# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_1_5LiT
_database_code_depnum_ccdc_archive 'CCDC 1866252'
loop_
_audit_author_name
_audit_author_address
'Bingjia Yan'
;University of Southampton
China
;
_audit_update_record             
;
2018-09-06 deposited with the CCDC.	2019-04-30 downloaded from the CCDC.
;

#2011pnh0066

_audit_creation_date             2018-09-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C22 H24 Li N4 O5'
_chemical_formula_sum            'C22 H24 Li N4 O5'
_chemical_formula_weight         431.39
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C22 H24 N4 O5 Li'
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   9.8106(3)
_cell_length_b                   15.2713(6)
_cell_length_c                   14.7499(6)
_cell_angle_alpha                90
_cell_angle_beta                 102.098(4)
_cell_angle_gamma                90
_cell_volume                     2160.76(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7995
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.0810
_cell_measurement_theta_min      2.6250
_shelx_estimated_absorpt_T_max   0.999
_shelx_estimated_absorpt_T_min   0.995
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark purple'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    purple
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18831
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.507
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  18.00   1.00  120.00    --  -20.00 -70.00 120.00  128
  2  ω   -110.00  18.00   1.00  120.00    --  -20.00 -70.00 270.00  128
  3  ω    -57.00  48.00   1.00  120.00    --  -20.00 -10.00 270.00  105
  4  ω     10.00  40.00   1.00  120.00    --  -20.00   0.00 240.00   30
;
_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  
'Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0716692000
_diffrn_orient_matrix_UB_12      0.0109421000
_diffrn_orient_matrix_UB_13      0.0064293000
_diffrn_orient_matrix_UB_21      -0.0143783000
_diffrn_orient_matrix_UB_22      0.0251047000
_diffrn_orient_matrix_UB_23      -0.0413825000
_diffrn_orient_matrix_UB_31      -0.0112171000
_diffrn_orient_matrix_UB_32      0.0375089000
_diffrn_orient_matrix_UB_33      0.0258028000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3352
_reflns_number_total             4942
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4942
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0454
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0315P)²+0.6370P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0905
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
 C30(H30A,H30B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Li1 Li -0.0051(3) 0.19328(18) 0.4744(2) 0.0187(6) Uani 1 1 d . . . . .
O21 O -0.23145(10) 0.22308(7) 0.46869(8) 0.0173(3) Uani 1 1 d . . . . .
O22 O -0.12089(11) 0.15058(7) 0.33081(8) 0.0189(3) Uani 1 1 d . . . . .
O23 O 0.14201(11) 0.22458(7) 0.37546(8) 0.0179(3) Uani 1 1 d . . . . .
O24 O 0.16762(10) 0.10647(7) 0.51367(8) 0.0160(3) Uani 1 1 d . . . . .
O25 O -0.04775(10) 0.13031(7) 0.59046(8) 0.0166(3) Uani 1 1 d . . . . .
C21 C -0.31991(16) 0.19276(12) 0.38532(12) 0.0188(4) Uani 1 1 d . . . . .
H21A H -0.407933 0.226596 0.372210 0.023 Uiso 1 1 calc R . . . .
H21B H -0.342619 0.130108 0.391055 0.023 Uiso 1 1 calc R . . . .
C22 C -0.24195(15) 0.20537(11) 0.30895(12) 0.0188(4) Uani 1 1 d . . . . .
H22A H -0.300848 0.188327 0.248530 0.023 Uiso 1 1 calc R . . . .
H22B H -0.214449 0.267455 0.305496 0.023 Uiso 1 1 calc R . . . .
C23 C -0.03646(16) 0.15413(11) 0.26213(12) 0.0185(4) Uani 1 1 d . . . . .
H23A H -0.097077 0.161146 0.199848 0.022 Uiso 1 1 calc R . . . .
H23B H 0.015874 0.098627 0.262773 0.022 Uiso 1 1 calc R . . . .
C24 C 0.06445(16) 0.22976(11) 0.28145(11) 0.0177(4) Uani 1 1 d . . . . .
H24A H 0.129167 0.227732 0.238225 0.021 Uiso 1 1 calc R . . . .
H24B H 0.012726 0.285810 0.271778 0.021 Uiso 1 1 calc R . . . .
C25 C 0.25509(16) 0.16330(11) 0.38926(12) 0.0195(4) Uani 1 1 d . . . . .
H25A H 0.336568 0.189348 0.369476 0.023 Uiso 1 1 calc R . . . .
H25B H 0.227141 0.109729 0.352230 0.023 Uiso 1 1 calc R . . . .
C26 C 0.29159(16) 0.14127(12) 0.49046(12) 0.0190(4) Uani 1 1 d . . . . .
H26A H 0.367566 0.097430 0.502841 0.023 Uiso 1 1 calc R . . . .
H26B H 0.322591 0.194350 0.527615 0.023 Uiso 1 1 calc R . . . .
C27 C 0.18516(16) 0.08550(11) 0.61028(11) 0.0160(4) Uani 1 1 d . . . . .
H27A H 0.220880 0.136904 0.648914 0.019 Uiso 1 1 calc R . . . .
H27B H 0.252025 0.036620 0.626862 0.019 Uiso 1 1 calc R . . . .
C28 C 0.04397(16) 0.05963(11) 0.62549(12) 0.0164(4) Uani 1 1 d . . . . .
H28A H 0.012315 0.004744 0.591893 0.020 Uiso 1 1 calc R . . . .
H28B H 0.046916 0.050538 0.692328 0.020 Uiso 1 1 calc R . . . .
C29 C -0.19150(15) 0.11055(11) 0.58616(12) 0.0171(4) Uani 1 1 d . . . . .
H29A H -0.206917 0.094313 0.648212 0.021 Uiso 1 1 calc R . . . .
H29B H -0.222172 0.061419 0.542900 0.021 Uiso 1 1 calc R . . . .
C30 C -0.26976(16) 0.19257(11) 0.55212(12) 0.0185(4) Uani 1 1 d . . . . .
H30A H -0.371217 0.180822 0.539787 0.022 Uiso 1 1 calc R . . . .
H30B H -0.248675 0.238430 0.600465 0.022 Uiso 1 1 calc R . . . .
N1 N 0.06433(13) 0.31267(9) 0.53484(10) 0.0179(3) Uani 1 1 d . . . . .
N2 N 0.12534(14) 0.56839(9) 0.67206(10) 0.0216(3) Uani 1 1 d . . . . .
N3 N 0.62206(14) 0.72148(10) 0.30568(10) 0.0207(3) Uani 1 1 d . . . . .
N4 N 0.55317(14) 0.46993(10) 0.15816(11) 0.0250(4) Uani 1 1 d . . . . .
C1 C 0.26689(15) 0.48842(10) 0.48448(11) 0.0129(3) Uani 1 1 d . . . . .
C2 C 0.28706(15) 0.43165(10) 0.41122(11) 0.0143(3) Uani 1 1 d . . . . .
H2 H 0.241340 0.376479 0.403647 0.017 Uiso 1 1 calc R . . . .
C3 C 0.37068(15) 0.45511(10) 0.35194(11) 0.0143(3) Uani 1 1 d . . . . .
H3 H 0.382138 0.415901 0.304100 0.017 Uiso 1 1 calc R . . . .
C4 C 0.44105(15) 0.53730(10) 0.36052(11) 0.0138(3) Uani 1 1 d . . . . .
C5 C 0.41960(15) 0.59387(10) 0.43282(11) 0.0138(3) Uani 1 1 d . . . . .
H5 H 0.464477 0.649315 0.440041 0.017 Uiso 1 1 calc R . . . .
C6 C 0.33587(15) 0.57039(10) 0.49229(11) 0.0141(3) Uani 1 1 d . . . . .
H6 H 0.323810 0.609889 0.539743 0.017 Uiso 1 1 calc R . . . .
C7 C 0.18238(15) 0.46400(10) 0.54761(11) 0.0140(3) Uani 1 1 d . . . . .
C8 C 0.52574(15) 0.56402(10) 0.29827(11) 0.0140(3) Uani 1 1 d . . . . .
C9 C 0.11597(16) 0.38089(11) 0.54136(11) 0.0138(3) Uani 1 1 d . . . . .
C10 C 0.15241(15) 0.52208(11) 0.61657(12) 0.0149(3) Uani 1 1 d . . . . .
C11 C 0.58213(15) 0.65015(11) 0.30308(11) 0.0150(4) Uani 1 1 d . . . . .
C12 C 0.54281(15) 0.51125(11) 0.22170(12) 0.0157(4) 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
Li1 O21 2.251(3) . ?
Li1 O22 2.278(3) . ?
Li1 O23 2.307(3) . ?
Li1 O24 2.134(3) . ?
Li1 O25 2.081(3) . ?
Li1 N1 2.081(3) . ?
O21 C21 1.4256(19) . ?
O21 C30 1.4376(19) . ?
O22 C22 1.4332(18) . ?
O22 C23 1.4376(19) . ?
O23 C24 1.4373(19) . ?
O23 C25 1.4329(19) . ?
O24 C26 1.4329(18) . ?
O24 C27 1.4352(19) . ?
O25 C28 1.4307(18) . ?
O25 C29 1.4306(18) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.501(2) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.509(2) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.499(2) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.502(2) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.500(2) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
N1 C9 1.154(2) . ?
N2 C10 1.154(2) . ?
N3 C11 1.156(2) . ?
N4 C12 1.152(2) . ?
C1 C2 1.431(2) . ?
C1 C6 1.416(2) . ?
C1 C7 1.420(2) . ?
C2 H2 0.9500 . ?
C2 C3 1.366(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.425(2) . ?
C4 C5 1.422(2) . ?
C4 C8 1.421(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.369(2) . ?
C6 H6 0.9500 . ?
C7 C9 1.421(2) . ?
C7 C10 1.426(2) . ?
C8 C11 1.423(2) . ?
C8 C12 1.426(2) . ?

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
O21 Li1 O22 74.18(9) . . ?
O21 Li1 O23 132.66(13) . . ?
O22 Li1 O23 74.20(9) . . ?
O24 Li1 O21 148.94(15) . . ?
O24 Li1 O22 106.71(12) . . ?
O24 Li1 O23 74.59(9) . . ?
O25 Li1 O21 75.94(10) . . ?
O25 Li1 O22 119.03(13) . . ?
O25 Li1 O23 151.19(14) . . ?
O25 Li1 O24 76.97(10) . . ?
N1 Li1 O21 94.05(12) . . ?
N1 Li1 O22 134.75(15) . . ?
N1 Li1 O23 84.13(11) . . ?
N1 Li1 O24 104.95(12) . . ?
N1 Li1 O25 98.99(13) . . ?
C21 O21 Li1 112.58(11) . . ?
C21 O21 C30 114.33(12) . . ?
C30 O21 Li1 109.60(11) . . ?
C22 O22 Li1 105.67(12) . . ?
C22 O22 C23 113.09(12) . . ?
C23 O22 Li1 113.29(11) . . ?
C24 O23 Li1 110.29(11) . . ?
C25 O23 Li1 110.07(11) . . ?
C25 O23 C24 114.24(12) . . ?
C26 O24 Li1 111.72(12) . . ?
C26 O24 C27 112.88(11) . . ?
C27 O24 Li1 109.36(11) . . ?
C28 O25 Li1 115.22(12) . . ?
C29 O25 Li1 115.30(12) . . ?
C29 O25 C28 113.36(11) . . ?
O21 C21 H21A 110.3 . . ?
O21 C21 H21B 110.3 . . ?
O21 C21 C22 106.97(12) . . ?
H21A C21 H21B 108.6 . . ?
C22 C21 H21A 110.3 . . ?
C22 C21 H21B 110.3 . . ?
O22 C22 C21 106.56(13) . . ?
O22 C22 H22A 110.4 . . ?
O22 C22 H22B 110.4 . . ?
C21 C22 H22A 110.4 . . ?
C21 C22 H22B 110.4 . . ?
H22A C22 H22B 108.6 . . ?
O22 C23 H23A 109.6 . . ?
O22 C23 H23B 109.6 . . ?
O22 C23 C24 110.36(13) . . ?
H23A C23 H23B 108.1 . . ?
C24 C23 H23A 109.6 . . ?
C24 C23 H23B 109.6 . . ?
O23 C24 C23 109.49(13) . . ?
O23 C24 H24A 109.8 . . ?
O23 C24 H24B 109.8 . . ?
C23 C24 H24A 109.8 . . ?
C23 C24 H24B 109.8 . . ?
H24A C24 H24B 108.2 . . ?
O23 C25 H25A 110.2 . . ?
O23 C25 H25B 110.2 . . ?
O23 C25 C26 107.72(13) . . ?
H25A C25 H25B 108.5 . . ?
C26 C25 H25A 110.2 . . ?
C26 C25 H25B 110.2 . . ?
O24 C26 C25 106.48(13) . . ?
O24 C26 H26A 110.4 . . ?
O24 C26 H26B 110.4 . . ?
C25 C26 H26A 110.4 . . ?
C25 C26 H26B 110.4 . . ?
H26A C26 H26B 108.6 . . ?
O24 C27 H27A 110.4 . . ?
O24 C27 H27B 110.4 . . ?
O24 C27 C28 106.54(12) . . ?
H27A C27 H27B 108.6 . . ?
C28 C27 H27A 110.4 . . ?
C28 C27 H27B 110.4 . . ?
O25 C28 C27 106.12(12) . . ?
O25 C28 H28A 110.5 . . ?
O25 C28 H28B 110.5 . . ?
C27 C28 H28A 110.5 . . ?
C27 C28 H28B 110.5 . . ?
H28A C28 H28B 108.7 . . ?
O25 C29 H29A 110.6 . . ?
O25 C29 H29B 110.6 . . ?
O25 C29 C30 105.63(13) . . ?
H29A C29 H29B 108.7 . . ?
C30 C29 H29A 110.6 . . ?
C30 C29 H29B 110.6 . . ?
O21 C30 C29 110.49(13) . . ?
O21 C30 H30A 109.6 . . ?
O21 C30 H30B 109.6 . . ?
C29 C30 H30A 109.6 . . ?
C29 C30 H30B 109.6 . . ?
H30A C30 H30B 108.1 . . ?
C9 N1 Li1 157.76(15) . . ?
C6 C1 C2 117.23(14) . . ?
C6 C1 C7 120.90(15) . . ?
C7 C1 C2 121.87(15) . . ?
C1 C2 H2 119.3 . . ?
C3 C2 C1 121.39(15) . . ?
C3 C2 H2 119.3 . . ?
C2 C3 H3 119.4 . . ?
C2 C3 C4 121.26(15) . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 117.16(14) . . ?
C8 C4 C3 122.24(15) . . ?
C8 C4 C5 120.56(14) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 C4 121.62(15) . . ?
C6 C5 H5 119.2 . . ?
C1 C6 H6 119.3 . . ?
C5 C6 C1 121.33(15) . . ?
C5 C6 H6 119.3 . . ?
C1 C7 C9 120.98(14) . . ?
C1 C7 C10 122.71(14) . . ?
C9 C7 C10 116.21(14) . . ?
C4 C8 C11 120.47(15) . . ?
C4 C8 C12 122.09(15) . . ?
C11 C8 C12 116.93(14) . . ?
N1 C9 C7 178.23(17) . . ?
N2 C10 C7 178.56(17) . . ?
N3 C11 C8 177.00(17) . . ?
N4 C12 C8 177.89(18) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Li1 O21 C21 C22 -36.25(17) . . . . ?
Li1 O21 C30 C29 -34.12(16) . . . . ?
Li1 O22 C22 C21 -56.86(15) . . . . ?
Li1 O22 C23 C24 -34.26(17) . . . . ?
Li1 O23 C24 C23 -44.79(16) . . . . ?
Li1 O23 C25 C26 -35.28(16) . . . . ?
Li1 O24 C26 C25 -53.85(17) . . . . ?
Li1 O24 C27 C28 48.86(16) . . . . ?
Li1 O25 C28 C27 34.83(17) . . . . ?
Li1 O25 C29 C30 -46.49(17) . . . . ?
O21 C21 C22 O22 63.19(16) . . . . ?
O22 C23 C24 O23 53.05(17) . . . . ?
O23 C25 C26 O24 58.23(17) . . . . ?
O24 C27 C28 O25 -54.00(16) . . . . ?
O25 C29 C30 O21 51.88(17) . . . . ?
C21 O21 C30 C29 93.34(15) . . . . ?
C22 O22 C23 C24 85.95(16) . . . . ?
C23 O22 C22 C21 178.67(13) . . . . ?
C24 O23 C25 C26 -159.98(13) . . . . ?
C25 O23 C24 C23 79.80(16) . . . . ?
C26 O24 C27 C28 173.89(13) . . . . ?
C27 O24 C26 C25 -177.59(13) . . . . ?
C28 O25 C29 C30 177.67(13) . . . . ?
C29 O25 C28 C27 170.70(13) . . . . ?
C30 O21 C21 C22 -162.18(13) . . . . ?
C1 C2 C3 C4 -0.2(2) . . . . ?
C2 C1 C6 C5 -0.7(2) . . . . ?
C2 C1 C7 C9 1.1(2) . . . . ?
C2 C1 C7 C10 -175.10(15) . . . . ?
C2 C3 C4 C5 -0.5(2) . . . . ?
C2 C3 C4 C8 -178.39(15) . . . . ?
C3 C4 C5 C6 0.5(2) . . . . ?
C3 C4 C8 C11 173.27(14) . . . . ?
C3 C4 C8 C12 1.7(2) . . . . ?
C4 C5 C6 C1 0.1(2) . . . . ?
C5 C4 C8 C11 -4.6(2) . . . . ?
C5 C4 C8 C12 -176.17(15) . . . . ?
C6 C1 C2 C3 0.7(2) . . . . ?
C6 C1 C7 C9 -178.37(14) . . . . ?
C6 C1 C7 C10 5.4(2) . . . . ?
C7 C1 C2 C3 -178.75(15) . . . . ?
C7 C1 C6 C5 178.79(15) . . . . ?
C8 C4 C5 C6 178.46(14) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.456
_oxdiff_exptl_absorpt_empirical_full_min 0.672
####################################################################### 
# 
# 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_2_5NaT
_database_code_depnum_ccdc_archive 'CCDC 1866253'
loop_
_audit_author_name
_audit_author_address
'Bingjia Yan'
;University of Southampton
China
;
_audit_update_record             
;
2018-09-06 deposited with the CCDC.	2019-04-30 downloaded from the CCDC.
;

#2011pnh0067
_audit_creation_date             2018-09-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C44 H48 N8 Na2 O10'
_chemical_formula_sum            'C44 H48 N8 Na2 O10'
_chemical_formula_weight         894.88
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C12H4N4 Na C10H20O5'
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'
Na Na 0.0362 0.0249 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.2736(6)
_cell_length_b                   11.0659(7)
_cell_length_c                   11.8680(6)
_cell_angle_alpha                83.741(5)
_cell_angle_beta                 89.921(4)
_cell_angle_gamma                68.591(6)
_cell_volume                     1126.14(12)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    4377
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.1420
_cell_measurement_theta_min      2.3880
_shelx_estimated_absorpt_T_max   0.999
_shelx_estimated_absorpt_T_min   0.991
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             470
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0896
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9835
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.361
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  18.00   1.00  120.00    --  -20.00 -70.00 180.00  128
  2  ω   -110.00  18.00   1.00  120.00    --  -20.00 -70.00   0.00  128
  3  ω    -35.00  25.00   1.00  120.00    --  -20.00   0.00   0.00   60
  4  ω    -48.00 -13.00   1.00  120.00    --  -20.00 -70.00 120.00   35
  5  ω     20.00  50.00   1.00  120.00    --  -20.00   0.00  90.00   30
;
_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  
'Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0112414000
_diffrn_orient_matrix_UB_12      -0.0668097000
_diffrn_orient_matrix_UB_13      0.0145032000
_diffrn_orient_matrix_UB_21      0.0747095000
_diffrn_orient_matrix_UB_22      -0.0117511000
_diffrn_orient_matrix_UB_23      0.0237444000
_diffrn_orient_matrix_UB_31      -0.0324531000
_diffrn_orient_matrix_UB_32      0.0142767000
_diffrn_orient_matrix_UB_33      0.0533573000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3145
_reflns_number_total             5096
_reflns_odcompleteness_completeness 98.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5096
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1133
_refine_ls_R_factor_gt           0.0576
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0503P)²+0.0954P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1242
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
 C30(H30A,H30B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.44331(10) 0.75208(8) 0.64608(7) 0.0200(2) Uani 1 1 d . . . . .
C1 C -0.0507(2) 1.0713(2) 0.82595(18) 0.0170(5) Uani 1 1 d . . . . .
C2 C -0.1356(3) 1.1560(2) 0.90412(18) 0.0181(5) Uani 1 1 d . . . . .
H2 H -0.129046 1.239827 0.902755 0.022 Uiso 1 1 calc R . . . .
C3 C -0.2263(2) 1.1207(2) 0.98115(18) 0.0174(5) Uani 1 1 d . . . . .
H3 H -0.282428 1.180661 1.031545 0.021 Uiso 1 1 calc R . . . .
C4 C -0.2383(2) 0.9961(2) 0.98743(18) 0.0166(5) Uani 1 1 d . . . . .
C5 C -0.1568(3) 0.9122(2) 0.90687(18) 0.0191(5) Uani 1 1 d . . . . .
H5 H -0.164805 0.828957 0.907231 0.023 Uiso 1 1 calc R . . . .
C6 C -0.0676(2) 0.9485(2) 0.82939(18) 0.0180(5) Uani 1 1 d . . . . .
H6 H -0.015536 0.890474 0.776387 0.022 Uiso 1 1 calc R . . . .
C7 C 0.0445(2) 1.1084(2) 0.74752(18) 0.0175(5) Uani 1 1 d . . . . .
C8 C -0.3266(2) 0.9571(2) 1.07070(18) 0.0174(5) Uani 1 1 d . . . . .
C9 C 0.1312(3) 1.0232(2) 0.67003(19) 0.0191(5) Uani 1 1 d . . . . .
C10 C 0.0460(2) 1.2372(2) 0.73493(18) 0.0176(5) Uani 1 1 d . . . . .
C11 C -0.4130(3) 1.0426(2) 1.14733(19) 0.0188(5) Uani 1 1 d . . . . .
C12 C -0.3419(3) 0.8329(2) 1.07809(18) 0.0202(5) Uani 1 1 d . . . . .
N1 N 0.2018(2) 0.95098(19) 0.60993(16) 0.0244(5) Uani 1 1 d . . . . .
N2 N 0.0418(2) 1.34331(19) 0.72463(17) 0.0258(5) Uani 1 1 d . . . . .
N3 N -0.4819(2) 1.11266(19) 1.21004(16) 0.0232(5) Uani 1 1 d . . . . .
N4 N -0.3568(3) 0.7340(2) 1.08409(18) 0.0327(5) Uani 1 1 d . . . . .
C21 C 0.7888(3) 0.7266(2) 0.5589(2) 0.0256(6) Uani 1 1 d . . . . .
H21A H 0.854122 0.778904 0.539866 0.031 Uiso 1 1 calc R . . . .
H21B H 0.826009 0.648429 0.517696 0.031 Uiso 1 1 calc R . . . .
C22 C 0.7993(3) 0.6861(2) 0.6842(2) 0.0258(6) Uani 1 1 d . . . . .
H22A H 0.907864 0.632429 0.709078 0.031 Uiso 1 1 calc R . . . .
H22B H 0.764556 0.764288 0.725442 0.031 Uiso 1 1 calc R . . . .
C23 C 0.7072(3) 0.5663(2) 0.8257(2) 0.0282(6) Uani 1 1 d . . . . .
H23A H 0.688720 0.639282 0.872085 0.034 Uiso 1 1 calc R . . . .
H23B H 0.810077 0.498677 0.848698 0.034 Uiso 1 1 calc R . . . .
C24 C 0.5835(3) 0.5099(2) 0.8437(2) 0.0281(6) Uani 1 1 d . . . . .
H24A H 0.594471 0.444227 0.790654 0.034 Uiso 1 1 calc R . . . .
H24B H 0.592307 0.466569 0.922247 0.034 Uiso 1 1 calc R . . . .
C25 C 0.3078(3) 0.5725(2) 0.8210(2) 0.0292(6) Uani 1 1 d . . . . .
H25A H 0.211746 0.645355 0.835763 0.035 Uiso 1 1 calc R . . . .
H25B H 0.323785 0.499728 0.881952 0.035 Uiso 1 1 calc R . . . .
C26 C 0.2887(3) 0.5279(2) 0.7086(2) 0.0282(6) Uani 1 1 d . . . . .
H26A H 0.381453 0.451660 0.694651 0.034 Uiso 1 1 calc R . . . .
H26B H 0.197066 0.502148 0.708085 0.034 Uiso 1 1 calc R . . . .
C27 C 0.2569(3) 0.6028(2) 0.5116(2) 0.0267(6) Uani 1 1 d . . . . .
H27A H 0.157376 0.591180 0.499419 0.032 Uiso 1 1 calc R . . . .
H27B H 0.342642 0.520454 0.499805 0.032 Uiso 1 1 calc R . . . .
C28 C 0.2655(3) 0.7134(2) 0.4303(2) 0.0243(6) Uani 1 1 d . . . . .
H28A H 0.250538 0.698195 0.351254 0.029 Uiso 1 1 calc R . . . .
H28B H 0.183564 0.796647 0.445097 0.029 Uiso 1 1 calc R . . . .
C29 C 0.4326(3) 0.8322(2) 0.3876(2) 0.0259(6) Uani 1 1 d . . . . .
H29A H 0.361420 0.912446 0.416568 0.031 Uiso 1 1 calc R . . . .
H29B H 0.408614 0.837766 0.305507 0.031 Uiso 1 1 calc R . . . .
C30 C 0.5980(3) 0.8186(2) 0.40723(19) 0.0269(6) Uani 1 1 d . . . . .
H30A H 0.668420 0.741858 0.373207 0.032 Uiso 1 1 calc R . . . .
H30B H 0.614213 0.897469 0.371364 0.032 Uiso 1 1 calc R . . . .
O21 O 0.63032(18) 0.80260(15) 0.52680(13) 0.0232(4) Uani 1 1 d . . . . .
O22 O 0.70280(18) 0.61235(15) 0.70822(12) 0.0229(4) Uani 1 1 d . . . . .
O23 O 0.43657(18) 0.61497(15) 0.82362(13) 0.0246(4) Uani 1 1 d . . . . .
O24 O 0.26883(18) 0.63441(15) 0.62351(13) 0.0250(4) Uani 1 1 d . . . . .
O25 O 0.41497(17) 0.71970(15) 0.44669(13) 0.0218(4) 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
Na1 N1 2.499(2) . ?
Na1 N3 2.497(2) 2_577 ?
Na1 O21 2.4192(18) . ?
Na1 O22 2.4012(17) . ?
Na1 O23 2.4733(18) . ?
Na1 O24 2.4496(18) . ?
Na1 O25 2.4602(17) . ?
C1 C2 1.417(3) . ?
C1 C6 1.419(3) . ?
C1 C7 1.412(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.362(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.418(3) . ?
C4 C5 1.424(3) . ?
C4 C8 1.413(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.361(3) . ?
C6 H6 0.9500 . ?
C7 C9 1.419(3) . ?
C7 C10 1.423(3) . ?
C8 C11 1.413(3) . ?
C8 C12 1.426(3) . ?
C9 N1 1.148(3) . ?
C10 N2 1.153(3) . ?
C11 N3 1.151(3) . ?
C12 N4 1.147(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.498(3) . ?
C21 O21 1.429(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 O22 1.424(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.498(4) . ?
C23 O22 1.427(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 O23 1.432(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.503(3) . ?
C25 O23 1.436(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 O24 1.423(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.500(3) . ?
C27 O24 1.425(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 O25 1.427(3) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.501(3) . ?
C29 O25 1.424(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 O21 1.429(3) . ?

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
N3 Na1 N1 79.30(7) 2_577 . ?
O21 Na1 N1 104.10(7) . . ?
O21 Na1 N3 90.59(6) . 2_577 ?
O21 Na1 O23 139.42(6) . . ?
O21 Na1 O24 134.08(6) . . ?
O21 Na1 O25 67.07(6) . . ?
O22 Na1 N1 160.82(7) . . ?
O22 Na1 N3 82.74(6) . 2_577 ?
O22 Na1 O21 69.25(6) . . ?
O22 Na1 O23 70.51(6) . . ?
O22 Na1 O24 113.76(6) . . ?
O22 Na1 O25 106.00(6) . . ?
O23 Na1 N1 112.28(7) . . ?
O23 Na1 N3 79.41(6) . 2_577 ?
O24 Na1 N1 84.04(6) . . ?
O24 Na1 N3 135.06(7) . 2_577 ?
O24 Na1 O23 68.92(6) . . ?
O24 Na1 O25 68.45(6) . . ?
O25 Na1 N1 86.71(6) . . ?
O25 Na1 N3 149.94(7) . 2_577 ?
O25 Na1 O23 130.64(6) . . ?
C2 C1 C6 116.8(2) . . ?
C7 C1 C2 121.4(2) . . ?
C7 C1 C6 121.80(19) . . ?
C1 C2 H2 119.0 . . ?
C3 C2 C1 121.9(2) . . ?
C3 C2 H2 119.0 . . ?
C2 C3 H3 119.4 . . ?
C2 C3 C4 121.2(2) . . ?
C4 C3 H3 119.4 . . ?
C3 C4 C5 117.1(2) . . ?
C8 C4 C3 121.2(2) . . ?
C8 C4 C5 121.7(2) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 C4 121.4(2) . . ?
C6 C5 H5 119.3 . . ?
C1 C6 H6 119.3 . . ?
C5 C6 C1 121.5(2) . . ?
C5 C6 H6 119.3 . . ?
C1 C7 C9 121.5(2) . . ?
C1 C7 C10 121.43(19) . . ?
C9 C7 C10 116.8(2) . . ?
C4 C8 C12 122.3(2) . . ?
C11 C8 C4 121.6(2) . . ?
C11 C8 C12 116.0(2) . . ?
N1 C9 C7 177.8(2) . . ?
N2 C10 C7 177.7(2) . . ?
N3 C11 C8 179.3(2) . . ?
N4 C12 C8 178.9(3) . . ?
C9 N1 Na1 130.77(17) . . ?
C11 N3 Na1 140.49(17) . 2_577 ?
H21A C21 H21B 108.4 . . ?
C22 C21 H21A 110.1 . . ?
C22 C21 H21B 110.1 . . ?
O21 C21 H21A 110.1 . . ?
O21 C21 H21B 110.1 . . ?
O21 C21 C22 108.06(18) . . ?
C21 C22 H22A 110.0 . . ?
C21 C22 H22B 110.0 . . ?
H22A C22 H22B 108.4 . . ?
O22 C22 C21 108.35(19) . . ?
O22 C22 H22A 110.0 . . ?
O22 C22 H22B 110.0 . . ?
H23A C23 H23B 108.4 . . ?
C24 C23 H23A 110.1 . . ?
C24 C23 H23B 110.1 . . ?
O22 C23 H23A 110.1 . . ?
O22 C23 H23B 110.1 . . ?
O22 C23 C24 108.11(19) . . ?
C23 C24 H24A 110.2 . . ?
C23 C24 H24B 110.2 . . ?
H24A C24 H24B 108.5 . . ?
O23 C24 C23 107.73(19) . . ?
O23 C24 H24A 110.2 . . ?
O23 C24 H24B 110.2 . . ?
H25A C25 H25B 107.9 . . ?
C26 C25 H25A 109.2 . . ?
C26 C25 H25B 109.2 . . ?
O23 C25 H25A 109.2 . . ?
O23 C25 H25B 109.2 . . ?
O23 C25 C26 111.84(19) . . ?
C25 C26 H26A 110.2 . . ?
C25 C26 H26B 110.2 . . ?
H26A C26 H26B 108.5 . . ?
O24 C26 C25 107.36(19) . . ?
O24 C26 H26A 110.2 . . ?
O24 C26 H26B 110.2 . . ?
H27A C27 H27B 108.5 . . ?
C28 C27 H27A 110.2 . . ?
C28 C27 H27B 110.2 . . ?
O24 C27 H27A 110.2 . . ?
O24 C27 H27B 110.2 . . ?
O24 C27 C28 107.52(19) . . ?
C27 C28 H28A 110.2 . . ?
C27 C28 H28B 110.2 . . ?
H28A C28 H28B 108.5 . . ?
O25 C28 C27 107.58(18) . . ?
O25 C28 H28A 110.2 . . ?
O25 C28 H28B 110.2 . . ?
H29A C29 H29B 108.5 . . ?
C30 C29 H29A 110.3 . . ?
C30 C29 H29B 110.3 . . ?
O25 C29 H29A 110.3 . . ?
O25 C29 H29B 110.3 . . ?
O25 C29 C30 107.13(18) . . ?
C29 C30 H30A 110.0 . . ?
C29 C30 H30B 110.0 . . ?
H30A C30 H30B 108.4 . . ?
O21 C30 C29 108.39(19) . . ?
O21 C30 H30A 110.0 . . ?
O21 C30 H30B 110.0 . . ?
C21 O21 Na1 114.94(13) . . ?
C30 O21 Na1 116.12(13) . . ?
C30 O21 C21 113.34(17) . . ?
C22 O22 Na1 107.11(13) . . ?
C22 O22 C23 112.86(18) . . ?
C23 O22 Na1 110.00(13) . . ?
C24 O23 Na1 108.95(13) . . ?
C24 O23 C25 113.64(18) . . ?
C25 O23 Na1 111.26(13) . . ?
C26 O24 Na1 114.82(14) . . ?
C26 O24 C27 113.07(17) . . ?
C27 O24 Na1 114.58(13) . . ?
C28 O25 Na1 107.69(12) . . ?
C29 O25 Na1 102.12(13) . . ?
C29 O25 C28 114.12(17) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 0.8(3) . . . . ?
C2 C1 C6 C5 -2.3(3) . . . . ?
C2 C1 C7 C9 179.2(2) . . . . ?
C2 C1 C7 C10 -7.1(3) . . . . ?
C2 C3 C4 C5 -2.5(3) . . . . ?
C2 C3 C4 C8 177.0(2) . . . . ?
C3 C4 C5 C6 1.8(3) . . . . ?
C3 C4 C8 C11 3.3(3) . . . . ?
C3 C4 C8 C12 179.3(2) . . . . ?
C4 C5 C6 C1 0.6(3) . . . . ?
C5 C4 C8 C11 -177.2(2) . . . . ?
C5 C4 C8 C12 -1.1(3) . . . . ?
C6 C1 C2 C3 1.7(3) . . . . ?
C6 C1 C7 C9 -1.6(3) . . . . ?
C6 C1 C7 C10 172.1(2) . . . . ?
C7 C1 C2 C3 -179.2(2) . . . . ?
C7 C1 C6 C5 178.5(2) . . . . ?
C8 C4 C5 C6 -177.7(2) . . . . ?
C21 C22 O22 Na1 -60.13(19) . . . . ?
C21 C22 O22 C23 178.66(18) . . . . ?
C22 C21 O21 Na1 -27.9(2) . . . . ?
C22 C21 O21 C30 -164.71(19) . . . . ?
C23 C24 O23 Na1 46.4(2) . . . . ?
C23 C24 O23 C25 171.05(18) . . . . ?
C24 C23 O22 Na1 51.3(2) . . . . ?
C24 C23 O22 C22 170.88(18) . . . . ?
C25 C26 O24 Na1 43.1(2) . . . . ?
C25 C26 O24 C27 177.11(19) . . . . ?
C26 C25 O23 Na1 43.5(2) . . . . ?
C26 C25 O23 C24 -80.0(2) . . . . ?
C27 C28 O25 Na1 -58.44(19) . . . . ?
C27 C28 O25 C29 -171.03(18) . . . . ?
C28 C27 O24 Na1 -35.8(2) . . . . ?
C28 C27 O24 C26 -169.96(19) . . . . ?
C29 C30 O21 Na1 14.0(2) . . . . ?
C29 C30 O21 C21 150.29(19) . . . . ?
C30 C29 O25 Na1 68.04(17) . . . . ?
C30 C29 O25 C28 -176.07(18) . . . . ?
O21 C21 C22 O22 59.2(2) . . . . ?
O22 C23 C24 O23 -67.3(2) . . . . ?
O23 C25 C26 O24 -57.9(2) . . . . ?
O24 C27 C28 O25 63.7(2) . . . . ?
O25 C29 C30 O21 -56.3(2) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.749
_oxdiff_exptl_absorpt_empirical_full_min 0.726
####################################################################### 
# 
# 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_4_5NaT2
_database_code_depnum_ccdc_archive 'CCDC 1866255'
loop_
_audit_author_name
_audit_author_address
'Bingjia Yan'
;University of Southampton
China
;
_audit_update_record             
;
2018-09-06 deposited with the CCDC.	2019-04-30 downloaded from the CCDC.
;

#2013by034

_audit_creation_date             2018-09-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H22 Na O6, 2(C12 H4 N4)'
_chemical_formula_sum            'C34 H30 N8 Na O6'
_chemical_formula_weight         669.65
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C34 H30 N8 Na O6'
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'
Na Na 0.0362 0.0249 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.3408(4)
_cell_length_b                   12.4515(6)
_cell_length_c                   16.7083(9)
_cell_angle_alpha                102.611(4)
_cell_angle_beta                 92.029(4)
_cell_angle_gamma                99.896(4)
_cell_volume                     1663.38(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5391
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.8150
_cell_measurement_theta_min      2.3150
_shelx_estimated_absorpt_T_max   0.998
_shelx_estimated_absorpt_T_min   0.983
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             698
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11862
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         1.872
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -31.00  73.00   1.00   35.00    --  -17.00  72.00 150.00  104
  2  ω    -69.00  22.00   1.00   35.00    --  -17.00 -72.00  30.00   91
  3  ω    -69.00  22.00   1.00   35.00    --  -17.00 -72.00-150.00   91
  4  ω    -58.00  26.00   1.00   35.00    --  -17.00   0.00   0.00   84
  5  ω    -21.00  -1.00   1.00   35.00    --  -17.00  54.00 -30.00   20
  6  ω    -31.00  73.00   1.00   35.00    --  -17.00  72.00  90.00  104
  7  ω    -69.00   0.00   1.00   35.00    --  -17.00 -72.00 -30.00   69
;
_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  
'Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0450675000
_diffrn_orient_matrix_UB_12      0.0083918000
_diffrn_orient_matrix_UB_13      -0.0342001000
_diffrn_orient_matrix_UB_21      0.0525593000
_diffrn_orient_matrix_UB_22      -0.0266269000
_diffrn_orient_matrix_UB_23      -0.0269117000
_diffrn_orient_matrix_UB_31      -0.0519762000
_diffrn_orient_matrix_UB_32      -0.0524179000
_diffrn_orient_matrix_UB_33      -0.0030722000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8612
_reflns_number_total             11862
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         11862
_refine_ls_number_restraints     1430
_refine_ls_R_factor_all          0.1466
_refine_ls_R_factor_gt           0.1083
_refine_ls_restrained_S_all      1.169
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0241P)²+3.5166P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1871
_refine_ls_wR_factor_ref         0.2025
_refine_special_details          
'Crystal used was a non-merohedral twin (80:20 at 180degrees about reciprocal axis 0 0 1). There is disorder of the 15-crown-5. As such various geomtrical (SADI, SAME) and displacement (SIMU, RIGU) restraints were employed.,Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.8002
 0.1998
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 C607-O604 \\sim C607-O704
 with sigma of 0.03
 O604-Na1 \\sim O704-Na1
 with sigma of 0.03
 C605-O604 \\sim C605-O704
 with sigma of 0.06
 C605-C606 \\sim C605-C706
 with sigma of 0.03
 C606-O604 \\sim C706-O704
 with sigma of 0.03
 C606-C607 \\sim C706-C607
 with sigma of 0.06
 C706-C605 \\sim C606-C605
 with sigma of 0.03
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{C301, C302, C303, C304, C305, C306, C307, C308, C309, C310, O301, O302, O303,
O304, O305} sigma for 1-2: 0.01, 1-3: 0.04
as
{C601, C602, C603, C604, C605, C606, C607, C608, C609, C610, O601, O602, O603,
O604, O605}
7. Others
 1*[Sof(C301)+Sof(H30A)+Sof(H30B)+Sof(C302)+Sof(H30C)+Sof(H30D)+Sof(C303)+
 Sof(H30E)+Sof(H30F)+Sof(C304)+Sof(H30G)+Sof(H30H)+Sof(C305)+Sof(H30I)+
 Sof(H30J)+Sof(C306)+Sof(H30K)+Sof(H30L)+Sof(C307)+Sof(H30M)+Sof(H30N)+
 Sof(C308)+Sof(H30O)+Sof(H30P)+Sof(C309)+Sof(H30Q)+Sof(H30R)+Sof(C310)+
 Sof(H31A)+Sof(H31B)+Sof(O301)+Sof(O302)+Sof(O303)+Sof(O304)+Sof(O305)+
 Sof(C601)+Sof(H60A)+Sof(H60B)+Sof(C602)+Sof(H60C)+Sof(H60D)+Sof(C603)+
 Sof(H60E)+Sof(H60F)+Sof(C604)+Sof(H60G)+Sof(H60H)+Sof(C605)+Sof(C607)+
 Sof(C608)+Sof(H60S)+Sof(H60T)+Sof(C609)+Sof(H60U)+Sof(H60V)+Sof(C610)+
 Sof(H61A)+Sof(H61B)+Sof(O601)+Sof(O602)+Sof(O603)+Sof(O605)]+1*[Sof(H60I)+
 Sof(H60J)+Sof(C606)+Sof(H60M)+Sof(H60N)+Sof(H60O)+Sof(H60P)+Sof(O604)]+1*
 [Sof(H60K)+Sof(H60L)+Sof(H60Q)+Sof(H60R)+Sof(O704)+Sof(C706)+Sof(H70A)+
 Sof(H70B)]=1 with esd of 0.00001
 Sof(C601)=Sof(H60A)=Sof(H60B)=Sof(C602)=Sof(H60C)=Sof(H60D)=Sof(C603)=
 Sof(H60E)=Sof(H60F)=Sof(C604)=Sof(H60G)=Sof(H60H)=Sof(C605)=Sof(C607)=
 Sof(C608)=Sof(H60S)=Sof(H60T)=Sof(C609)=Sof(H60U)=Sof(H60V)=Sof(C610)=
 Sof(H61A)=Sof(H61B)=Sof(O601)=Sof(O602)=Sof(O603)=Sof(O605)=1-FVAR(1)
 Sof(C301)=Sof(H30A)=Sof(H30B)=Sof(C302)=Sof(H30C)=Sof(H30D)=Sof(C303)=
 Sof(H30E)=Sof(H30F)=Sof(C304)=Sof(H30G)=Sof(H30H)=Sof(C305)=Sof(H30I)=
 Sof(H30J)=Sof(C306)=Sof(H30K)=Sof(H30L)=Sof(C307)=Sof(H30M)=Sof(H30N)=
 Sof(C308)=Sof(H30O)=Sof(H30P)=Sof(C309)=Sof(H30Q)=Sof(H30R)=Sof(C310)=
 Sof(H31A)=Sof(H31B)=Sof(O301)=Sof(O302)=Sof(O303)=Sof(O304)=Sof(O305)=FVAR(1)
 Sof(H60I)=Sof(H60J)=Sof(C606)=Sof(H60M)=Sof(H60N)=Sof(H60O)=Sof(H60P)=
 Sof(O604)=FVAR(2)
 Sof(H60K)=Sof(H60L)=Sof(H60Q)=Sof(H60R)=Sof(O704)=Sof(C706)=Sof(H70A)=
 Sof(H70B)=FVAR(3)
8.a Secondary CH2 refined with riding coordinates:
 C301(H30A,H30B), C302(H30C,H30D), C303(H30E,H30F), C304(H30G,H30H), C305(H30I,
 H30J), C306(H30K,H30L), C307(H30M,H30N), C308(H30O,H30P), C309(H30Q,H30R),
 C310(H31A,H31B), C601(H60A,H60B), C602(H60C,H60D), C603(H60E,H60F), C604(H60G,
 H60H), C605(H60I,H60J), C605(H60K,H60L), C606(H60M,H60N), C607(H60O,H60P),
 C607(H60Q,H60R), C608(H60S,H60T), C609(H60U,H60V), C610(H61A,H61B), C706(H70A,
 H70B)
8.b Aromatic/amide H refined with riding coordinates:
 C102(H102), C103(H103), C105(H105), C106(H106), C202(H202), C203(H203),
 C205(H205), C206(H206)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C301 C 0.2764(11) 0.6652(6) -0.1809(5) 0.0308(16) Uani 0.741(3) 1 d D U P A 1
H30A H 0.262856 0.615785 -0.236782 0.037 Uiso 0.741(3) 1 calc R . P A 1
H30B H 0.389003 0.670461 -0.157628 0.037 Uiso 0.741(3) 1 calc R . P A 1
C302 C 0.2458(11) 0.7797(6) -0.1849(4) 0.0310(18) Uani 0.741(3) 1 d D U P A 1
H30C H 0.317090 0.810663 -0.223668 0.037 Uiso 0.741(3) 1 calc R . P A 1
H30D H 0.130711 0.775309 -0.204019 0.037 Uiso 0.741(3) 1 calc R . P A 1
C303 C 0.2197(16) 0.9515(7) -0.0942(5) 0.047(2) Uani 0.741(3) 1 d D U P A 1
H30E H 0.099300 0.935522 -0.103748 0.056 Uiso 0.741(3) 1 calc R . P A 1
H30F H 0.265589 0.994282 -0.134255 0.056 Uiso 0.741(3) 1 calc R . P A 1
C304 C 0.2704(12) 1.0179(6) -0.0076(5) 0.050(2) Uani 0.741(3) 1 d D U P A 1
H30G H 0.390834 1.033964 0.001838 0.060 Uiso 0.741(3) 1 calc R . P A 1
H30H H 0.231035 1.089952 0.001847 0.060 Uiso 0.741(3) 1 calc R . P A 1
C305 C 0.2739(13) 0.9888(7) 0.1283(6) 0.031(2) Uani 0.741(3) 1 d D U P A 1
H30I H 0.238760 1.058620 0.156401 0.037 Uiso 0.741(3) 1 calc R . P A 1
H30J H 0.394175 1.004004 0.127454 0.037 Uiso 0.741(3) 1 calc R . P A 1
C306 C 0.2218(10) 0.8976(6) 0.1730(5) 0.0349(16) Uani 0.741(3) 1 d D U P A 1
H30K H 0.262012 0.922156 0.231778 0.042 Uiso 0.741(3) 1 calc R . P A 1
H30L H 0.101404 0.876075 0.169105 0.042 Uiso 0.741(3) 1 calc R . P A 1
C307 C 0.2572(14) 0.7087(8) 0.1639(5) 0.046(2) Uani 0.741(3) 1 d D U P A 1
H30M H 0.137860 0.687986 0.166801 0.055 Uiso 0.741(3) 1 calc R . P A 1
H30N H 0.310883 0.722143 0.219943 0.055 Uiso 0.741(3) 1 calc R . P A 1
C308 C 0.3201(15) 0.6162(8) 0.1059(6) 0.042(2) Uani 0.741(3) 1 d D U P A 1
H30O H 0.438030 0.638983 0.100221 0.050 Uiso 0.741(3) 1 calc R . P A 1
H30P H 0.303654 0.547100 0.127087 0.050 Uiso 0.741(3) 1 calc R . P A 1
C309 C 0.2975(12) 0.5333(7) -0.0374(5) 0.038(2) Uani 0.741(3) 1 d D U P A 1
H30Q H 0.307601 0.459818 -0.026096 0.045 Uiso 0.741(3) 1 calc R . P A 1
H30R H 0.407420 0.572581 -0.045228 0.045 Uiso 0.741(3) 1 calc R . P A 1
C310 C 0.1854(10) 0.5169(7) -0.1135(5) 0.0317(19) Uani 0.741(3) 1 d D U P A 1
H31A H 0.232341 0.474160 -0.161161 0.038 Uiso 0.741(3) 1 calc R . P A 1
H31B H 0.078572 0.472513 -0.106453 0.038 Uiso 0.741(3) 1 calc R . P A 1
O301 O 0.1612(5) 0.6213(3) -0.1299(2) 0.0275(9) Uani 0.741(3) 1 d D U P A 1
O302 O 0.2809(6) 0.8495(4) -0.1038(3) 0.0311(10) Uani 0.741(3) 1 d D U P A 1
O303 O 0.2000(7) 0.9523(4) 0.0470(3) 0.0345(12) Uani 0.741(3) 1 d D U P A 1
O304 O 0.2945(6) 0.8058(4) 0.1321(3) 0.0356(11) Uani 0.741(3) 1 d D U P A 1
O305 O 0.2302(6) 0.5977(4) 0.0292(3) 0.0350(11) Uani 0.741(3) 1 d D U P A 1
C601 C 0.242(3) 0.5346(19) -0.1235(11) 0.038(6) Uani 0.259(3) 1 d D U P A 2
H60A H 0.121822 0.512220 -0.124414 0.046 Uiso 0.259(3) 1 calc R . P A 2
H60B H 0.287688 0.467589 -0.147800 0.046 Uiso 0.259(3) 1 calc R . P A 2
C602 C 0.284(4) 0.6234(16) -0.1715(15) 0.042(5) Uani 0.259(3) 1 d D U P A 2
H60C H 0.404087 0.647453 -0.168724 0.051 Uiso 0.259(3) 1 calc R . P A 2
H60D H 0.243907 0.593294 -0.229916 0.051 Uiso 0.259(3) 1 calc R . P A 2
C603 C 0.273(4) 0.8155(14) -0.1645(15) 0.044(6) Uani 0.259(3) 1 d D U P A 2
H60E H 0.231374 0.808054 -0.222112 0.053 Uiso 0.259(3) 1 calc R . P A 2
H60F H 0.393431 0.827970 -0.161763 0.053 Uiso 0.259(3) 1 calc R . P A 2
C604 C 0.216(4) 0.912(2) -0.1087(11) 0.046(6) Uani 0.259(3) 1 d D U P A 2
H60G H 0.250739 0.981801 -0.127353 0.056 Uiso 0.259(3) 1 calc R . P A 2
H60H H 0.095689 0.897131 -0.108666 0.056 Uiso 0.259(3) 1 calc R . P A 2
C605 C 0.235(3) 0.9986(19) 0.0344(11) 0.041(5) Uani 0.259(3) 1 d D U P A 2
H60I H 0.115606 0.978301 0.035333 0.049 Uiso 0.172(3) 1 calc R . P B 3
H60J H 0.260706 1.074047 0.022639 0.049 Uiso 0.172(3) 1 calc R . P B 3
H60K H 0.116473 0.989445 0.021449 0.049 Uiso 0.087(3) 1 calc R . P C 4
H60L H 0.283777 1.073189 0.025662 0.049 Uiso 0.087(3) 1 calc R . P C 4
C606 C 0.315(6) 1.0018(19) 0.1171(17) 0.048(7) Uani 0.172(3) 1 d D U P A 3
H60M H 0.428050 1.044568 0.122801 0.058 Uiso 0.172(3) 1 calc R . P B 3
H60N H 0.253979 1.040029 0.160960 0.058 Uiso 0.172(3) 1 calc R . P B 3
C607 C 0.225(3) 0.8550(18) 0.1887(14) 0.049(5) Uani 0.259(3) 1 d D U P A 2
H60O H 0.106797 0.844103 0.174002 0.059 Uiso 0.172(3) 1 calc R . P B 3
H60P H 0.253074 0.909647 0.242133 0.059 Uiso 0.172(3) 1 calc R . P B 3
H60Q H 0.137313 0.859262 0.226745 0.059 Uiso 0.087(3) 1 calc R . P C 4
H60R H 0.319083 0.912461 0.217072 0.059 Uiso 0.087(3) 1 calc R . P C 4
C608 C 0.278(5) 0.7452(17) 0.1911(13) 0.054(6) Uani 0.259(3) 1 d D U P A 2
H60S H 0.398078 0.756337 0.198698 0.065 Uiso 0.259(3) 1 calc R . P A 2
H60T H 0.231207 0.716533 0.237750 0.065 Uiso 0.259(3) 1 calc R . P A 2
C609 C 0.309(4) 0.578(2) 0.1018(13) 0.043(6) Uani 0.259(3) 1 d D U P A 2
H60U H 0.282100 0.529621 0.141122 0.051 Uiso 0.259(3) 1 calc R . P A 2
H60V H 0.428091 0.607453 0.108722 0.051 Uiso 0.259(3) 1 calc R . P A 2
C610 C 0.260(2) 0.5122(13) 0.0147(10) 0.035(4) Uani 0.259(3) 1 d D U P A 2
H61A H 0.311834 0.445195 0.003314 0.042 Uiso 0.259(3) 1 calc R . P A 2
H61B H 0.140041 0.486773 0.007609 0.042 Uiso 0.259(3) 1 calc R . P A 2
O601 O 0.310(2) 0.5808(11) -0.0416(9) 0.034(3) Uani 0.259(3) 1 d D U P A 2
O602 O 0.2094(15) 0.7167(10) -0.1367(7) 0.034(3) Uani 0.259(3) 1 d D U P A 2
O603 O 0.2890(17) 0.9213(10) -0.0284(7) 0.040(3) Uani 0.259(3) 1 d D U P A 2
O604 O 0.318(3) 0.8904(14) 0.1262(10) 0.048(4) Uani 0.172(3) 1 d D U P A 3
O605 O 0.2210(18) 0.6673(10) 0.1161(8) 0.038(3) Uani 0.259(3) 1 d D U P A 2
Na1 Na 0.1650(3) 0.75489(16) -0.00313(12) 0.0413(5) Uani 1 1 d D U . . .
O401 O -0.1044(6) 0.7266(4) 0.0061(3) 0.0598(12) Uani 1 1 d . U . . .
H40A H -0.156(9) 0.728(6) -0.042(5) 0.090 Uiso 1 1 d R . . . .
H40B H -0.151(9) 0.750(6) 0.050(5) 0.090 Uiso 1 1 d R . . . .
C101 C -0.2748(5) 0.6278(3) -0.3686(3) 0.0206(8) Uani 1 1 d . U . . .
C102 C -0.2539(5) 0.5626(3) -0.4487(3) 0.0191(8) Uani 1 1 d . U . . .
H102 H -0.189789 0.505722 -0.453313 0.023 Uiso 1 1 calc R . . . .
C103 C -0.3236(5) 0.5807(3) -0.5173(3) 0.0184(8) Uani 1 1 d . U . . .
H103 H -0.308148 0.536237 -0.569437 0.022 Uiso 1 1 calc R . . . .
C104 C -0.4208(5) 0.6662(3) -0.5130(2) 0.0189(8) Uani 1 1 d . U . . .
C105 C -0.4400(5) 0.7324(3) -0.4333(3) 0.0212(9) Uani 1 1 d . U . . .
H105 H -0.502599 0.790036 -0.428823 0.025 Uiso 1 1 calc R . . . .
C106 C -0.3704(5) 0.7139(3) -0.3645(3) 0.0207(8) Uani 1 1 d . U . . .
H106 H -0.385123 0.758829 -0.312427 0.025 Uiso 1 1 calc R . . . .
C107 C -0.2080(5) 0.6053(4) -0.2977(3) 0.0251(9) Uani 1 1 d . U . . .
C108 C -0.4935(5) 0.6853(3) -0.5835(3) 0.0206(9) Uani 1 1 d . U . . .
C109 C -0.1188(6) 0.5161(4) -0.3001(3) 0.0257(9) Uani 1 1 d . U . . .
C110 C -0.2357(6) 0.6645(4) -0.2177(3) 0.0278(10) Uani 1 1 d . U . . .
C111 C -0.5905(5) 0.7707(3) -0.5804(3) 0.0207(9) Uani 1 1 d . U . . .
C112 C -0.4778(5) 0.6208(3) -0.6640(3) 0.0219(9) Uani 1 1 d . U . . .
N101 N -0.0499(5) 0.4436(3) -0.3021(2) 0.0358(10) Uani 1 1 d . U . . .
N102 N -0.2596(6) 0.7107(4) -0.1535(3) 0.0421(11) Uani 1 1 d . U . . .
N103 N -0.6662(4) 0.8402(3) -0.5788(2) 0.0284(9) Uani 1 1 d . U . . .
N104 N -0.4676(5) 0.5691(3) -0.7287(2) 0.0318(9) Uani 1 1 d . U . . .
C201 C -0.2250(5) 0.8678(3) 0.3716(3) 0.0209(8) Uani 1 1 d . U . . .
C202 C -0.2415(5) 0.9342(3) 0.4516(3) 0.0195(8) Uani 1 1 d . U . . .
H202 H -0.304458 0.991690 0.456509 0.023 Uiso 1 1 calc R . . . .
C203 C -0.1693(5) 0.9165(3) 0.5198(3) 0.0205(9) Uani 1 1 d . U . . .
H203 H -0.183092 0.961329 0.572033 0.025 Uiso 1 1 calc R . . . .
C204 C -0.0722(5) 0.8311(3) 0.5148(3) 0.0200(8) Uani 1 1 d . U . . .
C205 C -0.0552(5) 0.7649(3) 0.4351(3) 0.0200(8) Uani 1 1 d . U . . .
H205 H 0.007605 0.707263 0.430080 0.024 Uiso 1 1 calc R . . . .
C206 C -0.1270(5) 0.7830(3) 0.3668(3) 0.0224(9) Uani 1 1 d . U . . .
H206 H -0.112282 0.738748 0.314524 0.027 Uiso 1 1 calc R . . . .
C207 C -0.2965(5) 0.8888(3) 0.3015(3) 0.0238(9) Uani 1 1 d . U . . .
C208 C 0.0022(5) 0.8121(3) 0.5855(3) 0.0200(8) Uani 1 1 d . U . . .
C209 C -0.3859(5) 0.9771(4) 0.3052(3) 0.0236(9) Uani 1 1 d . U . . .
C210 C -0.2765(6) 0.8263(4) 0.2209(3) 0.0288(10) Uani 1 1 d . U . . .
C211 C 0.0979(5) 0.7263(3) 0.5827(3) 0.0227(9) Uani 1 1 d . U . . .
C212 C -0.0108(5) 0.8786(4) 0.6654(3) 0.0248(9) Uani 1 1 d . U . . .
N201 N -0.4551(5) 1.0498(3) 0.3080(2) 0.0334(9) Uani 1 1 d . U . . .
N202 N -0.2592(6) 0.7767(4) 0.1565(3) 0.0389(10) Uani 1 1 d . U . . .
N203 N 0.1715(4) 0.6562(3) 0.5819(2) 0.0294(9) Uani 1 1 d . U . . .
N204 N -0.0199(5) 0.9314(3) 0.7296(2) 0.0329(9) Uani 1 1 d . U . . .
O704 O 0.173(5) 0.898(3) 0.1258(18) 0.035(5) Uani 0.087(3) 1 d D U P A 4
C706 C 0.257(15) 1.009(5) 0.125(3) 0.043(9) Uani 0.087(3) 1 d D U P A 4
H70A H 0.372760 1.022223 0.145668 0.052 Uiso 0.087(3) 1 calc R . P C 4
H70B H 0.202240 1.067729 0.156715 0.052 Uiso 0.087(3) 1 calc R . P C 4


_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
C301 H30A 0.9900 . ?
C301 H30B 0.9900 . ?
C301 C302 1.505(10) . ?
C301 O301 1.425(8) . ?
C302 H30C 0.9900 . ?
C302 H30D 0.9900 . ?
C302 O302 1.430(8) . ?
C303 H30E 0.9900 . ?
C303 H30F 0.9900 . ?
C303 C304 1.507(11) . ?
C303 O302 1.429(8) . ?
C304 H30G 0.9900 . ?
C304 H30H 0.9900 . ?
C304 O303 1.429(9) . ?
C305 H30I 0.9900 . ?
C305 H30J 0.9900 . ?
C305 C306 1.503(12) . ?
C305 O303 1.417(9) . ?
C306 H30K 0.9900 . ?
C306 H30L 0.9900 . ?
C306 O304 1.438(8) . ?
C307 H30M 0.9900 . ?
C307 H30N 0.9900 . ?
C307 C308 1.516(13) . ?
C307 O304 1.417(10) . ?
C308 H30O 0.9900 . ?
C308 H30P 0.9900 . ?
C308 O305 1.415(9) . ?
C309 H30Q 0.9900 . ?
C309 H30R 0.9900 . ?
C309 C310 1.507(11) . ?
C309 O305 1.416(9) . ?
C310 H31A 0.9900 . ?
C310 H31B 0.9900 . ?
C310 O301 1.430(9) . ?
O301 Na1 2.387(4) . ?
O302 Na1 2.396(5) . ?
O303 Na1 2.380(5) . ?
O304 Na1 2.374(5) . ?
O305 Na1 2.286(5) . ?
C601 H60A 0.9900 . ?
C601 H60B 0.9900 . ?
C601 C602 1.504(15) . ?
C601 O601 1.418(14) . ?
C602 H60C 0.9900 . ?
C602 H60D 0.9900 . ?
C602 O602 1.434(13) . ?
C603 H60E 0.9900 . ?
C603 H60F 0.9900 . ?
C603 C604 1.505(16) . ?
C603 O602 1.432(14) . ?
C604 H60G 0.9900 . ?
C604 H60H 0.9900 . ?
C604 O603 1.425(14) . ?
C605 H60I 0.9900 . ?
C605 H60J 0.9900 . ?
C605 H60K 0.9900 . ?
C605 H60L 0.9900 . ?
C605 C606 1.503(18) . ?
C605 O603 1.402(14) . ?
C605 C706 1.50(4) . ?
C606 H60M 0.9900 . ?
C606 H60N 0.9900 . ?
C606 O604 1.432(15) . ?
C607 H60O 0.9900 . ?
C607 H60P 0.9900 . ?
C607 H60Q 0.9900 . ?
C607 H60R 0.9900 . ?
C607 C608 1.513(17) . ?
C607 O604 1.419(15) . ?
C607 O704 1.37(3) . ?
C608 H60S 0.9900 . ?
C608 H60T 0.9900 . ?
C608 O605 1.415(14) . ?
C609 H60U 0.9900 . ?
C609 H60V 0.9900 . ?
C609 C610 1.510(16) . ?
C609 O605 1.419(14) . ?
C610 H61A 0.9900 . ?
C610 H61B 0.9900 . ?
C610 O601 1.430(13) . ?
O601 Na1 2.628(16) . ?
O602 Na1 2.237(12) . ?
O603 Na1 2.284(13) . ?
O604 Na1 2.571(18) . ?
O605 Na1 2.537(14) . ?
Na1 O401 2.230(5) . ?
Na1 H40A 2.68(8) . ?
Na1 O704 2.47(3) . ?
O401 H40A 0.90(8) . ?
O401 H40B 0.85(8) . ?
C101 C102 1.440(6) . ?
C101 C106 1.435(5) . ?
C101 C107 1.393(6) . ?
C102 H102 0.9500 . ?
C102 C103 1.347(6) . ?
C103 H103 0.9500 . ?
C103 C104 1.436(5) . ?
C104 C105 1.435(6) . ?
C104 C108 1.390(6) . ?
C105 H105 0.9500 . ?
C105 C106 1.351(6) . ?
C106 H106 0.9500 . ?
C107 C109 1.433(6) . ?
C107 C110 1.426(6) . ?
C108 C111 1.437(6) . ?
C108 C112 1.431(6) . ?
C109 N101 1.146(5) . ?
C110 N102 1.143(6) . ?
C111 N103 1.152(5) . ?
C112 N104 1.146(5) . ?
C201 C202 1.434(6) . ?
C201 C206 1.432(5) . ?
C201 C207 1.390(6) . ?
C202 H202 0.9500 . ?
C202 C203 1.348(6) . ?
C203 H203 0.9500 . ?
C203 C204 1.435(5) . ?
C204 C205 1.432(6) . ?
C204 C208 1.398(6) . ?
C205 H205 0.9500 . ?
C205 C206 1.350(6) . ?
C206 H206 0.9500 . ?
C207 C209 1.423(6) . ?
C207 C210 1.432(6) . ?
C208 C211 1.434(6) . ?
C208 C212 1.427(6) . ?
C209 N201 1.148(5) . ?
C210 N202 1.144(6) . ?
C211 N203 1.148(5) . ?
C212 N204 1.142(6) . ?
O704 C706 1.43(4) . ?
C706 H70A 0.9900 . ?
C706 H70B 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
H30A C301 H30B 108.5 . . ?
C302 C301 H30A 110.2 . . ?
C302 C301 H30B 110.2 . . ?
O301 C301 H30A 110.2 . . ?
O301 C301 H30B 110.2 . . ?
O301 C301 C302 107.6(6) . . ?
C301 C302 H30C 110.2 . . ?
C301 C302 H30D 110.2 . . ?
H30C C302 H30D 108.5 . . ?
O302 C302 C301 107.5(6) . . ?
O302 C302 H30C 110.2 . . ?
O302 C302 H30D 110.2 . . ?
H30E C303 H30F 108.5 . . ?
C304 C303 H30E 110.3 . . ?
C304 C303 H30F 110.3 . . ?
O302 C303 H30E 110.3 . . ?
O302 C303 H30F 110.3 . . ?
O302 C303 C304 107.3(7) . . ?
C303 C304 H30G 110.2 . . ?
C303 C304 H30H 110.2 . . ?
H30G C304 H30H 108.5 . . ?
O303 C304 C303 107.6(7) . . ?
O303 C304 H30G 110.2 . . ?
O303 C304 H30H 110.2 . . ?
H30I C305 H30J 108.4 . . ?
C306 C305 H30I 110.1 . . ?
C306 C305 H30J 110.1 . . ?
O303 C305 H30I 110.1 . . ?
O303 C305 H30J 110.1 . . ?
O303 C305 C306 107.9(7) . . ?
C305 C306 H30K 110.8 . . ?
C305 C306 H30L 110.8 . . ?
H30K C306 H30L 108.9 . . ?
O304 C306 C305 104.7(7) . . ?
O304 C306 H30K 110.8 . . ?
O304 C306 H30L 110.8 . . ?
H30M C307 H30N 108.6 . . ?
C308 C307 H30M 110.4 . . ?
C308 C307 H30N 110.4 . . ?
O304 C307 H30M 110.4 . . ?
O304 C307 H30N 110.4 . . ?
O304 C307 C308 106.7(8) . . ?
C307 C308 H30O 110.4 . . ?
C307 C308 H30P 110.4 . . ?
H30O C308 H30P 108.6 . . ?
O305 C308 C307 106.7(7) . . ?
O305 C308 H30O 110.4 . . ?
O305 C308 H30P 110.4 . . ?
H30Q C309 H30R 108.4 . . ?
C310 C309 H30Q 110.1 . . ?
C310 C309 H30R 110.1 . . ?
O305 C309 H30Q 110.1 . . ?
O305 C309 H30R 110.1 . . ?
O305 C309 C310 108.0(7) . . ?
C309 C310 H31A 109.2 . . ?
C309 C310 H31B 109.2 . . ?
H31A C310 H31B 107.9 . . ?
O301 C310 C309 111.9(6) . . ?
O301 C310 H31A 109.2 . . ?
O301 C310 H31B 109.2 . . ?
C301 O301 C310 114.2(5) . . ?
C301 O301 Na1 109.9(4) . . ?
C310 O301 Na1 109.5(4) . . ?
C302 O302 Na1 111.1(4) . . ?
C303 O302 C302 113.1(6) . . ?
C303 O302 Na1 107.2(5) . . ?
C304 O303 Na1 115.4(4) . . ?
C305 O303 C304 113.3(6) . . ?
C305 O303 Na1 112.8(4) . . ?
C306 O304 Na1 104.1(4) . . ?
C307 O304 C306 114.0(6) . . ?
C307 O304 Na1 105.3(5) . . ?
C308 O305 C309 114.3(7) . . ?
C308 O305 Na1 114.9(4) . . ?
C309 O305 Na1 111.2(4) . . ?
H60A C601 H60B 108.5 . . ?
C602 C601 H60A 110.3 . . ?
C602 C601 H60B 110.3 . . ?
O601 C601 H60A 110.3 . . ?
O601 C601 H60B 110.3 . . ?
O601 C601 C602 107.2(17) . . ?
C601 C602 H60C 110.0 . . ?
C601 C602 H60D 110.0 . . ?
H60C C602 H60D 108.4 . . ?
O602 C602 C601 108.5(17) . . ?
O602 C602 H60C 110.0 . . ?
O602 C602 H60D 110.0 . . ?
H60E C603 H60F 108.6 . . ?
C604 C603 H60E 110.3 . . ?
C604 C603 H60F 110.3 . . ?
O602 C603 H60E 110.3 . . ?
O602 C603 H60F 110.3 . . ?
O602 C603 C604 107.0(18) . . ?
C603 C604 H60G 110.4 . . ?
C603 C604 H60H 110.4 . . ?
H60G C604 H60H 108.6 . . ?
O603 C604 C603 106.8(18) . . ?
O603 C604 H60G 110.4 . . ?
O603 C604 H60H 110.4 . . ?
H60I C605 H60J 107.9 . . ?
H60K C605 H60L 106.0 . . ?
C606 C605 H60I 109.3 . . ?
C606 C605 H60J 109.3 . . ?
O603 C605 H60I 109.3 . . ?
O603 C605 H60J 109.3 . . ?
O603 C605 H60K 105.3 . . ?
O603 C605 H60L 105.3 . . ?
O603 C605 C606 112(2) . . ?
O603 C605 C706 128(5) . . ?
C706 C605 H60K 105.3 . . ?
C706 C605 H60L 105.3 . . ?
C605 C606 H60M 109.6 . . ?
C605 C606 H60N 109.6 . . ?
H60M C606 H60N 108.1 . . ?
O604 C606 C605 110(2) . . ?
O604 C606 H60M 109.6 . . ?
O604 C606 H60N 109.6 . . ?
H60O C607 H60P 109.2 . . ?
H60Q C607 H60R 105.5 . . ?
C608 C607 H60O 111.3 . . ?
C608 C607 H60P 111.3 . . ?
C608 C607 H60Q 104.0 . . ?
C608 C607 H60R 104.0 . . ?
O604 C607 H60O 111.3 . . ?
O604 C607 H60P 111.3 . . ?
O604 C607 C608 102(2) . . ?
O704 C607 H60Q 104.0 . . ?
O704 C607 H60R 104.0 . . ?
O704 C607 C608 133(2) . . ?
C607 C608 H60S 110.0 . . ?
C607 C608 H60T 110.0 . . ?
H60S C608 H60T 108.3 . . ?
O605 C608 C607 108.7(18) . . ?
O605 C608 H60S 110.0 . . ?
O605 C608 H60T 110.0 . . ?
H60U C609 H60V 108.6 . . ?
C610 C609 H60U 110.4 . . ?
C610 C609 H60V 110.4 . . ?
O605 C609 H60U 110.4 . . ?
O605 C609 H60V 110.4 . . ?
O605 C609 C610 106.8(16) . . ?
C609 C610 H61A 109.7 . . ?
C609 C610 H61B 109.7 . . ?
H61A C610 H61B 108.2 . . ?
O601 C610 C609 109.8(16) . . ?
O601 C610 H61A 109.7 . . ?
O601 C610 H61B 109.7 . . ?
C601 O601 C610 114.0(14) . . ?
C601 O601 Na1 100.4(14) . . ?
C610 O601 Na1 106.2(11) . . ?
C602 O602 Na1 120.6(11) . . ?
C603 O602 C602 112.9(15) . . ?
C603 O602 Na1 112.2(11) . . ?
C604 O603 Na1 100.0(15) . . ?
C605 O603 C604 115.1(15) . . ?
C605 O603 Na1 101.7(13) . . ?
C606 O604 Na1 107.3(14) . . ?
C607 O604 C606 116(2) . . ?
C607 O604 Na1 100.9(14) . . ?
C608 O605 C609 111.5(16) . . ?
C608 O605 Na1 114.6(12) . . ?
C609 O605 Na1 118.0(12) . . ?
O301 Na1 O302 71.00(15) . . ?
O301 Na1 H40A 84.2(16) . . ?
O302 Na1 H40A 102.6(17) . . ?
O303 Na1 O301 139.38(18) . . ?
O303 Na1 O302 69.70(17) . . ?
O303 Na1 H40A 94.5(16) . . ?
O304 Na1 O301 140.37(17) . . ?
O304 Na1 O302 118.25(18) . . ?
O304 Na1 O303 70.42(18) . . ?
O304 Na1 H40A 125.7(17) . . ?
O305 Na1 O301 73.24(15) . . ?
O305 Na1 O302 127.26(18) . . ?
O305 Na1 O303 141.97(19) . . ?
O305 Na1 O304 71.79(16) . . ?
O305 Na1 H40A 111.0(16) . . ?
O601 Na1 H40A 118.9(16) . . ?
O602 Na1 O601 68.7(4) . . ?
O602 Na1 O603 74.7(4) . . ?
O602 Na1 O604 134.6(5) . . ?
O602 Na1 O605 134.3(4) . . ?
O602 Na1 H40A 90.3(17) . . ?
O602 Na1 O704 147.7(8) . . ?
O603 Na1 O601 118.7(5) . . ?
O603 Na1 O604 67.3(5) . . ?
O603 Na1 O605 129.1(5) . . ?
O603 Na1 H40A 108.4(16) . . ?
O603 Na1 O704 73.2(8) . . ?
O604 Na1 O601 108.9(6) . . ?
O604 Na1 H40A 124.4(17) . . ?
O605 Na1 O601 65.5(4) . . ?
O605 Na1 O604 64.4(5) . . ?
O605 Na1 H40A 111.2(17) . . ?
O401 Na1 O301 96.36(17) . . ?
O401 Na1 O302 119.63(19) . . ?
O401 Na1 O303 94.1(2) . . ?
O401 Na1 O304 108.35(17) . . ?
O401 Na1 O305 101.60(19) . . ?
O401 Na1 O601 119.0(4) . . ?
O401 Na1 O602 107.6(3) . . ?
O401 Na1 O603 118.1(4) . . ?
O401 Na1 O604 111.7(5) . . ?
O401 Na1 O605 94.1(4) . . ?
O401 Na1 H40A 18.3(16) . . ?
O401 Na1 O704 84.6(9) . . ?
O704 Na1 O601 131.9(8) . . ?
O704 Na1 O605 72.0(8) . . ?
O704 Na1 H40A 96.3(19) . . ?
Na1 O401 H40A 110(5) . . ?
Na1 O401 H40B 124(5) . . ?
H40A O401 H40B 116(7) . . ?
C106 C101 C102 117.6(4) . . ?
C107 C101 C102 120.8(4) . . ?
C107 C101 C106 121.5(4) . . ?
C101 C102 H102 119.4 . . ?
C103 C102 C101 121.3(4) . . ?
C103 C102 H102 119.4 . . ?
C102 C103 H103 119.5 . . ?
C102 C103 C104 121.0(4) . . ?
C104 C103 H103 119.5 . . ?
C105 C104 C103 117.9(4) . . ?
C108 C104 C103 121.4(4) . . ?
C108 C104 C105 120.7(4) . . ?
C104 C105 H105 119.5 . . ?
C106 C105 C104 121.0(4) . . ?
C106 C105 H105 119.5 . . ?
C101 C106 H106 119.4 . . ?
C105 C106 C101 121.2(4) . . ?
C105 C106 H106 119.4 . . ?
C101 C107 C109 122.5(4) . . ?
C101 C107 C110 121.6(4) . . ?
C110 C107 C109 115.8(4) . . ?
C104 C108 C111 122.2(4) . . ?
C104 C108 C112 122.4(4) . . ?
C112 C108 C111 115.4(4) . . ?
N101 C109 C107 178.8(5) . . ?
N102 C110 C107 179.0(6) . . ?
N103 C111 C108 178.6(5) . . ?
N104 C112 C108 179.0(5) . . ?
C206 C201 C202 117.5(4) . . ?
C207 C201 C202 120.7(4) . . ?
C207 C201 C206 121.8(4) . . ?
C201 C202 H202 119.4 . . ?
C203 C202 C201 121.3(4) . . ?
C203 C202 H202 119.4 . . ?
C202 C203 H203 119.5 . . ?
C202 C203 C204 121.0(4) . . ?
C204 C203 H203 119.5 . . ?
C205 C204 C203 117.8(4) . . ?
C208 C204 C203 121.2(4) . . ?
C208 C204 C205 121.0(4) . . ?
C204 C205 H205 119.5 . . ?
C206 C205 C204 121.1(4) . . ?
C206 C205 H205 119.5 . . ?
C201 C206 H206 119.3 . . ?
C205 C206 C201 121.3(4) . . ?
C205 C206 H206 119.3 . . ?
C201 C207 C209 122.2(4) . . ?
C201 C207 C210 121.6(4) . . ?
C209 C207 C210 116.1(4) . . ?
C204 C208 C211 122.6(4) . . ?
C204 C208 C212 121.8(4) . . ?
C212 C208 C211 115.6(4) . . ?
N201 C209 C207 178.6(5) . . ?
N202 C210 C207 179.4(6) . . ?
N203 C211 C208 178.0(5) . . ?
N204 C212 C208 179.3(5) . . ?
C607 O704 Na1 107.4(18) . . ?
C607 O704 C706 115(4) . . ?
C706 O704 Na1 116(3) . . ?
C605 C706 H70A 112.3 . . ?
C605 C706 H70B 112.3 . . ?
O704 C706 C605 97(3) . . ?
O704 C706 H70A 112.3 . . ?
O704 C706 H70B 112.3 . . ?
H70A C706 H70B 109.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C301 C302 O302 C303 -165.6(7) . . . . ?
C301 C302 O302 Na1 -44.9(7) . . . . ?
C302 C301 O301 C310 -174.1(6) . . . . ?
C302 C301 O301 Na1 -50.6(7) . . . . ?
C303 C304 O303 C305 162.9(7) . . . . ?
C303 C304 O303 Na1 30.7(8) . . . . ?
C304 C303 O302 C302 -178.0(7) . . . . ?
C304 C303 O302 Na1 59.2(9) . . . . ?
C305 C306 O304 C307 -178.7(7) . . . . ?
C305 C306 O304 Na1 -64.5(6) . . . . ?
C306 C305 O303 C304 -165.3(7) . . . . ?
C306 C305 O303 Na1 -31.9(9) . . . . ?
C307 C308 O305 C309 165.9(8) . . . . ?
C307 C308 O305 Na1 35.6(10) . . . . ?
C308 C307 O304 C306 171.3(7) . . . . ?
C308 C307 O304 Na1 57.8(8) . . . . ?
C309 C310 O301 C301 89.9(8) . . . . ?
C309 C310 O301 Na1 -33.8(7) . . . . ?
C310 C309 O305 C308 177.7(7) . . . . ?
C310 C309 O305 Na1 -50.2(7) . . . . ?
O301 C301 C302 O302 64.8(8) . . . . ?
O302 C303 C304 O303 -60.2(10) . . . . ?
O303 C305 C306 O304 65.8(9) . . . . ?
O304 C307 C308 O305 -63.7(11) . . . . ?
O305 C309 C310 O301 57.0(9) . . . . ?
C601 C602 O602 C603 166(2) . . . . ?
C601 C602 O602 Na1 29(3) . . . . ?
C602 C601 O601 C610 171.5(18) . . . . ?
C602 C601 O601 Na1 58.4(19) . . . . ?
C603 C604 O603 C605 -173(2) . . . . ?
C603 C604 O603 Na1 -65(2) . . . . ?
C604 C603 O602 C602 -166(2) . . . . ?
C604 C603 O602 Na1 -26(3) . . . . ?
C605 C606 O604 C607 -116(3) . . . . ?
C605 C606 O604 Na1 -4(3) . . . . ?
C606 C605 O603 C604 179(3) . . . . ?
C606 C605 O603 Na1 72(2) . . . . ?
C607 C608 O605 C609 160(3) . . . . ?
C607 C608 O605 Na1 23(3) . . . . ?
C607 O704 C706 C605 151(4) . . . . ?
C608 C607 O604 C606 -171(2) . . . . ?
C608 C607 O604 Na1 73.6(19) . . . . ?
C608 C607 O704 Na1 2(4) . . . . ?
C608 C607 O704 C706 -129(6) . . . . ?
C609 C610 O601 C601 -168(2) . . . . ?
C609 C610 O601 Na1 -58.9(17) . . . . ?
C610 C609 O605 C608 -170(2) . . . . ?
C610 C609 O605 Na1 -35(3) . . . . ?
O601 C601 C602 O602 -63(3) . . . . ?
O602 C603 C604 O603 64(3) . . . . ?
O603 C605 C606 O604 -44(4) . . . . ?
O603 C605 C706 O704 -59(9) . . . . ?
O604 C607 C608 O605 -67(3) . . . . ?
O605 C609 C610 O601 64(3) . . . . ?
Na1 O704 C706 C605 25(8) . . . . ?
C101 C102 C103 C104 0.3(6) . . . . ?
C102 C101 C106 C105 0.8(6) . . . . ?
C102 C101 C107 C109 -1.3(6) . . . . ?
C102 C101 C107 C110 -176.2(4) . . . . ?
C102 C103 C104 C105 0.6(5) . . . . ?
C102 C103 C104 C108 -179.8(4) . . . . ?
C103 C104 C105 C106 -0.8(6) . . . . ?
C103 C104 C108 C111 -179.7(4) . . . . ?
C103 C104 C108 C112 0.7(6) . . . . ?
C104 C105 C106 C101 0.1(6) . . . . ?
C105 C104 C108 C111 -0.1(6) . . . . ?
C105 C104 C108 C112 -179.7(4) . . . . ?
C106 C101 C102 C103 -0.9(6) . . . . ?
C106 C101 C107 C109 176.9(4) . . . . ?
C106 C101 C107 C110 2.0(6) . . . . ?
C107 C101 C102 C103 177.3(4) . . . . ?
C107 C101 C106 C105 -177.4(4) . . . . ?
C108 C104 C105 C106 179.6(4) . . . . ?
C201 C202 C203 C204 0.5(6) . . . . ?
C202 C201 C206 C205 1.2(6) . . . . ?
C202 C201 C207 C209 1.1(6) . . . . ?
C202 C201 C207 C210 177.7(4) . . . . ?
C202 C203 C204 C205 -0.3(6) . . . . ?
C202 C203 C204 C208 -179.7(4) . . . . ?
C203 C204 C205 C206 0.6(6) . . . . ?
C203 C204 C208 C211 179.0(4) . . . . ?
C203 C204 C208 C212 -1.9(6) . . . . ?
C204 C205 C206 C201 -1.0(6) . . . . ?
C205 C204 C208 C211 -0.4(6) . . . . ?
C205 C204 C208 C212 178.8(4) . . . . ?
C206 C201 C202 C203 -0.9(6) . . . . ?
C206 C201 C207 C209 -176.2(4) . . . . ?
C206 C201 C207 C210 0.3(6) . . . . ?
C207 C201 C202 C203 -178.3(4) . . . . ?
C207 C201 C206 C205 178.5(4) . . . . ?
C208 C204 C205 C206 180.0(4) . . . . ?
O704 C607 C608 O605 -18(5) . . . . ?
C706 C605 O603 C604 164(5) . . . . ?
C706 C605 O603 Na1 57(5) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.594
_oxdiff_exptl_absorpt_empirical_full_min 0.582
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.8002 7428 14542 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.1998 7422 14542 nmt -1.0004 0.0006 0.0000 -0.0005 -1.0002 -0.0001 0.3046
0.6229 1.0001

_twin_special_details            
;
Component 2 rotated by -179.9782° 
 around [0.00 0.00 1.00] (reciprocal) or [0.14 0.29 0.94] (direct)
;
####################################################################### 
# 
# 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_5_6KT2
_database_code_depnum_ccdc_archive 'CCDC 1866256'
loop_
_audit_author_name
_audit_author_address
'Bingjia Yan'
;University of Southampton
China
;
_audit_update_record             
;
2018-09-06 deposited with the CCDC.	2019-04-30 downloaded from the CCDC.
;

#2013by019

_audit_creation_date             2018-09-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C48 H56 K2 N8 O12'
_chemical_formula_sum            'C48 H56 K2 N8 O12'
_chemical_formula_weight         1015.20
_chemical_melting_point          ?
_chemical_oxdiff_formula         'K C12 H4N4 C12H24O6'
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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.6351(2)
_cell_length_b                   8.17770(10)
_cell_length_c                   26.7566(3)
_cell_angle_alpha                90
_cell_angle_beta                 98.0070(10)
_cell_angle_gamma                90
_cell_volume                     5121.12(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    25585
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2290
_cell_measurement_theta_min      2.6160
_shelx_estimated_absorpt_T_max   0.990
_shelx_estimated_absorpt_T_min   0.937
_exptl_absorpt_coefficient_mu    0.253
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            purple
_exptl_crystal_colour_primary    purple
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_unetI/netI     0.0096
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            30790
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.638
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -94.00  71.00   1.00   30.00    --  -19.00  18.00-120.00  165
  2  ω    -87.00  22.00   1.00   30.00    --  -19.00 -72.00   0.00  109
  3  ω    -27.00  44.00   1.00   30.00    --  -19.00  72.00 -90.00   71
  4  ω    -60.00  22.00   1.00   30.00    --  -19.00 -72.00 150.00   82
  5  ω    -52.00 -11.00   1.00   30.00    --  -19.00 -72.00 -30.00   41
  6  ω    -41.00 -21.00   1.00   30.00    --  -19.00  36.00-180.00   20
  7  ω    -93.00  38.00   1.00   30.00    --  -19.00   0.00-180.00  131
;
_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  
'Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0123517000
_diffrn_orient_matrix_UB_12      0.0421094000
_diffrn_orient_matrix_UB_13      0.0189843000
_diffrn_orient_matrix_UB_21      -0.0236653000
_diffrn_orient_matrix_UB_22      -0.0541197000
_diffrn_orient_matrix_UB_23      -0.0034569000
_diffrn_orient_matrix_UB_31      0.0143334000
_diffrn_orient_matrix_UB_32      -0.0531286000
_diffrn_orient_matrix_UB_33      0.0185619000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5500
_reflns_number_total             5880
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5880
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0252
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0326P)²+3.2442P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0679
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
K1 K 0.67865(2) 0.40857(2) 0.33034(2) 0.01790(6) Uani 1 1 d . . . . .
O21 O 0.70215(3) 0.67088(8) 0.26895(2) 0.02048(14) Uani 1 1 d . . . . .
O22 O 0.78913(3) 0.57032(8) 0.34632(2) 0.02066(14) Uani 1 1 d . . . . .
O23 O 0.76744(3) 0.29830(8) 0.40332(3) 0.02338(15) Uani 1 1 d . . . . .
O24 O 0.68802(3) 0.06713(9) 0.36213(3) 0.02364(15) Uani 1 1 d . . . . .
O25 O 0.60469(3) 0.16417(8) 0.28161(2) 0.02174(14) Uani 1 1 d . . . . .
O26 O 0.62760(3) 0.43404(8) 0.22318(2) 0.01951(14) Uani 1 1 d . . . . .
N1 N 0.56965(4) 0.55106(11) 0.32669(3) 0.02543(18) Uani 1 1 d . . . . .
N2 N 0.48133(4) 0.97158(11) 0.37766(3) 0.02913(19) Uani 1 1 d . . . . .
N3 N 0.32981(4) 0.39780(11) 0.57791(3) 0.02499(18) Uani 1 1 d . . . . .
N4 N 0.40878(4) -0.04449(11) 0.52318(3) 0.02647(18) Uani 1 1 d . . . . .
C1 C 0.47855(4) 0.56344(11) 0.42090(3) 0.01660(17) Uani 1 1 d . . . . .
C2 C 0.44460(4) 0.63376(12) 0.45523(3) 0.01771(17) Uani 1 1 d . . . . .
H2 H 0.440448 0.749218 0.456241 0.021 Uiso 1 1 calc R . . . .
C3 C 0.41789(4) 0.53877(12) 0.48670(3) 0.01808(18) Uani 1 1 d . . . . .
H3 H 0.395375 0.589356 0.509100 0.022 Uiso 1 1 calc R . . . .
C4 C 0.42304(4) 0.36585(12) 0.48667(3) 0.01709(17) Uani 1 1 d . . . . .
C5 C 0.45708(4) 0.29465(11) 0.45232(3) 0.01791(17) Uani 1 1 d . . . . .
H5 H 0.461149 0.179178 0.451277 0.021 Uiso 1 1 calc R . . . .
C6 C 0.48388(4) 0.39007(12) 0.42095(3) 0.01769(17) Uani 1 1 d . . . . .
H6 H 0.506584 0.339682 0.398659 0.021 Uiso 1 1 calc R . . . .
C7 C 0.50524(4) 0.66527(11) 0.38823(3) 0.01771(17) Uani 1 1 d . . . . .
C8 C 0.39596(4) 0.26804(11) 0.52023(3) 0.01824(18) Uani 1 1 d . . . . .
C9 C 0.54052(4) 0.60125(11) 0.35423(3) 0.01902(18) Uani 1 1 d . . . . .
C10 C 0.49253(4) 0.83504(12) 0.38303(3) 0.02038(19) Uani 1 1 d . . . . .
C11 C 0.35935(4) 0.33884(11) 0.55211(3) 0.01919(18) Uani 1 1 d . . . . .
C12 C 0.40281(4) 0.09562(12) 0.52212(3) 0.01988(18) Uani 1 1 d . . . . .
C21 C 0.75620(4) 0.74982(12) 0.27857(4) 0.02252(19) Uani 1 1 d . . . . .
H21A H 0.752398 0.866096 0.268351 0.027 Uiso 1 1 calc R . . . .
H21B H 0.783550 0.696750 0.258837 0.027 Uiso 1 1 calc R . . . .
C22 C 0.77768(4) 0.73769(12) 0.33394(4) 0.02200(19) Uani 1 1 d . . . . .
H22A H 0.812973 0.803207 0.342129 0.026 Uiso 1 1 calc R . . . .
H22B H 0.748611 0.780852 0.353787 0.026 Uiso 1 1 calc R . . . .
C23 C 0.81378(4) 0.55334(12) 0.39790(4) 0.0230(2) Uani 1 1 d . . . . .
H23A H 0.788279 0.602671 0.420142 0.028 Uiso 1 1 calc R . . . .
H23B H 0.851017 0.610607 0.403752 0.028 Uiso 1 1 calc R . . . .
C24 C 0.82197(4) 0.37507(13) 0.40974(4) 0.02309(19) Uani 1 1 d . . . . .
H24A H 0.846559 0.324864 0.386863 0.028 Uiso 1 1 calc R . . . .
H24B H 0.840764 0.360926 0.444922 0.028 Uiso 1 1 calc R . . . .
C25 C 0.77028(4) 0.13373(13) 0.42025(4) 0.0257(2) Uani 1 1 d . . . . .
H25A H 0.787649 0.128688 0.456084 0.031 Uiso 1 1 calc R . . . .
H25B H 0.794085 0.068305 0.400033 0.031 Uiso 1 1 calc R . . . .
C26 C 0.71058(5) 0.06693(13) 0.41436(4) 0.0267(2) Uani 1 1 d . . . . .
H26A H 0.710913 -0.045861 0.427831 0.032 Uiso 1 1 calc R . . . .
H26B H 0.686437 0.135337 0.433429 0.032 Uiso 1 1 calc R . . . .
C27 C 0.63167(4) -0.00067(13) 0.35393(4) 0.0273(2) Uani 1 1 d . . . . .
H27A H 0.605681 0.065248 0.371855 0.033 Uiso 1 1 calc R . . . .
H27B H 0.632227 -0.113871 0.367104 0.033 Uiso 1 1 calc R . . . .
C28 C 0.61109(4) -0.00025(12) 0.29838(4) 0.0258(2) Uani 1 1 d . . . . .
H28A H 0.638972 -0.057463 0.280167 0.031 Uiso 1 1 calc R . . . .
H28B H 0.574029 -0.058082 0.291465 0.031 Uiso 1 1 calc R . . . .
C29 C 0.58364(4) 0.17384(13) 0.22918(4) 0.02292(19) Uani 1 1 d . . . . .
H29A H 0.547296 0.112593 0.221863 0.028 Uiso 1 1 calc R . . . .
H29B H 0.611588 0.124918 0.209213 0.028 Uiso 1 1 calc R . . . .
C30 C 0.57412(4) 0.35022(13) 0.21511(4) 0.02260(19) Uani 1 1 d . . . . .
H30A H 0.557236 0.359114 0.179221 0.027 Uiso 1 1 calc R . . . .
H30B H 0.547282 0.400111 0.236005 0.027 Uiso 1 1 calc R . . . .
C31 C 0.62085(4) 0.60200(12) 0.21000(4) 0.02202(19) Uani 1 1 d . . . . .
H31A H 0.595752 0.656035 0.231696 0.026 Uiso 1 1 calc R . . . .
H31B H 0.602989 0.612614 0.174416 0.026 Uiso 1 1 calc R . . . .
C32 C 0.67874(4) 0.68181(12) 0.21707(3) 0.02201(19) Uani 1 1 d . . . . .
H32A H 0.704147 0.626004 0.196020 0.026 Uiso 1 1 calc R . . . .
H32B H 0.675233 0.797909 0.206609 0.026 Uiso 1 1 calc R . . . .


_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
K1 O21 2.8039(7) . ?
K1 O22 2.9051(7) . ?
K1 O23 2.8085(7) . ?
K1 O24 2.9183(7) . ?
K1 O25 2.8488(7) . ?
K1 O26 2.9591(7) . ?
K1 N1 2.8169(9) . ?
K1 N3 2.9514(9) 5_666 ?
O21 C21 1.4224(11) . ?
O21 C32 1.4239(11) . ?
O22 C22 1.4253(11) . ?
O22 C23 1.4280(11) . ?
O23 C24 1.4225(11) . ?
O23 C25 1.4186(12) . ?
O24 C26 1.4247(12) . ?
O24 C27 1.4311(12) . ?
O25 C28 1.4190(12) . ?
O25 C29 1.4238(11) . ?
O26 C30 1.4277(11) . ?
O26 C31 1.4216(11) . ?
N1 C9 1.1518(13) . ?
N2 C10 1.1519(14) . ?
N3 C11 1.1536(13) . ?
N4 C12 1.1543(13) . ?
C1 C2 1.4224(12) . ?
C1 C6 1.4234(13) . ?
C1 C7 1.4175(13) . ?
C2 H2 0.9500 . ?
C2 C3 1.3635(13) . ?
C3 H3 0.9500 . ?
C3 C4 1.4193(13) . ?
C4 C5 1.4274(12) . ?
C4 C8 1.4198(13) . ?
C5 H5 0.9500 . ?
C5 C6 1.3648(13) . ?
C6 H6 0.9500 . ?
C7 C9 1.4171(13) . ?
C7 C10 1.4232(13) . ?
C8 C11 1.4202(12) . ?
C8 C12 1.4194(13) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.5010(13) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.4987(14) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.5007(14) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.4980(14) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.4997(14) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.5040(13) . ?
C32 H32A 0.9900 . ?
C32 H32B 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
O21 K1 O22 59.376(19) . . ?
O21 K1 O23 117.59(2) . . ?
O21 K1 O24 152.81(2) . . ?
O21 K1 O25 115.31(2) . . ?
O21 K1 O26 57.714(19) . . ?
O21 K1 N1 85.30(2) . . ?
O21 K1 N3 96.82(2) . 5_666 ?
O22 K1 O24 111.26(2) . . ?
O22 K1 O26 110.328(19) . . ?
O22 K1 N3 78.29(2) . 5_666 ?
O23 K1 O22 58.308(19) . . ?
O23 K1 O24 58.07(2) . . ?
O23 K1 O25 116.38(2) . . ?
O23 K1 O26 149.38(2) . . ?
O23 K1 N1 138.42(2) . . ?
O23 K1 N3 74.02(2) . 5_666 ?
O24 K1 O26 110.72(2) . . ?
O24 K1 N3 106.39(2) . 5_666 ?
O25 K1 O22 150.28(2) . . ?
O25 K1 O24 58.596(19) . . ?
O25 K1 O26 57.621(19) . . ?
O25 K1 N3 130.45(2) . 5_666 ?
N1 K1 O22 128.01(2) . . ?
N1 K1 O24 115.96(2) . . ?
N1 K1 O25 76.96(2) . . ?
N1 K1 O26 71.93(2) . . ?
N1 K1 N3 68.85(2) . 5_666 ?
N3 K1 O26 134.62(2) 5_666 . ?
C21 O21 K1 119.17(5) . . ?
C21 O21 C32 111.41(7) . . ?
C32 O21 K1 122.51(5) . . ?
C22 O22 K1 105.38(5) . . ?
C22 O22 C23 110.89(7) . . ?
C23 O22 K1 109.59(5) . . ?
C24 O23 K1 121.27(5) . . ?
C25 O23 K1 121.61(5) . . ?
C25 O23 C24 112.23(7) . . ?
C26 O24 K1 106.85(6) . . ?
C26 O24 C27 111.29(8) . . ?
C27 O24 K1 107.15(6) . . ?
C28 O25 K1 119.24(5) . . ?
C28 O25 C29 111.81(7) . . ?
C29 O25 K1 121.33(5) . . ?
C30 O26 K1 110.22(5) . . ?
C31 O26 K1 108.97(5) . . ?
C31 O26 C30 111.09(7) . . ?
C9 N1 K1 138.63(7) . . ?
C11 N3 K1 147.02(7) . 5_666 ?
C2 C1 C6 117.39(8) . . ?
C7 C1 C2 120.01(8) . . ?
C7 C1 C6 122.59(8) . . ?
C1 C2 H2 119.3 . . ?
C3 C2 C1 121.31(9) . . ?
C3 C2 H2 119.3 . . ?
C2 C3 H3 119.3 . . ?
C2 C3 C4 121.35(8) . . ?
C4 C3 H3 119.3 . . ?
C3 C4 C5 117.57(8) . . ?
C3 C4 C8 120.98(8) . . ?
C8 C4 C5 121.45(9) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 C4 120.96(9) . . ?
C6 C5 H5 119.5 . . ?
C1 C6 H6 119.3 . . ?
C5 C6 C1 121.42(8) . . ?
C5 C6 H6 119.3 . . ?
C1 C7 C10 121.82(8) . . ?
C9 C7 C1 122.08(8) . . ?
C9 C7 C10 115.64(8) . . ?
C4 C8 C11 121.08(8) . . ?
C12 C8 C4 121.52(8) . . ?
C12 C8 C11 117.37(8) . . ?
N1 C9 C7 179.08(11) . . ?
N2 C10 C7 178.21(11) . . ?
N3 C11 C8 179.35(11) . . ?
N4 C12 C8 179.18(11) . . ?
O21 C21 H21A 110.0 . . ?
O21 C21 H21B 110.0 . . ?
O21 C21 C22 108.68(7) . . ?
H21A C21 H21B 108.3 . . ?
C22 C21 H21A 110.0 . . ?
C22 C21 H21B 110.0 . . ?
O22 C22 C21 108.66(8) . . ?
O22 C22 H22A 110.0 . . ?
O22 C22 H22B 110.0 . . ?
C21 C22 H22A 110.0 . . ?
C21 C22 H22B 110.0 . . ?
H22A C22 H22B 108.3 . . ?
O22 C23 H23A 109.9 . . ?
O22 C23 H23B 109.9 . . ?
O22 C23 C24 108.80(8) . . ?
H23A C23 H23B 108.3 . . ?
C24 C23 H23A 109.9 . . ?
C24 C23 H23B 109.9 . . ?
O23 C24 C23 108.39(8) . . ?
O23 C24 H24A 110.0 . . ?
O23 C24 H24B 110.0 . . ?
C23 C24 H24A 110.0 . . ?
C23 C24 H24B 110.0 . . ?
H24A C24 H24B 108.4 . . ?
O23 C25 H25A 110.1 . . ?
O23 C25 H25B 110.1 . . ?
O23 C25 C26 108.04(8) . . ?
H25A C25 H25B 108.4 . . ?
C26 C25 H25A 110.1 . . ?
C26 C25 H25B 110.1 . . ?
O24 C26 C25 108.69(8) . . ?
O24 C26 H26A 110.0 . . ?
O24 C26 H26B 110.0 . . ?
C25 C26 H26A 110.0 . . ?
C25 C26 H26B 110.0 . . ?
H26A C26 H26B 108.3 . . ?
O24 C27 H27A 110.0 . . ?
O24 C27 H27B 110.0 . . ?
O24 C27 C28 108.53(8) . . ?
H27A C27 H27B 108.4 . . ?
C28 C27 H27A 110.0 . . ?
C28 C27 H27B 110.0 . . ?
O25 C28 C27 108.76(8) . . ?
O25 C28 H28A 109.9 . . ?
O25 C28 H28B 109.9 . . ?
C27 C28 H28A 109.9 . . ?
C27 C28 H28B 109.9 . . ?
H28A C28 H28B 108.3 . . ?
O25 C29 H29A 110.0 . . ?
O25 C29 H29B 110.0 . . ?
O25 C29 C30 108.68(8) . . ?
H29A C29 H29B 108.3 . . ?
C30 C29 H29A 110.0 . . ?
C30 C29 H29B 110.0 . . ?
O26 C30 C29 108.97(8) . . ?
O26 C30 H30A 109.9 . . ?
O26 C30 H30B 109.9 . . ?
C29 C30 H30A 109.9 . . ?
C29 C30 H30B 109.9 . . ?
H30A C30 H30B 108.3 . . ?
O26 C31 H31A 110.0 . . ?
O26 C31 H31B 110.0 . . ?
O26 C31 C32 108.62(8) . . ?
H31A C31 H31B 108.3 . . ?
C32 C31 H31A 110.0 . . ?
C32 C31 H31B 110.0 . . ?
O21 C32 C31 108.57(7) . . ?
O21 C32 H32A 110.0 . . ?
O21 C32 H32B 110.0 . . ?
C31 C32 H32A 110.0 . . ?
C31 C32 H32B 110.0 . . ?
H32A C32 H32B 108.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
K1 O21 C21 C22 -29.84(9) . . . . ?
K1 O21 C32 C31 31.66(10) . . . . ?
K1 O22 C22 C21 -65.86(7) . . . . ?
K1 O22 C23 C24 60.97(8) . . . . ?
K1 O23 C24 C23 32.36(10) . . . . ?
K1 O23 C25 C26 -27.38(10) . . . . ?
K1 O24 C26 C25 -65.33(8) . . . . ?
K1 O24 C27 C28 64.78(9) . . . . ?
K1 O25 C28 C27 31.65(10) . . . . ?
K1 O25 C29 C30 -34.68(9) . . . . ?
K1 O26 C30 C29 -59.54(8) . . . . ?
K1 O26 C31 C32 60.88(8) . . . . ?
O21 C21 C22 O22 66.39(10) . . . . ?
O22 C23 C24 O23 -62.39(10) . . . . ?
O23 C25 C26 O24 63.05(11) . . . . ?
O24 C27 C28 O25 -66.01(11) . . . . ?
O25 C29 C30 O26 62.98(10) . . . . ?
O26 C31 C32 O21 -62.18(10) . . . . ?
C1 C2 C3 C4 0.26(13) . . . . ?
C2 C1 C6 C5 0.60(13) . . . . ?
C2 C1 C7 C9 178.51(8) . . . . ?
C2 C1 C7 C10 -9.58(13) . . . . ?
C2 C3 C4 C5 -0.22(13) . . . . ?
C2 C3 C4 C8 178.80(8) . . . . ?
C3 C4 C5 C6 0.38(13) . . . . ?
C3 C4 C8 C11 4.91(13) . . . . ?
C3 C4 C8 C12 -177.21(8) . . . . ?
C4 C5 C6 C1 -0.58(13) . . . . ?
C5 C4 C8 C11 -176.11(8) . . . . ?
C5 C4 C8 C12 1.77(13) . . . . ?
C6 C1 C2 C3 -0.43(13) . . . . ?
C6 C1 C7 C9 -1.82(13) . . . . ?
C6 C1 C7 C10 170.09(8) . . . . ?
C7 C1 C2 C3 179.25(8) . . . . ?
C7 C1 C6 C5 -179.08(8) . . . . ?
C8 C4 C5 C6 -178.64(8) . . . . ?
C21 O21 C32 C31 -177.80(8) . . . . ?
C22 O22 C23 C24 176.90(8) . . . . ?
C23 O22 C22 C21 175.63(7) . . . . ?
C24 O23 C25 C26 177.12(8) . . . . ?
C25 O23 C24 C23 -172.05(8) . . . . ?
C26 O24 C27 C28 -178.75(8) . . . . ?
C27 O24 C26 C25 178.02(8) . . . . ?
C28 O25 C29 C30 176.05(8) . . . . ?
C29 O25 C28 C27 -178.37(8) . . . . ?
C30 O26 C31 C32 -177.50(7) . . . . ?
C31 O26 C30 C29 179.58(7) . . . . ?
C32 O21 C21 C22 178.52(8) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.869
_oxdiff_exptl_absorpt_empirical_full_min 0.686
####################################################################### 
# 
# 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_3_5LiT2
_database_code_depnum_ccdc_archive 'CCDC 1866254'
loop_
_audit_author_name
_audit_author_address
'Bingjia Yan'
;University of Southampton
China
;
_audit_update_record             
;
2018-09-06 deposited with the CCDC.	2019-04-30 downloaded from the CCDC.
;

#2014by037

_audit_creation_date             2018-09-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H22 Li O6, 2(C12 H4 N4)'
_chemical_formula_sum            'C34 H30 Li N8 O6'
_chemical_formula_weight         653.60
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C10 H22 Li O6 (C12H4N4)2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.3032(5)
_cell_length_b                   12.4300(7)
_cell_length_c                   16.5807(12)
_cell_angle_alpha                97.615(5)
_cell_angle_beta                 100.354(5)
_cell_angle_gamma                100.015(5)
_cell_volume                     1633.89(18)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5650
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.7790
_cell_measurement_theta_min      2.5010
_shelx_estimated_absorpt_T_max   0.998
_shelx_estimated_absorpt_T_min   0.993
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             682
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0926
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20928
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         1.688
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -27.00  73.00   1.00   30.00    --  -17.00  72.00  30.00  100
  2  ω    -69.00  22.00   1.00   30.00    --  -17.00 -72.00 -90.00   91
  3  ω    -66.00  22.00   1.00   30.00    --  -17.00 -72.00  90.00   88
  4  ω    -84.00 -21.00   1.00   30.00    --  -17.00   0.00 -90.00   63
  5  ω     -4.00  16.00   1.00   30.00    --  -17.00 -36.00  90.00   20
  6  ω    -27.00  73.00   1.00   30.00    --  -17.00  72.00 -60.00  100
  7  ω    -69.00  22.00   1.00   30.00    --  -17.00 -72.00-180.00   91
  8  ω    -69.00 -48.00   1.00   30.00    --  -17.00 -72.00   0.00   21
;
_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  
'Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0210765000
_diffrn_orient_matrix_UB_12      0.0007140000
_diffrn_orient_matrix_UB_13      -0.0432954000
_diffrn_orient_matrix_UB_21      0.0489160000
_diffrn_orient_matrix_UB_22      0.0543623000
_diffrn_orient_matrix_UB_23      0.0062753000
_diffrn_orient_matrix_UB_31      0.0709051000
_diffrn_orient_matrix_UB_32      -0.0223793000
_diffrn_orient_matrix_UB_33      -0.0057342000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4263
_reflns_number_total             7458
_reflns_odcompleteness_completeness 99.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         7458
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1523
_refine_ls_R_factor_gt           0.0767
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0683P)²+1.7325P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1662
_refine_ls_wR_factor_ref         0.1938
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C301(H30A,H30B), C302(H30C,H30D), C303(H30E,H30F), C304(H30G,H30H), C305(H30I,
 H30J), C306(H30K,H30L), C307(H30M,H30N), C308(H30O,H30P), C309(H30Q,H30R),
 C310(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C102(H102), C103(H103), C105(H105), C106(H106), C202(H202), C203(H203),
 C205(H205), C206(H206)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
O301 O 0.2286(3) 0.24352(18) 0.37220(14) 0.0284(6) Uani 1 1 d . . . . .
O302 O 0.1707(3) 0.42521(18) 0.45430(14) 0.0287(6) Uani 1 1 d . . . . .
O303 O 0.3127(3) 0.39100(18) 0.60250(14) 0.0271(6) Uani 1 1 d . . . . .
O304 O 0.2102(3) 0.18010(18) 0.62701(13) 0.0253(5) Uani 1 1 d . . . . .
O305 O 0.2314(3) 0.09549(19) 0.47168(14) 0.0271(6) Uani 1 1 d . . . . .
O401 O -0.0552(3) 0.2212(2) 0.49344(16) 0.0252(6) Uani 1 1 d . . . . .
H40A H -0.089(5) 0.244(3) 0.540(3) 0.044(12) Uiso 1 1 d . . . . .
H40B H -0.138(6) 0.217(4) 0.450(3) 0.080(17) Uiso 1 1 d . . . . .
C301 C 0.1362(4) 0.3105(3) 0.3260(2) 0.0255(8) Uani 1 1 d . . . . .
H30A H 0.014990 0.287602 0.323820 0.031 Uiso 1 1 calc R . . . .
H30B H 0.155244 0.304417 0.268456 0.031 Uiso 1 1 calc R . . . .
C302 C 0.2018(4) 0.4271(3) 0.3724(2) 0.0279(8) Uani 1 1 d . . . . .
H30C H 0.322973 0.449834 0.374496 0.034 Uiso 1 1 calc R . . . .
H30D H 0.142836 0.479610 0.345119 0.034 Uiso 1 1 calc R . . . .
C303 C 0.2584(5) 0.5190(3) 0.5131(2) 0.0352(9) Uani 1 1 d . . . . .
H30E H 0.206197 0.583619 0.504828 0.042 Uiso 1 1 calc R . . . .
H30F H 0.376094 0.537668 0.507130 0.042 Uiso 1 1 calc R . . . .
C304 C 0.2506(5) 0.4903(3) 0.5975(2) 0.0315(9) Uani 1 1 d . . . . .
H30G H 0.319493 0.551042 0.641295 0.038 Uiso 1 1 calc R . . . .
H30H H 0.133799 0.479029 0.605401 0.038 Uiso 1 1 calc R . . . .
C305 C 0.3299(4) 0.3647(3) 0.6845(2) 0.0279(8) Uani 1 1 d . . . . .
H30I H 0.227720 0.371415 0.706128 0.033 Uiso 1 1 calc R . . . .
H30J H 0.426179 0.416394 0.722396 0.033 Uiso 1 1 calc R . . . .
C306 C 0.3570(4) 0.2473(3) 0.6800(2) 0.0273(8) Uani 1 1 d . . . . .
H30K H 0.456753 0.239274 0.656604 0.033 Uiso 1 1 calc R . . . .
H30L H 0.372723 0.226166 0.735930 0.033 Uiso 1 1 calc R . . . .
C307 C 0.2199(4) 0.0664(3) 0.6074(2) 0.0266(8) Uani 1 1 d . . . . .
H30M H 0.105557 0.020334 0.590769 0.032 Uiso 1 1 calc R . . . .
H30N H 0.278505 0.042613 0.657301 0.032 Uiso 1 1 calc R . . . .
C308 C 0.3114(4) 0.0490(3) 0.5380(2) 0.0266(8) Uani 1 1 d . . . . .
H30O H 0.430458 0.086318 0.556320 0.032 Uiso 1 1 calc R . . . .
H30P H 0.305300 -0.031096 0.520042 0.032 Uiso 1 1 calc R . . . .
C309 C 0.2823(5) 0.0703(3) 0.3955(2) 0.0301(8) Uani 1 1 d . . . . .
H30Q H 0.254132 -0.010620 0.375252 0.036 Uiso 1 1 calc R . . . .
H30R H 0.404474 0.096233 0.402591 0.036 Uiso 1 1 calc R . . . .
C310 C 0.1890(5) 0.1299(3) 0.3352(2) 0.0315(9) Uani 1 1 d . . . . .
H31A H 0.224540 0.120073 0.281238 0.038 Uiso 1 1 calc R . . . .
H31B H 0.067101 0.100754 0.325504 0.038 Uiso 1 1 calc R . . . .
Li1 Li 0.1840(7) 0.2594(5) 0.5008(4) 0.0316(14) Uani 1 1 d . . . . .
N101 N -0.1834(4) 0.2786(2) 0.64433(18) 0.0317(7) Uani 1 1 d . . . . .
N102 N -0.3821(3) 0.6320(2) 1.07397(16) 0.0236(6) Uani 1 1 d . . . . .
N103 N -0.1197(3) 0.4303(2) 1.22325(17) 0.0242(6) Uani 1 1 d . . . . .
N104 N 0.0988(4) 0.0912(2) 0.80060(17) 0.0286(7) Uani 1 1 d . . . . .
C101 C -0.0924(4) 0.3107(2) 0.86320(18) 0.0166(7) Uani 1 1 d . . . . .
C102 C -0.1902(3) 0.3948(2) 0.85753(18) 0.0161(7) Uani 1 1 d . . . . .
H102 H -0.230369 0.412709 0.804636 0.019 Uiso 1 1 calc R . . . .
C103 C -0.2264(3) 0.4492(2) 0.92633(18) 0.0168(7) Uani 1 1 d . . . . .
H103 H -0.290267 0.505297 0.920901 0.020 Uiso 1 1 calc R . . . .
C104 C -0.1699(4) 0.4236(2) 1.00715(19) 0.0166(7) Uani 1 1 d . . . . .
C105 C -0.0708(3) 0.3401(2) 1.01271(19) 0.0162(6) Uani 1 1 d . . . . .
H105 H -0.030407 0.322287 1.065612 0.019 Uiso 1 1 calc R . . . .
C106 C -0.0337(3) 0.2864(2) 0.94446(18) 0.0161(7) Uani 1 1 d . . . . .
H106 H 0.032313 0.231605 0.950168 0.019 Uiso 1 1 calc R . . . .
C107 C -0.0612(4) 0.2506(2) 0.79270(19) 0.0191(7) Uani 1 1 d . . . . .
C108 C -0.2093(3) 0.4784(2) 1.07758(18) 0.0159(7) Uani 1 1 d . . . . .
C109 C -0.1288(4) 0.2671(3) 0.7109(2) 0.0217(7) Uani 1 1 d . . . . .
C110 C -0.3065(4) 0.5628(2) 1.07403(19) 0.0176(7) Uani 1 1 d . . . . .
C111 C -0.1581(4) 0.4519(2) 1.15786(19) 0.0184(7) Uani 1 1 d . . . . .
C112 C 0.0283(4) 0.1632(3) 0.79658(19) 0.0224(7) Uani 1 1 d . . . . .
N201 N -0.3195(3) 0.2034(2) 0.34985(17) 0.0259(7) Uani 1 1 d . . . . .
N202 N -0.6082(3) 0.3961(2) 0.19804(16) 0.0243(6) Uani 1 1 d . . . . .
N203 N -0.4028(3) 0.0625(2) -0.23139(17) 0.0254(6) Uani 1 1 d . . . . .
N204 N -0.1223(3) -0.1318(2) -0.07984(17) 0.0248(6) Uani 1 1 d . . . . .
C201 C -0.4078(4) 0.1838(2) 0.13261(18) 0.0165(7) Uani 1 1 d . . . . .
C202 C -0.4684(3) 0.2101(2) 0.05229(18) 0.0169(7) Uani 1 1 d . . . . .
H202 H -0.535169 0.264713 0.047996 0.020 Uiso 1 1 calc R . . . .
C203 C -0.4320(3) 0.1584(2) -0.01745(19) 0.0164(7) Uani 1 1 d . . . . .
H203 H -0.473101 0.177477 -0.069817 0.020 Uiso 1 1 calc R . . . .
C204 C -0.3320(3) 0.0753(2) -0.01309(18) 0.0160(6) Uani 1 1 d . . . . .
C205 C -0.2705(3) 0.0498(2) 0.06697(19) 0.0167(7) Uani 1 1 d . . . . .
H205 H -0.203471 -0.004620 0.071316 0.020 Uiso 1 1 calc R . . . .
C206 C -0.3062(3) 0.1018(2) 0.13646(18) 0.0162(7) Uani 1 1 d . . . . .
H206 H -0.263011 0.083636 0.188866 0.019 Uiso 1 1 calc R . . . .
C207 C -0.4424(4) 0.2395(2) 0.20406(18) 0.0177(7) Uani 1 1 d . . . . .
C208 C -0.2973(4) 0.0210(2) -0.08513(19) 0.0171(7) Uani 1 1 d . . . . .
C209 C -0.3756(4) 0.2185(2) 0.2848(2) 0.0196(7) Uani 1 1 d . . . . .
C210 C -0.5350(4) 0.3252(3) 0.20092(18) 0.0195(7) Uani 1 1 d . . . . .
C211 C -0.3565(4) 0.0443(2) -0.1657(2) 0.0190(7) Uani 1 1 d . . . . .
C212 C -0.1988(4) -0.0629(3) -0.08177(19) 0.0192(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
O301 C301 1.431(4) . ?
O301 C310 1.420(4) . ?
O301 Li1 2.217(7) . ?
O302 C302 1.429(4) . ?
O302 C303 1.410(4) . ?
O302 Li1 2.308(7) . ?
O303 C304 1.425(4) . ?
O303 C305 1.429(4) . ?
O303 Li1 2.163(6) . ?
O304 C306 1.421(4) . ?
O304 C307 1.427(4) . ?
O304 Li1 2.420(7) . ?
O305 C308 1.423(4) . ?
O305 C309 1.416(4) . ?
O305 Li1 2.150(6) . ?
O401 H40A 0.90(4) . ?
O401 H40B 0.89(5) . ?
O401 Li1 1.938(6) . ?
C301 H30A 0.9900 . ?
C301 H30B 0.9900 . ?
C301 C302 1.507(5) . ?
C302 H30C 0.9900 . ?
C302 H30D 0.9900 . ?
C303 H30E 0.9900 . ?
C303 H30F 0.9900 . ?
C303 C304 1.499(5) . ?
C304 H30G 0.9900 . ?
C304 H30H 0.9900 . ?
C305 H30I 0.9900 . ?
C305 H30J 0.9900 . ?
C305 C306 1.509(4) . ?
C306 H30K 0.9900 . ?
C306 H30L 0.9900 . ?
C307 H30M 0.9900 . ?
C307 H30N 0.9900 . ?
C307 C308 1.501(5) . ?
C308 H30O 0.9900 . ?
C308 H30P 0.9900 . ?
C309 H30Q 0.9900 . ?
C309 H30R 0.9900 . ?
C309 C310 1.505(5) . ?
C310 H31A 0.9900 . ?
C310 H31B 0.9900 . ?
N101 C109 1.152(4) . ?
N102 C110 1.150(4) . ?
N103 C111 1.155(4) . ?
N104 C112 1.155(4) . ?
C101 C102 1.434(4) . ?
C101 C106 1.437(4) . ?
C101 C107 1.392(4) . ?
C102 H102 0.9500 . ?
C102 C103 1.356(4) . ?
C103 H103 0.9500 . ?
C103 C104 1.434(4) . ?
C104 C105 1.434(4) . ?
C104 C108 1.392(4) . ?
C105 H105 0.9500 . ?
C105 C106 1.348(4) . ?
C106 H106 0.9500 . ?
C107 C109 1.428(4) . ?
C107 C112 1.421(4) . ?
C108 C110 1.432(4) . ?
C108 C111 1.422(4) . ?
N201 C209 1.149(4) . ?
N202 C210 1.156(4) . ?
N203 C211 1.154(4) . ?
N204 C212 1.152(4) . ?
C201 C202 1.437(4) . ?
C201 C206 1.433(4) . ?
C201 C207 1.392(4) . ?
C202 H202 0.9500 . ?
C202 C203 1.356(4) . ?
C203 H203 0.9500 . ?
C203 C204 1.434(4) . ?
C204 C205 1.431(4) . ?
C204 C208 1.394(4) . ?
C205 H205 0.9500 . ?
C205 C206 1.351(4) . ?
C206 H206 0.9500 . ?
C207 C209 1.429(4) . ?
C207 C210 1.419(4) . ?
C208 C211 1.423(4) . ?
C208 C212 1.434(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
C301 O301 Li1 109.9(2) . . ?
C310 O301 C301 113.2(2) . . ?
C310 O301 Li1 109.4(3) . . ?
C302 O302 Li1 114.3(2) . . ?
C303 O302 C302 114.1(3) . . ?
C303 O302 Li1 113.7(2) . . ?
C304 O303 C305 111.5(2) . . ?
C304 O303 Li1 112.1(2) . . ?
C305 O303 Li1 117.1(3) . . ?
C306 O304 C307 113.9(2) . . ?
C306 O304 Li1 104.3(2) . . ?
C307 O304 Li1 109.1(2) . . ?
C308 O305 Li1 117.7(2) . . ?
C309 O305 C308 114.4(2) . . ?
C309 O305 Li1 116.3(3) . . ?
H40A O401 H40B 109(4) . . ?
Li1 O401 H40A 115(2) . . ?
Li1 O401 H40B 129(3) . . ?
O301 C301 H30A 110.8 . . ?
O301 C301 H30B 110.8 . . ?
O301 C301 C302 105.0(3) . . ?
H30A C301 H30B 108.8 . . ?
C302 C301 H30A 110.8 . . ?
C302 C301 H30B 110.8 . . ?
O302 C302 C301 105.7(3) . . ?
O302 C302 H30C 110.6 . . ?
O302 C302 H30D 110.6 . . ?
C301 C302 H30C 110.6 . . ?
C301 C302 H30D 110.6 . . ?
H30C C302 H30D 108.7 . . ?
O302 C303 H30E 110.3 . . ?
O302 C303 H30F 110.3 . . ?
O302 C303 C304 107.0(3) . . ?
H30E C303 H30F 108.6 . . ?
C304 C303 H30E 110.3 . . ?
C304 C303 H30F 110.3 . . ?
O303 C304 C303 107.6(3) . . ?
O303 C304 H30G 110.2 . . ?
O303 C304 H30H 110.2 . . ?
C303 C304 H30G 110.2 . . ?
C303 C304 H30H 110.2 . . ?
H30G C304 H30H 108.5 . . ?
O303 C305 H30I 110.1 . . ?
O303 C305 H30J 110.1 . . ?
O303 C305 C306 107.9(3) . . ?
H30I C305 H30J 108.4 . . ?
C306 C305 H30I 110.1 . . ?
C306 C305 H30J 110.1 . . ?
O304 C306 C305 105.6(2) . . ?
O304 C306 H30K 110.6 . . ?
O304 C306 H30L 110.6 . . ?
C305 C306 H30K 110.6 . . ?
C305 C306 H30L 110.6 . . ?
H30K C306 H30L 108.8 . . ?
O304 C307 H30M 109.4 . . ?
O304 C307 H30N 109.4 . . ?
O304 C307 C308 111.0(3) . . ?
H30M C307 H30N 108.0 . . ?
C308 C307 H30M 109.4 . . ?
C308 C307 H30N 109.4 . . ?
O305 C308 C307 106.4(2) . . ?
O305 C308 H30O 110.5 . . ?
O305 C308 H30P 110.5 . . ?
C307 C308 H30O 110.5 . . ?
C307 C308 H30P 110.5 . . ?
H30O C308 H30P 108.6 . . ?
O305 C309 H30Q 110.5 . . ?
O305 C309 H30R 110.5 . . ?
O305 C309 C310 106.1(3) . . ?
H30Q C309 H30R 108.7 . . ?
C310 C309 H30Q 110.5 . . ?
C310 C309 H30R 110.5 . . ?
O301 C310 C309 106.2(3) . . ?
O301 C310 H31A 110.5 . . ?
O301 C310 H31B 110.5 . . ?
C309 C310 H31A 110.5 . . ?
C309 C310 H31B 110.5 . . ?
H31A C310 H31B 108.7 . . ?
O301 Li1 O302 71.4(2) . . ?
O301 Li1 O304 145.0(3) . . ?
O302 Li1 O304 141.4(3) . . ?
O303 Li1 O301 125.6(3) . . ?
O303 Li1 O302 72.6(2) . . ?
O303 Li1 O304 72.53(19) . . ?
O305 Li1 O301 74.0(2) . . ?
O305 Li1 O302 145.4(3) . . ?
O305 Li1 O303 129.0(3) . . ?
O305 Li1 O304 72.1(2) . . ?
O401 Li1 O301 107.7(3) . . ?
O401 Li1 O302 93.3(2) . . ?
O401 Li1 O303 113.8(3) . . ?
O401 Li1 O304 86.0(3) . . ?
O401 Li1 O305 99.0(3) . . ?
C102 C101 C106 117.6(3) . . ?
C107 C101 C102 121.7(3) . . ?
C107 C101 C106 120.7(3) . . ?
C101 C102 H102 119.4 . . ?
C103 C102 C101 121.2(3) . . ?
C103 C102 H102 119.4 . . ?
C102 C103 H103 119.5 . . ?
C102 C103 C104 121.1(3) . . ?
C104 C103 H103 119.5 . . ?
C103 C104 C105 117.6(3) . . ?
C108 C104 C103 121.0(3) . . ?
C108 C104 C105 121.4(3) . . ?
C104 C105 H105 119.3 . . ?
C106 C105 C104 121.4(3) . . ?
C106 C105 H105 119.3 . . ?
C101 C106 H106 119.4 . . ?
C105 C106 C101 121.2(3) . . ?
C105 C106 H106 119.4 . . ?
C101 C107 C109 121.8(3) . . ?
C101 C107 C112 122.6(3) . . ?
C112 C107 C109 115.4(3) . . ?
C104 C108 C110 122.6(3) . . ?
C104 C108 C111 121.8(3) . . ?
C111 C108 C110 115.6(3) . . ?
N101 C109 C107 178.8(3) . . ?
N102 C110 C108 177.7(3) . . ?
N103 C111 C108 178.7(3) . . ?
N104 C112 C107 178.6(4) . . ?
C206 C201 C202 117.6(3) . . ?
C207 C201 C202 120.7(3) . . ?
C207 C201 C206 121.6(3) . . ?
C201 C202 H202 119.4 . . ?
C203 C202 C201 121.2(3) . . ?
C203 C202 H202 119.4 . . ?
C202 C203 H203 119.6 . . ?
C202 C203 C204 120.8(3) . . ?
C204 C203 H203 119.6 . . ?
C205 C204 C203 118.0(3) . . ?
C208 C204 C203 120.6(3) . . ?
C208 C204 C205 121.4(3) . . ?
C204 C205 H205 119.4 . . ?
C206 C205 C204 121.1(3) . . ?
C206 C205 H205 119.4 . . ?
C201 C206 H206 119.4 . . ?
C205 C206 C201 121.2(3) . . ?
C205 C206 H206 119.4 . . ?
C201 C207 C209 121.4(3) . . ?
C201 C207 C210 121.8(3) . . ?
C210 C207 C209 116.7(3) . . ?
C204 C208 C211 122.9(3) . . ?
C204 C208 C212 121.2(3) . . ?
C211 C208 C212 116.0(3) . . ?
N201 C209 C207 178.7(4) . . ?
N202 C210 C207 178.8(4) . . ?
N203 C211 C208 179.0(3) . . ?
N204 C212 C208 178.7(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O301 C301 C302 O302 -59.3(3) . . . . ?
O302 C303 C304 O303 54.5(4) . . . . ?
O303 C305 C306 O304 -61.9(3) . . . . ?
O304 C307 C308 O305 -53.1(3) . . . . ?
O305 C309 C310 O301 56.3(4) . . . . ?
C301 O301 C310 C309 -174.2(3) . . . . ?
C302 O302 C303 C304 -164.6(3) . . . . ?
C303 O302 C302 C301 165.4(3) . . . . ?
C304 O303 C305 C306 167.1(3) . . . . ?
C305 O303 C304 C303 172.6(3) . . . . ?
C306 O304 C307 C308 -81.6(3) . . . . ?
C307 O304 C306 C305 173.3(3) . . . . ?
C308 O305 C309 C310 -178.0(3) . . . . ?
C309 O305 C308 C307 -169.8(3) . . . . ?
C310 O301 C301 C302 -177.2(3) . . . . ?
Li1 O301 C301 C302 60.2(3) . . . . ?
Li1 O301 C310 C309 -51.4(3) . . . . ?
Li1 O302 C302 C301 32.1(3) . . . . ?
Li1 O302 C303 C304 -31.0(4) . . . . ?
Li1 O303 C304 C303 -53.9(4) . . . . ?
Li1 O303 C305 C306 36.1(4) . . . . ?
Li1 O304 C306 C305 54.6(3) . . . . ?
Li1 O304 C307 C308 34.4(3) . . . . ?
Li1 O305 C308 C307 48.2(4) . . . . ?
Li1 O305 C309 C310 -35.4(4) . . . . ?
C101 C102 C103 C104 -0.8(4) . . . . ?
C102 C101 C106 C105 0.6(4) . . . . ?
C102 C101 C107 C109 -1.8(5) . . . . ?
C102 C101 C107 C112 -176.8(3) . . . . ?
C102 C103 C104 C105 1.3(4) . . . . ?
C102 C103 C104 C108 -179.0(3) . . . . ?
C103 C104 C105 C106 -0.9(4) . . . . ?
C103 C104 C108 C110 -0.3(5) . . . . ?
C103 C104 C108 C111 178.3(3) . . . . ?
C104 C105 C106 C101 -0.1(5) . . . . ?
C105 C104 C108 C110 179.3(3) . . . . ?
C105 C104 C108 C111 -2.1(5) . . . . ?
C106 C101 C102 C103 -0.2(4) . . . . ?
C106 C101 C107 C109 175.1(3) . . . . ?
C106 C101 C107 C112 0.2(5) . . . . ?
C107 C101 C102 C103 176.9(3) . . . . ?
C107 C101 C106 C105 -176.4(3) . . . . ?
C108 C104 C105 C106 179.5(3) . . . . ?
C201 C202 C203 C204 0.3(4) . . . . ?
C202 C201 C206 C205 -1.0(4) . . . . ?
C202 C201 C207 C209 -176.6(3) . . . . ?
C202 C201 C207 C210 -1.3(5) . . . . ?
C202 C203 C204 C205 -0.8(4) . . . . ?
C202 C203 C204 C208 178.9(3) . . . . ?
C203 C204 C205 C206 0.4(4) . . . . ?
C203 C204 C208 C211 0.3(5) . . . . ?
C203 C204 C208 C212 -179.5(3) . . . . ?
C204 C205 C206 C201 0.5(4) . . . . ?
C205 C204 C208 C211 180.0(3) . . . . ?
C205 C204 C208 C212 0.2(4) . . . . ?
C206 C201 C202 C203 0.6(4) . . . . ?
C206 C201 C207 C209 1.0(5) . . . . ?
C206 C201 C207 C210 176.3(3) . . . . ?
C207 C201 C202 C203 178.3(3) . . . . ?
C207 C201 C206 C205 -178.7(3) . . . . ?
C208 C204 C205 C206 -179.2(3) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.906
_oxdiff_exptl_absorpt_empirical_full_min 0.580
