# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_ornall
_database_code_depnum_ccdc_archive 'CCDC 1581977'
_audit_update_record             
;
2017-10-25 deposited with the CCDC.
2018-01-04 downloaded from the CCDC.
;
_nottingham_internal_coll_name   ORNALL
_nottingham_internal_coll_number 15684
_nottingham_internal_coll_client RN/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '20.0000, 80.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pcxrn3
_nottingham_internal_coll_date   24/02/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'SN, XDA 017/09'
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 25/02/2016
_nottingham_internal_process_user pcxrn3
_nottingham_internal_solution_date 07/09/2017
_nottingham_internal_solution_user pcxrn3
_nottingham_internal_refinement_date 07/09/2017
_nottingham_internal_refinement_user pcxrn3
_nottingham_internal_self_archive_date ?
_nottingham_internal_self_validation_date 07/09/2017
_nottingham_internal_self_validation_user pcxrn3
_nottingham_internal_validation_date ?
_nottingham_internal_validation_user ?
_nottingham_internal_archive_date ?
_refine_special_details          ?
_audit_creation_date             2017-09-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H39 N3'
_chemical_formula_sum            'C42 H39 N3'
_chemical_formula_weight         585.76
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C42 H39 N3'
_chemical_oxdiff_usercomment     
'ORNALL - #15684 SN-884 IN FOMBLIN FILM ON A MICROMOUNT FOR RN/DLK'
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'

_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                   28.8139(16)
_cell_length_b                   8.5704(4)
_cell_length_c                   13.5865(7)
_cell_angle_alpha                90
_cell_angle_beta                 102.756(5)
_cell_angle_gamma                90
_cell_volume                     3272.3(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6322
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.2120
_cell_measurement_theta_min      4.7120
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.528
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.930
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.1792
_exptl_crystal_size_mid          0.1142
_exptl_crystal_size_min          0.0633
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24982
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.380
_diffrn_reflns_theta_min         4.721
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        
'flash frozen in gaseous N2' # assumed default, please check
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -53.00   -6.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  131.0000  -27.0000 47

#__ type_ start__ end____ width___ exp.time_
  2 omega -117.00   -4.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -19.0000   60.0000 113

#__ type_ start__ end____ width___ exp.time_
  3 omega  -50.00   34.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -120.0000 84

#__ type_ start__ end____ width___ exp.time_
  4 omega   20.00   58.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152   57.0000    0.0000 38

#__ type_ start__ end____ width___ exp.time_
  5 omega   27.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152  -57.0000 -150.0000 42

#__ type_ start__ end____ width___ exp.time_
  6 omega   24.00   80.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152  -99.0000   90.0000 56

#__ type_ start__ end____ width___ exp.time_
  7 omega   42.00   98.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -45.0000   60.0000 56

#__ type_ start__ end____ width___ exp.time_
  8 omega   36.00  121.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322 -125.0000 -150.0000 85

#__ type_ start__ end____ width___ exp.time_
  9 omega   83.00  158.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322   45.0000  -60.0000 75

#__ type_ start__ end____ width___ exp.time_
 10 omega   38.00   91.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000    0.0000 53

#__ type_ start__ end____ width___ exp.time_
 11 omega  127.00  176.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322   45.0000  -30.0000 49

#__ type_ start__ end____ width___ exp.time_
 12 omega   36.00   84.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000  -90.0000 48

#__ type_ start__ end____ width___ exp.time_
 13 omega   82.00  177.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322   45.0000   30.0000 95

#__ type_ start__ end____ width___ exp.time_
 14 omega  101.00  128.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  125.0000 -120.0000 27

#__ type_ start__ end____ width___ exp.time_
 15 omega   84.00  109.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -95.0000  -90.0000 25

#__ type_ start__ end____ width___ exp.time_
 16 omega   61.00   88.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000  120.0000 27

#__ type_ start__ end____ width___ exp.time_
 17 omega  149.00  177.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  125.0000 -120.0000 28

#__ type_ start__ end____ width___ exp.time_
 18 omega   95.00  121.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322 -125.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
 19 omega   37.00   69.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -95.0000  -90.0000 32

#__ type_ start__ end____ width___ exp.time_
 20 omega   98.00  124.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  125.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 21 omega  149.00  178.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  125.0000   30.0000 29

#__ type_ start__ end____ width___ exp.time_
 22 omega   32.00  131.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -77.0000  -60.0000 99

#__ type_ start__ end____ width___ exp.time_
 23 omega  112.00  166.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  131.0000  -27.0000 54

#__ type_ start__ end____ width___ exp.time_
 24 omega  105.00  130.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -77.0000  -30.0000 25
;
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova-Duo, Atlas'
_diffrn_measurement_method       ?
_diffrn_measurement_specimen_support 
'MiTeGen micromount' # assumed default, please check
_diffrn_orient_matrix_UB_11      0.0254750000
_diffrn_orient_matrix_UB_12      -0.0849320000
_diffrn_orient_matrix_UB_13      0.0968659000
_diffrn_orient_matrix_UB_21      -0.0485202000
_diffrn_orient_matrix_UB_22      -0.0403247000
_diffrn_orient_matrix_UB_23      0.0235476000
_diffrn_orient_matrix_UB_31      -0.0013449000
_diffrn_orient_matrix_UB_32      -0.1531885000
_diffrn_orient_matrix_UB_33      -0.0598356000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4764
_reflns_number_total             6597
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         6597
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0565
_refine_ls_restrained_S_all      1.029
_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)+(0.0781P)²+0.5806P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1415
_refine_ls_wR_factor_ref         0.1609
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C7(H7), C9(H9), C21(H21), C23(H23), C24(H24), C25(H25),
 C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C35(H35), C36(H36), C37(H37),
  C38(H38), C40(H40), C41(H41), C42(H42)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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
N1 N 0.27022(6) 0.66567(19) 0.39077(12) 0.0328(3) Uani 1 1 d . . . . .
H1 H 0.2409(10) 0.714(3) 0.367(2) 0.049(7) Uiso 1 1 d . . . . .
N2 N 0.18022(5) 0.59542(19) 0.41673(11) 0.0322(3) Uani 1 1 d . . . . .
N3 N 0.23703(6) 0.9237(2) 0.27490(12) 0.0365(4) Uani 1 1 d . . . . .
C1 C 0.31853(7) 0.8465(2) 0.30909(15) 0.0355(4) Uani 1 1 d . . . . .
C2 C 0.36471(7) 0.8714(3) 0.29714(16) 0.0394(5) Uani 1 1 d . . . . .
H2 H 0.370129 0.954772 0.255004 0.047 Uiso 1 1 calc R . . . .
C3 C 0.40363(7) 0.7798(3) 0.34400(17) 0.0408(5) Uani 1 1 d . . . . .
C4 C 0.39569(7) 0.6554(3) 0.40334(16) 0.0391(5) Uani 1 1 d . . . . .
H4 H 0.421628 0.592027 0.435869 0.047 Uiso 1 1 calc R . . . .
C5 C 0.34963(7) 0.6222(2) 0.41570(14) 0.0347(4) Uani 1 1 d . . . . .
C6 C 0.32888(7) 0.4997(2) 0.46628(14) 0.0341(4) Uani 1 1 d . . . . .
C7 C 0.34614(7) 0.3661(2) 0.51983(15) 0.0382(4) Uani 1 1 d . . . . .
H7 H 0.379211 0.343420 0.532764 0.046 Uiso 1 1 calc R . . . .
C8 C 0.31542(8) 0.2645(3) 0.55494(15) 0.0394(5) Uani 1 1 d . . . . .
C9 C 0.26688(7) 0.3032(2) 0.53662(14) 0.0359(4) Uani 1 1 d . . . . .
H9 H 0.245952 0.234957 0.560887 0.043 Uiso 1 1 calc R . . . .
C10 C 0.24797(7) 0.4372(2) 0.48445(14) 0.0327(4) Uani 1 1 d . . . . .
C11 C 0.27968(7) 0.5334(2) 0.44792(14) 0.0322(4) Uani 1 1 d . . . . .
C12 C 0.31186(7) 0.7189(2) 0.36923(14) 0.0325(4) Uani 1 1 d . . . . .
C13 C 0.45342(8) 0.8232(3) 0.3288(2) 0.0523(6) Uani 1 1 d . . . . .
C14 C 0.45372(10) 0.8123(4) 0.2160(2) 0.0728(9) Uani 1 1 d . . . . .
H14A H 0.447299 0.704479 0.193009 0.109 Uiso 1 1 calc GR . . . .
H14B H 0.484932 0.844402 0.205697 0.109 Uiso 1 1 calc GR . . . .
H14C H 0.429104 0.881075 0.177530 0.109 Uiso 1 1 calc GR . . . .
C15 C 0.46490(9) 0.9900(3) 0.3651(3) 0.0636(7) Uani 1 1 d . . . . .
H15A H 0.443025 1.062106 0.321918 0.095 Uiso 1 1 calc GR . . . .
H15B H 0.497700 1.015032 0.361767 0.095 Uiso 1 1 calc GR . . . .
H15C H 0.461347 0.999978 0.434910 0.095 Uiso 1 1 calc GR . . . .
C16 C 0.49177(8) 0.7159(4) 0.3882(3) 0.0711(9) Uani 1 1 d . . . . .
H16A H 0.491952 0.723241 0.460256 0.107 Uiso 1 1 calc GR . . . .
H16B H 0.522902 0.747524 0.377071 0.107 Uiso 1 1 calc GR . . . .
H16C H 0.485134 0.608101 0.365412 0.107 Uiso 1 1 calc GR . . . .
C17 C 0.33519(9) 0.1165(3) 0.61315(18) 0.0473(5) Uani 1 1 d . . . . .
C18 C 0.36599(15) 0.1648(4) 0.7161(2) 0.0834(11) Uani 1 1 d . . . . .
H18A H 0.389650 0.241850 0.706043 0.125 Uiso 1 1 calc GR . . . .
H18B H 0.382255 0.072851 0.750284 0.125 Uiso 1 1 calc GR . . . .
H18C H 0.345679 0.210598 0.757657 0.125 Uiso 1 1 calc GR . . . .
C19 C 0.36796(10) 0.0298(3) 0.5569(2) 0.0598(7) Uani 1 1 d . . . . .
H19A H 0.350501 0.006124 0.488066 0.090 Uiso 1 1 calc GR . . . .
H19B H 0.378838 -0.067599 0.592307 0.090 Uiso 1 1 calc GR . . . .
H19C H 0.395509 0.095453 0.554219 0.090 Uiso 1 1 calc GR . . . .
C20 C 0.29672(12) 0.0065(4) 0.6287(3) 0.0912(12) Uani 1 1 d . . . . .
H20A H 0.275915 0.059988 0.665984 0.137 Uiso 1 1 calc GR . . . .
H20B H 0.311214 -0.084514 0.667206 0.137 Uiso 1 1 calc GR . . . .
H20C H 0.277990 -0.027532 0.562995 0.137 Uiso 1 1 calc GR . . . .
C21 C 0.19726(7) 0.4740(2) 0.46700(14) 0.0324(4) Uani 1 1 d . . . . .
H21 H 0.176670 0.406994 0.493275 0.039 Uiso 1 1 calc R . . . .
C22 C 0.13064(6) 0.6225(2) 0.39494(13) 0.0318(4) Uani 1 1 d . . . . .
C23 C 0.09829(7) 0.5060(2) 0.36103(14) 0.0346(4) Uani 1 1 d . . . . .
H23 H 0.108994 0.401977 0.356611 0.042 Uiso 1 1 calc R . . . .
C24 C 0.04919(7) 0.5403(3) 0.33270(15) 0.0381(4) Uani 1 1 d . . . . .
H24 H 0.027068 0.458940 0.309551 0.046 Uiso 1 1 calc R . . . .
C25 C 0.03335(7) 0.6888(3) 0.33832(15) 0.0379(4) Uani 1 1 d . . . . .
H25 H 0.000282 0.710276 0.317632 0.045 Uiso 1 1 calc R . . . .
C26 C 0.06534(7) 0.8118(2) 0.37448(13) 0.0337(4) Uani 1 1 d . . . . .
C27 C 0.04965(8) 0.9654(3) 0.38550(15) 0.0401(5) Uani 1 1 d . . . . .
H27 H 0.016554 0.987906 0.368835 0.048 Uiso 1 1 calc R . . . .
C28 C 0.08123(8) 1.0819(3) 0.41968(16) 0.0435(5) Uani 1 1 d . . . . .
H28 H 0.070029 1.184355 0.427706 0.052 Uiso 1 1 calc R . . . .
C29 C 0.13036(8) 1.0511(3) 0.44312(16) 0.0409(5) Uani 1 1 d . . . . .
H29 H 0.152231 1.133615 0.464769 0.049 Uiso 1 1 calc R . . . .
C30 C 0.14689(7) 0.9035(2) 0.43502(14) 0.0358(4) Uani 1 1 d . . . . .
H30 H 0.180151 0.883883 0.452350 0.043 Uiso 1 1 calc R . . . .
C31 C 0.11502(7) 0.7793(2) 0.40110(13) 0.0310(4) Uani 1 1 d . . . . .
C32 C 0.27944(7) 0.9469(2) 0.26235(15) 0.0364(4) Uani 1 1 d . . . . .
H32 H 0.285239 1.031576 0.221580 0.044 Uiso 1 1 calc R . . . .
C33 C 0.20039(8) 1.0304(3) 0.23488(15) 0.0394(5) Uani 1 1 d . . . . .
C34 C 0.15479(7) 0.9655(3) 0.18885(14) 0.0409(5) Uani 1 1 d . . . . .
C35 C 0.14676(8) 0.8041(3) 0.17776(15) 0.0414(5) Uani 1 1 d . . . . .
H35 H 0.172442 0.733827 0.199990 0.050 Uiso 1 1 calc R . . . .
C36 C 0.10253(8) 0.7462(3) 0.13545(16) 0.0484(6) Uani 1 1 d . . . . .
H36 H 0.097698 0.636644 0.129641 0.058 Uiso 1 1 calc R . . . .
C37 C 0.06445(8) 0.8479(4) 0.10078(17) 0.0550(7) Uani 1 1 d . . . . .
H37 H 0.033781 0.807238 0.071995 0.066 Uiso 1 1 calc R . . . .
C38 C 0.07116(8) 1.0027(4) 0.10811(16) 0.0554(7) Uani 1 1 d . . . . .
H38 H 0.045115 1.070148 0.082526 0.066 Uiso 1 1 calc R . . . .
C39 C 0.11639(8) 1.0694(3) 0.15335(16) 0.0473(6) Uani 1 1 d . . . . .
C40 C 0.12395(10) 1.2305(3) 0.16468(18) 0.0561(7) Uani 1 1 d . . . . .
H40 H 0.098305 1.299972 0.140205 0.067 Uiso 1 1 calc R . . . .
C41 C 0.16739(10) 1.2898(3) 0.21017(19) 0.0549(6) Uani 1 1 d . . . . .
H41 H 0.171672 1.399453 0.217486 0.066 Uiso 1 1 calc R . . . .
C42 C 0.20611(9) 1.1876(3) 0.24649(17) 0.0467(5) Uani 1 1 d . . . . .
H42 H 0.236174 1.228960 0.279059 0.056 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
N1 C11 1.367(3) . ?
N1 C12 1.374(2) . ?
N2 C21 1.282(3) . ?
N2 C22 1.413(2) . ?
N3 C32 1.286(3) . ?
N3 C33 1.412(3) . ?
C1 C2 1.392(3) . ?
C1 C12 1.403(3) . ?
C1 C32 1.448(3) . ?
C2 C3 1.401(3) . ?
C3 C4 1.386(3) . ?
C3 C13 1.539(3) . ?
C4 C5 1.403(3) . ?
C5 C6 1.454(3) . ?
C5 C12 1.402(3) . ?
C6 C7 1.389(3) . ?
C6 C11 1.414(3) . ?
C7 C8 1.398(3) . ?
C8 C9 1.405(3) . ?
C8 C17 1.536(3) . ?
C9 C10 1.396(3) . ?
C10 C11 1.400(3) . ?
C10 C21 1.462(3) . ?
C13 C14 1.537(4) . ?
C13 C15 1.524(4) . ?
C13 C16 1.524(4) . ?
C17 C18 1.539(4) . ?
C17 C19 1.532(3) . ?
C17 C20 1.505(4) . ?
C22 C23 1.374(3) . ?
C22 C31 1.425(3) . ?
C23 C24 1.413(3) . ?
C24 C25 1.360(3) . ?
C25 C26 1.415(3) . ?
C26 C27 1.411(3) . ?
C26 C31 1.424(3) . ?
C27 C28 1.362(3) . ?
C28 C29 1.406(3) . ?
C29 C30 1.365(3) . ?
C30 C31 1.415(3) . ?
C33 C34 1.437(3) . ?
C33 C42 1.362(3) . ?
C34 C35 1.405(3) . ?
C34 C39 1.419(3) . ?
C35 C36 1.370(3) . ?
C36 C37 1.399(4) . ?
C37 C38 1.341(4) . ?
C38 C39 1.432(4) . ?
C39 C40 1.401(4) . ?
C40 C41 1.366(4) . ?
C41 C42 1.419(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
C11 N1 C12 108.80(16) . . ?
C21 N2 C22 119.72(16) . . ?
C32 N3 C33 120.06(18) . . ?
C2 C1 C12 116.37(19) . . ?
C2 C1 C32 121.94(19) . . ?
C12 C1 C32 121.68(17) . . ?
C1 C2 C3 123.44(19) . . ?
C2 C3 C13 118.7(2) . . ?
C4 C3 C2 118.49(18) . . ?
C4 C3 C13 122.8(2) . . ?
C3 C4 C5 120.5(2) . . ?
C4 C5 C6 134.53(19) . . ?
C12 C5 C4 119.15(19) . . ?
C12 C5 C6 106.28(16) . . ?
C7 C6 C5 134.92(18) . . ?
C7 C6 C11 119.35(18) . . ?
C11 C6 C5 105.67(17) . . ?
C6 C7 C8 120.76(19) . . ?
C7 C8 C9 118.23(19) . . ?
C7 C8 C17 119.92(19) . . ?
C9 C8 C17 121.8(2) . . ?
C10 C9 C8 123.09(19) . . ?
C9 C10 C11 116.87(18) . . ?
C9 C10 C21 121.60(17) . . ?
C11 C10 C21 121.52(17) . . ?
N1 C11 C6 109.64(16) . . ?
N1 C11 C10 128.71(17) . . ?
C10 C11 C6 121.65(18) . . ?
N1 C12 C1 128.38(18) . . ?
N1 C12 C5 109.58(17) . . ?
C5 C12 C1 122.02(17) . . ?
C14 C13 C3 109.2(2) . . ?
C15 C13 C3 109.0(2) . . ?
C15 C13 C14 109.3(2) . . ?
C16 C13 C3 111.8(2) . . ?
C16 C13 C14 109.1(2) . . ?
C16 C13 C15 108.3(2) . . ?
C8 C17 C18 108.6(2) . . ?
C19 C17 C8 110.1(2) . . ?
C19 C17 C18 106.8(2) . . ?
C20 C17 C8 112.9(2) . . ?
C20 C17 C18 109.6(3) . . ?
C20 C17 C19 108.7(2) . . ?
N2 C21 C10 120.87(17) . . ?
N2 C22 C31 117.40(17) . . ?
C23 C22 N2 122.08(18) . . ?
C23 C22 C31 120.31(17) . . ?
C22 C23 C24 120.35(19) . . ?
C25 C24 C23 120.49(18) . . ?
C24 C25 C26 121.05(18) . . ?
C25 C26 C31 118.91(18) . . ?
C27 C26 C25 122.19(19) . . ?
C27 C26 C31 118.90(18) . . ?
C28 C27 C26 121.0(2) . . ?
C27 C28 C29 120.2(2) . . ?
C30 C29 C28 120.5(2) . . ?
C29 C30 C31 120.71(19) . . ?
C26 C31 C22 118.83(17) . . ?
C30 C31 C22 122.52(17) . . ?
C30 C31 C26 118.63(18) . . ?
N3 C32 C1 121.35(18) . . ?
N3 C33 C34 116.81(19) . . ?
C42 C33 N3 122.3(2) . . ?
C42 C33 C34 120.6(2) . . ?
C35 C34 C33 122.77(19) . . ?
C35 C34 C39 118.9(2) . . ?
C39 C34 C33 118.3(2) . . ?
C36 C35 C34 121.1(2) . . ?
C35 C36 C37 120.2(3) . . ?
C38 C37 C36 120.1(2) . . ?
C37 C38 C39 121.9(2) . . ?
C34 C39 C38 117.6(2) . . ?
C40 C39 C34 119.4(2) . . ?
C40 C39 C38 123.0(2) . . ?
C41 C40 C39 121.4(2) . . ?
C40 C41 C42 120.0(2) . . ?
C33 C42 C41 120.3(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 N2 0.93(3) 2.25(3) 2.760(2) 114(2) . yes
N1 H1 N3 0.93(3) 2.19(3) 2.760(2) 119(2) . yes

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_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
3 -4 -6 0.0802 3.0025 -4.0028 -6.0057 -0.1653 -0.1257 0.9685
18 0 0 0.0254 17.9925 0.0047 -0.0093 0.4571 -0.8734 -0.0244
-18 -1 0 0.0243 -17.9931 -1.0049 0.0085 -0.3722 0.9137 0.1776
-3 4 6 0.0802 -3.0025 4.0028 6.0057 0.1653 0.1257 -0.9685
-6 -4 5 0.0446 -6.0050 -3.9998 5.0006 0.6711 0.5704 0.3216
6 4 -5 0.0446 6.0050 3.9998 -5.0006 -0.6711 -0.5704 -0.3216

_olex2_exptl_crystal_mounting_method "'in fomblin film on a micromount"
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_narnlb
_database_code_depnum_ccdc_archive 'CCDC 1581980'
_audit_update_record             
;
2017-10-25 deposited with the CCDC.
2018-01-04 downloaded from the CCDC.
;
_nottingham_internal_coll_name   NARNLB
_nottingham_internal_coll_number 16059
_nottingham_internal_coll_client RN/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '5.0000, 20.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pcxrn3
_nottingham_internal_coll_date   01/05/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'SN, XDA 017/09'
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 01/05/2016
_nottingham_internal_process_user pcxrn3
_nottingham_internal_solution_date 01/05/2016
_nottingham_internal_solution_user pcxrn3
_nottingham_internal_refinement_date 07/09/2017
_nottingham_internal_refinement_user pcxrn3
_nottingham_internal_self_archive_date 07/09/2017
_nottingham_internal_self_validation_date 07/09/2017
_nottingham_internal_self_validation_user pcxrn3
_nottingham_internal_validation_date 20/10/2017
_nottingham_internal_validation_user pczwl
_nottingham_internal_archive_date 20/10/2017
_refine_special_details          
'The iso-hexane molecules are disordered across a centre of symmetry. Chemically equivalent bond lengths and angles of the two molecules were restrained to be approximately equal. Iso-hexane(C47-C52) could not be sensibly refined anisotropically, so was refined isotropically. Atoms C44-C45 were disordered over two positions, the models were refined competitively, converging to a ratio of 0.37:0.63. Chemically equivalent bond lengths and angles of the two components were restrained to be approximately equal.'
_vrf_PLAT029_narnlb              
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.936 Note  
RESPONSE: The collection strategy was designed for a monoclinic cell 
(the initial symmetry determined). Subsequent investigation showed that 
the space group was triclinic. However, the sample had degraded and it 
was not possible to collect additional data.
;
_vrf_PLAT911_narnlb              
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L=  0.600        505 Report
RESPONSE: The collection strategy was designed for a monoclinic cell 
(the initial symmetry determined). Subsequent investigation showed that 
the space group was triclinic. However, the sample had degraded and it 
was not possible to collect additional data.
;
_audit_creation_date             2017-10-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C46 H46 N3 Na O, C6 H14'
_chemical_formula_sum            'C52 H60 N3 Na O'
_chemical_formula_weight         766.02
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C51 H49 N3 Na O'
_chemical_oxdiff_usercomment     
'NARNLB #16059 SN-945 in fomblin film on a micromount for RN/DLK'
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      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                   12.1323(9)
_cell_length_b                   13.7056(11)
_cell_length_c                   14.2286(11)
_cell_angle_alpha                90.659(7)
_cell_angle_beta                 106.001(7)
_cell_angle_gamma                103.336(7)
_cell_volume                     2205.8(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3926
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.9810
_cell_measurement_theta_min      4.4220
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.1705
_exptl_crystal_size_mid          0.1299
_exptl_crystal_size_min          0.0856
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0767
_diffrn_reflns_Laue_measured_fraction_full 0.936
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16325
_diffrn_reflns_point_group_measured_fraction_full 0.936
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.591
_diffrn_reflns_theta_min         3.908
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        
'flash frozen in gaseous N2' # assumed default, please check
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -65.00   32.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   57.0000 -180.0000 97

#__ type_ start__ end____ width___ exp.time_
  2 omega -109.00  -12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000   30.0000 97

#__ type_ start__ end____ width___ exp.time_
  3 omega   17.00  113.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152   57.0000   30.0000 96

#__ type_ start__ end____ width___ exp.time_
  4 omega   31.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000   60.0000 60

#__ type_ start__ end____ width___ exp.time_
  5 omega   31.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000  150.0000 60

#__ type_ start__ end____ width___ exp.time_
  6 omega   32.00  138.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -77.0000   90.0000 106

#__ type_ start__ end____ width___ exp.time_
  7 omega   82.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322   30.0000    0.0000 96

#__ type_ start__ end____ width___ exp.time_
  8 omega   94.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  125.0000 -180.0000 84

#__ type_ start__ end____ width___ exp.time_
  9 omega   61.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322   15.0000  -30.0000 117

#__ type_ start__ end____ width___ exp.time_
 10 omega   35.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322 -125.0000  -60.0000 86

#__ type_ start__ end____ width___ exp.time_
 11 omega   21.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152   38.0000 -150.0000 95

#__ type_ start__ end____ width___ exp.time_
 12 omega   12.00  117.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152   77.0000 -120.0000 105

#__ type_ start__ end____ width___ exp.time_
 13 omega  -29.00   66.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152  -38.0000  -90.0000 95

#__ type_ start__ end____ width___ exp.time_
 14 omega   61.00   86.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322   15.0000  150.0000 25
;
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova-Duo, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 
'MiTeGen micromount' # assumed default, please check
_diffrn_orient_matrix_UB_11      0.0630433000
_diffrn_orient_matrix_UB_12      0.1079140000
_diffrn_orient_matrix_UB_13      -0.0133529000
_diffrn_orient_matrix_UB_21      0.1203144000
_diffrn_orient_matrix_UB_22      -0.0216538000
_diffrn_orient_matrix_UB_23      0.0517550000
_diffrn_orient_matrix_UB_31      0.0098739000
_diffrn_orient_matrix_UB_32      -0.0362879000
_diffrn_orient_matrix_UB_33      -0.0995606000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5411
_reflns_number_total             8049
_reflns_odcompleteness_completeness 93.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         8049
_refine_ls_number_restraints     213
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0808
_refine_ls_restrained_S_all      1.067
_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)+(0.1265P)²+1.7844P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2270
_refine_ls_wR_factor_ref         0.2593
_olex2_refinement_description    
;
1. 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 C(H,H,H) groups
2. Restrained distances
 C56-C55 \\sim C50-C49
 with sigma of 0.02
 C55-C54 \\sim C48-C49
 with sigma of 0.02
 C58-C54 \\sim C54-C53 \\sim C48-C47 \\sim C48-C52
 with sigma of 0.02
 C56-C54 \\sim C50-C48
 with sigma of 0.02
 C49-C52 \\sim C49-C47 \\sim C55-C53 \\sim C55-C58
 with sigma of 0.02
 C53-C58 \\sim C52-C47
 with sigma of 0.02
 C50-C51 \\sim C56-C57
 with sigma of 0.02
 C57-C55 \\sim C51-C49
 with sigma of 0.02
 C45-C44 \\sim C45A-C44
 with sigma of 0.02
 C46-C45 \\sim C46A-C45A
 with sigma of 0.02
 O1-C46 \\sim O1-C46A
 with sigma of 0.02
 O1-C43 \\sim O1-C46 \\sim O1-C46A
 with sigma of 0.02
 C44-C43 \\sim C46-C45 \\sim C46A-C45A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C53 \\sim C55 \\sim C54 \\sim C56 \\sim C58 \\sim C57 \\sim C50 \\sim C49 \\sim
C48 \\sim C51 \\sim C52 \\sim C47: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
O1 \\sim C46A \\sim C46 \\sim C45 \\sim C45A \\sim C44 \\sim C43: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C50, C49, C48, C51, C52, C47, C54, C55, C56, C53, C58, C57
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C46A, C46, C45, C45A, C44, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H44C)=Sof(H44D)=Sof(C45A)=Sof(H45C)=Sof(H45D)=Sof(C46A)=Sof(H46C)=
 Sof(H46D)=1-FVAR(1)
 Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=
 FVAR(1)
 Fixed Sof: C55(0.5) H55A(0.5) H55B(0.5) C54(0.5) H54(0.5) C57(0.5) H57A(0.5)
 H57B(0.5) H57C(0.5) C53(0.5) H53A(0.5) H53B(0.5) H53C(0.5) C58(0.5) H58A(0.5)
 H58B(0.5) H58C(0.5) C49(0.5) H49A(0.5) H49B(0.5) C52(0.5) H52A(0.5) H52B(0.5)
 H52C(0.5) C47(0.5) H47A(0.5) H47B(0.5) H47C(0.5) C51(0.5) H51A(0.5) H51B(0.5)
 H51C(0.5) C56(0.5) H56A(0.5) H56B(0.5) C50(0.5) H50A(0.5) H50B(0.5) C48(0.5)
 H48(0.5)
6.a Ternary CH refined with riding coordinates:
 C54(H54), C48(H48)
6.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C44(H44A,H44B), C44(H44C,H44D), C45(H45A,H45B), C46(H46A,
 H46B), C55(H55A,H55B), C49(H49A,H49B), C56(H56A,H56B), C50(H50A,H50B),
 C45A(H45C,H45D), C46A(H46C,H46D)
6.c Me refined with riding coordinates:
 C51(H51A,H51B,H51C)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C7(H7), C9(H9), C21(H21), C23(H23), C24(H24), C25(H25),
 C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C35(H35), C36(H36), C37(H37),
  C38(H38), C40(H40), C41(H41), C42(H42)
6.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C57(H57A,H57B,H57C), C53(H53A,
 H53B,H53C), C58(H58A,H58B,H58C), C52(H52A,H52B,H52C), C47(H47A,H47B,H47C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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 0.40014(12) 0.75943(12) 0.08112(11) 0.0430(4) Uani 1 1 d . . . . .
O1 O 0.5006(3) 0.7524(3) 0.2421(2) 0.0640(9) Uani 1 1 d D U . . .
N1 N 0.2679(2) 0.7277(2) -0.0718(2) 0.0284(6) Uani 1 1 d . . . . .
N2 N 0.5202(2) 0.7020(2) -0.0054(2) 0.0304(6) Uani 1 1 d . . . . .
N3 N 0.2537(2) 0.8402(2) 0.1078(2) 0.0301(6) Uani 1 1 d . . . . .
C1 C 0.0954(3) 0.7852(2) -0.0439(2) 0.0283(7) Uani 1 1 d . . . . .
C2 C -0.0228(3) 0.7883(2) -0.0901(2) 0.0294(7) Uani 1 1 d . . . . .
H2 H -0.063468 0.816310 -0.052609 0.035 Uiso 1 1 calc R . . . .
C3 C -0.0835(3) 0.7529(2) -0.1874(3) 0.0294(7) Uani 1 1 d . . . . .
C4 C -0.0230(3) 0.7105(2) -0.2416(2) 0.0295(7) Uani 1 1 d . . . . .
H4 H -0.061298 0.686181 -0.308162 0.035 Uiso 1 1 calc R . . . .
C5 C 0.0933(3) 0.7039(2) -0.1986(2) 0.0265(7) Uani 1 1 d . . . . .
C6 C 0.1743(3) 0.6633(2) -0.2341(2) 0.0276(7) Uani 1 1 d . . . . .
C7 C 0.1679(3) 0.6177(2) -0.3236(3) 0.0310(7) Uani 1 1 d . . . . .
H7 H 0.097343 0.608270 -0.376119 0.037 Uiso 1 1 calc R . . . .
C8 C 0.2645(3) 0.5851(2) -0.3376(3) 0.0318(7) Uani 1 1 d . . . . .
C9 C 0.3658(3) 0.5999(2) -0.2567(3) 0.0309(7) Uani 1 1 d . . . . .
H9 H 0.431159 0.577176 -0.264808 0.037 Uiso 1 1 calc R . . . .
C10 C 0.3768(3) 0.6458(2) -0.1649(3) 0.0287(7) Uani 1 1 d . . . . .
C11 C 0.2789(3) 0.6802(2) -0.1523(3) 0.0286(7) Uani 1 1 d . . . . .
C12 C 0.1545(3) 0.7415(2) -0.1001(3) 0.0275(7) Uani 1 1 d . . . . .
C13 C -0.2108(3) 0.7598(3) -0.2360(3) 0.0350(8) Uani 1 1 d . . . . .
C14 C -0.2894(3) 0.6538(4) -0.2691(4) 0.0596(13) Uani 1 1 d . . . . .
H14A H -0.259562 0.621053 -0.315155 0.089 Uiso 1 1 calc GR . . . .
H14B H -0.370510 0.657882 -0.301419 0.089 Uiso 1 1 calc GR . . . .
H14C H -0.288384 0.614453 -0.211890 0.089 Uiso 1 1 calc GR . . . .
C15 C -0.2139(4) 0.8215(4) -0.3250(3) 0.0590(12) Uani 1 1 d . . . . .
H15A H -0.162429 0.889061 -0.303999 0.088 Uiso 1 1 calc GR . . . .
H15B H -0.295019 0.826531 -0.355778 0.088 Uiso 1 1 calc GR . . . .
H15C H -0.186085 0.788481 -0.372341 0.088 Uiso 1 1 calc GR . . . .
C16 C -0.2614(3) 0.8093(3) -0.1669(3) 0.0424(9) Uani 1 1 d . . . . .
H16A H -0.259425 0.771188 -0.108837 0.064 Uiso 1 1 calc GR . . . .
H16B H -0.343281 0.810300 -0.200551 0.064 Uiso 1 1 calc GR . . . .
H16C H -0.214108 0.878410 -0.146711 0.064 Uiso 1 1 calc GR . . . .
C17 C 0.2557(3) 0.5356(3) -0.4375(3) 0.0403(9) Uani 1 1 d . . . . .
C18 C 0.2202(4) 0.6040(4) -0.5174(3) 0.0619(13) Uani 1 1 d . . . . .
H18A H 0.278044 0.669172 -0.503236 0.093 Uiso 1 1 calc GR . . . .
H18B H 0.141913 0.613791 -0.520002 0.093 Uiso 1 1 calc GR . . . .
H18C H 0.217548 0.573180 -0.580758 0.093 Uiso 1 1 calc GR . . . .
C19 C 0.1635(4) 0.4352(4) -0.4565(4) 0.0589(12) Uani 1 1 d . . . . .
H19A H 0.153068 0.405267 -0.522252 0.088 Uiso 1 1 calc GR . . . .
H19B H 0.088041 0.446209 -0.452044 0.088 Uiso 1 1 calc GR . . . .
H19C H 0.190153 0.389565 -0.407531 0.088 Uiso 1 1 calc GR . . . .
C20 C 0.3735(4) 0.5157(4) -0.4408(3) 0.0558(12) Uani 1 1 d . . . . .
H20A H 0.434483 0.579118 -0.426172 0.084 Uiso 1 1 calc GR . . . .
H20B H 0.365313 0.486586 -0.506313 0.084 Uiso 1 1 calc GR . . . .
H20C H 0.396208 0.468648 -0.392023 0.084 Uiso 1 1 calc GR . . . .
C21 C 0.4889(3) 0.6563(2) -0.0906(3) 0.0299(7) Uani 1 1 d . . . . .
H21 H 0.544732 0.625985 -0.107132 0.036 Uiso 1 1 calc R . . . .
C22 C 0.6353(3) 0.7026(3) 0.0576(3) 0.0313(7) Uani 1 1 d . . . . .
C23 C 0.6659(3) 0.6158(3) 0.0869(3) 0.0402(9) Uani 1 1 d . . . . .
H23 H 0.612238 0.552843 0.061716 0.048 Uiso 1 1 calc R . . . .
C24 C 0.7769(3) 0.6188(3) 0.1547(3) 0.0464(10) Uani 1 1 d . . . . .
H24 H 0.797172 0.557995 0.175265 0.056 Uiso 1 1 calc R . . . .
C25 C 0.8548(3) 0.7091(3) 0.1904(3) 0.0427(9) Uani 1 1 d . . . . .
H25 H 0.929199 0.710343 0.235670 0.051 Uiso 1 1 calc R . . . .
C26 C 0.8267(3) 0.8004(3) 0.1614(3) 0.0344(8) Uani 1 1 d . . . . .
C27 C 0.9051(3) 0.8956(3) 0.1971(3) 0.0417(9) Uani 1 1 d . . . . .
H27 H 0.980450 0.898874 0.241861 0.050 Uiso 1 1 calc R . . . .
C28 C 0.8745(3) 0.9823(3) 0.1684(3) 0.0438(9) Uani 1 1 d . . . . .
H28 H 0.928279 1.045169 0.193614 0.053 Uiso 1 1 calc R . . . .
C29 C 0.7633(3) 0.9797(3) 0.1014(3) 0.0411(9) Uani 1 1 d . . . . .
H29 H 0.742254 1.040645 0.082168 0.049 Uiso 1 1 calc R . . . .
C30 C 0.6864(3) 0.8898(3) 0.0644(3) 0.0360(8) Uani 1 1 d . . . . .
H30 H 0.612678 0.888492 0.018129 0.043 Uiso 1 1 calc R . . . .
C31 C 0.7145(3) 0.7982(2) 0.0937(2) 0.0299(7) Uani 1 1 d . . . . .
C32 C 0.1454(3) 0.8298(2) 0.0549(3) 0.0302(7) Uani 1 1 d . . . . .
H32 H 0.094348 0.854005 0.084279 0.036 Uiso 1 1 calc R . . . .
C33 C 0.2852(3) 0.8858(2) 0.2044(2) 0.0303(7) Uani 1 1 d . . . . .
C34 C 0.3865(3) 0.9692(2) 0.2329(3) 0.0303(7) Uani 1 1 d . . . . .
C35 C 0.4510(3) 1.0087(3) 0.1671(3) 0.0342(8) Uani 1 1 d . . . . .
H35 H 0.428363 0.978439 0.102072 0.041 Uiso 1 1 calc R . . . .
C36 C 0.5459(3) 1.0901(3) 0.1965(3) 0.0378(8) Uani 1 1 d . . . . .
H36 H 0.588825 1.115627 0.151750 0.045 Uiso 1 1 calc R . . . .
C37 C 0.5800(3) 1.1360(3) 0.2917(3) 0.0419(9) Uani 1 1 d . . . . .
H37 H 0.645143 1.193065 0.310816 0.050 Uiso 1 1 calc R . . . .
C38 C 0.5206(3) 1.0996(3) 0.3572(3) 0.0396(9) Uani 1 1 d . . . . .
H38 H 0.545400 1.131221 0.421832 0.048 Uiso 1 1 calc R . . . .
C39 C 0.4221(3) 1.0149(2) 0.3302(3) 0.0327(7) Uani 1 1 d . . . . .
C40 C 0.3585(3) 0.9750(3) 0.3968(3) 0.0392(8) Uani 1 1 d . . . . .
H40 H 0.382025 1.004992 0.462035 0.047 Uiso 1 1 calc R . . . .
C41 C 0.2641(3) 0.8943(3) 0.3681(3) 0.0394(8) Uani 1 1 d . . . . .
H41 H 0.223037 0.867692 0.413755 0.047 Uiso 1 1 calc R . . . .
C42 C 0.2266(3) 0.8497(3) 0.2711(3) 0.0360(8) Uani 1 1 d . . . . .
H42 H 0.159845 0.793866 0.251834 0.043 Uiso 1 1 calc R . . . .
C43 C 0.4490(5) 0.6933(4) 0.3098(4) 0.0690(13) Uani 1 1 d D U . . .
H43A H 0.455528 0.622952 0.304103 0.083 Uiso 1 1 calc R . . . .
H43B H 0.364427 0.693281 0.296260 0.083 Uiso 1 1 calc R . . . .
C44 C 0.5174(5) 0.7422(5) 0.4097(4) 0.0757(14) Uani 1 1 d D U . . .
H44A H 0.465159 0.765880 0.442621 0.091 Uiso 0.373(16) 1 calc R . P A 1
H44B H 0.555584 0.694696 0.450923 0.091 Uiso 0.373(16) 1 calc R . P A 1
H44C H 0.523356 0.691435 0.458668 0.091 Uiso 0.627(16) 1 calc R . P A 2
H44D H 0.479203 0.792155 0.429856 0.091 Uiso 0.627(16) 1 calc R . P A 2
C45 C 0.6065(14) 0.8274(12) 0.3926(11) 0.060(3) Uani 0.373(16) 1 d D U P A 1
H45A H 0.681949 0.839549 0.445578 0.072 Uiso 0.373(16) 1 calc R . P A 1
H45B H 0.578012 0.889823 0.385635 0.072 Uiso 0.373(16) 1 calc R . P A 1
C46 C 0.6187(10) 0.7884(16) 0.2961(10) 0.057(3) Uani 0.373(16) 1 d D U P A 1
H46A H 0.660153 0.843024 0.264156 0.068 Uiso 0.373(16) 1 calc R . P A 1
H46B H 0.661138 0.734015 0.305817 0.068 Uiso 0.373(16) 1 calc R . P A 1
C55 C 0.0322(9) 1.0208(8) -0.4814(10) 0.071(2) Uani 0.5 1 d D U P B -1
H55A H 0.068716 1.072939 -0.425760 0.085 Uiso 0.5 1 calc R . P B -1
H55B H 0.082380 1.032898 -0.526417 0.085 Uiso 0.5 1 calc R . P B -1
C54 C 0.0379(9) 0.9248(8) -0.4432(8) 0.067(2) Uani 0.5 1 d D U P B -1
H54 H -0.008618 0.915449 -0.394502 0.080 Uiso 0.5 1 calc R . P B -1
C57 C -0.0771(12) 1.1502(10) -0.5557(11) 0.084(3) Uani 0.5 1 d D U P B -1
H57A H -0.051444 1.163593 -0.614807 0.126 Uiso 0.5 1 calc GR . P B -1
H57B H -0.021668 1.195364 -0.500305 0.126 Uiso 0.5 1 calc GR . P B -1
H57C H -0.156301 1.161677 -0.566417 0.126 Uiso 0.5 1 calc GR . P B -1
C53 C 0.1640(9) 0.9213(10) -0.3882(8) 0.079(3) Uani 0.5 1 d D U P B -1
H53A H 0.213359 0.932627 -0.433074 0.118 Uiso 0.5 1 calc GR . P B -1
H53B H 0.163718 0.855274 -0.362419 0.118 Uiso 0.5 1 calc GR . P B -1
H53C H 0.195931 0.973779 -0.333760 0.118 Uiso 0.5 1 calc GR . P B -1
C58 C -0.0174(11) 0.8354(8) -0.5210(10) 0.085(3) Uani 0.5 1 d D U P B -1
H58A H -0.090791 0.845539 -0.565492 0.127 Uiso 0.5 1 calc GR . P B -1
H58B H -0.034814 0.773250 -0.488770 0.127 Uiso 0.5 1 calc GR . P B -1
H58C H 0.038030 0.830347 -0.558529 0.127 Uiso 0.5 1 calc GR . P B -1
C49 C 0.0315(11) 0.4968(14) -0.0025(11) 0.096(4) Uiso 0.5 1 d D U P C -1
H49A H 0.056305 0.566112 -0.020974 0.115 Uiso 0.5 1 calc R . P C -1
H49B H -0.038421 0.497872 0.020171 0.115 Uiso 0.5 1 calc R . P C -1
C52 C 0.1016(11) 0.5488(9) 0.1790(8) 0.081(3) Uiso 0.5 1 d D U P C -1
H52A H 0.099064 0.619513 0.173960 0.121 Uiso 0.5 1 calc GR . P C -1
H52B H 0.171257 0.543812 0.231723 0.121 Uiso 0.5 1 calc GR . P C -1
H52C H 0.029978 0.510817 0.193497 0.121 Uiso 0.5 1 calc GR . P C -1
C47 C 0.2411(12) 0.5339(14) 0.0808(13) 0.124(5) Uiso 0.5 1 d D U P C -1
H47A H 0.274856 0.475435 0.095328 0.186 Uiso 0.5 1 calc GR . P C -1
H47B H 0.286004 0.589590 0.130295 0.186 Uiso 0.5 1 calc GR . P C -1
H47C H 0.245048 0.554238 0.015778 0.186 Uiso 0.5 1 calc GR . P C -1
C51 C -0.1695(15) 0.4376(16) -0.1079(15) 0.137(6) Uiso 0.5 1 d D U P C -1
H51A H -0.211794 0.405139 -0.173812 0.205 Uiso 0.5 1 calc R . P C -1
H51B H -0.194408 0.395043 -0.058999 0.205 Uiso 0.5 1 calc R . P C -1
H51C H -0.187469 0.503101 -0.101704 0.205 Uiso 0.5 1 calc R . P C -1
C56 C -0.0802(12) 1.0369(10) -0.5321(11) 0.083(3) Uani 0.5 1 d D U P B -1
H56A H -0.135213 1.015690 -0.492032 0.100 Uiso 0.5 1 calc R . P B -1
H56B H -0.111765 0.993801 -0.594507 0.100 Uiso 0.5 1 calc R . P B -1
C50 C -0.0237(16) 0.4539(15) -0.0895(12) 0.135(5) Uiso 0.5 1 d D U P C -1
H50A H -0.005015 0.388069 -0.096262 0.162 Uiso 0.5 1 calc R . P C -1
H50B H 0.001943 0.496426 -0.139085 0.162 Uiso 0.5 1 calc R . P C -1
C48 C 0.1084(15) 0.5055(17) 0.0824(12) 0.149(6) Uiso 0.5 1 d D U P C -1
H48 H 0.099351 0.433004 0.095612 0.179 Uiso 0.5 1 calc R . P C -1
C45A C 0.6373(8) 0.7925(8) 0.4004(6) 0.060(2) Uani 0.627(16) 1 d D U P A 2
H45C H 0.687684 0.744232 0.405864 0.072 Uiso 0.627(16) 1 calc R . P A 2
H45D H 0.677615 0.849140 0.451206 0.072 Uiso 0.627(16) 1 calc R . P A 2
C46A C 0.6091(7) 0.8300(9) 0.2980(6) 0.059(2) Uani 0.627(16) 1 d D U P A 2
H46C H 0.592836 0.897484 0.299511 0.071 Uiso 0.627(16) 1 calc R . P A 2
H46D H 0.674917 0.832956 0.268831 0.071 Uiso 0.627(16) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Na1 O1 2.294(3) . ?
Na1 N1 2.287(3) . ?
Na1 N2 2.398(3) . ?
Na1 N3 2.408(3) . ?
O1 C43 1.446(6) . ?
O1 C46 1.395(12) . ?
O1 C46A 1.501(9) . ?
N1 C11 1.364(4) . ?
N1 C12 1.380(4) . ?
N2 C21 1.275(4) . ?
N2 C22 1.435(4) . ?
N3 C32 1.296(4) . ?
N3 C33 1.416(4) . ?
C1 C2 1.415(4) . ?
C1 C12 1.420(5) . ?
C1 C32 1.434(5) . ?
C2 C3 1.397(5) . ?
C3 C4 1.404(5) . ?
C3 C13 1.533(4) . ?
C4 C5 1.399(4) . ?
C5 C6 1.432(4) . ?
C5 C12 1.419(5) . ?
C6 C7 1.387(5) . ?
C6 C11 1.435(4) . ?
C7 C8 1.408(4) . ?
C8 C9 1.405(5) . ?
C8 C17 1.534(5) . ?
C9 C10 1.403(5) . ?
C10 C11 1.428(4) . ?
C10 C21 1.449(4) . ?
C13 C14 1.530(6) . ?
C13 C15 1.528(6) . ?
C13 C16 1.521(5) . ?
C17 C18 1.516(6) . ?
C17 C19 1.528(6) . ?
C17 C20 1.529(5) . ?
C22 C23 1.362(5) . ?
C22 C31 1.426(5) . ?
C23 C24 1.415(5) . ?
C24 C25 1.365(5) . ?
C25 C26 1.407(5) . ?
C26 C27 1.419(5) . ?
C26 C31 1.428(4) . ?
C27 C28 1.359(6) . ?
C28 C29 1.414(5) . ?
C29 C30 1.360(5) . ?
C30 C31 1.413(5) . ?
C33 C34 1.431(5) . ?
C33 C42 1.368(5) . ?
C34 C35 1.414(5) . ?
C34 C39 1.422(5) . ?
C35 C36 1.370(5) . ?
C36 C37 1.397(5) . ?
C37 C38 1.360(6) . ?
C38 C39 1.422(5) . ?
C39 C40 1.418(5) . ?
C40 C41 1.360(5) . ?
C41 C42 1.412(5) . ?
C43 C44 1.493(7) . ?
C44 C45 1.471(14) . ?
C44 C45A 1.502(10) . ?
C45 C46 1.524(14) . ?
C55 C54 1.439(15) . ?
C55 C56 1.424(15) . ?
C54 C53 1.527(12) . ?
C54 C58 1.535(12) . ?
C57 C56 1.586(16) . ?
C49 C50 1.292(18) . ?
C49 C48 1.292(18) . ?
C52 C48 1.521(14) . ?
C47 C48 1.573(15) . ?
C51 C50 1.676(19) . ?
C45A C46A 1.526(10) . ?

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 N2 102.63(12) . . ?
O1 Na1 N3 98.21(12) . . ?
N1 Na1 O1 164.62(15) . . ?
N1 Na1 N2 81.18(10) . . ?
N1 Na1 N3 80.49(10) . . ?
N2 Na1 N3 158.09(12) . . ?
C43 O1 Na1 123.5(3) . . ?
C43 O1 C46A 109.9(4) . . ?
C46 O1 Na1 132.9(8) . . ?
C46 O1 C43 103.3(8) . . ?
C46A O1 Na1 124.0(4) . . ?
C11 N1 Na1 127.2(2) . . ?
C11 N1 C12 104.7(3) . . ?
C12 N1 Na1 127.8(2) . . ?
C21 N2 Na1 128.7(2) . . ?
C21 N2 C22 117.8(3) . . ?
C22 N2 Na1 112.2(2) . . ?
C32 N3 Na1 128.6(2) . . ?
C32 N3 C33 117.2(3) . . ?
C33 N3 Na1 112.51(19) . . ?
C2 C1 C12 117.4(3) . . ?
C2 C1 C32 116.4(3) . . ?
C12 C1 C32 126.2(3) . . ?
C3 C2 C1 124.1(3) . . ?
C2 C3 C4 117.4(3) . . ?
C2 C3 C13 122.8(3) . . ?
C4 C3 C13 119.8(3) . . ?
C5 C4 C3 120.6(3) . . ?
C4 C5 C6 132.9(3) . . ?
C4 C5 C12 121.4(3) . . ?
C12 C5 C6 105.7(3) . . ?
C5 C6 C11 104.4(3) . . ?
C7 C6 C5 133.5(3) . . ?
C7 C6 C11 122.1(3) . . ?
C6 C7 C8 120.9(3) . . ?
C7 C8 C17 119.9(3) . . ?
C9 C8 C7 116.9(3) . . ?
C9 C8 C17 123.2(3) . . ?
C10 C9 C8 124.4(3) . . ?
C9 C10 C11 118.1(3) . . ?
C9 C10 C21 116.7(3) . . ?
C11 C10 C21 125.2(3) . . ?
N1 C11 C6 112.9(3) . . ?
N1 C11 C10 129.5(3) . . ?
C10 C11 C6 117.6(3) . . ?
N1 C12 C1 128.6(3) . . ?
N1 C12 C5 112.4(3) . . ?
C5 C12 C1 119.1(3) . . ?
C14 C13 C3 109.2(3) . . ?
C15 C13 C3 109.3(3) . . ?
C15 C13 C14 109.4(4) . . ?
C16 C13 C3 112.5(3) . . ?
C16 C13 C14 108.1(3) . . ?
C16 C13 C15 108.2(3) . . ?
C18 C17 C8 109.8(3) . . ?
C18 C17 C19 110.0(4) . . ?
C18 C17 C20 108.0(4) . . ?
C19 C17 C8 108.9(3) . . ?
C19 C17 C20 108.4(4) . . ?
C20 C17 C8 111.8(3) . . ?
N2 C21 C10 126.7(3) . . ?
C23 C22 N2 121.6(3) . . ?
C23 C22 C31 120.9(3) . . ?
C31 C22 N2 117.4(3) . . ?
C22 C23 C24 120.5(3) . . ?
C25 C24 C23 120.0(3) . . ?
C24 C25 C26 121.2(3) . . ?
C25 C26 C27 122.8(3) . . ?
C25 C26 C31 119.2(3) . . ?
C27 C26 C31 117.9(3) . . ?
C28 C27 C26 121.2(3) . . ?
C27 C28 C29 120.6(3) . . ?
C30 C29 C28 119.8(3) . . ?
C29 C30 C31 121.1(3) . . ?
C22 C31 C26 118.2(3) . . ?
C30 C31 C22 122.5(3) . . ?
C30 C31 C26 119.3(3) . . ?
N3 C32 C1 126.0(3) . . ?
N3 C33 C34 117.5(3) . . ?
C42 C33 N3 122.4(3) . . ?
C42 C33 C34 120.0(3) . . ?
C35 C34 C33 122.2(3) . . ?
C35 C34 C39 119.0(3) . . ?
C39 C34 C33 118.7(3) . . ?
C36 C35 C34 120.5(3) . . ?
C35 C36 C37 120.5(4) . . ?
C38 C37 C36 120.6(3) . . ?
C37 C38 C39 120.9(3) . . ?
C38 C39 C34 118.4(3) . . ?
C40 C39 C34 119.3(3) . . ?
C40 C39 C38 122.3(3) . . ?
C41 C40 C39 120.6(3) . . ?
C40 C41 C42 120.6(4) . . ?
C33 C42 C41 120.8(3) . . ?
O1 C43 C44 105.9(4) . . ?
C43 C44 C45A 104.8(5) . . ?
C45 C44 C43 104.7(7) . . ?
C44 C45 C46 100.3(11) . . ?
O1 C46 C45 101.5(10) . . ?
C56 C55 C54 118.9(8) . . ?
C55 C54 C53 112.1(9) . . ?
C55 C54 C58 113.9(9) . . ?
C53 C54 C58 109.6(10) . . ?
C48 C49 C50 153.5(19) . . ?
C55 C56 C57 113.9(11) . . ?
C49 C50 C51 109.1(14) . . ?
C49 C48 C52 127.4(14) . . ?
C49 C48 C47 115.0(12) . . ?
C52 C48 C47 108.6(13) . . ?
C44 C45A C46A 103.0(6) . . ?
O1 C46A C45A 103.0(7) . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_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
0 -2 -9 0.0475 -0.0073 -2.0245 -8.9952 -0.0988 -0.4226 0.9690
3 -6 -7 0.0571 2.9941 -6.0255 -6.9958 -0.3681 0.1286 0.9447
2 7 -5 0.0535 2.0036 6.9903 -5.0116 0.9476 -0.1697 0.2651
0 -9 0 0.0389 -0.0063 -9.0067 0.0118 -0.9725 0.1949 0.3256
-1 9 2 0.0382 -0.9934 9.0129 1.9895 0.8834 -0.2117 -0.5349
8 -3 -2 0.0701 8.0043 -3.0158 -2.0099 0.2060 0.9243 0.3886
0 2 8 0.0639 0.0066 2.0219 7.9954 0.1118 0.3708 -0.8693
-8 3 1 0.0899 -8.0050 3.0133 1.0101 -0.1930 -0.9761 -0.2890
-2 -6 6 0.0507 -2.0022 -5.9870 6.0100 -0.8526 0.1998 -0.4009

_olex2_exptl_crystal_mounting_method "'in fomblin film on a micromount"
# This is the default assumed mounting details'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_brnalh
_database_code_depnum_ccdc_archive 'CCDC 1581982'
_audit_update_record             
;
2017-10-25 deposited with the CCDC.
2018-01-04 downloaded from the CCDC.
;
_nottingham_internal_coll_name   BRNALH
_nottingham_internal_coll_number 17093
_nottingham_internal_coll_client RN/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '10.00, 40.00'
_nottingham_internal_coll_frame_width 1.00
_nottingham_internal_coll_user   pcxrn3
_nottingham_internal_coll_date   19/06/2017
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 20/06/2017
_nottingham_internal_process_user pcxrn3
_nottingham_internal_solution_date 20/06/2017
_nottingham_internal_solution_user pcxrn3
_nottingham_internal_refinement_date 07/09/2017
_nottingham_internal_refinement_user pcxrn3
_nottingham_internal_self_archive_date 07/09/2017
_nottingham_internal_self_validation_date 07/09/2017
_nottingham_internal_self_validation_user pcxrn3
_nottingham_internal_validation_date ?
_nottingham_internal_validation_user ?
_nottingham_internal_archive_date ?
_refine_special_details          
;
The N3 anion is disordered over two positions. The occupancies of the two 
components were refined competitively, converging to a ratio of 0.70:0.30. 
Chemically equivalent bonds of the disordered atoms were restrained to be 
approximately equal. Enhanced rigid bond and similarity restraints were 
applied to the thermal parameters of the disordered atoms.       
;
_audit_creation_date             2017-09-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'K, C2 H12 B2 N'
_chemical_formula_sum            'C2 H12 B2 K N'
_chemical_formula_weight         110.85
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C2 H12 B2 K N'
_chemical_oxdiff_usercomment     
'BRNALH #17093 GVB-1367 IN FOMBLIN FILM ON MICROMOUNT FOR RN/DLK'
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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 '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'

_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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.6343(3)
_cell_length_b                   22.8460(8)
_cell_length_c                   13.1641(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.402(3)
_cell_angle_gamma                90
_cell_volume                     2896.63(17)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    5916
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.2280
_cell_measurement_theta_min      4.9840
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.437
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.673
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.017
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             960
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 -3 6 0.0418
4 3 -6 0.0477
-5 5 -5 0.2278
4 -6 6 0.2480
0 15 0 0.0177
-1 -15 0 0.0155

_exptl_crystal_size_max          0.525
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.07
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
-5.0006 -3.0351 5.9995 0.9974 -0.3547 -0.1629
4.0003 3.0320 -5.9996 -0.8807 0.2897 0.2508
-5.0039 5.0010 -4.9989 0.2700 -0.1501 1.0119
4.0040 -6.0074 5.9986 -0.0904 0.0501 -1.0385
-0.0078 15.0013 0.0079 0.1838 0.9008 0.4221
-0.9926 -15.0044 -0.0080 -0.0670 -0.9658 -0.3342

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16081
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.851
_diffrn_reflns_theta_min         3.870
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        
'flash frozen in gaseous N2' # assumed default, please check
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.2349
_diffrn_detector_type            'Agilent Diffraction Atlas S2 detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00  34.00   1.00   10.00    --  -38.50  38.00  30.00   84
  2  ω    -94.00  -2.00   1.00   10.00    --  -38.50 125.00-180.00   92
  3  ω   -117.00  -2.00   1.00   10.00    --  -38.50 -19.00-150.00  115
  4  ω     33.00  98.00   1.00   40.00    --  104.50 -45.00   0.00   65
  5  ω     30.00  91.00   1.00   40.00    --  104.50 -30.00-180.00   61
  6  ω     30.00  91.00   1.00   40.00    --  104.50 -30.00 -60.00   61
  7  ω     23.00 109.00   1.00   40.00    --  104.50 -94.00-120.00   86
  8  ω     33.00  98.00   1.00   40.00    --  104.50 -45.00-120.00   65
  9  ω     33.00  98.00   1.00   40.00    --  104.50 -45.00  30.00   65
 10  ω     40.00  90.00   1.00   40.00    --  104.50 -30.00-150.00   50
 11  ω     75.00 102.00   1.00   40.00    --  104.50  77.00 -60.00   27
 12  ω    104.00 170.00   1.00   40.00    --  104.50  77.00 -60.00   66
 13  ω     45.00  88.00   1.00   40.00    --  104.50 -94.00-180.00   43
 14  ω     59.00  88.00   1.00   40.00    --  104.50 -30.00  60.00   29
;
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Atlas S2'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 
'MiTeGen micromount' # assumed default, please check
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1167928000
_diffrn_orient_matrix_UB_12      0.0121518000
_diffrn_orient_matrix_UB_13      0.0750542000
_diffrn_orient_matrix_UB_21      0.0647821000
_diffrn_orient_matrix_UB_22      0.0600678000
_diffrn_orient_matrix_UB_23      0.0252658000
_diffrn_orient_matrix_UB_31      -0.0879614000
_diffrn_orient_matrix_UB_32      0.0281384000
_diffrn_orient_matrix_UB_33      -0.0862326000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4208
_reflns_number_total             5696
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.089
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.0011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         5696
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0867
_refine_ls_restrained_S_all      1.078
_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)+(0.0973P)²+4.9101P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2180
_refine_ls_wR_factor_ref         0.2395
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All B(H,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 N3-C5 \\sim N3A-C5A \\sim N3-C6 \\sim N3A-C6A
 with sigma of 0.02
 N3A-B5A \\sim N3-B5 \\sim N3A-B6A \\sim N3-B6
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 N3, C5, C6, B5, B6, H5A, H5B, H5C, H6A, H6B, H6C, H5D, H5E, H5F, H6D, H6E,
 H6F, N3A, C6A, B6A, B5A, C5A, H6AA, H6AB, H6AC, H6AD, H6AE, H6AF, H5AA, H5AB,
 H5AC, H5AD, H5AE, H5AF
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(N3A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(B6A)=Sof(H6AD)=Sof(H6AE)=
 Sof(H6AF)=Sof(B5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C5A)=Sof(H5AD)=Sof(H5AE)=
 Sof(H5AF)=1-FVAR(1)
 Sof(N3)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=
 Sof(B5)=Sof(H5D)=Sof(H5E)=Sof(H5F)=Sof(B6)=Sof(H6D)=Sof(H6E)=Sof(H6F)=FVAR(1)
5.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), B1(H1D,H1E,H1F),
 B2(H2D,H2E,H2F), B3(H3D,H3E,H3F), B4(H4D,H4E,H4F), B5(H5D,H5E,H5F), B6(H6D,H6E,
 H6F), B7(H7D,H7E,H7F), B8(H8D,H8E,H8F), C6A(H6AA,H6AB,H6AC), B6A(H6AD,H6AE,
 H6AF), B5A(H5AA,H5AB,H5AC), C5A(H5AD,H5AE,H5AF)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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 0.22973(12) 0.66000(5) 0.36631(9) 0.0590(3) Uani 1 1 d . . . . .
K2 K 0.94110(14) 0.73759(5) 0.58797(8) 0.0625(4) Uani 1 1 d . . . . .
K3 K 0.48721(14) 0.72594(8) 0.63656(9) 0.0865(5) Uani 1 1 d . . . . .
K4 K 0.67439(15) 0.54021(7) 0.58892(12) 0.0853(5) Uani 1 1 d . . . . .
N1 N 0.2637(3) 0.83084(15) 0.3965(3) 0.0405(8) Uani 1 1 d . . . . .
N2 N 0.7420(4) 0.67229(15) 0.3592(3) 0.0406(8) Uani 1 1 d . . . . .
N3 N 0.2093(8) 0.5755(4) 0.6539(6) 0.0452(17) Uani 0.696(10) 1 d D U P A 1
N4 N 0.7336(4) 0.42852(16) 0.8736(3) 0.0408(8) Uani 1 1 d . . . . .
C1 C 0.1395(6) 0.8672(2) 0.4127(4) 0.0621(13) Uani 1 1 d . . . . .
H1A H 0.145851 0.885146 0.480248 0.093 Uiso 1 1 calc GR . . . .
H1B H 0.056215 0.842694 0.407580 0.093 Uiso 1 1 calc GR . . . .
H1C H 0.134123 0.898001 0.360843 0.093 Uiso 1 1 calc GR . . . .
C2 C 0.3876(6) 0.8689(3) 0.4029(4) 0.0665(15) Uani 1 1 d . . . . .
H2A H 0.382080 0.898334 0.348836 0.100 Uiso 1 1 calc GR . . . .
H2B H 0.471259 0.845094 0.394978 0.100 Uiso 1 1 calc GR . . . .
H2C H 0.391580 0.888458 0.469159 0.100 Uiso 1 1 calc GR . . . .
C3 C 0.6444(5) 0.7087(3) 0.2998(5) 0.0656(14) Uani 1 1 d . . . . .
H3A H 0.674750 0.711033 0.229419 0.098 Uiso 1 1 calc GR . . . .
H3B H 0.641646 0.748048 0.329152 0.098 Uiso 1 1 calc GR . . . .
H3C H 0.551546 0.691190 0.301155 0.098 Uiso 1 1 calc GR . . . .
C4 C 0.7452(6) 0.6137(2) 0.3137(4) 0.0658(14) Uani 1 1 d . . . . .
H4A H 0.653337 0.595627 0.317954 0.099 Uiso 1 1 calc GR . . . .
H4B H 0.813819 0.589553 0.350512 0.099 Uiso 1 1 calc GR . . . .
H4C H 0.770735 0.616858 0.242318 0.099 Uiso 1 1 calc GR . . . .
C5 C 0.0974(9) 0.5465(5) 0.5915(9) 0.088(3) Uani 0.696(10) 1 d D U P A 1
H5A H 0.119509 0.504919 0.583521 0.132 Uiso 0.696(10) 1 calc GR U P A 1
H5B H 0.090778 0.565088 0.524416 0.132 Uiso 0.696(10) 1 calc GR U P A 1
H5C H 0.008602 0.550505 0.625528 0.132 Uiso 0.696(10) 1 calc GR U P A 1
C6 C 0.2141(12) 0.5472(4) 0.7539(7) 0.067(3) Uani 0.696(10) 1 d D U P A 1
H6A H 0.123226 0.550771 0.785228 0.100 Uiso 0.696(10) 1 calc GR U P A 1
H6B H 0.284772 0.566291 0.797252 0.100 Uiso 0.696(10) 1 calc GR U P A 1
H6C H 0.237362 0.505767 0.745981 0.100 Uiso 0.696(10) 1 calc GR U P A 1
C7 C 0.6083(6) 0.4496(3) 0.9235(4) 0.0670(14) Uani 1 1 d . . . . .
H7A H 0.611208 0.492379 0.928325 0.100 Uiso 1 1 calc GR . . . .
H7B H 0.604384 0.432782 0.991892 0.100 Uiso 1 1 calc GR . . . .
H7C H 0.525843 0.437655 0.883691 0.100 Uiso 1 1 calc GR . . . .
C8 C 0.8551(6) 0.4490(2) 0.9349(4) 0.0647(14) Uani 1 1 d . . . . .
H8A H 0.850452 0.433073 1.003862 0.097 Uiso 1 1 calc GR . . . .
H8B H 0.854571 0.491894 0.937988 0.097 Uiso 1 1 calc GR . . . .
H8C H 0.940691 0.435701 0.903503 0.097 Uiso 1 1 calc GR . . . .
B1 B 0.2541(6) 0.8020(3) 0.2875(4) 0.0515(13) Uani 1 1 d . . . . .
H1D H 0.173943 0.775622 0.283604 0.077 Uiso 1 1 calc GR . . . .
H1E H 0.339096 0.779822 0.275391 0.077 Uiso 1 1 calc GR . . . .
H1F H 0.243181 0.832742 0.235999 0.077 Uiso 1 1 calc GR . . . .
B2 B 0.2713(6) 0.7822(2) 0.4816(4) 0.0493(12) Uani 1 1 d . . . . .
H2D H 0.288124 0.800698 0.547949 0.074 Uiso 1 1 calc GR . . . .
H2E H 0.347194 0.755071 0.467517 0.074 Uiso 1 1 calc GR . . . .
H2F H 0.183330 0.760709 0.482167 0.074 Uiso 1 1 calc GR . . . .
B3 B 0.6928(6) 0.6681(2) 0.4729(4) 0.0542(13) Uani 1 1 d . . . . .
H3D H 0.600323 0.650256 0.474067 0.081 Uiso 1 1 calc GR . . . .
H3E H 0.689129 0.707422 0.502388 0.081 Uiso 1 1 calc GR . . . .
H3F H 0.758474 0.643973 0.512552 0.081 Uiso 1 1 calc GR . . . .
B4 B 0.8917(5) 0.7004(3) 0.3539(4) 0.0512(12) Uani 1 1 d . . . . .
H4D H 0.955699 0.679214 0.399735 0.077 Uiso 1 1 calc GR . . . .
H4E H 0.887422 0.741569 0.374581 0.077 Uiso 1 1 calc GR . . . .
H4F H 0.924591 0.697857 0.284227 0.077 Uiso 1 1 calc GR . . . .
B5 B 0.171(2) 0.6409(5) 0.6663(15) 0.073(5) Uani 0.696(10) 1 d D U P A 1
H5D H 0.076802 0.643933 0.692808 0.110 Uiso 0.696(10) 1 calc GR U P A 1
H5E H 0.173927 0.660433 0.600159 0.110 Uiso 0.696(10) 1 calc GR U P A 1
H5F H 0.236873 0.659553 0.713784 0.110 Uiso 0.696(10) 1 calc GR U P A 1
B6 B 0.3533(10) 0.5673(7) 0.6026(10) 0.080(4) Uani 0.696(10) 1 d D U P A 1
H6D H 0.422693 0.592289 0.636746 0.120 Uiso 0.696(10) 1 calc GR U P A 1
H6E H 0.344995 0.578253 0.530694 0.120 Uiso 0.696(10) 1 calc GR U P A 1
H6F H 0.382046 0.526283 0.608228 0.120 Uiso 0.696(10) 1 calc GR U P A 1
B7 B 0.7408(6) 0.4567(2) 0.7644(4) 0.0448(11) Uani 1 1 d . . . . .
H7D H 0.738186 0.499445 0.770187 0.067 Uiso 1 1 calc GR . . . .
H7E H 0.661461 0.443326 0.722529 0.067 Uiso 1 1 calc GR . . . .
H7F H 0.827301 0.444816 0.732552 0.067 Uiso 1 1 calc GR . . . .
B8 B 0.7318(6) 0.3595(2) 0.8725(4) 0.0537(13) Uani 1 1 d . . . . .
H8D H 0.653434 0.345777 0.830099 0.081 Uiso 1 1 calc GR . . . .
H8E H 0.722241 0.344922 0.941976 0.081 Uiso 1 1 calc GR . . . .
H8F H 0.818807 0.344993 0.844777 0.081 Uiso 1 1 calc GR . . . .
N3A N 0.2613(19) 0.5799(9) 0.6587(14) 0.059(5) Uani 0.304(10) 1 d D U P A 2
C6A C 0.157(2) 0.5450(10) 0.712(2) 0.073(6) Uani 0.304(10) 1 d D U P A 2
H6AA H 0.069298 0.545451 0.673634 0.109 Uiso 0.304(10) 1 calc GR U P A 2
H6AB H 0.143536 0.561697 0.780005 0.109 Uiso 0.304(10) 1 calc GR U P A 2
H6AC H 0.190300 0.504551 0.719422 0.109 Uiso 0.304(10) 1 calc GR U P A 2
B6A B 0.311(3) 0.5455(13) 0.5634(16) 0.073(7) Uani 0.304(10) 1 d D U P A 2
H6AD H 0.367955 0.512178 0.585420 0.110 Uiso 0.304(10) 1 calc GR U P A 2
H6AE H 0.365611 0.571524 0.520818 0.110 Uiso 0.304(10) 1 calc GR U P A 2
H6AF H 0.229731 0.531351 0.524258 0.110 Uiso 0.304(10) 1 calc GR U P A 2
B5A B 0.202(4) 0.6419(11) 0.635(3) 0.074(10) Uani 0.304(10) 1 d D U P A 2
H5AA H 0.137580 0.639684 0.576402 0.111 Uiso 0.304(10) 1 calc GR U P A 2
H5AB H 0.278641 0.668495 0.619265 0.111 Uiso 0.304(10) 1 calc GR U P A 2
H5AC H 0.153246 0.656637 0.694079 0.111 Uiso 0.304(10) 1 calc GR U P A 2
C5A C 0.381(2) 0.5893(9) 0.7314(18) 0.094(8) Uani 0.304(10) 1 d D U P A 2
H5AD H 0.350789 0.612899 0.788941 0.140 Uiso 0.304(10) 1 calc GR U P A 2
H5AE H 0.455643 0.609880 0.696659 0.140 Uiso 0.304(10) 1 calc GR U P A 2
H5AF H 0.415383 0.551412 0.756063 0.140 Uiso 0.304(10) 1 calc GR U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.476(6) . ?
N1 C2 1.477(6) . ?
N1 B1 1.579(6) . ?
N1 B2 1.578(6) . ?
N2 C3 1.466(6) . ?
N2 C4 1.466(6) . ?
N2 B3 1.584(6) . ?
N2 B4 1.582(6) . ?
N3 C5 1.495(10) . ?
N3 C6 1.466(8) . ?
N3 B5 1.547(10) . ?
N3 B6 1.569(10) . ?
N4 C7 1.469(6) . ?
N4 C8 1.482(6) . ?
N4 B7 1.578(6) . ?
N4 B8 1.576(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
B1 H1D 0.9800 . ?
B1 H1E 0.9800 . ?
B1 H1F 0.9800 . ?
B2 H2D 0.9800 . ?
B2 H2E 0.9800 . ?
B2 H2F 0.9800 . ?
B3 H3D 0.9800 . ?
B3 H3E 0.9800 . ?
B3 H3F 0.9800 . ?
B4 H4D 0.9800 . ?
B4 H4E 0.9800 . ?
B4 H4F 0.9800 . ?
B5 H5D 0.9800 . ?
B5 H5E 0.9800 . ?
B5 H5F 0.9800 . ?
B6 H6D 0.9800 . ?
B6 H6E 0.9800 . ?
B6 H6F 0.9800 . ?
B7 H7D 0.9800 . ?
B7 H7E 0.9800 . ?
B7 H7F 0.9800 . ?
B8 H8D 0.9800 . ?
B8 H8E 0.9800 . ?
B8 H8F 0.9800 . ?
N3A C6A 1.475(15) . ?
N3A B6A 1.565(15) . ?
N3A B5A 1.555(15) . ?
N3A C5A 1.496(15) . ?
C6A H6AA 0.9800 . ?
C6A H6AB 0.9800 . ?
C6A H6AC 0.9800 . ?
B6A H6AD 0.9800 . ?
B6A H6AE 0.9800 . ?
B6A H6AF 0.9800 . ?
B5A H5AA 0.9800 . ?
B5A H5AB 0.9800 . ?
B5A H5AC 0.9800 . ?
C5A H5AD 0.9800 . ?
C5A H5AE 0.9800 . ?
C5A H5AF 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C2 108.5(4) . . ?
C1 N1 B1 109.6(4) . . ?
C1 N1 B2 108.5(4) . . ?
C2 N1 B1 109.1(4) . . ?
C2 N1 B2 110.5(4) . . ?
B2 N1 B1 110.6(4) . . ?
C3 N2 C4 108.6(4) . . ?
C3 N2 B3 109.6(4) . . ?
C3 N2 B4 108.7(4) . . ?
C4 N2 B3 109.9(4) . . ?
C4 N2 B4 108.9(4) . . ?
B4 N2 B3 111.1(4) . . ?
C5 N3 B5 108.3(11) . . ?
C5 N3 B6 110.1(9) . . ?
C6 N3 C5 107.7(9) . . ?
C6 N3 B5 109.4(10) . . ?
C6 N3 B6 109.0(8) . . ?
B5 N3 B6 112.2(10) . . ?
C7 N4 C8 107.4(4) . . ?
C7 N4 B7 109.2(4) . . ?
C7 N4 B8 108.9(4) . . ?
C8 N4 B7 108.4(4) . . ?
C8 N4 B8 109.2(4) . . ?
B8 N4 B7 113.6(3) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
N3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N4 C8 H8A 109.5 . . ?
N4 C8 H8B 109.5 . . ?
N4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 B1 H1D 109.5 . . ?
N1 B1 H1E 109.5 . . ?
N1 B1 H1F 109.5 . . ?
H1D B1 H1E 109.5 . . ?
H1D B1 H1F 109.5 . . ?
H1E B1 H1F 109.5 . . ?
N1 B2 H2D 109.5 . . ?
N1 B2 H2E 109.5 . . ?
N1 B2 H2F 109.5 . . ?
H2D B2 H2E 109.5 . . ?
H2D B2 H2F 109.5 . . ?
H2E B2 H2F 109.5 . . ?
N2 B3 H3D 109.5 . . ?
N2 B3 H3E 109.5 . . ?
N2 B3 H3F 109.5 . . ?
H3D B3 H3E 109.5 . . ?
H3D B3 H3F 109.5 . . ?
H3E B3 H3F 109.5 . . ?
N2 B4 H4D 109.5 . . ?
N2 B4 H4E 109.5 . . ?
N2 B4 H4F 109.5 . . ?
H4D B4 H4E 109.5 . . ?
H4D B4 H4F 109.5 . . ?
H4E B4 H4F 109.5 . . ?
N3 B5 H5D 109.5 . . ?
N3 B5 H5E 109.5 . . ?
N3 B5 H5F 109.5 . . ?
H5D B5 H5E 109.5 . . ?
H5D B5 H5F 109.5 . . ?
H5E B5 H5F 109.5 . . ?
N3 B6 H6D 109.5 . . ?
N3 B6 H6E 109.5 . . ?
N3 B6 H6F 109.5 . . ?
H6D B6 H6E 109.5 . . ?
H6D B6 H6F 109.5 . . ?
H6E B6 H6F 109.5 . . ?
N4 B7 H7D 109.5 . . ?
N4 B7 H7E 109.5 . . ?
N4 B7 H7F 109.5 . . ?
H7D B7 H7E 109.5 . . ?
H7D B7 H7F 109.5 . . ?
H7E B7 H7F 109.5 . . ?
N4 B8 H8D 109.5 . . ?
N4 B8 H8E 109.5 . . ?
N4 B8 H8F 109.5 . . ?
H8D B8 H8E 109.5 . . ?
H8D B8 H8F 109.5 . . ?
H8E B8 H8F 109.5 . . ?
C6A N3A B6A 110(2) . . ?
C6A N3A B5A 110(2) . . ?
C6A N3A C5A 107(2) . . ?
B5A N3A B6A 114(2) . . ?
C5A N3A B6A 110(2) . . ?
C5A N3A B5A 105.7(19) . . ?
N3A C6A H6AA 109.5 . . ?
N3A C6A H6AB 109.5 . . ?
N3A C6A H6AC 109.5 . . ?
H6AA C6A H6AB 109.5 . . ?
H6AA C6A H6AC 109.5 . . ?
H6AB C6A H6AC 109.5 . . ?
N3A B6A H6AD 109.5 . . ?
N3A B6A H6AE 109.5 . . ?
N3A B6A H6AF 109.5 . . ?
H6AD B6A H6AE 109.5 . . ?
H6AD B6A H6AF 109.5 . . ?
H6AE B6A H6AF 109.5 . . ?
N3A B5A H5AA 109.5 . . ?
N3A B5A H5AB 109.5 . . ?
N3A B5A H5AC 109.5 . . ?
H5AA B5A H5AB 109.5 . . ?
H5AA B5A H5AC 109.5 . . ?
H5AB B5A H5AC 109.5 . . ?
N3A C5A H5AD 109.5 . . ?
N3A C5A H5AE 109.5 . . ?
N3A C5A H5AF 109.5 . . ?
H5AD C5A H5AE 109.5 . . ?
H5AD C5A H5AF 109.5 . . ?
H5AE C5A H5AF 109.5 . . ?

_olex2_exptl_crystal_mounting_method "'in fomblin film on a micromount"
# This is the default assumed mounting details'
_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 2.575
_oxdiff_exptl_absorpt_empirical_full_min 0.434


#=== END
####################################################################### 
# 
# 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_krnalg
_database_code_depnum_ccdc_archive 'CCDC 1581981'
_audit_update_record             
;
2017-10-25 deposited with the CCDC.
2018-01-04 downloaded from the CCDC.
;
_nottingham_internal_coll_name   KRNALG
_nottingham_internal_coll_number 16090
_nottingham_internal_coll_client RN/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'ofand \w scans'
_nottingham_internal_coll_frame_time 'degrees,, 10.00, 40.00'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_user   pcxrn3
_nottingham_internal_coll_date   12/05/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'SN, XDA 017/09'
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 13/05/2016
_nottingham_internal_process_user pcxrn3
_nottingham_internal_solution_date 13/05/2016
_nottingham_internal_solution_user pcxrn3
_nottingham_internal_refinement_date 07/09/2017
_nottingham_internal_refinement_user pcxrn3
_nottingham_internal_self_archive_date 07/09/2017
_nottingham_internal_self_validation_date 07/09/2017
_nottingham_internal_self_validation_user pcxrn3
_nottingham_internal_validation_date ?
_nottingham_internal_validation_user ?
_nottingham_internal_archive_date ?
_refine_special_details          ?
_vrf_PLAT084_krnalg              
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.39 Report
RESPONSE: This is reflective of the overall low quality of the diffraction data.
;
_vrf_PLAT340_krnalg              
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01507 Ang.  
RESPONSE: This is reflective of the overall low quality of the diffraction data.
;
_audit_creation_date             2017-09-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C84 H76 K2 N6'
_chemical_formula_sum            'C84 H76 K2 N6'
_chemical_formula_weight         1247.70
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C42 H38 K N3'
_chemical_oxdiff_usercomment     
'KRNALG #16090 SN-958 IN FOMBLIN FILM ON A MICROMOUNT FOR RN/DLK'
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'
K K 0.3868 1.0657 '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'

_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                   11.670(3)
_cell_length_b                   11.773(2)
_cell_length_c                   12.928(4)
_cell_angle_alpha                80.79(2)
_cell_angle_beta                 85.14(2)
_cell_angle_gamma                78.098(18)
_cell_volume                     1713.1(8)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1241
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.1180
_cell_measurement_theta_min      4.8520
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.602
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             660
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -8 -2 0.0469
-4 -7 0 0.0790
7 -1 0 0.2006
-7 0 0 0.2035
0 7 2 0.0430
1 -7 -2 0.0615
0 -1 8 0.0284
0 1 -8 0.0258

_exptl_crystal_size_max          0.432
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.054
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
-0.9855 -8.0086 -2.0150 0.0728 0.3948 -0.9751
-3.9892 -7.0064 -0.0020 0.1828 -0.1080 -0.9710
7.0153 -1.0070 -0.0377 0.2291 0.9424 0.1663
-7.0128 0.0056 0.0346 -0.1877 -0.8855 -0.2820
-0.0137 7.0080 2.0169 -0.0582 -0.4644 0.8192
1.0155 -7.0088 -2.0218 0.0850 0.5909 -0.7789
0.0203 -1.0076 7.9773 0.9688 -0.2088 -0.0783
-0.0203 1.0076 -7.9773 -0.9688 0.2088 0.0783

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1123
_diffrn_reflns_av_unetI/netI     0.1518
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10407
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        66.591
_diffrn_reflns_theta_max         66.591
_diffrn_reflns_theta_min         3.877
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        
'flash frozen in gaseous N2' # assumed default, please check
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -93.00 -55.00   1.00   10.00    --  -38.50 125.00   0.00   38
  2  ω    -49.00 -10.00   1.00   10.00    --  -38.50  38.00 150.00   39
  3  ω   -103.00 -24.00   1.00   10.00    --  -38.50 -38.00   0.00   79
  4  ω   -109.00 -15.00   1.00   10.00    --  -38.50 -57.00 150.00   94
  5  ω    -64.00  32.00   1.00   10.00    --  -38.50  57.00 -60.00   96
  6  ω     39.00  67.00   1.00   10.00    --   42.13-125.00   0.00   28
  7  ω     48.00  97.00   1.00   40.00    --  108.63 -45.00 150.00   49
  8  ω     47.00 109.00   1.00   40.00    --  108.63 -95.00   0.00   62
  9  ω     35.00 110.00   1.00   40.00    --  108.63 -95.00  90.00   75
 10  ω     50.00  84.00   1.00   40.00    --  108.63 -30.00  30.00   34
 11  ω     38.00  97.00   1.00   40.00    --  108.63-140.00 -44.00   59
 12  ω     92.00 178.00   1.00   40.00    --  108.63  30.00 -60.00   86
 13  ω     28.00 110.00   1.00   40.00    --  108.63 -95.00-180.00   82
 14  ω     93.00 122.00   1.00   40.00    --  108.63-125.00 -60.00   29
 15  ω     42.00  91.00   1.00   40.00    --  108.63 -30.00 -30.00   49
 16  ω     63.00  92.00   1.00   40.00    --  108.63 -45.00  60.00   29
 17  ω     41.00  88.00   1.00   40.00    --  108.63 -45.00 -30.00   47
 18  ω     49.00  82.00   1.00   40.00    --  108.63 -30.00-120.00   33
 19  ω     50.00  91.00   1.00   40.00    --  108.63 -30.00 -90.00   41
 20  ω     33.00  91.00   1.00   40.00    --  108.63 -95.00 -60.00   58
 21  ω     64.00 178.00   1.00   40.00    --  108.63  15.00-120.00  114
;
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova-Duo, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 
'MiTeGen micromount' # assumed default, please check
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0272983000
_diffrn_orient_matrix_UB_12      -0.0416700000
_diffrn_orient_matrix_UB_13      0.1161111000
_diffrn_orient_matrix_UB_21      0.1260654000
_diffrn_orient_matrix_UB_22      -0.0563510000
_diffrn_orient_matrix_UB_23      -0.0336179000
_diffrn_orient_matrix_UB_31      0.0403263000
_diffrn_orient_matrix_UB_32      0.1156202000
_diffrn_orient_matrix_UB_33      0.0046813000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2745
_reflns_number_total             5952
_reflns_odcompleteness_completeness 98.20
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         5952
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2312
_refine_ls_R_factor_gt           0.1335
_refine_ls_restrained_S_all      1.042
_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)+(0.1246P)²+9.4346P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3116
_refine_ls_wR_factor_ref         0.3859
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C11(H11), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18),
 C19(H19), C20(H20), C24(H24), C26(H26), C32(H32), C34(H34), C35(H35), C36(H36),
  C38(H38), C39(H39), C40(H40), C41(H41)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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 0.86139(18) 0.64850(17) 0.60349(18) 0.0515(6) Uani 1 1 d . . . . .
N1 N 0.9566(6) 0.6664(6) 0.4069(6) 0.0467(18) Uani 1 1 d . . . . .
N2 N 0.6970(6) 0.7719(6) 0.4662(7) 0.0475(19) Uani 1 1 d . . . . .
N3 N 1.0908(7) 0.6754(6) 0.6053(7) 0.053(2) Uani 1 1 d . . . . .
C1 C 0.9000(8) 0.6832(6) 0.3139(8) 0.042(2) Uani 1 1 d . . . . .
C2 C 0.7794(7) 0.7268(7) 0.2929(8) 0.044(2) Uani 1 1 d . . . . .
C3 C 0.7489(9) 0.7431(8) 0.1871(8) 0.053(2) Uani 1 1 d . . . . .
H3 H 0.668656 0.772548 0.173387 0.064 Uiso 1 1 calc R . . . .
C4 C 0.8245(8) 0.7201(7) 0.1027(8) 0.045(2) Uani 1 1 d . . . . .
C5 C 0.9436(8) 0.6738(7) 0.1249(8) 0.049(2) Uani 1 1 d . . . . .
H5 H 0.999968 0.655873 0.069466 0.059 Uiso 1 1 calc R . . . .
C6 C 0.9771(8) 0.6551(7) 0.2252(8) 0.046(2) Uani 1 1 d . . . . .
C7 C 0.7903(9) 0.7585(8) -0.0122(8) 0.052(2) Uani 1 1 d . . . . .
C8 C 0.8529(9) 0.6728(9) -0.0860(9) 0.061(3) Uani 1 1 d . . . . .
H8A H 0.837407 0.594267 -0.059987 0.092 Uiso 1 1 calc GR . . . .
H8B H 0.937552 0.670498 -0.088601 0.092 Uiso 1 1 calc GR . . . .
H8C H 0.823948 0.698897 -0.156525 0.092 Uiso 1 1 calc GR . . . .
C9 C 0.8227(10) 0.8795(9) -0.0487(9) 0.065(3) Uani 1 1 d . . . . .
H9A H 0.903781 0.876469 -0.032010 0.097 Uiso 1 1 calc GR . . . .
H9B H 0.769841 0.938510 -0.012541 0.097 Uiso 1 1 calc GR . . . .
H9C H 0.815258 0.900354 -0.124595 0.097 Uiso 1 1 calc GR . . . .
C10 C 0.6564(9) 0.7736(10) -0.0220(9) 0.063(3) Uani 1 1 d . . . . .
H10A H 0.614484 0.827795 0.024991 0.095 Uiso 1 1 calc GR . . . .
H10B H 0.633180 0.697287 -0.002708 0.095 Uiso 1 1 calc GR . . . .
H10C H 0.636802 0.805353 -0.094576 0.095 Uiso 1 1 calc GR . . . .
C11 C 0.6870(8) 0.7686(7) 0.3681(8) 0.046(2) Uani 1 1 d . . . . .
H11 H 0.610911 0.796541 0.342357 0.056 Uiso 1 1 calc R . . . .
C12 C 0.5937(9) 0.8172(8) 0.5244(8) 0.053(2) Uani 1 1 d . . . . .
C13 C 0.4865(9) 0.7865(9) 0.5165(9) 0.062(3) Uani 1 1 d . . . . .
H13 H 0.478960 0.737438 0.466866 0.074 Uiso 1 1 calc R . . . .
C14 C 0.3893(10) 0.8276(9) 0.5814(10) 0.074(3) Uani 1 1 d . . . . .
H14 H 0.315738 0.808800 0.572540 0.088 Uiso 1 1 calc R . . . .
C15 C 0.3977(10) 0.8939(9) 0.6570(10) 0.072(3) Uani 1 1 d . . . . .
H15 H 0.331338 0.917475 0.702032 0.086 Uiso 1 1 calc R . . . .
C16 C 0.5033(11) 0.9268(9) 0.6679(9) 0.064(3) Uani 1 1 d . . . . .
C17 C 0.5171(13) 0.9979(11) 0.7425(10) 0.081(4) Uani 1 1 d . . . . .
H17 H 0.452714 1.021525 0.789467 0.097 Uiso 1 1 calc R . . . .
C18 C 0.6194(14) 1.0335(11) 0.7492(11) 0.088(4) Uani 1 1 d . . . . .
H18 H 0.625714 1.078150 0.802762 0.106 Uiso 1 1 calc R . . . .
C19 C 0.7186(11) 1.0055(9) 0.6772(10) 0.074(3) Uani 1 1 d . . . . .
H19 H 0.787998 1.035437 0.678539 0.088 Uiso 1 1 calc R . . . .
C20 C 0.7079(10) 0.9325(8) 0.6057(9) 0.064(3) Uani 1 1 d . . . . .
H20 H 0.773229 0.909219 0.559449 0.076 Uiso 1 1 calc R . . . .
C21 C 0.6034(9) 0.8915(7) 0.5992(8) 0.052(2) Uani 1 1 d . . . . .
C22 C 1.0717(7) 0.6283(7) 0.3772(8) 0.043(2) Uani 1 1 d . . . . .
C23 C 1.0926(7) 0.6180(7) 0.2698(8) 0.044(2) Uani 1 1 d . . . . .
C24 C 1.2036(8) 0.5815(7) 0.2236(8) 0.050(2) Uani 1 1 d . . . . .
H24 H 1.212767 0.573810 0.151146 0.060 Uiso 1 1 calc R . . . .
C25 C 1.3025(8) 0.5559(7) 0.2854(9) 0.050(2) Uani 1 1 d . . . . .
C26 C 1.2829(8) 0.5661(7) 0.3912(8) 0.051(2) Uani 1 1 d . . . . .
H26 H 1.348614 0.544784 0.433863 0.061 Uiso 1 1 calc R . . . .
C27 C 1.1714(7) 0.6063(7) 0.4402(9) 0.050(2) Uani 1 1 d . . . . .
C28 C 1.4248(8) 0.5180(8) 0.2355(9) 0.054(3) Uani 1 1 d . . . . .
C29 C 1.5219(10) 0.5138(13) 0.3101(12) 0.095(5) Uani 1 1 d . . . . .
H29A H 1.516107 0.591697 0.330180 0.142 Uiso 1 1 calc GR . . . .
H29B H 1.598691 0.489887 0.274709 0.142 Uiso 1 1 calc GR . . . .
H29C H 1.512661 0.457116 0.373108 0.142 Uiso 1 1 calc GR . . . .
C30 C 1.4377(10) 0.3955(9) 0.2069(12) 0.082(4) Uani 1 1 d . . . . .
H30A H 1.424422 0.340680 0.270182 0.123 Uiso 1 1 calc GR . . . .
H30B H 1.516906 0.370745 0.176299 0.123 Uiso 1 1 calc GR . . . .
H30C H 1.379990 0.396204 0.155871 0.123 Uiso 1 1 calc GR . . . .
C31 C 1.4462(11) 0.6005(12) 0.1357(12) 0.099(5) Uani 1 1 d . . . . .
H31A H 1.384864 0.604732 0.087104 0.148 Uiso 1 1 calc GR . . . .
H31B H 1.522974 0.570997 0.102658 0.148 Uiso 1 1 calc GR . . . .
H31C H 1.444439 0.678922 0.153001 0.148 Uiso 1 1 calc GR . . . .
C32 C 1.1747(8) 0.6222(7) 0.5485(8) 0.046(2) Uani 1 1 d . . . . .
H32 H 1.246438 0.589940 0.581276 0.056 Uiso 1 1 calc R . . . .
C33 C 1.1210(8) 0.6851(8) 0.7070(8) 0.047(2) Uani 1 1 d . . . . .
C34 C 1.1682(8) 0.5925(8) 0.7772(8) 0.055(2) Uani 1 1 d . . . . .
H34 H 1.180936 0.516259 0.757755 0.066 Uiso 1 1 calc R . . . .
C35 C 1.1998(9) 0.6039(10) 0.8791(10) 0.067(3) Uani 1 1 d . . . . .
H35 H 1.230630 0.536836 0.927198 0.080 Uiso 1 1 calc R . . . .
C36 C 1.1839(9) 0.7164(9) 0.9053(9) 0.062(3) Uani 1 1 d . . . . .
H36 H 1.205378 0.727067 0.971859 0.075 Uiso 1 1 calc R . . . .
C37 C 1.1361(9) 0.8144(8) 0.8338(9) 0.058(3) Uani 1 1 d . . . . .
C38 C 1.1206(10) 0.9301(9) 0.8603(10) 0.069(3) Uani 1 1 d . . . . .
H38 H 1.140328 0.940581 0.927441 0.083 Uiso 1 1 calc R . . . .
C39 C 1.0780(11) 1.0250(9) 0.7902(11) 0.076(4) Uani 1 1 d . . . . .
H39 H 1.068377 1.100870 0.809900 0.091 Uiso 1 1 calc R . . . .
C40 C 1.0476(10) 1.0152(9) 0.6897(11) 0.068(3) Uani 1 1 d . . . . .
H40 H 1.019688 1.083359 0.641712 0.082 Uiso 1 1 calc R . . . .
C41 C 1.0592(8) 0.9046(8) 0.6618(9) 0.057(3) Uani 1 1 d . . . . .
H41 H 1.036878 0.896449 0.594813 0.069 Uiso 1 1 calc R . . . .
C42 C 1.1042(8) 0.8029(8) 0.7329(8) 0.049(2) 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
K1 N1 2.680(8) . ?
K1 N2 2.747(8) . ?
K1 N3 2.762(9) . ?
K1 C12 3.475(10) . ?
K1 C20 3.455(9) . ?
K1 C22 3.164(8) 2_766 ?
K1 C23 3.259(9) 2_766 ?
K1 C24 3.395(10) 2_766 ?
K1 C25 3.441(9) 2_766 ?
K1 C26 3.302(9) 2_766 ?
K1 C27 3.243(9) 2_766 ?
N1 C1 1.387(12) . ?
N1 C22 1.368(11) . ?
N2 C11 1.290(12) . ?
N2 C12 1.419(11) . ?
N3 C32 1.290(11) . ?
N3 C33 1.418(13) . ?
C1 C2 1.429(12) . ?
C1 C6 1.434(12) . ?
C2 C3 1.417(14) . ?
C2 C11 1.451(12) . ?
C3 C4 1.369(14) . ?
C4 C5 1.421(13) . ?
C4 C7 1.543(14) . ?
C5 C6 1.357(13) . ?
C6 C23 1.466(13) . ?
C7 C8 1.532(13) . ?
C7 C9 1.540(13) . ?
C7 C10 1.549(14) . ?
C12 C13 1.388(14) . ?
C12 C21 1.429(13) . ?
C13 C14 1.402(14) . ?
C14 C15 1.365(17) . ?
C15 C16 1.391(16) . ?
C16 C17 1.412(16) . ?
C16 C21 1.438(14) . ?
C17 C18 1.358(19) . ?
C18 C19 1.440(19) . ?
C19 C20 1.387(14) . ?
C20 C21 1.415(15) . ?
C22 C23 1.410(13) . ?
C22 C27 1.433(13) . ?
C23 C24 1.393(12) . ?
C24 C25 1.413(13) . ?
C25 C26 1.387(14) . ?
C25 C28 1.526(12) . ?
C26 C27 1.421(12) . ?
C27 C32 1.446(14) . ?
C28 C29 1.537(16) . ?
C28 C30 1.520(13) . ?
C28 C31 1.522(16) . ?
C33 C34 1.354(14) . ?
C33 C42 1.448(12) . ?
C34 C35 1.432(16) . ?
C35 C36 1.391(15) . ?
C36 C37 1.406(15) . ?
C37 C38 1.429(13) . ?
C37 C42 1.420(15) . ?
C38 C39 1.356(17) . ?
C39 C40 1.403(17) . ?
C40 C41 1.384(13) . ?
C41 C42 1.423(14) . ?

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
N1 K1 N2 69.9(2) . . ?
N1 K1 N3 70.5(2) . . ?
N1 K1 C12 92.5(2) . . ?
N1 K1 C20 100.2(3) . . ?
N1 K1 C22 89.8(2) . 2_766 ?
N1 K1 C23 114.0(2) . 2_766 ?
N1 K1 C24 132.9(2) . 2_766 ?
N1 K1 C25 125.4(2) . 2_766 ?
N1 K1 C26 101.9(2) . 2_766 ?
N1 K1 C27 84.0(2) . 2_766 ?
N2 K1 N3 126.7(3) . . ?
N2 K1 C12 22.7(2) . . ?
N2 K1 C20 53.0(2) . . ?
N2 K1 C22 119.9(2) . 2_766 ?
N2 K1 C23 133.6(2) . 2_766 ?
N2 K1 C24 119.3(2) . 2_766 ?
N2 K1 C25 95.6(2) . 2_766 ?
N2 K1 C26 84.3(2) . 2_766 ?
N2 K1 C27 94.4(2) . 2_766 ?
N3 K1 C12 138.1(2) . . ?
N3 K1 C20 102.0(3) . . ?
N3 K1 C22 94.1(2) . 2_766 ?
N3 K1 C23 94.9(2) . 2_766 ?
N3 K1 C24 113.7(2) . 2_766 ?
N3 K1 C25 136.7(2) . 2_766 ?
N3 K1 C26 138.3(2) . 2_766 ?
N3 K1 C27 115.4(2) . 2_766 ?
C20 K1 C12 42.0(2) . . ?
C22 K1 C12 124.8(2) 2_766 . ?
C22 K1 C20 163.1(3) 2_766 . ?
C22 K1 C23 25.3(2) 2_766 2_766 ?
C22 K1 C24 44.1(2) 2_766 2_766 ?
C22 K1 C25 51.3(2) 2_766 2_766 ?
C22 K1 C26 44.2(2) 2_766 2_766 ?
C22 K1 C27 25.8(2) 2_766 2_766 ?
C23 K1 C12 126.8(2) 2_766 . ?
C23 K1 C20 145.3(3) 2_766 . ?
C23 K1 C24 24.1(2) 2_766 2_766 ?
C23 K1 C25 42.3(2) 2_766 2_766 ?
C23 K1 C26 49.3(2) 2_766 2_766 ?
C24 K1 C12 105.9(2) 2_766 . ?
C24 K1 C20 122.5(3) 2_766 . ?
C24 K1 C25 23.9(2) 2_766 2_766 ?
C25 K1 C12 84.6(2) 2_766 . ?
C25 K1 C20 112.1(3) 2_766 . ?
C26 K1 C12 81.6(2) 2_766 . ?
C26 K1 C20 119.7(3) 2_766 . ?
C26 K1 C24 41.9(3) 2_766 2_766 ?
C26 K1 C25 23.6(2) 2_766 2_766 ?
C27 K1 C12 99.8(2) 2_766 . ?
C27 K1 C20 141.3(3) 2_766 . ?
C27 K1 C23 43.9(2) 2_766 2_766 ?
C27 K1 C24 50.7(2) 2_766 2_766 ?
C27 K1 C25 43.5(2) 2_766 2_766 ?
C27 K1 C26 25.1(2) 2_766 2_766 ?
C1 N1 K1 128.0(6) . . ?
C22 N1 K1 126.3(6) . . ?
C22 N1 C1 103.4(8) . . ?
C11 N2 K1 131.3(5) . . ?
C11 N2 C12 116.9(8) . . ?
C12 N2 K1 108.9(6) . . ?
C32 N3 K1 122.6(6) . . ?
C32 N3 C33 115.0(8) . . ?
C33 N3 K1 111.9(6) . . ?
N1 C1 C2 130.2(8) . . ?
N1 C1 C6 113.8(8) . . ?
C2 C1 C6 116.0(9) . . ?
C1 C2 C11 125.9(9) . . ?
C3 C2 C1 117.3(8) . . ?
C3 C2 C11 116.4(8) . . ?
C4 C3 C2 126.0(9) . . ?
C3 C4 C5 116.2(9) . . ?
C3 C4 C7 123.4(8) . . ?
C5 C4 C7 119.8(8) . . ?
C6 C5 C4 120.2(9) . . ?
C1 C6 C23 103.3(8) . . ?
C5 C6 C1 124.3(9) . . ?
C5 C6 C23 132.0(9) . . ?
C4 C7 C10 111.6(8) . . ?
C8 C7 C4 113.2(8) . . ?
C8 C7 C9 109.2(9) . . ?
C8 C7 C10 108.1(8) . . ?
C9 C7 C4 107.3(8) . . ?
C9 C7 C10 107.3(9) . . ?
N2 C11 C2 127.1(8) . . ?
N2 C12 K1 48.4(5) . . ?
N2 C12 C21 117.9(9) . . ?
C13 C12 K1 131.2(7) . . ?
C13 C12 N2 122.9(9) . . ?
C13 C12 C21 119.1(9) . . ?
C21 C12 K1 87.5(6) . . ?
C12 C13 C14 120.3(11) . . ?
C15 C14 C13 121.7(12) . . ?
C14 C15 C16 120.0(10) . . ?
C15 C16 C17 122.9(11) . . ?
C15 C16 C21 119.9(10) . . ?
C17 C16 C21 117.2(12) . . ?
C18 C17 C16 122.2(12) . . ?
C17 C18 C19 121.7(12) . . ?
C20 C19 C18 116.7(12) . . ?
C19 C20 K1 125.8(7) . . ?
C19 C20 C21 122.4(11) . . ?
C21 C20 K1 88.4(5) . . ?
C12 C21 C16 118.9(10) . . ?
C20 C21 C12 121.6(9) . . ?
C20 C21 C16 119.5(9) . . ?
N1 C22 K1 112.1(5) . 2_766 ?
N1 C22 C23 114.6(8) . . ?
N1 C22 C27 127.7(9) . . ?
C23 C22 K1 81.1(5) . 2_766 ?
C23 C22 C27 117.6(8) . . ?
C27 C22 K1 80.2(5) . 2_766 ?
C6 C23 K1 113.8(5) . 2_766 ?
C22 C23 K1 73.6(5) . 2_766 ?
C22 C23 C6 105.0(7) . . ?
C24 C23 K1 83.4(5) . 2_766 ?
C24 C23 C6 131.4(9) . . ?
C24 C23 C22 123.6(9) . . ?
C23 C24 K1 72.5(5) . 2_766 ?
C23 C24 C25 119.4(9) . . ?
C25 C24 K1 79.9(6) . 2_766 ?
C24 C25 K1 76.3(5) . 2_766 ?
C24 C25 C28 120.0(9) . . ?
C26 C25 K1 72.6(5) . 2_766 ?
C26 C25 C24 117.5(8) . . ?
C26 C25 C28 122.5(9) . . ?
C28 C25 K1 120.8(5) . 2_766 ?
C25 C26 K1 83.8(5) . 2_766 ?
C25 C26 C27 124.5(9) . . ?
C27 C26 K1 75.1(5) . 2_766 ?
C22 C27 K1 74.0(5) . 2_766 ?
C22 C27 C32 128.3(8) . . ?
C26 C27 K1 79.8(5) . 2_766 ?
C26 C27 C22 117.2(9) . . ?
C26 C27 C32 114.5(9) . . ?
C32 C27 K1 117.2(6) . 2_766 ?
C25 C28 C29 112.3(9) . . ?
C30 C28 C25 109.7(8) . . ?
C30 C28 C29 107.3(9) . . ?
C30 C28 C31 108.0(11) . . ?
C31 C28 C25 111.2(8) . . ?
C31 C28 C29 108.2(11) . . ?
N3 C32 C27 127.1(9) . . ?
N3 C33 C42 116.4(8) . . ?
C34 C33 N3 123.9(8) . . ?
C34 C33 C42 119.7(9) . . ?
C33 C34 C35 123.3(9) . . ?
C36 C35 C34 117.7(11) . . ?
C35 C36 C37 120.3(11) . . ?
C36 C37 C38 120.4(11) . . ?
C36 C37 C42 121.8(8) . . ?
C42 C37 C38 117.8(10) . . ?
C39 C38 C37 120.5(12) . . ?
C38 C39 C40 122.4(10) . . ?
C41 C40 C39 118.8(11) . . ?
C40 C41 C42 120.4(11) . . ?
C37 C42 C33 117.1(9) . . ?
C37 C42 C41 120.0(8) . . ?
C41 C42 C33 122.8(9) . . ?

_olex2_exptl_crystal_mounting_method "'in fomblin film on a micromount"
# This is the default assumed mounting details'
_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 2.858
_oxdiff_exptl_absorpt_empirical_full_min 0.411
####################################################################### 
# 
# 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_lirnlj
_database_code_depnum_ccdc_archive 'CCDC 1581979'
_audit_update_record             
;
2017-10-25 deposited with the CCDC.
2018-01-04 downloaded from the CCDC.
;
_nottingham_internal_coll_name   LIRNLJ
_nottingham_internal_coll_number 15977
_nottingham_internal_coll_client RNL/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'ofand \w scans'
_nottingham_internal_coll_frame_time 'degrees,, 5.00, 20.00'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_user   pcxrn3
_nottingham_internal_coll_date   19/04/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 20/04/2016
_nottingham_internal_process_user pcxrn3
_nottingham_internal_solution_date 17/06/16
_nottingham_internal_solution_user pcxrn3
_nottingham_internal_refinement_date 17/06/16
_nottingham_internal_refinement_user pcxrn3
_nottingham_internal_self_archive_date 21/09/2017
_nottingham_internal_self_validation_date 21/09/2017
_nottingham_internal_self_validation_user pcxrn3
_nottingham_internal_validation_date 20/10/2017
_nottingham_internal_validation_user pczwl
_nottingham_internal_archive_date 20/10/2017
_refine_special_details          
;
The unsubstituted flanking arm (starting from C26) and also atoms C9A and C10A, are disordered over two positions. 
The occupancies of the two components were refined competitively, converging at a ratio of 0.87:0.13. 
Chemically equivalent bond lengths and angles of the disordered atoms were restrained to be approximately equal. 
Enhanced rigid bond and similarity restraints were applied to the thermal parameters of the minor component atoms. 
Atom C9A could not be sensibly refined anisotropically, and so was refined isotropically.
;
_audit_creation_date             2017-10-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C50 H55 Li N3 O'
_chemical_formula_sum            'C50 H55 Li N3 O'
_chemical_formula_weight         720.91
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C50 H55 N3 Li O'
_chemical_oxdiff_usercomment     
'LIRNLJ #15977 GVB-992 IN FOMBLIN FILM ON MICROMOUNT FOR RN/DLK'
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'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.65773(16)
_cell_length_b                   21.7068(3)
_cell_length_c                   14.23975(17)
_cell_angle_alpha                90
_cell_angle_beta                 105.0737(12)
_cell_angle_gamma                90
_cell_volume                     4076.34(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    17705
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.3710
_cell_measurement_theta_min      3.7960
_shelx_estimated_absorpt_T_max   0.939
_shelx_estimated_absorpt_T_min   0.894
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1768.000
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 -11 3 0.0607
9 -3 -3 0.0709
-3 12 -3 0.0561
-6 -8 6 0.0762
5 -8 3 0.0673
-4 -9 6 0.0772
-2 10 -6 0.0710
-8 5 -1 0.0754
9 1 -3 0.0777
6 0 4 0.0606
-5 1 -5 0.0809
2 11 5 0.0853
-2 3 9 0.0920
2 -5 -9 0.0750
-2 -11 -5 0.0741
0 -14 0 0.0529

_exptl_crystal_size_max          0.219
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.121
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
3.9943 -11.0029 3.0007 0.1474 0.8757 0.4842
8.9949 -2.9821 -2.9991 0.1439 0.9147 -0.4702
-2.9942 12.0058 -3.0010 -0.2215 -0.8034 -0.5735
-6.0003 -8.0228 5.9999 0.0311 -0.1428 1.0001
4.9951 -7.9984 3.0001 -0.0198 0.8851 0.3079
-4.0015 -9.0196 5.9999 0.0223 0.0963 0.9521
-1.9958 10.0081 -5.9997 0.0973 -0.7507 -0.7210
-7.9949 4.9884 -1.0000 0.0734 -1.0260 0.0857
8.9966 1.0212 -2.9998 -0.0421 0.7887 -0.6442
5.9981 0.0096 3.9982 -0.5040 0.7749 -0.0229
-4.9982 0.9939 -4.9981 0.5143 -0.7406 -0.1293
2.0043 11.0099 4.9961 -0.9893 0.0513 -0.2554
-1.9970 2.9925 8.9966 -0.8446 0.0401 0.5274
1.9962 -4.9942 -8.9962 0.9376 0.0229 -0.4404
-2.0043 -11.0099 -4.9961 0.9893 -0.0513 0.2554
-0.0057 -14.0116 0.0026 0.6510 0.4409 0.6090

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            46635
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.839
_diffrn_reflns_theta_min         3.805
_diffrn_ambient_environment      ?
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'Agilent Diffraction Atlas S2 detector'
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9874
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00  34.00   1.00    5.00    --  -38.50  38.00  30.00   84
  2  ω   -111.00 -16.00   1.00    5.00    --  -38.50 -38.00 -60.00   95
  3  ω      2.00  98.00   1.00    5.00    --   42.83-125.00   0.00   96
  4  ω     20.00 115.00   1.00    5.00    --   42.83  38.00-150.00   95
  5  ω     24.00 150.00   1.00   20.00    --  104.50 -15.00  60.00  126
  6  ω     30.00  91.00   1.00   20.00    --  104.50 -30.00 -30.00   61
  7  ω     81.00 178.00   1.00   20.00    --  104.50  30.00  60.00   97
  8  ω     30.00  91.00   1.00   20.00    --  104.50 -30.00-150.00   61
  9  ω     33.00  98.00   1.00   20.00    --  104.50 -45.00-180.00   65
 10  ω     33.00  98.00   1.00   20.00    --  104.50 -45.00  90.00   65
 11  ω     30.00  91.00   1.00   20.00    --  104.50 -30.00 -90.00   61
 12  ω     23.00 109.00   1.00   20.00    --  104.50 -94.00-150.00   86
 13  ω      2.00  98.00   1.00    5.00    --   42.83-125.00 150.00   96
 14  ω     20.00 115.00   1.00    5.00    --   42.83  38.00 -60.00   95
 15  ω     16.00 113.00   1.00    5.00    --   42.83  57.00  90.00   97
 16  ω     23.00 109.00   1.00   20.00    --  104.50 -94.00   0.00   86
 17  ω     59.00 178.00   1.00   20.00    --  104.50  15.00-180.00  119
 18  ω     77.00 175.00   1.00   20.00    --  104.50  61.00 -60.00   98
 19  ω     80.00 105.00   1.00   20.00    --  104.50  45.00   0.00   25
 20  ω     23.00 109.00   1.00   20.00    --  104.50 -94.00  90.00   86
 21  ω     77.00 175.00   1.00   20.00    --  104.50  61.00-120.00   98
;
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Atlas'
_diffrn_measurement_method       ?
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0275936000
_diffrn_orient_matrix_UB_12      -0.0464671000
_diffrn_orient_matrix_UB_13      -0.0845461000
_diffrn_orient_matrix_UB_21      0.1039158000
_diffrn_orient_matrix_UB_22      -0.0315030000
_diffrn_orient_matrix_UB_23      0.0380034000
_diffrn_orient_matrix_UB_31      -0.0456925000
_diffrn_orient_matrix_UB_32      -0.0434323000
_diffrn_orient_matrix_UB_33      0.0629216000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6967
_reflns_number_total             8151
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.038
_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     625
_refine_ls_number_reflns         8151
_refine_ls_number_restraints     202
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0479
_refine_ls_restrained_S_all      1.012
_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)+(0.0625P)²+1.8272P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1304
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C11-C10 \\sim C11-C10A
 with sigma of 0.02
 C9A-C10A \\sim C9-C10
 with sigma of 0.02
 C9-C8 \\sim C9A-C8
 with sigma of 0.02
 C26A-C10A \\sim C26-C10
 with sigma of 0.02
 N3A-C26A \\sim N3-C26
 with sigma of 0.02
 N3A-C27A \\sim N3-C27
 with sigma of 0.02
 C36-C27 \\sim C36A-C27A
 with sigma of 0.02
 C36-C35 \\sim C36A-C35A
 with sigma of 0.02
 C35-C34 \\sim C35A-C34A
 with sigma of 0.02
 C34-C33 \\sim C34A-C33A
 with sigma of 0.02
 C33A-C32A \\sim C33-C32
 with sigma of 0.02
 C32A-C31A \\sim C32-C31
 with sigma of 0.02
 C31A-C30A \\sim C31-C30
 with sigma of 0.02
 C30-C29 \\sim C30A-C29A
 with sigma of 0.02
 C29A-C28A \\sim C29-C28
 with sigma of 0.02
 C28A-C27A \\sim C28-C27
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C10A \\sim C9A \\sim C26A \\sim N3A \\sim C27A \\sim C28A \\sim C29A \\sim C30A
\\sim C31A \\sim C36A \\sim C35A \\sim C34A \\sim C33A \\sim C32A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C10A, C9A, C26A, N3A, C27A, C28A, C29A, C30A, C31A, C36A, C35A, C34A, C33A,
 C32A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C10A)=Sof(C9A)=Sof(H9A)=Sof(C26A)=Sof(H26A)=Sof(N3A)=Sof(C27A)=Sof(C28A)=
 Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(C36A)=
 Sof(C35A)=Sof(H35A)=Sof(C34A)=Sof(H34A)=Sof(C33A)=Sof(H33A)=Sof(C32A)=
 Sof(H32A)=1-FVAR(1)
 Sof(N3)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(C28)=Sof(H28)=
 Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(C32)=Sof(H32)=Sof(C33)=
 Sof(H33)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35)=Sof(C36)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C21(H21)
6.b Secondary CH2 refined with riding coordinates:
 C22(H22a,H22b), C23(H23a,H23b), C24(H24a,H24b), C47(H47a,H47b), C48(H48a,
 H48b), C49(H49a,H49b), C50(H50a,H50b)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C7(H7), C9(H9), C26(H26), C28(H28), C29(H29), C30(H30),
 C32(H32), C33(H33), C34(H34), C35(H35), C38(H38), C39(H39), C40(H40), C42(H42),
  C43(H43), C44(H44), C45(H45), C9A(H9A), C26A(H26A), C28A(H28A), C29A(H29A),
 C30A(H30A), C35A(H35A), C34A(H34A), C33A(H33A), C32A(H32A)
6.d Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C16(H16a,H16b,H16c), C18(H18a,H18b,
 H18c), C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C25(H25a,H25b,H25c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.88264(8) 0.24399(5) 0.77081(8) 0.0345(3) Uani 1 1 d . . . . .
N1 N 0.61251(9) 0.29490(6) 0.67177(9) 0.0282(3) Uani 1 1 d . . . . .
N2 N 0.69794(9) 0.17994(6) 0.61136(9) 0.0295(3) Uani 1 1 d . . . . .
N3 N 0.79337(10) 0.37793(6) 0.73336(10) 0.0263(4) Uani 0.870(3) 1 d D . P A 1
C1 C 0.53072(11) 0.19015(7) 0.64020(11) 0.0294(3) Uani 1 1 d . . . . .
C2 C 0.43780(11) 0.16013(7) 0.61270(11) 0.0301(3) Uani 1 1 d . . . . .
H2 H 0.437765 0.116427 0.609173 0.036 Uiso 1 1 calc R . . . .
C3 C 0.34363(11) 0.19075(7) 0.58974(10) 0.0283(3) Uani 1 1 d . . . . .
C4 C 0.34462(11) 0.25483(7) 0.59269(10) 0.0275(3) Uani 1 1 d . . . . .
H4 H 0.282495 0.276973 0.576352 0.033 Uiso 1 1 calc R . . . .
C5 C 0.43629(10) 0.28668(7) 0.61949(10) 0.0251(3) Uani 1 1 d . . . . .
C6 C 0.46221(10) 0.35094(6) 0.63212(10) 0.0251(3) Uani 1 1 d . . . . .
C7 C 0.40552(11) 0.40484(7) 0.61893(11) 0.0285(3) Uani 1 1 d . . . . .
H7 H 0.333817 0.402490 0.595676 0.034 Uiso 1 1 calc R . . . .
C8 C 0.45171(12) 0.46238(7) 0.63913(11) 0.0320(3) Uani 1 1 d D . . . .
C9 C 0.55578(15) 0.46412(9) 0.67711(16) 0.0285(4) Uani 0.870(3) 1 d D . P A 1
H9 H 0.587317 0.502880 0.695333 0.034 Uiso 0.870(3) 1 calc R . P A 1
C10 C 0.61683(15) 0.41121(10) 0.68993(15) 0.0255(5) Uani 0.870(3) 1 d D . P A 1
C11 C 0.57014(10) 0.35234(7) 0.66503(10) 0.0270(3) Uani 1 1 d D . . . .
C12 C 0.53018(10) 0.25500(7) 0.64472(10) 0.0258(3) Uani 1 1 d . . . . .
C13 C 0.24204(12) 0.15604(7) 0.55998(12) 0.0347(3) Uani 1 1 d . . . . .
C14 C 0.25514(14) 0.08696(8) 0.58151(16) 0.0491(5) Uani 1 1 d . . . . .
H14A H 0.294682 0.068546 0.540316 0.074 Uiso 1 1 calc GR . . . .
H14B H 0.188355 0.067262 0.567922 0.074 Uiso 1 1 calc GR . . . .
H14C H 0.290760 0.080873 0.650081 0.074 Uiso 1 1 calc GR . . . .
C15 C 0.16941(14) 0.18108(8) 0.61648(15) 0.0459(4) Uani 1 1 d . . . . .
H15A H 0.200284 0.176682 0.686422 0.069 Uiso 1 1 calc GR . . . .
H15B H 0.105695 0.157889 0.598519 0.069 Uiso 1 1 calc GR . . . .
H15C H 0.155753 0.224707 0.600681 0.069 Uiso 1 1 calc GR . . . .
C16 C 0.19496(13) 0.16548(10) 0.45102(14) 0.0496(5) Uani 1 1 d . . . . .
H16A H 0.181907 0.209437 0.437743 0.074 Uiso 1 1 calc GR . . . .
H16B H 0.131017 0.142626 0.431104 0.074 Uiso 1 1 calc GR . . . .
H16C H 0.241817 0.150425 0.414479 0.074 Uiso 1 1 calc GR . . . .
C17 C 0.39003(13) 0.52240(7) 0.62577(13) 0.0402(4) Uani 1 1 d . . . . .
C18 C 0.28700(17) 0.51425(10) 0.5525(2) 0.0799(9) Uani 1 1 d . . . . .
H18A H 0.296834 0.497754 0.491496 0.120 Uiso 1 1 calc GR . . . .
H18B H 0.252632 0.554201 0.540055 0.120 Uiso 1 1 calc GR . . . .
H18C H 0.245492 0.485577 0.578814 0.120 Uiso 1 1 calc GR . . . .
C19 C 0.3743(2) 0.54173(10) 0.72365(18) 0.0652(6) Uani 1 1 d . . . . .
H19A H 0.338593 0.508958 0.748572 0.098 Uiso 1 1 calc GR . . . .
H19B H 0.333999 0.579619 0.715645 0.098 Uiso 1 1 calc GR . . . .
H19C H 0.440338 0.549040 0.769713 0.098 Uiso 1 1 calc GR . . . .
C20 C 0.44582(16) 0.57369(8) 0.58685(15) 0.0480(4) Uani 1 1 d . . . . .
H20A H 0.509489 0.583201 0.635136 0.072 Uiso 1 1 calc GR . . . .
H20B H 0.403164 0.610637 0.574195 0.072 Uiso 1 1 calc GR . . . .
H20C H 0.460513 0.560056 0.526337 0.072 Uiso 1 1 calc GR . . . .
C21 C 0.62891(12) 0.15381(7) 0.66672(11) 0.0315(3) Uani 1 1 d . . . . .
H21 H 0.613468 0.110165 0.645542 0.038 Uiso 1 1 calc R . . . .
C22 C 0.67912(13) 0.15411(8) 0.77710(11) 0.0357(3) Uani 1 1 d . . . . .
H22A H 0.742550 0.129794 0.789818 0.043 Uiso 1 1 calc R . . . .
H22B H 0.697719 0.197001 0.797899 0.043 Uiso 1 1 calc R . . . .
C23 C 0.61259(14) 0.12804(8) 0.83900(11) 0.0369(4) Uani 1 1 d . . . . .
H23A H 0.647749 0.134581 0.908383 0.044 Uiso 1 1 calc R . . . .
H23B H 0.548640 0.151894 0.824969 0.044 Uiso 1 1 calc R . . . .
C24 C 0.58630(15) 0.06007(8) 0.82392(13) 0.0430(4) Uani 1 1 d . . . . .
H24A H 0.649617 0.035561 0.839556 0.052 Uiso 1 1 calc R . . . .
H24B H 0.551196 0.052863 0.754704 0.052 Uiso 1 1 calc R . . . .
C25 C 0.51860(19) 0.03834(9) 0.88732(16) 0.0591(6) Uani 1 1 d . . . . .
H25A H 0.453973 0.060574 0.869052 0.089 Uiso 1 1 calc GR . . . .
H25B H 0.552306 0.046438 0.955810 0.089 Uiso 1 1 calc GR . . . .
H25C H 0.506031 -0.005965 0.877841 0.089 Uiso 1 1 calc GR . . . .
C26 C 0.72511(12) 0.42023(8) 0.72538(12) 0.0265(4) Uani 0.870(3) 1 d D . P A 1
H26 H 0.748053 0.460781 0.744463 0.032 Uiso 0.870(3) 1 calc R . P A 1
C27 C 0.89539(13) 0.39615(8) 0.77645(14) 0.0277(4) Uani 0.870(3) 1 d D . P A 1
C28 C 0.9231(2) 0.42247(15) 0.86757(18) 0.0336(6) Uani 0.870(3) 1 d D . P A 1
H28 H 0.872769 0.430706 0.901049 0.040 Uiso 0.870(3) 1 calc R . P A 1
C29 C 1.0256(2) 0.43740(11) 0.91199(16) 0.0379(5) Uani 0.870(3) 1 d D . P A 1
H29 H 1.043255 0.455012 0.975243 0.045 Uiso 0.870(3) 1 calc R . P A 1
C30 C 1.0990(2) 0.42682(14) 0.8651(2) 0.0358(6) Uani 0.870(3) 1 d D . P A 1
H30 H 1.167513 0.436982 0.895896 0.043 Uiso 0.870(3) 1 calc R . P A 1
C31 C 1.0737(3) 0.4007(3) 0.7705(4) 0.0312(7) Uani 0.870(3) 1 d D . P A 1
C32 C 1.14753(17) 0.38866(13) 0.7195(2) 0.0355(5) Uani 0.870(3) 1 d D . P A 1
H32 H 1.216516 0.398449 0.748826 0.043 Uiso 0.870(3) 1 calc R . P A 1
C33 C 1.12133(16) 0.36321(9) 0.62882(16) 0.0377(5) Uani 0.870(3) 1 d D . P A 1
H33 H 1.172177 0.355782 0.595617 0.045 Uiso 0.870(3) 1 calc R . P A 1
C34 C 1.01920(18) 0.34773(10) 0.58356(17) 0.0338(5) Uani 0.870(3) 1 d D . P A 1
H34 H 1.001988 0.330106 0.520323 0.041 Uiso 0.870(3) 1 calc R . P A 1
C35 C 0.9451(2) 0.35811(17) 0.6308(2) 0.0309(6) Uani 0.870(3) 1 d D . P A 1
H35 H 0.876611 0.347789 0.600077 0.037 Uiso 0.870(3) 1 calc R . P A 1
C36 C 0.97050(14) 0.38427(9) 0.72544(15) 0.0268(4) Uani 0.870(3) 1 d D . P A 1
C37 C 0.76324(11) 0.14132(8) 0.57693(11) 0.0324(3) Uani 1 1 d . . . . .
C38 C 0.78709(13) 0.08225(8) 0.61093(13) 0.0403(4) Uani 1 1 d . . . . .
H38 H 0.759548 0.066403 0.660783 0.048 Uiso 1 1 calc R . . . .
C39 C 0.85216(14) 0.04506(10) 0.57224(16) 0.0545(5) Uani 1 1 d . . . . .
H39 H 0.868715 0.004755 0.597349 0.065 Uiso 1 1 calc R . . . .
C40 C 0.89110(14) 0.06579(11) 0.50040(17) 0.0585(6) Uani 1 1 d . . . . .
H40 H 0.932578 0.039444 0.473830 0.070 Uiso 1 1 calc R . . . .
C41 C 0.87087(12) 0.12623(11) 0.46426(13) 0.0505(5) Uani 1 1 d . . . . .
C42 C 0.91098(14) 0.14943(15) 0.38907(15) 0.0655(7) Uani 1 1 d . . . . .
H42 H 0.950650 0.123103 0.360353 0.079 Uiso 1 1 calc R . . . .
C43 C 0.89416(15) 0.20828(16) 0.35706(14) 0.0715(8) Uani 1 1 d . . . . .
H43 H 0.922472 0.222701 0.306848 0.086 Uiso 1 1 calc R . . . .
C44 C 0.83462(14) 0.24838(13) 0.39804(13) 0.0598(6) Uani 1 1 d . . . . .
H44 H 0.823892 0.289801 0.376246 0.072 Uiso 1 1 calc R . . . .
C45 C 0.79246(12) 0.22696(10) 0.46959(12) 0.0443(4) Uani 1 1 d . . . . .
H45 H 0.752068 0.253864 0.496522 0.053 Uiso 1 1 calc R . . . .
C46 C 0.80806(11) 0.16559(9) 0.50389(11) 0.0375(4) Uani 1 1 d . . . . .
C47 C 0.91667(12) 0.24068(8) 0.87521(11) 0.0373(4) Uani 1 1 d . . . . .
H47A H 0.899370 0.200255 0.898830 0.045 Uiso 1 1 calc R . . . .
H47B H 0.885085 0.273611 0.905506 0.045 Uiso 1 1 calc R . . . .
C48 C 1.03072(12) 0.24915(7) 0.89901(11) 0.0322(3) Uani 1 1 d . . . . .
H48A H 1.065238 0.222692 0.954357 0.039 Uiso 1 1 calc R . . . .
H48B H 1.049493 0.292629 0.915477 0.039 Uiso 1 1 calc R . . . .
C49 C 1.05913(11) 0.22986(7) 0.80543(10) 0.0293(3) Uani 1 1 d . . . . .
H49A H 1.090911 0.264471 0.778951 0.035 Uiso 1 1 calc R . . . .
H49B H 1.106521 0.194496 0.817781 0.035 Uiso 1 1 calc R . . . .
C50 C 0.95815(11) 0.21200(7) 0.73582(11) 0.0317(3) Uani 1 1 d . . . . .
H50A H 0.955789 0.224864 0.668565 0.038 Uiso 1 1 calc R . . . .
H50B H 0.947575 0.166909 0.736669 0.038 Uiso 1 1 calc R . . . .
Li1 Li 0.7579(2) 0.28353(15) 0.7067(2) 0.0443(7) Uani 1 1 d . . . . .
C10A C 0.6311(9) 0.4021(6) 0.6611(12) 0.028(3) Uani 0.130(3) 1 d D U P A 2
C9A C 0.5674(9) 0.4538(7) 0.6504(12) 0.031(4) Uiso 0.130(3) 1 d D U P A 2
H9A H 0.602368 0.491555 0.649930 0.037 Uiso 0.130(3) 1 calc R . P A 2
C26A C 0.7388(8) 0.4030(5) 0.6670(10) 0.032(3) Uani 0.130(3) 1 d D U P A 2
H26A H 0.770347 0.442319 0.672387 0.038 Uiso 0.130(3) 1 calc R . P A 2
N3A N 0.7964(7) 0.3557(4) 0.6658(8) 0.035(2) Uani 0.130(3) 1 d D U P A 2
C27A C 0.9013(9) 0.3681(6) 0.6751(11) 0.041(3) Uani 0.130(3) 1 d D U P A 2
C28A C 0.9562(19) 0.3505(15) 0.611(2) 0.045(4) Uani 0.130(3) 1 d D U P A 2
H28A H 0.918061 0.329908 0.554811 0.054 Uiso 0.130(3) 1 calc R . P A 2
C29A C 1.0588(15) 0.3579(8) 0.6161(14) 0.047(3) Uani 0.130(3) 1 d D U P A 2
H29A H 1.088636 0.343740 0.566830 0.057 Uiso 0.130(3) 1 calc R . P A 2
C30A C 1.1121(15) 0.3872(11) 0.6974(16) 0.051(4) Uani 0.130(3) 1 d D U P A 2
H30A H 1.181472 0.397329 0.705590 0.061 Uiso 0.130(3) 1 calc R . P A 2
C31A C 1.062(3) 0.402(3) 0.770(3) 0.050(4) Uani 0.130(3) 1 d D U P A 2
C36A C 0.9588(14) 0.3970(8) 0.7591(12) 0.044(3) Uani 0.130(3) 1 d D U P A 2
C35A C 0.9176(19) 0.4149(13) 0.8354(17) 0.049(4) Uani 0.130(3) 1 d D U P A 2
H35A H 0.848198 0.407503 0.831992 0.059 Uiso 0.130(3) 1 calc R . P A 2
C34A C 0.9779(16) 0.4428(10) 0.9134(16) 0.059(4) Uani 0.130(3) 1 d D U P A 2
H34A H 0.948383 0.454231 0.964328 0.071 Uiso 0.130(3) 1 calc R . P A 2
C33A C 1.0811(15) 0.4563(10) 0.9260(15) 0.065(4) Uani 0.130(3) 1 d D U P A 2
H33A H 1.121672 0.476805 0.981614 0.079 Uiso 0.130(3) 1 calc R . P A 2
C32A C 1.117(2) 0.4370(14) 0.8500(19) 0.061(4) Uani 0.130(3) 1 d D U P A 2
H32A H 1.184741 0.447763 0.851349 0.073 Uiso 0.130(3) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C47 1.4395(18) . ?
O1 C50 1.4356(18) . ?
O1 Li1 1.914(3) . ?
N1 C11 1.3675(19) . ?
N1 C12 1.3919(18) . ?
N1 Li1 1.933(3) . ?
N2 C21 1.4895(19) . ?
N2 C37 1.4020(19) . ?
N2 Li1 2.644(4) . ?
N3 C26 1.292(2) . ?
N3 C27 1.425(2) . ?
N3 Li1 2.117(4) . ?
C1 C2 1.389(2) . ?
C1 C12 1.409(2) . ?
C1 C21 1.517(2) . ?
C2 H2 0.9500 . ?
C2 C3 1.408(2) . ?
C3 C4 1.392(2) . ?
C3 C13 1.538(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.3938(19) . ?
C5 C6 1.439(2) . ?
C5 C12 1.417(2) . ?
C6 C7 1.389(2) . ?
C6 C11 1.4262(19) . ?
C7 H7 0.9500 . ?
C7 C8 1.395(2) . ?
C8 C9 1.384(2) . ?
C8 C17 1.536(2) . ?
C8 C9A 1.558(12) . ?
C9 H9 0.9500 . ?
C9 C10 1.403(3) . ?
C10 C11 1.431(2) . ?
C10 C26 1.446(2) . ?
C11 C10A 1.373(12) . ?
C13 C14 1.532(2) . ?
C13 C15 1.530(2) . ?
C13 C16 1.531(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.529(3) . ?
C17 C19 1.523(3) . ?
C17 C20 1.532(2) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21 1.0000 . ?
C21 C22 1.543(2) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.529(2) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.521(2) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.525(3) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26 0.9500 . ?
C27 C28 1.378(3) . ?
C27 C36 1.426(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.415(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.361(4) . ?
C30 H30 0.9500 . ?
C30 C31 1.419(4) . ?
C31 C32 1.411(4) . ?
C31 C36 1.434(4) . ?
C32 H32 0.9500 . ?
C32 C33 1.364(3) . ?
C33 H33 0.9500 . ?
C33 C34 1.416(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.372(3) . ?
C35 H35 0.9500 . ?
C35 C36 1.420(3) . ?
C37 C38 1.379(2) . ?
C37 C46 1.437(2) . ?
C38 H38 0.9500 . ?
C38 C39 1.414(2) . ?
C39 H39 0.9500 . ?
C39 C40 1.347(3) . ?
C40 H40 0.9500 . ?
C40 C41 1.410(3) . ?
C41 C42 1.416(3) . ?
C41 C46 1.427(2) . ?
C42 H42 0.9500 . ?
C42 C43 1.356(4) . ?
C43 H43 0.9500 . ?
C43 C44 1.417(4) . ?
C44 H44 0.9500 . ?
C44 C45 1.375(2) . ?
C45 H45 0.9500 . ?
C45 C46 1.416(3) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.517(2) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C49 1.540(2) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C50 1.524(2) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
Li1 N3A 1.797(10) . ?
C10A C9A 1.403(15) . ?
C10A C26A 1.452(13) . ?
C9A H9A 0.9500 . ?
C26A H26A 0.9500 . ?
C26A N3A 1.296(13) . ?
N3A C27A 1.430(13) . ?
C27A C28A 1.373(17) . ?
C27A C36A 1.396(16) . ?
C28A H28A 0.9500 . ?
C28A C29A 1.394(18) . ?
C29A H29A 0.9500 . ?
C29A C30A 1.354(18) . ?
C30A H30A 0.9500 . ?
C30A C31A 1.42(2) . ?
C31A C36A 1.39(4) . ?
C31A C32A 1.41(2) . ?
C36A C35A 1.403(17) . ?
C35A H35A 0.9500 . ?
C35A C34A 1.342(18) . ?
C34A H34A 0.9500 . ?
C34A C33A 1.405(17) . ?
C33A H33A 0.9500 . ?
C33A C32A 1.365(18) . ?
C32A H32A 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C47 O1 Li1 121.56(14) . . ?
C50 O1 C47 105.43(11) . . ?
C50 O1 Li1 132.99(13) . . ?
C11 N1 C12 104.55(11) . . ?
C11 N1 Li1 121.46(14) . . ?
C12 N1 Li1 133.91(14) . . ?
C21 N2 Li1 101.90(11) . . ?
C37 N2 C21 120.34(13) . . ?
C37 N2 Li1 123.21(11) . . ?
C26 N3 C27 116.30(15) . . ?
C26 N3 Li1 123.07(13) . . ?
C27 N3 Li1 119.90(13) . . ?
C2 C1 C12 117.78(14) . . ?
C2 C1 C21 120.68(14) . . ?
C12 C1 C21 121.52(13) . . ?
C1 C2 H2 118.1 . . ?
C1 C2 C3 123.79(14) . . ?
C3 C2 H2 118.1 . . ?
C2 C3 C13 122.45(13) . . ?
C4 C3 C2 117.62(13) . . ?
C4 C3 C13 119.92(13) . . ?
C3 C4 H4 119.8 . . ?
C3 C4 C5 120.34(13) . . ?
C5 C4 H4 119.8 . . ?
C4 C5 C6 133.59(13) . . ?
C4 C5 C12 121.20(13) . . ?
C12 C5 C6 105.17(12) . . ?
C7 C6 C5 133.59(13) . . ?
C7 C6 C11 121.26(13) . . ?
C11 C6 C5 105.16(12) . . ?
C6 C7 H7 119.3 . . ?
C6 C7 C8 121.33(13) . . ?
C8 C7 H7 119.3 . . ?
C7 C8 C17 121.98(14) . . ?
C7 C8 C9A 107.8(6) . . ?
C9 C8 C7 117.95(15) . . ?
C9 C8 C17 119.98(15) . . ?
C17 C8 C9A 128.6(6) . . ?
C8 C9 H9 118.5 . . ?
C8 C9 C10 122.94(17) . . ?
C10 C9 H9 118.5 . . ?
C9 C10 C11 119.17(17) . . ?
C9 C10 C26 116.98(17) . . ?
C11 C10 C26 123.82(18) . . ?
N1 C11 C6 112.70(12) . . ?
N1 C11 C10 130.08(14) . . ?
N1 C11 C10A 118.0(6) . . ?
C6 C11 C10 117.15(14) . . ?
C10A C11 C6 126.1(6) . . ?
N1 C12 C1 128.37(13) . . ?
N1 C12 C5 112.40(12) . . ?
C1 C12 C5 119.23(13) . . ?
C14 C13 C3 111.98(14) . . ?
C15 C13 C3 110.04(12) . . ?
C15 C13 C14 107.49(14) . . ?
C15 C13 C16 109.05(15) . . ?
C16 C13 C3 108.94(13) . . ?
C16 C13 C14 109.29(15) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C8 111.36(14) . . ?
C18 C17 C20 107.05(17) . . ?
C19 C17 C8 108.87(15) . . ?
C19 C17 C18 109.5(2) . . ?
C19 C17 C20 109.41(16) . . ?
C20 C17 C8 110.66(14) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N2 C21 C1 108.10(12) . . ?
N2 C21 H21 108.3 . . ?
N2 C21 C22 111.27(12) . . ?
C1 C21 H21 108.3 . . ?
C1 C21 C22 112.43(13) . . ?
C22 C21 H21 108.3 . . ?
C21 C22 H22A 108.7 . . ?
C21 C22 H22B 108.7 . . ?
H22A C22 H22B 107.6 . . ?
C23 C22 C21 114.35(13) . . ?
C23 C22 H22A 108.7 . . ?
C23 C22 H22B 108.7 . . ?
C22 C23 H23A 108.4 . . ?
C22 C23 H23B 108.4 . . ?
H23A C23 H23B 107.5 . . ?
C24 C23 C22 115.56(14) . . ?
C24 C23 H23A 108.4 . . ?
C24 C23 H23B 108.4 . . ?
C23 C24 H24A 109.2 . . ?
C23 C24 H24B 109.2 . . ?
C23 C24 C25 111.95(15) . . ?
H24A C24 H24B 107.9 . . ?
C25 C24 H24A 109.2 . . ?
C25 C24 H24B 109.2 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N3 C26 C10 125.68(16) . . ?
N3 C26 H26 117.2 . . ?
C10 C26 H26 117.2 . . ?
N3 C27 C36 118.88(17) . . ?
C28 C27 N3 121.28(19) . . ?
C28 C27 C36 119.79(19) . . ?
C27 C28 H28 119.5 . . ?
C27 C28 C29 120.9(2) . . ?
C29 C28 H28 119.5 . . ?
C28 C29 H29 119.6 . . ?
C30 C29 C28 120.8(2) . . ?
C30 C29 H29 119.6 . . ?
C29 C30 H30 119.9 . . ?
C29 C30 C31 120.3(3) . . ?
C31 C30 H30 119.9 . . ?
C30 C31 C36 119.5(3) . . ?
C32 C31 C30 122.1(3) . . ?
C32 C31 C36 118.3(3) . . ?
C31 C32 H32 119.5 . . ?
C33 C32 C31 121.0(2) . . ?
C33 C32 H32 119.5 . . ?
C32 C33 H33 119.6 . . ?
C32 C33 C34 120.76(19) . . ?
C34 C33 H33 119.6 . . ?
C33 C34 H34 119.9 . . ?
C35 C34 C33 120.2(2) . . ?
C35 C34 H34 119.9 . . ?
C34 C35 H35 120.0 . . ?
C34 C35 C36 120.1(3) . . ?
C36 C35 H35 120.0 . . ?
C27 C36 C31 118.7(2) . . ?
C35 C36 C27 121.66(19) . . ?
C35 C36 C31 119.6(2) . . ?
N2 C37 C46 117.60(14) . . ?
C38 C37 N2 123.14(15) . . ?
C38 C37 C46 119.25(15) . . ?
C37 C38 H38 119.7 . . ?
C37 C38 C39 120.58(19) . . ?
C39 C38 H38 119.7 . . ?
C38 C39 H39 119.4 . . ?
C40 C39 C38 121.2(2) . . ?
C40 C39 H39 119.4 . . ?
C39 C40 H40 119.7 . . ?
C39 C40 C41 120.61(18) . . ?
C41 C40 H40 119.7 . . ?
C40 C41 C42 121.9(2) . . ?
C40 C41 C46 119.58(19) . . ?
C42 C41 C46 118.5(2) . . ?
C41 C42 H42 119.2 . . ?
C43 C42 C41 121.6(2) . . ?
C43 C42 H42 119.2 . . ?
C42 C43 H43 119.8 . . ?
C42 C43 C44 120.4(2) . . ?
C44 C43 H43 119.8 . . ?
C43 C44 H44 120.2 . . ?
C45 C44 C43 119.6(2) . . ?
C45 C44 H44 120.2 . . ?
C44 C45 H45 119.4 . . ?
C44 C45 C46 121.29(19) . . ?
C46 C45 H45 119.4 . . ?
C41 C46 C37 118.67(18) . . ?
C45 C46 C37 122.71(15) . . ?
C45 C46 C41 118.61(17) . . ?
O1 C47 H47A 110.7 . . ?
O1 C47 H47B 110.7 . . ?
O1 C47 C48 105.17(12) . . ?
H47A C47 H47B 108.8 . . ?
C48 C47 H47A 110.7 . . ?
C48 C47 H47B 110.7 . . ?
C47 C48 H48A 110.9 . . ?
C47 C48 H48B 110.9 . . ?
C47 C48 C49 104.42(12) . . ?
H48A C48 H48B 108.9 . . ?
C49 C48 H48A 110.9 . . ?
C49 C48 H48B 110.9 . . ?
C48 C49 H49A 110.9 . . ?
C48 C49 H49B 110.9 . . ?
H49A C49 H49B 109.0 . . ?
C50 C49 C48 104.06(12) . . ?
C50 C49 H49A 110.9 . . ?
C50 C49 H49B 110.9 . . ?
O1 C50 C49 105.15(12) . . ?
O1 C50 H50A 110.7 . . ?
O1 C50 H50B 110.7 . . ?
C49 C50 H50A 110.7 . . ?
C49 C50 H50B 110.7 . . ?
H50A C50 H50B 108.8 . . ?
O1 Li1 N1 155.11(18) . . ?
O1 Li1 N2 88.97(13) . . ?
O1 Li1 N3 102.39(15) . . ?
N1 Li1 N2 79.41(12) . . ?
N1 Li1 N3 95.42(14) . . ?
N3 Li1 N2 160.24(15) . . ?
N3A Li1 O1 104.3(3) . . ?
N3A Li1 N1 100.0(3) . . ?
N3A Li1 N2 130.7(4) . . ?
C11 C10A C9A 105.6(10) . . ?
C11 C10A C26A 128.6(11) . . ?
C9A C10A C26A 125.8(11) . . ?
C8 C9A H9A 113.2 . . ?
C10A C9A C8 133.7(12) . . ?
C10A C9A H9A 113.2 . . ?
C10A C26A H26A 116.6 . . ?
N3A C26A C10A 126.7(11) . . ?
N3A C26A H26A 116.6 . . ?
C26A N3A Li1 117.1(8) . . ?
C26A N3A C27A 116.5(10) . . ?
C27A N3A Li1 120.3(8) . . ?
C28A C27A N3A 126.3(17) . . ?
C28A C27A C36A 114.2(17) . . ?
C36A C27A N3A 119.4(14) . . ?
C27A C28A H28A 114.7 . . ?
C27A C28A C29A 131(2) . . ?
C29A C28A H28A 114.7 . . ?
C28A C29A H29A 123.0 . . ?
C30A C29A C28A 114(2) . . ?
C30A C29A H29A 123.0 . . ?
C29A C30A H30A 120.7 . . ?
C29A C30A C31A 119(2) . . ?
C31A C30A H30A 120.7 . . ?
C36A C31A C30A 125(3) . . ?
C36A C31A C32A 117(3) . . ?
C32A C31A C30A 117(3) . . ?
C27A C36A C35A 122.6(19) . . ?
C31A C36A C27A 117.6(19) . . ?
C31A C36A C35A 119(2) . . ?
C36A C35A H35A 120.6 . . ?
C34A C35A C36A 119(2) . . ?
C34A C35A H35A 120.6 . . ?
C35A C34A H34A 117.3 . . ?
C35A C34A C33A 125(2) . . ?
C33A C34A H34A 117.3 . . ?
C34A C33A H33A 123.6 . . ?
C32A C33A C34A 113(2) . . ?
C32A C33A H33A 123.6 . . ?
C31A C32A H32A 117.2 . . ?
C33A C32A C31A 126(3) . . ?
C33A C32A H32A 117.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C47 C48 C49 -23.21(16) . . . . ?
O1 Li1 N3A C26A -144.7(9) . . . . ?
O1 Li1 N3A C27A 7.0(11) . . . . ?
N1 C11 C10A C9A 177.6(9) . . . . ?
N1 C11 C10A C26A -2.7(19) . . . . ?
N1 Li1 N3A C26A 29.5(10) . . . . ?
N1 Li1 N3A C27A -178.8(10) . . . . ?
N2 C21 C22 C23 179.85(13) . . . . ?
N2 C37 C38 C39 178.95(14) . . . . ?
N2 C37 C46 C41 -177.00(13) . . . . ?
N2 C37 C46 C45 3.0(2) . . . . ?
N2 Li1 N3A C26A 114.1(9) . . . . ?
N2 Li1 N3A C27A -94.2(11) . . . . ?
N3 C27 C28 C29 176.6(2) . . . . ?
N3 C27 C36 C31 -177.8(4) . . . . ?
N3 C27 C36 C35 3.7(3) . . . . ?
C1 C2 C3 C4 1.6(2) . . . . ?
C1 C2 C3 C13 -179.71(14) . . . . ?
C1 C21 C22 C23 58.43(18) . . . . ?
C2 C1 C12 N1 178.71(13) . . . . ?
C2 C1 C12 C5 -1.2(2) . . . . ?
C2 C1 C21 N2 130.27(14) . . . . ?
C2 C1 C21 C22 -106.51(16) . . . . ?
C2 C3 C4 C5 -1.3(2) . . . . ?
C2 C3 C13 C14 13.4(2) . . . . ?
C2 C3 C13 C15 132.87(16) . . . . ?
C2 C3 C13 C16 -107.63(17) . . . . ?
C3 C4 C5 C6 -177.86(14) . . . . ?
C3 C4 C5 C12 -0.3(2) . . . . ?
C4 C3 C13 C14 -168.00(14) . . . . ?
C4 C3 C13 C15 -48.5(2) . . . . ?
C4 C3 C13 C16 70.99(18) . . . . ?
C4 C5 C6 C7 -2.7(3) . . . . ?
C4 C5 C6 C11 177.25(15) . . . . ?
C4 C5 C12 N1 -178.36(12) . . . . ?
C4 C5 C12 C1 1.6(2) . . . . ?
C5 C6 C7 C8 178.68(15) . . . . ?
C5 C6 C11 N1 1.22(16) . . . . ?
C5 C6 C11 C10 -175.93(14) . . . . ?
C5 C6 C11 C10A 160.5(9) . . . . ?
C6 C5 C12 N1 -0.20(15) . . . . ?
C6 C5 C12 C1 179.77(12) . . . . ?
C6 C7 C8 C9 -2.9(2) . . . . ?
C6 C7 C8 C17 -179.47(14) . . . . ?
C6 C7 C8 C9A 13.9(6) . . . . ?
C6 C11 C10A C9A 19.3(16) . . . . ?
C6 C11 C10A C26A -161.0(11) . . . . ?
C7 C6 C11 N1 -178.82(13) . . . . ?
C7 C6 C11 C10 4.0(2) . . . . ?
C7 C6 C11 C10A -19.6(9) . . . . ?
C7 C8 C9 C10 4.3(3) . . . . ?
C7 C8 C17 C18 -23.6(3) . . . . ?
C7 C8 C17 C19 97.18(19) . . . . ?
C7 C8 C17 C20 -142.54(16) . . . . ?
C7 C8 C9A C10A -13.1(19) . . . . ?
C8 C9 C10 C11 -1.5(3) . . . . ?
C8 C9 C10 C26 176.67(19) . . . . ?
C9 C8 C17 C18 159.9(2) . . . . ?
C9 C8 C17 C19 -79.3(2) . . . . ?
C9 C8 C17 C20 41.0(2) . . . . ?
C9 C10 C11 N1 -179.23(17) . . . . ?
C9 C10 C11 C6 -2.7(3) . . . . ?
C9 C10 C26 N3 -173.47(18) . . . . ?
C11 N1 C12 C1 -179.04(14) . . . . ?
C11 N1 C12 C5 0.92(15) . . . . ?
C11 C6 C7 C8 -1.3(2) . . . . ?
C11 C10 C26 N3 4.6(3) . . . . ?
C11 C10A C9A C8 -3(2) . . . . ?
C11 C10A C26A N3A 9(2) . . . . ?
C12 N1 C11 C6 -1.32(16) . . . . ?
C12 N1 C11 C10 175.37(17) . . . . ?
C12 N1 C11 C10A -162.4(8) . . . . ?
C12 C1 C2 C3 -0.4(2) . . . . ?
C12 C1 C21 N2 -51.25(18) . . . . ?
C12 C1 C21 C22 71.97(18) . . . . ?
C12 C5 C6 C7 179.47(15) . . . . ?
C12 C5 C6 C11 -0.58(15) . . . . ?
C13 C3 C4 C5 -179.95(13) . . . . ?
C17 C8 C9 C10 -179.05(18) . . . . ?
C17 C8 C9A C10A -178.6(14) . . . . ?
C21 N2 C37 C38 -16.8(2) . . . . ?
C21 N2 C37 C46 164.22(13) . . . . ?
C21 C1 C2 C3 178.17(14) . . . . ?
C21 C1 C12 N1 0.2(2) . . . . ?
C21 C1 C12 C5 -179.77(13) . . . . ?
C21 C22 C23 C24 64.7(2) . . . . ?
C22 C23 C24 C25 -179.13(16) . . . . ?
C26 N3 C27 C28 56.2(3) . . . . ?
C26 N3 C27 C36 -126.57(18) . . . . ?
C26 C10 C11 N1 2.7(3) . . . . ?
C26 C10 C11 C6 179.30(16) . . . . ?
C27 N3 C26 C10 -175.76(17) . . . . ?
C27 C28 C29 C30 0.9(4) . . . . ?
C28 C27 C36 C31 -0.5(5) . . . . ?
C28 C27 C36 C35 -179.0(3) . . . . ?
C28 C29 C30 C31 0.2(6) . . . . ?
C29 C30 C31 C32 -179.7(5) . . . . ?
C29 C30 C31 C36 -1.3(8) . . . . ?
C30 C31 C32 C33 179.7(5) . . . . ?
C30 C31 C36 C27 1.5(8) . . . . ?
C30 C31 C36 C35 180.0(5) . . . . ?
C31 C32 C33 C34 -0.4(5) . . . . ?
C32 C31 C36 C27 179.9(4) . . . . ?
C32 C31 C36 C35 -1.6(8) . . . . ?
C32 C33 C34 C35 -0.1(4) . . . . ?
C33 C34 C35 C36 -0.2(5) . . . . ?
C34 C35 C36 C27 179.5(2) . . . . ?
C34 C35 C36 C31 1.1(6) . . . . ?
C36 C27 C28 C29 -0.7(4) . . . . ?
C36 C31 C32 C33 1.3(8) . . . . ?
C37 N2 C21 C1 -144.60(13) . . . . ?
C37 N2 C21 C22 91.48(16) . . . . ?
C37 C38 C39 C40 -1.1(3) . . . . ?
C38 C37 C46 C41 4.0(2) . . . . ?
C38 C37 C46 C45 -176.00(15) . . . . ?
C38 C39 C40 C41 2.4(3) . . . . ?
C39 C40 C41 C42 179.76(17) . . . . ?
C39 C40 C41 C46 -0.4(3) . . . . ?
C40 C41 C42 C43 -177.63(18) . . . . ?
C40 C41 C46 C37 -2.8(2) . . . . ?
C40 C41 C46 C45 177.20(15) . . . . ?
C41 C42 C43 C44 -0.5(3) . . . . ?
C42 C41 C46 C37 177.06(15) . . . . ?
C42 C41 C46 C45 -2.9(2) . . . . ?
C42 C43 C44 C45 -1.1(3) . . . . ?
C43 C44 C45 C46 0.6(3) . . . . ?
C44 C45 C46 C37 -178.53(16) . . . . ?
C44 C45 C46 C41 1.5(2) . . . . ?
C46 C37 C38 C39 -2.1(2) . . . . ?
C46 C41 C42 C43 2.5(3) . . . . ?
C47 O1 C50 C49 -39.01(15) . . . . ?
C47 C48 C49 C50 0.07(16) . . . . ?
C48 C49 C50 O1 23.16(15) . . . . ?
C50 O1 C47 C48 39.09(16) . . . . ?
Li1 O1 C47 C48 -142.24(15) . . . . ?
Li1 O1 C50 C49 142.54(17) . . . . ?
Li1 N1 C11 C6 176.05(15) . . . . ?
Li1 N1 C11 C10 -7.3(3) . . . . ?
Li1 N1 C11 C10A 15.0(8) . . . . ?
Li1 N1 C12 C1 4.1(3) . . . . ?
Li1 N1 C12 C5 -175.97(16) . . . . ?
Li1 N2 C21 C1 74.87(13) . . . . ?
Li1 N2 C21 C22 -49.05(14) . . . . ?
Li1 N2 C37 C38 115.14(16) . . . . ?
Li1 N2 C37 C46 -63.80(17) . . . . ?
Li1 N3 C26 C10 -5.6(3) . . . . ?
Li1 N3 C27 C28 -114.4(2) . . . . ?
Li1 N3 C27 C36 62.9(2) . . . . ?
Li1 N3A C27A C28A 84(2) . . . . ?
Li1 N3A C27A C36A -90.9(15) . . . . ?
C10A C26A N3A Li1 -25.6(19) . . . . ?
C10A C26A N3A C27A -178.4(14) . . . . ?
C9A C8 C17 C18 140.1(8) . . . . ?
C9A C8 C17 C19 -99.1(8) . . . . ?
C9A C8 C17 C20 21.1(8) . . . . ?
C9A C10A C26A N3A -171.5(15) . . . . ?
C26A C10A C9A C8 177.5(13) . . . . ?
C26A N3A C27A C28A -124(2) . . . . ?
C26A N3A C27A C36A 60.9(17) . . . . ?
N3A C27A C28A C29A -177(2) . . . . ?
N3A C27A C36A C31A 173(4) . . . . ?
N3A C27A C36A C35A 0(3) . . . . ?
C27A C28A C29A C30A 0(4) . . . . ?
C27A C36A C35A C34A -179.6(19) . . . . ?
C28A C27A C36A C31A -2(4) . . . . ?
C28A C27A C36A C35A -176(2) . . . . ?
C28A C29A C30A C31A 5(5) . . . . ?
C29A C30A C31A C36A -9(8) . . . . ?
C29A C30A C31A C32A -175(4) . . . . ?
C30A C31A C36A C27A 7(8) . . . . ?
C30A C31A C36A C35A -179(4) . . . . ?
C30A C31A C32A C33A 179(3) . . . . ?
C31A C36A C35A C34A 7(5) . . . . ?
C36A C27A C28A C29A -2(4) . . . . ?
C36A C31A C32A C33A 12(8) . . . . ?
C36A C35A C34A C33A 0(4) . . . . ?
C35A C34A C33A C32A -1(3) . . . . ?
C34A C33A C32A C31A -5(5) . . . . ?
C32A C31A C36A C27A 174(4) . . . . ?
C32A C31A C36A C35A -12(7) . . . . ?

_olex2_exptl_crystal_mounting_method "'in fomblin film on a micromount"
# This is the default assumed mounting details'
_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 1.535
_oxdiff_exptl_absorpt_empirical_full_min 0.787
####################################################################### 
# 
# 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_lirnln
_database_code_depnum_ccdc_archive 'CCDC 1581978'
_audit_update_record             
;
2017-10-25 deposited with the CCDC.
2018-01-04 downloaded from the CCDC.
;
_nottingham_internal_coll_name   LIRNLN
_nottingham_internal_coll_number 16137
_nottingham_internal_coll_client RN/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'ofand \w scans'
_nottingham_internal_coll_frame_time 'degrees,, 10.00, 40.00'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_user   pcxrn3
_nottingham_internal_coll_date   30/05/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 01/06/2016
_nottingham_internal_process_user pcxrn3
_nottingham_internal_solution_date 01/06/16
_nottingham_internal_solution_user pcxrn3
_nottingham_internal_refinement_date 22/09/17
_nottingham_internal_refinement_user pcxrn3
_nottingham_internal_self_archive_date 22/09/17
_nottingham_internal_self_validation_date 22/09/17
_nottingham_internal_self_validation_user pcxrn3
_nottingham_internal_validation_date ?
_nottingham_internal_validation_user ?
_nottingham_internal_archive_date ?
_refine_special_details          
;
The diffraction limit of this data set was approximately 1.5Å, and hence this 
limit was applied during structure refinement. To reduce the parameter set used 
during refinement, the anisotropic thermal parameters for all the atoms were 
constrained to be identical.
;
_vrf_PLAT026_lirnln              
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..         35 %     
RESPONSE: This is a consequence of a poor quality data set.
;
_vrf_PLAT088_lirnln              
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.93 Note  
RESPONSE: The data was not observed beyond 1.5\%A, so this was the limit used 
during structure refinement. This has resulted in a low data to parameter ratio.
;
_vrf_PLAT250_lirnln              
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        5.7 Note  
RESPONSE: This is a consequence of a poor quality data set.
;
_vrf_PLAT340_lirnln              
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.04187 Ang.  
RESPONSE: This is a consequence of a poor quality data set.
;
_vrf_REFNR01_lirnln              
;
PROBLEM: Ratio of reflections to parameters is < 8 for a
RESPONSE: The data was not observed beyond 1.5\%A, so this was the limit used 
during structure refinement. This has resulted in a low data to parameter ratio.
;
_vrf_THETM01_lirnln              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The data was not observed beyond 1.5\%A, so this was the limit used 
during structure refinement.
;
_audit_creation_date             2017-10-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C46 H46 Li N3 O'
_chemical_formula_sum            'C46 H46 Li N3 O'
_chemical_formula_weight         663.80
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C46 H47 Li N3 O'
_chemical_oxdiff_usercomment     
'LIRNLN #16137 GVB-1048 IN FOMBLIN FILM ON MICROMOUNT FOR RN/DLK'
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'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   12.023(8)
_cell_length_b                   12.802(10)
_cell_length_c                   13.927(7)
_cell_angle_alpha                66.18(6)
_cell_angle_beta                 76.98(5)
_cell_angle_gamma                73.37(6)
_cell_volume                     1864(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    274
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      59.9020
_cell_measurement_theta_min      3.8690
_shelx_estimated_absorpt_T_max   0.977
_shelx_estimated_absorpt_T_min   0.911
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.949
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             708
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 7 0 0.0213
-6 -1 4 0.0440
0 2 9 0.0347
-1 -2 -9 0.0467
4 0 -6 0.0252
1 -7 0 0.0213
7 2 -1 0.0573

_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.043
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
-0.8211 7.1743 0.0652 -0.9767 0.1854 0.0289
-6.0823 -0.9388 3.9778 0.1911 0.9466 -0.2986
0.0124 2.1773 8.9639 0.1145 0.3695 -0.9467
-1.0188 -2.1726 -8.9621 -0.1342 -0.2367 0.9674
4.0522 -0.1047 -5.9712 -0.1800 -0.7674 0.5497
0.8211 -7.1743 -0.0652 0.9767 -0.1854 -0.0289
7.1016 2.0012 -0.9887 -0.1789 -0.9537 -0.0373

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0884
_diffrn_reflns_av_unetI/netI     0.2702
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1794
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        30.919
_diffrn_reflns_theta_max         30.919
_diffrn_reflns_theta_min         3.496
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        
'flash frozen in gaseous N2' # assumed default, please check
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00  34.00   1.00   10.00    --  -38.50  38.00 150.00   84
  2  ω    -89.00  48.00   1.00   10.00    --  -38.50   0.00  90.00  137
  3  ω    -89.00  -5.00   1.00   10.00    --  -38.50 125.00-120.00   84
  4  ω    -93.00 -53.00   1.00   10.00    --  -38.50 125.00  60.00   40
  5  ω     51.00  98.00   1.00   40.00    --  104.50 -94.00  30.00   47
  6  ω     37.00  89.00   1.00   40.00    --  104.50 -30.00-150.00   52
  7  ω    100.00 167.00   1.00   40.00    --  104.50  77.00-150.00   67
  8  ω     34.00  87.00   1.00   40.00    --  104.50 -45.00-180.00   53
  9  ω     57.00 102.00   1.00   40.00    --  104.50 -94.00 -90.00   45
 10  ω     44.00  92.00   1.00   40.00    --  104.50 -94.00  90.00   48
 11  ω     91.00 174.00   1.00   40.00    --  104.50 125.00 -30.00   83
 12  ω     31.00 109.00   1.00   40.00    --  104.50 -94.00 -30.00   78
 13  ω     47.00  90.00   1.00   40.00    --  104.50 -45.00  60.00   43
 14  ω     86.00 178.00   1.00   40.00    --  104.50  30.00 120.00   92
 15  ω     31.00  87.00   1.00   40.00    --  104.50 -30.00 -60.00   56
 16  ω     58.00  86.00   1.00   40.00    --  104.50 -38.00 -34.00   28
 17  ω     81.00 131.00   1.00   40.00    --  104.50  45.00-180.00   50
 18  ω     63.00 120.00   1.00   40.00    --  104.50-125.00-150.00   57
;
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova-Duo, Atlas'
_diffrn_measurement_method       ?
_diffrn_measurement_specimen_support 
'MiTeGen micromount' # assumed default, please check
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0189992000
_diffrn_orient_matrix_UB_12      -0.1343811000
_diffrn_orient_matrix_UB_13      0.0453883000
_diffrn_orient_matrix_UB_21      -0.1318098000
_diffrn_orient_matrix_UB_22      0.0104047000
_diffrn_orient_matrix_UB_23      0.0388777000
_diffrn_orient_matrix_UB_31      -0.0207790000
_diffrn_orient_matrix_UB_32      0.0026133000
_diffrn_orient_matrix_UB_33      -0.1062140000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                398
_reflns_number_total             1150
_reflns_odcompleteness_completeness 99.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.180
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.862
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         1150
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1929
_refine_ls_R_factor_gt           0.0967
_refine_ls_restrained_S_all      0.862
_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)+(0.0529P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1784
_refine_ls_wR_factor_ref         0.2415
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C33) = Uanis(C34) = Uanis(C35) = Uanis(C36) = Uanis(C37) = Uanis(C42) =
Uanis(C41) = Uanis(C40) = Uanis(C39) = Uanis(C38)
Uanis(C13) = Uanis(C3) = Uanis(C2) = Uanis(C1) = Uanis(C21) = Uanis(N2) =
Uanis(N1) = Uanis(C12) = Uanis(C5) = Uanis(C4) = Uanis(C6) = Uanis(C11) =
Uanis(C10) = Uanis(C9) = Uanis(C8) = Uanis(C7) = Uanis(C32) = Uanis(C17) =
Uanis(N3)
Uanis(C15) = Uanis(C14) = Uanis(C16)
Uanis(C19) = Uanis(C18) = Uanis(C20)
Uanis(O1) = Uanis(C46) = Uanis(C45) = Uanis(C44) = Uanis(C43)
Uanis(C22) = Uanis(C23) = Uanis(C24) = Uanis(C25) = Uanis(C26) = Uanis(C27) =
Uanis(C28) = Uanis(C29) = Uanis(C30) = Uanis(C31)
Uanis(C10) = Uanis(C15) = Uanis(C13) = Uanis(C12) = Uanis(C11) = Uanis(C6) =
Uanis(C14) = Uanis(C5) = Uanis(C8) = Uanis(C7) = Uanis(C9) = Uanis(N3) =
Uanis(C16) = Uanis(C4) = Uanis(C3) = Uanis(C1) = Uanis(C2) = Uanis(N2) =
Uanis(N1) = Uanis(O1) = Uanis(C18) = Uanis(C19) = Uanis(C17) = Uanis(C20) =
Uanis(C28) = Uanis(C27) = Uanis(C26) = Uanis(C25) = Uanis(C24) = Uanis(C23) =
Uanis(C22) = Uanis(C21) = Uanis(C29) = Uanis(C30) = Uanis(C31) = Uanis(C32) =
Uanis(C33) = Uanis(C34) = Uanis(C35) = Uanis(C36) = Uanis(C37) = Uanis(C38) =
Uanis(C39) = Uanis(C40) = Uanis(C41) = Uanis(C42) = Uanis(C43) = Uanis(C44) =
Uanis(C45) = Uanis(C46) = Uanis(Li1)
3. Others
 U11(O1)=U11(N1)=U11(N2)=U11(N3)=U11(C1)=U11(C2)=U11(C3)=U11(C4)=U11(C5)=
 U11(C6)=U11(C7)=U11(C8)=U11(C9)=U11(C10)=U11(C11)=U11(C12)=U11(C13)=U11(C14)=
 U11(C15)=U11(C16)=U11(C17)=U11(C18)=U11(C19)=U11(C20)=U11(C21)=U11(C22)=
 U11(C23)=U11(C24)=U11(C25)=U11(C26)=U11(C27)=U11(C28)=U11(C29)=U11(C30)=
 U11(C31)=U11(C32)=U11(C33)=U11(C34)=U11(C35)=U11(C36)=U11(C37)=U11(C38)=
 U11(C39)=U11(C40)=U11(C41)=U11(C42)=U11(C43)=U11(C44)=U11(C45)=U11(C46)=
 U11(Li1)=FVAR(1)
 U22(O1)=U22(N1)=U22(N2)=U22(N3)=U22(C1)=U22(C2)=U22(C3)=U22(C4)=U22(C5)=
 U22(C6)=U22(C7)=U22(C8)=U22(C9)=U22(C10)=U22(C11)=U22(C12)=U22(C13)=U22(C14)=
 U22(C15)=U22(C16)=U22(C17)=U22(C18)=U22(C19)=U22(C20)=U22(C21)=U22(C22)=
 U22(C23)=U22(C24)=U22(C25)=U22(C26)=U22(C27)=U22(C28)=U22(C29)=U22(C30)=
 U22(C31)=U22(C32)=U22(C33)=U22(C34)=U22(C35)=U22(C36)=U22(C37)=U22(C38)=
 U22(C39)=U22(C40)=U22(C41)=U22(C42)=U22(C43)=U22(C44)=U22(C45)=U22(C46)=
 U22(Li1)=FVAR(2)
 U33(O1)=U33(N1)=U33(N2)=U33(N3)=U33(C1)=U33(C2)=U33(C3)=U33(C4)=U33(C5)=
 U33(C6)=U33(C7)=U33(C8)=U33(C9)=U33(C10)=U33(C11)=U33(C12)=U33(C13)=U33(C14)=
 U33(C15)=U33(C16)=U33(C17)=U33(C18)=U33(C19)=U33(C20)=U33(C21)=U33(C22)=
 U33(C23)=U33(C24)=U33(C25)=U33(C26)=U33(C27)=U33(C28)=U33(C29)=U33(C30)=
 U33(C31)=U33(C32)=U33(C33)=U33(C34)=U33(C35)=U33(C36)=U33(C37)=U33(C38)=
 U33(C39)=U33(C40)=U33(C41)=U33(C42)=U33(C43)=U33(C44)=U33(C45)=U33(C46)=
 U33(Li1)=FVAR(3)
 U23(O1)=U23(N1)=U23(N2)=U23(N3)=U23(C1)=U23(C2)=U23(C3)=U23(C4)=U23(C5)=
 U23(C6)=U23(C7)=U23(C8)=U23(C9)=U23(C10)=U23(C11)=U23(C12)=U23(C13)=U23(C14)=
 U23(C15)=U23(C16)=U23(C17)=U23(C18)=U23(C19)=U23(C20)=U23(C21)=U23(C22)=
 U23(C23)=U23(C24)=U23(C25)=U23(C26)=U23(C27)=U23(C28)=U23(C29)=U23(C30)=
 U23(C31)=U23(C32)=U23(C33)=U23(C34)=U23(C35)=U23(C36)=U23(C37)=U23(C38)=
 U23(C39)=U23(C40)=U23(C41)=U23(C42)=U23(C43)=U23(C44)=U23(C45)=U23(C46)=
 U23(Li1)=FVAR(4)
 U13(O1)=U13(N1)=U13(N2)=U13(N3)=U13(C1)=U13(C2)=U13(C3)=U13(C4)=U13(C5)=
 U13(C6)=U13(C7)=U13(C8)=U13(C9)=U13(C10)=U13(C11)=U13(C12)=U13(C13)=U13(C14)=
 U13(C15)=U13(C16)=U13(C17)=U13(C18)=U13(C19)=U13(C20)=U13(C21)=U13(C22)=
 U13(C23)=U13(C24)=U13(C25)=U13(C26)=U13(C27)=U13(C28)=U13(C29)=U13(C30)=
 U13(C31)=U13(C32)=U13(C33)=U13(C34)=U13(C35)=U13(C36)=U13(C37)=U13(C38)=
 U13(C39)=U13(C40)=U13(C41)=U13(C42)=U13(C43)=U13(C44)=U13(C45)=U13(C46)=
 U13(Li1)=FVAR(5)
 U12(O1)=U12(N1)=U12(N2)=U12(N3)=U12(C1)=U12(C2)=U12(C3)=U12(C4)=U12(C5)=
 U12(C6)=U12(C7)=U12(C8)=U12(C9)=U12(C10)=U12(C11)=U12(C12)=U12(C13)=U12(C14)=
 U12(C15)=U12(C16)=U12(C17)=U12(C18)=U12(C19)=U12(C20)=U12(C21)=U12(C22)=
 U12(C23)=U12(C24)=U12(C25)=U12(C26)=U12(C27)=U12(C28)=U12(C29)=U12(C30)=
 U12(C31)=U12(C32)=U12(C33)=U12(C34)=U12(C35)=U12(C36)=U12(C37)=U12(C38)=
 U12(C39)=U12(C40)=U12(C41)=U12(C42)=U12(C43)=U12(C44)=U12(C45)=U12(C46)=
 U12(Li1)=FVAR(6)
4.a Secondary CH2 refined with riding coordinates:
 C43(H43a,H43b), C44(H44a,H44b), C45(H45a,H45b), C46(H46a,H46b)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C7(H7), C9(H9), C21(H21), C23(H23), C24(H24), C25(H25),
 C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C34(H34), C35(H35), C36(H36),
  C38(H38), C39(H39), C40(H40), C41(H41)
4.c Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C16(H16a,H16b,H16c), C18(H18a,H18b,
 H18c), C19(H19a,H19b,H19c), C20(H20a,H20b,H20c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.4675(14) 0.3937(15) 0.2983(11) 0.071(2) Uani 1 1 d . . . . .
N1 N 0.550(2) 0.2637(18) 0.5796(15) 0.071(2) Uani 1 1 d . . . . .
N2 N 0.6921(18) 0.2413(17) 0.3861(15) 0.071(2) Uani 1 1 d . . . . .
N3 N 0.3200(18) 0.3218(17) 0.5073(15) 0.071(2) Uani 1 1 d . . . . .
C1 C 0.771(3) 0.214(2) 0.545(2) 0.071(2) Uani 1 1 d . . . . .
C2 C 0.871(2) 0.177(2) 0.591(2) 0.071(2) Uani 1 1 d . . . . .
H2 H 0.944139 0.168179 0.548631 0.086 Uiso 1 1 calc R . . . .
C3 C 0.866(3) 0.153(2) 0.700(2) 0.071(2) Uani 1 1 d . . . . .
C4 C 0.764(3) 0.154(2) 0.7653(18) 0.071(2) Uani 1 1 d . . . . .
H4 H 0.762339 0.129505 0.839664 0.086 Uiso 1 1 calc R . . . .
C5 C 0.666(3) 0.192(2) 0.720(2) 0.071(2) Uani 1 1 d . . . . .
C6 C 0.542(3) 0.219(2) 0.755(2) 0.071(2) Uani 1 1 d . . . . .
C7 C 0.479(2) 0.207(2) 0.8572(19) 0.071(2) Uani 1 1 d . . . . .
H7 H 0.520227 0.171402 0.917118 0.086 Uiso 1 1 calc R . . . .
C8 C 0.358(3) 0.245(2) 0.872(2) 0.071(2) Uani 1 1 d . . . . .
C9 C 0.297(2) 0.288(2) 0.7851(19) 0.071(2) Uani 1 1 d . . . . .
H9 H 0.214227 0.314207 0.795271 0.086 Uiso 1 1 calc R . . . .
C10 C 0.353(3) 0.295(2) 0.682(2) 0.071(2) Uani 1 1 d . . . . .
C11 C 0.473(3) 0.257(2) 0.671(2) 0.071(2) Uani 1 1 d . . . . .
C12 C 0.660(3) 0.215(2) 0.610(2) 0.071(2) Uani 1 1 d . . . . .
C13 C 0.982(2) 0.110(3) 0.7464(19) 0.071(2) Uani 1 1 d . . . . .
C14 C 1.005(2) -0.025(2) 0.8054(14) 0.071(2) Uani 1 1 d . . . . .
H14A H 1.084163 -0.053226 0.826346 0.107 Uiso 1 1 calc GR . . . .
H14B H 0.998076 -0.061905 0.758690 0.107 Uiso 1 1 calc GR . . . .
H14C H 0.947703 -0.043400 0.868646 0.107 Uiso 1 1 calc GR . . . .
C15 C 0.975(2) 0.1609(19) 0.8322(14) 0.071(2) Uani 1 1 d . . . . .
H15A H 0.985154 0.241819 0.797919 0.107 Uiso 1 1 calc GR . . . .
H15B H 1.037447 0.113802 0.877143 0.107 Uiso 1 1 calc GR . . . .
H15C H 0.898993 0.159253 0.875765 0.107 Uiso 1 1 calc GR . . . .
C16 C 1.091(2) 0.131(2) 0.6719(14) 0.071(2) Uani 1 1 d . . . . .
H16A H 1.083414 0.215363 0.631919 0.107 Uiso 1 1 calc GR . . . .
H16B H 1.104124 0.090373 0.622772 0.107 Uiso 1 1 calc GR . . . .
H16C H 1.158220 0.101900 0.712124 0.107 Uiso 1 1 calc GR . . . .
C17 C 0.291(2) 0.237(3) 0.9833(19) 0.071(2) Uani 1 1 d . . . . .
C18 C 0.340(2) 0.2990(19) 1.0298(14) 0.071(2) Uani 1 1 d . . . . .
H18A H 0.293150 0.298563 1.097332 0.107 Uiso 1 1 calc GR . . . .
H18B H 0.337090 0.380034 0.980861 0.107 Uiso 1 1 calc GR . . . .
H18C H 0.421134 0.259211 1.041441 0.107 Uiso 1 1 calc GR . . . .
C19 C 0.157(2) 0.2890(19) 0.9821(14) 0.071(2) Uani 1 1 d . . . . .
H19A H 0.124590 0.250636 0.950067 0.107 Uiso 1 1 calc GR . . . .
H19B H 0.143836 0.373181 0.940723 0.107 Uiso 1 1 calc GR . . . .
H19C H 0.119032 0.276022 1.054730 0.107 Uiso 1 1 calc GR . . . .
C20 C 0.3081(19) 0.103(2) 1.0556(15) 0.071(2) Uani 1 1 d . . . . .
H20A H 0.390674 0.070644 1.065908 0.107 Uiso 1 1 calc GR . . . .
H20B H 0.283422 0.061459 1.021606 0.107 Uiso 1 1 calc GR . . . .
H20C H 0.260515 0.095121 1.124337 0.107 Uiso 1 1 calc GR . . . .
C21 C 0.782(2) 0.223(2) 0.4338(17) 0.071(2) Uani 1 1 d . . . . .
H21 H 0.857695 0.215972 0.395219 0.086 Uiso 1 1 calc R . . . .
C22 C 0.724(2) 0.257(3) 0.275(2) 0.071(2) Uani 1 1 d . . . . .
C23 C 0.785(2) 0.339(2) 0.204(2) 0.071(2) Uani 1 1 d . . . . .
H23 H 0.812789 0.385710 0.227297 0.086 Uiso 1 1 calc R . . . .
C24 C 0.805(2) 0.351(2) 0.099(2) 0.071(2) Uani 1 1 d . . . . .
H24 H 0.844968 0.409122 0.048322 0.086 Uiso 1 1 calc R . . . .
C25 C 0.767(2) 0.279(3) 0.0676(19) 0.071(2) Uani 1 1 d . . . . .
H25 H 0.778640 0.289862 -0.005164 0.086 Uiso 1 1 calc R . . . .
C26 C 0.711(2) 0.191(3) 0.142(3) 0.071(2) Uani 1 1 d . . . . .
C27 C 0.676(2) 0.119(2) 0.1049(18) 0.071(2) Uani 1 1 d . . . . .
H27 H 0.693674 0.128114 0.032215 0.086 Uiso 1 1 calc R . . . .
C28 C 0.614(2) 0.033(2) 0.1751(19) 0.071(2) Uani 1 1 d . . . . .
H28 H 0.586546 -0.012990 0.150242 0.086 Uiso 1 1 calc R . . . .
C29 C 0.593(2) 0.018(2) 0.283(2) 0.071(2) Uani 1 1 d . . . . .
H29 H 0.559616 -0.045347 0.332114 0.086 Uiso 1 1 calc R . . . .
C30 C 0.619(2) 0.093(3) 0.3176(19) 0.071(2) Uani 1 1 d . . . . .
H30 H 0.593272 0.089428 0.388127 0.086 Uiso 1 1 calc R . . . .
C31 C 0.683(2) 0.171(3) 0.250(2) 0.071(2) Uani 1 1 d . . . . .
C32 C 0.288(2) 0.326(2) 0.5996(19) 0.071(2) Uani 1 1 d . . . . .
H32 H 0.206340 0.355390 0.614502 0.086 Uiso 1 1 calc R . . . .
C33 C 0.228(3) 0.354(3) 0.4427(19) 0.071(2) Uani 1 1 d . . . . .
C34 C 0.157(2) 0.463(2) 0.4176(16) 0.071(2) Uani 1 1 d . . . . .
H34 H 0.167784 0.517051 0.444285 0.086 Uiso 1 1 calc R . . . .
C35 C 0.069(2) 0.498(2) 0.3531(16) 0.071(2) Uani 1 1 d . . . . .
H35 H 0.020289 0.573853 0.337567 0.086 Uiso 1 1 calc R . . . .
C36 C 0.053(2) 0.422(3) 0.3117(16) 0.071(2) Uani 1 1 d . . . . .
H36 H -0.004702 0.443588 0.266464 0.086 Uiso 1 1 calc R . . . .
C37 C 0.131(3) 0.306(3) 0.3422(19) 0.071(2) Uani 1 1 d . . . . .
C38 C 0.118(2) 0.216(3) 0.3058(17) 0.071(2) Uani 1 1 d . . . . .
H38 H 0.058878 0.234173 0.262934 0.086 Uiso 1 1 calc R . . . .
C39 C 0.187(2) 0.113(2) 0.3325(16) 0.071(2) Uani 1 1 d . . . . .
H39 H 0.175160 0.058370 0.307899 0.086 Uiso 1 1 calc R . . . .
C40 C 0.275(2) 0.077(2) 0.3923(17) 0.071(2) Uani 1 1 d . . . . .
H40 H 0.323996 0.001104 0.405595 0.086 Uiso 1 1 calc R . . . .
C41 C 0.292(2) 0.152(3) 0.4341(16) 0.071(2) Uani 1 1 d . . . . .
H41 H 0.350192 0.128834 0.479639 0.086 Uiso 1 1 calc R . . . .
C42 C 0.219(3) 0.263(3) 0.4044(19) 0.071(2) Uani 1 1 d . . . . .
C43 C 0.451(2) 0.381(2) 0.2075(16) 0.071(2) Uani 1 1 d . . . . .
H43A H 0.428912 0.305765 0.226146 0.086 Uiso 1 1 calc R . . . .
H43B H 0.523707 0.383087 0.156943 0.086 Uiso 1 1 calc R . . . .
C44 C 0.352(2) 0.484(2) 0.1589(15) 0.071(2) Uani 1 1 d . . . . .
H44A H 0.274503 0.468677 0.194734 0.086 Uiso 1 1 calc R . . . .
H44B H 0.356207 0.501895 0.082255 0.086 Uiso 1 1 calc R . . . .
C45 C 0.379(2) 0.584(2) 0.1794(15) 0.071(2) Uani 1 1 d . . . . .
H45A H 0.425041 0.631778 0.116961 0.086 Uiso 1 1 calc R . . . .
H45B H 0.306217 0.636037 0.198383 0.086 Uiso 1 1 calc R . . . .
C46 C 0.448(2) 0.519(2) 0.2699(15) 0.071(2) Uani 1 1 d . . . . .
H46A H 0.524824 0.541603 0.250955 0.086 Uiso 1 1 calc R . . . .
H46B H 0.406475 0.540096 0.331623 0.086 Uiso 1 1 calc R . . . .
Li1 Li 0.503(4) 0.304(4) 0.440(3) 0.071(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C43 1.401(19) . ?
O1 C46 1.45(2) . ?
O1 Li1 1.92(4) . ?
N1 C11 1.38(2) . ?
N1 C12 1.38(3) . ?
N1 Li1 1.97(4) . ?
N2 C21 1.31(2) . ?
N2 C22 1.46(2) . ?
N2 Li1 2.25(5) . ?
N3 C32 1.27(2) . ?
N3 C33 1.44(3) . ?
N3 Li1 2.17(5) . ?
C1 C2 1.36(3) . ?
C1 C12 1.43(3) . ?
C1 C21 1.49(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.42(2) . ?
C3 C4 1.35(3) . ?
C3 C13 1.53(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.33(3) . ?
C5 C6 1.44(3) . ?
C5 C12 1.45(3) . ?
C6 C7 1.43(3) . ?
C6 C11 1.44(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.39(3) . ?
C8 C9 1.39(2) . ?
C8 C17 1.55(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.42(3) . ?
C10 C11 1.38(3) . ?
C10 C32 1.39(3) . ?
C13 C14 1.55(3) . ?
C13 C15 1.56(3) . ?
C13 C16 1.50(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.50(3) . ?
C17 C19 1.56(3) . ?
C17 C20 1.57(3) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21 0.9500 . ?
C22 C23 1.36(3) . ?
C22 C31 1.51(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.38(2) . ?
C24 H24 0.9500 . ?
C24 C25 1.38(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.41(3) . ?
C26 C27 1.41(3) . ?
C26 C31 1.40(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.41(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.40(2) . ?
C29 H29 0.9500 . ?
C29 C30 1.37(3) . ?
C30 H30 0.9500 . ?
C30 C31 1.35(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.36(3) . ?
C33 C42 1.51(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.40(3) . ?
C35 H35 0.9500 . ?
C35 C36 1.39(3) . ?
C36 H36 0.9500 . ?
C36 C37 1.46(3) . ?
C37 C38 1.49(3) . ?
C37 C42 1.36(3) . ?
C38 H38 0.9500 . ?
C38 C39 1.30(3) . ?
C39 H39 0.9500 . ?
C39 C40 1.35(3) . ?
C40 H40 0.9500 . ?
C40 C41 1.38(3) . ?
C41 H41 0.9500 . ?
C41 C42 1.40(3) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.53(3) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.55(3) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.49(2) . ?
C46 H46A 0.9900 . ?
C46 H46B 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
C43 O1 C46 104.4(15) . . ?
C43 O1 Li1 142(2) . . ?
C46 O1 Li1 114(2) . . ?
C11 N1 C12 106(2) . . ?
C11 N1 Li1 124(2) . . ?
C12 N1 Li1 128(2) . . ?
C21 N2 C22 113(2) . . ?
C21 N2 Li1 127(2) . . ?
C22 N2 Li1 117.5(19) . . ?
C32 N3 C33 116(2) . . ?
C32 N3 Li1 121(2) . . ?
C33 N3 Li1 121.3(19) . . ?
C2 C1 C12 120(3) . . ?
C2 C1 C21 117(3) . . ?
C12 C1 C21 121(3) . . ?
C1 C2 H2 119.7 . . ?
C1 C2 C3 121(3) . . ?
C3 C2 H2 119.7 . . ?
C2 C3 C13 118(3) . . ?
C4 C3 C2 122(3) . . ?
C4 C3 C13 120(3) . . ?
C3 C4 H4 121.5 . . ?
C5 C4 C3 117(3) . . ?
C5 C4 H4 121.5 . . ?
C4 C5 C6 136(3) . . ?
C4 C5 C12 125(3) . . ?
C6 C5 C12 99(3) . . ?
C7 C6 C5 132(3) . . ?
C7 C6 C11 116(3) . . ?
C11 C6 C5 112(3) . . ?
C6 C7 H7 118.9 . . ?
C8 C7 C6 122(3) . . ?
C8 C7 H7 118.9 . . ?
C7 C8 C9 119(3) . . ?
C7 C8 C17 121(2) . . ?
C9 C8 C17 120(3) . . ?
C8 C9 H9 118.6 . . ?
C8 C9 C10 123(3) . . ?
C10 C9 H9 118.6 . . ?
C11 C10 C9 117(3) . . ?
C11 C10 C32 122(3) . . ?
C32 C10 C9 121(3) . . ?
N1 C11 C6 107(3) . . ?
N1 C11 C10 129(3) . . ?
C10 C11 C6 123(3) . . ?
N1 C12 C1 128(3) . . ?
N1 C12 C5 115(3) . . ?
C1 C12 C5 115(3) . . ?
C3 C13 C14 110(2) . . ?
C3 C13 C15 111(2) . . ?
C14 C13 C15 105.1(18) . . ?
C16 C13 C3 118(2) . . ?
C16 C13 C14 105(2) . . ?
C16 C13 C15 108(2) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C8 C17 C19 113(2) . . ?
C8 C17 C20 108(2) . . ?
C18 C17 C8 110(2) . . ?
C18 C17 C19 109(2) . . ?
C18 C17 C20 109.6(18) . . ?
C19 C17 C20 108(2) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N2 C21 C1 123(3) . . ?
N2 C21 H21 118.3 . . ?
C1 C21 H21 118.3 . . ?
N2 C22 C31 110(3) . . ?
C23 C22 N2 124(3) . . ?
C23 C22 C31 126(3) . . ?
C22 C23 H23 120.4 . . ?
C22 C23 C24 119(3) . . ?
C24 C23 H23 120.4 . . ?
C23 C24 H24 120.3 . . ?
C25 C24 C23 119(3) . . ?
C25 C24 H24 120.3 . . ?
C24 C25 H25 119.4 . . ?
C24 C25 C26 121(3) . . ?
C26 C25 H25 119.4 . . ?
C25 C26 C27 118(3) . . ?
C31 C26 C25 125(3) . . ?
C31 C26 C27 117(3) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 C26 120(3) . . ?
C28 C27 H27 119.8 . . ?
C27 C28 H28 120.8 . . ?
C29 C28 C27 118(3) . . ?
C29 C28 H28 120.8 . . ?
C28 C29 H29 119.3 . . ?
C30 C29 C28 121(3) . . ?
C30 C29 H29 119.3 . . ?
C29 C30 H30 120.5 . . ?
C31 C30 C29 119(3) . . ?
C31 C30 H30 120.5 . . ?
C26 C31 C22 109(3) . . ?
C30 C31 C22 127(3) . . ?
C30 C31 C26 123(3) . . ?
N3 C32 C10 130(3) . . ?
N3 C32 H32 114.8 . . ?
C10 C32 H32 114.8 . . ?
N3 C33 C42 116(3) . . ?
C34 C33 N3 120(3) . . ?
C34 C33 C42 123(3) . . ?
C33 C34 H34 119.4 . . ?
C33 C34 C35 121(3) . . ?
C35 C34 H34 119.4 . . ?
C34 C35 H35 119.7 . . ?
C36 C35 C34 121(3) . . ?
C36 C35 H35 119.7 . . ?
C35 C36 H36 122.2 . . ?
C35 C36 C37 116(3) . . ?
C37 C36 H36 122.2 . . ?
C36 C37 C38 120(3) . . ?
C42 C37 C36 129(3) . . ?
C42 C37 C38 111(3) . . ?
C37 C38 H38 119.9 . . ?
C39 C38 C37 120(3) . . ?
C39 C38 H38 119.9 . . ?
C38 C39 H39 117.2 . . ?
C38 C39 C40 126(3) . . ?
C40 C39 H39 117.2 . . ?
C39 C40 H40 120.3 . . ?
C39 C40 C41 119(3) . . ?
C41 C40 H40 120.3 . . ?
C40 C41 H41 122.5 . . ?
C40 C41 C42 115(3) . . ?
C42 C41 H41 122.5 . . ?
C37 C42 C33 111(3) . . ?
C37 C42 C41 128(3) . . ?
C41 C42 C33 121(3) . . ?
O1 C43 H43A 110.5 . . ?
O1 C43 H43B 110.5 . . ?
O1 C43 C44 106.1(19) . . ?
H43A C43 H43B 108.7 . . ?
C44 C43 H43A 110.5 . . ?
C44 C43 H43B 110.5 . . ?
C43 C44 H44A 111.4 . . ?
C43 C44 H44B 111.4 . . ?
C43 C44 C45 102(2) . . ?
H44A C44 H44B 109.3 . . ?
C45 C44 H44A 111.4 . . ?
C45 C44 H44B 111.4 . . ?
C44 C45 H45A 111.3 . . ?
C44 C45 H45B 111.3 . . ?
H45A C45 H45B 109.2 . . ?
C46 C45 C44 102(2) . . ?
C46 C45 H45A 111.3 . . ?
C46 C45 H45B 111.3 . . ?
O1 C46 C45 111(2) . . ?
O1 C46 H46A 109.3 . . ?
O1 C46 H46B 109.3 . . ?
C45 C46 H46A 109.3 . . ?
C45 C46 H46B 109.3 . . ?
H46A C46 H46B 108.0 . . ?
O1 Li1 N1 160(3) . . ?
O1 Li1 N2 92.7(18) . . ?
O1 Li1 N3 93.6(19) . . ?
N1 Li1 N2 87.5(19) . . ?
N1 Li1 N3 90.5(18) . . ?
N3 Li1 N2 167(3) . . ?

_olex2_exptl_crystal_mounting_method "'in fomblin film on a micromount"
# This is the default assumed mounting details'
_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 2.633
_oxdiff_exptl_absorpt_empirical_full_min 0.592
