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

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

data_dibaclc
_database_code_depnum_ccdc_archive 'CCDC 1994134'
loop_
_audit_author_name
_audit_author_address
'PROFESSOR J D WALLIS'
;Nottingham Trent University, UK
United Kingdom
;
_audit_update_record             
;
2020-04-01 deposited with the CCDC.	2020-05-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
methyl 2,6-diaminobenzoate
;
_chemical_name_common            ?
_chemical_melting_point          352-354
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H10 N2 O2'
_chemical_formula_weight         166.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   5.4015(6)
_cell_length_b                   11.0987(11)
_cell_length_c                   13.6141(17)
_cell_angle_alpha                90
_cell_angle_beta                 97.202(12)
_cell_angle_gamma                90
_cell_volume                     809.72(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1468
_cell_measurement_theta_min      3.5410
_cell_measurement_theta_max      29.2190


_exptl_crystal_description       'thick plate'
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_F_000             352
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_exptl_crystal_size_max          0.3349
_exptl_crystal_size_mid          0.1509
_exptl_crystal_size_min          0.1331
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_min  0.978
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_ambient_environment      N~2~
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_detector_area_resol_mean 15.9832
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            3599
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.016
_diffrn_reflns_theta_max         29.380
_diffrn_reflns_theta_full        27.000
_diffrn_measured_fraction_theta_max 0.840
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             1884
_reflns_number_gt                1556
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0500P)²+0.2298P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1884
_refine_ls_number_parameters     149
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.1101
_refine_ls_wR_factor_gt          0.1038
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.6305(2) 0.85961(10) 0.40619(7) 0.0261(3) Uani 1 1 d . . . . .
O2 O 0.47391(18) 0.71826(9) 0.30056(7) 0.0211(3) Uani 1 1 d . . . . .
N1 N 1.0030(3) 0.99212(13) 0.36488(10) 0.0298(3) Uani 1 1 d . . . . .
N2 N 0.5955(2) 0.70416(11) 0.12071(9) 0.0205(3) Uani 1 1 d . . . . .
C1 C 0.7853(2) 0.84599(12) 0.24964(9) 0.0169(3) Uani 1 1 d . . . . .
C2 C 0.9744(3) 0.93459(13) 0.27573(10) 0.0198(3) Uani 1 1 d . . . . .
C3 C 1.1405(3) 0.96482(14) 0.20807(11) 0.0225(3) Uani 1 1 d . . . . .
C4 C 1.1155(3) 0.91268(14) 0.11590(11) 0.0237(3) Uani 1 1 d . . . . .
C5 C 0.9313(3) 0.82894(14) 0.08740(10) 0.0228(3) Uani 1 1 d . . . . .
C6 C 0.7650(2) 0.79305(12) 0.15262(9) 0.0170(3) Uani 1 1 d . . . . .
C7 C 0.6267(2) 0.81212(12) 0.32497(9) 0.0172(3) Uani 1 1 d . . . . .
C8 C 0.3281(3) 0.67899(16) 0.37623(11) 0.0264(4) Uani 1 1 d . . . . .
H82 H 0.445(3) 0.6485(15) 0.4327(13) 0.028(4) Uiso 1 1 d . . . . .
H21 H 0.463(3) 0.6932(16) 0.1539(13) 0.031(5) Uiso 1 1 d . . . . .
H11 H 0.895(4) 0.9782(17) 0.4060(14) 0.038(5) Uiso 1 1 d . . . . .
H5 H 0.916(3) 0.7930(15) 0.0224(13) 0.031(5) Uiso 1 1 d . . . . .
H4 H 1.229(3) 0.9325(15) 0.0705(12) 0.026(4) Uiso 1 1 d . . . . .
H3 H 1.262(3) 1.0235(16) 0.2261(11) 0.023(4) Uiso 1 1 d . . . . .
H83 H 0.222(3) 0.6198(17) 0.3463(13) 0.034(5) Uiso 1 1 d . . . . .
H22 H 0.575(3) 0.6936(15) 0.0546(13) 0.025(4) Uiso 1 1 d . . . . .
H81 H 0.228(3) 0.7473(16) 0.3963(13) 0.030(4) Uiso 1 1 d . . . . .
H12 H 1.117(3) 1.0438(16) 0.3739(13) 0.030(5) Uiso 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 C7 1.2229(16) . ?
O2 C7 1.3448(16) . ?
O2 C8 1.4404(17) . ?
N1 C2 1.3629(19) . ?
N1 H11 0.87(2) . ?
N1 H12 0.837(19) . ?
N2 C6 1.3786(18) . ?
N2 H21 0.901(18) . ?
N2 H22 0.900(17) . ?
C1 C2 1.430(2) . ?
C1 C6 1.4372(18) . ?
C1 C7 1.4652(18) . ?
C2 C3 1.4044(19) . ?
C3 C4 1.373(2) . ?
C3 H3 0.935(17) . ?
C4 C5 1.381(2) . ?
C4 H4 0.949(17) . ?
C5 C6 1.3979(19) . ?
C5 H5 0.964(17) . ?
C8 H82 0.991(17) . ?
C8 H83 0.930(19) . ?
C8 H81 0.990(18) . ?

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
C7 O2 C8 115.55(11) . . ?
C2 N1 H11 118.5(12) . . ?
C2 N1 H12 116.8(12) . . ?
H11 N1 H12 124.4(17) . . ?
C6 N2 H21 118.4(11) . . ?
C6 N2 H22 113.8(11) . . ?
H21 N2 H22 118.4(15) . . ?
C2 C1 C6 118.63(12) . . ?
C2 C1 C7 117.68(12) . . ?
C6 C1 C7 123.66(13) . . ?
N1 C2 C3 117.50(14) . . ?
N1 C2 C1 122.74(13) . . ?
C3 C2 C1 119.75(13) . . ?
C4 C3 C2 120.08(14) . . ?
C4 C3 H3 121.2(10) . . ?
C2 C3 H3 118.6(10) . . ?
C3 C4 C5 121.67(13) . . ?
C3 C4 H4 120.0(10) . . ?
C5 C4 H4 118.3(10) . . ?
C4 C5 C6 120.73(13) . . ?
C4 C5 H5 120.9(10) . . ?
C6 C5 H5 118.4(10) . . ?
N2 C6 C5 117.26(12) . . ?
N2 C6 C1 123.60(12) . . ?
C5 C6 C1 119.09(13) . . ?
O1 C7 O2 119.84(12) . . ?
O1 C7 C1 125.26(13) . . ?
O2 C7 C1 114.86(11) . . ?
O2 C8 H82 107.8(10) . . ?
O2 C8 H83 105.1(11) . . ?
H82 C8 H83 113.3(15) . . ?
O2 C8 H81 109.4(10) . . ?
H82 C8 H81 111.4(14) . . ?
H83 C8 H81 109.5(15) . . ?

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
C6 C1 C2 N1 178.05(13) . . . . ?
C7 C1 C2 N1 -3.5(2) . . . . ?
C6 C1 C2 C3 -2.2(2) . . . . ?
C7 C1 C2 C3 176.28(12) . . . . ?
N1 C2 C3 C4 -177.88(14) . . . . ?
C1 C2 C3 C4 2.3(2) . . . . ?
C2 C3 C4 C5 -0.8(2) . . . . ?
C3 C4 C5 C6 -0.9(2) . . . . ?
C4 C5 C6 N2 -176.41(13) . . . . ?
C4 C5 C6 C1 1.0(2) . . . . ?
C2 C1 C6 N2 177.78(12) . . . . ?
C7 C1 C6 N2 -0.6(2) . . . . ?
C2 C1 C6 C5 0.52(19) . . . . ?
C7 C1 C6 C5 -177.84(13) . . . . ?
C8 O2 C7 O1 -1.59(19) . . . . ?
C8 O2 C7 C1 176.26(12) . . . . ?
C2 C1 C7 O1 5.6(2) . . . . ?
C6 C1 C7 O1 -176.02(13) . . . . ?
C2 C1 C7 O2 -172.11(11) . . . . ?
C6 C1 C7 O2 6.27(19) . . . . ?

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
N2 H21 O2 0.901(18) 2.009(18) 2.6180(15) 123.6(15) .
N1 H11 O1 0.87(2) 1.94(2) 2.6098(18) 132.3(16) .
C3 H3 O2 0.935(17) 2.640(17) 3.5108(18) 155.2(13) 2_755
N2 H22 O1 0.900(17) 2.163(17) 3.0339(15) 162.7(15) 4_575
N1 H12 N2 0.837(19) 2.359(19) 3.1896(19) 171.6(16) 2_755

_refine_diff_density_max         0.344
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.043

_shelxl_version_number           2014-3

_exptl_crystal_recrystallization_method 
'Slow crystallisation from oil under nitrogen'
_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# 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_fabs150MXA
_database_code_depnum_ccdc_archive 'CCDC 1994137'
loop_
_audit_author_name
_audit_author_address
'PROFESSOR J D WALLIS'
;Nottingham Trent University, UK
United Kingdom
;
_audit_update_record             
;
2020-04-01 deposited with the CCDC.	2020-05-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
Methyl 2-tosylamino-6-aminobenzoate
;
_chemical_name_common            ?
_chemical_melting_point          424-426
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H16 N2 O4 S'
_chemical_formula_weight         320.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   9.7212(3)
_cell_length_b                   35.4733(12)
_cell_length_c                   26.2238(10)
_cell_angle_alpha                90
_cell_angle_beta                 97.360(3)
_cell_angle_gamma                90
_cell_volume                     8968.6(5)
_cell_formula_units_Z            24
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9346
_cell_measurement_theta_min      3.5280
_cell_measurement_theta_max      29.9900


_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_F_000             4032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.441
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.043
_exptl_absorpt_coefficient_mu    0.236
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
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_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_detector_area_resol_mean 15.9832
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            56001
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         3.271
_diffrn_reflns_theta_max         30.963
_diffrn_reflns_theta_full        28.500
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             24833
_reflns_number_gt                14496
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0623P)²+0.3682P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         24833
_refine_ls_number_parameters     1273
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1213
_refine_ls_R_factor_gt           0.0625
_refine_ls_wR_factor_ref         0.1580
_refine_ls_wR_factor_gt          0.1317
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1A S 0.20668(6) 0.51047(2) 0.88514(2) 0.02620(13) Uani 1 1 d . . . . .
O1A O -0.01808(16) 0.56132(4) 0.78245(6) 0.0302(4) Uani 1 1 d . . . . .
O2A O -0.24499(16) 0.57104(4) 0.77182(5) 0.0278(4) Uani 1 1 d . . . . .
O3A O 0.32316(16) 0.52485(5) 0.86294(6) 0.0372(4) Uani 1 1 d . . . . .
O4A O 0.22255(17) 0.47678(5) 0.91516(6) 0.0354(4) Uani 1 1 d . . . . .
N1A N 0.08672(19) 0.50374(6) 0.83608(7) 0.0243(4) Uani 1 1 d . . . . .
N2A N -0.4154(2) 0.52875(6) 0.81451(8) 0.0307(5) Uani 1 1 d . . . . .
C1A C -0.1629(2) 0.51910(6) 0.82319(7) 0.0209(4) Uani 1 1 d . . . . .
C2A C -0.0520(2) 0.49548(6) 0.84443(7) 0.0218(5) Uani 1 1 d . . . . .
C3A C -0.0747(3) 0.46411(6) 0.87312(8) 0.0294(5) Uani 1 1 d . . . . .
H3A H 0.0001 0.4479 0.8852 0.035 Uiso 1 1 calc R U . . .
C4A C -0.2076(3) 0.45635(7) 0.88426(8) 0.0323(6) Uani 1 1 d . . . . .
H4A H -0.2227 0.4353 0.9053 0.039 Uiso 1 1 calc R U . . .
C5A C -0.3168(2) 0.47858(6) 0.86531(8) 0.0294(5) Uani 1 1 d . . . . .
H5A H -0.4068 0.4728 0.8735 0.035 Uiso 1 1 calc R U . . .
C6A C -0.2991(2) 0.50992(6) 0.83380(8) 0.0236(5) Uani 1 1 d . . . . .
C7A C -0.1330(2) 0.55174(6) 0.79136(7) 0.0209(4) Uani 1 1 d . . . . .
C8A C -0.2225(2) 0.60324(6) 0.74033(8) 0.0281(5) Uani 1 1 d . . . . .
H84A H -0.1566 0.5966 0.7165 0.042 Uiso 1 1 calc R U . . .
H83A H -0.1850 0.6241 0.7623 0.042 Uiso 1 1 calc R U . . .
H82A H -0.3108 0.6109 0.7208 0.042 Uiso 1 1 calc R U . . .
C9A C 0.1429(2) 0.54582(6) 0.92248(8) 0.0251(5) Uani 1 1 d . . . . .
C10A C 0.0568(3) 0.53576(7) 0.95835(9) 0.0361(6) Uani 1 1 d . . . . .
H10A H 0.0380 0.5099 0.9641 0.043 Uiso 1 1 calc R U . . .
C11A C -0.0015(3) 0.56345(7) 0.98569(9) 0.0367(6) Uani 1 1 d . . . . .
H11A H -0.0615 0.5564 1.0099 0.044 Uiso 1 1 calc R U . . .
C12A C 0.0259(3) 0.60120(7) 0.97843(8) 0.0313(6) Uani 1 1 d . . . . .
C13A C 0.1121(3) 0.61054(7) 0.94211(9) 0.0397(6) Uani 1 1 d . . . . .
H13A H 0.1315 0.6363 0.9363 0.048 Uiso 1 1 calc R U . . .
C14A C 0.1706(3) 0.58316(7) 0.91410(9) 0.0341(6) Uani 1 1 d . . . . .
H14A H 0.2292 0.5901 0.8893 0.041 Uiso 1 1 calc R U . . .
C15A C -0.0375(3) 0.63080(7) 1.00855(9) 0.0441(7) Uani 1 1 d . . . . .
H52A H -0.1165 0.6201 1.0233 0.066 Uiso 1 1 calc R U . . .
H53A H -0.0693 0.6518 0.9858 0.066 Uiso 1 1 calc R U . . .
H51A H 0.0318 0.6399 1.0363 0.066 Uiso 1 1 calc R U . . .
H1A H 0.094(3) 0.5219(8) 0.8176(10) 0.050(9) Uiso 1 1 d . . . . .
H21A H -0.407(3) 0.5497(7) 0.7999(9) 0.043(8) Uiso 1 1 d . . . . .
H22A H -0.487(3) 0.5242(7) 0.8295(9) 0.031(7) Uiso 1 1 d . . . . .
S1B S 0.70317(6) 0.66448(2) 0.87916(2) 0.02792(14) Uani 1 1 d . . . . .
O1B O 0.48071(16) 0.61021(4) 0.77900(6) 0.0312(4) Uani 1 1 d . . . . .
O2B O 0.25460(16) 0.59912(4) 0.77105(6) 0.0276(4) Uani 1 1 d . . . . .
O3B O 0.81996(16) 0.64892(5) 0.85849(6) 0.0394(4) Uani 1 1 d . . . . .
O4B O 0.71807(17) 0.69941(5) 0.90649(6) 0.0382(4) Uani 1 1 d . . . . .
N1B N 0.5841(2) 0.66946(6) 0.82927(7) 0.0262(4) Uani 1 1 d . . . . .
N2B N 0.0817(2) 0.64403(6) 0.80857(8) 0.0306(5) Uani 1 1 d . . . . .
C1B C 0.3347(2) 0.65390(6) 0.81676(7) 0.0218(5) Uani 1 1 d . . . . .
C2B C 0.4454(2) 0.67834(6) 0.83637(7) 0.0230(5) Uani 1 1 d . . . . .
C3B C 0.4213(3) 0.71095(6) 0.86256(8) 0.0302(5) Uani 1 1 d . . . . .
H3B H 0.4957 0.7276 0.8737 0.036 Uiso 1 1 calc R U . . .
C4B C 0.2879(3) 0.71927(7) 0.87257(9) 0.0328(6) Uani 1 1 d . . . . .
H4B H 0.2719 0.7411 0.8918 0.039 Uiso 1 1 calc R U . . .
C5B C 0.1791(2) 0.69619(6) 0.85488(8) 0.0307(5) Uani 1 1 d . . . . .
H5B H 0.0886 0.7024 0.8622 0.037 Uiso 1 1 calc R U . . .
C6B C 0.1982(2) 0.66362(6) 0.82618(8) 0.0235(5) Uani 1 1 d . . . . .
C7B C 0.3657(2) 0.61982(6) 0.78791(7) 0.0221(5) Uani 1 1 d . . . . .
C8B C 0.2785(2) 0.56551(6) 0.74213(8) 0.0291(5) Uani 1 1 d . . . . .
H83B H 0.3435 0.5713 0.7176 0.044 Uiso 1 1 calc R U . . .
H82B H 0.1905 0.5568 0.7235 0.044 Uiso 1 1 calc R U . . .
H81B H 0.3177 0.5457 0.7658 0.044 Uiso 1 1 calc R U . . .
C9B C 0.6384(2) 0.63114(6) 0.91907(8) 0.0251(5) Uani 1 1 d . . . . .
C10B C 0.5455(3) 0.64261(7) 0.95177(9) 0.0361(6) Uani 1 1 d . . . . .
H10B H 0.5209 0.6685 0.9535 0.043 Uiso 1 1 calc R U . . .
C11B C 0.4886(3) 0.61627(7) 0.98183(9) 0.0384(6) Uani 1 1 d . . . . .
H11B H 0.4242 0.6243 1.0040 0.046 Uiso 1 1 calc R U . . .
C12B C 0.5236(3) 0.57857(7) 0.98035(8) 0.0316(6) Uani 1 1 d . . . . .
C13B C 0.6170(3) 0.56777(7) 0.94716(9) 0.0400(6) Uani 1 1 d . . . . .
H13B H 0.6425 0.5420 0.9456 0.048 Uiso 1 1 calc R U . . .
C14B C 0.6734(3) 0.59353(7) 0.91650(9) 0.0353(6) Uani 1 1 d . . . . .
H14B H 0.7360 0.5855 0.8937 0.042 Uiso 1 1 calc R U . . .
C15B C 0.4611(3) 0.55075(8) 1.01349(10) 0.0445(7) Uani 1 1 d . . . . .
H53B H 0.4216 0.5297 0.9923 0.067 Uiso 1 1 calc R U . . .
H51B H 0.3879 0.5630 1.0299 0.067 Uiso 1 1 calc R U . . .
H52B H 0.5330 0.5413 1.0400 0.067 Uiso 1 1 calc R U . . .
H1B H 0.590(3) 0.6500(7) 0.8124(9) 0.041(8) Uiso 1 1 d . . . . .
H21B H 0.091(3) 0.6230(8) 0.7933(10) 0.048(9) Uiso 1 1 d . . . . .
H22B H 0.011(3) 0.6478(7) 0.8232(9) 0.037(8) Uiso 1 1 d . . . . .
S1C S 0.30136(6) 0.82161(2) 0.61657(2) 0.02953(14) Uani 1 1 d . . . . .
O1C O 0.53004(16) 0.77563(4) 0.72428(6) 0.0309(4) Uani 1 1 d . . . . .
O2C O 0.75767(16) 0.76717(4) 0.73650(6) 0.0288(4) Uani 1 1 d . . . . .
O3C O 0.18571(16) 0.80786(5) 0.63977(6) 0.0406(4) Uani 1 1 d . . . . .
O4C O 0.28509(17) 0.85462(5) 0.58501(6) 0.0390(4) Uani 1 1 d . . . . .
N1C N 0.4219(2) 0.82953(6) 0.66477(7) 0.0278(4) Uani 1 1 d . . . . .
N2C N 0.9271(2) 0.80914(6) 0.69219(8) 0.0298(5) Uani 1 1 d . . . . .
C1C C 0.6730(2) 0.81666(6) 0.68091(7) 0.0215(4) Uani 1 1 d . . . . .
C2C C 0.5602(2) 0.83862(6) 0.65684(8) 0.0246(5) Uani 1 1 d . . . . .
C3C C 0.5812(3) 0.86891(7) 0.62602(8) 0.0311(5) Uani 1 1 d . . . . .
H3C H 0.5050 0.8841 0.6121 0.037 Uiso 1 1 calc R U . . .
C4C C 0.7137(3) 0.87713(7) 0.61542(8) 0.0332(6) Uani 1 1 d . . . . .
H4C H 0.7277 0.8974 0.5929 0.040 Uiso 1 1 calc R U . . .
C5C C 0.8248(2) 0.85643(6) 0.63697(8) 0.0303(5) Uani 1 1 d . . . . .
H5C H 0.9148 0.8624 0.6289 0.036 Uiso 1 1 calc R U . . .
C6C C 0.8090(2) 0.82645(6) 0.67078(8) 0.0231(5) Uani 1 1 d . . . . .
C7C C 0.6446(2) 0.78526(6) 0.71506(8) 0.0226(5) Uani 1 1 d . . . . .
C8C C 0.7351(3) 0.73573(6) 0.76962(8) 0.0316(5) Uani 1 1 d . . . . .
H83C H 0.6945 0.7146 0.7487 0.047 Uiso 1 1 calc R U . . .
H82C H 0.6716 0.7434 0.7939 0.047 Uiso 1 1 calc R U . . .
H81C H 0.8238 0.7279 0.7887 0.047 Uiso 1 1 calc R U . . .
C9C C 0.3622(2) 0.78520(6) 0.57988(8) 0.0276(5) Uani 1 1 d . . . . .
C10C C 0.4594(3) 0.79317(7) 0.54734(9) 0.0435(7) Uani 1 1 d . . . . .
H10C H 0.4920 0.8182 0.5446 0.052 Uiso 1 1 calc R U . . .
C11C C 0.5094(3) 0.76458(8) 0.51864(10) 0.0453(7) Uani 1 1 d . . . . .
H11C H 0.5774 0.7702 0.4968 0.054 Uiso 1 1 calc R U . . .
C12C C 0.4622(3) 0.72832(7) 0.52128(9) 0.0354(6) Uani 1 1 d . . . . .
C13C C 0.3669(3) 0.72057(7) 0.55494(10) 0.0439(7) Uani 1 1 d . . . . .
H13C H 0.3354 0.6954 0.5580 0.053 Uiso 1 1 calc R U . . .
C14C C 0.3165(3) 0.74853(7) 0.58413(9) 0.0375(6) Uani 1 1 d . . . . .
H14C H 0.2512 0.7426 0.6069 0.045 Uiso 1 1 calc R U . . .
C15C C 0.5150(3) 0.69811(8) 0.48888(10) 0.0507(8) Uani 1 1 d . . . . .
H51C H 0.4397 0.6896 0.4629 0.076 Uiso 1 1 calc R U . . .
H52C H 0.5487 0.6768 0.5107 0.076 Uiso 1 1 calc R U . . .
H53C H 0.5910 0.7081 0.4718 0.076 Uiso 1 1 calc R U . . .
H1C H 0.420(3) 0.8124(7) 0.6847(8) 0.031(7) Uiso 1 1 d . . . . .
H21C H 0.919(3) 0.7893(8) 0.7112(9) 0.046(8) Uiso 1 1 d . . . . .
H22C H 1.002(3) 0.8151(8) 0.6797(10) 0.052(9) Uiso 1 1 d . . . . .
S1D S 0.79495(6) 0.67360(2) 0.63242(2) 0.02883(14) Uani 1 1 d . . . . .
O1D O 1.02909(16) 0.73063(4) 0.72975(6) 0.0309(4) Uani 1 1 d . . . . .
O2D O 1.25555(16) 0.74076(4) 0.73746(6) 0.0294(4) Uani 1 1 d . . . . .
O3D O 0.68688(16) 0.69327(5) 0.65356(6) 0.0415(5) Uani 1 1 d . . . . .
O4D O 0.76842(18) 0.63664(5) 0.61206(6) 0.0419(5) Uani 1 1 d . . . . .
N2D N 1.4250(2) 0.69521(6) 0.69957(9) 0.0322(5) Uani 1 1 d . . . . .
N1D N 0.9222(2) 0.67215(6) 0.67970(7) 0.0262(4) Uani 1 1 d . . . . .
C1D C 1.1723(2) 0.68640(6) 0.69134(7) 0.0213(4) Uani 1 1 d . . . . .
C2D C 1.0596(2) 0.66257(6) 0.67162(7) 0.0225(5) Uani 1 1 d . . . . .
C3D C 1.0815(3) 0.62991(6) 0.64526(8) 0.0295(5) Uani 1 1 d . . . . .
H3D H 1.0059 0.6138 0.6335 0.035 Uiso 1 1 calc R U . . .
C4D C 1.2148(3) 0.62076(6) 0.63607(8) 0.0313(6) Uani 1 1 d . . . . .
H4D H 1.2297 0.5985 0.6173 0.038 Uiso 1 1 calc R U . . .
C5D C 1.3250(2) 0.64319(6) 0.65355(8) 0.0292(5) Uani 1 1 d . . . . .
H5D H 1.4151 0.6365 0.6463 0.035 Uiso 1 1 calc R U . . .
C6D C 1.3079(2) 0.67603(6) 0.68211(8) 0.0240(5) Uani 1 1 d . . . . .
C7D C 1.1435(2) 0.72050(6) 0.72042(8) 0.0222(5) Uani 1 1 d . . . . .
C8D C 1.2346(3) 0.77458(6) 0.76598(8) 0.0316(5) Uani 1 1 d . . . . .
H83D H 1.1980 0.7945 0.7421 0.047 Uiso 1 1 calc R U . . .
H82D H 1.3232 0.7827 0.7848 0.047 Uiso 1 1 calc R U . . .
H81D H 1.1684 0.7695 0.7903 0.047 Uiso 1 1 calc R U . . .
C9D C 0.8545(2) 0.70135(6) 0.58437(8) 0.0246(5) Uani 1 1 d . . . . .
C10D C 0.8862(3) 0.68478(7) 0.54016(8) 0.0371(6) Uani 1 1 d . . . . .
H10D H 0.8702 0.6586 0.5343 0.045 Uiso 1 1 calc R U . . .
C11D C 0.9416(3) 0.70656(7) 0.50430(9) 0.0406(7) Uani 1 1 d . . . . .
H11D H 0.9626 0.6951 0.4734 0.049 Uiso 1 1 calc R U . . .
C12D C 0.9676(3) 0.74457(7) 0.51203(9) 0.0339(6) Uani 1 1 d . . . . .
C13D C 0.9326(3) 0.76055(7) 0.55658(9) 0.0424(7) Uani 1 1 d . . . . .
H13D H 0.9480 0.7867 0.5625 0.051 Uiso 1 1 calc R U . . .
C14D C 0.8760(3) 0.73946(7) 0.59268(9) 0.0380(6) Uani 1 1 d . . . . .
H14D H 0.8520 0.7510 0.6230 0.046 Uiso 1 1 calc R U . . .
C15D C 1.0348(3) 0.76712(8) 0.47350(9) 0.0467(7) Uani 1 1 d . . . . .
H51D H 1.0894 0.7503 0.4543 0.070 Uiso 1 1 calc R U . . .
H53D H 1.0959 0.7862 0.4915 0.070 Uiso 1 1 calc R U . . .
H52D H 0.9631 0.7796 0.4497 0.070 Uiso 1 1 calc R U . . .
H1D H 0.917(3) 0.6908(7) 0.6960(9) 0.035(8) Uiso 1 1 d . . . . .
H21D H 1.417(3) 0.7169(7) 0.7120(9) 0.039(8) Uiso 1 1 d . . . . .
H22D H 1.499(3) 0.6910(7) 0.6843(9) 0.035(7) Uiso 1 1 d . . . . .
S1E S -0.19360(6) 0.34958(2) 0.63602(2) 0.02977(14) Uani 1 1 d . . . . .
O1E O 0.05123(16) 0.39780(4) 0.74084(6) 0.0302(4) Uani 1 1 d . . . . .
O2E O 0.27929(16) 0.40492(4) 0.75185(5) 0.0273(4) Uani 1 1 d . . . . .
O3E O -0.29673(16) 0.36937(5) 0.66016(6) 0.0405(4) Uani 1 1 d . . . . .
O4E O -0.22895(18) 0.31383(5) 0.61365(6) 0.0448(5) Uani 1 1 d . . . . .
N1E N -0.0634(2) 0.34561(6) 0.68139(7) 0.0282(5) Uani 1 1 d . . . . .
N2E N 0.4423(2) 0.36131(6) 0.70734(8) 0.0289(5) Uani 1 1 d . . . . .
C1E C 0.1885(2) 0.35601(6) 0.69627(7) 0.0220(5) Uani 1 1 d . . . . .
C2E C 0.0720(2) 0.33536(6) 0.67146(8) 0.0243(5) Uani 1 1 d . . . . .
C3E C 0.0892(3) 0.30589(6) 0.63907(8) 0.0319(6) Uani 1 1 d . . . . .
H3E H 0.0110 0.2919 0.6241 0.038 Uiso 1 1 calc R U . . .
C4E C 0.2206(3) 0.29660(7) 0.62819(8) 0.0353(6) Uani 1 1 d . . . . .
H4E H 0.2316 0.2765 0.6051 0.042 Uiso 1 1 calc R U . . .
C5E C 0.3351(3) 0.31590(6) 0.65032(8) 0.0311(5) Uani 1 1 d . . . . .
H5E H 0.4242 0.3092 0.6420 0.037 Uiso 1 1 calc R U . . .
C6E C 0.3223(2) 0.34540(6) 0.68511(8) 0.0240(5) Uani 1 1 d . . . . .
C7E C 0.1650(2) 0.38742(6) 0.73082(8) 0.0229(5) Uani 1 1 d . . . . .
C8E C 0.2602(3) 0.43717(6) 0.78392(8) 0.0306(5) Uani 1 1 d . . . . .
H82E H 0.2208 0.4581 0.7624 0.046 Uiso 1 1 calc R U . . .
H83E H 0.3499 0.4448 0.8024 0.046 Uiso 1 1 calc R U . . .
H81E H 0.1969 0.4305 0.8087 0.046 Uiso 1 1 calc R U . . .
C9E C -0.1377(2) 0.37827(6) 0.58826(8) 0.0251(5) Uani 1 1 d . . . . .
C10E C -0.1453(3) 0.36516(7) 0.53877(8) 0.0351(6) Uani 1 1 d . . . . .
H10E H -0.1826 0.3409 0.5303 0.042 Uiso 1 1 calc R U . . .
C11E C -0.0989(3) 0.38730(8) 0.50155(9) 0.0389(6) Uani 1 1 d . . . . .
H11E H -0.1050 0.3781 0.4673 0.047 Uiso 1 1 calc R U . . .
C12E C -0.0431(3) 0.42286(8) 0.51267(9) 0.0370(6) Uani 1 1 d . . . . .
C13E C -0.0369(3) 0.43509(8) 0.56257(10) 0.0516(8) Uani 1 1 d . . . . .
H13E H 0.0011 0.4593 0.5713 0.062 Uiso 1 1 calc R U . . .
C14E C -0.0839(3) 0.41347(7) 0.60036(9) 0.0438(7) Uani 1 1 d . . . . .
H14E H -0.0793 0.4228 0.6345 0.053 Uiso 1 1 calc R U . . .
C15E C 0.0100(3) 0.44613(9) 0.47147(10) 0.0559(9) Uani 1 1 d . . . . .
H53E H 0.0741 0.4310 0.4540 0.084 Uiso 1 1 calc R U . . .
H51E H 0.0586 0.4683 0.4871 0.084 Uiso 1 1 calc R U . . .
H52E H -0.0681 0.4543 0.4465 0.084 Uiso 1 1 calc R U . . .
H1E H -0.059(3) 0.3625(8) 0.7014(10) 0.053(9) Uiso 1 1 d . . . . .
H21E H 0.440(3) 0.3811(8) 0.7253(10) 0.051(9) Uiso 1 1 d . . . . .
H22E H 0.518(3) 0.3565(7) 0.6947(9) 0.039(8) Uiso 1 1 d . . . . .
S1F S 0.30832(6) 0.49088(2) 0.64115(2) 0.02722(13) Uani 1 1 d . . . . .
O1F O 0.55141(16) 0.43800(4) 0.74278(6) 0.0292(4) Uani 1 1 d . . . . .
O2F O 0.77926(16) 0.43023(4) 0.75335(5) 0.0276(4) Uani 1 1 d . . . . .
O3F O 0.20493(16) 0.46970(5) 0.66327(6) 0.0383(4) Uani 1 1 d . . . . .
O4F O 0.27382(18) 0.52799(5) 0.62245(6) 0.0378(4) Uani 1 1 d . . . . .
N1F N 0.4392(2) 0.49257(6) 0.68683(7) 0.0246(4) Uani 1 1 d . . . . .
N2F N 0.9445(2) 0.47545(6) 0.71225(8) 0.0287(4) Uani 1 1 d . . . . .
C1F C 0.6907(2) 0.48127(6) 0.70132(7) 0.0209(4) Uani 1 1 d . . . . .
C2F C 0.5750(2) 0.50273(6) 0.67815(7) 0.0231(5) Uani 1 1 d . . . . .
C3F C 0.5936(3) 0.53361(6) 0.64771(8) 0.0295(5) Uani 1 1 d . . . . .
H3F H 0.5162 0.5483 0.6338 0.035 Uiso 1 1 calc R U . . .
C4F C 0.7255(3) 0.54302(7) 0.63764(8) 0.0328(6) Uani 1 1 d . . . . .
H4F H 0.7374 0.5638 0.6157 0.039 Uiso 1 1 calc R U . . .
C5F C 0.8387(2) 0.52305(6) 0.65858(8) 0.0278(5) Uani 1 1 d . . . . .
H5F H 0.9281 0.5300 0.6509 0.033 Uiso 1 1 calc R U . . .
C6F C 0.8248(2) 0.49224(6) 0.69137(8) 0.0221(4) Uani 1 1 d . . . . .
C7F C 0.6649(2) 0.44868(6) 0.73371(8) 0.0218(5) Uani 1 1 d . . . . .
C8F C 0.7585(3) 0.39696(6) 0.78343(8) 0.0310(5) Uani 1 1 d . . . . .
H81F H 0.7182 0.3768 0.7606 0.047 Uiso 1 1 calc R U . . .
H82F H 0.6953 0.4029 0.8086 0.047 Uiso 1 1 calc R U . . .
H83F H 0.8478 0.3886 0.8015 0.047 Uiso 1 1 calc R U . . .
C9F C 0.3647(2) 0.46515(6) 0.59066(8) 0.0255(5) Uani 1 1 d . . . . .
C10F C 0.3539(2) 0.48053(6) 0.54196(8) 0.0296(5) Uani 1 1 d . . . . .
H10F H 0.3146 0.5048 0.5355 0.035 Uiso 1 1 calc R U . . .
C11F C 0.4007(3) 0.46039(6) 0.50281(8) 0.0312(6) Uani 1 1 d . . . . .
H11F H 0.3917 0.4710 0.4693 0.037 Uiso 1 1 calc R U . . .
C12F C 0.4603(2) 0.42523(7) 0.51083(8) 0.0304(5) Uani 1 1 d . . . . .
C13F C 0.4703(3) 0.41047(7) 0.56015(9) 0.0427(7) Uani 1 1 d . . . . .
H13F H 0.5109 0.3863 0.5668 0.051 Uiso 1 1 calc R U . . .
C14F C 0.4227(3) 0.42999(7) 0.59973(9) 0.0390(7) Uani 1 1 d . . . . .
H14F H 0.4299 0.4193 0.6332 0.047 Uiso 1 1 calc R U . . .
C15F C 0.5172(3) 0.40464(7) 0.46809(9) 0.0401(6) Uani 1 1 d . . . . .
H52F H 0.4411 0.3924 0.4461 0.060 Uiso 1 1 calc R U . . .
H53F H 0.5836 0.3855 0.4827 0.060 Uiso 1 1 calc R U . . .
H51F H 0.5639 0.4226 0.4477 0.060 Uiso 1 1 calc R U . . .
H1F H 0.438(3) 0.4743(7) 0.7069(9) 0.045(8) Uiso 1 1 d . . . . .
H21F H 0.945(2) 0.4543(7) 0.7294(8) 0.027(6) Uiso 1 1 d . . . . .
H22F H 1.019(3) 0.4814(7) 0.6980(9) 0.040(8) Uiso 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
S1A O4A 1.4287(16) . ?
S1A O3A 1.4318(17) . ?
S1A N1A 1.6394(18) . ?
S1A C9A 1.753(2) . ?
O1A C7A 1.219(3) . ?
O2A C7A 1.332(2) . ?
O2A C8A 1.443(2) . ?
N1A C2A 1.424(3) . ?
N1A H1A 0.82(3) . ?
N2A C6A 1.354(3) . ?
N2A H21A 0.84(3) . ?
N2A H22A 0.86(3) . ?
C1A C2A 1.422(3) . ?
C1A C6A 1.425(3) . ?
C1A C7A 1.478(3) . ?
C2A C3A 1.377(3) . ?
C3A C4A 1.388(3) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.364(3) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.409(3) . ?
C5A H5A 0.9500 . ?
C8A H84A 0.9800 . ?
C8A H83A 0.9800 . ?
C8A H82A 0.9800 . ?
C9A C14A 1.375(3) . ?
C9A C10A 1.383(3) . ?
C10A C11A 1.380(3) . ?
C10A H10A 0.9500 . ?
C11A C12A 1.383(3) . ?
C11A H11A 0.9500 . ?
C12A C13A 1.387(3) . ?
C12A C15A 1.493(3) . ?
C13A C14A 1.383(3) . ?
C13A H13A 0.9500 . ?
C14A H14A 0.9500 . ?
C15A H52A 0.9800 . ?
C15A H53A 0.9800 . ?
C15A H51A 0.9800 . ?
S1B O4B 1.4296(17) . ?
S1B O3B 1.4300(18) . ?
S1B N1B 1.6416(18) . ?
S1B C9B 1.749(2) . ?
O1B C7B 1.219(3) . ?
O2B C7B 1.334(2) . ?
O2B C8B 1.448(2) . ?
N1B C2B 1.420(3) . ?
N1B H1B 0.83(2) . ?
N2B C6B 1.358(3) . ?
N2B H21B 0.86(3) . ?
N2B H22B 0.84(3) . ?
C1B C6B 1.423(3) . ?
C1B C2B 1.425(3) . ?
C1B C7B 1.478(3) . ?
C2B C3B 1.380(3) . ?
C3B C4B 1.387(3) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.370(3) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.404(3) . ?
C5B H5B 0.9500 . ?
C8B H83B 0.9800 . ?
C8B H82B 0.9800 . ?
C8B H81B 0.9800 . ?
C9B C14B 1.381(3) . ?
C9B C10B 1.384(3) . ?
C10B C11B 1.383(3) . ?
C10B H10B 0.9500 . ?
C11B C12B 1.382(3) . ?
C11B H11B 0.9500 . ?
C12B C13B 1.389(4) . ?
C12B C15B 1.494(3) . ?
C13B C14B 1.377(3) . ?
C13B H13B 0.9500 . ?
C14B H14B 0.9500 . ?
C15B H53B 0.9800 . ?
C15B H51B 0.9800 . ?
C15B H52B 0.9800 . ?
S1C O3C 1.4309(18) . ?
S1C O4C 1.4310(17) . ?
S1C N1C 1.6341(19) . ?
S1C C9C 1.758(2) . ?
O1C C7C 1.219(3) . ?
O2C C7C 1.333(2) . ?
O2C C8C 1.447(2) . ?
N1C C2C 1.423(3) . ?
N1C H1C 0.80(2) . ?
N2C C6C 1.358(3) . ?
N2C H21C 0.87(3) . ?
N2C H22C 0.86(3) . ?
C1C C6C 1.424(3) . ?
C1C C2C 1.425(3) . ?
C1C C7C 1.477(3) . ?
C2C C3C 1.375(3) . ?
C3C C4C 1.384(3) . ?
C3C H3C 0.9500 . ?
C4C C5C 1.367(3) . ?
C4C H4C 0.9500 . ?
C5C C6C 1.406(3) . ?
C5C H5C 0.9500 . ?
C8C H83C 0.9800 . ?
C8C H82C 0.9800 . ?
C8C H81C 0.9800 . ?
C9C C10C 1.381(3) . ?
C9C C14C 1.383(3) . ?
C10C C11C 1.387(3) . ?
C10C H10C 0.9500 . ?
C11C C12C 1.371(3) . ?
C11C H11C 0.9500 . ?
C12C C13C 1.387(4) . ?
C12C C15C 1.498(3) . ?
C13C C14C 1.380(4) . ?
C13C H13C 0.9500 . ?
C14C H14C 0.9500 . ?
C15C H51C 0.9800 . ?
C15C H52C 0.9800 . ?
C15C H53C 0.9800 . ?
S1D O4D 1.4267(17) . ?
S1D O3D 1.4307(18) . ?
S1D N1D 1.6362(19) . ?
S1D C9D 1.755(2) . ?
O1D C7D 1.223(3) . ?
O2D C7D 1.333(2) . ?
O2D C8D 1.442(2) . ?
N2D C6D 1.354(3) . ?
N2D H21D 0.84(3) . ?
N2D H22D 0.88(3) . ?
N1D C2D 1.420(3) . ?
N1D H1D 0.79(2) . ?
C1D C6D 1.419(3) . ?
C1D C2D 1.427(3) . ?
C1D C7D 1.475(3) . ?
C2D C3D 1.380(3) . ?
C3D C4D 1.387(3) . ?
C3D H3D 0.9500 . ?
C4D C5D 1.366(3) . ?
C4D H4D 0.9500 . ?
C5D C6D 1.406(3) . ?
C5D H5D 0.9500 . ?
C8D H83D 0.9800 . ?
C8D H82D 0.9800 . ?
C8D H81D 0.9800 . ?
C9D C10D 1.370(3) . ?
C9D C14D 1.381(3) . ?
C10D C11D 1.379(3) . ?
C10D H10D 0.9500 . ?
C11D C12D 1.382(3) . ?
C11D H11D 0.9500 . ?
C12D C13D 1.380(3) . ?
C12D C15D 1.502(3) . ?
C13D C14D 1.375(3) . ?
C13D H13D 0.9500 . ?
C14D H14D 0.9500 . ?
C15D H51D 0.9800 . ?
C15D H53D 0.9800 . ?
C15D H52D 0.9800 . ?
S1E O4E 1.4205(17) . ?
S1E O3E 1.4358(18) . ?
S1E N1E 1.6283(19) . ?
S1E C9E 1.753(2) . ?
O1E C7E 1.226(3) . ?
O2E C7E 1.329(2) . ?
O2E C8E 1.446(2) . ?
N1E C2E 1.422(3) . ?
N1E H1E 0.79(3) . ?
N2E C6E 1.359(3) . ?
N2E H21E 0.85(3) . ?
N2E H22E 0.86(3) . ?
C1E C6E 1.420(3) . ?
C1E C2E 1.433(3) . ?
C1E C7E 1.472(3) . ?
C2E C3E 1.371(3) . ?
C3E C4E 1.384(3) . ?
C3E H3E 0.9500 . ?
C4E C5E 1.371(3) . ?
C4E H4E 0.9500 . ?
C5E C6E 1.404(3) . ?
C5E H5E 0.9500 . ?
C8E H82E 0.9800 . ?
C8E H83E 0.9800 . ?
C8E H81E 0.9800 . ?
C9E C10E 1.372(3) . ?
C9E C14E 1.375(3) . ?
C10E C11E 1.374(3) . ?
C10E H10E 0.9500 . ?
C11E C12E 1.389(3) . ?
C11E H11E 0.9500 . ?
C12E C13E 1.373(3) . ?
C12E C15E 1.503(3) . ?
C13E C14E 1.377(3) . ?
C13E H13E 0.9500 . ?
C14E H14E 0.9500 . ?
C15E H53E 0.9800 . ?
C15E H51E 0.9800 . ?
C15E H52E 0.9800 . ?
S1F O4F 1.4295(16) . ?
S1F O3F 1.4355(18) . ?
S1F N1F 1.6330(18) . ?
S1F C9F 1.753(2) . ?
O1F C7F 1.219(3) . ?
O2F C7F 1.335(2) . ?
O2F C8F 1.448(2) . ?
N1F C2F 1.415(3) . ?
N1F H1F 0.84(2) . ?
N2F C6F 1.358(3) . ?
N2F H21F 0.88(2) . ?
N2F H22F 0.88(3) . ?
C1F C6F 1.416(3) . ?
C1F C2F 1.428(3) . ?
C1F C7F 1.475(3) . ?
C2F C3F 1.381(3) . ?
C3F C4F 1.382(3) . ?
C3F H3F 0.9500 . ?
C4F C5F 1.364(3) . ?
C4F H4F 0.9500 . ?
C5F C6F 1.408(3) . ?
C5F H5F 0.9500 . ?
C8F H81F 0.9800 . ?
C8F H82F 0.9800 . ?
C8F H83F 0.9800 . ?
C9F C14F 1.377(3) . ?
C9F C10F 1.381(3) . ?
C10F C11F 1.375(3) . ?
C10F H10F 0.9500 . ?
C11F C12F 1.380(3) . ?
C11F H11F 0.9500 . ?
C12F C13F 1.387(3) . ?
C12F C15F 1.501(3) . ?
C13F C14F 1.376(3) . ?
C13F H13F 0.9500 . ?
C14F H14F 0.9500 . ?
C15F H52F 0.9800 . ?
C15F H53F 0.9800 . ?
C15F H51F 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
O4A S1A O3A 119.13(11) . . ?
O4A S1A N1A 109.05(10) . . ?
O3A S1A N1A 104.65(10) . . ?
O4A S1A C9A 108.15(10) . . ?
O3A S1A C9A 109.10(11) . . ?
N1A S1A C9A 106.00(10) . . ?
C7A O2A C8A 116.83(18) . . ?
C2A N1A S1A 120.10(15) . . ?
C2A N1A H1A 115(2) . . ?
S1A N1A H1A 103.9(19) . . ?
C6A N2A H21A 118.5(19) . . ?
C6A N2A H22A 115.3(16) . . ?
H21A N2A H22A 120(2) . . ?
C2A C1A C6A 117.78(19) . . ?
C2A C1A C7A 119.2(2) . . ?
C6A C1A C7A 122.99(19) . . ?
C3A C2A C1A 121.5(2) . . ?
C3A C2A N1A 118.2(2) . . ?
C1A C2A N1A 120.29(19) . . ?
C2A C3A C4A 119.6(2) . . ?
C2A C3A H3A 120.2 . . ?
C4A C3A H3A 120.2 . . ?
C5A C4A C3A 120.7(2) . . ?
C5A C4A H4A 119.7 . . ?
C3A C4A H4A 119.7 . . ?
C4A C5A C6A 121.5(2) . . ?
C4A C5A H5A 119.3 . . ?
C6A C5A H5A 119.3 . . ?
N2A C6A C5A 116.7(2) . . ?
N2A C6A C1A 124.5(2) . . ?
C5A C6A C1A 118.8(2) . . ?
O1A C7A O2A 120.46(19) . . ?
O1A C7A C1A 125.35(19) . . ?
O2A C7A C1A 114.18(19) . . ?
O2A C8A H84A 109.5 . . ?
O2A C8A H83A 109.5 . . ?
H84A C8A H83A 109.5 . . ?
O2A C8A H82A 109.5 . . ?
H84A C8A H82A 109.5 . . ?
H83A C8A H82A 109.5 . . ?
C14A C9A C10A 120.3(2) . . ?
C14A C9A S1A 120.62(19) . . ?
C10A C9A S1A 118.93(18) . . ?
C11A C10A C9A 119.6(2) . . ?
C11A C10A H10A 120.2 . . ?
C9A C10A H10A 120.2 . . ?
C10A C11A C12A 121.2(2) . . ?
C10A C11A H11A 119.4 . . ?
C12A C11A H11A 119.4 . . ?
C11A C12A C13A 118.0(2) . . ?
C11A C12A C15A 120.5(2) . . ?
C13A C12A C15A 121.5(2) . . ?
C14A C13A C12A 121.5(2) . . ?
C14A C13A H13A 119.2 . . ?
C12A C13A H13A 119.2 . . ?
C9A C14A C13A 119.3(2) . . ?
C9A C14A H14A 120.3 . . ?
C13A C14A H14A 120.3 . . ?
C12A C15A H52A 109.5 . . ?
C12A C15A H53A 109.5 . . ?
H52A C15A H53A 109.5 . . ?
C12A C15A H51A 109.5 . . ?
H52A C15A H51A 109.5 . . ?
H53A C15A H51A 109.5 . . ?
O4B S1B O3B 119.35(11) . . ?
O4B S1B N1B 108.78(10) . . ?
O3B S1B N1B 104.63(10) . . ?
O4B S1B C9B 107.88(10) . . ?
O3B S1B C9B 109.27(11) . . ?
N1B S1B C9B 106.18(10) . . ?
C7B O2B C8B 116.70(18) . . ?
C2B N1B S1B 120.25(15) . . ?
C2B N1B H1B 112.6(19) . . ?
S1B N1B H1B 104.4(17) . . ?
C6B N2B H21B 118.0(19) . . ?
C6B N2B H22B 117.4(17) . . ?
H21B N2B H22B 120(3) . . ?
C6B C1B C2B 117.87(19) . . ?
C6B C1B C7B 122.89(19) . . ?
C2B C1B C7B 119.2(2) . . ?
C3B C2B N1B 118.4(2) . . ?
C3B C2B C1B 121.4(2) . . ?
N1B C2B C1B 120.21(19) . . ?
C2B C3B C4B 119.6(2) . . ?
C2B C3B H3B 120.2 . . ?
C4B C3B H3B 120.2 . . ?
C5B C4B C3B 120.6(2) . . ?
C5B C4B H4B 119.7 . . ?
C3B C4B H4B 119.7 . . ?
C4B C5B C6B 121.6(2) . . ?
C4B C5B H5B 119.2 . . ?
C6B C5B H5B 119.2 . . ?
N2B C6B C5B 116.2(2) . . ?
N2B C6B C1B 124.9(2) . . ?
C5B C6B C1B 118.9(2) . . ?
O1B C7B O2B 120.4(2) . . ?
O1B C7B C1B 125.4(2) . . ?
O2B C7B C1B 114.23(19) . . ?
O2B C8B H83B 109.5 . . ?
O2B C8B H82B 109.5 . . ?
H83B C8B H82B 109.5 . . ?
O2B C8B H81B 109.5 . . ?
H83B C8B H81B 109.5 . . ?
H82B C8B H81B 109.5 . . ?
C14B C9B C10B 119.9(2) . . ?
C14B C9B S1B 120.95(19) . . ?
C10B C9B S1B 119.05(18) . . ?
C11B C10B C9B 119.7(2) . . ?
C11B C10B H10B 120.2 . . ?
C9B C10B H10B 120.2 . . ?
C12B C11B C10B 121.4(2) . . ?
C12B C11B H11B 119.3 . . ?
C10B C11B H11B 119.3 . . ?
C11B C12B C13B 117.8(2) . . ?
C11B C12B C15B 120.2(2) . . ?
C13B C12B C15B 121.9(2) . . ?
C14B C13B C12B 121.6(2) . . ?
C14B C13B H13B 119.2 . . ?
C12B C13B H13B 119.2 . . ?
C13B C14B C9B 119.6(2) . . ?
C13B C14B H14B 120.2 . . ?
C9B C14B H14B 120.2 . . ?
C12B C15B H53B 109.5 . . ?
C12B C15B H51B 109.5 . . ?
H53B C15B H51B 109.5 . . ?
C12B C15B H52B 109.5 . . ?
H53B C15B H52B 109.5 . . ?
H51B C15B H52B 109.5 . . ?
O3C S1C O4C 119.36(11) . . ?
O3C S1C N1C 104.74(10) . . ?
O4C S1C N1C 108.78(11) . . ?
O3C S1C C9C 108.66(11) . . ?
O4C S1C C9C 107.75(10) . . ?
N1C S1C C9C 106.94(10) . . ?
C7C O2C C8C 116.34(18) . . ?
C2C N1C S1C 121.55(16) . . ?
C2C N1C H1C 111.2(18) . . ?
S1C N1C H1C 107.7(17) . . ?
C6C N2C H21C 117.7(19) . . ?
C6C N2C H22C 116.4(18) . . ?
H21C N2C H22C 124(3) . . ?
C6C C1C C2C 117.66(19) . . ?
C6C C1C C7C 123.15(19) . . ?
C2C C1C C7C 119.2(2) . . ?
C3C C2C N1C 118.5(2) . . ?
C3C C2C C1C 121.6(2) . . ?
N1C C2C C1C 119.9(2) . . ?
C2C C3C C4C 119.6(2) . . ?
C2C C3C H3C 120.2 . . ?
C4C C3C H3C 120.2 . . ?
C5C C4C C3C 120.7(2) . . ?
C5C C4C H4C 119.6 . . ?
C3C C4C H4C 119.6 . . ?
C4C C5C C6C 121.5(2) . . ?
C4C C5C H5C 119.2 . . ?
C6C C5C H5C 119.2 . . ?
N2C C6C C5C 116.6(2) . . ?
N2C C6C C1C 124.6(2) . . ?
C5C C6C C1C 118.7(2) . . ?
O1C C7C O2C 120.4(2) . . ?
O1C C7C C1C 125.3(2) . . ?
O2C C7C C1C 114.25(19) . . ?
O2C C8C H83C 109.5 . . ?
O2C C8C H82C 109.5 . . ?
H83C C8C H82C 109.5 . . ?
O2C C8C H81C 109.5 . . ?
H83C C8C H81C 109.5 . . ?
H82C C8C H81C 109.5 . . ?
C10C C9C C14C 119.6(2) . . ?
C10C C9C S1C 119.50(19) . . ?
C14C C9C S1C 120.87(19) . . ?
C9C C10C C11C 120.0(2) . . ?
C9C C10C H10C 120.0 . . ?
C11C C10C H10C 120.0 . . ?
C12C C11C C10C 121.0(3) . . ?
C12C C11C H11C 119.5 . . ?
C10C C11C H11C 119.5 . . ?
C11C C12C C13C 118.3(2) . . ?
C11C C12C C15C 120.1(3) . . ?
C13C C12C C15C 121.6(2) . . ?
C14C C13C C12C 121.6(2) . . ?
C14C C13C H13C 119.2 . . ?
C12C C13C H13C 119.2 . . ?
C13C C14C C9C 119.4(3) . . ?
C13C C14C H14C 120.3 . . ?
C9C C14C H14C 120.3 . . ?
C12C C15C H51C 109.5 . . ?
C12C C15C H52C 109.5 . . ?
H51C C15C H52C 109.5 . . ?
C12C C15C H53C 109.5 . . ?
H51C C15C H53C 109.5 . . ?
H52C C15C H53C 109.5 . . ?
O4D S1D O3D 119.12(11) . . ?
O4D S1D N1D 109.72(10) . . ?
O3D S1D N1D 104.07(10) . . ?
O4D S1D C9D 107.89(11) . . ?
O3D S1D C9D 109.34(11) . . ?
N1D S1D C9D 105.95(10) . . ?
C7D O2D C8D 117.32(18) . . ?
C6D N2D H21D 118.4(18) . . ?
C6D N2D H22D 117.6(16) . . ?
H21D N2D H22D 117(2) . . ?
C2D N1D S1D 121.93(15) . . ?
C2D N1D H1D 113.9(19) . . ?
S1D N1D H1D 106.8(18) . . ?
C6D C1D C2D 118.12(19) . . ?
C6D C1D C7D 122.82(19) . . ?
C2D C1D C7D 119.1(2) . . ?
C3D C2D N1D 118.9(2) . . ?
C3D C2D C1D 121.3(2) . . ?
N1D C2D C1D 119.81(19) . . ?
C2D C3D C4D 119.4(2) . . ?
C2D C3D H3D 120.3 . . ?
C4D C3D H3D 120.3 . . ?
C5D C4D C3D 121.1(2) . . ?
C5D C4D H4D 119.5 . . ?
C3D C4D H4D 119.5 . . ?
C4D C5D C6D 121.3(2) . . ?
C4D C5D H5D 119.3 . . ?
C6D C5D H5D 119.3 . . ?
N2D C6D C5D 116.4(2) . . ?
N2D C6D C1D 124.8(2) . . ?
C5D C6D C1D 118.8(2) . . ?
O1D C7D O2D 119.95(19) . . ?
O1D C7D C1D 125.5(2) . . ?
O2D C7D C1D 114.51(19) . . ?
O2D C8D H83D 109.5 . . ?
O2D C8D H82D 109.5 . . ?
H83D C8D H82D 109.5 . . ?
O2D C8D H81D 109.5 . . ?
H83D C8D H81D 109.5 . . ?
H82D C8D H81D 109.5 . . ?
C10D C9D C14D 120.5(2) . . ?
C10D C9D S1D 119.86(18) . . ?
C14D C9D S1D 119.54(18) . . ?
C9D C10D C11D 119.1(2) . . ?
C9D C10D H10D 120.4 . . ?
C11D C10D H10D 120.4 . . ?
C10D C11D C12D 121.8(2) . . ?
C10D C11D H11D 119.1 . . ?
C12D C11D H11D 119.1 . . ?
C13D C12D C11D 117.7(2) . . ?
C13D C12D C15D 121.7(2) . . ?
C11D C12D C15D 120.5(2) . . ?
C14D C13D C12D 121.5(2) . . ?
C14D C13D H13D 119.2 . . ?
C12D C13D H13D 119.2 . . ?
C13D C14D C9D 119.3(2) . . ?
C13D C14D H14D 120.3 . . ?
C9D C14D H14D 120.3 . . ?
C12D C15D H51D 109.5 . . ?
C12D C15D H53D 109.5 . . ?
H51D C15D H53D 109.5 . . ?
C12D C15D H52D 109.5 . . ?
H51D C15D H52D 109.5 . . ?
H53D C15D H52D 109.5 . . ?
O4E S1E O3E 118.23(12) . . ?
O4E S1E N1E 110.41(11) . . ?
O3E S1E N1E 103.96(10) . . ?
O4E S1E C9E 107.70(11) . . ?
O3E S1E C9E 109.20(11) . . ?
N1E S1E C9E 106.80(10) . . ?
C7E O2E C8E 116.62(18) . . ?
C2E N1E S1E 122.66(16) . . ?
C2E N1E H1E 110(2) . . ?
S1E N1E H1E 113(2) . . ?
C6E N2E H21E 119.9(19) . . ?
C6E N2E H22E 118.8(16) . . ?
H21E N2E H22E 118(3) . . ?
C6E C1E C2E 117.53(19) . . ?
C6E C1E C7E 123.04(19) . . ?
C2E C1E C7E 119.4(2) . . ?
C3E C2E N1E 119.8(2) . . ?
C3E C2E C1E 121.3(2) . . ?
N1E C2E C1E 118.8(2) . . ?
C2E C3E C4E 119.9(2) . . ?
C2E C3E H3E 120.1 . . ?
C4E C3E H3E 120.1 . . ?
C5E C4E C3E 121.0(2) . . ?
C5E C4E H4E 119.5 . . ?
C3E C4E H4E 119.5 . . ?
C4E C5E C6E 120.8(2) . . ?
C4E C5E H5E 119.6 . . ?
C6E C5E H5E 119.6 . . ?
N2E C6E C5E 116.4(2) . . ?
N2E C6E C1E 124.1(2) . . ?
C5E C6E C1E 119.4(2) . . ?
O1E C7E O2E 120.0(2) . . ?
O1E C7E C1E 125.0(2) . . ?
O2E C7E C1E 114.96(19) . . ?
O2E C8E H82E 109.5 . . ?
O2E C8E H83E 109.5 . . ?
H82E C8E H83E 109.5 . . ?
O2E C8E H81E 109.5 . . ?
H82E C8E H81E 109.5 . . ?
H83E C8E H81E 109.5 . . ?
C10E C9E C14E 119.9(2) . . ?
C10E C9E S1E 119.67(18) . . ?
C14E C9E S1E 120.39(17) . . ?
C9E C10E C11E 119.7(2) . . ?
C9E C10E H10E 120.1 . . ?
C11E C10E H10E 120.1 . . ?
C10E C11E C12E 121.7(2) . . ?
C10E C11E H11E 119.2 . . ?
C12E C11E H11E 119.2 . . ?
C13E C12E C11E 117.1(2) . . ?
C13E C12E C15E 122.3(3) . . ?
C11E C12E C15E 120.6(2) . . ?
C12E C13E C14E 122.1(3) . . ?
C12E C13E H13E 118.9 . . ?
C14E C13E H13E 118.9 . . ?
C9E C14E C13E 119.4(2) . . ?
C9E C14E H14E 120.3 . . ?
C13E C14E H14E 120.3 . . ?
C12E C15E H53E 109.5 . . ?
C12E C15E H51E 109.5 . . ?
H53E C15E H51E 109.5 . . ?
C12E C15E H52E 109.5 . . ?
H53E C15E H52E 109.5 . . ?
H51E C15E H52E 109.5 . . ?
O4F S1F O3F 118.36(11) . . ?
O4F S1F N1F 110.14(10) . . ?
O3F S1F N1F 104.05(10) . . ?
O4F S1F C9F 107.63(10) . . ?
O3F S1F C9F 109.60(11) . . ?
N1F S1F C9F 106.48(10) . . ?
C7F O2F C8F 116.26(18) . . ?
C2F N1F S1F 123.15(15) . . ?
C2F N1F H1F 113.0(19) . . ?
S1F N1F H1F 110.9(18) . . ?
C6F N2F H21F 122.1(16) . . ?
C6F N2F H22F 115.7(16) . . ?
H21F N2F H22F 118(2) . . ?
C6F C1F C2F 117.92(19) . . ?
C6F C1F C7F 123.39(19) . . ?
C2F C1F C7F 118.7(2) . . ?
C3F C2F N1F 119.3(2) . . ?
C3F C2F C1F 121.0(2) . . ?
N1F C2F C1F 119.75(19) . . ?
C2F C3F C4F 119.7(2) . . ?
C2F C3F H3F 120.2 . . ?
C4F C3F H3F 120.2 . . ?
C5F C4F C3F 121.2(2) . . ?
C5F C4F H4F 119.4 . . ?
C3F C4F H4F 119.4 . . ?
C4F C5F C6F 120.9(2) . . ?
C4F C5F H5F 119.5 . . ?
C6F C5F H5F 119.5 . . ?
N2F C6F C5F 116.3(2) . . ?
N2F C6F C1F 124.5(2) . . ?
C5F C6F C1F 119.24(19) . . ?
O1F C7F O2F 120.13(19) . . ?
O1F C7F C1F 125.56(19) . . ?
O2F C7F C1F 114.31(19) . . ?
O2F C8F H81F 109.5 . . ?
O2F C8F H82F 109.5 . . ?
H81F C8F H82F 109.5 . . ?
O2F C8F H83F 109.5 . . ?
H81F C8F H83F 109.5 . . ?
H82F C8F H83F 109.5 . . ?
C14F C9F C10F 119.9(2) . . ?
C14F C9F S1F 120.14(17) . . ?
C10F C9F S1F 119.94(18) . . ?
C11F C10F C9F 119.5(2) . . ?
C11F C10F H10F 120.2 . . ?
C9F C10F H10F 120.2 . . ?
C10F C11F C12F 121.9(2) . . ?
C10F C11F H11F 119.1 . . ?
C12F C11F H11F 119.1 . . ?
C11F C12F C13F 117.5(2) . . ?
C11F C12F C15F 120.9(2) . . ?
C13F C12F C15F 121.6(2) . . ?
C14F C13F C12F 121.5(2) . . ?
C14F C13F H13F 119.2 . . ?
C12F C13F H13F 119.2 . . ?
C13F C14F C9F 119.7(2) . . ?
C13F C14F H14F 120.1 . . ?
C9F C14F H14F 120.1 . . ?
C12F C15F H52F 109.5 . . ?
C12F C15F H53F 109.5 . . ?
H52F C15F H53F 109.5 . . ?
C12F C15F H51F 109.5 . . ?
H52F C15F H51F 109.5 . . ?
H53F C15F H51F 109.5 . . ?

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
O4A S1A N1A C2A 62.07(19) . . . . ?
O3A S1A N1A C2A -169.43(17) . . . . ?
C9A S1A N1A C2A -54.2(2) . . . . ?
C6A C1A C2A C3A 1.8(3) . . . . ?
C7A C1A C2A C3A -178.12(18) . . . . ?
C6A C1A C2A N1A -178.62(18) . . . . ?
C7A C1A C2A N1A 1.4(3) . . . . ?
S1A N1A C2A C3A -58.4(3) . . . . ?
S1A N1A C2A C1A 122.04(18) . . . . ?
C1A C2A C3A C4A -3.8(3) . . . . ?
N1A C2A C3A C4A 176.65(19) . . . . ?
C2A C3A C4A C5A 2.7(3) . . . . ?
C3A C4A C5A C6A 0.3(3) . . . . ?
C4A C5A C6A N2A 176.1(2) . . . . ?
C4A C5A C6A C1A -2.2(3) . . . . ?
C2A C1A C6A N2A -177.0(2) . . . . ?
C7A C1A C6A N2A 2.9(3) . . . . ?
C2A C1A C6A C5A 1.1(3) . . . . ?
C7A C1A C6A C5A -178.92(18) . . . . ?
C8A O2A C7A O1A -0.1(3) . . . . ?
C8A O2A C7A C1A -179.96(16) . . . . ?
C2A C1A C7A O1A -2.3(3) . . . . ?
C6A C1A C7A O1A 177.8(2) . . . . ?
C2A C1A C7A O2A 177.53(17) . . . . ?
C6A C1A C7A O2A -2.4(3) . . . . ?
O4A S1A C9A C14A 152.57(18) . . . . ?
O3A S1A C9A C14A 21.6(2) . . . . ?
N1A S1A C9A C14A -90.6(2) . . . . ?
O4A S1A C9A C10A -31.5(2) . . . . ?
O3A S1A C9A C10A -162.48(18) . . . . ?
N1A S1A C9A C10A 85.3(2) . . . . ?
C14A C9A C10A C11A 0.1(4) . . . . ?
S1A C9A C10A C11A -175.82(18) . . . . ?
C9A C10A C11A C12A -0.9(4) . . . . ?
C10A C11A C12A C13A 1.1(4) . . . . ?
C10A C11A C12A C15A -179.7(2) . . . . ?
C11A C12A C13A C14A -0.6(4) . . . . ?
C15A C12A C13A C14A -179.8(2) . . . . ?
C10A C9A C14A C13A 0.4(3) . . . . ?
S1A C9A C14A C13A 176.24(18) . . . . ?
C12A C13A C14A C9A -0.1(4) . . . . ?
O4B S1B N1B C2B -62.0(2) . . . . ?
O3B S1B N1B C2B 169.36(17) . . . . ?
C9B S1B N1B C2B 53.8(2) . . . . ?
S1B N1B C2B C3B 58.4(3) . . . . ?
S1B N1B C2B C1B -121.59(19) . . . . ?
C6B C1B C2B C3B -1.6(3) . . . . ?
C7B C1B C2B C3B 178.52(19) . . . . ?
C6B C1B C2B N1B 178.33(18) . . . . ?
C7B C1B C2B N1B -1.5(3) . . . . ?
N1B C2B C3B C4B -176.4(2) . . . . ?
C1B C2B C3B C4B 3.5(3) . . . . ?
C2B C3B C4B C5B -2.7(3) . . . . ?
C3B C4B C5B C6B -0.1(3) . . . . ?
C4B C5B C6B N2B -176.8(2) . . . . ?
C4B C5B C6B C1B 2.0(3) . . . . ?
C2B C1B C6B N2B 177.6(2) . . . . ?
C7B C1B C6B N2B -2.6(3) . . . . ?
C2B C1B C6B C5B -1.1(3) . . . . ?
C7B C1B C6B C5B 178.74(18) . . . . ?
C8B O2B C7B O1B -0.2(3) . . . . ?
C8B O2B C7B C1B 179.51(16) . . . . ?
C6B C1B C7B O1B -179.7(2) . . . . ?
C2B C1B C7B O1B 0.1(3) . . . . ?
C6B C1B C7B O2B 0.6(3) . . . . ?
C2B C1B C7B O2B -179.59(17) . . . . ?
O4B S1B C9B C14B -148.32(18) . . . . ?
O3B S1B C9B C14B -17.1(2) . . . . ?
N1B S1B C9B C14B 95.2(2) . . . . ?
O4B S1B C9B C10B 34.9(2) . . . . ?
O3B S1B C9B C10B 166.09(17) . . . . ?
N1B S1B C9B C10B -81.58(19) . . . . ?
C14B C9B C10B C11B 0.3(3) . . . . ?
S1B C9B C10B C11B 177.07(18) . . . . ?
C9B C10B C11B C12B 0.6(4) . . . . ?
C10B C11B C12B C13B -0.7(4) . . . . ?
C10B C11B C12B C15B 179.7(2) . . . . ?
C11B C12B C13B C14B -0.1(4) . . . . ?
C15B C12B C13B C14B 179.6(2) . . . . ?
C12B C13B C14B C9B 0.9(4) . . . . ?
C10B C9B C14B C13B -1.0(3) . . . . ?
S1B C9B C14B C13B -177.77(18) . . . . ?
O3C S1C N1C C2C 171.21(18) . . . . ?
O4C S1C N1C C2C -60.1(2) . . . . ?
C9C S1C N1C C2C 56.0(2) . . . . ?
S1C N1C C2C C3C 55.5(3) . . . . ?
S1C N1C C2C C1C -124.90(19) . . . . ?
C6C C1C C2C C3C -1.8(3) . . . . ?
C7C C1C C2C C3C 177.88(19) . . . . ?
C6C C1C C2C N1C 178.62(18) . . . . ?
C7C C1C C2C N1C -1.7(3) . . . . ?
N1C C2C C3C C4C -176.5(2) . . . . ?
C1C C2C C3C C4C 3.9(3) . . . . ?
C2C C3C C4C C5C -2.7(3) . . . . ?
C3C C4C C5C C6C -0.5(3) . . . . ?
C4C C5C C6C N2C -176.4(2) . . . . ?
C4C C5C C6C C1C 2.6(3) . . . . ?
C2C C1C C6C N2C 177.5(2) . . . . ?
C7C C1C C6C N2C -2.1(3) . . . . ?
C2C C1C C6C C5C -1.4(3) . . . . ?
C7C C1C C6C C5C 178.91(18) . . . . ?
C8C O2C C7C O1C 1.2(3) . . . . ?
C8C O2C C7C C1C -178.96(17) . . . . ?
C6C C1C C7C O1C -179.0(2) . . . . ?
C2C C1C C7C O1C 1.3(3) . . . . ?
C6C C1C C7C O2C 1.2(3) . . . . ?
C2C C1C C7C O2C -178.48(17) . . . . ?
O3C S1C C9C C10C 169.96(19) . . . . ?
O4C S1C C9C C10C 39.3(2) . . . . ?
N1C S1C C9C C10C -77.5(2) . . . . ?
O3C S1C C9C C14C -11.6(2) . . . . ?
O4C S1C C9C C14C -142.29(19) . . . . ?
N1C S1C C9C C14C 100.9(2) . . . . ?
C14C C9C C10C C11C 0.8(4) . . . . ?
S1C C9C C10C C11C 179.3(2) . . . . ?
C9C C10C C11C C12C 1.1(4) . . . . ?
C10C C11C C12C C13C -2.5(4) . . . . ?
C10C C11C C12C C15C 178.4(2) . . . . ?
C11C C12C C13C C14C 2.0(4) . . . . ?
C15C C12C C13C C14C -178.9(2) . . . . ?
C12C C13C C14C C9C -0.1(4) . . . . ?
C10C C9C C14C C13C -1.3(4) . . . . ?
S1C C9C C14C C13C -179.70(19) . . . . ?
O4D S1D N1D C2D 65.9(2) . . . . ?
O3D S1D N1D C2D -165.54(18) . . . . ?
C9D S1D N1D C2D -50.3(2) . . . . ?
S1D N1D C2D C3D -51.8(3) . . . . ?
S1D N1D C2D C1D 129.01(18) . . . . ?
C6D C1D C2D C3D 1.4(3) . . . . ?
C7D C1D C2D C3D -178.42(18) . . . . ?
C6D C1D C2D N1D -179.50(18) . . . . ?
C7D C1D C2D N1D 0.7(3) . . . . ?
N1D C2D C3D C4D 178.43(19) . . . . ?
C1D C2D C3D C4D -2.4(3) . . . . ?
C2D C3D C4D C5D 1.3(3) . . . . ?
C3D C4D C5D C6D 0.9(3) . . . . ?
C4D C5D C6D N2D 177.0(2) . . . . ?
C4D C5D C6D C1D -2.0(3) . . . . ?
C2D C1D C6D N2D -178.1(2) . . . . ?
C7D C1D C6D N2D 1.7(3) . . . . ?
C2D C1D C6D C5D 0.8(3) . . . . ?
C7D C1D C6D C5D -179.41(18) . . . . ?
C8D O2D C7D O1D -0.9(3) . . . . ?
C8D O2D C7D C1D 179.69(17) . . . . ?
C6D C1D C7D O1D -179.5(2) . . . . ?
C2D C1D C7D O1D 0.2(3) . . . . ?
C6D C1D C7D O2D -0.1(3) . . . . ?
C2D C1D C7D O2D 179.62(17) . . . . ?
O4D S1D C9D C10D -9.2(2) . . . . ?
O3D S1D C9D C10D -140.17(19) . . . . ?
N1D S1D C9D C10D 108.2(2) . . . . ?
O4D S1D C9D C14D 174.20(19) . . . . ?
O3D S1D C9D C14D 43.3(2) . . . . ?
N1D S1D C9D C14D -68.3(2) . . . . ?
C14D C9D C10D C11D 0.8(4) . . . . ?
S1D C9D C10D C11D -175.70(19) . . . . ?
C9D C10D C11D C12D 0.8(4) . . . . ?
C10D C11D C12D C13D -1.7(4) . . . . ?
C10D C11D C12D C15D 176.8(2) . . . . ?
C11D C12D C13D C14D 1.1(4) . . . . ?
C15D C12D C13D C14D -177.4(2) . . . . ?
C12D C13D C14D C9D 0.4(4) . . . . ?
C10D C9D C14D C13D -1.4(4) . . . . ?
S1D C9D C14D C13D 175.1(2) . . . . ?
O4E S1E N1E C2E 66.8(2) . . . . ?
O3E S1E N1E C2E -165.46(18) . . . . ?
C9E S1E N1E C2E -50.1(2) . . . . ?
S1E N1E C2E C3E -45.7(3) . . . . ?
S1E N1E C2E C1E 135.09(18) . . . . ?
C6E C1E C2E C3E 1.5(3) . . . . ?
C7E C1E C2E C3E -179.90(19) . . . . ?
C6E C1E C2E N1E -179.27(18) . . . . ?
C7E C1E C2E N1E -0.6(3) . . . . ?
N1E C2E C3E C4E 178.1(2) . . . . ?
C1E C2E C3E C4E -2.7(3) . . . . ?
C2E C3E C4E C5E 1.5(4) . . . . ?
C3E C4E C5E C6E 0.7(4) . . . . ?
C4E C5E C6E N2E 176.2(2) . . . . ?
C4E C5E C6E C1E -1.9(3) . . . . ?
C2E C1E C6E N2E -177.11(19) . . . . ?
C7E C1E C6E N2E 4.3(3) . . . . ?
C2E C1E C6E C5E 0.8(3) . . . . ?
C7E C1E C6E C5E -177.80(19) . . . . ?
C8E O2E C7E O1E -3.2(3) . . . . ?
C8E O2E C7E C1E 176.90(17) . . . . ?
C6E C1E C7E O1E 178.9(2) . . . . ?
C2E C1E C7E O1E 0.3(3) . . . . ?
C6E C1E C7E O2E -1.2(3) . . . . ?
C2E C1E C7E O2E -179.76(17) . . . . ?
O4E S1E C9E C10E 5.1(2) . . . . ?
O3E S1E C9E C10E -124.42(19) . . . . ?
N1E S1E C9E C10E 123.73(19) . . . . ?
O4E S1E C9E C14E -173.6(2) . . . . ?
O3E S1E C9E C14E 56.8(2) . . . . ?
N1E S1E C9E C14E -55.0(2) . . . . ?
C14E C9E C10E C11E 0.1(4) . . . . ?
S1E C9E C10E C11E -178.6(2) . . . . ?
C9E C10E C11E C12E 0.3(4) . . . . ?
C10E C11E C12E C13E -0.3(4) . . . . ?
C10E C11E C12E C15E 178.6(3) . . . . ?
C11E C12E C13E C14E -0.3(4) . . . . ?
C15E C12E C13E C14E -179.1(3) . . . . ?
C10E C9E C14E C13E -0.7(4) . . . . ?
S1E C9E C14E C13E 178.1(2) . . . . ?
C12E C13E C14E C9E 0.7(5) . . . . ?
O4F S1F N1F C2F -67.9(2) . . . . ?
O3F S1F N1F C2F 164.22(18) . . . . ?
C9F S1F N1F C2F 48.5(2) . . . . ?
S1F N1F C2F C3F 45.2(3) . . . . ?
S1F N1F C2F C1F -135.49(17) . . . . ?
C6F C1F C2F C3F -1.1(3) . . . . ?
C7F C1F C2F C3F 179.65(19) . . . . ?
C6F C1F C2F N1F 179.60(18) . . . . ?
C7F C1F C2F N1F 0.3(3) . . . . ?
N1F C2F C3F C4F -177.9(2) . . . . ?
C1F C2F C3F C4F 2.8(3) . . . . ?
C2F C3F C4F C5F -2.1(3) . . . . ?
C3F C4F C5F C6F -0.3(3) . . . . ?
C4F C5F C6F N2F -176.8(2) . . . . ?
C4F C5F C6F C1F 2.0(3) . . . . ?
C2F C1F C6F N2F 177.37(19) . . . . ?
C7F C1F C6F N2F -3.4(3) . . . . ?
C2F C1F C6F C5F -1.3(3) . . . . ?
C7F C1F C6F C5F 177.95(18) . . . . ?
C8F O2F C7F O1F 2.3(3) . . . . ?
C8F O2F C7F C1F -177.17(17) . . . . ?
C6F C1F C7F O1F -179.1(2) . . . . ?
C2F C1F C7F O1F 0.1(3) . . . . ?
C6F C1F C7F O2F 0.3(3) . . . . ?
C2F C1F C7F O2F 179.53(17) . . . . ?
O4F S1F C9F C14F 171.1(2) . . . . ?
O3F S1F C9F C14F -59.0(2) . . . . ?
N1F S1F C9F C14F 53.0(2) . . . . ?
O4F S1F C9F C10F -7.4(2) . . . . ?
O3F S1F C9F C10F 122.58(19) . . . . ?
N1F S1F C9F C10F -125.46(19) . . . . ?
C14F C9F C10F C11F 0.4(4) . . . . ?
S1F C9F C10F C11F 178.86(19) . . . . ?
C9F C10F C11F C12F -1.0(4) . . . . ?
C10F C11F C12F C13F 0.7(4) . . . . ?
C10F C11F C12F C15F -176.8(2) . . . . ?
C11F C12F C13F C14F 0.0(4) . . . . ?
C15F C12F C13F C14F 177.6(3) . . . . ?
C12F C13F C14F C9F -0.5(4) . . . . ?
C10F C9F C14F C13F 0.3(4) . . . . ?
S1F C9F C14F C13F -178.1(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
C3A H3A O4A 0.95 2.43 2.992(3) 117.6 .
N1A H1A O1A 0.82(3) 1.94(3) 2.612(2) 140(3) .
N2A H21A O2A 0.84(3) 1.97(3) 2.593(3) 130(2) .
N2A H21A O1B 0.84(3) 2.44(3) 3.162(3) 144(2) 1_455
N2A H22A O3A 0.86(3) 2.14(3) 2.987(3) 168(2) 1_455
C3B H3B O4B 0.95 2.44 2.994(3) 117.3 .
C8B H81B O3A 0.98 2.65 3.457(3) 140.1 .
N1B H1B O1B 0.83(2) 1.91(2) 2.613(2) 143(3) .
N2B H21B O1A 0.86(3) 2.43(3) 3.138(3) 140(2) .
N2B H21B O2B 0.86(3) 1.95(3) 2.599(3) 131(2) .
N2B H22B O3B 0.84(3) 2.18(3) 3.012(3) 172(2) 1_455
C3C H3C O4C 0.95 2.40 2.984(3) 119.1 .
C8C H83C O3D 0.98 2.60 3.374(3) 136.0 .
N1C H1C O1C 0.80(2) 1.91(2) 2.603(2) 145(2) .
N2C H21C O2C 0.87(3) 1.94(3) 2.602(3) 131(2) .
N2C H21C O1D 0.87(3) 2.36(3) 3.076(3) 139(2) .
N2C H22C O3C 0.86(3) 2.20(3) 3.016(3) 159(3) 1_655
C3D H3D O4D 0.95 2.44 3.065(3) 123.0 .
N1D H1D O1D 0.79(2) 1.93(2) 2.599(2) 142(3) .
N2D H21D O1C 0.84(3) 2.36(3) 3.071(3) 143(2) 1_655
N2D H21D O2D 0.84(3) 1.97(3) 2.594(3) 130(2) .
N2D H22D O3D 0.88(3) 2.09(3) 2.955(3) 167(2) 1_655
C3E H3E O4E 0.95 2.44 3.092(3) 125.6 .
C8E H82E O3F 0.98 2.62 3.346(3) 131.3 .
N1E H1E O1E 0.79(3) 1.87(3) 2.580(3) 148(3) .
N2E H21E O2E 0.85(3) 1.98(3) 2.596(3) 129(2) .
N2E H21E O1F 0.85(3) 2.31(3) 3.023(3) 142(3) .
N2E H22E O3E 0.86(3) 2.16(3) 2.975(3) 156(2) 1_655
C3F H3F O4F 0.95 2.45 3.101(3) 126.0 .
C8F H81F O3E 0.98 2.63 3.354(3) 130.6 1_655
N1F H1F O1F 0.84(2) 1.87(3) 2.585(2) 142(3) .
N2F H21F O1E 0.88(2) 2.26(2) 3.004(3) 143(2) 1_655
N2F H21F O2F 0.88(2) 1.99(2) 2.600(3) 125(2) .
N2F H22F O3F 0.88(3) 2.16(3) 2.989(3) 155(2) 1_655

_refine_diff_density_max         0.392
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.065

_shelxl_version_number           2014-3


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetone'
####################################################################### 
# 
# 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_bf4absH
_database_code_depnum_ccdc_archive 'CCDC 1994135'
loop_
_audit_author_name
_audit_author_address
'PROFESSOR J D WALLIS'
;Nottingham Trent University, UK
United Kingdom
;
_audit_update_record             
;
2020-04-01 deposited with the CCDC.	2020-05-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
Methyl2,6-dinitrobenzoate bis HBF4 salt
;
_chemical_name_common            ?
_chemical_melting_point          483-485
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H12 B2 F8 N2 O2'
_chemical_formula_weight         341.82

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   7.1001(4)
_cell_length_b                   10.8475(7)
_cell_length_c                   16.4165(11)
_cell_angle_alpha                90
_cell_angle_beta                 94.379(6)
_cell_angle_gamma                90
_cell_volume                     1260.68(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2362
_cell_measurement_theta_min      4.1030
_cell_measurement_theta_max      29.2360

_exptl_crystal_description       'thick plate'
_exptl_crystal_colour            'pale brown'

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_F_000             688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3349
_exptl_crystal_size_mid          0.1509
_exptl_crystal_size_min          0.1331
_exptl_absorpt_coefficient_mu    0.200
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.978
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_detector_area_resol_mean 15.9832
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            6957
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.047
_diffrn_reflns_theta_max         29.372
_diffrn_reflns_theta_full        27.000
_diffrn_measured_fraction_theta_max 0.855
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.855
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             2966
_reflns_number_gt                2368
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;

_computing_structure_solution    SHELXS-97
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0315P)²+0.2125P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2966
_refine_ls_number_parameters     224
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0440
_refine_ls_wR_factor_ref         0.0884
_refine_ls_wR_factor_gt          0.0818
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
F1 F 0.41716(14) 0.30171(9) 0.01871(6) 0.0174(3) Uani 1 1 d . . . . .
F2 F 0.42408(14) 0.34702(9) -0.11621(6) 0.0182(3) Uani 1 1 d . . . . .
F3 F 0.66838(14) 0.40683(9) -0.02709(7) 0.0180(3) Uani 1 1 d . . . . .
F4 F 0.62858(15) 0.20344(9) -0.05661(7) 0.0216(3) Uani 1 1 d . . . . .
F5 F 1.07428(15) 0.38768(10) 0.09352(7) 0.0228(3) Uani 1 1 d . . . . .
F6 F 1.06141(16) 0.32146(10) 0.22311(7) 0.0259(3) Uani 1 1 d . . . . .
F7 F 0.82115(15) 0.27277(9) 0.12811(7) 0.0247(3) Uani 1 1 d . . . . .
F8 F 0.85578(14) 0.46987(9) 0.17146(7) 0.0162(2) Uani 1 1 d . . . . .
O1 O -0.19660(16) 0.39527(10) -0.20945(7) 0.0128(3) Uani 1 1 d . . . . .
O2 O -0.04654(17) 0.33261(10) -0.31818(7) 0.0129(3) Uani 1 1 d . . . . .
N1 N 0.0284(2) 0.33565(14) -0.07288(11) 0.0121(3) Uani 1 1 d . . . . .
N2 N -0.0357(2) 0.08358(14) -0.32574(10) 0.0111(3) Uani 1 1 d . . . . .
C1 C -0.0123(2) 0.21158(15) -0.19980(11) 0.0096(4) Uani 1 1 d . . . . .
C2 C 0.0416(2) 0.21807(15) -0.11607(11) 0.0105(4) Uani 1 1 d . . . . .
C3 C 0.1152(2) 0.11815(15) -0.07271(11) 0.0124(4) Uani 1 1 d . . . . .
H3 H 0.1507 0.1255 -0.0159 0.015 Uiso 1 1 calc R U . . .
C4 C 0.1371(2) 0.00686(16) -0.11222(11) 0.0132(4) Uani 1 1 d . . . . .
H4 H 0.1861 -0.0627 -0.0825 0.016 Uiso 1 1 calc R U . . .
C5 C 0.0875(2) -0.00294(15) -0.19526(12) 0.0120(4) Uani 1 1 d . . . . .
H5 H 0.1029 -0.0790 -0.2227 0.014 Uiso 1 1 calc R U . . .
C6 C 0.0154(2) 0.09854(15) -0.23789(11) 0.0098(4) Uani 1 1 d . . . . .
C7 C -0.0980(2) 0.32315(15) -0.24231(11) 0.0102(4) Uani 1 1 d . . . . .
C8 C -0.1114(3) 0.44219(16) -0.36309(12) 0.0158(4) Uani 1 1 d . . . . .
H8A H -0.2498 0.4436 -0.3683 0.024 Uiso 1 1 calc R U . . .
H8B H -0.0638 0.4409 -0.4176 0.024 Uiso 1 1 calc R U . . .
H8C H -0.0642 0.5159 -0.3336 0.024 Uiso 1 1 calc R U . . .
B1 B 0.5355(3) 0.31290(18) -0.04509(13) 0.0139(4) Uani 1 1 d . . . . .
B2 B 0.9516(3) 0.36019(19) 0.15515(14) 0.0142(4) Uani 1 1 d . . . . .
H11 H -0.086(3) 0.3531(19) -0.0654(13) 0.024(6) Uiso 1 1 d . . . . .
H12 H 0.076(3) 0.401(2) -0.1043(14) 0.029(6) Uiso 1 1 d . . . . .
H13 H 0.093(3) 0.3332(19) -0.0244(14) 0.023(6) Uiso 1 1 d . . . . .
H21 H -0.168(3) 0.088(2) -0.3383(14) 0.034(6) Uiso 1 1 d . . . . .
H22 H 0.021(3) 0.141(2) -0.3567(15) 0.033(6) Uiso 1 1 d . . . . .
H23 H 0.005(3) 0.007(2) -0.3417(13) 0.026(6) Uiso 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
F1 B1 1.397(2) . ?
F2 B1 1.409(2) . ?
F3 B1 1.404(2) . ?
F4 B1 1.379(2) . ?
F5 B2 1.416(2) . ?
F6 B2 1.377(2) . ?
F7 B2 1.375(2) . ?
F8 B2 1.406(2) . ?
O1 C7 1.205(2) . ?
O2 C7 1.328(2) . ?
O2 C8 1.455(2) . ?
N1 C2 1.466(2) . ?
N1 H11 0.85(2) . ?
N1 H12 0.95(2) . ?
N1 H13 0.89(2) . ?
N2 C6 1.469(2) . ?
N2 H21 0.95(2) . ?
N2 H22 0.92(2) . ?
N2 H23 0.92(2) . ?
C1 C6 1.397(2) . ?
C1 C2 1.400(2) . ?
C1 C7 1.502(2) . ?
C2 C3 1.377(2) . ?
C3 C4 1.385(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(2) . ?
C5 H5 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 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
C7 O2 C8 116.06(13) . . ?
C2 N1 H11 111.1(14) . . ?
C2 N1 H12 110.2(13) . . ?
H11 N1 H12 107.3(19) . . ?
C2 N1 H13 111.1(14) . . ?
H11 N1 H13 108(2) . . ?
H12 N1 H13 109.0(19) . . ?
C6 N2 H21 112.1(14) . . ?
C6 N2 H22 112.5(14) . . ?
H21 N2 H22 108(2) . . ?
C6 N2 H23 108.6(14) . . ?
H21 N2 H23 107.9(19) . . ?
H22 N2 H23 107.4(19) . . ?
C6 C1 C2 116.50(15) . . ?
C6 C1 C7 124.41(16) . . ?
C2 C1 C7 119.08(15) . . ?
C3 C2 C1 122.15(16) . . ?
C3 C2 N1 118.07(16) . . ?
C1 C2 N1 119.72(15) . . ?
C2 C3 C4 119.71(17) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 119.89(16) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C6 C5 C4 119.59(16) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C1 122.14(17) . . ?
C5 C6 N2 117.61(15) . . ?
C1 C6 N2 120.24(15) . . ?
O1 C7 O2 125.49(16) . . ?
O1 C7 C1 122.95(16) . . ?
O2 C7 C1 111.54(14) . . ?
O2 C8 H8A 109.5 . . ?
O2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
F4 B1 F1 110.48(15) . . ?
F4 B1 F3 109.42(15) . . ?
F1 B1 F3 109.75(15) . . ?
F4 B1 F2 110.94(16) . . ?
F1 B1 F2 108.18(15) . . ?
F3 B1 F2 108.03(14) . . ?
F7 B2 F6 112.14(16) . . ?
F7 B2 F8 108.72(15) . . ?
F6 B2 F8 110.86(16) . . ?
F7 B2 F5 110.51(16) . . ?
F6 B2 F5 107.58(15) . . ?
F8 B2 F5 106.90(15) . . ?

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
C6 C1 C2 C3 -1.1(2) . . . . ?
C7 C1 C2 C3 177.80(15) . . . . ?
C6 C1 C2 N1 176.06(15) . . . . ?
C7 C1 C2 N1 -5.0(2) . . . . ?
C1 C2 C3 C4 -0.1(3) . . . . ?
N1 C2 C3 C4 -177.35(15) . . . . ?
C2 C3 C4 C5 0.9(3) . . . . ?
C3 C4 C5 C6 -0.3(3) . . . . ?
C4 C5 C6 C1 -1.0(3) . . . . ?
C4 C5 C6 N2 -179.81(15) . . . . ?
C2 C1 C6 C5 1.7(2) . . . . ?
C7 C1 C6 C5 -177.16(15) . . . . ?
C2 C1 C6 N2 -179.54(14) . . . . ?
C7 C1 C6 N2 1.6(2) . . . . ?
C8 O2 C7 O1 2.2(2) . . . . ?
C8 O2 C7 C1 -175.97(14) . . . . ?
C6 C1 C7 O1 145.37(17) . . . . ?
C2 C1 C7 O1 -33.4(2) . . . . ?
C6 C1 C7 O2 -36.4(2) . . . . ?
C2 C1 C7 O2 144.77(15) . . . . ?

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
C8 H8C F6 0.98 2.53 3.443(2) 155.0 3_665
N2 H23 F2 0.92(2) 1.95(2) 2.8699(18) 175(2) 2_544
N2 H23 F3 0.92(2) 2.63(2) 3.1707(19) 118.0(16) 2_544
N1 H13 F1 0.89(2) 2.38(2) 3.063(2) 133.8(18) .
N1 H13 F5 0.89(2) 2.04(2) 2.784(2) 140.9(19) 1_455
N2 H22 F1 0.92(2) 2.21(2) 2.8373(19) 125.1(18) 4_565
N2 H22 F7 0.92(2) 2.36(2) 3.1168(19) 139.9(19) 4_565
N2 H22 O2 0.92(2) 2.23(2) 2.7056(19) 111.5(17) .
N2 H21 F5 0.95(2) 2.09(2) 2.9937(19) 160(2) 4_465
N2 H21 F6 0.95(2) 2.44(2) 3.1996(19) 136.8(18) 4_465
N1 H12 F5 0.95(2) 2.54(2) 3.1009(19) 117.5(16) 3_665
N1 H12 F8 0.95(2) 1.87(2) 2.8195(19) 173.8(19) 3_665
N1 H11 F3 0.85(2) 1.98(2) 2.8262(19) 169(2) 1_455
N1 H11 F4 0.85(2) 2.61(2) 3.210(2) 128.5(17) 1_455

_refine_diff_density_max         0.294
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.060

_shelxl_version_number           2014-3

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_BPh3COMPLEX
_database_code_depnum_ccdc_archive 'CCDC 1994136'
loop_
_audit_author_name
_audit_author_address
'PROFESSOR J D WALLIS'
;Nottingham Trent University, UK
United Kingdom
;
_audit_update_record             
;
2020-04-01 deposited with the CCDC.	2020-05-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
'Methyl 2,6-diaminobenzoate bis BPh3 complex bis acetontrile solvate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H46 B2 N4 O2'
_chemical_formula_weight         732.51

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   11.5169(8)
_cell_length_b                   12.9904(10)
_cell_length_c                   15.2893(9)
_cell_angle_alpha                67.212(6)
_cell_angle_beta                 77.440(5)
_cell_angle_gamma                77.991(6)
_cell_volume                     2038.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)

_cell_measurement_reflns_used    2166
_cell_measurement_theta_max      29.0500
_cell_measurement_theta_min      3.6150

_exptl_crystal_description       block
_exptl_crystal_colour            colourless

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_F_000             776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_exptl_crystal_size_max          0.414
_exptl_crystal_size_mid          0.316
_exptl_crystal_size_min          0.213


_exptl_absorpt_coefficient_mu    0.072
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?

_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
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_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_detector_area_resol_mean 15.9832
_diffrn_detector_type            Sapphire3
_diffrn_measurement_method       'ω scans'

_diffrn_reflns_number            13681
_diffrn_reflns_av_unetI/netI     0.1154
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.883
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             8170
_reflns_number_gt                4549
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0635P)²+0.0734P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8170
_refine_ls_number_parameters     524
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1469
_refine_ls_R_factor_gt           0.0721
_refine_ls_wR_factor_ref         0.1797
_refine_ls_wR_factor_gt          0.1450
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.44780(19) 0.56137(19) 0.11317(14) 0.0355(5) Uani 1 1 d . . . . .
O2 O 0.26415(18) 0.51946(18) 0.12599(13) 0.0323(5) Uani 1 1 d . . . . .
N1 N 0.5307(2) 0.4572(2) 0.28449(19) 0.0258(6) Uani 1 1 d . . . . .
N2 N 0.0992(2) 0.5951(2) 0.25111(19) 0.0254(6) Uani 1 1 d . . . . .
N71 N 0.6315(3) 0.6244(3) 0.3272(2) 0.0468(8) Uani 1 1 d . . . . .
N81 N -0.0527(3) 0.4169(3) 0.37523(19) 0.0431(7) Uani 1 1 d . . . . .
C1 C 0.3168(3) 0.5273(2) 0.2636(2) 0.0245(7) Uani 1 1 d . . . . .
C2 C 0.4073(3) 0.4891(2) 0.3220(2) 0.0256(7) Uani 1 1 d . . . . .
C3 C 0.3805(3) 0.4765(3) 0.4180(2) 0.0274(7) Uani 1 1 d . . . . .
H3 H 0.4425 0.4504 0.4567 0.033 Uiso 1 1 calc R U . . .
C4 C 0.2639(3) 0.5020(3) 0.4572(2) 0.0293(7) Uani 1 1 d . . . . .
H4 H 0.2457 0.4932 0.5231 0.035 Uiso 1 1 calc R U . . .
C5 C 0.1732(3) 0.5402(3) 0.4018(2) 0.0269(7) Uani 1 1 d . . . . .
H5 H 0.0929 0.5581 0.4293 0.032 Uiso 1 1 calc R U . . .
C6 C 0.1995(2) 0.5522(2) 0.3059(2) 0.0237(7) Uani 1 1 d . . . . .
C7 C 0.3515(3) 0.5392(3) 0.1604(2) 0.0273(7) Uani 1 1 d . . . . .
C8 C 0.2896(3) 0.5285(3) 0.0260(2) 0.0407(9) Uani 1 1 d . . . . .
H8C H 0.2851 0.6081 -0.0156 0.061 Uiso 1 1 calc R U . . .
H8B H 0.2305 0.4937 0.0132 0.061 Uiso 1 1 calc R U . . .
H8A H 0.3703 0.4896 0.0131 0.061 Uiso 1 1 calc R U . . .
C11 C 0.7066(3) 0.3138(3) 0.2367(2) 0.0281(7) Uani 1 1 d . . . . .
C12 C 0.7824(3) 0.3962(3) 0.2026(2) 0.0307(7) Uani 1 1 d . . . . .
H12 H 0.7554 0.4641 0.2151 0.037 Uiso 1 1 calc R U . . .
C13 C 0.8962(3) 0.3828(3) 0.1508(2) 0.0363(8) Uani 1 1 d . . . . .
H13 H 0.9455 0.4408 0.1292 0.044 Uiso 1 1 calc R U . . .
C14 C 0.9378(3) 0.2857(3) 0.1308(2) 0.0386(9) Uani 1 1 d . . . . .
H14 H 1.0146 0.2771 0.0939 0.046 Uiso 1 1 calc R U . . .
C15 C 0.8662(3) 0.2010(3) 0.1650(2) 0.0344(8) Uani 1 1 d . . . . .
H15 H 0.8945 0.1329 0.1531 0.041 Uiso 1 1 calc R U . . .
C16 C 0.7537(3) 0.2151(3) 0.2165(2) 0.0313(8) Uani 1 1 d . . . . .
H16 H 0.7060 0.1557 0.2393 0.038 Uiso 1 1 calc R U . . .
C21 C 0.5955(3) 0.2528(3) 0.4138(2) 0.0262(7) Uani 1 1 d . . . . .
C22 C 0.6371(3) 0.2996(3) 0.4678(2) 0.0327(8) Uani 1 1 d . . . . .
H22 H 0.6463 0.3773 0.4408 0.039 Uiso 1 1 calc R U . . .
C23 C 0.6652(3) 0.2371(3) 0.5592(2) 0.0382(8) Uani 1 1 d . . . . .
H23 H 0.6913 0.2725 0.5940 0.046 Uiso 1 1 calc R U . . .
C24 C 0.6555(3) 0.1240(3) 0.5994(2) 0.0400(9) Uani 1 1 d . . . . .
H24 H 0.6753 0.0808 0.6617 0.048 Uiso 1 1 calc R U . . .
C25 C 0.6166(3) 0.0740(3) 0.5482(2) 0.0388(8) Uani 1 1 d . . . . .
H25 H 0.6098 -0.0042 0.5750 0.047 Uiso 1 1 calc R U . . .
C26 C 0.5873(3) 0.1385(3) 0.4572(2) 0.0344(8) Uani 1 1 d . . . . .
H26 H 0.5605 0.1025 0.4232 0.041 Uiso 1 1 calc R U . . .
C31 C 0.4726(3) 0.2797(3) 0.2706(2) 0.0267(7) Uani 1 1 d . . . . .
C32 C 0.3680(3) 0.2470(3) 0.3329(2) 0.0318(8) Uani 1 1 d . . . . .
H32 H 0.3594 0.2439 0.3971 0.038 Uiso 1 1 calc R U . . .
C33 C 0.2758(3) 0.2189(3) 0.3050(2) 0.0394(9) Uani 1 1 d . . . . .
H33 H 0.2049 0.1991 0.3491 0.047 Uiso 1 1 calc R U . . .
C34 C 0.2875(3) 0.2198(3) 0.2129(2) 0.0405(9) Uani 1 1 d . . . . .
H34 H 0.2255 0.1990 0.1936 0.049 Uiso 1 1 calc R U . . .
C35 C 0.3890(3) 0.2507(3) 0.1498(2) 0.0380(8) Uani 1 1 d . . . . .
H35 H 0.3976 0.2516 0.0863 0.046 Uiso 1 1 calc R U . . .
C36 C 0.4801(3) 0.2812(3) 0.1780(2) 0.0320(8) Uani 1 1 d . . . . .
H36 H 0.5494 0.3036 0.1326 0.038 Uiso 1 1 calc R U . . .
C41 C 0.1845(3) 0.7855(2) 0.1463(2) 0.0277(7) Uani 1 1 d . . . . .
C42 C 0.2231(3) 0.8001(3) 0.0493(2) 0.0309(7) Uani 1 1 d . . . . .
H42 H 0.1741 0.7812 0.0167 0.037 Uiso 1 1 calc R U . . .
C43 C 0.3288(3) 0.8405(3) -0.0008(2) 0.0373(8) Uani 1 1 d . . . . .
H43 H 0.3504 0.8506 -0.0670 0.045 Uiso 1 1 calc R U . . .
C44 C 0.4031(3) 0.8664(3) 0.0448(3) 0.0437(9) Uani 1 1 d . . . . .
H44 H 0.4765 0.8938 0.0108 0.052 Uiso 1 1 calc R U . . .
C45 C 0.3695(3) 0.8520(3) 0.1402(3) 0.0476(10) Uani 1 1 d . . . . .
H45 H 0.4201 0.8696 0.1724 0.057 Uiso 1 1 calc R U . . .
C46 C 0.2629(3) 0.8122(3) 0.1898(2) 0.0371(8) Uani 1 1 d . . . . .
H46 H 0.2422 0.8026 0.2558 0.045 Uiso 1 1 calc R U . . .
C51 C -0.0066(3) 0.7813(3) 0.2896(2) 0.0275(7) Uani 1 1 d . . . . .
C52 C -0.0848(3) 0.7213(3) 0.3680(2) 0.0348(8) Uani 1 1 d . . . . .
H52 H -0.0918 0.6467 0.3756 0.042 Uiso 1 1 calc R U . . .
C53 C -0.1522(3) 0.7658(3) 0.4349(2) 0.0415(9) Uani 1 1 d . . . . .
H53 H -0.2024 0.7211 0.4881 0.050 Uiso 1 1 calc R U . . .
C54 C -0.1465(3) 0.8752(3) 0.4242(2) 0.0453(9) Uani 1 1 d . . . . .
H54 H -0.1933 0.9068 0.4694 0.054 Uiso 1 1 calc R U . . .
C55 C -0.0722(3) 0.9376(3) 0.3472(2) 0.0472(10) Uani 1 1 d . . . . .
H55 H -0.0688 1.0135 0.3384 0.057 Uiso 1 1 calc R U . . .
C56 C -0.0022(3) 0.8908(3) 0.2822(2) 0.0383(8) Uani 1 1 d . . . . .
H56 H 0.0506 0.9349 0.2309 0.046 Uiso 1 1 calc R U . . .
C61 C -0.0376(3) 0.7560(3) 0.1356(2) 0.0265(7) Uani 1 1 d . . . . .
C62 C -0.1053(3) 0.6770(3) 0.1394(2) 0.0315(8) Uani 1 1 d . . . . .
H62 H -0.0911 0.6020 0.1833 0.038 Uiso 1 1 calc R U . . .
C63 C -0.1931(3) 0.7036(3) 0.0813(2) 0.0343(8) Uani 1 1 d . . . . .
H63 H -0.2366 0.6468 0.0855 0.041 Uiso 1 1 calc R U . . .
C64 C -0.2171(3) 0.8117(3) 0.0181(2) 0.0339(8) Uani 1 1 d . . . . .
H64 H -0.2773 0.8302 -0.0214 0.041 Uiso 1 1 calc R U . . .
C65 C -0.1529(3) 0.8931(3) 0.0124(2) 0.0334(8) Uani 1 1 d . . . . .
H65 H -0.1684 0.9681 -0.0312 0.040 Uiso 1 1 calc R U . . .
C66 C -0.0659(3) 0.8652(3) 0.0705(2) 0.0304(7) Uani 1 1 d . . . . .
H66 H -0.0233 0.9227 0.0661 0.036 Uiso 1 1 calc R U . . .
C71 C 0.6413(3) 0.7174(3) 0.2982(2) 0.0357(8) Uani 1 1 d . . . . .
C72 C 0.6542(3) 0.8372(3) 0.2605(3) 0.0467(9) Uani 1 1 d . . . . .
H72C H 0.6464 0.8694 0.1922 0.070 Uiso 1 1 calc R U . . .
H72A H 0.7334 0.8459 0.2684 0.070 Uiso 1 1 calc R U . . .
H72B H 0.5916 0.8765 0.2956 0.070 Uiso 1 1 calc R U . . .
C81 C -0.0589(3) 0.3256(3) 0.3874(2) 0.0354(8) Uani 1 1 d . . . . .
C82 C -0.0655(3) 0.2112(3) 0.4009(3) 0.0459(9) Uani 1 1 d . . . . .
H82A H -0.0126 0.1912 0.3487 0.069 Uiso 1 1 calc R U . . .
H82C H -0.1484 0.2034 0.4010 0.069 Uiso 1 1 calc R U . . .
H82B H -0.0402 0.1609 0.4624 0.069 Uiso 1 1 calc R U . . .
B1 B 0.5762(3) 0.3201(3) 0.3023(2) 0.0251(8) Uani 1 1 d . . . . .
B2 B 0.0611(3) 0.7355(3) 0.2043(2) 0.0273(8) Uani 1 1 d . . . . .
H21B H 0.034(3) 0.558(2) 0.292(2) 0.027(8) Uiso 1 1 d . . . . .
H11A H 0.546(3) 0.496(3) 0.216(2) 0.045(10) Uiso 1 1 d . . . . .
H21A H 0.126(2) 0.576(2) 0.197(2) 0.027(8) Uiso 1 1 d . . . . .
H11B H 0.581(3) 0.489(3) 0.308(2) 0.050(10) Uiso 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 C7 1.207(3) . ?
O2 C7 1.340(3) . ?
O2 C8 1.456(3) . ?
N1 C2 1.451(4) . ?
N1 B1 1.679(4) . ?
N1 H11A 0.96(3) . ?
N1 H11B 0.97(4) . ?
N2 C6 1.462(3) . ?
N2 B2 1.681(4) . ?
N2 H21B 0.95(3) . ?
N2 H21A 0.93(3) . ?
N71 C71 1.135(4) . ?
N81 C81 1.142(4) . ?
C1 C6 1.397(4) . ?
C1 C2 1.406(4) . ?
C1 C7 1.495(4) . ?
C2 C3 1.384(4) . ?
C3 C4 1.375(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.378(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(4) . ?
C5 H5 0.9500 . ?
C8 H8C 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8A 0.9800 . ?
C11 C12 1.393(4) . ?
C11 C16 1.406(4) . ?
C11 B1 1.620(5) . ?
C12 C13 1.391(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.378(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.381(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.379(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C26 1.386(4) . ?
C21 C22 1.402(4) . ?
C21 B1 1.628(4) . ?
C22 C23 1.387(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.374(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.380(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.391(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C32 1.393(4) . ?
C31 C36 1.393(4) . ?
C31 B1 1.626(4) . ?
C32 C33 1.386(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.381(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.364(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.394(4) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C46 1.396(4) . ?
C41 C42 1.400(4) . ?
C41 B2 1.618(5) . ?
C42 C43 1.376(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.376(5) . ?
C43 H43 0.9500 . ?
C44 C45 1.373(5) . ?
C44 H44 0.9500 . ?
C45 C46 1.380(4) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C51 C56 1.393(4) . ?
C51 C52 1.397(4) . ?
C51 B2 1.621(4) . ?
C52 C53 1.381(4) . ?
C52 H52 0.9500 . ?
C53 C54 1.380(5) . ?
C53 H53 0.9500 . ?
C54 C55 1.374(5) . ?
C54 H54 0.9500 . ?
C55 C56 1.387(5) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C61 C62 1.389(4) . ?
C61 C66 1.401(4) . ?
C61 B2 1.626(4) . ?
C62 C63 1.392(4) . ?
C62 H62 0.9500 . ?
C63 C64 1.373(4) . ?
C63 H63 0.9500 . ?
C64 C65 1.378(4) . ?
C64 H64 0.9500 . ?
C65 C66 1.382(4) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C71 C72 1.463(5) . ?
C72 H72C 0.9800 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C81 C82 1.435(5) . ?
C82 H82A 0.9800 . ?
C82 H82C 0.9800 . ?
C82 H82B 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
C7 O2 C8 116.4(2) . . ?
C2 N1 B1 117.5(2) . . ?
C2 N1 H11A 110(2) . . ?
B1 N1 H11A 105.7(19) . . ?
C2 N1 H11B 107(2) . . ?
B1 N1 H11B 113(2) . . ?
H11A N1 H11B 103(3) . . ?
C6 N2 B2 117.8(2) . . ?
C6 N2 H21B 106.0(17) . . ?
B2 N2 H21B 112.2(17) . . ?
C6 N2 H21A 105.0(17) . . ?
B2 N2 H21A 102.7(17) . . ?
H21B N2 H21A 113(2) . . ?
C6 C1 C2 117.6(2) . . ?
C6 C1 C7 123.9(2) . . ?
C2 C1 C7 118.5(3) . . ?
C3 C2 C1 121.0(3) . . ?
C3 C2 N1 118.0(3) . . ?
C1 C2 N1 121.0(3) . . ?
C4 C3 C2 119.8(3) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 120.7(3) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C6 119.7(3) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C5 C6 C1 121.2(3) . . ?
C5 C6 N2 116.7(2) . . ?
C1 C6 N2 122.1(2) . . ?
O1 C7 O2 123.2(3) . . ?
O1 C7 C1 124.5(3) . . ?
O2 C7 C1 112.3(3) . . ?
O2 C8 H8C 109.5 . . ?
O2 C8 H8B 109.5 . . ?
H8C C8 H8B 109.5 . . ?
O2 C8 H8A 109.5 . . ?
H8C C8 H8A 109.5 . . ?
H8B C8 H8A 109.5 . . ?
C12 C11 C16 115.4(3) . . ?
C12 C11 B1 125.4(3) . . ?
C16 C11 B1 119.1(3) . . ?
C13 C12 C11 122.4(3) . . ?
C13 C12 H12 118.8 . . ?
C11 C12 H12 118.8 . . ?
C14 C13 C12 120.3(3) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 119.0(3) . . ?
C13 C14 H14 120.5 . . ?
C15 C14 H14 120.5 . . ?
C16 C15 C14 120.2(3) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C15 C16 C11 122.6(3) . . ?
C15 C16 H16 118.7 . . ?
C11 C16 H16 118.7 . . ?
C26 C21 C22 115.2(3) . . ?
C26 C21 B1 120.6(3) . . ?
C22 C21 B1 123.6(3) . . ?
C23 C22 C21 122.6(3) . . ?
C23 C22 H22 118.7 . . ?
C21 C22 H22 118.7 . . ?
C24 C23 C22 120.1(3) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 119.2(3) . . ?
C23 C24 H24 120.4 . . ?
C25 C24 H24 120.4 . . ?
C24 C25 C26 119.8(3) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C21 C26 C25 123.1(3) . . ?
C21 C26 H26 118.5 . . ?
C25 C26 H26 118.5 . . ?
C32 C31 C36 115.8(3) . . ?
C32 C31 B1 122.1(3) . . ?
C36 C31 B1 122.0(3) . . ?
C33 C32 C31 122.6(3) . . ?
C33 C32 H32 118.7 . . ?
C31 C32 H32 118.7 . . ?
C34 C33 C32 119.8(3) . . ?
C34 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C35 C34 C33 119.4(3) . . ?
C35 C34 H34 120.3 . . ?
C33 C34 H34 120.3 . . ?
C34 C35 C36 120.4(3) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
C31 C36 C35 122.0(3) . . ?
C31 C36 H36 119.0 . . ?
C35 C36 H36 119.0 . . ?
C46 C41 C42 115.1(3) . . ?
C46 C41 B2 122.7(3) . . ?
C42 C41 B2 122.1(3) . . ?
C43 C42 C41 123.0(3) . . ?
C43 C42 H42 118.5 . . ?
C41 C42 H42 118.5 . . ?
C44 C43 C42 120.0(3) . . ?
C44 C43 H43 120.0 . . ?
C42 C43 H43 120.0 . . ?
C45 C44 C43 118.9(3) . . ?
C45 C44 H44 120.5 . . ?
C43 C44 H44 120.5 . . ?
C44 C45 C46 120.7(3) . . ?
C44 C45 H45 119.6 . . ?
C46 C45 H45 119.6 . . ?
C45 C46 C41 122.3(3) . . ?
C45 C46 H46 118.9 . . ?
C41 C46 H46 118.9 . . ?
C56 C51 C52 115.4(3) . . ?
C56 C51 B2 120.9(3) . . ?
C52 C51 B2 123.2(3) . . ?
C53 C52 C51 122.9(3) . . ?
C53 C52 H52 118.5 . . ?
C51 C52 H52 118.5 . . ?
C54 C53 C52 119.9(3) . . ?
C54 C53 H53 120.1 . . ?
C52 C53 H53 120.1 . . ?
C55 C54 C53 119.0(3) . . ?
C55 C54 H54 120.5 . . ?
C53 C54 H54 120.5 . . ?
C54 C55 C56 120.5(3) . . ?
C54 C55 H55 119.7 . . ?
C56 C55 H55 119.7 . . ?
C55 C56 C51 122.2(3) . . ?
C55 C56 H56 118.9 . . ?
C51 C56 H56 118.9 . . ?
C62 C61 C66 115.1(3) . . ?
C62 C61 B2 126.4(3) . . ?
C66 C61 B2 118.3(3) . . ?
C61 C62 C63 122.6(3) . . ?
C61 C62 H62 118.7 . . ?
C63 C62 H62 118.7 . . ?
C64 C63 C62 120.2(3) . . ?
C64 C63 H63 119.9 . . ?
C62 C63 H63 119.9 . . ?
C63 C64 C65 119.3(3) . . ?
C63 C64 H64 120.4 . . ?
C65 C64 H64 120.4 . . ?
C64 C65 C66 119.7(3) . . ?
C64 C65 H65 120.1 . . ?
C66 C65 H65 120.1 . . ?
C65 C66 C61 123.1(3) . . ?
C65 C66 H66 118.5 . . ?
C61 C66 H66 118.5 . . ?
N71 C71 C72 179.8(5) . . ?
C71 C72 H72C 109.5 . . ?
C71 C72 H72A 109.5 . . ?
H72C C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72C C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
N81 C81 C82 179.0(4) . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
C81 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
H82C C82 H82B 109.5 . . ?
C11 B1 C31 114.4(2) . . ?
C11 B1 C21 107.4(2) . . ?
C31 B1 C21 114.2(3) . . ?
C11 B1 N1 106.1(2) . . ?
C31 B1 N1 105.2(2) . . ?
C21 B1 N1 109.2(2) . . ?
C41 B2 C51 115.6(3) . . ?
C41 B2 C61 113.4(2) . . ?
C51 B2 C61 106.8(2) . . ?
C41 B2 N2 105.6(2) . . ?
C51 B2 N2 109.2(2) . . ?
C61 B2 N2 105.7(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
C6 C1 C2 C3 0.1(4) . . . . ?
C7 C1 C2 C3 180.0(3) . . . . ?
C6 C1 C2 N1 177.6(3) . . . . ?
C7 C1 C2 N1 -2.6(4) . . . . ?
B1 N1 C2 C3 82.2(3) . . . . ?
B1 N1 C2 C1 -95.3(3) . . . . ?
C1 C2 C3 C4 -0.2(4) . . . . ?
N1 C2 C3 C4 -177.7(3) . . . . ?
C2 C3 C4 C5 -0.1(4) . . . . ?
C3 C4 C5 C6 0.5(4) . . . . ?
C4 C5 C6 C1 -0.6(4) . . . . ?
C4 C5 C6 N2 -178.9(3) . . . . ?
C2 C1 C6 C5 0.3(4) . . . . ?
C7 C1 C6 C5 -179.6(3) . . . . ?
C2 C1 C6 N2 178.5(3) . . . . ?
C7 C1 C6 N2 -1.4(4) . . . . ?
B2 N2 C6 C5 84.6(3) . . . . ?
B2 N2 C6 C1 -93.7(3) . . . . ?
C8 O2 C7 O1 -1.4(4) . . . . ?
C8 O2 C7 C1 -179.7(2) . . . . ?
C6 C1 C7 O1 149.8(3) . . . . ?
C2 C1 C7 O1 -30.1(4) . . . . ?
C6 C1 C7 O2 -31.8(4) . . . . ?
C2 C1 C7 O2 148.3(3) . . . . ?
C16 C11 C12 C13 0.9(4) . . . . ?
B1 C11 C12 C13 176.5(3) . . . . ?
C11 C12 C13 C14 0.5(5) . . . . ?
C12 C13 C14 C15 -1.7(5) . . . . ?
C13 C14 C15 C16 1.5(4) . . . . ?
C14 C15 C16 C11 -0.1(4) . . . . ?
C12 C11 C16 C15 -1.1(4) . . . . ?
B1 C11 C16 C15 -177.0(3) . . . . ?
C26 C21 C22 C23 -1.6(4) . . . . ?
B1 C21 C22 C23 -172.8(3) . . . . ?
C21 C22 C23 C24 1.5(5) . . . . ?
C22 C23 C24 C25 -0.5(5) . . . . ?
C23 C24 C25 C26 -0.3(5) . . . . ?
C22 C21 C26 C25 0.7(4) . . . . ?
B1 C21 C26 C25 172.2(3) . . . . ?
C24 C25 C26 C21 0.2(5) . . . . ?
C36 C31 C32 C33 -0.8(4) . . . . ?
B1 C31 C32 C33 176.0(3) . . . . ?
C31 C32 C33 C34 1.8(5) . . . . ?
C32 C33 C34 C35 -1.4(5) . . . . ?
C33 C34 C35 C36 0.0(5) . . . . ?
C32 C31 C36 C35 -0.6(4) . . . . ?
B1 C31 C36 C35 -177.4(3) . . . . ?
C34 C35 C36 C31 1.0(5) . . . . ?
C46 C41 C42 C43 -1.6(4) . . . . ?
B2 C41 C42 C43 -178.8(3) . . . . ?
C41 C42 C43 C44 1.4(5) . . . . ?
C42 C43 C44 C45 -0.5(5) . . . . ?
C43 C44 C45 C46 0.0(5) . . . . ?
C44 C45 C46 C41 -0.4(5) . . . . ?
C42 C41 C46 C45 1.1(5) . . . . ?
B2 C41 C46 C45 178.3(3) . . . . ?
C56 C51 C52 C53 -1.0(4) . . . . ?
B2 C51 C52 C53 -172.7(3) . . . . ?
C51 C52 C53 C54 1.9(5) . . . . ?
C52 C53 C54 C55 -0.7(5) . . . . ?
C53 C54 C55 C56 -1.3(5) . . . . ?
C54 C55 C56 C51 2.3(5) . . . . ?
C52 C51 C56 C55 -1.1(5) . . . . ?
B2 C51 C56 C55 170.8(3) . . . . ?
C66 C61 C62 C63 1.3(4) . . . . ?
B2 C61 C62 C63 176.1(3) . . . . ?
C61 C62 C63 C64 -0.9(5) . . . . ?
C62 C63 C64 C65 0.3(5) . . . . ?
C63 C64 C65 C66 -0.2(5) . . . . ?
C64 C65 C66 C61 0.7(5) . . . . ?
C62 C61 C66 C65 -1.3(4) . . . . ?
B2 C61 C66 C65 -176.5(3) . . . . ?
C12 C11 B1 C31 136.7(3) . . . . ?
C16 C11 B1 C31 -47.9(4) . . . . ?
C12 C11 B1 C21 -95.5(3) . . . . ?
C16 C11 B1 C21 79.9(3) . . . . ?
C12 C11 B1 N1 21.2(4) . . . . ?
C16 C11 B1 N1 -163.4(2) . . . . ?
C32 C31 B1 C11 160.2(3) . . . . ?
C36 C31 B1 C11 -23.2(4) . . . . ?
C32 C31 B1 C21 36.0(4) . . . . ?
C36 C31 B1 C21 -147.5(3) . . . . ?
C32 C31 B1 N1 -83.8(3) . . . . ?
C36 C31 B1 N1 92.8(3) . . . . ?
C26 C21 B1 C11 -90.4(3) . . . . ?
C22 C21 B1 C11 80.4(4) . . . . ?
C26 C21 B1 C31 37.6(4) . . . . ?
C22 C21 B1 C31 -151.7(3) . . . . ?
C26 C21 B1 N1 155.0(3) . . . . ?
C22 C21 B1 N1 -34.2(4) . . . . ?
C2 N1 B1 C11 169.7(2) . . . . ?
C2 N1 B1 C31 48.2(3) . . . . ?
C2 N1 B1 C21 -74.9(3) . . . . ?
C46 C41 B2 C51 33.9(4) . . . . ?
C42 C41 B2 C51 -149.2(3) . . . . ?
C46 C41 B2 C61 157.7(3) . . . . ?
C42 C41 B2 C61 -25.4(4) . . . . ?
C46 C41 B2 N2 -87.0(3) . . . . ?
C42 C41 B2 N2 90.0(3) . . . . ?
C56 C51 B2 C41 33.2(4) . . . . ?
C52 C51 B2 C41 -155.5(3) . . . . ?
C56 C51 B2 C61 -94.0(3) . . . . ?
C52 C51 B2 C61 77.3(3) . . . . ?
C56 C51 B2 N2 152.0(3) . . . . ?
C52 C51 B2 N2 -36.7(4) . . . . ?
C62 C61 B2 C41 134.7(3) . . . . ?
C66 C61 B2 C41 -50.7(4) . . . . ?
C62 C61 B2 C51 -96.8(3) . . . . ?
C66 C61 B2 C51 77.8(3) . . . . ?
C62 C61 B2 N2 19.4(4) . . . . ?
C66 C61 B2 N2 -165.9(2) . . . . ?
C6 N2 B2 C41 51.2(3) . . . . ?
C6 N2 B2 C51 -73.7(3) . . . . ?
C6 N2 B2 C61 171.7(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
N2 H21B N81 0.95(3) 2.09(3) 2.976(4) 154(2) .
N1 H11A O1 0.96(3) 1.96(3) 2.722(3) 135(3) .
N2 H21A O2 0.93(3) 1.90(3) 2.708(3) 144(2) .
N1 H11B N71 0.97(4) 2.10(4) 2.995(4) 152(3) .

_refine_diff_density_max         0.274
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.051

_vrf_PLAT910_BPh3COMPLEX         
;
PROBLEM:  Missing # of FCF Reflection(s) Below Theta(Min).         11 Note 
RESPONSE: We only had one crystal of this serendipitously obtained material,
and took a pragmatic approach to the data processing.
;

_shelxl_version_number           2014-3

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
