# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 2002496'
loop_
_audit_author_name
_audit_author_address
'Gary Stephen Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2020-05-07 deposited with the CCDC.	2020-10-05 downloaded from the CCDC.
;
# local name jg19012
_audit_creation_date             2020-05-04
_audit_creation_method           
;
Olex2 1.3-beta
(compiled 2020.04.02 svn.r1fbe7b6f for OlexSys, GUI svn.r6076)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
g.s.nichol@ed.ac.uk
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C51 H61 N2 Na O5, 2(C4 H8 O)'
_chemical_formula_sum            'C59 H77 N2 Na O7'
_chemical_formula_weight         949.21
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C61 H79 N2 Na1 O5'
_chemical_oxdiff_usercomment     '@ 120 K '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      tetragonal
_space_group_IT_number           78
_space_group_name_H-M_alt        'P 43'
_space_group_name_Hall           'P 4cw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x, z+3/4'
'y, -x, z+1/4'

_cell_length_a                   9.8142(4)
_cell_length_b                   9.8142(4)
_cell_length_c                   54.0271(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5203.8(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    15205
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      74.8770
_cell_measurement_theta_min      4.4630
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2048
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 -3 -27 0.0390
-6 1 14 0.0283
0 3 29 0.0523
6 0 -6 0.0147
-2 -6 8 0.0037
3 0 30 0.0521
2 6 -6 0.0323

_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of THF and toluene  by slow cooling'
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.039
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-2.2473 -3.3603 -27.1331 -0.2414 0.0328 0.9699
-5.7507 1.2211 13.5260 0.9780 -0.1279 0.1648
0.3456 3.4915 29.3031 0.5205 -0.0692 -0.8510
6.2870 -0.2378 -5.5189 -0.8909 0.1162 -0.4390
-1.7706 -5.9263 8.4151 -0.0224 -0.8982 0.4391
3.1298 0.3096 30.4946 -0.0130 -0.4640 -0.8857
1.9828 5.9450 -6.3365 0.0215 0.8662 -0.4992

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            10795
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.239
_diffrn_reflns_theta_min         4.505
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.8095
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -75.00  34.00   1.00   25.00    --  -41.67  83.00-128.00  109
  2  ω    -12.00  75.00   1.00   25.00    --   41.67 -83.00 111.00   87
  3  ω     34.00 144.00   1.00   30.00    --  111.00 -83.00 111.00  110
  4  ω    100.00 178.00   1.00   30.00    --  111.00  83.00-128.00   78
  5  ω    -68.00  28.00   1.00   25.00    --  -41.67  57.00 120.00   96
  6  ω   -112.00 -15.00   1.00   25.00    --  -41.67 -57.00 -30.00   97
  7  ω   -126.00 -37.00   1.00   25.00    --  -41.67 178.00  90.00   89
  8  ω     10.00  42.00   1.00   25.00    --   41.67  78.00 -72.37   32
  9  ω    103.00 178.00   1.00   30.00    --  111.00  77.00 -90.00   75
 10  ω     40.00 135.00   1.00   30.00    --  111.00 -45.00  90.00   95
 11  ω     97.00 178.00   1.00   30.00    --  111.00 125.00  60.00   81
 12  ω     87.00 178.00   1.00   30.00    --  111.00  30.00  60.00   91
 13  ω    103.00 178.00   1.00   30.00    --  111.00  77.00   0.00   75
 14  ω     39.00 112.00   1.00   30.00    --  111.00-125.00 -30.00   73
 15  ω     39.00 112.00   1.00   30.00    --  111.00-125.00 120.00   73
 16  ω     97.00 178.00   1.00   30.00    --  111.00 125.00  90.00   81
 17  ω     39.00 112.00   1.00   30.00    --  111.00-125.00-120.00   73
 18  ω     39.00 112.00   1.00   30.00    --  111.00-125.00-180.00   73
 19  ω     39.00 112.00   1.00   30.00    --  111.00-125.00  90.00   73
 20  ω     39.00 112.00   1.00   30.00    --  111.00-125.00 -60.00   73
 21  ω     39.00 112.00   1.00   30.00    --  111.00-125.00   0.00   73
 22  ω     87.00 178.00   1.00   30.00    --  111.00  45.00-180.00   91
 23  ω     97.00 178.00   1.00   30.00    --  111.00 125.00-180.00   81
 24  ω     97.00 178.00   1.00   30.00    --  111.00 125.00 120.00   81
 25  ω   -112.00 -15.00   1.00   25.00    --  -41.67 -57.00-120.00   97
 26  ω   -112.00 -15.00   1.00   25.00    --  -41.67 -57.00 150.00   97
 27  ω   -112.00 -15.00   1.00   25.00    --  -41.67 -57.00  60.00   97
 28  ω   -128.00 -39.00   1.00   25.00    --  -41.67-178.00-120.00   89
 29  ω     10.00  42.00   1.00   25.00    --   41.67  80.00 106.94   32
 30  ω     83.00 167.00   1.00   30.00    --  111.00  61.00 120.00   84
 31  ω     83.00 178.00   1.00   30.00    --  111.00  61.00 -30.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1287592000
_diffrn_orient_matrix_UB_12      0.0595515000
_diffrn_orient_matrix_UB_13      0.0121855000
_diffrn_orient_matrix_UB_21      0.0080028000
_diffrn_orient_matrix_UB_22      0.1245964000
_diffrn_orient_matrix_UB_23      -0.0173030000
_diffrn_orient_matrix_UB_31      -0.0894283000
_diffrn_orient_matrix_UB_32      -0.0745097000
_diffrn_orient_matrix_UB_33      -0.0191104000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.975
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                7788
_reflns_number_total             10795
_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 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.06(19)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         10795
_refine_ls_number_restraints     71
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0690
_refine_ls_restrained_S_all      0.975
_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)+(0.1117P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1656
_refine_ls_wR_factor_ref         0.1760
_refine_special_details          
;The O-bound H atoms were initially located from a difference Fourier map and controlled using the AFIX 147 restraint. The diffraction pattern was twinned. This was deconvoluted with CrysAlisPro.

The measured data set is rather weak and was cut at a resolution of 0.83 A.

#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text340

_ALERT_3_B Low Bond Precision on  C-C Bonds ...............    0.01288 Ang.

Not significant - relatively poor and twinned data

#===============================================================================
220_ALERT_2_C Non-Solvent  Resd 1  C   Ueq(max)/Ueq(min) Range        3.4 Ratio
234_ALERT_4_C Large Hirshfeld Difference C40      --C41      .       0.17 Ang.
243_ALERT_4_C High   'Solvent' Ueq as Compared to Neighbors of         O6 Check
243_ALERT_4_C High   'Solvent' Ueq as Compared to Neighbors of         O7 Check
244_ALERT_4_C Low    'Solvent' Ueq as Compared to Neighbors of        C52 Check
244_ALERT_4_C Low    'Solvent' Ueq as Compared to Neighbors of        C56 Check
244_ALERT_4_C Low    'Solvent' Ueq as Compared to Neighbors of        C57 Check
244_ALERT_4_C Low    'Solvent' Ueq as Compared to Neighbors of        C59 Check

All pertains to solvent THF906_ALERT_3_C Large K Value in the Analysis of Variance ......      2.271 Check
918_ALERT_3_C Reflection(s) with I(obs) much Smaller I(calc) .          4 Check
#===============================================================================,Twin
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.500(3)
 0.500(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
O7 \\sim C56 \\sim C57 \\sim C58 \\sim C59: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 O7, C56, C57, C58, C59
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O6, C52, C53, C54, C55} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O7, C56, C57, C58, C59}
6.a Ternary CH refined with riding coordinates:
 C2(H2), C27(H27)
6.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C18(H18A,H18B), C28(H28A,H28B),
 C29(H29A,H29B), C30(H30A,H30B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B),
  C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,
 H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B),
 C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B)
6.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C21(H21), C23(H23), C32(H32), C33(H33), C34(H34), C35(H35),
  C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
6.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C)
6.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 0.6512(3) 0.0735(3) 0.54384(6) 0.0297(6) Uani 1 1 d . . . . .
O1 O 0.5792(6) 0.0986(6) 0.50441(9) 0.0293(12) Uani 1 1 d . . . . .
H1 H 0.526308 0.158444 0.509989 0.035 Uiso 1 1 calc R U . . .
O2 O 0.4812(5) 0.2427(5) 0.54231(10) 0.0273(11) Uani 1 1 d . . . . .
O3 O 0.6165(5) 0.1407(6) 0.58323(9) 0.0315(12) Uani 1 1 d . . . . .
H3 H 0.546054 0.175684 0.577122 0.038 Uiso 1 1 calc R U . . .
O4 O 0.5752(9) -0.1459(7) 0.54395(13) 0.0563(18) Uani 1 1 d . . . . .
O5 O 0.8774(6) 0.1152(7) 0.54338(12) 0.0465(16) Uani 1 1 d . . . . .
N1 N 0.4147(7) 0.2868(6) 0.48450(11) 0.0237(13) Uani 1 1 d . . . . .
N2 N 0.4325(7) 0.3138(6) 0.60071(11) 0.0253(13) Uani 1 1 d . . . . .
C1 C 0.5971(7) 0.1184(7) 0.47865(12) 0.0214(15) Uani 1 1 d . . . . .
C2 C 0.4609(8) 0.1736(8) 0.46804(12) 0.0247(16) Uani 1 1 d . . . . .
H2 H 0.391659 0.099001 0.468698 0.030 Uiso 1 1 calc R U . . .
C3 C 0.4637(8) 0.2315(9) 0.44169(14) 0.0303(18) Uani 1 1 d . . . . .
H3A H 0.379725 0.207005 0.432565 0.036 Uiso 1 1 calc R U . . .
H3B H 0.543650 0.197280 0.432422 0.036 Uiso 1 1 calc R U . . .
C4 C 0.4730(9) 0.3873(9) 0.44558(14) 0.0318(18) Uani 1 1 d . . . . .
H4A H 0.435493 0.437717 0.431253 0.038 Uiso 1 1 calc R U . . .
H4B H 0.568134 0.416685 0.448530 0.038 Uiso 1 1 calc R U . . .
C5 C 0.3839(9) 0.4066(9) 0.46893(14) 0.0324(19) Uani 1 1 d . . . . .
H5A H 0.407983 0.492081 0.477624 0.039 Uiso 1 1 calc R U . . .
H5B H 0.286022 0.409195 0.464530 0.039 Uiso 1 1 calc R U . . .
C6 C 0.6369(8) -0.0205(7) 0.46869(13) 0.0259(16) Uani 1 1 d . . . . .
C7 C 0.5577(9) -0.0905(10) 0.45087(15) 0.038(2) Uani 1 1 d . . . . .
H7 H 0.479467 -0.048370 0.443897 0.046 Uiso 1 1 calc R U . . .
C8 C 0.5954(10) -0.2233(9) 0.44350(16) 0.038(2) Uani 1 1 d . . . . .
H8 H 0.541985 -0.270312 0.431581 0.046 Uiso 1 1 calc R U . . .
C9 C 0.7086(10) -0.2851(8) 0.45340(15) 0.0365(19) Uani 1 1 d . . . . .
H9 H 0.732709 -0.374808 0.448468 0.044 Uiso 1 1 calc R U . . .
C10 C 0.7884(9) -0.2154(8) 0.47076(16) 0.0350(19) Uani 1 1 d . . . . .
H10 H 0.867289 -0.257750 0.477450 0.042 Uiso 1 1 calc R U . . .
C11 C 0.7527(9) -0.0842(8) 0.47830(15) 0.0305(17) Uani 1 1 d . . . . .
H11 H 0.807596 -0.037813 0.490070 0.037 Uiso 1 1 calc R U . . .
C12 C 0.7158(8) 0.2200(7) 0.47412(13) 0.0244(16) Uani 1 1 d . . . . .
C13 C 0.7398(9) 0.3282(8) 0.49105(15) 0.0330(18) Uani 1 1 d . . . . .
H13 H 0.684292 0.337746 0.505344 0.040 Uiso 1 1 calc R U . . .
C14 C 0.8432(10) 0.4184(9) 0.48670(16) 0.0385(19) Uani 1 1 d . . . . .
H14 H 0.857527 0.490728 0.498084 0.046 Uiso 1 1 calc R U . . .
C15 C 0.9288(9) 0.4078(9) 0.46599(16) 0.0341(19) Uani 1 1 d . . . . .
H15 H 1.002150 0.469527 0.463573 0.041 Uiso 1 1 calc R U . . .
C16 C 0.9027(8) 0.3039(9) 0.44911(16) 0.0361(19) Uani 1 1 d . . . . .
H16 H 0.957607 0.296532 0.434683 0.043 Uiso 1 1 calc R U . . .
C17 C 0.7984(8) 0.2110(9) 0.45288(15) 0.0320(18) Uani 1 1 d . . . . .
H17 H 0.782654 0.140943 0.441096 0.038 Uiso 1 1 calc R U . . .
C18 C 0.3011(8) 0.2507(8) 0.50090(13) 0.0249(15) Uani 1 1 d . . . . .
H18A H 0.315531 0.157612 0.507476 0.030 Uiso 1 1 calc R U . . .
H18B H 0.215148 0.250585 0.491316 0.030 Uiso 1 1 calc R U . . .
C19 C 0.3869(7) 0.3369(7) 0.54203(14) 0.0227(14) Uani 1 1 d . . . . .
C20 C 0.3727(8) 0.4336(8) 0.56187(12) 0.0236(16) Uani 1 1 d . . . . .
C21 C 0.2711(8) 0.5304(7) 0.56146(15) 0.0276(17) Uani 1 1 d . . . . .
H21 H 0.263892 0.590939 0.575123 0.033 Uiso 1 1 calc R U . . .
C22 C 0.1782(8) 0.5445(8) 0.54212(16) 0.0281(16) Uani 1 1 d . . . . .
C23 C 0.1902(8) 0.4485(7) 0.52294(14) 0.0258(16) Uani 1 1 d . . . . .
H23 H 0.126252 0.452393 0.509755 0.031 Uiso 1 1 calc R U . . .
C24 C 0.2889(8) 0.3494(8) 0.52215(13) 0.0262(16) Uani 1 1 d . . . . .
C25 C 0.0655(11) 0.6487(11) 0.54199(18) 0.047(2) Uani 1 1 d . . . . .
H25A H -0.022635 0.602322 0.540687 0.071 Uiso 1 1 calc R U . . .
H25B H 0.077337 0.709984 0.527837 0.071 Uiso 1 1 calc R U . . .
H25C H 0.068522 0.701523 0.557374 0.071 Uiso 1 1 calc R U . . .
C26 C 0.6032(7) 0.1344(8) 0.60953(12) 0.0235(16) Uani 1 1 d . . . . .
C27 C 0.5433(8) 0.2724(8) 0.61806(12) 0.0234(15) Uani 1 1 d . . . . .
H27 H 0.617142 0.342481 0.617231 0.028 Uiso 1 1 calc R U . . .
C28 C 0.4798(9) 0.2776(9) 0.64393(13) 0.0342(19) Uani 1 1 d . . . . .
H28A H 0.513099 0.201505 0.654313 0.041 Uiso 1 1 calc R U . . .
H28B H 0.501230 0.364883 0.652263 0.041 Uiso 1 1 calc R U . . .
C29 C 0.3285(9) 0.2649(9) 0.63923(14) 0.0345(19) Uani 1 1 d . . . . .
H29A H 0.274757 0.303917 0.653020 0.041 Uiso 1 1 calc R U . . .
H29B H 0.301529 0.168621 0.636738 0.041 Uiso 1 1 calc R U . . .
C30 C 0.3106(9) 0.3485(9) 0.61532(14) 0.0321(18) Uani 1 1 d . . . . .
H30A H 0.226291 0.321989 0.606490 0.038 Uiso 1 1 calc R U . . .
H30B H 0.307339 0.447311 0.618961 0.038 Uiso 1 1 calc R U . . .
C31 C 0.5070(8) 0.0144(8) 0.61608(15) 0.0297(18) Uani 1 1 d . . . . .
C32 C 0.4058(9) -0.0272(8) 0.60000(18) 0.039(2) Uani 1 1 d . . . . .
H32 H 0.397198 0.015539 0.584303 0.047 Uiso 1 1 calc R U . . .
C33 C 0.3155(10) -0.1317(12) 0.6066(2) 0.060(3) Uani 1 1 d . . . . .
H33 H 0.244569 -0.157478 0.595590 0.071 Uiso 1 1 calc R U . . .
C34 C 0.3300(11) -0.1990(11) 0.6296(3) 0.070(4) Uani 1 1 d . . . . .
H34 H 0.271535 -0.272215 0.634085 0.084 Uiso 1 1 calc R U . . .
C35 C 0.4290(10) -0.1562(10) 0.6451(2) 0.053(3) Uani 1 1 d . . . . .
H35 H 0.437422 -0.199272 0.660786 0.063 Uiso 1 1 calc R U . . .
C36 C 0.5195(10) -0.0517(10) 0.63916(17) 0.042(2) Uani 1 1 d . . . . .
H36 H 0.588651 -0.025353 0.650497 0.051 Uiso 1 1 calc R U . . .
C37 C 0.7447(7) 0.1053(8) 0.61979(14) 0.0267(17) Uani 1 1 d . . . . .
C38 C 0.8164(9) -0.0043(10) 0.60990(16) 0.038(2) Uani 1 1 d . . . . .
H38 H 0.776615 -0.057984 0.597167 0.045 Uiso 1 1 calc R U . . .
C39 C 0.9476(9) -0.0359(10) 0.61871(19) 0.044(2) Uani 1 1 d . . . . .
H39 H 0.995725 -0.110758 0.611784 0.053 Uiso 1 1 calc R U . . .
C40 C 1.0071(9) 0.0395(10) 0.63713(18) 0.045(2) Uani 1 1 d . . . . .
H40 H 1.096212 0.018559 0.642837 0.053 Uiso 1 1 calc R U . . .
C41 C 0.9338(11) 0.1478(12) 0.6473(2) 0.056(3) Uani 1 1 d . . . . .
H41 H 0.971852 0.199038 0.660549 0.067 Uiso 1 1 calc R U . . .
C42 C 0.8039(10) 0.1816(11) 0.63815(17) 0.044(2) Uani 1 1 d . . . . .
H42 H 0.756787 0.257973 0.644728 0.052 Uiso 1 1 calc R U . . .
C43 C 0.4710(8) 0.4250(8) 0.58350(13) 0.0248(16) Uani 1 1 d . . . . .
H43A H 0.564332 0.408649 0.577194 0.030 Uiso 1 1 calc R U . . .
H43B H 0.471195 0.512795 0.592526 0.030 Uiso 1 1 calc R U . . .
C44 C 0.4664(12) -0.1936(12) 0.5289(3) 0.067(3) Uani 1 1 d . . . . .
H44A H 0.443951 -0.126299 0.515876 0.080 Uiso 1 1 calc R U . . .
H44B H 0.384016 -0.210661 0.538999 0.080 Uiso 1 1 calc R U . . .
C45 C 0.5174(12) -0.3234(11) 0.51763(18) 0.056(3) Uani 1 1 d . . . . .
H45A H 0.543223 -0.309411 0.500100 0.068 Uiso 1 1 calc R U . . .
H45B H 0.447118 -0.395606 0.518515 0.068 Uiso 1 1 calc R U . . .
C46 C 0.6401(13) -0.3608(12) 0.5330(2) 0.061(3) Uani 1 1 d . . . . .
H46A H 0.725197 -0.350800 0.523317 0.073 Uiso 1 1 calc R U . . .
H46B H 0.633318 -0.455604 0.539122 0.073 Uiso 1 1 calc R U . . .
C47 C 0.6351(16) -0.2583(12) 0.5545(2) 0.073(4) Uani 1 1 d . . . . .
H47A H 0.579661 -0.293647 0.568355 0.087 Uiso 1 1 calc R U . . .
H47B H 0.727775 -0.236895 0.560551 0.087 Uiso 1 1 calc R U . . .
C48 C 0.9955(10) 0.0563(14) 0.5328(2) 0.060(3) Uani 1 1 d . . . . .
H48A H 1.022107 0.104896 0.517502 0.073 Uiso 1 1 calc R U . . .
H48B H 0.980104 -0.040969 0.528848 0.073 Uiso 1 1 calc R U . . .
C49 C 1.1046(10) 0.0717(12) 0.5527(2) 0.055(3) Uani 1 1 d . . . . .
H49A H 1.195131 0.087458 0.545127 0.066 Uiso 1 1 calc R U . . .
H49B H 1.109210 -0.010750 0.563205 0.066 Uiso 1 1 calc R U . . .
C50 C 1.0599(10) 0.1953(11) 0.56783(17) 0.049(3) Uani 1 1 d . . . . .
H50A H 1.048552 0.171465 0.585517 0.059 Uiso 1 1 calc R U . . .
H50B H 1.126411 0.270723 0.566371 0.059 Uiso 1 1 calc R U . . .
C51 C 0.9258(12) 0.2325(11) 0.5562(2) 0.058(3) Uani 1 1 d . . . . .
H51A H 0.859775 0.260233 0.569110 0.070 Uiso 1 1 calc R U . . .
H51B H 0.937952 0.309386 0.544546 0.070 Uiso 1 1 calc R U . . .
O6 O 0.1498(13) -0.3104(9) 0.4522(2) 0.107(4) Uani 1 1 d D . . . .
C52 C 0.2192(13) -0.2618(12) 0.47269(19) 0.060(3) Uani 1 1 d D . . . .
H52A H 0.318072 -0.256428 0.469218 0.073 Uiso 1 1 calc R U . . .
H52B H 0.204927 -0.322980 0.487027 0.073 Uiso 1 1 calc R U . . .
C53 C 0.1630(12) -0.1225(10) 0.47808(18) 0.054(3) Uani 1 1 d D . . . .
H53A H 0.231648 -0.063877 0.486229 0.064 Uiso 1 1 calc R U . . .
H53B H 0.080556 -0.127655 0.488606 0.064 Uiso 1 1 calc R U . . .
C54 C 0.1290(12) -0.0713(11) 0.4523(2) 0.064(3) Uani 1 1 d D . . . .
H54A H 0.040647 -0.022580 0.452146 0.077 Uiso 1 1 calc R U . . .
H54B H 0.200834 -0.009137 0.446076 0.077 Uiso 1 1 calc R U . . .
C55 C 0.1219(16) -0.1983(12) 0.4368(2) 0.071(3) Uani 1 1 d D . . . .
H55A H 0.030071 -0.207647 0.429431 0.085 Uiso 1 1 calc R U . . .
H55B H 0.189486 -0.193676 0.423230 0.085 Uiso 1 1 calc R U . . .
O7 O 0.8759(17) 0.5973(15) 0.64367(17) 0.144(6) Uani 1 1 d D U . . .
C56 C 0.7715(12) 0.6208(12) 0.6269(2) 0.064(3) Uani 1 1 d D U . . .
H56A H 0.742137 0.717260 0.627516 0.077 Uiso 1 1 calc R U . . .
H56B H 0.692134 0.561935 0.630617 0.077 Uiso 1 1 calc R U . . .
C57 C 0.8314(11) 0.5863(12) 0.60184(18) 0.058(3) Uani 1 1 d D U . . .
H57A H 0.764926 0.535529 0.591594 0.069 Uiso 1 1 calc R U . . .
H57B H 0.858886 0.669990 0.592896 0.069 Uiso 1 1 calc R U . . .
C58 C 0.9516(16) 0.5006(18) 0.6077(2) 0.089(5) Uani 1 1 d D U . . .
H58A H 0.929152 0.402565 0.606282 0.107 Uiso 1 1 calc R U . . .
H58B H 1.028511 0.521598 0.596452 0.107 Uiso 1 1 calc R U . . .
C59 C 0.9851(16) 0.5370(17) 0.6334(3) 0.092(4) Uani 1 1 d D U . . .
H59A H 1.009477 0.454133 0.642843 0.110 Uiso 1 1 calc R U . . .
H59B H 1.063894 0.599931 0.633691 0.110 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Na1 O1 2.258(6) . ?
Na1 O2 2.355(5) . ?
Na1 O3 2.254(6) . ?
Na1 O4 2.278(7) . ?
Na1 O5 2.258(7) . ?
O1 H1 0.8400 . ?
O1 C1 1.416(8) . ?
O2 C19 1.308(8) . ?
O3 H3 0.8400 . ?
O3 C26 1.428(8) . ?
O4 C44 1.422(14) . ?
O4 C47 1.372(13) . ?
O5 C48 1.415(11) . ?
O5 C51 1.426(11) . ?
N1 C2 1.494(9) . ?
N1 C5 1.476(9) . ?
N1 C18 1.468(10) . ?
N2 C27 1.492(9) . ?
N2 C30 1.473(10) . ?
N2 C43 1.483(10) . ?
C1 C2 1.552(10) . ?
C1 C6 1.517(10) . ?
C1 C12 1.552(10) . ?
C2 H2 1.0000 . ?
C2 C3 1.533(10) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.545(12) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.547(11) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.415(11) . ?
C6 C11 1.397(12) . ?
C7 H7 0.9500 . ?
C7 C8 1.411(12) . ?
C8 H8 0.9500 . ?
C8 C9 1.374(13) . ?
C9 H9 0.9500 . ?
C9 C10 1.400(12) . ?
C10 H10 0.9500 . ?
C10 C11 1.395(11) . ?
C11 H11 0.9500 . ?
C12 C13 1.421(10) . ?
C12 C17 1.408(11) . ?
C13 H13 0.9500 . ?
C13 C14 1.366(12) . ?
C14 H14 0.9500 . ?
C14 C15 1.403(13) . ?
C15 H15 0.9500 . ?
C15 C16 1.392(12) . ?
C16 H16 0.9500 . ?
C16 C17 1.386(11) . ?
C17 H17 0.9500 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C24 1.507(10) . ?
C19 C20 1.438(10) . ?
C19 C24 1.447(10) . ?
C20 C21 1.378(11) . ?
C20 C43 1.518(10) . ?
C21 H21 0.9500 . ?
C21 C22 1.393(12) . ?
C22 C23 1.405(11) . ?
C22 C25 1.507(10) . ?
C23 H23 0.9500 . ?
C23 C24 1.374(10) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.547(11) . ?
C26 C31 1.550(11) . ?
C26 C37 1.522(10) . ?
C27 H27 1.0000 . ?
C27 C28 1.531(10) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.512(12) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.540(11) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.382(12) . ?
C31 C36 1.411(12) . ?
C32 H32 0.9500 . ?
C32 C33 1.401(13) . ?
C33 H33 0.9500 . ?
C33 C34 1.417(19) . ?
C34 H34 0.9500 . ?
C34 C35 1.348(17) . ?
C35 H35 0.9500 . ?
C35 C36 1.395(14) . ?
C36 H36 0.9500 . ?
C37 C38 1.392(12) . ?
C37 C42 1.372(12) . ?
C38 H38 0.9500 . ?
C38 C39 1.408(12) . ?
C39 H39 0.9500 . ?
C39 C40 1.371(14) . ?
C40 H40 0.9500 . ?
C40 C41 1.397(16) . ?
C41 H41 0.9500 . ?
C41 C42 1.407(13) . ?
C42 H42 0.9500 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.498(17) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.507(16) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 C47 1.537(16) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C49 1.524(13) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C50 1.527(16) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C50 C51 1.503(16) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
O6 C52 1.386(13) . ?
O6 C55 1.405(13) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C52 C53 1.502(15) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C54 1.520(14) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C54 C55 1.502(14) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
O7 C56 1.386(15) . ?
O7 C59 1.344(17) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C56 C57 1.516(14) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C57 C58 1.483(16) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C58 C59 1.471(16) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Na1 O2 70.6(2) . . ?
O1 Na1 O4 90.2(3) . . ?
O3 Na1 O1 144.3(2) . . ?
O3 Na1 O2 73.7(2) . . ?
O3 Na1 O4 103.0(3) . . ?
O3 Na1 O5 96.1(2) . . ?
O4 Na1 O2 115.7(3) . . ?
O5 Na1 O1 106.1(3) . . ?
O5 Na1 O2 124.6(3) . . ?
O5 Na1 O4 119.6(3) . . ?
Na1 O1 H1 86.0 . . ?
C1 O1 Na1 154.6(5) . . ?
C1 O1 H1 109.5 . . ?
C19 O2 Na1 178.6(5) . . ?
Na1 O3 H3 82.7 . . ?
C26 O3 Na1 160.1(5) . . ?
C26 O3 H3 109.5 . . ?
C44 O4 Na1 123.8(6) . . ?
C47 O4 Na1 128.3(8) . . ?
C47 O4 C44 107.0(9) . . ?
C48 O5 Na1 137.4(6) . . ?
C48 O5 C51 104.7(8) . . ?
C51 O5 Na1 118.0(6) . . ?
C5 N1 C2 108.4(5) . . ?
C18 N1 C2 114.2(6) . . ?
C18 N1 C5 112.4(6) . . ?
C30 N2 C27 108.5(6) . . ?
C30 N2 C43 111.9(6) . . ?
C43 N2 C27 114.1(6) . . ?
O1 C1 C2 107.7(6) . . ?
O1 C1 C6 104.9(6) . . ?
O1 C1 C12 109.7(5) . . ?
C2 C1 C12 111.3(6) . . ?
C6 C1 C2 113.8(6) . . ?
C6 C1 C12 109.2(6) . . ?
N1 C2 C1 107.5(5) . . ?
N1 C2 H2 108.5 . . ?
N1 C2 C3 106.4(6) . . ?
C1 C2 H2 108.5 . . ?
C3 C2 C1 117.2(6) . . ?
C3 C2 H2 108.5 . . ?
C2 C3 H3A 111.0 . . ?
C2 C3 H3B 111.0 . . ?
C2 C3 C4 104.0(6) . . ?
H3A C3 H3B 109.0 . . ?
C4 C3 H3A 111.0 . . ?
C4 C3 H3B 111.0 . . ?
C3 C4 H4A 111.5 . . ?
C3 C4 H4B 111.5 . . ?
C3 C4 C5 101.5(7) . . ?
H4A C4 H4B 109.3 . . ?
C5 C4 H4A 111.5 . . ?
C5 C4 H4B 111.5 . . ?
N1 C5 C4 104.6(6) . . ?
N1 C5 H5A 110.8 . . ?
N1 C5 H5B 110.8 . . ?
C4 C5 H5A 110.8 . . ?
C4 C5 H5B 110.8 . . ?
H5A C5 H5B 108.9 . . ?
C7 C6 C1 122.5(7) . . ?
C11 C6 C1 118.7(6) . . ?
C11 C6 C7 118.8(7) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 C6 119.7(8) . . ?
C8 C7 H7 120.1 . . ?
C7 C8 H8 119.7 . . ?
C9 C8 C7 120.6(8) . . ?
C9 C8 H8 119.7 . . ?
C8 C9 H9 120.1 . . ?
C8 C9 C10 119.8(8) . . ?
C10 C9 H9 120.1 . . ?
C9 C10 H10 119.8 . . ?
C11 C10 C9 120.4(8) . . ?
C11 C10 H10 119.8 . . ?
C6 C11 H11 119.7 . . ?
C10 C11 C6 120.6(7) . . ?
C10 C11 H11 119.7 . . ?
C13 C12 C1 120.2(7) . . ?
C17 C12 C1 121.3(6) . . ?
C17 C12 C13 118.4(7) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 C12 119.8(8) . . ?
C14 C13 H13 120.1 . . ?
C13 C14 H14 118.9 . . ?
C13 C14 C15 122.3(8) . . ?
C15 C14 H14 118.9 . . ?
C14 C15 H15 121.1 . . ?
C16 C15 C14 117.8(8) . . ?
C16 C15 H15 121.1 . . ?
C15 C16 H16 119.3 . . ?
C17 C16 C15 121.4(8) . . ?
C17 C16 H16 119.3 . . ?
C12 C17 H17 119.9 . . ?
C16 C17 C12 120.3(8) . . ?
C16 C17 H17 119.9 . . ?
N1 C18 H18A 109.3 . . ?
N1 C18 H18B 109.3 . . ?
N1 C18 C24 111.4(6) . . ?
H18A C18 H18B 108.0 . . ?
C24 C18 H18A 109.3 . . ?
C24 C18 H18B 109.3 . . ?
O2 C19 C20 121.8(7) . . ?
O2 C19 C24 122.6(7) . . ?
C20 C19 C24 115.7(6) . . ?
C19 C20 C43 118.4(7) . . ?
C21 C20 C19 120.9(7) . . ?
C21 C20 C43 120.7(7) . . ?
C20 C21 H21 118.2 . . ?
C20 C21 C22 123.6(7) . . ?
C22 C21 H21 118.2 . . ?
C21 C22 C23 115.6(6) . . ?
C21 C22 C25 123.4(8) . . ?
C23 C22 C25 120.9(8) . . ?
C22 C23 H23 118.1 . . ?
C24 C23 C22 123.8(7) . . ?
C24 C23 H23 118.1 . . ?
C19 C24 C18 117.3(6) . . ?
C23 C24 C18 122.4(7) . . ?
C23 C24 C19 120.4(7) . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O3 C26 C27 107.1(6) . . ?
O3 C26 C31 108.4(6) . . ?
O3 C26 C37 106.7(6) . . ?
C27 C26 C31 111.4(6) . . ?
C37 C26 C27 113.8(6) . . ?
C37 C26 C31 109.3(6) . . ?
N2 C27 C26 109.2(6) . . ?
N2 C27 H27 108.2 . . ?
N2 C27 C28 105.5(6) . . ?
C26 C27 H27 108.2 . . ?
C28 C27 C26 117.1(6) . . ?
C28 C27 H27 108.2 . . ?
C27 C28 H28A 110.9 . . ?
C27 C28 H28B 110.9 . . ?
H28A C28 H28B 109.0 . . ?
C29 C28 C27 104.1(6) . . ?
C29 C28 H28A 110.9 . . ?
C29 C28 H28B 110.9 . . ?
C28 C29 H29A 111.4 . . ?
C28 C29 H29B 111.4 . . ?
C28 C29 C30 102.0(7) . . ?
H29A C29 H29B 109.2 . . ?
C30 C29 H29A 111.4 . . ?
C30 C29 H29B 111.4 . . ?
N2 C30 C29 103.5(6) . . ?
N2 C30 H30A 111.1 . . ?
N2 C30 H30B 111.1 . . ?
C29 C30 H30A 111.1 . . ?
C29 C30 H30B 111.1 . . ?
H30A C30 H30B 109.0 . . ?
C32 C31 C26 121.3(7) . . ?
C32 C31 C36 118.8(8) . . ?
C36 C31 C26 119.9(7) . . ?
C31 C32 H32 119.6 . . ?
C31 C32 C33 120.8(10) . . ?
C33 C32 H32 119.6 . . ?
C32 C33 H33 119.9 . . ?
C32 C33 C34 120.1(10) . . ?
C34 C33 H33 119.9 . . ?
C33 C34 H34 120.9 . . ?
C35 C34 C33 118.1(11) . . ?
C35 C34 H34 120.9 . . ?
C34 C35 H35 118.5 . . ?
C34 C35 C36 123.0(11) . . ?
C36 C35 H35 118.5 . . ?
C31 C36 H36 120.4 . . ?
C35 C36 C31 119.1(9) . . ?
C35 C36 H36 120.4 . . ?
C38 C37 C26 117.8(7) . . ?
C42 C37 C26 123.2(8) . . ?
C42 C37 C38 119.0(8) . . ?
C37 C38 H38 119.9 . . ?
C37 C38 C39 120.2(9) . . ?
C39 C38 H38 119.9 . . ?
C38 C39 H39 119.5 . . ?
C40 C39 C38 121.1(9) . . ?
C40 C39 H39 119.5 . . ?
C39 C40 H40 120.7 . . ?
C39 C40 C41 118.6(8) . . ?
C41 C40 H40 120.7 . . ?
C40 C41 H41 119.8 . . ?
C40 C41 C42 120.4(10) . . ?
C42 C41 H41 119.8 . . ?
C37 C42 C41 120.7(10) . . ?
C37 C42 H42 119.7 . . ?
C41 C42 H42 119.7 . . ?
N2 C43 C20 111.2(6) . . ?
N2 C43 H43A 109.4 . . ?
N2 C43 H43B 109.4 . . ?
C20 C43 H43A 109.4 . . ?
C20 C43 H43B 109.4 . . ?
H43A C43 H43B 108.0 . . ?
O4 C44 H44A 110.7 . . ?
O4 C44 H44B 110.7 . . ?
O4 C44 C45 105.2(9) . . ?
H44A C44 H44B 108.8 . . ?
C45 C44 H44A 110.7 . . ?
C45 C44 H44B 110.7 . . ?
C44 C45 H45A 110.9 . . ?
C44 C45 H45B 110.9 . . ?
C44 C45 C46 104.5(9) . . ?
H45A C45 H45B 108.9 . . ?
C46 C45 H45A 110.9 . . ?
C46 C45 H45B 110.9 . . ?
C45 C46 H46A 111.1 . . ?
C45 C46 H46B 111.1 . . ?
C45 C46 C47 103.3(10) . . ?
H46A C46 H46B 109.1 . . ?
C47 C46 H46A 111.1 . . ?
C47 C46 H46B 111.1 . . ?
O4 C47 C46 103.2(9) . . ?
O4 C47 H47A 111.1 . . ?
O4 C47 H47B 111.1 . . ?
C46 C47 H47A 111.1 . . ?
C46 C47 H47B 111.1 . . ?
H47A C47 H47B 109.1 . . ?
O5 C48 H48A 110.8 . . ?
O5 C48 H48B 110.8 . . ?
O5 C48 C49 104.5(8) . . ?
H48A C48 H48B 108.9 . . ?
C49 C48 H48A 110.8 . . ?
C49 C48 H48B 110.8 . . ?
C48 C49 H49A 110.8 . . ?
C48 C49 H49B 110.8 . . ?
C48 C49 C50 104.8(9) . . ?
H49A C49 H49B 108.9 . . ?
C50 C49 H49A 110.8 . . ?
C50 C49 H49B 110.8 . . ?
C49 C50 H50A 111.2 . . ?
C49 C50 H50B 111.2 . . ?
H50A C50 H50B 109.1 . . ?
C51 C50 C49 102.8(8) . . ?
C51 C50 H50A 111.2 . . ?
C51 C50 H50B 111.2 . . ?
O5 C51 C50 107.4(9) . . ?
O5 C51 H51A 110.2 . . ?
O5 C51 H51B 110.2 . . ?
C50 C51 H51A 110.2 . . ?
C50 C51 H51B 110.2 . . ?
H51A C51 H51B 108.5 . . ?
C52 O6 C55 107.4(9) . . ?
O6 C52 H52A 110.4 . . ?
O6 C52 H52B 110.4 . . ?
O6 C52 C53 106.7(9) . . ?
H52A C52 H52B 108.6 . . ?
C53 C52 H52A 110.4 . . ?
C53 C52 H52B 110.4 . . ?
C52 C53 H53A 111.4 . . ?
C52 C53 H53B 111.4 . . ?
C52 C53 C54 101.8(8) . . ?
H53A C53 H53B 109.3 . . ?
C54 C53 H53A 111.4 . . ?
C54 C53 H53B 111.4 . . ?
C53 C54 H54A 110.9 . . ?
C53 C54 H54B 110.9 . . ?
H54A C54 H54B 108.9 . . ?
C55 C54 C53 104.2(8) . . ?
C55 C54 H54A 110.9 . . ?
C55 C54 H54B 110.9 . . ?
O6 C55 C54 108.3(9) . . ?
O6 C55 H55A 110.0 . . ?
O6 C55 H55B 110.0 . . ?
C54 C55 H55A 110.0 . . ?
C54 C55 H55B 110.0 . . ?
H55A C55 H55B 108.4 . . ?
C59 O7 C56 113.1(10) . . ?
O7 C56 H56A 110.7 . . ?
O7 C56 H56B 110.7 . . ?
O7 C56 C57 105.1(9) . . ?
H56A C56 H56B 108.8 . . ?
C57 C56 H56A 110.7 . . ?
C57 C56 H56B 110.7 . . ?
C56 C57 H57A 110.9 . . ?
C56 C57 H57B 110.9 . . ?
H57A C57 H57B 108.9 . . ?
C58 C57 C56 104.1(9) . . ?
C58 C57 H57A 110.9 . . ?
C58 C57 H57B 110.9 . . ?
C57 C58 H58A 111.0 . . ?
C57 C58 H58B 111.0 . . ?
H58A C58 H58B 109.0 . . ?
C59 C58 C57 103.9(11) . . ?
C59 C58 H58A 111.0 . . ?
C59 C58 H58B 111.0 . . ?
O7 C59 C58 108.6(12) . . ?
O7 C59 H59A 110.0 . . ?
O7 C59 H59B 110.0 . . ?
C58 C59 H59A 110.0 . . ?
C58 C59 H59B 110.0 . . ?
H59A C59 H59B 108.3 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O2 0.84 1.98 2.668(7) 138.2 . yes
O3 H3 O2 0.84 2.09 2.767(7) 137.1 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Na1 O1 C1 C2 -159.0(9) . . . . ?
Na1 O1 C1 C6 79.5(12) . . . . ?
Na1 O1 C1 C12 -37.7(14) . . . . ?
Na1 O3 C26 C27 -169.3(11) . . . . ?
Na1 O3 C26 C31 -48.9(15) . . . . ?
Na1 O3 C26 C37 68.6(15) . . . . ?
Na1 O4 C44 C45 133.1(7) . . . . ?
Na1 O4 C47 C46 -127.5(8) . . . . ?
Na1 O5 C48 C49 -142.0(8) . . . . ?
Na1 O5 C51 C50 142.9(7) . . . . ?
O1 C1 C2 N1 47.6(7) . . . . ?
O1 C1 C2 C3 167.3(6) . . . . ?
O1 C1 C6 C7 119.0(8) . . . . ?
O1 C1 C6 C11 -58.1(8) . . . . ?
O1 C1 C12 C13 -33.6(10) . . . . ?
O1 C1 C12 C17 148.9(7) . . . . ?
O2 C19 C20 C21 -178.7(7) . . . . ?
O2 C19 C20 C43 0.3(12) . . . . ?
O2 C19 C24 C18 -1.7(12) . . . . ?
O2 C19 C24 C23 178.7(8) . . . . ?
O3 C26 C27 N2 42.4(7) . . . . ?
O3 C26 C27 C28 162.2(6) . . . . ?
O3 C26 C31 C32 -28.8(10) . . . . ?
O3 C26 C31 C36 153.1(7) . . . . ?
O3 C26 C37 C38 -51.4(9) . . . . ?
O3 C26 C37 C42 128.6(8) . . . . ?
O4 C44 C45 C46 15.6(11) . . . . ?
O5 C48 C49 C50 -26.3(12) . . . . ?
N1 C2 C3 C4 21.4(8) . . . . ?
N1 C18 C24 C19 -75.8(9) . . . . ?
N1 C18 C24 C23 103.8(8) . . . . ?
N2 C27 C28 C29 22.4(9) . . . . ?
C1 C2 C3 C4 -98.9(8) . . . . ?
C1 C6 C7 C8 -176.0(7) . . . . ?
C1 C6 C11 C10 176.2(7) . . . . ?
C1 C12 C13 C14 -179.0(8) . . . . ?
C1 C12 C17 C16 179.2(7) . . . . ?
C2 N1 C5 C4 -25.7(8) . . . . ?
C2 N1 C18 C24 161.7(6) . . . . ?
C2 C1 C6 C7 1.6(10) . . . . ?
C2 C1 C6 C11 -175.5(6) . . . . ?
C2 C1 C12 C13 85.5(8) . . . . ?
C2 C1 C12 C17 -92.0(9) . . . . ?
C2 C3 C4 C5 -36.0(8) . . . . ?
C3 C4 C5 N1 38.0(8) . . . . ?
C5 N1 C2 C1 129.0(7) . . . . ?
C5 N1 C2 C3 2.6(8) . . . . ?
C5 N1 C18 C24 -74.3(8) . . . . ?
C6 C1 C2 N1 163.5(6) . . . . ?
C6 C1 C2 C3 -76.8(8) . . . . ?
C6 C1 C12 C13 -148.0(7) . . . . ?
C6 C1 C12 C17 34.5(10) . . . . ?
C6 C7 C8 C9 -0.2(13) . . . . ?
C7 C6 C11 C10 -1.0(11) . . . . ?
C7 C8 C9 C10 -0.7(13) . . . . ?
C8 C9 C10 C11 0.8(13) . . . . ?
C9 C10 C11 C6 0.1(12) . . . . ?
C11 C6 C7 C8 1.1(12) . . . . ?
C12 C1 C2 N1 -72.6(7) . . . . ?
C12 C1 C2 C3 47.1(8) . . . . ?
C12 C1 C6 C7 -123.5(8) . . . . ?
C12 C1 C6 C11 59.4(8) . . . . ?
C12 C13 C14 C15 -0.6(14) . . . . ?
C13 C12 C17 C16 1.6(12) . . . . ?
C13 C14 C15 C16 2.3(14) . . . . ?
C14 C15 C16 C17 -2.0(13) . . . . ?
C15 C16 C17 C12 0.0(13) . . . . ?
C17 C12 C13 C14 -1.3(12) . . . . ?
C18 N1 C2 C1 -104.8(7) . . . . ?
C18 N1 C2 C3 128.8(6) . . . . ?
C18 N1 C5 C4 -152.9(6) . . . . ?
C19 C20 C21 C22 -1.5(12) . . . . ?
C19 C20 C43 N2 -78.4(9) . . . . ?
C20 C19 C24 C18 179.5(6) . . . . ?
C20 C19 C24 C23 -0.1(11) . . . . ?
C20 C21 C22 C23 2.6(13) . . . . ?
C20 C21 C22 C25 178.7(9) . . . . ?
C21 C20 C43 N2 100.7(8) . . . . ?
C21 C22 C23 C24 -2.6(13) . . . . ?
C22 C23 C24 C18 -178.2(8) . . . . ?
C22 C23 C24 C19 1.4(12) . . . . ?
C24 C19 C20 C21 0.1(12) . . . . ?
C24 C19 C20 C43 179.2(6) . . . . ?
C25 C22 C23 C24 -178.8(9) . . . . ?
C26 C27 C28 C29 -99.3(8) . . . . ?
C26 C31 C32 C33 -177.1(8) . . . . ?
C26 C31 C36 C35 177.7(8) . . . . ?
C26 C37 C38 C39 -179.9(8) . . . . ?
C26 C37 C42 C41 178.4(8) . . . . ?
C27 N2 C30 C29 -25.9(8) . . . . ?
C27 N2 C43 C20 163.2(6) . . . . ?
C27 C26 C31 C32 88.7(9) . . . . ?
C27 C26 C31 C36 -89.3(8) . . . . ?
C27 C26 C37 C38 -169.2(7) . . . . ?
C27 C26 C37 C42 10.8(11) . . . . ?
C27 C28 C29 C30 -37.6(8) . . . . ?
C28 C29 C30 N2 39.2(8) . . . . ?
C30 N2 C27 C26 129.2(7) . . . . ?
C30 N2 C27 C28 2.6(8) . . . . ?
C30 N2 C43 C20 -73.1(8) . . . . ?
C31 C26 C27 N2 -75.9(7) . . . . ?
C31 C26 C27 C28 43.8(9) . . . . ?
C31 C26 C37 C38 65.5(9) . . . . ?
C31 C26 C37 C42 -114.5(8) . . . . ?
C31 C32 C33 C34 -1.9(15) . . . . ?
C32 C31 C36 C35 -0.4(13) . . . . ?
C32 C33 C34 C35 2.3(16) . . . . ?
C33 C34 C35 C36 -1.8(16) . . . . ?
C34 C35 C36 C31 0.8(15) . . . . ?
C36 C31 C32 C33 1.0(13) . . . . ?
C37 C26 C27 N2 160.0(6) . . . . ?
C37 C26 C27 C28 -80.2(8) . . . . ?
C37 C26 C31 C32 -144.7(8) . . . . ?
C37 C26 C31 C36 37.3(10) . . . . ?
C37 C38 C39 C40 0.2(14) . . . . ?
C38 C37 C42 C41 -1.6(13) . . . . ?
C38 C39 C40 C41 0.9(14) . . . . ?
C39 C40 C41 C42 -2.5(15) . . . . ?
C40 C41 C42 C37 2.8(15) . . . . ?
C42 C37 C38 C39 0.1(13) . . . . ?
C43 N2 C27 C26 -105.3(7) . . . . ?
C43 N2 C27 C28 128.1(7) . . . . ?
C43 N2 C30 C29 -152.7(6) . . . . ?
C43 C20 C21 C22 179.5(7) . . . . ?
C44 O4 C47 C46 42.1(13) . . . . ?
C44 C45 C46 C47 8.3(11) . . . . ?
C45 C46 C47 O4 -30.4(12) . . . . ?
C47 O4 C44 C45 -37.2(12) . . . . ?
C48 O5 C51 C50 -38.4(11) . . . . ?
C48 C49 C50 C51 3.5(11) . . . . ?
C49 C50 C51 O5 20.5(11) . . . . ?
C51 O5 C48 C49 39.7(11) . . . . ?
O6 C52 C53 C54 -32.9(13) . . . . ?
C52 O6 C55 C54 -20.9(16) . . . . ?
C52 C53 C54 C55 19.3(13) . . . . ?
C53 C54 C55 O6 -0.4(15) . . . . ?
C55 O6 C52 C53 34.2(14) . . . . ?
O7 C56 C57 C58 19.1(15) . . . . ?
C56 O7 C59 C58 -6(2) . . . . ?
C56 C57 C58 C59 -22.3(16) . . . . ?
C57 C58 C59 O7 18.4(19) . . . . ?
C59 O7 C56 C57 -8.2(18) . . . . ?

_olex2_date_sample_data_collection 2019-12-02
_olex2_date_sample_submission    2019-11-20
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil.'
_olex2_submission_original_sample_id WG-03-37
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.705
_oxdiff_exptl_absorpt_empirical_full_min 0.559
_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 0.500(3) 880 82908 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.500(3) 709 82908 nmt 0.9994 0.0008 -0.0002 -0.0006 -1.0004 0.0009 -0.0087
-0.0532 -1.0005

_twin_special_details            
;
Component 2 rotated by -179.4464° 
 around [1.00 -0.00 -0.00] (reciprocal) or [1.00 -0.00 -0.00] (direct)
;
_vrf_PLAT340_1                   
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01288 Ang.  
RESPONSE:  relatively poor, weak and twinned data
;
