 118.34(17) . . ?
C15 C14 C19 117.85(17) . . ?
C13 C14 C19 123.79(15) . . ?
C16 C15 C14 121.72(18) . . ?
C16 C15 H15A 119.1 . . ?
C14 C15 H15A 119.1 . . ?
C15 C16 C17 119.38(17) . . ?
C15 C16 H16A 120.3 . . ?
C17 C16 H16A 120.3 . . ?
C16 C17 C18 121.57(18) . . ?
C16 C17 H17A 119.2 . . ?
C18 C17 H17A 119.2 . . ?
C17 C18 C13 118.17(17) . . ?
C17 C18 C22 119.01(17) . . ?
C13 C18 C22 122.82(16) . . ?
C14 C19 C21 110.64(15) . . ?
C14 C19 C20 110.77(15) . . ?
C21 C19 C20 110.90(16) . . ?
C14 C19 H19A 108.1 . . ?
C21 C19 H19A 108.1 . . ?
C20 C19 H19A 108.1 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C24 C22 C23 109.98(18) . . ?
C24 C22 C18 110.65(18) . . ?
C23 C22 C18 112.99(17) . . ?
C24 C22 H22A 107.7 . . ?
C23 C22 H22A 107.7 . . ?
C18 C22 H22A 107.7 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O2 C25 C26 129.09(15) . . ?
O2 C25 C29 124.13(14) . . ?
C26 C25 C29 106.77(14) . . ?
O2 C25 Na3 46.69(8) . . ?
C26 C25 Na3 126.20(11) . . ?
C29 C25 Na3 101.66(10) . . ?
O2 C25 Na2 43.54(7) . . ?
C26 C25 Na2 85.56(10) . . ?
C29 C25 Na2 167.67(11) . . ?
Na3 C25 Na2 69.67(4) . . ?
C25 C26 N2 122.25(15) . . ?
C25 C26 C27 110.00(14) . . ?
N2 C26 C27 127.71(15) . . ?
C36 C27 C28 116.90(16) . . ?
C36 C27 C26 137.21(16) . . ?
C28 C27 C26 105.88(14) . . ?
C33 C28 C29 124.24(16) . . ?
C33 C28 C27 125.27(16) . . ?
C29 C28 C27 110.46(15) . . ?
C30 C29 C28 119.06(15) . . ?
C30 C29 C25 134.18(15) . . ?
C28 C29 C25 106.75(14) . . ?
C29 C30 C31 118.32(16) . . ?
C29 C30 H30A 120.8 . . ?
C31 C30 H30A 120.8 . . ?
C32 C31 C30 122.11(17) . . ?
C32 C31 H31A 118.9 . . ?
C30 C31 H31A 118.9 . . ?
C31 C32 C33 120.51(16) . . ?
C31 C32 H32A 119.7 . . ?
C33 C32 H32A 119.7 . . ?
C28 C33 C32 115.71(16) . . ?
C28 C33 C34 116.22(16) . . ?
C32 C33 C34 128.06(16) . . ?
C35 C34 C33 119.29(16) . . ?
C35 C34 H34A 120.4 . . ?
C33 C34 H34A 120.4 . . ?
C34 C35 C36 123.43(17) . . ?
C34 C35 H35A 118.3 . . ?
C36 C35 H35A 118.3 . . ?
C27 C36 C35 118.77(17) . . ?
C27 C36 H36A 120.6 . . ?
C35 C36 H36A 120.6 . . ?
C42 C37 C38 120.55(16) . . ?
C42 C37 N2 119.39(16) . . ?
C38 C37 N2 119.97(17) . . ?
C39 C38 C37 118.08(19) . . ?
C39 C38 C43 117.86(18) . . ?
C37 C38 C43 124.04(16) . . ?
C40 C39 C38 121.86(19) . . ?
C40 C39 H39A 119.1 . . ?
C38 C39 H39A 119.1 . . ?
C39 C40 C41 119.52(18) . . ?
C39 C40 H40A 120.2 . . ?
C41 C40 H40A 120.2 . . ?
C40 C41 C42 121.4(2) . . ?
C40 C41 H41A 119.3 . . ?
C42 C41 H41A 119.3 . . ?
C41 C42 C37 118.57(18) . . ?
C41 C42 C46 117.79(18) . . ?
C37 C42 C46 123.64(16) . . ?
C45 C43 C38 109.65(18) . . ?
C45 C43 C44 109.3(2) . . ?
C38 C43 C44 113.86(19) . . ?
C45 C43 H43A 108.0 . . ?
C38 C43 H43A 108.0 . . ?
C44 C43 H43A 108.0 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C42 C46 C47 111.42(16) . . ?
C42 C46 C48 110.51(16) . . ?
C47 C46 C48 111.03(17) . . ?
C42 C46 H46A 107.9 . . ?
C47 C46 H46A 107.9 . . ?
C48 C46 H46A 107.9 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
O3 C49 C50 129.02(15) . . ?
O3 C49 C53 123.95(14) . . ?
C50 C49 C53 107.03(13) . . ?
O3 C49 Na1 50.11(8) . . ?
C50 C49 Na1 119.18(11) . . ?
C53 C49 Na1 105.25(10) . . ?
O3 C49 Na4 45.86(7) . . ?
C50 C49 Na4 83.23(9) . . ?
C53 C49 Na4 169.50(11) . . ?
Na1 C49 Na4 70.51(4) . . ?
C49 C50 N3 122.98(14) . . ?
C49 C50 C51 109.86(14) . . ?
N3 C50 C51 127.16(14) . . ?
C60 C51 C52 116.87(15) . . ?
C60 C51 C50 137.23(16) . . ?
C52 C51 C50 105.89(14) . . ?
C57 C52 C53 124.26(15) . . ?
C57 C52 C51 125.22(15) . . ?
C53 C52 C51 110.52(14) . . ?
C54 C53 C52 118.93(15) . . ?
C54 C53 C49 134.39(15) . . ?
C52 C53 C49 106.68(14) . . ?
C53 C54 C55 118.19(16) . . ?
C53 C54 H54A 120.9 . . ?
C55 C54 H54A 120.9 . . ?
C56 C55 C54 122.51(17) . . ?
C56 C55 H55A 118.7 . . ?
C54 C55 H55A 118.7 . . ?
C55 C56 C57 120.29(16) . . ?
C55 C56 H56A 119.9 . . ?
C57 C56 H56A 119.9 . . ?
C52 C57 C56 115.81(15) . . ?
C52 C57 C58 116.18(16) . . ?
C56 C57 C58 128.02(16) . . ?
C59 C58 C57 119.38(16) . . ?
C59 C58 H58A 120.3 . . ?
C57 C58 H58A 120.3 . . ?
C58 C59 C60 123.28(16) . . ?
C58 C59 H59A 118.4 . . ?
C60 C59 H59A 118.4 . . ?
C51 C60 C59 119.06(16) . . ?
C51 C60 H60A 120.5 . . ?
C59 C60 H60A 120.5 . . ?
C62 C61 C66 120.28(15) . . ?
C62 C61 N3 119.32(14) . . ?
C66 C61 N3 120.33(15) . . ?
C63 C62 C61 118.47(15) . . ?
C63 C62 C67 118.07(15) . . ?
C61 C62 C67 123.43(14) . . ?
C64 C63 C62 121.53(16) . . ?
C64 C63 H63A 119.2 . . ?
C62 C63 H63A 119.2 . . ?
C65 C64 C63 119.03(16) . . ?
C65 C64 H64A 120.5 . . ?
C63 C64 H64A 120.5 . . ?
C64 C65 C66 122.16(17) . . ?
C64 C65 H65A 118.9 . . ?
C66 C65 H65A 118.9 . . ?
C65 C66 C61 118.25(16) . . ?
C65 C66 C70 119.42(15) . . ?
C61 C66 C70 122.31(15) . . ?
C62 C67 C69 111.33(14) . . ?
C62 C67 C68 110.73(14) . . ?
C69 C67 C68 110.92(14) . . ?
C62 C67 H67A 107.9 . . ?
C69 C67 H67A 107.9 . . ?
C68 C67 H67A 107.9 . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C67 C69 H69A 109.5 . . ?
C67 C69 H69B 109.5 . . ?
H69A C69 H69B 109.5 . . ?
C67 C69 H69C 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C72 C70 C71 110.29(18) . . ?
C72 C70 C66 110.75(16) . . ?
C71 C70 C66 113.51(15) . . ?
C72 C70 H70A 107.3 . . ?
C71 C70 H70A 107.3 . . ?
C66 C70 H70A 107.3 . . ?
C70 C71 H71A 109.5 . . ?
C70 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
C70 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C70 C72 H72A 109.5 . . ?
C70 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C70 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
O4 C73 C74 129.08(15) . . ?
O4 C73 C77 124.00(14) . . ?
C74 C73 C77 106.91(14) . . ?
O4 C73 Na1 45.40(7) . . ?
C74 C73 Na1 83.87(10) . . ?
C77 C73 Na1 167.96(11) . . ?
O4 C73 Na4 44.69(7) . . ?
C74 C73 Na4 122.77(11) . . ?
C77 C73 Na4 108.14(9) . . ?
Na1 C73 Na4 68.78(4) . . ?
C73 C74 N4 123.49(14) . . ?
C73 C74 C75 109.91(14) . . ?
N4 C74 C75 126.49(14) . . ?
C84 C75 C76 117.04(15) . . ?
C84 C75 C74 136.82(16) . . ?
C76 C75 C74 106.10(14) . . ?
C81 C76 C77 124.52(15) . . ?
C81 C76 C75 125.20(15) . . ?
C77 C76 C75 110.27(14) . . ?
C78 C77 C76 118.80(15) . . ?
C78 C77 C73 134.39(15) . . ?
C76 C77 C73 106.79(14) . . ?
C77 C78 C79 118.18(16) . . ?
C77 C78 H78A 120.9 . . ?
C79 C78 H78A 120.9 . . ?
C80 C79 C78 122.57(16) . . ?
C80 C79 H79A 118.7 . . ?
C78 C79 H79A 118.7 . . ?
C79 C80 C81 120.25(16) . . ?
C79 C80 H80A 119.9 . . ?
C81 C80 H80A 119.9 . . ?
C76 C81 C80 115.68(15) . . ?
C76 C81 C82 116.26(15) . . ?
C80 C81 C82 128.06(16) . . ?
C83 C82 C81 119.35(15) . . ?
C83 C82 H82A 120.3 . . ?
C81 C82 H82A 120.3 . . ?
C82 C83 C84 123.26(16) . . ?
C82 C83 H83A 118.4 . . ?
C84 C83 H83A 118.4 . . ?
C75 C84 C83 118.89(16) . . ?
C75 C84 H84A 120.6 . . ?
C83 C84 H84A 120.6 . . ?
C90 C85 C86 120.19(14) . . ?
C90 C85 N4 119.09(14) . . ?
C86 C85 N4 120.71(14) . . ?
C87 C86 C85 118.30(15) . . ?
C87 C86 C91 117.64(15) . . ?
C85 C86 C91 124.03(14) . . ?
C88 C87 C86 121.98(16) . . ?
C88 C87 H87A 119.0 . . ?
C86 C87 H87A 119.0 . . ?
C89 C88 C87 118.89(16) . . ?
C89 C88 H88A 120.6 . . ?
C87 C88 H88A 120.6 . . ?
C88 C89 C90 122.01(16) . . ?
C88 C89 H89A 119.0 . . ?
C90 C89 H89A 119.0 . . ?
C89 C90 C85 118.44(15) . . ?
C89 C90 C94 117.12(15) . . ?
C85 C90 C94 124.44(14) . . ?
C86 C91 C92 110.09(16) . . ?
C86 C91 C93 112.77(16) . . ?
C92 C91 C93 109.38(17) . . ?
C86 C91 H91A 108.2 . . ?
C92 C91 H91A 108.2 . . ?
C93 C91 H91A 108.2 . . ?
C91 C92 H92A 109.5 . . ?
C91 C92 H92B 109.5 . . ?
H92A C92 H92B 109.5 . . ?
C91 C92 H92C 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
C91 C93 H93A 109.5 . . ?
C91 C93 H93B 109.5 . . ?
H93A C93 H93B 109.5 . . ?
C91 C93 H93C 109.5 . . ?
H93A C93 H93C 109.5 . . ?
H93B C93 H93C 109.5 . . ?
C90 C94 C95 110.48(14) . . ?
C90 C94 C96 111.14(15) . . ?
C95 C94 C96 110.17(15) . . ?
C90 C94 H94A 108.3 . . ?
C95 C94 H94A 108.3 . . ?
C96 C94 H94A 108.3 . . ?
C94 C95 H95A 109.5 . . ?
C94 C95 H95B 109.5 . . ?
H95A C95 H95B 109.5 . . ?
C94 C95 H95C 109.5 . . ?
H95A C95 H95C 109.5 . . ?
H95B C95 H95C 109.5 . . ?
C94 C96 H96A 109.5 . . ?
C94 C96 H96B 109.5 . . ?
H96A C96 H96B 109.5 . . ?
C94 C96 H96C 109.5 . . ?
H96A C96 H96C 109.5 . . ?
H96B C96 H96C 109.5 . . ?
C4S O1S C1S 104.0(4) . . ?
C4S O1S Na1 129.1(3) . . ?
C1S O1S Na1 126.1(3) . . ?
O1S C1S C2S 105.7(3) . . ?
O1S C1S H1SA 110.6 . . ?
C2S C1S H1SA 110.6 . . ?
O1S C1S H1SB 110.6 . . ?
C2S C1S H1SB 110.6 . . ?
H1SA C1S H1SB 108.7 . . ?
C1S C2S C3S 102.4(3) . . ?
C1S C2S H2SA 111.3 . . ?
C3S C2S H2SA 111.3 . . ?
C1S C2S H2SB 111.3 . . ?
C3S C2S H2SB 111.3 . . ?
H2SA C2S H2SB 109.2 . . ?
C4S C3S C2S 105.1(4) . . ?
C4S C3S H3SA 110.7 . . ?
C2S C3S H3SA 110.7 . . ?
C4S C3S H3SB 110.7 . . ?
C2S C3S H3SB 110.7 . . ?
H3SA C3S H3SB 108.8 . . ?
O1S C4S C3S 107.1(4) . . ?
O1S C4S H4SA 110.3 . . ?
C3S C4S H4SA 110.3 . . ?
O1S C4S H4SB 110.3 . . ?
C3S C4S H4SB 110.3 . . ?
H4SA C4S H4SB 108.6 . . ?
C4* O1* C1* 109.1(5) . . ?
C4* O1* Na1 122.7(4) . . ?
C1* O1* Na1 126.4(4) . . ?
O1* C1* C2* 106.6(5) . . ?
O1* C1* H1*A 110.4 . . ?
C2* C1* H1*A 110.4 . . ?
O1* C1* H1*B 110.4 . . ?
C2* C1* H1*B 110.4 . . ?
H1*A C1* H1*B 108.6 . . ?
C3* C2* C1* 107.5(5) . . ?
C3* C2* H2*A 110.2 . . ?
C1* C2* H2*A 110.2 . . ?
C3* C2* H2*B 110.2 . . ?
C1* C2* H2*B 110.2 . . ?
H2*A C2* H2*B 108.5 . . ?
C2* C3* C4* 102.4(5) . . ?
C2* C3* H3*A 111.3 . . ?
C4* C3* H3*A 111.3 . . ?
C2* C3* H3*B 111.3 . . ?
C4* C3* H3*B 111.3 . . ?
H3*A C3* H3*B 109.2 . . ?
O1* C4* C3* 108.4(5) . . ?
O1* C4* H4*A 110.0 . . ?
C3* C4* H4*A 110.0 . . ?
O1* C4* H4*B 110.0 . . ?
C3* C4* H4*B 110.0 . . ?
H4*A C4* H4*B 108.4 . . ?
C5S O2S C8S 106.78(17) . . ?
C5S O2S Na2 129.83(14) . . ?
C8S O2S Na2 122.90(13) . . ?
O2S C5S C6S 107.0(2) . . ?
O2S C5S H5SA 110.3 . . ?
C6S C5S H5SA 110.3 . . ?
O2S C5S H5SB 110.3 . . ?
C6S C5S H5SB 110.3 . . ?
H5SA C5S H5SB 108.6 . . ?
C5S C6S C7S 105.2(2) . . ?
C5S C6S H6SA 110.7 . . ?
C7S C6S H6SA 110.7 . . ?
C5S C6S H6SB 110.7 . . ?
C7S C6S H6SB 110.7 . . ?
H6SA C6S H6SB 108.8 . . ?
C8S C7S C6S 103.6(2) . . ?
C8S C7S H7SA 111.0 . . ?
C6S C7S H7SA 111.0 . . ?
C8S C7S H7SB 111.0 . . ?
C6S C7S H7SB 111.0 . . ?
H7SA C7S H7SB 109.0 . . ?
O2S C8S C7S 106.3(2) . . ?
O2S C8S H8SA 110.5 . . ?
C7S C8S H8SA 110.5 . . ?
O2S C8S H8SB 110.5 . . ?
C7S C8S H8SB 110.5 . . ?
H8SA C8S H8SB 108.7 . . ?
C12S O3S C9S 107.45(13) . . ?
C12S O3S Na3 125.76(11) . . ?
C9S O3S Na3 126.04(11) . . ?
O3S C9S C10S 106.96(15) . . ?
O3S C9S H9SA 110.3 . . ?
C10S C9S H9SA 110.3 . . ?
O3S C9S H9SB 110.3 . . ?
C10S C9S H9SB 110.3 . . ?
H9SA C9S H9SB 108.6 . . ?
C11S C10S C9S 104.41(15) . . ?
C11S C10S H10B 110.9 . . ?
C9S C10S H10B 110.9 . . ?
C11S C10S H10C 110.9 . . ?
C9S C10S H10C 110.9 . . ?
H10B C10S H10C 108.9 . . ?
C12S C11S C10S 102.76(16) . . ?
C12S C11S H11B 111.2 . . ?
C10S C11S H11B 111.2 . . ?
C12S C11S H11C 111.2 . . ?
C10S C11S H11C 111.2 . . ?
H11B C11S H11C 109.1 . . ?
O3S C12S C11S 104.41(15) . . ?
O3S C12S H12B 110.9 . . ?
C11S C12S H12B 110.9 . . ?
O3S C12S H12C 110.9 . . ?
C11S C12S H12C 110.9 . . ?
H12B C12S H12C 108.9 . . ?
C16S O4S C13S 108.50(15) . . ?
C16S O4S Na4 123.87(11) . . ?
C13S O4S Na4 127.61(12) . . ?
O4S C13S C14S 106.70(17) . . ?
O4S C13S H13A 110.4 . . ?
C14S C13S H13A 110.4 . . ?
O4S C13S H13B 110.4 . . ?
C14S C13S H13B 110.4 . . ?
H13A C13S H13B 108.6 . . ?
C15S C14S C13S 104.55(16) . . ?
C15S C14S H14A 110.8 . . ?
C13S C14S H14A 110.8 . . ?
C15S C14S H14B 110.8 . . ?
C13S C14S H14B 110.8 . . ?
H14A C14S H14B 108.9 . . ?
C16S C15S C14S 102.58(18) . . ?
C16S C15S H15B 111.3 . . ?
C14S C15S H15B 111.3 . . ?
C16S C15S H15C 111.3 . . ?
C14S C15S H15C 111.3 . . ?
H15B C15S H15C 109.2 . . ?
O4S C16S C15S 104.74(16) . . ?
O4S C16S H16B 110.8 . . ?
C15S C16S H16B 110.8 . . ?
O4S C16S H16C 110.8 . . ?
C15S C16S H16C 110.8 . . ?
H16B C16S H16C 108.9 . . ?
C18S C17S C22S 120.0 . . ?
C18S C17S C23S 117.0(2) . . ?
C22S C17S C23S 122.8(2) . . ?
C17S C18S C19S 120.0 . . ?
C17S C18S H18A 120.0 . . ?
C19S C18S H18A 120.0 . . ?
C18S C19S C20S 120.0 . . ?
C18S C19S H19B 120.0 . . ?
C20S C19S H19B 120.0 . . ?
C21S C20S C19S 120.0 . . ?
C21S C20S H20D 120.0 . . ?
C19S C20S H20D 120.0 . . ?
C22S C21S C20S 120.0 . . ?
C22S C21S H21D 120.0 . . ?
C20S C21S H21D 120.0 . . ?
C21S C22S C17S 120.0 . . ?
C21S C22S H22B 120.0 . . ?
C17S C22S H22B 120.0 . . ?
C17S C23S H23D 109.5 . . ?
C17S C23S H23E 109.5 . . ?
H23D C23S H23E 109.5 . . ?
C17S C23S H23F 109.5 . . ?
H23D C23S H23F 109.5 . . ?
H23E C23S H23F 109.5 . . ?
C25S C24S C29S 120.0 . . ?
C25S C24S C30S 114.5(5) . . ?
C29S C24S C30S 125.2(5) . . ?
C26S C25S C24S 120.0 . . ?
C26S C25S H25A 120.0 . . ?
C24S C25S H25A 120.0 . . ?
C25S C26S C27S 120.0 . . ?
C25S C26S H26A 120.0 . . ?
C27S C26S H26A 120.0 . . ?
C28S C27S C26S 120.0 . . ?
C28S C27S H27A 120.0 . . ?
C26S C27S H27A 120.0 . . ?
C29S C28S C27S 120.0 . . ?
C29S C28S H28A 120.0 . . ?
C27S C28S H28A 120.0 . . ?
C28S C29S C24S 120.0 . . ?
C28S C29S H29A 120.0 . . ?
C24S C29S H29A 120.0 . . ?
C24S C30S H30B 109.5 . . ?
C24S C30S H30C 109.5 . . ?
H30B C30S H30C 109.5 . . ?
C24S C30S H30D 109.5 . . ?
H30B C30S H30D 109.5 . . ?
H30C C30S H30D 109.5 . . ?
C25* C24* C29* 120.0 . . ?
C25* C24* C30* 117.9(5) . . ?
C29* C24* C30* 122.1(5) . . ?
C26* C25* C24* 120.0 . . ?
C26* C25* H25B 120.0 . . ?
C24* C25* H25B 120.0 . . ?
C25* C26* C27* 120.0 . . ?
C25* C26* H26B 120.0 . . ?
C27* C26* H26B 120.0 . . ?
C28* C27* C26* 120.0 . . ?
C28* C27* H27B 120.0 . . ?
C26* C27* H27B 120.0 . . ?
C27* C28* C29* 120.0 . . ?
C27* C28* H28B 120.0 . . ?
C29* C28* H28B 120.0 . . ?
C28* C29* C24* 120.0 . . ?
C28* C29* H29B 120.0 . . ?
C24* C29* H29B 120.0 . . ?
C24* C30* H30E 109.5 . . ?
C24* C30* H30F 109.5 . . ?
H30E C30* H30F 109.5 . . ?
C24* C30* H30G 109.5 . . ?
H30E C30* H30G 109.5 . . ?
H30F C30* H30G 109.5 . . ?

_refine_diff_density_max         0.985
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.053

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mianh2
_database_code_depnum_ccdc_archive 'CCDC 2395058'
loop_
_audit_author_name
_audit_author_address
'Anton Cherkasov'
;IOMC RAS
Russia
;
_audit_update_record             
;
2024-10-30 deposited with the CCDC.	2025-02-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H25 N O'
_chemical_formula_sum            'C24 H25 N O'
_chemical_formula_weight         343.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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'

_cell_length_a                   14.8981(6)
_cell_length_b                   8.6526(3)
_cell_length_c                   16.0807(8)
_cell_angle_alpha                90
_cell_angle_beta                 110.599(5)
_cell_angle_gamma                90
_cell_volume                     1940.39(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6154
_cell_measurement_theta_min      3.96
_cell_measurement_theta_max      30.43

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_F_000             736
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.390
_exptl_crystal_size_min          0.310
_exptl_absorpt_coefficient_mu    0.071
_shelx_estimated_absorpt_T_min   0.964
_shelx_estimated_absorpt_T_max   0.978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.978
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_process_details   'CAP 38.43'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Rigaku OD Xcalibur E'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27809
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.209
_diffrn_reflns_theta_max         27.100
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4273
_reflns_number_gt                3081
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CAP 38.43'
_computing_cell_refinement       'CAP 38.43'
_computing_data_reduction        'CAP 38.43'
_computing_structure_solution    'SHELXT 2018/2'
_computing_structure_refinement  'SHELXL 2019/2'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0950P)²+0.9168P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4273
_refine_ls_number_parameters     247
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0673
_refine_ls_wR_factor_ref         0.1959
_refine_ls_wR_factor_gt          0.1805
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.48378(12) 0.67751(18) 0.52008(11) 0.0474(4) Uani 1 1 d . . . . .
N1 N 0.38909(13) 0.4257(2) 0.57789(12) 0.0363(4) Uani 1 1 d . . . . .
H1A H 0.4271(17) 0.362(3) 0.5699(16) 0.042(7) Uiso 1 1 d . . . . .
C1 C 0.50826(15) 0.6316(2) 0.59583(16) 0.0385(5) Uani 1 1 d . . . . .
C2 C 0.43963(15) 0.5500(3) 0.63630(15) 0.0379(5) Uani 1 1 d . . . . .
H2A H 0.3898(16) 0.630(3) 0.6382(15) 0.040(6) Uiso 1 1 d . . . . .
C3 C 0.50627(15) 0.5077(2) 0.73117(14) 0.0364(5) Uani 1 1 d . . . . .
C4 C 0.59831(15) 0.5690(2) 0.74480(16) 0.0407(5) Uani 1 1 d . . . . .
C5 C 0.60407(16) 0.6410(3) 0.66718(17) 0.0451(6) Uani 1 1 d . . . . .
C6 C 0.69046(18) 0.7029(3) 0.6696(2) 0.0635(8) Uani 1 1 d . . . . .
H6A H 0.697133 0.749283 0.618536 0.076 Uiso 1 1 calc R U . . .
C7 C 0.7675(2) 0.6947(4) 0.7498(3) 0.0770(10) Uani 1 1 d . . . . .
H7A H 0.826976 0.737634 0.752128 0.092 Uiso 1 1 calc R U . . .
C8 C 0.76265(19) 0.6287(4) 0.8254(2) 0.0705(9) Uani 1 1 d . . . . .
H8A H 0.817523 0.628609 0.878264 0.085 Uiso 1 1 calc R U . . .
C9 C 0.67477(17) 0.5595(3) 0.82505(19) 0.0524(6) Uani 1 1 d . . . . .
C10 C 0.65696(19) 0.4813(3) 0.89467(18) 0.0580(7) Uani 1 1 d . . . . .
H10A H 0.707082 0.471048 0.950639 0.070 Uiso 1 1 calc R U . . .
C11 C 0.56787(19) 0.4193(3) 0.88278(17) 0.0525(6) Uani 1 1 d . . . . .
H11A H 0.557954 0.366988 0.930761 0.063 Uiso 1 1 calc R U . . .
C12 C 0.49096(16) 0.4321(3) 0.80060(15) 0.0424(5) Uani 1 1 d . . . . .
H12A H 0.429926 0.389448 0.793392 0.051 Uiso 1 1 calc R U . . .
C13 C 0.31748(14) 0.3473(2) 0.60164(13) 0.0337(4) Uani 1 1 d . . . . .
C14 C 0.33381(15) 0.1970(2) 0.63871(14) 0.0373(5) Uani 1 1 d . . . . .
C15 C 0.25932(18) 0.1265(3) 0.65877(17) 0.0487(6) Uani 1 1 d . . . . .
H15A H 0.268150 0.025211 0.683106 0.058 Uiso 1 1 calc R U . . .
C16 C 0.17353(19) 0.2013(3) 0.64386(19) 0.0559(7) Uani 1 1 d . . . . .
H16A H 0.124576 0.152274 0.659393 0.067 Uiso 1 1 calc R U . . .
C17 C 0.15810(17) 0.3468(3) 0.60656(18) 0.0502(6) Uani 1 1 d . . . . .
H17A H 0.098249 0.396321 0.596309 0.060 Uiso 1 1 calc R U . . .
C18 C 0.22842(15) 0.4224(3) 0.58365(14) 0.0384(5) Uani 1 1 d . . . . .
C19 C 0.42767(17) 0.1130(3) 0.65340(15) 0.0429(5) Uani 1 1 d . . . . .
H19A H 0.478937 0.193116 0.664347 0.052 Uiso 1 1 calc R U . . .
C20 C 0.4234(2) 0.0235(3) 0.57036(17) 0.0512(6) Uani 1 1 d . . . . .
H20A H 0.407339 0.094346 0.519660 0.077 Uiso 1 1 calc R U . . .
H20B H 0.374256 -0.057124 0.558256 0.077 Uiso 1 1 calc R U . . .
H20C H 0.485880 -0.024232 0.579812 0.077 Uiso 1 1 calc R U . . .
C21 C 0.4580(3) 0.0035(4) 0.73305(19) 0.0721(9) Uani 1 1 d . . . . .
H21A H 0.462440 0.061010 0.786860 0.108 Uiso 1 1 calc R U . . .
H21B H 0.520609 -0.041604 0.740165 0.108 Uiso 1 1 calc R U . . .
H21C H 0.410393 -0.079144 0.723210 0.108 Uiso 1 1 calc R U . . .
C22 C 0.20550(17) 0.5764(3) 0.53498(16) 0.0464(6) Uani 1 1 d . . . . .
H22A H 0.266019 0.616547 0.529303 0.056 Uiso 1 1 calc R U . . .
C23 C 0.1328(2) 0.5527(4) 0.44114(19) 0.0720(9) Uani 1 1 d . . . . .
H23A H 0.117985 0.652499 0.410524 0.108 Uiso 1 1 calc R U . . .
H23B H 0.073893 0.507546 0.444718 0.108 Uiso 1 1 calc R U . . .
H23C H 0.159811 0.482873 0.408101 0.108 Uiso 1 1 calc R U . . .
C24 C 0.1696(3) 0.6967(3) 0.5847(2) 0.0709(9) Uani 1 1 d . . . . .
H24A H 0.160055 0.795211 0.552688 0.106 Uiso 1 1 calc R U . . .
H24B H 0.217021 0.710174 0.644535 0.106 Uiso 1 1 calc R U . . .
H24C H 0.108711 0.662202 0.588861 0.106 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 C1 1.209(3) . ?
N1 C13 1.425(3) . ?
N1 C2 1.453(3) . ?
N1 H1A 0.83(3) . ?
C1 C5 1.486(3) . ?
C1 C2 1.561(3) . ?
C2 C3 1.543(3) . ?
C2 H2A 1.03(2) . ?
C3 C12 1.380(3) . ?
C3 C4 1.413(3) . ?
C4 C9 1.391(3) . ?
C4 C5 1.424(3) . ?
C5 C6 1.382(3) . ?
C6 C7 1.394(4) . ?
C6 H6A 0.9500 . ?
C7 C8 1.367(5) . ?
C7 H7A 0.9500 . ?
C8 C9 1.438(4) . ?
C8 H8A 0.9500 . ?
C9 C10 1.411(4) . ?
C10 C11 1.381(4) . ?
C10 H10A 0.9500 . ?
C11 C12 1.416(3) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9500 . ?
C13 C18 1.413(3) . ?
C13 C14 1.416(3) . ?
C14 C15 1.400(3) . ?
C14 C19 1.519(3) . ?
C15 C16 1.376(4) . ?
C15 H15A 0.9500 . ?
C16 C17 1.379(4) . ?
C16 H16A 0.9500 . ?
C17 C18 1.390(3) . ?
C17 H17A 0.9500 . ?
C18 C22 1.522(3) . ?
C19 C20 1.526(3) . ?
C19 C21 1.528(4) . ?
C19 H19A 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C24 1.519(4) . ?
C22 C23 1.531(4) . ?
C22 H22A 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

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
C13 N1 C2 116.47(17) . . ?
C13 N1 H1A 109.9(17) . . ?
C2 N1 H1A 111.4(17) . . ?
O1 C1 C5 128.9(2) . . ?
O1 C1 C2 124.0(2) . . ?
C5 C1 C2 107.16(19) . . ?
N1 C2 C3 118.06(18) . . ?
N1 C2 C1 109.40(17) . . ?
C3 C2 C1 103.39(17) . . ?
N1 C2 H2A 107.8(13) . . ?
C3 C2 H2A 110.6(13) . . ?
C1 C2 H2A 107.1(13) . . ?
C12 C3 C4 118.7(2) . . ?
C12 C3 C2 132.85(19) . . ?
C4 C3 C2 108.41(18) . . ?
C9 C4 C3 123.7(2) . . ?
C9 C4 C5 123.8(2) . . ?
C3 C4 C5 112.5(2) . . ?
C6 C5 C4 119.2(2) . . ?
C6 C5 C1 132.4(2) . . ?
C4 C5 C1 108.37(19) . . ?
C5 C6 C7 117.5(3) . . ?
C5 C6 H6A 121.3 . . ?
C7 C6 H6A 121.3 . . ?
C8 C7 C6 124.1(3) . . ?
C8 C7 H7A 118.0 . . ?
C6 C7 H7A 118.0 . . ?
C7 C8 C9 120.2(3) . . ?
C7 C8 H8A 119.9 . . ?
C9 C8 H8A 119.9 . . ?
C4 C9 C10 116.3(2) . . ?
C4 C9 C8 115.2(2) . . ?
C10 C9 C8 128.5(2) . . ?
C11 C10 C9 121.1(2) . . ?
C11 C10 H10A 119.5 . . ?
C9 C10 H10A 119.5 . . ?
C10 C11 C12 121.4(2) . . ?
C10 C11 H11A 119.3 . . ?
C12 C11 H11A 119.3 . . ?
C3 C12 C11 118.8(2) . . ?
C3 C12 H12A 120.6 . . ?
C11 C12 H12A 120.6 . . ?
C18 C13 C14 121.23(18) . . ?
C18 C13 N1 117.66(19) . . ?
C14 C13 N1 121.06(19) . . ?
C15 C14 C13 117.7(2) . . ?
C15 C14 C19 121.1(2) . . ?
C13 C14 C19 121.17(19) . . ?
C16 C15 C14 121.2(2) . . ?
C16 C15 H15A 119.4 . . ?
C14 C15 H15A 119.4 . . ?
C15 C16 C17 120.5(2) . . ?
C15 C16 H16A 119.7 . . ?
C17 C16 H16A 119.7 . . ?
C16 C17 C18 121.3(2) . . ?
C16 C17 H17A 119.4 . . ?
C18 C17 H17A 119.4 . . ?
C17 C18 C13 118.0(2) . . ?
C17 C18 C22 119.7(2) . . ?
C13 C18 C22 122.17(19) . . ?
C14 C19 C20 110.75(19) . . ?
C14 C19 C21 114.3(2) . . ?
C20 C19 C21 109.1(2) . . ?
C14 C19 H19A 107.5 . . ?
C20 C19 H19A 107.5 . . ?
C21 C19 H19A 107.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C24 C22 C18 112.7(2) . . ?
C24 C22 C23 110.6(2) . . ?
C18 C22 C23 110.1(2) . . ?
C24 C22 H22A 107.8 . . ?
C18 C22 H22A 107.8 . . ?
C23 C22 H22A 107.8 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

_refine_diff_density_max         0.555
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.049

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ca3mianh6
_database_code_depnum_ccdc_archive 'CCDC 2395055'
loop_
_audit_author_name
_audit_author_address
'Anton Cherkasov'
;IOMC RAS
Russia
;
_audit_update_record             
;
2024-10-30 deposited with the CCDC.	2025-02-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C186 H192 Ca3 N6 O6'
_chemical_formula_sum            'C186 H192 Ca3 N6 O6'
_chemical_formula_weight         2727.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   26.9692(16)
_cell_length_b                   26.9692(16)
_cell_length_c                   17.5013(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     11023.9(15)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9838
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      24.76

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_F_000             4374
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.175
_shelx_estimated_absorpt_T_min   0.940
_shelx_estimated_absorpt_T_max   0.979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus source'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29412
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.097
_diffrn_reflns_theta_max         25.021
_diffrn_reflns_theta_full        25.021
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4332
_reflns_number_gt                2811
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       APEX2
_computing_cell_refinement       'Saint 8.37a'
_computing_data_reduction        'Saint 8.37a'
_computing_structure_solution    'SHELXT 2018/2'
_computing_structure_refinement  'SHELXL 2019/2'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1069P)²+51.0152P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL 2019/2'
_refine_ls_extinction_coef       0.0008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4332
_refine_ls_number_parameters     411
_refine_ls_number_restraints     524
_refine_ls_R_factor_all          0.1390
_refine_ls_R_factor_gt           0.0895
_refine_ls_wR_factor_ref         0.2493
_refine_ls_wR_factor_gt          0.2150
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Ca1 Ca 0.666667 0.333333 0.52053(8) 0.0551(5) Uani 1 3 d S T P . .
Ca2 Ca 0.666667 0.333333 0.333333 0.0441(5) Uani 1 6 d S T P . .
O1 O 0.73457(11) 0.34812(12) 0.42787(15) 0.0484(7) Uani 1 1 d . . . . .
N1 N 0.75134(17) 0.43396(17) 0.5386(2) 0.0610(11) Uani 1 1 d . . . . .
H1A H 0.733(2) 0.445(2) 0.509(3) 0.073 Uiso 1 1 d . U . . .
C1 C 0.78492(17) 0.39347(18) 0.4411(2) 0.0462(10) Uani 1 1 d . . . . .
C2 C 0.79647(18) 0.43655(17) 0.4940(2) 0.0471(10) Uani 1 1 d . . . . .
C3 C 0.85711(18) 0.47987(17) 0.4901(2) 0.0478(10) Uani 1 1 d . . . . .
C4 C 0.88133(17) 0.45855(17) 0.4364(2) 0.0455(9) Uani 1 1 d . . . . .
C5 C 0.83933(17) 0.40629(17) 0.4053(2) 0.0451(10) Uani 1 1 d . . . . .
C6 C 0.85563(19) 0.3779(2) 0.3541(3) 0.0572(11) Uani 1 1 d . . . . .
H6A H 0.828155 0.342356 0.332439 0.069 Uiso 1 1 calc R U . . .
C7 C 0.91389(19) 0.4032(2) 0.3351(3) 0.0647(13) Uani 1 1 d . . . . .
H7A H 0.925629 0.383606 0.300950 0.078 Uiso 1 1 calc R U . . .
C8 C 0.9547(2) 0.4554(2) 0.3644(3) 0.0634(12) Uani 1 1 d . . . . .
H8A H 0.993562 0.471545 0.349237 0.076 Uiso 1 1 calc R U . . .
C9 C 0.93868(18) 0.48519(19) 0.4172(3) 0.0538(11) Uani 1 1 d . . . . .
C10 C 0.9747(2) 0.5391(2) 0.4529(3) 0.0658(13) Uani 1 1 d . . . . .
H10A H 1.014471 0.559774 0.441684 0.079 Uiso 1 1 calc R U . . .
C11 C 0.9519(2) 0.5609(2) 0.5030(3) 0.0710(14) Uani 1 1 d . . . . .
H11A H 0.976526 0.597137 0.525634 0.085 Uiso 1 1 calc R U . . .
C12 C 0.8931(2) 0.53192(18) 0.5230(3) 0.0611(12) Uani 1 1 d . . . . .
H12A H 0.878816 0.548302 0.558636 0.073 Uiso 1 1 calc R U . . .
C13 C 0.7641(2) 0.4703(2) 0.6044(3) 0.0590(12) Uani 1 1 d . . . . .
C14 C 0.7901(2) 0.4617(2) 0.6684(3) 0.0611(12) Uani 1 1 d . . . . .
C15 C 0.7999(2) 0.4962(2) 0.7322(3) 0.0661(13) Uani 1 1 d . . . . .
H15A H 0.818062 0.491346 0.775807 0.079 Uiso 1 1 calc R U . . .
C16 C 0.7837(3) 0.5371(2) 0.7332(3) 0.0743(15) Uani 1 1 d . . . . .
H16A H 0.791609 0.560985 0.776675 0.089 Uiso 1 1 calc R U . . .
C17 C 0.7560(3) 0.5435(2) 0.6710(3) 0.0788(16) Uani 1 1 d . . . . .
H17A H 0.743843 0.571014 0.672833 0.095 Uiso 1 1 calc R U . . .
C18 C 0.7454(2) 0.5103(2) 0.6056(3) 0.0708(14) Uani 1 1 d . . . . .
C19 C 0.8048(2) 0.4141(2) 0.6730(3) 0.0706(13) Uani 1 1 d . . . . .
H19A H 0.798077 0.395693 0.621572 0.085 Uiso 1 1 calc R U . . .
C20 C 0.7660(3) 0.3686(3) 0.7307(4) 0.101(2) Uani 1 1 d . . . . .
H20A H 0.725956 0.352739 0.715443 0.151 Uiso 1 1 calc R U . . .
H20B H 0.771872 0.385925 0.781460 0.151 Uiso 1 1 calc R U . . .
H20C H 0.775445 0.337882 0.732039 0.151 Uiso 1 1 calc R U . . .
C21 C 0.8674(3) 0.4366(3) 0.6949(4) 0.0942(19) Uani 1 1 d . . . . .
H21A H 0.892435 0.464464 0.656613 0.141 Uiso 1 1 calc R U . . .
H21B H 0.874939 0.404684 0.697012 0.141 Uiso 1 1 calc R U . . .
H21C H 0.874974 0.455200 0.745031 0.141 Uiso 1 1 calc R U . . .
C22 C 0.7152(3) 0.5187(3) 0.5369(3) 0.0875(17) Uani 1 1 d . . . . .
H22A H 0.689(3) 0.479(3) 0.511(4) 0.105 Uiso 1 1 d . U . . .
C23 C 0.6748(3) 0.5387(3) 0.5536(3) 0.0882(17) Uani 1 1 d . . . . .
H23A H 0.655006 0.538479 0.506486 0.132 Uiso 1 1 calc R U . . .
H23B H 0.695655 0.577679 0.574107 0.132 Uiso 1 1 calc R U . . .
H23C H 0.646672 0.513208 0.591221 0.132 Uiso 1 1 calc R U . . .
C24 C 0.7567(3) 0.5538(4) 0.4790(5) 0.131(3) Uani 1 1 d . U . . .
H24A H 0.736473 0.553956 0.432554 0.197 Uiso 1 1 calc R U . . .
H24B H 0.781555 0.537956 0.467404 0.197 Uiso 1 1 calc R U . . .
H24C H 0.779871 0.592997 0.498076 0.197 Uiso 1 1 calc R U . . .
C1S C 1.0001(3) 0.7148(4) 0.5799(6) 0.075(3) Uani 0.428(3) 1 d DG U P A 1
C2S C 0.9669(4) 0.7166(5) 0.5204(5) 0.098(5) Uani 0.428(3) 1 d DG U P A 1
H2SA H 0.984852 0.738662 0.476042 0.117 Uiso 0.428(3) 1 calc R U P A 1
C3S C 0.9076(4) 0.6861(5) 0.5257(6) 0.087(4) Uani 0.428(3) 1 d G U P A 1
H3SA H 0.884902 0.687381 0.485037 0.104 Uiso 0.428(3) 1 calc R U P A 1
C4S C 0.8813(3) 0.6538(4) 0.5906(6) 0.088(4) Uani 0.428(3) 1 d G U P A 1
H4SA H 0.840771 0.633020 0.594268 0.106 Uiso 0.428(3) 1 calc R U P A 1
C5S C 0.9145(4) 0.6520(4) 0.6502(5) 0.092(4) Uani 0.428(3) 1 d G U P A 1
H5SA H 0.896590 0.629939 0.694504 0.110 Uiso 0.428(3) 1 calc R U P A 1
C6S C 0.9739(4) 0.6825(5) 0.6448(5) 0.096(5) Uani 0.428(3) 1 d DG U P A 1
H6SA H 0.996540 0.681219 0.685510 0.116 Uiso 0.428(3) 1 calc R U P A 1
C7S C 1.0657(4) 0.7465(7) 0.5733(9) 0.118(6) Uani 0.428(3) 1 d D U P A 1
H7SA H 1.076589 0.749161 0.519380 0.178 Uiso 0.428(3) 1 calc R U P A 1
H7SB H 1.080742 0.725581 0.601645 0.178 Uiso 0.428(3) 1 calc R U P A 1
H7SC H 1.081563 0.785149 0.594563 0.178 Uiso 0.428(3) 1 calc R U P A 1
C1' C 0.9758(7) 0.6794(8) 0.6226(9) 0.084(6) Uani 0.260(3) 1 d DG U P B 2
C2' C 1.0303(6) 0.7166(10) 0.5947(11) 0.107(7) Uani 0.260(3) 1 d DG U P B 2
H2SB H 1.063092 0.723366 0.623189 0.128 Uiso 0.260(3) 1 calc R U P B 2
C3' C 1.0369(7) 0.7440(9) 0.5250(11) 0.105(7) Uani 0.260(3) 1 d G U P B 2
H3SB H 1.074147 0.769518 0.505971 0.126 Uiso 0.260(3) 1 calc R U P B 2
C4' C 0.9890(9) 0.7342(9) 0.4833(9) 0.110(7) Uani 0.260(3) 1 d G U P B 2
H4SB H 0.993442 0.752926 0.435715 0.132 Uiso 0.260(3) 1 calc R U P B 2
C5' C 0.9344(8) 0.6969(10) 0.5112(11) 0.106(7) Uani 0.260(3) 1 d G U P B 2
H5SB H 0.901681 0.690181 0.482675 0.128 Uiso 0.260(3) 1 calc R U P B 2
C6' C 0.9279(6) 0.6695(8) 0.5808(11) 0.096(7) Uani 0.260(3) 1 d DG U P B 2
H6SB H 0.890624 0.644028 0.599893 0.115 Uiso 0.260(3) 1 calc R U P B 2
C7' C 0.9685(10) 0.6416(10) 0.6925(12) 0.112(8) Uani 0.260(3) 1 d D U P B 2
H7SD H 0.996672 0.664692 0.731589 0.167 Uiso 0.260(3) 1 calc R U P B 2
H7SE H 0.974381 0.610009 0.677042 0.167 Uiso 0.260(3) 1 calc R U P B 2
H7SF H 0.929803 0.626175 0.713244 0.167 Uiso 0.260(3) 1 calc R U P B 2
C1" C 0.9647(7) 0.7080(9) 0.5409(9) 0.111(7) Uani 0.312(3) 1 d DG U P C 3
C2" C 1.0230(6) 0.7321(8) 0.5547(9) 0.124(7) Uani 0.312(3) 1 d DG U P C 3
H2SC H 1.049952 0.757953 0.518785 0.149 Uiso 0.312(3) 1 calc R U P C 3
C3" C 1.0419(5) 0.7183(7) 0.6209(9) 0.090(5) Uani 0.312(3) 1 d G U P C 3
H3SC H 1.081810 0.734797 0.630328 0.108 Uiso 0.312(3) 1 calc R U P C 3
C4" C 1.0025(6) 0.6804(7) 0.6735(8) 0.091(5) Uani 0.312(3) 1 d G U P C 3
H4SC H 1.015478 0.671040 0.718749 0.109 Uiso 0.312(3) 1 calc R U P C 3
C5" C 0.9442(6) 0.6563(7) 0.6597(9) 0.087(5) Uani 0.312(3) 1 d G U P C 3
H5SC H 0.917287 0.630439 0.695629 0.105 Uiso 0.312(3) 1 calc R U P C 3
C6" C 0.9253(5) 0.6701(8) 0.5935(10) 0.115(8) Uani 0.312(3) 1 d DG U P C 3
H6SC H 0.885428 0.653594 0.584087 0.138 Uiso 0.312(3) 1 calc R U P C 3
C7" C 0.9437(11) 0.7146(14) 0.4619(12) 0.181(12) Uani 0.312(3) 1 d D U P C 3
H7SG H 0.973982 0.724263 0.424013 0.272 Uiso 0.312(3) 1 calc R U P C 3
H7SH H 0.934135 0.745130 0.463795 0.272 Uiso 0.312(3) 1 calc R U P C 3
H7SI H 0.909639 0.678490 0.447441 0.272 Uiso 0.312(3) 1 calc R U P C 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Ca1 O1 2.326(3) . ?
Ca1 O1 2.326(3) 3_665 ?
Ca1 O1 2.326(3) 2_655 ?
Ca1 N1 2.546(4) . ?
Ca1 N1 2.546(4) 3_665 ?
Ca1 N1 2.546(4) 2_655 ?
Ca1 C1 3.092(4) . ?
Ca1 C1 3.092(4) 3_665 ?
Ca1 C1 3.092(4) 2_655 ?
Ca1 C2 3.236(4) 3_665 ?
Ca1 C2 3.236(4) . ?
Ca1 C2 3.237(4) 2_655 ?
Ca1 H1A 2.62(5) . ?
Ca2 O1 2.349(3) 16_655 ?
Ca2 O1 2.349(3) 3_665 ?
Ca2 O1 2.349(3) 18_545 ?
Ca2 O1 2.349(3) 2_655 ?
Ca2 O1 2.349(3) . ?
Ca2 O1 2.349(3) 17 ?
O1 C1 1.316(5) . ?
N1 C2 1.418(6) . ?
N1 C13 1.438(6) . ?
N1 H1A 0.87(5) . ?
C1 C2 1.393(6) . ?
C1 C5 1.469(6) . ?
C2 C3 1.461(6) . ?
C3 C12 1.371(6) . ?
C3 C4 1.420(6) . ?
C4 C9 1.382(6) . ?
C4 C5 1.403(6) . ?
C5 C6 1.385(6) . ?
C6 C7 1.405(6) . ?
C6 H6A 0.9500 . ?
C7 C8 1.381(7) . ?
C7 H7A 0.9500 . ?
C8 C9 1.426(7) . ?
C8 H8A 0.9500 . ?
C9 C10 1.427(6) . ?
C10 C11 1.362(7) . ?
C10 H10A 0.9500 . ?
C11 C12 1.418(7) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9500 . ?
C13 C14 1.400(7) . ?
C13 C18 1.402(7) . ?
C14 C15 1.390(6) . ?
C14 C19 1.523(7) . ?
C15 C16 1.376(7) . ?
C15 H15A 0.9500 . ?
C16 C17 1.379(7) . ?
C16 H16A 0.9500 . ?
C17 C18 1.392(7) . ?
C17 H17A 0.9500 . ?
C18 C22 1.531(8) . ?
C19 C20 1.529(8) . ?
C19 C21 1.530(8) . ?
C19 H19A 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C24 1.453(9) . ?
C22 C23 1.466(8) . ?
C22 H22A 1.04(6) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C1S C2S 1.3900 . ?
C1S C6S 1.3900 . ?
C1S C7S 1.537(5) . ?
C2S C3S 1.3900 . ?
C2S H2SA 0.9500 . ?
C3S C4S 1.3900 . ?
C3S H3SA 0.9500 . ?
C4S C5S 1.3900 . ?
C4S H4SA 0.9500 . ?
C5S C6S 1.3900 . ?
C5S H5SA 0.9500 . ?
C6S H6SA 0.9500 . ?
C7S H7SA 0.9800 . ?
C7S H7SB 0.9800 . ?
C7S H7SC 0.9800 . ?
C1' C2' 1.3900 . ?
C1' C6' 1.3900 . ?
C1' C7' 1.539(5) . ?
C2' C3' 1.3900 . ?
C2' H2SB 0.9500 . ?
C3' C4' 1.3900 . ?
C3' H3SB 0.9500 . ?
C4' C5' 1.3900 . ?
C4' H4SB 0.9500 . ?
C5' C6' 1.3900 . ?
C5' H5SB 0.9500 . ?
C6' H6SB 0.9500 . ?
C7' H7SD 0.9800 . ?
C7' H7SE 0.9800 . ?
C7' H7SF 0.9800 . ?
C1" C2" 1.3900 . ?
C1" C6" 1.3900 . ?
C1" C7" 1.539(5) . ?
C2" C3" 1.3900 . ?
C2" H2SC 0.9500 . ?
C3" C4" 1.3900 . ?
C3" H3SC 0.9500 . ?
C4" C5" 1.3900 . ?
C4" H4SC 0.9500 . ?
C5" C6" 1.3900 . ?
C5" H5SC 0.9500 . ?
C6" H6SC 0.9500 . ?
C7" H7SG 0.9800 . ?
C7" H7SH 0.9800 . ?
C7" H7SI 0.9800 . ?

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
O1 Ca1 O1 76.77(11) . 3_665 ?
O1 Ca1 O1 76.77(11) . 2_655 ?
O1 Ca1 O1 76.76(11) 3_665 2_655 ?
O1 Ca1 N1 72.19(11) . . ?
O1 Ca1 N1 142.81(13) 3_665 . ?
O1 Ca1 N1 76.63(12) 2_655 . ?
O1 Ca1 N1 76.63(12) . 3_665 ?
O1 Ca1 N1 72.19(11) 3_665 3_665 ?
O1 Ca1 N1 142.81(13) 2_655 3_665 ?
N1 Ca1 N1 118.48(4) . 3_665 ?
O1 Ca1 N1 142.81(13) . 2_655 ?
O1 Ca1 N1 76.63(12) 3_665 2_655 ?
O1 Ca1 N1 72.19(11) 2_655 2_655 ?
N1 Ca1 N1 118.48(4) . 2_655 ?
N1 Ca1 N1 118.48(4) 3_665 2_655 ?
O1 Ca1 C1 23.02(10) . . ?
O1 Ca1 C1 99.61(11) 3_665 . ?
O1 Ca1 C1 79.22(10) 2_655 . ?
N1 Ca1 C1 49.95(11) . . ?
N1 Ca1 C1 86.20(13) 3_665 . ?
N1 Ca1 C1 151.29(12) 2_655 . ?
O1 Ca1 C1 79.22(10) . 3_665 ?
O1 Ca1 C1 23.02(10) 3_665 3_665 ?
O1 Ca1 C1 99.61(11) 2_655 3_665 ?
N1 Ca1 C1 151.29(12) . 3_665 ?
N1 Ca1 C1 49.95(11) 3_665 3_665 ?
N1 Ca1 C1 86.20(13) 2_655 3_665 ?
C1 Ca1 C1 101.35(9) . 3_665 ?
O1 Ca1 C1 99.61(11) . 2_655 ?
O1 Ca1 C1 79.22(10) 3_665 2_655 ?
O1 Ca1 C1 23.02(10) 2_655 2_655 ?
N1 Ca1 C1 86.21(13) . 2_655 ?
N1 Ca1 C1 151.29(12) 3_665 2_655 ?
N1 Ca1 C1 49.95(11) 2_655 2_655 ?
C1 Ca1 C1 101.35(9) . 2_655 ?
C1 Ca1 C1 101.34(9) 3_665 2_655 ?
O1 Ca1 C2 79.33(10) . 3_665 ?
O1 Ca1 C2 48.10(10) 3_665 3_665 ?
O1 Ca1 C2 123.52(11) 2_655 3_665 ?
N1 Ca1 C2 140.02(12) . 3_665 ?
N1 Ca1 C2 24.92(11) 3_665 3_665 ?
N1 Ca1 C2 101.19(12) 2_655 3_665 ?
C1 Ca1 C2 96.62(10) . 3_665 ?
C1 Ca1 C2 25.30(10) 3_665 3_665 ?
C1 Ca1 C2 126.51(11) 2_655 3_665 ?
O1 Ca1 C2 48.10(10) . . ?
O1 Ca1 C2 123.53(11) 3_665 . ?
O1 Ca1 C2 79.34(10) 2_655 . ?
N1 Ca1 C2 24.92(11) . . ?
N1 Ca1 C2 101.20(12) 3_665 . ?
N1 Ca1 C2 140.02(12) 2_655 . ?
C1 Ca1 C2 25.30(10) . . ?
C1 Ca1 C2 126.51(11) 3_665 . ?
C1 Ca1 C2 96.62(10) 2_655 . ?
C2 Ca1 C2 117.97(4) 3_665 . ?
O1 Ca1 C2 123.53(11) . 2_655 ?
O1 Ca1 C2 79.33(10) 3_665 2_655 ?
O1 Ca1 C2 48.10(10) 2_655 2_655 ?
N1 Ca1 C2 101.20(12) . 2_655 ?
N1 Ca1 C2 140.02(12) 3_665 2_655 ?
N1 Ca1 C2 24.92(11) 2_655 2_655 ?
C1 Ca1 C2 126.51(11) . 2_655 ?
C1 Ca1 C2 96.62(10) 3_665 2_655 ?
C1 Ca1 C2 25.30(10) 2_655 2_655 ?
C2 Ca1 C2 117.97(4) 3_665 2_655 ?
C2 Ca1 C2 117.97(4) . 2_655 ?
O1 Ca1 H1A 73.9(11) . . ?
O1 Ca1 H1A 130.1(12) 3_665 . ?
O1 Ca1 H1A 57.9(12) 2_655 . ?
N1 Ca1 H1A 19.2(11) . . ?
N1 Ca1 H1A 135.5(11) 3_665 . ?
N1 Ca1 H1A 105.1(11) 2_655 . ?
C1 Ca1 H1A 55.4(11) . . ?
C1 Ca1 H1A 148.1(12) 3_665 . ?
C1 Ca1 H1A 67.3(12) 2_655 . ?
C2 Ca1 H1A 152.0(11) 3_665 . ?
C2 Ca1 H1A 34.9(11) . . ?
C2 Ca1 H1A 84.5(11) 2_655 . ?
O1 Ca2 O1 104.12(10) 16_655 3_665 ?
O1 Ca2 O1 75.88(10) 16_655 18_545 ?
O1 Ca2 O1 180.0 3_665 18_545 ?
O1 Ca2 O1 104.12(10) 16_655 2_655 ?
O1 Ca2 O1 75.88(10) 3_665 2_655 ?
O1 Ca2 O1 104.12(10) 18_545 2_655 ?
O1 Ca2 O1 180.0 16_655 . ?
O1 Ca2 O1 75.88(10) 3_665 . ?
O1 Ca2 O1 104.12(10) 18_545 . ?
O1 Ca2 O1 75.88(10) 2_655 . ?
O1 Ca2 O1 75.88(10) 16_655 17 ?
O1 Ca2 O1 104.12(10) 3_665 17 ?
O1 Ca2 O1 75.88(10) 18_545 17 ?
O1 Ca2 O1 180.0 2_655 17 ?
O1 Ca2 O1 104.12(10) . 17 ?
O1 Ca2 Ca1 134.77(7) 16_655 . ?
O1 Ca2 Ca1 45.23(7) 3_665 . ?
O1 Ca2 Ca1 134.77(7) 18_545 . ?
O1 Ca2 Ca1 45.23(7) 2_655 . ?
O1 Ca2 Ca1 45.23(7) . . ?
O1 Ca2 Ca1 134.77(7) 17 . ?
O1 Ca2 Ca1 45.23(7) 16_655 16_655 ?
O1 Ca2 Ca1 134.77(7) 3_665 16_655 ?
O1 Ca2 Ca1 45.23(7) 18_545 16_655 ?
O1 Ca2 Ca1 134.77(7) 2_655 16_655 ?
O1 Ca2 Ca1 134.76(7) . 16_655 ?
O1 Ca2 Ca1 45.23(7) 17 16_655 ?
Ca1 Ca2 Ca1 180.0 . 16_655 ?
C1 O1 Ca1 113.3(2) . . ?
C1 O1 Ca2 129.5(2) . . ?
Ca1 O1 Ca2 88.96(10) . . ?
C2 N1 C13 120.0(4) . . ?
C2 N1 Ca1 105.9(3) . . ?
C13 N1 Ca1 127.4(3) . . ?
C2 N1 H1A 106(4) . . ?
C13 N1 H1A 104(4) . . ?
Ca1 N1 H1A 85(3) . . ?
O1 C1 C2 126.0(4) . . ?
O1 C1 C5 126.1(4) . . ?
C2 C1 C5 107.8(4) . . ?
O1 C1 Ca1 43.72(18) . . ?
C2 C1 Ca1 83.1(3) . . ?
C5 C1 Ca1 164.2(3) . . ?
C1 C2 N1 119.8(4) . . ?
C1 C2 C3 109.3(4) . . ?
N1 C2 C3 130.9(4) . . ?
C1 C2 Ca1 71.6(2) . . ?
N1 C2 Ca1 49.2(2) . . ?
C3 C2 Ca1 172.5(3) . . ?
C12 C3 C4 117.3(4) . . ?
C12 C3 C2 137.4(4) . . ?
C4 C3 C2 105.3(3) . . ?
C9 C4 C5 124.0(4) . . ?
C9 C4 C3 124.9(4) . . ?
C5 C4 C3 111.1(4) . . ?
C6 C5 C4 119.1(4) . . ?
C6 C5 C1 134.6(4) . . ?
C4 C5 C1 106.3(3) . . ?
C5 C6 C7 118.2(4) . . ?
C5 C6 H6A 120.9 . . ?
C7 C6 H6A 120.9 . . ?
C8 C7 C6 122.3(4) . . ?
C8 C7 H7A 118.9 . . ?
C6 C7 H7A 118.9 . . ?
C7 C8 C9 120.3(4) . . ?
C7 C8 H8A 119.9 . . ?
C9 C8 H8A 119.9 . . ?
C4 C9 C8 116.1(4) . . ?
C4 C9 C10 116.0(4) . . ?
C8 C9 C10 127.9(4) . . ?
C11 C10 C9 119.9(5) . . ?
C11 C10 H10A 120.1 . . ?
C9 C10 H10A 120.1 . . ?
C10 C11 C12 122.8(4) . . ?
C10 C11 H11A 118.6 . . ?
C12 C11 H11A 118.6 . . ?
C3 C12 C11 119.0(4) . . ?
C3 C12 H12A 120.5 . . ?
C11 C12 H12A 120.5 . . ?
C14 C13 C18 121.2(4) . . ?
C14 C13 N1 119.9(4) . . ?
C18 C13 N1 118.7(4) . . ?
C15 C14 C13 118.4(4) . . ?
C15 C14 C19 118.6(5) . . ?
C13 C14 C19 122.9(4) . . ?
C16 C15 C14 121.0(5) . . ?
C16 C15 H15A 119.5 . . ?
C14 C15 H15A 119.5 . . ?
C15 C16 C17 120.0(4) . . ?
C15 C16 H16A 120.0 . . ?
C17 C16 H16A 120.0 . . ?
C16 C17 C18 121.2(5) . . ?
C16 C17 H17A 119.4 . . ?
C18 C17 H17A 119.4 . . ?
C17 C18 C13 118.0(5) . . ?
C17 C18 C22 120.2(5) . . ?
C13 C18 C22 121.7(4) . . ?
C14 C19 C20 110.5(4) . . ?
C14 C19 C21 112.3(5) . . ?
C20 C19 C21 109.2(5) . . ?
C14 C19 H19A 108.2 . . ?
C20 C19 H19A 108.2 . . ?
C21 C19 H19A 108.2 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C24 C22 C23 111.8(6) . . ?
C24 C22 C18 110.5(6) . . ?
C23 C22 C18 116.5(5) . . ?
C24 C22 H22A 106(3) . . ?
C23 C22 H22A 102(3) . . ?
C18 C22 H22A 109(3) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C2S C1S C6S 120.0 . . ?
C2S C1S C7S 120.3(5) . . ?
C6S C1S C7S 119.6(5) . . ?
C1S C2S C3S 120.0 . . ?
C1S C2S H2SA 120.0 . . ?
C3S C2S H2SA 120.0 . . ?
C4S C3S C2S 120.0 . . ?
C4S C3S H3SA 120.0 . . ?
C2S C3S H3SA 120.0 . . ?
C3S C4S C5S 120.0 . . ?
C3S C4S H4SA 120.0 . . ?
C5S C4S H4SA 120.0 . . ?
C6S C5S C4S 120.0 . . ?
C6S C5S H5SA 120.0 . . ?
C4S C5S H5SA 120.0 . . ?
C5S C6S C1S 120.0 . . ?
C5S C6S H6SA 120.0 . . ?
C1S C6S H6SA 120.0 . . ?
C1S C7S H7SA 109.5 . . ?
C1S C7S H7SB 109.5 . . ?
H7SA C7S H7SB 109.5 . . ?
C1S C7S H7SC 109.5 . . ?
H7SA C7S H7SC 109.5 . . ?
H7SB C7S H7SC 109.5 . . ?
C2' C1' C6' 120.0 . . ?
C2' C1' C7' 119.8(6) . . ?
C6' C1' C7' 119.4(6) . . ?
C3' C2' C1' 120.0 . . ?
C3' C2' H2SB 120.0 . . ?
C1' C2' H2SB 120.0 . . ?
C4' C3' C2' 120.0 . . ?
C4' C3' H3SB 120.0 . . ?
C2' C3' H3SB 120.0 . . ?
C3' C4' C5' 120.0 . . ?
C3' C4' H4SB 120.0 . . ?
C5' C4' H4SB 120.0 . . ?
C6' C5' C4' 120.0 . . ?
C6' C5' H5SB 120.0 . . ?
C4' C5' H5SB 120.0 . . ?
C5' C6' C1' 120.0 . . ?
C5' C6' H6SB 120.0 . . ?
C1' C6' H6SB 120.0 . . ?
C1' C7' H7SD 109.5 . . ?
C1' C7' H7SE 109.5 . . ?
H7SD C7' H7SE 109.5 . . ?
C1' C7' H7SF 109.5 . . ?
H7SD C7' H7SF 109.5 . . ?
H7SE C7' H7SF 109.5 . . ?
C2" C1" C6" 120.0 . . ?
C2" C1" C7" 119.8(6) . . ?
C6" C1" C7" 119.3(6) . . ?
C3" C2" C1" 120.0 . . ?
C3" C2" H2SC 120.0 . . ?
C1" C2" H2SC 120.0 . . ?
C2" C3" C4" 120.0 . . ?
C2" C3" H3SC 120.0 . . ?
C4" C3" H3SC 120.0 . . ?
C5" C4" C3" 120.0 . . ?
C5" C4" H4SC 120.0 . . ?
C3" C4" H4SC 120.0 . . ?
C6" C5" C4" 120.0 . . ?
C6" C5" H5SC 120.0 . . ?
C4" C5" H5SC 120.0 . . ?
C5" C6" C1" 120.0 . . ?
C5" C6" H6SC 120.0 . . ?
C1" C6" H6SC 120.0 . . ?
C1" C7" H7SG 109.5 . . ?
C1" C7" H7SH 109.5 . . ?
H7SG C7" H7SH 109.5 . . ?
C1" C7" H7SI 109.5 . . ?
H7SG C7" H7SI 109.5 . . ?
H7SH C7" H7SI 109.5 . . ?

_refine_diff_density_max         0.741
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.060

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_miannaph
_database_code_depnum_ccdc_archive 'CCDC 2395059'
loop_
_audit_author_name
_audit_author_address
'Anton Cherkasov'
;IOMC RAS
Russia
;
_audit_update_record             
;
2024-10-30 deposited with the CCDC.	2025-02-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H15 N O'
_chemical_formula_sum            'C22 H15 N O'
_chemical_formula_weight         309.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_H-M_alt        'A b a 2'
_space_group_name_Hall           'A 2 -2ac'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, z+1/2'

_cell_length_a                   24.2597(8)
_cell_length_b                   44.3767(15)
_cell_length_c                   8.5031(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9154.1(5)
_cell_formula_units_Z            24
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9890
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      30.04

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_F_000             3888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.082
_shelx_estimated_absorpt_T_min   0.952
_shelx_estimated_absorpt_T_max   0.991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus source'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            66504
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -56
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.913
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10079
_reflns_number_gt                7759
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.870
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       APEX2
_computing_cell_refinement       'Saint 8.37a'
_computing_data_reduction        'Saint 8.37a'
_computing_structure_solution    'SHELXT 2018/2'
_computing_structure_refinement  'SHELXL 2019/2'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0698P)²+1.5518P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2984 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   unk
_chemical_absolute_configuration unk
_refine_ls_number_reflns         10079
_refine_ls_number_parameters     673
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0489
_refine_ls_wR_factor_ref         0.1220
_refine_ls_wR_factor_gt          0.1107
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
O1A O 0.46814(10) 0.69884(5) 0.7133(3) 0.0194(6) Uani 1 1 d . . . . .
N1A N 0.58731(10) 0.69918(5) 0.6560(3) 0.0150(6) Uani 1 1 d D . . . .
H1A H 0.5755(14) 0.6812(6) 0.685(5) 0.037(11) Uiso 1 1 d D . . . .
C1A C 0.48897(12) 0.70569(6) 0.5882(4) 0.0144(7) Uani 1 1 d . . . . .
C2A C 0.54854(12) 0.71824(7) 0.5722(4) 0.0134(6) Uani 1 1 d D . . . .
H2A H 0.5474(12) 0.7392(4) 0.618(4) 0.019(8) Uiso 1 1 d D . . . .
C3A C 0.55660(13) 0.71973(7) 0.3945(4) 0.0138(7) Uani 1 1 d . . . . .
C4A C 0.50754(12) 0.71000(6) 0.3218(4) 0.0122(7) Uani 1 1 d . . . . .
C5A C 0.46606(13) 0.70192(7) 0.4286(4) 0.0145(7) Uani 1 1 d . . . . .
C6A C 0.41644(13) 0.69091(6) 0.3756(4) 0.0145(7) Uani 1 1 d . . . . .
H6AA H 0.387899 0.685579 0.446828 0.017 Uiso 1 1 calc R U . . .
C7A C 0.40935(15) 0.68778(7) 0.2111(5) 0.0188(8) Uani 1 1 d . . . . .
H7AA H 0.375480 0.680059 0.172138 0.023 Uiso 1 1 calc R U . . .
C8A C 0.45011(14) 0.69561(7) 0.1058(4) 0.0194(8) Uani 1 1 d . . . . .
H8AA H 0.443681 0.693212 -0.003699 0.023 Uiso 1 1 calc R U . . .
C9A C 0.50168(13) 0.70722(7) 0.1580(5) 0.0161(8) Uani 1 1 d . . . . .
C10A C 0.54744(14) 0.71601(7) 0.0645(4) 0.0205(8) Uani 1 1 d . . . . .
H10A H 0.545147 0.715156 -0.046950 0.025 Uiso 1 1 calc R U . . .
C11A C 0.59472(15) 0.72570(7) 0.1353(4) 0.0222(9) Uani 1 1 d . . . . .
H11A H 0.624986 0.731385 0.070906 0.027 Uiso 1 1 calc R U . . .
C12A C 0.60056(13) 0.72763(7) 0.3018(5) 0.0190(8) Uani 1 1 d . . . . .
H12A H 0.634173 0.734244 0.347533 0.023 Uiso 1 1 calc R U . . .
C13A C 0.63528(14) 0.70993(7) 0.7233(4) 0.0130(8) Uani 1 1 d . . . . .
C14A C 0.65089(14) 0.73970(7) 0.7127(4) 0.0186(8) Uani 1 1 d . . . . .
H14A H 0.628755 0.753333 0.654173 0.022 Uiso 1 1 calc R U . . .
C15A C 0.69893(13) 0.75031(7) 0.7868(5) 0.0219(7) Uani 1 1 d . . . . .
H15A H 0.708268 0.771057 0.779734 0.026 Uiso 1 1 calc R U . . .
C16A C 0.73211(12) 0.73128(7) 0.8684(4) 0.0223(7) Uani 1 1 d . . . . .
H16A H 0.763777 0.738860 0.920868 0.027 Uiso 1 1 calc R U . . .
C17A C 0.71954(12) 0.70002(7) 0.8753(4) 0.0170(7) Uani 1 1 d . . . . .
C18A C 0.75516(15) 0.67926(7) 0.9516(4) 0.0237(8) Uani 1 1 d . . . . .
H18A H 0.787455 0.686543 1.002068 0.028 Uiso 1 1 calc R U . . .
C19A C 0.74415(14) 0.64914(7) 0.9543(4) 0.0225(8) Uani 1 1 d . . . . .
H19A H 0.768606 0.635628 1.005698 0.027 Uiso 1 1 calc R U . . .
C20A C 0.69627(13) 0.63822(7) 0.8803(4) 0.0192(7) Uani 1 1 d . . . . .
H20A H 0.688579 0.617236 0.881677 0.023 Uiso 1 1 calc R U . . .
C21A C 0.66066(12) 0.65749(6) 0.8065(4) 0.0153(6) Uani 1 1 d . . . . .
H21A H 0.628548 0.649675 0.757273 0.018 Uiso 1 1 calc R U . . .
C22A C 0.67089(11) 0.68888(6) 0.8022(4) 0.0142(6) Uani 1 1 d . . . . .
O1B O 0.53039(10) 0.63960(5) 0.7038(3) 0.0175(5) Uani 1 1 d . . . . .
N1B N 0.41256(10) 0.63631(5) 0.6494(3) 0.0146(6) Uani 1 1 d D . . . .
H1B H 0.4262(13) 0.6525(6) 0.696(4) 0.029(10) Uiso 1 1 d D . . . .
C1B C 0.51056(12) 0.63134(6) 0.5792(4) 0.0134(6) Uani 1 1 d . . . . .
C2B C 0.45199(12) 0.61760(6) 0.5660(4) 0.0127(6) Uani 1 1 d D . . . .
H2B H 0.4537(12) 0.5965(4) 0.611(3) 0.015(8) Uiso 1 1 d D . . . .
C3B C 0.44418(13) 0.61460(7) 0.3891(4) 0.0136(7) Uani 1 1 d . . . . .
C4B C 0.49363(13) 0.62330(7) 0.3150(4) 0.0130(8) Uani 1 1 d . . . . .
C5B C 0.53450(13) 0.63317(7) 0.4203(4) 0.0140(7) Uani 1 1 d . . . . .
C6B C 0.58435(13) 0.64335(6) 0.3659(4) 0.0155(7) Uani 1 1 d . . . . .
H6BA H 0.612031 0.650268 0.436159 0.019 Uiso 1 1 calc R U . . .
C7B C 0.59311(14) 0.64319(7) 0.2016(5) 0.0178(7) Uani 1 1 d . . . . .
H7BA H 0.627390 0.650155 0.161682 0.021 Uiso 1 1 calc R U . . .
C8B C 0.55350(13) 0.63325(7) 0.0973(4) 0.0190(8) Uani 1 1 d . . . . .
H8BA H 0.561134 0.633318 -0.012270 0.023 Uiso 1 1 calc R U . . .
C9B C 0.50141(13) 0.62289(7) 0.1517(4) 0.0169(8) Uani 1 1 d . . . . .
C10B C 0.45587(13) 0.61303(7) 0.0596(4) 0.0202(8) Uani 1 1 d . . . . .
H10B H 0.459019 0.612043 -0.051682 0.024 Uiso 1 1 calc R U . . .
C11B C 0.40782(15) 0.60500(7) 0.1308(4) 0.0218(8) Uani 1 1 d . . . . .
H11B H 0.377734 0.598807 0.067046 0.026 Uiso 1 1 calc R U . . .
C12B C 0.40083(13) 0.60552(7) 0.2969(5) 0.0194(8) Uani 1 1 d . . . . .
H12B H 0.366807 0.599684 0.343046 0.023 Uiso 1 1 calc R U . . .
C13B C 0.36524(14) 0.62440(7) 0.7168(4) 0.0138(7) Uani 1 1 d . . . . .
C14B C 0.34989(13) 0.59481(7) 0.6945(4) 0.0171(7) Uani 1 1 d . . . . .
H14B H 0.372004 0.582025 0.630844 0.021 Uiso 1 1 calc R U . . .
C15B C 0.30173(14) 0.58331(7) 0.7651(4) 0.0187(7) Uani 1 1 d . . . . .
H15B H 0.292079 0.562792 0.749151 0.022 Uiso 1 1 calc R U . . .
C16B C 0.26888(12) 0.60099(6) 0.8554(4) 0.0206(7) Uani 1 1 d . . . . .
H16B H 0.237055 0.592689 0.904018 0.025 Uiso 1 1 calc R U . . .
C17B C 0.28209(12) 0.63202(7) 0.8774(4) 0.0170(7) Uani 1 1 d . . . . .
C18B C 0.24769(14) 0.65122(7) 0.9669(4) 0.0224(8) Uani 1 1 d . . . . .
H18B H 0.215709 0.643155 1.015775 0.027 Uiso 1 1 calc R U . . .
C19B C 0.25950(14) 0.68111(7) 0.9845(4) 0.0238(8) Uani 1 1 d . . . . .
H19B H 0.235986 0.693664 1.045283 0.029 Uiso 1 1 calc R U . . .
C20B C 0.30692(13) 0.69327(7) 0.9118(4) 0.0191(7) Uani 1 1 d . . . . .
H20B H 0.315153 0.714082 0.923268 0.023 Uiso 1 1 calc R U . . .
C21B C 0.34109(12) 0.67519(6) 0.8248(4) 0.0142(6) Uani 1 1 d . . . . .
H21B H 0.372579 0.683740 0.775619 0.017 Uiso 1 1 calc R U . . .
C22B C 0.33044(11) 0.64415(6) 0.8069(4) 0.0126(6) Uani 1 1 d . . . . .
O1C O 0.46911(11) 0.52931(5) 0.2624(3) 0.0191(6) Uani 1 1 d . . . . .
N1C N 0.58773(11) 0.53093(6) 0.3207(3) 0.0158(6) Uani 1 1 d D . . . .
H1C H 0.5753(14) 0.5142(6) 0.277(4) 0.024(10) Uiso 1 1 d D . . . .
C1C C 0.48965(13) 0.53668(7) 0.3887(4) 0.0143(7) Uani 1 1 d . . . . .
C2C C 0.54872(13) 0.54999(7) 0.4031(4) 0.0161(8) Uani 1 1 d D . . . .
H2C H 0.5470(12) 0.5704(5) 0.350(4) 0.018(9) Uiso 1 1 d D . . . .
C3C C 0.55647(14) 0.55262(7) 0.5793(4) 0.0149(7) Uani 1 1 d . . . . .
C4C C 0.50737(13) 0.54336(7) 0.6538(4) 0.0134(8) Uani 1 1 d . . . . .
C5C C 0.46591(14) 0.53413(7) 0.5472(4) 0.0139(7) Uani 1 1 d . . . . .
C6C C 0.41630(14) 0.52381(7) 0.6024(5) 0.0185(8) Uani 1 1 d . . . . .
H6CA H 0.388375 0.517419 0.531502 0.022 Uiso 1 1 calc R U . . .
C7C C 0.40747(16) 0.52284(8) 0.7655(5) 0.0206(8) Uani 1 1 d . . . . .
H7CA H 0.373243 0.515687 0.804937 0.025 Uiso 1 1 calc R U . . .
C8C C 0.44779(14) 0.53212(7) 0.8698(4) 0.0212(8) Uani 1 1 d . . . . .
H8CA H 0.440449 0.531292 0.979485 0.025 Uiso 1 1 calc R U . . .
C9C C 0.49978(13) 0.54286(7) 0.8179(4) 0.0160(8) Uani 1 1 d . . . . .
C10C C 0.54530(14) 0.55217(7) 0.9094(5) 0.0199(8) Uani 1 1 d . . . . .
H10C H 0.542473 0.552415 1.020850 0.024 Uiso 1 1 calc R U . . .
C11C C 0.59373(14) 0.56089(7) 0.8383(5) 0.0209(8) Uani 1 1 d . . . . .
H11C H 0.624013 0.566809 0.902042 0.025 Uiso 1 1 calc R U . . .
C12C C 0.59960(14) 0.56127(7) 0.6716(5) 0.0190(8) Uani 1 1 d . . . . .
H12C H 0.633339 0.567495 0.625127 0.023 Uiso 1 1 calc R U . . .
C13C C 0.63561(14) 0.54229(7) 0.2546(4) 0.0125(8) Uani 1 1 d . . . . .
C14C C 0.65124(14) 0.57196(7) 0.2711(5) 0.0173(7) Uani 1 1 d . . . . .
H14C H 0.628787 0.585264 0.330732 0.021 Uiso 1 1 calc R U . . .
C15C C 0.69959(15) 0.58289(7) 0.2016(5) 0.0225(8) Uani 1 1 d . . . . .
H15C H 0.709235 0.603492 0.214554 0.027 Uiso 1 1 calc R U . . .
C16C C 0.73325(14) 0.56444(7) 0.1152(4) 0.0232(8) Uani 1 1 d . . . . .
H16C H 0.764967 0.572416 0.064619 0.028 Uiso 1 1 calc R U . . .
C17C C 0.72051(13) 0.53344(7) 0.1018(4) 0.0200(8) Uani 1 1 d . . . . .
C18C C 0.75555(15) 0.51337(7) 0.0215(5) 0.0233(8) Uani 1 1 d . . . . .
H18C H 0.787756 0.521025 -0.027939 0.028 Uiso 1 1 calc R U . . .
C19C C 0.74466(16) 0.48324(7) 0.0124(4) 0.0236(8) Uani 1 1 d . . . . .
H19C H 0.769188 0.470204 -0.041945 0.028 Uiso 1 1 calc R U . . .
C20C C 0.69682(13) 0.47158(7) 0.0841(4) 0.0203(8) Uani 1 1 d . . . . .
H20C H 0.689363 0.450579 0.079426 0.024 Uiso 1 1 calc R U . . .
C21C C 0.66095(13) 0.49049(7) 0.1607(4) 0.0175(7) Uani 1 1 d . . . . .
H21C H 0.628575 0.482439 0.207490 0.021 Uiso 1 1 calc R U . . .
C22C C 0.67148(12) 0.52172(7) 0.1711(4) 0.0147(7) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
O1A C1A 1.216(4) . ?
N1A C13A 1.382(4) . ?
N1A C2A 1.452(4) . ?
N1A H1A 0.88(2) . ?
C1A C5A 1.476(5) . ?
C1A C2A 1.555(4) . ?
C2A C3A 1.525(5) . ?
C2A H2A 1.011(16) . ?
C3A C12A 1.372(5) . ?
C3A C4A 1.409(4) . ?
C4A C5A 1.402(5) . ?
C4A C9A 1.405(6) . ?
C5A C6A 1.375(4) . ?
C6A C7A 1.416(5) . ?
C6A H6AA 0.9500 . ?
C7A C8A 1.379(5) . ?
C7A H7AA 0.9500 . ?
C8A C9A 1.424(4) . ?
C8A H8AA 0.9500 . ?
C9A C10A 1.420(5) . ?
C10A C11A 1.365(5) . ?
C10A H10A 0.9500 . ?
C11A C12A 1.425(6) . ?
C11A H11A 0.9500 . ?
C12A H12A 0.9500 . ?
C13A C14A 1.377(4) . ?
C13A C22A 1.439(4) . ?
C14A C15A 1.406(5) . ?
C14A H14A 0.9500 . ?
C15A C16A 1.357(5) . ?
C15A H15A 0.9500 . ?
C16A C17A 1.422(4) . ?
C16A H16A 0.9500 . ?
C17A C18A 1.420(4) . ?
C17A C22A 1.422(4) . ?
C18A C19A 1.363(4) . ?
C18A H18A 0.9500 . ?
C19A C20A 1.407(5) . ?
C19A H19A 0.9500 . ?
C20A C21A 1.368(4) . ?
C20A H20A 0.9500 . ?
C21A C22A 1.415(4) . ?
C21A H21A 0.9500 . ?
O1B C1B 1.219(4) . ?
N1B C13B 1.388(4) . ?
N1B C2B 1.452(4) . ?
N1B H1B 0.88(2) . ?
C1B C5B 1.473(5) . ?
C1B C2B 1.550(4) . ?
C2B C3B 1.522(4) . ?
C2B H2B 1.012(16) . ?
C3B C12B 1.372(5) . ?
C3B C4B 1.409(4) . ?
C4B C9B 1.401(6) . ?
C4B C5B 1.406(5) . ?
C5B C6B 1.372(5) . ?
C6B C7B 1.413(5) . ?
C6B H6BA 0.9500 . ?
C7B C8B 1.380(5) . ?
C7B H7BA 0.9500 . ?
C8B C9B 1.422(5) . ?
C8B H8BA 0.9500 . ?
C9B C10B 1.423(5) . ?
C10B C11B 1.361(5) . ?
C10B H10B 0.9500 . ?
C11B C12B 1.422(5) . ?
C11B H11B 0.9500 . ?
C12B H12B 0.9500 . ?
C13B C14B 1.378(4) . ?
C13B C22B 1.438(4) . ?
C14B C15B 1.409(4) . ?
C14B H14B 0.9500 . ?
C15B C16B 1.356(5) . ?
C15B H15B 0.9500 . ?
C16B C17B 1.426(4) . ?
C16B H16B 0.9500 . ?
C17B C18B 1.415(4) . ?
C17B C22B 1.423(4) . ?
C18B C19B 1.365(4) . ?
C18B H18B 0.9500 . ?
C19B C20B 1.413(5) . ?
C19B H19B 0.9500 . ?
C20B C21B 1.370(4) . ?
C20B H20B 0.9500 . ?
C21B C22B 1.410(4) . ?
C21B H21B 0.9500 . ?
O1C C1C 1.228(4) . ?
N1C C13C 1.385(4) . ?
N1C C2C 1.450(4) . ?
N1C H1C 0.88(2) . ?
C1C C5C 1.471(5) . ?
C1C C2C 1.555(4) . ?
C2C C3C 1.514(5) . ?
C2C H2C 1.011(16) . ?
C3C C12C 1.363(5) . ?
C3C C4C 1.410(5) . ?
C4C C9C 1.408(6) . ?
C4C C5C 1.414(5) . ?
C5C C6C 1.370(5) . ?
C6C C7C 1.404(5) . ?
C6C H6CA 0.9500 . ?
C7C C8C 1.383(6) . ?
C7C H7CA 0.9500 . ?
C8C C9C 1.419(5) . ?
C8C H8CA 0.9500 . ?
C9C C10C 1.412(5) . ?
C10C C11C 1.377(5) . ?
C10C H10C 0.9500 . ?
C11C C12C 1.425(6) . ?
C11C H11C 0.9500 . ?
C12C H12C 0.9500 . ?
C13C C14C 1.378(4) . ?
C13C C22C 1.447(4) . ?
C14C C15C 1.400(5) . ?
C14C H14C 0.9500 . ?
C15C C16C 1.370(5) . ?
C15C H15C 0.9500 . ?
C16C C17C 1.414(4) . ?
C16C H16C 0.9500 . ?
C17C C18C 1.408(5) . ?
C17C C22C 1.425(4) . ?
C18C C19C 1.365(4) . ?
C18C H18C 0.9500 . ?
C19C C20C 1.410(5) . ?
C19C H19C 0.9500 . ?
C20C C21C 1.373(4) . ?
C20C H20C 0.9500 . ?
C21C C22C 1.412(4) . ?
C21C H21C 0.9500 . ?

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
C13A N1A C2A 123.2(3) . . ?
C13A N1A H1A 118(3) . . ?
C2A N1A H1A 117(2) . . ?
O1A C1A C5A 128.3(3) . . ?
O1A C1A C2A 123.5(3) . . ?
C5A C1A C2A 108.1(3) . . ?
N1A C2A C3A 115.4(3) . . ?
N1A C2A C1A 110.5(2) . . ?
C3A C2A C1A 102.8(2) . . ?
N1A C2A H2A 111.4(18) . . ?
C3A C2A H2A 110.4(19) . . ?
C1A C2A H2A 105.6(16) . . ?
C12A C3A C4A 118.9(3) . . ?
C12A C3A C2A 132.9(3) . . ?
C4A C3A C2A 108.2(3) . . ?
C5A C4A C9A 123.2(3) . . ?
C5A C4A C3A 113.6(3) . . ?
C9A C4A C3A 123.2(3) . . ?
C6A C5A C4A 120.4(3) . . ?
C6A C5A C1A 132.2(3) . . ?
C4A C5A C1A 107.2(3) . . ?
C5A C6A C7A 117.7(3) . . ?
C5A C6A H6AA 121.1 . . ?
C7A C6A H6AA 121.1 . . ?
C8A C7A C6A 122.0(3) . . ?
C8A C7A H7AA 119.0 . . ?
C6A C7A H7AA 119.0 . . ?
C7A C8A C9A 121.3(3) . . ?
C7A C8A H8AA 119.4 . . ?
C9A C8A H8AA 119.4 . . ?
C4A C9A C10A 116.9(3) . . ?
C4A C9A C8A 115.4(3) . . ?
C10A C9A C8A 127.7(4) . . ?
C11A C10A C9A 119.8(4) . . ?
C11A C10A H10A 120.1 . . ?
C9A C10A H10A 120.1 . . ?
C10A C11A C12A 122.7(3) . . ?
C10A C11A H11A 118.6 . . ?
C12A C11A H11A 118.6 . . ?
C3A C12A C11A 118.6(3) . . ?
C3A C12A H12A 120.7 . . ?
C11A C12A H12A 120.7 . . ?
C14A C13A N1A 122.4(3) . . ?
C14A C13A C22A 119.2(3) . . ?
N1A C13A C22A 118.3(3) . . ?
C13A C14A C15A 121.3(3) . . ?
C13A C14A H14A 119.3 . . ?
C15A C14A H14A 119.3 . . ?
C16A C15A C14A 120.8(3) . . ?
C16A C15A H15A 119.6 . . ?
C14A C15A H15A 119.6 . . ?
C15A C16A C17A 120.1(3) . . ?
C15A C16A H16A 120.0 . . ?
C17A C16A H16A 120.0 . . ?
C18A C17A C16A 121.4(3) . . ?
C18A C17A C22A 118.6(3) . . ?
C16A C17A C22A 120.0(3) . . ?
C19A C18A C17A 121.6(3) . . ?
C19A C18A H18A 119.2 . . ?
C17A C18A H18A 119.2 . . ?
C18A C19A C20A 119.5(3) . . ?
C18A C19A H19A 120.3 . . ?
C20A C19A H19A 120.3 . . ?
C21A C20A C19A 120.8(3) . . ?
C21A C20A H20A 119.6 . . ?
C19A C20A H20A 119.6 . . ?
C20A C21A C22A 121.1(3) . . ?
C20A C21A H21A 119.5 . . ?
C22A C21A H21A 119.5 . . ?
C21A C22A C17A 118.5(3) . . ?
C21A C22A C13A 123.1(3) . . ?
C17A C22A C13A 118.4(3) . . ?
C13B N1B C2B 121.9(2) . . ?
C13B N1B H1B 116(3) . . ?
C2B N1B H1B 116(2) . . ?
O1B C1B C5B 128.6(3) . . ?
O1B C1B C2B 122.9(3) . . ?
C5B C1B C2B 108.4(3) . . ?
N1B C2B C3B 116.8(3) . . ?
N1B C2B C1B 110.1(2) . . ?
C3B C2B C1B 102.7(2) . . ?
N1B C2B H2B 111.7(18) . . ?
C3B C2B H2B 107.6(18) . . ?
C1B C2B H2B 107.3(16) . . ?
C12B C3B C4B 118.5(3) . . ?
C12B C3B C2B 133.3(3) . . ?
C4B C3B C2B 108.2(3) . . ?
C9B C4B C5B 122.7(3) . . ?
C9B C4B C3B 123.7(3) . . ?
C5B C4B C3B 113.6(3) . . ?
C6B C5B C4B 120.6(3) . . ?
C6B C5B C1B 132.5(3) . . ?
C4B C5B C1B 106.8(3) . . ?
C5B C6B C7B 117.7(3) . . ?
C5B C6B H6BA 121.1 . . ?
C7B C6B H6BA 121.1 . . ?
C8B C7B C6B 122.2(3) . . ?
C8B C7B H7BA 118.9 . . ?
C6B C7B H7BA 118.9 . . ?
C7B C8B C9B 120.9(3) . . ?
C7B C8B H8BA 119.6 . . ?
C9B C8B H8BA 119.6 . . ?
C4B C9B C8B 116.0(3) . . ?
C4B C9B C10B 116.4(3) . . ?
C8B C9B C10B 127.6(3) . . ?
C11B C10B C9B 120.0(3) . . ?
C11B C10B H10B 120.0 . . ?
C9B C10B H10B 120.0 . . ?
C10B C11B C12B 122.7(3) . . ?
C10B C11B H11B 118.7 . . ?
C12B C11B H11B 118.7 . . ?
C3B C12B C11B 118.7(3) . . ?
C3B C12B H12B 120.6 . . ?
C11B C12B H12B 120.6 . . ?
C14B C13B N1B 122.0(3) . . ?
C14B C13B C22B 119.7(3) . . ?
N1B C13B C22B 118.3(3) . . ?
C13B C14B C15B 120.7(3) . . ?
C13B C14B H14B 119.7 . . ?
C15B C14B H14B 119.7 . . ?
C16B C15B C14B 121.3(3) . . ?
C16B C15B H15B 119.4 . . ?
C14B C15B H15B 119.4 . . ?
C15B C16B C17B 120.0(3) . . ?
C15B C16B H16B 120.0 . . ?
C17B C16B H16B 120.0 . . ?
C18B C17B C22B 119.0(3) . . ?
C18B C17B C16B 121.3(3) . . ?
C22B C17B C16B 119.7(3) . . ?
C19B C18B C17B 121.4(3) . . ?
C19B C18B H18B 119.3 . . ?
C17B C18B H18B 119.3 . . ?
C18B C19B C20B 119.6(3) . . ?
C18B C19B H19B 120.2 . . ?
C20B C19B H19B 120.2 . . ?
C21B C20B C19B 120.3(3) . . ?
C21B C20B H20B 119.8 . . ?
C19B C20B H20B 119.8 . . ?
C20B C21B C22B 121.3(3) . . ?
C20B C21B H21B 119.4 . . ?
C22B C21B H21B 119.4 . . ?
C21B C22B C17B 118.4(3) . . ?
C21B C22B C13B 123.1(3) . . ?
C17B C22B C13B 118.5(3) . . ?
C13C N1C C2C 122.1(3) . . ?
C13C N1C H1C 115(3) . . ?
C2C N1C H1C 118(2) . . ?
O1C C1C C5C 128.5(3) . . ?
O1C C1C C2C 123.0(3) . . ?
C5C C1C C2C 108.5(3) . . ?
N1C C2C C3C 116.2(3) . . ?
N1C C2C C1C 110.0(3) . . ?
C3C C2C C1C 102.8(3) . . ?
N1C C2C H2C 109.4(19) . . ?
C3C C2C H2C 112(2) . . ?
C1C C2C H2C 105.5(17) . . ?
C12C C3C C4C 118.1(3) . . ?
C12C C3C C2C 133.4(3) . . ?
C4C C3C C2C 108.5(3) . . ?
C9C C4C C3C 124.1(3) . . ?
C9C C4C C5C 122.5(3) . . ?
C3C C4C C5C 113.4(3) . . ?
C6C C5C C4C 120.2(4) . . ?
C6C C5C C1C 133.1(3) . . ?
C4C C5C C1C 106.6(3) . . ?
C5C C6C C7C 118.8(4) . . ?
C5C C6C H6CA 120.6 . . ?
C7C C6C H6CA 120.6 . . ?
C8C C7C C6C 121.1(4) . . ?
C8C C7C H7CA 119.5 . . ?
C6C C7C H7CA 119.5 . . ?
C7C C8C C9C 122.0(4) . . ?
C7C C8C H8CA 119.0 . . ?
C9C C8C H8CA 119.0 . . ?
C4C C9C C10C 116.0(3) . . ?
C4C C9C C8C 115.5(3) . . ?
C10C C9C C8C 128.5(4) . . ?
C11C C10C C9C 120.5(4) . . ?
C11C C10C H10C 119.8 . . ?
C9C C10C H10C 119.8 . . ?
C10C C11C C12C 121.7(3) . . ?
C10C C11C H11C 119.1 . . ?
C12C C11C H11C 119.1 . . ?
C3C C12C C11C 119.5(3) . . ?
C3C C12C H12C 120.2 . . ?
C11C C12C H12C 120.2 . . ?
C14C C13C N1C 122.5(3) . . ?
C14C C13C C22C 119.1(3) . . ?
N1C C13C C22C 118.3(3) . . ?
C13C C14C C15C 121.3(3) . . ?
C13C C14C H14C 119.4 . . ?
C15C C14C H14C 119.4 . . ?
C16C C15C C14C 121.2(3) . . ?
C16C C15C H15C 119.4 . . ?
C14C C15C H15C 119.4 . . ?
C15C C16C C17C 119.6(3) . . ?
C15C C16C H16C 120.2 . . ?
C17C C16C H16C 120.2 . . ?
C18C C17C C16C 121.5(3) . . ?
C18C C17C C22C 118.3(3) . . ?
C16C C17C C22C 120.2(3) . . ?
C19C C18C C17C 122.0(3) . . ?
C19C C18C H18C 119.0 . . ?
C17C C18C H18C 119.0 . . ?
C18C C19C C20C 119.7(3) . . ?
C18C C19C H19C 120.2 . . ?
C20C C19C H19C 120.2 . . ?
C21C C20C C19C 120.2(3) . . ?
C21C C20C H20C 119.9 . . ?
C19C C20C H20C 119.9 . . ?
C20C C21C C22C 121.0(3) . . ?
C20C C21C H21C 119.5 . . ?
C22C C21C H21C 119.5 . . ?
C21C C22C C17C 118.9(3) . . ?
C21C C22C C13C 122.7(3) . . ?
C17C C22C C13C 118.3(3) . . ?

_refine_diff_density_max         0.352
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.056

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_C24H26ClNO
_database_code_depnum_ccdc_archive 'CCDC 2395056'
loop_
_audit_author_name
_audit_author_address
'Anton Cherkasov'
;IOMC RAS
Russia
;
_audit_update_record             
;
2024-10-30 deposited with the CCDC.	2025-02-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H26 Cl N O'
_chemical_formula_sum            'C24 H26 Cl N O'
_chemical_formula_weight         379.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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'

_cell_length_a                   14.4234(7)
_cell_length_b                   10.4958(4)
_cell_length_c                   14.8391(7)
_cell_angle_alpha                90
_cell_angle_beta                 110.630(5)
_cell_angle_gamma                90
_cell_volume                     2102.37(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5174
_cell_measurement_theta_min      3.5760
_cell_measurement_theta_max      25.3980

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_F_000             808
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    0.195
_shelx_estimated_absorpt_T_min   0.944
_shelx_estimated_absorpt_T_max   0.983
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.925
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CAP 38.46'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine focus sealed tube'
_diffrn_measurement_device_type  'Rigaku OD Xcalibur E'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24215
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.934
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_full        25.026
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3713
_reflns_number_gt                2820
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CAP 38.46'
_computing_cell_refinement       'CAP 38.46'
_computing_data_reduction        'CAP 38.46'
_computing_structure_solution    'SHELXT 2018/2'
_computing_structure_refinement  'SHELXL 2018/3'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0499P)²+2.4059P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3713
_refine_ls_number_parameters     347
_refine_ls_number_restraints     489
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0501
_refine_ls_wR_factor_ref         0.1259
_refine_ls_wR_factor_gt          0.1130
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.68021(13) 0.65417(18) 0.46566(13) 0.0335(5) Uani 1 1 d . . . . .
H1A H 0.684(2) 0.580(3) 0.493(2) 0.058(10) Uiso 1 1 d . . . . .
N1 N 0.53449(14) 0.49317(17) 0.32271(14) 0.0215(4) Uani 1 1 d D . . . .
H1B H 0.566(2) 0.444(3) 0.386(2) 0.045(8) Uiso 1 1 d . . . . .
C1 C 0.53093(16) 0.6168(2) 0.32630(16) 0.0198(5) Uani 1 1 d . . . . .
C2 C 0.57852(18) 0.6852(2) 0.42345(17) 0.0246(6) Uani 1 1 d . . . . .
H2A H 0.5432(18) 0.662(2) 0.4687(18) 0.021(6) Uiso 1 1 d . . . . .
C3 C 0.56387(18) 0.8231(2) 0.39357(18) 0.0261(6) Uani 1 1 d . . . . .
C4 C 0.51378(17) 0.8300(2) 0.29416(17) 0.0224(5) Uani 1 1 d . . . . .
C5 C 0.49056(16) 0.7091(2) 0.24930(17) 0.0209(5) Uani 1 1 d . . . . .
C6 C 0.43803(17) 0.7023(2) 0.15130(17) 0.0259(6) Uani 1 1 d . . . . .
H6A H 0.421380 0.622499 0.119483 0.031 Uiso 1 1 calc R U . . .
C7 C 0.41029(19) 0.8168(3) 0.10068(18) 0.0307(6) Uani 1 1 d . . . . .
H7A H 0.373276 0.813291 0.033611 0.037 Uiso 1 1 calc R U . . .
C8 C 0.43421(19) 0.9342(3) 0.14371(19) 0.0312(6) Uani 1 1 d . . . . .
H8A H 0.414275 1.009088 0.105807 0.037 Uiso 1 1 calc R U . . .
C9 C 0.48807(19) 0.9452(2) 0.24359(18) 0.0269(6) Uani 1 1 d . . . . .
C10 C 0.5167(2) 1.0584(2) 0.2985(2) 0.0343(6) Uani 1 1 d . . . . .
H10A H 0.502711 1.139114 0.267632 0.041 Uiso 1 1 calc R U . . .
C11 C 0.5646(2) 1.0513(3) 0.3960(2) 0.0410(7) Uani 1 1 d . . . . .
H11A H 0.582816 1.128031 0.431861 0.049 Uiso 1 1 calc R U . . .
C12 C 0.5881(2) 0.9331(3) 0.4452(2) 0.0384(7) Uani 1 1 d . . . . .
H12A H 0.620130 0.930724 0.513172 0.046 Uiso 1 1 calc R U . . .
C13 C 0.4979(2) 0.42464(17) 0.23360(15) 0.0197(11) Uani 0.713(7) 1 d DG U P A 1
C14 C 0.5586(2) 0.4053(3) 0.1800(3) 0.0366(9) Uani 0.713(7) 1 d DG U P A 1
C15 C 0.5230(3) 0.3393(4) 0.0934(3) 0.0452(14) Uani 0.713(7) 1 d G U P A 1
H15A H 0.564532 0.326038 0.056751 0.054 Uiso 0.713(7) 1 calc R U P A 1
C16 C 0.4266(4) 0.2927(3) 0.0603(2) 0.0360(13) Uani 0.713(7) 1 d G U P A 1
H16A H 0.402270 0.247577 0.001021 0.043 Uiso 0.713(7) 1 calc R U P A 1
C17 C 0.3659(2) 0.3121(3) 0.1138(2) 0.0279(12) Uani 0.713(7) 1 d G U P A 1
H17A H 0.299983 0.280196 0.091198 0.033 Uiso 0.713(7) 1 calc R U P A 1
C18 C 0.4015(2) 0.3780(2) 0.2005(2) 0.0135(10) Uani 0.713(7) 1 d DG U P A 1
C19 C 0.6651(4) 0.4547(6) 0.2142(5) 0.0540(16) Uani 0.713(7) 1 d D U P A 1
H19A H 0.665610 0.539194 0.245477 0.065 Uiso 0.713(7) 1 calc R U P A 1
C20 C 0.7084(4) 0.4745(6) 0.1360(4) 0.0622(17) Uani 0.713(7) 1 d D U P A 1
H20A H 0.773026 0.516347 0.163349 0.093 Uiso 0.713(7) 1 calc R U P A 1
H20B H 0.663671 0.528178 0.085089 0.093 Uiso 0.713(7) 1 calc R U P A 1
H20C H 0.716426 0.391875 0.108911 0.093 Uiso 0.713(7) 1 calc R U P A 1
C21 C 0.7314(5) 0.3649(8) 0.2917(4) 0.0724(19) Uani 0.713(7) 1 d D U P A 1
H21A H 0.799306 0.398022 0.315662 0.109 Uiso 0.713(7) 1 calc R U P A 1
H21B H 0.730962 0.280038 0.263943 0.109 Uiso 0.713(7) 1 calc R U P A 1
H21C H 0.706433 0.359153 0.344993 0.109 Uiso 0.713(7) 1 calc R U P A 1
C22 C 0.3335(4) 0.3960(5) 0.2586(5) 0.0226(12) Uani 0.713(7) 1 d D U P A 1
H22A H 0.364442 0.455039 0.313993 0.027 Uiso 0.713(7) 1 calc R U P A 1
C23 C 0.3080(4) 0.2706(4) 0.2934(3) 0.0365(12) Uani 0.713(7) 1 d D U P A 1
H23A H 0.368827 0.228978 0.335044 0.055 Uiso 0.713(7) 1 calc R U P A 1
H23B H 0.274629 0.215709 0.237976 0.055 Uiso 0.713(7) 1 calc R U P A 1
H23C H 0.263968 0.285458 0.329733 0.055 Uiso 0.713(7) 1 calc R U P A 1
C24 C 0.2389(4) 0.4566(6) 0.1851(5) 0.0657(19) Uani 0.713(7) 1 d D U P A 1
H24A H 0.257540 0.527977 0.152455 0.099 Uiso 0.713(7) 1 calc R U P A 1
H24B H 0.195968 0.487563 0.218985 0.099 Uiso 0.713(7) 1 calc R U P A 1
H24C H 0.203279 0.392503 0.137431 0.099 Uiso 0.713(7) 1 calc R U P A 1
C13* C 0.5088(6) 0.4157(4) 0.2404(4) 0.030(3) Uani 0.287(7) 1 d DG U P A 2
C14* C 0.5809(5) 0.3820(6) 0.2026(5) 0.0366(9) Uani 0.287(7) 1 d DG U P A 2
C15* C 0.5563(6) 0.3058(8) 0.1210(5) 0.030(3) Uani 0.287(7) 1 d G U P A 2
H15B H 0.605579 0.282788 0.095164 0.036 Uiso 0.287(7) 1 calc R U P A 2
C16* C 0.4595(6) 0.2631(8) 0.0771(5) 0.028(3) Uani 0.287(7) 1 d G U P A 2
H16B H 0.442682 0.210922 0.021341 0.034 Uiso 0.287(7) 1 calc R U P A 2
C17* C 0.3874(5) 0.2967(8) 0.1149(6) 0.025(3) Uani 0.287(7) 1 d G U P A 2
H17B H 0.321275 0.267493 0.084971 0.030 Uiso 0.287(7) 1 calc R U P A 2
C18* C 0.4121(5) 0.3730(6) 0.1966(6) 0.044(4) Uani 0.287(7) 1 d DG U P A 2
C19* C 0.6866(7) 0.4276(9) 0.2526(9) 0.031(3) Uani 0.287(7) 1 d D U P A 2
H19B H 0.690944 0.467289 0.315176 0.037 Uiso 0.287(7) 1 calc R U P A 2
C20* C 0.7200(11) 0.5243(12) 0.1965(13) 0.076(4) Uani 0.287(7) 1 d D U P A 2
H20D H 0.772228 0.577258 0.240913 0.114 Uiso 0.287(7) 1 calc R U P A 2
H20E H 0.663825 0.578234 0.160127 0.114 Uiso 0.287(7) 1 calc R U P A 2
H20F H 0.745811 0.480808 0.151871 0.114 Uiso 0.287(7) 1 calc R U P A 2
C21* C 0.7561(9) 0.3106(9) 0.2750(9) 0.040(3) Uani 0.287(7) 1 d D U P A 2
H21D H 0.734827 0.249449 0.313763 0.060 Uiso 0.287(7) 1 calc R U P A 2
H21E H 0.824148 0.337904 0.310968 0.060 Uiso 0.287(7) 1 calc R U P A 2
H21F H 0.753477 0.270128 0.214656 0.060 Uiso 0.287(7) 1 calc R U P A 2
C22* C 0.3327(10) 0.4073(14) 0.2403(12) 0.039(4) Uani 0.287(7) 1 d D U P A 2
H22B H 0.351897 0.492717 0.271145 0.047 Uiso 0.287(7) 1 calc R U P A 2
C23* C 0.3527(10) 0.3079(13) 0.3268(9) 0.052(3) Uani 0.287(7) 1 d D U P A 2
H23D H 0.419930 0.319986 0.373214 0.077 Uiso 0.287(7) 1 calc R U P A 2
H23E H 0.345769 0.220876 0.301281 0.077 Uiso 0.287(7) 1 calc R U P A 2
H23F H 0.304635 0.321854 0.358815 0.077 Uiso 0.287(7) 1 calc R U P A 2
C24* C 0.2188(9) 0.4091(15) 0.1932(10) 0.052(4) Uani 0.287(7) 1 d D U P A 2
H24D H 0.199501 0.461383 0.134751 0.078 Uiso 0.287(7) 1 calc R U P A 2
H24E H 0.190117 0.444983 0.238417 0.078 Uiso 0.287(7) 1 calc R U P A 2
H24F H 0.194468 0.321912 0.176365 0.078 Uiso 0.287(7) 1 calc R U P A 2
Cl1 Cl 0.63943(5) 0.38132(6) 0.52031(4) 0.02984(19) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 C2 1.415(3) . ?
O1 H1A 0.87(4) . ?
N1 C1 1.301(3) . ?
N1 C13* 1.404(6) . ?
N1 C13 1.433(3) . ?
N1 H1B 1.03(3) . ?
C1 C5 1.454(3) . ?
C1 C2 1.538(3) . ?
C2 C3 1.507(3) . ?
C2 H2A 1.01(3) . ?
C3 C12 1.361(4) . ?
C3 C4 1.397(3) . ?
C4 C9 1.402(3) . ?
C4 C5 1.417(3) . ?
C5 C6 1.385(3) . ?
C6 C7 1.399(4) . ?
C6 H6A 0.9500 . ?
C7 C8 1.375(4) . ?
C7 H7A 0.9500 . ?
C8 C9 1.415(4) . ?
C8 H8A 0.9500 . ?
C9 C10 1.417(4) . ?
C10 C11 1.368(4) . ?
C10 H10A 0.9500 . ?
C11 C12 1.419(4) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9500 . ?
C13 C14 1.3900 . ?
C13 C18 1.3900 . ?
C14 C15 1.3900 . ?
C14 C19 1.529(5) . ?
C15 C16 1.3900 . ?
C15 H15A 0.9500 . ?
C16 C17 1.3900 . ?
C16 H16A 0.9500 . ?
C17 C18 1.3900 . ?
C17 H17A 0.9500 . ?
C18 C22 1.528(4) . ?
C19 C20 1.513(6) . ?
C19 C21 1.533(6) . ?
C19 H19A 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.507(6) . ?
C22 C24 1.552(6) . ?
C22 H22A 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C13* C14* 1.3900 . ?
C13* C18* 1.3900 . ?
C14* C15* 1.3900 . ?
C14* C19* 1.519(9) . ?
C15* C16* 1.3900 . ?
C15* H15B 0.9500 . ?
C16* C17* 1.3900 . ?
C16* H16B 0.9500 . ?
C17* C18* 1.3900 . ?
C17* H17B 0.9500 . ?
C18* C22* 1.544(10) . ?
C19* C20* 1.495(9) . ?
C19* C21* 1.546(9) . ?
C19* H19B 1.0000 . ?
C20* H20D 0.9800 . ?
C20* H20E 0.9800 . ?
C20* H20F 0.9800 . ?
C21* H21D 0.9800 . ?
C21* H21E 0.9800 . ?
C21* H21F 0.9800 . ?
C22* C24* 1.543(10) . ?
C22* C23* 1.599(9) . ?
C22* H22B 1.0000 . ?
C23* H23D 0.9800 . ?
C23* H23E 0.9800 . ?
C23* H23F 0.9800 . ?
C24* H24D 0.9800 . ?
C24* H24E 0.9800 . ?
C24* H24F 0.9800 . ?

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
C2 O1 H1A 108(2) . . ?
C1 N1 C13* 127.7(2) . . ?
C1 N1 C13 122.12(17) . . ?
C1 N1 H1B 118.3(17) . . ?
C13* N1 H1B 113.7(17) . . ?
C13 N1 H1B 119.6(17) . . ?
N1 C1 C5 130.0(2) . . ?
N1 C1 C2 119.5(2) . . ?
C5 C1 C2 110.40(19) . . ?
O1 C2 C3 111.5(2) . . ?
O1 C2 C1 111.0(2) . . ?
C3 C2 C1 101.66(19) . . ?
O1 C2 H2A 109.8(14) . . ?
C3 C2 H2A 112.3(14) . . ?
C1 C2 H2A 110.3(14) . . ?
C12 C3 C4 119.0(2) . . ?
C12 C3 C2 131.9(2) . . ?
C4 C3 C2 109.1(2) . . ?
C3 C4 C9 123.4(2) . . ?
C3 C4 C5 113.5(2) . . ?
C9 C4 C5 123.1(2) . . ?
C6 C5 C4 119.4(2) . . ?
C6 C5 C1 135.2(2) . . ?
C4 C5 C1 105.3(2) . . ?
C5 C6 C7 117.8(2) . . ?
C5 C6 H6A 121.1 . . ?
C7 C6 H6A 121.1 . . ?
C8 C7 C6 122.9(2) . . ?
C8 C7 H7A 118.5 . . ?
C6 C7 H7A 118.5 . . ?
C7 C8 C9 121.0(2) . . ?
C7 C8 H8A 119.5 . . ?
C9 C8 H8A 119.5 . . ?
C4 C9 C8 115.7(2) . . ?
C4 C9 C10 116.5(2) . . ?
C8 C9 C10 127.7(2) . . ?
C11 C10 C9 119.9(2) . . ?
C11 C10 H10A 120.0 . . ?
C9 C10 H10A 120.0 . . ?
C10 C11 C12 122.2(3) . . ?
C10 C11 H11A 118.9 . . ?
C12 C11 H11A 118.9 . . ?
C3 C12 C11 118.9(2) . . ?
C3 C12 H12A 120.5 . . ?
C11 C12 H12A 120.5 . . ?
C14 C13 C18 120.0 . . ?
C14 C13 N1 120.0(2) . . ?
C18 C13 N1 120.0(2) . . ?
C13 C14 C15 120.0 . . ?
C13 C14 C19 121.5(3) . . ?
C15 C14 C19 118.5(3) . . ?
C16 C15 C14 120.0 . . ?
C16 C15 H15A 120.0 . . ?
C14 C15 H15A 120.0 . . ?
C15 C16 C17 120.0 . . ?
C15 C16 H16A 120.0 . . ?
C17 C16 H16A 120.0 . . ?
C18 C17 C16 120.0 . . ?
C18 C17 H17A 120.0 . . ?
C16 C17 H17A 120.0 . . ?
C17 C18 C13 120.0 . . ?
C17 C18 C22 118.8(3) . . ?
C13 C18 C22 121.2(3) . . ?
C20 C19 C14 115.5(4) . . ?
C20 C19 C21 110.1(4) . . ?
C14 C19 C21 109.2(4) . . ?
C20 C19 H19A 107.3 . . ?
C14 C19 H19A 107.3 . . ?
C21 C19 H19A 107.3 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C18 111.6(4) . . ?
C23 C22 C24 109.8(5) . . ?
C18 C22 C24 103.6(4) . . ?
C23 C22 H22A 110.6 . . ?
C18 C22 H22A 110.6 . . ?
C24 C22 H22A 110.6 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C14* C13* C18* 120.0 . . ?
C14* C13* N1 119.5(5) . . ?
C18* C13* N1 120.5(5) . . ?
C15* C14* C13* 120.0 . . ?
C15* C14* C19* 120.7(6) . . ?
C13* C14* C19* 119.3(6) . . ?
C14* C15* C16* 120.0 . . ?
C14* C15* H15B 120.0 . . ?
C16* C15* H15B 120.0 . . ?
C15* C16* C17* 120.0 . . ?
C15* C16* H16B 120.0 . . ?
C17* C16* H16B 120.0 . . ?
C18* C17* C16* 120.0 . . ?
C18* C17* H17B 120.0 . . ?
C16* C17* H17B 120.0 . . ?
C17* C18* C13* 120.0 . . ?
C17* C18* C22* 120.1(9) . . ?
C13* C18* C22* 119.9(9) . . ?
C20* C19* C14* 114.0(8) . . ?
C20* C19* C21* 110.4(8) . . ?
C14* C19* C21* 108.6(7) . . ?
C20* C19* H19B 107.9 . . ?
C14* C19* H19B 107.9 . . ?
C21* C19* H19B 107.9 . . ?
C19* C20* H20D 109.5 . . ?
C19* C20* H20E 109.5 . . ?
H20D C20* H20E 109.5 . . ?
C19* C20* H20F 109.5 . . ?
H20D C20* H20F 109.5 . . ?
H20E C20* H20F 109.5 . . ?
C19* C21* H21D 109.5 . . ?
C19* C21* H21E 109.5 . . ?
H21D C21* H21E 109.5 . . ?
C19* C21* H21F 109.5 . . ?
H21D C21* H21F 109.5 . . ?
H21E C21* H21F 109.5 . . ?
C24* C22* C18* 129.9(14) . . ?
C24* C22* C23* 103.5(8) . . ?
C18* C22* C23* 103.5(7) . . ?
C24* C22* H22B 106.0 . . ?
C18* C22* H22B 106.0 . . ?
C23* C22* H22B 106.0 . . ?
C22* C23* H23D 109.5 . . ?
C22* C23* H23E 109.5 . . ?
H23D C23* H23E 109.5 . . ?
C22* C23* H23F 109.5 . . ?
H23D C23* H23F 109.5 . . ?
H23E C23* H23F 109.5 . . ?
C22* C24* H24D 109.5 . . ?
C22* C24* H24E 109.5 . . ?
H24D C24* H24E 109.5 . . ?
C22* C24* H24F 109.5 . . ?
H24D C24* H24F 109.5 . . ?
H24E C24* H24F 109.5 . . ?

_refine_diff_density_max         0.625
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.053

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mianhbf4
_database_code_depnum_ccdc_archive 'CCDC 2395057'
loop_
_audit_author_name
_audit_author_address
'Anton Cherkasov'
;IOMC RAS
Russia
;
_audit_update_record             
;
2024-10-30 deposited with the CCDC.	2025-02-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H26 B F4 N O'
_chemical_formula_sum            'C24 H26 B F4 N O'
_chemical_formula_weight         431.27

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   15.9889(10)
_cell_length_b                   14.0339(9)
_cell_length_c                   19.2410(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4317.4(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4974
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      29.82

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_F_000             1808
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.103
_shelx_estimated_absorpt_T_min   0.986
_shelx_estimated_absorpt_T_max   0.997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.473
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus source'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18653
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.471
_diffrn_reflns_theta_max         26.018
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             4232
_reflns_number_gt                2878
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       APEX2
_computing_cell_refinement       'Saint 8.37a'
_computing_data_reduction        'Saint 8.37a'
_computing_structure_solution    'SHELXT 2018/2'
_computing_structure_refinement  'SHELXL 2018/3'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0995P)²+3.8625P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL 2018/3'
_refine_ls_extinction_coef       0.0053(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4232
_refine_ls_number_parameters     296
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0710
_refine_ls_wR_factor_ref         0.2049
_refine_ls_wR_factor_gt          0.1825
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.55680(12) 0.41269(16) 0.55048(12) 0.0251(5) Uani 1 1 d . . . . .
N1 N 0.44749(15) 0.3848(2) 0.43384(13) 0.0193(6) Uani 1 1 d . . . . .
H1A H 0.504(2) 0.380(2) 0.4300(18) 0.027(9) Uiso 1 1 d . . . . .
H1B H 0.438(2) 0.450(3) 0.4238(18) 0.026(9) Uiso 1 1 d . . . . .
C1 C 0.49807(18) 0.3576(2) 0.55572(16) 0.0221(7) Uani 1 1 d . . . . .
C2 C 0.41931(18) 0.3645(2) 0.50791(16) 0.0208(7) Uani 1 1 d . . . . .
H2A H 0.386(2) 0.418(3) 0.5218(17) 0.025 Uiso 1 1 d . U . . .
C3 C 0.37273(18) 0.2728(2) 0.52191(17) 0.0244(7) Uani 1 1 d . . . . .
C4 C 0.41342(18) 0.2276(2) 0.57781(17) 0.0228(7) Uani 1 1 d . . . . .
C5 C 0.48718(18) 0.2739(2) 0.59990(16) 0.0231(7) Uani 1 1 d . . . . .
C6 C 0.5334(2) 0.2378(2) 0.65453(17) 0.0286(8) Uani 1 1 d . . . . .
H6A H 0.583185 0.268331 0.669652 0.034 Uiso 1 1 calc R U . . .
C7 C 0.5045(2) 0.1545(3) 0.68701(18) 0.0324(8) Uani 1 1 d . . . . .
H7A H 0.535540 0.128772 0.724666 0.039 Uiso 1 1 calc R U . . .
C8 C 0.4325(2) 0.1089(2) 0.66607(18) 0.0310(8) Uani 1 1 d . . . . .
H8A H 0.414743 0.053155 0.689833 0.037 Uiso 1 1 calc R U . . .
C9 C 0.3843(2) 0.1439(2) 0.60954(17) 0.0269(7) Uani 1 1 d . . . . .
C10 C 0.3100(2) 0.1041(3) 0.58182(19) 0.0336(8) Uani 1 1 d . . . . .
H10A H 0.287657 0.047176 0.601059 0.040 Uiso 1 1 calc R U . . .
C11 C 0.2702(2) 0.1480(3) 0.52684(19) 0.0350(9) Uani 1 1 d . . . . .
H11A H 0.220834 0.120014 0.508544 0.042 Uiso 1 1 calc R U . . .
C12 C 0.30059(19) 0.2336(3) 0.49668(18) 0.0292(8) Uani 1 1 d . . . . .
H12A H 0.271235 0.263176 0.459564 0.035 Uiso 1 1 calc R U . . .
C13 C 0.40871(17) 0.3267(2) 0.37852(16) 0.0206(7) Uani 1 1 d . . . . .
C14 C 0.33504(17) 0.3623(2) 0.34835(16) 0.0233(7) Uani 1 1 d . . . . .
C15 C 0.30018(19) 0.3078(2) 0.29488(16) 0.0253(7) Uani 1 1 d . . . . .
H15A H 0.250748 0.329323 0.272422 0.030 Uiso 1 1 calc R U . . .
C16 C 0.33657(19) 0.2233(2) 0.27427(17) 0.0280(8) Uani 1 1 d . . . . .
H16A H 0.312347 0.187882 0.237313 0.034 Uiso 1 1 calc R U . . .
C17 C 0.40793(19) 0.1893(2) 0.30672(17) 0.0280(8) Uani 1 1 d . . . . .
H17A H 0.431275 0.130220 0.292375 0.034 Uiso 1 1 calc R U . . .
C18 C 0.44614(18) 0.2408(2) 0.36040(16) 0.0227(7) Uani 1 1 d . . . . .
C19 C 0.29534(18) 0.4561(2) 0.37019(17) 0.0254(7) Uani 1 1 d . . . . .
H19A H 0.320783 0.475130 0.415603 0.030 Uiso 1 1 calc R U . . .
C20 C 0.20041(19) 0.4477(3) 0.38117(19) 0.0326(8) Uani 1 1 d . . . . .
H20A H 0.188882 0.397435 0.415232 0.049 Uiso 1 1 calc R U . . .
H20B H 0.173409 0.431700 0.336952 0.049 Uiso 1 1 calc R U . . .
H20C H 0.178406 0.508449 0.398327 0.049 Uiso 1 1 calc R U . . .
C21 C 0.3149(2) 0.5344(3) 0.31786(18) 0.0310(8) Uani 1 1 d . . . . .
H21A H 0.375611 0.540669 0.312819 0.047 Uiso 1 1 calc R U . . .
H21B H 0.291431 0.594892 0.334275 0.047 Uiso 1 1 calc R U . . .
H21C H 0.290130 0.518077 0.272813 0.047 Uiso 1 1 calc R U . . .
C22 C 0.52345(19) 0.1996(2) 0.39607(18) 0.0276(7) Uani 1 1 d . . . . .
H22A H 0.540355 0.244896 0.433659 0.033 Uiso 1 1 calc R U . . .
C23 C 0.5039(2) 0.1035(3) 0.4304(2) 0.0334(8) Uani 1 1 d . . . . .
H23A H 0.456455 0.110846 0.462182 0.050 Uiso 1 1 calc R U . . .
H23B H 0.552908 0.081448 0.456359 0.050 Uiso 1 1 calc R U . . .
H23C H 0.489737 0.056642 0.394433 0.050 Uiso 1 1 calc R U . . .
C24 C 0.5972(2) 0.1906(3) 0.3455(2) 0.0372(9) Uani 1 1 d . . . . .
H24A H 0.611085 0.253562 0.326760 0.056 Uiso 1 1 calc R U . . .
H24B H 0.581856 0.147797 0.307346 0.056 Uiso 1 1 calc R U . . .
H24C H 0.645787 0.164668 0.370147 0.056 Uiso 1 1 calc R U . . .
B1 B 0.6163(2) 0.4843(3) 0.34083(19) 0.0250(8) Uani 1 1 d . . . . .
F1 F 0.53540(11) 0.50764(15) 0.31952(10) 0.0362(5) Uani 1 1 d . . . . .
F2 F 0.66129(12) 0.56445(15) 0.35743(10) 0.0366(5) Uani 1 1 d . . . . .
F3 F 0.60869(11) 0.42700(15) 0.40122(10) 0.0318(5) Uani 1 1 d . . . . .
F4 F 0.65621(11) 0.43233(16) 0.29004(10) 0.0366(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 C1 1.221(4) . ?
N1 C13 1.478(4) . ?
N1 C2 1.522(4) . ?
N1 H1A 0.90(4) . ?
N1 H1B 0.95(4) . ?
C1 C5 1.460(4) . ?
C1 C2 1.563(4) . ?
C2 C3 1.511(4) . ?
C2 H2A 0.96(4) . ?
C3 C12 1.367(4) . ?
C3 C4 1.408(5) . ?
C4 C9 1.403(5) . ?
C4 C5 1.412(4) . ?
C5 C6 1.381(5) . ?
C6 C7 1.403(5) . ?
C6 H6A 0.9500 . ?
C7 C8 1.377(5) . ?
C7 H7A 0.9500 . ?
C8 C9 1.420(5) . ?
C8 H8A 0.9500 . ?
C9 C10 1.417(5) . ?
C10 C11 1.380(5) . ?
C10 H10A 0.9500 . ?
C11 C12 1.420(5) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9500 . ?
C13 C18 1.390(4) . ?
C13 C14 1.405(4) . ?
C14 C15 1.398(4) . ?
C14 C19 1.521(5) . ?
C15 C16 1.380(5) . ?
C15 H15A 0.9500 . ?
C16 C17 1.385(5) . ?
C16 H16A 0.9500 . ?
C17 C18 1.401(5) . ?
C17 H17A 0.9500 . ?
C18 C22 1.527(4) . ?
C19 C21 1.522(5) . ?
C19 C20 1.537(4) . ?
C19 H19A 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C24 1.534(5) . ?
C22 C23 1.534(5) . ?
C22 H22A 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
B1 F2 1.372(4) . ?
B1 F4 1.377(4) . ?
B1 F1 1.396(4) . ?
B1 F3 1.419(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
C13 N1 C2 116.5(2) . . ?
C13 N1 H1A 109(2) . . ?
C2 N1 H1A 111(2) . . ?
C13 N1 H1B 109(2) . . ?
C2 N1 H1B 109(2) . . ?
H1A N1 H1B 102(3) . . ?
O1 C1 C5 130.5(3) . . ?
O1 C1 C2 122.1(3) . . ?
C5 C1 C2 107.3(2) . . ?
C3 C2 N1 118.2(3) . . ?
C3 C2 C1 103.8(3) . . ?
N1 C2 C1 108.9(2) . . ?
C3 C2 H2A 110(2) . . ?
N1 C2 H2A 106(2) . . ?
C1 C2 H2A 109(2) . . ?
C12 C3 C4 118.7(3) . . ?
C12 C3 C2 134.0(3) . . ?
C4 C3 C2 107.0(3) . . ?
C9 C4 C3 123.8(3) . . ?
C9 C4 C5 122.1(3) . . ?
C3 C4 C5 114.1(3) . . ?
C6 C5 C4 120.5(3) . . ?
C6 C5 C1 132.4(3) . . ?
C4 C5 C1 107.1(3) . . ?
C5 C6 C7 117.9(3) . . ?
C5 C6 H6A 121.0 . . ?
C7 C6 H6A 121.0 . . ?
C8 C7 C6 122.1(3) . . ?
C8 C7 H7A 118.9 . . ?
C6 C7 H7A 118.9 . . ?
C7 C8 C9 121.1(3) . . ?
C7 C8 H8A 119.4 . . ?
C9 C8 H8A 119.4 . . ?
C4 C9 C10 116.4(3) . . ?
C4 C9 C8 116.3(3) . . ?
C10 C9 C8 127.3(3) . . ?
C11 C10 C9 119.9(3) . . ?
C11 C10 H10A 120.1 . . ?
C9 C10 H10A 120.1 . . ?
C10 C11 C12 122.3(3) . . ?
C10 C11 H11A 118.9 . . ?
C12 C11 H11A 118.9 . . ?
C3 C12 C11 118.9(3) . . ?
C3 C12 H12A 120.5 . . ?
C11 C12 H12A 120.5 . . ?
C18 C13 C14 124.5(3) . . ?
C18 C13 N1 118.6(3) . . ?
C14 C13 N1 116.9(3) . . ?
C15 C14 C13 116.3(3) . . ?
C15 C14 C19 120.7(3) . . ?
C13 C14 C19 122.9(3) . . ?
C16 C15 C14 120.9(3) . . ?
C16 C15 H15A 119.5 . . ?
C14 C15 H15A 119.5 . . ?
C15 C16 C17 120.9(3) . . ?
C15 C16 H16A 119.5 . . ?
C17 C16 H16A 119.5 . . ?
C16 C17 C18 120.9(3) . . ?
C16 C17 H17A 119.5 . . ?
C18 C17 H17A 119.5 . . ?
C13 C18 C17 116.4(3) . . ?
C13 C18 C22 124.3(3) . . ?
C17 C18 C22 119.3(3) . . ?
C14 C19 C21 110.9(3) . . ?
C14 C19 C20 112.5(3) . . ?
C21 C19 C20 110.4(3) . . ?
C14 C19 H19A 107.6 . . ?
C21 C19 H19A 107.6 . . ?
C20 C19 H19A 107.6 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22 C24 111.6(3) . . ?
C18 C22 C23 111.1(3) . . ?
C24 C22 C23 110.9(3) . . ?
C18 C22 H22A 107.7 . . ?
C24 C22 H22A 107.7 . . ?
C23 C22 H22A 107.7 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
F2 B1 F4 110.9(3) . . ?
F2 B1 F1 111.2(3) . . ?
F4 B1 F1 110.2(3) . . ?
F2 B1 F3 108.6(3) . . ?
F4 B1 F3 108.7(3) . . ?
F1 B1 F3 107.1(2) . . ?

_refine_diff_density_max         0.364
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.077

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_alh2mianlithf2
_database_code_depnum_ccdc_archive 'CCDC 2395060'
loop_
_audit_author_name
_audit_author_address
'Anton Cherkasov'
;IOMC RAS
Russia
;
_audit_update_record             
;
2024-10-30 deposited with the CCDC.	2025-02-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C72 H102 Al2 Li2 N2 O8'
_chemical_formula_sum            'C72 H102 Al2 Li2 N2 O8'
_chemical_formula_weight         1191.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 '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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.6320(6)
_cell_length_b                   13.0113(7)
_cell_length_c                   13.1794(7)
_cell_angle_alpha                80.2304(17)
_cell_angle_beta                 76.6792(18)
_cell_angle_gamma                69.7594(17)
_cell_volume                     1656.48(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9755
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      30.08

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_F_000             644
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    0.100
_shelx_estimated_absorpt_T_min   0.957
_shelx_estimated_absorpt_T_max   0.982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.876
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus source'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24492
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.213
_diffrn_reflns_theta_max         28.700
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             8503
_reflns_number_gt                7204
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       APEX2
_computing_cell_refinement       'Saint 8.37a'
_computing_data_reduction        'Saint 8.37a'
_computing_structure_solution    'SHELXT 2018/2'
_computing_structure_refinement  'SHELXL 2019/2'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0452P)²+0.8779P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8503
_refine_ls_number_parameters     415
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0414
_refine_ls_wR_factor_ref         0.1078
_refine_ls_wR_factor_gt          0.1015
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Al1 Al 0.40554(3) 0.51208(3) 0.66552(3) 0.01159(8) Uani 1 1 d . . . . .
H1 H 0.3908(17) 0.5090(13) 0.7890(13) 0.027(4) Uiso 1 1 d . . . . .
H2 H 0.2986(17) 0.6099(14) 0.6223(13) 0.030(4) Uiso 1 1 d . . . . .
Li1 Li 0.5685(2) 0.54917(17) 0.77698(16) 0.0188(4) Uani 1 1 d . . . . .
O1 O 0.56666(8) 0.53549(7) 0.63809(6) 0.01359(16) Uani 1 1 d . . . . .
O2 O 0.54469(10) 0.69714(7) 0.80018(7) 0.02128(19) Uani 1 1 d . . . . .
O3 O 0.64433(9) 0.44696(7) 0.88581(7) 0.01924(18) Uani 1 1 d . . . . .
N1 N 0.59004(10) 0.62271(7) 0.36576(7) 0.01115(18) Uani 1 1 d . . . . .
C1 C 0.65416(11) 0.55420(9) 0.54290(8) 0.0119(2) Uani 1 1 d . . . . .
H1A H 0.6896(14) 0.4878(11) 0.5044(11) 0.011(3) Uiso 1 1 d . . . . .
C2 C 0.58030(11) 0.65543(9) 0.46986(8) 0.0116(2) Uani 1 1 d . . . . .
H2A H 0.4840(14) 0.6847(11) 0.5072(10) 0.009(3) Uiso 1 1 d . . . . .
C3 C 0.65114(12) 0.74032(9) 0.46759(8) 0.0129(2) Uani 1 1 d . . . . .
C4 C 0.76225(12) 0.69148(9) 0.52018(8) 0.0131(2) Uani 1 1 d . . . . .
C5 C 0.77135(11) 0.58361(9) 0.56446(8) 0.0129(2) Uani 1 1 d . . . . .
C6 C 0.87445(12) 0.52597(10) 0.61865(9) 0.0170(2) Uani 1 1 d . . . . .
H6A H 0.882265 0.453187 0.649932 0.020 Uiso 1 1 calc R U . . .
C7 C 0.96944(12) 0.57753(11) 0.62699(10) 0.0195(2) Uani 1 1 d . . . . .
H7A H 1.042109 0.537363 0.663121 0.023 Uiso 1 1 calc R U . . .
C8 C 0.95954(12) 0.68345(10) 0.58452(9) 0.0181(2) Uani 1 1 d . . . . .
H8A H 1.024940 0.715101 0.591565 0.022 Uiso 1 1 calc R U . . .
C9 C 0.85215(12) 0.74576(10) 0.53021(9) 0.0156(2) Uani 1 1 d . . . . .
C10 C 0.82331(13) 0.85715(10) 0.48646(10) 0.0187(2) Uani 1 1 d . . . . .
H10A H 0.881140 0.897595 0.489997 0.022 Uiso 1 1 calc R U . . .
C11 C 0.71191(14) 0.90634(10) 0.43907(10) 0.0198(2) Uani 1 1 d . . . . .
H11A H 0.692925 0.981518 0.412059 0.024 Uiso 1 1 calc R U . . .
C12 C 0.62358(13) 0.84919(10) 0.42875(9) 0.0167(2) Uani 1 1 d . . . . .
H12A H 0.547096 0.885613 0.395672 0.020 Uiso 1 1 calc R U . . .
C13 C 0.55238(11) 0.71245(9) 0.28713(8) 0.0116(2) Uani 1 1 d . . . . .
C14 C 0.41539(12) 0.77990(9) 0.28944(9) 0.0131(2) Uani 1 1 d . . . . .
C15 C 0.38375(13) 0.86481(9) 0.20969(9) 0.0170(2) Uani 1 1 d . . . . .
H15A H 0.292200 0.911944 0.212682 0.020 Uiso 1 1 calc R U . . .
C16 C 0.48349(13) 0.88163(10) 0.12616(10) 0.0193(2) Uani 1 1 d . . . . .
H16A H 0.459819 0.938101 0.071240 0.023 Uiso 1 1 calc R U . . .
C17 C 0.61776(13) 0.81550(10) 0.12345(9) 0.0176(2) Uani 1 1 d . . . . .
H17A H 0.685920 0.826799 0.066042 0.021 Uiso 1 1 calc R U . . .
C18 C 0.65471(12) 0.73237(9) 0.20380(9) 0.0139(2) Uani 1 1 d . . . . .
C19 C 0.29985(12) 0.76171(9) 0.37504(9) 0.0140(2) Uani 1 1 d . . . . .
H19A H 0.338310 0.692109 0.419148 0.017 Uiso 1 1 calc R U . . .
C20 C 0.18732(12) 0.74784(10) 0.32958(10) 0.0187(2) Uani 1 1 d . . . . .
H20A H 0.226998 0.688604 0.283275 0.028 Uiso 1 1 calc R U . . .
H20B H 0.143805 0.816724 0.289577 0.028 Uiso 1 1 calc R U . . .
H20C H 0.119042 0.729299 0.386758 0.028 Uiso 1 1 calc R U . . .
C21 C 0.24025(13) 0.85563(11) 0.44626(10) 0.0217(3) Uani 1 1 d . . . . .
H21A H 0.312365 0.860908 0.477927 0.033 Uiso 1 1 calc R U . . .
H21B H 0.167695 0.840807 0.501616 0.033 Uiso 1 1 calc R U . . .
H21C H 0.202635 0.925145 0.404712 0.033 Uiso 1 1 calc R U . . .
C22 C 0.80396(12) 0.66584(10) 0.20024(9) 0.0179(2) Uani 1 1 d . . . . .
H22A H 0.810504 0.614167 0.265719 0.022 Uiso 1 1 calc R U . . .
C23 C 0.86049(14) 0.59627(12) 0.10751(12) 0.0287(3) Uani 1 1 d . . . . .
H23A H 0.803683 0.550199 0.109924 0.043 Uiso 1 1 calc R U . . .
H23B H 0.954223 0.549239 0.111238 0.043 Uiso 1 1 calc R U . . .
H23C H 0.859830 0.644757 0.041898 0.043 Uiso 1 1 calc R U . . .
C24 C 0.89012(14) 0.73924(13) 0.19891(11) 0.0268(3) Uani 1 1 d . . . . .
H24A H 0.853247 0.781732 0.259870 0.040 Uiso 1 1 calc R U . . .
H24B H 0.887702 0.789729 0.134577 0.040 Uiso 1 1 calc R U . . .
H24C H 0.984569 0.693254 0.201434 0.040 Uiso 1 1 calc R U . . .
C25 C 0.64901(15) 0.73324(11) 0.82283(12) 0.0279(3) Uani 1 1 d D . . . .
H25A H 0.740545 0.690052 0.787628 0.033 Uiso 0.849(3) 1 calc R U P A 1
H25B H 0.647156 0.723958 0.899228 0.033 Uiso 0.849(3) 1 calc R U P A 1
H25C H 0.730537 0.718220 0.766240 0.033 Uiso 0.151(3) 1 calc R U P A 2
H25D H 0.676518 0.695814 0.889967 0.033 Uiso 0.151(3) 1 calc R U P A 2
C26 C 0.61643(19) 0.85442(13) 0.78127(18) 0.0337(5) Uani 0.849(3) 1 d D . P A 1
H26A H 0.664964 0.863718 0.708336 0.040 Uiso 0.849(3) 1 calc R U P A 1
H26B H 0.640539 0.896189 0.825841 0.040 Uiso 0.849(3) 1 calc R U P A 1
C27 C 0.46228(19) 0.89053(13) 0.78706(16) 0.0310(4) Uani 0.849(3) 1 d D . P A 1
H27A H 0.411754 0.904418 0.859161 0.037 Uiso 0.849(3) 1 calc R U P A 1
H27B H 0.430726 0.957105 0.738641 0.037 Uiso 0.849(3) 1 calc R U P A 1
C26* C 0.5813(11) 0.8561(4) 0.8294(8) 0.0337(5) Uani 0.151(3) 1 d D . P A 2
H26C H 0.648755 0.895294 0.820383 0.040 Uiso 0.151(3) 1 calc R U P A 2
H26D H 0.515255 0.872853 0.895710 0.040 Uiso 0.151(3) 1 calc R U P A 2
C27* C 0.5112(11) 0.8812(7) 0.7355(8) 0.0310(4) Uani 0.151(3) 1 d D . P A 2
H27C H 0.577708 0.877678 0.668757 0.037 Uiso 0.151(3) 1 calc R U P A 2
H27D H 0.440486 0.954537 0.735818 0.037 Uiso 0.151(3) 1 calc R U P A 2
C28 C 0.44815(17) 0.78942(11) 0.75246(11) 0.0290(3) Uani 1 1 d D . . . .
H28A H 0.354219 0.786163 0.777253 0.035 Uiso 0.849(3) 1 calc R U P A 1
H28B H 0.470297 0.790609 0.675166 0.035 Uiso 0.849(3) 1 calc R U P A 1
H28C H 0.357890 0.809774 0.799417 0.035 Uiso 0.151(3) 1 calc R U P A 2
H28D H 0.437452 0.772559 0.685062 0.035 Uiso 0.151(3) 1 calc R U P A 2
C29 C 0.60278(13) 0.35271(10) 0.93341(10) 0.0202(2) Uani 1 1 d . . . B 2
H29A H 0.572358 0.323045 0.882401 0.024 Uiso 1 1 calc R U . B 2
H29B H 0.527789 0.371986 0.994430 0.024 Uiso 1 1 calc R U . B 2
C30 C 0.73040(14) 0.27054(11) 0.96713(10) 0.0243(3) Uani 1 1 d . . . B 2
H30A H 0.794049 0.232150 0.907466 0.029 Uiso 1 1 calc R U . B 2
H30B H 0.708096 0.215416 1.023624 0.029 Uiso 1 1 calc R U . B 2
C31 C 0.78979(14) 0.34457(11) 1.00651(10) 0.0238(3) Uani 1 1 d . . . B 2
H31A H 0.751818 0.354477 1.081509 0.029 Uiso 1 1 calc R U . B 2
H31B H 0.890444 0.313610 0.996914 0.029 Uiso 1 1 calc R U . B 2
C32 C 0.74606(15) 0.45281(12) 0.93835(12) 0.0275(3) Uani 1 1 d . . . B 2
H32A H 0.707662 0.515221 0.982133 0.033 Uiso 1 1 calc R U . B 2
H32B H 0.825256 0.463614 0.886475 0.033 Uiso 1 1 calc R U . B 2
O1S O 0.87950(18) 0.86979(17) 0.89101(12) 0.0754(6) Uani 1 1 d . . . C 2
C1S C 0.93389(17) 0.94113(13) 0.91944(12) 0.0355(3) Uani 1 1 d . . . C 2
H1SA H 0.970983 0.909734 0.984371 0.043 Uiso 1 1 calc R U . C 2
H1SB H 0.862101 1.012602 0.932597 0.043 Uiso 1 1 calc R U . C 2
C2S C 1.04670(19) 0.95754(15) 0.83052(14) 0.0422(4) Uani 1 1 d . . . C 2
H2SA H 1.032212 1.036753 0.808357 0.051 Uiso 1 1 calc R U . C 2
H2SB H 1.137068 0.923783 0.851353 0.051 Uiso 1 1 calc R U . C 2
C3S C 1.0357(2) 0.90010(17) 0.74435(14) 0.0476(5) Uani 1 1 d . . . C 2
H3SA H 0.980548 0.952823 0.695170 0.057 Uiso 1 1 calc R U . C 2
H3SB H 1.126985 0.862233 0.704784 0.057 Uiso 1 1 calc R U . C 2
C4S C 0.9667(2) 0.81958(18) 0.80164(15) 0.0501(5) Uani 1 1 d . . . C 2
H4SA H 0.913367 0.804148 0.757063 0.060 Uiso 1 1 calc R U . C 2
H4SB H 1.034577 0.749572 0.822871 0.060 Uiso 1 1 calc R U . C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Al1 O1 1.7878(9) . ?
Al1 N1 1.8513(10) 2_666 ?
Al1 Li1 2.717(2) . ?
Al1 H1 1.594(16) . ?
Al1 H2 1.513(17) . ?
Li1 O1 1.874(2) . ?
Li1 O3 1.903(2) . ?
Li1 O2 1.921(2) . ?
Li1 H1 2.094(17) . ?
O1 C1 1.4192(13) . ?
O2 C28 1.4419(16) . ?
O2 C25 1.4492(16) . ?
O3 C32 1.4405(15) . ?
O3 C29 1.4418(14) . ?
N1 C13 1.4334(13) . ?
N1 C2 1.4754(14) . ?
C1 C5 1.5196(15) . ?
C1 C2 1.5750(15) . ?
C1 H1A 0.991(14) . ?
C2 C3 1.5303(15) . ?
C2 H2A 0.999(14) . ?
C3 C12 1.3750(15) . ?
C3 C4 1.4100(16) . ?
C4 C5 1.4050(15) . ?
C4 C9 1.4095(15) . ?
C5 C6 1.3727(16) . ?
C6 C7 1.4238(17) . ?
C6 H6A 0.9500 . ?
C7 C8 1.3743(18) . ?
C7 H7A 0.9500 . ?
C8 C9 1.4186(17) . ?
C8 H8A 0.9500 . ?
C9 C10 1.4204(16) . ?
C10 C11 1.3724(18) . ?
C10 H10A 0.9500 . ?
C11 C12 1.4247(16) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9500 . ?
C13 C14 1.4131(16) . ?
C13 C18 1.4159(15) . ?
C14 C15 1.3965(15) . ?
C14 C19 1.5197(15) . ?
C15 C16 1.3876(17) . ?
C15 H15A 0.9500 . ?
C16 C17 1.3844(18) . ?
C16 H16A 0.9500 . ?
C17 C18 1.3981(16) . ?
C17 H17A 0.9500 . ?
C18 C22 1.5161(17) . ?
C19 C20 1.5295(16) . ?
C19 C21 1.5347(16) . ?
C19 H19A 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.5280(18) . ?
C22 C24 1.5310(17) . ?
C22 H22A 1.0000 . ?
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 C26* 1.518(4) . ?
C25 C26 1.5240(19) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 H25C 0.9900 . ?
C25 H25D 0.9900 . ?
C26 C27 1.528(2) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.5275(19) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C26* C27* 1.522(4) . ?
C26* H26C 0.9900 . ?
C26* H26D 0.9900 . ?
C27* C28 1.523(4) . ?
C27* H27C 0.9900 . ?
C27* H27D 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 H28C 0.9900 . ?
C28 H28D 0.9900 . ?
C29 C30 1.5147(18) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.529(2) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.5221(18) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
O1S C1S 1.388(2) . ?
O1S C4S 1.419(2) . ?
C1S C2S 1.517(2) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
C2S C3S 1.507(3) . ?
C2S H2SA 0.9900 . ?
C2S H2SB 0.9900 . ?
C3S C4S 1.487(3) . ?
C3S H3SA 0.9900 . ?
C3S H3SB 0.9900 . ?
C4S H4SA 0.9900 . ?
C4S H4SB 0.9900 . ?

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
O1 Al1 N1 115.39(4) . 2_666 ?
O1 Al1 Li1 43.33(5) . . ?
N1 Al1 Li1 127.09(6) 2_666 . ?
O1 Al1 H1 93.4(6) . . ?
N1 Al1 H1 109.0(6) 2_666 . ?
Li1 Al1 H1 50.2(6) . . ?
O1 Al1 H2 110.7(6) . . ?
N1 Al1 H2 114.4(6) 2_666 . ?
Li1 Al1 H2 118.5(6) . . ?
H1 Al1 H2 112.0(9) . . ?
O1 Li1 O3 132.78(12) . . ?
O1 Li1 O2 112.83(11) . . ?
O3 Li1 O2 110.81(11) . . ?
O1 Li1 Al1 40.89(5) . . ?
O3 Li1 Al1 123.21(10) . . ?
O2 Li1 Al1 119.79(10) . . ?
O1 Li1 H1 76.6(5) . . ?
O3 Li1 H1 99.2(5) . . ?
O2 Li1 H1 116.8(5) . . ?
Al1 Li1 H1 35.8(4) . . ?
C1 O1 Al1 132.42(7) . . ?
C1 O1 Li1 131.20(9) . . ?
Al1 O1 Li1 95.78(8) . . ?
C28 O2 C25 109.25(10) . . ?
C28 O2 Li1 120.62(10) . . ?
C25 O2 Li1 124.96(10) . . ?
C32 O3 C29 108.45(9) . . ?
C32 O3 Li1 126.66(10) . . ?
C29 O3 Li1 124.80(10) . . ?
C13 N1 C2 114.85(8) . . ?
C13 N1 Al1 115.06(7) . 2_666 ?
C2 N1 Al1 127.45(7) . 2_666 ?
O1 C1 C5 110.49(9) . . ?
O1 C1 C2 112.52(9) . . ?
C5 C1 C2 104.79(9) . . ?
O1 C1 H1A 109.7(8) . . ?
C5 C1 H1A 110.4(8) . . ?
C2 C1 H1A 108.8(8) . . ?
N1 C2 C3 113.95(9) . . ?
N1 C2 C1 110.92(9) . . ?
C3 C2 C1 104.08(9) . . ?
N1 C2 H2A 112.7(8) . . ?
C3 C2 H2A 108.0(8) . . ?
C1 C2 H2A 106.5(8) . . ?
C12 C3 C4 118.40(10) . . ?
C12 C3 C2 132.68(11) . . ?
C4 C3 C2 108.88(9) . . ?
C5 C4 C9 123.47(11) . . ?
C5 C4 C3 112.62(10) . . ?
C9 C4 C3 123.88(10) . . ?
C6 C5 C4 119.07(10) . . ?
C6 C5 C1 131.81(10) . . ?
C4 C5 C1 109.10(10) . . ?
C5 C6 C7 118.62(11) . . ?
C5 C6 H6A 120.7 . . ?
C7 C6 H6A 120.7 . . ?
C8 C7 C6 122.21(11) . . ?
C8 C7 H7A 118.9 . . ?
C6 C7 H7A 118.9 . . ?
C7 C8 C9 120.32(11) . . ?
C7 C8 H8A 119.8 . . ?
C9 C8 H8A 119.8 . . ?
C4 C9 C8 116.25(11) . . ?
C4 C9 C10 116.26(11) . . ?
C8 C9 C10 127.48(11) . . ?
C11 C10 C9 119.99(11) . . ?
C11 C10 H10A 120.0 . . ?
C9 C10 H10A 120.0 . . ?
C10 C11 C12 122.63(11) . . ?
C10 C11 H11A 118.7 . . ?
C12 C11 H11A 118.7 . . ?
C3 C12 C11 118.73(11) . . ?
C3 C12 H12A 120.6 . . ?
C11 C12 H12A 120.6 . . ?
C14 C13 C18 119.22(10) . . ?
C14 C13 N1 121.66(10) . . ?
C18 C13 N1 119.10(10) . . ?
C15 C14 C13 119.38(10) . . ?
C15 C14 C19 118.48(10) . . ?
C13 C14 C19 122.12(10) . . ?
C16 C15 C14 121.25(11) . . ?
C16 C15 H15A 119.4 . . ?
C14 C15 H15A 119.4 . . ?
C17 C16 C15 119.50(11) . . ?
C17 C16 H16A 120.3 . . ?
C15 C16 H16A 120.3 . . ?
C16 C17 C18 121.09(11) . . ?
C16 C17 H17A 119.5 . . ?
C18 C17 H17A 119.5 . . ?
C17 C18 C13 119.47(11) . . ?
C17 C18 C22 119.21(10) . . ?
C13 C18 C22 121.32(10) . . ?
C14 C19 C20 111.70(9) . . ?
C14 C19 C21 111.28(9) . . ?
C20 C19 C21 110.33(10) . . ?
C14 C19 H19A 107.8 . . ?
C20 C19 H19A 107.8 . . ?
C21 C19 H19A 107.8 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22 C23 111.55(10) . . ?
C18 C22 C24 111.65(11) . . ?
C23 C22 C24 110.95(10) . . ?
C18 C22 H22A 107.5 . . ?
C23 C22 H22A 107.5 . . ?
C24 C22 H22A 107.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O2 C25 C26* 104.1(4) . . ?
O2 C25 C26 106.14(12) . . ?
O2 C25 H25A 110.5 . . ?
C26 C25 H25A 110.5 . . ?
O2 C25 H25B 110.5 . . ?
C26 C25 H25B 110.5 . . ?
H25A C25 H25B 108.7 . . ?
O2 C25 H25C 110.9 . . ?
C26* C25 H25C 110.9 . . ?
O2 C25 H25D 110.9 . . ?
C26* C25 H25D 110.9 . . ?
H25C C25 H25D 109.0 . . ?
C25 C26 C27 102.24(13) . . ?
C25 C26 H26A 111.3 . . ?
C27 C26 H26A 111.3 . . ?
C25 C26 H26B 111.3 . . ?
C27 C26 H26B 111.3 . . ?
H26A C26 H26B 109.2 . . ?
C28 C27 C26 100.65(13) . . ?
C28 C27 H27A 111.6 . . ?
C26 C27 H27A 111.6 . . ?
C28 C27 H27B 111.6 . . ?
C26 C27 H27B 111.6 . . ?
H27A C27 H27B 109.4 . . ?
C25 C26* C27* 97.8(6) . . ?
C25 C26* H26C 112.2 . . ?
C27* C26* H26C 112.2 . . ?
C25 C26* H26D 112.2 . . ?
C27* C26* H26D 112.2 . . ?
H26C C26* H26D 109.8 . . ?
C26* C27* C28 102.0(6) . . ?
C26* C27* H27C 111.4 . . ?
C28 C27* H27C 111.4 . . ?
C26* C27* H27D 111.4 . . ?
C28 C27* H27D 111.4 . . ?
H27C C27* H27D 109.2 . . ?
O2 C28 C27* 103.8(4) . . ?
O2 C28 C27 104.64(12) . . ?
O2 C28 H28A 110.8 . . ?
C27 C28 H28A 110.8 . . ?
O2 C28 H28B 110.8 . . ?
C27 C28 H28B 110.8 . . ?
H28A C28 H28B 108.9 . . ?
O2 C28 H28C 111.0 . . ?
C27* C28 H28C 111.0 . . ?
O2 C28 H28D 111.0 . . ?
C27* C28 H28D 111.0 . . ?
H28C C28 H28D 109.0 . . ?
O3 C29 C30 103.85(10) . . ?
O3 C29 H29A 111.0 . . ?
C30 C29 H29A 111.0 . . ?
O3 C29 H29B 111.0 . . ?
C30 C29 H29B 111.0 . . ?
H29A C29 H29B 109.0 . . ?
C29 C30 C31 102.01(10) . . ?
C29 C30 H30A 111.4 . . ?
C31 C30 H30A 111.4 . . ?
C29 C30 H30B 111.4 . . ?
C31 C30 H30B 111.4 . . ?
H30A C30 H30B 109.2 . . ?
C32 C31 C30 103.43(10) . . ?
C32 C31 H31A 111.1 . . ?
C30 C31 H31A 111.1 . . ?
C32 C31 H31B 111.1 . . ?
C30 C31 H31B 111.1 . . ?
H31A C31 H31B 109.0 . . ?
O3 C32 C31 107.16(11) . . ?
O3 C32 H32A 110.3 . . ?
C31 C32 H32A 110.3 . . ?
O3 C32 H32B 110.3 . . ?
C31 C32 H32B 110.3 . . ?
H32A C32 H32B 108.5 . . ?
C1S O1S C4S 109.22(14) . . ?
O1S C1S C2S 108.18(13) . . ?
O1S C1S H1SA 110.1 . . ?
C2S C1S H1SA 110.1 . . ?
O1S C1S H1SB 110.1 . . ?
C2S C1S H1SB 110.1 . . ?
H1SA C1S H1SB 108.4 . . ?
C3S C2S C1S 103.59(15) . . ?
C3S C2S H2SA 111.0 . . ?
C1S C2S H2SA 111.0 . . ?
C3S C2S H2SB 111.0 . . ?
C1S C2S H2SB 111.0 . . ?
H2SA C2S H2SB 109.0 . . ?
C4S C3S C2S 103.43(15) . . ?
C4S C3S H3SA 111.1 . . ?
C2S C3S H3SA 111.1 . . ?
C4S C3S H3SB 111.1 . . ?
C2S C3S H3SB 111.1 . . ?
H3SA C3S H3SB 109.0 . . ?
O1S C4S C3S 105.65(16) . . ?
O1S C4S H4SA 110.6 . . ?
C3S C4S H4SA 110.6 . . ?
O1S C4S H4SB 110.6 . . ?
C3S C4S H4SB 110.6 . . ?
H4SA C4S H4SB 108.7 . . ?

_refine_diff_density_max         0.548
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.049

